# Electronic Supplementary Material (ESI) for Chemical Science. # This journal is © The Royal Society of Chemistry 2021 ####################################################################### # # This file contains crystal structure data downloaded from the # Cambridge Structural Database (CSD) hosted by the Cambridge # Crystallographic Data Centre (CCDC). # # Full information about CCDC data access policies and citation # guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 # # Audit and citation data items may have been added by the CCDC. # Please retain this information to preserve the provenance of # this file and to allow appropriate attribution of the data. # ####################################################################### data_m4279_0m _database_code_depnum_ccdc_archive 'CCDC 2071227' loop_ _audit_author_name _audit_author_address 'Qilin Wang' ;Henan University China ; _audit_update_record ; 2021-03-18 deposited with the CCDC. 2021-11-08 downloaded from the CCDC. ; _audit_creation_date 2020-09-15 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _shelx_SHELXL_version_number 2014/7 _chemical_name_common ? _chemical_name_systematic ? _chemical_formula_moiety 'C36 H28 N2 O5' _chemical_formula_sum 'C36 H28 N2 O5' _chemical_formula_weight 568.60 _chemical_absolute_configuration ? _chemical_melting_point ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _space_group_crystal_system orthorhombic _space_group_IT_number 33 _space_group_name_H-M_alt 'P n a 21' _space_group_name_Hall 'P 2c -2n' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z+1/2' _cell_length_a 17.46(3) _cell_length_b 13.75(2) _cell_length_c 23.42(6) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 5624(19) _cell_formula_units_Z 8 _cell_measurement_reflns_used 4397 _cell_measurement_temperature 150(2) _cell_measurement_theta_max 27.650 _cell_measurement_theta_min 2.568 _shelx_estimated_absorpt_T_max 0.996 _shelx_estimated_absorpt_T_min 0.988 _exptl_absorpt_coefficient_mu 0.090 _exptl_absorpt_correction_T_max 0.7457 _exptl_absorpt_correction_T_min 0.6214 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1345 before and 0.0821 after correction. The Ratio of minimum to maximum transmission is 0.8333. The \l/2 correction factor is Not present.' _exptl_absorpt_special_details ? _exptl_crystal_colour yellow _exptl_crystal_colour_primary yellow _exptl_crystal_density_diffrn 1.343 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description plate _exptl_crystal_F_000 2384 _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.05 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.1053 _diffrn_reflns_av_unetI/netI 0.1056 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_number 38519 _diffrn_reflns_point_group_measured_fraction_full 0.962 _diffrn_reflns_point_group_measured_fraction_max 0.957 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 26.365 _diffrn_reflns_theta_min 2.333 _diffrn_ambient_temperature 150.02 _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device_type 'Bruker AXS area detector' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source ? _reflns_Friedel_coverage 0.868 _reflns_Friedel_fraction_full 0.923 _reflns_Friedel_fraction_max 0.912 _reflns_number_gt 6628 _reflns_number_total 10995 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement 'SAINT V8.38A (?, 2016)' _computing_data_collection ? _computing_data_reduction 'SAINT V8.38A (?, 2016)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'ShelXT (Sheldrick, 2015)' _refine_diff_density_max 0.330 _refine_diff_density_min -0.270 _refine_diff_density_rms 0.065 _refine_ls_abs_structure_details ; Flack x determined using 2231 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack 0.1(10) _refine_ls_extinction_coef 0.0065(6) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method 'SHELXL-2014/7 (Sheldrick 2014' _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 776 _refine_ls_number_reflns 10995 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1261 _refine_ls_R_factor_gt 0.0619 _refine_ls_restrained_S_all 1.021 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0659P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1254 _refine_ls_wR_factor_ref 0.1575 _refine_special_details ? _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups 2.a Ternary CH refined with riding coordinates: C8(H8), C9(H9), C19(H19), C8'(H8'), C9'(H9'), C19'(H19') 2.b Secondary CH2 refined with riding coordinates: C16(H16a,H16b), C20(H20a,H20b), C16'(H16c,H16d), C20'(H20c,H20d) 2.c Aromatic/amide H refined with riding coordinates: C1(H1), C2(H2), C3(H3), C4(H4), C5(H5), C11(H11), C12(H12), C13(H13), C14(H14), C17(H17), C21(H21), C25(H25), C26(H26), C27(H27), C28(H28), C29(H29), C32(H32), C33(H33), C34(H34), C35(H35), C36(H36), C1'(H1'), C2'(H2'), C3'(H3'), C4'(H4'), C5'(H5'), C11'(H11'), C12'(H12'), C13'(H13'), C14'(H14'), C17'(H17'), C21'(H21'), C25'(H25'), C26'(H26'), C27'(H27'), C28'(H28'), C29'(H29'), C32'(H32'), C33'(H33'), C34'(H34'), C35'(H35'), C36'(H36') ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _atom_sites_solution_secondary ? loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.7675(3) 0.4004(4) 0.6371(3) 0.0340(15) Uani 1 1 d . . . . . H1 H 0.7416 0.4573 0.6245 0.041 Uiso 1 1 calc R . . . . C2 C 0.8466(3) 0.4021(5) 0.6458(3) 0.0407(17) Uani 1 1 d . . . . . H2 H 0.8747 0.4603 0.6396 0.049 Uiso 1 1 calc R . . . . C3 C 0.8838(3) 0.3186(5) 0.6634(3) 0.0375(16) Uani 1 1 d . . . . . H3 H 0.9376 0.3197 0.6691 0.045 Uiso 1 1 calc R . . . . C4 C 0.8444(3) 0.2349(5) 0.6725(3) 0.0379(16) Uani 1 1 d . . . . . H4 H 0.8710 0.1781 0.6844 0.046 Uiso 1 1 calc R . . . . C5 C 0.7657(3) 0.2315(5) 0.6648(3) 0.0375(16) Uani 1 1 d . . . . . H5 H 0.7385 0.1728 0.6716 0.045 Uiso 1 1 calc R . . . . C6 C 0.7264(3) 0.3148(4) 0.6469(3) 0.0302(14) Uani 1 1 d . . . . . C7 C 0.6422(3) 0.3084(4) 0.6397(3) 0.0301(14) Uani 1 1 d . . . . . C8 C 0.6040(3) 0.3701(4) 0.5947(3) 0.0288(14) Uani 1 1 d . . . . . H8 H 0.6277 0.4362 0.5955 0.035 Uiso 1 1 calc R . . . . C9 C 0.5180(3) 0.3809(4) 0.6069(3) 0.0325(15) Uani 1 1 d . . . . . H9 H 0.4951 0.3150 0.6127 0.039 Uiso 1 1 calc R . . . . C10 C 0.4957(3) 0.4464(4) 0.6566(3) 0.0330(15) Uani 1 1 d . . . . . C11 C 0.5224(4) 0.4490(5) 0.7120(3) 0.0376(16) Uani 1 1 d . . . . . H11 H 0.5604 0.4042 0.7243 0.045 Uiso 1 1 calc R . . . . C12 C 0.4934(4) 0.5173(5) 0.7494(3) 0.0448(18) Uani 1 1 d . . . . . H12 H 0.5128 0.5204 0.7873 0.054 Uiso 1 1 calc R . . . . C13 C 0.4368(4) 0.5811(5) 0.7326(3) 0.0429(18) Uani 1 1 d . . . . . H13 H 0.4167 0.6268 0.7591 0.052 Uiso 1 1 calc R . . . . C14 C 0.4093(3) 0.5789(5) 0.6773(3) 0.0418(18) Uani 1 1 d . . . . . H14 H 0.3705 0.6229 0.6654 0.050 Uiso 1 1 calc R . . . . C15 C 0.4391(3) 0.5113(4) 0.6393(3) 0.0358(16) Uani 1 1 d . . . . . C16 C 0.4180(3) 0.4961(5) 0.5777(3) 0.0418(18) Uani 1 1 d . . . . . H16A H 0.3667 0.4662 0.5738 0.050 Uiso 1 1 calc R . . . . H16B H 0.4194 0.5578 0.5559 0.050 Uiso 1 1 calc R . . . . C17 C 0.5067(3) 0.4267(4) 0.5070(3) 0.0315(16) Uani 1 1 d . . . . . H17 H 0.4798 0.4606 0.4779 0.038 Uiso 1 1 calc R . . . . C18 C 0.5723(3) 0.3779(4) 0.4923(3) 0.0330(15) Uani 1 1 d . . . . . C19 C 0.6201(3) 0.3241(4) 0.5353(3) 0.0310(15) Uani 1 1 d . . . . . H19 H 0.6753 0.3348 0.5258 0.037 Uiso 1 1 calc R . . . . C20 C 0.6045(3) 0.2131(4) 0.5352(3) 0.0330(15) Uani 1 1 d . . . . . H20A H 0.6412 0.1817 0.5615 0.040 Uiso 1 1 calc R . . . . H20B H 0.5524 0.2019 0.5506 0.040 Uiso 1 1 calc R . . . . C21 C 0.6101(3) 0.1640(4) 0.4782(3) 0.0324(15) Uani 1 1 d . . . . . H21 H 0.6583 0.1647 0.4594 0.039 Uiso 1 1 calc R . . . . C22 C 0.5518(3) 0.1192(4) 0.4521(3) 0.0328(16) Uani 1 1 d . . . . . C23 C 0.5597(4) 0.0591(4) 0.3991(3) 0.0407(17) Uani 1 1 d . . . . . C24 C 0.6218(3) 0.0757(5) 0.3575(3) 0.0392(17) Uani 1 1 d . . . . . C25 C 0.6507(4) -0.0045(5) 0.3277(3) 0.050(2) Uani 1 1 d . . . . . H25 H 0.6321 -0.0680 0.3356 0.060 Uiso 1 1 calc R . . . . C26 C 0.7067(5) 0.0092(6) 0.2866(4) 0.062(2) Uani 1 1 d . . . . . H26 H 0.7275 -0.0453 0.2671 0.074 Uiso 1 1 calc R . . . . C27 C 0.7327(4) 0.1014(7) 0.2736(4) 0.065(2) Uani 1 1 d . . . . . H27 H 0.7708 0.1101 0.2451 0.077 Uiso 1 1 calc R . . . . C28 C 0.7033(4) 0.1814(6) 0.3022(4) 0.059(2) Uani 1 1 d . . . . . H28 H 0.7207 0.2448 0.2929 0.071 Uiso 1 1 calc R . . . . C29 C 0.6481(4) 0.1686(5) 0.3446(3) 0.0476(19) Uani 1 1 d . . . . . H29 H 0.6285 0.2233 0.3646 0.057 Uiso 1 1 calc R . . . . C30 C 0.4735(3) 0.1196(5) 0.4792(3) 0.0386(16) Uani 1 1 d . . . . . C31 C 0.4209(3) 0.2006(4) 0.4632(3) 0.0351(16) Uani 1 1 d . . . . . C32 C 0.3639(3) 0.2297(5) 0.5011(3) 0.0463(19) Uani 1 1 d . . . . . H32 H 0.3573 0.1962 0.5362 0.056 Uiso 1 1 calc R . . . . C33 C 0.3172(3) 0.3068(6) 0.4878(4) 0.056(2) Uani 1 1 d . . . . . H33 H 0.2792 0.3275 0.5141 0.067 Uiso 1 1 calc R . . . . C34 C 0.3254(4) 0.3544(5) 0.4362(4) 0.053(2) Uani 1 1 d . . . . . H34 H 0.2926 0.4073 0.4271 0.064 Uiso 1 1 calc R . . . . C35 C 0.3807(3) 0.3258(5) 0.3977(4) 0.0468(18) Uani 1 1 d . . . . . H35 H 0.3851 0.3576 0.3618 0.056 Uiso 1 1 calc R . . . . C36 C 0.4301(3) 0.2501(5) 0.4117(3) 0.0382(16) Uani 1 1 d . . . . . H36 H 0.4701 0.2322 0.3863 0.046 Uiso 1 1 calc R . . . . N1 N 0.4790(2) 0.4292(4) 0.5593(3) 0.0329(13) Uani 1 1 d . . . . . N2 N 0.5988(3) 0.3835(4) 0.4363(3) 0.0371(14) Uani 1 1 d . . . . . O1 O 0.6047(2) 0.2479(3) 0.6672(2) 0.0369(11) Uani 1 1 d . . . . . O2 O 0.5560(3) 0.4181(3) 0.3976(2) 0.0473(12) Uani 1 1 d . . . . . O3 O 0.6638(3) 0.3534(3) 0.4245(2) 0.0443(12) Uani 1 1 d . . . . . O4 O 0.5124(3) -0.0072(3) 0.3914(2) 0.0567(14) Uani 1 1 d . . . . . O5 O 0.4558(3) 0.0584(4) 0.5146(2) 0.0549(14) Uani 1 1 d . . . . . C1' C 0.4671(3) 0.7823(5) 0.3142(3) 0.0385(16) Uani 1 1 d . . . . . H1' H 0.4989 0.8346 0.3024 0.046 Uiso 1 1 calc R . . . . C2' C 0.3896(3) 0.7852(5) 0.3029(3) 0.0411(17) Uani 1 1 d . . . . . H2' H 0.3683 0.8399 0.2839 0.049 Uiso 1 1 calc R . . . . C3' C 0.3435(3) 0.7097(5) 0.3188(3) 0.0414(17) Uani 1 1 d . . . . . H3' H 0.2905 0.7110 0.3096 0.050 Uiso 1 1 calc R . . . . C4' C 0.3738(3) 0.6309(5) 0.3487(3) 0.0388(16) Uani 1 1 d . . . . . H4' H 0.3416 0.5789 0.3603 0.047 Uiso 1 1 calc R . . . . C5' C 0.4521(3) 0.6292(4) 0.3612(3) 0.0328(15) Uani 1 1 d . . . . . H5' H 0.4732 0.5769 0.3825 0.039 Uiso 1 1 calc R . . . . C6' C 0.4989(3) 0.7041(4) 0.3425(3) 0.0274(14) Uani 1 1 d . . . . . C7' C 0.5838(3) 0.7031(4) 0.3510(3) 0.0276(14) Uani 1 1 d . . . . . C8' C 0.6176(3) 0.6407(4) 0.3985(3) 0.0250(13) Uani 1 1 d . . . . . H8' H 0.5939 0.5745 0.3967 0.030 Uiso 1 1 calc R . . . . C9' C 0.7044(3) 0.6305(4) 0.3920(3) 0.0258(13) Uani 1 1 d . . . . . H9' H 0.7280 0.6964 0.3880 0.031 Uiso 1 1 calc R . . . . C10' C 0.7331(3) 0.5647(4) 0.3440(3) 0.0257(13) Uani 1 1 d . . . . . C11' C 0.7144(3) 0.5656(4) 0.2868(3) 0.0325(15) Uani 1 1 d . . . . . H11' H 0.6771 0.6097 0.2726 0.039 Uiso 1 1 calc R . . . . C12' C 0.7510(3) 0.5011(4) 0.2504(3) 0.0345(15) Uani 1 1 d . . . . . H12' H 0.7384 0.5007 0.2110 0.041 Uiso 1 1 calc R . . . . C13' C 0.8056(3) 0.4374(5) 0.2710(3) 0.0395(17) Uani 1 1 d . . . . . H13' H 0.8303 0.3936 0.2456 0.047 Uiso 1 1 calc R . . . . C14' C 0.8247(3) 0.4369(5) 0.3281(3) 0.0371(16) Uani 1 1 d . . . . . H14' H 0.8621 0.3929 0.3423 0.045 Uiso 1 1 calc R . . . . C15' C 0.7884(3) 0.5016(4) 0.3643(3) 0.0313(15) Uani 1 1 d . . . . . C16' C 0.8003(3) 0.5137(5) 0.4275(3) 0.0370(16) Uani 1 1 d . . . . . H16C H 0.7955 0.4509 0.4478 0.044 Uiso 1 1 calc R . . . . H16D H 0.8510 0.5426 0.4359 0.044 Uiso 1 1 calc R . . . . C17' C 0.7052(3) 0.5848(4) 0.4938(3) 0.0299(15) Uani 1 1 d . . . . . H17' H 0.7284 0.5515 0.5248 0.036 Uiso 1 1 calc R . . . . C18' C 0.6399(3) 0.6353(4) 0.5029(3) 0.0273(14) Uani 1 1 d . . . . . C19' C 0.5966(3) 0.6883(4) 0.4573(3) 0.0253(13) Uani 1 1 d . . . . . H19' H 0.5406 0.6788 0.4641 0.030 Uiso 1 1 calc R . . . . C20' C 0.6135(3) 0.7997(4) 0.4567(3) 0.0308(15) Uani 1 1 d . . . . . H20C H 0.6650 0.8099 0.4401 0.037 Uiso 1 1 calc R . . . . H20D H 0.5761 0.8314 0.4309 0.037 Uiso 1 1 calc R . . . . C21' C 0.6104(3) 0.8497(4) 0.5132(3) 0.0282(14) Uani 1 1 d . . . . . H21' H 0.5621 0.8542 0.5316 0.034 Uiso 1 1 calc R . . . . C22' C 0.6705(3) 0.8883(4) 0.5397(3) 0.0282(15) Uani 1 1 d . . . . . C23' C 0.6649(3) 0.9494(4) 0.5917(3) 0.0318(15) Uani 1 1 d . . . . . C24' C 0.6028(3) 0.9307(4) 0.6347(3) 0.0301(15) Uani 1 1 d . . . . . C25' C 0.5798(3) 0.8371(5) 0.6475(3) 0.0364(16) Uani 1 1 d . . . . . H25' H 0.6011 0.7838 0.6271 0.044 Uiso 1 1 calc R . . . . C26' C 0.5263(4) 0.8203(5) 0.6896(3) 0.0448(18) Uani 1 1 d . . . . . H26' H 0.5119 0.7557 0.6989 0.054 Uiso 1 1 calc R . . . . C27' C 0.4937(4) 0.8975(6) 0.7181(3) 0.0465(19) Uani 1 1 d . . . . . H27' H 0.4552 0.8861 0.7460 0.056 Uiso 1 1 calc R . . . . C28' C 0.5167(4) 0.9913(6) 0.7063(3) 0.0451(18) Uani 1 1 d . . . . . H28' H 0.4953 1.0442 0.7269 0.054 Uiso 1 1 calc R . . . . C29' C 0.5708(3) 1.0083(5) 0.6644(3) 0.0382(16) Uani 1 1 d . . . . . H29' H 0.5862 1.0730 0.6560 0.046 Uiso 1 1 calc R . . . . C30' C 0.7493(3) 0.8810(4) 0.5127(3) 0.0295(14) Uani 1 1 d . . . . . C31' C 0.7990(3) 0.7996(4) 0.5325(3) 0.0290(14) Uani 1 1 d . . . . . C32' C 0.8569(3) 0.7656(5) 0.4959(3) 0.0356(16) Uani 1 1 d . . . . . H32' H 0.8648 0.7958 0.4599 0.043 Uiso 1 1 calc R . . . . C33' C 0.9019(3) 0.6888(5) 0.5122(3) 0.0398(18) Uani 1 1 d . . . . . H33' H 0.9394 0.6641 0.4866 0.048 Uiso 1 1 calc R . . . . C34' C 0.8932(3) 0.6469(5) 0.5656(3) 0.0408(17) Uani 1 1 d . . . . . H34' H 0.9262 0.5956 0.5771 0.049 Uiso 1 1 calc R . . . . C35' C 0.8364(3) 0.6797(4) 0.6023(3) 0.0386(16) Uani 1 1 d . . . . . H35' H 0.8299 0.6503 0.6387 0.046 Uiso 1 1 calc R . . . . C36' C 0.7893(3) 0.7553(4) 0.5856(3) 0.0320(15) Uani 1 1 d . . . . . H36' H 0.7501 0.7773 0.6105 0.038 Uiso 1 1 calc R . . . . N1' N 0.7375(3) 0.5806(3) 0.4427(2) 0.0302(12) Uani 1 1 d . . . . . N2' N 0.6085(3) 0.6320(3) 0.5582(2) 0.0314(13) Uani 1 1 d . . . . . O1' O 0.6256(2) 0.7565(3) 0.32254(19) 0.0357(11) Uani 1 1 d . . . . . O2' O 0.6464(2) 0.5993(3) 0.5993(2) 0.0380(11) Uani 1 1 d . . . . . O3' O 0.5413(2) 0.6630(3) 0.56540(19) 0.0369(11) Uani 1 1 d . . . . . O4' O 0.7111(2) 1.0153(3) 0.5990(2) 0.0440(12) Uani 1 1 d . . . . . O5' O 0.7692(2) 0.9360(3) 0.4745(2) 0.0495(13) Uani 1 1 d . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.035(3) 0.026(3) 0.041(4) 0.003(3) -0.010(3) -0.003(3) C2 0.033(3) 0.037(4) 0.052(5) -0.002(3) -0.002(3) -0.007(3) C3 0.025(3) 0.043(4) 0.044(4) -0.008(3) -0.002(3) 0.001(3) C4 0.033(3) 0.038(4) 0.042(4) 0.004(3) 0.001(3) 0.010(3) C5 0.037(3) 0.029(3) 0.047(4) 0.007(3) 0.001(3) 0.005(3) C6 0.028(3) 0.031(3) 0.031(4) 0.002(3) -0.004(3) 0.000(3) C7 0.033(3) 0.022(3) 0.036(4) 0.001(3) -0.003(3) -0.001(3) C8 0.021(3) 0.024(3) 0.042(4) 0.003(3) -0.005(3) -0.002(2) C9 0.029(3) 0.022(3) 0.046(4) 0.007(3) -0.009(3) -0.004(2) C10 0.030(3) 0.028(3) 0.041(5) 0.006(3) 0.006(3) 0.001(3) C11 0.038(3) 0.033(4) 0.042(5) 0.004(3) 0.004(3) 0.000(3) C12 0.056(4) 0.034(4) 0.045(5) 0.007(4) 0.004(3) 0.008(3) C13 0.045(4) 0.032(4) 0.053(5) 0.005(4) 0.015(4) 0.008(3) C14 0.035(3) 0.034(4) 0.056(5) 0.007(4) 0.009(3) 0.013(3) C15 0.025(3) 0.028(3) 0.055(5) 0.005(3) 0.003(3) -0.002(3) C16 0.026(3) 0.036(4) 0.064(5) 0.004(4) -0.006(3) 0.001(3) C17 0.031(3) 0.023(3) 0.042(5) 0.004(3) -0.014(3) -0.002(3) C18 0.039(3) 0.022(3) 0.038(4) 0.000(3) -0.007(3) -0.010(3) C19 0.029(3) 0.026(3) 0.039(4) 0.004(3) -0.005(3) -0.004(3) C20 0.032(3) 0.026(3) 0.041(4) 0.000(3) -0.006(3) -0.004(3) C21 0.033(3) 0.021(3) 0.044(4) 0.005(3) -0.005(3) -0.003(3) C22 0.029(3) 0.027(3) 0.042(4) 0.001(3) -0.012(3) 0.000(3) C23 0.041(4) 0.024(4) 0.058(5) 0.003(4) -0.014(3) 0.005(3) C24 0.039(3) 0.032(4) 0.047(5) -0.003(4) -0.018(3) 0.004(3) C25 0.068(5) 0.040(4) 0.043(5) -0.002(4) -0.010(4) 0.011(4) C26 0.075(5) 0.065(6) 0.046(6) -0.006(5) -0.014(4) 0.028(5) C27 0.054(5) 0.090(7) 0.050(6) 0.005(5) -0.005(4) 0.005(5) C28 0.059(5) 0.064(5) 0.054(5) -0.001(5) -0.008(4) -0.015(4) C29 0.050(4) 0.039(4) 0.054(5) -0.002(4) -0.012(4) -0.009(3) C30 0.038(3) 0.032(4) 0.045(5) 0.002(4) -0.007(3) -0.011(3) C31 0.027(3) 0.031(4) 0.047(5) -0.002(3) -0.008(3) -0.005(3) C32 0.025(3) 0.055(5) 0.059(5) -0.007(4) -0.006(3) -0.007(3) C33 0.024(3) 0.062(5) 0.080(7) -0.024(5) -0.005(4) -0.007(3) C34 0.041(4) 0.036(4) 0.082(7) -0.010(4) -0.016(4) 0.002(3) C35 0.039(4) 0.036(4) 0.066(5) -0.001(4) -0.013(4) 0.001(3) C36 0.035(3) 0.032(4) 0.048(5) -0.008(3) -0.007(3) -0.002(3) N1 0.024(2) 0.030(3) 0.045(4) 0.003(3) -0.008(2) 0.001(2) N2 0.048(3) 0.025(3) 0.039(4) 0.005(3) -0.009(3) -0.011(2) O1 0.036(2) 0.027(2) 0.048(3) 0.005(2) -0.002(2) 0.001(2) O2 0.066(3) 0.039(3) 0.036(3) 0.007(2) -0.015(2) -0.011(2) O3 0.045(3) 0.039(3) 0.048(3) 0.003(2) 0.005(2) -0.007(2) O4 0.056(3) 0.041(3) 0.073(4) -0.014(3) -0.012(3) -0.012(2) O5 0.048(3) 0.050(3) 0.066(4) 0.023(3) -0.009(3) -0.014(2) C1' 0.037(3) 0.033(4) 0.046(5) -0.003(3) -0.005(3) 0.004(3) C2' 0.033(3) 0.041(4) 0.049(5) -0.003(4) -0.010(3) 0.013(3) C3' 0.027(3) 0.052(4) 0.045(5) -0.014(4) -0.008(3) 0.011(3) C4' 0.026(3) 0.048(4) 0.042(4) -0.005(4) -0.001(3) -0.002(3) C5' 0.026(3) 0.036(4) 0.036(4) -0.002(3) -0.002(3) 0.002(3) C6' 0.027(3) 0.028(3) 0.027(4) -0.003(3) -0.003(2) 0.003(3) C7' 0.031(3) 0.018(3) 0.034(4) -0.005(3) -0.003(3) 0.001(2) C8' 0.024(3) 0.019(3) 0.033(4) 0.004(3) -0.001(3) 0.000(2) C9' 0.019(2) 0.031(3) 0.028(4) 0.004(3) -0.002(2) 0.000(2) C10' 0.018(3) 0.023(3) 0.035(4) -0.001(3) -0.001(3) 0.000(2) C11' 0.028(3) 0.034(4) 0.036(4) 0.000(3) 0.000(3) -0.003(3) C12' 0.031(3) 0.039(4) 0.034(4) -0.004(3) 0.000(3) 0.000(3) C13' 0.040(4) 0.035(4) 0.043(5) -0.002(3) 0.011(3) 0.005(3) C14' 0.034(3) 0.031(4) 0.046(5) 0.003(3) 0.005(3) 0.010(3) C15' 0.025(3) 0.028(3) 0.041(4) 0.002(3) -0.001(3) 0.002(3) C16' 0.027(3) 0.038(4) 0.047(5) -0.002(3) -0.002(3) 0.012(3) C17' 0.030(3) 0.023(3) 0.036(4) 0.001(3) -0.005(3) -0.004(2) C18' 0.029(3) 0.022(3) 0.030(4) 0.002(3) 0.001(3) -0.004(2) C19' 0.022(3) 0.023(3) 0.031(4) -0.002(3) -0.002(2) -0.002(2) C20' 0.037(3) 0.023(3) 0.033(4) 0.001(3) 0.000(3) 0.002(3) C21' 0.027(3) 0.024(3) 0.034(4) -0.001(3) 0.001(3) 0.003(2) C22' 0.023(3) 0.018(3) 0.043(4) 0.000(3) 0.001(3) -0.001(2) C23' 0.029(3) 0.027(3) 0.039(4) 0.000(3) -0.004(3) -0.006(3) C24' 0.029(3) 0.027(3) 0.034(4) -0.002(3) -0.002(3) 0.000(3) C25' 0.036(3) 0.037(4) 0.036(4) -0.005(3) -0.002(3) -0.006(3) C26' 0.046(4) 0.043(4) 0.046(5) 0.001(4) 0.004(3) -0.017(3) C27' 0.033(4) 0.069(6) 0.037(5) -0.004(4) 0.003(3) -0.003(4) C28' 0.037(4) 0.049(5) 0.049(5) -0.005(4) 0.000(3) 0.016(3) C29' 0.039(3) 0.033(4) 0.042(4) -0.004(3) -0.006(3) 0.004(3) C30' 0.026(3) 0.029(3) 0.034(4) -0.002(3) -0.003(3) 0.000(3) C31' 0.023(3) 0.025(3) 0.040(4) -0.004(3) 0.000(3) -0.006(2) C32' 0.026(3) 0.039(4) 0.042(4) -0.001(3) 0.006(3) -0.004(3) C33' 0.016(3) 0.049(4) 0.055(5) -0.011(4) 0.002(3) 0.005(3) C34' 0.025(3) 0.040(4) 0.057(5) -0.001(4) -0.004(3) 0.003(3) C35' 0.037(3) 0.031(4) 0.047(5) 0.005(3) 0.000(3) -0.001(3) C36' 0.034(3) 0.024(3) 0.039(4) 0.002(3) 0.000(3) -0.003(3) N1' 0.028(2) 0.029(3) 0.033(3) 0.001(3) -0.008(2) 0.004(2) N2' 0.034(3) 0.022(3) 0.039(4) 0.000(3) -0.002(3) -0.007(2) O1' 0.037(2) 0.030(2) 0.039(3) 0.006(2) 0.0012(19) -0.001(2) O2' 0.048(2) 0.029(2) 0.037(3) 0.006(2) -0.006(2) -0.0020(19) O3' 0.031(2) 0.035(2) 0.045(3) 0.001(2) 0.006(2) -0.0025(18) O4' 0.044(2) 0.040(3) 0.049(3) -0.006(2) 0.002(2) -0.020(2) O5' 0.042(2) 0.045(3) 0.062(4) 0.022(3) 0.007(2) -0.002(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 H1 0.9500 . ? C1 C2 1.396(8) . ? C1 C6 1.398(8) . ? C2 H2 0.9500 . ? C2 C3 1.382(9) . ? C3 H3 0.9500 . ? C3 C4 1.358(9) . ? C4 H4 0.9500 . ? C4 C5 1.386(9) . ? C5 H5 0.9500 . ? C5 C6 1.399(8) . ? C6 C7 1.481(8) . ? C7 C8 1.510(8) . ? C7 O1 1.240(7) . ? C8 H8 1.0000 . ? C8 C9 1.535(8) . ? C8 C19 1.553(9) . ? C9 H9 1.0000 . ? C9 C10 1.524(9) . ? C9 N1 1.466(8) . ? C10 C11 1.378(10) . ? C10 C15 1.393(8) . ? C11 H11 0.9500 . ? C11 C12 1.381(9) . ? C12 H12 0.9500 . ? C12 C13 1.380(9) . ? C13 H13 0.9500 . ? C13 C14 1.382(10) . ? C14 H14 0.9500 . ? C14 C15 1.388(9) . ? C15 C16 1.504(10) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C16 N1 1.472(8) . ? C17 H17 0.9500 . ? C17 C18 1.372(9) . ? C17 N1 1.317(9) . ? C18 C19 1.502(9) . ? C18 N2 1.392(9) . ? C19 H19 1.0000 . ? C19 C20 1.551(9) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C20 C21 1.498(10) . ? C21 H21 0.9500 . ? C21 C22 1.338(8) . ? C22 C23 1.499(10) . ? C22 C30 1.507(9) . ? C23 C24 1.475(10) . ? C23 O4 1.242(7) . ? C24 C25 1.400(9) . ? C24 C29 1.392(9) . ? C25 H25 0.9500 . ? C25 C26 1.385(11) . ? C26 H26 0.9500 . ? C26 C27 1.380(11) . ? C27 H27 0.9500 . ? C27 C28 1.385(12) . ? C28 H28 0.9500 . ? C28 C29 1.396(10) . ? C29 H29 0.9500 . ? C30 C31 1.491(9) . ? C30 O5 1.221(8) . ? C31 C32 1.391(9) . ? C31 C36 1.395(10) . ? C32 H32 0.9500 . ? C32 C33 1.372(10) . ? C33 H33 0.9500 . ? C33 C34 1.383(11) . ? C34 H34 0.9500 . ? C34 C35 1.378(10) . ? C35 H35 0.9500 . ? C35 C36 1.392(9) . ? C36 H36 0.9500 . ? N2 O2 1.268(7) . ? N2 O3 1.239(7) . ? C1' H1' 0.9500 . ? C1' C2' 1.379(8) . ? C1' C6' 1.379(8) . ? C2' H2' 0.9500 . ? C2' C3' 1.366(9) . ? C3' H3' 0.9500 . ? C3' C4' 1.394(9) . ? C4' H4' 0.9500 . ? C4' C5' 1.398(8) . ? C5' H5' 0.9500 . ? C5' C6' 1.386(8) . ? C6' C7' 1.496(8) . ? C7' C8' 1.525(8) . ? C7' O1' 1.231(7) . ? C8' H8' 1.0000 . ? C8' C9' 1.530(7) . ? C8' C19' 1.567(9) . ? C9' H9' 1.0000 . ? C9' C10' 1.525(9) . ? C9' N1' 1.489(8) . ? C10' C11' 1.379(9) . ? C10' C15' 1.382(8) . ? C11' H11' 0.9500 . ? C11' C12' 1.387(9) . ? C12' H12' 0.9500 . ? C12' C13' 1.382(9) . ? C13' H13' 0.9500 . ? C13' C14' 1.378(10) . ? C14' H14' 0.9500 . ? C14' C15' 1.384(9) . ? C15' C16' 1.504(10) . ? C16' H16C 0.9900 . ? C16' H16D 0.9900 . ? C16' N1' 1.476(7) . ? C17' H17' 0.9500 . ? C17' C18' 1.351(8) . ? C17' N1' 1.322(8) . ? C18' C19' 1.498(8) . ? C18' N2' 1.408(8) . ? C19' H19' 1.0000 . ? C19' C20' 1.560(8) . ? C20' H20C 0.9900 . ? C20' H20D 0.9900 . ? C20' C21' 1.493(9) . ? C21' H21' 0.9500 . ? C21' C22' 1.329(8) . ? C22' C23' 1.484(9) . ? C22' C30' 1.517(8) . ? C23' C24' 1.502(9) . ? C23' O4' 1.226(7) . ? C24' C25' 1.381(8) . ? C24' C29' 1.393(9) . ? C25' H25' 0.9500 . ? C25' C26' 1.378(9) . ? C26' H26' 0.9500 . ? C26' C27' 1.377(10) . ? C27' H27' 0.9500 . ? C27' C28' 1.379(11) . ? C28' H28' 0.9500 . ? C28' C29' 1.381(10) . ? C29' H29' 0.9500 . ? C30' C31' 1.491(8) . ? C30' O5' 1.221(8) . ? C31' C32' 1.407(8) . ? C31' C36' 1.395(9) . ? C32' H32' 0.9500 . ? C32' C33' 1.371(9) . ? C33' H33' 0.9500 . ? C33' C34' 1.386(10) . ? C34' H34' 0.9500 . ? C34' C35' 1.388(9) . ? C35' H35' 0.9500 . ? C35' C36' 1.382(8) . ? C36' H36' 0.9500 . ? N2' O2' 1.251(7) . ? N2' O3' 1.260(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 H1 120.1 . . ? C2 C1 C6 119.8(6) . . ? C6 C1 H1 120.1 . . ? C1 C2 H2 120.2 . . ? C3 C2 C1 119.6(6) . . ? C3 C2 H2 120.2 . . ? C2 C3 H3 119.5 . . ? C4 C3 C2 120.9(6) . . ? C4 C3 H3 119.5 . . ? C3 C4 H4 119.7 . . ? C3 C4 C5 120.6(6) . . ? C5 C4 H4 119.7 . . ? C4 C5 H5 120.1 . . ? C4 C5 C6 119.8(6) . . ? C6 C5 H5 120.1 . . ? C1 C6 C5 119.2(5) . . ? C1 C6 C7 122.7(5) . . ? C5 C6 C7 118.1(5) . . ? C6 C7 C8 119.0(5) . . ? O1 C7 C6 120.3(5) . . ? O1 C7 C8 120.5(5) . . ? C7 C8 H8 108.3 . . ? C7 C8 C9 110.9(5) . . ? C7 C8 C19 108.4(5) . . ? C9 C8 H8 108.3 . . ? C9 C8 C19 112.6(5) . . ? C19 C8 H8 108.3 . . ? C8 C9 H9 109.2 . . ? C10 C9 C8 116.7(5) . . ? C10 C9 H9 109.2 . . ? N1 C9 C8 110.9(5) . . ? N1 C9 H9 109.2 . . ? N1 C9 C10 101.2(5) . . ? C11 C10 C9 130.4(6) . . ? C11 C10 C15 119.9(6) . . ? C15 C10 C9 109.7(6) . . ? C10 C11 H11 120.3 . . ? C10 C11 C12 119.4(6) . . ? C12 C11 H11 120.3 . . ? C11 C12 H12 119.5 . . ? C13 C12 C11 120.9(7) . . ? C13 C12 H12 119.5 . . ? C12 C13 H13 119.9 . . ? C12 C13 C14 120.2(7) . . ? C14 C13 H13 119.9 . . ? C13 C14 H14 120.5 . . ? C13 C14 C15 119.0(6) . . ? C15 C14 H14 120.5 . . ? C10 C15 C16 111.4(6) . . ? C14 C15 C10 120.5(7) . . ? C14 C15 C16 128.1(6) . . ? C15 C16 H16A 111.6 . . ? C15 C16 H16B 111.6 . . ? H16A C16 H16B 109.4 . . ? N1 C16 C15 101.0(5) . . ? N1 C16 H16A 111.6 . . ? N1 C16 H16B 111.6 . . ? C18 C17 H17 118.2 . . ? N1 C17 H17 118.2 . . ? N1 C17 C18 123.5(6) . . ? C17 C18 C19 122.4(6) . . ? C17 C18 N2 119.1(6) . . ? N2 C18 C19 118.3(6) . . ? C8 C19 H19 108.3 . . ? C18 C19 C8 107.4(5) . . ? C18 C19 H19 108.3 . . ? C18 C19 C20 112.7(5) . . ? C20 C19 C8 111.7(5) . . ? C20 C19 H19 108.3 . . ? C19 C20 H20A 108.4 . . ? C19 C20 H20B 108.4 . . ? H20A C20 H20B 107.4 . . ? C21 C20 C19 115.7(5) . . ? C21 C20 H20A 108.4 . . ? C21 C20 H20B 108.4 . . ? C20 C21 H21 117.8 . . ? C22 C21 C20 124.4(6) . . ? C22 C21 H21 117.8 . . ? C21 C22 C23 124.3(6) . . ? C21 C22 C30 119.8(6) . . ? C23 C22 C30 115.7(5) . . ? C24 C23 C22 121.9(6) . . ? O4 C23 C22 117.7(6) . . ? O4 C23 C24 120.3(7) . . ? C25 C24 C23 118.2(6) . . ? C29 C24 C23 121.9(6) . . ? C29 C24 C25 119.7(7) . . ? C24 C25 H25 120.2 . . ? C26 C25 C24 119.6(7) . . ? C26 C25 H25 120.2 . . ? C25 C26 H26 119.7 . . ? C27 C26 C25 120.7(8) . . ? C27 C26 H26 119.7 . . ? C26 C27 H27 119.9 . . ? C26 C27 C28 120.1(8) . . ? C28 C27 H27 119.9 . . ? C27 C28 H28 120.0 . . ? C27 C28 C29 120.0(8) . . ? C29 C28 H28 120.0 . . ? C24 C29 C28 119.9(7) . . ? C24 C29 H29 120.1 . . ? C28 C29 H29 120.1 . . ? C31 C30 C22 117.1(6) . . ? O5 C30 C22 120.9(6) . . ? O5 C30 C31 121.9(6) . . ? C32 C31 C30 119.8(7) . . ? C32 C31 C36 119.5(6) . . ? C36 C31 C30 120.7(6) . . ? C31 C32 H32 119.9 . . ? C33 C32 C31 120.2(8) . . ? C33 C32 H32 119.9 . . ? C32 C33 H33 119.9 . . ? C32 C33 C34 120.1(7) . . ? C34 C33 H33 119.9 . . ? C33 C34 H34 119.7 . . ? C35 C34 C33 120.7(7) . . ? C35 C34 H34 119.7 . . ? C34 C35 H35 120.2 . . ? C34 C35 C36 119.5(8) . . ? C36 C35 H35 120.2 . . ? C31 C36 H36 120.1 . . ? C35 C36 C31 119.9(6) . . ? C35 C36 H36 120.1 . . ? C9 N1 C16 113.4(6) . . ? C17 N1 C9 121.7(5) . . ? C17 N1 C16 123.6(5) . . ? O2 N2 C18 120.0(6) . . ? O3 N2 C18 119.7(6) . . ? O3 N2 O2 120.3(6) . . ? C2' C1' H1' 119.7 . . ? C2' C1' C6' 120.6(6) . . ? C6' C1' H1' 119.7 . . ? C1' C2' H2' 119.9 . . ? C3' C2' C1' 120.2(6) . . ? C3' C2' H2' 119.9 . . ? C2' C3' H3' 119.9 . . ? C2' C3' C4' 120.3(6) . . ? C4' C3' H3' 119.9 . . ? C3' C4' H4' 120.4 . . ? C3' C4' C5' 119.3(6) . . ? C5' C4' H4' 120.4 . . ? C4' C5' H5' 120.1 . . ? C6' C5' C4' 119.8(6) . . ? C6' C5' H5' 120.1 . . ? C1' C6' C5' 119.6(5) . . ? C1' C6' C7' 118.1(5) . . ? C5' C6' C7' 122.3(5) . . ? C6' C7' C8' 119.1(5) . . ? O1' C7' C6' 120.6(6) . . ? O1' C7' C8' 120.2(5) . . ? C7' C8' H8' 108.8 . . ? C7' C8' C9' 111.2(5) . . ? C7' C8' C19' 108.4(5) . . ? C9' C8' H8' 108.8 . . ? C9' C8' C19' 111.0(5) . . ? C19' C8' H8' 108.8 . . ? C8' C9' H9' 109.5 . . ? C10' C9' C8' 116.9(5) . . ? C10' C9' H9' 109.5 . . ? N1' C9' C8' 110.2(5) . . ? N1' C9' H9' 109.5 . . ? N1' C9' C10' 100.8(5) . . ? C11' C10' C9' 129.2(5) . . ? C11' C10' C15' 120.3(6) . . ? C15' C10' C9' 110.4(6) . . ? C10' C11' H11' 120.6 . . ? C10' C11' C12' 118.9(6) . . ? C12' C11' H11' 120.6 . . ? C11' C12' H12' 119.7 . . ? C13' C12' C11' 120.6(7) . . ? C13' C12' H12' 119.7 . . ? C12' C13' H13' 119.7 . . ? C14' C13' C12' 120.6(6) . . ? C14' C13' H13' 119.7 . . ? C13' C14' H14' 120.7 . . ? C13' C14' C15' 118.7(6) . . ? C15' C14' H14' 120.7 . . ? C10' C15' C14' 120.9(6) . . ? C10' C15' C16' 111.4(5) . . ? C14' C15' C16' 127.6(6) . . ? C15' C16' H16C 111.4 . . ? C15' C16' H16D 111.4 . . ? H16C C16' H16D 109.3 . . ? N1' C16' C15' 101.8(5) . . ? N1' C16' H16C 111.4 . . ? N1' C16' H16D 111.4 . . ? C18' C17' H17' 119.2 . . ? N1' C17' H17' 119.2 . . ? N1' C17' C18' 121.7(6) . . ? C17' C18' C19' 124.2(6) . . ? C17' C18' N2' 117.2(6) . . ? N2' C18' C19' 118.5(5) . . ? C8' C19' H19' 108.3 . . ? C18' C19' C8' 107.8(5) . . ? C18' C19' H19' 108.3 . . ? C18' C19' C20' 112.9(5) . . ? C20' C19' C8' 111.0(5) . . ? C20' C19' H19' 108.3 . . ? C19' C20' H20C 108.3 . . ? C19' C20' H20D 108.3 . . ? H20C C20' H20D 107.4 . . ? C21' C20' C19' 115.9(5) . . ? C21' C20' H20C 108.3 . . ? C21' C20' H20D 108.3 . . ? C20' C21' H21' 117.6 . . ? C22' C21' C20' 124.7(5) . . ? C22' C21' H21' 117.6 . . ? C21' C22' C23' 123.9(5) . . ? C21' C22' C30' 119.6(6) . . ? C23' C22' C30' 116.1(5) . . ? C22' C23' C24' 120.1(5) . . ? O4' C23' C22' 119.3(6) . . ? O4' C23' C24' 120.6(6) . . ? C25' C24' C23' 121.0(6) . . ? C25' C24' C29' 119.4(6) . . ? C29' C24' C23' 119.6(5) . . ? C24' C25' H25' 119.7 . . ? C26' C25' C24' 120.5(6) . . ? C26' C25' H25' 119.7 . . ? C25' C26' H26' 120.1 . . ? C27' C26' C25' 119.9(7) . . ? C27' C26' H26' 120.1 . . ? C26' C27' H27' 119.9 . . ? C26' C27' C28' 120.3(7) . . ? C28' C27' H27' 119.9 . . ? C27' C28' H28' 120.0 . . ? C27' C28' C29' 120.0(7) . . ? C29' C28' H28' 120.0 . . ? C24' C29' H29' 120.0 . . ? C28' C29' C24' 119.9(6) . . ? C28' C29' H29' 120.0 . . ? C31' C30' C22' 116.6(5) . . ? O5' C30' C22' 121.4(5) . . ? O5' C30' C31' 121.9(5) . . ? C32' C31' C30' 118.5(6) . . ? C36' C31' C30' 122.4(6) . . ? C36' C31' C32' 119.1(6) . . ? C31' C32' H32' 120.1 . . ? C33' C32' C31' 119.9(6) . . ? C33' C32' H32' 120.1 . . ? C32' C33' H33' 119.7 . . ? C32' C33' C34' 120.6(6) . . ? C34' C33' H33' 119.7 . . ? C33' C34' H34' 119.9 . . ? C33' C34' C35' 120.2(6) . . ? C35' C34' H34' 119.9 . . ? C34' C35' H35' 120.2 . . ? C36' C35' C34' 119.6(7) . . ? C36' C35' H35' 120.2 . . ? C31' C36' H36' 119.7 . . ? C35' C36' C31' 120.6(6) . . ? C35' C36' H36' 119.7 . . ? C16' N1' C9' 112.4(5) . . ? C17' N1' C9' 122.4(5) . . ? C17' N1' C16' 124.3(5) . . ? O2' N2' C18' 121.0(5) . . ? O2' N2' O3' 120.7(5) . . ? O3' N2' C18' 118.3(5) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 C2 C3 C4 -0.2(11) . . . . ? C1 C6 C7 C8 32.1(9) . . . . ? C1 C6 C7 O1 -153.3(6) . . . . ? C2 C1 C6 C5 -0.7(10) . . . . ? C2 C1 C6 C7 178.7(6) . . . . ? C2 C3 C4 C5 -0.4(11) . . . . ? C3 C4 C5 C6 0.5(10) . . . . ? C4 C5 C6 C1 0.0(10) . . . . ? C4 C5 C6 C7 -179.4(6) . . . . ? C5 C6 C7 C8 -148.5(6) . . . . ? C5 C6 C7 O1 26.1(9) . . . . ? C6 C1 C2 C3 0.8(11) . . . . ? C6 C7 C8 C9 -160.4(5) . . . . ? C6 C7 C8 C19 75.5(6) . . . . ? C7 C8 C9 C10 72.7(7) . . . . ? C7 C8 C9 N1 -172.2(5) . . . . ? C7 C8 C19 C18 171.9(5) . . . . ? C7 C8 C19 C20 47.9(6) . . . . ? C8 C9 C10 C11 -49.3(9) . . . . ? C8 C9 C10 C15 130.9(5) . . . . ? C8 C9 N1 C16 -142.6(5) . . . . ? C8 C9 N1 C17 24.8(7) . . . . ? C8 C19 C20 C21 173.6(5) . . . . ? C9 C8 C19 C18 48.8(6) . . . . ? C9 C8 C19 C20 -75.2(6) . . . . ? C9 C10 C11 C12 179.0(6) . . . . ? C9 C10 C15 C14 -180.0(5) . . . . ? C9 C10 C15 C16 0.1(7) . . . . ? C10 C9 N1 C16 -18.1(6) . . . . ? C10 C9 N1 C17 149.3(5) . . . . ? C10 C11 C12 C13 1.7(10) . . . . ? C10 C15 C16 N1 -10.6(6) . . . . ? C11 C10 C15 C14 0.1(9) . . . . ? C11 C10 C15 C16 -179.8(6) . . . . ? C11 C12 C13 C14 -1.4(10) . . . . ? C12 C13 C14 C15 0.4(10) . . . . ? C13 C14 C15 C10 0.2(9) . . . . ? C13 C14 C15 C16 -179.9(6) . . . . ? C14 C15 C16 N1 169.5(6) . . . . ? C15 C10 C11 C12 -1.1(9) . . . . ? C15 C16 N1 C9 18.1(6) . . . . ? C15 C16 N1 C17 -149.0(5) . . . . ? C17 C18 C19 C8 -24.0(7) . . . . ? C17 C18 C19 C20 99.5(7) . . . . ? C17 C18 N2 O2 -12.6(8) . . . . ? C17 C18 N2 O3 168.3(5) . . . . ? C18 C17 N1 C9 1.5(9) . . . . ? C18 C17 N1 C16 167.6(5) . . . . ? C18 C19 C20 C21 52.5(7) . . . . ? C19 C8 C9 C10 -165.6(5) . . . . ? C19 C8 C9 N1 -50.5(6) . . . . ? C19 C18 N2 O2 171.7(5) . . . . ? C19 C18 N2 O3 -7.4(8) . . . . ? C19 C20 C21 C22 -117.5(7) . . . . ? C20 C21 C22 C23 -171.6(6) . . . . ? C20 C21 C22 C30 2.4(9) . . . . ? C21 C22 C23 C24 -26.6(9) . . . . ? C21 C22 C23 O4 152.2(6) . . . . ? C21 C22 C30 C31 91.0(8) . . . . ? C21 C22 C30 O5 -85.7(8) . . . . ? C22 C23 C24 C25 147.6(6) . . . . ? C22 C23 C24 C29 -36.9(9) . . . . ? C22 C30 C31 C32 -153.4(6) . . . . ? C22 C30 C31 C36 23.9(9) . . . . ? C23 C22 C30 C31 -94.6(7) . . . . ? C23 C22 C30 O5 88.8(8) . . . . ? C23 C24 C25 C26 177.2(6) . . . . ? C23 C24 C29 C28 -175.6(6) . . . . ? C24 C25 C26 C27 -1.8(11) . . . . ? C25 C24 C29 C28 -0.2(10) . . . . ? C25 C26 C27 C28 0.5(12) . . . . ? C26 C27 C28 C29 0.9(12) . . . . ? C27 C28 C29 C24 -1.0(11) . . . . ? C29 C24 C25 C26 1.6(10) . . . . ? C30 C22 C23 C24 159.2(6) . . . . ? C30 C22 C23 O4 -21.9(8) . . . . ? C30 C31 C32 C33 177.3(6) . . . . ? C30 C31 C36 C35 -179.7(5) . . . . ? C31 C32 C33 C34 1.5(10) . . . . ? C32 C31 C36 C35 -2.3(9) . . . . ? C32 C33 C34 C35 -0.5(11) . . . . ? C33 C34 C35 C36 -1.8(10) . . . . ? C34 C35 C36 C31 3.2(9) . . . . ? C36 C31 C32 C33 -0.1(9) . . . . ? N1 C9 C10 C11 -169.7(6) . . . . ? N1 C9 C10 C15 10.5(6) . . . . ? N1 C17 C18 C19 -1.5(9) . . . . ? N1 C17 C18 N2 -177.0(5) . . . . ? N2 C18 C19 C8 151.6(5) . . . . ? N2 C18 C19 C20 -84.9(7) . . . . ? O1 C7 C8 C9 25.0(8) . . . . ? O1 C7 C8 C19 -99.1(6) . . . . ? O4 C23 C24 C25 -31.3(9) . . . . ? O4 C23 C24 C29 144.2(6) . . . . ? O5 C30 C31 C32 23.2(9) . . . . ? O5 C30 C31 C36 -159.4(6) . . . . ? C1' C2' C3' C4' 2.5(10) . . . . ? C1' C6' C7' C8' 158.3(6) . . . . ? C1' C6' C7' O1' -17.0(9) . . . . ? C2' C1' C6' C5' -2.0(10) . . . . ? C2' C1' C6' C7' 177.1(6) . . . . ? C2' C3' C4' C5' -1.0(10) . . . . ? C3' C4' C5' C6' -2.0(10) . . . . ? C4' C5' C6' C1' 3.4(9) . . . . ? C4' C5' C6' C7' -175.6(6) . . . . ? C5' C6' C7' C8' -22.6(9) . . . . ? C5' C6' C7' O1' 162.0(6) . . . . ? C6' C1' C2' C3' -1.0(10) . . . . ? C6' C7' C8' C9' 166.9(5) . . . . ? C6' C7' C8' C19' -70.9(6) . . . . ? C7' C8' C9' C10' -73.2(6) . . . . ? C7' C8' C9' N1' 172.5(5) . . . . ? C7' C8' C19' C18' -171.5(4) . . . . ? C7' C8' C19' C20' -47.4(6) . . . . ? C8' C9' C10' C11' 52.2(8) . . . . ? C8' C9' C10' C15' -131.8(5) . . . . ? C8' C9' N1' C16' 142.2(5) . . . . ? C8' C9' N1' C17' -27.5(8) . . . . ? C8' C19' C20' C21' -168.5(5) . . . . ? C9' C8' C19' C18' -49.2(6) . . . . ? C9' C8' C19' C20' 75.0(6) . . . . ? C9' C10' C11' C12' 176.8(5) . . . . ? C9' C10' C15' C14' -177.9(5) . . . . ? C9' C10' C15' C16' 2.9(6) . . . . ? C10' C9' N1' C16' 18.1(6) . . . . ? C10' C9' N1' C17' -151.7(5) . . . . ? C10' C11' C12' C13' -0.4(8) . . . . ? C10' C15' C16' N1' 8.1(6) . . . . ? C11' C10' C15' C14' -1.5(8) . . . . ? C11' C10' C15' C16' 179.3(5) . . . . ? C11' C12' C13' C14' 0.0(9) . . . . ? C12' C13' C14' C15' -0.3(9) . . . . ? C13' C14' C15' C10' 1.1(9) . . . . ? C13' C14' C15' C16' -179.9(6) . . . . ? C14' C15' C16' N1' -171.1(6) . . . . ? C15' C10' C11' C12' 1.1(8) . . . . ? C15' C16' N1' C9' -16.7(6) . . . . ? C15' C16' N1' C17' 152.9(5) . . . . ? C17' C18' C19' C8' 23.5(7) . . . . ? C17' C18' C19' C20' -99.4(7) . . . . ? C17' C18' N2' O2' 12.8(8) . . . . ? C17' C18' N2' O3' -167.2(5) . . . . ? C18' C17' N1' C9' -0.2(9) . . . . ? C18' C17' N1' C16' -168.7(5) . . . . ? C18' C19' C20' C21' -47.4(7) . . . . ? C19' C8' C9' C10' 166.1(5) . . . . ? C19' C8' C9' N1' 51.8(6) . . . . ? C19' C18' N2' O2' -171.1(5) . . . . ? C19' C18' N2' O3' 8.8(7) . . . . ? C19' C20' C21' C22' 113.0(7) . . . . ? C20' C21' C22' C23' 171.2(6) . . . . ? C20' C21' C22' C30' -1.4(9) . . . . ? C21' C22' C23' C24' 32.6(9) . . . . ? C21' C22' C23' O4' -147.0(6) . . . . ? C21' C22' C30' C31' -96.1(7) . . . . ? C21' C22' C30' O5' 80.1(8) . . . . ? C22' C23' C24' C25' 37.6(9) . . . . ? C22' C23' C24' C29' -146.1(6) . . . . ? C22' C30' C31' C32' 155.4(5) . . . . ? C22' C30' C31' C36' -23.6(8) . . . . ? C23' C22' C30' C31' 90.7(7) . . . . ? C23' C22' C30' O5' -93.0(7) . . . . ? C23' C24' C25' C26' 175.8(6) . . . . ? C23' C24' C29' C28' -176.4(6) . . . . ? C24' C25' C26' C27' 1.8(10) . . . . ? C25' C24' C29' C28' -0.1(10) . . . . ? C25' C26' C27' C28' -2.6(10) . . . . ? C26' C27' C28' C29' 2.1(10) . . . . ? C27' C28' C29' C24' -0.7(10) . . . . ? C29' C24' C25' C26' -0.5(10) . . . . ? C30' C22' C23' C24' -154.6(5) . . . . ? C30' C22' C23' O4' 25.8(8) . . . . ? C30' C31' C32' C33' -177.9(5) . . . . ? C30' C31' C36' C35' 179.6(5) . . . . ? C31' C32' C33' C34' -2.8(9) . . . . ? C32' C31' C36' C35' 0.6(8) . . . . ? C32' C33' C34' C35' 2.8(10) . . . . ? C33' C34' C35' C36' -1.0(9) . . . . ? C34' C35' C36' C31' -0.7(9) . . . . ? C36' C31' C32' C33' 1.1(8) . . . . ? N1' C9' C10' C11' 171.6(6) . . . . ? N1' C9' C10' C15' -12.4(6) . . . . ? N1' C17' C18' C19' 1.8(9) . . . . ? N1' C17' C18' N2' 177.6(5) . . . . ? N2' C18' C19' C8' -152.2(5) . . . . ? N2' C18' C19' C20' 84.8(6) . . . . ? O1' C7' C8' C9' -17.7(8) . . . . ? O1' C7' C8' C19' 104.5(6) . . . . ? O4' C23' C24' C25' -142.8(6) . . . . ? O4' C23' C24' C29' 33.5(9) . . . . ? O5' C30' C31' C32' -20.9(9) . . . . ? O5' C30' C31' C36' 160.1(6) . . . . ? _shelx_res_file ; m4279_0m.res created by SHELXL-2014/7 TITL m4279_0m_a.res in Pna2(1) REM Old TITL Integration of M4279 REM SHELXT solution in Pna2(1) REM R1 0.185, Rweak 0.034, Alpha 0.004, Orientation a'=b, b'=a, c'=-c REM Flack x = -9.990 ( 9.990 ) from Parsons' quotients REM Formula found by SHELXT: C86 CELL 0.71073 17.4569 13.7547 23.4228 90 90 90 ZERR 8 0.0297 0.0238 0.0553 0 0 0 LATT -1 SYMM -X,-Y,0.5+Z SYMM 0.5+X,0.5-Y,+Z SYMM 0.5-X,0.5+Y,0.5+Z SFAC C H N O UNIT 288 224 16 40 L.S. 4 0 0 PLAN 20 SIZE 0.13 0.1 0.05 TEMP -123.13 MPLA C1 C2 C3 C4 C5 C6 MPLA C9 C17 C18 C19 N1 MPLA C8 C9 C19 MPLA C10 C11 C12 C13 C14 C15 MPLA C24 C25 C26 C27 C28 C29 MPLA C31 C32 C33 C34 C35 C36 MPLA C1' C2' C3' C4' C5' C6' MPLA C9' C17' C18' C19' N1' MPLA C8' C9' C19' MPLA C10' C11' C12' C13' C14' C15' MPLA C24' C25' C26' C27' C28' C29' MPLA C31' C32' C33' C34' C35' C36' list 4 bond $h conf fmap 2 acta SHEL 999 0.8 REM REM REM WGHT 0.065900 EXTI 0.006498 FVAR 0.30243 C1 1 0.767476 0.400420 0.637076 11.00000 0.03521 0.02570 = 0.04121 0.00314 -0.01017 -0.00315 AFIX 43 H1 2 0.741635 0.457329 0.624535 11.00000 -1.20000 AFIX 0 C2 1 0.846606 0.402075 0.645762 11.00000 0.03323 0.03667 = 0.05214 -0.00198 -0.00209 -0.00690 AFIX 43 H2 2 0.874731 0.460267 0.639609 11.00000 -1.20000 AFIX 0 C3 1 0.883768 0.318575 0.663361 11.00000 0.02514 0.04346 = 0.04392 -0.00831 -0.00164 0.00143 AFIX 43 H3 2 0.937629 0.319730 0.669118 11.00000 -1.20000 AFIX 0 C4 1 0.844366 0.234900 0.672538 11.00000 0.03340 0.03832 = 0.04204 0.00387 0.00131 0.00997 AFIX 43 H4 2 0.870975 0.178132 0.684388 11.00000 -1.20000 AFIX 0 C5 1 0.765674 0.231524 0.664779 11.00000 0.03696 0.02870 = 0.04674 0.00665 0.00084 0.00503 AFIX 43 H5 2 0.738497 0.172821 0.671594 11.00000 -1.20000 AFIX 0 C6 1 0.726386 0.314789 0.646886 11.00000 0.02806 0.03145 = 0.03105 0.00172 -0.00423 0.00025 C7 1 0.642245 0.308362 0.639671 11.00000 0.03283 0.02167 = 0.03568 0.00051 -0.00266 -0.00111 C8 1 0.603955 0.370075 0.594657 11.00000 0.02096 0.02361 = 0.04183 0.00348 -0.00504 -0.00217 AFIX 13 H8 2 0.627707 0.436216 0.595547 11.00000 -1.20000 AFIX 0 C9 1 0.518009 0.380879 0.606880 11.00000 0.02922 0.02218 = 0.04600 0.00730 -0.00910 -0.00361 AFIX 13 H9 2 0.495074 0.315008 0.612732 11.00000 -1.20000 AFIX 0 C10 1 0.495749 0.446445 0.656632 11.00000 0.03001 0.02754 = 0.04131 0.00568 0.00600 0.00070 C11 1 0.522448 0.448994 0.711994 11.00000 0.03772 0.03294 = 0.04214 0.00406 0.00379 -0.00025 AFIX 43 H11 2 0.560431 0.404189 0.724297 11.00000 -1.20000 AFIX 0 C12 1 0.493435 0.517336 0.749412 11.00000 0.05584 0.03363 = 0.04497 0.00748 0.00371 0.00845 AFIX 43 H12 2 0.512754 0.520443 0.787285 11.00000 -1.20000 AFIX 0 C13 1 0.436805 0.581138 0.732564 11.00000 0.04452 0.03153 = 0.05276 0.00508 0.01526 0.00764 AFIX 43 H13 2 0.416682 0.626770 0.759060 11.00000 -1.20000 AFIX 0 C14 1 0.409251 0.578886 0.677259 11.00000 0.03497 0.03420 = 0.05627 0.00663 0.00918 0.01269 AFIX 43 H14 2 0.370463 0.622939 0.665424 11.00000 -1.20000 AFIX 0 C15 1 0.439068 0.511341 0.639270 11.00000 0.02493 0.02788 = 0.05460 0.00515 0.00341 -0.00161 C16 1 0.417999 0.496113 0.577660 11.00000 0.02553 0.03562 = 0.06431 0.00388 -0.00598 0.00058 AFIX 23 H16A 2 0.366692 0.466179 0.573762 11.00000 -1.20000 H16B 2 0.419414 0.557827 0.555936 11.00000 -1.20000 AFIX 0 C17 1 0.506701 0.426725 0.506987 11.00000 0.03057 0.02251 = 0.04155 0.00406 -0.01357 -0.00230 AFIX 43 H17 2 0.479769 0.460567 0.477881 11.00000 -1.20000 AFIX 0 C18 1 0.572338 0.377898 0.492287 11.00000 0.03934 0.02179 = 0.03784 0.00007 -0.00665 -0.01047 C19 1 0.620110 0.324145 0.535278 11.00000 0.02854 0.02567 = 0.03892 0.00404 -0.00488 -0.00444 AFIX 13 H19 2 0.675327 0.334823 0.525799 11.00000 -1.20000 AFIX 0 C20 1 0.604458 0.213144 0.535181 11.00000 0.03227 0.02605 = 0.04082 0.00042 -0.00634 -0.00423 AFIX 23 H20A 2 0.641249 0.181697 0.561517 11.00000 -1.20000 H20B 2 0.552412 0.201902 0.550617 11.00000 -1.20000 AFIX 0 C21 1 0.610096 0.164006 0.478245 11.00000 0.03299 0.02077 = 0.04356 0.00509 -0.00466 -0.00282 AFIX 43 H21 2 0.658312 0.164687 0.459442 11.00000 -1.20000 AFIX 0 C22 1 0.551808 0.119245 0.452112 11.00000 0.02926 0.02745 = 0.04176 0.00071 -0.01162 -0.00003 C23 1 0.559658 0.059095 0.399069 11.00000 0.04097 0.02367 = 0.05759 0.00300 -0.01443 0.00549 C24 1 0.621751 0.075660 0.357508 11.00000 0.03908 0.03168 = 0.04670 -0.00252 -0.01830 0.00393 C25 1 0.650727 -0.004542 0.327683 11.00000 0.06779 0.03993 = 0.04268 -0.00169 -0.00962 0.01088 AFIX 43 H25 2 0.632099 -0.068021 0.335599 11.00000 -1.20000 AFIX 0 C26 1 0.706722 0.009243 0.286564 11.00000 0.07518 0.06528 = 0.04571 -0.00551 -0.01356 0.02810 AFIX 43 H26 2 0.727455 -0.045301 0.267062 11.00000 -1.20000 AFIX 0 C27 1 0.732690 0.101446 0.273647 11.00000 0.05366 0.09001 = 0.04985 0.00461 -0.00453 0.00537 AFIX 43 H27 2 0.770795 0.110097 0.245139 11.00000 -1.20000 AFIX 0 C28 1 0.703295 0.181367 0.302172 11.00000 0.05919 0.06362 = 0.05392 -0.00078 -0.00803 -0.01463 AFIX 43 H28 2 0.720721 0.244847 0.292860 11.00000 -1.20000 AFIX 0 C29 1 0.648071 0.168623 0.344598 11.00000 0.04980 0.03911 = 0.05393 -0.00202 -0.01206 -0.00932 AFIX 43 H29 2 0.628478 0.223290 0.364628 11.00000 -1.20000 AFIX 0 C30 1 0.473511 0.119573 0.479167 11.00000 0.03812 0.03240 = 0.04525 0.00169 -0.00717 -0.01134 C31 1 0.420904 0.200559 0.463244 11.00000 0.02697 0.03125 = 0.04692 -0.00184 -0.00774 -0.00529 C32 1 0.363910 0.229740 0.501072 11.00000 0.02487 0.05545 = 0.05872 -0.00693 -0.00600 -0.00679 AFIX 43 H32 2 0.357285 0.196232 0.536192 11.00000 -1.20000 AFIX 0 C33 1 0.317236 0.306785 0.487800 11.00000 0.02448 0.06246 = 0.07973 -0.02405 -0.00452 -0.00670 AFIX 43 H33 2 0.279203 0.327456 0.514147 11.00000 -1.20000 AFIX 0 C34 1 0.325443 0.354383 0.436173 11.00000 0.04101 0.03639 = 0.08191 -0.01014 -0.01639 0.00201 AFIX 43 H34 2 0.292632 0.407294 0.427141 11.00000 -1.20000 AFIX 0 C35 1 0.380740 0.325838 0.397691 11.00000 0.03865 0.03574 = 0.06589 -0.00065 -0.01341 0.00145 AFIX 43 H35 2 0.385117 0.357621 0.361830 11.00000 -1.20000 AFIX 0 C36 1 0.430140 0.250101 0.411738 11.00000 0.03451 0.03224 = 0.04791 -0.00793 -0.00722 -0.00190 AFIX 43 H36 2 0.470088 0.232174 0.386287 11.00000 -1.20000 AFIX 0 N1 3 0.479017 0.429208 0.559282 11.00000 0.02391 0.02951 = 0.04536 0.00286 -0.00784 0.00051 N2 3 0.598776 0.383499 0.436303 11.00000 0.04800 0.02458 = 0.03857 0.00459 -0.00912 -0.01148 O1 4 0.604749 0.247925 0.667246 11.00000 0.03604 0.02677 = 0.04802 0.00519 -0.00219 0.00062 O2 4 0.556017 0.418121 0.397571 11.00000 0.06649 0.03917 = 0.03636 0.00667 -0.01470 -0.01146 O3 4 0.663800 0.353428 0.424502 11.00000 0.04523 0.03936 = 0.04821 0.00317 0.00524 -0.00710 O4 4 0.512427 -0.007168 0.391351 11.00000 0.05551 0.04135 = 0.07310 -0.01421 -0.01247 -0.01218 O5 4 0.455771 0.058407 0.514574 11.00000 0.04815 0.05022 = 0.06638 0.02266 -0.00874 -0.01367 C1' 1 0.467128 0.782274 0.314183 11.00000 0.03675 0.03275 = 0.04614 -0.00296 -0.00480 0.00416 AFIX 43 H1' 2 0.498926 0.834597 0.302380 11.00000 -1.20000 AFIX 0 C2' 1 0.389642 0.785205 0.302875 11.00000 0.03317 0.04068 = 0.04931 -0.00346 -0.01035 0.01271 AFIX 43 H2' 2 0.368273 0.839901 0.283909 11.00000 -1.20000 AFIX 0 C3' 1 0.343484 0.709731 0.318848 11.00000 0.02720 0.05225 = 0.04474 -0.01441 -0.00835 0.01086 AFIX 43 H3' 2 0.290505 0.710976 0.309606 11.00000 -1.20000 AFIX 0 C4' 1 0.373827 0.630905 0.348651 11.00000 0.02646 0.04757 = 0.04247 -0.00511 -0.00112 -0.00168 AFIX 43 H4' 2 0.341649 0.578866 0.360313 11.00000 -1.20000 AFIX 0 C5' 1 0.452116 0.629248 0.361197 11.00000 0.02562 0.03644 = 0.03627 -0.00165 -0.00160 0.00200 AFIX 43 H5' 2 0.473183 0.576924 0.382512 11.00000 -1.20000 AFIX 0 C6' 1 0.498914 0.704131 0.342459 11.00000 0.02748 0.02824 = 0.02659 -0.00283 -0.00270 0.00322 C7' 1 0.583840 0.703075 0.350962 11.00000 0.03133 0.01756 = 0.03392 -0.00486 -0.00280 0.00092 C8' 1 0.617582 0.640658 0.398515 11.00000 0.02369 0.01857 = 0.03261 0.00418 -0.00097 -0.00031 AFIX 13 H8' 2 0.593930 0.574515 0.396688 11.00000 -1.20000 AFIX 0 C9' 1 0.704443 0.630471 0.391969 11.00000 0.01895 0.03101 = 0.02756 0.00402 -0.00245 0.00038 AFIX 13 H9' 2 0.727987 0.696396 0.387956 11.00000 -1.20000 AFIX 0 C10' 1 0.733062 0.564749 0.344049 11.00000 0.01830 0.02340 = 0.03532 -0.00127 -0.00050 0.00037 C11' 1 0.714379 0.565621 0.286827 11.00000 0.02808 0.03366 = 0.03588 -0.00014 0.00002 -0.00295 AFIX 43 H11' 2 0.677059 0.609664 0.272598 11.00000 -1.20000 AFIX 0 C12' 1 0.751004 0.501111 0.250428 11.00000 0.03124 0.03864 = 0.03366 -0.00442 -0.00018 0.00014 AFIX 43 H12' 2 0.738413 0.500703 0.210970 11.00000 -1.20000 AFIX 0 C13' 1 0.805634 0.437423 0.271001 11.00000 0.04003 0.03509 = 0.04341 -0.00237 0.01095 0.00457 AFIX 43 H13' 2 0.830257 0.393634 0.245565 11.00000 -1.20000 AFIX 0 C14' 1 0.824714 0.436857 0.328073 11.00000 0.03424 0.03116 = 0.04587 0.00341 0.00512 0.01042 AFIX 43 H14' 2 0.862081 0.392871 0.342293 11.00000 -1.20000 AFIX 0 C15' 1 0.788369 0.501639 0.364291 11.00000 0.02512 0.02815 = 0.04054 0.00172 -0.00096 0.00193 C16' 1 0.800284 0.513705 0.427467 11.00000 0.02669 0.03795 = 0.04650 -0.00165 -0.00173 0.01213 AFIX 23 H16C 2 0.795491 0.450882 0.447782 11.00000 -1.20000 H16D 2 0.850962 0.542619 0.435929 11.00000 -1.20000 AFIX 0 C17' 1 0.705155 0.584814 0.493752 11.00000 0.03033 0.02331 = 0.03601 0.00119 -0.00457 -0.00363 AFIX 43 H17' 2 0.728437 0.551514 0.524761 11.00000 -1.20000 AFIX 0 C18' 1 0.639865 0.635267 0.502891 11.00000 0.02904 0.02234 = 0.03039 0.00229 0.00052 -0.00397 C19' 1 0.596602 0.688303 0.457253 11.00000 0.02220 0.02318 = 0.03052 -0.00189 -0.00175 -0.00219 AFIX 13 H19' 2 0.540561 0.678777 0.464108 11.00000 -1.20000 AFIX 0 C20' 1 0.613469 0.799683 0.456653 11.00000 0.03663 0.02279 = 0.03296 0.00074 -0.00022 0.00160 AFIX 23 H20C 2 0.665045 0.809855 0.440124 11.00000 -1.20000 H20D 2 0.576081 0.831411 0.430907 11.00000 -1.20000 AFIX 0 C21' 1 0.610443 0.849674 0.513193 11.00000 0.02690 0.02363 = 0.03393 -0.00078 0.00073 0.00262 AFIX 43 H21' 2 0.562072 0.854179 0.531588 11.00000 -1.20000 AFIX 0 C22' 1 0.670531 0.888338 0.539659 11.00000 0.02280 0.01830 = 0.04342 0.00025 0.00075 -0.00094 C23' 1 0.664878 0.949383 0.591705 11.00000 0.02948 0.02690 = 0.03911 -0.00001 -0.00390 -0.00619 C24' 1 0.602755 0.930675 0.634675 11.00000 0.02933 0.02659 = 0.03443 -0.00220 -0.00185 0.00010 C25' 1 0.579830 0.837070 0.647487 11.00000 0.03624 0.03666 = 0.03642 -0.00462 -0.00156 -0.00596 AFIX 43 H25' 2 0.601134 0.783815 0.627118 11.00000 -1.20000 AFIX 0 C26' 1 0.526290 0.820346 0.689591 11.00000 0.04566 0.04267 = 0.04617 0.00098 0.00447 -0.01679 AFIX 43 H26' 2 0.511898 0.755672 0.698947 11.00000 -1.20000 AFIX 0 C27' 1 0.493696 0.897496 0.718068 11.00000 0.03303 0.06926 = 0.03709 -0.00444 0.00338 -0.00300 AFIX 43 H27' 2 0.455226 0.886081 0.745961 11.00000 -1.20000 AFIX 0 C28' 1 0.516665 0.991280 0.706269 11.00000 0.03748 0.04868 = 0.04924 -0.00517 0.00011 0.01585 AFIX 43 H28' 2 0.495258 1.044163 0.726910 11.00000 -1.20000 AFIX 0 C29' 1 0.570786 1.008347 0.664448 11.00000 0.03950 0.03283 = 0.04222 -0.00400 -0.00559 0.00359 AFIX 43 H29' 2 0.586189 1.073009 0.655999 11.00000 -1.20000 AFIX 0 C30' 1 0.749293 0.881034 0.512677 11.00000 0.02552 0.02870 = 0.03420 -0.00167 -0.00272 -0.00004 C31' 1 0.798995 0.799648 0.532547 11.00000 0.02254 0.02468 = 0.03972 -0.00402 0.00038 -0.00598 C32' 1 0.856906 0.765605 0.495872 11.00000 0.02574 0.03947 = 0.04167 -0.00123 0.00595 -0.00441 AFIX 43 H32' 2 0.864800 0.795781 0.459867 11.00000 -1.20000 AFIX 0 C33' 1 0.901926 0.688811 0.512181 11.00000 0.01569 0.04853 = 0.05520 -0.01114 0.00201 0.00455 AFIX 43 H33' 2 0.939438 0.664082 0.486637 11.00000 -1.20000 AFIX 0 C34' 1 0.893205 0.646932 0.565597 11.00000 0.02515 0.03977 = 0.05742 -0.00058 -0.00434 0.00272 AFIX 43 H34' 2 0.926217 0.595650 0.577119 11.00000 -1.20000 AFIX 0 C35' 1 0.836387 0.679684 0.602313 11.00000 0.03742 0.03111 = 0.04725 0.00509 -0.00043 -0.00060 AFIX 43 H35' 2 0.829879 0.650280 0.638691 11.00000 -1.20000 AFIX 0 C36' 1 0.789338 0.755327 0.585631 11.00000 0.03401 0.02351 = 0.03855 0.00183 0.00003 -0.00325 AFIX 43 H36' 2 0.750056 0.777348 0.610544 11.00000 -1.20000 AFIX 0 N1' 3 0.737458 0.580620 0.442742 11.00000 0.02828 0.02925 = 0.03293 0.00138 -0.00752 0.00398 N2' 3 0.608538 0.632027 0.558230 11.00000 0.03359 0.02193 = 0.03873 -0.00017 -0.00212 -0.00743 O1' 4 0.625607 0.756489 0.322535 11.00000 0.03743 0.03028 = 0.03934 0.00624 0.00117 -0.00085 O2' 4 0.646382 0.599315 0.599342 11.00000 0.04812 0.02865 = 0.03726 0.00598 -0.00572 -0.00204 O3' 4 0.541266 0.662991 0.565402 11.00000 0.03107 0.03482 = 0.04481 0.00096 0.00575 -0.00251 O4' 4 0.711111 1.015309 0.598985 11.00000 0.04372 0.03959 = 0.04870 -0.00649 0.00222 -0.01960 O5' 4 0.769150 0.936049 0.474534 11.00000 0.04163 0.04530 = 0.06169 0.02202 0.00669 -0.00159 HKLF 4 REM m4279_0m_a.res in Pna2(1) REM R1 = 0.0619 for 6628 Fo > 4sig(Fo) and 0.1261 for all 10995 data REM 776 parameters refined using 1 restraints END WGHT 0.0658 0.0000 REM Highest difference peak 0.330, deepest hole -0.270, 1-sigma level 0.065 Q1 1 0.5408 0.8035 0.3467 11.00000 0.05 0.33 Q2 1 0.6901 0.2013 0.6423 11.00000 0.05 0.33 Q3 1 0.6148 0.1995 0.6515 11.00000 0.05 0.28 Q4 1 0.6553 0.3559 0.4817 11.00000 0.05 0.27 Q5 1 0.7437 0.5029 0.6305 11.00000 0.05 0.26 Q6 1 0.6687 0.7620 0.3272 11.00000 0.05 0.26 Q7 1 0.5242 0.9936 0.7493 11.00000 0.05 0.26 Q8 1 0.6577 0.2421 0.6720 11.00000 0.05 0.26 Q9 1 0.6169 0.7429 0.3394 11.00000 0.05 0.26 Q10 1 0.4688 0.0098 0.5664 11.00000 0.05 0.26 Q11 1 0.7234 0.5650 0.5972 11.00000 0.05 0.25 Q12 1 0.7490 0.5011 0.2873 11.00000 0.05 0.25 Q13 1 0.5414 1.0845 0.6489 11.00000 0.05 0.25 Q14 1 0.6162 0.2782 0.6511 11.00000 0.05 0.24 Q15 1 0.8280 0.1094 0.6329 11.00000 0.05 0.24 Q16 1 0.6978 0.8873 0.5374 11.00000 0.05 0.24 Q17 1 0.7192 0.1486 0.4308 11.00000 0.05 0.24 Q18 1 0.4295 0.7180 0.3114 11.00000 0.05 0.24 Q19 1 0.5294 0.0644 0.5486 11.00000 0.05 0.24 Q20 1 0.6714 0.2233 0.4472 11.00000 0.05 0.23 ; _shelx_res_checksum 58661 _shelx_hkl_file ; 0 -2 0 1.79 1.97 0 2 0 -0.42 1.56 0 2 0 3.39 2.14 0 -2 0 2.36 2.18 0 -3 0 0.06 3.32 0 3 0 1.49 3.48 0 -3 0 0.54 3.71 0 3 0 -4.13 3.57 0 -4 0 426.37 20.20 0 4 0 421.55 20.75 0 -4 0 416.57 20.85 0 4 0 440.54 20.00 0 -5 0 0.16 3.59 0 5 0 0.42 3.28 0 -5 0 -3.42 2.87 0 5 0 6.14 3.91 0 6 0 -0.24 3.33 0 -6 0 1.17 3.93 0 -6 0 7.27 5.10 0 6 0 -1.23 3.61 0 7 0 2.38 4.32 0 -7 0 -4.13 3.89 0 -7 0 0.13 4.68 0 7 0 3.78 4.59 0 8 0 7.12 4.88 0 -8 0 -1.87 4.70 0 8 0 4.66 5.30 0 -8 0 5.97 4.91 0 9 0 -0.81 5.03 0 -9 0 -2.24 3.84 0 -9 0 -0.52 4.36 0 -10 0 97.15 15.55 0 10 0 120.46 16.38 0 11 0 -2.30 6.18 0 -11 0 5.56 6.79 0 -11 0 -1.23 6.04 0 -12 0 187.22 21.27 0 12 0 197.04 19.47 0 -12 0 152.60 22.49 0 -13 0 6.76 9.74 0 -13 0 -0.58 8.51 0 -14 0 164.00 24.81 0 -15 0 -21.47 7.88 0 -16 0 499.95 41.76 0 -17 0 17.18 11.98 0 -18 0 9.09 14.16 1 -2 0 0.28 2.43 -1 -2 0 -0.84 1.68 -1 2 0 1.69 2.50 -1 2 0 -1.45 2.34 1 -2 0 0.56 2.33 -1 -2 0 0.94 1.60 -1 3 0 316.71 16.16 1 3 0 335.10 14.54 -1 3 0 297.98 16.72 1 -3 0 306.76 16.93 1 -3 0 330.79 16.42 -1 -3 0 320.06 14.99 -1 -3 0 321.62 15.03 -1 4 0 149.24 11.65 1 4 0 169.30 10.16 1 -4 0 148.73 11.72 1 4 0 145.42 10.10 -1 4 0 146.79 10.88 -1 -4 0 151.12 10.44 1 -4 0 161.25 11.22 -1 -4 0 144.98 10.20 1 -5 0 1359.32 54.45 -1 5 0 1328.04 54.22 -1 -5 0 1358.41 51.64 -1 -5 0 1360.01 52.31 -1 5 0 1319.46 52.35 1 -5 0 1350.40 52.90 1 5 0 1427.31 51.00 -1 6 0 -2.10 3.53 -1 6 0 -6.41 3.51 -1 -6 0 -1.26 3.70 1 -6 0 3.04 4.92 1 6 0 2.06 4.02 -1 -6 0 -0.84 3.69 1 -6 0 3.84 4.38 1 -7 0 -1.48 3.59 -1 7 0 1.70 4.99 1 7 0 2.73 4.87 -1 -7 0 5.31 4.71 1 -7 0 10.42 5.94 -1 7 0 2.55 4.12 -1 -7 0 5.38 4.71 -1 -8 0 94.59 11.71 1 -8 0 107.60 15.74 -1 8 0 116.93 12.82 1 8 0 98.91 12.60 1 -8 0 104.10 12.56 -1 -8 0 107.34 12.39 -1 8 0 99.50 14.56 -1 9 0 -4.97 3.82 1 -9 0 6.67 5.71 -1 -9 0 -6.51 4.18 -1 9 0 0.98 5.23 -1 -9 0 -2.36 4.43 1 -9 0 3.45 6.48 1 9 0 -6.97 4.39 1 -10 0 8.71 7.25 1 -10 0 -4.80 5.01 -1 -10 0 -1.05 5.43 1 10 0 2.76 5.81 -1 10 0 -0.40 5.95 -1 -10 0 5.59 6.29 -1 -11 0 22.54 10.06 -1 -11 0 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6.71 7 -5 0 125.24 12.24 -7 5 0 126.61 14.41 7 -6 0 34.37 12.28 -7 6 0 34.98 10.51 -7 -6 0 40.30 4.73 7 -6 0 70.68 11.66 -7 6 0 47.53 10.75 7 -7 0 92.71 17.55 -7 -7 0 80.10 7.18 -7 7 0 88.96 16.92 7 -7 0 102.67 14.90 -7 -7 0 82.53 8.55 -7 7 0 127.84 17.55 -7 8 0 -0.47 5.82 -7 -8 0 8.30 3.83 -7 8 0 5.90 7.28 7 -8 0 9.76 8.45 -7 -8 0 2.87 4.17 7 -8 0 -10.51 5.34 7 -9 0 -2.59 6.71 -7 -9 0 7.61 4.38 -7 9 0 -10.33 5.93 -7 9 0 15.39 9.89 7 -9 0 0.74 6.53 -7 10 0 9.54 9.01 7 -10 0 9.01 10.41 -7 -10 0 4.13 4.68 -7 10 0 7.53 8.78 7 -10 0 0.91 7.12 -7 -10 0 -3.54 4.71 7 -11 0 25.18 10.77 -7 -11 0 32.70 8.43 -7 11 0 29.39 10.95 7 -11 0 28.29 12.94 -7 -11 0 40.61 10.58 -7 11 0 22.13 11.57 -7 -12 0 9.09 6.55 -7 12 0 -16.83 7.41 7 -12 0 13.85 11.49 -7 12 0 7.89 10.28 -7 -12 0 24.11 9.77 -7 13 0 31.20 13.61 7 -13 0 45.42 15.17 -7 -14 0 2.36 12.17 -7 14 0 9.54 10.94 -7 -14 0 -5.15 6.04 7 -14 0 -0.27 9.05 7 -15 0 -8.07 10.52 -7 15 0 0.11 11.15 7 -16 0 19.50 16.17 -7 -16 0 12.73 9.47 -7 16 0 18.00 15.37 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80.07 12.95 -8 9 0 103.91 18.62 8 -9 0 71.15 17.23 -8 -9 0 76.09 8.31 8 -9 0 85.75 15.61 -8 -10 0 8.85 4.92 8 -10 0 2.38 9.12 -8 10 0 11.71 10.82 -8 10 0 5.71 11.94 -8 -10 0 16.57 8.45 -8 -11 0 6.32 4.71 -8 11 0 15.86 9.09 8 -11 0 14.02 10.34 -8 11 0 24.09 10.52 -8 -11 0 -1.03 6.35 8 -11 0 3.22 8.79 -8 12 0 -0.99 8.28 8 -12 0 4.06 9.72 -8 -12 0 13.03 6.31 -8 -12 0 7.40 7.72 -8 13 0 60.55 17.40 -8 -13 0 66.63 11.06 8 -13 0 81.77 20.79 -8 -14 0 -7.91 4.65 -8 14 0 2.49 11.30 -8 -14 0 -4.56 10.21 8 -14 0 -11.38 8.94 -8 -15 0 4.32 6.54 8 -15 0 7.13 12.07 -8 15 0 -9.91 10.75 -8 -16 0 -13.94 8.44 8 -16 0 2.16 12.94 -8 16 0 11.09 12.97 8 -17 0 22.68 14.22 -8 17 0 40.19 18.80 9 0 0 0.06 3.83 -9 0 0 1.90 3.89 -9 0 0 0.93 2.65 9 -1 0 111.48 12.42 9 1 0 112.15 10.65 -9 1 0 139.52 13.60 -9 -1 0 122.24 6.55 -9 1 0 109.45 9.66 -9 -1 0 129.22 11.25 9 2 0 5.58 3.74 9 -2 0 11.07 6.37 -9 2 0 9.22 5.16 -9 2 0 -0.92 3.68 -9 -2 0 3.67 3.63 9 -2 0 6.83 2.88 -9 -3 0 3.78 2.98 -9 3 0 3.49 5.01 -9 3 0 4.87 5.86 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87.75 9.59 -9 13 0 59.97 18.50 9 -13 0 78.68 20.76 -9 -13 0 80.25 25.28 -9 -13 0 84.13 10.23 -9 14 0 0.85 10.90 -9 -14 0 16.76 6.05 -9 -14 0 -15.49 9.46 9 -14 0 13.66 12.40 -9 -15 0 17.10 6.53 -9 15 0 8.91 14.93 9 -15 0 25.19 15.55 9 -16 0 1.27 13.44 -9 -16 0 -6.43 5.30 -9 16 0 -1.10 11.34 10 0 0 250.04 18.00 -10 0 0 302.50 19.59 -10 0 0 246.25 13.80 -10 -1 0 1.89 3.38 10 1 0 0.13 3.60 -10 1 0 4.40 4.47 10 -1 0 -3.02 4.30 -10 -1 0 -2.52 1.96 -10 1 0 8.52 4.02 -10 2 0 7.36 5.82 10 -2 0 7.84 5.83 -10 2 0 6.31 4.67 10 2 0 -0.49 2.91 10 -2 0 2.94 2.42 -10 -2 0 2.64 3.64 10 -3 0 156.62 16.52 10 -3 0 167.90 11.08 -10 -3 0 156.19 11.60 -10 3 0 164.36 14.30 -10 3 0 169.71 16.80 -10 -4 0 103.63 8.53 10 -4 0 79.58 9.38 -10 4 0 100.11 16.66 -10 4 0 123.42 15.89 10 -4 0 129.97 18.73 10 -5 0 10.76 8.04 -10 5 0 8.21 6.57 -10 -5 0 6.42 2.81 10 -5 0 4.58 5.81 -10 5 0 8.65 6.54 -10 6 0 202.15 19.47 -10 -6 0 171.50 8.27 -10 6 0 181.60 20.03 10 -6 0 189.67 16.35 10 -6 0 171.57 20.55 10 -7 0 2.14 6.28 10 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0 196.24 18.81 11 2 0 202.53 14.72 11 -2 0 209.27 9.59 -11 -2 0 201.98 15.20 -11 3 0 64.23 13.81 11 -3 0 42.25 6.42 -11 3 0 62.02 10.73 -11 -3 0 45.59 7.68 -11 -4 0 5.40 3.90 -11 4 0 7.35 5.76 11 -4 0 3.87 3.88 -11 4 0 27.65 8.42 11 -4 0 20.12 8.64 11 -5 0 13.64 8.75 -11 5 0 2.57 6.49 -11 5 0 -2.70 5.64 -11 -5 0 1.71 2.48 11 -5 0 -1.02 5.54 11 -6 0 -1.55 5.54 -11 6 0 -0.21 6.45 11 -6 0 7.30 8.22 -11 6 0 -4.23 6.16 11 -7 0 24.77 9.25 -11 7 0 15.90 9.76 -11 7 0 13.11 8.89 11 -7 0 14.17 10.08 11 -8 0 0.17 7.61 -11 8 0 3.10 10.15 -11 8 0 -0.86 7.71 -11 -8 0 -4.35 4.02 11 -8 0 2.47 7.03 -11 -9 0 67.00 10.91 11 -9 0 96.33 17.43 -11 9 0 76.98 17.54 11 -9 0 83.11 19.98 -11 10 0 6.96 9.83 11 -10 0 -8.09 7.78 11 -10 0 -6.67 6.85 -11 -10 0 4.19 7.31 -11 -11 0 11.41 8.14 -11 11 0 -4.98 9.63 11 -11 0 11.30 10.31 -11 -12 0 9.08 9.16 -11 12 0 2.66 11.46 -11 13 0 17.09 12.97 -11 -13 0 23.02 13.02 11 -13 0 20.25 14.50 -11 14 0 9.57 11.27 11 -14 0 -0.45 11.75 -11 -14 0 12.92 15.81 11 -15 0 4.85 11.32 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4.57 -14 4 0 302.44 27.90 -14 -4 0 309.49 19.24 14 -4 0 314.25 28.09 -14 4 0 298.90 24.38 14 -4 0 310.13 16.48 14 -5 0 69.77 9.64 -14 5 0 67.92 14.50 -14 5 0 44.18 14.23 14 -5 0 55.13 15.35 -14 -5 0 75.48 8.26 -14 6 0 6.07 9.90 14 -6 0 5.70 9.75 -14 6 0 20.69 10.76 14 -6 0 26.98 7.57 -14 7 0 -8.74 7.38 14 -7 0 -14.39 6.58 -14 7 0 14.27 9.67 14 -7 0 -2.23 5.64 14 -8 0 23.54 10.17 -14 -8 0 22.81 5.28 -14 8 0 16.57 12.55 14 -8 0 17.20 12.73 14 -9 0 1.71 9.74 -14 9 0 8.20 10.29 -14 -9 0 11.86 6.44 14 -9 0 8.57 11.38 14 -10 0 69.09 16.49 -14 10 0 67.09 19.20 -14 -11 0 13.50 9.97 14 -11 0 2.82 9.75 -14 11 0 5.20 13.00 14 -12 0 32.05 16.24 -14 12 0 53.97 19.31 -14 13 0 9.89 15.19 14 -13 0 -1.09 12.45 -14 14 0 14.50 17.02 14 -14 0 -9.88 10.99 -15 0 0 3.34 4.59 15 0 0 0.92 7.00 -15 0 0 2.38 4.67 -15 1 0 9.19 6.37 15 -1 0 6.12 7.58 -15 1 0 -9.73 4.30 15 1 0 -1.82 6.02 -15 -1 0 3.71 5.19 -15 -1 0 4.44 4.77 -15 2 0 3.91 6.52 15 2 0 1.95 5.54 -15 2 0 8.23 7.11 15 -2 0 29.71 11.48 -15 -2 0 10.27 4.47 -15 -2 0 -5.32 4.31 -15 -3 0 49.21 9.89 15 -3 0 68.95 15.80 -15 3 0 74.84 14.71 -15 3 0 38.31 12.77 -15 -3 0 51.26 6.36 15 -4 0 71.35 6.69 -15 -4 0 69.06 10.53 -15 4 0 60.22 13.46 15 -4 0 37.07 14.34 -15 4 0 59.43 15.10 15 -5 0 9.24 4.96 -15 5 0 7.01 8.38 15 -5 0 11.34 10.93 -15 -5 0 -1.16 3.70 -15 5 0 12.01 11.07 15 -6 0 1.85 8.83 -15 6 0 -4.95 7.92 15 -6 0 1.76 5.93 -15 6 0 18.04 10.88 15 -7 0 14.77 7.49 15 -7 0 15.15 12.44 -15 7 0 14.66 11.04 -15 8 0 -4.18 9.92 15 -8 0 10.14 8.65 -15 -8 0 -3.19 3.80 15 -8 0 -0.70 8.66 15 -9 0 2.88 11.16 -15 9 0 -5.71 10.46 -15 -9 0 -2.31 5.30 15 -9 0 10.19 11.54 15 -10 0 7.93 11.15 -15 10 0 5.09 18.64 15 -10 0 7.62 10.67 15 -11 0 0.40 12.34 -15 11 0 14.11 13.67 15 -12 0 -14.66 9.49 -15 12 0 -11.10 11.40 15 -13 0 7.08 13.39 -15 13 0 5.36 15.08 15 -14 0 -13.29 13.02 -15 14 0 -24.60 10.85 -16 0 0 20.85 10.08 16 0 0 15.88 8.99 -16 0 0 5.81 6.02 -16 -1 0 1.61 4.73 -16 -1 0 12.97 7.95 16 1 0 8.91 8.06 16 -1 0 5.16 7.52 -16 1 0 10.08 8.43 -16 1 0 13.23 8.37 -16 2 0 -0.97 7.04 16 -2 0 -7.31 7.67 -16 2 0 22.25 10.39 -16 -2 0 18.35 6.30 -16 3 0 6.29 7.64 16 -3 0 13.31 10.67 -16 -3 0 15.87 5.02 -16 -3 0 13.32 6.52 -16 3 0 8.14 8.79 -16 -4 0 -5.73 4.00 16 -4 0 0.43 8.96 -16 -4 0 -3.00 2.69 -16 4 0 5.42 8.05 -16 -5 0 12.61 5.05 16 -5 0 18.31 10.60 -16 5 0 6.83 9.51 -16 5 0 17.92 11.98 16 -5 0 12.27 4.40 16 -6 0 15.44 11.72 16 -6 0 -2.48 6.99 -16 6 0 18.56 12.37 -16 6 0 -2.55 9.09 16 -7 0 9.34 7.03 16 -7 0 37.26 15.01 -16 7 0 25.82 12.96 16 -8 0 9.15 10.88 16 -8 0 14.09 8.41 -16 8 0 11.83 11.68 -16 -8 0 14.59 4.16 -16 9 0 17.53 13.60 16 -9 0 9.21 10.84 16 -9 0 -4.36 9.60 16 -10 0 2.72 11.50 -16 10 0 -27.90 9.72 16 -10 0 -3.58 10.81 -16 11 0 12.35 15.26 16 -11 0 -7.51 10.59 -16 12 0 -4.59 12.15 16 -12 0 36.08 16.49 -16 13 0 20.49 16.87 16 -13 0 11.43 17.56 -17 0 0 2.15 6.06 17 0 0 12.01 8.26 -17 0 0 1.78 6.89 -17 -1 0 13.26 7.98 -17 1 0 7.87 8.47 -17 -1 0 2.36 6.43 -17 1 0 23.92 8.85 17 -1 0 19.40 9.25 17 1 0 0.17 6.92 -17 -2 0 35.90 10.14 17 -2 0 26.70 11.71 -17 2 0 31.32 11.96 -17 -2 0 13.77 7.15 -17 2 0 17.53 8.99 -17 3 0 15.71 8.04 17 -3 0 39.33 14.36 -17 -3 0 16.65 7.65 -17 -3 0 11.32 5.95 -17 3 0 9.42 10.77 -17 -4 0 96.51 8.94 -17 4 0 102.97 20.66 17 -4 0 98.16 21.63 -17 -4 0 120.87 12.89 -17 4 0 125.17 20.15 -17 5 0 35.31 15.69 -17 -5 0 46.47 8.19 17 -5 0 50.51 16.32 17 -5 0 64.65 8.86 -17 5 0 81.99 18.38 17 -6 0 2.68 4.87 17 -6 0 -1.72 8.63 -17 6 0 7.00 10.39 -17 7 0 33.05 14.54 17 -7 0 35.94 9.33 17 -7 0 51.15 18.18 -17 8 0 10.84 13.60 17 -8 0 -10.68 6.99 17 -8 0 -18.05 7.54 17 -9 0 21.25 11.02 17 -9 0 3.76 12.22 17 -10 0 16.54 13.45 17 -10 0 7.03 12.12 -17 10 0 0.41 13.80 -17 11 0 20.59 18.10 17 -11 0 22.98 14.77 -17 12 0 14.69 18.07 17 -12 0 4.85 14.76 18 0 0 154.26 22.24 -18 0 0 129.59 15.61 -18 0 0 84.51 18.49 -18 1 0 80.17 17.05 -18 -1 0 96.57 17.07 -18 -1 0 101.15 17.33 18 -1 0 82.07 18.90 18 1 0 86.59 15.28 -18 2 0 -4.35 7.43 -18 -2 0 0.60 6.33 -18 2 0 -12.43 8.97 18 -2 0 13.45 10.85 -18 -2 0 9.83 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-3 1 28 1.92 10.09 3 -1 28 19.93 11.79 -3 -2 28 -12.22 8.45 3 2 28 -9.47 9.56 3 -2 28 6.70 11.68 -3 2 28 6.22 11.59 3 3 28 8.63 11.80 -3 -3 28 11.82 11.05 -3 3 28 8.67 11.26 3 -3 28 3.88 10.63 3 4 28 8.92 11.20 -3 -4 28 -11.67 9.87 3 -4 28 11.92 11.63 -3 4 28 0.61 10.53 3 5 28 -4.98 9.92 -3 -5 28 17.73 13.09 -3 5 28 -15.16 10.29 3 -5 28 6.35 12.13 -3 -6 28 4.70 11.61 3 6 28 4.70 12.13 -3 6 28 -10.63 11.45 3 -6 28 -1.99 11.08 3 7 28 -0.82 12.30 -3 -7 28 8.44 11.69 -3 7 28 14.67 13.24 3 -7 28 12.05 11.23 4 0 28 24.21 12.54 -4 0 28 14.84 11.95 4 1 28 -5.88 9.92 -4 -1 28 6.32 10.41 4 -1 28 7.49 10.29 -4 1 28 10.09 10.28 -4 -2 28 5.95 10.89 4 2 28 39.42 13.65 4 -2 28 14.53 11.52 -4 2 28 35.07 13.55 4 3 28 8.45 11.67 -4 -3 28 -7.09 8.65 -4 3 28 5.00 11.22 4 -3 28 12.08 10.78 -4 -4 28 -6.18 8.63 4 4 28 -1.05 10.63 -4 4 28 11.54 13.11 4 -4 28 3.71 10.60 4 5 28 21.89 13.51 -4 -5 28 26.57 13.80 4 -5 28 -11.83 10.64 -4 5 28 10.54 12.33 4 6 28 0.78 12.02 -4 -6 28 -8.02 13.56 4 -6 28 33.72 14.70 -4 6 28 15.94 13.70 -4 -7 28 30.73 15.60 4 7 28 6.60 12.90 4 -7 28 58.31 17.45 -4 7 28 -6.78 12.99 -5 0 28 16.66 11.37 5 0 28 -7.89 9.01 -5 -1 28 -3.72 10.26 5 1 28 5.83 10.69 5 -1 28 7.95 9.77 -5 1 28 -5.16 10.11 5 2 28 11.52 11.07 -5 -2 28 0.37 10.08 -5 2 28 19.07 12.71 5 -2 28 7.83 12.58 -5 -3 28 14.80 11.99 5 3 28 2.06 10.44 5 -3 28 -17.16 9.54 -5 3 28 14.36 12.55 5 4 28 7.14 11.17 -5 -4 28 11.30 12.27 -5 4 28 24.99 13.74 5 -4 28 13.60 12.42 5 5 28 9.14 11.87 -5 -5 28 8.32 11.72 5 -5 28 11.41 12.24 -5 5 28 -5.49 11.14 -5 -6 28 10.66 12.81 5 6 28 16.90 12.06 5 -6 28 21.56 12.65 -5 6 28 -18.23 9.33 -5 -7 28 0.97 12.08 5 7 28 -5.06 10.87 5 -7 28 4.16 12.32 -5 7 28 -14.22 10.87 6 0 28 4.68 11.41 -6 0 28 1.48 10.24 6 1 28 -4.49 9.75 -6 -1 28 8.69 12.30 -6 1 28 -1.74 12.13 6 -1 28 0.07 10.50 6 2 28 -14.27 8.98 -6 -2 28 -3.88 10.89 -6 2 28 -6.59 9.59 6 -2 28 -11.03 8.39 -6 -3 28 -4.09 9.83 6 3 28 -17.28 8.44 6 -3 28 -11.77 9.58 -6 3 28 -5.17 12.45 6 4 28 -22.45 9.34 -6 -4 28 5.76 10.52 -6 4 28 15.89 12.47 6 -4 28 6.41 11.11 6 5 28 -11.02 21.79 -6 -5 28 -9.63 10.45 -6 5 28 5.14 12.48 6 -5 28 -4.69 10.86 -6 -6 28 26.99 13.70 6 -6 28 13.51 13.69 -6 6 28 6.95 12.37 -7 0 28 -0.25 9.89 7 0 28 2.96 11.22 7 1 28 -2.34 10.04 -7 -1 28 -0.63 10.73 7 -1 28 -4.93 9.51 -7 1 28 -0.59 9.38 -7 -2 28 7.94 10.60 7 2 28 7.75 13.41 7 -2 28 13.29 11.72 -7 2 28 5.03 11.82 -7 -3 28 3.47 11.25 -7 3 28 6.16 12.16 7 -3 28 -2.63 11.84 7 4 28 3.57 10.36 -7 -4 28 4.91 11.35 7 -4 28 0.52 10.69 -7 4 28 9.63 12.54 7 5 28 6.43 11.23 -7 -5 28 -26.81 9.81 -7 5 28 3.31 12.77 7 -5 28 21.61 14.63 -8 0 28 -4.45 9.78 8 0 28 4.92 10.32 -8 -1 28 23.16 14.57 8 1 28 19.78 14.12 8 -1 28 41.82 14.37 -8 1 28 28.83 13.93 8 2 28 9.91 12.39 -8 -2 28 -1.01 10.35 8 -2 28 -5.72 10.34 -8 2 28 3.12 11.29 -8 -3 28 2.21 10.92 8 3 28 6.04 9.26 8 -3 28 3.31 10.97 -8 3 28 -12.49 10.00 -8 -4 28 24.42 14.83 8 4 28 10.35 10.64 8 -4 28 9.92 12.98 -8 4 28 -9.70 10.81 8 5 28 -5.72 9.43 -8 -5 28 -2.01 11.66 8 -5 28 2.78 12.01 -8 5 28 -8.95 12.86 9 0 28 1.64 10.01 -9 0 28 1.38 12.26 -9 -1 28 -4.62 11.20 9 1 28 21.46 15.59 -9 1 28 20.41 13.38 9 -1 28 -11.56 9.18 9 2 28 8.56 9.95 -9 -2 28 3.21 11.16 9 -2 28 9.30 10.85 -9 2 28 -15.18 10.41 -9 -3 28 8.25 10.48 9 3 28 12.79 11.35 9 -3 28 -3.27 10.76 -9 3 28 8.20 11.87 -10 0 28 -21.40 11.28 -10 -1 28 6.35 11.26 10 1 28 17.49 11.31 -10 1 28 0.36 11.70 10 -1 28 13.16 11.65 0 0 29 -6.56 10.20 0 1 29 12.57 12.30 0 -1 29 33.81 14.13 0 2 29 -0.37 10.03 0 -2 29 -0.36 10.39 0 -3 29 3.38 10.66 0 3 29 4.09 12.02 0 4 29 -1.17 10.11 0 -4 29 6.68 12.26 0 5 29 0.53 11.01 0 -5 29 31.60 15.29 0 -6 29 -4.64 11.70 0 6 29 1.61 12.42 1 0 29 -3.85 10.25 -1 0 29 16.73 13.71 1 1 29 -1.50 11.00 -1 -1 29 3.63 10.79 -1 1 29 5.71 10.97 1 -1 29 30.99 14.23 -1 -2 29 -8.99 10.18 1 2 29 25.39 12.66 -1 2 29 8.55 12.24 1 -2 29 9.73 12.05 1 3 29 0.05 11.56 -1 -3 29 17.46 12.05 1 -3 29 38.06 14.37 -1 3 29 9.10 12.46 1 4 29 13.28 12.02 -1 -4 29 18.27 12.71 -1 4 29 -3.38 11.01 1 -4 29 -7.55 11.72 1 5 29 1.28 12.70 -1 -5 29 8.40 13.33 1 -5 29 10.75 14.17 -1 5 29 10.75 13.07 -1 -6 29 -12.44 12.53 1 6 29 -1.83 12.72 -1 6 29 -19.73 11.40 1 -6 29 -4.24 12.02 -2 0 29 38.56 14.55 2 0 29 22.57 12.86 -2 -1 29 -10.20 10.64 2 1 29 -11.00 10.20 2 -1 29 -0.57 10.94 -2 1 29 -0.85 11.30 2 2 29 -7.28 11.18 -2 -2 29 -6.79 9.89 -2 2 29 -15.29 9.26 2 -2 29 -14.29 8.84 2 3 29 12.97 12.23 -2 -3 29 6.63 10.79 -2 3 29 -9.03 12.08 2 -3 29 -0.47 11.57 2 4 29 13.65 11.55 -2 -4 29 -1.50 10.91 -2 4 29 -23.83 9.13 2 -4 29 0.36 11.47 -2 -5 29 -10.28 11.69 2 5 29 19.75 13.12 -2 5 29 2.46 12.36 2 -5 29 -3.35 12.45 -2 -6 29 6.98 12.07 2 6 29 2.79 13.50 -2 6 29 6.87 12.99 2 -6 29 -2.31 12.56 -3 0 29 1.23 9.82 3 0 29 10.87 11.65 -3 -1 29 -12.23 10.06 3 1 29 -9.24 10.09 3 -1 29 -10.69 10.04 -3 1 29 -4.42 11.06 -3 -2 29 17.70 12.75 3 2 29 -3.60 10.75 3 -2 29 -3.86 10.19 -3 2 29 8.32 10.86 3 3 29 14.71 13.53 -3 -3 29 28.04 13.74 3 -3 29 -0.11 11.19 -3 3 29 41.08 15.93 -3 -4 29 11.00 12.21 3 4 29 20.10 12.06 -3 4 29 4.99 11.77 3 -4 29 -15.17 10.59 3 5 29 -2.29 10.67 -3 -5 29 -6.87 11.48 3 -5 29 -2.89 12.20 -3 5 29 20.74 13.42 3 6 29 25.40 14.39 -3 -6 29 6.10 11.52 -3 6 29 -10.16 12.61 3 -6 29 9.17 12.97 -4 0 29 4.74 9.88 4 0 29 0.64 11.19 -4 -1 29 -9.12 10.71 4 1 29 -7.21 9.65 4 -1 29 7.59 11.70 -4 1 29 6.79 12.53 -4 -2 29 8.36 12.52 4 2 29 -3.44 10.07 -4 2 29 -1.71 9.75 4 -2 29 -5.83 11.24 4 3 29 14.63 13.72 -4 -3 29 18.26 13.29 -4 3 29 16.34 12.46 4 -3 29 -4.63 9.42 -4 -4 29 20.89 12.36 4 4 29 -7.93 10.72 4 -4 29 16.34 12.95 -4 4 29 -16.45 9.41 4 5 29 4.27 11.75 -4 -5 29 -1.29 10.72 -4 5 29 9.40 12.93 4 -5 29 3.02 11.55 5 0 29 -7.80 10.85 -5 0 29 12.76 11.63 -5 -1 29 1.32 10.64 5 1 29 15.46 12.29 5 -1 29 5.05 10.48 -5 1 29 8.22 12.43 -5 -2 29 9.37 13.11 5 2 29 12.57 12.24 5 -2 29 13.07 12.01 -5 2 29 18.73 12.61 5 3 29 -9.27 10.69 -5 -3 29 -6.19 10.91 5 -3 29 -1.62 11.83 -5 3 29 5.14 12.97 5 4 29 5.41 11.31 -5 -4 29 35.47 13.52 -5 4 29 -6.94 11.87 5 -4 29 3.99 12.72 -5 -5 29 19.23 12.95 5 5 29 35.89 14.88 5 -5 29 21.45 14.79 -6 0 29 5.69 12.27 6 0 29 0.08 11.72 -6 -1 29 6.71 13.00 6 1 29 -10.92 9.51 -6 1 29 -2.56 11.82 6 -1 29 -15.46 8.97 -6 -2 29 4.84 11.44 6 2 29 16.23 12.73 6 -2 29 23.89 13.46 -6 2 29 6.66 13.61 -6 -3 29 -17.06 10.03 6 3 29 -12.27 8.37 -6 3 29 7.89 10.90 6 -3 29 2.65 11.11 -6 -4 29 2.31 10.42 6 4 29 0.08 10.31 6 -4 29 3.06 12.63 -6 4 29 4.81 12.33 7 0 29 7.85 10.45 -7 0 29 3.91 11.86 -7 -1 29 -1.70 11.25 7 1 29 2.72 10.01 7 -1 29 -1.66 10.62 -7 1 29 18.41 13.66 -7 -2 29 5.68 10.25 7 2 29 -8.24 10.08 -7 2 29 4.24 11.75 7 -2 29 14.34 12.51 -7 -3 29 10.63 12.97 7 3 29 4.85 10.57 7 -3 29 25.01 14.59 -7 3 29 2.64 13.46 -8 0 29 -14.50 11.40 8 0 29 19.86 12.06 -8 -1 29 0.35 12.35 8 1 29 1.03 11.63 8 -1 29 9.77 11.14 -8 1 29 -9.81 8.34 8 2 29 26.05 12.15 -8 -2 29 -11.37 9.94 -8 2 29 13.22 13.31 8 -2 29 13.42 12.62 0 0 30 18.55 13.78 0 -1 30 2.96 10.74 0 1 30 -24.73 9.62 0 -2 30 0.99 12.83 0 2 30 19.22 13.61 0 3 30 -2.52 13.02 0 -3 30 1.88 12.34 0 4 30 -7.78 11.20 0 -4 30 3.28 11.56 1 0 30 -18.44 9.41 -1 0 30 -12.81 9.91 -1 -1 30 -18.32 9.39 1 1 30 11.79 12.30 -1 1 30 -7.44 10.49 1 -1 30 -0.47 10.38 -1 -2 30 10.30 12.42 1 2 30 10.76 11.23 1 -2 30 14.74 12.46 -1 2 30 8.69 11.89 -1 -3 30 28.69 14.49 1 3 30 12.59 13.83 -1 3 30 20.47 13.80 1 -3 30 47.03 16.66 -1 -4 30 1.71 11.96 1 4 30 -1.03 12.57 1 -4 30 -0.48 11.44 -1 4 30 17.00 13.12 -2 0 30 5.62 14.24 2 0 30 1.18 11.88 -2 -1 30 3.60 10.49 2 1 30 -7.92 11.25 -2 1 30 -5.88 10.87 2 -1 30 5.68 11.54 -2 -2 30 1.93 11.19 2 2 30 9.79 11.33 -2 2 30 27.98 14.33 2 -2 30 -3.99 11.18 2 3 30 2.31 12.27 -2 -3 30 9.84 12.40 -2 3 30 17.79 14.49 2 -3 30 47.37 17.06 2 4 30 3.11 10.99 -2 -4 30 -10.22 11.35 2 -4 30 32.11 14.86 -2 4 30 17.42 12.62 -3 0 30 3.65 11.16 3 0 30 4.02 11.62 3 1 30 -15.31 10.07 -3 -1 30 1.03 10.98 -3 1 30 -5.76 10.33 3 -1 30 7.04 11.07 3 2 30 28.91 14.69 -3 -2 30 16.43 11.79 3 -2 30 -20.35 10.85 -3 2 30 5.16 12.14 3 3 30 26.17 15.80 -3 -3 30 1.35 12.05 -3 3 30 27.28 15.27 3 -3 30 29.98 14.75 3 4 30 9.62 11.93 -3 -4 30 -15.75 9.80 -3 4 30 6.25 12.40 3 -4 30 3.51 12.76 -4 0 30 37.24 16.52 4 0 30 44.77 15.84 -4 -1 30 -0.28 11.24 4 1 30 -6.92 10.49 4 -1 30 9.11 11.98 -4 1 30 -1.41 10.85 -4 -2 30 0.25 11.22 4 2 30 4.41 12.49 4 -2 30 -9.27 10.29 -4 2 30 2.44 12.73 4 3 30 -9.83 10.97 -4 -3 30 -8.54 11.13 -4 3 30 -1.81 11.30 4 -3 30 -13.03 10.02 5 0 30 5.16 13.10 -5 0 30 -5.05 10.35 -5 -1 30 3.12 13.03 5 1 30 1.43 12.17 5 -1 30 -2.70 11.07 -5 1 30 10.71 13.77 5 2 30 2.31 11.17 -5 -2 30 -15.98 10.39 -5 2 30 1.62 10.87 5 -2 30 -1.42 11.72 5 3 30 9.48 11.29 -5 -3 30 9.28 11.67 -5 3 30 -21.89 10.42 5 -3 30 -12.24 9.86 -6 0 30 16.43 13.36 6 0 30 -5.93 11.31 6 1 30 12.50 11.65 -6 -1 30 5.06 12.99 -6 1 30 3.25 13.51 6 -1 30 1.34 12.41 0 0 31 -14.01 10.59 0 -1 31 7.55 13.54 0 1 31 1.18 12.45 1 0 31 21.41 13.41 -1 0 31 8.47 12.71 1 1 31 3.23 11.79 -1 -1 31 -0.33 10.11 -1 1 31 21.73 14.44 1 -1 31 2.98 12.05 2 0 31 -3.75 11.64 -2 0 31 -14.65 10.42 2 1 31 15.35 14.21 -2 -1 31 0.19 12.34 2 -1 31 7.11 13.26 -2 1 31 1.20 11.28 0 0 0 0.00 0.00 _exptl_absorpt_process_details ) SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., J. Appl. Cryst. 48 (2015) 3-10 ) _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_max 0.7457 _exptl_absorpt_correction_T_min 0.6214 _exptl_special_details ) The following wavelength and cell were deduced by SADABS from the direction cosines etc. They are given here for emergency use only: CELL 0.71073 13.753 17.455 23.418 89.987 89.991 90.011 ) _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 1964 _olex2_submission_special_instructions 'No special instructions were received' ####################################################################### # # This file contains crystal structure data downloaded from the # Cambridge Structural Database (CSD) hosted by the Cambridge # Crystallographic Data Centre (CCDC). # # Full information about CCDC data access policies and citation # guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 # # Audit and citation data items may have been added by the CCDC. # Please retain this information to preserve the provenance of # this file and to allow appropriate attribution of the data. # ####################################################################### data_glj-104 _database_code_depnum_ccdc_archive 'CCDC 2116271' loop_ _audit_author_name _audit_author_address 'Qilin Wang' ;Henan University China ; _audit_update_record ; 2021-10-18 deposited with the CCDC. 2021-11-08 downloaded from the CCDC. ; _audit_creation_date 2021-10-18 _audit_creation_method ; Olex2 1.3-alpha (compiled 2020.09.11 svn.r3730fd0d for OlexSys, GUI svn.r6159) ; _shelx_SHELXL_version_number 2018/3 _chemical_name_common ? _chemical_name_systematic ? _chemical_formula_moiety 'C16 H16 N2 O4' _chemical_formula_sum 'C16 H16 N2 O4' _chemical_formula_weight 300.31 _chemical_melting_point ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_H-M_alt 'P 1 21/n 1' _space_group_name_Hall '-P 2yn' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.6890(9) _cell_length_b 5.8460(4) _cell_length_c 19.4233(15) _cell_angle_alpha 90 _cell_angle_beta 92.761(7) _cell_angle_gamma 90 _cell_volume 1325.74(18) _cell_formula_units_Z 4 _cell_measurement_reflns_used 1520 _cell_measurement_temperature 150.00(10) _cell_measurement_theta_max 72.7260 _cell_measurement_theta_min 4.3070 _shelx_estimated_absorpt_T_max ? _shelx_estimated_absorpt_T_min ? _exptl_absorpt_coefficient_mu 0.908 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.64575 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.38.43f (Rigaku Oxford Diffraction, 2015) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_special_details ? _exptl_crystal_colour yellow _exptl_crystal_colour_primary yellow _exptl_crystal_density_diffrn 1.505 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description block _exptl_crystal_F_000 632 _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.11 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0386 _diffrn_reflns_av_unetI/netI 0.0538 _diffrn_reflns_Laue_measured_fraction_full 0.996 _diffrn_reflns_Laue_measured_fraction_max 0.956 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_k_min -3 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_number 4331 _diffrn_reflns_point_group_measured_fraction_full 0.996 _diffrn_reflns_point_group_measured_fraction_max 0.956 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 73.522 _diffrn_reflns_theta_min 4.325 _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 150.00(10) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 5.2684 _diffrn_detector_type AtlasS2 _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.956 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames #-------------------------------------------------------------------------- 1 \w 7.00 32.00 1.00 1.20 -- -40.73 57.00 120.00 25 2 \w -64.00 -38.00 1.00 1.20 -- -40.73 57.00 120.00 26 3 \w -64.00 29.00 1.00 1.20 -- -40.73 38.00 30.00 93 4 \w -103.00 -17.00 1.00 1.20 -- -40.73 -38.00-150.00 86 5 \w 114.00 169.00 1.00 2.00 -- 107.58 125.00-180.00 55 6 \w 82.00 169.00 1.00 2.00 -- 107.58 30.00 -30.00 87 7 \w 37.00 85.00 1.00 2.00 -- 107.58 -95.00-180.00 48 8 \w 26.00 104.00 1.00 2.00 -- 107.58 -95.00 120.00 78 9 \w 37.00 133.00 1.00 2.00 -- 107.58 -45.00 150.00 96 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, AtlasS2' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 -0.1100038000 _diffrn_orient_matrix_UB_12 0.0543533000 _diffrn_orient_matrix_UB_13 0.0374711000 _diffrn_orient_matrix_UB_21 0.0724288000 _diffrn_orient_matrix_UB_22 0.0549907000 _diffrn_orient_matrix_UB_23 0.0663194000 _diffrn_orient_matrix_UB_31 0.0080147000 _diffrn_orient_matrix_UB_32 0.2518207000 _diffrn_orient_matrix_UB_33 -0.0225284000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54184 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'SuperNova (Cu) X-ray Source' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 2022 _reflns_number_total 2563 _reflns_odcompleteness_completeness 99.66 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 66.97 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement 'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)' _computing_data_collection 'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)' _computing_data_reduction 'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)' _computing_molecular_graphics 'Olex2 1.3-alpha (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.3-alpha (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT (Sheldrick, 2015)' _refine_diff_density_max 0.304 _refine_diff_density_min -0.450 _refine_diff_density_rms 0.078 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.070 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 199 _refine_ls_number_reflns 2563 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0722 _refine_ls_R_factor_gt 0.0576 _refine_ls_restrained_S_all 1.070 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0906P)^2^+0.0681P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1507 _refine_ls_wR_factor_ref 0.1660 _refine_special_details ? _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All O(H) groups 2.a Ternary CH refined with riding coordinates: C10(H10), C11(H11), C12(H12), C15(H15) 2.b Secondary CH2 refined with riding coordinates: C7(H7A,H7B), C14(H14A,H14B), C16(H16A,H16B) 2.c Aromatic/amide H refined with riding coordinates: C2(H2), C3(H3A), C4(H4), C5(H5), C8(H8) 2.d Tetrahedral OH refined with riding coordinates: O3(H3) ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _atom_sites_solution_secondary ? loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group O1 O 0.65004(17) 0.9122(3) 0.54281(10) 0.0375(5) Uani 1 1 d . . . . . O2 O 0.76770(16) 0.6302(3) 0.56574(9) 0.0342(4) Uani 1 1 d . . . . . O3 O 0.89288(17) 0.0337(3) 0.46108(11) 0.0431(5) Uani 1 1 d . . . . . H3 H 0.909223 0.079593 0.500213 0.065 Uiso 1 1 calc R U . . . O4 O 0.66626(15) -0.0407(3) 0.33056(9) 0.0314(4) Uani 1 1 d . . . . . N1 N 0.49772(16) 0.5782(3) 0.38580(10) 0.0227(4) Uani 1 1 d . . . . . N2 N 0.69193(17) 0.7211(3) 0.52755(10) 0.0267(4) Uani 1 1 d . . . . . C1 C 0.47886(19) 0.3508(4) 0.28815(11) 0.0221(5) Uani 1 1 d . . . . . C2 C 0.4847(2) 0.1870(4) 0.23654(12) 0.0263(5) Uani 1 1 d . . . . . H2 H 0.528980 0.056045 0.243493 0.032 Uiso 1 1 calc R U . . . C3 C 0.4231(2) 0.2223(4) 0.17420(13) 0.0302(5) Uani 1 1 d . . . . . H3A H 0.425739 0.112780 0.139595 0.036 Uiso 1 1 calc R U . . . C4 C 0.3582(2) 0.4179(4) 0.16302(12) 0.0284(5) Uani 1 1 d . . . . . H4 H 0.321029 0.442704 0.120258 0.034 Uiso 1 1 calc R U . . . C5 C 0.3483(2) 0.5781(4) 0.21562(13) 0.0278(5) Uani 1 1 d . . . . . H5 H 0.302834 0.707472 0.208929 0.033 Uiso 1 1 calc R U . . . C6 C 0.40780(19) 0.5402(4) 0.27820(12) 0.0239(5) Uani 1 1 d . . . . . C7 C 0.40473(19) 0.6816(4) 0.34232(12) 0.0260(5) Uani 1 1 d . . . . . H7A H 0.419935 0.841451 0.333014 0.031 Uiso 1 1 calc R U . . . H7B H 0.331545 0.668176 0.363488 0.031 Uiso 1 1 calc R U . . . C8 C 0.55371(19) 0.6887(4) 0.43625(11) 0.0240(5) Uani 1 1 d . . . . . H8 H 0.524787 0.827704 0.450899 0.029 Uiso 1 1 calc R U . . . C9 C 0.65241(19) 0.6070(4) 0.46777(11) 0.0235(5) Uani 1 1 d . . . . . C10 C 0.71495(19) 0.4015(4) 0.44152(11) 0.0232(5) Uani 1 1 d . . . . . H10 H 0.698992 0.268899 0.470404 0.028 Uiso 1 1 calc R U . . . C11 C 0.66816(18) 0.3538(4) 0.36604(11) 0.0215(5) Uani 1 1 d . . . . . H11 H 0.695732 0.475847 0.336496 0.026 Uiso 1 1 calc R U . . . C12 C 0.53653(18) 0.3551(4) 0.36014(11) 0.0214(5) Uani 1 1 d . . . . . H12 H 0.506345 0.231345 0.388069 0.026 Uiso 1 1 calc R U . . . C13 C 0.7216(2) 0.1306(4) 0.34394(11) 0.0245(5) Uani 1 1 d . . . . . C14 C 0.8502(2) 0.1382(4) 0.34347(13) 0.0300(5) Uani 1 1 d . . . . . H14A H 0.873003 0.242171 0.307711 0.036 Uiso 1 1 calc R U . . . H14B H 0.879066 -0.012767 0.332986 0.036 Uiso 1 1 calc R U . . . C15 C 0.9026(2) 0.2175(4) 0.41334(14) 0.0307(5) Uani 1 1 d . . . . . H15 H 0.984100 0.249241 0.408244 0.037 Uiso 1 1 calc R U . . . C16 C 0.8461(2) 0.4328(4) 0.43903(13) 0.0292(5) Uani 1 1 d . . . . . H16A H 0.862298 0.559425 0.408729 0.035 Uiso 1 1 calc R U . . . H16B H 0.877708 0.469670 0.484778 0.035 Uiso 1 1 calc R U . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.0473(11) 0.0265(9) 0.0378(10) -0.0100(7) -0.0069(8) 0.0052(8) O2 0.0385(10) 0.0377(10) 0.0256(9) 0.0023(7) -0.0085(7) 0.0027(8) O3 0.0425(11) 0.0402(11) 0.0465(11) 0.0164(9) 0.0009(9) 0.0106(9) O4 0.0354(10) 0.0227(9) 0.0360(10) 0.0001(7) 0.0007(7) 0.0033(7) N1 0.0209(9) 0.0225(9) 0.0246(9) 0.0004(7) -0.0011(7) 0.0031(7) N2 0.0307(10) 0.0257(11) 0.0236(10) 0.0007(7) 0.0006(8) -0.0024(8) C1 0.0207(10) 0.0213(11) 0.0243(11) 0.0026(8) 0.0002(8) -0.0030(8) C2 0.0242(11) 0.0238(12) 0.0306(12) 0.0002(9) -0.0018(9) -0.0020(9) C3 0.0287(12) 0.0325(13) 0.0292(12) -0.0051(9) -0.0015(9) -0.0064(10) C4 0.0250(11) 0.0342(13) 0.0253(11) 0.0049(9) -0.0056(9) -0.0070(10) C5 0.0229(11) 0.0263(12) 0.0338(13) 0.0054(9) -0.0028(9) -0.0012(9) C6 0.0212(11) 0.0218(11) 0.0286(12) 0.0019(8) -0.0014(9) -0.0033(8) C7 0.0246(11) 0.0242(11) 0.0290(12) 0.0001(9) -0.0018(9) 0.0057(9) C8 0.0265(11) 0.0234(11) 0.0225(11) -0.0010(8) 0.0048(8) -0.0008(9) C9 0.0261(11) 0.0244(11) 0.0201(10) 0.0001(8) 0.0008(8) -0.0024(9) C10 0.0235(11) 0.0237(11) 0.0222(11) 0.0028(8) 0.0001(8) -0.0005(9) C11 0.0217(11) 0.0222(11) 0.0208(10) 0.0032(8) 0.0020(8) 0.0013(8) C12 0.0223(11) 0.0174(10) 0.0245(11) 0.0004(8) 0.0002(8) 0.0013(8) C13 0.0294(12) 0.0234(12) 0.0208(11) 0.0040(8) 0.0018(9) 0.0037(9) C14 0.0266(12) 0.0282(13) 0.0355(13) -0.0001(10) 0.0040(10) 0.0073(10) C15 0.0235(11) 0.0300(13) 0.0384(14) 0.0055(10) 0.0001(10) 0.0047(10) C16 0.0230(11) 0.0300(13) 0.0344(13) -0.0003(9) -0.0016(9) 0.0004(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1 N2 1.260(3) . ? O2 N2 1.247(3) . ? O3 H3 0.8200 . ? O3 C15 1.427(3) . ? O4 C13 1.214(3) . ? N1 C7 1.474(3) . ? N1 C8 1.321(3) . ? N1 C12 1.476(3) . ? N2 C9 1.398(3) . ? C1 C2 1.390(3) . ? C1 C6 1.392(3) . ? C1 C12 1.523(3) . ? C2 H2 0.9300 . ? C2 C3 1.394(3) . ? C3 H3A 0.9300 . ? C3 C4 1.384(3) . ? C4 H4 0.9300 . ? C4 C5 1.395(3) . ? C5 H5 0.9300 . ? C5 C6 1.389(3) . ? C6 C7 1.497(3) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 H8 0.9300 . ? C8 C9 1.366(3) . ? C9 C10 1.508(3) . ? C10 H10 0.9800 . ? C10 C11 1.565(3) . ? C10 C16 1.547(3) . ? C11 H11 0.9800 . ? C11 C12 1.537(3) . ? C11 C13 1.518(3) . ? C12 H12 0.9800 . ? C13 C14 1.504(3) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C14 C15 1.534(3) . ? C15 H15 0.9800 . ? C15 C16 1.518(3) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C15 O3 H3 109.5 . . ? C7 N1 C12 113.53(18) . . ? C8 N1 C7 123.4(2) . . ? C8 N1 C12 122.25(18) . . ? O1 N2 C9 120.1(2) . . ? O2 N2 O1 120.7(2) . . ? O2 N2 C9 119.2(2) . . ? C2 C1 C6 119.8(2) . . ? C2 C1 C12 129.7(2) . . ? C6 C1 C12 110.43(19) . . ? C1 C2 H2 120.6 . . ? C1 C2 C3 118.9(2) . . ? C3 C2 H2 120.6 . . ? C2 C3 H3A 119.5 . . ? C4 C3 C2 121.0(2) . . ? C4 C3 H3A 119.5 . . ? C3 C4 H4 119.9 . . ? C3 C4 C5 120.3(2) . . ? C5 C4 H4 119.9 . . ? C4 C5 H5 120.7 . . ? C6 C5 C4 118.6(2) . . ? C6 C5 H5 120.7 . . ? C1 C6 C7 111.2(2) . . ? C5 C6 C1 121.2(2) . . ? C5 C6 C7 127.5(2) . . ? N1 C7 C6 101.76(18) . . ? N1 C7 H7A 111.4 . . ? N1 C7 H7B 111.4 . . ? C6 C7 H7A 111.4 . . ? C6 C7 H7B 111.4 . . ? H7A C7 H7B 109.3 . . ? N1 C8 H8 118.7 . . ? N1 C8 C9 122.6(2) . . ? C9 C8 H8 118.7 . . ? N2 C9 C10 121.0(2) . . ? C8 C9 N2 116.3(2) . . ? C8 C9 C10 122.7(2) . . ? C9 C10 H10 109.1 . . ? C9 C10 C11 107.79(18) . . ? C9 C10 C16 114.42(19) . . ? C11 C10 H10 109.1 . . ? C16 C10 H10 109.1 . . ? C16 C10 C11 107.10(18) . . ? C10 C11 H11 108.0 . . ? C12 C11 C10 111.86(17) . . ? C12 C11 H11 108.0 . . ? C13 C11 C10 106.74(18) . . ? C13 C11 H11 108.0 . . ? C13 C11 C12 114.05(19) . . ? N1 C12 C1 101.25(17) . . ? N1 C12 C11 107.58(17) . . ? N1 C12 H12 109.9 . . ? C1 C12 C11 117.74(18) . . ? C1 C12 H12 109.9 . . ? C11 C12 H12 109.9 . . ? O4 C13 C11 123.2(2) . . ? O4 C13 C14 123.1(2) . . ? C14 C13 C11 113.7(2) . . ? C13 C14 H14A 109.4 . . ? C13 C14 H14B 109.4 . . ? C13 C14 C15 111.1(2) . . ? H14A C14 H14B 108.0 . . ? C15 C14 H14A 109.4 . . ? C15 C14 H14B 109.4 . . ? O3 C15 C14 107.8(2) . . ? O3 C15 H15 108.5 . . ? O3 C15 C16 111.2(2) . . ? C14 C15 H15 108.5 . . ? C16 C15 C14 112.3(2) . . ? C16 C15 H15 108.5 . . ? C10 C16 H16A 109.4 . . ? C10 C16 H16B 109.4 . . ? C15 C16 C10 111.1(2) . . ? C15 C16 H16A 109.4 . . ? C15 C16 H16B 109.4 . . ? H16A C16 H16B 108.0 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 N2 C9 C8 -12.8(3) . . . . ? O1 N2 C9 C10 168.7(2) . . . . ? O2 N2 C9 C8 166.3(2) . . . . ? O2 N2 C9 C10 -12.2(3) . . . . ? O3 C15 C16 C10 -66.3(3) . . . . ? O4 C13 C14 C15 -123.2(2) . . . . ? N1 C8 C9 N2 -169.6(2) . . . . ? N1 C8 C9 C10 8.8(3) . . . . ? N2 C9 C10 C11 -166.07(19) . . . . ? N2 C9 C10 C16 -47.1(3) . . . . ? C1 C2 C3 C4 0.8(3) . . . . ? C1 C6 C7 N1 10.2(2) . . . . ? C2 C1 C6 C5 -4.6(3) . . . . ? C2 C1 C6 C7 174.0(2) . . . . ? C2 C1 C12 N1 177.9(2) . . . . ? C2 C1 C12 C11 61.0(3) . . . . ? C2 C3 C4 C5 -3.5(4) . . . . ? C3 C4 C5 C6 2.1(3) . . . . ? C4 C5 C6 C1 2.0(3) . . . . ? C4 C5 C6 C7 -176.5(2) . . . . ? C5 C6 C7 N1 -171.2(2) . . . . ? C6 C1 C2 C3 3.2(3) . . . . ? C6 C1 C12 N1 -5.1(2) . . . . ? C6 C1 C12 C11 -122.0(2) . . . . ? C7 N1 C8 C9 -167.8(2) . . . . ? C7 N1 C12 C1 12.2(2) . . . . ? C7 N1 C12 C11 136.32(19) . . . . ? C8 N1 C7 C6 155.6(2) . . . . ? C8 N1 C12 C1 -157.6(2) . . . . ? C8 N1 C12 C11 -33.5(3) . . . . ? C8 C9 C10 C11 15.6(3) . . . . ? C8 C9 C10 C16 134.6(2) . . . . ? C9 C10 C11 C12 -47.9(2) . . . . ? C9 C10 C11 C13 -173.32(17) . . . . ? C9 C10 C16 C15 178.97(19) . . . . ? C10 C11 C12 N1 56.6(2) . . . . ? C10 C11 C12 C1 170.03(18) . . . . ? C10 C11 C13 O4 115.8(2) . . . . ? C10 C11 C13 C14 -61.4(2) . . . . ? C11 C10 C16 C15 -61.6(2) . . . . ? C11 C13 C14 C15 54.0(3) . . . . ? C12 N1 C7 C6 -14.1(2) . . . . ? C12 N1 C8 C9 1.0(3) . . . . ? C12 C1 C2 C3 179.9(2) . . . . ? C12 C1 C6 C5 178.0(2) . . . . ? C12 C1 C6 C7 -3.3(3) . . . . ? C12 C11 C13 O4 -8.3(3) . . . . ? C12 C11 C13 C14 174.52(19) . . . . ? C13 C11 C12 N1 177.85(17) . . . . ? C13 C11 C12 C1 -68.7(2) . . . . ? C13 C14 C15 O3 73.8(2) . . . . ? C13 C14 C15 C16 -49.1(3) . . . . ? C14 C15 C16 C10 54.7(3) . . . . ? C16 C10 C11 C12 -171.49(18) . . . . ? C16 C10 C11 C13 63.1(2) . . . . ? _shelx_res_file ; TITL glj-104_a.res in P2(1)/n glj-104.res created by SHELXL-2018/3 at 16:53:35 on 18-Oct-2021 REM Old TITL GLJ-104 in P2(1)/n REM SHELXT solution in P2(1)/n: R1 0.143, Rweak 0.471, Alpha 0.027 REM 0.468 for 257 systematic absences, Orientation as input REM Formula found by SHELXT: C16 N3 O3 CELL 1.54184 11.689044 5.846015 19.423305 90 92.7611 90 ZERR 4 0.000941 0.000414 0.00153 0 0.0072 0 LATT 1 SYMM 0.5-X,0.5+Y,0.5-Z SFAC C H N O UNIT 64 64 8 16 L.S. 20 PLAN 5 CONF BOND list 4 fmap 2 53 acta MORE -1 BOND $H REM REM REM WGHT 0.090600 0.068100 FVAR 6.86633 O1 4 0.650037 0.912165 0.542815 11.00000 0.04728 0.02650 = 0.03784 -0.00998 -0.00687 0.00518 O2 4 0.767704 0.630190 0.565741 11.00000 0.03846 0.03771 = 0.02559 0.00232 -0.00850 0.00273 O3 4 0.892882 0.033662 0.461078 11.00000 0.04250 0.04019 = 0.04646 0.01638 0.00089 0.01057 AFIX 83 H3 2 0.909223 0.079593 0.500213 11.00000 -1.50000 AFIX 0 O4 4 0.666265 -0.040703 0.330561 11.00000 0.03539 0.02271 = 0.03602 0.00012 0.00070 0.00328 N1 3 0.497725 0.578193 0.385797 11.00000 0.02086 0.02246 = 0.02463 0.00044 -0.00113 0.00306 N2 3 0.691929 0.721134 0.527554 11.00000 0.03068 0.02574 = 0.02361 0.00070 0.00064 -0.00242 C1 1 0.478859 0.350769 0.288147 11.00000 0.02075 0.02130 = 0.02430 0.00261 0.00020 -0.00297 C2 1 0.484725 0.186968 0.236540 11.00000 0.02422 0.02384 = 0.03059 0.00018 -0.00177 -0.00196 AFIX 43 H2 2 0.528980 0.056045 0.243493 11.00000 -1.20000 AFIX 0 C3 1 0.423147 0.222329 0.174203 11.00000 0.02870 0.03254 = 0.02918 -0.00514 -0.00150 -0.00638 AFIX 43 H3A 2 0.425739 0.112780 0.139595 11.00000 -1.20000 AFIX 0 C4 1 0.358210 0.417941 0.163019 11.00000 0.02495 0.03417 = 0.02532 0.00487 -0.00564 -0.00704 AFIX 43 H4 2 0.321029 0.442704 0.120258 11.00000 -1.20000 AFIX 0 C5 1 0.348304 0.578080 0.215617 11.00000 0.02287 0.02634 = 0.03385 0.00538 -0.00284 -0.00123 AFIX 43 H5 2 0.302834 0.707472 0.208929 11.00000 -1.20000 AFIX 0 C6 1 0.407800 0.540176 0.278196 11.00000 0.02118 0.02181 = 0.02856 0.00186 -0.00138 -0.00332 C7 1 0.404728 0.681574 0.342317 11.00000 0.02465 0.02419 = 0.02901 0.00013 -0.00176 0.00574 AFIX 23 H7A 2 0.419935 0.841451 0.333014 11.00000 -1.20000 H7B 2 0.331545 0.668176 0.363488 11.00000 -1.20000 AFIX 0 C8 1 0.553711 0.688703 0.436247 11.00000 0.02645 0.02338 = 0.02247 -0.00096 0.00481 -0.00083 AFIX 43 H8 2 0.524787 0.827704 0.450899 11.00000 -1.20000 AFIX 0 C9 1 0.652410 0.606987 0.467767 11.00000 0.02609 0.02441 = 0.02008 0.00007 0.00082 -0.00239 C10 1 0.714949 0.401478 0.441517 11.00000 0.02351 0.02368 = 0.02218 0.00280 0.00008 -0.00050 AFIX 13 H10 2 0.698992 0.268899 0.470404 11.00000 -1.20000 AFIX 0 C11 1 0.668160 0.353770 0.366045 11.00000 0.02166 0.02217 = 0.02084 0.00322 0.00196 0.00135 AFIX 13 H11 2 0.695732 0.475847 0.336496 11.00000 -1.20000 AFIX 0 C12 1 0.536531 0.355075 0.360141 11.00000 0.02233 0.01739 = 0.02449 0.00044 0.00023 0.00127 AFIX 13 H12 2 0.506345 0.231345 0.388069 11.00000 -1.20000 AFIX 0 C13 1 0.721638 0.130560 0.343941 11.00000 0.02944 0.02344 = 0.02078 0.00396 0.00182 0.00369 C14 1 0.850182 0.138192 0.343469 11.00000 0.02661 0.02822 = 0.03554 -0.00010 0.00405 0.00726 AFIX 23 H14A 2 0.873003 0.242171 0.307711 11.00000 -1.20000 H14B 2 0.879066 -0.012767 0.332986 11.00000 -1.20000 AFIX 0 C15 1 0.902627 0.217454 0.413345 11.00000 0.02347 0.03004 = 0.03836 0.00550 0.00009 0.00474 AFIX 13 H15 2 0.984100 0.249241 0.408244 11.00000 -1.20000 AFIX 0 C16 1 0.846068 0.432836 0.439034 11.00000 0.02303 0.03001 = 0.03441 -0.00032 -0.00161 0.00041 AFIX 23 H16A 2 0.862298 0.559425 0.408729 11.00000 -1.20000 H16B 2 0.877708 0.469670 0.484778 11.00000 -1.20000 AFIX 0 HKLF 4 REM glj-104_a.res in P2(1)/n REM wR2 = 0.1660, GooF = S = 1.070, Restrained GooF = 1.070 for all data REM R1 = 0.0576 for 2022 Fo > 4sig(Fo) and 0.0722 for all 2563 data REM 199 parameters refined using 0 restraints END WGHT 0.0906 0.0681 REM Highest difference peak 0.304, deepest hole -0.450, 1-sigma level 0.078 Q1 1 0.6860 0.2364 0.3557 11.00000 0.05 0.30 Q2 1 0.9685 0.0119 0.4816 11.00000 0.05 0.30 Q3 1 0.5359 0.3562 0.3177 11.00000 0.05 0.30 Q4 1 0.5964 -0.0254 0.3011 11.00000 0.05 0.29 Q5 1 0.5841 -0.2961 0.3042 11.00000 0.05 0.27 ; _shelx_res_checksum 10501 _shelx_hkl_file ; 0 0 1 21.5303 20.8967 4 0 0 2 39373.4 921.584 4 0 0 3 67.0621 91.1937 4 0 0 4 49376.9 1642.19 4 0 0 5-86.4529 166.763 4 0 0 6 60181.6 2160.56 4 0 0 7-42.8124 196.569 4 0 0 8 178542. 4373.77 4 0 0 9 239.084 285.908 4 0 0 9 119.566 81.8062 2 0 0 10 423897. 7887.74 4 0 0 11 243.073 897.923 4 0 0 12 8180.48 1279.20 4 0 0 13-168.391 285.384 4 0 0 14 1026.54 539.299 4 0 0 -14 1294.65 331.918 9 0 0 15-59.6062 377.191 4 0 0 -15-193.431 259.274 9 0 0 -16 29280.0 1892.92 9 0 0 16 29456.5 3012.36 4 0 0 -17 4.41009 179.974 9 0 0 -18 22033.2 1670.29 9 0 0 -19-12.4734 215.783 9 0 0 -20 6499.91 857.688 9 0 0 -21-74.7126 113.327 9 0 0 -22 9697.83 825.421 9 0 0 -23-84.6113 122.462 9 0 1 0-22.8580 35.2147 3 0 1 -1 38417.3 753.807 3 0 1 -2 127958. 1455.95 2 0 1 -2 131838. 1620.49 3 0 -1 3 18582.6 839.890 4 0 1 -3 20261.2 759.049 3 0 1 3 19574.3 957.925 4 0 1 4 142894. 2862.04 4 0 -1 4 145704. 2669.50 4 0 -1 5 135735. 2870.16 4 0 1 5 137693. 3115.41 4 0 1 6 31831.0 1662.87 4 0 -1 6 34337.7 1607.90 4 0 -1 7 79860.0 2720.29 4 0 1 7 76523.5 2800.79 4 0 1 8 229.512 399.384 4 0 -1 8 379.331 256.905 4 0 1 9 78576.5 3303.63 4 0 -1 9 79488.3 3213.79 4 0 -1 10 19848.8 1791.56 4 0 1 10 19848.9 1775.90 4 0 1 10 19946.3 1281.32 2 0 -1 11 23837.0 2057.66 4 0 1 11 24682.2 2118.53 4 0 1 11 28407.9 1590.91 2 0 1 12 8832.59 1383.21 4 0 -1 12 9851.81 1420.88 4 0 1 13 865.406 538.584 4 0 -1 13 1777.44 704.664 4 0 1 14 5055.42 1139.37 4 0 1 -14 6275.26 897.289 9 0 -1 14 4988.32 1100.87 4 0 1 -15 61297.3 2775.98 9 0 1 15 58896.4 4168.83 4 0 -1 15 60749.2 4201.63 4 0 -1 16 40361.9 3593.29 4 0 1 -16 41072.6 2313.58 9 0 1 16 43676.7 3723.93 4 0 1 -17 9278.41 1154.06 9 0 1 -18 8125.34 1041.26 9 0 1 -19 5436.81 835.062 9 0 1 -20 354.778 228.315 9 0 1 -21-130.194 226.554 9 0 1 -22-69.7275 119.652 9 0 1 -23 6086.01 570.350 9 0 2 0 12019.6 586.589 3 0 2 1 21921.1 806.480 3 0 2 -1 23421.8 1102.09 2 0 2 -1 23021.4 780.833 3 0 2 -2 1358.23 196.849 3 0 2 2 1451.38 229.728 3 0 2 -2 1109.11 233.492 2 0 2 -3 8766.69 585.258 2 0 -2 3 8552.73 643.296 4 0 2 -3 8725.49 555.204 3 0 -2 4 11290.7 821.560 4 0 2 -4 11834.3 732.466 3 0 -2 5 6598.60 696.030 4 0 2 5 7773.52 794.751 4 0 2 6 1583.45 395.800 4 0 -2 6 1453.15 372.952 4 0 2 7 452.375 252.158 4 0 -2 7 97.6403 248.539 4 0 -2 8 4705.27 770.412 4 0 2 8 5249.19 874.672 4 0 2 9 32023.5 1868.32 2 0 -2 9 31790.9 2176.36 4 0 2 9 29106.6 2185.33 4 0 2 10 2680.66 722.563 4 0 2 10 2462.95 561.144 2 0 -2 10 2686.82 756.233 4 0 -2 11 16323.8 1807.90 4 0 2 11 15055.2 1387.57 2 0 2 11 15609.6 1792.86 4 0 2 12 17901.0 1550.98 2 0 -2 12 16826.0 1949.29 4 0 2 12 16481.1 1941.23 4 0 -2 13 30226.4 2760.58 4 0 2 13 36188.3 2247.99 2 0 2 13 32719.4 2882.55 4 0 2 -13 29839.5 1678.18 7 0 2 -13 31017.3 1903.69 9 0 2 14 4188.28 1207.55 4 0 -2 14 5179.13 1228.94 4 0 2 -14 3696.47 684.308 9 0 2 15 277.170 431.432 4 0 2 -15 95.2327 185.793 9 0 2 -16 625.260 290.825 9 0 2 -17 31028.3 2020.33 9 0 2 -18 16844.0 1446.92 9 0 2 -19 4011.91 670.494 9 0 2 -20 33.4289 159.735 9 0 2 -21 233.200 174.097 9 0 2 -22-140.401 153.538 9 0 2 -23 4313.85 429.391 9 0 3 0-184.368 213.701 2 0 3 1 140214. 3676.12 2 0 3 -1 138561. 3364.08 2 0 3 -2 7886.17 770.976 2 0 3 2 6191.62 798.519 2 0 3 3 2711.24 390.827 3 0 3 3 2537.32 508.922 2 0 3 -3 2466.71 403.229 2 0 3 4 16468.5 1383.50 2 0 3 4 18022.5 1077.12 3 0 3 5 10094.3 866.695 3 0 3 5 9366.65 1091.44 2 0 3 6 66659.6 2917.97 2 0 3 6 61816.0 2289.89 3 0 3 7 435.683 296.419 2 0 3 8 7833.79 1066.27 2 0 3 9 15150.8 1527.25 2 0 3 10 6824.39 1027.74 2 0 3 -10 8819.97 875.233 8 0 3 -10 7679.49 903.933 7 0 3 -11 19318.6 1293.12 8 0 3 -11 18121.8 1392.91 7 0 3 -11 18343.6 1388.56 9 0 3 11 17676.5 1718.32 2 0 3 -12 73253.2 2864.70 9 0 3 12 70184.9 3479.77 2 0 3 -12 75960.4 2899.71 7 0 3 -13 333.918 213.948 7 0 3 -13 713.883 315.757 9 0 3 13 600.679 283.410 2 0 3 -14 20799.6 1588.25 9 0 3 -15 1631.61 434.243 9 0 3 -16 196.862 214.911 9 0 3 -17 453.233 246.790 9 0 3 -18-220.276 189.290 9 0 3 -19 5824.46 720.071 9 0 3 -20 1770.53 360.290 9 0 3 21 634.492 230.081 5 0 3 -21 424.639 177.743 9 0 4 0 67205.5 2975.60 2 0 4 -1 3134.09 615.767 2 0 4 1 3591.25 697.171 2 0 4 2 698.841 348.652 2 0 4 3 232.043 212.321 2 0 4 -4 20350.1 1293.65 5 0 4 4 18983.2 1360.81 5 0 4 4 18518.3 1762.73 2 0 4 5 23044.2 1543.21 5 0 4 5 24747.7 2040.19 2 0 4 -5 26092.1 1573.42 7 0 4 -5 24251.1 1425.00 8 0 4 -5 24272.2 1428.42 5 0 4 -6 138.896 211.690 7 0 4 6 30.3654 175.816 5 0 4 -6-23.9696 136.062 8 0 4 6 179.631 159.830 2 0 4 -7 2763.76 591.272 7 0 4 7 3117.02 607.063 5 0 4 7 2325.21 658.771 2 0 4 -7 2320.91 452.247 8 0 4 -8 179.263 210.015 7 0 4 8 156.226 279.537 5 0 4 8-129.126 351.040 2 0 4 -8-110.173 111.615 8 0 4 -9 20364.8 1547.22 7 0 4 9 20670.6 2013.32 2 0 4 -9 23637.1 1454.34 8 0 4 9 21840.5 1612.34 5 0 4 -10 30117.6 1650.72 8 0 4 10 27061.4 1807.48 5 0 4 -10 28142.2 1838.64 7 0 4 -11 129504. 3395.50 8 0 4 -11 134628. 4015.54 7 0 4 11 122688. 