####################################################################### # # 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_b12b _database_code_depnum_ccdc_archive 'CCDC 2104641' loop_ _audit_author_name _audit_author_address 'Cynthia S. Day' ;Wake Forest University United States of America ; _audit_update_record ; 2021-08-21 deposited with the CCDC. 2021-12-17 downloaded from the CCDC. ; _audit_creation_date 2021-08-21 _audit_creation_method ; Olex2 1.3 (compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272) ; _shelx_SHELXL_version_number 2018/3 _audit_contact_author_address ? _audit_contact_author_email ? _audit_contact_author_phone ? _publ_contact_author_id_orcid ? _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. (2015). Acta Cryst. A71, 3-8. Sheldrick, G.M. (2015). Acta Cryst. C71, 3-8. ; _chemical_name_common ? _chemical_name_systematic ? _chemical_formula_moiety 'C7 H7 O3 S, C12 H16 N O2' _chemical_formula_sum 'C19 H23 N O5 S' _chemical_formula_weight 377.44 _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' S S 0.1246 0.1234 '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 8.2854(6) _cell_length_b 10.5892(7) _cell_length_c 20.7453(14) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 1820.1(2) _cell_formula_units_Z 4 _cell_measurement_reflns_used 9220 _cell_measurement_temperature 193.65 _cell_measurement_theta_max 30.069 _cell_measurement_theta_min 3.519 _shelx_estimated_absorpt_T_max 0.969 _shelx_estimated_absorpt_T_min 0.923 _exptl_absorpt_coefficient_mu 0.208 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_correction_T_min 0.8948 _exptl_absorpt_correction_type none _exptl_absorpt_process_details ; SADABS-2016/2 (Bruker,2016) was used for absorption correction. wR2(int) was 0.0634 before and 0.0558 after correction. The Ratio of minimum to maximum transmission is 0.8948. 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 1.377 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description block _exptl_crystal_F_000 800 _exptl_crystal_preparation ? _exptl_crystal_recrystallization_method 'The material was recrystallised from a mixture of DCM and pentane by vapour diffusion.' _exptl_crystal_size_max 0.39 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.15 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0488 _diffrn_reflns_av_unetI/netI 0.0337 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.997 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_number 30904 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.997 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 30.069 _diffrn_reflns_theta_min 3.519 _diffrn_ambient_temperature 193.65 _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source ? _diffrn_source_current 30.0 _diffrn_source_power 1.5 _diffrn_source_voltage 50.0 _diffrn_special_details ? _diffrn_standards_number 0 _reflns_Friedel_coverage 0.949 _reflns_Friedel_fraction_full 0.997 _reflns_Friedel_fraction_max 0.996 _reflns_number_gt 4847 _reflns_number_total 5317 _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 V8.40B (?, 2016)' _computing_data_collection ? _computing_data_reduction 'SAINT V8.40B (?, 2016)' _computing_molecular_graphics 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _refine_diff_density_max 0.411 _refine_diff_density_min -0.377 _refine_diff_density_rms 0.068 _refine_ls_abs_structure_details ; Flack x determined using 2200 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack -0.02(3) _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 240 _refine_ls_number_reflns 5317 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0415 _refine_ls_R_factor_gt 0.0365 _refine_ls_restrained_S_all 1.027 _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^)+(0.0516P)^2^+0.3296P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0899 _refine_ls_wR_factor_ref 0.0940 _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.a Secondary CH2 refined with riding coordinates: C14(H14A,H14B), C9(H9A,H9B), C11(H11A,H11B), C15(H15A,H15B), C12(H12A,H12B) 2.b Aromatic/amide H refined with riding coordinates: C17(H17), C22(H22), C21(H21), C3(H3), C18(H18), C7(H7), C4(H4), C5(H5), C6(H6) 2.c Idealised Me refined as rotating group: C20(H20A,H20B,H20C) ; _atom_sites_solution_hydrogens mixed _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 S23 S 0.27114(6) 0.45737(4) 0.40980(3) 0.02493(12) Uani 1 1 d . . . . . O26 O 0.4000(2) 0.53101(17) 0.38030(9) 0.0329(4) Uani 1 1 d . . . . . O8 O 0.5864(2) 0.69407(17) 0.50888(9) 0.0355(4) Uani 1 1 d . . . . . O13 O 0.7889(2) 0.60324(18) 0.27586(8) 0.0332(4) Uani 1 1 d . . . . . O27 O 0.1296(2) 0.5358(2) 0.42114(11) 0.0445(5) Uani 1 1 d . . . . . N10 N 0.7208(2) 0.56277(14) 0.41025(10) 0.0198(3) Uani 1 1 d . . . . . O24 O 0.2358(4) 0.34148(19) 0.37695(12) 0.0637(8) Uani 1 1 d . . . . . C16 C 0.3444(3) 0.41530(19) 0.48706(10) 0.0235(4) Uani 1 1 d . . . . . C19 C 0.4727(3) 0.3547(2) 0.60811(11) 0.0289(5) Uani 1 1 d . . . . . C1 C 0.6941(3) 0.6239(2) 0.52563(11) 0.0242(4) Uani 1 1 d . . . . . C14 C 0.7348(3) 0.7040(2) 0.31596(12) 0.0285(5) Uani 1 1 d . . . . . H14A H 0.615612 0.708995 0.314129 0.034 Uiso 1 1 calc R U . . . H14B H 0.778840 0.784801 0.299565 0.034 Uiso 1 1 calc R U . . . C17 C 0.4491(3) 0.3126(2) 0.49336(11) 0.0270(4) Uani 1 1 d . . . . . H17 H 0.476537 0.262856 0.456863 0.032 Uiso 1 1 calc R U . . . C9 C 0.7770(3) 0.5381(2) 0.47708(11) 0.0230(4) Uani 1 1 d . . . . . H9A H 0.895132 0.551451 0.479377 0.028 Uiso 1 1 calc R U . . . H9B H 0.754854 0.448951 0.488347 0.028 Uiso 1 1 calc R U . . . C22 C 0.3041(3) 0.4872(2) 0.54077(12) 0.0283(5) Uani 