# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2012 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_ic13562 _database_code_depnum_ccdc_archive 'CCDC 859737' #TrackingRef '2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C63 H83 Cl4 N10 O3.50 Pt2 S4 Zn2' _chemical_formula_weight 1827.35 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' Zn Zn 0.2839 1.4301 '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' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M I-42d loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'y, -x, -z' '-y, x, -z' '-x+1/2, y, -z+3/4' 'x+1/2, -y, -z+3/4' '-y+1/2, -x, z+3/4' 'y+1/2, x, z+3/4' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-y+1/2, x+1/2, -z+1/2' '-x+1, y+1/2, -z+5/4' 'x+1, -y+1/2, -z+5/4' '-y+1, -x+1/2, z+5/4' 'y+1, x+1/2, z+5/4' _cell_length_a 25.4025(2) _cell_length_b 25.4025(2) _cell_length_c 46.8244(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 30215.2(4) _cell_formula_units_Z 16 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used all _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.50 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.27 _exptl_crystal_density_meas not_measured _exptl_crystal_density_diffrn 1.607 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 14512 _exptl_absorpt_coefficient_mu 4.620 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.198 _exptl_absorpt_correction_T_max 0.296 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'NONIUS KappaCCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 47615 _diffrn_reflns_av_R_equivalents 0.0503 _diffrn_reflns_av_sigmaI/netI 0.0651 _diffrn_reflns_limit_h_min -33 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -60 _diffrn_reflns_limit_l_max 60 _diffrn_reflns_theta_min 1.43 _diffrn_reflns_theta_max 27.50 _reflns_number_total 16959 _reflns_number_gt 13350 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'NONIUS KappaCCD' _computing_cell_refinement DENZO-SMN _computing_data_reduction DENZO-SMN _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0717P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.011(5) _refine_ls_number_reflns 16959 _refine_ls_number_parameters 772 _refine_ls_number_restraints 11 _refine_ls_R_factor_all 0.0655 _refine_ls_R_factor_gt 0.0446 _refine_ls_wR_factor_ref 0.1247 _refine_ls_wR_factor_gt 0.1157 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.059 _refine_ls_shift/su_max 0.011 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.212179(12) 0.500821(13) -0.094456(7) 0.03444(9) Uani 1 1 d . . . Pt2 Pt 0.025244(12) 0.707977(12) 0.097136(7) 0.02949(8) Uani 1 1 d . . . Zn1 Zn -0.03480(4) 0.66356(4) -0.06127(2) 0.0344(2) Uani 1 1 d . . . Zn2 Zn 0.16318(4) 0.44878(4) 0.06432(2) 0.0362(2) Uani 1 1 d . . . Cl1 Cl -0.06484(9) 0.73439(10) -0.08449(5) 0.0458(6) Uani 1 1 d . . . Cl2 Cl -0.08712(9) 0.59550(11) -0.05332(5) 0.0504(6) Uani 1 1 d . . . Cl3 Cl 0.08886(10) 0.40531(9) 0.05557(5) 0.0470(6) Uani 1 1 d . . . Cl4 Cl 0.22931(9) 0.41229(9) 0.08954(5) 0.0436(5) Uani 1 1 d . . . S1 S 0.19398(9) 0.58514(9) -0.10896(6) 0.0431(6) Uani 1 1 d . . . S2 S 0.06878(9) 0.74767(9) 0.06014(5) 0.0377(5) Uani 1 1 d . . . S3 S 0.26041(9) 0.53488(9) -0.05770(5) 0.0436(6) Uani 1 1 d . . . S4 S 0.10543(8) 0.68278(8) 0.11478(5) 0.0344(5) Uani 1 1 d . . . N1 N 0.0301(3) 0.6362(3) -0.08145(15) 0.0362(16) Uani 1 1 d . . . N2 N -0.0020(3) 0.6885(3) -0.02303(14) 0.0345(16) Uani 1 1 d . . . N3 N 0.1930(3) 0.4730(3) 0.02579(15) 0.0388(17) Uani 1 1 d . . . N4 N 0.1433(3) 0.5173(3) 0.08387(15) 0.0338(16) Uani 1 1 d . . . N5 N 0.2281(3) 0.4224(3) -0.08502(14) 0.0324(16) Uani 1 1 d . . . N6 N 0.1654(3) 0.4636(3) -0.12387(14) 0.0343(16) Uani 1 1 d . . . N7 N -0.0192(3) 0.6663(3) 0.12546(14) 0.0300(15) Uani 1 1 d . . . N8 N -0.0499(3) 0.7296(3) 0.08496(14) 0.0294(15) Uani 1 1 d . . . C1 C 0.0465(3) 0.5874(4) -0.07726(18) 0.039(2) Uani 1 1 d . . . H1 H 0.0232 0.5643 -0.0675 0.047 Uiso 1 1 calc R . . C2 C 0.0952(4) 0.5666(3) -0.08585(18) 0.039(2) Uani 1 1 d . . . H2 H 0.1042 0.5308 -0.0826 0.047 Uiso 1 1 calc R . . C3 C 0.1291(3) 0.6006(3) -0.09908(19) 0.036(2) Uani 1 1 d . . . C4 C 0.1111(4) 0.6532(4) -0.1054(2) 0.044(2) Uani 1 1 d . . . H4 H 0.1328 0.6771 -0.1156 0.052 Uiso 1 1 calc R . . C5 C 0.0637(3) 0.6674(3) -0.09663(19) 0.038(2) Uani 1 1 d . . . H5 H 0.0522 0.7020 -0.1013 0.046 Uiso 1 1 calc R . . C6 C 0.0327(3) 0.7267(3) -0.0224(2) 0.039(2) Uani 1 1 d . . . H6 H 0.0434 0.7422 -0.0399 0.046 Uiso 1 1 calc R . . C7 C 0.0548(3) 0.7454(4) 0.00293(19) 0.037(2) Uani 1 1 d . . . H7 H 0.0793 0.7736 0.0024 0.045 Uiso 1 1 calc R . . C8 C 0.0409(3) 0.7228(3) 0.02925(18) 0.0344(19) Uani 1 1 d . . . C9 C 0.0046(4) 0.6813(3) 0.02773(18) 0.0361(19) Uani 1 1 d . . . H9 H -0.0061 0.6640 0.0448 0.043 Uiso 1 1 calc R . . C10 C -0.0157(3) 0.6651(3) 0.00221(17) 0.0334(19) Uani 1 1 d . . . H10 H -0.0400 0.6368 0.0020 0.040 Uiso 1 1 calc R . . C11 C 0.2363(4) 0.5029(4) 0.0244(2) 0.043(2) Uani 1 1 d . . . H11 H 0.2527 0.5125 0.0419 0.051 Uiso 1 1 calc R . . C12 C 0.2587(4) 0.5205(4) -0.0004(2) 0.052(3) Uani 1 1 d . . . H12 H 0.2904 0.5402 0.0001 0.062 Uiso 1 1 calc R . . C13 C 0.2345(3) 0.5094(3) -0.0263(2) 0.038(2) Uani 1 1 d . . . C14 C 0.1882(4) 0.4794(4) -0.0238(2) 0.043(2) Uani 1 1 d . . . H14 H 0.1693 0.4709 -0.0407 0.052 Uiso 1 1 calc R . . C15 C 0.1689(4) 0.4620(3) 0.00166(19) 0.040(2) Uani 1 1 d . . . H15 H 0.1375 0.4416 0.0020 0.048 Uiso 1 1 calc R . . C16 C 0.1756(3) 0.5452(3) 0.09993(17) 0.0294(18) Uani 1 1 d . . . H16 H 0.2085 0.5299 0.1047 0.035 Uiso 1 1 calc R . . C17 C 0.1652(3) 0.5950(3) 0.11035(17) 0.0296(18) Uani 1 1 d . . . H17 H 0.1899 0.6127 0.1222 0.036 Uiso 1 1 calc R . . C18 C 0.1164(3) 0.6193(3) 0.10282(16) 0.0303(18) Uani 1 1 d . . . C19 C 0.0820(3) 0.5892(3) 0.08640(18) 0.036(2) Uani 1 1 d . . . H19 H 0.0491 0.6038 0.0809 0.043 Uiso 1 1 calc R . . C20 C 0.0944(3) 0.5393(3) 0.07798(19) 0.039(2) Uani 1 1 d . . . H20 H 0.0690 0.5192 0.0678 0.046 Uiso 1 1 calc R . . C21 C 0.2655(3) 0.4039(4) -0.06734(18) 0.036(2) Uani 1 1 d . . . H21 H 0.2880 0.4284 -0.0581 0.044 Uiso 1 1 calc R . . C22 C 0.2725(3) 0.3528(3) -0.06227(18) 0.0345(19) Uani 1 1 d . . . H22 H 0.2998 0.3415 -0.0499 0.041 Uiso 1 1 calc R . . C23 C 0.2391(3) 0.3155(3) -0.07539(17) 0.035(2) Uani 1 1 d . . . C24 C 0.2012(3) 0.3332(3) -0.09353(16) 0.0327(18) Uani 1 1 d . . . H24 H 0.1783 0.3090 -0.1028 0.039 Uiso 1 1 calc R . . C25 C 0.1960(3) 0.3879(3) -0.09853(17) 0.0317(18) Uani 1 1 d . . . C26 C 0.1589(3) 0.4108(3) -0.11859(16) 0.0300(18) Uani 1 1 d . . . C27 C 0.1213(3) 0.3824(4) -0.13344(17) 0.038(2) Uani 1 1 d . . . H27 H 0.1180 0.3457 -0.1301 0.046 Uiso 1 1 calc R . . C28 C 0.0880(3) 0.4068(3) -0.15332(18) 0.037(2) Uani 1 1 d . . . C29 C 0.0984(4) 0.4590(4) -0.15953(18) 0.045(2) Uani 1 1 d . . . H29 H 0.0794 0.4764 -0.1742 0.054 Uiso 1 1 calc R . . C30 C 0.1365(4) 0.4858(3) -0.14420(17) 0.040(2) Uani 1 1 d . . . H30 H 0.1423 0.5219 -0.1485 0.048 Uiso 1 1 calc R . . C31 C 0.2470(4) 0.2570(3) -0.06942(18) 0.036(2) Uani 1 1 d . . . C32 C 0.2356(4) 0.2465(4) -0.0380(2) 0.045(2) Uani 1 1 d . . . H32A H 0.1985 0.2542 -0.0340 0.068 Uiso 1 1 calc R . . H32B H 0.2579 0.2691 -0.0262 0.068 Uiso 1 1 calc R . . H32C H 0.2429 0.2095 -0.0336 0.068 Uiso 1 1 calc R . . C33 C 0.3043(4) 0.2425(4) -0.0752(2) 0.049(2) Uani 1 1 d . . . H33A H 0.3272 0.2628 -0.0624 0.073 Uiso 1 1 calc R . . H33B H 0.3131 0.2507 -0.0951 0.073 Uiso 1 1 calc R . . H33C H 0.3094 0.2048 -0.0717 0.073 Uiso 1 1 calc R . . C34 C 0.2117(4) 0.2215(3) -0.08741(18) 0.042(2) Uani 1 1 d . . . H34A H 0.2185 0.1846 -0.0825 0.062 Uiso 1 1 calc R . . H34B H 0.2193 0.2272 -0.1077 0.062 Uiso 1 1 calc R . . H34C H 0.1747 0.2299 -0.0836 0.062 Uiso 1 1 calc R . . C35 C 0.0434(4) 0.3784(4) -0.16806(19) 0.045(2) Uani 1 1 d . . . C36 C 0.0369(4) 0.3210(4) -0.1580(2) 0.058(3) Uani 1 1 d . . . H36A H 0.0675 0.3003 -0.1640 0.087 Uiso 1 1 calc R . . H36B H 0.0049 0.3060 -0.1664 0.087 Uiso 1 1 calc R . . H36C H 0.0342 0.3202 -0.1371 0.087 Uiso 1 1 calc R . . C37 C 0.0514(5) 0.3787(4) -0.2010(2) 0.063(3) Uani 1 1 d . . . H37A H 0.0468 0.4146 -0.2083 0.094 Uiso 1 1 calc R . . H37B H 0.0255 0.3554 -0.2100 0.094 Uiso 1 1 calc R . . H37C H 0.0870 0.3663 -0.2056 0.094 Uiso 1 1 calc R . . C38 C -0.0089(4) 0.4061(5) -0.1602(2) 0.058(3) Uani 1 1 d . . . H38A H -0.0108 0.4107 -0.1394 0.087 Uiso 1 1 calc R . . H38B H -0.0386 0.3846 -0.1667 0.087 Uiso 1 1 calc R . . H38C H -0.0103 0.4406 -0.1695 0.087 Uiso 1 1 calc R . . C39 C -0.0016(4) 0.6356(3) 0.14653(16) 0.0360(19) Uani 1 1 d . . . H39 H 0.0346 0.6383 0.1515 0.043 Uiso 1 1 calc R . . C40 C -0.0313(4) 0.6011(3) 0.16127(17) 0.039(2) Uani 1 1 d . . . H40 H -0.0162 0.5802 0.1760 0.047 Uiso 1 1 calc R . . C41 C -0.0848(3) 0.5965(3) 0.15459(18) 0.0328(18) Uani 1 1 d . . . C42 C -0.1049(3) 0.6289(3) 0.13300(16) 0.0320(18) Uani 1 1 d . . . H42 H -0.1409 0.6266 0.1277 0.038 Uiso 1 1 calc R . . C43 C -0.0715(3) 0.6649(3) 0.11929(17) 0.0295(18) Uani 1 1 d . . . C44 C -0.0889(3) 0.7013(3) 0.09733(16) 0.0279(17) Uani 1 1 d . . . C45 C -0.1407(3) 0.7104(3) 0.08994(16) 0.0329(18) Uani 1 1 d . . . H45 H -0.1677 0.6905 0.0989 0.039 Uiso 1 1 calc R . . C46 C -0.1541(3) 0.7483(3) 0.06961(18) 0.037(2) Uani 1 1 d . . . C47 C -0.1127(3) 0.7772(3) 0.05837(17) 0.0345(19) Uani 1 1 d . . . H47 H -0.1196 0.8041 0.0448 0.041 Uiso 1 1 calc R . . C48 C -0.0620(3) 0.7673(3) 0.06669(17) 0.0308(18) Uani 1 1 d . . . H48 H -0.0345 0.7883 0.0590 0.037 Uiso 1 1 calc R . . C49 C -0.1183(4) 0.5541(4) 0.16935(19) 0.042(2) Uani 1 1 d . . . C50 C -0.0943(4) 0.4991(4) 0.1621(2) 0.054(3) Uani 1 1 d . . . H50A H -0.1129 0.4718 0.1729 0.080 Uiso 1 1 calc R . . H50B H -0.0569 0.4987 0.1672 0.080 Uiso 1 1 calc R . . H50C H -0.0980 0.4923 0.1416 0.080 Uiso 1 1 calc R . . C51 C -0.1153(5) 0.5629(4) 0.20194(18) 0.053(3) Uani 1 1 d . . . H51A H -0.1298 0.5975 0.2067 0.079 Uiso 1 1 calc R . . H51B H -0.0785 0.5610 0.2082 0.079 Uiso 1 1 calc R . . H51C H -0.1357 0.5355 0.2117 0.079 Uiso 1 1 calc R . . C52 C -0.1760(4) 0.5551(4) 0.15977(19) 0.045(2) Uani 1 1 d . . . H52A H -0.1956 0.5275 0.1698 0.068 Uiso 1 1 calc R . . H52B H -0.1779 0.5490 0.1391 0.068 Uiso 1 1 calc R . . H52C H -0.1914 0.5895 0.1642 0.068 Uiso 1 1 calc R . . C53 C -0.2110(4) 0.7540(4) 0.05927(18) 0.044(2) Uani 1 1 d . . . C54 C -0.2486(4) 0.7531(5) 0.0851(2) 0.078(4) Uani 1 1 d . . . H54A H -0.2397 0.7820 0.0981 0.117 Uiso 1 1 calc R . . H54B H -0.2451 0.7195 0.0952 0.117 Uiso 1 1 calc R . . H54C H -0.2850 0.7574 0.0785 0.117 Uiso 1 1 calc R . . C55 C -0.2189(4) 0.8038(4) 0.0426(2) 0.063(3) Uani 1 1 d . . . H55A H -0.1965 0.8032 0.0256 0.094 Uiso 1 1 calc R . . H55B H -0.2096 0.8341 0.0545 0.094 Uiso 1 1 calc R . . H55C H -0.2559 0.8065 0.0368 0.094 Uiso 1 1 calc R . . C56 C -0.2238(4) 0.7059(4) 0.0406(2) 0.058(3) Uani 1 1 d . . . H56A H -0.2580 0.7110 0.0314 0.086 Uiso 1 1 calc R . . H56B H -0.2250 0.6743 0.0526 0.086 Uiso 1 1 calc R . . H56C H -0.1965 0.7017 0.0260 0.086 Uiso 1 1 calc R . . O1 O 0.0316(4) 0.5831(5) 0.2208(2) 0.109(4) Uani 1 1 d D . . N9 N 0.1224(4) 0.5844(3) 0.22559(19) 0.059(2) Uani 1 1 d D . . C57 C 0.0729(4) 0.5650(5) 0.2333(3) 0.080(4) Uani 1 1 d D . . H57 H 0.0698 0.5388 0.2477 0.097 Uiso 1 1 calc R . . C58 C 0.1279(5) 0.6281(4) 0.2055(3) 0.078(4) Uani 1 1 d D . . H58A H 0.1442 0.6154 0.1878 0.116 Uiso 1 1 calc R . . H58B H 0.1501 0.6555 0.2140 0.116 Uiso 1 1 calc R . . H58C H 0.0931 0.6426 0.2012 0.116 Uiso 1 1 calc R . . C59 C 0.1680(5) 0.5621(6) 0.2358(3) 0.093(4) Uiso 1 1 d D . . H59A H 0.1599 0.5404 0.2525 0.140 Uiso 1 1 calc R . . H59B H 0.1928 0.5899 0.2413 0.140 Uiso 1 1 calc R . . H59C H 0.1839 0.5401 0.2209 0.140 Uiso 1 1 calc R . . O2 O 0.2166(6) 0.6480(6) -0.2589(3) 0.176(6) Uiso 1 1 d D . . N10 N 0.3159(6) 0.6336(6) -0.2469(3) 0.129(5) Uiso 1 1 d D . . C60 C 0.2605(7) 0.6462(8) -0.2419(4) 0.150 Uiso 1 1 d D . . H60 H 0.2533 0.6551 -0.2226 0.180 Uiso 1 1 calc R . . C61 C 0.3441(8) 0.6212(8) -0.2744(4) 0.155(8) Uiso 1 1 d D . . H61A H 0.3599 0.6534 -0.2821 0.232 Uiso 1 1 calc R . . H61B H 0.3190 0.6068 -0.2883 0.232 Uiso 1 1 calc R . . H61C H 0.3718 0.5952 -0.2708 0.232 Uiso 1 1 calc R . . C62 C 0.3531(7) 0.6269(8) -0.2258(4) 0.137(7) Uiso 1 1 d D . . H62A H 0.3724 0.6599 -0.2230 0.205 Uiso 1 1 calc R . . H62B H 0.3777 0.5990 -0.2314 0.205 Uiso 1 1 calc R . . H62C H 0.3355 0.6170 -0.2079 0.205 Uiso 1 1 calc R . . O3 O 0.1007(11) 0.6511(10) -0.2247(5) 0.138(9) Uiso 0.50 1 d PD A 1 H3 H 0.1271 0.6357 -0.2315 0.207 Uiso 0.50 1 d PR A 1 C63 C 0.1367(14) 0.6404(17) -0.2027(7) 0.150 Uiso 0.50 1 d PD A 1 H63A H 0.1723 0.6427 -0.1948 0.225 Uiso 0.50 1 d PR A 1 H63B H 0.1221 0.6054 -0.1988 0.225 Uiso 0.50 1 d PR A 1 H63C H 0.1143 0.6672 -0.1939 0.225 Uiso 0.50 1 d PR A 1 O3' O 0.0793(9) 0.5366(9) -0.2212(5) 0.119(7) Uiso 0.50 1 d PD B 2 H3' H 0.0625 0.5355 -0.2058 0.178 Uiso 0.50 1 d PR B 2 C63' C 0.0840(17) 0.5888(11) -0.2302(8) 0.150 Uiso 0.50 1 d PD B 2 H63D H 0.0766 0.6145 -0.2152 0.225 Uiso 0.50 1 d PR B 2 H63E H 0.0552 0.5889 -0.2442 0.225 Uiso 0.50 1 d PR B 2 H63F H 0.1170 0.5981 -0.2398 0.225 Uiso 0.50 1 d PR B 2 O4 O 0.0000 0.5000 0.0015(4) 0.192(9) Uiso 1 2 d S . . H4A H -0.0255 0.5090 0.0129 0.288 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.03477(16) 0.03184(16) 0.03670(18) -0.00287(16) 0.00909(15) -0.00529(16) Pt2 0.03035(16) 0.02805(16) 0.03009(16) -0.00439(14) -0.00344(14) 0.00085(14) Zn1 0.0296(5) 0.0458(6) 0.0277(5) 0.0063(4) 0.0008(4) -0.0008(4) Zn2 0.0469(6) 0.0277(5) 0.0341(5) -0.0037(4) -0.0031(5) 0.0002(4) Cl1 0.0421(12) 0.0529(13) 0.0425(13) 0.0135(11) -0.0015(10) 0.0077(11) Cl2 0.0410(12) 0.0678(16) 0.0423(13) 0.0128(12) -0.0047(11) -0.0193(12) Cl3 0.0585(14) 0.0387(12) 0.0437(13) 0.0028(10) -0.0126(12) -0.0134(11) Cl4 0.0470(12) 0.0412(12) 0.0424(13) -0.0050(10) -0.0067(10) 0.0075(10) S1 0.0390(12) 0.0337(11) 0.0567(15) 0.0044(11) 0.0196(11) -0.0023(10) S2 0.0374(12) 0.0399(12) 0.0359(12) -0.0016(10) -0.0019(10) -0.0110(10) S3 0.0419(13) 0.0421(13) 0.0467(14) -0.0095(11) 0.0107(11) -0.0158(11) S4 0.0305(10) 0.0309(10) 0.0420(13) -0.0102(10) -0.0069(10) 0.0004(9) N1 0.037(4) 0.034(4) 0.038(4) 0.009(3) 0.006(3) 0.004(3) N2 0.027(3) 0.039(4) 0.037(4) 0.001(3) -0.002(3) 0.009(4) N3 0.050(4) 0.034(4) 0.032(4) 0.003(3) -0.001(3) -0.005(4) N4 0.032(4) 0.027(4) 0.042(4) -0.003(3) -0.005(3) 0.000(3) N5 0.040(4) 0.028(3) 0.030(4) -0.008(3) 0.012(3) -0.006(3) N6 0.035(4) 0.044(4) 0.023(3) -0.001(3) 0.008(3) -0.003(4) N7 0.029(3) 0.029(3) 0.032(4) -0.007(3) -0.003(3) 0.007(3) N8 0.038(4) 0.026(3) 0.023(3) -0.004(3) -0.002(3) -0.002(3) C1 0.028(4) 0.049(5) 0.041(5) 0.009(4) 0.006(4) -0.010(4) C2 0.047(5) 0.031(4) 0.039(5) 0.004(4) 0.003(4) -0.003(4) C3 0.037(4) 0.037(4) 0.033(5) 0.000(4) 0.006(4) -0.011(4) C4 0.045(5) 0.038(5) 0.049(6) 0.009(4) 0.012(5) -0.007(4) C5 0.042(5) 0.035(4) 0.038(5) 0.008(4) 0.008(4) 0.002(4) C6 0.033(5) 0.041(5) 0.042(5) 0.006(4) 0.011(4) -0.011(4) C7 0.031(4) 0.040(5) 0.041(5) 0.004(4) 0.007(4) -0.008(4) C8 0.029(4) 0.031(4) 0.043(5) 0.002(4) 0.006(4) 0.000(3) C9 0.039(5) 0.039(4) 0.030(4) 0.001(4) -0.007(4) -0.007(4) C10 0.031(4) 0.045(5) 0.025(4) -0.003(4) 0.008(3) -0.006(4) C11 0.047(5) 0.043(5) 0.038(5) -0.002(5) -0.008(4) -0.009(5) C12 0.048(6) 0.040(5) 0.067(7) 0.011(5) -0.019(5) -0.020(5) C13 0.036(4) 0.029(5) 0.048(5) -0.009(4) 0.003(4) -0.005(4) C14 0.047(5) 0.040(5) 0.043(5) -0.011(4) 0.000(4) -0.006(4) C15 0.047(5) 0.036(5) 0.038(5) -0.012(4) 0.004(4) -0.008(4) C16 0.032(4) 0.027(4) 0.029(4) 0.006(3) 0.001(4) 0.002(3) C17 0.029(4) 0.031(4) 0.029(4) 0.004(4) 0.002(3) -0.006(4) C18 0.028(4) 0.035(4) 0.028(5) 0.000(4) 0.008(3) -0.007(3) C19 0.031(4) 0.036(5) 0.041(5) -0.004(4) -0.006(4) -0.001(4) C20 0.035(5) 0.032(5) 0.049(5) -0.013(4) -0.006(4) 0.002(4) C21 0.036(5) 0.042(5) 0.031(5) -0.003(4) -0.001(4) -0.007(4) C22 0.032(4) 0.038(5) 0.034(5) -0.007(4) 0.001(4) 0.001(4) C23 0.040(5) 0.038(5) 0.027(4) -0.007(4) 0.006(4) -0.003(4) C24 0.031(4) 0.040(4) 0.026(4) -0.006(4) 0.008(4) 0.000(4) C25 0.034(4) 0.037(4) 0.024(4) -0.011(4) 0.010(4) -0.004(4) C26 0.036(4) 0.035(4) 0.019(4) -0.006(3) 0.007(4) 0.000(4) C27 0.042(5) 0.042(5) 0.031(5) -0.005(4) 0.008(4) -0.002(4) C28 0.044(5) 0.043(5) 0.023(4) 0.006(4) -0.002(4) 0.009(4) C29 0.051(6) 0.056(6) 0.027(5) -0.004(4) 0.000(4) -0.004(5) C30 0.046(5) 0.040(5) 0.034(5) -0.001(4) 0.012(4) -0.005(4) C31 0.043(5) 0.037(5) 0.029(4) -0.007(4) 0.002(4) 0.002(4) C32 0.051(6) 0.043(5) 0.043(5) 0.003(4) 0.004(5) 0.003(5) C33 0.054(6) 0.037(5) 0.056(6) -0.016(5) 0.010(5) 0.000(4) C34 0.047(5) 0.037(5) 0.041(5) -0.009(4) 0.003(4) -0.006(4) C35 0.049(6) 0.056(6) 0.030(5) 0.004(4) -0.004(4) -0.009(5) C36 0.062(7) 0.057(6) 0.054(6) -0.015(5) -0.020(5) -0.025(6) C37 0.084(8) 0.057(7) 0.048(6) -0.010(5) -0.011(6) -0.002(6) C38 0.050(6) 0.076(7) 0.049(6) -0.007(5) -0.010(5) -0.001(5) C39 0.036(4) 0.045(5) 0.027(4) 0.004(4) -0.005(4) 0.013(4) C40 0.047(5) 0.040(5) 0.030(5) -0.002(4) -0.007(4) 