3827.61 5 0 4 12 5581.10 810.159 5 0 4 13 7880.42 969.949 5 0 4 14 21941.4 1569.59 5 0 4 15 762.130 360.741 5 0 4 16 313.929 175.381 5 0 4 -17 268.752 151.332 9 0 4 17 70.8718 204.152 5 0 4 18 558.904 211.477 5 0 4 19 4485.13 504.223 5 0 4 20 3988.83 410.728 5 0 5 0-325.071 255.355 5 0 5 -1 158.842 188.278 5 0 5 1 254.541 278.825 5 0 5 -2 31431.8 1811.43 5 0 5 2 29479.5 1841.85 5 0 5 3 7020.35 908.409 5 0 5 -3 8012.83 957.570 5 0 5 -4 54947.3 2212.00 8 0 5 4 60119.3 2665.72 5 0 5 5 26434.7 1783.57 5 0 5 -5 26806.1 1541.48 8 0 5 -6 20451.5 1329.73 8 0 5 6 21569.0 1620.03 5 0 5 -7 2069.84 436.691 8 0 5 7 2529.80 623.457 5 0 5 8 134.834 256.877 5 0 5 -8-111.342 172.221 8 0 5 9 848.153 241.409 5 0 5 -9 747.797 280.672 8 0 5 10 1526.65 437.450 5 0 5 11 1161.54 350.087 5 0 5 12 7024.08 859.125 5 0 5 13 8067.39 859.128 5 0 5 14 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10 1 9 1404.54 483.325 6 10 -1 9 1587.89 528.710 6 10 1 10 146.435 184.768 6 10 -1 10 217.186 280.602 6 10 1 11 3716.70 674.646 6 10 -1 11 2955.71 660.968 6 10 1 12 931.240 329.380 6 10 -1 12 1226.20 421.344 6 10 1 13 146.730 153.784 6 10 -1 13 152.367 259.623 6 10 -1 14 1903.98 479.500 6 10 1 14 1501.53 381.311 6 10 -1 15 13707.9 1129.29 6 10 -1 16-287.448 195.429 6 10 2 -17 358.979 128.917 9 10 2 -16 2010.13 354.735 9 10 2 -15 1635.25 397.285 9 10 2 -14 3322.08 567.143 9 10 2 -14 2524.35 391.643 7 10 2 -13 1621.48 444.051 9 10 2 -13 1597.99 367.380 7 10 2 -12 1282.67 359.685 7 10 -2 -12 1735.72 447.979 6 10 2 -11 3546.02 622.804 7 10 -2 -11 2901.45 654.956 6 10 2 -10 429.375 269.557 7 10 2 -10 636.780 285.563 6 10 -2 -10 620.934 335.337 6 10 2 -9 6328.19 863.895 6 10 -2 -9 5655.26 933.873 6 10 2 -8 5317.56 780.463 6 10 -2 -8 5384.59 900.453 6 10 -2 -7 1383.04 454.789 6 10 -2 -6 1986.72 547.764 6 10 -2 -5 2937.28 728.633 6 10 -2 -4-5.64774 343.645 6 10 -2 -3 6511.70 1038.36 6 10 -2 -2 2252.92 746.082 6 10 -2 -1 396.431 217.608 6 10 -2 0 5975.11 994.508 6 10 -2 1 13700.2 1461.74 6 10 -2 2 190.803 395.718 6 10 -2 3 11087.1 1313.20 6 10 -2 4 1079.10 406.338 6 10 -2 5 25928.5 1971.01 6 10 -2 6 767.893 384.181 6 10 2 6 718.972 245.045 8 10 2 7 14825.7 1248.80 8 10 -2 7 12541.3 1341.86 6 10 -2 8-262.988 204.728 6 10 2 8-398.868 234.821 8 10 -2 9 6442.61 934.660 6 10 2 9 5851.13 772.776 8 10 -2 10 597.204 353.985 6 10 2 10 155.039 185.751 8 10 -2 11 1464.86 437.782 6 10 2 11 1391.64 378.253 8 10 -2 12 5929.23 790.737 6 10 2 12 4614.46 622.204 8 10 -2 13 344.948 200.335 6 10 2 13 148.627 132.793 8 10 -2 14 0.94808 144.076 6 10 2 14 462.119 203.187 8 10 -2 15 1441.81 318.947 6 10 3 -14 2076.81 337.980 9 10 3 -14 2385.27 339.543 7 10 3 -13 330.300 149.512 9 10 3 -13 330.518 170.632 7 10 3 -12 2724.00 487.925 9 10 3 -12 3262.13 504.379 7 10 3 -11 726.653 252.590 9 10 3 -11 475.142 232.579 7 10 3 -10 11273.5 1059.58 7 10 3 -9 2284.08 516.480 7 10 3 -8 5737.35 812.216 7 10 -3 -8 6602.01 845.451 6 10 3 -7 6320.35 911.032 7 10 -3 -7 6936.18 898.459 6 10 -3 -6 864.781 346.960 6 10 -3 -5-151.615 236.132 6 10 -3 -4 7916.44 1021.35 6 10 -3 -3 523.693 339.743 6 10 -3 -2 2576.49 640.457 6 10 3 -1 2230.16 446.834 8 10 -3 -1 1691.12 486.840 6 10 3 0 1172.55 313.654 8 10 -3 0 1630.37 467.712 6 10 3 1 5265.02 722.201 8 10 -3 1 4805.72 827.568 6 10 3 2 11255.7 1066.08 8 10 -3 2 10317.3 1170.57 6 10 3 3 1365.30 415.223 8 10 -3 3 1240.75 465.305 6 10 3 4 1883.20 485.314 8 10 -3 4 1227.38 413.363 6 10 3 5 10371.0 1051.37 8 10 -3 5 9079.10 1048.28 6 10 3 6 52.2915 158.932 8 10 -3 6-286.806 246.691 6 10 3 7 97.5049 142.245 8 10 -3 7 635.880 271.511 6 10 3 8 14742.9 1186.76 8 10 -3 8 14428.8 1217.05 6 10 3 9 98.9834 163.155 8 10 -3 9 183.426 186.108 6 10 3 10 274.396 174.675 8 10 -3 10 284.500 240.676 6 10 3 11 1312.19 344.298 8 10 -3 11 987.409 300.659 6 10 3 12 429.967 178.374 8 10 -3 12 373.102 140.318 6 10 3 13-219.772 164.512 8 10 4 -12 2729.24 345.745 7 10 4 -11 1832.06 326.707 7 10 4 -10 19246.6 1098.67 7 10 4 -9 2092.21 392.123 7 10 4 -8 5668.55 669.524 7 10 4 -7 3570.12 548.415 7 10 4 -6 434.339 171.688 8 10 4 -6 262.355 199.250 7 10 4 -5 364.480 172.241 8 10 4 -5 198.584 121.360 7 10 4 -4 248.524 101.739 8 10 4 -4 461.427 260.875 7 10 4 -3 1033.76 277.293 8 10 4 -3 1466.90 400.545 7 10 4 -2 10764.1 894.014 8 10 4 -2 9002.98 870.704 7 10 4 -1-201.825 156.488 8 10 4 -1 350.523 191.820 7 10 4 0 17149.4 1171.22 8 10 4 1 534.063 231.397 8 10 4 2 598.478 236.714 8 10 4 3 2381.27 459.252 8 10 4 4-145.279 207.206 8 10 4 5 300.888 197.682 8 10 4 6 551.148 257.096 8 10 4 7 150.861 105.914 8 10 4 8 7111.73 686.816 8 10 4 9 296.100 108.531 8 10 4 10 1155.78 248.680 8 10 5 -3 2210.38 282.597 8 10 5 -2 480.982 139.293 8 10 5 -1 3271.09 369.667 8 10 5 0 1422.95 262.320 8 10 5 1 109.396 83.8130 8 10 5 2 3901.49 409.469 8 10 5 3 361.216 160.024 8 10 5 4 580.640 166.659 8 11 0 -15 53.1261 126.921 9 11 0 -14-102.052 140.948 9 11 0 -13 23.9488 244.804 6 11 0 -12 47.4331 149.232 6 11 0 -11 396.703 264.014 6 11 0 -10 106.296 278.331 6 11 0 -9 9483.80 1157.83 6 11 0 -8 433.743 328.671 6 11 0 -7 421.843 308.984 6 11 0 -6-245.544 335.777 6 11 0 -5 1782.66 581.732 6 11 0 -4 147.311 229.175 6 11 0 -3 22423.7 1939.64 6 11 0 -2-52.7073 255.766 6 11 0 -1 4287.70 846.025 6 11 0 0-15.0019 234.905 6 11 0 1 318.905 358.471 6 11 0 2-55.5558 383.081 6 11 0 3 5241.28 921.218 6 11 0 4-49.1043 229.927 6 11 0 5 2795.52 645.794 6 11 0 6-109.369 268.756 6 11 0 7 3211.03 703.557 6 11 0 8 186.700 316.358 6 11 0 9-248.978 450.582 6 11 0 10-82.8779 195.459 6 11 0 11 437.197 282.253 6 11 0 12 12.6288 186.088 6 11 0 13-98.9839 214.355 6 11 0 14-90.0029 215.929 6 11 1 -16 129.752 120.120 9 11 1 -15 1146.63 281.713 9 11 1 -14 52.8239 129.852 9 11 -1 -13 275.807 350.704 6 11 1 -12 3512.81 510.652 7 11 1 -12 3896.39 628.618 6 11 -1 -12 3583.12 638.531 6 11 1 -11 169.203 189.865 7 11 1 -11-108.802 177.087 6 11 1 -10 12507.2 1214.76 6 11 -1 -10 12605.2 1288.87 6 11 1 -9 98.8934 192.518 6 11 -1 -9-180.000 261.151 6 11 1 -8 434.485 281.062 6 11 -1 -8 169.406 254.800 6 11 1 -7 360.437 325.767 6 11 -1 -7 363.207 342.743 6 11 1 -6 1816.58 501.970 6 11 -1 -6 2065.35 648.868 6 11 1 -5 2831.52 674.804 6 11 -1 -5 3448.71 778.011 6 11 1 -4 3003.11 675.825 6 11 -1 -4 2600.98 681.698 6 11 1 -3 576.679 337.810 6 11 -1 -3 664.880 421.459 6 11 1 -2 6236.71 992.566 6 11 -1 -2 6854.83 1085.43 6 11 1 -1 10.4583 248.512 6 11 -1 -1 326.391 372.467 6 11 1 0 3621.90 752.912 6 11 -1 0 3623.02 819.093 6 11 1 1 3062.03 713.682 6 11 -1 1 3710.71 785.982 6 11 1 2-144.701 355.242 6 11 -1 2 79.1878 216.848 6 11 1 3 4201.76 815.696 6 11 -1 3 4101.41 739.613 6 11 1 4 4032.20 761.989 6 11 -1 4 4210.50 774.886 6 11 1 5 22558.6 1932.43 6 11 -1 5 18080.5 1698.18 6 11 1 6 29902.4 1994.45 6 11 -1 6 28572.4 2043.55 6 11 1 7 5699.90 880.130 6 11 -1 7 5675.55 947.173 6 11 1 8 1097.38 414.853 6 11 -1 8 1507.82 503.224 6 11 1 9-51.0654 271.020 6 11 -1 9-46.6306 234.073 6 11 1 10 6699.23 839.510 6 11 -1 10 6936.86 950.104 6 11 1 11 3049.76 547.209 6 11 -1 11 3646.46 661.909 6 11 1 12 1635.50 364.108 6 11 -1 12 1540.63 479.033 6 11 -1 13 2091.35 456.017 6 11 -1 14 60.0634 120.206 6 11 2 -15 397.519 154.803 9 11 2 -14-56.6513 117.869 9 11 2 -13 6272.87 576.109 7 11 2 -13 6515.95 754.073 9 11 2 -12 1092.60 277.401 7 11 -2 -12 1186.91 342.225 6 11 2 -11 71.3889 112.943 7 11 -2 -11 130.417 230.860 6 11 2 -10 10837.5 1022.10 7 11 -2 -10 10990.7 1112.99 6 11 -2 -9 472.715 201.414 6 11 -2 -8 4525.14 769.498 6 11 -2 -7 4919.95 861.556 6 11 -2 -6 3703.69 745.331 6 11 -2 -5 8081.39 1100.54 6 11 -2 -4 2645.83 645.900 6 11 -2 -3 3120.85 730.719 6 11 -2 -2 4430.80 822.037 6 11 -2 -1 116.950 215.100 6 11 -2 0 355.267 259.116 6 11 -2 1 1741.80 549.410 6 11 -2 2-77.3713 286.255 6 11 -2 3 11219.3 1265.88 6 11 -2 4 6427.74 964.093 6 11 -2 5 3397.50 693.806 6 11 -2 6 6114.60 910.941 6 11 -2 7 3279.67 678.894 6 11 -2 8 1361.21 445.107 6 11 -2 9 8826.63 974.405 6 11 -2 10 173.508 221.686 6 11 -2 11 3668.24 596.345 6 11 -2 12 5173.73 629.608 6 11 -2 13 33.3414 111.686 6 11 3 -12 758.419 205.029 9 11 3 -12 731.353 206.611 7 11 3 -11 469.963 212.754 9 11 3 -11 978.277 257.248 7 11 3 -10 1510.95 351.095 9 11 3 -10 2553.02 439.630 7 11 3 -9 5567.23 689.476 7 11 3 -8 1472.95 417.013 7 11 3 -7 1343.64 384.919 7 11 -3 -7 1030.45 332.504 6 11 3 -6 3637.80 631.246 7 11 -3 -6 3217.23 550.654 6 11 3 -5 5442.16 772.737 7 11 -3 -5 6094.38 781.401 6 11 -3 -4 5359.45 770.415 6 11 -3 -3-385.505 227.941 6 11 -3 -2 1047.10 400.137 6 11 -3 -1-115.844 319.223 6 11 -3 0-122.207 223.864 6 11 -3 1 20306.0 1507.42 6 11 -3 2 367.958 264.511 6 11 -3 3 2190.97 522.407 6 11 -3 4 632.757 293.905 6 11 3 5 2191.06 416.115 8 11 -3 5 1661.11 403.878 6 11 3 6 126.579 137.417 8 11 -3 6 100.082 159.422 6 11 3 7 2148.53 397.688 8 11 -3 7 2644.31 474.177 6 11 3 8 210.911 109.151 8 11 -3 8 643.554 215.670 6 11 3 9 656.838 244.078 8 11 -3 9 806.034 232.246 6 11 -3 10 984.241 243.173 6 11 4 -9 405.601 156.005 7 11 4 -8 15490.3 886.846 7 11 4 -7-138.326 156.868 7 11 4 -6 91.9758 139.619 7 11 4 -5 2714.35 412.578 7 11 4 -4 3992.66 491.109 7 11 4 -3 993.626 256.971 7 11 4 -2 359.640 158.849 7 11 4 1 279.574 156.601 8 11 4 2 791.637 212.877 8 11 4 3 303.073 134.968 8 11 4 4 2.29107 104.290 8 11 4 5 1164.89 244.093 8 12 0 -13 20.5343 113.501 9 12 0 -12 402.061 180.161 6 12 0 -11 107.272 191.618 6 12 0 -10 1705.41 421.270 6 12 0 -9 128.157 180.080 6 12 0 -8 1179.92 444.381 6 12 0 -7 16.4441 179.375 6 12 0 -6 16619.9 1496.21 6 12 0 -5-24.3856 330.779 6 12 0 -4 653.318 385.654 6 12 0 -3 265.691 346.973 6 12 0 -2 2808.86 745.271 6 12 0 -1-96.9351 233.479 6 12 0 0 19670.3 1714.03 6 12 0 1-590.803 329.179 6 12 0 2 46070.6 2578.02 6 12 0 3 236.954 321.657 6 12 0 4 2016.44 565.098 6 12 0 5 143.889 195.020 6 12 0 6 14010.7 1344.27 6 12 0 7 59.5170 274.045 6 12 0 8 335.332 260.568 6 12 0 9-245.869 296.636 6 12 0 10 1952.50 454.312 6 12 0 11 466.615 239.085 6 12 0 12-55.8861 132.146 6 12 1 -14 989.854 231.024 9 12 1 -13 914.279 265.256 9 12 -1 -12 143.457 181.132 6 12 1 -11 232.812 163.527 7 12 1 -11-179.429 178.719 6 12 -1 -11 160.107 182.891 6 12 1 -10 4785.81 612.852 7 12 1 -10 5720.71 728.115 6 12 -1 -10 5577.06 756.038 6 12 1 -9 3046.06 566.264 6 12 -1 -9 2210.15 526.423 6 12 1 -8 4324.95 700.377 6 12 -1 -8 4797.13 773.063 6 12 1 -7 778.107 293.175 6 12 -1 -7 211.047 303.154 6 12 1 -6 6119.71 865.758 6 12 -1 -6 5677.17 877.725 6 12 1 -5 31.5494 201.613 6 12 -1 -5 9.60024 230.124 6 12 1 -4-255.770 235.796 6 12 -1 -4 19.7497 231.284 6 12 1 -3-175.045 306.591 6 12 -1 -3-150.965 207.801 6 12 1 -2 967.757 418.859 6 12 -1 -2 763.072 453.766 6 12 1 -1 145.881 183.570 6 12 -1 -1 253.526 269.133 6 12 1 0-133.171 307.693 6 12 -1 0-57.6828 214.314 6 12 1 1 200.095 248.936 6 12 -1 1-382.226 416.488 6 12 1 2 2884.04 634.482 6 12 -1 2 2112.06 619.088 6 12 1 3 882.245 388.415 6 12 -1 3 631.687 387.067 6 12 1 4 19366.7 1522.92 6 12 -1 4 19684.8 1637.33 6 12 1 5 3430.12 619.494 6 12 -1 5 3329.69 694.491 6 12 1 6 8004.40 930.901 6 12 -1 6 7589.23 1043.75 6 12 1 7-20.1908 192.515 6 12 -1 7 744.976 403.932 6 12 1 8 1700.18 423.668 6 12 -1 8 2030.10 519.381 6 12 1 9 3710.52 571.095 6 12 -1 9 3845.44 670.212 6 12 -1 10 2524.93 493.341 6 12 -1 11 2609.06 465.707 6 12 -1 12 1025.17 298.723 6 12 2 -12 1679.05 326.674 9 12 2 -11 808.877 227.285 7 12 -2 -11 1306.56 320.183 6 12 2 -10 3033.39 453.688 7 12 -2 -10 2680.81 464.080 6 12 2 -9 132.862 152.597 7 12 -2 -9 278.340 219.310 6 12 2 -8-24.5029 141.843 7 12 -2 -8 175.162 228.157 6 12 -2 -7 1141.31 370.130 6 12 -2 -6 43.5620 223.128 6 12 -2 -5 729.182 300.762 6 12 -2 -4 1595.60 450.547 6 12 -2 -3-90.3867 308.255 6 12 -2 -2 187.863 236.016 6 12 -2 -1 747.778 336.340 6 12 -2 0 811.043 347.798 6 12 -2 1 4799.73 794.321 6 12 -2 2 1546.34 449.433 6 12 -2 3-146.023 202.224 6 12 -2 4 4506.91 743.402 6 12 -2 5-257.296 251.425 6 12 -2 6 164.055 193.417 6 12 -2 7 987.553 357.423 6 12 -2 8 624.119 269.375 6 12 -2 9 2069.29 418.137 6 12 -2 10 1597.03 325.534 6 12 3 -10 1230.71 245.654 7 12 3 -9 468.757 191.898 7 12 3 -8 1409.80 285.259 9 12 3 -8 1658.66 330.524 7 12 3 -7 21503.8 1200.94 7 12 3 -6 747.790 250.802 7 12 3 -5 2790.50 468.236 7 12 -3 -5 2467.54 405.834 6 12 3 -4 642.232 215.885 7 12 -3 -4 973.309 266.159 6 12 3 -3 177.862 178.944 7 12 -3 -3 147.287 150.953 6 12 3 -2 173.983 147.209 7 12 -3 -2 175.970 254.236 6 12 -3 -1 936.974 308.048 6 12 -3 0 2728.80 501.994 6 12 -3 1 1185.10 318.128 6 12 -3 2 3519.89 547.832 6 12 -3 3 10458.2 876.291 6 12 -3 4 781.100 225.767 6 12 -3 5-114.539 137.661 6 12 -3 6 505.400 221.289 6 13 0 -10 174.177 147.200 6 13 0 -9 1650.32 390.893 6 13 0 -8-55.3829 186.278 6 13 0 -7 1244.84 402.243 6 13 0 -6 120.209 243.475 6 13 0 -5 1706.79 455.472 6 13 0 -4 166.509 209.082 6 13 0 -3 898.664 344.158 6 13 0 -2-213.634 240.203 6 13 0 -1 1822.91 463.153 6 13 0 0-15.2447 193.790 6 13 0 1 5853.08 873.267 6 13 0 2-91.9150 220.944 6 13 0 3 11361.5 1145.76 6 13 0 4 381.696 244.343 6 13 0 5 10942.4 1061.06 6 13 0 6-115.636 147.671 6 13 0 7 1968.61 445.489 6 13 0 8 54.2282 155.509 6 13 0 9 2454.56 416.723 6 13 -1 -10 2000.61 377.850 6 13 1 -9 707.971 219.110 7 13 1 -9 222.558 134.009 6 13 -1 -9 310.449 170.367 6 13 1 -8 1398.90 330.674 6 13 -1 -8 1537.52 396.073 6 13 1 -7 209.820 196.358 6 13 -1 -7 45.2893 155.838 6 13 1 -6 8976.26 865.943 6 13 -1 -6 9517.73 977.145 6 13 1 -5 5101.75 675.107 6 13 -1 -5 3660.10 624.943 6 13 1 -4-158.832 229.860 6 13 -1 -4-10.0604 178.006 6 13 1 -3 1534.08 449.725 6 13 -1 -3 1466.56 472.670 6 13 1 -2-56.6662 190.210 6 13 -1 -2 182.923 260.195 6 13 1 -1 395.388 322.180 6 13 -1 -1 182.229 259.418 6 13 1 0 350.911 140.933 6 13 -1 0 737.413 326.312 6 13 1 1 4006.80 631.857 6 13 -1 1 4187.67 721.576 6 13 1 2 15355.2 1192.36 6 13 -1 2 15047.4 1308.68 6 13 1 3 1795.04 431.914 6 13 -1 3 1590.61 475.189 6 13 1 4-167.605 170.697 6 13 -1 4 126.253 197.659 6 13 1 5 231.693 188.995 6 13 -1 5 375.853 266.727 6 13 1 6 7611.90 718.120 6 13 -1 6 8045.46 885.226 6 13 -1 7-435.473 205.285 6 13 -1 8 6382.11 705.412 6 13 -1 9 2447.66 425.024 6 13 2 -9 809.921 198.048 7 13 2 -8-34.7848 116.289 7 13 -2 -8 138.586 168.117 6 13 2 -7 1058.34 281.904 7 13 -2 -7 819.638 245.738 6 13 2 -6 2268.16 411.106 7 13 -2 -6 1975.92 395.107 6 13 -2 -5 1772.79 383.938 6 13 -2 -4 18164.6 1239.20 6 13 -2 -3 1398.21 410.542 6 13 -2 -2 13441.8 1104.36 6 13 -2 -1 1053.96 324.595 6 13 -2 0 4155.24 623.656 6 13 -2 1 7208.60 806.595 6 13 -2 2 210.998 218.832 6 13 -2 3 104.250 167.666 6 13 -2 4 507.074 252.687 6 13 -2 5 69.0890 116.330 6 13 -2 6 6207.05 650.842 6 13 -2 7 6433.59 622.870 6 13 3 -5 158.637 82.1938 7 13 3 -4 1636.82 280.390 7 13 3 -3 187.703 122.684 7 13 3 -2 395.399 158.859 7 14 0 -7 8.70625 99.8612 6 14 0 -6-51.8853 144.492 6 14 0 -5 152.864 100.909 6 14 0 -4 110.152 155.922 6 14 0 -3 327.152 220.618 6 14 0 -2 40.1058 133.568 6 14 0 -1 13.5867 141.645 6 14 0 0 4551.12 603.830 6 14 0 1-140.252 118.918 6 14 0 2 182.749 175.737 6 14 0 3-190.997 197.900 6 14 0 4 416.298 201.696 6 14 -1 -6 2291.03 364.980 6 14 -1 -5 1193.11 274.116 6 14 -1 -4 707.770 217.619 6 14 -1 -3 1557.69 363.988 6 14 -1 -2-121.192 136.938 6 14 -1 -1 6674.02 705.467 6 14 -1 0 109.832 121.895 6 14 -1 1 564.280 225.991 6 14 -1 2 4079.38 546.434 6 14 -1 3 14519.1 997.426 6 14 -1 4 1497.87 326.947 6 0 0 0 0.00 0.00 0 TITL GLJ-104 in P2(1)/n REM P2(1)/n (#14 in standard setting) CELL 1.54184 11.689044 5.846015 19.423305 90.0000 92.7611 90.0000 ZERR 6.00 0.000941 0.000414 0.001530 0.0000 0.0072 0.0000 LATT 1 SYMM -x+1/2, y+1/2,-z+1/2 SFAC C H N O UNIT 66.00 60.00 6.00 6.00 TREF HKLF 4 END ; _shelx_hkl_checksum 99667 _olex2_date_sample_data_collection 2021-10-18 _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; _oxdiff_exptl_absorpt_empirical_full_max 1.676 _oxdiff_exptl_absorpt_empirical_full_min 0.648 ####################################################################### # # This file contains crystal structure data downloaded from the # Cambridge Structural Database (CSD) hosted by the Cambridge # Crystallographic Data Centre (CCDC). # # Full information about CCDC data access policies and citation # guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 # # Audit and citation data items may have been added by the CCDC. # Please retain this information to preserve the provenance of # this file and to allow appropriate attribution of the data. # ####################################################################### data_a _database_code_depnum_ccdc_archive 'CCDC 2071228' loop_ _audit_author_name _audit_author_address 'Qilin Wang' ;Henan University China ; _audit_update_record ; 2021-03-18 deposited with the CCDC. 2021-11-08 downloaded from the CCDC. ; _audit_creation_date 2019-10-15 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _shelx_SHELXL_version_number 2014/7 _chemical_name_common ? _chemical_name_systematic ? _chemical_formula_moiety 'C27 H23 N3 O5' _chemical_formula_sum 'C27 H23 N3 O5' _chemical_formula_weight 469.48 _chemical_melting_point ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.719(3) _cell_length_b 11.529(5) _cell_length_c 12.887(5) _cell_angle_alpha 86.887(13) _cell_angle_beta 72.756(13) _cell_angle_gamma 74.684(12) _cell_volume 1192.8(8) _cell_formula_units_Z 2 _cell_measurement_reflns_used 1948 _cell_measurement_temperature 298(2) _cell_measurement_theta_max 23.22 _cell_measurement_theta_min 2.50 _shelx_estimated_absorpt_T_max 0.989 _shelx_estimated_absorpt_T_min 0.977 _exptl_absorpt_coefficient_mu 0.092 _exptl_absorpt_correction_T_max 0.7457 _exptl_absorpt_correction_T_min 0.5953 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1117 before and 0.0660 after correction. The Ratio of minimum to maximum transmission is 0.7983. The \l/2 correction factor is Not present.' _exptl_absorpt_special_details ? _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.307 _exptl_crystal_density_meas . _exptl_crystal_density_method ? _exptl_crystal_description block _exptl_crystal_F_000 492 _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.12 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0856 _diffrn_reflns_av_unetI/netI 0.0888 _diffrn_reflns_Laue_measured_fraction_full 0.997 _diffrn_reflns_Laue_measured_fraction_max 0.997 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_number 16372 _diffrn_reflns_point_group_measured_fraction_full 0.997 _diffrn_reflns_point_group_measured_fraction_max 0.997 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 26.498 _diffrn_reflns_theta_min 2.437 _diffrn_ambient_temperature 298.0 _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source ? _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 2473 _reflns_number_total 4927 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement 'SAINT V8.38A (?, 2016)' _computing_data_collection ? _computing_data_reduction 'SAINT V8.38A (?, 2016)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'ShelXS (Sheldrick, 2008)' _refine_diff_density_max 0.423 _refine_diff_density_min -0.283 _refine_diff_density_rms 0.047 _refine_ls_extinction_coef 0.029(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method 'SHELXL-2014/7 (Sheldrick 2014' _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 320 _refine_ls_number_reflns 4927 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.1507 _refine_ls_R_factor_gt 0.0685 _refine_ls_restrained_S_all 1.021 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0856P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1620 _refine_ls_wR_factor_ref 0.1937 _refine_special_details ? _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All C(H,H,H) groups, All O(H) groups 2. Restrained distances C24-C23 1.55 with sigma of 0.02 C26-C27 1.55 with sigma of 0.02 3.a Ternary CH refined with riding coordinates: C9(H9), C19(H19) 3.b Secondary CH2 refined with riding coordinates: C16(H16A,H16B) 3.c Aromatic/amide H refined with riding coordinates: C1(H1), C2(H2), C3(H3), C4(H4), C5(H5), C11(H11), C12(H12), C13(H13), C14(H14), C17(H17), C20(H20), C21(H21) 3.d Idealised Me refined as rotating group: C23(H23A,H23B,H23C), C27(H27A,H27B,H27C) 3.e Idealised tetrahedral OH refined as rotating group: O5(H5A) ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary ? loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.2877(5) 0.0480(3) 0.9882(3) 0.0801(12) Uani 1 1 d . . . . . H1 H 0.3870 -0.0085 0.9560 0.096 Uiso 1 1 calc R . . . . C2 C 0.2260(6) 0.0569(4) 1.0994(3) 0.1094(17) Uani 1 1 d . . . . . H2 H 0.2841 0.0068 1.1418 0.131 Uiso 1 1 calc R . . . . C3 C 0.0808(5) 0.1383(4) 1.1478(3) 0.0976(14) Uani 1 1 d . . . . . H3 H 0.0408 0.1447 1.2232 0.117 Uiso 1 1 calc R . . . . C4 C -0.0067(5) 0.2108(4) 1.0863(3) 0.0782(11) Uani 1 1 d . . . . . H4 H -0.1074 0.2652 1.1199 0.094 Uiso 1 1 calc R . . . . C5 C 0.0539(4) 0.2036(3) 0.9742(2) 0.0605(9) Uani 1 1 d . . . . . H5 H -0.0058 0.2535 0.9325 0.073 Uiso 1 1 calc R . . . . C6 C 0.2038(4) 0.1220(3) 0.9237(2) 0.0486(7) Uani 1 1 d . . . . . C7 C 0.2860(4) 0.1112(2) 0.8047(2) 0.0451(7) Uani 1 1 d . . . . . C8 C 0.2045(3) 0.1897(2) 0.7234(2) 0.0412(7) Uani 1 1 d . . . . . C9 C 0.3028(3) 0.1405(2) 0.60566(19) 0.0390(6) Uani 1 1 d . . . . . H9 H 0.4217 0.1320 0.5937 0.047 Uiso 1 1 calc R . . . . C10 C 0.2783(3) 0.0240(2) 0.5711(2) 0.0427(7) Uani 1 1 d . . . . . C11 C 0.2886(4) -0.0858(2) 0.6233(2) 0.0553(8) Uani 1 1 d . . . . . H11 H 0.3149 -0.0966 0.6886 0.066 Uiso 1 1 calc R . . . . C12 C 0.2581(4) -0.1787(3) 0.5741(3) 0.0636(9) Uani 1 1 d . . . . . H12 H 0.2620 -0.2522 0.6082 0.076 Uiso 1 1 calc R . . . . C13 C 0.2223(4) -0.1645(3) 0.4764(3) 0.0612(9) Uani 1 1 d . . . . . H13 H 0.2030 -0.2281 0.4450 0.073 Uiso 1 1 calc R . . . . C14 C 0.2151(4) -0.0568(3) 0.4252(2) 0.0552(8) Uani 1 1 d . . . . . H14 H 0.1928 -0.0471 0.3586 0.066 Uiso 1 1 calc R . . . . C15 C 0.2411(3) 0.0368(2) 0.4733(2) 0.0448(7) Uani 1 1 d . . . . . C16 C 0.2347(4) 0.1609(2) 0.4327(2) 0.0499(8) Uani 1 1 d . . . . . H16A H 0.3278 0.1616 0.3690 0.060 Uiso 1 1 calc R . . . . H16B H 0.1316 0.1966 0.4153 0.060 Uiso 1 1 calc R . . . . C17 C 0.1848(4) 0.3412(2) 0.5463(2) 0.0465(7) Uani 1 1 d . . . . . H17 H 0.1506 0.3900 0.4931 0.056 Uiso 1 1 calc R . . . . C18 C 0.1718(4) 0.3926(2) 0.6416(2) 0.0471(7) Uani 1 1 d . . . . . C19 C 0.2118(3) 0.3232(2) 0.7361(2) 0.0438(7) Uani 1 1 d . . . . . H19 H 0.1246 0.3586 0.8022 0.053 Uiso 1 1 calc R . . . . C20 C 0.3750(3) 0.3321(2) 0.7471(2) 0.0476(7) Uani 1 1 d . . . . . H20 H 0.4719 0.2949 0.6939 0.057 Uiso 1 1 calc R . . . . C21 C 0.3884(4) 0.3895(3) 0.8276(3) 0.0554(8) Uani 1 1 d . . . . . H21 H 0.2957 0.4112 0.8881 0.067 Uiso 1 1 calc R . . . . C22 C 0.0303(4) 0.1861(2) 0.7425(2) 0.0430(7) Uani 1 1 d . . . . . C23 C 0.5506(7) 0.3005(4) 0.9936(4) 0.1171(18) Uani 1 1 d D . . . . H23A H 0.4336 0.3338 1.0262 0.176 Uiso 1 1 calc GR . . . . H23B H 0.6067 0.2897 1.0486 0.176 Uiso 1 1 calc GR . . . . H23C H 0.5687 0.2242 0.9593 0.176 Uiso 1 1 calc GR . . . . C24 C 0.6163(6) 0.3829(4) 0.9119(4) 0.0952(15) Uani 1 1 d D . . . . C25 C 0.5436(4) 0.4229(3) 0.8290(3) 0.0719(10) Uani 1 1 d . . . . . C26 C 0.6099(5) 0.4990(4) 0.7490(4) 0.0900(13) Uani 1 1 d D . . . . C27 C 0.5344(8) 0.5538(6) 0.6633(5) 0.146(2) Uani 1 1 d D . . . . H27A H 0.5943 0.5103 0.5958 0.218 Uiso 1 1 calc GR . . . . H27B H 0.5395 0.6361 0.6553 0.218 Uiso 1 1 calc GR . . . . H27C H 0.4204 0.5507 0.6833 0.218 Uiso 1 1 calc GR . . . . N1 N 0.2445(3) 0.22363(19) 0.52614(17) 0.0444(6) Uani 1 1 d . . . . . N2 N 0.1153(3) 0.5189(2) 0.6527(2) 0.0605(7) Uani 1 1 d . . . . . N3 N -0.1028(3) 0.1840(2) 0.7524(2) 0.0627(7) Uani 1 1 d . . . . . O1 O 0.4234(3) 0.04468(19) 0.76728(16) 0.0642(7) Uani 1 1 d . . . . . O2 O 0.0905(3) 0.56568(19) 0.7420(2) 0.0755(7) Uani 1 1 d . . . . . O3 O 0.0951(3) 0.57994(19) 0.5726(2) 0.0811(8) Uani 1 1 d . . . . . O4 O 0.7429(4) 0.4167(3) 0.9163(3) 0.1329(15) Uani 1 1 d . . . . . O5 O 0.7423(4) 0.5302(4) 0.7513(4) 0.1398(14) Uani 1 1 d . . . . . H5A H 0.7826 0.4899 0.7958 0.210 Uiso 1 1 calc GR . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.074(2) 0.089(3) 0.054(2) 0.0177(19) -0.0114(18) 0.005(2) C2 0.095(3) 0.142(4) 0.054(2) 0.027(2) -0.012(2) 0.016(3) C3 0.088(3) 0.150(4) 0.043(2) 0.013(2) -0.015(2) -0.019(3) C4 0.064(2) 0.106(3) 0.050(2) -0.014(2) -0.0070(17) -0.006(2) C5 0.0569(19) 0.072(2) 0.0470(19) -0.0047(15) -0.0150(15) -0.0057(16) C6 0.0482(17) 0.0529(17) 0.0411(16) 0.0016(13) -0.0120(13) -0.0086(14) C7 0.0469(17) 0.0399(15) 0.0463(17) -0.0003(12) -0.0138(13) -0.0070(13) C8 0.0423(15) 0.0387(15) 0.0416(15) -0.0018(12) -0.0134(12) -0.0070(12) C9 0.0415(15) 0.0365(14) 0.0373(15) -0.0009(11) -0.0109(12) -0.0078(11) C10 0.0401(15) 0.0355(14) 0.0442(17) -0.0042(12) -0.0015(12) -0.0071(12) C11 0.065(2) 0.0406(16) 0.0541(19) 0.0029(14) -0.0126(15) -0.0097(14) C12 0.070(2) 0.0374(16) 0.075(2) -0.0022(15) -0.0072(18) -0.0153(15) C13 0.058(2) 0.054(2) 0.070(2) -0.0171(16) -0.0082(17) -0.0189(15) C14 0.058(2) 0.0534(18) 0.0539(18) -0.0143(15) -0.0110(15) -0.0168(15) C15 0.0430(16) 0.0443(16) 0.0439(17) -0.0052(13) -0.0074(13) -0.0105(12) C16 0.0615(19) 0.0502(17) 0.0411(16) -0.0016(13) -0.0200(14) -0.0137(14) C17 0.0555(18) 0.0344(14) 0.0534(18) 0.0078(13) -0.0210(14) -0.0139(13) C18 0.0525(18) 0.0329(14) 0.0588(19) -0.0027(13) -0.0229(14) -0.0076(12) C19 0.0449(16) 0.0398(15) 0.0462(16) -0.0073(12) -0.0146(13) -0.0070(12) C20 0.0421(16) 0.0439(16) 0.0545(18) -0.0053(13) -0.0136(14) -0.0066(12) C21 0.0473(18) 0.0582(19) 0.062(2) -0.0118(15) -0.0206(15) -0.0075(14) C22 0.0451(17) 0.0388(15) 0.0415(16) -0.0065(12) -0.0100(13) -0.0065(13) C23 0.166(5) 0.081(3) 0.117(4) -0.006(3) -0.092(4) 0.007(3) C24 0.089(3) 0.064(2) 0.132(4) -0.044(3) -0.064(3) 0.025(2) C25 0.060(2) 0.063(2) 0.096(3) -0.025(2) -0.039(2) 0.0022(18) C26 0.059(2) 0.092(3) 0.129(4) -0.003(3) -0.025(2) -0.038(2) C27 0.148(5) 0.168(5) 0.155(5) 0.072(4) -0.063(4) -0.090(4) N1 0.0561(15) 0.0400(13) 0.0404(13) 0.0039(10) -0.0176(11) -0.0145(11) N2 0.0669(18) 0.0394(15) 0.083(2) -0.0029(15) -0.0356(16) -0.0109(12) N3 0.0523(17) 0.0698(18) 0.0645(18) -0.0155(13) -0.0133(14) -0.0143(13) O1 0.0539(13) 0.0678(14) 0.0531(13) -0.0009(10) -0.0132(10) 0.0119(11) O2 0.0912(18) 0.0465(13) 0.0938(18) -0.0189(12) -0.0432(15) -0.0041(11) O3 0.116(2) 0.0409(12) 0.106(2) 0.0163(13) -0.0637(17) -0.0202(12) O4 0.087(2) 0.111(2) 0.224(4) -0.080(2) -0.103(2) 0.0171(17) O5 0.073(2) 0.144(3) 0.214(5) -0.023(3) -0.033(2) -0.053(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 H1 0.9300 . ? C1 C2 1.372(5) . ? C1 C6 1.381(4) . ? C2 H2 0.9300 . ? C2 C3 1.357(5) . ? C3 H3 0.9300 . ? C3 C4 1.363(5) . ? C4 H4 0.9300 . ? C4 C5 1.383(4) . ? C5 H5 0.9300 . ? C5 C6 1.389(4) . ? C6 C7 1.485(4) . ? C7 C8 1.556(4) . ? C7 O1 1.211(3) . ? C8 C9 1.557(4) . ? C8 C19 1.576(4) . ? C8 C22 1.477(4) . ? C9 H9 0.9800 . ? C9 C10 1.523(4) . ? C9 N1 1.474(3) . ? C10 C11 1.395(4) . ? C10 C15 1.383(4) . ? C11 H11 0.9300 . ? C11 C12 1.394(4) . ? C12 H12 0.9300 . ? C12 C13 1.377(5) . ? C13 H13 0.9300 . ? C13 C14 1.370(4) . ? C14 H14 0.9300 . ? C14 C15 1.373(4) . ? C15 C16 1.489(4) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C16 N1 1.473(3) . ? C17 H17 0.9300 . ? C17 C18 1.354(4) . ? C17 N1 1.327(3) . ? C18 C19 1.497(4) . ? C18 N2 1.409(3) . ? C19 H19 0.9800 . ? C19 C20 1.502(4) . ? C20 H20 0.9300 . ? C20 C21 1.309(4) . ? C21 H21 0.9300 . ? C21 C25 1.507(5) . ? C22 N3 1.136(3) . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C23 C24 1.470(6) . ? C24 C25 1.395(5) . ? C24 O4 1.281(5) . ? C25 C26 1.407(6) . ? C26 C27 1.479(6) . ? C26 O5 1.305(5) . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? N2 O2 1.233(3) . ? N2 O3 1.248(3) . ? O5 H5A 0.8200 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 H1 119.6 . . ? C2 C1 C6 120.7(3) . . ? C6 C1 H1 119.6 . . ? C1 C2 H2 119.8 . . ? C3 C2 C1 120.4(4) . . ? C3 C2 H2 119.8 . . ? C2 C3 H3 119.9 . . ? C2 C3 C4 120.2(4) . . ? C4 C3 H3 119.9 . . ? C3 C4 H4 119.9 . . ? C3 C4 C5 120.1(3) . . ? C5 C4 H4 119.9 . . ? C4 C5 H5 119.9 . . ? C4 C5 C6 120.1(3) . . ? C6 C5 H5 119.9 . . ? C1 C6 C5 118.3(3) . . ? C1 C6 C7 116.7(3) . . ? C5 C6 C7 124.9(3) . . ? C6 C7 C8 121.6(2) . . ? O1 C7 C6 121.1(3) . . ? O1 C7 C8 117.2(2) . . ? C7 C8 C9 109.0(2) . . ? C7 C8 C19 108.3(2) . . ? C9 C8 C19 110.2(2) . . ? C22 C8 C7 112.1(2) . . ? C22 C8 C9 107.5(2) . . ? C22 C8 C19 109.8(2) . . ? C8 C9 H9 109.5 . . ? C10 C9 C8 117.4(2) . . ? C10 C9 H9 109.5 . . ? N1 C9 C8 110.1(2) . . ? N1 C9 H9 109.5 . . ? N1 C9 C10 100.6(2) . . ? C11 C10 C9 129.4(3) . . ? C15 C10 C9 110.8(2) . . ? C15 C10 C11 119.8(3) . . ? C10 C11 H11 121.1 . . ? C12 C11 C10 117.7(3) . . ? C12 C11 H11 121.1 . . ? C11 C12 H12 119.2 . . ? C13 C12 C11 121.7(3) . . ? C13 C12 H12 119.2 . . ? C12 C13 H13 120.0 . . ? C14 C13 C12 120.0(3) . . ? C14 C13 H13 120.0 . . ? C13 C14 H14 120.3 . . ? C13 C14 C15 119.4(3) . . ? C15 C14 H14 120.3 . . ? C10 C15 C16 110.9(2) . . ? C14 C15 C10 121.5(3) . . ? C14 C15 C16 127.7(3) . . ? C15 C16 H16A 111.3 . . ? C15 C16 H16B 111.3 . . ? H16A C16 H16B 109.2 . . ? N1 C16 C15 102.2(2) . . ? N1 C16 H16A 111.3 . . ? N1 C16 H16B 111.3 . . ? C18 C17 H17 118.9 . . ? N1 C17 H17 118.9 . . ? N1 C17 C18 122.3(3) . . ? C17 C18 C19 124.0(2) . . ? C17 C18 N2 117.9(3) . . ? N2 C18 C19 118.2(3) . . ? C8 C19 H19 107.8 . . ? C18 C19 C8 108.5(2) . . ? C18 C19 H19 107.8 . . ? C18 C19 C20 111.5(2) . . ? C20 C19 C8 113.3(2) . . ? C20 C19 H19 107.8 . . ? C19 C20 H20 118.2 . . ? C21 C20 C19 123.6(3) . . ? C21 C20 H20 118.2 . . ? C20 C21 H21 117.7 . . ? C20 C21 C25 124.5(3) . . ? C25 C21 H21 117.7 . . ? N3 C22 C8 177.0(3) . . ? H23A C23 H23B 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C24 C23 H23A 109.5 . . ? C24 C23 H23B 109.5 . . ? C24 C23 H23C 109.5 . . ? C25 C24 C23 120.7(4) . . ? O4 C24 C23 119.4(4) . . ? O4 C24 C25 119.9(5) . . ? C24 C25 C21 120.0(4) . . ? C24 C25 C26 120.5(4) . . ? C26 C25 C21 119.4(3) . . ? C25 C26 C27 124.5(4) . . ? O5 C26 C25 119.6(4) . . ? O5 C26 C27 115.7(4) . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27B 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C16 N1 C9 112.9(2) . . ? C17 N1 C9 122.2(2) . . ? C17 N1 C16 124.2(2) . . ? O2 N2 C18 118.3(3) . . ? O2 N2 O3 122.0(3) . . ? O3 N2 C18 119.7(3) . . ? C26 O5 H5A 109.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C17 H17 O3 0.93 2.47 3.165(4) 132.1 2_566 O5 H5A O4 0.82 1.71 2.436(6) 145.8 . loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 C2 C3 C4 1.1(8) . . . . ? C1 C6 C7 C8 -179.8(3) . . . . ? C1 C6 C7 O1 -3.4(5) . . . . ? C2 C1 C6 C5 -1.4(6) . . . . ? C2 C1 C6 C7 176.0(4) . . . . ? C2 C3 C4 C5 -1.4(7) . . . . ? C3 C4 C5 C6 0.4(6) . . . . ? C4 C5 C6 C1 1.0(5) . . . . ? C4 C5 C6 C7 -176.1(3) . . . . ? C5 C6 C7 C8 -2.7(5) . . . . ? C5 C6 C7 O1 173.8(3) . . . . ? C6 C1 C2 C3 0.3(8) . . . . ? C6 C7 C8 C9 -169.1(2) . . . . ? C6 C7 C8 C19 71.0(3) . . . . ? C6 C7 C8 C22 -50.2(3) . . . . ? C7 C8 C9 C10 74.4(3) . . . . ? C7 C8 C9 N1 -171.5(2) . . . . ? C7 C8 C19 C18 166.7(2) . . . . ? C7 C8 C19 C20 42.3(3) . . . . ? C8 C9 C10 C11 -50.8(4) . . . . ? C8 C9 C10 C15 129.3(2) . . . . ? C8 C9 N1 C16 -140.8(2) . . . . ? C8 C9 N1 C17 30.0(3) . . . . ? C8 C19 C20 C21 -125.6(3) . . . . ? C9 C8 C19 C18 47.5(3) . . . . ? C9 C8 C19 C20 -76.9(3) . . . . ? C9 C10 C11 C12 179.2(3) . . . . ? C9 C10 C15 C14 179.4(3) . . . . ? C9 C10 C15 C16 -0.7(3) . . . . ? C10 C9 N1 C16 -16.3(3) . . . . ? C10 C9 N1 C17 154.5(2) . . . . ? C10 C11 C12 C13 1.3(5) . . . . ? C10 C15 C16 N1 -9.0(3) . . . . ? C11 C10 C15 C14 -0.5(4) . . . . ? C11 C10 C15 C16 179.4(2) . . . . ? C11 C12 C13 C14 -0.4(5) . . . . ? C12 C13 C14 C15 -1.1(5) . . . . ? C13 C14 C15 C10 1.5(4) . . . . ? C13 C14 C15 C16 -178.4(3) . . . . ? C14 C15 C16 N1 170.9(3) . . . . ? C15 C10 C11 C12 -0.9(4) . . . . ? C15 C16 N1 C9 16.2(3) . . . . ? C15 C16 N1 C17 -154.4(2) . . . . ? C17 C18 C19 C8 -20.6(4) . . . . ? C17 C18 C19 C20 104.9(3) . . . . ? C17 C18 N2 O2 174.3(3) . . . . ? C17 C18 N2 O3 -7.1(4) . . . . ? C18 C17 N1 C9 -0.7(4) . . . . ? C18 C17 N1 C16 169.0(3) . . . . ? C18 C19 C20 C21 111.7(3) . . . . ? C19 C8 C9 C10 -166.9(2) . . . . ? C19 C8 C9 N1 -52.7(3) . . . . ? C19 C18 N2 O2 -5.0(4) . . . . ? C19 C18 N2 O3 173.7(3) . . . . ? C19 C20 C21 C25 -166.2(3) . . . . ? C20 C21 C25 C24 -122.4(4) . . . . ? C20 C21 C25 C26 60.4(5) . . . . ? C21 C25 C26 C27 2.2(6) . . . . ? C21 C25 C26 O5 178.5(3) . . . . ? C22 C8 C9 C10 -47.3(3) . . . . ? C22 C8 C9 N1 66.9(3) . . . . ? C22 C8 C19 C18 -70.7(3) . . . . ? C22 C8 C19 C20 164.9(2) . . . . ? C23 C24 C25 C21 4.7(5) . . . . ? C23 C24 C25 C26 -178.1(4) . . . . ? C24 C25 C26 C27 -174.9(4) . . . . ? C24 C25 C26 O5 1.3(6) . . . . ? N1 C9 C10 C11 -170.1(3) . . . . ? N1 C9 C10 C15 10.0(3) . . . . ? N1 C17 C18 C19 -4.2(5) . . . . ? N1 C17 C18 N2 176.6(3) . . . . ? N2 C18 C19 C8 158.6(2) . . . . ? N2 C18 C19 C20 -75.9(3) . . . . ? O1 C7 C8 C9 14.3(4) . . . . ? O1 C7 C8 C19 -105.6(3) . . . . ? O1 C7 C8 C22 133.2(3) . . . . ? O4 C24 C25 C21 -176.2(3) . . . . ? O4 C24 C25 C26 1.0(5) . . . . ? loop_ _refln_index_h _refln_index_k _refln_index_l _refln_F_squared_meas _refln_F_squared_sigma -3 0 0 7.15 0.78 -4 0 0 104.53 5.1 -4 0 0 102.92 5.01 -4 0 0 99.95 5.66 -5 0 0 8.57 1.19 -5 0 0 9.31 1.82 -5 0 0 8.07 1.27 -6 0 0 86.34 5.53 -6 0 0 82.3 4.73 -6 0 0 88.12 5.63 -6 0 0 79.38 4.58 -7 0 0 1 0.71 -7 0 0 0.46 0.63 -7 0 0 0.02 0.74 -7 0 0 0.9 0.9 -8 0 0 1.91 1.17 -8 0 0 1.16 0.67 -8 0 0 1.59 0.81 -8 0 0 2.37 1.29 -9 0 0 -1.51 0.58 -9 0 0 -1.23 0.89 -9 0 0 0.77 1.01 -9 0 0 -0.24 0.55 -10 0 0 3.49 1.72 -10 0 0 0.83 0.85 -10 0 0 0.95 1.25 -10 0 0 0.51 0.87 -10 1 0 1.11 1.44 -10 1 0 0.29 0.78 -10 1 0 0.96 0.71 -10 1 0 0.58 1.25 -9 1 0 0.44 1.2 -9 1 0 0.84 0.64 -9 1 0 0.55 0.67 -9 1 0 -0.22 0.94 -8 1 0 -0.74 0.74 -8 1 0 0.39 1.06 -8 1 0 0.48 0.64 -7 1 0 10.33 2.37 -7 1 0 11.3 2.27 -7 1 0 12.9 1.44 -7 1 0 12.81 1.75 -6 1 0 9.79 1.43 -6 1 0 10.04 2.02 -6 1 0 12.44 1.32 -5 1 0 1.4 0.53 -5 1 0 3.1 1.1 -5 1 0 2.08 0.67 -4 1 0 75.77 3.75 -4 1 0 75.81 4.67 -3 1 0 -0.56 0.33 -3 1 0 0.19 0.25 2 -1 0 227.66 10.53 -2 1 0 232.1 9.84 -2 1 0 261.93 10.66 1 -1 0 377.13 15.62 -1 -1 0 135.2 5.58 -1 -1 0 135.58 5.43 1 1 0 122.34 5.44 1 1 0 128.3 5.56 -2 -1 0 354.78 15 -2 -1 0 367.36 14.88 -3 -1 0 161.3 7.49 -3 -1 0 171.9 7.55 -4 -1 0 251.56 11.37 -4 -1 0 255.58 11.24 -4 -1 0 254.4 11.26 -5 -1 0 1.36 0.69 -5 -1 0 2.12 0.84 -5 -1 0 0.97 0.64 -6 -1 0 29.15 2.44 -6 -1 0 30.68 2.46 -6 -1 0 32.15 2.82 -7 -1 0 -0.13 0.65 -7 -1 0 0.24 0.67 -7 -1 0 0.66 0.64 -7 -1 0 -0.15 0.98 -8 -1 0 7.91 1.64 -8 -1 0 8.93 2.01 -8 -1 0 3.98 1.49 -8 -1 0 7.94 1.6 -9 -1 0 2.79 1.34 -9 -1 0 2.14 1.05 -9 -1 0 0.36 1.01 -9 -1 0 1.83 1.05 -10 -1 0 -0.86 0.9 -10 -1 0 -0.28 1.1 -10 -1 0 -1.15 0.76 -10 -1 0 -0.89 1.14 -10 2 0 -0.78 0.64 -10 2 0 1.14 0.74 -9 2 0 -0.81 1.13 -9 2 0 -0.02 1.17 -9 2 0 0.85 0.66 -8 2 0 -0.84 1.19 -8 2 0 -1.02 0.44 -8 2 0 0.45 0.5 -8 2 0 -1.96 0.79 -7 2 0 6.39 1.83 -7 2 0 5.39 1.16 -7 2 0 4.99 0.96 -6 2 0 31.78 3.25 -6 2 0 27.03 2.21 -6 2 0 33.06 2.09 -5 2 0 5.81 1.39 -5 2 0 6.21 0.85 -4 2 0 10.03 1.68 -4 2 0 10.84 0.89 3 -2 0 2.82 0.89 -3 2 0 4.27 0.49 -3 2 0 5.74 1.21 2 -2 0 41.8 2.81 -2 2 0 46.34 2.87 -2 2 0 44.76 1.88 -2 2 0 41.82 2.07 1 -2 0 2.15 0.37 1 -2 0 2.75 0.7 -1 2 0 1.94 0.35 -1 2 0 1.69 0.54 0 -2 0 134.54 5.5 0 -2 0 130.64 5.87 0 2 0 126.06 5.49 0 2 0 127.16 5.87 -1 -2 0 456.11 18.75 1 2 0 435.53 18.75 1 2 0 462.56 18.41 -2 -2 0 71.02 3.6 -2 -2 0 75.13 3.33 2 2 0 64.19 3.53 2 2 0 73.01 3.28 -3 -2 0 22.61 1.74 -3 -2 0 21.51 1.49 3 2 0 21.2 1.67 -4 -2 0 85.93 4.6 -4 -2 0 81.07 4.55 -4 -2 0 85.91 4.38 -5 -2 0 127.07 6.61 -5 -2 0 128.01 6.63 -5 -2 0 131.2 6.51 -6 -2 0 2.41 0.96 -6 -2 0 4.04 1.09 -7 -2 0 4.3 1.24 -7 -2 0 4.46 1.28 -7 -2 0 4.81 1.33 -8 -2 0 -0.18 0.78 -8 -2 0 -1.52 0.52 -8 -2 0 0.59 0.76 -8 -2 0 0.12 0.74 -9 -2 0 -0.58 0.91 -9 -2 0 1.22 0.83 -9 -2 0 0.96 1.15 -9 -2 0 0.39 0.95 -10 -2 0 0.62 0.92 -10 -2 0 0.51 1.18 -10 -2 0 1.03 1.06 -10 -2 0 0.24 1.2 -9 3 0 2.68 0.79 -9 3 0 2.93 0.92 -9 3 0 3.47 1.75 -9 3 0 3.03 1.96 -9 3 0 2.15 0.64 -8 3 0 1.89 0.54 -8 3 0 1.7 0.72 -8 3 0 2.65 1.28 -8 3 0 2.72 0.7 -7 3 0 1.33 1.06 -7 3 0 0.51 0.4 -7 3 0 0.84 0.62 -6 3 0 1.13 0.94 -6 3 0 0.6 0.35 -5 3 0 5.27 0.61 -5 3 0 4.95 1.43 4 -3 0 42.36 3.44 -4 3 0 38.21 2.18 -4 3 0 41.5 1.95 -4 3 0 45.25 3.47 3 -3 0 23.49 2.35 -3 3 0 26.62 1.53 -3 3 0 25.81 2.35 -3 3 0 27.14 1.17 2 -3 0 50.5 3.32 -2 3 0 49.66 2.37 -2 3 0 46.91 3.22 1 -3 0 220.22 9.33 1 -3 0 219.78 10.17 -1 3 0 224.29 10.2 -1 3 0 234.44 9.37 0 -3 0 213.66 8.69 0 -3 0 201.73 9.24 0 3 0 201.8 8.69 0 3 0 205.54 9.29 -1 -3 0 406.74 16.69 -1 -3 0 414.73 17.14 1 3 0 402.2 17.16 1 3 0 386.81 16.66 -2 -3 0 71.19 3.86 2 3 0 67.11 3.32 2 3 0 60.3 3.41 -3 -3 0 2.15 0.66 -3 -3 0 1.37 0.44 3 3 0 0.26 0.43 3 3 0 1.71 0.43 -4 -3 0 1.11 0.48 -4 -3 0 0.46 0.65 4 3 0 0.39 0.53 -5 -3 0 27.98 2.4 -5 -3 0 27.55 2.44 -5 -3 0 27.37 2.09 -6 -3 0 19.15 1.92 -6 -3 0 20.44 3.8 -6 -3 0 22.86 2.31 -7 -3 0 -0.14 0.69 -7 -3 0 -1.05 0.56 -7 -3 0 0 0.59 -8 -3 0 6.52 1.61 -8 -3 0 14.77 2.31 -8 -3 0 7.9 1.7 -9 -3 0 -0.87 0.82 -9 -3 0 -0.14 0.75 -9 -3 0 1.32 0.77 -9 -3 0 0.68 0.91 -10 -3 0 1.49 1.3 -10 -3 0 -1.86 1.3 -10 -3 0 0 0.97 -10 -3 0 0.95 0.97 -11 -3 0 -1.76 1 -11 -3 0 -0.96 0.89 -11 -3 0 -1.19 1.31 -11 -3 0 -0.57 0.99 -9 4 0 0.34 0.63 -9 4 0 -2.26 1.69 -9 4 0 -0.51 1.56 -8 4 0 0.34 0.47 -8 4 0 0.35 1.06 -8 4 0 -0.19 0.18 -7 4 0 1.75 0.3 -7 4 0 3.5 0.67 -7 4 0 2.53 0.74 -7 4 0 4.59 1.73 -6 4 0 12.63 0.72 -6 4 0 15.05 2.72 -6 4 0 12.66 1.22 -5 4 0 -0.07 0.78 -5 4 0 0.23 0.34 4 -4 0 0.15 0.92 -4 4 0 1.91 0.47 -4 4 0 2.24 1.1 3 -4 0 13.11 2.12 -3 4 0 10.59 1.84 -3 4 0 12.5 0.98 2 -4 0 36.77 2.98 -2 4 0 36.92 3 -2 4 0 42.51 2.14 1 -4 0 100.94 5.51 1 -4 0 103.33 4.57 -1 4 0 99.33 5.51 -1 4 0 100.01 4.6 0 -4 0 62.98 3.05 0 -4 0 60.47 3.68 0 4 0 62.05 3.75 0 4 0 56.57 3.04 -1 -4 0 113.45 5.24 -1 -4 0 119.46 5.84 1 4 0 109.11 5.83 1 4 0 101.84 5.19 -2 -4 0 2.75 0.89 -2 -4 0 2.88 0.75 2 4 0 2.41 0.68 2 4 0 2.46 0.72 2 4 0 3.22 0.95 -3 -4 0 13.85 1.43 -3 -4 0 12.49 1.83 3 4 0 12.22 1.12 3 4 0 8.42 1.28 -4 -4 0 9.36 1.43 -4 -4 0 9.5 1.69 -4 -4 0 10.53 1.05 4 4 0 7.86 0.84 4 4 0 9.05 1.43 -5 -4 0 1.38 0.74 -5 -4 0 1.04 0.65 -5 -4 0 0.09 0.33 -6 -4 0 0.38 0.74 -6 -4 0 0.38 0.73 -6 -4 0 0.03 0.39 -7 -4 0 23.07 2.58 -7 -4 0 20.96 2.48 -7 -4 0 22.47 2.09 -8 -4 0 9.29 2.09 -8 -4 0 13.59 1.75 -8 -4 0 11.57 2.17 -9 -4 0 0.05 1.11 -9 -4 0 1.43 1.03 -9 -4 0 0.29 0.7 -10 -4 0 2.07 1.22 -10 -4 0 1.43 1.14 -10 -4 0 -0.2 1.04 -10 -4 0 -0.23 0.85 -11 -4 0 0.14 0.9 -11 -4 0 -1.45 1.41 -11 -4 0 -0.22 1.04 -11 -4 0 -0.54 1.19 -9 5 0 -1.14 1.94 -9 5 0 4.03 1.82 -9 5 0 -0.09 0.42 -9 5 0 -0.2 0.38 -8 5 0 1.28 0.52 -8 5 0 2 0.6 -8 5 0 2.83 1.77 -7 5 0 2.92 0.74 -7 5 0 1.44 1.37 -7 5 0 1.49 0.54 -6 5 0 7.09 0.95 -6 5 0 10.55 2.42 5 -5 0 7.66 1.99 -5 5 0 9.51 2.19 -5 5 0 9.73 0.98 4 -5 0 0.18 0.89 -4 5 0 0.82 0.39 -4 5 0 0.85 0.84 3 -5 0 5.19 1.49 -3 5 0 5.54 1.47 -3 5 0 7.25 0.8 2 -5 0 20.56 1.5 2 -5 0 22.88 2.37 -2 5 0 27.01 1.63 -2 5 0 25.57 2.49 1 -5 0 5.91 0.62 1 -5 0 5.23 0.77 -1 5 0 5.6 1.37 -1 5 0 4.64 0.78 0 -5 0 156.71 7.91 0 -5 0 164.16 7.01 0 5 0 153.18 7.97 0 5 0 146.13 7 -1 -5 0 217.25 9.1 -1 -5 0 202.02 9.75 1 5 0 191.76 9.03 1 5 0 196.58 9.86 -2 -5 0 111.26 5.44 -2 -5 0 115.33 6.05 2 5 0 113.9 5.53 2 5 0 98.46 5.96 2 5 0 92.63 5.28 -3 -5 0 27.53 2.53 3 5 0 22.95 2.04 3 5 0 25.26 1.97 -4 -5 0 9.18 1.53 -4 -5 0 10.06 1.83 4 5 0 9.28 0.97 4 5 0 5.88 1.15 -5 -5 0 4.9 1.37 -5 -5 0 6.25 1.33 -5 -5 0 8.96 1.75 5 5 0 9.54 1.55 -6 -5 0 0.72 0.94 -6 -5 0 0.71 0.51 -6 -5 0 -0.48 0.6 -6 -5 0 0.74 0.95 -7 -5 0 1.91 0.69 -7 -5 0 0.09 0.82 -7 -5 0 2.07 1.18 -8 -5 0 -0.17 0.85 -8 -5 0 -0.73 0.42 -8 -5 0 0.27 1.04 -9 -5 0 -1.22 1.04 -9 -5 0 1 1.14 -9 -5 0 0.72 0.58 -10 -5 0 2.91 1.43 -10 -5 0 0.24 1.03 -10 -5 0 0.99 0.69 -11 -5 0 2.02 1.6 -11 -5 0 1.14 0.67 -11 -5 0 1.26 1.16 -11 -5 0 2.08 1.41 -8 6 0 1.33 0.46 -8 6 0 0.31 1.09 -8 6 0 0.72 0.41 -7 6 0 0.05 1.23 -7 6 0 0.51 0.43 -6 6 0 0.79 1.09 -6 6 0 -0.24 0.3 5 -6 0 12.4 2.52 -5 6 0 16.57 1.32 -5 6 0 18.25 3.05 4 -6 0 1 0.88 -4 6 0 1.35 0.49 -4 6 0 1.47 1.07 3 -6 0 5.66 1.55 -3 6 0 5.58 1.63 -3 6 0 4.48 0.79 2 -6 0 0.65 0.43 2 -6 0 1.27 0.86 -2 6 0 0.23 0.34 -2 6 0 -0.47 0.33 1 -6 0 20.99 1.38 1 -6 0 20.85 2.36 1 -6 0 23.61 1.66 -1 6 0 21.93 1.67 -1 6 0 22.34 2.51 0 -6 0 14.12 1.31 0 -6 0 12.4 2.01 0 6 0 12.26 2.05 0 6 0 11.11 1.25 -1 -6 0 9.46 1.29 -1 -6 0 9.71 1.72 1 6 0 7.61 1.65 1 6 0 6.39 1.14 -2 -6 0 41.57 2.73 -2 -6 0 39.4 3.26 2 6 0 36.24 3.18 2 6 0 32.78 2.56 2 6 0 39.29 2.94 -3 -6 0 15.44 2.31 -3 -6 0 16.69 1.78 3 6 0 11.56 1.67 3 6 0 12.54 1.58 3 6 0 14.42 2.27 -4 -6 0 1.63 0.91 -4 -6 0 3.68 1.06 4 6 0 2.17 0.82 4 6 0 0.81 0.55 -5 -6 0 7.39 1.71 -5 -6 0 6.84 1.53 -5 -6 0 7.84 1.83 5 6 0 7.99 0.87 5 6 0 5.12 1.34 -6 -6 0 2.44 1.23 -6 -6 0 3.19 1.23 -6 -6 0 2.51 1.29 -7 -6 0 0.51 0.83 -7 -6 0 -1.16 0.8 -7 -6 0 1.88 1.23 -8 -6 0 -0.01 0.76 -8 -6 0 -1.05 0.81 -8 -6 0 -0.29 0.77 -9 -6 0 -1.57 0.96 -9 -6 0 0.13 0.92 -9 -6 0 2.38 1.28 -10 -6 0 1.1 1.24 -8 7 0 -0.39 0.19 -8 7 0 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1.05 0 -3 -15 -1.63 1.8 0 3 15 -0.13 1.16 0 3 15 -0.71 1.33 -1 -3 -15 0.33 0.88 -1 -3 -15 2.73 2.7 1 3 15 0.04 1.35 1 3 15 1.21 0.94 -2 -3 -15 -0.15 1.77 2 3 15 2.55 1.32 -3 -3 -15 -0.38 1.84 3 3 15 -0.88 0.83 -4 -3 -15 -2.41 1.87 4 3 15 1.12 1.04 -5 -3 -15 1.07 2.31 5 3 15 0.64 0.69 -6 -3 -15 4.08 2.85 -7 -3 -15 -1.09 2.5 -8 -3 -15 -0.34 1.88 1 -4 -15 0.77 0.92 -1 4 15 1 0.96 -1 4 15 -1.52 1.37 0 -4 -15 -0.76 0.84 0 4 15 0.87 1.03 0 4 15 0.77 1.55 -1 -4 -15 2.08 2.5 -1 -4 -15 0.53 0.86 1 4 15 1.02 1.92 -2 -4 -15 -2.34 2.19 2 4 15 -1.97 1.08 -3 -4 -15 0.99 2.17 3 4 15 2.02 1.25 -4 -4 -15 -0.12 1.84 4 4 15 -0.33 0.92 -5 -4 -15 1.39 2.49 5 4 15 0.78 0.69 -6 -4 -15 2.83 2.59 6 4 15 1.2 0.54 6 4 15 1.91 0.48 -7 -4 -15 1.06 1.95 -8 -4 -15 -1.93 2.4 0 -5 -15 -1.11 0.84 0 5 15 1.5 1.54 -1 -5 -15 0.72 1.04 1 5 15 2.06 1.66 -2 -5 -15 0.85 1.64 -2 -5 -15 1.04 2.2 2 5 15 -0.05 1.23 -3 -5 -15 -0.18 2.25 3 5 15 -0.64 1.15 -4 -5 -15 4.77 3.27 -5 -5 -15 -0.94 1.48 5 5 15 -0.34 0.74 -6 -5 -15 0.59 2.69 6 5 15 0.82 0.53 -7 -5 -15 -0.43 2.2 -8 -5 -15 -0.27 1.94 -1 -6 -15 1.55 1.12 -1 -6 -15 1.17 1.03 1 6 15 -0.7 1.56 -2 -6 -15 -0.76 2.1 -2 -6 -15 0.37 1.07 2 6 15 1.2 1.48 -3 -6 -15 -4.35 1.96 -4 -6 -15 -4.24 2.04 4 6 15 -0.9 1.07 -5 -6 -15 -0.07 2.33 5 6 15 0.33 0.81 -6 -6 -15 -0.69 2.62 6 6 15 0.65 0.61 -7 -6 -15 -0.97 2.07 -2 -7 -15 -0.27 1.1 -2 -7 -15 1.62 1.15 2 7 15 -0.42 1.18 -3 -7 -15 -3.37 1.56 -3 -7 -15 1.28 1.32 3 7 15 -0.59 1.12 -4 -7 -15 0.48 2.2 4 7 15 -1.1 1.06 -5 -7 -15 -1 2.62 5 7 15 0.01 0.92 -6 -7 -15 -2.26 2.45 6 7 15 -0.61 0.72 -7 -7 -15 3.47 3.07 -4 -8 -15 2.08 2.45 4 8 15 3.33 1.54 -5 -8 -15 2.52 1.43 -5 -8 -15 2.41 2.84 -1 4 -16 0.94 1.91 1 -4 16 2.28 1.36 -2 4 -16 0.13 1.9 2 -4 16 1.74 1.47 -3 4 -16 -3.04 1.88 3 -4 16 1.15 1.21 -4 4 -16 -3.01 1.7 4 -4 16 -2.64 0.94 0 3 -16 1.11 2.18 0 -3 16 1.39 1.06 -1 3 -16 5.57 2.47 1 -3 16 1.2 1.07 -2 3 -16 -1.45 2 2 -3 16 1.3 1.19 -3 3 -16 0.59 1.77 3 -3 16 0.92 1.06 -4 3 -16 0.55 2.11 4 -3 16 -1.81 1.97 4 -3 16 1.27 1.1 -5 3 -16 3.45 2.67 0 2 -16 1.06 2.35 0 -2 16 -1.54 0.76 -1 2 -16 -0.87 1.93 1 -2 16 -0.7 0.83 -2 2 -16 -1.46 1.69 2 -2 16 0.79 1.06 -3 2 -16 3.19 2.35 3 -2 16 3.52 1.49 -4 2 -16 0.59 1.86 4 -2 16 -0.78 0.77 4 -2 16 -1.73 1.65 -5 2 -16 2.42 2.57 5 -2 16 2.12 1.66 -6 2 -16 0.83 2.46 6 -2 16 1.13 1.19 0 1 -16 2.41 2.32 0 -1 16 2.24 1.3 -1 1 -16 -4.04 1.42 1 -1 16 0.34 0.81 -2 1 -16 -0.38 1.61 2 -1 16 0.29 1.17 -3 1 -16 0.06 2.25 3 -1 16 -0.89 0.86 -4 1 -16 -1.56 1.87 -5 1 -16 6.2 3.09 5 -1 16 0.09 1.51 -6 1 -16 -1.95 1.83 6 -1 16 0.27 1.22 6 -1 16 0.33 0.73 0 0 -16 3.47 2.46 0 0 16 2.09 1.12 -1 0 -16 -0.62 2.24 1 0 16 0.51 1.12 -2 0 -16 -1.35 2.07 2 0 16 0.03 1.03 -3 0 -16 0.08 1.98 3 0 16 3.51 2.07 3 0 16 1.22 1.03 -4 0 -16 -1.81 1.99 4 0 16 0.57 1.12 4 0 16 0.31 1.47 -5 0 -16 -2.46 1.61 5 0 16 1.1 0.96 5 0 16 -1.82 1.18 -6 0 -16 -4.68 1.71 6 0 16 -0.24 0.6 6 0 16 0.85 0.78 0 -1 -16 -1.93 1.79 0 1 16 -0.73 0.99 0 1 16 -0.93 1.3 -1 -1 -16 -2.94 2.01 1 1 16 2.3 1.51 1 1 16 0.29 1.07 -2 -1 -16 1.6 2.71 2 1 16 -0.46 1.25 -3 -1 -16 -2.73 1.6 3 1 16 0.76 1.26 -4 -1 -16 2.03 2.42 4 1 16 1.2 1.61 -5 -1 -16 -2.32 1.49 5 1 16 2 1.34 5 1 16 -0.26 1.17 -6 -1 -16 3.61 2.41 -7 -1 -16 -2.48 1.85 0 -2 -16 2.91 2.73 0 2 16 2.57 1.28 0 2 16 1.43 1.68 -1 -2 -16 -0.42 2.44 1 2 16 0.28 1.38 1 2 16 -2.27 0.68 -2 -2 -16 -3.3 1.98 2 2 16 1.66 1.22 2 2 16 1.07 1.37 -3 -2 -16 1.89 2.53 3 2 16 1.71 1.34 -4 -2 -16 -1.02 1.81 4 2 16 0.69 1.27 -5 -2 -16 0.4 2.47 5 2 16 0.89 1.21 -6 -2 -16 -0.04 2.19 6 2 16 0.31 0.33 6 2 16 0.32 0.5 -7 -2 -16 -1.19 2.06 -1 -3 -16 0.11 2.31 1 3 16 -0.99 0.78 1 3 16 1.92 1.6 -2 -3 -16 -0.97 2.23 2 3 16 -0.96 1.13 -3 -3 -16 -0.22 2.58 3 3 16 1.32 1.06 -4 -3 -16 -2.42 2.09 4 3 16 1.39 1.03 -5 -3 -16 0.62 1.83 5 3 16 1.26 1.38 -6 -3 -16 -2.07 2 6 3 16 0.23 0.37 6 3 16 0.42 0.54 -7 -3 -16 -0.86 2.43 -1 -4 -16 -2.29 1.97 1 4 16 0.99 1.54 -2 -4 -16 -0.91 2.29 2 4 16 -1.67 0.93 -3 -4 -16 0.13 2.33 3 4 16 -0.22 1.14 -4 -4 -16 4.4 2.87 4 4 16 0.7 1.15 -5 -4 -16 -4.83 2.09 5 4 16 -1.22 0.81 -6 -4 -16 -1.48 2.05 6 4 16 0.03 0.72 6 4 16 0.96 0.46 -2 -5 -16 1.33 2.26 2 5 16 5.38 2.76 -3 -5 -16 1.24 2.51 3 5 16 -0.22 1.11 -4 -5 -16 6.2 3.02 -5 -5 -16 0.71 2.51 5 5 16 0.56 0.88 -6 -5 -16 -1.98 2.03 6 5 16 1.75 0.68 -3 -6 -16 -2.92 1.87 3 6 16 -1.8 1.12 -4 -6 -16 2.43 2.96 4 6 16 2.7 1.51 -5 -6 -16 0.72 2.25 5 6 16 1.23 1.08 -3 1 -17 1.61 2.22 3 -1 17 4.17 1.67 -2 0 -17 5.38 2.86 2 0 17 1.47 1.92 2 0 17 -0.4 1.21 -3 0 -17 1.34 2.54 3 0 17 1.08 1.33 3 0 17 0.16 1.1 4 0 17 -0.55 1.15 4 0 17 -1.51 2.3 -2 -1 -17 -1.91 2.02 2 1 17 -0.78 0.55 2 1 17 0.17 1.81 -3 -1 -17 1.11 2.63 3 1 17 0.25 1.38 -4 -1 -17 3.37 2.9 4 1 17 3.11 1.53 4 1 17 3.24 2.11 -3 -2 -17 -1.04 2.63 3 2 17 -0.99 1.21 -4 -2 -17 -0.24 2.55 4 2 17 3.01 1.52 -4 -3 -17 1.96 2.71 _iucr_refine_instructions_details ; a.res created by SHELXL-2014/7 TITL A in P-1 #2 REM reset to P-1 #2 CELL 0.71073 8.7186 11.5293 12.8873 86.887 72.756 74.684 ZERR 2 0.0034 0.0047 0.0054 0.013 0.013 0.012 LATT 1 SFAC C H N O UNIT 54 46 6 10 EQIV $1 -X,1-Y,1-Z DFIX 1.55 C24 C23 DFIX 1.55 C26 C27 L.S. 4 0 0 PLAN 20 SIZE 0.25 0.14 0.12 TEMP 24.85 MPLA C1 C2 C3 C4 C5 C6 MPLA C9 C10 C11 C12 C13 C14 C15 C16 MPLA C9 C16 N1 MPLA C9 C17 C18 C19 N1 MPLA C8 C9 C19 HTAB O5 O4 HTAB C17 O3_$1 BOND $H CONF fmap acta OMIT 0 53 REM REM REM WGHT 0.085600 EXTI 0.028954 FVAR 0.33187 C1 1 0.287657 0.048000 0.988229 11.00000 0.07446 0.08912 = 0.05407 0.01767 -0.01141 0.00527 AFIX 43 H1 2 0.387018 -0.008450 0.955966 11.00000 -1.20000 AFIX 0 C2 1 0.225999 0.056908 1.099397 11.00000 0.09465 0.14186 = 0.05445 0.02652 -0.01216 0.01606 AFIX 43 H2 2 0.284115 0.006816 1.141842 11.00000 -1.20000 AFIX 0 C3 1 0.080770 0.138331 1.147814 11.00000 0.08784 0.15050 = 0.04305 0.01332 -0.01527 -0.01855 AFIX 43 H3 2 0.040788 0.144714 1.223230 11.00000 -1.20000 AFIX 0 C4 1 -0.006735 0.210804 1.086328 11.00000 0.06413 0.10636 = 0.04982 -0.01440 -0.00695 -0.00594 AFIX 43 H4 2 -0.107445 0.265225 1.119874 11.00000 -1.20000 AFIX 0 C5 1 0.053905 0.203584 0.974194 11.00000 0.05693 0.07161 = 0.04702 -0.00474 -0.01502 -0.00571 AFIX 43 H5 2 -0.005780 0.253491 0.932482 11.00000 -1.20000 AFIX 0 C6 1 0.203762 0.121960 0.923715 11.00000 0.04824 0.05292 = 0.04115 0.00159 -0.01204 -0.00855 C7 1 0.286041 0.111191 0.804687 11.00000 0.04688 0.03991 = 0.04629 -0.00034 -0.01376 -0.00700 C8 1 0.204526 0.189749 0.723409 11.00000 0.04227 0.03871 = 0.04157 -0.00177 -0.01337 -0.00700 C9 1 0.302849 0.140458 0.605655 11.00000 0.04149 0.03650 = 0.03726 -0.00087 -0.01088 -0.00780 AFIX 13 H9 2 0.421706 0.131974 0.593654 11.00000 -1.20000 AFIX 0 C10 1 0.278275 0.024010 0.571119 11.00000 0.04008 0.03550 = 0.04421 -0.00420 -0.00153 -0.00709 C11 1 0.288582 -0.085786 0.623256 11.00000 0.06522 0.04061 = 0.05405 0.00287 -0.01259 -0.00969 AFIX 43 H11 2 0.314898 -0.096635 0.688579 11.00000 -1.20000 AFIX 0 C12 1 0.258091 -0.178736 0.574111 11.00000 0.07003 0.03743 = 0.07508 -0.00217 -0.00721 -0.01529 AFIX 43 H12 2 0.262027 -0.252187 0.608238 11.00000 -1.20000 AFIX 0 C13 1 0.222310 -0.164522 0.476355 11.00000 0.05774 0.05356 = 0.07003 -0.01713 -0.00819 -0.01891 AFIX 43 H13 2 0.203047 -0.228053 0.445035 11.00000 -1.20000 AFIX 0 C14 1 0.215095 -0.056764 0.425246 11.00000 0.05782 0.05345 = 0.05392 -0.01430 -0.01099 -0.01682 AFIX 43 H14 2 0.192763 -0.047095 0.358617 11.00000 -1.20000 AFIX 0 C15 1 0.241125 0.036835 0.473263 11.00000 0.04295 0.04431 = 0.04386 -0.00520 -0.00738 -0.01051 C16 1 0.234665 0.160887 0.432698 11.00000 0.06153 0.05023 = 0.04111 -0.00159 -0.01997 -0.01367 AFIX 23 H16A 2 0.327847 0.161587 0.369027 11.00000 -1.20000 H16B 2 0.131645 0.196609 0.415274 11.00000 -1.20000 AFIX 0 C17 1 0.184750 0.341204 0.546289 11.00000 0.05553 0.03444 = 0.05345 0.00781 -0.02097 -0.01394 AFIX 43 H17 2 0.150621 0.389989 0.493126 11.00000 -1.20000 AFIX 0 C18 1 0.171792 0.392569 0.641579 11.00000 0.05252 0.03286 = 0.05878 -0.00268 -0.02295 -0.00764 C19 1 0.211773 0.323217 0.736066 11.00000 0.04490 0.03977 = 0.04617 -0.00731 -0.01456 -0.00697 AFIX 13 H19 2 0.124633 0.358649 0.802198 11.00000 -1.20000 AFIX 0 C20 1 0.375027 0.332134 0.747120 11.00000 0.04209 0.04391 = 0.05445 -0.00531 -0.01358 -0.00659 AFIX 43 H20 2 0.471872 0.294860 0.693908 11.00000 -1.20000 AFIX 0 C21 1 0.388411 0.389540 0.827608 11.00000 0.04729 0.05819 = 0.06181 -0.01184 -0.02061 -0.00745 AFIX 43 H21 2 0.295667 0.411207 0.888116 11.00000 -1.20000 AFIX 0 C22 1 0.030290 0.186103 0.742470 11.00000 0.04507 0.03880 = 0.04149 -0.00648 -0.00999 -0.00654 C23 1 0.550599 0.300516 0.993586 11.00000 0.16565 0.08070 = 0.11676 -0.00615 -0.09170 0.00680 AFIX 137 H23A 2 0.433559 0.333834 1.026183 11.00000 -1.50000 H23B 2 0.606662 0.289714 1.048636 11.00000 -1.50000 H23C 2 0.568671 0.224203 0.959324 11.00000 -1.50000 AFIX 0 C24 1 0.616283 0.382875 0.911856 11.00000 0.08948 0.06418 = 0.13173 -0.04404 -0.06360 0.02507 C25 1 0.543639 0.422931 0.829003 11.00000 0.06007 0.06347 = 0.09565 -0.02532 -0.03940 0.00217 C26 1 0.609896 0.498960 0.749032 11.00000 0.05880 0.09209 = 0.12885 -0.00299 -0.02477 -0.03819 C27 1 0.534395 0.553811 0.663340 11.00000 0.14768 0.16826 = 0.15474 0.07196 -0.06300 -0.09044 AFIX 137 H27A 2 0.594279 0.510251 0.595818 11.00000 -1.50000 H27B 2 0.539509 0.636091 0.655258 11.00000 -1.50000 H27C 2 0.420397 0.550689 0.683330 11.00000 -1.50000 AFIX 0 N1 3 0.244477 0.223634 0.526135 11.00000 0.05613 0.03998 = 0.04036 0.00388 -0.01758 -0.01448 N2 3 0.115336 0.518886 0.652739 11.00000 0.06691 0.03943 = 0.08305 -0.00291 -0.03563 -0.01094 N3 3 -0.102808 0.184021 0.752394 11.00000 0.05228 0.06978 = 0.06448 -0.01550 -0.01329 -0.01431 O1 4 0.423371 0.044684 0.767277 11.00000 0.05392 0.06783 = 0.05309 -0.00094 -0.01324 0.01186 O2 4 0.090502 0.565680 0.742005 11.00000 0.09122 0.04655 = 0.09380 -0.01893 -0.04318 -0.00407 O3 4 0.095064 0.579939 0.572570 11.00000 0.11581 0.04095 = 0.10570 0.01634 -0.06366 -0.02025 O4 4 0.742870 0.416723 0.916346 11.00000 0.08678 0.11148 = 0.22392 -0.08030 -0.10314 0.01708 O5 4 0.742250 0.530230 0.751321 11.00000 0.07333 0.14409 = 0.21405 -0.02265 -0.03346 -0.05302 AFIX 147 H5A 2 0.782613 0.489909 0.795780 11.00000 -1.50000 AFIX 0 HKLF 4 REM A in P-1 #2 REM R1 = 0.0685 for 2473 Fo > 4sig(Fo) and 0.1507 for all 4927 data REM 320 parameters refined using 2 restraints END WGHT 0.0856 0.0000 REM Highest difference peak 0.423, deepest hole -0.283, 1-sigma level 0.047 Q1 1 0.6326 0.3459 1.0412 11.00000 0.05 0.42 Q2 1 0.4057 0.2833 1.0712 11.00000 0.05 0.31 Q3 1 0.6569 0.4424 0.8083 11.00000 0.05 0.27 Q4 1 0.5011 0.3747 0.8959 11.00000 0.05 0.26 Q5 1 0.7518 0.4615 0.8221 11.00000 0.05 0.24 Q6 1 0.7800 0.4253 0.9134 11.00000 0.05 0.24 Q7 1 0.2595 0.0197 0.5197 11.00000 0.05 0.20 Q8 1 0.5560 0.3267 0.9794 11.00000 0.05 0.19 Q9 1 0.2997 -0.0200 0.5867 11.00000 0.05 0.18 Q10 1 0.2205 0.0397 0.5854 11.00000 0.05 0.17 Q11 1 0.1958 0.2331 0.7394 11.00000 0.05 0.17 Q12 1 0.4527 0.2433 1.0001 11.00000 0.05 0.17 Q13 1 0.3280 -0.3308 0.3655 11.00000 0.05 0.17 Q14 1 -0.0095 0.6801 0.6616 11.00000 0.05 0.16 Q15 1 0.6077 0.4670 0.7012 11.00000 0.05 0.16 Q16 1 0.5448 0.4090 0.8024 11.00000 0.05 0.15 Q17 1 0.0566 0.0470 0.9379 11.00000 0.05 0.15 Q18 1 0.1717 0.0513 0.4957 11.00000 0.05 0.15 Q19 1 0.6409 0.3788 0.7505 11.00000 0.05 0.15 Q20 1 0.2604 0.0873 0.4597 11.00000 0.05 0.14 REM The information below was added by Olex2. REM REM R1 = 0.0685 for 2473 Fo > 4sig(Fo) and 0.1507 for all 18524 data REM n/a parameters refined using n/a restraints REM Highest difference peak 0.42, deepest hole -0.28 REM Mean Shift 0, Max Shift 0.000. REM +++ Tabular Listing of Refinement Information +++ REM R1_all = 0.1507 REM R1_gt = 0.0685 REM wR_ref = 0.1937 REM GOOF = 1.019 REM Shift_max = 0.000 REM Shift_mean = 0 REM Reflections_all = 18524 REM Reflections_gt = 2473 REM Parameters = n/a REM Hole = -0.28 REM Peak = 0.42 REM Flack = n/a ; _olex2_submission_special_instructions 'No special instructions were received' ####################################################################### # # This file contains crystal structure data downloaded from the # Cambridge Structural Database (CSD) hosted by the Cambridge # Crystallographic Data Centre (CCDC). # # Full information about CCDC data access policies and citation # guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 # # Audit and citation data items may have been added by the CCDC. # Please retain this information to preserve the provenance of # this file and to allow appropriate attribution of the data. # ####################################################################### data_hd_wql33 _database_code_depnum_ccdc_archive 'CCDC 2086413' loop_ _audit_author_name _audit_author_address 'Qilin Wang' ;Henan University China ; _audit_update_record ; 2021-05-28 deposited with the CCDC. 2021-11-08 downloaded from the CCDC. ; _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety 'C25 H23 F N2 O5' _chemical_formula_sum 'C25 H23 F N2 O5' _chemical_formula_iupac ? _chemical_formula_weight 450.45 _chemical_melting_point ? _space_group_crystal_system monoclinic _space_group_name_H-M_alt 'P 1 21/c 1' _space_group_name_Hall '-P 2ybc' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 5.98830(10) _cell_length_b 22.0176(5) _cell_length_c 16.5031(4) _cell_angle_alpha 90 _cell_angle_beta 95.3100(10) _cell_angle_gamma 90 _cell_volume 2166.56(8) _cell_formula_units_Z 4 _cell_measurement_reflns_used 9803 _cell_measurement_theta_min 2.6890 _cell_measurement_theta_max 72.4123 _cell_measurement_temperature 100.(2) _exptl_crystal_description prism _exptl_crystal_colour 'translucent light yellow' _exptl_crystal_size_max 0.470 _exptl_crystal_size_mid 0.090 _exptl_crystal_size_min 0.080 _exptl_crystal_density_diffrn 1.381 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 944 _exptl_absorpt_coefficient_mu 0.854 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_process_details ; SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction ; _exptl_absorpt_correction_T_min 0.64 _exptl_absorpt_correction_T_max 0.94 _exptl_special_details ; ; _diffrn_ambient_temperature 100.(2) _diffrn_source 'Ius Diamond' _diffrn_source_type Microfocus _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_monochromator 'Helixos MX multilayer Optic' _diffrn_measurement_device_type 'Bruker D8 QUEST PHOTON II' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean 7.3910 _diffrn_reflns_number 24084 _diffrn_reflns_av_R_equivalents 0.0784 _diffrn_reflns_av_unetI/netI 0.0488 _diffrn_reflns_theta_min 3.36 _diffrn_reflns_theta_max 72.43 _diffrn_reflns_theta_full 72.43 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measured_fraction_theta_full 0.999 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _refine_special_details ; ; _reflns_number_total 4294 _reflns_number_gt 3737 _reflns_threshold_expression 'I > 2\s(I)' _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_R_factor_all 0.0553 _refine_ls_R_factor_gt 0.0492 _refine_ls_wR_factor_gt 0.1297 _refine_ls_wR_factor_ref 0.1362 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.053 _refine_ls_number_reflns 4294 _refine_ls_number_parameters 300 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_hydrogen_treatment constr _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0751P)^2^+0.8196P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.399 _refine_diff_density_min -0.300 _refine_ls_extinction_method 'SHELXL-2017/1 (Sheldrick 2017)' _refine_ls_extinction_coef 0.0028(4) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _computing_data_collection 'Bruker Instrument Service vV6.2.9' _computing_cell_refinement 'SAINT V8.38A (Bruker AXS Inc., 2017)' _computing_data_reduction 'SAINT V8.38A (Bruker AXS Inc., 2017)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _computing_structure_refinement 'SHELXL-2017/1 (Sheldrick, 2017)' _computing_molecular_graphics ? _computing_publication_material ? loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_refinement_flags_posn _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group F F1 0.80594(17) 0.52158(6) 0.10900(6) 0.0346(3) Uani d . . . 1 . . O O1 0.73516(19) 0.85827(5) 0.41638(7) 0.0252(3) Uani d . . . 1 . . O O2 0.9859(2) 0.79244(6) 0.47693(8) 0.0290(3) Uani d . . . 1 . . O O3 -0.02811(18) 0.63977(6) 0.36829(8) 0.0256(3) Uani d . . . 1 . . O O4 0.5630(2) 0.58590(6) 0.62521(7) 0.0269(3) Uani d . . . 1 . . O O5 0.8514(2) 0.53918(6) 0.58384(7) 0.0271(3) Uani d . . . 1 . . N N1 0.6018(2) 0.54737(6) 0.35241(8) 0.0186(3) Uani d . . . 1 . . N N2 0.6709(2) 0.56763(6) 0.56886(8) 0.0206(3) Uani d . . . 1 . . C C1 0.8101(3) 0.93517(9) 0.32267(11) 0.0305(4) Uani d . . . 1 . . H H23 0.729973 0.91083 0.279561 0.046 Uiso calc U . R 1 . . H H3 0.927314 0.959032 0.299762 0.046 Uiso calc U . R 1 . . H H1 0.704531 0.9626 0.34615 0.046 Uiso calc U . R 1 . . C C2 0.9153(3) 0.89382(8) 0.38787(11) 0.0273(4) Uani d . . . 1 . . H H22 1.027279 0.866968 0.365556 0.033 Uiso calc U . R 1 . . H H21 0.991347 0.917841 0.433057 0.033 Uiso calc U . R 1 . . C C3 0.7941(3) 0.80759(7) 0.45961(10) 0.0214(3) Uani d . . . 1 . . C C4 0.5916(3) 0.77458(8) 0.47814(10) 0.0222(3) Uani d . . . 1 . . H H4 0.450812 0.794735 0.471753 0.027 Uiso calc U . R 1 . . C C5 0.6003(3) 0.71736(8) 0.50354(10) 0.0208(3) Uani d . . . 1 . . H H5 0.743209 0.698695 0.513414 0.025 Uiso calc U . R 1 . . C C6 0.3971(3) 0.68070(7) 0.51746(10) 0.0210(3) Uani d . . . 1 . . H H7 0.261276 0.705018 0.501214 0.025 Uiso calc U . R 1 . . H H6 0.398441 0.671681 0.576275 0.025 Uiso calc U . R 1 . . C C7 0.3845(2) 0.62023(7) 0.46932(9) 0.0185(3) Uani d . . . 1 . . H H20 0.245144 0.598183 0.481094 0.022 Uiso calc U . R 1 . . C C8 0.3688(2) 0.63557(7) 0.37703(9) 0.0170(3) Uani d . . . 1 . . H H13 0.492685 0.663991 0.366073 0.02 Uiso calc U . R 1 . . C C9 0.3870(2) 0.57710(7) 0.32668(9) 0.0178(3) Uani d . . . 1 . . H H12 0.261041 0.549149 0.336953 0.021 Uiso calc U . R 1 . . C C10 0.3998(3) 0.58315(7) 0.23612(10) 0.0201(3) Uani d . . . 1 . . C C11 0.2483(3) 0.61055(8) 0.17821(11) 0.0249(4) Uani d . . . 1 . . H H11 0.117153 0.629898 0.193866 0.03 Uiso calc U . R 1 . . C C12 0.2929(3) 0.60900(8) 0.09685(11) 0.0301(4) Uani d . . . 1 . . H H8 0.192809 0.628436 0.056962 0.036 Uiso calc U . R 1 . . C C13 0.4809(3) 0.57957(9) 0.07316(11) 0.0293(4) Uani d . . . 1 . . H H2 0.509848 0.578608 0.017536 0.035 Uiso calc U . R 1 . . C C14 0.5836(2) 0.57840(7) 0.48822(9) 0.0187(3) Uani d . . . 1 . . C C15 0.6870(2) 0.54810(7) 0.42923(10) 0.0185(3) Uani d . . . 1 . . H H19 0.823244 0.527102 0.444031 0.022 Uiso calc U . R 1 . . C C16 0.6254(3) 0.55168(8) 0.13179(11) 0.0246(4) Uani d . . . 1 . . C C17 0.5886(3) 0.55340(7) 0.21322(10) 0.0212(3) Uani d . . . 1 . . C C18 0.7182(3) 0.52339(8) 0.28492(10) 0.0216(3) Uani d . . . 1 . . H H9 0.707323 0.478581 0.281615 0.026 Uiso calc U . R 1 . . H H10 0.878033 0.535537 0.289622 0.026 Uiso calc U . R 1 . . C C19 0.1419(2) 0.66540(7) 0.35106(9) 0.0186(3) Uani d . . . 1 . . C C20 0.1251(3) 0.72164(7) 0.30036(9) 0.0192(3) Uani d . . . 1 . . C C21 -0.0838(3) 0.73538(8) 0.25923(10) 0.0244(4) Uani d . . . 1 . . H H14 -0.208385 0.709632 0.265349 0.029 Uiso calc U . R 1 . . C C22 -0.1105(3) 0.78619(9) 0.20965(11) 0.0286(4) Uani d . . . 1 . . H H15 -0.25232 0.794694 0.181223 0.034 Uiso calc U . R 1 . . C C23 0.0698(3) 0.82465(8) 0.20153(11) 0.0278(4) Uani d . . . 1 . . H H16 0.051018 0.859673 0.16796 0.033 Uiso calc U . R 1 . . C C24 0.2773(3) 0.81191(8) 0.24247(10) 0.0246(4) Uani d . . . 1 . . H H18 0.400306 0.838446 0.237376 0.03 Uiso calc U . R 1 . . C C25 0.3055(3) 0.76019(7) 0.29110(10) 0.0203(3) Uani d . . . 1 . . H H17 0.448662 0.751173 0.318104 0.024 Uiso calc U . R 1 . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 F1 0.0255(5) 0.0488(7) 0.0297(6) 0.0073(5) 0.0037(4) -0.0029(5) O1 0.0207(6) 0.0238(6) 0.0304(6) 0.0020(5) -0.0012(5) 0.0060(5) O2 0.0190(6) 0.0258(6) 0.0397(7) -0.0023(5) -0.0111(5) 0.0035(5) O3 0.0119(5) 0.0294(6) 0.0347(7) -0.0026(4) -0.0018(5) 0.0050(5) O4 0.0296(6) 0.0292(6) 0.0212(6) 0.0014(5) -0.0016(5) 0.0010(5) O5 0.0219(6) 0.0290(6) 0.0280(6) 0.0046(5) -0.0106(5) 0.0041(5) N1 0.0122(6) 0.0206(7) 0.0217(7) 0.0006(5) -0.0049(5) 0.0003(5) N2 0.0173(6) 0.0201(7) 0.0229(7) -0.0028(5) -0.0062(5) 0.0027(5) C1 0.0296(9) 0.0285(9) 0.0319(9) -0.0046(7) -0.0045(7) 0.0076(7) C2 0.0233(8) 0.0285(9) 0.0291(9) -0.0037(7) -0.0027(7) 0.0036(7) C3 0.0227(8) 0.0184(7) 0.0218(7) 0.0007(6) -0.0054(6) -0.0025(6) C4 0.0184(7) 0.0239(8) 0.0232(8) 0.0019(6) -0.0039(6) -0.0014(6) C5 0.0169(7) 0.0237(8) 0.0204(7) 0.0011(6) -0.0065(6) -0.0025(6) C6 0.0172(7) 0.0219(8) 0.0230(8) 0.0012(6) -0.0017(6) -0.0004(6) C7 0.0129(7) 0.0209(8) 0.0208(7) -0.0025(6) -0.0030(6) 0.0021(6) C8 0.0110(6) 0.0179(7) 0.0213(7) -0.0009(5) -0.0032(5) 0.0014(6) C9 0.0108(6) 0.0193(7) 0.0221(8) -0.0011(5) -0.0059(5) 0.0002(6) C10 0.0158(7) 0.0209(7) 0.0222(8) -0.0035(6) -0.0057(6) -0.0013(6) C11 0.0221(8) 0.0252(8) 0.0256(8) 0.0049(6) -0.0073(6) -0.0025(6) C12 0.0351(10) 0.0289(9) 0.0239(8) 0.0045(7) -0.0098(7) 0.0023(7) C13 0.0321(9) 0.0323(9) 0.0225(8) -0.0014(7) -0.0033(7) 0.0012(7) C14 0.0139(7) 0.0191(7) 0.0217(8) -0.0030(6) -0.0052(6) 0.0032(6) C15 0.0124(7) 0.0175(7) 0.0243(8) -0.0025(5) -0.0055(6) 0.0032(6) C16 0.0191(8) 0.0282(9) 0.0259(8) -0.0014(6) -0.0006(6) -0.0013(6) C17 0.0155(7) 0.0219(8) 0.0248(8) -0.0024(6) -0.0057(6) -0.0003(6) C18 0.0147(7) 0.0260(8) 0.0232(8) 0.0024(6) -0.0037(6) -0.0015(6) C19 0.0114(7) 0.0227(8) 0.0209(7) 0.0008(6) -0.0029(6) -0.0008(6) C20 0.0141(7) 0.0230(8) 0.0200(7) 0.0037(6) -0.0013(6) -0.0006(6) C21 0.0143(7) 0.0309(9) 0.0273(8) 0.0039(6) -0.0015(6) 0.0013(7) C22 0.0175(7) 0.0378(10) 0.0291(9) 0.0112(7) -0.0058(7) 0.0040(7) C23 0.0266(8) 0.0305(9) 0.0260(8) 0.0095(7) 0.0015(7) 0.0081(7) C24 0.0212(8) 0.0256(8) 0.0271(8) 0.0012(6) 0.0021(6) 0.0037(7) C25 0.0149(7) 0.0233(8) 0.0218(7) 0.0026(6) -0.0028(6) 0.0019(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag F1 C16 . 1.351(2) ? O1 C3 . 1.353(2) ? O1 C2 . 1.447(2) ? O2 C3 . 1.205(2) ? O3 C19 . 1.220(2) ? O4 N2 . 1.2472(19) ? O5 N2 . 1.2539(18) ? N1 C15 . 1.322(2) ? N1 C18 . 1.466(2) ? N1 C9 . 1.4706(19) ? N2 C14 . 1.404(2) ? C1 C2 . 1.503(2) ? C1 H23 . 0.98 ? C1 H3 . 0.98 ? C1 H1 . 0.98 ? C2 H22 . 0.99 ? C2 H21 . 0.99 ? C3 C4 . 1.470(2) ? C4 C5 . 1.327(2) ? C4 H4 . 0.95 ? C5 C6 . 1.495(2) ? C5 H5 . 0.95 ? C6 C7 . 1.549(2) ? C6 H7 . 0.99 ? C6 H6 . 0.99 ? C7 C14 . 1.516(2) ? C7 C8 . 1.554(2) ? C7 H20 . 1.0 ? C8 C19 . 1.534(2) ? C8 C9 . 1.542(2) ? C8 H13 . 1.0 ? C9 C10 . 1.509(2) ? C9 H12 . 1.0 ? C10 C17 . 1.389(2) ? C10 C11 . 1.393(2) ? C11 C12 . 1.393(3) ? C11 H11 . 0.95 ? C12 C13 . 1.386(3) ? C12 H8 . 0.95 ? C13 C16 . 1.381(2) ? C13 H2 . 0.95 ? C14 C15 . 1.374(2) ? C15 H19 . 0.95 ? C16 C17 . 1.382(2) ? C17 C18 . 1.506(2) ? C18 H9 . 0.99 ? C18 H10 . 0.99 ? C19 C20 . 1.493(2) ? C20 C25 . 1.393(2) ? C20 C21 . 1.400(2) ? C21 C22 . 1.387(3) ? C21 H14 . 0.95 ? C22 C23 . 1.388(3) ? C22 H15 . 0.95 ? C23 C24 . 1.387(2) ? C23 H16 . 0.95 ? C24 C25 . 1.394(2) ? C24 H18 . 0.95 ? C25 H17 . 0.95 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C3 O1 C2 . . 116.84(13) ? C15 N1 C18 . . 124.38(13) ? C15 N1 C9 . . 121.40(13) ? C18 N1 C9 . . 113.93(12) ? O4 N2 O5 . . 120.72(13) ? O4 N2 C14 . . 118.63(13) ? O5 N2 C14 . . 120.64(14) ? C2 C1 H23 . . 109.5 ? C2 C1 H3 . . 109.5 ? H23 C1 H3 . . 109.5 ? C2 C1 H1 . . 109.5 ? H23 C1 H1 . . 109.5 ? H3 C1 H1 . . 109.5 ? O1 C2 C1 . . 106.55(14) ? O1 C2 H22 . . 110.4 ? C1 C2 H22 . . 110.4 ? O1 C2 H21 . . 110.4 ? C1 C2 H21 . . 110.4 ? H22 C2 H21 . . 108.6 ? O2 C3 O1 . . 123.35(16) ? O2 C3 C4 . . 126.90(15) ? O1 C3 C4 . . 109.71(13) ? C5 C4 C3 . . 121.75(15) ? C5 C4 H4 . . 119.1 ? C3 C4 H4 . . 119.1 ? C4 C5 C6 . . 123.54(15) ? C4 C5 H5 . . 118.2 ? C6 C5 H5 . . 118.2 ? C5 C6 C7 . . 112.77(13) ? C5 C6 H7 . . 109.0 ? C7 C6 H7 . . 109.0 ? C5 C6 H6 . . 109.0 ? C7 C6 H6 . . 109.0 ? H7 C6 H6 . . 107.8 ? C14 C7 C6 . . 114.62(12) ? C14 C7 C8 . . 107.98(12) ? C6 C7 C8 . . 108.16(12) ? C14 C7 H20 . . 108.6 ? C6 C7 H20 . . 108.6 ? C8 C7 H20 . . 108.6 ? C19 C8 C9 . . 108.18(12) ? C19 C8 C7 . . 109.80(12) ? C9 C8 C7 . . 110.24(12) ? C19 C8 H13 . . 109.5 ? C9 C8 H13 . . 109.5 ? C7 C8 H13 . . 109.5 ? N1 C9 C10 . . 101.65(12) ? N1 C9 C8 . . 108.65(11) ? C10 C9 C8 . . 118.21(13) ? N1 C9 H12 . . 109.3 ? C10 C9 H12 . . 109.3 ? C8 C9 H12 . . 109.3 ? C17 C10 C11 . . 120.82(15) ? C17 C10 C9 . . 110.18(13) ? C11 C10 C9 . . 128.91(15) ? C10 C11 C12 . . 118.68(16) ? C10 C11 H11 . . 120.7 ? C12 C11 H11 . . 120.7 ? C13 C12 C11 . . 121.08(16) ? C13 C12 H8 . . 119.5 ? C11 C12 H8 . . 119.5 ? C16 C13 C12 . . 118.86(17) ? C16 C13 H2 . . 120.6 ? C12 C13 H2 . . 120.6 ? C15 C14 N2 . . 115.93(14) ? C15 C14 C7 . . 123.13(14) ? N2 C14 C7 . . 120.93(14) ? N1 C15 C14 . . 121.76(14) ? N1 C15 H19 . . 119.1 ? C14 C15 H19 . . 119.1 ? F1 C16 C13 . . 119.26(16) ? F1 C16 C17 . . 119.20(15) ? C13 C16 C17 . . 121.54(16) ? C16 C17 C10 . . 118.98(15) ? C16 C17 C18 . . 129.40(15) ? C10 C17 C18 . . 111.48(14) ? N1 C18 C17 . . 101.09(12) ? N1 C18 H9 . . 111.6 ? C17 C18 H9 . . 111.6 ? N1 C18 H10 . . 111.6 ? C17 C18 H10 . . 111.6 ? H9 C18 H10 . . 109.4 ? O3 C19 C20 . . 119.98(14) ? O3 C19 C8 . . 118.25(14) ? C20 C19 C8 . . 121.60(13) ? C25 C20 C21 . . 118.83(15) ? C25 C20 C19 . . 123.66(14) ? C21 C20 C19 . . 117.50(14) ? C22 C21 C20 . . 120.64(16) ? C22 C21 H14 . . 119.7 ? C20 C21 H14 . . 119.7 ? C21 C22 C23 . . 120.05(15) ? C21 C22 H15 . . 120.0 ? C23 C22 H15 . . 120.0 ? C24 C23 C22 . . 119.95(16) ? C24 C23 H16 . . 120.0 ? C22 C23 H16 . . 120.0 ? C23 C24 C25 . . 120.05(16) ? C23 C24 H18 . . 120.0 ? C25 C24 H18 . . 120.0 ? C20 C25 C24 . . 120.46(14) ? C20 C25 H17 . . 119.8 ? C24 C25 H17 . . 119.8 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag C3 O1 C2 C1 . . . . 163.46(15) ? C2 O1 C3 O2 . . . . 2.3(2) ? C2 O1 C3 C4 . . . . -175.58(14) ? O2 C3 C4 C5 . . . . -13.1(3) ? O1 C3 C4 C5 . . . . 164.70(15) ? C3 C4 C5 C6 . . . . -175.54(14) ? C4 C5 C6 C7 . . . . 125.06(17) ? C5 C6 C7 C14 . . . . 58.56(17) ? C5 C6 C7 C8 . . . . -61.95(16) ? C14 C7 C8 C19 . . . . 167.12(12) ? C6 C7 C8 C19 . . . . -68.31(15) ? C14 C7 C8 C9 . . . . 48.02(15) ? C6 C7 C8 C9 . . . . 172.60(11) ? C15 N1 C9 C10 . . . . 161.49(14) ? C18 N1 C9 C10 . . . . -12.57(16) ? C15 N1 C9 C8 . . . . 36.12(19) ? C18 N1 C9 C8 . . . . -137.94(13) ? C19 C8 C9 N1 . . . . -178.73(12) ? C7 C8 C9 N1 . . . . -58.66(15) ? C19 C8 C9 C10 . . . . 66.25(16) ? C7 C8 C9 C10 . . . . -173.68(12) ? N1 C9 C10 C17 . . . . 6.51(16) ? C8 C9 C10 C17 . . . . 125.27(14) ? N1 C9 C10 C11 . . . . -176.82(16) ? C8 C9 C10 C11 . . . . -58.1(2) ? C17 C10 C11 C12 . . . . -1.8(2) ? C9 C10 C11 C12 . . . . -178.11(16) ? C10 C11 C12 C13 . . . . 1.6(3) ? C11 C12 C13 C16 . . . . -0.2(3) ? O4 N2 C14 C15 . . . . -168.66(14) ? O5 N2 C14 C15 . . . . 9.9(2) ? O4 N2 C14 C7 . . . . 10.2(2) ? O5 N2 C14 C7 . . . . -171.17(13) ? C6 C7 C14 C15 . . . . -136.21(15) ? C8 C7 C14 C15 . . . . -15.60(19) ? C6 C7 C14 N2 . . . . 44.98(19) ? C8 C7 C14 N2 . . . . 165.60(13) ? C18 N1 C15 C14 . . . . 171.03(14) ? C9 N1 C15 C14 . . . . -2.4(2) ? N2 C14 C15 N1 . . . . 170.13(14) ? C7 C14 C15 N1 . . . . -8.7(2) ? C12 C13 C16 F1 . . . . 178.33(16) ? C12 C13 C16 C17 . . . . -1.1(3) ? F1 C16 C17 C10 . . . . -178.47(14) ? C13 C16 C17 C10 . . . . 1.0(3) ? F1 C16 C17 C18 . . . . -3.0(3) ? C13 C16 C17 C18 . . . . 176.43(17) ? C11 C10 C17 C16 . . . . 0.5(2) ? C9 C10 C17 C16 . . . . 177.46(14) ? C11 C10 C17 C18 . . . . -175.74(15) ? C9 C10 C17 C18 . . . . 1.25(18) ? C15 N1 C18 C17 . . . . -160.70(14) ? C9 N1 C18 C17 . . . . 13.16(16) ? C16 C17 C18 N1 . . . . 175.85(16) ? C10 C17 C18 N1 . . . . -8.43(17) ? C9 C8 C19 O3 . . . . 68.56(18) ? C7 C8 C19 O3 . . . . -51.79(19) ? C9 C8 C19 C20 . . . . -106.63(16) ? C7 C8 C19 C20 . . . . 133.02(15) ? O3 C19 C20 C25 . . . . 166.90(16) ? C8 C19 C20 C25 . . . . -18.0(2) ? O3 C19 C20 C21 . . . . -14.1(2) ? C8 C19 C20 C21 . . . . 161.05(15) ? C25 C20 C21 C22 . . . . 0.5(3) ? C19 C20 C21 C22 . . . . -178.61(15) ? C20 C21 C22 C23 . . . . -1.2(3) ? C21 C22 C23 C24 . . . . 0.6(3) ? C22 C23 C24 C25 . . . . 0.7(3) ? C21 C20 C25 C24 . . . . 0.8(2) ? C19 C20 C25 C24 . . . . 179.80(15) ? C23 C24 C25 C20 . . . . -1.3(3) ? _shelx_res_file ; TITL hd_wql33_0m_a.res in P2(1)/c hd_wql33_0m.res created by SHELXL-2017/1 at 20:51:51 on 14-Oct-2020 CELL 1.54178 5.9883 22.0176 16.5031 90.000 95.310 90.000 ZERR 4.00 0.0001 0.0005 0.0004 0.000 0.001 0.000 LATT 1 SYMM -x, y+1/2, -z+1/2 SFAC C H N O F UNIT 100 92 8 20 4 LIST 4 ! automatically inserted. Change 6 to 4 for CHECKCIF!! TEMP -173.160 SIZE 0.080 0.090 0.470 ACTA L.S. 4 FMAP 2 PLAN -5 0 0.00 HTAB BOND $H CONF WGHT 0.075100 0.819600 EXTI 0.002794 FVAR 0.61392 F1 5 0.805938 0.521579 0.109000 11.00000 0.02546 0.04878 = 0.02974 -0.00289 0.00370 0.00730 O1 4 0.735160 0.858266 0.416375 11.00000 0.02071 0.02378 = 0.03042 0.00597 -0.00120 0.00196 O2 4 0.985892 0.792438 0.476932 11.00000 0.01896 0.02581 = 0.03971 0.00345 -0.01112 -0.00234 O3 4 -0.028107 0.639773 0.368289 11.00000 0.01192 0.02941 = 0.03474 0.00499 -0.00182 -0.00255 O4 4 0.562966 0.585902 0.625209 11.00000 0.02963 0.02918 = 0.02118 0.00096 -0.00164 0.00141 O5 4 0.851385 0.539182 0.583844 11.00000 0.02187 0.02897 = 0.02802 0.00410 -0.01063 0.00462 N1 3 0.601808 0.547372 0.352412 11.00000 0.01217 0.02056 = 0.02173 0.00028 -0.00494 0.00058 N2 3 0.670890 0.567634 0.568860 11.00000 0.01730 0.02013 = 0.02286 0.00272 -0.00622 -0.00276 C1 1 0.810143 0.935166 0.322665 11.00000 0.02958 0.02849 = 0.03192 0.00757 -0.00451 -0.00459 AFIX 137 H23 2 0.729973 0.910830 0.279561 11.00000 -1.50000 H3 2 0.927314 0.959032 0.299762 11.00000 -1.50000 H1 2 0.704531 0.962600 0.346150 11.00000 -1.50000 AFIX 0 C2 1 0.915350 0.893822 0.387869 11.00000 0.02334 0.02848 = 0.02907 0.00359 -0.00266 -0.00369 AFIX 23 H22 2 1.027279 0.866968 0.365556 11.00000 -1.20000 H21 2 0.991347 0.917841 0.433057 11.00000 -1.20000 AFIX 0 C3 1 0.794107 0.807592 0.459611 11.00000 0.02269 0.01844 = 0.02180 -0.00252 -0.00539 0.00071 C4 1 0.591611 0.774579 0.478136 11.00000 0.01841 0.02389 = 0.02322 -0.00137 -0.00395 0.00185 AFIX 43 H4 2 0.450812 0.794735 0.471753 11.00000 -1.20000 AFIX 0 C5 1 0.600254 0.717363 0.503542 11.00000 0.01694 0.02369 = 0.02037 -0.00248 -0.00645 0.00112 AFIX 43 H5 2 0.743209 0.698695 0.513414 11.00000 -1.20000 AFIX 0 C6 1 0.397130 0.680698 0.517463 11.00000 0.01720 0.02195 = 0.02304 -0.00036 -0.00166 0.00120 AFIX 23 H7 2 0.261276 0.705018 0.501214 11.00000 -1.20000 H6 2 0.398441 0.671681 0.576275 11.00000 -1.20000 AFIX 0 C7 1 0.384512 0.620235 0.469323 11.00000 0.01287 0.02090 = 0.02080 0.00206 -0.00302 -0.00252 AFIX 13 H20 2 0.245144 0.598183 0.481094 11.00000 -1.20000 AFIX 0 C8 1 0.368751 0.635567 0.377031 11.00000 0.01098 0.01788 = 0.02132 0.00141 -0.00316 -0.00089 AFIX 13 H13 2 0.492685 0.663991 0.366073 11.00000 -1.20000 AFIX 0 C9 1 0.386983 0.577102 0.326679 11.00000 0.01076 0.01927 = 0.02211 0.00023 -0.00591 -0.00107 AFIX 13 H12 2 0.261041 0.549149 0.336953 11.00000 -1.20000 AFIX 0 C10 1 0.399782 0.583152 0.236122 11.00000 0.01579 0.02086 = 0.02223 -0.00128 -0.00573 -0.00350 C11 1 0.248287 0.610545 0.178211 11.00000 0.02212 0.02525 = 0.02555 -0.00250 -0.00727 0.00489 AFIX 43 H11 2 0.117153 0.629898 0.193866 11.00000 -1.20000 AFIX 0 C12 1 0.292884 0.609002 0.096848 11.00000 0.03513 0.02888 = 0.02394 0.00229 -0.00979 0.00446 AFIX 43 H8 2 0.192809 0.628436 0.056962 11.00000 -1.20000 AFIX 0 C13 1 0.480893 0.579572 0.073156 11.00000 0.03209 0.03234 = 0.02252 0.00124 -0.00328 -0.00142 AFIX 43 H2 2 0.509848 0.578608 0.017536 11.00000 -1.20000 AFIX 0 C14 1 0.583642 0.578400 0.488217 11.00000 0.01393 0.01906 = 0.02170 0.00323 -0.00522 -0.00302 C15 1 0.686960 0.548098 0.429228 11.00000 0.01235 0.01747 = 0.02426 0.00324 -0.00552 -0.00247 AFIX 43 H19 2 0.823244 0.527102 0.444031 11.00000 -1.20000 AFIX 0 C16 1 0.625372 0.551679 0.131791 11.00000 0.01910 0.02817 = 0.02590 -0.00125 -0.00060 -0.00143 C17 1 0.588566 0.553396 0.213216 11.00000 0.01547 0.02187 = 0.02483 -0.00026 -0.00565 -0.00238 C18 1 0.718178 0.523395 0.284918 11.00000 0.01468 0.02602 = 0.02319 -0.00154 -0.00370 0.00239 AFIX 23 H9 2 0.707323 0.478581 0.281615 11.00000 -1.20000 H10 2 0.878033 0.535537 0.289622 11.00000 -1.20000 AFIX 0 C19 1 0.141939 0.665397 0.351062 11.00000 0.01144 0.02267 = 0.02091 -0.00078 -0.00294 0.00077 C20 1 0.125142 0.721643 0.300360 11.00000 0.01408 0.02301 = 0.01996 -0.00058 -0.00130 0.00366 C21 1 -0.083751 0.735378 0.259231 11.00000 0.01434 0.03092 = 0.02734 0.00127 -0.00149 0.00386 AFIX 43 H14 2 -0.208385 0.709632 0.265349 11.00000 -1.20000 AFIX 0 C22 1 -0.110517 0.786192 0.209653 11.00000 0.01754 0.03784 = 0.02905 0.00402 -0.00579 0.01124 AFIX 43 H15 2 -0.252320 0.794694 0.181223 11.00000 -1.20000 AFIX 0 C23 1 0.069765 0.824654 0.201531 11.00000 0.02656 0.03052 = 0.02603 0.00810 0.00145 0.00952 AFIX 43 H16 2 0.051018 0.859673 0.167960 11.00000 -1.20000 AFIX 0 C24 1 0.277287 0.811913 0.242471 11.00000 0.02119 0.02556 = 0.02714 0.00371 0.00212 0.00120 AFIX 43 H18 2 0.400306 0.838446 0.237376 11.00000 -1.20000 AFIX 0 C25 1 0.305473 0.760187 0.291101 11.00000 0.01493 0.02333 = 0.02178 0.00188 -0.00280 0.00258 AFIX 43 H17 2 0.448662 0.751173 0.318104 11.00000 -1.20000 AFIX 0 HKLF 4 1 1 0 0 0 1 0 0 0 1 REM hd_wql33_0m_a.res in P2(1)/c REM R1 = 0.0492 for 3737 Fo > 4sig(Fo) and 0.0553 for all 4294 data REM 300 parameters refined using 0 restraints END WGHT 0.0751 0.8196 REM Instructions for potential hydrogen bonds EQIV $1 x, -y+3/2, z-1/2 HTAB C1 O4_$1 EQIV $2 -x+2, y+1/2, -z+1/2 HTAB C1 F1_$2 EQIV $3 -x+1, -y+1, -z+1 HTAB C9 O5_$3 HTAB C13 O1_$1 EQIV $4 -x+2, -y+1, -z+1 HTAB C15 O5_$4 REM Highest difference peak 0.399, deepest hole -0.300, 1-sigma level 0.062 Q1 1 0.2623 0.6487 0.3678 11.00000 0.05 0.40 Q2 1 0.1741 0.8184 0.2343 11.00000 0.05 0.31 Q3 1 0.5003 0.7021 0.5135 11.00000 0.05 0.31 Q4 1 0.4914 0.5970 0.4806 11.00000 0.05 0.30 Q5 1 0.6858 0.7935 0.4663 11.00000 0.05 0.27 ; _shelx_res_checksum 30921 _shelx_hkl_file ; 1 0 0 1817.92 141.89 -1 0 0 1869.21 141.29 2 0 0 198.48 16.90 -2 0 0 201.08 15.40 2 0 0 165.98 18.50 3 0 0 792.32 62.89 3 0 0 760.62 67.09 4 0 0 663.63 61.89 4 0 0 723.53 55.09 4 0 0 574.74 53.69 5 0 0 387.66 34.90 -5 0 0 379.96 35.40 5 0 0 411.26 34.60 5 0 0 454.25 47.40 -6 0 0 260.57 26.60 6 0 0 288.37 26.30 -6 0 0 304.87 26.60 6 0 0 321.17 25.10 7 0 0 212.48 17.20 -7 0 0 195.28 17.30 -7 0 0 178.58 17.20 1 -1 0 23.00 2.60 1 -1 0 19.10 3.30 -1 -1 0 21.60 3.60 1 -1 0 29.70 2.80 -1 1 0 26.50 2.60 1 1 0 24.10 3.10 -1 1 0 21.00 2.60 -2 -1 0 347.57 25.60 2 -1 0 311.87 26.80 2 -1 0 292.17 29.10 2 1 0 329.77 27.60 -2 1 0 346.87 26.30 3 -1 0 166.88 20.00 3 -1 0 176.78 16.60 3 1 0 197.58 17.90 4 -1 0 24.30 6.00 4 -1 0 32.00 6.40 4 -1 0 37.30 10.20 4 1 0 24.10 4.80 -4 1 0 20.10 5.00 4 1 0 28.60 6.80 4 1 0 23.30 9.40 4 1 0 29.70 6.40 5 -1 0 197.38 28.70 -5 -1 0 173.08 19.10 5 -1 0 185.58 17.30 -5 -1 0 143.19 17.50 5 -1 0 168.28 17.30 -5 1 0 155.98 17.40 5 1 0 181.08 17.70 5 1 0 175.48 17.00 5 1 0 217.18 24.40 5 1 0 187.08 28.30 -5 1 0 191.68 18.00 6 -1 0 65.09 7.70 -6 -1 0 73.39 9.40 -6 -1 0 60.59 8.70 6 -1 0 68.59 8.40 6 1 0 66.49 8.40 -6 1 0 66.09 8.60 -6 1 0 73.89 9.10 -7 -1 0 10.40 2.70 7 -1 0 18.10 3.10 -7 -1 0 14.80 4.70 -7 1 0 17.30 3.00 7 1 0 12.00 2.30 -7 1 0 13.00 2.90 0 -2 0 290.27 22.20 0 -2 0 267.17 22.80 0 -2 0 298.37 22.70 0 2 0 277.07 22.20 1 -2 0 3128.59 261.27 1 -2 0 3478.95 259.37 -1 -2 0 3326.57 261.97 -1 2 0 3638.64 260.17 1 2 0 3589.64 260.77 -1 2 0 3177.58 259.57 2 -2 0 720.43 66.39 2 -2 0 794.42 63.49 -2 -2 0 847.02 62.89 -2 -2 0 729.63 67.69 2 2 0 853.91 65.19 -2 2 0 913.11 63.79 3 -2 0 134.89 12.70 3 -2 0 125.59 16.20 3 2 0 139.79 14.50 3 2 0 136.69 16.70 4 -2 0 72.19 8.80 4 -2 0 71.79 14.10 4 2 0 59.29 12.80 4 2 0 55.69 7.70 4 2 0 59.19 7.80 5 -2 0 122.19 12.80 5 -2 0 150.38 30.40 5 -2 0 128.89 12.80 -5 -2 0 111.69 13.30 5 2 0 156.78 24.20 5 2 0 129.69 12.50 5 2 0 102.39 12.60 -5 2 0 98.89 20.00 5 2 0 78.49 24.20 -5 2 0 103.39 12.80 -5 2 0 112.99 12.90 6 -2 0 42.10 5.80 6 -2 0 35.20 5.90 -6 -2 0 57.59 7.80 -6 -2 0 36.80 6.90 -6 2 0 35.50 6.60 6 2 0 40.50 6.10 -6 2 0 40.60 6.20 7 -2 0 4.70 1.60 -7 -2 0 3.10 1.70 -7 2 0 2.00 2.20 -7 2 0 4.90 1.60 7 2 0 5.20 1.70 0 -3 0 0.80 1.40 0 3 0 -0.50 0.30 0 3 0 0.10 1.00 0 3 0 0.20 0.40 -1 -3 0 1714.13 130.39 1 -3 0 1545.45 129.39 1 3 0 1662.83 128.79 -1 3 0 1538.95 127.09 -1 3 0 1802.42 128.49 -1 3 0 1698.83 127.59 -2 -3 0 2.80 3.70 2 -3 0 0.20 0.80 2 -3 0 -0.10 1.40 -2 3 0 1.30 1.30 2 3 0 0.20 1.40 3 -3 0 0.50 1.50 3 -3 0 -0.40 2.40 3 3 0 2.50 3.90 3 3 0 2.60 2.50 4 -3 0 -2.40 3.00 4 -3 0 -1.70 3.90 4 -3 0 -1.80 1.90 4 3 0 -1.10 2.30 4 3 0 2.30 3.80 4 3 0 -1.90 1.50 -4 3 0 2.30 2.30 4 3 0 -7.00 4.10 -4 3 0 1.30 2.10 5 -3 0 20.80 4.60 5 -3 0 18.30 12.90 5 -3 0 17.30 4.20 -5 -3 0 14.30 4.80 -5 -3 0 20.30 7.10 5 3 0 12.90 3.50 5 3 0 12.00 3.80 -5 3 0 20.10 5.00 5 3 0 13.80 9.40 -5 3 0 13.20 3.80 5 3 0 24.00 8.70 6 -3 0 156.88 14.80 6 -3 0 156.38 15.30 -6 -3 0 167.98 16.30 -6 -3 0 145.09 16.20 -6 3 0 187.98 16.40 6 3 0 140.39 15.30 -6 3 0 147.89 15.50 7 -3 0 241.38 19.10 -7 3 0 202.78 19.10 7 3 0 221.78 18.90 0 4 0 216.18 17.60 0 4 0 213.78 17.50 1 -4 0 466.45 41.00 -1 4 0 561.64 39.10 1 4 0 454.15 40.30 -1 4 0 510.45 40.30 2 -4 0 248.08 19.10 2 -4 0 248.18 23.60 2 4 0 262.87 22.30 -2 4 0 214.18 19.90 3 -4 0 392.06 39.40 3 -4 0 419.26 33.30 3 4 0 461.65 37.80 3 4 0 389.76 39.50 4 -4 0 100.69 18.20 4 -4 0 109.69 11.70 4 -4 0 119.59 12.10 4 4 0 119.79 18.50 4 4 0 117.19 15.30 4 4 0 104.69 11.40 -4 4 0 111.49 12.30 4 4 0 95.89 11.40 -4 4 0 124.69 12.30 5 -4 0 18.60 4.50 -5 -4 0 13.20 4.40 -5 -4 0 19.90 6.50 5 -4 0 11.60 13.50 5 -4 0 29.60 5.10 -5 4 0 18.30 4.50 -5 4 0 22.40 5.00 5 4 0 35.90 11.30 5 4 0 22.40 5.10 5 4 0 13.60 4.10 5 4 0 8.00 9.80 6 -4 0 31.50 5.10 6 -4 0 39.80 5.80 -6 -4 0 35.60 6.30 6 4 0 42.40 6.00 -6 4 0 40.40 6.00 -6 4 0 40.60 6.50 7 -4 0 32.90 4.70 -7 -4 0 34.90 5.10 7 4 0 37.20 4.60 -7 4 0 44.50 4.50 -7 4 0 42.00 5.20 0 5 0 -0.10 1.70 0 5 0 0.10 0.80 0 5 0 5.80 1.60 1 -5 0 8742.23 644.54 1 5 0 8038.40 643.34 -2 -5 0 476.95 46.50 2 -5 0 504.95 44.80 -2 5 0 529.85 40.90 2 5 0 542.75 43.60 3 -5 0 1861.21 154.08 3 5 0 2083.79 152.08 -3 5 0 1777.12 147.79 4 -5 0 249.48 23.60 4 -5 0 310.47 33.00 4 -5 0 250.87 23.40 4 5 0 233.58 23.10 -4 5 0 268.97 23.90 4 5 0 232.28 23.60 4 5 0 311.97 28.60 -4 5 0 256.37 23.80 -4 5 0 271.37 23.50 4 5 0 291.57 32.30 4 5 0 300.97 32.60 5 -5 0 291.57 38.30 5 -5 0 265.07 24.20 5 5 0 236.38 24.30 -5 5 0 273.37 24.30 5 5 0 296.97 31.50 -5 5 0 263.87 24.40 6 -5 0 33.30 5.10 6 -5 0 35.10 5.00 -6 -5 0 30.00 5.50 -6 5 0 31.40 5.80 -6 5 0 34.70 5.30 6 5 0 31.10 5.10 7 -5 0 71.89 6.60 -7 -5 0 51.59 7.70 7 5 0 69.99 7.90 7 5 0 47.50 6.80 -7 5 0 67.09 6.80 0 6 0 3065.99 229.98 0 6 0 2907.31 229.78 1 -6 0 5006.00 363.86 1 6 0 4735.63 363.36 1 6 0 4208.28 361.96 -1 6 0 4867.41 360.56 2 -6 0 718.03 64.99 -2 6 0 858.71 61.09 2 6 0 788.12 65.99 2 6 0 742.23 63.69 -3 -6 0 71.09 8.20 3 -6 0 74.39 12.70 -3 6 0 69.19 7.70 3 6 0 78.29 11.00 4 -6 0 440.16 43.10 4 -6 0 344.37 32.40 4 -6 0 361.06 32.40 4 6 0 435.06 42.70 4 6 0 379.86 40.70 4 6 0 444.96 38.40 -4 6 0 407.26 33.00 4 6 0 357.86 32.70 4 6 0 320.17 32.40 -4 6 0 386.76 32.40 5 -6 0 -0.50 1.40 5 -6 0 1.70 1.90 -5 6 0 0.60 2.00 5 6 0 4.60 2.30 5 6 0 -12.00 9.00 -5 6 0 0.50 1.80 -6 -6 0 81.49 10.50 6 -6 0 94.69 9.70 6 -6 0 91.19 9.50 -6 6 0 85.29 9.80 -6 6 0 90.19 9.70 6 6 0 87.69 10.00 -7 -6 0 2.00 1.60 7 -6 0 1.50 1.30 7 6 0 2.00 1.20 -7 6 0 2.50 1.20 -7 6 0 2.70 4.00 -7 6 0 1.00 1.50 0 7 0 -0.60 1.00 0 7 0 -0.90 0.90 0 7 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10.60 -3 -8 0 49.80 6.90 3 8 0 40.80 9.60 4 -8 0 253.27 24.10 4 -8 0 251.77 23.80 4 8 0 270.07 32.10 4 8 0 300.87 34.00 -4 8 0 309.57 24.50 -4 8 0 281.17 24.00 4 8 0 304.27 30.30 4 8 0 225.08 24.00 5 -8 0 190.88 18.90 5 -8 0 218.78 19.10 -5 8 0 230.78 19.30 -5 8 0 203.18 19.10 5 8 0 209.18 30.50 5 8 0 168.98 28.10 5 8 0 183.08 19.20 -6 -8 0 -0.90 2.00 6 -8 0 1.80 1.60 6 -8 0 1.80 1.50 -6 8 0 -0.20 1.30 -6 8 0 -1.60 2.30 -6 8 0 3.80 1.80 6 8 0 -0.50 1.50 -7 -8 0 20.00 3.40 7 -8 0 12.10 2.10 7 8 0 14.60 1.80 -7 8 0 8.80 2.00 0 9 0 -0.10 3.70 0 9 0 0.80 1.60 0 9 0 -0.40 1.50 1 -9 0 628.64 54.49 1 9 0 632.64 53.49 1 9 0 661.03 52.19 -1 9 0 596.44 49.99 2 -9 0 119.19 16.90 2 9 0 124.79 17.20 2 9 0 126.59 14.50 -2 9 0 114.89 11.00 3 -9 0 29.60 5.00 3 -9 0 58.99 12.70 3 9 0 35.80 8.80 3 9 0 42.50 9.40 -3 9 0 38.00 5.50 4 -9 0 9.70 3.10 4 -9 0 7.20 2.50 4 9 0 23.90 9.00 -4 9 0 8.40 3.20 4 9 0 10.90 6.80 4 9 0 27.10 8.50 4 9 0 14.20 3.70 -4 9 0 13.20 3.20 5 -9 0 56.19 7.10 5 -9 0 55.09 7.00 5 9 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16.10 -3 14 0 94.09 9.80 -3 14 0 65.29 12.90 -3 14 0 108.19 13.00 4 -14 0 -1.30 1.70 4 -14 0 2.40 1.50 4 14 0 -0.90 1.40 4 14 0 0.00 2.50 -4 14 0 -0.30 1.20 4 14 0 -10.70 8.90 4 14 0 0.50 3.70 4 14 0 -1.20 7.30 -4 14 0 1.70 4.00 -4 14 0 4.30 2.30 5 -14 0 195.98 16.70 5 -14 0 214.38 17.70 -5 14 0 158.48 16.40 5 14 0 158.78 15.80 6 -14 0 17.80 4.10 -6 -14 0 5.50 2.10 6 -14 0 18.50 3.50 -6 14 0 10.30 2.30 0 15 0 -4.00 2.50 0 15 0 -0.90 1.80 0 15 0 0.50 3.50 1 -15 0 292.77 24.40 -1 15 0 317.47 25.00 -1 15 0 269.57 25.00 1 15 0 311.37 25.90 1 15 0 267.97 28.00 1 15 0 267.97 24.80 2 -15 0 6.20 2.60 2 15 0 18.80 4.10 2 15 0 8.10 5.80 2 15 0 1.80 3.50 -2 15 0 3.40 2.80 -2 15 0 9.50 2.60 3 -15 0 113.99 11.40 3 15 0 124.59 12.70 3 15 0 106.99 18.00 3 15 0 95.69 17.90 -3 15 0 112.79 11.70 -3 15 0 106.59 24.30 4 -15 0 10.10 2.60 -4 15 0 11.80 3.10 4 15 0 13.50 3.50 4 15 0 11.70 6.80 4 15 0 7.70 7.90 4 15 0 12.30 5.70 5 -15 0 284.57 22.60 5 -15 0 287.17 22.40 -5 15 0 234.28 22.50 5 15 0 234.28 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9.90 3 -4 9 63.09 7.80 3 -4 9 31.60 7.10 3 4 9 48.80 5.60 3 4 9 52.19 5.00 3 4 9 69.99 11.90 3 4 9 40.50 5.40 3 4 9 32.70 9.10 -3 4 -9 53.49 11.10 -4 -4 -9 236.88 21.90 -4 -4 -9 290.77 31.50 4 -4 9 255.87 20.80 4 -4 9 201.28 22.90 4 4 9 209.88 23.60 4 4 9 234.28 31.90 4 4 9 247.78 19.50 -4 4 -9 245.48 29.00 5 -4 9 565.34 53.29 -5 -4 -9 703.63 51.89 5 -4 9 664.93 50.69 5 4 9 590.64 53.29 6 -4 9 2.80 1.50 -6 -4 -9 5.80 1.70 6 -4 9 2.50 2.10 -6 4 -9 6.20 1.80 6 4 9 1.80 2.10 -6 -5 9 106.09 11.40 6 -5 -9 120.89 12.90 -6 -5 9 136.79 13.30 -6 5 9 146.89 16.80 -6 5 9 139.69 12.00 6 5 -9 119.89 12.70 6 5 -9 118.19 12.40 5 -5 -9 185.78 19.00 -5 -5 9 184.18 18.40 5 5 -9 169.08 18.80 5 5 -9 174.68 19.00 -5 5 9 187.38 17.40 -5 5 9 237.38 24.60 -4 -5 9 232.58 34.40 4 -5 -9 197.48 20.70 -4 -5 9 203.28 20.90 -4 -5 9 216.08 29.20 4 5 -9 198.78 21.50 -4 5 9 195.98 19.00 -4 5 9 281.67 31.40 4 5 -9 257.77 30.40 -3 -5 9 640.24 52.79 3 -5 -9 476.25 47.00 -3 -5 9 608.14 60.49 -3 -5 9 565.64 47.60 3 5 -9 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9 17.10 5.20 6 7 -9 22.30 3.90 5 -7 -9 216.68 20.90 -5 -7 9 208.38 20.90 -5 7 9 231.08 19.40 -5 7 9 257.77 26.50 5 7 -9 182.68 20.80 5 7 -9 211.68 21.30 -4 -7 9 -9.90 13.50 -4 -7 9 2.00 5.50 -4 -7 9 29.70 23.10 4 -7 -9 0.30 2.30 -4 -7 9 9.60 3.40 -4 7 9 3.10 3.40 -4 7 9 -3.70 13.30 -4 7 9 -0.20 1.30 4 7 -9 3.40 7.60 4 7 -9 1.00 2.80 -3 -7 9 208.88 21.90 -3 -7 9 259.57 33.90 -3 7 9 235.88 22.30 3 7 -9 223.38 22.80 -3 7 9 236.88 25.20 -3 7 9 245.78 27.40 -3 7 9 224.38 19.90 -2 -7 9 26.10 10.00 -2 -7 9 17.30 6.70 -2 -7 9 31.50 6.00 -2 7 9 15.40 6.00 -2 7 9 20.80 7.60 -2 7 9 26.80 9.10 -2 7 9 26.90 8.20 2 7 -9 23.30 8.60 -2 7 9 23.40 3.70 2 7 -9 29.20 5.50 -1 -7 9 289.87 29.40 -1 -7 9 311.47 33.60 -1 -7 9 301.47 26.10 -1 7 9 296.27 29.90 -1 7 9 365.56 33.40 -1 7 9 307.37 27.40 1 7 -9 281.47 26.40 1 7 -9 287.57 28.50 -1 7 9 257.27 27.70 0 -7 -9 5.10 2.60 0 -7 9 1.80 3.20 0 -7 9 7.60 4.60 0 7 -9 3.70 3.00 0 7 9 1.30 2.30 0 7 9 3.50 4.80 0 7 -9 8.50 3.00 1 -7 9 4.20 3.90 1 -7 9 0.10 2.40 -1 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16.70 -4 -8 9 107.09 30.90 -4 8 9 129.69 11.70 -4 8 9 144.39 18.30 4 8 -9 121.09 22.00 4 8 -9 108.49 13.90 -4 8 9 73.19 18.50 3 -8 -9 71.99 10.20 -3 -8 9 114.19 20.50 -3 -8 9 80.89 11.10 -3 -8 9 101.99 17.80 -3 8 9 83.39 16.70 -3 8 9 105.59 11.60 -3 8 9 70.89 13.90 -3 8 9 122.09 17.20 -3 8 9 88.39 8.90 -2 -8 9 61.09 8.90 -2 -8 9 94.79 17.10 -2 -8 9 81.69 12.60 2 8 -9 76.39 9.60 2 8 -9 72.19 11.80 -2 8 9 81.19 13.30 -2 8 9 68.39 7.10 -2 8 9 78.79 10.00 -2 8 9 61.49 12.60 -2 8 9 71.79 11.00 -1 -8 9 503.85 43.80 -1 -8 9 553.94 52.49 -1 -8 9 528.85 47.20 -1 8 9 468.45 44.70 -1 8 9 591.64 50.69 -1 8 9 505.55 47.40 -1 8 9 511.35 45.80 1 8 -9 485.95 45.60 0 -8 9 1380.06 119.69 0 -8 9 1641.04 125.19 0 -8 9 1469.75 115.39 0 -8 -9 1556.84 115.29 0 8 9 1384.76 117.09 0 8 -9 1389.06 117.69 0 8 9 1284.27 114.59 0 8 9 1453.75 117.09 0 8 9 1435.56 119.79 0 8 9 1587.74 125.39 0 8 -9 1609.34 115.89 1 -8 9 137.29 19.50 1 -8 9 110.19 12.40 1 -8 9 155.08 13.20 1 -8 9 140.39 17.30 1 8 9 138.49 13.20 1 8 9 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8.10 1 4 19 64.59 10.60 2 5 -19 74.79 8.30 -2 5 19 79.29 8.50 -1 -5 19 46.60 6.30 1 5 -19 50.29 5.90 -1 5 19 51.39 6.50 -1 5 19 44.30 6.30 0 -5 19 15.20 3.70 0 5 19 16.30 3.90 1 -5 19 17.40 3.40 1 5 19 34.80 5.00 -1 5 -19 28.30 3.70 1 5 19 23.60 3.60 -2 -6 19 0.60 0.90 2 6 -19 -1.70 1.60 -2 6 19 1.10 1.20 -1 -6 19 3.20 1.70 -1 6 19 3.90 2.20 1 6 -19 8.60 2.10 -1 6 19 1.20 1.90 0 -6 19 0.30 1.20 0 6 -19 -1.10 2.00 0 6 19 -0.90 0.90 1 -6 19 0.50 2.60 1 6 19 4.00 1.80 -1 6 -19 7.10 1.90 1 6 19 5.60 2.10 -2 -7 19 136.79 11.70 2 7 -19 115.99 11.60 -2 7 19 101.19 11.40 -1 -7 19 20.80 3.90 -1 7 19 21.40 5.50 -1 7 19 26.50 4.80 1 7 -19 20.00 3.40 0 -7 19 37.20 5.30 0 7 19 50.59 5.90 0 7 -19 56.29 7.50 0 7 19 33.20 6.90 -1 7 -19 17.60 3.00 1 7 19 17.70 3.00 2 8 -19 3.80 1.40 -2 8 19 3.30 1.30 -1 -8 19 21.60 3.90 -1 8 19 30.60 4.50 -1 8 19 34.10 5.10 1 8 -19 30.40 4.20 0 -8 19 67.09 7.80 0 8 19 51.49 6.80 0 8 -19 53.49 6.60 -1 -9 19 1.50 1.50 -1 9 19 1.20 1.30 0 -9 19 0.80 1.30 0 9 -19 2.60 1.30 0 9 19 1.60 1.30 0 9 19 3.10 1.70 -2 0 20 9.30 2.10 -1 0 20 13.60 3.10 -1 0 20 21.30 3.40 0 0 20 73.89 8.50 0 0 20 101.69 9.10 -2 -1 20 7.20 2.00 -1 -1 20 -0.40 0.80 -1 1 20 0.20 1.20 -1 1 20 1.00 1.60 0 -1 20 11.40 2.40 0 -1 20 7.50 2.30 0 1 20 5.20 2.00 0 1 20 2.10 1.60 -2 2 20 18.80 3.00 -1 -2 20 28.80 4.20 -1 2 20 30.90 4.60 -1 2 20 23.40 3.80 0 -2 20 136.59 12.80 0 2 20 146.89 13.00 0 2 20 128.19 12.90 -1 -3 20 3.40 1.60 -1 3 20 3.90 1.60 -1 3 20 2.40 2.20 0 -3 20 19.20 3.30 0 3 20 26.20 3.50 -1 4 20 21.50 3.30 -1 4 20 17.10 3.60 1 4 -20 11.80 3.10 0 -4 20 62.79 6.50 0 4 20 54.89 6.50 1 5 -20 4.20 1.80 -1 5 20 1.40 1.10 -1 5 20 4.80 2.00 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 87899 ####################################################################### # # This file contains crystal structure data downloaded from the # Cambridge Structural Database (CSD) hosted by the Cambridge # Crystallographic Data Centre (CCDC). # # Full information about CCDC data access policies and citation # guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 # # Audit and citation data items may have been added by the CCDC. # Please retain this information to preserve the provenance of # this file and to allow appropriate attribution of the data. # ####################################################################### data_wll148 _database_code_depnum_ccdc_archive 'CCDC 2071232' loop_ _audit_author_name _audit_author_address 'Qilin Wang' ;Henan University China ; _audit_update_record ; 2021-03-18 deposited with the CCDC. 2021-11-08 downloaded from the CCDC. ; _audit_creation_date 2019-12-18 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _shelx_SHELXL_version_number 2014/7 _chemical_name_common ? _chemical_name_systematic ? _chemical_formula_moiety 'C26 H23 N3 O4' _chemical_formula_sum 'C26 H23 N3 O4' _chemical_formula_weight 441.47 _chemical_melting_point ? _chemical_oxdiff_formula C40H40O2N4 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_H-M_alt 'P 1 21/c 1' _space_group_name_Hall '-P 2ybc' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.0994(5) _cell_length_b 10.9354(3) _cell_length_c 16.3508(6) _cell_angle_alpha 90 _cell_angle_beta 115.198(4) _cell_angle_gamma 90 _cell_volume 2281.11(14) _cell_formula_units_Z 4 _cell_measurement_reflns_used 2870 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 70.3790 _cell_measurement_theta_min 5.0380 _shelx_estimated_absorpt_T_max 0.938 _shelx_estimated_absorpt_T_min 0.894 _exptl_absorpt_coefficient_mu 0.717 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.94327 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_special_details ? _exptl_crystal_colour yellow _exptl_crystal_colour_primary yellow _exptl_crystal_density_diffrn 1.285 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description prism _exptl_crystal_F_000 928 _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.09 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0227 _diffrn_reflns_av_unetI/netI 0.0288 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 8092 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_theta_full 67.066 _diffrn_reflns_theta_max 67.066 _diffrn_reflns_theta_min 5.029 _diffrn_ambient_temperature 293(2) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 16.2312 _diffrn_detector_type Eos _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames #-------------------------------------------------------------------------- 1 \w -52.00 35.00 1.00 2.10 -- -33.50 57.00 0.00 87 2 \w -4.00 77.00 1.00 2.10 -- 36.47 -99.00 150.00 81 3 \w 58.00 92.00 1.00 2.10 -- 36.47 178.00 -60.00 34 4 \w 66.00 96.00 1.00 2.10 -- 36.47 178.00-150.00 30 5 \w 76.00 110.00 1.00 2.10 -- 36.47 178.00 90.00 34 6 \w -1.00 77.00 1.00 2.10 -- 36.47 -99.00 -60.00 78 7 \w 9.00 38.00 1.00 2.10 -- 36.47 77.00 90.00 29 8 \w 63.00 104.00 1.00 2.10 -- 36.47 77.00 90.00 41 9 \w 47.00 73.00 1.00 14.50 -- 108.00 -30.00-150.00 26 10 \w 78.00 118.00 1.00 14.50 -- 108.00 -45.00 150.00 40 11 \w 46.00 103.00 1.00 14.50 -- 108.00 -94.00-180.00 57 12 \w 98.00 127.00 1.00 14.50 -- 108.00 -30.00-150.00 29 13 \w 113.00 172.00 1.00 14.50 -- 108.00 111.00 150.00 59 14 \w 96.00 173.00 1.00 14.50 -- 108.00 61.00 -60.00 77 15 \w 45.00 109.00 1.00 14.50 -- 108.00 -45.00 0.00 64 16 \w 63.00 178.00 1.00 14.50 -- 108.00 15.00-120.00 115 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'Xcalibur, Eos, Gemini' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 0.0864300000 _diffrn_orient_matrix_UB_12 -0.0927519000 _diffrn_orient_matrix_UB_13 0.0536231000 _diffrn_orient_matrix_UB_21 -0.0744726000 _diffrn_orient_matrix_UB_22 -0.0620072000 _diffrn_orient_matrix_UB_23 0.0341683000 _diffrn_orient_matrix_UB_31 -0.0395202000 _diffrn_orient_matrix_UB_32 -0.0860887000 _diffrn_orient_matrix_UB_33 -0.0824242000 _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_source 'fine-focus sealed X-ray tube' _diffrn_source_type 'Enhance (Cu) X-ray Source' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 3204 _reflns_number_total 4065 _reflns_odcompleteness_completeness 99.72 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 66.97 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement 'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)' _computing_data_collection 'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)' _computing_data_reduction 'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'ShelXS (Sheldrick, 2008)' _refine_diff_density_max 0.253 _refine_diff_density_min -0.198 _refine_diff_density_rms 0.040 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 317 _refine_ls_number_reflns 4065 _refine_ls_number_restraints 30 _refine_ls_R_factor_all 0.0575 _refine_ls_R_factor_gt 0.0445 _refine_ls_restrained_S_all 1.028 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0652P)^2^+0.2535P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1156 _refine_ls_wR_factor_ref 0.1275 _refine_special_details ? _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All C(H,H,H) groups 2. Restrained distances C24-N3A 1.45 with sigma of 0.02 O4A-N3A 1.4 with sigma of 0.02 N2A-C11 1.45 with sigma of 0.02 N2A-O2A 1.2 with sigma of 0.02 3. Rigid bond restraints N3, O4 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01 N2, O2 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01 4. Uiso/Uaniso restraints and constraints Uanis(N2) \\sim Ueq, Uanis(O2) \\sim Ueq, Uanis(N3) \\sim Ueq, Uanis(O4) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02 Uanis(O4) = Uanis(O4A) Uanis(N3) = Uanis(N3A) Uanis(O2) = Uanis(O2A) Uanis(O1) = Uanis(O1A) Uanis(N2) = Uanis(N2A) 5. Others Sof(O4A)=Sof(N3A)=1-FVAR(1) Sof(O4)=Sof(N3)=FVAR(1) Sof(O2A)=Sof(O1A)=Sof(N2A)=1-FVAR(2) Sof(O1)=Sof(O2)=Sof(N2)=FVAR(2) 6.a Ternary CH refined with riding coordinates: C8(H8), C9(H9), C10(H10) 6.b Secondary CH2 refined with riding coordinates: C7(H7A,H7B) 6.c Aromatic/amide H refined with riding coordinates: C1(H1), C2(H2), C3(H3), C4(H4), C12(H12), C15(H15), C16(H16), C17(H17), C18(H18), C19(H19), C20(H20), C21(H21) 6.d Idealised Me refined as rotating group: C25(H25A,H25B,H25C), C26(H26A,H26B,H26C) ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary ? loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group O1 O 0.03814(17) 0.5433(7) 0.65287(18) 0.0699(10) Uani 0.92(2) 1 d . . P A 1 O2 O 0.0891(2) 0.6671(4) 0.5752(3) 0.0639(7) Uani 0.92(2) 1 d . U P A 1 O3 O 0.37199(10) 0.34646(13) 0.47997(10) 0.0656(4) Uani 1 1 d . . . . . O4 O 0.5909(4) 0.8099(6) 0.6757(3) 0.0577(12) Uani 0.644(16) 1 d . U P B 1 N1 N 0.16516(12) 0.25297(14) 0.58593(10) 0.0534(4) Uani 1 1 d . . . . . N2 N 0.0863(3) 0.5620(3) 0.6046(3) 0.0518(7) Uani 0.92(2) 1 d . U P A 1 N3 N 0.6083(5) 0.7399(7) 0.7532(6) 0.0555(14) Uani 0.644(16) 1 d . U P B 1 C1 C 0.1393(2) -0.0586(2) 0.4986(2) 0.0860(8) Uani 1 1 d . . . . . H1 H 0.1131 -0.1124 0.5280 0.103 Uiso 1 1 calc R . . . . C2 C 0.1548(2) -0.0963(2) 0.4252(2) 0.0944(9) Uani 1 1 d . . . . . H2 H 0.1377 -0.1760 0.4042 0.113 Uiso 1 1 calc R . . . . C3 C 0.1953(2) -0.0176(2) 0.38189(19) 0.0884(8) Uani 1 1 d . . . . . H3 H 0.2043 -0.0447 0.3317 0.106 Uiso 1 1 calc R . . . . C4 C 0.22275(18) 0.1019(2) 0.41272(15) 0.0689(5) Uani 1 1 d . . . . . H4 H 0.2515 0.1545 0.3846 0.083 Uiso 1 1 calc R . . . . C5 C 0.20604(14) 0.14003(16) 0.48610(13) 0.0550(4) Uani 1 1 d . . . . . C6 C 0.16332(15) 0.06104(19) 0.52813(15) 0.0655(5) Uani 1 1 d . . . . . C7 C 0.15004(17) 0.12451(19) 0.60367(15) 0.0681(6) Uani 1 1 d . . . . . H7A H 0.0807 0.1109 0.6008 0.082 Uiso 1 1 calc R . . . . H7B H 0.2024 0.0981 0.6621 0.082 Uiso 1 1 calc R . . . . C8 C 0.22872(12) 0.26225(15) 0.53434(11) 0.0459(4) Uani 1 1 d . . . . . H8 H 0.3029 0.2644 0.5771 0.055 Uiso 1 1 calc R . . . . C9 C 0.20345(12) 0.37802(14) 0.47686(11) 0.0418(3) Uani 1 1 d . . . . . H9 H 0.1359 0.3681 0.4243 0.050 Uiso 1 1 calc R . . . . C10 C 0.19945(12) 0.49340(14) 0.53176(11) 0.0425(3) Uani 1 1 d . . . . . H10 H 0.1648 0.5594 0.4888 0.051 Uiso 1 1 calc R . . . . C11 C 0.13456(12) 0.46463(16) 0.58166(11) 0.0471(4) Uani 1 1 d D . . . . C12 C 0.12248(13) 0.34853(18) 0.60606(12) 0.0526(4) Uani 1 1 d . . . . . H12 H 0.0825 0.3364 0.6382 0.063 Uiso 1 1 calc R . . . . C13 C 0.28917(13) 0.40021(15) 0.44476(12) 0.0471(4) Uani 1 1 d . . . . . C14 C 0.27313(14) 0.49498(15) 0.37467(12) 0.0494(4) Uani 1 1 d . . . . . C15 C 0.17528(16) 0.54052(19) 0.31781(13) 0.0597(5) Uani 1 1 d . . . . . H15 H 0.1155 0.5108 0.3215 0.072 Uiso 1 1 calc R . . . . C16 C 0.1669(2) 0.6307(2) 0.25521(15) 0.0748(6) Uani 1 1 d . . . . . H16 H 0.1013 0.6610 0.2168 0.090 Uiso 1 1 calc R . . . . C17 C 0.2555(2) 0.6755(2) 0.24989(18) 0.0827(7) Uani 1 1 d . . . . . H17 H 0.2496 0.7364 0.2082 0.099 Uiso 1 1 calc R . . . . C18 C 0.3526(2) 0.6303(2) 0.3061(2) 0.0833(7) Uani 1 1 d . . . . . H18 H 0.4123 0.6604 0.3022 0.100 Uiso 1 1 calc R . . . . C19 C 0.36178(18) 0.54068(19) 0.36825(16) 0.0647(5) Uani 1 1 d . . . . . H19 H 0.4276 0.5105 0.4061 0.078 Uiso 1 1 calc R . . . . C20 C 0.30715(12) 0.53676(15) 0.59563(11) 0.0454(4) Uani 1 1 d . . . . . H20 H 0.3482 0.4859 0.6432 0.054 Uiso 1 1 calc R . . . . C21 C 0.34598(13) 0.64322(15) 0.58740(12) 0.0465(4) Uani 1 1 d . . . . . H21 H 0.3022 0.6927 0.5402 0.056 Uiso 1 1 calc R . . . . C22 C 0.52020(14) 0.66567(17) 0.73192(12) 0.0534(4) Uani 1 1 d . . . . . C23 C 0.44943(13) 0.69252(15) 0.64357(12) 0.0462(4) Uani 1 1 d . . . . . C24 C 0.50008(14) 0.78096(16) 0.61666(13) 0.0519(4) Uani 1 1 d D . . . . C25 C 0.51349(19) 0.5802(2) 0.79967(15) 0.0762(6) Uani 1 1 d . . . . . H25A H 0.5251 0.4981 0.7852 0.114 Uiso 1 1 calc GR . . . . H25B H 0.4452 0.5860 0.7990 0.114 Uiso 1 1 calc GR . . . . H25C H 0.5658 0.6013 0.8587 0.114 Uiso 1 1 calc GR . . . . C26 C 0.46731(17) 0.8468(2) 0.52998(16) 0.0682(5) Uani 1 1 d . . . . . H26A H 0.4119 0.9028 0.5228 0.102 Uiso 1 1 calc GR . . . . H26B H 0.4429 0.7892 0.4811 0.102 Uiso 1 1 calc GR . . . . H26C H 0.5259 0.8914 0.5297 0.102 Uiso 1 1 calc GR . . . . O4A O 0.6033(10) 0.7187(10) 0.7624(11) 0.0577(12) Uani 0.356(16) 1 d D . P B 2 N3A N 0.5982(8) 0.7984(16) 0.6957(10) 0.0555(14) Uani 0.356(16) 1 d D . P B 2 O2A O 0.098(3) 0.641(4) 0.597(4) 0.0639(7) Uani 0.08(2) 1 d D . P A 2 O1A O 0.034(2) 0.491(6) 0.660(2) 0.0699(10) Uani 0.08(2) 1 d . . P A 2 N2A N 0.071(3) 0.541(4) 0.612(3) 0.0518(7) Uani 0.08(2) 1 d D . P A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.0594(8) 0.096(3) 0.0624(9) 0.0035(13) 0.0335(7) 0.0104(12) O2 0.0638(10) 0.0512(15) 0.0732(18) -0.0068(11) 0.0258(11) 0.0004(10) O3 0.0545(7) 0.0670(9) 0.0800(9) 0.0201(7) 0.0332(7) 0.0154(6) O4 0.0640(16) 0.0553(17) 0.055(2) 0.0005(18) 0.0260(16) -0.0165(12) N1 0.0516(8) 0.0543(9) 0.0500(8) 0.0119(7) 0.0176(6) -0.0070(7) N2 0.0363(12) 0.0692(16) 0.0436(10) -0.0088(12) 0.0112(8) -0.0056(11) N3 0.0514(17) 0.061(3) 0.046(2) -0.002(2) 0.0128(13) -0.0232(16) C1 0.0766(14) 0.0509(12) 0.0999(19) 0.0092(13) 0.0081(13) -0.0139(10) C2 0.0858(17) 0.0516(13) 0.107(2) -0.0108(14) 0.0039(15) -0.0053(11) C3 0.0938(17) 0.0641(14) 0.0802(16) -0.0144(12) 0.0110(13) 0.0103(13) C4 0.0746(13) 0.0551(11) 0.0635(12) -0.0007(9) 0.0165(10) 0.0082(9) C5 0.0502(9) 0.0435(9) 0.0551(10) 0.0059(8) 0.0067(8) 0.0015(7) C6 0.0565(10) 0.0501(10) 0.0696(12) 0.0108(9) 0.0073(9) -0.0071(8) C7 0.0649(12) 0.0608(12) 0.0710(13) 0.0198(10) 0.0216(10) -0.0130(9) C8 0.0413(8) 0.0467(9) 0.0428(8) 0.0073(7) 0.0114(6) -0.0010(6) C9 0.0403(7) 0.0418(8) 0.0378(7) 0.0033(6) 0.0115(6) -0.0010(6) C10 0.0404(7) 0.0425(8) 0.0402(8) 0.0039(6) 0.0130(6) -0.0007(6) C11 0.0395(8) 0.0566(10) 0.0400(8) -0.0036(7) 0.0119(6) -0.0040(7) C12 0.0423(8) 0.0694(12) 0.0419(9) 0.0048(8) 0.0140(7) -0.0080(8) C13 0.0482(9) 0.0451(9) 0.0475(9) 0.0014(7) 0.0199(7) 0.0016(7) C14 0.0635(10) 0.0435(8) 0.0484(9) 0.0003(7) 0.0308(8) 0.0017(7) C15 0.0689(11) 0.0632(11) 0.0509(10) 0.0089(9) 0.0292(9) 0.0077(9) C16 0.0989(17) 0.0690(13) 0.0582(12) 0.0179(10) 0.0352(12) 0.0208(12) C17 0.126(2) 0.0638(13) 0.0779(15) 0.0203(12) 0.0627(16) 0.0058(13) C18 0.109(2) 0.0710(14) 0.0964(18) 0.0129(13) 0.0691(17) -0.0084(13) C19 0.0727(12) 0.0614(12) 0.0729(13) 0.0056(10) 0.0433(11) -0.0003(9) C20 0.0422(8) 0.0450(9) 0.0448(8) 0.0028(7) 0.0143(7) -0.0009(6) C21 0.0452(8) 0.0454(9) 0.0479(9) -0.0005(7) 0.0188(7) -0.0012(7) C22 0.0518(10) 0.0568(10) 0.0471(9) -0.0098(8) 0.0168(8) -0.0086(8) C23 0.0489(9) 0.0405(8) 0.0523(9) -0.0070(7) 0.0244(7) -0.0036(7) C24 0.0572(10) 0.0419(9) 0.0627(11) -0.0068(8) 0.0315(9) -0.0068(7) C25 0.0776(14) 0.0869(16) 0.0551(11) 0.0066(11) 0.0195(10) -0.0179(12) C26 0.0737(13) 0.0546(11) 0.0805(14) 0.0112(10) 0.0368(11) -0.0040(9) O4A 0.0640(16) 0.0553(17) 0.055(2) 0.0005(18) 0.0260(16) -0.0165(12) N3A 0.0514(17) 0.061(3) 0.046(2) -0.002(2) 0.0128(13) -0.0232(16) O2A 0.0638(10) 0.0512(15) 0.0732(18) -0.0068(11) 0.0258(11) 0.0004(10) O1A 0.0594(8) 0.096(3) 0.0624(9) 0.0035(13) 0.0335(7) 0.0104(12) N2A 0.0363(12) 0.0692(16) 0.0436(10) -0.0088(12) 0.0112(8) -0.0056(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1 N2 1.257(3) . ? O2 N2 1.253(3) . ? O3 C13 1.212(2) . ? O4 N3 1.410(5) . ? O4 C24 1.272(6) . ? N1 C7 1.468(2) . ? N1 C8 1.473(2) . ? N1 C12 1.316(3) . ? N2 C11 1.399(3) . ? N3 C22 1.398(6) . ? C1 H1 0.9300 . ? C1 C2 1.372(4) . ? C1 C6 1.386(3) . ? C2 H2 0.9300 . ? C2 C3 1.382(4) . ? C3 H3 0.9300 . ? C3 C4 1.395(3) . ? C4 H4 0.9300 . ? C4 C5 1.382(3) . ? C5 C6 1.391(3) . ? C5 C8 1.515(2) . ? C6 C7 1.497(3) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 H8 0.9800 . ? C8 C9 1.526(2) . ? C9 H9 0.9800 . ? C9 C10 1.563(2) . ? C9 C13 1.528(2) . ? C10 H10 0.9800 . ? C10 C11 1.496(2) . ? C10 C20 1.507(2) . ? C11 C12 1.363(3) . ? C11 N2A 1.46(2) . ? C12 H12 0.9300 . ? C13 C14 1.489(2) . ? C14 C15 1.387(3) . ? C14 C19 1.391(3) . ? C15 H15 0.9300 . ? C15 C16 1.390(3) . ? C16 H16 0.9300 . ? C16 C17 1.378(4) . ? C17 H17 0.9300 . ? C17 C18 1.376(4) . ? C18 H18 0.9300 . ? C18 C19 1.378(3) . ? C19 H19 0.9300 . ? C20 H20 0.9300 . ? C20 C21 1.318(2) . ? C21 H21 0.9300 . ? C21 C23 1.456(2) . ? C22 C23 1.393(3) . ? C22 C25 1.483(3) . ? C22 O4A 1.209(11) . ? C23 C24 1.381(2) . ? C24 C26 1.478(3) . ? C24 N3A 1.448(9) . