# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_FO3784 _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C12 H14 Br Cl O2 Pt S3' _chemical_formula_sum 'C12 H14 Br Cl O2 Pt S3' _chemical_formula_weight 596.86 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' 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' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P b c a' _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 10.3014(3) _cell_length_b 18.1303(5) _cell_length_c 35.8617(12) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6697.8(3) _cell_formula_units_Z 16 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.11 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.368 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4480 _exptl_absorpt_coefficient_mu 11.296 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [SORTAV, R.H. Blessing, J. Applied Cryst. 1997, 30, 421-426] ; _exptl_absorpt_correction_T_min 0.1351 _exptl_absorpt_correction_T_max 0.2893 _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_reflns_number 38176 _diffrn_reflns_av_R_equivalents 0.1633 _diffrn_reflns_av_sigmaI/netI 0.1739 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 46 _diffrn_reflns_theta_min 2.25 _diffrn_reflns_theta_max 27.47 _reflns_number_total 7665 _reflns_number_gt 3686 _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^)+(0.0147P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7665 _refine_ls_number_parameters 367 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1527 _refine_ls_R_factor_gt 0.0470 _refine_ls_wR_factor_ref 0.0729 _refine_ls_wR_factor_gt 0.0570 _refine_ls_goodness_of_fit_ref 0.898 _refine_ls_restrained_S_all 0.898 _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 Pt1A Pt -0.40421(3) 0.49914(2) 0.169999(10) 0.02308(10) Uani 1 1 d . . . Br1A Br -0.69748(10) 0.15711(6) 0.01828(3) 0.0482(3) Uani 1 1 d . . . Cl1A Cl -0.6253(2) 0.52756(13) 0.16903(7) 0.0387(7) Uani 1 1 d . . . S1A S -0.1921(2) 0.46932(12) 0.17281(7) 0.0265(6) Uani 1 1 d . . . S2A S -0.0125(2) 0.35392(13) 0.14639(7) 0.0331(7) Uani 1 1 d . . . S3A S -0.3675(2) 0.58422(13) 0.21245(7) 0.0286(6) Uani 1 1 d . . . O1A O -0.4528(5) 0.4227(3) 0.13176(15) 0.0226(15) Uani 1 1 d . . . O2A O -0.2324(6) 0.6022(3) 0.22026(16) 0.0392(17) Uani 1 1 d . . . C1A C -0.1680(8) 0.3931(4) 0.1477(2) 0.024(2) Uani 1 1 d . . . C2A C -0.2573(10) 0.3546(4) 0.1244(2) 0.027(2) Uani 1 1 d . . . H2AA H -0.2238 0.3128 0.1117 0.032 Uiso 1 1 calc R . . C3A C -0.3885(9) 0.3709(5) 0.1180(2) 0.021(2) Uani 1 1 d . . . C4A C -0.4617(9) 0.3213(4) 0.0919(2) 0.020(2) Uani 1 1 d . . . C5A C -0.4001(9) 0.2780(5) 0.0647(2) 0.027(2) Uani 1 1 d . . . H5AA H -0.3089 0.2813 0.0612 0.033 Uiso 1 1 calc R . . C6A C -0.4734(9) 0.2304(5) 0.0432(3) 0.030(3) Uani 1 1 d . . . H6AA H -0.4321 0.2015 0.0246 0.036 Uiso 1 1 calc R . . C7A C -0.6016(10) 0.2245(5) 0.0481(2) 0.028(2) Uani 1 1 d . . . C8A C -0.6661(9) 0.2660(5) 0.0744(2) 0.027(2) Uani 1 1 d . . . H8AA H -0.7571 0.2609 0.0777 0.033 Uiso 1 1 calc R . . C9A C -0.5942(9) 0.3162(5) 0.0961(2) 0.029(2) Uani 1 1 d . . . H9AA H -0.6374 0.3467 0.1138 0.035 Uiso 1 1 calc R . . C10A C 0.0866(8) 0.4124(5) 0.1751(2) 0.033(2) Uani 1 1 d . . . H10A H 0.1784 0.4029 0.1697 0.049 Uiso 1 1 calc R . . H10B H 0.0690 0.4020 0.2014 0.049 Uiso 1 1 calc R . . H10C H 0.0665 0.4642 0.1697 0.049 Uiso 1 1 calc R . . C11A C -0.4492(10) 0.6666(5) 0.2021(3) 0.058(4) Uani 1 1 d . . . H11A H -0.4263 0.7042 0.2206 0.087 Uiso 1 1 calc R . . H11B H -0.5431 0.6580 0.2027 0.087 Uiso 1 1 calc R . . H11C H -0.4238 0.6836 0.1772 0.087 Uiso 1 1 calc R . . C12A C -0.4427(9) 0.5576(5) 0.2544(3) 0.059(3) Uani 1 1 d . . . H12A H -0.4421 0.5992 0.2719 0.089 Uiso 1 1 calc R . . H12B H -0.3954 0.5160 0.2653 0.089 Uiso 1 1 calc R . . H12C H -0.5326 0.5429 0.2494 0.089 Uiso 1 1 calc R . . Pt1B Pt 0.75851(4) 0.096547(19) 0.085655(10) 0.02554(10) Uani 1 1 d . . . Br1B Br 0.33877(10) 0.36110(5) 0.24820(3) 0.0416(3) Uani 1 1 d . . . Cl1B Cl 0.9121(2) 0.18597(13) 0.10203(7) 0.0399(7) Uani 1 1 d . . . S1B S 0.6131(2) 0.01277(12) 0.06658(7) 0.0300(6) Uani 1 1 d . . . S2B S 0.3432(2) -0.03204(14) 0.07918(7) 0.0365(7) Uani 1 1 d . . . S3B S 0.8939(2) 0.05396(13) 0.04397(7) 0.0282(6) Uani 1 1 d . . . O1B O 0.6445(6) 0.1434(3) 0.12426(16) 0.0249(16) Uani 1 1 d . . . O2B O 0.8508(6) -0.0099(3) 0.02165(16) 0.0381(17) Uani 1 1 d . . . C1B C 0.4724(8) 0.0274(5) 0.0896(3) 0.026(2) Uani 1 1 d . . . C2B C 0.4421(9) 0.0807(5) 0.1173(2) 0.030(3) Uani 1 1 d . . . H2BA H 0.3559 0.0799 0.1268 0.036 Uiso 1 1 calc R . . C3B C 0.5244(9) 0.1337(5) 0.1321(2) 0.022(2) Uani 1 1 d . . . C4B C 0.4725(9) 0.1853(5) 0.1612(2) 0.026(3) Uani 1 1 d . . . C5B C 0.3432(9) 0.1936(5) 0.1696(2) 0.032(3) Uani 1 1 d . . . H5BA H 0.2815 0.1625 0.1577 0.039 Uiso 1 1 calc R . . C6B C 0.3001(9) 0.2458(5) 0.1949(3) 0.031(3) Uani 1 1 d . . . H6BA H 0.2103 0.2503 0.2004 0.037 Uiso 1 1 calc R . . C7B C 0.3894(9) 0.2910(5) 0.2118(2) 0.025(2) Uani 1 1 d . . . C8B C 0.5205(9) 0.2846(5) 0.2049(3) 0.031(3) Uani 1 1 d . . . H8BA H 0.5813 0.3154 0.2174 0.037 Uiso 1 1 calc R . . C9B C 0.5620(8) 0.2316(5) 0.1792(3) 0.026(2) Uani 1 1 d . . . H9BA H 0.6520 0.2270 0.1738 0.032 Uiso 1 1 calc R . . C10B C 0.4048(9) -0.0935(5) 0.0439(2) 0.041(3) Uani 1 1 d . . . H10D H 0.3351 -0.1264 0.0355 0.062 Uiso 1 1 calc R . . H10E H 0.4759 -0.1229 0.0543 0.062 Uiso 1 1 calc R . . H10F H 0.4368 -0.0646 0.0227 0.062 Uiso 1 1 calc R . . C11B C 0.9346(8) 0.1249(5) 0.0127(2) 0.039(3) Uani 1 1 d . . . H11D H 1.0002 0.1070 -0.0049 0.059 Uiso 1 1 calc R . . H11E H 0.9694 0.1671 0.0265 0.059 Uiso 1 1 calc R . . H11F H 0.8569 0.1402 -0.0011 0.059 Uiso 1 1 calc R . . C12B C 1.0462(8) 0.0348(4) 0.0643(2) 0.032(3) Uani 1 1 d . . . H12D H 1.1089 0.0226 0.0447 0.049 Uiso 1 1 calc R . . H12E H 1.0379 -0.0070 0.0815 0.049 Uiso 1 1 calc R . . H12F H 1.0765 0.0782 0.0781 0.049 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 Pt1A 0.0238(2) 0.02192(19) 0.02348(19) -0.0008(2) -0.0023(2) 0.0002(2) Br1A 0.0524(8) 0.0471(7) 0.0449(7) -0.0046(6) -0.0149(6) -0.0165(6) Cl1A 0.0258(15) 0.0386(15) 0.0516(18) -0.0108(13) -0.0033(13) 0.0016(11) S1A 0.0257(15) 0.0234(14) 0.0303(15) -0.0016(12) -0.0032(12) -0.0021(11) S2A 0.0271(16) 0.0308(16) 0.0415(18) -0.0060(14) -0.0066(13) 0.0000(13) S3A 