#------------------------------------------------------------------------------ #$Date: 2019-10-08 06:43:13 +0300 (Tue, 08 Oct 2019) $ #$Revision: 219152 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/23/44/7234448.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_7234448 loop_ _publ_author_name 'Bellam, Rajesh' 'Jaganyi, Deogratius' 'Mambanda, Allen' 'Robinson, Ross' 'BalaKumaran, Manickam Dakshinamoorthi' _publ_section_title ; Seven membered chelate Pt(ii) complexes with 2,3-di(2-pyridyl)quinoxaline ligands: studies of substitution kinetics by sulfur donor nucleophiles, interactions with CT-DNA, BSA and in vitro cytotoxicity activities ; _journal_issue 55 _journal_name_full 'RSC Advances' _journal_page_first 31877 _journal_paper_doi 10.1039/C9RA06488E _journal_volume 9 _journal_year 2019 _chemical_formula_moiety 'C20 H16 Cl2 N4 Pt, C2 H6 O S' _chemical_formula_sum 'C22 H22 Cl2 N4 O Pt S' _chemical_formula_weight 656.48 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _atom_sites_solution_hydrogens geom _audit_block_doi 10.5517/ccdc.csd.cc20by0b _audit_creation_date 2018-07-19 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _audit_update_record ; 2018-07-23 deposited with the CCDC. 2019-09-18 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 93.454(4) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 9.7436(13) _cell_length_b 13.0705(17) _cell_length_c 17.656(2) _cell_measurement_reflns_used 9996 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 28.60 _cell_measurement_theta_min 2.31 _cell_volume 2244.5(5) _computing_cell_refinement 'COSMO (Bruker, V1.61, 2009)' _computing_data_collection 'COSMO (Bruker, V1.61, 2009)' _computing_data_reduction 'SAINT (Bruker)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'ShelXS-2013 (Sheldrick, 2008)' _diffrn_ambient_temperature 99.99 _diffrn_detector 'Bruker APEX2 area detector' _diffrn_detector_area_resol_mean 7.9 _diffrn_detector_type 'CCD area detector' _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device 'three-circle diffractometer' _diffrn_measurement_device_type 'Bruker SMART APEX2 area detector' _diffrn_measurement_method '\w and \f scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0268 _diffrn_reflns_av_unetI/netI 0.0206 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_number 26005 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.499 _diffrn_reflns_theta_min 1.940 _diffrn_source 'sealed X-ray tube' _diffrn_source_type 'sealed X-ray tube' _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 6.606 _exptl_absorpt_correction_T_max 0.7457 _exptl_absorpt_correction_T_min 0.5894 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Bruker)' _exptl_crystal_colour yellow _exptl_crystal_colour_primary yellow _exptl_crystal_density_diffrn 1.943 _exptl_crystal_description block _exptl_crystal_F_000 1272 _exptl_crystal_recrystallization_method 'The material was recrystallised from DMSO by slow evaporation' _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.12 _refine_diff_density_max 0.421 _refine_diff_density_min -0.339 _refine_diff_density_rms 0.084 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 284 _refine_ls_number_reflns 5153 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.037 _refine_ls_R_factor_all 0.0172 _refine_ls_R_factor_gt 0.0154 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0128P)^2^+1.7517P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0337 _refine_ls_wR_factor_ref 0.0343 _reflns_Friedel_coverage 0.000 _reflns_number_gt 4832 _reflns_number_total 5153 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c9ra06488e2.cif _cod_data_source_block mo_dj_rb_dmpt_dmso_2_0m _cod_database_code 7234448 _shelx_shelxl_version_number 2016/6 _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. ; _shelx_estimated_absorpt_t_max 0.504 _shelx_estimated_absorpt_t_min 0.250 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups At 1.5 times of: All C(H,H,H) groups 2.a Aromatic/amide H refined with riding coordinates: C3(H3), C4(H4), C5(H5), C6(H6), C10(H10), C15(H15), C22(H22), C21(H21), C20(H20), C19(H19) 2.b Idealised Me refined as rotating group: C14(H14A,H14B,H14C), C12(H12A,H12B,H12C), C1(H1A,H1B,H1C), C2(H2A,H2B,H2C) ; _shelx_res_file ; TITL mo_DJ_RB_dmPt_DMSO_2_0m in P2(1)/c mo_dj_rb_dmpt_dmso_2_0m.res created by SHELXL-2016/6 at 18:48:58 on 19-Jul-2018 CELL 0.71073 9.7436 13.0705 17.6559 90 93.454 90 ZERR 4 0.0013 0.0017 0.0024 0 0.004 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H Cl N O Pt S UNIT 88 88 8 16 4 4 4 EQIV $1 -X,1-Y,1-Z EQIV $2 +X,0.5-Y,0.5+Z EQIV $3 -X,-0.5+Y,0.5-Z L.S. 14 PLAN 20 SIZE 0.12 0.22 0.29 TEMP -173.16 HTAB C4 Cl1_$1 HTAB C22 O1_$2 HTAB C19 Cl1_$3 HTAB 2.00000 BOND $H CONF fmap 2 acta MERG 2 OMIT -2 55 REM REM REM WGHT 0.012800 1.751700 FVAR 0.06689 PT1 6 0.188554 0.412890 0.320859 11.00000 0.00764 0.01109 = 0.00766 -0.00046 -0.00092 -0.00086 CL1 3 0.152097 0.579495 0.358142 11.00000 0.01626 0.01305 = 0.01645 -0.00392 -0.00248 -0.00005 CL2 3 0.414439 0.448773 0.300827 11.00000 0.00965 0.02115 = 0.02111 -0.00042 0.00123 -0.00426 S1 7 0.515862 0.195399 0.039300 11.00000 0.01455 0.04406 = 0.01149 0.00474 0.00311 0.00422 N1 4 -0.006977 0.373662 0.342838 11.00000 0.00979 0.01102 = 0.00813 0.00103 0.00069 0.00175 N2 4 -0.162807 0.365254 0.161832 11.00000 0.00875 0.01154 = 0.00940 0.00015 0.00193 -0.00179 N3 4 0.084701 0.290696 0.108400 11.00000 0.00898 0.00945 = 0.00939 -0.00090 0.00134 -0.00048 N4 4 0.221916 0.265629 0.291346 11.00000 0.00772 0.01301 = 0.00978 0.00129 0.00184 0.00084 O1 5 0.470203 0.283904 -0.010674 11.00000 0.02763 0.04087 = 0.01386 0.01071 -0.00384 -0.00863 C3 1 -0.045926 0.386905 0.414784 11.00000 0.01363 0.01308 = 0.00877 -0.00070 -0.00058 0.00244 AFIX 43 H3 2 0.017633 0.416498 0.451384 11.00000 -1.20000 AFIX 0 C4 1 -0.174216 0.359044 0.436773 11.00000 0.01676 0.01571 = 0.00825 0.00126 0.00297 0.00422 AFIX 43 H4 2 -0.198347 0.369584 0.487522 11.00000 -1.20000 AFIX 0 C5 1 -0.267681 0.315329 0.383616 11.00000 0.01265 0.01699 = 0.01553 0.00445 0.00544 0.00316 AFIX 43 H5 2 -0.356044 0.294316 0.397526 11.00000 -1.20000 AFIX 0 C6 1 -0.229047 0.303103 0.309897 11.00000 0.00932 0.01457 = 0.00967 0.00222 -0.00081 0.00079 AFIX 43 H6 2 -0.291617 0.273993 0.272564 11.00000 -1.20000 AFIX 0 C7 1 -0.098624 0.333399 0.290366 11.00000 0.01004 0.00866 = 0.00871 0.00040 0.00014 0.00141 C8 1 -0.064418 0.328642 0.208918 11.00000 0.00955 0.00815 = 0.00857 0.00082 0.00190 -0.00321 C9 1 -0.137383 0.371567 0.086691 11.00000 0.01023 0.00979 = 0.00856 -0.00119 0.00071 -0.00319 C10 1 -0.236793 0.415653 0.034971 11.00000 0.00768 0.01570 = 0.01314 -0.00054 0.00025 -0.00244 AFIX 43 H10 2 -0.324091 0.434206 0.051917 11.00000 -1.20000 AFIX 0 C11 1 -0.209140 0.432070 -0.039354 11.00000 0.01294 0.01327 = 0.01076 -0.00068 -0.00263 -0.00369 C13 1 -0.077563 0.402494 -0.065430 11.00000 0.01372 0.00925 = 0.00795 -0.00112 -0.00032 -0.00474 C15 1 0.017554 0.355848 -0.016258 11.00000 0.01278 0.01044 = 0.01085 -0.00144 0.00380 -0.00081 AFIX 43 H15 2 0.103246 0.334814 -0.034011 11.00000 -1.20000 AFIX 0 C16 1 -0.010156 0.338749 0.060140 11.00000 0.00961 0.00948 = 0.00959 -0.00133 -0.00048 -0.00182 C17 1 0.058587 0.286208 0.181197 11.00000 0.00893 0.00762 = 0.00994 -0.00163 -0.00006 -0.00240 C18 1 0.159020 0.223880 0.228464 11.00000 0.00775 0.01121 = 0.00948 0.00200 0.00413 -0.00102 C22 1 0.314395 0.209519 0.333643 11.00000 0.01058 0.01834 = 0.01398 0.00330 -0.00114 -0.00171 AFIX 43 H22 2 0.357712 0.238817 0.378157 11.00000 -1.20000 AFIX 0 C21 1 0.347710 0.110439 0.313831 11.00000 0.00727 0.01853 = 0.01990 0.00762 0.00075 0.00216 AFIX 43 H21 2 0.412660 0.072377 0.344645 11.00000 -1.20000 AFIX 0 C20 1 0.285630 0.067135 0.248706 11.00000 0.00975 0.01145 = 0.02303 0.00212 0.00618 0.00139 AFIX 43 