1 1 d . . . . . H22 H 0.233843 0.557617 0.536451 0.034 Uiso 1 1 calc R U . . . C2 C 0.7483(3) 0.6132(2) 0.59405(11) 0.0267(4) Uani 1 1 d . . . . . C21 C 0.3666(3) 0.4559(2) 0.60055(12) 0.0304(5) Uani 1 1 d . . . . . H21 H 0.336567 0.504399 0.637186 0.037 Uiso 1 1 calc R U . . . C11 C 0.7702(3) 0.45655(19) 0.36599(12) 0.0261(4) Uani 1 1 d . . . . . H11A H 0.718201 0.376989 0.380032 0.031 Uiso 1 1 calc R U . . . H11B H 0.888617 0.444815 0.367943 0.031 Uiso 1 1 calc R U . . . C3 C 0.8810(3) 0.5396(2) 0.61172(12) 0.0324(5) Uani 1 1 d . . . . . H3 H 0.941075 0.496125 0.579640 0.039 Uiso 1 1 calc R U . . . C15 C 0.7873(3) 0.68577(19) 0.38505(11) 0.0234(4) Uani 1 1 d . . . . . H15A H 0.906664 0.684809 0.387530 0.028 Uiso 1 1 calc R U . . . H15B H 0.747374 0.756629 0.411783 0.028 Uiso 1 1 calc R U . . . C18 C 0.5128(3) 0.2841(2) 0.55360(12) 0.0297(5) Uani 1 1 d . . . . . H18 H 0.585289 0.215075 0.557770 0.036 Uiso 1 1 calc R U . . . C7 C 0.6601(4) 0.6763(2) 0.64140(13) 0.0359(5) Uani 1 1 d . . . . . H7 H 0.570043 0.726920 0.629734 0.043 Uiso 1 1 calc R U . . . C20 C 0.5432(4) 0.3236(3) 0.67283(13) 0.0413(6) Uani 1 1 d . . . . . H20A H 0.568812 0.401920 0.695813 0.062 Uiso 1 1 calc R U . . . H20B H 0.641932 0.273898 0.667042 0.062 Uiso 1 1 calc R U . . . H20C H 0.464912 0.274585 0.697902 0.062 Uiso 1 1 calc R U . . . C4 C 0.9256(4) 0.5299(3) 0.67631(14) 0.0414(6) Uani 1 1 d . . . . . H4 H 1.016277 0.480130 0.688179 0.050 Uiso 1 1 calc R U . . . C5 C 0.8380(4) 0.5925(3) 0.72305(13) 0.0453(7) Uani 1 1 d . . . . . H5 H 0.868893 0.586107 0.767029 0.054 Uiso 1 1 calc R U . . . C12 C 0.7201(3) 0.4869(2) 0.29763(12) 0.0319(5) Uani 1 1 d . . . . . H12A H 0.754940 0.417657 0.268743 0.038 Uiso 1 1 calc R U . . . H12B H 0.600920 0.492579 0.295420 0.038 Uiso 1 1 calc R U . . . C6 C 0.7047(4) 0.6647(3) 0.70595(13) 0.0437(7) Uani 1 1 d . . . . . H6 H 0.643741 0.706363 0.738365 0.052 Uiso 1 1 calc R U . . . H10 H 0.614(4) 0.566(3) 0.4077(16) 0.032(7) Uiso 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 S23 0.0229(2) 0.0224(2) 0.0294(2) 0.0046(2) -0.0051(2) -0.00407(17) O26 0.0199(8) 0.0462(10) 0.0326(9) 0.0145(8) -0.0004(7) -0.0015(6) O8 0.0329(9) 0.0428(9) 0.0309(9) 0.0038(7) 0.0045(7) 0.0119(7) O13 0.0383(10) 0.0366(9) 0.0246(8) -0.0016(7) 0.0108(7) 0.0008(7) O27 0.0189(8) 0.0650(12) 0.0498(13) 0.0154(9) -0.0003(8) 0.0074(8) N10 0.0174(7) 0.0193(6) 0.0226(7) 0.0012(7) 0.0016(7) -0.0010(5) O24 0.115(2) 0.0275(9) 0.0481(13) 0.0013(9) -0.0373(14) -0.0122(11) C16 0.0212(10) 0.0230(9) 0.0262(10) 0.0045(8) 0.0006(8) -0.0035(7) C19 0.0279(11) 0.0328(11) 0.0261(10) 0.0065(8) 0.0005(9) -0.0033(9) C1 0.0232(10) 0.0265(9) 0.0228(10) 0.0023(8) 0.0032(8) -0.0016(8) C14 0.0336(12) 0.0282(10) 0.0237(10) 0.0033(8) 0.0047(9) 0.0038(9) C17 0.0272(11) 0.0263(10) 0.0274(11) 0.0024(8) 0.0043(8) 0.0022(8) C9 0.0230(10) 0.0254(10) 0.0207(9) 0.0024(7) -0.0006(8) 0.0013(7) C22 0.0258(11) 0.0248(10) 0.0345(12) 0.0007(8) 0.0030(9) -0.0001(8) C2 0.0291(11) 0.0273(10) 0.0238(10) 0.0001(8) 0.0008(8) -0.0045(8) C21 0.0317(12) 0.0305(11) 0.0292(11) -0.0015(8) 0.0043(9) -0.0008(9) C11 0.0278(11) 0.0197(9) 0.0307(11) -0.0036(8) 0.0018(9) 0.0017(7) C3 0.0322(13) 0.0390(12) 0.0260(11) 0.0018(9) -0.0028(9) -0.0011(9) C15 0.0277(10) 0.0197(8) 0.0229(9) 0.0028(7) 0.0022(8) -0.0032(8) C18 0.0274(11) 0.0292(10) 0.0324(12) 0.0082(9) 0.0028(9) 0.0043(9) C7 0.0440(14) 0.0332(11) 0.0306(12) -0.0033(9) 0.0048(11) 0.0004(11) C20 0.0452(16) 0.0506(15) 0.0281(12) 0.0104(11) -0.0033(11) 0.0004(12) C4 0.0423(16) 0.0482(15) 0.0338(14) 0.0087(11) -0.0112(12) -0.0041(12) C5 0.0579(19) 0.0535(16) 0.0244(12) 0.0021(11) -0.0070(12) -0.0147(15) C12 0.0366(13) 0.0321(11) 0.0271(11) -0.0085(9) 0.0029(10) -0.0007(9) C6 0.0598(19) 0.0422(14) 0.0289(13) -0.0074(10) 0.0068(12) -0.0087(13) _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 S23 O26 1.4568(17) . ? S23 O27 1.456(2) . ? S23 O24 1.434(2) . ? S23 C16 1.771(2) . ? O8 C1 1.213(3) . ? O13 C14 1.425(3) . ? O13 C12 1.431(3) . ? N10 C9 1.486(3) . ? N10 C11 1.509(3) . ? N10 C15 1.508(2) . ? N10 H10 0.89(3) . ? C16 C17 1.397(3) . ? C16 C22 1.390(3) . ? C19 C21 1.395(3) . ? C19 C18 1.396(3) . ? C19 C20 1.501(3) . ? C1 C9 1.520(3) . ? C1 C2 1.493(3) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C14 C15 1.510(3) . ? C17 H17 0.9500 . ? C17 C18 1.390(3) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C22 H22 0.9500 . ? C22 C21 1.384(4) . ? C2 C3 1.396(3) . ? C2 C7 1.395(3) . ? C21 H21 0.9500 . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C11 C12 1.512(4) . ? C3 H3 0.9500 . ? C3 C4 1.394(4) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C18 H18 0.9500 . ? C7 H7 0.9500 . ? C7 C6 1.395(4) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C4 H4 0.9500 . ? C4 C5 1.381(5) . ? C5 H5 0.9500 . ? C5 C6 1.389(5) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C6 H6 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 O26 S23 C16 105.30(10) . . ? O27 S23 O26 110.63(11) . . ? O27 S23 C16 105.86(12) . . ? O24 S23 O26 114.10(15) . . ? O24 S23 O27 113.61(16) . . ? O24 S23 C16 106.55(11) . . ? C14 O13 C12 109.60(18) . . ? C9 N10 C11 110.62(16) . . ? C9 N10 C15 111.14(16) . . ? C9 N10 H10 112(2) . . ? C11 N10 H10 105(2) . . ? C15 N10 C11 109.50(17) . . ? C15 N10 H10 108.1(19) . . ? C17 C16 S23 119.55(17) . . ? C22 C16 S23 120.35(17) . . ? C22 C16 C17 120.0(2) . . ? C21 C19 C18 118.1(2) . . ? C21 C19 C20 121.0(2) . . ? C18 C19 C20 120.9(2) . . ? O8 C1 C9 120.6(2) . . ? O8 C1 C2 122.7(2) . . ? C2 C1 C9 116.7(2) . . ? O13 C14 H14A 109.3 . . ? O13 C14 H14B 109.3 . . ? O13 C14 C15 111.57(19) . . ? H14A