0.0292(16) 0.0291(16) 0.0273(15) -0.0036(12) -0.0005(12) -0.0005(13) O1A 0.027(4) 0.018(4) 0.023(4) -0.004(3) -0.007(3) 0.002(3) O2A 0.035(5) 0.044(4) 0.038(4) -0.016(3) -0.003(3) -0.006(4) C1A 0.023(6) 0.015(5) 0.033(6) 0.009(5) -0.001(5) 0.001(5) C2A 0.044(7) 0.015(5) 0.022(5) 0.000(4) 0.002(6) -0.004(5) C3A 0.027(6) 0.016(5) 0.018(5) 0.006(4) -0.003(5) -0.009(5) C4A 0.022(6) 0.019(5) 0.021(6) 0.010(4) -0.010(5) -0.005(5) C5A 0.022(6) 0.025(6) 0.034(6) 0.011(5) 0.000(5) -0.002(5) C6A 0.033(7) 0.022(6) 0.034(7) -0.005(5) -0.009(5) -0.011(5) C7A 0.040(7) 0.020(6) 0.024(6) 0.011(5) -0.015(6) -0.006(6) C8A 0.017(6) 0.041(7) 0.024(6) 0.010(5) 0.000(5) -0.007(5) C9A 0.038(7) 0.018(5) 0.032(6) 0.003(4) -0.006(5) 0.002(5) C10A 0.022(6) 0.042(6) 0.035(6) 0.002(5) -0.010(5) 0.003(5) C11A 0.071(9) 0.031(7) 0.072(9) -0.002(6) -0.035(7) 0.012(6) C12A 0.079(9) 0.065(8) 0.035(7) -0.008(6) 0.026(7) -0.012(7) Pt1B 0.0237(2) 0.0259(2) 0.0271(2) 0.00023(19) 0.0043(2) 0.0010(2) Br1B 0.0406(7) 0.0457(7) 0.0385(7) -0.0110(6) 0.0035(5) 0.0034(6) Cl1B 0.0341(17) 0.0311(15) 0.0545(18) -0.0106(13) 0.0062(14) -0.0032(13) S1B 0.0302(16) 0.0307(16) 0.0290(14) -0.0047(12) 0.0040(12) -0.0020(13) S2B 0.0271(16) 0.0416(17) 0.0409(18) -0.0039(13) -0.0004(13) -0.0052(13) S3B 0.0244(15) 0.0337(15) 0.0265(15) 0.0008(12) 0.0055(13) 0.0003(13) O1B 0.019(4) 0.019(4) 0.037(4) -0.004(3) 0.012(3) -0.004(3) O2B 0.037(4) 0.041(4) 0.036(4) -0.006(4) 0.013(3) 0.002(4) C1B 0.028(6) 0.025(6) 0.026(6) 0.012(5) -0.005(5) 0.005(5) C2B 0.026(6) 0.030(6) 0.034(7) 0.005(5) 0.012(5) 0.007(5) C3B 0.029(7) 0.019(6) 0.019(6) 0.012(4) -0.003(5) 0.001(5) C4B 0.029(7) 0.022(6) 0.026(7) 0.012(5) 0.008(5) 0.004(5) C5B 0.034(7) 0.033(6) 0.030(6) -0.012(5) 0.003(5) 0.001(5) C6B 0.014(6) 0.027(6) 0.052(8) 0.001(5) 0.003(5) -0.004(5) C7B 0.018(6) 0.030(6) 0.027(6) -0.006(5) 0.001(5) 0.013(5) C8B 0.037(7) 0.023(6) 0.034(7) 0.000(5) -0.003(5) -0.003(5) C9B 0.010(6) 0.033(6) 0.036(7) 0.004(5) 0.004(5) 0.004(5) C10B 0.048(7) 0.054(7) 0.022(6) -0.017(5) 0.003(5) -0.021(6) C11B 0.032(7) 0.062(7) 0.024(6) 0.013(5) -0.004(5) 0.008(5) C12B 0.036(7) 0.029(6) 0.032(6) 0.012(5) 0.005(5) 0.006(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 Pt1A O1A 2.013(5) . ? Pt1A S3A 2.200(2) . ? Pt1A S1A 2.253(2) . ? Pt1A Cl1A 2.336(2) . ? Br1A C7A 1.901(9) . ? S1A C1A 1.668(9) . ? S2A C1A 1.752(8) . ? S2A C10A 1.796(8) . ? S3A O2A 1.457(6) . ? S3A C11A 1.754(8) . ? S3A C12A 1.761(9) . ? O1A C3A 1.251(9) . ? C1A C2A 1.425(11) . ? C2A C3A 1.403(11) . ? C2A H2AA 0.9500 . ? C3A C4A 1.500(11) . ? C4A C9A 1.377(11) . ? C4A C5A 1.404(11) . ? C5A C6A 1.383(11) . ? C5A H5AA 0.9500 . ? C6A C7A 1.336(11) . ? C6A H6AA 0.9500 . ? C7A C8A 1.376(11) . ? C8A C9A 1.410(11) . ? C8A H8AA 0.9500 . ? C9A H9AA 0.9500 . ? C10A H10A 0.9800 . ? C10A H10B 0.9800 . ? C10A H10C 0.9800 . ? C11A H11A 0.9800 . ? C11A H11B 0.9800 . ? C11A H11C 0.9800 . ? C12A H12A 0.9800 . ? C12A H12B 0.9800 . ? C12A H12C 0.9800 . ? Pt1B O1B 2.004(5) . ? Pt1B S3B 2.185(2) . ? Pt1B S1B 2.240(2) . ? Pt1B Cl1B 2.341(2) . ? Br1B C7B 1.895(8) . ? S1B C1B 1.690(9) . ? S2B C1B 1.754(9) . ? S2B C10B 1.801(8) . ? S3B O2B 1.476(6) . ? S3B C11B 1.758(8) . ? S3B C12B 1.765(8) . ? O1B C3B 1.280(9) . ? C1B C2B 1.419(11) . ? C2B C3B 1.388(11) . ? C2B H2BA 0.9500 . ? C3B C4B 1.501(11) . ? C4B C5B 1.374(11) . ? C4B C9B 1.404(11) . ? C5B C6B 1.383(11) . ? C5B H5BA 0.9500 . ? C6B C7B 1.374(11) . ? C6B H6BA 0.9500 . ? C7B C8B 1.378(11) . ? C8B C9B 1.399(11) . ? C8B H8BA 0.9500 . ? C9B H9BA 0.9500 . ? C10B H10D 0.9800 . ? C10B H10E 0.9800 . ? C10B H10F 0.9800 . ? C11B H11D 0.9800 . ? C11B H11E 0.9800 . ? C11B H11F 0.9800 . ? C12B H12D 0.9800 . ? C12B H12E 0.9800 . ? C12B H12F 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 O1A Pt1A S3A 175.49(17) . . ? O1A Pt1A S1A 96.11(17) . . ? S3A Pt1A S1A 88.32(8) . . ? O1A Pt1A Cl1A 84.21(17) . . ? S3A Pt1A Cl1A 91.33(9) . . ? S1A Pt1A Cl1A 177.94(9) . . ? C1A S1A Pt1A 108.6(3) . . ? C1A S2A C10A 105.3(4) . . ? O2A S3A C11A 107.9(4) . . ? O2A S3A C12A 108.5(4) . . ? C11A S3A C12A 101.8(5) . . ? O2A S3A Pt1A 117.0(3) . . ? C11A S3A Pt1A 111.6(3) . . ? C12A S3A Pt1A 108.9(3) . . ? C3A O1A Pt1A 130.9(6) . . ? C2A C1A S1A 128.7(7) . . ? C2A C1A S2A 112.1(7) . . ? S1A C1A S2A 119.1(5) . . ? C3A C2A C1A 128.0(8) . . ? C3A C2A H2AA 116.0 . . ? C1A C2A H2AA 116.0 . . ? O1A C3A C2A 127.1(8) . . ? O1A C3A C4A 115.5(8) . . ? C2A C3A C4A 117.4(8) . . ? C9A C4A C5A 119.2(8) . . ? C9A C4A C3A 118.1(8) . . ? C5A C4A C3A 122.7(8) . . ? C6A C5A C4A 119.3(9) . . ? C6A C5A H5AA 120.3 . . ? C4A C5A H5AA 120.3 . . ? C7A C6A C5A 121.1(9) . . ? C7A C6A H6AA 119.5 . . ? C5A C6A H6AA 119.5 . . ? C6A C7A C8A 121.6(9) . . ? C6A C7A Br1A 119.4(8) . . ? C8A C7A Br1A 119.0(8) . . ? C7A C8A C9A 118.6(9) . . ? C7A C8A H8AA 120.7 . . ? C9A C8A H8AA 120.7 . . ? C4A C9A C8A 120.2(9) . . ? C4A C9A H9AA 119.9 . . ? C8A C9A H9AA 119.9 . . ? S2A C10A H10A 109.5 . . ? S2A C10A H10B 109.5 . . ? H10A C10A H10B 109.5 . . ? S2A C10A H10C 109.5 . . ? H10A C10A H10C 109.5 . . ? H10B C10A H10C 109.5 . . ? S3A C11A H11A 109.5 . . ? S3A C11A H11B 109.5 . . ? H11A C11A H11B 109.5 . . ? S3A C11A H11C 109.5 . . ? H11A C11A H11C 109.5 . . ? H11B C11A H11C 109.5 . . ? S3A C12A H12A 109.5 . . ? S3A C12A H12B 109.5 . . ? H12A C12A H12B 109.5 . . ? S3A C12A H12C 109.5 . . ? H12A C12A H12C 109.5 . . ? H12B C12A H12C 109.5 . . ? O1B Pt1B S3B 174.97(17) . . ? O1B Pt1B S1B 96.10(17) . . ? S3B Pt1B S1B 88.76(9) . . ? O1B Pt1B Cl1B 85.96(17) . . ? S3B Pt1B Cl1B 89.13(9) . . ? S1B Pt1B Cl1B 176.74(9) . . ? C1B S1B Pt1B 108.5(3) . . ? C1B S2B C10B 105.3(4) . . ? O2B S3B C11B 107.4(4) . . ? O2B S3B C12B 109.7(4) . . ? C11B S3B C12B 101.3(4) . . ? O2B S3B Pt1B 117.1(3) . . ? C11B S3B Pt1B 109.3(3) . . ? C12B S3B Pt1B 110.7(3) . . ? C3B O1B Pt1B 131.2(6) . . ? C2B C1B S1B 129.7(7) . . ? C2B C1B S2B 113.6(7) . . ? S1B C1B S2B 116.7(5) . . ? C3B C2B C1B 127.1(9) . . ? C3B C2B H2BA 116.4 . . ? C1B C2B H2BA 116.4 . . ? O1B C3B C2B 127.0(9) . . ? O1B C3B C4B 114.3(8) . . ? C2B C3B C4B 118.7(9) . . ? C5B C4B C9B 118.0(9) . . ? C5B C4B C3B 124.5(9) . . ? C9B C4B C3B 117.3(9) . . ? C4B C5B C6B 122.0(9) . . ? C4B C5B H5BA 119.0 . . ? C6B C5B H5BA 119.0 . . ? C7B C6B C5B 118.9(9) . . ? C7B C6B H6BA 120.6 . . ? C5B C6B H6BA 120.6 . . ? C6B C7B C8B 