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? O4A N3A 1.374(10) . ? O2A N2A 1.21(2) . ? O1A N2A 1.23(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C24 O4 N3 106.3(5) . . ? C7 N1 C8 110.74(16) . . ? C12 N1 C7 126.16(16) . . ? C12 N1 C8 122.91(15) . . ? O1 N2 C11 119.9(2) . . ? O2 N2 O1 120.3(4) . . ? O2 N2 C11 119.7(4) . . ? C22 N3 O4 107.2(6) . . ? C2 C1 H1 120.6 . . ? C2 C1 C6 118.8(3) . . ? C6 C1 H1 120.6 . . ? C1 C2 H2 119.5 . . ? C1 C2 C3 121.0(2) . . ? C3 C2 H2 119.5 . . ? C2 C3 H3 119.7 . . ? C2 C3 C4 120.6(3) . . ? C4 C3 H3 119.7 . . ? C3 C4 H4 120.9 . . ? C5 C4 C3 118.2(2) . . ? C5 C4 H4 120.9 . . ? C4 C5 C6 120.77(19) . . ? C4 C5 C8 129.93(18) . . ? C6 C5 C8 109.30(18) . . ? C1 C6 C5 120.5(2) . . ? C1 C6 C7 128.9(2) . . ? C5 C6 C7 110.64(18) . . ? N1 C7 C6 101.59(16) . . ? N1 C7 H7A 111.5 . . ? N1 C7 H7B 111.5 . . ? C6 C7 H7A 111.5 . . ? C6 C7 H7B 111.5 . . ? H7A C7 H7B 109.3 . . ? N1 C8 C5 101.09(14) . . ? N1 C8 H8 108.5 . . ? N1 C8 C9 111.75(14) . . ? C5 C8 H8 108.5 . . ? C5 C8 C9 117.97(14) . . ? C9 C8 H8 108.5 . . ? C8 C9 H9 109.4 . . ? C8 C9 C10 111.83(13) . . ? C8 C9 C13 109.38(13) . . ? C10 C9 H9 109.4 . . ? C13 C9 H9 109.4 . . ? C13 C9 C10 107.23(13) . . ? C9 C10 H10 108.2 . . ? C11 C10 C9 108.87(13) . . ? C11 C10 H10 108.2 . . ? C11 C10 C20 110.98(13) . . ? C20 C10 C9 112.32(13) . . ? C20 C10 H10 108.2 . . ? N2 C11 C10 117.9(3) . . ? C12 C11 N2 119.6(3) . . ? C12 C11 C10 122.50(16) . . ? C12 C11 N2A 105(2) . . ? N2A C11 C10 132(2) . . ? N1 C12 C11 122.61(16) . . ? N1 C12 H12 118.7 . . ? C11 C12 H12 118.7 . . ? O3 C13 C9 120.19(15) . . ? O3 C13 C14 120.21(16) . . ? C14 C13 C9 119.44(14) . . ? C15 C14 C13 123.20(16) . . ? C15 C14 C19 119.32(18) . . ? C19 C14 C13 117.46(17) . . ? C14 C15 H15 120.1 . . ? C14 C15 C16 119.8(2) . . ? C16 C15 H15 120.1 . . ? C15 C16 H16 119.9 . . ? C17 C16 C15 120.2(2) . . ? C17 C16 H16 119.9 . . ? C16 C17 H17 120.0 . . ? C18 C17 C16 120.1(2) . . ? C18 C17 H17 120.0 . . ? C17 C18 H18 119.9 . . ? C17 C18 C19 120.2(2) . . ? C19 C18 H18 119.9 . . ? C14 C19 H19 119.8 . . ? C18 C19 C14 120.4(2) . . ? C18 C19 H19 119.8 . . ? C10 C20 H20 118.4 . . ? C21 C20 C10 123.18(15) . . ? C21 C20 H20 118.4 . . ? C20 C21 H21 116.2 . . ? C20 C21 C23 127.65(16) . . ? C23 C21 H21 116.2 . . ? N3 C22 C25 120.8(4) . . ? C23 C22 N3 107.7(4) . . ? C23 C22 C25 131.46(17) . . ? O4A C22 C23 117.9(8) . . ? O4A C22 C25 110.7(8) . . ? C22 C23 C21 131.20(16) . . ? C24 C23 C21 124.99(17) . . ? C24 C23 C22 103.81(16) . . ? O4 C24 C23 115.0(4) . . ? O4 C24 C26 114.1(3) . . ? C23 C24 C26 130.85(18) . . ? C23 C24 N3A 103.6(8) . . ? N3A C24 C26 125.6(9) . . ? C22 C25 H25A 109.5 . . ? C22 C25 H25B 109.5 . . ? C22 C25 H25C 109.5 . . ? H25A C25 H25B 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26B 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C22 O4A N3A 105.2(13) . . ? O4A N3A C24 109.4(13) . . ? O2A N2A C11 99(3) . . ? O2A N2A O1A 141(4) . . ? O1A N2A C11 117(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 N2 C11 C10 -174.2(2) . . . . ? O1 N2 C11 C12 4.9(4) . . . . ? O2 N2 C11 C10 7.5(5) . . . . ? O2 N2 C11 C12 -173.4(3) . . . . ? O3 C13 C14 C15 165.34(19) . . . . ? O3 C13 C14 C19 -16.0(3) . . . . ? O4 N3 C22 C23 -1.4(4) . . . . ? O4 N3 C22 C25 -179.9(3) . . . . ? N1 C8 C9 C10 46.75(18) . . . . ? N1 C8 C9 C13 165.40(13) . . . . ? N2 C11 C12 N1 179.5(2) . . . . ? N3 O4 C24 C23 -1.5(4) . . . . ? N3 O4 C24 C26 179.4(3) . . . . ? N3 C22 C23 C21 -180.0(4) . . . . ? N3 C22 C23 C24 0.6(4) . . . . ? C1 C2 C3 C4 0.8(4) . . . . ? C1 C6 C7 N1 -166.9(2) . . . . ? C2 C1 C6 C5 -2.4(3) . . . . ? C2 C1 C6 C7 177.7(2) . . . . ? C2 C3 C4 C5 -1.5(4) . . . . ? C3 C4 C5 C6 0.2(3) . . . . ? C3 C4 C5 C8 179.35(19) . . . . ? C4 C5 C6 C1 1.7(3) . . . . ? C4 C5 C6 C7 -178.31(18) . . . . ? C4 C5 C8 N1 164.00(19) . . . . ? C4 C5 C8 C9 41.9(3) . . . . ? C5 C6 C7 N1 13.1(2) . . . . ? C5 C8 C9 C10 163.27(15) . . . . ? C5 C8 C9 C13 -78.09(18) . . . . ? C6 C1 C2 C3 1.1(4) . . . . ? C6 C5 C8 N1 -16.78(18) . . . . ? C6 C5 C8 C9 -138.90(16) . . . . ? C7 N1 C8 C5 25.92(18) . . . . ? C7 N1 C8 C9 152.28(15) . . . . ? C7 N1 C12 C11 -175.27(17) . . . . ? C8 N1 C7 C6 -24.67(19) . . . . ? C8 N1 C12 C11 -0.8(3) . . . . ? C8 C5 C6 C1 -177.57(18) . . . . ? C8 C5 C6 C7 2.4(2) . . . . ? C8 C9 C10 C11 -47.43(17) . . . . ? C8 C9 C10 C20 75.90(17) . . . . ? C8 C9 C13 O3 -15.1(2) . . . . ? C8 C9 C13 C14 169.40(14) . . . . ? C9 C10 C11 N2 -155.0(2) . . . . ? C9 C10 C11 C12 25.9(2) . . . . ? C9 C10 C11 N2A -152(3) . . . . ? C9 C10 C20 C21 115.10(18) . . . . ? C9 C13 C14 C15 -19.1(3) . . . . ? C9 C13 C14 C19 159.51(17) . . . . ? C10 C9 C13 O3 106.37(19) . . . . ? C10 C9 C13 C14 -69.14(18) . . . . ? C10 C11 C12 N1 -1.4(3) . . . . ? C10 C11 N2A O2A -10(6) . . . . ? C10 C11 N2A O1A -173(2) . . . . ? C10 C20 C21 C23 -178.30(16) . . . . ? C11 C10 C20 C21 -122.76(18) . . . . ? C12 N1 C7 C6 150.39(18) . . . . ? C12 N1 C8 C5 -149.33(16) . . . . ? C12 N1 C8 C9 -23.0(2) . . . . ? C12 C11 N2A O2A 172(4) . . . . ? C12 C11 N2A O1A 9(4) . . . . ? C13 C9 C10 C11 -167.34(13) . . . . ? C13 C9 C10 C20 -44.01(17) . . . . ? C13 C14 C15 C16 178.75(18) . . . . ? C13 C14 C19 C18 -178.7(2) . . . . ? C14 C15 C16 C17 -0.4(3) . . . . ? C15 C14 C19 C18 0.1(3) . . . . ? C15 C16 C17 C18 0.5(4) . . . . ? C16 C17 C18 C19 -0.4(4) . . . . ? C17 C18 C19 C14 0.1(4) . . . . ? C19 C14 C15 C16 0.1(3) . . . . ? C20 C10 C11 N2 80.9(2) . . . . ? C20 C10 C11 C12 -98.21(18) . . . . ? C20 C10 C11 N2A 84(3) . . . . ? C20 C21 C23 C22 -22.8(3) . . . . ? C20 C21 C23 C24 156.53(18) . . . . ? C21 C23 C24 O4 -178.9(3) . . . . ? C21 C23 C24 C26 0.0(3) . . . . ? C21 C23 C24 N3A 179.7(6) . . . . ? C22 C23 C24 O4 0.6(3) . . . . ? C22 C23 C24 C26 179.5(2) . . . . ? C22 C23 C24 N3A -0.9(6) . . . . ? C22 O4A N3A C24 -3.1(10) . . . . ? C23 C22 O4A N3A 2.7(9) . . . . ? C23 C24 N3A O4A 2.4(9) . . . . ? C24 O4 N3 C22 1.8(4) . . . . ? C25 C22 C23 C21 -1.7(4) . . . . ? C25 C22 C23 C24 178.8(2) . . . . ? C25 C22 O4A N3A -177.3(6) . . . . ? C26 C24 N3A O4A -177.9(5) . . . . ? O4A C22 C23 C21 178.2(7) . . . . ? O4A C22 C23 C24 -1.2(7) . . . . ? N2A C11 C12 N1 177(2) . . . . ? _shelx_res_file ; wll148.res created by SHELXL-2014/7 TITL WLL148 in P21/c #14 REM reset to P21/c #14 CELL 1.54184 14.099395 10.935373 16.350793 90 115.1975 90 ZERR 4 0.000454 0.000274 0.000562 0 0.004 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H N O UNIT 104 92 12 16 DFIX 1.45 C24 N3A DFIX 1.4 O4A N3A DFIX 1.45 N2A C11 DFIX 1.2 N2A O2A DELU N3 O4 DELU N2 O2 ISOR 0.01 0.02 N2 O2 N3 O4 EADP O4 O4A EADP N3 N3A EADP O2 O2A EADP O1 O1A EADP N2 N2A L.S. 4 0 0 PLAN 20 SIZE 0.09 0.1 0.16 MPLA C1 C2 C3 C4 C5 C6 MPLA C8 C10 C11 C12 N1 MPLA C8 C9 C10 MPLA C14 C15 C16 C17 C18 C19 MPLA C22 C23 C24 O4 N3 bond $h conf fmap 2 acta REM REM REM WGHT 0.065200 0.253500 FVAR 5.34776 0.64437 0.92146 PART 1 O1 4 0.038139 0.543267 0.652866 31.00000 0.05935 0.09567 = 0.06244 0.00350 0.03350 0.01040 O2 4 0.089115 0.667072 0.575161 31.00000 0.06380 0.05116 = 0.07316 -0.00678 0.02582 0.00040 PART 0 O3 4 0.371993 0.346462 0.479974 11.00000 0.05449 0.06698 = 0.07999 0.02009 0.03319 0.01542 PART 1 O4 4 0.590928 0.809853 0.675683 21.00000 0.06396 0.05525 = 0.05469 0.00046 0.02599 -0.01649 PART 0 N1 3 0.165162 0.252969 0.585929 11.00000 0.05162 0.05426 = 0.05001 0.01185 0.01760 -0.00703 PART 1 N2 3 0.086261 0.561991 0.604635 31.00000 0.03633 0.06921 = 0.04363 -0.00876 0.01115 -0.00556 N3 3 0.608296 0.739864 0.753230 21.00000 0.05137 0.06101 = 0.04581 -0.00189 0.01280 -0.02316 PART 0 C1 1 0.139269 -0.058619 0.498582 11.00000 0.07656 0.05089 = 0.09989 0.00924 0.00809 -0.01386 AFIX 43 H1 2 0.113096 -0.112412 0.528008 11.00000 -1.20000 AFIX 0 C2 1 0.154760 -0.096285 0.425163 11.00000 0.08580 0.05165 = 0.10699 -0.01084 0.00389 -0.00533 AFIX 43 H2 2 0.137738 -0.175987 0.404171 11.00000 -1.20000 AFIX 0 C3 1 0.195280 -0.017626 0.381888 11.00000 0.09381 0.06410 = 0.08018 -0.01441 0.01102 0.01028 AFIX 43 H3 2 0.204316 -0.044652 0.331739 11.00000 -1.20000 AFIX 0 C4 1 0.222749 0.101911 0.412718 11.00000 0.07456 0.05515 = 0.06348 -0.00068 0.01653 0.00820 AFIX 43 H4 2 0.251525 0.154517 0.384641 11.00000 -1.20000 AFIX 0 C5 1 0.206042 0.140026 0.486099 11.00000 0.05017 0.04353 = 0.05509 0.00594 0.00671 0.00150 C6 1 0.163321 0.061039 0.528127 11.00000 0.05650 0.05006 = 0.06956 0.01080 0.00734 -0.00712 C7 1 0.150039 0.124511 0.603674 11.00000 0.06487 0.06081 = 0.07103 0.01978 0.02157 -0.01302 AFIX 23 H7A 2 0.080690 0.110855 0.600755 11.00000 -1.20000 H7B 2 0.202361 0.098139 0.662146 11.00000 -1.20000 AFIX 0 C8 1 0.228722 0.262245 0.534343 11.00000 0.04134 0.04673 = 0.04277 0.00725 0.01144 -0.00103 AFIX 13 H8 2 0.302887 0.264439 0.577111 11.00000 -1.20000 AFIX 0 C9 1 0.203452 0.378020 0.476858 11.00000 0.04025 0.04183 = 0.03783 0.00330 0.01145 -0.00104 AFIX 13 H9 2 0.135861 0.368114 0.424347 11.00000 -1.20000 AFIX 0 C10 1 0.199449 0.493396 0.531764 11.00000 0.04037 0.04253 = 0.04025 0.00388 0.01303 -0.00071 AFIX 13 H10 2 0.164845 0.559422 0.488838 11.00000 -1.20000 AFIX 0 C11 1 0.134560 0.464627 0.581661 11.00000 0.03954 0.05662 = 0.04003 -0.00363 0.01192 -0.00396 C12 1 0.122476 0.348530 0.606063 11.00000 0.04228 0.06940 = 0.04194 0.00483 0.01399 -0.00799 AFIX 43 H12 2 0.082469 0.336377 0.638223 11.00000 -1.20000 AFIX 0 C13 1 0.289172 0.400207 0.444759 11.00000 0.04815 0.04514 = 0.04747 0.00143 0.01991 0.00160 C14 1 0.273128 0.494984 0.374672 11.00000 0.06353 0.04346 = 0.04841 0.00028 0.03077 0.00174 C15 1 0.175282 0.540522 0.317807 11.00000 0.06890 0.06316 = 0.05087 0.00885 0.02917 0.00768 AFIX 43 H15 2 0.115455 0.510788 0.321546 11.00000 -1.20000 AFIX 0 C16 1 0.166918 0.630747 0.255205 11.00000 0.09891 0.06901 = 0.05823 0.01791 0.03519 0.02077 AFIX 43 H16 2 0.101317 0.660996 0.216773 11.00000 -1.20000 AFIX 0 C17 1 0.255508 0.675545 0.249886 11.00000 0.12639 0.06379 = 0.07790 0.02033 0.06274 0.00576 AFIX 43 H17 2 0.249617 0.736386 0.208249 11.00000 -1.20000 AFIX 0 C18 1 0.352642 0.630337 0.306118 11.00000 0.10881 0.07097 = 0.09638 0.01289 0.06905 -0.00840 AFIX 43 H18 2 0.412270 0.660367 0.302180 11.00000 -1.20000 AFIX 0 C19 1 0.361777 0.540684 0.368246 11.00000 0.07273 0.06137 = 0.07288 0.00555 0.04326 -0.00034 AFIX 43 H19 2 0.427635 0.510529 0.406129 11.00000 -1.20000 AFIX 0 C20 1 0.307153 0.536762 0.595632 11.00000 0.04215 0.04496 = 0.04475 0.00278 0.01429 -0.00094 AFIX 43 H20 2 0.348195 0.485916 0.643152 11.00000 -1.20000 AFIX 0 C21 1 0.345982 0.643225 0.587403 11.00000 0.04517 0.04542 = 0.04787 -0.00048 0.01883 -0.00119 AFIX 43 H21 2 0.302168 0.692720 0.540163 11.00000 -1.20000 AFIX 0 C22 1 0.520201 0.665670 0.731921 11.00000 0.05180 0.05677 = 0.04715 -0.00984 0.01677 -0.00857 C23 1 0.449426 0.692520 0.643568 11.00000 0.04890 0.04045 = 0.05235 -0.00703 0.02441 -0.00364 C24 1 0.500085 0.780961 0.616664 11.00000 0.05724 0.04193 = 0.06268 -0.00676 0.03149 -0.00684 C25 1 0.513488 0.580218 0.799670 11.00000 0.07761 0.08690 = 0.05508 0.00657 0.01945 -0.01795 AFIX 137 H25A 2 0.525058 0.498123 0.785179 11.00000 -1.50000 H25B 2 0.445237 0.585952 0.799040 11.00000 -1.50000 H25C 2 0.565822 0.601252 0.858656 11.00000 -1.50000 AFIX 0 C26 1 0.467306 0.846850 0.529977 11.00000 0.07371 0.05461 = 0.08053 0.01116 0.03681 -0.00399 AFIX 137 H26A 2 0.411869 0.902823 0.522846 11.00000 -1.50000 H26B 2 0.442904 0.789156 0.481071 11.00000 -1.50000 H26C 2 0.525852 0.891371 0.529702 11.00000 -1.50000 AFIX 0 PART 2 O4A 4 0.603304 0.718726 0.762442 -21.00000 0.06396 0.05525 = 0.05469 0.00046 0.02599 -0.01649 N3A 3 0.598193 0.798352 0.695685 -21.00000 0.05137 0.06101 = 0.04581 -0.00189 0.01280 -0.02316 O2A 4 0.097850 0.640576 0.597370 -31.00000 0.06380 0.05116 = 0.07316 -0.00678 0.02582 0.00040 O1A 4 0.034265 0.491318 0.659622 -31.00000 0.05935 0.09567 = 0.06244 0.00350 0.03350 0.01040 N2A 3 0.070797 0.540814 0.612058 -31.00000 0.03633 0.06921 = 0.04363 -0.00876 0.01115 -0.00556 HKLF 4 REM WLL148 in P21/c #14 REM R1 = 0.0445 for 3204 Fo > 4sig(Fo) and 0.0575 for all 4065 data REM 317 parameters refined using 30 restraints END WGHT 0.0652 0.2535 REM Highest difference peak 0.253, deepest hole -0.198, 1-sigma level 0.040 Q1 1 -0.0411 0.7666 0.2413 11.00000 0.05 0.25 Q2 1 0.3835 0.8407 0.4854 11.00000 0.05 0.16 Q3 1 0.5968 0.5430 0.8378 11.00000 0.05 0.15 Q4 1 0.2079 0.3156 0.5029 11.00000 0.05 0.13 Q5 1 0.2002 0.4388 0.5049 11.00000 0.05 0.12 Q6 1 0.5185 0.8217 0.4991 11.00000 0.05 0.12 Q7 1 0.2290 0.3820 0.4499 11.00000 0.05 0.12 Q8 1 0.2728 0.4410 0.3995 11.00000 0.05 0.12 Q9 1 0.2579 0.5274 0.5603 11.00000 0.05 0.12 Q10 1 0.5015 0.6556 0.8499 11.00000 0.05 0.12 Q11 1 0.4903 0.6377 0.6742 11.00000 0.05 0.12 Q12 1 0.3135 0.6071 0.6217 11.00000 0.05 0.11 Q13 1 -0.0133 0.6114 0.6479 11.00000 0.05 0.11 Q14 1 0.1532 0.1119 0.4862 11.00000 0.05 0.11 Q15 1 0.3694 0.4590 0.6172 11.00000 0.05 0.11 Q16 1 0.7096 0.9093 0.7682 11.00000 0.05 0.11 Q17 1 0.6678 0.6847 0.7689 11.00000 0.05 0.11 Q18 1 0.1169 0.4765 0.2971 11.00000 0.05 0.11 Q19 1 0.4282 0.6459 0.2102 11.00000 0.05 0.11 Q20 1 0.3459 0.5595 0.5714 11.00000 0.05 0.11 ; _shelx_res_checksum 44121 _shelx_hkl_file ; 0 0 -2 352473. 1792.04 6 0 0 -3 171.136 65.4328 6 0 0 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5582.30 287.198 14 3 -5 9 5357.58 293.638 16 -3 -5 -9 5081.42 268.912 11 -3 -5 -10 249.912 70.5716 11 3 -5 10 221.198 81.7952 16 3 -5 11 83.8313 58.5174 16 -3 -5 -11 172.112 64.0535 11 3 -5 12 81.3208 54.4914 16 -3 -5 -12 45.3286 56.8332 11 -3 -5 -13-18.8416 55.2099 11 3 -5 13 103.939 49.5637 16 -3 -5 -14 219.758 52.5280 11 -3 -6 15-58.6453 49.7346 16 3 -6 -15 185.622 80.6741 11 -3 -6 14 83.8611 61.7745 16 3 -6 -14 266.877 91.2809 11 -3 -6 13 1798.30 171.365 16 3 -6 -13 1986.15 175.808 11 -3 -6 12 191.451 78.3741 16 3 -6 -12 260.929 92.4348 11 -3 -6 11 1405.43 151.586 16 3 -6 -11 1399.49 153.481 11 3 -6 -10 9395.33 371.470 13 3 -6 -10 8877.72 349.617 11 -3 -6 10 8431.51 358.960 16 3 -6 -9 8107.31 338.753 13 3 -6 -9 7614.27 315.159 11 -3 -6 9 7275.87 326.322 16 3 -6 -8 2164.56 438.789 5 3 -6 -8 1441.76 345.049 6 3 -6 -7 5332.79 652.172 6 3 -6 -7 6442.46 731.208 5 3 -6 -6 5782.39 631.098 1 3 -6 -6 5868.86 671.975 5 3 -6 -6 5743.95 668.486 6 3 -6 -5 3306.85 468.889 1 3 -6 -5 3929.72 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43.5401 32.2732 14 -12 -7 13 1467.71 119.972 16 -12 -7 12 22.0205 43.0142 16 -12 -7 11 16.1483 45.3225 16 12 -7 -11 52.6524 42.3958 12 -12 -7 10-40.2398 62.0283 16 12 -7 -10 28.9227 42.9826 12 -12 -7 9 829.853 106.318 16 12 -7 -9 979.738 121.760 12 -12 -7 8 1540.85 133.387 15 12 -7 -8 1390.12 147.198 12 -12 -7 8 1516.00 142.931 16 -12 -7 7 6.38480 46.6185 16 -12 -7 7-1.40883 46.2678 15 12 -7 -7-14.6249 59.3251 12 -12 -7 6 78.5190 47.1823 16 -12 -7 6 56.2299 48.2544 15 12 -7 -6 145.941 68.3664 12 -12 -7 5 219.290 65.5291 15 12 -7 -5 247.723 84.5515 12 -12 -7 4 3969.29 225.386 15 12 -7 -4 4078.33 241.408 12 -12 -7 3 207.149 68.1828 15 12 -7 -3 308.488 84.0643 12 -12 -7 2 3647.21 211.412 15 12 -7 -2 3991.03 228.195 12 12 -7 -1 254.815 70.5755 16 -12 -7 1 197.565 65.6681 15 12 -7 -1 218.625 75.4121 12 12 -7 0 61.6253 52.8645 16 -12 -7 0 74.9645 51.9419 15 12 -7 1-29.0520 45.5244 16 -12 -7 -1 45.8625 40.0849 15 12 -7 2 138.403 46.7489 16 -12 -8 11 31.5725 40.9767 16 -12 -8 10 614.367 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56.4762 57.2165 9 13 0 -10 1852.72 166.029 9 13 0 -9 1.06738 45.5242 9 13 0 -8-87.5140 56.3082 9 13 0 -7-28.5727 39.3161 9 -13 0 7 26.3055 59.6497 14 -13 0 6 1639.74 159.685 14 -13 0 5-2.71602 51.2247 14 -13 0 4 13748.1 452.813 14 -13 0 3 58.8149 69.2246 14 -13 0 2 3175.62 220.567 14 -13 0 1 19.9645 53.7664 14 -13 0 0 451.905 87.7714 14 -13 0 -1 36.5992 53.4137 14 -13 0 -2 62.1581 52.7907 14 -13 0 -3 24.6080 43.4466 14 -13 0 -4 761.383 84.4556 14 13 -1 -17 223.769 50.0840 9 13 1 -17 310.996 61.0562 9 13 -1 -16 209.593 62.5605 9 13 1 -16 114.046 53.8558 9 13 -1 -15 8.70264 46.0636 9 13 1 -15 31.6647 47.9050 9 13 -1 -14 16.2571 58.1846 9 13 1 -14-97.1661 61.8074 9 13 -1 -13 635.056 110.712 9 13 1 -13 509.653 94.1593 9 13 -1 -12 144.293 66.5782 9 13 1 -12-50.9064 56.8128 9 13 -1 -11 1387.94 149.230 9 13 1 -11 1332.69 140.139 9 13 -1 -10 442.828 93.9419 9 13 1 -10 455.786 86.7395 9 13 1 -9 1253.20 138.475 9 13 -1 -9 1102.83 132.931 9 13 -1 -8 18.0625 47.0811 9 13 1 -8 21.2181 38.4309 9 -13 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52.3860 48.4435 9 13 3 -11 1274.44 130.374 9 -13 -3 11 1418.49 144.998 16 -13 -3 10 206.939 68.7922 16 13 3 -10 288.952 73.3691 9 -13 3 9 8176.64 348.626 14 -13 -3 9 8145.20 340.124 16 -13 -3 8 879.119 118.766 16 -13 3 8 863.330 124.377 14 -13 -3 7 17429.7 482.196 15 -13 3 7 15742.2 487.959 14 -13 -3 7 16143.4 485.097 16 -13 -3 6 1330.04 142.095 15 -13 3 6 1208.76 143.179 14 -13 -3 5 5258.09 278.686 15 -13 3 5 5102.09 278.700 14 -13 -3 4 1116.02 134.357 15 -13 3 4 965.000 131.451 14 -13 -3 3 1255.52 142.182 15 -13 3 3 1023.15 133.117 14 13 -3 -3 782.564 109.765 12 -13 -3 2-31.6798 63.9066 15 13 -3 -2 27.5019 42.7386 12 -13 3 1 53.6398 59.5395 14 -13 3 0 4449.69 255.398 14 -13 3 -1 71.5478 66.7271 14 -13 3 -2 1500.21 142.119 14 -13 3 -3 350.112 75.4627 14 13 -3 4 28.7688 38.8687 16 -13 3 -4 41.2393 36.6902 14 13 4 -16 1220.84 101.008 9 -13 -4 15 120.342 44.4132 16 13 4 -15 133.075 48.4973 9 -13 -4 14 78.8713 45.7009 16 13 4 -14 56.6378 39.4656 9 -13 -4 13 25.2434 47.8859 16 13 4 -13 40.8743 45.2048 9 -13 -4 12 89.8952 60.7513 16 13 4 -12 99.5105 50.9383 9 -13 -4 11 1172.24 130.691 16 13 4 -11 1288.15 126.200 9 -13 -4 10 893.186 120.161 16 -13 4 10 1016.30 123.759 14 -13 -4 9 1244.96 139.230 16 -13 4 9 1140.14 138.138 14 -13 4 8 5992.33 296.638 14 -13 -4 8 6422.85 302.441 16 -13 -4 7 77.2442 52.9762 15 -13 4 7-29.4333 54.4564 14 -13 -4 6 7270.84 316.374 15 -13 4 6 7185.36 322.693 14 -13 -4 5 404.431 85.4515 15 -13 4 5 245.023 72.4235 14 -13 -4 4 214.322 72.4472 15 -13 4 4 103.085 59.2588 14 13 -4 -4 225.179 75.1162 12 -13 -4 3 590.115 105.868 15 -13 4 3 428.514 94.6133 14 13 -4 -3 227.282 71.8358 12 -13 -4 2 230.541 80.6774 15 -13 4 2 386.043 84.3739 14 13 -4 -2 327.034 78.3608 12 -13 -4 1 1730.41 157.401 15 -13 4 1 2182.34 178.433 14 13 -4 -1 1861.52 150.920 12 -13 4 0-65.8641 64.0755 14 -13 4 -1 200.906 64.3536 14 -13 4 -2 20.6721 47.0302 14 13 -4 3 459.076 72.2780 16 -13 4 -3 585.405 81.4236 14 -13 -5 15 59.7713 37.3163 16 13 5 -15 70.7269 31.8817 9 -13 5 15 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332.073 75.7206 12 -13 5 0 2347.17 167.114 14 13 -5 0 2219.08 150.402 12 -13 5 -1 1009.83 103.994 14 13 -5 2 1181.90 109.204 16 -13 5 -2 1210.19 105.966 14 -13 -6 14 925.530 89.9139 16 -13 -6 13 789.903 90.8453 16 -13 -6 12-16.6275 41.9461 16 -13 -6 11 1962.25 151.426 16 -13 -6 10-10.9043 52.1738 16 -13 -6 9 59.4748 51.0830 16 -13 6 9 38.9135 35.8723 14 -13 -6 8 568.852 96.6748 16 -13 -6 8 567.751 78.7231 15 -13 6 8 581.122 87.3166 14 -13 -6 7 33.7386 53.2420 16 -13 -6 7-12.2661 50.9082 15 -13 6 7 73.3574 42.6266 14 13 -6 -7-17.4757 70.6198 12 -13 -6 6 156.479 59.2457 15 -13 6 6 339.661 75.1064 14 13 -6 -6 186.599 76.6804 12 -13 -6 5 1.16785 49.2680 15 -13 6 5 46.9160 40.5037 14 13 -6 -5-39.8419 68.0234 12 -13 -6 4-68.7359 55.8125 15 -13 6 4 49.2293 42.6562 14 13 -6 -4 20.6562 53.3807 12 -13 -6 3 346.212 79.7442 15 -13 6 3 307.839 67.0462 14 13 -6 -3 366.135 79.5541 12 -13 -6 2 2459.87 171.983 15 -13 6 2 2520.97 166.733 14 13 -6 -2 2535.55 174.597 12 -13 -6 1 24.6811 44.8092 15 -13 6 1 21.3964 40.8515 14 13 -6 -1-23.0825 46.3249 12 13 -6 0 3522.83 182.427 16 -13 6 0 3214.81 171.074 14 13 -6 1 1172.39 104.075 16 -13 6 -1 1032.37 92.8536 14 -13 -7 12-97.0104 48.5804 16 13 -7 -12-74.4793 37.7669 12 -13 -7 11 47.3336 45.0409 16 13 -7 -11-53.1822 38.2480 12 -13 -7 10 102.252 51.4360 16 13 -7 -10 122.854 48.2056 12 -13 -7 9 526.645 81.8925 16 13 -7 -9 625.283 87.5044 12 -13 -7 8 11.8453 39.9333 16 -13 -7 8 40.7264 34.4060 15 13 -7 -8 127.630 51.8166 12 -13 -7 7 146.577 52.9463 15 13 -7 -7 61.4617 50.2080 12 -13 -7 6 1040.45 111.008 15 13 -7 -6 1169.72 124.696 12 -13 -7 5 1494.14 129.659 15 13 -7 -5 1527.50 139.791 12 -13 -7 4 3144.77 184.808 15 13 -7 -4 3008.77 186.705 12 -13 -7 3 532.631 80.9210 15 13 -7 -3 527.696 85.9604 12 -13 -7 2 1021.65 104.226 15 13 -7 -2 900.457 99.4630 12 13 -7 -1 1336.34 98.2998 16 -13 -7 1 1461.59 115.236 15 13 -8 -9 269.270 50.8301 12 -13 -8 8 84.1529 35.6022 15 13 -8 -8 56.2703 45.3625 12 -13 -8 7 199.176 45.7365 15 13 -8 -7 323.008 64.6266 12 -13 -8 6 41.3682 38.4011 15 13 -8 -6 34.7472 42.3475 12 -13 -8 5 755.193 83.2958 15 13 -8 -5 783.380 94.5282 12 -13 -8 4-8.11865 36.6452 15 13 -8 -4 28.1942 42.5867 12 14 0 -16 13.0215 42.8226 9 14 0 -15 50.1884 45.5900 9 14 0 -14 358.294 81.5790 9 14 0 -13-31.3363 50.4634 9 14 0 -12 1690.84 151.357 9 14 0 -11 23.4808 54.0525 9 14 0 -10 4402.76 244.032 9 -14 0 10 4597.76 255.440 14 14 0 -9-68.4503 49.2903 9 -14 0 9-20.7164 63.1168 14 -14 0 8 41.1888 51.7558 14 -14 0 7-32.8599 54.5048 14 -14 0 6 1470.06 148.011 14 -14 0 5-45.0226 57.4729 14 -14 0 4 501.338 94.9240 14 -14 0 3 74.1967 55.2931 14 -14 0 2 13789.9 429.358 14 -14 0 1 34.2778 54.0980 14 -14 0 0 1667.08 141.387 14 -14 0 -1 51.6184 47.4207 14 -14 0 -2 738.336 82.9202 14 14 -1 -16 849.544 91.5548 9 14 1 -16 635.955 81.6340 9 14 -1 -15 150.594 56.8216 9 14 1 -15 53.9915 48.6511 9 14 -1 -14-7.92339 46.2185 9 14 1 -14-25.4261 44.5631 9 14 -1 -13 1644.66 149.467 9 14 1 -13 1364.31 135.304 9 14 -1 -12 83.1899 63.3978 9 14 1 -12 31.9462 50.3841 9 14 -1 -11 418.784 94.9023 9 14 1 -11 324.889 74.0269 9 14 -1 -10 129.823 65.1944 9 14 1 -10 52.8851 41.4168 9 -14 -1 10 145.218 68.5654 14 -14 1 10 223.095 87.5993 14 14 1 -9 362.771 79.4047 9 -14 -1 9 388.251 78.3733 14 -14 1 9 403.773 86.8830 14 -14 -1 8 1121.93 132.952 14 -14 1 8 990.774 127.553 14 -14 -1 7 4587.93 253.137 14 -14 1 7 4165.59 247.841 14 -14 -1 6-23.0598 63.0880 14 -14 1 6-56.8770 62.1211 14 -14 -1 5 1327.49 138.483 14 -14 1 5 1179.62 140.634 14 -14 -1 4 2655.21 188.905 14 -14 1 4 2379.57 189.854 14 -14 -1 3 402.888 80.8350 14 -14 1 3 478.365 101.472 14 -14 -1 2 2530.79 179.656 14 -14 1 2 2183.84 177.309 14 -14 -1 1 513.668 82.6678 14 -14 1 1 409.136 83.4789 14 -14 -1 0 549.793 78.8904 14 -14 1 0 591.408 93.5481 14 -14 1 -1 22.4612 44.9512 14 -14 1 -2 344.776 64.6555 14 14 2 -16 26.4414 36.2843 9 14 2 -15 115.419 47.2184 9 14 2 -14 123.829 55.5690 9 14 2 -13 235.777 61.6199 9 14 2 -12 915.520 107.062 9 14 2 -11 510.784 90.1775 9 -14 -2 11 579.518 96.4543 14 14 2 -10 239.945 65.5866 9 -14 -2 10 204.345 72.6438 14 -14 2 10 164.605 73.3816 14 -14 -2 9 1670.53 147.406 14 -14 2 9 1588.10 157.061 14 -14 -2 8 397.770 81.3493 14 -14 2 8 287.834 82.2347 14 -14 2 7 401.550 88.0042 14 -14 2 6 9079.65 363.899 14 -14 2 5 8216.35 344.992 14 -14 2 4 212.114 69.0971 14 -14 2 3 1110.07 138.470 14 -14 2 2 180.023 62.4534 14 -14 2 1 765.078 108.043 14 -14 2 0 485.161 88.2397 14 -14 2 -1 934.485 106.173 14 -14 2 -2 14.8469 41.5981 14 14 3 -15 128.873 47.8569 9 14 3 -14 241.984 54.1428 9 14 3 -13 655.983 89.8290 9 14 3 -12 88.5352 47.1238 9 -14 3 12 242.834 71.5326 14 14 3 -11 375.854 71.8252 9 -14 3 11 310.880 79.5568 14 -14 3 10 1539.36 150.298 14 -14 3 9 47.7221 55.9206 14 -14 3 8 125.546 71.5247 14 -14 3 7 654.275 108.337 14 -14 3 6 4024.77 242.014 14 -14 3 5 3934.21 237.808 14 -14 3 4 449.401 94.3264 14 14 -3 -4 309.365 67.2131 12 -14 3 3-4.07354 63.6134 14 14 -3 -3 126.934 51.8235 12 -14 3 2 889.349 118.285 14 -14 3 1-41.8953 58.2664 14 -14 3 0 1364.60 130.403 14 -14 3 -1 35.0454 50.7083 14 -14 3 -2 190.793 54.4637 14 14 4 -15 109.521 40.8608 9 -14 4 15 43.9683 32.0015 14 14 4 -14 49.3455 34.7326 9 -14 4 14 98.9519 49.6710 14 -14 -4 13 357.219 70.0477 16 14 4 -13 300.705 58.9534 9 -14 4 13 341.473 73.3114 14 -14 -4 12 491.815 80.8173 16 14 4 -12 408.463 68.3945 9 -14 4 12 567.437 88.1335 14 -14 4 11 1683.68 147.631 14 -14 -4 11 1473.24 137.877 16 -14 -4 10 247.448 73.9623 16 -14 4 10 156.668 54.9893 14 -14 4 9 618.608 98.4713 14 -14 4 8-107.253 60.4846 14 -14 -4 7 19.6535 42.6618 15 -14 4 7 52.3257 55.5875 14 -14 -4 6 829.125 111.923 15 -14 4 6 694.278 107.198 14 -14 -4 5 94.3640 59.3636 15 -14 4 5 56.0813 49.0768 14 14 -4 -5 77.8273 54.6981 12 -14 -4 4 42.8173 59.2696 15 -14 4 4 82.2612 51.3849 14 14 -4 -4 29.2443 45.4238 12 -14 4 3 857.898 113.842 14 14 -4 -3 843.549 104.312 12 -14 4 2 1283.29 128.933 14 14 -4 -2 1266.26 115.725 12 -14 4 1 1395.48 130.213 14 -14 4 0 1152.75 112.654 14 -14 4 -1 878.422 93.0163 14 -14 5 14 275.632 50.1592 14 -14 -5 13 452.904 72.1626 16 -14 5 13 378.331 62.4069 14 -14 -5 12 328.761 67.4353 16 -14 5 12 366.863 67.7055 14 -14 -5 11 196.856 64.1158 16 -14 5 11 179.521 55.2724 14 -14 -5 10 600.862 92.0317 16 -14 5 10 646.778 86.0163 14 -14 5 9 917.435 107.894 14 -14 -5 8 391.968 68.5414 15 -14 5 8 229.228 61.7587 14 -14 -5 7 1071.63 111.431 15 -14 5 7 936.632 112.167 14 14 -5 -7 1028.93 125.973 12 -14 -5 6 169.457 54.7308 15 -14 5 6 236.732 67.6010 14 14 -5 -6 233.395 69.5528 12 -14 -5 5 93.3314 58.6211 15 -14 5 5-28.7610 44.7972 14 14 -5 -5-17.8896 51.8946 12 -14 -5 4 133.808 61.2092 15 -14 5 4 201.471 54.8429 14 14 -5 -4 201.882 63.9285 12 -14 -5 3 116.249 49.1754 15 -14 5 3 141.018 58.5547 14 14 -5 -3 95.9583 54.5270 12 -14 5 2-58.9824 50.2447 14 14 -5 -2 14.2125 36.7251 12 -14 5 1-30.3517 47.7337 14 14 -5 0 58.3256 42.5985 16 -14 5 0 32.7730 32.1909 14 14 -6 -12 1550.41 113.971 12 -14 -6 12 1551.13 114.679 16 -14 -6 11-26.9188 39.5028 16 14 -6 -11 25.0781 43.6651 12 14 -6 -10 199.178 65.0503 12 -14 6 9 1501.05 117.652 14 14 -6 -9 1833.08 143.047 12 -14 -6 8-31.6850 37.0594 15 -14 6 8 32.1819 39.2423 14 14 -6 -8-43.3572 52.0707 12 -14 -6 7 521.122 75.3160 15 -14 6 7 389.158 67.2959 14 14 -6 -7 399.038 77.4015 12 -14 -6 6 114.990 51.0712 15 -14 6 6 65.4070 38.6012 14 14 -6 -6 78.1732 49.2573 12 -14 -6 5 21.0819 41.3103 15 -14 6 5 39.8958 39.2357 14 14 -6 -5 21.6391 51.2421 12 -14 -6 4 2040.21 141.501 15 -14 6 4 2198.98 144.130 14 14 -6 -4 2300.42 153.573 12 -14 -6 3 1812.86 131.886 15 -14 6 3 1953.39 131.432 14 14 -6 -3 2046.23 141.692 12 14 -6 -2 214.524 48.4543 16 -14 6 2 290.621 55.1135 14 14 -6 -2 359.515 63.1490 12 14 -7 -9-59.2827 40.3577 12 14 -7 -8 74.0457 42.7256 12 -14 -7 7 260.976 50.3605 15 14 -7 -7 302.613 70.0759 12 -14 -7 6 1744.16 116.927 15 14 -7 -6 1692.32 124.870 12 -14 -7 5 67.6313 40.6807 15 14 -7 -5 50.9893 42.3833 12 15 0 -15 15.4388 36.9298 9 -15 0 15 19.4255 35.9614 14 15 0 -14 71.4933 47.0379 9 -15 0 14-34.8025 49.0236 14 15 0 -13-72.1228 44.4900 9 -15 0 13-49.2626 42.2085 14 15 0 -12 1688.57 138.698 9 -15 0 12 1760.08 148.835 14 -15 0 11 25.0353 51.7841 14 -15 0 10 383.819 79.7701 14 -15 0 9 49.4034 52.0141 14 -15 0 8 169.170 55.1791 14 -15 0 7 32.7534 51.9018 14 -15 0 6 176.111 58.1426 14 -15 0 5-30.2602 49.8399 14 -15 0 4 4246.36 226.037 14 -15 0 3 71.6164 53.0205 14 -15 0 2 93.0347 43.7646 14 -15 0 1 13.1047 36.7169 14 -15 0 0-11.6797 30.6196 14 15 1 -15-13.5117 33.5177 9 -15 1 15 39.8381 44.1314 14 15 1 -14 361.447 68.3379 9 -15 -1 14 425.502 71.4931 14 15 1 -13 327.804 64.5440 9 -15 -1 13 462.534 77.4592 14 -15 1 13 501.416 82.1624 14 15 1 -12 92.2803 50.8986 9 -15 -1 12 34.1208 44.9879 14 -15 1 12 70.3942 53.3522 14 15 1 -11 147.427 54.0705 9 -15 -1 11 158.126 66.1135 14 -15 1 11 176.280 72.0436 14 -15 -1 10 1292.26 128.501 14 -15 1 10 1004.36 118.377 14 -15 -1 9 182.450 58.3968 14 -15 1 9 164.406 71.9181 14 -15 -1 8 463.458 79.7622 14 -15 1 8 436.477 86.0489 14 -15 -1 7 406.902 77.0697 14 -15 1 7 377.624 83.3133 14 -15 -1 6 4769.41 235.782 14 -15 1 6 4020.66 226.389 14 -15 -1 5 181.363 60.2400 14 -15 1 5 19.4252 49.1570 14 -15 -1 4 198.116 62.9804 14 -15 1 4 86.1814 47.4837 14 -15 -1 3 562.880 80.0005 14 -15 1 3 711.748 98.8506 14 -15 -1 2 31.0952 39.9017 14 -15 1 2 33.8404 53.5668 14 -15 1 1 21.8304 44.0043 14 -15 1 0 177.519 51.7753 14 15 2 -14 82.5315 42.7202 9 -15 -2 14 77.7726 39.0092 14 -15 2 14 38.2291 41.8005 14 15 2 -13 199.490 52.6581 9 -15 -2 13 137.717 43.2291 14 -15 2 13 237.450 66.5619 14 15 2 -12 289.677 61.6347 9 -15 -2 12 299.154 62.8422 14 -15 2 12 397.833 84.0483 14 15 2 -11 3188.12 177.256 9 -15 -2 11 3494.13 182.777 14 -15 2 11 3517.04 208.334 14 -15 2 10 285.086 82.2576 14 -15 2 9 1283.80 136.534 14 -15 2 8-13.5292 61.0333 14 -15 2 7 16.0715 59.1759 14 -15 2 6 398.507 79.0184 14 -15 2 5 285.394 76.8742 14 -15 2 4 652.559 101.105 14 -15 2 3 405.551 81.2778 14 -15 2 2 2548.64 168.182 14 -15 2 1 757.355 89.0529 14 -15 2 0 191.369 53.5772 14 15 3 -14 308.311 53.4226 9 -15 3 14 322.281 60.8538 14 15 3 -13 710.635 76.8127 9 -15 3 13 673.230 90.2281 14 15 3 -12 217.179 48.9737 9 -15 3 12 232.190 63.1975 14 -15 3 11 89.7851 55.5144 14 -15 3 10 866.520 113.173 14 -15 3 9 72.0638 50.0661 14 -15 3 8 23.5093 56.9778 14 -15 3 7-4.03981 59.1933 14 -15 3 6 47.4116 53.7172 14 15 -3 -6-76.3713 58.1706 12 -15 3 5 232.215 65.4540 14 15 -3 -5 132.198 49.0870 12 -15 3 4 90.8651 60.7862 14 -15 3 3 752.415 100.950 14 -15 3 2 694.690 91.1479 14 -15 3 1 439.906 72.4289 14 -15 4 13-84.6880 42.3688 14 -15 4 12 30.5942 44.0115 14 -15 4 11 2007.03 144.856 14 -15 4 10 116.836 47.1011 14 -15 4 9 215.188 61.2200 14 -15 4 8 25.0918 45.3386 14 -15 4 7 12.8712 44.4875 14 15 -4 -7 131.625 55.4084 12 -15 4 6 71.6197 51.4542 14 15 -4 -6 199.154 54.6170 12 -15 4 5 206.075 64.7874 14 15 -4 -5 117.739 48.3064 12 -15 4 4 158.711 59.5724 14 15 -4 -4 121.880 46.0264 12 -15 4 3 103.085 49.8014 14 -15 4 2 548.822 76.0317 14 -15 5 11 507.097 66.4739 14 -15 5 10 365.081 63.7875 14 -15 5 9 18.0058 34.5710 14 15 -5 -9-48.9232 49.0733 12 -15 5 8 366.878 68.1055 14 15 -5 -8 302.038 66.0747 12 -15 5 7 381.931 72.0440 14 15 -5 -7 425.195 73.7409 12 -15 5 6 24.9457 41.4736 14 15 -5 -6-8.34168 38.5133 12 -15 5 5 13.7199 36.6682 14 15 -5 -5-38.9904 36.1252 12 -15 5 4 249.573 55.7906 14 15 -5 -4 172.797 48.1924 12 -16 0 13-49.0917 40.6893 14 -16 0 12 1826.19 129.236 14 -16 0 11-98.8575 48.0841 14 -16 0 10 87.5078 44.9326 14 -16 0 9-0.74186 40.8978 14 -16 0 8 317.158 59.9348 14 -16 0 7 62.1949 51.3658 14 -16 0 6 115.905 53.2532 14 -16 0 5 78.6571 43.4324 14 -16 0 4 148.099 45.8077 14 -16 0 3-10.2516 25.2657 14 -16 -1 13 173.540 42.2192 14 -16 1 13 388.124 66.4713 14 -16 -1 12 221.288 48.5952 14 -16 1 12 159.768 58.8242 14 -16 -1 11 794.246 84.5504 14 -16 1 11 799.499 93.8911 14 -16 -1 10 1819.98 127.906 14 -16 1 10 1782.31 136.381 14 -16 -1 9 81.4773 46.6981 14 -16 1 9-11.1211 48.7006 14 -16 -1 8 798.819 87.4262 14 -16 1 8 590.078 85.4062 14 -16 -1 7 285.489 62.8140 14 -16 1 7 226.382 62.7826 14 -16 -1 6-54.9700 32.3204 14 -16 1 6 27.7001 40.1003 14 -16 1 5 902.129 99.3607 14 -16 1 4 174.299 52.6092 14 -16 1 3 836.056 84.3137 14 -16 2 12 2895.36 161.252 14 -16 2 11 1073.57 104.280 14 -16 2 10-64.5272 55.8320 14 -16 2 9 340.246 72.5968 14 -16 2 8 996.135 106.077 14 -16 2 7 1954.78 145.987 14 16 -2 -7 1955.61 130.365 12 -16 2 6 16.8819 42.0627 14 -16 2 5 196.228 57.4147 14 -16 2 4 2251.29 144.710 14 -16 3 11 740.625 84.0736 14 -16 3 10 16.5327 37.4709 14 -16 3 9 1.89664 43.5932 14 -16 3 8 109.911 54.3273 14 16 -3 -8 54.5251 35.7653 12 -16 3 7 1341.86 118.548 14 16 -3 -7 1260.64 105.126 12 -16 3 6 760.115 93.2844 14 16 -3 -6 602.787 71.2504 12 -16 3 5 90.5222 43.4469 14 -16 4 9 167.420 48.2814 14 16 -4 -9 231.161 56.1161 12 -16 4 8 45.8982 41.0002 14 16 -4 -8-40.5342 38.7537 12 -16 4 7 854.661 87.9081 14 16 -4 -7 911.608 85.8427 12 0 0 0 0.00 0.00 0 TITL WLL148 in P2(1)/c REM P2(1)/c (#14 in standard setting) CELL 1.54184 14.098624 10.934614 16.350884 90.0000 115.1910 90.0000 ZERR 3.00 0.000439 0.000259 0.000541 0.0000 0.0039 0.0000 LATT 1 SYMM -x, y+1/2,-z+1/2 SFAC C H N O UNIT 120.00 120.00 12.00 6.00 TREF HKLF 4 END ; _shelx_hkl_checksum 51936 _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; _oxdiff_exptl_absorpt_empirical_full_max 1.317 _oxdiff_exptl_absorpt_empirical_full_min 0.919 ####################################################################### # # This file contains crystal structure data downloaded from the # Cambridge Structural Database (CSD) hosted by the Cambridge # Crystallographic Data Centre (CCDC). # # Full information about CCDC data access policies and citation # guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 # # Audit and citation data items may have been added by the CCDC. # Please retain this information to preserve the provenance of # this file and to allow appropriate attribution of the data. # ####################################################################### data_hd_wql32 _database_code_depnum_ccdc_archive 'CCDC 2086416' loop_ _audit_author_name _audit_author_address 'Qilin Wang' ;Henan University China ; _audit_update_record ; 2021-05-28 deposited with the CCDC. 2021-11-08 downloaded from the CCDC. ; _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety 'C25 H24 N2 O5' _chemical_formula_sum 'C25 H24 N2 O5' _chemical_formula_iupac ? _chemical_formula_weight 432.46 _chemical_melting_point ? _space_group_crystal_system orthorhombic _space_group_name_H-M_alt 'P b c n' _space_group_name_Hall '-P 2n 2ab' loop_ _space_group_symop_operation_xyz 'x, y, z' 'x+1/2, -y+1/2, -z' '-x, y, -z+1/2' '-x+1/2, -y+1/2, z+1/2' '-x, -y, -z' '-x-1/2, y-1/2, z' 'x, -y, z-1/2' 'x-1/2, y-1/2, -z-1/2' _cell_length_a 25.4779(15) _cell_length_b 11.8085(6) _cell_length_c 13.8705(7) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 4173.0(4) _cell_formula_units_Z 8 _cell_measurement_reflns_used 9961 _cell_measurement_theta_min 3.4695 _cell_measurement_theta_max 72.4255 _cell_measurement_temperature 100.(2) _exptl_crystal_description plate _exptl_crystal_colour 'clear light yellow' _exptl_crystal_size_max 0.350 _exptl_crystal_size_mid 0.330 _exptl_crystal_size_min 0.010 _exptl_crystal_density_diffrn 1.377 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1824 _exptl_absorpt_coefficient_mu 0.792 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_process_details ; SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction ; _exptl_absorpt_correction_T_min 0.57 _exptl_absorpt_correction_T_max 0.99 _exptl_special_details ; ; _diffrn_ambient_temperature 100.(2) _diffrn_source 'Ius Diamond' _diffrn_source_type Microfocus _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_monochromator 'Helixos MX multilayer Optic' _diffrn_measurement_device_type 'Bruker D8 QUEST PHOTON II' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean 7.3910 _diffrn_reflns_number 45327 _diffrn_reflns_av_R_equivalents 0.1556 _diffrn_reflns_av_unetI/netI 0.0586 _diffrn_reflns_theta_min 3.47 _diffrn_reflns_theta_max 72.73 _diffrn_reflns_theta_full 72.73 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measured_fraction_theta_full 0.998 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _refine_special_details ; ; _reflns_number_total 4147 _reflns_number_gt 3183 _reflns_threshold_expression 'I > 2\s(I)' _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_R_factor_all 0.0928 _refine_ls_R_factor_gt 0.0766 _refine_ls_wR_factor_gt 0.2010 _refine_ls_wR_factor_ref 0.2225 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.053 _refine_ls_number_reflns 4147 _refine_ls_number_parameters 291 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_hydrogen_treatment constr _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.1569P)^2^+0.5614P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.430 _refine_diff_density_min -0.462 _refine_ls_extinction_method 'SHELXL-2017/1 (Sheldrick 2017)' _refine_ls_extinction_coef 0.0008(3) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _computing_data_collection 'Bruker Instrument Service vV6.2.9' _computing_cell_refinement 'SAINT V8.38A (Bruker AXS Inc., 2017)' _computing_data_reduction 'SAINT V8.38A (Bruker AXS Inc., 2017)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _computing_structure_refinement 'SHELXL-2017/1 (Sheldrick, 2017)' _computing_molecular_graphics 'shelXle (C.B. Huebschle, rev 882)' _computing_publication_material ? loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_refinement_flags_posn _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group O O1 0.51621(7) 0.86936(16) 0.57694(13) 0.0320(4) Uani d . . . 1 . . O O2 0.52499(8) 0.76466(18) 0.44214(14) 0.0367(5) Uani d . . . 1 . . O O3 0.81679(9) 0.79248(18) 0.32222(16) 0.0448(6) Uani d . . . 1 . . O O4 0.79965(8) 0.62734(17) 0.25898(13) 0.0345(5) Uani d . . . 1 . . O O5 0.73013(8) 0.53745(15) 0.58533(14) 0.0341(5) Uani d . . . 1 . . N N1 0.66848(8) 0.60215(17) 0.41986(15) 0.0260(5) Uani d . . . 1 . . N N2 0.78896(9) 0.70482(19) 0.31735(15) 0.0309(5) Uani d . . . 1 . . C C1 0.43772(12) 0.8975(3) 0.6666(2) 0.0397(7) Uani d . . . 1 . . H H1 0.454784 0.872121 0.726095 0.06 Uiso calc U . R 1 . . H H4 0.400072 0.881008 0.669927 0.06 Uiso calc U . R 1 . . H H3 0.442908 0.979281 0.658916 0.06 Uiso calc U . R 1 . . C C2 0.46131(11) 0.8366(3) 0.5821(2) 0.0362(6) Uani d . . . 1 . . H H23 0.458203 0.753666 0.590796 0.043 Uiso calc U . R 1 . . H H24 0.442922 0.858007 0.521885 0.043 Uiso calc U . R 1 . . C C3 0.54358(10) 0.8259(2) 0.50235(18) 0.0289(6) Uani d . . . 1 . . C C4 0.59951(10) 0.8679(2) 0.50489(18) 0.0282(5) Uani d . . . 1 . . H H21 0.611932 0.867113 0.572516 0.034 Uiso calc U . R 1 . . H H22 0.600182 0.947458 0.482352 0.034 Uiso calc U . R 1 . . C C5 0.63739(10) 0.7989(2) 0.44363(17) 0.0267(5) Uani d . . . 1 . . H H5 0.61953 0.776897 0.382214 0.032 Uiso calc U . R 1 . . C C6 0.65765(10) 0.6887(2) 0.49574(17) 0.0265(5) Uani d . . . 1 . . C C7 0.70974(10) 0.7276(2) 0.53986(18) 0.0251(5) Uani d . . . 1 . . H H11 0.702087 0.785814 0.590306 0.03 Uiso calc U . R 1 . . C C8 0.74373(10) 0.6366(2) 0.58405(17) 0.0264(5) Uani d . . . 1 . . C C9 0.79605(10) 0.6714(2) 0.62284(17) 0.0268(5) Uani d . . . 1 . . C C10 0.83391(10) 0.5881(2) 0.63798(17) 0.0280(5) Uani d . . . 1 . . H H14 0.825403 0.510731 0.627696 0.034 Uiso calc U . R 1 . . C C11 0.88402(11) 0.6180(2) 0.66805(18) 0.0313(6) Uani d . . . 1 . . H H15 0.909971 0.561088 0.676776 0.038 Uiso calc U . R 1 . . C C12 0.89629(10) 0.7306(2) 0.68539(19) 0.0318(6) Uani d . . . 1 . . H H2 0.930712 0.750999 0.70518 0.038 Uiso calc U . R 1 . . C C13 0.61809(10) 0.6273(2) 0.55624(18) 0.0265(5) Uani d . . . 1 . . C C14 0.59995(10) 0.6562(2) 0.64744(19) 0.0278(5) Uani d . . . 1 . . H H20 0.614592 0.718318 0.681657 0.033 Uiso calc U . R 1 . . C C15 0.55969(10) 0.5916(2) 0.68730(19) 0.0299(6) Uani d . . . 1 . . H H6 0.546641 0.609841 0.749546 0.036 Uiso calc U . R 1 . . C C16 0.53835(10) 0.5006(2) 0.6371(2) 0.0319(6) Uani d . . . 1 . . H H7 0.509955 0.459282 0.664231 0.038 Uiso calc U . R 1 . . C C17 0.55827(10) 0.4695(2) 0.54747(19) 0.0292(5) Uani d . . . 1 . . H H8 0.544477 0.406035 0.51387 0.035 Uiso calc U . R 1 . . C C18 0.59860(10) 0.5331(2) 0.50841(18) 0.0269(5) Uani d . . . 1 . . C C19 0.62776(11) 0.5144(2) 0.41524(19) 0.0307(6) Uani d . . . 1 . . H H10 0.643342 0.437687 0.41252 0.037 Uiso calc U . R 1 . . H H9 0.604544 0.525424 0.358779 0.037 Uiso calc U . R 1 . . C C20 0.71151(10) 0.6072(2) 0.36648(17) 0.0271(5) Uani d . . . 1 . . H H19 0.718711 0.5497 0.32046 0.033 Uiso calc U . R 1 . . C C21 0.74578(10) 0.6964(2) 0.37809(17) 0.0280(5) Uani d . . . 1 . . C C22 0.73417(10) 0.7882(2) 0.45091(17) 0.0278(5) Uani d . . . 1 . . H H16 0.766267 0.832446 0.468302 0.033 Uiso calc U . R 1 . . C C23 0.80823(10) 0.7850(2) 0.64181(18) 0.0283(5) Uani d . . . 1 . . H H12 0.782466 0.842178 0.632834 0.034 Uiso calc U . R 1 . . C C24 0.85812(11) 0.8135(2) 0.67375(18) 0.0301(6) Uani d . . . 1 . . H H13 0.866232 0.890267 0.68777 0.036 Uiso calc U . R 1 . . C C25 0.68871(10) 0.8652(2) 0.41916(18) 0.0284(5) Uani d . . . 1 . . H H17 0.690778 0.880884 0.349143 0.034 Uiso calc U . R 1 . . H H18 0.689785 0.938051 0.454442 0.034 Uiso calc U . R 1 . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 O1 0.0348(9) 0.0273(10) 0.0340(10) 0.0026(7) 0.0003(7) -0.0041(8) O2 0.0394(10) 0.0341(11) 0.0365(10) 0.0015(8) -0.0023(8) -0.0076(8) O3 0.0522(12) 0.0353(12) 0.0468(12) -0.0174(9) 0.0162(10) -0.0120(9) O4 0.0409(10) 0.0321(10) 0.0304(9) -0.0002(8) 0.0047(7) -0.0063(8) O5 0.0435(11) 0.0187(9) 0.0400(10) -0.0020(7) -0.0059(8) 0.0016(7) N1 0.0341(11) 0.0163(10) 0.0277(10) -0.0005(8) 0.0006(8) -0.0027(8) N2 0.0391(12) 0.0270(11) 0.0264(10) -0.0023(9) 0.0027(8) -0.0023(9) C1 0.0416(15) 0.0410(16) 0.0366(14) 0.0048(12) 0.0020(11) 0.0013(12) C2 0.0323(13) 0.0355(15) 0.0408(15) 0.0013(11) -0.0011(10) -0.0029(12) C3 0.0379(13) 0.0204(12) 0.0286(12) 0.0023(10) -0.0015(10) -0.0013(10) C4 0.0362(13) 0.0190(12) 0.0294(12) 0.0007(9) -0.0016(9) -0.0024(10) C5 0.0354(13) 0.0178(12) 0.0270(11) 0.0024(9) -0.0002(9) 0.0004(9) C6 0.0330(12) 0.0202(12) 0.0263(12) 0.0037(9) 0.0004(9) -0.0025(9) C7 0.0324(12) 0.0149(11) 0.0282(11) -0.0006(9) -0.0016(9) -0.0021(9) C8 0.0361(12) 0.0189(11) 0.0243(11) 0.0004(9) 0.0005(9) -0.0001(9) C9 0.0356(12) 0.0203(12) 0.0244(11) -0.0008(9) 0.0009(9) 0.0016(9) C10 0.0395(13) 0.0187(12) 0.0259(11) 0.0015(10) 0.0016(9) 0.0010(9) C11 0.0380(13) 0.0291(14) 0.0268(12) 0.0012(10) -0.0012(10) 0.0040(10) C12 0.0347(13) 0.0309(14) 0.0296(12) -0.0016(10) -0.0007(9) 0.0013(11) C13 0.0337(12) 0.0187(11) 0.0271(11) 0.0003(9) -0.0004(9) 0.0042(9) C14 0.0342(12) 0.0212(12) 0.0279(12) -0.0017(10) -0.0011(9) -0.0013(10) C15 0.0328(12) 0.0274(13) 0.0295(12) 0.0004(10) 0.0011(10) 0.0045(10) C16 0.0325(12) 0.0253(12) 0.0379(13) 0.0006(10) 0.0021(10) 0.0049(11) C17 0.0332(12) 0.0188(11) 0.0356(13) -0.0012(9) -0.0034(10) -0.0004(10) C18 0.0345(12) 0.0172(11) 0.0291(12) 0.0010(9) -0.0022(9) 0.0031(9) C19 0.0386(13) 0.0202(12) 0.0332(13) -0.0062(10) 0.0011(10) -0.0043(10) C20 0.0349(12) 0.0214(12) 0.0251(11) 0.0001(9) -0.0014(9) -0.0029(9) C21 0.0358(12) 0.0222(12) 0.0260(11) -0.0021(10) 0.0019(9) -0.0012(10) C22 0.0389(13) 0.0195(11) 0.0249(11) 0.0001(9) -0.0021(9) 0.0010(9) C23 0.0365(13) 0.0221(12) 0.0263(11) -0.0010(10) 0.0001(9) 0.0008(9) C24 0.0425(14) 0.0210(12) 0.0267(12) -0.0033(10) 0.0004(10) -0.0002(9) C25 0.0386(13) 0.0194(12) 0.0270(11) -0.0008(10) 0.0003(9) 0.0031(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag O1 C3 . 1.349(3) ? O1 C2 . 1.453(3) ? O2 C3 . 1.202(3) ? O3 N2 . 1.256(3) ? O4 N2 . 1.252(3) ? O5 C8 . 1.222(3) ? N1 C20 . 1.324(3) ? N1 C19 . 1.467(3) ? N1 C6 . 1.493(3) ? N2 C21 . 1.389(3) ? C1 C2 . 1.501(4) ? C1 H1 . 0.98 ? C1 H4 . 0.98 ? C1 H3 . 0.98 ? C2 H23 . 0.99 ? C2 H24 . 0.99 ? C3 C4 . 1.509(4) ? C4 C5 . 1.523(3) ? C4 H21 . 0.99 ? C4 H22 . 0.99 ? C5 C25 . 1.562(3) ? C5 C6 . 1.575(3) ? C5 H5 . 1.0 ? C6 C13 . 1.499(3) ? C6 C7 . 1.532(3) ? C7 C8 . 1.510(3) ? C7 C22 . 1.556(3) ? C7 H11 . 1.0 ? C8 C9 . 1.495(3) ? C9 C10 . 1.394(4) ? C9 C23 . 1.401(3) ? C10 C11 . 1.389(4) ? C10 H14 . 0.95 ? C11 C12 . 1.387(4) ? C11 H15 . 0.95 ? C12 C24 . 1.389(4) ? C12 H2 . 0.95 ? C13 C18 . 1.387(4) ? C13 C14 . 1.389(4) ? C14 C15 . 1.393(4) ? C14 H20 . 0.95 ? C15 C16 . 1.391(4) ? C15 H6 . 0.95 ? C16 C17 . 1.392(4) ? C16 H7 . 0.95 ? C17 C18 . 1.383(4) ? C17 H8 . 0.95 ? C18 C19 . 1.507(4) ? C19 H10 . 0.99 ? C19 H9 . 0.99 ? C20 C21 . 1.378(3) ? C20 H19 . 0.95 ? C21 C22 . 1.511(3) ? C22 C25 . 1.537(3) ? C22 H16 . 1.0 ? C23 C24 . 1.387(4) ? C23 H12 . 0.95 ? C24 H13 . 0.95 ? C25 H17 . 0.99 ? C25 H18 . 0.99 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C3 O1 C2 . . 115.7(2) ? C20 N1 C19 . . 126.4(2) ? C20 N1 C6 . . 121.1(2) ? C19 N1 C6 . . 112.6(2) ? O4 N2 O3 . . 121.0(2) ? O4 N2 C21 . . 120.8(2) ? O3 N2 C21 . . 118.2(2) ? C2 C1 H1 . . 109.5 ? C2 C1 H4 . . 109.5 ? H1 C1 H4 . . 109.5 ? C2 C1 H3 . . 109.5 ? H1 C1 H3 . . 109.5 ? H4 C1 H3 . . 109.5 ? O1 C2 C1 . . 107.2(2) ? O1 C2 H23 . . 110.3 ? C1 C2 H23 . . 110.3 ? O1 C2 H24 . . 110.3 ? C1 C2 H24 . . 110.3 ? H23 C2 H24 . . 108.5 ? O2 C3 O1 . . 123.9(2) ? O2 C3 C4 . . 125.9(2) ? O1 C3 C4 . . 110.2(2) ? C3 C4 C5 . . 114.2(2) ? C3 C4 H21 . . 108.7 ? C5 C4 H21 . . 108.7 ? C3 C4 H22 . . 108.7 ? C5 C4 H22 . . 108.7 ? H21 C4 H22 . . 107.6 ? C4 C5 C25 . . 112.5(2) ? C4 C5 C6 . . 113.2(2) ? C25 C5 C6 . . 103.87(19) ? C4 C5 H5 . . 109.0 ? C25 C5 H5 . . 109.0 ? C6 C5 H5 . . 109.0 ? N1 C6 C13 . . 100.81(19) ? N1 C6 C7 . . 109.07(19) ? C13 C6 C7 . . 120.3(2) ? N1 C6 C5 . . 107.61(19) ? C13 C6 C5 . . 115.9(2) ? C7 C6 C5 . . 102.69(19) ? C8 C7 C6 . . 116.5(2) ? C8 C7 C22 . . 114.8(2) ? C6 C7 C22 . . 99.65(19) ? C8 C7 H11 . . 108.5 ? C6 C7 H11 . . 108.5 ? C22 C7 H11 . . 108.5 ? O5 C8 C9 . . 120.7(2) ? O5 C8 C7 . . 121.7(2) ? C9 C8 C7 . . 117.5(2) ? C10 C9 C23 . . 119.6(2) ? C10 C9 C8 . . 118.5(2) ? C23 C9 C8 . . 121.9(2) ? C11 C10 C9 . . 120.2(2) ? C11 C10 H14 . . 119.9 ? C9 C10 H14 . . 119.9 ? C12 C11 C10 . . 120.2(2) ? C12 C11 H15 . . 119.9 ? C10 C11 H15 . . 119.9 ? C11 C12 C24 . . 119.8(2) ? C11 C12 H2 . . 120.1 ? C24 C12 H2 . . 120.1 ? C18 C13 C14 . . 120.9(2) ? C18 C13 C6 . . 111.2(2) ? C14 C13 C6 . . 127.9(2) ? C13 C14 C15 . . 118.1(2) ? C13 C14 H20 . . 120.9 ? C15 C14 H20 . . 120.9 ? C16 C15 C14 . . 120.8(2) ? C16 C15 H6 . . 119.6 ? C14 C15 H6 . . 119.6 ? C15 C16 C17 . . 120.5(2) ? C15 C16 H7 . . 119.7 ? C17 C16 H7 . . 119.7 ? C18 C17 C16 . . 118.5(2) ? C18 C17 H8 . . 120.7 ? C16 C17 H8 . . 120.7 ? C17 C18 C13 . . 120.9(2) ? C17 C18 C19 . . 128.5(2) ? C13 C18 C19 . . 110.6(2) ? N1 C19 C18 . . 102.0(2) ? N1 C19 H10 . . 111.4 ? C18 C19 H10 . . 111.4 ? N1 C19 H9 . . 111.4 ? C18 C19 H9 . . 111.4 ? H10 C19 H9 . . 109.2 ? N1 C20 C21 . . 119.6(2) ? N1 C20 H19 . . 120.2 ? C21 C20 H19 . . 120.2 ? C20 C21 N2 . . 119.0(2) ? C20 C21 C22 . . 120.2(2) ? N2 C21 C22 . . 120.6(2) ? C21 C22 C25 . . 112.4(2) ? C21 C22 C7 . . 106.2(2) ? C25 C22 C7 . . 101.41(19) ? C21 C22 H16 . . 112.1 ? C25 C22 H16 . . 112.1 ? C7 C22 H16 . . 112.1 ? C24 C23 C9 . . 119.7(2) ? C24 C23 H12 . . 120.2 ? C9 C23 H12 . . 120.2 ? C23 C24 C12 . . 120.5(2) ? C23 C24 H13 . . 119.8 ? C12 C24 H13 . . 119.8 ? C22 C25 C5 . . 105.77(19) ? C22 C25 H17 . . 110.6 ? C5 C25 H17 . . 110.6 ? C22 C25 H18 . . 110.6 ? C5 C25 H18 . . 110.6 ? H17 C25 H18 . . 108.7 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag C3 O1 C2 C1 . . . . -177.5(2) ? C2 O1 C3 O2 . . . . 0.7(4) ? C2 O1 C3 C4 . . . . 179.2(2) ? O2 C3 C4 C5 . . . . -18.7(4) ? O1 C3 C4 C5 . . . . 162.8(2) ? C3 C4 C5 C25 . . . . 160.3(2) ? C3 C4 C5 C6 . . . . -82.3(3) ? C20 N1 C6 C13 . . . . -160.9(2) ? C19 N1 C6 C13 . . . . 17.6(3) ? C20 N1 C6 C7 . . . . -33.4(3) ? C19 N1 C6 C7 . . . . 145.1(2) ? C20 N1 C6 C5 . . . . 77.3(3) ? C19 N1 C6 C5 . . . . -104.1(2) ? C4 C5 C6 N1 . . . . 149.9(2) ? C25 C5 C6 N1 . . . . -87.7(2) ? C4 C5 C6 C13 . . . . 38.0(3) ? C25 C5 C6 C13 . . . . 160.4(2) ? C4 C5 C6 C7 . . . . -95.1(2) ? C25 C5 C6 C7 . . . . 27.3(2) ? N1 C6 C7 C8 . . . . -57.6(3) ? C13 C6 C7 C8 . . . . 57.9(3) ? C5 C6 C7 C8 . . . . -171.6(2) ? N1 C6 C7 C22 . . . . 66.4(2) ? C13 C6 C7 C22 . . . . -178.0(2) ? C5 C6 C7 C22 . . . . -47.5(2) ? C6 C7 C8 O5 . . . . -0.7(3) ? C22 C7 C8 O5 . . . . -116.6(3) ? C6 C7 C8 C9 . . . . 176.8(2) ? C22 C7 C8 C9 . . . . 60.9(3) ? O5 C8 C9 C10 . . . . 15.8(4) ? C7 C8 C9 C10 . . . . -161.7(2) ? O5 C8 C9 C23 . . . . -165.8(2) ? C7 C8 C9 C23 . . . . 16.7(3) ? C23 C9 C10 C11 . . . . -2.5(4) ? C8 C9 C10 C11 . . . . 175.9(2) ? C9 C10 C11 C12 . . . . 1.5(4) ? C10 C11 C12 C24 . . . . 0.8(4) ? N1 C6 C13 C18 . . . . -14.3(3) ? C7 C6 C13 C18 . . . . -134.0(2) ? C5 C6 C13 C18 . . . . 101.5(2) ? N1 C6 C13 C14 . . . . 167.4(2) ? C7 C6 C13 C14 . . . . 47.7(4) ? C5 C6 C13 C14 . . . . -76.8(3) ? C18 C13 C14 C15 . . . . -3.4(4) ? C6 C13 C14 C15 . . . . 174.8(2) ? C13 C14 C15 C16 . . . . 0.1(4) ? C14 C15 C16 C17 . . . . 2.6(4) ? C15 C16 C17 C18 . . . . -1.9(4) ? C16 C17 C18 C13 . . . . -1.4(4) ? C16 C17 C18 C19 . . . . 177.6(2) ? C14 C13 C18 C17 . . . . 4.1(4) ? C6 C13 C18 C17 . . . . -174.4(2) ? C14 C13 C18 C19 . . . . -175.1(2) ? C6 C13 C18 C19 . . . . 6.5(3) ? C20 N1 C19 C18 . . . . 164.2(2) ? C6 N1 C19 C18 . . . . -14.2(3) ? C17 C18 C19 N1 . . . . -174.5(2) ? C13 C18 C19 N1 . . . . 4.6(3) ? C19 N1 C20 C21 . . . . 178.9(2) ? C6 N1 C20 C21 . . . . -2.9(4) ? N1 C20 C21 N2 . . . . -175.8(2) ? N1 C20 C21 C22 . . . . -0.3(4) ? O4 N2 C21 C20 . . . . -6.8(4) ? O3 N2 C21 C20 . . . . 172.8(2) ? O4 N2 C21 C22 . . . . 177.8(2) ? O3 N2 C21 C22 . . . . -2.6(4) ? C20 C21 C22 C25 . . . . -71.8(3) ? N2 C21 C22 C25 . . . . 103.6(3) ? C20 C21 C22 C7 . . . . 38.2(3) ? N2 C21 C22 C7 . . . . -146.4(2) ? C8 C7 C22 C21 . . . . 57.5(3) ? C6 C7 C22 C21 . . . . -67.7(2) ? C8 C7 C22 C25 . . . . 175.1(2) ? C6 C7 C22 C25 . . . . 49.9(2) ? C10 C9 C23 C24 . . . . 1.2(4) ? C8 C9 C23 C24 . . . . -177.2(2) ? C9 C23 C24 C12 . . . . 1.2(4) ? C11 C12 C24 C23 . . . . -2.1(4) ? C21 C22 C25 C5 . . . . 80.0(2) ? C7 C22 C25 C5 . . . . -32.9(2) ? C4 C5 C25 C22 . . . . 126.6(2) ? C6 C5 C25 C22 . . . . 3.8(2) ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag C7 H11 O4 4_665 1.00 2.55 3.497(3) 156.9 ? C19 H10 O3 6_755 0.99 2.35 3.245(3) 149.3 ? _shelx_res_file ; TITL hd_wql32_0m_a.res in Pbcn hd_wql32_0m.res created by SHELXL-2017/1 at 13:00:23 on 15-Oct-2020 CELL 1.54178 25.4779 11.8085 13.8705 90.000 90.000 90.000 ZERR 8.00 0.0015 0.0006 0.0007 0.000 0.000 0.000 LATT 1 SYMM x+1/2, -y+1/2, -z SYMM -x, y, -z+1/2 SYMM -x+1/2, -y+1/2, z+1/2 SFAC C H N O UNIT 200 192 16 40 LIST 4 ! automatically inserted. Change 6 to 4 for CHECKCIF!! TEMP -173.190 SIZE 0.010 0.330 0.350 ACTA EQIV $1 -x+3/2, -y+3/2, z+1/2 HTAB C7 O4_$1 EQIV $2 -x+3/2, y-1/2, z HTAB C19 O3_$2 L.S. 4 FMAP 2 PLAN -5 0 0.00 HTAB BOND $H CONF WGHT 0.156900 0.561400 EXTI 0.000842 FVAR 0.36266 O1 4 0.516210 0.869364 0.576942 11.00000 0.03485 0.02732 = 0.03398 -0.00413 0.00027 0.00258 O2 4 0.524993 0.764662 0.442141 11.00000 0.03944 0.03414 = 0.03652 -0.00763 -0.00232 0.00153 O3 4 0.816789 0.792477 0.322225 11.00000 0.05216 0.03529 = 0.04680 -0.01200 0.01618 -0.01740 O4 4 0.799646 0.627341 0.258975 11.00000 0.04094 0.03212 = 0.03039 -0.00633 0.00471 -0.00017 O5 4 0.730133 0.537451 0.585335 11.00000 0.04347 0.01866 = 0.04004 0.00162 -0.00592 -0.00200 N1 3 0.668480 0.602145 0.419857 11.00000 0.03415 0.01628 = 0.02772 -0.00271 0.00055 -0.00055 N2 3 0.788964 0.704821 0.317350 11.00000 0.03910 0.02702 = 0.02645 -0.00232 0.00269 -0.00227 C1 1 0.437722 0.897543 0.666587 11.00000 0.04162 0.04104 = 0.03658 0.00132 0.00204 0.00480 AFIX 137 H1 2 0.454784 0.872121 0.726095 11.00000 -1.50000 H4 2 0.400072 0.881008 0.669927 11.00000 -1.50000 H3 2 0.442908 0.979281 0.658916 11.00000 -1.50000 AFIX 0 C2 1 0.461315 0.836601 0.582058 11.00000 0.03235 0.03551 = 0.04081 -0.00288 -0.00110 0.00128 AFIX 23 H23 2 0.458203 0.753666 0.590796 11.00000 -1.20000 H24 2 0.442922 0.858007 0.521885 11.00000 -1.20000 AFIX 0 C3 1 0.543582 0.825911 0.502348 11.00000 0.03790 0.02036 = 0.02857 -0.00131 -0.00145 0.00228 C4 1 0.599508 0.867924 0.504892 11.00000 0.03616 0.01905 = 0.02944 -0.00244 -0.00160 0.00073 AFIX 23 H21 2 0.611932 0.867113 0.572516 11.00000 -1.20000 H22 2 0.600182 0.947458 0.482352 11.00000 -1.20000 AFIX 0 C5 1 0.637389 0.798860 0.443631 11.00000 0.03540 0.01776 = 0.02705 0.00044 -0.00021 0.00235 AFIX 13 H5 2 0.619530 0.776897 0.382214 11.00000 -1.20000 AFIX 0 C6 1 0.657648 0.688724 0.495735 11.00000 0.03297 0.02018 = 0.02630 -0.00255 0.00043 0.00370 C7 1 0.709736 0.727609 0.539859 11.00000 0.03237 0.01487 = 0.02818 -0.00212 -0.00160 -0.00062 AFIX 13 H11 2 0.702087 0.785814 0.590306 11.00000 -1.20000 AFIX 0 C8 1 0.743730 0.636637 0.584045 11.00000 0.03607 0.01892 = 0.02432 -0.00013 0.00046 0.00038 C9 1 0.796049 0.671447 0.622843 11.00000 0.03561 0.02035 = 0.02440 0.00157 0.00095 -0.00079 C10 1 0.833905 0.588125 0.637979 11.00000 0.03953 0.01874 = 0.02585 0.00099 0.00160 0.00146 AFIX 43 H14 2 0.825403 0.510731 0.627696 11.00000 -1.20000 AFIX 0 C11 1 0.884025 0.617950 0.668054 11.00000 0.03804 0.02908 = 0.02681 0.00395 -0.00123 0.00125 AFIX 43 H15 2 0.909971 0.561088 0.676776 11.00000 -1.20000 AFIX 0 C12 1 0.896290 0.730596 0.685393 11.00000 0.03472 0.03093 = 0.02965 0.00135 -0.00073 -0.00156 AFIX 43 H2 2 0.930712 0.750999 0.705180 11.00000 -1.20000 AFIX 0 C13 1 0.618089 0.627278 0.556240 11.00000 0.03365 0.01868 = 0.02706 0.00423 -0.00041 0.00035 C14 1 0.599949 0.656199 0.647441 11.00000 0.03418 0.02122 = 0.02792 -0.00132 -0.00106 -0.00173 AFIX 43 H20 2 0.614592 0.718318 0.681657 11.00000 -1.20000 AFIX 0 C15 1 0.559687 0.591550 0.687303 11.00000 0.03284 0.02737 = 0.02948 0.00453 0.00112 0.00041 AFIX 43 H6 2 0.546641 0.609841 0.749546 11.00000 -1.20000 AFIX 0 C16 1 0.538351 0.500569 0.637119 11.00000 0.03246 0.02533 = 0.03795 0.00489 0.00214 0.00060 AFIX 43 H7 2 0.509955 0.459282 0.664231 11.00000 -1.20000 AFIX 0 C17 1 0.558272 0.469509 0.547469 11.00000 0.03319 0.01883 = 0.03565 -0.00038 -0.00340 -0.00123 AFIX 43 H8 2 0.544477 0.406035 0.513870 11.00000 -1.20000 AFIX 0 C18 1 0.598596 0.533125 0.508409 11.00000 0.03447 0.01721 = 0.02910 0.00314 -0.00222 0.00099 C19 1 0.627765 0.514427 0.415236 11.00000 0.03864 0.02020 = 0.03319 -0.00434 0.00108 -0.00620 AFIX 23 H10 2 0.643342 0.437687 0.412520 11.00000 -1.20000 H9 2 0.604544 0.525424 0.358779 11.00000 -1.20000 AFIX 0 C20 1 0.711514 0.607227 0.366477 11.00000 0.03485 0.02136 = 0.02507 -0.00291 -0.00141 0.00009 AFIX 43 H19 2 0.718711 0.549700 0.320460 11.00000 -1.20000 AFIX 0 C21 1 0.745776 0.696435 0.378087 11.00000 0.03584 0.02217 = 0.02600 -0.00115 0.00191 -0.00210 C22 1 0.734171 0.788192 0.450909 11.00000 0.03888 0.01953 = 0.02486 0.00102 -0.00205 0.00009 AFIX 13 H16 2 0.766267 0.832446 0.468302 11.00000 -1.20000 AFIX 0 C23 1 0.808234 0.784993 0.641806 11.00000 0.03652 0.02206 = 0.02628 0.00085 0.00006 -0.00103 AFIX 43 H12 2 0.782466 0.842178 0.632834 11.00000 -1.20000 AFIX 0 C24 1 0.858117 0.813491 0.673751 11.00000 0.04253 0.02104 = 0.02667 -0.00024 0.00038 -0.00332 AFIX 43 H13 2 0.866232 0.890267 0.687770 11.00000 -1.20000 AFIX 0 C25 1 0.688710 0.865212 0.419156 11.00000 0.03865 0.01944 = 0.02704 0.00309 0.00028 -0.00078 AFIX 23 H17 2 0.690778 0.880884 0.349143 11.00000 -1.20000 H18 2 0.689785 0.938051 0.454442 11.00000 -1.20000 AFIX 0 HKLF 4 1 1 0 0 0 1 0 0 0 1 REM hd_wql32_0m_a.res in Pbcn REM R1 = 0.0766 for 3183 Fo > 4sig(Fo) and 0.0928 for all 4147 data REM 291 parameters refined using 0 restraints END WGHT 0.1569 0.5614 REM Instructions for potential hydrogen bonds HTAB C7 O4_$1 HTAB C19 O3_$2 REM Highest difference peak 0.430, deepest hole -0.462, 1-sigma level 0.089 Q1 1 0.6489 0.7487 0.4742 11.00000 0.05 0.36 Q2 1 0.7360 0.7464 0.4171 11.00000 0.05 0.34 Q3 1 0.6129 0.4646 0.3583 11.00000 0.05 0.33 Q4 1 0.7101 0.7875 0.5561 11.00000 0.05 0.32 Q5 1 0.7318 0.4499 0.5779 11.00000 0.05 0.29 ; _shelx_res_checksum 90990 _shelx_hkl_file ; 0 -1 0 -0.70 0.60 0 1 0 -0.10 1.10 0 -1 0 0.60 1.90 0 -2 0 5028.70 463.45 0 -2 0 5566.24 460.85 0 -3 0 -3.50 3.90 0 -3 0 2.40 3.40 0 -3 0 2.80 2.70 0 -4 0 1360.66 117.89 0 -4 0 1209.98 122.29 0 -5 0 0.10 4.50 0 -5 0 5.60 6.70 0 -6 0 335.87 44.10 0 -7 0 6.50 9.20 0 -7 0 -6.30 7.40 0 -8 0 569.94 55.29 0 -8 0 523.95 56.29 0 -9 0 19.50 19.10 0 -9 0 32.00 23.30 0 -10 0 432.16 47.10 0 -10 0 561.54 67.99 0 -10 0 481.85 81.09 0 -10 0 429.16 45.90 0 -11 0 25.70 40.40 0 -11 0 41.90 25.10 0 -11 0 8.70 5.20 0 11 0 2.50 3.60 0 -12 0 763.52 73.69 0 12 0 772.32 72.79 0 -13 0 -6.10 4.40 0 13 0 2.20 3.20 0 14 0 4.70 4.00 0 -14 0 6.50 3.90 0 0 1 0.90 1.70 0 0 -1 0.00 0.40 0 0 1 -1.50 2.20 0 0 -1 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0.10 6.30 0 -9 -6 1.60 3.80 0 9 -6 3.10 5.50 0 -9 -6 -31.10 42.30 0 -9 6 -4.60 3.00 0 -9 6 1.50 5.40 0 9 -6 1.40 2.80 0 10 -6 410.16 40.00 0 -10 6 576.84 101.69 0 -10 6 279.37 79.79 0 -10 6 435.56 45.50 0 -10 6 349.47 44.40 0 -10 -6 374.86 42.20 0 11 -6 -3.10 2.40 0 11 -6 -4.50 8.00 0 -11 -6 -0.30 3.20 0 -11 6 -6.10 4.30 0 12 -6 63.59 8.80 0 -12 -6 61.79 11.30 0 -13 -6 1.30 2.30 0 -13 6 0.60 3.90 0 13 -6 -3.00 2.40 0 0 -7 6.60 3.70 0 -1 -7 9.60 8.90 0 -1 -7 6.60 4.10 0 1 -7 1.80 3.20 0 -2 -7 481.15 46.90 0 2 7 429.86 48.20 0 2 -7 464.65 43.00 0 3 -7 4.00 3.30 0 -3 7 44.40 30.90 0 3 7 4.40 4.50 0 -4 -7 90.99 29.50 0 4 7 167.88 22.70 0 -4 7 250.37 57.19 0 -4 -7 171.28 22.80 0 -4 7 132.59 19.40 0 -5 -7 11.90 22.50 0 -5 7 2.20 3.70 0 5 -7 -1.00 4.10 0 -5 7 0.30 3.80 0 5 7 2.10 6.20 0 -5 -7 5.90 8.00 0 -5 -7 8.10 7.00 0 -6 -7 -5.70 8.60 0 -6 -7 0.60 5.60 0 -6 -7 2.70 22.20 0 -6 7 0.00 7.10 0 -6 7 1.40 2.70 0 -6 -7 3.70 5.80 0 6 -7 -3.00 3.70 0 -6 7 1.30 6.50 0 6 -7 2.10 3.20 0 -6 7 1.60 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41.40 9.40 6 -3 1 70.59 11.90 -6 -3 -1 66.99 10.60 -6 -3 -1 45.20 7.90 -6 -3 -1 50.49 15.00 6 -3 -1 40.20 6.60 -6 -3 1 57.39 7.50 -6 -3 1 47.30 8.90 -6 -3 1 50.39 15.90 6 -3 -1 50.69 14.10 -6 3 -1 51.99 8.80 6 -3 -1 28.60 11.40 6 -4 1 5.70 8.50 -6 4 1 5.20 3.80 -6 -4 -1 5.70 8.30 -6 -4 -1 4.90 5.30 -6 -4 -1 9.50 3.40 6 -4 1 -1.30 3.60 6 -4 1 7.60 2.90 6 -4 -1 4.80 5.10 -6 -4 1 2.60 8.60 -6 -4 1 8.80 3.60 6 -4 -1 9.70 7.70 -6 -4 1 8.60 4.70 6 4 1 1.20 2.50 -6 -5 -1 206.98 34.70 6 -5 1 196.58 20.90 6 -5 1 250.57 35.70 -6 -5 -1 183.58 31.70 6 -5 1 254.47 32.80 -6 -5 -1 212.98 27.80 -6 -5 1 212.38 26.50 6 -5 -1 232.78 34.90 -6 -5 1 226.88 30.00 -6 -5 1 200.28 35.80 6 -5 -1 216.88 30.10 -6 -5 1 176.48 24.90 6 -6 1 108.59 24.50 6 -6 1 172.38 28.60 -6 -6 -1 132.59 22.40 -6 -6 -1 88.69 26.00 -6 -6 1 126.99 28.90 -6 -6 1 142.79 21.40 6 -6 -1 124.19 28.90 -6 -6 1 171.78 25.70 6 -6 -1 123.49 22.40 6 -7 1 696.43 64.69 6 -7 1 646.74 78.69 6 -7 1 717.83 80.19 -6 -7 -1 517.75 73.09 6 -7 1 624.14 61.69 -6 -7 -1 689.13 76.39 -6 -7 -1 621.94 69.39 6 -7 -1 622.34 72.89 -6 -7 1 562.44 79.99 -6 -7 1 721.43 76.59 6 -7 -1 635.14 81.29 -6 -7 1 649.43 68.49 6 -7 -1 599.84 60.79 6 8 -1 66.99 12.20 -6 -8 -1 56.39 12.50 -6 -8 -1 105.29 30.40 -6 -8 -1 59.99 15.80 -6 -8 -1 67.09 24.60 6 -8 1 83.69 11.70 6 -8 1 83.09 24.80 -6 -8 -1 71.19 13.20 -6 8 1 48.30 9.90 6 8 -1 96.29 16.70 6 -8 1 60.59 25.80 6 -8 -1 63.89 26.70 -6 -8 1 80.49 15.80 -6 8 -1 74.29 10.60 6 -8 -1 42.50 18.20 6 -8 -1 74.59 11.50 -6 -8 1 64.69 13.60 -6 -8 1 76.19 23.50 6 8 1 69.09 11.40 -6 -8 1 79.29 32.80 6 8 1 70.59 15.30 6 -8 -1 69.49 12.10 -6 -9 -1 1.20 4.90 6 9 -1 10.10 3.60 -6 -9 -1 23.00 16.30 6 -9 1 13.70 7.30 6 -9 1 13.90 36.60 6 -9 1 -2.50 3.20 -6 9 1 8.80 4.90 6 9 -1 3.30 6.80 -6 -9 -1 -11.30 22.80 6 9 1 -0.70 4.70 6 9 1 -1.30 6.80 -6 -9 1 -9.70 8.00 -6 -9 1 -3.10 25.10 -6 9 -1 1.10 3.20 -6 -9 1 0.40 5.80 6 -9 -1 -2.10 2.50 6 -9 -1 1.10 5.00 6 -10 1 34.70 8.70 6 10 -1 29.30 7.40 -6 -10 -1 74.09 52.39 6 -10 1 13.40 25.70 -6 -10 -1 22.00 8.30 6 -10 1 -20.60 23.20 -6 -10 -1 8.40 8.90 6 -10 1 33.40 8.50 -6 -10 -1 61.29 25.30 -6 10 1 24.20 6.30 6 10 -1 31.20 9.60 6 10 1 45.80 11.90 6 -10 -1 37.20 8.90 -6 -10 1 76.99 38.20 -6 -10 1 1.80 34.90 -6 -10 1 21.20 9.90 6 -10 -1 35.10 31.90 -6 -10 1 37.30 10.30 6 10 1 38.60 9.10 -6 10 -1 27.80 6.20 6 -10 -1 27.00 7.30 -6 -11 -1 32.10 9.40 -6 -11 -1 42.50 12.40 6 11 -1 52.49 10.80 -6 11 1 54.79 10.30 6 -11 1 27.30 9.10 6 -11 -1 48.00 10.80 -6 11 -1 37.80 8.60 -6 -11 1 76.29 43.70 -6 -11 1 42.70 11.40 6 11 1 41.20 11.80 6 -12 1 33.80 7.00 -6 12 1 17.90 5.20 6 -12 1 8.30 5.70 6 12 -1 11.20 4.90 -6 -12 -1 14.60 6.20 -6 -12 1 20.40 7.50 -6 -12 1 17.70 7.10 6 -12 -1 22.90 5.80 -6 12 -1 19.60 5.70 6 13 -1 -1.60 2.60 -6 13 1 3.20 2.90 -6 -13 -1 -3.40 3.60 6 -13 -1 2.30 3.30 -6 -13 1 2.90 5.00 -6 13 -1 3.70 2.70 6 13 1 1.90 2.40 -6 -14 -1 3.70 3.10 -6 14 1 -0.60 2.20 6 14 -1 -0.50 2.00 -6 14 -1 2.10 2.20 6 0 2 9.80 3.10 6 0 2 10.40 2.70 6 0 -2 7.90 7.40 -6 0 2 31.90 13.20 6 0 2 21.40 9.20 -6 -1 -2 2016.30 170.38 6 -1 2 1825.52 168.08 6 -1 2 1677.93 168.78 -6 -1 -2 2222.68 179.48 -6 1 2 1981.00 179.18 6 -1 2 1946.91 178.38 -6 -1 2 1825.72 167.08 6 1 2 1846.02 167.98 -6 -1 2 1925.41 180.48 6 -2 2 387.26 40.70 -6 -2 -2 392.56 47.60 6 -2 2 455.05 49.00 -6 -2 -2 399.06 40.60 6 -2 2 412.16 38.00 -6 -2 2 367.76 37.60 6 -2 -2 327.67 45.60 6 2 2 451.65 38.00 6 -3 2 1285.17 117.59 -6 -3 -2 998.70 105.19 -6 -3 -2 1163.98 107.69 6 -3 2 1209.88 109.39 -6 -3 -2 1354.66 115.69 -6 -3 2 1032.50 117.79 -6 -3 2 1096.39 104.29 6 -4 2 105.49 28.00 6 -4 2 108.69 18.80 -6 -4 -2 82.69 19.50 6 -4 2 130.29 13.60 -6 -4 -2 112.89 17.50 -6 -4 -2 122.39 19.30 6 4 2 145.39 14.00 -6 -4 2 91.99 28.10 6 -4 -2 73.79 23.60 6 -5 2 269.37 40.60 6 -5 2 258.37 34.30 -6 -5 -2 209.88 33.70 -6 5 2 237.68 25.30 -6 -5 -2 266.67 32.30 -6 -5 -2 279.57 35.00 6 -5 -2 194.48 36.10 -6 -5 2 217.18 40.80 6 5 2 247.28 24.20 -6 -5 2 230.68 28.40 -6 -6 -2 168.18 27.30 6 -6 2 207.18 31.90 6 -6 2 243.18 39.50 6 -6 2 194.68 20.00 -6 -6 -2 188.08 31.50 -6 -6 -2 209.78 32.80 -6 -6 2 187.48 31.20 -6 -6 2 182.48 39.00 -6 -6 2 180.88 25.90 6 -6 -2 200.28 35.80 -6 -7 -2 7.10 10.70 -6 -7 -2 -1.50 6.80 -6 -7 -2 -3.70 7.80 6 -7 2 -14.40 12.80 6 7 -2 5.60 3.70 6 -7 2 7.20 14.50 6 -7 2 6.40 4.30 6 7 -2 -1.10 5.80 -6 -7 -2 -20.00 15.20 -6 -7 -2 4.00 5.20 -6 -7 2 11.00 8.40 6 -7 -2 5.80 9.80 6 -7 -2 3.30 3.20 -6 -7 2 1.80 18.60 -6 7 -2 3.20 3.50 -6 -8 -2 4.80 22.70 -6 -8 -2 -4.50 6.30 6 -8 2 9.90 15.90 6 -8 2 -1.00 15.20 6 8 -2 -1.50 5.30 6 8 -2 10.40 4.40 6 -8 2 2.00 4.90 6 -8 2 0.20 5.20 -6 -8 -2 -8.60 10.60 -6 8 -2 -0.50 3.10 -6 -8 2 6.80 6.80 -6 -8 2 10.00 6.50 6 -8 -2 6.30 5.60 6 -8 -2 4.40 3.70 -6 -8 2 13.30 24.00 6 -8 -2 22.20 18.30 -6 -9 -2 334.57 46.00 -6 9 2 233.38 27.70 6 -9 2 324.37 30.40 6 -9 2 296.07 56.69 6 9 -2 307.57 34.40 6 -9 2 306.07 31.10 -6 -9 -2 247.28 31.50 6 9 -2 242.48 39.80 -6 -9 -2 246.08 29.20 6 -9 -2 208.18 27.10 -6 -9 2 190.78 45.30 -6 -9 2 263.47 32.60 6 -9 -2 270.97 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43.50 -10 9 -4 70.69 9.90 10 -9 -4 85.49 12.10 -10 -9 4 59.79 17.00 -10 -9 4 31.50 57.29 -10 -9 4 52.79 48.90 10 10 -4 3.20 3.60 10 -10 4 -24.50 69.19 -10 10 4 -2.90 5.60 10 -10 4 -2.70 5.60 -10 -10 -4 10.60 7.30 10 10 4 0.40 4.60 -10 -10 4 -5.10 5.00 10 -10 -4 -1.90 3.20 -10 10 -4 1.90 3.30 -10 -10 4 52.19 77.79 10 -11 4 21.70 5.70 -10 -11 -4 19.10 7.40 10 11 -4 19.90 6.10 -10 11 4 21.90 6.80 10 11 4 17.60 6.70 10 -11 -4 37.70 8.00 -10 11 -4 28.40 5.80 -10 -11 4 16.80 8.70 10 12 -4 29.90 8.40 -10 -12 -4 39.60 10.00 -10 12 4 26.90 6.90 10 -12 4 36.50 8.00 -10 -12 4 23.40 13.50 -10 12 -4 31.80 6.60 10 12 4 40.80 7.80 10 13 -4 -0.20 2.20 -10 13 4 1.40 2.70 -10 -13 -4 0.20 3.50 10 13 4 2.30 2.90 -10 -13 4 3.50 4.80 -10 13 -4 4.10 2.00 10 0 5 0.60 2.40 -10 0 -5 2.50 4.10 10 -1 5 79.69 28.60 10 -1 5 109.19 17.70 -10 -1 -5 128.09 28.30 -10 -1 -5 108.29 19.50 -10 -1 -5 129.09 53.59 10 -1 5 142.59 17.60 -10 1 -5 146.49 19.20 10 1 5 126.29 16.70 -10 -1 5 65.29 40.80 10 -2 5 391.16 37.80 10 -2 5 340.87 39.10 -10 -2 -5 387.26 52.59 -10 -2 -5 313.87 60.19 10 -2 5 291.77 52.09 -10 -2 5 266.37 57.69 10 2 5 357.96 36.90 10 -3 5 97.09 14.20 -10 -3 -5 82.99 39.30 10 -3 5 53.19 24.50 -10 -3 -5 73.69 18.30 -10 -3 -5 92.89 26.90 10 -3 5 82.09 19.70 -10 -3 5 110.39 39.10 10 3 5 105.29 14.20 10 -4 5 638.94 56.79 10 -4 5 530.25 80.09 -10 -4 -5 529.05 64.59 10 -4 5 481.75 52.69 10 -4 5 596.74 64.09 -10 -4 -5 513.65 72.99 10 4 -5 607.94 57.29 -10 -4 -5 537.05 73.29 10 -4 5 554.84 51.69 -10 -4 5 556.44 56.39 -10 -4 5 544.25 54.19 10 -4 -5 600.64 58.69 -10 -5 -5 44.40 15.20 10 -5 5 68.29 8.80 -10 -5 -5 44.80 26.00 10 5 -5 58.19 10.30 10 5 -5 66.19 13.50 10 -5 5 62.69 12.50 10 -5 5 51.79 9.20 -10 -5 -5 75.49 23.70 -10 -5 -5 61.69 18.90 10 -5 5 28.10 31.70 10 -5 5 48.70 17.70 -10 -5 -5 39.40 12.40 10 5 -5 46.30 12.40 -10 -5 -5 42.60 10.40 -10 -5 5 38.00 13.60 10 -5 -5 60.59 10.40 -10 -5 5 44.00 9.90 10 5 5 67.29 13.20 -10 -5 5 64.19 12.70 10 -5 -5 39.80 14.20 -10 5 -5 71.69 8.30 -10 -5 5 28.50 33.40 -10 -6 -5 101.09 37.80 10 -6 5 90.99 9.40 10 -6 5 86.99 16.70 10 -6 5 69.69 35.10 10 6 -5 60.29 15.00 10 -6 5 71.19 10.80 10 -6 5 94.89 24.80 10 6 -5 55.69 11.10 -10 -6 -5 54.99 15.20 10 -6 5 73.39 14.80 -10 -6 -5 62.39 20.90 -10 -6 -5 102.79 18.00 10 6 -5 81.39 18.70 -10 -6 -5 52.39 12.20 -10 -6 5 48.40 49.00 10 -6 -5 103.69 16.50 -10 -6 5 63.09 11.00 -10 -6 5 69.19 13.30 -10 -6 5 96.09 20.20 -10 6 -5 82.89 10.10 10 6 5 74.79 15.90 -10 -7 -5 16.60 9.50 10 -7 5 -29.60 26.00 10 -7 5 14.00 5.00 10 -7 5 9.50 6.80 10 -7 5 7.50 18.50 -10 -7 -5 10.00 8.00 10 7 -5 9.50 5.00 10 7 -5 9.10 6.80 10 7 -5 8.10 13.60 -10 -7 -5 8.20 15.40 -10 -7 5 22.50 10.70 10 -7 -5 4.20 7.20 10 -7 -5 10.80 5.40 -10 -7 5 9.90 5.90 -10 -7 5 28.00 41.10 -10 7 -5 18.10 5.00 10 -7 -5 1.40 28.00 -10 -8 -5 46.00 10.90 -10 -8 -5 38.70 11.50 10 8 -5 37.90 10.80 10 -8 5 40.00 7.30 10 -8 5 3.70 24.00 10 8 -5 31.80 12.50 10 -8 5 -37.20 35.90 10 -8 5 28.30 8.10 10 -8 -5 14.60 9.80 10 -8 -5 32.30 8.00 -10 -8 5 30.90 11.20 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21.50 10 11 -7 28.80 9.70 10 -11 7 41.90 14.00 10 -11 -7 45.20 7.80 10 11 7 30.30 9.00 -10 -12 -7 8.10 5.10 -10 -12 7 13.40 8.60 10 0 8 104.09 13.70 -10 0 8 127.99 15.60 10 0 8 82.99 13.70 -10 0 -8 122.79 16.00 10 0 -8 91.59 15.40 10 0 8 140.99 21.00 -10 0 -8 101.99 21.30 -10 0 8 93.19 17.20 10 0 -8 134.09 20.10 10 -1 8 32.60 14.70 -10 -1 -8 24.70 9.80 10 1 -8 -0.80 8.00 -10 -1 -8 38.60 20.40 10 -1 8 23.60 8.00 10 -1 8 21.20 5.80 -10 -1 -8 32.80 13.80 10 1 8 19.40 8.30 -10 1 -8 11.70 8.70 -10 -1 8 15.40 9.80 10 -1 -8 9.00 7.10 10 -1 -8 17.60 6.30 10 1 8 10.10 6.70 10 -2 8 209.78 28.80 -10 -2 -8 215.78 25.50 -10 -2 -8 261.37 30.60 -10 -2 -8 208.28 39.90 10 2 -8 240.48 33.80 10 -2 8 245.78 24.20 10 -2 8 193.88 24.20 10 2 -8 207.08 26.90 10 -2 8 216.18 33.50 -10 -2 -8 208.08 33.90 -10 -2 8 226.38 25.80 -10 2 -8 211.08 30.20 10 2 8 235.98 30.70 -10 -2 8 224.28 27.30 10 -2 -8 246.98 29.60 -10 -3 -8 10.10 12.20 -10 -3 -8 9.00 8.00 10 -3 8 12.30 17.30 -10 -3 -8 23.80 6.70 10 -3 8 31.50 7.00 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2.50 4.10 12 5 -5 55.79 13.10 12 -5 5 64.39 7.40 12 -5 5 58.49 9.10 12 -5 5 45.40 12.40 -12 -5 -5 40.00 11.80 12 -5 5 29.20 31.30 -12 -5 -5 56.09 20.60 12 -5 5 35.70 19.20 12 5 -5 60.79 9.80 -12 -5 -5 40.70 23.20 -12 -5 -5 27.50 47.00 12 5 -5 51.69 13.70 -12 -5 -5 50.99 11.00 12 -5 5 46.40 9.90 12 -5 -5 30.70 22.10 -12 -5 5 42.20 10.00 12 5 5 37.60 12.30 12 -5 -5 41.20 8.70 12 -5 -5 55.59 14.80 -12 -5 5 167.58 54.09 -12 -5 5 61.39 15.00 12 5 5 34.10 12.60 -12 -5 5 63.89 10.30 12 5 5 58.09 9.30 12 -6 5 -41.80 36.00 12 6 -5 2.40 3.90 -12 -6 -5 8.40 6.20 12 -6 5 9.10 3.40 -12 -6 -5 30.10 20.90 12 -6 5 12.20 12.80 12 -6 5 13.70 8.10 12 6 -5 11.80 7.70 -12 -6 -5 8.10 8.40 -12 -6 -5 18.70 16.00 -12 -6 -5 5.90 8.00 12 -6 5 16.70 33.30 -12 -6 -5 3.10 36.40 12 6 -5 17.70 7.50 12 -6 5 4.30 3.50 -12 -6 5 -1.10 8.40 -12 -6 5 8.20 4.70 12 6 5 8.10 5.30 12 -6 -5 40.80 29.50 12 -6 -5 11.70 4.20 -12 -6 5 5.60 4.80 12 -6 -5 3.20 6.80 -12 6 -5 6.30 3.00 -12 -6 5 31.20 49.00 12 -6 -5 8.90 6.10 -12 -7 -5 240.28 33.60 12 7 -5 287.37 35.10 -12 -7 -5 222.58 31.40 12 7 -5 258.07 29.10 12 -7 5 220.48 49.40 12 -7 5 259.37 107.19 12 -7 5 275.57 31.40 -12 -7 -5 293.67 47.70 12 7 -5 281.07 37.20 -12 -7 5 334.67 150.88 12 7 5 255.27 28.20 12 -7 -5 271.47 34.00 -12 -7 5 272.47 37.20 -12 7 -5 303.07 27.20 -12 -7 5 258.37 31.70 12 8 -5 325.17 41.80 -12 8 5 303.17 34.20 12 -8 5 236.98 60.59 -12 -8 -5 349.07 41.40 -12 -8 -5 452.65 61.89 -12 -8 -5 382.06 38.90 12 -8 5 316.57 38.00 12 8 -5 359.76 43.00 -12 -8 5 396.76 45.00 -12 -8 5 217.68 99.59 12 -8 -5 343.47 41.00 -12 -8 5 308.57 37.50 -12 8 -5 381.46 34.00 12 8 5 342.07 35.20 12 9 -5 25.70 10.70 -12 -9 -5 22.40 9.20 -12 9 5 5.50 6.50 12 -9 5 27.80 8.70 12 -9 5 30.70 44.90 12 9 -5 32.20 12.00 12 9 -5 24.70 7.30 -12 -9 5 80.69 130.49 12 9 5 29.30 7.00 -12 -9 5 22.50 7.30 12 -9 -5 16.60 9.20 -12 9 -5 16.30 5.10 -12 -9 5 63.09 21.30 12 10 -5 4.60 3.90 12 -10 5 12.20 4.50 -12 -10 5 16.00 7.90 -12 10 -5 5.60 3.20 12 10 5 7.60 5.40 12 -10 -5 10.10 5.00 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36.10 11.50 -15 -5 -4 49.80 11.30 15 -5 4 14.60 27.50 15 -5 4 29.20 9.80 15 -5 4 17.90 11.90 15 -5 4 34.80 5.70 -15 -5 -4 54.89 23.50 15 5 -4 29.60 7.20 -15 -5 4 36.20 7.60 15 5 4 20.70 8.60 15 -5 -4 44.30 9.10 -15 -5 4 98.09 54.29 -15 5 -4 41.80 6.60 15 5 4 35.20 14.30 -15 -5 4 47.80 11.20 -15 -5 4 34.00 12.00 15 5 4 40.50 7.00 15 -5 -4 27.80 23.10 -15 6 4 1.30 5.80 -15 -6 -4 35.40 23.60 15 6 -4 5.20 8.10 -15 -6 -4 34.40 16.30 15 -6 4 -4.20 4.30 15 -6 4 2.70 4.10 15 -6 4 -24.90 38.10 -15 -6 -4 3.10 6.10 -15 -6 -4 12.30 8.00 15 6 -4 -1.40 3.30 -15 -6 4 5.70 5.50 15 6 4 -2.30 8.50 -15 -6 4 21.10 9.40 -15 6 -4 3.90 2.60 15 6 4 5.70 4.10 15 -6 -4 18.60 31.40 -15 -6 4 15.00 50.99 15 -6 -4 5.30 4.60 -15 -7 -4 53.89 14.70 15 7 -4 43.10 11.80 15 -7 4 32.40 9.90 15 7 -4 55.49 9.80 -15 7 4 40.30 7.90 -15 -7 -4 20.70 33.40 -15 -7 -4 18.00 26.40 15 -7 4 24.00 41.50 -15 -7 4 -21.40 83.39 15 -7 -4 33.60 12.00 15 -7 -4 42.30 8.00 -15 7 -4 44.20 7.40 15 7 4 43.50 11.40 15 7 4 56.49 9.30 15 -7 -4 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15.90 5.40 -15 -9 9 22.10 8.70 15 -9 -9 15.60 6.90 15 -10 9 6.80 6.60 15 10 -9 7.10 4.00 -15 -10 -9 4.60 3.80 -15 10 -9 3.90 4.20 -15 -10 9 12.70 5.60 15 0 10 6.30 5.40 -15 0 -10 4.30 7.70 15 0 -10 8.00 5.10 -15 0 -10 -8.70 21.20 -15 0 10 2.00 4.30 15 0 10 1.10 2.90 15 0 -10 2.30 6.20 -15 0 -10 12.70 38.70 -15 0 10 5.50 5.50 15 -1 10 2.40 2.70 -15 -1 -10 14.70 17.00 15 -1 10 1.60 3.20 -15 1 10 -0.30 3.70 -15 1 10 9.60 6.90 -15 -1 -10 4.10 32.40 -15 -1 -10 50.39 28.40 -15 -1 -10 -8.10 6.80 -15 1 -10 7.00 41.60 -15 1 -10 7.20 5.70 15 1 10 1.90 2.90 -15 -1 10 8.80 5.10 15 -1 -10 8.20 4.90 -15 1 -10 5.30 23.00 15 1 10 -1.30 4.00 -15 -2 -10 26.30 8.30 15 2 -10 25.40 8.50 -15 -2 -10 38.00 26.80 -15 2 10 11.30 6.40 -15 2 10 27.50 8.50 -15 -2 -10 31.30 12.90 -15 -2 -10 62.29 33.30 15 -2 10 23.30 5.30 15 -2 10 23.80 6.30 15 2 -10 20.60 8.60 -15 -2 -10 34.80 9.80 15 -2 -10 23.30 6.90 15 -2 -10 9.50 7.60 -15 -2 10 17.00 7.60 15 2 10 12.50 7.10 -15 2 -10 22.40 8.90 -15 2 -10 -10.70 39.10 15 2 10 12.90 4.80 -15 2 -10 -11.70 26.40 -15 -2 10 23.60 6.80 15 3 -10 40.00 11.10 -15 -3 -10 17.20 12.20 -15 3 10 43.60 9.40 15 3 -10 37.70 10.60 -15 3 10 30.50 7.70 15 -3 10 39.10 8.20 15 -3 10 44.10 6.90 15 3 10 36.60 7.20 15 -3 -10 36.10 11.90 15 3 10 19.60 9.10 -15 -3 10 35.30 8.70 -15 3 -10 94.69 41.30 -15 -3 10 21.50 8.00 -15 4 10 3.70 4.80 15 4 -10 4.00 5.30 15 -4 10 -6.10 9.50 -15 -4 -10 15.30 9.00 15 -4 10 2.50 2.70 -15 -4 -10 9.30 7.00 15 -4 10 6.10 2.70 -15 -4 10 7.70 4.30 15 -4 -10 0.70 6.30 -15 -4 10 4.00 5.60 -15 4 -10 -5.90 59.09 15 4 10 12.80 6.20 -15 4 -10 5.90 5.30 15 4 10 -0.20 3.40 -15 -5 -10 17.80 7.80 15 5 -10 22.40 8.90 15 -5 10 17.40 5.10 15 -5 10 16.60 3.70 -15 5 10 16.60 6.00 15 -5 10 15.30 9.60 -15 -5 -10 29.20 9.40 -15 -5 10 9.40 4.20 -15 -5 10 4.00 15.80 -15 -5 10 14.60 6.80 -15 5 -10 28.50 8.90 15 5 10 20.40 5.60 15 -5 -10 19.20 8.60 -15 -6 -10 6.60 6.00 15 -6 10 13.70 4.50 15 6 -10 9.80 6.00 -15 6 10 22.10 6.20 15 -6 10 9.90 2.90 -15 -6 -10 14.00 7.20 15 -6 10 9.80 7.80 -15 -6 10 14.60 6.20 15 6 10 -2.50 4.50 -15 -6 10 5.20 3.30 -15 6 -10 9.90 5.10 15 -6 -10 5.10 4.90 -15 -7 -10 144.19 18.80 15 7 -10 161.58 21.60 15 -7 10 154.68 16.60 15 -7 10 145.99 19.00 -15 -7 -10 135.99 18.90 15 7 10 147.39 17.00 -15 -7 10 145.29 18.60 -15 -7 10 134.29 24.90 -15 7 -10 125.79 17.90 15 -7 -10 105.29 17.80 15 8 -10 4.80 3.90 15 -8 10 5.80 5.50 15 -8 10 3.20 2.50 -15 -8 -10 4.20 4.30 15 8 10 6.60 4.30 15 -8 -10 1.00 3.00 -15 -8 10 -1.60 2.30 -15 8 -10 5.70 4.60 15 -9 10 4.00 4.90 -15 -9 -10 4.30 4.10 -15 -9 10 11.40 6.40 -15 -9 10 4.60 3.20 -15 9 -10 -0.60 4.00 15 -9 -10 6.40 4.50 -15 0 11 6.80 5.40 15 0 11 -2.00 4.30 -15 0 11 -5.00 3.10 -15 0 -11 -0.30 5.80 15 0 11 3.10 2.60 -15 0 -11 -62.29 42.20 15 0 -11 -6.00 3.50 15 0 -11 -1.10 5.10 15 1 -11 2.60 5.10 15 -1 11 -2.10 2.10 -15 -1 -11 -0.30 6.40 -15 -1 -11 -0.70 7.50 -15 1 11 -0.90 4.80 15 1 -11 1.50 5.10 15 1 11 -0.40 2.30 -15 1 -11 -3.30 44.70 -15 -1 11 0.90 2.90 -15 -1 11 1.40 5.00 -15 1 -11 2.10 6.50 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132.49 30.40 -16 -4 0 146.09 50.49 16 -5 0 9.40 7.60 16 5 0 1.50 5.40 -16 5 0 0.10 2.40 -16 -5 0 6.10 7.20 16 -5 0 -17.70 24.30 16 5 0 -2.00 3.00 16 -5 0 -4.70 3.90 -16 -5 0 -31.30 23.30 16 -6 0 4.10 4.00 -16 -6 0 -35.20 19.40 -16 -6 0 12.10 6.20 16 6 0 7.70 3.70 -16 6 0 -0.20 4.00 16 -6 0 -33.40 27.80 -16 -6 0 33.20 64.79 -16 -6 0 -10.90 11.00 -16 7 0 1.60 2.40 -16 -7 0 39.50 53.59 16 7 0 -1.10 2.60 -16 -7 0 -0.70 7.10 16 -7 0 6.20 3.70 -16 -7 0 -33.10 24.50 16 -7 0 -49.70 31.70 -16 -7 0 2.70 6.10 16 -8 0 37.90 8.10 -16 -8 0 50.19 43.50 -16 -8 0 20.30 9.70 16 -8 0 -28.40 52.09 -16 -8 0 51.29 51.29 -16 -8 0 44.00 12.20 -16 8 0 31.60 6.30 16 8 0 28.50 6.90 16 8 0 27.60 9.70 -16 -9 0 90.69 83.99 16 9 0 -0.20 5.50 -16 -9 0 10.90 7.00 -16 10 0 59.89 9.30 16 -10 0 79.39 10.10 -16 -10 0 75.29 15.80 -16 -10 0 59.29 13.80 16 10 0 70.29 10.70 -16 -11 0 -7.20 6.00 -16 -11 0 4.60 5.30 -16 11 0 2.10 2.30 16 11 0 5.70 4.80 16 11 0 0.20 2.70 -16 12 0 115.79 14.50 16 12 0 157.28 16.10 -16 -12 0 137.49 19.40 16 0 -1 2.20 5.10 -16 0 1 -2.70 3.20 -16 0 1 -6.00 4.50 16 0 -1 9.20 8.80 -16 0 1 19.50 30.10 -16 0 -1 3.60 8.10 16 0 1 -3.00 5.30 16 0 1 -1.70 3.30 -16 0 -1 17.50 24.60 16 0 -1 5.80 5.00 16 -1 1 11.70 5.20 -16 -1 -1 26.40 14.30 -16 -1 -1 6.10 6.10 -16 1 1 12.10 33.90 16 -1 1 6.20 3.00 16 1 -1 13.20 3.90 -16 -1 -1 2.50 25.40 -16 1 1 11.50 4.10 16 1 -1 9.30 8.60 -16 1 1 17.40 8.10 16 -1 1 14.10 8.10 16 1 -1 19.40 6.00 16 -1 -1 4.20 5.40 16 -1 -1 2.80 6.80 -16 1 -1 15.40 7.00 16 1 1 6.30 3.20 -16 -1 1 11.60 4.80 16 1 1 14.70 7.50 -16 1 -1 13.10 3.70 16 1 1 15.10 5.40 -16 -1 1 17.00 23.00 -16 -1 1 9.50 6.40 16 -1 -1 12.70 5.30 -16 1 -1 7.60 25.10 16 -2 1 78.99 10.70 -16 -2 -1 57.89 13.90 16 -2 1 59.89 15.10 -16 -2 -1 105.69 33.90 16 2 -1 74.79 13.20 -16 2 1 76.29 52.99 16 2 -1 63.29 9.20 16 -2 1 67.69 11.90 -16 2 1 92.69 10.40 16 -2 1 9.60 26.00 -16 -2 -1 92.59 17.70 16 -2 -1 27.20 24.50 16 2 1 49.30 11.80 -16 -2 1 66.19 14.80 16 2 1 63.19 9.10 16 2 1 71.39 12.00 -16 -2 1 66.79 16.50 -16 2 -1 90.59 10.10 16 -2 -1 55.19 15.10 -16 -2 1 69.19 11.00 16 -2 -1 71.69 10.80 16 -2 -1 50.59 11.80 -16 -2 1 -0.90 33.60 16 -3 1 131.99 18.00 16 -3 1 93.29 13.50 -16 -3 -1 158.78 47.20 16 3 -1 79.59 17.90 -16 -3 -1 108.69 17.30 16 3 -1 114.59 16.30 16 3 -1 97.39 12.50 -16 -3 1 66.19 40.50 -16 3 -1 117.09 12.00 16 -3 -1 79.79 12.40 16 3 1 108.39 15.60 -16 -3 1 81.49 18.70 16 3 1 75.99 16.80 -16 -3 1 83.79 18.10 -16 3 -1 84.59 43.50 16 3 1 107.09 12.20 16 -3 -1 103.09 14.50 -16 -3 1 63.39 12.90 16 4 -1 23.80 9.00 -16 -4 -1 17.60 7.80 -16 -4 -1 26.40 8.10 16 -4 1 12.80 5.40 16 4 -1 11.40 4.10 -16 -4 -1 8.70 26.00 -16 4 1 10.30 4.50 16 -4 1 -43.50 26.00 16 -4 1 16.00 7.50 16 4 -1 8.00 6.60 -16 -4 -1 46.80 14.40 16 -4 1 17.30 5.50 16 4 1 7.30 6.80 -16 -4 1 -11.20 11.70 16 4 1 6.20 3.50 -16 4 -1 9.00 4.20 -16 -4 1 17.60 35.10 16 4 1 5.30 7.10 -16 -4 1 33.20 10.60 16 -4 -1 17.90 5.30 16 -4 -1 15.10 8.30 -16 -4 1 -1.80 6.20 16 -4 -1 1.20 21.10 16 5 -1 54.89 13.90 16 -5 1 -9.40 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7.20 23 -3 4 0.20 5.70 23 3 -4 5.00 5.80 23 3 -4 7.70 5.80 -23 3 4 7.40 3.80 -23 -3 4 8.50 4.90 -23 -3 4 7.10 8.30 -23 -3 4 3.10 3.70 23 3 4 5.00 4.00 23 -3 -4 7.90 4.40 23 3 4 5.30 3.60 23 4 -4 2.50 5.10 23 4 -4 0.00 4.90 23 -4 4 5.10 4.00 -23 4 4 3.90 2.60 23 -4 4 4.90 5.00 23 4 4 4.50 3.70 -23 -4 4 8.00 5.10 -23 -4 4 10.50 7.80 23 4 4 -0.40 2.10 23 -4 -4 6.40 4.80 23 -5 4 3.50 3.20 -23 -5 -4 0.20 5.50 -23 -5 -4 4.30 4.90 -23 5 4 4.30 2.30 23 5 -4 -3.00 4.60 23 5 -4 -1.40 3.40 23 -5 4 -3.50 3.10 23 5 4 -6.90 3.60 23 -5 -4 4.00 4.30 23 5 4 0.60 2.10 -23 -5 4 18.00 13.60 -23 -5 4 0.30 3.50 23 -5 -4 2.30 3.50 -23 -5 4 3.70 7.20 -23 -6 -4 -4.10 5.80 -23 6 4 0.60 2.20 23 6 -4 -3.90 3.50 23 6 -4 0.20 5.20 -23 -6 -4 5.70 5.00 23 -6 4 -2.50 3.00 23 -6 4 -2.10 4.20 -23 -6 4 11.50 4.60 23 -6 -4 -2.10 3.50 23 6 4 2.80 4.20 23 6 4 -2.80 2.00 23 -6 -4 4.80 3.40 -23 -6 4 -3.30 6.40 23 7 -4 5.00 4.70 23 -7 4 19.30 5.40 -23 7 4 5.90 3.40 -23 -7 -4 15.00 7.10 -23 -7 -4 5.90 5.60 23 7 -4 18.10 7.60 -23 7 -4 29.70 10.00 -23 -7 4 9.70 6.80 23 7 4 10.80 5.50 23 7 4 11.90 4.10 23 -7 -4 14.20 6.30 -23 -8 -4 0.70 4.10 -23 8 4 -0.50 2.00 23 8 -4 2.80 3.70 23 8 -4 22.70 9.50 23 -8 4 1.90 2.20 23 -8 -4 -1.00 4.50 -23 8 -4 -3.30 10.30 23 8 4 2.00 2.60 -23 -8 4 0.10 4.40 23 8 4 5.00 5.60 23 -9 4 0.20 1.90 -23 9 4 4.10 2.20 -23 -9 -4 -2.60 3.20 23 9 4 -4.50 4.50 23 9 4 0.60 2.20 -23 -9 4 -3.00 4.00 23 0 5 -6.30 3.10 -23 0 -5 3.20 69.99 23 0 -5 -1.40 5.70 -23 0 5 -4.10 3.10 23 0 5 17.90 10.10 -23 0 -5 5.30 6.10 23 0 5 2.00 2.70 23 1 -5 1.60 5.70 23 1 -5 4.80 7.70 23 -1 5 17.30 7.40 -23 -1 -5 -17.80 85.39 23 -1 5 2.80 2.70 23 -1 5 2.60 3.90 23 1 -5 5.80 8.40 -23 -1 -5 6.60 9.20 -23 1 5 4.30 4.20 23 -1 -5 -5.60 3.80 23 -1 -5 7.90 6.80 23 1 5 5.00 4.50 -23 -1 5 2.20 5.50 23 1 5 0.10 2.90 -23 1 -5 6.30 8.60 23 1 5 6.30 13.60 -23 -1 5 2.00 3.30 -23 -1 5 18.60 11.50 23 -2 5 33.90 9.00 23 -2 5 36.90 5.90 -23 2 5 27.80 6.90 23 2 -5 28.80 9.20 23 -2 5 42.30 8.60 23 2 -5 37.00 9.90 -23 -2 -5 35.90 9.60 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63.89 10.30 23 6 -5 37.80 9.60 23 6 5 51.09 8.20 -23 -6 5 66.79 14.50 23 -6 -5 40.30 11.50 23 6 5 38.40 8.90 -23 -6 5 30.40 8.90 -23 7 5 1.30 2.00 23 -7 5 2.60 2.60 23 7 -5 -0.40 3.40 23 7 -5 1.00 4.80 -23 -7 -5 8.40 5.10 23 7 5 0.60 2.20 -23 7 -5 -8.00 8.50 23 7 5 11.70 5.70 23 -7 -5 2.70 3.40 -23 -7 5 0.30 5.50 -23 -7 5 8.00 9.90 -23 8 5 1.80 2.10 23 -8 5 6.50 3.00 -23 -8 -5 3.80 3.60 23 8 -5 10.40 5.80 -23 -8 5 3.80 4.80 23 -8 -5 1.90 3.00 23 8 5 -3.60 5.60 23 8 5 -0.90 2.10 -23 -9 -5 -3.60 3.70 -23 9 5 1.90 2.10 -23 -9 5 -3.90 4.20 23 9 5 1.40 2.00 23 0 6 20.40 12.90 23 0 -6 3.20 5.10 -23 0 6 -4.60 3.40 23 0 -6 6.80 5.60 -23 0 6 -2.20 2.00 23 0 6 -2.70 2.70 -23 0 -6 -3.90 4.50 23 -1 6 25.20 11.10 -23 1 6 13.00 4.60 -23 -1 -6 23.10 8.50 23 1 -6 7.70 7.60 23 1 -6 24.50 8.20 23 -1 6 18.60 6.30 23 -1 6 22.00 4.30 23 -1 -6 13.80 7.70 23 1 6 20.00 4.80 23 -1 -6 12.20 8.40 -23 -1 6 15.30 4.90 -23 -1 6 12.50 6.50 23 1 6 27.50 7.80 -23 -1 6 42.60 15.10 -23 1 -6 15.60 7.50 23 2 -6 131.69 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-1 3 8.60 3.50 -30 1 3 5.20 3.10 -30 -1 3 20.90 7.00 30 1 3 6.50 3.50 -30 1 -3 8.00 4.00 30 -1 -3 3.90 3.40 30 -1 -3 9.50 4.50 -30 -1 3 6.70 3.80 30 1 3 5.60 6.50 30 2 -3 12.70 3.60 30 -2 3 7.10 4.50 -30 -2 -3 8.80 4.00 -30 2 3 7.60 3.60 30 2 3 11.60 4.00 30 -2 -3 3.00 3.50 -30 2 -3 10.90 5.50 -30 -2 3 26.20 7.40 30 -2 -3 9.00 3.90 30 -3 3 1.50 3.20 -30 -3 -3 3.90 3.10 30 3 -3 12.20 4.40 -30 3 3 1.90 3.10 -30 -3 -3 5.30 4.10 -30 3 -3 -0.30 3.90 30 -3 -3 1.80 3.70 -30 -3 3 2.00 4.60 30 3 3 4.30 3.80 -30 0 4 2.40 2.60 30 0 4 -0.70 2.80 30 0 -4 0.80 3.40 30 0 4 -3.00 8.10 -30 0 -4 -4.10 3.30 30 -1 4 -2.80 2.60 30 1 -4 0.20 2.50 -30 1 4 -1.70 1.90 -30 -1 -4 0.60 2.80 30 -1 -4 -3.80 2.20 30 1 4 -3.50 2.70 -30 1 -4 1.70 3.60 30 -1 -4 -0.50 2.30 -30 -1 4 -2.70 2.20 -30 2 4 0.30 2.20 -30 -2 -4 -0.80 2.90 30 2 -4 3.40 3.50 -30 -2 -4 6.10 4.20 30 -2 4 3.50 3.30 30 -2 -4 0.30 2.30 -30 2 -4 5.00 3.50 -30 -2 4 2.80 2.40 30 -2 -4 -1.50 2.30 30 3 4 2.10 3.30 -30 0 -5 1.70 3.20 30 0 -5 -0.70 2.90 30 0 5 -1.70 2.10 -30 0 5 1.50 1.90 30 1 -5 7.50 3.20 -30 -1 -5 9.60 3.90 30 -1 5 5.60 3.20 -30 -1 -5 6.30 3.40 -30 -1 5 6.90 2.80 -30 1 -5 9.20 3.60 30 -1 -5 15.60 3.80 30 1 5 10.10 3.60 -31 0 0 -6.10 3.70 31 0 0 -3.50 3.10 31 0 0 1.10 3.30 31 -1 0 8.70 6.10 -31 -1 0 14.70 5.50 -31 1 0 12.80 6.00 31 1 0 19.00 5.80 31 -1 0 11.30 4.40 31 2 0 -5.50 3.60 31 -2 0 3.20 2.70 31 -2 0 -3.70 2.90 -31 -2 0 2.80 4.30 -31 -2 0 3.60 3.00 -31 2 0 0.40 2.30 -31 0 1 -4.70 4.40 31 0 1 0.10 3.80 31 0 1 0.30 4.20 -31 0 1 -1.50 2.70 31 0 -1 4.40 3.20 -31 0 -1 -4.10 4.10 31 -1 1 2.60 2.80 -31 1 1 0.30 1.90 31 1 -1 -1.30 3.50 -31 -1 -1 3.40 3.40 31 -1 1 4.40 3.80 31 -1 -1 -1.30 2.60 -31 -1 1 3.40 5.70 31 -1 -1 4.30 5.00 31 1 1 -2.60 4.80 -31 1 -1 4.30 4.60 31 2 -1 3.00 4.00 -31 -2 -1 1.10 3.80 -31 2 1 -2.10 1.90 -31 -2 -1 -1.90 2.80 31 -2 1 -4.00 3.20 -31 2 -1 6.20 7.10 -31 -2 1 4.40 4.30 31 -2 -1 -1.50 2.20 -31 -2 1 -5.20 3.50 31 -2 -1 -2.40 2.60 31 2 1 -1.50 3.00 31 2 1 -2.40 7.10 -31 0 2 10.70 9.40 31 0 2 26.30 5.50 -31 0 -2 32.60 7.10 -31 0 2 18.10 3.80 31 0 -2 20.50 5.90 -31 1 2 3.20 2.40 -31 -1 -2 2.10 3.90 31 -1 2 4.30 4.20 31 1 -2 3.70 3.70 -31 1 -2 7.10 4.10 31 1 2 11.70 7.00 31 1 2 0.90 2.90 -31 -1 2 -2.60 5.40 31 -1 -2 5.20 3.00 31 -1 -2 0.90 3.30 -31 2 2 -0.30 2.10 -31 -2 -2 0.80 2.50 31 2 2 -0.80 2.50 -31 0 3 -1.50 1.90 -31 0 -3 -2.20 3.30 31 0 -3 1.30 3.70 31 1 3 7.30 3.30 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 93390 ####################################################################### # # This file contains crystal structure data downloaded from the # Cambridge Structural Database (CSD) hosted by the Cambridge # Crystallographic Data Centre (CCDC). # # Full information about CCDC data access policies and citation # guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 # # Audit and citation data items may have been added by the CCDC. # Please retain this information to preserve the provenance of # this file and to allow appropriate attribution of the data. # ####################################################################### data_zzy1062 _database_code_depnum_ccdc_archive 'CCDC 2071230' loop_ _audit_author_name _audit_author_address 'Qilin Wang' ;Henan University China ; _audit_update_record ; 2021-03-18 deposited with the CCDC. 2021-11-08 downloaded from the CCDC. ; _audit_creation_date 2019-12-15 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _shelx_SHELXL_version_number 2014/7 _chemical_name_common ? _chemical_name_systematic ? _chemical_formula_moiety 'C26 H23 N3 O5' _chemical_formula_sum 'C26 H23 N3 O5' _chemical_formula_weight 457.47 _chemical_melting_point ? _chemical_oxdiff_formula C40H40O2N4 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_H-M_alt 'P 1 21/n 1' _space_group_name_Hall '-P 2yn' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.6642(4) _cell_length_b 18.5733(7) _cell_length_c 13.4479(6) _cell_angle_alpha 90 _cell_angle_beta 110.324(4) _cell_angle_gamma 90 _cell_volume 2263.57(17) _cell_formula_units_Z 4 _cell_measurement_reflns_used 1769 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 58.1690 _cell_measurement_theta_min 4.2220 _shelx_estimated_absorpt_T_max 0.970 _shelx_estimated_absorpt_T_min 0.892 _exptl_absorpt_coefficient_mu 0.776 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.85403 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_special_details ? _exptl_crystal_colour yellow _exptl_crystal_colour_primary yellow _exptl_crystal_density_diffrn 1.342 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description prism _exptl_crystal_F_000 960 _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.04 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0255 _diffrn_reflns_av_unetI/netI 0.0376 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 1.000 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_number 9067 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 1.000 _diffrn_reflns_theta_full 67.073 _diffrn_reflns_theta_max 67.073 _diffrn_reflns_theta_min 4.238 _diffrn_ambient_temperature 293(2) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 16.2312 _diffrn_detector_type Eos _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames #-------------------------------------------------------------------------- 1 \w -47.00 31.00 0.50 8.50 -- -33.50 57.00 0.00 156 2 \w -32.00 64.00 0.50 8.50 -- 36.47 -77.00 150.00 192 3 \w -14.00 18.00 0.50 8.50 -- 36.47 -57.00 0.00 64 4 \w 58.00 97.00 0.50 8.50 -- 36.47 178.00 -90.00 78 5 \w 14.00 72.00 0.50 8.50 -- 36.47 37.00 -30.00 116 6 \w 57.00 110.00 0.50 8.50 -- 36.47 178.00 0.00 106 7 \w 37.00 78.00 0.50 8.50 -- 36.47 57.00-180.00 82 8 \w -32.00 27.00 0.50 8.50 -- 36.47 -77.00-150.00 118 9 \w 38.00 63.00 0.50 8.50 -- 36.47 -77.00-150.00 50 10 \w 40.00 78.00 0.50 35.00 -- 108.00 -94.00 -90.00 76 11 \w 82.00 176.00 0.50 35.00 -- 108.00 30.00-150.00 188 12 \w 50.00 112.00 0.50 35.00 -- 108.00-111.00-150.00 124 13 \w 48.00 129.00 0.50 35.00 -- 108.00 -77.00 -90.00 162 14 \w 101.00 130.00 0.50 35.00 -- 108.00 111.00-120.00 58 15 \w 63.00 131.00 0.50 35.00 -- 108.00 -30.00 150.00 136 16 \w 106.00 171.00 0.50 35.00 -- 108.00 61.00 -60.00 130 17 \w 79.00 144.00 0.50 35.00 -- 108.00 178.00-150.00 130 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'Xcalibur, Eos, Gemini' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 -0.0416056000 _diffrn_orient_matrix_UB_12 0.0756337000 _diffrn_orient_matrix_UB_13 0.0273016000 _diffrn_orient_matrix_UB_21 0.1399874000 _diffrn_orient_matrix_UB_22 0.0311090000 _diffrn_orient_matrix_UB_23 -0.0138731000 _diffrn_orient_matrix_UB_31 -0.0870440000 _diffrn_orient_matrix_UB_32 0.0138644000 _diffrn_orient_matrix_UB_33 -0.1182468000 _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_source 'fine-focus sealed X-ray tube' _diffrn_source_type 'Enhance (Cu) X-ray Source' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 2516 _reflns_number_total 4038 _reflns_odcompleteness_completeness 99.95 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 66.97 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement 'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)' _computing_data_collection 'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)' _computing_data_reduction 'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'ShelXS (Sheldrick, 2008)' _refine_diff_density_max 0.289 _refine_diff_density_min -0.171 _refine_diff_density_rms 0.043 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 321 _refine_ls_number_reflns 4038 _refine_ls_number_restraints 45 _refine_ls_R_factor_all 0.1041 _refine_ls_R_factor_gt 0.0685 _refine_ls_restrained_S_all 1.050 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.1138P)^2^+0.3704P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1907 _refine_ls_wR_factor_ref 0.2181 _refine_special_details ? _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups, All N(H) groups At 1.5 times of: All C(H,H,H) groups, All O(H) groups 2. Restrained distances N2A-C11A 1.44 with sigma of 0.02 C13A-N2A 1.44 with sigma of 0.02 C11A-C10 1.39 with sigma of 0.02 C14A-N2A 2.5 with sigma of 0.02 C13A-C15A 2.5 with sigma of 0.02 C13-C14 1.53 with sigma of 0.02 C14A-C13A 1.53 with sigma of 0.02 N2A-C12 1.43 with sigma of 0.02 N2-C11 1.43 with sigma of 0.02 3. Uiso/Uaniso restraints and constraints Uanis(C17) \\sim Ueq, Uanis(C18) \\sim Ueq, Uanis(C19) \\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(C15) \\sim Ueq, Uanis(C16) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02 Uanis(C21) = Uanis(C21A) Uanis(C20) = Uanis(C20A) Uanis(C15) = Uanis(C15A) Uanis(C16) = Uanis(C16A) Uanis(C17) = Uanis(C17A) Uanis(C18) = Uanis(C18A) Uanis(C19) = Uanis(C19A) Uanis(C14) = Uanis(C14A) Uanis(C13) = Uanis(C13A) Uanis(C11) = Uanis(C11A) Uanis(N2) = Uanis(N2A) 4. Others Sof(H9B)=Sof(C20A)=Sof(H20A)=Sof(C21A)=Sof(H21A)=1-FVAR(1) Sof(H9A)=Sof(C20)=Sof(H20)=Sof(C21)=Sof(H21)=FVAR(1) Sof(H12A)=Sof(N2A)=Sof(C11A)=Sof(H11A)=Sof(C13A)=Sof(H13C)=Sof(H13D)= Sof(C19A)=Sof(H19A)=Sof(C18A)=Sof(H18A)=Sof(C17A)=Sof(H17A)=Sof(C16A)= Sof(H16A)=Sof(C15A)=Sof(C14A)=1-FVAR(2) Sof(H12)=Sof(N2)=Sof(C11)=Sof(H11)=Sof(C13)=Sof(H13A)=Sof(H13B)=Sof(C14)= Sof(C19)=Sof(H19)=Sof(C18)=Sof(H18)=Sof(C17)=Sof(H17)=Sof(C16)=Sof(H16)= Sof(C15)=FVAR(2) 5.a Ternary CH refined with riding coordinates: C9(H9A), C9(H9B), C12(H12), C12(H12A) 5.b Secondary CH2 refined with riding coordinates: C13(H13A,H13B), C13A(H13C,H13D) 5.c Aromatic/amide H refined with riding coordinates: N1(H1), C1(H1A), C2(H2), C3(H3), C4(H4A), C11(H11), C19(H19), C18(H18), C17(H17), C16(H16), C20(H20), C21(H21), C11A(H11A), C19A(H19A), C18A(H18A), C17A(H17A), C16A(H16A), C20A(H20A), C21A(H21A) 5.d Fitted hexagon refined as free rotating group: C14(C19,C18,C17,C16,C15), C19A(C18A,C17A,C16A,C15A,C14A) 5.e Idealised Me refined as rotating group: C24(H24A,H24B,H24C), C26(H26A,H26B,H26C) 5.f Idealised tetrahedral OH refined as rotating group: O4(H4) ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary ? loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group O1 O 0.4372(3) 0.63915(16) 0.5248(2) 0.0866(8) Uani 1 1 d . . . . . O2 O 0.5347(4) 0.81561(17) 0.1173(3) 0.1064(10) Uani 1 1 d . . . . . O3 O 0.3951(3) 0.72123(18) 0.1022(2) 0.0898(8) Uani 1 1 d . . . . . O4 O 0.8361(4) 0.46250(17) 0.4370(3) 0.1042(10) Uani 1 1 d . . . . . H4 H 0.8335 0.4486 0.3784 0.156 Uiso 1 1 calc GR . . . . O5 O 0.8021(3) 0.47147(15) 0.2454(3) 0.0998(9) Uani 1 1 d . . . . . N1 N 0.2260(3) 0.7069(2) 0.4821(2) 0.0842(10) Uani 1 1 d . . . . . H1 H 0.1809 0.6824 0.5157 0.101 Uiso 1 1 calc R . . . . N3 N 0.4747(3) 0.76935(18) 0.1566(2) 0.0736(8) Uani 1 1 d . . . . . C1 C 0.2325(4) 0.8563(2) 0.3172(3) 0.0719(9) Uani 1 1 d . . . . . H1A H 0.2977 0.8752 0.2868 0.086 Uiso 1 1 calc R . . . . C2 C 0.0949(5) 0.8880(3) 0.2986(4) 0.0954(13) Uani 1 1 d . . . . . H2 H 0.0676 0.9281 0.2547 0.115 Uiso 1 1 calc R . . . . C3 C 0.0003(5) 0.8609(4) 0.3441(4) 0.1104(18) Uani 1 1 d . . . . . H3 H -0.0902 0.8833 0.3317 0.133 Uiso 1 1 calc R . . . . C4 C 0.0358(4) 0.8012(3) 0.4080(3) 0.1044(16) Uani 1 1 d . . . . . H4A H -0.0294 0.7828 0.4386 0.125 Uiso 1 1 calc R . . . . C5 C 0.1692(4) 0.7695(2) 0.4253(3) 0.0747(10) Uani 1 1 d . . . . . C6 C 0.2698(3) 0.79633(19) 0.3816(2) 0.0602(8) Uani 1 1 d . . . . . C7 C 0.4017(3) 0.74648(17) 0.4121(2) 0.0566(7) Uani 1 1 d . . . . . C8 C 0.3594(4) 0.6891(2) 0.4783(2) 0.0667(8) Uani 1 1 d . . . . . C9 C 0.4280(3) 0.71405(17) 0.3124(2) 0.0580(7) Uani 1 1 d . . . . . H9A H 0.3298 0.7055 0.2598 0.070 Uiso 0.808(6) 1 calc R . P A 1 H9B H 0.3399 0.6923 0.2608 0.070 Uiso 0.192(6) 1 calc R . P A 2 C10 C 0.4975(3) 0.77216(18) 0.2662(3) 0.0598(8) Uani 1 1 d D . . . . C12 C 0.5490(3) 0.78086(18) 0.4842(3) 0.0649(8) Uani 1 1 d D . . . . H12 H 0.6252 0.7435 0.5078 0.078 Uiso 0.695(17) 1 calc R . P B 1 H12A H 0.6190 0.7413 0.5118 0.078 Uiso 0.305(17) 1 calc R . P B 2 C22 C 0.7078(5) 0.5594(2) 0.3313(4) 0.0863(11) Uani 1 1 d . . . . . C23 C 0.7624(5) 0.5228(2) 0.4266(4) 0.0944(13) Uani 1 1 d . . . . . C24 C 0.7467(7) 0.5481(4) 0.5276(4) 0.139(2) Uani 1 1 d . . . . . H24A H 0.7060 0.5101 0.5573 0.208 Uiso 1 1 calc GR . . . . H24B H 0.6822 0.5891 0.5135 0.208 Uiso 1 1 calc GR . . . . H24C H 0.8418 0.5614 0.5769 0.208 Uiso 1 1 calc GR . . . . C25 C 0.7283(5) 0.5280(2) 0.2406(4) 0.0878(12) Uani 1 1 d . . . . . C26 C 0.6601(6) 0.5626(3) 0.1319(4) 0.1078(15) Uani 1 1 d . . . . . H26A H 0.7337 0.5672 0.0994 0.162 Uiso 1 1 calc GR . . . . H26B H 0.6227 0.6094 0.1395 0.162 Uiso 1 1 calc GR . . . . H26C H 0.5807 0.5330 0.0882 0.162 Uiso 1 1 calc GR . . . . N2 N 0.5992(19) 0.8383(5) 0.4291(9) 0.0661(17) Uani 0.695(17) 1 d D . P B 1 C11 C 0.5766(16) 0.8232(5) 0.3281(8) 0.0610(19) Uani 0.695(17) 1 d D . P B 1 H11 H 0.6245 0.8537 0.2958 0.073 Uiso 0.695(17) 1 calc R . P B 1 C13 C 0.6581(13) 0.8999(5) 0.4957(8) 0.077(2) Uani 0.695(17) 1 d D . P B 1 H13A H 0.6205 0.9446 0.4587 0.092 Uiso 0.695(17) 1 calc R . P B 1 H13B H 0.7651 0.9005 0.5201 0.092 Uiso 0.695(17) 1 calc R . P B 1 C14 C 0.6042(11) 0.8885(4) 0.5840(6) 0.0799(17) Uani 0.695(17) 1 d D U P B 1 C19 C 0.6173(9) 0.9346(4) 0.6682(7) 0.092(2) Uani 0.695(17) 1 d G U P B 1 H19 H 0.6604 0.9797 0.6710 0.110 Uiso 0.695(17) 1 calc R . P B 1 C18 C 0.5658(9) 0.9134(5) 0.7482(6) 0.099(3) Uani 0.695(17) 1 d G U P B 1 H18 H 0.5746 0.9442 0.8046 0.119 Uiso 0.695(17) 1 calc R . P B 1 C17 C 0.5013(9) 0.8460(5) 0.7441(5) 0.089(2) Uani 0.695(17) 1 d G U P B 1 H17 H 0.4669 0.8318 0.7976 0.106 Uiso 0.695(17) 1 calc R . P B 1 C16 C 0.4882(10) 0.7999(4) 0.6599(5) 0.0735(16) Uani 0.695(17) 1 d G U P B 1 H16 H 0.4450 0.7549 0.6571 0.088 Uiso 0.695(17) 1 calc R . P B 1 C15 C 0.5397(11) 0.8212(4) 0.5798(5) 0.0654(15) Uani 0.695(17) 1 d G U P B 1 C20 C 0.5065(5) 0.6428(2) 0.3289(3) 0.0573(10) Uani 0.808(6) 1 d . . P A 1 H20 H 0.4588 0.6035 0.3454 0.069 Uiso 0.808(6) 1 calc R . P A 1 C21 C 0.6360(5) 0.6315(2) 0.3219(4) 0.0680(11) Uani 0.808(6) 1 d . . P A 1 H21 H 0.6873 0.6711 0.3103 0.082 Uiso 0.808(6) 1 calc R . P A 1 N2A N 0.607(5) 0.8248(12) 0.415(2) 0.0661(17) Uani 0.305(17) 1 d D . P B 2 C11A C 0.568(4) 0.8351(12) 0.308(2) 0.0610(19) Uani 0.305(17) 1 d D . P B 2 H11A H 0.5856 0.8750 0.2718 0.073 Uiso 0.305(17) 1 calc R . P B 2 C13A C 0.663(4) 0.8986(13) 0.4600(17) 0.077(2) Uani 0.305(17) 1 d D . P B 2 H13C H 0.6109 0.9369 0.4126 0.092 Uiso 0.305(17) 1 calc R . P B 2 H13D H 0.7678 0.9034 0.4750 0.092 Uiso 0.305(17) 1 calc R . P B 2 C19A C 0.636(2) 0.9517(8) 0.6371(15) 0.092(2) Uani 0.305(17) 1 d . . P B 2 H19A H 0.6752 0.9964 0.6298 0.110 Uiso 0.305(17) 1 calc R . P B 2 C18A C 0.589(2) 0.9390(9) 0.7222(13) 0.099(3) Uani 0.305(17) 1 d G . P B 2 H18A H 0.5967 0.9751 0.7717 0.119 Uiso 0.305(17) 1 calc R . P B 2 C17A C 0.531(2) 0.8722(10) 0.7332(12) 0.089(2) Uani 0.305(17) 1 d G . P B 2 H17A H 0.4997 0.8637 0.7901 0.106 Uiso 0.305(17) 1 calc R . P B 2 C16A C 0.520(2) 0.8183(9) 0.6592(15) 0.0735(16) Uani 0.305(17) 1 d G . P B 2 H16A H 0.4812 0.7736 0.6666 0.088 Uiso 0.305(17) 1 calc R . P B 2 C15A C 0.567(3) 0.8311(9) 0.5742(15) 0.0654(15) Uani 0.305(17) 1 d DG . P B 2 C14A C 0.625(3) 0.8978(10) 0.5631(14) 0.0799(17) Uani 0.305(17) 1 d DG . P B 2 C20A C 0.578(2) 0.6567(11) 0.3555(17) 0.0573(10) Uani 0.192(6) 1 d . . P A 2 H20A H 0.6662 0.6687 0.4089 0.069 Uiso 0.192(6) 1 calc R . P A 2 C21A C 0.556(2) 0.5954(10) 0.3064(16) 0.0680(11) Uani 0.192(6) 1 d . . P A 2 H21A H 0.4659 0.5766 0.2639 0.082 Uiso 0.192(6) 1 calc R . P A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.0997(18) 0.0812(18) 0.0814(16) 0.0209(14) 0.0346(14) 0.0035(16) O2 0.143(3) 0.095(2) 0.114(2) 0.0090(18) 0.087(2) -0.0129(19) O3 0.0940(18) 0.110(2) 0.0724(16) -0.0069(16) 0.0378(14) -0.0103(17) O4 0.0896(19) 0.0756(18) 0.146(3) 0.0277(19) 0.039(2) 0.0221(16) O5 0.0960(19) 0.0646(16) 0.144(3) -0.0094(16) 0.0482(18) 0.0176(15) N1 0.0717(18) 0.120(3) 0.0656(17) 0.0155(18) 0.0299(14) -0.0090(18) N3 0.0745(17) 0.081(2) 0.0778(19) 0.0098(17) 0.0424(15) 0.0072(16) C1 0.0670(19) 0.073(2) 0.075(2) -0.0015(18) 0.0235(16) 0.0147(18) C2 0.081(3) 0.099(3) 0.097(3) -0.004(2) 0.019(2) 0.031(2) C3 0.066(2) 0.171(5) 0.095(3) -0.007(3) 0.029(2) 0.039(3) C4 0.067(2) 0.178(5) 0.078(2) 0.006(3) 0.0366(19) 0.018(3) C5 0.0595(18) 0.115(3) 0.0509(17) -0.0045(19) 0.0205(14) 0.0023(19) C6 0.0548(15) 0.073(2) 0.0520(15) -0.0093(15) 0.0172(12) 0.0039(15) C7 0.0570(16) 0.0557(17) 0.0594(16) 0.0007(14) 0.0230(13) 0.0032(14) C8 0.073(2) 0.075(2) 0.0532(17) 0.0018(16) 0.0223(14) -0.0085(18) C9 0.0561(15) 0.0576(18) 0.0635(17) 0.0034(14) 0.0248(13) 0.0015(14) C10 0.0555(16) 0.0605(18) 0.0681(19) 0.0066(15) 0.0276(14) 0.0065(15) C12 0.0547(16) 0.0603(19) 0.073(2) 0.0076(16) 0.0136(14) 0.0074(14) C22 0.081(2) 0.072(2) 0.110(3) 0.006(2) 0.038(2) 0.023(2) C23 0.084(3) 0.081(3) 0.120(3) 0.019(3) 0.038(2) 0.018(2) C24 0.145(5) 0.158(6) 0.111(4) 0.041(4) 0.040(3) 0.066(4) C25 0.077(2) 0.069(2) 0.118(3) -0.008(2) 0.036(2) 0.007(2) C26 0.115(4) 0.099(3) 0.107(3) 0.000(3) 0.036(3) 0.027(3) N2 0.059(2) 0.052(4) 0.080(3) -0.005(2) 0.016(2) -0.002(4) C11 0.052(2) 0.057(4) 0.074(5) 0.032(3) 0.023(3) 0.008(3) C13 0.087(3) 0.069(2) 0.061(6) -0.005(4) 0.007(5) -0.011(2) C14 0.067(3) 0.071(3) 0.085(4) -0.009(3) 0.005(2) 0.007(2) C19 0.093(4) 0.069(4) 0.094(5) -0.015(4) 0.009(3) 0.000(3) C18 0.096(4) 0.087(6) 0.095(5) -0.027(4) 0.009(3) 0.010(4) C17 0.082(4) 0.095(5) 0.074(3) -0.012(3) 0.009(2) 0.014(4) C16 0.061(4) 0.079(4) 0.067(2) -0.013(3) 0.005(2) 0.001(3) C15 0.047(4) 0.066(3) 0.071(2) -0.005(2) 0.0056(19) 0.004(2) C20 0.055(3) 0.054(2) 0.064(2) 0.0010(18) 0.023(2) -0.005(2) C21 0.065(3) 0.053(2) 0.093(3) 0.000(2) 0.035(2) -0.0023(19) N2A 0.059(2) 0.052(4) 0.080(3) -0.005(2) 0.016(2) -0.002(4) C11A 0.052(2) 0.057(4) 0.074(5) 0.032(3) 0.023(3) 0.008(3) C13A 0.087(3) 0.069(2) 0.061(6) -0.005(4) 0.007(5) -0.011(2) C19A 0.093(4) 0.069(4) 0.094(5) -0.015(4) 0.009(3) 0.000(3) C18A 0.096(4) 0.087(6) 0.095(5) -0.027(4) 0.009(3) 0.010(4) C17A 0.082(4) 0.095(5) 0.074(3) -0.012(3) 0.009(2) 0.014(4) C16A 0.061(4) 0.079(4) 0.067(2) -0.013(3) 0.005(2) 0.001(3) C15A 0.047(4) 0.066(3) 0.071(2) -0.005(2) 0.0056(19) 0.004(2) C14A 0.067(3) 0.071(3) 0.085(4) -0.009(3) 0.005(2) 0.007(2) C20A 0.055(3) 0.054(2) 0.064(2) 0.0010(18) 0.023(2) -0.005(2) C21A 0.065(3) 0.053(2) 0.093(3) 0.000(2) 0.035(2) -0.0023(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1 C8 1.221(4) . ? O2 N3 1.252(4) . ? O3 N3 1.239(4) . ? O4 H4 0.8200 . ? O4 C23 1.309(5) . ? O5 C25 1.258(5) . ? N1 H1 0.8600 . ? N1 C5 1.394(5) . ? N1 C8 1.349(5) . ? N3 C10 1.414(4) . ? C1 H1A 0.9300 . ? C1 C2 1.395(5) . ? C1 C6 1.380(5) . ? C2 H2 0.9300 . ? C2 C3 1.362(7) . ? C3 H3 0.9300 . ? C3 C4 1.372(8) . ? C4 H4A 0.9300 . ? C4 C5 1.361(5) . ? C5 C6 1.391(5) . ? C6 C7 1.513(4) . ? C7 C8 1.533(5) . ? C7 C9 1.568(4) . ? C7 C12 1.554(4) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 C10 1.513(4) . ? C9 C20 1.503(5) . ? C9 C20A 1.73(2) . ? C10 C11 1.317(9) . ? C10 C11A 1.371(19) . ? C12 H12 0.9800 . ? C12 H12A 0.9800 . ? C12 N2 1.474(9) . ? C12 C15 1.518(6) . ? C12 N2A 1.487(18) . ? C12 C15A 1.489(12) . ? C22 C23 1.384(6) . ? C22 C25 1.425(6) . ? C22 C21 1.493(6) . ? C22 C21A 1.536(19) . ? C23 C24 1.493(7) . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 C26 1.522(6) . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? N2 C11 1.328(9) . ? N2 C13 1.443(9) . ? C11 H11 0.9300 . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C13 C14 1.469(8) . ? C14 C19 1.3900 . ? C14 C15 1.3900 . ? C19 H19 0.9300 . ? C19 C18 1.3900 . ? C18 H18 0.9300 . ? C18 C17 1.3900 . ? C17 H17 0.9300 . ? C17 C16 1.3900 . ? C16 H16 0.9300 . ? C16 C15 1.3900 . ? C20 H20 0.9300 . ? C20 C21 1.304(7) . ? C21 H21 0.9300 . ? N2A C11A 1.370(18) . ? N2A C13A 1.520(18) . ? C11A H11A 0.9300 . ? C13A H13C 0.9700 . ? C13A H13D 0.9700 . ? C13A C14A 1.550(14) . ? C19A H19A 0.9300 . ? C19A C18A 1.3900 . ? C19A C14A 1.3900 . ? C18A H18A 0.9300 . ? C18A C17A 1.3900 . ? C17A H17A 0.9300 . ? C17A C16A 1.3900 . ? C16A H16A 0.9300 . ? C16A C15A 1.3900 . ? C15A C14A 1.3900 . ? C20A H20A 0.9300 . ? C20A C21A 1.30(3) . ? C21A H21A 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C23 O4 H4 109.5 . . ? C5 N1 H1 123.7 . . ? C8 N1 H1 123.7 . . ? C8 N1 C5 112.6(3) . . ? O2 N3 C10 119.2(3) . . ? O3 N3 O2 122.0(3) . . ? O3 N3 C10 118.9(3) . . ? C2 C1 H1A 120.7 . . ? C6 C1 H1A 120.7 . . ? C6 C1 C2 118.6(4) . . ? C1 C2 H2 119.7 . . ? C3 C2 C1 120.7(4) . . ? C3 C2 H2 119.7 . . ? C2 C3 H3 119.4 . . ? C2 C3 C4 121.3(4) . . ? C4 C3 H3 119.4 . . ? C3 C4 H4A 120.9 . . ? C5 C4 C3 118.2(4) . . ? C5 C4 H4A 120.9 . . ? C4 C5 N1 128.5(4) . . ? C4 C5 C6 122.2(4) . . ? C6 C5 N1 109.3(3) . . ? C1 C6 C5 119.1(3) . . ? C1 C6 C7 132.5(3) . . ? C5 C6 C7 108.3(3) . . ? C6 C7 C8 102.3(3) . . ? C6 C7 C9 112.0(2) . . ? C6 C7 C12 114.9(3) . . ? C8 C7 C9 112.6(3) . . ? C8 C7 C12 107.1(3) . . ? C12 C7 C9 107.8(2) . . ? O1 C8 N1 126.5(3) . . ? O1 C8 C7 125.8(3) . . ? N1 C8 C7 107.6(3) . . ? C7 C9 H9A 106.0 . . ? C7 C9 H9B 113.8 . . ? C7 C9 C20A 108.4(7) . . ? C10 C9 C7 107.7(3) . . ? C10 C9 H9A 106.0 . . ? C10 C9 H9B 113.8 . . ? C10 C9 C20A 97.9(7) . . ? C20 C9 C7 115.8(3) . . ? C20 C9 H9A 106.0 . . ? C20 C9 C10 114.5(3) . . ? C20A C9 H9B 113.8 . . ? N3 C10 C9 118.1(3) . . ? C11 C10 N3 122.1(6) . . ? C11 C10 C9 119.8(6) . . ? C11A C10 N3 109.2(12) . . ? C11A C10 C9 132.2(13) . . ? C7 C12 H12 109.5 . . ? C7 C12 H12A 106.9 . . ? N2 C12 C7 111.9(6) . . ? N2 C12 H12 109.5 . . ? N2 C12 C15 101.3(4) . . ? C15 C12 C7 114.8(4) . . ? C15 C12 H12 109.5 . . ? N2A C12 C7 107.1(14) . . ? N2A C12 H12A 106.9 . . ? N2A C12 C15A 101.7(11) . . ? C15A C12 C7 126.0(9) . . ? C15A C12 H12A 106.9 . . ? C23 C22 C25 118.1(4) . . ? C23 C22 C21 122.3(4) . . ? C23 C22 C21A 116.3(8) . . ? C25 C22 C21 119.5(4) . . ? C25 C22 C21A 113.3(8) . . ? O4 C23 C22 122.4(5) . . ? O4 C23 C24 113.3(4) . . ? C22 C23 C24 124.2(4) . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24B 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? O5 C25 C22 122.8(4) . . ? O5 C25 C26 116.7(4) . . ? C22 C25 C26 120.4(4) . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26B 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C11 N2 C12 113.3(9) . . ? C11 N2 C13 133.8(9) . . ? C13 N2 C12 113.0(6) . . ? C10 C11 N2 130.7(11) . . ? C10 C11 H11 114.7 . . ? N2 C11 H11 114.7 . . ? N2 C13 H13A 111.3 . . ? N2 C13 H13B 111.3 . . ? N2 C13 C14 102.3(6) . . ? H13A C13 H13B 109.2 . . ? C14 C13 H13A 111.3 . . ? C14 C13 H13B 111.3 . . ? C19 C14 C13 127.8(4) . . ? C19 C14 C15 120.0 . . ? C15 C14 C13 112.2(4) . . ? C14 C19 H19 120.0 . . ? C14 C19 C18 120.0 . . ? C18 C19 H19 120.0 . . ? C19 C18 H18 120.0 . . ? C17 C18 C19 120.0 . . ? C17 C18 H18 120.0 . . ? C18 C17 H17 120.0 . . ? C18 C17 C16 120.0 . . ? C16 C17 H17 120.0 . . ? C17 C16 H16 120.0 . . ? C15 C16 C17 120.0 . . ? C15 C16 H16 120.0 . . ? C14 C15 C12 108.7(4) . . ? C16 C15 C12 131.2(4) . . ? C16 C15 C14 120.0 . . ? C9 C20 H20 117.3 . . ? C21 C20 C9 125.4(4) . . ? C21 C20 H20 117.3 . . ? C22 C21 H21 117.7 . . ? C20 C21 C22 124.6(4) . . ? C20 C21 H21 117.7 . . ? C12 N2A C13A 113.7(13) . . ? C11A N2A C12 136(3) . . ? C11A N2A C13A 103.0(18) . . ? C10 C11A H11A 128.6 . . ? N2A C11A C10 102.9(19) . . ? N2A C11A H11A 128.6 . . ? N2A C13A H13C 111.6 . . ? N2A C13A H13D 111.6 . . ? N2A C13A C14A 100.9(11) . . ? H13C C13A H13D 109.4 . . ? C14A C13A H13C 111.6 . . ? C14A C13A H13D 111.6 . . ? C18A C19A H19A 120.0 . . ? C18A C19A C14A 120.0 . . ? C14A C19A H19A 120.0 . . ? C19A C18A H18A 120.0 . . ? C17A C18A C19A 120.0 . . ? C17A C18A H18A 120.0 . . ? C18A C17A H17A 120.0 . . ? C18A C17A C16A 120.0 . . ? C16A C17A H17A 120.0 . . ? C17A C16A H16A 120.0 . . ? C15A C16A C17A 120.0 . . ? C15A C16A H16A 120.0 . . ? C16A C15A C12 125.6(10) . . ? C16A C15A C14A 120.0 . . ? C14A C15A C12 114.2(10) . . ? C19A C14A C13A 130.5(10) . . ? C15A C14A C13A 109.4(10) . . ? C15A C14A C19A 120.0 . . ? C9 C20A H20A 123.1 . . ? C21A C20A C9 113.7(18) . . ? C21A C20A H20A 123.1 . . ? C22 C21A H21A 126.3 . . ? C20A C21A C22 107.3(18) . . ? C20A C21A H21A 126.3 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O4 H4 O5 0.82 1.76 2.486(5) 146.8 . N1 H1 O2 0.86 2.28 3.039(4) 147.1 4_576 N1 H1 O4 0.86 2.78 3.450(5) 135.5 3_666 loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 N3 C10 C9 -177.9(3) . . . . ? O2 N3 C10 C11 2.0(9) . . . . ? O2 N3 C10 C11A 9.2(18) . . . . ? O3 N3 C10 C9 2.5(4) . . . . ? O3 N3 C10 C11 -177.7(8) . . . . ? O3 N3 C10 C11A -170.5(18) . . . . ? N1 C5 C6 C1 176.6(3) . . . . ? N1 C5 C6 C7 0.5(4) . . . . ? N3 C10 C11 N2 173.3(15) . . . . ? N3 C10 C11A N2A -169(3) . . . . ? C1 C2 C3 C4 -1.1(8) . . . . ? C1 C6 C7 C8 -175.5(3) . . . . ? C1 C6 C7 C9 -54.7(5) . . . . ? C1 C6 C7 C12 68.8(5) . . . . ? C2 C1 C6 C5 0.2(5) . . . . ? C2 C1 C6 C7 175.3(4) . . . . ? C2 C3 C4 C5 0.3(8) . . . . ? C3 C4 C5 N1 -176.4(4) . . . . ? C3 C4 C5 C6 0.8(7) . . . . ? C4 C5 C6 C1 -1.0(6) . . . . ? C4 C5 C6 C7 -177.2(4) . . . . ? C5 N1 C8 O1 176.3(3) . . . . ? C5 N1 C8 C7 0.7(4) . . . . ? C5 C6 C7 C8 -0.1(3) . . . . ? C5 C6 C7 C9 120.8(3) . . . . ? C5 C6 C7 C12 -115.8(3) . . . . ? C6 C1 C2 C3 0.8(6) . . . . ? C6 C7 C8 O1 -176.0(3) . . . . ? C6 C7 C8 N1 -0.3(3) . . . . ? C6 C7 C9 C10 76.3(3) . . . . ? C6 C7 C9 C20 -154.0(3) . . . . ? C6 C7 C9 C20A -178.8(8) . . . . ? C6 C7 C12 N2 -65.9(6) . . . . ? C6 C7 C12 C15 48.9(5) . . . . ? C6 C7 C12 N2A -78.9(13) . . . . ? C6 C7 C12 C15A 40.2(11) . . . . ? C7 C9 C10 N3 -153.1(3) . . . . ? C7 C9 C10 C11 27.1(8) . . . . ? C7 C9 C10 C11A 18(2) . . . . ? C7 C9 C20 C21 -115.5(5) . . . . ? C7 C9 C20A C21A 133.7(15) . . . . ? C7 C12 N2 C11 -39.0(16) . . . . ? C7 C12 N2 C13 139.1(11) . . . . ? C7 C12 C15 C14 -130.8(4) . . . . ? C7 C12 C15 C16 53.5(8) . . . . ? C7 C12 N2A C11A -7(5) . . . . ? C7 C12 N2A C13A 135(3) . . . . ? C7 C12 C15A C16A 53.7(19) . . . . ? C7 C12 C15A C14A -120.6(10) . . . . ? C8 N1 C5 C4 176.7(4) . . . . ? C8 N1 C5 C6 -0.8(4) . . . . ? C8 C7 C9 C10 -169.0(3) . . . . ? C8 C7 C9 C20 -39.3(4) . . . . ? C8 C7 C9 C20A -64.1(8) . . . . ? C8 C7 C12 N2 -178.8(6) . . . . ? C8 C7 C12 C15 -64.0(5) . . . . ? C8 C7 C12 N2A 168.2(13) . . . . ? C8 C7 C12 C15A -72.6(11) . . . . ? C9 C7 C8 O1 63.5(4) . . . . ? C9 C7 C8 N1 -120.8(3) . . . . ? C9 C7 C12 N2 59.7(6) . . . . ? C9 C7 C12 C15 174.5(4) . . . . ? C9 C7 C12 N2A 46.8(13) . . . . ? C9 C7 C12 C15A 165.9(11) . . . . ? C9 C10 C11 N2 -7(2) . . . . ? C9 C10 C11A N2A 19(4) . . . . ? C9 C20 C21 C22 -175.6(4) . . . . ? C9 C20A C21A C22 165.4(11) . . . . ? C10 C9 C20 C21 10.8(6) . . . . ? C10 C9 C20A C21A -114.6(16) . . . . ? C12 C7 C8 O1 -54.8(4) . . . . ? C12 C7 C8 N1 120.8(3) . . . . ? C12 C7 C9 C10 -51.1(3) . . . . ? C12 C7 C9 C20 78.6(4) . . . . ? C12 C7 C9 C20A 53.9(8) . . . . ? C12 N2 C11 C10 12(3) . . . . ? C12 N2 C13 C14 -15.9(16) . . . . ? C12 N2A C11A C10 -26(6) . . . . ? C12 N2A C13A C14A -3(4) . . . . ? C12 C15A C14A C13A -3.0(19) . . . . ? C12 C15A C14A C19A 174.7(18) . . . . ? C23 C22 C25 O5 -5.0(7) . . . . ? C23 C22 C25 C26 175.1(4) . . . . ? C23 C22 C21 C20 -71.2(7) . . . . ? C23 C22 C21A C20A 82.2(16) . . . . ? C25 C22 C23 O4 2.6(7) . . . . ? C25 C22 C23 C24 -178.7(5) . . . . ? C25 C22 C21 C20 112.1(6) . . . . ? C25 C22 C21A C20A -136.0(13) . . . . ? N2 C12 C15 C14 -9.9(8) . . . . ? N2 C12 C15 C16 174.3(9) . . . . ? N2 C13 C14 C19 -174.2(9) . . . . ? N2 C13 C14 C15 8.8(12) . . . . ? C11 N2 C13 C14 161.7(19) . . . . ? C13 N2 C11 C10 -165.3(14) . . . . ? C13 C14 C19 C18 -176.7(11) . . . . ? C13 C14 C15 C12 0.9(7) . . . . ? C13 C14 C15 C16 177.2(9) . . . . ? C14 C19 C18 C17 0.0 . . . . ? C19 C14 C15 C12 -176.3(7) . . . . ? C19 C14 C15 C16 0.0 . . . . ? C19 C18 C17 C16 0.0 . . . . ? C18 C17 C16 C15 0.0 . . . . ? C17 C16 C15 C12 175.4(9) . . . . ? C17 C16 C15 C14 0.0 . . . . ? C15 C12 N2 C11 -161.8(13) . . . . ? C15 C12 N2 C13 16.3(14) . . . . ? C15 C14 C19 C18 0.0 . . . . ? C20 C9 C10 N3 76.5(4) . . . . ? C20 C9 C10 C11 -103.3(8) . . . . ? C21 C22 C23 O4 -174.2(4) . . . . ? C21 C22 C23 C24 4.5(8) . . . . ? C21 C22 C25 O5 171.9(4) . . . . ? C21 C22 C25 C26 -8.0(6) . . . . ? N2A C12 C15A C16A 175(2) . . . . ? N2A C12 C15A C14A 1(2) . . . . ? N2A C13A C14A C19A -174(2) . . . . ? N2A C13A C14A C15A 4(3) . . . . ? C11A N2A C13A C14A 151(3) . . . . ? C13A N2A C11A C10 -171(3) . . . . ? C19A C18A C17A C16A 0.0 . . . . ? C18A C19A C14A C13A 177(3) . . . . ? C18A C19A C14A C15A 0.0 . . . . ? C18A C17A C16A C15A 0.0 . . . . ? C17A C16A C15A C12 -174(2) . . . . ? C17A C16A C15A C14A 0.0 . . . . ? C16A C15A C14A C13A -178(2) . . . . ? C16A C15A C14A C19A 0.0 . . . . ? C15A C12 N2A C11A -141(4) . . . . ? C15A C12 N2A C13A 2(4) . . . . ? C14A C19A C18A C17A 0.0 . . . . ? C20A C9 C10 N3 94.6(8) . . . . ? C20A C9 C10 C11A -94(2) . . . . ? C21A C22 C23 O4 142.5(9) . . . . ? C21A C22 C23 C24 -38.8(11) . . . . ? C21A C22 C25 O5 -146.0(9) . . . . ? C21A C22 C25 C26 34.1(10) . . . . ? _shelx_res_file ; zzy1062.res created by SHELXL-2014/7 TITL zzy1062 in P21/n #14 REM reset to P21/n #14 CELL 1.54184 9.664174 18.573294 13.447942 90 110.324 90 ZERR 4 0.0004 0.000701 0.000556 0 0.0044 0 LATT 1 SYMM 0.5-X,0.5+Y,0.5-Z SFAC C H N O UNIT 104 92 12 20 EQIV $1 -0.5+X,1.5-Y,0.5+Z EQIV $2 1-X,1-Y,1-Z DFIX 1.44 N2A C11A DFIX 1.44 C13A N2A DFIX 1.39 C11A C10 DFIX 2.5 C14A N2A DFIX 2.5 C13A C15A DFIX 1.53 C13 C14 DFIX 1.53 C14A C13A DFIX 1.43 N2A C12 DFIX 1.43 N2 C11 ISOR 0.01 0.02 C17 C18 C19 C14 C15 C16 EADP C21 C21A EADP C20 C20A EADP C15 C15A EADP C16 C16A EADP C17 C17A EADP C18 C18A EADP C19 C19A EADP C14 C14A EADP C13 C13A EADP C11 C11A EADP N2 N2A L.S. 4 0 0 PLAN 20 SIZE 0.04 0.07 0.15 MPLA C1 C2 C3 C4 C5 C6 C7 C8 N1 MPLA C14 C15 C16 C17 C18 C19 HTAB O4 O5 HTAB N1 O2_$1 HTAB N1 O4_$2 bond $h conf fmap 2 acta REM REM REM WGHT 0.113800 0.370400 FVAR 5.30639 0.80774 0.69450 O1 4 0.437219 0.639153 0.524758 11.00000 0.09971 0.08123 = 0.08144 0.02086 0.03464 0.00348 O2 4 0.534715 0.815610 0.117310 11.00000 0.14330 0.09530 = 0.11395 0.00896 0.08678 -0.01293 O3 4 0.395126 0.721225 0.102150 11.00000 0.09403 0.11019 = 0.07236 -0.00690 0.03783 -0.01033 O4 4 0.836149 0.462497 0.436956 11.00000 0.08957 0.07562 = 0.14580 0.02774 0.03883 0.02208 AFIX 147 H4 2 0.833492 0.448597 0.378445 11.00000 -1.50000 AFIX 0 O5 4 0.802116 0.471474 0.245421 11.00000 0.09602 0.06459 = 0.14399 -0.00937 0.04818 0.01755 N1 3 0.225987 0.706946 0.482056 11.00000 0.07167 0.12026 = 0.06556 0.01550 0.02988 -0.00899 AFIX 43 H1 2 0.180903 0.682428 0.515747 11.00000 -1.20000 AFIX 0 N3 3 0.474693 0.769350 0.156592 11.00000 0.07450 0.08121 = 0.07778 0.00983 0.04240 0.00725 C1 1 0.232494 0.856305 0.317163 11.00000 0.06704 0.07268 = 0.07516 -0.00146 0.02351 0.01469 AFIX 43 H1A 2 0.297661 0.875175 0.286795 11.00000 -1.20000 AFIX 0 C2 1 0.094910 0.888036 0.298589 11.00000 0.08066 0.09909 = 0.09748 -0.00448 0.01946 0.03123 AFIX 43 H2 2 0.067559 0.928127 0.254656 11.00000 -1.20000 AFIX 0 C3 1 0.000287 0.860914 0.344116 11.00000 0.06641 0.17108 = 0.09455 -0.00743 0.02892 0.03903 AFIX 43 H3 2 -0.090228 0.883332 0.331679 11.00000 -1.20000 AFIX 0 C4 1 0.035837 0.801176 0.407965 11.00000 0.06662 0.17778 = 0.07800 0.00614 0.03662 0.01808 AFIX 43 H4A 2 -0.029425 0.782788 0.438614 11.00000 -1.20000 AFIX 0 C5 1 0.169239 0.769531 0.425254 11.00000 0.05945 0.11488 = 0.05087 -0.00452 0.02053 0.00231 C6 1 0.269785 0.796327 0.381555 11.00000 0.05481 0.07284 = 0.05196 -0.00930 0.01723 0.00395 C7 1 0.401717 0.746482 0.412055 11.00000 0.05698 0.05566 = 0.05938 0.00066 0.02299 0.00320 C8 1 0.359398 0.689105 0.478330 11.00000 0.07265 0.07452 = 0.05318 0.00179 0.02225 -0.00848 C9 1 0.428040 0.714048 0.312427 11.00000 0.05614 0.05760 = 0.06347 0.00344 0.02481 0.00155 PART 1 AFIX 13 H9A 2 0.329837 0.705465 0.259800 21.00000 -1.20000 AFIX 13 PART 0 PART 2 H9B 2 0.339881 0.692254 0.260842 -21.00000 -1.20000 AFIX 0 PART 0 C10 1 0.497450 0.772162 0.266225 11.00000 0.05548 0.06051 = 0.06813 0.00659 0.02756 0.00651 C12 1 0.549037 0.780864 0.484185 11.00000 0.05468 0.06027 = 0.07301 0.00756 0.01360 0.00739 PART 1 AFIX 13 H12 2 0.625186 0.743548 0.507777 31.00000 -1.20000 AFIX 13 PART 0 PART 2 H12A 2 0.619018 0.741316 0.511807 -31.00000 -1.20000 AFIX 0 PART 0 C22 1 0.707817 0.559370 0.331267 11.00000 0.08108 0.07207 = 0.10969 0.00616 0.03819 0.02294 C23 1 0.762418 0.522826 0.426644 11.00000 0.08444 0.08109 = 0.11964 0.01917 0.03783 0.01823 C24 1 0.746713 0.548095 0.527602 11.00000 0.14481 0.15798 = 0.11077 0.04079 0.04026 0.06619 AFIX 137 H24A 2 0.706026 0.510103 0.557333 11.00000 -1.50000 H24B 2 0.682207 0.589069 0.513477 11.00000 -1.50000 H24C 2 0.841810 0.561358 0.576903 11.00000 -1.50000 AFIX 0 C25 1 0.728254 0.527988 0.240629 11.00000 0.07715 0.06935 = 0.11816 -0.00797 0.03553 0.00733 C26 1 0.660064 0.562579 0.131889 11.00000 0.11496 0.09916 = 0.10720 -0.00024 0.03590 0.02659 AFIX 137 H26A 2 0.733714 0.567181 0.099357 11.00000 -1.50000 H26B 2 0.622736 0.609376 0.139480 11.00000 -1.50000 H26C 2 0.580730 0.533001 0.088234 11.00000 -1.50000 AFIX 0 PART 1 N2 3 0.599214 0.838307 0.429094 31.00000 0.05940 0.05195 = 0.08014 -0.00540 0.01558 -0.00189 C11 1 0.576551 0.823206 0.328117 31.00000 0.05194 0.05749 = 0.07406 0.03194 0.02261 0.00788 AFIX 43 H11 2 0.624472 0.853728 0.295777 31.00000 -1.20000 AFIX 0 C13 1 0.658076 0.899919 0.495667 31.00000 0.08658 0.06903 = 0.06072 -0.00531 0.00680 -0.01116 AFIX 23 H13A 2 0.620537 0.944559 0.458700 31.00000 -1.20000 H13B 2 0.765050 0.900510 0.520094 31.00000 -1.20000 AFIX 66 C14 1 0.604180 0.888508 0.584028 31.00000 0.06665 0.07074 = 0.08509 -0.00902 0.00466 0.00683 C19 1 0.617257 0.934616 0.668229 31.00000 0.09344 0.06905 = 0.09446 -0.01460 0.00877 0.00026 AFIX 43 H19 2 0.660425 0.979674 0.671031 31.00000 -1.20000 AFIX 65 C18 1 0.565815 0.913379 0.748240 31.00000 0.09585 0.08696 = 0.09524 -0.02660 0.00923 0.00958 AFIX 43 H18 2 0.574565 0.944229 0.804576 31.00000 -1.20000 AFIX 65 C17 1 0.501296 0.846035 0.744053 31.00000 0.08187 0.09549 = 0.07409 -0.01224 0.00910 0.01385 AFIX 43 H17 2 0.466878 0.831827 0.797586 31.00000 -1.20000 AFIX 65 C16 1 0.488218 0.799926 0.659853 31.00000 0.06093 0.07895 = 0.06702 -0.01327 0.00488 0.00089 AFIX 43 H16 2 0.445049 0.754869 0.657052 31.00000 -1.20000 AFIX 65 C15 1 0.539659 0.821162 0.579841 31.00000 0.04670 0.06632 = 0.07139 -0.00492 0.00562 0.00399 AFIX 0 C20 1 0.506547 0.642772 0.328882 21.00000 0.05508 0.05440 = 0.06396 0.00098 0.02256 -0.00529 AFIX 43 H20 2 0.458826 0.603516 0.345407 21.00000 -1.20000 AFIX 0 C21 1 0.636050 0.631451 0.321896 21.00000 0.06484 0.05271 = 0.09272 -0.00011 0.03529 -0.00225 AFIX 43 H21 2 0.687284 0.671068 0.310258 21.00000 -1.20000 AFIX 0 PART 0 PART 2 N2A 3 0.606560 0.824845 0.414637 -31.00000 0.05940 0.05195 = 0.08014 -0.00540 0.01558 -0.00189 C11A 1 0.568105 0.835135 0.307583 -31.00000 0.05194 0.05749 = 0.07406 0.03194 0.02261 0.00788 AFIX 43 H11A 2 0.585597 0.874992 0.271783 -31.00000 -1.20000 AFIX 0 C13A 1 0.662536 0.898600 0.459982 -31.00000 0.08658 0.06903 = 0.06072 -0.00531 0.00680 -0.01116 AFIX 23 H13C 2 0.610900 0.936944 0.412636 -31.00000 -1.20000 H13D 2 0.767793 0.903424 0.474986 -31.00000 -1.20000 AFIX 66 C19A 1 0.636295 0.951748 0.637145 -31.00000 0.09344 0.06905 = 0.09446 -0.01460 0.00877 0.00026 AFIX 43 H19A 2 0.675178 0.996404 0.629762 -31.00000 -1.20000 AFIX 65 C18A 1 0.589262 0.938955 0.722187 -31.00000 0.09585 0.08696 = 0.09524 -0.02660 0.00923 0.00958 AFIX 43 H18A 2 0.596678 0.975052 0.771704 -31.00000 -1.20000 AFIX 65 C17A 1 0.531147 0.872211 0.733221 -31.00000 0.08187 0.09549 = 0.07409 -0.01224 0.00910 0.01385 AFIX 43 H17A 2 0.499679 0.863652 0.790121 -31.00000 -1.20000 AFIX 65 C16A 1 0.520064 0.818260 0.659213 -31.00000 0.06093 0.07895 = 0.06702 -0.01327 0.00488 0.00089 AFIX 43 H16A 2 0.481181 0.773604 0.666596 -31.00000 -1.20000 AFIX 65 C15A 1 0.567096 0.831052 0.574170 -31.00000 0.04670 0.06632 = 0.07139 -0.00492 0.00562 0.00399 C14A 1 0.625211 0.897795 0.563134 -31.00000 0.06665 0.07074 = 0.08509 -0.00902 0.00466 0.00683 AFIX 0 C20A 1 0.578125 0.656656 0.355525 -21.00000 0.05508 0.05440 = 0.06396 0.00098 0.02256 -0.00529 AFIX 43 H20A 2 0.666151 0.668652 0.408947 -21.00000 -1.20000 AFIX 0 C21A 1 0.556425 0.595369 0.306399 -21.00000 0.06484 0.05271 = 0.09272 -0.00011 0.03529 -0.00225 AFIX 43 H21A 2 0.465927 0.576650 0.263943 -21.00000 -1.20000 AFIX 0 HKLF 4 REM zzy1062 in P21/n #14 REM R1 = 0.0685 for 2516 Fo > 4sig(Fo) and 0.1041 for all 4038 data REM 321 parameters refined using 45 restraints END WGHT 0.1140 0.3703 REM Highest difference peak 0.289, deepest hole -0.171, 1-sigma level 0.043 Q1 1 0.5574 0.6496 0.5395 11.00000 0.05 0.29 Q2 1 0.6162 0.5422 0.6246 11.00000 0.05 0.29 Q3 1 0.6798 0.5938 0.5962 11.00000 0.05 0.26 Q4 1 0.6271 0.6934 0.4799 11.00000 0.05 0.22 Q5 1 0.6350 0.5302 0.3334 11.00000 0.05 0.21 Q6 1 0.6102 0.8795 0.3976 11.00000 0.05 0.18 Q7 1 0.5906 0.7706 0.3004 11.00000 0.05 0.17 Q8 1 0.6231 0.9390 0.5560 11.00000 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213.442 13 2 15 -4 1075.05 188.784 11 -2 15 3 49.0757 128.023 11 2 15 -3 279.501 156.323 11 -2 15 2 532.559 158.763 11 2 15 -2 522.258 169.262 11 -2 15 1 2173.73 233.708 11 2 15 -1 2136.55 245.843 11 2 15 0 1274.91 214.801 11 2 15 1 6536.48 387.507 11 2 15 2 261.363 149.577 11 -2 15 -2 192.366 172.810 13 -2 15 -3 1528.84 227.964 13 2 15 3 1609.27 213.825 11 -2 15 -4 3798.09 321.162 13 2 15 4 4061.27 301.460 11 -2 15 -5-37.2614 177.426 13 2 15 5 50.0602 114.715 11 -2 15 -6-52.2075 194.743 13 2 15 6 69.4357 111.679 11 -2 15 -7-19.1919 176.680 13 -2 15 -8 66.7354 162.888 13 -2 15 -9 276.237 156.886 13 -2 16 11 48.4545 77.8133 11 2 -16 -11-60.4336 96.0951 12 -2 16 10 339.351 115.054 11 -2 16 9 113.708 121.699 11 -2 16 8-32.6890 129.355 11 2 -16 -8 36.8396 140.243 16 2 -16 -7-66.2107 138.653 16 -2 16 7 130.998 143.749 11 -2 16 6 3245.77 282.216 11 2 -16 -6 3183.26 275.322 16 -2 16 5 4965.94 332.587 11 2 16 -4 1188.46 193.221 11 -2 16 4 865.249 187.556 11 2 16 -3 5090.86 337.266 11 -2 16 3 4185.05 313.170 11 -2 16 2 1569.82 207.074 11 2 16 -2 1707.37 229.955 11 2 16 -1 9569.12 458.459 11 -2 16 1 9228.70 417.730 11 2 16 0 224.168 147.374 11 2 16 1 220.276 148.736 11 -2 16 -2 273.263 175.542 13 2 16 2 443.953 158.213 11 2 16 3 556.266 168.441 11 -2 16 -3 834.976 209.483 13 -2 16 -4 714.128 199.939 13 2 16 4 571.328 162.134 11 -2 16 -5 625.920 200.700 13 2 16 5 1055.08 181.444 11 2 16 6 379.503 137.337 11 -2 16 -6 233.564 181.037 13 -2 16 -7 115.242 164.235 13 -2 16 -8 125.793 152.283 13 -2 16 -9 115.178 124.803 13 -2 17 10 343.630 108.188 11 -2 17 9 102.687 115.520 11 -2 17 8 110.900 131.977 11 -2 17 7 271.081 142.250 11 -2 17 6-71.6075 144.410 11 -2 17 5 632.752 173.994 11 -2 17 4 201.391 142.674 11 2 17 -4 93.4086 122.783 11 -2 17 3 1780.32 229.266 11 2 17 -3 1980.83 230.546 11 2 17 -2 9130.65 443.336 11 -2 17 2 8911.00 418.097 11 2 17 -1 865.365 192.325 11 -2 17 1 939.725 163.346 11 2 17 0 2524.62 272.962 11 2 17 1-51.9420 146.039 11 -2 17 -2 1586.64 226.272 13 2 17 2 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441.015 2 -4 9 3 2483.72 437.400 1 -4 9 2 1741.28 417.309 1 -4 9 1-195.519 294.797 1 -4 9 0 42708.4 1745.46 1 -4 -9 0 45962.0 1608.77 8 -4 -9 -1-125.167 293.564 8 -4 9 -1 140.448 254.477 3 -4 -9 -1 255.171 262.781 6 -4 9 -1-31.2438 250.506 1 -4 9 -2 663.033 302.934 1 -4 -9 -2 747.927 361.745 8 -4 9 -2 694.479 302.964 3 -4 -9 -2 266.381 232.999 6 -4 9 -3 1331.86 495.728 1 -4 -9 -3 960.531 389.099 6 -4 9 -4 279.816 141.839 13 -4 9 -5 935.864 197.292 13 -4 9 -6-118.591 191.701 13 -4 9 -7 20.0920 164.893 13 -4 9 -8 856.809 201.143 13 -4 9 -9 167.540 145.338 13 -4 9 -10 341.459 129.907 13 4 -10 -14 75.3091 96.0531 12 4 10 -14 62.3190 87.9360 17 4 10 -13-61.1890 106.495 17 4 10 -12 45.5932 120.018 17 4 -10 -12-98.8577 141.999 16 4 10 -11 857.318 168.450 17 4 -10 -11 715.586 202.026 16 4 -10 -10 1474.91 243.143 16 4 -10 -9-55.1233 166.175 16 4 -10 -8 2355.41 273.900 16 4 10 -8 2433.15 243.893 11 4 10 -7 5178.31 317.937 11 4 -10 -7 5820.42 367.267 16 4 -10 -6 1787.91 465.306 2 4 -10 -6 2375.43 661.212 8 -4 10 6 949.330 364.549 7 -4 10 5 300.450 295.505 1 -4 10 5 970.143 343.371 7 -4 10 4 3359.35 539.928 1 -4 10 3 1152.38 367.003 1 -4 10 2 6379.91 706.332 1 -4 10 1 11035.0 931.308 1 -4 10 0 164.126 296.347 1 -4 -10 0-181.204 201.703 6 -4 10 -1 1818.50 484.598 1 -4 -10 -1 1215.13 368.371 8 -4 10 -1 611.501 273.851 3 -4 -10 -1 729.703 324.707 6 -4 10 -2 1407.15 412.524 1 -4 -10 -2 1558.39 434.999 8 -4 10 -2 1548.76 409.924 3 -4 10 -3 22.9365 149.186 13 -4 10 -4 8891.57 434.498 13 -4 10 -5 4747.53 340.924 13 -4 10 -6 983.372 209.606 13 -4 10 -7 1901.24 258.974 13 -4 10 -8 366.679 170.914 13 -4 10 -9 772.457 177.834 13 -4 10 -10 16.5966 118.163 13 4 11 -13 73.0665 91.2818 17 -4 11 13 286.231 102.813 11 4 -11 -13 291.982 132.235 12 4 -11 -12 224.935 152.472 16 4 -11 -11 534.050 199.503 16 4 -11 -10 359.309 180.800 16 4 -11 -9 876.133 212.161 16 4 -11 -8 1931.22 256.433 16 4 11 -8 1970.13 220.857 11 4 11 -7 2754.92 253.178 11 4 -11 -7 2922.89 294.556 16 4 -11 -6 432.347 177.275 16 4 11 -6 411.918 151.101 11 4 -11 -5 1620.80 615.459 8 4 11 -5 1080.82 178.211 11 -4 11 4 5685.94 695.467 1 -4 11 3 107.590 262.451 1 -4 11 2 5469.80 698.507 1 -4 11 1 571.768 326.481 1 -4 11 0 415.792 252.188 3 -4 11 0 110.051 316.462 1 -4 11 -1 105.967 267.986 3 -4 11 -2-22.1217 152.677 13 4 11 2 275.844 122.011 11 -4 11 -3 587.677 168.827 13 -4 11 -4 21529.4 668.506 13 -4 11 -5 327.139 169.039 13 -4 11 -6-52.7251 155.162 13 -4 11 -7 971.202 211.440 13 -4 11 -8 1405.48 217.848 13 -4 11 -9 558.145 158.946 13 -4 11 -10-0.81565 95.3563 13 -4 12 13-66.7609 90.4835 11 4 -12 -13 128.908 115.704 12 4 -12 -12 104.182 153.511 16 4 -12 -11 605.805 188.660 16 4 -12 -10 28.5485 182.495 16 4 -12 -9 39.5589 171.345 16 4 12 -8 1052.16 180.654 11 4 -12 -8 1055.37 228.041 16 4 12 -7 2839.00 254.855 11 4 -12 -7 2673.30 278.446 16 4 -12 -6 413.191 177.186 16 4 12 -6 389.055 159.818 11 4 12 -5 2883.35 259.527 11 4 -12 -5 3608.03 301.676 16 4 -12 -4 2176.41 243.846 16 4 12 -4 2199.11 229.926 11 4 12 -3 42.4719 121.485 11 4 12 -2 75.1847 117.853 11 4 12 -1 11217.5 457.182 11 4 12 0 3436.81 269.054 11 -4 12 -1 2850.66 253.694 13 4 12 1 3056.27 258.071 11 4 12 2 1626.26 206.090 11 -4 12 -2 1903.74 234.142 13 -4 12 -3 1024.14 196.964 13 -4 12 -4 3522.44 313.558 13 -4 12 -5 1987.45 253.558 13 -4 12 -6-77.7999 156.728 13 -4 12 -7 207.117 171.008 13 -4 -12 -8-63.7212 107.184 15 -4 12 -8 491.226 172.447 13 -4 12 -9 84.5534 126.509 13 -4 13 12 87.9591 112.569 11 4 -13 -11 22.1210 156.146 16 4 -13 -10-88.2799 156.466 16 4 -13 -9 881.846 196.535 16 4 13 -8 1633.91 201.170 11 4 -13 -8 1351.89 220.029 16 4 13 -7 247.881 137.027 11 4 -13 -7 290.184 160.216 16 4 13 -6 4899.72 326.222 11 4 -13 -6 4363.10 334.513 16 4 -13 -5 984.844 198.731 16 4 13 -5 1238.63 194.715 11 4 13 -4 1878.07 225.690 11 4 -13 -4 2325.51 254.596 16 4 13 -3 3.37888 131.557 11 4 13 -2 5809.60 353.456 11 4 13 -1 375.237 143.087 11 4 13 0 2438.99 244.717 11 4 13 1 1663.47 215.178 11 -4 13 -2 4279.04 318.634 13 4 13 2 4147.77 298.793 11 -4 13 -3 1825.89 233.128 13 4 13 3 2076.32 226.229 11 -4 13 -4 1907.03 246.867 13 -4 13 -5 1331.02 237.725 13 -4 13 -6 45.3077 168.197 13 -4 13 -7 356.337 182.501 13 -4 13 -8 841.138 169.837 13 -4 -13 -8 1016.34 144.134 15 -4 13 -9 318.248 126.568 13 -4 14 12 266.056 107.877 11 -4 14 11 315.359 124.647 11 4 -14 -11 124.077 141.370 16 -4 14 10 338.971 150.438 11 4 -14 -10 470.919 172.523 16 4 -14 -9-50.8615 155.837 16 4 -14 -8 310.041 167.975 16 4 14 -8 604.745 140.348 11 4 14 -7 327.899 145.508 11 4 -14 -7 425.400 164.573 16 4 14 -6 4825.79 323.404 11 4 -14 -6 4374.74 335.419 16 4 -14 -5 1139.27 199.916 16 4 14 -5 1231.34 202.887 11 4 14 -4 3525.59 292.361 11 4 14 -3 717.518 177.053 11 4 14 -2 425.417 152.168 11 4 14 -1 699.751 178.337 11 4 14 0 5322.01 343.503 11 4 14 1 74.0012 118.974 11 4 14 2 433.736 146.714 11 -4 14 -2 586.266 182.220 13 4 14 3 1444.37 194.216 11 -4 14 -3 1372.94 212.797 13 -4 14 -4 1918.24 246.424 13 -4 14 -5 552.740 184.505 13 -4 14 -6 198.505 163.525 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4170.60 319.672 13 -5 8 -5 5783.39 360.711 13 -5 -8 -6 1902.88 213.183 15 -5 8 -6 2013.36 245.652 13 -5 -8 -7 1643.28 219.781 10 -5 8 -7 1263.26 211.941 13 -5 -8 -8-94.6658 118.296 10 -5 8 -8-37.2200 155.329 13 -5 8 -9-66.6178 122.062 13 -5 8 -10 317.140 101.340 13 5 -9 -14 401.568 104.521 12 5 9 -14 484.879 121.978 17 5 9 -13 445.196 132.259 17 5 -9 -13 472.298 149.458 16 5 9 -12 212.294 132.320 17 5 -9 -12 320.621 156.847 16 5 9 -11 188.876 123.107 17 5 -9 -11 403.716 165.434 16 5 9 -10 885.044 171.740 17 5 -9 -10 348.517 194.092 16 5 -9 -9 1448.66 236.514 16 5 9 -9 1338.83 197.274 11 5 -9 -8 2443.39 277.156 16 5 9 -8 2399.08 238.359 11 5 -9 -7 122.534 159.435 16 5 9 -7 562.199 155.454 11 5 -9 -6 4032.33 633.175 2 -5 9 6 5337.73 698.025 7 5 9 -6 4710.53 305.676 11 5 -9 -6 4044.24 310.324 16 -5 9 5 4868.49 638.221 7 5 -9 -5 5001.08 687.135 2 5 -9 -4 280.917 312.925 2 -5 9 4 263.159 280.790 1 -5 9 3 2915.55 532.447 1 5 9 -2 15839.5 1061.87 5 -5 9 2 16168.6 1136.30 1 -5 9 1 2204.24 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4 -8 1043.53 140.485 13 7 5 -14-66.4625 117.639 17 7 5 -13 398.468 149.049 17 7 -5 -13 336.418 120.161 17 7 5 -12 319.780 150.381 17 7 -5 -12 366.229 137.741 17 7 -5 -11 754.107 178.922 16 7 5 -11 735.728 182.309 14 7 5 -11 849.480 182.621 17 7 -5 -10 2262.45 258.721 16 7 5 -10 1987.11 244.766 14 7 -5 -9 1833.61 245.963 16 7 5 -9 2160.46 252.331 14 7 5 -8 3998.53 326.537 14 7 -5 -8 3942.69 338.021 16 7 -5 -7 424.403 196.630 16 -7 -5 6 31.4533 114.003 15 7 5 -6 135.500 128.859 11 -7 5 5-74.1156 130.831 15 -7 -5 5 56.0122 124.057 15 7 5 -5 157.513 123.835 11 -7 5 4-51.5740 129.452 15 7 5 -4-420.236 322.450 5 -7 -5 4 10.0826 122.679 15 -7 5 3 168.167 142.119 15 -7 -5 3 34.8301 118.895 15 -7 5 2 3382.16 271.307 15 -7 -5 2 3371.53 268.144 15 -7 5 1 981.804 165.865 15 -7 -5 1 1113.94 184.522 15 -7 -5 0 1326.82 206.357 15 -7 -5 -1 127.239 132.569 15 -7 5 -1-666.686 168.004 13 -7 -5 -2 11460.4 464.005 15 -7 5 -2 10741.2 484.796 13 -7 5 -3 305.844 147.933 10 -7 -5 -3 499.085 150.279 15 -7 5 -3 180.332 143.635 13 -7 5 -4 1432.89 208.746 10 -7 -5 -4 1348.50 181.447 15 -7 -5 -4 1588.89 217.295 10 -7 5 -4 1374.57 211.416 13 -7 5 -5 252.940 144.975 10 -7 -5 -5 20.8180 128.307 10 -7 5 -5 156.365 166.318 13 -7 -5 -6 738.859 162.036 10 -7 5 -6 979.332 194.962 13 -7 -5 -7 979.274 160.073 10 -7 5 -7 559.436 147.687 13 -7 -5 -8 60.3224 97.0541 10 -7 5 -8-148.178 109.918 13 7 6 -14 177.576 117.998 17 7 6 -13 14.5987 118.866 17 7 6 -12 1062.91 187.337 17 7 -6 -12 1154.70 188.575 16 7 -6 -11 506.879 177.162 16 7 6 -11 332.864 150.200 14 7 6 -11 544.808 176.142 17 7 -6 -10 1715.45 234.520 16 7 6 -10 1908.58 236.225 14 7 6 -10 2081.50 238.796 17 7 6 -9 4716.02 337.694 14 7 -6 -9 4564.59 341.770 16 7 -6 -8 793.655 212.585 16 7 6 -8 1380.88 235.319 14 7 -6 -7 314.352 211.332 16 7 6 -7 83.2074 123.790 11 7 6 -6 1452.62 208.444 11 -7 -6 5 1996.76 211.438 15 7 6 -5 2010.74 221.353 11 -7 6 4 1478.24 202.700 15 -7 -6 4 1410.10 199.819 15 7 6 -4 1429.96 187.547 11 -7 6 3 1514.77 209.123 15 -7 -6 3 1337.78 195.716 15 7 6 -3 1165.13 173.045 11 -7 6 2 340.290 176.183 15 -7 -6 2 191.453 133.538 15 -7 6 1 233.581 132.450 15 -7 -6 1 338.245 161.475 15 -7 -6 0 312.230 171.334 15 -7 6 0 29.1468 124.620 13 -7 -6 -1 574.483 166.877 15 -7 6 -1 834.326 179.121 13 -7 -6 -2 1336.20 202.455 15 -7 6 -2 1446.32 211.257 13 -7 -6 -3 3282.65 268.798 15 -7 6 -3 4129.09 309.074 10 -7 6 -3 3768.69 302.534 13 -7 6 -4 2230.21 239.742 10 -7 -6 -4 1807.33 204.437 15 -7 6 -4 2075.05 252.411 13 -7 -6 -5 416.539 153.122 10 -7 6 -5 278.514 172.959 13 -7 -6 -6 240.283 129.347 10 -7 6 -6 892.506 194.027 13 -7 -6 -7 154.318 115.167 10 -7 6 -7-148.947 141.870 13 7 7 -14 173.236 98.5304 17 7 7 -13-190.674 121.262 17 7 7 -12 1169.97 179.745 17 7 -7 -12 1243.50 193.026 16 7 -7 -11 367.110 170.473 16 7 7 -11 173.009 142.032 14 7 7 -11 261.457 143.722 17 7 7 -10 2298.44 243.653 14 7 7 -10 2094.71 233.276 17 7 -7 -10 2540.55 281.557 16 7 -7 -9 470.000 181.919 16 7 7 -9 790.636 183.312 14 7 7 -9 607.736 163.684 17 7 7 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154.053 16 8 6 -9-157.278 167.045 14 8 -6 -8-30.0897 176.918 16 8 6 -8 136.519 186.756 14 8 -6 -7 2311.43 276.968 16 -8 -6 6 1031.61 174.716 15 -8 -6 5 118.580 133.805 15 8 6 -5 331.319 140.254 11 -8 -6 4 509.492 164.806 15 8 6 -4 539.679 152.206 11 -8 6 3 1502.46 223.311 15 -8 -6 3 1101.43 192.819 15 -8 6 2 3527.65 282.609 15 -8 -6 2 3038.08 277.691 15 -8 6 1 3068.77 256.117 15 -8 -6 1 2999.78 275.443 15 -8 -6 0 229.348 155.125 15 -8 6 0-161.289 141.542 13 -8 -6 -1 1693.22 220.493 15 -8 6 -1 2021.15 231.737 13 -8 -6 -2 1944.06 219.822 15 -8 6 -2 1828.49 227.797 13 -8 -6 -3-0.28210 122.018 15 -8 -6 -3-54.3062 130.897 10 -8 6 -3 214.447 156.658 13 -8 -6 -4 418.264 125.917 15 -8 -6 -4 298.437 135.472 10 -8 6 -4 499.471 163.357 13 -8 -6 -5 97.6014 115.194 10 -8 6 -5 309.617 142.955 13 -8 -6 -6-46.9830 93.6692 10 -8 6 -6-142.895 122.101 13 -8 -6 -6 4.98278 91.0869 13 8 7 -13 706.652 130.861 17 8 7 -12 648.998 135.128 17 8 -7 -12 570.891 146.744 16 8 -7 -11-57.0656 137.223 16 8 7 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8 -9 -10 2204.38 249.130 16 8 9 -10 1972.05 201.822 14 8 -9 -9-97.4202 182.094 16 8 9 -9 205.889 141.785 14 8 -9 -8-180.875 193.067 16 8 9 -8 93.3985 137.668 14 8 -9 -7 148.191 173.581 16 8 9 -7 210.295 147.535 14 8 9 -7 160.847 139.540 11 8 -9 -6 1055.77 220.129 16 8 9 -6 1455.13 218.563 14 8 9 -6 1012.80 187.116 11 8 -9 -5 641.273 213.725 16 -8 -9 5 317.787 131.952 15 8 9 -5 417.184 150.774 11 8 -9 -4 642.641 211.543 16 -8 -9 4 697.934 162.377 15 8 9 -4 515.215 141.459 11 -8 -9 3 3006.47 262.535 15 8 9 -3 2553.51 229.185 11 -8 -9 2 3899.66 293.567 15 -8 -9 1 109.360 141.785 15 -8 -9 0 43.1767 147.139 15 -8 -9 -1 16.8461 142.531 15 -8 9 -1 7.79800 129.019 13 -8 -9 -2 158.992 146.712 15 -8 9 -2-150.232 148.255 13 -8 -9 -3 317.191 133.114 15 -8 9 -3 7.58913 134.462 13 -8 -9 -4 681.520 130.751 15 -8 -9 -4 564.534 140.019 10 -8 9 -4 761.595 151.040 13 -8 -9 -5-33.9773 91.8778 10 -8 9 -5 148.348 106.574 13 8 -10 -12-116.483 107.319 16 8 -10 -11 72.4066 127.673 16 8 -10 -10 197.707 156.929 16 8 -10 -9 630.894 203.932 16 8 -10 -8-174.100 192.462 16 8 -10 -7 1687.39 247.575 16 8 10 -7 1524.39 213.316 11 8 -10 -6 86.9754 181.176 16 8 10 -6 95.8404 136.855 11 8 -10 -5 2294.98 270.695 16 -8 -10 5 2284.49 218.786 15 8 10 -5 2491.25 238.955 11 8 -10 -4 31.7957 151.895 16 -8 -10 4 13.0874 122.368 15 8 10 -4-12.5775 115.259 11 8 -10 -3 659.369 194.100 16 -8 -10 3 477.357 154.561 15 8 10 -3 393.002 129.525 11 8 -10 -2 129.290 158.314 16 -8 -10 2 339.355 149.324 15 8 -10 -1 115.479 138.233 16 -8 -10 1 7.02212 136.818 15 -8 -10 0 140.146 153.474 15 -8 -10 -1 69.2740 141.833 15 -8 -10 -2 1677.62 205.057 15 -8 10 -2 1474.78 185.641 13 -8 -10 -3 730.108 151.459 15 -8 10 -3 701.211 152.125 13 -8 -10 -4 302.303 105.972 15 -8 -10 -4 46.4407 103.626 10 -8 10 -4 263.267 121.061 13 8 -11 -11-128.893 120.898 16 8 -11 -10 123.318 146.011 16 8 -11 -9 1034.26 202.865 16 8 -11 -8 90.6841 165.564 16 8 -11 -7 304.917 179.844 16 8 11 -7 514.176 158.704 11 8 -11 -6 99.3615 170.832 16 8 11 -6-0.64335 130.697 11 8 -11 -5 470.597 188.929 16 8 11 -5 176.201 134.309 11 8 -11 -4 778.052 192.595 16 -8 -11 4 578.224 144.874 15 8 11 -4 692.854 155.916 11 8 -11 -3 461.067 169.570 16 -8 -11 3 89.1841 128.704 15 8 11 -3 301.556 128.670 11 8 -11 -2 81.7948 143.684 16 -8 -11 2 154.507 132.960 15 -8 -11 1 939.072 184.110 15 -8 -11 0 501.603 165.032 15 -8 -11 -1 74.5902 133.600 15 -8 -11 -2 54.6272 125.687 15 -8 11 -2 53.5860 115.301 13 -8 -11 -3-166.441 118.139 15 -8 11 -3 132.963 115.115 13 -8 -11 -4 134.520 76.3443 15 -8 -11 -4 13.6505 94.9488 10 8 -12 -11-18.7819 106.195 16 8 -12 -10 29.1512 128.367 16 8 -12 -9 360.250 157.748 16 8 -12 -8 187.690 154.557 16 8 -12 -7 407.656 165.619 16 8 12 -7 6.79838 122.261 11 8 -12 -6-87.0901 166.468 16 8 12 -6 134.187 125.419 11 8 -12 -5-160.154 157.140 16 8 12 -5-209.575 131.822 11 8 -12 -4 49.1547 144.226 16 -8 -12 4-119.320 117.420 15 8 12 -4 124.480 114.206 11 8 -12 -3 1347.25 208.445 16 -8 -12 3 1105.02 171.668 15 8 12 -3 991.139 157.635 11 -8 -12 2 1595.70 196.583 15 -8 -12 1 544.474 157.536 15 -8 -12 0 218.113 136.923 15 -8 -12 -1 75.8999 126.483 15 -8 -12 -2 12.0792 117.375 15 -8 -12 -3-185.284 111.034 15 -8 -12 -3-158.449 116.718 10 8 -13 -10-58.7341 108.496 16 8 -13 -9 427.138 140.873 16 8 -13 -8 385.770 151.514 16 8 -13 -7 211.847 151.747 16 8 13 -7 79.1116 116.376 11 8 -13 -6 303.611 166.804 16 8 13 -6 110.332 124.051 11 8 -13 -5-235.698 152.309 16 8 13 -5-135.240 121.692 11 8 -13 -4 396.651 148.827 16 -8 -13 4 392.953 117.658 15 8 13 -4 371.730 126.876 11 -8 -13 3 1148.60 162.934 15 8 13 -3 1430.69 169.714 11 -8 -13 2 195.250 123.211 15 -8 -13 1 278.970 134.127 15 -8 -13 0 154.979 127.406 15 -8 -13 -1 510.869 144.344 15 -8 -13 -2 235.711 110.903 15 8 -14 -9 69.4012 107.912 16 8 -14 -8 19.9981 112.131 16 8 -14 -7 352.319 138.568 16 8 -14 -6 46.1076 116.302 16 8 14 -6-34.3463 107.448 11 8 -14 -5 230.043 127.576 16 8 14 -5 82.5805 111.726 11 8 14 -4 116.157 103.430 11 -8 -14 3 34.3719 99.6006 15 8 14 -3 166.770 105.588 11 -8 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78.7383 120.661 13 -9 -1 -4-30.3200 122.126 13 -9 -1 -5 173.625 97.4164 10 -9 1 -5 197.740 107.425 13 -9 -1 -5 112.275 100.080 13 9 2 -13 683.217 146.818 17 9 -2 -13 559.882 133.434 17 9 2 -12 1078.56 191.241 17 9 -2 -12 730.163 163.128 17 9 -2 -11 498.672 140.187 14 9 2 -11 699.033 174.258 14 9 -2 -10 259.641 142.072 14 9 2 -10 195.801 164.643 14 9 -2 -9 684.628 169.703 16 9 -2 -9 701.303 173.702 14 9 2 -9 831.180 208.079 14 9 -2 -8 489.541 184.172 16 -9 -2 8 579.968 155.454 15 9 -2 -8 1108.12 202.695 14 9 2 -8 970.825 227.206 14 -9 2 7 1535.07 222.753 15 -9 -2 7 1144.25 190.547 15 -9 2 6 364.688 163.536 15 -9 -2 6 405.519 163.465 15 -9 2 5 1475.47 216.798 15 -9 -2 5 1844.23 225.625 15 -9 2 4 5694.79 350.950 15 -9 -2 4 5412.17 344.091 15 -9 2 3 154.672 146.380 15 -9 -2 3 17.7201 141.385 15 -9 2 2 158.453 146.688 15 -9 -2 2 66.4385 137.147 15 -9 2 1 33.5964 131.588 15 -9 -2 1 185.291 144.454 15 -9 2 0 425.914 149.850 15 -9 -2 0 869.033 182.188 15 -9 -2 -1 127.364 126.901 15 -9 -2 -1 241.911 120.808 10 -9 2 -1 148.531 139.012 13 -9 -2 -2 852.319 155.990 15 -9 -2 -2 805.754 155.855 10 -9 2 -2 529.508 156.311 13 -9 2 -3 676.551 146.045 10 -9 -2 -3 447.146 127.376 10 -9 2 -3 343.297 146.047 13 -9 2 -4 443.374 122.069 10 -9 -2 -4 822.506 143.992 10 -9 2 -4 390.271 140.129 13 -9 -2 -4 535.206 148.584 13 9 3 -13 19.4505 106.962 17 9 -3 -13 83.1449 101.072 17 9 3 -12 81.3350 129.852 17 9 -3 -12 123.993 127.296 17 9 -3 -11-98.5374 126.092 14 9 3 -11 97.7652 163.843 14 9 -3 -10 1397.99 198.039 16 9 -3 -10 1054.99 171.152 14 9 3 -10 1222.83 216.298 14 9 -3 -9 3721.96 281.944 14 9 3 -9 4047.60 328.830 14 9 -3 -9 4135.78 303.145 16 9 -3 -8 23.0762 155.002 16 -9 -3 8 30.1498 124.098 15 9 -3 -8 57.8999 143.288 14 9 3 -8 93.3434 174.637 14 -9 -3 7 2297.80 232.179 15 9 -3 -7 2337.78 256.157 14 -9 -3 6 2450.63 248.756 15 -9 3 6 2426.46 257.110 15 -9 3 5 356.022 180.336 15 -9 -3 5 422.631 159.761 15 -9 3 4 163.442 160.179 15 -9 -3 4-133.062 140.732 15 -9 3 3 897.679 192.484 15 -9 -3 3 921.759 194.551 15 -9 3 2 1997.87 227.572 15 -9 -3 2 1738.00 224.296 15 -9 3 1 1057.54 186.256 15 -9 -3 1 805.843 179.055 15 -9 3 0 159.920 123.733 15 -9 -3 0 255.233 148.278 15 -9 -3 0 398.615 136.232 10 -9 3 0 226.571 135.605 13 -9 -3 -1 535.683 152.309 15 -9 -3 -1 380.525 134.452 10 -9 3 -1 640.920 164.657 13 -9 -3 -2 56.0191 108.548 15 -9 -3 -2 263.502 120.738 10 -9 3 -2 195.909 133.064 13 -9 3 -3 1670.39 184.362 10 -9 -3 -3 1362.88 174.390 10 -9 3 -3 1214.53 184.474 13 -9 -3 -4 305.322 113.315 10 -9 3 -4 520.985 137.692 13 -9 -3 -4 224.798 121.213 13 9 4 -13-86.4953 112.359 17 9 -4 -13 40.0674 85.3126 17 9 4 -12-61.6597 119.018 17 9 -4 -12 222.832 125.248 17 9 4 -11 14.8839 162.704 14 9 4 -11 518.275 161.471 17 9 -4 -10-240.799 156.129 16 9 -4 -10-93.2085 128.894 14 9 4 -10-129.204 176.414 14 9 -4 -9 67.7752 152.967 16 9 -4 -9 373.288 152.826 14 9 4 -9 145.452 177.409 14 9 -4 -8 288.536 175.106 16 9 -4 -8 97.0440 134.757 14 9 4 -8 180.430 194.041 14 9 -4 -7 448.432 188.126 16 -9 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9 -5 -9 402.511 176.449 16 9 5 -9 48.1350 158.051 14 9 5 -8 2980.75 300.773 14 9 -5 -8 2689.17 282.620 16 9 -5 -7 1731.39 263.897 16 -9 -5 7 1311.96 187.041 15 -9 -5 6 263.084 141.884 15 -9 -5 5 290.313 151.442 15 -9 -5 4 265.893 154.199 15 -9 5 3 973.219 190.634 15 -9 -5 3 617.250 172.489 15 -9 5 2 114.604 147.797 15 -9 -5 2 30.6522 146.766 15 -9 5 1 3367.25 259.314 15 -9 -5 1 2947.57 263.466 15 -9 -5 0 671.825 165.179 15 -9 5 0 670.175 159.064 13 -9 -5 -1 44.6688 125.099 15 -9 -5 -1-109.295 124.975 10 -9 5 -1-183.485 136.163 13 -9 -5 -2 910.411 152.553 15 -9 -5 -2 914.137 156.978 10 -9 5 -2 1338.44 188.415 13 -9 -5 -3 427.597 115.111 15 -9 -5 -3 334.778 120.563 10 -9 5 -3 589.169 148.750 13 -9 -5 -4 134.748 103.219 10 -9 5 -4 218.772 117.758 13 9 6 -12 55.4847 98.3236 17 9 -6 -12 225.552 99.0705 17 9 -6 -11 197.116 132.104 16 9 6 -11 59.8798 133.306 14 9 6 -11 33.4214 107.445 17 9 -6 -10 88.0009 142.549 16 9 6 -10 128.166 151.045 14 9 6 -10 96.6206 124.486 17 9 -6 -9 21.6949 160.340 16 9 6 -9 128.347 153.002 14 9 -6 -8 886.769 203.963 16 9 6 -8 876.196 201.603 14 9 -6 -7 282.081 192.212 16 -9 -6 7 395.175 140.699 15 9 6 -7 505.441 204.917 14 -9 -6 6 2928.79 253.274 15 9 -6 -6 3292.20 312.260 16 -9 -6 5 1139.21 193.842 15 -9 -6 4 198.771 147.543 15 -9 -6 3 431.172 159.355 15 -9 -6 2 6050.91 356.322 15 -9 -6 1-195.601 164.104 15 -9 -6 0 339.362 155.229 15 -9 6 0 292.571 140.041 13 -9 -6 -1 418.584 145.328 15 -9 -6 -1 450.978 132.580 10 -9 6 -1 484.420 144.414 13 -9 -6 -2 263.408 125.764 15 -9 -6 -2 540.615 137.701 10 -9 6 -2 691.989 156.416 13 -9 -6 -3-124.515 90.4165 15 -9 -6 -3-33.2659 105.093 10 -9 -6 -4 204.940 101.385 10 -9 6 -4-90.8536 110.350 13 9 7 -12 335.003 102.202 17 9 -7 -12 293.285 106.087 16 9 -7 -11 3.59438 117.019 16 9 7 -11-224.323 135.042 14 9 7 -11 6.46916 93.3089 17 9 -7 -10-14.7287 136.096 16 9 7 -10-28.4047 145.402 14 9 7 -10 158.114 116.781 17 9 -7 -9-122.444 163.137 16 9 7 -9-11.9136 147.753 14 9 -7 -8 1486.81 234.242 16 9 7 -8 1821.03 235.741 14 9 -7 -7 398.615 207.046 16 9 7 -7 527.627 189.124 14 9 -7 -6 344.310 198.569 16 -9 -7 6 290.385 134.338 15 9 -7 -5 432.446 195.203 16 -9 -7 5 418.611 141.409 15 -9 -7 4 89.1528 134.466 15 -9 -7 3 178.219 145.408 15 -9 -7 2 2241.26 241.420 15 -9 -7 1 1197.38 204.073 15 -9 -7 0 850.170 181.001 15 -9 -7 -1 471.404 148.204 15 -9 -7 -1 329.228 128.793 10 -9 -7 -2 374.912 132.456 15 -9 -7 -2 202.411 114.286 10 -9 7 -2 343.629 133.853 13 -9 -7 -3-149.183 92.2311 15 -9 -7 -3-78.7216 101.797 10 -9 7 -3-173.888 127.310 13 9 -8 -12 284.391 96.8209 16 9 -8 -11 174.705 119.990 16 9 -8 -10 105.850 141.739 16 9 8 -10-198.431 136.957 14 9 -8 -9 477.614 172.150 16 9 8 -9 385.270 153.462 14 9 -8 -8-60.7358 168.130 16 9 8 -8 401.512 158.597 14 9 -8 -7 2557.86 279.892 16 9 8 -7 3203.98 280.196 14 9 -8 -6 171.110 183.239 16 -9 -8 6 186.312 121.645 15 9 -8 -5 121.853 175.552 16 -9 -8 5 149.361 130.409 15 9 -8 -4 396.521 202.217 16 -9 -8 4 150.266 137.900 15 -9 -8 3 18.1945 135.050 15 -9 -8 2 361.801 163.709 15 -9 -8 1 271.454 151.684 15 -9 -8 0-66.5852 140.517 15 -9 -8 -1 184.403 132.101 15 -9 8 -1-1.78037 115.024 13 -9 -8 -2-42.5726 107.574 15 -9 -8 -2-191.245 116.680 10 -9 8 -2-325.530 132.398 13 -9 -8 -3 662.911 101.938 15 -9 -8 -3 923.764 142.817 10 -9 8 -3 1027.88 142.403 13 9 -9 -11 558.303 133.744 16 9 -9 -10 287.731 144.646 16 9 9 -10-67.0043 114.054 14 9 -9 -9 447.589 165.109 16 9 9 -9 15.9232 123.386 14 9 -9 -8 481.691 187.681 16 9 9 -8 532.839 146.813 14 9 -9 -7 311.684 184.204 16 9 9 -7 424.390 154.714 14 -9 -9 6 329.816 124.528 15 9 9 -6 578.627 175.706 14 9 -9 -5 65.8777 161.599 16 -9 -9 5 81.2957 120.894 15 9 -9 -4 215.059 175.626 16 -9 -9 4 57.3975 122.672 15 9 -9 -3 443.323 169.750 16 -9 -9 3 510.576 157.657 15 9 -9 -2 407.548 168.779 16 -9 -9 2 301.758 149.134 15 9 -9 -1 1399.82 199.916 16 -9 -9 1 874.817 174.843 15 -9 -9 0 156.247 135.108 15 -9 -9 -1 109.781 125.154 15 -9 -9 -2-65.8353 104.136 15 -9 -9 -2-23.4221 103.376 10 -9 9 -2-32.9616 101.181 13 9 -10 -10-47.9408 121.486 16 9 -10 -9 13.7200 136.292 16 9 -10 -8 182.432 160.961 16 9 -10 -7 53.8554 165.669 16 9 -10 -6 47.7932 158.820 16 9 -10 -5 155.252 167.937 16 -9 -10 5 221.049 126.785 15 9 -10 -4 302.027 162.744 16 -9 -10 4-67.8904 122.038 15 9 -10 -3 213.390 153.607 16 -9 -10 3-121.072 134.011 15 9 -10 -2 456.874 156.185 16 -9 -10 2 401.926 149.146 15 9 -10 -1 742.346 152.621 16 -9 -10 1 759.384 168.308 15 -9 -10 0 1023.16 166.940 15 -9 -10 -1 115.404 118.963 15 -9 -10 -2 40.4803 93.8181 15 -9 -10 -2-21.9051 93.0608 10 9 -11 -10 51.2158 107.192 16 9 -11 -9 2.56638 121.898 16 9 -11 -8 312.844 146.899 16 9 -11 -7 1133.08 181.354 16 9 -11 -6-82.8977 140.102 16 9 -11 -5-260.541 160.763 16 -9 -11 5-6.65591 98.4684 15 9 -11 -4 453.407 158.327 16 -9 -11 4 177.511 117.231 15 9 -11 -3 1546.31 200.468 16 -9 -11 3 1291.48 173.343 15 9 -11 -2 351.716 132.006 16 -9 -11 2 566.917 142.807 15 -9 -11 1 91.4223 119.662 15 -9 -11 0-112.101 114.940 15 -9 -11 -1-91.7257 98.5019 15 9 -12 -9 29.0904 106.872 16 9 -12 -8 695.209 154.203 16 9 -12 -7 929.204 164.078 16 9 -12 -6 105.909 129.423 16 9 -12 -5-196.012 131.473 16 9 -12 -4 94.1544 122.864 16 -9 -12 4 74.2963 94.2409 15 9 -12 -3 119.593 122.205 16 -9 -12 3-12.6595 101.038 15 -9 -12 2 652.927 135.506 15 -9 -12 1 525.602 127.336 15 -9 -12 0 162.973 102.415 15 9 -13 -7 253.443 115.943 16 9 -13 -6 201.143 119.075 16 9 -13 -5 274.707 112.331 16 9 -13 -4 466.232 122.741 16 -9 -13 4 582.160 107.404 15 -9 -13 3 321.577 105.971 15 -9 -13 2-100.219 97.7932 15 10 0 -12 453.804 130.327 17 10 0 -11-0.24570 118.817 14 10 0 -10 92.8963 128.666 14 10 0 -9 151.754 151.537 14 10 0 -8 798.394 185.899 14 -10 0 7 190.278 149.522 15 10 0 -7 372.473 171.272 14 -10 0 6 914.098 190.053 15 -10 0 5-14.3936 147.913 15 -10 0 4 150.473 156.154 15 -10 0 3 2.77632 139.720 15 -10 0 2 3055.26 255.660 15 -10 0 1-93.4981 132.833 15 -10 0 0 202.238 120.857 15 -10 0 -1-176.720 129.520 13 -10 0 -2 955.416 146.153 13 10 1 -12 829.221 144.747 17 10 -1 -12 793.042 148.825 17 10 -1 -11 414.849 125.450 14 10 1 -11 290.649 126.571 14 10 -1 -10 575.356 147.157 14 10 1 -10 440.708 144.404 14 10 -1 -9 130.750 137.519 14 10 1 -9 109.296 145.480 14 10 -1 -8 389.680 152.903 16 -10 -1 8 528.823 149.891 15 10 -1 -8 531.668 162.587 14 10 1 -8 725.669 192.730 14 10 -1 -7 280.694 172.445 16 -10 1 7-20.7185 144.388 15 -10 -1 7 182.750 140.721 15 10 -1 -7 191.172 160.032 14 -10 1 6 253.298 159.348 15 -10 -1 6 79.9990 141.087 15 -10 1 5-46.6098 155.054 15 -10 -1 5 114.071 157.350 15 -10 1 4 430.025 174.716 15 -10 -1 4 303.431 166.188 15 -10 1 3 35.8039 146.259 15 -10 -1 3 161.988 156.586 15 -10 1 2 11.7310 132.069 15 -10 -1 2 389.021 151.834 15 -10 1 1 979.066 169.934 15 -10 -1 1 913.827 169.056 15 -10 1 1 678.110 144.149 13 -10 1 0-89.3097 116.601 15 -10 -1 0 117.893 110.188 15 -10 1 0-76.7848 124.013 13 -10 -1 -1 190.764 108.301 15 -10 1 -1-57.6198 117.025 13 -10 1 -2 37.1192 104.692 13 -10 -1 -2-49.3980 112.364 13 10 2 -12-8.32139 102.195 17 10 -2 -12 138.305 103.897 17 10 -2 -11 0.22228 109.848 14 10 2 -11-0.50178 128.965 14 10 -2 -10 35.7467 117.892 14 10 2 -10-42.6366 147.480 14 10 -2 -9-144.862 137.810 16 10 -2 -9 103.708 129.873 14 10 2 -9 40.9308 145.856 14 10 -2 -8 479.530 166.686 16 -10 -2 8 266.231 139.353 15 10 -2 -8 116.230 132.649 14 10 2 -8 353.236 186.893 14 10 -2 -7 404.949 165.504 16 -10 -2 7 345.397 146.456 15 10 -2 -7 740.991 179.233 14 -10 2 6 1236.73 206.714 15 -10 -2 6 1635.48 215.139 15 -10 2 5 316.687 171.898 15 -10 -2 5 168.337 147.988 15 -10 2 4 36.7788 146.806 15 -10 -2 4 137.627 152.722 15 -10 2 3 24.1204 135.620 15 -10 -2 3 26.0133 143.172 15 -10 2 2 42.1967 129.504 15 -10 -2 2 104.170 135.403 15 -10 2 1 47.7312 117.774 15 -10 -2 1 232.247 142.627 15 -10 2 1-227.794 127.910 13 -10 -2 0 6.91332 114.613 15 -10 2 0-116.573 120.670 13 -10 -2 -1 194.521 107.881 15 -10 2 -1-27.8612 106.657 13 -10 -2 -2 197.568 100.994 10 -10 2 -2 270.790 118.487 13 -10 -2 -2-46.9001 114.297 13 10 3 -12 402.910 116.841 17 10 -3 -12 802.089 133.695 17 10 3 -11 8.02323 126.390 14 10 3 -11 554.203 137.791 17 10 -3 -10 40.6429 110.032 14 10 3 -10 249.798 140.767 14 10 -3 -9-153.375 141.728 16 10 -3 -9-125.667 116.737 14 10 3 -9 241.990 160.181 14 10 -3 -8 523.456 169.229 16 -10 -3 8 622.279 148.803 15 10 -3 -8 676.673 157.831 14 10 3 -8 547.088 179.302 14 10 -3 -7 1350.36 215.374 16 -10 -3 7 1289.54 190.038 15 10 -3 -7 1295.14 188.277 14 10 3 -7 1389.99 244.647 14 -10 -3 6 108.023 139.809 15 -10 3 5 131.205 155.031 15 -10 -3 5 135.575 143.111 15 -10 3 4 632.547 173.032 15 -10 -3 4 740.667 182.818 15 -10 3 3 323.872 150.085 15 -10 -3 3 241.535 158.000 15 -10 3 2 188.080 131.906 15 -10 -3 2 313.472 158.378 15 -10 3 1 425.812 137.096 15 -10 -3 1 303.135 140.638 15 -10 -3 0 130.956 117.791 15 -10 3 0 283.211 117.387 13 -10 -3 -1 125.311 101.013 15 -10 3 -1 214.058 114.115 13 -10 -3 -2 300.453 103.518 10 -10 3 -2 126.928 105.516 13 -10 -3 -2 191.658 107.509 13 10 4 -11-111.644 129.820 14 10 4 -11 420.479 126.837 17 10 -4 -10-134.082 122.210 16 10 4 -10-170.795 152.258 14 10 4 -10 261.109 132.730 17 10 -4 -9-139.015 136.287 16 10 4 -9-224.083 159.909 14 10 -4 -8 54.3577 156.196 16 -10 -4 8 41.1169 109.300 15 10 4 -8 219.665 171.272 14 10 -4 -7 824.732 193.653 16 -10 -4 7 543.473 145.810 15 10 4 -7 939.657 213.298 14 10 -4 -6 550.454 187.717 16 -10 -4 6 220.152 143.391 15 -10 -4 5-190.176 146.706 15 -10 -4 4 351.422 159.118 15 -10 -4 3 222.213 151.891 15 -10 -4 2 506.617 161.431 15 -10 -4 1 795.136 160.784 15 -10 -4 0-37.2047 118.042 15 -10 4 0 178.079 106.532 13 -10 -4 -1 190.654 106.268 15 -10 -4 -1 51.1520 87.1507 10 -10 4 -1 265.400 109.138 13 -10 -4 -2-31.0808 81.9617 10 -10 4 -2 228.558 106.365 13 10 5 -11 34.2409 116.436 14 10 5 -11-7.06084 90.3076 17 10 -5 -10 374.814 129.345 16 10 5 -10 524.059 130.867 17 10 -5 -9 217.149 138.987 16 10 5 -9 176.574 154.416 14 10 -5 -8-65.1502 151.586 16 10 5 -8 215.499 165.869 14 10 -5 -7 458.346 178.884 16 -10 -5 7 336.936 135.381 15 10 5 -7 439.589 180.640 14 10 -5 -6 410.910 179.803 16 -10 -5 6 301.004 142.292 15 -10 -5 5 83.0701 137.166 15 -10 -5 4-184.317 145.593 15 -10 -5 3 162.697 138.596 15 -10 -5 2 233.261 140.796 15 -10 -5 1 79.4997 128.661 15 -10 -5 0 228.113 126.710 15 -10 -5 0 237.876 99.2127 10 -10 -5 -1 242.001 107.020 15 -10 -5 -1 327.539 105.356 10 -10 5 -1 509.539 116.194 13 10 -6 -11 80.5805 91.5846 16 10 -6 -11 79.0147 78.9328 17 10 -6 -10 65.9296 120.667 16 10 6 -10-90.4196 130.724 14 10 -6 -9-216.752 148.640 16 10 6 -9-200.321 140.360 14 10 -6 -8 261.539 151.880 16 10 6 -8 602.571 173.380 14 10 -6 -7 277.531 165.217 16 -10 -6 7 23.8815 109.730 15 10 -6 -6 659.720 200.854 16 -10 -6 6 130.572 120.812 15 10 -6 -5 439.022 191.606 16 -10 -6 5 496.674 153.198 15 -10 -6 4 195.356 146.028 15 -10 -6 3 73.3725 137.515 15 -10 -6 2 218.708 134.041 15 -10 -6 1 141.635 126.438 15 -10 -6 0 153.720 118.118 15 -10 -6 0 151.638 96.9408 10 -10 -6 -1 152.430 97.1206 15 -10 -6 -1-80.4729 83.3549 10 10 -7 -10 156.714 115.930 16 10 7 -10-260.131 131.269 14 10 -7 -9-261.251 146.108 16 10 7 -9-148.693 130.125 14 10 -7 -8 425.360 157.076 16 10 7 -8 202.113 136.729 14 10 -7 -7 265.350 164.775 16 -10 -7 7 234.255 110.670 15 10 7 -7 275.543 159.702 14 10 -7 -6 543.781 181.577 16 -10 -7 6 395.336 134.072 15 10 7 -6 619.938 177.811 14 10 -7 -5 480.310 185.228 16 -10 -7 5 84.8667 119.969 15 10 -7 -4 595.517 182.693 16 -10 -7 4 469.014 144.465 15 -10 -7 3-17.7404 125.709 15 -10 -7 2 48.5149 128.724 15 -10 -7 1 37.9944 119.923 15 -10 -7 0-109.479 112.234 15 -10 -7 0-112.805 93.4127 10 -10 -7 -1 706.830 116.238 15 -10 -7 -1 609.604 109.385 10 10 -8 -10 501.518 120.318 16 10 8 -10-103.494 91.6454 14 10 -8 -9 196.582 133.841 16 10 8 -9-59.2647 117.287 14 10 -8 -8-68.9471 135.652 16 10 8 -8-226.138 128.814 14 10 -8 -7 655.496 176.543 16 10 8 -7 844.948 162.916 14 10 -8 -6 133.720 150.282 16 -10 -8 6 85.2751 103.639 15 10 8 -6 353.291 146.925 14 10 -8 -5 233.163 158.808 16 -10 -8 5 54.3196 111.016 15 10 -8 -4 214.750 155.271 16 -10 -8 4 207.026 124.941 15 10 -8 -3 1158.64 184.452 16 -10 -8 3 1396.95 179.329 15 10 -8 -2-38.3451 125.547 16 -10 -8 2 103.710 118.368 15 10 -8 -1 307.626 129.711 16 -10 -8 1 291.562 122.330 15 -10 -8 1 178.885 97.0151 10 10 -8 0 383.531 110.806 16 -10 -8 0 457.815 118.020 15 -10 -8 0 344.297 106.410 10 10 -9 -9 103.825 111.227 16 10 9 -9-185.386 98.8138 14 10 -9 -8 381.418 137.770 16 10 9 -8 240.663 99.5356 14 10 -9 -7 53.1746 131.671 16 10 9 -7 325.821 124.828 14 10 -9 -6 196.605 146.117 16 -10 -9 6 1.49140 94.3069 15 10 9 -6 251.313 129.417 14 10 -9 -5 26.4281 134.116 16 -10 -9 5 196.866 110.367 15 10 9 -5 383.328 142.164 14 10 -9 -4-7.98509 134.054 16 -10 -9 4 524.505 132.730 15 10 -9 -3 1158.68 176.598 16 -10 -9 3 1041.26 153.540 15 10 -9 -2 256.315 125.679 16 -10 -9 2 252.613 116.213 15 10 -9 -1 43.7705 101.594 16 -10 -9 1-1.19130 105.542 15 -10 -9 1-103.100 98.6148 10 10 -10 -8 279.491 124.210 16 10 -10 -7-200.496 133.954 16 10 -10 -6-103.152 127.883 16 10 -10 -5 405.355 138.141 16 -10 -10 5 241.133 99.2995 15 10 -10 -4-17.3885 117.015 16 -10 -10 4 246.013 105.277 15 -10 -10 3 2497.57 185.814 15 10 -10 -3 2490.98 199.571 16 10 -10 -2 17.9133 95.9823 16 -10 -10 2 195.024 109.624 15 10 -11 -5-34.8326 109.621 16 10 -11 -4-84.0796 106.560 16 -10 -11 4 277.290 91.6683 15 11 0 -9 10.5424 104.771 14 11 0 -8 104.903 114.537 14 11 0 -7 416.410 119.827 16 11 0 -7 868.426 160.241 14 11 0 -6 374.399 141.462 16 11 0 -6 194.688 137.375 14 -11 0 5 72.7109 125.897 15 -11 0 4 61.4961 118.616 15 -11 0 3 41.8685 111.623 15 -11 0 2 20.6657 101.729 15 -11 0 1 39.3636 82.2507 13 11 -1 -9 1481.52 159.594 14 11 1 -9 1629.80 175.637 14 11 -1 -8 27.4145 111.283 14 11 1 -8 173.768 125.050 14 11 -1 -7 205.032 128.153 16 11 -1 -7 268.715 134.491 14 11 1 -7 315.343 142.262 14 11 -1 -6 215.585 141.601 16 11 1 -6 349.977 139.147 16 -11 -1 6 40.8296 123.595 15 11 -1 -6 355.884 135.603 14 11 1 -6 308.485 150.673 14 -11 -1 5 423.809 143.152 15 -11 1 4-136.528 124.185 15 -11 -1 4 46.8261 122.115 15 -11 1 3 121.682 118.732 15 -11 -1 3 223.751 122.000 15 -11 -1 2 27.3870 98.9514 15 -11 -1 1 252.227 82.7165 15 -11 -1 1 321.862 98.1815 13 11 -2 -9-61.9464 96.7618 14 11 2 -9 112.309 113.095 14 11 -2 -8-60.6627 89.7931 16 11 -2 -8-63.9371 105.169 14 11 2 -8 76.9857 124.188 14 11 -2 -7 340.612 135.476 16 11 -2 -7 311.950 120.885 14 11 2 -7 496.118 151.847 14 11 -2 -6 407.016 148.477 16 -11 -2 6 174.524 118.493 15 11 -2 -6 454.239 131.891 14 -11 -2 5 65.7357 126.059 15 11 -2 -5 178.288 123.140 14 -11 -2 4-72.2127 120.968 15 -11 -2 3 644.681 148.138 15 -11 -2 2-31.0490 105.073 15 -11 -2 2-12.0375 87.0886 13 -11 -2 1 180.483 82.0844 15 -11 -2 1-45.2494 83.5333 13 11 -3 -9 124.429 93.0916 16 11 3 -9 181.385 116.036 14 11 -3 -8 800.672 138.084 16 11 3 -8 1138.06 167.279 14 11 -3 -7-36.2571 118.979 16 -11 -3 7 37.2782 105.008 15 11 -3 -7-2.39930 99.1642 14 11 3 -7 120.505 134.502 14 11 -3 -6 291.499 145.703 16 -11 -3 6 179.576 119.253 15 11 -3 -6-154.267 96.7864 14 11 3 -6 352.115 148.708 14 11 -3 -5 397.508 153.468 16 -11 -3 5 26.0530 113.958 15 11 -3 -5 175.851 111.178 14 -11 -3 4 7.78258 113.256 15 -11 -3 3 309.055 117.247 15 -11 -3 2 165.426 114.002 15 11 -4 -9-94.7970 99.2134 16 11 4 -9 120.755 111.067 14 11 -4 -8 445.952 129.826 16 11 4 -8 203.860 120.170 14 11 -4 -7 526.006 146.220 16 -11 -4 7 245.245 108.694 15 11 4 -7 358.071 146.145 14 11 -4 -6 16.0138 133.033 16 -11 -4 6-32.6534 105.552 15 11 4 -6 162.524 137.599 14 11 -4 -5 98.6902 139.804 16 -11 -4 5-4.99763 107.947 15 -11 -4 4 119.872 110.524 15 -11 -4 3 100.528 110.137 15 -11 -4 2 241.587 110.916 15 11 -5 -8 58.0243 107.791 16 11 5 -8 90.8169 112.272 14 11 -5 -7-5.57344 117.204 16 -11 -5 7 131.402 92.4286 15 11 -5 -6 284.407 137.764 16 -11 -5 6 83.6048 100.070 15 11 5 -6 343.235 137.049 14 11 -5 -5 97.5253 137.767 16 -11 -5 5-19.7835 104.797 15 11 -5 -4-5.41773 123.362 16 -11 -5 4 93.3165 111.198 15 11 -5 -3 551.283 143.558 16 -11 -5 3 583.874 129.817 15 11 -6 -7 46.8575 112.381 16 -11 -6 7-1.93064 82.2284 15 11 6 -7 183.561 123.480 14 11 -6 -6 422.753 134.304 16 -11 -6 6 249.056 101.403 15 11 6 -6 583.658 144.042 14 11 -6 -5 144.812 125.591 16 -11 -6 5 16.3284 101.344 15 11 6 -5 334.715 131.898 14 11 -6 -4 108.525 119.892 16 -11 -6 4 140.332 107.705 15 0 0 0 0.00 0.00 0 TITL zzy1062 in P2(1)/n REM P2(1)/n (#14 in standard setting) CELL 1.54184 9.664174 18.573294 13.447942 90.0000 110.3240 90.0000 ZERR 3.00 0.000400 0.000701 0.000556 0.0000 0.0044 0.0000 LATT 1 SYMM -x+1/2, y+1/2,-z+1/2 SFAC C H N O UNIT 120.00 120.00 12.00 6.00 TREF HKLF 4 END ; _shelx_hkl_checksum 52170 _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; _oxdiff_exptl_absorpt_empirical_full_max 1.360 _oxdiff_exptl_absorpt_empirical_full_min 0.840 ####################################################################### # # This file contains crystal structure data downloaded from the # Cambridge Structural Database (CSD) hosted by the Cambridge # Crystallographic Data Centre (CCDC). # # Full information about CCDC data access policies and citation # guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 # # Audit and citation data items may have been added by the CCDC. # Please retain this information to preserve the provenance of # this file and to allow appropriate attribution of the data. # ####################################################################### data_a_CCDC1 _database_code_depnum_ccdc_archive 'CCDC 2086417' loop_ _audit_author_name _audit_author_address 'Qilin Wang' ;Henan University China ; _audit_update_record ; 2021-05-28 deposited with the CCDC. 2021-11-08 downloaded from the CCDC. ; _audit_creation_date 2021-01-26 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _shelx_SHELXL_version_number 2014/7 _chemical_name_common ? _chemical_name_systematic ? _chemical_formula_moiety 'C21 H18 N2 O4, C H4 O' _chemical_formula_sum 'C22 H22 N2 O5' _chemical_formula_weight 394.41 _chemical_melting_point ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.5481(2) _cell_length_b 11.4787(3) _cell_length_c 12.3488(4) _cell_angle_alpha 64.2362(13) _cell_angle_beta 78.0893(13) _cell_angle_gamma 87.4663(15) _cell_volume 941.57(5) _cell_formula_units_Z 2 _cell_measurement_reflns_used 7405 _cell_measurement_temperature 150(2) _cell_measurement_theta_max 68.25 _cell_measurement_theta_min 4.06 _shelx_estimated_absorpt_T_max 0.923 _shelx_estimated_absorpt_T_min 0.779 _exptl_absorpt_coefficient_mu 0.820 _exptl_absorpt_correction_T_max 0.7531 _exptl_absorpt_correction_T_min 0.5493 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1259 before and 0.0793 after correction. The Ratio of minimum to maximum transmission is 0.7294. The \l/2 correction factor is Not present.' _exptl_absorpt_special_details ? _exptl_crystal_colour yellow _exptl_crystal_colour_primary yellow _exptl_crystal_density_diffrn 1.391 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description block _exptl_crystal_F_000 416 _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.1 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0632 _diffrn_reflns_av_unetI/netI 0.0561 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.995 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_number 11740 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.995 _diffrn_reflns_theta_full 67.679 _diffrn_reflns_theta_max 68.437 _diffrn_reflns_theta_min 4.064 _diffrn_ambient_temperature 150.0 _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.995 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _diffrn_source ? _diffrn_standards_number 0 _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 3000 _reflns_number_total 3432 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement 'SAINT V8.38A (?, 2016)' _computing_data_collection ? _computing_data_reduction 'SAINT V8.38A (?, 2016)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'ShelXS (Sheldrick, 2008)' _refine_diff_density_max 0.397 _refine_diff_density_min -0.326 _refine_diff_density_rms 0.065 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 278 _refine_ls_number_reflns 3432 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0606 _refine_ls_R_factor_gt 0.0543 _refine_ls_restrained_S_all 1.053 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0955P)^2^+0.2495P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1490 _refine_ls_wR_factor_ref 0.1564 _refine_special_details ? _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H,H) groups, H2 of C2, H3 of C3, H1A of C1, H9 of C9, H4 of C4, H12 of C12, H13 of C13, H10 of C10, H18 of C18, H17 of C17, H21 of C21, H19 of C19, H20 of C20 At 1.5 times of: All C(H,H,H) groups, H5 of C21, All C(H,H,H,H) groups, All O(H) groups 2. Restrained distances O5A-C22A 1.43 with sigma of 0.02 H1-O1 0.9 with sigma of 0.02 O5-C22 1.4 with sigma of 0.02 3. Uiso/Uaniso restraints and constraints Uanis(O5) = Uanis(O5A) Uanis(C22) = Uanis(C22A) 4. Others Sof(O5A)=Sof(H5A)=Sof(C22A)=Sof(H22D)=Sof(H22E)=Sof(H22F)=1-FVAR(1) Sof(H5)=Sof(O5)=Sof(C22)=Sof(H22A)=Sof(H22B)=Sof(H22C)=FVAR(1) 5.a Ternary CH refined with riding coordinates: C9(H9), C10(H10), C13(H13) 5.b Secondary CH2 refined with riding coordinates: C7(H7A,H7B), C14(H14A,H14B) 5.c Aromatic/amide H refined with riding coordinates: C1(H1A), C2(H2), C3(H3), C4(H4), C12(H12), C17(H17), C18(H18), C19(H19), C20(H20), C21(H21) 5.d Idealised Me refined as rotating group: C22(H22A,H22B,H22C), C22A(H22D,H22E,H22F) 5.e Idealised tetrahedral OH refined as rotating group: O5A(H5A) ; _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary direct _atom_sites_solution_secondary ? loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group O1 O 1.04314(16) 0.59253(13) 0.53904(11) 0.0322(3) Uani 1 1 d D . . . . O2 O 0.47969(17) 0.37830(14) 0.89071(13) 0.0383(3) Uani 1 1 d . . . . . O3 O 0.99676(18) 0.18728(13) 1.07214(12) 0.0375(3) Uani 1 1 d . . . . . O4 O 0.87299(19) 0.31378(14) 1.15358(11) 0.0382(3) Uani 1 1 d . . . . . N1 N 0.76008(19) 0.56708(14) 0.83166(12) 0.0269(3) Uani 1 1 d . . . . . N2 N 0.91801(18) 0.28892(14) 1.06262(13) 0.0285(3) Uani 1 1 d . . . . . C1 C 0.4769(3) 0.7976(2) 0.63468(18) 0.0426(5) Uani 1 1 d . . . . . H1A H 0.4273 0.8581 0.6647 0.051 Uiso 1 1 calc R . . . . C2 C 0.4321(3) 0.7973(2) 0.53196(19) 0.0488(5) Uani 1 1 d . . . . . H2 H 0.3516 0.8586 0.4906 0.059 Uiso 1 1 calc R . . . . C3 C 0.5038(3) 0.7080(2) 0.48820(19) 0.0465(5) Uani 1 1 d . . . . . H3 H 0.4696 0.7077 0.4185 0.056 Uiso 1 1 calc R . . . . C4 C 0.6246(3) 0.6198(2) 0.54555(17) 0.0377(4) Uani 1 1 d . . . . . H4 H 0.6743 0.5593 0.5156 0.045 Uiso 1 1 calc R . . . . C5 C 0.6714(2) 0.62178(18) 0.64747(15) 0.0305(4) Uani 1 1 d . . . . . C6 C 0.5956(2) 0.70806(18) 0.69345(16) 0.0335(4) Uani 1 1 d . . . . . C7 C 0.6558(3) 0.68371(18) 0.80958(17) 0.0361(4) Uani 1 1 d . . . . . H7A H 0.7327 0.7575 0.7982 0.043 Uiso 1 1 calc R . . . . H7B H 0.5508 0.6677 0.8782 0.043 Uiso 1 1 calc R . . . . C8 C 0.7964(2) 0.53601(16) 0.72419(14) 0.0260(4) Uani 1 1 d . . . . . C9 C 0.7737(2) 0.38961(16) 0.76805(14) 0.0256(4) Uani 1 1 d . . . . . H9 H 0.8062 0.3717 0.6942 0.031 Uiso 1 1 calc R . . . . C10 C 0.9299(2) 0.34408(17) 0.84002(15) 0.0271(4) Uani 1 1 d . . . . . H10 H 0.9525 0.2504 0.8642 0.033 Uiso 1 1 calc R . . . . C11 C 0.8809(2) 0.37376(16) 0.94941(15) 0.0260(4) Uani 1 1 d . . . . . C12 C 0.7976(2) 0.48681(17) 0.93787(14) 0.0266(4) Uani 1 1 d . . . . . H12 H 0.7676 0.5066 1.0064 0.032 Uiso 1 1 calc R . . . . C13 C 1.0047(2) 0.56202(17) 0.66622(15) 0.0282(4) Uani 1 1 d . . . . . H13 H 1.0522 0.6346 0.6782 0.034 Uiso 1 1 calc R . . . . C14 C 1.0896(2) 0.43431(18) 0.74213(15) 0.0307(4) Uani 1 1 d . . . . . H14A H 1.1504 0.3944 0.6885 0.037 Uiso 1 1 calc R . . . . H14B H 1.1798 0.4511 0.7822 0.037 Uiso 1 1 calc R . . . . C15 C 0.5862(2) 0.32742(17) 0.83791(15) 0.0277(4) Uani 1 1 d . . . . . C16 C 0.5360(2) 0.20245(17) 0.83975(14) 0.0276(4) Uani 1 1 d . . . . . C17 C 0.3589(2) 0.15093(18) 0.89476(16) 0.0336(4) Uani 1 1 d . . . . . H17 H 0.2753 0.1948 0.9309 0.040 Uiso 1 1 calc R . . . . C18 C 0.3041(3) 0.0362(2) 0.89704(19) 0.0410(5) Uani 1 1 d . . . . . H18 H 0.1828 0.0023 0.9337 0.049 Uiso 1 1 calc R . . . . C19 C 0.4260(3) -0.02908(19) 0.84584(18) 0.0410(5) Uani 1 1 d . . . . . H19 H 0.3882 -0.1080 0.8479 0.049 Uiso 1 1 calc R . . . . C20 C 0.6021(3) 0.02017(19) 0.79194(18) 0.0386(4) Uani 1 1 d . . . . . H20 H 0.6856 -0.0250 0.7573 0.046 Uiso 1 1 calc R . . . . C21 C 0.6573(2) 0.13565(18) 0.78840(16) 0.0326(4) Uani 1 1 d . . . . . H21 H 0.7785 0.1695 0.7508 0.039 Uiso 1 1 calc R . . . . H5 H 0.053(7) 0.849(5) 0.712(5) 0.049 Uiso 0.486(3) 1 d R . P . . O5 O 0.0111(4) 0.9115(3) 0.6424(3) 0.0454(5) Uani 0.486(3) 1 d D . P A 1 O5A O -0.0219(4) 0.1428(3) 0.5539(3) 0.0454(5) Uani 0.514(3) 1 d D . P A 2 H5A H -0.0286 0.1260 0.4951 0.068 Uiso 0.514(3) 1 calc GR . P A 2 C22 C 0.079(4) 1.0370(17) 0.623(4) 0.066(2) Uani 0.486(3) 1 d D . P A 1 H22A H 0.0127 1.1052 0.5680 0.098 Uiso 0.486(3) 1 calc GR . P A 1 H22B H 0.2082 1.0491 0.5848 0.098 Uiso 0.486(3) 1 calc GR . P A 1 H22C H 0.0607 1.0415 0.7015 0.098 Uiso 0.486(3) 1 calc GR . P A 1 C22A C 0.100(4) 0.0602(17) 0.622(3) 0.066(2) Uani 0.514(3) 1 d D . P A 2 H22D H 0.2014 0.0467 0.5654 0.098 Uiso 0.514(3) 1 calc GR . P A 2 H22E H 0.0367 -0.0233 0.6796 0.098 Uiso 0.514(3) 1 calc GR . P A 2 H22F H 0.1455 0.0999 0.6673 0.098 Uiso 0.514(3) 1 calc GR . P A 2 H1 H 1.022(5) 0.678(2) 0.503(3) 0.098 Uiso 1 1 d DR . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.0298(6) 0.0433(7) 0.0227(6) -0.0154(5) -0.0015(5) 0.0024(5) O2 0.0257(6) 0.0567(8) 0.0435(8) -0.0357(7) 0.0021(5) 0.0011(6) O3 0.0353(7) 0.0393(7) 0.0313(7) -0.0106(5) -0.0057(5) 0.0083(5) O4 0.0442(8) 0.0500(8) 0.0223(6) -0.0171(6) -0.0077(5) 0.0011(6) N1 0.0289(7) 0.0346(7) 0.0229(7) -0.0181(6) -0.0053(5) 0.0045(6) N2 0.0217(7) 0.0378(8) 0.0246(7) -0.0128(6) -0.0026(5) -0.0032(6) C1 0.0397(11) 0.0503(11) 0.0351(10) -0.0182(8) -0.0059(8) 0.0168(9) C2 0.0382(11) 0.0649(14) 0.0360(10) -0.0153(10) -0.0112(8) 0.0185(10) C3 0.0385(11) 0.0722(14) 0.0319(10) -0.0229(10) -0.0149(8) 0.0128(10) C4 0.0311(9) 0.0580(12) 0.0277(9) -0.0217(8) -0.0077(7) 0.0078(8) C5 0.0256(8) 0.0416(9) 0.0243(8) -0.0158(7) -0.0019(6) 0.0030(7) C6 0.0315(9) 0.0408(9) 0.0264(9) -0.0145(7) -0.0041(7) 0.0077(7) C7 0.0464(11) 0.0372(9) 0.0297(9) -0.0195(8) -0.0097(8) 0.0142(8) C8 0.0250(8) 0.0376(9) 0.0202(7) -0.0172(7) -0.0047(6) 0.0035(6) C9 0.0235(8) 0.0364(9) 0.0228(8) -0.0188(7) -0.0037(6) 0.0029(6) C10 0.0233(8) 0.0359(9) 0.0253(8) -0.0169(7) -0.0040(6) 0.0043(6) C11 0.0230(8) 0.0350(9) 0.0221(8) -0.0142(7) -0.0047(6) -0.0006(6) C12 0.0244(8) 0.0376(9) 0.0219(8) -0.0173(7) -0.0029(6) -0.0015(6) C13 0.0245(8) 0.0397(9) 0.0232(8) -0.0167(7) -0.0041(6) 0.0018(6) C14 0.0217(8) 0.0454(10) 0.0268(8) -0.0181(7) -0.0041(6) 0.0052(7) C15 0.0234(8) 0.0420(9) 0.0237(8) -0.0196(7) -0.0060(6) 0.0046(7) C16 0.0274(8) 0.0373(9) 0.0198(7) -0.0133(6) -0.0063(6) 0.0020(7) C17 0.0281(9) 0.0427(10) 0.0292(9) -0.0157(7) -0.0045(7) 0.0030(7) C18 0.0348(10) 0.0444(11) 0.0383(10) -0.0141(8) -0.0026(8) -0.0085(8) C19 0.0505(12) 0.0360(10) 0.0355(10) -0.0145(8) -0.0079(8) -0.0041(8) C20 0.0443(11) 0.0378(10) 0.0354(10) -0.0191(8) -0.0051(8) 0.0035(8) C21 0.0305(9) 0.0395(9) 0.0292(9) -0.0172(7) -0.0041(7) 0.0022(7) O5 0.0461(12) 0.0483(12) 0.0336(10) -0.0105(9) -0.0095(9) 0.0093(9) O5A 0.0461(12) 0.0483(12) 0.0336(10) -0.0105(9) -0.0095(9) 0.0093(9) C22 0.042(6) 0.077(5) 0.0537(15) -0.009(5) -0.007(3) 0.014(5) C22A 0.042(6) 0.077(5) 0.0537(15) -0.009(5) -0.007(3) 0.014(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1 C13 1.420(2) . ? O1 H1 0.906(19) . ? O2 C15 1.219(2) . ? O3 N2 1.256(2) . ? O4 N2 1.253(2) . ? N1 C7 1.471(2) . ? N1 C8 1.4888(19) . ? N1 C12 1.315(2) . ? N2 C11 1.391(2) . ? C1 H1A 0.9500 . ? C1 C2 1.380(3) . ? C1 C6 1.387(3) . ? C2 H2 0.9500 . ? C2 C3 1.396(3) . ? C3 H3 0.9500 . ? C3 C4 1.386(3) . ? C4 H4 0.9500 . ? C4 C5 1.385(3) . ? C5 C6 1.391(3) . ? C5 C8 1.494(2) . ? C6 C7 1.500(3) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.531(2) . ? C8 C13 1.570(2) . ? C9 H9 1.0000 . ? C9 C10 1.558(2) . ? C9 C15 1.519(2) . ? C10 H10 1.0000 . ? C10 C11 1.503(2) . ? C10 C14 1.552(2) . ? C11 C12 1.380(2) . ? C12 H12 0.9500 . ? C13 H13 1.0000 . ? C13 C14 1.552(2) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.489(2) . ? C16 C17 1.394(3) . ? C16 C21 1.396(2) . ? C17 H17 0.9500 . ? C17 C18 1.384(3) . ? C18 H18 0.9500 . ? C18 C19 1.386(3) . ? C19 H19 0.9500 . ? C19 C20 1.380(3) . ? C20 H20 0.9500 . ? C20 C21 1.387(3) . ? C21 H21 0.9500 . ? O5 H5 0.96(6) . ? O5 C22 1.449(18) . ? O5A H5A 0.8400 . ? O5A C22A 1.412(19) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C22A H22D 0.9800 . ? C22A H22E 0.9800 . ? C22A H22F 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C13 O1 H1 103(2) . . ? C7 N1 C8 112.34(13) . . ? C12 N1 C7 125.45(14) . . ? C12 N1 C8 121.58(14) . . ? O3 N2 C11 118.99(14) . . ? O4 N2 O3 120.69(15) . . ? O4 N2 C11 120.32(15) . . ? C2 C1 H1A 120.6 . . ? C2 C1 C6 118.90(19) . . ? C6 C1 H1A 120.6 . . ? C1 C2 H2 119.7 . . ? C1 C2 C3 120.68(19) . . ? C3 C2 H2 119.7 . . ? C2 C3 H3 119.7 . . ? C4 C3 C2 120.55(19) . . ? C4 C3 H3 119.7 . . ? C3 C4 H4 120.7 . . ? C5 C4 C3 118.55(19) . . ? C5 C4 H4 120.7 . . ? C4 C5 C6 120.93(17) . . ? C4 C5 C8 127.98(17) . . ? C6 C5 C8 111.06(15) . . ? C1 C6 C5 120.34(18) . . ? C1 C6 C7 128.94(17) . . ? C5 C6 C7 110.68(16) . . ? N1 C7 C6 102.49(14) . . ? N1 C7 H7A 111.3 . . ? N1 C7 H7B 111.3 . . ? C6 C7 H7A 111.3 . . ? C6 C7 H7B 111.3 . . ? H7A C7 H7B 109.2 . . ? N1 C8 C5 101.89(13) . . ? N1 C8 C9 109.99(13) . . ? N1 C8 C13 107.96(13) . . ? C5 C8 C9 118.51(14) . . ? C5 C8 C13 116.66(14) . . ? C9 C8 C13 101.61(13) . . ? C8 C9 H9 107.9 . . ? C8 C9 C10 99.71(13) . . ? C10 C9 H9 107.9 . . ? C15 C9 C8 116.38(14) . . ? C15 C9 H9 107.9 . . ? C15 C9 C10 116.46(13) . . ? C9 C10 H10 112.2 . . ? C11 C10 C9 107.36(13) . . ? C11 C10 H10 112.2 . . ? C11 C10 C14 111.81(14) . . ? C14 C10 C9 100.33(13) . . ? C14 C10 H10 112.2 . . ? N2 C11 C10 121.09(15) . . ? C12 C11 N2 119.21(15) . . ? C12 C11 C10 119.70(15) . . ? N1 C12 C11 119.76(15) . . ? N1 C12 H12 120.1 . . ? C11 C12 H12 120.1 . . ? O1 C13 C8 112.35(13) . . ? O1 C13 H13 109.5 . . ? O1 C13 C14 111.75(13) . . ? C8 C13 H13 109.5 . . ? C14 C13 C8 104.08(13) . . ? C14 C13 H13 109.5 . . ? C10 C14 C13 105.96(13) . . ? C10 C14 H14A 110.5 . . ? C10 C14 H14B 110.5 . . ? C13 C14 H14A 110.5 . . ? C13 C14 H14B 110.5 . . ? H14A C14 H14B 108.7 . . ? O2 C15 C9 121.07(15) . . ? O2 C15 C16 120.90(15) . . ? C16 C15 C9 118.03(14) . . ? C17 C16 C15 118.05(15) . . ? C17 C16 C21 118.89(17) . . ? C21 C16 C15 123.06(15) . . ? C16 C17 H17 119.8 . . ? C18 C17 C16 120.43(17) . . ? C18 C17 H17 119.8 . . ? C17 C18 H18 120.0 . . ? C17 C18 C19 120.06(18) . . ? C19 C18 H18 120.0 . . ? C18 C19 H19 119.9 . . ? C20 C19 C18 120.18(18) . . ? C20 C19 H19 119.9 . . ? C19 C20 H20 120.0 . . ? C19 C20 C21 120.01(18) . . ? C21 C20 H20 120.0 . . ? C16 C21 H21 119.8 . . ? C20 C21 C16 120.44(17) . . ? C20 C21 H21 119.8 . . ? C22 O5 H5 106(3) . . ? C22A O5A H5A 109.5 . . ? O5 C22 H22A 109.5 . . ? O5 C22 H22B 109.5 . . ? O5 C22 H22C 109.5 . . ? H22A C22 H22B 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? O5A C22A H22D 109.5 . . ? O5A C22A H22E 109.5 . . ? O5A C22A H22F 109.5 . . ? H22D C22A H22E 109.5 . . ? H22D C22A H22F 109.5 . . ? H22E C22A H22F 109.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O5 H5 O3 0.96(6) 2.46(6) 3.187(3) 133(4) 2_667 O5 H5 O4 0.96(6) 2.04(6) 2.974(3) 167(5) 2_667 O5 H5 N2 0.96(6) 2.59(6) 3.501(3) 160(4) 2_667 O1 H1 O5A 0.906(19) 1.86(2) 2.752(3) 167(4) 2_666 loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 C13 C14 C10 -122.74(14) . . . . ? O2 C15 C16 C17 5.2(2) . . . . ? O2 C15 C16 C21 -175.22(16) . . . . ? O3 N2 C11 C10 1.3(2) . . . . ? O3 N2 C11 C12 -178.72(14) . . . . ? O4 N2 C11 C10 -178.53(14) . . . . ? O4 N2 C11 C12 1.4(2) . . . . ? N1 C8 C9 C10 -64.12(15) . . . . ? N1 C8 C9 C15 62.00(17) . . . . ? N1 C8 C13 O1 -153.46(14) . . . . ? N1 C8 C13 C14 85.45(15) . . . . ? N2 C11 C12 N1 -179.25(14) . . . . ? C1 C2 C3 C4 -1.5(3) . . . . ? C1 C6 C7 N1 172.7(2) . . . . ? C2 C1 C6 C5 1.6(3) . . . . ? C2 C1 C6 C7 -175.9(2) . . . . ? C2 C3 C4 C5 0.4(3) . . . . ? C3 C4 C5 C6 1.6(3) . . . . ? C3 C4 C5 C8 179.37(18) . . . . ? C4 C5 C6 C1 -2.6(3) . . . . ? C4 C5 C6 C7 175.29(17) . . . . ? C4 C5 C8 N1 -168.67(18) . . . . ? C4 C5 C8 C9 -47.9(2) . . . . ? C4 C5 C8 C13 74.1(2) . . . . ? C5 C6 C7 N1 -5.0(2) . . . . ? C5 C8 C9 C10 179.33(13) . . . . ? C5 C8 C9 C15 -54.55(19) . . . . ? C5 C8 C13 O1 -39.6(2) . . . . ? C5 C8 C13 C14 -160.65(14) . . . . ? C6 C1 C2 C3 0.4(3) . . . . ? C6 C5 C8 N1 9.29(18) . . . . ? C6 C5 C8 C9 130.08(16) . . . . ? C6 C5 C8 C13 -107.98(17) . . . . ? C7 N1 C8 C5 -12.83(18) . . . . ? C7 N1 C8 C9 -139.39(15) . . . . ? C7 N1 C8 C13 110.55(16) . . . . ? C7 N1 C12 C11 173.46(16) . . . . ? C8 N1 C7 C6 11.33(19) . . . . ? C8 N1 C12 C11 3.3(2) . . . . ? C8 C5 C6 C1 179.24(17) . . . . ? C8 C5 C6 C7 -2.8(2) . . . . ? C8 C9 C10 C11 66.47(15) . . . . ? C8 C9 C10 C14 -50.44(14) . . . . ? C8 C9 C15 O2 -23.3(2) . . . . ? C8 C9 C15 C16 156.52(14) . . . . ? C8 C13 C14 C10 -1.26(16) . . . . ? C9 C8 C13 O1 90.85(15) . . . . ? C9 C8 C13 C14 -30.23(15) . . . . ? C9 C10 C11 N2 141.60(15) . . . . ? C9 C10 C11 C12 -38.3(2) . . . . ? C9 C10 C14 C13 31.54(16) . . . . ? C9 C15 C16 C17 -174.59(15) . . . . ? C9 C15 C16 C21 5.0(2) . . . . ? C10 C9 C15 O2 93.9(2) . . . . ? C10 C9 C15 C16 -86.27(18) . . . . ? C10 C11 C12 N1 0.7(2) . . . . ? C11 C10 C14 C13 -82.01(16) . . . . ? C12 N1 C7 C6 -159.64(16) . . . . ? C12 N1 C8 C5 158.54(15) . . . . ? C12 N1 C8 C9 32.0(2) . . . . ? C12 N1 C8 C13 -78.08(18) . . . . ? C13 C8 C9 C10 50.07(14) . . . . ? C13 C8 C9 C15 176.19(13) . . . . ? C14 C10 C11 N2 -109.28(17) . . . . ? C14 C10 C11 C12 70.77(19) . . . . ? C15 C9 C10 C11 -59.60(18) . . . . ? C15 C9 C10 C14 -176.51(14) . . . . ? C15 C16 C17 C18 178.83(16) . . . . ? C15 C16 C21 C20 -179.40(16) . . . . ? C16 C17 C18 C19 0.8(3) . . . . ? C17 C16 C21 C20 0.1(3) . . . . ? C17 C18 C19 C20 -0.3(3) . . . . ? C18 C19 C20 C21 -0.3(3) . . . . ? C19 C20 C21 C16 0.4(3) . . . . ? C21 C16 C17 C18 -0.7(3) . . . . ? _shelx_res_file ; a.res created by SHELXL-2014/7 TITL A in P-1 #2 REM reset to P-1 #2 CELL 1.54178 7.5481 11.4787 12.3488 64.2362 78.0893 87.4663 ZERR 2 0.0002 0.0003 0.0004 0.0013 0.0013 0.0015 LATT 1 SFAC C H N O UNIT 44 44 4 10 EQIV $1 1-X,1-Y,1-Z EQIV $2 1-X,1-Y,2-Z DFIX 1.43 O5A C22A DFIX 0.9 H1 O1 DFIX 1.4 O5 C22 EADP O5 O5A EADP C22 C22A L.S. 4 0 0 PLAN 20 SIZE 0.32 0.17 0.1 TEMP -123.15 HTAB O1 O5A_$1 HTAB O5 O3_$2 HTAB O5 O4_$2 HTAB O5 N2_$2 MPLA C1 C2 C3 C4 C5 C6 MPLA C8 C9 C10 MPLA C8 C10 C11 C12 N1 MPLA C8 C10 C13 C14 MPLA C16 C17 C18 C19 C20 C21 BOND $h conf fmap 2 acta REM REM REM WGHT 0.095500 0.249500 FVAR 0.33548 0.48582 O1 4 1.043140 0.592530 0.539042 11.00000 0.02983 0.04330 = 0.02268 -0.01542 -0.00153 0.00243 O2 4 0.479689 0.378303 0.890706 11.00000 0.02571 0.05675 = 0.04345 -0.03573 0.00209 0.00112 O3 4 0.996763 0.187276 1.072138 11.00000 0.03529 0.03929 = 0.03131 -0.01057 -0.00574 0.00829 O4 4 0.872994 0.313776 1.153579 11.00000 0.04424 0.05001 = 0.02225 -0.01710 -0.00766 0.00108 N1 3 0.760077 0.567081 0.831663 11.00000 0.02886 0.03460 = 0.02294 -0.01814 -0.00527 0.00451 N2 3 0.918008 0.288921 1.062620 11.00000 0.02170 0.03777 = 0.02458 -0.01280 -0.00256 -0.00319 C1 1 0.476904 0.797580 0.634683 11.00000 0.03966 0.05026 = 0.03507 -0.01823 -0.00595 0.01684 AFIX 43 H1A 2 0.427273 0.858056 0.664665 11.00000 -1.20000 AFIX 0 C2 1 0.432105 0.797330 0.531955 11.00000 0.03824 0.06492 = 0.03600 -0.01532 -0.01123 0.01848 AFIX 43 H2 2 0.351607 0.858575 0.490591 11.00000 -1.20000 AFIX 0 C3 1 0.503844 0.708017 0.488195 11.00000 0.03851 0.07217 = 0.03186 -0.02292 -0.01493 0.01278 AFIX 43 H3 2 0.469561 0.707700 0.418497 11.00000 -1.20000 AFIX 0 C4 1 0.624643 0.619812 0.545553 11.00000 0.03108 0.05804 = 0.02771 -0.02175 -0.00774 0.00785 AFIX 43 H4 2 0.674310 0.559306 0.515621 11.00000 -1.20000 AFIX 0 C5 1 0.671395 0.621783 0.647467 11.00000 0.02557 0.04156 = 0.02426 -0.01578 -0.00194 0.00297 C6 1 0.595619 0.708057 0.693451 11.00000 0.03151 0.04085 = 0.02639 -0.01447 -0.00406 0.00774 C7 1 0.655831 0.683709 0.809579 11.00000 0.04637 0.03724 = 0.02971 -0.01952 -0.00969 0.01424 AFIX 23 H7A 2 0.732724 0.757491 0.798187 11.00000 -1.20000 H7B 2 0.550775 0.667712 0.878151 11.00000 -1.20000 AFIX 0 C8 1 0.796373 0.536007 0.724189 11.00000 0.02498 0.03756 = 0.02021 -0.01716 -0.00467 0.00354 C9 1 0.773684 0.389609 0.768048 11.00000 0.02348 0.03638 = 0.02279 -0.01882 -0.00371 0.00291 AFIX 13 H9 2 0.806238 0.371693 0.694216 11.00000 -1.20000 AFIX 0 C10 1 0.929857 0.344075 0.840019 11.00000 0.02331 0.03588 = 0.02525 -0.01692 -0.00397 0.00432 AFIX 13 H10 2 0.952486 0.250415 0.864170 11.00000 -1.20000 AFIX 0 C11 1 0.880899 0.373758 0.949413 11.00000 0.02296 0.03501 = 0.02212 -0.01424 -0.00472 -0.00058 C12 1 0.797645 0.486808 0.937870 11.00000 0.02441 0.03762 = 0.02192 -0.01734 -0.00291 -0.00153 AFIX 43 H12 2 0.767562 0.506595 1.006398 11.00000 -1.20000 AFIX 0 C13 1 1.004700 0.562019 0.666221 11.00000 0.02453 0.03969 = 0.02318 -0.01670 -0.00415 0.00179 AFIX 13 H13 2 1.052202 0.634588 0.678218 11.00000 -1.20000 AFIX 0 C14 1 1.089590 0.434314 0.742126 11.00000 0.02173 0.04542 = 0.02684 -0.01809 -0.00413 0.00516 AFIX 23 H14A 2 1.150398 0.394355 0.688471 11.00000 -1.20000 H14B 2 1.179836 0.451140 0.782201 11.00000 -1.20000 AFIX 0 C15 1 0.586230 0.327421 0.837909 11.00000 0.02344 0.04202 = 0.02371 -0.01962 -0.00604 0.00464 C16 1 0.535991 0.202445 0.839746 11.00000 0.02737 0.03728 = 0.01980 -0.01330 -0.00627 0.00197 C17 1 0.358868 0.150930 0.894761 11.00000 0.02806 0.04273 = 0.02916 -0.01568 -0.00454 0.00302 AFIX 43 H17 2 0.275266 0.194827 0.930907 11.00000 -1.20000 AFIX 0 C18 1 0.304070 0.036242 0.897044 11.00000 0.03482 0.04437 = 0.03826 -0.01407 -0.00265 -0.00854 AFIX 43 H18 2 0.182756 0.002287 0.933746 11.00000 -1.20000 AFIX 0 C19 1 0.426005 -0.029083 0.845845 11.00000 0.05053 0.03601 = 0.03549 -0.01451 -0.00788 -0.00413 AFIX 43 H19 2 0.388244 -0.107985 0.847854 11.00000 -1.20000 AFIX 0 C20 1 0.602148 0.020168 0.791943 11.00000 0.04431 0.03779 = 0.03543 -0.01911 -0.00511 0.00354 AFIX 43 H20 2 0.685615 -0.025034 0.757258 11.00000 -1.20000 AFIX 0 C21 1 0.657334 0.135654 0.788403 11.00000 0.03054 0.03949 = 0.02919 -0.01723 -0.00412 0.00224 AFIX 43 H21 2 0.778500 0.169536 0.750794 11.00000 -1.20000 AFIX 0 H5 2 0.053442 0.848740 0.711956 21.00000 -1.50000 PART 1 O5 4 0.011136 0.911533 0.642415 21.00000 0.04607 0.04834 = 0.03362 -0.01053 -0.00949 0.00932 PART 0 PART 2 O5A 4 -0.021871 0.142811 0.553898 -21.00000 0.04607 0.04834 = 0.03362 -0.01053 -0.00949 0.00932 AFIX 147 H5A 2 -0.028578 0.125998 0.495064 -21.00000 -1.50000 AFIX 0 PART 0 PART 1 C22 1 0.078640 1.036972 0.622559 21.00000 0.04191 0.07740 = 0.05366 -0.00907 -0.00683 0.01434 AFIX 137 H22A 2 0.012681 1.105151 0.567953 21.00000 -1.50000 H22B 2 0.208185 1.049113 0.584786 21.00000 -1.50000 H22C 2 0.060710 1.041496 0.701507 21.00000 -1.50000 AFIX 0 PART 0 PART 2 C22A 1 0.099741 0.060240 0.621742 -21.00000 0.04191 0.07740 = 0.05366 -0.00907 -0.00683 0.01434 AFIX 137 H22D 2 0.201443 0.046741 0.565381 -21.00000 -1.50000 H22E 2 0.036698 -0.023260 0.679628 -21.00000 -1.50000 H22F 2 0.145503 0.099922 0.667311 -21.00000 -1.50000 AFIX 0 PART 0 H1 2 1.022240 0.677998 0.502908 11.00000 -1.50000 HKLF 4 REM A in P-1 #2 REM R1 = 0.0543 for 3000 Fo > 4sig(Fo) and 0.0606 for all 3432 data REM 278 parameters refined using 3 restraints END WGHT 0.0955 0.2495 REM Highest difference peak 0.397, deepest hole -0.326, 1-sigma level 0.065 Q1 1 1.0019 0.5254 0.5265 11.00000 0.05 0.40 Q2 1 0.7048 0.7646 0.8230 11.00000 0.05 0.35 Q3 1 0.6028 0.7204 0.8804 11.00000 0.05 0.30 Q4 1 0.9115 0.5577 0.6842 11.00000 0.05 0.29 Q5 1 0.8581 0.8322 0.6982 11.00000 0.05 0.28 Q6 1 0.7274 0.3265 1.1811 11.00000 0.05 0.24 Q7 1 0.8500 0.3678 0.8077 11.00000 0.05 0.23 Q8 1 0.6853 0.3531 0.7943 11.00000 0.05 0.22 Q9 1 -0.0320 0.9440 0.6495 11.00000 0.05 0.22 Q10 1 1.1071 0.3994 0.6372 11.00000 0.05 0.21 Q11 1 0.1087 0.1157 0.6505 11.00000 0.05 0.20 Q12 1 -0.0518 0.9424 0.5642 11.00000 0.05 0.20 Q13 1 0.9839 0.2567 1.1998 11.00000 0.05 0.19 Q14 1 0.9196 0.5965 0.5215 11.00000 0.05 0.19 Q15 1 0.6262 0.8651 0.7449 11.00000 0.05 0.19 Q16 1 0.5863 0.3444 0.9254 11.00000 0.05 0.19 Q17 1 0.8878 0.3534 0.8918 11.00000 0.05 0.19 Q18 1 0.6378 0.5975 0.6032 11.00000 0.05 0.19 Q19 1 0.4230 -0.0069 0.8998 11.00000 0.05 0.18 Q20 1 0.5507 0.6436 0.5401 11.00000 0.05 0.18 ; _shelx_res_checksum 75834 _shelx_hkl_file ; -1 0 0 0.15 0.08 -1 0 0 0.12 0.06 -3 0 0 25.38 1.94 3 0 0 21.28 1.79 -4 0 0 3.59 0.61 -4 0 0 4.76 0.60 4 0 0 3.29 0.50 -5 0 0 4.06 0.78 -5 0 0 5.51 0.75 -5 0 0 4.32 0.40 -5 0 0 3.72 0.46 -5 0 0 3.52 0.38 5 0 0 4.21 0.67 5 0 0 4.71 0.69 -6 0 0 0.11 0.09 -6 0 0 -0.02 0.10 -6 0 0 0.00 0.09 -6 0 0 0.01 0.16 -7 0 0 10.66 0.97 -8 0 0 1.34 0.20 -8 0 0 0.99 0.19 -8 1 0 0.78 0.16 -8 1 0 0.94 0.14 -8 1 0 0.92 0.18 -8 1 0 1.11 0.21 -7 1 0 9.06 0.86 -6 1 0 6.61 0.58 -6 1 0 6.72 0.64 -6 1 0 6.85 0.68 -6 1 0 6.42 0.59 -6 1 0 4.74 1.63 5 -1 0 31.75 2.87 -5 1 0 35.55 2.44 -5 1 0 38.04 3.20 -5 1 0 34.56 2.45 -5 1 0 39.38 3.00 -5 1 0 35.64 2.54 -5 1 0 34.01 2.46 -4 1 0 6.89 0.79 -4 1 0 5.27 0.81 -3 1 0 7.60 0.75 -3 1 0 6.17 0.78 -2 1 0 72.95 4.96 -2 1 0 70.42 4.87 1 -1 0 177.07 12.94 -1 1 0 212.63 12.99 -1 -1 0 90.29 5.75 -1 -1 0 93.61 6.10 1 1 0 79.69 5.79 1 1 0 81.92 5.74 -2 -1 0 379.89 22.73 2 1 0 303.86 22.72 -3 -1 0 423.50 24.93 -3 -1 0 367.92 25.02 3 1 0 328.21 24.87 -4 -1 0 16.25 1.31 4 1 0 12.05 1.20 4 1 0 13.44 1.31 -5 -1 0 30.17 2.16 -5 -1 0 30.35 2.35 -5 -1 0 30.92 2.15 5 1 0 30.70 2.50 5 1 0 32.38 2.70 -6 -1 0 0.01 0.08 -6 -1 0 0.05 0.12 -6 -1 0 0.03 0.09 -6 -1 0 -0.01 0.10 6 1 0 -0.28 0.29 -7 -1 0 23.17 1.66 -7 -1 0 24.16 1.67 -8 -1 0 -0.01 0.09 -8 -1 0 -0.08 0.09 -8 2 0 0.88 0.15 -8 2 0 1.11 0.17 -7 2 0 15.12 1.05 -7 2 0 13.09 1.05 -7 2 0 10.66 1.05 -6 2 0 0.18 0.12 -6 2 0 0.74 0.55 -6 2 0 0.52 0.24 -5 2 0 18.43 1.41 -5 2 0 18.23 1.36 -5 2 0 20.21 1.34 -5 2 0 15.40 1.92 -5 2 0 19.81 1.85 -4 2 0 43.57 3.37 -4 2 0 43.18 3.57 -3 2 0 8.28 0.76 -3 2 0 7.20 0.93 -3 2 0 9.04 0.89 -3 2 0 8.94 0.76 -2 2 0 27.35 2.16 -2 2 0 28.05 2.26 -2 2 0 32.08 2.56 -2 2 0 29.12 2.44 1 -2 0 80.41 5.45 -1 2 0 77.54 5.34 -1 2 0 74.11 5.32 -1 2 0 80.75 5.43 0 -2 0 2.52 0.77 0 -2 0 3.22 0.38 0 2 0 3.34 0.36 0 2 0 3.63 0.38 -1 -2 0 184.11 12.09 -1 -2 0 175.26 11.32 -1 -2 0 162.16 11.49 1 2 0 188.12 11.46 1 2 0 145.53 11.46 -2 -2 0 881.37 58.48 3 2 0 0.13 0.10 3 2 0 0.17 0.15 -4 -2 0 5.14 0.59 4 2 0 5.21 0.63 4 2 0 4.40 0.68 -5 -2 0 11.81 0.85 -5 -2 0 9.92 0.86 -5 -2 0 11.94 0.88 -5 -2 0 11.00 0.93 -5 -2 0 11.49 1.02 -5 -2 0 10.86 0.92 5 2 0 13.10 1.23 5 2 0 12.31 1.34 -6 -2 0 1.78 0.32 -6 -2 0 1.21 0.31 -6 -2 0 2.34 0.26 -6 -2 0 1.76 0.23 6 2 0 3.01 0.77 -7 -2 0 2.09 0.36 -7 -2 0 2.45 0.26 -7 -2 0 2.86 0.28 -8 -2 0 5.29 0.58 -8 -2 0 7.76 0.52 -8 3 0 16.41 1.14 -8 3 0 15.53 1.13 -7 3 0 0.35 0.12 -7 3 0 0.28 0.11 -7 3 0 0.20 0.13 -7 3 0 0.33 0.13 -6 3 0 72.58 5.02 -6 3 0 67.45 4.99 -6 3 0 71.66 5.04 -6 3 0 83.26 4.99 -6 3 0 72.46 6.22 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4.68 0.49 -5 5 0 5.06 0.51 -5 5 0 3.34 1.18 -5 5 0 5.75 0.46 -4 5 0 60.90 4.42 -4 5 0 64.87 5.51 -4 5 0 64.92 5.47 -4 5 0 57.34 5.62 -4 5 0 73.21 4.39 -3 5 0 1.16 0.75 -3 5 0 0.12 0.21 -3 5 0 0.12 0.30 -2 5 0 201.51 13.42 -2 5 0 172.30 13.11 -2 5 0 200.76 14.53 -1 5 0 17.57 1.65 -1 5 0 18.67 1.73 -1 5 0 19.04 2.71 0 5 0 92.80 6.45 0 5 0 102.05 6.48 0 5 0 75.53 6.33 1 5 0 122.36 8.00 1 5 0 106.93 9.67 1 5 0 107.88 7.89 2 5 0 10.64 1.16 2 5 0 10.37 1.08 -3 -5 0 5.80 0.60 -3 -5 0 7.35 0.56 -3 -5 0 6.24 0.61 3 5 0 6.93 0.85 3 5 0 7.55 0.97 -4 -5 0 9.23 0.72 -4 -5 0 8.80 0.80 -4 -5 0 8.60 0.80 -4 -5 0 9.22 0.69 -4 -5 0 9.02 0.90 4 5 0 8.96 1.10 4 5 0 10.78 1.33 -5 -5 0 1.55 0.37 -5 -5 0 1.90 0.32 -5 -5 0 2.04 0.25 -5 -5 0 2.00 0.33 -5 -5 0 1.80 0.22 5 5 0 1.86 0.59 -6 -5 0 1.91 0.38 -6 -5 0 1.72 0.29 -6 -5 0 1.93 0.50 -6 -5 0 2.69 0.31 -6 -5 0 2.03 0.27 -7 -5 0 5.07 0.42 -7 -5 0 4.26 0.54 -8 6 0 0.16 0.08 -8 6 0 0.15 0.07 -7 6 0 2.22 0.26 -7 6 0 2.41 0.28 -6 6 0 0.11 0.11 -6 6 0 0.05 0.11 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0.17 -7 7 0 0.35 0.10 -7 7 0 0.48 0.12 -6 7 0 1.92 0.27 -6 7 0 1.65 0.22 -6 7 0 1.57 0.27 5 -7 0 0.52 0.15 -5 7 0 0.14 0.14 -5 7 0 -0.24 0.87 -5 7 0 0.19 0.11 -5 7 0 0.23 0.13 4 -7 0 3.09 0.36 -4 7 0 1.57 0.79 -4 7 0 1.99 1.50 -4 7 0 3.45 0.33 3 -7 0 0.36 0.13 3 -7 0 -0.08 0.10 -3 7 0 -0.06 0.56 -3 7 0 0.53 1.16 -3 7 0 0.10 0.09 2 -7 0 4.39 0.43 2 -7 0 4.51 0.45 -2 7 0 4.76 0.47 -2 7 0 2.52 1.52 -2 7 0 4.11 0.91 -2 7 0 3.14 0.81 -2 7 0 4.35 0.39 1 -7 0 11.05 0.90 1 -7 0 12.84 0.95 -1 7 0 10.31 1.39 -1 7 0 11.33 1.36 0 -7 0 8.73 0.82 0 -7 0 8.58 0.72 0 7 0 11.66 3.48 0 7 0 10.13 1.21 0 7 0 9.99 1.21 0 7 0 8.06 0.67 0 7 0 8.06 0.73 -1 -7 0 0.48 0.12 -1 -7 0 0.64 0.17 1 7 0 0.29 0.15 1 7 0 0.31 0.33 1 7 0 0.30 0.27 -2 -7 0 9.23 0.78 -2 -7 0 8.30 0.74 -2 -7 0 8.48 0.77 -2 -7 0 8.90 0.71 2 7 0 11.29 1.32 2 7 0 10.63 1.21 2 7 0 7.68 1.07 2 7 0 8.12 0.77 -3 -7 0 59.14 4.12 -3 -7 0 59.47 4.22 -3 -7 0 62.14 4.23 3 7 0 69.28 5.03 3 7 0 53.15 4.67 -4 -7 0 23.55 1.86 -4 -7 0 22.72 1.84 -4 -7 0 25.30 2.00 -4 -7 0 23.56 1.74 4 7 0 23.93 1.84 4 7 0 30.06 2.68 -5 -7 0 1.31 0.27 -5 -7 0 1.37 0.35 -5 -7 0 1.73 0.29 -5 -7 0 1.43 0.20 5 7 0 1.45 0.26 -6 -7 0 5.64 0.56 -6 -7 0 5.37 0.46 -6 -7 0 5.27 0.61 6 7 0 6.24 0.53 -7 -7 0 0.66 0.15 -7 8 0 3.29 0.28 -6 8 0 0.27 0.10 -6 8 0 0.32 0.12 5 -8 0 0.34 0.13 -5 8 0 0.09 0.11 -5 8 0 0.09 0.09 -5 8 0 -0.09 0.11 4 -8 0 4.63 0.48 -4 8 0 4.94 0.50 -4 8 0 5.01 1.56 -4 8 0 5.48 0.46 -4 8 0 1.75 2.29 -3 8 0 -1.93 1.73 -3 8 0 0.09 0.41 2 -8 0 33.08 2.54 2 -8 0 33.78 2.29 -2 8 0 32.53 3.28 -2 8 0 31.25 5.04 -2 8 0 26.78 2.93 -2 8 0 30.47 2.28 -2 8 0 37.40 2.31 1 -8 0 4.59 0.45 1 -8 0 4.51 0.45 -1 8 0 4.31 0.48 -1 8 0 4.04 0.90 -1 8 0 10.75 3.03 -1 8 0 4.47 0.41 0 -8 0 11.31 0.90 0 -8 0 10.68 0.89 0 -8 0 11.27 0.90 0 8 0 10.66 0.92 0 8 0 12.07 1.49 0 8 0 11.01 1.42 -1 -8 0 10.97 1.05 -1 -8 0 11.10 0.89 -1 -8 0 10.46 0.89 1 8 0 11.55 1.53 1 8 0 10.37 1.36 -2 -8 0 1.30 0.24 -2 -8 0 1.44 0.28 -2 -8 0 1.51 0.29 -2 -8 0 1.58 0.23 2 8 0 1.30 0.49 2 8 0 1.82 0.30 2 8 0 1.85 0.94 -3 -8 0 0.40 0.18 -3 -8 0 0.34 0.12 -3 -8 0 0.37 0.16 3 8 0 0.83 0.23 3 8 0 -0.15 0.49 -4 -8 0 2.20 0.40 -4 -8 0 1.86 0.46 4 8 0 1.81 0.36 -5 -8 0 0.12 0.11 -5 -8 0 0.06 0.08 -5 -8 0 0.23 0.12 -5 -8 0 0.06 0.13 5 8 0 0.09 0.12 -6 -8 0 4.27 0.49 -6 -8 0 4.96 0.39 -6 -8 0 4.63 0.43 6 8 0 5.03 0.46 -6 9 0 5.04 0.41 -6 9 0 4.29 0.38 5 -9 0 2.77 0.42 -5 9 0 2.47 0.31 -5 9 0 2.91 0.29 -5 9 0 3.25 0.33 4 -9 0 0.00 0.09 -4 9 0 0.02 0.10 -4 9 0 0.12 0.08 3 -9 0 -0.04 0.19 3 -9 0 0.18 0.11 -3 9 0 -0.76 1.94 -3 9 0 -0.07 0.08 -3 9 0 -0.59 0.70 2 -9 0 1.18 0.24 2 -9 0 1.22 0.23 -2 9 0 1.24 0.20 -2 9 0 5.57 2.64 -2 9 0 1.49 0.77 -1 9 0 0.13 0.50 -1 9 0 3.32 3.03 0 -9 0 2.32 0.30 0 -9 0 2.11 0.30 0 -9 0 1.76 0.31 0 9 0 2.65 0.84 0 9 0 1.97 0.32 0 9 0 2.34 0.91 -1 -9 0 0.28 0.14 -1 -9 0 0.10 0.11 -1 -9 0 0.08 0.11 1 9 0 -0.57 0.49 1 9 0 0.21 0.12 1 9 0 0.63 0.65 -2 -9 0 0.17 0.13 -2 -9 0 0.01 0.11 -2 -9 0 0.11 0.11 2 9 0 -0.19 0.11 2 9 0 0.59 0.60 -3 -9 0 0.07 0.15 -3 -9 0 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3 14 -0.05 0.04 4 3 14 0.02 0.06 0 -4 -14 3.65 0.39 0 4 14 4.22 0.36 -1 -4 -14 8.19 0.63 1 4 14 6.71 0.56 1 4 14 7.55 0.59 -2 -4 -14 0.22 0.11 2 4 14 0.29 0.09 2 4 14 0.35 0.11 2 4 14 0.17 0.08 3 4 14 -0.01 0.08 3 4 14 0.04 0.07 4 4 14 2.87 0.29 4 4 14 2.83 0.28 1 -5 -14 0.60 0.14 -1 5 14 0.44 0.11 0 -5 -14 14.92 1.13 0 5 14 15.07 1.10 -1 -5 -14 2.79 0.34 1 5 14 3.04 0.30 -2 -5 -14 0.22 0.12 2 5 14 0.29 0.10 2 5 14 0.26 0.10 2 5 14 0.12 0.09 3 5 14 7.59 0.60 3 5 14 7.51 0.57 3 5 14 6.96 0.55 4 5 14 0.57 0.13 4 5 14 0.44 0.10 1 -6 -14 0.08 0.08 -1 6 14 0.07 0.07 0 6 14 8.43 0.67 -1 -6 -14 1.35 0.23 1 6 14 1.31 0.22 -2 -6 -14 0.12 0.10 2 6 14 0.05 0.08 2 6 14 0.23 0.16 2 6 14 -0.01 0.08 3 6 14 20.01 1.32 3 6 14 18.78 1.34 3 6 14 17.23 1.31 4 6 14 0.18 0.08 4 6 14 0.40 0.11 1 -7 -14 3.95 0.37 -1 7 14 3.74 0.35 0 -7 -14 0.18 0.11 0 7 14 -0.13 0.07 -1 -7 -14 2.04 0.28 1 7 14 1.96 0.25 -2 -7 -14 0.13 0.11 2 7 14 0.20 0.09 2 7 14 0.21 0.09 3 7 14 3.00 0.28 3 7 14 2.67 0.28 3 7 14 2.99 0.30 4 7 14 0.60 0.11 4 7 14 0.46 0.14 0 -8 -14 2.71 0.31 0 8 14 2.73 0.28 1 8 14 15.39 1.12 -2 -8 -14 28.11 1.98 2 8 14 29.71 1.95 2 8 14 27.40 1.98 3 8 14 10.80 0.82 3 8 14 11.65 0.84 4 8 14 1.13 0.14 4 8 14 0.95 0.15 0 -9 -14 0.03 0.08 0 9 14 -0.01 0.05 -1 -9 -14 0.06 0.09 1 9 14 0.23 0.09 -2 -9 -14 6.06 0.48 2 9 14 5.86 0.49 2 9 14 5.78 0.45 3 9 14 0.30 0.09 3 9 14 0.39 0.10 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 58966 _olex2_submission_special_instructions 'No special instructions were received' ####################################################################### # # This file contains crystal structure data downloaded from the # Cambridge Structural Database (CSD) hosted by the Cambridge # Crystallographic Data Centre (CCDC). # # Full information about CCDC data access policies and citation # guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 # # Audit and citation data items may have been added by the CCDC. # Please retain this information to preserve the provenance of # this file and to allow appropriate attribution of the data. # ####################################################################### data_wll149_sq _database_code_depnum_ccdc_archive 'CCDC 2071233' loop_ _audit_author_name _audit_author_address 'Qilin Wang' ;Henan University China ; _audit_update_record ; 2021-03-27 deposited with the CCDC. 2021-11-08 downloaded from the CCDC. ; _audit_creation_date 2020-06-24 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _shelx_SHELXL_version_number 2014/7 _chemical_name_common ? _chemical_name_systematic ? _chemical_formula_moiety '1(C26 H22 N2 O5)' _chemical_formula_sum 'C26 H22 N2 O5' _chemical_formula_weight 442.45 _chemical_melting_point ? _chemical_oxdiff_formula C14H15N2O4 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.5554(4) _cell_length_b 11.9041(4) _cell_length_c 20.6216(6) _cell_angle_alpha 82.000(3) _cell_angle_beta 89.792(3) _cell_angle_gamma 61.583(4) _cell_volume 2464.17(16) _cell_formula_units_Z 4 _cell_measurement_reflns_used 6025 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 70.6170 _cell_measurement_theta_min 4.2670 _shelx_estimated_absorpt_T_max 0.941 _shelx_estimated_absorpt_T_min 0.898 _exptl_absorpt_coefficient_mu 0.685 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.59573 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_special_details ? _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.193 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description prism _exptl_crystal_F_000 928 _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.09 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0259 _diffrn_reflns_av_unetI/netI 0.0354 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 1.000 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_number 17983 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 1.000 _diffrn_reflns_theta_full 67.069 _diffrn_reflns_theta_max 67.069 _diffrn_reflns_theta_min 4.275 _diffrn_ambient_temperature 293(2) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 16.2312 _diffrn_detector_type Eos _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames #-------------------------------------------------------------------------- 1 \w -102.00 -18.00 0.50 1.50 -- -33.50 -57.00-180.00 168 2 \w -55.00 -29.00 0.50 1.50 -- -33.50 77.00 30.00 52 3 \w -7.00 25.00 0.50 1.50 -- -33.50 77.00 30.00 64 4 \w -59.00 -33.00 0.50 1.50 -- -33.50 -57.00 -90.00 52 5 \w -58.00 -32.00 0.50 1.50 -- -33.50 178.00 120.00 52 6 \w 82.00 107.00 0.50 1.50 -- 36.47 37.00 -30.00 50 7 \w 2.00 33.00 0.50 1.50 -- 36.47 -99.00-120.00 62 8 \w 9.00 98.00 0.50 1.50 -- 36.47 77.00 120.00 178 9 \w 14.00 78.00 0.50 1.50 -- 36.47 37.00 -30.00 128 10 \w 45.00 75.00 0.50 1.50 -- 36.47 -99.00-120.00 60 11 \w 15.00 41.00 0.50 1.50 -- 36.47 37.00 90.00 52 12 \w 19.00 47.00 0.50 1.50 -- 36.47 57.00 150.00 56 13 \w 49.00 75.00 0.50 1.50 -- 36.47 37.00 90.00 52 14 \w -27.00 63.00 0.50 1.50 -- 36.47 -77.00 0.00 180 15 \w 50.00 77.00 0.50 1.50 -- 36.47 -99.00 -90.00 54 16 \w 10.00 42.00 0.50 1.50 -- 36.47 -99.00 -90.00 64 17 \w 72.00 109.00 0.50 1.50 -- 36.47 178.00-120.00 74 18 \w -35.00 21.00 0.50 1.50 -- 36.47 -19.00-150.00 112 19 \w 75.00 101.00 0.50 1.50 -- 36.47 57.00 150.00 52 20 \w 80.00 105.00 0.50 7.50 -- 108.00 -94.00 -60.00 50 21 \w 89.00 168.00 0.50 7.50 -- 108.00 61.00 150.00 158 22 \w 89.00 115.00 0.50 7.50 -- 108.00 77.00 -30.00 52 23 \w 85.00 130.00 0.50 7.50 -- 108.00 -77.00 60.00 90 24 \w 43.00 111.00 0.50 7.50 -- 108.00-111.00-120.00 136 25 \w 133.00 175.00 0.50 7.50 -- 108.00 30.00-180.00 84 26 \w 41.00 128.00 0.50 7.50 -- 108.00 -45.00 0.00 174 27 \w 82.00 108.00 0.50 7.50 -- 108.00 30.00-180.00 52 28 \w 39.00 127.00 0.50 7.50 -- 108.00 -45.00-180.00 176 29 \w 55.00 109.00 0.50 7.50 -- 108.00 -94.00 90.00 108 30 \w 105.00 131.00 0.50 7.50 -- 108.00 111.00-150.00 52 31 \w 64.00 119.00 0.50 7.50 -- 108.00 178.00 60.00 110 32 \w 73.00 123.00 0.50 7.50 -- 108.00 -45.00 90.00 100 33 \w 38.00 112.00 0.50 7.50 -- 108.00-111.00 60.00 148 34 \w 64.00 178.00 0.50 7.50 -- 108.00 0.00 120.00 228 35 \w 63.00 137.00 0.50 7.50 -- 108.00 -77.00-120.00 148 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'Xcalibur, Eos, Gemini' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 0.0659802000 _diffrn_orient_matrix_UB_12 0.0556547000 _diffrn_orient_matrix_UB_13 0.0409196000 _diffrn_orient_matrix_UB_21 -0.1329452000 _diffrn_orient_matrix_UB_22 0.1242534000 _diffrn_orient_matrix_UB_23 -0.0015494000 _diffrn_orient_matrix_UB_31 -0.0327024000 _diffrn_orient_matrix_UB_32 -0.0604757000 _diffrn_orient_matrix_UB_33 0.0635926000 _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_source 'fine-focus sealed X-ray tube' _diffrn_source_type 'Enhance (Cu) X-ray Source' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 6803 _reflns_number_total 8791 _reflns_odcompleteness_completeness 99.95 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 66.97 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. Structure factors included contributions from the .fab file. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement 'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)' _computing_data_collection 'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)' _computing_data_reduction 'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'olex2.solve (Bourhis et al., 2015)' _refine_diff_density_max 0.315 _refine_diff_density_min -0.236 _refine_diff_density_rms 0.039 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 606 _refine_ls_number_reflns 8791 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0650 _refine_ls_R_factor_gt 0.0505 _refine_ls_restrained_S_all 1.035 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0852P)^2^+0.3079P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1427 _refine_ls_wR_factor_ref 0.1574 _refine_special_details ? _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All C(H,H,H) groups 2. Uiso/Uaniso restraints and constraints Uanis(C22) = Uanis(C22A) Uanis(C23) = Uanis(C23A) Uanis(C24) = Uanis(C24A) Uanis(C25) = Uanis(C25A) Uanis(C26) = Uanis(C26A) Uanis(C21) = Uanis(C21A) 3. Others Sof(C21A)=Sof(C26A)=Sof(H26A)=Sof(C25A)=Sof(H25A)=Sof(C24A)=Sof(H24A)= Sof(C23A)=Sof(H23A)=Sof(C22A)=Sof(H22A)=1-FVAR(1) Sof(C21)=Sof(C22)=Sof(H22)=Sof(C23)=Sof(H23)=Sof(C24)=Sof(H24)=Sof(C25)= Sof(H25)=Sof(C26)=Sof(H26)=FVAR(1) 4.a Ternary CH refined with riding coordinates: C8(H8), C9(H9), C10(H10), C8'(H8'), C9'(H9'), C10'(H10') 4.b Secondary CH2 refined with riding coordinates: C7(H7A,H7B), C7'(H7'A,H7'B) 4.c Aromatic/amide H refined with riding coordinates: C1(H1), C2(H2), C3(H3), C4(H4), C12(H12), C14(H14), C26A(H26A), C25A(H25A), C24A(H24A), C23A(H23A), C22A(H22A), C22(H22), C23(H23), C24(H24), C25(H25), C26(H26), C1'(H1'), C2'(H2'), C3'(H3'), C4'(H4'), C12'(H12'), C14'(H14'), C22'(H22'), C23'(H23'), C24'(H24'), C25'(H25'), C26'(H26') 4.d Fitted hexagon refined as free rotating group: C21A(C26A,C25A,C24A,C23A,C22A) 4.e Idealised Me refined as rotating group: C17(H17A,H17B,H17C), C19(H19A,H19B,H19C), C17'(H17D,H17E,H17F), C19'(H19D, H19E,H19F) ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary iterative _atom_sites_solution_secondary ? loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group O1 O 0.67898(17) 0.32221(16) 0.04745(8) 0.0639(4) Uani 1 1 d . . . . . O2 O 0.68604(18) 0.49325(19) 0.06685(9) 0.0717(5) Uani 1 1 d . . . . . O3 O 0.51418(16) 0.69678(15) 0.19450(7) 0.0552(4) Uani 1 1 d . . . . . O4 O 0.6502(2) 0.3684(2) 0.36442(10) 0.0896(6) Uani 1 1 d . . . . . O5 O 0.21684(19) 0.77285(15) 0.20304(7) 0.0639(4) Uani 1 1 d . . . . . N1 N 0.31217(16) 0.45244(15) 0.10442(8) 0.0441(4) Uani 1 1 d . . . . . N2 N 0.62783(18) 0.42887(18) 0.06695(8) 0.0524(4) Uani 1 1 d . . . . . C1 C 0.0039(2) 0.6895(2) 0.16363(12) 0.0593(5) Uani 1 1 d . . . . . H1 H 0.0156 0.7445 0.1875 0.071 Uiso 1 1 calc R . . . . C2 C -0.1195(3) 0.7005(3) 0.15389(15) 0.0737(7) Uani 1 1 d . . . . . H2 H -0.1914 0.7645 0.1710 0.088 Uiso 1 1 calc R . . . . C3 C -0.1385(3) 0.6185(3) 0.11940(14) 0.0696(7) Uani 1 1 d . . . . . H3 H -0.2226 0.6280 0.1132 0.084 Uiso 1 1 calc R . . . . C4 C -0.0328(2) 0.5224(2) 0.09404(12) 0.0601(6) Uani 1 1 d . . . . . H4 H -0.0444 0.4662 0.0710 0.072 Uiso 1 1 calc R . . . . C5 C 0.0907(2) 0.5115(2) 0.10357(10) 0.0484(4) Uani 1 1 d . . . . . C6 C 0.1098(2) 0.59492(19) 0.13718(9) 0.0454(4) Uani 1 1 d . . . . . C7 C 0.2198(2) 0.4099(2) 0.08444(12) 0.0561(5) Uani 1 1 d . . . . . H7A H 0.2420 0.3247 0.1077 0.067 Uiso 1 1 calc R . . . . H7B H 0.2180 0.4084 0.0376 0.067 Uiso 1 1 calc R . . . . C8 C 0.25286(19) 0.56140(17) 0.14203(9) 0.0407(4) Uani 1 1 d . . . . . H8 H 0.2881 0.5315 0.1879 0.049 Uiso 1 1 calc R . . . . C9 C 0.28917(19) 0.66462(17) 0.11092(9) 0.0416(4) Uani 1 1 d . . . . . H9 H 0.2562 0.6900 0.0646 0.050 Uiso 1 1 calc R . . . . C10 C 0.4429(2) 0.60635(19) 0.11411(9) 0.0446(4) Uani 1 1 d . . . . . H10 H 0.4634 0.6649 0.0841 0.054 Uiso 1 1 calc R . . . . C11 C 0.5000(2) 0.47942(19) 0.08897(9) 0.0441(4) Uani 1 1 d . . . . . C12 C 0.4298(2) 0.41650(18) 0.08160(9) 0.0446(4) Uani 1 1 d . . . . . H12 H 0.4659 0.3454 0.0596 0.054 Uiso 1 1 calc R . . . . C13 C 0.5038(2) 0.5913(2) 0.18111(10) 0.0476(4) Uani 1 1 d . . . . . C14 C 0.5500(2) 0.4986(2) 0.23309(10) 0.0510(5) Uani 1 1 d . . . . . H14 H 0.5548 0.4178 0.2362 0.061 Uiso 1 1 calc R . . . . C15 C 0.5913(2) 0.5469(2) 0.28403(10) 0.0538(5) Uani 1 1 d . . . . . C16 C 0.5677(2) 0.6678(2) 0.25760(11) 0.0564(5) Uani 1 1 d . . . . . C17 C 0.5819(4) 0.7757(3) 0.27956(15) 0.0856(9) Uani 1 1 d . . . . . H17A H 0.6733 0.7471 0.2905 0.128 Uiso 1 1 calc GR . . . . H17B H 0.5328 0.8008 0.3174 0.128 Uiso 1 1 calc GR . . . . H17C H 0.5486 0.8482 0.2448 0.128 Uiso 1 1 calc GR . . . . C18 C 0.6423(2) 0.4737(3) 0.35018(12) 0.0637(6) Uani 1 1 d . . . . . C19 C 0.6801(4) 0.5327(4) 0.40068(15) 0.0949(10) Uani 1 1 d . . . . . H19A H 0.6957 0.4807 0.4430 0.142 Uiso 1 1 calc GR . . . . H19B H 0.6099 0.6185 0.4021 0.142 Uiso 1 1 calc GR . . . . H19C H 0.7589 0.5365 0.3892 0.142 Uiso 1 1 calc GR . . . . C20 C 0.2251(2) 0.78473(19) 0.14428(9) 0.0441(4) Uani 1 1 d . . . . . C21 C 0.1736(17) 0.9061(11) 0.1074(9) 0.0466(6) Uani 0.268(10) 1 d . . P A 1 C21A C 0.1709(5) 0.9182(3) 0.1023(3) 0.0466(6) Uani 0.732(10) 1 d . . P A 2 C26A C 0.1907(7) 0.9358(5) 0.0359(3) 0.0589(16) Uani 0.732(10) 1 d G . P A 2 H26A H 0.2433 0.8648 0.0157 0.071 Uiso 0.732(10) 1 calc R . P A 2 C25A C 0.1318(7) 1.0596(6) -0.00023(19) 0.0859(11) Uani 0.732(10) 1 d G . P A 2 H25A H 0.1450 1.0713 -0.0446 0.103 Uiso 0.732(10) 1 calc R . P A 2 C24A C 0.0531(6) 1.1657(4) 0.02997(18) 0.0859(17) Uani 0.732(10) 1 d G . P A 2 H24A H 0.0137 1.2485 0.0058 0.103 Uiso 0.732(10) 1 calc R . P A 2 C23A C 0.0333(7) 1.1481(3) 0.0963(2) 0.0910(19) Uani 0.732(10) 1 d G . P A 2 H23A H -0.0194 1.2191 0.1165 0.109 Uiso 0.732(10) 1 calc R . P A 2 C22A C 0.0922(5) 1.0244(3) 0.13248(19) 0.0658(12) Uani 0.732(10) 1 d G . P A 2 H22A H 0.0789 1.0126 0.1769 0.079 Uiso 0.732(10) 1 calc R . P A 2 C22 C 0.1465(15) 1.0119(13) 0.1410(7) 0.0658(12) Uani 0.268(10) 1 d . . P A 1 H22 H 0.1565 0.9988 0.1866 0.079 Uiso 0.268(10) 1 calc R . P A 1 C23 C 0.1047(19) 1.1354(12) 0.1055(8) 0.0910(19) Uani 0.268(10) 1 d . . P A 1 H23 H 0.0777 1.2054 0.1280 0.109 Uiso 0.268(10) 1 calc R . P A 1 C24 C 0.1029(18) 1.1543(16) 0.0414(8) 0.0859(17) Uani 0.268(10) 1 d . . P A 1 H24 H 0.0800 1.2360 0.0187 0.103 Uiso 0.268(10) 1 calc R . P A 1 C25 C 0.134(2) 1.057(2) 0.0095(9) 0.0859(11) Uani 0.268(10) 1 d . . P A 1 H25 H 0.1334 1.0718 -0.0360 0.103 Uiso 0.268(10) 1 calc R . P A 1 C26 C 0.166(3) 0.9334(17) 0.0403(10) 0.0589(16) Uani 0.268(10) 1 d . . P A 1 H26 H 0.1829 0.8687 0.0152 0.071 Uiso 0.268(10) 1 calc R . P A 1 O1' O 0.5293(2) 0.11579(18) 0.57420(7) 0.0687(5) Uani 1 1 d . . . . . O2' O 0.3206(2) 0.20164(19) 0.54454(9) 0.0739(5) Uani 1 1 d . . . . . O3' O 0.14318(16) 0.42474(15) 0.39147(10) 0.0654(4) Uani 1 1 d . . . . . O4' O 0.07122(19) 0.81001(16) 0.36601(12) 0.0804(5) Uani 1 1 d . . . . . O5' O 0.29746(16) 0.34175(15) 0.25562(8) 0.0624(4) Uani 1 1 d . . . . . N1' N 0.62565(17) 0.10750(16) 0.38845(8) 0.0476(4) Uani 1 1 d . . . . . N2' N 0.4366(2) 0.16023(17) 0.53064(9) 0.0552(5) Uani 1 1 d . . . . . C1' C 0.5649(3) 0.1600(2) 0.20895(11) 0.0638(6) Uani 1 1 d . . . . . H1' H 0.4772 0.2163 0.1944 0.077 Uiso 1 1 calc R . . . . C2' C 0.6591(3) 0.1053(3) 0.16417(12) 0.0741(7) Uani 1 1 d . . . . . H2' H 0.6336 0.1259 0.1195 0.089 Uiso 1 1 calc R . . . . C3' C 0.7880(3) 0.0221(2) 0.18483(11) 0.0654(6) Uani 1 1 d . . . . . H3' H 0.8494 -0.0127 0.1542 0.078 Uiso 1 1 calc R . . . . C4' C 0.8280(2) -0.0107(2) 0.25111(12) 0.0597(5) Uani 1 1 d . . . . . H4' H 0.9155 -0.0680 0.2654 0.072 Uiso 1 1 calc R . . . . C5' C 0.7347(2) 0.0437(2) 0.29564(10) 0.0493(5) Uani 1 1 d . . . . . C6' C 0.6039(2) 0.12935(19) 0.27531(9) 0.0468(4) Uani 1 1 d . . . . . C7' C 0.7583(2) 0.0283(3) 0.36835(11) 0.0619(6) Uani 1 1 d . . . . . H7'A H 0.7943 -0.0614 0.3885 0.074 Uiso 1 1 calc R . . . . H7'B H 0.8176 0.0602 0.3794 0.074 Uiso 1 1 calc R . . . . C8' C 0.5261(2) 0.18437(18) 0.33277(9) 0.0441(4) Uani 1 1 d . . . . . H8' H 0.5051 0.2751 0.3295 0.053 Uiso 1 1 calc R . . . . C9' C 0.4012(2) 0.17431(18) 0.34655(9) 0.0438(4) Uani 1 1 d . . . . . H9' H 0.4218 0.0837 0.3497 0.053 Uiso 1 1 calc R . . . . C10' C 0.3492(2) 0.22310(19) 0.41363(10) 0.0470(4) Uani 1 1 d . . . . . H10' H 0.2872 0.1918 0.4280 0.056 Uiso 1 1 calc R . . . . C11' C 0.4633(2) 0.16417(19) 0.46405(9) 0.0477(4) Uani 1 1 d . . . . . C12' C 0.5916(2) 0.10537(19) 0.44906(9) 0.0479(5) Uani 1 1 d . . . . . H12' H 0.6574 0.0622 0.4830 0.058 Uiso 1 1 calc R . . . . C13' C 0.2773(2) 0.3681(2) 0.40593(10) 0.0486(4) Uani 1 1 d . . . . . C14' C 0.3124(2) 0.4604(2) 0.40344(11) 0.0512(5) Uani 1 1 d . . . . . H14' H 0.3974 0.4479 0.4106 0.061 Uiso 1 1 calc R . . . . C15' C 0.1940(2) 0.5828(2) 0.38750(12) 0.0534(5) Uani 1 1 d . . . . . C16' C 0.0949(2) 0.5555(2) 0.37998(15) 0.0665(6) Uani 1 1 d . . . . . C17' C -0.0492(3) 0.6346(3) 0.3610(2) 0.1043(12) Uani 1 1 d . . . . . H17D H -0.0760 0.5905 0.3340 0.156 Uiso 1 1 calc GR . . . . H17E H -0.0671 0.7170 0.3371 0.156 Uiso 1 1 calc GR . . . . H17F H -0.0972 0.6472 0.3998 0.156 Uiso 1 1 calc GR . . . . C18' C 0.1784(2) 0.7144(2) 0.37727(13) 0.0623(6) Uani 1 1 d . . . . . C19' C 0.3002(3) 0.7266(3) 0.3809(2) 0.1027(12) Uani 1 1 d . . . . . H19D H 0.2773 0.8164 0.3730 0.154 Uiso 1 1 calc GR . . . . H19E H 0.3572 0.6829 0.3484 0.154 Uiso 1 1 calc GR . . . . H19F H 0.3448 0.6884 0.4238 0.154 Uiso 1 1 calc GR . . . . C20' C 0.2916(2) 0.25592(19) 0.29266(9) 0.0465(4) Uani 1 1 d . . . . . C21' C 0.1749(2) 0.2350(2) 0.28754(9) 0.0474(4) Uani 1 1 d . . . . . C22' C 0.0592(2) 0.3369(2) 0.25562(11) 0.0574(5) Uani 1 1 d . . . . . H22' H 0.0575 0.4141 0.2382 0.069 Uiso 1 1 calc R . . . . C23' C -0.0525(3) 0.3247(3) 0.24962(13) 0.0678(6) Uani 1 1 d . . . . . H23' H -0.1297 0.3937 0.2286 0.081 Uiso 1 1 calc R . . . . C24' C -0.0499(3) 0.2094(3) 0.27500(14) 0.0715(7) Uani 1 1 d . . . . . H24' H -0.1254 0.2010 0.2709 0.086 Uiso 1 1 calc R . . . . C25' C 0.0635(3) 0.1079(3) 0.30612(13) 0.0687(7) Uani 1 1 d . . . . . H25' H 0.0649 0.0305 0.3226 0.082 Uiso 1 1 calc R . . . . C26' C 0.1765(3) 0.1198(2) 0.31323(11) 0.0588(5) Uani 1 1 d . . . . . H26' H 0.2529 0.0510 0.3351 0.071 Uiso 1 1 calc R . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.0622(10) 0.0611(10) 0.0576(9) -0.0195(7) 0.0172(7) -0.0184(8) O2 0.0637(10) 0.0906(13) 0.0774(11) -0.0260(10) 0.0197(8) -0.0471(10) O3 0.0706(10) 0.0579(9) 0.0521(8) -0.0156(7) 0.0099(7) -0.0411(8) O4 0.1115(17) 0.1039(16) 0.0703(12) 0.0106(11) -0.0250(11) -0.0713(14) O5 0.0958(13) 0.0563(9) 0.0415(8) -0.0137(6) 0.0158(8) -0.0366(9) N1 0.0496(9) 0.0361(8) 0.0457(8) -0.0061(6) 0.0010(7) -0.0200(7) N2 0.0538(10) 0.0606(11) 0.0402(9) -0.0106(8) 0.0063(7) -0.0246(9) C1 0.0579(13) 0.0551(13) 0.0675(14) -0.0134(10) 0.0124(10) -0.0283(11) C2 0.0538(14) 0.0632(15) 0.100(2) -0.0145(14) 0.0163(13) -0.0242(12) C3 0.0523(13) 0.0659(15) 0.0878(18) 0.0008(13) -0.0029(12) -0.0294(12) C4 0.0610(14) 0.0581(13) 0.0642(13) 0.0011(10) -0.0080(10) -0.0337(11) C5 0.0529(11) 0.0440(10) 0.0480(10) 0.0008(8) -0.0019(8) -0.0252(9) C6 0.0515(11) 0.0408(10) 0.0414(9) 0.0009(7) 0.0019(8) -0.0220(9) C7 0.0597(13) 0.0484(12) 0.0657(13) -0.0144(10) 0.0018(10) -0.0289(10) C8 0.0481(10) 0.0373(9) 0.0362(9) -0.0044(7) 0.0017(7) -0.0204(8) C9 0.0526(11) 0.0377(9) 0.0346(9) -0.0050(7) 0.0036(7) -0.0220(8) C10 0.0541(11) 0.0468(10) 0.0389(9) -0.0066(8) 0.0080(8) -0.0290(9) C11 0.0488(11) 0.0459(10) 0.0366(9) -0.0078(7) 0.0059(8) -0.0215(9) C12 0.0524(11) 0.0364(9) 0.0386(9) -0.0061(7) 0.0003(8) -0.0161(8) C13 0.0509(11) 0.0537(11) 0.0488(11) -0.0171(9) 0.0101(8) -0.0313(10) C14 0.0538(12) 0.0553(12) 0.0491(11) -0.0109(9) 0.0028(9) -0.0297(10) C15 0.0498(11) 0.0705(14) 0.0487(11) -0.0176(10) 0.0074(9) -0.0328(11) C16 0.0609(13) 0.0753(15) 0.0514(12) -0.0243(10) 0.0134(10) -0.0437(12) C17 0.122(3) 0.098(2) 0.0758(17) -0.0360(16) 0.0179(17) -0.078(2) C18 0.0588(14) 0.0897(18) 0.0533(12) -0.0118(12) -0.0004(10) -0.0439(13) C19 0.108(3) 0.126(3) 0.0669(17) -0.0174(17) -0.0148(16) -0.069(2) C20 0.0520(11) 0.0458(10) 0.0413(10) -0.0117(8) 0.0100(8) -0.0275(9) C21 0.0535(12) 0.0374(12) 0.0497(15) -0.0090(11) 0.0085(10) -0.0219(11) C21A 0.0535(12) 0.0374(12) 0.0497(15) -0.0090(11) 0.0085(10) -0.0219(11) C26A 0.085(4) 0.0445(12) 0.0482(15) -0.0088(10) 0.0119(17) -0.0316(16) C25A 0.145(3) 0.0569(15) 0.045(2) 0.0017(16) -0.002(2) -0.0423(18) C24A 0.113(5) 0.0410(17) 0.074(3) 0.0094(16) -0.025(3) -0.018(3) C23A 0.100(5) 0.0382(16) 0.092(3) -0.0158(16) 0.008(3) 0.003(3) C22A 0.072(3) 0.0483(16) 0.0592(19) -0.0122(14) 0.011(2) -0.013(2) C22 0.072(3) 0.0483(16) 0.0592(19) -0.0122(14) 0.011(2) -0.013(2) C23 0.100(5) 0.0382(16) 0.092(3) -0.0158(16) 0.008(3) 0.003(3) C24 0.113(5) 0.0410(17) 0.074(3) 0.0094(16) -0.025(3) -0.018(3) C25 0.145(3) 0.0569(15) 0.045(2) 0.0017(16) -0.002(2) -0.0423(18) C26 0.085(4) 0.0445(12) 0.0482(15) -0.0088(10) 0.0119(17) -0.0316(16) O1' 0.0961(13) 0.0721(11) 0.0388(8) -0.0052(7) -0.0006(8) -0.0419(10) O2' 0.0865(13) 0.0844(13) 0.0590(10) -0.0198(9) 0.0271(9) -0.0454(11) O3' 0.0487(9) 0.0499(9) 0.1018(13) -0.0172(8) 0.0121(8) -0.0256(7) O4' 0.0621(11) 0.0431(9) 0.1193(16) -0.0073(9) 0.0003(10) -0.0132(8) O5' 0.0581(9) 0.0557(9) 0.0657(9) 0.0209(7) -0.0071(7) -0.0290(8) N1' 0.0504(9) 0.0462(9) 0.0402(8) -0.0045(7) -0.0021(7) -0.0189(8) N2' 0.0812(14) 0.0467(9) 0.0432(9) -0.0085(7) 0.0106(9) -0.0348(9) C1' 0.0646(14) 0.0598(13) 0.0427(11) 0.0016(9) -0.0026(10) -0.0128(11) C2' 0.0881(19) 0.0709(16) 0.0399(11) -0.0045(10) 0.0044(11) -0.0206(14) C3' 0.0746(16) 0.0607(14) 0.0516(12) -0.0184(10) 0.0174(11) -0.0227(12) C4' 0.0553(13) 0.0559(13) 0.0588(13) -0.0156(10) 0.0048(10) -0.0177(10) C5' 0.0518(11) 0.0459(11) 0.0476(11) -0.0092(8) 0.0007(8) -0.0209(9) C6' 0.0541(11) 0.0414(10) 0.0421(10) -0.0025(8) 0.0023(8) -0.0217(9) C7' 0.0483(12) 0.0757(16) 0.0500(12) -0.0127(11) -0.0016(9) -0.0196(11) C8' 0.0518(11) 0.0365(9) 0.0406(9) -0.0021(7) -0.0002(8) -0.0194(8) C9' 0.0531(11) 0.0354(9) 0.0410(9) 0.0004(7) -0.0008(8) -0.0214(8) C10' 0.0554(11) 0.0428(10) 0.0465(10) -0.0045(8) 0.0069(8) -0.0270(9) C11' 0.0653(13) 0.0405(10) 0.0374(9) -0.0028(7) 0.0040(8) -0.0264(9) C12' 0.0604(12) 0.0414(10) 0.0384(10) -0.0033(7) -0.0054(8) -0.0222(9) C13' 0.0443(10) 0.0452(11) 0.0534(11) -0.0070(8) 0.0083(8) -0.0194(9) C14' 0.0433(11) 0.0450(11) 0.0646(13) -0.0099(9) 0.0060(9) -0.0202(9) C15' 0.0459(11) 0.0430(11) 0.0676(13) -0.0111(9) 0.0087(9) -0.0176(9) C16' 0.0482(12) 0.0476(12) 0.0986(19) -0.0158(12) 0.0106(12) -0.0177(10) C17' 0.0465(15) 0.0706(19) 0.189(4) -0.028(2) 0.0022(18) -0.0205(13) C18' 0.0548(13) 0.0465(12) 0.0805(16) -0.0106(11) 0.0089(11) -0.0201(11) C19' 0.0669(18) 0.0561(16) 0.190(4) -0.0210(19) 0.022(2) -0.0332(14) C20' 0.0524(11) 0.0391(10) 0.0431(10) 0.0004(8) 0.0020(8) -0.0199(9) C21' 0.0551(11) 0.0475(11) 0.0392(9) -0.0031(8) 0.0022(8) -0.0254(9) C22' 0.0561(13) 0.0551(12) 0.0587(13) 0.0015(10) 0.0005(10) -0.0276(10) C23' 0.0543(13) 0.0706(16) 0.0726(15) 0.0000(12) -0.0013(11) -0.0282(12) C24' 0.0679(16) 0.0869(19) 0.0753(16) -0.0123(14) 0.0066(12) -0.0499(15) C25' 0.0824(18) 0.0663(15) 0.0719(15) -0.0023(12) 0.0001(13) -0.0495(14) C26' 0.0679(14) 0.0516(12) 0.0590(13) -0.0002(10) -0.0024(10) -0.0325(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1 N2 1.245(2) . ? O2 N2 1.237(3) . ? O3 C13 1.381(2) . ? O3 C16 1.368(3) . ? O4 C18 1.206(3) . ? O5 C20 1.209(2) . ? N1 C7 1.464(3) . ? N1 C8 1.478(2) . ? N1 C12 1.322(3) . ? N2 C11 1.405(3) . ? C1 H1 0.9300 . ? C1 C2 1.381(4) . ? C1 C6 1.384(3) . ? C2 H2 0.9300 . ? C2 C3 1.380(4) . ? C3 H3 0.9300 . ? C3 C4 1.381(4) . ? C4 H4 0.9300 . ? C4 C5 1.381(3) . ? C5 C6 1.384(3) . ? C5 C7 1.502(3) . ? C6 C8 1.505(3) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 H8 0.9800 . ? C8 C9 1.538(2) . ? C9 H9 0.9800 . ? C9 C10 1.567(3) . ? C9 C20 1.526(3) . ? C10 H10 0.9800 . ? C10 C11 1.501(3) . ? C10 C13 1.502(3) . ? C11 C12 1.362(3) . ? C12 H12 0.9300 . ? C13 C14 1.329(3) . ? C14 H14 0.9300 . ? C14 C15 1.447(3) . ? C15 C16 1.361(3) . ? C15 C18 1.468(3) . ? C16 C17 1.499(3) . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 C19 1.506(4) . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 C21 1.379(13) . ? C20 C21A 1.530(4) . ? C21 C22 1.424(15) . ? C21 C26 1.370(13) . ? C21A C26A 1.3900 . ? C21A C22A 1.3900 . ? C26A H26A 0.9300 . ? C26A C25A 1.3900 . ? C25A H25A 0.9300 . ? C25A C24A 1.3900 . ? C24A H24A 0.9300 . ? C24A C23A 1.3900 . ? C23A H23A 0.9300 . ? C23A C22A 1.3900 . ? C22A H22A 0.9300 . ? C22 H22 0.9300 . ? C22 C23 1.399(17) . ? C23 H23 0.9300 . ? C23 C24 1.31(2) . ? C24 H24 0.9300 . ? C24 C25 1.31(2) . ? C25 H25 0.9300 . ? C25 C26 1.389(14) . ? C26 H26 0.9300 . ? O1' N2' 1.252(3) . ? O2' N2' 1.237(3) . ? O3' C13' 1.377(3) . ? O3' C16' 1.365(3) . ? O4' C18' 1.212(3) . ? O5' C20' 1.217(2) . ? N1' C7' 1.462(3) . ? N1' C8' 1.482(2) . ? N1' C12' 1.309(3) . ? N2' C11' 1.406(3) . ? C1' H1' 0.9300 . ? C1' C2' 1.395(4) . ? C1' C6' 1.385(3) . ? C2' H2' 0.9300 . ? C2' C3' 1.365(4) . ? C3' H3' 0.9300 . ? C3' C4' 1.385(3) . ? C4' H4' 0.9300 . ? C4' C5' 1.385(3) . ? C5' C6' 1.386(3) . ? C5' C7' 1.495(3) . ? C6' C8' 1.513(3) . ? C7' H7'A 0.9700 . ? C7' H7'B 0.9700 . ? C8' H8' 0.9800 . ? C8' C9' 1.526(3) . ? C9' H9' 0.9800 . ? C9' C10' 1.580(3) . ? C9' C20' 1.524(3) . ? C10' H10' 0.9800 . ? C10' C11' 1.497(3) . ? C10' C13' 1.501(3) . ? C11' C12' 1.361(3) . ? C12' H12' 0.9300 . ? C13' C14' 1.335(3) . ? C14' H14' 0.9300 . ? C14' C15' 1.441(3) . ? C15' C16' 1.345(3) . ? C15' C18' 1.474(3) . ? C16' C17' 1.490(4) . ? C17' H17D 0.9600 . ? C17' H17E 0.9600 . ? C17' H17F 0.9600 . ? C18' C19' 1.485(4) . ? C19' H19D 0.9600 . ? C19' H19E 0.9600 . ? C19' H19F 0.9600 . ? C20' C21' 1.490(3) . ? C21' C22' 1.390(3) . ? C21' C26' 1.391(3) . ? C22' H22' 0.9300 . ? C22' C23' 1.374(3) . ? C23' H23' 0.9300 . ? C23' C24' 1.385(4) . ? C24' H24' 0.9300 . ? C24' C25' 1.368(4) . ? C25' H25' 0.9300 . ? C25' C26' 1.389(4) . ? C26' H26' 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C16 O3 C13 107.37(17) . . ? C7 N1 C8 113.72(16) . . ? C12 N1 C7 124.37(17) . . ? C12 N1 C8 120.74(16) . . ? O1 N2 C11 119.78(19) . . ? O2 N2 O1 121.71(19) . . ? O2 N2 C11 118.51(19) . . ? C2 C1 H1 120.6 . . ? C2 C1 C6 118.7(2) . . ? C6 C1 H1 120.6 . . ? C1 C2 H2 119.3 . . ? C3 C2 C1 121.5(3) . . ? C3 C2 H2 119.3 . . ? C2 C3 H3 120.0 . . ? C2 C3 C4 120.0(2) . . ? C4 C3 H3 120.0 . . ? C3 C4 H4 120.7 . . ? C3 C4 C5 118.6(2) . . ? C5 C4 H4 120.7 . . ? C4 C5 C6 121.6(2) . . ? C4 C5 C7 127.6(2) . . ? C6 C5 C7 110.71(18) . . ? C1 C6 C5 119.6(2) . . ? C1 C6 C8 129.0(2) . . ? C5 C6 C8 111.30(18) . . ? N1 C7 C5 102.23(16) . . ? N1 C7 H7A 111.3 . . ? N1 C7 H7B 111.3 . . ? C5 C7 H7A 111.3 . . ? C5 C7 H7B 111.3 . . ? H7A C7 H7B 109.2 . . ? N1 C8 C6 101.49(15) . . ? N1 C8 H8 109.9 . . ? N1 C8 C9 107.58(15) . . ? C6 C8 H8 109.9 . . ? C6 C8 C9 117.68(16) . . ? C9 C8 H8 109.9 . . ? C8 C9 H9 108.2 . . ? C8 C9 C10 109.88(15) . . ? C10 C9 H9 108.2 . . ? C20 C9 C8 111.24(15) . . ? C20 C9 H9 108.2 . . ? C20 C9 C10 111.03(15) . . ? C9 C10 H10 107.8 . . ? C11 C10 C9 107.94(15) . . ? C11 C10 H10 107.8 . . ? C11 C10 C13 111.30(17) . . ? C13 C10 C9 113.98(16) . . ? C13 C10 H10 107.8 . . ? N2 C11 C10 118.41(17) . . ? C12 C11 N2 118.48(18) . . ? C12 C11 C10 122.88(18) . . ? N1 C12 C11 122.65(18) . . ? N1 C12 H12 118.7 . . ? C11 C12 H12 118.7 . . ? O3 C13 C10 115.32(18) . . ? C14 C13 O3 109.86(18) . . ? C14 C13 C10 134.80(19) . . ? C13 C14 H14 126.4 . . ? C13 C14 C15 107.3(2) . . ? C15 C14 H14 126.4 . . ? C14 C15 C18 123.3(2) . . ? C16 C15 C14 105.94(19) . . ? C16 C15 C18 130.8(2) . . ? O3 C16 C17 113.3(2) . . ? C15 C16 O3 109.54(18) . . ? C15 C16 C17 137.2(2) . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17B 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? O4 C18 C15 119.9(2) . . ? O4 C18 C19 120.3(3) . . ? C15 C18 C19 119.7(3) . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19B 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? O5 C20 C9 119.59(18) . . ? O5 C20 C21 120.2(7) . . ? O5 C20 C21A 121.3(3) . . ? C9 C20 C21A 119.1(2) . . ? C21 C20 C9 120.2(7) . . ? C20 C21 C22 117.7(14) . . ? C26 C21 C20 126.1(12) . . ? C26 C21 C22 115.3(9) . . ? C26A C21A C20 123.0(3) . . ? C26A C21A C22A 120.0 . . ? C22A C21A C20 116.9(3) . . ? C21A C26A H26A 120.0 . . ? C21A C26A C25A 120.0 . . ? C25A C26A H26A 120.0 . . ? C26A C25A H25A 120.0 . . ? C26A C25A C24A 120.0 . . ? C24A C25A H25A 120.0 . . ? C25A C24A H24A 120.0 . . ? C23A C24A C25A 120.0 . . ? C23A C24A H24A 120.0 . . ? C24A C23A H23A 120.0 . . ? C24A C23A C22A 120.0 . . ? C22A C23A H23A 120.0 . . ? C21A C22A H22A 120.0 . . ? C23A C22A C21A 120.0 . . ? C23A C22A H22A 120.0 . . ? C21 C22 H22 119.9 . . ? C23 C22 C21 120.1(11) . . ? C23 C22 H22 119.9 . . ? C22 C23 H23 119.4 . . ? C24 C23 C22 121.3(12) . . ? C24 C23 H23 119.4 . . ? C23 C24 H24 120.3 . . ? C23 C24 C25 119.4(12) . . ? C25 C24 H24 120.3 . . ? C24 C25 H25 118.4 . . ? C24 C25 C26 123.3(12) . . ? C26 C25 H25 118.4 . . ? C21 C26 C25 120.3(9) . . ? C21 C26 H26 119.9 . . ? C25 C26 H26 119.9 . . ? C16' O3' C13' 107.76(17) . . ? C7' N1' C8' 113.77(16) . . ? C12' N1' C7' 124.85(17) . . ? C12' N1' C8' 121.15(18) . . ? O1' N2' C11' 120.0(2) . . ? O2' N2' O1' 121.64(19) . . ? O2' N2' C11' 118.4(2) . . ? C2' C1' H1' 120.5 . . ? C6' C1' H1' 120.5 . . ? C6' C1' C2' 119.0(2) . . ? C1' C2' H2' 119.5 . . ? C3' C2' C1' 121.1(2) . . ? C3' C2' H2' 119.5 . . ? C2' C3' H3' 119.8 . . ? C2' C3' C4' 120.5(2) . . ? C4' C3' H3' 119.8 . . ? C3' C4' H4' 120.7 . . ? C5' C4' C3' 118.5(2) . . ? C5' C4' H4' 120.7 . . ? C4' C5' C6' 121.6(2) . . ? C4' C5' C7' 127.1(2) . . ? C6' C5' C7' 111.17(19) . . ? C1' C6' C5' 119.3(2) . . ? C1' C6' C8' 129.6(2) . . ? C5' C6' C8' 110.90(17) . . ? N1' C7' C5' 102.31(17) . . ? N1' C7' H7'A 111.3 . . ? N1' C7' H7'B 111.3 . . ? C5' C7' H7'A 111.3 . . ? C5' C7' H7'B 111.3 . . ? H7'A C7' H7'B 109.2 . . ? N1' C8' C6' 101.10(16) . . ? N1' C8' H8' 108.8 . . ? N1' C8' C9' 108.61(15) . . ? C6' C8' H8' 108.8 . . ? C6' C8' C9' 120.06(17) . . ? C9' C8' H8' 108.8 . . ? C8' C9' H9' 109.0 . . ? C8' C9' C10' 109.86(16) . . ? C10' C9' H9' 109.0 . . ? C20' C9' C8' 111.77(15) . . ? C20' C9' H9' 109.0 . . ? C20' C9' C10' 108.03(16) . . ? C9' C10' H10' 108.1 . . ? C11' C10' C9' 108.64(17) . . ? C11' C10' H10' 108.1 . . ? C11' C10' C13' 112.23(17) . . ? C13' C10' C9' 111.63(16) . . ? C13' C10' H10' 108.1 . . ? N2' C11' C10' 118.1(2) . . ? C12' C11' N2' 118.18(19) . . ? C12' C11' C10' 123.48(18) . . ? N1' C12' C11' 122.30(18) . . ? N1' C12' H12' 118.9 . . ? C11' C12' H12' 118.9 . . ? O3' C13' C10' 115.04(18) . . ? C14' C13' O3' 109.13(18) . . ? C14' C13' C10' 135.5(2) . . ? C13' C14' H14' 126.4 . . ? C13' C14' C15' 107.16(19) . . ? C15' C14' H14' 126.4 . . ? C14' C15' C18' 129.1(2) . . ? C16' C15' C14' 106.4(2) . . ? C16' C15' C18' 124.4(2) . . ? O3' C16' C17' 116.0(2) . . ? C15' C16' O3' 109.5(2) . . ? C15' C16' C17' 134.5(2) . . ? C16' C17' H17D 109.5 . . ? C16' C17' H17E 109.5 . . ? C16' C17' H17F 109.5 . . ? H17D C17' H17E 109.5 . . ? H17D C17' H17F 109.5 . . ? H17E C17' H17F 109.5 . . ? O4' C18' C15' 122.1(2) . . ? O4' C18' C19' 120.5(2) . . ? C15' C18' C19' 117.4(2) . . ? C18' C19' H19D 109.5 . . ? C18' C19' H19E 109.5 . . ? C18' C19' H19F 109.5 . . ? H19D C19' H19E 109.5 . . ? H19D C19' H19F 109.5 . . ? H19E C19' H19F 109.5 . . ? O5' C20' C9' 119.48(19) . . ? O5' C20' C21' 120.28(18) . . ? C21' C20' C9' 120.17(16) . . ? C22' C21' C20' 117.55(18) . . ? C22' C21' C26' 119.2(2) . . ? C26' C21' C20' 123.3(2) . . ? C21' C22' H22' 119.7 . . ? C23' C22' C21' 120.7(2) . . ? C23' C22' H22' 119.7 . . ? C22' C23' H23' 120.1 . . ? C22' C23' C24' 119.8(2) . . ? C24' C23' H23' 120.1 . . ? C23' C24' H24' 119.9 . . ? C25' C24' C23' 120.2(2) . . ? C25' C24' H24' 119.9 . . ? C24' C25' H25' 119.8 . . ? C24' C25' C26' 120.5(2) . . ? C26' C25' H25' 119.8 . . ? C21' C26' H26' 120.1 . . ? C25' C26' C21' 119.7(2) . . ? C25' C26' H26' 120.1 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 N2 C11 C10 178.13(17) . . . . ? O1 N2 C11 C12 -7.1(3) . . . . ? O2 N2 C11 C10 -2.7(3) . . . . ? O2 N2 C11 C12 172.07(18) . . . . ? O3 C13 C14 C15 0.9(2) . . . . ? O5 C20 C21 C22 18(2) . . . . ? O5 C20 C21 C26 -174.0(12) . . . . ? O5 C20 C21A C26A 172.9(3) . . . . ? O5 C20 C21A C22A -10.9(6) . . . . ? N1 C8 C9 C10 -59.96(19) . . . . ? N1 C8 C9 C20 176.68(15) . . . . ? N2 C11 C12 N1 175.78(17) . . . . ? C1 C2 C3 C4 0.3(4) . . . . ? C1 C6 C8 N1 179.2(2) . . . . ? C1 C6 C8 C9 -63.7(3) . . . . ? C2 C1 C6 C5 -2.0(3) . . . . ? C2 C1 C6 C8 -178.5(2) . . . . ? C2 C3 C4 C5 -0.5(4) . . . . ? C3 C4 C5 C6 -0.6(3) . . . . ? C3 C4 C5 C7 175.6(2) . . . . ? C4 C5 C6 C1 1.8(3) . . . . ? C4 C5 C6 C8 178.90(18) . . . . ? C4 C5 C7 N1 177.7(2) . . . . ? C5 C6 C8 N1 2.5(2) . . . . ? C5 C6 C8 C9 119.54(18) . . . . ? C6 C1 C2 C3 0.9(4) . . . . ? C6 C5 C7 N1 -5.8(2) . . . . ? C6 C8 C9 C10 -173.67(15) . . . . ? C6 C8 C9 C20 63.0(2) . . . . ? C7 N1 C8 C6 -6.5(2) . . . . ? C7 N1 C8 C9 -130.71(17) . . . . ? C7 N1 C12 C11 164.30(19) . . . . ? C7 C5 C6 C1 -174.92(19) . . . . ? C7 C5 C6 C8 2.1(2) . . . . ? C8 N1 C7 C5 7.7(2) . . . . ? C8 N1 C12 C11 -2.5(3) . . . . ? C8 C9 C10 C11 48.82(19) . . . . ? C8 C9 C10 C13 -75.4(2) . . . . ? C8 C9 C20 O5 38.1(3) . . . . ? C8 C9 C20 C21 -140.1(10) . . . . ? C8 C9 C20 C21A -141.1(3) . . . . ? C9 C10 C11 N2 159.64(16) . . . . ? C9 C10 C11 C12 -14.9(2) . . . . ? C9 C10 C13 O3 -89.7(2) . . . . ? C9 C10 C13 C14 88.8(3) . . . . ? C9 C20 C21 C22 -164.1(11) . . . . ? C9 C20 C21 C26 4.2(15) . . . . ? C9 C20 C21A C26A -7.8(4) . . . . ? C9 C20 C21A C22A 168.3(3) . . . . ? C10 C9 C20 O5 -84.6(2) . . . . ? C10 C9 C20 C21 97.2(10) . . . . ? C10 C9 C20 C21A 96.2(3) . . . . ? C10 C11 C12 N1 -9.7(3) . . . . ? C10 C13 C14 C15 -177.7(2) . . . . ? C11 C10 C13 O3 147.91(17) . . . . ? C11 C10 C13 C14 -33.6(3) . . . . ? C12 N1 C7 C5 -159.94(18) . . . . ? C12 N1 C8 C6 161.62(16) . . . . ? C12 N1 C8 C9 37.5(2) . . . . ? C13 O3 C16 C15 0.1(2) . . . . ? C13 O3 C16 C17 -178.7(2) . . . . ? C13 C10 C11 N2 -74.6(2) . . . . ? C13 C10 C11 C12 110.9(2) . . . . ? C13 C14 C15 C16 -0.8(3) . . . . ? C13 C14 C15 C18 177.1(2) . . . . ? C14 C15 C16 O3 0.4(3) . . . . ? C14 C15 C16 C17 178.8(3) . . . . ? C14 C15 C18 O4 -0.8(4) . . . . ? C14 C15 C18 C19 -178.6(3) . . . . ? C16 O3 C13 C10 178.25(17) . . . . ? C16 O3 C13 C14 -0.6(2) . . . . ? C16 C15 C18 O4 176.6(3) . . . . ? C16 C15 C18 C19 -1.2(4) . . . . ? C18 C15 C16 O3 -177.3(2) . . . . ? C18 C15 C16 C17 1.1(5) . . . . ? C20 C9 C10 C11 172.30(15) . . . . ? C20 C9 C10 C13 48.1(2) . . . . ? C20 C21 C22 C23 174.6(13) . . . . ? C20 C21 C26 C25 -168.7(19) . . . . ? C20 C21A C26A C25A 176.0(5) . . . . ? C20 C21A C22A C23A -176.3(5) . . . . ? C21 C22 C23 C24 -7(2) . . . . ? C21A C26A C25A C24A 0.0 . . . . ? C26A C21A C22A C23A 0.0 . . . . ? C26A C25A C24A C23A 0.0 . . . . ? C25A C24A C23A C22A 0.0 . . . . ? C24A C23A C22A C21A 0.0 . . . . ? C22A C21A C26A C25A 0.0 . . . . ? C22 C21 C26 C25 -0.2(18) . . . . ? C22 C23 C24 C25 4(3) . . . . ? C23 C24 C25 C26 1(3) . . . . ? C24 C25 C26 C21 -3(2) . . . . ? C26 C21 C22 C23 5.0(19) . . . . ? O1' N2' C11' C10' -177.51(18) . . . . ? O1' N2' C11' C12' 7.5(3) . . . . ? O2' N2' C11' C10' 2.3(3) . . . . ? O2' N2' C11' C12' -172.66(19) . . . . ? O3' C13' C14' C15' 0.9(3) . . . . ? O5' C20' C21' C22' -20.0(3) . . . . ? O5' C20' C21' C26' 160.3(2) . . . . ? N1' C8' C9' C10' 57.6(2) . . . . ? N1' C8' C9' C20' 177.51(15) . . . . ? N2' C11' C12' N1' -177.97(18) . . . . ? C1' C2' C3' C4' 0.5(5) . . . . ? C1' C6' C8' N1' 179.0(2) . . . . ? C1' C6' C8' C9' 59.7(3) . . . . ? C2' C1' C6' C5' -1.0(4) . . . . ? C2' C1' C6' C8' 173.3(2) . . . . ? C2' C3' C4' C5' -0.6(4) . . . . ? C3' C4' C5' C6' -0.1(4) . . . . ? C3' C4' C5' C7' -175.7(2) . . . . ? C4' C5' C6' C1' 1.0(3) . . . . ? C4' C5' C6' C8' -174.3(2) . . . . ? C4' C5' C7' N1' 179.5(2) . . . . ? C5' C6' C8' N1' -6.3(2) . . . . ? C5' C6' C8' C9' -125.61(19) . . . . ? C6' C1' C2' C3' 0.3(5) . . . . ? C6' C5' C7' N1' 3.6(3) . . . . ? C6' C8' C9' C10' 173.04(16) . . . . ? C6' C8' C9' C20' -67.0(2) . . . . ? C7' N1' C8' C6' 8.9(2) . . . . ? C7' N1' C8' C9' 136.13(19) . . . . ? C7' N1' C12' C11' -168.7(2) . . . . ? C7' C5' C6' C1' 177.2(2) . . . . ? C7' C5' C6' C8' 1.9(3) . . . . ? C8' N1' C7' C5' -8.0(2) . . . . ? C8' N1' C12' C11' 5.5(3) . . . . ? C8' C9' C10' C11' -46.0(2) . . . . ? C8' C9' C10' C13' 78.3(2) . . . . ? C8' C9' C20' O5' -18.4(3) . . . . ? C8' C9' C20' C21' 164.68(17) . . . . ? C9' C10' C11' N2' -160.39(16) . . . . ? C9' C10' C11' C12' 14.3(3) . . . . ? C9' C10' C13' O3' 91.5(2) . . . . ? C9' C10' C13' C14' -80.6(3) . . . . ? C9' C20' C21' C22' 156.90(19) . . . . ? C9' C20' C21' C26' -22.8(3) . . . . ? C10' C9' C20' O5' 102.6(2) . . . . ? C10' C9' C20' C21' -74.3(2) . . . . ? C10' C11' C12' N1' 7.3(3) . . . . ? C10' C13' C14' C15' 173.4(2) . . . . ? C11' C10' C13' O3' -146.21(19) . . . . ? C11' C10' C13' C14' 41.6(3) . . . . ? C12' N1' C7' C5' 166.49(19) . . . . ? C12' N1' C8' C6' -165.80(18) . . . . ? C12' N1' C8' C9' -38.6(2) . . . . ? C13' O3' C16' C15' -0.7(3) . . . . ? C13' O3' C16' C17' 177.9(3) . . . . ? C13' C10' C11' N2' 75.7(2) . . . . ? C13' C10' C11' C12' -109.6(2) . . . . ? C13' C14' C15' C16' -1.3(3) . . . . ? C13' C14' C15' C18' -178.3(2) . . . . ? C14' C15' C16' O3' 1.2(3) . . . . ? C14' C15' C16' C17' -177.0(4) . . . . ? C14' C15' C18' O4' -177.6(3) . . . . ? C14' C15' C18' C19' 2.7(4) . . . . ? C16' O3' C13' C10' -174.3(2) . . . . ? C16' O3' C13' C14' -0.2(3) . . . . ? C16' C15' C18' O4' 5.9(4) . . . . ? C16' C15' C18' C19' -173.8(3) . . . . ? C18' C15' C16' O3' 178.4(2) . . . . ? C18' C15' C16' C17' 0.1(6) . . . . ? C20' C9' C10' C11' -168.15(16) . . . . ? C20' C9' C10' C13' -43.9(2) . . . . ? C20' C21' C22' C23' -179.4(2) . . . . ? C20' C21' C26' C25' -179.7(2) . . . . ? C21' C22' C23' C24' -0.7(4) . . . . ? C22' C21' C26' C25' 0.6(3) . . . . ? C22' C23' C24' C25' 0.2(4) . . . . ? C23' C24' C25' C26' 0.7(4) . . . . ? C24' C25' C26' C21' -1.1(4) . . . . ? C26' C21' C22' C23' 0.3(4) . . . . ? _shelx_res_file ; wll149_sq.res created by SHELXL-2014/7 TITL CF solution in P-1 CELL 1.54184 11.555433 11.9041 20.621576 81.9998 89.7919 61.5825 ZERR 4 0.000388 0.000407 0.000649 0.0027 0.0026 0.0035 LATT 1 SFAC C H N O UNIT 104 88 8 20 EADP C22 C22A EADP C23 C23A EADP C24 C24A EADP C25 C25A EADP C26 C26A EADP C21 C21A L.S. 5 0 46 PLAN 20 SIZE 0.16 0.13 0.09 MPLA C1 C2 C3 C4 C5 C6 C7 N1 MPLA C13 C14 C15 C16 O3 MPLA C21 C22 C23 C24 C25 C26 BOND $h ABIN conf fmap 2 acta REM REM REM WGHT 0.085200 0.307900 FVAR 4.62382 0.26787 O1 4 0.678976 0.322211 0.047453 11.00000 0.06222 0.06111 = 0.05763 -0.01952 0.01723 -0.01839 O2 4 0.686042 0.493251 0.066854 11.00000 0.06367 0.09062 = 0.07740 -0.02596 0.01974 -0.04713 O3 4 0.514182 0.696782 0.194498 11.00000 0.07056 0.05794 = 0.05215 -0.01557 0.00993 -0.04115 O4 4 0.650176 0.368429 0.364415 11.00000 0.11146 0.10386 = 0.07030 0.01060 -0.02502 -0.07134 O5 4 0.216840 0.772846 0.203038 11.00000 0.09581 0.05630 = 0.04148 -0.01368 0.01584 -0.03656 N1 3 0.312166 0.452442 0.104418 11.00000 0.04965 0.03606 = 0.04567 -0.00607 0.00098 -0.01998 N2 3 0.627830 0.428867 0.066947 11.00000 0.05379 0.06062 = 0.04020 -0.01057 0.00627 -0.02460 C1 1 0.003891 0.689454 0.163627 11.00000 0.05790 0.05505 = 0.06745 -0.01343 0.01242 -0.02829 AFIX 43 H1 2 0.015624 0.744508 0.187492 11.00000 -1.20000 AFIX 0 C2 1 -0.119530 0.700455 0.153889 11.00000 0.05384 0.06319 = 0.09958 -0.01455 0.01629 -0.02419 AFIX 43 H2 2 -0.191404 0.764516 0.170952 11.00000 -1.20000 AFIX 0 C3 1 -0.138515 0.618480 0.119400 11.00000 0.05232 0.06594 = 0.08778 0.00078 -0.00288 -0.02945 AFIX 43 H3 2 -0.222568 0.627951 0.113236 11.00000 -1.20000 AFIX 0 C4 1 -0.032761 0.522398 0.094041 11.00000 0.06105 0.05806 = 0.06420 0.00109 -0.00796 -0.03368 AFIX 43 H4 2 -0.044372 0.466200 0.071033 11.00000 -1.20000 AFIX 0 C5 1 0.090661 0.511517 0.103568 11.00000 0.05288 0.04405 = 0.04803 0.00080 -0.00188 -0.02516 C6 1 0.109752 0.594923 0.137185 11.00000 0.05150 0.04080 = 0.04141 0.00093 0.00185 -0.02201 C7 1 0.219798 0.409857 0.084444 11.00000 0.05969 0.04838 = 0.06572 -0.01438 0.00181 -0.02890 AFIX 23 H7A 2 0.242041 0.324736 0.107724 11.00000 -1.20000 H7B 2 0.218010 0.408372 0.037556 11.00000 -1.20000 AFIX 0 C8 1 0.252864 0.561397 0.142027 11.00000 0.04810 0.03729 = 0.03616 -0.00435 0.00168 -0.02035 AFIX 13 H8 2 0.288141 0.531482 0.187946 11.00000 -1.20000 AFIX 0 C9 1 0.289171 0.664619 0.110923 11.00000 0.05264 0.03765 = 0.03460 -0.00503 0.00360 -0.02201 AFIX 13 H9 2 0.256180 0.690038 0.064637 11.00000 -1.20000 AFIX 0 C10 1 0.442887 0.606349 0.114114 11.00000 0.05414 0.04677 = 0.03895 -0.00663 0.00803 -0.02902 AFIX 13 H10 2 0.463375 0.664913 0.084131 11.00000 -1.20000 AFIX 0 C11 1 0.500024 0.479422 0.088967 11.00000 0.04877 0.04589 = 0.03661 -0.00778 0.00595 -0.02145 C12 1 0.429759 0.416499 0.081599 11.00000 0.05240 0.03637 = 0.03859 -0.00606 0.00029 -0.01609 AFIX 43 H12 2 0.465929 0.345393 0.059637 11.00000 -1.20000 AFIX 0 C13 1 0.503843 0.591286 0.181110 11.00000 0.05090 0.05372 = 0.04882 -0.01705 0.01012 -0.03129 C14 1 0.549982 0.498643 0.233091 11.00000 0.05375 0.05531 = 0.04909 -0.01090 0.00278 -0.02968 AFIX 43 H14 2 0.554833 0.417805 0.236164 11.00000 -1.20000 AFIX 0 C15 1 0.591274 0.546869 0.284025 11.00000 0.04980 0.07047 = 0.04868 -0.01761 0.00744 -0.03280 C16 1 0.567668 0.667751 0.257595 11.00000 0.06087 0.07530 = 0.05138 -0.02426 0.01342 -0.04368 C17 1 0.581884 0.775673 0.279557 11.00000 0.12172 0.09840 = 0.07577 -0.03600 0.01794 -0.07840 AFIX 137 H17A 2 0.673324 0.747120 0.290517 11.00000 -1.50000 H17B 2 0.532808 0.800797 0.317436 11.00000 -1.50000 H17C 2 0.548626 0.848233 0.244785 11.00000 -1.50000 AFIX 0 C18 1 0.642321 0.473711 0.350178 11.00000 0.05876 0.08972 = 0.05328 -0.01180 -0.00045 -0.04389 C19 1 0.680110 0.532712 0.400684 11.00000 0.10816 0.12621 = 0.06691 -0.01737 -0.01482 -0.06868 AFIX 137 H19A 2 0.695674 0.480727 0.442998 11.00000 -1.50000 H19B 2 0.609876 0.618496 0.402092 11.00000 -1.50000 H19C 2 0.758871 0.536526 0.389160 11.00000 -1.50000 AFIX 0 C20 1 0.225078 0.784731 0.144276 11.00000 0.05197 0.04578 = 0.04128 -0.01173 0.00995 -0.02751 PART 1 C21 1 0.173641 0.906149 0.107392 21.00000 0.05353 0.03737 = 0.04968 -0.00898 0.00849 -0.02188 PART 0 PART 2 AFIX 66 C21A 1 0.170866 0.918249 0.102281 -21.00000 0.05353 0.03737 = 0.04968 -0.00898 0.00849 -0.02188 C26A 1 0.190668 0.935844 0.035927 -21.00000 0.08514 0.04447 = 0.04824 -0.00879 0.01194 -0.03158 AFIX 43 H26A 2 0.243323 0.864841 0.015723 -21.00000 -1.20000 AFIX 65 C25A 1 0.131773 1.059559 -0.000229 -21.00000 0.14493 0.05686 = 0.04505 0.00173 -0.00199 -0.04228 AFIX 43 H25A 2 0.145023 1.071331 -0.044624 -21.00000 -1.20000 AFIX 65 C24A 1 0.053074 1.165682 0.029967 -21.00000 0.11322 0.04098 = 0.07418 0.00936 -0.02475 -0.01803 AFIX 43 H24A 2 0.013669 1.248456 0.005776 -21.00000 -1.20000 AFIX 65 C23A 1 0.033270 1.148089 0.096321 -21.00000 0.09971 0.03816 = 0.09191 -0.01578 0.00822 0.00288 AFIX 43 H23A 2 -0.019385 1.219093 0.116524 -21.00000 -1.20000 AFIX 65 C22A 1 0.092165 1.024374 0.132478 -21.00000 0.07181 0.04831 = 0.05925 -0.01221 0.01061 -0.01348 AFIX 43 H22A 2 0.078914 1.012604 0.176873 -21.00000 -1.20000 AFIX 0 PART 0 PART 1 C22 1 0.146471 1.011881 0.140997 21.00000 0.07181 0.04831 = 0.05925 -0.01221 0.01061 -0.01348 AFIX 43 H22 2 0.156513 0.998797 0.186600 21.00000 -1.20000 AFIX 0 C23 1 0.104704 1.135395 0.105543 21.00000 0.09971 0.03816 = 0.09191 -0.01578 0.00822 0.00288 AFIX 43 H23 2 0.077710 1.205414 0.127977 21.00000 -1.20000 AFIX 0 C24 1 0.102885 1.154314 0.041388 21.00000 0.11322 0.04098 = 0.07418 0.00936 -0.02475 -0.01803 AFIX 43 H24 2 0.080050 1.236007 0.018653 21.00000 -1.20000 AFIX 0 C25 1 0.133512 1.057159 0.009521 21.00000 0.14493 0.05686 = 0.04505 0.00173 -0.00199 -0.04228 AFIX 43 H25 2 0.133423 1.071774 -0.035975 21.00000 -1.20000 AFIX 0 C26 1 0.166123 0.933365 0.040298 21.00000 0.08514 0.04447 = 0.04824 -0.00879 0.01194 -0.03158 AFIX 43 H26 2 0.182922 0.868696 0.015248 21.00000 -1.20000 AFIX 0 PART 0 O1' 4 0.529260 0.115785 0.574198 11.00000 0.09606 0.07213 = 0.03876 -0.00520 -0.00056 -0.04189 O2' 4 0.320623 0.201644 0.544541 11.00000 0.08649 0.08439 = 0.05899 -0.01985 0.02713 -0.04537 O3' 4 0.143176 0.424744 0.391474 11.00000 0.04867 0.04990 = 0.10183 -0.01718 0.01207 -0.02559 O4' 4 0.071221 0.810010 0.366008 11.00000 0.06209 0.04311 = 0.11934 -0.00732 0.00028 -0.01319 O5' 4 0.297457 0.341749 0.255618 11.00000 0.05806 0.05573 = 0.06568 0.02089 -0.00711 -0.02901 N1' 3 0.625647 0.107497 0.388453 11.00000 0.05040 0.04620 = 0.04025 -0.00452 -0.00211 -0.01891 N2' 3 0.436625 0.160231 0.530643 11.00000 0.08119 0.04674 = 0.04320 -0.00854 0.01059 -0.03482 C1' 1 0.564912 0.160043 0.208949 11.00000 0.06463 0.05985 = 0.04266 0.00158 -0.00265 -0.01279 AFIX 43 H1' 2 0.477245 0.216296 0.194446 11.00000 -1.20000 AFIX 0 C2' 1 0.659068 0.105342 0.164172 11.00000 0.08812 0.07093 = 0.03988 -0.00451 0.00444 -0.02056 AFIX 43 H2' 2 0.633615 0.125882 0.119523 11.00000 -1.20000 AFIX 0 C3' 1 0.787986 0.022136 0.184826 11.00000 0.07463 0.06068 = 0.05157 -0.01842 0.01738 -0.02272 AFIX 43 H3' 2 0.849384 -0.012740 0.154167 11.00000 -1.20000 AFIX 0 C4' 1 0.827978 -0.010700 0.251107 11.00000 0.05532 0.05591 = 0.05877 -0.01558 0.00477 -0.01774 AFIX 43 H4' 2 0.915528 -0.067988 0.265389 11.00000 -1.20000 AFIX 0 C5' 1 0.734726 0.043651 0.295642 11.00000 0.05182 0.04592 = 0.04758 -0.00923 0.00074 -0.02092 C6' 1 0.603898 0.129354 0.275307 11.00000 0.05412 0.04143 = 0.04208 -0.00249 0.00229 -0.02166 C7' 1 0.758255 0.028288 0.368349 11.00000 0.04835 0.07574 = 0.04997 -0.01269 -0.00157 -0.01959 AFIX 23 H7'A 2 0.794263 -0.061405 0.388515 11.00000 -1.20000 H7'B 2 0.817604 0.060238 0.379440 11.00000 -1.20000 AFIX 0 C8' 1 0.526064 0.184369 0.332768 11.00000 0.05181 0.03650 = 0.04056 -0.00206 -0.00023 -0.01942 AFIX 13 H8' 2 0.505068 0.275103 0.329477 11.00000 -1.20000 AFIX 0 C9' 1 0.401249 0.174307 0.346551 11.00000 0.05311 0.03539 = 0.04099 0.00043 -0.00075 -0.02140 AFIX 13 H9' 2 0.421824 0.083706 0.349738 11.00000 -1.20000 AFIX 0 C10' 1 0.349183 0.223101 0.413625 11.00000 0.05542 0.04275 = 0.04647 -0.00454 0.00693 -0.02703 AFIX 13 H10' 2 0.287203 0.191837 0.427961 11.00000 -1.20000 AFIX 0 C11' 1 0.463335 0.164169 0.464051 11.00000 0.06530 0.04052 = 0.03738 -0.00282 0.00405 -0.02641 C12' 1 0.591610 0.105366 0.449057 11.00000 0.06040 0.04135 = 0.03842 -0.00333 -0.00539 -0.02225 AFIX 43 H12' 2 0.657387 0.062161 0.483043 11.00000 -1.20000 AFIX 0 C13' 1 0.277254 0.368079 0.405926 11.00000 0.04431 0.04525 = 0.05343 -0.00697 0.00831 -0.01938 C14' 1 0.312378 0.460359 0.403435 11.00000 0.04331 0.04496 = 0.06460 -0.00988 0.00601 -0.02016 AFIX 43 H14' 2 0.397352 0.447947 0.410638 11.00000 -1.20000 AFIX 0 C15' 1 0.193964 0.582779 0.387498 11.00000 0.04586 0.04298 = 0.06762 -0.01108 0.00871 -0.01762 C16' 1 0.094883 0.555531 0.379976 11.00000 0.04816 0.04758 = 0.09861 -0.01583 0.01059 -0.01772 C17' 1 -0.049175 0.634604 0.361023 11.00000 0.04651 0.07058 = 0.18901 -0.02823 0.00215 -0.02052 AFIX 137 H17D 2 -0.076042 0.590501 0.333953 11.00000 -1.50000 H17E 2 -0.067122 0.717014 0.337070 11.00000 -1.50000 H17F 2 -0.097161 0.647237 0.399835 11.00000 -1.50000 AFIX 0 C18' 1 0.178410 0.714424 0.377273 11.00000 0.05480 0.04647 = 0.08054 -0.01065 0.00890 -0.02008 C19' 1 0.300185 0.726585 0.380940 11.00000 0.06693 0.05608 = 0.19023 -0.02104 0.02153 -0.03323 AFIX 137 H19D 2 0.277329 0.816358 0.372984 11.00000 -1.50000 H19E 2 0.357157 0.682884 0.348423 11.00000 -1.50000 H19F 2 0.344807 0.688374 0.423785 11.00000 -1.50000 AFIX 0 C20' 1 0.291581 0.255919 0.292660 11.00000 0.05235 0.03909 = 0.04311 0.00045 0.00205 -0.01988 C21' 1 0.174891 0.234992 0.287543 11.00000 0.05511 0.04755 = 0.03917 -0.00311 0.00223 -0.02540 C22' 1 0.059239 0.336906 0.255624 11.00000 0.05614 0.05506 = 0.05871 0.00151 0.00054 -0.02760 AFIX 43 H22' 2 0.057480 0.414107 0.238154 11.00000 -1.20000 AFIX 0 C23' 1 -0.052508 0.324744 0.249621 11.00000 0.05430 0.07060 = 0.07262 -0.00001 -0.00127 -0.02820 AFIX 43 H23' 2 -0.129711 0.393733 0.228580 11.00000 -1.20000 AFIX 0 C24' 1 -0.049868 0.209439 0.274996 11.00000 0.06794 0.08694 = 0.07534 -0.01233 0.00660 -0.04990 AFIX 43 H24' 2 -0.125375 0.201008 0.270861 11.00000 -1.20000 AFIX 0 C25' 1 0.063499 0.107932 0.306122 11.00000 0.08242 0.06630 = 0.07189 -0.00231 0.00011 -0.04955 AFIX 43 H25' 2 0.064898 0.030474 0.322637 11.00000 -1.20000 AFIX 0 C26' 1 0.176510 0.119773 0.313226 11.00000 0.06790 0.05158 = 0.05898 -0.00024 -0.00242 -0.03248 AFIX 43 H26' 2 0.252924 0.050987 0.335054 11.00000 -1.20000 AFIX 0 HKLF 4 REM CF solution in P-1 REM R1 = 0.0505 for 6803 Fo > 4sig(Fo) and 0.0650 for all 8791 data REM 606 parameters refined using 0 restraints END WGHT 0.0852 0.3079 REM Highest difference peak 0.315, deepest hole -0.236, 1-sigma level 0.039 Q1 1 -0.0409 0.6255 0.4211 11.00000 0.05 0.32 Q2 1 0.1501 0.4127 0.4382 11.00000 0.05 0.23 Q3 1 0.1089 0.5475 0.4234 11.00000 0.05 0.22 Q4 1 0.6146 0.8212 0.2439 11.00000 0.05 0.19 Q5 1 0.2638 0.6234 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1 -6 7 195.856 71.4041 28 1 -6 8 1191.44 142.937 28 1 -6 9 5083.33 297.321 28 1 -6 10 11121.4 436.076 31 1 -6 10 11458.5 437.210 28 1 -6 11 5485.88 312.799 31 1 -6 11 4998.25 291.683 28 1 -6 12 1351.88 162.952 31 1 -6 12 1353.06 154.816 28 1 -6 13 867.932 131.602 31 1 -6 13 583.903 110.111 35 1 -6 13 832.325 123.208 28 1 -6 14 1033.57 128.152 28 1 -6 14 1147.50 145.816 31 1 -6 14 984.433 145.019 35 1 -6 15-1.14912 55.0269 35 1 -6 15 49.2928 52.6831 31 1 -6 16 1275.15 150.788 35 1 -6 17 855.720 115.679 35 1 -6 18 191.116 59.8967 35 -1 5 23 9.31001 44.4338 33 -1 5 23 57.7058 38.0610 26 -1 5 22 13.7898 44.8213 33 -1 5 22 24.7515 41.4097 26 -1 5 21 1706.62 170.366 33 -1 5 21 1736.03 160.971 26 -1 5 20 207.676 74.8346 33 -1 5 19 4143.90 278.396 33 -1 5 18 106.256 58.1408 33 -1 5 17 631.641 112.108 25 -1 5 16 1238.87 148.989 25 -1 5 15 1449.98 157.241 25 -1 5 15 1285.49 158.949 21 -1 5 14 2624.83 206.246 25 -1 5 14 2250.00 198.209 21 -1 5 13 231.751 75.6573 25 -1 5 13 143.080 61.8239 21 1 -5 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18 1 -5 1 18202.2 891.434 7 1 -5 2 8828.54 692.030 18 -1 5 -2 9536.12 745.205 9 1 -5 2 9736.25 666.076 7 1 -5 3 22727.2 1096.82 18 1 -5 3 20974.8 1137.58 16 -1 5 -3 21416.2 1123.72 9 1 -5 4 47.3082 93.8316 18 1 -5 4 179.111 126.150 16 -1 5 -5 38.7977 145.372 9 1 -5 5-61.3148 83.2476 18 1 -5 5 43.1748 88.0002 16 1 -5 5 131.527 97.1525 10 1 -5 6 15770.5 1018.74 16 1 -5 6 17058.1 946.821 10 -1 5 -6 15609.0 1058.21 9 1 -5 7 11145.2 874.904 16 -1 5 -7 10039.5 876.510 9 1 -5 7 9750.23 739.830 10 1 -5 8-140.023 97.7644 10 1 -5 8 207.065 140.110 16 -1 5 -8 104.559 112.900 9 1 -5 9 306.920 149.899 10 -1 5 -9 344.688 166.932 9 1 -5 10 1067.24 137.123 31 1 -5 10 655.316 106.364 28 1 -5 11 795.356 119.797 28 1 -5 11 944.927 134.143 31 1 -5 12 154.276 61.3285 28 1 -5 12 79.4345 47.2253 31 1 -5 13 2602.65 225.742 31 1 -5 13 2430.83 220.791 35 1 -5 13 2803.13 214.930 28 1 -5 14 1640.47 183.069 31 1 -5 14 1432.01 170.582 35 1 -5 15 1108.79 152.789 35 1 -5 15 1085.78 152.312 31 1 -5 16 1034.21 143.950 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33950.7 1294.48 9 1 -4 4 32976.5 1204.93 18 1 -4 5 6100.36 522.306 18 1 -4 5 6568.31 586.890 16 -1 4 -5 6081.29 733.362 4 -1 4 -5 6307.42 578.522 9 1 -4 5 6334.16 507.869 10 1 -4 6 23566.7 1019.04 10 1 -4 6 22737.7 1092.88 16 -1 4 -6 22703.9 1125.13 9 -1 4 -6 21546.0 1344.33 4 -1 4 -7 1610.35 386.120 4 1 -4 7 1969.73 310.327 10 -1 4 -7 2323.39 376.685 9 1 -4 7 1757.62 326.718 16 -1 4 -8 9346.42 777.579 9 1 -4 8 8602.38 720.586 16 -1 4 -8 7546.72 841.527 4 1 -4 8 7640.30 632.459 10 -1 4 -9 2865.43 440.813 9 -1 4 -9 2395.95 489.086 4 1 -4 9 3268.37 435.562 10 1 -4 10 1800.37 349.576 10 -1 4 -10 1048.89 281.416 9 1 -4 10 1496.54 319.487 15 -1 4 -10 1709.34 454.966 4 -1 4 -11 4434.59 711.260 4 1 -4 11 4909.22 588.022 15 1 -4 12 741.978 121.205 31 1 -4 12 829.048 113.698 28 1 -4 13 4250.74 264.468 24 1 -4 13 4385.76 289.685 31 1 -4 13 4347.25 285.926 35 1 -4 14 1414.13 169.388 35 1 -4 14 1381.84 155.558 24 1 -4 14 1280.53 163.666 31 1 -4 15 4490.77 278.502 24 1 -4 15 4136.89 284.206 31 1 -4 15 3988.96 278.928 35 1 -4 16 6457.58 354.131 31 1 -4 16 6692.29 332.231 24 1 -4 16 6512.52 353.104 35 1 -4 17 752.899 128.847 35 1 -4 17 1056.97 151.710 31 1 -4 17 1034.48 135.319 24 1 -4 18 43.1890 61.8160 31 1 -4 18 27.2952 56.1045 35 1 -4 19-3.83324 65.5146 35 1 -4 19 59.1761 61.9514 31 1 -4 20-34.4694 58.3128 35 1 -4 21 22.4679 45.4283 35 1 -4 21-77.0399 62.3472 20 -1 3 24 47.9052 41.2854 33 -1 3 23 385.765 80.9732 33 -1 3 22 272.384 84.4416 33 -1 3 22 385.710 82.7654 35 -1 3 21 15.7640 54.1375 33 -1 3 21 120.020 66.0426 35 -1 3 20 20.8440 56.4602 35 -1 3 20-32.3897 68.9783 33 -1 3 19 883.561 135.182 35 -1 3 19 786.812 129.955 33 -1 3 18 1616.39 179.885 33 -1 3 18 1576.38 180.446 35 -1 3 18 1641.52 190.054 20 -1 3 17 4348.33 285.230 35 -1 3 17 4276.16 290.228 33 -1 3 17 4565.32 297.094 20 -1 3 16 4961.77 295.717 35 -1 3 16 4887.24 301.734 20 -1 3 16 5254.42 298.908 21 -1 3 15 12164.3 439.799 21 -1 3 14 299.434 161.144 14 -1 3 13 1251.30 298.942 14 1 -3 -13 642.254 258.511 11 1 -3 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21679.8 738.874 7 1 -3 1 23514.5 536.720 8 1 -3 1 22870.2 844.183 18 1 -3 1 24166.8 557.737 12 1 -3 2 1449.00 201.981 7 -1 3 -2 957.728 178.687 9 1 -3 2 1547.58 233.319 18 -1 3 -2 1178.80 290.854 4 -1 3 -3 18367.1 814.499 9 -1 3 -3 18557.7 1019.29 4 1 -3 3 18671.3 823.429 16 1 -3 3 20182.4 815.411 18 1 -3 4 487.690 160.248 18 -1 3 -4 378.296 134.071 9 -1 3 -4 574.574 236.162 4 1 -3 4 602.986 181.036 16 -1 3 -5 14429.6 768.755 9 1 -3 5 14922.2 776.221 16 1 -3 5 15583.8 738.872 18 -1 3 -5 13979.9 899.561 4 1 -3 5 14427.7 686.270 10 -1 3 -6 5121.56 480.595 9 1 -3 6 5025.60 469.596 16 -1 3 -6 4767.21 538.497 4 1 -3 6 4623.31 416.003 10 1 -3 7 6272.82 509.739 10 -1 3 -7 5809.97 534.423 9 1 -3 7 5664.15 513.471 16 -1 3 -7 6160.19 632.780 4 -1 3 -8 9421.80 812.195 4 1 -3 8 11007.7 703.613 10 -1 3 -8 10079.1 720.071 9 -1 3 -9 471.289 228.682 4 1 -3 9 863.547 211.864 10 -1 3 -9 987.180 237.469 9 1 -3 10 6514.30 621.532 15 -1 3 -10 7270.68 772.194 4 -1 3 -10 6729.09 632.529 9 1 -3 10 7349.06 645.403 10 1 -3 11 1152.68 269.440 15 -1 3 -11 1375.44 364.028 4 1 -3 12 9335.18 804.809 15 -1 3 -12 12822.5 1122.84 4 1 -3 13 2601.86 216.136 31 1 -3 13 2619.85 216.105 35 1 -3 14-21.4692 59.1365 35 1 -3 14-66.5731 69.5872 31 1 -3 14-50.8668 55.1201 24 1 -3 15 8613.42 409.025 35 1 -3 15 8477.27 408.275 31 1 -3 15 8933.54 391.528 24 1 -3 16 10909.3 458.848 35 1 -3 16 10528.0 428.448 24 1 -3 16 10010.4 443.774 31 1 -3 17 1976.73 190.424 24 1 -3 17 2003.87 202.317 35 1 -3 17 1999.19 201.003 31 1 -3 18 1155.47 159.153 35 1 -3 18 813.188 134.237 31 1 -3 19 109.368 72.0644 31 1 -3 19 124.738 63.9752 35 1 -3 20-113.769 82.9892 35 1 -3 20 29.7111 49.8973 31 1 -3 21 41.0643 52.2422 35 1 -3 22 514.681 83.5147 35 1 -3 22 505.277 79.6272 20 -1 2 24 30.2123 46.4503 33 -1 2 23 303.997 75.7243 35 -1 2 23 120.873 63.0273 33 -1 2 22 22.9530 54.0243 33 -1 2 22-47.8632 54.4582 35 -1 2 21 791.135 129.152 35 -1 2 21 664.593 119.818 33 -1 2 21 624.727 122.778 20 -1 2 20 19.5976 61.0609 33 -1 2 20-23.4426 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36.5699 26 -2 4 22 4226.82 216.895 26 -2 4 22 4327.93 251.474 33 -2 4 21 335.130 80.4023 26 -2 4 21 276.977 81.7381 33 -2 4 20 49.4723 56.4725 33 -2 4 20 63.5337 68.5881 26 -2 4 19 664.414 123.368 33 -2 4 18 3507.17 260.638 33 -2 4 17-60.5179 63.5834 33 -2 4 16 292.445 91.8328 33 -2 4 16 259.962 78.5701 25 -2 4 15 2382.94 195.814 25 -2 4 15 2375.24 209.923 33 -2 4 14 4034.37 247.051 25 -2 4 13 1839.10 397.741 14 2 -4 -12-37.3370 101.824 13 -2 4 12 403.230 189.929 3 -2 4 11 2410.01 430.329 3 -2 4 11 3366.15 464.186 14 2 -4 -11 3041.76 548.748 13 -2 4 10 1141.57 264.787 14 2 -4 -10 1400.33 382.276 13 -2 4 10 1016.29 275.021 3 -2 4 9 340.178 162.414 14 -2 4 9 81.6532 89.8599 3 2 -4 -9-3.78016 110.288 13 -2 4 8 887.968 238.629 3 -2 4 8 1328.62 272.437 14 2 -4 -8 1088.06 259.025 18 2 -4 -8 641.877 265.945 13 2 -4 -8 1027.48 277.651 8 2 -4 -7 38890.2 1472.64 18 2 -4 -7 42882.1 1695.40 8 -2 4 7 40212.8 1317.35 14 -2 4 7 41422.7 1660.47 3 2 -4 -7 39167.4 1736.13 13 2 -4 -6 172.320 137.904 18 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571.442 236.851 4 -2 4 -6 847.477 247.929 9 2 -4 6 737.452 186.591 10 2 -4 7 2562.84 402.651 16 2 -4 7 3285.98 406.684 10 -2 4 -7 2647.20 441.101 9 -2 4 -7 2189.51 502.218 4 2 -4 8 19562.3 1027.74 10 -2 4 -8 16474.8 1107.90 9 -2 4 -8 16573.1 1370.03 4 -2 4 -9 614.883 291.907 4 -2 4 -9-20.6135 91.3041 9 2 -4 10-57.4971 83.4934 15 -2 4 -10 178.261 138.713 9 2 -4 11 1261.38 143.713 28 2 -4 11 1956.43 187.674 31 2 -4 12 1447.82 165.715 35 2 -4 12 1532.62 162.221 28 2 -4 12 1434.01 164.992 31 2 -4 13 5750.27 328.939 35 2 -4 13 6439.71 325.184 28 2 -4 13 6014.40 338.322 31 2 -4 14 422.341 98.8559 35 2 -4 14 516.950 104.397 31 2 -4 14 432.795 95.0199 28 2 -4 15 1535.79 176.071 35 2 -4 15 1515.28 177.751 31 2 -4 16 2681.24 226.063 35 2 -4 16 2574.43 223.824 31 2 -4 17 97.7261 64.0898 31 2 -4 17 89.1259 71.5491 35 2 -4 18 6.82958 55.5218 35 2 -4 18 103.707 65.7561 31 2 -4 19 351.213 84.4894 31 2 -4 19 175.965 58.5285 35 2 -4 20 960.786 115.418 35 -2 3 24 152.904 51.6425 33 -2 3 23 42.4179 50.4456 33 -2 3 22 749.906 119.918 33 -2 3 21 6772.25 301.155 26 -2 3 21 6209.32 329.783 33 -2 3 20 1294.21 162.717 33 -2 3 20 1206.22 140.172 26 -2 3 19 294.722 90.3319 33 -2 3 18 38.9182 62.2754 33 -2 3 17 378.283 97.0975 33 -2 3 16 4840.16 301.023 33 -2 3 15 5624.48 319.005 33 2 -3 -14 41.6813 116.215 13 -2 3 14 196.848 153.438 14 2 -3 -13 1447.38 385.465 13 -2 3 13 980.590 289.861 14 2 -3 -12 5042.99 676.154 13 -2 3 12 4957.29 567.461 14 -2 3 11 2323.31 380.299 3 2 -3 -11 2364.76 467.848 13 -2 3 11 2797.60 425.360 14 -2 3 10 55.3287 85.0911 14 -2 3 10-102.274 106.029 3 2 -3 -10 100.224 131.357 13 2 -3 -9 6494.04 685.754 13 2 -3 -9 7781.31 612.674 18 -2 3 9 8207.61 644.665 14 -2 3 9 8184.47 683.237 3 -2 3 8 4113.37 434.381 14 2 -3 -8 3756.08 421.623 18 2 -3 -8 3659.31 506.737 13 -2 3 8 4715.58 514.513 3 2 -3 -7 8454.88 732.556 13 -2 3 7 9009.55 696.777 3 2 -3 -7 8915.95 630.404 18 -2 3 7 8654.06 601.155 14 2 -3 -6 17779.4 976.728 8 2 -3 -6 18457.3 886.636 18 2 -3 -6 15303.9 948.952 13 -2 3 6 18640.7 834.455 14 2 -3 -5 1675.25 268.490 18 2 -3 -5 1578.54 316.372 13 -2 3 5 1373.25 227.381 14 2 -3 -5 1491.56 284.935 8 2 -3 -4 10746.8 654.517 18 2 -3 -4 10290.5 701.843 8 -2 3 4 11389.4 554.686 9 2 -3 -4 10903.9 790.617 13 2 -3 -3 638.103 209.835 8 -2 3 3 466.855 131.921 9 2 -3 -3 519.350 163.361 18 2 -3 -3 432.543 173.677 13 -2 3 2 24109.7 858.684 9 2 -3 -2 23576.7 985.099 5 2 -3 -2 23959.5 960.209 18 2 -3 -2 24065.2 1015.77 8 2 -3 -2 21986.8 756.871 7 2 -3 -1 34798.1 922.801 7 -2 3 1 34977.8 1052.68 9 2 -3 -1 34686.4 1144.88 18 2 -3 -1 34906.1 997.257 5 -2 3 0-50.1927 72.4803 9 2 -3 0 105.831 87.7750 18 2 -3 0-12.9120 63.2425 7 2 -3 1 1657.86 270.696 18 -2 3 -1 1582.30 261.201 9 2 -3 1 1541.73 203.208 7 2 -3 2 59.0016 87.2003 18 2 -3 3 23024.3 796.794 10 -2 3 -3 23125.8 1304.73 4 2 -3 3 24580.5 1005.19 18 2 -3 3 23660.7 995.135 16 -2 3 -3 25271.4 1022.80 9 2 -3 4 4353.69 363.760 10 2 -3 4 4924.41 457.916 18 2 -3 4 4823.81 459.700 16 -2 3 -4 4431.92 599.425 4 -2 3 -4 4959.17 480.237 9 -2 3 -5 21473.8 1278.45 4 2 -3 5 22129.5 866.381 10 -2 3 -5 23856.0 1091.34 9 2 -3 5 22114.1 999.010 16 2 -3 6 731.019 212.230 16 -2 3 -6 285.711 156.781 9 -2 3 -6 374.001 224.143 4 2 -3 6 328.868 121.416 10 2 -3 7 1744.31 275.342 10 2 -3 7 1633.06 295.543 16 -2 3 -7 1490.01 309.184 9 -2 3 -7 1248.12 329.002 4 -2 3 -8 129.586 159.333 4 -2 3 -8 708.941 217.216 9 2 -3 8 557.981 166.050 10 -2 3 -9 336.726 159.039 9 -2 3 -9 11.2482 139.155 4 2 -3 9 158.740 107.291 10 -2 3 -10 738.233 234.005 9 2 -3 10 525.471 181.903 15 -2 3 -10 399.750 234.914 4 -2 3 -11 236.559 150.081 9 -2 3 -11 712.251 289.425 4 2 -3 11 380.018 171.261 15 2 -3 12 120.289 63.4817 28 2 -3 12 14.2867 57.3431 31 2 -3 12 65.5155 50.2856 35 2 -3 13 387.806 96.4863 31 2 -3 13 325.739 85.6328 35 2 -3 13 395.662 90.1577 28 2 -3 14 6549.79 354.901 31 2 -3 14 5859.92 333.024 35 2 -3 15 1298.98 164.409 31 2 -3 15 1066.46 152.144 35 2 -3 16 6917.96 366.235 35 2 -3 16 7342.86 380.414 31 2 -3 17 811.721 134.757 31 2 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41998.7 1158.64 18 -2 2 6 42603.5 802.614 9 -2 2 6 39893.0 1266.38 3 -2 2 6 42265.1 1186.22 14 2 -2 -6 40668.6 1389.57 13 2 -2 -5 27168.0 1089.49 13 -2 2 5 27999.1 925.895 14 2 -2 -5 26783.9 904.886 18 2 -2 -4 18340.0 882.300 13 2 -2 -4 21735.1 911.359 8 -2 2 4 19329.6 740.204 14 2 -2 -4 18846.1 748.933 18 -2 2 4 21163.8 600.231 17 2 -2 -3 1049.63 220.292 8 2 -2 -3 788.159 164.920 18 2 -2 -3 657.879 192.136 13 -2 2 3 603.012 104.698 17 -2 2 2 75721.5 1268.05 9 2 -2 -2 80389.1 1797.56 13 2 -2 -1 3926.50 301.868 5 -2 2 1 3712.03 295.401 9 2 -2 -1 3392.37 233.723 7 2 -2 -1 3267.25 312.454 18 2 -2 0 6466.71 439.827 18 -2 2 0 7164.57 421.457 9 2 -2 0 6884.66 324.331 7 -2 2 -1 18994.4 711.241 9 2 -2 1 17972.8 737.959 18 2 -2 1 19297.6 638.188 12 -2 2 -2 2267.03 265.993 9 2 -2 2 2006.72 260.528 18 2 -2 3 25962.9 735.118 10 -2 2 -3 25439.7 903.904 9 2 -2 3 27174.0 936.732 18 -2 2 -3 26249.1 1162.55 4 2 -2 3 26188.1 889.992 16 2 -2 4 11272.7 605.083 16 2 -2 4 10530.5 507.182 10 -2 2 -4 10436.8 611.044 9 2 -2 4 11095.5 423.987 19 -2 2 -4 10713.0 747.813 4 2 -2 5 524.610 112.862 14 2 -2 5 627.988 142.355 10 -2 2 -5 475.462 147.425 9 2 -2 5 606.442 159.363 16 -2 2 -5 983.158 250.616 4 2 -2 6 9223.27 545.202 10 2 -2 6 9089.46 493.029 14 -2 2 -6 9100.90 617.283 9 -2 2 -6 8629.95 712.239 4 2 -2 6 8669.02 573.143 16 2 -2 7 78056.5 1518.17 14 -2 2 -7 75784.5 2156.49 4 -2 2 -7 75994.5 1873.03 9 2 -2 7 77986.5 1698.54 10 -2 2 -8 9913.12 705.594 9 -2 2 -8 9417.13 793.898 4 2 -2 8 10366.5 660.721 10 2 -2 8 10003.3 590.841 14 -2 2 -9 68.6596 134.863 9 2 -2 9 102.838 71.9684 15 -2 2 -10 13208.4 879.223 9 2 -2 10 13550.8 853.653 15 -2 2 -11 393.207 161.805 9 2 -2 11-61.4741 84.7928 15 2 -2 12 16014.5 1020.87 15 2 -2 13 8391.61 382.687 31 2 -2 13 8149.20 374.076 35 2 -2 13 7368.62 716.493 15 2 -2 14-40.7426 56.3277 31 2 -2 14-37.9784 52.2801 35 2 -2 14 128.477 67.2432 24 2 -2 15 2967.07 242.181 31 2 -2 15 3209.25 251.080 35 2 -2 15 3486.86 244.519 24 2 -2 16 1399.09 173.998 35 2 -2 16 1331.13 167.173 31 2 -2 17 10187.8 447.140 31 2 -2 17 9786.03 436.181 35 2 -2 18 61.5183 59.5068 35 2 -2 18 94.7706 62.2572 31 2 -2 19 2995.92 238.832 35 2 -2 19 2866.92 234.995 31 2 -2 20-28.8337 57.4576 35 2 -2 20 175.956 78.1798 31 2 -2 21 121.818 69.0472 35 2 -2 21 153.166 56.3969 31 2 -2 22 21.7243 54.0634 35 2 -2 22 24.8619 40.1102 20 -2 1 24 746.440 101.732 33 -2 1 23-31.9297 56.6677 33 -2 1 22 1803.32 178.347 33 -2 1 21 793.934 128.860 33 -2 1 21 918.549 151.502 20 -2 1 20 93.1660 75.9550 33 -2 1 20 262.608 108.932 20 -2 1 19 900.264 145.583 33 -2 1 19 1132.05 165.329 20 -2 1 18 4276.98 293.272 33 -2 1 18 4311.80 299.810 20 -2 1 17 284.719 91.0828 33 -2 1 17 249.706 76.9120 20 -2 1 16 7540.13 372.078 33 -2 1 16 7239.71 369.715 20 -2 1 15 522.433 218.577 14 -2 1 15 588.230 221.255 2 -2 1 14 3637.23 501.414 14 2 -1 -13 4391.19 571.005 11 -2 1 13 4100.28 517.122 14 -2 1 12 2973.59 421.123 14 2 -1 -12 2960.54 448.699 11 -2 1 11 9151.45 691.847 14 2 -1 -11 9689.46 775.504 11 -2 1 10 1156.12 249.515 14 2 -1 -10 1383.34 270.371 11 2 -1 -9 33684.4 1283.50 11 -2 1 9 32502.5 1167.82 14 -2 1 8 13870.3 718.477 3 -2 1 8 13529.9 715.409 14 2 -1 -8 13535.1 574.802 18 -2 1 7 9089.63 558.776 14 2 -1 -7 9815.28 478.813 18 -2 1 7 9290.89 561.730 3 -2 1 6 40669.3 992.055 17 -2 1 6 41040.1 1100.10 3 2 -1 -6 39965.9 932.681 18 -2 1 6 41698.0 1117.30 14 -2 1 5 8550.59 486.406 14 -2 1 5 8572.89 263.024 9 2 -1 -5 8495.74 417.531 18 2 -1 -5 7701.53 520.482 13 -2 1 5 8493.62 486.325 3 2 -1 -4 39738.5 1128.23 13 -2 1 4 42349.8 648.554 9 2 -1 -4 39865.8 895.071 18 -2 1 4 40245.0 1008.54 14 -2 1 3 10083.6 430.363 17 2 -1 -3 9360.59 547.692 13 -2 1 3 8986.34 328.020 9 2 -1 -3 8903.55 425.075 18 -2 1 3 9199.51 466.318 14 2 -1 -2 215835. 2047.25 18 -2 1 2 228693. 1747.32 9 -2 1 1 6217.52 312.544 9 2 -1 -1 5722.42 344.855 18 2 -1 -1 5800.98 206.053 7 2 -1 0 19654.4 777.983 8 2 -1 0 20578.2 642.901 12 2 -1 1 1803.82 132.156 10 -2 1 -1 1760.24 271.759 4 2 -1 1 1900.95 198.578 12 2 -1 2 65606.1 1117.60 16 2 -1 2 66739.4 910.261 10 -2 1 -3 19133.0 812.156 4 2 -1 3 18378.2 623.161 16 2 -1 3 18323.4 541.334 10 2 -1 4 18800.3 590.581 19 2 -1 4 19413.9 696.972 8 2 -1 4 17580.2 635.341 16 -2 1 -4 18862.1 715.306 9 2 -1 4 19290.1 620.304 10 2 -1 5 1083.08 172.580 14 -2 1 -5 728.722 161.647 9 2 -1 5 961.840 173.223 16 2 -1 5 858.051 147.720 10 2 -1 6 40648.2 1044.11 14 2 -1 6 41387.3 1092.40 10 -2 1 -6 38821.5 1147.24 9 2 -1 7 304.381 102.302 14 -2 1 -7 256.590 110.210 9 2 -1 7 199.581 101.594 15 2 -1 8 14849.4 711.418 14 -2 1 -8 16051.4 815.895 9 2 -1 8 15212.4 757.054 15 -2 1 -9 11211.7 711.547 9 2 -1 9 11461.2 667.484 14 2 -1 9 11357.5 700.828 15 -2 1 -10 47.7778 79.1961 9 2 -1 10 103.314 86.1734 15 2 -1 10-109.665 92.7833 14 2 -1 11 40950.7 1489.50 15 2 -1 11 43765.0 1471.46 14 -2 1 -11 40285.2 1452.86 9 2 -1 12 5843.74 595.507 15 2 -1 12 6419.80 596.224 14 2 -1 13 4433.85 514.973 14 2 -1 13 4105.71 521.152 15 2 -1 14 42.4063 41.6587 31 2 -1 14 89.3311 54.8492 35 2 -1 15 765.462 128.529 31 2 -1 15 782.192 128.742 35 2 -1 16 5715.24 334.602 35 2 -1 16 5423.16 325.924 31 2 -1 17 4.18061 71.1073 35 2 -1 17-10.4625 53.7210 31 2 -1 18 3774.49 271.113 35 2 -1 18 4001.00 281.310 31 2 -1 19 351.356 92.1131 31 2 -1 19 429.720 109.426 35 2 -1 20 293.127 84.2280 31 2 -1 20 248.077 84.5793 35 2 -1 21 108.523 55.0391 31 2 -1 21 62.6872 69.7014 35 2 -1 21 48.7294 60.9273 20 2 -1 22 80.2230 48.6159 31 2 -1 22 132.790 70.3910 35 2 -1 22-73.1547 57.1032 20 2 -1 23 18.2486 44.2634 35 2 -1 23 7.70847 37.1882 20 -2 0 24 10.8449 41.7043 33 -2 0 23 1143.96 132.454 33 -2 0 22 49.2602 54.8201 33 -2 0 22 226.189 89.0479 20 -2 0 21 75.5149 66.3052 33 -2 0 21 334.522 98.9782 20 -2 0 20 6154.07 328.521 35 -2 0 20 6215.48 346.754 33 -2 0 20 6096.11 349.137 20 -2 0 19 564.987 119.919 33 -2 0 19 350.611 97.5055 35 -2 0 19 348.454 96.6474 20 -2 0 18 474.191 115.190 33 -2 0 18 360.959 99.4851 35 -2 0 18 360.073 100.727 20 -2 0 17 1832.58 190.519 33 -2 0 17 1818.85 197.612 20 -2 0 16 1519.02 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16320.7 890.362 16 -3 3 -5 14295.6 1188.42 4 -3 3 -6 8635.97 727.681 9 3 -3 6 9361.54 693.517 16 -3 3 -6 9095.06 964.858 4 -3 3 -7 3743.14 634.468 4 -3 3 -7 3023.98 453.911 9 3 -3 7 3298.02 428.309 16 -3 3 -8-152.955 122.835 9 -3 3 -8-58.6185 150.165 4 -3 3 -9 2335.07 433.024 9 -3 3 -9 2031.07 485.065 4 3 -3 9 2499.53 389.350 15 -3 3 -10 56.5835 101.400 9 3 -3 11 2347.08 202.867 35 3 -3 11 2433.63 208.800 31 3 -3 11 2676.97 210.241 28 3 -3 12 3522.22 252.674 35 3 -3 12 4168.48 262.209 28 3 -3 12 3969.09 272.787 31 3 -3 13 5497.22 305.179 28 3 -3 13 5112.81 307.212 35 3 -3 13 5298.72 318.619 31 3 -3 14 101.718 69.0267 35 3 -3 14 170.968 82.0836 28 3 -3 14 185.339 65.3057 31 3 -3 15 6602.80 353.996 35 3 -3 15 6672.77 361.311 31 3 -3 15 7060.89 335.067 28 3 -3 16 2852.83 211.471 28 3 -3 16 3020.36 243.869 31 3 -3 16 3065.70 240.234 35 3 -3 17 153.565 78.3693 35 3 -3 17 81.6114 54.6616 31 3 -3 18 196.817 73.0475 31 3 -3 18 31.1373 60.9060 35 3 -3 19 263.752 74.0417 31 3 -3 19 237.610 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162.033 21 4 5 15 71.9769 75.2222 35 4 5 15 72.2861 60.3642 21 4 5 16 7164.48 378.760 35 4 5 16 7488.35 358.371 21 4 5 17 3765.68 283.830 35 4 5 17 4207.47 270.897 21 4 5 18 7424.02 383.076 35 -4 -5 -18 8692.61 537.626 22 4 5 18 8021.58 371.604 21 4 5 19 3873.81 275.286 35 -4 -5 -19 3521.85 338.626 22 4 5 19 4119.60 263.078 21 4 5 20 136.533 67.4524 33 4 5 20-34.6737 76.0146 35 4 5 20-3.07144 45.8266 21 -4 -5 -20-39.7554 89.7953 22 4 5 21 123.319 58.4657 33 4 5 21 126.606 63.7561 35 4 5 21 164.396 73.1451 21 4 5 22 93.8549 64.8741 35 4 5 22-1.28362 40.6621 21 -4 -6 20-32.7036 46.5932 20 -4 -6 19 346.643 84.1214 24 -4 -6 19 151.075 60.8978 20 -4 -6 18 18.7857 54.9512 20 -4 -6 18 31.1900 51.4681 24 -4 -6 17 91.1668 63.9137 33 -4 -6 17-50.3550 71.6927 20 -4 -6 17 30.8289 64.1223 24 -4 -6 16 477.983 106.571 33 -4 -6 16 306.831 93.6594 24 -4 -6 15 3837.35 271.146 33 -4 -6 15 3094.73 244.155 24 -4 -6 14 355.600 102.044 33 -4 -6 14 266.473 86.9986 24 -4 -6 13 10103.2 441.775 33 -4 -6 13 9760.71 431.781 24 -4 -6 12 3905.98 275.991 33 -4 -6 12 4905.62 303.603 29 -4 -6 12 4222.95 282.027 24 -4 -6 11 4894.11 301.680 29 -4 -6 11 4716.82 299.273 33 -4 -6 11 4780.25 297.847 24 -4 -6 10 5303.72 301.893 24 -4 -6 10 4374.72 572.651 15 -4 -6 9 120.616 99.1006 10 -4 -6 9 468.476 189.146 15 -4 -6 8 4815.45 561.940 10 4 6 -8 5622.15 624.463 1 -4 -6 8 5768.70 608.197 15 4 6 -7 2536.90 419.750 1 -4 -6 7 2143.66 362.716 10 4 6 -6 13764.5 945.351 1 4 6 -5 224.447 169.679 1 -4 -6 5 235.017 131.801 16 -4 -6 4 8038.09 697.928 7 -4 -6 4 6992.94 548.015 17 -4 -6 4 6611.96 592.807 16 4 6 -4 7712.53 679.814 1 -4 -6 3 5135.52 558.777 7 -4 -6 3 4620.26 432.635 17 -4 -6 3 5259.69 505.243 16 4 6 -3 4329.42 507.053 1 -4 -6 2 3613.07 376.401 17 -4 -6 2 3800.49 425.201 16 4 6 -2 3574.17 448.419 1 -4 -6 2 3148.98 434.271 7 4 6 -1 57400.8 1757.51 1 -4 -6 1 58968.9 1487.56 17 -4 -6 1 57963.2 1600.36 16 -4 -6 1 57935.8 1866.71 7 -4 -6 0 9547.25 787.547 7 -4 -6 0 9177.70 586.527 17 -4 -6 0 9652.16 646.768 16 4 6 0 8355.15 666.624 1 4 6 1 84051.2 1712.48 19 -4 -6 -1 79996.4 2263.90 5 4 6 1 79459.1 2050.37 1 4 6 2 133.268 96.3793 19 -4 -6 -2 86.6042 115.379 5 4 6 2-49.0627 120.496 1 4 6 3 14430.9 884.947 1 -4 -6 -3 12186.1 985.046 5 4 6 4 149.628 83.4321 14 4 6 4 155.554 93.1407 3 -4 -6 -4 145.847 92.8840 11 -4 -6 -4 113.608 170.448 5 4 6 4 98.7304 116.779 1 4 6 5 12519.4 823.360 1 -4 -6 -5 14048.4 773.806 11 -4 -6 -5 13834.2 1240.42 5 4 6 5 13290.6 704.168 14 4 6 5 13190.7 724.532 3 4 6 6 31255.9 1143.24 14 4 6 6 32904.4 1165.27 3 -4 -6 -6 33141.5 1241.28 11 4 6 6 33642.2 1331.55 1 4 6 7 22181.6 1007.27 14 -4 -6 -7 21663.8 1050.45 11 4 6 7 21526.2 1071.03 1 4 6 7 20032.0 936.952 3 4 6 8 4082.12 441.705 3 4 6 8 3863.61 462.354 1 4 6 8 3916.17 440.714 14 -4 -6 -8 3726.24 458.382 11 4 6 9 822.446 222.897 1 -4 -6 -9 612.193 206.127 11 4 6 9 838.997 223.823 14 4 6 10 9052.04 722.039 1 -4 -6 -10 8975.43 778.378 11 4 6 11-338.019 160.076 14 -4 -6 -11-273.849 160.279 11 4 6 11 106.678 143.200 1 -4 -6 -12 1609.59 372.654 11 4 6 12 2580.13 420.957 14 4 6 13 1473.71 167.826 35 -4 -6 -13 1797.92 242.828 22 4 6 13 1455.01 155.220 21 4 6 14 352.896 99.4210 35 -4 -6 -14 203.904 129.735 22 4 6 14 332.370 86.8071 21 4 6 15 330.454 98.7022 35 4 6 15 216.134 72.8326 21 -4 -6 -15 423.105 169.440 22 4 6 16 711.638 108.725 25 4 6 16 1044.93 149.786 35 -4 -6 -16 1032.24 208.258 22 4 6 16 1086.03 145.074 21 4 6 17 154.585 63.8747 25 4 6 17 232.237 92.8812 35 -4 -6 -17 75.6059 86.5273 22 4 6 17 187.274 59.1165 21 4 6 18 5418.32 323.499 35 -4 -6 -18 5264.00 410.903 22 4 6 18 5084.07 297.949 21 4 6 19 256.173 87.3156 35 4 6 19 253.007 73.2556 21 4 6 20-31.8515 65.4658 35 4 6 20 9.87652 47.0640 21 4 6 21 127.617 65.4587 35 4 6 21 231.459 71.4802 33 4 6 21 232.893 77.2393 21 4 6 22 170.379 55.7426 33 4 6 22 138.953 57.1150 21 4 6 23 180.738 47.7980 33 -4 -7 19 629.850 94.5018 24 -4 -7 19 520.518 77.0593 20 -4 -7 18 163.660 61.0353 20 -4 -7 18 316.404 78.6094 24 -4 -7 17 1490.10 155.964 24 -4 -7 17 1385.51 143.976 20 -4 -7 16 427.816 103.941 24 -4 -7 15 1109.96 149.397 24 -4 -7 14 420.436 92.9100 35 -4 -7 14 351.668 92.9115 24 -4 -7 13 5224.45 306.689 35 -4 -7 13 4813.55 307.434 24 -4 -7 12 65.3822 62.9704 29 -4 -7 12 75.5881 65.1444 33 -4 -7 12 70.2161 61.2403 24 -4 -7 11 8490.23 406.681 33 -4 -7 11 8850.56 415.827 29 -4 -7 11 8192.89 394.997 24 -4 -7 10 2415.61 219.650 29 -4 -7 10 2814.12 231.031 24 -4 -7 9 2010.92 204.711 33 -4 -7 9 1625.36 182.784 29 -4 -7 9 1992.66 196.563 24 -4 -7 8 84.3560 63.4526 24 4 7 -8-202.162 137.996 1 -4 -7 7 6411.56 691.311 10 4 7 -7 8920.89 843.560 1 -4 -7 6 5129.00 586.125 16 4 7 -6 5938.10 684.420 1 -4 -7 5 8013.47 730.403 16 4 7 -5 7221.70 743.382 1 -4 -7 4 377.398 179.930 7 4 7 -4 1097.65 312.417 1 -4 -7 4 1020.91 262.904 16 4 7 -3 260.970 154.315 1 -4 -7 3 277.702 128.128 7 -4 -7 3 234.004 142.381 16 -4 -7 2-238.143 152.109 7 4 7 -2 13.6043 93.9427 1 -4 -7 2 38.7126 88.7957 16 -4 -7 1 4070.01 544.792 7 4 7 -1 2944.98 444.791 1 -4 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15 486.917 104.981 21 4 7 16 759.362 135.646 35 4 7 16 714.184 116.342 25 4 7 16 790.620 123.141 21 4 7 17 5247.56 290.598 25 4 7 17 5772.34 319.339 21 4 7 18 166.719 64.8164 25 4 7 18 62.3503 61.9527 21 4 7 19 1140.38 123.742 25 4 7 19 1370.23 155.661 21 4 7 20 474.939 98.9010 21 4 7 21 192.134 65.7088 33 4 7 21 146.680 58.9964 21 4 7 22 1129.02 114.878 33 4 7 22 1116.37 113.844 21 -4 -8 18 1011.21 108.653 24 -4 -8 17 19.1599 47.6352 24 -4 -8 16 49.0932 54.4266 24 -4 -8 15 913.786 122.573 35 -4 -8 15 873.890 128.705 24 -4 -8 14 452.278 95.3112 35 -4 -8 14 495.960 103.444 24 -4 -8 13 168.281 60.8183 35 -4 -8 13 347.474 91.4480 24 -4 -8 12 718.548 128.033 24 -4 -8 11 427.351 107.327 24 -4 -8 10 1088.62 158.084 29 -4 -8 10 1028.31 146.155 24 -4 -8 9 4108.34 294.576 29 -4 -8 9 3802.27 277.547 24 -4 -8 8 388.730 104.577 29 -4 -8 8 205.301 70.0713 24 -4 -8 7 247.409 99.8427 29 -4 -8 7 156.159 74.9742 24 -4 -8 6 12163.5 477.233 29 -4 -8 6 10729.8 450.661 24 -4 -8 5 7567.77 771.871 16 4 8 -4 82.1750 119.334 1 -4 -8 4 219.770 150.058 16 4 8 -3 1320.95 336.522 1 -4 -8 3 1152.47 347.940 7 -4 -8 3 1745.21 360.091 16 -4 -8 2 19565.8 1274.66 7 -4 -8 2 19870.9 1205.59 16 4 8 -2 18965.0 1234.81 1 -4 -8 1 1097.00 312.438 7 4 8 -1 1947.31 401.909 1 -4 -8 1 1485.13 327.493 16 -4 -8 0 2445.39 456.349 7 4 8 0 2356.75 436.425 1 -4 -8 0 2322.22 400.748 18 -4 -8 0 2124.62 418.747 16 -4 -8 -1 8360.90 863.552 7 -4 -8 -1 7905.28 746.811 18 4 8 1 8133.24 782.135 1 -4 -8 -2 22568.3 1406.91 7 4 8 2 23179.7 1322.29 1 -4 -8 -3 961.348 330.064 7 -4 -8 -3 862.307 296.465 5 4 8 3 883.236 271.017 1 -4 -8 -4 1570.97 432.698 5 4 8 4 2030.20 403.601 1 -4 -8 -5 330.665 229.677 5 4 8 5 45.6385 141.127 1 4 8 6 3307.02 502.531 1 -4 -8 -6 2144.14 551.692 5 4 8 7 2972.30 470.655 1 -4 -8 -7 2005.51 550.498 5 4 8 8 2202.84 392.603 1 -4 -8 -8 3291.80 696.839 5 4 8 9 165.455 133.139 1 4 8 10-47.6561 55.5042 21 4 8 11 119.770 70.3561 21 -4 -8 -12 12842.2 587.450 22 4 8 12 11893.1 446.956 21 4 8 13 6305.05 328.667 25 -4 -8 -13 6810.30 430.399 22 4 8 13 6125.57 326.098 21 4 8 14 1388.39 161.841 25 4 8 14 1723.87 181.170 21 4 8 15 338.625 87.3785 25 4 8 15 260.572 79.4118 21 4 8 16 723.056 116.110 25 4 8 16 655.904 116.309 21 4 8 17 1135.86 140.948 25 4 8 17 985.198 138.981 21 4 8 18 3461.83 225.189 25 4 8 18 3742.08 247.724 21 4 8 19 1787.33 155.104 25 4 8 19 1632.80 158.613 21 4 8 20 1874.68 143.085 25 4 8 20 1993.39 164.876 21 4 8 21 15.8965 39.3645 33 4 8 21 12.3019 48.2043 21 -4 -9 16 96.8710 50.2563 24 -4 -9 15 2296.56 167.113 35 -4 -9 15 2089.70 170.444 24 -4 -9 14-21.5760 52.4610 35 -4 -9 14 9.57754 51.3878 24 -4 -9 13 287.161 78.6777 35 -4 -9 13 491.630 103.263 24 -4 -9 12 88.7865 61.8298 24 -4 -9 11 299.464 81.2426 24 -4 -9 10 7989.09 390.804 24 -4 -9 9 2438.75 219.607 24 -4 -9 8 3590.84 269.050 24 -4 -9 7 322.338 87.7578 28 -4 -9 7 398.244 103.024 24 -4 -9 6 6551.22 340.759 28 -4 -9 6 6331.59 357.984 24 -4 -9 5 282.625 88.0182 24 -4 -9 4 690.832 128.808 24 -4 -9 3 429.261 98.1647 32 -4 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512.915 89.6687 25 4 9 18 621.526 104.261 21 4 9 19 1471.98 134.593 25 4 9 19 1574.61 146.223 21 4 9 20-18.3389 34.3411 25 4 9 20-58.4792 45.6808 21 4 9 21 40.8201 38.5856 33 -4 -10 14 93.7595 44.9216 35 -4 -10 14 6.40366 37.2617 24 -4 -10 13 1834.29 152.944 35 -4 -10 13 1839.23 158.229 24 -4 -10 12 1007.36 124.359 35 -4 -10 12 1000.34 125.304 24 -4 -10 11 845.602 126.288 24 -4 -10 10 2229.52 197.948 24 -4 -10 9 444.386 95.7952 24 -4 -10 8 4140.28 258.888 28 -4 -10 8 3698.25 264.977 24 -4 -10 7 1091.76 141.951 28 -4 -10 7 931.568 143.438 24 -4 -10 6 1410.08 164.769 28 -4 -10 6 1411.04 170.738 24 -4 -10 5 1124.28 149.269 28 -4 -10 5 907.116 143.948 24 -4 -10 4 1596.89 176.507 28 -4 -10 4 1504.17 179.647 24 -4 -10 3 2548.59 215.553 32 -4 -10 3 2111.35 212.837 24 -4 -10 2 3618.78 259.042 32 -4 -10 1 1067.11 147.115 32 -4 -10 0 222.284 81.0396 32 -4 -10 -1 27541.8 705.880 32 -4 -10 -2 2668.86 226.625 32 -4 -10 -3 25004.8 677.576 32 -4 -10 -4 219.574 77.6269 32 -4 -10 -5 873.913 135.704 32 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124.601 22 5 6 14 78.6218 50.9662 21 5 6 15 210.884 93.3047 35 -5 -6 -15 107.797 133.751 22 5 6 15 68.0381 55.4623 21 5 6 16 6752.15 364.684 35 -5 -6 -16 6412.20 471.330 22 5 6 16 6612.72 340.191 21 5 6 17 9519.03 426.272 35 -5 -6 -17 9147.65 548.862 22 5 6 17 8966.63 393.365 21 5 6 18 532.356 113.711 35 -5 -6 -18 723.870 183.497 22 5 6 18 549.071 109.156 21 5 6 19-43.1066 65.2927 35 5 6 19-71.9553 58.3789 21 5 6 20-39.3199 70.4640 35 -5 -6 -20 0.56792 89.4060 22 5 6 20 143.116 62.8299 21 5 6 21 73.5018 46.1729 33 -5 -6 -21 71.1068 76.0643 22 5 6 21 77.8182 48.3806 21 5 6 22 93.1345 45.9382 21 -5 -7 19 122.693 56.5585 24 -5 -7 18 1923.00 164.584 24 -5 -7 17 156.872 72.8751 33 -5 -7 17 65.4014 58.5708 24 -5 -7 16 386.460 94.7865 33 -5 -7 16 449.383 101.879 24 -5 -7 15 1051.33 147.662 33 -5 -7 15 1402.87 165.114 24 -5 -7 14 155.226 72.5810 29 -5 -7 14 108.597 76.9429 33 -5 -7 14 42.2743 59.9039 24 -5 -7 13 4507.00 299.727 29 -5 -7 13 4527.46 300.498 33 -5 -7 13 4225.09 288.567 24 -5 -7 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139.795 22 6 6 11 226.898 69.4806 21 6 6 12 366.633 86.6532 35 -6 -6 -12 315.912 134.915 22 6 6 12 273.431 74.8514 21 6 6 13 6084.98 329.831 35 -6 -6 -13 5093.25 410.868 22 6 6 13 5758.98 310.366 21 6 6 14 8900.57 403.717 35 -6 -6 -14 7869.31 512.511 22 6 6 14 8947.20 387.797 21 6 6 15 65.3085 68.3243 35 6 6 15 44.8431 44.8048 21 6 6 16-18.2078 62.3773 35 -6 -6 -16 27.4144 120.914 22 6 6 16-29.0272 45.6393 21 6 6 17 3602.94 262.544 35 -6 -6 -17 3216.12 337.737 22 6 6 17 3419.78 239.762 21 6 6 18 1688.00 175.698 35 -6 -6 -18 1793.86 265.778 22 6 6 18 1800.32 173.738 21 6 6 19 1927.36 180.223 35 -6 -6 -19 2179.82 269.406 22 6 6 19 1871.18 167.166 21 -6 -6 -20-125.996 102.816 22 6 6 20 9.98723 39.4052 21 -6 -6 -21 126.328 77.4726 22 6 6 21 18.3541 32.0602 21 -6 -6 -22 879.879 119.612 22 6 6 22 1057.81 93.6056 21 -6 -7 19 469.478 76.1655 24 -6 -7 18 1902.01 159.364 24 -6 -7 18 1788.14 153.774 33 -6 -7 17 65.3417 56.3672 33 -6 -7 17 32.0407 55.2513 24 -6 -7 16 1635.25 175.568 33 -6 -7 16 1259.55 146.080 24 -6 -7 16 1680.37 168.011 29 -6 -7 15 69.3104 70.7942 29 -6 -7 15 92.3377 82.4251 33 -6 -7 15 54.4556 45.7426 24 -6 -7 14 888.799 137.886 29 -6 -7 14 872.177 140.704 33 -6 -7 14 909.485 136.423 24 -6 -7 13 2258.26 217.428 29 -6 -7 13 2183.28 218.169 33 -6 -7 13 2245.65 207.487 24 -6 -7 12 5808.50 344.125 29 -6 -7 12 5868.82 350.163 33 -6 -7 12 5809.04 338.368 24 -6 -7 11 116.942 77.1819 29 -6 -7 11 103.751 88.6666 33 -6 -7 11 82.6525 59.0373 24 -6 -7 10 1124.96 163.980 33 -6 -7 10 1182.68 160.896 29 -6 -7 10 1191.57 150.859 24 -6 -7 9-41.7716 59.2806 29 -6 -7 9-8.60209 69.8777 33 -6 -7 9-21.6114 53.0347 23 -6 -7 9 0.41890 61.9009 24 -6 -7 8 55.0899 62.0064 29 -6 -7 8 35.4026 63.4484 33 -6 -7 8 6.72266 52.9996 23 -6 -7 8 57.4321 64.0736 24 -6 -7 7-63.3624 73.6492 29 -6 -7 7 127.847 87.3591 33 -6 -7 7-46.2873 63.5075 24 -6 -7 6 354.608 173.239 17 6 7 -5 7505.21 774.652 1 -6 -7 5 6902.76 673.400 17 6 7 -4 4597.55 597.063 1 -6 -7 4 5159.06 580.226 17 -6 -7 3 401.853 186.081 7 -6 -7 3 188.161 120.076 17 6 7 -2 7066.73 724.714 1 -6 -7 2 6765.83 684.294 7 -6 -7 2 7401.41 677.473 17 6 7 -1 9149.06 824.937 1 -6 -7 1 8874.20 780.984 7 6 7 0 362.592 166.532 1 -6 -7 0 553.061 216.371 7 -6 -7 -1 831.404 246.651 7 6 7 1 1054.54 253.059 19 6 7 1 824.083 256.197 1 6 7 2 3163.73 476.396 1 -6 -7 -2 3115.64 501.275 7 6 7 2 3387.73 435.799 19 6 7 3 13032.7 945.804 1 6 7 3 12406.8 849.996 19 -6 -7 -3 12241.1 977.021 5 6 7 4 71.4489 123.732 1 6 7 4 292.430 106.774 19 -6 -7 -4 25.4832 114.456 5 6 7 5 7294.64 698.070 1 -6 -7 -5 5656.86 720.814 5 -6 -7 -6 112.495 187.155 5 6 7 6 151.229 134.307 1 6 7 7 7088.15 691.971 1 -6 -7 -7 6578.13 862.943 5 -6 -7 -8 4702.73 790.040 5 6 7 8 5293.79 603.204 1 6 7 8 5137.72 577.187 14 6 7 9 23.3065 79.6534 14 -6 -7 -9 268.663 243.930 5 6 7 9 151.588 124.123 1 -6 -7 -10 180.550 102.727 22 6 7 10 252.291 73.4922 21 -6 -7 -11 124.491 100.379 22 6 7 11 78.5252 67.7929 21 -6 -7 -12 120.939 106.255 22 6 7 12 462.131 100.846 21 -6 -7 -13 4163.03 372.175 22 6 7 13 4025.03 266.679 21 6 7 14 4040.41 274.871 35 -6 -7 -14 3930.93 361.695 22 6 7 14 3842.58 261.755 21 6 7 15 79.7314 62.5313 35 -6 -7 -15 241.959 123.744 22 6 7 15 83.2464 57.7613 21 -6 -7 -16 2206.42 274.387 22 6 7 16 2450.02 210.036 21 6 7 17 1673.60 159.863 25 -6 -7 -17 1616.10 244.668 22 6 7 17 1662.66 169.945 21 6 7 18-52.0842 46.4859 25 -6 -7 -18-43.2533 105.575 22 6 7 18 41.8563 54.2947 21 -6 -7 -19 368.796 115.343 22 6 7 19 983.202 127.409 21 6 7 20 106.611 36.0782 33 -6 -7 -20 261.248 115.870 22 6 7 20 167.593 59.7411 21 -6 -7 -21-50.0656 66.2255 22 6 7 21 52.8322 40.7201 21 -6 -8 17 1192.63 128.969 24 -6 -8 16 336.958 81.4307 24 -6 -8 15 2901.45 216.556 24 -6 -8 15 2734.80 205.508 29 -6 -8 14 2182.38 196.501 29 -6 -8 14 2270.50 203.010 24 -6 -8 13 2085.67 205.034 33 -6 -8 13 2320.51 209.979 24 -6 -8 13 2253.90 211.664 29 -6 -8 12 1415.53 176.768 29 -6 -8 12 1325.64 174.854 33 -6 -8 12 1625.86 183.153 24 -6 -8 11 22.0817 59.2841 29 -6 -8 11 93.6046 79.5691 33 -6 -8 11 106.596 67.5174 24 -6 -8 10 1436.81 179.635 29 -6 -8 10 1757.88 198.542 33 -6 -8 10 1327.96 169.316 24 -6 -8 9 68.3179 68.4650 29 -6 -8 9 128.692 83.3157 33 -6 -8 9 156.158 76.6218 24 -6 -8 8 3652.43 274.186 29 -6 -8 8 3601.64 281.003 33 -6 -8 8 3606.59 272.445 24 -6 -8 7 64.0716 74.4311 29 -6 -8 7-41.7062 63.7919 23 -6 -8 7 39.8991 51.0101 24 -6 -8 6 1075.71 160.352 29 -6 -8 6 858.006 133.374 23 -6 -8 6 930.547 143.551 24 -6 -8 5 1412.66 176.529 29 -6 -8 5 1348.50 157.327 23 -6 -8 5 1351.29 164.530 24 -6 -8 4 289.392 88.7649 29 -6 -8 3 141.794 133.524 7 6 8 -3 223.273 173.919 1 -6 -8 2 4971.23 652.886 7 6 8 -2 4216.55 608.324 1 6 8 -1 39574.9 1815.22 1 -6 -8 1 35438.1 1704.29 7 -6 -8 0-193.669 156.398 7 6 8 0 233.458 199.271 1 -6 -8 -1 15879.6 1180.06 7 6 8 1 15153.4 1108.38 1 -6 -8 -2 433.756 218.098 7 6 8 2 647.032 249.613 1 6 8 3 3466.72 528.939 1 -6 -8 -3 3721.32 585.231 7 6 8 4 563.505 232.676 1 -6 -8 -4 299.703 199.404 5 6 8 5 16101.7 1110.13 1 -6 -8 -5 11646.0 1071.10 5 6 8 6 6561.45 705.059 1 -6 -8 -6 6228.82 799.026 5 -6 -8 -7 1037.70 365.134 5 -6 -8 -8 1737.22 223.207 22 6 8 8 1974.85 177.601 21 -6 -8 -9 2201.87 263.845 22 6 8 9 1905.41 182.193 21 -6 -8 -10 6537.47 432.171 22 6 8 10 7283.22 344.759 21 -6 -8 -11 875.799 179.608 22 6 8 11 691.959 115.382 21 -6 -8 -12 7268.99 472.847 22 6 8 12 7086.64 346.918 21 -6 -8 -13 719.256 161.720 22 6 8 13 895.362 128.537 21 -6 -8 -14 694.422 162.555 22 6 8 14 736.548 120.737 21 -6 -8 -15 409.956 132.867 22 6 8 15 629.086 112.692 21 6 8 16 72.4902 61.6030 25 -6 -8 -16-16.4168 108.210 22 6 8 16 34.6730 49.6657 21 6 8 17 1577.19 154.335 25 -6 -8 -17 1449.80 212.897 22 6 8 17 1119.68 136.188 21 6 8 18 3518.07 214.250 25 -6 -8 -18 3694.51 306.810 22 6 8 18 3601.51 233.582 21 6 8 19 133.271 48.5581 25 6 8 19 94.0812 60.2830 21 6 8 20 5210.93 243.816 21 6 8 21 36.6339 31.9624 33 6 8 21 46.3316 41.9011 21 -6 -9 16 911.032 108.637 24 -6 -9 15 197.056 65.7176 24 -6 -9 14 99.2904 61.1183 24 -6 -9 13 1308.94 155.813 24 -6 -9 12 886.954 133.210 24 -6 -9 11 228.198 92.6723 29 -6 -9 11 19.9965 56.0221 24 -6 -9 10 57.2421 77.0756 29 -6 -9 10-15.2018 70.1918 24 -6 -9 9 96.9742 78.7715 29 -6 -9 9-71.5640 74.0137 24 -6 -9 8 1609.49 197.371 29 -6 -9 8 1063.01 153.482 24 -6 -9 7 5336.25 333.187 29 -6 -9 7 4814.38 317.970 24 -6 -9 6 29.0607 65.4594 29 -6 -9 6-44.9258 67.5059 24 -6 -9 5 623.205 140.102 29 -6 -9 5 622.784 112.804 23 -6 -9 5 529.166 117.725 24 -6 -9 4 127.169 87.0226 29 -6 -9 4 149.485 71.9103 32 -6 -9 4 51.3940 64.9092 23 -6 -9 4 279.151 95.8454 24 -6 -9 3 101.902 72.4529 29 -6 -9 3 105.287 63.8603 32 -6 -9 3 121.778 69.9457 23 -6 -9 2 2102.43 197.722 32 -6 -9 2 2041.53 195.967 23 -6 -9 1 574.556 112.123 32 -6 -9 1 685.696 123.098 23 -6 -9 0 96.2854 69.5459 32 -6 -9 0 78.3610 65.2248 23 -6 -9 -1 214.387 78.6476 32 -6 -9 -1 230.303 90.2295 23 -6 -9 -2 155.764 69.8649 32 -6 -9 -2 151.393 76.7484 23 -6 -9 -3 54.0566 56.1283 32 -6 -9 -3 107.901 67.4441 23 -6 -9 -4 413.953 94.2081 32 -6 -9 -4 299.100 88.2847 23 -6 -9 -5-43.4371 47.3301 32 -6 -9 -5 42.5785 61.3542 23 -6 -9 -6 1443.77 167.040 32 -6 -9 -7 3222.44 244.354 32 -6 -9 -8 1244.55 159.547 32 6 9 8 1237.03 142.314 21 -6 -9 -9 10078.0 421.507 32 6 9 9 10895.6 415.792 21 6 9 10 2586.07 207.093 21 6 9 11 5134.21 292.519 21 6 9 12 355.525 92.7883 21 6 9 13 2106.59 192.763 21 6 9 14 1679.41 173.587 21 6 9 15 413.964 93.1310 25 6 9 15 384.709 91.8724 21 6 9 16 2011.12 180.793 25 6 9 16 1930.68 178.787 21 6 9 17 3225.73 213.363 25 6 9 17 2842.10 207.589 21 6 9 18 82.7134 58.9604 25 6 9 18 11.9016 44.1560 21 6 9 19 3083.42 176.743 25 6 9 19 3469.57 202.305 21 6 9 20 75.3542 40.1897 25 6 9 20-15.8708 34.7029 21 -6 -10 14 155.468 64.2294 24 -6 -10 13-10.7694 44.2578 24 -6 -10 12 145.684 63.8305 24 -6 -10 11 836.055 123.437 24 -6 -10 10-56.1519 73.0031 24 -6 -10 9 2030.70 198.467 24 -6 -10 8 350.855 88.9825 24 -6 -10 7 1129.50 155.189 24 -6 -10 6 1351.60 171.611 24 -6 -10 5 1204.88 161.761 24 -6 -10 4 1064.25 145.342 32 -6 -10 4 1256.61 155.751 23 -6 -10 4 836.533 146.747 24 -6 -10 3 89.0780 57.5933 32 -6 -10 3 131.321 72.4096 23 -6 -10 3 281.448 98.8957 24 -6 -10 2 6220.36 341.907 32 -6 -10 2 6619.27 352.516 23 -6 -10 1 3342.56 252.869 32 -6 -10 1 3038.81 249.087 23 -6 -10 0 4773.24 305.312 32 -6 -10 0 5154.87 317.399 23 -6 -10 -1 1439.46 169.303 32 -6 -10 -1 1402.37 171.406 23 -6 -10 -2 4580.73 299.653 32 -6 -10 -2 4147.69 289.536 23 -6 -10 -3 1055.01 148.706 32 -6 -10 -3 909.200 136.328 23 -6 -10 -4-39.6470 64.4627 32 -6 -10 -5 2748.53 236.228 32 -6 -10 -6-68.6303 61.2923 32 -6 -10 -7 1290.51 164.560 32 -6 -10 -8 2913.11 236.739 32 -6 -10 -9 2891.85 230.909 32 -6 -10 -10 1079.16 143.530 32 6 10 11 297.738 83.9094 21 6 10 12 1535.89 164.528 25 6 10 12 1818.34 173.703 21 6 10 13 144.066 72.9245 25 6 10 13 190.450 70.0952 21 6 10 14 86.8559 61.1946 25 6 10 14 138.029 65.7116 21 6 10 15 1271.95 146.360 25 6 10 15 1377.22 146.269 21 6 10 16 976.899 124.601 25 6 10 16 1096.24 132.466 21 6 10 17 100.423 49.2005 25 6 10 17 34.3581 44.8824 21 6 10 18-20.1590 39.3634 25 6 10 18-74.8462 45.9973 21 6 10 19 33.2870 33.7865 25 6 10 19-20.4534 29.8885 21 -6 -11 12 97.6028 45.9286 24 -6 -11 11 94.0819 52.7445 24 -6 -11 10 945.272 122.555 24 -6 -11 9 367.927 90.3561 24 -6 -11 8 146.143 66.8321 24 -6 -11 7 31.0394 60.4618 24 -6 -11 6 15.9279 66.3544 24 -6 -11 5 2079.93 191.030 28 -6 -11 5 2180.84 218.024 24 -6 -11 4 878.925 129.286 32 -6 -11 4 847.655 130.423 28 -6 -11 4 840.849 140.019 24 -6 -11 3 693.018 113.997 32 -6 -11 3 490.351 115.720 24 -6 -11 2-15.3736 53.3026 32 -6 -11 2 32.9374 61.4401 24 -6 -11 1 370.673 95.8292 32 -6 -11 0-26.4339 64.0027 32 -6 -11 -1 6015.47 336.575 32 -6 -11 -2 5668.84 327.532 32 -6 -11 -3 663.008 121.525 32 -6 -11 -4 12420.2 487.400 32 -6 -11 -5 27.0696 52.8986 32 -6 -11 -6 60.3294 66.4229 32 6 11 7 110.333 55.8799 25 -6 -11 -7 111.236 61.9288 32 -6 -11 -8 7482.48 370.204 32 6 11 8 7641.11 343.727 25 6 11 9 226.720 72.3094 25 -6 -11 -9 268.178 83.1132 32 -6 -11 -10 910.085 127.222 32 6 11 10 1161.37 142.018 25 -6 -11 -11 1658.69 162.026 32 6 11 11 1702.09 163.559 25 6 11 12 953.522 127.588 25 6 11 13 1866.24 170.510 25 6 11 14 54.9207 59.0443 25 6 11 14 43.9565 33.9248 21 6 11 15 309.343 78.9527 25 6 11 15 317.394 70.1856 21 6 11 16 21.1340 42.7458 25 6 11 16 47.8998 36.5192 21 6 11 17 404.239 74.7808 25 6 11 17 432.182 69.8469 21 -6 -12 10 39.3517 39.1927 24 -6 -12 9 1316.79 127.748 24 -6 -12 8 107.902 50.7775 24 -6 -12 7 401.209 82.2661 24 -6 -12 6 514.341 101.883 24 -6 -12 5 1376.12 143.924 28 -6 -12 5 1015.82 137.078 24 -6 -12 4 326.951 82.9976 28 -6 -12 4 322.184 86.8706 24 -6 -12 3 194.216 68.5247 32 -6 -12 3 120.152 54.5470 28 -6 -12 3 162.023 77.0129 24 -6 -12 2 136.141 65.0546 32 -6 -12 2 157.351 65.5543 28 -6 -12 2 179.117 79.1142 24 -6 -12 1 286.856 79.3993 32 -6 -12 1 238.453 88.2075 24 -6 -12 0 65.2234 56.6327 32 -6 -12 0 232.181 83.2866 24 -6 -12 -1 188.866 67.0114 32 -6 -12 -2 111.519 67.1083 32 -6 -12 -3 71.0583 69.8046 32 -6 -12 -4 325.069 101.231 32 -6 -12 -5 124.814 73.9461 32 -6 -12 -6 9743.94 412.567 32 -6 -12 -7 841.270 131.210 32 -6 -12 -8 64.3251 68.1899 32 6 12 8 44.5184 39.2612 25 -6 -12 -9 3326.12 231.571 32 6 12 9 3384.22 212.885 25 -6 -12 -10 818.217 117.225 32 6 12 10 693.509 102.581 25 -6 -12 -11 120.190 51.9597 32 6 12 11 107.116 54.2820 25 6 12 12 1134.42 124.408 25 6 12 13 295.785 65.7665 25 6 12 14 73.3287 47.3989 25 6 12 15 286.963 62.9681 25 -6 -13 6 58.6758 45.0742 24 -6 -13 5 775.031 87.6110 28 -6 -13 5 770.283 99.7771 24 -6 -13 4 10.0381 35.6610 28 -6 -13 4-31.4145 46.1360 24 -6 -13 3 1.69684 38.2286 32 -6 -13 3 64.4467 50.2265 28 -6 -13 3-30.3985 51.7337 24 -6 -13 2-8.51034 39.4743 32 -6 -13 2-45.6506 50.7040 28 -6 -13 2 75.1380 59.2434 24 -6 -13 1 652.158 101.122 32 -6 -13 1 700.180 107.993 28 -6 -13 1 652.631 103.898 24 -6 -13 0 49.0825 41.8478 32 -6 -13 0 88.4320 66.7055 28 -6 -13 0-12.3580 49.3340 24 -6 -13 -1 408.197 83.0928 32 -6 -13 -1 470.199 92.0560 28 -6 -13 -1 381.100 85.0003 24 -6 -13 -2 532.197 95.9710 32 -6 -13 -2 503.453 102.291 24 -6 -13 -3 57.2866 53.3645 32 -6 -13 -4 187.105 66.3486 32 -6 -13 -5 249.329 74.6976 32 -6 -13 -6 495.124 99.6502 32 -6 -13 -7 104.513 59.8866 32 -6 -13 -8 406.440 84.5999 32 -6 -13 -9 32.9485 48.3813 32 6 13 10 109.783 41.1551 25 6 13 11 0.30971 30.7445 25 6 13 12 15.5186 34.5706 25 6 13 13 85.9261 41.6255 25 -6 -14 0 1071.37 108.427 28 -6 -14 0 1065.65 104.014 24 -6 -14 -1 287.706 65.8398 28 -6 -14 -1 307.360 63.9530 24 -6 -14 -2 82.8208 47.6700 28 -6 -14 -2 34.5342 28.1072 24 -6 -14 -3 880.450 105.720 28 -6 -14 -3 903.283 100.796 24 -6 -14 -4 47.8452 37.5324 28 -6 -14 -4-40.9424 41.9238 24 -6 -14 -5 865.692 102.136 28 -6 -14 -5 645.499 90.0926 24 -6 -14 -6 144.260 47.5337 28 -6 -14 -6 154.043 46.0014 24 -6 -14 -7 1.12263 30.3844 28 -6 -14 -7 112.865 47.3895 24 7 -7 -8 383.460 67.7447 34 -7 7 8 454.816 72.1019 30 7 -7 -7 47.8806 37.5160 34 -7 7 7 24.6107 35.7080 30 7 -7 -6 502.281 81.6925 34 -7 7 6 446.078 74.2825 30 7 -7 -5 258.768 65.5487 34 -7 7 5 310.656 64.2261 30 7 -7 -4 238.470 64.7496 34 -7 7 4 232.711 54.4191 30 7 -7 -3 42.3029 39.0550 34 -7 7 3 77.1075 36.2530 30 7 -7 -2-26.6263 41.5091 34 -7 7 2 102.708 43.4503 30 7 -7 -1 155.801 56.0924 34 7 -7 0 484.940 77.4039 34 7 -7 1 365.587 67.4812 34 7 -7 2 367.196 64.3304 34 -7 6 13 193.441 52.6164 26 -7 6 12 206.004 55.2209 26 -7 6 11 93.4116 48.8714 26 -7 6 11-64.4573 53.3216 30 7 -6 -10 406.076 69.8924 34 -7 6 10 473.937 78.3627 26 -7 6 10 472.432 88.9074 30 7 -6 -9 423.123 82.5107 34 -7 6 9 365.111 78.7171 30 7 -6 -8 142.745 60.2074 34 -7 6 8 42.3905 46.1427 30 7 -6 -7-23.4146 49.8357 34 -7 6 7 72.5851 46.3017 30 7 -6 -6 76.0669 54.4437 34 -7 6 6 68.9747 47.6638 30 -7 6 5 414.578 87.1630 30 7 -6 -5 319.835 84.5739 34 -7 6 4 52.4073 42.2874 30 7 -6 -4-39.1589 62.1184 34 7 -6 -3 946.506 132.665 34 -7 6 3 1173.17 136.606 30 -7 6 2 52.0434 41.8563 30 7 -6 -2 45.1743 57.6278 34 7 -6 -1 2205.43 188.573 34 7 -6 0 50.3861 48.9678 34 7 -6 1 1140.39 132.306 34 7 -6 2 786.173 111.351 34 7 -6 3 21.4525 45.6632 34 7 -6 4 2311.63 156.735 28 7 -6 4 2633.21 176.770 34 7 -6 5 884.672 100.012 28 7 -6 5 891.953 100.585 34 7 -6 6 756.905 84.5034 34 7 -6 6 718.897 87.8660 28 7 -6 7 78.4556 40.5400 28 -7 5 15 121.234 48.2970 26 -7 5 14 144.805 56.1097 26 -7 5 13 290.248 72.7819 26 -7 5 12 97.8615 61.2472 30 -7 5 12 58.7450 55.3500 26 -7 5 11 2263.35 183.640 26 -7 5 11 1931.74 179.058 30 7 -5 -10 412.015 86.5761 34 -7 5 10 376.369 87.9125 30 -7 5 10 424.147 90.9933 26 7 -5 -9 292.034 78.5380 34 -7 5 9 333.491 74.7545 26 -7 5 9 410.748 94.9489 30 7 -5 -8 25.0623 51.2711 34 -7 5 8 62.7280 52.4655 26 -7 5 8 100.617 59.0780 30 7 -5 -7 54.9987 49.2702 34 -7 5 7 100.328 56.1545 26 -7 5 7 23.3726 43.0868 30 -7 5 6 688.849 114.163 30 7 -5 -6 668.386 118.604 34 -7 5 5 96.9941 71.0741 30 7 -5 -5 75.3009 66.3202 34 -7 5 4 256.200 78.6490 30 7 -5 -4 189.760 71.9398 34 -7 5 3 120.952 58.5027 30 7 -5 -3 48.2455 58.6532 34 -7 5 2 490.944 100.287 30 7 -5 -2 460.238 107.352 34 7 -5 -1 1164.65 155.695 34 7 -5 0 38.8450 59.0769 34 7 -5 1 1625.38 173.251 34 7 -5 2 70.5633 54.7901 34 7 -5 3 111.538 66.6971 34 7 -5 4 1270.48 143.700 34 7 -5 4 1271.95 137.353 28 7 -5 5 1417.10 145.584 34 7 -5 5 1539.18 152.516 28 7 -5 6 3313.81 209.492 34 7 -5 6 3254.72 212.157 28 7 -5 7 27.1438 41.1307 34 7 -5 7 51.7998 44.3422 28 7 -5 8 204.558 64.8674 28 7 -5 9 743.858 98.5889 28 7 -5 10 941.884 101.923 28 -7 4 17-73.4639 53.2913 26 -7 4 16 168.019 66.4138 26 -7 4 15 142.398 58.7210 26 -7 4 14 1233.20 141.119 26 -7 4 13 190.812 88.1010 26 -7 4 12 163.994 79.2416 26 -7 4 12 32.3009 52.0315 30 -7 4 11 788.701 121.550 26 -7 4 11 711.786 118.357 30 -7 4 10 565.282 111.969 26 -7 4 10 588.607 112.603 30 -7 4 9 119.811 75.9584 26 7 -4 -9 63.5035 44.9922 34 -7 4 9-30.6954 62.1669 30 -7 4 8 222.962 85.3228 26 7 -4 -8 217.942 79.7423 34 -7 4 8 200.774 74.6982 30 7 -4 -7 757.414 125.870 34 -7 4 7 652.390 111.925 26 -7 4 7 847.500 131.083 30 7 -4 -6 7347.85 372.104 34 -7 4 6 7382.67 360.064 26 -7 4 6 6705.69 351.553 30 7 -4 -5 6499.63 356.747 34 -7 4 5 6915.76 347.202 26 -7 4 5 6847.25 352.862 30 -7 4 4 558.074 106.141 30 -7 4 4 477.152 102.694 26 7 -4 -4 605.590 119.026 34 7 -4 -3 5561.60 329.574 34 -7 4 3 5594.75 315.383 30 7 -4 -2 7914.93 392.842 34 -7 4 2 8164.66 373.254 30 7 -4 -1 1176.84 154.478 34 7 -4 0 5121.24 317.878 34 7 -4 1 5467.43 322.811 34 7 -4 2 1423.67 173.295 34 7 -4 3 3332.61 247.652 34 7 -4 3 3284.60 230.161 28 7 -4 4 6009.19 326.137 34 7 -4 4 6257.97 320.518 28 7 -4 5 5770.14 312.515 34 7 -4 5 5875.50 310.363 28 7 -4 6 328.485 89.4967 34 7 -4 6 280.600 75.7971 28 7 -4 7 73.4350 57.4710 34 7 -4 7 104.472 58.4797 28 7 -4 8 1485.93 148.633 34 7 -4 8 1621.05 161.705 28 7 -4 9 1566.70 159.133 28 7 -4 10 139.762 70.2466 28 7 -4 11 53.7295 46.8850 28 7 -4 12 38.5941 41.2041 28 -7 3 18 7.51030 40.4319 26 -7 3 17 131.767 61.8911 26 -7 3 16 64.6091 51.5383 26 -7 3 15 240.467 77.3330 26 -7 3 14 597.863 111.789 26 -7 3 13 92.7723 58.4683 26 -7 3 12 344.790 91.3877 26 -7 3 12 373.059 94.7328 30 -7 3 11 190.334 76.8073 26 -7 3 11 145.959 74.2422 30 -7 3 10 190.855 79.0823 26 -7 3 10 157.688 71.4487 30 -7 3 9-45.0310 49.2147 26 -7 3 9-31.5820 59.8910 30 -7 3 8-19.0508 66.9103 26 7 -3 -8 97.0209 62.9143 34 -7 3 8 53.6931 52.4070 30 -7 3 7 1086.60 148.496 26 7 -3 -7 1206.57 151.946 34 -7 3 7 1277.57 158.854 30 -7 3 6 547.900 107.617 30 -7 3 6 570.047 115.707 26 7 -3 -6 507.281 106.467 34 7 -3 -5 5690.36 330.944 34 -7 3 5 5075.25 306.973 26 -7 3 5 5354.31 312.863 30 7 -3 -4 1693.94 183.719 34 -7 3 4 1573.14 175.254 26 -7 3 4 1813.68 182.317 30 -7 3 3 193.153 74.0310 30 7 -3 -3 259.066 81.7472 34 -7 3 3 159.880 68.7518 26 -7 3 2 2523.14 216.668 26 7 -3 -2 2764.94 237.438 34 -7 3 2 2874.11 221.628 30 7 -3 -1 181.093 84.6549 34 7 -3 0 6687.33 355.457 34 7 -3 1 729.625 124.670 34 7 -3 2 2580.33 222.588 34 7 -3 3 1140.37 151.655 34 7 -3 3 1214.98 145.582 28 7 -3 4 11826.4 461.077 34 7 -3 4 11739.2 448.427 28 7 -3 5 623.609 112.912 28 7 -3 5 344.233 85.2103 34 7 -3 6 10.5965 49.2185 34 7 -3 6-23.1284 46.9843 28 7 -3 7-2.09011 48.3767 34 7 -3 7 24.4182 53.9143 28 7 -3 8 6086.01 313.353 34 7 -3 8 6357.19 327.871 28 7 -3 9 1211.65 140.377 34 7 -3 9 1432.49 165.947 28 7 -3 10 220.127 74.8765 28 7 -3 11-18.1287 51.0665 28 7 -3 12 34.6554 58.2154 28 7 -3 13 1207.74 127.231 28 7 -3 13 1308.23 125.562 31 7 -3 14 487.622 78.6237 28 7 -3 14 568.999 79.4185 31 -7 2 19 32.0866 40.1567 29 -7 2 19 40.0672 39.3837 26 -7 2 18 107.908 51.9976 26 -7 2 17 902.442 120.432 26 -7 2 16 17.3240 61.3105 26 -7 2 15-3.67753 52.3389 26 -7 2 14 673.841 115.194 26 -7 2 13 4338.56 276.290 26 -7 2 12 2228.39 201.401 26 -7 2 11 498.698 111.234 26 -7 2 11 471.615 102.918 30 -7 2 10 20.8517 54.9571 26 -7 2 10-46.5400 56.6328 30 -7 2 9 2369.73 211.144 26 -7 2 9 2506.52 216.944 30 -7 2 8 172.235 73.8387 26 -7 2 8 161.231 67.0248 30 -7 2 7 5047.02 302.969 26 -7 2 7 4604.93 291.321 30 -7 2 6 640.493 119.402 26 7 -2 -6 660.748 116.908 34 -7 2 6 561.749 108.951 30 -7 2 5 350.105 84.9519 30 -7 2 5 348.612 95.6120 26 7 -2 -5 506.810 108.300 34 -7 2 4 1185.46 144.993 30 7 -2 -4 1021.18 139.627 34 -7 2 4 1171.85 152.826 26 -7 2 3 1192.09 143.469 30 7 -2 -3 1170.59 154.798 34 -7 2 3 1041.16 147.363 26 7 -2 -2 5093.42 304.329 34 -7 2 2 4521.93 289.369 26 7 -2 -1 4726.64 292.660 34 -7 2 1 4555.51 293.250 26 7 -2 0 112.704 60.0389 34 -7 2 0 180.050 80.4537 26 7 -2 1 893.411 140.211 34 7 -2 2 10079.0 423.701 34 7 -2 3 60.3471 53.5675 34 7 -2 3 37.5403 47.1527 28 7 -2 4 4176.17 275.825 34 7 -2 4 4251.90 266.363 28 7 -2 5 146.997 73.7676 34 7 -2 5 118.410 61.1882 28 7 -2 6 3406.95 247.737 28 7 -2 6 3311.36 244.348 34 7 -2 7 539.611 103.857 34 7 -2 7 315.795 89.9300 28 7 -2 8 735.630 121.318 34 7 -2 8 702.814 116.881 28 7 -2 9 407.538 89.4871 34 7 -2 9 527.531 105.912 28 7 -2 9 436.019 91.6203 31 7 -2 10 431.853 97.3839 34 7 -2 10 334.584 85.9818 28 7 -2 10 426.657 95.8492 31 7 -2 11 890.505 132.337 28 7 -2 11 1278.64 155.075 31 7 -2 12 856.797 127.328 28 7 -2 12 867.162 125.918 31 7 -2 13-18.3376 61.0392 28 7 -2 13-1.41345 48.4058 31 7 -2 14 76.3479 50.9467 28 7 -2 14-28.7597 45.0785 31 7 -2 15 428.962 79.7323 28 7 -2 15 417.478 79.0369 31 7 -2 16 12.8059 37.8253 28 7 -2 16 46.6832 40.3541 31 -7 1 20 884.448 106.342 29 -7 1 19 37.4346 43.7914 29 -7 1 19 29.3020 42.4651 26 -7 1 18 3217.46 200.257 26 -7 1 18 3206.57 224.168 29 -7 1 17 73.6572 57.7151 26 -7 1 16 863.387 118.533 26 -7 1 15 115.103 64.0723 26 -7 1 14 1725.10 177.241 26 -7 1 13 2891.97 222.554 26 -7 1 12 738.028 122.481 26 -7 1 11 2880.62 224.790 26 -7 1 10 41.1370 53.9524 26 -7 1 10 91.9306 61.3185 30 -7 1 9 3944.52 259.840 26 -7 1 9 4614.11 289.761 30 -7 1 8 796.470 120.851 26 -7 1 8 646.372 113.251 30 -7 1 7 555.520 111.641 26 -7 1 7 656.417 110.590 30 -7 1 6 776.961 121.891 26 -7 1 6 638.319 106.943 30 -7 1 5 255.607 69.9784 26 7 -1 -5 360.626 218.051 12 7 -1 -5 116.070 204.794 8 7 -1 -4 14961.3 1178.28 12 7 -1 -4 16678.1 1411.24 8 7 -1 -3 1974.89 427.134 12 7 -1 -3 2946.75 589.755 8 7 -1 -2 1423.52 417.522 8 7 -1 -1-54.3307 146.831 8 7 -1 0 132.828 181.319 8 -7 1 -1 4197.02 516.357 9 7 -1 1 