0.014(4) C41 0.033(4) 0.035(4) 0.030(4) -0.007(4) -0.002(4) 0.006(4) C42 0.036(4) 0.033(4) 0.027(4) 0.003(4) 0.001(4) 0.001(4) C43 0.037(4) 0.026(4) 0.026(4) -0.009(3) -0.003(4) 0.010(4) C44 0.033(4) 0.030(4) 0.021(4) -0.004(3) -0.005(4) 0.001(3) C45 0.025(4) 0.045(5) 0.028(4) 0.010(4) -0.004(3) 0.002(4) C46 0.040(5) 0.040(5) 0.033(5) -0.009(4) -0.009(4) 0.013(4) C47 0.041(5) 0.031(4) 0.031(4) 0.003(4) -0.010(4) -0.001(4) C48 0.038(5) 0.021(4) 0.032(5) -0.001(4) -0.002(4) 0.002(4) C49 0.051(6) 0.042(5) 0.034(5) 0.010(4) -0.003(4) 0.008(5) C50 0.070(6) 0.041(5) 0.051(6) 0.012(5) 0.003(5) 0.006(6) C51 0.073(7) 0.060(6) 0.025(5) 0.012(5) -0.002(5) 0.016(6) C52 0.047(5) 0.046(5) 0.043(6) 0.011(5) 0.003(5) -0.004(5) C53 0.044(5) 0.051(5) 0.036(5) 0.015(4) -0.010(4) -0.003(5) C54 0.047(6) 0.116(11) 0.070(8) 0.030(7) 0.019(6) 0.023(7) C55 0.058(7) 0.072(7) 0.058(6) 0.000(6) -0.016(5) 0.015(6) C56 0.057(6) 0.062(6) 0.053(6) 0.005(6) -0.016(5) 0.004(6) O1 0.079(7) 0.158(11) 0.090(7) -0.001(7) 0.011(6) 0.039(7) N9 0.078(7) 0.036(4) 0.064(6) -0.003(4) 0.019(5) 0.011(4) C57 0.069(8) 0.077(9) 0.095(10) -0.039(8) 0.032(8) -0.009(7) C58 0.093(9) 0.034(6) 0.105(10) 0.007(6) -0.009(8) -0.004(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 N6 2.051(7) . ? Pt1 N5 2.079(7) . ? Pt1 S3 2.283(2) . ? Pt1 S1 2.294(2) . ? Pt2 N7 2.038(7) . ? Pt2 N8 2.066(7) . ? Pt2 S4 2.289(2) . ? Pt2 S2 2.289(2) . ? Zn1 N1 2.023(7) . ? Zn1 N2 2.074(7) . ? Zn1 Cl2 2.212(3) . ? Zn1 Cl1 2.236(2) . ? Zn2 N4 2.030(7) . ? Zn2 N3 2.051(7) . ? Zn2 Cl3 2.225(3) . ? Zn2 Cl4 2.253(2) . ? S1 C3 1.755(9) . ? S2 C8 1.730(9) . ? S3 C13 1.734(10) . ? S4 C18 1.730(8) . ? N1 C1 1.323(11) . ? N1 C5 1.366(11) . ? N2 C6 1.311(11) . ? N2 C10 1.368(10) . ? N3 C15 1.315(11) . ? N3 C11 1.339(12) . ? N4 C16 1.319(10) . ? N4 C20 1.391(11) . ? N5 C21 1.346(11) . ? N5 C25 1.354(11) . ? N6 C30 1.328(11) . ? N6 C26 1.373(10) . ? N7 C39 1.334(10) . ? N7 C43 1.360(10) . ? N8 C48 1.319(10) . ? N8 C44 1.356(10) . ? C1 C2 1.405(12) . ? C2 C3 1.368(12) . ? C3 C4 1.442(12) . ? C4 C5 1.322(12) . ? C6 C7 1.395(13) . ? C7 C8 1.405(12) . ? C8 C9 1.403(12) . ? C9 C10 1.364(11) . ? C11 C12 1.368(14) . ? C12 C13 1.392(13) . ? C13 C14 1.407(13) . ? C14 C15 1.362(13) . ? C16 C17 1.382(11) . ? C17 C18 1.429(11) . ? C18 C19 1.392(11) . ? C19 C20 1.363(12) . ? C21 C22 1.331(12) . ? C22 C23 1.411(11) . ? C23 C24 1.361(12) . ? C23 C31 1.527(12) . ? C24 C25 1.414(12) . ? C25 C26 1.454(12) . ? C26 C27 1.385(12) . ? C27 C28 1.402(12) . ? C28 C29 1.384(12) . ? C28 C35 1.509(13) . ? C29 C30 1.385(12) . ? C31 C32 1.522(12) . ? C31 C33 1.524(12) . ? C31 C34 1.526(12) . ? C35 C38 1.546(14) . ? C35 C36 1.543(14) . ? C35 C37 1.558(13) . ? C39 C40 1.348(12) . ? C40 C41 1.398(12) . ? C41 C42 1.401(11) . ? C41 C49 1.535(13) . ? C42 C43 1.404(12) . ? C43 C44 1.450(11) . ? C44 C45 1.380(10) . ? C45 C46 1.395(11) . ? C46 C47 1.387(12) . ? C46 C53 1.533(12) . ? C47 C48 1.369(12) . ? C49 C52 1.534(13) . ? C49 C51 1.544(12) . ? C49 C50 1.562(13) . ? C53 C55 1.500(13) . ? C53 C56 1.536(13) . ? C53 C54 1.542(13) . ? O1 C57 1.287(8) . ? N9 C59 1.375(14) . ? N9 C57 1.399(13) . ? N9 C58 1.461(12) . ? O2 C60 1.369(15) . ? N10 C62 1.379(16) . ? N10 C60 1.463(16) . ? N10 C61 1.506(16) . ? O3 C63 1.401(10) . ? O3' C63' 1.397(10) . ? 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 N6 Pt1 N5 79.3(3) . . ? N6 Pt1 S3 172.9(2) . . ? N5 Pt1 S3 95.6(2) . . ? N6 Pt1 S1 96.6(2) . . ? N5 Pt1 S1 175.01(19) . . ? S3 Pt1 S1 88.71(9) . . ? N7 Pt2 N8 78.9(3) . . ? N7 Pt2 S4 96.45(19) . . ? N8 Pt2 S4 174.71(19) . . ? N7 Pt2 S2 171.41(19) . . ? N8 Pt2 S2 96.88(19) . . ? S4 Pt2 S2 88.08(8) . . ? N1 Zn1 N2 100.4(3) . . ? N1 Zn1 Cl2 107.4(2) . . ? N2 Zn1 Cl2 109.6(2) . . ? N1 Zn1 Cl1 109.1(2) . . ? N2 Zn1 Cl1 108.1(2) . . ? Cl2 Zn1 Cl1 120.37(10) . . ? N4 Zn2 N3 103.4(3) . . ? N4 Zn2 Cl3 107.3(2) . . ? N3 Zn2 Cl3 107.4(2) . . ? N4 Zn2 Cl4 107.5(2) . . ? N3 Zn2 Cl4 108.0(2) . . ? Cl3 Zn2 Cl4 121.67(9) . . ? C3 S1 Pt1 108.7(3) . . ? C8 S2 Pt2 105.9(3) . . ? C13 S3 Pt1 107.0(3) . . ? C18 S4 Pt2 106.7(3) . . ? C1 N1 C5 115.2(7) . . ? C1 N1 Zn1 120.6(6) . . ? C5 N1 Zn1 123.6(6) . . ? C6 N2 C10 118.2(7) . . ? C6 N2 Zn1 121.1(6) . . ? C10 N2 Zn1 120.8(6) . . ? C15 N3 C11 117.5(8) . . ? C15 N3 Zn2 121.4(6) . . ? C11 N3 Zn2 121.0(6) . . ? C16 N4 C20 116.8(7) . . ? C16 N4 Zn2 124.3(5) . . ? C20 N4 Zn2 118.6(5) . . ? C21 N5 C25 119.0(7) . . ? C21 N5 Pt1 127.1(6) . . ? C25 N5 Pt1 113.9(6) . . ? C30 N6 C26 118.6(7) . . ? C30 N6 Pt1 127.3(6) . . ? C26 N6 Pt1 113.5(5) . . ? C39 N7 C43 118.0(8) . . ? C39 N7 Pt2 126.8(6) . . ? C43 N7 Pt2 114.5(5) . . ? C48 N8 C44 119.5(7) . . ? C48 N8 Pt2 126.0(6) . . ? C44 N8 Pt2 114.5(5) . . ? N1 C1 C2 126.0(8) . . ? C3 C2 C1 116.6(8) . . ? C2 C3 C4 118.5(8) . . ? C2 C3 S1 124.7(7) . . ? C4 C3 S1 116.9(6) . . ? C5 C4 C3 118.7(8) . . ? C4 C5 N1 124.8(8) . . ? N2 C6 C7 122.8(8) . . ? C6 C7 C8 120.4(8) . . ? C9 C8 C7 115.3(8) . . ? C9 C8 S2 125.9(7) . . ? C7 C8 S2 118.7(6) . . ? C10 C9 C8 121.2(8) . . ? C9 C10 N2 122.1(8) . . ? N3 C11 C12 124.5(9) . . ? C11 C12 C13 119.6(8) . . ? C12 C13 C14 113.8(9) . . ? C12 C13 S3 119.8(7) . . ? C14 C13 S3 126.3(7) . . ? C15 C14 C13 123.5(9) . . ? N3 C15 C14 121.0(9) . . ? N4 C16 C17 125.2(7) . . ? C16 C17 C18 118.2(7) . . ? C19 C18 C17 116.4(7) . . ? C19 C18 S4 126.1(7) . . ? C17 C18 S4 117.5(6) . . ? C20 C19 C18 121.7(8) . . ? C19 C20 N4 121.6(8) . . ? C22 C21 N5 123.0(8) . . ? C21 C22 C23 119.8(8) . . ? C24 C23 C22 118.4(8) . . ? C24 C23 C31 121.9(8) . . ? C22 C23 C31 119.7(8) . . ? C23 C24 C25 119.5(8) . . ? N5 C25 C24 120.3(8) . . ? N5 C25 C26 115.6(7) . . ? C24 C25 C26 124.1(7) . . ? N6 C26 C27 120.1(8) . . ? N6 C26 C25 115.5(7) . . ? C27 C26 C25 124.3(8) . . ? C26 C27 C28 121.3(8) . . ? C29 C28 C27 116.6(8) . . ? C29 C28 C35 120.3(8) . . ? C27 C28 C35 123.1(8) . . ? C28 C29 C30 119.8(9) . . ? N6 C30 C29 123.2(8) . . ? C32 C31 C33 108.1(8) . . ? C32 C31 C34 108.5(7) . . ? C33 C31 C34 108.8(7) . . ? C32 C31 C23 108.8(7) . . ? C33 C31 C23 109.1(8) . . ? C34 C31 C23 113.4(7) . . ? C28 C35 C38 108.6(8) . . ? C28 C35 C36 113.0(8) . . ? C38 C35 C36 105.4(8) . . ? C28 C35 C37 110.7(8) . . ? C38 C35 C37 110.3(8) . . ? C36 C35 C37 108.8(8) . . ? N7 C39 C40 124.8(8) . . ? C39 C40 C41 119.0(8) . . ? C40 C41 C42 117.8(8) . . ? C40 C41 C49 119.7(8) . . ? C42 C41 C49 122.4(7) . . ? C41 C42 C43 119.5(8) . . ? N7 C43 C42 120.7(7) . . ? N7 C43 C44 115.6(7) . . ? C42 C43 C44 123.7(7) . . ? N8 C44 C45 120.0(7) . . ? N8 C44 C43 114.7(7) . . ? C45 C44 C43 125.1(7) . . ? C44 C45 C46 121.3(8) . . ? C47 C46 C45 116.0(8) . . ? C47 C46 C53 123.0(8) . . ? C45 C46 C53 120.8(8) . . ? C48 C47 C46 120.5(8) . . ? N8 C48 C47 122.5(8) . . ? C52 C49 C41 112.7(7) . . ? C52 C49 C51 109.5(8) . . ? C41 C49 C51 108.5(8) . . ? C52 C49 C50 108.9(8) . . ? C41 C49 C50 108.2(7) . . ? C51 C49 C50 109.0(7) . . ? C55 C53 C46 111.8(8) . . ? C55 C53 C56 110.3(8) . . ? C46 C53 C56 107.6(8) . . ? C55 C53 C54 109.8(9) . . ? C46 C53 C54 109.6(8) . . ? C56 C53 C54 107.7(9) . . ? C59 N9 C57 121.5(10) . . ? C59 N9 C58 117.2(10) . . ? C57 N9 C58 121.3(10) . . ? O1 C57 N9 119.2(12) . . ? C62 N10 C60 124.8(15) . . ? C62 N10 C61 105.2(14) . . ? C60 N10 C61 129.8(15) . . ? O2 C60 N10 134.2(18) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.683 _refine_diff_density_min -0.876 _refine_diff_density_rms 0.156 data_bct-3 _database_code_depnum_ccdc_archive 'CCDC 859738' #TrackingRef '3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C64 H83.50 Br4 Cl N10.50 O3 Pt2 S4 Zn2' _chemical_formula_weight 2052.16 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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 '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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M I-42d loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'y, -x, -z' '-y, x, -z' '-x+1/2, y, -z+3/4' 'x+1/2, -y, -z+3/4' '-y+1/2, -x, z+3/4' 'y+1/2, x, z+3/4' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-y+1/2, x+1/2, -z+1/2' '-x+1, y+1/2, -z+5/4' 'x+1, -y+1/2, -z+5/4' '-y+1, -x+1/2, z+5/4' 'y+1, x+1/2, z+5/4' _cell_length_a 25.6733(10) _cell_length_b 25.6733(10) _cell_length_c 47.043(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 31007(3) _cell_formula_units_Z 16 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 95741 _cell_measurement_theta_min 1.42 _cell_measurement_theta_max 27.50 _exptl_crystal_description octahedron _exptl_crystal_colour yellow _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.758 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 16032 _exptl_absorpt_coefficient_mu 6.461 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3306 _exptl_absorpt_correction_T_max 0.4649 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART ApexCCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 95741 _diffrn_reflns_av_R_equivalents 0.0893 _diffrn_reflns_av_sigmaI/netI 0.0618 _diffrn_reflns_limit_h_min -33 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 60 _diffrn_reflns_theta_min 1.42 _diffrn_reflns_theta_max 27.50 _reflns_number_total 17751 _reflns_number_gt 14658 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0690P)^2^+135.0941P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.467(7) _refine_ls_number_reflns 17751 _refine_ls_number_parameters 828 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0639 _refine_ls_R_factor_gt 0.0452 _refine_ls_wR_factor_ref 0.1267 _refine_ls_wR_factor_gt 0.1117 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.052 _refine_ls_shift/su_max 0.012 _refine_ls_shift/su_mean 0.001 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.000536(14) 0.286930(13) 1.094351(8) 0.02781(9) Uani 1 1 d . . . Pt2 Pt 0.209481(13) 0.472628(13) 0.903097(7) 0.02015(8) Uani 1 1 d . . . Zn1 Zn -0.04658(4) 0.33477(5) 0.93607(2) 0.0288(2) Uani 1 1 d . . . Zn2 Zn 0.16367(4) 0.52965(4) 1.06054(2) 0.0252(2) Uani 1 1 d . . . Br1 Br 0.23843(4) 0.56177(4) 1.08411(2) 0.0348(2) Uani 1 1 d . . . Br2 Br 0.09309(5) 0.58605(4) 1.05243(2) 0.0410(3) Uani 1 1 d . . . Br3 Br -0.09231(4) 0.41317(5) 0.94479(2) 0.0390(3) Uani 1 1 d . . . Br4 Br -0.08631(4) 0.26730(4) 0.90905(2) 0.0357(2) Uani 1 1 d . . . S1 S 0.24991(10) 0.42976(10) 0.93960(5) 0.0290(5) Uani 1 1 d . . . S2 S 0.08404(10) 0.30505(10) 1.10879(7) 0.0389(6) Uani 1 1 d . . . S3 S 0.18472(9) 0.39306(9) 0.88561(5) 0.0253(5) Uani 1 1 d . . . S4 S 0.03447(11) 0.23766(11) 1.05824(6) 0.0397(6) Uani 1 1 d . . . N1 N -0.0241(3) 0.3044(3) 0.97448(18) 0.0335(19) Uani 1 1 d . . . N2 N 0.0217(3) 0.3552(3) 0.91745(18) 0.0336(19) Uani 1 1 d . . . N3 N 0.1362(3) 0.4662(3) 1.08111(16) 0.0297(18) Uani 1 1 d . . . N4 N 0.1888(3) 0.4972(3) 1.02292(16) 0.0242(16) Uani 1 1 d . . . N5 N -0.0356(3) 0.3343(3) 1.12321(17) 0.0310(19) Uani 1 1 d . . . N6 N -0.0760(3) 0.2717(3) 1.08524(17) 0.0271(17) Uani 1 1 d . . . N7 N 0.2306(3) 0.5473(3) 0.91509(16) 0.0224(16) Uani 1 1 d . . . N8 N 0.1677(3) 0.5162(3) 0.87466(16) 0.0250(17) Uani 1 1 d . . . C1 C -0.0344(4) 0.3284(4) 0.9990(2) 0.035(2) Uani 1 1 d . . . H1 H -0.0543 0.3596 0.9986 0.042 Uiso 1 1 calc R . . C2 C -0.0173(4) 0.3100(4) 1.0250(2) 0.034(2) Uani 1 1 d . . . H2 H -0.0250 0.3288 1.0419 0.041 Uiso 1 1 calc R . . C3 C 0.0108(3) 0.2642(4) 1.0265(2) 0.028(2) Uani 1 1 d . . . C4 C 0.0220(4) 0.2386(4) 1.0012(3) 0.041(3) Uani 1 1 d . . . H4 H 0.0410 0.2068 1.0012 0.049 Uiso 1 1 calc R . . C5 C 0.0048(4) 0.2603(4) 0.9759(2) 0.040(3) Uani 1 1 d . . . H5 H 0.0137 0.2434 0.9586 0.048 Uiso 1 1 calc R . . C6 C 0.0486(4) 0.3232(4) 0.89998(19) 0.027(2) Uani 1 1 d . . . H6 H 0.0328 0.2913 0.8944 0.032 Uiso 1 1 calc R . . C7 C 0.0979(4) 0.3343(3) 0.88977(19) 0.026(2) Uani 1 1 d . . . H7 H 0.1151 0.3104 0.8775 0.031 Uiso 1 1 calc R . . C8 C 0.1225(3) 0.3815(3) 0.89764(19) 0.0232(19) Uani 1 1 d . . . C9 C 0.0929(4) 0.4154(4) 0.9145(2) 0.039(3) Uani 1 1 d . . . H9 H 0.1073 0.4479 0.9202 0.047 Uiso 1 1 calc R . . C10 C 0.0431(4) 0.4023(4) 0.9231(2) 0.037(3) Uani 1 1 d . . . H10 H 0.0231 0.4272 0.9333 0.045 Uiso 1 1 calc R . . C11 C 0.1666(4) 0.4337(4) 1.0960(2) 0.032(2) Uani 1 1 d . . . H11 H 0.2009 0.4447 1.1005 0.038 Uiso 1 1 calc R . . C12 C 0.1506(4) 0.3854(4) 1.1049(2) 0.033(2) Uani 1 1 d . . . H12 H 0.1739 0.3638 1.1153 0.040 Uiso 1 1 calc R . . C13 C 0.1007(4) 0.3682(4) 1.0989(2) 0.034(2) Uani 1 1 d . . . C14 C 0.0674(4) 0.4032(4) 1.0851(2) 0.034(2) Uani 1 1 d . . . H14 H 0.0320 0.3944 1.0817 0.041 Uiso 1 1 calc R . . C15 C 0.0869(4) 0.4507(4) 1.0764(2) 0.032(2) Uani 1 1 d . . . H15 H 0.0643 0.4737 1.0666 0.038 Uiso 1 1 calc R . . C16 C 0.2279(4) 0.4624(4) 1.0219(2) 0.032(2) Uani 1 1 d . . . H16 H 0.2434 0.4518 1.0393 0.039 Uiso 1 1 calc R . . C17 C 0.2465(4) 0.4414(4) 0.9971(2) 0.033(2) Uani 1 1 d . . . H17 H 0.2743 0.4171 0.9977 0.040 Uiso 1 1 calc R . . C18 C 0.2249(4) 0.4555(3) 0.9708(2) 0.026(2) Uani 1 1 d . . . C19 C 0.1835(3) 0.4913(4) 0.97195(19) 0.0257(19) Uani 1 1 d . . . H19 H 0.1666 0.5020 0.9550 0.031 Uiso 1 1 calc R . . C20 C 0.1675(3) 0.5109(3) 0.9982(2) 0.0251(19) Uani 1 1 d . . . H20 H 0.1398 0.5354 0.9984 0.030 Uiso 1 1 calc R . . C21 C -0.0130(4) 0.3631(4) 1.1437(2) 0.036(2) Uani 1 1 d . . . H21 H 0.0228 0.3573 1.1478 0.044 Uiso 1 1 calc R . . C22 C -0.0394(4) 0.4006(4) 1.1589(2) 0.037(2) Uani 1 1 d . . . H22 H -0.0219 0.4199 1.1733 0.045 Uiso 1 1 calc R . . C23 C -0.0925(4) 0.4103(4) 1.1531(2) 0.031(2) Uani 1 1 d . . . C24 C -0.1169(4) 0.3777(4) 1.1332(2) 0.029(2) Uani 1 1 d . . . H24 H -0.1531 0.3814 1.1296 0.035 Uiso 1 1 calc R . . C25 C -0.0883(4) 0.3402(4) 1.1188(2) 0.027(2) Uani 1 1 d . . . C26 C -0.1112(4) 0.3028(3) 1.0983(2) 0.0255(19) Uani 1 1 d . . . C27 C -0.1643(3) 0.2988(4) 1.0938(2) 0.0271(19) Uani 1 1 d . . . H27 H -0.1875 0.3219 1.1032 0.033 Uiso 1 1 calc R . . C28 C -0.1837(4) 0.2606(4) 1.07521(19) 0.028(2) Uani 1 1 d . . . C29 C -0.1474(4) 0.2290(4) 1.0619(2) 0.031(2) Uani 1 1 d . . . H29 H -0.1587 0.2028 1.0491 0.037 Uiso 1 1 calc R . . C30 C -0.0951(4) 0.2353(4) 1.0672(2) 0.030(2) Uani 1 1 d . . . H30 H -0.0712 0.2130 1.0577 0.035 Uiso 1 1 calc R . . C31 C -0.1201(4) 0.4550(4) 1.1681(2) 0.040(3) Uani 1 1 d . . . C32 C -0.0924(6) 0.5064(5) 1.1599(3) 0.056(3) Uani 1 1 d . . . H32A H -0.0582 0.5078 1.1691 0.084 Uiso 1 1 calc R . . H32B H -0.1135 0.5361 1.1662 0.084 Uiso 1 1 calc R . . H32C H -0.0880 0.5079 1.1393 0.084 Uiso 1 1 calc R . . C33 C -0.1190(5) 0.4455(6) 1.2005(2) 0.059(4) Uani 1 1 d . . . H33A H -0.1393 0.4142 1.2050 0.088 Uiso 1 1 calc R . . H33B H -0.1342 0.4755 1.2103 0.088 Uiso 1 1 calc R . . H33C H -0.0830 0.4406 1.2068 0.088 Uiso 1 1 calc R . . C34 C -0.1783(5) 0.4584(5) 1.1587(3) 0.055(3) Uani 1 1 d . . . H34A H -0.1802 0.4695 1.1388 0.083 Uiso 1 1 calc R . . H34B H -0.1966 0.4837 1.1707 0.083 Uiso 1 1 calc R . . H34C H -0.1947 0.4241 1.1608 0.083 Uiso 1 1 calc R . . C35 C -0.2423(4) 0.2545(4) 1.0693(2) 0.028(2) Uani 1 1 d . . . C36 C -0.2762(4) 0.2898(4) 1.0875(2) 0.037(2) Uani 1 1 d . . . H36A H -0.2675 0.3263 1.0835 0.056 Uiso 1 1 calc R . . H36B H -0.2700 0.2823 1.1076 0.056 Uiso 1 1 calc R . . H36C H -0.3130 0.2836 1.0830 0.056 Uiso 1 1 calc R . . C37 C -0.2571(4) 0.1969(4) 1.0752(3) 0.045(3) Uani 1 1 d . . . H37A H -0.2936 0.1912 1.0701 0.067 Uiso 1 1 calc R . . H37B H -0.2522 0.1893 1.0955 0.067 Uiso 1 1 calc R . . H37C H -0.2348 0.1739 1.0639 0.067 Uiso 1 1 calc R . . C38 C -0.2523(4) 0.2666(5) 1.0382(2) 0.041(3) Uani 1 1 d . . . H38A H -0.2886 0.2585 1.0336 0.062 Uiso 1 1 calc R . . H38B H -0.2291 0.2454 1.0264 0.062 Uiso 1 1 calc R . . H38C H -0.2457 0.3036 1.0347 0.062 Uiso 1 1 calc R . . C39 C 0.2666(4) 0.5592(4) 0.9336(2) 0.029(2) Uani 1 1 d . . . H39 H 0.2867 0.5320 0.9418 0.035 Uiso 1 1 calc R . . C40 C 0.2764(3) 0.6100(4) 0.9417(2) 0.029(2) Uani 1 1 d . . . H40 H 0.3033 0.6171 0.9550 0.034 Uiso 1 1 calc R . . C41 C 0.2474(4) 0.6505(4) 0.9306(2) 0.030(2) Uani 1 1 d . . . C42 C 0.2106(4) 0.6369(4) 0.91024(19) 0.0269(19) Uani 1 1 d . . . H42 H 0.1902 0.6633 0.9015 0.032 Uiso 1 1 calc R . . C43 C 0.2034(3) 0.5860(4) 0.90267(18) 0.0227(18) Uani 1 1 d . . . C44 C 0.1658(3) 0.5681(4) 0.88055(19) 0.0237(19) Uani 1 1 d . . . C45 C 0.1301(3) 0.6008(4) 0.86670(19) 0.026(2) Uani 1 1 d . . . H45 H 0.1277 0.6365 0.8719 0.031 Uiso 1 1 calc R . . C46 C 0.0983(4) 0.5812(4) 0.8453(2) 0.028(2) Uani 1 1 d . . . C47 C 0.1029(4) 0.5283(4) 0.83888(19) 0.029(2) Uani 1 1 d . . . H47 H 0.0823 0.5132 0.8243 0.035 Uiso 1 1 calc R . . C48 C 0.1379(4) 0.4984(4) 0.85393(18) 0.0277(19) Uani 1 1 d . . . H48 H 0.1408 0.4626 0.8491 0.033 Uiso 1 1 calc R . . C49 C 0.2529(4) 0.7072(4) 0.9408(2) 0.039(3) Uani 1 1 d . . . C50 C 0.2063(5) 0.7190(5) 0.9601(3) 0.053(3) Uani 1 1 d . . . H50A H 0.2057 0.7562 0.9645 0.079 Uiso 1 1 calc R . . H50B H 0.2095 0.6989 0.9777 0.079 Uiso 1 1 calc R . . H50C H 0.1741 0.7093 0.9503 0.079 Uiso 1 1 calc R . . C51 C 0.3022(5) 0.7152(5) 0.9587(3) 0.055(3) Uani 1 1 d . . . H51A H 0.3036 0.7512 0.9655 0.083 Uiso 1 1 calc R . . H51B H 0.3330 0.7079 0.9470 