# Electronic Supplementary Material (ESI) for RSC Advances. # This journal is © The Royal Society of Chemistry 2021 ####################################################################### # # This file contains crystal structure data downloaded from the # Cambridge Structural Database (CSD) hosted by the Cambridge # Crystallographic Data Centre (CCDC). # # Full information about CCDC data access policies and citation # guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 # # Audit and citation data items may have been added by the CCDC. # Please retain this information to preserve the provenance of # this file and to allow appropriate attribution of the data. # ####################################################################### data_Himali38 _database_code_depnum_ccdc_archive 'CCDC 1867219' loop_ _audit_author_name _audit_author_address 'Frank R Fronczek' ;Louisiana State University United States of America ; _audit_update_record ; 2018-09-12 deposited with the CCDC. 2021-05-04 downloaded from the CCDC. ; _audit_creation_method SHELXL-2014/7 _shelx_SHELXL_version_number 2014/7 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C22 H19 N3 O2 S' _chemical_formula_sum 'C22 H19 N3 O2 S' _chemical_formula_weight 389.46 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' _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_H-M_alt 'P 21/c' _space_group_name_Hall '-P 2ybc' _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. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 20.8714(8) _cell_length_b 5.6704(2) _cell_length_c 17.1989(6) _cell_angle_alpha 90 _cell_angle_beta 114.2072(18) _cell_angle_gamma 90 _cell_volume 1856.49(12) _cell_formula_units_Z 4 _cell_measurement_temperature 90.0(5) _cell_measurement_reflns_used 9840 _cell_measurement_theta_min 3.19 _cell_measurement_theta_max 37.05 _exptl_crystal_description lath _exptl_crystal_colour colourless _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.393 _exptl_crystal_F_000 816 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.480 _exptl_crystal_size_mid 0.310 _exptl_crystal_size_min 0.070 _exptl_absorpt_coefficient_mu 0.198 _shelx_estimated_absorpt_T_min 0.911 _shelx_estimated_absorpt_T_max 0.986 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.921 _exptl_absorpt_correction_T_max 0.986 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2004)' _exptl_absorpt_special_details ? _diffrn_ambient_temperature 90.0(5) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'TRIUMPH curved graphite' _diffrn_measurement_device_type 'Bruker Kappa APEX-II DUO' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 49006 _diffrn_reflns_av_unetI/netI 0.0178 _diffrn_reflns_av_R_equivalents 0.0221 _diffrn_reflns_limit_h_min -34 _diffrn_reflns_limit_h_max 35 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.070 _diffrn_reflns_theta_max 37.046 _diffrn_reflns_theta_full 25.000 _diffrn_measured_fraction_theta_max 0.995 _diffrn_measured_fraction_theta_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.995 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.995 _diffrn_reflns_point_group_measured_fraction_full 1.000 _reflns_number_total 9447 _reflns_number_gt 8248 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _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. ; _computing_data_collection 'Bruker APEX3' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ? _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0542P)^2^+0.5444P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 9447 _refine_ls_number_parameters 253 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0418 _refine_ls_R_factor_gt 0.0352 _refine_ls_wR_factor_ref 0.1024 _refine_ls_wR_factor_gt 0.0974 _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_restrained_S_all 1.057 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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 S1 S 0.30266(2) 0.34838(3) 0.31303(2) 0.01154(4) Uani 1 1 d . . . . . O1 O 0.26435(3) 0.16310(9) 0.25611(4) 0.01610(10) Uani 1 1 d . . . . . O2 O 0.35525(3) 0.29034(12) 0.39583(4) 0.01986(11) Uani 1 1 d . . . . . N1 N 0.18687(4) 0.85514(12) 0.45085(5) 0.02020(12) Uani 1 1 d . . . . . N2 N 0.24504(3) 0.51454(11) 0.32780(4) 0.01284(9) Uani 1 1 d . . . . . N3 N 0.08437(4) 0.41001(14) 0.13638(4) 0.02051(12) Uani 1 1 d . . . . . C1 C 0.14903(5) 0.84296(15) 0.49802(7) 0.02483(16) Uani 1 1 d . . . . . H1 H 0.1217 0.9763 0.4987 0.030 Uiso 1 1 calc R U . . . C2 C 0.14756(4) 0.64850(16) 0.54546(5) 0.02136(15) Uani 1 1 d . . . . . H2 H 0.1204 0.6493 0.5783 0.026 Uiso 1 1 calc R U . . . C3 C 0.18653(4) 0.45193(16) 0.54412(5) 0.02057(14) Uani 1 1 d . . . . . H3 H 0.1871 0.3156 0.5765 0.025 Uiso 1 1 calc R U . . . C4 C 0.22483(4) 0.45868(14) 0.49438(5) 0.01854(13) Uani 1 1 d . . . . . H4 H 0.2510 0.3252 0.4908 0.022 Uiso 1 1 calc R U . . . C5 C 0.22419(4) 0.66463(12) 0.44986(4) 0.01371(11) Uani 1 1 d . . . . . C6 C 0.26833(4) 0.68366(14) 0.39925(5) 0.01699(12) Uani 1 1 d . . . . . H6A H 0.2650 0.8459 0.3767 0.020 Uiso 1 1 calc R U . . . H6B H 0.3181 0.6527 0.4372 0.020 Uiso 1 1 calc R U . . . C7 C 0.18350(4) 0.58080(13) 0.25026(5) 0.01578(12) Uani 1 1 d . . . . . H7A H 0.1991 0.6100 0.2040 0.019 Uiso 1 1 calc R U . . . H7B H 0.1642 0.7306 0.2612 0.019 Uiso 1 1 calc R U . . . C8 C 0.12540(4) 0.39919(13) 0.22001(5) 0.01456(11) Uani 1 1 d . . . . . C9 C 0.11450(4) 0.23756(14) 0.27437(5) 0.01815(13) Uani 1 1 d . . . . . H9 H 0.1448 0.2341 0.3333 0.022 Uiso 1 1 calc R U . . . C10 C 0.05844(4) 0.08139(15) 0.24059(6) 0.02184(14) Uani 1 1 d . . . . . H10 H 0.0496 -0.0302 0.2762 0.026 Uiso 1 1 calc R U . . . C11 C 0.01556(4) 0.09080(17) 0.15417(6) 0.02443(16) Uani 1 1 d . . . . . H11 H -0.0231 -0.0137 0.1293 0.029 Uiso 1 1 calc R U . . . C12 C 0.03076(5) 0.25722(19) 0.10494(6) 0.02569(17) Uani 1 1 d . . . . . H12 H 0.0015 0.2632 0.0457 0.031 Uiso 1 1 calc R U . . . C13 C 0.34407(3) 0.51736(11) 0.26031(4) 0.01124(10) Uani 1 1 d . . . . . C14 C 0.34710(3) 0.42986(12) 0.18749(4) 0.01187(10) Uani 1 1 d . . . . . H14 H 0.3236 0.2872 0.1631 0.014 Uiso 1 1 calc R U . . . C15 C 0.38556(3) 0.55346(11) 0.14867(4) 0.01095(10) Uani 1 1 d . . . . . C16 C 0.39342(4) 0.46295(13) 0.07619(4) 0.01324(11) Uani 1 1 d . . . . . H16 H 0.3709 0.3197 0.0510 0.016 Uiso 1 1 calc R U . . . C17 C 0.43342(4) 0.58090(14) 0.04217(4) 0.01458(11) Uani 1 1 d . . . . . H17 H 0.4389 0.5175 -0.0059 0.017 Uiso 1 1 calc R U . . . C18 C 0.46644(4) 0.79591(14) 0.07822(5) 0.01576(12) Uani 1 1 d . . . . . H18 H 0.4941 0.8761 0.0544 0.019 Uiso 1 1 calc R U . . . C19 C 0.45875(4) 0.88976(13) 0.14757(5) 0.01466(11) Uani 1 1 d . . . . . H19 H 0.4805 1.0359 0.1707 0.018 Uiso 1 1 calc R U . . . C20 C 0.41869(3) 0.77045(11) 0.18503(4) 0.01135(10) Uani 1 1 d . . . . . C21 C 0.41292(4) 0.85734(12) 0.25942(4) 0.01321(11) Uani 1 1 d . . . . . H21 H 0.4341 1.0036 0.2832 0.016 Uiso 1 1 calc R U . . . C22 C 0.37715(4) 0.73288(12) 0.29722(4) 0.01304(10) Uani 1 1 d . . . . . H22 H 0.3745 0.7903 0.3477 0.016 Uiso 1 1 calc R U . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 S1 0.01264(7) 0.01219(7) 0.01181(7) 0.00243(5) 0.00707(5) 0.00144(5) O1 0.0207(2) 0.0114(2) 0.0209(2) -0.00214(17) 0.0133(2) -0.00242(17) O2 0.0164(2) 0.0274(3) 0.0153(2) 0.0097(2) 0.00604(19) 0.0048(2) N1 0.0244(3) 0.0151(3) 0.0264(3) -0.0008(2) 0.0158(3) 0.0018(2) N2 0.0128(2) 0.0149(2) 0.0121(2) -0.00146(18) 0.00646(18) 0.00084(18) N3 0.0166(3) 0.0284(3) 0.0168(3) 0.0001(2) 0.0072(2) -0.0042(2) C1 0.0265(4) 0.0207(3) 0.0359(4) -0.0056(3) 0.0215(4) 0.0012(3) C2 0.0210(3) 0.0293(4) 0.0188(3) -0.0077(3) 0.0132(3) -0.0062(3) C3 0.0210(3) 0.0266(4) 0.0158(3) 0.0043(3) 0.0092(3) -0.0013(3) C4 0.0194(3) 0.0189(3) 0.0207(3) 0.0046(3) 0.0117(3) 0.0036(2) C5 0.0160(3) 0.0142(3) 0.0132(2) -0.0021(2) 0.0083(2) -0.0008(2) C6 0.0212(3) 0.0172(3) 0.0174(3) -0.0055(2) 0.0129(3) -0.0057(2) C7 0.0136(3) 0.0142(3) 0.0183(3) 0.0032(2) 0.0053(2) 0.0011(2) C8 0.0122(2) 0.0159(3) 0.0170(3) 0.0010(2) 0.0075(2) 0.0013(2) C9 0.0154(3) 0.0183(3) 0.0208(3) 0.0042(2) 0.0075(2) 0.0002(2) C10 0.0178(3) 0.0194(3) 0.0304(4) 0.0031(3) 0.0120(3) -0.0016(3) C11 0.0181(3) 0.0264(4) 0.0299(4) -0.0041(3) 0.0109(3) -0.0064(3) C12 0.0194(3) 0.0366(5) 0.0202(3) -0.0037(3) 0.0073(3) -0.0083(3) C13 0.0120(2) 0.0115(2) 0.0115(2) 0.00040(19) 0.00621(19) 0.00017(18) C14 0.0135(2) 0.0118(2) 0.0117(2) -0.00072(19) 0.0064(2) -0.00168(19) C15 0.0115(2) 0.0117(2) 0.0101(2) 0.00019(18) 0.00490(19) -0.00089(18) C16 0.0144(2) 0.0157(3) 0.0108(2) -0.0008(2) 0.0064(2) -0.0016(2) C17 0.0143(3) 0.0195(3) 0.0111(2) 0.0019(2) 0.0064(2) -0.0003(2) C18 0.0152(3) 0.0191(3) 0.0143(3) 0.0039(2) 0.0073(2) -0.0019(2) C19 0.0147(3) 0.0140(3) 0.0156(3) 0.0021(2) 0.0065(2) -0.0026(2) C20 0.0113(2) 0.0108(2) 0.0118(2) 0.00091(19) 0.00462(19) -0.00046(18) C21 0.0143(2) 0.0113(2) 0.0144(3) -0.0018(2) 0.0063(2) -0.00118(19) C22 0.0143(2) 0.0129(2) 0.0132(2) -0.0020(2) 0.0070(2) -0.0002(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag S1 O2 1.4350(6) . ? S1 O1 1.4352(6) . ? S1 N2 1.6277(6) . ? S1 C13 1.7692(6) . ? N1 C5 1.3359(10) . ? N1 C1 1.3462(11) . ? N2 C7 1.4712(9) . ? N2 C6 1.4752(9) . ? N3 C8 1.3401(10) . ? N3 C12 1.3412(11) . ? C1 C2 1.3794(13) . ? C1 H1 0.9500 . ? C2 C3 1.3857(13) . ? C2 H2 0.9500 . ? C3 C4 1.3903(11) . ? C3 H3 0.9500 . ? C4 C5 1.3935(10) . ? C4 H4 0.9500 . ? C5 C6 1.5085(10) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.5115(10) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.3930(10) . ? C9 C10 1.3904(11) . ? C9 H9 0.9500 . ? C10 C11 1.3865(13) . ? C10 H10 0.9500 . ? C11 C12 1.3886(14) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C14 1.3725(9) . ? C13 C22 1.4191(9) . ? C14 C15 1.4216(9) . ? C14 H14 0.9500 . ? C15 C16 1.4184(9) . ? C15 C20 1.4243(9) . ? C16 C17 1.3737(9) . ? C16 H16 0.9500 . ? C17 C18 1.4126(11) . ? C17 H17 0.9500 . ? C18 C19 1.3744(11) . ? C18 H18 0.9500 . ? C19 C20 1.4189(9) . ? C19 H19 0.9500 . ? C20 C21 1.4215(9) . ? C21 C22 1.3697(10) . ? C21 H21 0.9500 . ? C22 H22 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 O2 S1 O1 119.64(4) . . ? O2 S1 N2 106.94(3) . . ? O1 S1 N2 106.83(3) . . ? O2 S1 C13 107.29(3) . . ? O1 S1 C13 107.43(3) . . ? N2 S1 C13 108.30(3) . . ? C5 N1 C1 117.09(7) . . ? C7 N2 C6 117.13(6) . . ? C7 N2 S1 115.64(5) . . ? C6 N2 S1 119.61(5) . . ? C8 N3 C12 117.61(7) . . ? N1 