# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Weigand, Wolfgang' _publ_contact_author_email c8wewo@uni-jena.de _publ_section_title ; Structure, solution chemistry, antiproliferative actions and protein binding properties of non-conventional platinum(II) compounds with sulfur and phosphorus donors ; loop_ _publ_author_name W.Weigand C.Rothenburger C.Mugge A.Beyer H.Gorls C.Gabbiani A.Casini E.Michelucci I.Landini S.Nobili E.Mini L.Messori # Attachment '- dalton.cif' data_FO3203 _database_code_depnum_ccdc_archive 'CCDC 776102' #TrackingRef '- dalton.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C39 H36 O P2 Pt S2, C H Cl3' _chemical_formula_sum 'C40 H37 Cl3 O P2 Pt S2' _chemical_formula_weight 961.20 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'p -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.6368(13) _cell_length_b 12.5618(13) _cell_length_c 14.784(2) _cell_angle_alpha 87.969(8) _cell_angle_beta 78.924(7) _cell_angle_gamma 64.993(4) _cell_volume 1919.4(4) _cell_formula_units_Z 2 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used 12394 _cell_measurement_theta_min 1.97 _cell_measurement_theta_max 27.47 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.03 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.663 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 952 _exptl_absorpt_coefficient_mu 4.088 _exptl_absorpt_correction_type NONE _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 183(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 KappaCCD _diffrn_measurement_method 'phi- + omega-scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12394 _diffrn_reflns_av_R_equivalents 0.0557 _diffrn_reflns_av_sigmaI/netI 0.1194 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.97 _diffrn_reflns_theta_max 27.47 _reflns_number_total 8227 _reflns_number_gt 4729 _reflns_threshold_expression >2sigma(I) _computing_data_collection COLLECT _computing_cell_refinement DENZO _computing_data_reduction DENZO _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL/PC _computing_publication_material SHELXL-97 _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^)+(0.0412P)^2^+10.7195P] 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 8227 _refine_ls_number_parameters 488 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1701 _refine_ls_R_factor_gt 0.0894 _refine_ls_wR_factor_ref 0.1753 _refine_ls_wR_factor_gt 0.1486 _refine_ls_goodness_of_fit_ref 1.126 _refine_ls_restrained_S_all 1.126 _refine_ls_shift/su_max 0.043 _refine_ls_shift/su_mean 0.002 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 Pt Pt -0.00703(4) -0.82735(4) -0.74063(5) 0.0691(2) Uani 1 1 d . . . P1 P -0.1278(2) -0.9317(2) -0.7126(2) 0.0406(7) Uani 1 1 d . A . P2 P -0.1662(3) -0.6552(2) -0.7748(2) 0.0527(8) Uani 1 1 d . A . S1 S 0.1611(14) -0.9872(12) -0.6910(8) 0.054(3) Uani 0.562(10) 1 d P A 1 S1A S 0.1766(17) -0.9988(17) -0.7341(11) 0.056(4) Uani 0.438(10) 1 d P A 2 C2 C 0.2747(11) -0.8332(11) -0.7366(12) 0.075(4) Uani 1 1 d . . . H2A H 0.3281 -0.7959 -0.7181 0.090 Uiso 0.562(10) 1 calc PR A 1 H2B H 0.3504 -0.8180 -0.7615 0.090 Uiso 0.438(10) 1 d PR A 2 C1 C 0.278(2) -0.9294(17) -0.664(2) 0.067(7) Uani 0.562(10) 1 d P A 1 H1A H 0.2502 -0.8942 -0.6003 0.080 Uiso 0.562(10) 1 calc PR A 1 H1B H 0.3662 -0.9935 -0.6707 0.080 Uiso 0.562(10) 1 calc PR A 1 C3 C 0.333(2) -0.877(2) -0.8285(15) 0.064(6) Uani 0.562(10) 1 d P A 1 H3A H 0.2953 -0.9285 -0.8475 0.076 Uiso 0.562(10) 1 calc PR A 1 H3B H 0.4268 -0.9244 -0.8334 0.076 Uiso 0.562(10) 1 calc PR A 1 O3 O 0.3102(18) -0.7808(16) -0.8871(13) 0.096(6) Uani 0.562(10) 1 d P A 1 H3C H 0.3447 -0.8064 -0.9419 0.144 Uiso 0.562(10) 1 calc PR A 1 S2 S 0.1117(5) -0.7172(4) -0.7220(6) 0.055(2) Uani 0.562(10) 1 d P A 1 S2A S 0.1376(7) -0.7407(6) -0.8011(7) 0.052(3) Uani 0.438(10) 1 d P A 2 C1A C 0.307(3) -0.954(2) -0.757(3) 0.078(11) Uani 0.438(10) 1 d P A 2 H1AA H 0.3730 -1.0026 -0.7210 0.094 Uiso 0.438(10) 1 calc PR A 2 H1AB H 0.3481 -0.9724 -0.8231 0.094 Uiso 0.438(10) 1 calc PR A 2 C3A C 0.231(3) -0.799(4) -0.630(2) 0.085(11) Uani 0.438(10) 1 d P A 2 H3AA H 0.1689 -0.8301 -0.6004 0.102 Uiso 0.438(10) 1 calc PR A 2 H3AB H 0.3069 -0.8296 -0.5991 0.102 Uiso 0.438(10) 1 calc PR A 2 O3A O 0.171(3) -0.669(3) -0.6248(17) 0.124(11) Uani 0.438(10) 1 d P A 2 H3AC H 0.1451 -0.6446 -0.5693 0.186 Uiso 0.438(10) 1 calc PR A 2 C4 C -0.0452(9) -1.0803(8) -0.6738(8) 0.042(3) Uani 1 1 d . . . C5 C -0.0600(9) -1.1078(9) -0.5823(8) 0.046(3) Uani 1 1 d . A . H5A H -0.1173 -1.0488 -0.5362 0.055 Uiso 1 1 calc R . . C6 C 0.0082(11) -1.2208(10) -0.5577(9) 0.058(3) Uani 1 1 d . . . H6A H -0.0024 -1.2393 -0.4946 0.069 Uiso 1 1 calc R A . C7 C 0.0924(11) -1.3079(10) -0.6244(10) 0.062(3) Uani 1 1 d . A . H7A H 0.1390 -1.3857 -0.6070 0.075 Uiso 1 1 calc R . . C8 C 0.1080(11) -1.2819(10) -0.7144(10) 0.061(3) Uani 1 1 d . . . H8A H 0.1654 -1.3417 -0.7600 0.073 Uiso 1 1 calc R A . C9 C 0.0402(10) -1.1679(9) -0.7405(9) 0.055(3) Uani 1 1 d . A . H9A H 0.0522 -1.1499 -0.8036 0.066 Uiso 1 1 calc R . . C10 C -0.1851(10) -0.9637(9) -0.8089(8) 0.049(3) Uani 1 1 d . . . C11 C -0.2562(11) -1.0295(9) -0.7977(9) 0.057(3) Uani 1 1 d . A . H11A H -0.2799 -1.0521 -0.7376 0.068 Uiso 1 1 calc R . . C12 C -0.2943(14) -1.0638(11) -0.8705(14) 0.084(5) Uani 1 1 d . . . H12A H -0.3465 -1.1059 -0.8606 0.100 Uiso 1 1 calc R A . C13 C -0.254(2) -1.0352(15) -0.9566(14) 0.100(6) Uani 1 1 d . A . H13A H -0.2771 -1.0603 -1.0076 0.120 Uiso 1 1 calc R . . C14 C -0.1834(16) -0.9718(15) -0.9719(10) 0.091(6) Uani 1 1 d . . . H14A H -0.1591 -0.9517 -1.0329 0.109 Uiso 1 1 calc R A . C15 C -0.1460(12) -0.9360(10) -0.8992(10) 0.070(4) Uani 1 1 d . A . H15A H -0.0946 -0.8932 -0.9103 0.084 Uiso 1 1 calc R . . C16 C -0.2660(10) -0.8611(9) -0.6178(8) 0.047(3) Uani 1 1 d . . . C17 C -0.3897(10) -0.8476(9) -0.6171(8) 0.051(3) Uani 1 1 d . A . H17A H -0.4098 -0.8731 -0.6693 0.061 Uiso 1 1 calc R . . C18 C -0.4838(11) -0.7969(12) -0.5401(10) 0.071(4) Uani 1 1 d . . . H18A H -0.5694 -0.7872 -0.5397 0.085 Uiso 1 1 calc R A . C19 C -0.4569(13) -0.7596(12) -0.4629(11) 0.081(4) Uani 1 1 d . A . H19A H -0.5230 -0.7247 -0.4100 0.097 Uiso 1 1 calc R . . C20 C -0.3345(13) -0.7738(11) -0.4643(8) 0.067(4) Uani 1 1 d . . . H20A H -0.3149 -0.7494 -0.4114 0.080 Uiso 1 1 calc R A . C21 C -0.2382(12) -0.8228(10) -0.5405(9) 0.060(3) Uani 1 1 d . A . H21A H -0.1534 -0.8306 -0.5407 0.072 Uiso 1 1 calc R . . C22 C -0.3354(9) -0.6285(8) -0.7526(8) 0.045(3) Uani 1 1 d . . . C23 C -0.3850(10) -0.6693(8) -0.8156(9) 0.053(3) Uani 1 1 d . A . H23A H -0.3283 -0.7125 -0.8701 0.064 Uiso 1 1 calc R . . C24 C -0.5120(11) -0.6496(9) -0.8017(8) 0.052(3) Uani 1 1 d . . . H24A H -0.5440 -0.6758 -0.8466 0.063 Uiso 1 1 calc R A . C25 C -0.5931(10) -0.5902(10) -0.7201(10) 0.063(3) Uani 1 1 d . A . H25A H -0.6814 -0.5769 -0.7093 0.075 Uiso 1 1 calc R . . C26 C -0.5491(11) -0.5502(10) -0.6547(10) 0.060(3) Uani 1 1 d . . . H26A H -0.6061 -0.5095 -0.5995 0.072 Uiso 1 1 calc R A . C27 C -0.4210(10) -0.5703(9) -0.6707(9) 0.056(3) Uani 1 1 d . A . H27A H -0.3896 -0.5442 -0.6253 0.067 Uiso 1 1 calc R . . C28 C -0.1399(11) -0.6221(9) -0.8958(9) 0.059(3) Uani 1 1 d . . . C29 C -0.2321(12) -0.5262(10) -0.9304(9) 0.065(4) Uani 1 1 d . A . H29A H -0.3125 -0.4808 -0.8910 0.078 Uiso 1 1 calc R . . C30 C -0.2098(14) -0.4953(11) -1.0210(10) 0.074(4) Uani 1 1 d . . . H30A H -0.2745 -0.4300 -1.0433 0.089 Uiso 1 1 calc R A . C31 C -0.0929(16) -0.5602(12) -1.0783(10) 0.085(5) Uani 1 1 d . A . H31A H -0.0768 -0.5392 -1.1402 0.103 Uiso 1 1 calc R . . C32 C 0.0004(15) -0.6553(12) -1.0462(12) 0.096(5) Uani 1 1 d . . . H32A H 0.0808 -0.6994 -1.0862 0.115 Uiso 1 1 calc R A . C33 C -0.0217(12) -0.6871(10) -0.9566(11) 0.077(4) Uani 1 1 d . A . H33A H 0.0432 -0.7535 -0.9355 0.092 Uiso 1 1 calc R . . C34 C -0.1719(10) -0.5318(9) -0.7071(10) 0.055(3) Uani 1 1 d . . . C35 C -0.1868(11) -0.4258(9) -0.7468(9) 0.059(3) Uani 1 1 d . A . H35A H -0.1924 -0.4158 -0.8101 0.071 Uiso 1 1 calc R . . C36 C -0.1933(12) -0.3345(11) -0.6922(12) 0.074(4) Uani 1 1 d . . . H36A H -0.2016 -0.2622 -0.7188 0.089 Uiso 1 1 calc R A . C37 C -0.1878(11) -0.3478(11) -0.6000(12) 0.070(4) Uani 1 1 d . A . H37A H -0.1943 -0.2842 -0.5633 0.084 Uiso 1 1 calc R . . C38 C -0.1729(13) -0.4521(13) -0.5611(11) 0.076(4) Uani 1 1 d . . . H38A H -0.1680 -0.4615 -0.4977 0.091 Uiso 1 1 calc R A . C39 C -0.1652(13) -0.5443(12) -0.6150(11) 0.073(4) Uani 1 1 d . A . H39A H -0.1551 -0.6167 -0.5880 0.088 Uiso 1 1 calc R . . C1M C 0.3982(13) -0.2356(13) -0.8761(10) 0.087(5) Uani 1 1 d . . . H1MA H 0.3186 -0.1618 -0.8547 0.104 Uiso 1 1 calc R . . Cl1M Cl 0.4662(5) -0.2953(5) -0.7802(3) 0.145(2) Uani 1 1 d . . . Cl2M Cl 0.3541(6) -0.3296(4) -0.9270(3) 0.1203(16) Uani 1 1 d . . . Cl3M Cl 0.5057(4) -0.1986(3) -0.9567(3) 0.0934(12) 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 Pt 0.0329(2) 0.0329(2) 0.1363(6) 0.0184(2) -0.0174(3) -0.00978(17) P1 0.0301(13) 0.0283(13) 0.0551(19) 0.0018(12) -0.0054(13) -0.0057(10) P2 0.0357(15) 0.0311(14) 0.080(2) 0.0104(14) -0.0031(15) -0.0073(12) S1 0.036(4) 0.030(4) 0.089(9) -0.001(6) -0.011(6) -0.008(3) S1A 0.025(5) 0.041(6) 0.090(11) 0.001(8) -0.014(8) -0.002(4) C2 0.041(7) 0.067(9) 0.127(15) 0.011(9) -0.027(8) -0.028(6) C1 0.053(13) 0.029(10) 0.10(2) -0.003(12) -0.001(13) -0.004(9) C3 0.071(15) 0.059(14) 0.052(15) -0.005(12) 0.006(12) -0.027(12) O3 0.098(14) 0.097(14) 0.090(14) 0.012(11) -0.006(11) -0.044(11) S2 0.033(3) 0.035(3) 0.085(7) -0.006(3) 0.002(3) -0.008(2) S2A 0.052(4) 0.046(4) 0.053(7) -0.006(4) 0.005(4) -0.024(3) C1A 0.036(15) 0.050(18) 0.14(4) 0.00(2) -0.014(19) -0.010(13) C3A 0.09(2) 0.12(3) 0.07(3) -0.01(2) -0.01(2) -0.08(2) O3A 0.14(3) 0.15(3) 0.090(19) -0.060(18) 0.034(17) -0.09(2) C4 0.030(5) 0.032(5) 0.057(8) 0.000(5) -0.004(5) -0.009(4) C5 0.035(5) 0.051(6) 0.055(8) 0.018(5) -0.012(5) -0.022(5) C6 0.050(7) 0.061(7) 0.061(8) 0.019(7) -0.015(6) -0.021(6) C7 0.043(7) 0.045(7) 0.095(11) 