C14 H14B 108.0 . . ? C15 C14 H14A 109.3 . . ? C15 C14 H14B 109.3 . . ? C16 C17 H17 120.4 . . ? C18 C17 C16 119.3(2) . . ? C18 C17 H17 120.4 . . ? N10 C9 C1 111.84(18) . . ? N10 C9 H9A 109.2 . . ? N10 C9 H9B 109.2 . . ? C1 C9 H9A 109.2 . . ? C1 C9 H9B 109.2 . . ? H9A C9 H9B 107.9 . . ? C16 C22 H22 120.1 . . ? C21 C22 C16 119.8(2) . . ? C21 C22 H22 120.1 . . ? C3 C2 C1 121.9(2) . . ? C7 C2 C1 118.4(2) . . ? C7 C2 C3 119.7(2) . . ? C19 C21 H21 119.3 . . ? C22 C21 C19 121.3(2) . . ? C22 C21 H21 119.3 . . ? N10 C11 H11A 109.7 . . ? N10 C11 H11B 109.7 . . ? N10 C11 C12 109.76(18) . . ? H11A C11 H11B 108.2 . . ? C12 C11 H11A 109.7 . . ? C12 C11 H11B 109.7 . . ? C2 C3 H3 119.9 . . ? C4 C3 C2 120.2(3) . . ? C4 C3 H3 119.9 . . ? N10 C15 C14 109.53(18) . . ? N10 C15 H15A 109.8 . . ? N10 C15 H15B 109.8 . . ? C14 C15 H15A 109.8 . . ? C14 C15 H15B 109.8 . . ? H15A C15 H15B 108.2 . . ? C19 C18 H18 119.3 . . ? C17 C18 C19 121.4(2) . . ? C17 C18 H18 119.3 . . ? C2 C7 H7 120.2 . . ? C6 C7 C2 119.7(3) . . ? C6 C7 H7 120.2 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20B 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C3 C4 H4 120.0 . . ? C5 C4 C3 120.0(3) . . ? C5 C4 H4 120.0 . . ? C4 C5 H5 119.9 . . ? C4 C5 C6 120.2(3) . . ? C6 C5 H5 119.9 . . ? O13 C12 C11 111.7(2) . . ? O13 C12 H12A 109.3 . . ? O13 C12 H12B 109.3 . . ? C11 C12 H12A 109.3 . . ? C11 C12 H12B 109.3 . . ? H12A C12 H12B 107.9 . . ? C7 C6 H6 119.8 . . ? C5 C6 C7 120.3(3) . . ? C5 C6 H6 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 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag S23 C16 C17 C18 176.67(18) . . . . ? S23 C16 C22 C21 -177.77(18) . . . . ? O26 S23 C16 C17 -81.12(19) . . . . ? O26 S23 C16 C22 95.94(19) . . . . ? O8 C1 C9 N10 5.7(3) . . . . ? O8 C1 C2 C3 -174.7(2) . . . . ? O8 C1 C2 C7 7.0(3) . . . . ? O13 C14 C15 N10 -58.9(2) . . . . ? O27 S23 C16 C17 161.66(18) . . . . ? O27 S23 C16 C22 -21.3(2) . . . . ? N10 C11 C12 O13 57.7(3) . . . . ? O24 S23 C16 C17 40.4(2) . . . . ? O24 S23 C16 C22 -142.5(2) . . . . ? C16 C17 C18 C19 0.9(4) . . . . ? C16 C22 C21 C19 1.4(4) . . . . ? C1 C2 C3 C4 -178.6(2) . . . . ? C1 C2 C7 C6 177.9(2) . . . . ? C14 O13 C12 C11 -60.9(3) . . . . ? C17 C16 C22 C21 -0.7(3) . . . . ? C9 N10 C11 C12 -176.85(19) . . . . ? C9 N10 C15 C14 177.03(18) . . . . ? C9 C1 C2 C3 7.4(3) . . . . ? C9 C1 C2 C7 -170.8(2) . . . . ? C22 C16 C17 C18 -0.4(3) . . . . ? C2 C1 C9 N10 -176.38(18) . . . . ? C2 C3 C4 C5 0.3(4) . . . . ? C2 C7 C6 C5 1.1(4) . . . . ? C21 C19 C18 C17 -0.3(4) . . . . ? C11 N10 C9 C1 -165.28(18) . . . . ? C11 N10 C15 C14 54.5(2) . . . . ? C3 C2 C7 C6 -0.4(4) . . . . ? C3 C4 C5 C6 0.4(4) . . . . ? C15 N10 C9 C1 72.9(2) . . . . ? C15 N10 C11 C12 -54.0(2) . . . . ? C18 C19 C21 C22 -0.9(4) . . . . ? C7 C2 C3 C4 -0.3(4) . . . . ? C20 C19 C21 C22 178.4(2) . . . . ? C20 C19 C18 C17 -179.6(2) . . . . ? C4 C5 C6 C7 -1.1(5) . . . . ? C12 O13 C14 C15 61.5(3) . . . . ? _shelx_res_file ; TITL b12b_a.res in Pna2(1) b12b.res created by SHELXL-2018/3 at 12:01:26 on 21-Aug-2021 REM Old TITL b12b in Pna2(1) REM SHELXT solution in Pna2(1): R1 0.097, Rweak 0.011, Alpha 0.002 REM 0.495 for 245 systematic absences, Orientation as input REM Flack x = 0.010 ( 0.029 ) from 1680 Parsons' quotients REM Formula found by SHELXT: C19 N O5 S CELL 0.71073 8.2854 10.5892 20.7453 90 90 90 ZERR 4 0.0006 0.0007 0.0014 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 S UNIT 76 92 4 20 4 L.S. 10 PLAN 1 SIZE 0.15 0.21 0.39 TEMP -79.5 CONF BOND list 4 fmap 2 MORE -1 BOND $H ACTA REM REM REM WGHT 0.051600 0.329600 FVAR 0.48828 S23 5 0.271143 0.457366 0.409799 11.00000 0.02294 0.02243 = 0.02942 0.00457 -0.00512 -0.00407 O26 4 0.399986 0.531010 0.380299 11.00000 0.01987 0.04623 = 0.03265 0.01448 -0.00040 -0.00148 O8 4 0.586378 0.694067 0.508879 11.00000 0.03286 0.04279 = 0.03092 0.00385 0.00449 0.01194 O13 4 0.788870 0.603242 0.275861 11.00000 0.03829 0.03662 = 0.02465 -0.00159 0.01076 0.00076 O27 4 0.129632 0.535847 0.421138 11.00000 0.01887 0.06496 = 0.04979 0.01540 -0.00033 0.00736 N10 3 0.720807 0.562769 0.410253 11.00000 0.01736 0.01933 = 0.02260 0.00118 0.00165 -0.00099 O24 4 0.235765 0.341476 0.376952 11.00000 0.11549 0.02750 = 0.04814 0.00132 -0.03731 -0.01216 C16 1 0.344378 0.415297 0.487061 11.00000 0.02120 0.02300 = 0.02622 0.00448 0.00060 -0.00351 C19 1 0.472665 0.354743 0.608113 11.00000 0.02791 0.03279 = 0.02609 0.00649 0.00050 -0.00332 C1 1 0.694139 0.623868 0.525633 11.00000 0.02323 0.02650 = 0.02277 0.00233 0.00322 -0.00162 C14 1 0.734843 0.704034 0.315964 11.00000 0.03365 0.02815 = 0.02368 0.00335 0.00466 0.00378 AFIX 23 H14A 2 0.615612 0.708995 0.314129 11.00000 -1.20000 H14B 2 0.778840 0.784801 0.299565 11.00000 -1.20000 AFIX 0 C17 1 0.449148 0.312625 0.493359 11.00000 0.02717 0.02629 = 0.02743 0.00241 0.00433 0.00216 AFIX 43 H17 2 0.476537 0.262856 0.456863 11.00000 -1.20000 AFIX 0 C9 1 0.777003 0.538134 0.477084 11.00000 0.02304 0.02537 = 0.02068 0.00238 -0.00061 0.00133 AFIX 23 H9A 2 0.895132 0.551451 0.479377 11.00000 -1.20000 H9B 2 0.754854 0.448951 0.488347 11.00000 -1.20000 AFIX 0 C22 1 0.304076 0.487210 0.540772 11.00000 0.02579 0.02476 = 0.03446 0.00073 0.00302 -0.00008 AFIX 43 H22 2 0.233843 0.557617 0.536451 11.00000 -1.20000 AFIX 0 C2 1 0.748319 0.613178 0.594051 11.00000 0.02915 0.02726 = 0.02377 0.00012 0.00077 -0.00450 C21 1 0.366555 0.455947 0.600554 11.00000 0.03166 0.03045 = 0.02921 -0.00151 0.00431 -0.00083 AFIX 43 H21 2 0.336567 0.504399 0.637186 11.00000 -1.20000 AFIX 0 C11 1 0.770176 0.456548 0.365985 11.00000 0.02783 0.01967 = 0.03073 -0.00361 0.00181 0.00170 AFIX 23 H11A 