C1 C2 123.93(8) . . ? N1 C1 H1 118.0 . . ? C2 C1 H1 118.0 . . ? C1 C2 C3 118.53(7) . . ? C1 C2 H2 120.7 . . ? C3 C2 H2 120.7 . . ? C2 C3 C4 118.53(8) . . ? C2 C3 H3 120.7 . . ? C4 C3 H3 120.7 . . ? C3 C4 C5 118.86(7) . . ? C3 C4 H4 120.6 . . ? C5 C4 H4 120.6 . . ? N1 C5 C4 123.03(7) . . ? N1 C5 C6 116.53(7) . . ? C4 C5 C6 120.42(6) . . ? N2 C6 C5 111.32(6) . . ? N2 C6 H6A 109.4 . . ? C5 C6 H6A 109.4 . . ? N2 C6 H6B 109.4 . . ? C5 C6 H6B 109.4 . . ? H6A C6 H6B 108.0 . . ? N2 C7 C8 114.65(6) . . ? N2 C7 H7A 108.6 . . ? C8 C7 H7A 108.6 . . ? N2 C7 H7B 108.6 . . ? C8 C7 H7B 108.6 . . ? H7A C7 H7B 107.6 . . ? N3 C8 C9 122.83(7) . . ? N3 C8 C7 114.06(6) . . ? C9 C8 C7 123.10(7) . . ? C10 C9 C8 118.66(7) . . ? C10 C9 H9 120.7 . . ? C8 C9 H9 120.7 . . ? C11 C10 C9 119.08(8) . . ? C11 C10 H10 120.5 . . ? C9 C10 H10 120.5 . . ? C10 C11 C12 118.13(8) . . ? C10 C11 H11 120.9 . . ? C12 C11 H11 120.9 . . ? N3 C12 C11 123.68(8) . . ? N3 C12 H12 118.2 . . ? C11 C12 H12 118.2 . . ? C14 C13 C22 121.57(6) . . ? C14 C13 S1 119.14(5) . . ? C22 C13 S1 119.17(5) . . ? C13 C14 C15 119.77(6) . . ? C13 C14 H14 120.1 . . ? C15 C14 H14 120.1 . . ? C16 C15 C14 121.70(6) . . ? C16 C15 C20 119.22(6) . . ? C14 C15 C20 119.06(6) . . ? C17 C16 C15 120.50(6) . . ? C17 C16 H16 119.7 . . ? C15 C16 H16 119.7 . . ? C16 C17 C18 120.38(6) . . ? C16 C17 H17 119.8 . . ? C18 C17 H17 119.8 . . ? C19 C18 C17 120.36(6) . . ? C19 C18 H18 119.8 . . ? C17 C18 H18 119.8 . . ? C18 C19 C20 120.64(6) . . ? C18 C19 H19 119.7 . . ? C20 C19 H19 119.7 . . ? C19 C20 C21 121.77(6) . . ? C19 C20 C15 118.88(6) . . ? C21 C20 C15 119.31(6) . . ? C22 C21 C20 120.83(6) . . ? C22 C21 H21 119.6 . . ? C20 C21 H21 119.6 . . ? C21 C22 C13 119.42(6) . . ? C21 C22 H22 120.3 . . ? C13 C22 H22 120.3 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 S1 N2 C7 -175.92(5) . . . . ? O1 S1 N2 C7 -46.70(6) . . . . ? C13 S1 N2 C7 68.74(6) . . . . ? O2 S1 N2 C6 35.36(6) . . . . ? O1 S1 N2 C6 164.58(5) . . . . ? C13 S1 N2 C6 -79.98(6) . . . . ? C5 N1 C1 C2 0.89(14) . . . . ? N1 C1 C2 C3 -0.80(14) . . . . ? C1 C2 C3 C4 -0.61(13) . . . . ? C2 C3 C4 C5 1.83(12) . . . . ? C1 N1 C5 C4 0.45(12) . . . . ? C1 N1 C5 C6 -177.93(8) . . . . ? C3 C4 C5 N1 -1.81(12) . . . . ? C3 C4 C5 C6 176.50(7) . . . . ? C7 N2 C6 C5 80.47(8) . . . . ? S1 N2 C6 C5 -131.26(6) . . . . ? N1 C5 C6 N2 -117.06(8) . . . . ? C4 C5 C6 N2 64.52(9) . . . . ? C6 N2 C7 C8 -126.69(7) . . . . ? S1 N2 C7 C8 83.79(7) . . . . ? C12 N3 C8 C9 0.05(12) . . . . ? C12 N3 C8 C7 -178.79(8) . . . . ? N2 C7 C8 N3 -154.76(7) . . . . ? N2 C7 C8 C9 26.40(10) . . . . ? N3 C8 C9 C10 -0.34(12) . . . . ? C7 C8 C9 C10 178.40(7) . . . . ? C8 C9 C10 C11 0.29(12) . . . . ? C9 C10 C11 C12 0.02(13) . . . . ? C8 N3 C12 C11 0.28(14) . . . . ? C10 C11 C12 N3 -0.32(15) . . . . ? O2 S1 C13 C14 116.74(6) . . . . ? O1 S1 C13 C14 -13.10(6) . . . . ? N2 S1 C13 C14 -128.15(5) . . . . ? O2 S1 C13 C22 -59.34(6) . . . . ? O1 S1 C13 C22 170.82(5) . . . . ? N2 S1 C13 C22 55.77(6) . . . . ? C22 C13 C14 C15 1.57(10) . . . . ? S1 C13 C14 C15 -174.42(5) . . . . ? C13 C14 C15 C16 176.39(6) . . . . ? C13 C14 C15 C20 -1.79(10) . . . . ? C14 C15 C16 C17 -177.14(6) . . . . ? C20 C15 C16 C17 1.04(10) . . . . ? C15 C16 C17 C18 -0.93(11) . . . . ? C16 C17 C18 C19 -0.18(11) . . . . ? C17 C18 C19 C20 1.18(11) . . . . ? C18 C19 C20 C21 176.66(7) . . . . ? C18 C19 C20 C15 -1.04(10) . . . . ? C16 C15 C20 C19 -0.06(10) . . . . ? C14 C15 C20 C19 178.17(6) . . . . ? C16 C15 C20 C21 -177.82(6) . . . . ? C14 C15 C20 C21 0.41(9) . . . . ? C19 C20 C21 C22 -176.43(7) . . . . ? C15 C20 C21 C22 1.26(10) . . . . ? C20 C21 C22 C13 -1.53(10) . . . . ? C14 C13 C22 C21 0.11(10) . . . . ? S1 C13 C22 C21 176.09(5) . . . . ? _refine_diff_density_max 0.679 _refine_diff_density_min -0.256 _refine_diff_density_rms 0.067 _shelx_res_file ; Himali38.res created by SHELXL-2014/7 TITL Himali38 in P2(1)/c CELL 0.71073 20.87140 5.67040 17.19890 90.0000 114.2072 90.0000 ZERR 4.00 0.00080 0.00020 0.00060 0.0000 0.0018 0.0000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H N O S UNIT 88 76 12 8 4 ACTA 50 CONF L.S. 15 BOND $H FMAP 2 PLAN 10 SIZE 0.070 0.310 0.480 TEMP -183 WGHT 0.054200 0.544400 FVAR 0.15210 S1 5 0.302664 0.348383 0.313031 11.00000 0.01264 0.01219 = 0.01181 0.00243 0.00707 0.00144 O1 4 0.264348 0.163099 0.256105 11.00000 0.02071 0.01139 = 0.02091 -0.00214 0.01332 -0.00242 O2 4 0.355250 0.290342 0.395829 11.00000 0.01635 0.02742 = 0.01534 0.00969 0.00604 0.00480 N1 3 0.186871 0.855139 0.450852 11.00000 0.02439 0.01512 = 0.02643 -0.00080 0.01583 0.00175 N2 3 0.245040 0.514543 0.327800 11.00000 0.01284 0.01486 = 0.01214 -0.00146 0.00646 0.00084 N3 3 0.084371 0.410006 0.136380 11.00000 0.01664 0.02842 = 0.01676 0.00010 0.00716 -0.00420 C1 1 0.149026 0.842961 0.498023 11.00000 0.02646 0.02070 = 0.03587 -0.00560 0.02145 0.00119 AFIX 43 H1 2 0.121691 0.976289 0.498682 11.00000 -1.20000 AFIX 0 C2 1 0.147558 0.648504 0.545459 11.00000 0.02099 0.02934 = 0.01876 -0.00767 0.01324 -0.00618 AFIX 43 H2 2 0.120427 0.649335 0.578318 11.00000 -1.20000 AFIX 0 C3 1 0.186534 0.451928 0.544118 11.00000 0.02097 0.02659 = 0.01582 0.00429 0.00923 -0.00129 AFIX 43 H3 2 0.187074 0.315564 0.576471 11.00000 -1.20000 AFIX 0 C4 1 0.224832 0.458676 0.494377 11.00000 0.01935 0.01895 = 0.02073 0.00460 0.01166 0.00363 AFIX 43 H4 2 0.250990 0.325171 0.490800 11.00000 -1.20000 AFIX 0 C5 1 0.224187 0.664629 0.449862 11.00000 0.01598 0.01422 = 0.01318 -0.00207 0.00825 -0.00083 C6 1 0.268327 0.683655 0.399251 11.00000 0.02124 0.01722 = 0.01739 -0.00551 0.01288 -0.00572 AFIX 23 H6A 2 0.265017 0.845940 0.376695 11.00000 -1.20000 H6B 2 0.318110 0.652654 0.437165 11.00000 -1.20000 AFIX 0 C7 1 0.183504 0.580800 0.250264 11.00000 0.01363 0.01424 = 0.01828 0.00320 0.00534 0.00113 AFIX 23 H7A 2 0.199103 0.609967 0.203962 11.00000 -1.20000 H7B 2 0.164241 0.730613 0.261151 11.00000 -1.20000 AFIX 0 C8 1 0.125398 0.399191 0.220009 11.00000 0.01222 0.01592 = 0.01702 0.00105 0.00750 0.00134 C9 1 0.114495 0.237563 0.274373 11.00000 0.01541 0.01827 = 0.02085 0.00420 0.00751 0.00022 AFIX 43 H9 2 0.144751 0.234115 0.333340 11.00000 -1.20000 AFIX 0 C10 1 0.058441 0.081390 0.240594 11.00000 0.01780 0.01938 = 0.03040 0.00315 0.01197 -0.00156 AFIX 43 H10 2 0.049641 -0.030226 0.276240 11.00000 -1.20000 AFIX 0 C11 1 0.015563 0.090800 0.154170 11.00000 0.01807 0.02637 = 0.02987 -0.00411 0.01088 -0.00637 AFIX 43 H11 2 -0.023123 -0.013669 0.129331 11.00000 -1.20000 AFIX 0 C12 1 0.030757 0.257225 0.104938 11.00000 0.01942 0.03662 = 0.02025 -0.00374 0.00734 -0.00828 AFIX 43 H12 2 0.001539 0.263199 0.045664 11.00000 -1.20000 AFIX 0 C13 1 0.344074 0.517359 0.260307 11.00000 0.01203 0.01154 = 0.01151 0.00040 0.00621 0.00017 C14 1 0.347101 0.429855 0.187486 11.00000 0.01346 0.01177 = 0.01167 -0.00072 0.00644 -0.00168 AFIX 43 H14 2 0.323576 0.287186 0.163108 11.00000 -1.20000 AFIX 0 C15 1 0.385560 0.553457 0.148666 11.00000 0.01150 0.01173 = 0.01008 0.00019 0.00490 -0.00089 C16 1 0.393421 0.462948 0.076191 11.00000 0.01442 0.01571 = 0.01077 -0.00085 0.00636 -0.00163 AFIX 43 H16 2 0.370854 0.319661 0.050982 11.00000 -1.20000 AFIX 0 C17 1 0.433416 0.580898 0.042173 11.00000 0.01429 0.01954 = 0.01111 0.00185 0.00644 -0.00031 AFIX 43 H17 2 0.438897 0.517507 -0.005868 11.00000 -1.20000 AFIX 0 C18 1 0.466439 0.795911 0.078217 11.00000 0.01520 0.01906 = 0.01428 0.00395 0.00734 -0.00191 AFIX 43 H18 2 0.494118 0.876078 0.054387 11.00000 -1.20000 AFIX 0 C19 1 0.458746 0.889762 0.147572 11.00000 0.01472 0.01395 = 0.01556 0.00210 0.00647 -0.00265 AFIX 43 H19 2 0.480457 1.035940 0.170659 11.00000 -1.20000 AFIX 0 C20 1 0.418692 0.770449 0.185026 11.00000 0.01131 0.01084 = 0.01180 0.00091 0.00462 -0.00046 C21 1 0.412922 0.857336 0.259419 11.00000 0.01428 0.01130 = 0.01443 -0.00175 0.00627 -0.00118 AFIX 43 H21 2 0.434140 1.003561 0.283217 11.00000 -1.20000 AFIX 0 C22 1 0.377153 0.732878 0.297222 11.00000 0.01434 0.01287 = 0.01324 -0.00196 0.00701 -0.00023 AFIX 43 H22 2 0.374513 0.790335 0.347712 11.00000 -1.20000 AFIX 0 HKLF 4 REM Himali38 in P2(1)/c REM R1 = 0.0352 for 8248 Fo > 4sig(Fo) and 0.0418 for all 9447 data REM 253 parameters refined using 0 restraints END WGHT 0.0542 0.5444 REM Highest difference peak 0.679, deepest hole -0.256, 1-sigma level 0.067 Q1 1 0.2845 0.2220 0.2864 11.00000 0.05 0.68 Q2 1 0.4481 0.6940 0.0583 11.00000 0.05 0.65 Q3 1 0.2240 0.5599 0.4695 11.00000 0.05 0.64 Q4 1 0.3482 0.4649 0.2304 11.00000 0.05 0.63 Q5 1 0.3941 0.7963 0.2797 11.00000 0.05 0.63 Q6 1 0.4021 0.6631 0.1676 11.00000 0.05 0.62 Q7 1 0.1564 0.7536 0.5302 11.00000 0.05 0.62 Q8 1 0.0866 0.1532 0.2611 11.00000 0.05 0.61 Q9 1 0.4126 0.5225 0.0574 11.00000 0.05 0.61 Q10 1 0.3880 0.5079 0.1121 11.00000 0.05 0.59 ; _shelx_res_checksum 39973 ####################################################################### # # 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_Himali46 _database_code_depnum_ccdc_archive 'CCDC 1867221' loop_ _audit_author_name _audit_author_address 'Frank R Fronczek' ;Louisiana State University United States of America ; _audit_update_record ; 2018-09-12 deposited with the CCDC. 2021-05-04 downloaded from the CCDC. ; _audit_creation_method SHELXL-2014/7 _shelx_SHELXL_version_number 2014/7 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C22 H19 Cl2 N3 O2 Pt S' _chemical_formula_sum 'C22 H19 Cl2 N3 O2 Pt S' _chemical_formula_weight 655.45 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system monoclinic _space_group_IT_number 15 _space_group_name_H-M_alt 'C 2/c' _space_group_name_Hall '-C 2yc' _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. ; 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' '-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 26.7076(7) _cell_length_b 8.7572(2) _cell_length_c 18.7201(4) _cell_angle_alpha 90 _cell_angle_beta 91.3560(10) _cell_angle_gamma 90 _cell_volume 4377.10(18) _cell_formula_units_Z 8 _cell_measurement_temperature 100.0(5) _cell_measurement_reflns_used 7940 _cell_measurement_theta_min 2.18 _cell_measurement_theta_max 30.85 _exptl_crystal_description lath _exptl_crystal_colour colourless _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.989 _exptl_crystal_F_000 2528 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.300 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_min 0.020 _exptl_absorpt_coefficient_mu 6.776 _shelx_estimated_absorpt_T_min 0.236 _shelx_estimated_absorpt_T_max 0.876 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.639 _exptl_absorpt_correction_T_max 0.876 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2004)' _exptl_absorpt_special_details ? _diffrn_ambient_temperature 100.0(5) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'TRIUMPH curved graphite' _diffrn_measurement_device_type 'Bruker Kappa APEX-II DUO' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 48008 _diffrn_reflns_av_unetI/netI 0.0514 _diffrn_reflns_av_R_equivalents 0.0639 _diffrn_reflns_limit_h_min -41 _diffrn_reflns_limit_h_max 41 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.525 _diffrn_reflns_theta_max 33.264 _diffrn_reflns_theta_full 25.000 _diffrn_measured_fraction_theta_max 0.995 _diffrn_measured_fraction_theta_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.995 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.995 _diffrn_reflns_point_group_measured_fraction_full 1.000 _reflns_number_total 8404 _reflns_number_gt 5686 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _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. ; _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ? _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0268P)^2^+21.6239P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 8404 _refine_ls_number_parameters 398 _refine_ls_number_restraints 107 _refine_ls_R_factor_all 0.0719 _refine_ls_R_factor_gt 0.0365 _refine_ls_wR_factor_ref 0.0795 _refine_ls_wR_factor_gt 0.0689 _refine_ls_goodness_of_fit_ref 1.003 _refine_ls_restrained_S_all 1.003 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 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 Pt1 Pt 0.26849(2) 0.49247(2) 0.55376(2) 0.01973(4) Uani 1 1 d . . . . . Cl1 Cl 0.23734(4) 0.51331(11) 0.43888(5) 0.02728(19) Uani 1 1 d . . . . . Cl2 Cl 0.19077(4) 0.53260(12) 0.60009(6) 0.0300(2) Uani 1 1 d . . . . . N1 N 0.33640(13) 0.4570(4) 0.51030(18) 0.0207(7) Uani 1 1 d . . . . . N2 N 0.37028(15) 0.7078(4) 0.6187(2) 0.0323(9) Uani 1 1 d . . . . . N3 N 0.29376(14) 0.4546(4) 0.65515(19) 0.0239(7) Uani 1 1 d . . . . . C1 C 0.34383(17) 0.3208(5) 0.4794(2) 0.0277(9) Uani 1 1 d . . . . . H1 H 0.3194 0.2430 0.4844 0.033 Uiso 1 1 calc R U . . . C2 C 0.38582(19) 0.2909(6) 0.4408(3) 0.0371(11) Uani 1 1 d . . . . . H2 H 0.3906 0.1929 0.4203 0.045 Uiso 1 1 calc R U . . . C3 C 0.4204(2) 0.4029(7) 0.4322(4) 0.0587(19) Uani 1 1 d . . . . . H3 H 0.4492 0.3857 0.4044 0.070 Uiso 1 1 calc R U . . . C4 C 0.4128(2) 0.5419(7) 0.4646(4) 0.0569(19) Uani 1 1 d . . . . . H4 H 0.4369 0.6208 0.4597 0.068 Uiso 1 1 calc R U . . . C5 C 0.37096(18) 0.5682(5) 0.5040(3) 0.0327(10) Uani 1 1 d . . . . . C6 C 0.36235(19) 0.7172(5) 0.5405(3) 0.0350(11) Uani 1 1 d . . . . . H6A H 0.3854 0.7946 0.5210 0.042 Uiso 1 1 calc R U . . . H6B H 0.3276 0.7515 0.5299 0.042 Uiso 1 1 calc R U . . . C7 C 0.32761(16) 0.7124(5) 0.6666(3) 0.0268(9) Uani 1 1 d . . . . . H7A H 0.2978 0.7508 0.6397 0.032 Uiso 1 1 calc R U . . . H7B H 0.3351 0.7855 0.7058 0.032 Uiso 1 1 calc R U . . . C8 C 0.31533(17) 0.5597(5) 0.6984(2) 0.0259(9) Uani 1 1 d . . . . . C9 C 0.3254(2) 0.5260(5) 0.7697(3) 0.0350(11) Uani 1 1 d . . . . . H9 H 0.3409 0.6007 0.7997 0.042 Uiso 1 1 calc R U . . . C10 C 0.3134(2) 0.3866(6) 0.7972(3) 0.0391(12) Uani 1 1 d . . . . . H10 H 0.3188 0.3653 0.8466 0.047 Uiso 1 1 calc R U . . . C11 C 0.2933(2) 0.2770(6) 0.7517(3) 0.0423(13) Uani 1 1 d . . . . . H11 H 0.2863 0.1771 0.7687 0.051 Uiso 1 1 calc R U . . . C12 C 0.2835(2) 0.3149(5) 0.6822(3) 0.0349(11) Uani 1 1 d . . . . . H12 H 0.2690 0.2402 0.6514 0.042 Uiso 1 1 calc R U . . . S1 S 0.42600(11) 0.7467(3) 0.64133(18) 0.0238(5) Uani 0.557(4) 1 d D . P A 1 O1 O 0.4599(4) 0.6881(10) 0.5909(5) 0.030(2) Uani 0.557(4) 1 d D . P A 1 O2 O 0.4286(2) 0.6981(7) 0.7157(4) 0.0282(14) Uani 0.557(4) 1 d D . P A 1 C13 C 0.4339(3) 0.9479(8) 0.6404(4) 0.0270(17) Uani 0.557(4) 1 d D . P A 1 C14 C 0.3915(3) 1.0409(9) 0.6283(3) 0.0310(18) Uani 0.557(4) 1 d D . P A 1 H14 H 0.3596 0.9958 0.6195 0.037 Uiso 0.557(4) 1 calc R U P A 1 C15 C 0.3965(3) 1.1977(9) 0.6292(4) 0.0327(19) Uani 0.557(4) 1 d D . P A 1 H15 H 0.3677 1.2601 0.6223 0.039 Uiso 0.557(4) 1 calc R U P A 1 C16 C 0.4411(4) 1.2629(12) 0.6397(6) 0.045(3) Uani 0.557(4) 1 d D . P A 1 H16 H 0.4435 1.3712 0.6384 0.053 Uiso 0.557(4) 1 calc R U P A 1 C17 C 0.4849(3) 1.1772(8) 0.6525(5) 0.036(2) Uani 0.557(4) 1 d D . P A 1 C18 C 0.5317(4) 1.2477(10) 0.6661(5) 0.046(3) Uani 0.557(4) 1 d D . P A 1 H18 H 0.5338 1.3560 0.6658 0.055 Uiso 0.557(4) 1 calc R U P A 1 C19 C 0.5749(4) 1.1613(11) 0.6799(6) 0.044(3) Uani 0.557(4) 1 d D . P A 1 H19 H 0.6065 1.2087 0.6885 0.053 Uiso 0.557(4) 1 calc R U P A 1 C20 C 0.5699(3) 1.0054(12) 0.6806(5) 0.0348(19) Uani 0.557(4) 1 d D . P A 1 H20 H 0.5990 0.9457 0.6900 0.042 Uiso 0.557(4) 1 calc R U P A 1 C21 C 0.5256(3) 0.9309(10) 0.6688(5) 0.0305(18) Uani 0.557(4) 1 d D . P A 1 H21 H 0.5245 0.8226 0.6711 0.037 Uiso 0.557(4) 1 calc R U P A 1 C22 C 0.4811(3) 1.0150(8) 0.6529(4) 0.0247(14) Uani 0.557(4) 1 d D . P A 1 S1A S 0.42645(14) 0.7155(4) 0.6692(3) 0.0283(8) Uani 0.443(4) 1 d D . P A 2 O1A O 0.4620(5) 0.6761(18) 0.6171(6) 0.042(4) Uani 0.443(4) 1 d D . P A 2 O2A O 0.4247(3) 0.6179(11) 0.7312(4) 0.040(2) Uani 0.443(4) 1 d D . P A 2 C13A C 0.4326(4) 0.9028(10) 0.7041(5) 0.032(2) Uani 0.443(4) 1 d D U P A 2 C14A C 0.4214(3) 0.9244(13) 0.7752(6) 0.042(3) Uani 0.443(4) 1 d D U P A 2 H14A H 0.4135 0.8382 0.8037 0.051 Uiso 0.443(4) 1 calc R U P A 2 C15A C 0.4212(5) 1.0712(16) 0.8065(8) 0.048(4) Uani 0.443(4) 1 d D U P A 2 H15A H 0.4141 1.0824 0.8558 0.057 Uiso 0.443(4) 1 calc R U P A 2 C16A C 0.4308(5) 1.1914(14) 0.7681(7) 0.046(3) Uani 0.443(4) 1 d D U P A 2 H16A H 0.4301 1.2896 0.7896 0.055 Uiso 0.443(4) 1 calc R U P A 2 C17A C 0.4424(5) 1.1784(12) 0.6944(7) 0.045(3) Uani 0.443(4) 1 d D U P A 2 C18A C 0.4529(6) 1.3098(14) 0.6571(8) 0.041(3) Uani 0.443(4) 1 d D U P A 2 H18A H 0.4503 1.4076 0.6786 0.050 Uiso 0.443(4) 1 calc R U P A 2 C19A C 0.4677(6) 1.2932(16) 0.5853(8) 0.064(4) Uani 0.443(4) 1 d D U P A 2 H19A H 0.4752 1.3822 0.5586 0.076 Uiso 0.443(4) 1 calc R U P A 2 C21A C 0.4596(5) 1.0240(13) 0.5888(6) 0.045(3) Uani 0.443(4) 1 d D U P A 2 H21A H 0.4615 0.9276 0.5656 0.054 Uiso 0.443(4) 1 calc R U P A 2 C20A C 0.4715(5) 1.1523(13) 0.5528(7) 0.048(3) Uani 0.443(4) 1 d D U P A 2 H20A H 0.4826 1.1455 0.5050 0.058 Uiso 0.443(4) 1 calc R U P A 2 C22A C 0.4438(4) 1.0319(10) 0.6625(5) 0.028(2) Uani 0.443(4) 1 d D U P A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.02134(6) 0.02089(6) 0.01696(7) -0.00021(7) 0.00048(4) -0.00151(7) Cl1 0.0309(5) 0.0299(4) 0.0209(4) -0.0001(4) -0.0039(4) 0.0042(4) Cl2 0.0272(5) 0.0345(5) 0.0284(5) -0.0106(4) 0.0054(4) -0.0015(4) N1 0.0237(17) 0.0206(14) 0.0179(17) 0.0020(12) -0.0003(13) 0.0022(12) N2 0.027(2) 0.0228(16) 0.048(3) -0.0038(16) 0.0049(18) -0.0043(14) N3 0.0321(19) 0.0230(15) 0.0164(17) 0.0028(12) 0.0009(14) -0.0023(13) C1 0.031(2) 0.028(2) 0.024(2) -0.0036(16) -0.0021(18) 0.0026(17) C2 0.031(3) 0.037(2) 0.043(3) -0.013(2) 0.000(2) 0.005(2) C3 0.027(3) 0.064(4) 0.086(5) -0.034(3) 0.021(3) -0.002(3) C4 0.039(3) 0.051(3) 0.082(5) -0.028(3) 0.034(3) -0.020(2) C5 0.026(2) 0.029(2) 0.044(3) -0.0037(19) 0.010(2) -0.0017(17) C6 0.035(3) 0.0231(19) 0.048(3) 0.0005(19) 0.018(2) -0.0045(18) C7 0.024(2) 0.0235(18) 0.033(3) -0.0007(17) -0.0012(18) 0.0036(15) C8 0.028(2) 0.0265(18) 0.023(2) 0.0005(16) -0.0036(17) 0.0005(16) C9 0.047(3) 0.034(2) 0.023(2) -0.0046(18) -0.0109(19) -0.003(2) C10 0.051(3) 0.044(3) 0.021(2) 0.007(2) -0.004(2) 0.002(2) C11 0.063(4) 0.037(2) 0.028(3) 0.011(2) -0.002(3) -0.005(2) C12 0.048(3) 0.031(2) 0.025(3) 0.0036(18) -0.003(2) -0.012(2) S1 0.0245(11) 0.0192(11) 0.0273(16) 0.0004(9) -0.0045(11) -0.0036(8) O1 0.026(4) 0.020(3) 0.043(6) 0.000(3) -0.001(4) -0.002(2) O2 0.037(3) 0.018(3) 0.029(4) 0.015(3) -0.012(3) -0.007(2) C13 0.035(4) 0.017(3) 0.029(4) 0.004(3) -0.006(3) -0.009(3) C14 0.029(4) 0.038(4) 0.026(4) 0.005(3) -0.004(3) -0.002(3) C15 0.036(5) 0.029(4) 0.033(5) 0.004(3) 0.002(4) 0.012(3) C16 0.066(9) 0.036(5) 0.032(6) -0.010(4) 0.009(6) -0.002(5) C17 0.052(6) 0.026(4) 0.032(5) 0.005(3) 0.014(4) -0.007(4) C18 0.063(7) 0.037(5) 0.038(6) -0.001(4) 0.012(5) -0.019(4) C19 0.043(6) 0.037(5) 0.054(7) -0.010(5) 0.021(5) -0.017(4) C20 0.023(4) 0.054(6) 0.027(4) 0.003(5) 0.007(3) 0.002(5) C21 0.022(4) 0.040(4) 0.030(5) 0.000(3) -0.002(3) 0.001(3) C22 0.029(4) 0.026(3) 0.020(3) -0.003(3) 0.005(3) -0.003(3) S1A 0.0266(14) 0.0188(14) 0.039(3) 0.0014(15) -0.0004(18) -0.0003(11) O1A 0.025(5) 0.066(7) 0.037(7) 0.015(6) 0.010(5) 0.011(4) O2A 0.037(5) 0.051(5) 0.032(5) 0.011(4) -0.001(4) 0.002(4) C13A 0.031(4) 0.030(4) 0.035(4) -0.001(3) 0.004(3) -0.001(3) C14A 0.042(5) 0.044(4) 0.041(5) -0.004(4) 0.003(4) -0.004(4) C15A 0.044(5) 0.048(5) 0.051(6) -0.002(4) 0.002(4) -0.003(4) C16A 0.041(5) 0.048(5) 0.048(5) -0.006(4) -0.003(4) 0.005(4) C17A 0.039(5) 0.043(4) 0.051(5) -0.001(4) -0.010(4) 0.001(4) C18A 0.037(5) 0.036(5) 0.050(5) 0.002(4) -0.004(4) 0.000(4) C19A 0.060(6) 0.064(5) 0.067(6) 0.004(4) -0.006(4) -0.008(4) C21A 0.047(5) 0.045(5) 0.043(5) 0.000(4) -0.005(4) -0.007(4) C20A 0.046(5) 0.053(5) 0.046(5) 0.015(4) 0.003(4) -0.015(4) C22A 0.023(4) 0.028(4) 0.033(4) 0.008(3) -0.004(3) -0.003(3) _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 Pt1 N3 2.027(4) . ? Pt1 N1 2.029(3) . ? Pt1 Cl1 2.2947(10) . ? Pt1 Cl2 2.2955(11) . ? N1 C1 1.343(5) . ? N1 C5 1.349(6) . ? N2 C7 1.467(6) . ? N2 C6 1.478(7) . ? N2 S1 1.575(5) . ? N2 S1A 1.756(6) . ? N3 C8 1.347(6) . ? N3 C12 1.354(5) . ? C1 C2 1.374(6) . ? C2 C3 1.360(8) . ? C3 C4 1.378(8) . ? C4 C5 1.373(7) . ? C5 C6 1.493(6) . ? C7 C8 1.503(6) . ? C8 C9 1.387(6) . ? C9 C10 1.366(7) . ? C10 C11 1.384(8) . ? C11 C12 1.363(7) . ? S1 O1 1.419(8) . ? S1 O2 1.456(7) . ? S1 C13 1.774(7) . ? C13 C22 1.406(10) . ? C13 C14 1.407(11) . ? C14 C15 1.380(10) . ? C15 C16 1.332(13) . ? C16 C17 1.405(14) . ? C17 C18 1.411(12) . ? C17 C22 1.424(9) . ? C18 C19 1.400(14) . ? C19 C20 1.372(12) . ? C20 C21 1.363(11) . ? C21 C22 1.425(10) . ? S1A O1A 1.420(10) . ? S1A O2A 1.443(8) . ? S1A C13A 1.771(9) . ? C13A C14A 1.386(13) . ? C13A C22A 1.408(11) . ? C14A C15A 1.414(15) . ? C15A C16A 1.304(16) . ? C16A C17A 1.426(15) . ? C17A C18A 1.378(15) . ? C17A C22A 1.415(12) . ? C18A C19A 1.417(17) . ? C19A C20A 1.381(15) . ? C21A C20A 1.353(13) . ? C21A C22A 1.455(13) . ? 