# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2008 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 loop_ _publ_author_name _publ_author_footnote _publ_author_address 'Mark Stradiotto' . ; Department of Chemistry Dalhousie University Dalhousie, Nova Scotia B3H 4J3 Canada ; 'Michael Ferguson' . ; Department of Chemistry Dalhousie University Dalhousie, Nova Scotia B3H 4J3 Canada ; 'Kevin D. Hesp' . ; Saskatchewan Structural Sciences Centre University of Saskatchewan Saskatoon, Saskatchewan S7N 5C9 Canada ; 'Robert McDonald' '' '' 'Gabriele Schatte' '' '' _publ_contact_author_name 'Mark Stradiotto' _publ_contact_author_email MARK.STRADIOTTO@DAL.CA _publ_section_title ; (kappa2-P,S)Pt(benzyl) Complexes Derived from 1/3-PiPr2-2-StBu-Indene: Facile Synthesis of Carbanion- and Borate-Containing Zwitterions ; _publ_contact_author_address ; Department of Chemistry Dalhousie University Dalhousie, Nova Scotia B3H 4J3 Canada ; _publ_contact_author_fax '001 902 494 1310' _publ_contact_author_phone '001 902 494 7190' _publ_contact_letter ; To: Cambridge Crystallographic Data Centre Please accept the following CIF file which is being submitted in support of an upcoming communication to be published in 'Journal'. Please forward any questions concerning this CIF to Dr. Gabriele Schatte (gabriele.schatte@usask.ca). ; # Attachment 'dal0727.cif' data_dal0727 _database_code_depnum_ccdc_archive 'CCDC 687090' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C33 H45 N2 P Pt S' _chemical_formula_sum 'C33 H45 N2 P Pt S' _chemical_formula_weight 727.83 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 10.6807(9) _cell_length_b 14.1937(11) _cell_length_c 20.6273(17) _cell_angle_alpha 90.00 _cell_angle_beta 97.7681(9) _cell_angle_gamma 90.00 _cell_volume 3098.4(4) _cell_formula_units_Z 4 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 6967 _cell_measurement_theta_min 2.46 _cell_measurement_theta_max 27.46 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.560 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1464 _exptl_absorpt_coefficient_mu 4.672 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2698 _exptl_absorpt_correction_T_max 0.4002 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker PLATFORM diffractometer/SMART 1000 CCD area detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 8.192 _diffrn_standards_number 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 23093 _diffrn_reflns_av_R_equivalents 0.0264 _diffrn_reflns_av_sigmaI/netI 0.0255 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.75 _diffrn_reflns_theta_max 27.50 _reflns_number_total 7060 _reflns_number_gt 6143 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART (Bruker, 1997)' _computing_cell_refinement 'Bruker SAINT (Bruker, 1997)' _computing_data_reduction 'Bruker SAINT (Bruker, 