121.8(8) . . ? C6B C7B Br1B 121.3(7) . . ? C8B C7B Br1B 116.8(7) . . ? C7B C8B C9B 118.4(9) . . ? C7B C8B H8BA 120.8 . . ? C9B C8B H8BA 120.8 . . ? C8B C9B C4B 120.9(9) . . ? C8B C9B H9BA 119.6 . . ? C4B C9B H9BA 119.6 . . ? S2B C10B H10D 109.5 . . ? S2B C10B H10E 109.5 . . ? H10D C10B H10E 109.5 . . ? S2B C10B H10F 109.5 . . ? H10D C10B H10F 109.5 . . ? H10E C10B H10F 109.5 . . ? S3B C11B H11D 109.5 . . ? S3B C11B H11E 109.5 . . ? H11D C11B H11E 109.5 . . ? S3B C11B H11F 109.5 . . ? H11D C11B H11F 109.5 . . ? H11E C11B H11F 109.5 . . ? S3B C12B H12D 109.5 . . ? S3B C12B H12E 109.5 . . ? H12D C12B H12E 109.5 . . ? S3B C12B H12F 109.5 . . ? H12D C12B H12F 109.5 . . ? H12E C12B H12F 109.5 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.190 _refine_diff_density_min -1.751 _refine_diff_density_rms 0.255 _database_code_depnum_ccdc_archive 'CCDC 915584' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_FO3919 _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C13 H17 Cl O2 Pt S3' _chemical_formula_sum 'C13 H17 Cl O2 Pt S3' _chemical_formula_weight 531.99 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' 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 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 7.2779(2) _cell_length_b 38.6448(11) _cell_length_c 11.8038(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.262(1) _cell_angle_gamma 90.00 _cell_volume 3319.82(16) _cell_formula_units_Z 8 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.09 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.129 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2032 _exptl_absorpt_coefficient_mu 8.988 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [SORTAV, R.H. Blessing, J. Applied Cryst. 1997, 30, 421-426] ; _exptl_absorpt_correction_T_min 0.2216 _exptl_absorpt_correction_T_max 0.4757 _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_reflns_number 25423 _diffrn_reflns_av_R_equivalents 0.1051 _diffrn_reflns_av_sigmaI/netI 0.0860 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -50 _diffrn_reflns_limit_k_max 49 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.80 _diffrn_reflns_theta_max 27.48 _reflns_number_total 7448 _reflns_number_gt 5405 _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^)+(0.0445P)^2^+1.9785P] 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 7448 _refine_ls_number_parameters 367 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0799 _refine_ls_R_factor_gt 0.0467 _refine_ls_wR_factor_ref 0.1034 _refine_ls_wR_factor_gt 0.0927 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.023 _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 Pt1A Pt 0.99470(4) 0.084084(7) 0.19041(3) 0.02228(10) Uani 1 1 d . . . Cl1A Cl 0.9910(3) 0.06855(5) -0.00292(16) 0.0303(4) Uani 1 1 d . . . S1A S 1.0028(3) 0.09764(5) 0.37568(17) 0.0244(4) Uani 1 1 d . . . S2A S 0.9966(3) 0.15868(5) 0.52553(18) 0.0360(5) Uani 1 1 d . . . S3A S 1.0023(2) 0.02944(5) 0.23813(16) 0.0239(4) Uani 1 1 d . . . O1A O 0.9829(7) 0.13299(14) 0.1339(5) 0.0290(12) Uani 1 1 d . . . O2A O 1.0046(7) 0.02039(14) 0.3592(4) 0.0340(13) Uani 1 1 d . . . C1A C 0.9922(10) 0.1407(2) 0.3885(6) 0.0264(18) Uani 1 1 d . . . C2A C 0.9748(11) 0.1660(2) 0.3083(7) 0.033(2) Uani 1 1 d . . . H2AA H 0.9646 0.1891 0.3354 0.039 Uiso 1 1 calc R . . C3A C 0.9704(10) 0.1617(2) 0.1884(7) 0.0271(18) Uani 1 1 d . . . C4A C 0.9370(10) 0.1927(2) 0.1177(7) 0.0293(18) Uani 1 1 d . . . C5A C 0.9644(12) 0.2259(2) 0.1570(8) 0.040(2) Uani 1 1 d . . . H5AA H 1.0192 0.2294 0.2293 0.048 Uiso 1 1 calc R . . C6A C 0.9134(13) 0.2542(2) 0.0929(8) 0.050(3) Uani 1 1 d . . . H6AA H 0.9291 0.2770 0.1219 0.060 Uiso 1 1 calc R . . C7A C 0.8386(12) 0.2492(3) -0.0150(9) 0.053(3) Uani 1 1 d . . . H7AA H 0.8031 0.2687 -0.0593 0.064 Uiso 1 1 calc R . . C8A C 0.8161(12) 0.2169(3) -0.0569(9) 0.053(3) Uani 1 1 d . . . H8AA H 0.7662 0.2137 -0.1307 0.064 Uiso 1 1 calc R . . C9A C 0.8666(11) 0.1878(2) 0.0087(8) 0.043(2) Uani 1 1 d . . . H9AA H 0.8529 0.1651 -0.0210 0.051 Uiso 1 1 calc R . . C10A C 0.9947(11) 0.1237(2) 0.6242(7) 0.0302(19) Uani 1 1 d . . . H10A H 0.8888 0.1083 0.6087 0.036 Uiso 1 1 calc R . . H10B H 1.1088 0.1100 0.6172 0.036 Uiso 1 1 calc R . . C11A C 0.9803(14) 0.1387(3) 0.7432(8) 0.057(3) Uani 1 1 d . . . H11A H 0.9734 0.1198 0.7984 0.085 Uiso 1 1 calc R . . H11B H 0.8695 0.1530 0.7484 0.085 Uiso 1 1 calc R . . H11C H 1.0888 0.1530 0.7592 0.085 Uiso 1 1 calc R . . C12A C 1.1910(11) 0.0084(2) 0.1735(7) 0.0324(19) Uani 1 1 d . . . H12A H 1.1758 -0.0167 0.1798 0.049 Uiso 1 1 calc R . . H12B H 1.3051 0.0154 0.2115 0.049 Uiso 1 1 calc R . . H12C H 1.1966 0.0149 0.0933 0.049 Uiso 1 1 calc R . . C13A C 0.8119(10) 0.0083(2) 0.1749(7) 0.0321(19) Uani 1 1 d . . . H13A H 0.8224 -0.0167 0.1870 0.048 Uiso 1 1 calc R . . H13B H 0.8099 0.0132 0.0934 0.048 Uiso 1 1 calc R . . H13C H 0.6981 0.0168 0.2093 0.048 Uiso 1 1 calc R . . Pt1B Pt 1.49377(4) 0.111289(8) 0.41596(2) 0.02165(9) Uani 1 1 d . . . Cl1B Cl 1.4935(3) 0.12786(5) 0.60685(16) 0.0294(4) Uani 1 1 d . . . S1B S 1.4990(3) 0.09470(5) 0.23296(16) 0.0257(4) Uani 1 1 d . . . S2B S 1.4734(3) 0.12368(6) 0.00274(17) 0.0348(5) Uani 1 1 d . . . S3B S 1.5012(2) 0.05652(5) 0.46602(16) 0.0221(4) Uani 1 1 d . . . O1B O 1.4787(7) 0.16231(13) 0.3828(4) 0.0277(12) Uani 1 1 d . . . O2B O 1.5019(7) 0.03075(13) 0.3737(4) 0.0280(12) Uani 1 1 d . . . C1B C 1.4746(9) 0.1298(2) 0.1490(6) 0.0255(18) Uani 1 1 d . . . C2B C 1.4582(10) 0.1645(2) 0.1800(6) 0.0290(18) Uani 1 1 d . . . H2BA H 1.4453 0.1806 0.1195 0.035 Uiso 1 1 calc R . . C3B C 1.4584(10) 0.1789(2) 0.2914(7) 0.0277(18) Uani 1 1 d . . . C4B C 1.4271(10) 0.2168(2) 0.3019(7) 0.0283(18) Uani 1 1 d . . . C5B C 1.4729(10) 0.2402(2) 0.2160(7) 0.0293(18) Uani 1 1 d . . . H5BA H 1.5281 0.2320 0.1483 0.035 Uiso 1 1 calc R . . C6B C 1.4386(12) 0.2748(2) 0.2291(7) 0.038(2) Uani 1 1 d . . . H6BA H 1.4715 0.2904 0.1706 0.046 Uiso 1 1 calc R . . C7B C 1.3569(11) 0.2872(2) 0.3262(8) 0.043(2) Uani 1 1 d . . . H7BA H 1.3315 0.3112 0.3336 0.051 Uiso 1 1 calc R . . C8B C 1.3114(11) 0.2643(2) 0.4141(8) 0.039(2) Uani 1 1 d . . . H8BA H 1.2563 0.2727 0.4815 0.047 Uiso 1 1 calc R . . C9B C 1.3479(10) 0.2291(2) 0.4014(7) 0.0322(19) Uani 1 1 d . . . H9BA H 1.3186 0.2135 0.4608 0.039 Uiso 1 1 calc R . . C10B C 1.4897(11) 0.0780(2) -0.0176(6) 