data_p16282_a _audit_creation_date 2016-09-08 _audit_creation_method ; Olex2 1.2 (compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155) ; _publ_contact_author_address ; Beckman Institute Caltech 139-74 Pasadena CA 91125 USA ; _publ_contact_author_email xray@caltech.edu _publ_contact_author_name 'Sarah E. Reisman' _publ_contact_author_phone ? _publ_section_references ; Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H. (2009), J. Appl. Cryst. 42, 339-341. Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122. Sheldrick, G.M. (2015). Acta Cryst. A71, 3-8. ; _chemical_name_common CX-10-028 _chemical_name_systematic CX-10-028 _chemical_formula_moiety 'C42 H48 B N O10' _chemical_formula_sum 'C42 H48 B N O10' _chemical_formula_weight 737.62 _chemical_absolute_configuration ad _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' 'B' 'B' 0.0090 0.0039 '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 4 _space_group_name_H-M_alt 'P 1 21 1' _space_group_name_Hall 'P 2yb' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 8.7826(4) _cell_length_b 22.1496(10) _cell_length_c 10.3099(5) _cell_angle_alpha 90 _cell_angle_beta 109.928(2) _cell_angle_gamma 90 _cell_volume 1885.50(15) _cell_formula_units_Z 2 _cell_measurement_reflns_used 9806 _cell_measurement_temperature 100 _cell_measurement_theta_max 78.65 _cell_measurement_theta_min 3.99 _shelx_estimated_absorpt_T_max 0.938 _shelx_estimated_absorpt_T_min 0.774 _exptl_absorpt_coefficient_mu 0.749 _exptl_absorpt_correction_T_max 0.7542 _exptl_absorpt_correction_T_min 0.6245 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS-2014/5 (Sheldrick, 2014)' _exptl_absorpt_special_details ? _exptl_crystal_colour 'clear colourless' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.299 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description Plate _exptl_crystal_F_000 784 _exptl_crystal_preparation ? _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.09 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0483 _diffrn_reflns_av_unetI/netI 0.0370 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.995 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_number 32011 _diffrn_reflns_point_group_measured_fraction_full 0.997 _diffrn_reflns_point_group_measured_fraction_max 0.980 _diffrn_reflns_theta_full 67.679 _diffrn_reflns_theta_max 79.080 _diffrn_reflns_theta_min 3.991 _diffrn_ambient_temperature 100 _diffrn_detector 'CMOS Area Detector' _diffrn_detector_area_resol_mean 10.24 _diffrn_detector_type 'Bruker PHOTON 100 CMOS' _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.995 _diffrn_measurement_device '\k-geometry diffractometer' _diffrn_measurement_device_type 'Bruker D8 VENTURE Kappa Duo PHOTON 100 CMOS' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_monochromator 'multilayer mirrors' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _diffrn_source 'I\mS HB micro-focus sealed tube' _diffrn_source_current 1 _diffrn_source_power 0.05 _diffrn_source_type 'Incoatech I\mS HB' _diffrn_source_voltage 50 _diffrn_standards_number 0 _reflns_Friedel_coverage 0.918 _reflns_Friedel_fraction_full 0.995 _reflns_Friedel_fraction_max 0.963 _reflns_number_gt 7609 _reflns_number_total 7996 _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 v8.34A (Bruker-AXS, 2007)' _computing_data_collection 'APEX2 v2014.11-0 (Bruker-AXS, 2014)' _computing_data_reduction 'SAINT v8.34A (Bruker-AXS, 2007)' _computing_molecular_graphics ? _computing_publication_material ? _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_structure_solution 'SHELXS-2013/1 (She ldrick, 2013)' _refine_diff_density_max 0.196 _refine_diff_density_min -0.192 _refine_diff_density_rms 0.038 _refine_ls_abs_structure_details ; Flack x determined using 3460 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack 0.12(5) _refine_ls_extinction_coef 0.00071(18) _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 1.047 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 496 _refine_ls_number_reflns 7996 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0338 _refine_ls_R_factor_gt 0.0311 _refine_ls_restrained_S_all 1.047 _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^)+(0.0361P)^2^+0.2542P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0732 _refine_ls_wR_factor_ref 0.0747 _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, {H17A,H17B,H1} of C17, All C(H,H) groups At 1.5 times of: {H16A,H16B,H16C} of C16, {H26A,H26B,H26C} of C26, {H20A,H20B,H20C} of C20, {H19A,H19B,H19C} of C19, {H18A,H18B,H18C} of C18 2.a Ternary CH refined with riding coordinates: C3(H3), C10(H10), C9(H9) 2.b Secondary CH2 refined with riding coordinates: C35(H35A,H35B), C27(H27A,H27B), C14(H14A,H14B), C36(H36A,H36B), C8(H8A,H8B), C7(H7A,H7B), C28(H28A,H28B) 2.c Aromatic/amide H refined with riding coordinates: C38(H38), C42(H42), C25(H25), C24(H24), C23(H23), C34(H34), C41(H41), C39(H39), C40(H40), C32(H32), C30(H30), C33(H33), C31(H31) 2.d X=CH2 refined with riding coordinates: C17(H17A,H17B) 2.e Idealised Me refined as rotating group: C20(H20A,H20B,H20C), C19(H19A,H19B,H19C), C16(H16A,H16B,H16C), C26(H26A,H26B, H26C), C18(H18A,H18B,H18C) ; _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap 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 0.42688(17) 0.42719(6) 0.51220(14) 0.0147(3) Uani 1 1 d . . . . . O8 O 0.39297(17) 0.46371(6) 0.08369(14) 0.0138(3) Uani 1 1 d . . . . . O6 O 0.76858(16) 0.44690(6) 0.60086(14) 0.0143(3) Uani 1 1 d . . . . . O3 O 0.10299(17) 0.36104(6) 0.09571(14) 0.0151(3) Uani 1 1 d . . . . . O7 O 0.47402(16) 0.54799(6) 0.28915(14) 0.0142(3) Uani 1 1 d . . . . . O5 O 0.62998(16) 0.43826(7) 0.25745(14) 0.0147(3) Uani 1 1 d . . . . . O10 O 0.54580(18) 0.63221(7) 0.19832(15) 0.0180(3) Uani 1 1 d . . . . . O9 O 0.98935(17) 0.49556(7) 0.56475(15) 0.0166(3) Uani 1 1 d . . . . . O2 O 0.22140(18) 0.37562(7) 0.53040(16) 0.0208(3) Uani 1 1 d . . . . . O4 O 0.05582(18) 0.39842(7) -0.11879(16) 0.0193(3) Uani 1 1 d . . . . . N1 N -0.2788(2) 0.37428(8) -0.17945(19) 0.0176(3) Uani 1 1 d . . . . . C37 C 1.1582(2) 0.57036(10) 0.7162(2) 0.0163(4) Uani 1 1 d . . . . . C15 C 0.2690(2) 0.41055(9) 0.4630(2) 0.0157(4) Uani 1 1 d . . . . . C21 C 0.0070(2) 0.37518(9) -0.0339(2) 0.0140(4) Uani 1 1 d . . . . . C1 C 0.4991(2) 0.35290(9) 0.3321(2) 0.0146(4) Uani 1 1 d . . . . . C5 C 0.2420(2) 0.47545(9) 0.2452(2) 0.0134(4) Uani 1 1 d . . . . . C22 C -0.1605(3) 0.35901(9) -0.0573(2) 0.0166(4) Uani 1 1 d . . . . . C35 C 0.9016(2) 0.44158(9) 0.5521(2) 0.0155(4) Uani 1 1 d . . . . . H35A H 0.9753 0.4095 0.6049 0.019 Uiso 1 1 calc R . . . . H35B H 0.8606 0.4293 0.4540 0.019 Uiso 1 1 calc R . . . . C27 C 0.4166(3) 0.60417(10) 0.2233(2) 0.0165(4) Uani 1 1 d . . . . . H27A H 0.3266 0.5974 0.1355 0.020 Uiso 1 1 calc R . . . . H27B H 0.3767 0.6298 0.2836 0.020 Uiso 1 1 calc R . . . . C14 C 0.1598(2) 0.43959(10) 0.3318(2) 0.0154(4) Uani 1 1 d . . . . . H14A H 0.0853 0.4672 0.3562 0.019 Uiso 1 1 calc R . . . . H14B H 0.0929 0.4075 0.2725 0.019 Uiso 1 1 calc R . . . . C6 C 0.3777(2) 0.51352(9) 0.3516(2) 0.0130(4) Uani 1 1 d . . . . . C36 C 1.1048(2) 0.50543(10) 0.6992(2) 0.0175(4) Uani 1 1 d . . . . . H36A H 1.1999 0.4790 0.7131 0.021 Uiso 1 1 calc R . . . . H36B H 1.0559 0.4949 0.7697 0.021 Uiso 1 1 calc R . . . . C2 C 0.3682(2) 0.32730(9) 0.2411(2) 0.0150(4) Uani 1 1 d . . . . . C8 C 0.4796(3) 0.57792(9) 0.5636(2) 0.0165(4) Uani 1 1 d . . . . . H8A H 0.4465 0.5997 0.6336 0.020 Uiso 1 1 calc R . . . . H8B H 0.5316 0.6074 0.5199 0.020 Uiso 1 1 calc R . . . . C3 C 0.2751(2) 0.37046(9) 0.12813(19) 0.0138(4) Uani 1 1 d . . . . . H3 H 0.3034 0.3620 0.0438 0.017 Uiso 1 1 calc R . . . . C20 C 0.7513(3) 0.55729(10) 0.7432(2) 0.0191(4) Uani 1 1 d . . . . . H20A H 0.8081 0.5829 0.6968 0.029 Uiso 1 1 calc GR . . . . H20B H 0.8243 0.5254 0.7947 0.029 Uiso 1 1 calc GR . . . . H20C H 0.7165 0.5819 0.8070 0.029 Uiso 1 1 calc GR . . . . C19 C 0.1125(2) 0.51071(9) 0.1339(2) 0.0169(4) Uani 1 1 d . . . . . H19A H 0.0216 0.4839 0.0871 0.025 Uiso 1 1 calc GR . . . . H19B H 0.1587 0.5266 0.0666 0.025 Uiso 1 1 calc GR . . . . H19C