1997)' _computing_structure_solution 'DIRDIF-96 (Beurskens et al., 1996)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL (Bruker, 1997)' _computing_publication_material 'Bruker SHELXTL (Bruker, 1997)' _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^)+(0.0313P)^2^+0.8293P] 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 7060 _refine_ls_number_parameters 345 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0301 _refine_ls_R_factor_gt 0.0235 _refine_ls_wR_factor_ref 0.0573 _refine_ls_wR_factor_gt 0.0547 _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_restrained_S_all 1.059 _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 0.039024(9) 0.128552(7) 0.373705(5) 0.02268(4) Uani 1 1 d . . . S S -0.05081(6) -0.02300(5) 0.39074(3) 0.02448(14) Uani 1 1 d . . . P P 0.20470(7) 0.05346(5) 0.34243(3) 0.02335(14) Uani 1 1 d . . . N30 N -0.1155(2) 0.20525(15) 0.39902(11) 0.0264(5) Uani 1 1 d . . . N31 N -0.4285(3) 0.35545(18) 0.44618(14) 0.0383(6) Uani 1 1 d . . . C1 C 0.0606(3) -0.20010(19) 0.36765(13) 0.0281(6) Uani 1 1 d . . . H1 H -0.0027 -0.2385 0.3824 0.034 Uiso 1 1 calc R . . C2 C 0.0606(3) -0.1017(2) 0.36383(13) 0.0248(5) Uani 1 1 d . . . C3 C 0.1710(3) -0.06848(18) 0.33978(14) 0.0253(6) Uani 1 1 d . . . C3A C 0.2443(3) -0.15040(18) 0.32966(13) 0.0256(6) Uani 1 1 d . . . C4 C 0.3656(3) -0.1649(2) 0.31149(15) 0.0319(6) Uani 1 1 d . . . H4 H 0.4162 -0.1125 0.3030 0.038 Uiso 1 1 calc R . . C5 C 0.4106(3) -0.2549(2) 0.30614(15) 0.0358(7) Uani 1 1 d . . . H5 H 0.4922 -0.2639 0.2937 0.043 Uiso 1 1 calc R . . C6 C 0.3382(3) -0.3337(2) 0.31870(16) 0.0368(7) Uani 1 1 d . . . H6 H 0.3702 -0.3954 0.3136 0.044 Uiso 1 1 calc R . . C7 C 0.2213(3) -0.3222(2) 0.33828(15) 0.0326(6) Uani 1 1 d . . . H7 H 0.1732 -0.3758 0.3471 0.039 Uiso 1 1 calc R . . C7A C 0.1726(3) -0.23135(19) 0.34528(13) 0.0264(6) Uani 1 1 d . . . C10 C 0.1171(3) 0.25997(19) 0.36090(14) 0.0299(6) Uani 1 1 d . . . H10A H 0.2008 0.2504 0.3463 0.036 Uiso 1 1 calc R . . H10B H 0.0629 0.2926 0.3251 0.036 Uiso 1 1 calc R . . C11 C 0.1345(3) 0.32482(19) 0.41997(14) 0.0281(6) Uani 1 1 d . . . C12 C 0.1767(3) 0.2928(2) 0.48306(15) 0.0356(7) Uani 1 1 d . . . H12 H 0.1893 0.2272 0.4903 0.043 Uiso 1 1 calc R . . C13 C 0.2007(3) 0.3542(2) 0.53544(16) 0.0394(7) Uani 1 1 d . . . H13 H 0.2297 0.3303 0.5778 0.047 Uiso 1 1 calc R . . C14 C 0.1828(3) 0.4499(2) 0.52659(17) 0.0428(8) Uani 1 1 d . . . H14 H 0.2004 0.4922 0.5624 0.051 Uiso 1 1 calc R . . C15 C 0.1390(4) 0.4831(2) 0.46511(18) 0.0482(9) Uani 1 1 d . . . H15 H 0.1247 0.5486 0.4585 0.058 Uiso 1 1 calc R . . C16 C 0.1153(3) 0.4215(2) 0.41235(16) 0.0388(7) Uani 1 1 d . . . H16 H 0.0855 0.4459 0.3702 0.047 Uiso 1 1 calc R . . C21 C 0.2349(3) 0.0976(2) 0.26158(14) 0.0288(6) Uani 1 1 d . . . H21 H 0.2516 0.1668 0.2665 0.035 Uiso 1 1 calc R . . C22 C 0.1145(3) 0.0864(3) 