0.0265(18) Uani 1 1 d . . . H10C H 1.6040 0.0690 0.0176 0.032 Uiso 1 1 calc R . . H10D H 1.3838 0.0662 0.0181 0.032 Uiso 1 1 calc R . . C11B C 1.4904(13) 0.0710(2) -0.1443(7) 0.045(2) Uani 1 1 d . . . H11D H 1.4885 0.0460 -0.1577 0.067 Uiso 1 1 calc R . . H11E H 1.6016 0.0809 -0.1778 0.067 Uiso 1 1 calc R . . H11F H 1.3817 0.0816 -0.1792 0.067 Uiso 1 1 calc R . . C12B C 1.6886(10) 0.04704(19) 0.5574(6) 0.0272(18) Uani 1 1 d . . . H12D H 1.6750 0.0235 0.5874 0.041 Uiso 1 1 calc R . . H12E H 1.6906 0.0636 0.6201 0.041 Uiso 1 1 calc R . . H12F H 1.8037 0.0487 0.5150 0.041 Uiso 1 1 calc R . . C13B C 1.3124(9) 0.0466(2) 0.5546(6) 0.0262(18) Uani 1 1 d . . . H13D H 1.3272 0.0232 0.5852 0.039 Uiso 1 1 calc R . . H13E H 1.1983 0.0478 0.5104 0.039 Uiso 1 1 calc R . . H13F H 1.3074 0.0632 0.6171 0.039 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 Pt1A 0.02704(16) 0.02088(16) 0.01893(18) -0.00124(12) 0.00133(12) 0.00021(12) Cl1A 0.0368(10) 0.0357(11) 0.0185(10) -0.0032(8) 0.0014(8) 0.0005(9) S1A 0.0337(10) 0.0194(9) 0.0202(11) -0.0008(8) -0.0023(8) 0.0028(8) S2A 0.0619(14) 0.0226(11) 0.0236(12) -0.0031(9) 0.0018(10) -0.0011(10) S3A 0.0301(9) 0.0207(10) 0.0208(11) -0.0046(8) 0.0013(8) 0.0009(8) O1A 0.031(3) 0.027(3) 0.029(3) 0.004(3) -0.003(2) -0.001(2) O2A 0.056(3) 0.025(3) 0.021(3) -0.001(2) -0.002(3) 0.001(3) C1A 0.031(4) 0.031(4) 0.017(4) -0.002(3) 0.006(3) 0.005(4) C2A 0.058(5) 0.015(4) 0.026(5) 0.002(4) 0.004(4) -0.004(4) C3A 0.029(4) 0.025(4) 0.027(5) 0.001(4) 0.005(3) -0.002(3) C4A 0.036(4) 0.027(5) 0.025(5) 0.008(4) 0.008(4) -0.002(4) C5A 0.053(5) 0.033(5) 0.034(5) 0.014(4) 0.009(4) -0.002(4) C6A 0.074(7) 0.029(5) 0.048(6) 0.013(5) 0.018(5) 0.015(5) C7A 0.040(5) 0.046(7) 0.073(8) 0.031(6) 0.013(5) 0.002(5) C8A 0.039(5) 0.072(8) 0.048(6) 0.027(6) -0.003(5) -0.010(5) C9A 0.043(5) 0.037(5) 0.049(6) 0.015(5) -0.002(4) -0.011(4) C10A 0.035(4) 0.034(5) 0.022(5) 0.002(4) 0.007(3) -0.004(4) C11A 0.085(7) 0.053(7) 0.033(6) 0.005(5) -0.008(5) -0.011(6) C12A 0.045(5) 0.025(5) 0.028(5) -0.007(4) -0.003(4) 0.007(4) C13A 0.032(4) 0.027(5) 0.037(5) -0.008(4) 0.001(4) -0.004(3) Pt1B 0.02802(16) 0.01934(16) 0.01761(17) 0.00223(12) 0.00174(12) 0.00031(12) Cl1B 0.0407(10) 0.0277(11) 0.0198(10) -0.0021(8) 0.0005(9) 0.0018(9) S1B 0.0355(10) 0.0245(10) 0.0172(10) 0.0017(8) 0.0035(8) -0.0003(9) S2B 0.0575(13) 0.0269(11) 0.0201(11) 0.0033(9) 0.0010(10) -0.0009(10) S3B 0.0280(9) 0.0203(9) 0.0182(10) 0.0017(8) 0.0008(8) 0.0002(8) O1B 0.042(3) 0.022(3) 0.019(3) 0.003(2) 0.000(2) 0.000(2) O2B 0.045(3) 0.020(3) 0.020(3) 0.001(2) 0.006(2) 0.000(2) C1B 0.022(4) 0.034(5) 0.020(4) 0.003(4) -0.004(3) 0.000(3) C2B 0.047(5) 0.023(4) 0.017(4) -0.002(3) -0.005(4) -0.002(4) C3B 0.029(4) 0.028(4) 0.027(5) -0.002(4) 0.001(4) 0.003(3) C4B 0.033(4) 0.022(4) 0.029(5) 0.005(4) -0.006(4) -0.002(3) C5B 0.037(4) 0.026(4) 0.024(5) 0.000(4) -0.004(4) -0.001(4) C6B 0.060(6) 0.027(5) 0.028(5) 0.006(4) -0.005(4) -0.002(4) C7B 0.045(5) 0.023(5) 0.061(7) -0.004(5) -0.007(5) 0.004(4) C8B 0.040(5) 0.038(5) 0.039(5) -0.009(4) -0.003(4) 0.004(4) C9B 0.036(4) 0.028(5) 0.033(5) 0.000(4) 0.000(4) -0.001(4) C10B 0.032(4) 0.031(4) 0.017(4) -0.003(3) -0.005(3) 0.002(3) C11B 0.071(6) 0.030(5) 0.033(5) -0.012(4) -0.003(5) -0.002(5) C12B 0.040(4) 0.023(4) 0.018(4) 0.009(3) -0.001(3) 0.000(3) C13B 0.029(4) 0.024(4) 0.025(4) 0.007(3) 0.007(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 Pt1A O1A 2.006(5) . ? Pt1A S3A 2.186(2) . ? Pt1A S1A 2.249(2) . ? Pt1A Cl1A 2.3597(19) . ? S1A C1A 1.674(8) . ? S2A C1A 1.760(8) . ? S2A C10A 1.784(8) . ? S3A O2A 1.472(6) . ? S3A C13A 1.770(7) . ? S3A C12A 1.772(8) . ? O1A C3A 1.285(9) . ? C1A C2A 1.366(10) . ? C2A C3A 1.426(11) . ? C2A H2AA 0.9500 . ? C3A C4A 1.481(10) . ? C4A C5A 1.378(12) . ? C4A C9A 1.396(11) . ? C5A C6A 1.380(11) . ? C5A H5AA 0.9500 . ? C6A C7A 1.396(13) . ? C6A H6AA 0.9500 . ? C7A C8A 1.355(14) . ? C7A H7AA 0.9500 . ? C8A C9A 1.411(12) . ? C8A H8AA 0.9500 . ? C9A H9AA 0.9500 . ? C10A C11A 1.523(12) . ? C10A H10A 0.9900 . ? C10A H10B 0.9900 . ? C11A H11A 0.9800 . ? C11A H11B 0.9800 . ? C11A H11C 0.9800 . ? C12A H12A 0.9800 . ? C12A H12B 0.9800 . ? C12A H12C 0.9800 . ? C13A H13A 0.9800 . ? C13A H13B 0.9800 . ? C13A H13C 0.9800 . ? Pt1B O1B 2.013(5) . ? Pt1B S3B 2.1981(19) . ? Pt1B S1B 2.254(2) . ? Pt1B Cl1B 2.3425(19) . ? S1B C1B 1.690(8) . ? S2B C1B 1.743(8) . ? S2B C10B 1.787(8) . ? S3B O2B 1.477(5) . ? S3B C13B 1.772(7) . ? S3B C12B 1.773(7) . ? O1B C3B 1.263(9) . ? C1B C2B 1.395(11) . ? C2B C3B 1.427(10) . ? C2B H2BA 0.9500 . ? C3B C4B 1.487(11) . ? C4B C9B 1.396(11) . ? C4B C5B 1.400(10) . ? C5B C6B 1.369(11) . ? C5B H5BA 0.9500 . ? C6B C7B 1.380(12) . ? C6B H6BA 0.9500 . ? C7B C8B 1.404(12) . ? C7B H7BA 0.9500 . ? C8B C9B 1.393(11) . ? C8B H8BA 0.9500 . ? C9B H9BA 0.9500 . ? C10B C11B 1.521(11) . ? C10B H10C 0.9900 . ? C10B H10D 0.9900 . ? C11B H11D 0.9800 . ? C11B H11E 0.9800 . ? C11B H11F 0.9800 . ? C12B H12D 0.9800 . ? C12B H12E 0.9800 . ? C12B H12F 0.9800 . ? C13B H13D 0.9800 . ? C13B H13E 0.9800 . ? C13B H13F 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 O1A Pt1A S3A 175.39(16) . . ? O1A Pt1A S1A 96.02(16) . . ? S3A Pt1A S1A 88.50(7) . . ? O1A Pt1A Cl1A 85.28(16) . . ? S3A Pt1A Cl1A 90.20(7) . . ? S1A Pt1A Cl1A 178.47(7) . . ? C1A S1A Pt1A 108.6(3) . . ? C1A S2A C10A 107.6(4) . . ? O2A S3A C13A 107.8(4) . . ? O2A S3A C12A 107.7(4) . . ? C13A S3A C12A 102.3(4) . . ? O2A S3A Pt1A 118.7(2) . . ? C13A S3A Pt1A 108.5(3) . . ? C12A S3A Pt1A 110.5(3) . . ? C3A O1A Pt1A 130.5(5) . . ? C2A C1A S1A 130.8(6) . . ? C2A C1A S2A 110.9(6) . . ? S1A C1A S2A 118.3(5) . . ? C1A C2A C3A 127.3(8) . . ? C1A C2A H2AA 116.4 . . ? C3A C2A H2AA 116.4 . . ? O1A C3A C2A 126.7(7) . . ? O1A C3A C4A 115.4(7) . . ? C2A C3A C4A 117.8(7) . . ? C5A C4A C9A 119.2(8) . . ? C5A C4A C3A 122.9(7) . . ? C9A C4A C3A 117.8(7) . . ? C4A C5A C6A 121.0(9) . . ? C4A C5A H5AA 119.5 . . ? C6A C5A H5AA 119.5 . . ? C5A C6A C7A 119.5(9) . . ? C5A C6A H6AA 120.2 . . ? C7A C6A H6AA 120.2 . . ? C8A C7A C6A 120.5(9) . . ? C8A C7A H7AA 119.8 . . ? C6A C7A H7AA 119.8 . . ? C7A C8A C9A 120.2(9) . . ? C7A C8A H8AA 119.9 . . ? C9A C8A H8AA 119.9 . . ? C4A C9A C8A 119.4(9) . . ? C4A C9A H9AA 120.3 . . ? C8A C9A H9AA 120.3 . . ? C11A C10A S2A 108.3(6) . . ? C11A C10A H10A 110.0 . . ? S2A C10A H10A 