H20 2 0.308317 -0.000321 0.233799 11.00000 -1.20000 AFIX 0 C19 1 0.189653 0.124554 0.205820 11.00000 0.00923 0.01379 = 0.01273 -0.00032 0.00371 -0.00135 AFIX 43 H19 2 0.145002 0.096397 0.161258 11.00000 -1.20000 AFIX 0 C14 1 -0.046289 0.423491 -0.146542 11.00000 0.01912 0.01554 = 0.00903 0.00035 0.00127 -0.00197 AFIX 137 H14A 2 -0.107112 0.382244 -0.180594 11.00000 -1.50000 H14B 2 0.049657 0.405660 -0.153992 11.00000 -1.50000 H14C 2 -0.061077 0.496223 -0.157780 11.00000 -1.50000 AFIX 0 C12 1 -0.313280 0.483073 -0.093153 11.00000 0.01412 0.02826 = 0.01323 0.00384 -0.00151 -0.00048 AFIX 137 H12A 2 -0.398567 0.494151 -0.067592 11.00000 -1.50000 H12B 2 -0.331997 0.439286 -0.137637 11.00000 -1.50000 H12C 2 -0.277161 0.549029 -0.109300 11.00000 -1.50000 AFIX 0 C1 1 0.503699 0.237401 0.135167 11.00000 0.02229 0.03752 = 0.01324 0.00291 -0.00060 -0.01039 AFIX 137 H1A 2 0.411044 0.263854 0.141695 11.00000 -1.50000 H1B 2 0.571297 0.291623 0.146528 11.00000 -1.50000 H1C 2 0.522097 0.179720 0.169761 11.00000 -1.50000 AFIX 0 C2 1 0.375834 0.106522 0.036140 11.00000 0.03943 0.03110 = 0.01793 -0.00284 0.00205 -0.00591 AFIX 137 H2A 2 0.363176 0.077492 -0.014980 11.00000 -1.50000 H2B 2 0.291618 0.141951 0.048859 11.00000 -1.50000 H2C 2 0.396056 0.051471 0.072812 11.00000 -1.50000 AFIX 0 HKLF 4 REM mo_DJ_RB_dmPt_DMSO_2_0m in P2(1)/c REM R1 = 0.0154 for 4832 Fo > 4sig(Fo) and 0.0172 for all 5153 data REM 284 parameters refined using 0 restraints END WGHT 0.0128 1.7517 REM Instructions for potential hydrogen bonds HTAB C4 Cl1_$1 HTAB C22 O1_$2 HTAB C19 Cl1_$3 REM Highest difference peak 0.421, deepest hole -0.339, 1-sigma level 0.084 Q1 1 -0.2082 0.4383 0.0026 11.00000 0.05 0.42 Q2 1 0.1833 0.2414 0.2617 11.00000 0.05 0.42 Q3 1 -0.0220 0.3965 -0.0332 11.00000 0.05 0.41 Q4 1 -0.1788 0.4023 0.0625 11.00000 0.05 0.40 Q5 1 -0.2253 0.2977 0.3529 11.00000 0.05 0.38 Q6 1 0.0048 0.3286 0.1977 11.00000 0.05 0.38 Q7 1 0.2302 0.1027 0.2319 11.00000 0.05 0.38 Q8 1 -0.0154 0.3397 0.0143 11.00000 0.05 0.37 Q9 1 0.1112 0.2568 0.2077 11.00000 0.05 0.37 Q10 1 -0.0822 0.3295 0.2519 11.00000 0.05 0.37 Q11 1 -0.0629 0.3738 0.0747 11.00000 0.05 0.37 Q12 1 0.2474 0.2269 0.3221 11.00000 0.05 0.36 Q13 1 0.1278 0.4187 0.2759 11.00000 0.05 0.36 Q14 1 -0.1535 0.3034 0.3021 11.00000 0.05 0.36 Q15 1 0.2617 0.4174 0.3569 11.00000 0.05 0.36 Q16 1 0.1545 0.1714 0.2261 11.00000 0.05 0.36 Q17 1 0.1953 0.3589 0.3546 11.00000 0.05 0.36 Q18 1 -0.2528 0.4557 -0.0658 11.00000 0.05 0.36 Q19 1 -0.1512 0.4031 -0.0569 11.00000 0.05 0.35 Q20 1 -0.0314 0.3836 0.3787 11.00000 0.05 0.35 ; _shelx_res_checksum 