3474.61 554.756 8 7 -1 2 66.4412 56.5591 34 -7 1 -2 319.416 153.247 9 7 -1 3 8317.98 375.541 34 -7 1 -3 7904.81 737.697 9 7 -1 3 8876.19 844.397 8 7 -1 4 544.787 102.432 34 7 -1 4 510.788 90.7662 28 7 -1 5 3236.39 240.699 34 7 -1 5 3170.18 233.304 28 7 -1 6 2559.33 215.524 34 7 -1 6 2699.06 218.878 28 7 -1 7-42.8718 54.9344 34 7 -1 7-32.2853 59.9423 28 7 -1 8 1252.80 153.803 34 7 -1 8 1232.02 154.133 28 7 -1 8 1395.50 166.121 31 7 -1 9 126.206 66.8548 34 7 -1 9 191.940 71.7872 28 7 -1 9 247.605 66.2050 31 7 -1 10 59.8598 54.0364 34 7 -1 10 43.5474 49.9984 28 7 -1 10 127.473 66.4068 31 7 -1 11 2043.75 185.603 34 7 -1 11 1636.87 174.455 28 7 -1 11 2351.37 214.303 31 7 -1 12 104.031 69.8106 28 7 -1 12 207.326 81.5619 31 7 -1 13 155.613 67.8362 28 7 -1 13 191.081 72.0563 31 7 -1 14-31.2638 52.0298 28 7 -1 14 21.5794 53.6544 31 7 -1 15 562.938 93.3270 28 7 -1 15 603.228 105.977 31 7 -1 16 271.633 66.8455 28 7 -1 16 225.368 66.3509 31 7 -1 17-4.84616 44.1650 31 -7 0 20 634.952 95.3739 29 -7 0 20 484.363 83.4141 33 -7 0 19 1493.40 152.679 29 -7 0 19 1362.05 139.194 33 -7 0 18 816.123 124.251 29 -7 0 18 592.714 100.793 33 -7 0 17 414.452 86.2087 26 -7 0 17 401.546 94.8821 33 -7 0 16 3839.43 241.139 26 -7 0 16 4252.84 269.854 33 -7 0 15-4.24171 59.2773 26 -7 0 15 43.3102 50.4650 33 -7 0 14 613.996 108.285 26 -7 0 13 605.413 108.374 26 -7 0 12 217.513 76.9851 26 -7 0 11 3299.96 231.822 26 -7 0 10 339.203 84.1917 26 -7 0 9 1606.96 162.618 26 -7 0 9 1490.10 163.023 30 -7 0 8 10539.5 402.994 26 -7 0 8 10296.3 413.958 30 7 0 -7 2226.04 506.351 12 7 0 -7 2067.01 571.946 8 7 0 -6 10899.9 1024.30 12 7 0 -6 6757.30 962.817 8 7 0 -5 1979.06 432.202 12 -7 0 5 3973.28 551.521 17 7 0 -5 3245.77 651.836 8 7 0 -4 6893.81 780.746 12 -7 0 4 8582.04 802.762 17 7 0 -4 7324.40 950.394 8 7 0 -3 609.411 241.012 12 -7 0 3 143.619 124.827 17 7 0 -3 596.188 263.379 8 7 0 -2 4209.49 663.535 8 7 0 -1 137.519 175.208 8 7 0 0 218.459 187.800 8 7 0 1 143.267 150.659 8 7 0 2 7007.96 771.173 8 -7 0 -3 2481.46 395.273 9 7 0 3 2328.40 453.172 8 7 0 4 2135.71 426.896 8 7 0 5 11497.8 958.250 8 7 0 6-26.6385 60.0019 34 7 0 6 183.735 69.2886 28 7 0 6-201.836 153.136 8 7 0 7 12945.7 467.348 34 7 0 7 12615.5 461.378 28 7 0 8 369.288 92.1094 34 7 0 8 179.555 72.5839 28 7 0 9 3897.36 260.288 34 7 0 9 3636.90 257.334 28 7 0 10 2862.81 223.260 34 7 0 10 2758.87 226.799 28 7 0 10 3024.46 242.746 31 7 0 11 8467.40 379.194 34 7 0 11 8785.08 396.935 28 7 0 11 8362.31 408.027 31 7 0 12 1897.58 182.194 34 7 0 12 1646.66 176.771 28 7 0 12 1684.00 186.237 31 7 0 13 151.245 68.7745 28 7 0 13 241.450 88.7848 31 7 0 14 1289.13 151.422 28 7 0 14 1298.68 160.324 31 7 0 15 293.760 81.6834 28 7 0 15 317.792 90.8810 31 7 0 16 17.2220 49.9895 28 7 0 16 46.6649 62.1566 31 7 0 17 1130.38 133.428 31 7 0 18 1098.41 121.682 31 -7 -1 21 69.4350 38.8134 29 -7 -1 21 77.2630 48.9804 33 -7 -1 20 1674.69 148.233 29 -7 -1 20 1185.27 129.559 33 -7 -1 19 564.689 97.0827 29 -7 -1 19 519.572 100.963 33 -7 -1 18-49.1952 55.2601 29 -7 -1 18 25.0235 64.3085 33 -7 -1 17 442.842 106.349 29 -7 -1 17 540.466 111.872 33 -7 -1 16 36.9206 61.0706 29 -7 -1 16 163.556 74.8826 33 -7 -1 15 68.5342 49.8319 33 -7 -1 14 1751.49 171.912 26 -7 -1 14 1804.31 188.127 33 -7 -1 13 10228.9 402.488 26 -7 -1 13 9973.95 422.598 33 -7 -1 12 699.317 111.482 26 -7 -1 12 572.431 109.112 33 -7 -1 11 3454.56 233.177 26 -7 -1 10 488.595 91.3753 26 -7 -1 9 1715.56 162.342 26 -7 -1 9 1979.07 386.672 17 7 1 -8 714.367 279.795 12 -7 -1 8 283.177 167.085 17 7 1 -8 533.280 314.653 8 7 1 -7 4872.16 693.113 12 -7 -1 7 4785.03 591.805 17 7 1 -7 3338.67 720.225 8 7 1 -6 15862.4 1206.32 12 -7 -1 6 16669.0 1104.03 17 7 1 -6 16615.5 1502.02 8 7 1 -5 600.321 276.954 12 -7 -1 5 8.49953 80.1708 17 7 1 -5 418.182 272.653 8 7 1 -4 795.284 297.797 12 -7 -1 4 585.952 222.261 17 7 1 -4 975.159 351.529 8 7 1 -3 9428.45 869.112 12 7 1 -3 10405.3 1075.48 8 7 1 -2-148.600 283.096 8 7 1 -1 6142.06 790.099 8 -7 -1 0 5280.07 520.462 6 7 1 0 6451.84 771.511 8 -7 -1 -1 1461.99 277.297 6 7 1 1 1234.84 362.611 8 -7 -1 -2 4445.13 506.848 6 7 1 2 4864.18 634.587 8 -7 -1 -3-86.9862 85.4846 6 7 1 3-98.5329 136.864 8 -7 -1 -4 44.6591 88.0534 6 7 1 4-337.417 190.958 8 -7 -1 -5 64.2840 124.186 6 7 1 5 103.105 117.289 19 -7 -1 -6 357.486 165.106 6 7 1 6 874.074 260.712 19 7 1 6 961.397 298.561 8 -7 -1 -7 14716.5 1041.26 6 7 1 8 98.4936 78.3255 34 7 1 8 82.7957 58.6051 28 7 1 9 6052.99 319.403 34 7 1 9 6087.31 327.774 28 7 1 10 1273.05 150.236 34 7 1 10 1188.10 155.357 28 7 1 11 87.4273 54.1591 34 7 1 11 79.0664 61.2323 28 7 1 12 1811.05 179.629 34 7 1 12 1701.14 182.112 28 7 1 12 1438.18 172.213 31 7 1 13 750.228 117.589 34 7 1 13 849.126 133.823 28 7 1 13 716.054 127.658 31 7 1 14 93.3659 67.4362 28 7 1 14 31.8404 59.9354 31 7 1 15 1918.14 178.205 28 7 1 15 1790.28 189.042 31 7 1 16 267.242 82.7175 31 7 1 17 154.624 72.6884 31 7 1 18 295.405 77.9863 31 7 1 19 2010.76 160.050 31 -7 -2 21 1677.86 124.895 29 -7 -2 21 1580.37 141.365 33 -7 -2 20 1350.61 134.535 29 -7 -2 20 1326.59 141.758 33 -7 -2 19-49.7808 53.7459 29 -7 -2 19 4.19221 61.0077 33 -7 -2 18 1905.52 186.984 29 -7 -2 18 1967.84 189.598 33 -7 -2 17 1469.38 171.255 29 -7 -2 17 1697.05 185.333 33 -7 -2 16 27.7327 57.4987 29 -7 -2 16 184.080 79.1608 33 -7 -2 15 855.793 132.190 29 -7 -2 15 802.538 132.027 33 -7 -2 14 506.948 108.567 29 -7 -2 14 682.616 126.288 33 -7 -2 13 11611.2 465.450 33 -7 -2 12 15392.9 523.423 33 -7 -2 11 5534.70 310.003 33 -7 -2 10 2208.01 179.189 26 7 2 -9 8804.22 948.024 12 7 2 -9 8696.17 1170.87 8 7 2 -8 2404.74 523.509 12 -7 -2 8 2025.78 410.400 17 7 2 -8 3188.46 701.886 8 7 2 -7 1062.68 330.961 12 -7 -2 7 884.470 275.203 17 7 2 -7 904.171 354.156 8 7 2 -6 3312.13 535.140 12 -7 -2 6 3545.55 522.354 17 7 2 -6 3003.34 665.045 8 7 2 -5 5049.41 652.386 12 -7 -2 5 4864.83 609.484 17 7 2 -5 4203.36 731.141 8 7 2 -4 2141.84 428.159 12 -7 -2 4 1512.27 329.785 17 7 2 -4 1955.58 477.751 8 7 2 -3 3685.90 542.774 12 7 2 -3 2290.39 518.447 8 7 2 -2-426.337 253.549 8 7 2 -1-23.0329 169.542 8 -7 -2 0 446.638 136.665 6 7 2 0 775.595 276.092 8 -7 -2 -1 374.204 178.412 6 7 2 1 601.072 275.341 8 -7 -2 -2 4554.51 496.966 6 7 2 2 5124.91 643.307 8 -7 -2 -3 2188.52 348.621 6 7 2 3 1756.18 398.705 8 -7 -2 -4 10356.5 781.543 6 7 2 4 9474.34 851.972 8 -7 -2 -5 2717.03 422.270 6 7 2 5 2159.66 394.292 19 7 2 5 1967.96 395.452 8 -7 -2 -6 370.497 176.037 6 7 2 6 567.432 211.843 19 7 2 6 151.750 144.822 8 -7 -2 -7 2415.22 415.270 6 7 2 7 1973.78 375.909 19 7 2 7 1612.21 353.116 8 -7 -2 -8 7595.07 752.257 6 7 2 8 7076.27 723.314 19 7 2 9 137.316 67.7867 34 7 2 9 138.883 66.6374 28 7 2 9 251.767 80.7251 19 7 2 10 1409.35 157.168 34 7 2 10 1640.73 175.261 28 7 2 11 1667.58 174.020 34 7 2 11 1773.42 184.485 28 7 2 12 596.402 113.844 34 7 2 12 366.961 91.8471 28 7 2 13 356.150 86.4136 34 7 2 13 446.580 103.394 28 7 2 13 349.556 95.3018 31 7 2 14 2972.36 221.579 34 7 2 14 2931.35 224.885 28 7 2 14 2523.14 229.746 31 7 2 15 700.504 122.962 31 7 2 16 428.435 99.2173 31 7 2 17-15.4498 57.6438 31 7 2 18 32.3900 55.7826 31 7 2 19-45.1288 52.3836 31 7 2 20 254.692 59.1755 31 -7 -2 -20 447.296 143.980 22 -7 -3 21 456.527 81.0801 33 -7 -3 20 211.798 59.1637 29 -7 -3 20 216.638 68.1454 33 -7 -3 19 1171.14 136.142 29 -7 -3 19 1097.55 140.276 33 -7 -3 18 176.415 75.5978 29 -7 -3 18 203.489 75.7383 33 -7 -3 17 74.7462 63.7803 29 -7 -3 17 139.204 65.9459 33 -7 -3 16 360.537 100.378 29 -7 -3 16 316.215 100.231 33 -7 -3 15 750.992 132.445 29 -7 -3 15 836.039 138.783 33 -7 -3 14 551.090 118.526 29 -7 -3 14 738.868 134.478 33 -7 -3 13 24.0800 62.5559 29 -7 -3 13 62.5587 61.6580 33 -7 -3 12 176.512 78.8556 29 -7 -3 12 193.677 79.5141 33 -7 -3 11 2146.61 201.930 29 -7 -3 11 2410.35 212.012 33 -7 -3 10-36.9285 50.8491 29 -7 -3 10 90.2594 70.7006 33 7 3 -9 2659.86 506.421 12 -7 -3 9 2166.81 418.026 17 7 3 -9 1172.02 474.392 8 7 3 -8 275.234 209.707 12 -7 -3 8 169.228 129.489 17 7 3 -8-74.9657 217.428 8 7 3 -7 508.871 221.798 12 -7 -3 7 318.974 174.039 17 7 3 -7 702.854 336.952 8 7 3 -6 43.0685 130.570 12 -7 -3 6-126.474 134.903 17 7 3 -6-138.099 201.459 8 7 3 -5 3224.46 518.950 12 -7 -3 5 2654.99 476.470 17 7 3 -5 2824.32 603.519 8 7 3 -4 4311.52 583.850 12 -7 -3 4 4066.47 571.282 17 7 3 -4 3266.70 603.533 8 7 3 -3 1341.74 384.939 8 7 3 -2 1995.00 474.602 8 7 3 -1 1538.98 413.412 8 -7 -3 0-26.0070 124.424 6 7 3 0 68.4168 183.271 8 -7 -3 -1 1086.45 244.297 6 7 3 1 574.936 251.456 8 -7 -3 -2 11200.8 757.883 6 7 3 2 10782.3 911.383 8 -7 -3 -3 10945.5 769.163 6 7 3 3 11685.9 932.242 8 -7 -3 -4 25.3806 137.638 6 7 3 4 139.797 133.952 19 7 3 4 407.937 150.780 8 -7 -3 -5 2153.17 359.680 6 7 3 5 2471.52 430.743 19 7 3 5 2342.86 418.255 8 -7 -3 -6 2486.62 394.253 6 7 3 6 3455.36 499.414 19 7 3 6 3129.39 493.528 8 7 3 7 9609.55 826.608 19 7 3 7 10074.5 878.307 8 -7 -3 -8-46.8855 113.251 6 7 3 8 15.7467 76.7972 19 7 3 9 692.774 239.736 14 7 3 9 165.027 147.789 19 7 3 10 1400.73 158.925 28 7 3 10 1350.27 155.996 34 7 3 10 1449.02 154.113 27 7 3 10 1147.18 137.015 21 7 3 11 867.523 132.894 34 7 3 11 885.677 132.998 28 7 3 11 1005.00 133.767 21 7 3 12 3167.55 239.380 34 7 3 12 3254.01 228.463 21 7 3 13 8242.76 382.030 34 7 3 14 706.117 117.939 34 7 3 14 744.510 132.789 31 7 3 15 1425.24 157.309 34 7 3 15 1206.91 158.048 31 7 3 16 1212.18 156.440 31 7 3 17 1857.51 187.755 31 7 3 18 214.916 72.5291 31 7 3 19-12.7993 43.3106 31 7 3 20 88.1140 44.5564 31 -7 -3 -20 188.951 119.409 22 -7 -4 20 350.000 81.4958 33 -7 -4 19-56.4486 58.4682 29 -7 -4 19 51.4918 61.9000 33 -7 -4 18 1259.34 143.784 29 -7 -4 18 1338.09 161.338 33 -7 -4 17 168.315 85.9094 29 -7 -4 17 29.3970 68.7102 33 -7 -4 16 840.746 133.559 29 -7 -4 16 548.184 115.096 33 -7 -4 15 836.531 137.047 29 -7 -4 15 673.511 124.533 33 -7 -4 14 1592.23 184.750 29 -7 -4 14 1524.43 179.405 33 -7 -4 13 2185.21 207.028 29 -7 -4 13 1857.96 197.618 33 -7 -4 12 423.522 101.877 29 -7 -4 12 597.071 126.348 33 -7 -4 11 127.581 73.7429 29 -7 -4 11 73.6293 68.1977 33 -7 -4 10 1965.27 193.709 29 -7 -4 10 1905.89 190.394 33 -7 -4 9 5952.16 321.530 29 7 4 -9 6316.32 970.273 8 7 4 -8 487.936 225.949 12 7 4 -8 156.723 241.854 8 -7 -4 8 524.225 192.171 17 7 4 -7 20758.9 1337.53 12 -7 -4 7 20503.7 1276.41 17 7 4 -7 18318.5 1558.96 8 -7 -4 6-89.3017 116.295 17 7 4 -6-70.5204 229.605 8 -7 -4 5 29.7136 122.249 17 7 4 -5 767.187 330.268 8 -7 -4 4 310.483 209.215 17 7 4 -4 456.296 267.186 8 -7 -4 3 4908.98 621.838 17 7 4 -3 4748.25 707.147 8 7 4 -2 2189.43 491.660 8 7 4 -1 10335.7 692.998 1 7 4 -1 10269.6 947.059 8 7 4 0 8198.73 822.990 8 7 4 0 7544.65 613.976 1 7 4 1 21882.7 1308.70 8 7 4 1 21187.4 1037.27 1 7 4 2 23840.7 1327.53 8 7 4 2 24201.5 1132.39 1 7 4 3 1987.90 335.738 1 7 4 3 1325.62 319.024 8 -7 -4 -4 12950.6 858.618 6 7 4 4 13377.5 954.024 19 7 4 4 13466.4 982.094 8 7 4 4 12132.2 839.379 1 -7 -4 -5 144.377 148.059 6 7 4 5 26.7250 96.8730 19 7 4 5-124.124 129.879 8 7 4 5 38.8343 98.6288 1 -7 -4 -6 136.046 117.638 6 7 4 6 53.7468 112.655 8 -7 -4 -7 5926.58 628.071 6 7 4 7 5568.40 632.304 19 7 4 8 146.208 200.285 14 -7 -4 -8 11.2072 84.2385 6 7 4 8 108.331 80.1769 19 -7 -4 -9 5335.82 630.677 6 7 4 9 4793.86 614.658 14 7 4 10 97.4613 49.1020 27 7 4 10 62.4647 49.4922 34 7 4 10-5.55026 47.8863 21 7 4 11 1983.10 191.025 34 7 4 11 1612.01 158.805 27 7 4 11 1603.27 163.348 21 7 4 12 817.627 114.209 27 7 4 12 646.590 112.009 34 7 4 12 803.525 116.750 21 7 4 13 17733.3 564.053 34 7 4 13 17429.0 532.781 21 7 4 14 831.682 130.850 34 7 4 14 747.994 116.866 21 7 4 15 14090.9 521.560 31 7 4 15 15603.2 498.011 21 7 4 16 455.545 100.846 31 7 4 16 320.550 75.7950 21 7 4 17 166.451 67.2784 31 7 4 18 1594.27 161.128 31 -7 -4 -18 1539.54 246.627 22 7 4 19 175.929 59.7012 31 -7 -4 -19 153.710 116.195 22 7 4 20 151.880 49.9587 31 -7 -4 -20 157.595 121.058 22 -7 -4 -21 1456.59 182.750 22 -7 -5 20 7.06088 51.0689 33 -7 -5 19 212.162 59.4897 29 -7 -5 19 308.267 88.1539 33 -7 -5 18-14.6890 52.0054 29 -7 -5 18-15.4999 66.8951 33 -7 -5 17 256.443 81.5155 29 -7 -5 17 207.139 81.0198 33 -7 -5 16 2587.19 216.913 29 -7 -5 16 2400.87 224.261 33 -7 -5 15 185.955 93.9951 29 -7 -5 15 46.4252 68.7214 33 -7 -5 14 935.655 142.788 29 -7 -5 14 770.412 136.209 33 -7 -5 13 351.659 91.8924 29 -7 -5 13 436.501 111.555 33 -7 -5 12 1537.81 180.498 29 -7 -5 12 1514.51 184.926 33 -7 -5 11 9682.13 425.412 29 -7 -5 11 8604.31 411.524 33 -7 -5 10-77.9073 74.6763 29 -7 -5 10-149.752 97.3115 33 -7 -5 9-45.3308 56.7825 29 -7 -5 9 0.20944 78.1191 33 -7 -5 8 67.5888 102.628 17 -7 -5 7 238.253 143.798 17 7 5 -7 432.692 261.848 8 -7 -5 6 237.375 156.554 17 7 5 -6 417.928 261.246 8 -7 -5 5 17.9066 104.501 17 7 5 -5-120.637 175.611 8 -7 -5 4 20618.7 1279.34 17 7 5 -4 22123.8 1483.41 8 -7 -5 3 457.648 200.399 17 7 5 -3 1133.78 335.813 8 7 5 -2 13671.7 851.785 1 -7 -5 2 14258.6 1053.28 17 7 5 -2 15169.3 1147.16 8 7 5 -1 3314.68 427.891 1 7 5 -1 4638.18 626.070 8 7 5 0 7823.62 651.674 1 7 5 0 7172.19 744.027 8 7 5 1 254.097 136.321 1 7 5 1 15.6432 111.813 8 7 5 2 12579.2 926.929 19 7 5 2 11397.0 810.757 1 7 5 2 12317.4 942.527 8 7 5 3-61.4280 95.4202 1 7 5 3-10.0239 88.7633 8 7 5 4 3741.75 515.150 19 7 5 4 3009.22 454.272 8 7 5 4 2702.90 405.100 1 7 5 5 12060.5 920.762 19 7 5 5 10592.3 813.065 1 7 5 6 2516.06 424.295 19 7 5 6 1850.16 373.611 8 7 5 6 2551.72 406.055 1 7 5 7 2108.39 389.992 19 7 5 7 1923.79 360.846 1 7 5 8 1725.23 354.985 14 7 5 8 2497.57 433.853 19 7 5 9 1353.48 322.272 14 7 5 10 4492.95 279.695 34 7 5 10 4347.15 260.730 27 7 5 10 4138.34 255.711 21 7 5 11 3088.03 236.990 34 7 5 11 2895.40 215.018 27 7 5 11 2905.19 217.903 21 7 5 12 226.389 78.2668 27 7 5 12 387.375 97.8336 34 7 5 12 237.884 74.2338 21 7 5 13 680.868 118.551 21 7 5 14 2857.34 222.126 21 7 5 15 3181.22 243.434 31 -7 -5 -15 3222.30 347.771 22 7 5 15 3194.87 233.614 21 7 5 16 2002.54 189.282 31 -7 -5 -16 2214.60 293.977 22 7 5 16 2468.62 200.604 21 7 5 17 403.136 88.1727 31 -7 -5 -17 614.255 186.253 22 7 5 17 327.435 80.8582 21 -7 -5 -18 170.962 141.927 22 7 5 18-5.57743 41.7198 21 7 5 19 79.1834 59.4589 35 -7 -5 -19 56.3046 115.090 22 7 5 19 91.9826 44.9636 21 -7 -5 -20 885.042 170.045 22 -7 -5 -21 455.674 116.209 22 -7 -6 19 52.5494 46.5093 33 -7 -6 18 105.402 60.7654 29 -7 -6 18 15.7952 51.2542 33 -7 -6 18 18.3127 34.6646 24 -7 -6 17 217.650 78.4930 29 -7 -6 17 96.9034 69.8657 33 -7 -6 17 260.624 71.1714 24 -7 -6 16 694.420 122.103 29 -7 -6 16 663.960 121.228 33 -7 -6 16 846.365 114.538 24 -7 -6 15 7447.91 344.867 24 -7 -6 15 7368.55 369.599 29 -7 -6 15 7371.85 379.771 33 -7 -6 14 172.002 72.4161 29 -7 -6 14 295.237 93.7549 33 -7 -6 14 312.263 84.2735 24 -7 -6 13 176.830 68.0696 29 -7 -6 13 234.888 88.1704 33 -7 -6 13 165.082 71.6438 24 -7 -6 12 540.730 116.709 29 -7 -6 12 637.592 128.535 33 -7 -6 12 708.327 115.828 24 -7 -6 11 3483.14 264.672 29 -7 -6 11 3827.53 284.260 33 -7 -6 11 3862.54 262.445 24 -7 -6 10-41.0046 82.6492 33 -7 -6 10 14.5628 47.3712 24 -7 -6 9 2842.18 235.234 29 -7 -6 9 2443.92 226.165 33 -7 -6 9 3065.32 231.404 24 -7 -6 8 1931.65 190.861 29 -7 -6 8 1868.90 200.381 33 -7 -6 7 649.497 122.381 29 -7 -6 7 707.308 130.833 33 -7 -6 7 437.519 188.419 17 -7 -6 6 1624.51 353.486 17 -7 -6 5 6118.61 696.619 17 -7 -6 4 3175.72 499.179 17 7 6 -3 13579.6 928.022 1 -7 -6 3 14417.4 1059.77 17 7 6 -2 46.9219 89.2332 1 -7 -6 2 525.548 212.466 17 7 6 -1 377.515 176.787 1 -7 -6 1 326.319 174.196 17 7 6 0 5232.36 579.829 1 7 6 0 5824.04 617.938 19 7 6 0 5773.36 638.546 8 7 6 1 18540.8 1079.24 1 7 6 1 18468.9 1125.33 19 7 6 1 18721.9 1116.93 8 7 6 2 1043.43 281.074 19 7 6 2 939.075 250.733 1 7 6 2 806.389 246.754 8 7 6 3 539.329 180.230 19 7 6 3 690.642 234.157 8 7 6 3 721.277 234.813 1 7 6 4 2961.17 448.216 1 7 6 4 3713.15 507.947 19 7 6 4 3777.98 498.828 8 7 6 5 5252.85 619.017 19 7 6 5 6650.75 665.349 8 7 6 5 5908.45 619.338 1 7 6 6 165.700 135.898 19 7 6 6 128.263 124.633 1 7 6 7 4767.54 597.208 19 7 6 7 5922.33 644.861 1 7 6 7 4867.61 589.711 14 7 6 8 3946.79 533.943 1 7 6 8 2521.76 421.332 14 7 6 9 1598.93 170.743 34 7 6 9 1603.37 160.365 27 -7 -6 -9 1818.00 235.655 22 7 6 9 1610.12 164.001 21 7 6 10 5988.47 306.379 27 -7 -6 -10 5216.84 400.504 22 7 6 10 5945.11 308.038 21 7 6 11 57.7558 49.9906 27 7 6 11-9.44025 45.0051 21 -7 -6 -12 8317.31 519.957 22 7 6 12 8687.60 382.749 21 -7 -6 -13 174.763 143.209 22 7 6 13 18.9318 47.2108 21 -7 -6 -14 8355.17 528.197 22 7 6 14 9009.32 388.142 21 -7 -6 -15 64.2281 141.028 22 7 6 15 131.622 68.6324 21 -7 -6 -16 1476.80 240.296 22 7 6 16 1915.29 179.998 21 7 6 17 1261.18 145.951 35 -7 -6 -17 1216.99 211.314 22 7 6 17 1073.48 135.988 21 -7 -6 -18 737.248 173.143 22 7 6 18 828.089 114.427 21 -7 -6 -19 1486.01 215.488 22 7 6 19 1444.09 138.382 21 -7 -6 -20-3.22556 86.6651 22 7 6 20-12.0814 38.2604 21 -7 -6 -21 215.409 92.7692 22 7 6 21 130.919 41.7712 21 -7 -7 18 104.086 47.7427 24 -7 -7 17 1886.64 155.935 29 -7 -7 17 1773.33 152.362 24 -7 -7 17 1608.80 162.384 33 -7 -7 16 1304.60 145.395 29 -7 -7 16 1478.69 166.046 33 -7 -7 16 1295.99 143.921 24 -7 -7 15 6.04473 56.0292 29 -7 -7 15 70.0889 75.9330 33 -7 -7 15 98.1272 59.3414 24 -7 -7 14 5727.68 324.018 29 -7 -7 14 5964.93 319.129 24 -7 -7 14 5590.16 332.297 33 -7 -7 13 168.724 82.8165 29 -7 -7 13 273.760 134.670 33 -7 -7 13 141.428 65.0578 24 -7 -7 12 1879.40 198.424 29 -7 -7 12 1737.88 197.403 33 -7 -7 12 2120.18 199.549 24 -7 -7 11 138.941 86.2583 29 -7 -7 11 50.2201 67.2286 33 -7 -7 11 47.0782 58.3126 23 -7 -7 11 56.0196 46.9241 24 -7 -7 10 3027.20 247.498 29 -7 -7 10 3001.55 260.811 33 -7 -7 10 3230.99 244.012 24 -7 -7 10 2949.08 228.971 23 -7 -7 9 1980.62 204.566 29 -7 -7 9 1841.54 206.629 33 -7 -7 9 2173.05 197.712 23 -7 -7 9 2266.12 207.045 24 -7 -7 8 1912.40 199.398 29 -7 -7 8 2064.75 217.157 33 -7 -7 8 2300.79 207.988 24 -7 -7 8 2381.72 208.171 23 -7 -7 7 2763.95 231.727 29 -7 -7 7 2335.98 228.630 33 -7 -7 7 2628.28 220.544 24 -7 -7 7 2309.11 200.658 23 -7 -7 6 10565.6 441.930 29 -7 -7 6 11368.1 482.870 33 -7 -7 6 11207.0 443.800 24 -7 -7 6 10924.6 427.429 23 -7 -7 5 1980.32 208.917 33 -7 -7 5 1897.70 379.249 17 -7 -7 5 1837.94 188.539 23 -7 -7 4 294.188 162.968 17 7 7 -3 22975.2 1315.08 1 -7 -7 3 20651.5 1254.51 17 7 7 -2 7788.29 775.072 1 -7 -7 2 9239.23 838.552 17 7 7 -1-155.632 133.704 1 -7 -7 1-334.361 173.755 17 7 7 0 857.832 258.128 1 7 7 0 300.416 153.523 19 -7 -7 0 722.329 245.106 17 7 7 1 2835.67 460.677 1 7 7 1 2766.22 439.401 19 7 7 2-44.2881 100.358 19 7 7 2 169.225 128.244 1 7 7 3 1849.71 359.762 19 7 7 3 1902.38 368.832 1 7 7 4 4639.96 576.214 19 7 7 4 4185.05 545.337 1 7 7 5 67.3711 104.865 1 7 7 5 173.450 131.790 19 7 7 6 1873.15 366.874 14 7 7 6 2407.83 414.717 1 7 7 7 3092.44 472.216 14 7 7 8 699.290 111.280 27 -7 -7 -8 701.547 156.680 22 7 7 8 676.896 108.713 21 7 7 9 157.509 65.6185 27 -7 -7 -9 264.732 105.706 22 7 7 9 252.916 73.3074 21 7 7 10 2136.58 198.137 27 -7 -7 -10 2297.61 270.999 22 7 7 10 2212.54 195.695 21 -7 -7 -11 2549.80 296.288 22 7 7 11 2986.37 226.572 21 -7 -7 -12 0.34540 105.863 22 7 7 12 15.3572 51.2410 21 -7 -7 -13 1723.11 250.958 22 7 7 13 2145.63 194.928 21 -7 -7 -14 735.799 177.619 22 7 7 14 801.311 122.625 21 -7 -7 -15 167.768 115.377 22 7 7 15 347.233 94.6776 21 -7 -7 -16 716.649 180.126 22 7 7 16 515.539 102.402 21 -7 -7 -17 290.806 129.131 22 7 7 17 181.379 78.2065 21 -7 -7 -18 13.5189 84.6585 22 7 7 18 70.2718 60.5845 21 -7 -7 -19 1794.67 221.462 22 7 7 19 2073.43 164.442 21 -7 -7 -20 480.367 116.126 22 7 7 20 637.296 88.1502 21 -7 -8 17 164.692 54.7596 24 -7 -8 16 519.675 85.7487 29 -7 -8 16 462.887 85.7043 24 -7 -8 15 457.070 94.5325 29 -7 -8 15 305.650 76.6723 24 -7 -8 14 507.429 104.844 29 -7 -8 14 670.379 111.949 24 -7 -8 13 232.382 84.3651 29 -7 -8 13 236.682 93.1563 33 -7 -8 13 330.694 89.2712 24 -7 -8 12 154.220 84.2208 29 -7 -8 12 164.380 90.5764 33 -7 -8 12 234.432 79.7322 24 -7 -8 11 360.965 106.241 33 -7 -8 11 514.035 118.424 29 -7 -8 11 362.719 98.5925 24 -7 -8 10 11.8459 64.2882 29 -7 -8 10 57.7352 78.6809 33 -7 -8 10 16.6044 50.3989 23 -7 -8 10 50.1530 53.7966 24 -7 -8 9 1501.63 183.697 29 -7 -8 9 1464.07 193.069 33 -7 -8 9 1614.67 182.260 24 -7 -8 9 1442.98 166.257 23 -7 -8 8 2908.34 250.102 29 -7 -8 8 3064.00 266.017 33 -7 -8 8 3046.63 246.701 24 -7 -8 8 2631.41 218.613 23 -7 -8 7-10.9944 67.6785 29 -7 -8 7 53.4973 55.8304 23 -7 -8 7-12.2605 44.9867 24 -7 -8 6 3760.36 276.297 29 -7 -8 6 3912.99 277.905 24 -7 -8 6 3892.64 261.721 23 -7 -8 5 23.8510 57.4784 29 -7 -8 5 118.665 64.0104 23 -7 -8 5 123.622 79.5211 24 -7 -8 4 477.004 110.704 29 -7 -8 4 521.934 111.936 23 -7 -8 4 266.072 80.2034 24 -7 -8 3 2003.63 198.858 29 -7 -8 3 2359.70 210.469 23 -7 -8 2 13245.3 1035.38 7 -7 -8 2 14655.7 504.041 23 -7 -8 1 750.675 129.552 23 -7 -8 1 310.354 199.420 7 7 8 0 1124.96 315.313 1 -7 -8 0 949.176 246.919 7 -7 -8 -1 9834.74 906.820 7 7 8 1 11176.3 960.048 1 -7 -8 -2 10087.0 941.330 7 7 8 2 9638.26 892.113 1 -7 -8 -3 4185.69 610.126 7 -7 -8 -4 2975.74 521.508 7 -7 -8 -5 1781.39 179.990 23 7 8 6 485.420 92.5850 27 -7 -8 -6 418.025 93.5389 23 7 8 6 516.708 96.9249 21 7 8 7 1116.39 136.238 27 -7 -8 -7 1047.12 137.598 23 -7 -8 -7 1123.65 184.121 22 7 8 7 1315.69 151.084 21 -7 -8 -8 691.828 111.096 32 -7 -8 -8 707.153 154.510 22 7 8 8 971.235 131.439 21 -7 -8 -9 3303.23 324.183 22 7 8 9 3035.25 226.078 21 -7 -8 -10 663.093 163.437 22 7 8 10 516.381 98.1360 21 -7 -8 -11 589.962 163.563 22 7 8 11 741.983 120.807 21 -7 -8 -12 1519.36 225.328 22 7 8 12 1452.50 159.363 21 -7 -8 -13 210.179 117.701 22 7 8 13 278.466 73.4250 21 -7 -8 -14 65.0400 94.4516 22 7 8 14 39.0611 50.4921 21 -7 -8 -15 759.115 170.927 22 7 8 15 689.376 115.122 21 -7 -8 -16-14.1094 95.8376 22 7 8 16 2.81621 48.5155 21 7 8 17 21.1285 46.7789 25 -7 -8 -17-12.0684 99.3643 22 7 8 17-49.0352 60.9378 21 7 8 18 160.242 53.0304 25 -7 -8 -18 79.2302 82.3527 22 7 8 18 149.285 59.4148 21 7 8 19 1066.14 115.361 21 7 8 20 1559.17 125.230 21 -7 -9 16 46.9592 42.0163 24 -7 -9 15 342.920 70.8339 24 -7 -9 14 135.666 59.2814 24 -7 -9 13 197.202 80.6648 29 -7 -9 13 43.2222 55.1064 24 -7 -9 12 149.137 78.7695 29 -7 -9 12 24.4986 50.0528 24 -7 -9 11 8.45765 59.4423 29 -7 -9 11-49.4758 63.0241 24 -7 -9 10 106.053 78.1466 29 -7 -9 10-27.0718 62.0050 24 -7 -9 9 2892.08 242.021 29 -7 -9 9 2713.09 233.005 24 -7 -9 8 174.302 82.4699 29 -7 -9 8 95.2245 59.1761 23 -7 -9 8 111.505 63.5887 24 -7 -9 7 1054.75 160.722 29 -7 -9 7 913.653 131.285 23 -7 -9 7 1054.70 160.248 24 -7 -9 6 4236.12 298.514 29 -7 -9 6 4179.57 293.922 24 -7 -9 6 4180.06 271.148 23 -7 -9 5 1559.73 185.543 29 -7 -9 5 1576.33 170.883 32 -7 -9 5 1586.06 184.725 24 -7 -9 5 1638.04 179.290 23 -7 -9 4 4124.41 293.125 29 -7 -9 4 4489.67 285.689 32 -7 -9 4 4482.40 306.602 24 -7 -9 4 4158.39 281.561 23 -7 -9 3 5380.71 335.394 29 -7 -9 3 6167.70 335.629 32 -7 -9 3 5853.87 328.941 23 -7 -9 2 174.630 76.9403 29 -7 -9 2 217.206 82.0339 32 -7 -9 2 206.245 84.2185 23 -7 -9 1 1342.21 172.384 29 -7 -9 1 1199.28 153.425 32 -7 -9 1 1501.34 177.068 23 -7 -9 0 14158.8 508.111 32 -7 -9 0 13995.3 507.735 23 -7 -9 -1 94.8513 61.9263 32 -7 -9 -1 164.930 78.5981 23 -7 -9 -2 370.522 93.5309 32 -7 -9 -2 481.257 112.617 23 -7 -9 -3 798.536 129.680 32 -7 -9 -3 773.993 127.148 23 -7 -9 -4 1832.46 189.031 32 -7 -9 -4 1352.26 165.489 23 -7 -9 -5 3447.58 255.844 32 -7 -9 -5 3374.68 254.929 23 -7 -9 -6 7530.65 375.892 32 -7 -9 -6 6328.73 347.299 23 -7 -9 -7 539.265 109.660 32 7 9 7 680.404 110.062 21 -7 -9 -8 504.351 110.110 32 7 9 8 544.557 98.9032 21 -7 -9 -9 6644.70 342.732 32 7 9 9 7791.84 356.595 21 7 9 10 6369.71 327.203 21 7 9 11 3331.41 240.693 21 7 9 12 162.467 66.3458 21 7 9 13 801.930 121.883 21 7 9 14 254.678 80.4329 21 7 9 15 512.314 94.8829 21 7 9 16 1642.67 155.597 25 7 9 16 1624.64 161.621 21 7 9 17 283.002 70.4100 25 7 9 17 318.936 76.8292 21 7 9 18 277.318 65.8396 25 7 9 18 146.125 56.3711 21 7 9 19 2311.06 141.718 25 7 9 19 2484.55 162.155 21 -7 -10 14 109.291 53.2560 24 -7 -10 13 49.2444 42.7440 24 -7 -10 12 22.3774 43.5399 24 -7 -10 11 29.7438 51.6042 24 -7 -10 10 674.267 118.673 24 -7 -10 9 1010.54 140.159 24 -7 -10 8 551.557 111.682 24 -7 -10 7 94.4067 59.8107 24 -7 -10 6 39.2270 62.6618 23 -7 -10 6 80.4696 81.3347 24 -7 -10 5 3240.28 240.382 32 -7 -10 5 2878.24 249.820 24 -7 -10 5 3480.56 251.441 23 -7 -10 4 1959.96 189.714 32 -7 -10 4 2052.88 213.006 24 -7 -10 4 1849.90 188.678 23 -7 -10 3-15.0020 53.9860 32 -7 -10 3 88.9566 70.8921 24 -7 -10 2 1106.76 147.299 32 -7 -10 2 1053.17 148.155 23 -7 -10 1 1139.14 158.209 32 -7 -10 1 943.622 149.961 23 -7 -10 0 15097.7 532.809 32 -7 -10 0 14509.2 528.815 23 -7 -10 -1 3583.54 269.178 32 -7 -10 -1 3854.71 283.483 23 -7 -10 -2 12944.9 494.873 32 -7 -10 -2 12676.7 502.935 23 -7 -10 -3 10532.0 447.696 32 -7 -10 -3 10812.4 463.409 23 -7 -10 -4 3383.50 261.072 32 -7 -10 -4 2676.56 235.565 23 -7 -10 -5 9071.95 418.774 32 -7 -10 -6 4530.52 298.968 32 -7 -10 -7 338.268 89.8914 32 -7 -10 -8 1049.59 143.303 32 -7 -10 -9 155.935 68.2404 32 7 10 9 19.2427 38.9859 21 -7 -10 -10 1684.17 172.844 32 7 10 10 1950.38 175.495 21 7 10 11 2013.55 181.831 21 7 10 12 1080.15 135.669 21 7 10 13 290.531 77.4722 21 7 10 14 1282.87 148.047 25 7 10 14 1472.14 151.284 21 7 10 15 113.507 63.7849 25 7 10 15-0.78980 44.9827 21 7 10 16 1153.49 127.502 25 7 10 16 842.042 109.186 21 7 10 17 15.0674 43.2349 25 7 10 17 68.6390 49.3272 21 7 10 18 1195.88 111.680 25 7 10 18 1270.00 116.014 21 -7 -11 12-32.0666 44.6911 24 -7 -11 11 53.8101 44.8604 24 -7 -11 10 220.405 74.4935 24 -7 -11 9-14.9368 45.0284 24 -7 -11 8 1078.68 142.811 24 -7 -11 7 289.970 83.6059 24 -7 -11 6 926.325 137.680 24 -7 -11 5 2701.53 233.611 24 -7 -11 5 2555.54 204.765 23 -7 -11 4 1126.74 143.496 32 -7 -11 4 1086.21 145.624 23 -7 -11 4 1073.69 153.478 24 -7 -11 3 693.296 113.226 32 -7 -11 3 668.252 118.763 23 -7 -11 3 546.750 114.435 24 -7 -11 2 5152.22 307.664 32 -7 -11 2 5061.62 328.647 24 -7 -11 2 5159.77 307.988 23 -7 -11 1 832.173 131.075 32 -7 -11 1 689.706 131.433 23 -7 -11 0 329.860 101.718 32 -7 -11 0 124.919 66.3191 23 -7 -11 -1 1424.00 170.687 32 -7 -11 -1 1492.80 176.451 23 -7 -11 -2 5294.90 319.821 32 -7 -11 -3 6693.02 359.082 32 -7 -11 -4 1064.46 144.804 32 -7 -11 -5 1541.88 176.938 32 -7 -11 -6 148.140 74.4173 32 -7 -11 -7 569.953 110.555 32 -7 -11 -8 663.506 116.875 32 -7 -11 -9 518.973 101.720 32 7 11 9 512.743 95.3076 25 7 11 10 59.6333 53.0002 25 -7 -11 -10 103.893 53.4404 32 7 11 11-41.1896 53.6563 25 7 11 12 117.317 48.8538 25 7 11 12 152.852 50.6354 21 7 11 13 214.570 64.9347 25 7 11 13 303.096 66.6445 21 7 11 14 577.038 96.3811 25 7 11 14 666.898 99.4024 21 7 11 15 2627.88 183.692 25 7 11 15 2657.60 175.370 21 7 11 16 48.7265 42.8194 25 7 11 16-17.2314 37.7127 21 7 11 17 21.4739 34.6253 25 7 11 17 50.9498 41.7457 21 -7 -12 10 20.9286 33.3656 24 -7 -12 9 1027.95 113.745 24 -7 -12 8-0.14654 42.9011 24 -7 -12 7 661.887 108.723 24 -7 -12 6 258.873 78.0386 24 -7 -12 5 150.773 64.3459 24 -7 -12 4 764.130 108.920 32 -7 -12 4 839.555 114.350 28 -7 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51.1749 32 -7 -13 2 25.4161 37.9615 28 -7 -13 2 49.6606 48.7758 24 -7 -13 1 56.4489 46.7605 32 -7 -13 1 49.8977 45.7180 28 -7 -13 1 22.8573 47.1351 24 -7 -13 0 230.529 63.5373 32 -7 -13 0 283.258 77.1220 24 -7 -13 -1 698.631 103.559 32 -7 -13 -1 883.656 129.674 24 -7 -13 -2 72.8869 61.9031 32 -7 -13 -2 39.9914 56.7016 24 -7 -13 -3 77.2430 54.1022 32 -7 -13 -4 1288.36 144.051 32 -7 -13 -5 873.697 122.128 32 -7 -13 -6 1688.10 159.150 32 -7 -13 -7 99.0461 48.4620 32 -7 -13 -8 107.480 55.8411 32 -7 -13 -9 118.793 54.0698 32 -7 -13 -10 32.8464 31.2038 32 7 13 10 98.7032 39.3302 25 7 13 11 4.99656 34.1451 25 7 13 12-34.5904 30.7848 25 -7 -14 0 86.8652 40.5001 32 -7 -14 0 180.907 53.4196 28 -7 -14 0 213.499 55.6005 24 -7 -14 -1 150.681 51.5706 32 -7 -14 -1 129.994 53.0146 28 -7 -14 -1 139.324 47.9639 24 -7 -14 -2 472.539 72.7068 32 -7 -14 -2 577.310 84.5941 28 -7 -14 -2 436.745 78.3500 24 -7 -14 -3 250.887 58.7956 32 -7 -14 -3 190.326 56.3797 28 -7 -14 -3 224.190 61.1648 24 -7 -14 -4-11.8232 40.9259 32 -7 -14 -4 113.867 50.2715 28 -7 -14 -4 38.8990 45.3537 24 -7 -14 -5-8.71550 40.3760 32 -7 -14 -5 147.912 54.9607 24 -7 -14 -6 1049.55 109.294 32 -7 -14 -6 1043.82 112.050 24 -7 -14 -7 45.5506 34.3197 32 8 -6 -7-20.6173 34.3685 34 -8 6 7 5.65552 33.4043 30 8 -6 -6 1059.52 108.877 34 -8 6 6 931.400 96.7928 30 8 -6 -5-18.6072 35.6099 34 -8 6 5 77.5595 39.5258 30 8 -6 -4 541.658 85.3884 34 -8 6 4 638.717 80.5125 30 8 -6 -3 31.1264 36.8487 34 8 -6 -2 59.3183 48.1332 34 8 -6 -1 322.395 71.6804 34 8 -6 0 74.0885 42.0891 34 8 -6 1 67.2093 45.1415 34 -8 5 12 52.6049 43.0920 26 -8 5 11 137.824 54.9164 26 -8 5 10 34.9934 36.3339 26 8 -5 -9 670.562 89.5441 34 -8 5 9 906.843 108.084 26 -8 5 9 828.296 106.685 30 8 -5 -8 35.3443 38.7757 34 -8 5 8-58.6870 47.3109 26 -8 5 8 54.8128 38.6488 30 8 -5 -7 116.831 61.0863 34 -8 5 7 90.7723 51.1029 30 8 -5 -6 933.116 123.031 34 -8 5 6 1049.79 124.901 30 8 -5 -5 334.366 87.6135 34 -8 5 5 305.235 70.5670 30 8 -5 -4 119.845 58.5226 34 -8 5 4 86.0957 47.1973 30 8 -5 -3 31.2665 47.8802 34 8 -5 -2 679.117 107.206 34 8 -5 -1 112.666 58.5372 34 8 -5 0 88.3396 60.9968 34 8 -5 1 907.754 117.982 34 8 -5 2 136.391 56.4668 34 8 -5 3 229.838 67.8928 34 8 -5 4 217.335 61.4550 34 8 -5 5 41.5759 44.4333 34 8 -5 6 276.181 58.4717 34 8 -5 6 276.665 56.9223 28 -8 4 14 34.6283 38.2884 26 -8 4 13 391.288 75.8963 26 -8 4 12 434.892 86.6896 26 -8 4 11 446.066 92.1601 26 -8 4 10 2517.61 199.410 26 -8 4 10 2163.94 183.958 30 -8 4 9 1287.04 147.125 26 -8 4 9 1276.59 147.932 30 8 -4 -8 594.242 98.2711 34 -8 4 8 634.938 110.379 26 -8 4 8 516.971 103.342 30 8 -4 -7 1366.42 151.502 34 -8 4 7 1313.27 147.059 26 -8 4 7 1293.49 150.206 30 8 -4 -6 354.085 79.7535 34 -8 4 6 583.979 105.644 26 -8 4 6 374.911 84.7313 30 8 -4 -5 54.9169 62.0372 34 -8 4 5-43.7758 53.2104 26 -8 4 5 31.5373 45.0640 30 8 -4 -4 1425.81 160.209 34 -8 4 4 1251.28 140.721 30 8 -4 -3 728.729 118.310 34 -8 4 3 698.992 105.124 30 8 -4 -2 90.8231 56.6528 34 8 -4 -1 75.8893 62.9283 34 8 -4 0 1865.32 185.095 34 8 -4 1 34.4133 52.8793 34 8 -4 2 1678.08 172.830 34 8 -4 3-61.2678 64.5749 34 8 -4 4 2420.53 196.051 34 8 -4 5 468.059 91.5918 34 8 -4 5 383.222 78.3732 28 8 -4 6 59.4479 48.3942 34 8 -4 6 70.8271 49.3664 28 8 -4 7 1198.92 122.413 34 8 -4 7 1009.99 116.099 28 8 -4 8 146.400 53.1816 34 8 -4 8 57.0592 45.8106 28 8 -4 9 87.0935 46.4205 28 8 -4 10-43.0255 30.3308 28 -8 3 16 33.4500 44.7370 26 -8 3 15-64.7949 55.2277 26 -8 3 14 63.9531 54.7706 26 -8 3 13 1195.58 140.641 26 -8 3 12 69.3297 60.0578 26 -8 3 11 71.3711 52.5220 26 -8 3 10 554.852 108.607 30 -8 3 10 663.786 112.997 26 -8 3 9 777.876 126.957 26 -8 3 9 693.531 116.538 30 -8 3 8 26.5491 54.6258 26 -8 3 8 13.1413 51.8681 30 8 -3 -7 33.5082 47.1607 34 -8 3 7-2.02423 56.4859 26 -8 3 7-45.9743 55.4843 30 8 -3 -6 14.3414 48.0887 34 -8 3 6-1.22975 55.9960 26 -8 3 6-24.6279 44.8388 30 8 -3 -5 2479.87 215.597 34 -8 3 5 2535.06 220.776 26 -8 3 5 2491.03 209.601 30 8 -3 -4 8371.71 395.036 34 -8 3 4 8682.12 400.661 26 -8 3 4 8462.49 372.604 30 8 -3 -3 20.5307 56.0429 34 -8 3 3 31.2050 44.0500 26 8 -3 -2 2553.11 224.659 34 -8 3 2 2604.46 220.247 26 8 -3 -1 517.257 106.406 34 8 -3 0 1858.15 192.466 34 8 -3 1 1159.71 153.050 34 8 -3 2-78.8008 61.2449 34 8 -3 3 1875.10 188.729 34 8 -3 4 59.5648 51.4590 34 8 -3 4 79.3412 52.7483 28 8 -3 5 1178.13 151.051 34 8 -3 5 1513.72 159.254 28 8 -3 6 1524.88 160.627 34 8 -3 6 1501.70 156.343 28 8 -3 7 16.7166 49.3477 34 8 -3 7 32.0591 53.0354 28 8 -3 8 49.2717 47.1380 34 8 -3 8 14.0328 50.4077 28 8 -3 9 86.5021 45.3687 34 8 -3 9 28.3444 44.7171 28 8 -3 10 1019.42 105.151 34 8 -3 10 1155.39 126.216 28 8 -3 11 354.095 75.8763 28 8 -3 12 575.565 83.1162 28 -8 2 17 48.2223 41.4964 29 -8 2 17 125.994 52.4234 26 -8 2 16 386.291 84.7243 26 -8 2 15 8.17360 51.2126 26 -8 2 14 126.582 70.1166 26 -8 2 13-20.2906 57.9996 26 -8 2 12 707.515 124.240 26 -8 2 11 873.541 130.177 26 -8 2 10 49.0876 62.1628 26 -8 2 9 371.046 98.8928 26 -8 2 9 365.793 91.0397 30 -8 2 8 497.075 104.538 30 -8 2 8 320.502 87.9858 26 -8 2 7 355.597 97.3641 26 -8 2 7 222.275 70.6006 30 8 -2 -6 7018.13 347.886 34 -8 2 6 7637.13 379.282 26 -8 2 6 7483.05 361.828 30 8 -2 -5 395.581 101.964 34 -8 2 5 331.220 92.0066 26 -8 2 5 444.157 98.3824 30 8 -2 -4 502.162 103.202 34 -8 2 4 457.723 102.481 26 -8 2 4 737.262 117.588 30 8 -2 -3 140.585 67.2649 34 -8 2 3 179.745 81.5715 26 8 -2 -2 2403.53 216.575 34 -8 2 2 2688.56 233.926 26 8 -2 -1 2748.66 230.949 34 -8 2 1 2826.38 244.304 26 8 -2 0 4.67701 52.6869 34 -8 2 0 137.553 77.9485 26 8 -2 1 1774.88 184.845 34 8 -2 2 302.954 79.8255 34 8 -2 3 716.876 122.427 34 8 -2 4 1154.10 154.396 34 8 -2 4 1053.32 134.274 28 8 -2 5-2.60740 50.7841 34 8 -2 5 53.0485 41.8481 28 8 -2 6 4.90160 64.3420 34 8 -2 6 90.4419 58.1170 28 8 -2 7 1382.08 160.547 28 8 -2 7 1580.34 167.209 34 8 -2 8 39.7924 49.8786 34 8 -2 8 1.84047 50.6183 28 8 -2 9 320.057 80.7114 34 8 -2 9 310.727 78.5628 28 8 -2 10 626.026 96.6165 34 8 -2 10 578.314 104.550 28 8 -2 11 215.718 62.0860 34 8 -2 11 108.417 66.0589 28 8 -2 11 158.925 52.1774 31 8 -2 12 426.230 84.9951 28 8 -2 12 322.058 71.2481 31 8 -2 13 155.385 56.9153 28 8 -2 13 100.358 38.0696 31 8 -2 14 626.339 81.3202 28 8 -2 14 799.391 88.2857 31 -8 1 18 60.4343 52.5399 29 -8 1 18 98.1637 50.2682 26 -8 1 17-11.8712 54.1099 29 -8 1 17 45.9435 50.2551 26 -8 1 16 223.034 70.2059 26 -8 1 15 223.434 72.0107 26 -8 1 14 388.531 93.5080 26 -8 1 13-59.4419 73.3067 26 -8 1 12 205.553 79.3422 26 -8 1 11 1175.87 148.249 26 -8 1 10 59.7285 61.0508 26 -8 1 9 2375.82 210.919 26 -8 1 9 2216.05 205.163 30 -8 1 8 2367.00 210.716 26 -8 1 8 2150.67 202.630 30 -8 1 7 438.544 98.8441 30 -8 1 7 547.755 109.696 26 -8 1 6 6180.26 338.323 26 -8 1 6 6180.97 327.827 30 8 -1 -5 141.711 66.2252 34 -8 1 5 161.776 78.0386 26 -8 1 5 285.636 76.8483 30 8 -1 -4-8.14527 45.2015 34 -8 1 4 14.2860 57.8512 26 8 -1 -3 1357.93 157.895 34 -8 1 3 1231.56 162.746 26 8 -1 -2 8058.24 385.856 34 -8 1 2 8135.06 400.531 26 8 -1 -1-87.0964 68.7124 34 -8 1 1-0.67411 54.9932 26 8 -1 0 3752.50 263.689 34 -8 1 0 3546.58 273.719 26 8 -1 1 2693.03 225.945 34 -8 1 -1 2751.58 247.972 26 8 -1 2 18559.1 580.385 34 -8 1 -2 16679.8 603.389 26 8 -1 3 12357.3 476.448 34 8 -1 4 2728.37 226.137 34 8 -1 4 2341.20 196.662 28 8 -1 5 152.988 70.9346 34 8 -1 5 147.325 67.3005 28 8 -1 6 57.2241 52.8528 34 8 -1 6 206.970 77.3360 28 8 -1 7 1598.04 173.594 34 8 -1 7 1690.03 177.434 28 8 -1 8 1331.81 154.642 34 8 -1 8 1616.80 171.768 28 8 -1 9-55.6661 55.3166 34 8 -1 9 108.947 69.9420 28 8 -1 9-50.9539 55.0648 31 8 -1 10 34.0456 47.8632 34 8 -1 10-56.2214 50.6041 28 8 -1 10-101.842 57.8278 31 8 -1 11 44.0434 41.4327 34 8 -1 11 71.1089 59.8812 28 8 -1 11 6.49671 43.5417 31 8 -1 12 44.6221 45.3529 34 8 -1 12 42.7591 56.8198 28 8 -1 12 48.8239 48.8535 31 8 -1 13 288.250 78.2420 28 8 -1 13 327.370 76.8536 31 8 -1 14 86.3042 53.1775 28 8 -1 14 67.8948 45.9616 31 8 -1 15 130.148 47.3726 31 -8 0 19 310.069 71.8462 29 -8 0 18 49.8423 45.5396 29 -8 0 17 682.302 113.649 29 -8 0 17 797.253 103.880 26 -8 0 16 695.529 116.722 29 -8 0 16 759.472 111.617 26 -8 0 15 74.1405 60.5545 26 -8 0 14 2573.93 203.425 26 -8 0 13 2360.31 201.624 26 -8 0 12 280.461 77.3440 26 -8 0 11 489.072 100.916 26 -8 0 10 32.2298 59.8782 26 -8 0 9 365.690 94.7765 26 -8 0 8 1822.94 182.849 26 -8 0 7 3992.91 267.784 26 -8 0 7 3848.31 261.319 30 -8 0 6 26623.4 676.465 26 -8 0 6 25715.3 652.964 30 -8 0 5 147.372 76.6662 26 -8 0 5-7.15194 43.5565 30 -8 0 4 5523.42 319.307 26 8 0 -3 2607.19 213.338 34 -8 0 3 2937.09 236.046 26 8 0 -2 473.905 96.9555 34 -8 0 2 572.055 118.130 26 8 0 -1 1428.40 163.506 34 -8 0 1 1537.98 183.915 26 8 0 0 10286.5 424.199 34 -8 0 0 9191.42 428.451 26 8 0 1 295.568 77.7610 34 -8 0 -1 241.311 84.8207 26 -8 0 -2 2157.98 220.797 26 8 0 2 1995.43 191.407 34 8 0 3 2123.56 197.494 34 -8 0 -3 2039.23 220.812 26 8 0 4 6784.85 350.244 34 -8 0 -4 6012.62 375.521 26 8 0 4 6398.34 314.533 28 8 0 5 6281.86 336.684 34 8 0 5 5575.06 305.148 28 8 0 6 769.949 129.219 34 8 0 6 842.795 127.971 28 8 0 7 142.427 65.1798 34 8 0 7 228.448 78.0765 28 8 0 8 123.447 66.4450 34 8 0 8 71.3876 64.4224 28 8 0 9 446.574 96.9466 34 8 0 9 386.854 99.3119 28 8 0 9 339.177 83.8183 31 8 0 10 60.5976 55.4397 34 8 0 10 111.084 71.5419 28 8 0 10 73.7017 66.8765 31 8 0 11 23.1837 47.1266 34 8 0 11 66.7064 63.6871 28 8 0 11-71.1842 66.5714 31 8 0 12 290.218 80.9991 34 8 0 12 225.149 74.5287 28 8 0 12 270.075 77.4251 31 8 0 13 165.180 62.2035 34 8 0 13 162.440 71.1740 28 8 0 13 106.101 59.3743 31 8 0 14 2991.01 204.698 28 8 0 14 3125.35 229.004 31 8 0 15 328.547 76.6202 31 8 0 16 477.039 87.4363 31 8 0 17 38.8025 36.1319 31 -8 -1 19 1806.43 153.722 29 -8 -1 19 1562.37 134.219 33 -8 -1 18 537.853 101.824 29 -8 -1 18 339.875 75.0000 33 -8 -1 17 65.4808 63.1279 29 -8 -1 17-73.3453 57.9590 33 -8 -1 16 231.129 82.8480 29 -8 -1 16 141.519 63.5899 33 -8 -1 15 380.740 99.9997 29 -8 -1 15 434.100 92.1493 26 -8 -1 14 254.767 75.6157 26 -8 -1 13 406.127 93.3582 26 -8 -1 12 766.869 123.596 26 -8 -1 11 5532.84 301.705 26 -8 -1 10 206.397 77.9304 26 -8 -1 9 131.812 62.5907 26 -8 -1 8 2181.69 195.021 26 -8 -1 7 2937.03 223.451 26 -8 -1 6 5849.15 310.697 26 -8 -1 5 2225.16 195.511 26 -8 -1 5 2125.68 432.957 17 -8 -1 4 4999.43 292.719 26 -8 -1 4 5664.90 691.936 17 -8 -1 3 10824.2 965.436 17 8 1 -3 10665.3 1154.28 8 8 1 -2 152.047 194.874 8 8 1 -1 2571.40 528.857 8 8 1 0 1819.96 435.683 8 8 1 1 1095.27 383.112 8 -8 -1 -2 7975.00 734.904 6 8 1 2 8118.04 865.963 8 8 1 3 8918.91 391.217 34 -8 -1 -3 8060.89 411.909 26 -8 -1 -3 9401.24 810.662 6 8 1 4 125.286 61.5538 34 8 1 4 161.822 61.4599 28 -8 -1 -4-23.1161 65.5088 26 8 1 5 5415.16 308.972 34 -8 -1 -5 4653.01 328.548 26 8 1 5 5322.09 289.076 28 8 1 6 11962.2 459.946 34 8 1 6 11137.2 430.244 28 8 1 7 719.123 121.905 34 8 1 7 1057.43 144.356 28 8 1 8 9409.10 409.965 34 8 1 8 8593.19 393.476 28 8 1 9 167.600 74.8788 34 8 1 9 160.624 71.8129 28 8 1 10 4150.30 271.200 34 8 1 10 3679.86 258.744 28 8 1 11 412.296 100.613 34 8 1 11 375.513 92.1132 28 8 1 11 387.387 96.4877 31 8 1 12 206.757 80.6638 34 8 1 12 184.122 71.6292 28 8 1 12 144.931 70.7812 31 8 1 13 67.4562 53.1933 34 8 1 13 61.4960 54.5794 28 8 1 13 86.8596 63.9770 31 8 1 14 2587.30 193.172 34 8 1 14 2601.40 221.871 31 8 1 15 18.1530 48.9649 31 8 1 16 180.329 70.7111 31 8 1 17 717.569 103.086 31 8 1 18 1410.77 124.709 31 -8 -1 -18 1778.07 196.929 22 -8 -2 20 10.2034 39.1443 29 -8 -2 20-24.4230 39.3883 33 -8 -2 19 1123.19 123.231 29 -8 -2 19 1333.75 135.898 33 -8 -2 18 71.7122 49.9906 29 -8 -2 18 116.892 59.5211 33 -8 -2 17 44.7281 56.2405 29 -8 -2 17-69.4817 69.4967 33 -8 -2 16 32.6298 61.6214 29 -8 -2 16 76.1198 63.6233 33 -8 -2 15 934.354 137.542 29 -8 -2 15 1001.73 137.906 33 -8 -2 14 388.265 100.277 29 -8 -2 14 340.297 93.8256 33 -8 -2 13 1534.38 179.465 29 -8 -2 13 1548.83 173.497 33 -8 -2 12 9138.85 379.240 26 -8 -2 11 214.243 77.4566 26 -8 -2 10 1249.50 146.263 26 -8 -2 9 31.8170 52.9064 26 -8 -2 8 8494.86 362.801 26 -8 -2 7 3452.12 233.455 26 -8 -2 6 546.272 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2649.26 207.309 34 8 2 14 2430.53 215.899 31 8 2 15-22.9982 45.0095 34 8 2 15 57.0116 53.6680 31 8 2 16 23.9943 48.1167 31 8 2 17 191.265 70.5448 31 8 2 18 143.699 53.2214 31 -8 -2 -18 453.460 146.072 22 -8 -3 19 75.8855 48.3912 29 -8 -3 19-21.3457 45.4415 33 -8 -3 18 118.831 61.3016 29 -8 -3 18 102.835 63.5984 33 -8 -3 17 256.118 82.0716 29 -8 -3 17 120.096 65.8302 33 -8 -3 16 2812.32 227.782 29 -8 -3 16 2542.40 215.082 33 -8 -3 15 35.0316 61.3004 29 -8 -3 15-15.2141 65.8509 33 -8 -3 14 593.497 120.112 29 -8 -3 14 486.575 106.028 33 -8 -3 13 856.315 136.782 29 -8 -3 13 958.018 140.226 33 -8 -3 12 1248.73 165.262 29 -8 -3 12 1439.36 170.021 33 -8 -3 11 7952.10 393.855 29 -8 -3 11 8350.10 392.171 33 -8 -3 10 1437.11 171.712 29 -8 -3 10 1348.49 159.520 33 -8 -3 9 184.787 69.4801 29 -8 -3 8 1822.40 181.164 29 -8 -3 8 1471.26 152.186 26 -8 -3 7 1131.05 142.042 29 -8 -3 7 1095.53 133.343 26 8 3 -6 11591.0 1073.06 12 -8 -3 6 10307.2 959.201 17 8 3 -6 9381.35 1148.79 8 -8 -3 5 22.4769 67.8038 17 8 3 -5 122.849 207.590 8 -8 -3 4 589.985 234.200 17 8 3 -4 1426.96 469.896 8 -8 -3 3 177.636 146.523 17 8 3 -3 541.697 282.448 8 8 3 -2 396.102 262.788 8 8 3 -1 9471.71 1007.35 8 8 3 0 100.231 214.426 8 -8 -3 -1 813.298 224.983 6 8 3 1 539.840 272.781 8 -8 -3 -2 1320.30 289.682 6 8 3 2 984.989 308.927 8 -8 -3 -3 10057.9 808.151 6 8 3 3 9982.62 936.313 8 -8 -3 -4 5000.00 586.436 6 8 3 4 3806.00 548.678 19 8 3 4 5664.74 690.291 8 -8 -3 -5 6187.10 661.264 6 8 3 5 6458.02 727.503 19 8 3 6 3801.49 253.402 34 -8 -3 -6 3437.20 265.617 26 8 3 6 3002.87 499.065 19 8 3 7 3584.79 249.307 34 -8 -3 -7 2742.17 246.561 26 8 3 7 3174.02 226.165 28 8 3 7 3503.66 240.696 21 8 3 8 19599.9 581.767 34 8 3 8 17584.9 541.987 28 8 3 9 1975.22 194.154 34 8 3 9 1878.94 185.253 28 8 3 9 2140.14 190.413 27 8 3 9 2012.19 180.834 21 8 3 10 15327.6 525.789 34 8 3 10 15853.1 499.302 27 8 3 10 16221.1 504.773 21 8 3 11 4681.09 293.798 34 8 3 11 4598.77 269.368 21 8 3 12 9137.97 404.107 34 8 3 13 3962.38 265.874 34 8 3 14 1194.74 144.767 34 8 3 14 1155.47 152.436 31 8 3 15 25.6622 52.6880 31 8 3 16 339.050 91.9011 31 8 3 17 1537.20 157.305 31 8 3 18 1046.86 121.988 31 -8 -3 -18 1003.75 180.683 22 8 3 19 445.955 74.2634 31 -8 -3 -19 678.744 144.328 22 -8 -4 19 916.419 109.755 29 -8 -4 19 970.517 120.681 33 -8 -4 18-22.7957 59.5194 29 -8 -4 18-9.46371 62.2643 33 -8 -4 17 160.301 69.5574 29 -8 -4 17 90.0931 62.5196 33 -8 -4 16 294.096 94.6051 29 -8 -4 16 135.044 71.4423 33 -8 -4 15 349.845 99.3552 29 -8 -4 15-101.975 91.4145 33 -8 -4 14 142.232 80.9557 29 -8 -4 14-49.9019 77.7641 33 -8 -4 13 3352.43 257.237 29 -8 -4 13 2877.01 239.343 33 -8 -4 12 3.94174 61.6775 29 -8 -4 12-14.7296 57.1496 33 -8 -4 11 1761.26 188.041 29 -8 -4 11 1884.38 194.816 33 -8 -4 10 673.458 125.084 29 -8 -4 10 784.316 130.442 33 -8 -4 9 5328.29 315.123 29 -8 -4 9 5351.75 313.936 33 -8 -4 8 1033.09 141.919 29 -8 -4 8 601.803 114.710 33 -8 -4 7 344.306 81.9364 29 8 4 -6 59.2309 206.479 8 -8 -4 5 3124.13 561.426 17 8 4 -5 1538.86 456.737 8 -8 -4 4 5868.30 739.610 17 8 4 -4 5623.51 845.099 8 -8 -4 3 380.338 206.083 17 8 4 -3 341.333 252.263 8 8 4 -2 1498.02 464.005 8 8 4 -1 832.183 305.495 8 8 4 0 7694.09 860.441 8 8 4 1 2286.66 459.441 8 8 4 2 964.932 323.315 8 8 4 3 1679.16 388.356 19 8 4 3 537.268 193.489 8 8 4 4 2101.77 409.301 19 8 4 4 1938.33 423.008 8 -8 -4 -5 1627.86 357.070 6 8 4 5 2016.33 425.284 19 8 4 5 2068.07 410.262 8 -8 -4 -6 11811.7 926.688 6 8 4 6 13372.1 1037.21 19 8 4 6 12866.0 1030.83 8 8 4 7 1356.62 154.729 34 -8 -4 -7 1523.03 233.674 22 8 4 7 1319.08 150.477 21 8 4 8 335.186 90.4419 34 8 4 8 408.803 88.1179 27 8 4 8 343.120 98.7896 21 8 4 9 2642.98 221.268 34 8 4 9 2538.84 208.484 27 8 4 9 2538.32 208.174 21 8 4 10 121.211 56.1443 27 8 4 10 115.293 61.6245 34 8 4 10 127.926 63.2259 21 8 4 11 679.841 110.658 27 8 4 11 600.651 114.942 34 8 4 11 546.864 101.693 21 8 4 12 586.735 100.018 27 8 4 12 637.398 116.838 34 8 4 12 790.139 119.057 21 8 4 13 920.016 140.154 34 8 4 13 822.005 122.677 21 8 4 14 44.0726 47.4988 34 8 4 14 71.4326 51.7736 21 8 4 15 1387.31 166.011 31 8 4 15 1341.55 143.498 21 8 4 16-6.36932 43.0023 31 -8 -4 -16 292.620 145.022 22 8 4 17 1048.66 133.899 31 -8 -4 -17 1122.09 201.154 22 8 4 18 587.680 95.1360 31 -8 -4 -18 651.939 163.389 22 8 4 19-21.1041 32.6995 31 -8 -4 -19 9.98698 101.922 22 -8 -5 19 328.771 65.4763 29 -8 -5 19 308.069 77.8087 33 -8 -5 18 1278.52 132.836 29 -8 -5 18 1049.18 131.747 33 -8 -5 17 195.952 70.4530 29 -8 -5 17 332.154 95.1093 33 -8 -5 17 336.012 71.8628 23 -8 -5 16 1910.12 185.095 29 -8 -5 16 2127.96 198.298 33 -8 -5 15 1161.96 152.421 29 -8 -5 15 840.385 142.927 33 -8 -5 14 4.60856 55.6785 29 -8 -5 14-38.2796 57.7051 33 -8 -5 13 54.9818 63.2390 29 -8 -5 13 1.54220 69.5656 33 -8 -5 12 5235.36 319.997 29 -8 -5 12 5210.87 323.550 33 -8 -5 11 15610.3 549.859 29 -8 -5 11 16547.9 566.443 33 -8 -5 10 3208.67 251.914 29 -8 -5 10 2966.11 244.382 33 -8 -5 9 223.049 86.5709 29 -8 -5 9 64.1961 66.9195 33 -8 -5 8 295.594 85.5875 29 -8 -5 8 277.077 93.3050 33 -8 -5 7-24.2707 55.4155 29 -8 -5 7 106.270 78.8849 33 8 5 -6-375.970 256.370 8 -8 -5 5 6064.77 738.498 17 8 5 -5 7195.33 964.945 8 -8 -5 4 118.241 112.869 17 8 5 -4 266.477 224.263 8 -8 -5 3 6524.39 763.318 17 8 5 -3 7158.95 872.383 8 -8 -5 2 6314.35 754.373 17 8 5 -2 6621.53 821.277 8 8 5 -1 169.385 204.986 8 8 5 0-81.5121 209.239 8 8 5 0 112.674 101.284 1 8 5 1 2021.21 365.930 1 8 5 1 2092.89 434.160 8 8 5 2 10057.6 895.672 19 8 5 2 12085.6 997.064 8 8 5 2 11692.6 868.014 1 8 5 3 3790.76 554.846 19 8 5 3 3214.34 506.584 8 8 5 3 4067.83 526.511 1 8 5 4 2222.23 390.862 1 8 5 4 2396.87 435.789 19 8 5 4 3004.00 507.687 8 8 5 5 1198.22 295.513 1 8 5 5 1602.59 380.911 19 8 5 5 1833.77 380.222 8 8 5 6 3843.42 567.802 19 8 5 6 4075.16 582.554 8 8 5 7 1669.12 173.399 34 8 5 7 1672.42 168.549 27 -8 -5 -7 1759.57 232.573 22 8 5 7 1481.15 163.913 21 8 5 8-44.7573 47.7477 34 8 5 8-8.94013 50.6587 27 -8 -5 -8 138.150 118.754 22 8 5 8-24.1748 46.1781 21 8 5 9 519.369 100.553 27 8 5 9 382.603 98.1780 34 -8 -5 -9 658.797 178.450 22 8 5 9 558.670 108.702 21 8 5 10 3221.71 248.722 34 8 5 10 3589.69 245.934 27 -8 -5 -10 3191.86 326.237 22 8 5 10 3040.41 228.808 21 8 5 11 6600.74 351.788 34 8 5 11 6668.25 329.437 27 -8 -5 -11 6233.08 446.522 22 8 5 11 6358.44 324.416 21 8 5 12 1202.48 156.260 34 8 5 12 1169.51 138.565 27 -8 -5 -12 1053.32 210.205 22 8 5 12 1225.56 148.757 21 8 5 13 635.892 103.506 27 -8 -5 -13 1042.14 216.885 22 8 5 13 866.733 126.358 21 -8 -5 -14 720.174 194.908 22 8 5 14 654.148 108.004 21 8 5 15 305.776 83.9828 31 -8 -5 -15 170.053 137.182 22 8 5 15 122.671 66.0451 21 8 5 16 1723.79 175.884 31 -8 -5 -16 1554.77 246.876 22 8 5 16 1954.69 173.325 21 8 5 17 433.583 88.9444 31 -8 -5 -17 486.299 183.902 22 8 5 17 336.671 75.2516 21 8 5 18 392.087 76.7097 31 -8 -5 -18 487.956 153.344 22 8 5 18 572.036 85.9666 21 8 5 19 67.8798 41.0618 31 -8 -5 -19 209.147 111.306 22 -8 -5 -20-21.4000 75.3229 22 -8 -6 18 296.363 65.4475 29 -8 -6 18 403.480 89.4476 33 -8 -6 17 100.782 62.4406 29 -8 -6 17 92.2376 74.9274 33 -8 -6 16 2485.62 199.492 29 -8 -6 16 2355.84 214.117 33 -8 -6 15 7607.61 361.753 29 -8 -6 15 8048.03 388.095 33 -8 -6 15 7564.85 326.478 23 -8 -6 14-82.0952 66.7464 29 -8 -6 14 83.7553 77.7496 33 -8 -6 14 19.0451 56.4848 23 -8 -6 13 141.006 67.9358 29 -8 -6 13 109.323 76.0828 33 -8 -6 12-30.1576 72.8461 29 -8 -6 12-54.3991 75.7322 33 -8 -6 11 154.956 77.9147 29 -8 -6 11 184.895 87.0136 33 -8 -6 10 20996.9 633.755 29 -8 -6 10 21410.1 655.167 33 -8 -6 9 475.829 106.748 29 -8 -6 9 645.876 134.718 33 -8 -6 8 5000.47 306.214 29 -8 -6 8 4442.74 301.197 33 -8 -6 7 10277.9 433.259 29 -8 -6 7 9828.56 446.202 33 -8 -6 6 426.036 110.295 29 -8 -6 6 536.275 116.723 33 -8 -6 5 8720.07 393.363 29 -8 -6 5 8773.00 420.928 33 -8 -6 4 7981.10 848.642 17 -8 -6 3 6182.38 742.975 17 -8 -6 2 1140.93 323.177 17 -8 -6 1 4728.67 653.401 17 8 6 -1 6710.89 759.609 8 8 6 0 19309.7 1241.13 19 8 6 0 17107.1 1065.40 1 8 6 0 17755.3 1222.12 8 8 6 1 6716.53 732.654 19 8 6 1 7897.05 729.432 1 8 6 1 7763.75 797.005 8 8 6 2 330.222 164.907 19 8 6 2 554.744 226.352 1 8 6 2 101.541 134.978 8 8 6 3 2046.22 401.531 19 8 6 3 1654.37 329.332 1 8 6 3 2042.32 406.736 8 8 6 4 1070.63 279.901 1 8 6 4 1155.54 319.610 19 8 6 4 1325.33 324.091 8 8 6 5 1874.99 390.628 19 8 6 5 2250.45 420.953 8 8 6 6 181.334 69.2339 34 8 6 6 157.464 55.2696 27 -8 -6 -6 114.748 88.2536 22 8 6 6 256.943 78.5860 21 8 6 7 518.271 103.860 34 8 6 7 526.899 100.886 27 -8 -6 -7 262.859 120.872 22 8 6 7 287.729 79.1731 21 8 6 8 2041.67 195.163 34 8 6 8 2419.34 200.638 27 -8 -6 -8 2326.43 264.982 22 8 6 8 2197.35 194.341 21 8 6 9 370.572 89.1267 27 8 6 9 269.743 82.4211 34 -8 -6 -9 457.015 158.571 22 8 6 9 415.474 99.8323 21 8 6 10 834.917 123.051 27 8 6 10 564.422 114.161 34 -8 -6 -10 815.436 197.496 22 8 6 10 605.050 109.541 21 8 6 11 895.708 127.085 27 -8 -6 -11 850.551 192.656 22 8 6 11 953.414 132.938 21 8 6 12 105.941 59.2912 27 8 6 12 157.036 69.1191 21 -8 -6 -13 477.592 141.948 22 8 6 13 327.674 85.5297 21 -8 -6 -14 823.848 194.677 22 8 6 14 987.876 133.936 21 8 6 15 6289.59 322.300 31 -8 -6 -15 5820.67 436.130 22 8 6 15 5997.18 310.132 21 8 6 16 843.165 117.924 31 -8 -6 -16 705.324 192.035 22 8 6 16 839.555 121.622 21 -8 -6 -17 21.0483 104.702 22 8 6 17 211.824 66.7797 21 -8 -6 -18 433.098 135.478 22 8 6 18 366.672 71.7557 21 -8 -6 -19 80.7863 92.8038 22 8 6 19 118.843 42.9744 21 -8 -6 -20 561.861 115.116 22 -8 -7 17 1554.00 139.006 29 -8 -7 16 352.444 91.1425 29 -8 -7 16 540.825 110.449 33 -8 -7 15 1748.15 175.486 29 -8 -7 15 1629.48 179.646 33 -8 -7 15 1717.39 152.529 24 -8 -7 14 1303.65 164.550 29 -8 -7 14 1343.76 172.861 33 -8 -7 14 1514.72 151.874 24 -8 -7 14 1379.02 143.180 23 -8 -7 13 701.430 123.833 29 -8 -7 13 574.695 116.454 33 -8 -7 13 609.286 106.342 23 -8 -7 13 797.873 115.965 24 -8 -7 12 1359.59 169.213 29 -8 -7 12 1172.37 168.653 33 -8 -7 12 1318.50 150.003 24 -8 -7 12 1428.27 158.729 23 -8 -7 11 231.062 90.3042 29 -8 -7 11 259.976 95.1323 33 -8 -7 11 335.476 89.5478 23 -8 -7 10 503.332 111.377 29 -8 -7 10 756.710 142.728 33 -8 -7 10 443.056 96.7430 23 -8 -7 9 7789.63 392.529 29 -8 -7 9 7298.54 392.347 33 -8 -7 9 8169.06 381.861 23 -8 -7 8 1148.76 158.913 29 -8 -7 8 1319.19 180.686 33 -8 -7 8 1150.22 147.475 23 -8 -7 7 16667.5 565.351 29 -8 -7 7 16720.5 592.923 33 -8 -7 7 17750.3 558.091 23 -8 -7 6 1098.76 150.667 29 -8 -7 6 1165.82 172.838 33 -8 -7 6 1109.55 147.157 23 -8 -7 5 2164.70 206.395 29 -8 -7 5 1799.55 185.288 23 -8 -7 4 3084.64 243.047 29 -8 -7 4 3007.32 236.580 23 -8 -7 3 6219.15 339.240 29 -8 -7 3 6510.60 343.156 23 -8 -7 2 3160.97 536.803 17 -8 -7 2 3719.82 255.649 23 -8 -7 1 2662.70 486.057 17 8 7 -1 2795.91 455.083 1 -8 -7 1 2622.30 217.155 23 8 7 0 3982.21 559.225 19 -8 -7 0 3787.97 577.426 17 8 7 0 3933.35 540.649 1 8 7 1 1066.02 293.205 19 8 7 1 1477.21 336.084 1 8 7 2 1435.05 351.690 1 8 7 2 1836.10 376.711 19 8 7 3 2425.05 434.382 19 8 7 4 42.5051 44.9854 27 8 7 4 30.6251 43.4023 21 8 7 5 4671.32 272.369 27 8 7 5 5138.78 291.164 21 8 7 6 661.316 110.463 27 -8 -7 -6 771.604 156.279 22 8 7 6 547.157 104.326 21 8 7 7 66.7786 50.7262 27 -8 -7 -7 155.926 136.693 22 8 7 7 49.0271 50.8117 21 8 7 8 235.678 69.9165 27 -8 -7 -8 272.050 117.737 22 8 7 8 272.750 79.0899 21 8 7 9 194.457 71.3559 27 -8 -7 -9 13.2975 96.2217 22 8 7 9 146.348 64.0320 21 8 7 10 344.254 83.5474 27 -8 -7 -10 242.598 114.230 22 8 7 10 277.318 79.6028 21 8 7 11 2122.36 192.189 27 -8 -7 -11 2081.05 275.626 22 8 7 11 2250.00 198.507 21 -8 -7 -12 2191.80 272.324 22 8 7 12 2183.62 196.621 21 -8 -7 -13 409.712 147.860 22 8 7 13 338.387 86.3012 21 -8 -7 -14-46.5117 106.428 22 8 7 14 23.2064 43.9824 21 -8 -7 -15 85.6393 102.273 22 8 7 15 242.910 68.8111 21 -8 -7 -16 321.786 140.312 22 8 7 16 401.596 91.6723 21 -8 -7 -17 61.9306 97.6495 22 8 7 17 64.0422 53.1487 21 -8 -7 -18 41.5820 86.5398 22 8 7 18 82.6584 49.5809 21 -8 -7 -19 332.081 104.987 22 8 7 19 638.732 89.3017 21 -8 -8 16 2029.72 142.769 24 -8 -8 16 2163.97 161.713 29 -8 -8 15 131.215 66.2488 29 -8 -8 15 197.767 63.0654 24 -8 -8 14 10.7832 51.4770 29 -8 -8 14 67.2824 54.8841 24 -8 -8 13 1022.47 146.261 29 -8 -8 13 1103.26 135.448 24 -8 -8 12 5664.76 325.685 29 -8 -8 12 5813.51 309.268 24 -8 -8 12 5594.56 286.622 23 -8 -8 11 3095.85 249.723 29 -8 -8 11 3695.14 279.322 33 -8 -8 11 3901.86 259.321 24 -8 -8 11 3915.19 251.005 23 -8 -8 10 1878.62 196.262 29 -8 -8 10 1954.66 189.566 24 -8 -8 10 2027.75 188.945 23 -8 -8 9 366.066 97.3333 29 -8 -8 9 578.782 119.317 23 -8 -8 9 507.770 110.238 24 -8 -8 8 8817.45 423.945 29 -8 -8 8 9712.85 421.929 24 -8 -8 8 9733.54 414.741 23 -8 -8 7 1924.49 201.771 29 -8 -8 7 2144.36 203.765 24 -8 -8 7 2424.71 215.590 23 -8 -8 6 1186.43 160.708 29 -8 -8 6 1274.09 166.147 23 -8 -8 6 1483.25 170.336 24 -8 -8 5 686.819 124.219 29 -8 -8 5 723.314 127.397 23 -8 -8 5 825.805 128.892 24 -8 -8 4 5883.68 349.225 29 -8 -8 4 6278.71 345.039 24 -8 -8 4 6035.59 334.549 23 -8 -8 3 636.503 125.524 29 -8 -8 3 572.002 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533.464 99.7922 21 8 9 14 14.0635 47.4885 21 8 9 15 1489.47 153.795 21 8 9 16 38.8206 53.7507 25 8 9 16 28.3357 42.6519 21 8 9 17 404.790 76.0932 25 8 9 17 215.182 58.4426 21 8 9 18 308.004 58.9454 25 8 9 18 265.740 65.5394 21 -8 -10 13 2663.61 173.399 24 -8 -10 12 57.5331 43.4341 24 -8 -10 11 875.736 118.880 24 -8 -10 10-70.7289 59.9604 24 -8 -10 9 9.83042 53.3017 24 -8 -10 8 332.453 106.680 29 -8 -10 8 305.695 80.9757 23 -8 -10 8 169.284 65.0227 24 -8 -10 7 402.997 108.606 29 -8 -10 7 494.782 107.042 23 -8 -10 7 316.073 92.3916 24 -8 -10 6 1878.65 201.960 29 -8 -10 6 2218.49 210.280 24 -8 -10 6 1889.04 184.758 23 -8 -10 5 75.9973 63.8442 32 -8 -10 5 98.4142 89.8358 23 -8 -10 5 79.4445 54.6793 24 -8 -10 4 2387.14 207.819 32 -8 -10 4 2416.49 223.966 24 -8 -10 4 2296.37 212.075 23 -8 -10 3 958.897 135.543 32 -8 -10 3 1119.11 154.141 23 -8 -10 3 1045.38 154.981 24 -8 -10 2 695.265 122.401 32 -8 -10 2 795.935 137.127 23 -8 -10 1 1257.20 161.626 32 -8 -10 1 1313.34 170.783 23 -8 -10 0 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1268.05 177.109 26 9 0 1 13708.8 505.257 34 -9 0 -1 13734.0 550.948 26 9 0 2 1019.78 141.541 34 -9 0 -2 1007.91 162.812 26 9 0 3 2244.96 208.499 34 -9 0 -3 2051.48 221.969 26 9 0 4 1176.55 157.984 34 -9 0 -4 1050.29 168.298 26 9 0 5 1403.44 152.229 28 -9 0 -5 1272.88 177.476 26 9 0 5 1397.22 168.569 34 9 0 6 3116.48 237.929 34 9 0 6 2793.89 216.951 28 9 0 7 4077.66 267.831 34 9 0 7 4276.54 267.217 28 9 0 7 4659.31 287.687 31 9 0 8 1112.66 144.220 34 9 0 8 1312.77 150.572 28 9 0 9 326.165 88.4852 34 9 0 9 338.389 88.8123 28 9 0 9 435.570 96.9823 31 9 0 10 846.875 118.812 34 9 0 10 654.838 109.656 28 9 0 10 893.220 131.045 31 9 0 11 117.111 52.2537 34 9 0 11 86.9793 60.8948 28 9 0 11 111.657 56.8283 31 9 0 12 564.521 91.8579 34 9 0 12 522.639 87.8271 28 9 0 12 576.402 96.0306 31 9 0 13 813.292 97.5610 34 9 0 13 638.659 98.8841 31 9 0 14 1045.18 114.250 31 9 0 15 48.9268 33.4786 31 -9 -1 18 339.805 72.3116 29 -9 -1 17 74.2174 49.3976 29 -9 -1 16 1412.30 151.968 29 -9 -1 15 13.5220 53.8348 29 -9 -1 15 21.2208 51.6407 26 -9 -1 14 349.431 86.3709 29 -9 -1 14 429.255 98.3098 26 -9 -1 13 689.246 122.276 29 -9 -1 13 808.938 118.903 26 -9 -1 12 7157.08 336.401 26 -9 -1 11 2024.86 186.266 26 -9 -1 10 302.235 86.7573 26 -9 -1 9 1721.38 177.663 26 -9 -1 8 14574.3 501.928 26 -9 -1 7-14.8666 58.0091 26 -9 -1 6 6282.83 339.566 26 -9 -1 5 35.9555 63.0179 26 -9 -1 4 363.296 100.884 26 -9 -1 3 5399.78 329.561 26 9 1 -2 65.6945 64.2659 34 -9 -1 2 110.185 75.1936 26 9 1 -1 2422.69 213.232 34 -9 -1 1 2196.88 221.227 26 9 1 0 1330.55 160.513 34 -9 -1 0 1304.74 176.471 26 9 1 1 218.223 71.8168 34 -9 -1 -1 119.180 83.6262 26 9 1 2 5616.10 324.325 34 -9 -1 -2 5368.61 352.565 26 9 1 3 5599.92 323.994 34 -9 -1 -3 5422.79 356.149 26 9 1 4 3415.98 254.873 34 -9 -1 -4 3318.98 280.999 26 9 1 5 29.6684 49.4349 34 9 1 5 71.2833 44.1693 28 -9 -1 -5 6.73506 56.1243 26 9 1 6 1333.09 161.422 34 9 1 6 1171.35 143.470 28 -9 -1 -6 820.183 142.547 26 9 1 7 1678.02 181.663 34 9 1 7 1676.51 174.203 28 -9 -1 -7 1515.47 200.732 26 9 1 8 3714.61 258.701 34 9 1 8 3646.71 250.996 28 9 1 9 240.152 80.6234 34 9 1 9 352.123 91.9940 28 9 1 10 89.9004 58.1132 34 9 1 10 143.359 68.5494 28 9 1 10 252.607 78.7707 31 9 1 11-46.4607 57.1419 34 9 1 11 14.6176 49.2711 28 9 1 11 70.1902 54.3350 31 9 1 12 83.4657 54.4978 34 9 1 12-8.25762 54.8606 31 9 1 13 1120.62 126.339 34 9 1 13 870.343 124.212 31 9 1 14 160.068 58.8352 34 9 1 14 105.273 52.3806 31 9 1 15 335.645 71.2680 31 -9 -1 -15 619.029 123.246 22 9 1 16 559.820 83.4669 31 -9 -1 -16 653.123 115.356 22 -9 -2 18 848.472 107.268 29 -9 -2 17 1806.86 161.014 29 -9 -2 16 1438.11 155.428 29 -9 -2 15 148.749 77.8043 29 -9 -2 14 888.671 134.818 29 -9 -2 13 100.334 73.3541 29 -9 -2 13 90.8407 56.8827 26 -9 -2 12 2053.31 201.039 29 -9 -2 12 2172.25 189.818 26 -9 -2 11 2033.76 201.025 29 -9 -2 11 1820.75 178.192 26 -9 -2 10 2555.69 222.485 29 -9 -2 10 2185.30 194.607 26 -9 -2 9 393.386 106.239 29 -9 -2 9 249.813 71.5943 26 -9 -2 8 5332.72 302.086 26 -9 -2 7 3267.83 239.134 26 -9 -2 6 44.8504 54.4758 26 -9 -2 5 339.012 94.1446 26 -9 -2 4 11202.3 450.148 26 -9 -2 3 4.22054 65.0331 26 -9 -2 2 81.1777 76.5905 26 9 2 -1 2111.15 190.523 34 -9 -2 1 2336.81 223.462 26 9 2 0 440.523 94.0358 34 -9 -2 0 376.508 102.400 26 9 2 1 1975.51 194.420 34 -9 -2 -1 2018.67 215.596 26 9 2 2 1786.80 184.173 34 -9 -2 -2 1897.84 210.739 26 9 2 3 13991.3 503.848 34 -9 -2 -3 13456.9 551.045 26 9 2 4 767.537 125.625 34 9 2 4 573.220 94.1830 28 -9 -2 -4 594.068 128.363 26 9 2 5 651.467 118.911 34 9 2 5 576.062 98.9166 28 -9 -2 -5 622.403 129.590 26 9 2 6 41.2700 48.4254 34 9 2 6 30.0136 40.6865 28 -9 -2 -6-43.1405 79.5231 26 9 2 7 78.6174 60.1949 34 -9 -2 -7 4.93811 75.0550 26 9 2 7 56.4722 48.7018 28 9 2 8 174.153 70.5235 34 9 2 8 276.312 81.5298 28 9 2 9 1233.74 159.825 34 9 2 9 1020.95 143.500 28 9 2 10 421.474 94.4824 34 9 2 11 429.284 96.4069 34 9 2 12 20.9276 56.2771 34 9 2 12 75.7291 59.1448 31 9 2 13 205.451 59.3321 34 9 2 13 308.902 87.9437 31 9 2 14 23.5966 49.1003 34 9 2 14 131.182 52.9236 31 9 2 15 63.3530 56.9291 31 -9 -2 -15 155.638 98.6950 22 9 2 16-27.6675 44.3395 31 -9 -2 -16 51.9803 77.7481 22 9 2 17 35.4727 38.6353 31 -9 -2 -17 215.393 91.0655 22 -9 -3 18 298.226 71.8194 29 -9 -3 18 289.085 66.3033 33 -9 -3 17 1994.70 174.038 29 -9 -3 17 1850.13 159.141 33 -9 -3 16 423.935 92.9894 29 -9 -3 16 391.382 88.3470 33 -9 -3 15 36.7000 61.6284 29 -9 -3 15 162.070 71.9457 33 -9 -3 14 3676.00 261.870 29 -9 -3 14 3797.26 253.826 33 -9 -3 13 567.279 112.571 29 -9 -3 13 570.846 110.996 33 -9 -3 12 3439.14 261.055 29 -9 -3 11 1036.44 149.307 29 -9 -3 10 281.150 91.9881 29 -9 -3 10 92.6067 49.2128 26 -9 -3 9 2089.35 202.073 29 -9 -3 9 2320.06 198.173 26 -9 -3 8 3686.17 259.738 29 -9 -3 8 4183.28 266.904 26 -9 -3 7 510.086 99.5706 29 -9 -3 7 500.707 105.934 26 -9 -3 6 1894.73 180.899 29 -9 -3 6 2009.05 194.452 26 -9 -3 5 3941.07 263.897 26 -9 -3 4 733.487 126.101 26 -9 -3 3 153.510 72.9559 26 -9 -3 2 2568.65 226.017 26 -9 -3 1 1253.01 164.922 26 9 3 0 72.2953 56.7933 34 -9 -3 0 149.511 71.6249 26 9 3 1 481.889 96.7462 34 -9 -3 -1 357.345 107.058 26 9 3 2 2646.02 219.524 34 -9 -3 -2 2673.30 244.180 26 9 3 3 3290.89 244.246 34 -9 -3 -3 3076.77 264.841 26 9 3 4 11119.1 446.038 34 -9 -3 -4 10894.8 490.816 26 9 3 5 6.50628 53.0620 34 -9 -3 -5 48.2211 74.5954 26 9 3 6 252.236 82.8737 34 -9 -3 -6 224.260 77.0067 26 9 3 7 1061.84 146.680 34 -9 -3 -7 1262.74 177.325 26 9 3 7 1277.37 148.665 21 9 3 8-4.92503 69.6648 34 9 3 8 52.1309 55.9632 21 9 3 9 122.157 65.6763 34 9 3 9 293.767 78.2178 27 9 3 9 131.300 59.7817 21 9 3 10 49.0211 43.7078 27 9 3 10-42.9549 62.5006 34 9 3 10-22.7770 45.1383 21 9 3 11 1819.40 185.788 34 -9 -3 -11 2139.64 268.417 22 9 3 12 512.046 103.795 34 -9 -3 -12 749.560 174.728 22 9 3 13 1700.24 169.262 34 9 3 13 1527.04 169.751 31 -9 -3 -13 1720.55 230.208 22 9 3 14 1106.59 136.331 34 9 3 14 975.967 135.569 31 -9 -3 -14 924.515 182.057 22 9 3 15 1814.50 172.358 31 -9 -3 -15 1469.81 205.017 22 9 3 16 196.388 64.8541 31 -9 -3 -16 221.228 115.310 22 9 3 17 336.469 73.2970 31 -9 -3 -17 680.412 144.886 22 -9 -4 18 8.59501 41.1280 29 -9 -4 18 16.6811 48.6956 33 -9 -4 18-5.72904 40.7902 23 -9 -4 17-13.5905 49.9229 29 -9 -4 17 20.0276 55.9195 33 -9 -4 16 1793.31 170.625 29 -9 -4 16 2069.39 186.910 33 -9 -4 15 394.521 104.320 29 -9 -4 15 440.343 102.472 33 -9 -4 14 5096.49 303.190 29 -9 -4 14 4957.92 296.228 33 -9 -4 13 35.3151 60.5260 29 -9 -4 13 14.8197 55.2063 33 -9 -4 12 104.179 70.3415 29 -9 -4 12 74.2706 59.3910 33 -9 -4 11 64.9792 72.3042 29 -9 -4 11 12.9083 55.9618 33 -9 -4 10 422.066 102.327 29 -9 -4 10 449.438 103.772 33 -9 -4 9-62.2876 64.1103 29 -9 -4 9 19.4558 56.5163 33 -9 -4 8 267.391 82.0616 29 -9 -4 7 161.128 62.8862 29 -9 -4 7 254.661 80.0972 26 -9 -4 6 569.250 106.083 29 -9 -4 6 453.723 88.7833 26 -9 -4 5 5906.83 316.155 29 -9 -4 5 5836.08 317.688 26 -9 -4 4-1.37622 48.0800 26 -9 -4 3 3971.25 271.723 26 -9 -4 2-5.20285 62.6689 26 -9 -4 1 6894.38 368.243 26 -9 -4 0 35.9613 64.5800 26 9 4 1 5211.52 291.575 34 -9 -4 -1 5873.03 346.135 26 9 4 2 4964.83 289.736 34 -9 -4 -2 4930.66 324.026 26 9 4 3 1711.88 174.382 34 -9 -4 -3 1335.32 176.115 26 9 4 4 1441.17 162.621 34 -9 -4 -4 1284.44 173.262 26 9 4 5 11067.7 443.445 34 -9 -4 -5 10634.3 480.129 26 9 4 6 3280.38 245.560 34 -9 -4 -6 2948.18 259.896 26 9 4 7 243.627 81.3430 34 9 4 7 299.669 80.4303 21 9 4 8 1841.58 190.527 34 9 4 8 1631.88 172.219 27 9 4 8 1276.51 154.629 21 9 4 9 1881.13 190.850 34 9 4 9 2279.29 197.671 27 -9 -4 -9 1830.98 245.203 22 9 4 9 1845.25 180.166 21 9 4 10 126.915 60.6054 27 9 4 10 234.021 84.8709 34 -9 -4 -10 309.884 137.729 22 9 4 10 136.944 49.8965 21 9 4 11 1577.55 174.833 34 9 4 11 1621.66 161.641 27 -9 -4 -11 1753.83 242.716 22 9 4 11 1604.24 164.146 21 9 4 12 997.716 120.727 27 9 4 12 1048.61 144.880 34 -9 -4 -12 882.005 189.477 22 9 4 12 918.038 127.162 21 9 4 13 924.653 135.291 34 -9 -4 -13 872.572 177.894 22 9 4 13 903.328 118.782 21 9 4 14 82.1486 57.2505 31 -9 -4 -14 129.839 108.255 22 9 4 15-18.3552 54.3403 31 -9 -4 -15 234.961 116.849 22 9 4 16 458.761 89.7342 31 -9 -4 -16 395.678 137.851 22 9 4 17 82.7311 48.0870 31 -9 -4 -17 196.050 107.678 22 9 4 18 44.9452 36.8586 31 -9 -4 -18 145.320 94.7864 22 -9 -5 18 484.841 81.0312 29 -9 -5 18 331.459 76.6998 33 -9 -5 18 502.260 69.8089 23 -9 -5 17 150.659 61.1927 29 -9 -5 17 197.168 79.4031 33 -9 -5 17 89.4263 48.5776 23 -9 -5 16 90.2475 54.9313 29 -9 -5 16 281.230 88.8157 33 -9 -5 15-81.5342 73.0713 29 -9 -5 15 31.6716 60.6329 33 -9 -5 14 426.295 104.776 29 -9 -5 14 386.779 103.999 33 -9 -5 13 7720.89 377.163 29 -9 -5 13 7458.97 368.501 33 -9 -5 12 4449.13 292.682 29 -9 -5 12 4670.33 300.819 33 -9 -5 11 639.324 128.157 29 -9 -5 11 902.720 147.628 33 -9 -5 10 2494.36 221.171 29 -9 -5 10 2488.72 224.697 33 -9 -5 9 5722.08 332.099 29 -9 -5 9 5721.82 336.039 33 -9 -5 8 22.3692 53.3657 29 -9 -5 8-68.7666 64.7728 33 -9 -5 7 45.6350 55.2229 29 -9 -5 7 171.916 86.8792 33 -9 -5 6 1662.80 175.358 29 -9 -5 6 2002.23 209.945 33 -9 -5 5 7263.66 360.871 29 -9 -5 4 10620.6 430.106 26 -9 -5 3 4289.68 281.364 26 -9 -5 2 108.673 71.9748 26 -9 -5 1 4425.65 292.703 26 -9 -5 1 6180.02 330.020 23 -9 -5 0 2011.62 203.229 26 -9 -5 -1 397.833 92.4829 26 9 5 2 38.7916 43.4660 34 -9 -5 -2 183.147 84.0609 26 9 5 3 55.4102 42.5846 34 -9 -5 -3 21.4227 61.8443 26 9 5 4 99.2249 56.1277 34 -9 -5 -4 156.262 89.8694 26 9 5 5 16347.5 539.951 34 -9 -5 -5 16464.3 590.000 26 9 5 6 7.02368 52.4652 34 9 5 7 3799.18 268.626 34 9 5 7 3999.78 267.215 27 -9 -5 -7 4130.16 345.406 22 9 5 7 3733.35 259.442 21 9 5 8 478.607 113.300 34 9 5 8 496.682 102.963 27 -9 -5 -8 561.065 149.213 22 9 5 8 520.847 99.4419 21 9 5 9 420.393 99.1608 27 9 5 9 493.831 105.242 34 -9 -5 -9 300.440 135.959 22 9 5 9 489.647 104.556 21 9 5 10 3214.30 246.725 34 9 5 10 3228.26 232.937 27 -9 -5 -10 3404.71 326.870 22 9 5 10 3173.67 231.751 21 9 5 11 57.1847 48.9513 27 9 5 11 159.690 74.5148 34 -9 -5 -11 85.8005 115.106 22 9 5 11 102.710 49.2912 21 9 5 12 4981.88 302.105 34 9 5 12 4791.42 269.973 27 -9 -5 -12 5066.73 398.779 22 9 5 12 5346.47 294.739 21 -9 -5 -13 5733.44 413.451 22 9 5 13 6431.49 313.055 21 -9 -5 -14 1138.91 200.766 22 9 5 14 1367.35 144.320 21 9 5 15 671.515 106.039 31 -9 -5 -15 732.414 178.733 22 9 5 15 808.491 107.178 21 9 5 16 72.1445 44.7105 31 -9 -5 -16 132.048 110.591 22 9 5 16 173.307 49.1431 21 9 5 17 30.9860 32.9230 31 -9 -5 -17-11.4811 80.6408 22 9 5 18 56.2992 35.2589 31 -9 -5 -18 14.5734 79.3088 22 -9 -6 17 342.323 70.0188 29 -9 -6 17 412.717 90.5599 33 -9 -6 16 40.6323 49.2147 29 -9 -6 16-18.6844 54.0189 33 -9 -6 16-5.67619 44.8151 23 -9 -6 15 485.624 97.2952 29 -9 -6 15 704.494 121.964 33 -9 -6 15 510.304 89.1720 23 -9 -6 14 407.321 97.2366 29 -9 -6 14 469.097 102.722 33 -9 -6 14 471.586 93.9251 23 -9 -6 13 2148.57 199.861 29 -9 -6 13 1958.48 196.971 33 -9 -6 12 8358.50 396.118 29 -9 -6 12 8520.22 403.050 33 -9 -6 11 1315.69 167.830 29 -9 -6 11 1415.48 173.464 33 -9 -6 10 5052.26 311.985 29 -9 -6 10 4931.50 319.260 33 -9 -6 9 3572.67 268.650 29 -9 -6 9 3289.78 259.338 33 -9 -6 8 1816.88 194.363 29 -9 -6 8 1779.75 199.652 33 -9 -6 7 306.052 92.7208 29 -9 -6 7 273.002 97.5816 33 -9 -6 6 3648.90 264.677 29 -9 -6 6 3626.07 278.400 33 -9 -6 5 1659.26 180.326 29 -9 -6 4 6422.06 341.498 29 -9 -6 3 1901.33 193.949 23 -9 -6 2 144.821 71.7112 23 -9 -6 1 1700.90 183.557 26 -9 -6 1 1379.46 165.022 23 -9 -6 0 36.9869 54.0266 26 -9 -6 0 37.5757 58.6379 23 -9 -6 -1-5.20991 59.6559 26 -9 -6 -1-0.20256 63.4330 23 -9 -6 -2 209.676 81.8414 26 -9 -6 -2 14.2707 61.5377 23 9 6 3 385.301 90.0223 34 -9 -6 -3 431.904 102.767 26 9 6 4-34.1528 53.4615 34 -9 -6 -4-71.3954 90.0559 26 9 6 5 832.508 127.570 34 9 6 5 800.077 121.955 27 -9 -6 -5 896.096 184.422 22 9 6 6 439.484 102.825 34 9 6 6 451.518 99.2431 27 -9 -6 -6 633.224 158.332 22 9 6 6 499.822 102.281 21 9 6 7 2547.12 223.829 34 9 6 7 2259.75 200.179 27 -9 -6 -7 2591.62 278.013 22 9 6 7 2325.07 206.246 21 9 6 8 2539.52 224.052 34 9 6 8 2692.85 219.204 27 -9 -6 -8 2545.33 285.852 22 9 6 8 2674.34 220.890 21 9 6 9 92.6528 51.5325 27 9 6 9 251.783 84.1627 34 -9 -6 -9 263.005 146.298 22 9 6 9 213.328 74.5296 21 9 6 10 2689.52 231.339 34 9 6 10 2861.50 219.533 27 -9 -6 -10 2616.92 286.885 22 9 6 10 3061.21 230.897 21 9 6 11 2433.32 201.806 27 -9 -6 -11 2266.29 276.346 22 9 6 11 2253.67 200.226 21 9 6 12 183.904 71.4276 27 -9 -6 -12 347.599 137.851 22 9 6 12 216.025 73.1766 21 -9 -6 -13 477.626 166.384 22 9 6 13 489.552 97.5178 21 -9 -6 -14 936.252 183.034 22 9 6 14 1341.78 149.563 21 9 6 15 1.02874 42.1862 31 -9 -6 -15 66.8829 94.9492 22 9 6 15 43.7704 49.6218 21 9 6 16 37.1572 45.2287 31 -9 -6 -16-29.1452 91.9004 22 9 6 16 141.237 56.2409 21 9 6 17 274.694 62.1719 31 -9 -6 -17 328.700 122.469 22 9 6 17 329.775 67.7619 21 -9 -6 -18 415.147 111.403 22 9 6 18 588.166 76.5095 21 -9 -7 16 1577.63 142.941 29 -9 -7 15 4.08524 54.4547 29 -9 -7 15 40.7848 47.6550 23 -9 -7 14 2004.00 182.961 29 -9 -7 14 1975.68 192.142 33 -9 -7 14 1803.89 159.713 23 -9 -7 13 2851.01 226.322 29 -9 -7 13 2723.34 225.256 33 -9 -7 13 2676.31 202.774 23 -9 -7 12 1146.75 152.663 29 -9 -7 12 1370.90 177.099 33 -9 -7 12 1351.14 151.814 23 -9 -7 11 5927.66 338.172 29 -9 -7 11 6412.24 354.388 33 -9 -7 11 6722.99 336.436 23 -9 -7 10 1066.41 150.130 29 -9 -7 10 1308.75 176.716 33 -9 -7 10 1288.37 159.103 23 -9 -7 9 678.407 126.894 29 -9 -7 9 530.789 122.335 33 -9 -7 9 411.519 103.524 23 -9 -7 8 3185.05 250.989 29 -9 -7 8 3332.40 269.495 33 -9 -7 8 3332.52 250.738 23 -9 -7 7 305.308 90.2057 29 -9 -7 7 404.268 101.811 23 -9 -7 6 4205.84 287.582 29 -9 -7 6 4275.07 282.534 23 -9 -7 5 3525.15 261.624 29 -9 -7 5 3692.42 266.923 23 -9 -7 4 260.892 88.6938 29 -9 -7 4 437.491 106.916 23 -9 -7 3 130.346 66.2827 29 -9 -7 3 165.278 79.5452 23 -9 -7 2-54.9919 76.2982 23 -9 -7 1 177.788 85.6559 23 9 7 0 366.009 84.6427 27 -9 -7 0 414.446 103.059 23 9 7 1 2160.34 191.644 27 -9 -7 -1 2394.42 217.231 23 9 7 2-32.7950 43.5529 27 -9 -7 -2 89.6020 69.5456 23 9 7 3 1103.44 142.908 27 -9 -7 -3 1112.63 150.174 23 9 7 4 2261.09 199.469 34 9 7 4 2106.63 192.624 27 9 7 4 2224.98 201.742 21 -9 -7 -4 2252.08 205.834 23 9 7 5 178.200 64.8536 34 9 7 5 232.068 69.4868 27 9 7 5 321.076 91.6100 21 9 7 6 98.3795 59.1300 34 9 7 6 12.2767 46.0712 27 -9 -7 -6 120.259 88.4151 22 9 7 6 252.305 85.7390 21 9 7 7 1197.20 147.670 27 9 7 7 1424.16 164.139 21 9 7 8 1570.23 166.114 27 -9 -7 -8 1879.72 247.387 22 9 7 8 1803.25 181.209 21 9 7 9 142.175 60.1212 27 -9 -7 -9 85.6265 100.148 22 9 7 9 81.7659 58.9032 21 9 7 10 3715.68 251.410 27 9 7 10 3755.79 255.659 21 9 7 11 2186.01 192.896 27 -9 -7 -11 2112.53 266.471 22 9 7 11 2238.47 198.017 21 -9 -7 -12 17.8504 97.9701 22 9 7 12-25.8590 53.2906 21 -9 -7 -13 645.645 165.489 22 9 7 13 876.335 125.694 21 -9 -7 -14 94.5497 100.353 22 9 7 14-37.5437 50.0222 21 9 7 15 571.918 93.9407 31 -9 -7 -15 507.625 151.597 22 9 7 15 550.757 98.2045 21 -9 -7 -16 149.893 103.017 22 9 7 16 205.635 61.4913 21 -9 -7 -17 355.703 109.658 22 9 7 17 415.691 76.9877 21 -9 -7 -18 178.873 89.8680 22 9 7 18 226.056 53.9829 21 -9 -8 15 655.467 96.4308 29 -9 -8 14 253.856 78.2340 29 -9 -8 13 185.979 79.3223 29 -9 -8 13 147.214 65.3648 23 -9 -8 12 694.805 125.115 29 -9 -8 12 595.637 103.429 23 -9 -8 11 2128.53 201.628 29 -9 -8 11 2183.33 189.921 23 -9 -8 10 1678.99 185.038 29 -9 -8 10 2102.27 189.969 23 -9 -8 9 434.273 99.4545 29 -9 -8 9 615.998 115.616 23 -9 -8 8 734.274 132.018 29 -9 -8 8 668.940 119.330 23 -9 -8 7 3548.05 268.514 29 -9 -8 7 3498.51 255.676 23 -9 -8 6 2379.19 220.933 29 -9 -8 6 2491.23 221.343 23 -9 -8 5 801.614 134.620 29 -9 -8 5 892.329 148.773 23 -9 -8 4 871.989 140.426 29 -9 -8 4 980.503 151.935 23 -9 -8 3 3506.30 265.045 29 -9 -8 3 2555.46 225.784 23 -9 -8 2 376.434 103.790 29 -9 -8 2 408.331 102.624 23 -9 -8 1 13562.5 509.134 23 -9 -8 0 3694.13 272.346 23 9 8 1 892.673 122.649 27 -9 -8 -1 938.246 146.316 23 9 8 2 1238.84 143.231 27 9 8 2 1703.45 177.091 21 -9 -8 -2 1696.29 186.209 23 9 8 3 20.6798 44.1798 27 -9 -8 -3 11.1697 57.1522 23 9 8 3 49.5755 48.1177 21 9 8 4 43.6998 49.0408 27 -9 -8 -4 158.150 80.1207 23 9 8 4 94.6571 58.9812 21 9 8 5 5592.16 309.672 27 9 8 5 5851.26 320.337 21 -9 -8 -5 5567.18 325.759 23 9 8 6 2853.55 219.999 27 9 8 6 2805.46 222.470 21 -9 -8 -6 2736.06 230.947 23 9 8 7 4833.71 288.361 27 9 8 7 5066.70 295.139 21 9 8 8 356.533 91.6748 27 9 8 8 332.678 90.6000 21 9 8 9 13395.0 477.744 27 9 8 9 13604.2 480.972 21 -9 -8 -10 929.304 187.508 22 9 8 10 945.970 133.581 21 -9 -8 -11 2090.07 261.070 22 9 8 11 1894.88 183.523 21 -9 -8 -12 236.071 108.483 22 9 8 12 219.932 74.5456 21 -9 -8 -13 1244.06 202.269 22 9 8 13 1462.29 159.395 21 -9 -8 -14 577.932 160.537 22 9 8 14 443.863 96.0010 21 -9 -8 -15 8.64686 102.795 22 9 8 15 71.7659 47.6008 21 -9 -8 -16 1071.59 168.805 22 9 8 16 1019.96 117.779 21 9 8 17-27.6300 37.9805 25 9 8 17-38.9390 47.9295 21 9 8 18 52.2409 38.9436 21 -9 -9 14 155.431 66.6724 29 -9 -9 13 2306.94 180.822 29 -9 -9 13 2281.88 155.092 24 -9 -9 12 166.404 74.7056 29 -9 -9 12 138.055 50.2300 23 -9 -9 12 293.365 69.9028 24 -9 -9 11 1810.46 183.604 29 -9 -9 11 1707.63 154.797 24 -9 -9 11 1864.57 160.971 23 -9 -9 10 2474.12 218.538 29 -9 -9 10 2683.53 197.660 24 -9 -9 10 2331.76 186.831 23 -9 -9 9 170.539 77.0150 29 -9 -9 9 36.6661 57.1334 23 -9 -9 9 137.504 52.2898 24 -9 -9 8 459.125 107.765 29 -9 -9 8 462.954 103.583 23 -9 -9 8 459.964 91.7297 24 -9 -9 7-32.4925 57.8040 29 -9 -9 7-111.222 79.6263 23 -9 -9 7-39.2895 50.8898 24 -9 -9 6 184.655 75.9420 29 -9 -9 6 266.172 83.3022 32 -9 -9 6 341.096 94.3633 23 -9 -9 6 245.587 82.6461 24 -9 -9 5 2115.96 210.237 29 -9 -9 5 2238.97 205.065 24 -9 -9 5 2247.46 208.224 23 -9 -9 4 7408.83 385.154 29 -9 -9 4 7980.74 383.104 24 -9 -9 4 7491.47 379.276 23 -9 -9 3 1464.28 178.913 29 -9 -9 3 1947.53 195.202 24 -9 -9 3 1621.27 183.815 23 -9 -9 2 745.050 130.676 29 -9 -9 2 965.325 147.410 23 -9 -9 2 923.256 135.141 24 -9 -9 1 1052.85 148.896 29 -9 -9 1 775.632 138.024 23 -9 -9 0 204.728 95.7963 23 -9 -9 -1 3987.36 286.841 23 9 9 2 788.826 114.150 27 -9 -9 -2 739.792 131.498 23 9 9 3 338.759 82.0752 27 -9 -9 -3 384.369 102.736 23 9 9 3 355.716 83.1647 21 9 9 4 590.593 103.816 27 -9 -9 -4 566.312 118.460 23 9 9 4 615.309 106.550 21 9 9 5 17732.9 534.362 27 9 9 5 19149.3 558.585 21 -9 -9 -5 17357.2 585.629 23 9 9 6 2502.04 206.710 27 9 9 6 2378.31 204.643 21 -9 -9 -6 2315.08 218.103 23 -9 -9 -7 98.8718 65.7584 32 9 9 7 28.0678 53.5568 21 -9 -9 -8 956.466 137.970 32 9 9 8 695.160 112.935 21 9 9 9 13080.1 466.432 21 9 9 10 177.061 62.7284 21 9 9 11 1703.75 170.439 21 9 9 12 1067.84 133.317 21 9 9 13 371.207 87.1414 21 9 9 14 145.836 58.2854 21 9 9 15 537.554 95.3621 21 9 9 16-5.35086 38.7259 25 9 9 16-47.0336 37.8336 21 9 9 17-7.36324 35.0985 25 9 9 17 28.2293 34.4801 21 -9 -10 13 1143.59 98.6245 24 -9 -10 12 455.648 78.9692 24 -9 -10 11 386.705 74.4363 24 -9 -10 10 121.828 52.8714 23 -9 -10 10 188.695 63.6703 24 -9 -10 9 624.400 111.513 29 -9 -10 9 609.189 99.2913 23 -9 -10 9 641.117 101.695 24 -9 -10 8 83.7909 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34 10 -3 4 22.5045 33.1963 34 -10 2 12 18.8144 45.4820 26 -10 2 11 8.41927 41.6767 26 -10 2 10 261.510 74.4493 26 -10 2 9 40.2284 59.4029 26 -10 2 8 38.0764 49.0039 26 -10 2 7 141.970 68.1328 26 -10 2 6 958.067 130.189 26 10 -2 -5 1115.94 122.003 34 -10 2 5 1069.26 139.737 26 10 -2 -4 526.048 89.5168 34 -10 2 4 464.354 97.7689 26 10 -2 -3-25.3580 44.3410 34 -10 2 3 13.5682 46.4344 26 10 -2 -2 245.349 72.6445 34 -10 2 2 159.948 63.0367 26 10 -2 -1-3.15829 46.1111 34 -10 2 1 6.88128 51.1076 26 10 -2 0 0.66587 45.4433 34 10 -2 1 30.1956 44.3453 34 10 -2 2 436.130 90.6994 34 10 -2 3-9.07099 44.9098 34 10 -2 4 222.168 67.1642 34 10 -2 5 5.32814 39.0639 34 10 -2 6 28.1603 43.3634 34 10 -2 7 184.171 50.5000 34 -10 1 13 53.7376 42.9689 29 -10 1 13 155.969 61.3096 26 -10 1 12 11.4096 34.0682 29 -10 1 12 44.8242 50.0949 26 -10 1 11 277.979 68.7361 29 -10 1 11 345.802 84.4073 26 -10 1 10 2448.24 192.169 26 -10 1 9 976.394 135.138 26 -10 1 8 4336.99 268.441 26 -10 1 7 741.159 123.583 26 -10 1 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159.421 26 -10 0 8 1737.71 177.279 26 -10 0 7 39.7853 65.6813 26 -10 0 6 309.080 91.3403 26 -10 0 5 130.193 74.2408 26 -10 0 4 472.372 109.313 26 10 0 -3 358.542 86.2807 34 -10 0 3 490.440 114.472 26 10 0 -2 173.701 72.0506 34 -10 0 2 91.2068 76.6288 26 10 0 -1 37.9909 55.1976 34 -10 0 1-33.9071 61.1666 26 10 0 0 25.3606 49.7842 34 -10 0 0 200.853 93.6827 26 10 0 1 2769.65 226.908 34 -10 0 -1 2446.01 229.310 26 10 0 2 444.418 101.672 34 -10 0 -2 255.669 87.3778 26 10 0 3 26.7961 47.1796 34 -10 0 -3 128.404 75.5343 26 10 0 4 236.299 80.9047 34 -10 0 -4 218.633 80.7843 26 10 0 5 69.7006 54.3323 34 10 0 6 418.276 89.2956 34 10 0 7 77.2002 59.0102 34 10 0 8 165.912 68.0967 34 10 0 9-13.8839 44.3402 34 10 0 9-12.0704 41.4456 31 10 0 10 425.676 81.9327 34 10 0 10 624.302 91.6973 31 10 0 11 1517.61 128.615 34 10 0 11 1656.18 134.063 31 10 0 12 173.407 48.9055 34 10 0 12 137.452 45.0623 31 -10 -1 16-17.1615 34.8899 29 -10 -1 15 266.095 65.2094 29 -10 -1 15 320.965 63.4159 26 -10 -1 14 33.6882 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603.592 106.098 34 10 1 8 735.909 114.459 31 10 1 9-3.71957 48.8042 34 10 1 9 37.7646 48.3381 31 10 1 10 1850.67 166.864 34 10 1 10 2128.19 180.095 31 10 1 11 671.434 101.631 34 10 1 11 544.894 94.2951 31 10 1 12 153.387 52.4959 34 10 1 12 172.147 51.4735 31 10 1 13 204.906 52.9022 34 10 1 13 185.686 58.2550 31 -10 -2 16-11.2735 42.2957 29 -10 -2 15-80.6971 52.7822 29 -10 -2 14 203.750 72.1216 29 -10 -2 14 97.2512 46.9693 26 -10 -2 13 14.8684 47.7016 29 -10 -2 13 212.072 68.6909 26 -10 -2 12 374.823 93.7716 29 -10 -2 12 353.767 87.4988 26 -10 -2 11 489.785 101.416 29 -10 -2 11 321.204 85.1692 26 -10 -2 10 534.189 103.549 29 -10 -2 10 454.000 100.422 26 -10 -2 9 216.706 75.5640 29 -10 -2 9 176.513 74.8307 26 -10 -2 8 435.329 96.4221 29 -10 -2 8 323.041 91.1948 26 -10 -2 7 56.7991 65.6008 26 -10 -2 6 1412.71 170.715 26 -10 -2 5 218.107 86.0037 26 -10 -2 4 377.389 109.454 26 -10 -2 3 191.049 90.4125 26 -10 -2 2 1779.82 199.225 26 10 2 -1 5302.81 302.278 34 -10 -2 1 5249.10 339.931 26 10 2 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52.0222 54.8836 29 -10 -3 9 49.2130 72.9882 26 -10 -3 8 2756.65 219.147 29 -10 -3 8 3091.85 231.233 26 -10 -3 7 1257.37 150.375 29 -10 -3 7 1423.39 166.006 26 -10 -3 6 504.813 112.433 26 -10 -3 5 8866.00 403.237 26 -10 -3 4 9.57782 64.8316 26 -10 -3 3 1729.28 190.697 26 -10 -3 2 54.0420 78.5542 26 -10 -3 1 651.678 140.559 26 10 3 0 4200.59 270.762 34 -10 -3 0 4541.95 317.318 26 10 3 1 155.024 70.5907 34 -10 -3 -1 370.647 108.895 26 10 3 2 2097.23 198.967 34 -10 -3 -2 2048.99 220.474 26 10 3 3 1290.11 158.440 34 -10 -3 -3 1295.05 181.820 26 10 3 4 3611.67 262.443 34 -10 -3 -4 3785.84 298.603 26 10 3 5 73.2659 64.0204 34 -10 -3 -5-21.0407 70.4889 26 10 3 6 12841.9 483.159 34 -10 -3 -6 13447.7 562.739 26 10 3 6 14301.3 482.148 21 10 3 7 359.999 96.3024 34 10 3 7 475.340 96.9855 21 10 3 8 218.756 88.2341 34 10 3 8 223.489 73.8252 27 10 3 8 266.967 81.1026 21 10 3 9 2321.30 208.977 34 10 3 9 2232.91 184.360 27 10 3 10 2616.61 212.913 34 10 3 10 2787.35 197.909 27 10 3 11 1389.46 157.204 34 10 3 12 146.666 68.3494 34 10 3 12 253.503 73.3346 31 10 3 13-19.4764 47.5113 34 10 3 13-6.42033 43.1968 31 10 3 14 355.771 79.0690 31 -10 -3 -14 243.398 88.4514 22 10 3 15-22.5219 33.7961 31 -10 -3 -15 29.2709 59.2104 22 -10 -4 16 145.914 56.7082 29 -10 -4 16 301.040 68.3174 33 -10 -4 15 9.79401 51.2754 29 -10 -4 15 10.8658 46.5480 33 -10 -4 14 1884.35 174.409 29 -10 -4 14 1870.51 164.346 33 -10 -4 13 290.535 88.7089 29 -10 -4 12 182.355 70.3119 29 -10 -4 11 801.635 128.255 29 -10 -4 10 2338.39 208.186 29 -10 -4 9 46.9931 66.6539 29 -10 -4 9 42.9038 50.5689 26 -10 -4 8 248.128 74.5681 29 -10 -4 8 280.544 80.7339 26 -10 -4 7 1371.57 159.513 29 -10 -4 7 1295.27 156.306 26 -10 -4 6 542.248 107.948 26 -10 -4 5 230.339 77.5744 26 -10 -4 4 8755.91 405.665 26 -10 -4 3-1.51705 57.4763 26 -10 -4 2 397.643 106.514 26 -10 -4 1 602.299 119.886 26 -10 -4 0 7953.24 413.547 26 10 4 1-15.7579 58.2951 34 -10 -4 -1-11.8912 63.2960 26 10 4 2 7816.56 374.128 34 -10 -4 -2 8379.45 439.951 26 10 4 3 3568.58 259.046 34 -10 -4 -3 3630.94 290.062 26 10 4 4 0.63139 49.4887 34 -10 -4 -4-9.22664 67.8546 26 10 4 5 2354.28 211.647 34 -10 -4 -5 2008.86 220.583 26 10 4 6 396.932 98.9384 34 10 4 6 381.833 96.9603 21 10 4 7 3101.31 242.626 34 10 4 7 2778.17 222.390 27 10 4 7 3242.79 236.230 21 10 4 8 1708.22 181.744 34 10 4 8 1721.11 176.052 27 10 4 8 1907.37 179.261 21 10 4 9 82.5005 54.2305 27 10 4 9 82.5473 69.2389 34 10 4 9 49.8392 43.7768 21 10 4 10-27.0573 46.6021 27 10 4 10 22.6163 58.4637 34 10 4 10-31.6961 42.8236 21 10 4 11 695.068 101.406 27 10 4 11 528.416 106.551 34 10 4 11 638.416 100.345 21 10 4 12 33.8607 60.9064 34 -10 -4 -12 17.6011 77.8536 22 10 4 12 69.9400 45.7626 21 10 4 13-34.0989 43.7597 34 10 4 13 80.4379 60.4083 31 -10 -4 -13 126.875 103.716 22 10 4 14 111.384 56.1105 31 -10 -4 -14 41.2812 77.6680 22 10 4 15 383.984 77.2920 31 -10 -4 -15 348.760 98.0396 22 10 4 16 112.250 47.7413 31 -10 -4 -16 184.613 72.8743 22 -10 -5 16 296.501 70.5335 29 -10 -5 16 374.636 72.5770 23 -10 -5 15-73.4312 54.3828 29 -10 -5 15 90.1239 55.3359 33 -10 -5 15 68.3012 54.0816 23 -10 -5 14 891.793 127.568 29 -10 -5 14 757.666 110.642 33 -10 -5 13 89.6297 58.8223 29 -10 -5 13 128.674 64.4322 33 -10 -5 12 227.902 85.2524 29 -10 -5 12 373.840 97.8749 33 -10 -5 11 1762.42 184.331 29 -10 -5 11 2021.65 190.893 33 -10 -5 10 5.65474 53.8815 29 -10 -5 10 68.9391 58.0795 33 -10 -5 9 16.8748 52.2771 29 -10 -5 9 87.0305 73.7484 33 -10 -5 8 354.574 87.9695 29 -10 -5 7-17.3542 45.8321 29 -10 -5 6 1.19995 42.1690 29 -10 -5 6 73.3207 57.2854 26 -10 -5 5 800.093 127.699 26 -10 -5 4 7935.59 384.389 26 -10 -5 3 174.599 76.1875 26 -10 -5 3 288.597 89.2501 23 -10 -5 2 4865.95 315.658 26 -10 -5 2 4528.70 286.909 23 -10 -5 1 74.6025 73.1943 26 -10 -5 1 41.0941 69.3291 23 -10 -5 0 10271.8 460.954 26 -10 -5 -1 69.3250 79.0681 26 10 5 2 32543.1 750.831 34 -10 -5 -2 34872.1 870.308 26 10 5 3 2454.30 212.937 34 -10 -5 -3 2580.25 243.251 26 10 5 4 52.4678 48.7011 34 -10 -5 -4-36.6868 80.0070 26 10 5 5 58.0078 64.0034 34 -10 -5 -5 1.00573 78.3914 26 10 5 6 9360.45 422.507 34 10 5 6 10125.0 426.027 27 10 5 6 10330.4 427.499 21 10 5 7 3.84258 50.8836 34 10 5 7 92.3820 63.8147 27 10 5 7 103.070 72.4417 21 10 5 8 1220.67 159.196 34 10 5 8 1114.58 146.730 27 10 5 8 1219.58 149.134 21 10 5 9 2859.32 235.535 34 10 5 9 2556.19 210.748 27 10 5 9 2769.69 215.178 21 10 5 10 5925.81 326.915 34 10 5 10 5435.03 293.033 27 -10 -5 -10 5779.15 389.748 22 10 5 10 5568.07 295.246 21 10 5 11 281.061 67.8581 27 10 5 11 338.228 89.8459 34 -10 -5 -11 394.735 132.425 22 10 5 11 396.582 96.1213 21 10 5 12 1569.70 165.725 34 10 5 12 1651.75 150.399 27 -10 -5 -12 1532.52 208.776 22 10 5 12 1705.50 159.636 21 -10 -5 -13 1326.38 193.785 22 10 5 13 1273.22 131.072 21 10 5 14 289.597 76.1312 31 -10 -5 -14 290.211 105.996 22 10 5 14 254.598 64.0419 21 10 5 15-42.6976 49.0938 31 -10 -5 -15-115.968 94.0965 22 10 5 16 416.586 75.8929 31 -10 -5 -16 188.744 88.3679 22 -10 -6 16 1910.86 147.616 29 -10 -6 16 2011.06 136.364 23 -10 -6 15 25.3937 51.4302 29 -10 -6 15 156.238 56.7181 23 -10 -6 14 721.912 111.553 29 -10 -6 14 645.800 100.920 23 -10 -6 13 405.786 97.3493 29 -10 -6 13 394.601 91.0374 23 -10 -6 12 2390.11 205.889 29 -10 -6 12 2293.65 199.832 33 -10 -6 12 2370.92 199.083 23 -10 -6 11 59.2869 61.6800 29 -10 -6 10 2771.46 226.071 29 -10 -6 9 101.473 53.5316 29 -10 -6 8 1863.49 189.366 29 -10 -6 7 1737.87 184.640 29 -10 -6 6 2043.27 200.452 29 -10 -6 6 2170.95 201.607 23 -10 -6 5 3413.27 249.746 29 -10 -6 5 3106.60 240.670 23 -10 -6 4 9289.19 410.337 23 -10 -6 3 8238.07 388.634 26 -10 -6 3 6948.38 358.427 23 -10 -6 2 515.918 106.370 26 -10 -6 2 407.954 103.772 23 -10 -6 1 392.876 101.346 26 -10 -6 1 264.448 89.3485 23 -10 -6 0 374.667 106.825 26 -10 -6 0 401.378 97.0115 23 -10 -6 -1 4484.38 308.851 26 -10 -6 -2 3067.99 256.917 26 10 6 3 3240.75 240.454 34 -10 -6 -3 3646.61 284.194 26 10 6 4 6835.94 351.954 34 10 6 4 6251.22 337.146 27 10 6 5 6011.48 335.854 34 10 6 5 5398.72 313.801 27 10 6 5 5707.89 321.716 21 10 6 6 3182.93 248.672 34 10 6 6 2949.72 231.842 27 10 6 6 3278.77 245.303 21 10 6 7 161.758 75.8771 34 10 6 7 99.8496 72.8473 27 10 6 7 7.33231 49.5171 21 10 6 8 275.459 78.1767 27 10 6 8 124.764 66.0350 34 10 6 8 218.706 82.0688 21 10 6 9 865.204 124.780 27 10 6 9 910.852 139.364 34 -10 -6 -9 788.086 169.675 22 10 6 9 663.841 112.888 21 10 6 10 3.40494 44.8925 27 10 6 10 12.2993 51.6604 34 -10 -6 -10-74.3266 105.398 22 10 6 10-56.7837 56.6909 21 10 6 11 471.026 91.7948 27 -10 -6 -11 701.823 161.158 22 10 6 11 607.056 102.104 21 10 6 12 162.328 61.8440 27 -10 -6 -12 169.385 97.2470 22 10 6 12 246.516 74.5255 21 -10 -6 -13 277.268 106.458 22 10 6 13 502.639 94.3453 21 10 6 14 38.8533 51.1009 31 -10 -6 -14-7.52199 82.3342 22 10 6 14 52.7048 47.0163 21 10 6 15 472.757 85.8342 31 -10 -6 -15 495.313 117.136 22 10 6 15 340.921 66.1641 21 10 6 16-14.0467 37.0090 31 -10 -6 -16 54.6847 75.0161 22 10 6 16 46.8770 32.2817 21 10 6 17 14.8825 31.6616 31 -10 -6 -17-61.5770 74.3311 22 -10 -7 15 72.1981 51.1119 29 -10 -7 15 254.709 61.7112 23 -10 -7 14-41.1937 52.3971 29 -10 -7 14 51.9669 47.1495 23 -10 -7 13 243.907 73.9445 29 -10 -7 13 169.642 60.4086 23 -10 -7 12 59.2478 54.4279 29 -10 -7 12 66.0034 54.1614 23 -10 -7 11 207.277 77.8766 29 -10 -7 11 192.007 76.5980 23 -10 -7 10 592.867 118.924 29 -10 -7 10 699.777 117.522 23 -10 -7 9 4073.58 272.954 29 -10 -7 9 4121.92 268.843 23 -10 -7 8 5.36123 55.1266 29 -10 -7 8 49.1299 70.7133 23 -10 -7 7 3271.66 248.317 29 -10 -7 7 3039.61 237.593 23 -10 -7 6 530.717 110.146 29 -10 -7 6 409.037 100.546 23 -10 -7 5 9300.37 413.718 29 -10 -7 5 8387.12 391.619 23 -10 -7 4 720.033 126.967 29 -10 -7 4 781.071 137.516 23 -10 -7 3 3160.03 246.432 23 -10 -7 2 160.744 84.1110 23 10 7 -1 448.312 94.0517 27 -10 -7 1 270.718 83.5405 23 10 7 0 133.756 64.0834 27 -10 -7 0 175.097 64.6333 26 -10 -7 0 159.751 73.1518 23 10 7 1 336.471 94.3313 27 -10 -7 -1 278.695 80.7825 26 -10 -7 -1 302.968 93.3310 23 10 7 2 3816.93 265.721 27 -10 -7 -2 3979.55 276.356 23 10 7 3 1993.98 192.681 27 10 7 4 1174.06 150.068 34 10 7 4 936.482 138.033 27 10 7 4 1124.42 155.260 21 10 7 5 1005.55 140.966 34 10 7 5 1022.19 144.077 27 10 7 5 1064.98 143.222 21 10 7 6 1307.77 159.747 34 10 7 6 1294.00 157.705 27 10 7 6 1373.78 165.200 21 10 7 7 419.957 94.1777 27 10 7 7 356.039 94.5695 21 10 7 8 295.387 89.1583 27 -10 -7 -8 125.098 129.809 22 10 7 8 228.436 69.5919 21 10 7 9 118.173 63.3836 27 -10 -7 -9-19.2536 85.6833 22 10 7 9 79.7921 62.0477 21 10 7 10-64.0481 62.5725 27 10 7 10 23.2580 50.7392 21 10 7 11 2071.90 181.343 27 -10 -7 -11 2160.32 251.529 22 10 7 11 2404.46 196.854 21 -10 -7 -12 51.4095 84.2253 22 10 7 12-17.6331 49.6796 21 -10 -7 -13 3689.58 297.536 22 10 7 13 3350.65 218.164 21 10 7 14 487.973 90.2771 31 -10 -7 -14 370.020 113.261 22 10 7 14 469.449 86.9034 21 10 7 15 55.8031 39.8871 31 -10 -7 -15 30.8121 72.8605 22 10 7 15-35.3214 48.9372 21 10 7 16 21.7983 28.8912 31 -10 -7 -16 3.71404 75.1771 22 10 7 16 59.9963 39.0417 21 -10 -8 14 844.557 108.993 29 -10 -8 14 676.490 83.4738 23 -10 -8 13 720.416 107.428 29 -10 -8 13 653.493 90.9797 23 -10 -8 12 437.401 92.1351 29 -10 -8 12 449.943 91.2595 23 -10 -8 11 642.774 121.205 29 -10 -8 11 762.072 113.377 23 -10 -8 10 900.060 135.302 29 -10 -8 10 715.095 115.808 23 -10 -8 9 4365.37 280.785 29 -10 -8 9 4677.43 277.582 23 -10 -8 8 179.608 76.0599 29 -10 -8 8 223.199 83.8372 23 -10 -8 7 461.136 109.667 29 -10 -8 7 274.938 83.6719 23 -10 -8 6 1684.32 181.040 29 -10 -8 6 1907.10 189.310 23 -10 -8 5 45.6660 60.0716 29 -10 -8 5 130.688 80.0938 23 -10 -8 4 403.515 100.841 29 -10 -8 4 303.567 90.9920 23 -10 -8 3 2424.22 217.389 29 -10 -8 3 1864.54 191.175 23 -10 -8 2-33.5582 65.9063 23 -10 -8 1 729.710 130.197 23 10 8 0-62.7127 46.7675 27 -10 -8 0-22.6101 65.1032 23 10 8 1 615.782 105.069 27 -10 -8 -1 572.564 113.633 23 10 8 2 44.4455 50.4790 27 -10 -8 -2 66.3273 65.8038 23 10 8 2-21.4246 49.9913 21 10 8 3 736.220 120.154 27 -10 -8 -3 838.605 139.954 23 10 8 3 705.854 121.866 21 10 8 4 309.577 84.7700 27 -10 -8 -4 227.990 80.5474 23 10 8 4 164.421 61.4544 21 10 8 5 198.982 68.2594 27 10 8 5 264.866 80.4390 21 10 8 6 705.963 118.081 27 10 8 6 745.316 122.970 21 10 8 7 1701.30 174.882 27 10 8 7 1700.85 175.026 21 10 8 8 176.841 69.7088 27 10 8 8 152.506 77.4592 21 10 8 9 3321.32 238.196 27 10 8 9 3727.27 250.983 21 10 8 10-25.7879 51.5075 21 10 8 11 183.365 69.4941 21 10 8 12 857.946 117.980 21 10 8 13 104.749 44.4031 21 10 8 14 29.1053 43.8051 21 10 8 15 541.759 84.6032 21 10 8 16 75.0082 41.9864 21 -10 -9 13 1459.98 133.276 29 -10 -9 13 1212.34 105.287 23 -10 -9 12 2003.88 166.310 29 -10 -9 12 2015.51 147.564 23 -10 -9 11 1578.37 155.232 29 -10 -9 11 1745.01 149.658 23 -10 -9 10 462.592 98.9767 29 -10 -9 10 520.527 97.1150 23 -10 -9 9 161.625 70.4429 29 -10 -9 9 61.8113 53.1248 23 -10 -9 8 605.898 116.739 29 -10 -9 8 535.281 102.563 23 -10 -9 7 928.657 135.139 29 -10 -9 7 1134.73 143.534 23 -10 -9 6 349.499 97.6034 29 -10 -9 6 289.655 86.8520 23 -10 -9 5 208.249 81.4130 29 -10 -9 5 99.4008 75.0201 23 -10 -9 4 787.279 130.918 29 -10 -9 4 937.024 146.859 23 -10 -9 3 2739.08 229.465 29 -10 -9 3 3117.80 244.098 23 -10 -9 2 2857.69 234.431 29 -10 -9 2 2346.52 219.438 23 -10 -9 1 351.040 102.943 23 -10 -9 0 1172.84 160.147 23 10 9 1 1685.00 169.829 21 -10 -9 -1 1557.52 179.873 23 10 9 2 1009.85 129.622 27 -10 -9 -2 906.145 149.786 23 10 9 2 908.919 129.084 21 10 9 3 945.873 125.045 27 -10 -9 -3 903.087 145.936 23 10 9 3 917.448 128.591 21 10 9 4 3035.26 223.753 27 10 9 4 2857.20 218.302 21 -10 -9 -4 2769.16 237.479 23 10 9 5 212.979 67.3757 27 -10 -9 -5 214.143 84.6522 23 10 9 5 326.583 80.3670 21 10 9 6 2238.68 193.651 27 10 9 6 2123.61 189.200 21 -10 -9 -6 2058.09 199.357 23 -10 -9 -7-56.3903 48.5789 32 10 9 7 2.73656 49.3820 27 10 9 7-9.84422 45.2254 21 -10 -9 -8 15.2213 48.0214 32 10 9 8 26.4411 45.2370 21 10 9 9 892.573 130.028 21 10 9 10 1044.20 132.469 21 10 9 11 10.1434 53.1594 21 10 9 12 34.6079 46.4935 21 10 9 13-3.16721 41.5622 21 10 9 14 87.3337 47.6000 21 10 9 15 28.9558 38.0186 21 10 9 16 867.862 86.2947 25 10 9 16 767.937 87.5378 21 -10 -10 11 45.0029 38.2241 23 -10 -10 10 748.504 97.6422 23 -10 -10 9 2124.21 178.165 29 -10 -10 9 2217.58 171.736 23 -10 -10 8 73.0630 66.8972 29 -10 -10 8 97.1930 65.9995 23 -10 -10 7 127.630 67.9202 29 -10 -10 7 14.3518 63.1888 23 -10 -10 6 4939.59 290.528 29 -10 -10 6 4607.73 255.696 32 -10 -10 6 4631.31 269.506 23 -10 -10 5 417.029 90.7844 32 -10 -10 5 536.450 114.208 23 -10 -10 4 666.747 114.411 32 -10 -10 4 699.222 128.156 23 -10 -10 3 4655.63 281.725 32 -10 -10 3 4907.33 296.954 23 -10 -10 2 92.4791 60.6791 32 -10 -10 2 300.879 93.2350 23 -10 -10 1-18.8640 53.8333 32 -10 -10 1-10.6999 67.5478 23 -10 -10 0 810.042 128.729 32 -10 -10 0 706.924 132.818 23 -10 -10 -1 846.258 132.892 32 -10 -10 -1 751.008 130.612 23 -10 -10 -2 18.9735 53.1686 32 -10 -10 -2 19.2694 69.0387 23 -10 -10 -3 170.042 77.3912 32 -10 -10 -3 197.816 80.5249 23 -10 -10 -4 348.245 94.1307 32 -10 -10 -4 217.691 87.8443 23 10 10 4 407.959 85.2103 21 -10 -10 -5 100.767 67.3150 32 -10 -10 -5-10.7356 57.1820 23 10 10 5 64.5394 57.0664 21 -10 -10 -6 4488.36 284.862 32 10 10 6 4776.08 267.564 21 -10 -10 -7 1237.22 152.573 32 10 10 7 1054.13 132.286 21 -10 -10 -8 878.619 127.138 32 10 10 8 744.621 110.561 21 -10 -10 -9 468.921 92.0682 32 10 10 9 335.099 74.0096 21 10 10 10 537.089 89.4531 21 10 10 11 175.300 58.9950 21 10 10 12 49.7159 48.3833 21 10 10 13 170.265 58.1695 21 10 10 14 128.117 54.0489 21 10 10 15-13.0286 33.6643 25 10 10 15 14.0270 34.3222 21 -10 -11 9 42.5302 40.8850 23 -10 -11 9 91.3311 41.8351 24 -10 -11 8 76.2370 40.9948 23 -10 -11 8 27.7597 36.2111 24 -10 -11 7 317.130 72.5616 23 -10 -11 7 324.616 69.6629 24 -10 -11 6 220.793 76.7627 23 -10 -11 6 166.255 63.0690 24 -10 -11 5 530.993 91.0566 32 -10 -11 5 561.943 101.455 23 -10 -11 5 506.440 84.1246 24 -10 -11 4 1209.22 138.899 32 -10 -11 4 1026.36 138.190 23 -10 -11 4 1084.94 125.002 24 -10 -11 3 1344.31 144.522 32 -10 -11 3 1606.76 156.670 24 -10 -11 3 1436.13 161.883 23 -10 -11 2 67.1620 55.7436 32 -10 -11 2 38.8149 63.9419 23 -10 -11 2 105.491 56.9014 24 -10 -11 1 818.755 124.719 32 -10 -11 1 796.578 130.729 23 -10 -11 1 806.200 117.374 24 -10 -11 0 74.2372 55.7411 32 -10 -11 0 173.870 82.1449 23 -10 -11 0 231.056 64.7402 24 -10 -11 -1 220.365 72.0026 32 -10 -11 -1 252.542 80.0497 23 -10 -11 -1 252.937 78.6954 24 -10 -11 -2 81.7559 62.5035 32 -10 -11 -2 21.6160 62.5154 23 -10 -11 -3 92.1202 70.0675 32 -10 -11 -3 20.0928 64.3996 23 -10 -11 -4-48.2030 62.9506 32 -10 -11 -5 1087.55 140.930 32 -10 -11 -6 721.641 114.029 32 -10 -11 -7 616.257 107.287 32 -10 -11 -8 79.3501 57.1203 32 10 11 8 102.828 48.6967 21 -10 -11 -9 80.1953 48.9996 32 10 11 9 12.8081 40.2878 21 10 11 10 150.573 54.0550 21 10 11 11 746.076 94.8382 21 10 11 12-0.46309 33.7909 21 10 11 13 302.660 62.3073 25 10 11 13 221.453 51.9714 21 -10 -12 7 834.745 87.6813 24 -10 -12 6 128.290 45.3201 24 -10 -12 5 1512.68 130.819 24 -10 -12 5 1443.68 133.120 23 -10 -12 4 889.781 102.509 32 -10 -12 4 915.311 114.861 23 -10 -12 4 970.388 109.186 24 -10 -12 3 129.441 53.3181 32 -10 -12 3 110.504 58.2588 23 -10 -12 3 260.136 64.3792 24 -10 -12 2 16.6873 43.2542 32 -10 -12 2 54.0743 48.7510 23 -10 -12 2 69.0836 51.1085 24 -10 -12 1 559.749 94.5916 32 -10 -12 1 509.090 93.1450 23 -10 -12 1 590.724 98.2370 24 -10 -12 0 64.8523 56.8829 32 -10 -12 0 95.0781 53.2474 24 -10 -12 -1-23.9176 51.1903 32 -10 -12 -1 80.6755 56.0184 24 -10 -12 -2 49.2228 53.6307 32 -10 -12 -2 70.1443 53.0982 24 -10 -12 -3 446.398 95.7897 32 -10 -12 -4 122.473 63.7539 32 -10 -12 -5 132.172 56.1972 32 -10 -12 -6-30.2087 59.2164 32 -10 -12 -7 247.401 68.4740 32 -10 -12 -8 327.058 72.2377 32 -10 -12 -9 155.778 56.8627 32 10 12 9 184.698 52.8921 25 10 12 10 74.1710 39.0058 25 10 12 11 2436.92 151.331 25 -10 -13 3 38.7232 35.5903 32 -10 -13 3-30.5251 37.4576 24 -10 -13 2 1630.25 122.900 32 -10 -13 2 1837.77 136.539 24 -10 -13 1 95.6226 39.9150 32 -10 -13 1 75.7999 37.1752 24 -10 -13 0 33.4690 40.9150 32 -10 -13 0-68.2371 47.1261 24 -10 -13 -1 53.8215 40.7465 32 -10 -13 -1 49.3598 34.4285 24 -10 -13 -2-45.5271 40.6260 32 -10 -13 -2 79.0829 49.6930 24 -10 -13 -3 39.2465 45.5344 32 -10 -13 -3 119.047 50.9787 24 -10 -13 -4 969.436 113.190 32 -10 -13 -4 943.581 108.019 24 -10 -13 -5 34.2969 38.4223 32 -10 -13 -5 75.1978 50.4230 24 -10 -13 -6-21.0003 38.1055 32 -10 -13 -7 251.947 62.3023 32 -10 -13 -8 49.1042 40.0642 32 -11 2 5 67.8080 41.4941 26 11 -2 -4 28.1842 28.2380 34 -11 2 4-22.0898 36.4268 26 11 -2 -3 89.1293 37.3733 34 -11 2 3 135.243 49.2013 26 11 -2 -2 676.213 83.4822 34 11 -2 -1-5.52121 31.2526 34 11 -2 0 50.2851 40.4526 34 -11 1 9 70.5508 47.5874 26 -11 1 8 584.738 95.5541 26 -11 1 7-53.5303 54.5536 26 -11 1 6-4.09410 52.6695 26 -11 1 5 81.5860 53.0100 26 -11 1 4 236.004 74.0068 26 11 -1 -3-35.2084 39.2207 34 -11 1 3-0.31787 51.8981 26 11 -1 -2 132.943 54.3071 34 -11 1 2 97.5307 52.4452 26 11 -1 -1 365.632 73.4900 34 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56.9802 34 11 2 9 118.041 54.2835 31 11 2 10 1833.73 152.424 34 11 2 10 1861.97 153.433 31 11 2 11 653.027 91.3194 34 11 2 11 735.169 95.3456 31 11 2 12 590.847 78.6528 34 11 2 12 655.807 84.0245 31 -11 -3 14 108.667 42.9103 29 -11 -3 13 424.496 78.6508 29 -11 -3 12 78.2692 45.8506 29 -11 -3 12 56.5823 43.3995 26 -11 -3 11 455.298 91.1279 29 -11 -3 11 439.965 86.4974 26 -11 -3 10-11.8100 44.0226 29 -11 -3 10 71.2927 62.0418 26 -11 -3 9 439.982 84.8272 29 -11 -3 9 601.096 106.396 26 -11 -3 8-32.6161 51.6654 26 -11 -3 7 143.787 74.9155 26 -11 -3 6 117.136 64.4922 26 -11 -3 5 394.497 95.9147 26 -11 -3 4 2004.10 201.233 26 -11 -3 3 76.9672 69.4801 26 -11 -3 2 337.010 103.527 26 -11 -3 1-0.45700 81.1478 26 11 3 0 334.111 77.6262 34 -11 -3 0 109.728 69.0935 26 11 3 1 53.9911 47.6472 34 -11 -3 -1 21.2552 72.2598 26 11 3 2 391.536 85.2944 34 -11 -3 -2 476.110 120.842 26 11 3 3 1901.36 186.237 34 -11 -3 -3 1811.90 204.899 26 11 3 4 4044.03 267.188 34 -11 -3 -4 3533.60 282.096 26 11 3 5 7.32027 58.3217 34 -11 -3 -5-21.1168 64.6350 26 11 3 5 34.9310 56.0352 21 11 3 6 1265.10 154.475 34 11 3 6 1263.69 138.358 21 11 3 7 1099.37 143.565 34 11 3 7 1181.44 137.155 27 11 3 7 1216.72 126.842 21 11 3 8 1356.93 152.828 34 11 3 8 1308.13 137.074 27 11 3 9 2029.17 178.461 34 11 3 9 1922.16 153.830 27 11 3 10 777.882 108.205 34 11 3 10 678.362 104.229 31 11 3 11 857.052 110.237 34 11 3 11 887.696 115.078 31 11 3 12 65.1482 45.2077 34 11 3 12 67.5790 45.6018 31 11 3 13 256.078 61.3294 31 -11 -4 14 114.115 54.0941 29 -11 -4 13 499.392 89.1647 29 -11 -4 12 110.135 60.1135 29 -11 -4 11 3071.58 209.793 29 -11 -4 10 782.369 112.623 29 -11 -4 9-9.99079 40.7020 29 -11 -4 9 36.4191 50.9626 26 -11 -4 8 863.647 119.517 29 -11 -4 8 813.135 120.089 26 -11 -4 7 1346.83 153.870 26 -11 -4 6 425.092 101.455 26 -11 -4 5 1199.21 158.686 26 -11 -4 4 1746.48 186.873 26 -11 -4 4 1811.86 176.941 23 -11 -4 3 70.8784 68.3075 26 -11 -4 2 5411.57 328.639 26 -11 -4 1-29.6120 62.2570 26 -11 -4 0 529.573 119.872 26 11 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83.1082 27 11 5 9 278.008 86.7244 34 11 5 9 274.637 67.2076 21 11 5 10 6.95898 44.2371 27 11 5 10 78.9718 64.6934 34 11 5 10-15.8197 45.2567 21 11 5 11 216.997 61.6639 27 11 5 11 123.449 58.7891 34 11 5 11 188.314 57.4351 21 11 5 12-5.17064 36.8196 21 11 5 13 1573.45 145.025 31 11 5 14 72.8882 40.5565 31 -11 -6 14 20.8451 44.0329 29 -11 -6 14 58.2999 46.9825 23 -11 -6 13 250.339 72.2489 29 -11 -6 13 286.994 70.7260 23 -11 -6 12 138.566 63.6383 29 -11 -6 12 40.7429 54.7939 23 -11 -6 11 4.09396 45.7084 29 -11 -6 11-34.3820 