H 0.0742 0.5443 0.1764 0.025 Uiso 1 1 calc GR . . . . C10 C 0.6507(2) 0.49118(9) 0.52907(19) 0.0129(4) Uani 1 1 d . . . . . H10 H 0.6999 0.5186 0.4771 0.015 Uiso 1 1 calc R . . . . C7 C 0.3289(2) 0.55223(9) 0.4538(2) 0.0154(4) Uani 1 1 d . . . . . H7A H 0.2583 0.5857 0.4040 0.018 Uiso 1 1 calc R . . . . H7B H 0.2670 0.5274 0.4985 0.018 Uiso 1 1 calc R . . . . C38 C 1.2792(3) 0.58727(10) 0.8377(2) 0.0208(4) Uani 1 1 d . . . . . H38 H 1.3256 0.5578 0.9070 0.025 Uiso 1 1 calc R . . . . C12 C 0.5033(2) 0.42036(9) 0.30738(19) 0.0130(4) Uani 1 1 d . . . . . C29 C 0.7961(3) 0.68667(10) 0.2829(2) 0.0201(4) Uani 1 1 d . . . . . C42 C 1.0907(3) 0.61411(10) 0.6156(2) 0.0189(4) Uani 1 1 d . . . . . H42 H 1.0071 0.6033 0.5323 0.023 Uiso 1 1 calc R . . . . C4 C 0.3422(2) 0.43323(9) 0.18465(19) 0.0127(4) Uani 1 1 d . . . . . C25 C -0.4231(3) 0.35260(11) -0.1792(2) 0.0240(5) Uani 1 1 d . . . . . H25 H -0.5242 0.3571 -0.2514 0.029 Uiso 1 1 calc R . . . . C13 C 0.3129(3) 0.26380(10) 0.2364(2) 0.0204(4) Uani 1 1 d . . . . . C11 C 0.4967(2) 0.46260(9) 0.4270(2) 0.0125(4) Uani 1 1 d . . . . . C16 C 0.6322(3) 0.32153(10) 0.4424(2) 0.0202(4) Uani 1 1 d . . . . . H16A H 0.6328 0.3349 0.5332 0.030 Uiso 1 1 calc GR . . . . H16B H 0.7364 0.3313 0.4323 0.030 Uiso 1 1 calc GR . . . . H16C H 0.6147 0.2778 0.4340 0.030 Uiso 1 1 calc GR . . . . C9 C 0.6035(2) 0.52887(9) 0.6358(2) 0.0156(4) Uani 1 1 d . . . . . H9 H 0.5514 0.5012 0.6849 0.019 Uiso 1 1 calc R . . . . C24 C -0.3977(3) 0.32283(13) -0.0559(3) 0.0310(5) Uani 1 1 d . . . . . H24 H -0.4779 0.3031 -0.0284 0.037 Uiso 1 1 calc R . . . . C23 C -0.2321(3) 0.32695(12) 0.0214(2) 0.0245(5) Uani 1 1 d . . . . . H23 H -0.1792 0.3107 0.1108 0.029 Uiso 1 1 calc R . . . . C34 C 0.8846(3) 0.65114(10) 0.2235(3) 0.0249(5) Uani 1 1 d . . . . . H34 H 0.8541 0.6103 0.2013 0.030 Uiso 1 1 calc R . . . . C26 C 0.6583(3) 0.49486(11) 0.0473(2) 0.0215(4) Uani 1 1 d . . . . . H26A H 0.6301 0.4753 -0.0431 0.032 Uiso 1 1 calc GR . . . . H26B H 0.7742 0.4896 0.0979 0.032 Uiso 1 1 calc GR . . . . H26C H 0.6332 0.5380 0.0349 0.032 Uiso 1 1 calc GR . . . . C28 C 0.6575(3) 0.66018(11) 0.3179(2) 0.0236(5) Uani 1 1 d . . . . . H28A H 0.6988 0.6299 0.3923 0.028 Uiso 1 1 calc R . . . . H28B H 0.6019 0.6924 0.3513 0.028 Uiso 1 1 calc R . . . . C41 C 1.1455(3) 0.67353(11) 0.6368(2) 0.0230(4) Uani 1 1 d . . . . . H41 H 1.0997 0.7030 0.5675 0.028 Uiso 1 1 calc R . . . . C39 C 1.3334(3) 0.64665(11) 0.8595(2) 0.0262(5) Uani 1 1 d . . . . . H39 H 1.4159 0.6576 0.9431 0.031 Uiso 1 1 calc R . . . . C40 C 1.2663(3) 0.68995(11) 0.7583(2) 0.0254(5) Uani 1 1 d . . . . . H40 H 1.3032 0.7306 0.7725 0.030 Uiso 1 1 calc R . . . . C32 C 1.0651(3) 0.73388(12) 0.2318(3) 0.0298(5) Uani 1 1 d . . . . . H32 H 1.1580 0.7497 0.2162 0.036 Uiso 1 1 calc R . . . . C30 C 0.8427(3) 0.74657(11) 0.3146(2) 0.0262(5) Uani 1 1 d . . . . . H30 H 0.7823 0.7719 0.3535 0.031 Uiso 1 1 calc R . . . . C33 C 1.0170(3) 0.67450(11) 0.1963(3) 0.0287(5) Uani 1 1 d . . . . . H33 H 1.0749 0.6500 0.1534 0.034 Uiso 1 1 calc R . . . . C18 C 0.2785(3) 0.23080(11) 0.1038(3) 0.0282(5) Uani 1 1 d . . . . . H18A H 0.1972 0.2530 0.0299 0.042 Uiso 1 1 calc GR . . . . H18B H 0.2375 0.1904 0.1121 0.042 Uiso 1 1 calc GR . . . . H18C H 0.3783 0.2273 0.0818 0.042 Uiso 1 1 calc GR . . . . C31 C 0.9776(3) 0.76927(12) 0.2893(2) 0.0303(5) Uani 1 1 d . . . . . H31 H 1.0093 0.8100 0.3123 0.036 Uiso 1 1 calc R . . . . B1 B 0.5590(3) 0.46571(10) 0.1305(2) 0.0152(4) Uani 1 1 d . . . . . C17 C 0.2881(4) 0.23960(11) 0.3459(3) 0.0324(6) Uani 1 1 d . . . . . H17A H 0.3059 0.2630 0.4269 0.039 Uiso 1 1 calc R . . . . H17B H 0.2527 0.1989 0.3429 0.039 Uiso 1 1 calc R . . . . H1 H -0.263(4) 0.3947(16) -0.247(4) 0.039 Uiso 1 1 d 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 0.0146(6) 0.0169(7) 0.0137(6) 0.0019(5) 0.0062(6) -0.0012(5) O8 0.0143(6) 0.0168(7) 0.0112(6) 0.0023(5) 0.0055(5) 0.0001(5) O6 0.0112(6) 0.0183(7) 0.0128(6) 0.0024(5) 0.0031(5) 0.0003(5) O3 0.0124(6) 0.0188(7) 0.0127(6) 0.0016(5) 0.0025(5) -0.0013(5) O7 0.0137(6) 0.0146(7) 0.0151(7) 0.0026(5) 0.0061(6) 0.0007(5) O5 0.0115(6) 0.0197(7) 0.0139(6) -0.0013(5) 0.0055(5) 0.0004(5) O10 0.0171(7) 0.0205(7) 0.0150(7) 0.0014(5) 0.0037(6) -0.0042(6) O9 0.0142(7) 0.0198(7) 0.0144(7) 0.0010(5) 0.0029(6) -0.0038(5) O2 0.0193(7) 0.0234(8) 0.0215(7) 0.0042(6) 0.0091(6) -0.0026(6) O4 0.0172(7) 0.0234(8) 0.0162(7) 0.0043(6) 0.0041(6) -0.0021(6) N1 0.0158(8) 0.0205(9) 0.0149(8) 0.0013(7) 0.0032(7) -0.0007(7) C37 0.0148(9) 0.0213(10) 0.0151(9) 0.0003(7) 0.0083(8) -0.0009(8) C15 0.0155(9) 0.0173(10) 0.0161(9) -0.0017(7) 0.0078(8) -0.0001(7) C21 0.0148(9) 0.0135(9) 0.0123(8) 0.0003(7) 0.0026(8) 0.0009(7) C1 0.0159(9) 0.0154(9) 0.0128(9) 0.0001(7) 0.0052(8) 0.0029(7) C5 0.0132(9) 0.0151(9) 0.0128(8) -0.0008(7) 0.0057(8) -0.0004(7) C22 0.0168(10) 0.0175(10) 0.0142(9) 0.0009(7) 0.0035(8) 0.0008(8) C35 0.0120(8) 0.0186(10) 0.0160(9) 0.0000(7) 0.0050(8) 0.0001(7) C27 0.0144(9) 0.0194(10) 0.0144(9) 0.0040(7) 0.0033(8) 0.0004(7) C14 0.0123(9) 0.0190(10) 0.0164(9) -0.0007(7) 0.0066(8) -0.0013(7) C6 0.0109(8) 0.0160(9) 0.0125(9) 0.0010(7) 0.0048(8) -0.0004(7) C36 0.0142(9) 0.0220(10) 0.0140(9) 0.0001(7) 0.0020(8) -0.0021(8) C2 0.0155(9) 0.0161(9) 0.0126(9) 0.0000(7) 0.0037(8) 0.0032(7) C8 0.0181(10) 0.0172(10) 0.0154(9) -0.0028(7) 0.0073(8) -0.0002(8) C3 0.0115(9) 0.0160(9) 0.0127(8) 0.0009(7) 0.0028(7) 0.0007(7) C20 0.0210(10) 0.0212(11) 0.0148(9) -0.0045(8) 0.0055(9) -0.0023(8) C19 0.0127(9) 0.0180(10) 0.0189(10) -0.0009(7) 0.0038(8) 0.0002(7) C10 0.0121(9) 0.0143(9) 0.0109(8) 0.0002(7) 0.0022(7) 0.0007(7) C7 0.0158(9) 0.0169(9) 0.0152(9) -0.0004(7) 0.0076(8) 0.0018(7) C38 0.0218(10) 0.0264(11) 0.0139(9) 0.0030(8) 0.0054(9) -0.0031(8) C12 0.0109(8) 0.0173(9) 0.0110(8) 0.0007(7) 0.0039(7) 0.0014(7) C29 0.0201(10) 0.0197(10) 0.0165(9) 0.0020(8) 0.0009(9) -0.0034(8) C42 0.0159(10) 0.0237(11) 0.0165(10) 0.0013(8) 0.0047(8) 0.0013(8) C4 0.0118(8) 0.0161(9) 0.0108(8) 0.0011(7) 0.0044(7) -0.0001(7) C25 0.0147(10) 0.0315(12) 0.0221(11) 0.0044(9) 0.0017(9) -0.0003(9) C13 0.0187(10) 0.0168(10) 0.0201(10) 0.0009(8) -0.0007(8) 0.0017(8) C11 0.0127(8) 0.0152(9) 0.0103(8) 0.0012(7) 0.0050(7) -0.0004(7) C16 0.0193(10) 0.0188(10) 0.0168(9) -0.0015(8) -0.0013(8) 0.0039(8) C9 0.0176(9) 0.0177(9) 0.0119(9) -0.0019(7) 0.0056(8) -0.0030(8) C24 0.0182(11) 0.0432(15) 0.0312(12) 0.0122(11) 0.0081(10) -0.0051(10) C23 0.0188(10) 0.0345(13) 0.0199(10) 0.0095(9) 0.0062(9) -0.0003(9) C34 0.0227(11) 0.0161(10) 0.0346(13) 0.0039(9) 0.0080(10) 0.0000(8) C26 0.0177(10) 0.0273(11) 0.0200(10) 0.0015(9) 0.0071(9) -0.0011(8) C28 0.0240(11) 0.0279(12) 0.0186(10) -0.0048(8) 0.0067(9) -0.0062(9) C41 0.0245(11) 0.0220(11) 0.0233(11) 0.0050(8) 0.0090(9) 0.0027(9) C39 0.0303(12) 0.0292(12) 0.0169(10) -0.0029(9) 0.0052(10) -0.0102(10) C40 0.0337(13) 0.0186(11) 0.0258(11) -0.0041(8) 0.0127(11) -0.0038(9) C32 0.0205(11) 0.0308(13) 0.0320(12) 0.0096(10) 0.0011(10) -0.0079(10) C30 0.0369(13) 0.0216(11) 0.0175(10) -0.0018(8) 0.0061(10) -0.0036(9) C33 0.0204(11) 0.0262(12) 0.0392(13) 0.0073(10) 0.0097(10) 0.0042(9) C18 0.0348(13) 0.0194(11) 0.0245(11) -0.0016(9) 0.0024(10) 0.0002(9) C31 0.0395(13) 0.0225(11) 0.0234(11) -0.0001(9) 0.0036(11) -0.0129(11) B1 0.0150(10) 0.0174(10) 0.0135(10) -0.0038(8) 0.0052(9) 0.0000(8) C17 0.0484(15) 0.0199(11) 0.0292(12) 0.0019(9) 0.0135(12) -0.0070(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 C15 1.355(3) . ? O1 C11 1.459(2) . ? O8 C4 1.433(2) . ? O8 B1 1.371(3) . ? O6 C35 1.426(2) . ? O6 C10 1.435(2) . ? O3 C21 1.351(2) . ? O3 C3 1.448(2) . ? O7 C27 1.424(2) . ? O7 C6 1.444(2) . ? O5 C12 1.432(2) . ? O5 B1 1.384(3) . ? O10 C27 1.392(3) . ? O10 C28 1.429(3) . ? O9 C35 1.404(2) . ? O9 C36 1.428(2) . ? O2 C15 1.206(3) . ? O4 C21 1.212(3) . ? N1 C22 1.374(3) . ? N1 C25 1.356(3) . ? N1 H1 0.89(4) . ? C37 C36 1.504(3) . ? C37 C38 1.390(3) . ? C37 C42 1.396(3) . ? C15 C14 1.510(3) . ? C21 C22 1.453(3) . ? C1 C2 1.337(3) . ? C1 C12 1.519(3) . ? C1 C16 1.495(3) . ? C5 C14 1.545(3) . ? C5 C6 1.564(3) . ? C5 C19 1.526(3) . ? C5 C4 1.554(3) . ? C22 C23 