97747 _olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems' _olex2_exptl_crystal_mounting_method 'The crystal was mounted on a MITIGEN holder in paratone oil' _olex2_submission_original_sample_id dmPt_DMSO_2 _olex2_submission_special_instructions 'No special instructions were received' 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' 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 Pt1 Pt 0.18855(2) 0.41289(2) 0.32086(2) 0.00885(3) Uani 1 1 d . Cl1 Cl 0.15210(6) 0.57950(4) 0.35814(3) 0.01539(11) Uani 1 1 d . Cl2 Cl 0.41444(5) 0.44877(4) 0.30083(3) 0.01729(11) Uani 1 1 d . S1 S 0.51586(6) 0.19540(5) 0.03930(3) 0.02327(14) Uani 1 1 d . N1 N -0.00698(17) 0.37366(13) 0.34284(9) 0.0096(3) Uani 1 1 d . N2 N -0.16281(17) 0.36525(14) 0.16183(9) 0.0098(3) Uani 1 1 d . N3 N 0.08470(17) 0.29070(13) 0.10840(9) 0.0092(3) Uani 1 1 d . N4 N 0.22192(17) 0.26563(13) 0.29135(9) 0.0101(3) Uani 1 1 d . O1 O 0.47020(18) 0.28390(15) -0.01067(9) 0.0277(4) Uani 1 1 d . C3 C -0.0459(2) 0.38690(16) 0.41478(11) 0.0119(4) Uani 1 1 d . H3 H 0.017633 0.416498 0.451384 0.014 Uiso 1 1 calc R C4 C -0.1742(2) 0.35904(17) 0.43677(12) 0.0135(4) Uani 1 1 d . H4 H -0.198347 0.369584 0.487522 0.016 Uiso 1 1 calc R C5 C -0.2677(2) 0.31533(17) 0.38362(12) 0.0149(4) Uani 1 1 d . H5 H -0.356044 0.294316 0.397526 0.018 Uiso 1 1 calc R C6 C -0.2290(2) 0.30310(16) 0.30990(11) 0.0112(4) Uani 1 1 d . H6 H -0.291617 0.273993 0.272564 0.013 Uiso 1 1 calc R C7 C -0.0986(2) 0.33340(15) 0.29037(11) 0.0092(4) Uani 1 1 d . C8 C -0.0644(2) 0.32864(15) 0.20892(11) 0.0087(4) Uani 1 1 d . C9 C -0.1374(2) 0.37157(16) 0.08669(11) 0.0095(4) Uani 1 1 d . C10 C -0.2368(2) 0.41565(16) 0.03497(12) 0.0122(4) Uani 1 1 d . H10 H -0.324091 0.434206 0.051917 0.015 Uiso 1 1 calc R C11 C -0.2091(2) 0.43207(16) -0.03935(12) 0.0125(4) Uani 1 1 d . C13 C -0.0776(2) 0.40249(15) -0.06543(11) 0.0103(4) Uani 1 1 d . C15 C 0.0176(2) 0.35585(16) -0.01626(11) 0.0112(4) Uani 1 1 d . H15 H 0.103246 0.334814 -0.034011 0.013 Uiso 1 1 calc R C16 C -0.0102(2) 0.33875(16) 0.06014(11) 0.0096(4) Uani 1 1 d . C17 C 0.0586(2) 0.28621(15) 0.18120(11) 0.0089(4) Uani 1 1 d . C18 C 0.1590(2) 0.22388(16) 0.22846(11) 0.0093(4) Uani 1 1 d . C22 C 0.3144(2) 0.20952(17) 0.33364(12) 0.0144(4) Uani 1 1 d . H22 H 0.357712 0.238817 0.378157 0.017 Uiso 1 1 calc R C21 C 0.3477(2) 0.11044(17) 0.31383(13) 0.0152(5) Uani 1 1 d . H21 H 0.412660 0.072377 0.344645 0.018 Uiso 1 1 calc R C20 C 0.2856(2) 0.06714(17) 0.24871(13) 0.0145(4) Uani 1 1 d . H20 H 0.308317 -0.000321 0.233799 0.017 Uiso 1 1 calc R C19 C 0.1897(2) 0.12455(17) 0.20582(12) 