0.21329(16) 0.0479(9) Uani 1 1 d . . . H22A H 0.0438 0.1161 0.2312 0.057 Uiso 1 1 calc R . . H22B H 0.0966 0.0192 0.2059 0.057 Uiso 1 1 calc R . . H22C H 0.1258 0.1165 0.1717 0.057 Uiso 1 1 calc R . . C23 C 0.3468(3) 0.0548(2) 0.23398(16) 0.0394(7) Uani 1 1 d . . . H23A H 0.4235 0.0636 0.2652 0.047 Uiso 1 1 calc R . . H23B H 0.3571 0.0859 0.1926 0.047 Uiso 1 1 calc R . . H23C H 0.3319 -0.0126 0.2263 0.047 Uiso 1 1 calc R . . C24 C 0.3545(3) 0.0607(2) 0.39842(15) 0.0302(6) Uani 1 1 d . . . H24 H 0.4135 0.0136 0.3830 0.036 Uiso 1 1 calc R . . C25 C 0.4214(3) 0.1560(2) 0.40152(18) 0.0418(8) Uani 1 1 d . . . H25A H 0.4374 0.1741 0.3575 0.050 Uiso 1 1 calc R . . H25B H 0.5018 0.1514 0.4305 0.050 Uiso 1 1 calc R . . H25C H 0.3679 0.2036 0.4185 0.050 Uiso 1 1 calc R . . C26 C 0.3289(3) 0.0292(2) 0.46659(15) 0.0406(7) Uani 1 1 d . . . H26A H 0.2855 -0.0318 0.4632 0.049 Uiso 1 1 calc R . . H26B H 0.2757 0.0760 0.4846 0.049 Uiso 1 1 calc R . . H26C H 0.4092 0.0232 0.4955 0.049 Uiso 1 1 calc R . . C27 C -0.1988(3) -0.0465(2) 0.33307(14) 0.0301(6) Uani 1 1 d . . . C28 C -0.2952(3) 0.0266(2) 0.34795(18) 0.0421(8) Uani 1 1 d . . . H28A H -0.2642 0.0897 0.3394 0.051 Uiso 1 1 calc R . . H28B H -0.3078 0.0217 0.3940 0.051 Uiso 1 1 calc R . . H28C H -0.3756 0.0154 0.3200 0.051 Uiso 1 1 calc R . . C29 C -0.1718(3) -0.0406(3) 0.26302(15) 0.0438(8) Uani 1 1 d . . . H29A H -0.1379 0.0218 0.2550 0.053 Uiso 1 1 calc R . . H29B H -0.2501 -0.0510 0.2332 0.053 Uiso 1 1 calc R . . H29C H -0.1098 -0.0890 0.2555 0.053 Uiso 1 1 calc R . . C30 C -0.2462(3) -0.1449(2) 0.3483(2) 0.0506(10) Uani 1 1 d . . . H30A H -0.1815 -0.1917 0.3421 0.061 Uiso 1 1 calc R . . H30B H -0.3238 -0.1589 0.3188 0.061 Uiso 1 1 calc R . . H30C H -0.2637 -0.1469 0.3937 0.061 Uiso 1 1 calc R . . C31 C -0.1881(3) 0.2583(2) 0.35426(14) 0.0311(6) Uani 1 1 d . . . H31 H -0.1668 0.2608 0.3110 0.037 Uiso 1 1 calc R . . C32 C -0.2908(3) 0.3087(2) 0.36807(15) 0.0323(6) Uani 1 1 d . . . H32 H -0.3391 0.3441 0.3345 0.039 Uiso 1 1 calc R . . C33 C -0.3254(3) 0.30837(19) 0.43133(14) 0.0296(6) Uani 1 1 d . . . C34 C -0.2463(3) 0.2550(2) 0.47818(14) 0.0316(6) Uani 1 1 d . . . H34 H -0.2623 0.2533 0.5224 0.038 Uiso 1 1 calc R . . C35 C -0.1466(3) 0.20585(19) 0.45983(14) 0.0291(6) Uani 1 1 d . . . H35 H -0.0962 0.1698 0.4923 0.035 Uiso 1 1 calc R . . C36 C -0.5109(3) 0.4060(3) 0.39613(19) 0.0490(9) Uani 1 1 d . . . H36A H -0.4669 0.4618 0.3826 0.059 Uiso 1 1 calc R . . H36B H -0.5876 0.4255 0.4137 0.059 Uiso 1 1 calc R . . H36C H -0.5338 0.3648 0.3583 0.059 Uiso 1 1 calc R . . C37 C -0.4594(4) 0.3550(3) 0.51275(19) 0.0512(9) Uani 1 1 d . . . H37A H -0.4693 0.2899 0.5269 0.061 Uiso 1 1 calc R . . H37B H -0.5385 0.3895 0.5142 0.061 Uiso 1 1 calc R . . H37C H -0.3912 0.3854 0.5419 0.061 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 0.02313(6) 