1.380(3) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C6 C7 1.529(3) . ? C6 C11 1.554(3) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C2 C3 1.513(3) . ? C2 C13 1.483(3) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C8 C7 1.528(3) . ? C8 C9 1.539(3) . ? C3 H3 1.0000 . ? C3 C4 1.545(3) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C20 C9 1.526(3) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C10 H10 1.0000 . ? C10 C11 1.538(3) . ? C10 C9 1.546(3) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C38 H38 0.9500 . ? C38 C39 1.391(3) . ? C12 C4 1.569(3) . ? C12 C11 1.565(3) . ? C29 C34 1.386(3) . ? C29 C28 1.502(3) . ? C29 C30 1.394(3) . ? C42 H42 0.9500 . ? C42 C41 1.393(3) . ? C25 H25 0.9500 . ? C25 C24 1.381(3) . ? C13 C18 1.488(3) . ? C13 C17 1.334(3) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C9 H9 1.0000 . ? C24 H24 0.9500 . ? C24 C23 1.403(3) . ? C23 H23 0.9500 . ? C34 H34 0.9500 . ? C34 C33 1.387(3) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C26 B1 1.557(3) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C41 H41 0.9500 . ? C41 C40 1.387(4) . ? C39 H39 0.9500 . ? C39 C40 1.391(4) . ? C40 H40 0.9500 . ? C32 H32 0.9500 . ? C32 C33 1.392(4) . ? C32 C31 1.367(4) . ? C30 H30 0.9500 . ? C30 C31 1.391(4) . ? C33 H33 0.9500 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C31 H31 0.9500 . ? C17 H17A 0.9500 . ? C17 H17B 0.9500 . ? 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 O1 C11 120.47(15) . . ? B1 O8 C4 108.43(16) . . ? C35 O6 C10 114.14(14) . . ? C21 O3 C3 116.42(15) . . ? C27 O7 C6 120.55(15) . . ? B1 O5 C12 107.85(15) . . ? C27 O10 C28 113.36(16) . . ? C35 O9 C36 113.94(15) . . ? C22 N1 H1 125(2) . . ? C25 N1 C22 109.02(18) . . ? C25 N1 H1 126(2) . . ? C38 C37 C36 118.36(19) . . ? C38 C37 C42 118.9(2) . . ? C42 C37 C36 122.74(19) . . ? O1 C15 C14 118.44(17) . . ? O2 C15 O1 118.05(19) . . ? O2 C15 C14 123.40(19) . . ? O3 C21 C22 111.21(17) . . ? O4 C21 O3 123.89(18) . . ? O4 C21 C22 124.90(18) . . ? C2 C1 C12 111.31(17) . . ? C2 C1 C16 126.79(19) . . ? C16 C1 C12 121.85(18) . . ? C14 C5 C6 105.43(15) . . ? C14 C5 C4 111.27(16) . . ? C19 C5 C14 108.83(16) . . ? C19 C5 C6 116.49(16) . . ? C19 C5 C4 112.64(16) . . ? C4 C5 C6 101.86(15) . . ? N1 C22 C21 119.86(18) . . ? N1 C22 C23 108.20(19) . . ? C23 C22 C21 131.89(19) . . ? O6 C35 H35A 109.0 . . ? O6 C35 H35B 109.0 . . ? O9 C35 O6 112.74(16) . . ? O9 C35 H35A 109.0 . . ? O9 C35 H35B 109.0 . . ? H35A C35 H35B 107.8 . . ? O7 C27 H27A 110.2 . . ? O7 C27 H27B 110.2 . . ? O10 C27 O7 107.43(16) . . ? O10 C27 H27A 110.2 . . ? O10 C27 H27B 110.2 . . ? H27A C27 H27B 108.5 . . ? C15 C14 C5 117.24(17) . . ? C15 C14 H14A 108.0 . . ? C15 C14 H14B 108.0 . . ? C5 C14 H14A 108.0 . . ? C5 C14 H14B 108.0 . . ? H14A C14 H14B 107.2 . . ? O7 C6 C5 113.25(15) . . ? O7 C6 C7 110.82(16) . . ? O7 C6 C11 102.15(14) . . ? C7 C6 C5 117.40(16) . . ? C7 C6 C11 111.16(16) . . ? C11 C6 C5 100.47(15) . . ? O9 C36 C37 110.44(17) . . ? O9 C36 H36A 109.6 . . ? O9 C36 H36B 109.6 . . ? C37 C36 H36A 109.6 . . ? C37 C36 H36B 109.6 . . ? H36A C36 H36B 108.1 . . ? C1 C2 C3 112.47(18) . . ? C1 C2 C13 128.21(19) . . ? C13 C2 C3 119.25(17) . . ? H8A C8 H8B 107.8 . . ? C7 C8 H8A 109.0 . . ? C7 C8 H8B 109.0 . . ? C7 C8 C9 112.75(17) . . ? C9 C8 H8A 109.0 . . ? C9 C8 H8B 109.0 . . ? O3 C3 C2 109.54(16) . . ? O3 C3 H3 108.7 . . ? O3 C3 C4 116.82(16) . . ? C2 C3 H3 108.7 . . ? C2 C3 C4 103.98(16) . . ? C4 C3 H3 108.7 . . ? H20A C20 H20B 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C9 C20 H20A 109.5 . . ? C9 C20 H20B 109.5 . . ? C9 C20 H20C 109.5 . . ? C5 C19 H19A 109.5 . . ? C5 C19 H19B 109.5 . . ? C5 C19 H19C 109.5 . . ? H19A C19 H19B 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? O6 C10 H10 108.9 . . ? O6 C10 C11 112.52(16) . . ? O6 C10 C9 108.86(15) . . ? C11 C10 H10 108.9 . . ? C11 C10 C9 108.83(15) . . ? C9 C10 H10 108.9 . . ? C6 C7 H7A 109.6 . . ? C6 C7 H7B 109.6 . . ? C8 C7 C6 110.11(16) . . ? C8 C7 H7A 109.6 . . ? C8 C7 H7B 109.6 . . ? H7A C7 H7B 108.2 . . ? C37 C38 H38 119.5 . . ? C37 C38 C39 121.0(2) . . ? C39 C38 H38 119.5 . . ? O5 C12 C1 113.53(16) . . ? O5 C12 C4 104.90(14) . . ? O5 C12 C11 111.08(15) . . ? C1 C12 C4 104.33(16) . . ? C1 C12 C11 116.51(16) . . ? C11 C12 C4 105.18(15) . . ? C34 C29 C28 120.4(2) . . ? C34 C29 C30 118.7(2) . . ? C30 C29 C28 120.9(2) . . ? C37 C42 H42 119.9 . . ? C41 C42 C37 120.2(2) . . ? C41 C42 H42 119.9 . . ? O8 C4 C5 111.55(15) . . ? O8 C4 C3 108.85(15) . . ? O8 C4 C12 104.66(15) . . ? C5 C4 C12 105.31(15) . . ? C3 C4 C5 119.85(16) . . ? C3 C4 C12 105.30(15) . . ? N1 C25 H25 125.9 . . ? N1 C25 C24 108.3(2) . . ? C24 C25 H25 125.9 . . ? C2 C13 C18 117.23(19) . . ? C17 C13 C2 120.0(2) . . ? C17 C13 C18 122.7(2) . . ? O1 C11 C6 110.00(15) . . ? O1 C11 C10 105.15(15) . . ? O1 C11 C12 106.79(15) . . ? C6 C11 C12 103.80(15) . . ? C10 C11 C6 109.15(16) . . ? C10 C11 C12 121.70(16) . . ? C1 C16 H16A 109.5 . . ? C1 C16 H16B 109.5 . . ? C1 C16 H16C 109.5 . . ? H16A C16 H16B 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C8 C9 C10 110.72(16) . . ? C8 C9 H9 108.0 . . ? C20 C9 C8 110.27(17) . . ? C20 C9 C10 111.76(17) . . ? C20 C9 H9 108.0 . . ? C10 C9 H9 108.0 . . ? C25 C24 H24 126.2 . . ? C25 C24 C23 107.6(2) . . ? C23 C24 H24 126.2 . . ? C22 C23 C24 106.9(2) . . ? C22 C23 H23 126.5 . . ? C24 C23 H23 126.5 . . ? C29 C34 H34 119.6 . . ? C29 C34 C33 120.9(2) . . ? C33 C34 H34 119.6 . . ? H26A C26 H26B 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? B1 C26 H26A 109.5 . . ? B1 C26 H26B 109.5 . . ? B1 C26 H26C 109.5 . . ? O10 C28 C29 109.64(18) . . ? O10 C28 H28A 109.7 . . ? O10 C28 H28B 109.7 . . ? C29 C28 H28A 109.7 . . ? C29 C28 H28B 109.7 . . ? H28A C28 H28B 108.2 . . ? C42 C41 H41 119.8 . . ? C40 C41 C42 120.5(2) . . ? C40 C41 H41 119.8 . . ? C38 C39 H39 120.1 . . ? C38 C39 C40 119.8(2) . . ? C40 C39 H39 120.1 . . ? C41 C40 C39 119.6(2) . . ? C41 C40 H40 120.2 . . ? C39 C40 H40 120.2 . . ? C33 C32 H32 120.3 . . ? C31 C32 H32 120.3 . . ? C31 C32 C33 119.4(2) . . ? C29 C30 H30 120.0 . . ? C31 C30 C29 120.1(2) . . ? C31 C30 H30 120.0 . . ? C34 C33 C32 120.0(2) . . ? C34 C33 H33 120.0 . . ? C32 C33 H33 120.0 . . ? C13 C18 H18A 109.5 . . ? C13 C18 H18B 109.5 . . ? C13 C18 H18C 109.5 . . ? H18A C18 H18B 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C32 C31 C30 121.0(2) . . ? C32 C31 H31 119.5 . . ? C30 C31 H31 119.5 . . ? O8 B1 O5 113.65(18) . . ? O8 B1 C26 123.21(19) . . ? O5 B1 C26 123.12(19) . . ? C13 C17 H17A 120.0 . . ? C13 C17 H17B 120.0 . . ? H17A C17 H17B 120.0 . . ? 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 C15 C14 C5 13.3(3) . . . . ? O6 C10 C11 O1 63.33(19) . . . . ? O6 C10 C11 C6 -178.69(15) . . . . ? O6 C10 C11 C12 -57.9(2) . . . . ? O6 C10 C9 C8 178.83(16) . . . . ? O6 C10 C9 C20 55.5(2) . . . . ? O3 C21 C22 N1 174.79(18) . . . . ? O3 C21 C22 C23 -8.2(3) . . . . ? O3 C3 C4 O8 -111.77(17) . . . . ? O3 C3 C4 C5 18.3(2) . . . . ? O3 C3 C4 C12 136.47(16) . . . . ? O7 C6 C7 C8 -56.9(2) . . . . ? O7 C6 C11 O1 172.58(14) . . . . ? O7 C6 C11 C10 57.69(18) . . . . ? O7 C6 C11 C12 -73.47(17) . . . . ? O5 C12 C4 O8 -6.63(19) . . . . ? O5 C12 C4 C5 -124.35(16) . . . . ? O5 C12 C4 C3 108.07(16) . . . . ? O5 C12 C11 O1 -153.39(14) . . . . ? O5 C12 C11 C6 90.38(17) . . . . ? O5 C12 C11 C10 -32.9(2) . . . . ? O2 C15 C14 C5 -170.78(19) . . . . ? O4 C21 C22 N1 -5.1(3) . . . . ? O4 C21 C22 C23 171.9(2) . . . . ? N1 C22 C23 C24 0.1(3) . . . . ? N1 C25 C24 C23 0.3(3) . . . . ? C37 C38 C39 C40 -0.2(4) . . . . ? C37 C42 C41 C40 -0.6(3) . . . . ? C15 O1 C11 C6 43.1(2) . . . . ? C15 O1 C11 C10 160.51(16) . . . . ? C15 O1 C11 C12 -68.9(2) . . . . ? C21 O3 C3 C2 -152.69(16) . . . . ? C21 O3 C3 C4 89.5(2) . . . . ? C21 C22 C23 C24 -177.2(2) . . . . ? C1 C2 C3 O3 -140.85(17) . . . . ? C1 C2 C3 C4 -15.3(2) . . . . ? C1 C2 C13 C18 -127.7(2) . . . . ? C1 C2 C13 C17 55.7(3) . . . . ? C1 C12 C4 O8 -126.25(16) . . . . ? C1 C12 C4 C5 116.02(16) . . . . ? C1 C12 C4 C3 -11.55(19) . . . . ? C1 C12 C11 O1 -21.3(2) . . . . ? C1 C12 C11 C6 -137.54(17) . . . . ? C1 C12 C11 C10 99.2(2) . . . . ? C5 C6 C7 C8 