0.0118(4) Uani 1 1 d . H19 H 0.145002 0.096397 0.161258 0.014 Uiso 1 1 calc R C14 C -0.0463(2) 0.42349(17) -0.14654(12) 0.0145(4) Uani 1 1 d . H14A H -0.107112 0.382244 -0.180594 0.022 Uiso 1 1 calc GR H14B H 0.049657 0.405660 -0.153992 0.022 Uiso 1 1 calc GR H14C H -0.061077 0.496223 -0.157780 0.022 Uiso 1 1 calc GR C12 C -0.3133(2) 0.48307(19) -0.09315(12) 0.0186(5) Uani 1 1 d . H12A H -0.398567 0.494151 -0.067592 0.028 Uiso 1 1 calc GR H12B H -0.331997 0.439286 -0.137637 0.028 Uiso 1 1 calc GR H12C H -0.277161 0.549029 -0.109300 0.028 Uiso 1 1 calc GR C1 C 0.5037(3) 0.2374(2) 0.13517(12) 0.0244(6) Uani 1 1 d . H1A H 0.411044 0.263854 0.141695 0.037 Uiso 1 1 calc GR H1B H 0.571297 0.291623 0.146528 0.037 Uiso 1 1 calc GR H1C H 0.522097 0.179720 0.169761 0.037 Uiso 1 1 calc GR C2 C 0.3758(3) 0.1065(2) 0.03614(14) 0.0295(6) Uani 1 1 d . H2A H 0.363176 0.077492 -0.014980 0.044 Uiso 1 1 calc GR H2B H 0.291618 0.141951 0.048859 0.044 Uiso 1 1 calc GR H2C H 0.396056 0.051471 0.072812 0.044 Uiso 1 1 calc GR loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.00764(4) 0.01109(5) 0.00766(4) -0.00046(3) -0.00092(3) -0.00086(3) Cl1 0.0163(3) 0.0130(3) 0.0165(3) -0.0039(2) -0.0025(2) 0.0000(2) Cl2 0.0097(2) 0.0211(3) 0.0211(3) -0.0004(2) 0.0012(2) -0.0043(2) S1 0.0146(3) 0.0441(4) 0.0115(3) 0.0047(3) 0.0031(2) 0.0042(3) N1 0.0098(9) 0.0110(9) 0.0081(8) 0.0010(7) 0.0007(7) 0.0018(7) N2 0.0087(8) 0.0115(9) 0.0094(8) 0.0001(7) 0.0019(7) -0.0018(7) N3 0.0090(8) 0.0095(8) 0.0094(8) -0.0009(7) 0.0013(7) -0.0005(7) N4 0.0077(8) 0.0130(9) 0.0098(8) 0.0013(7) 0.0018(6) 0.0008(7) O1 0.0276(10) 0.0409(11) 0.0139(8) 0.0107(8) -0.0038(7) -0.0086(8) C3 0.0136(11) 0.0131(10) 0.0088(10) -0.0007(8) -0.0006(8) 0.0024(8) C4 0.0168(11) 0.0157(11) 0.0083(10) 0.0013(8) 0.0030(8) 0.0042(9) C5 0.0126(11) 0.0170(11) 0.0155(11) 0.0045(9) 0.0054(9) 0.0032(9) C6 0.0093(10) 0.0146(11) 0.0097(10) 0.0022(8) -0.0008(8) 0.0008(8) C7 0.0100(10) 0.0087(10) 0.0087(10) 0.0004(8) 0.0001(8) 0.0014(8) C8 0.0095(10) 0.0082(10) 0.0086(9) 0.0008(8) 0.0019(8) -0.0032(8) C9 0.0102(10) 0.0098(10) 0.0086(10) -0.0012(8) 0.0007(8) -0.0032(8) C10 0.0077(10) 0.0157(11) 0.0131(10) -0.0005(8) 0.0003(8) -0.0024(8) C11 0.0129(11) 0.0133(10) 0.0108(10) -0.0007(8) -0.0026(8) -0.0037(8) C13 0.0137(10) 0.0093(10) 0.0080(9) -0.0011(8) -0.0003(8) -0.0047(8) C15 0.0128(10) 0.0104(10) 0.0109(10) -0.0014(8) 0.0038(8) -0.0008(8) C16 0.0096(10) 0.0095(10) 0.0096(10) -0.0013(8) -0.0005(8) -0.0018(8) C17 0.0089(10) 0.0076(10) 0.0099(9) -0.0016(8) -0.0001(8) -0.0024(8) C18 0.0077(10) 0.0112(10) 0.0095(9) 0.0020(8) 