0.083 Uiso 1 1 calc R . . H51C H 0.3017 0.6914 0.9750 0.083 Uiso 1 1 calc R . . C52 C 0.2533(6) 0.7449(4) 0.9162(3) 0.068(4) Uani 1 1 d . . . H52A H 0.2200 0.7428 0.9061 0.102 Uiso 1 1 calc R . . H52B H 0.2818 0.7359 0.9032 0.102 Uiso 1 1 calc R . . H52C H 0.2584 0.7803 0.9234 0.102 Uiso 1 1 calc R . . C53 C 0.0568(4) 0.6134(5) 0.8302(2) 0.036(2) Uani 1 1 d . . . C54 C 0.0591(4) 0.6717(4) 0.8389(2) 0.042(3) Uani 1 1 d . . . H54A H 0.0939 0.6855 0.8350 0.063 Uiso 1 1 calc R . . H54B H 0.0515 0.6750 0.8592 0.063 Uiso 1 1 calc R . . H54C H 0.0332 0.6914 0.8279 0.063 Uiso 1 1 calc R . . C55 C 0.0649(4) 0.6090(5) 0.7986(2) 0.047(3) Uani 1 1 d . . . H55A H 0.0998 0.6214 0.7937 0.070 Uiso 1 1 calc R . . H55B H 0.0388 0.6301 0.7887 0.070 Uiso 1 1 calc R . . H55C H 0.0613 0.5725 0.7928 0.070 Uiso 1 1 calc R . . C56 C 0.0019(4) 0.5920(5) 0.8385(3) 0.050(3) Uani 1 1 d . . . H56A H -0.0251 0.6132 0.8294 0.075 Uiso 1 1 calc R . . H56B H -0.0022 0.5935 0.8592 0.075 Uiso 1 1 calc R . . H56C H -0.0013 0.5558 0.8321 0.075 Uiso 1 1 calc R . . O1 O 0.0851(5) 0.4664(4) 0.77969(19) 0.071(3) Uani 1 1 d . . . N9 N 0.0822(4) 0.3782(4) 0.7750(2) 0.040(2) Uani 1 1 d . . . C57 C 0.0661(5) 0.4259(5) 0.7700(2) 0.049(3) Uani 1 1 d . . . H57 H 0.0370 0.4297 0.7578 0.059 Uiso 1 1 calc R . . C58 C 0.0562(5) 0.3343(5) 0.7632(3) 0.060(4) Uani 1 1 d . . . H58A H 0.0306 0.3210 0.7768 0.090 Uiso 1 1 calc R . . H58B H 0.0817 0.3069 0.7589 0.090 Uiso 1 1 calc R . . H58C H 0.0384 0.3446 0.7456 0.090 Uiso 1 1 calc R . . C59 C 0.1244(5) 0.3693(6) 0.7951(3) 0.060(4) Uani 1 1 d . . . H59A H 0.1417 0.4024 0.7993 0.089 Uiso 1 1 calc R . . H59B H 0.1497 0.3450 0.7868 0.089 Uiso 1 1 calc R . . H59C H 0.1103 0.3544 0.8126 0.089 Uiso 1 1 calc R . . O2 O 0.1479(5) 0.2172(8) 0.9905(3) 0.129(7) Uani 1 1 d . . . N10 N 0.1346(5) 0.3118(6) 1.0052(3) 0.076(4) Uani 1 1 d . . . C60 C 0.1447(6) 0.2525(10) 1.0085(6) 0.118(9) Uani 1 1 d . . . H60 H 0.1493 0.2412 1.0276 0.142 Uiso 1 1 calc R . . C61 C 0.1330(6) 0.3435(6) 1.0288(3) 0.075(5) Uani 1 1 d . . . H61A H 0.1360 0.3221 1.0460 0.113 Uiso 1 1 calc R . . H61B H 0.0999 0.3624 1.0292 0.113 Uiso 1 1 calc R . . H61C H 0.1619 0.3683 1.0281 0.113 Uiso 1 1 calc R . . C62 C 0.1255(7) 0.3341(7) 0.9772(3) 0.081(5) Uani 1 1 d . . . H62A H 0.0998 0.3622 0.9787 0.122 Uiso 1 1 calc R . . H62B H 0.1123 0.3070 0.9644 0.122 Uiso 1 1 calc R . . H62C H 0.1582 0.3481 0.9697 0.122 Uiso 1 1 calc R . . O3 O 0.0320(9) 0.0778(9) 1.0276(5) 0.088(7) Uiso 0.50 1 d PD A 1 N11 N 0.1243(9) 0.1041(10) 1.0313(5) 0.080(8) Uiso 0.50 1 d PD A 1 C64 C 0.1351(11) 0.1360(10) 1.0566(5) 0.061(7) Uiso 0.50 1 d PD A 1 H64A H 0.1594 0.1175 1.0691 0.091 Uiso 0.50 1 calc PR A 1 H64B H 0.1025 0.1427 1.0669 0.091 Uiso 0.50 1 calc PR A 1 H64C H 0.1506 0.1692 1.0508 0.091 Uiso 0.50 1 calc PR A 1 C65 C 0.1723(9) 0.1040(11) 1.0165(5) 0.054(6) Uiso 0.50 1 d PD A 1 H65A H 0.1678 0.0863 0.9982 0.081 Uiso 0.50 1 calc PR A 1 H65B H 0.1986 0.0857 1.0278 0.081 Uiso 0.50 1 calc PR A 1 H65C H 0.1836 0.1400 1.0132 0.081 Uiso 0.50 1 calc PR A 1 C63 C 0.0780(10) 0.0822(16) 1.0216(8) 0.107(13) Uiso 0.50 1 d PD A 1 H63 H 0.0845 0.0645 1.0043 0.128 Uiso 0.50 1 calc PR A 1 O4 O 0.1528(14) 0.1488(14) 1.0319(7) 0.144(12) Uiso 0.50 1 d P B 2 C66 C 0.0000 0.5000 0.9931(9) 0.171(16) Uiso 1 2 d S . . H66A H -0.0236 0.4808 0.9802 0.205 Uiso 0.50 1 calc PR . . H66B H 0.0236 0.5192 0.9802 0.205 Uiso 0.50 1 calc PR . . Cl1 Cl 0.0367(3) 0.4550(3) 1.0022(2) 0.188(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.02419(17) 0.02375(17) 0.03550(19) 0.00984(15) 0.00583(17) 0.00567(15) Pt2 0.01644(15) 0.02208(16) 0.02194(15) -0.00245(14) 0.00020(13) 0.00143(14) Zn1 0.0198(5) 0.0357(6) 0.0307(6) -0.0077(5) 0.0046(4) -0.0011(5) Zn2 0.0324(6) 0.0208(5) 0.0225(5) 0.0013(4) -0.0042(4) 0.0015(5) Br1 0.0372(5) 0.0329(5) 0.0341(5) -0.0020(4) -0.0085(4) -0.0053(4) Br2 0.0545(7) 0.0304(5) 0.0381(6) -0.0026(4) -0.0109(5) 0.0185(5) Br3 0.0300(5) 0.0493(6) 0.0376(6) -0.0133(5) -0.0033(4) 0.0144(5) Br4 0.0310(5) 0.0368(5) 0.0392(6) -0.0101(5) 0.0048(4) -0.0062(4) S1 0.0298(12) 0.0296(12) 0.0275(12) -0.0020(10) -0.0018(10) 0.0120(10) S2 0.0262(12) 0.0311(13) 0.0594(18) 0.0229(12) 0.0004(12) 0.0039(10) S3 0.0196(10) 0.0240(11) 0.0324(13) -0.0062(10) 0.0065(9) 0.0019(9) S4 0.0367(14) 0.0345(14) 0.0478(16) 0.0103(12) 0.0138(13) 0.0166(12) N1 0.037(5) 0.030(4) 0.034(5) -0.002(3) 0.001(4) 0.001(4) N2 0.018(4) 0.045(5) 0.038(5) -0.013(4) 0.002(3) 0.004(4) N3 0.032(4) 0.032(4) 0.025(4) 0.003(3) -0.001(3) 0.006(4) N4 0.025(4) 0.021(3) 0.027(4) -0.002(3) -0.004(3) 0.001(3) N5 0.037(5) 0.023(4) 0.033(4) 0.009(3) 0.010(4) 0.002(4) N6 0.030(4) 0.023(4) 0.028(4) 0.005(3) 0.006(3) 0.001(3) N7 0.013(3) 0.026(4) 0.028(4) -0.006(3) 0.000(3) 0.000(3) N8 0.025(4) 0.027(4) 0.023(4) 0.002(3) 0.004(3) -0.007(3) C1 0.037(6) 0.034(5) 0.033(5) 0.003(4) 0.012(5) 0.014(5) C2 0.038(6) 0.029(5) 0.036(6) 0.002(4) 0.012(4) 0.009(4) C3 0.022(5) 0.023(4) 0.040(6) 0.002(4) 0.008(4) 0.002(4) C4 0.030(5) 0.033(5) 0.059(7) -0.008(5) 0.006(5) 0.009(5) C5 0.036(6) 0.043(6) 0.040(6) -0.015(5) 0.007(5) 0.010(5) C6 0.031(5) 0.031(5) 0.018(5) -0.006(4) -0.001(4) -0.001(4) C7 0.032(5) 0.019(4) 0.026(5) -0.004(4) 0.004(4) -0.001(4) C8 0.022(4) 0.021(4) 0.027(5) 0.004(4) -0.002(4) 0.003(4) C9 0.043(6) 0.025(5) 0.049(6) -0.016(5) 0.011(5) -0.007(5) C10 0.025(5) 0.038(6) 0.049(6) -0.017(5) 0.017(5) -0.004(4) C11 0.028(5) 0.039(5) 0.029(5) 0.003(5) -0.003(4) 0.003(4) C12 0.029(5) 0.036(5) 0.034(6) 0.015(4) 0.002(4) -0.003(4) C13 0.037(5) 0.034(5) 0.032(5) 0.012(4) 0.010(5) 0.005(4) C14 0.025(5) 0.037(6) 0.041(6) 0.015(5) -0.001(4) 0.000(4) C15 0.030(5) 0.029(5) 0.036(6) 0.010(4) -0.011(4) 0.007(4) C16 0.032(5) 0.030(5) 0.036(6) 0.002(4) -0.010(4) 0.006(4) C17 0.035(5) 0.031(5) 0.033(5) 0.009(4) -0.003(4) 0.009(4) C18 0.026(5) 0.018(4) 0.033(5) 0.003(4) -0.003(4) 0.003(3) C19 0.024(4) 0.032(5) 0.021(4) 0.004(4) -0.003(4) 0.002(4) C20 0.020(4) 0.024(5) 0.031(5) 0.003(4) 0.001(4) 0.002(4) C21 0.033(6) 0.041(6) 0.036(6) 0.008(5) -0.010(4) -0.005(4) C22 0.039(6) 0.042(6) 0.031(6) -0.001(5) -0.002(5) 0.006(5) C23 0.034(5) 0.032(5) 0.028(5) -0.005(4) -0.001(4) 0.000(4) C24 0.025(5) 0.032(5) 0.031(5) 0.004(4) -0.001(4) 0.007(4) C25 0.027(5) 0.022(5) 0.033(5) 0.004(4) 0.000(4) 0.004(4) C26 0.034(5) 0.015(4) 0.028(5) 0.008(4) 0.012(4) 0.003(4) C27 0.026(4) 0.031(5) 0.025(5) 0.005(4) 0.002(4) 0.000(4) C28 0.038(5) 0.027(5) 0.019(4) 0.002(4) 0.008(4) -0.004(4) C29 0.038(5) 0.025(5) 0.029(5) -0.002(4) 0.008(4) 0.000(4) C30 0.039(5) 0.024(5) 0.026(5) 0.000(4) 0.006(4) 0.003(4) C31 0.040(6) 0.045(6) 0.034(6) -0.015(5) 0.001(5) 0.003(5) C32 0.081(9) 0.038(6) 0.050(7) -0.012(6) 0.003(7) 0.007(7) C33 0.061(8) 0.082(10) 0.034(7) -0.007(7) 0.003(6) 0.015(7) C34 0.061(8) 0.064(8) 0.041(7) -0.021(6) -0.005(6) 0.031(7) C35 0.030(5) 0.023(5) 0.029(5) -0.002(4) 0.007(4) -0.005(4) C36 0.035(5) 0.042(6) 0.035(6) 0.002(5) 0.011(4) 0.003(5) C37 0.038(6) 0.041(6) 0.056(7) 0.000(5) 0.015(5) -0.003(5) C38 0.040(6) 0.049(7) 0.034(6) 0.003(5) 0.001(5) 0.004(5) C39 0.023(5) 0.040(5) 0.023(5) 0.005(4) -0.006(4) 0.001(4) C40 0.022(5) 0.040(5) 0.023(5) -0.007(4) -0.005(4) -0.003(4) C41 0.031(5) 0.029(5) 0.031(5) -0.005(4) -0.001(4) -0.007(4) C42 0.023(4) 0.028(5) 0.029(5) -0.006(4) 0.003(4) -0.008(4) C43 0.017(4) 0.035(5) 0.016(4) -0.005(4) 0.002(3) 0.003(4) C44 0.023(4) 0.029(5) 0.019(4) -0.003(4) -0.001(4) -0.007(4) C45 0.022(4) 0.028(5) 0.027(5) -0.003(4) -0.001(4) 0.001(4) C46 0.023(4) 0.037(5) 0.024(5) 0.000(4) 0.000(4) 0.003(4) C47 0.029(5) 0.034(5) 0.024(5) -0.003(4) -0.002(4) -0.002(4) C48 0.036(5) 0.023(4) 0.023(5) -0.002(4) 0.002(4) -0.009(4) C49 0.050(6) 0.024(5) 0.042(6) -0.008(5) -0.021(5) 0.001(5) C50 0.061(8) 0.046(7) 0.052(7) -0.017(6) -0.009(6) 0.008(6) C51 0.050(7) 0.045(7) 0.071(8) -0.024(6) -0.016(6) -0.012(6) C52 0.117(13) 0.032(6) 0.055(8) 0.012(6) -0.016(8) -0.041(8) C53 0.028(5) 0.050(6) 0.030(5) -0.003(5) -0.003(4) 0.004(5) C54 0.041(6) 0.043(6) 0.042(7) 0.004(5) -0.017(5) 0.009(5) C55 0.034(6) 0.071(8) 0.036(6) -0.003(6) -0.001(5) 0.002(6) C56 0.025(5) 0.069(8) 0.056(7) 0.007(6) -0.008(5) 0.003(6) O1 0.117(9) 0.046(5) 0.050(5) -0.002(4) -0.011(6) -0.019(6) N9 0.040(5) 0.039(5) 0.041(5) -0.006(4) 0.005(4) -0.007(4) C57 0.052(7) 0.059(8) 0.036(6) 0.006(6) -0.001(5) -0.014(6) C58 0.054(8) 0.063(9) 0.062(9) -0.036(7) 0.012(7) -0.003(7) C59 0.029(6) 0.085(10) 0.065(9) 0.010(8) -0.008(6) -0.002(6) O2 0.066(8) 0.25(2) 0.069(8) -0.034(11) 0.040(7) -0.014(11) N10 0.068(8) 0.092(10) 0.068(8) -0.001(8) 0.004(7) 0.017(7) C60 0.034(8) 0.18(3) 0.14(2) 0.088(19) -0.013(11) -0.014(12) C61 0.078(11) 0.075(10) 0.072(10) -0.027(9) 0.014(9) -0.018(9) C62 0.096(13) 0.081(11) 0.066(10) 0.006(9) 0.017(9) 0.010(10) Cl1 0.157(7) 0.155(7) 0.253(10) 0.012(7) -0.069(7) -0.007(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 N5 2.046(8) . ? Pt1 N6 2.049(8) . ? Pt1 S4 2.290(3) . ? Pt1 S2 2.296(3) . ? Pt2 N8 2.048(8) . ? Pt2 N7 2.070(7) . ? Pt2 S1 2.288(2) . ? Pt2 S3 2.292(2) . ? Zn1 N2 2.029(8) . ? Zn1 N1 2.051(9) . ? Zn1 Br3 2.3661(15) . ? Zn1 Br4 2.3784(15) . ? Zn2 N3 2.023(8) . ? Zn2 N4 2.060(8) . ? Zn2 Br2 2.3507(15) . ? Zn2 Br1 2.3649(14) . ? S1 C18 1.733(10) . ? S2 C13 1.741(10) . ? S3 C8 1.719(9) . ? S4 C3 1.752(10) . ? N1 C1 1.336(13) . ? N1 C5 1.355(14) . ? N2 C6 1.352(12) . ? N2 C10 1.354(13) . ? N3 C11 1.339(12) . ? N3 C15 1.343(13) . ? N4 C20 1.333(12) . ? N4 C16 1.344(12) . ? N5 C21 1.346(13) . ? N5 C25 1.376(12) . ? N6 C26 1.352(12) . ? N6 C30 1.356(12) . ? N7 C39 1.306(11) . ? N7 C43 1.349(12) . ? N8 C48 1.321(11) . ? N8 C44 1.361(12) . ? C1 C2 1.380(15) . ? C2 C3 1.380(13) . ? C3 C4 1.390(15) . ? C4 C5 1.386(16) . ? C6 C7 1.384(13) . ? C7 C8 1.417(12) . ? C8 C9 1.403(13) . ? C9 C10 1.382(14) . ? C11 C12 1.372(14) . ? C12 C13 1.384(14) . ? C13 C14 1.401(14) . ? C14 C15 1.379(14) . ? C16 C17 1.372(15) . ? C17 C18 1.403(13) . ? C18 C19 1.404(13) . ? C19 C20 1.395(13) . ? C21 C22 1.379(15) . ? C22 C23 1.412(14) . ? C23 C24 1.403(14) . ? C23 C31 1.522(14) . ? C24 C25 1.389(13) . ? C25 C26 1.483(13) . ? C26 C27 1.382(13) . ? C27 C28 1.405(13) . ? C28 C29 1.385(13) . ? C28 C35 1.537(13) . ? C29 C30 1.374(14) . ? C31 C33 1.546(16) . ? C31 C32 1.547(17) . ? C31 C34 1.560(16) . ? C35 C38 1.515(14) . ? C35 C36 1.520(13) . ? C35 C37 1.552(14) . ? C39 C40 1.381(14) . ? C40 C41 1.381(14) . ? C41 C42 1.390(13) . ? C41 C49 1.540(13) . ? C42 C43 1.367(12) . ? C43 C44 1.491(12) . ? C44 C45 1.404(13) . ? C45 C46 1.391(13) . ? C46 C47 1.394(13) . ? C46 C53 1.526(14) . ? C47 C48 1.377(13) . ? C49 C52 1.507(16) . ? C49 C50 1.530(17) . ? C49 C51 1.533(14) . ? C53 C55 1.505(14) . ? C53 C54 1.552(16) . ? C53 C56 1.562(15) . ? O1 C57 1.235(15) . ? N9 C57 1.315(16) . ? N9 C58 1.424(15) . ? N9 C59 1.455(15) . ? O2 C60 1.24(3) . ? N10 C61 1.375(18) . ? N10 C62 1.457(19) . ? N10 C60 1.55(3) . ? O3 C63 1.221(18) . ? N11 C63 1.391(18) . ? N11 C65 1.415(18) . ? N11 C64 1.473(18) . ? C66 Cl1 1.551(13) . ? C66 Cl1 1.551(13) 2_565 ? 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 N5 Pt1 N6 79.4(3) . . ? N5 Pt1 S4 173.4(2) . . ? N6 Pt1 S4 96.0(2) . . ? N5 Pt1 S2 96.2(3) . . ? N6 Pt1 S2 174.8(2) . . ? S4 Pt1 S2 88.63(11) . . ? N8 Pt2 N7 79.0(3) . . ? N8 Pt2 S1 172.2(2) . . ? N7 Pt2 S1 97.0(2) . . ? N8 Pt2 S3 96.2(2) . . ? N7 Pt2 S3 174.6(2) . . ? S1 Pt2 S3 88.08(9) . . ? N2 Zn1 N1 103.6(4) . . ? N2 Zn1 Br3 106.5(3) . . ? N1 Zn1 Br3 108.1(2) . . ? N2 Zn1 Br4 109.2(2) . . ? N1 Zn1 Br4 108.3(2) . . ? Br3 Zn1 Br4 119.95(6) . . ? N3 Zn2 N4 101.3(3) . . ? N3 Zn2 Br2 107.7(2) . . ? N4 Zn2 Br2 110.6(2) . . ? N3 Zn2 Br1 109.9(2) . . ? N4 Zn2 Br1 106.8(2) . . ? Br2 Zn2 Br1 119.13(6) . . ? C18 S1 Pt2 106.5(3) . . ? C13 S2 Pt1 109.8(4) . . ? C8 S3 Pt2 107.0(3) . . ? C3 S4 Pt1 106.6(3) . . ? C1 N1 C5 116.8(9) . . ? C1 N1 Zn1 122.1(7) . . ? C5 N1 Zn1 121.0(7) . . ? C6 N2 C10 117.1(8) . . ? C6 N2 Zn1 123.1(7) . . ? C10 N2 Zn1 119.8(6) . . ? C11 N3 C15 116.7(9) . . ? C11 N3 Zn2 123.2(7) . . ? C15 N3 Zn2 119.3(6) . . ? C20 N4 C16 116.8(8) . . ? C20 N4 Zn2 121.0(6) . . ? C16 N4 Zn2 122.2(6) . . ? C21 N5 C25 118.2(9) . . ? C21 N5 Pt1 127.2(7) . . ? C25 N5 Pt1 114.3(7) . . ? C26 N6 C30 116.7(8) . . ? C26 N6 Pt1 115.7(6) . . ? C30 N6 Pt1 127.5(7) . . ? C39 N7 C43 118.9(8) . . ? C39 N7 Pt2 125.7(7) . . ? C43 N7 Pt2 115.4(6) . . ? C48 N8 C44 118.0(8) . . ? C48 N8 Pt2 126.6(7) . . ? C44 N8 Pt2 114.8(6) . . ? N1 C1 C2 123.0(9) . . ? C1 C2 C3 120.1(10) . . ? C2 C3 C4 118.0(10) . . ? C2 C3 S4 123.7(8) . . ? C4 C3 S4 118.3(8) . . ? C5 C4 C3 118.5(9) . . ? N1 C5 C4 123.6(10) . . ? N2 C6 C7 123.6(9) . . ? C6 C7 C8 119.6(8) . . ? C9 C8 C7 115.9(8) . . ? C9 C8 S3 125.7(7) . . ? C7 C8 S3 118.4(7) . . ? C10 C9 C8 121.1(9) . . ? N2 C10 C9 122.4(9) . . ? N3 C11 C12 123.3(9) . . ? C11 C12 C13 120.1(9) . . ? C12 C13 C14 117.1(9) . . ? C12 C13 S2 118.1(8) . . ? C14 C13 S2 124.8(8) . . ? C15 C14 C13 118.7(9) . . ? N3 C15 C14 123.8(9) . . ? N4 C16 C17 123.3(9) . . ? C16 C17 C18 120.8(9) . . ? C17 C18 C19 115.7(9) . . ? C17 C18 S1 120.1(7) . . ? C19 C18 S1 124.2(7) . . ? C20 C19 C18 119.6(9) . . ? N4 C20 C19 123.8(8) . . ? N5 C21 C22 122.9(10) . . ? C21 C22 C23 119.8(10) . . ? C24 C23 C22 117.1(9) . . ? C24 C23 C31 123.4(9) . . ? C22 C23 C31 119.5(9) . . ? C25 C24 C23 120.2(9) . . ? N5 C25 C24 121.5(9) . . ? N5 C25 C26 114.7(8) . . ? C24 C25 C26 123.9(9) . . ? N6 C26 C27 123.1(9) . . ? N6 C26 C25 114.3(8) . . ? C27 C26 C25 122.5(8) . . ? C26 C27 C28 119.8(9) . . ? C29 C28 C27 116.7(9) . . ? C29 C28 C35 121.2(9) . . ? C27 C28 C35 122.1(8) . . ? C30 C29 C28 120.6(9) . . ? N6 C30 C29 123.1(9) . . ? C23 C31 C33 109.2(10) . . ? C23 C31 C32 108.3(9) . . ? C33 C31 C32 111.9(10) . . ? C23 C31 C34 110.9(9) . . ? C33 C31 C34 107.7(10) . . ? C32 C31 C34 108.8(10) . . ? C38 C35 C36 108.9(8) . . ? C38 C35 C28 108.7(8) . . ? C36 C35 C28 113.4(8) . . ? C38 C35 C37 109.0(9) . . ? C36 C35 C37 109.1(8) . . ? C28 C35 C37 107.7(8) . . ? N7 C39 C40 122.2(9) . . ? C39 C40 C41 120.6(8) . . ? C40 C41 C42 116.0(9) . . ? C40 C41 C49 123.0(9) . . ? C42 C41 C49 121.0(9) . . ? C43 C42 C41 120.7(9) . . ? N7 C43 C42 121.5(8) . . ? N7 C43 C44 114.1(8) . . ? C42 C43 C44 124.4(8) . . ? N8 C44 C45 120.9(8) . . ? N8 C44 C43 115.0(8) . . ? C45 C44 C43 124.1(8) . . ? C46 C45 C44 120.1(9) . . ? C45 C46 C47 117.4(9) . . ? C45 C46 C53 123.4(9) . . ? C47 C46 C53 119.1(9) . . ? C48 C47 C46 119.1(9) . . ? N8 C48 C47 124.3(9) . . ? C52 C49 C50 109.4(10) . . ? C52 C49 C51 109.2(11) . . ? C50 C49 C51 107.2(9) . . ? C52 C49 C41 111.6(9) . . ? C50 C49 C41 107.4(9) . . ? C51 C49 C41 111.9(9) . . ? C55 C53 C46 108.9(9) . . ? C55 C53 C54 109.2(10) . . ? C46 C53 C54 112.0(8) . . ? C55 C53 C56 110.2(9) . . ? C46 C53 C56 108.7(9) . . ? C54 C53 C56 107.9(9) . . ? C57 N9 C58 121.5(11) . . ? C57 N9 C59 119.7(11) . . ? C58 N9 C59 118.6(11) . . ? O1 C57 N9 126.6(13) . . ? C61 N10 C62 119.6(14) . . ? C61 N10 C60 120.3(17) . . ? C62 N10 C60 120.1(15) . . ? O2 C60 N10 131(2) . . ? C63 N11 C65 126(2) . . ? C63 N11 C64 131(3) . . ? C65 N11 C64 104(2) . . ? O3 C63 N11 142(4) . . ? Cl1 C66 Cl1 148(3) . 