2 0.718201 0.376989 0.380032 11.00000 -1.20000 H11B 2 0.888617 0.444815 0.367943 11.00000 -1.20000 AFIX 0 C3 1 0.881032 0.539616 0.611720 11.00000 0.03219 0.03899 = 0.02604 0.00181 -0.00281 -0.00106 AFIX 43 H3 2 0.941075 0.496125 0.579640 11.00000 -1.20000 AFIX 0 C15 1 0.787344 0.685774 0.385054 11.00000 0.02768 0.01967 = 0.02285 0.00285 0.00223 -0.00318 AFIX 23 H15A 2 0.906664 0.684809 0.387530 11.00000 -1.20000 H15B 2 0.747374 0.756629 0.411783 11.00000 -1.20000 AFIX 0 C18 1 0.512833 0.284124 0.553596 11.00000 0.02742 0.02922 = 0.03237 0.00822 0.00284 0.00432 AFIX 43 H18 2 0.585289 0.215075 0.557770 11.00000 -1.20000 AFIX 0 C7 1 0.660083 0.676291 0.641398 11.00000 0.04403 0.03316 = 0.03057 -0.00329 0.00485 0.00042 AFIX 43 H7 2 0.570043 0.726920 0.629734 11.00000 -1.20000 AFIX 0 C20 1 0.543202 0.323583 0.672834 11.00000 0.04518 0.05061 = 0.02811 0.01035 -0.00329 0.00039 AFIX 137 H20A 2 0.568812 0.401920 0.695813 11.00000 -1.50000 H20B 2 0.641932 0.273898 0.667042 11.00000 -1.50000 H20C 2 0.464912 0.274585 0.697902 11.00000 -1.50000 AFIX 0 C4 1 0.925593 0.529860 0.676307 11.00000 0.04230 0.04819 = 0.03381 0.00873 -0.01115 -0.00414 AFIX 43 H4 2 1.016277 0.480130 0.688179 11.00000 -1.20000 AFIX 0 C5 1 0.837969 0.592456 0.723052 11.00000 0.05790 0.05347 = 0.02440 0.00212 -0.00695 -0.01467 AFIX 43 H5 2 0.868893 0.586107 0.767029 11.00000 -1.20000 AFIX 0 C12 1 0.720057 0.486884 0.297632 11.00000 0.03658 0.03207 = 0.02707 -0.00846 0.00287 -0.00072 AFIX 23 H12A 2 0.754940 0.417657 0.268743 11.00000 -1.20000 H12B 2 0.600920 0.492579 0.295420 11.00000 -1.20000 AFIX 0 C6 1 0.704732 0.664682 0.705946 11.00000 0.05980 0.04223 = 0.02892 -0.00735 0.00680 -0.00865 AFIX 43 H6 2 0.643741 0.706363 0.738365 11.00000 -1.20000 AFIX 0 H10 2 0.613505 0.565990 0.407728 11.00000 0.03226 HKLF 4 REM b12b_a.res in Pna2(1) REM wR2 = 0.0940, GooF = S = 1.027, Restrained GooF = 1.027 for all data REM R1 = 0.0365 for 4847 Fo > 4sig(Fo) and 0.0415 for all 5317 data REM 240 parameters refined using 1 restraints END WGHT 0.0516 0.3296 REM Highest difference peak 0.411, deepest hole -0.377, 1-sigma level 0.068 Q1 1 0.1264 0.4641 0.4138 11.00000 0.05 0.41 ; _shelx_res_checksum 30249 _shelx_hkl_file ; 2 0 0 5846.11 281.57 -2 0 0 7301.07 282.27 2 0 0 7136.39 282.67 -3 0 0 0.40 0.40 3 0 0 -0.30 0.80 -3 0 0 -0.10 0.30 3 0 0 0.20 0.30 3 0 0 0.40 0.40 -4 0 0 887.81 37.90 -4 0 0 864.61 38.10 4 0 0 925.31 38.00 4 0 0 866.91 38.10 4 0 0 916.41 38.60 5 0 0 -0.50 0.50 -5 0 0 -0.10 0.40 -5 0 0 -0.60 0.60 5 0 0 0.00 0.50 5 0 0 -0.50 0.90 -6 0 0 494.35 21.90 6 0 0 472.65 21.80 6 0 0 485.75 21.60 -6 0 0 502.95 21.60 7 0 0 0.40 0.80 -7 0 0 -0.30 0.90 7 0 0 -0.70 0.70 8 0 0 89.89 5.60 -8 0 0 85.29 5.70 9 0 0 1.90 1.50 -9 0 0 0.30 1.30 -10 0 0 -0.50 1.40 10 0 0 0.90 1.60 -11 0 0 -0.40 1.80 11 0 0 2.60 2.00 2 1 0 530.15 23.20 -2 1 0 543.15 23.00 2 1 0 538.15 23.00 -2 -1 0 544.35 23.10 2 -1 0 558.04 23.10 -2 -1 0 531.55 22.90 2 -1 0 539.65 23.00 -3 1 0 79.69 4.10 3 1 0 81.79 4.10 3 -1 0 82.59 4.10 3 -1 0 77.89 4.10 -3 -1 0 84.59 4.10 3 1 0 85.99 4.00 -3 -1 0 83.29 4.20 3 1 0 77.29 4.40 4 -1 0 0.50 0.60 -4 1 0 1.30 0.50 4 1 0 1.00 0.80 4 -1 0 1.10 0.60 4 1 0 0.50 0.40 -4 1 0 1.90 0.70 -4 -1 0 1.20 0.60 -4 -1 0 0.80 0.60 4 1 0 1.60 0.70 5 -1 0 240.18 11.40 -5 -1 0 240.18 11.40 5 1 0 249.97 11.20 -5 1 0 261.37 11.00 -5 1 0 244.28 11.50 5 -1 0 251.47 11.40 -5 -1 0 241.08 11.40 5 -1 0 252.07 12.00 5 1 0 229.08 11.90 5 1 0 241.88 11.40 -6 -1 0 3.20 1.10 6 -1 0 4.30 1.10 6 1 0 5.80 1.30 6 1 0 4.50 1.70 -6 -1 0 4.40 1.10 -6 1 0 4.60 1.20 6 1 0 4.60 1.00 6 -1 0 4.50 1.20 -7 -1 0 109.29 6.10 -7 1 0 106.69 6.30 7 -1 0 104.79 6.20 7 1 0 110.89 6.30 -7 -1 0 112.69 6.30 7 -1 0 112.19 6.10 8 -1 0 1.30 1.40 8 -1 0 0.10 1.00 8 1 0 0.40 1.10 -8 1 0 0.90 1.10 -8 -1 0 0.80 1.20 -9 1 0 15.50 2.80 9 1 0 17.30 2.70 9 -1 0 23.20 3.10 -9 -1 0 20.50 3.00 -10 1 0 1.30 1.80 10 1 0 0.50 1.50 10 -1 0 1.20 1.60 -10 -1 0 1.30 1.60 11 -1 0 3.80 2.20 -11 1 0 4.30 2.30 11 1 0 1.40 2.10 -11 -1 0 5.30 2.20 0 -2 0 3751.42 156.48 -1 -2 0 9999.00 374.26 -1 -2 0 8731.73 373.56 1 -2 0 9867.21 373.76 1 -2 0 7784.52 373.26 1 2 0 7858.51 373.26 -1 2 0 9442.55 373.36 2 2 0 2859.51 118.79 2 -2 0 3058.39 118.89 2 -2 0 2642.14 118.69 2 2 0 2727.13 118.89 -2 -2 0 2929.81 118.89 -2 2 0 2922.61 118.79 -2 -2 0 2732.73 118.59 -3 -2 0 919.81 39.00 3 2 0 914.31 39.20 3 -2 0 896.91 39.10 -3 -2 0 954.10 39.40 3 2 0 953.40 38.90 3 -2 0 916.41 39.30 3 2 0 909.61 39.50 -3 2 0 906.91 39.20 4 2 0 58.29 3.10 -4 2 0 60.29 3.50 4 2 0 58.59 3.40 4 -2 0 59.39 3.30 4 -2 0 61.19 3.50 -4 -2 0 52.49 3.40 -4 -2 0 58.69 3.30 4 2 0 60.99 3.80 -5 2 0 167.78 8.30 5 -2 0 165.78 8.20 5 -2 0 166.38 8.10 -5 -2 0 160.18 8.00 -5 -2 0 163.48 8.20 5 2 0 170.68 8.70 5 2 0 177.78 7.80 5 2 0 157.88 8.10 -6 2 0 166.38 8.70 -6 -2 0 172.88 8.50 6 2 0 164.68 9.30 6 2 0 171.08 8.60 6 -2 0 180.18 8.70 -6 -2 0 167.28 8.60 6 -2 0 170.88 8.50 6 2 0 167.88 8.10 -7 2 0 -0.80 0.70 7 2 0 -1.00 1.90 7 2 0 -0.30 0.90 -7 -2 0 0.00 0.90 7 -2 0 -0.20 0.70 7 -2 0 0.50 0.90 -7 -2 0 0.50 0.90 8 -2 0 98.79 6.00 8 -2 0 98.49 5.90 -8 2 0 97.79 6.20 -8 -2 0 92.39 5.90 8 2 0 96.89 6.10 -9 2 0 -0.20 1.30 9 2 0 -0.20 1.30 -9 -2 0 0.70 1.40 9 -2 0 -0.90 1.20 -10 2 0 1.30 1.80 10 -2 0 -2.10 1.30 -10 -2 0 1.30 1.70 10 2 0 0.60 1.60 -11 -2 0 -0.50 1.90 11 2 0 -1.00 1.70 11 -2 0 1.50 1.90 -11 2 0 0.40 2.10 0 -3 0 0.10 0.40 0 -3 0 0.00 0.30 0 -3 0 -0.30 0.30 -1 3 0 1855.31 77.89 -1 3 0 1936.51 77.99 1 3 0 1955.90 77.99 -1 -3 0 1765.32 78.19 1 -3 0 1942.81 78.19 1 3 0 1719.93 77.89 1 -3 0 1817.52 78.09 1 3 0 1934.71 77.99 -1 -3 0 1825.82 78.09 -2 -3 0 4.20 0.90 