0.022(7) -0.024(7) -0.013(6) C8 0.047(7) 0.040(6) 0.077(10) 0.001(6) -0.003(6) -0.005(5) C9 0.050(7) 0.042(6) 0.069(8) 0.010(6) -0.016(6) -0.014(5) C10 0.042(6) 0.033(5) 0.064(9) 0.004(5) -0.020(6) -0.004(5) C11 0.051(7) 0.038(6) 0.069(9) -0.002(6) -0.020(6) -0.004(5) C12 0.073(9) 0.051(8) 0.120(15) -0.008(9) -0.057(10) -0.003(7) C13 0.115(15) 0.068(11) 0.085(15) -0.026(10) -0.056(12) 0.010(10) C14 0.085(11) 0.076(11) 0.049(10) -0.009(8) -0.028(9) 0.032(8) C15 0.058(8) 0.048(7) 0.065(10) 0.009(7) -0.007(7) 0.011(6) C16 0.039(6) 0.039(6) 0.054(8) 0.011(5) -0.011(5) -0.007(5) C17 0.037(6) 0.053(6) 0.053(8) -0.008(6) -0.003(6) -0.011(5) C18 0.038(7) 0.085(9) 0.076(10) -0.019(8) -0.004(7) -0.014(6) C19 0.058(9) 0.084(10) 0.079(11) -0.008(8) 0.006(8) -0.017(8) C20 0.068(9) 0.073(8) 0.037(8) -0.014(6) 0.002(7) -0.012(7) C21 0.052(7) 0.056(7) 0.072(9) 0.000(7) -0.020(7) -0.019(6) C22 0.038(6) 0.025(5) 0.057(8) 0.006(5) -0.004(6) -0.002(4) C23 0.045(7) 0.027(5) 0.070(9) -0.001(5) 0.001(6) -0.004(5) C24 0.047(7) 0.043(6) 0.061(8) -0.002(6) -0.013(6) -0.013(5) C25 0.028(6) 0.048(7) 0.093(10) 0.013(7) -0.010(7) -0.001(5) C26 0.038(6) 0.049(7) 0.081(10) 0.000(6) 0.002(6) -0.011(5) C27 0.043(6) 0.045(6) 0.072(9) 0.003(6) -0.004(6) -0.015(5) C28 0.049(7) 0.034(6) 0.082(9) 0.003(6) 0.006(6) -0.012(5) C29 0.055(7) 0.046(7) 0.072(10) 0.000(6) 0.011(7) -0.010(6) C30 0.081(10) 0.049(7) 0.069(10) 0.000(7) 0.014(8) -0.017(7) C31 0.115(13) 0.058(8) 0.071(10) -0.002(7) 0.019(9) -0.040(9) C32 0.081(10) 0.050(8) 0.123(14) -0.006(9) 0.047(10) -0.022(8) C33 0.053(8) 0.034(6) 0.120(12) -0.002(7) 0.023(8) -0.013(6) C34 0.036(6) 0.032(5) 0.089(10) 0.009(6) -0.002(6) -0.012(5) C35 0.059(7) 0.043(6) 0.069(9) 0.010(6) 0.002(6) -0.022(6) C36 0.059(8) 0.044(7) 0.108(13) 0.002(8) 0.005(8) -0.020(6) C37 0.047(7) 0.059(8) 0.102(12) -0.004(8) 0.005(7) -0.027(6) C38 0.079(10) 0.078(10) 0.082(10) 0.009(8) -0.020(8) -0.044(8) C39 0.083(10) 0.061(8) 0.082(11) 0.026(8) -0.028(8) -0.033(7) C1M 0.059(8) 0.091(11) 0.087(11) -0.004(9) -0.020(8) -0.007(8) Cl1M 0.107(3) 0.152(4) 0.065(3) -0.015(3) -0.025(2) 0.055(3) Cl2M 0.169(5) 0.108(3) 0.091(3) 0.006(3) -0.014(3) -0.070(3) Cl3M 0.082(3) 0.079(2) 0.107(3) -0.007(2) -0.032(2) -0.017(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt P1 2.271(3) . ? Pt S1A 2.321(18) . ? Pt P2 2.293(3) . ? Pt S2A 2.392(7) . ? Pt S1 2.350(15) . ? Pt S2 2.385(5) . ? P1 C10 1.806(12) . ? P1 C16 1.832(11) . ? P1 C4 1.832(9) . ? P2 C22 1.816(11) . ? P2 C28 1.819(13) . ? P2 C34 1.846(12) . ? S1 C1 1.90(3) . ? S1A C1A 1.80(3) . ? C2 C3 1.41(3) . ? C2 C1A 1.43(3) . ? C2 C3A 1.58(3) . ? C2 C1 1.58(3) . ? C2 S2 1.816(13) . ? C2 S2A 1.935(14) . ? C2 H2A 1.0000 . ? C2 H2B 0.9800 . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C3 O3 1.42(3) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? O3 H3C 0.8400 . ? C1A H1AA 0.9900 . ? C1A H1AB 0.9900 . ? C3A O3A 1.47(4) . ? C3A H3AA 0.9900 . ? C3A H3AB 0.9900 . ? O3A H3AC 0.8400 . ? C4 C5 1.380(14) . ? C4 C9 1.396(15) . ? C5 C6 1.378(14) . ? C5 H5A 0.9500 . ? C6 C7 1.389(17) . ? C6 H6A 0.9500 . ? C7 C8 1.355(16) . ? C7 H7A 0.9500 . ? C8 C9 1.395(14) . ? C8 H8A 0.9500 . ? C9 H9A 0.9500 . ? C10 C11 1.382(15) . ? C10 C15 1.406(16) . ? C11 C12 1.385(18) . ? C11 H11A 0.9500 . ? C12 C13 1.36(2) . ? C12 H12A 0.9500 . ? C13 C14 1.36(2) . ? C13 H13A 0.9500 . ? C14 C15 1.39(2) . ? C14 H14A 0.9500 . ? C15 H15A 0.9500 . ? C16 C17 1.374(14) . ? C16 C21 1.398(16) . ? C17 C18 1.373(16) . ? C17 H17A 0.9500 . ? C18 C19 1.385(18) . ? C18 H18A 0.9500 . ? C19 C20 1.354(18) . ? C19 H19A 0.9500 . ? C20 C21 1.372(16) . ? C20 H20A 0.9500 . ? C21 H21A 0.9500 . ? C22 C23 1.397(15) . ? C22 C27 1.406(15) . ? C23 C24 1.365(15) . ? C23 H23A 0.9500 . ? C24 C25 1.390(17) . ? C24 H24A 0.9500 . ? C25 C26 1.375(17) . ? C25 H25A 0.9500 . ? C26 C27 1.376(15) . ? C26 H26A 0.9500 . ? C27 H27A 0.9500 . ? C28 C29 1.393(15) . ? C28 C33 1.412(16) . ? C29 C30 1.388(17) . ? C29 H29A 0.9500 . ? C30 C31 1.378(18) . ? C30 H30A 0.9500 . ? C31 C32 1.38(2) . ? C31 H31A 0.9500 . ? C32 C33 1.38(2) . ? C32 H32A 0.9500 . ? C33 H33A 0.9500 . ? C34 C39 1.379(17) . ? C34 C35 1.392(14) . ? C35 C36 1.393(17) . ? C35 H35A 0.9500 . ? C36 C37 1.377(18) . ? C36 H36A 0.9500 . ? C37 C38 1.368(17) . ? C37 H37A 0.9500 . ? C38 C39 1.390(18) . ? C38 H38A 0.9500 . ? C39 H39A 0.9500 . ? C1M Cl2M 1.717(16) . ? C1M Cl1M 1.746(14) . ? C1M Cl3M 1.754(16) . ? C1M H1MA 1.0000 . ? 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 P1 Pt S1A 89.3(5) . . ? P1 Pt P2 97.22(10) . . ? S1A Pt P2 168.8(4) . . ? P1 Pt S2A 167.8(2) . . ? S1A Pt S2A 86.4(5) . . ? P2 Pt S2A 85.38(18) . . ? P1 Pt S1 88.0(4) . . ? S1A Pt S1 15.6(4) . . ? P2 Pt S1 171.8(3) . . ? S2A Pt S1 90.9(4) . . ? P1 Pt S2 163.2(2) . . ? S1A Pt S2 88.8(5) . . ? P2 Pt S2 87.51(14) . . ? S2A Pt S2 28.2(2) . . ? S1 Pt S2 85.8(4) . . ? C10 P1 C16 108.7(5) . . ? C10 P1 C4 100.4(5) . . ? C16 P1 C4 103.1(5) . . ? C10 P1 Pt 117.2(4) . . ? C16 P1 Pt 110.9(4) . . ? C4 P1 Pt 115.3(3) . . ? C22 P2 C28 101.8(5) . . ? C22 P2 C34 101.6(5) . . ? C28 P2 C34 107.0(5) . . ? C22 P2 Pt 122.5(3) . . ? C28 P2 Pt 113.3(4) . . ? C34 P2 Pt 109.2(4) . . ? C1 S1 Pt 106.6(9) . . ? C1A S1A Pt 104.5(12) . . ? C3 C2 C1A 63(2) . . ? C3 C2 C3A 170.6(19) . . ? C1A C2 C3A 113(2) . . ? C3 C2 C1 115.3(16) . . ? C1A C2 C1 53.6(17) . . ? C3A C2 C1 59.3(17) . . ? C3 C2 S2 114.7(13) . . ? C1A C2 S2 123.9(13) . . ? C3A C2 S2 74.7(16) . . ? C1 C2 S2 109.4(12) . . ? C3 C2 S2A 78.7(12) . . ? C1A C2 S2A 107.0(16) . . ? C3A C2 S2A 110.7(16) . . ? C1 C2 S2A 128.5(11) . . ? S2 C2 S2A 36.0(3) . . ? C3 C2 H2A 105.5 . . ? C1A C2 H2A 130.0 . . ? C3A C2 H2A 70.5 . . ? C1 C2 H2A 105.5 . . ? S2 C2 H2A 105.5 . . ? S2A C2 H2A 118.4 . . ? C3 C2 H2B 66.2 . . ? C1A C2 H2B 108.3 . . ? C3A C2 H2B 109.4 . . ? C1 C2 H2B 122.7 . . ? S2 C2 H2B 121.5 . . ? S2A C2 H2B 108.4 . . ? H2A C2 H2B 39.3 . . ? C2 C1 S1 105.2(15) . . ? C2 C1 H1A 110.7 . . ? S1 C1 H1A 110.7 . . ? C2 C1 H1B 110.7 . . ? S1 C1 H1B 110.7 . . ? H1A C1 H1B 108.8 . . ? C2 C3 O3 109.0(18) . . ? C2 C3 H2B 41.4 . . ? O3 C3 H2B 91.6 . . ? C2 C3 H3A 109.9 . . ? O3 C3 H3A 109.9 . . ? H2B C3 H3A 150.1 . . ? C2 C3 H3B 109.9 . . ? O3 C3 H3B 109.9 . . ? H2B C3 H3B 81.9 . . ? H3A C3 H3B 108.3 . . ? C3 O3 H3C 109.5 . . ? C2 S2 Pt 101.0(5) . . ? C2 S2A Pt 97.2(5) . . ? C2 C1A S1A 116.8(19) . . ? C2 C1A H1AA 108.1 . . ? S1A C1A H1AA 108.1 . . ? C2 C1A H1AB 108.1 . . ? S1A C1A H1AB 108.1 . . ? H1AA C1A H1AB 107.3 . . ? O3A C3A C2 104(2) . . ? O3A C3A H3AA 110.9 . . ? C2 C3A H3AA 110.9 . . ? O3A C3A H3AB 110.9 . . ? C2 C3A H3AB 110.9 . . ? H3AA C3A H3AB 108.9 . . ? C3A O3A H3AC 109.5 . . ? C5 C4 C9 119.2(9) . . ? C5 C4 P1 123.3(8) . . ? C9 C4 P1 117.5(8) . . ? C6 C5 C4 120.2(11) . . ? C6 C5 H5A 119.9 . . ? C4 C5 H5A 119.9 . . ? C5 C6 C7 120.5(11) . . ? C5 C6 H6A 119.8 . . ? C7 C6 H6A 119.8 . . ? C8 C7 C6 119.9(10) . . ? C8 C7 H7A 120.0 . . ? C6 C7 H7A 120.0 . . ? C7 C8 C9 120.4(12) . . ? C7 C8 H8A 119.8 . . ? C9 C8 H8A 119.8 . . ? C4 C9 C8 119.9(11) . . ? C4 C9 H9A 120.0 . . ? C8 C9 H9A 120.0 . . ? C11 C10 C15 117.5(12) . . ? C11 C10 P1 120.5(9) . . ? C15 C10 P1 121.5(10) . . ? C10 C11 C12 122.8(14) . . ? C10 C11 H11A 118.6 . . ? C12 C11 H11A 118.6 . . ? C13 C12 C11 117.7(16) . . ? C13 C12 H12A 121.1 . . ? C11 C12 H12A 121.1 . . ? C14 C13 C12 122.1(16) . . ? C14 C13 H13A 119.0 . . ? C12 C13 H13A 119.0 . . ? C13 C14 C15 120.5(16) . . ? C13 C14 H14A 119.8 . . ? C15 C14 H14A 119.8 . . ? C14 C15 C10 119.3(15) . . ? C14 C15 H15A 120.3 . . ? C10 C15 H15A 120.3 . . ? C17 C16 C21 119.6(11) . . ? C17 C16 P1 125.0(9) . . ? C21 C16 P1 115.4(8) . . ? C18 C17 C16 119.2(11) . . ? C18 C17 H17A 120.4 . . ? C16 C17 H17A 120.4 . . ? C17 C18 C19 121.6(12) . . ? C17 C18 H18A 119.2 . . ? C19 C18 H18A 119.2 . . ? C20 C19 C18 118.6(13) . . ? C20 C19 H19A 120.7 . . ? C18 C19 H19A 120.7 . . ? C19 C20 C21 121.4(13) . . ? C19 C20 H20A 119.3 . . ? C21 C20 H20A 119.3 . . ? C20 C21 C16 119.5(11) . . ? C20 C21 H21A 120.2 . . ? C16 C21 H21A 120.2 . . ? C23 C22 C27 117.0(10) . . ? C23 C22 P2 120.9(8) . . ? C27 C22 P2 122.0(9) . . ? C24 C23 C22 122.5(11) . . ? C24 C23 H23A 118.8 . . ? C22 C23 H23A 118.8 . . ? C23 C24 C25 118.3(12) . . ? C23 C24 H24A 120.9 . . ? C25 C24 H24A 120.9 . . ? C26 C25 C24 121.8(11) . . ? C26 C25 H25A 119.1 . . ? C24 C25 H25A 119.1 . . ? C25 C26 C27 118.8(12) . . ? C25 C26 H26A 120.6 . . ? C27 C26 H26A 120.6 . . ? C26 C27 C22 121.6(12) . . ? C26 C27 H27A 119.2 . . ? C22 C27 H27A 119.2 . . ? C29 C28 C33 117.3(12) . . ? C29 C28 P2 121.1(9) . . ? C33 C28 P2 121.4(10) . . ? C30 C29 C28 121.7(11) . . ? C30 C29 H29A 119.1 . . ? C28 C29 H29A 119.1 . . ? C31 C30 C29 119.4(13) . . ? C31 C30 H30A 120.3 . . ? C29 C30 H30A 120.3 . . ? C32 C31 C30 120.4(13) . . ? C32 C31 H31A 119.8 . . ? C30 C31 H31A 119.8 . . ? C31 C32 C33 120.5(13) . . ? C31 C32 H32A 119.8 . . ? C33 C32 H32A 119.8 . . ? C32 C33 C28 120.7(12) . . ? C32 C33 H33A 119.7 . . ? C28 C33 H33A 119.7 . . ? C39 C34 C35 119.8(12) . . ? C39 C34 P2 119.1(9) . . ? C35 C34 P2 121.1(11) . . ? C36 C35 C34 118.8(13) . . ? C36 C35 H35A 120.6 . . ? C34 C35 H35A 120.6 . . ? C37 C36 C35 120.7(12) . . ? C37 C36 H36A 119.6 . . ? C35 C36 H36A 119.6 . . ? C38 C37 C36 120.4(14) . . ? C38 C37 H37A 119.8 . . ? C36 C37 H37A 119.8 . . ? C37 C38 C39 119.5(14) . . ? C37 C38 H38A 120.3 . . ? C39 C38 H38A 120.3 . . ? C34 C39 C38 120.8(12) . . ? C34 C39 H39A 119.6 . . ? C38 C39 H39A 119.6 . . ? Cl2M C1M Cl1M 111.8(9) . . ? Cl2M C1M Cl3M 110.3(8) . . ? Cl1M C1M Cl3M 110.5(8) . . ? Cl2M C1M H1MA 108.0 . . ? Cl1M C1M H1MA 108.0 . . ? Cl3M C1M H1MA 108.0 . . ? _diffrn_measured_fraction_theta_max 0.935 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.935 _refine_diff_density_max 1.446 _refine_diff_density_min -1.670 _refine_diff_density_rms 0.129 #==== END data_FO3147 _database_code_depnum_ccdc_archive 'CCDC 776103' #TrackingRef '- dalton.