170.86(16) . . . . ? C5 C6 C11 O1 -70.65(18) . . . . ? C5 C6 C11 C10 174.45(15) . . . . ? C5 C6 C11 C12 43.30(17) . . . . ? C22 N1 C25 C24 -0.3(3) . . . . ? C35 O6 C10 C11 103.96(18) . . . . ? C35 O6 C10 C9 -135.33(16) . . . . ? C35 O9 C36 C37 -163.82(16) . . . . ? C27 O7 C6 C5 80.9(2) . . . . ? C27 O7 C6 C7 -53.5(2) . . . . ? C27 O7 C6 C11 -171.96(16) . . . . ? C27 O10 C28 C29 177.42(18) . . . . ? C14 C5 C6 O7 176.94(15) . . . . ? C14 C5 C6 C7 -51.9(2) . . . . ? C14 C5 C6 C11 68.74(17) . . . . ? C14 C5 C4 O8 168.92(16) . . . . ? C14 C5 C4 C3 40.1(2) . . . . ? C14 C5 C4 C12 -78.12(19) . . . . ? C6 O7 C27 O10 168.28(15) . . . . ? C6 C5 C14 C15 -43.6(2) . . . . ? C6 C5 C4 O8 -79.15(18) . . . . ? C6 C5 C4 C3 152.01(16) . . . . ? C6 C5 C4 C12 33.82(18) . . . . ? C36 O9 C35 O6 82.1(2) . . . . ? C36 C37 C38 C39 -179.9(2) . . . . ? C36 C37 C42 C41 -179.7(2) . . . . ? C2 C1 C12 O5 -111.08(19) . . . . ? C2 C1 C12 C4 2.5(2) . . . . ? C2 C1 C12 C11 117.98(19) . . . . ? C2 C3 C4 O8 127.42(16) . . . . ? C2 C3 C4 C5 -102.53(18) . . . . ? C2 C3 C4 C12 15.66(19) . . . . ? C3 O3 C21 O4 -5.0(3) . . . . ? C3 O3 C21 C22 175.14(16) . . . . ? C3 C2 C13 C18 49.1(3) . . . . ? C3 C2 C13 C17 -127.5(2) . . . . ? C19 C5 C14 C15 -169.29(17) . . . . ? C19 C5 C6 O7 -62.3(2) . . . . ? C19 C5 C6 C7 68.9(2) . . . . ? C19 C5 C6 C11 -170.49(16) . . . . ? C19 C5 C4 O8 46.4(2) . . . . ? C19 C5 C4 C3 -82.4(2) . . . . ? C19 C5 C4 C12 159.36(16) . . . . ? C10 O6 C35 O9 60.4(2) . . . . ? C7 C6 C11 O1 54.3(2) . . . . ? C7 C6 C11 C10 -60.6(2) . . . . ? C7 C6 C11 C12 168.28(16) . . . . ? C7 C8 C9 C20 179.55(17) . . . . ? C7 C8 C9 C10 55.3(2) . . . . ? C38 C37 C36 O9 -175.55(18) . . . . ? C38 C37 C42 C41 0.6(3) . . . . ? C38 C39 C40 C41 0.2(4) . . . . ? C12 O5 B1 O8 -5.1(2) . . . . ? C12 O5 B1 C26 176.15(19) . . . . ? C12 C1 C2 C3 8.1(2) . . . . ? C12 C1 C2 C13 -174.9(2) . . . . ? C29 C34 C33 C32 1.6(4) . . . . ? C29 C30 C31 C32 0.8(4) . . . . ? C42 C37 C36 O9 4.8(3) . . . . ? C42 C37 C38 C39 -0.2(3) . . . . ? C42 C41 C40 C39 0.2(4) . . . . ? C4 O8 B1 O5 0.5(2) . . . . ? C4 O8 B1 C26 179.27(19) . . . . ? C4 C5 C14 C15 66.0(2) . . . . ? C4 C5 C6 O7 60.68(19) . . . . ? C4 C5 C6 C7 -168.14(16) . . . . ? C4 C5 C6 C11 -47.52(17) . . . . ? C4 C12 C11 O1 93.65(17) . . . . ? C4 C12 C11 C6 -22.58(19) . . . . ? C4 C12 C11 C10 -145.87(17) . . . . ? C25 N1 C22 C21 177.74(19) . . . . ? C25 N1 C22 C23 0.1(3) . . . . ? C25 C24 C23 C22 -0.2(3) . . . . ? C13 C2 C3 O3 41.9(2) . . . . ? C13 C2 C3 C4 167.43(18) . . . . ? C11 O1 C15 O2 171.60(17) . . . . ? C11 O1 C15 C14 -12.3(3) . . . . ? C11 C6 C7 C8 56.0(2) . . . . ? C11 C10 C9 C8 -58.2(2) . . . . ? C11 C10 C9 C20 178.44(16) . . . . ? C11 C12 C4 O8 110.62(16) . . . . ? C11 C12 C4 C5 -7.11(19) . . . . ? C11 C12 C4 C3 -134.69(16) . . . . ? C16 C1 C2 C3 -169.32(19) . . . . ? C16 C1 C2 C13 7.7(3) . . . . ? C16 C1 C12 O5 66.5(2) . . . . ? C16 C1 C12 C4 -179.89(17) . . . . ? C16 C1 C12 C11 -64.5(2) . . . . ? C9 C8 C7 C6 -53.6(2) . . . . ? C9 C10 C11 O1 -57.41(19) . . . . ? C9 C10 C11 C6 60.57(19) . . . . ? C9 C10 C11 C12 -178.68(16) . . . . ? C34 C29 C28 O10 -54.3(3) . . . . ? C34 C29 C30 C31 -1.3(3) . . . . ? C28 O10 C27 O7 -78.2(2) . . . . ? C28 C29 C34 C33 -177.2(2) . . . . ? C28 C29 C30 C31 176.0(2) . . . . ? C30 C29 C34 C33 0.1(3) . . . . ? C30 C29 C28 O10 128.5(2) . . . . ? C33 C32 C31 C30 0.9(4) . . . . ? C31 C32 C33 C34 -2.2(4) . . . . ? B1 O8 C4 C5 117.18(17) . . . . ? B1 O8 C4 C3 -108.37(18) . . . . ? B1 O8 C4 C12 3.8(2) . . . . ? B1 O5 C12 C1 120.28(18) . . . . ? B1 O5 C12 C4 7.00(19) . . . . ? B1 O5 C12 C11 -106.14(18) . . . . ? _shelx_res_file ; p16282_a.res created by SHELXL-2014/7 TITL p16282_a.res in P2(1) REM Old TITL P16282 in P2(1) REM SHELXT solution in P2(1) REM R1 0.074, Rweak 0.035, Alpha 0.001, Orientation as input REM Flack x = 0.102 ( 0.052 ) from Parsons' quotients REM Formula found by SHELXT: C43 N O9 CELL 1.54178 8.7826 22.1496 10.3099 90 109.928 90 ZERR 2 0.0004 0.001 0.0005 0 0.002 0 LATT -1 SYMM -X,0.5+Y,-Z SFAC C H B N O UNIT 84 96 2 2 20 L.S. 20 PLAN 20 SIZE 0.087 0.251 0.361 TEMP -173.15 BOND $H LIST 6 MORE -1 CONF fmap 2 acta REM REM REM WGHT 0.036100 0.254200 EXTI 0.000715 FVAR 0.78989 O1 5 0.426876 0.427186 0.512201 11.00000 0.01456 0.01694 = 0.01372 0.00186 0.00623 -0.00122 O8 5 0.392974 0.463707 0.083686 11.00000 0.01429 0.01682 = 0.01123 0.00228 0.00549 0.00008 O6 5 0.768576 0.446901 0.600863 11.00000 0.01119 0.01833 = 0.01279 0.00243 0.00314 0.00028 O3 5 0.102992 0.361036 0.095713 11.00000 0.01241 0.01879 = 0.01269 0.00155 0.00249 -0.00133 O7 5 0.474019 0.547992 0.289148 11.00000 0.01375 0.01457 = 0.01510 0.00255 0.00610 0.00075 O5 5 0.629979 0.438263 0.257449 11.00000 0.01152 0.01972 = 0.01387 -0.00129 0.00547 0.00036 O10 5 0.545797 0.632210 0.198316 11.00000 0.01712 0.02051 = 0.01499 0.00137 0.00373 -0.00420 O9 5 0.989345 0.495564 0.564754 11.00000 0.01422 0.01979 = 0.01441 0.00104 0.00292 -0.00379 O2 5 0.221403 0.375617 0.530403 11.00000 0.01926 0.02337 = 0.02149 0.00417 0.00906 -0.00264 O4 5 0.055818 0.398422 -0.118789 11.00000 0.01720 0.02337 = 0.01621 0.00429 0.00406 -0.00213 N1 4 -0.278791 0.374277 -0.179454 11.00000 0.01585 0.02053 = 0.01490 0.00128 0.00317 -0.00068 C37 1 1.158150 0.570356 0.716226 11.00000 0.01481 0.02134 = 0.01514 0.00029 0.00829 -0.00087 C15 1 0.269046 0.410546 0.462973 11.00000 0.01551 0.01727 = 0.01607 -0.00172 0.00784 -0.00007 C21 1 0.007050 0.375179 -0.033902 11.00000 0.01479 0.01346 = 0.01229 0.00028 0.00255 0.00094 C1 1 0.499087 0.352898 0.332143 11.00000 0.01589 0.01544 = 0.01285 0.00007 0.00524 0.00293 C5 1 0.241965 0.475453 0.245164 11.00000 0.01321 0.01513 = 0.01282 -0.00077 0.00568 -0.00036 C22 1 -0.160536 0.359015 -0.057269 11.00000 0.01680 0.01751 = 0.01420 0.00089 0.00347 0.00084 C35 1 0.901650 0.441579 0.552139 11.00000 0.01203 0.01861 = 0.01604 -0.00005 0.00498 0.00008 AFIX 23 H35A 2 0.975257 0.409457 0.604866 11.00000 -1.20000 H35B 2 0.860575 0.429280 0.453956 11.00000 -1.20000 AFIX 0 C27 1 0.416641 0.604165 0.223350 11.00000 0.01444 0.01940 = 0.01438 0.00401 0.00326 0.00039 AFIX 23 H27A 2 0.326560 0.597382 0.135520 11.00000 -1.20000 H27B 2 0.376696 0.629805 0.283606 11.00000 -1.20000 AFIX 0 C14 1 0.159844 0.439592 0.331779 11.00000 0.01230 0.01898 = 0.01636 -0.00074 0.00659 -0.00132 AFIX 23 H14A 2 0.085269 0.467239 0.356234 11.00000 -1.20000 H14B 2 0.092907 0.407471 0.272533 11.00000 -1.20000 AFIX 0 C6 1 0.377707 0.513524 0.351600 11.00000 0.01090 0.01604 = 0.01253 0.00097 0.00478 -0.00039 C36 1 1.104801 0.505426 0.699215 11.00000 0.01418 0.02200 = 0.01404 0.00006 0.00196 -0.00210 AFIX 23 H36A 2 1.199931 0.478981 0.713094 11.00000 -1.20000 H36B 2 1.055907 0.494925 0.769745 11.00000 -1.20000 AFIX 0 C2 1 0.368217 0.327302 0.241080 11.00000 0.01550 0.01609 = 0.01258 0.00001 0.00367 0.00317 C8 1 0.479553 0.577923 0.563597 11.00000 0.01813 0.01716 = 0.01544 -0.00282 0.00726 -0.00025 AFIX 23 H8A 2 0.446501 0.599705 0.633562 11.00000 -1.20000 H8B 2 0.531627 0.607427 0.519863 11.00000 -1.20000 AFIX 0 C3 1 0.275091 0.370462 0.128130 11.00000 0.01151 0.01601 = 0.01274 0.00090 0.00282 0.00073 AFIX 13 H3 2 0.303350 0.361980 0.043795 11.00000 -1.20000 AFIX 0 C20 1 0.751347 0.557289 0.743187 11.00000 0.02098 0.02116 = 0.01482 -0.00451 0.00548 -0.00227 AFIX 137 H20A 2 0.808133 0.582852 0.696817 11.00000 -1.50000 H20B 2 0.824338 0.525380 0.794689 11.00000 -1.50000 H20C 2 0.716545 0.581890 0.807009 11.00000 -1.50000 AFIX 0 C19 1 0.112540 0.510710 0.133874 11.00000 0.01266 0.01800 = 0.01886 -0.00089 0.00377 0.00020 AFIX 137 H19A 2 0.021582 0.483912 0.087104 11.00000 -1.50000 H19B 2 0.158733 0.526553 0.066613 11.00000 -1.50000 H19C 2 0.074201 0.544303 0.176446 11.00000 -1.50000 AFIX 0 C10 1 0.650661 0.491178 0.529071 11.00000 0.01209 0.01430 = 0.01093 0.00015 0.00223 0.00066 AFIX 13 H10 2 0.699898 0.518581 0.477132 11.00000 -1.20000 AFIX 0 C7 1 0.328861 0.552231 0.453790 11.00000 0.01580 0.01690 = 0.01523 -0.00042 0.00762 0.00178 AFIX 23 H7A 2 0.258296 0.585702 0.404041 11.00000 -1.20000 H7B 2 0.267046 0.527388 0.498462 11.00000 -1.20000 AFIX 0 C38 1 1.279187 0.587270 0.837731 