110.0 . . ? C11A C10A H10B 110.0 . . ? S2A C10A H10B 110.0 . . ? H10A C10A H10B 108.4 . . ? C10A C11A H11A 109.5 . . ? C10A C11A H11B 109.5 . . ? H11A C11A H11B 109.5 . . ? C10A C11A H11C 109.5 . . ? H11A C11A H11C 109.5 . . ? H11B C11A H11C 109.5 . . ? S3A C12A H12A 109.5 . . ? S3A C12A H12B 109.5 . . ? H12A C12A H12B 109.5 . . ? S3A C12A H12C 109.5 . . ? H12A C12A H12C 109.5 . . ? H12B C12A H12C 109.5 . . ? S3A C13A H13A 109.5 . . ? S3A C13A H13B 109.5 . . ? H13A C13A H13B 109.5 . . ? S3A C13A H13C 109.5 . . ? H13A C13A H13C 109.5 . . ? H13B C13A H13C 109.5 . . ? O1B Pt1B S3B 175.31(16) . . ? O1B Pt1B S1B 95.35(16) . . ? S3B Pt1B S1B 89.04(7) . . ? O1B Pt1B Cl1B 85.35(16) . . ? S3B Pt1B Cl1B 90.28(7) . . ? S1B Pt1B Cl1B 178.87(7) . . ? C1B S1B Pt1B 109.3(3) . . ? C1B S2B C10B 105.5(4) . . ? O2B S3B C13B 107.1(3) . . ? O2B S3B C12B 107.7(3) . . ? C13B S3B C12B 101.1(4) . . ? O2B S3B Pt1B 116.8(2) . . ? C13B S3B Pt1B 110.4(3) . . ? C12B S3B Pt1B 112.4(3) . . ? C3B O1B Pt1B 132.0(5) . . ? C2B C1B S1B 128.9(6) . . ? C2B C1B S2B 113.0(6) . . ? S1B C1B S2B 118.1(5) . . ? C1B C2B C3B 128.0(7) . . ? C1B C2B H2BA 116.0 . . ? C3B C2B H2BA 116.0 . . ? O1B C3B C2B 126.1(7) . . ? O1B C3B C4B 116.5(7) . . ? C2B C3B C4B 117.4(7) . . ? C9B C4B C5B 119.3(8) . . ? C9B C4B C3B 118.1(7) . . ? C5B C4B C3B 122.6(8) . . ? C6B C5B C4B 120.3(8) . . ? C6B C5B H5BA 119.8 . . ? C4B C5B H5BA 119.8 . . ? C5B C6B C7B 120.9(8) . . ? C5B C6B H6BA 119.5 . . ? C7B C6B H6BA 119.5 . . ? C6B C7B C8B 119.9(8) . . ? C6B C7B H7BA 120.1 . . ? C8B C7B H7BA 120.1 . . ? C9B C8B C7B 119.4(8) . . ? C9B C8B H8BA 120.3 . . ? C7B C8B H8BA 120.3 . . ? C8B C9B C4B 120.2(8) . . ? C8B C9B H9BA 119.9 . . ? C4B C9B H9BA 119.9 . . ? C11B C10B S2B 107.9(6) . . ? C11B C10B H10C 110.1 . . ? S2B C10B H10C 110.1 . . ? C11B C10B H10D 110.1 . . ? S2B C10B H10D 110.1 . . ? H10C C10B H10D 108.4 . . ? C10B C11B H11D 109.5 . . ? C10B C11B H11E 109.5 . . ? H11D C11B H11E 109.5 . . ? C10B C11B H11F 109.5 . . ? H11D C11B H11F 109.5 . . ? H11E C11B H11F 109.5 . . ? S3B C12B H12D 109.5 . . ? S3B C12B H12E 109.5 . . ? H12D C12B H12E 109.5 . . ? S3B C12B H12F 109.5 . . ? H12D C12B H12F 109.5 . . ? H12E C12B H12F 109.5 . . ? S3B C13B H13D 109.5 . . ? S3B C13B H13E 109.5 . . ? H13D C13B H13E 109.5 . . ? S3B C13B H13F 109.5 . . ? H13D C13B H13F 109.5 . . ? H13E C13B H13F 109.5 . . ? _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.978 _refine_diff_density_max 2.206 _refine_diff_density_min -2.008 _refine_diff_density_rms 0.278 _database_code_depnum_ccdc_archive 'CCDC 915585' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_FO3796 _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H18 O2 Pt S4' _chemical_formula_sum 'C20 H18 O2 Pt S4' _chemical_formula_weight 613.67 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' 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 9.2471(4) _cell_length_b 22.4832(9) _cell_length_c 10.1091(5) _cell_angle_alpha 90.00 _cell_angle_beta 103.774(3) _cell_angle_gamma 90.00 _cell_volume 2041.29(16) _cell_formula_units_Z 4 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.997 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1184 _exptl_absorpt_coefficient_mu 7.296 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [SORTAV, R.H. Blessing, J. Applied Cryst. 1997, 30, 421-426] ; _exptl_absorpt_correction_T_min 0.2637 _exptl_absorpt_correction_T_max 0.3365 _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_reflns_number 19736 _diffrn_reflns_av_R_equivalents 0.0772 _diffrn_reflns_av_sigmaI/netI 0.0741 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.81 _diffrn_reflns_theta_max 27.54 _reflns_number_total 4669 _reflns_number_gt 3261 _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^)+(0.0338P)^2^+2.6544P] 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 4669 _refine_ls_number_parameters 246 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0846 _refine_ls_R_factor_gt 0.0435 _refine_ls_wR_factor_ref 0.0929 _refine_ls_wR_factor_gt 0.0828 _refine_ls_goodness_of_fit_ref 1.117 _refine_ls_restrained_S_all 1.117 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.32358(3) 0.012528(13) 0.39088(3) 0.02945(10) Uani 1 1 d . . . S1 S 0.4211(2) 0.09855(8) 0.34361(17) 0.0337(4) Uani 1 1 d . . . S2 S 0.4913(2) 0.21854(9) 0.45944(19) 0.0363(4) Uani 1 1 d . . . S3 S 0.3682(2) -0.02396(8) 0.19909(17) 0.0334(4) Uani 1 1 d . . . S4 S 0.2968(2) -0.12838(9) 0.01976(19) 0.0396(5) Uani 1 1 d . . . O1 O 0.2700(5) 0.0404(2) 0.5629(5) 0.0329(11) Uani 1 1 d . . . O2 O 0.2298(5) -0.0616(2) 0.4433(4) 0.0330(12) Uani 1 1 d . . . C1 C 0.2859(8) 0.1319(3) 0.8562(6) 0.0307(16) Uani 1 1 d . . . H1A H 0.3591 0.1605 0.8489 0.037 Uiso 1 1 calc R . . C2 C 0.2301(8) 0.1307(4) 0.9717(7) 0.0383(18) Uani 1 1 d . . . H2A H 0.2637 0.1590 1.0420 0.046 Uiso 1 1 calc R . . C3 C 0.1259(8) 0.0887(4) 0.9851(7) 0.0374(18) Uani 1 1 d . . . H3A H 0.0899 0.0871 1.0656 0.045 Uiso 1 1 calc R . . C4 C 0.0750(8) 0.0495(4) 0.8817(7) 0.0401(19) Uani 1 1 d . . . H4A H 0.0011 0.0213 0.8895 0.048 Uiso 1 1 calc R . . C5 C 0.1288(7) 0.0502(3) 0.7671(7) 0.0310(16) Uani 1 1 d . . . H5A H 0.0927 0.0221 0.6969 0.037 Uiso 1 1 calc R . . C6 C 0.2363(7) 0.0918(3) 0.7515(6) 0.0282(15) Uani 1 1 d . . . C7 C 0.2936(7) 0.0899(3) 0.6258(6) 0.0267(15) Uani 1 1 d . . . C8 C 0.3651(8) 0.1392(3) 0.5865(7) 0.0310(16) Uani 1 1 d . . . H8A H 0.3778 0.1721 0.6474 0.037 Uiso 1 1 calc R . . C9 C 0.4199(7) 0.1473(3) 0.4720(6) 0.0289(16) Uani 1 1 d . . . C10 C 0.5630(9) 0.2172(4) 0.3095(7) 0.0393(19) Uani 1 1 d . . . H10A H 0.6051 0.2562 0.2968 0.059 Uiso 1 1 calc R . . H10B H 0.4822 0.2078 0.2300 0.059 Uiso 1 1 calc R . . H10C H 0.6407 0.1867 0.3196 0.059 Uiso 1 1 calc R . . C11 C 0.0573(8) -0.1297(3) 0.5580(7) 0.0326(17) Uani 1 1 d . . . H11A H 0.0707 -0.0888 0.5814 0.039 Uiso 1 1 calc R . . C12 C -0.0217(8) -0.1660(4) 0.6274(7) 0.0407(19) Uani 1 1 d . . . H12A H -0.0629 -0.1497 0.6970 0.049 Uiso 1 1 calc R . . C13 C -0.0404(8) -0.2254(4) 0.5958(8) 0.043(2) Uani 1 1 d . . . H13A H -0.0937 -0.2503 0.6435 0.051 Uiso 1 1 calc R . . C14 C 0.0196(8) -0.2483(4) 0.4932(7) 0.043(2) Uani 1 1 d . . . H14A H 0.0058 -0.2891 0.4694 0.052 Uiso 1 1 calc R . . C15 C 0.0993(8) -0.2125(3) 0.4252(7) 0.0351(17) Uani 1 1 d . . . H15A H 0.1426 -0.2290 0.3572 0.042 Uiso 1 1 