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 N3 Pt1 N1 93.98(14) . . ? N3 Pt1 Cl1 174.89(10) . . ? N1 Pt1 Cl1 86.79(10) . . ? N3 Pt1 Cl2 87.44(11) . . ? N1 Pt1 Cl2 178.56(10) . . ? Cl1 Pt1 Cl2 91.77(4) . . ? C1 N1 C5 119.7(4) . . ? C1 N1 Pt1 116.8(3) . . ? C5 N1 Pt1 123.0(3) . . ? C7 N2 C6 120.6(4) . . ? C7 N2 S1 124.9(4) . . ? C6 N2 S1 111.5(3) . . ? C7 N2 S1A 109.6(4) . . ? C6 N2 S1A 129.2(4) . . ? C8 N3 C12 118.7(4) . . ? C8 N3 Pt1 125.4(3) . . ? C12 N3 Pt1 115.6(3) . . ? N1 C1 C2 121.8(4) . . ? C3 C2 C1 119.4(5) . . ? C2 C3 C4 118.5(5) . . ? C5 C4 C3 121.0(5) . . ? N1 C5 C4 119.6(4) . . ? N1 C5 C6 118.6(4) . . ? C4 C5 C6 121.9(4) . . ? N2 C6 C5 112.6(4) . . ? N2 C7 C8 113.4(3) . . ? N3 C8 C9 120.2(4) . . ? N3 C8 C7 117.7(4) . . ? C9 C8 C7 122.1(4) . . ? C10 C9 C8 120.8(4) . . ? C9 C10 C11 118.6(5) . . ? C12 C11 C10 118.8(5) . . ? N3 C12 C11 122.8(5) . . ? O1 S1 O2 120.9(5) . . ? O1 S1 N2 110.9(5) . . ? O2 S1 N2 102.5(3) . . ? O1 S1 C13 105.9(5) . . ? O2 S1 C13 107.3(4) . . ? N2 S1 C13 108.9(3) . . ? C22 C13 C14 119.9(6) . . ? C22 C13 S1 121.3(6) . . ? C14 C13 S1 118.7(6) . . ? C15 C14 C13 119.8(8) . . ? C16 C15 C14 120.9(8) . . ? C15 C16 C17 122.3(9) . . ? C16 C17 C18 121.7(8) . . ? C16 C17 C22 118.3(8) . . ? C18 C17 C22 119.9(8) . . ? C19 C18 C17 121.3(8) . . ? C20 C19 C18 117.3(9) . . ? C21 C20 C19 124.0(9) . . ? C20 C21 C22 120.2(8) . . ? C13 C22 C17 118.7(7) . . ? C13 C22 C21 124.0(7) . . ? C17 C22 C21 117.2(7) . . ? O1A S1A O2A 116.4(7) . . ? O1A S1A N2 101.3(7) . . ? O2A S1A N2 111.5(4) . . ? O1A S1A C13A 114.8(8) . . ? O2A S1A C13A 104.9(6) . . ? N2 S1A C13A 107.7(4) . . ? C14A C13A C22A 118.4(9) . . ? C14A C13A S1A 117.4(8) . . ? C22A C13A S1A 124.0(8) . . ? C13A C14A C15A 121.7(11) . . ? C16A C15A C14A 120.2(13) . . ? C15A C16A C17A 121.3(12) . . ? C18A C17A C22A 122.4(11) . . ? C18A C17A C16A 118.3(11) . . ? C22A C17A C16A 119.3(10) . . ? C17A C18A C19A 117.3(12) . . ? C20A C19A C18A 122.4(13) . . ? C20A C21A C22A 120.7(10) . . ? C21A C20A C19A 120.1(12) . . ? C13A C22A C17A 119.1(9) . . ? C13A C22A C21A 123.7(9) . . ? C17A C22A C21A 117.0(9) . . ? _refine_diff_density_max 1.953 _refine_diff_density_min -1.181 _refine_diff_density_rms 0.173 _shelx_res_file ; shelxl.res created by SHELXL-2014/7 TITL Himali46 in C2/c CELL 0.71073 26.7076 8.7572 18.7201 90.000 91.356 90.000 ZERR 8.00 0.0007 0.0002 0.0004 0.000 0.001 0.000 LATT 7 SYMM - X, Y, 1/2 - Z SFAC C H N O S CL PT UNIT 176 152 24 16 8 16 8 MERG 2 FLAT C13 > C22 FLAT C13A > C22A ISOR 0.005 C13A C14A C15A C16A C17A C18A C19A C20A C21A C22A FMAP 2 PLAN 20 SIZE 0.02 0.10 0.30 ACTA 50.00 L.S. 15 TEMP -173.00 WGHT 0.026800 21.623901 FVAR 0.03648 0.55690 PT1 7 0.268490 0.492469 0.553763 11.00000 0.02134 0.02089 = 0.01696 -0.00021 0.00048 -0.00151 CL1 6 0.237344 0.513307 0.438881 11.00000 0.03089 0.02988 = 0.02086 -0.00014 -0.00393 0.00423 CL2 6 0.190771 0.532596 0.600088 11.00000 0.02720 0.03450 = 0.02845 -0.01056 0.00542 -0.00155 N1 3 0.336404 0.457020 0.510295 11.00000 0.02373 0.02058 = 0.01790 0.00200 -0.00028 0.00223 N2 3 0.370281 0.707833 0.618706 11.00000 0.02657 0.02280 = 0.04762 -0.00378 0.00488 -0.00428 N3 3 0.293765 0.454575 0.655154 11.00000 0.03212 0.02305 = 0.01641 0.00276 0.00092 -0.00226 C1 1 0.343834 0.320807 0.479392 11.00000 0.03063 0.02794 = 0.02425 -0.00362 -0.00207 0.00262 AFIX 43 H1 2 0.319388 0.242969 0.484375 11.00000 -1.20000 AFIX 0 C2 1 0.385816 0.290894 0.440765 11.00000 0.03117 0.03689 = 0.04323 -0.01347 -0.00030 0.00525 AFIX 43 H2 2 0.390622 0.192906 0.420259 11.00000 -1.20000 AFIX 0 C3 1 0.420439 0.402896 0.432153 11.00000 0.02694 0.06375 = 0.08632 -0.03388 0.02092 -0.00197 AFIX 43 H3 2 0.449216 0.385656 0.404390 11.00000 -1.20000 AFIX 0 C4 1 0.412830 0.541921 0.464608 11.00000 0.03899 0.05115 = 0.08220 -0.02812 0.03405 -0.01977 AFIX 43 H4 2 0.436918 0.620808 0.459664 11.00000 -1.20000 AFIX 0 C5 1 0.370960 0.568203 0.503992 11.00000 0.02572 0.02870 = 0.04417 -0.00367 0.00974 -0.00165 C6 1 0.362351 0.717243 0.540450 11.00000 0.03512 0.02305 = 0.04760 0.00048 0.01809 -0.00453 AFIX 23 H6A 2 0.385369 0.794633 0.521020 11.00000 -1.20000 H6B 2 0.327632 0.751459 0.529875 11.00000 -1.20000 AFIX 0 C7 1 0.327608 0.712439 0.666611 11.00000 0.02362 0.02350 = 0.03311 -0.00074 -0.00120 0.00365 AFIX 23 H7A 2 0.297849 0.750807 0.639664 11.00000 -1.20000 H7B 2 0.335122 0.785469 0.705785 11.00000 -1.20000 AFIX 0 C8 1 0.315333 0.559726 0.698405 11.00000 0.02755 0.02647 = 0.02337 0.00047 -0.00357 0.00048 C9 1 0.325437 0.525980 0.769685 11.00000 0.04709 0.03403 = 0.02345 -0.00455 -0.01090 -0.00340 AFIX 43 H9 2 0.340874 0.600665 0.799700 11.00000 -1.20000 AFIX 0 C10 1 0.313446 0.386564 0.797239 11.00000 0.05143 0.04436 = 0.02113 0.00735 -0.00410 0.00179 AFIX 43 H10 2 0.318844 0.365311 0.846586 11.00000 -1.20000 AFIX 0 C11 1 0.293276 0.277002 0.751745 11.00000 0.06265 0.03659 = 0.02761 0.01102 -0.00205 -0.00467 AFIX 43 H11 2 0.286340 0.177137 0.768687 11.00000 -1.20000 AFIX 0 C12 1 0.283539 0.314932 0.682192 11.00000 0.04821 0.03114 = 0.02515 0.00357 -0.00256 -0.01165 AFIX 43 H12 2 0.268952 0.240193 0.651366 11.00000 -1.20000 AFIX 0 PART 1 SAME S1A O1A O2A C13A C14A C15A C16A C17A C18A C19A C20A C21A C22A S1 5 0.425998 0.746722 0.641331 21.00000 0.02452 0.01917 = 0.02733 0.00043 -0.00447 -0.00364 O1 4 0.459876 0.688104 0.590924 21.00000 0.02562 0.02039 = 0.04296 0.00043 -0.00051 -0.00193 O2 4 0.428571 0.698143 0.715707 21.00000 0.03690 0.01838 = 0.02880 0.01526 -0.01180 -0.00695 C13 1 0.433880 0.947900 0.640363 21.00000 0.03460 0.01701 = 0.02905 0.00447 -0.00580 -0.00898 C14 1 0.391541 1.040852 0.628273 21.00000 0.02937 0.03756 = 0.02580 0.00514 -0.00388 -0.00185 AFIX 43 H14 2 0.359633 0.995753 0.619502 21.00000 -1.20000 AFIX 0 C15 1 0.396503 1.197735 0.629195 21.00000 0.03587 0.02900 = 0.03322 0.00414 0.00226 0.01187 AFIX 43 H15 2 0.367687 1.260080 0.622260 21.00000 -1.20000 AFIX 0 C16 1 0.441149 1.262943 0.639678 21.00000 0.06632 0.03602 = 0.03161 -0.00990 0.00911 -0.00193 AFIX 43 H16 2 0.443478 1.371154 0.638402 21.00000 -1.20000 AFIX 0 C17 1 0.484890 1.177230 0.652548 21.00000 0.05153 0.02567 = 0.03188 0.00473 0.01351 -0.00711 C18 1 0.531658 1.247728 0.666098 21.00000 0.06300 0.03709 = 0.03821 -0.00075 0.01171 -0.01874 AFIX 43 H18 2 0.533848 1.356002 0.665838 21.00000 -1.20000 AFIX 0 C19 1 0.574889 1.161285 0.679916 21.00000 0.04349 0.03684 = 0.05411 -0.01040 0.02133 -0.01651 AFIX 43 H19 2 0.606462 1.208677 0.688460 21.00000 -1.20000 AFIX 0 C20 1 0.569854 1.005385 0.680631 21.00000 0.02346 0.05431 = 0.02704 0.00346 0.00693 0.00169 AFIX 43 H20 2 0.598983 0.945690 0.689953 21.00000 -1.20000 AFIX 0 C21 1 0.525624 0.930902 0.668785 21.00000 0.02213 0.03952 = 0.02963 -0.00049 -0.00172 0.00120 AFIX 43 H21 2 0.524498 0.822592 0.671110 21.00000 -1.20000 AFIX 0 C22 1 0.481079 1.015013 0.652928 21.00000 0.02879 0.02589 = 0.01952 -0.00310 0.00526 -0.00251 PART 2 S1A 5 0.426454 0.715491 0.669234 -21.00000 0.02664 0.01884 = 0.03935 0.00143 -0.00037 -0.00031 O1A 4 0.461994 0.676079 0.617078 -21.00000 0.02472 0.06611 = 0.03689 0.01492 0.00988 0.01064 O2A 4 0.424683 0.617857 0.731222 -21.00000 0.03688 0.05126 = 0.03217 0.01114 -0.00073 0.00197 C13A 1 0.432624 0.902787 0.704054 -21.00000 0.03115 0.03029 = 0.03531 -0.00107 0.00375 -0.00084 C14A 1 0.421358 0.924371 0.775214 -21.00000 0.04173 0.04364 = 0.04125 -0.00375 0.00345 -0.00378 AFIX 43 H14A 2 0.413511 0.838225 0.803692 -21.00000 -1.20000 AFIX 0 C15A 1 0.421236 1.071242 0.806544 -21.00000 0.04368 0.04787 = 0.05138 -0.00168 0.00195 -0.00296 AFIX 43 H15A 2 0.414149 1.082412 0.855760 -21.00000 -1.20000 AFIX 0 C16A 1 0.430821 1.191415 0.768096 -21.00000 0.04070 0.04819 = 0.04750 -0.00575 -0.00328 0.00535 AFIX 43 H16A 2 0.430079 1.289609 0.789617 -21.00000 -1.20000 AFIX 0 C17A 1 0.442399 1.178355 0.694366 -21.00000 0.03899 0.04334 = 0.05147 -0.00068 -0.00958 0.00106 C18A 1 0.452883 1.309813 0.657079 -21.00000 0.03743 0.03610 = 0.05038 0.00244 -0.00369 -0.00001 AFIX 43 H18A 2 0.450304 1.407617 0.678636 -21.00000 -1.20000 AFIX 0 C19A 1 0.467659 1.293180 0.585311 -21.00000 0.06000 0.06355 = 0.06660 0.00366 -0.00625 -0.00755 AFIX 43 H19A 2 0.475182 1.382183 0.558609 -21.00000 -1.20000 AFIX 0 C21A 1 0.459559 1.023969 0.588757 -21.00000 0.04667 0.04528 = 0.04337 -0.00047 -0.00512 -0.00691 AFIX 43 H21A 2 0.461484 0.927644 0.565642 -21.00000 -1.20000 AFIX 0 C20A 1 0.471525 1.152301 0.552755 -21.00000 0.04642 0.05291 = 0.04607 0.01496 0.00349 -0.01514 AFIX 43 H20A 2 0.482603 1.145513 0.505008 -21.00000 -1.20000 AFIX 0 C22A 1 0.443775 1.031922 0.662502 -21.00000 0.02269 0.02846 = 0.03345 0.00754 -0.00399 -0.00287 HKLF 4 REM Himali46 in C2/c REM R1 = 0.0365 for 5686 Fo > 4sig(Fo) and 0.0719 for all 8404 data REM 398 parameters refined using 107 restraints END WGHT 0.0268 21.5829 REM Highest difference peak 1.953, deepest hole -1.181, 1-sigma level 0.173 Q1 1 0.2723 0.5589 0.5708 11.00000 0.05 1.95 Q2 1 0.2717 0.4231 0.5720 11.00000 0.05 1.52 Q3 1 0.3101 0.5185 0.5279 11.00000 0.05 1.10 Q4 1 0.2903 0.4785 0.5489 11.00000 0.05 1.06 Q5 1 0.2472 0.5946 0.4490 11.00000 0.05 1.06 Q6 1 0.2462 0.4867 0.5513 11.00000 0.05 0.92 Q7 1 0.2345 0.5722 0.5518 11.00000 0.05 0.89 Q8 1 0.2677 0.5747 0.5332 11.00000 0.05 0.88 Q9 1 0.2358 0.5544 0.5776 11.00000 0.05 0.86 Q10 1 0.2623 0.4998 0.4687 11.00000 0.05 0.85 Q11 1 0.4538 1.1858 0.6421 11.00000 0.05 0.85 Q12 1 0.3046 0.5687 0.5636 11.00000 0.05 0.83 Q13 1 0.4462 1.3137 0.6993 11.00000 0.05 0.78 Q14 1 0.4250 1.3079 0.7557 11.00000 0.05 0.77 Q15 1 0.3019 0.9367 0.6699 11.00000 0.05 0.77 Q16 1 0.4825 1.0747 0.5470 11.00000 0.05 0.77 Q17 1 0.4224 1.0227 0.7458 11.00000 0.05 0.77 Q18 1 0.2361 0.4205 0.5552 11.00000 0.05 0.76 Q19 1 0.2684 0.4163 0.5301 11.00000 0.05 0.74 Q20 1 0.3246 0.9799 0.7017 11.00000 0.05 0.74 ; _shelx_res_checksum 89364 ####################################################################### # # 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_Himali45 _database_code_depnum_ccdc_archive 'CCDC 1867220' loop_ _audit_author_name _audit_author_address 'Frank R Fronczek' ;Louisiana State University United States of America ; _audit_update_record ; 2018-09-12 deposited with the CCDC. 2021-05-04 downloaded from the CCDC. ; _audit_creation_method