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C29 H30 O P2 Pt S2), C H4 O, 2(H2 O)' _chemical_formula_sum 'C29.50 H34 O2.50 P2 Pt S2' _chemical_formula_weight 749.72 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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' 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 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' 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 9.0685(3) _cell_length_b 28.1277(9) _cell_length_c 12.3952(3) _cell_angle_alpha 90.00 _cell_angle_beta 103.898(2) _cell_angle_gamma 90.00 _cell_volume 3069.16(16) _cell_formula_units_Z 4 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used 18527 _cell_measurement_theta_min 3.17 _cell_measurement_theta_max 27.47 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.04 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.623 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1484 _exptl_absorpt_coefficient_mu 4.839 _exptl_absorpt_correction_type NONE _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 183(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 KappaCCD _diffrn_measurement_method 'phi- + omega-scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18527 _diffrn_reflns_av_R_equivalents 0.0698 _diffrn_reflns_av_sigmaI/netI 0.0879 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -36 _diffrn_reflns_limit_k_max 35 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.17 _diffrn_reflns_theta_max 27.47 _reflns_number_total 6922 _reflns_number_gt 4638 _reflns_threshold_expression >2sigma(I) _computing_data_collection COLLECT _computing_cell_refinement DENZO _computing_data_reduction DENZO _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL/PC _computing_publication_material SHELXL-97 _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^)+(0.1068P)^2^+5.0322P] 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 6922 _refine_ls_number_parameters 333 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1072 _refine_ls_R_factor_gt 0.0638 _refine_ls_wR_factor_ref 0.1845 _refine_ls_wR_factor_gt 0.1612 _refine_ls_goodness_of_fit_ref 1.014 _refine_ls_restrained_S_all 1.014 _refine_ls_shift/su_max 0.002 _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 Pt Pt 0.33769(4) 0.348775(12) 0.16027(3) 0.03158(15) Uani 1 1 d . . . S1 S 0.3079(4) 0.42889(10) 0.1969(2) 0.0537(7) Uani 1 1 d . . . S2 S 0.5053(4) 0.33720(11) 0.3347(2) 0.0525(7) Uani 1 1 d . . . P1 P 0.1617(3) 0.35860(9) -0.0003(2) 0.0330(5) Uani 1 1 d . . . P2 P 0.3532(3) 0.27301(9) 0.10412(19) 0.0318(5) Uani 1 1 d . . . O1 O 0.432(2) 0.4565(6) 0.4746(15) 0.100(5) Uiso 0.639(15) 1 d P A 1 H1 H 0.4588 0.4849 0.4709 0.150 Uiso 0.639(15) 1 calc PR A 1 O1A O 0.630(4) 0.4444(11) 0.476(3) 0.100(5) Uiso 0.361(15) 1 d P A 2 H1OA H 0.6453 0.4727 0.4601 0.150 Uiso 0.361(15) 1 calc PR A 2 C1 C 0.4840(17) 0.4477(5) 0.2955(11) 0.076(4) Uani 1 1 d . A . H1A H 0.5719 0.4364 0.2682 0.091 Uiso 1 1 calc R . . H1B H 0.4877 0.4828 0.2978 0.091 Uiso 1 1 calc R . . C2 C 0.4984(16) 0.4293(4) 0.4106(10) 0.063(3) Uani 1 1 d . . . H2A H 0.6095 0.4297 0.4469 0.076 Uiso 0.639(15) 1 calc PR A 1 H2B H 0.4212 0.4488 0.4365 0.076 Uiso 0.361(15) 1 d PR A 2 C3 C 0.4480(15) 0.3812(4) 0.4229(9) 0.057(3) Uani 1 1 d . A . H3A H 0.3357 0.3812 0.4074 0.068 Uiso 1 1 calc R . . H3B H 0.4872 0.3714 0.5012 0.068 Uiso 1 1 calc R . . C4 C 0.0986(11) 0.2994(3) -0.0516(8) 0.039(2) Uani 1 1 d . . . H4A H 0.0298 0.2860 -0.0083 0.047 Uiso 1 1 calc R . . H4B H 0.0431 0.3011 -0.1307 0.047 Uiso 1 1 calc R . . C5 C 0.2402(12) 0.2682(3) -0.0386(8) 0.037(2) Uani 1 1 d . . . H5A H 0.3008 0.2788 -0.0908 0.045 Uiso 1 1 calc R . . H5B H 0.2100 0.2347 -0.0557 0.045 Uiso 1 1 calc R . . C6 C -0.0083(11) 0.3908(3) 0.0133(8) 0.038(2) Uani 1 1 d . . . C7 C -0.0918(12) 0.3722(4) 0.0815(9) 0.049(3) Uani 1 1 d . . . H7A H -0.0615 0.3432 0.1197 0.058 Uiso 1 1 calc R . . C8 C -0.2227(14) 0.3960(5) 0.0952(10) 0.066(4) Uani 1 1 d . . . H8A H -0.2854 0.3820 0.1378 0.079 Uiso 1 1 calc R . . C9 C -0.2582(14) 0.4385(5) 0.0477(11) 0.061(3) Uani 1 1 d . . . H9A H -0.3425 0.4555 0.0611 0.073 Uiso 1 1 calc R . . C10 C -0.1755(14) 0.4577(4) -0.0197(12) 0.063(3) Uani 1 1 d . . . H10A H -0.2026 0.4877 -0.0540 0.076 Uiso 1 1 calc R . . C11 C -0.0514(13) 0.4330(4) -0.0378(10) 0.050(3) Uani 1 1 d . . . H11A H 0.0044 0.4459 -0.0868 0.059 Uiso 1 1 calc R . . C12 C 0.2235(12) 0.3870(3) -0.1122(8) 0.039(2) Uani 1 1 d . . . C13 C 0.3488(11) 0.4176(4) -0.0901(9) 0.052(3) Uani 1 1 d . . . H13A H 0.4016 0.4239 -0.0156 0.063 Uiso 1 1 calc R . . C14 C 0.3946(13) 0.4382(4) -0.1760(10) 0.055(3) Uani 1 1 d . . . H14A H 0.4826 0.4578 -0.1592 0.066 Uiso 1 1 calc R . . C15 C 0.3227(18) 0.4325(5) -0.2817(11) 0.070(4) Uani 1 1 d . . . H15A H 0.3551 0.4493 -0.3384 0.085 Uiso 1 1 calc R . . C16 C 0.205(2) 0.4030(6) -0.3077(11) 0.103(6) Uani 1 1 d . . . H16A H 0.1578 0.3971 -0.3836 0.124 Uiso 1 1 calc R . . C17 C 0.1491(19) 0.3801(5) -0.2222(9) 0.090(6) Uani 1 1 d . . . H17A H 0.0616 0.3605 -0.2409 0.108 Uiso 1 1 calc R . . C18 C 0.5361(11) 0.2504(4) 0.0959(9) 0.042(2) Uani 1 1 d . . . C19 C 0.5494(14) 0.2148(4) 0.0177(11) 0.058(3) Uani 1 1 d . . . H19A H 0.4612 0.2027 -0.0324 0.070 Uiso 1 1 calc R . . C20 C 0.6930(16) 0.1978(5) 0.0148(12) 0.073(4) Uani 1 1 d . . . H20A H 0.7022 0.1750 -0.0397 0.087 Uiso 1 1 calc R . . C21 C 0.8273(14) 0.2142(5) 0.0932(12) 0.067(4) Uani 1 1 d . . . H21A H 0.9236 0.2006 0.0946 0.080 Uiso 1 1 calc R . . C22 C 0.8140(12) 0.2501(5) 0.1664(10) 0.060(3) Uani 1 1 d . . . H22A H 0.9026 0.2628 0.2150 0.072 Uiso 1 1 calc R . . C23 C 0.6704(11) 0.2680(4) 0.1693(8) 0.046(3) Uani 1 1 d . . . H23A H 0.6628 0.2921 0.2212 0.055 Uiso 1 1 calc R . . C24 C 0.2777(10) 0.2267(3) 0.1787(8) 0.033(2) Uani 1 1 d . . . C25 C 0.2623(13) 0.1800(4) 0.1422(9) 0.049(3) Uani 1 1 d . . . H25A H 0.2867 0.1720 0.0741 0.058 Uiso 1 1 calc R . . C26 C 0.2130(14) 0.1451(4) 0.2013(10) 0.056(3) Uani 1 1 d . . . H26A H 0.2050 0.1133 0.1748 0.067 Uiso 1 1 calc R . . C27 C 0.1751(13) 0.1558(5) 0.2986(12) 0.063(4) Uani 1 1 d . . . H27A H 0.1453 0.1312 0.3415 0.076 Uiso 1 1 calc R . . C28 C 0.1803(12) 0.2048(5) 0.3366(9) 0.054(3) Uani 1 1 d . . . H28A H 0.1484 0.2132 0.4017 0.064 Uiso 1 1 calc R . . C29 C 0.2324(10) 0.2384(4) 0.2755(8) 0.042(2) Uani 1 1 d . . . H29A H 0.2382 0.2706 0.2995 0.050 Uiso 1 1 calc R . . O1W O -0.0634(13) 0.4002(4) 0.3901(9) 0.021(2) Uiso 0.50 1 d P B 1 O1WA O -0.0147(18) 0.4187(6) 0.3834(12) 0.050(4) Uiso 0.50 1 d P C 2 O1M O 0.1193(15) 0.5034(4) 0.3908(11) 0.039(3) Uiso 0.50 1 d P . . H1M H 0.1521 0.5250 0.3560 0.059 Uiso 0.50 1 calc PR . . C1M C -0.054(3) 0.4911(9) 0.328(2) 0.060(6) Uiso 0.50 1 d P . . H1M1 H -0.1218 0.4997 0.3763 0.089 Uiso 0.50 1 calc PR . . H1M2 H -0.0636 0.4570 0.3120 0.089 Uiso 0.50 1 calc PR . . H1M3 H -0.0832 0.5091 0.2588 0.089 Uiso 0.50 1 calc PR . . 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 Pt 0.0291(2) 0.0347(2) 0.0267(2) 0.00009(14) -0.00168(15) 0.00054(16) S1 0.076(2) 0.0380(15) 0.0385(14) -0.0020(12) -0.0026(14) 0.0020(14) S2 0.0543(18) 0.0571(17) 0.0344(15) -0.0025(12) -0.0124(13) 0.0102(14) P1 0.0268(12) 0.0371(14) 0.0305(13) 0.0036(10) -0.0019(10) 0.0004(10) P2 0.0261(12) 0.0393(14) 0.0276(13) 0.0013(10) 0.0019(10) 0.0014(10) C1 0.083(10) 0.074(9) 0.066(9) -0.003(7) 0.009(8) -0.030(8) C2 0.071(9) 0.064(8) 0.047(7) -0.010(6) 0.001(6) -0.015(7) C3 0.066(8) 0.058(7) 0.044(6) 0.000(5) 0.009(6) -0.007(6) C4 0.029(5) 0.050(6) 0.034(5) 0.003(4) -0.001(4) -0.006(5) C5 0.047(6) 0.030(5) 0.032(5) -0.002(4) 0.005(4) -0.001(4) C6 0.038(5) 0.040(6) 0.029(5) -0.002(4) -0.003(4) 0.000(5) C7 0.044(6) 0.052(7) 0.050(6) 0.007(5) 0.012(5) 0.011(5) C8 0.050(8) 0.091(10) 0.057(8) -0.012(7) 0.016(6) 0.010(7) C9 0.039(7) 0.063(8) 0.066(8) -0.010(6) -0.017(6) 0.020(6) C10 0.047(7) 0.039(6) 0.092(10) 0.000(6) -0.008(7) 0.010(6) C11 0.042(6) 0.044(6) 0.058(7) 0.003(5) 0.002(5) -0.001(5) C12 0.042(6) 0.040(6) 0.030(5) 0.002(4) -0.003(4) -0.001(5) C13 0.023(5) 0.081(8) 0.045(6) 0.011(6) -0.007(4) -0.013(5) C14 0.039(6) 0.074(8) 0.051(7) 0.025(6) 0.010(5) -0.007(6) C15 0.103(12) 0.068(9) 0.047(8) 0.011(6) 0.031(8) -0.016(8) C16 0.165(18) 0.104(13) 0.036(7) 0.002(7) 0.015(9) -0.056(13) C17 0.133(14) 0.092(11) 0.030(6) -0.003(6) -0.007(7) -0.071(10) C18 0.031(5) 0.043(6) 0.052(6) 0.005(5) 0.009(5) 0.009(5) C19 0.050(7) 0.055(7) 0.073(8) 0.000(6) 0.022(6) 0.012(6) C20 0.074(10) 0.067(9) 0.089(10) -0.021(7) 0.042(8) 0.013(7) C21 0.039(7) 0.085(10) 0.082(10) 0.023(8) 0.026(7) 0.007(7) C22 0.026(6) 0.093(10) 0.060(8) 0.018(7) 0.009(5) 0.008(6) C23 0.031(6) 0.065(7) 0.038(6) 0.012(5) 0.002(4) 0.013(5) C24 0.020(4) 0.042(6) 0.036(5) 0.011(4) 0.006(4) 0.004(4) C25 0.055(7) 0.044(6) 0.045(6) 0.005(5) 0.009(5) 0.006(5) C26 0.058(8) 0.053(7) 0.051(7) 0.004(5) 0.004(6) -0.005(6) C27 0.036(6) 0.079(10) 0.068(8) 0.020(7) -0.001(6) -0.018(6) C28 0.042(7) 0.070(9) 0.047(7) 0.008(6) 0.008(5) -0.007(6) C29 0.021(5) 0.053(7) 0.045(6) 0.001(5) -0.004(4) 0.001(4) _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 Pt P1 2.249(2) . ? Pt P2 2.257(2) . ? Pt S1 2.327(3) . ? Pt S2 2.348(3) . ? S1 C1 1.840(13) . ? S2 C3 1.807(12) . ? P1 C12 1.802(10) . ? P1 C4 1.824(10) . ? P1 C6 1.830(10) . ? P2 C18 1.802(10) . ? P2 C24 1.823(9) . ? P2 C5 1.824(10) . ? O1 C2 1.34(2) . ? O1 H1 0.8400 . ? O1 H2B 0.5082 . ? O1A C2 1.34(3) . ? O1A H1OA 0.8400 . ? C1 C2 1.493(18) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C3 1.449(16) . ? C2 H2A 1.0000 . ? C2 H2B 1.0000 . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.532(13) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C11 1.359(14) . ? C6 C7 1.367(14) . ? C7 C8 1.408(15) . ? C7 H7A 0.9500 . ? C8 C9 1.337(17) . ? C8 H8A 0.9500 . ? C9 C10 1.361(18) . ? C9 H9A 0.9500 . ? C10 C11 1.385(16) . ? C10 H10A 0.9500 . ? C11 H11A 0.9500 . ? C12 C17 1.381(16) . ? C12 C13 1.399(14) . ? C13 C14 1.362(14) . ? C13 H13A 0.9500 . ? C14 C15 1.327(17) . ? C14 H14A 0.9500 . ? C15 C16 1.33(2) . ? C15 H15A 0.9500 . ? C16 C17 1.434(18) . ? C16 H16A 0.9500 . ? C17 H17A 0.9500 . ? C18 C19 1.418(15) . ? C18 C23 1.423(14) . ? C19 C20 1.396(16) . ? C19 H19A 0.9500 . ? C20 C21 1.440(19) . ? C20 H20A 0.9500 . ? C21 C22 1.382(19) . ? C21 H21A 0.9500 . ? C22 C23 1.404(14) . ? C22 H22A 0.9500 . ? C23 H23A 0.9500 . ? C24 C25 1.386(14) . ? C24 C29 1.399(13) . ? C25 C26 1.363(15) . ? C25 H25A 0.9500 . ? C26 C27 1.364(19) . ? C26 H26A 0.9500 . ? C27 C28 1.454(17) . ? C27 H27A 0.9500 . ? C28 C29 1.365(15) . ? C28 H28A 0.9500 . ? C29 H29A 0.9500 . ? O1M C1M 1.62(3) . ? O1M H1M 0.8400 . ? C1M H1M1 0.9800 . ? C1M H1M2 0.9800 . ? C1M H1M3 0.9800 . ? 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 P1 Pt P2 85.80(9) . . ? P1 Pt S1 87.86(10) . . ? P2 Pt S1 173.38(9) . . ? P1 Pt S2 175.38(10) . . ? P2 Pt S2 94.51(9) . . ? S1 Pt S2 91.97(10) . . ? C1 S1 Pt 106.5(5) . . ? C3 S2 Pt 104.2(4) . . ? C12 P1 C4 105.4(5) . . ? C12 P1 C6 106.0(5) . . ? C4 P1 C6 106.5(4) . . ? C12 P1 Pt 116.7(3) . . ? C4 P1 Pt 107.0(3) . . ? C6 P1 Pt 114.4(3) . . ? C18 P2 C24 103.8(4) . . ? C18 P2 C5 103.2(5) . . ? C24 P2 C5 104.3(4) . . ? C18 P2 Pt 118.5(4) . . ? C24 P2 Pt 117.4(3) . . ? C5 P2 Pt 107.9(3) . . ? C2 O1 H1 109.5 . . ? C2 O1 H2B 38.9 . . ? H1 O1 H2B 110.5 . . ? C2 O1A H1OA 109.5 . . ? C2 C1 S1 113.5(9) . . ? C2 C1 H1A 108.9 . . ? S1 C1 H1A 108.9 . . ? C2 C1 H1B 108.9 . . ? S1 C1 H1B 108.9 . . ? H1A C1 H1B 107.7 . . ? O1A C2 O1 85.6(16) . . ? O1A C2 C3 119.4(18) . . ? O1 C2 C3 105.8(13) . . ? O1A C2 C1 109.1(17) . . ? O1 C2 C1 114.8(14) . . ? C3 C2 C1 117.8(10) . . ? O1A C2 H2A 21.4 . . ? O1 C2 H2A 105.8 . . ? C3 C2 H2A 105.8 . . ? C1 C2 H2A 105.8 . . ? O1A C2 H2B 103.0 . . ? O1 C2 H2B 18.6 . . ? C3 C2 H2B 102.4 . . ? C1 C2 H2B 102.1 . . ? H2A C2 H2B 123.8 . . ? C2 C3 S2 115.6(9) . . ? C2 C3 H3A 108.4 . . ? S2 C3 H3A 108.4 . . ? C2 C3 H3B 108.4 . . ? S2 C3 H3B 108.4 . . ? H3A C3 H3B 107.4 . . ? C5 C4 P1 107.6(6) . . ? C5 C4 H4A 110.2 . . ? P1 C4 H4A 110.2 . . ? C5 C4 H4B 110.2 . . ? P1 C4 H4B 110.2 . . ? H4A C4 H4B 108.5 . . ? C4 C5 P2 108.7(6) . . ? C4 C5 H5A 109.9 . . ? P2 C5 H5A 109.9 . . ? C4 C5 H5B 109.9 . . ? P2 C5 H5B 109.9 . . ? H5A C5 H5B 108.3 . . ? C11 C6 C7 118.8(10) . . ? C11 C6 P1 123.0(8) . . ? C7 C6 P1 118.1(8) . . ? C6 C7 C8 120.1(11) . . ? C6 C7 H7A 120.0 . . ? C8 C7 H7A 120.0 . . ? C9 C8 C7 119.5(12) . . ? C9 C8 H8A 120.2 . . ? C7 C8 H8A 120.2 . . ? C8 C9 C10 121.0(12) . . ? C8 C9 H9A 119.5 . . ? C10 C9 H9A 119.5 . . ? C9 C10 C11 119.3(11) . . ? C9 C10 H10A 120.3 . . ? C11 C10 H10A 120.3 . . ? C6 C11 C10 121.1(11) . . ? C6 C11 H11A 119.5 . . ? C10 C11 H11A 119.5 . . ? C17 C12 C13 117.4(10) . . ? C17 C12 P1 122.0(9) . . ? C13 C12 P1 120.6(7) . . ? C14 C13 C12 119.7(10) . . ? C14 C13 H13A 120.2 . . ? C12 C13 H13A 120.2 . . ? C15 C14 C13 123.4(11) . . ? C15 C14 H14A 118.3 . . ? C13 C14 H14A 118.3 . . ? C14 C15 C16 119.5(12) . . ? C14 C15 H15A 120.3 . . ? C16 C15 H15A 120.3 . . ? C15 C16 C17 120.5(13) . . ? C15 C16 H16A 119.8 . . ? C17 C16 H16A 119.8 . . ? C12 C17 C16 119.5(12) . . ? C12 C17 H17A 120.3 . . ? C16 C17 H17A 120.3 . . ? C19 C18 C23 118.8(9) . . ? C19 C18 P2 121.3(8) . . ? C23 C18 P2 119.9(8) . . ? C20 C19 C18 119.6(12) . . ? C20 C19 H19A 120.2 . . ? C18 C19 H19A 120.2 . . ? C19 C20 C21 121.0(11) . . ? C19 C20 H20A 119.5 . . ? C21 C20 H20A 119.5 . . ? C22 C21 C20 119.0(11) . . ? C22 C21 H21A 120.5 . . ? C20 C21 H21A 120.5 . . ? C21 C22 C23 120.4(12) . . ? C21 C22 H22A 119.8 . . ? C23 C22 H22A 119.8 . . ? C22 C23 C18 121.1(11) . . ? C22 C23 H23A 119.5 . . ? C18 C23 H23A 119.5 . . ? C25 C24 C29 118.4(9) . . ? C25 C24 P2 122.2(7) . . ? C29 C24 P2 119.3(8) . . ? C26 C25 C24 121.9(10) . . ? C26 C25 H25A 119.1 . . ? C24 C25 H25A 119.1 . . ? C25 C26 C27 120.1(11) . . ? C25 C26 H26A 120.0 . . ? C27 C26 H26A 120.0 . . ? C26 C27 C28 120.0(11) . . ? C26 C27 H27A 120.0 . . ? C28 C27 H27A 120.0 . . ? C29 C28 C27 117.8(11) . . ? C29 C28 H28A 121.1 . . ? C27 C28 H28A 121.1 . . ? C28 C29 C24 121.7(10) . . ? C28 C29 H29A 119.2 . . ? C24 C29 H29A 119.2 . . ? C1M O1M H1M 109.5 . . ? O1M C1M H1M1 109.5 . . ? O1M C1M H1M2 109.5 . . ? H1M1 C1M H1M2 109.5 . . ? O1M C1M H1M3 109.5 . . ? H1M1 C1M H1M3 109.5 . . ? H1M2 C1M H1M3 109.5 . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 2.860 _refine_diff_density_min -2.192 _refine_diff_density_rms 0.221 #==== END data_FO3119 _database_code_depnum_ccdc_archive 'CCDC 776104' #TrackingRef '- dalton.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C31 H34 O P2 Pt S2' _chemical_formula_sum 'C31 H34 O P2 Pt S2' _chemical_formula_weight 743.73 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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' 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 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 15.6013(6) _cell_length_b 18.2591(7) _cell_length_c 10.9863(4) _cell_angle_alpha 90.00 _cell_angle_beta 104.966(2) _cell_angle_gamma 90.00 _cell_volume 3023.5(2) _cell_formula_units_Z 4 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used 20310 _cell_measurement_theta_min 2.61 _cell_measurement_theta_max 27.48 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.634 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1472 _exptl_absorpt_coefficient_mu 4.908 _exptl_absorpt_correction_type NONE _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 183(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 KappaCCD _diffrn_measurement_method 'phi- + omega-scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20310 _diffrn_reflns_av_R_equivalents 0.0591 _diffrn_reflns_av_sigmaI/netI 0.0563 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.61 _diffrn_reflns_theta_max 27.48 _reflns_number_total 6808 _reflns_number_gt 5116 _reflns_threshold_expression >2sigma(I) _computing_data_collection COLLECT _computing_cell_refinement DENZO _computing_data_reduction DENZO _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL/PC _computing_publication_material SHELXL-97 _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^)+(0.0496P)^2^+2.6203P] 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 6808 _refine_ls_number_parameters 333 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0633 _refine_ls_R_factor_gt 0.0386 _refine_ls_wR_factor_ref 0.0979 _refine_ls_wR_factor_gt 0.0869 _refine_ls_goodness_of_fit_ref 1.007 _refine_ls_restrained_S_all 1.007 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt Pt 0.736416(13) 0.058080(10) 0.341124(17) 0.03015(8) Uani 1 1 d . A . P1 P 0.75646(8) 0.17701(7) 0.39556(12) 0.0285(3) Uani 1 1 d . . . P2 P 0.73430(9) 0.03960(7) 0.54364(13) 0.0304(3) Uani 1 1 d . . . S1 S 0.74980(11) 0.07751(10) 0.13671(14) 0.0495(4) Uani 1 1 d . A . S2 S 0.69772(18) -0.06171(9) 0.28399(19) 0.0748(6) Uani 1 1 d . . . O1 O 0.7723(6) -0.1411(5) -0.0179(7) 0.126(3) Uani 1 1 d . . . C1 C 0.7033(7) -0.0032(4) 0.0527(7) 0.092(3) Uani 1 1 d . . . H1A H 0.6382 -0.0049 0.0408 0.110 Uiso 0.490(17) 1 calc PR A 1 H1B H 0.7164 -0.0055 -0.0307 0.110 Uiso 0.490(17) 1 calc PR A 1 H1C H 0.6464 0.0112 -0.0063 0.110 Uiso 0.510(17) 1 calc PR A 2 H1D H 0.7434 -0.0183 0.0006 0.110 Uiso 0.510(17) 1 calc PR A 2 C2 C 0.7463(9) -0.0621(7) 0.1326(12) 0.044(3) Uiso 0.490(17) 1 d P A 1 H2A H 0.8123 -0.0561 0.1566 0.052 Uiso 0.490(17) 1 calc PR A 1 C3 C 0.7178(8) -0.1384(7) 0.0678(11) 0.045(4) Uiso 0.490(17) 1 d P A 1 H3A H 0.7313 -0.1791 0.1294 0.054 Uiso 0.490(17) 1 calc PR A 1 H3B H 0.6540 -0.1394 0.0233 0.054 Uiso 0.490(17) 1 calc PR A 1 C2A C 0.6846(18) -0.0734(13) 0.125(2) 0.116(8) Uiso 0.510(17) 1 d P A 2 H2AB H 0.6359 -0.1067 0.0801 0.140 Uiso 0.510(17) 1 calc PR A 2 C3A C 0.7856(17) -0.0942(14) 0.121(2) 0.120(8) Uiso 0.510(17) 1 d P A 2 H3AA H 0.8147 -0.1254 0.1940 0.144 Uiso 0.510(17) 1 calc PR A 2 H3AB H 0.8216 -0.0495 0.1222 0.144 Uiso 0.510(17) 1 calc PR A 2 C4 C 0.7594(8) -0.2153(9) -0.0636(13) 0.145(5) Uani 1 1 d . A . H4B H 0.7741 -0.2498 0.0084 0.174 Uiso 1 1 calc R . . H4A H 0.6964 -0.2228 -0.1091 0.174 Uiso 1 1 calc R . . C5 C 0.8121(8) -0.2292(5) -0.1425(9) 0.114(4) Uani 1 1 d . . . H5A H 0.8035 -0.2799 -0.1722 0.171 Uiso 1 1 calc R A . H5B H 0.8744 -0.2217 -0.0973 0.171 Uiso 1 1 calc R . . H5C H 0.7963 -0.1958 -0.2148 0.171 Uiso 1 1 calc R . . C6 C 0.7135(3) 0.1284(3) 0.6081(5) 0.0327(11) Uani 1 1 d . . . H6A H 0.6502 0.1420 0.5764 0.039 Uiso 1 1 calc R . . H6B H 0.7281 0.1261 0.7012 0.039 Uiso 1 1 calc R . . C7 C 0.7720(4) 0.1847(3) 0.5661(5) 0.0353(12) Uani 1 1 d . . . H7A H 0.8350 0.1760 0.6101 0.042 Uiso 1 1 calc R . . H7B H 0.7558 0.2346 0.5875 0.042 Uiso 1 1 calc R . . C8 C 0.8508(3) 0.2268(3) 0.3684(5) 0.0309(11) Uani 1 1 d . . . C9 C 0.9123(4) 0.1903(3) 0.3184(6) 0.0507(16) Uani 1 1 d . . . H9A H 0.9042 0.1399 0.2973 0.061 Uiso 1 1 calc R . . C10 C 0.9849(4) 0.2271(4) 0.2994(8) 0.070(2) Uani 1 1 d . . . H10A H 1.0265 0.2018 0.2652 0.084 Uiso 1 1 calc R . . C11 C 0.9974(4) 0.3000(4) 0.3297(7) 0.0628(19) Uani 1 1 d . . . H11A H 1.0475 0.3249 0.3158 0.075 Uiso 1 1 calc R . . C12 C 0.9374(4) 0.3375(3) 0.3803(6) 0.0475(14) Uani 1 1 d . . . H12A H 0.9465 0.3878 0.4018 0.057 Uiso 1 1 calc R . . C13 C 0.8638(4) 0.3008(3) 0.3994(5) 0.0382(12) Uani 1 1 d . . . H13A H 0.8223 0.3262 0.4337 0.046 Uiso 1 1 calc R . . C14 C 0.6585(3) 0.2326(3) 0.3256(5) 0.0297(11) Uani 1 1 d . . . C15 C 0.6057(3) 0.2143(3) 0.2073(5) 0.0328(11) Uani 1 1 d . . . H15A H 0.6211 0.1735 0.1637 0.039 Uiso 1 1 calc R . . C16 C 0.5312(3) 0.2547(3) 0.1526(5) 0.0406(13) Uani 1 1 d . . . H16A H 0.4963 0.2419 0.0710 0.049 Uiso 1 1 calc R . . C17 C 0.5066(4) 0.3135(3) 0.2145(6) 0.0448(14) Uani 1 1 d . . . H17A H 0.4545 0.3406 0.1768 0.054 Uiso 1 1 calc R . . C18 C 0.5583(4) 0.3326(3) 0.3316(6) 0.0466(14) Uani 1 1 d . . . H18A H 0.5418 0.3730 0.3752 0.056 Uiso 1 1 calc R . . C19 C 0.6345(4) 0.2931(3) 0.3862(5) 0.0387(12) Uani 1 1 d . . . H19A H 0.6707 0.3075 0.4660 0.046 Uiso 1 1 calc R . . C20 C 0.6578(4) -0.0250(3) 0.5844(5) 0.0387(12) Uani 1 1 d . . . C21 C 