59.4816 23 -11 -6 10-44.9890 52.0354 29 -11 -6 10 38.3419 61.0433 23 -11 -6 9 1895.64 176.561 29 -11 -6 9 1678.98 167.485 23 -11 -6 8 48.9350 47.0575 29 -11 -6 8 71.8504 59.2531 23 -11 -6 7 303.726 82.3133 29 -11 -6 7 472.545 103.071 23 -11 -6 6 115.693 76.5098 23 -11 -6 5 1624.52 173.096 23 -11 -6 4 572.883 111.232 26 -11 -6 4 551.916 112.108 23 -11 -6 3 169.758 65.6741 26 -11 -6 3 93.7514 56.9394 23 -11 -6 2 596.373 114.062 26 -11 -6 2 223.721 84.2749 23 -11 -6 1 4624.69 299.311 26 -11 -6 1 3739.34 258.530 23 -11 -6 0 4.64425 65.0983 26 -11 -6 -1 983.575 151.484 26 -11 -6 -2 649.696 133.723 26 11 6 3 12597.5 460.771 34 11 6 3 12088.7 467.118 27 11 6 4 391.310 101.920 34 11 6 4 238.942 78.6689 27 11 6 4 513.757 113.241 21 11 6 5 132.484 79.4886 34 11 6 5 6.08190 58.3963 27 11 6 5 51.1833 54.0234 21 11 6 6 1474.99 169.034 34 11 6 6 1365.85 159.772 27 11 6 6 1563.49 169.974 21 11 6 7 2861.65 229.037 34 11 6 7 2651.85 212.522 27 11 6 7 2976.26 224.823 21 11 6 8 208.135 74.3827 27 11 6 8 89.3805 66.4347 34 11 6 8 97.5586 59.2814 21 11 6 9 560.959 97.1705 27 11 6 9 667.676 112.393 34 11 6 9 635.318 107.106 21 11 6 10 43.7702 53.8662 27 11 6 10-16.9583 46.6439 21 11 6 11 72.8428 47.9903 27 -11 -6 -11-56.6461 75.4512 22 11 6 11-6.06981 44.5504 21 -11 -6 -12 150.207 84.2076 22 11 6 12 309.684 72.5097 21 11 6 13 77.5486 48.5056 31 -11 -6 -13 63.6482 57.3645 22 11 6 13 62.8554 40.4946 21 11 6 14 325.377 68.7399 31 11 6 14 243.701 52.7541 21 -11 -7 13 59.9531 48.1293 29 -11 -7 13 10.3870 41.6992 23 -11 -7 12-10.4747 42.7986 29 -11 -7 12 62.6870 50.7365 23 -11 -7 11 510.808 95.3976 29 -11 -7 11 515.843 91.1932 23 -11 -7 10 458.026 88.2249 29 -11 -7 10 544.849 98.6364 23 -11 -7 9-80.8359 71.6011 29 -11 -7 9-25.0395 51.1068 23 -11 -7 8 564.665 99.8844 29 -11 -7 8 743.014 127.609 23 -11 -7 7-9.64469 42.7971 29 -11 -7 7 98.6609 62.6129 23 -11 -7 6 538.933 102.362 29 -11 -7 6 291.221 85.7681 23 -11 -7 5 622.230 115.047 23 -11 -7 4 278.905 85.9211 23 -11 -7 3-56.7404 61.2070 23 11 7 -2 156.696 59.1706 27 -11 -7 2 220.973 75.4624 23 11 7 -1 489.572 100.990 27 -11 -7 1 438.129 97.3895 26 -11 -7 1 556.466 115.591 23 11 7 0 1050.88 140.806 27 -11 -7 0 982.466 142.096 23 11 7 1 5440.06 312.061 27 -11 -7 -1 5025.41 304.494 23 11 7 2 1732.80 180.632 27 11 7 3 368.144 86.6702 27 11 7 3 419.934 101.696 21 11 7 4 801.741 125.132 27 11 7 4 732.478 123.141 21 11 7 5 1816.10 184.417 27 11 7 5 1818.59 180.703 21 11 7 6 695.030 117.943 27 11 7 6 902.208 131.609 21 11 7 7 250.847 88.9725 27 11 7 7 77.4935 53.5251 21 11 7 8 150.030 63.6833 27 11 7 8 265.543 83.7795 21 11 7 9 272.924 75.0679 27 11 7 9 400.395 86.6364 21 11 7 10 2547.49 192.862 27 11 7 10 2384.82 186.945 21 11 7 11 19.2124 42.6856 21 11 7 12 237.333 67.7913 21 11 7 13 553.819 85.4525 21 11 7 14 305.702 64.2928 31 11 7 14 376.022 68.3555 21 -11 -8 12 470.443 83.0532 29 -11 -8 12 349.182 72.3826 23 -11 -8 11 327.332 81.8356 29 -11 -8 11 413.394 85.1675 23 -11 -8 10 105.015 62.8882 29 -11 -8 10-18.0146 48.9818 23 -11 -8 9 88.3630 56.6322 29 -11 -8 9 148.583 71.0701 23 -11 -8 8 177.582 71.1253 29 -11 -8 8 201.440 75.6099 23 -11 -8 7 250.926 78.2708 29 -11 -8 7 288.531 81.9275 23 -11 -8 6 418.037 96.5190 29 -11 -8 6 421.812 99.8253 23 -11 -8 5 146.804 71.4897 29 -11 -8 5 101.467 71.9076 23 -11 -8 4 169.160 81.3170 23 -11 -8 3 53.3131 53.5753 23 -11 -8 2 859.792 135.191 23 -11 -8 1-57.3537 70.9318 23 11 8 0 239.462 71.7986 27 -11 -8 0 522.603 109.831 23 11 8 1 299.999 82.8328 27 -11 -8 -1 228.264 85.4101 23 11 8 1 214.203 84.0679 21 11 8 2 2038.18 189.221 27 11 8 2 1889.42 185.590 21 -11 -8 -2 2181.89 202.724 23 11 8 3 58.3594 47.4151 27 -11 -8 -3 101.184 67.7009 23 11 8 3 47.8250 59.3314 21 11 8 4 146.869 66.1182 27 11 8 4 26.9078 50.9350 21 11 8 5 112.864 63.8873 27 11 8 5 13.3232 55.9989 21 11 8 6 446.355 102.137 27 11 8 6 360.111 85.8498 21 11 8 7 160.027 69.1714 27 11 8 7 121.025 57.9383 21 11 8 8 1310.88 150.162 27 11 8 8 1325.88 148.178 21 11 8 9 348.524 83.0104 27 11 8 9 401.951 90.9208 21 11 8 10-23.7288 53.2989 21 11 8 11 336.248 78.8431 21 11 8 12 104.901 53.3750 21 11 8 13-36.3366 41.1444 21 11 8 14 386.585 63.5437 31 11 8 14 323.245 62.1806 21 -11 -9 11 164.271 61.0881 29 -11 -9 11 71.7755 47.5261 23 -11 -9 10 232.207 70.6848 29 -11 -9 10 99.5483 47.7680 23 -11 -9 9-13.8746 53.9670 29 -11 -9 9 66.0459 58.6922 23 -11 -9 8 283.935 79.9140 29 -11 -9 8 293.118 82.9078 23 -11 -9 7 3352.82 224.192 29 -11 -9 7 3121.22 200.263 32 -11 -9 7 3078.38 214.583 23 -11 -9 6 684.359 111.398 29 -11 -9 6 607.515 111.447 23 -11 -9 5 251.919 76.0757 29 -11 -9 5 206.072 77.7577 23 -11 -9 4 167.558 69.8987 29 -11 -9 4 101.857 73.1682 23 -11 -9 3 93.8791 67.8071 23 -11 -9 2 51.6020 63.1681 23 11 9 -1 1853.50 170.859 21 -11 -9 1 1951.98 191.661 23 -11 -9 0 1340.74 159.771 23 11 9 0 1586.74 164.050 21 11 9 1 18.1368 35.2445 27 -11 -9 -1 84.2779 68.9545 23 11 9 2 170.413 57.0028 27 -11 -9 -2 280.145 87.4871 23 11 9 2 224.073 76.2038 21 11 9 3 131.351 71.1463 27 -11 -9 -3 152.243 73.2029 23 11 9 3 167.478 61.3700 21 11 9 4 1144.24 137.540 27 -11 -9 -4 1190.92 151.178 23 11 9 4 1445.68 156.628 21 11 9 5 514.853 98.0088 27 11 9 5 483.652 95.6678 21 11 9 6 200.872 66.5127 27 11 9 6 210.901 75.1062 21 -11 -9 -7 398.799 90.1979 32 11 9 7 401.330 87.3496 27 11 9 7 173.704 62.4453 21 -11 -9 -8 778.608 112.717 32 11 9 8 807.768 119.245 21 11 9 9 176.752 68.9069 21 11 9 10 32.4400 49.2082 21 11 9 11 164.555 55.9934 21 11 9 12 12.7374 42.7758 21 11 9 13 362.071 67.3045 21 11 9 14 14.9422 31.2590 21 -11 -10 10 2159.30 142.165 23 -11 -10 9-48.1235 47.5358 23 -11 -10 8 2023.44 159.249 23 -11 -10 7 270.311 78.0240 23 -11 -10 6 2562.73 177.320 32 -11 -10 6 2444.86 190.393 23 -11 -10 5 118.096 53.0931 32 -11 -10 5 94.1706 68.4451 23 -11 -10 4 795.228 112.180 32 -11 -10 4 853.915 126.945 23 -11 -10 3 77.6559 50.3221 32 -11 -10 3-36.8880 54.8525 23 -11 -10 2 177.845 70.2460 32 -11 -10 2 83.7389 60.2729 23 -11 -10 1 1739.00 174.922 23 -11 -10 0 1474.62 167.024 23 -11 -10 -1 1047.33 147.036 23 -11 -10 -2 3099.94 231.448 32 -11 -10 -2 3043.82 234.150 23 -11 -10 -3 1152.62 146.626 32 -11 -10 -3 1081.93 142.624 23 11 10 3 1345.75 140.538 21 -11 -10 -4 1006.52 139.337 32 -11 -10 -4 708.517 114.622 23 11 10 4 916.670 117.824 21 -11 -10 -5 56.3292 56.3111 32 11 10 5 47.0093 52.8687 21 -11 -10 -6 809.815 118.310 32 11 10 6 791.451 110.186 21 -11 -10 -7 294.016 72.7004 32 11 10 7 109.049 50.7466 21 -11 -10 -8 1017.48 126.634 32 11 10 8 819.993 107.022 21 11 10 9 188.340 61.3230 21 11 10 10 171.094 52.5427 21 11 10 11 304.030 66.7190 21 11 10 12 820.531 94.5445 21 11 10 13 8.46060 34.9007 21 -11 -11 8 11.5809 38.4420 23 -11 -11 7 16.4203 46.7178 23 -11 -11 6 809.009 106.025 23 -11 -11 5-19.8541 41.3573 32 -11 -11 5 47.9780 52.5679 23 -11 -11 4 18.2898 41.3691 32 -11 -11 4 62.0653 59.4959 23 -11 -11 3 357.734 79.9977 32 -11 -11 3 250.980 79.2854 23 -11 -11 2 902.329 114.783 32 -11 -11 2 1110.22 135.114 23 -11 -11 1 72.3071 55.0768 32 -11 -11 1 90.9290 73.3374 23 -11 -11 0-6.11723 48.2265 32 -11 -11 0 4.10669 60.5230 23 -11 -11 -1 85.7317 60.8265 32 -11 -11 -1 160.903 75.3555 23 -11 -11 -2 230.255 85.3701 32 -11 -11 -2 67.0877 56.9173 23 -11 -11 -3 182.476 69.4438 32 -11 -11 -4 908.070 124.170 32 -11 -11 -5 954.627 126.164 32 -11 -11 -6 293.806 77.7739 32 11 11 6 329.630 65.9272 21 -11 -11 -7 100.461 53.7025 32 11 11 7 55.2375 33.8836 21 -11 -11 -8 501.732 84.0901 32 11 11 8 488.786 77.2514 21 11 11 9 348.395 64.7617 21 11 11 10 207.575 54.6369 21 11 11 11 115.063 43.1939 21 -11 -12 5-4.80348 44.5913 23 -11 -12 4 30.9566 32.7028 32 -11 -12 4 35.0509 39.6144 23 -11 -12 3 479.353 78.5475 32 -11 -12 3 364.183 73.0873 23 -11 -12 2 269.750 61.1627 32 -11 -12 2 138.725 53.6190 23 -11 -12 1 220.059 61.8242 32 -11 -12 0 318.801 75.9341 32 -11 -12 -1-11.0588 42.5429 32 -11 -12 -2 454.898 86.2907 32 -11 -12 -3 161.773 61.9879 32 -11 -12 -4 68.3912 52.8139 32 -11 -12 -5 1106.86 119.762 32 -11 -12 -6-20.3785 40.5418 32 -11 -12 -7 21.2075 42.8656 32 -11 -12 -8-29.2205 41.7011 32 11 12 9 132.551 43.1455 25 -12 0 5-124.120 55.6586 26 -12 0 4-3.19806 43.9952 26 -12 0 3 350.996 74.6601 26 -12 0 2 108.664 52.0024 26 12 0 -1 124.422 42.1414 34 -12 0 1 332.439 70.4160 26 12 0 0 17.0597 32.5885 34 -12 0 0-37.7763 38.6803 26 12 0 1-14.4223 29.2056 34 -12 -1 8 150.207 59.8461 26 -12 -1 7 415.375 80.9394 26 -12 -1 6 66.7530 50.6662 26 -12 -1 5 12.4293 49.2371 26 -12 -1 4 301.823 78.3507 26 -12 -1 3 107.653 62.5111 26 -12 -1 2 209.946 66.2620 26 12 1 -1 175.671 54.2874 34 -12 -1 1 138.461 68.2677 26 12 1 0 195.093 56.8319 34 -12 -1 0 230.163 71.9618 26 12 1 1 644.114 93.5008 34 -12 -1 -1 808.776 115.939 26 12 1 2 106.611 51.5859 34 12 1 3 6.05875 36.7831 34 12 1 4 320.943 65.0481 34 12 1 4 326.616 61.1179 27 12 1 5 50.0027 46.7284 34 12 1 5-50.6548 39.5152 27 -12 -2 10 421.817 73.5902 26 -12 -2 9 196.559 62.1047 26 -12 -2 8 10.2567 46.6360 26 -12 -2 7 298.672 76.5495 26 -12 -2 6 54.0406 57.7690 26 -12 -2 5 255.255 72.5976 26 -12 -2 4 229.127 74.8590 26 -12 -2 3 153.510 64.3097 26 -12 -2 2 16.4112 54.0181 26 -12 -2 1 260.638 83.3086 26 12 2 0 602.372 89.0787 34 -12 -2 0 769.411 123.603 26 12 2 1 64.6261 38.4911 34 -12 -2 -1 87.7957 67.4923 26 12 2 2 375.894 78.3726 34 -12 -2 -2 376.776 93.3894 26 12 2 3 654.437 98.5408 34 12 2 4 851.438 109.670 34 12 2 5 201.266 62.0112 34 12 2 5 298.300 65.6865 27 12 2 6 7.84735 33.3483 27 12 2 6 84.7626 45.1776 34 12 2 7 15.5319 39.1666 34 12 2 8 816.814 94.2882 34 -12 -3 11 88.8864 42.1026 26 -12 -3 11-29.7300 34.0814 23 -12 -3 10 545.382 82.0564 26 -12 -3 10 536.092 78.9766 23 -12 -3 9 72.1134 47.0311 26 -12 -3 9 43.7421 34.5624 23 -12 -3 8 75.1266 53.9712 26 -12 -3 8 15.5860 36.0951 23 -12 -3 7 25.4334 48.0260 26 -12 -3 6 239.207 79.6550 26 -12 -3 5 54.7747 50.2938 26 -12 -3 4 1245.99 150.938 26 -12 -3 3 741.913 122.590 26 -12 -3 2 196.093 77.3164 26 -12 -3 1-7.76025 57.6317 26 -12 -3 0 1689.00 178.920 26 12 3 1-19.1378 38.1464 34 -12 -3 -1-70.1640 72.1771 26 12 3 2-24.0347 37.6922 34 -12 -3 -2-46.8876 64.7165 26 12 3 3 83.6244 57.7096 34 -12 -3 -3-27.1226 66.1678 26 12 3 3 103.899 56.9607 21 12 3 4 124.095 57.8436 34 12 3 4 126.016 48.8319 21 12 3 5 1698.51 157.901 34 12 3 5 1541.87 144.819 27 12 3 5 1472.60 127.724 21 12 3 6 181.454 63.6375 34 12 3 6 47.0508 37.8207 27 12 3 7-47.9575 42.4762 27 12 3 7 93.7001 48.2984 34 12 3 8 1739.63 143.709 31 12 3 8 1570.43 119.213 27 12 3 9 376.407 72.0780 34 12 3 9 427.882 74.1756 31 -12 -4 11 9.33405 32.7571 29 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27 12 4 9 3.10385 40.5423 34 12 4 10 628.986 72.0354 27 12 4 10 812.503 100.143 34 12 4 10 752.876 98.6646 31 -12 -5 12-42.7043 33.6793 29 -12 -5 12 23.6299 39.9067 23 -12 -5 11 283.396 62.5011 29 -12 -5 11 272.387 64.3478 23 -12 -5 10 383.066 72.3040 29 -12 -5 10 351.341 71.2385 23 -12 -5 9 139.879 58.2082 23 -12 -5 8 353.208 80.5367 23 -12 -5 7 132.664 56.1184 26 -12 -5 7 116.991 60.9699 23 -12 -5 6 705.205 108.130 26 -12 -5 6 894.055 117.608 23 -12 -5 5 669.745 109.624 26 -12 -5 5 478.492 94.6354 23 -12 -5 4 215.321 76.7604 26 -12 -5 3 80.2855 62.3170 26 -12 -5 2 853.713 132.484 26 -12 -5 1 947.531 140.846 26 -12 -5 0 282.485 85.2953 26 -12 -5 -1 890.682 145.016 26 12 5 2 114.566 52.2454 34 -12 -5 -2-63.8065 69.6501 26 12 5 3 1006.19 124.079 34 12 5 3 1105.98 142.123 27 12 5 3 1017.75 133.122 21 12 5 4 401.459 89.3116 34 12 5 4 440.819 98.6514 27 12 5 4 524.815 102.817 21 12 5 5 451.158 96.3661 34 12 5 5 258.704 82.4823 27 12 5 5 200.807 69.4794 21 12 5 6 67.3806 51.2844 34 12 5 6 81.1312 58.3557 27 12 5 6 34.3810 45.9350 21 12 5 7 1271.66 144.368 34 12 5 7 1608.52 149.428 27 12 5 7 1391.60 135.912 21 12 5 8 240.220 64.9988 27 12 5 8 292.140 77.7799 34 12 5 8 144.199 49.5448 21 12 5 9 566.219 86.2650 27 12 5 9 507.042 88.1928 34 12 5 9 699.726 90.8991 21 12 5 10 45.4760 33.1511 27 12 5 10 120.586 39.4708 21 12 5 11-2.07302 35.8120 31 -12 -6 11 498.708 79.1585 29 -12 -6 11 374.112 75.6395 23 -12 -6 10 317.417 67.2112 29 -12 -6 10 200.697 58.6480 23 -12 -6 9 306.808 68.0184 29 -12 -6 9 356.879 77.0030 23 -12 -6 8 94.7146 47.9036 23 -12 -6 7 111.285 61.1195 23 -12 -6 6 348.632 80.7871 23 -12 -6 5 2007.26 172.941 26 -12 -6 5 1889.77 169.489 23 -12 -6 4 371.223 83.0939 26 -12 -6 4 395.287 85.8340 23 -12 -6 3 884.442 126.128 26 -12 -6 3 1063.67 130.586 23 -12 -6 2 727.577 123.511 26 -12 -6 1 211.256 75.8924 26 -12 -6 0 1016.14 144.869 26 12 6 1 695.790 115.892 27 12 6 2 315.211 87.3408 27 12 6 3 164.757 65.0047 34 12 6 3 18.6392 47.2583 27 12 6 3 28.1371 49.8469 21 12 6 4 70.1052 44.9939 34 12 6 4 69.7282 49.3205 27 12 6 4 58.5861 56.2495 21 12 6 5 15.8632 40.2143 34 12 6 5 44.6422 60.0789 27 12 6 5 52.8844 64.3141 21 12 6 6 780.627 114.789 27 12 6 6 1011.77 131.794 34 12 6 6 755.434 111.690 21 12 6 7 74.3334 51.0594 27 12 6 7 52.0548 48.7019 34 12 6 7-23.6279 42.9735 21 12 6 8 468.172 88.8200 27 12 6 8 469.471 83.3935 21 12 6 9 400.850 76.2635 27 12 6 9 342.569 69.4845 21 12 6 10 177.676 56.8761 27 12 6 10 113.492 48.1036 21 12 6 11 130.598 44.5826 21 12 6 12 3.72623 30.6357 31 12 6 12 58.1034 28.5295 21 -12 -7 11 148.905 48.4528 29 -12 -7 11 0.89544 37.5479 23 -12 -7 10 25.9588 43.1925 29 -12 -7 10 13.3290 44.4455 23 -12 -7 9 12.7761 45.7969 29 -12 -7 9 16.3627 48.1199 23 -12 -7 8-31.6997 41.6615 29 -12 -7 8-55.5366 54.8186 23 -12 -7 7 50.1709 51.5981 23 -12 -7 6 251.321 76.8364 23 -12 -7 5 69.3083 57.3044 23 -12 -7 4 726.123 113.593 23 -12 -7 3 388.509 90.5904 23 12 7 -2 247.054 66.9850 27 -12 -7 2 211.732 69.9018 23 12 7 -1 1219.38 137.147 27 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1043.47 119.353 21 -12 -9 1-15.6774 45.8400 23 12 9 -1-47.4480 50.9044 21 -12 -9 0-29.0902 47.9543 23 12 9 0 140.758 60.3705 21 12 9 1 523.614 85.4896 27 -12 -9 -1 306.297 82.7635 23 12 9 1 286.384 75.4545 21 12 9 2 172.067 57.5284 27 -12 -9 -2 175.028 72.5630 23 12 9 2 113.806 53.9071 21 12 9 3 141.322 54.8298 27 12 9 3 60.2162 45.5035 21 12 9 4 66.4027 56.7766 27 12 9 4 15.2550 45.0907 21 12 9 5 446.572 81.8358 27 12 9 5 382.392 77.5839 21 -12 -9 -6-80.1639 56.7791 32 12 9 6 57.3133 49.1807 27 12 9 6 49.9328 42.3210 21 -12 -9 -7-72.3990 43.7929 32 12 9 7 44.7450 50.0658 21 12 9 8 683.791 96.2152 21 12 9 9 270.713 64.2950 21 12 9 10 24.8890 32.9926 21 12 9 11 238.893 56.5965 21 -12 -10 7 133.093 50.5209 23 -12 -10 6 245.549 53.6954 32 -12 -10 6 299.449 71.0740 23 -12 -10 5 293.753 65.8771 32 -12 -10 5 143.071 53.1428 23 -12 -10 4 35.3550 37.3241 32 -12 -10 4 17.9752 45.3484 23 -12 -10 3 156.423 59.7913 32 -12 -10 3 244.368 78.9916 23 -12 -10 2 411.251 85.9057 32 -12 -10 2 390.214 91.0289 23 -12 -10 1 280.417 75.1450 32 -12 -10 1 197.041 68.2436 23 -12 -10 0 386.079 84.9553 32 -12 -10 0 221.613 73.4112 23 -12 -10 -1 188.458 66.1901 32 -12 -10 -1 164.511 64.4709 23 12 10 1 126.963 45.7135 21 -12 -10 -2 331.298 79.0483 32 -12 -10 -2 358.940 81.1668 23 12 10 2 305.662 66.4141 21 -12 -10 -3 1707.26 158.456 32 12 10 3 1966.46 153.932 21 -12 -10 -3 1723.01 156.709 23 -12 -10 -4 156.795 65.5458 32 12 10 4 58.1793 37.0763 21 -12 -10 -5-4.27722 42.0895 32 12 10 5 15.2291 35.1022 21 -12 -10 -6 671.461 94.7607 32 12 10 6 628.855 92.1549 21 -12 -10 -7 553.033 85.9284 32 12 10 7 490.830 79.5716 21 12 10 8 122.604 47.5732 21 12 10 9 96.0338 39.9702 21 12 10 10-65.7087 42.4312 21 -12 -11 5 17.5085 30.7431 32 -12 -11 5-53.7537 46.6368 23 -12 -11 4 27.9362 37.3218 32 -12 -11 4-7.33207 39.9860 23 -12 -11 3 687.650 91.3618 32 -12 -11 3 697.245 95.9885 23 -12 -11 2 92.7204 50.9436 32 -12 -11 2 45.1367 46.4220 23 -12 -11 1 74.7576 52.8321 32 -12 -11 1-29.0499 49.7100 23 -12 -11 0 9.72680 43.9265 32 -12 -11 0-23.0781 49.8659 23 -12 -11 -1 111.078 55.1569 32 -12 -11 -1 73.3935 51.1726 23 -12 -11 -2 98.9871 57.1868 32 -12 -11 -3 56.1694 47.0035 32 -12 -11 -4 25.0530 46.2744 32 -12 -11 -5 284.287 67.7854 32 12 11 5 395.475 64.5969 21 -12 -11 -6 491.437 79.6138 32 12 11 6 436.670 66.2384 21 -12 -11 -7 188.705 51.9072 32 12 11 7 219.509 49.6501 21 12 11 8 267.659 53.1029 21 -12 -12 -1 973.708 101.899 32 -12 -12 -2 184.490 53.4782 32 -12 -12 -3 203.476 58.6725 32 -13 -3 5 340.450 66.2441 26 -13 -3 4 454.069 81.4692 26 -13 -3 3 29.4527 42.3364 26 -13 -3 2-18.7297 45.7241 26 -13 -3 1 158.649 65.4812 26 -13 -3 0-0.97527 46.5896 26 13 3 0-0.74794 33.5656 21 13 3 1 18.9926 35.4391 21 13 3 2 13.6215 26.7530 34 13 3 2 55.9901 38.9849 27 13 3 2 17.0421 26.6090 21 13 3 3 508.420 70.5807 34 13 3 3 528.548 75.6828 27 -13 -4 7 130.767 50.6199 26 -13 -4 6 13.5611 39.1374 26 -13 -4 5 161.287 54.4349 26 -13 -4 4 21.0339 43.1778 26 -13 -4 3 34.3529 48.3661 26 -13 -4 2-5.89261 44.3590 26 -13 -4 1 80.7961 56.7351 26 -13 -4 0 825.747 117.312 26 13 4 1 65.8217 45.9976 27 13 4 1 7.08689 42.4520 21 13 4 2 336.055 71.9494 27 13 4 2 463.097 75.8574 21 13 4 3 338.335 63.2098 34 13 4 3 335.675 72.1561 27 13 4 3 330.628 63.0658 21 13 4 4-85.8940 40.5270 34 13 4 4-13.0962 32.5221 27 13 4 4-13.3344 39.4700 21 13 4 5 62.7518 39.2850 27 13 4 5 23.1056 30.8281 34 13 4 5 27.8501 27.3636 21 13 4 6 27.9451 32.3395 27 13 4 6-16.0435 28.1228 34 13 4 6 59.0560 40.5325 31 -13 -5 8 730.805 79.4198 23 -13 -5 7-3.23516 35.9015 26 -13 -5 7 103.163 49.3088 23 -13 -5 6 556.829 82.7791 26 13 5 -5 132.606 41.7363 27 -13 -5 5 107.187 53.0310 26 -13 -5 4 874.745 111.175 26 -13 -5 3-17.2901 49.5958 26 -13 -5 2 841.754 115.255 26 13 5 -1-24.7649 46.0276 27 -13 -5 1 70.0239 51.1605 26 13 5 0 487.814 87.3730 27 13 5 1 415.570 78.6050 27 13 5 1 189.308 61.4810 21 13 5 2 52.3749 38.5144 27 13 5 2 64.9962 52.6761 21 13 5 3 135.964 46.3260 34 13 5 3 97.1253 42.3673 27 13 5 3 93.1358 46.8300 21 13 5 4 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13 9 7 168.822 52.3696 21 -13 -10 2 44.4446 39.2073 32 -13 -10 2 43.9229 37.4666 23 -13 -10 1 12.7760 36.5341 32 -13 -10 1 18.4287 35.7211 23 -13 -10 0-46.5619 39.9484 32 -13 -10 0-27.9831 42.9242 23 -13 -10 -1 482.677 78.7765 32 13 10 1 575.520 73.1350 21 -13 -10 -2 183.544 54.0350 32 13 10 2 242.000 51.4827 21 -13 -10 -3 1734.61 134.357 32 13 10 3 1693.02 123.865 21 -13 -10 -4 113.646 46.3600 32 13 10 4 94.5303 37.0309 21 -13 -10 -5 90.7873 39.1021 32 13 10 5 132.508 45.1031 21 0 0 0 0.00 0.00 0 TITL WLL149 in P-1 REM P-1 (#2 in standard setting) CELL 1.54184 11.555433 11.904100 20.621576 81.9998 89.7919 61.5825 ZERR 7.00 0.000388 0.000407 0.000649 0.0027 0.0026 0.0035 LATT 1 SFAC C H N O UNIT 98.00 105.00 14.00 28.00 TREF HKLF 4 END ; _shelx_hkl_checksum 96526 _shelx_fab_file ; 0 0 3 -18.15 0.00 0 0 4 33.70 0.00 0 0 5 -19.85 0.00 0 0 6 18.58 0.00 0 0 7 -8.47 0.00 0 0 8 12.63 0.00 0 0 9 -0.24 0.00 0 0 10 6.48 0.00 0 0 11 1.47 0.00 0 0 12 1.17 0.00 0 0 13 1.59 0.00 0 0 14 -1.26 0.00 0 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-0.26 0.00 -5 -5 23 0.09 0.00 -4 -5 23 0.07 0.00 -3 -5 23 -0.50 0.00 -2 -5 23 0.31 0.00 -1 -5 23 -0.22 0.00 0 -5 23 0.32 0.00 -7 -4 23 0.23 0.00 -6 -4 23 -0.14 0.00 -5 -4 23 0.57 0.00 -4 -4 23 -0.38 0.00 -3 -4 23 0.03 0.00 -2 -4 23 -0.06 0.00 -1 -4 23 -0.26 0.00 0 -4 23 0.17 0.00 1 -4 23 0.13 0.00 2 -4 23 -0.13 0.00 -7 -3 23 0.13 0.00 -6 -3 23 0.01 0.00 -5 -3 23 0.33 0.00 -4 -3 23 -0.32 0.00 -1 -3 23 -0.07 0.00 0 -3 23 -0.11 0.00 1 -3 23 0.35 0.00 2 -3 23 -0.20 0.00 3 -3 23 0.02 0.00 -7 -2 23 0.04 0.00 -6 -2 23 0.15 0.00 -5 -2 23 -0.15 0.00 2 -2 23 0.10 0.00 3 -2 23 0.45 0.00 4 -2 23 -0.02 0.00 -7 -1 23 0.40 0.00 -6 -1 23 0.12 0.00 -5 -1 23 0.17 0.00 3 -1 23 0.65 0.00 4 -1 23 0.00 0.00 5 -1 23 0.23 0.00 -7 0 23 0.29 0.00 -6 0 23 -0.17 0.00 -5 0 23 0.28 0.00 4 0 23 0.08 0.00 5 0 23 0.32 0.00 -7 1 23 0.05 0.00 -6 1 23 0.01 0.00 -5 1 23 0.30 0.00 4 1 23 -0.01 0.00 5 1 23 0.12 0.00 6 1 23 0.20 0.00 -6 2 23 0.16 0.00 -5 2 23 0.09 0.00 5 2 23 -0.17 0.00 6 2 23 -0.13 0.00 7 2 23 -0.09 0.00 -6 3 23 -0.05 0.00 -5 3 23 -0.23 0.00 -4 3 23 -0.07 0.00 5 3 23 -0.06 0.00 6 3 23 -0.28 0.00 7 3 23 0.03 0.00 -5 4 23 0.04 0.00 -4 4 23 0.26 0.00 -3 4 23 -0.22 0.00 5 4 23 -0.09 0.00 6 4 23 -0.22 0.00 7 4 23 0.26 0.00 -4 5 23 0.02 0.00 -3 5 23 -0.12 0.00 -2 5 23 0.08 0.00 4 5 23 -0.63 0.00 5 5 23 -0.48 0.00 6 5 23 -0.21 0.00 7 5 23 0.09 0.00 -3 6 23 -0.10 0.00 -2 6 23 -0.18 0.00 -1 6 23 -0.03 0.00 5 6 23 -0.65 0.00 6 6 23 -0.12 0.00 7 6 23 -0.14 0.00 -2 7 23 -0.26 0.00 -1 7 23 -0.01 0.00 0 7 23 -0.20 0.00 1 7 23 0.07 0.00 2 7 23 -0.13 0.00 3 7 23 -0.31 0.00 4 7 23 -0.16 0.00 5 7 23 -0.44 0.00 6 7 23 -0.05 0.00 7 7 23 -0.25 0.00 -1 8 23 -0.18 0.00 0 8 23 -0.38 0.00 1 8 23 0.01 0.00 2 8 23 -0.38 0.00 3 8 23 -0.18 0.00 4 8 23 0.04 0.00 5 8 23 -0.24 0.00 6 8 23 0.26 0.00 7 8 23 -0.08 0.00 1 9 23 -0.03 0.00 2 9 23 -0.26 0.00 3 9 23 -0.10 0.00 4 9 23 0.08 0.00 5 9 23 -0.13 0.00 6 9 23 0.43 0.00 -4 -5 24 -0.05 0.00 -3 -5 24 -0.06 0.00 -5 -4 24 0.13 0.00 -4 -4 24 -0.17 0.00 -3 -4 24 0.09 0.00 -2 -4 24 0.25 0.00 -1 -4 24 0.03 0.00 0 -4 24 -0.09 0.00 -6 -3 24 -0.08 0.00 -5 -3 24 0.03 0.00 -4 -3 24 -0.21 0.00 -3 -3 24 0.27 0.00 -2 -3 24 -0.03 0.00 -1 -3 24 0.20 0.00 0 -3 24 -0.08 0.00 1 -3 24 0.15 0.00 2 -3 24 -0.17 0.00 -6 -2 24 0.05 0.00 -5 -2 24 0.03 0.00 -4 -2 24 0.02 0.00 -3 -2 24 0.08 0.00 -2 -2 24 -0.01 0.00 -1 -2 24 -0.21 0.00 0 -2 24 -0.34 0.00 1 -2 24 0.00 0.00 2 -2 24 -0.65 0.00 3 -2 24 0.05 0.00 -6 -1 24 -0.26 0.00 -5 -1 24 -0.15 0.00 -4 -1 24 -0.05 0.00 -3 -1 24 -0.15 0.00 0 -1 24 -0.15 0.00 1 -1 24 -0.18 0.00 2 -1 24 -0.56 0.00 3 -1 24 -0.01 0.00 4 -1 24 -0.32 0.00 -6 0 24 -0.27 0.00 -5 0 24 0.23 0.00 -4 0 24 -0.14 0.00 2 0 24 -0.33 0.00 3 0 24 -0.05 0.00 4 0 24 -0.37 0.00 -6 1 24 -0.19 0.00 -5 1 24 0.20 0.00 -4 1 24 -0.31 0.00 3 1 24 -0.26 0.00 4 1 24 -0.12 0.00 5 1 24 -0.10 0.00 -5 2 24 -0.12 0.00 -4 2 24 -0.19 0.00 -3 2 24 0.14 0.00 3 2 24 0.03 0.00 4 2 24 0.22 0.00 5 2 24 0.27 0.00 6 2 24 0.10 0.00 -5 3 24 -0.05 0.00 -4 3 24 0.23 0.00 -3 3 24 0.17 0.00 4 3 24 0.21 0.00 5 3 24 0.32 0.00 6 3 24 -0.01 0.00 -4 4 24 0.02 0.00 -3 4 24 -0.25 0.00 -2 4 24 0.31 0.00 4 4 24 0.17 0.00 5 4 24 0.20 0.00 6 4 24 -0.10 0.00 -3 5 24 -0.07 0.00 -2 5 24 0.23 0.00 -1 5 24 -0.04 0.00 0 5 24 0.48 0.00 3 5 24 0.53 0.00 4 5 24 0.52 0.00 5 5 24 0.24 0.00 6 5 24 0.11 0.00 -2 6 24 0.09 0.00 -1 6 24 -0.04 0.00 0 6 24 0.22 0.00 1 6 24 0.07 0.00 2 6 24 0.57 0.00 3 6 24 0.49 0.00 4 6 24 0.56 0.00 5 6 24 0.36 0.00 6 6 24 0.08 0.00 -1 7 24 0.15 0.00 0 7 24 0.00 0.00 1 7 24 0.12 0.00 2 7 24 0.14 0.00 3 7 24 0.11 0.00 4 7 24 0.34 0.00 5 7 24 0.22 0.00 6 7 24 0.13 0.00 0 8 24 0.16 0.00 1 8 24 0.30 0.00 2 8 24 0.04 0.00 3 8 24 0.10 0.00 4 8 24 0.19 0.00 5 8 24 -0.13 0.00 -4 -3 25 -0.04 0.00 -3 -3 25 -0.05 0.00 -2 -3 25 -0.15 0.00 -1 -3 25 -0.12 0.00 0 -3 25 -0.27 0.00 -5 -2 25 -0.17 0.00 -4 -2 25 0.03 0.00 -3 -2 25 -0.02 0.00 -2 -2 25 -0.01 0.00 -1 -2 25 0.17 0.00 0 -2 25 0.03 0.00 1 -2 25 0.38 0.00 -5 -1 25 0.13 0.00 -4 -1 25 0.06 0.00 -3 -1 25 0.07 0.00 -2 -1 25 0.07 0.00 -1 -1 25 -0.10 0.00 0 -1 25 0.25 0.00 1 -1 25 0.25 0.00 2 -1 25 -0.01 0.00 -5 0 25 0.14 0.00 -4 0 25 -0.17 0.00 -3 0 25 0.05 0.00 -2 0 25 0.10 0.00 -1 0 25 -0.09 0.00 0 0 25 0.22 0.00 1 0 25 0.08 0.00 2 0 25 0.23 0.00 3 0 25 0.20 0.00 -5 1 25 0.16 0.00 -4 1 25 -0.24 0.00 -3 1 25 0.17 0.00 -2 1 25 0.05 0.00 -1 1 25 0.26 0.00 0 1 25 0.41 0.00 1 1 25 0.32 0.00 2 1 25 0.56 0.00 3 1 25 0.21 0.00 4 1 25 0.10 0.00 -4 2 25 -0.05 0.00 -3 2 25 0.18 0.00 -2 2 25 -0.14 0.00 -1 2 25 0.08 0.00 0 2 25 0.21 0.00 1 2 25 0.19 0.00 2 2 25 0.23 0.00 3 2 25 0.02 0.00 4 2 25 -0.14 0.00 5 2 25 -0.26 0.00 -4 3 25 0.07 0.00 -3 3 25 -0.19 0.00 -2 3 25 -0.21 0.00 -1 3 25 -0.33 0.00 0 3 25 -0.29 0.00 1 3 25 -0.09 0.00 2 3 25 -0.10 0.00 3 3 25 -0.01 0.00 4 3 25 -0.21 0.00 5 3 25 -0.21 0.00 -3 4 25 -0.08 0.00 -2 4 25 0.12 0.00 -1 4 25 -0.21 0.00 0 4 25 -0.23 0.00 1 4 25 -0.14 0.00 2 4 25 -0.06 0.00 3 4 25 -0.05 0.00 4 4 25 -0.12 0.00 5 4 25 -0.13 0.00 -2 5 25 0.13 0.00 -1 5 25 -0.30 0.00 0 5 25 -0.06 0.00 1 5 25 -0.40 0.00 2 5 25 -0.29 0.00 3 5 25 -0.28 0.00 4 5 25 -0.32 0.00 5 5 25 -0.16 0.00 -1 6 25 -0.11 0.00 0 6 25 0.05 0.00 1 6 25 -0.28 0.00 2 6 25 -0.26 0.00 3 6 25 -0.43 0.00 4 6 25 -0.36 0.00 5 6 25 -0.23 0.00 0 7 25 -0.03 0.00 1 7 25 -0.13 0.00 2 7 25 -0.07 0.00 3 7 25 -0.27 0.00 4 7 25 -0.15 0.00 0 0 0 0.00 0.00 # SQUEEZE RESULTS (Version = 91117) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.001 0.500 194 39 ' ' 2 0.500 0.000 0.000 211 43 ' ' 3 0.500 0.500 0.500 26 -1 ' ' # Missing Reflections Below sin(th)/lambda = 0.25 loop_ _platon_missing_refln_index_h _platon_missing_refln_index_k _platon_missing_refln_index_l _platon_missing_refln_theta 0 0 1 2.169 0 0 2 4.341 _platon_squeeze_void_probe_radius 1.20 _platon_squeeze_details ) TITL CF solution in P-1 CELL 11.5554 11.9041 20.6216 82.00 89.79 61.58 SPGR P-1 # Solvent Accessible Volume = 429 # Electrons Found in S.A.V. = 81 # Note: Atoms in Void are Labelled as Cxxx and Qxxx for all Others C101 0.016 0.998 0.502 ! 4.30 eA-3 C102 0.453 0.136 0.004 ! 3.54 eA-3 C103 0.483 0.021 0.026 ! 3.13 eA-3 C104 0.486 0.945 0.093 ! 2.92 eA-3 C105 0.939 0.176 0.468 ! 2.81 eA-3 C106 0.140 0.027 0.469 ! 2.78 eA-3 C107 0.016 0.227 0.467 ! 1.85 eA-3 Q108 0.611 0.130 0.390 ! 0.83 eA-3 Q109 0.309 0.449 0.108 ! 0.77 eA-3 Q110 0.500 0.283 0.323 ! 0.74 eA-3 Q111 0.670 0.046 0.484 ! 0.70 eA-3 Q112 0.293 0.530 0.188 ! 0.68 eA-3 Q113 0.294 0.196 0.424 ! 0.62 eA-3 Q114 0.455 0.680 0.078 ! 0.62 eA-3 Q115 0.017 0.741 0.190 ! 0.61 eA-3 Q116 0.405 0.446 0.411 ! 0.61 eA-3 Q117 0.422 0.069 0.363 ! 0.59 eA-3 Q118 0.561 0.408 0.236 ! 0.59 eA-3 Q119 0.466 0.335 0.058 ! 0.58 eA-3 Q120 0.922 0.941 0.264 ! 0.57 eA-3 Q121 0.639 0.440 0.063 ! 0.56 eA-3 Q122 0.255 0.692 0.065 ! 0.56 eA-3 Q123 0.263 0.057 0.327 ! 0.55 eA-3 Q124 0.859 0.976 0.155 ! 0.55 eA-3 Q125 0.949 0.620 0.421 ! 0.53 eA-3 Q126 0.060 0.421 0.232 ! 0.53 eA-3 Q127 0.799 0.917 0.393 ! 0.52 eA-3 Q128 0.236 0.880 0.012 ! 0.52 eA-3 Q129 0.221 0.394 0.046 ! 0.51 eA-3 Q130 0.814 0.069 0.375 ! 0.51 eA-3 Q131 0.074 0.010 0.327 ! 0.50 eA-3 ) ; _shelx_fab_checksum 46070 _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; _oxdiff_exptl_absorpt_empirical_full_max 2.086 _oxdiff_exptl_absorpt_empirical_full_min 0.766 ####################################################################### # # This file contains crystal structure data downloaded from the # Cambridge Structural Database (CSD) hosted by the Cambridge # Crystallographic Data Centre (CCDC). # # Full information about CCDC data access policies and citation # guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 # # Audit and citation data items may have been added by the CCDC. # Please retain this information to preserve the provenance of # this file and to allow appropriate attribution of the data. # ####################################################################### data_hd_wql34 _database_code_depnum_ccdc_archive 'CCDC 2086415' loop_ _audit_author_name _audit_author_address 'Qilin Wang' ;Henan University China ; _audit_update_record ; 2021-05-28 deposited with the CCDC. 2021-11-08 downloaded from the CCDC. ; _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety 'C26 H24 N2 O3' _chemical_formula_sum 'C26 H24 N2 O3' _chemical_formula_iupac ? _chemical_formula_weight 412.47 _chemical_melting_point ? _space_group_crystal_system monoclinic _space_group_name_H-M_alt 'P 1 21/n 1' _space_group_name_Hall '-P 2yn' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.8952(8) _cell_length_b 8.6715(6) _cell_length_c 21.1913(13) _cell_angle_alpha 90 _cell_angle_beta 94.064(2) _cell_angle_gamma 90 _cell_volume 2180.4(2) _cell_formula_units_Z 4 _cell_measurement_reflns_used 9896 _cell_measurement_theta_min 4.1415 _cell_measurement_theta_max 72.4441 _cell_measurement_temperature 100.(2) _exptl_crystal_description plate _exptl_crystal_colour 'clear light colourless' _exptl_crystal_size_max 0.600 _exptl_crystal_size_mid 0.430 _exptl_crystal_size_min 0.100 _exptl_crystal_density_diffrn 1.257 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 872 _exptl_absorpt_coefficient_mu 0.662 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_process_details ; SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction ; _exptl_absorpt_correction_T_min 0.43 _exptl_absorpt_correction_T_max 0.94 _exptl_special_details ; ; _diffrn_ambient_temperature 100.(2) _diffrn_source 'Ius Diamond' _diffrn_source_type Microfocus _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_monochromator 'Helixos MX multilayer Optic' _diffrn_measurement_device_type 'Bruker D8 QUEST PHOTON II' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean 7.3910 _diffrn_reflns_number 21965 _diffrn_reflns_av_R_equivalents 0.0828 _diffrn_reflns_av_unetI/netI 0.0615 _diffrn_reflns_theta_min 4.14 _diffrn_reflns_theta_max 72.52 _diffrn_reflns_theta_full 72.52 _diffrn_measured_fraction_theta_max 0.996 _diffrn_measured_fraction_theta_full 0.996 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _refine_special_details ; ; _reflns_number_total 4310 _reflns_number_gt 3685 _reflns_threshold_expression 'I > 2\s(I)' _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_R_factor_all 0.0817 _refine_ls_R_factor_gt 0.0738 _refine_ls_wR_factor_gt 0.2043 _refine_ls_wR_factor_ref 0.2161 _refine_ls_goodness_of_fit_ref 1.072 _refine_ls_restrained_S_all 1.072 _refine_ls_number_reflns 4310 _refine_ls_number_parameters 281 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_hydrogen_treatment constr _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.1537P)^2^+0.3407P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.415 _refine_diff_density_min -0.384 _refine_ls_extinction_method none _refine_ls_extinction_coef ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _computing_data_collection 'Bruker Instrument Service vV6.2.9' _computing_cell_refinement 'SAINT V8.38A (Bruker AXS Inc., 2017)' _computing_data_reduction 'SAINT V8.38A (Bruker AXS Inc., 2017)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _computing_structure_refinement 'SHELXL-2017/1 (Sheldrick, 2017)' _computing_molecular_graphics 'shelXle (C.B. Huebschle, rev 882)' _computing_publication_material ? loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_refinement_flags_posn _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group O O1 0.67648(14) 0.62278(19) 0.76482(7) 0.0458(4) Uani d . . . 1 . . O O2 0.07823(13) 0.82441(16) 0.61041(6) 0.0375(4) Uani d . . . 1 . . O O3 0.66820(17) 0.5182(2) 0.66841(8) 0.0608(5) Uani d . . . 1 . . N N1 0.22901(15) 0.49422(19) 0.49927(7) 0.0353(4) Uani d . . . 1 . . N N2 0.54035(17) 0.8208(2) 0.46963(8) 0.0446(4) Uani d . . . 1 . . C C1 0.17792(19) 0.7217(2) 0.83879(8) 0.0394(5) Uani d . . . 1 . . H H1 0.183817 0.719476 0.88372 0.047 Uiso calc U . R 1 . . C C2 0.26058(19) 0.6535(2) 0.80550(8) 0.0387(5) Uani d . . . 1 . . H H18 0.323487 0.605537 0.827611 0.046 Uiso calc U . R 1 . . C C3 0.25174(17) 0.6549(2) 0.73963(8) 0.0353(4) Uani d . . . 1 . . H H15 0.307497 0.605325 0.716881 0.042 Uiso calc U . R 1 . . C C4 0.16125(16) 0.7290(2) 0.70696(8) 0.0318(4) Uani d . . . 1 . . C C5 0.15078(16) 0.7420(2) 0.63651(8) 0.0306(4) Uani d . . . 1 . . C C6 0.22942(16) 0.6559(2) 0.59513(8) 0.0301(4) Uani d . . . 1 . . H H6 0.276059 0.580154 0.621151 0.036 Uiso calc U . R 1 . . C C7 0.30684(16) 0.7741(2) 0.56416(8) 0.0319(4) Uani d . . . 1 . . H H19 0.258963 0.861792 0.547386 0.038 Uiso calc U . R 1 . . C C8 0.39744(17) 0.8394(2) 0.61319(8) 0.0334(4) Uani d . . . 1 . . H H5 0.433215 0.930117 0.594513 0.04 Uiso calc U . R 1 . . H H20 0.359757 0.875399 0.650688 0.04 Uiso calc U . R 1 . . C C9 0.48737(17) 0.7269(2) 0.63436(8) 0.0353(4) Uani d . . . 1 . . H H21 0.513121 0.659726 0.603023 0.042 Uiso calc U . R 1 . . C C10 0.53494(17) 0.7112(2) 0.69262(9) 0.0355(4) Uani d . . . 1 . . H H22 0.506551 0.768102 0.726356 0.043 Uiso calc U . R 1 . . C C11 0.63175(18) 0.6060(2) 0.70544(9) 0.0386(5) Uani d . . . 1 . . C C12 0.7782(2) 0.5359(3) 0.78181(12) 0.0579(7) Uani d . . . 1 . . H H23 0.836997 0.560916 0.752592 0.069 Uiso calc U . R 1 . . H H24 0.762575 0.423905 0.779109 0.069 Uiso calc U . R 1 . . C C13 0.8176(3) 0.5792(4) 0.84815(12) 0.0626(7) Uani d . . . 1 . . H H3 0.823415 0.691644 0.851516 0.094 Uiso calc U . R 1 . . H H4 0.891536 0.532794 0.859023 0.094 Uiso calc U . R 1 . . H H2 0.763458 0.541387 0.877336 0.094 Uiso calc U . R 1 . . C C14 0.15656(16) 0.5711(2) 0.54283(8) 0.0317(4) Uani d . . . 1 . . H H14 0.106737 0.646999 0.518871 0.038 Uiso calc U . R 1 . . C C15 0.08668(16) 0.4392(2) 0.56413(8) 0.0333(4) Uani d . . . 1 . . C C16 0.00400(17) 0.4392(2) 0.60746(8) 0.0354(4) Uani d . . . 1 . . H H13 -0.014395 0.531501 0.628546 0.042 Uiso calc U . R 1 . . C C17 -0.05121(19) 0.3023(2) 0.61942(9) 0.0406(5) Uani d . . . 1 . . H H12 -0.10857 0.301241 0.648416 0.049 Uiso calc U . R 1 . . C C18 -0.0230(2) 0.1661(2) 0.58913(10) 0.0435(5) Uani d . . . 1 . . H H7 -0.060037 0.072651 0.598431 0.052 Uiso calc U . R 1 . . C C19 0.05882(19) 0.1662(2) 0.54553(10) 0.0412(5) Uani d . . . 1 . . H H8 0.077937 0.073683 0.524791 0.049 Uiso calc U . R 1 . . C C20 0.11212(17) 0.3040(2) 0.53281(8) 0.0360(4) Uani d . . . 1 . . C C21 0.19860(18) 0.3329(2) 0.48585(9) 0.0377(5) Uani d . . . 1 . . H H10 0.26444 0.263688 0.493221 0.045 Uiso calc U . R 1 . . H H9 0.166187 0.319805 0.441844 0.045 Uiso calc U . R 1 . . C C22 0.32271(17) 0.5636(2) 0.48259(8) 0.0358(4) Uani d . . . 1 . . H H11 0.364484 0.516714 0.451168 0.043 Uiso calc U . R 1 . . C C23 0.36074(17) 0.6991(2) 0.50887(8) 0.0342(4) Uani d . . . 1 . . C C24 0.45949(18) 0.7661(2) 0.48632(8) 0.0374(5) Uani d . . . 1 . . C C25 0.08647(19) 0.7933(2) 0.80685(9) 0.0411(5) Uani d . . . 1 . . H H16 0.02948 0.839232 0.829858 0.049 Uiso calc U . R 1 . . C C26 0.07832(18) 0.7979(2) 0.74103(9) 0.0373(4) Uani d . . . 1 . . H H17 0.016109 0.848046 0.719183 0.045 Uiso calc U . R 1 . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 O1 0.0569(9) 0.0523(9) 0.0267(7) 0.0164(7) -0.0079(6) -0.0105(6) O2 0.0511(8) 0.0359(7) 0.0254(6) 0.0071(6) 0.0029(5) 0.0010(5) O3 0.0719(11) 0.0750(12) 0.0335(8) 0.0309(9) -0.0090(7) -0.0202(8) N1 0.0491(9) 0.0359(8) 0.0211(7) 0.0008(7) 0.0048(6) -0.0054(6) N2 0.0529(11) 0.0503(10) 0.0315(8) 0.0006(8) 0.0102(7) 0.0071(7) C1 0.0598(12) 0.0396(10) 0.0193(8) -0.0094(8) 0.0066(8) -0.0015(7) C2 0.0516(11) 0.0436(10) 0.0208(9) -0.0026(8) 0.0018(7) 0.0022(7) C3 0.0465(10) 0.0386(10) 0.0210(8) -0.0007(7) 0.0050(7) 0.0001(7) C4 0.0447(10) 0.0290(8) 0.0220(8) -0.0045(7) 0.0053(7) -0.0015(6) C5 0.0429(10) 0.0276(8) 0.0216(8) -0.0005(7) 0.0044(7) -0.0005(6) C6 0.0426(9) 0.0319(9) 0.0158(7) 0.0010(7) 0.0027(6) -0.0004(6) C7 0.0431(10) 0.0340(9) 0.0186(7) 0.0023(7) 0.0033(7) 0.0020(6) C8 0.0439(10) 0.0326(9) 0.0240(8) -0.0014(7) 0.0042(7) 0.0001(7) C9 0.0457(10) 0.0376(10) 0.0229(8) 0.0007(7) 0.0046(7) -0.0031(7) C10 0.0458(10) 0.0367(9) 0.0240(8) 0.0009(7) 0.0034(7) -0.0036(7) C11 0.0503(11) 0.0403(10) 0.0246(8) 0.0031(8) -0.0009(7) -0.0066(7) C12 0.0653(15) 0.0631(15) 0.0426(12) 0.0270(12) -0.0146(11) -0.0189(11) C13 0.0683(16) 0.0734(17) 0.0430(13) 0.0258(13) -0.0181(11) -0.0151(12) C14 0.0438(10) 0.0332(9) 0.0182(7) 0.0022(7) 0.0018(7) -0.0014(6) C15 0.0442(10) 0.0330(9) 0.0220(8) 0.0005(7) -0.0032(7) 0.0008(7) C16 0.0480(10) 0.0359(10) 0.0219(8) -0.0015(7) 0.0005(7) 0.0019(7) C17 0.0513(11) 0.0435(11) 0.0262(8) -0.0052(8) -0.0018(8) 0.0070(8) C18 0.0561(12) 0.0346(10) 0.0381(10) -0.0068(8) -0.0085(9) 0.0086(8) C19 0.0528(12) 0.0323(9) 0.0369(10) 0.0025(8) -0.0085(8) -0.0013(7) C20 0.0464(10) 0.0352(9) 0.0252(8) 0.0035(7) -0.0057(7) -0.0008(7) C21 0.0509(11) 0.0363(10) 0.0255(8) 0.0018(8) -0.0011(8) -0.0081(7) C22 0.0468(10) 0.0422(10) 0.0186(7) 0.0043(8) 0.0035(7) -0.0008(7) C23 0.0448(10) 0.0394(10) 0.0188(8) 0.0032(7) 0.0052(7) 0.0024(7) C24 0.0494(11) 0.0416(10) 0.0218(8) 0.0035(8) 0.0056(7) 0.0044(7) C25 0.0549(12) 0.0421(11) 0.0278(9) -0.0016(9) 0.0140(8) -0.0031(8) C26 0.0498(11) 0.0368(10) 0.0260(9) 0.0004(8) 0.0076(7) -0.0005(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag O1 C11 . 1.339(2) ? O1 C12 . 1.449(3) ? O2 C5 . 1.222(2) ? O3 C11 . 1.196(3) ? N1 C22 . 1.336(3) ? N1 C14 . 1.467(2) ? N1 C21 . 1.468(3) ? N2 C24 . 1.150(3) ? C1 C2 . 1.383(3) ? C1 C25 . 1.387(3) ? C1 H1 . 0.95 ? C2 C3 . 1.392(2) ? C2 H18 . 0.95 ? C3 C4 . 1.395(3) ? C3 H15 . 0.95 ? C4 C26 . 1.397(3) ? C4 C5 . 1.494(2) ? C5 C6 . 1.522(2) ? C6 C14 . 1.544(2) ? C6 C7 . 1.554(2) ? C6 H6 . 1.0 ? C7 C23 . 1.521(2) ? C7 C8 . 1.550(3) ? C7 H19 . 1.0 ? C8 C9 . 1.493(3) ? C8 H5 . 0.99 ? C8 H20 . 0.99 ? C9 C10 . 1.328(3) ? C9 H21 . 0.95 ? C10 C11 . 1.479(3) ? C10 H22 . 0.95 ? C12 C13 . 1.498(3) ? C12 H23 . 0.99 ? C12 H24 . 0.99 ? C13 H3 . 0.98 ? C13 H4 . 0.98 ? C13 H2 . 0.98 ? C14 C15 . 1.502(3) ? C14 H14 . 1.0 ? C15 C20 . 1.392(3) ? C15 C16 . 1.392(3) ? C16 C17 . 1.389(3) ? C16 H13 . 0.95 ? C17 C18 . 1.396(3) ? C17 H12 . 0.95 ? C18 C19 . 1.389(3) ? C18 H7 . 0.95 ? C19 C20 . 1.388(3) ? C19 H8 . 0.95 ? C20 C21 . 1.502(3) ? C21 H10 . 0.99 ? C21 H9 . 0.99 ? C22 C23 . 1.364(3) ? C22 H11 . 0.95 ? C23 C24 . 1.423(3) ? C25 C26 . 1.392(3) ? C25 H16 . 0.95 ? C26 H17 . 0.95 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C11 O1 C12 . . 116.51(16) ? C22 N1 C14 . . 120.02(16) ? C22 N1 C21 . . 125.22(16) ? C14 N1 C21 . . 114.04(16) ? C2 C1 C25 . . 120.28(17) ? C2 C1 H1 . . 119.9 ? C25 C1 H1 . . 119.9 ? C1 C2 C3 . . 120.10(19) ? C1 C2 H18 . . 120.0 ? C3 C2 H18 . . 120.0 ? C2 C3 C4 . . 120.17(18) ? C2 C3 H15 . . 119.9 ? C4 C3 H15 . . 119.9 ? C3 C4 C26 . . 119.26(16) ? C3 C4 C5 . . 122.52(17) ? C26 C4 C5 . . 118.19(17) ? O2 C5 C4 . . 120.17(16) ? O2 C5 C6 . . 117.97(15) ? C4 C5 C6 . . 121.86(16) ? C5 C6 C14 . . 108.08(15) ? C5 C6 C7 . . 109.07(14) ? C14 C6 C7 . . 109.29(13) ? C5 C6 H6 . . 110.1 ? C14 C6 H6 . . 110.1 ? C7 C6 H6 . . 110.1 ? C23 C7 C8 . . 111.20(16) ? C23 C7 C6 . . 109.75(15) ? C8 C7 C6 . . 111.25(14) ? C23 C7 H19 . . 108.2 ? C8 C7 H19 . . 108.2 ? C6 C7 H19 . . 108.2 ? C9 C8 C7 . . 114.31(15) ? C9 C8 H5 . . 108.7 ? C7 C8 H5 . . 108.7 ? C9 C8 H20 . . 108.7 ? C7 C8 H20 . . 108.7 ? H5 C8 H20 . . 107.6 ? C10 C9 C8 . . 126.50(17) ? C10 C9 H21 . . 116.7 ? C8 C9 H21 . . 116.7 ? C9 C10 C11 . . 120.56(17) ? C9 C10 H22 . . 119.7 ? C11 C10 H22 . . 119.7 ? O3 C11 O1 . . 123.17(19) ? O3 C11 C10 . . 125.85(18) ? O1 C11 C10 . . 110.97(16) ? O1 C12 C13 . . 107.63(18) ? O1 C12 H23 . . 110.2 ? C13 C12 H23 . . 110.2 ? O1 C12 H24 . . 110.2 ? C13 C12 H24 . . 110.2 ? H23 C12 H24 . . 108.5 ? C12 C13 H3 . . 109.5 ? C12 C13 H4 . . 109.5 ? H3 C13 H4 . . 109.5 ? C12 C13 H2 . . 109.5 ? H3 C13 H2 . . 109.5 ? H4 C13 H2 . . 109.5 ? N1 C14 C15 . . 101.87(15) ? N1 C14 C6 . . 110.08(15) ? C15 C14 C6 . . 116.20(14) ? N1 C14 H14 . . 109.5 ? C15 C14 H14 . . 109.5 ? C6 C14 H14 . . 109.5 ? C20 C15 C16 . . 120.13(18) ? C20 C15 C14 . . 110.77(17) ? C16 C15 C14 . . 129.09(17) ? C17 C16 C15 . . 119.08(19) ? C17 C16 H13 . . 120.5 ? C15 C16 H13 . . 120.5 ? C16 C17 C18 . . 120.4(2) ? C16 C17 H12 . . 119.8 ? C18 C17 H12 . . 119.8 ? C19 C18 C17 . . 120.56(19) ? C19 C18 H7 . . 119.7 ? C17 C18 H7 . . 119.7 ? C20 C19 C18 . . 118.74(19) ? C20 C19 H8 . . 120.6 ? C18 C19 H8 . . 120.6 ? C19 C20 C15 . . 121.0(2) ? C19 C20 C21 . . 128.02(19) ? C15 C20 C21 . . 110.96(17) ? N1 C21 C20 . . 101.62(15) ? N1 C21 H10 . . 111.4 ? C20 C21 H10 . . 111.4 ? N1 C21 H9 . . 111.4 ? C20 C21 H9 . . 111.4 ? H10 C21 H9 . . 109.3 ? N1 C22 C23 . . 122.60(17) ? N1 C22 H11 . . 118.7 ? C23 C22 H11 . . 118.7 ? C22 C23 C24 . . 118.20(17) ? C22 C23 C7 . . 122.51(18) ? C24 C23 C7 . . 119.14(17) ? N2 C24 C23 . . 178.3(2) ? C1 C25 C26 . . 119.89(19) ? C1 C25 H16 . . 120.1 ? C26 C25 H16 . . 120.1 ? C25 C26 C4 . . 120.3(2) ? C25 C26 H17 . . 119.9 ? C4 C26 H17 . . 119.9 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag C25 C1 C2 C3 . . . . -0.7(3) ? C1 C2 C3 C4 . . . . 1.9(3) ? C2 C3 C4 C26 . . . . -1.7(3) ? C2 C3 C4 C5 . . . . 176.48(18) ? C3 C4 C5 O2 . . . . -170.60(18) ? C26 C4 C5 O2 . . . . 7.6(3) ? C3 C4 C5 C6 . . . . 8.7(3) ? C26 C4 C5 C6 . . . . -173.06(17) ? O2 C5 C6 C14 . . . . -50.5(2) ? C4 C5 C6 C14 . . . . 130.15(17) ? O2 C5 C6 C7 . . . . 68.2(2) ? C4 C5 C6 C7 . . . . -111.12(18) ? C5 C6 C7 C23 . . . . -163.48(14) ? C14 C6 C7 C23 . . . . -45.51(19) ? C5 C6 C7 C8 . . . . 73.02(18) ? C14 C6 C7 C8 . . . . -169.01(15) ? C23 C7 C8 C9 . . . . -51.5(2) ? C6 C7 C8 C9 . . . . 71.2(2) ? C7 C8 C9 C10 . . . . -141.2(2) ? C8 C9 C10 C11 . . . . -173.40(19) ? C12 O1 C11 O3 . . . . 4.2(4) ? C12 O1 C11 C10 . . . . -174.8(2) ? C9 C10 C11 O3 . . . . -7.3(4) ? C9 C10 C11 O1 . . . . 171.57(19) ? C11 O1 C12 C13 . . . . 176.4(2) ? C22 N1 C14 C15 . . . . -162.80(16) ? C21 N1 C14 C15 . . . . 7.91(19) ? C22 N1 C14 C6 . . . . -38.9(2) ? C21 N1 C14 C6 . . . . 131.77(16) ? C5 C6 C14 N1 . . . . 176.44(14) ? C7 C6 C14 N1 . . . . 57.85(19) ? C5 C6 C14 C15 . . . . -68.48(19) ? C7 C6 C14 C15 . . . . 172.94(15) ? N1 C14 C15 C20 . . . . -3.41(19) ? C6 C14 C15 C20 . . . . -123.04(17) ? N1 C14 C15 C16 . . . . 178.04(18) ? C6 C14 C15 C16 . . . . 58.4(3) ? C20 C15 C16 C17 . . . . 0.8(3) ? C14 C15 C16 C17 . . . . 179.28(18) ? C15 C16 C17 C18 . . . . 1.0(3) ? C16 C17 C18 C19 . . . . -1.5(3) ? C17 C18 C19 C20 . . . . 0.2(3) ? C18 C19 C20 C15 . . . . 1.6(3) ? C18 C19 C20 C21 . . . . -177.08(18) ? C16 C15 C20 C19 . . . . -2.2(3) ? C14 C15 C20 C19 . . . . 179.13(17) ? C16 C15 C20 C21 . . . . 176.75(16) ? C14 C15 C20 C21 . . . . -2.0(2) ? C22 N1 C21 C20 . . . . 161.20(17) ? C14 N1 C21 C20 . . . . -8.9(2) ? C19 C20 C21 N1 . . . . -174.79(19) ? C15 C20 C21 N1 . . . . 6.4(2) ? C14 N1 C22 C23 . . . . 6.2(3) ? C21 N1 C22 C23 . . . . -163.44(18) ? N1 C22 C23 C24 . . . . -177.98(17) ? N1 C22 C23 C7 . . . . 6.6(3) ? C8 C7 C23 C22 . . . . 138.51(18) ? C6 C7 C23 C22 . . . . 15.0(2) ? C8 C7 C23 C24 . . . . -36.9(2) ? C6 C7 C23 C24 . . . . -160.42(16) ? C2 C1 C25 C26 . . . . -0.6(3) ? C1 C25 C26 C4 . . . . 0.7(3) ? C3 C4 C26 C25 . . . . 0.4(3) ? C5 C4 C26 C25 . . . . -177.85(18) ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag C21 H10 N2 3_666 0.99 2.51 3.449(3) 158.6 ? C22 H11 O3 3_666 0.95 2.55 3.287(2) 134.1 ? _shelx_res_file ; TITL hd_wql34_0m_a.res in P2(1)/n hd_wql34_0m.res created by SHELXL-2017/1 at 22:21:16 on 14-Oct-2020 CELL 1.54178 11.8952 8.6715 21.1913 90.000 94.064 90.000 ZERR 4.00 0.0008 0.0006 0.0013 0.000 0.002 0.000 LATT 1 SYMM -x+1/2, y+1/2, -z+1/2 SFAC C H N O UNIT 104 96 8 12 LIST 4 ! automatically inserted. Change 6 to 4 for CHECKCIF!! TEMP -173.130 SIZE 0.100 0.430 0.600 ACTA EQIV $1 -x+1, -y+1, -z+1 HTAB C21 N2_$1 HTAB C22 O3_$1 L.S. 4 FMAP 2 PLAN -5 0 0.00 HTAB BOND $H CONF WGHT 0.153700 0.340700 FVAR 0.59847 O1 4 0.676483 0.622784 0.764818 11.00000 0.05686 0.05234 = 0.02666 -0.01046 -0.00792 0.01639 O2 4 0.078227 0.824412 0.610409 11.00000 0.05109 0.03594 = 0.02541 0.00097 0.00288 0.00714 O3 4 0.668195 0.518223 0.668410 11.00000 0.07193 0.07503 = 0.03353 -0.02017 -0.00902 0.03088 N1 3 0.229009 0.494220 0.499271 11.00000 0.04909 0.03591 = 0.02114 -0.00544 0.00481 0.00082 N2 3 0.540345 0.820814 0.469633 11.00000 0.05295 0.05030 = 0.03149 0.00709 0.01015 0.00057 C1 1 0.177922 0.721699 0.838786 11.00000 0.05976 0.03956 = 0.01933 -0.00148 0.00664 -0.00939 AFIX 43 H1 2 0.183817 0.719476 0.883720 11.00000 -1.20000 AFIX 0 C2 1 0.260582 0.653471 0.805501 11.00000 0.05158 0.04361 = 0.02078 0.00223 0.00185 -0.00264 AFIX 43 H18 2 0.323487 0.605537 0.827611 11.00000 -1.20000 AFIX 0 C3 1 0.251745 0.654929 0.739629 11.00000 0.04650 0.03865 = 0.02100 0.00012 0.00495 -0.00068 AFIX 43 H15 2 0.307497 0.605325 0.716881 11.00000 -1.20000 AFIX 0 C4 1 0.161253 0.729025 0.706963 11.00000 0.04472 0.02898 = 0.02200 -0.00146 0.00532 -0.00445 C5 1 0.150775 0.741963 0.636511 11.00000 0.04289 0.02763 = 0.02158 -0.00052 0.00443 -0.00046 C6 1 0.229422 0.655911 0.595131 11.00000 0.04265 0.03191 = 0.01579 -0.00037 0.00273 0.00103 AFIX 13 H6 2 0.276059 0.580154 0.621151 11.00000 -1.20000 AFIX 0 C7 1 0.306844 0.774121 0.564159 11.00000 0.04309 0.03404 = 0.01859 0.00202 0.00333 0.00230 AFIX 13 H19 2 0.258963 0.861792 0.547386 11.00000 -1.20000 AFIX 0 C8 1 0.397441 0.839426 0.613191 11.00000 0.04386 0.03261 = 0.02396 0.00011 0.00424 -0.00139 AFIX 23 H5 2 0.433215 0.930117 0.594513 11.00000 -1.20000 H20 2 0.359757 0.875399 0.650688 11.00000 -1.20000 AFIX 0 C9 1 0.487372 0.726855 0.634361 11.00000 0.04572 0.03756 = 0.02294 -0.00306 0.00464 0.00070 AFIX 43 H21 2 0.513121 0.659726 0.603023 11.00000 -1.20000 AFIX 0 C10 1 0.534941 0.711225 0.692624 11.00000 0.04585 0.03672 = 0.02397 -0.00358 0.00343 0.00086 AFIX 43 H22 2 0.506551 0.768102 0.726356 11.00000 -1.20000 AFIX 0 C11 1 0.631751 0.606008 0.705436 11.00000 0.05030 0.04035 = 0.02460 -0.00661 -0.00092 0.00310 C12 1 0.778246 0.535925 0.781812 11.00000 0.06533 0.06308 = 0.04257 -0.01893 -0.01463 0.02697 AFIX 23 H23 2 0.836997 0.560916 0.752592 11.00000 -1.20000 H24 2 0.762575 0.423905 0.779109 11.00000 -1.20000 AFIX 0 C13 1 0.817560 0.579174 0.848154 11.00000 0.06832 0.07344 = 0.04299 -0.01508 -0.01806 0.02581 AFIX 137 H3 2 0.823415 0.691644 0.851516 11.00000 -1.50000 H4 2 0.891536 0.532794 0.859023 11.00000 -1.50000 H2 2 0.763458 0.541387 0.877336 11.00000 -1.50000 AFIX 0 C14 1 0.156564 0.571070 0.542834 11.00000 0.04376 0.03319 = 0.01816 -0.00145 0.00180 0.00218 AFIX 13 H14 2 0.106737 0.646999 0.518871 11.00000 -1.20000 AFIX 0 C15 1 0.086675 0.439232 0.564132 11.00000 0.04424 0.03299 = 0.02202 0.00082 -0.00322 0.00054 C16 1 0.004000 0.439168 0.607458 11.00000 0.04797 0.03593 = 0.02194 0.00193 0.00048 -0.00154 AFIX 43 H13 2 -0.014395 0.531501 0.628546 11.00000 -1.20000 AFIX 0 C17 1 -0.051209 0.302263 0.619425 11.00000 0.05135 0.04350 = 0.02618 0.00703 -0.00184 -0.00521 AFIX 43 H12 2 -0.108570 0.301241 0.648416 11.00000 -1.20000 AFIX 0 C18 1 -0.022975 0.166124 0.589132 11.00000 0.05610 0.03461 = 0.03814 0.00857 -0.00854 -0.00682 AFIX 43 H7 2 -0.060037 0.072651 0.598431 11.00000 -1.20000 AFIX 0 C19 1 0.058820 0.166193 0.545527 11.00000 0.05283 0.03234 = 0.03686 -0.00134 -0.00846 0.00251 AFIX 43 H8 2 0.077937 0.073683 0.524791 11.00000 -1.20000 AFIX 0 C20 1 0.112121 0.303969 0.532810 11.00000 0.04639 0.03522 = 0.02517 -0.00082 -0.00575 0.00348 C21 1 0.198605 0.332855 0.485848 11.00000 0.05095 0.03626 = 0.02546 -0.00808 -0.00111 0.00180 AFIX 23 H10 2 0.264440 0.263688 0.493221 11.00000 -1.20000 H9 2 0.166187 0.319805 0.441844 11.00000 -1.20000 AFIX 0 C22 1 0.322708 0.563615 0.482585 11.00000 0.04679 0.04221 = 0.01861 -0.00081 0.00355 0.00428 AFIX 43 H11 2 0.364484 0.516714 0.451168 11.00000 -1.20000 AFIX 0 C23 1 0.360740 0.699100 0.508870 11.00000 0.04480 0.03939 = 0.01877 0.00242 0.00523 0.00317 C24 1 0.459490 0.766146 0.486315 11.00000 0.04938 0.04159 = 0.02178 0.00441 0.00563 0.00348 C25 1 0.086471 0.793340 0.806851 11.00000 0.05493 0.04210 = 0.02778 -0.00306 0.01396 -0.00162 AFIX 43 H16 2 0.029480 0.839232 0.829858 11.00000 -1.20000 AFIX 0 C26 1 0.078318 0.797899 0.741032 11.00000 0.04977 0.03677 = 0.02595 -0.00047 0.00756 0.00043 AFIX 43 H17 2 0.016109 0.848046 0.719183 11.00000 -1.20000 AFIX 0 HKLF 4 1 1 0 0 0 1 0 0 0 1 REM hd_wql34_0m_a.res in P2(1)/n REM R1 = 0.0738 for 3685 Fo > 4sig(Fo) and 0.0817 for all 4310 data REM 281 parameters refined using 0 restraints END WGHT 0.1537 0.3407 REM Instructions for potential hydrogen bonds HTAB C21 N2_$1 HTAB C22 O3_$1 REM Highest difference peak 0.415, deepest hole -0.384, 1-sigma level 0.079 Q1 1 0.7094 0.5896 0.6573 11.00000 0.05 0.42 Q2 1 0.3343 0.7236 0.5360 11.00000 0.05 0.40 Q3 1 0.1984 0.6975 0.6212 11.00000 0.05 0.35 Q4 1 0.8075 0.4547 0.7610 11.00000 0.05 0.34 Q5 1 0.2672 0.7132 0.5800 11.00000 0.05 0.32 ; _shelx_res_checksum 37285 _shelx_hkl_file ; -1 0 0 1.70 0.60 -1 0 0 3.20 1.20 -2 0 0 518.95 54.89 -2 0 0 672.93 54.29 -3 0 0 8.50 3.40 -4 0 0 58.89 8.90 -4 0 0 57.29 7.40 -5 0 0 1.90 1.70 -5 0 0 0.20 3.70 -6 0 0 210.78 22.70 -6 0 0 205.38 25.30 -6 0 0 223.78 25.50 -7 0 0 12.30 8.40 -7 0 0 1.90 3.50 -7 0 0 3.80 4.60 8 0 0 89.79 9.70 -8 0 0 116.39 20.60 -9 0 0 -15.60 14.20 -9 0 0 3.60 6.10 -9 0 0 6.70 7.70 -9 0 0 -0.10 1.30 9 0 0 0.60 0.80 -10 0 0 19.70 3.80 -10 0 0 30.00 10.40 -10 0 0 7.80 26.80 -11 0 0 -28.90 35.30 11 0 0 -0.30 0.60 11 0 0 -0.40 0.50 -11 0 0 10.90 10.90 -11 0 0 0.60 1.10 12 0 0 77.89 7.90 12 0 0 77.89 8.50 13 0 0 -0.70 0.50 13 0 0 0.50 0.60 14 0 0 11.10 1.60 -14 0 0 11.80 1.60 14 0 0 7.40 1.50 0 1 0 0.40 0.80 0 1 0 2.90 1.20 -1 -1 0 15.10 2.70 -1 -1 0 16.20 2.50 1 -1 0 15.90 2.70 -2 -1 0 1325.97 106.29 2 1 0 1019.80 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-1 0 5.40 1.40 11 1 0 4.60 1.40 11 1 0 4.50 1.20 -11 1 0 5.40 10.60 12 -1 0 38.50 4.80 12 1 0 36.80 4.70 12 1 0 34.20 4.30 -13 -1 0 4.60 1.20 13 -1 0 4.40 1.30 13 -1 0 2.20 1.00 13 1 0 4.40 1.20 13 1 0 3.70 1.30 14 -1 0 36.20 4.10 14 -1 0 34.60 3.90 -14 -1 0 40.30 4.00 14 1 0 33.40 4.00 0 -2 0 8920.61 796.62 -1 -2 0 290.07 26.10 -1 -2 0 276.87 26.00 1 -2 0 238.98 25.20 -2 -2 0 3879.11 311.37 -2 -2 0 3514.85 310.87 -2 -2 0 2983.90 309.17 -3 -2 0 1894.81 184.78 -3 -2 0 1953.60 185.28 -3 -2 0 1981.00 183.78 -3 2 0 2319.77 187.38 -4 -2 0 20.60 4.80 -4 -2 0 23.10 5.70 -4 -2 0 20.40 6.10 -4 2 0 26.20 9.10 -5 -2 0 190.58 22.20 -5 -2 0 195.98 24.00 -5 -2 0 163.08 21.50 -5 2 0 225.08 19.90 -5 2 0 223.28 28.00 -6 -2 0 22.80 8.00 -6 -2 0 14.80 6.00 -6 -2 0 14.30 5.90 -6 2 0 -1.20 13.20 -6 2 0 17.00 4.60 7 -2 0 3.60 0.80 -7 -2 0 7.80 6.20 -7 -2 0 7.80 6.40 -7 2 0 -0.70 1.30 -7 2 0 -8.70 14.70 -8 -2 0 57.39 12.80 -8 -2 0 39.00 9.80 8 -2 0 35.40 4.00 8 -2 0 37.60 4.60 -8 2 0 28.40 4.90 8 2 0 34.20 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2.50 14 3 0 20.10 2.60 0 -4 0 219.98 22.30 0 -4 0 206.58 22.20 -1 -4 0 109.19 13.60 1 -4 0 107.79 12.30 -1 -4 0 117.09 13.50 -2 -4 0 32.90 6.70 -2 -4 0 30.40 6.60 2 4 0 27.60 3.80 -3 -4 0 379.06 37.50 -3 -4 0 336.47 36.80 -4 -4 0 3.60 4.00 -4 -4 0 2.70 2.10 -4 -4 0 1.40 1.50 -4 -4 0 1.10 3.20 -5 -4 0 34.20 8.60 -5 -4 0 42.40 9.50 -5 -4 0 33.70 6.00 -5 -4 0 44.60 8.00 -5 -4 0 26.80 4.00 -6 -4 0 125.29 12.30 -6 -4 0 140.69 13.80 -6 -4 0 161.88 20.40 -6 -4 0 121.99 12.50 -6 -4 0 140.19 19.80 6 -4 0 108.19 12.00 -6 4 0 124.49 14.20 7 -4 0 1.10 0.80 -7 -4 0 -4.20 4.50 -7 -4 0 0.40 0.90 -7 -4 0 -8.30 12.10 7 -4 0 2.60 1.30 -7 -4 0 -0.60 4.70 -7 -4 0 2.00 1.50 -7 -4 0 1.30 1.90 -7 -4 0 -3.20 4.40 7 4 0 1.30 1.60 -7 4 0 3.70 2.40 8 -4 0 4.10 1.10 8 -4 0 6.40 1.90 -8 -4 0 9.20 2.30 -8 -4 0 2.80 7.60 -8 -4 0 3.40 6.70 -8 -4 0 2.90 1.30 -8 -4 0 8.10 2.10 -8 -4 0 -2.10 5.50 -8 4 0 5.10 2.30 8 4 0 4.00 1.50 -9 -4 0 128.89 21.60 -9 -4 0 122.79 12.00 -9 -4 0 111.69 11.20 -9 -4 0 90.49 19.60 9 -4 0 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4.30 6.10 -5 -2 9 1.20 3.50 -5 2 9 -3.30 14.50 -4 -2 9 224.78 25.60 -4 -2 9 205.98 23.60 -4 2 9 203.88 29.50 -3 -2 9 29.10 7.20 -3 -2 9 30.30 6.40 -3 -2 9 30.40 3.60 -3 2 9 28.30 12.00 2 -2 -9 277.07 25.50 -2 -2 9 295.17 27.70 -2 -2 9 246.78 28.10 -2 -2 9 272.47 24.50 -2 2 9 223.78 30.10 -1 -2 9 72.59 10.10 -1 -2 9 71.39 9.00 -1 -2 9 65.39 6.70 -1 2 9 53.19 7.10 -1 2 9 41.20 14.30 0 -2 9 77.89 10.20 0 -2 9 64.49 7.10 0 -2 -9 74.59 9.00 0 2 9 60.59 14.30 0 2 9 57.59 7.40 -1 -2 -9 1.40 1.90 1 -2 9 -0.30 3.50 1 2 9 4.70 1.60 1 2 9 1.90 9.80 -2 -2 -9 264.77 27.90 2 -2 9 280.77 26.70 2 -2 9 286.87 30.10 -2 -2 -9 288.87 29.20 2 2 9 286.37 26.60 -3 -2 -9 614.44 60.19 3 -2 9 598.64 57.29 -3 -2 -9 584.54 59.69 3 2 9 686.33 57.09 -4 -2 -9 122.19 14.90 4 -2 9 85.49 11.60 -4 -2 -9 77.19 14.00 -4 2 -9 114.99 19.50 4 2 9 106.09 10.70 -5 -2 -9 3.50 4.20 5 -2 9 5.00 2.00 5 -2 9 4.60 1.10 5 -2 9 5.90 1.30 -5 -2 -9 3.70 4.40 -5 -2 -9 3.50 5.50 -5 -2 -9 7.90 2.30 5 2 9 3.00 1.10 5 2 9 4.90 2.60 -5 2 -9 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3.50 1.90 -8 -4 9 129.49 12.90 -8 -4 9 150.58 13.30 8 -4 -9 130.09 12.80 -8 -4 9 109.89 22.70 -8 -4 9 145.19 20.70 8 4 -9 115.09 13.60 -7 -4 9 20.50 8.10 -7 -4 9 18.50 2.40 -7 -4 9 12.10 9.20 -7 -4 9 13.10 2.50 -7 -4 9 13.30 2.60 7 -4 -9 11.80 2.30 7 4 -9 12.50 2.80 -7 4 9 11.90 3.60 -6 -4 9 9.30 2.00 -6 -4 9 5.10 5.70 -6 -4 9 13.90 7.00 -6 -4 9 12.00 2.00 -6 -4 9 7.20 1.70 6 -4 -9 9.20 1.80 -6 4 9 7.30 3.10 6 4 -9 5.40 1.90 -5 -4 9 2.80 1.10 5 -4 -9 5.70 1.90 -5 -4 9 1.80 1.30 -5 -4 9 2.80 1.10 -5 -4 9 6.30 5.50 5 -4 -9 4.50 1.20 -5 -4 9 3.10 4.30 -5 4 9 1.20 2.40 4 -4 -9 147.79 14.30 -4 -4 9 156.28 14.60 -3 -4 9 297.67 26.40 3 -4 -9 271.97 26.30 2 -4 -9 -4.50 10.40 2 -4 -9 10.20 2.10 -2 -4 9 9.90 4.60 -2 -4 9 5.00 1.40 -2 -4 9 5.50 4.80 -2 4 9 2.90 2.50 -1 -4 9 144.99 13.80 1 -4 -9 112.39 16.20 -1 -4 9 171.68 18.50 -1 4 9 125.39 14.70 0 -4 -9 32.30 9.20 0 -4 9 20.00 2.60 0 -4 -9 15.40 5.40 0 -4 9 15.50 5.40 0 4 9 20.30 4.20 -1 -4 -9 8.30 4.30 -1 -4 -9 5.80 10.10 1 4 9 8.70 2.70 2 -4 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25.50 3.10 6 -5 -9 20.90 2.90 -6 -5 9 25.30 3.20 -6 -5 9 20.90 3.30 -6 -5 9 22.10 3.60 -6 5 9 21.10 5.20 5 -5 -9 23.20 3.10 -5 -5 9 26.80 3.20 -5 -5 9 14.70 3.60 -5 -5 9 14.00 7.70 -5 -5 9 23.50 3.40 5 5 -9 19.30 3.70 -5 5 9 16.30 4.40 -4 -5 9 79.99 14.30 -4 -5 9 69.19 7.00 -4 -5 9 56.39 6.90 -4 -5 9 70.49 7.10 -4 -5 9 65.99 6.80 -4 5 9 58.59 10.70 -3 -5 9 74.69 14.30 -3 -5 9 73.59 7.20 -3 -5 9 60.19 7.30 -3 -5 9 73.69 7.50 -3 -5 9 74.79 7.40 -3 5 9 63.89 10.50 -2 -5 9 196.88 18.60 -2 -5 9 218.88 18.40 -2 -5 9 162.08 18.50 -2 -5 9 241.88 26.20 -2 -5 9 192.18 18.60 -2 -5 9 197.18 18.80 -2 5 9 198.28 21.50 -1 -5 9 49.80 5.30 1 -5 -9 37.10 6.30 -1 -5 9 48.80 5.10 -1 -5 9 45.20 5.20 -1 -5 9 49.30 5.20 1 -5 -9 44.80 4.70 -1 5 9 51.39 8.10 0 -5 9 27.30 3.20 0 -5 -9 26.80 4.70 0 -5 9 31.30 3.50 0 -5 -9 22.90 4.60 0 -5 9 32.50 3.70 0 -5 9 24.40 3.30 0 -5 9 25.60 3.60 0 -5 -9 29.60 3.00 0 5 9 34.70 6.30 -1 -5 -9 4.60 4.80 1 -5 9 2.30 0.80 1 -5 9 -0.40 1.10 -1 -5 -9 -0.70 2.30 1 -5 9 3.10 1.00 1 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23 28.70 3.10 -2 -4 23 23.80 2.90 -2 -4 23 25.50 3.50 2 4 -23 30.30 3.60 -1 -4 23 5.40 1.00 -1 -4 23 4.30 0.90 1 -4 -23 4.00 1.10 -1 4 23 6.60 1.40 0 -4 23 169.38 14.20 0 -4 23 163.58 13.70 0 -4 -23 132.69 13.50 0 4 -23 126.59 14.20 1 -4 23 0.10 0.80 1 -4 23 0.70 0.60 -1 -4 -23 0.10 0.60 1 4 23 0.50 0.60 -1 4 -23 0.00 0.70 -2 -4 -23 11.70 2.60 2 -4 23 12.80 1.70 2 4 23 14.80 1.90 3 -4 23 29.20 3.10 -3 -4 -23 25.00 3.60 3 4 23 29.60 3.20 -2 -5 23 62.39 5.80 2 5 -23 57.09 6.20 -1 -5 23 1.40 0.50 -1 5 23 2.10 0.70 1 5 -23 1.20 0.80 0 -5 23 27.60 3.40 0 5 23 35.80 3.60 -6 0 24 75.69 6.80 -6 0 24 58.29 7.10 -5 0 24 -0.60 0.70 5 0 -24 0.90 0.70 -5 0 24 1.00 0.80 5 0 -24 0.20 0.40 4 0 -24 87.49 9.20 4 0 -24 108.89 9.60 -4 0 24 97.49 9.30 3 0 -24 0.30 0.50 3 0 -24 -0.50 0.80 -3 0 24 -0.40 0.60 -3 0 24 -0.30 0.40 -2 0 24 0.90 0.60 -2 0 24 2.30 0.90 2 0 -24 0.70 0.60 2 0 -24 -0.30 0.80 -2 0 24 1.60 0.90 -1 0 24 -1.50 0.90 1 0 -24 1.60 0.80 -1 0 24 -0.20 0.30 1 0 -24 -0.10 1.60 -1 0 24 -0.20 0.70 1 0 -24 0.30 0.80 0 0 24 5.00 1.00 0 0 -24 4.20 0.90 0 0 24 2.70 0.90 0 0 -24 0.30 1.20 -1 0 -24 0.10 0.60 1 0 24 0.60 0.40 1 0 24 0.40 0.50 2 0 24 15.30 2.60 -2 0 -24 15.50 2.30 2 0 24 19.80 2.20 3 0 24 1.70 0.80 -3 0 -24 -0.80 0.50 3 0 24 -0.40 0.30 -4 0 -24 0.40 0.50 -4 0 -24 0.20 0.70 4 0 24 -0.40 0.30 4 0 24 0.00 0.40 -6 -1 24 19.30 2.60 6 1 -24 24.90 2.70 -6 1 24 25.60 2.60 -6 1 24 20.30 2.90 5 -1 -24 30.40 3.70 -5 -1 24 25.20 3.90 5 1 -24 37.40 3.70 -5 1 24 30.40 3.70 4 -1 -24 63.59 6.50 -4 1 24 68.79 6.70 4 1 -24 69.09 6.50 4 1 -24 63.59 6.80 3 -1 -24 1.70 0.50 -3 -1 24 0.80 0.90 -3 -1 24 1.40 0.70 -3 1 24 0.60 1.00 -3 1 24 1.40 0.70 3 1 -24 2.00 0.90 3 1 -24 1.00 0.70 2 -1 -24 137.09 12.40 -2 -1 24 118.99 12.10 2 1 -24 143.09 12.50 2 1 -24 130.09 12.80 1 -1 -24 2.80 0.80 -1 -1 24 2.10 0.90 -1 -1 24 3.20 0.80 -1 -1 24 2.70 1.30 -1 -1 24 2.50 0.90 -1 1 24 4.40 1.20 -1 1 24 4.50 1.20 1 1 -24 1.60 1.10 -1 1 24 2.20 1.00 0 -1 -24 58.89 5.40 0 -1 24 47.00 5.20 0 -1 24 49.40 5.50 0 -1 -24 38.30 6.20 0 1 24 55.39 5.70 0 1 -24 55.79 5.50 0 1 24 60.89 5.70 -1 -1 -24 8.10 2.50 -1 -1 -24 14.10 1.90 1 -1 24 9.30 1.60 1 -1 24 12.50 2.00 1 1 24 15.10 1.90 1 1 24 12.60 2.20 -1 1 -24 13.20 2.00 -2 -1 -24 0.60 0.60 2 -1 24 0.50 0.50 2 -1 24 0.20 0.50 -2 1 -24 -0.40 0.50 -2 1 -24 0.00 0.70 2 1 24 0.60 0.50 2 1 24 2.20 0.90 -3 -1 -24 18.70 2.50 -3 -1 -24 25.40 3.10 3 1 24 20.30 2.60 -3 1 -24 17.00 2.40 -4 -1 -24 45.10 4.60 -4 1 -24 44.80 4.60 -6 -2 24 33.90 4.10 6 -2 -24 44.00 4.10 -6 -2 24 36.90 4.10 6 2 -24 45.30 4.40 -6 2 24 45.90 4.30 -5 -2 24 3.50 0.80 5 -2 -24 4.60 0.90 -5 -2 24 4.50 0.90 -5 -2 24 4.30 1.10 5 2 -24 4.60 1.20 -5 2 24 6.70 1.20 -4 -2 24 3.20 0.80 -4 -2 24 2.90 0.90 -4 -2 24 4.50 1.10 -4 2 24 6.00 1.80 -4 2 24 5.30 1.20 4 2 -24 3.00 1.10 -3 -2 24 7.30 1.50 3 -2 -24 12.60 1.60 -3 -2 24 9.70 1.80 -3 2 24 9.50 2.00 3 2 -24 10.70 1.90 3 2 -24 11.50 1.80 -3 2 24 12.10 1.90 -2 -2 24 14.30 2.20 -2 -2 24 12.00 1.90 -2 -2 24 14.50 2.20 2 2 -24 17.40 2.20 -2 2 24 12.80 2.30 2 2 -24 14.80 2.40 -1 -2 24 5.40 1.40 -1 -2 24 4.80 1.30 1 -2 -24 9.30 1.50 -1 2 24 8.40 1.60 1 2 -24 7.50 2.00 0 -2 24 4.20 1.10 0 -2 -24 6.90 1.40 0 -2 24 6.30 1.20 0 2 -24 6.70 2.20 0 2 24 9.20 1.60 -1 -2 -24 87.99 10.30 -1 -2 -24 101.39 9.90 1 -2 24 109.89 10.00 1 2 24 116.89 10.20 -2 -2 -24 22.90 3.80 2 -2 24 25.70 2.90 2 2 24 23.50 2.90 -3 -2 -24 24.20 2.70 -3 2 -24 20.50 2.70 -4 -2 -24 3.90 1.20 -4 -2 -24 2.80 0.80 -4 2 -24 2.40 0.80 4 2 24 2.80 0.80 -5 -3 24 2.10 0.50 -5 -3 24 3.40 0.80 -5 -3 24 3.10 0.70 -5 3 24 3.60 0.90 5 3 -24 3.00 0.90 -4 -3 24 0.80 0.50 4 -3 -24 3.40 0.70 -4 -3 24 1.90 0.60 -4 -3 24 1.30 0.60 -4 3 24 2.30 0.90 4 3 -24 0.80 0.80 -3 -3 24 51.39 5.50 -3 -3 24 50.59 5.00 3 -3 -24 49.50 5.30 -3 -3 24 52.69 5.10 3 3 -24 46.10 6.00 -2 -3 24 3.90 0.80 -2 -3 24 2.50 0.90 2 -3 -24 3.60 0.80 -2 -3 24 4.30 0.80 2 3 -24 2.00 1.00 -2 3 24 3.00 1.00 -1 -3 24 45.00 4.70 -1 -3 24 42.60 4.90 1 -3 -24 49.10 4.60 0 -3 -24 15.40 2.00 0 -3 24 12.10 1.80 0 -3 24 14.70 1.90 0 3 24 16.90 2.20 -1 -3 -24 5.30 1.10 1 -3 24 4.20 1.10 1 3 24 4.30 1.20 -2 -3 -24 25.30 2.90 -2 -3 -24 31.60 4.00 -3 -3 -24 23.90 3.10 -3 -3 -24 18.30 2.10 3 4 -24 0.50 0.70 -3 4 24 0.10 0.60 2 -4 -24 19.90 2.30 -2 -4 24 20.80 2.30 -2 -4 24 23.80 2.30 -1 -4 24 1.50 0.60 -1 -4 24 1.00 0.40 -1 4 24 0.40 0.50 1 4 -24 0.30 0.70 0 -4 24 18.00 2.00 1 -4 24 41.90 4.40 1 4 24 51.19 4.80 -5 0 25 9.30 1.40 -5 0 25 9.10 1.60 5 0 -25 10.30 1.40 -4 0 25 0.50 0.50 4 0 -25 0.20 0.40 -4 0 25 1.60 0.70 -3 0 25 31.90 2.90 -3 0 25 22.40 3.10 3 0 -25 33.50 3.10 -3 0 25 22.40 2.90 -2 0 25 0.20 0.60 -2 0 25 -0.30 0.40 -2 0 25 0.00 1.20 -2 0 25 0.50 0.60 2 0 -25 -0.70 0.40 -1 0 25 1.20 0.60 0 0 25 0.40 0.50 0 0 -25 -2.10 1.40 0 0 -25 -0.50 0.70 0 0 25 -0.10 0.30 -1 0 -25 37.60 4.70 1 0 25 45.00 4.30 -1 0 -25 43.90 4.40 2 0 25 -0.30 0.40 -2 0 -25 -0.10 0.50 -2 0 -25 1.00 0.80 -3 0 -25 19.30 2.30 -3 0 -25 21.50 2.60 -5 -1 25 13.10 2.00 5 -1 -25 19.90 2.00 -5 -1 25 14.90 2.00 5 1 -25 16.40 2.50 -5 1 25 15.70 2.10 -5 1 25 20.80 2.50 -4 -1 25 5.10 1.00 -4 -1 25 5.00 1.10 4 1 -25 6.90 1.20 -4 1 25 4.70 1.00 -4 1 25 6.10 1.30 3 -1 -25 85.99 7.60 -3 -1 25 66.19 7.60 -3 1 25 70.19 7.80 3 1 -25 89.39 7.90 -3 1 25 83.19 7.80 -2 -1 25 1.90 0.70 -2 -1 25 0.60 0.80 -2 1 25 2.40 0.90 2 1 -25 3.30 0.80 2 1 -25 1.60 1.00 -1 -1 25 9.70 2.20 1 -1 -25 12.60 1.70 -1 1 25 15.10 1.90 1 1 -25 14.30 2.30 -1 1 25 11.00 2.10 0 -1 25 0.40 0.50 0 -1 -25 -0.10 0.50 0 1 -25 0.70 0.70 0 1 25 0.70 0.40 0 1 -25 -0.10 0.60 0 1 25 0.40 0.80 -1 -1 -25 5.80 1.70 -1 -1 -25 4.50 1.20 -1 1 -25 3.70 0.80 1 1 25 4.80 1.30 -2 -1 -25 16.40 2.30 -2 -1 -25 15.40 1.90 2 1 25 13.90 2.00 -2 1 -25 11.20 1.80 -3 -1 -25 22.00 2.70 -3 -1 -25 16.70 2.30 3 1 25 20.80 2.20 -3 1 -25 22.00 2.70 -4 -2 25 46.30 4.90 4 -2 -25 47.70 4.80 4 2 -25 47.60 4.90 -3 -2 25 28.30 3.30 -3 -2 25 35.40 3.50 3 -2 -25 38.80 3.40 -3 -2 25 25.50 3.30 3 2 -25 33.20 3.90 2 -2 -25 0.20 0.40 -2 -2 25 0.10 0.40 -2 -2 25 -0.40 0.50 2 2 -25 -0.30 0.50 2 2 -25 1.20 1.20 -2 2 25 -0.10 0.30 1 -2 -25 24.00 2.90 -1 -2 25 23.50 2.80 -1 2 25 23.40 2.80 0 -2 25 115.99 10.30 0 -2 -25 99.49 10.10 0 2 25 120.39 10.40 0 2 -25 96.89 10.50 1 -2 25 0.70 0.40 -1 -2 -25 0.50 0.40 -1 2 -25 -0.20 0.50 -1 2 -25 2.90 1.10 1 2 25 0.90 0.50 -2 -2 -25 57.59 6.20 2 2 25 67.19 6.20 -2 -3 25 0.80 0.40 -2 -3 25 0.30 0.50 2 -3 -25 0.40 0.40 2 3 -25 -0.50 0.40 -2 3 25 0.20 0.40 1 -3 -25 6.00 1.10 0 -3 25 32.50 3.30 0 3 25 31.00 3.40 2 0 -26 5.50 1.10 -2 0 26 4.70 1.00 1 0 -26 0.50 0.40 -1 0 26 0.60 0.60 0 0 26 9.60 1.50 0 0 -26 9.30 1.40 -2 1 26 9.00 1.30 -1 -1 26 -0.10 0.30 1 -1 -26 -0.40 0.30 -1 1 26 0.00 0.40 1 1 -26 0.20 0.80 0 1 26 4.20 0.80 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 87990 ####################################################################### # # This file contains crystal structure data downloaded from the # Cambridge Structural Database (CSD) hosted by the Cambridge # Crystallographic Data Centre (CCDC). # # Full information about CCDC data access policies and citation # guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 # # Audit and citation data items may have been added by the CCDC. # Please retain this information to preserve the provenance of # this file and to allow appropriate attribution of the data. # ####################################################################### data_zzy119 _database_code_depnum_ccdc_archive 'CCDC 2086418' loop_ _audit_author_name _audit_author_address 'Qilin Wang' ;Henan University China ; _audit_update_record ; 2021-05-28 deposited with the CCDC. 2021-11-08 downloaded from the CCDC. ; _audit_creation_date 2020-06-24 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _shelx_SHELXL_version_number 2014/7 _chemical_name_common ? _chemical_name_systematic ? _chemical_formula_moiety 'C26 H26 N4 O3' _chemical_formula_sum 'C26 H26 N4 O3' _chemical_formula_weight 442.51 _chemical_melting_point ? _chemical_oxdiff_formula C14H15N2O4 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.5216(3) _cell_length_b 10.7823(4) _cell_length_c 12.6332(5) _cell_angle_alpha 106.178(4) _cell_angle_beta 93.800(3) _cell_angle_gamma 114.614(3) _cell_volume 1107.47(8) _cell_formula_units_Z 2 _cell_measurement_reflns_used 2433 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 67.7780 _cell_measurement_theta_min 4.7750 _shelx_estimated_absorpt_T_max 0.938 _shelx_estimated_absorpt_T_min 0.859 _exptl_absorpt_coefficient_mu 0.715 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.86956 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_special_details ? _exptl_crystal_colour yellow _exptl_crystal_colour_primary yellow _exptl_crystal_density_diffrn 1.327 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description prism _exptl_crystal_F_000 468 _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.09 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0229 _diffrn_reflns_av_unetI/netI 0.0326 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_number 7986 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_theta_full 67.068 _diffrn_reflns_theta_max 67.068 _diffrn_reflns_theta_min 3.725 _diffrn_ambient_temperature 293(2) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 16.2312 _diffrn_detector_type Eos _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames #-------------------------------------------------------------------------- 1 \w -52.00 35.00 0.50 1.50 -- -33.50 57.00 -60.00 174 2 \w -108.00 -32.00 0.50 1.50 -- -33.50 178.00 120.00 152 3 \w -102.00 -15.00 0.50 1.50 -- -33.50 -57.00 150.00 174 4 \w -34.00 59.00 0.50 1.50 -- 36.47 -37.00-120.00 186 5 \w 57.00 110.00 0.50 1.50 -- 36.47 178.00-180.00 106 6 \w 57.00 110.00 0.50 1.50 -- 36.47 178.00 150.00 106 7 \w 14.00 107.00 0.50 1.50 -- 36.47 37.00 60.00 186 8 \w -4.00 53.00 0.50 1.50 -- 36.47 -99.00 30.00 114 9 \w 11.00 40.00 0.50 1.50 -- 36.47 77.00 60.00 58 10 \w -32.00 19.00 0.50 1.50 -- 36.47 -77.00 120.00 102 11 \w 40.00 65.00 0.50 1.50 -- 36.47 -77.00 120.00 50 12 \w 31.00 105.00 0.50 1.50 -- 36.47 57.00 -30.00 148 13 \w 19.00 72.00 0.50 1.50 -- 36.47 -99.00 120.00 106 14 \w 5.00 75.00 0.50 1.50 -- 36.47 -99.00 -90.00 140 15 \w 61.00 105.00 0.50 1.50 -- 36.47 77.00 60.00 88 16 \w 152.00 178.00 0.50 6.50 -- 108.00 111.00 150.00 52 17 \w 44.00 99.00 0.50 6.50 -- 108.00-111.00 150.00 110 18 \w 38.00 127.00 0.50 6.50 -- 108.00 -45.00 0.00 178 19 \w 80.00 132.00 0.50 6.50 -- 108.00 -77.00 90.00 104 20 \w 76.00 108.00 0.50 6.50 -- 108.00 -94.00 -60.00 64 21 \w 45.00 123.00 0.50 6.50 -- 108.00 -45.00-180.00 156 22 \w 97.00 149.00 0.50 6.50 -- 108.00 30.00 30.00 104 23 \w 37.00 122.00 0.50 6.50 -- 108.00 -30.00 90.00 170 24 \w 76.00 109.00 0.50 6.50 -- 108.00 -94.00-180.00 66 25 \w 68.00 109.00 0.50 6.50 -- 108.00-111.00 90.00 82 26 \w 40.00 127.00 0.50 6.50 -- 108.00 -45.00 -90.00 174 27 \w 60.00 101.00 0.50 6.50 -- 108.00 -94.00 -90.00 82 28 \w 38.00 178.00 0.50 6.50 -- 108.00 0.00 150.00 280 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'Xcalibur, Eos, Gemini' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 -0.0063998000 _diffrn_orient_matrix_UB_12 0.0251273000 _diffrn_orient_matrix_UB_13 0.1253772000 _diffrn_orient_matrix_UB_21 -0.1810276000 _diffrn_orient_matrix_UB_22 -0.0903974000 _diffrn_orient_matrix_UB_23 -0.0325428000 _diffrn_orient_matrix_UB_31 0.0174674000 _diffrn_orient_matrix_UB_32 -0.1381035000 _diffrn_orient_matrix_UB_33 -0.0088731000 _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_source 'fine-focus sealed X-ray tube' _diffrn_source_type 'Enhance (Cu) X-ray Source' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 2883 _reflns_number_total 3949 _reflns_odcompleteness_completeness 99.92 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 66.97 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement 'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)' _computing_data_collection 'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)' _computing_data_reduction 'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'ShelXS (Sheldrick, 2008)' _refine_diff_density_max 0.334 _refine_diff_density_min -0.206 _refine_diff_density_rms 0.041 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 326 _refine_ls_number_reflns 3949 _refine_ls_number_restraints 40 _refine_ls_R_factor_all 0.0763 _refine_ls_R_factor_gt 0.0570 _refine_ls_restrained_S_all 1.063 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.1040P)^2^+0.0918P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1642 _refine_ls_wR_factor_ref 0.1847 _refine_special_details ? _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups, All N(H) groups 2. Restrained distances C21A-N4 1.45 with sigma of 0.02 C25A-C24A 1.52 with sigma of 0.02 C24A-C23A 1.52 with sigma of 0.02 C26A-C25A 1.52 with sigma of 0.02 3. Uiso/Uaniso restraints and constraints Uanis(N4) \\sim Ueq, Uanis(C22) \\sim Ueq, Uanis(C26) \\sim Ueq, Uanis(C25) \\sim Ueq, Uanis(C24) \\sim Ueq, Uanis(C23) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02 Uanis(C20) = Uanis(C20A) Uanis(C21) = Uanis(C21A) Uanis(N4) = Uanis(N4A) Uanis(C22) = Uanis(C22A) Uanis(C23) = Uanis(C23A) Uanis(C24) = Uanis(C24A) Uanis(C25) = Uanis(C25A) Uanis(C26) = Uanis(C26A) 4. Others Sof(N4A)=Sof(C20A)=Sof(H20A)=Sof(C21A)=Sof(H21A)=Sof(C22A)=Sof(H22C)= Sof(H22D)=Sof(C23A)=Sof(H23C)=Sof(H23D)=Sof(C24A)=Sof(H24C)=Sof(H24D)= Sof(C25A)=Sof(H25C)=Sof(H25D)=Sof(C26A)=Sof(H26C)=Sof(H26D)=1-FVAR(1) Sof(N4)=Sof(C20)=Sof(H20)=Sof(C21)=Sof(H21)=Sof(C22)=Sof(H22A)=Sof(H22B)= Sof(C23)=Sof(H23A)=Sof(H23B)=Sof(C24)=Sof(H24A)=Sof(H24B)=Sof(C25)=Sof(H25A)= Sof(H25B)=Sof(C26)=Sof(H26A)=Sof(H26B)=FVAR(1) 5.a Ternary CH refined with riding coordinates: C9(H9) 5.b Secondary CH2 refined with riding coordinates: C10(H10A,H10B), C22(H22A,H22B), C22A(H22C,H22D), C23(H23A,H23B), C23A(H23C, H23D), C24(H24A,H24B), C24A(H24C,H24D), C25(H25A,H25B), C25A(H25C,H25D), C26(H26A,H26B), C26A(H26C,H26D) 5.c Aromatic/amide H refined with riding coordinates: N1(H1), C5(H5), C6(H6), C7(H7), C8(H8), C13(H13), C14(H14), C15(H15), C16(H16), C17(H17), C20(H20), C20A(H20A), C21(H21), C21A(H21A) ; _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary direct _atom_sites_solution_secondary ? loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group O1 O 0.89738(19) 0.31207(18) 0.50692(17) 0.0676(5) Uani 1 1 d . . . . . O2 O 0.5901(4) -0.3333(3) 0.1411(2) 0.1162(10) Uani 1 1 d . . . . . O3 O 0.8335(4) -0.1799(3) 0.2243(2) 0.1010(9) Uani 1 1 d . . . . . N1 N 0.8373(2) 0.4069(2) 0.37849(19) 0.0578(5) Uani 1 1 d . . . . . H1 H 0.9039 0.4964 0.4120 0.069 Uiso 1 1 calc R . . . . N2 N 0.4428(2) -0.05588(19) 0.31626(17) 0.0556(5) Uani 1 1 d . . . . . N3 N 0.6913(4) -0.2119(3) 0.2005(2) 0.0836(8) Uani 1 1 d . . . . . N4 N 1.1080(7) 0.2046(7) 0.1508(5) 0.0908(17) Uani 0.763(5) 1 d D U P A 1 N4A N 1.057(3) 0.169(3) 0.108(2) 0.0908(17) Uani 0.237(5) 1 d . . P A 2 C1 C 0.8214(2) 0.2996(2) 0.4190(2) 0.0521(5) Uani 1 1 d . . . . . C2 C 0.6917(3) 0.1563(2) 0.33495(19) 0.0478(5) Uani 1 1 d . . . . . C3 C 0.6406(3) 0.2055(2) 0.24592(19) 0.0511(5) Uani 1 1 d . . . . . C4 C 0.7327(3) 0.3553(2) 0.2755(2) 0.0516(5) Uani 1 1 d . . . . . C5 C 0.7174(3) 0.4325(3) 0.2093(2) 0.0612(6) Uani 1 1 d . . . . . H5 H 0.7798 0.5322 0.2310 0.073 Uiso 1 1 calc R . . . . C6 C 0.6066(4) 0.3574(3) 0.1098(2) 0.0733(8) Uani 1 1 d . . . . . H6 H 0.5936 0.4068 0.0633 0.088 Uiso 1 1 calc R . . . . C7 C 0.5146(4) 0.2093(3) 0.0782(2) 0.0796(9) Uani 1 1 d . . . . . H7 H 0.4410 0.1605 0.0103 0.096 Uiso 1 1 calc R . . . . C8 C 0.5299(4) 0.1315(3) 0.1462(2) 0.0686(7) Uani 1 1 d . . . . . H8 H 0.4668 0.0320 0.1246 0.082 Uiso 1 1 calc R . . . . C9 C 0.5605(2) 0.0844(2) 0.39509(18) 0.0448(5) Uani 1 1 d . . . . . H9 H 0.6084 0.0673 0.4572 0.054 Uiso 1 1 calc R . . . . C10 C 0.2793(3) -0.0823(3) 0.3183(3) 0.0709(7) Uani 1 1 d . . . . . H10A H 0.2240 -0.1626 0.3446 0.085 Uiso 1 1 calc R . . . . H10B H 0.2219 -0.1017 0.2444 0.085 Uiso 1 1 calc R . . . . C11 C 0.3015(3) 0.0579(3) 0.4000(2) 0.0597(6) Uani 1 1 d . . . . . C12 C 0.4598(3) 0.1551(2) 0.43977(18) 0.0486(5) Uani 1 1 d . . . . . C13 C 0.5047(3) 0.2914(3) 0.5165(2) 0.0631(6) Uani 1 1 d . . . . . H13 H 0.6111 0.3575 0.5423 0.076 Uiso 1 1 calc R . . . . C14 C 0.3899(4) 0.3285(4) 0.5544(3) 0.0821(9) Uani 1 1 d . . . . . H14 H 0.4191 0.4203 0.6055 0.099 Uiso 1 1 calc R . . . . C15 C 0.2325(4) 0.2302(4) 0.5169(3) 0.0896(10) Uani 1 1 d . . . . . H15 H 0.1564 0.2556 0.5442 0.108 Uiso 1 1 calc R . . . . C16 C 0.1864(3) 0.0947(4) 0.4394(3) 0.0819(9) Uani 1 1 d . . . . . H16 H 0.0800 0.0290 0.4139 0.098 Uiso 1 1 calc R . . . . C17 C 0.4915(3) -0.1446(2) 0.2528(2) 0.0622(7) Uani 1 1 d . . . . . H17 H 0.4181 -0.2389 0.2102 0.075 Uiso 1 1 calc R . . . . C18 C 0.6453(4) -0.1006(3) 0.2489(2) 0.0630(7) Uani 1 1 d . . . . . C19 C 0.7694(3) 0.0521(3) 0.2952(3) 0.0633(7) Uani 1 1 d . . . . . H19 H 0.834(4) 0.069(3) 0.363(3) 0.076 Uiso 1 1 d R . . . . C20 C 0.8552(4) 0.0878(3) 0.1997(3) 0.0577(8) Uani 0.763(5) 1 d . . P A 1 H20 H 0.7981 0.0558 0.1267 0.069 Uiso 0.763(5) 1 calc R . P A 1 C20A C 0.9309(15) 0.1395(12) 0.2706(10) 0.0577(8) Uani 0.237(5) 1 d . . P A 2 H20A H 1.0168 0.2069 0.3288 0.069 Uiso 0.237(5) 1 calc R . P A 2 C21 C 1.0081(6) 0.1630(5) 0.2229(4) 0.0766(13) Uani 0.763(5) 1 d . . P A 1 H21 H 1.0570 0.1929 0.2979 0.092 Uiso 0.763(5) 1 calc R . P A 1 C21A C 0.9429(18) 0.1164(18) 0.1678(15) 0.0766(13) Uani 0.237(5) 1 d D . P A 2 H21A H 0.8485 0.0441 0.1197 0.092 Uiso 0.237(5) 1 calc R . P A 2 C22 C 1.0428(9) 0.1886(9) 0.0365(6) 0.097(2) Uani 0.763(5) 1 d . U P A 1 H22A H 0.9524 0.0939 0.0032 0.117 Uiso 0.763(5) 1 calc R . P A 1 H22B H 1.1218 0.1929 -0.0090 0.117 Uiso 0.763(5) 1 calc R . P A 1 C22A C 0.986(4) 0.170(3) 0.000(2) 0.097(2) Uani 0.237(5) 1 d . . P A 2 H22C H 1.0328 0.1392 -0.0615 0.117 Uiso 0.237(5) 1 calc R . P A 2 H22D H 0.8725 0.1129 -0.0195 0.117 Uiso 0.237(5) 1 calc R . P A 2 C23 C 0.9899(11) 0.3085(14) 0.0327(16) 0.106(2) Uani 0.763(5) 1 d . U P A 1 H23A H 0.9606 0.3011 -0.0447 0.127 Uiso 0.763(5) 1 calc R . P A 1 H23B H 0.8999 0.2971 0.0680 0.127 Uiso 0.763(5) 1 calc R . P A 1 C23A C 1.032(4) 0.315(5) 0.034(6) 0.106(2) Uani 0.237(5) 1 d D . P A 2 H23C H 0.9709 0.3284 0.0911 0.127 Uiso 0.237(5) 1 calc R . P A 2 H23D H 0.9849 0.3271 -0.0300 0.127 Uiso 0.237(5) 1 calc R . P A 2 C24 C 1.1295(9) 0.4523(9) 0.0960(7) 0.116(2) Uani 0.763(5) 1 d . U P A 1 H24A H 1.0977 0.5285 0.1038 0.139 Uiso 0.763(5) 1 calc R . P A 1 H24B H 1.2115 0.4686 0.0523 0.139 Uiso 0.763(5) 1 calc R . P A 1 C24A C 1.188(3) 0.451(3) 0.080(3) 0.116(2) Uani 0.237(5) 1 d D . P A 2 H24C H 1.2625 0.4472 0.0316 0.139 Uiso 0.237(5) 1 calc R . P A 2 H24D H 1.1741 0.5364 0.0867 0.139 Uiso 0.237(5) 1 calc R . P A 2 C25 C 1.1976(11) 0.4627(10) 0.2129(8) 0.120(2) Uani 0.763(5) 1 d . U P A 1 H25A H 1.2900 0.5558 0.2475 0.144 Uiso 0.763(5) 1 calc R . P A 1 H25B H 1.1199 0.4580 0.2596 0.144 Uiso 0.763(5) 1 calc R . P A 1 C25A C 1.242(4) 0.448(3) 0.193(3) 0.120(2) Uani 0.237(5) 1 d D . P A 2 H25C H 1.1724 0.4582 0.2439 0.144 Uiso 0.237(5) 1 calc R . P A 2 H25D H 1.3495 0.5213 0.2277 0.144 Uiso 0.237(5) 1 calc R . P A 2 C26 C 1.2431(9) 0.3436(8) 0.2091(6) 0.113(2) Uani 0.763(5) 1 d . U P A 1 H26A H 1.3296 0.3541 0.1700 0.135 Uiso 0.763(5) 1 calc R . P A 1 H26B H 1.2779 0.3496 0.2851 0.135 Uiso 0.763(5) 1 calc R . P A 1 C26A C 1.228(3) 0.297(3) 0.156(2) 0.113(2) Uani 0.237(5) 1 d D . P A 2 H26C H 1.2762 0.2836 0.2194 0.135 Uiso 0.237(5) 1 calc R . P A 2 H26D H 1.2898 0.2893 0.0980 0.135 Uiso 0.237(5) 1 calc R . P A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.0501(9) 0.0521(9) 0.0927(13) 0.0329(9) -0.0044(8) 0.0135(7) O2 0.199(3) 0.0638(13) 0.0939(17) 0.0084(12) 0.0197(18) 0.0796(17) O3 0.146(2) 0.0890(16) 0.130(2) 0.0617(15) 0.0795(18) 0.0870(17) N1 0.0503(10) 0.0399(9) 0.0821(14) 0.0262(9) 0.0117(9) 0.0165(8) N2 0.0565(11) 0.0406(9) 0.0594(11) 0.0147(8) 0.0053(9) 0.0149(8) N3 0.153(3) 0.0663(15) 0.0727(15) 0.0393(13) 0.0491(17) 0.0739(18) N4 0.096(4) 0.103(4) 0.122(5) 0.068(4) 0.062(3) 0.065(3) N4A 0.096(4) 0.103(4) 0.122(5) 0.068(4) 0.062(3) 0.065(3) C1 0.0406(11) 0.0445(11) 0.0755(15) 0.0268(10) 0.0134(10) 0.0189(9) C2 0.0529(12) 0.0396(10) 0.0573(12) 0.0214(9) 0.0178(9) 0.0227(9) C3 0.0687(14) 0.0422(11) 0.0536(12) 0.0203(9) 0.0234(10) 0.0313(10) C4 0.0581(13) 0.0459(11) 0.0631(13) 0.0236(10) 0.0251(10) 0.0297(10) C5 0.0784(16) 0.0472(12) 0.0775(16) 0.0327(12) 0.0324(13) 0.0365(12) C6 0.119(2) 0.0684(16) 0.0615(15) 0.0349(13) 0.0303(15) 0.0591(17) C7 0.130(3) 0.0646(16) 0.0488(13) 0.0179(12) 0.0097(15) 0.0510(17) C8 0.106(2) 0.0431(12) 0.0528(13) 0.0121(10) 0.0129(13) 0.0327(13) C9 0.0454(11) 0.0395(10) 0.0478(11) 0.0170(8) 0.0071(8) 0.0167(8) C10 0.0486(13) 0.0678(16) 0.0805(17) 0.0297(14) -0.0044(12) 0.0116(12) C11 0.0511(13) 0.0718(15) 0.0676(15) 0.0409(13) 0.0096(10) 0.0278(11) C12 0.0506(12) 0.0548(12) 0.0504(11) 0.0262(10) 0.0138(9) 0.0272(10) C13 0.0690(15) 0.0636(15) 0.0593(14) 0.0171(11) 0.0185(11) 0.0339(13) C14 0.104(2) 0.092(2) 0.0791(19) 0.0319(16) 0.0375(17) 0.066(2) C15 0.093(2) 0.121(3) 0.107(3) 0.062(2) 0.0476(19) 0.078(2) C16 0.0532(15) 0.111(2) 0.111(2) 0.066(2) 0.0239(15) 0.0455(16) C17 0.0898(19) 0.0369(11) 0.0540(13) 0.0154(9) 0.0068(12) 0.0245(12) C18 0.106(2) 0.0487(13) 0.0574(13) 0.0270(11) 0.0301(13) 0.0481(14) C19 0.0767(17) 0.0548(13) 0.0871(18) 0.0400(13) 0.0412(14) 0.0424(13) C20 0.073(2) 0.0516(17) 0.0600(19) 0.0216(15) 0.0250(16) 0.0351(16) C20A 0.073(2) 0.0516(17) 0.0600(19) 0.0216(15) 0.0250(16) 0.0351(16) C21 0.087(3) 0.092(3) 0.096(4) 0.060(3) 0.043(2) 0.059(3) C21A 0.087(3) 0.092(3) 0.096(4) 0.060(3) 0.043(2) 0.059(3) C22 0.119(6) 0.089(3) 0.101(5) 0.043(4) 0.058(4) 0.049(4) C22A 0.119(6) 0.089(3) 0.101(5) 0.043(4) 0.058(4) 0.049(4) C23 0.126(6) 0.100(3) 0.110(3) 0.049(2) 0.031(6) 0.059(4) C23A 0.126(6) 0.100(3) 0.110(3) 0.049(2) 0.031(6) 0.059(4) C24 0.138(6) 0.088(3) 0.131(4) 0.067(3) 0.041(4) 0.039(4) C24A 0.138(6) 0.088(3) 0.131(4) 0.067(3) 0.041(4) 0.039(4) C25 0.132(6) 0.106(3) 0.122(4) 0.062(3) 0.032(3) 0.038(3) C25A 0.132(6) 0.106(3) 0.122(4) 0.062(3) 0.032(3) 0.038(3) C26 0.096(3) 0.134(5) 0.129(5) 0.076(4) 0.050(4) 0.048(4) C26A 0.096(3) 0.134(5) 0.129(5) 0.076(4) 0.050(4) 0.048(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1 C1 1.227(3) . ? O2 N3 1.229(4) . ? O3 N3 1.242(4) . ? N1 H1 0.8600 . ? N1 C1 1.348(3) . ? N1 C4 1.399(3) . ? N2 C9 1.461(3) . ? N2 C10 1.464(3) . ? N2 C17 1.328(3) . ? N3 C18 1.439(3) . ? N4 C21 1.386(8) . ? N4 C22 1.468(8) . ? N4 C26 1.448(9) . ? N4A C21A 1.38(3) . ? N4A C22A 1.49(3) . ? N4A C26A 1.57(4) . ? C1 C2 1.537(3) . ? C2 C3 1.502(3) . ? C2 C9 1.545(3) . ? C2 C19 1.578(3) . ? C3 C4 1.400(3) . ? C3 C8 1.378(4) . ? C4 C5 1.373(3) . ? C5 H5 0.9300 . ? C5 C6 1.376(4) . ? C6 H6 0.9300 . ? C6 C7 1.382(4) . ? C7 H7 0.9300 . ? C7 C8 1.396(4) . ? C8 H8 0.9300 . ? C9 H9 0.9800 . ? C9 C12 1.504(3) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C10 C11 1.493(4) . ? C11 C12 1.383(3) . ? C11 C16 1.390(4) . ? C12 C13 1.382(3) . ? C13 H13 0.9300 . ? C13 C14 1.383(4) . ? C14 H14 0.9300 . ? C14 C15 1.377(5) . ? C15 H15 0.9300 . ? C15 C16 1.377(5) . ? C16 H16 0.9300 . ? C17 H17 0.9300 . ? C17 C18 1.347(4) . ? C18 C19 1.483(4) . ? C19 H19 0.94(3) . ? C19 C20 1.550(4) . ? C19 C20A 1.540(12) . ? C20 H20 0.9300 . ? C20 C21 1.300(6) . ? C20A H20A 0.9300 . ? C20A C21A 1.27(2) . ? C21 H21 0.9300 . ? C21A H21A 0.9300 . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C22 C23 1.581(18) . ? C22A H22C 0.9700 . ? C22A H22D 0.9700 . ? C22A C23A 1.36(6) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C23 C24 1.505(10) . ? C23A H23C 0.9700 . ? C23A H23D 0.9700 . ? C23A C24A 1.51(2) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C24 C25 1.528(9) . ? C24A H24C 0.9700 . ? C24A H24D 0.9700 . ? C24A C25A 1.50(2) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C25 C26 1.508(10) . ? C25A H25C 0.9700 . ? C25A H25D 0.9700 . ? C25A C26A 1.513(19) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C26A H26C 0.9700 . ? C26A H26D 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 N1 H1 124.0 . . ? C1 N1 C4 111.99(19) . . ? C4 N1 H1 124.0 . . ? C9 N2 C10 113.92(19) . . ? C17 N2 C9 118.9(2) . . ? C17 N2 C10 127.2(2) . . ? O2 N3 O3 123.3(3) . . ? O2 N3 C18 119.6(3) . . ? O3 N3 C18 117.1(3) . . ? C21 N4 C22 120.1(5) . . ? C21 N4 C26 110.8(5) . . ? C26 N4 C22 113.5(6) . . ? C21A N4A C22A 111(2) . . ? C21A N4A C26A 128(2) . . ? C22A N4A C26A 111(2) . . ? O1 C1 N1 126.6(2) . . ? O1 C1 C2 125.20(19) . . ? N1 C1 C2 108.2(2) . . ? C1 C2 C9 109.78(18) . . ? C1 C2 C19 107.18(19) . . ? C3 C2 C1 102.06(17) . . ? C3 C2 C9 114.53(18) . . ? C3 C2 C19 115.52(19) . . ? C9 C2 C19 107.37(17) . . ? C4 C3 C2 108.6(2) . . ? C8 C3 C2 132.4(2) . . ? C8 C3 C4 118.9(2) . . ? C3 C4 N1 109.1(2) . . ? C5 C4 N1 128.1(2) . . ? C5 C4 C3 122.8(2) . . ? C4 C5 H5 121.1 . . ? C4 C5 C6 117.7(2) . . ? C6 C5 H5 121.1 . . ? C5 C6 H6 119.6 . . ? C5 C6 C7 120.7(2) . . ? C7 C6 H6 119.6 . . ? C6 C7 H7 119.4 . . ? C6 C7 C8 121.3(3) . . ? C8 C7 H7 119.4 . . ? C3 C8 C7 118.5(2) . . ? C3 C8 H8 120.7 . . ? C7 C8 H8 120.7 . . ? N2 C9 C2 109.31(17) . . ? N2 C9 H9 108.1 . . ? N2 C9 C12 102.10(17) . . ? C2 C9 H9 108.1 . . ? C12 C9 C2 120.44(17) . . ? C12 C9 H9 108.1 . . ? N2 C10 H10A 111.4 . . ? N2 C10 H10B 111.4 . . ? N2 C10 C11 101.83(19) . . ? H10A C10 H10B 109.3 . . ? C11 C10 H10A 111.4 . . ? C11 C10 H10B 111.4 . . ? C12 C11 C10 111.6(2) . . ? C12 C11 C16 120.3(3) . . ? C16 C11 C10 128.1(3) . . ? C11 C12 C9 110.2(2) . . ? C13 C12 C9 129.3(2) . . ? C13 C12 C11 120.3(2) . . ? C12 C13 H13 120.4 . . ? C12 C13 C14 119.3(3) . . ? C14 C13 H13 120.4 . . ? C13 C14 H14 119.8 . . ? C15 C14 C13 120.3(3) . . ? C15 C14 H14 119.8 . . ? C14 C15 H15 119.6 . . ? C16 C15 C14 120.8(3) . . ? C16 C15 H15 119.6 . . ? C11 C16 H16 120.5 . . ? C15 C16 C11 119.0(3) . . ? C15 C16 H16 120.5 . . ? N2 C17 H17 119.4 . . ? N2 C17 C18 121.3(2) . . ? C18 C17 H17 119.4 . . ? N3 C18 C19 118.5(3) . . ? C17 C18 N3 116.7(3) . . ? C17 C18 C19 124.7(2) . . ? C2 C19 H19 102.6(19) . . ? C18 C19 C2 110.0(2) . . ? C18 C19 H19 111.0(19) . . ? C18 C19 C20 107.6(2) . . ? C18 C19 C20A 135.3(5) . . ? C20 C19 C2 109.2(2) . . ? C20 C19 H19 116.4(19) . . ? C20A C19 C2 108.3(4) . . ? C20A C19 H19 81.8(19) . . ? C19 C20 H20 120.4 . . ? C21 C20 C19 119.1(4) . . ? C21 C20 H20 120.4 . . ? C19 C20A H20A 121.1 . . ? C21A C20A C19 117.7(12) . . ? C21A C20A H20A 121.1 . . ? N4 C21 H21 115.7 . . ? C20 C21 N4 128.7(5) . . ? C20 C21 H21 115.7 . . ? N4A C21A H21A 111.1 . . ? C20A C21A N4A 137.7(18) . . ? C20A C21A H21A 111.1 . . ? N4 C22 H22A 108.9 . . ? N4 C22 H22B 108.9 . . ? N4 C22 C23 113.5(9) . . ? H22A C22 H22B 107.7 . . ? C23 C22 H22A 108.9 . . ? C23 C22 H22B 108.9 . . ? N4A C22A H22C 112.4 . . ? N4A C22A H22D 112.4 . . ? H22C C22A H22D 110.0 . . ? C23A C22A N4A 97(4) . . ? C23A C22A H22C 112.4 . . ? C23A C22A H22D 112.4 . . ? C22 C23 H23A 110.5 . . ? C22 C23 H23B 110.5 . . ? H23A C23 H23B 108.7 . . ? C24 C23 C22 106.3(9) . . ? C24 C23 H23A 110.5 . . ? C24 C23 H23B 110.5 . . ? C22A C23A H23C 103.3 . . ? C22A C23A H23D 103.3 . . ? C22A C23A C24A 135(4) . . ? H23C C23A H23D 105.2 . . ? C24A C23A H23C 103.3 . . ? C24A C23A H23D 103.3 . . ? C23 C24 H24A 108.9 . . ? C23 C24 H24B 108.9 . . ? C23 C24 C25 113.3(10) . . ? H24A C24 H24B 107.7 . . ? C25 C24 H24A 108.9 . . ? C25 C24 H24B 108.9 . . ? C23A C24A H24C 111.2 . . ? C23A C24A H24D 111.2 . . ? H24C C24A H24D 109.1 . . ? C25A C24A C23A 103(4) . . ? C25A C24A H24C 111.2 . . ? C25A C24A H24D 111.2 . . ? C24 C25 H25A 109.1 . . ? C24 C25 H25B 109.1 . . ? H25A C25 H25B 107.8 . . ? C26 C25 C24 112.5(7) . . ? C26 C25 H25A 109.1 . . ? C26 C25 H25B 109.1 . . ? C24A C25A H25C 112.1 . . ? C24A C25A H25D 112.1 . . ? C24A C25A C26A 98(2) . . ? H25C C25A H25D 109.7 . . ? C26A C25A H25C 112.1 . . ? C26A C25A H25D 112.1 . . ? N4 C26 C25 109.2(7) . . ? N4 C26 H26A 109.8 . . ? N4 C26 H26B 109.8 . . ? C25 C26 H26A 109.8 . . ? C25 C26 H26B 109.8 . . ? H26A C26 H26B 108.3 . . ? N4A C26A H26C 108.2 . . ? N4A C26A H26D 108.2 . . ? C25A C26A N4A 116(3) . . ? C25A C26A H26C 108.2 . . ? C25A C26A H26D 108.2 . . ? H26C C26A H26D 107.4 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1 O1 0.86 2.05 2.890(2) 165.2 2_766 loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 C1 C2 C3 179.7(2) . . . . ? O1 C1 C2 C9 57.8(3) . . . . ? O1 C1 C2 C19 -58.5(3) . . . . ? O2 N3 C18 C17 18.0(4) . . . . ? O2 N3 C18 C19 -164.8(3) . . . . ? O3 N3 C18 C17 -160.2(2) . . . . ? O3 N3 C18 C19 17.1(4) . . . . ? N1 C1 C2 C3 -1.0(2) . . . . ? N1 C1 C2 C9 -122.9(2) . . . . ? N1 C1 C2 C19 120.8(2) . . . . ? N1 C4 C5 C6 179.1(2) . . . . ? N2 C9 C12 C11 6.4(2) . . . . ? N2 C9 C12 C13 -178.7(2) . . . . ? N2 C10 C11 C12 0.7(3) . . . . ? N2 C10 C11 C16 -177.2(3) . . . . ? N2 C17 C18 N3 165.4(2) . . . . ? N2 C17 C18 C19 -11.6(4) . . . . ? N3 C18 C19 C2 175.6(2) . . . . ? N3 C18 C19 C20 56.7(3) . . . . ? N3 C18 C19 C20A 28.1(8) . . . . ? N4 C22 C23 C24 52.7(12) . . . . ? N4A C22A C23A C24A 58(8) . . . . ? C1 N1 C4 C3 0.6(3) . . . . ? C1 N1 C4 C5 -178.9(2) . . . . ? C1 C2 C3 C4 1.3(2) . . . . ? C1 C2 C3 C8 179.1(3) . . . . ? C1 C2 C9 N2 -176.54(16) . . . . ? C1 C2 C9 C12 65.8(2) . . . . ? C1 C2 C19 C18 159.5(2) . . . . ? C1 C2 C19 C20 -82.6(3) . . . . ? C1 C2 C19 C20A -44.0(6) . . . . ? C2 C3 C4 N1 -1.3(2) . . . . ? C2 C3 C4 C5 178.3(2) . . . . ? C2 C3 C8 C7 -177.3(3) . . . . ? C2 C9 C12 C11 127.6(2) . . . . ? C2 C9 C12 C13 -57.5(3) . . . . ? C2 C19 C20 C21 102.3(4) . . . . ? C2 C19 C20A C21A -106.4(11) . . . . ? C3 C2 C9 N2 69.4(2) . . . . ? C3 C2 C9 C12 -48.3(3) . . . . ? C3 C2 C19 C18 -87.6(2) . . . . ? C3 C2 C19 C20 30.3(3) . . . . ? C3 C2 C19 C20A 68.9(6) . . . . ? C3 C4 C5 C6 -0.3(4) . . . . ? C4 N1 C1 O1 179.6(2) . . . . ? C4 N1 C1 C2 0.3(3) . . . . ? C4 C3 C8 C7 0.3(4) . . . . ? C4 C5 C6 C7 -0.1(4) . . . . ? C5 C6 C7 C8 0.5(5) . . . . ? C6 C7 C8 C3 -0.6(5) . . . . ? C8 C3 C4 N1 -179.4(2) . . . . ? C8 C3 C4 C5 0.1(4) . . . . ? C9 N2 C10 C11 3.7(3) . . . . ? C9 N2 C17 C18 -8.8(3) . . . . ? C9 C2 C3 C4 119.9(2) . . . . ? C9 C2 C3 C8 -62.4(3) . . . . ? C9 C2 C19 C18 41.6(3) . . . . ? C9 C2 C19 C20 159.5(2) . . . . ? C9 C2 C19 C20A -161.9(5) . . . . ? C9 C12 C13 C14 -173.3(2) . . . . ? C10 N2 C9 C2 -134.8(2) . . . . ? C10 N2 C9 C12 -6.2(2) . . . . ? C10 N2 C17 C18 171.8(2) . . . . ? C10 C11 C12 C9 -4.6(3) . . . . ? C10 C11 C12 C13 180.0(2) . . . . ? C10 C11 C16 C15 178.8(3) . . . . ? C11 C12 C13 C14 1.1(4) . . . . ? C12 C11 C16 C15 1.2(4) . . . . ? C12 C13 C14 C15 0.6(4) . . . . ? C13 C14 C15 C16 -1.4(5) . . . . ? C14 C15 C16 C11 0.5(5) . . . . ? C16 C11 C12 C9 173.4(2) . . . . ? C16 C11 C12 C13 -2.0(4) . . . . ? C17 N2 C9 C2 45.7(3) . . . . ? C17 N2 C9 C12 174.38(19) . . . . ? C17 N2 C10 C11 -176.9(2) . . . . ? C17 C18 C19 C2 -7.4(4) . . . . ? C17 C18 C19 C20 -126.3(3) . . . . ? C17 C18 C19 C20A -154.9(7) . . . . ? C18 C19 C20 C21 -138.3(3) . . . . ? C18 C19 C20A C21A 41.4(14) . . . . ? C19 C2 C3 C4 -114.6(2) . . . . ? C19 C2 C3 C8 63.2(3) . . . . ? C19 C2 C9 N2 -60.3(2) . . . . ? C19 C2 C9 C12 -178.0(2) . . . . ? C19 C20 C21 N4 178.7(5) . . . . ? C19 C20A C21A N4A 178(2) . . . . ? C21 N4 C22 C23 76.5(9) . . . . ? C21 N4 C26 C25 -81.8(6) . . . . ? C21A N4A C22A C23A 103(3) . . . . ? C21A N4A C26A C25A -75(3) . . . . ? C22 N4 C21 C20 12.0(9) . . . . ? C22 N4 C26 C25 56.8(8) . . . . ? C22 C23 C24 C25 -51.5(12) . . . . ? C22A N4A C21A C20A -145(2) . . . . ? C22A N4A C26A C25A 67(3) . . . . ? C22A C23A C24A C25A -68(8) . . . . ? C23 C24 C25 C26 55.9(10) . . . . ? C23A C24A C25A C26A 53(3) . . . . ? C24 C25 C26 N4 -55.1(7) . . . . ? C24A C25A C26A N4A -67(3) . . . . ? C26 N4 C21 C20 147.5(5) . . . . ? C26 N4 C22 C23 -57.9(8) . . . . ? C26A N4A C21A C20A -4(4) . . . . ? C26A N4A C22A C23A -45(3) . . . . ? _shelx_res_file ; zzy119.res created by SHELXL-2014/7 TITL zzy119 in P-1 #2 REM reset to P-1 #2 CELL 1.54184 9.52155 10.782304 12.633213 106.1775 93.8002 114.6144 ZERR 2 0.000264 0.000403 0.000527 0.0035 0.0028 0.0031 LATT 1 SFAC C H N O UNIT 52 52 8 6 EQIV $1 2-X,1-Y,1-Z DFIX 1.45 C21A N4 DFIX 1.52 C25A C24A DFIX 1.52 C24A C23A DFIX 1.52 C26A C25A ISOR 0.01 0.02 N4 C22 C26 C25 C24 C23 EADP C20 C20A EADP C21 C21A EADP N4 N4A EADP C22 C22A EADP C23 C23A EADP C24 C24A EADP C25 C25A EADP C26 C26A L.S. 19 0 0 PLAN 20 SIZE 0.22 0.1 0.09 MPLA C1 C2 C3 C4 C5 C6 C7 C8 N1 MPLA C11 C12 C13 C14 C15 C16 HTAB N1 O1_$1 BOND $h conf fmap 2 ACTA REM REM REM WGHT 0.104000 0.091800 FVAR 8.78794 0.76261 O1 4 0.897379 0.312074 0.506916 11.00000 0.05014 0.05212 = 0.09270 0.03287 -0.00441 0.01348 O2 4 0.590068 -0.333300 0.141119 11.00000 0.19853 0.06381 = 0.09388 0.00842 0.01972 0.07958 O3 4 0.833474 -0.179854 0.224268 11.00000 0.14591 0.08901 = 0.13025 0.06168 0.07947 0.08705 N1 3 0.837313 0.406851 0.378492 11.00000 0.05033 0.03995 = 0.08213 0.02619 0.01166 0.01649 AFIX 43 H1 2 0.903880 0.496365 0.411983 11.00000 -1.20000 AFIX 0 N2 3 0.442767 -0.055882 0.316259 11.00000 0.05648 0.04061 = 0.05940 0.01470 0.00526 0.01485 N3 3 0.691262 -0.211893 0.200523 11.00000 0.15322 0.06633 = 0.07265 0.03933 0.04912 0.07394 PART 1 N4 3 1.108041 0.204570 0.150846 21.00000 0.09553 0.10321 = 0.12236 0.06827 0.06156 0.06476 PART 0 PART 2 N4A 3 1.056673 0.168523 0.108190 -21.00000 0.09553 0.10321 = 0.12236 0.06827 0.06156 0.06476 PART 0 C1 1 0.821366 0.299582 0.418993 11.00000 0.04060 0.04450 = 0.07547 0.02678 0.01336 0.01891 C2 1 0.691707 0.156339 0.334951 11.00000 0.05288 0.03959 = 0.05733 0.02143 0.01779 0.02275 C3 1 0.640637 0.205488 0.245924 11.00000 0.06871 0.04219 = 0.05358 0.02026 0.02339 0.03126 C4 1 0.732729 0.355323 0.275494 11.00000 0.05814 0.04589 = 0.06308 0.02359 0.02505 0.02972 C5 1 0.717418 0.432515 0.209294 11.00000 0.07837 0.04719 = 0.07755 0.03269 0.03238 0.03652 AFIX 43 H5 2 0.779777 0.532156 0.230971 11.00000 -1.20000 AFIX 0 C6 1 0.606642 0.357385 0.109780 11.00000 0.11909 0.06836 = 0.06148 0.03488 0.03029 0.05912 AFIX 43 H6 2 0.593593 0.406838 0.063280 11.00000 -1.20000 AFIX 0 C7 1 0.514579 0.209289 0.078168 11.00000 0.13042 0.06464 = 0.04876 0.01786 0.00969 0.05099 AFIX 43 H7 2 0.440991 0.160499 0.010293 11.00000 -1.20000 AFIX 0 C8 1 0.529911 0.131508 0.146156 11.00000 0.10554 0.04311 = 0.05275 0.01212 0.01290 0.03271 AFIX 43 H8 2 0.466815 0.031994 0.124604 11.00000 -1.20000 AFIX 0 C9 1 0.560482 0.084360 0.395091 11.00000 0.04537 0.03951 = 0.04778 0.01704 0.00711 0.01673 AFIX 13 H9 2 0.608411 0.067321 0.457201 11.00000 -1.20000 AFIX 0 C10 1 0.279286 -0.082299 0.318259 11.00000 0.04855 0.06776 = 0.08051 0.02965 -0.00436 0.01157 AFIX 23 H10A 2 0.223989 -0.162595 0.344557 11.00000 -1.20000 H10B 2 0.221899 -0.101663 0.244433 11.00000 -1.20000 AFIX 0 C11 1 0.301530 0.057860 0.399984 11.00000 0.05109 0.07176 = 0.06759 0.04086 0.00962 0.02778 C12 1 0.459790 0.155128 0.439770 11.00000 0.05056 0.05479 = 0.05042 0.02619 0.01385 0.02716 C13 1 0.504749 0.291434 0.516482 11.00000 0.06902 0.06358 = 0.05929 0.01713 0.01847 0.03394 AFIX 43 H13 2 0.611082 0.357500 0.542326 11.00000 -1.20000 AFIX 0 C14 1 0.389910 0.328510 0.554391 11.00000 0.10403 0.09154 = 0.07906 0.03192 0.03751 0.06560 AFIX 43 H14 2 0.419096 0.420316 0.605500 11.00000 -1.20000 AFIX 0 C15 1 0.232524 0.230191 0.516855 11.00000 0.09350 0.12097 = 0.10691 0.06229 0.04760 0.07765 AFIX 43 H15 2 0.156430 0.255602 0.544167 11.00000 -1.20000 AFIX 0 C16 1 0.186426 0.094746 0.439401 11.00000 0.05318 0.11140 = 0.11095 0.06601 0.02390 0.04547 AFIX 43 H16 2 0.079963 0.028975 0.413858 11.00000 -1.20000 AFIX 0 C17 1 0.491529 -0.144570 0.252792 11.00000 0.08978 0.03687 = 0.05396 0.01536 0.00676 0.02450 AFIX 43 H17 2 0.418103 -0.238856 0.210234 11.00000 -1.20000 AFIX 0 C18 1 0.645298 -0.100557 0.248891 11.00000 0.10553 0.04867 = 0.05736 0.02699 0.03006 0.04805 C19 1 0.769357 0.052077 0.295245 11.00000 0.07671 0.05481 = 0.08711 0.03998 0.04115 0.04239 H19 2 0.833689 0.068823 0.362906 11.00000 -1.20000 PART 1 C20 1 0.855202 0.087775 0.199671 21.00000 0.07282 0.05156 = 0.06001 0.02161 0.02501 0.03510 AFIX 43 H20 2 0.798120 0.055849 0.126686 21.00000 -1.20000 AFIX 0 PART 0 PART 2 C20A 1 0.930913 0.139477 0.270636 -21.00000 0.07282 0.05156 = 0.06001 0.02161 0.02501 0.03510 AFIX 43 H20A 2 1.016848 0.206857 0.328801 -21.00000 -1.20000 AFIX 0 PART 0 PART 1 C21 1 1.008137 0.162979 0.222909 21.00000 0.08672 0.09161 = 0.09555 0.05969 0.04332 0.05936 AFIX 43 H21 2 1.057029 0.192858 0.297916 21.00000 -1.20000 AFIX 0 PART 0 PART 2 C21A 1 0.942901 0.116353 0.167810 -21.00000 0.08672 0.09161 = 0.09555 0.05969 0.04332 0.05936 AFIX 43 H21A 2 0.848467 0.044117 0.119701 -21.00000 -1.20000 AFIX 0 PART 0 PART 1 C22 1 1.042803 0.188627 0.036507 21.00000 0.11863 0.08889 = 0.10081 0.04310 0.05849 0.04948 AFIX 23 H22A 2 0.952416 0.093918 0.003250 21.00000 -1.20000 H22B 2 1.121758 0.192889 -0.008993 21.00000 -1.20000 AFIX 0 PART 0 PART 2 C22A 1 0.986439 0.170124 0.000328 -21.00000 0.11863 0.08889 = 0.10081 0.04310 0.05849 0.04948 AFIX 23 H22C 2 1.032836 0.139154 -0.061547 -21.00000 -1.20000 H22D 2 0.872482 0.112913 -0.019489 -21.00000 -1.20000 AFIX 0 PART 0 PART 1 C23 1 0.989862 0.308455 0.032663 21.00000 0.12559 0.09986 = 0.11025 0.04855 0.03075 0.05910 AFIX 23 H23A 2 0.960606 0.301123 -0.044672 21.00000 -1.20000 H23B 2 0.899931 0.297060 0.067978 21.00000 -1.20000 AFIX 0 PART 0 PART 2 C23A 1 1.031939 0.314793 0.034373 -21.00000 0.12559 0.09986 = 0.11025 0.04855 0.03075 0.05910 AFIX 23 H23C 2 0.970929 0.328446 0.091132 -21.00000 -1.20000 H23D 2 0.984888 0.327102 -0.029993 -21.00000 -1.20000 AFIX 0 PART 0 PART 1 C24 1 1.129504 0.452339 0.095999 21.00000 0.13828 0.08787 = 0.13063 0.06669 0.04120 0.03874 AFIX 23 H24A 2 1.097744 0.528490 0.103848 21.00000 -1.20000 H24B 2 1.211462 0.468567 0.052339 21.00000 -1.20000 AFIX 0 PART 0 PART 2 C24A 1 1.187952 0.450534 0.079692 -21.00000 0.13828 0.08787 = 0.13063 0.06669 0.04120 0.03874 AFIX 23 H24C 2 1.262508 0.447237 0.031575 -21.00000 -1.20000 H24D 2 1.174093 0.536446 0.086727 -21.00000 -1.20000 AFIX 0 PART 0 PART 1 C25 1 1.197573 0.462749 0.212931 21.00000 0.13158 0.10561 = 0.12173 0.06165 0.03247 0.03765 AFIX 23 H25A 2 1.289978 0.555785 0.247520 21.00000 -1.20000 H25B 2 1.119903 0.457970 0.259645 21.00000 -1.20000 AFIX 0 PART 0 PART 2 C25A 1 1.241846 0.447837 0.193035 -21.00000 0.13158 0.10561 = 0.12173 0.06165 0.03247 0.03765 AFIX 23 H25C 2 1.172391 0.458169 0.243925 -21.00000 -1.20000 H25D 2 1.349518 0.521314 0.227660 -21.00000 -1.20000 AFIX 0 PART 0 PART 1 C26 1 1.243149 0.343555 0.209083 21.00000 0.09616 0.13387 = 0.12942 0.07598 0.04979 0.04829 AFIX 23 H26A 2 1.329600 0.354130 0.170036 21.00000 -1.20000 H26B 2 1.277926 0.349633 0.285100 21.00000 -1.20000 AFIX 0 PART 0 PART 2 C26A 1 1.228427 0.296528 0.155696 -21.00000 0.09616 0.13387 = 0.12942 0.07598 0.04979 0.04829 AFIX 23 H26C 2 1.276233 0.283635 0.219410 -21.00000 -1.20000 H26D 2 1.289799 0.289316 0.098033 -21.00000 -1.20000 AFIX 0 HKLF 4 REM zzy119 in P-1 #2 REM R1 = 0.0570 for 2883 Fo > 4sig(Fo) and 0.0763 for all 3949 data REM 326 parameters refined using 40 restraints END WGHT 0.1037 0.0896 REM Highest difference peak 0.334, deepest hole -0.206, 1-sigma level 0.041 Q1 1 1.1057 0.3514 0.3521 11.00000 0.05 0.33 Q2 1 0.7005 0.2846 0.2537 11.00000 0.05 0.20 Q3 1 1.0000 0.5000 0.0000 10.50000 0.05 0.18 Q4 1 0.6489 0.1323 0.3671 11.00000 0.05 0.16 Q5 1 0.6790 -0.2661 0.1225 11.00000 0.05 0.15 Q6 1 0.3873 0.1348 0.3998 11.00000 0.05 0.15 Q7 1 0.3966 0.0247 0.1484 11.00000 0.05 0.15 Q8 1 0.9180 0.3615 0.5594 11.00000 0.05 0.14 Q9 1 0.4776 0.2039 0.4843 11.00000 0.05 0.14 Q10 1 0.7197 0.1031 0.3047 11.00000 0.05 0.14 Q11 1 0.7458 0.2032 0.3815 11.00000 0.05 0.14 Q12 1 0.6288 0.1754 0.1868 11.00000 0.05 0.14 Q13 1 0.8560 0.2241 0.5036 11.00000 0.05 0.14 Q14 1 0.9211 -0.1257 0.2114 11.00000 0.05 0.13 Q15 1 0.2413 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109.303 23 0 -7 -6 139.327 97.8190 17 0 -7 -6 334.776 119.543 18 0 -7 -7-67.3569 77.5428 17 0 -7 -7 1.57385 77.2661 23 0 -7 -7 7.82943 72.5500 19 0 -7 -8 352.920 83.8967 23 0 -8 13 968.325 161.273 26 0 -8 12 72.3166 103.915 26 0 -8 11 2151.62 249.146 26 0 -8 10 1020.58 190.587 26 0 -8 9 60.7435 105.198 26 0 -8 9 402.936 209.433 20 0 -8 8 2333.96 298.851 20 0 -8 8 1964.39 248.228 26 0 -8 7 10348.9 555.673 20 0 -8 6 85.6998 86.3471 18 0 -8 6 436.144 191.652 20 0 -8 5 5980.65 387.411 18 0 -8 5 6684.89 454.881 20 0 -8 4 3826.23 339.004 16 0 -8 4 3687.86 369.922 20 0 -8 3 1120.27 200.763 16 0 -8 3 1703.82 283.454 20 0 -8 2 4552.40 368.649 16 0 -8 2 4750.08 366.976 17 0 -8 1 3290.53 320.532 17 0 -8 1 4300.90 357.320 16 0 -8 0 22850.4 796.560 25 0 -8 0 23661.2 834.406 17 0 -8 -1 398.405 130.652 17 0 -8 -1 438.385 139.293 25 0 -8 -2 12.0746 87.4013 18 0 -8 -2 226.432 122.550 17 0 -8 -3 707.728 167.665 17 0 -8 -3 793.383 153.919 18 0 -8 -4 55.5382 92.3129 17 0 -8 -4-100.973 78.5909 18 0 -8 -5 440.780 130.436 17 0 -8 -6 130.502 85.0585 17 0 -9 12 217.592 105.675 26 0 -9 12 241.137 85.3124 18 0 -9 11 1675.57 203.550 26 0 -9 11 1680.38 188.591 18 0 -9 10 28.5080 88.9959 26 0 -9 10 51.0359 88.9831 18 0 -9 9 163.320 99.5179 26 0 -9 9 229.418 102.704 18 0 -9 8 723.914 148.760 18 0 -9 7 33.4656 107.779 16 0 -9 7-30.8274 76.9602 18 0 -9 6 9184.27 531.601 16 0 -9 6 9963.20 553.627 20 0 -9 5 291.053 127.404 16 0 -9 4 3235.38 323.803 16 0 -9 3 21697.5 802.188 16 0 -9 2 460.139 129.425 17 0 -9 1 3438.86 323.488 17 0 -9 1 3744.44 331.977 25 0 -9 0 45.3668 93.9947 25 0 -9 0 38.5543 91.0776 17 0 -9 -1 3189.64 291.047 25 0 -9 -1 3270.50 314.729 17 0 -9 -2 457.310 141.035 17 0 -9 -3 1561.77 208.037 17 0 -9 -4 33.3986 75.6783 17 0 -9 -5 834.906 128.331 17 0 -10 11 1134.52 161.572 16 0 -10 10 171.126 88.0849 16 0 -10 9 1179.40 189.241 16 0 -10 8 634.420 148.788 16 0 -10 7 1195.33 201.745 16 0 -10 6-6.76985 84.7881 16 0 -10 5 2468.82 275.778 16 0 -10 4 1357.66 211.393 16 0 -10 3 2448.55 269.681 25 0 -10 2 3712.53 309.449 17 0 -10 2 3792.83 323.106 25 0 -10 1 359.588 117.136 25 0 -10 1 646.979 160.385 17 0 -10 0-29.0665 71.1476 25 0 -10 0-24.8988 89.1037 17 0 -10 -1-99.5690 86.6769 17 0 -10 -2 792.124 143.833 17 0 -10 -3 171.124 88.8251 17 0 -11 9 3500.10 233.208 25 0 -11 9 2979.73 235.593 16 0 -11 8 794.689 142.306 16 0 -11 8 996.334 148.489 25 0 -11 7 133.891 89.2914 25 0 -11 7 227.931 90.4581 16 0 -11 6 3090.13 266.957 25 0 -11 6 3182.15 264.916 16 0 -11 5-4.78502 83.1659 25 0 -11 4 177.475 93.2236 25 0 -11 3 27.1321 78.3575 25 0 -11 2 19.9444 73.8324 25 0 -11 1 392.698 106.545 17 0 -11 1 488.324 104.579 25 0 -11 0 313.465 93.1496 17 1 -12 3 1613.60 165.531 25 1 -12 4-45.8085 77.9221 25 1 -12 5 2940.25 230.899 25 1 -12 6 1113.39 149.284 25 1 -12 7 330.598 91.8179 25 1 -11 -1 1527.97 177.688 17 1 -11 0 1120.78 152.116 25 1 -11 0 1078.56 162.254 17 1 -11 1 642.129 135.306 17 1 -11 1 523.697 116.083 25 1 -11 2 7739.61 404.707 17 1 -11 2 7209.97 401.774 25 1 -11 3 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153.851 26 1 -8 -7 429.130 101.433 19 1 -8 -6-17.2450 75.0949 17 1 -8 -5 533.960 150.735 17 1 -8 -4 2997.70 302.028 17 1 -8 -3 83.2860 91.9902 17 1 -8 -2 318.882 115.057 17 1 -8 -2 458.163 143.918 25 1 -8 -1-83.2480 137.615 25 1 -8 -1 48.1433 96.7998 17 1 -8 0 9804.73 522.625 25 1 -8 0 10632.0 548.282 17 1 -8 1 1864.01 237.946 17 1 -8 1 1560.51 223.705 16 1 -8 2 4942.25 359.637 17 1 -8 2 4410.00 359.399 16 1 -8 3 12524.5 1172.71 13 1 -8 3 13214.2 589.926 20 1 -8 3 12296.8 588.630 16 1 -8 4 11852.5 556.628 27 1 -8 4 11596.9 570.050 16 1 -8 5 1593.46 241.546 20 1 -8 6 2531.93 288.579 20 1 -8 7 1717.57 246.188 20 1 -8 8 136.972 148.084 20 1 -8 8-32.2886 112.904 26 1 -8 9 123.499 113.117 26 1 -8 9 284.213 165.388 20 1 -8 10 1211.00 207.247 26 1 -8 11 1977.48 256.571 26 1 -8 12 556.187 152.380 26 1 -8 13 8136.45 411.994 26 1 -7 -8 344.896 98.3492 23 1 -7 -7 1740.55 215.760 19 1 -7 -7 1988.98 216.490 23 1 -7 -6 442.076 141.235 17 1 -7 -6 490.429 135.618 23 1 -7 -5 7682.07 464.610 17 1 -7 -4 7330.22 462.211 17 1 -7 -3 4546.91 368.310 17 1 -7 -2 281.388 116.298 25 1 -7 -2 193.810 109.520 17 1 -7 -1 5007.97 732.418 5 1 -7 -1 3016.80 579.734 13 1 -7 0 9481.73 1001.12 13 1 -7 0 8016.07 886.739 5 1 -7 1 5140.55 723.301 5 1 -7 1 6410.50 757.272 6 1 -7 1 6663.82 818.329 13 1 -7 2 6940.39 821.784 5 -1 7 -2 7753.18 918.196 9 1 -7 2 7242.25 837.445 13 1 -7 2 6481.66 789.941 6 -1 7 -3 21326.8 1514.56 9 1 -7 3 22410.4 1468.01 5 1 -7 3 22946.7 1404.14 13 1 -7 3 21051.4 1429.05 6 1 -7 4 10193.2 1002.33 5 1 -7 4 9226.96 956.724 6 -1 7 -4 9202.47 1028.80 9 1 -7 5 559.337 280.188 6 1 -7 5 235.608 215.717 8 -1 7 -5 25.5306 269.751 9 1 -7 5-249.298 184.345 5 -1 7 -6 4210.51 781.282 9 1 -7 6 3928.07 675.116 8 1 -7 6 2613.54 530.524 6 1 -7 7 563.529 206.119 27 1 -7 8 3200.61 306.147 26 1 -7 8 2854.96 287.889 20 1 -7 9 396.871 134.986 26 1 -7 9 382.379 153.891 20 1 -7 10 27582.8 889.022 26 1 -7 11 70.5286 104.556 26 1 -7 12 6571.06 429.970 26 1 -7 13 822.386 169.870 26 1 -7 14 231.660 106.121 26 -1 7 -14 328.714 89.5425 22 1 -6 -10 93.5829 66.4097 23 1 -6 -9 2.08776 67.9919 23 1 -6 -8 1568.70 207.421 23 1 -6 -7 11795.6 555.686 23 1 -6 -6 7204.85 442.499 17 1 -6 -6 7317.79 443.001 23 1 -6 -5 27533.1 860.145 17 1 -6 -4 119.913 86.3338 17 1 -6 -3 917.424 334.220 13 1 -6 -2 9344.79 959.611 13 1 -6 -1 1052.64 299.769 5 1 -6 -1 1535.00 408.754 13 1 -6 0 135.476 176.432 13 1 -6 0 157.013 144.205 6 1 -6 0 221.522 214.753 5 1 -6 1 2693.39 467.077 13 1 -6 1 3163.18 521.996 5 -1 6 -1 3345.38 528.892 9 1 -6 1 3456.91 527.373 6 1 -6 2-321.380 201.756 6 -1 6 -2 380.796 203.998 9 1 -6 2-40.8590 144.781 5 1 -6 2 145.122 145.455 13 1 -6 3 221.853 179.489 13 1 -6 3 680.615 254.812 5 -1 6 -3 687.833 283.121 9 1 -6 3 237.119 183.765 8 1 -6 3 604.099 237.154 6 -1 6 -4 20471.4 1373.17 9 1 -6 4 19389.1 1231.72 5 1 -6 4 19742.1 1273.06 6 1 -6 4 20737.8 1294.89 8 1 -6 4 19710.7 1105.20 13 1 -6 5 389.210 224.698 8 1 -6 5 127.995 160.410 6 -1 6 -5 54.2282 231.427 9 1 -6 5 225.587 157.354 5 -1 6 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2421.77 409.542 5 -1 5 0 2299.45 352.344 3 -1 5 0 2585.65 410.613 9 1 -5 0 3007.76 432.498 6 1 -5 1 7110.07 655.949 13 1 -5 1 6902.07 649.908 6 1 -5 1 6809.78 649.470 5 -1 5 -1 6510.69 627.472 9 1 -5 2 2096.17 385.255 6 -1 5 -2 2010.61 395.168 9 1 -5 2 2038.85 356.819 13 1 -5 2 1579.73 354.912 8 1 -5 2 1664.90 339.026 5 1 -5 3 3911.65 507.632 6 1 -5 3 3210.57 469.898 8 1 -5 3 3714.94 491.196 5 -1 5 -3 3723.88 424.208 7 1 -5 3 3433.14 422.598 13 1 -5 4 11479.5 877.181 6 -1 5 -4 10569.4 779.074 7 1 -5 4 10264.0 831.007 8 1 -5 4 10453.8 684.327 13 1 -5 4 9423.62 771.154 5 1 -5 5 6768.05 696.579 6 1 -5 5 5842.66 656.294 8 -1 5 -5 6719.93 690.641 7 1 -5 6 957.310 283.425 6 -1 5 -6 816.386 323.861 7 1 -5 6 1643.95 405.739 8 -1 5 -7 24549.6 1520.44 7 1 -5 7 22283.1 1451.67 8 1 -5 7 22781.8 1329.83 6 1 -5 8-2.31407 152.982 8 -1 5 -8 275.592 256.007 7 -1 5 -9 11210.4 1170.99 9 1 -5 9 12069.2 565.080 26 1 -5 10 31.9707 109.250 26 1 -5 11 623.591 173.738 26 1 -5 12 255.941 134.339 26 1 -5 13 160.880 113.940 26 1 -5 14 386.941 113.716 26 1 -4 -12 426.467 97.6057 23 1 -4 -11 280.446 106.038 23 1 -4 -10 8666.29 475.302 23 1 -4 -9 1143.07 194.673 23 1 -4 -8 9867.27 528.657 23 1 -4 -7 409.762 136.452 18 -1 4 6 428.933 291.623 3 -1 4 5 1475.47 448.780 3 1 -4 -5 1048.89 325.625 13 -1 4 4 9857.09 926.145 3 1 -4 -4 11758.4 926.348 13 1 -4 -3 232.425 201.647 13 1 -4 -3 182.820 129.812 2 -1 4 3 511.703 216.473 3 1 -4 -2 3539.15 410.741 2 1 -4 -2 3947.57 506.496 13 -1 4 2 3987.74 499.469 3 1 -4 -2 4224.63 454.183 5 1 -4 -1 56.9694 95.4954 14 -1 4 1 170.293 147.540 3 1 -4 -1 3.39454 111.445 13 1 -4 -1 204.937 134.705 2 -1 4 1 187.749 145.422 9 1 -4 -1 135.955 128.095 6 1 -4 -1 124.379 147.522 5 1 -4 0 377.298 156.992 5 1 -4 0 486.273 200.772 13 -1 4 0 679.807 209.923 9 1 -4 0 494.147 165.033 14 1 -4 0 806.339 206.682 6 -1 4 0 675.646 179.515 3 -1 4 -1 1819.17 200.609 7 1 -4 1 1884.04 308.693 13 1 -4 1 1338.02 249.296 14 1 -4 1 1242.01 263.908 5 -1 4 -1 1784.07 223.639 3 1 -4 1 1698.67 297.066 6 -1 4 -2 1985.09 187.513 3 1 -4 2 2132.32 323.610 14 -1 4 -2 2080.53 265.271 7 1 -4 2 2191.69 335.834 8 1 -4 2 2002.29 301.974 13 1 -4 2 1710.25 300.746 6 1 -4 2 2167.57 328.606 5 -1 4 -2 1947.00 224.700 12 1 -4 3 72.8058 121.278 5 -1 4 -3 260.625 132.490 12 1 -4 3 327.976 190.733 6 1 -4 3 202.914 167.965 8 -1 4 -3 297.954 173.116 7 1 -4 3 111.215 77.0319 11 1 -4 3 246.762 134.528 13 -1 4 -4 97452.8 2072.17 12 -1 4 -4 99108.2 2238.10 7 1 -4 4 96875.9 2235.02 6 1 -4 4 97668.3 2296.94 8 1 -4 4 89724.8 2090.15 5 -1 4 -5 83875.0 2275.54 7 -1 4 -5 84789.9 2229.38 12 1 -4 5 82810.7 2274.14 8 1 -4 5 79674.9 2085.15 6 -1 4 -6 59286.6 2102.37 7 1 -4 6 60792.2 2111.19 8 1 -4 6 59230.6 1862.14 6 -1 4 -6 61630.0 2132.62 12 -1 4 -7 142884. 