SHELXL-2014/7 _shelx_SHELXL_version_number 2014/7 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C22 H19 Cl2 N3 O2 Pt S' _chemical_formula_sum 'C22 H19 Cl2 N3 O2 Pt S' _chemical_formula_weight 655.45 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system monoclinic _space_group_IT_number 15 _space_group_name_H-M_alt 'C 2/c' _space_group_name_Hall '-C 2yc' _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. ; 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' '-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 25.9376(10) _cell_length_b 9.6371(3) _cell_length_c 17.6498(6) _cell_angle_alpha 90 _cell_angle_beta 97.188(4) _cell_angle_gamma 90 _cell_volume 4377.1(3) _cell_formula_units_Z 8 _cell_measurement_temperature 100.0(5) _cell_measurement_reflns_used 9997 _cell_measurement_theta_min 2.26 _cell_measurement_theta_max 29.27 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.989 _exptl_crystal_F_000 2528 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.260 _exptl_crystal_size_mid 0.060 _exptl_crystal_size_min 0.020 _exptl_absorpt_coefficient_mu 6.776 _shelx_estimated_absorpt_T_min 0.272 _shelx_estimated_absorpt_T_max 0.876 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.632 _exptl_absorpt_correction_T_max 0.876 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2004)' _exptl_absorpt_special_details ? _diffrn_ambient_temperature 100.0(5) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'TRIUMPH curved graphite' _diffrn_measurement_device_type 'Bruker Kappa APEX-II DUO' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 40590 _diffrn_reflns_av_unetI/netI 0.0413 _diffrn_reflns_av_R_equivalents 0.0425 _diffrn_reflns_limit_h_min -37 _diffrn_reflns_limit_h_max 36 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.257 _diffrn_reflns_theta_max 30.562 _diffrn_reflns_theta_full 25.000 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measured_fraction_theta_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_point_group_measured_fraction_full 1.000 _reflns_number_total 6705 _reflns_number_gt 5248 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _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. ; _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ? _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0353P)^2^+5.0712P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 6705 _refine_ls_number_parameters 371 _refine_ls_number_restraints 75 _refine_ls_R_factor_all 0.0501 _refine_ls_R_factor_gt 0.0298 _refine_ls_wR_factor_ref 0.0697 _refine_ls_wR_factor_gt 0.0629 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.033 _refine_ls_shift/su_max 0.006 _refine_ls_shift/su_mean 0.000 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 Pt1 Pt 0.74038(2) 0.48291(2) 0.45334(2) 0.01900(5) Uani 1 1 d . . . . . Cl1 Cl 0.77094(4) 0.53219(9) 0.57799(5) 0.02717(19) Uani 1 1 d . . . . . Cl2 Cl 0.81924(4) 0.53538(10) 0.41388(6) 0.0303(2) Uani 1 1 d . . . . . S1 S 0.57754(4) 0.69968(10) 0.31948(6) 0.0304(2) Uani 1 1 d . . . . . N1 N 0.67013(11) 0.4383(3) 0.48639(16) 0.0203(6) Uani 1 1 d . . . . . N2 N 0.63499(12) 0.6718(3) 0.36541(18) 0.0281(7) Uani 1 1 d . . . . . N3 N 0.71316(11) 0.4299(3) 0.34434(16) 0.0208(6) Uani 1 1 d . . . . . C1 C 0.66169(14) 0.3116(4) 0.51394(19) 0.0242(8) Uani 1 1 d . . . . . H1 H 0.6881 0.2433 0.5143 0.029 Uiso 1 1 calc R U . . . C2 C 0.61606(15) 0.2772(4) 0.5417(2) 0.0326(9) Uani 1 1 d . . . . . H2 H 0.6111 0.1870 0.5612 0.039 Uiso 1 1 calc R U . . . C3 C 0.57770(16) 0.3764(5) 0.5406(2) 0.0381(10) Uani 1 1 d . . . . . H3 H 0.5462 0.3562 0.5605 0.046 Uiso 1 1 calc R U . . . C4 C 0.58558(17) 0.5048(4) 0.5102(2) 0.0325(9) Uani 1 1 d . . . . . H4 H 0.5589 0.5727 0.5075 0.039 Uiso 1 1 calc R U . . . C5 C 0.63219(15) 0.5359(4) 0.4836(2) 0.0249(8) Uani 1 1 d . . . . . C6 C 0.64173(14) 0.6756(4) 0.4497(2) 0.0263(8) Uani 1 1 d . . . . . H6A H 0.6173 0.7441 0.4671 0.032 Uiso 1 1 calc R U . . . H6B H 0.6775 0.7064 0.4683 0.032 Uiso 1 1 calc R U . . . C7 C 0.67957(15) 0.6673(4) 0.3218(2) 0.0269(8) Uani 1 1 d . . . . . H7A H 0.7109 0.7006 0.3546 0.032 Uiso 1 1 calc R U . . . H7B H 0.6730 0.7309 0.2776 0.032 Uiso 1 1 calc R U . . . C8 C 0.68988(15) 0.5235(4) 0.2933(2) 0.0244(8) Uani 1 1 d . . . . . C9 C 0.67534(17) 0.4829(4) 0.2182(2) 0.0317(9) Uani 1 1 d . . . . . H9 H 0.6598 0.5484 0.1821 0.038 Uiso 1 1 calc R U . . . C10 C 0.68316(16) 0.3490(5) 0.1955(2) 0.0344(9) Uani 1 1 d . . . . . H10 H 0.6738 0.3221 0.1439 0.041 Uiso 1 1 calc R U . . . C11 C 0.70499(15) 0.2537(4) 0.2492(2) 0.0308(9) Uani 1 1 d . . . . . H11 H 0.7095 0.1596 0.2354 0.037 Uiso 1 1 calc R U . . . C12 C 0.71992(14) 0.2985(4) 0.3227(2) 0.0262(8) Uani 1 1 d . . . . . H12 H 0.7355 0.2341 0.3594 0.031 Uiso 1 1 calc R U . . . O1 O 0.54104(17) 0.6971(6) 0.3813(3) 0.0289(12) Uani 0.570(4) 1 d . . P A 1 O2 O 0.5695(2) 0.6117(6) 0.2596(3) 0.0310(12) Uani 0.570(4) 1 d . . P A 1 C13 C 0.57922(18) 0.8733(7) 0.2890(4) 0.0254(15) Uani 0.570(4) 1 d D . P A 1 C14 C 0.55947(18) 0.8968(7) 0.2146(4) 0.0300(16) Uani 0.570(4) 1 d D . P A 1 H14 H 0.5515 0.8208 0.1809 0.036 Uiso 0.570(4) 1 calc R U P A 1 C15 C 0.55094(16) 1.0347(8) 0.1878(4) 0.0381(18) Uani 0.570(4) 1 d D U P A 1 C16 C 0.5302(3) 1.0598(11) 0.1095(6) 0.052(3) Uani 0.570(4) 1 d D U P A 1 H16 H 0.5221 0.9861 0.0743 0.062 Uiso 0.570(4) 1 calc R U P A 1 C17 C 0.5230(3) 1.1970(11) 0.0883(6) 0.067(3) Uani 0.570(4) 1 d D U P A 1 H17 H 0.5093 1.2188 0.0373 0.080 Uiso 0.570(4) 1 calc R U P A 1 C18 C 0.5357(3) 1.3081(11) 0.1425(6) 0.054(2) Uani 0.570(4) 1 d D U P A 1 H18 H 0.5301 1.4014 0.1262 0.064 Uiso 0.570(4) 1 calc R U P A 1 C19 C 0.5545(2) 1.2839(9) 0.2120(5) 0.055(2) Uani 0.570(4) 1 d D U P A 1 H19 H 0.5624 1.3593 0.2461 0.066 Uiso 0.570(4) 1 calc R U P A 1 C20 C 0.5635(2) 1.1445(8) 0.2390(5) 0.0415(19) Uani 0.570(4) 1 d D U P A 1 C21 C 0.5843(3) 1.1152(11) 0.3183(6) 0.0407(14) Uani 0.570(4) 1 d D . P A 1 H21 H 0.5923 1.1894 0.3532 0.049 Uiso 0.570(4) 1 calc R U P A 1 C22 C 0.5920(2) 0.9817(9) 0.3421(5) 0.0313(16) Uani 0.570(4) 1 d D . P A 1 H22 H 0.6056 0.9617 0.3934 0.038 Uiso 0.570(4) 1 calc R U P A 1 O1A O 0.5420(2) 0.6184(8) 0.3462(4) 0.0364(17) Uani 0.430(4) 1 d . . P A 2 O2A O 0.5843(3) 0.6811(8) 0.2311(4) 0.0371(18) Uani 0.430(4) 1 d . . P A 2 C13A C 0.5663(3) 0.8752(9) 0.3288(4) 0.027(2) Uani 0.430(4) 1 d D . P A 2 C14A C 0.5184(3) 0.9090(9) 0.3484(3) 0.0256(19) Uani 0.430(4) 1 d D . P A 2 H14A H 0.4944 0.8391 0.3586 0.031 Uiso 0.430(4) 1 calc R U P A 2 C15A C 0.5056(3) 1.0534(9) 0.3531(2) 0.0265(19) Uani 0.430(4) 1 d D . P A 2 C16A C 0.4559(4) 1.0932(10) 0.3734(4) 0.026(2) Uani 0.430(4) 1 d D . P A 2 H16A H 0.4311 1.0256 0.3839 0.032 Uiso 0.430(4) 1 calc R U P A 2 C17A C 0.4454(4) 1.2309(10) 0.3771(4) 0.054(4) Uani 0.430(4) 1 d D . P A 2 H17A H 0.4129 1.2615 0.3904 0.065 Uiso 0.430(4) 1 calc R U P A 2 C18A C 0.4836(4) 1.3293(13) 0.3608(4) 0.054(2) Uani 0.430(4) 1 d D . P A 2 H18A H 0.4753 1.4249 0.3637 0.064 Uiso 0.430(4) 1 calc R U P A 2 C19A C 0.5282(4) 1.2977(10) 0.3427(4) 0.040(3) Uani 0.430(4) 1 d D . P A 2 H19A H 0.5519 1.3683 0.3324 0.048 Uiso 0.430(4) 1 calc R U P A 2 C20A C 0.5420(3) 1.1543(9) 0.3379(3) 0.032(2) Uani 0.430(4) 1 d D . P A 2 C21A C 0.5932(5) 1.1147(14) 0.3167(5) 0.0407(14) Uani 0.430(4) 1 d D . P A 2 H21A H 0.6183 1.1812 0.3059 0.049 Uiso 0.430(4) 1 calc R U P A 2 C22A C 0.6017(4) 0.9772(12) 0.3139(4) 0.0313(16) Uani 0.430(4) 1 d D . P A 2 H22A H 0.6343 0.9474 0.3007 0.038 Uiso 0.430(4) 1 calc R U P A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.01924(7) 0.01660(7) 0.02066(7) 0.00388(5) 0.00056(5) 0.00117(5) Cl1 0.0319(5) 0.0238(5) 0.0238(4) 0.0029(3) -0.0042(4) -0.0036(4) Cl2 0.0237(5) 0.0306(5) 0.0369(5) 0.0103(4) 0.0049(4) -0.0028(4) S1 0.0249(5) 0.0223(5) 0.0413(6) 0.0030(4) -0.0060(4) 0.0021(4) N1 0.0222(15) 0.0196(14) 0.0188(14) -0.0015(12) 0.0019(12) 0.0009(12) N2 0.0222(16) 0.0267(17) 0.0336(17) 0.0037(14) -0.0034(13) 0.0049(13) N3 0.0211(15) 0.0196(15) 0.0221(15) 0.0038(12) 0.0042(12) 0.0001(12) C1 0.028(2) 0.0234(19) 0.0209(17) 0.0033(14) 0.0018(15) 0.0003(15) C2 0.033(2) 0.034(2) 0.031(2) 0.0128(17) 0.0036(17) -0.0036(17) C3 0.025(2) 0.052(3) 0.039(2) 0.010(2) 0.0086(18) 0.0012(19) C4 0.028(2) 0.037(2) 0.034(2) 0.0032(17) 0.0101(17) 0.0101(16) C5 0.027(2) 0.0217(19) 0.0257(18) -0.0014(15) 0.0031(15) 0.0007(15) C6 0.0229(19) 0.0230(19) 0.032(2) -0.0013(15) -0.0012(15) 0.0048(14) C7 0.030(2) 0.0206(19) 0.0285(19) 0.0088(15) -0.0017(16) 0.0027(15) C8 0.0242(19) 0.0234(19) 0.0250(18) 0.0048(15) 0.0010(15) -0.0004(14) C9 0.033(2) 0.035(2) 0.0252(19) 0.0073(16) -0.0003(16) 0.0033(17) C10 0.041(2) 0.042(3) 0.0211(19) -0.0036(17) 0.0055(17) 0.0066(19) C11 0.034(2) 0.031(2) 0.029(2) -0.0029(17) 0.0082(17) 0.0054(17) C12 0.027(2) 0.025(2) 0.0285(19) 0.0003(15) 0.0074(15) 0.0052(15) O1 0.023(3) 0.033(3) 0.031(3) 0.008(2) 0.006(2) 0.003(2) O2 0.032(3) 0.027(3) 0.032(3) -0.002(2) -0.007(2) -0.001(2) C13 0.025(4) 0.017(3) 0.034(4) 0.003(3) 0.004(3) 0.004(3) C14 0.022(3) 0.035(4) 0.036(4) 0.014(3) 0.011(3) 0.005(3) C15 0.034(3) 0.041(3) 0.041(3) 0.015(3) 0.012(3) 0.010(3) C16 0.050(5) 0.054(5) 0.052(4) 0.013(4) 0.007(4) 0.005(4) C17 0.067(5) 0.069(5) 0.065(4) 0.026(4) 0.015(4) 0.006(4) C18 0.047(5) 0.057(3) 0.063(3) 0.009(4) 0.028(3) 0.007(3) C19 0.050(4) 0.047(4) 0.072(4) 0.012(3) 0.024(3) 0.005(3) C20 0.032(3) 0.039(3) 0.057(4) 0.014(3) 0.019(3) 0.002(3) C21 0.019(3) 0.027(2) 0.079(4) -0.003(2) 0.019(3) -0.005(2) C22 0.031(4) 0.031(3) 0.031(5) -0.003(4) 0.004(3) 0.004(3) O1A 0.021(3) 0.030(4) 0.054(5) 0.001(4) -0.011(3) 0.000(3) O2A 0.039(4) 0.039(5) 0.031(4) -0.008(3) -0.007(3) 0.010(3) C13A 0.023(5) 0.027(5) 0.029(5) 0.000(4) -0.007(4) 0.011(4) C14A 0.027(5) 0.030(5) 0.019(4) 0.000(3) 0.001(3) 0.004(3) C15A 0.024(4) 0.034(5) 0.023(4) 0.005(4) 0.005(3) 0.008(4) C16A 0.021(5) 0.026(5) 0.032(6) -0.002(4) 0.007(4) 0.009(4) C17A 0.082(10) 0.028(6) 0.061(8) 0.001(6) 0.041(7) 0.019(6) C18A 0.047(5) 0.057(3) 0.063(3) 0.009(4) 0.028(3) 0.007(3) C19A 0.061(7) 0.029(5) 0.033(5) 0.005(4) 0.015(5) 0.008(5) C20A 0.037(6) 0.035(5) 0.025(5) 0.000(4) 0.008(4) -0.007(4) C21A 0.019(3) 0.027(2) 0.079(4) -0.003(2) 0.019(3) -0.005(2) C22A 0.031(4) 0.031(3) 0.031(5) -0.003(4) 0.004(3) 0.004(3) _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 Pt1 N1 2.028(3) . ? Pt1 N3 2.030(3) . ? Pt1 Cl1 2.2930(9) . ? Pt1 