0.5872(4) -0.0027(4) 0.6295(6) 0.0538(16) Uani 1 1 d . . . H21A H 0.5765 0.0479 0.6391 0.065 Uiso 1 1 calc R . . C22 C 0.5312(5) -0.0560(5) 0.6611(7) 0.071(2) Uani 1 1 d . . . H22A H 0.4822 -0.0416 0.6920 0.085 Uiso 1 1 calc R . . C23 C 0.5481(5) -0.1293(5) 0.6467(7) 0.069(2) Uani 1 1 d . . . H23A H 0.5100 -0.1651 0.6675 0.083 Uiso 1 1 calc R . . C24 C 0.6175(5) -0.1513(4) 0.6038(6) 0.0605(18) Uani 1 1 d . . . H24A H 0.6284 -0.2020 0.5957 0.073 Uiso 1 1 calc R . . C25 C 0.6727(4) -0.0997(3) 0.5715(6) 0.0510(15) Uani 1 1 d . . . H25A H 0.7212 -0.1151 0.5403 0.061 Uiso 1 1 calc R . . C26 C 0.8405(3) 0.0111(3) 0.6460(5) 0.0344(11) Uani 1 1 d . . . C27 C 0.8463(4) -0.0212(3) 0.7619(5) 0.0426(13) Uani 1 1 d . . . H27A H 0.7936 -0.0298 0.7877 0.051 Uiso 1 1 calc R . . C28 C 0.9268(4) -0.0411(3) 0.8406(6) 0.0476(15) Uani 1 1 d . . . H28A H 0.9292 -0.0642 0.9189 0.057 Uiso 1 1 calc R . . C29 C 1.0039(4) -0.0273(3) 0.8054(6) 0.0517(16) Uani 1 1 d . . . H29A H 1.0595 -0.0409 0.8596 0.062 Uiso 1 1 calc R . . C30 C 1.0006(4) 0.0063(3) 0.6915(6) 0.0491(15) Uani 1 1 d . . . H30A H 1.0539 0.0163 0.6680 0.059 Uiso 1 1 calc R . . C31 C 0.9190(4) 0.0253(3) 0.6114(5) 0.0421(13) Uani 1 1 d . . . H31A H 0.9167 0.0480 0.5328 0.051 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 Pt 0.03247(12) 0.02669(12) 0.03318(12) -0.00151(8) 0.01193(9) 0.00269(8) P1 0.0295(7) 0.0278(7) 0.0294(6) 0.0016(5) 0.0101(5) 0.0023(5) P2 0.0278(7) 0.0296(7) 0.0354(7) 0.0024(5) 0.0109(6) 0.0003(5) S1 0.0601(10) 0.0571(9) 0.0369(8) 0.0017(7) 0.0224(7) 0.0189(7) S2 0.136(2) 0.0322(9) 0.0581(11) -0.0112(7) 0.0285(12) -0.0131(10) O1 0.149(7) 0.146(7) 0.105(5) -0.003(5) 0.074(5) 0.035(6) C1 0.174(10) 0.065(5) 0.044(4) -0.016(4) 0.042(5) -0.016(6) C4 0.120(10) 0.212(16) 0.122(10) 0.037(11) 0.065(8) 0.002(10) C5 0.155(10) 0.081(7) 0.095(7) -0.024(6) 0.010(7) -0.024(7) C6 0.036(3) 0.035(3) 0.028(2) 0.003(2) 0.011(2) 0.008(2) C7 0.045(3) 0.026(3) 0.035(3) -0.003(2) 0.009(2) 0.006(2) C8 0.028(3) 0.027(3) 0.036(3) 0.001(2) 0.004(2) -0.002(2) C9 0.040(3) 0.041(3) 0.079(4) -0.002(3) 0.030(3) 0.000(3) C10 0.051(4) 0.052(4) 0.120(7) 0.002(4) 0.047(4) -0.003(3) C11 0.038(4) 0.062(5) 0.092(5) 0.010(4) 0.022(4) -0.010(3) C12 0.045(3) 0.034(3) 0.058(4) 0.002(3) 0.002(3) -0.012(3) C13 0.041(3) 0.032(3) 0.039(3) -0.002(2) 0.003(2) -0.001(2) C14 0.031(3) 0.030(3) 0.033(3) 0.004(2) 0.016(2) 0.005(2) C15 0.033(3) 0.036(3) 0.032(3) 0.004(2) 0.013(2) 0.000(2) C16 0.033(3) 0.046(3) 0.043(3) 0.006(3) 0.009(2) 0.001(2) C17 0.040(3) 0.047(4) 0.051(3) 0.013(3) 0.017(3) 0.013(3) C18 0.054(4) 0.041(3) 0.052(3) 0.003(3) 0.026(3) 0.013(3) C19 0.040(3) 0.038(3) 0.038(3) -0.002(2) 0.011(2) 0.004(2) C20 0.033(3) 0.045(3) 0.036(3) 0.010(2) 0.006(2) -0.004(2) C21 0.042(4) 0.068(4) 0.056(4) 0.017(3) 0.021(3) 0.000(3) C22 0.040(4) 0.110(7) 0.068(5) 0.024(4) 0.025(4) 0.001(4) C23 0.059(5) 0.080(6) 0.063(4) 0.018(4) 0.008(4) -0.029(4) C24 0.065(5) 0.059(4) 0.053(4) 0.010(3) 0.008(3) -0.026(4) C25 0.055(4) 0.046(4) 0.052(4) 0.004(3) 0.012(3) -0.020(3) C26 0.037(3) 0.025(3) 0.040(3) 0.001(2) 0.008(2) 0.009(2) C27 0.037(3) 0.035(3) 0.053(3) 0.008(3) 0.007(3) 0.004(2) C28 0.051(4) 0.036(3) 0.048(3) 0.004(3) -0.001(3) 0.006(3) C29 0.039(3) 0.047(4) 0.060(4) -0.014(3) -0.005(3) 0.019(3) C30 0.033(3) 0.051(4) 0.063(4) -0.019(3) 0.012(3) 0.004(3) C31 0.035(3) 0.047(3) 0.044(3) -0.004(3) 0.011(3) 0.005(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 Pt P1 2.2527(13) . ? Pt P2 2.2590(13) . ? Pt S2 2.3124(16) . ? Pt S1 2.3356(14) . ? P1 C8 1.820(5) . ? P1 C14 1.830(5) . ? P1 C7 1.832(5) . ? P2 C20 1.815(5) . ? P2 C26 1.821(5) . ? P2 C6 1.832(5) . ? S1 C1 1.790(8) . ? S2 C2A 1.71(2) . ? S2 C2 1.998(12) . ? O1 C3 1.423(12) . ? O1 C4 1.442(16) . ? O1 C3A 1.72(2) . ? C1 C2 1.439(15) . ? C1 C2A 1.58(2) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C1 H1C 0.9900 . ? C1 H1D 0.9900 . ? C2 C3 1.576(18) . ? C2 H2A 1.0000 . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C2A C3A 1.63(4) . ? C2A H2AB 1.0000 . ? C3A H3AA 0.9900 . ? C3A H3AB 0.9900 . ? C4 C5 1.364(13) . ? C4 H4B 0.9900 . ? C4 H4A 0.9900 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 C7 1.523(7) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.391(7) . ? C8 C13 1.396(7) . ? C9 C10 1.378(8) . ? C9 H9A 0.9500 . ? C10 C11 1.374(9) . ? C10 H10A 0.9500 . ? C11 C12 1.386(9) . ? C11 H11A 0.9500 . ? C12 C13 1.392(7) . ? C12 H12A 0.9500 . ? C13 H13A 0.9500 . ? C14 C15 1.388(7) . ? C14 C19 1.390(7) . ? C15 C16 1.377(7) . ? C15 H15A 0.9500 . ? C16 C17 1.378(8) . ? C16 H16A 0.9500 . ? C17 C18 1.375(8) . ? C17 H17A 0.9500 . ? C18 C19 1.388(8) . ? C18 H18A 0.9500 . ? C19 H19A 0.9500 . ? C20 C21 1.380(8) . ? C20 C25 1.396(9) . ? C21 C22 1.410(9) . ? C21 H21A 0.9500 . ? C22 C23 1.382(10) . ? C22 H22A 0.9500 . ? C23 C24 1.349(10) . ? C23 H23A 0.9500 . ? C24 C25 1.384(8) . ? C24 H24A 0.9500 . ? C25 H25A 0.9500 . ? C26 C27 1.384(7) . ? C26 C31 1.398(7) . ? C27 C28 1.377(8) . ? C27 H27A 0.9500 . ? C28 C29 1.377(9) . ? C28 H28A 0.9500 . ? C29 C30 1.382(9) . ? C29 H29A 0.9500 . ? C30 C31 1.392(8) . ? C30 H30A 0.9500 . ? C31 H31A 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P1 Pt P2 85.35(5) . . ? P1 Pt S2 172.99(7) . . ? P2 Pt S2 93.26(6) . . ? P1 Pt S1 93.91(5) . . ? P2 Pt S1 175.85(5) . . ? S2 Pt S1 87.97(7) . . ? C8 P1 C14 106.1(2) . . ? C8 P1 C7 103.3(2) . . ? C14 P1 C7 105.2(2) . . ? C8 P1 Pt 120.05(16) . . ? C14 P1 Pt 112.29(17) . . ? C7 P1 Pt 108.56(16) . . ? C20 P2 C26 102.3(2) . . ? C20 P2 C6 106.6(3) . . ? C26 P2 C6 103.8(2) . . ? C20 P2 Pt 121.19(19) . . ? C26 P2 Pt 114.12(17) . . ? C6 P2 Pt 107.32(16) . . ? C1 S1 Pt 104.2(2) . . ? C2A S2 C2 29.0(9) . . ? C2A S2 Pt 110.4(8) . . ? C2 S2 Pt 95.8(4) . . ? C3 O1 C4 102.0(9) . . ? C3 O1 C3A 49.4(9) . . ? C4 O1 C3A 138.8(12) . . ? C2 C1 C2A 37.1(9) . . ? C2 C1 S1 103.7(7) . . ? C2A C1 S1 120.8(10) . . ? C2 C1 H1A 111.0 . . ? C2A C1 H1A 74.0 . . ? S1 C1 H1A 111.0 . . ? C2 C1 H1B 111.0 . . ? C2A C1 H1B 123.0 . . ? S1 C1 H1B 111.0 . . ? H1A C1 H1B 109.0 . . ? C2 C1 H1C 142.7 . . ? C2A C1 H1C 107.1 . . ? S1 C1 H1C 107.1 . . ? H1A C1 H1C 37.4 . . ? H1B C1 H1C 76.6 . . ? C2 C1 H1D 83.1 . . ? C2A C1 H1D 107.1 . . ? S1 C1 H1D 107.1 . . ? H1A C1 H1D 134.0 . . ? H1B C1 H1D 30.8 . . ? H1C C1 H1D 106.8 . . ? C1 C2 C3 110.6(10) . . ? C1 C2 S2 106.7(8) . . ? C3 C2 S2 104.8(8) . . ? C1 C2 H2A 111.5 . . ? C3 C2 H2A 111.5 . . ? S2 C2 H2A 111.5 . . ? O1 C3 C2 100.5(10) . . ? O1 C3 H3A 111.7 . . ? C2 C3 H3A 111.7 . . ? O1 C3 H3B 111.7 . . ? C2 C3 H3B 111.7 . . ? H3A C3 H3B 109.4 . . ? C1 C2A C3A 82.4(16) . . ? C1 C2A S2 115.1(15) . . ? C3A C2A S2 101.2(16) . . ? C1 C2A H2AB 117.3 . . ? C3A C2A H2AB 117.3 . . ? S2 C2A H2AB 117.3 . . ? C2A C3A O1 104.2(16) . . ? C2A C3A H3AA 110.9 . . ? O1 C3A H3AA 110.9 . . ? C2A C3A H3AB 110.9 . . ? O1 C3A H3AB 110.9 . . ? H3AA C3A H3AB 108.9 . . ? C5 C4 O1 110.0(10) . . ? C5 C4 H4B 109.7 . . ? O1 C4 H4B 109.7 . . ? C5 C4 H4A 109.7 . . ? O1 C4 H4A 109.7 . . ? H4B C4 H4A 108.2 . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C7 C6 P2 107.5(3) . . ? C7 C6 H6A 110.2 . . ? P2 C6 H6A 110.2 . . ? C7 C6 H6B 110.2 . . ? P2 C6 H6B 110.2 . . ? H6A C6 H6B 108.5 . . ? C6 C7 P1 109.1(3) . . ? C6 C7 H7A 109.9 . . ? P1 C7 H7A 109.9 . . ? C6 C7 H7B 109.9 . . ? P1 C7 H7B 109.9 . . ? H7A C7 H7B 108.3 . . ? C9 C8 C13 119.3(5) . . ? C9 C8 P1 119.7(4) . . ? C13 C8 P1 121.0(4) . . ? C10 C9 C8 120.2(6) . . ? C10 C9 H9A 119.9 . . ? C8 C9 H9A 119.9 . . ? C11 C10 C9 120.5(6) . . ? C11 C10 H10A 119.8 . . ? C9 C10 H10A 119.8 . . ? C10 C11 C12 120.4(6) . . ? C10 C11 H11A 119.8 . . ? C12 C11 H11A 119.8 . . ? C13 C12 C11 119.5(6) . . ? C13 C12 H12A 120.2 . . ? C11 C12 H12A 120.2 . . ? C12 C13 C8 120.1(5) . . ? C12 C13 H13A 119.9 . . ? C8 C13 H13A 119.9 . . ? C15 C14 C19 118.1(5) . . ? C15 C14 P1 119.3(4) . . ? C19 C14 P1 122.6(4) . . ? C16 C15 C14 120.7(5) . . ? C16 C15 H15A 119.7 . . ? C14 C15 H15A 119.7 . . ? C15 C16 C17 120.9(5) . . ? C15 C16 H16A 119.5 . . ? C17 C16 H16A 119.5 . . ? C18 C17 C16 119.2(5) . . ? C18 C17 H17A 120.4 . . ? C16 C17 H17A 120.4 . . ? C17 C18 C19 120.2(5) . . ? C17 C18 H18A 119.9 . . ? C19 C18 H18A 119.9 . . ? C18 C19 C14 120.9(5) . . ? C18 C19 H19A 119.6 . . ? C14 C19 H19A 119.6 . . ? C21 C20 C25 119.6(5) . . ? C21 C20 P2 122.2(5) . . ? C25 C20 P2 118.2(4) . . ? C20 C21 C22 119.2(7) . . ? C20 C21 H21A 120.4 . . ? C22 C21 H21A 120.4 . . ? C23 C22 C21 119.4(6) . . ? C23 C22 H22A 120.3 . . ? C21 C22 H22A 120.3 . . ? C24 C23 C22 121.5(6) . . ? C24 C23 H23A 119.2 . . ? C22 C23 H23A 119.2 . . ? C23 C24 C25 119.8(7) . . ? C23 C24 H24A 120.1 . . ? C25 C24 H24A 120.1 . . ? C24 C25 C20 120.5(6) . . ? C24 C25 H25A 119.8 . . ? C20 C25 H25A 119.8 . . ? C27 C26 C31 118.3(5) . . ? C27 C26 P2 121.5(4) . . ? C31 C26 P2 120.0(4) . . ? C28 C27 C26 121.5(5) . . ? C28 C27 H27A 119.2 . . ? C26 C27 H27A 119.2 . . ? C29 C28 C27 119.7(6) . . ? C29 C28 H28A 120.1 . . ? C27 C28 H28A 120.1 . . ? C28 C29 C30 120.3(6) . . ? C28 C29 H29A 119.8 . . ? C30 C29 H29A 119.8 . . ? C29 C30 C31 119.8(5) . . ? C29 C30 H30A 120.1 . . ? C31 C30 H30A 120.1 . . ? C30 C31 C26 120.3(5) . . ? C30 C31 H31A 119.8 . . ? C26 C31 H31A 119.8 . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 1.396 _refine_diff_density_min -1.953 _refine_diff_density_rms 0.132 #==== END data_FO3097 _database_code_depnum_ccdc_archive 'CCDC 776105' #TrackingRef '- dalton.