11.00000 0.02177 0.02637 = 0.01388 0.00303 0.00540 -0.00313 AFIX 43 H38 2 1.325595 0.557827 0.906956 11.00000 -1.20000 AFIX 0 C12 1 0.503270 0.420362 0.307378 11.00000 0.01090 0.01726 = 0.01101 0.00066 0.00388 0.00135 C29 1 0.796065 0.686673 0.282860 11.00000 0.02010 0.01970 = 0.01646 0.00199 0.00089 -0.00341 C42 1 1.090686 0.614112 0.615572 11.00000 0.01588 0.02367 = 0.01651 0.00126 0.00468 0.00134 AFIX 43 H42 2 1.007137 0.603332 0.532346 11.00000 -1.20000 AFIX 0 C4 1 0.342212 0.433232 0.184650 11.00000 0.01182 0.01605 = 0.01081 0.00105 0.00443 -0.00006 C25 1 -0.423055 0.352603 -0.179192 11.00000 0.01473 0.03152 = 0.02213 0.00445 0.00168 -0.00028 AFIX 43 H25 2 -0.524197 0.357121 -0.251400 11.00000 -1.20000 AFIX 0 C13 1 0.312894 0.263804 0.236358 11.00000 0.01872 0.01678 = 0.02015 0.00085 -0.00074 0.00166 C11 1 0.496741 0.462600 0.427032 11.00000 0.01274 0.01519 = 0.01035 0.00119 0.00504 -0.00035 C16 1 0.632210 0.321527 0.442410 11.00000 0.01931 0.01880 = 0.01685 -0.00151 -0.00126 0.00389 AFIX 137 H16A 2 0.632779 0.334928 0.533164 11.00000 -1.50000 H16B 2 0.736439 0.331297 0.432335 11.00000 -1.50000 H16C 2 0.614655 0.277796 0.433996 11.00000 -1.50000 AFIX 0 C9 1 0.603466 0.528866 0.635821 11.00000 0.01765 0.01769 = 0.01194 -0.00186 0.00560 -0.00296 AFIX 13 H9 2 0.551436 0.501151 0.684950 11.00000 -1.20000 AFIX 0 C24 1 -0.397696 0.322832 -0.055925 11.00000 0.01818 0.04324 = 0.03124 0.01222 0.00805 -0.00513 AFIX 43 H24 2 -0.477861 0.303130 -0.028435 11.00000 -1.20000 AFIX 0 C23 1 -0.232052 0.326948 0.021401 11.00000 0.01880 0.03446 = 0.01986 0.00946 0.00622 -0.00030 AFIX 43 H23 2 -0.179243 0.310749 0.110834 11.00000 -1.20000 AFIX 0 C34 1 0.884572 0.651139 0.223534 11.00000 0.02269 0.01614 = 0.03457 0.00393 0.00801 -0.00003 AFIX 43 H34 2 0.854079 0.610258 0.201259 11.00000 -1.20000 AFIX 0 C26 1 0.658314 0.494855 0.047349 11.00000 0.01770 0.02730 = 0.02004 0.00148 0.00714 -0.00115 AFIX 137 H26A 2 0.630072 0.475324 -0.043089 11.00000 -1.50000 H26B 2 0.774250 0.489562 0.097900 11.00000 -1.50000 H26C 2 0.633169 0.538029 0.034883 11.00000 -1.50000 AFIX 0 C28 1 0.657483 0.660179 0.317908 11.00000 0.02403 0.02787 = 0.01856 -0.00484 0.00672 -0.00621 AFIX 23 H28A 2 0.698828 0.629914 0.392335 11.00000 -1.20000 H28B 2 0.601935 0.692393 0.351296 11.00000 -1.20000 AFIX 0 C41 1 1.145480 0.673533 0.636773 11.00000 0.02451 0.02198 = 0.02331 0.00501 0.00902 0.00266 AFIX 43 H41 2 1.099743 0.703013 0.567478 11.00000 -1.20000 AFIX 0 C39 1 1.333358 0.646648 0.859470 11.00000 0.03030 0.02917 = 0.01686 -0.00293 0.00521 -0.01024 AFIX 43 H39 2 1.415905 0.657612 0.943150 11.00000 -1.20000 AFIX 0 C40 1 1.266326 0.689955 0.758326 11.00000 0.03369 0.01860 = 0.02583 -0.00415 0.01270 -0.00378 AFIX 43 H40 2 1.303152 0.730557 0.772465 11.00000 -1.20000 AFIX 0 C32 1 1.065143 0.733876 0.231788 11.00000 0.02046 0.03075 = 0.03198 0.00956 0.00109 -0.00793 AFIX 43 H32 2 1.158006 0.749663 0.216215 11.00000 -1.20000 AFIX 0 C30 1 0.842723 0.746569 0.314576 11.00000 0.03695 0.02160 = 0.01751 -0.00182 0.00606 -0.00358 AFIX 43 H30 2 0.782341 0.771906 0.353518 11.00000 -1.20000 AFIX 0 C33 1 1.017047 0.674502 0.196284 11.00000 0.02044 0.02617 = 0.03924 0.00733 0.00968 0.00422 AFIX 43 H33 2 1.074948 0.649980 0.153389 11.00000 -1.20000 AFIX 0 C18 1 0.278533 0.230803 0.103756 11.00000 0.03478 0.01936 = 0.02446 -0.00162 0.00243 0.00017 AFIX 137 H18A 2 0.197157 0.252973 0.029932 11.00000 -1.50000 H18B 2 0.237462 0.190382 0.112137 11.00000 -1.50000 H18C 2 0.378344 0.227315 0.081847 11.00000 -1.50000 AFIX 0 C31 1 0.977579 0.769269 0.289263 11.00000 0.03953 0.02249 = 0.02335 -0.00015 0.00356 -0.01288 AFIX 43 H31 2 1.009305 0.809993 0.312273 11.00000 -1.20000 AFIX 0 B1 3 0.558956 0.465709 0.130508 11.00000 0.01505 0.01737 = 0.01348 -0.00384 0.00517 -0.00004 C17 1 0.288094 0.239598 0.345920 11.00000 0.04840 0.01993 = 0.02919 0.00192 0.01347 -0.00699 AFIX 93 H17A 2 0.305859 0.263020 0.426948 11.00000 -1.20000 H17B 2 0.252663 0.198934 0.342937 11.00000 -1.20000 AFIX 0 H1 2 -0.262542 0.394692 -0.247392 11.00000 -1.20000 HKLF 4 REM p16282_a.res in P2(1) REM R1 = 0.0311 for 7609 Fo > 4sig(Fo) and 0.0338 for all 7996 data REM 496 parameters refined using 1 restraints END WGHT 0.0361 0.2542 REM Highest difference peak 0.196, deepest hole -0.192, 1-sigma level 0.038 Q1 1 0.5116 0.4411 0.3659 11.00000 0.05 0.20 Q2 1 0.5767 0.4779 0.4773 11.00000 0.05 0.20 Q3 1 0.4078 0.3392 0.3262 11.00000 0.05 0.19 Q4 1 0.4203 0.4296 0.2484 11.00000 0.05 0.19 Q5 1 0.2923 0.4564 0.2166 11.00000 0.05 0.18 Q6 1 0.1975 0.4574 0.2874 11.00000 0.05 0.18 Q7 1 0.6170 0.5086 0.5770 11.00000 0.05 0.18 Q8 1 0.1725 0.4973 0.1981 11.00000 0.05 0.18 Q9 1 0.3028 0.4976 0.2904 11.00000 0.05 0.17 Q10 1 0.6138 0.4865 0.1011 11.00000 0.05 0.17 Q11 1 0.3405 0.5336 0.3889 11.00000 0.05 0.17 Q12 1 0.6820 0.5400 0.6939 11.00000 0.05 0.16 Q13 1 1.0039 0.7498 0.2340 11.00000 0.05 0.16 Q14 1 0.5901 0.5115 -0.0490 11.00000 0.05 0.15 Q15 1 0.4338 0.4872 0.4014 11.00000 0.05 0.15 Q16 1 -0.4470 0.3568 -0.1001 11.00000 0.05 0.15 Q17 1 0.7298 0.6759 0.2983 11.00000 0.05 0.15 Q18 1 -0.5274 0.3717 -0.2820 11.00000 0.05 0.15 Q19 1 0.3164 0.3465 0.1858 11.00000 0.05 0.15 Q20 1 1.1612 0.6710 0.9013 11.00000 0.05 0.14 ; _shelx_res_checksum 74179 _shelx_hkl_file ; 1 0 0 2329.67 85.79 1 0 0 2270.07 84.99 -1 0 0 2361.76 85.69 -1 0 0 2344.37 84.99 2 0 0 180.18 12.00 2 0 0 195.48 10.80 -2 0 0 192.58 11.80 -2 0 0 195.18 10.40 -3 0 0 507.85 23.00 -3 0 0 493.15 25.20 3 0 0 466.85 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4 60.59 8.40 -3 10 -4 59.99 5.80 4 -10 4 47.20 7.60 4 -10 4 40.10 8.10 4 -10 4 44.70 8.30 4 -10 4 37.90 8.60 4 -10 4 49.10 7.60 4 -10 4 32.20 5.90 -4 10 -4 45.70 5.80 4 10 4 50.29 10.40 4 10 4 44.60 8.40 4 10 4 51.79 7.40 5 -10 4 13.40 4.50 5 -10 4 32.10 6.90 5 -10 4 18.50 5.40 5 -10 4 21.10 6.30 5 -10 4 26.10 7.90 5 -10 4 3.80 8.60 5 10 4 6.90 8.10 5 10 4 26.00 5.90 -5 10 -4 23.40 3.70 5 10 4 21.30 4.40 6 -10 4 40.50 7.50 6 10 4 47.10 11.10 6 10 4 58.49 8.70 -6 10 -4 60.39 5.80 7 -10 4 37.90 5.30 7 -10 4 35.10 5.00 7 -10 4 34.10 5.00 -7 10 -4 27.20 5.20 7 10 4 36.50 8.90 7 10 4 31.30 6.00 8 -10 4 81.59 5.30 8 -10 4 89.39 5.50 8 10 4 85.79 7.10 10 -11 -4 4.80 3.40 -10 -11 4 1.60 2.00 10 11 -4 8.00 4.40 10 11 -4 6.90 4.60 -9 -11 4 11.10 2.90 9 -11 -4 14.30 3.70 -9 -11 4 10.30 5.20 9 11 -4 25.70 7.00 9 11 -4 7.20 5.10 -9 11 4 9.10 3.70 9 11 -4 10.90 3.70 9 11 -4 13.60 5.70 -8 -11 4 123.29 8.40 8 -11 -4 126.09 9.70 8 -11 -4 102.79 12.20 -8 -11 4 112.39 8.20 -8 11 4 109.29 7.00 8 11 -4 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15.20 6 7 5 198.78 11.80 6 7 5 193.18 13.40 7 -7 5 95.79 6.80 7 -7 5 85.09 6.10 7 7 5 91.79 9.00 10 -8 -5 10.70 5.20 -10 -8 5 5.90 2.50 10 8 -5 7.90 4.90 10 8 -5 11.40 5.50 9 -8 -5 10.20 4.50 -9 -8 5 13.80 3.60 9 -8 -5 14.70 3.40 -9 -8 5 12.40 3.10 9 -8 -5 16.90 4.50 9 8 -5 13.40 4.30 9 8 -5 10.90 6.20 9 8 -5 19.00 5.80 8 -8 -5 76.39 9.90 8 -8 -5 86.99 8.30 8 -8 -5 94.99 9.40 -8 -8 5 83.99 7.10 -8 -8 5 82.49 7.50 -8 8 5 74.29 5.60 8 8 -5 63.39 10.30 8 8 -5 67.69 13.10 -8 8 5 77.79 6.30 8 8 -5 93.39 11.20 7 -8 -5 932.51 37.60 7 -8 -5 927.61 37.20 -7 -8 5 935.61 36.30 7 -8 -5 939.91 37.50 7 -8 -5 877.01 37.70 -7 -8 5 937.61 36.70 -7 8 5 924.61 35.10 7 8 -5 892.91 40.70 7 8 -5 912.01 39.20 7 8 -5 925.01 39.00 -7 8 5 933.91 35.20 6 -8 -5 108.99 12.50 6 -8 -5 150.78 14.80 6 -8 -5 97.69 14.20 -6 -8 5 132.79 9.90 6 -8 -5 122.09 8.30 -6 8 5 139.59 7.70 5 -8 -5 24.40 7.40 -5 -8 5 31.40 5.50 -5 -8 5 27.10 4.70 5 -8 -5 21.90 5.60 5 -8 -5 27.80 5.10 5 8 -5 15.70 7.00 5 8 -5 39.40 10.80 5 8 -5 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5.50 8 -9 -5 169.68 11.40 8 -9 -5 193.18 12.40 -8 -9 5 183.58 10.60 -8 -9 5 179.38 10.10 8 -9 -5 192.38 11.00 8 9 -5 187.38 13.60 -8 9 5 170.58 9.50 8 9 -5 187.68 13.20 8 9 -5 189.68 15.80 7 -9 -5 149.19 10.90 7 -9 -5 138.09 13.70 -7 -9 5 149.19 10.00 7 -9 -5 175.18 11.60 7 -9 -5 122.69 12.40 -7 -9 5 154.38 9.80 7 9 -5 145.89 13.50 -7 9 5 164.08 8.20 -7 9 5 159.38 8.60 7 9 -5 164.08 14.40 7 9 -5 174.28 17.80 6 -9 -5 69.09 9.50 6 -9 -5 83.29 8.90 -6 -9 5 