0.0041(8) -0.0010(8) C22 0.0106(10) 0.0183(11) 0.0140(10) 0.0033(9) -0.0011(8) -0.0017(9) C21 0.0073(10) 0.0185(11) 0.0199(11) 0.0076(9) 0.0008(8) 0.0022(9) C20 0.0098(10) 0.0114(10) 0.0230(12) 0.0021(9) 0.0062(9) 0.0014(8) C19 0.0092(10) 0.0138(10) 0.0127(10) -0.0003(8) 0.0037(8) -0.0014(8) C14 0.0191(12) 0.0155(11) 0.0090(10) 0.0003(8) 0.0013(8) -0.0020(9) C12 0.0141(11) 0.0283(13) 0.0132(11) 0.0038(10) -0.0015(9) -0.0005(10) C1 0.0223(13) 0.0375(15) 0.0132(11) 0.0029(10) -0.0006(9) -0.0104(11) C2 0.0394(16) 0.0311(15) 0.0179(12) -0.0028(11) 0.0020(11) -0.0059(12) 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' Cl Cl 0.1484 0.1585 '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' Pt Pt -1.7033 8.3905 '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' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle Cl2 Pt1 Cl1 90.95(2) N1 Pt1 Cl1 91.23(5) N1 Pt1 Cl2 176.37(5) N4 Pt1 Cl1 178.33(5) N4 Pt1 Cl2 89.10(5) N4 Pt1 N1 88.64(7) O1 S1 C1 106.52(12) O1 S1 C2 106.41(12) C1 S1 C2 97.74(12) C3 N1 Pt1 117.66(14) C7 N1 Pt1 123.68(13) C7 N1 C3 118.65(18) C8 N2 C9 117.77(18) C17 N3 C16 117.45(17) C18 N4 Pt1 121.57(14) C18 N4 C22 119.30(18) C22 N4 Pt1 119.05(14) N1 C3 H3 118.7 N1 C3 C4 122.56(19) C4 C3 H3 118.7 C3 C4 H4 120.5 C3 C4 C5 119.08(19) C5 C4 H4 120.5 C4 C5 H5 120.7 C6 C5 C4 118.5(2) C6 C5 H5 120.7 C5 C6 H6 119.9 C5 C6 C7 120.2(2) C7 C6 H6 119.9 N1 C7 C6 120.97(18) N1 C7 C8 119.85(18) C6 C7 C8 119.00(18) N2 C8 C7 113.24(17) N2 C8 C17 121.04(18) C17 C8 C7 125.68(18) N2 C9 C10 119.64(18) N2 C9 C16 121.06(18) C10 C9 C16 119.24(18) C9 C10 H10 119.5 C11 C10 C9 121.0(2) C11 C10 H10 119.5 C10 C11 C13 119.56(19) C10 C11 C12 120.6(2) C13 C11 C12 119.79(19) C11 C13 C14 119.30(19) C15 C13 C11 119.77(19) C15 C13 C14 120.93(19) C13 C15 H15 119.5 C13 C15 C16 120.95(19) C16 C15 H15 119.5 N3 C16 C9 120.21(18) N3 C16 C15 120.44(18) C15 C16 C9 119.35(19) N3 C17 C8 121.80(18) N3 C17 C18 114.15(17) C8 C17 C18 123.70(17) N4 C18 C17 119.33(18) N4 C18 C19 121.13(19) C19 C18 C17 119.52(18) N4 C22 H22 119.1 N4 C22 C21 121.8(2) C21 C22 H22 119.1 C22 C21 H21 120.2 C22 C21 C20 119.6(2) C20 C21 H21 120.2 C21 C20 H20 120.7 C21 C20 C19 118.5(2) C19 C20 H20 120.7 C18 C19 H19 120.2 C20 C19 C18 119.7(2) C20 C19 H19 120.2 C13 C14 H14A 109.5 C13 C14 H14B 109.5 C13 C14 H14C 109.5 H14A C14 H14B 109.5 H14A C14 H14C 109.5 H14B C14 H14C 109.5 C11 C12 H12A 109.5 C11 C12 H12B 109.5 C11 C12 H12C 109.5 H12A C12 H12B 109.5 H12A C12 H12C 109.5 H12B C12 H12C 109.5 S1 C1 H1A 109.5 S1 C1 H1B 109.5 S1 C1 H1C 109.5 H1A C1 H1B 109.5 H1A C1 H1C 109.5 H1B C1 H1C 109.5 S1 C2 H2A 109.5 S1 