0.01950(6) 0.02602(6) -0.00061(4) 0.00551(4) 0.00079(4) S 0.0220(3) 0.0243(3) 0.0275(3) 0.0006(3) 0.0048(3) -0.0006(2) P 0.0219(3) 0.0193(3) 0.0296(4) -0.0012(3) 0.0062(3) -0.0019(3) N30 0.0272(12) 0.0231(11) 0.0290(12) -0.0017(9) 0.0040(10) 0.0010(9) N31 0.0303(14) 0.0343(14) 0.0510(17) -0.0095(12) 0.0088(12) 0.0050(11) C1 0.0270(15) 0.0228(14) 0.0348(15) 0.0023(11) 0.0047(12) -0.0038(11) C2 0.0254(14) 0.0233(13) 0.0248(13) 0.0009(10) 0.0002(11) 0.0003(10) C3 0.0241(14) 0.0192(12) 0.0333(15) -0.0006(11) 0.0063(11) -0.0004(10) C3A 0.0252(14) 0.0229(13) 0.0277(14) -0.0015(11) -0.0006(11) 0.0002(10) C4 0.0288(16) 0.0247(14) 0.0428(17) -0.0033(12) 0.0076(13) -0.0004(12) C5 0.0289(16) 0.0330(16) 0.0455(18) -0.0022(13) 0.0051(13) 0.0055(12) C6 0.0380(18) 0.0245(15) 0.0464(18) -0.0041(13) 0.0010(14) 0.0070(12) C7 0.0370(17) 0.0217(14) 0.0370(16) 0.0003(12) -0.0021(13) -0.0008(12) C7A 0.0238(14) 0.0255(14) 0.0284(14) -0.0013(11) -0.0017(11) -0.0020(11) C10 0.0374(16) 0.0220(14) 0.0314(15) 0.0003(11) 0.0079(12) -0.0013(12) C11 0.0259(15) 0.0237(14) 0.0364(15) -0.0003(12) 0.0112(12) 0.0002(11) C12 0.0445(18) 0.0228(14) 0.0403(17) 0.0000(12) 0.0090(14) 0.0029(12) C13 0.046(2) 0.0364(17) 0.0364(17) -0.0030(13) 0.0079(15) -0.0014(14) C14 0.053(2) 0.0313(17) 0.0467(19) -0.0129(14) 0.0178(16) -0.0081(15) C15 0.065(2) 0.0221(15) 0.060(2) -0.0046(15) 0.0185(19) 0.0034(15) C16 0.051(2) 0.0244(15) 0.0420(18) 0.0026(13) 0.0086(15) 0.0046(13) C21 0.0303(15) 0.0259(14) 0.0317(15) 0.0008(11) 0.0101(12) -0.0012(11) C22 0.0381(19) 0.073(3) 0.0322(17) 0.0108(17) 0.0044(14) -0.0006(17) C23 0.0398(18) 0.0388(17) 0.0431(18) 0.0031(14) 0.0177(15) 0.0041(14) C24 0.0234(15) 0.0275(14) 0.0394(16) -0.0047(12) 0.0037(12) 0.0002(11) C25 0.0330(18) 0.0367(17) 0.055(2) -0.0113(15) 0.0031(15) -0.0079(13) C26 0.0369(18) 0.0422(18) 0.0411(18) 0.0012(14) -0.0004(14) 0.0055(14) C27 0.0232(14) 0.0280(15) 0.0376(16) -0.0008(12) -0.0010(12) -0.0015(11) C28 0.0271(17) 0.0402(18) 0.058(2) -0.0060(15) 0.0022(15) 0.0043(13) C29 0.0384(19) 0.055(2) 0.0355(17) -0.0056(15) -0.0044(14) 0.0027(15) C30 0.0317(19) 0.0365(18) 0.080(3) 0.0045(17) -0.0068(18) -0.0095(14) C31 0.0343(16) 0.0291(15) 0.0306(15) 0.0013(12) 0.0067(12) 0.0015(12) C32 0.0328(16) 0.0269(14) 0.0372(16) 0.0046(12) 0.0041(13) 0.0056(12) C33 0.0270(15) 0.0228(13) 0.0390(16) -0.0079(12) 0.0048(12) -0.0019(11) C34 0.0303(15) 0.0345(15) 0.0309(15) -0.0064(12) 0.0073(12) -0.0001(12) C35 0.0303(15) 0.0282(14) 0.0283(14) 0.0006(11) 0.0027(12) 0.0012(11) C36 0.0371(19) 0.0404(19) 0.071(2) 0.0037(17) 0.0117(18) 0.0146(15) C37 0.040(2) 0.062(2) 0.054(2) -0.0179(18) 0.0161(17) 0.0091(16) _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 C10 2.075(3) . ? Pt N30 2.102(2) . ? Pt P 2.2342(7) . ? Pt S 2.4005(7) . ? S C2 1.775(3) . ? S C27 1.875(3) . ? P C3 1.767(3) . ? P C24 