calc R . . C16 C 0.1163(7) -0.1524(3) 0.4559(6) 0.0279(15) Uani 1 1 d . . . C17 C 0.1987(7) -0.1113(3) 0.3838(7) 0.0278(15) Uani 1 1 d . . . C18 C 0.2237(7) -0.1264(3) 0.2563(7) 0.0292(15) Uani 1 1 d . . . H18A H 0.1877 -0.1643 0.2217 0.035 Uiso 1 1 calc R . . C19 C 0.2939(7) -0.0932(3) 0.1746(7) 0.0297(16) Uani 1 1 d . . . C20 C 0.3750(9) -0.0750(4) -0.0757(7) 0.043(2) Uani 1 1 d . . . H20A H 0.3782 -0.0920 -0.1643 0.064 Uiso 1 1 calc R . . H20B H 0.4762 -0.0648 -0.0253 0.064 Uiso 1 1 calc R . . H20C H 0.3134 -0.0391 -0.0897 0.064 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 Pt1 0.03547(16) 0.02758(17) 0.02739(14) -0.00055(13) 0.01161(11) -0.00276(14) S1 0.0443(11) 0.0306(11) 0.0300(9) -0.0012(8) 0.0164(8) -0.0061(8) S2 0.0465(11) 0.0298(11) 0.0352(9) 0.0006(8) 0.0149(9) -0.0038(9) S3 0.0411(10) 0.0333(12) 0.0296(9) -0.0007(7) 0.0161(8) -0.0032(8) S4 0.0487(12) 0.0394(13) 0.0366(10) -0.0070(8) 0.0217(9) -0.0046(9) O1 0.034(3) 0.032(3) 0.035(3) 0.003(2) 0.013(2) -0.005(2) O2 0.035(3) 0.039(3) 0.027(2) -0.002(2) 0.012(2) -0.005(2) C1 0.033(4) 0.034(5) 0.024(3) -0.001(3) 0.004(3) -0.002(3) C2 0.038(4) 0.042(5) 0.032(4) -0.004(3) 0.003(3) 0.008(4) C3 0.043(5) 0.045(5) 0.024(4) 0.007(3) 0.007(3) 0.015(4) C4 0.041(4) 0.047(6) 0.034(4) 0.009(4) 0.012(4) 0.002(4) C5 0.028(4) 0.037(5) 0.026(3) 0.004(3) 0.004(3) 0.002(3) C6 0.029(4) 0.033(4) 0.022(3) 0.006(3) 0.007(3) 0.002(3) C7 0.023(3) 0.027(4) 0.029(3) 0.001(3) 0.006(3) 0.001(3) C8 0.035(4) 0.027(4) 0.030(4) -0.003(3) 0.006(3) 0.003(3) C9 0.032(4) 0.029(4) 0.025(3) 0.000(3) 0.004(3) 0.001(3) C10 0.051(5) 0.036(5) 0.032(4) 0.002(3) 0.011(4) -0.012(4) C11 0.033(4) 0.037(5) 0.028(4) 0.004(3) 0.007(3) 0.003(3) C12 0.040(4) 0.049(6) 0.036(4) 0.007(4) 0.014(4) 0.004(4) C13 0.032(4) 0.048(6) 0.047(5) 0.016(4) 0.006(4) -0.006(4) C14 0.046(5) 0.044(6) 0.041(4) 0.003(4) 0.015(4) -0.005(4) C15 0.033(4) 0.036(5) 0.037(4) -0.003(3) 0.010(3) -0.001(3) C16 0.025(4) 0.034(5) 0.025(3) 0.005(3) 0.005(3) -0.001(3) C17 0.023(3) 0.025(4) 0.036(4) 0.000(3) 0.009(3) 0.004(3) C18 0.035(4) 0.021(4) 0.031(3) -0.001(3) 0.006(3) -0.001(3) C19 0.030(4) 0.028(4) 0.030(4) -0.004(3) 0.004(3) 0.005(3) C20 0.058(5) 0.041(5) 0.035(4) -0.002(3) 0.025(4) 0.004(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 Pt1 O2 2.007(5) . ? Pt1 O1 2.018(4) . ? Pt1 S3 2.2323(17) . ? Pt1 S1 2.2333(18) . ? S1 C9 1.701(7) . ? S2 C9 1.749(7) . ? S2 C10 1.794(7) . ? S3 C19 1.696(7) . ? S4 C19 1.759(7) . ? S4 C20 1.796(7) . ? O1 C7 1.273(8) . ? O2 C17 1.270(8) . ? C1 C6 1.382(9) . ? C1 C2 1.384(9) . ? C1 H1A 0.9500 . ? C2 C3 1.380(11) . ? C2 H2A 0.9500 . ? C3 C4 1.362(10) . ? C3 H3A 0.9500 . ? C4 C5 1.365(9) . ? C4 H4A 0.9500 . ? C5 C6 1.401(9) . ? C5 H5A 0.9500 . ? C6 C7 1.490(9) . ? C7 C8 1.397(9) . ? C8 C9 1.382(9) . ? C8 H8A 0.9500 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C16 1.375(9) . ? C11 C12 1.392(10) . ? C11 H11A 0.9500 . ? C12 C13 1.373(11) . ? C12 H12A 0.9500 . ? C13 C14 1.388(10) . ? C13 H13A 0.9500 . ? C14 C15 1.380(10) . ? C14 H14A 0.9500 . ? C15 C16 1.386(10) . ? C15 H15A 0.9500 . ? C16 C17 1.494(9) . ? C17 C18 1.404(9) . ? C18 C19 1.384(9) . ? C18 H18A 0.9500 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 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 O2 Pt1 O1 79.65(19) . . ? O2 Pt1 S3 96.03(13) . . ? O1 Pt1 S3 175.29(14) . . ? O2 Pt1 S1 175.85(13) . . ? O1 Pt1 S1 96.31(15) . . ? S3 Pt1 S1 87.98(6) . . ? C9 S1 Pt1 108.6(2) . . ? C9 S2 C10 105.5(3) . . ? C19 S3 Pt1 108.2(2) . . ? C19 S4 C20 105.7(3) . . ? C7 O1 Pt1 130.8(4) . . ? C17 O2 Pt1 132.0(4) . . ? C6 C1 C2 120.7(7) . . ? C6 C1 H1A 119.6 . . ? C2 C1 H1A 119.6 . . ? C3 C2 C1 120.3(7) . . ? C3 C2 H2A 119.8 . . ? C1 C2 H2A 119.8 . . ? C4 C3 C2 119.3(7) . . ? C4 C3 H3A 120.3 . . ? C2 C3 H3A 120.3 . . ? C3 C4 C5 121.0(7) . . ? C3 C4 H4A 119.5 . . ? C5 C4 H4A 119.5 . . ? C4 C5 C6 121.0(7) . . ? C4 C5 H5A 119.5 . . ? C6 C5 H5A 119.5 . . ? C1 C6 C5 117.6(6) . . ? C1 C6 C7 123.5(6) . . ? C5 C6 C7 118.8(6) . . ? O1 C7 C8 126.1(6) . . ? O1 C7 C6 113.5(6) . . ? C8 C7 C6 120.5(6) . . ? C9 C8 C7 129.4(7) . . ? C9 C8 H8A 115.3 . . ? C7 C8 H8A 115.3 . . ? C8 C9 S1 128.7(6) . . ? C8 C9 S2 113.6(5) . . ? S1 C9 S2 117.6(4) . . ? S2 C10 H10A 109.5 . . ? S2 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? S2 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C16 C11 C12 120.7(7) . . ? C16 C11 H11A 119.7 . . ? C12 C11 H11A 119.7 . . ? C13 C12 C11 120.3(7) . . ? C13 C12 H12A 119.8 . . ? C11 C12 H12A 119.8 . . ? C12 C13 C14 119.0(7) . . ? C12 C13 H13A 120.5 . . ? C14 C13 H13A 120.5 . . ? C15 C14 C13 120.8(8) . . ? C15 C14 H14A 119.6 . . ? C13 C14 H14A 119.6 . . ? C14 C15 C16 120.1(7) . . ? C14 C15 H15A 119.9 . . ? C16 C15 H15A 119.9 . . ? C11 C16 C15 119.1(6) . . ? C11 C16 C17 118.4(7) . . ? C15 C16 C17 122.5(6) . . ? O2 C17 C18 125.4(6) . . ? O2 C17 C16 113.4(6) . . ? C18 C17 C16 120.9(6) . . ? C19 C18 C17 128.4(7) . . ? C19 C18 H18A 115.8 . . ? C17 C18 H18A 115.8 . . ? C18 C19 S3 129.7(5) . . ? C18 C19 S4 113.4(5) . . ? S3 C19 S4 116.8(4) . . ? S4 C20 H20A 109.5 . . ? S4 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? S4 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.54 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.677 _refine_diff_density_min -1.818 _refine_diff_density_rms 0.245 _database_code_depnum_ccdc_archive 'CCDC 915586' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_FO3918 _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H38 O2 Pt S4' _chemical_formula_sum 'C30 H38 O2 Pt S4' _chemical_formula_weight 753.93 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' 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 21 21 21' _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' _cell_length_a 5.6712(1) _cell_length_b 15.4429(3) _cell_length_c 34.9571(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3061.53(10) _cell_formula_units_Z 4 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.636 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1504 _exptl_absorpt_coefficient_mu 4.881 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [SORTAV, R.H. Blessing, J. Applied Cryst. 