2 3 0 3.70 0.70 2 3 0 3.40 0.60 -2 -3 0 4.40 0.70 2 -3 0 3.80 0.70 2 -3 0 3.50 0.70 -2 3 0 4.00 0.70 2 3 0 4.60 0.80 3 3 0 312.57 13.10 3 -3 0 324.67 13.70 -3 -3 0 283.87 13.60 -3 -3 0 304.27 13.20 3 -3 0 295.97 13.40 3 3 0 289.77 13.50 3 3 0 285.27 13.60 -3 3 0 312.17 13.50 4 -3 0 267.17 12.30 4 3 0 271.27 12.80 4 -3 0 256.67 12.50 4 3 0 286.47 12.00 4 3 0 271.37 12.40 -4 -3 0 272.57 12.20 -4 -3 0 273.47 12.70 -4 3 0 270.37 12.50 5 3 0 67.09 3.60 5 3 0 74.89 4.60 5 -3 0 70.29 4.20 5 -3 0 63.39 3.90 -5 -3 0 59.39 4.10 5 3 0 68.19 4.10 -5 3 0 65.49 4.10 -5 -3 0 68.89 3.90 6 -3 0 50.49 3.80 6 -3 0 58.99 3.80 6 3 0 57.89 3.80 6 3 0 65.29 4.60 -6 3 0 50.39 3.80 -6 -3 0 55.69 3.60 -6 -3 0 53.89 3.90 7 -3 0 63.19 4.50 7 -3 0 71.39 4.60 7 3 0 72.19 4.70 -7 -3 0 70.89 4.50 7 3 0 71.19 5.60 -7 -3 0 73.69 4.80 -7 3 0 62.09 4.70 -8 -3 0 0.70 1.00 -8 3 0 0.80 1.20 -8 -3 0 0.50 1.10 8 -3 0 -0.60 1.20 8 -3 0 -0.50 1.00 8 3 0 1.70 1.30 -9 3 0 64.09 5.10 9 -3 0 64.69 4.90 9 -3 0 64.39 4.80 9 3 0 65.69 5.10 -9 -3 0 65.09 4.90 -10 3 0 60.09 6.00 -10 -3 0 58.39 5.50 10 -3 0 64.49 5.20 10 3 0 55.49 5.40 11 3 0 0.40 2.10 -11 3 0 -1.00 2.30 11 -3 0 2.80 2.30 0 -4 0 420.76 18.00 0 -4 0 419.26 17.70 0 -4 0 457.95 18.10 0 -4 0 359.16 17.90 1 4 0 5.60 0.80 1 4 0 7.10 0.90 1 -4 0 6.40 0.90 -1 4 0 6.90 0.90 -1 -4 0 5.80 0.90 1 -4 0 7.80 1.00 1 -4 0 6.40 0.90 1 4 0 7.30 0.80 -1 -4 0 7.00 0.80 -1 -4 0 6.40 1.00 -1 4 0 6.30 0.60 2 -4 0 57.69 3.20 2 4 0 54.79 3.10 2 4 0 53.29 3.10 -2 -4 0 63.89 3.00 2 4 0 59.49 3.10 -2 4 0 56.19 3.10 -2 -4 0 57.79 3.30 -3 -4 0 244.18 10.90 3 4 0 251.07 11.40 -3 -4 0 242.18 11.50 3 4 0 233.58 11.30 -3 4 0 234.78 11.20 3 4 0 269.77 11.00 3 -4 0 227.88 11.40 3 -4 0 260.27 11.30 4 -4 0 50.69 3.10 4 4 0 54.59 3.60 -4 4 0 47.30 3.20 4 -4 0 43.30 3.20 -4 -4 0 46.10 3.40 4 4 0 49.20 3.20 4 4 0 54.99 2.90 -4 -4 0 47.80 2.90 -5 4 0 0.90 0.80 5 -4 0 0.30 0.80 -5 -4 0 -0.20 0.70 5 4 0 -0.30 0.90 5 -4 0 1.20 0.70 -5 -4 0 0.30 0.60 5 4 0 0.30 0.70 6 -4 0 130.49 7.00 6 4 0 130.29 7.10 -6 4 0 136.19 7.20 6 4 0 128.89 7.60 -6 -4 0 130.59 7.30 6 -4 0 127.89 7.10 -6 -4 0 126.09 6.70 -7 -4 0 1.50 1.10 7 4 0 1.20 1.60 7 4 0 1.20 1.20 -7 4 0 0.40 1.00 -7 -4 0 0.30 0.90 7 -4 0 1.30 1.00 7 -4 0 0.90 1.00 8 4 0 62.09 4.70 8 -4 0 61.39 4.40 8 -4 0 55.39 4.30 -8 4 0 56.19 4.50 -8 -4 0 57.99 4.20 -8 -4 0 55.69 4.60 -9 -4 0 14.30 2.80 -9 4 0 20.70 3.20 9 -4 0 18.60 2.80 9 4 0 19.00 3.10 -9 -4 0 17.80 3.20 9 -4 0 21.20 3.10 10 4 0 1.10 1.80 -10 4 0 2.80 2.10 10 -4 0 3.20 1.90 -11 4 0 -3.80 2.20 11 4 0 1.20 2.30 0 -5 0 -0.20 0.50 0 -5 0 -0.10 0.50 0 -5 0 0.10 0.50 0 -5 0 0.10 0.40 1 5 0 508.45 21.30 1 5 0 476.55 20.90 1 5 0 434.76 21.10 -1 -5 0 467.05 21.30 1 -5 0 483.95 21.40 1 -5 0 495.85 21.30 -1 -5 0 496.15 20.90 -1 5 0 508.85 21.10 -1 5 0 485.75 20.60 1 -5 0 519.75 21.20 -1 -5 0 493.85 21.50 2 5 0 0.10 0.40 -2 -5 0 0.40 0.60 2 -5 0 0.50 0.60 -2 -5 0 0.50 0.60 2 -5 0 -0.40 0.50 2 -5 0 0.50 0.50 -2 5 0 1.40 0.60 -2 -5 0 0.10 0.50 2 5 0 1.10 0.50 2 5 0 0.90 0.60 -2 5 0 -0.60 0.40 -3 -5 0 5.90 1.30 3 5 0 6.00 1.20 3 5 0 5.40 0.90 3 5 0 5.80 1.20 3 -5 0 5.90 1.10 -3 5 0 7.70 1.20 3 -5 0 6.70 1.30 -3 -5 0 8.10 1.00 -4 5 0 306.37 13.60 4 5 0 286.47 13.70 4 5 0 305.87 13.10 4 -5 0 282.47 13.40 4 5 0 278.77 13.50 -4 -5 0 310.47 13.10 -4 -5 0 290.57 13.90 4 -5 0 270.37 13.70 5 -5 0 25.00 2.50 -5 -5 0 24.10 2.10 5 -5 0 28.00 2.90 5 5 0 27.90 2.80 -5 -5 0 27.10 3.10 5 5 0 31.10 3.30 -5 5 0 21.10 2.50 -6 5 0 40.90 3.30 6 5 0 40.30 4.30 -6 -5 0 35.80 3.40 -6 -5 0 41.90 3.00 6 5 0 38.60 3.30 6 -5 0 38.40 3.30 6 -5 0 41.30 3.20 7 -5 0 27.90 3.20 -7 -5 0 22.50 3.00 7 -5 0 29.30 3.10 7 5 0 23.90 3.60 -7 5 0 23.70 3.00 7 5 0 26.30 3.20 -7 -5 0 28.10 2.90 8 5 0 44.00 4.50 -8 5 0 47.30 4.00 8 -5 0 42.20 4.30 8 5 0 46.80 5.30 -8 -5 0 42.80 4.60 8 -5 0 43.30 4.20 -9 -5 0 2.50 1.60 9 -5 0 0.00 1.30 9 5 0 0.80 1.50 9 -5 0 -0.70 1.20 -9 5 0 2.70 1.70 10 -5 0 67.79 7.00 10 -5 0 60.09 5.80 -10 5 0 66.69 5.50 10 5 0 60.19 5.90 -11 5 0 -1.30 2.40 0 -6 0 495.65 20.30 0 -6 0 436.56 20.20 0 6 0 457.85 20.20 0 6 0 433.86 19.40 0 -6 0 444.46 20.20 0 -6 0 484.75 19.80 0 6 0 445.86 20.20 1 -6 0 214.88 10.10 1 6 0 218.28 10.10 -1 -6 0 232.98 9.60 -1 6 0 216.58 9.80 1 6 0 209.48 9.90 -1 -6 0 228.38 10.30 1 6 0 196.28 9.50 -1 -6 0 216.18 10.20 -1 6 0 213.68 9.30 1 -6 0 205.48 10.20 1 -6 0 209.68 9.90 2 6 0 28.50 2.10 2 -6 0 26.50 1.90 -2 6 0 27.30 1.90 2 6 0 27.80 2.00 2 6 0 26.20 2.00 -2 -6 0 30.40 1.90 -2 -6 0 24.90 2.20 -2 -6 0 27.40 2.40 2 -6 0 27.70 2.20 -2 6 0 21.10 1.90 3 6 0 22.90 1.90 -3 6 0 23.50 2.20 -3 -6 0 21.10 2.60 3 6 0 18.10 2.20 3 -6 0 20.50 2.10 3 -6 0 25.80 2.60 -3 -6 0 22.10 1.70 3 6 0 16.70 2.00 4 -6 0 9.00 1.70 4 -6 0 8.60 1.50 4 6 0 10.70 1.80 -4 -6 0 10.00 1.80 -4 6 0 9.50 1.60 -4 -6 0 11.50 1.50 4 6 0 9.80 1.80 5 -6 0 80.39 4.70 5 -6 0 72.29 4.90 -5 -6 0 69.19 5.10 -5 6 0 79.99 4.80 5 6 0 74.89 5.10 5 6 0 75.59 4.80 6 -6 0 21.60 2.80 6 -6 0 16.80 2.40 -6 -6 0 18.50 2.80 -6 6 0 15.70 2.30 6 6 0 14.00 2.70 6 6 0 21.70 2.80 7 6 0 58.39 5.60 -7 6 0 61.29 4.50 7 -6 0 46.50 4.20 -7 -6 0 62.69 4.80 7 6 0 60.79 4.50 7 -6 0 49.80 4.10 8 -6 0 20.60 3.00 -8 6 0 19.10 2.90 8 6 0 12.70 2.40 8 6 0 14.90 3.10 -8 -6 0 10.60 2.60 8 -6 0 19.80 2.80 9 6 0 2.30 1.60 9 -6 0 1.80 1.50 -9 -6 0 -0.80 1.50 9 -6 0 1.90 1.60 -9 6 0 0.40 1.40 10 -6 0 2.90 2.00 -10 6 0 2.60 1.70 -10 -6 0 1.50 2.70 10 6 0 4.30 2.20 0 7 0 0.00 0.60 0 7 0 -0.20 0.40 0 -7 0 0.40 0.50 0 -7 0 -0.50 0.60 0 7 0 -0.90 0.50 0 -7 0 -1.00 0.50 -1 7 0 14.30 1.60 1 -7 0 17.10 1.90 1 -7 0 17.10 2.00 1 -7 0 17.70 2.10 1 7 0 14.60 1.80 1 7 0 15.20 1.50 -1 -7 0 18.00 2.20 -1 7 0 