1.845(3) . ? P C21 1.850(3) . ? N30 C35 1.340(3) . ? N30 C31 1.351(4) . ? N31 C33 1.358(4) . ? N31 C36 1.452(4) . ? N31 C37 1.455(4) . ? C1 C2 1.399(4) . ? C1 C7A 1.411(4) . ? C2 C3 1.420(4) . ? C3 C3A 1.433(4) . ? C3A C4 1.412(4) . ? C3A C7A 1.441(4) . ? C4 C5 1.374(4) . ? C5 C6 1.405(4) . ? C6 C7 1.373(4) . ? C7 C7A 1.405(4) . ? C10 C11 1.518(4) . ? C11 C16 1.393(4) . ? C11 C12 1.395(4) . ? C12 C13 1.385(4) . ? C13 C14 1.380(4) . ? C14 C15 1.374(5) . ? C15 C16 1.392(5) . ? C21 C23 1.518(4) . ? C21 C22 1.524(4) . ? C24 C25 1.526(4) . ? C24 C26 1.535(4) . ? C27 C29 1.513(4) . ? C27 C28 1.522(4) . ? C27 C30 1.532(4) . ? C31 C32 1.372(4) . ? C32 C33 1.403(4) . ? C33 C34 1.414(4) . ? C34 C35 1.369(4) . ? 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 C10 Pt N30 84.77(10) . . ? C10 Pt P 92.54(8) . . ? N30 Pt P 176.65(6) . . ? C10 Pt S 178.90(8) . . ? N30 Pt S 94.87(6) . . ? P Pt S 87.86(2) . . ? C2 S C27 103.48(13) . . ? C2 S Pt 102.70(10) . . ? C27 S Pt 112.71(9) . . ? C3 P C24 103.30(13) . . ? C3 P C21 111.32(13) . . ? C24 P C21 107.65(14) . . ? C3 P Pt 108.07(9) . . ? C24 P Pt 116.49(10) . . ? C21 P Pt 109.87(9) . . ? C35 N30 C31 116.4(2) . . ? C35 N30 Pt 122.54(19) . . ? C31 N30 Pt 121.05(19) . . ? C33 N31 C36 121.0(3) . . ? C33 N31 C37 120.3(3) . . ? C36 N31 C37 118.7(3) . . ? C2 C1 C7A 106.8(2) . . ? C1 C2 C3 111.0(2) . . ? C1 C2 S 127.2(2) . . ? C3 C2 S 121.6(2) . . ? C2 C3 C3A 106.1(2) . . ? C2 C3 P 119.3(2) . . ? C3A C3 P 133.3(2) . . ? C4 C3A C3 134.1(3) . . ? C4 C3A C7A 118.5(2) . . ? C3 C3A C7A 107.3(2) . . ? C5 C4 C3A 120.0(3) . . ? C4 C5 C6 121.2(3) . . ? C7 C6 C5 120.3(3) . . ? C6 C7 C7A 120.3(3) . . ? C7 C7A C1 131.6(3) . . ? C7 C7A C3A 119.6(3) . . ? C1 C7A C3A 108.8(2) . . ? C11 C10 Pt 116.77(19) . . ? C16 C11 C12 116.8(3) . . ? C16 C11 C10 120.4(3) . . ? C12 C11 C10 122.7(2) . . ? C13 C12 C11 121.7(3) . . ? C14 C13 C12 120.6(3) . . ? C15 C14 C13 118.8(3) . . ? C14 C15 C16 120.7(3) . . ? C15 C16 C11 121.5(3) . . ? C23 C21 C22 110.5(3) . . ? C23 C21 P 116.4(2) . . ? C22 C21 P 108.6(2) . . ? C25 C24 C26 111.1(3) . . ? C25 C24 P 115.9(2) . . ? C26 C24 P 108.1(2) . . ? C29 C27 C28 112.1(3) . . ? C29 C27 C30 110.9(3) . . ? C28 C27 C30 109.2(3) . . ? C29 C27 S 110.0(2) . . ? C28 C27 S 106.6(2) . . ? C30 C27 S 107.8(2) . . ? N30 C31 C32 123.3(3) . . ? C31 C32 C33 120.7(3) . . ? N31 C33 C32 122.1(3) . . ? N31 C33 C34 122.5(3) . . ? C32 C33 C34 115.4(3) . . ? C35 C34 C33 120.0(3) . . ? N30 C35 C34 124.2(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C10 Pt S C2 -115(4) . . . . ? N30 Pt S C2 174.47(11) . . . . ? P Pt S C2 -3.59(9) . . . . ? C10 Pt S C27 135(4) . . . . ? N30 Pt S C27 63.78(12) . . . . ? P Pt S C27 -114.27(10) . . . . ? C10 Pt P C3 -175.32(13) . . . . ? N30 Pt P C3 -138.9(11) . . . . ? S Pt P C3 5.70(10) . . . . ? C10 Pt P C24 69.02(13) . . . . ? N30 