2_565 ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.385 _refine_diff_density_min -1.257 _refine_diff_density_rms 0.187 data_ic13423 _database_code_depnum_ccdc_archive 'CCDC 859739' #TrackingRef '4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C60.50 H73 Cl9 I4 N8 Pt2 S4 Zn2' _chemical_formula_weight 2388.08 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 '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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 25.7484(8) _cell_length_b 22.6562(6) _cell_length_c 27.7603(8) _cell_angle_alpha 90.00 _cell_angle_beta 98.9677(11) _cell_angle_gamma 90.00 _cell_volume 15996.3(8) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used all _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 25.00 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas not_measured _exptl_crystal_density_diffrn 1.983 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 9096 _exptl_absorpt_coefficient_mu 6.070 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2813 _exptl_absorpt_correction_T_max 0.4434 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'NONIUS KappaCCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 93824 _diffrn_reflns_av_R_equivalents 0.0792 _diffrn_reflns_av_sigmaI/netI 0.0793 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 1.00 _diffrn_reflns_theta_max 25.00 _reflns_number_total 28176 _reflns_number_gt 18271 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'NONIUS COLLECT' _computing_cell_refinement DENZO-SMN _computing_data_reduction DENZO-SMN _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0558P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 28176 _refine_ls_number_parameters 1599 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0842 _refine_ls_R_factor_gt 0.0419 _refine_ls_wR_factor_ref 0.1144 _refine_ls_wR_factor_gt 0.0960 _refine_ls_goodness_of_fit_ref 1.006 _refine_ls_restrained_S_all 1.010 _refine_ls_shift/su_max 0.025 _refine_ls_shift/su_mean 0.001 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.441178(14) 0.486165(15) 0.568052(12) 0.02774(9) Uani 1 1 d . . . Pt2 Pt 0.219224(13) 0.161263(14) 0.821228(13) 0.02797(9) Uani 1 1 d . . . Zn1 Zn 0.32887(4) 0.17321(4) 0.58127(4) 0.0299(2) Uani 1 1 d . . . Zn2 Zn 0.41127(4) 0.43098(4) 0.83555(4) 0.0310(2) Uani 1 1 d . . . I1 I 0.27911(2) 0.11520(3) 0.51029(2) 0.03949(16) Uani 1 1 d . . . I2 I 0.41710(2) 0.13307(3) 0.62449(2) 0.03758(16) Uani 1 1 d . . . I3 I 0.49664(2) 0.37116(3) 0.85669(3) 0.04744(18) Uani 1 1 d . . . I4 I 0.38617(3) 0.51435(3) 0.89029(2) 0.04561(18) Uani 1 1 d . . . S1 S 0.36243(9) 0.45244(10) 0.52764(9) 0.0345(6) Uani 1 1 d . . . S2 S 0.17093(9) 0.16411(10) 0.74481(8) 0.0320(5) Uani 1 1 d . . . S3 S 0.39591(9) 0.54480(10) 0.61458(8) 0.0349(6) Uani 1 1 d . . . S4 S 0.20237(9) 0.25974(10) 0.82667(9) 0.0372(6) Uani 1 1 d . . . N1 N 0.3408(3) 0.2587(3) 0.5620(2) 0.0254(16) Uani 1 1 d . . . N2 N 0.2805(3) 0.1794(3) 0.6321(2) 0.0285(17) Uani 1 1 d . . . N3 N 0.4112(3) 0.4665(3) 0.7676(3) 0.0299(17) Uani 1 1 d . . . N4 N 0.3485(3) 0.3735(3) 0.8288(2) 0.0287(17) Uani 1 1 d . . . N5 N 0.5142(3) 0.5187(3) 0.5978(2) 0.0272(17) Uani 1 1 d . . . N6 N 0.4898(3) 0.4369(3) 0.5312(2) 0.0304(17) Uani 1 1 d . . . N7 N 0.2574(3) 0.1493(3) 0.8909(2) 0.0283(17) Uani 1 1 d . . . N8 N 0.2337(3) 0.0717(3) 0.8217(3) 0.0297(17) Uani 1 1 d . . . C1 C 0.3844(3) 0.2881(4) 0.5833(3) 0.031(2) Uani 1 1 d . . . H1 H 0.4097 0.2676 0.6057 0.037 Uiso 1 1 calc R . . C2 C 0.3932(3) 0.3470(3) 0.5737(3) 0.028(2) Uani 1 1 d . . . H2 H 0.4241 0.3661 0.5894 0.034 Uiso 1 1 calc R . . C3 C 0.3572(3) 0.3779(4) 0.5414(3) 0.027(2) Uani 1 1 d . . . C4 C 0.3132(3) 0.3469(4) 0.5190(3) 0.030(2) Uani 1 1 d . . . H4 H 0.2875 0.3661 0.4960 0.036 Uiso 1 1 calc R . . C5 C 0.3069(3) 0.2886(4) 0.5303(3) 0.029(2) Uani 1 1 d . . . H5 H 0.2765 0.2685 0.5146 0.035 Uiso 1 1 calc R . . C6 C 0.2994(3) 0.1811(4) 0.6797(3) 0.031(2) Uani 1 1 d . . . H6 H 0.3364 0.1846 0.6892 0.037 Uiso 1 1 calc R . . C7 C 0.2684(3) 0.1779(3) 0.7160(3) 0.031(2) Uani 1 1 d . . . H7 H 0.2839 0.1792 0.7493 0.038 Uiso 1 1 calc R . . C8 C 0.2146(3) 0.1729(3) 0.7031(3) 0.024(2) Uani 1 1 d . . . C9 C 0.1937(4) 0.1736(4) 0.6532(3) 0.039(2) Uani 1 1 d . . . H9 H 0.1568 0.1722 0.6428 0.046 Uiso 1 1 calc R . . C10 C 0.2279(4) 0.1764(4) 0.6199(3) 0.041(2) Uani 1 1 d . . . H10 H 0.2135 0.1763 0.5863 0.049 Uiso 1 1 calc R . . C11 C 0.4040(3) 0.5248(4) 0.7585(3) 0.030(2) Uani 1 1 d . . . H11 H 0.4008 0.5506 0.7849 0.036 Uiso 1 1 calc R . . C12 C 0.4010(3) 0.5483(4) 0.7122(3) 0.037(2) Uani 1 1 d . . . H12 H 0.3964 0.5896 0.7074 0.044 Uiso 1 1 calc R . . C13 C 0.4048(3) 0.5126(4) 0.6730(3) 0.027(2) Uani 1 1 d . . . C14 C 0.4131(4) 0.4532(4) 0.6822(3) 0.034(2) Uani 1 1 d . . . H14 H 0.4171 0.4268 0.6564 0.041 Uiso 1 1 calc R . . C15 C 0.4155(4) 0.4324(4) 0.7293(3) 0.036(2) Uani 1 1 d . . . H15 H 0.4205 0.3912 0.7347 0.043 Uiso 1 1 calc R . . C16 C 0.2997(3) 0.3950(4) 0.8305(3) 0.031(2) Uani 1 1 d . . . H16 H 0.2960 0.4366 0.8330 0.037 Uiso 1 1 calc R . . C17 C 0.2566(3) 0.3621(4) 0.8289(3) 0.030(2) Uani 1 1 d . . . H17 H 0.2236 0.3808 0.8291 0.036 Uiso 1 1 calc R . . C18 C 0.2591(3) 0.3000(3) 0.8268(3) 0.0239(19) Uani 1 1 d . . . C19 C 0.3095(3) 0.2775(4) 0.8251(3) 0.028(2) Uani 1 1 d . . . H19 H 0.3144 0.2360 0.8232 0.034 Uiso 1 1 calc R . . C20 C 0.3516(3) 0.3142(4) 0.8262(3) 0.029(2) Uani 1 1 d . . . H20 H 0.3850 0.2970 0.8251 0.035 Uiso 1 1 calc R . . C21 C 0.5241(4) 0.5635(4) 0.6286(3) 0.037(2) Uani 1 1 d . . . H21 H 0.4957 0.5814 0.6411 0.045 Uiso 1 1 calc R . . C22 C 0.5741(4) 0.5850(4) 0.6431(3) 0.043(3) Uani 1 1 d . . . H22 H 0.5790 0.6177 0.6648 0.051 Uiso 1 1 calc R . . C23 C 0.6174(4) 0.5602(4) 0.6268(3) 0.035(2) Uani 1 1 d . . . C24 C 0.6064(4) 0.5129(4) 0.5956(3) 0.035(2) Uani 1 1 d . . . H24 H 0.6345 0.4937 0.5833 0.042 Uiso 1 1 calc R . . C25 C 0.5562(3) 0.4928(4) 0.5818(3) 0.030(2) Uani 1 1 d . . . C26 C 0.5418(3) 0.4431(3) 0.5471(3) 0.027(2) Uani 1 1 d . . . C27 C 0.5789(3) 0.4081(4) 0.5303(3) 0.029(2) Uani 1 1 d . . . H27 H 0.6151 0.4149 0.5416 0.035 Uiso 1 1 calc R . . C28 C 0.5641(4) 0.3631(4) 0.4972(3) 0.034(2) Uani 1 1 d . . . C29 C 0.5112(4) 0.3580(4) 0.4800(3) 0.036(2) Uani 1 1 d . . . H29 H 0.4993 0.3292 0.4558 0.043 Uiso 1 1 calc R . . C30 C 0.4747(4) 0.3947(4) 0.4978(3) 0.034(2) Uani 1 1 d . . . H30 H 0.4383 0.3896 0.4859 0.041 Uiso 1 1 calc R . . C31 C 0.6725(4) 0.5844(4) 0.6410(4) 0.047(3) Uani 1 1 d . . . C32 C 0.6893(5) 0.5722(7) 0.6961(4) 0.106(6) Uani 1 1 d . . . H32A H 0.7257 0.5853 0.7061 0.159 Uiso 1 1 calc R . . H32B H 0.6869 0.5298 0.7023 0.159 Uiso 1 1 calc R . . H32C H 0.6661 0.5937 0.7148 0.159 Uiso 1 1 calc R . . C33 C 0.6725(5) 0.6490(5) 0.6307(6) 0.107(5) Uani 1 1 d . . . H33A H 0.6580 0.6560 0.5964 0.161 Uiso 1 1 calc R . . H33B H 0.7086 0.6641 0.6374 0.161 Uiso 1 1 calc R . . H33C H 0.6508 0.6695 0.6515 0.161 Uiso 1 1 calc R . . C34 C 0.7133(4) 0.5555(5) 0.6149(4) 0.064(3) Uani 1 1 d . . . H34A H 0.7027 0.5594 0.5796 0.096 Uiso 1 1 calc R . . H34B H 0.7163 0.5136 0.6236 0.096 Uiso 1 1 calc R . . H34C H 0.7474 0.5748 0.6246 0.096 Uiso 1 1 calc R . . C35 C 0.6042(4) 0.3183(4) 0.4837(3) 0.041(2) Uani 1 1 d . . . C36 C 0.6585(4) 0.3449(5) 0.4876(4) 0.058(3) Uani 1 1 d . . . H36A H 0.6568 0.3815 0.4686 0.086 Uiso 1 1 calc R . . H36B H 0.6821 0.3169 0.4749 0.086 Uiso 1 1 calc R . . H36C H 0.6720 0.3535 0.5219 0.086 Uiso 1 1 calc R . . C37 C 0.5888(4) 0.2956(4) 0.4314(3) 0.048(3) Uani 1 1 d . . . H37A H 0.5819 0.3292 0.4091 0.072 Uiso 1 1 calc R . . H37B H 0.5570 0.2713 0.4294 0.072 Uiso 1 1 calc R . . H37C H 0.6175 0.2719 0.4223 0.072 Uiso 1 1 calc R . . C38 C 0.6047(5) 0.2680(4) 0.5204(4) 0.064(3) Uani 1 1 d . . . H38A H 0.6280 0.2365 0.5124 0.096 Uiso 1 1 calc R . . H38B H 0.5690 0.2524 0.5190 0.096 Uiso 1 1 calc R . . H38C H 0.6174 0.2828 0.5533 0.096 Uiso 1 1 calc R . . C39 C 0.2733(3) 0.1928(4) 0.9239(3) 0.035(2) Uani 1 1 d . . . H39 H 0.2665 0.2327 0.9146 0.042 Uiso 1 1 calc R . . C40 C 0.2989(4) 0.1808(4) 0.9703(3) 0.041(2) Uani 1 1 d . . . H40 H 0.3093 0.2124 0.9922 0.049 Uiso 1 1 calc R . . C41 C 0.3097(4) 0.1226(4) 0.9854(3) 0.042(2) Uani 1 1 d . . . C42 C 0.2953(4) 0.0792(4) 0.9503(3) 0.040(2) Uani 1 1 d . . . H42 H 0.3037 0.0391 0.9581 0.048 Uiso 1 1 calc R . . C43 C 0.2693(3) 0.0928(4) 0.9048(3) 0.031(2) Uani 1 1 d . . . C44 C 0.2554(3) 0.0491(4) 0.8661(3) 0.028(2) Uani 1 1 d . . . C45 C 0.2636(3) -0.0115(4) 0.8719(3) 0.032(2) Uani 1 1 d . . . H45 H 0.2770 -0.0267 0.9032 0.039 Uiso 1 1 calc R . . C46 C 0.2524(3) -0.0502(4) 0.8327(3) 0.031(2) Uani 1 1 d . . . C47 C 0.2336(3) -0.0246(4) 0.7886(3) 0.034(2) Uani 1 1 d . . . H47 H 0.2274 -0.0489 0.7604 0.041 Uiso 1 1 calc R . . C48 C 0.2237(3) 0.0339(4) 0.7838(3) 0.033(2) Uani 1 1 d . . . H48 H 0.2091 0.0489 0.7526 0.040 Uiso 1 1 calc R . . C49 C 0.3399(5) 0.1068(5) 1.0356(4) 0.061(3) Uani 1 1 d . . . C50 C 0.3955(4) 0.0891(5) 1.0288(4) 0.076(4) Uani 1 1 d . . . H50A H 0.3946 0.0507 1.0125 0.113 Uiso 1 1 calc R . . H50B H 0.4178 0.0865 1.0607 0.113 Uiso 1 1 calc R . . H50C H 0.4099 0.1188 1.0088 0.113 Uiso 1 1 calc R . . C51 C 0.3123(5) 0.0556(5) 1.0582(4) 0.075(4) Uani 1 1 d . . . H51A H 0.2752 0.0656 1.0580 0.113 Uiso 1 1 calc R . . H51B H 0.3294 0.0491 1.0919 0.113 Uiso 1 1 calc R . . H51C H 0.3148 0.0196 1.0391 0.113 Uiso 1 1 calc R . . C52 C 0.3427(6) 0.1588(5) 1.0703(4) 0.101(5) Uani 1 1 d . . . H52A H 0.3609 0.1917 1.0572 0.151 Uiso 1 1 calc R . . H52B H 0.3619 0.1472 1.1022 0.151 Uiso 1 1 calc R . . H52C H 0.3070 0.1710 1.0740 0.151 Uiso 1 1 calc R . . C53 C 0.2610(4) -0.1166(4) 0.8385(3) 0.036(2) Uani 1 1 d . . . C54 C 0.2092(4) -0.1484(4) 0.8193(4) 0.056(3) Uani 1 1 d . . . H54A H 0.2005 -0.1423 0.7840 0.084 Uiso 1 1 calc R . . H54B H 0.1810 -0.1323 0.8354 0.084 Uiso 1 1 calc R . . H54C H 0.2131 -0.1907 0.8263 0.084 Uiso 1 1 calc R . . C55 C 0.2794(4) -0.1341(4) 0.8914(4) 0.051(3) Uani 1 1 d . . . H55A H 0.2793 -0.1772 0.8943 0.076 Uiso 1 1 calc R . . H55B H 0.2556 -0.1171 0.9121 0.076 Uiso 1 1 calc R . . H55C H 0.3151 -0.1192 0.9019 0.076 Uiso 1 1 calc R . . C56 C 0.3016(4) -0.1366(4) 0.8079(4) 0.049(3) Uani 1 1 d . . . H56A H 0.3352 -0.1169 0.8192 0.074 Uiso 1 1 calc R . . H56B H 0.2896 -0.1265 0.7736 0.074 Uiso 1 1 calc R . . H56C H 0.3062 -0.1795 0.8109 0.074 Uiso 1 1 calc R . . Pt3 Pt 0.163625(14) 0.247377(16) 0.456012(13) 0.03194(10) Uani 1 1 d . . . Pt4 Pt 0.029566(14) 0.492179(16) 0.102069(14) 0.03456(10) Uani 1 1 d . . . Zn3 Zn -0.05127(4) 0.45964(4) 0.35781(4) 0.0342(3) Uani 1 1 d . . . Zn4 Zn 0.12713(4) 0.17916(5) 0.17682(4) 0.0366(3) Uani 1 1 d . . . I5 I -0.07576(3) 0.54627(3) 0.40845(3) 0.0567(2) Uani 1 1 d . . . I6 I -0.11972(3) 0.37874(3) 0.33176(2) 0.04742(18) Uani 1 1 d . . . I7 I 0.03445(3) 0.13563(3) 0.16340(2) 0.04495(17) Uani 1 1 d . . . I8 I 0.20195(3) 0.12899(3) 0.14091(3) 0.0557(2) Uani 1 1 d . . . S5 S 0.17384(9) 0.34804(10) 0.46254(9) 0.0423(6) Uani 1 1 d . . . S6 S 0.05473(10) 0.54970(11) 0.16975(9) 0.0427(6) Uani 1 1 d . . . S7 S 0.22300(10) 0.24785(12) 0.40300(9) 0.0451(7) Uani 1 1 d . . . S8 S 0.11442(9) 0.45877(11) 0.11057(10) 0.0439(6) Uani 1 1 d . . . N9 N 0.0149(3) 0.4220(3) 0.3947(3) 0.0338(18) Uani 1 1 d . . . N10 N -0.0234(3) 0.4885(3) 0.2969(3) 0.0361(19) Uani 1 1 d . . . N11 N 0.1545(3) 0.1943(3) 0.2485(2) 0.0350(19) Uani 1 1 d . . . N12 N 0.1207(3) 0.2641(3) 0.1506(3) 0.0365(19) Uani 1 1 d . . . N13 N 0.1470(3) 0.1598(3) 0.4534(2) 0.0315(18) Uani 1 1 d . . . N14 N 0.1161(3) 0.2413(3) 0.5091(3) 0.0333(18) Uani 1 1 d . . . N15 N 0.0011(3) 0.4435(3) 0.0409(2) 0.0305(17) Uani 1 1 d . . . N16 N -0.0454(3) 0.5246(3) 0.0864(3) 0.0347(19) Uani 1 1 d . . . C57 C 0.0340(5) 0.3746(5) 0.3794(4) 0.083(4) Uani 1 1 d . . . H57 H 0.0130 0.3548 0.3530 0.099 Uiso 1 1 calc R . . C58 C 0.0823(5) 0.3491(5) 0.3974(4) 0.082(4) Uani 1 1 d . . . H58 H 0.0939 0.3146 0.3828 0.098 Uiso 1 1 calc R . . C59 C 0.1125(4) 0.3747(4) 0.4363(3) 0.037(2) Uani 1 1 d . . . C60 C 0.0918(4) 0.4242(4) 0.4533(4) 0.053(3) Uani 1 1 d . . . H60 H 0.1111 0.4445 0.4802 0.064 Uiso 1 1 calc R . . C61 C 0.0437(4) 0.4457(4) 0.4323(4) 0.054(3) Uani 1 1 d . . . H61 H 0.0307 0.4800 0.4462 0.064 Uiso 1 1 calc R . . C62 C -0.0246(3) 0.4556(4) 0.2569(3) 0.035(2) Uani 1 1 d . . . H62 H -0.0420 0.4186 0.2560 0.042 Uiso 1 1 calc R . . C63 C -0.0030(3) 0.4711(4) 0.2180(3) 0.033(2) Uani 1 1 d . . . H63 H -0.0060 0.4452 0.1907 0.040 Uiso 1 1 calc R . . C64 C 0.0236(3) 0.5245(4) 0.2164(3) 0.033(2) Uani 1 1 d . . . C65 C 0.0247(4) 0.5594(4) 0.2575(3) 0.042(2) Uani 1 1 d . . . H65 H 0.0420 0.5965 0.2590 0.050 Uiso 1 1 calc R . . C66 C 0.0008(4) 0.5412(4) 0.2964(3) 0.040(2) Uani 1 1 d . . . H66 H 0.0015 0.5667 0.3236 0.048 Uiso 1 1 calc R . . C67 C 0.2042(4) 0.2104(4) 0.2620(4) 0.044(3) Uani 1 1 d . . . H67 H 0.2266 0.2106 0.2378 0.053 Uiso 1 1 calc R . . C68 C 0.2257(4) 0.2269(4) 0.3088(3) 0.042(3) Uani 1 1 d . . . H68 H 0.2619 0.2369 0.3163 0.051 Uiso 1 1 calc R . . C69 C 0.1934(3) 0.2284(4) 0.3448(3) 0.034(2) Uani 1 1 d . . . C70 C 0.1412(3) 0.2125(4) 0.3306(3) 0.036(2) Uani 1 1 d . . . H70 H 0.1177 0.2129 0.3538 0.043 Uiso 1 1 calc R . . C71 C 0.1234(4) 0.1960(4) 0.2831(3) 0.039(2) Uani 1 1 d . . . H71 H 0.0874 0.1853 0.2744 0.046 Uiso 1 1 calc R . . C72 C 0.1634(4) 0.2953(4) 0.1449(3) 0.039(2) Uani 1 1 d . . . H72 H 0.1965 0.2757 0.1498 0.046 Uiso 1 1 calc R . . C73 C 0.1624(4) 0.3536(4) 0.1327(3) 0.037(2) Uani 1 1 d . . . H73 H 0.1941 0.3733 0.1287 0.045 Uiso 1 1 calc R . . C74 C 0.1145(3) 0.3848(4) 0.1258(3) 0.033(2) Uani 1 1 d . . . C75 C 0.0711(4) 0.3518(4) 0.1326(3) 0.039(2) Uani 1 1 d . . . H75 H 0.0375 0.3701 0.1287 0.047 Uiso 1 1 calc R . . C76 C 0.0755(4) 0.2929(4) 0.1449(3) 0.037(2) Uani 1 1 d . . . H76 H 0.0446 0.2721 0.1495 0.044 Uiso 1 1 calc R . . C77 C 0.1650(3) 0.1207(4) 0.4241(3) 0.035(2) Uani 1 1 d . . . H77 H 0.1906 0.1331 0.4051 0.042 Uiso 1 1 calc R . . C78 C 0.1479(3) 0.0629(4) 0.4204(3) 0.033(2) Uani 1 1 d . . . H78 H 0.1615 0.0369 0.3987 0.040 Uiso 1 1 calc R . . C79 C 0.1104(3) 0.0417(4) 0.4484(3) 0.031(2) Uani 1 1 d . . . C80 C 0.0926(3) 0.0830(4) 0.4796(3) 0.030(2) Uani 1 1 d . . . H80 H 0.0671 0.0716 0.4991 0.036 Uiso 1 1 calc R . . C81 C 0.1119(3) 0.1411(4) 0.4827(3) 0.030(2) Uani 1 1 d . . . C82 C 0.0959(3) 0.1867(4) 0.5157(3) 0.028(2) Uani 1 1 d . . . C83 C 0.0658(3) 0.1765(4) 0.5520(3) 0.029(2) Uani 1 1 d . . . H83 H 0.0524 0.1380 0.5560 0.035 Uiso 1 1 calc R . . C84 C 0.0549(3) 0.2224(4) 0.5830(3) 0.033(2) Uani 1 1 d . . . C85 C 0.0769(4) 0.2769(4) 0.5750(3) 0.041(2) Uani 1 1 d . . . H85 H 0.0713 0.3092 0.5954 0.049 Uiso 1 1 calc R . . C86 C 0.1061(4) 0.2850(4) 0.5389(3) 0.040(2) Uani 1 1 d . . . H86 H 0.1201 0.3231 0.5345 0.048 Uiso 1 1 calc R . . C87 C 0.0912(3) -0.0217(4) 0.4426(3) 0.033(2) Uani 1 1 d . . . C88 C 0.0760(4) -0.0363(4) 0.3884(4) 0.060(3) Uani 1 1 d . . . H88A H 0.0623 -0.0767 0.3848 0.090 Uiso 1 1 calc R . . H88B H 0.1070 -0.0329 0.3721 0.090 Uiso 1 1 calc R . . H88C H 0.0489 -0.0086 0.3735 0.090 Uiso 1 1 calc R . . C89 C 0.1372(4) -0.0614(4) 0.4641(4) 0.062(3) Uani 1 1 d . . . H89A H 0.1462 -0.0540 0.4992 0.093 Uiso 1 1 calc R . . H89B H 0.1677 -0.0528 0.4481 0.093 Uiso 1 1 calc R . . H89C H 0.1271 -0.1029 0.4587 0.093 Uiso 1 1 calc R . . C90 C 0.0447(4) -0.0328(4) 0.4683(4) 0.051(3) Uani 1 1 d . . . H90A H 0.0342 -0.0744 0.4644 0.077 Uiso 1 1 calc R . . H90B H 0.0153 -0.0077 0.4541 0.077 Uiso 1 1 calc R . . H90C H 0.0543 -0.0237 0.5031 0.077 Uiso 1 1 calc R . . C91 C 0.0208(4) 0.2133(4) 0.6217(3) 0.034(2) Uani 1 1 d . . . C92 C 0.0337(4) 0.1559(4) 0.6499(3) 0.050(3) Uani 1 1 d . . . H92A H 0.0276 0.1224 0.6275 0.074 Uiso 1 1 calc R . . H92B H 0.0110 0.1522 0.6751 0.074 Uiso 1 1 calc R . . H92C H 0.0706 0.1563 0.6654 0.074 Uiso 1 1 calc R . . C93 C 0.0247(5) 0.2644(5) 0.6581(4) 0.081(4) Uani 1 1 d . . . H93A H 0.0618 0.2729 0.6701 0.122 Uiso 1 1 calc R . . H93B H 0.0069 0.2535 0.6856 0.122 Uiso 1 1 calc R . . H93C H 0.0079 0.2995 0.6420 0.122 Uiso 1 1 calc R . . C94 C -0.0363(4) 0.2108(5) 0.5959(4) 0.058(3) Uani 1 1 d . . . H94A H -0.0453 0.2480 0.5785 0.087 Uiso 1 1 calc R . . H94B H -0.0598 0.2048 0.6201 0.087 Uiso 1 1 calc R . . H94C H -0.0404 0.1780 0.5726 0.087 Uiso 1 1 calc R . . C95 C 0.0270(4) 0.4013(4) 0.0210(3) 0.039(2) Uani 1 1 d . . . H95 H 0.0635 0.3959 0.0322 0.047 Uiso 1 1 calc R . . C96 C 0.0018(4) 0.3653(4) -0.0156(3) 0.039(2) Uani 1 1 d . . . H96 H 0.0214 0.3359 -0.0293 0.046 Uiso 1 1 calc R . . C97 C -0.0515(4) 0.3711(4) -0.0327(3) 0.039(2) Uani 1 1 d . . . C98 C -0.0771(4) 0.4173(4) -0.0137(3) 0.036(2) Uani 1 1 d . . . H98 H -0.1130 0.4252 -0.0259 0.043 Uiso 1 1 calc R . . C99 C -0.0500(4) 0.4523(4) 0.0238(3) 0.036(2) Uani 1 1 d . . . C100 C -0.0757(4) 0.5008(4) 0.0470(3) 0.033(2) Uani 1 1 d . . . C101 C -0.1245(4) 0.5223(4) 0.0286(3) 0.035(2) Uani 1 1 d . . . H10A H -0.1441 0.5047 0.0003 0.042 Uiso 1 1 calc R . . C102 C -0.1456(4) 0.5695(4) 0.0508(3) 0.037(2) Uani 1 1 d . . . C103 C -0.1146(4) 0.5928(4) 0.0928(3) 0.044(3) Uani 1 1 d . . . H10B H -0.1275 0.6243 0.1102 0.053 Uiso 1 1 calc R . . C104 C -0.0652(4) 0.5692(4) 0.1087(3) 0.039(2) Uani 1 1 d . . . H10C H -0.0446 0.5858 0.1367 0.046 Uiso 1 1 calc R . . C105 C -0.0820(4) 0.3261(4) -0.0694(4) 0.045(3) Uani 1 1 d . . . C106 C -0.0980(5) 0.2752(4) -0.0379(4) 0.073(4) Uani 1 1 d . . . H10D H -0.1139 0.2433 -0.0592 0.109 Uiso 1 1 calc R . . H10E H -0.1235 0.2896 -0.0179 0.109 Uiso 1 1 calc R . . H10F H -0.0668 0.2601 -0.0167 0.109 Uiso 1 1 calc R . . C107 C -0.0467(4) 0.3017(4) -0.1047(3) 0.053(3) Uani 1 1 d . . . H10G H -0.0289 0.3345 -0.1184 0.079 Uiso 1 1 calc R . . H10H H -0.0683 0.2801 -0.1312 0.079 Uiso 1 1 calc R . . H10I H -0.0204 0.2750 -0.0871 0.079 Uiso 1 1 calc R . . C108 C -0.1305(4) 0.3515(4) -0.0981(4) 0.054(3) Uani 1 1 d . . . H10J H -0.1218 0.3886 -0.1132 0.082 Uiso 1 1 calc R . . H10K H -0.1564 0.3591 -0.0764 0.082 Uiso 1 1 calc R . . H10L H -0.1451 0.3236 -0.1235 0.082 Uiso 1 1 calc R . . C109 C -0.2000(4) 0.5936(4) 0.0326(3) 0.042(2) Uani 1 1 d . . . C110 C -0.2135(4) 0.5864(6) -0.0232(4) 0.070(4) Uani 1 1 d . . . H11A H -0.1868 0.6063 -0.0389 0.105 Uiso 1 1 calc R . . H11B H -0.2480 0.6041 -0.0345 0.105 Uiso 1 1 calc R . . H11C H -0.2144 0.5444 -0.0315 0.105 Uiso 1 1 calc R . . C111 C -0.2064(4) 0.6590(4) 0.0449(4) 0.063(3) Uani 1 1 d . . . H11D H -0.1804 0.6826 0.0311 0.094 Uiso 1 1 calc R . . H11E H -0.2012 0.6641 0.0804 0.094 Uiso 1 1 calc R . . H11F H -0.2419 0.6722 0.0311 0.094 Uiso 1 1 calc R . . C112 C -0.2397(4) 0.5584(4) 0.0576(4) 0.051(3) Uani 1 1 d . . . H11G H -0.2284 0.5587 0.0930 0.077 Uiso 1 1 calc R . . H11H H -0.2413 0.5176 0.0458 0.077 Uiso 1 1 calc R . . H11I H -0.2745 0.5765 0.0500 0.077 Uiso 1 1 calc R . . C113 C 0.3414(5) 0.0275(5) 0.7056(4) 0.070(4) Uani 1 1 d . . . H11J H 0.3399 0.0480 0.7368 0.084 Uiso 1 1 calc R . . H11K H 0.3666 0.0490 