15.50 1.20 1 7 0 12.10 1.70 -1 -7 0 17.60 2.00 -1 -7 0 16.20 1.40 2 7 0 81.49 4.40 2 -7 0 73.69 4.60 -2 7 0 81.49 4.40 2 7 0 80.89 4.50 2 -7 0 83.99 4.90 2 -7 0 81.49 4.30 -2 -7 0 80.49 4.20 -2 -7 0 82.89 4.80 2 7 0 72.69 4.40 -2 -7 0 78.89 5.00 3 7 0 8.50 1.40 3 -7 0 6.20 1.30 -3 7 0 4.80 1.20 3 7 0 7.00 1.30 3 7 0 6.90 1.40 -3 -7 0 6.00 1.50 3 -7 0 9.90 1.80 3 7 0 7.20 1.40 4 -7 0 135.99 7.20 4 -7 0 148.59 7.80 4 7 0 129.89 7.30 -4 -7 0 128.19 7.70 -4 7 0 129.89 7.20 4 7 0 142.59 7.50 5 7 0 3.20 1.30 5 7 0 2.80 1.50 5 -7 0 4.00 1.50 -5 -7 0 3.70 1.40 5 -7 0 6.70 1.50 -5 7 0 2.20 1.10 -6 7 0 43.60 3.50 6 -7 0 43.90 3.80 6 7 0 39.00 4.00 6 7 0 44.70 4.60 6 -7 0 32.00 3.40 -6 -7 0 38.40 4.30 7 -7 0 -0.40 1.10 -7 7 0 1.70 1.20 7 7 0 -0.40 1.10 7 -7 0 -0.20 1.20 7 7 0 -2.20 1.30 -7 -7 0 -0.80 1.20 8 -7 0 8.80 2.10 8 7 0 9.60 2.80 8 7 0 9.50 2.30 -8 7 0 5.60 1.90 -8 -7 0 8.40 2.50 8 -7 0 7.20 2.00 -9 -7 0 5.10 2.30 -9 7 0 3.20 1.80 9 -7 0 0.10 1.70 9 -7 0 6.50 2.30 9 7 0 3.10 1.90 10 7 0 26.60 4.30 -10 7 0 24.40 4.00 10 -7 0 24.60 4.00 -10 -7 0 30.90 4.60 0 8 0 521.45 23.00 0 -8 0 572.64 24.10 0 -8 0 531.75 24.00 0 8 0 559.04 24.10 0 -8 0 543.55 23.30 0 8 0 496.65 23.80 1 -8 0 38.70 3.00 -1 -8 0 39.90 3.10 1 -8 0 40.90 2.90 -1 8 0 36.20 2.50 1 8 0 34.60 2.80 1 8 0 36.50 2.40 -1 -8 0 44.20 3.30 1 8 0 39.50 3.00 1 -8 0 33.80 3.00 2 8 0 31.50 2.50 2 -8 0 36.80 3.10 2 -8 0 36.20 2.90 -2 -8 0 34.10 2.90 -2 8 0 35.80 2.50 -2 -8 0 35.70 3.20 2 8 0 32.20 2.70 2 8 0 32.10 2.60 -3 8 0 65.59 4.30 -3 -8 0 76.29 5.10 3 -8 0 73.19 4.60 3 8 0 76.09 4.90 3 8 0 70.69 4.40 3 8 0 64.69 4.60 3 8 0 79.79 4.90 3 -8 0 78.79 5.00 -4 8 0 2.40 1.20 4 8 0 4.70 1.50 -4 -8 0 3.50 1.50 4 -8 0 3.70 1.50 4 8 0 4.00 1.30 4 -8 0 4.80 1.40 5 8 0 56.99 4.30 5 -8 0 61.09 4.30 -5 8 0 54.89 4.10 5 -8 0 62.79 4.60 5 8 0 55.99 4.60 -5 -8 0 55.39 4.60 -6 8 0 33.40 3.60 -6 -8 0 33.40 4.20 6 8 0 36.80 4.40 6 -8 0 36.40 3.70 6 -8 0 38.70 4.20 6 8 0 29.80 3.50 7 8 0 -0.10 1.70 7 -8 0 -0.40 1.20 7 8 0 1.00 1.30 -7 8 0 1.50 1.40 7 -8 0 0.00 1.30 -7 -8 0 -0.90 1.30 -8 8 0 7.30 2.20 8 -8 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12.80 2.50 7 -9 0 11.90 2.60 7 9 0 14.00 2.80 7 -9 0 14.50 2.70 7 9 0 10.80 2.90 8 -9 0 2.40 1.70 8 -9 0 0.30 1.90 8 9 0 0.10 1.50 -8 -9 0 -0.90 1.80 -8 9 0 1.50 1.70 8 9 0 0.00 2.30 9 9 0 -3.80 2.60 -9 -9 0 -1.10 1.60 9 -9 0 1.20 1.80 9 9 0 -0.10 1.90 -9 9 0 -1.60 1.50 0 10 0 52.39 3.30 0 -10 0 60.59 4.30 0 10 0 60.49 4.20 0 10 0 53.69 4.20 0 -10 0 53.59 4.10 -1 10 0 0.30 1.10 -1 -10 0 0.60 1.20 -1 10 0 1.20 0.70 -1 -10 0 0.00 1.10 1 10 0 1.60 1.10 1 10 0 0.90 1.10 1 -10 0 1.50 1.20 1 10 0 0.10 0.70 -1 10 0 2.50 1.20 2 10 0 57.19 3.90 2 10 0 63.59 4.60 -2 -10 0 61.09 4.50 -2 -10 0 56.59 4.60 2 -10 0 60.39 4.70 2 -10 0 60.19 4.40 2 10 0 57.19 4.80 3 -10 0 15.30 2.40 3 10 0 15.00 2.10 3 10 0 12.90 2.30 3 -10 0 15.10 2.60 -3 -10 0 16.80 2.90 4 -10 0 25.50 3.50 4 10 0 20.60 2.90 4 -10 0 21.90 3.00 -4 10 0 20.90 2.70 -4 -10 0 23.20 3.40 4 10 0 22.40 2.90 5 10 0 15.60 2.90 -5 -10 0 18.30 3.40 5 10 0 22.60 3.30 5 -10 0 22.30 3.00 5 -10 0 25.20 3.60 -5 10 0 17.90 2.60 -6 10 0 17.30 2.70 6 -10 0 22.50 3.10 -6 -10 0 15.80 3.20 6 10 0 20.70 3.60 6 10 0 18.30 3.10 6 -10 0 25.20 3.70 -7 -10 0 4.50 2.10 7 -10 0 4.90 2.20 7 10 0 5.00 2.10 -7 10 0 3.70 1.80 7 -10 0 1.40 1.50 7 10 0 6.90 2.80 8 10 0 29.90 4.90 -8 -10 0 28.20 4.50 -8 10 0 32.40 4.30 8 10 0 39.10 4.90 8 -10 0 32.40 4.60 0 11 0 -0.80 1.00 0 11 0 0.60 0.80 0 -11 0 -1.50 1.20 0 11 0 2.80 1.40 0 -11 0 0.70 1.30 1 11 0 3.90 1.40 -1 11 0 2.50 1.40 1 11 0 0.90 1.40 1 -11 0 3.80 1.70 1 11 0 3.60 1.20 -1 11 0 1.50 0.90 -1 -11 0 3.80 1.80 -1 11 0 5.10 1.80 -1 -11 0 1.70 1.50 -2 -11 0 4.00 1.60 -2 -11 0 6.40 1.90 -2 11 0 6.40 1.30 -2 11 0 6.50 1.70 2 -11 0 4.50 1.70 2 11 0 4.90 1.40 -2 11 0 6.70 1.90 3 -11 0 -1.80 1.00 3 11 0 0.10 0.90 3 -11 0 -0.10 1.30 3 11 0 -1.50 0.90 -3 -11 0 0.30 1.60 4 11 0 1.80 1.50 4 -11 0 1.50 1.40 -4 -11 0 1.30 1.80 4 11 0 1.30 1.30 4 -11 0 3.20 1.70 5 -11 0 32.80 4.30 5 11 0 28.80 3.80 5 11 0 23.20 3.50 -5 -11 0 30.80 4.50 5 -11 0 32.70 3.90 6 11 0 5.10 2.50 6 11 0 2.60 1.60 -6 -11 0 2.00 2.30 6 -11 0 5.70 2.40 6 -11 0 4.40 2.00 -7 11 0 8.60 2.80 7 11 0 7.80 2.70 7 -11 0 5.50 2.20 7 11 0 6.90 3.30 -7 -11 0 4.00 2.30 0 12 0 161.48 8.20 0 -12 0 162.98 9.40 0 12 0 159.38 9.40 0 12 0 164.08 9.30 -1 12 0 15.90 2.10 -1 12 0 14.20 2.70 1 -12 0 15.50 2.80 -1 12 0 13.50 2.90 1 12 0 16.50 2.20 -1 -12 0 17.70 3.00 -1 -12 0 16.40 2.80 -2 -12 0 41.40 4.50 -2 12 0 55.29 4.60 2 -12 0 49.99 5.00 -2 12 0 57.89 4.90 -2 -12 0 48.20 5.10 2 12 0 48.30 3.80 -2 12 0 45.90 3.50 -3 12 0 0.00 1.20 3 -12 0 1.10 1.60 3 12 0 -0.30 1.30 -3 -12 0 -0.20 1.70 3 12 0 -0.10 1.20 -3 12 0 1.80 1.70 -3 12 0 -0.20 1.10 4 -12 0 41.00 4.50 -4 -12 0 40.70 5.10 4 12 0 48.30 4.80 4 -12 0 44.40 5.20 4 12 0 52.59 5.40 5 12 0 -1.90 1.70 5 -12 0 1.40 1.70 5 -12 0 -1.20 1.40 5 12 0 0.00 1.40 -5 -12 0 1.80 2.00 6 12 0 68.09 5.80 -6 -12 0 75.49 7.70 6 -12 0 78.29 7.60 6 12 0 81.99 7.50 6 -12 0 66.79 6.40 0 13 0 -1.20 1.70 0 13 0 1.00 1.10 0 -13 0 1.10 1.50 0 13 0 -0.40 1.70 1 13 0 0.10 1.20 -1 13 0 0.00 1.70 1 -13 0 -0.80 1.50 -1 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-0.80 0.80 -7 0 3 -0.30 1.00 7 0 3 1.50 1.10 7 0 -3 -0.40 0.90 -8 0 -3 162.28 8.80 8 0 -3 154.88 8.40 8 0 3 147.29 8.40 8 0 -3 154.88 8.50 -8 0 3 152.88 8.30 -9 0 3 -0.50 1.30 -9 0 -3 0.40 1.40 9 0 -3 0.80 1.40 9 0 3 0.40 1.20 10 0 3 2.20 1.80 -10 0 3 0.90 1.60 10 0 -3 -1.00 1.50 -10 0 -3 -0.40 1.50 -11 0 -3 -0.30 1.70 -11 0 3 -1.50 1.80 11 0 3 2.20 2.00 0 1 -3 268.37 11.30 0 -1 -3 259.87 11.30 0 1 3 244.88 