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C35 H44 O P2 Pt S2 Si' _chemical_formula_sum 'C35 H44 O P2 Pt S2 Si' _chemical_formula_weight 829.94 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P bca' _symmetry_space_group_name_Hall '-P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 17.8444(14) _cell_length_b 13.7455(11) _cell_length_c 28.9636(18) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7104.2(9) _cell_formula_units_Z 8 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used 19282 _cell_measurement_theta_min 2.34 _cell_measurement_theta_max 27.42 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.552 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3328 _exptl_absorpt_coefficient_mu 4.218 _exptl_absorpt_correction_type NONE _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 183(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 KappaCCD _diffrn_measurement_method 'phi- + omega-scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19282 _diffrn_reflns_av_R_equivalents 0.1662 _diffrn_reflns_av_sigmaI/netI 0.1345 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 2.34 _diffrn_reflns_theta_max 27.42 _reflns_number_total 6757 _reflns_number_gt 3924 _reflns_threshold_expression >2sigma(I) _computing_data_collection COLLECT _computing_cell_refinement DENZO _computing_data_reduction DENZO _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL/PC _computing_publication_material SHELXL-97 _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^)+(0.1064P)^2^+156.5095P] 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 6757 _refine_ls_number_parameters 393 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1576 _refine_ls_R_factor_gt 0.0876 _refine_ls_wR_factor_ref 0.2660 _refine_ls_wR_factor_gt 0.2150 _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_restrained_S_all 1.018 _refine_ls_shift/su_max 0.002 _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 Pt Pt 0.92390(3) -0.19857(5) 0.616971(18) 0.0336(2) Uani 1 1 d . . . S1 S 0.9009(3) -0.3676(3) 0.61341(14) 0.0494(11) Uani 1 1 d . . . S2 S 1.0524(3) -0.2219(4) 0.60558(15) 0.0516(12) Uani 1 1 d . . . P1 P 0.8032(3) -0.1633(4) 0.62996(14) 0.0436(11) Uani 1 1 d . . . P2 P 0.9452(3) -0.0373(3) 0.62337(14) 0.0404(10) Uani 1 1 d . . . Si Si 1.1095(5) -0.6040(5) 0.6059(3) 0.085(2) Uani 1 1 d . . . O1A O 1.0682(13) -0.5002(17) 0.6305(8) 0.045(6) Uani 0.50 1 d P A 1 O1 O 1.0938(16) -0.486(2) 0.5932(10) 0.063(7) Uani 0.50 1 d P A 2 C1 C 0.9814(10) -0.4181(15) 0.5812(6) 0.057(5) Uani 1 1 d . A . H1A H 0.9681 -0.4837 0.5697 0.069 Uiso 1 1 calc R . . H1B H 0.9917 -0.3763 0.5541 0.069 Uiso 1 1 calc R . . C2 C 1.0504(16) -0.4254(19) 0.6097(10) 0.100(10) Uani 1 1 d . . . H2A H 1.0891 -0.4259 0.5847 0.120 Uiso 0.50 1 calc PR A 1 H2B H 1.0303 -0.4641 0.6362 0.120 Uiso 0.50 1 calc PR A 2 C3 C 1.0732(10) -0.3338(13) 0.6351(7) 0.050(5) Uani 1 1 d . A . H3A H 1.1278 -0.3365 0.6410 0.060 Uiso 1 1 calc R . . H3B H 1.0477 -0.3330 0.6654 0.060 Uiso 1 1 calc R . . C4 C 1.141(3) -0.619(2) 0.5464(8) 0.158(17) Uani 1 1 d . A . H4A H 1.0984 -0.6341 0.5266 0.237 Uiso 1 1 calc R . . H4B H 1.1780 -0.6716 0.5448 0.237 Uiso 1 1 calc R . . H4C H 1.1646 -0.5580 0.5358 0.237 Uiso 1 1 calc R . . C5 C 1.0286(16) -0.687(2) 0.6161(10) 0.109(11) Uani 1 1 d . A . H5A H 0.9838 -0.6603 0.6011 0.163 Uiso 1 1 calc R . . H5B H 1.0197 -0.6929 0.6494 0.163 Uiso 1 1 calc R . . H5C H 1.0398 -0.7512 0.6031 0.163 Uiso 1 1 calc R . . C6 C 1.1856(13) -0.6305(19) 0.6486(8) 0.079(7) Uani 1 1 d . A . C7 C 1.2115(17) -0.735(2) 0.6436(11) 0.120(11) Uani 1 1 d . . . H7A H 1.2539 -0.7467 0.6644 0.179 Uiso 1 1 calc R A . H7B H 1.2271 -0.7466 0.6117 0.179 Uiso 1 1 calc R . . H7C H 1.1703 -0.7789 0.6516 0.179 Uiso 1 1 calc R . . C8 C 1.1599(18) -0.619(2) 0.6982(9) 0.114(10) Uani 1 1 d . . . H8A H 1.1986 -0.6437 0.7191 0.171 Uiso 1 1 calc R A . H8B H 1.1132 -0.6547 0.7029 0.171 Uiso 1 1 calc R . . H8C H 1.1514 -0.5494 0.7047 0.171 Uiso 1 1 calc R . . C9 C 1.2493(14) -0.558(2) 0.6418(11) 0.114(10) Uani 1 1 d . . . H9A H 1.2881 -0.5696 0.6651 0.171 Uiso 1 1 calc R A . H9B H 1.2300 -0.4918 0.6449 0.171 Uiso 1 1 calc R . . H9C H 1.2708 -0.5668 0.6109 0.171 Uiso 1 1 calc R . . C10 C 0.7968(9) -0.0361(12) 0.6509(6) 0.047(4) Uani 1 1 d . . . H10A H 0.7452 -0.0112 0.6468 0.056 Uiso 1 1 calc R . . H10B H 0.8096 -0.0330 0.6841 0.056 Uiso 1 1 calc R . . C11 C 0.8518(10) 0.0253(13) 0.6230(6) 0.048(5) Uani 1 1 d . . . H11A H 0.8563 0.0909 0.6367 0.058 Uiso 1 1 calc R . . H11B H 0.8336 0.0324 0.5908 0.058 Uiso 1 1 calc R . . C12 C 0.7514(10) -0.2327(14) 0.6743(5) 0.045(4) Uani 1 1 d . . . C13 C 0.7869(11) -0.2969(14) 0.7020(5) 0.054(5) Uani 1 1 d . . . H13A H 0.8392 -0.3074 0.6982 0.064 Uiso 1 1 calc R . . C14 C 0.7488(14) -0.3473(16) 0.7357(6) 0.066(6) Uani 1 1 d . . . H14A H 0.7739 -0.3949 0.7537 0.079 Uiso 1 1 calc R . . C15 C 0.6759(14) -0.3289(16) 0.7428(8) 0.073(7) Uani 1 1 d . . . H15A H 0.6503 -0.3608 0.7673 0.087 Uiso 1 1 calc R . . C16 C 0.6384(16) -0.265(2) 0.7155(10) 0.106(9) Uani 1 1 d . . . H16A H 0.5860 -0.2561 0.7194 0.127 Uiso 1 1 calc R . . C17 C 0.6762(14) -0.2136(18) 0.6825(8) 0.088(8) Uani 1 1 d . . . H17A H 0.6510 -0.1648 0.6653 0.106 Uiso 1 1 calc R . . C18 C 0.7420(9) -0.1696(13) 0.5794(6) 0.043(4) Uani 1 1 d . . . C19 C 0.7421(11) -0.2556(15) 0.5541(6) 0.058(5) Uani 1 1 d . . . H19A H 0.7739 -0.3075 0.5633 0.070 Uiso 1 1 calc R . . C20 C 0.6970(12) -0.2667(17) 0.5160(7) 0.065(6) Uani 1 1 d . . . H20A H 0.6955 -0.3266 0.4997 0.078 Uiso 1 1 calc R . . C21 C 0.6537(14) -0.1884(19) 0.5020(7) 0.080(7) Uani 1 1 d . . . H21A H 0.6234 -0.1943 0.4752 0.096 Uiso 1 1 calc R . . C22 C 0.6537(12) -0.1042(19) 0.5256(7) 0.074(7) Uani 1 1 d . . . H22A H 0.6233 -0.0517 0.5155 0.089 Uiso 1 1 calc R . . C23 C 0.6975(11) -0.0935(15) 0.5646(6) 0.059(5) Uani 1 1 d . . . H23A H 0.6971 -0.0339 0.5812 0.071 Uiso 1 1 calc R . . C24 C 0.9877(8) -0.0043(13) 0.6785(5) 0.037(4) Uani 1 1 d . . . C25 C 1.0112(15) 0.0862(15) 0.6884(8) 0.089(9) Uani 1 1 d . . . H25A H 1.0055 0.1355 0.6657 0.107 Uiso 1 1 calc R . . C26 C 1.0428(17) 0.110(2) 0.7299(9) 0.098(9) Uani 1 1 d . . . H26A H 1.0614 0.1744 0.7345 0.118 Uiso 1 1 calc R . . C27 C 1.0481(13) 0.0458(16) 0.7641(6) 0.067(6) Uani 1 1 d . . . H27A H 1.0689 0.0630 0.7932 0.081 Uiso 1 1 calc R . . C28 C 1.023(2) -0.0444(19) 0.7558(8) 0.110(11) Uani 1 1 d . . . H28A H 1.0248 -0.0919 0.7796 0.132 Uiso 1 1 calc R . . C29 C 0.9939(15) -0.0698(17) 0.7118(6) 0.087(8) Uani 1 1 d . . . H29A H 0.9787 -0.1350 0.7062 0.105 Uiso 1 1 calc R . . C30 C 1.0009(10) 0.0252(12) 0.5804(6) 0.047(4) Uani 1 1 d . . . C31 C 0.9716(11) 0.0849(14) 0.5472(5) 0.055(5) Uani 1 1 d . . . H31A H 0.9190 0.0959 0.5468 0.066 Uiso 1 1 calc R . . C32 C 1.0153(17) 0.1302(15) 0.5140(6) 0.075(7) Uani 1 1 d . . . H32A H 0.9926 0.1675 0.4901 0.090 Uiso 1 1 calc R . . C33 C 1.0930(16) 0.1204(15) 0.5160(6) 0.072(7) Uani 1 1 d . . . H33A H 1.1241 0.1518 0.4939 0.087 Uiso 1 1 calc R . . C34 C 1.1233(15) 0.0653(15) 0.5499(7) 0.075(7) Uani 1 1 d . . . H34A H 1.1762 0.0579 0.5518 0.090 Uiso 1 1 calc R . . C35 C 1.0755(11) 0.0176(15) 0.5831(7) 0.064(5) Uani 1 1 d . . . H35A H 1.0974 -0.0196 0.6073 0.076 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 Pt 0.0345(3) 0.0361(4) 0.0301(3) -0.0012(2) -0.0027(2) 0.0033(3) S1 0.063(3) 0.039(3) 0.047(2) -0.0062(18) -0.001(2) -0.007(2) S2 0.053(3) 0.058(3) 0.044(2) 0.0030(19) 0.003(2) 0.010(2) P1 0.047(3) 0.043(3) 0.041(2) -0.0063(19) -0.0070(19) 0.001(2) P2 0.040(2) 0.041(3) 0.040(2) -0.0002(18) -0.0043(18) 0.002(2) Si 0.095(5) 0.045(4) 0.115(5) -0.007(4) -0.027(4) 0.018(4) O1A 0.039(13) 0.031(15) 0.065(15) 0.015(11) 0.010(11) 0.019(11) O1 0.062(19) 0.046(18) 0.08(2) -0.001(14) 0.013(15) 0.019(14) C1 0.059(12) 0.062(13) 0.051(10) -0.010(9) 0.005(9) 0.018(10) C2 0.10(2) 0.067(18) 0.13(2) -0.045(16) -0.083(18) 0.033(15) C3 0.042(10) 0.046(12) 0.062(11) -0.010(9) -0.019(8) 0.016(9) C4 0.30(5) 0.11(3) 0.061(16) 0.016(15) -0.01(2) -0.06(3) C5 0.070(18) 0.10(2) 0.15(3) -0.041(18) -0.039(17) 0.021(16) C6 0.071(15) 0.089(19) 0.076(14) 0.028(12) 0.002(12) -0.015(14) C7 0.10(2) 0.11(2) 0.15(3) 0.05(2) 0.00(2) 0.047(19) C8 0.13(3) 0.11(2) 0.093(19) 0.010(16) 0.020(18) -0.04(2) C9 0.075(19) 0.13(3) 0.13(2) 0.039(19) -0.032(17) -0.006(18) C10 0.035(9) 0.050(12) 0.056(10) -0.010(8) 0.002(8) -0.001(8) C11 0.042(10) 0.045(11) 0.056(10) -0.022(8) -0.022(8) 0.017(8) C12 0.042(9) 0.058(12) 0.036(9) -0.007(8) 0.015(7) -0.006(9) C13 0.058(12) 0.069(14) 0.034(9) 0.002(9) 0.000(8) 0.000(11) C14 0.086(16) 0.074(15) 0.038(10) 0.010(9) -0.004(10) -0.006(13) C15 0.089(18) 0.057(15) 0.072(14) -0.002(11) 0.037(13) -0.008(13) C16 0.076(18) 0.13(3) 0.11(2) 0.031(19) 0.038(16) -0.002(18) C17 0.074(16) 0.11(2) 0.086(16) 0.038(14) 0.034(13) 0.029(15) C18 0.035(9) 0.040(11) 0.054(10) 0.005(8) -0.004(7) -0.006(8) C19 0.063(13) 0.046(12) 0.065(12) 0.003(9) -0.020(10) -0.015(10) C20 0.057(13) 0.069(15) 0.068(12) -0.009(10) -0.027(10) -0.016(11) C21 0.074(16) 0.12(2) 0.045(11) -0.017(13) -0.021(10) -0.002(15) C22 0.058(13) 0.11(2) 0.057(12) 0.003(12) -0.025(10) 0.026(13) C23 0.058(12) 0.049(13) 0.070(12) 0.003(9) -0.023(10) 0.009(10) C24 0.034(8) 0.052(11) 0.025(7) -0.002(7) 0.002(6) -0.002(8) C25 0.14(2) 0.044(13) 0.083(15) 0.010(11) -0.071(15) -0.037(14) C26 0.13(2) 0.081(19) 0.080(16) -0.006(14) -0.045(16) -0.019(18) C27 0.092(16) 0.067(16) 0.043(11) -0.018(10) -0.010(10) -0.009(13) C28 0.20(3) 0.076(19) 0.053(14) 0.008(12) -0.016(17) -0.02(2) C29 0.15(2) 0.073(16) 0.038(11) -0.009(10) -0.012(12) -0.051(16) C30 0.049(11) 0.039(11) 0.052(10) 0.009(8) -0.017(8) -0.011(9) C31 0.056(12) 0.075(14) 0.033(9) -0.008(9) -0.007(8) 0.007(11) C32 0.13(2) 0.058(15) 0.038(11) -0.006(9) -0.007(12) 0.015(14) C33 0.13(2) 0.059(15) 0.031(10) 0.010(9) 0.012(11) -0.007(14) C34 0.099(19) 0.062(15) 0.065(13) 0.007(11) 0.026(12) -0.006(13) C35 0.059(13) 0.056(14) 0.076(13) 0.011(10) -0.021(10) -0.004(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt P1 2.240(5) . ? Pt P2 2.257(5) . ? Pt S2 2.339(5) . ? Pt S1 2.361(5) . ? S1 C1 1.848(18) . ? S2 C3 1.798(19) . ? P1 C18 1.830(17) . ? P1 C12 1.846(17) . ? P1 C10 1.854(17) . ? P2 C30 1.809(18) . ? P2 C24 1.824(14) . ? P2 C11 1.876(16) . ? Si O1 1.69(3) . ? Si O1A 1.76(2) . ? Si C4 1.83(3) . ? Si C5 1.86(3) . ? Si C6 1.87(2) . ? O1A C2 1.23(3) . ? O1 C2 1.23(3) . ? C1 C2 1.48(3) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C3 1.51(3) . ? C2 H2A 1.0000 . ? C2 H2B 1.0000 . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 C7 1.51(4) . ? C6 C8 1.52(3) . ? C6 C9 1.52(3) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C11 1.53(2) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C13 1.35(2) . ? C12 C17 1.39(3) . ? C13 C14 1.38(3) . ? C13 H13A 0.9500 . ? C14 C15 1.34(3) . ? C14 H14A 0.9500 . ? C15 C16 1.36(3) . ? C15 H15A 0.9500 . ? C16 C17 1.37(3) . ? C16 H16A 0.9500 . ? C17 H17A 0.9500 . ? C18 C23 1.38(2) . ? C18 C19 1.39(3) . ? C19 C20 1.37(2) . ? C19 H19A 0.9500 . ? C20 C21 1.39(3) . ? C20 H20A 0.9500 . ? C21 C22 1.34(3) . ? C21 H21A 0.9500 . ? C22 C23 1.38(2) . ? C22 H22A 0.9500 . ? C23 H23A 0.9500 . ? C24 C29 1.33(3) . ? C24 C25 1.34(2) . ? C25 C26 1.37(3) . ? C25 H25A 0.9500 . ? C26 C27 1.33(3) . ? C26 H26A 0.9500 . ? C27 C28 1.34(3) . ? C27 H27A 0.9500 . ? C28 C29 1.42(3) . ? C28 H28A 0.9500 . ? C29 H29A 0.9500 . ? C30 C35 1.34(3) . ? C30 C31 1.37(2) . ? C31 C32 1.39(3) . ? C31 H31A 0.9500 . ? C32 C33 1.39(3) . ? C32 H32A 0.9500 . ? C33 C34 1.35(3) . ? C33 H33A 0.9500 . ? C34 C35 1.44(3) . ? C34 H34A 0.9500 . ? C35 H35A 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P1 Pt P2 86.31(17) . . ? P1 Pt S2 175.07(17) . . ? P2 Pt S2 88.90(17) . . ? P1 Pt S1 93.05(18) . . ? P2 Pt S1 177.77(15) . . ? S2 Pt S1 91.69(18) . . ? C1 S1 Pt 104.9(7) . . ? C3 S2 Pt 104.6(6) . . ? C18 P1 C12 103.5(8) . . ? C18 P1 C10 105.7(8) . . ? C12 P1 C10 103.3(8) . . ? C18 P1 Pt 115.4(6) . . ? C12 P1 Pt 119.1(6) . . ? C10 P1 Pt 108.5(6) . . ? C30 P2 C24 104.9(7) . . ? C30 P2 C11 105.4(9) . . ? C24 P2 C11 105.1(7) . . ? C30 P2 Pt 120.1(6) . . ? C24 P2 Pt 112.7(6) . . ? C11 P2 Pt 107.4(6) . . ? O1 Si O1A 40.3(11) . . ? O1 Si C4 87.3(15) . . ? O1A Si C4 127.1(14) . . ? O1 Si C5 119.7(14) . . ? O1A Si C5 96.2(12) . . ? C4 Si C5 108.9(14) . . ? O1 Si C6 116.8(13) . . ? O1A Si C6 101.1(12) . . ? C4 Si C6 112.1(16) . . ? C5 Si C6 109.7(11) . . ? C2 O1A Si 126(2) . . ? C2 O1 Si 132(3) . . ? C2 C1 S1 112.9(16) . . ? C2 C1 H1A 109.0 . . ? S1 C1 H1A 109.0 . . ? C2 C1 H1B 109.0 . . ? S1 C1 H1B 109.0 . . ? H1A C1 H1B 107.8 . . ? O1 C2 O1A 57.8(19) . . ? O1 C2 C1 111(2) . . ? O1A C2 C1 123(3) . . ? O1 C2 C3 125(3) . . ? O1A C2 C3 113(2) . . ? C1 C2 C3 115.9(18) . . ? O1 C2 H2A 44.0 . . ? O1A C2 H2A 99.8 . . ? C1 C2 H2A 99.8 . . ? C3 C2 H2A 99.8 . . ? O1 C2 H2B 99.5 . . ? O1A C2 H2B 43.5 . . ? C1 C2 H2B 99.5 . . ? C3 C2 H2B 99.5 . . ? H2A C2 H2B 143.1 . . ? C2 C3 S2 115.2(14) . . ? C2 C3 H3A 108.5 . . ? S2 C3 H3A 108.5 . . ? C2 C3 H3B 108.5 . . ? S2 C3 H3B 108.5 . . ? H3A C3 H3B 107.5 . . ? Si C4 H4A 109.5 . . ? Si C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? Si C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? Si C5 H5A 109.5 . . ? Si C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? Si C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C7 C6 C8 107(2) . . ? C7 C6 C9 112(2) . . ? C8 C6 C9 106(2) . . ? C7 C6 Si 110.0(19) . . ? C8 C6 Si 113(2) . . ? C9 C6 Si 109.2(16) . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C6 C8 H8A 109.5 . . ? C6 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C6 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C6 C9 H9A 109.5 . . ? C6 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C6 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C11 C10 P1 108.0(11) . . ? C11 C10 H10A 110.1 . . ? P1 C10 H10A 110.1 . . ? C11 C10 H10B 110.1 . . ? P1 C10 H10B 110.1 . . ? H10A C10 H10B 108.4 . . ? C10 C11 P2 108.3(12) . . ? C10 C11 H11A 110.0 . . ? P2 C11 H11A 110.0 . . ? C10 C11 H11B 110.0 . . ? P2 C11 H11B 110.0 . . ? H11A C11 H11B 108.4 . . ? C13 C12 C17 118.3(17) . . ? C13 C12 P1 121.1(14) . . ? C17 C12 P1 120.4(15) . . ? C12 C13 C14 121.2(19) . . ? C12 C13 H13A 119.4 . . ? C14 C13 H13A 119.4 . . ? C15 C14 C13 120(2) . . ? C15 C14 H14A 120.2 . . ? C13 C14 H14A 120.2 . . ? C14 C15 C16 121(2) . . ? C14 C15 H15A 119.7 . . ? C16 C15 H15A 119.7 . . ? C15 C16 C17 120(2) . . ? C15 C16 H16A 120.1 . . ? C17 C16 H16A 120.1 . . ? C16 C17 C12 120(2) . . ? C16 C17 H17A 120.0 . . ? C12 C17 H17A 120.0 . . ? C23 C18 C19 118.8(16) . . ? C23 C18 P1 123.7(14) . . ? C19 C18 P1 117.5(13) . . ? C20 C19 C18 121(2) . . ? C20 C19 H19A 119.5 . . ? C18 C19 H19A 119.5 . . ? C19 C20 C21 118(2) . . ? C19 C20 H20A 120.8 . . ? C21 C20 H20A 120.8 . . ? C22 C21 C20 121.3(19) . . ? C22 C21 H21A 119.3 . . ? C20 C21 H21A 119.3 . . ? C21 C22 C23 120(2) . . ? C21 C22 H22A 119.8 . . ? C23 C22 H22A 119.8 . . ? C18 C23 C22 119.9(19) . . ? C18 C23 H23A 120.1 . . ? C22 C23 H23A 120.1 . . ? C29 C24 C25 116.5(16) . . ? C29 C24 P2 120.2(14) . . ? C25 C24 P2 123.2(13) . . ? C24 C25 C26 123(2) . . ? C24 C25 H25A 118.6 . . ? C26 C25 H25A 118.6 . . ? C27 C26 C25 121(2) . . ? C27 C26 H26A 119.3 . . ? C25 C26 H26A 119.3 . . ? C26 C27 C28 117(2) . . ? C26 C27 H27A 121.3 . . ? C28 C27 H27A 121.3 . . ? C27 C28 C29 121(2) . . ? C27 C28 H28A 119.6 . . ? C29 C28 H28A 119.6 . . ? C24 C29 C28 121(2) . . ? C24 C29 H29A 119.4 . . ? C28 C29 H29A 119.4 . . ? C35 C30 C31 117.9(18) . . ? C35 C30 P2 118.0(14) . . ? C31 C30 P2 124.0(15) . . ? C30 C31 C32 123(2) . . ? C30 C31 H31A 118.6 . . ? C32 C31 H31A 118.6 . . ? C31 C32 C33 119.1(19) . . ? C31 C32 H32A 120.4 . . ? C33 C32 H32A 120.4 . . ? C34 C33 C32 119(2) . . ? C34 C33 H33A 120.6 . . ? C32 C33 H33A 120.6 . . ? C33 C34 C35 120(2) . . ? C33 C34 H34A 119.9 . . ? C35 C34 H34A 119.9 . . ? C30 C35 C34 120.9(19) . . ? C30 C35 H35A 119.6 . . ? C34 C35 H35A 119.6 . . ? _diffrn_measured_fraction_theta_max 0.836 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.879 _refine_diff_density_max 2.655 _refine_diff_density_min -2.228 _refine_diff_density_rms 0.286 #==== END data_FO3219 _database_code_depnum_ccdc_archive 'CCDC 776106' #TrackingRef '- dalton.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C29 H30 O P2 Pt S2' _chemical_formula_sum 'C29 H30 O P2 Pt S2' _chemical_formula_weight 715.68 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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' 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 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' 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 9.1382(3) _cell_length_b 25.8648(9) _cell_length_c 12.1756(4) _cell_angle_alpha 90.00 _cell_angle_beta 106.278(2) _cell_angle_gamma 90.00 _cell_volume 2762.43(16) _cell_formula_units_Z 4 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used 15833 _cell_measurement_theta_min 2.45 _cell_measurement_theta_max 27.49 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.06 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.721 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1408 _exptl_absorpt_coefficient_mu 5.368 _exptl_absorpt_correction_type NONE _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 183(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 KappaCCD _diffrn_measurement_method 'phi- + omega-scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15833 _diffrn_reflns_av_R_equivalents 0.0636 _diffrn_reflns_av_sigmaI/netI 0.0776 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.45 _diffrn_reflns_theta_max 27.49 _reflns_number_total 6188 _reflns_number_gt 4081 _reflns_threshold_expression >2sigma(I) _computing_data_collection COLLECT _computing_cell_refinement DENZO _computing_data_reduction DENZO _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL/PC _computing_publication_material SHELXL-97 _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^)+(0.0815P)^2^+8.5584P] 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 6188 _refine_ls_number_parameters 311 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1019 _refine_ls_R_factor_gt 0.0569 _refine_ls_wR_factor_ref 0.1598 _refine_ls_wR_factor_gt 0.1359 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.023 _refine_ls_shift/su_max 0.087 _refine_ls_shift/su_mean 0.004 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 Pt Pt 0.43649(4) 0.358770(13) 0.17636(3) 0.03952(15) Uani 1 1 d . . . S1 S 0.2412(4) 0.34951(11) 0.0087(3) 0.0728(10) Uani 1 1 d . A . S2 S 0.4260(5) 0.44768(17) 0.1440(4) 0.0331(9) Uiso 0.50 1 d P A 1 S2A S 0.4818(7) 0.4407(2) 0.1124(5) 0.0561(14) Uiso 0.50 1 d P A 2 P1 P 0.4405(2) 0.27584(8) 0.23538(18) 0.0303(5) Uani 1 1 d . A . P2 P 0.6343(3) 0.37054(9) 0.33264(19) 0.0352(5) Uani 1 1 d . A . C4 C 0.5695(10) 0.2730(3) 0.3801(7) 0.038(2) Uani 1 1 d . . . H4A H 0.5159 0.2849 0.4357 0.046 Uiso 1 1 calc R A . H4B H 0.6031 0.2369 0.3992 0.046 Uiso 1 1 calc R . . C5 C 0.7056(10) 0.3068(3) 0.3876(8) 0.041(2) Uani 1 1 d . A . H5A H 0.7689 0.2920 0.3415 0.049 Uiso 1 1 calc R . . H5B H 0.7688 0.3096 0.4680 0.049 Uiso 1 1 calc R . . C6 C 0.2696(10) 0.2420(3) 0.2484(8) 0.040(2) Uani 1 1 d . . . C7 C 0.1286(11) 0.2569(5) 0.1811(8) 0.057(3) Uani 1 1 d . A . H7A H 0.1188 0.2846 0.1285 0.068 Uiso 1 1 calc R . . C8 C -0.0022(14) 0.2301(6) 0.1916(10) 0.077(4) Uani 1 1 d . . . H8A H -0.1008 0.2399 0.1461 0.092 Uiso 1 1 calc R A . C9 C 0.0138(16) 0.1900(5) 0.2675(14) 0.080(4) Uani 1 1 d . A . H9A H -0.0745 0.1722 0.2738 0.096 Uiso 1 1 calc R . . C10 C 0.1519(16) 0.1751(5) 0.3335(12) 0.075(4) Uani 1 1 d . . . H10A H 0.1609 0.1466 0.3842 0.090 Uiso 1 1 calc R A . C11 C 0.2824(12) 0.2022(4) 0.3268(10) 0.056(3) Uani 1 1 d . A . H11A H 0.3795 0.1932 0.3759 0.067 Uiso 1 1 calc R . . C12 C 0.5208(9) 0.2301(3) 0.1526(7) 0.0308(18) Uani 1 1 d . . . C13 C 0.5569(11) 0.1793(3) 0.1900(8) 0.043(2) Uani 1 1 d . A . H13A H 0.5419 0.1679 0.2602 0.052 Uiso 1 1 calc R . . C14 C 0.6146(11) 0.1458(4) 0.1241(8) 0.046(2) Uani 1 1 d . . . H14A H 0.6393 0.1113 0.1493 0.056 Uiso 1 1 calc R A . C15 C 0.6365(12) 0.1619(5) 0.0226(9) 0.054(3) Uani 1 1 d . A . H15A H 0.6748 0.1384 -0.0226 0.065 Uiso 1 1 calc R . . C16 C 0.6037(10) 0.2112(4) -0.0134(8) 0.044(2) Uani 1 1 d . . . H16A H 0.6190 0.2220 -0.0839 0.053 Uiso 1 1 calc R A . C17 C 0.5489(9) 0.2457(4) 0.0506(7) 0.037(2) Uani 1 1 d . A . H17A H 0.5298 0.2804 0.0254 0.045 Uiso 1 1 calc R . . C18 C 0.7993(10) 