C2 H2B 109.5 S1 C2 H2C 109.5 H2A C2 H2B 109.5 H2A C2 H2C 109.5 H2B C2 H2C 109.5 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Pt1 Cl1 2.3086(6) Pt1 Cl2 2.2985(6) Pt1 N1 2.0328(17) Pt1 N4 2.0254(18) S1 O1 1.5058(18) S1 C1 1.790(2) S1 C2 1.790(3) N1 C3 1.359(3) N1 C7 1.354(3) N2 C8 1.320(3) N2 C9 1.367(3) N3 C16 1.371(3) N3 C17 1.326(3) N4 C18 1.351(3) N4 C22 1.351(3) C3 H3 0.9500 C3 C4 1.380(3) C4 H4 0.9500 C4 C5 1.391(3) C5 H5 0.9500 C5 C6 1.386(3) C6 H6 0.9500 C6 C7 1.394(3) C7 C8 1.497(3) C8 C17 1.433(3) C9 C10 1.413(3) C9 C16 1.418(3) C10 H10 0.9500 C10 C11 1.372(3) C11 C13 1.441(3) C11 C12 1.503(3) C13 C15 1.374(3) C13 C14 1.507(3) C15 H15 0.9500 C15 C16 1.409(3) C17 C18 1.490(3) C18 C19 1.396(3) C22 H22 0.9500 C22 C21 1.385(3) C21 H21 0.9500 C21 C20 1.387(3) C20 H20 0.9500 C20 C19 1.388(3) C19 H19 0.9500 C14 H14A 0.9800 C14 H14B 0.9800 C14 H14C 0.9800 C12 H12A 0.9800 C12 H12B 0.9800 C12 H12C 0.9800 C1 H1A 0.9800 C1 H1B 0.9800 C1 H1C 0.9800 C2 H2A 0.9800 C2 H2B 0.9800 C2 H2C 0.9800 loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C4 H4 Cl1 0.95 2.81 3.703(2) 155.9 3_566 C22 H22 O1 0.95 2.21 3.060(3) 148.5 4_566 C19 H19 Cl1 0.95 2.90 3.501(2) 122.1 2_545 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 Pt1 N1 C3 C4 -177.32(16) Pt1 N1 C7 C6 176.64(15) Pt1 N1 C7 C8 -8.2(3) Pt1 N4 C18 C17 -2.4(2) Pt1 N4 C18 C19 175.64(14) Pt1 N4 C22 C21 -176.11(16) N1 C3 C4 C5 0.2(3) N1 C7 C8 N2 -130.5(2) N1 C7 C8 C17 51.7(3) N2 C8 C17 N3 6.6(3) N2 C8 C17 C18 -166.25(19) N2 C9 C10 C11 173.68(19) N2 C9 C16 N3 6.4(3) N2 C9 C16 C15 -173.69(18) N3 C17 C18 N4 126.59(19) N3 C17 C18 C19 -51.5(3) N4 C18 C19 C20 0.4(3) N4 C22 C21 C20 0.4(3) C3 N1 C7 C6 -1.9(3) C3 N1 C7 C8 173.22(18) C3 C4 C5 C6 -1.2(3) C4 C5 C6 C7 0.6(3) C5 C6 C7 N1 1.0(3) C5 C6 C7 C8 -174.20(19) C6 C7 C8 N2 44.7(3) C6 C7 C8 C17 -133.1(2) C7 N1 C3 C4 1.3(3) C7 C8 C17 N3 -175.78(18) C7 C8 C17 C18 11.4(3) C8 N2 C9 C10 -176.42(19) C8 N2 C9 C16 0.7(3) C8 C17 C18 N4 -60.1(3) C8 C17 C18 C19 121.8(2) C9 N2 C8 C7 175.11(17) C9 N2 C8 C17 -7.0(3) C9 C10 C11 C13 1.0(3) C9 C10 C11 C12 -177.4(2) C10 C9 C16 N3 -176.41(18) C10 C9 C16 C15 3.5(3) C10 C11 C13 C15 1.6(3) C10 C11 C13 C14 -178.25(19) C11 C13 C15 C16 -1.7(3) C13 C15 C16 N3 178.98(19) C13 C15 C16 C9 -0.9(3) C16 N3 C17 C8 0.7(3) C16 N3 C17 C18 174.13(17) C16 C9 C10 C11 -3.5(3) C17 N3 C16 C9 -6.8(3) C17 N3 C16 C15 173.29(18) C17 C18 C19 C20 178.44(18) C18 N4 C22 C21 0.7(3) C22 N4 C18 C17 -179.11(18) C22 N4 C18 C19 -1.1(3) C22 C21 C20 C19 -1.0(3) C21 C20 C19 C18 0.6(3) C14 C13 C15 C16 178.23(19) C12 C11 C13 C15 -180.0(2) C12 C11 C13 C14 0.1(3)