Pt P C24 105.4(11) . . . . ? S Pt P C24 -109.95(11) . . . . ? C10 Pt P C21 -53.69(13) . . . . ? N30 Pt P C21 -17.3(11) . . . . ? S Pt P C21 127.33(10) . . . . ? C10 Pt N30 C35 -112.2(2) . . . . ? P Pt N30 C35 -148.7(10) . . . . ? S Pt N30 C35 66.8(2) . . . . ? C10 Pt N30 C31 66.7(2) . . . . ? P Pt N30 C31 30.1(12) . . . . ? S Pt N30 C31 -114.3(2) . . . . ? C7A C1 C2 C3 -0.4(3) . . . . ? C7A C1 C2 S -175.2(2) . . . . ? C27 S C2 C1 -68.0(3) . . . . ? Pt S C2 C1 174.5(2) . . . . ? C27 S C2 C3 117.6(2) . . . . ? Pt S C2 C3 0.2(2) . . . . ? C1 C2 C3 C3A -1.4(3) . . . . ? S C2 C3 C3A 173.83(19) . . . . ? C1 C2 C3 P -170.30(19) . . . . ? S C2 C3 P 4.9(3) . . . . ? C24 P C3 C2 116.4(2) . . . . ? C21 P C3 C2 -128.3(2) . . . . ? Pt P C3 C2 -7.6(2) . . . . ? C24 P C3 C3A -48.8(3) . . . . ? C21 P C3 C3A 66.4(3) . . . . ? Pt P C3 C3A -172.9(3) . . . . ? C2 C3 C3A C4 -174.4(3) . . . . ? P C3 C3A C4 -7.8(5) . . . . ? C2 C3 C3A C7A 2.5(3) . . . . ? P C3 C3A C7A 169.2(2) . . . . ? C3 C3A C4 C5 179.6(3) . . . . ? C7A C3A C4 C5 2.9(4) . . . . ? C3A C4 C5 C6 -0.2(5) . . . . ? C4 C5 C6 C7 -1.6(5) . . . . ? C5 C6 C7 C7A 0.6(5) . . . . ? C6 C7 C7A C1 -176.1(3) . . . . ? C6 C7 C7A C3A 2.1(4) . . . . ? C2 C1 C7A C7 -179.7(3) . . . . ? C2 C1 C7A C3A 2.0(3) . . . . ? C4 C3A C7A C7 -3.8(4) . . . . ? C3 C3A C7A C7 178.6(2) . . . . ? C4 C3A C7A C1 174.7(3) . . . . ? C3 C3A C7A C1 -2.8(3) . . . . ? N30 Pt C10 C11 59.0(2) . . . . ? P Pt C10 C11 -123.0(2) . . . . ? S Pt C10 C11 -12(5) . . . . ? Pt C10 C11 C16 -143.2(2) . . . . ? Pt C10 C11 C12 40.6(4) . . . . ? C16 C11 C12 C13 -1.2(5) . . . . ? C10 C11 C12 C13 175.2(3) . . . . ? C11 C12 C13 C14 0.3(5) . . . . ? C12 C13 C14 C15 0.9(5) . . . . ? C13 C14 C15 C16 -1.2(5) . . . . ? C14 C15 C16 C11 0.3(5) . . . . ? C12 C11 C16 C15 0.9(5) . . . . ? C10 C11 C16 C15 -175.6(3) . . . . ? C3 P C21 C23 -61.6(3) . . . . ? C24 P C21 C23 51.0(3) . . . . ? Pt P C21 C23 178.8(2) . . . . ? C3 P C21 C22 63.8(2) . . . . ? C24 P C21 C22 176.4(2) . . . . ? Pt P C21 C22 -55.8(2) . . . . ? C3 P C24 C25 169.4(2) . . . . ? C21 P C24 C25 51.6(3) . . . . ? Pt P C24 C25 -72.3(2) . . . . ? C3 P C24 C26 -65.1(2) . . . . ? C21 P C24 C26 177.1(2) . . . . ? Pt P C24 C26 53.2(2) . . . . ? C2 S C27 C29 -51.7(2) . . . . ? Pt S C27 C29 58.5(2) . . . . ? C2 S C27 C28 -173.5(2) . . . . ? Pt S C27 C28 -63.3(2) . . . . ? C2 S C27 C30 69.4(2) . . . . ? Pt S C27 C30 179.6(2) . . . . ? C35 N30 C31 C32 -1.9(4) . . . . ? Pt N30 C31 C32 179.1(2) . . . . ? N30 C31 C32 C33 0.8(5) . . . . ? C36 N31 C33 C32 2.2(4) . . . . ? C37 N31 C33 C32 -178.6(3) . . . . ? C36 N31 C33 C34 -177.1(3) . . . . ? C37 N31 C33 C34 2.0(4) . . . . ? C31 C32 C33 N31 -178.2(3) . . . . ? C31 C32 C33 C34 1.2(4) . . . . ? N31 C33 C34 C35 177.3(3) . . . . ? C32 C33 C34 C35 -2.1(4) . . . . ? C31 N30 C35 C34 0.9(4) . . . . ? Pt N30 C35 C34 179.9(2) . . . . ? C33 C34 C35 N30 1.1(4) . . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.25 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.653 _refine_diff_density_min -0.318 _refine_diff_density_rms 0.104 # Attachment 'dal0745.cif' data_dal0745 _database_code_depnum_ccdc_archive 'CCDC 687091' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C51 H43 B F15 P Pt S' _chemical_formula_weight 1209.78 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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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 Pbca 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 21.679(2) _cell_length_b 18.6294(17) _cell_length_c 23.275(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 9400.0(15) _cell_formula_units_Z 8 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 5324 _cell_measurement_theta_min 2.19 _cell_measurement_theta_max 23.35 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.710 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4784 _exptl_absorpt_coefficient_mu 3.160 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4408 _exptl_absorpt_correction_T_max 0.8091 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker PLATFORM diffractometer/SMART 1000 CCD area detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 8.192 _diffrn_standards_number 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 69138 _diffrn_reflns_av_R_equivalents 0.1001 _diffrn_reflns_av_sigmaI/netI 0.0582 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.69 _diffrn_reflns_theta_max 27.00 _reflns_number_total 10253 _reflns_number_gt 6580 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART (Bruker, 1997)' _computing_cell_refinement 'Bruker SAINT (Bruker, 1997)' _computing_data_reduction 'Bruker SAINT (Bruker, 1997)' _computing_structure_solution 'DIRDIF-96 (Beurskens et al., 1996)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL (Bruker, 1997)' _computing_publication_material 'Bruker SHELXTL (Bruker, 1997)' _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^+7.9483P] 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 10253 _refine_ls_number_parameters 632 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0840 _refine_ls_R_factor_gt 0.0379 _refine_ls_wR_factor_ref 0.0892 _refine_ls_wR_factor_gt 0.0716 _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_restrained_S_all 1.060 _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 0.182154(8) 0.162979(10) 0.342316(8) 0.02619(6) Uani 1 1 d . . . P P 0.12188(6) 0.25579(7) 0.36402(6) 0.0264(3) Uani 1 1 d . . . S S 0.26973(5) 0.23517(7) 0.36074(5) 0.0255(3) Uani 1 1 d . . . F32 F 0.26903(13) 0.17911(15) 0.48250(13) 0.0366(7) Uani 1 1 d . . . F33 F 0.19537(15) 0.10939(17) 0.55386(15) 0.0508(9) Uani 1 1 d . . . F34 F 0.13338(16) 0.18051(19) 0.63802(15) 