Cl2 2.2980(9) . ? S1 O1A 1.340(7) . ? S1 O2 1.350(5) . ? S1 O1 1.532(5) . ? S1 O2A 1.601(7) . ? S1 N2 1.627(3) . ? S1 C13A 1.728(9) . ? S1 C13 1.759(6) . ? N1 C1 1.342(5) . ? N1 C5 1.358(5) . ? N2 C7 1.468(5) . ? N2 C6 1.477(5) . ? N3 C12 1.340(5) . ? N3 C8 1.362(5) . ? C1 C2 1.377(5) . ? C1 H1 0.9500 . ? C2 C3 1.378(6) . ? C2 H2 0.9500 . ? C3 C4 1.374(6) . ? C3 H3 0.9500 . ? C4 C5 1.383(6) . ? C4 H4 0.9500 . ? C5 C6 1.507(5) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.509(5) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.388(6) . ? C9 C10 1.373(6) . ? C9 H9 0.9500 . ? C10 C11 1.388(5) . ? C10 H10 0.9500 . ? C11 C12 1.377(5) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C14 1.368(9) . ? C13 C22 1.415(9) . ? C14 C15 1.419(9) . ? C14 H14 0.9500 . ? C15 C20 1.403(10) . ? C15 C16 1.439(11) . ? C16 C17 1.381(12) . ? C16 H16 0.9500 . ? C17 C18 1.445(12) . ? C17 H17 0.9500 . ? C18 C19 1.283(11) . ? C18 H18 0.9500 . ? C19 C20 1.434(10) . ? C19 H19 0.9500 . ? C20 C21 1.463(11) . ? C21 C22 1.361(10) . ? C21 H21 0.9500 . ? C22 H22 0.9500 . ? C13A C14A 1.372(10) . ? C13A C22A 1.391(12) . ? C14A C15A 1.435(11) . ? C14A H14A 0.9500 . ? C15A C20A 1.402(11) . ? C15A C16A 1.434(11) . ? C16A C17A 1.358(12) . ? C16A H16A 0.9500 . ? C17A C18A 1.427(13) . ? C17A H17A 0.9500 . ? C18A C19A 1.274(13) . ? C18A H18A 0.9500 . ? C19A C20A 1.433(11) . ? C19A H19A 0.9500 . ? C20A C21A 1.475(13) . ? C21A C22A 1.345(12) . ? C21A H21A 0.9500 . ? C22A H22A 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 N1 Pt1 N3 90.05(11) . . ? N1 Pt1 Cl1 89.03(8) . . ? N3 Pt1 Cl1 177.34(9) . . ? N1 Pt1 Cl2 178.95(8) . . ? N3 Pt1 Cl2 89.16(8) . . ? Cl1 Pt1 Cl2 91.79(4) . . ? O2 S1 O1 120.0(3) . . ? O1A S1 O2A 116.3(4) . . ? O1A S1 N2 110.8(3) . . ? O2 S1 N2 109.1(2) . . ? O1 S1 N2 104.6(2) . . ? O2A S1 N2 105.1(3) . . ? O1A S1 C13A 114.1(4) . . ? O2A S1 C13A 104.0(4) . . ? N2 S1 C13A 105.6(3) . . ? O2 S1 C13 111.4(3) . . ? O1 S1 C13 105.9(3) . . ? N2 S1 C13 104.7(2) . . ? C1 N1 C5 119.5(3) . . ? C1 N1 Pt1 119.4(2) . . ? C5 N1 Pt1 121.1(3) . . ? C7 N2 C6 121.8(3) . . ? C7 N2 S1 118.4(3) . . ? C6 N2 S1 118.9(2) . . ? C12 N3 C8 120.1(3) . . ? C12 N3 Pt1 117.7(2) . . ? C8 N3 Pt1 122.2(2) . . ? N1 C1 C2 122.3(4) . . ? N1 C1 H1 118.8 . . ? C2 C1 H1 118.8 . . ? C1 C2 C3 118.6(4) . . ? C1 C2 H2 120.7 . . ? C3 C2 H2 120.7 . . ? C4 C3 C2 119.2(4) . . ? C4 C3 H3 120.4 . . ? C2 C3 H3 120.4 . . ? C3 C4 C5 120.4(4) . . ? C3 C4 H4 119.8 . . ? C5 C4 H4 119.8 . . ? N1 C5 C4 119.9(3) . . ? N1 C5 C6 118.6(3) . . ? C4 C5 C6 121.5(3) . . ? N2 C6 C5 111.9(3) . . ? N2 C6 H6A 109.2 . . ? C5 C6 H6A 109.2 . . ? N2 C6 H6B 109.2 . . ? C5 C6 H6B 109.2 . . ? H6A C6 H6B 107.9 . . ? N2 C7 C8 112.7(3) . . ? N2 C7 H7A 109.0 . . ? C8 C7 H7A 109.0 . . ? N2 C7 H7B 109.0 . . ? C8 C7 H7B 109.0 . . ? H7A C7 H7B 107.8 . . ? N3 C8 C9 119.3(3) . . ? N3 C8 C7 118.0(3) . . ? C9 C8 C7 122.6(3) . . ? C10 C9 C8 120.8(4) . . ? C10 C9 H9 119.6 . . ? C8 C9 H9 119.6 . . ? C9 C10 C11 119.0(4) . . ? C9 C10 H10 120.5 . . ? C11 C10 H10 120.5 . . ? C12 C11 C10 118.6(4) . . ? C12 C11 H11 120.7 . . ? C10 C11 H11 120.7 . . ? N3 C12 C11 122.2(4) . . ? N3 C12 H12 118.9 . . ? C11 C12 H12 118.9 . . ? C14 C13 C22 122.8(7) . . ? C14 C13 S1 115.5(5) . . ? C22 C13 S1 120.8(6) . . ? C13 C14 C15 119.9(7) . . ? C13 C14 H14 120.0 . . ? C15 C14 H14 120.0 . . ? C20 C15 C14 118.6(7) . . ? C20 C15 C16 121.3(8) . . ? C14 C15 C16 120.1(8) . . ? C17 C16 C15 116.3(10) . . ? C17 C16 H16 121.9 . . ? C15 C16 H16 121.9 . . ? C16 C17 C18 121.2(10) . . ? C16 C17 H17 119.4 . . ? C18 C17 H17 119.4 . . ? C19 C18 C17 121.7(10) . . ? C19 C18 H18 119.2 . . ? C17 C18 H18 119.2 . . ? C18 C19 C20 121.0(10) . . ? C18 C19 H19 119.5 . . ? C20 C19 H19 119.5 . . ? C15 C20 C19 118.5(8) . . ? C15 C20 C21 119.9(7) . . ? C19 C20 C21 121.6(8) . . ? C22 C21 C20 120.1(9) . . ? C22 C21 H21 120.0 . . ? C20 C21 H21 120.0 . . ? C21 C22 C13 118.7(8) . . ? C21 C22 H22 120.7 . . ? C13 C22 H22 120.7 . . ? C14A C13A C22A 121.3(9) . . ? C14A C13A S1 115.2(7) . . ? C22A C13A S1 123.4(7) . . ? C13A C14A C15A 117.8(8) . . ? C13A C14A H14A 121.1 . . ? C15A C14A H14A 121.1 . . ? C20A C15A C16A 120.6(8) . . ? C20A C15A C14A 119.8(7) . . ? C16A C15A C14A 119.6(8) . . ? C17A C16A C15A 117.8(9) . . ? C17A C16A H16A 121.1 . . ? C15A C16A H16A 121.1 . . ? C16A C17A C18A 119.4(10) . . ? C16A C17A H17A 120.3 . . ? C18A C17A H17A 120.3 . . ? C19A C18A C17A 124.6(12) . . ? C19A C18A H18A 117.7 . . ? C17A C18A H18A 117.7 . . ? C18A C19A C20A 119.1(10) . . ? C18A C19A H19A 120.5 . . ? C20A C19A H19A 120.5 . . ? C15A C20A C19A 118.6(8) . . ? C15A C20A C21A 121.1(9) . . ? C19A C20A C21A 120.3(9) . . ? C22A C21A C20A 114.9(11) . . ? C22A C21A H21A 122.6 . . ? C20A C21A H21A 122.6 . . ? C21A C22A C13A 125.0(10) . . ? C21A C22A H22A 117.5 . . ? C13A C22A H22A 117.5 . . ? _refine_diff_density_max 2.522 _refine_diff_density_min -1.195 _refine_diff_density_rms 0.162 _shelx_res_file ; shelxl.res created by SHELXL-2014/7 TITL Himali45 in C2/c CELL 0.71073 25.9376 9.6371 17.6498 90.000 97.188 90.000 ZERR 8.00 0.0010 0.0003 0.0006 0.000 0.004 0.000 LATT 7 SYMM - X, Y, 1/2 - Z SFAC C H N O S CL PT UNIT 176 152 24 16 8 16 8 MERG 2 ACTA 50 FLAT 0.005 C13 > C22 FLAT 0.005 C13A > C22A REM SADI C13 C14 C14 C15 C15 C16 C16 C17 C17 C18 C18 C19 C19 C20 C20 C21 C21 C22 REM C22 C13 C15 C20 C13A C14A C14A C15A C15A C16A C16A C17A C17A C18A = REM C18A C19A C19A C20A C20A C21A C21A C22A C22A C13A C15A C20A EADP C21 C21A EADP C22 C22A EADP C18 C18A ISOR 0.005 C15 > C20 FMAP 2 PLAN 10 SIZE 0.02 0.06 0.26 BOND $H L.S. 15 TEMP -173.00 WGHT 0.035300 5.071200 FVAR 0.09533 0.56983 PT1 7 0.740377 0.482910 0.453336 11.00000 0.01924 0.01660 = 0.02066 0.00388 0.00056 0.00117 CL1 6 0.770941 0.532186 0.577989 11.00000 0.03192 0.02383 = 0.02381 0.00289 -0.00423 -0.00359 CL2 6 0.819237 0.535379 0.413880 11.00000 0.02369 0.03055 = 0.03689 0.01029 0.00495 -0.00279 S1 5 0.577541 0.699680 0.319478 11.00000 0.02489 0.02231 = 0.04132 0.00298 -0.00602 0.00205 N1 3 0.670130 0.438275 0.486392 11.00000 0.02222 0.01958 = 0.01884 -0.00148 0.00195 0.00090 N2 3 0.634986 0.671798 0.365406 11.00000 0.02215 0.02671 = 0.03360 0.00366 -0.00337 0.00494 N3 3 0.713159 0.429875 0.344345 11.00000 0.02109 0.01956 = 0.02210 0.00379 0.00425 0.00009 C1 1 0.661688 0.311620 0.513944 11.00000 0.02784 0.02340 = 0.02091 0.00328 0.00182 0.00033 AFIX 43 H1 2 0.688125 0.243308 0.514320 11.00000 -1.20000 AFIX 0 C2 1 0.616063 0.277216 0.541681 11.00000 0.03312 0.03375 = 0.03078 0.01276 0.00360 -0.00355 AFIX 43 H2 2 0.611123 0.186969 0.561196 11.00000 -1.20000 AFIX 0 C3 1 0.577705 0.376402 0.540551 11.00000 0.02519 0.05162 = 0.03878 0.00981 0.00859 0.00116 AFIX 43 H3 2 0.546185 0.356222 0.560519 11.00000 -1.20000 AFIX 0 C4 1 0.585584 0.504846 0.510200 11.00000 0.02845 0.03700 = 0.03362 0.00317 0.01009 0.01013 AFIX 43 H4 2 0.558857 0.572729 0.507460 11.00000 -1.20000 AFIX 0 C5 1 0.632189 0.535891 0.483617 11.00000 0.02719 0.02174 = 0.02567 -0.00140 0.00306 0.00075 C6 1 0.641734 0.675649 0.449727 11.00000 0.02285 0.02296 = 0.03200 -0.00134 -0.00117 0.00480 AFIX 23 H6A 2 0.617301 0.744130 0.467120 11.00000 -1.20000 H6B 2 0.677508 0.706366 0.468318 11.00000 -1.20000 AFIX 0 C7 1 0.679571 0.667263 0.321794 11.00000 0.03015 0.02058 = 0.02849 0.00883 -0.00170 0.00272 AFIX 23 H7A 2 0.710882 0.700613 0.354580 11.00000 -1.20000 H7B 2 0.673049 0.730949 0.277623 11.00000 -1.20000 AFIX 0 C8 1 0.689881 0.523549 0.293276 11.00000 0.02424 0.02337 = 0.02501 0.00479 0.00098 -0.00041 C9 1 0.675337 0.482865 0.218235 11.00000 0.03328 0.03549 = 0.02524 0.00728 -0.00030 0.00335 AFIX 43 H9 2 0.659790 0.548357 0.182141 11.00000 -1.20000 AFIX 0 C10 1 0.683157 0.349023 0.195541 11.00000 0.04094 0.04172 = 0.02107 -0.00356 0.00549 0.00665 AFIX 43 H10 2 0.673766 0.322068 0.143884 11.00000 -1.20000 AFIX 0 C11 1 0.704986 0.253672 0.249190 11.00000 0.03411 0.03062 = 0.02890 -0.00294 0.00819 0.00537 AFIX 43 H11 2 0.709520 0.159553 0.235449 11.00000 -1.20000 AFIX 0 C12 1 0.719921 0.298462 0.322742 11.00000 0.02674 0.02451 = 0.02846 0.00025 0.00738 0.00523 AFIX 43 H12 2 0.735543 0.234069 0.359410 11.00000 -1.20000 AFIX 0 PART 1 O1 4 0.541044 0.697131 0.381302 21.00000 0.02282 0.03336 = 0.03130 0.00837 0.00596 0.00328 O2 4 0.569543 0.611700 0.259612 21.00000 0.03169 0.02680 = 0.03169 -0.00208 -0.00721 -0.00053 SAME C13A C14A C15A C16A C17A C18A C19A C20A C21A C22A C13 1 0.579221 0.873265 0.289043 21.00000 0.02525 0.01664 = 0.03437 0.00259 0.00384 0.00447 C14 1 0.559467 0.896754 0.214592 21.00000 0.02158 0.03455 = 0.03577 0.01354 0.01125 0.00540 AFIX 43 H14 2 0.551469 0.820789 0.180861 21.00000 -1.20000 AFIX 0 C15 1 0.550939 1.034719 0.187813 21.00000 0.03380 0.04098 = 0.04129 0.01471 0.01159 0.01037 C16 1 0.530246 1.059804 0.109502 21.00000 0.04954 0.05416 = 0.05236 0.01331 0.00692 0.00533 AFIX 43 H16 2 0.522052 0.986062 0.074333 21.00000 -1.20000 AFIX 0 C17 1 0.522969 1.197012 0.088342 21.00000 0.06684 0.06919 = 0.06545 0.02628 0.01484 0.00566 AFIX 43 H17 2 0.509309 1.218818 0.037264 21.00000 -1.20000 AFIX 0 C18 1 0.535746 1.308104 0.142462 21.00000 0.04670 0.05723 = 0.06252 0.00907 0.02764 0.00665 AFIX 43 H18 2 0.530147 1.401435 0.126150 21.00000 -1.20000 AFIX 0 C19 1 0.554463 1.283870 0.211984 21.00000 0.05017 0.04661 = 0.07219 0.01221 0.02414 0.00540 AFIX 43 H19 2 0.562435 1.359324 0.246079 21.00000 -1.20000 AFIX 0 C20 1 0.563522 1.144525 0.238963 21.00000 0.03201 0.03896 = 0.05690 0.01394 0.01881 0.00198 C21 1 0.584255 1.115171 0.318279 21.00000 0.01857 0.02732 = 0.07926 -0.00345 0.01860 -0.00459 AFIX 43 H21 2 0.592344 1.189405 0.353160 21.00000 -1.20000 AFIX 0 C22 1 0.591964 0.981676 0.342146 21.00000 0.03148 0.03135 = 0.03103 -0.00339 0.00418 0.00374 AFIX 43 H22 2 0.605633 0.961663 0.393450 21.00000 -1.20000 AFIX 0 PART 2 O1A 4 0.542002 0.618387 0.346225 -21.00000 0.02089 0.03039 = 0.05389 0.00059 -0.01097 -0.00049 O2A 4 0.584340 0.681127 0.231134 -21.00000 0.03866 0.03878 = 0.03099 -0.00787 -0.00672 0.00979 C13A 1 0.566348 0.875237 0.328795 -21.00000 0.02323 0.02721 = 0.02873 0.00006 -0.00690 0.01106 C14A 1 0.518375 0.909043 0.348431 -21.00000 0.02697 0.03003 = 0.01944 0.00027 0.00148 0.00362 AFIX 43 H14A 2 0.494364 0.839113 0.358629 -21.00000 -1.20000 AFIX 0 C15A 1 0.505646 1.053431 0.353065 -21.00000 0.02351 0.03383 = 0.02263 0.00466 0.00512 0.00795 C16A 1 