3552.42 12 -1 4 -7 139560. 3480.20 7 1 -4 7 137070. 2913.62 6 1 -4 7 143758. 3484.39 8 -1 4 -8 970.594 336.428 7 -1 4 -8 517.079 307.086 12 1 -4 8 1136.85 369.618 8 1 -4 9 1385.81 422.300 8 -1 4 -9 126.817 226.461 7 -1 4 -9 1165.68 407.468 12 1 -4 10 6505.26 426.168 26 1 -4 10 6599.78 410.025 28 1 -4 11 2997.05 292.154 28 1 -4 11 2656.55 292.339 26 1 -4 12 173.297 117.570 26 1 -4 12 222.770 123.287 28 1 -4 13 17.8724 90.9238 26 1 -4 13 21.5038 82.9019 28 1 -4 14-76.6375 92.3666 28 -1 3 12 767.256 126.066 28 1 -3 -12 843.538 146.511 23 1 -3 -11 247.731 106.849 23 -1 3 11 357.678 112.068 28 -1 3 10 2639.60 263.319 28 1 -3 -10 2328.40 268.508 23 -1 3 9-117.362 121.921 28 1 -3 -9 60.2944 85.3746 23 -1 3 8 193.718 105.524 28 1 -3 -8 75.7063 79.1104 23 1 -3 -7 983.643 322.972 11 -1 3 7 1809.16 497.542 3 -1 3 6 1600.31 451.110 3 1 -3 -5 179.942 185.311 13 -1 3 5-46.9569 176.476 3 1 -3 -4 2094.30 321.859 2 1 -3 -4 1614.44 319.328 13 -1 3 4 2111.68 430.502 3 1 -3 -3 214.221 162.222 13 -1 3 3-18.4710 164.094 3 1 -3 -3 117.075 122.498 2 1 -3 -3-73.1538 99.9608 5 1 -3 -2 71879.5 1293.18 14 1 -3 -2 67289.8 1711.15 13 -1 3 2 67774.0 1763.62 3 1 -3 -2 69458.5 1584.71 2 1 -3 -2 66341.8 1458.05 5 1 -3 -1 31102.3 1093.59 13 -1 3 1 33604.6 1077.97 3 1 -3 -1 33817.2 1070.18 2 -1 3 1 30160.6 839.228 9 1 -3 -1 31323.8 996.438 5 1 -3 0 135697. 2058.62 5 1 -3 0 140920. 2117.27 6 1 -3 0 141280. 2148.23 2 -1 3 0 142039. 1896.41 3 -1 3 0 137609. 963.573 7 -1 3 -1 3449.54 253.194 7 1 -3 1 3233.47 249.871 1 -1 3 -2 82399.4 1396.48 12 1 -3 2 86161.7 1255.88 11 1 -3 2 83568.7 1166.49 1 -1 3 -2 83280.1 1492.45 7 1 -3 2 82766.7 1396.19 4 1 -3 3 23203.6 896.105 5 1 -3 3 22697.0 944.049 14 1 -3 3 22421.5 694.318 13 1 -3 3 23317.5 690.217 1 -1 3 -3 22055.3 900.397 7 -1 3 -3 21813.1 851.512 12 1 -3 3 24135.3 942.966 6 1 -3 3 23421.3 881.598 4 1 -3 3 24094.0 962.947 8 1 -3 4 155103. 2644.12 8 -1 3 -4 150827. 2642.57 7 -1 3 -4 150376. 2588.29 12 1 -3 4 151767. 2429.75 6 1 -3 4 149054. 2037.67 1 1 -3 4 147913. 2516.46 4 -1 3 -5 29350.1 1303.25 7 1 -3 5 27314.6 1223.50 8 -1 3 -5 29989.3 1343.26 12 1 -3 5 29520.9 1115.87 6 1 -3 6 201175. 3657.02 8 -1 3 -6 208258. 3788.01 7 -1 3 -6 212951. 3982.12 12 1 -3 6 212903. 3058.78 6 1 -3 6 208076. 3048.25 3 -1 3 -7 1735.33 430.405 12 -1 3 -7 1827.46 405.543 7 -1 3 -8 3906.91 682.705 12 -1 3 -8 4082.51 653.194 7 1 -3 9 2886.58 561.965 8 -1 3 -9 1724.24 447.336 7 1 -3 10 14549.3 609.705 28 1 -3 10 14807.7 625.148 26 1 -3 11 917.632 179.497 28 1 -3 11 738.995 163.065 26 1 -3 12 17740.3 683.598 26 1 -3 12 16579.7 663.722 28 1 -3 13 289.558 122.954 28 1 -3 14 536.159 127.548 28 1 -2 -13 214.499 79.9578 23 -1 2 13 215.703 87.8006 28 1 -2 -12 713.954 144.731 23 -1 2 12 816.840 155.649 28 1 -2 -11 527.797 138.563 23 -1 2 11 322.055 117.373 28 -1 2 10 194.838 112.031 28 1 -2 -10 232.693 105.623 23 1 -2 -9 27.1332 79.4923 23 -1 2 9 104.698 102.177 28 -1 2 8 3659.46 735.728 3 -1 2 7 1785.62 468.367 3 -1 2 6 45986.5 2019.09 3 1 -2 -6 48380.5 1818.69 11 -1 2 5 6183.26 693.391 3 1 -2 -5 5321.52 522.989 2 1 -2 -5 5933.47 530.322 13 -1 2 4 21355.0 1140.94 3 1 -2 -4 23831.8 984.518 13 1 -2 -4 23730.6 1000.58 2 1 -2 -3 15338.5 728.122 2 -1 2 3 14257.9 823.085 3 1 -2 -3 15093.2 523.414 14 1 -2 -3 14776.8 519.958 5 1 -2 -3 14537.0 725.592 13 1 -2 -3 15932.1 513.004 7 1 -2 -2 104.313 89.5775 5 -1 2 2 101.237 150.567 3 1 -2 -2 148.952 52.6747 7 1 -2 -2 92.8422 71.1286 14 1 -2 -2 65.0565 103.657 13 1 -2 -2 134.916 105.006 2 -1 2 1 8230.04 472.451 3 1 -2 -1 8191.47 401.169 14 1 -2 -1 7680.25 399.846 5 1 -2 -1 8462.80 459.615 2 1 -2 0 18213.1 641.918 2 1 -2 0 18334.2 609.982 14 1 -2 0 18921.8 577.225 1 1 -2 0 18872.4 366.482 4 1 -2 1 139211. 1419.11 1 1 -2 1 141018. 1436.26 11 1 -2 1 139868. 1403.70 4 1 -2 1 140392. 1588.40 13 1 -2 1 138060. 1773.47 2 1 -2 2 116072. 1663.75 6 -1 2 -2 111890. 1625.78 12 1 -2 2 112280. 1390.48 1 1 -2 2 113565. 1594.74 4 1 -2 2 115045. 1660.83 8 1 -2 2 114096. 1299.86 13 1 -2 3 697637. 4496.77 14 1 -2 3 707554. 3960.93 3 -1 2 -3 708494. 4879.66 12 -1 2 -4 95267.5 2105.72 12 1 -2 4 96567.7 1743.66 3 1 -2 4 99664.3 2013.14 4 1 -2 5 668.846 210.131 3 1 -2 5 583.818 237.964 4 -1 2 -5 628.222 257.737 12 1 -2 6 73737.6 2019.67 3 -1 2 -6 75771.4 2411.31 12 -1 2 -7 909.510 315.452 7 1 -2 7 1060.47 312.356 3 -1 2 -7 926.962 331.090 12 -1 2 -8 3747.73 672.877 12 -1 2 -8 4572.59 700.650 7 1 -2 8 3590.71 561.056 3 -1 2 -9 254.654 224.623 7 -1 2 -9 519.864 358.362 12 1 -2 10 427.053 134.094 28 1 -2 11 8330.11 480.980 28 1 -2 12 999.635 189.068 28 1 -2 13 210.711 106.221 28 1 -2 14 288.777 96.0069 28 -1 1 13 336.361 107.760 28 1 -1 -13 481.479 112.905 23 -1 1 12 1982.90 240.603 28 1 -1 -12 2330.29 252.602 23 -1 1 11 46.0013 88.3245 28 1 -1 -11 71.5019 80.5262 23 -1 1 10-101.823 95.3073 28 1 -1 -10-90.6747 82.0899 23 1 -1 -9 201.769 109.075 23 -1 1 9-84.8241 96.8687 28 -1 1 8 1094.37 404.724 3 -1 1 7 10289.7 999.925 3 1 -1 -6-508.506 196.379 11 1 -1 -6 63.4280 169.372 2 1 -1 -6 38.4309 181.379 7 -1 1 6-245.143 216.250 3 1 -1 -5 11340.4 694.009 7 1 -1 -5 11471.4 723.354 11 -1 1 5 10869.8 826.844 3 1 -1 -5 11445.5 770.970 2 -1 1 4 16949.7 920.555 3 1 -1 -4 18679.3 883.183 2 1 -1 -4 17874.0 707.448 13 1 -1 -3 40196.5 1143.56 2 1 -1 -3 40176.7 977.893 13 -1 1 3 38911.1 1216.05 3 1 -1 -3 41586.7 956.514 7 1 -1 -2 46926.5 964.231 13 1 -1 -2 48838.8 819.369 7 -1 1 2 48196.6 1119.28 3 1 -1 -2 50092.4 1110.59 2 1 -1 -1 2089.20 203.689 1 1 -1 -1 2203.18 138.754 7 1 -1 -1 2419.43 220.020 2 1 -1 0 69032.2 954.073 1 1 -1 0 70434.6 983.425 2 1 -1 1 392331. 2254.29 2 1 -1 1 390838. 2041.28 8 1 -1 1 388696. 2371.56 1 1 -1 2 166139. 1835.06 3 1 -1 2 164100. 1630.07 14 1 -1 3 816623. 3985.46 14 -1 1 -3 819317. 3809.15 10 1 -1 3 829245. 4960.50 3 -1 1 -4 8177.62 660.581 12 1 -1 4 8406.65 595.772 3 -1 1 -4 8325.23 439.770 10 1 -1 4 8508.84 592.199 4 1 -1 5 57218.4 1710.21 4 -1 1 -5 58001.7 1280.36 10 -1 1 -5 58059.9 1942.89 12 1 -1 5 56100.1 1709.08 3 1 -1 6 12299.4 898.260 4 1 -1 6 12020.6 896.646 3 -1 1 -6 12891.0 1024.96 12 -1 1 -7 6621.81 823.508 12 1 -1 7 6904.09 750.884 3 -1 1 -8 3687.78 683.645 12 1 -1 8 3808.17 631.998 3 -1 1 -8 4123.49 633.983 7 -1 1 -9 10609.0 1055.93 7 1 -1 9 10988.2 1114.21 3 1 -1 9 10755.0 514.283 28 1 -1 10 192.116 111.966 28 1 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3 -1 0 -2 27457.5 868.108 12 1 0 2 28908.5 911.602 3 -1 0 -2 26358.0 800.865 10 1 0 2 26779.4 480.118 14 1 0 2 26679.0 779.877 4 1 0 3 11724.4 700.924 3 -1 0 -3 11701.4 601.212 10 -1 0 -3 13099.0 730.725 12 1 0 3 13141.2 647.034 4 -1 0 -4 2801.67 421.994 12 1 0 4 2785.51 354.961 4 1 0 4 2553.25 385.438 3 -1 0 -4 2080.76 298.092 10 1 0 5 46008.4 1536.30 4 1 0 5 43644.2 1654.78 3 -1 0 -5 44942.0 1739.19 12 -1 0 -5 45636.9 1413.68 10 1 0 6 18148.6 1087.34 4 1 0 6 16913.7 1134.44 3 -1 0 -6 14711.9 1121.26 12 1 0 7 28169.3 1597.46 3 -1 0 -7 28582.8 1684.40 12 1 0 8 395.305 277.559 3 -1 0 -8 67.4528 250.421 12 1 0 9-14.3445 88.4268 28 1 0 10 596.205 151.960 28 -1 0 -10 658.698 149.724 23 -1 0 -11 242.393 114.868 23 1 0 11 79.0647 92.4691 28 1 0 12 131.220 98.8291 28 -1 0 -12 82.0827 73.9223 23 1 0 13 788.999 144.707 28 -1 -1 14 22.7448 76.0107 28 1 1 -14 105.537 82.5017 22 -1 -1 13 1083.82 185.795 28 -1 -1 12 91.9827 109.057 28 -1 -1 11 2724.22 285.465 28 1 1 -10 2445.90 253.814 23 -1 -1 10 2684.69 273.721 28 1 1 -9 1381.02 388.023 7 -1 -1 8 16808.8 1179.17 3 1 1 -8 17161.1 1241.76 7 1 1 -7 6166.29 750.976 12 1 1 -7 5427.18 649.555 7 -1 -1 7 4629.96 575.908 3 -1 -1 6-1.12475 134.293 3 1 1 -6 117.664 160.531 7 1 1 -6-142.870 241.232 12 1 1 -6 397.082 161.722 9 -1 -1 5 26392.1 1035.84 3 1 1 -5 27138.1 1166.08 7 1 1 -5 29715.0 1054.11 9 1 1 -5 28724.0 1257.78 12 1 1 -4 17738.6 868.147 12 -1 -1 4 18587.3 533.373 5 1 1 -4 18087.4 855.621 7 -1 -1 4 18576.8 742.926 3 1 1 -3 153028. 2147.54 12 -1 -1 3 156313. 1689.18 5 -1 -1 3 154414. 1731.76 3 -1 -1 2 89189.7 1334.04 8 1 1 -2 91520.1 1537.09 9 1 1 -1 23613.7 478.630 1 -1 -1 1 23561.8 600.145 8 1 1 0 97935.8 1359.05 7 1 1 0 98920.7 1295.73 3 1 1 1 19403.3 731.523 3 1 1 1 19031.9 592.315 4 -1 -1 -1 20364.7 628.856 12 1 1 1 19700.5 706.955 15 1 1 2 39993.2 1008.61 15 -1 -1 -2 38564.2 1177.76 10 1 1 2 40281.8 1233.33 3 -1 -1 -2 37369.5 623.863 6 1 1 2 40027.7 978.737 4 1 1 3 162.773 105.354 15 1 1 3 53.1011 156.367 3 -1 -1 -3 127.056 46.5536 2 -1 -1 -3 81.8132 133.045 12 -1 -1 -3 126.600 142.355 10 1 1 3 126.118 124.732 4 -1 -1 -4 4348.24 480.028 10 -1 -1 -4 5204.23 448.151 13 -1 -1 -4 5176.13 566.435 12 1 1 4 5132.89 470.695 4 1 1 4 4140.06 533.763 3 1 1 5 5451.57 648.007 3 -1 -1 -5 5197.41 629.677 12 -1 -1 -5 5706.61 582.605 10 1 1 5 5644.61 543.656 4 1 1 6 2083.34 483.907 3 -1 -1 -6 2087.55 452.129 12 -1 -1 -6 1779.19 371.430 10 1 1 7 1999.72 491.592 3 -1 -1 -7 2718.23 564.039 12 -1 -1 -8 2216.81 251.980 18 -1 -1 -8 2396.93 574.301 12 1 1 9 280.990 122.466 28 -1 -1 -10 1.73730 71.8122 23 1 1 10-50.3624 94.5048 28 -1 -1 -11 87.5856 81.1412 23 1 1 11 23.7174 86.1137 28 1 1 12 11.6706 68.8190 28 -1 -1 -12 11.6256 77.2384 23 1 1 13 717.421 127.312 28 -1 -1 -13 489.765 101.352 23 -1 -2 14 211.383 102.809 28 1 2 -14 215.366 109.038 22 -1 -2 13 3305.30 298.907 28 -1 -2 12 1558.31 230.744 28 -1 -2 11 1719.42 235.735 28 -1 -2 10 76.9029 95.8154 28 1 2 -9 350.473 247.613 7 1 2 -8 38373.1 1890.26 7 1 2 -7 1715.30 411.610 7 1 2 -7 1377.54 381.802 12 1 2 -6 6068.07 647.631 7 -1 -2 6 6423.97 572.194 6 1 2 -6 6324.11 615.548 9 1 2 -6 5683.21 633.957 12 1 2 -5 248.235 180.236 7 -1 -2 5 379.263 146.324 3 1 2 -5 392.013 194.147 12 1 2 -5 218.631 162.567 9 1 2 -4 8719.47 642.401 9 -1 -2 4 8254.08 396.585 3 1 2 -4 8313.35 575.744 12 1 2 -4 8005.70 619.126 7 -1 -2 4 8274.60 591.472 8 -1 -2 3 109922. 1006.40 3 1 2 -3 112675. 2120.89 9 1 2 -3 109082. 2002.93 7 -1 -2 3 111719. 1944.22 8 -1 -2 2 13012.1 612.649 8 1 2 -2 13215.0 657.748 7 -1 -2 2 13037.3 579.468 10 1 2 -1 148244. 2006.24 7 1 2 -1 148342. 1286.27 1 -1 -2 1 151178. 2008.78 8 -1 -2 0 10295.7 608.230 10 1 2 0 8778.79 425.763 4 -1 -2 0 9564.45 292.653 12 1 2 0 9684.92 502.770 3 1 2 0 9453.88 495.241 7 -1 -2 -1 1995.63 232.446 6 -1 -2 -1 2434.39 241.461 12 -1 -2 -1 2011.20 321.786 10 1 2 1 2104.59 300.489 3 1 2 1 2093.35 216.382 4 1 2 1 2629.78 339.132 15 1 2 2 37430.6 1148.78 15 -1 -2 -2 36150.2 847.038 6 -1 -2 -2 36355.9 1335.42 10 1 2 2 37350.4 1319.57 3 1 2 2 37186.1 959.738 4 -1 -2 -3 55063.8 1611.90 12 1 2 3 55184.3 1391.72 15 -1 -2 -3 53654.0 1720.70 10 1 2 3 53802.1 1765.51 3 1 2 3 54792.8 1317.90 4 -1 -2 -4 28839.6 1377.16 10 -1 -2 -4 29234.0 1248.21 13 -1 -2 -4 30566.2 1388.91 12 1 2 4 27211.5 1406.33 3 -1 -2 -5 32262.4 1564.91 10 -1 -2 -5 35603.6 1669.58 12 -1 -2 -6 2758.48 551.263 12 1 2 6 2683.22 547.485 3 1 2 7 90.8054 189.495 3 1 2 8-42.0920 91.9821 28 -1 -2 -8-38.3112 96.5050 18 1 2 9 2722.27 278.750 28 1 2 10 2900.82 279.911 28 -1 -2 -10 2486.77 270.474 23 1 2 11 92.8934 91.7519 28 -1 -2 -11 143.413 93.6236 23 -1 -2 -12-22.0761 67.3691 23 1 2 12 42.3938 69.8568 28 1 3 -15 17.5286 58.7416 22 1 3 -14 672.915 141.934 22 -1 -3 13 973.756 180.134 28 -1 -3 12 1568.94 221.438 28 -1 -3 12 2007.07 248.275 26 -1 -3 11 685.332 180.188 26 -1 -3 11 554.696 151.043 28 -1 -3 10 738.626 165.461 28 -1 -3 10 841.567 184.933 26 1 3 -9 2587.70 564.579 7 -1 -3 9 3908.30 663.795 8 1 3 -8 58861.2 2406.56 7 -1 -3 8 52903.8 2203.24 8 -1 -3 7 4167.52 540.449 6 -1 -3 7 4673.77 615.601 8 1 3 -7 4765.01 646.250 9 1 3 -7 5339.44 685.490 7 -1 -3 6 115572. 2670.75 6 1 3 -6 119861. 2906.44 9 -1 -3 6 118298. 2821.98 8 1 3 -6 115735. 2886.60 7 -1 -3 5 1703.79 338.174 6 -1 -3 5 2126.72 366.580 8 -1 -3 5 1983.80 314.491 5 1 3 -5 2162.45 419.529 9 1 3 -5 2275.17 397.179 7 1 3 -4 15030.9 902.164 7 -1 -3 4 15526.1 918.592 6 -1 -3 4 16483.8 864.477 5 1 3 -4 17655.0 1030.30 9 -1 -3 4 16631.4 924.809 8 -1 -3 3 73763.8 1832.83 5 -1 -3 3 75512.5 1808.13 8 1 3 -3 73457.2 1802.55 7 1 3 -3 70991.3 1963.41 9 1 3 -2 44753.2 1316.45 7 -1 -3 2 39928.7 1363.62 6 -1 -3 2 44694.4 1435.18 5 -1 -3 2 45233.5 1281.79 10 -1 -3 2 42959.6 1320.83 8 1 3 -2 43276.8 1528.57 9 1 3 -1 2740.86 320.401 7 -1 -3 1 2422.29 373.695 5 -1 -3 1 2824.78 355.913 6 1 3 -1 2643.87 202.599 1 -1 -3 1 1930.61 317.015 10 1 3 -1 2676.14 248.189 3 1 3 0 35905.1 1070.14 7 -1 -3 0 37121.3 1342.66 10 -1 -3 0 32509.6 1286.95 5 -1 -3 0 34976.6 1169.49 6 1 3 0 35754.3 895.703 4 1 3 0 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2 -5 -11 466.488 108.335 23 2 -5 -10 190.864 95.9898 23 2 -5 -9 922.097 167.362 23 2 -5 -8 3533.17 325.330 23 2 -5 -8 3549.48 324.275 19 2 -5 -7 9734.22 522.361 23 2 -5 -6 100.370 84.6429 23 2 -5 -5 1978.76 446.542 13 2 -5 -5 1870.26 457.882 11 -2 5 5 1085.90 389.139 3 -2 5 4 1237.58 378.357 3 2 -5 -4 1630.19 393.542 13 2 -5 -4 813.913 299.553 11 2 -5 -3 149.414 175.198 13 2 -5 -3 282.882 168.953 2 2 -5 -3 608.165 289.954 11 -2 5 3 332.972 234.451 3 2 -5 -2 22251.1 1287.42 13 -2 5 2 22994.2 1288.62 3 2 -5 -2 23608.7 1242.13 2 2 -5 -1 7070.56 600.268 14 2 -5 -1 6053.01 618.881 2 -2 5 1 6962.56 663.063 3 2 -5 -1 8023.56 692.392 5 2 -5 -1 6847.80 675.192 11 2 -5 -1 7541.94 716.514 13 -2 5 0 760.601 228.305 3 2 -5 0 1080.02 291.846 13 2 -5 0 760.145 247.045 5 2 -5 0 490.859 194.671 14 2 -5 0 1087.05 283.451 2 2 -5 0 997.465 261.685 11 -2 5 0 676.724 211.458 9 2 -5 1 7503.42 669.882 5 2 -5 1 7418.44 608.910 11 -2 5 -1 7881.38 560.390 3 2 -5 1 7430.02 657.976 13 2 -5 1 7569.10 681.821 6 2 -5 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65.4826 23 2 -4 -11 1184.88 182.308 23 2 -4 -10 345.675 127.902 23 2 -4 -9 2941.15 297.934 23 2 -4 -8 2990.70 302.706 23 2 -4 -7 734.754 160.456 23 2 -4 -7 531.854 142.825 19 2 -4 -6 683.596 276.288 11 -2 4 6 656.433 379.481 3 2 -4 -5 291.984 191.932 13 2 -4 -5 162.934 182.387 11 2 -4 -4 27780.3 1343.97 2 -2 4 4 26705.5 1495.42 3 2 -4 -4 27427.9 1406.52 13 2 -4 -4 28385.1 1483.25 11 2 -4 -3 99027.6 2523.37 13 -2 4 3 97078.8 2583.27 3 2 -4 -3 95943.6 2371.86 2 2 -4 -3 98568.9 2577.64 11 -2 4 2 2083.00 376.474 3 2 -4 -2 2900.38 352.415 14 2 -4 -2 2914.53 429.032 11 2 -4 -2 2414.45 374.708 2 2 -4 -2 2970.17 429.849 13 2 -4 -1 837.718 246.517 13 -2 4 1 487.100 197.131 3 2 -4 -1 735.318 214.621 2 2 -4 -1 771.278 226.121 11 2 -4 -1 781.516 212.139 14 2 -4 0 271207. 3592.90 2 2 -4 0 276539. 3385.83 14 2 -4 0 272794. 3559.92 13 2 -4 0 273673. 3432.87 11 -2 4 -1 97673.2 1456.73 7 2 -4 1 98817.7 2088.98 14 2 -4 1 97202.7 1767.47 1 2 -4 1 102110. 1449.95 4 2 -4 1 98766.1 1909.28 11 2 -4 1 94841.1 2121.79 2 2 -4 1 98912.5 2032.92 13 2 -4 2 263.919 174.960 6 2 -4 2 267.611 132.746 11 2 -4 2 512.570 180.323 14 2 -4 2 487.938 186.273 8 2 -4 2 256.245 121.175 1 2 -4 2 302.142 145.507 13 2 -4 3 235305. 3250.47 8 2 -4 3 229120. 3358.49 6 2 -4 3 234471. 2733.90 1 -2 4 -3 231553. 3188.24 12 2 -4 3 226039. 3353.01 14 2 -4 3 231651. 3009.69 4 2 -4 3 236284. 2849.94 13 2 -4 4 1819.95 323.511 4 2 -4 4 2148.38 356.159 8 2 -4 4 2009.96 286.509 1 -2 4 -4 2039.05 347.295 12 2 -4 4 1993.52 363.201 14 2 -4 4 2717.95 385.430 6 -2 4 -5 27785.0 1355.51 12 2 -4 5 28078.9 1304.52 4 2 -4 5 29351.3 1249.65 6 2 -4 5 27797.3 1135.72 1 2 -4 5 29569.3 1354.81 8 2 -4 6 4672.56 598.069 8 -2 4 -6 5718.58 710.360 12 2 -4 6 5210.73 622.795 4 2 -4 6 4651.64 531.546 1 -2 4 -7 5159.52 751.966 12 2 -4 7 5471.02 695.140 8 2 -4 8 9566.54 993.325 8 -2 4 -8 10831.0 1135.51 12 -2 4 -8 9933.30 1029.81 7 2 -4 9 4828.30 769.320 8 2 -4 9 4650.90 360.131 26 2 -4 10 6687.74 414.217 28 2 -4 10 6901.72 442.683 26 2 -4 11 1058.12 200.003 26 2 -4 11 810.769 165.908 28 2 -4 12 700.647 162.409 26 2 -4 12 1007.57 174.401 28 2 -4 13 1191.49 179.540 28 2 -4 13 1122.57 182.619 26 2 -4 14 310.366 99.4724 28 2 -3 -13 1379.87 151.627 23 -2 3 12 56.7080 62.0667 28 2 -3 -12 119.786 86.3772 23 -2 3 11 37.4611 85.6589 28 2 -3 -11 80.9593 91.0807 23 -2 3 10 2380.91 254.502 28 2 -3 -10 1830.05 237.585 23 -2 3 9 883.712 161.752 28 2 -3 -9 965.859 191.588 23 2 -3 -8 7580.56 452.367 23 -2 3 7 3320.50 644.238 3 2 -3 -7 3346.61 586.708 11 -2 3 6 19980.6 1423.58 3 2 -3 -6 21214.0 1334.64 11 2 -3 -5 63.1266 116.833 13 2 -3 -5 225.050 165.947 11 2 -3 -5-149.407 151.401 2 -2 3 5-219.156 214.073 3 2 -3 -4 8245.35 699.475 2 2 -3 -4 8910.53 712.821 13 -2 3 4 9114.49 816.097 3 2 -3 -4 9736.50 784.740 11 -2 3 3 6403.96 632.053 3 2 -3 -3 7815.78 518.677 14 2 -3 -3 7138.45 614.187 13 2 -3 -3 6510.87 603.042 11 2 -3 -3 6835.67 585.713 2 2 -3 -2 75565.1 1812.23 2 2 -3 -2 75766.9 1829.70 13 2 -3 -2 72406.7 1801.22 11 2 -3 -2 77401.3 1610.34 14 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1152.87 191.394 28 2 -2 11 584.624 153.021 28 2 -2 12 17.2743 89.2074 28 2 -2 13-3.35677 78.0078 28 2 -2 14 54.7896 81.2668 28 2 -1 -14 731.758 111.637 23 2 -1 -13 2641.16 238.066 23 -2 1 13 2728.41 250.120 28 2 -1 -12 113.973 90.8776 23 -2 1 12 40.1873 83.6929 28 -2 1 11 1600.89 226.841 28 2 -1 -11 1735.49 233.974 23 2 -1 -10 3579.00 326.965 23 -2 1 10 3767.52 330.657 28 -2 1 9 8988.41 478.943 28 2 -1 -9 8928.25 484.159 23 -2 1 8 10106.8 1055.23 3 2 -1 -8 8013.39 876.134 2 -2 1 7 16286.6 1219.94 3 2 -1 -7 14784.9 1114.79 2 -2 1 6 14173.3 1047.31 3 2 -1 -6 13544.3 866.068 7 2 -1 -6 14562.8 894.140 11 2 -1 -6 12319.9 956.341 2 2 -1 -5 159.469 208.665 2 2 -1 -5 138.515 143.726 11 2 -1 -5 76.3414 132.216 7 -2 1 5-6.53258 173.469 3 2 -1 -4 1111.72 297.291 2 2 -1 -4 956.535 218.927 7 -2 1 4 889.858 262.859 3 2 -1 -4 832.122 205.292 11 2 -1 -3 6729.77 315.712 15 2 -1 -3 6938.68 494.756 11 2 -1 -3 6264.11 547.951 2 2 -1 -2 764662. 3589.28 15 2 -1 -2 762596. 4163.80 7 2 -1 -2 757358. 4781.89 1 2 -1 -2 754611. 5038.03 2 2 -1 -1 77574.6 1244.84 15 2 -1 -1 78380.4 1431.67 1 2 -1 -1 81769.5 1296.19 7 2 -1 -1 80284.1 1448.27 2 2 -1 0 54953.1 1065.42 2 2 -1 0 53012.4 1142.19 1 2 -1 1 295443. 1653.60 8 2 -1 1 287111. 2612.46 14 2 -1 1 290276. 2265.40 2 2 -1 1 293482. 2824.49 1 2 -1 2 3959.61 316.464 14 2 -1 2 4473.85 400.151 1 -2 1 -3 19205.3 920.044 12 2 -1 3 17458.6 652.038 14 2 -1 3 17523.4 857.836 3 2 -1 3 18205.9 843.289 4 2 -1 4 8625.37 460.028 14 2 -1 4 8145.41 662.092 3 2 -1 4 8027.26 640.536 4 -2 1 -4 8820.35 714.235 12 -2 1 -4 8992.17 598.772 10 -2 1 -5 2474.66 464.726 12 2 -1 5 2283.89 406.352 3 -2 1 -5 2201.39 327.471 10 2 -1 5 2019.96 374.515 4 2 -1 6 10761.6 883.163 4 -2 1 -6 11035.7 1007.35 12 2 -1 6 9580.08 856.214 3 -2 1 -7 3367.23 632.425 12 2 -1 7 4036.33 631.081 3 2 -1 7 2893.53 513.014 4 2 -1 8 1571.78 445.097 3 -2 1 -8 832.898 389.406 12 2 -1 9 1156.30 186.191 28 2 -1 10 74.9023 96.5463 28 2 -1 11 327.232 126.900 28 2 -1 12 174.371 108.748 28 2 -1 13 57.9698 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12 2 0 3 14188.0 845.641 3 -2 0 -3 14509.6 809.141 10 -2 0 -4 107.016 179.101 12 2 0 4 130.808 193.620 3 -2 0 -4-12.9208 140.155 10 2 0 4 171.516 151.019 4 -2 0 -5 22126.0 1122.66 10 -2 0 -5 22060.0 1313.16 12 2 0 5 22809.8 1180.00 4 2 0 5 22099.6 1276.23 3 2 0 6 9006.40 826.470 4 2 0 6 8114.25 857.330 3 -2 0 -6 9060.00 940.733 12 2 0 7 6618.59 842.406 3 -2 0 -7 6539.88 875.898 12 2 0 7 5555.59 708.783 4 2 0 8 5233.06 372.133 28 -2 0 -8 4511.58 811.660 12 -2 0 -8 5001.86 358.625 18 2 0 9 5166.76 383.447 28 2 0 10 1431.49 216.511 28 -2 0 -10 1515.71 208.595 23 2 0 11 100.775 98.5709 28 -2 0 -11-11.6563 69.9518 23 2 0 12 14.1489 75.5921 28 -2 0 -12 191.675 93.5361 23 2 0 13 46.4563 68.2014 28 2 1 -14 3053.06 238.907 22 -2 -1 13 45.6568 92.4061 28 2 1 -13 81.9065 93.9140 22 -2 -1 12 1050.28 190.444 28 2 1 -12 1352.83 194.060 23 2 1 -11-21.1822 86.0563 23 -2 -1 11-203.569 114.508 28 2 1 -10 56.1267 87.8912 23 -2 -1 10 24.1391 109.818 28 2 1 -9-483.809 270.678 7 2 1 -8 329.149 237.534 7 2 1 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327.180 3 3 -6 0 1004.97 312.282 13 3 -6 0 1286.44 337.981 2 3 -6 0 1158.69 344.418 11 3 -6 1 3416.09 518.935 14 3 -6 1 3804.57 535.588 13 3 -6 1 4017.61 527.666 11 3 -6 2 37558.7 1677.28 14 3 -6 2 36831.0 1597.59 13 3 -6 3 4500.88 602.829 14 3 -6 3 3834.17 534.178 8 -3 6 -4 26855.3 1379.67 12 3 -6 4 23792.1 1410.33 14 3 -6 4 27064.4 1417.71 8 -3 6 -5 3343.40 532.350 12 3 -6 5 2875.59 502.040 8 -3 6 -5 2525.08 457.750 7 -3 6 -6 1136.08 330.068 7 -3 6 -6 1443.61 413.369 12 3 -6 6 1485.70 372.162 8 -3 6 -7 28.8115 150.546 7 3 -6 7-180.451 206.834 8 -3 6 -7-480.670 305.611 12 3 -6 8 677.502 171.274 26 3 -6 9 5478.46 393.515 26 3 -6 10 3515.79 333.799 26 3 -6 11 81.3392 122.226 26 3 -6 12 757.247 173.863 26 3 -6 13 198.297 103.445 26 3 -6 14 1213.30 154.856 26 3 -5 -11-63.1154 77.7625 23 3 -5 -10 1297.74 190.588 23 3 -5 -9-88.6053 92.8792 23 3 -5 -8 9.48001 89.2297 23 3 -5 -8-85.8476 101.165 19 3 -5 -7 959.850 175.621 23 3 -5 -7 1180.44 202.604 19 3 -5 -6 5533.29 390.422 19 3 -5 -6 5926.48 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4 8142.75 762.435 14 -3 5 -4 9200.95 795.614 12 3 -5 4 8977.36 683.857 1 3 -5 4 9015.47 740.196 4 3 -5 4 9509.48 768.020 8 3 -5 5-8.10670 143.822 14 -3 5 -5 327.138 228.831 12 3 -5 5 50.3611 126.449 8 3 -5 5 115.862 133.936 4 -3 5 -6 1466.32 404.899 12 3 -5 6 1072.95 305.141 8 3 -5 6 1407.43 380.863 4 -3 5 -7-452.430 257.944 7 -3 5 -7-69.3060 212.345 12 3 -5 8-301.147 254.918 8 -3 5 -8 686.008 331.499 7 -3 5 -8 562.804 325.966 12 3 -5 9 543.970 152.401 26 3 -5 10 1311.17 217.757 26 3 -5 11 639.730 166.299 26 3 -5 12 173.327 113.025 26 3 -5 13 1324.69 185.913 26 3 -5 14 634.116 118.559 26 3 -4 -12 731.565 129.987 23 3 -4 -11 64.5889 94.6467 23 3 -4 -10 53.0901 92.9226 23 3 -4 -9 13.0110 88.8260 23 3 -4 -8 102.091 107.135 23 3 -4 -8-16.6494 104.367 19 3 -4 -7 1363.53 202.194 23 3 -4 -7 1284.27 197.526 19 -3 4 6 871.155 322.799 3 3 -4 -6 1956.68 456.461 11 3 -4 -5 5632.99 693.002 2 -3 4 5 6595.64 826.788 3 3 -4 -5 7106.24 806.360 11 3 -4 -4 9852.01 871.873 2 -3 4 4 9908.48 924.660 3 3 -4 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1 3 -4 5 8346.87 725.780 8 3 -4 6 3370.82 509.406 1 3 -4 6 3869.04 549.320 8 -3 4 -6 2195.67 489.590 12 3 -4 6 2465.79 471.316 4 -3 4 -7 18176.2 1423.06 12 3 -4 7 18559.5 1338.85 4 3 -4 7 18159.9 1271.22 1 3 -4 7 18040.6 1265.99 8 3 -4 8 573.683 274.363 8 -3 4 -8 929.524 379.381 12 3 -4 9 1028.85 198.241 26 3 -4 9 1217.69 208.081 21 3 -4 10 20967.2 721.551 28 3 -4 10 19440.5 746.101 26 3 -4 11 1865.62 237.450 28 3 -4 11 1641.02 240.274 26 3 -4 12 175.769 106.070 28 3 -4 12 121.796 101.265 26 3 -4 13 30.9458 86.3598 26 3 -4 13-26.9228 81.1917 28 3 -4 14 512.904 101.247 28 3 -3 -13 251.980 83.5385 23 3 -3 -12 1059.36 163.943 23 -3 3 11 1077.08 173.153 28 3 -3 -11 1074.55 183.647 23 -3 3 10 5712.36 385.672 28 3 -3 -10 5440.01 405.395 23 3 -3 -9 4095.93 352.382 23 3 -3 -8 1057.06 187.487 23 3 -3 -7 1034.67 327.589 2 -3 3 7 1016.95 389.426 3 -3 3 6 6889.23 858.709 3 3 -3 -6 7037.21 796.882 11 3 -3 -6 6175.39 747.977 2 3 -3 -5-312.924 190.903 2 -3 3 5 294.151 267.799 3 3 -3 -5-58.3366 155.091 11 -3 3 4 59310.4 2082.26 3 3 -3 -4 59831.3 1725.75 14 3 -3 -4 59051.1 1968.26 11 3 -3 -4 54980.2 1942.88 2 -3 3 3 84330.2 2259.83 3 3 -3 -3 84260.9 2002.57 14 3 -3 -3 83458.6 2203.95 11 3 -3 -3 82135.3 2228.33 2 3 -3 -2 86842.8 1973.80 14 3 -3 -2 83081.4 2050.74 11 3 -3 -2 85813.4 2078.27 1 3 -3 -2 81505.4 2077.63 2 3 -3 -1 26984.9 1139.85 2 3 -3 -1 28651.3 1121.08 14 3 -3 -1 27946.7 1126.99 1 3 -3 0 16588.4 844.910 1 3 -3 0 17715.4 883.196 14 3 -3 0 16149.5 858.431 2 3 -3 0 17229.4 741.351 4 3 -3 1 3377.42 393.951 2 3 -3 1 3558.08 399.264 1 3 -3 1 3905.93 430.574 14 3 -3 1 3374.68 361.196 4 3 -3 2 47431.5 1439.42 1 3 -3 2 48679.0 1421.70 2 3 -3 2 48888.9 1492.59 14 3 -3 2 50919.8 1448.90 4 3 -3 3 2301.22 359.896 14 -3 3 -3 2510.63 377.576 12 3 -3 3 3057.53 403.892 4 3 -3 3 3166.02 409.902 1 3 -3 3 2964.00 330.305 8 3 -3 4 6847.72 594.700 14 -3 3 -4 5983.98 639.491 12 3 -3 4 6237.94 628.176 4 3 -3 4 5563.15 576.062 1 3 -3 4 6648.41 551.524 8 3 -3 5 43591.7 1562.18 8 3 -3 5 42221.6 1495.87 14 -3 3 -5 40992.0 1784.35 12 3 -3 5 44102.2 1742.95 4 3 -3 5 43605.6 1708.95 1 3 -3 6 4961.85 594.289 8 3 -3 6 3874.67 562.840 1 -3 3 -6 3389.97 605.411 12 3 -3 6 3079.38 512.347 4 3 -3 7 433.015 221.657 8 -3 3 -7-134.470 234.366 12 3 -3 7 206.446 171.611 4 3 -3 7-150.660 182.584 1 3 -3 8-178.465 171.717 1 3 -3 8 1127.67 372.475 8 -3 3 -8 461.411 335.592 12 3 -3 8 770.199 318.637 4 3 -3 9 3380.49 306.457 26 3 -3 9 2606.45 275.156 28 3 -3 9 2811.50 290.970 21 3 -3 10 79.6705 104.454 28 3 -3 10-17.2456 93.4320 26 3 -3 11 656.324 163.415 26 3 -3 11 604.195 151.934 28 3 -3 12 547.319 142.778 28 3 -3 12 471.291 131.343 26 3 -3 13 107.455 87.3029 28 3 -2 -13 1146.12 157.388 23 -3 2 12 1161.17 179.375 28 3 -2 -12 1623.49 211.002 23 -3 2 11-73.9793 98.1758 28 3 -2 -11 8.80947 82.2390 23 -3 2 10-62.3982 85.3558 28 3 -2 -10 50.0902 90.5994 23 3 -2 -9 467.512 133.782 23 -3 2 9 325.372 119.765 28 3 -2 -8 990.311 344.135 2 -3 2 8 1358.30 450.223 3 3 -2 -7-35.0741 141.765 2 -3 2 7 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4945.83 685.447 2 -4 6 1 6501.90 733.135 3 4 -6 -1 6206.45 715.238 14 4 -6 0 21442.4 1382.15 2 4 -6 0 22976.6 1347.62 14 4 -6 1 184.625 203.986 14 4 -6 1 63.2492 150.432 2 4 -6 1-8.72364 128.701 1 4 -6 2 104512. 2917.61 14 4 -6 2 108720. 2671.45 1 4 -6 3 22038.9 1385.25 14 -4 6 -3 23674.7 1363.14 12 4 -6 4 20368.2 1351.54 14 -4 6 -4 20672.6 1339.36 12 4 -6 4 23380.2 1295.65 4 4 -6 4 21995.4 1275.36 8 4 -6 5 8247.54 899.739 14 -4 6 -5 7716.84 872.441 12 4 -6 5 9093.85 885.493 4 4 -6 5 9646.90 881.911 8 -4 6 -6-261.310 216.939 12 4 -6 6 118.564 160.533 4 -4 6 -7 6112.89 809.658 7 -4 6 -7 5972.09 901.798 12 4 -6 8 78.4420 102.471 26 4 -6 9 2638.15 292.652 26 4 -6 10 2856.76 304.067 26 4 -6 11 1870.19 246.648 26 4 -6 12 334.189 128.618 26 4 -6 13 258.066 105.936 26 4 -5 -11-68.3718 80.8018 23 4 -5 -10 93.4404 98.2050 23 4 -5 -9 3823.58 331.059 23 4 -5 -9 3632.44 315.817 19 4 -5 -8 4809.80 373.645 23 4 -5 -8 4690.02 378.180 19 4 -5 -7 2697.49 288.028 23 4 -5 -7 2073.16 256.970 19 4 -5 -6 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270.502 14 4 -3 2 948.749 234.004 2 4 -3 2 892.437 263.425 1 4 -3 3 0.66450 156.607 4 4 -3 3 255.097 162.541 14 4 -3 3-79.6664 203.649 1 -4 3 -3 50.1689 150.417 12 4 -3 4 16.8579 140.434 4 4 -3 4 171.037 142.525 14 4 -3 4-78.7676 151.063 1 -4 3 -4 114.864 190.653 12 4 -3 5 1280.00 343.504 1 -4 3 -5 1016.27 361.852 12 4 -3 5 797.548 291.808 4 -4 3 -6 2347.90 543.388 12 4 -3 6 1893.33 452.753 1 4 -3 6 1112.56 367.377 4 4 -3 7-219.069 228.976 1 -4 3 -7-26.2059 295.189 12 4 -3 7-327.644 230.592 4 4 -3 8 11686.9 536.279 28 4 -3 8 12456.4 589.125 21 4 -3 9 1999.47 240.540 28 4 -3 9 1508.56 231.084 21 4 -3 10 9.04999 91.3684 28 4 -3 10-159.986 126.340 26 4 -3 11-11.9882 91.8787 28 4 -3 11 129.781 107.534 26 4 -3 12 933.520 151.554 26 4 -3 12 961.665 167.355 28 4 -3 13 156.266 85.7198 28 4 -2 -13 214.803 96.0811 23 4 -2 -12 20.8924 76.1564 23 4 -2 -11 889.602 176.618 23 -4 2 10 319.488 125.900 28 4 -2 -10 253.133 119.874 23 -4 2 9 1284.38 195.587 28 4 -2 -9 1356.73 210.852 23 4 -2 -8 2443.29 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243.716 12 4 -2 5 316.361 205.161 4 4 -2 6-54.1048 226.382 1 -4 2 -6 102.059 217.633 12 4 -2 6 57.5883 160.010 4 4 -2 7 854.606 330.015 1 -4 2 -7 479.010 317.587 12 4 -2 7 127.918 210.558 4 4 -2 8 164.018 98.3414 28 4 -2 8 499.117 165.422 21 4 -2 9 2424.85 271.095 28 4 -2 9 2375.82 281.898 21 4 -2 10 2527.56 263.690 26 4 -2 10 2234.23 266.320 28 4 -2 11 1836.34 223.252 28 4 -2 12 68.1138 93.0015 28 4 -1 -13 1950.79 205.543 23 4 -1 -12 2100.46 237.071 23 4 -1 -11 1704.52 229.410 23 4 -1 -11 1897.95 232.042 22 4 -1 -10 167.992 104.370 23 4 -1 -10 141.800 112.416 22 -4 1 9 1634.49 225.298 28 4 -1 -9 1729.93 244.147 23 4 -1 -9 1245.18 200.642 22 4 -1 -8-718.792 337.691 2 -4 1 8 1205.22 402.126 3 4 -1 -7 281.898 277.902 2 -4 1 7 496.710 292.531 3 4 -1 -6 598.968 274.803 7 4 -1 -6 927.621 338.905 2 -4 1 6 510.145 290.105 3 4 -1 -5 15047.3 983.822 7 -4 1 5 16177.1 1094.13 3 4 -1 -5 14114.3 1097.12 2 4 -1 -4 92682.4 2065.95 15 4 -1 -4 86885.4 2231.70 7 4 -1 -4 90021.2 2564.79 2 4 -1 -3 7588.99 648.853 7 4 -1 -3 7986.60 633.634 15 4 -1 -3 7540.62 657.324 1 4 -1 -3 8429.00 740.037 2 4 -1 -2 20341.9 1020.54 7 4 -1 -2 19698.3 1003.87 15 4 -1 -2 20435.7 1043.86 1 4 -1 -2 21078.1 1053.70 2 4 -1 -1 1239.84 282.377 1 4 -1 -1 1332.70 298.556 15 4 -1 -1 1068.74 242.021 2 4 -1 -1 1162.96 286.132 4 4 -1 0 18355.1 994.513 1 4 -1 0 17486.3 994.530 15 4 -1 0 17637.4 973.598 4 4 -1 0 18745.3 845.538 2 4 -1 1 3032.94 313.615 2 4 -1 1 2663.11 416.862 4 4 -1 1 2487.08 412.718 15 4 -1 1 2501.62 360.180 14 4 -1 1 2737.42 420.274 1 4 -1 2 1558.87 334.256 4 4 -1 2 1722.62 375.869 1 4 -1 2 1104.20 246.373 14 -4 1 -2 1348.62 337.700 12 -4 1 -3 21201.2 1242.89 12 4 -1 3 19630.1 1152.96 4 4 -1 3 19730.1 1206.79 1 -4 1 -4 35967.0 1750.19 12 4 -1 4 36936.9 1677.56 4 -4 1 -4 33975.7 1630.61 10 4 -1 4 35605.4 1736.57 1 -4 1 -5 1696.59 446.041 12 4 -1 5 2440.35 489.338 1 -4 1 -5 1580.06 393.663 10 4 -1 5 1961.64 430.652 4 -4 1 -6 8880.11 1044.53 12 4 -1 6 9158.43 959.143 4 4 -1 6 9742.51 1029.61 1 4 -1 7 5847.60 396.182 28 -4 1 -7 6657.15 410.059 18 4 -1 8 24.6119 95.0333 28 4 -1 8-51.7551 106.677 21 4 -1 9 480.419 159.751 28 4 -1 10 1729.51 227.681 28 4 -1 11 2092.91 229.819 28 4 -1 12 421.859 112.113 28 4 0 -14 632.128 111.377 23 4 0 -13 109.972 82.5505 23 4 0 -13-126.551 98.9201 22 4 0 -12 3532.52 308.691 23 4 0 -12 3264.98 290.694 22 4 0 -11 1074.23 189.213 23 4 0 -11 1394.19 219.666 22 4 0 -10 332.194 112.606 23 4 0 -10 317.641 131.081 22 4 0 -9 200.768 101.512 23 4 0 -9 202.588 114.777 22 4 0 -8 958.638 363.804 2 4 0 -8 712.158 241.205 7 4 0 -7 12423.0 1070.32 7 4 0 -7 11783.1 1146.94 2 4 0 -6 7716.92 792.709 7 -4 0 6 10297.8 893.641 3 4 0 -6 9449.00 980.838 2 4 0 -5 12390.2 949.134 7 4 0 -5 12391.1 880.831 15 4 0 -5 12434.5 1042.43 2 4 0 -4 10959.0 844.677 7 4 0 -4 10581.9 824.838 15 4 0 -4 10410.7 900.043 2 4 0 -4 11311.5 803.021 1 4 0 -3 138090. 2902.34 15 4 0 -3 141481. 2928.63 7 4 0 -3 141483. 2725.63 1 4 0 -3 146784. 3028.76 2 4 0 -2 7098.51 656.094 7 4 0 -2 5859.14 615.521 15 4 0 -2 7084.30 611.987 1 4 0 -2 6234.08 575.943 2 4 0 -1 2150.80 315.093 2 4 0 -1 2242.65 379.735 4 4 0 -1 2558.11 400.160 7 4 0 -1 1687.11 341.827 15 4 0 -1 2866.65 396.360 1 4 0 0 7780.27 665.853 1 4 0 0 7240.07 694.516 15 4 0 0 8029.32 694.071 4 4 0 1-179.052 159.303 4 4 0 1 15.3939 147.179 15 4 0 1 147.195 161.704 1 -4 0 -1 389.602 188.849 12 4 0 2 1941.49 375.782 4 4 0 2 2266.67 423.003 1 4 0 2 1593.93 363.409 15 -4 0 -2 2419.09 425.928 12 -4 0 -3 9864.54 869.743 12 -4 0 -3 8938.65 882.548 10 4 0 3 9928.82 856.528 4 4 0 3 9161.39 870.886 1 -4 0 -4 11690.4 1031.87 12 4 0 4 8977.12 868.079 4 4 0 4 9874.68 981.254 1 -4 0 -4 11167.6 1004.82 10 4 0 5 599.418 289.634 1 -4 0 -5 1107.49 449.988 12 -4 0 -5 1042.71 373.452 10 4 0 5 1056.15 331.833 4 4 0 6 562.749 140.224 28 -4 0 -6 1116.47 417.880 12 4 0 7 6683.93 427.722 21 4 0 7 6604.88 431.874 28 -4 0 -7 5895.66 395.369 18 4 0 8 7644.43 466.172 28 -4 0 -8 7569.01 457.209 18 4 0 9 102.550 103.862 28 4 0 10 72.5433 85.7233 28 4 0 11 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549.396 17 5 -8 2 11993.1 552.173 27 5 -8 2 12066.5 560.612 25 5 -8 2 10634.0 538.211 24 5 -8 3 680.897 156.141 27 5 -8 3 559.572 130.884 24 5 -8 3 640.018 162.491 17 5 -8 4 6242.61 417.929 27 5 -8 4 6324.68 409.379 24 5 -8 5 1421.77 218.453 27 5 -8 5 2109.62 259.757 24 5 -8 6 3047.76 309.586 27 5 -8 7 1362.26 224.029 27 5 -8 7 1076.50 182.271 26 5 -8 8 1372.94 213.833 27 5 -8 8 1690.07 227.360 26 5 -8 9 648.071 166.693 27 5 -8 9 547.439 142.422 26 5 -8 10 435.360 137.665 26 5 -8 11 168.539 107.562 26 5 -8 12 80.2790 89.2701 26 5 -7 -9 513.336 104.596 23 5 -7 -9 711.614 135.985 19 5 -7 -8-48.0403 71.3967 23 5 -7 -8 29.3977 88.0139 19 5 -7 -7 20.0835 84.7395 19 5 -7 -6 5799.63 424.877 19 5 -7 -5 2487.61 295.275 19 5 -7 -4 1687.61 233.470 17 5 -7 -4 2013.31 258.121 19 5 -7 -3 19275.4 724.336 17 5 -7 -3 18455.7 716.519 25 5 -7 -3 20571.7 764.304 19 5 -7 -2 5939.88 398.745 17 5 -7 -2 5654.39 401.435 25 5 -7 -2 6011.50 403.625 19 5 -7 -1 5130.25 747.906 14 -5 7 1 5821.59 803.550 3 5 -7 -1 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2167.09 450.447 1 -5 -1 -1 787.468 347.344 10 5 1 2 349.671 251.449 15 5 1 2 945.129 330.225 1 -5 -1 -2 586.172 317.546 10 5 1 3 3112.35 587.237 1 -5 -1 -3 3106.89 627.955 10 -5 -1 -4 1268.05 190.776 18 5 1 4 1478.42 212.980 28 5 1 5 9491.91 515.439 28 -5 -1 -5 8734.23 480.606 18 5 1 6 972.340 192.652 28 -5 -1 -6 971.085 181.110 18 5 1 7 431.090 142.020 28 -5 -1 -7 520.939 146.558 18 5 1 8 1053.43 183.797 28 5 1 9 335.680 113.311 28 5 1 10-14.8705 58.3339 28 -5 -1 -10 4.82798 52.0823 23 5 2 -13 327.518 101.684 22 5 2 -12 525.170 136.619 22 -5 -2 11 182.894 102.628 26 5 2 -11 243.074 104.344 23 5 2 -11 168.544 117.902 22 -5 -2 10 245.962 134.751 26 5 2 -10 188.510 114.328 23 5 2 -10 303.499 129.705 22 -5 -2 9 2257.81 267.120 26 5 2 -9 2279.16 256.120 23 5 2 -9 2340.57 267.921 22 -5 -2 8 896.002 179.570 26 5 2 -8 687.640 154.076 23 5 2 -8 883.349 171.476 22 -5 -2 7 193.225 115.356 26 5 2 -7 32.6801 82.6504 23 5 2 -7 245.202 106.995 22 5 2 -6 1036.57 407.790 2 5 2 -6 999.673 406.194 15 5 2 -5 2265.54 526.058 7 5 2 -5 2383.73 548.337 15 5 2 -4 237.662 241.665 7 5 2 -4 33.8453 195.372 15 5 2 -3 7018.74 842.578 7 5 2 -3 6085.84 821.232 15 5 2 -3 5363.31 725.077 4 5 2 -2 2770.61 517.947 4 5 2 -2 2237.23 502.501 15 -5 -2 2 2947.92 603.768 10 5 2 -1 5145.51 765.382 15 -5 -2 1 6359.07 859.916 10 5 2 -1 6123.52 757.865 4 5 2 0 10038.7 1055.55 15 -5 -2 0 7717.26 941.785 10 5 2 1 2552.20 549.891 15 -5 -2 -1 1516.46 468.585 10 -5 -2 -2 44.6323 84.3147 18 5 2 2 32.7355 92.9195 28 5 2 3 5716.78 396.036 28 -5 -2 -3 5042.61 366.665 18 -5 -2 -4 1693.46 223.892 18 5 2 4 1737.77 240.191 28 5 2 5 681.467 172.203 28 -5 -2 -5 589.620 153.180 18 5 2 6 1486.33 214.721 28 -5 -2 -6 1330.55 200.421 18 5 2 7 669.643 145.222 28 -5 -2 -7 921.420 169.504 18 5 2 8 457.736 120.000 28 5 2 9 490.424 103.840 28 5 3 -13-9.13833 68.3546 22 -5 -3 12-6.70564 89.0195 26 5 3 -12 173.123 96.3551 22 -5 -3 11 460.617 150.881 26 5 3 -11 308.888 127.239 22 -5 -3 10 2574.84 279.010 26 5 3 -10 2564.45 279.735 22 -5 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668.005 283.847 4 6 -2 2 526.437 263.273 1 6 -2 3 671.579 289.345 4 -6 2 -3 910.669 348.687 12 6 -2 3 756.252 330.645 1 -6 2 -4 1906.01 530.506 12 -6 2 -4 1864.54 491.965 10 6 -2 5 6616.52 423.442 28 6 -2 5 5933.40 417.183 21 6 -2 6 173.530 118.120 28 6 -2 6 188.175 129.969 21 6 -2 7 1641.09 235.748 28 6 -2 7 1630.09 239.328 21 6 -2 8 203.731 105.358 28 6 -2 8 85.5189 112.840 21 6 -2 9 501.506 126.090 28 6 -2 10 475.347 122.832 28 6 -2 11 318.010 89.6795 28 6 -1 -13 201.284 80.0303 23 6 -1 -12 303.842 111.193 23 6 -1 -12 191.376 84.4028 22 6 -1 -11 450.443 128.826 23 6 -1 -11 469.645 124.245 22 6 -1 -10 2076.00 252.444 23 6 -1 -10 2007.73 238.172 22 6 -1 -9 1745.53 234.570 23 6 -1 -9 1692.20 231.900 22 6 -1 -8 93.5860 91.9062 23 6 -1 -8 85.5677 112.154 22 6 -1 -7 8791.11 500.555 23 6 -1 -7 9872.60 511.541 22 6 -1 -7 8974.36 503.826 19 6 -1 -6 131.029 80.0580 23 6 -1 -6 223.576 96.2732 22 6 -1 -6 388.235 117.369 19 6 -1 -5 1107.27 394.296 7 6 -1 -5 1059.10 348.569 2 6 -1 -4 6546.90 788.027 7 6 -1 -4 7047.33 807.987 1 6 -1 -4 7337.20 853.811 4 6 -1 -4 7986.25 883.987 2 6 -1 -3 11460.2 1021.79 15 6 -1 -3 9447.96 919.707 1 6 -1 -3 10660.7 1008.57 4 6 -1 -3 11080.1 1000.57 2 6 -1 -2 8633.95 907.727 15 6 -1 -2 7761.00 853.654 1 6 -1 -2 7815.82 853.296 4 6 -1 -1 5591.04 739.151 15 6 -1 -1 5565.63 716.140 1 6 -1 -1 5593.46 725.862 4 6 -1 0 12072.6 1080.68 1 6 -1 0 12137.6 1055.65 14 6 -1 0 12838.7 1099.73 4 6 -1 1 3371.92 585.954 4 -6 1 -1 4581.15 662.403 12 6 -1 1 3835.40 635.335 1 6 -1 2 9322.05 1009.57 1 6 -1 2 10983.9 1055.68 4 6 -1 3 1817.91 445.314 4 6 -1 3 1913.02 497.440 1 -6 1 -3 1954.46 514.828 10 6 -1 4 6778.23 426.002 28 6 -1 4 6737.96 431.710 21 6 -1 5 951.144 187.000 28 6 -1 5 949.222 181.817 21 6 -1 6 553.470 169.081 28 6 -1 6 738.263 173.985 21 6 -1 7 66.9494 91.3709 28 6 -1 7 60.2621 103.570 21 6 -1 8 114.030 104.118 28 6 -1 9 318.949 119.413 28 6 -1 10 300.497 97.8633 28 6 0 -13 474.495 102.503 23 6 0 -13 564.960 109.146 22 6 0 -12 999.212 156.268 23 6 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376.588 123.783 23 8 -3 -8 201.277 109.289 23 8 -3 -8 283.880 109.469 22 8 -3 -7 49.7879 87.5889 23 8 -3 -7-38.2118 86.3844 22 8 -3 -6 8352.18 480.020 23 8 -3 -6 8374.77 468.115 22 8 -3 -5 3486.47 315.581 23 8 -3 -4 2068.32 251.386 23 8 -3 -3 33.6905 92.3306 23 8 -3 -3 123.691 107.470 21 8 -3 -2 441.976 147.078 21 8 -3 -1 2.69539 91.8506 21 8 -3 0 127.183 109.996 21 8 -3 1 293.048 114.244 21 8 -3 2 4886.62 364.297 28 8 -3 2 5270.90 400.965 21 8 -3 3 1485.94 212.531 28 8 -3 3 1515.74 229.811 21 8 -3 4 903.861 172.606 28 8 -3 4 1375.77 220.730 21 8 -3 5 1203.04 188.588 28 8 -3 5 754.937 179.241 21 8 -3 6 204.756 107.688 28 8 -3 6 169.318 114.326 21 8 -3 7 1556.92 197.110 28 8 -3 7 1327.54 198.952 21 8 -3 8 180.991 86.1197 28 8 -3 8 283.079 106.457 21 8 -2 -11 148.864 67.1589 28 8 -2 -11 275.292 89.9929 23 8 -2 -10 512.124 113.850 28 8 -2 -10 399.575 120.492 23 8 -2 -10 435.560 106.088 22 8 -2 -9 56.2178 90.9668 23 8 -2 -9 31.1444 74.6702 22 8 -2 -8 1215.07 196.285 23 8 -2 -8 1211.83 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300.852 113.232 21 8 -1 6 230.833 106.328 28 8 -1 6 177.321 91.8401 21 8 -1 7 49.1785 70.8621 28 8 0 -11 175.655 84.8992 28 8 0 -11 75.0195 71.2128 22 8 0 -10 243.652 103.806 28 8 0 -10 166.442 82.0489 23 8 0 -10 89.4133 78.9146 22 8 0 -9-28.0639 82.5597 28 8 0 -9 111.975 97.3776 23 8 0 -9 26.2989 88.8252 22 8 0 -8 3246.64 287.257 28 8 0 -8 3232.65 298.523 23 8 0 -8 3017.02 286.972 22 8 0 -7 739.449 163.299 28 8 0 -7 672.783 151.469 22 8 0 -6 130.788 109.904 28 8 0 -6 92.9316 89.8318 22 8 0 -5 2783.65 276.400 28 8 0 -4 17843.2 679.407 28 8 0 -3 5212.78 377.623 28 8 0 -2 38.9573 90.8780 28 8 0 -1 757.044 166.894 28 8 0 0 210.922 119.896 28 8 0 1 3602.68 327.434 28 8 0 2 390.300 142.761 28 8 0 3 614.099 155.217 28 8 0 4 912.855 168.139 28 8 0 5 388.289 120.060 28 8 0 6 77.0093 71.9495 28 8 1 -11 1760.81 168.278 28 8 1 -10 100.227 75.2095 28 8 1 -10 28.7730 74.2091 22 8 1 -9 39.3109 87.8309 28 8 1 -9 12.5616 77.0781 22 8 1 -8 42.5918 88.7928 28 8 1 -8-25.7043 90.5822 22 8 1 -7 303.053 113.019 28 8 1 -7 199.056 112.897 22 8 1 -6 638.958 152.689 28 8 1 -5 24.1914 85.8468 28 8 1 -4 460.246 135.745 28 8 1 -3 3535.16 314.984 28 8 1 -2 244.442 115.736 28 8 1 -1 3394.32 311.485 28 8 1 0 883.878 169.039 28 8 1 1-5.93785 89.6269 28 8 1 2 1708.24 219.010 28 8 1 3 969.006 170.013 28 8 1 4 701.715 137.650 28 8 1 5 507.648 116.065 28 8 2 -10 134.708 85.5475 28 8 2 -9 266.922 102.939 28 8 2 -8 1046.38 164.212 28 8 2 -7 479.422 127.348 28 8 2 -6 64.0609 87.7940 28 8 2 -5 542.820 137.050 28 8 2 -4 48.8685 83.5511 28 8 2 -3 34.1190 93.4372 28 8 2 -2 298.636 113.768 28 8 2 -1 43.7058 82.0763 28 8 2 0 1365.30 194.940 28 8 2 1 105.522 92.5366 28 8 2 2 119.045 85.7346 28 8 2 3 113.038 81.7828 28 8 2 4 48.8842 57.9530 28 8 3 -9 22.7120 73.4479 28 8 3 -8 262.590 99.9202 28 8 3 -7 26.1016 79.3099 28 8 3 -6 16.5177 77.8021 28 8 3 -5 531.826 134.179 28 8 3 -4 1047.19 167.076 28 8 3 -3 181.100 98.1123 28 8 3 -2-12.8766 79.6908 28 8 3 -1 643.598 135.388 28 8 3 0 696.922 132.690 28 8 3 1 10.5647 61.3806 28 8 3 2 215.673 78.4487 28 8 4 -7 547.276 103.177 28 8 4 -6 133.121 73.6002 28 8 4 -5 58.9058 65.3219 28 8 4 -4 958.894 141.379 28 8 4 -3 87.5974 74.7770 28 8 4 -2 3.50541 63.3016 28 8 4 -1 412.869 95.2094 28 9 -11 0 1747.98 177.914 24 9 -11 1 56.7940 71.6512 27 9 -11 1 55.0214 75.5068 24 9 -11 2 1606.81 181.111 27 9 -11 3 228.266 101.043 27 9 -11 3 15.9442 87.2554 20 9 -11 4 1182.00 160.273 27 9 -11 4 895.723 133.741 20 9 -11 5 1342.28 156.685 27 9 -11 5 1430.10 157.899 20 9 -10 -3 136.455 78.6416 24 9 -10 -2 210.422 88.9547 24 9 -10 -1 341.648 105.041 27 9 -10 -1 199.359 92.8440 24 9 -10 0 633.200 137.214 27 9 -10 0 509.255 130.259 24 9 -10 1 244.258 110.229 27 9 -10 1 279.705 106.229 24 9 -10 2 242.761 107.098 27 9 -10 2 298.735 112.699 24 9 -10 3 541.336 132.284 27 9 -10 4 1041.07 163.661 27 9 -10 5 15.0598 79.6941 27 9 -10 6 396.441 106.200 27 9 -9 -5 21.0155 59.5192 24 9 -9 -5 143.886 74.3112 19 9 -9 -4 110.053 74.4591 24 9 -9 -4 156.391 86.0874 19 9 -9 -3 656.492 129.416 24 9 -9 -3 538.232 119.758 19 9 -9 -2 1088.75 160.583 27 9 -9 -2 995.663 162.527 24 9 -9 -1 76.7622 94.6420 27 9 -9 -1 205.858 103.790 24 9 -9 0 58.9580 89.9077 24 9 -9 1-127.937 136.461 27 9 -9 1 49.1920 90.1791 24 9 -9 2-134.997 132.232 27 9 -9 2 30.6692 101.679 24 9 -9 3 284.302 120.400 27 9 -9 4 406.317 135.124 27 9 -9 5 1650.73 202.403 27 9 -9 6 27.6163 75.3530 27 9 -9 7 197.870 85.7008 27 9 -8 -6 64.7628 68.4731 19 9 -8 -5 6.59752 62.1147 24 9 -8 -5 111.408 92.5805 21 9 -8 -5 70.2638 77.8803 19 9 -8 -4 187.317 79.0831 24 9 -8 -4 131.566 84.6990 21 9 -8 -4 279.206 109.049 19 9 -8 -3-7.90379 82.4307 24 9 -8 -3 19.9457 85.4293 21 9 -8 -3 95.2102 90.1201 19 9 -8 -2 691.257 155.598 24 9 -8 -2 791.652 153.986 21 9 -8 -1 511.846 134.507 24 9 -8 -1 509.435 134.446 21 9 -8 0 1032.76 179.992 24 9 -8 0 1234.34 188.595 21 9 -8 1 48.2036 86.6123 24 9 -8 1 76.9931 98.6946 21 9 -8 2 1474.41 222.628 24 9 -8 2 1213.72 185.573 21 9 -8 3 1848.31 227.137 21 9 -8 4 30.2646 100.512 27 9 -8 4 241.983 114.322 21 9 -8 5 5244.44 349.521 27 9 -8 5 6070.19 366.166 21 9 -8 6 2148.58 211.176 27 9 -8 6 2889.08 248.085 21 9 -8 7 469.419 113.949 26 9 -8 7 428.821 114.649 21 9 -8 8 3466.43 220.827 26 9 -8 8 3134.01 209.729 21 9 -7 -7 11.1445 67.9106 21 9 -7 -6 29.4155 80.8677 21 9 -7 -6 163.685 97.0524 19 9 -7 -5 193.407 100.119 21 9 -7 -5 42.2895 89.9594 19 9 -7 -4 130.801 87.8023 21 9 -7 -4 282.633 114.322 19 9 -7 -3 284.212 117.862 21 9 -7 -3 49.0282 93.3139 19 9 -7 -2 73.6111 83.6443 24 9 -7 -2 130.381 104.344 21 9 -7 -1 826.869 164.018 24 9 -7 -1 756.834 158.291 21 9 -7 0 218.336 109.902 24 9 -7 0 125.482 112.971 21 9 -7 1 85.0599 91.0347 24 9 -7 1 20.3078 98.1194 21 9 -7 2 4687.72 374.649 21 9 -7 3 158.723 119.528 21 9 -7 4 657.979 170.983 21 9 -7 5 970.875 172.439 27 9 -7 5 983.185 181.218 21 9 -7 6 366.885 133.122 21 9 -7 7 81.9826 78.7847 26 9 -7 7-18.5003 85.3132 21 9 -7 8 1166.86 150.694 26 9 -7 8 1430.09 169.199 21 9 -6 -8 1150.61 151.912 21 9 -6 -7 23.1864 77.0730 21 9 -6 -6 1624.94 204.305 21 9 -6 -5 1147.55 185.581 21 9 -6 -5 978.779 179.923 19 9 -6 -4 219.382 123.912 21 9 -6 -3 48.6185 88.7448 21 9 -6 -2-84.7640 101.365 21 9 -6 -1 2092.21 256.757 21 9 -6 0 2418.46 272.396 21 9 -6 1 470.833 150.604 21 9 -6 2 3330.05 319.183 21 9 -6 3 2059.03 260.389 21 9 -6 4 129.222 127.187 21 9 -6 5 69.7061 98.7870 21 9 -6 6 2132.68 242.344 21 9 -6 7 1135.09 176.441 21 9 -6 8 81.7263 72.2592 26 9 -6 8 6.27136 78.5353 21 9 -5 -9 184.341 66.3891 23 9 -5 -9 215.932 89.1730 21 9 -5 -8 1902.04 187.539 23 9 -5 -7 4921.66 316.214 23 9 -5 -6 3240.41 270.273 23 9 -5 -6 3265.16 297.884 21 9 -5 -5 22.1806 67.9822 23 9 -5 -5 56.1997 98.5074 21 9 -5 -4 1409.91 212.938 21 9 -5 -3 2351.45 268.820 21 9 -5 -2 297.809 129.566 21 9 -5 -1 900.450 183.515 21 9 -5 0 1199.54 205.323 21 9 -5 1-11.1114 100.860 21 9 -5 2 45.8219 115.366 21 9 -5 3 638.692 156.697 21 9 -5 4 3118.78 309.169 21 9 -5 5 1130.70 199.267 21 9 -5 6 0.24604 92.7263 21 9 -5 7 113.854 98.5519 21 9 -5 8 39.5138 70.0984 26 9 -5 8 85.0227 84.4366 21 9 -4 -9 166.480 75.8480 23 9 -4 -8 1523.58 185.849 23 9 -4 -7 252.613 103.015 23 9 -4 -6 509.196 134.991 23 9 -4 -6 448.363 138.216 21 9 -4 -5 167.442 97.1256 23 9 -4 -5 175.726 115.299 21 9 -4 -4 270.806 123.724 21 9 -4 -3 845.956 182.874 21 9 -4 -2 69.5067 96.9310 21 9 -4 -1 336.019 130.190 21 9 -4 0 236.371 119.191 21 9 -4 1 230.263 117.918 21 9 -4 2 1209.21 208.229 21 9 -4 3-69.3175 110.758 21 9 -4 4 1244.79 203.147 21 9 -4 5 1106.21 187.600 21 9 -4 6 647.885 144.953 21 9 -4 7 122.220 90.3890 21 9 -3 -9 280.818 94.9605 23 9 -3 -9 594.288 129.707 21 9 -3 -8-206.584 94.4803 23 9 -3 -7 2819.00 264.249 23 9 -3 -7 2636.43 261.681 21 9 -3 -6 422.078 126.174 23 9 -3 -6 416.105 132.016 21 9 -3 -5 470.305 147.642 21 9 -3 -4 76.0316 98.2647 21 9 -3 -3 119.736 91.1077 21 9 -3 -2 121.896 101.794 21 9 -3 -1 2958.81 301.172 21 9 -3 0 1983.39 232.962 28 9 -3 0 1878.66 245.309 21 9 -3 1 2077.99 234.516 28 9 -3 1 1873.74 245.347 21 9 -3 2 4021.51 321.965 28 9 -3 2 3957.57 337.503 21 9 -3 3 458.249 131.316 28 9 -3 3 474.369 144.042 21 9 -3 4 1150.58 176.695 28 9 -3 4 1427.28 203.294 21 9 -3 5 768.304 137.550 28 9 -3 5 743.575 160.618 21 9 -3 6 319.715 99.6535 28 9 -3 6 208.420 101.331 21 9 -3 7 141.228 63.9799 28 9 -3 7 390.466 100.133 21 9 -2 -9 554.022 107.346 28 9 -2 -9 717.801 126.511 21 9 -2 -8 455.040 112.456 28 9 -2 -8 395.102 118.079 23 9 -2 -8 380.643 110.587 21 9 -2 -7 1462.45 184.597 28 9 -2 -7 1633.00 205.771 21 9 -2 -6 830.410 155.063 28 9 -2 -6 948.484 166.292 21 9 -2 -5 1069.37 175.162 28 9 -2 -5 1024.17 174.612 21 9 -2 -4 316.337 117.586 28 9 -2 -4 261.154 109.122 21 9 -2 -3 1799.25 223.220 28 9 -2 -3 1893.99 228.557 21 9 -2 -2 861.964 158.051 28 9 -2 -2 900.907 163.613 21 9 -2 -1 3750.30 315.878 28 9 -2 -1 4011.17 334.888 21 9 -2 0 55.8452 88.9898 28 9 -2 0 199.714 109.042 21 9 -2 1 2708.90 278.666 28 9 -2 1 2920.13 287.816 21 9 -2 2 3253.41 289.621 28 9 -2 2 3759.01 315.550 21 9 -2 3 4162.42 317.390 28 9 -2 3 3454.68 299.288 21 9 -2 4 464.141 125.570 28 9 -2 4 526.289 135.836 21 9 -2 5 110.012 90.9167 28 9 -2 5 91.1445 76.9805 21 9 -2 6 72.9804 66.0098 28 9 -2 6-62.8471 69.2132 21 9 -1 -9 101.278 84.7141 28 9 -1 -8 2.17904 72.3674 28 9 -1 -8 0.19738 69.4877 21 9 -1 -7 9.00581 71.8799 28 9 -1 -7-37.1703 89.0177 21 9 -1 -6-97.8826 88.3211 28 9 -1 -6-34.4229 86.7898 21 9 -1 -5-56.4860 98.8493 28 9 -1 -5 174.942 94.3363 21 9 -1 -4 185.915 92.0239 28 9 -1 -4 283.747 109.580 21 9 -1 -3 278.906 107.836 28 9 -1 -2 26.5170 86.7414 28 9 -1 -1 2215.98 248.817 28 9 -1 0 1606.01 221.144 28 9 -1 1 748.974 158.234 28 9 -1 2 12.6010 84.3180 28 9 -1 3 93.7548 92.9883 28 9 -1 4 623.523 134.194 28 9 -1 5 291.694 100.771 28 9 0 -9 302.488 94.3199 28 9 0 -8 207.991 92.4318 28 9 0 -7 488.087 121.643 28 9 0 -6 2296.75 234.955 28 9 0 -5 686.304 144.929 28 9 0 -4 49.6027 83.5978 28 9 0 -3 58.1402 91.4380 28 9 0 -2 112.458 93.6719 28 9 0 -1 165.449 107.480 28 9 0 0 64.2291 93.2976 28 9 0 1 21.9505 81.2482 28 9 0 2 202.108 101.371 28 9 0 3 277.564 100.277 28 9 0 4 42.1928 70.7958 28 9 1 -8-46.1386 72.2598 28 9 1 -7 876.956 142.432 28 9 1 -6 616.933 136.827 28 9 1 -5 23.4249 87.8202 28 9 1 -4-43.8753 79.3036 28 9 1 -3 12.6572 75.6137 28 9 1 -2 409.251 121.973 28 9 1 -1 115.047 82.9808 28 9 1 0 275.135 103.640 28 9 1 1 129.988 91.8330 28 9 1 2 109.929 75.9656 28 9 2 -7 216.644 84.4371 28 9 2 -6 381.764 106.261 28 9 2 -5 122.833 82.1410 28 9 2 -4 61.5090 74.0989 28 9 2 -3-46.8957 86.5877 28 9 2 -2 113.173 89.8546 28 9 2 -1 321.519 97.6123 28 9 2 0-34.9107 66.0778 28 10 -10 0 270.092 89.1389 27 10 -10 1 1009.17 140.499 27 10 -10 2 1269.84 158.889 27 10 -10 3 1069.11 143.074 27 10 -9 -3 659.659 105.615 24 10 -9 -2 161.581 89.6523 27 10 -9 -2 157.032 78.8427 24 10 -9 -1 107.803 87.1487 27 10 -9 -1 294.718 106.526 24 10 -9 0-79.9464 113.793 27 10 -9 1-58.6230 88.3362 27 10 -9 2 61.5700 91.6247 27 10 -9 3-60.4335 82.3699 27 10 -9 4-120.960 91.2897 27 10 -9 5 1467.13 156.611 27 10 -8 -4 76.0297 73.3080 21 10 -8 -3 1297.88 163.121 21 10 -8 -2 56.6084 78.4335 21 10 -8 -1 422.548 117.895 24 10 -8 -1 244.839 102.724 21 10 -8 0 601.060 124.119 21 10 -8 1 768.186 150.392 21 10 -8 2 188.846 106.171 21 10 -8 3-157.101 118.863 27 10 -8 3-66.6453 91.1527 21 10 -8 4 1442.25 177.138 27 10 -8 4 1457.99 175.395 21 10 -8 5 616.519 108.432 27 10 -8 5 821.708 130.836 21 10 -8 6 183.912 86.1613 21 10 -7 -6 292.042 89.3662 21 10 -7 -5 920.620 142.000 21 10 -7 -4 202.740 100.483 21 10 -7 -3 73.7246 79.7667 21 10 -7 -2 603.796 141.962 21 10 -7 -1-70.2315 103.298 21 10 -7 0 41.1517 104.962 21 10 -7 1 30.3411 93.8161 21 10 -7 2 234.815 120.814 21 10 -7 3 352.889 128.675 21 10 -7 4 3489.81 259.274 27 10 -7 4 3431.07 278.840 21 10 -7 5 217.624 102.910 21 10 -7 6 233.282 80.9338 26 10 -7 6 168.456 86.3208 21 10 -6 -6 216.726 93.6370 21 10 -6 -5 950.558 162.876 21 10 -6 -4-12.2633 80.9092 21 10 -6 -3 722.606 152.904 21 10 -6 -2 97.3731 107.547 21 10 -6 -1-70.7134 101.093 21 10 -6 0 1148.83 192.756 21 10 -6 1 632.063 148.244 21 10 -6 2 145.355 114.636 21 10 -6 3 540.666 144.247 21 10 -6 4-43.6707 101.776 21 10 -6 5 581.413 135.864 21 10 -6 6 511.675 117.187 21 10 -5 -7 1314.50 162.200 21 10 -5 -6 2639.12 238.205 21 10 -5 -5 161.941 93.6361 21 10 -5 -4 130.439 96.3150 21 10 -5 -3 1140.11 187.188 21 10 -5 -2-22.6870 87.1579 21 10 -5 -1 954.631 176.164 21 10 -5 0 208.413 116.018 21 10 -5 1 148.313 110.915 21 10 -5 2 184.642 119.097 21 10 -5 3 391.745 135.968 21 10 -5 4 1539.54 195.109 21 10 -5 5 1199.16 166.462 21 10 -4 -7 869.930 136.762 21 10 -4 -6 53.5206 89.5995 21 10 -4 -5 204.512 108.765 21 10 -4 -4 752.100 158.704 21 10 -4 -3 121.011 99.8760 21 10 -4 -2 194.566 116.686 21 10 -4 -1-120.036 115.775 21 10 -4 0 45.2960 88.2419 21 10 -4 1-46.1605 89.0251 21 10 -4 2-71.3262 93.8283 21 10 -4 3 118.266 87.9309 21 10 -4 4 103.423 90.8498 21 10 -4 5 150.186 90.9164 21 10 -3 -8 823.644 124.003 21 10 -3 -7 25.5771 71.9896 21 10 -3 -6 547.127 126.083 21 10 -3 -5 16.3355 81.3031 21 10 -3 -4 167.491 95.5295 21 10 -3 -3 339.181 116.726 21 10 -3 -2-0.49298 98.6545 21 10 -3 -1-3.94479 97.6772 21 10 -3 0 5.81441 92.1307 21 10 -3 1 356.098 128.593 21 10 -3 2 1499.90 191.277 21 10 -3 3 1136.10 161.461 21 10 -3 4 88.4883 75.6036 21 10 -2 -7-123.559 80.0957 28 10 -2 -7-13.6708 57.5286 21 10 -2 -6 9.45649 66.8881 28 10 -2 -6 79.7500 88.0561 21 10 -2 -5-32.9795 72.4480 28 10 -2 -5 104.633 74.9201 21 10 -2 -4 199.918 90.0657 28 10 -2 -4 137.984 85.8463 21 10 -2 -3 60.0106 76.3436 28 10 -2 -3-27.8805 83.3799 21 10 -2 -2 424.878 119.901 28 10 -2 -2 250.588 88.2161 21 10 -2 -1 123.168 95.7526 28 10 -2 -1 62.2846 90.2910 21 10 -2 0 2324.05 224.181 28 10 -2 0 2441.68 226.649 21 10 -2 1 3027.05 243.362 28 10 -2 1 3179.93 250.022 21 10 -2 2 1234.10 157.533 28 10 -2 2 1375.29 160.146 21 10 -2 3 18.3015 67.1120 28 10 -1 -7-44.3958 67.3098 28 10 -1 -6 74.5054 75.6302 28 10 -1 -5 573.163 121.349 28 10 -1 -4 316.869 97.3346 28 10 -1 -3 132.662 89.2071 28 10 -1 -2 37.8239 72.8718 28 10 -1 -1 361.430 110.848 28 10 -1 0 245.773 98.2959 28 10 -1 1 395.856 108.190 28 10 -1 2 885.964 127.539 28 10 0 -6 1152.05 141.855 28 10 0 -5 10.5189 72.3155 28 10 0 -4 149.490 84.2923 28 10 0 -3 695.996 129.613 28 10 0 -2 1266.54 160.832 28 10 0 -1-3.93137 68.5748 28 10 0 0-79.4130 72.6891 28 11 -8 0 520.307 106.352 21 11 -8 1-181.055 85.8384 27 11 -8 1 14.6060 69.4408 21 11 -7 -3 37.0804 69.7151 21 11 -7 -2 166.986 86.2919 21 11 -7 -1 6.84248 73.0687 21 11 -7 0-78.0722 92.1482 21 11 -7 1 72.7452 77.1385 21 11 -7 2 536.706 104.046 27 11 -7 2 466.729 111.322 21 11 -6 -4 406.678 104.895 21 11 -6 -3 353.065 102.417 21 11 -6 -2 29.7709 88.7656 21 11 -6 -1 475.684 119.038 21 11 -6 0 477.653 114.166 21 11 -6 1-68.1645 86.6048 21 11 -6 2 258.699 100.406 21 11 -5 -4-28.2571 79.0247 21 11 -5 -3 50.5885 73.8862 21 11 -5 -2 1359.35 169.835 21 11 -5 -1 873.157 147.533 21 11 -5 0 89.0742 84.0394 21 11 -5 1 158.102 88.6223 21 11 -5 2 317.793 101.307 21 11 -4 -4 224.408 87.2474 21 11 -4 -3-94.4801 78.1004 21 11 -4 -2-11.1313 69.8970 21 11 -4 -1 304.015 95.6166 21 11 -4 0 195.742 98.1495 21 11 -4 1 4.69824 68.1941 21 11 -3 -4 47.8534 65.4015 21 11 -3 -3 691.316 115.717 21 11 -3 -2-72.5780 76.2560 21 11 -3 -1 508.074 103.659 21 11 -3 0 762.432 114.624 21 0 0 0 0.00 0.00 0 TITL zzy119 in P-1 REM P-1 (#2 in standard setting) CELL 1.54184 9.521550 10.782304 12.633213 106.1775 93.8002 114.6144 ZERR 3.00 0.000264 0.000403 0.000527 0.0035 0.0028 0.0031 LATT 1 SFAC C H N O UNIT 42.00 45.00 6.00 12.00 TREF HKLF 4 END ; _shelx_hkl_checksum 63701 _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; _oxdiff_exptl_absorpt_empirical_full_max 1.244 _oxdiff_exptl_absorpt_empirical_full_min 0.883 ####################################################################### # # This file contains crystal structure data downloaded from the # Cambridge Structural Database (CSD) hosted by the Cambridge # Crystallographic Data Centre (CCDC). # # Full information about CCDC data access policies and citation # guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 # # Audit and citation data items may have been added by the CCDC. # Please retain this information to preserve the provenance of # this file and to allow appropriate attribution of the data. # ####################################################################### data_b _database_code_depnum_ccdc_archive 'CCDC 2071226' loop_ _audit_author_name _audit_author_address 'Qilin Wang' ;Henan University China ; _audit_update_record ; 2021-03-18 deposited with the CCDC. 2021-11-08 downloaded from the CCDC. ; _audit_creation_date 2019-09-12 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _shelx_SHELXL_version_number 2014/7 _chemical_name_common ? _chemical_name_systematic ? _chemical_formula_moiety 'C26 H24 N2 O5' _chemical_formula_sum 'C26 H24 N2 O5' _chemical_formula_weight 444.47 _chemical_melting_point ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _space_group_crystal_system orthorhombic _space_group_IT_number 60 _space_group_name_H-M_alt 'P b c n' _space_group_name_Hall '-P 2n 2ab' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y, z-1/2' _cell_length_a 15.5191(7) _cell_length_b 9.0804(5) _cell_length_c 30.9354(13) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 4359.4(4) _cell_formula_units_Z 8 _cell_measurement_reflns_used 2609 _cell_measurement_temperature 150(2) _cell_measurement_theta_max 24.47 _cell_measurement_theta_min 2.60 _shelx_estimated_absorpt_T_max 0.992 _shelx_estimated_absorpt_T_min 0.980 _exptl_absorpt_coefficient_mu 0.095 _exptl_absorpt_correction_T_max 0.7457 _exptl_absorpt_correction_T_min 0.6472 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1065 before and 0.0774 after correction. The Ratio of minimum to maximum transmission is 0.8679. The \l/2 correction factor is Not present.' _exptl_absorpt_special_details ? _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.354 _exptl_crystal_density_meas . _exptl_crystal_density_method ? _exptl_crystal_description prism _exptl_crystal_F_000 1872 _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.08 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0999 _diffrn_reflns_av_unetI/netI 0.0820 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_l_max 38 _diffrn_reflns_limit_l_min -37 _diffrn_reflns_number 24240 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 26.370 _diffrn_reflns_theta_min 2.599 _diffrn_ambient_temperature 149.99 _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source ? _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 2370 _reflns_number_total 4463 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement 'SAINT V8.38A (?, 2016)' _computing_data_collection ? _computing_data_reduction 'SAINT V8.38A (?, 2016)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'ShelXS (Sheldrick, 2008)' _refine_diff_density_max 0.206 _refine_diff_density_min -0.249 _refine_diff_density_rms 0.055 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 301 _refine_ls_number_reflns 4463 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1353 _refine_ls_R_factor_gt 0.0556 _refine_ls_restrained_S_all 1.037 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0442P)^2^+0.8235P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1024 _refine_ls_wR_factor_ref 0.1364 _refine_special_details ? _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All C(H,H,H) groups, All O(H) groups 2.a Ternary CH refined with riding coordinates: C8(H8), C9(H9), C19(H19) 2.b Secondary CH2 refined with riding coordinates: C16(H16A,H16B) 2.c Aromatic/amide H refined with riding coordinates: C1(H1), C2(H2), C3(H3), C4(H4), C5(H5), C11(H11), C12(H12), C13(H13), C14(H14), C17(H17), C20(H20), C21(H21) 2.d Idealised Me refined as rotating group: C22(H22A,H22B,H22C), C26(H26A,H26B,H26C) 2.e Idealised tetrahedral OH refined as rotating group: O4(H4A) ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary ? loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.63221(18) 0.3613(3) 0.28830(8) 0.0341(7) Uani 1 1 d . . . . . H1 H 0.6113 0.4231 0.3107 0.041 Uiso 1 1 calc R . . . . C2 C 0.62019(19) 0.4009(3) 0.24526(8) 0.0410(8) Uani 1 1 d . . . . . H2 H 0.5895 0.4883 0.2384 0.049 Uiso 1 1 calc R . . . . C3 C 0.6527(2) 0.3138(4) 0.21264(9) 0.0524(9) Uani 1 1 d . . . . . H3 H 0.6451 0.3421 0.1833 0.063 Uiso 1 1 calc R . . . . C4 C 0.6962(2) 0.1852(4) 0.22257(9) 0.0526(9) Uani 1 1 d . . . . . H4 H 0.7190 0.1256 0.2001 0.063 Uiso 1 1 calc R . . . . C5 C 0.70638(19) 0.1436(3) 0.26525(8) 0.0419(8) Uani 1 1 d . . . . . H5 H 0.7352 0.0542 0.2720 0.050 Uiso 1 1 calc R . . . . C6 C 0.67473(17) 0.2315(3) 0.29845(8) 0.0298(7) Uani 1 1 d . . . . . C7 C 0.68904(17) 0.1800(3) 0.34394(8) 0.0281(6) Uani 1 1 d . . . . . C8 C 0.65595(17) 0.2720(3) 0.38109(7) 0.0256(6) Uani 1 1 d . . . . . H8 H 0.6712 0.3774 0.3757 0.031 Uiso 1 1 calc R . . . . C9 C 0.69513(17) 0.2239(3) 0.42464(7) 0.0279(6) Uani 1 1 d . . . . . H9 H 0.6810 0.1180 0.4299 0.033 Uiso 1 1 calc R . . . . C10 C 0.79033(18) 0.2488(3) 0.43327(8) 0.0299(7) Uani 1 1 d . . . . . C11 C 0.86188(18) 0.1978(3) 0.41086(9) 0.0348(7) Uani 1 1 d . . . . . H11 H 0.8550 0.1444 0.3847 0.042 Uiso 1 1 calc R . . . . C12 C 0.9438(2) 0.2259(3) 0.42723(9) 0.0395(7) Uani 1 1 d . . . . . H12 H 0.9930 0.1914 0.4121 0.047 Uiso 1 1 calc R . . . . C13 C 0.9542(2) 0.3033(3) 0.46520(9) 0.0406(8) Uani 1 1 d . . . . . H13 H 1.0106 0.3221 0.4758 0.049 Uiso 1 1 calc R . . . . C14 C 0.88388(19) 0.3535(3) 0.48782(9) 0.0403(8) Uani 1 1 d . . . . . H14 H 0.8913 0.4071 0.5139 0.048 Uiso 1 1 calc R . . . . C15 C 0.80192(18) 0.3250(3) 0.47197(8) 0.0334(7) Uani 1 1 d . . . . . C16 C 0.71770(18) 0.3636(3) 0.49239(8) 0.0402(8) Uani 1 1 d . . . . . H16A H 0.7093 0.3101 0.5199 0.048 Uiso 1 1 calc R . . . . H16B H 0.7131 0.4708 0.4977 0.048 Uiso 1 1 calc R . . . . C17 C 0.57545(17) 0.3642(3) 0.45670(8) 0.0305(7) Uani 1 1 d . . . . . H17 H 0.5534 0.4228 0.4796 0.037 Uiso 1 1 calc R . . . . C18 C 0.52387(17) 0.3338(3) 0.42243(8) 0.0276(6) Uani 1 1 d . . . . . C19 C 0.55526(17) 0.2569(3) 0.38244(7) 0.0266(6) Uani 1 1 d . . . . . H19 H 0.5316 0.3111 0.3569 0.032 Uiso 1 1 calc R . . . . C20 C 0.52480(17) 0.1003(3) 0.37951(8) 0.0301(7) Uani 1 1 d . . . . . H20 H 0.5357 0.0376 0.4035 0.036 Uiso 1 1 calc R . . . . C21 C 0.48399(17) 0.0435(3) 0.34608(8) 0.0337(7) Uani 1 1 d . . . . . H21 H 0.4750 0.1049 0.3216 0.040 Uiso 1 1 calc R . . . . C22 C 0.3225(2) -0.0471(4) 0.39146(10) 0.0543(9) Uani 1 1 d . . . . . H22A H 0.3304 -0.0674 0.4223 0.082 Uiso 1 1 calc GR . . . . H22B H 0.2620 -0.0620 0.3837 0.082 Uiso 1 1 calc GR . . . . H22C H 0.3390 0.0550 0.3854 0.082 Uiso 1 1 calc GR . . . . C23 C 0.3777(2) -0.1488(4) 0.36564(9) 0.0424(8) Uani 1 1 d . . . . . C24 C 0.45120(19) -0.1096(3) 0.34407(8) 0.0356(7) Uani 1 1 d . . . . . C25 C 0.4988(2) -0.2195(4) 0.32036(9) 0.0460(8) Uani 1 1 d . . . . . C26 C 0.5780(2) -0.1756(4) 0.29600(10) 0.0576(10) Uani 1 1 d . . . . . H26A H 0.5985 -0.2594 0.2789 0.086 Uiso 1 1 calc GR . . . . H26B H 0.6229 -0.1456 0.3164 0.086 Uiso 1 1 calc GR . . . . H26C H 0.5644 -0.0933 0.2767 0.086 Uiso 1 1 calc GR . . . . N1 N 0.65565(14) 0.3147(2) 0.45927(6) 0.0307(6) Uani 1 1 d . . . . . N2 N 0.43876(15) 0.3860(3) 0.42295(7) 0.0337(6) Uani 1 1 d . . . . . O1 O 0.72464(12) 0.0623(2) 0.35086(5) 0.0391(5) Uani 1 1 d . . . . . O2 O 0.41049(12) 0.4551(2) 0.45497(6) 0.0420(5) Uani 1 1 d . . . . . O3 O 0.39207(12) 0.3586(2) 0.39125(6) 0.0459(6) Uani 1 1 d . . . . . O4 O 0.34920(15) -0.2875(2) 0.36647(7) 0.0592(7) Uani 1 1 d . . . . . H4A H 0.3821 -0.3410 0.3517 0.089 Uiso 1 1 calc GR . . . . O5 O 0.47664(15) -0.3530(2) 0.32043(7) 0.0619(7) Uani 1 1 d . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0321(17) 0.0406(19) 0.0295(14) 0.0039(13) -0.0010(12) -0.0046(14) C2 0.0380(19) 0.047(2) 0.0378(16) 0.0128(14) -0.0112(14) -0.0093(15) C3 0.053(2) 0.076(3) 0.0284(16) 0.0063(16) -0.0078(15) -0.019(2) C4 0.052(2) 0.076(3) 0.0298(16) -0.0064(16) 0.0030(15) 0.002(2) C5 0.0341(18) 0.058(2) 0.0341(15) -0.0049(14) 0.0025(14) 0.0054(16) C6 0.0252(16) 0.0374(18) 0.0267(13) 0.0002(12) -0.0009(12) -0.0001(13) C7 0.0266(15) 0.0278(17) 0.0298(14) -0.0027(12) 0.0024(12) 0.0019(13) C8 0.0296(16) 0.0221(15) 0.0252(13) 0.0022(11) 0.0017(12) 0.0004(12) C9 0.0295(16) 0.0274(16) 0.0266(13) -0.0012(11) 0.0001(12) 0.0029(13) C10 0.0341(17) 0.0268(17) 0.0288(13) 0.0046(12) -0.0036(13) 0.0022(13) C11 0.0388(19) 0.0276(17) 0.0380(15) 0.0034(12) -0.0017(14) 0.0045(14) C12 0.0334(18) 0.041(2) 0.0442(17) 0.0112(14) 0.0008(15) 0.0068(15) C13 0.0331(18) 0.047(2) 0.0417(16) 0.0103(14) -0.0074(14) -0.0001(15) C14 0.042(2) 0.046(2) 0.0326(15) 0.0022(14) -0.0113(14) -0.0011(16) C15 0.0362(18) 0.0378(18) 0.0264(13) 0.0031(12) -0.0044(13) 0.0031(14) C16 0.0356(18) 0.059(2) 0.0266(14) -0.0047(14) -0.0050(13) 0.0028(15) C17 0.0302(17) 0.0341(18) 0.0272(14) -0.0019(12) 0.0044(12) 0.0007(14) C18 0.0248(16) 0.0307(17) 0.0275(13) -0.0015(11) 0.0024(12) 0.0008(13) C19 0.0301(16) 0.0258(16) 0.0240(13) -0.0009(11) 0.0005(12) -0.0008(12) C20 0.0344(17) 0.0261(17) 0.0299(14) -0.0003(12) 0.0001(12) -0.0006(13) C21 0.0351(18) 0.0296(18) 0.0365(15) -0.0006(13) -0.0041(13) -0.0004(13) C22 0.039(2) 0.057(2) 0.067(2) -0.0010(18) 0.0033(17) -0.0044(18) C23 0.040(2) 0.035(2) 0.0518(18) -0.0005(14) -0.0157(15) -0.0070(16) C24 0.0354(18) 0.0342(19) 0.0373(15) -0.0061(13) -0.0078(14) -0.0048(14) C25 0.049(2) 0.041(2) 0.0478(18) -0.0125(16) -0.0141(16) -0.0017(17) C26 0.058(2) 0.057(2) 0.058(2) -0.0232(17) 0.0054(18) 0.0044(19) N1 0.0307(14) 0.0392(15) 0.0222(11) -0.0044(10) 0.0002(10) -0.0003(11) N2 0.0328(14) 0.0395(16) 0.0287(12) -0.0046(11) 0.0010(11) 0.0026(12) O1 0.0451(13) 0.0373(13) 0.0348(10) -0.0044(9) -0.0028(9) 0.0138(10) O2 0.0321(12) 0.0596(15) 0.0344(10) -0.0149(10) 0.0038(9) 0.0074(10) O3 0.0348(12) 0.0678(16) 0.0351(11) -0.0146(10) -0.0081(10) 0.0085(11) O4 0.0513(16) 0.0434(15) 0.0828(18) -0.0008(12) -0.0124(13) -0.0163(12) O5 0.0712(18) 0.0365(15) 0.0778(16) -0.0215(12) -0.0080(13) -0.0081(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 H1 0.9500 . ? C1 C2 1.392(3) . ? C1 C6 1.387(4) . ? C2 H2 0.9500 . ? C2 C3 1.377(4) . ? C3 H3 0.9500 . ? C3 C4 1.384(4) . ? C4 H4 0.9500 . ? C4 C5 1.383(4) . ? C5 H5 0.9500 . ? C5 C6 1.390(4) . ? C6 C7 1.499(3) . ? C7 C8 1.510(3) . ? C7 O1 1.222(3) . ? C8 H8 1.0000 . ? C8 C9 1.541(3) . ? C8 C19 1.569(4) . ? C9 H9 1.0000 . ? C9 C10 1.518(4) . ? C9 N1 1.484(3) . ? C10 C11 1.389(4) . ? C10 C15 1.395(3) . ? C11 H11 0.9500 . ? C11 C12 1.392(4) . ? C12 H12 0.9500 . ? C12 C13 1.379(4) . ? C13 H13 0.9500 . ? C13 C14 1.374(4) . ? C14 H14 0.9500 . ? C14 C15 1.388(4) . ? C15 C16 1.493(4) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C16 N1 1.474(3) . ? C17 H17 0.9500 . ? C17 C18 1.357(3) . ? C17 N1 1.326(3) . ? C18 C19 1.502(3) . ? C18 N2 1.403(3) . ? C19 H19 1.0000 . ? C19 C20 1.502(3) . ? C20 H20 0.9500 . ? C20 C21 1.318(3) . ? C21 H21 0.9500 . ? C21 C24 1.482(4) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C22 C23 1.492(4) . ? C23 C24 1.368(4) . ? C23 O4 1.335(3) . ? C24 C25 1.442(4) . ? C25 C26 1.496(4) . ? C25 O5 1.259(3) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? N2 O2 1.252(2) . ? N2 O3 1.244(3) . ? O4 H4A 0.8400 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 H1 120.0 . . ? C6 C1 H1 120.0 . . ? C6 C1 C2 120.0(3) . . ? C1 C2 H2 119.9 . . ? C3 C2 C1 120.2(3) . . ? C3 C2 H2 119.9 . . ? C2 C3 H3 120.0 . . ? C2 C3 C4 120.0(3) . . ? C4 C3 H3 120.0 . . ? C3 C4 H4 120.0 . . ? C5 C4 C3 119.9(3) . . ? C5 C4 H4 120.0 . . ? C4 C5 H5 119.7 . . ? C4 C5 C6 120.5(3) . . ? C6 C5 H5 119.7 . . ? C1 C6 C5 119.3(2) . . ? C1 C6 C7 123.2(2) . . ? C5 C6 C7 117.5(2) . . ? C6 C7 C8 119.5(2) . . ? O1 C7 C6 120.3(2) . . ? O1 C7 C8 120.2(2) . . ? C7 C8 H8 108.8 . . ? C7 C8 C9 112.0(2) . . ? C7 C8 C19 108.1(2) . . ? C9 C8 H8 108.8 . . ? C9 C8 C19 110.18(19) . . ? C19 C8 H8 108.8 . . ? C8 C9 H9 109.1 . . ? C10 C9 C8 119.7(2) . . ? C10 C9 H9 109.1 . . ? N1 C9 C8 108.1(2) . . ? N1 C9 H9 109.1 . . ? N1 C9 C10 101.1(2) . . ? C11 C10 C9 129.9(2) . . ? C11 C10 C15 119.4(3) . . ? C15 C10 C9 110.5(2) . . ? C10 C11 H11 120.4 . . ? C10 C11 C12 119.2(3) . . ? C12 C11 H11 120.4 . . ? C11 C12 H12 119.6 . . ? C13 C12 C11 120.7(3) . . ? C13 C12 H12 119.6 . . ? C12 C13 H13 119.7 . . ? C14 C13 C12 120.6(3) . . ? C14 C13 H13 119.7 . . ? C13 C14 H14 120.5 . . ? C13 C14 C15 119.1(3) . . ? C15 C14 H14 120.5 . . ? C10 C15 C16 111.5(2) . . ? C14 C15 C10 121.0(3) . . ? C14 C15 C16 127.5(2) . . ? C15 C16 H16A 111.4 . . ? C15 C16 H16B 111.4 . . ? H16A C16 H16B 109.2 . . ? N1 C16 C15 102.0(2) . . ? N1 C16 H16A 111.4 . . ? N1 C16 H16B 111.4 . . ? C18 C17 H17 118.9 . . ? N1 C17 H17 118.9 . . ? N1 C17 C18 122.1(2) . . ? C17 C18 C19 123.1(2) . . ? C17 C18 N2 118.5(2) . . ? N2 C18 C19 118.1(2) . . ? C8 C19 H19 107.6 . . ? C18 C19 C8 107.7(2) . . ? C18 C19 H19 107.6 . . ? C18 C19 C20 112.8(2) . . ? C20 C19 C8 113.2(2) . . ? C20 C19 H19 107.6 . . ? C19 C20 H20 117.7 . . ? C21 C20 C19 124.7(2) . . ? C21 C20 H20 117.7 . . ? C20 C21 H21 117.8 . . ? C20 C21 C24 124.4(3) . . ? C24 C21 H21 117.8 . . ? H22A C22 H22B 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C23 C22 H22A 109.5 . . ? C23 C22 H22B 109.5 . . ? C23 C22 H22C 109.5 . . ? C24 C23 C22 125.3(3) . . ? O4 C23 C22 112.6(3) . . ? O4 C23 C24 122.1(3) . . ? C23 C24 C21 120.7(3) . . ? C23 C24 C25 119.6(3) . . ? C25 C24 C21 119.7(3) . . ? C24 C25 C26 119.5(3) . . ? O5 C25 C24 121.7(3) . . ? O5 C25 C26 118.8(3) . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26B 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C16 N1 C9 113.5(2) . . ? C17 N1 C9 122.2(2) . . ? C17 N1 C16 123.6(2) . . ? O2 N2 C18 120.5(2) . . ? O3 N2 C18 118.1(2) . . ? O3 N2 O2 121.3(2) . . ? C23 O4 H4A 109.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O4 H4A O5 0.84 1.76 2.509(3) 147.3 . loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 C2 C3 C4 1.0(5) . . . . ? C1 C6 C7 C8 0.1(4) . . . . ? C1 C6 C7 O1 177.7(3) . . . . ? C2 C1 C6 C5 1.2(4) . . . . ? C2 C1 C6 C7 -179.1(3) . . . . ? C2 C3 C4 C5 0.6(5) . . . . ? C3 C4 C5 C6 -1.3(5) . . . . ? C4 C5 C6 C1 0.4(4) . . . . ? C4 C5 C6 C7 -179.3(3) . . . . ? C5 C6 C7 C8 179.9(2) . . . . ? C5 C6 C7 O1 -2.5(4) . . . . ? C6 C1 C2 C3 -1.9(4) . . . . ? C6 C7 C8 C9 -165.9(2) . . . . ? C6 C7 C8 C19 72.5(3) . . . . ? C7 C8 C9 C10 68.1(3) . . . . ? C7 C8 C9 N1 -177.1(2) . . . . ? C7 C8 C19 C18 173.4(2) . . . . ? C7 C8 C19 C20 48.0(3) . . . . ? C8 C9 C10 C11 -58.9(4) . . . . ? C8 C9 C10 C15 126.8(2) . . . . ? C8 C9 N1 C16 -138.8(2) . . . . ? C8 C9 N1 C17 31.7(3) . . . . ? C8 C19 C20 C21 -110.7(3) . . . . ? C9 C8 C19 C18 50.7(3) . . . . ? C9 C8 C19 C20 -74.7(3) . . . . ? C9 C10 C11 C12 -174.8(2) . . . . ? C9 C10 C15 C14 176.5(2) . . . . ? C9 C10 C15 C16 -2.0(3) . . . . ? C10 C9 N1 C16 -12.3(3) . . . . ? C10 C9 N1 C17 158.2(2) . . . . ? C10 C11 C12 C13 0.0(4) . . . . ? C10 C15 C16 N1 -5.4(3) . . . . ? C11 C10 C15 C14 1.5(4) . . . . ? C11 C10 C15 C16 -176.9(2) . . . . ? C11 C12 C13 C14 0.4(4) . . . . ? C12 C13 C14 C15 0.2(4) . . . . ? C13 C14 C15 C10 -1.1(4) . . . . ? C13 C14 C15 C16 177.1(3) . . . . ? C14 C15 C16 N1 176.3(3) . . . . ? C15 C10 C11 C12 -1.0(4) . . . . ? C15 C16 N1 C9 11.3(3) . . . . ? C15 C16 N1 C17 -159.1(2) . . . . ? C17 C18 C19 C8 -19.6(3) . . . . ? C17 C18 C19 C20 106.1(3) . . . . ? C17 C18 N2 O2 -2.2(4) . . . . ? C17 C18 N2 O3 179.4(2) . . . . ? C18 C17 N1 C9 0.7(4) . . . . ? C18 C17 N1 C16 170.3(2) . . . . ? C18 C19 C20 C21 126.6(3) . . . . ? C19 C8 C9 C10 -171.6(2) . . . . ? C19 C8 C9 N1 -56.7(3) . . . . ? C19 C18 N2 O2 -177.6(2) . . . . ? C19 C18 N2 O3 4.0(4) . . . . ? C19 C20 C21 C24 -177.6(2) . . . . ? C20 C21 C24 C23 76.3(4) . . . . ? C20 C21 C24 C25 -101.6(3) . . . . ? C21 C24 C25 C26 -3.5(4) . . . . ? C21 C24 C25 O5 174.8(3) . . . . ? C22 C23 C24 C21 1.9(4) . . . . ? C22 C23 C24 C25 179.8(3) . . . . ? C23 C24 C25 C26 178.6(3) . . . . ? C23 C24 C25 O5 -3.1(4) . . . . ? N1 C9 C10 C11 -177.4(3) . . . . ? N1 C9 C10 C15 8.3(3) . . . . ? N1 C17 C18 C19 -7.1(4) . . . . ? N1 C17 C18 N2 177.7(2) . . . . ? N2 C18 C19 C8 155.6(2) . . . . ? N2 C18 C19 C20 -78.7(3) . . . . ? O1 C7 C8 C9 16.5(4) . . . . ? O1 C7 C8 C19 -105.0(3) . . . . ? O4 C23 C24 C21 -176.2(3) . . . . ? O4 C23 C24 C25 1.7(4) . . . . ? loop_ _refln_index_h _refln_index_k _refln_index_l _refln_F_squared_meas _refln_F_squared_sigma 0 -1 0 0.02 0.08 0 2 0 1000 18.63 0 -2 0 994.87 18.81 0 3 0 -0.18 0.2 0 -3 0 0.11 0.24 0 3 0 0.17 0.23 0 4 0 72.64 2.6 0 4 0 72.3 2.63 0 -4 0 81.07 2.78 0 -5 0 0.09 0.38 0 5 0 -0.08 0.26 0 5 0 -0.08 0.31 0 -6 0 5.33 1.12 0 6 0 4.73 1 0 6 0 3.95 0.95 0 -7 0 0.55 0.48 0 -8 0 0.35 0.54 0 -9 0 0.4 0.55 0 -10 0 3.47 1.51 0 -11 0 0.84 0.7 0 -12 0 1.43 1.05 -1 1 0 14.28 0.53 -1 -1 0 14.77 0.59 1 -1 0 14.61 0.54 1 -1 0 13.73 0.58 1 1 0 13.76 0.58 -1 2 0 -0.12 0.18 -1 -2 0 -0.12 0.19 1 -2 0 0.01 0.19 1 2 0 0.12 0.24 -1 3 0 66.93 2.11 1 -3 0 66.26 2.2 -1 3 0 63.83 2.11 1 3 0 67.65 2.19 -1 -3 0 64.96 2.15 -1 4 0 -0.01 0.27 -1 4 0 0.02 0.26 1 -4 0 -0.42 0.26 1 4 0 -0.3 0.21 1 4 0 -0.11 0.24 -1 -4 0 -0.17 0.24 1 -5 0 0.49 0.41 -1 -5 0 1.59 0.57 -1 5 0 0.02 0.39 -1 5 0 0.73 0.39 1 5 0 1.35 0.51 -1 -6 0 -0.33 0.25 -1 6 0 0.26 0.31 1 -6 0 -0.06 0.43 -1 6 0 0.11 0.34 1 -7 0 5.23 1.2 -1 -7 0 4.87 1.24 1 -8 0 0.85 0.68 -1 -8 0 0.72 0.63 -1 -9 0 0.67 0.74 1 -9 0 0.16 0.62 1 -10 0 0.16 0.68 -1 -10 0 0.44 0.7 -1 -11 0 -0.35 0.73 1 -11 0 0.39 0.7 1 -12 0 0.58 0.89 -1 -12 0 0.26 1.08 2 0 0 23 1.48 2 1 0 0.2 0.16 -2 1 0 -0.01 0.12 -2 -1 0 0 0.13 2 -1 0 0.04 0.12 -2 2 0 11.54 0.67 -2 -2 0 11.15 0.74 2 -2 0 10.71 0.7 2 -2 0 10.75 0.76 2 2 0 12.58 0.81 -2 3 0 -0.07 0.21 -2 3 0 0.08 0.19 2 -3 0 0.02 0.24 2 -3 0 0.1 0.22 -2 -3 0 0.02 0.22 2 3 0 0.13 0.24 2 4 0 31.09 1.74 2 -4 0 35.23 1.85 -2 4 0 33.38 1.67 -2 4 0 33.77 1.76 -2 -4 0 33.59 1.77 2 5 0 0.01 0.27 -2 5 0 0.12 0.31 -2 5 0 -0.07 0.26 2 -5 0 -0.34 0.21 -2 -5 0 -0.27 0.27 2 5 0 0.44 0.36 2 6 0 -0.69 0.28 -2 6 0 0.14 0.35 -2 -6 0 -0.46 0.19 2 -6 0 -0.11 0.39 -2 6 0 -0.39 0.29 2 -7 0 -0.37 0.36 -2 -7 0 -0.19 0.38 2 -8 0 3.15 1.06 -2 -8 0 4.21 1.19 -2 -9 0 0.68 0.71 2 -9 0 -0.41 0.55 2 -10 0 -0.17 0.65 -2 -10 0 1.18 0.85 2 -11 0 -0.11 0.79 -2 -11 0 0.79 0.8 2 -12 0 0.25 1.01 -2 -12 0 -1.56 0.71 -3 0 0 -0.13 0.15 3 0 0 -0.15 0.23 -3 1 0 0.8 0.19 3 -1 0 0.57 0.18 3 1 0 0.49 0.21 -3 -1 0 0.31 0.18 3 -2 0 0.05 0.14 -3 2 0 0.06 0.14 3 2 0 -0.07 0.16 -3 -2 0 -0.01 0.14 3 -3 0 0.26 0.24 3 -3 0 0.01 0.23 -3 -3 0 0.12 0.24 -3 3 0 0.36 0.25 3 3 0 0.68 0.34 3 4 0 0.38 0.34 -3 4 0 0.5 0.3 3 -4 0 -0.17 0.28 -3 -4 0 0.46 0.28 3 -5 0 1.09 0.58 3 5 0 1.09 0.46 -3 -5 0 0.73 0.44 3 -6 0 -0.29 0.36 -3 6 0 0.21 0.43 -3 -6 0 0.24 0.46 3 -7 0 10.14 1.64 -3 -7 0 12.23 1.49 -3 7 0 14.58 1.5 -3 -8 0 -0.42 0.56 3 -8 0 -0.36 0.44 3 -9 0 8.39 1.74 -3 -9 0 10.18 1.88 -3 -10 0 -0.44 0.47 3 -10 0 -0.72 0.64 3 -11 0 0.03 0.67 -3 -11 0 -0.35 0.74 4 0 0 54.23 3.22 -4 0 0 52.62 3.23 4 -1 0 0.07 0.13 -4 1 0 0.01 0.13 -4 -1 0 0.02 0.15 -4 -2 0 27.01 1.19 4 -2 0 31.42 1.37 -4 2 0 29.32 1.05 4 2 0 29.28 1.33 4 -3 0 0.01 0.24 4 -3 0 0.08 0.22 -4 3 0 -0.06 0.15 -4 -3 0 0.07 0.2 4 3 0 -0.07 0.21 -4 -4 0 5.45 0.88 -4 4 0 6.78 0.76 4 -4 0 6.5 0.78 4 -4 0 6.13 0.99 4 4 0 6.25 1.01 4 -5 0 0.23 0.35 -4 5 0 0 0.33 4 5 0 0.07 0.32 -4 -5 0 -0.02 0.31 4 -6 0 9.79 1.83 -4 6 0 9.86 1.08 -4 7 0 -0.37 0.34 -4 -7 0 -0.24 0.39 4 -7 0 -0.53 0.39 -4 -8 0 -1.05 0.42 4 -8 0 -0.42 0.52 4 -9 0 -0.13 0.53 -4 -9 0 -0.14 0.5 -4 -10 0 1.32 0.74 4 -10 0 1.51 0.97 -4 -11 0 -0.66 0.57 4 -11 0 0.67 0.96 5 0 0 -0.09 0.12 -5 1 0 275.72 3.69 5 -1 0 282.84 3.76 5 1 0 282.09 4.24 5 2 0 0.22 0.22 -5 2 0 0.41 0.19 5 -2 0 -0.13 0.13 -5 -2 0 0 0.15 -5 3 0 1.54 0.38 5 3 0 1.58 0.49 -5 -3 0 1.49 0.42 5 -3 0 1.43 0.38 5 4 0 0.34 0.32 -5 -4 0 -0.03 0.24 5 -4 0 0.05 0.22 -5 4 0 0.49 0.28 5 -4 0 0.07 0.33 -5 5 0 1.21 0.43 5 -5 0 1.81 0.66 5 5 0 1.9 0.53 -5 -5 0 1.08 0.49 -5 6 0 -0.39 0.27 -5 -6 0 -0.1 0.3 5 -6 0 0.24 0.41 -5 -7 0 16.94 1.74 5 -7 0 16.96 1.83 5 -8 0 0.24 0.56 -5 -8 0 0.69 0.58 5 -9 0 -0.52 0.55 -5 -9 0 0.05 0.59 5 -10 0 0.21 0.7 -5 -10 0 -0.07 0.73 5 -11 0 -0.2 0.73 -5 -11 0 0.17 0.76 6 0 0 90.69 2.19 6 1 0 0.1 0.22 6 -1 0 0.06 0.17 6 2 0 142.87 3.31 6 -2 0 138.26 2.68 -6 -2 0 142.28 3.08 -6 2 0 142.15 2.67 6 3 0 0.14 0.3 6 -3 0 -0.07 0.2 -6 3 0 0.04 0.21 -6 -3 0 0.04 0.25 -6 -4 0 28.17 1.64 -6 4 0 24.75 1.33 6 -4 0 25.73 1.42 6 4 0 29.11 2.08 6 -4 0 26.87 1.81 -6 -5 0 -0.15 0.29 -6 5 0 0.47 0.29 6 -5 0 -0.4 0.28 6 -5 0 -0.16 0.29 6 5 0 0.28 0.44 -6 6 0 1.39 0.61 6 -6 0 2.6 0.92 -6 -6 0 2.98 0.84 6 -7 0 -0.25 0.36 -6 -7 0 -0.01 0.45 -6 -8 0 4.34 1.18 6 -8 0 3.8 1.22 6 -9 0 1.08 0.83 -6 -9 0 -0.37 0.48 -6 -10 0 0.6 0.85 6 -10 0 2.56 1.29 6 -11 0 -0.06 0.9 -6 -11 0 0.3 0.85 7 0 0 -0.14 0.15 7 1 0 7.51 0.72 7 -1 0 7.86 0.65 -7 -2 0 -0.16 0.16 7 2 0 0.35 0.23 7 -2 0 -0.02 0.17 -7 2 0 0.39 0.2 -7 3 0 100.44 2.45 -7 -3 0 104.14 2.93 7 -3 0 101.78 2.56 7 3 0 97.61 3.14 -7 4 0 -0.05 0.22 -7 -4 0 0.2 0.28 7 -4 0 0.05 0.24 7 -5 0 37.11 1.91 -7 -5 0 34.4 2.01 7 -5 0 34.37 2.26 -7 5 0 32.8 1.7 -7 -6 0 -0.72 0.38 7 -6 0 0.16 0.44 -7 6 0 0.27 0.36 7 -7 0 2.63 1.03 -7 7 0 2.66 0.66 -7 -7 0 2.44 0.81 -7 -8 0 -0.01 0.53 7 -8 0 1.85 0.87 -7 -9 0 1.45 0.82 7 -9 0 1.36 0.99 7 -10 0 -0.75 0.74 -7 -10 0 0.15 0.56 -7 -11 0 1.59 1.08 7 -11 0 1.03 1.2 8 0 0 29.18 1.39 8 -1 0 0.11 0.21 8 1 0 -0.15 0.19 8 2 0 22.69 1.41 -8 2 0 22.49 1.1 8 -2 0 25.81 1.2 8 3 0 0.69 0.36 -8 3 0 -0.15 0.17 -8 -3 0 -0.26 0.19 -8 -4 0 21.57 1.47 -8 4 0 21.21 1.24 8 -4 0 21.74 1.32 8 4 0 21.73 1.66 8 -5 0 0.07 0.46 -8 -5 0 0.08 0.27 8 -5 0 -0.25 0.23 -8 5 0 -0.06 0.27 8 -6 0 3.34 0.94 -8 6 0 3.31 0.74 -8 -6 0 4.51 0.99 8 -7 0 -0.61 0.46 -8 -7 0 0.45 0.41 -8 7 0 -0.86 0.38 8 -8 0 0.63 0.73 -8 -8 0 0.64 0.59 8 -9 0 0.58 0.89 -8 -9 0 0.83 0.73 -8 -10 0 0.69 0.94 8 -10 0 1.23 0.96 -8 -11 0 -0.19 0.78 8 -11 0 0.8 1.08 9 0 0 0.04 0.23 9 -1 0 0.63 0.29 9 1 0 0.6 0.38 9 -2 0 0.29 0.26 9 2 0 0.26 0.31 9 3 0 2.77 0.72 -9 -3 0 2.16 0.56 9 -3 0 3.29 0.58 -9 3 0 2.93 0.54 -9 4 0 0.21 0.26 -9 -4 0 0.1 0.25 9 -4 0 0.29 0.28 9 -5 0 4.81 1.25 -9 -5 0 4.75 0.96 9 -5 0 6.96 0.87 -9 5 0 6.44 0.94 -9 -6 0 -0.59 0.39 9 -6 0 0.96 0.69 -9 6 0 -0.05 0.34 -9 -7 0 3.82 1.02 -9 7 0 4.27 0.83 9 -7 0 3.15 1.06 -9 -8 0 0.56 0.62 9 -8 0 -0.02 0.71 9 -9 0 0.65 0.88 -9 -9 0 1.6 0.81 -9 -10 0 -0.14 0.77 9 -10 0 -0.22 0.71 10 0 0 1.76 0.48 10 1 0 0.37 0.24 10 -1 0 0.09 0.23 10 2 0 8.12 0.98 10 -2 0 9.89 0.85 -10 3 0 0.28 0.23 10 -3 0 0 0.21 10 3 0 0.11 0.31 10 -4 0 2.36 0.57 -10 -4 0 2.24 0.57 -10 4 0 2.59 0.51 10 -5 0 -0.24 0.32 -10 -5 0 0.09 0.34 -10 5 0 -0.47 0.3 -10 6 0 3.81 0.76 10 -6 0 2.96 0.74 10 -6 0 4.78 1.28 -10 -6 0 3.56 0.89 -10 7 0 -0.39 0.39 10 -7 0 -0.3 0.46 -10 -7 0 -0.41 0.35 -10 -8 0 0.25 0.59 10 -8 0 -0.7 0.64 10 -9 0 -0.13 0.79 -10 -9 0 -0.41 0.48 -10 -10 0 3.22 1.09 10 -10 0 3.52 1.57 11 0 0 -0.13 0.25 11 1 0 0.24 0.35 11 -1 0 -0.08 0.29 11 1 0 0.17 0.34 11 -2 0 0.25 0.22 11 -3 0 23.7 1.35 11 -4 0 0.29 0.36 -11 4 0 -0.01 0.26 -11 5 0 15.04 1.18 11 -5 0 17.83 1.35 -11 -5 0 16.47 1.5 -11 6 0 0.62 0.39 11 -6 0 -0.55 0.5 11 -6 0 -0.3 0.3 -11 -6 0 -0.12 0.32 -11 -7 0 1.87 0.75 -11 7 0 3.88 0.84 11 -7 0 3.38 1.13 -11 -8 0 -0.49 0.63 11 -8 0 0.21 0.7 11 -9 0 0.6 0.93 -11 -9 0 0.54 0.72 -11 -10 0 -0.24 0.79 11 -10 0 -0.1 1.11 12 0 0 19.05 1.38 12 0 0 19.41 1.47 12 -1 0 0.12 0.27 12 1 0 0.11 0.3 12 1 0 -0.12 0.41 12 -2 0 4.55 0.74 -12 4 0 13.82 1.05 12 -4 0 11.31 1.05 -12 5 0 -0.14 0.31 -12 6 0 0.58 0.43 -12 -6 0 1.79 0.67 12 -6 0 0.47 0.47 12 -6 0 -0.78 0.55 12 -7 0 0.63 0.74 -12 -7 0 0.01 0.53 -12 7 0 -0.43 0.53 -12 -8 0 2.43 0.93 -12 -9 0 -0.18 0.72 12 -9 0 0.14 0.77 13 0 0 -0.15 0.33 13 -1 0 8.01 0.93 13 1 0 6.12 1.08 13 -2 0 0.01 0.29 13 -3 0 24.99 1.45 13 -4 0 0.43 0.33 -13 5 0 7.73 0.9 13 -5 0 8.76 1.01 13 -6 0 0.27 0.43 -13 6 0 0.88 0.48 -13 -6 0 -0.43 0.35 13 -6 0 0.58 0.78 -13 -7 0 -0.22 0.42 13 -7 0 -0.02 0.63 13 -8 0 -0.18 0.77 -13 -8 0 0.57 0.66 13 -9 0 1.67 1.16 -13 -9 0 1.34 0.87 14 0 0 4.46 0.89 14 1 0 -0.24 0.39 14 -1 0 -0.35 0.28 14 -2 0 3.17 0.65 14 2 0 2.49 0.82 14 -3 0 0.04 0.32 14 -4 0 0.08 0.38 14 -5 0 -0.06 0.35 14 -6 0 -0.61 0.71 -14 6 0 -0.16 0.46 14 -7 0 -0.28 0.76 -14 -7 0 1.24 0.7 -14 7 0 1.08 0.71 14 -8 0 -0.82 0.7 -14 -8 0 -0.65 0.57 15 0 0 1.19 0.48 15 -1 0 -0.72 0.27 15 1 0 -0.35 0.42 15 -2 0 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0.91 3 -3 38 2.84 1.29 3 -3 38 0.26 0.8 3 -4 -38 1 0.67 -3 -4 38 1 1.04 3 4 38 0.36 0.96 3 -4 38 0.53 0.83 -3 -4 -38 0.37 0.81 3 -4 38 0.31 1.1 -3 4 38 2.08 0.96 -4 0 38 1.93 0.87 4 0 38 -0.19 0.8 4 0 38 -0.25 0.66 4 1 38 0.04 0.89 4 -1 38 0.3 0.8 -4 1 38 -0.18 0.77 4 -1 38 -0.38 0.73 -4 -2 38 0.24 0.9 4 2 38 -0.46 0.59 4 -2 -38 0.43 0.6 4 -2 38 -0.92 0.78 -4 2 38 -0.58 0.54 4 -2 38 0.17 0.74 4 3 38 -0.86 0.71 -4 -3 38 1.17 1.09 4 -3 -38 2 0.87 4 -3 38 1.55 1.16 -4 3 38 1.57 0.87 4 -3 38 -0.56 0.64 4 4 38 2.29 1.22 4 -4 -38 0.02 0.67 -4 -4 38 0.33 0.93 -4 -4 -38 -0.49 0.73 -4 4 38 -1.15 0.59 4 -4 38 0.63 1 4 -4 38 0.33 0.98 -5 0 38 0.23 0.74 5 0 38 1.05 0.99 5 1 38 1.08 0.75 -5 -1 38 -0.99 0.59 5 -1 38 -0.01 0.79 -5 1 38 -0.94 0.64 5 -1 38 1.39 0.93 -5 -2 38 1.45 0.86 5 -2 -38 -0.46 0.51 5 2 38 0.04 0.8 5 -2 38 0.05 0.71 5 -2 38 0.02 0.77 -5 2 38 -0.38 0.64 5 -3 -38 0.58 0.79 -5 -3 38 0.38 0.92 5 3 38 -0.2 0.75 5 -3 38 -1.21 0.62 -5 3 38 0.43 0.8 5 -3 38 -0.02 0.95 6 0 38 -0.73 0.78 -6 0 38 1.38 0.83 6 1 38 1.35 0.9 -6 -1 38 0.57 0.7 6 -1 38 -0.94 0.78 -6 1 38 1.87 0.89 6 -1 38 -0.04 0.72 6 2 38 0.14 0.92 6 -2 -38 -0.46 0.52 -6 -2 38 0.23 0.85 6 -2 38 0.31 0.91 6 -2 38 -1.31 0.73 -6 2 38 0.25 0.66 6 3 38 0.87 0.89 6 -3 -38 1.78 0.82 -6 -3 38 0.5 0.88 6 -3 38 0.31 1.03 6 -3 38 -1.51 0.74 -6 3 38 0.86 0.78 -7 0 38 -0.28 0.69 7 0 38 -0.79 0.77 7 1 38 1.13 0.97 -7 -1 38 -0.7 0.66 7 -1 38 1.41 1.09 -7 1 38 0 0.76 -7 -2 38 2.72 1.08 7 2 38 0.23 0.86 7 -2 38 -1.67 0.71 -7 2 38 0.36 0.83 7 -2 38 -1.02 0.82 -8 0 38 -1.21 0.66 8 0 38 0.53 0.85 0 0 39 -0.15 0.67 0 -1 39 0.45 0.78 0 1 39 1.06 0.88 0 -2 39 1.28 1.13 0 2 39 2.44 1.17 0 -3 39 -1.78 0.7 0 -3 -39 -0.69 0.48 0 3 39 0.63 0.85 1 0 39 0.86 0.67 -1 0 39 0.36 0.95 1 1 39 -0.45 0.77 -1 -1 39 1.01 0.97 -1 1 39 0.35 0.77 1 -1 39 1.24 0.96 -1 -2 39 2.72 1.08 1 2 39 -0.14 0.7 1 -2 39 0.41 1.05 -1 2 39 0.81 0.85 1 -3 -39 0.48 0.87 1 3 39 -1.24 0.56 -1 -3 39 0.6 1.05 -1 3 39 0.21 0.68 1 -3 39 0.24 1.04 -1 -3 -39 0 0.67 2 0 39 0.28 0.68 2 0 39 1.07 0.69 -2 0 39 -1.08 0.64 2 1 39 1.18 0.85 2 1 39 -0.42 0.53 -2 -1 39 0.9 0.9 2 -1 39 0.38 0.58 -2 1 39 1.25 0.85 2 -1 39 0.6 0.8 -2 -2 39 0.87 0.82 2 2 39 0.46 0.72 2 2 39 0.65 0.63 2 -2 39 -1.05 0.87 -2 2 39 0.79 1.01 2 -2 39 1.49 1.05 2 -3 -39 -0.1 0.58 -2 -3 39 0.56 0.83 2 3 39 0.17 0.78 2 3 39 -0.56 0.83 -2 3 39 -1.68 0.78 2 -3 39 -0.35 0.88 3 0 39 1.09 0.86 3 0 39 0.07 0.68 -3 0 39 -0.14 0.67 -3 -1 39 -0.62 0.87 3 1 39 -0.54 0.66 3 1 39 -0.11 0.67 3 -1 39 -1.16 0.58 -3 1 39 1.15 1.17 3 -1 39 0.44 0.95 -3 -2 39 0.8 0.88 3 -2 39 1.22 0.75 -3 2 39 -1.26 0.67 3 -2 39 1.09 0.97 3 3 39 0.97 1.11 -3 -3 39 1.26 1.08 3 -3 -39 0.64 0.71 -3 3 39 0.19 0.77 3 -3 39 2.2 1.09 3 -3 39 0.6 0.73 4 0 39 0.19 0.97 4 0 39 0.77 0.76 4 1 39 3.29 1.33 -4 -1 39 0.63 0.81 4 -1 39 1.58 1.06 -4 1 39 3.84 1.14 4 -1 39 3.04 1.04 4 2 39 -0.64 0.66 -4 -2 39 -0.42 0.71 4 -2 39 1.31 1.11 4 -2 39 0.6 0.84 -4 2 39 0.14 0.74 4 3 39 3.16 1.14 4 -3 -39 1.62 0.69 -4 -3 39 -0.98 0.81 4 -3 39 0.29 0.79 4 -3 39 1.84 1.24 -4 3 39 -1.04 0.79 5 0 39 0.47 0.9 -5 0 39 0.89 0.78 5 0 39 -0.24 0.84 -5 -1 39 -0.46 0.74 5 1 39 0.79 0.87 5 -1 39 -0.67 0.78 -5 1 39 -0.35 0.71 5 -1 39 0.47 0.93 -5 -2 39 0.77 0.83 5 2 39 -0.18 0.85 5 -2 39 -0.69 0.74 -5 2 39 -0.2 0.78 5 -2 39 -0.82 0.71 -6 0 39 -0.08 0.73 6 0 39 -1.46 0.77 6 1 39 0.04 0.76 6 -1 39 0.03 0.69 -6 1 39 1.24 0.89 6 -1 39 -0.09 0.8 0 0 40 1.07 0.89 0 -1 40 -0.86 0.8 0 1 40 0.2 0.89 0 2 40 1.03 0.88 0 -2 40 3.02 1.3 -1 0 40 0.02 0.77 1 0 40 0.67 0.99 -1 -1 40 0.22 0.79 1 1 40 -0.17 0.9 -1 1 40 -0.51 0.51 1 -1 40 0.82 0.89 1 2 40 1.7 0.99 -1 -2 40 -0.9 0.56 1 -2 40 0.16 0.83 -1 2 40 0.09 0.58 -2 0 40 0.24 0.66 2 0 40 -1.31 0.66 2 1 40 -0.39 0.89 -2 -1 40 -0.85 0.71 2 -1 40 -0.04 0.59 2 -1 40 -0.7 0.7 -2 1 40 -0.17 0.69 2 2 40 -0.78 0.79 -2 -2 40 0.04 0.84 -2 2 40 -0.27 0.77 2 -2 40 0.04 0.85 2 -2 40 0.1 0.65 3 0 40 1.54 0.88 -3 0 40 1.98 0.97 3 0 40 1.64 1.13 3 1 40 3.62 1.39 -3 -1 40 -0.67 0.68 -3 1 40 -0.43 0.69 3 -1 40 -0.01 0.77 3 -1 40 -0.71 0.66 -3 -2 40 1.93 1.02 3 2 40 1.44 1 3 -2 40 1.41 0.96 -3 2 40 3.32 1.08 3 -2 40 1.76 0.86 4 0 40 4.99 1.65 -4 0 40 4.56 1.38 4 0 40 4.55 1.26 4 1 40 0.65 0.93 -4 -1 40 1.37 0.82 4 1 40 1.23 0.8 4 -1 40 0.98 0.97 4 -1 40 -0.44 0.74 5 0 40 0.21 0.96 5 0 40 -0.14 0.82 -5 0 40 -0.01 0.88 0 0 41 -0.88 0.81 0 -1 41 0.7 0.99 0 1 41 0.04 0.85 1 0 41 0.75 1.05 -1 0 41 0.57 0.8 -1 -1 41 1.51 0.99 1 1 41 -0.02 1.06 -1 1 41 0.89 0.91 1 -1 41 0.34 0.85 -2 0 41 2.88 1.25 2 0 41 2.02 1 _iucr_refine_instructions_details ; b.res created by SHELXL-2014/7 TITL B in Pbcn #60 REM reset to Pbcn #60 CELL 0.71073 15.5191 9.0804 30.9354 90 90 90 ZERR 8 0.0007 0.0005 0.0013 0 0 0 LATT 1 SYMM 0.5-X,0.5-Y,0.5+Z SYMM 0.5+X,0.5-Y,-Z SYMM -X,+Y,0.5-Z SFAC C H N O UNIT 208 192 16 40 L.S. 7 0 0 PLAN 20 SIZE 0.21 0.14 0.08 TEMP -123.16 MPLA C1 C2 C3 C4 C5 C6 MPLA C10 C11 C12 C13 C14 C15 HTAB O4 O5 BOND $H CONF HTAB fmap 2 acta SHEL 999 0.8 REM REM REM WGHT 0.044200 0.823500 FVAR 0.08049 C1 1 0.632208 0.361272 0.288301 11.00000 0.03210 0.04065 = 0.02948 0.00390 -0.00100 -0.00463 AFIX 43 H1 2 0.611276 0.423139 0.310729 11.00000 -1.20000 AFIX 0 C2 1 0.620192 0.400904 0.245259 11.00000 0.03799 0.04717 = 0.03782 0.01277 -0.01120 -0.00930 AFIX 43 H2 2 0.589498 0.488313 0.238356 11.00000 -1.20000 AFIX 0 C3 1 0.652652 0.313828 0.212636 11.00000 0.05321 0.07561 = 0.02841 0.00632 -0.00781 -0.01854 AFIX 43 H3 2 0.645149 0.342082 0.183308 11.00000 -1.20000 AFIX 0 C4 1 0.696179 0.185232 0.222569 11.00000 0.05195 0.07620 = 0.02978 -0.00643 0.00301 0.00156 AFIX 43 H4 2 0.719032 0.125624 0.200086 11.00000 -1.20000 AFIX 0 C5 1 0.706380 0.143567 0.265253 11.00000 0.03407 0.05766 = 0.03411 -0.00491 0.00246 0.00544 AFIX 43 H5 2 0.735240 0.054169 0.271951 11.00000 -1.20000 AFIX 0 C6 1 0.674734 0.231476 0.298448 11.00000 0.02524 0.03740 = 0.02670 0.00021 -0.00092 -0.00012 C7 1 0.689040 0.180050 0.343938 11.00000 0.02659 0.02780 = 0.02984 -0.00269 0.00238 0.00189 C8 1 0.655953 0.271973 0.381086 11.00000 0.02962 0.02209 = 0.02521 0.00217 0.00169 0.00036 AFIX 13 H8 2 0.671164 0.377420 0.375727 11.00000 -1.20000 AFIX 0 C9 1 0.695126 0.223943 0.424642 11.00000 0.02950 0.02744 = 0.02662 -0.00115 0.00008 0.00287 AFIX 13 H9 2 0.681028 0.117970 0.429870 11.00000 -1.20000 AFIX 0 C10 1 0.790329 0.248774 0.433270 11.00000 0.03409 0.02676 = 0.02879 0.00461 -0.00359 0.00222 C11 1 0.861880 0.197791 0.410856 11.00000 0.03881 0.02758 = 0.03795 0.00343 -0.00172 0.00450 AFIX 43 H11 2 0.855018 0.144374 0.384677 11.00000 -1.20000 AFIX 0 C12 1 0.943775 0.225926 0.427225 11.00000 0.03335 0.04112 = 0.04418 0.01115 0.00082 0.00683 AFIX 43 H12 2 0.993024 0.191412 0.412059 11.00000 -1.20000 AFIX 0 C13 1 0.954223 0.303326 0.465203 11.00000 0.03306 0.04694 = 0.04171 0.01027 -0.00745 -0.00010 AFIX 43 H13 2 1.010582 0.322131 0.475843 11.00000 -1.20000 AFIX 0 C14 1 0.883885 0.353546 0.487821 11.00000 0.04198 0.04624 = 0.03261 0.00221 -0.01134 -0.00110 AFIX 43 H14 2 0.891278 0.407058 0.513947 11.00000 -1.20000 AFIX 0 C15 1 0.801924 0.325010 0.471969 11.00000 0.03616 0.03777 = 0.02639 0.00311 -0.00435 0.00311 C16 1 0.717695 0.363594 0.492386 11.00000 0.03556 0.05862 = 0.02655 -0.00470 -0.00496 0.00279 AFIX 23 H16A 2 0.709282 0.310083 0.519947 11.00000 -1.20000 H16B 2 0.713077 0.470806 0.497718 11.00000 -1.20000 AFIX 0 C17 1 0.575454 0.364191 0.456696 11.00000 0.03019 0.03414 = 0.02719 -0.00188 0.00436 0.00071 AFIX 43 H17 2 0.553383 0.422840 0.479589 11.00000 -1.20000 AFIX 0 C18 1 0.523871 0.333803 0.422433 11.00000 0.02481 0.03068 = 0.02745 -0.00151 0.00242 0.00081 C19 1 0.555262 0.256941 0.382436 11.00000 0.03013 0.02582 = 0.02399 -0.00090 0.00048 -0.00079 AFIX 13 H19 2 0.531565 0.311095 0.356923 11.00000 -1.20000 AFIX 0 C20 1 0.524795 0.100274 0.379510 11.00000 0.03436 0.02614 = 0.02987 -0.00032 0.00012 -0.00061 AFIX 43 H20 2 0.535727 0.037594 0.403479 11.00000 -1.20000 AFIX 0 C21 1 0.483989 0.043548 0.346079 11.00000 0.03510 0.02960 = 0.03646 -0.00062 -0.00414 -0.00040 AFIX 43 H21 2 0.474980 0.104916 0.321622 11.00000 -1.20000 AFIX 0 C22 1 0.322545 -0.047083 0.391464 11.00000 0.03936 0.05716 = 0.06650 -0.00097 0.00334 -0.00441 AFIX 137 H22A 2 0.330406 -0.067434 0.422324 11.00000 -1.50000 H22B 2 0.261967 -0.061984 0.383661 11.00000 -1.50000 H22C 2 0.339008 0.055021 0.385370 11.00000 -1.50000 AFIX 0 C23 1 0.377729 -0.148839 0.365645 11.00000 0.04047 0.03487 = 0.05183 -0.00053 -0.01569 -0.00696 C24 1 0.451195 -0.109627 0.344075 11.00000 0.03538 0.03419 = 0.03725 -0.00606 -0.00779 -0.00476 C25 1 0.498769 -0.219531 0.320363 11.00000 0.04892 0.04131 = 0.04782 -0.01249 -0.01407 -0.00172 C26 1 0.577960 -0.175642 0.295998 11.00000 0.05784 0.05661 = 0.05849 -0.02316 0.00538 0.00440 AFIX 137 H26A 2 0.598537 -0.259367 0.278880 11.00000 -1.50000 H26B 2 0.622865 -0.145550 0.316445 11.00000 -1.50000 H26C 2 0.564361 -0.093252 0.276707 11.00000 -1.50000 AFIX 0 N1 3 0.655649 0.314713 0.459271 11.00000 0.03075 0.03918 = 0.02216 -0.00441 0.00019 -0.00026 N2 3 0.438757 0.385957 0.422955 11.00000 0.03284 0.03950 = 0.02868 -0.00457 0.00102 0.00260 O1 4 0.724640 0.062325 0.350860 11.00000 0.04513 0.03728 = 0.03475 -0.00443 -0.00282 0.01377 O2 4 0.410489 0.455060 0.454973 11.00000 0.03208 0.05958 = 0.03439 -0.01489 0.00381 0.00737 O3 4 0.392068 0.358606 0.391250 11.00000 0.03485 0.06778 = 0.03514 -0.01461 -0.00808 0.00846 O4 4 0.349200 -0.287476 0.366470 11.00000 0.05128 0.04338 = 0.08284 -0.00084 -0.01239 -0.01634 AFIX 147 H4A 2 0.382093 -0.340961 0.351686 11.00000 -1.50000 AFIX 0 O5 4 0.476638 -0.352968 0.320426 11.00000 0.07124 0.03655 = 0.07782 -0.02145 -0.00797 -0.00806 HKLF 4 REM B in Pbcn #60 REM R1 = 0.0556 for 2370 Fo > 4sig(Fo) and 0.1353 for all 4463 data REM 301 parameters refined using 0 restraints END WGHT 0.0443 0.8120 REM Instructions for potential hydrogen bonds EQIV $1 -x+3/2, y+1/2, z HTAB C8 O1_$1 EQIV $2 -x+1, -y+1, -z+1 HTAB C16 O2_$2 HTAB C17 O2_$2 EQIV $3 -x+1/2, y-1/2, z HTAB C22 O3_$3 HTAB O4 O5 REM Highest difference peak 0.206, deepest hole -0.249, 1-sigma level 0.055 Q1 1 0.9215 0.5028 0.4701 11.00000 0.05 0.21 Q2 1 0.3367 0.2755 0.3990 11.00000 0.05 0.19 Q3 1 0.2821 -0.3587 0.3996 11.00000 0.05 0.19 Q4 1 0.3951 0.2476 0.3791 11.00000 0.05 0.19 Q5 1 0.6360 -0.0383 0.2487 11.00000 0.05 0.19 Q6 1 0.7990 0.2417 0.4603 11.00000 0.05 0.19 Q7 1 0.6581 -0.0487 0.4301 11.00000 0.05 0.19 Q8 1 0.5378 0.2983 0.4052 11.00000 0.05 0.19 Q9 1 0.6948 0.0729 0.2001 11.00000 0.05 0.18 Q10 1 0.5671 0.4748 0.4220 11.00000 0.05 0.18 Q11 1 0.4032 -0.2018 0.4209 11.00000 0.05 0.17 Q12 1 0.5485 0.4110 0.3228 11.00000 0.05 0.17 Q13 1 0.6981 0.4967 0.3611 11.00000 0.05 0.17 Q14 1 0.2634 -0.1024 0.4216 11.00000 0.05 0.17 Q15 1 0.6189 0.3256 0.2353 11.00000 0.05 0.17 Q16 1 0.4753 0.4490 0.3420 11.00000 0.05 0.17 Q17 1 0.4756 0.3035 0.3317 11.00000 0.05 0.17 Q18 1 0.5387 -0.3798 0.2715 11.00000 0.05 0.17 Q19 1 0.7412 0.4009 0.3426 11.00000 0.05 0.17 Q20 1 0.6450 0.4959 0.3500 11.00000 0.05 0.17 REM The information below was added by Olex2. REM REM R1 = 0.0556 for 2370 Fo > 4sig(Fo) and 0.1353 for all 29959 data REM n/a parameters refined using n/a restraints REM Highest difference peak 0.21, deepest hole -0.25 REM Mean Shift 0, Max Shift 0.000. REM +++ Tabular Listing of Refinement Information +++ REM R1_all = 0.1353 REM R1_gt = 0.0556 REM wR_ref = 0.1364 REM GOOF = 1.037 REM Shift_max = 0.000 REM Shift_mean = 0 REM Reflections_all = 29959 REM Reflections_gt = 2370 REM Parameters = n/a REM Hole = -0.25 REM Peak = 0.21 REM Flack = n/a ; _olex2_submission_special_instructions 'No special instructions were received'