0.6885 0.084 Uiso 1 1 calc R . . Cl1 Cl 0.27913(12) 0.02907(11) 0.66987(10) 0.0602(8) Uani 1 1 d . . . Cl2 Cl 0.36427(12) -0.04561(13) 0.71780(12) 0.0734(9) Uani 1 1 d . . . C114 C 0.0545(4) 1.0110(4) 0.2575(4) 0.054(3) Uani 1 1 d . . . H11L H 0.0319 1.0309 0.2783 0.065 Uiso 1 1 calc R . . H11M H 0.0418 1.0223 0.2232 0.065 Uiso 1 1 calc R . . Cl3 Cl 0.04840(13) 0.93470(13) 0.26345(10) 0.0706(9) Uani 1 1 d . . . Cl4 Cl 0.11942(12) 1.03549(14) 0.27391(12) 0.0759(9) Uani 1 1 d . . . C115 C 0.9256(5) 0.2505(5) 0.4317(4) 0.082(4) Uani 1 1 d . . . H11N H 0.9413 0.2321 0.4050 0.099 Uiso 1 1 calc R . . H11O H 0.9006 0.2811 0.4171 0.099 Uiso 1 1 calc R . . Cl5 Cl 0.89056(17) 0.19567(16) 0.45972(13) 0.1026(13) Uani 1 1 d . . . Cl6 Cl 0.97470(16) 0.28385(18) 0.47174(13) 0.1029(12) Uani 1 1 d . . . C116 C 0.9325(4) 0.7582(4) 0.2022(4) 0.053(3) Uani 1 1 d . . . H11P H 0.9096 0.7652 0.1706 0.064 Uiso 1 1 calc R . . H11Q H 0.9124 0.7686 0.2286 0.064 Uiso 1 1 calc R . . Cl7 Cl 0.98794(13) 0.80330(14) 0.20615(12) 0.0780(9) Uani 1 1 d . . . Cl8 Cl 0.95043(14) 0.68265(13) 0.20699(13) 0.0871(11) Uani 1 1 d . . . C117 C 0.4705(7) 0.2406(8) 0.7639(7) 0.152(7) Uiso 1 1 d . . . H11R H 0.4883 0.2767 0.7783 0.183 Uiso 1 1 calc R . . H11S H 0.4566 0.2204 0.7908 0.183 Uiso 1 1 calc R . . Cl9 Cl 0.51671(14) 0.19858(14) 0.75026(13) 0.0836(10) Uani 1 1 d . . . Cl10 Cl 0.41635(13) 0.26478(14) 0.72464(13) 0.0870(11) Uani 1 1 d . . . C118 C 0.1298(12) 0.4285(13) 0.2690(10) 0.285(15) Uiso 1 1 d . . . H11T H 0.1467 0.4563 0.2487 0.342 Uiso 0.50 1 calc PR A 1 H11U H 0.0930 0.4233 0.2528 0.342 Uiso 0.50 1 calc PR A 1 H11V H 0.0950 0.4220 0.2763 0.342 Uiso 0.50 1 d PR A 2 H11W H 0.1258 0.4406 0.2354 0.342 Uiso 0.50 1 d PR A 2 Cl11 Cl 0.15959(18) 0.36401(19) 0.26738(18) 0.1242(15) Uani 1 1 d . B . Cl1A Cl 0.1282(3) 0.4594(4) 0.3197(3) 0.111(3) Uiso 0.50 1 d P B 1 Cl1B Cl 0.1564(4) 0.4893(4) 0.2986(3) 0.120(3) Uiso 0.50 1 d P B 2 C119 C -0.3355(8) 0.6598(9) -0.1712(8) 0.188(9) Uiso 1 1 d D . . H11X H -0.3313 0.6163 -0.1695 0.226 Uiso 0.67 1 calc PR C 1 H11Y H -0.3734 0.6693 -0.1793 0.226 Uiso 0.67 1 calc PR C 1 H11Z H -0.3277 0.6821 -0.1998 0.226 Uiso 0.33 1 calc PR C 2 H11' H -0.3740 0.6542 -0.1735 0.226 Uiso 0.33 1 calc PR C 2 Cl12 Cl -0.3091(3) 0.6913(3) -0.1185(3) 0.214(3) Uiso 1 1 d . D . Cl2A Cl -0.3020(6) 0.6885(7) -0.2120(6) 0.230(8) Uiso 0.67 1 d PD D 1 Cl2B Cl -0.2996(9) 0.5898(10) -0.1631(8) 0.233(10) Uiso 0.33 1 d PD D 2 C120 C -0.2277(9) 0.4880(9) -0.1927(8) 0.189(9) Uiso 1 1 d . . . H12B H -0.2376 0.4982 -0.2276 0.227 Uiso 0.67 1 calc PR E 1 H12C H -0.1893 0.4931 -0.1831 0.227 Uiso 0.67 1 calc PR E 1 H12D H -0.1918 0.5050 -0.1879 0.227 Uiso 0.33 1 d PR E 2 H12E H -0.2535 0.5202 -0.2004 0.227 Uiso 0.33 1 d PR E 2 Cl3A Cl -0.2638(3) 0.5306(4) -0.1549(3) 0.148(3) Uiso 0.67 1 d P F 1 Cl3B Cl -0.2476(4) 0.4166(4) -0.1804(3) 0.166(3) Uiso 0.67 1 d P F 1 Cl4A Cl -0.2366(7) 0.4446(8) -0.1402(6) 0.157(6) Uiso 0.33 1 d P F 2 Cl4B Cl -0.2320(7) 0.4368(8) -0.2360(7) 0.176(7) Uiso 0.33 1 d P F 2 C121 C 0.1091(11) 0.7069(12) 0.2500(9) 0.36(2) Uiso 1 1 d D . . H12F H 0.0766 0.7018 0.2262 0.436 Uiso 0.67 1 calc PR G 1 H12G H 0.1206 0.7485 0.2491 0.436 Uiso 0.67 1 calc PR G 1 H12H H 0.0839 0.6870 0.2246 0.436 Uiso 0.33 1 calc PR G 2 H12I H 0.0884 0.7298 0.2707 0.436 Uiso 0.33 1 calc PR G 2 Cl5A Cl 0.0985(6) 0.6893(7) 0.3059(5) 0.290(6) Uiso 0.67 1 d PD H 1 Cl5B Cl 0.1531(6) 0.6646(6) 0.2376(5) 0.278(6) Uiso 0.67 1 d PD H 1 Cl6A Cl 0.1478(11) 0.6482(11) 0.2894(11) 0.291(13) Uiso 0.33 1 d PD H 2 Cl6B Cl 0.1438(11) 0.7524(11) 0.2236(11) 0.278(6) Uiso 0.33 1 d PD H 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 0.0319(2) 0.02521(19) 0.02711(19) 0.00331(16) 0.00777(16) -0.00107(15) Pt2 0.0282(2) 0.02318(19) 0.0342(2) 0.00144(16) 0.00991(16) 0.00043(15) Zn1 0.0296(6) 0.0290(6) 0.0321(6) 0.0024(5) 0.0085(5) 0.0012(4) Zn2 0.0363(6) 0.0271(6) 0.0297(6) 0.0013(5) 0.0057(5) -0.0044(5) I1 0.0385(4) 0.0381(4) 0.0408(4) -0.0041(3) 0.0029(3) 0.0011(3) I2 0.0334(3) 0.0394(4) 0.0405(4) 0.0023(3) 0.0076(3) 0.0099(3) I3 0.0354(4) 0.0452(4) 0.0589(4) 0.0090(3) -0.0013(3) -0.0013(3) I4 0.0627(5) 0.0377(4) 0.0374(4) -0.0091(3) 0.0108(3) -0.0089(3) S1 0.0328(13) 0.0288(13) 0.0408(14) 0.0070(11) 0.0019(11) -0.0012(10) S2 0.0272(13) 0.0350(13) 0.0359(13) 0.0058(11) 0.0112(11) 0.0007(10) S3 0.0441(15) 0.0280(13) 0.0346(13) 0.0070(11) 0.0124(12) 0.0076(11) S4 0.0316(13) 0.0237(12) 0.0580(16) 0.0017(12) 0.0124(12) -0.0004(10) N1 0.028(4) 0.029(4) 0.021(4) 0.001(3) 0.008(3) 0.003(3) N2 0.022(4) 0.032(4) 0.032(4) 0.002(3) 0.004(3) 0.002(3) N3 0.027(4) 0.027(4) 0.036(4) -0.003(4) 0.008(4) -0.010(3) N4 0.037(5) 0.024(4) 0.025(4) -0.003(3) 0.004(3) -0.002(3) N5 0.026(4) 0.028(4) 0.027(4) 0.000(3) 0.004(3) -0.009(3) N6 0.031(4) 0.030(4) 0.030(4) 0.004(4) 0.004(4) -0.005(3) N7 0.025(4) 0.030(4) 0.031(4) -0.002(4) 0.009(3) -0.005(3) N8 0.029(4) 0.029(4) 0.033(4) -0.003(4) 0.009(4) 0.000(3) C1 0.038(6) 0.031(5) 0.026(5) -0.003(4) 0.009(4) 0.001(4) C2 0.034(5) 0.026(5) 0.027(5) -0.002(4) 0.010(4) -0.004(4) C3 0.026(5) 0.031(5) 0.026(5) 0.002(4) 0.009(4) 0.004(4) C4 0.031(5) 0.038(6) 0.021(5) 0.003(4) 0.007(4) -0.003(4) C5 0.021(5) 0.033(5) 0.034(5) -0.003(4) 0.002(4) -0.006(4) C6 0.026(5) 0.029(5) 0.037(6) 0.002(4) 0.006(5) -0.003(4) C7 0.040(6) 0.029(5) 0.025(5) -0.006(4) 0.005(4) -0.001(4) C8 0.027(5) 0.015(4) 0.035(5) -0.001(4) 0.014(4) 0.007(4) C9 0.026(5) 0.052(6) 0.039(6) 0.009(5) 0.007(5) 0.006(4) C10 0.044(6) 0.051(6) 0.028(5) 0.012(5) 0.007(5) 0.011(5) C11 0.038(6) 0.025(5) 0.031(5) -0.005(4) 0.014(4) 0.003(4) C12 0.041(6) 0.013(5) 0.058(7) 0.001(5) 0.017(5) -0.001(4) C13 0.030(5) 0.023(5) 0.031(5) -0.006(4) 0.013(4) -0.002(4) C14 0.055(6) 0.022(5) 0.027(5) -0.005(4) 0.012(5) 0.002(4) C15 0.052(6) 0.014(5) 0.042(6) -0.004(4) 0.009(5) 0.002(4) C16 0.039(6) 0.015(5) 0.040(6) 0.002(4) 0.011(5) 0.006(4) C17 0.025(5) 0.029(5) 0.037(5) 0.003(4) 0.006(4) 0.005(4) C18 0.021(5) 0.023(5) 0.028(5) 0.000(4) 0.005(4) -0.005(4) C19 0.032(5) 0.023(5) 0.031(5) -0.004(4) 0.010(4) -0.003(4) C20 0.032(5) 0.022(5) 0.035(5) 0.002(4) 0.010(4) 0.005(4) C21 0.049(7) 0.037(6) 0.029(5) -0.001(5) 0.017(5) 0.001(5) C22 0.065(8) 0.031(6) 0.032(6) 0.001(5) 0.006(5) -0.021(5) C23 0.040(6) 0.030(5) 0.034(5) 0.004(4) 0.003(5) -0.010(4) C24 0.039(6) 0.037(6) 0.032(5) 0.003(5) 0.013(5) -0.002(4) C25 0.035(6) 0.031(5) 0.028(5) 0.001(4) 0.011(4) 0.002(4) C26 0.037(6) 0.023(5) 0.021(5) 0.007(4) 0.005(4) 0.000(4) C27 0.028(5) 0.034(5) 0.026(5) 0.002(4) 0.009(4) -0.001(4) C28 0.045(6) 0.033(5) 0.027(5) 0.008(4) 0.012(5) 0.005(5) C29 0.054(7) 0.033(5) 0.019(5) -0.002(4) 0.005(5) 0.006(5) C30 0.034(6) 0.039(6) 0.028(5) -0.002(5) 0.002(4) -0.003(4) C31 0.037(6) 0.047(7) 0.056(7) -0.003(5) 0.003(5) -0.016(5) C32 0.059(9) 0.205(17) 0.052(8) -0.004(10) 0.003(7) -0.046(10) C33 0.089(11) 0.065(9) 0.170(16) 0.017(10) 0.026(11) -0.032(8) C34 0.046(7) 0.082(9) 0.062(8) -0.017(7) 0.001(6) -0.021(6) C35 0.043(6) 0.048(6) 0.035(6) 0.011(5) 0.019(5) 0.012(5) C36 0.059(8) 0.080(8) 0.036(6) -0.015(6) 0.015(6) 0.026(6) C37 0.065(7) 0.041(6) 0.042(6) -0.009(5) 0.020(6) 0.007(5) C38 0.087(9) 0.056(7) 0.053(7) 0.016(6) 0.026(7) 0.035(6) C39 0.043(6) 0.028(5) 0.037(6) 0.000(5) 0.018(5) -0.002(4) C40 0.043(6) 0.043(6) 0.037(6) -0.007(5) 0.007(5) -0.011(5) C41 0.048(6) 0.044(6) 0.034(6) -0.001(5) 0.003(5) -0.002(5) C42 0.051(7) 0.034(6) 0.033(6) 0.004(5) 0.005(5) -0.001(5) C43 0.038(6) 0.020(5) 0.037(6) 0.001(4) 0.015(5) 0.004(4) C44 0.024(5) 0.031(5) 0.031(5) 0.002(4) 0.006(4) 0.005(4) C45 0.042(6) 0.027(5) 0.028(5) 0.007(4) 0.007(4) -0.003(4) C46 0.028(5) 0.023(5) 0.042(6) 0.004(4) 0.009(5) 0.000(4) C47 0.031(5) 0.033(6) 0.040(6) -0.009(5) 0.010(5) -0.003(4) C48 0.030(5) 0.030(5) 0.039(6) 0.001(5) 0.006(4) 0.008(4) C49 0.087(9) 0.054(7) 0.036(6) -0.010(6) -0.011(6) -0.002(6) C50 0.066(9) 0.075(9) 0.078(9) 0.014(7) -0.013(7) -0.005(7) C51 0.094(10) 0.092(10) 0.035(7) 0.016(7) -0.001(7) -0.009(8) C52 0.159(15) 0.082(10) 0.045(8) -0.016(7) -0.037(8) -0.001(9) C53 0.035(6) 0.027(5) 0.050(6) 0.012(5) 0.018(5) 0.001(4) C54 0.049(7) 0.043(7) 0.073(8) 0.005(6) -0.002(6) -0.008(5) C55 0.056(7) 0.035(6) 0.064(7) 0.016(5) 0.017(6) 0.004(5) C56 0.054(7) 0.033(6) 0.060(7) 0.004(5) 0.005(6) 0.009(5) Pt3 0.0292(2) 0.0347(2) 0.0307(2) 0.00245(17) 0.00084(16) -0.00378(16) Pt4 0.0327(2) 0.0337(2) 0.0387(2) 0.00588(18) 0.01018(18) -0.00396(16) Zn3 0.0338(6) 0.0296(6) 0.0386(6) -0.0006(5) 0.0041(5) -0.0007(5) Zn4 0.0417(7) 0.0370(6) 0.0311(6) -0.0022(5) 0.0050(5) 0.0017(5) I5 0.0635(5) 0.0448(4) 0.0639(5) -0.0118(4) 0.0165(4) 0.0136(4) I6 0.0422(4) 0.0469(4) 0.0507(4) 0.0092(3) -0.0003(3) -0.0172(3) I7 0.0467(4) 0.0419(4) 0.0440(4) -0.0037(3) -0.0004(3) -0.0068(3) I8 0.0533(5) 0.0604(5) 0.0543(5) -0.0141(4) 0.0109(4) 0.0113(4) S5 0.0334(14) 0.0370(14) 0.0538(16) 0.0088(12) -0.0022(12) -0.0055(11) S6 0.0438(15) 0.0385(15) 0.0462(15) 0.0031(12) 0.0084(13) -0.0122(12) S7 0.0373(15) 0.0650(18) 0.0322(14) -0.0022(13) 0.0027(12) -0.0188(13) S8 0.0328(14) 0.0425(15) 0.0580(17) 0.0119(13) 0.0124(13) -0.0047(12) N9 0.041(5) 0.023(4) 0.038(5) -0.010(4) 0.006(4) 0.000(4) N10 0.041(5) 0.028(4) 0.040(5) -0.002(4) 0.007(4) -0.002(4) N11 0.045(5) 0.035(5) 0.027(4) 0.001(4) 0.012(4) -0.002(4) N12 0.036(5) 0.046(5) 0.028(4) -0.004(4) 0.005(4) -0.004(4) N13 0.029(4) 0.042(5) 0.024(4) -0.002(4) 0.003(4) 0.004(3) N14 0.027(4) 0.035(5) 0.038(5) 0.004(4) 0.007(4) 0.008(3) N15 0.028(4) 0.033(4) 0.032(4) 0.004(4) 0.009(4) 0.002(3) N16 0.042(5) 0.028(4) 0.034(5) 0.002(4) 0.008(4) -0.003(4) C57 0.086(10) 0.075(9) 0.066(8) -0.029(7) -0.056(7) 0.035(7) C58 0.103(10) 0.065(8) 0.059(8) -0.037(6) -0.045(7) 0.052(7) C59 0.040(6) 0.039(6) 0.030(5) 0.011(5) 0.002(5) -0.008(5) C60 0.047(7) 0.046(7) 0.060(7) -0.029(6) -0.013(6) 0.005(5) C61 0.042(7) 0.050(7) 0.064(7) -0.035(6) -0.007(6) 0.003(5) C62 0.037(6) 0.025(5) 0.044(6) -0.002(5) 0.009(5) -0.007(4) C63 0.040(6) 0.027(5) 0.034(5) -0.001(4) 0.008(5) -0.001(4) C64 0.032(5) 0.025(5) 0.041(6) 0.003(4) -0.001(4) 0.003(4) C65 0.044(6) 0.031(6) 0.049(6) 0.003(5) 0.007(5) -0.006(5) C66 0.055(7) 0.028(5) 0.038(6) -0.005(5) 0.011(5) -0.010(5) C67 0.032(6) 0.054(7) 0.047(7) 0.006(5) 0.008(5) -0.018(5) C68 0.037(6) 0.059(7) 0.031(6) -0.005(5) 0.004(5) -0.017(5) C69 0.028(5) 0.037(6) 0.034(5) -0.001(4) -0.002(4) -0.009(4) C70 0.032(6) 0.043(6) 0.033(6) 0.004(5) 0.006(5) -0.003(4) C71 0.041(6) 0.036(6) 0.038(6) -0.002(5) 0.001(5) -0.004(4) C72 0.029(6) 0.045(6) 0.041(6) 0.006(5) 0.002(5) 0.008(5) C73 0.028(5) 0.046(6) 0.040(6) 0.008(5) 0.010(5) -0.005(4) C74 0.026(5) 0.043(6) 0.032(5) 0.008(4) 0.007(4) -0.004(4) C75 0.035(6) 0.048(6) 0.038(6) 0.005(5) 0.018(5) 0.006(5) C76 0.038(6) 0.038(6) 0.036(6) 0.001(5) 0.012(5) -0.005(5) C77 0.033(5) 0.039(6) 0.031(5) -0.002(5) 0.005(4) -0.002(4) C78 0.030(5) 0.039(6) 0.029(5) -0.012(4) -0.001(4) 0.006(4) C79 0.030(5) 0.030(5) 0.033(5) -0.003(4) -0.001(4) -0.001(4) C80 0.030(5) 0.029(5) 0.029(5) 0.000(4) 0.001(4) 0.003(4) C81 0.035(5) 0.027(5) 0.025(5) 0.001(4) -0.001(4) 0.004(4) C82 0.030(5) 0.026(5) 0.024(5) 0.000(4) -0.005(4) -0.002(4) C83 0.033(5) 0.025(5) 0.029(5) 0.002(4) 0.004(4) 0.000(4) C84 0.037(6) 0.028(5) 0.034(5) -0.002(4) 0.006(4) 0.002(4) C85 0.050(6) 0.035(6) 0.040(6) -0.011(5) 0.011(5) -0.002(5) C86 0.044(6) 0.034(6) 0.043(6) -0.006(5) 0.007(5) 0.000(5) C87 0.029(5) 0.035(6) 0.037(5) 0.000(4) 0.009(4) 0.003(4) C88 0.084(9) 0.044(7) 0.049(7) -0.014(5) 0.003(6) -0.021(6) C89 0.064(8) 0.031(6) 0.087(9) 0.006(6) 0.000(7) 0.005(5) C90 0.055(7) 0.037(6) 0.064(7) -0.010(5) 0.018(6) -0.014(5) C91 0.046(6) 0.034(5) 0.027(5) -0.005(4) 0.020(5) -0.007(4) C92 0.051(7) 0.056(7) 0.043(6) 0.016(5) 0.014(5) 0.011(5) C93 0.141(13) 0.056(8) 0.061(8) -0.032(6) 0.058(8) -0.041(8) C94 0.044(7) 0.078(8) 0.057(7) 0.014(6) 0.027(6) 0.015(6) C95 0.041(6) 0.048(6) 0.031(6) 0.012(5) 0.019(5) 0.002(5) C96 0.048(7) 0.037(6) 0.038(6) 0.006(5) 0.028(5) 0.004(5) C97 0.051(7) 0.037(6) 0.034(6) 0.006(5) 0.019(5) -0.008(5) C98 0.041(6) 0.029(5) 0.038(6) 0.003(5) 0.009(5) 0.004(4) C99 0.044(6) 0.031(5) 0.036(6) 0.011(5) 0.015(5) 0.000(5) C100 0.035(6) 0.032(5) 0.037(6) 0.010(4) 0.018(5) -0.005(4) C101 0.045(6) 0.035(6) 0.026(5) 0.004(4) 0.012(5) -0.004(5) C102 0.038(6) 0.040(6) 0.035(6) 0.007(5) 0.009(5) -0.003(5) C103 0.049(7) 0.042(6) 0.043(6) -0.009(5) 0.012(5) 0.003(5) C104 0.037(6) 0.041(6) 0.038(6) -0.004(5) 0.003(5) -0.002(5) C105 0.052(7) 0.043(6) 0.043(6) -0.001(5) 0.017(6) -0.004(5) C106 0.117(11) 0.043(7) 0.065(8) -0.022(6) 0.039(8) -0.032(7) C107 0.075(8) 0.047(7) 0.041(6) -0.005(5) 0.021(6) 0.008(6) C108 0.060(8) 0.059(7) 0.051(7) -0.010(6) 0.028(6) -0.015(6) C109 0.048(6) 0.038(6) 0.040(6) 0.001(5) 0.010(5) -0.005(5) C110 0.040(7) 0.122(11) 0.051(7) 0.018(7) 0.014(6) 0.021(7) C111 0.058(8) 0.043(7) 0.089(9) 0.021(6) 0.015(7) 0.006(6) C112 0.042(6) 0.054(7) 0.060(7) 0.002(6) 0.014(6) -0.002(5) C113 0.080(9) 0.058(8) 0.070(8) -0.015(6) 0.003(7) -0.036(7) Cl1 0.077(2) 0.0403(16) 0.0621(18) -0.0070(14) 0.0092(16) -0.0194(14) Cl2 0.069(2) 0.062(2) 0.085(2) 0.0088(17) -0.0015(18) -0.0258(16) C114 0.047(7) 0.060(7) 0.055(7) 0.007(6) 0.003(6) 0.006(5) Cl3 0.093(2) 0.069(2) 0.0503(18) -0.0043(15) 0.0120(17) -0.0235(17) Cl4 0.063(2) 0.069(2) 0.096(2) 0.0083(18) 0.0119(19) -0.0090(16) C115 0.107(11) 0.095(10) 0.042(7) 0.000(7) 0.007(7) 0.036(8) Cl5 0.152(4) 0.083(3) 0.072(2) 0.020(2) 0.018(2) 0.026(2) Cl6 0.114(3) 0.118(3) 0.068(2) -0.001(2) -0.012(2) 0.016(2) C116 0.044(6) 0.060(7) 0.055(7) 0.004(6) 0.006(6) 0.005(5) Cl7 0.079(2) 0.073(2) 0.081(2) 0.0083(18) 0.0110(19) -0.0256(18) Cl8 0.102(3) 0.0490(19) 0.108(3) -0.0261(19) 0.010(2) 0.0077(18) Cl9 0.095(3) 0.061(2) 0.098(3) 0.0060(19) 0.024(2) 0.0029(18) Cl10 0.079(2) 0.073(2) 0.103(3) -0.032(2) -0.003(2) 0.0071(18) Cl11 0.113(3) 0.094(3) 0.158(4) -0.016(3) -0.006(3) -0.008(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 N6 2.063(7) . ? Pt1 N5 2.068(7) . ? Pt1 S1 2.290(2) . ? Pt1 S3 2.294(2) . ? Pt2 N7 2.047(7) . ? Pt2 N8 2.063(7) . ? Pt2 S4 2.282(2) . ? Pt2 S2 2.287(2) . ? Zn1 N2 2.026(7) . ? Zn1 N1 2.046(7) . ? Zn1 I1 2.5425(12) . ? Zn1 I2 2.5647(12) . ? Zn2 N3 2.051(7) . ? Zn2 N4 2.061(7) . ? Zn2 I4 2.5691(11) . ? Zn2 I3 2.5711(12) . ? S1 C3 1.741(8) . ? S2 C8 1.747(8) . ? S3 C13 1.761(9) . ? S4 C18 1.722(8) . ? N1 C5 1.324(10) . ? N1 C1 1.359(10) . ? N2 C6 1.337(10) . ? N2 C10 1.347(11) . ? N3 C15 1.333(10) . ? N3 C11 1.352(10) . ? N4 C20 1.350(10) . ? N4 C16 1.354(10) . ? N5 C21 1.326(10) . ? N5 C25 1.364(10) . ? N6 C30 1.349(10) . ? N6 C26 1.351(10) . ? N7 C43 1.358(10) . ? N7 C39 1.364(10) . ? N8 C48 1.351(10) . ? N8 C44 1.371(10) . ? C1 C2 1.386(11) . ? C2 C3 1.377(11) . ? C3 C4 1.395(11) . ? C4 C5 1.374(11) . ? C6 C7 1.381(11) . ? C7 C8 1.379(11) . ? C8 C9 1.406(12) . ? C9 C10 1.374(11) . ? C11 C12 1.383(11) . ? C12 C13 1.370(11) . ? C13 C14 1.381(11) . ? C14 C15 1.383(11) . ? C16 C17 1.333(11) . ? C17 C18 1.411(11) . ? C18 C19 1.402(11) . ? C19 C20 1.361(11) . ? C21 C22 1.375(12) . ? C22 C23 1.387(13) . ? C23 C24 1.380(12) . ? C23 C31 1.514(12) . ? C24 C25 1.368(12) . ? C25 C26 1.490(11) . ? C26 C27 1.376(11) . ? C27 C28 1.386(11) . ? C28 C29 1.375(12) . ? C28 C35 1.536(12) . ? C29 C30 1.402(11) . ? C31 C33 1.492(14) . ? C31 C34 1.516(13) . ? C31 C32 1.547(14) . ? C35 C36 1.512(13) . ? C35 C37 1.532(12) . ? C35 C38 1.527(12) . ? C39 C40 1.380(12) . ? C40 C41 1.398(13) . ? C41 C42 1.395(12) . ? C41 C49 1.526(13) . ? C42 C43 1.368(12) . ? C43 C44 1.464(11) . ? C44 C45 1.393(11) . ? C45 C46 1.392(11) . ? C46 C47 1.371(12) . ? C46 C53 1.525(11) . ? C47 C48 1.354(11) . ? C49 C52 1.516(14) . ? C49 C50 1.527(15) . ? C49 C51 1.544(14) . ? C53 C56 1.517(12) . ? C53 C55 1.524(12) . ? C53 C54 1.537(13) . ? Pt3 N13 2.028(7) . ? Pt3 N14 2.060(7) . ? Pt3 S7 2.281(2) . ? Pt3 S5 2.300(2) . ? Pt4 N16 2.047(7) . ? Pt4 N15 2.062(7) . ? Pt4 S8 2.289(2) . ? Pt4 S6 2.295(3) . ? Zn3 N9 2.032(7) . ? Zn3 N10 2.046(7) . ? Zn3 I5 2.5498(12) . ? Zn3 I6 2.5675(12) . ? Zn4 N11 2.034(7) . ? Zn4 N12 2.055(7) . ? Zn4 I7 2.5550(13) . ? Zn4 I8 2.5683(12) . ? S5 C59 1.742(9) . ? S6 C64 1.723(9) . ? S7 C69 1.733(9) . ? S8 C74 1.729(9) . ? N9 C57 1.283(12) . ? N9 C61 1.299(11) . ? N10 C62 1.333(10) . ? N10 C66 1.346(10) . ? N11 C67 1.327(11) . ? N11 C71 1.344(10) . ? N12 C76 1.324(11) . ? N12 C72 1.337(11) . ? N13 C77 1.333(10) . ? N13 C81 1.376(10) . ? N14 C86 1.339(10) . ? N14 C82 1.368(10) . ? N15 C95 1.335(10) . ? N15 C99 1.340(11) . ? N16 C104 1.327(10) . ? N16 C100 1.354(11) . ? C57 C58 1.393(14) . ? C58 C59 1.357(13) . ? C59 C60 1.358(12) . ? C60 C61 1.372(13) . ? C62 C63 1.336(11) . ? C63 C64 1.395(11) . ? C64 C65 1.384(12) . ? C65 C66 1.387(12) . ? C67 C68 1.380(12) . ? C68 C69 1.398(12) . ? C69 C70 1.387(11) . ? C70 C71 1.380(12) . ? C72 C73 1.364(12) . ? C73 C74 1.408(12) . ? C74 C75 1.382(11) . ? C75 C76 1.376(12) . ? C77 C78 1.380(11) . ? C78 C79 1.414(11) . ? C79 C80 1.401(11) . ? C79 C87 1.519(11) . ? C80 C81 1.404(11) . ? C81 C82 1.480(11) . ? C82 C83 1.382(11) . ? C83 C84 1.405(11) . ? C84 C85 1.391(12) . ? C84 C91 1.503(11) . ? C85 C86 1.359(12) . ? C87 C90 1.507(12) . ? C87 C89 1.533(12) . ? C87 C88 1.533(12) . ? C91 C94 1.534(13) . ? C91 C93 1.528(12) . ? C91 C92 1.528(12) . ? C95 C96 1.383(12) . ? C96 C97 1.387(13) . ? C97 C98 1.385(12) . ? C97 C105 1.561(13) . ? C98 C99 1.405(12) . ? C99 C100 1.481(12) . ? C100 C101 1.371(12) . ? C101 C102 1.387(12) . ? C102 C103 1.409(12) . ? C102 C109 1.513(13) . ? C103 C104 1.386(12) . ? C105 C108 1.488(14) . ? C105 C106 1.542(13) . ? C105 C107 1.542(12) . ? C109 C111 1.537(13) . ? C109 C110 1.542(13) . ? C109 C112 1.545(12) . ? C113 Cl1 1.750(11) . ? C113 Cl2 1.772(11) . ? C114 Cl3 1.745(10) . ? C114 Cl4 1.754(10) . ? C115 Cl6 1.721(13) . ? C115 Cl5 1.784(13) . ? C116 Cl7 1.744(10) . ? C116 Cl8 1.773(10) . ? C117 Cl9 1.614(17) . ? C117 Cl10 1.721(18) . ? C118 Cl1A 1.58(3) . ? C118 Cl11 1.65(3) . ? C118 Cl1B 1.69(3) . ? C119 Cl2A 1.659(15) . ? C119 Cl12 1.67(2) . ? C119 Cl2B 1.831(17) . ? C120 Cl4B 1.66(2) . ? C120 Cl3B 1.75(2) . ? C120 Cl3A 1.79(2) . ? C120 Cl4A 1.80(2) . ? C121 Cl5B 1.564(17) . ? C121 Cl6B 1.613(18) . ? C121 Cl5A 1.664(17) . ? C121 Cl6A 1.902(18) . ? 