10.50 0 1 -3 246.18 11.30 -1 -1 -3 1839.82 76.39 1 1 -3 1896.21 76.39 -1 1 3 1868.11 79.19 1 -1 3 1859.31 79.19 -1 -1 -3 1750.32 76.29 1 -1 -3 1917.21 76.39 -1 1 -3 1829.92 76.69 -1 1 -3 1771.52 76.29 -1 1 -3 1798.92 76.29 1 -1 -3 1782.02 76.29 1 1 3 1892.21 79.19 -1 1 -3 1819.02 76.29 -1 -1 3 1911.11 79.39 1 1 3 1935.91 79.29 2 1 -3 724.53 29.70 2 -1 3 662.43 28.60 2 -1 3 661.53 28.70 -2 1 3 719.23 28.60 2 1 -3 679.43 29.40 2 1 -3 675.43 29.30 -2 -1 -3 715.73 29.50 -2 -1 -3 706.33 29.50 -2 1 3 696.23 28.70 -2 -1 3 661.03 28.80 -2 -1 3 633.94 28.40 2 -1 -3 663.13 29.50 2 1 3 676.53 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111.19 5.80 -3 -2 -3 110.79 5.60 3 2 3 111.59 5.50 3 -2 -3 119.89 5.70 -3 -2 3 109.39 5.20 -3 -2 3 107.59 5.60 -3 2 -3 109.89 5.50 3 -2 -3 112.59 5.30 3 2 3 111.89 5.80 -4 2 3 70.99 4.10 4 2 -3 72.79 3.90 -4 -2 -3 71.79 3.90 4 2 -3 72.29 3.80 4 -2 3 74.79 4.20 -4 -2 -3 67.29 4.00 -4 2 3 78.29 3.80 4 -2 3 76.29 4.10 4 2 -3 68.79 4.30 4 -2 -3 72.29 3.70 4 -2 -3 64.69 4.00 4 2 3 77.39 4.60 -4 -2 3 74.29 4.30 4 2 3 78.59 4.30 -4 2 -3 65.19 3.90 -4 -2 3 70.39 3.90 5 2 -3 4.30 1.00 5 -2 3 3.40 0.90 -5 -2 -3 2.70 1.00 -5 2 3 5.70 1.20 5 2 -3 7.30 1.70 -5 2 3 4.90 0.90 -5 -2 -3 4.60 1.00 5 -2 3 4.40 1.10 5 2 -3 6.90 1.20 5 2 3 5.50 1.50 -5 2 -3 4.40 1.10 5 -2 -3 4.80 1.20 5 -2 -3 6.40 1.10 -5 -2 3 5.60 1.10 5 2 3 6.40 1.30 -5 -2 3 4.10 1.10 6 2 -3 102.69 5.40 6 -2 3 104.39 5.60 6 2 -3 107.69 6.40 6 2 -3 98.89 5.50 -6 -2 -3 100.49 5.60 -6 2 3 103.29 5.80 6 -2 3 96.39 5.70 -6 -2 -3 98.59 5.60 6 2 3 106.79 6.50 -6 2 -3 91.79 5.60 6 -2 -3 89.99 5.60 6 2 3 94.69 5.70 6 -2 -3 100.49 5.40 -6 -2 3 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100.39 4.80 0 -3 -3 114.79 5.10 1 3 -3 40.80 2.60 1 3 -3 49.30 2.70 -1 -3 -3 47.60 2.60 1 -3 3 45.50 2.30 1 3 -3 41.00 2.60 -1 -3 -3 49.50 2.80 1 3 3 44.40 2.40 -1 3 -3 45.00 2.60 1 3 3 44.10 2.10 1 3 3 41.80 2.10 -1 3 -3 41.60 2.60 -1 3 -3 47.60 2.70 1 -3 -3 57.19 2.70 1 -3 -3 44.30 2.40 -1 3 -3 46.70 2.40 1 -3 -3 46.60 2.60 -1 -3 3 41.20 2.60 1 -3 -3 53.99 2.70 2 -3 3 493.35 21.20 -2 3 3 497.65 21.20 -2 -3 -3 494.55 22.50 2 -3 3 444.46 21.20 2 3 -3 500.95 22.40 2 3 -3 496.05 22.20 -2 3 3 505.55 20.90 -2 -3 -3 552.64 22.20 -2 -3 3 492.75 21.10 2 -3 -3 519.85 22.00 2 3 3 470.85 21.00 -2 3 -3 487.35 22.10 2 3 3 504.05 21.10 -2 -3 3 497.05 21.30 2 -3 -3 552.44 22.40 3 3 -3 117.89 6.10 3 -3 3 119.79 5.90 -3 3 3 112.69 5.80 3 3 -3 120.79 5.80 -3 -3 -3 105.49 5.90 3 -3 3 117.19 5.80 3 3 -3 119.09 5.80 -3 -3 -3 114.39 5.70 -3 3 3 122.59 5.40 3 3 3 116.49 5.80 -3 -3 3 100.19 5.90 -3 -3 3 119.99 5.40 -3 3 -3 114.79 5.70 3 -3 -3 125.49 6.00 3 -3 -3 113.89 5.50 3 3 3 117.99 5.90 -4 -3 -3 848.22 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2.30 -1 -8 -3 20.90 2.10 1 8 -3 16.80 2.10 -1 -8 -3 17.70 2.50 -1 8 -3 17.40 2.00 1 -8 -3 23.00 2.30 1 8 3 18.60 2.10 1 8 3 18.60 1.30 1 -8 -3 21.90 2.40 -1 -8 3 18.20 2.30 1 -8 -3 20.70 2.30 -1 -8 3 21.30 2.50 1 -8 -3 23.70 2.60 -1 8 -3 21.10 2.60 1 8 3 19.70 2.30 -1 8 -3 17.20 2.40 -2 -8 -3 6.90 1.70 2 8 -3 8.00 1.60 2 -8 3 9.90 1.70 -2 8 3 8.70 1.00 -2 -8 -3 5.60 1.40 2 8 -3 6.80 1.50 -2 -8 -3 7.80 1.40 -2 8 3 5.80 1.30 2 8 -3 8.70 1.60 2 8 3 7.90 1.60 2 8 3 8.60 1.50 -2 -8 3 7.20 1.70 -2 -8 3 7.50 1.60 2 8 3 7.40 1.50 2 -8 -3 5.40 1.50 -2 8 -3 4.10 1.30 2 -8 -3 6.40 1.50 -2 8 -3 7.60 1.40 -2 8 -3 7.00 1.70 2 -8 -3 6.90 1.40 2 8 3 4.80 1.00 -2 8 -3 4.10 1.20 -3 8 3 39.70 3.10 3 -8 3 45.60 3.60 -3 -8 -3 40.70 3.70 3 -8 3 39.50 3.20 3 8 -3 40.90 3.20 3 8 -3 39.50 3.40 3 -8 -3 39.30 3.90 3 8 3 37.20 3.10 3 8 3 39.50 2.90 -3 -8 3 27.70 3.30 3 -8 -3 40.20 3.10 -3 8 -3 43.40 3.10 -3 -8 3 36.90 3.10 4 8 -3 5.60 1.80 4 8 -3 7.10 2.10 4 -8 3 8.50 1.90 4 8 -3 5.50 1.60 -4 -8 -3 7.80 2.10 4 -8 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29.90 3.30 -3 9 3 22.10 2.60 3 -9 3 30.20 3.60 3 9 -3 29.20 3.20 -3 -9 -3 28.00 3.60 -3 9 -3 28.00 3.50 -3 -9 3 27.00 3.40 -3 9 -3 34.10 2.90 -3 -9 3 27.80 3.20 3 9 3 27.00 2.70 -3 9 -3 29.00 3.40 3 -9 -3 30.80 3.50 3 -9 -3 32.40 3.20 3 9 3 30.10 3.30 4 -9 3 114.89 7.20 -4 9 3 105.59 6.50 4 9 -3 135.19 7.70 4 9 -3 115.99 7.30 -4 -9 -3 119.09 7.90 4 -9 3 117.49 6.90 -4 9 -3 130.69 7.10 4 9 3 126.89 7.10 4 9 3 115.49 6.70 4 -9 -3 139.39 7.80 -4 -9 3 116.79 7.40 4 -9 -3 128.79 7.20 5 9 -3 8.60 2.20 -5 9 3 6.30 1.60 -5 -9 -3 6.60 2.10 5 -9 3 6.80 2.00 5 9 -3 9.10 2.30 5 -9 3 7.50 1.90 5 9 3 7.90 1.90 5 -9 -3 7.70 1.90 -5 9 -3 11.30 2.00 -5 -9 3 8.20 2.10 5 -9 -3 8.80 2.20 5 9 3 9.60 2.20 -6 9 3 20.60 3.00 6 -9 3 18.10 2.90 -6 -9 -3 21.40 3.50 6 9 -3 18.60 3.00 6 9 -3 20.40 3.50 6 -9 3 21.60 3.30 6 9 3 20.50 3.30 6 -9 -3 20.60 3.30 6 9 3 17.00 2.70 -6 -9 3 19.80 3.40 -6 9 -3 24.30 3.10 -7 9 3 7.00 2.10 7 -9 3 5.50 2.10 7 -9 3 8.90 2.20 7 9 -3 8.50 3.00 -7 -9 -3 14.70 3.10 7 9 -3 7.00 2.30 7 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21.70 3.50 6 10 -3 22.20 3.30 6 -10 3 21.20 3.20 6 10 -3 14.70 3.30 -6 10 3 16.90 2.80 -6 10 -3 18.50 3.40 6 -10 -3 19.20 3.40 6 10 3 23.10 3.30 -6 -10 3 23.30 3.80 6 10 3 15.30 3.10 7 -10 3 18.30 3.10 -7 10 3 12.30 2.90 7 10 -3 13.20 2.80 -7 -10 -3 16.10 3.30 7 10 -3 13.10 3.40 7 -10 3 13.40 2.80 -7 -10 3 13.30 3.00 7 -10 -3 17.90 3.30 7 10 3 19.50 3.30 -7 10 -3 9.40 2.60 7 10 3 15.70 3.60 8 -10 3 32.20 4.20 8 10 -3 31.80 5.20 8 10 -3 39.20 5.00 8 -10 3 31.00 4.60 -8 -10 -3 28.50 4.60 -8 10 3 29.90 4.10 -8 -10 3 25.60 4.30 8 10 3 29.30 5.00 8 10 3 25.20 3.90 -8 10 -3 29.80 4.20 8 -10 -3 30.50 4.60 0 11 -3 21.80 3.00 0 -11 -3 28.80 3.60 0 11 -3 21.20 3.10 0 11 3 15.00 2.40 0 -11 3 13.60 2.50 0 11 3 16.10 1.50 0 11 -3 16.00 2.30 