1997, 30, 421-426] ; _exptl_absorpt_correction_T_min 0.3258 _exptl_absorpt_correction_T_max 0.5948 _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_reflns_number 25247 _diffrn_reflns_av_R_equivalents 0.0714 _diffrn_reflns_av_sigmaI/netI 0.0635 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -43 _diffrn_reflns_limit_l_max 39 _diffrn_reflns_theta_min 2.33 _diffrn_reflns_theta_max 27.48 _reflns_number_total 6855 _reflns_number_gt 6015 _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^)+(0.0200P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.378(5) _refine_ls_number_reflns 6855 _refine_ls_number_parameters 337 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0461 _refine_ls_R_factor_gt 0.0343 _refine_ls_wR_factor_ref 0.0539 _refine_ls_wR_factor_gt 0.0516 _refine_ls_goodness_of_fit_ref 1.005 _refine_ls_restrained_S_all 1.005 _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 Pt1 Pt -0.21805(3) 0.101300(10) 0.181398(5) 0.02236(5) Uani 1 1 d . . . S1 S -0.4287(2) 0.14576(8) 0.23138(3) 0.0251(3) Uani 1 1 d . . . S2 S -0.8371(2) 0.25628(8) 0.24921(3) 0.0279(3) Uani 1 1 d . . . S3 S -0.0169(2) 0.02106(8) 0.22323(3) 0.0271(3) Uani 1 1 d . . . S4 S 0.37613(19) -0.10557(8) 0.22442(3) 0.0310(3) Uani 1 1 d . . . O1 O -0.3964(5) 0.1695(2) 0.14113(9) 0.0299(8) Uani 1 1 d . . . O2 O -0.0306(6) 0.06769(19) 0.13480(9) 0.0286(8) Uani 1 1 d . . . C1 C -0.5807(8) 0.2165(3) 0.14463(14) 0.0240(11) Uani 1 1 d . . . C2 C -0.7002(8) 0.2362(3) 0.17820(12) 0.0271(10) Uani 1 1 d . . . H2A H -0.8353 0.2720 0.1753 0.033 Uiso 1 1 calc R . . C3 C -0.6494(7) 0.2108(3) 0.21520(13) 0.0225(10) Uani 1 1 d . . . C4 C -0.7501(9) 0.2141(3) 0.29492(12) 0.0326(11) Uani 1 1 d . . . H4A H -0.7827 0.1512 0.2961 0.039 Uiso 1 1 calc R . . H4B H -0.5789 0.2230 0.2988 0.039 Uiso 1 1 calc R . . C5 C -0.8877(9) 0.2608(3) 0.32582(13) 0.0368(13) Uani 1 1 d . . . H5A H -0.8611 0.3239 0.3233 0.044 Uiso 1 1 calc R . . H5B H -1.0581 0.2498 0.3220 0.044 Uiso 1 1 calc R . . C6 C -0.8196(10) 0.2328(3) 0.36580(13) 0.0428(14) Uani 1 1 d . . . H6A H -0.8399 0.1694 0.3680 0.051 Uiso 1 1 calc R . . H6B H -0.6508 0.2461 0.3700 0.051 Uiso 1 1 calc R . . C7 C -0.9628(9) 0.2763(3) 0.39649(14) 0.0402(14) Uani 1 1 d . . . H7A H -1.1316 0.2636 0.3920 0.048 Uiso 1 1 calc R . . H7B H -0.9415 0.3398 0.3943 0.048 Uiso 1 1 calc R . . C8 C -0.8995(10) 0.2490(3) 0.43685(14) 0.0436(14) Uani 1 1 d . . . H8A H -0.7346 0.2661 0.4422 0.052 Uiso 1 1 calc R . . H8B H -0.9089 0.1851 0.4387 0.052 Uiso 1 1 calc R . . C9 C -1.0595(10) 0.2887(4) 0.46693(15) 0.0589(17) Uani 1 1 d . . . H9A H -1.0072 0.2706 0.4924 0.088 Uiso 1 1 calc R . . H9B H -1.2219 0.2692 0.4627 0.088 Uiso 1 1 calc R . . H9C H -1.0528 0.3520 0.4651 0.088 Uiso 1 1 calc R . . C10 C -0.6634(8) 0.2546(3) 0.10773(13) 0.0246(11) Uani 1 1 d . . . C11 C -0.5195(9) 0.2466(3) 0.07571(14) 0.0341(13) Uani 1 1 d . . . H11A H -0.3760 0.2152 0.0776 0.041 Uiso 1 1 calc R . . C12 C -0.5815(10) 0.2834(3) 0.04141(16) 0.0449(14) Uani 1 1 d . . . H12A H -0.4794 0.2775 0.0200 0.054 Uiso 1 1 calc R . . C13 C -0.7906(9) 0.3288(3) 0.03752(13) 0.0362(12) Uani 1 1 d . . . H13A H -0.8322 0.3548 0.0138 0.043 Uiso 1 1 calc R . . C14 C -0.9358(9) 0.3354(4) 0.06861(16) 0.0469(15) Uani 1 1 d . . . H14A H -1.0807 0.3659 0.0664 0.056 Uiso 1 1 calc R . . C15 C -0.8737(9) 0.2980(4) 0.10356(15) 0.0432(14) Uani 1 1 d . . . H15A H -0.9780 0.3026 0.1247 0.052 Uiso 1 1 calc R . . C16 C 0.1519(8) 0.0195(3) 0.13130(13) 0.0260(11) Uani 1 1 d . . . C17 C 0.2553(9) -0.0277(2) 0.16081(12) 0.0251(10) Uani 1 1 d . . . H17A H 0.3862 -0.0623 0.1534 0.030 Uiso 1 1 calc R . . C18 C 0.1974(8) -0.0324(3) 0.19935(13) 0.0256(11) Uani 1 1 d . . . C19 C 0.2913(7) -0.1011(3) 0.27416(11) 0.0276(9) Uani 1 1 d . . . H19A H 0.1280 -0.0788 0.2759 0.033 Uiso 1 1 calc R . . H19B H 0.2923 -0.1606 0.2847 0.033 Uiso 1 1 calc R . . C20 C 0.4515(9) -0.0443(3) 0.29845(13) 0.0290(12) Uani 1 1 d . . . H20A H 0.4495 0.0155 0.2882 0.035 Uiso 1 1 calc R . . H20B H 0.6153 -0.0662 0.2967 0.035 Uiso 1 1 calc R . . C21 C 0.3754(9) -0.0427(3) 0.34047(13) 0.0284(12) Uani 1 1 d . . . H21A H 0.2144 -0.0183 0.3423 0.034 Uiso 1 1 calc R . . H21B H 0.3704 -0.1028 0.3504 0.034 Uiso 1 1 calc R . . C22 C 0.5424(9) 0.0109(3) 0.36511(13) 0.0341(12) Uani 1 1 d . . . H22A H 0.5463 0.0710 0.3552 0.041 Uiso 1 1 calc R . . H22B H 0.7036 -0.0133 0.3630 0.041 Uiso 1 1 calc R . . C23 C 0.4703(10) 0.0125(3) 0.40715(14) 0.0397(13) Uani 1 1 d . . . H23A H 0.3068 0.0344 0.4092 0.048 Uiso 1 1 calc R . . H23B H 0.4730 -0.0473 0.4173 0.048 Uiso 1 1 calc R . . C24 C 0.6313(11) 0.0688(4) 0.43109(16) 0.0555(17) Uani 1 1 d . . . H24A H 0.5778 0.0682 0.4577 0.083 Uiso 1 1 calc R . . H24B H 0.6276 0.1283 0.4213 0.083 Uiso 1 1 calc R . . H24C H 0.7928 0.0464 0.4297 0.083 Uiso 1 1 calc R . . C25 C 0.2448(8) 0.0130(3) 0.09136(12) 0.0259(10) Uani 1 1 d . . . C26 C 0.4528(10) -0.0256(4) 0.08206(16) 0.0434(15) Uani 1 1 d . . . H26A H 0.5497 -0.0481 0.1019 0.052 Uiso 1 1 calc R . . C27 C 0.5275(9) -0.0328(4) 0.04403(17) 0.0478(15) Uani 1 1 d . . . H27A H 0.6732 -0.0602 0.0382 0.057 Uiso 1 1 calc R . . C28 C 0.3895(10) -0.0004(3) 0.01533(16) 0.0400(14) Uani 1 1 d . . . H28A H 0.4375 -0.0062 -0.0106 0.048 Uiso 1 1 calc R . . C29 C 0.1831(11) 0.0403(3) 0.02399(14) 0.0461(14) Uani 1 1 d . . . H29A H 0.0891 0.0641 0.0041 0.055 Uiso 1 1 calc R . . C30 C 0.1088(9) 0.0472(3) 0.06208(15) 0.0384(13) Uani 1 1 d . . . H30A H -0.0357 0.0754 0.0679 0.046 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 Pt1 0.01992(8) 0.02283(8) 0.02435(9) 0.00171(8) -0.00080(8) 0.00214(7) S1 0.0245(6) 0.0257(6) 0.0250(7) 0.0035(5) -0.0003(5) 0.0047(5) S2 0.0255(7) 0.0291(6) 0.0292(7) -0.0022(5) -0.0015(5) 0.0061(5) S3 0.0269(7) 0.0283(7) 0.0262(7) 0.0026(5) 0.0000(5) 0.0074(5) S4 0.0309(6) 0.0311(7) 0.0309(7) 0.0004(6) -0.0044(5) 0.0098(6) O1 0.0284(18) 0.036(2) 0.0257(19) 0.0071(15) -0.0011(15) 0.0068(15) O2 0.0300(18) 0.0329(19) 0.0229(18) 0.0026(14) 0.0019(15) 0.0080(15) C1 0.018(2) 0.021(3) 0.034(3) -0.002(2) -0.005(2) -0.003(2) C2 0.026(2) 0.024(2) 0.031(3) 0.003(2) -0.011(3) 0.0001(19) C3 0.014(2) 0.018(2) 0.036(3) 0.000(2) 0.002(2) -0.0026(18) C4 0.036(3) 0.034(3) 0.028(3) 0.004(2) 0.004(2) 0.001(3) C5 0.033(3) 0.050(3) 0.027(3) 0.004(2) 0.001(2) 0.016(2) C6 0.046(3) 0.046(3) 0.036(3) -0.004(2) 0.000(3) 0.013(3) C7 0.040(3) 0.047(4) 0.033(3) -0.001(3) 0.002(3) 0.011(3) C8 0.053(4) 0.045(3) 0.034(3) 0.000(3) -0.002(3) 0.008(3) C9 0.055(4) 0.087(5) 