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 N6 Pt1 N5 78.8(3) . . ? N6 Pt1 S1 97.8(2) . . ? N5 Pt1 S1 174.30(19) . . ? N6 Pt1 S3 173.3(2) . . ? N5 Pt1 S3 94.5(2) . . ? S1 Pt1 S3 88.87(9) . . ? N7 Pt2 N8 78.7(3) . . ? N7 Pt2 S4 97.8(2) . . ? N8 Pt2 S4 175.7(2) . . ? N7 Pt2 S2 172.85(19) . . ? N8 Pt2 S2 96.1(2) . . ? S4 Pt2 S2 87.26(9) . . ? N2 Zn1 N1 104.5(3) . . ? N2 Zn1 I1 106.6(2) . . ? N1 Zn1 I1 111.39(19) . . ? N2 Zn1 I2 107.1(2) . . ? N1 Zn1 I2 107.4(2) . . ? I1 Zn1 I2 118.80(4) . . ? N3 Zn2 N4 106.1(3) . . ? N3 Zn2 I4 106.9(2) . . ? N4 Zn2 I4 104.58(19) . . ? N3 Zn2 I3 107.2(2) . . ? N4 Zn2 I3 108.55(19) . . ? I4 Zn2 I3 122.51(5) . . ? C3 S1 Pt1 108.0(3) . . ? C8 S2 Pt2 107.7(3) . . ? C13 S3 Pt1 105.9(3) . . ? C18 S4 Pt2 110.3(3) . . ? C5 N1 C1 117.0(7) . . ? C5 N1 Zn1 123.1(6) . . ? C1 N1 Zn1 119.9(6) . . ? C6 N2 C10 116.5(7) . . ? C6 N2 Zn1 121.5(6) . . ? C10 N2 Zn1 121.7(6) . . ? C15 N3 C11 116.3(7) . . ? C15 N3 Zn2 121.2(6) . . ? C11 N3 Zn2 122.4(6) . . ? C20 N4 C16 115.0(7) . . ? C20 N4 Zn2 125.6(6) . . ? C16 N4 Zn2 119.2(5) . . ? C21 N5 C25 117.1(7) . . ? C21 N5 Pt1 127.0(6) . . ? C25 N5 Pt1 115.7(6) . . ? C30 N6 C26 117.6(7) . . ? C30 N6 Pt1 126.4(6) . . ? C26 N6 Pt1 115.5(6) . . ? C43 N7 C39 117.4(8) . . ? C43 N7 Pt2 116.6(6) . . ? C39 N7 Pt2 126.0(6) . . ? C48 N8 C44 117.8(7) . . ? C48 N8 Pt2 127.2(6) . . ? C44 N8 Pt2 114.9(5) . . ? N1 C1 C2 122.5(8) . . ? C3 C2 C1 120.1(8) . . ? C2 C3 C4 116.8(8) . . ? C2 C3 S1 124.7(7) . . ? C4 C3 S1 118.5(7) . . ? C5 C4 C3 120.0(8) . . ? N1 C5 C4 123.6(8) . . ? N2 C6 C7 123.8(8) . . ? C6 C7 C8 119.2(8) . . ? C7 C8 C9 118.0(8) . . ? C7 C8 S2 124.2(7) . . ? C9 C8 S2 117.8(6) . . ? C10 C9 C8 118.4(8) . . ? N2 C10 C9 124.0(9) . . ? N3 C11 C12 122.4(8) . . ? C13 C12 C11 120.7(8) . . ? C12 C13 C14 117.2(8) . . ? C12 C13 S3 118.1(7) . . ? C14 C13 S3 124.6(6) . . ? C13 C14 C15 119.2(8) . . ? N3 C15 C14 124.1(8) . . ? C17 C16 N4 124.7(8) . . ? C16 C17 C18 121.0(8) . . ? C19 C18 C17 114.5(7) . . ? C19 C18 S4 126.6(6) . . ? C17 C18 S4 118.9(6) . . ? C20 C19 C18 120.9(8) . . ? N4 C20 C19 123.8(8) . . ? N5 C21 C22 122.5(9) . . ? C21 C22 C23 121.6(9) . . ? C24 C23 C22 115.0(8) . . ? C24 C23 C31 122.5(9) . . ? C22 C23 C31 122.4(9) . . ? C25 C24 C23 121.8(9) . . ? N5 C25 C24 121.9(8) . . ? N5 C25 C26 114.0(8) . . ? C24 C25 C26 124.1(8) . . ? N6 C26 C27 122.3(8) . . ? N6 C26 C25 115.0(7) . . ? C27 C26 C25 122.7(8) . . ? C26 C27 C28 121.0(8) . . ? C29 C28 C27 116.6(8) . . ? C29 C28 C35 121.7(8) . . ? C27 C28 C35 121.5(9) . . ? C28 C29 C30 120.6(8) . . ? N6 C30 C29 121.8(8) . . ? C33 C31 C34 108.1(9) . . ? C33 C31 C23 109.4(9) . . ? C34 C31 C23 114.2(8) . . ? C33 C31 C32 110.9(11) . . ? C34 C31 C32 106.6(9) . . ? C23 C31 C32 107.5(8) . . ? C36 C35 C37 107.6(7) . . ? C36 C35 C38 109.8(9) . . ? C37 C35 C38 110.8(8) . . ? C36 C35 C28 111.7(8) . . ? C37 C35 C28 111.6(8) . . ? C38 C35 C28 105.5(7) . . ? N7 C39 C40 122.3(8) . . ? C39 C40 C41 120.7(9) . . ? C42 C41 C40 115.9(9) . . ? C42 C41 C49 121.0(9) . . ? C40 C41 C49 123.0(9) . . ? C43 C42 C41 121.7(9) . . ? N7 C43 C42 122.1(8) . . ? N7 C43 C44 114.2(8) . . ? C42 C43 C44 123.6(8) . . ? N8 C44 C45 120.3(8) . . ? N8 C44 C43 115.2(7) . . ? C45 C44 C43 124.5(8) . . ? C44 C45 C46 121.4(8) . . ? C47 C46 C45 115.6(8) . . ? C47 C46 C53 122.5(8) . . ? C45 C46 C53 121.9(8) . . ? C48 C47 C46 122.6(8) . . ? N8 C48 C47 122.1(8) . . ? C52 C49 C50 109.2(11) . . ? C52 C49 C41 111.4(9) . . ? C50 C49 C41 107.6(9) . . ? C52 C49 C51 107.7(10) . . ? C50 C49 C51 110.6(10) . . ? C41 C49 C51 110.3(9) . . ? C56 C53 C46 109.7(7) . . ? C56 C53 C55 109.0(8) . . ? C46 C53 C55 112.2(8) . . ? C56 C53 C54 107.5(8) . . ? C46 C53 C54 108.7(8) . . ? C55 C53 C54 109.6(7) . . ? N13 Pt3 N14 79.4(3) . . ? N13 Pt3 S7 98.0(2) . . ? N14 Pt3 S7 173.5(2) . . ? N13 Pt3 S5 173.6(2) . . ? N14 Pt3 S5 94.8(2) . . ? S7 Pt3 S5 88.07(9) . . ? N16 Pt4 N15 79.3(3) . . ? N16 Pt4 S8 173.4(2) . . ? N15 Pt4 S8 96.9(2) . . ? N16 Pt4 S6 96.1(2) . . ? N15 Pt4 S6 175.4(2) . . ? S8 Pt4 S6 87.72(9) . . ? N9 Zn3 N10 100.2(3) . . ? N9 Zn3 I5 107.7(2) . . ? N10 Zn3 I5 111.0(2) . . ? N9 Zn3 I6 109.1(2) . . ? N10 Zn3 I6 108.0(2) . . ? I5 Zn3 I6 119.14(5) . . ? N11 Zn4 N12 100.7(3) . . ? N11 Zn4 I7 112.4(2) . . ? N12 Zn4 I7 106.8(2) . . ? N11 Zn4 I8 106.7(2) . . ? N12 Zn4 I8 107.5(2) . . ? I7 Zn4 I8 120.84(5) . . ? C59 S5 Pt3 103.0(3) . . ? C64 S6 Pt4 108.8(3) . . ? C69 S7 Pt3 111.0(3) . . ? C74 S8 Pt4 108.1(3) . . ? C57 N9 C61 114.3(9) . . ? C57 N9 Zn3 121.2(7) . . ? C61 N9 Zn3 124.1(6) . . ? C62 N10 C66 115.9(8) . . ? C62 N10 Zn3 123.0(6) . . ? C66 N10 Zn3 120.9(6) . . ? C67 N11 C71 116.5(8) . . ? C67 N11 Zn4 119.7(6) . . ? C71 N11 Zn4 123.3(6) . . ? C76 N12 C72 116.7(8) . . ? C76 N12 Zn4 121.7(6) . . ? C72 N12 Zn4 121.0(6) . . ? C77 N13 C81 118.6(7) . . ? C77 N13 Pt3 125.5(6) . . ? C81 N13 Pt3 115.7(5) . . ? C86 N14 C82 118.1(7) . . ? C86 N14 Pt3 125.8(6) . . ? C82 N14 Pt3 116.0(6) . . ? C95 N15 C99 119.1(8) . . ? C95 N15 Pt4 126.0(6) . . ? C99 N15 Pt4 114.6(6) . . ? C104 N16 C100 117.7(8) . . ? C104 N16 Pt4 126.4(6) . . ? C100 N16 Pt4 115.7(6) . . ? N9 C57 C58 126.5(10) . . ? C59 C58 C57 118.6(10) . . ? C60 C59 C58 115.0(9) . . ? C60 C59 S5 121.3(7) . . ? C58 C59 S5 123.7(8) . . ? C59 C60 C61 121.5(9) . . ? N9 C61 C60 124.0(9) . . ? N10 C62 C63 124.6(8) . . ? C62 C63 C64 121.4(9) . . ? C65 C64 C63 114.7(8) . . ? C65 C64 S6 118.6(7) . . ? C63 C64 S6 126.8(7) . . ? C64 C65 C66 121.1(9) . . ? N10 C66 C65 122.3(8) . . ? N11 C67 C68 124.6(9) . . ? C67 C68 C69 118.8(9) . . ? C70 C69 C68 116.7(8) . . ? C70 C69 S7 126.6(7) . . ? C68 C69 S7 116.7(7) . . ? C71 C70 C69 120.3(9) . . ? N11 C71 C70 122.9(9) . . ? N12 C72 C73 123.9(9) . . ? C72 C73 C74 120.1(8) . . ? C75 C74 C73 114.9(8) . . ? C75 C74 S8 126.1(7) . . ? C73 C74 S8 119.1(7) . . ? C76 C75 C74 121.4(9) . . ? N12 C76 C75 123.0(9) . . ? N13 C77 C78 122.6(8) . . ? C77 C78 C79 121.3(8) . . ? C80 C79 C78 115.4(8) . . ? C80 C79 C87 124.4(8) . . ? C78 C79 C87 120.2(7) . . ? C79 C80 C81 121.2(8) . . ? N13 C81 C80 120.7(8) . . ? N13 C81 C82 115.1(7) . . ? C80 C81 C82 124.2(8) . . ? N14 C82 C83 121.2(8) . . ? N14 C82 C81 113.5(7) . . ? C83 C82 C81 125.2(8) . . ? C82 C83 C84 120.7(8) . . ? C85 C84 C83 115.7(8) . . ? C85 C84 C91 122.1(8) . . ? C83 C84 C91 122.1(8) . . ? C86 C85 C84 121.5(9) . . ? N14 C86 C85 122.7(9) . . ? C90 C87 C79 112.2(7) . . ? C90 C87 C89 109.9(8) . . ? C79 C87 C89 107.2(7) . . ? C90 C87 C88 109.1(8) . . ? C79 C87 C88 109.7(7) . . ? C89 C87 C88 108.6(8) . . ? C84 C91 C94 107.2(7) . . ? C84 C91 C93 112.7(7) . . ? C94 C91 C93 107.2(9) . . ? C84 C91 C92 112.3(7) . . ? C94 C91 C92 108.8(8) . . ? C93 C91 C92 108.6(8) . . ? N15 C95 C96 121.2(9) . . ? C95 C96 C97 121.5(9) . . ? C98 C97 C96 116.4(9) . . ? C98 C97 C105 121.4(9) . . ? C96 C97 C105 122.1(9) . . ? C97 C98 C99 119.8(9) . . ? N15 C99 C98 121.8(8) . . ? N15 C99 C100 115.8(8) . . ? C98 C99 C100 122.5(9) . . ? N16 C100 C101 122.7(8) . . ? N16 C100 C99 114.1(8) . . ? C101 C100 C99 123.1(9) . . ? C100 C101 C102 120.5(9) . . ? C101 C102 C103 116.5(9) . . ? C101 C102 C109 122.4(9) . . ? C103 C102 C109 121.1(8) . . ? C104 C103 C102 119.5(9) . . ? N16 C104 C103 123.1(9) . . ? C108 C105 C106 108.5(9) . . ? C108 C105 C107 109.1(8) . . ? C106 C105 C107 109.1(8) . . ? C108 C105 C97 113.0(8) . . ? C106 C105 C97 105.8(8) . . ? C107 C105 C97 111.2(8) . . ? C102 C109 C111 113.6(8) . . ? C102 C109 C110 110.5(8) . . ? C111 C109 C110 108.0(9) . . ? C102 C109 C112 107.9(8) . . ? C111 C109 C112 107.2(8) . . ? C110 C109 C112 109.6(8) . . ? Cl1 C113 Cl2 112.0(5) . . ? Cl3 C114 Cl4 112.7(6) . . ? Cl6 C115 Cl5 113.2(6) . . ? Cl7 C116 Cl8 111.1(6) . . ? Cl9 C117 Cl10 126.4(11) . . ? Cl1A C118 Cl11 119.4(18) . . ? Cl1A C118 Cl1B 43.2(8) . . ? Cl11 C118 Cl1B 125.2(19) . . ? Cl2A C119 Cl12 104.2(14) . . ? Cl2A C119 Cl2B 96.7(14) . . ? Cl12 C119 Cl2B 97.7(14) . . ? Cl4B C120 Cl3B 60.4(10) . . ? Cl4B C120 Cl3A 144.8(17) . . ? Cl3B C120 Cl3A 100.9(12) . . ? Cl4B C120 Cl4A 101.6(14) . . ? Cl3B C120 Cl4A 42.1(7) . . ? Cl3A C120 Cl4A 71.2(10) . . ? Cl5B C121 Cl6B 79.6(15) . . ? Cl5B C121 Cl5A 106.8(14) . . ? Cl6B C121 Cl5A 139(3) . . ? Cl5B C121 Cl6A 50.6(11) . . ? Cl6B C121 Cl6A 115(2) . . ? Cl5A C121 Cl6A 56.3(11) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 2.458 _refine_diff_density_min -1.381 _refine_diff_density_rms 0.190 data_bct-5 _database_code_depnum_ccdc_archive 'CCDC 859740' #TrackingRef '5.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C60 H80 N10 O11 Pt2 S4 Zn2' _chemical_formula_weight 1766.50 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' Zn Zn 0.2839 1.4301 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_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 27.540(3) _cell_length_b 19.1614(17) _cell_length_c 16.0561(15) _cell_angle_alpha 90.00 _cell_angle_beta 119.2720(10) _cell_angle_gamma 90.00 _cell_volume 7391.0(12) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 35221 _cell_measurement_theta_min 1.36 _cell_measurement_theta_max 25.00 _exptl_crystal_description cuboid _exptl_crystal_colour yellow _exptl_crystal_size_max 0.07 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.588 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3512 _exptl_absorpt_coefficient_mu 4.586 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7396 _exptl_absorpt_correction_T_max 0.8031 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART ApexCCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 35221 _diffrn_reflns_av_R_equivalents 0.0409 _diffrn_reflns_av_sigmaI/netI 0.0311 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.36 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6518 _reflns_number_gt 5223 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0977P)^2^+7.7026P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6518 _refine_ls_number_parameters 427 _refine_ls_number_restraints 124 _refine_ls_R_factor_all 0.0636 _refine_ls_R_factor_gt 0.0469 _refine_ls_wR_factor_ref 0.1564 _refine_ls_wR_factor_gt 0.1383 _refine_ls_goodness_of_fit_ref 1.127 _refine_ls_restrained_S_all 1.127 _refine_ls_shift/su_max 0.017 _refine_ls_shift/su_mean 0.001 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.216360(12) 0.192355(15) 0.89258(2) 0.04789(15) Uani 1 1 d . . . Zn1 Zn 0.01741(4) 0.09893(5) 0.36691(7) 0.0606(3) Uani 1 1 d . . . S1 S 0.19622(10) 0.25642(12) 0.75948(16) 0.0672(6) Uani 1 1 d . A . S2 S 0.12499(9) 0.20452(11) 0.85336(17) 0.0597(6) Uani 1 1 d . . . O1 O -0.0487(8) 0.0570(10) 0.3727(13) 0.092(4) Uani 0.68(3) 1 d PU A 3 O2 O -0.0579(9) 0.1621(13) 0.3742(17) 0.135(5) Uani 0.68(3) 1 d PU A 3 O3 O -0.1134(7) 0.1081(14) 0.3902(13) 0.129(5) Uani 0.68(3) 1 d PU A 3 O1' O -0.0381(18) 0.055(2) 0.410(3) 0.092(4) Uani 0.32(3) 1 d PU A 4 O2' O -0.044(2) 0.159(3) 0.423(4) 0.135(5) Uani 0.32(3) 1 d PU A 4 O3' O -0.1125(15) 0.064(3) 0.394(3) 0.129(5) Uani 0.32(3) 1 d PU A 4 O4 O 0.0000 0.1438(5) 0.2500 0.080(3) Uani 1 2 d S . . N1 N 0.2428(3) 0.1369(3) 1.0167(4) 0.0488(15) Uani 1 1 d . . . N2 N 0.3001(3) 0.1812(3) 0.9384(5) 0.0504(16) Uani 1 1 d . . . N3 N 0.0750(3) 0.1455(4) 0.4867(5) 0.0598(18) Uani 1 1 d . A . N4 N 0.0503(3) -0.0050(4) 0.8656(5) 0.0580(17) Uani 1 1 d . . . N5 N -0.0737(4) 0.1006(8) 0.3842(8) 0.104(3) Uani 1 1 d . . . C1 C 0.2124(3) 0.1207(4) 1.0589(6) 0.058(2) Uani 1 1 d . . . H1 H 0.1771 0.1399 1.0345 0.070 Uiso 1 1 calc R . . C2 C 0.2310(4) 0.0780(5) 1.1348(6) 0.068(2) Uani 1 1 d . . . H2 H 0.2083 0.0683 1.1613 0.082 Uiso 1 1 calc R . . C3 C 0.2829(4) 0.0485(5) 1.1736(7) 0.076(3) Uani 1 1 d . B . C4 C 0.3158(3) 0.0673(5) 1.1337(7) 0.067(2) Uani 1 1 d . . . H4 H 0.3518 0.0499 1.1591 0.080 Uiso 1 1 calc R . . C5 C 0.2950(3) 0.1117(4) 1.0566(5) 0.0492(18) Uani 1 1 d . . . C6 C 0.3274(3) 0.1384(4) 1.0127(5) 0.0498(18) Uani 1 1 d . . . C7 C 0.3836(3) 0.1231(5) 1.0474(6) 0.062(2) Uani 1 1 d . . . H7 H 0.4010 0.0911 1.0969 0.075 Uiso 1 1 calc R . . C8 C 0.4136(4) 0.1538(5) 1.0108(7) 0.063(2) Uani 1 1 d . B . C9 C 0.3848(4) 0.2011(5) 0.9378(7) 0.069(3) Uani 1 1 d . . . H9 H 0.4035 0.2255 0.9119 0.083 Uiso 1 1 calc R . . C10 C 0.3286(4) 0.2123(4) 0.9029(6) 0.058(2) Uani 1 1 d . . . H10 H 0.3101 0.2431 0.8522 0.069 Uiso 1 1 calc R . . C11 C 0.3051(5) 0.0004(8) 1.2638(9) 0.117(5) Uani 1 1 d D . . C12 C 0.2753(13) 0.014(2) 1.324(2) 0.133(8) Uani 0.485(12) 1 d PDU B 1 H12A H 0.2905 -0.0160 1.3788 0.200 Uiso 0.485(12) 1 calc PR B 1 H12B H 0.2361 0.0055 1.2857 0.200 Uiso 0.485(12) 1 calc PR B 1 H12C H 0.2810 0.0620 1.3452 0.200 Uiso 0.485(12) 1 calc PR B 1 C13 C 0.2851(16) -0.0736(13) 1.229(3) 0.156(9) Uani 0.485(12) 1 d PDU B 1 H13A H 0.2984 -0.1047 1.2823 0.234 Uiso 0.485(12) 1 calc PR B 1 H13B H 0.2992 -0.0883 1.1873 0.234 Uiso 0.485(12) 1 calc PR B 1 H13C H 0.2452 -0.0745 1.1942 0.234 Uiso 0.485(12) 1 calc PR B 1 C14 C 0.3646(9) 0.0137(19) 1.335(2) 0.122(7) Uani 0.485(12) 1 d PDU B 1 H14A H 0.3759 -0.0173 1.3883 0.182 Uiso 0.485(12) 1 calc PR B 1 H14B H 0.3689 0.0611 1.3565 0.182 Uiso 0.485(12) 1 calc PR B 1 H14C H 0.3873 0.0056 1.3058 0.182 Uiso 0.485(12) 1 calc PR B 1 C12' C 0.2607(11) -0.0316(19) 1.281(2) 0.133(8) Uani 0.515(12) 1 d PDU B 2 H12D H 0.2779 -0.0599 1.3379 0.200 Uiso 0.515(12) 1 calc PR B 2 H12E H 0.2365 -0.0601 1.2278 0.200 Uiso 0.515(12) 1 calc PR B 2 H12F H 0.2395 0.0048 1.2896 0.200 Uiso 0.515(12) 1 calc PR B 2 C13' C 0.3566(12) -0.0446(17) 1.284(3) 0.156(9) Uani 0.515(12) 1 d PDU B 2 H13D H 0.3675 -0.0722 1.3401 0.234 Uiso 0.515(12) 1 calc PR B 2 H13E H 0.3868 -0.0145 1.2933 0.234 Uiso 0.515(12) 1 calc PR B 2 H13F H 0.3474 -0.0747 1.2304 0.234 Uiso 0.515(12) 1 calc PR B 2 C14' C 0.3435(12) 0.0423(15) 1.3540(17) 0.122(7) Uani 0.515(12) 1 d PDU B 2 H14D H 0.3572 0.0125 1.4089 0.182 Uiso 0.515(12) 1 calc PR B 2 H14E H 0.3230 0.0803 1.3610 0.182 Uiso 0.515(12) 1 calc PR B 2 H14F H 0.3743 0.0605 1.3484 0.182 Uiso 0.515(12) 1 calc PR B 2 C15 C 0.4756(4) 0.1398(5) 1.0493(7) 0.077(3) Uani 1 1 d D . . C16 C 0.4979(12) 0.0835(13) 1.1316(18) 0.104(6) Uani 0.485(12) 1 d PDU B 1 H16A H 0.4810 0.0392 1.1056 0.156 Uiso 0.485(12) 1 calc PR B 1 H16B H 0.4886 0.0975 1.1795 0.156 Uiso 0.485(12) 1 calc PR B 1 H16C H 0.5376 0.0797 1.1597 0.156 Uiso 0.485(12) 1 calc PR B 1 C17 C 0.4863(13) 0.1122(16) 0.9731(18) 0.105(6) Uani 0.485(12) 1 d PDU B 1 H17A H 0.4741 0.1457 0.9223 0.158 Uiso 0.485(12) 1 calc PR B 1 H17B H 0.4662 0.0693 0.9487 0.158 Uiso 0.485(12) 1 calc PR B 1 H17C H 0.5254 0.1038 0.9991 0.158 Uiso 0.485(12) 1 calc PR B 1 C18 C 0.5037(13) 0.2093(12) 1.094(2) 0.103(6) Uani 0.485(12) 1 d PDU B 1 H18A H 0.4905 0.2447 1.0451 0.154 Uiso 0.485(12) 1 calc PR B 1 H18B H 0.5433 0.2045 1.1210 0.154 Uiso 0.485(12) 1 calc PR B 1 H18C H 0.4949 0.2223 1.1425 0.154 Uiso 0.485(12) 1 calc PR B 1 C16' C 0.4883(11) 0.0649(10) 1.084(2) 0.104(6) Uani 0.515(12) 1 d PDU B 2 H16D H 0.4788 0.0346 1.0303 0.156 Uiso 0.515(12) 1 calc PR B 2 H16E H 0.4668 0.0523 1.1139 0.156 Uiso 0.515(12) 1 calc PR B 2 H16F H 0.5272 0.0604 1.1287 0.156 Uiso 0.515(12) 1 calc PR B 2 C17' C 0.4887(13) 0.1493(15) 0.9681(17) 0.105(6) Uani 0.515(12) 1 d PDU B 2 H17D H 0.4700 0.1901 0.9318 0.158 Uiso 0.515(12) 1 calc PR B 2 H17E H 0.4764 0.1091 0.9273 0.158 Uiso 0.515(12) 1 calc PR B 2 H17F H 0.5282 0.1549 0.9941 0.158 Uiso 0.515(12) 1 calc PR B 2 C18' C 0.5084(12) 0.1865(13) 1.1327(17) 0.103(6) Uani 0.515(12) 1 d PDU B 2 H18D H 0.5057 0.2338 1.1110 0.154 Uiso 0.515(12) 1 calc PR B 2 H18E H 0.5467 0.1723 1.1646 0.154 Uiso 0.515(12) 1 calc PR B 2 H18F H 0.4940 0.1836 1.1763 0.154 Uiso 0.515(12) 1 calc PR B 2 C19 C 0.0975(4) 0.1116(4) 0.5704(6) 0.061(2) Uani 1 1 d . . . H19 H 0.0885 0.0649 0.5711 0.073 Uiso 1 1 calc R A . C20 C 0.1327(4) 0.1430(4) 0.6539(6) 0.062(2) Uani 1 1 d . A . H20 H 0.1450 0.1180 0.7103 0.075 Uiso 1 1 calc R . . C21 C 0.1513(3) 0.2111(4) 0.6585(6) 0.055(2) Uani 1 1 d . . . C22 C 0.1290(4) 0.2448(5) 0.5694(6) 0.071(3) Uani 1 1 d . A . H22 H 0.1403 0.2900 0.5659 0.086 Uiso 1 1 calc R . . C23 C 0.0913(4) 0.2120(6) 0.4891(7) 0.075(3) Uani 1 1 d . . . H23 H 0.0758 0.2368 0.4321 0.090 Uiso 1 1 calc R A . C24 C 0.0970(4) -0.0019(5) 0.8572(6) 0.062(2) Uani 1 1 d . . . H24 H 0.1133 -0.0437 0.8546 0.074 Uiso 1 1 calc R . . C25 C 0.1215(3) 0.0594(4) 0.8524(6) 0.057(2) Uani 1 1 d . . . H25 H 0.1534 0.0582 0.8462 0.069 Uiso 1 1 calc R . . C26 C 0.0989(3) 0.1222(4) 0.8566(5) 0.0522(19) Uani 1 1 d . . . C27 C 0.0504(4) 0.1205(5) 0.8648(7) 0.071(2) Uani 1 1 d . . . H27 H 0.0335 0.1618 0.8675 0.085 Uiso 1 1 calc R . . C28 C 0.0280(4) 0.0567(5) 0.8687(7) 0.071(2) Uani 1 1 d . . . H28 H -0.0042 0.0565 0.8738 0.085 Uiso 1 1 calc R . . O5 O 0.5702(12) 0.0422(16) 0.824(2) 0.180(10) Uiso 0.50 1 d PD C -1 C29 C 0.6128(15) 0.068(2) 0.913(2) 0.153(13) Uiso 0.50 1 d PD C -1 O6 O 0.5315(15) 0.2042(18) 0.769(3) 0.224(16) Uiso 0.50 1 d PD D -1 C30 C 0.571(2) 0.154(3) 0.831(4) 0.21(2) Uiso 0.50 1 d PD D -1 O5' O 0.5862(15) 0.101(2) 0.872(3) 0.214(14) Uiso 0.50 1 d PD E 2 C29' C 0.5308(16) 0.099(3) 0.796(3) 0.181(16) Uiso 0.50 1 d PD . 