0.4046(3) 0.3108(7) 0.038(2) Uani 1 1 d . . . C19 C 0.8809(13) 0.3813(5) 0.2427(9) 0.063(3) Uani 1 1 d . A . H19A H 0.8497 0.3487 0.2077 0.076 Uiso 1 1 calc R . . C20 C 1.0082(14) 0.4061(4) 0.2265(10) 0.063(3) Uani 1 1 d . . . H20A H 1.0652 0.3900 0.1817 0.076 Uiso 1 1 calc R A . C21 C 1.0514(12) 0.4524(5) 0.2734(9) 0.059(3) Uani 1 1 d . A . H21A H 1.1389 0.4686 0.2616 0.071 Uiso 1 1 calc R . . C22 C 0.9717(11) 0.4766(4) 0.3381(10) 0.060(3) Uani 1 1 d . . . H22A H 1.0010 0.5100 0.3690 0.072 Uiso 1 1 calc R A . C23 C 0.8475(11) 0.4517(4) 0.3577(9) 0.051(2) Uani 1 1 d . A . H23A H 0.7942 0.4678 0.4053 0.062 Uiso 1 1 calc R . . C24 C 0.5917(10) 0.4019(3) 0.4538(7) 0.039(2) Uani 1 1 d . . . C25 C 0.6982(12) 0.4058(4) 0.5594(8) 0.054(3) Uani 1 1 d . A . H25A H 0.7983 0.3928 0.5698 0.065 Uiso 1 1 calc R . . C26 C 0.6595(18) 0.4286(4) 0.6499(9) 0.075(4) Uani 1 1 d . . . H26A H 0.7327 0.4309 0.7226 0.090 Uiso 1 1 calc R A . C27 C 0.5145(18) 0.4481(4) 0.6348(11) 0.071(3) Uani 1 1 d . A . H27A H 0.4895 0.4650 0.6965 0.086 Uiso 1 1 calc R . . C28 C 0.4104(15) 0.4433(4) 0.5353(12) 0.069(3) Uani 1 1 d . . . H28A H 0.3094 0.4550 0.5271 0.083 Uiso 1 1 calc R A . C29 C 0.4476(11) 0.4210(4) 0.4413(9) 0.050(2) Uani 1 1 d . A . H29A H 0.3732 0.4192 0.3691 0.060 Uiso 1 1 calc R . . O1 O 0.294(2) 0.5466(9) 0.0357(18) 0.113(3) Uiso 0.50 1 d P A 1 H1A H 0.2316 0.5668 0.0526 0.169 Uiso 0.50 1 calc PR A 1 C1 C 0.237(5) 0.4086(14) -0.064(3) 0.113(3) Uiso 0.50 1 d P A 1 H1B H 0.2447 0.4000 -0.1411 0.135 Uiso 0.50 1 calc PR A 1 H1C H 0.1343 0.4234 -0.0739 0.135 Uiso 0.50 1 calc PR A 1 C2 C 0.350(4) 0.4520(16) -0.019(3) 0.113(3) Uiso 0.50 1 d P A 1 H2A H 0.4151 0.4660 -0.0660 0.135 Uiso 0.50 1 calc PR A 1 C3 C 0.219(4) 0.4882(14) 0.013(3) 0.113(3) Uiso 0.50 1 d P A 1 H3A H 0.1244 0.4886 -0.0511 0.135 Uiso 0.50 1 calc PR A 1 H3B H 0.1954 0.4751 0.0823 0.135 Uiso 0.50 1 calc PR A 1 O1A O 0.316(2) 0.4539(9) -0.2010(19) 0.113(3) Uiso 0.50 1 d P A 2 H1AA H 0.3394 0.4379 -0.2539 0.169 Uiso 0.50 1 calc PR A 2 C1A C 0.163(4) 0.4221(14) -0.031(3) 0.113(3) Uiso 0.50 1 d P A 2 H1AB H 0.1194 0.4259 -0.1144 0.135 Uiso 0.50 1 calc PR A 2 H1AC H 0.0830 0.4305 0.0071 0.135 Uiso 0.50 1 calc PR A 2 C2A C 0.288(5) 0.4547(18) 0.009(3) 0.113(3) Uiso 0.50 1 d P A 2 H2AA H 0.2684 0.4919 -0.0122 0.135 Uiso 0.50 1 calc PR A 2 C3A C 0.353(5) 0.4181(15) -0.088(3) 0.113(3) Uiso 0.50 1 d P A 2 H3AA H 0.4633 0.4111 -0.0589 0.135 Uiso 0.50 1 calc PR A 2 H3AB H 0.2974 0.3848 -0.1045 0.135 Uiso 0.50 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt 0.0404(2) 0.0302(2) 0.0351(2) 0.00288(14) -0.01053(15) -0.00428(15) S1 0.086(2) 0.0460(15) 0.0511(16) 0.0092(12) -0.0396(15) -0.0164(14) P1 0.0285(11) 0.0311(11) 0.0285(11) -0.0013(9) 0.0032(9) -0.0025(9) P2 0.0298(12) 0.0329(11) 0.0347(12) -0.0007(9) -0.0046(9) -0.0050(9) C4 0.040(5) 0.041(5) 0.026(4) 0.001(4) -0.005(4) 0.001(4) C5 0.034(5) 0.041(5) 0.040(5) 0.009(4) -0.001(4) -0.002(4) C6 0.034(5) 0.036(5) 0.051(5) -0.015(4) 0.014(4) -0.007(4) C7 0.045(6) 0.082(8) 0.044(6) -0.020(5) 0.014(5) -0.018(6) C8 0.049(7) 0.116(12) 0.064(8) -0.036(8) 0.014(6) -0.025(8) C9 0.066(9) 0.073(9) 0.114(11) -0.032(8) 0.047(9) -0.040(7) C10 0.083(10) 0.064(8) 0.094(10) -0.010(7) 0.050(8) -0.013(7) C11 0.055(6) 0.040(6) 0.083(8) -0.008(5) 0.036(6) -0.011(5) C12 0.026(4) 0.032(4) 0.030(4) -0.002(3) 0.001(3) -0.003(3) C13 0.050(6) 0.041(5) 0.039(5) -0.005(4) 0.013(4) 0.003(4) C14 0.051(6) 0.043(5) 0.046(6) -0.001(4) 0.015(5) 0.021(4) C15 0.047(6) 0.072(7) 0.049(6) -0.019(5) 0.021(5) 0.008(5) C16 0.031(5) 0.072(7) 0.032(5) -0.005(5) 0.011(4) 0.001(5) C17 0.030(5) 0.047(5) 0.033(5) 0.005(4) 0.005(4) -0.003(4) C18 0.032(5) 0.034(5) 0.039(5) -0.006(4) -0.002(4) -0.006(4) C19 0.079(8) 0.069(7) 0.049(6) -0.011(6) 0.031(6) -0.024(7) C20 0.081(8) 0.057(7) 0.059(7) 0.008(6) 0.032(6) 0.000(6) C21 0.044(6) 0.076(8) 0.058(7) 0.003(6) 0.016(5) -0.008(6) C22 0.039(6) 0.054(6) 0.080(8) -0.017(6) 0.005(6) -0.021(5) C23 0.042(6) 0.046(6) 0.064(6) -0.006(5) 0.011(5) -0.008(5) C24 0.035(5) 0.040(5) 0.038(5) 0.003(4) 0.007(4) -0.001(4) C25 0.054(6) 0.052(6) 0.047(6) -0.006(5) -0.001(5) 0.005(5) C26 0.120(12) 0.049(7) 0.041(6) -0.008(5) -0.004(7) -0.015(7) C27 0.104(11) 0.046(7) 0.072(9) -0.016(6) 0.038(8) -0.014(7) C28 0.081(9) 0.042(6) 0.096(10) -0.027(6) 0.045(8) -0.010(6) C29 0.048(6) 0.042(5) 0.055(6) 0.002(5) 0.007(5) -0.012(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 Pt P2 2.248(2) . ? Pt P1 2.259(2) . ? Pt S1 2.316(3) . ? Pt S2 2.330(4) . ? Pt S2A 2.336(6) . ? S1 C1 1.76(4) . ? S1 C1A 2.02(4) . ? S2 C2 1.91(4) . ? S2A C2A 1.90(4) . ? P1 C4 1.827(8) . ? P1 C6 1.835(9) . ? P1 C12 1.837(8) . ? P2 C24 1.819(9) . ? P2 C5 1.830(9) . ? P2 C18 1.829(9) . ? C4 C5 1.501(12) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C7 1.374(14) . ? C6 C11 1.387(14) . ? C7 C8 1.419(15) . ? C7 H7A 0.9500 . ? C8 C9 1.369(19) . ? C8 H8A 0.9500 . ? C9 C10 1.348(19) . ? C9 H9A 0.9500 . ? C10 C11 1.404(15) . ? C10 H10A 0.9500 . ? C11 H11A 0.9500 . ? C12 C17 1.396(11) . ? C12 C13 1.400(12) . ? C13 C14 1.381(12) . ? C13 H13A 0.9500 . ? C14 C15 1.370(14) . ? C14 H14A 0.9500 . ? C15 C16 1.356(15) . ? C15 H15A 0.9500 . ? C16 C17 1.368(12) . ? C16 H16A 0.9500 . ? C17 H17A 0.9500 . ? C18 C23 1.364(12) . ? C18 C19 1.399(14) . ? C19 C20 1.390(15) . ? C19 H19A 0.9500 . ? C20 C21 1.336(15) . ? C20 H20A 0.9500 . ? C21 C22 1.366(15) . ? C21 H21A 0.9500 . ? C22 C23 1.384(13) . ? C22 H22A 0.9500 . ? C23 H23A 0.9500 . ? C24 C25 1.382(13) . ? C24 C29 1.374(13) . ? C25 C26 1.380(16) . ? C25 H25A 0.9500 . ? C26 C27 1.380(18) . ? C26 H26A 0.9500 . ? C27 C28 1.321(17) . ? C27 H27A 0.9500 . ? C28 C29 1.405(14) . ? C28 H28A 0.9500 . ? C29 H29A 0.9500 . ? O1 C3 1.65(4) . ? O1 H1A 0.8400 . ? C1 C2 1.52(5) . ? C1 H1B 0.9900 . ? C1 H1C 0.9900 . ? C2 C3 1.65(5) . ? C2 H2A 1.0000 . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? O1A C3A 1.61(4) . ? O1A H1AA 0.8400 . ? C1A C2A 1.39(5) . ? C1A H1AB 0.9900 . ? C1A H1AC 0.9900 . ? C2A C3A 1.74(5) . ? C2A H2AA 1.0000 . ? C3A H3AA 0.9900 . ? C3A H3AB 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P2 Pt P1 85.53(8) . . ? P2 Pt S1 176.37(11) . . ? P1 Pt S1 96.99(9) . . ? P2 Pt S2 89.69(12) . . ? P1 Pt S2 170.68(12) . . ? S1 Pt S2 88.18(12) . . ? P2 Pt S2A 89.06(15) . . ? P1 Pt S2A 168.37(17) . . ? S1 Pt S2A 87.99(16) . . ? S2 Pt S2A 18.31(14) . . ? C1 S1 C1A 27.9(14) . . ? C1 S1 Pt 104.7(12) . . ? C1A S1 Pt 104.3(11) . . ? C2 S2 Pt 102.6(12) . . ? C2A S2A Pt 100.1(13) . . ? C4 P1 C6 103.4(4) . . ? C4 P1 C12 104.7(4) . . ? C6 P1 C12 102.8(4) . . ? C4 P1 Pt 107.0(3) . . ? C6 P1 Pt 122.8(3) . . ? C12 P1 Pt 114.3(3) . . ? C24 P2 C5 103.9(4) . . ? C24 P2 C18 106.0(4) . . ? C5 P2 C18 105.3(4) . . ? C24 P2 Pt 116.3(3) . . ? C5 P2 Pt 107.9(3) . . ? C18 P2 Pt 116.3(3) . . ? C5 C4 P1 109.6(6) . . ? C5 C4 H4A 109.8 . . ? P1 C4 H4A 109.8 . . ? C5 C4 H4B 109.7 . . ? P1 C4 H4B 109.8 . . ? H4A C4 H4B 108.2 . . ? C4 C5 P2 107.3(6) . . ? C4 C5 H5A 110.2 . . ? P2 C5 H5A 110.2 . . ? C4 C5 H5B 110.2 . . ? P2 C5 H5B 110.2 . . ? H5A C5 H5B 108.5 . . ? C7 C6 C11 120.2(9) . . ? C7 C6 P1 119.6(8) . . ? C11 C6 P1 120.3(7) . . ? C6 C7 C8 118.9(12) . . ? C6 C7 H7A 120.6 . . ? C8 C7 H7A 120.6 . . ? C9 C8 C7 119.8(12) . . ? C9 C8 H8A 120.1 . . ? C7 C8 H8A 120.1 . . ? C10 C9 C8 121.5(11) . . ? C10 C9 H9A 119.2 . . ? C8 C9 H9A 119.2 . . ? C9 C10 C11 119.5(13) . . ? C9 C10 H10A 120.3 . . ? C11 C10 H10A 120.3 . . ? C6 C11 C10 120.0(11) . . ? C6 C11 H11A 120.0 . . ? C10 C11 H11A 120.0 . . ? C17 C12 C13 118.4(8) . . ? C17 C12 P1 120.2(6) . . ? C13 C12 P1 121.4(6) . . ? C14 C13 C12 119.5(8) . . ? C14 C13 H13A 120.2 . . ? C12 C13 H13A 120.2 . . ? C15 C14 C13 120.6(9) . . ? C15 C14 H14A 119.7 . . ? C13 C14 H14A 119.7 . . ? C16 C15 C14 120.2(9) . . ? C16 C15 H15A 119.9 . . ? C14 C15 H15A 119.9 . . ? C15 C16 C17 120.8(9) . . ? C15 C16 H16A 119.6 . . ? C17 C16 H16A 119.6 . . ? C16 C17 C12 120.4(9) . . ? C16 C17 H17A 119.8 . . ? C12 C17 H17A 119.8 . . ? C23 C18 C19 118.1(9) . . ? C23 C18 P2 123.5(7) . . ? C19 C18 P2 118.5(7) . . ? C20 C19 C18 119.4(10) . . ? C20 C19 H19A 120.3 . . ? C18 C19 H19A 120.3 . . ? C21 C20 C19 120.8(11) . . ? C21 C20 H20A 119.6 . . ? C19 C20 H20A 119.6 . . ? C20 C21 C22 121.1(10) . . ? C20 C21 H21A 119.5 . . ? C22 C21 H21A 119.5 . . ? C21 C22 C23 118.7(10) . . ? C21 C22 H22A 120.6 . . ? C23 C22 H22A 120.6 . . ? C18 C23 C22 121.9(10) . . ? C18 C23 H23A 119.1 . . ? C22 C23 H23A 119.1 . . ? C25 C24 C29 118.7(9) . . ? C25 C24 P2 122.2(7) . . ? C29 C24 P2 119.1(7) . . ? C24 C25 C26 120.2(10) . . ? C24 C25 H25A 119.9 . . ? C26 C25 H25A 119.9 . . ? C27 C26 C25 120.0(11) . . ? C27 C26 H26A 120.0 . . ? C25 C26 H26A 120.0 . . ? C28 C27 C26 120.4(11) . . ? C28 C27 H27A 119.8 . . ? C26 C27 H27A 119.8 . . ? C27 C28 C29 120.6(12) . . ? C27 C28 H28A 119.7 . . ? C29 C28 H28A 119.7 . . ? C24 C29 C28 120.0(10) . . ? C24 C29 H29A 120.0 . . ? C28 C29 H29A 120.0 . . ? C3 O1 H1A 109.5 . . ? C2 C1 S1 123(3) . . ? C2 C1 H1B 106.5 . . ? S1 C1 H1B 106.6 . . ? C2 C1 H1C 106.6 . . ? S1 C1 H1C 106.5 . . ? H1B C1 H1C 106.5 . . ? C1 C2 C3 92(3) . . ? C1 C2 S2 110(3) . . ? C3 C2 S2 82(2) . . ? C1 C2 H2A 120.9 . . ? C3 C2 H2A 121.1 . . ? S2 C2 H2A 120.9 . . ? O1 C3 C2 105(2) . . ? O1 C3 H3A 110.5 . . ? C2 C3 H3A 110.6 . . ? O1 C3 H3B 110.7 . . ? C2 C3 H3B 110.8 . . ? H3A C3 H3B 108.7 . . ? C3A O1A H1AA 109.5 . . ? C2A C1A S1 106(3) . . ? C2A C1A H1AB 110.5 . . ? S1 C1A H1AB 110.5 . . ? C2A C1A H1AC 110.5 . . ? S1 C1A H1AC 110.5 . . ? H1AB C1A H1AC 108.7 . . ? C1A C2A C3A 81(3) . . ? C1A C2A S2A 130(3) . . ? C3A C2A S2A 85(2) . . ? C1A C2A H2AA 115.0 . . ? C3A C2A H2AA 114.9 . . ? S2A C2A H2AA 114.9 . . ? O1A C3A C2A 104(3) . . ? O1A C3A H3AA 111.1 . . ? C2A C3A H3AA 111.0 . . ? O1A C3A H3AB 111.0 . . ? C2A C3A H3AB 111.0 . . ? H3AA C3A H3AB 109.0 . . ? _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 1.946 _refine_diff_density_min -1.788 _refine_diff_density_rms 0.218