0 11 3 16.50 2.50 0 -11 -3 17.50 2.70 1 11 -3 133.59 7.60 -1 -11 -3 136.59 7.80 -1 11 3 120.29 5.70 -1 11 3 119.89 7.20 -1 -11 -3 142.49 8.20 -1 11 3 124.79 7.50 1 11 -3 125.09 7.20 1 -11 3 116.79 7.40 1 11 -3 142.49 8.00 -1 11 -3 117.59 7.00 1 -11 -3 135.59 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14 -5 18.00 3.50 -3 14 5 27.30 4.50 -3 14 -5 16.00 3.60 -3 14 -5 27.50 4.30 3 14 5 30.10 3.40 -3 -14 5 28.00 4.60 -3 14 -5 27.20 3.70 3 14 5 29.00 4.20 0 0 -6 1205.08 52.59 0 0 6 1154.18 49.50 0 0 6 1186.18 49.50 0 0 -6 1296.67 52.69 -1 0 -6 0.40 0.40 -1 0 6 0.80 0.60 -1 0 -6 0.70 0.40 1 0 6 0.10 0.30 -1 0 6 -0.20 0.30 1 0 -6 0.80 0.40 1 0 -6 -0.40 0.40 1 0 6 0.20 0.50 1 0 6 0.30 0.40 -2 0 6 1304.77 56.19 2 0 6 1337.57 55.99 2 0 -6 1352.16 57.79 2 0 6 1323.17 56.39 2 0 -6 1363.36 57.59 2 0 6 1347.67 56.09 -2 0 -6 1354.46 57.69 -2 0 -6 1346.17 57.39 -2 0 -6 1420.66 57.39 3 0 -6 0.20 0.50 -3 0 -6 0.80 0.50 -3 0 6 0.30 0.50 -3 0 -6 -0.20 0.90 -3 0 -6 0.40 0.40 3 0 6 0.60 0.80 3 0 6 0.40 0.50 -3 0 6 1.30 0.50 3 0 -6 -0.10 0.30 -3 0 -6 0.80 0.60 -3 0 -6 0.30 0.40 4 0 6 217.68 10.30 -4 0 6 226.18 10.20 -4 0 -6 234.58 10.50 4 0 -6 223.78 10.70 4 0 -6 240.48 11.10 4 0 -6 218.08 10.10 4 0 6 214.98 10.80 -4 0 6 207.48 10.30 -4 0 -6 217.58 10.60 4 0 6 228.98 9.80 -5 0 -6 0.30 0.70 5 0 6 0.50 0.60 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2.90 3 -1 -27 2.00 2.20 4 1 -27 -2.50 1.90 -4 1 27 -0.80 1.90 -4 -1 -27 -1.10 1.70 -4 1 -27 3.50 4.10 4 -1 -27 0.30 2.10 4 1 27 -5.20 2.20 -4 -1 27 -1.70 1.50 0 -2 27 -2.20 2.10 0 2 27 1.40 2.50 0 2 -27 0.90 2.10 0 -2 -27 0.10 1.70 1 -2 27 10.20 3.50 -1 2 27 8.30 2.80 1 2 -27 11.00 2.90 -1 -2 -27 9.60 2.60 -1 2 27 7.30 5.20 1 -2 -27 8.40 2.50 -1 -2 27 9.70 3.20 1 2 27 6.00 2.90 2 2 -27 -0.10 1.80 -2 -2 -27 2.20 1.90 -2 2 27 3.60 2.10 2 -2 27 3.40 2.60 -2 -2 27 -0.90 2.50 2 2 27 4.80 2.90 2 -2 -27 2.70 3.30 2 -2 -27 3.50 2.20 3 -2 27 7.90 4.20 -3 -2 -27 11.60 2.90 -3 2 27 3.70 2.50 3 2 -27 10.20 3.10 3 -2 -27 11.30 3.00 3 2 27 6.20 3.20 -3 -2 27 8.60 3.40 -4 2 27 0.50 2.40 -4 -2 -27 2.60 2.30 4 2 -27 -2.10 2.00 4 2 27 0.30 2.90 4 -2 -27 0.50 2.30 -4 -2 27 -2.20 2.10 0 3 27 3.10 2.70 0 3 -27 4.40 2.30 0 -3 -27 5.40 2.20 0 -3 27 8.00 3.10 0 3 27 5.10 3.20 -1 3 27 15.90 4.10 1 -3 27 24.70 4.30 -1 -3 -27 21.90 3.60 1 3 -27 19.00 3.70 -1 3 27 14.20 3.60 1 3 27 21.10 4.50 1 -3 -27 20.80 3.60 -1 -3 27 15.90 3.80 1 3 27 19.30 4.40 -2 -3 -27 5.70 2.30 -2 3 27 5.00 3.10 2 3 -27 5.50 2.50 2 -3 27 3.10 2.70 -2 3 27 2.10 2.10 2 3 27 0.80 3.40 2 3 27 12.40 3.70 -2 -3 27 3.90 2.80 2 -3 -27 5.80 2.20 3 3 -27 19.40 3.90 -3 3 27 14.00 3.60 -3 -3 -27 21.10 3.80 3 3 27 17.10 4.40 3 -3 -27 20.80 3.80 3 -3 -27 22.50 3.70 -3 -3 27 21.70 4.90 0 4 27 0.00 1.60 0 -4 27 -0.40 2.30 0 4 27 -0.70 2.40 0 4 -27 -2.80 1.50 0 -4 -27 0.10 1.60 1 4 -27 7.70 2.90 -1 -4 -27 3.30 1.90 -1 4 27 3.20 3.00 1 -4 27 3.00 2.60 -1 4 27 3.50 2.20 1 -4 -27 4.70 2.30 1 4 27 4.10 3.00 -1 -4 27 4.70 2.70 -1 4 -27 4.40 2.30 1 4 27 6.70 3.50 -2 4 27 6.20 2.70 2 4 -27 -1.50 1.80 -2 4 27 1.40 3.20 -2 -4 -27 0.50 2.00 2 4 27 8.10 3.60 -2 -4 27 5.00 2.90 2 4 27 5.40 3.50 2 -4 -27 6.10 2.40 3 4 -27 9.10 3.30 -3 -4 -27 3.70 2.60 -3 4 27 7.40 3.20 3 4 27 0.70 2.80 3 4 27 6.50 3.90 -3 -4 27 8.30 4.00 3 -4 -27 8.10 2.60 0 5 27 34.80 5.80 0 -5 -27 46.90 5.60 0 5 -27 41.40 5.50 0 5 27 45.30 6.00 0 -5 27 40.10 5.60 1 5 -27 4.50 2.50 -1 -5 -27 1.20 1.90 1 -5 27 2.50 2.90 -1 5 27 2.30 2.30 -1 5 27 5.70 3.60 1 -5 -27 3.30 2.20 -1 5 -27 6.30 2.70 -1 -5 27 3.80 2.80 1 5 27 9.30 3.70 1 5 27 9.00 3.80 -2 -5 -27 25.20 4.30 -2 5 27 19.60 4.70 -2 5 27 19.90 4.40 2 5 -27 30.30 4.90 -2 -5 27 31.10 5.30 2 5 27 16.00 4.70 2 -5 -27 25.10 4.20 2 5 27 26.90 5.60 0 0 28 54.49 6.70 1 0 28 -3.80 2.30 -1 0 28 0.20 2.70 -2 0 28 47.30 6.50 2 0 28 70.49 7.30 2 0 -28 57.29 6.10 -3 0 28 0.70 2.10 -3 0 -28 4.60 2.80 3 0 28 -0.70 2.70 3 0 -28 5.50 2.50 0 1 28 -4.70 2.40 0 -1 28 -0.40 2.60 -1 -1 -28 6.70 2.60 1 -1 28 8.00 3.40 -1 1 28 10.00 3.90 1 1 -28 6.50 2.60 1 1 28 9.00 3.50 -1 -1 28 6.00 3.50 -2 -1 -28 3.50 2.40 2 1 -28 1.00 2.00 -2 1 28 -0.20 1.90 2 -1 28 3.20 3.00 2 1 28 -1.10 2.80 2 -1 -28 0.70 2.40 -2 -1 28 1.30 2.80 3 -1 28 3.00 3.20 -3 1 28 8.00 3.20 3 1 -28 8.50 2.90 -3 -1 -28 8.40 2.90 -3 -1 28 8.50 3.20 3 1 28 3.60 3.20 3 -1 -28 10.10 3.30 0 2 28 41.40 6.20 0 -2 28 51.09 6.40 0 -2 -28 49.70 5.50 -1 2 28 24.20 4.90 1 -2 28 33.50 5.10 1 2 -28 35.10 4.80 -1 -2 -28 44.50 5.20 1 -2 -28 30.90 4.50 -1 -2 28 38.20 5.80 1 2 28 33.20 5.30 2 -2 28 59.09 6.80 2 2 -28 60.59 6.40 -2 -2 -28 62.29 6.40 -2 2 28 76.39 7.80 -2 -2 28 55.89 7.10 2 2 28 58.79 7.20 0 3 -28 -2.10 1.80 0 3 28 3.30 3.00 0 -3 28 0.90 3.00 0 -3 -28 -1.10 1.60 0 3 28 2.10 3.30 -1 3 28 10.30 3.20 -1 3 28 15.90 4.50 1 3 -28 11.30 3.10 -1 -3 -28 8.20 2.70 1 -3 28 9.60 3.50 1 -3 -28 13.30 3.10 1 3 28 8.60 4.30 1 3 28 12.00 3.90 -1 -3 28 7.40 3.40 2 -3 28 12.10 4.00 -2 -3 -28 7.70 2.60 -2 3 28 5.20 3.00 -2 3 28 8.90 4.20 2 3 -28 4.70 2.70 2 3 28 12.90 4.10 2 -3 -28 9.10 2.90 -2 -3 28 16.40 4.20 0 -4 28 26.90 4.80 0 4 28 23.90 4.60 0 4 -28 28.90 4.30 0 4 28 29.70 5.60 0 -4 -28 16.00 3.50 -1 4 28 38.30 5.90 1 -4 28 36.40 5.70 1 4 -28 42.40 5.50 -1 4 28 57.89 7.20 -1 -4 -28 39.70 5.20 -1 -4 28 53.39 6.50 1 4 28 44.40 6.60 1 4 28 36.90 6.10 1 -4 -28 39.30 5.00 0 0 29 4.60 3.40 1 0 29 -4.60 2.90 -1 0 29 0.20 3.40 0 1 29 5.60 4.00 0 -1 29 1.60 3.40 1 -1 29 3.10 3.20 -1 1 29 -1.10 3.70 -1 -1 29 2.00 3.50 1 1 29 4.20 3.70 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' ; _shelx_hkl_checksum 16469 _olex2_submission_special_instructions 'No special instructions were received'