2 O6' O 0.2802(17) 0.367(2) 0.555(3) 0.273(17) Uiso 0.50 1 d PD F 2 C30' C 0.302(2) 0.316(3) 0.634(4) 0.22(2) Uiso 0.50 1 d PD F 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 0.0470(2) 0.0424(2) 0.0434(2) -0.00243(12) 0.01363(15) -0.00343(12) Zn1 0.0532(6) 0.0697(7) 0.0474(5) -0.0047(4) 0.0158(5) 0.0090(5) S1 0.0691(14) 0.0590(13) 0.0518(12) 0.0057(10) 0.0128(11) -0.0145(11) S2 0.0504(12) 0.0478(12) 0.0653(14) -0.0002(9) 0.0163(11) 0.0034(9) O1 0.091(6) 0.097(5) 0.095(8) -0.006(6) 0.050(6) 0.008(4) O2 0.131(7) 0.139(7) 0.138(9) -0.001(7) 0.068(7) 0.019(5) O3 0.107(6) 0.144(9) 0.156(7) -0.001(7) 0.079(6) 0.002(6) O1' 0.091(6) 0.097(5) 0.095(8) -0.006(6) 0.050(6) 0.008(4) O2' 0.131(7) 0.139(7) 0.138(9) -0.001(7) 0.068(7) 0.019(5) O3' 0.107(6) 0.144(9) 0.156(7) -0.001(7) 0.079(6) 0.002(6) O4 0.108(7) 0.061(6) 0.047(5) 0.000 0.020(5) 0.000 N1 0.050(4) 0.045(4) 0.043(3) -0.002(3) 0.016(3) -0.004(3) N2 0.050(4) 0.042(4) 0.053(4) -0.009(3) 0.021(3) -0.005(3) N3 0.054(4) 0.067(5) 0.046(4) -0.004(3) 0.015(3) 0.000(3) N4 0.055(4) 0.056(4) 0.054(4) -0.003(3) 0.020(3) -0.008(3) N5 0.066(6) 0.149(11) 0.118(9) -0.014(8) 0.061(6) -0.004(7) C1 0.049(5) 0.060(5) 0.051(5) 0.003(4) 0.014(4) -0.005(4) C2 0.056(5) 0.077(6) 0.060(5) 0.004(5) 0.019(4) -0.014(5) C3 0.064(6) 0.076(6) 0.069(6) 0.025(5) 0.017(5) -0.009(5) C4 0.039(4) 0.067(6) 0.075(6) 0.016(5) 0.013(4) -0.001(4) C5 0.038(4) 0.051(4) 0.048(4) -0.002(3) 0.013(3) -0.003(3) C6 0.046(4) 0.046(4) 0.053(5) 0.000(4) 0.021(4) -0.001(3) C7 0.053(5) 0.061(5) 0.060(5) 0.003(4) 0.018(4) 0.001(4) C8 0.054(5) 0.056(5) 0.075(6) -0.014(5) 0.030(5) -0.002(4) C9 0.065(6) 0.078(7) 0.074(6) -0.022(5) 0.042(5) -0.019(5) C10 0.064(6) 0.054(5) 0.056(5) -0.006(4) 0.030(4) -0.007(4) C11 0.086(8) 0.136(12) 0.119(11) 0.072(9) 0.042(8) 0.007(8) C12 0.132(9) 0.139(10) 0.131(9) 0.019(7) 0.067(7) -0.006(7) C13 0.158(11) 0.147(11) 0.154(11) 0.017(7) 0.070(7) -0.001(7) C14 0.123(9) 0.125(9) 0.112(9) 0.010(6) 0.054(6) 0.004(6) C12' 0.132(9) 0.139(10) 0.131(9) 0.019(7) 0.067(7) -0.006(7) C13' 0.158(11) 0.147(11) 0.154(11) 0.017(7) 0.070(7) -0.001(7) C14' 0.123(9) 0.125(9) 0.112(9) 0.010(6) 0.054(6) 0.004(6) C15 0.056(6) 0.086(7) 0.095(7) -0.008(6) 0.042(5) 0.006(5) C16 0.086(7) 0.107(9) 0.123(9) -0.007(6) 0.054(7) 0.008(6) C17 0.093(7) 0.110(10) 0.113(8) -0.010(6) 0.050(6) 0.011(7) C18 0.092(8) 0.109(9) 0.103(9) -0.008(6) 0.045(6) 0.002(6) C16' 0.086(7) 0.107(9) 0.123(9) -0.007(6) 0.054(7) 0.008(6) C17' 0.093(7) 0.110(10) 0.113(8) -0.010(6) 0.050(6) 0.011(7) C18' 0.092(8) 0.109(9) 0.103(9) -0.008(6) 0.045(6) 0.002(6) C19 0.068(6) 0.049(5) 0.053(5) 0.000(4) 0.019(4) -0.002(4) C20 0.073(6) 0.052(5) 0.044(5) 0.006(4) 0.014(4) 0.006(4) C21 0.050(5) 0.058(5) 0.045(4) 0.001(4) 0.016(4) 0.003(4) C22 0.075(6) 0.072(6) 0.047(5) 0.007(4) 0.015(5) -0.012(5) C23 0.073(7) 0.080(7) 0.050(5) 0.021(5) 0.014(5) 0.012(5) C24 0.053(5) 0.061(5) 0.062(5) -0.008(4) 0.019(4) 0.002(4) C25 0.045(4) 0.050(5) 0.072(6) -0.003(4) 0.026(4) -0.002(4) C26 0.040(4) 0.057(5) 0.047(4) -0.002(4) 0.011(3) -0.003(3) C27 0.064(6) 0.063(6) 0.074(6) -0.004(5) 0.025(5) 0.003(5) C28 0.051(5) 0.074(7) 0.079(7) -0.001(5) 0.026(5) -0.004(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 N1 2.052(6) . ? Pt1 N2 2.060(7) . ? Pt1 S1 2.285(2) . ? Pt1 S2 2.288(2) . ? Zn1 O4 1.901(4) . ? Zn1 N3 2.007(7) . ? Zn1 N4 2.021(7) 6 ? Zn1 O1 2.034(19) . ? Zn1 O1' 2.14(4) . ? Zn1 O2 2.45(2) . ? Zn1 O2' 2.55(5) . ? S1 C21 1.718(8) . ? S2 C26 1.744(8) . ? O1 N5 1.15(2) . ? O2 N5 1.29(2) . ? O3 N5 1.153(18) . ? O1' N5 1.23(4) . ? O2' N5 1.35(5) . ? O3' N5 1.35(4) . ? O4 Zn1 1.901(4) 2 ? N1 C5 1.344(10) . ? N1 C1 1.346(10) . ? N2 C10 1.319(11) . ? N2 C6 1.335(10) . ? N3 C19 1.341(10) . ? N3 C23 1.345(12) . ? N4 C28 1.344(11) . ? N4 C24 1.356(11) . ? N4 Zn1 2.021(7) 6_556 ? C1 C2 1.344(12) . ? C2 C3 1.372(13) . ? C3 C4 1.388(13) . ? C3 C11 1.567(14) . ? C4 C5 1.376(11) . ? C5 C6 1.474(11) . ? C6 C7 1.395(11) . ? C7 C8 1.359(12) . ? C8 C9 1.384(14) . ? C8 C15 1.529(12) . ? C9 C10 1.380(13) . ? C11 C14 1.491(18) . ? C11 C12' 1.513(17) . ? C11 C13 1.526(18) . ? C11 C14' 1.538(18) . ? C11 C13' 1.552(18) . ? C11 C12 1.572(18) . ? C15 C17 1.488(17) . ? C15 C18' 1.494(17) . ? C15 C16' 1.515(17) . ? C15 C17' 1.526(17) . ? C15 C18 1.531(17) . ? C15 C16 1.579(17) . ? C19 C20 1.351(11) . ? C20 C21 1.390(12) . ? C21 C22 1.408(11) . ? C22 C23 1.352(13) . ? C24 C25 1.376(12) . ? C25 C26 1.372(11) . ? C26 C27 1.406(12) . ? C27 C28 1.385(13) . ? O5 C29 1.421(19) . ? O6 C30 1.43(2) . ? O5' C29' 1.412(19) . ? C29' C29' 1.61(7) 2_656 ? O6' C30' 1.47(2) . ? 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 N2 78.2(3) . . ? N1 Pt1 S1 174.16(19) . . ? N2 Pt1 S1 96.2(2) . . ? N1 Pt1 S2 98.09(19) . . ? N2 Pt1 S2 175.72(19) . . ? S1 Pt1 S2 87.51(9) . . ? O4 Zn1 N3 116.4(3) . . ? O4 Zn1 N4 106.9(3) . 6 ? N3 Zn1 N4 105.0(3) . 6 ? O4 Zn1 O1 115.1(5) . . ? N3 Zn1 O1 115.9(6) . . ? N4 Zn1 O1 93.7(6) 6 . ? O4 Zn1 O1' 128.7(11) . . ? N3 Zn1 O1' 102.6(11) . . ? N4 Zn1 O1' 92.7(12) 6 . ? O1 Zn1 O1' 14.3(11) . . ? O4 Zn1 O2 90.7(6) . . ? N3 Zn1 O2 91.4(6) . . ? N4 Zn1 O2 146.5(6) 6 . ? O1 Zn1 O2 52.8(8) . . ? O1' Zn1 O2 54.8(13) . . ? O4 Zn1 O2' 104.6(12) . . ? N3 Zn1 O2' 79.0(12) . . ? N4 Zn1 O2' 141.9(12) 6 . ? O1 Zn1 O2' 53.1(13) . . ? O1' Zn1 O2' 50.3(17) . . ? O2 Zn1 O2' 15.6(11) . . ? C21 S1 Pt1 110.1(3) . . ? C26 S2 Pt1 108.2(3) . . ? N5 O1 Zn1 109.8(14) . . ? N5 O2 Zn1 84.3(11) . . ? N5 O1' Zn1 101(3) . . ? N5 O2' Zn1 79(2) . . ? Zn1 O4 Zn1 126.2(5) 2 . ? C5 N1 C1 117.4(7) . . ? C5 N1 Pt1 116.0(5) . . ? C1 N1 Pt1 126.6(5) . . ? C10 N2 C6 118.0(7) . . ? C10 N2 Pt1 126.7(6) . . ? C6 N2 Pt1 115.3(5) . . ? C19 N3 C23 116.5(7) . . ? C19 N3 Zn1 120.4(6) . . ? C23 N3 Zn1 123.0(6) . . ? C28 N4 C24 116.0(8) . . ? C28 N4 Zn1 124.5(6) . 6_556 ? C24 N4 Zn1 119.4(6) . 6_556 ? O1 N5 O3 140(2) . . ? O1 N5 O1' 25(2) . . ? O3 N5 O1' 134(3) . . ? O1 N5 O2 112.1(16) . . ? O3 N5 O2 106.8(19) . . ? O1' N5 O2 116(2) . . ? O1 N5 O3' 102(3) . . ? O3 N5 O3' 38.3(17) . . ? O1' N5 O3' 98(3) . . ? O2 N5 O3' 145(3) . . ? O1 N5 O2' 114(2) . . ? O3 N5 O2' 104(2) . . ? O1' N5 O2' 104(3) . . ? O2 N5 O2' 30(2) . . ? O3' N5 O2' 136(3) . . ? C2 C1 N1 122.9(8) . . ? C1 C2 C3 120.8(9) . . ? C2 C3 C4 117.0(8) . . ? C2 C3 C11 120.8(9) . . ? C4 C3 C11 122.0(9) . . ? C5 C4 C3 119.8(8) . . ? N1 C5 C4 121.9(7) . . ? N1 C5 C6 113.8(7) . . ? C4 C5 C6 124.2(7) . . ? N2 C6 C7 121.1(7) . . ? N2 C6 C5 115.5(7) . . ? C7 C6 C5 123.3(7) . . ? C8 C7 C6 121.7(8) . . ? C7 C8 C9 115.6(8) . . ? C7 C8 C15 122.9(9) . . ? C9 C8 C15 121.4(9) . . ? C10 C9 C8 120.7(9) . . ? N2 C10 C9 122.7(9) . . ? C14 C11 C12' 128(2) . . ? C14 C11 C13 120(2) . . ? C12' C11 C13 61.0(19) . . ? C14 C11 C14' 36.6(15) . . ? C12' C11 C14' 106(2) . . ? C13 C11 C14' 142(2) . . ? C14 C11 C13' 52.1(17) . . ? C12' C11 C13' 118(2) . . ? C13 C11 C13' 72(2) . . ? C14' C11 C13' 87.5(19) . . ? C14 C11 C3 113.2(15) . . ? C12' C11 C3 115.1(15) . . ? C13 C11 C3 107.3(17) . . ? C14' C11 C3 109.9(15) . . ? C13' C11 C3 115.0(16) . . ? C14 C11 C12 102(2) . . ? C12' C11 C12 40.4(15) . . ? C13 C11 C12 101(2) . . ? C14' C11 C12 69.8(18) . . ? C13' C11 C12 131.9(19) . . ? C3 C11 C12 112.6(16) . . ? C17 C15 C18' 132.3(19) . . ? C17 C15 C16' 82.0(16) . . ? C18' C15 C16' 108.1(17) . . ? C17 C15 C17' 27.7(15) . . ? C18' C15 C17' 113.7(18) . . ? C16' C15 C17' 108.4(16) . . ? C17 C15 C8 111.2(14) . . ? C18' C15 C8 108.9(14) . . ? C16' C15 C8 109.1(13) . . ? C17' C15 C8 108.6(14) . . ? C17 C15 C18 115.6(19) . . ? C18' C15 C18 27.6(15) . . ? C16' C15 C18 132.9(18) . . ? C17' C15 C18 90.9(17) . . ? C8 C15 C18 104.2(14) . . ? C17 C15 C16 107.0(17) . . ? C18' C15 C16 80.9(16) . . ? C16' C15 C16 28.6(14) . . ? C17' C15 C16 129.8(17) . . ? C8 C15 C16 111.0(13) . . ? C18 C15 C16 107.7(18) . . ? N3 C19 C20 122.3(8) . . ? C19 C20 C21 122.5(8) . . ? C20 C21 C22 114.2(7) . . ? C20 C21 S1 127.0(6) . . ? C22 C21 S1 118.7(7) . . ? C23 C22 C21 120.3(9) . . ? N3 C23 C22 123.9(8) . . ? N4 C24 C25 123.9(8) . . ? C26 C25 C24 119.9(8) . . ? C25 C26 C27 117.3(8) . . ? C25 C26 S2 126.1(6) . . ? C27 C26 S2 116.6(7) . . ? C28 C27 C26 119.3(9) . . ? N4 C28 C27 123.5(9) . . ? O5' C29' C29' 176(6) . 2_656 ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.493 _refine_diff_density_min -0.673 _refine_diff_density_rms 0.287 data_ic13674 _database_code_depnum_ccdc_archive 'CCDC 859741' #TrackingRef '7.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C65 H86 Cl4 N11 O3.50 Pd2 S4 Zn2' _chemical_formula_weight 1691.03 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' 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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 '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' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M I-42d loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'y, -x, -z' '-y, x, -z' '-x+1/2, y, -z+3/4' 'x+1/2, -y, -z+3/4' '-y+1/2, -x, z+3/4' 'y+1/2, x, z+3/4' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-y+1/2, x+1/2, -z+1/2' '-x+1, y+1/2, -z+5/4' 'x+1, -y+1/2, -z+5/4' '-y+1, -x+1/2, z+5/4' 'y+1, x+1/2, z+5/4' _cell_length_a 25.4591(7) _cell_length_b 25.4591(7) _cell_length_c 46.7498(13) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 30301.6(14) _cell_formula_units_Z 16 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 5277 _cell_measurement_theta_min 2.26 _cell_measurement_theta_max 19.57 _exptl_crystal_description block _exptl_crystal_colour orange-yellow _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas not_measured _exptl_crystal_density_diffrn 1.483 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 13840 _exptl_absorpt_coefficient_mu 1.395 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7490 _exptl_absorpt_correction_T_max 0.8731 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'BRUKER SMART APEXCCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 68185 _diffrn_reflns_av_R_equivalents 0.1103 _diffrn_reflns_av_sigmaI/netI 0.0824 _diffrn_reflns_limit_h_min -33 _diffrn_reflns_limit_h_max 33 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 60 _diffrn_reflns_theta_min 0.91 _diffrn_reflns_theta_max 27.50 _reflns_number_total 17420 _reflns_number_gt 14460 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0560P)^2^+32.4547P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.339(19) _refine_ls_number_reflns 17420 _refine_ls_number_parameters 785 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0958 _refine_ls_R_factor_gt 0.0782 _refine_ls_wR_factor_ref 0.1621 _refine_ls_wR_factor_gt 0.1553 _refine_ls_goodness_of_fit_ref 1.261 _refine_ls_restrained_S_all 1.263 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.00238(2) -0.20994(2) 0.153333(13) 0.02493(13) Uani 1 1 d . . . Pd2 Pd 0.20837(2) -0.02649(2) 0.346654(14) 0.02566(14) Uani 1 1 d . . . Zn1 Zn 0.16551(4) 0.03422(4) 0.18807(2) 0.0307(2) Uani 1 1 d . . . Zn2 Zn -0.05014(4) -0.16205(4) 0.31224(2) 0.0312(2) Uani 1 1 d . . . Cl1 Cl 0.23592(10) 0.06383(9) 0.16489(5) 0.0435(6) Uani 1 1 d . . . Cl2 Cl 0.09812(12) 0.08689(10) 0.19695(6) 0.0536(7) Uani 1 1 d . . . Cl3 Cl -0.09324(9) -0.08753(10) 0.30394(5) 0.0455(6) Uani 1 1 d . . . Cl4 Cl -0.08671(9) -0.22736(9) 0.33749(5) 0.0378(5) Uani 1 1 d . . . S1 S 0.08615(8) -0.19182(8) 0.13816(5) 0.0325(5) Uani 1 1 d . . . S2 S 0.24781(10) -0.07068(9) 0.30978(5) 0.0375(5) Uani 1 1 d . . . S3 S 0.03820(9) -0.25721(9) 0.19006(5) 0.0344(5) Uani 1 1 d . . . S4 S 0.18297(9) -0.10651(8) 0.36426(5) 0.0323(5) Uani 1 1 d . . . N1 N -0.0742(3) -0.2259(2) 0.16364(14) 0.0242(15) Uani 1 1 d . . . N2 N -0.0362(3) -0.1636(2) 0.12410(14) 0.0240(14) Uani 1 1 d . . . N3 N 0.1660(3) 0.0186(3) 0.37532(15) 0.0272(15) Uani 1 1 d . . . N4 N 0.2306(3) 0.0484(3) 0.33468(14) 0.0284(16) Uani 1 1 d . . . N5 N 0.1365(3) -0.0295(3) 0.16690(15) 0.0339(17) Uani 1 1 d . . . N6 N 0.1895(3) 0.0013(3) 0.22587(14) 0.0295(15) Uani 1 1 d . . . N7 N -0.0261(3) -0.1923(3) 0.27382(15) 0.0342(17) Uani 1 1 d . . . N8 N 0.0182(2) -0.1418(3) 0.33195(14) 0.0270(15) Uani 1 1 d . . . C1 C -0.0931(3) -0.2633(3) 0.18109(18) 0.0310(19) Uani 1 1 d . . . H1 H -0.0689 -0.2868 0.1898 0.037 Uiso 1 1 calc R . . C2 C -0.1460(3) -0.2695(3) 0.18713(16) 0.0256(17) Uani 1 1 d . . . H2 H -0.1569 -0.2958 0.2003 0.031 Uiso 1 1 calc R . . C3 C -0.1837(3) -0.2372(3) 0.17395(16) 0.0252(17) Uani 1 1 d . . . C4 C -0.1636(3) -0.1990(3) 0.15544(16) 0.0233(16) Uani 1 1 d . . . H4 H -0.1874 -0.1757 0.1462 0.028 Uiso 1 1 calc R . . C5 C -0.1106(3) -0.1940(3) 0.15007(17) 0.0274(18) Uani 1 1 d . . . C6 C -0.0871(3) -0.1573(3) 0.12932(16) 0.0239(17) Uani 1 1 d . . . C7 C -0.1173(3) -0.1190(3) 0.11596(17) 0.0272(18) Uani 1 1 d . . . H7 H -0.1533 -0.1151 0.1208 0.033 Uiso 1 1 calc R . . C8 C -0.0942(3) -0.0859(3) 0.09516(17) 0.0244(17) Uani 1 1 d . . . C9 C -0.0430(3) -0.0962(3) 0.08810(17) 0.031(2) Uani 1 1 d . . . H9 H -0.0270 -0.0779 0.0727 0.037 Uiso 1 1 calc R . . C10 C -0.0138(3) -0.1342(3) 0.10362(16) 0.0293(19) Uani 1 1 d . . . H10 H 0.0224 -0.1389 0.0994 0.035 Uiso 1 1 calc R . . C11 C -0.2422(3) -0.2447(3) 0.18006(16) 0.0211(16) Uani 1 1 d . . . C12 C -0.2504(4) -0.2326(4) 0.21187(18) 0.039(2) Uani 1 1 d . . . H12A H -0.2872 -0.2392 0.2170 0.059 Uiso 1 1 calc R . . H12B H -0.2419 -0.1956 0.2155 0.059 Uiso 1 1 calc R . . H12C H -0.2275 -0.2551 0.2234 0.059 Uiso 1 1 calc R . . C13 C -0.2559(3) -0.3026(3) 0.17394(19) 0.033(2) Uani 1 1 d . . . H13A H -0.2489 -0.3105 0.1538 0.050 Uiso 1 1 calc R . . H13B H -0.2932 -0.3087 0.1780 0.050 Uiso 1 1 calc R . . H13C H -0.2344 -0.3255 0.1861 0.050 Uiso 1 1 calc R . . C14 C -0.2761(3) -0.2083(3) 0.16220(17) 0.0292(18) Uani 1 1 d . . . H14A H -0.2713 -0.2164 0.1419 0.044 Uiso 1 1 calc R . . H14B H -0.2658 -0.1718 0.1658 0.044 Uiso 1 1 calc R . . H14C H -0.3131 -0.2130 0.1674 0.044 Uiso 1 1 calc R . . C15 C -0.1230(3) -0.0414(4) 0.08125(17) 0.031(2) Uani 1 1 d . . . C16 C -0.0949(4) 0.0104(4) 0.0883(2) 0.046(3) Uani 1 1 d . . . H16A H -0.0597 0.0101 0.0798 0.069 Uiso 1 1 calc R . . H16B H -0.0920 0.0142 0.1091 0.069 Uiso 1 1 calc R . . H16C H -0.1150 0.0398 0.0804 0.069 Uiso 1 1 calc R . . C17 C -0.1225(4) -0.0511(5) 0.04780(18) 0.051(3) Uani 1 1 d . . . H17A H -0.1457 -0.0806 0.0431 0.076 Uiso 1 1 calc R . . H17B H -0.0866 -0.0592 0.0416 0.076 Uiso 1 1 calc R . . H17C H -0.1349 -0.0194 0.0380 0.076 Uiso 1 1 calc R . . C18 C -0.1801(3) -0.0378(4) 0.0911(2) 0.040(2) Uani 1 1 d . . . H18A H -0.1814 -0.0243 0.1107 0.059 Uiso 1 1 calc R . . H18B H -0.1962 -0.0728 0.0905 0.059 Uiso 1 1 calc R . . H18C H -0.1995 -0.0141 0.0784 0.059 Uiso 1 1 calc R . . C19 C 0.1353(3) -0.0004(3) 0.39644(17) 0.0316(19) Uani 1 1 d . . . H19 H 0.1379 -0.0364 0.4018 0.038 Uiso 1 1 calc R . . C20 C 0.1003(4) 0.0319(4) 0.41029(17) 0.037(2) Uani 1 1 d . . . H20 H 0.0787 0.0177 0.4249 0.044 Uiso 1 1 calc R . . C21 C 0.0958(3) 0.0853(3) 0.40342(18) 0.0305(19) Uani 1 1 d . . . C22 C 0.1289(3) 0.1037(3) 0.38211(17) 0.0268(18) Uani 1 1 d . . . H22 H 0.1273 0.1396 0.3765 0.032 Uiso 1 1 calc R . . C23 C 0.1639(3) 0.0707(3) 0.36905(16) 0.0249(17) Uani 1 1 d . . . C24 C 0.2021(3) 0.0882(3) 0.34684(17) 0.0243(17) Uani 1 1 d . . . C25 C 0.2099(3) 0.1399(3) 0.33929(16) 0.0265(17) Uani 1 1 d . . . H25 H 0.1889 0.1668 0.3475 0.032 Uiso 1 1 calc R . . C26 C 0.2490(4) 0.1524(3) 0.31939(17) 0.031(2) Uani 1 1 d . . . C27 C 0.2782(3) 0.1121(3) 0.30783(17) 0.0316(19) Uani 1 1 d . . . H27 H 0.3050 0.1193 0.2942 0.038 Uiso 1 1 calc R . . C28 C 0.2681(3) 0.0611(3) 0.31628(17) 0.0296(19) Uani 1 1 d . . . H28 H 0.2891 0.0337 0.3085 0.035 Uiso 1 1 calc R . . C29 C 0.0537(4) 0.1189(4) 0.41778(19) 0.039(2) Uani 1 1 d . . . C30 C -0.0009(4) 0.0950(5) 0.4102(2) 0.053(3) Uani 1 1 d . . . H30A H -0.0059 0.0958 0.3894 0.080 Uiso 1 1 calc R . . H30B H -0.0286 0.1155 0.4195 0.080 Uiso 1 1 calc R . . H30C H -0.0024 0.0585 0.4169 0.080 Uiso 1 1 calc R . . C31 C 0.0610(4) 0.1172(5) 0.4510(2) 0.052(3) Uani 1 1 d . . . H31A H 0.0345 0.1396 0.4601 0.079 Uiso 1 1 calc R . . H31B H 0.0962 0.1299 0.4559 0.079 Uiso 1 1 calc R . . H31C H 0.0568 0.0810 0.4577 0.079 Uiso 1 1 calc R . . C32 C 0.0550(4) 0.1750(4) 0.4082(2) 0.046(3) Uani 1 1 d . . . H32A H 0.0508 0.1765 0.3873 0.068 Uiso 1 1 calc R . . H32B H 0.0887 0.1907 0.4135 0.068 Uiso 1 1 calc R . . H32C H 0.0263 0.1944 0.4173 0.068 Uiso 1 1 calc R . . C33 C 0.2547(4) 0.2099(4) 0.3090(2) 0.045(2) Uani 1 1 d . . . C34 C 0.2538(6) 0.2477(4) 0.3344(3) 0.082(5) Uani 1 1 d . . . H34A H 0.2551 0.2839 0.3274 0.123 Uiso 1 1 calc R . . H34B H 0.2843 0.2410 0.3466 0.123 Uiso 1 1 calc R . . H34C H 0.2215 0.2424 0.3454 0.123 Uiso 1 1 calc R . . C35 C 0.3060(4) 0.2176(5) 0.2919(3) 0.066(3) Uani 1 1 d . . . H35A H 0.3362 0.2096 0.3041 0.099 Uiso 1 1 calc R . . H35B H 0.3083 0.2541 0.2853 0.099 Uiso 1 1 calc R . . H35C H 0.3059 0.1941 0.2753 0.099 Uiso 1 1 calc R . . C36 C 0.2082(5) 0.2228(4) 0.2895(2) 0.060(3) Uani 1 1 d . . . H36A H 0.2043 0.1951 0.2751 0.089 Uiso 1 1 calc R . . H36B H 0.2144 0.2565 0.2799 0.089 Uiso 1 1 calc R . . H36C H 0.1760 0.2251 0.3010 0.089 Uiso 1 1 calc R . . C37 C 0.0876(3) -0.0455(3) 0.17167(17) 0.0265(18) Uani 1 1 d . . . H37 H 0.0648 -0.0229 0.1820 0.032 Uiso 1 1 calc R . . C38 C 0.0679(4) -0.0943(3) 0.16212(18) 0.033(2) Uani 1 1 d . . . H38 H 0.0322 -0.1036 0.1651 0.040 Uiso 1 1 calc R . . C39 C 0.1021(3) -0.1285(3) 0.14820(16) 0.0218(16) Uani 1 1 d . . . C40 C 0.1530(3) -0.1100(3) 0.14255(18) 0.0305(19) Uani 1 1 d . . . H40 H 0.1769 -0.1311 0.1320 0.037 Uiso 1 1 calc R . . C41 C 0.1679(3) -0.0628(3) 0.15212(18) 0.0295(18) Uani 1 1 d . . . H41 H 0.2028 -0.0518 0.1483 0.035 Uiso 1 1 calc R . . C42 C 0.1673(3) 0.0153(3) 0.25110(18) 0.0295(19) Uani 1 1 d . . . H42 H 0.1399 0.0406 0.2510 0.035 Uiso 1 1 calc R . . C43 C 0.1829(3) -0.0057(4) 0.2767(2) 0.034(2) Uani 1 1 d . . . H43 H 0.1653 0.0047 0.2937 0.041 Uiso 1 1 calc R . . C44 C 0.2241(3) -0.0422(3) 0.27853(19) 0.032(2) Uani 1 1 d . . . C45 C 0.2458(4) -0.0561(3) 0.2516(2) 0.040(2) Uani 1 1 d . . . H45 H 0.2739 -0.0806 0.2509 0.048 Uiso 1 1 calc R . . C46 C 0.2278(4) -0.0355(4) 0.22694(19) 0.037(2) Uani 1 1 d . . . H46 H 0.2427 -0.0474 0.2095 0.045 Uiso 1 1 calc R . . C47 C -0.0367(3) -0.1669(4) 0.24903(19) 0.034(2) Uani 1 1 d . . . H47 H -0.0572 -0.1357 0.2496 0.040 Uiso 1 1 calc R . . C48 C -0.0185(4) -0.1850(3) 0.22270(19) 0.034(2) Uani 1 1 d . . . H48 H -0.0262 -0.1658 0.2058 0.041 Uiso 1 1 calc R . . C49 C 0.0111(3) -0.2312(3) 0.22103(18) 0.0285(18) Uani 1 1 d . . . C50 C 0.0219(3) -0.2565(3) 0.2471(2) 0.035(2) Uani 1 1 d . . . H50 H 0.0417 -0.2881 0.2475 0.042 Uiso 1 1 calc R . . C51 C 0.0040(4) -0.2358(4) 0.2712(2) 0.040(2) Uani 1 1 d . . . H51 H 0.0133 -0.2533 0.2884 0.048 Uiso 1 1 calc R . . C52 C 0.0408(3) -0.0960(3) 0.32636(19) 0.033(2) Uani 1 1 d . . . H52 H 0.0215 -0.0712 0.3153 0.039 Uiso 1 1 calc R . . C53 C 0.0899(3) -0.0820(3) 0.33546(17) 0.0291(19) Uani 1 1 d . . . H53 H 0.1039 -0.0486 0.3305 0.035 Uiso 1 1 calc R . . C54 C 0.1200(3) -0.1171(3) 0.35226(15) 0.0217(16) Uani 1 1 d . . . C55 C 0.0956(3) -0.1646(3) 0.35896(16) 0.0263(17) Uani 1 1 d . . . H55 H 0.1133 -0.1892 0.3708 0.032 Uiso 1 1 calc R . . C56 C 0.0453(3) -0.1764(3) 0.34840(18) 0.0280(18) Uani 1 1 d . . . H56 H 0.0299 -0.2093 0.3529 0.034 Uiso 1 1 calc R . . O1 O 0.0000 0.0000 0.2501(8) 0.242(12) Uiso 1 2 d S . . O2 O 0.1472(3) -0.2683(3) 0.2580(2) 0.070(2) Uani 1 1 d . . . N9 N 0.1330(3) -0.1804(4) 0.24524(19) 0.054(2) Uani 1 1 d . . . C58 C 0.1430(4) -0.2327(5) 0.2402(3) 0.063(3) Uani 1 1 d . . . H58 H 0.1471 -0.2426 0.2207 0.075 Uiso 1 1 calc R . . C59 C 0.1267(5) -0.1455(5) 0.2225(3) 0.067(4) Uani 1 1 d . . . H59A H 0.1232 -0.1653 0.2047 0.101 Uiso 1 1 calc R . . H59B H 0.1573 -0.1223 0.2214 0.101 Uiso 1 1 calc R . . H59C H 0.0950 -0.1244 0.2256 0.101 Uiso 1 1 calc R . . C60 C 0.1251(5) -0.1639(4) 0.2742(2) 0.060(3) Uani 1 1 d . . . H60A H 0.1188 -0.1947 0.2863 0.089 Uiso 1 1 calc R . . H60B H 0.0948 -0.1403 0.2752 0.089 Uiso 1 1 calc R . . H60C H 0.1565 -0.1453 0.2810 0.089 Uiso 1 1 calc R . . O3 O 0.4164(6) -0.0333(6) 0.2787(3) 0.145(5) Uiso 1 1 d D . . N10 N 0.4153(4) -0.1241(4) 0.2737(2) 0.064(3) Uiso 1 1 d . . . C61 C 0.4364(7) -0.0750(6) 0.2671(4) 0.106(5) Uiso 1 1 d D . . H61 H 0.4651 -0.0721 0.2542 0.127 Uiso 1 1 calc R . . C62 C 0.4365(6) -0.1682(6) 0.2641(3) 0.093(5) Uiso 1 1 d . . . H62A H 0.4092 -0.1952 0.2624 0.139 Uiso 1 1 calc R . . H62B H 0.4637 -0.1801 0.2774 0.139 Uiso 1 1 calc R . . H62C H 0.4522 -0.1618 0.2453 0.139 Uiso 1 1 calc R . . C63 C 0.3752(5) -0.1244(6) 0.2936(3) 0.080(4) Uiso 1 1 d . . . H63A H 0.3882 -0.1389 0.3117 0.119 Uiso 1 1 calc R . . H63B H 0.3462 -0.1460 0.2865 0.119 Uiso 1 1 calc R . . H63C H 0.3628 -0.0884 0.2967 0.119 Uiso 1 1 calc R . . O4 O 0.0340(8) -0.0824(7) 0.0306(4) 0.200(7) Uiso 1 1 d D . . N11 N 0.1229(7) -0.1099(7) 0.0297(4) 0.140(6) Uiso 1 1 d . . . C64 C 0.0782(9) -0.0740(12) 0.0180(6) 0.203(12) Uiso 1 1 d D . . H64 H 0.0830 -0.0487 0.0033 0.244 Uiso 1 1 calc R . . C65 C 0.1402(8) -0.1401(8) 0.0536(4) 0.140(8) Uiso 1 1 d . . . H65A H 0.1638 -0.1188 0.0654 0.210 Uiso 1 1 calc R . . H65B H 0.1589 -0.1714 0.0468 0.210 Uiso 1 1 calc R . . H65C H 0.1098 -0.1509 0.0650 0.210 Uiso 1 1 calc R . . C66 C 0.1677(8) -0.1012(9) 0.0128(5) 0.146(8) Uiso 1 1 d . . . H66A H 0.1717 -0.1300 -0.0009 0.219 Uiso 1 1 calc R . . H66B H 0.1988 -0.0994 0.0251 0.219 Uiso 1 1 calc R . . H66C H 0.1638 -0.0680 0.0023 0.219 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.0248(3) 0.0237(3) 0.0263(3) -0.0033(2) -0.0016(3) 0.0029(3) Pd2 0.0271(3) 0.0231(3) 0.0268(3) 0.0044(3) -0.0064(3) -0.0018(3) Zn1 0.0464(6) 0.0204(5) 0.0252(5) -0.0021(4) 0.0067(4) -0.0017(4) Zn2 0.0233(5) 0.0437(6) 0.0265(5) 0.0038(5) -0.0023(4) -0.0006(4) Cl1 0.0558(15) 0.0331(12) 0.0415(14) -0.0039(10) 0.0133(11) -0.0132(11) Cl2 0.082(2) 0.0350(13) 0.0439(15) 0.0042(11) 0.0180(13) 0.0254(13) Cl3 0.0369(13) 0.0614(16) 0.0383(14) 0.0151(12) 0.0057(10) 0.0195(12) Cl4 0.0325(11) 0.0486(13) 0.0324(12) 0.0055(10) -0.0017(9) -0.0068(10) S1 0.0287(11) 0.0246(11) 0.0443(14) -0.0122(9) 0.0037(9) 0.0024(9) S2 0.0430(13) 0.0320(12) 0.0376(13) 0.0038(10) -0.0053(11) 0.0111(10) S3 0.0306(11) 0.0363(12) 0.0363(13) -0.0043(10) -0.0051(10) 0.0116(10) S4 0.0286(11) 0.0265(11) 0.0417(13) 0.0088(9) -0.0123(10) 0.0001(9) N1 0.032(4) 0.018(3) 0.022(4) 0.003(3) -0.003(3) -0.002(3) N2 0.028(4) 0.019(3) 0.025(4) -0.002(3) 0.001(3) -0.001(3) N3 0.027(3) 0.029(4) 0.026(4) 0.010(3) -0.007(3) -0.011(3) N4 0.028(4) 0.028(4) 0.030(4) 0.008(3) -0.009(3) 0.004(3) N5 0.044(4) 0.031(4) 0.026(4) 0.005(3) 0.010(3) 0.003(4) N6 0.036(4) 0.026(3) 0.027(4) 0.001(3) 0.007(3) -0.002(3) N7 0.030(4) 0.045(5) 0.027(4) 0.006(3) -0.005(3) -0.002(4) N8 0.020(3) 0.038(4) 0.023(4) 0.002(3) -0.003(3) 0.000(3) C1 0.029(4) 0.034(5) 0.030(5) 0.001(4) -0.008(4) 0.009(4) C2 0.034(4) 0.032(4) 0.012(4) 0.008(3) 0.003(3) -0.003(4) C3 0.037(5) 0.024(4) 0.015(4) -0.004(3) -0.001(3) -0.006(4) C4 0.028(4) 0.023(4) 0.019(4) 0.000(3) -0.003(3) 0.002(3) C5 0.039(5) 0.020(4) 0.023(4) 0.004(3) 0.005(4) 0.002(3) C6 0.030(4) 0.025(4) 0.017(4) 0.001(3) -0.002(3) -0.002(3) C7 0.028(4) 0.022(4) 0.031(5) 0.002(3) -0.004(4) 0.001(3) C8 0.022(4) 0.027(4) 0.024(4) 0.003(3) -0.001(3) 0.002(3) C9 0.039(5) 0.034(5) 0.021(5) 0.006(4) 0.001(3) -0.006(4) C10 0.030(5) 0.044(5) 0.014(4) -0.004(3) 0.011(3) -0.007(4) C11 0.020(4) 0.025(4) 0.019(4) 0.006(3) -0.001(3) 0.009(3) C12 0.037(5) 0.050(6) 0.031(5) -0.001(4) 0.008(4) -0.001(4) C13 0.033(5) 0.031(5) 0.037(5) 0.006(4) -0.012(4) -0.005(4) C14 0.027(4) 0.031(4) 0.030(4) 0.006(4) 0.001(3) -0.002(4) C15 0.035(5) 0.040(5) 0.019(4) 0.005(4) -0.002(4) -0.001(4) C16 0.052(6) 0.038(6) 0.048(6) 0.005(4) 0.002(5) 0.005(5) C17 0.061(7) 0.076(8) 0.015(5) 0.007(5) -0.008(4) 0.015(6) C18 0.040(5) 0.041(5) 0.038(6) 0.022(4) 0.000(4) 0.003(4) C19 0.051(5) 0.022(4) 0.022(4) 0.003(4) 0.002(4) -0.010(4) C20 0.043(5) 0.047(5) 0.020(5) 0.006(4) 0.003(4) -0.017(5) C21 0.029(4) 0.043(5) 0.020(4) 0.009(4) -0.004(3) -0.013(4) C22 0.032(5) 0.027(4) 0.021(4) 0.005(3) -0.002(3) -0.010(4) C23 0.029(4) 0.036(4) 0.010(4) 0.006(3) -0.005(3) -0.005(4) C24 0.018(4) 0.032(4) 0.023(4) 0.000(3) -0.008(3) -0.009(3) C25 0.026(4) 0.028(4) 0.025(4) 0.000(3) -0.002(3) -0.004(4) C26 0.043(5) 0.034(5) 0.017(4) 0.007(3) 0.003(4) -0.011(4) C27 0.037(5) 0.035(5) 0.023(4) -0.002(4) 0.001(4) -0.007(4) C28 0.034(5) 0.037(5) 0.018(4) 0.002(3) 0.007(4) 0.003(4) C29 0.043(5) 0.047(6) 0.026(5) -0.002(4) 0.014(4) -0.012(5) C30 0.031(5) 0.078(7) 0.050(7) -0.004(5) 0.017(5) -0.005(6) C31 0.055(7) 0.072(8) 0.030(6) -0.008(5) 0.008(5) -0.019(6) C32 0.042(6) 0.045(6) 0.050(7) 0.005(5) 0.014(5) 0.005(5) C33 0.053(6) 0.029(5) 0.052(6) 0.007(5) 0.019(5) -0.014(5) C34 0.140(13) 0.043(7) 0.062(8) 0.003(6) 0.041(8) -0.026(8) C35 0.053(7) 0.060(8) 0.085(9) 0.031(6) 0.018(6) 0.000(6) C36 0.074(8) 0.043(6) 0.062(7) 0.023(5) 0.013(6) 0.003(6) C37 0.029(4) 0.026(4) 0.025(5) 0.000(3) 0.007(3) 0.007(4) C38 0.045(5) 0.022(4) 0.032(5) -0.009(4) -0.002(4) -0.004(4) C39 0.030(4) 0.017(4) 0.018(4) -0.001(3) -0.001(3) 0.009(3) C40 0.033(5) 0.028(4) 0.031(5) -0.005(4) 0.008(4) 0.005(4) C41 0.033(4) 0.025(4) 0.030(5) -0.001(4) 0.015(4) -0.002(4) C42 0.033(4) 0.028(4) 0.028(5) -0.004(3) -0.008(4) -0.004(4) C43 0.027(4) 0.039(5) 0.038(5) 0.005(4) -0.002(4) 0.006(4) C44 0.038(5) 0.019(4) 0.041(5) -0.004(4) -0.007(4) 0.003(4) C45 0.043(6) 0.027(5) 0.049(6) -0.006(4) 0.011(5) 0.003(4) C46 0.051(6) 0.036(5) 0.025(5) -0.004(4) 0.003(4) 0.008(4) C47 0.030(5) 0.037(5) 0.034(5) 0.006(4) -0.010(4) 0.009(4) C48 0.045(5) 0.034(5) 0.023(5) 0.003(4) -0.010(4) 0.005(4) C49 0.023(4) 0.035(4) 0.027(4) 0.003(3) -0.005(3) 0.003(4) C50 0.033(5) 0.028(4) 0.044(6) 0.011(4) -0.004(4) 0.009(4) C51 0.031(5) 0.044(5) 0.046(6) 0.005(4) -0.007(5) 0.006(4) C52 0.026(4) 0.038(5) 0.035(5) 0.014(4) -0.010(4) 0.007(4) C53 0.037(5) 0.027(4) 0.023(4) 0.009(3) -0.003(4) 0.001(4) C54 0.024(4) 0.029(4) 0.012(4) 0.000(3) -0.002(3) 0.001(3) C55 0.031(4) 0.031(4) 0.018(4) 0.007(3) -0.001(3) 0.012(4) C56 0.024(4) 0.033(4) 0.027(4) -0.009(4) 0.001(3) 0.001(3) O2 0.060(5) 0.069(6) 0.081(6) -0.005(5) -0.032(5) 0.012(4) N9 0.035(5) 0.082(7) 0.045(5) 0.001(5) 0.001(4) 0.003(5) C58 0.039(6) 0.081(9) 0.069(9) -0.034(7) -0.003(6) -0.004(6) C59 0.056(7) 0.087(9) 0.059(8) 0.033(7) -0.009(6) -0.012(7) C60 0.082(9) 0.044(6) 0.053(7) -0.016(5) -0.003(6) 0.009(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 N1 2.049(7) . ? Pd1 N2 2.056(7) . ? Pd1 S3 2.287(2) . ? Pd1 S1 2.295(2) . ? Pd2 N4 2.066(7) . ? Pd2 N3 2.068(7) . ? Pd2 S2 2.290(2) . ? Pd2 S4 2.290(2) . ? Zn1 N5 2.039(8) . ? Zn1 N6 2.049(7) . ? Zn1 Cl2 2.217(3) . ? Zn1 Cl1 2.226(3) . ? Zn2 N8 2.034(6) . ? Zn2 N7 2.048(8) . ? Zn2 Cl3 2.226(3) . ? Zn2 Cl4 2.242(2) . ? S1 C39 1.726(8) . ? S2 C44 1.739(9) . ? S3 C49 1.735(9) . ? S4 C54 1.721(8) . ? N1 C1 1.344(10) . ? N1 C5 1.385(10) . ? N2 C6 1.329(10) . ? N2 C10 1.342(10) . ? N3 C19 1.350(10) . ? N3 C23 1.360(10) . ? N4 C28 1.326(10) . ? N4 C24 1.370(10) . ? N5 C37 1.329(10) . ? N5 C41 1.354(10) . ? N6 C46 1.353(11) . ? N6 C42 1.356(11) . ? N7 C51 1.352(12) . ? N7 C47 1.354(11) . ? N8 C52 1.327(11) . ? N8 C56 1.357(10) . ? C1 C2 1.385(11) . ? C2 C3 1.406(11) . ? C3 C4 1.399(10) . ? C3 C11 1.528(10) . ? C4 C5 1.380(11) . ? C5 C6 1.474(11) . ? C6 C7 1.389(11) . ? C7 C8 1.415(11) . ? C8 C9 1.369(11) . ? C8 C15 1.497(11) . ? C9 C10 1.419(12) . ? C11 C14 1.518(10) . ? C11 C12 1.533(11) . ? C11 C13 1.542(11) . ? C15 C18 1.528(12) . ? C15 C16 1.536(13) . ? C15 C17 1.583(12) . ? C19 C20 1.374(12) . ? C20 C21 1.402(12) . ? C21 C22 1.388(11) . ? C21 C29 1.527(13) . ? C22 C23 1.369(12) . ? C23 C24 1.490(11) . ? C24 C25 1.377(11) . ? C25 C26 1.400(11) . ? C26 C27 1.378(12) . ? C26 C33 1.549(12) . ? C27 C28 1.382(11) . ? C29 C32 1.496(13) . ? C29 C30 1.558(13) . ? C29 C31 1.564(13) . ? C33 C34 1.525(14) . ? C33 C36 1.532(15) . ? C33 C35 1.545(13) . ? C37 C38 1.413(11) . ? C38 C39 1.392(11) . ? C39 C40 1.405(11) . ? C40 C41 1.338(11) . ? C42 C43 1.371(12) . ? C43 C44 1.404(12) . ? C44 C45 1.421(12) . ? C45 C46 1.345(13) . ? C47 C48 1.394(12) . ? C48 C49 1.399(12) . ? C49 C50 1.407(12) . ? C50 C51 1.322(13) . ? C52 C53 1.369(12) . ? C53 C54 1.416(10) . ? C54 C55 1.392(11) . ? C55 C56 1.407(11) . ? O2 C58 1.237(15) . ? N9 C58 1.377(15) . ? N9 C59 1.392(13) . ? N9 C60 1.431(13) . ? O3 C61 1.297(9) . ? N10 C62 1.324(17) . ? N10 C63 1.380(15) . ? N10 C61 1.396(18) . ? O4 C64 1.287(10) . ? N11 C66 1.40(2) . ? N11 C65 1.43(2) . ? N11 C64 1.56(3) . ? 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 Pd1 N2 79.4(3) . . ? N1 Pd1 S3 95.67(18) . . ? N2 Pd1 S3 172.76(19) . . ? N1 Pd1 S1 175.57(19) . . ? N2 Pd1 S1 97.07(19) . . ? S3 Pd1 S1 88.12(9) . . ? N4 Pd2 N3 78.8(3) . . ? N4 Pd2 S2 97.4(2) . . ? N3 Pd2 S2 171.52(19) . . ? N4 Pd2 S4 174.6(2) . . ? N3 Pd2 S4 96.52(18) . . ? S2 Pd2 S4 87.55(9) . . ? N5 Zn1 N6 101.6(3) . . ? N5 Zn1 Cl2 107.0(2) . . ? N6 Zn1 Cl2 108.5(2) . . ? N5 Zn1 Cl1 108.9(2) . . ? N6 Zn1 Cl1 108.5(2) . . ? Cl2 Zn1 Cl1 120.64(11) . . ? N8 Zn2 N7 103.7(3) . . ? N8 Zn2 Cl3 106.5(2) . . ? N7 Zn2 Cl3 108.4(2) . . ? N8 Zn2 Cl4 107.7(2) . . ? N7 Zn2 Cl4 107.9(2) . . ? Cl3 Zn2 Cl4 121.29(10) . . ? C39 S1 Pd1 108.8(3) . . ? C44 S2 Pd2 106.0(3) . . ? C49 S3 Pd1 105.5(3) . . ? C54 S4 Pd2 106.6(3) . . ? C1 N1 C5 117.0(7) . . ? C1 N1 Pd1 128.6(5) . . ? C5 N1 Pd1 114.3(5) . . ? C6 N2 C10 118.6(7) . . ? C6 N2 Pd1 114.4(5) . . ? C10 N2 Pd1 126.2(6) . . ? C19 N3 C23 119.0(7) . . ? C19 N3 Pd2 125.3(6) . . ? C23 N3 Pd2 115.0(5) . . ? C28 N4 C24 118.1(7) . . ? C28 N4 Pd2 126.7(6) . . ? C24 N4 Pd2 115.2(5) . . ? C37 N5 C41 116.5(8) . . ? C37 N5 Zn1 120.1(6) . . ? C41 N5 Zn1 122.2(6) . . ? C46 N6 C42 116.8(7) . . ? C46 N6 Zn1 122.0(5) . . ? C42 N6 Zn1 121.2(6) . . ? C51 N7 C47 115.2(8) . . ? C51 N7 Zn2 123.9(6) . . ? C47 N7 Zn2 120.8(6) . . ? C52 N8 C56 117.5(7) . . ? C52 N8 Zn2 120.3(5) . . ? C56 N8 Zn2 121.8(5) . . ? N1 C1 C2 123.6(7) . . ? C1 C2 C3 120.5(7) . . ? C4 C3 C2 115.4(7) . . ? C4 C3 C11 124.0(7) . . ? C2 C3 C11 120.6(7) . . ? C5 C4 C3 122.4(7) . . ? C4 C5 N1 121.1(7) . . ? C4 C5 C6 125.1(7) . . ? N1 C5 C6 113.7(7) . . ? N2 C6 C7 122.8(7) . . ? N2 C6 C5 116.1(7) . . ? C7 C6 C5 121.1(7) . . ? C6 C7 C8 119.8(7) . . ? C9 C8 C7 116.5(7) . . ? C9 C8 C15 120.5(7) . . ? C7 C8 C15 123.0(7) . . ? C8 C9 C10 120.4(7) . . ? N2 C10 C9 121.4(7) . . ? C14 C11 C3 112.0(6) . . ? C14 C11 C12 109.4(7) . . ? C3 C11 C12 106.8(6) . . ? C14 C11 C13 110.8(7) . . ? C3 C11 C13 107.8(6) . . ? C12 C11 C13 110.0(7) . . ? C8 C15 C18 112.4(7) . . ? C8 C15 C16 109.1(7) . . ? C18 C15 C16 109.1(8) . . ? C8 C15 C17 107.9(7) . . ? C18 C15 C17 108.3(7) . . ? C16 C15 C17 109.9(8) . . ? N3 C19 C20 120.4(8) . . ? C19 C20 C21 121.8(8) . . ? C22 C21 C20 116.3(8) . . ? C22 C21 C29 123.5(8) . . ? C20 C21 C29 120.1(8) . . ? C23 C22 C21 120.5(8) . . ? N3 C23 C22 121.9(7) . . ? N3 C23 C24 114.6(7) . . ? C22 C23 C24 123.5(7) . . ? N4 C24 C25 121.7(7) . . ? N4 C24 C23 114.4(7) . . ? C25 C24 C23 123.9(7) . . ? C24 C25 C26 119.4(8) . . ? C27 C26 C25 118.4(8) . . ? C27 C26 C33 122.1(8) . . ? C25 C26 C33 119.3(8) . . ? C26 C27 C28 119.1(8) . . ? N4 C28 C27 123.3(8) . . ? C32 C29 C21 112.7(7) . . ? C32 C29 C30 109.0(9) . . ? C21 C29 C30 107.8(8) . . ? C32 C29 C31 108.8(8) . . ? C21 C29 C31 109.7(8) . . ? C30 C29 C31 108.7(7) . . ? C34 C33 C36 108.5(10) . . ? C34 C33 C35 109.6(9) . . ? C36 C33 C35 108.4(8) . . ? C34 C33 C26 110.6(8) . . ? C36 C33 C26 108.4(8) . . ? C35 C33 C26 111.2(8) . . ? N5 C37 C38 123.3(8) . . ? C39 C38 C37 118.4(8) . . ? C38 C39 C40 117.1(7) . . ? C38 C39 S1 124.3(6) . . ? C40 C39 S1 118.6(6) . . ? C41 C40 C39 120.0(8) . . ? C40 C41 N5 124.5(8) . . ? N6 C42 C43 122.5(8) . . ? C42 C43 C44 121.8(9) . . ? C43 C44 C45 113.7(8) . . ? C43 C44 S2 125.8(7) . . ? C45 C44 S2 120.4(7) . . ? C46 C45 C44 122.0(9) . . ? C45 C46 N6 123.2(8) . . ? N7 C47 C48 122.1(8) . . ? C47 C48 C49 120.4(8) . . ? C48 C49 C50 116.2(8) . . ? C48 C49 S3 125.6(7) . . ? C50 C49 S3 118.1(7) . . ? C51 C50 C49 119.2(8) . . ? C50 C51 N7 126.9(9) . . ? N8 C52 C53 124.3(8) . . ? C52 C53 C54 120.1(8) . . ? C55 C54 C53 115.7(7) . . ? C55 C54 S4 118.5(6) . . ? C53 C54 S4 125.8(6) . . ? C54 C55 C56 120.8(7) . . ? N8 C56 C55 121.6(8) . . ? C58 N9 C59 120.5(11) . . ? C58 N9 C60 118.1(10) . . ? C59 N9 C60 121.2(10) . . ? O2 C58 N9 127.6(12) . . ? C62 N10 C63 121.8(12) . . ? C62 N10 C61 121.8(12) . . ? C63 N10 C61 116.0(12) . . ? O3 C61 N10 119.3(16) . . ? C66 N11 C65 106.0(18) . . ? C66 N11 C64 107.6(18) . . ? C65 N11 C64 145(2) . . ? O4 C64 N11 112(3) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.586 _refine_diff_density_min -0.879 _refine_diff_density_rms 0.142