0.035(4) -0.008(3) 0.010(3) 0.012(3) C10 0.024(3) 0.022(2) 0.027(3) -0.002(2) -0.005(2) -0.005(2) C11 0.035(3) 0.034(3) 0.034(3) 0.003(2) -0.002(3) 0.011(2) C12 0.061(4) 0.044(4) 0.030(3) 0.001(3) -0.003(3) 0.016(3) C13 0.048(3) 0.033(3) 0.028(3) 0.007(2) -0.011(3) -0.003(3) C14 0.036(3) 0.061(4) 0.044(4) 0.016(3) -0.010(3) 0.008(3) C15 0.026(3) 0.065(4) 0.039(3) 0.009(3) -0.001(2) 0.010(3) C16 0.022(3) 0.020(2) 0.035(3) -0.005(2) 0.000(2) -0.005(2) C17 0.018(3) 0.028(2) 0.029(3) 0.0003(18) 0.000(2) 0.002(2) C18 0.023(3) 0.020(2) 0.034(3) -0.0007(18) -0.009(2) -0.003(2) C19 0.030(2) 0.023(2) 0.030(2) 0.006(2) -0.007(2) 0.004(3) C20 0.027(3) 0.024(3) 0.037(3) 0.000(2) -0.004(2) 0.000(2) C21 0.030(3) 0.025(3) 0.029(3) 0.004(2) 0.000(2) 0.001(2) C22 0.043(3) 0.025(3) 0.035(3) 0.002(2) -0.008(2) 0.002(2) C23 0.048(3) 0.040(3) 0.032(3) -0.003(2) 0.001(3) 0.000(3) C24 0.065(4) 0.057(4) 0.045(4) -0.008(3) -0.013(3) -0.012(3) C25 0.023(3) 0.026(2) 0.029(2) -0.0015(18) 0.002(2) -0.008(2) C26 0.037(3) 0.058(4) 0.035(3) 0.001(3) 0.002(3) 0.007(3) C27 0.031(3) 0.058(4) 0.054(4) -0.002(3) 0.016(3) 0.010(3) C28 0.047(3) 0.040(3) 0.033(3) 0.000(3) 0.009(3) -0.010(3) C29 0.061(4) 0.051(4) 0.027(3) 0.007(2) 0.006(3) 0.008(3) C30 0.040(3) 0.034(3) 0.041(3) 0.004(2) 0.005(3) 0.006(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 Pt1 O2 2.013(3) . ? Pt1 O1 2.028(3) . ? Pt1 S1 2.2252(12) . ? Pt1 S3 2.2306(12) . ? S1 C3 1.702(4) . ? S2 C3 1.743(4) . ? S2 C4 1.795(4) . ? S3 C18 1.690(5) . ? S4 C18 1.753(4) . ? S4 C19 1.806(4) . ? O1 C1 1.279(5) . ? O2 C16 1.281(5) . ? C1 C2 1.389(6) . ? C1 C10 1.493(6) . ? C2 C3 1.382(6) . ? C2 H2A 0.9500 . ? C4 C5 1.515(6) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.513(6) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C7 1.504(6) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.516(7) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.519(7) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C15 1.376(6) . ? C10 C11 1.390(7) . ? C11 C12 1.372(7) . ? C11 H11A 0.9500 . ? C12 C13 1.385(7) . ? C12 H12A 0.9500 . ? C13 C14 1.367(7) . ? C13 H13A 0.9500 . ? C14 C15 1.396(7) . ? C14 H14A 0.9500 . ? C15 H15A 0.9500 . ? C16 C17 1.393(6) . ? C16 C25 1.496(6) . ? C17 C18 1.388(6) . ? C17 H17A 0.9500 . ? C19 C20 1.522(6) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 C21 1.531(6) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 C22 1.524(6) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C23 1.526(6) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.514(7) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C26 1.360(7) . ? C25 C30 1.386(6) . ? C26 C27 1.400(7) . ? C26 H26A 0.9500 . ? C27 C28 1.368(7) . ? C27 H27A 0.9500 . ? C28 C29 1.363(7) . ? C28 H28A 0.9500 . ? C29 C30 1.401(7) . ? C29 H29A 0.9500 . ? C30 H30A 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Pt1 O1 80.54(12) . . ? O2 Pt1 S1 176.75(9) . . ? O1 Pt1 S1 96.72(9) . . ? O2 Pt1 S3 96.73(9) . . ? O1 Pt1 S3 176.89(9) . . ? S1 Pt1 S3 86.06(4) . . ? C3 S1 Pt1 108.43(16) . . ? C3 S2 C4 107.0(2) . . ? C18 S3 Pt1 108.38(16) . . ? C18 S4 C19 107.6(2) . . ? C1 O1 Pt1 129.5(3) . . ? C16 O2 Pt1 130.8(3) . . ? O1 C1 C2 127.2(4) . . ? O1 C1 C10 113.4(4) . . ? C2 C1 C10 119.4(4) . . ? C3 C2 C1 128.8(4) . . ? C3 C2 H2A 115.6 . . ? C1 C2 H2A 115.6 . . ? C2 C3 S1 129.2(4) . . ? C2 C3 S2 113.4(3) . . ? S1 C3 S2 117.4(3) . . ? C5 C4 S2 108.7(3) . . ? C5 C4 H4A 110.0 . . ? S2 C4 H4A 110.0 . . ? C5 C4 H4B 110.0 . . ? S2 C4 H4B 110.0 . . ? H4A C4 H4B 108.3 . . ? C6 C5 C4 113.0(4) . . ? C6 C5 H5A 109.0 . . ? C4 C5 H5A 109.0 . . ? C6 C5 H5B 109.0 . . ? C4 C5 H5B 109.0 . . ? H5A C5 H5B 107.8 . . ? C7 C6 C5 113.2(4) . . ? C7 C6 H6A 108.9 . . ? C5 C6 H6A 108.9 . . ? C7 C6 H6B 108.9 . . ? C5 C6 H6B 108.9 . . ? H6A C6 H6B 107.8 . . ? C6 C7 C8 114.3(4) . . ? C6 C7 H7A 108.7 . . ? C8 C7 H7A 108.7 . . ? C6 C7 H7B 108.7 . . ? C8 C7 H7B 108.7 . . ? H7A C7 H7B 107.6 . . ? C7 C8 C9 113.0(4) . . ? C7 C8 H8A 109.0 . . ? C9 C8 H8A 109.0 . . ? C7 C8 H8B 109.0 . . ? C9 C8 H8B 109.0 . . ? H8A C8 H8B 107.8 . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C15 C10 C11 117.8(4) . . ? C15 C10 C1 123.7(4) . . ? C11 C10 C1 118.5(4) . . ? C12 C11 C10 121.1(5) . . ? C12 C11 H11A 119.5 . . ? C10 C11 H11A 119.5 . . ? C11 C12 C13 121.0(5) . . ? C11 C12 H12A 119.5 . . ? C13 C12 H12A 119.5 . . ? C14 C13 C12 118.4(5) . . ? C14 C13 H13A 120.8 . . ? C12 C13 H13A 120.8 . . ? C13 C14 C15 120.9(5) . . ? C13 C14 H14A 119.6 . . ? C15 C14 H14A 119.6 . . ? C10 C15 C14 120.8(5) . . ? C10 C15 H15A 119.6 . . ? C14 C15 H15A 119.6 . . ? O2 C16 C17 125.0(4) . . ? O2 C16 C25 114.4(4) . . ? C17 C16 C25 120.5(4) . . ? C18 C17 C16 130.3(5) . . ? C18 C17 H17A 114.9 . . ? C16 C17 H17A 114.9 . . ? C17 C18 S3 128.6(4) . . ? C17 C18 S4 112.4(4) . . ? S3 C18 S4 118.9(3) . . ? C20 C19 S4 113.6(3) . . ? C20 C19 H19A 108.8 . . ? S4 C19 H19A 108.8 . . ? C20 C19 H19B 108.8 . . ? S4 C19 H19B 108.8 . . ? H19A C19 H19B 107.7 . . ? C19 C20 C21 112.1(4) . . ? C19 C20 H20A 109.2 . . ? C21 C20 H20A 109.2 . . ? C19 C20 H20B 109.2 . . ? C21 C20 H20B 109.2 . . ? H20A C20 H20B 107.9 . . ? C22 C21 C20 112.1(4) . . ? C22 C21 H21A 109.2 . . ? C20 C21 H21A 109.2 . . ? C22 C21 H21B 109.2 . . ? C20 C21 H21B 109.2 . . ? H21A C21 H21B 107.9 . . ? C21 C22 C23 112.7(4) . . ? C21 C22 H22A 109.0 . . ? C23 C22 H22A 109.0 . . ? C21 C22 H22B 109.0 . . ? C23 C22 H22B 109.0 . . ? H22A C22 H22B 107.8 . . ? C24 C23 C22 112.3(4) . . ? C24 C23 H23A 109.1 . . ? C22 C23 H23A 109.1 . . ? C24 C23 H23B 109.1 . . ? C22 C23 H23B 109.1 . . ? H23A C23 H23B 107.9 . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C26 C25 C30 118.2(4) . . ? C26 C25 C16 123.9(4) . . ? C30 C25 C16 117.9(4) . . ? C25 C26 C27 121.6(5) . . ? C25 C26 H26A 119.2 . . ? C27 C26 H26A 119.2 . . ? C28 C27 C26 119.6(5) . . ? C28 C27 H27A 120.2 . . ? C26 C27 H27A 120.2 . . ? C29 C28 C27 119.8(5) . . ? C29 C28 H28A 120.1 . . ? C27 C28 H28A 120.1 . . ? C28 C29 C30 120.3(5) . . ? C28 C29 H29A 119.8 . . ? C30 C29 H29A 119.8 . . ? C25 C30 C29 120.4(5) . . ? C25 C30 H30A 119.8 . . ? C29 C30 H30A 119.8 . . ? _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.979 _refine_diff_density_max 0.560 _refine_diff_density_min -0.975 _refine_diff_density_rms 0.153 _database_code_depnum_ccdc_archive 'CCDC 915587'