0.455904 1.093247 0.373402 -21.00000 0.02117 0.02629 = 0.03242 -0.00173 0.00706 0.00879 AFIX 43 H16A 2 0.431141 1.025565 0.383942 -21.00000 -1.20000 AFIX 0 C17A 1 0.445387 1.230948 0.377087 -21.00000 0.08193 0.02761 = 0.06111 0.00118 0.04057 0.01850 AFIX 43 H17A 2 0.412876 1.261524 0.390382 -21.00000 -1.20000 AFIX 0 C18A 1 0.483628 1.329261 0.360803 -21.00000 0.04670 0.05723 = 0.06252 0.00907 0.02764 0.00665 AFIX 43 H18A 2 0.475287 1.424948 0.363685 -21.00000 -1.20000 AFIX 0 C19A 1 0.528179 1.297681 0.342668 -21.00000 0.06059 0.02880 = 0.03341 0.00461 0.01518 0.00837 AFIX 43 H19A 2 0.551929 1.368254 0.332435 -21.00000 -1.20000 AFIX 0 C20A 1 0.541972 1.154266 0.337917 -21.00000 0.03698 0.03493 = 0.02496 0.00044 0.00759 -0.00662 C21A 1 0.593214 1.114673 0.316695 -21.00000 0.01857 0.02732 = 0.07926 -0.00345 0.01860 -0.00459 AFIX 43 H21A 2 0.618309 1.181203 0.305858 -21.00000 -1.20000 AFIX 0 C22A 1 0.601683 0.977151 0.313867 -21.00000 0.03148 0.03135 = 0.03103 -0.00339 0.00418 0.00374 AFIX 43 H22A 2 0.634312 0.947355 0.300654 -21.00000 -1.20000 AFIX 0 HKLF 4 REM Himali45 in C2/c REM R1 = 0.0298 for 5248 Fo > 4sig(Fo) and 0.0501 for all 6705 data REM 371 parameters refined using 75 restraints END WGHT 0.0353 5.0618 REM Highest difference peak 2.522, deepest hole -1.195, 1-sigma level 0.162 Q1 1 0.7404 0.5675 0.4531 11.00000 0.05 2.52 Q2 1 0.7081 0.5129 0.4642 11.00000 0.05 1.30 Q3 1 0.7464 0.3844 0.4477 11.00000 0.05 1.29 Q4 1 0.7709 0.4108 0.4446 11.00000 0.05 1.28 Q5 1 0.7140 0.4025 0.4629 11.00000 0.05 1.19 Q6 1 0.7102 0.5439 0.4171 11.00000 0.05 1.17 Q7 1 0.7781 0.5353 0.4504 11.00000 0.05 1.17 Q8 1 0.7791 0.4776 0.6422 11.00000 0.05 1.15 Q9 1 0.5197 1.2771 0.1180 11.00000 0.05 1.11 Q10 1 0.5320 1.3408 0.1619 11.00000 0.05 0.85 ; _shelx_res_checksum 55873 ####################################################################### # # 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_Himali39 _database_code_depnum_ccdc_archive 'CCDC 1867222' loop_ _audit_author_name _audit_author_address 'Frank R Fronczek' ;Louisiana State University United States of America ; _audit_update_record ; 2018-09-12 deposited with the CCDC. 2021-05-04 downloaded from the CCDC. ; # start Validation Reply Form _vrf_PLAT971_Himali39 ; PROBLEM: Check Calcd Resid. Dens. 0.61A From Pt1 3.96 eA-3 RESPONSE: vrf reply has been inserted into the CIF file ; _vrf_PLAT971_Himali39_2 ; PROBLEM: Check Calcd Resid. Dens. 0.57A From Pt1 3.34 eA-3 RESPONSE: vrf reply into the Himali39 CIF ; # Added during the CSD deposition process: Wednesday 12 September 2018 04:43 AM # end Validation Reply Form _audit_creation_method SHELXL-2014/7 _shelx_SHELXL_version_number 2014/7 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C17 H22 Cl2 N4 O2 Pt S' _chemical_formula_sum 'C17 H22 Cl2 N4 O2 Pt S' _chemical_formula_weight 612.43 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system monoclinic _space_group_IT_number 15 _space_group_name_H-M_alt 'I 2/a' _space_group_name_Hall '-I 2ya' _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. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y, -z' 'x+1/2, y+1/2, z+1/2' '-x+1, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y, z' '-x+1/2, -y+1/2, -z+1/2' 'x, -y+1/2, z+1/2' _cell_length_a 17.5316(5) _cell_length_b 9.5135(2) _cell_length_c 24.2020(9) _cell_angle_alpha 90 _cell_angle_beta 91.872(2) _cell_angle_gamma 90 _cell_volume 4034.4(2) _cell_formula_units_Z 8 _cell_measurement_temperature 90.0(5) _cell_measurement_reflns_used 5775 _cell_measurement_theta_min 3.29 _cell_measurement_theta_max 36.19 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 2.017 _exptl_crystal_F_000 2368 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.160 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_min 0.040 _exptl_absorpt_coefficient_mu 7.345 _shelx_estimated_absorpt_T_min 0.386 _shelx_estimated_absorpt_T_max 0.758 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.570 _exptl_absorpt_correction_T_max 0.758 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2004)' _exptl_absorpt_special_details ? _diffrn_ambient_temperature 90.0(5) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'TRIUMPH curved graphite' _diffrn_measurement_device_type 'Bruker Kappa APEX-II DUO' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 33042 _diffrn_reflns_av_unetI/netI 0.0756 _diffrn_reflns_av_R_equivalents 0.0647 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -41 _diffrn_reflns_limit_l_max 42 _diffrn_reflns_theta_min 3.291 _diffrn_reflns_theta_max 38.593 _diffrn_reflns_theta_full 25.000 _diffrn_measured_fraction_theta_max 0.989 _diffrn_measured_fraction_theta_full 0.990 _diffrn_reflns_Laue_measured_fraction_max 0.989 _diffrn_reflns_Laue_measured_fraction_full 0.990 _diffrn_reflns_point_group_measured_fraction_max 0.989 _diffrn_reflns_point_group_measured_fraction_full 0.990 _reflns_number_total 11296 _reflns_number_gt 8144 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _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. ; _computing_data_collection 'Bruker APEX3' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ? _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0294P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 11296 _refine_ls_number_parameters 244 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0704 _refine_ls_R_factor_gt 0.0397 _refine_ls_wR_factor_ref 0.0767 _refine_ls_wR_factor_gt 0.0688 _refine_ls_goodness_of_fit_ref 0.979 _refine_ls_restrained_S_all 0.979 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 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 Pt1 Pt 0.29652(2) 0.51601(2) 0.25999(2) 0.00908(3) Uani 1 1 d . . . . . Cl1 Cl 0.17402(4) 0.47806(8) 0.22646(3) 0.01430(12) Uani 1 1 d . . . . . Cl2 Cl 0.34630(4) 0.47725(8) 0.17435(3) 0.01474(13) Uani 1 1 d . . . . . S1 S 0.40730(5) 0.25938(8) 0.43016(3) 0.01370(14) Uani 1 1 d . . . . . O1 O 0.35369(15) 0.3011(3) 0.47040(10) 0.0209(5) Uani 1 1 d . . . . . O2 O 0.48399(15) 0.3100(3) 0.43203(10) 0.0189(5) Uani 1 1 d . . . . . N1 N 0.25367(14) 0.5475(3) 0.33604(10) 0.0099(4) Uani 1 1 d . . . . . N2 N 0.37051(16) 0.3112(3) 0.37050(11) 0.0130(5) Uani 1 1 d . . . . . N3 N 0.40277(15) 0.5622(3) 0.28889(10) 0.0109(4) Uani 1 1 d . . . . . N4 N 0.41292(16) 0.0884(3) 0.43384(12) 0.0155(5) Uani 1 1 d . . . . . C1 C 0.22370(18) 0.6754(3) 0.34738(14) 0.0141(5) Uani 1 1 d . . . . . H1 H 0.2289 0.7496 0.3215 0.017 Uiso 1 1 calc R U . . . C2 C 0.1858(2) 0.7005(3) 0.39564(14) 0.0164(6) Uani 1 1 d . . . . . H2 H 0.1657 0.7910 0.4030 0.020 Uiso 1 1 calc R U . . . C3 C 0.1776(2) 0.5917(4) 0.43306(14) 0.0177(6) Uani 1 1 d . . . . . H3 H 0.1499 0.6053 0.4657 0.021 Uiso 1 1 calc R U . . . C4 C 0.21053(19) 0.4625(3) 0.42203(13) 0.0158(6) Uani 1 1 d . . . . . H4 H 0.2067 0.3876 0.4477 0.019 Uiso 1 1 calc R U . . . C5 C 0.24896(18) 0.4427(3) 0.37359(12) 0.0117(5) Uani 1 1 d . . . . . C6 C 0.28689(18) 0.3043(3) 0.36137(13) 0.0128(5) Uani 1 1 d . . . . . H6A H 0.2659 0.2305 0.3854 0.015 Uiso 1 1 calc R U . . . H6B H 0.2751 0.2777 0.3225 0.015 Uiso 1 1 calc R U . . . C7 C 0.42058(19) 0.3216(3) 0.32308(13) 0.0132(5) Uani 1 1 d . . . . . H7A H 0.3920 0.2904 0.2893 0.016 Uiso 1 1 calc R U . . . H7B H 0.4645 0.2574 0.3291 0.016 Uiso 1 1 calc R U . . . C8 C 0.44991(18) 0.4690(3) 0.31424(13) 0.0125(5) Uani 1 1 d . . . . . C9 C 0.52346(19) 0.5084(3) 0.33070(14) 0.0168(6) Uani 1 1 d . . . . . H9 H 0.5566 0.4420 0.3483 0.020 Uiso 1 1 calc R U . . . C10 C 0.5487(2) 0.6441(4) 0.32154(14) 0.0178(6) Uani 1 1 d . . . . . H10 H 0.5992 0.6712 0.3323 0.021 Uiso 1 1 calc R U . . . C11 C 0.49956(19) 0.7389(3) 0.29660(14) 0.0157(6) Uani 1 1 d . . . . . H11 H 0.5153 0.8331 0.2905 0.019 Uiso 1 1 calc R U . . . C12 C 0.42675(19) 0.6957(3) 0.28041(14) 0.0140(5) Uani 1 1 d . . . . . H12 H 0.3928 0.7612 0.2630 0.017 Uiso 1 1 calc R U . . . C13 C 0.47092(19) 0.0155(3) 0.40125(13) 0.0161(5) Uani 1 1 d . . . . . H13A H 0.5170 0.0749 0.3988 0.019 Uiso 1 1 calc R U . . . H13B H 0.4504 -0.0026 0.3633 0.019 Uiso 1 1 calc R U . . . C14 C 0.4913(2) -0.1227(4) 0.42954(15) 0.0194(6) Uani 1 1 d . . . . . H14A H 0.5156 -0.1033 0.4662 0.023 Uiso 1 1 calc R U . . . H14B H 0.5286 -0.1741 0.4072 0.023 Uiso 1 1 calc R U . . . C15 C 0.4209(2) -0.2139(4) 0.43665(16) 0.0239(8) Uani 1 1 d . . . . . H15A H 0.4352 -0.3000 0.4575 0.029 Uiso 1 1 calc R U . . . H15B H 0.3998 -0.2425 0.3999 0.029 Uiso 1 1 calc R U . . . C16 C 0.3606(2) -0.1326(4) 0.46768(16) 0.0212(7) Uani 1 1 d . . . . . H16A H 0.3137 -0.1901 0.4696 0.025 Uiso 1 1 calc R U . . . H16B H 0.3796 -0.1142 0.5060 0.025 Uiso 1 1 calc R U . . . C17 C 0.3416(2) 0.0066(4) 0.43912(15) 0.0200(6) Uani 1 1 d . . . . . H17A H 0.3180 -0.0112 0.4021 0.024 Uiso 1 1 calc R U . . . H17B H 0.3049 0.0603 0.4611 0.024 Uiso 1 1 calc R U . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.00990(4) 0.01001(4) 0.00734(4) 0.00102(4) 0.00040(3) 0.00172(4) Cl1 0.0123(3) 0.0170(3) 0.0135(3) -0.0021(2) -0.0016(2) 0.0018(3) Cl2 0.0160(3) 0.0175(3) 0.0108(3) 0.0009(2) 0.0028(2) 0.0037(3) S1 0.0159(4) 0.0168(3) 0.0084(3) -0.0001(2) -0.0003(3) 0.0020(3) O1 0.0240(13) 0.0271(12) 0.0119(11) -0.0028(9) 0.0030(9) 0.0068(10) O2 0.0196(12) 0.0204(11) 0.0164(12) -0.0002(9) -0.0042(9) -0.0008(9) N1 0.0098(10) 0.0108(10) 0.0091(10) 0.0002(8) 0.0018(8) -0.0001(8) N2 0.0137(12) 0.0170(11) 0.0083(11) 0.0023(9) 0.0003(9) 0.0035(9) N3 0.0117(11) 0.0124(10) 0.0087(11) -0.0012(8) 0.0006(9) 0.0006(9) N4 0.0151(13) 0.0178(12) 0.0137(12) 0.0025(9) 0.0017(10) 0.0032(10) C1 0.0141(14) 0.0130(12) 0.0150(14) -0.0013(10) 0.0000(11) 0.0021(10) C2 0.0175(15) 0.0179(14) 0.0138(14) -0.0021(11) 0.0015(11) 0.0027(12) C3 0.0169(15) 0.0231(15) 0.0131(14) -0.0016(11) 0.0026(12) 0.0031(12) C4 0.0158(14) 0.0184(14) 0.0133(13) 0.0027(10) 0.0034(11) -0.0005(11) C5 0.0117(12) 0.0137(11) 0.0097(12) 0.0029(9) 0.0008(10) 0.0011(10) C6 0.0143(13) 0.0122(12) 0.0119(13) 0.0017(10) 0.0020(10) 0.0013(10) C7 0.0148(14) 0.0129(12) 0.0119(13) 0.0007(10) -0.0006(11) 0.0030(10) C8 0.0125(12) 0.0147(13) 0.0103(12) -0.0003(10) -0.0002(10) 0.0017(10) C9 0.0124(12) 0.0205(14) 0.0174(14) 0.0031(11) -0.0003(10) 0.0019(11) C10 0.0137(15) 0.0232(15) 0.0167(15) -0.0035(12) 0.0012(12) -0.0025(12) C11 0.0162(14) 0.0151(13) 0.0161(14) -0.0022(11) 0.0029(11) -0.0039(11) C12 0.0141(13) 0.0138(12) 0.0143(14) 0.0000(10) 0.0032(11) -0.0017(11) C13 0.0170(14) 0.0182(13) 0.0131(13) -0.0009(11) 0.0025(10) 0.0015(12) C14 0.0219(17) 0.0211(15) 0.0149(15) 0.0009(12) -0.0046(13) 0.0047(13) C15 0.036(2) 0.0156(14) 0.0198(17) 0.0005(12) -0.0057(15) -0.0026(14) C16 0.0221(17) 0.0205(15) 0.0207(17) 0.0078(12) -0.0019(14) -0.0036(13) C17 0.0177(14) 0.0222(16) 0.0203(15) 0.0049(12) 0.0019(12) -0.0027(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 N3 2.017(3) . ? Pt1 N1 2.033(2) . ? Pt1 Cl1 2.2996(8) . ? Pt1 Cl2 2.3048(7) . ? S1 O2 1.428(3) . ? S1 O1 1.432(3) . ? S1 N4 1.632(3) . ? S1 N2 1.638(3) . ? N1 C5 1.353(4) . ? N1 C1 1.357(4) . ? N2 C7 1.471(4) . ? N2 C6 1.477(4) . ? N3 C8 1.346(4) . ? N3 C12 1.356(4) . ? N4 C13 1.480(4) . ? N4 C17 1.481(4) . ? C1 C2 1.384(5) . ? C1 H1 0.9500 . ? C2 C3 1.386(5) . ? C2 H2 0.9500 . ? C3 C4 1.387(5) . ? C3 H3 0.9500 . ? C4 C5 1.384(4) . ? C4 H4 0.9500 . ? C5 C6 1.509(4) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.511(4) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.389(5) . ? C9 C10 1.385(5) . ? C9 H9 0.9500 . ? C10 C11 1.374(5) . ? C10 H10 0.9500 . ? C11 C12 1.385(5) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C14 1.519(5) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.524(5) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.527(6) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.526(5) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? 