72.59 7.70 -6 -9 5 75.69 8.10 6 -9 -5 66.59 9.60 6 9 -5 70.59 11.90 -6 9 5 64.79 6.50 -6 9 5 66.59 6.00 6 9 -5 61.19 11.90 6 9 -5 80.09 15.40 -5 -9 5 491.55 21.20 5 -9 -5 444.86 21.20 -5 -9 5 494.15 20.80 5 -9 -5 475.85 19.30 5 -9 -5 474.45 22.80 5 9 -5 495.05 25.40 5 9 -5 495.35 27.70 5 9 -5 477.65 24.10 -4 -9 5 326.87 25.20 -4 -9 5 408.26 18.10 -4 -9 5 381.76 46.90 -4 -9 5 428.16 18.70 4 -9 -5 429.96 16.30 4 -9 -5 405.26 19.20 4 -9 -5 311.57 26.00 4 9 -5 394.26 21.40 4 9 -5 431.66 25.30 -4 9 5 364.26 20.10 -4 9 5 435.86 68.49 4 9 -5 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7.10 7 -14 -7 46.80 7.10 7 14 -7 46.00 7.30 7 14 -7 45.10 8.60 7 14 -7 42.60 8.50 -7 14 7 55.79 6.90 6 -14 -7 115.49 10.00 6 -14 -7 106.29 6.90 6 -14 -7 113.49 9.80 6 14 -7 133.19 17.30 -6 14 7 116.39 12.20 6 14 -7 131.99 18.90 6 14 -7 99.49 12.60 5 -14 -7 299.37 12.80 -5 -14 7 284.77 19.00 5 -14 -7 287.67 16.20 5 -14 -7 290.17 13.00 5 -14 -7 281.57 14.60 5 14 -7 287.57 17.10 -5 14 7 301.77 14.40 5 14 -7 298.47 21.30 4 -14 -7 135.69 7.90 -4 -14 7 128.89 14.30 4 -14 -7 126.89 7.80 4 -14 -7 133.29 10.20 -4 14 7 142.79 10.50 4 14 -7 139.89 9.40 4 14 -7 159.48 20.20 4 14 -7 104.19 20.40 4 14 -7 143.99 13.10 -4 14 7 140.49 9.60 3 -14 -7 72.89 5.80 -3 -14 7 75.29 10.30 -3 14 7 59.79 7.50 3 14 -7 80.29 7.10 -3 14 7 72.29 8.40 3 14 -7 98.69 16.20 -2 -14 7 133.99 11.70 2 -14 -7 139.09 7.70 -2 -14 7 100.99 14.40 -2 -14 7 130.79 13.80 -2 -14 7 133.39 15.10 -2 14 7 119.99 10.40 -2 14 7 157.78 10.30 2 14 -7 117.49 26.00 -2 14 7 132.59 11.40 2 14 -7 138.49 8.70 -2 14 7 145.89 11.70 -1 -14 7 182.68 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5.10 8 7 -9 28.10 5.60 8 7 -9 33.90 9.00 7 -7 -9 99.99 13.20 7 -7 -9 104.89 8.70 7 -7 -9 98.89 6.30 7 -7 -9 117.19 8.50 7 7 -9 94.69 9.90 7 7 -9 107.59 10.60 7 7 -9 87.39 12.60 6 -7 -9 45.50 8.20 6 -7 -9 50.49 5.70 -6 7 9 61.39 11.10 6 7 -9 59.09 7.20 6 7 -9 54.09 8.10 6 7 -9 52.29 16.40 5 -7 -9 162.88 8.80 -5 -7 9 173.18 13.50 -5 -7 9 144.39 15.40 5 -7 -9 165.18 11.20 -5 7 9 182.18 10.90 -5 7 9 140.89 12.50 5 7 -9 169.48 13.90 -5 7 9 160.08 12.40 5 7 -9 172.18 9.60 -4 -7 9 409.16 21.00 -4 -7 9 406.96 21.60 4 -7 -9 416.66 19.90 -4 -7 9 383.96 22.30 4 -7 -9 478.45 19.50 -4 7 9 420.26 19.50 4 7 -9 420.86 21.40 -4 7 9 400.66 21.30 -4 7 9 410.76 20.30 -4 7 9 418.16 19.20 4 7 -9 459.25 21.30 -3 -7 9 116.69 17.00 -3 -7 9 121.29 12.60 3 -7 -9 92.69 11.80 -3 -7 9 94.69 13.30 -3 -7 9 110.09 12.80 3 -7 -9 117.89 7.40 3 7 -9 126.59 15.90 -3 7 9 123.79 11.30 -3 7 9 111.89 9.00 -3 7 9 121.49 9.80 3 7 -9 125.99 8.40 2 -7 -9 19.80 3.50 -2 -7 9 8.10 6.00 -2 -7 9 15.60 6.00 -2 -7 9 4.70 7.00 -2 -7 9 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21.00 8.50 6 -12 -9 38.70 4.20 -6 12 9 39.90 5.50 6 12 -9 29.80 5.90 6 12 -9 46.90 10.70 -5 -12 9 34.00 7.70 5 -12 -9 31.80 4.80 -5 -12 9 29.50 6.90 5 -12 -9 38.40 7.00 -5 12 9 41.20 5.80 5 12 -9 23.10 4.40 -5 12 9 30.90 5.20 5 12 -9 33.00 6.00 -4 -12 9 59.39 8.80 4 -12 -9 64.39 5.30 -4 12 9 44.60 8.70 -4 12 9 53.39 8.60 4 12 -9 71.49 10.00 -4 12 9 64.19 9.50 4 12 -9 59.59 6.40 -3 -12 9 44.30 7.10 -3 -12 9 34.90 8.50 3 -12 -9 46.90 4.90 -3 12 9 45.20 8.20 -3 12 9 32.10 7.00 3 12 -9 40.40 5.90 3 12 -9 39.20 7.20 -3 12 9 33.00 6.70 -3 12 9 43.70 7.00 -2 -12 9 18.80 6.40 -2 -12 9 17.20 5.80 -2 -12 9 23.10 6.60 2 -12 -9 17.50 3.10 -2 12 9 8.20 4.40 -2 12 9 10.70 3.90 -2 12 9 25.70 5.00 -2 12 9 17.50 6.40 2 12 -9 12.00 3.50 1 -12 -9 252.17 11.30 -1 -12 9 212.78 17.10 -1 -12 9 226.78 13.80 1 12 -9 248.68 12.20 -1 12 9 253.57 13.00 -1 12 9 247.38 12.90 -1 12 9 287.27 16.60 0 -12 -9 146.59 8.10 0 -12 9 170.18 12.20 0 -12 9 143.09 10.30 0 -12 -9 162.88 9.70 0 -12 9 143.79 10.20 0 -12 9 132.39 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10 111.39 9.70 0 -3 -10 91.99 8.80 0 -3 10 97.99 10.20 0 -3 10 130.49 11.30 0 3 10 117.99 9.40 0 3 10 122.69 9.80 0 3 -10 122.89 8.70 0 3 10 99.29 9.00 1 -3 10 121.79 10.30 1 -3 10 124.19 9.50 1 -3 10 123.39 8.80 1 3 10 110.99 8.30 1 3 10 109.39 8.80 1 3 10 118.39 8.90 1 3 10 117.09 8.30 2 -3 10 76.19 6.60 2 -3 10 72.99 6.70 2 -3 10 74.19 7.70 2 3 10 54.19 6.50 2 3 10 72.99 6.60 2 3 10 57.09 6.10 2 3 10 64.49 5.80 3 -3 10 9.60 3.20 3 -3 10 5.00 2.90 3 3 10 7.30 3.70 3 3 10 11.00 3.20 9 -4 -10 11.40 3.10 9 -4 -10 1.80 6.40 9 4 -10 9.50 5.00 9 4 -10 16.00 4.90 8 -4 -10 9.00 3.30 8 -4 -10 15.60 6.70 8 4 -10 6.30 3.90 8 4 -10 6.20 5.00 8 4 -10 14.80 9.90 -8 4 10 4.00 9.80 7 -4 -10 86.89 7.70 7 4 -10 87.99 9.80 -7 4 10 91.19 9.10 7 4 -10 90.39 8.90 6 -4 -10 -2.40 7.40 6 -4 -10 2.10 2.90 6 4 -10 12.70 6.30 6 4 -10 6.80 3.50 -6 4 10 12.40 5.30 5 -4 -10 145.19 10.50 5 -4 -10 149.79 8.20 -5 -4 10 163.98 21.70 5 4 -10 135.79 14.50 -5 4 10 151.98 10.20 5 4 -10 146.29 8.80 -5 4 10 154.18 11.30 -4 -4 10 336.87 16.60 4 -4 -10 336.97 16.50 -4 -4 10 313.87 18.80 4 -4 -10 335.17 14.60 -4 4 10 342.07 16.40 -4 4 10 328.37 15.90 -4 4 10 341.47 17.00 -4 4 10 308.37 17.50 4 4 -10 337.47 15.10 4 4 -10 338.57 19.70 -3 -4 10 80.09 10.10 -3 -4 10 72.89 8.80 -3 -4 10 59.69 9.80 3 -4 -10 68.29 6.10 -3 -4 10 55.29 10.00 -3 -4 10 61.99 10.70 3 4 -10 66.29 6.50 -3 4 10 67.99 8.90 3 4 -10 68.49 10.00 -3 4 10 68.69 7.60 -3 4 10 64.39 7.90 -3 4 10 68.79 9.60 -2 -4 10 22.30 6.00 2 -4 -10 11.40 3.40 -2 -4 10 21.20 6.30 -2 -4 10 16.10 6.00 -2 -4 10 19.10 5.90 -2 -4 10 8.20 4.40 -2 4 10 18.40 4.50 2 4 -10 4.90 3.60 -2 4 10 8.00 4.30 -2 4 10 9.40 5.20 -2 4 10 16.70 4.90 -1 -4 10 133.39 10.70 -1 -4 10 113.89 11.30 -1 -4 10 123.69 11.90 1 -4 -10 123.69 8.10 -1 -4 10 122.19 10.00 -1 4 10 131.19 10.40 1 4 -10 127.49 8.70 -1 4 10 133.29 10.00 -1 4 10 125.79 9.30 -1 4 10 128.69 9.40 0 -4 -10 107.89 8.80 0 -4 10 117.79 10.70 0 -4 10 145.49 15.20 0 -4 10 115.29 10.10 0 -4 10 125.59 10.50 0 4 -10 115.79 8.80 0 4 10 109.79 9.20 0 4 10 113.19 11.50 0 4 10 133.09 9.50 1 -4 10 97.89 8.60 1 -4 10 115.49 9.80 1 -4 10 104.79 8.30 1 4 10 90.79 7.40 1 4 10 99.79 8.30 1 4 10 94.19 7.90 1 4 10 99.29 8.20 2 -4 10 102.99 7.60 2 -4 10 119.19 7.50 2 -4 10 118.39 8.90 2 4 10 96.69 7.20 2 4 10 107.89 7.40 2 4 10 87.69 7.30 2 4 10 91.89 6.60 3 -4 10 35.00 4.80 3 -4 10 33.20 5.10 3 4 10 33.50 5.10 3 4 10 25.80 5.60 9 -5 -10 129.39 7.30 9 5 -10 134.59 9.70 9 5 -10 124.39 9.20 8 -5 -10 37.20 5.30 8 -5 -10 36.50 6.80 8 5 -10 29.60 7.30 7 -5 -10 235.48 11.80 7 5 -10 224.88 12.60 7 5 -10 255.87 14.00 -7 5 10 225.18 13.00 6 -5 -10 52.79 7.50 6 -5 -10 50.49 5.40 -6 5 10 45.20 8.10 6 5 -10 44.10 7.10 6 5 -10 35.00 6.20 5 -5 -10 60.99 5.50 -5 -5 10 54.39 10.00 -5 5 10 68.29 7.90 5 5 -10 54.99 11.90 -5 5 10 55.39 8.90 5 5 -10 56.59 6.00 -4 -5 10 81.29 10.10 -4 -5 10 72.49 11.60 4 -5 -10 84.19 6.20 4 -5 -10 80.29 9.40 -4 -5 10 97.69 9.60 -4 5 10 79.79 8.50 4 5 -10 76.49 12.90 4 5 -10 84.39 7.00 -4 5 10 83.99 8.00 -4 5 10 66.59 10.30 -4 5 10 81.49 9.10 3 -5 -10 180.78 9.80 -3 -5 10 177.78 13.40 -3 -5 10 210.58 13.70 -3 -5 10 205.68 12.40 -3 -5 10 197.08 14.50 -3 -5 10 180.08 12.70 3 -5 -10 191.38 12.80 3 5 -10 195.18 10.60 -3 5 10 209.48 11.70 -3 5 10 194.98 12.60 -3 5 10 176.98 10.90 -3 5 10 194.58 12.30 3 5 -10 172.18 16.40 -2 -5 10 474.65 22.10 2 -5 -10 443.46 19.00 -2 -5 10 495.55 22.40 -2 -5 10 444.46 21.80 -2 -5 10 430.86 22.80 2 -5 -10 440.96 23.80 -2 -5 10 487.45 21.10 2 5 -10 465.25 19.70 2 5 -10 439.66 24.60 -2 5 10 479.05 21.80 -2 5 10 453.65 21.30 -2 5 10 473.35 20.70 -2 5 10 461.25 20.20 -1 -5 10 50.99 9.50 -1 -5 10 37.60 10.10 -1 -5 10 42.10 8.40 1 -5 -10 42.60 6.00 -1 5 10 47.40 7.50 -1 5 10 51.69 7.70 1 5 -10 53.29 6.50 -1 5 10 34.50 6.50 -1 5 10 49.80 6.90 0 -5 10 42.60 8.10 0 -5 -10 46.40 7.10 0 -5 10 54.79 10.10 0 5 10 48.30 6.90 0 5 10 52.09 9.40 1 -5 10 24.10 4.70 1 -5 10 18.90 4.40 1 -5 10 36.00 7.70 1 5 10 26.90 5.80 1 5 10 27.80 5.30 1 5 10 18.10 3.90 -1 5 -10 17.10 5.20 1 5 10 18.20 4.00 2 -5 10 22.20 4.10 2 -5 10 16.10 3.50 2 -5 10 25.70 6.60 2 5 10 19.60 5.80 2 5 10 19.70 3.50 2 5 10 11.70 3.30 3 -5 10 33.30 5.00 3 -5 10 22.40 4.50 3 5 10 25.90 3.80 9 -6 -10 74.69 5.50 9 6 -10 69.49 7.30 -9 6 10 69.39 5.10 8 -6 -10 71.59 6.20 8 -6 -10 97.09 11.40 8 6 -10 76.29 10.00 8 6 -10 78.69 8.30 8 6 -10 83.79 8.50 7 -6 -10 67.69 6.50 7 6 -10 47.50 7.50 7 6 -10 69.79 8.40 -7 6 10 60.99 8.80 6 -6 -10 78.29 6.50 6 -6 -10 91.79 8.10 6 6 -10 102.99 11.60 6 6 -10 74.59 7.30 -6 6 10 102.19 9.80 5 -6 -10 138.09 14.20 5 -6 -10 155.28 8.40 -5 -6 10 149.49 16.90 -5 6 10 179.38 14.00 -5 6 10 167.58 10.30 5 6 -10 164.48 9.10 -4 -6 10 81.59 11.80 -4 -6 10 86.89 10.60 -4 -6 10 101.49 11.10 4 -6 -10 95.19 6.60 4 -6 -10 84.29 9.60 -4 6 10 103.79 8.80 -4 6 10 113.09 9.50 -4 6 10 105.59 8.50 4 6 -10 90.49 7.30 4 6 -10 98.09 12.70 -3 -6 10 61.09 10.80 -3 -6 10 69.59 11.10 3 -6 -10 69.19 5.90 3 -6 -10 60.59 10.50 -3 -6 10 81.39 9.90 -3 -6 10 73.69 9.20 3 6 -10 84.99 12.60 3 6 -10 73.69 6.80 -3 6 10 65.09 7.50 -3 6 10 82.29 8.00 -3 6 10 67.09 8.80 -3 6 10 82.99 9.30 -2 -6 10 25.40 5.60 -2 -6 10 56.89 10.20 -2 -6 10 17.60 6.40 -2 -6 10 48.40 9.00 -2 -6 10 31.60 5.50 2 -6 -10 37.60 5.20 -2 6 10 30.10 5.50 -2 6 10 38.00 6.60 -2 6 10 49.00 6.90 2 6 -10 38.40 5.80 2 6 -10 28.00 11.70 1 -6 -10 16.80 3.50 -1 -6 10 20.20 6.10 -1 -6 10 18.10 5.80 -1 -6 10 10.20 9.00 -1 -6 10 6.00 5.00 -1 -6 10 19.90 6.50 -1 -6 10 12.80 4.70 -1 6 10 18.00 4.10 -1 6 10 16.60 3.90 1 6 -10 18.50 4.00 -1 6 10 16.20 4.70 -1 6 10 14.00 4.70 0 -6 10 76.89 11.70 0 -6 -10 99.49 8.00 0 -6 10 100.79 8.60 0 -6 10 96.39 10.40 0 -6 10 103.89 9.30 0 6 10 99.59 7.90 0 6 -10 87.49 7.70 0 6 10 101.39 8.20 0 6 10 107.19 8.70 0 6 10 91.49 7.80 1 -6 10 156.28 10.10 1 -6 10 164.78 12.70 1 -6 10 161.58 10.60 1 -6 10 165.68 11.30 1 6 10 149.99 9.10 1 6 10 176.58 9.50 1 6 10 189.18 11.30 1 6 10 168.98 10.00 2 -6 10 119.99 7.90 2 -6 10 137.49 12.90 2 -6 10 118.99 8.10 2 6 10 125.99 7.80 2 6 10 127.19 7.60 2 6 10 121.49 7.10 3 -6 10 28.90 4.90 3 -6 10 28.40 4.20 3 6 10 22.00 3.60 9 -7 -10 50.09 5.00 9 7 -10 45.80 6.60 8 -7 -10 23.00 6.20 8 7 -10 28.20 4.80 8 7 -10 39.20 6.80 8 7 -10 30.30 5.20 7 -7 -10 109.79 8.00 7 -7 -10 112.59 6.30 7 -7 -10 112.09 7.90 7 7 -10 107.69 8.60 7 7 -10 107.89 9.30 6 -7 -10 3.90 3.00 -6 -7 10 -11.80 10.20 6 -7 -10 -2.10 4.00 6 7 -10 -0.50 4.00 6 7 -10 5.20 5.70 -6 7 10 -3.30 5.80 -5 -7 10 123.29 13.80 5 -7 -10 137.29 7.60 -5 -7 10 146.19 12.00 5 -7 -10 121.69 9.80 -5 7 10 145.39 13.30 5 7 -10 143.39 8.30 -5 7 10 129.09 11.20 5 7 -10 140.19 13.40 -5 7 10 138.19 10.70 4 -7 -10 39.10 4.90 -4 -7 10 50.49 11.20 -4 -7 10 39.50 6.70 -4 -7 10 52.99 9.50 4 7 -10 41.80 10.80 -4 7 10 38.50 6.80 -4 7 10 49.70 7.00 -4 7 10 48.80 6.60 4 7 -10 37.30 5.80 -3 -7 10 85.29 11.60 3 -7 -10 104.99 6.90 3 -7 -10 111.99 12.80 -3 -7 10 118.89 10.10 -3 -7 10 107.29 10.70 -3 -7 10 92.39 10.10 3 7 -10 101.89 7.70 -3 7 10 113.49 9.90 -3 7 10 99.19 8.40 3 7 -10 130.99 12.40 -3 7 10 126.19 8.90 -3 7 10 115.09 9.40 -2 -7 10 481.65 22.20 2 -7 -10 439.46 18.80 -2 -7 10 439.56 26.80 -2 -7 10 485.85 22.30 -2 -7 10 439.16 23.10 -2 -7 10 492.15 20.90 -2 7 10 482.55 21.10 -2 7 10 435.56 20.70 -2 7 10 477.15 20.50 -2 7 10 449.95 19.90 2 7 -10 447.86 19.60 1 -7 -10 102.09 7.00 -1 -7 10 78.49 11.00 -1 -7 10 105.49 11.90 -1 -7 10 125.19 14.40 1 7 -10 97.19 7.60 -1 7 10 99.99 8.00 -1 7 10 104.89 8.60 0 -7 -10 163.88 9.50 0 -7 10 172.88 12.60 0 -7 10 179.08 10.70 0 -7 10 174.38 11.70 0 -7 10 134.69 12.30 0 7 -10 156.58 9.60 0 7 10 183.08 10.50 0 7 10 181.28 9.90 0 7 10 176.18 10.10 0 7 10 167.78 9.80 1 -7 10 59.59 8.70 1 -7 10 74.59 9.30 1 -7 10 73.59 7.10 1 -7 10 72.09 7.60 1 7 10 77.59 6.80 1 7 10 64.89 6.30 -1 7 -10 59.99 7.60 1 7 10 73.19 7.00 1 7 10 73.29 6.30 2 -7 10 2.90 3.10 2 -7 10 8.80 5.20 2 -7 10 -5.60 7.50 2 -7 10 4.30 3.20 2 7 10 8.30 3.00 2 7 10 6.80 3.10 2 7 10 3.90 2.50 3 -7 10 31.80 4.30 3 -7 10 35.10 4.80 9 -8 -10 7.40 3.80 8 -8 -10 34.80 5.70 8 -8 -10 38.90 5.40 8 8 -10 45.50 8.00 8 8 -10 61.99 9.50 -8 8 10 42.50 4.40 7 -8 -10 14.00 3.70 7 -8 -10 18.90 3.80 7 8 -10 9.00 4.50 7 8 -10 12.70 5.70 -6 -8 10 83.99 15.80 6 -8 -10 125.49 8.40 6 -8 -10 117.29 7.10 6 8 -10 127.19 11.10 -6 8 10 99.09 10.00 -5 -8 10 20.10 6.10 5 -8 -10 34.80 4.50 -5 -8 10 26.30 7.40 5 -8 -10 25.60 5.20 -5 8 10 27.90 5.90 5 8 -10 24.20 6.50 -5 8 10 33.20 5.90 5 8 -10 24.10 3.80 4 -8 -10 21.60 5.90 -4 -8 10 55.99 10.80 -4 -8 10 53.89 11.30 4 -8 -10 41.20 4.70 -4 -8 10 31.40 6.70 4 8 -10 39.50 5.70 -4 8 10 28.70 4.90 -4 8 10 34.80 6.70 -3 -8 10 53.09 10.00 -3 -8 10 46.70 6.80 -3 -8 10 53.29 9.30 3 -8 -10 47.60 5.10 -3 -8 10 55.69 10.70 3 8 -10 38.40 5.90 -3 8 10 37.90 8.30 -3 8 10 37.10 6.80 -3 8 10 45.30 6.80 -3 8 10 47.10 8.20 -3 8 10 42.00 6.60 -2 -8 10 83.29 15.20 2 -8 -10 73.09 6.10 -2 -8 10 83.99 11.40 -2 -8 10 90.29 11.10 -2 -8 10 107.89 10.70 2 8 -10 91.09 7.20 -2 8 10 79.19 7.90 -2 8 10 89.79 8.60 2 8 -10 77.39 12.00 -2 8 10 94.79 7.80 -1 -8 10 31.30 6.20 -1 -8 10 41.40 9.20 1 -8 -10 40.90 5.30 -1 -8 10 35.20 6.60 -1 -8 10 39.50 8.10 -1 8 10 39.40 6.70 -1 8 10 56.39 8.30 1 8 -10 40.30 5.90 -1 8 10 43.70 7.00 0 -8 10 18.90 4.50 0 -8 10 29.80 5.50 0 -8 10 25.70 6.30 0 -8 10 14.20 5.70 0 -8 -10 34.10 6.20 0 8 10 22.80 4.20 0 8 10 36.20 6.30 0 8 10 30.80 5.50 0 8 10 27.70 5.60 0 8 -10 23.50 4.10 1 -8 10 3.60 5.10 1 -8 10 -0.10 3.40 1 -8 10 2.00 3.30 1 -8 10 0.90 4.70 1 8 10 5.00 2.80 1 8 10 3.50 3.10 1 8 10 12.40 4.40 -1 8 -10 5.30 4.00 1 8 10 5.70 3.10 2 -8 10 88.59 9.30 2 -8 10 66.39 6.00 2 -8 10 70.79 6.40 2 8 10 68.99 6.30 2 8 10 80.99 5.90 2 8 10 89.39 7.50 3 -8 10 17.30 2.90 8 -9 -10 4.50 3.10 8 9 -10 12.60 6.30 8 9 -10 4.90 4.60 7 -9 -10 139.39 8.30 7 -9 -10 123.19 7.90 7 9 -10 130.59 9.50 7 9 -10 144.59 9.00 6 -9 -10 49.90 7.00 -6 -9 10 42.90 10.10 6 9 -10 52.19 8.90 -5 -9 10 -0.70 5.50 5 -9 -10 5.70 2.60 -5 -9 10 -8.00 6.70 5 -9 -10 1.00 4.70 5 9 -10 -0.60 3.20 -5 9 10 6.40 5.50 5 9 -10 9.00 5.90 -5 9 10 0.70 5.10 4 -9 -10 179.28 9.10 -4 -9 10 181.68 14.10 -4 -9 10 196.48 13.60 -4 9 10 190.98 11.80 4 9 -10 184.58 9.90 -4 9 10 169.78 13.00 -4 9 10 184.88 9.60 4 9 -10 213.08 13.70 -4 9 10 166.18 10.60 -3 -9 10 90.19 11.20 3 -9 -10 97.29 6.20 -3 -9 10 83.29 9.90 -3 -9 10 92.09 10.40 3 9 -10 100.99 11.90 -3 9 10 101.69 12.60 3 9 -10 83.69 7.00 -3 9 10 93.99 8.90 -3 9 10 93.19 9.00 -2 -9 10 220.98 13.80 -2 -9 10 209.78 14.70 -2 -9 10 233.58 12.80 -2 -9 10 186.58 18.10 2 -9 -10 229.28 10.60 2 9 -10 237.28 15.40 -2 9 10 250.17 12.80 2 9 -10 230.08 11.50 -2 9 10 240.28 12.00 -1 -9 10 38.60 6.30 -1 -9 10 34.20 6.40 -1 -9 10 45.60 7.90 -1 -9 10 36.30 6.30 1 -9 -10 30.90 5.00 -1 9 10 35.00 6.20 -1 9 10 35.20 5.80 -1 9 10 33.30 5.90 1 9 -10 28.20 4.20 -1 9 10 24.20 4.30 0 -9 -10 36.40 6.10 0 -9 10 34.70 5.80 0 -9 10 45.70 7.50 0 -9 10 37.50 8.40 0 -9 10 40.80 7.00 0 9 -10 32.90 5.90 0 9 10 38.40 5.70 0 9 10 40.20 6.50 0 9 10 41.30 5.80 0 9 10 38.90 5.30 1 -9 10 60.69 9.60 1 -9 10 74.19 8.30 1 -9 10 74.79 6.70 1 -9 10 73.89 7.50 -1 9 -10 73.69 7.10 1 9 10 82.39 5.90 1 9 10 79.39 6.10 1 9 10 77.29 6.30 2 -9 10 2.00 3.00 2 -9 10 4.70 4.90 2 -9 10 -1.60 2.60 2 9 10 1.50 2.80 2 9 10 6.90 3.10 2 9 10 2.90 2.50 3 -9 10 48.20 4.20 8 -10 -10 80.09 6.00 8 10 -10 73.59 7.20 -8 10 10 84.69 5.20 7 -10 -10 29.30 5.20 7 -10 -10 38.80 6.20 -7 10 10 41.50 4.40 7 10 -10 25.30 4.60 6 -10 -10 3.60 3.70 -6 -10 10 23.10 9.20 6 -10 -10 10.40 4.40 6 -10 -10 12.20 2.50 6 -10 -10 14.90 3.40 6 10 -10 14.90 4.70 -6 10 10 8.30 2.90 6 10 -10 9.00 5.00 -5 -10 10 71.39 11.10 5 -10 -10 62.99 5.20 5 -10 -10 60.19 8.70 -5 -10 10 57.59 9.40 -5 10 10 70.39 8.20 -5 10 10 47.80 8.90 5 10 -10 54.29 6.40 -5 10 10 63.79 5.80 5 10 -10 79.39 10.10 -4 -10 10 449.86 22.40 4 -10 -10 441.76 18.20 -4 -10 10 463.15 21.40 -4 10 10 435.06 20.00 -4 10 10 450.15 18.50 -4 10 10 450.35 19.40 4 10 -10 483.85 21.60 4 10 -10 450.85 18.90 3 -10 -10 35.80 4.50 -3 -10 10 32.50 7.20 -3 -10 10 37.80 6.60 -3 -10 10 41.50 6.80 -3 -10 10 51.39 9.90 -3 -10 10 30.30 7.50 -3 10 10 35.00 6.30 3 10 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5.90 3 -15 -11 16.70 2.90 -2 -15 11 49.90 8.50 -7 0 12 28.80 5.20 6 0 -12 122.39 7.40 -6 0 12 110.09 7.40 -5 0 12 0.80 3.20 -5 0 12 5.90 3.60 5 0 -12 2.60 3.40 5 0 -12 3.90 2.60 4 0 -12 121.39 6.70 -4 0 12 115.59 7.50 -4 0 12 122.39 10.40 4 0 -12 127.29 8.20 -4 0 12 126.09 8.20 -3 0 12 21.90 4.00 -3 0 12 11.20 3.90 3 0 -12 8.20 4.20 -3 0 12 14.90 3.10 3 0 -12 11.60 2.60 -3 0 12 16.70 4.00 2 0 -12 92.89 9.70 2 0 -12 90.19 6.20 -2 0 12 99.89 6.50 -2 0 12 100.89 7.40 -2 0 12 97.89 6.70 -2 0 12 106.49 7.30 -1 0 12 30.60 4.80 -1 0 12 36.20 4.20 -1 0 12 25.50 4.00 -1 0 12 23.30 4.40 0 0 12 56.29 4.90 0 0 12 62.29 4.60 0 0 12 53.99 4.40 -7 -1 12 59.69 5.70 7 -1 -12 52.99 4.90 7 1 -12 53.39 5.20 6 -1 -12 8.00 3.20 -6 -1 12 7.50 3.60 -6 1 12 8.20 3.40 6 1 -12 13.50 3.50 -5 -1 12 172.38 9.30 5 -1 -12 167.68 8.40 5 -1 -12 195.08 9.60 -5 -1 12 179.38 9.80 -5 1 12 191.48 9.80 -5 1 12 169.78 9.00 5 1 -12 185.28 9.70 5 1 -12 184.68 8.60 -4 -1 12 25.70 4.80 -4 -1 12 36.00 6.10 4 -1 -12 39.00 4.20 4 -1 -12 28.80 4.50 -4 -1 12 34.50 5.20 4 1 -12 34.90 5.80 -4 1 12 37.00 5.20 -4 1 12 33.00 6.00 -4 1 12 45.40 8.30 4 1 -12 29.40 4.20 -3 -1 12 160.28 8.60 3 -1 -12 159.48 8.00 -3 -1 12 175.68 9.90 -3 -1 12 154.38 9.40 -3 -1 12 149.19 9.30 -3 1 12 157.48 9.40 3 1 -12 161.18 9.80 -3 1 12 159.98 8.50 -3 1 12 156.68 9.20 -3 1 12 161.58 8.70 3 1 -12 158.98 8.10 -2 -1 12 14.30 3.40 -2 -1 12 12.90 3.60 -2 -1 12 13.30 3.50 -2 -1 12 11.10 2.80 2 -1 -12 16.10 3.00 -2 1 12 14.60 3.50 -2 1 12 13.70 3.00 2 1 -12 11.40 2.90 2 1 -12 21.40 5.20 -2 1 12 11.30 3.00 -2 1 12 8.70 3.40 -1 -1 12 15.70 3.90 -1 -1 12 17.10 2.90 -1 -1 12 12.50 3.30 -1 -1 12 23.30 4.10 -1 1 12 14.40 2.90 -1 1 12 16.10 2.90 -1 1 12 15.80 3.30 -1 1 12 15.80 3.50 0 -1 12 42.20 4.60 0 -1 12 41.70 4.30 0 -1 12 43.70 4.30 0 1 12 42.10 4.50 0 1 12 40.80 4.00 0 1 12 39.70 4.40 -7 -2 12 -5.90 3.40 7 -2 -12 6.70 2.80 -7 2 12 0.40 3.70 6 -2 -12 9.20 4.10 -6 -2 12 17.20 4.00 6 2 -12 15.40 3.50 -6 2 12 20.10 4.20 5 -2 -12 144.69 7.50 5 -2 -12 156.78 8.80 -5 -2 12 124.09 11.80 -5 -2 12 146.09 8.90 -5 2 12 167.68 8.80 5 2 -12 157.28 7.80 5 2 -12 159.68 8.70 -4 -2 12 392.36 17.30 4 -2 -12 394.36 15.60 -4 -2 12 377.66 16.10 -4 -2 12 388.26 16.80 4 -2 -12 380.16 16.60 4 2 -12 378.16 15.60 -4 2 12 395.76 16.80 -4 2 12 383.06 16.10 4 2 -12 398.56 16.70 -4 2 12 344.17 19.00 -3 -2 12 70.39 7.00 3 -2 -12 61.19 4.90 3 -2 -12 77.99 8.70 -3 -2 12 71.39 7.10 -3 -2 12 67.69 5.90 3 2 -12 77.99 5.40 -3 2 12 65.59 6.50 -3 2 12 68.49 5.70 -3 2 12 61.99 6.50 -3 2 12 63.79 6.20 -2 -2 12 110.09 7.90 -2 -2 12 99.69 7.60 -2 -2 12 96.19 6.70 -2 -2 12 117.89 7.20 2 -2 -12 107.09 6.30 -2 2 12 99.59 7.20 2 2 -12 102.29 7.10 -2 2 12 114.89 6.80 -2 2 12 105.59 7.30 -2 2 12 119.39 6.90 -1 -2 12 153.48 8.60 -1 -2 12 139.39 8.80 -1 -2 12 148.29 7.80 -1 -2 12 151.28 8.10 -1 2 12 144.49 8.20 -1 2 12 157.58 7.70 -1 2 12 152.38 7.70 0 -2 12 56.29 4.80 0 -2 12 50.59 4.80 0 -2 12 47.20 4.40 0 2 12 49.50 4.60 0 2 12 59.09 4.50 0 2 12 48.90 4.80 -7 -3 12 30.60 4.70 7 -3 -12 33.20 4.80 7 3 -12 24.20 4.80 6 -3 -12 3.60 2.80 -6 -3 12 2.80 3.60 6 3 -12 8.70 3.30 -6 3 12 2.50 4.30 5 -3 -12 152.88 7.40 5 -3 -12 157.58 10.20 -5 -3 12 147.19 9.20 -5 3 12 144.09 8.60 5 3 -12 148.69 7.80 5 3 -12 158.08 8.80 4 -3 -12 35.40 4.20 -4 -3 12 35.80 6.60 -4 -3 12 42.80 6.40 -4 -3 12 35.90 7.00 4 -3 -12 32.40 8.00 -4 3 12 48.10 5.10 -4 3 12 33.20 5.10 -4 3 12 43.50 8.30 4 3 -12 38.60 4.50 -4 3 12 31.80 5.40 -3 -3 12 112.99 7.00 -3 -3 12 116.09 8.40 -3 -3 12 95.09 8.00 3 -3 -12 112.89 6.30 -3 -3 12 86.19 8.40 -3 3 12 109.69 7.80 -3 3 12 114.79 7.50 -3 3 12 99.09 8.60 3 3 -12 118.09 6.60 -3 3 12 114.49 6.80 -2 -3 12 52.89 6.20 -2 -3 12 49.90 5.70 2 -3 -12 56.59 5.10 -2 -3 12 59.79 5.40 -2 3 12 61.99 5.20 -2 3 12 51.99 5.50 2 3 -12 50.09 5.20 -2 3 12 58.99 5.80 -2 3 12 60.79 5.00 -1 -3 12 113.19 7.40 -1 -3 12 117.59 8.00 -1 -3 12 114.39 6.90 -1 3 12 110.19 6.80 -1 3 12 112.59 6.60 -1 3 12 107.29 6.40 -1 3 12 95.69 9.00 0 -3 12 3.10 3.30 0 -3 12 7.40 2.40 0 -3 12 4.20 2.40 0 3 12 8.80 2.60 0 3 12 4.30 2.10 7 -4 -12 36.70 4.90 -7 -4 12 27.10 5.30 7 4 -12 41.80 4.90 6 -4 -12 11.90 3.20 -6 -4 12 2.50 3.70 -6 4 12 10.70 3.40 6 4 -12 8.50 3.40 -5 -4 12 31.90 5.50 -5 -4 12 23.80 6.00 5 -4 -12 27.20 4.30 5 -4 -12 30.30 4.20 -5 4 12 32.90 5.40 5 4 -12 30.50 4.20 5 4 -12 35.70 4.80 -4 -4 12 33.60 6.10 4 -4 -12 31.80 3.90 -4 -4 12 44.20 7.90 -4 -4 12 25.60 5.30 4 -4 -12 19.50 5.40 -4 4 12 29.10 4.70 -4 4 12 25.70 4.80 -4 4 12 40.80 7.70 4 4 -12 32.50 4.60 -3 -4 12 50.49 7.10 -3 -4 12 44.80 7.00 -3 -4 12 30.80 4.90 3 -4 -12 35.50 4.30 -3 -4 12 36.20 5.10 -3 4 12 36.60 5.20 -3 4 12 43.80 4.90 -3 4 12 31.70 4.70 -3 4 12 31.50 5.20 3 4 -12 42.30 4.70 -2 -4 12 35.80 4.90 -2 -4 12 47.20 6.00 2 -4 -12 46.70 4.90 -2 -4 12 42.30 5.10 -2 4 12 51.59 4.70 -2 4 12 52.49 5.30 -2 4 12 43.00 4.70 2 4 -12 52.79 5.10 -2 4 12 49.30 5.50 -1 -4 12 14.30 4.10 -1 -4 12 10.00 4.90 -1 -4 12 14.60 3.10 -1 4 12 13.00 4.30 -1 4 12 9.10 3.50 -1 4 12 10.60 2.90 -1 4 12 16.70 4.60 0 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16.70 0 -5 12 44.70 5.20 0 -5 12 43.00 4.10 0 -5 12 47.50 4.30 0 5 12 51.39 4.40 0 5 12 54.99 4.10 -7 -6 12 17.70 3.50 -6 -6 12 11.40 3.80 6 -6 -12 6.10 2.90 6 -6 -12 12.40 2.10 6 6 -12 11.90 3.20 -6 6 12 2.00 4.20 5 -6 -12 8.60 2.60 -5 -6 12 -1.90 6.40 5 6 -12 0.40 3.10 -5 6 12 3.40 5.40 -4 -6 12 96.19 8.20 4 -6 -12 113.99 6.00 4 6 -12 126.99 6.80 -4 6 12 106.79 7.90 -4 6 12 112.49 7.20 -3 -6 12 34.70 5.40 -3 -6 12 32.00 6.40 -3 -6 12 34.60 5.20 3 -6 -12 34.70 4.10 -3 6 12 34.40 4.50 3 6 -12 38.30 4.60 -3 6 12 42.70 6.00 -3 6 12 39.70 4.80 2 -6 -12 38.50 4.60 -2 -6 12 42.30 5.50 -2 -6 12 45.60 5.40 -2 -6 12 44.70 5.90 2 6 -12 42.20 5.00 -2 6 12 37.10 5.00 -2 6 12 39.60 6.30 -2 6 12 37.90 4.80 -2 6 12 51.39 5.40 -1 -6 12 62.79 5.50 -1 -6 12 68.59 5.50 -1 -6 12 74.29 6.00 -1 6 12 66.49 5.10 -1 6 12 56.39 5.10 -1 6 12 63.59 4.50 -1 6 12 60.19 4.90 0 -6 12 64.59 4.90 0 -6 12 76.39 4.80 0 6 12 72.39 4.70 0 6 12 81.79 4.90 -6 -7 12 13.50 3.70 6 -7 -12 23.40 3.70 6 -7 -12 15.30 3.00 6 7 -12 20.60 3.90 -5 -7 12 90.99 7.10 5 -7 -12 91.79 6.80 5 7 -12 74.89 9.00 -5 7 12 102.09 7.00 -4 -7 12 9.70 4.50 -4 -7 12 -4.50 4.60 4 -7 -12 1.00 2.30 4 7 -12 1.20 2.80 -4 7 12 2.10 4.80 -4 7 12 -3.10 4.90 -3 -7 12 80.59 7.00 -3 -7 12 97.79 8.10 3 -7 -12 90.09 5.40 -3 -7 12 73.49 8.00 -3 7 12 98.29 5.90 -3 7 12 91.99 6.00 -3 7 12 100.79 6.20 -3 7 12 96.29 7.20 3 7 -12 83.29 5.80 -2 -7 12 27.20 5.60 2 -7 -12 30.70 5.90 -2 -7 12 25.20 3.70 -2 7 12 30.10 4.10 -2 7 12 27.20 4.90 2 7 -12 26.20 4.60 -2 7 12 30.40 4.10 -2 7 12 32.70 5.60 -1 -7 12 132.89 7.70 -1 -7 12 135.49 8.00 -1 -7 12 130.69 7.20 -1 7 12 131.99 6.70 -1 7 12 130.89 7.10 -1 7 12 139.39 7.10 6 -8 -12 125.49 6.90 -6 -8 12 119.49 7.10 6 8 -12 137.99 7.10 5 -8 -12 40.70 3.30 5 -8 -12 38.40 4.50 -5 -8 12 32.20 5.70 5 8 -12 40.60 5.40 -5 8 12 51.19 5.90 -4 -8 12 62.09 7.80 -4 -8 12 68.89 7.70 4 -8 -12 81.59 5.10 -4 8 12 81.29 5.90 4 8 -12 74.19 6.00 -3 -8 12 73.19 7.30 3 -8 -12 66.59 5.00 -3 8 12 75.59 5.30 -3 8 12 71.29 6.30 3 8 -12 63.09 5.40 -2 -8 12 105.29 7.40 -2 -8 12 112.79 7.20 -2 8 12 101.19 6.50 -2 8 12 115.09 6.60 -2 8 12 108.69 6.80 -1 -8 12 91.89 6.60 -1 8 12 90.19 5.20 -1 8 12 93.29 5.60 -1 8 12 96.29 5.70 6 -9 -12 3.70 2.70 5 -9 -12 48.80 4.60 5 -9 -12 45.30 3.50 5 9 -12 54.69 5.40 4 -9 -12 84.59 4.50 -4 -9 12 64.89 8.00 4 -9 -12 86.09 5.50 -4 9 12 89.89 6.10 3 -9 -12 13.90 2.30 -3 -9 12 9.40 4.00 -3 9 12 11.10 3.00 -3 9 12 22.50 4.50 2 -9 -12 91.49 5.40 -2 -9 12 84.29 6.50 -2 9 12 81.59 5.50 -2 9 12 85.89 5.10 -1 -9 12 7.70 3.90 -1 9 12 7.50 2.20 5 -10 -12 15.30 2.80 5 -10 -12 12.70 2.50 5 10 -12 17.10 3.50 4 -10 -12 13.90 2.90 4 -10 -12 18.20 2.90 3 -10 -12 42.40 3.60 -3 -10 12 33.10 6.10 -3 10 12 42.90 4.60 -3 10 12 40.90 5.70 -2 -10 12 6.90 3.40 -2 10 12 6.60 2.70 -2 10 12 4.80 2.20 4 -11 -12 26.70 2.90 4 11 -12 39.10 5.10 -3 -11 12 286.07 12.70 3 -11 -12 284.27 11.20 -5 0 13 40.60 4.70 -4 0 13 26.30 4.40 -3 0 13 0.90 2.90 -5 -1 13 21.80 4.40 -5 1 13 24.50 4.60 -4 -1 13 91.49 6.30 -4 1 13 98.99 5.90 -3 -1 13 1.10 2.80 -3 1 13 -0.40 3.40 -3 1 13 3.70 2.40 -5 2 13 7.30 4.60 -4 2 13 91.49 5.60 -3 2 13 98.59 5.60 -3 2 13 109.09 6.20 -4 3 13 36.10 4.60 -3 3 13 31.50 5.30 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 33234 _shelx_SHELXL_version_number '2014/7' _olex2_submission_special_instructions 'No special instructions were received'