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 N3 Pt1 N1 91.06(10) . . ? N3 Pt1 Cl1 176.44(7) . . ? N1 Pt1 Cl1 88.52(8) . . ? N3 Pt1 Cl2 88.52(7) . . ? N1 Pt1 Cl2 179.05(7) . . ? Cl1 Pt1 Cl2 91.96(3) . . ? O2 S1 O1 121.56(16) . . ? O2 S1 N4 106.23(15) . . ? O1 S1 N4 106.21(15) . . ? O2 S1 N2 105.64(15) . . ? O1 S1 N2 105.54(15) . . ? N4 S1 N2 111.69(15) . . ? C5 N1 C1 119.5(3) . . ? C5 N1 Pt1 122.2(2) . . ? C1 N1 Pt1 118.2(2) . . ? C7 N2 C6 120.1(3) . . ? C7 N2 S1 118.7(2) . . ? C6 N2 S1 118.6(2) . . ? C8 N3 C12 119.8(3) . . ? C8 N3 Pt1 124.1(2) . . ? C12 N3 Pt1 116.0(2) . . ? C13 N4 C17 113.3(3) . . ? C13 N4 S1 118.7(2) . . ? C17 N4 S1 118.6(2) . . ? N1 C1 C2 121.7(3) . . ? N1 C1 H1 119.1 . . ? C2 C1 H1 119.1 . . ? C1 C2 C3 119.0(3) . . ? C1 C2 H2 120.5 . . ? C3 C2 H2 120.5 . . ? C2 C3 C4 118.9(3) . . ? C2 C3 H3 120.6 . . ? C4 C3 H3 120.6 . . ? C5 C4 C3 120.1(3) . . ? C5 C4 H4 120.0 . . ? C3 C4 H4 120.0 . . ? N1 C5 C4 120.7(3) . . ? N1 C5 C6 118.3(3) . . ? C4 C5 C6 121.0(3) . . ? N2 C6 C5 111.9(3) . . ? N2 C6 H6A 109.2 . . ? C5 C6 H6A 109.2 . . ? N2 C6 H6B 109.2 . . ? C5 C6 H6B 109.2 . . ? H6A C6 H6B 107.9 . . ? N2 C7 C8 112.8(2) . . ? N2 C7 H7A 109.0 . . ? C8 C7 H7A 109.0 . . ? N2 C7 H7B 109.0 . . ? C8 C7 H7B 109.0 . . ? H7A C7 H7B 107.8 . . ? N3 C8 C9 120.2(3) . . ? N3 C8 C7 118.0(3) . . ? C9 C8 C7 121.8(3) . . ? C10 C9 C8 120.3(3) . . ? C10 C9 H9 119.8 . . ? C8 C9 H9 119.8 . . ? C11 C10 C9 118.9(3) . . ? C11 C10 H10 120.6 . . ? C9 C10 H10 120.6 . . ? C10 C11 C12 119.2(3) . . ? C10 C11 H11 120.4 . . ? C12 C11 H11 120.4 . . ? N3 C12 C11 121.5(3) . . ? N3 C12 H12 119.2 . . ? C11 C12 H12 119.2 . . ? N4 C13 C14 108.7(3) . . ? N4 C13 H13A 109.9 . . ? C14 C13 H13A 109.9 . . ? N4 C13 H13B 109.9 . . ? C14 C13 H13B 109.9 . . ? H13A C13 H13B 108.3 . . ? C13 C14 C15 111.3(3) . . ? C13 C14 H14A 109.4 . . ? C15 C14 H14A 109.4 . . ? C13 C14 H14B 109.4 . . ? C15 C14 H14B 109.4 . . ? H14A C14 H14B 108.0 . . ? C14 C15 C16 110.1(3) . . ? C14 C15 H15A 109.6 . . ? C16 C15 H15A 109.6 . . ? C14 C15 H15B 109.6 . . ? C16 C15 H15B 109.6 . . ? H15A C15 H15B 108.2 . . ? C17 C16 C15 111.2(3) . . ? C17 C16 H16A 109.4 . . ? C15 C16 H16A 109.4 . . ? C17 C16 H16B 109.4 . . ? C15 C16 H16B 109.4 . . ? H16A C16 H16B 108.0 . . ? N4 C17 C16 108.8(3) . . ? N4 C17 H17A 109.9 . . ? C16 C17 H17A 109.9 . . ? N4 C17 H17B 109.9 . . ? C16 C17 H17B 109.9 . . ? H17A C17 H17B 108.3 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 S1 N2 C7 32.4(3) . . . . ? O1 S1 N2 C7 162.4(2) . . . . ? N4 S1 N2 C7 -82.7(3) . . . . ? O2 S1 N2 C6 -165.9(2) . . . . ? O1 S1 N2 C6 -36.0(3) . . . . ? N4 S1 N2 C6 79.0(2) . . . . ? O2 S1 N4 C13 -42.4(3) . . . . ? O1 S1 N4 C13 -173.2(2) . . . . ? N2 S1 N4 C13 72.3(3) . . . . ? O2 S1 N4 C17 173.3(3) . . . . ? O1 S1 N4 C17 42.6(3) . . . . ? N2 S1 N4 C17 -72.0(3) . . . . ? C5 N1 C1 C2 -2.4(5) . . . . ? Pt1 N1 C1 C2 172.6(3) . . . . ? N1 C1 C2 C3 -0.7(5) . . . . ? C1 C2 C3 C4 2.7(5) . . . . ? C2 C3 C4 C5 -1.8(5) . . . . ? C1 N1 C5 C4 3.4(5) . . . . ? Pt1 N1 C5 C4 -171.5(2) . . . . ? C1 N1 C5 C6 -176.4(3) . . . . ? Pt1 N1 C5 C6 8.8(4) . . . . ? C3 C4 C5 N1 -1.3(5) . . . . ? C3 C4 C5 C6 178.5(3) . . . . ? C7 N2 C6 C5 -103.3(3) . . . . ? S1 N2 C6 C5 95.3(3) . . . . ? N1 C5 C6 N2 76.4(4) . . . . ? C4 C5 C6 N2 -103.3(3) . . . . ? C6 N2 C7 C8 102.1(3) . . . . ? S1 N2 C7 C8 -96.5(3) . . . . ? C12 N3 C8 C9 -1.3(4) . . . . ? Pt1 N3 C8 C9 177.2(2) . . . . ? C12 N3 C8 C7 179.7(3) . . . . ? Pt1 N3 C8 C7 -1.8(4) . . . . ? N2 C7 C8 N3 -79.0(3) . . . . ? N2 C7 C8 C9 102.0(3) . . . . ? N3 C8 C9 C10 0.4(5) . . . . ? C7 C8 C9 C10 179.4(3) . . . . ? C8 C9 C10 C11 0.8(5) . . . . ? C9 C10 C11 C12 -1.2(5) . . . . ? C8 N3 C12 C11 0.9(4) . . . . ? Pt1 N3 C12 C11 -177.7(2) . . . . ? C10 C11 C12 N3 0.4(5) . . . . ? C17 N4 C13 C14 -60.1(4) . . . . ? S1 N4 C13 C14 153.8(2) . . . . ? N4 C13 C14 C15 56.8(4) . . . . ? C13 C14 C15 C16 -55.3(4) . . . . ? C14 C15 C16 C17 54.9(4) . . . . ? C13 N4 C17 C16 59.8(4) . . . . ? S1 N4 C17 C16 -154.1(3) . . . . ? C15 C16 C17 N4 -56.1(4) . . . . ? _refine_diff_density_max 4.711 _refine_diff_density_min -2.794 _refine_diff_density_rms 0.271 _shelx_res_file ; Himali39I2a.res created by SHELXL-2014/7 TITL Himali39I2a in I2/a CELL 0.71073 17.5316 9.5135 24.2020 90.000 91.872 90.000 ZERR 8.00 0.0005 0.0002 0.0009 0.000 0.002 0.000 LATT 2 SYMM -x+1/2, y, -z SFAC C H N O S CL PT UNIT 136 176 32 16 8 16 8 TEMP -183 SIZE 0.040 0.100 0.160 ACTA 50 CONF OMIT -4 0 12 L.S. 15 FMAP 2 PLAN -5 0 0.00 BOND $H CONF WGHT 0.029400 FVAR 0.03962 PT1 7 0.296524 0.516007 0.259993 11.00000 0.00990 0.01001 = 0.00734 0.00102 0.00040 0.00172 CL1 6 0.174016 0.478062 0.226456 11.00000 0.01227 0.01695 = 0.01355 -0.00207 -0.00159 0.00183 CL2 6 0.346295 0.477255 0.174345 11.00000 0.01604 0.01748 = 0.01085 0.00086 0.00277 0.00370 S1 5 0.407298 0.259376 0.430157 11.00000 0.01588 0.01677 = 0.00840 -0.00008 -0.00031 0.00200 O1 4 0.353693 0.301116 0.470404 11.00000 0.02398 0.02706 = 0.01192 -0.00281 0.00305 0.00676 O2 4 0.483992 0.310026 0.432026 11.00000 0.01961 0.02040 = 0.01639 -0.00022 -0.00422 -0.00081 N1 3 0.253669 0.547450 0.336035 11.00000 0.00979 0.01080 = 0.00915 0.00019 0.00176 -0.00012 N2 3 0.370505 0.311199 0.370496 11.00000 0.01375 0.01699 = 0.00835 0.00232 0.00029 0.00351 N3 3 0.402774 0.562193 0.288886 11.00000 0.01170 0.01245 = 0.00865 -0.00121 0.00056 0.00056 N4 3 0.412921 0.088386 0.433841 11.00000 0.01514 0.01781 = 0.01371 0.00251 0.00175 0.00320 C1 1 0.223705 0.675356 0.347381 11.00000 0.01406 0.01305 = 0.01503 -0.00125 -0.00003 0.00210 AFIX 43 H1 2 0.228901 0.749570 0.321512 11.00000 -1.20000 AFIX 0 C2 1 0.185784 0.700493 0.395641 11.00000 0.01749 0.01787 = 0.01383 -0.00211 0.00151 0.00266 AFIX 43 H2 2 0.165654 0.791030 0.403027 11.00000 -1.20000 AFIX 0 C3 1 0.177591 0.591657 0.433057 11.00000 0.01692 0.02314 = 0.01310 -0.00163 0.00262 0.00314 AFIX 43 H3 2 0.149877 0.605274 0.465712 11.00000 -1.20000 AFIX 0 C4 1 0.210530 0.462537 0.422026 11.00000 0.01585 0.01839 = 0.01326 0.00267 0.00336 -0.00051 AFIX 43 H4 2 0.206712 0.387631 0.447746 11.00000 -1.20000 AFIX 0 C5 1 0.248956 0.442721 0.373587 11.00000 0.01169 0.01374 = 0.00974 0.00286 0.00075 0.00110 C6 1 0.286890 0.304281 0.361374 11.00000 0.01433 0.01221 = 0.01195 0.00171 0.00197 0.00130 AFIX 23 H6A 2 0.265937 0.230501 0.385414 11.00000 -1.20000 H6B 2 0.275078 0.277703 0.322481 11.00000 -1.20000 AFIX 0 C7 1 0.420575 0.321602 0.323079 11.00000 0.01484 0.01289 = 0.01193 0.00072 -0.00065 0.00303 AFIX 23 H7A 2 0.392047 0.290426 0.289291 11.00000 -1.20000 H7B 2 0.464528 0.257431 0.329055 11.00000 -1.20000 AFIX 0 C8 1 0.449907 0.468994 0.314235 11.00000 0.01251 0.01472 = 0.01030 -0.00033 -0.00019 0.00165 C9 1 0.523461 0.508438 0.330705 11.00000 0.01238 0.02053 = 0.01741 0.00308 -0.00026 0.00193 AFIX 43 H9 2 0.556594 0.442034 0.348340 11.00000 -1.20000 AFIX 0 C10 1 0.548732 0.644119 0.321540 11.00000 0.01369 0.02319 = 0.01671 -0.00351 0.00121 -0.00247 AFIX 43 H10 2 0.599217 0.671161 0.332318 11.00000 -1.20000 AFIX 0 C11 1 0.499556 0.738943 0.296599 11.00000 0.01619 0.01506 = 0.01611 -0.00217 0.00290 -0.00388 AFIX 43 H11 2 0.515303 0.833077 0.290521 11.00000 -1.20000 AFIX 0 C12 1 0.426753 0.695739 0.280413 11.00000 0.01413 0.01380 = 0.01431 0.00003 0.00318 -0.00173 AFIX 43 H12 2 0.392847 0.761172 0.262978 11.00000 -1.20000 AFIX 0 C13 1 0.470924 0.015461 0.401245 11.00000 0.01699 0.01824 = 0.01311 -0.00094 0.00248 0.00146 AFIX 23 H13A 2 0.517025 0.074927 0.398755 11.00000 -1.20000 H13B 2 0.450449 -0.002575 0.363300 11.00000 -1.20000 AFIX 0 C14 1 0.491327 -0.122691 0.429543 11.00000 0.02189 0.02114 = 0.01493 0.00085 -0.00463 0.00467 AFIX 23 H14A 2 0.515640 -0.103316 0.466249 11.00000 -1.20000 H14B 2 0.528575 -0.174119 0.407243 11.00000 -1.20000 AFIX 0 C15 1 0.420887 -0.213900 0.436648 11.00000 0.03584 0.01559 = 0.01981 0.00055 -0.00574 -0.00262 AFIX 23 H15A 2 0.435181 -0.299994 0.457501 11.00000 -1.20000 H15B 2 0.399751 -0.242492 0.399915 11.00000 -1.20000 AFIX 0 C16 1 0.360599 -0.132594 0.467681 11.00000 0.02215 0.02051 = 0.02068 0.00776 -0.00186 -0.00360 AFIX 23 H16A 2 0.313709 -0.190135 0.469601 11.00000 -1.20000 H16B 2 0.379648 -0.114168 0.505955 11.00000 -1.20000 AFIX 0 C17 1 0.341623 0.006621 0.439116 11.00000 0.01769 0.02216 = 0.02028 0.00492 0.00188 -0.00269 AFIX 23 H17A 2 0.318009 -0.011159 0.402059 11.00000 -1.20000 H17B 2 0.304899 0.060314 0.461070 11.00000 -1.20000 AFIX 0 HKLF 4 1 1 0 0 0 1 0 0 0 1 REM Himali39I2a in I2/a REM R1 = 0.0397 for 8144 Fo > 4sig(Fo) and 0.0704 for all 11296 data REM 244 parameters refined using 0 restraints END WGHT 0.0293 0.0000 REM Highest difference peak 4.711, deepest hole -2.794, 1-sigma level 0.271 Q1 1 0.3005 0.4515 0.2590 11.00000 0.05 4.71 Q2 1 0.3036 0.5814 0.2628 11.00000 0.05 3.15 Q3 1 0.3082 0.5188 0.2366 11.00000 0.05 2.35 Q4 1 0.2832 0.5152 0.2813 11.00000 0.05 2.21 Q5 1 0.1819 0.5554 0.2257 11.00000 0.05 1.41 ; _shelx_res_checksum 79644