0.0561(10) Uani 1 1 d . . . F35 F 0.14866(15) 0.32507(18) 0.64929(13) 0.0490(9) Uani 1 1 d . . . F36 F 0.22802(14) 0.39526(16) 0.58353(13) 0.0394(8) Uani 1 1 d . . . F42 F 0.36145(14) 0.20246(17) 0.55449(14) 0.0428(8) Uani 1 1 d . . . F43 F 0.46135(14) 0.13115(17) 0.52839(16) 0.0539(9) Uani 1 1 d . . . F44 F 0.53345(15) 0.1705(2) 0.43855(17) 0.0654(11) Uani 1 1 d . . . F45 F 0.49821(15) 0.2848(2) 0.37241(16) 0.0642(11) Uani 1 1 d . . . F46 F 0.39692(14) 0.35549(18) 0.39478(14) 0.0477(9) Uani 1 1 d . . . F52 F 0.36131(14) 0.47635(16) 0.44893(14) 0.0463(8) Uani 1 1 d . . . F53 F 0.44054(16) 0.55643(18) 0.50454(19) 0.0683(12) Uani 1 1 d . . . F54 F 0.46761(18) 0.5314(2) 0.61732(19) 0.0795(13) Uani 1 1 d . . . F55 F 0.41554(16) 0.4173(2) 0.67068(15) 0.0616(11) Uani 1 1 d . . . F56 F 0.34214(15) 0.32948(18) 0.61504(13) 0.0459(8) Uani 1 1 d . . . C1 C 0.2693(2) 0.3651(3) 0.4328(2) 0.0246(11) Uani 1 1 d . . . H1 H 0.2989 0.3913 0.4074 0.030 Uiso 1 1 calc R . . C2 C 0.2356(2) 0.3096(3) 0.3971(2) 0.0223(10) Uani 1 1 d . . . C3 C 0.1739(2) 0.3207(2) 0.3964(2) 0.0242(11) Uani 1 1 d . . . C3A C 0.1603(2) 0.3877(3) 0.4261(2) 0.0256(11) Uani 1 1 d . . . C4 C 0.1054(2) 0.4255(3) 0.4324(2) 0.0335(13) Uani 1 1 d . . . H4 H 0.0678 0.4066 0.4180 0.040 Uiso 1 1 calc R . . C5 C 0.1066(2) 0.4905(3) 0.4600(2) 0.0381(14) Uani 1 1 d . . . H5 H 0.0695 0.5171 0.4644 0.046 Uiso 1 1 calc R . . C6 C 0.1613(2) 0.5178(3) 0.4813(2) 0.0377(13) Uani 1 1 d . . . H6 H 0.1612 0.5629 0.5003 0.045 Uiso 1 1 calc R . . C7 C 0.2160(2) 0.4807(3) 0.4754(2) 0.0298(12) Uani 1 1 d . . . H7 H 0.2533 0.5001 0.4904 0.036 Uiso 1 1 calc R . . C7A C 0.2162(2) 0.4149(3) 0.4474(2) 0.0254(11) Uani 1 1 d . . . C10 C 0.1209(3) 0.0790(3) 0.3264(3) 0.0395(14) Uani 1 1 d . . . H10A H 0.1055 0.0533 0.3608 0.047 Uiso 1 1 calc R . . H10B H 0.0879 0.0892 0.2982 0.047 Uiso 1 1 calc R . . C11 C 0.1785(3) 0.0527(3) 0.3026(2) 0.0351(12) Uani 1 1 d . . . C12 C 0.2296(2) 0.0493(3) 0.3404(2) 0.0331(12) Uani 1 1 d . . . H12 H 0.2207 0.0205 0.3757 0.040 Uiso 1 1 calc R . . C13 C 0.2888(3) 0.0358(3) 0.3182(3) 0.0437(15) Uani 1 1 d . . . H13 H 0.3230 0.0320 0.3435 0.052 Uiso 1 1 calc R . . C14 C 0.2976(3) 0.0282(3) 0.2606(3) 0.0491(17) Uani 1 1 d . . . H14 H 0.3378 0.0193 0.2459 0.059 Uiso 1 1 calc R . . C15 C 0.2475(3) 0.0335(3) 0.2231(3) 0.0498(17) Uani 1 1 d . . . H15 H 0.2541 0.0280 0.1830 0.060 Uiso 1 1 calc R . . C16 C 0.1896(3) 0.0464(3) 0.2425(3) 0.0453(15) Uani 1 1 d . . . H16 H 0.1565 0.0513 0.2161 0.054 Uiso 1 1 calc R . . C21 C 0.0640(2) 0.2395(3) 0.4209(2) 0.0311(12) Uani 1 1 d . . . H21 H 0.0450 0.2868 0.4308 0.037 Uiso 1 1 calc R . . C22 C 0.0969(3) 0.2125(3) 0.4737(2) 0.0417(14) Uani 1 1 d . . . H22A H 0.1286 0.2471 0.4851 0.050 Uiso 1 1 calc R . . H22B H 0.1163 0.1662 0.4652 0.050 Uiso 1 1 calc R . . H22C H 0.0672 0.2065 0.5050 0.050 Uiso 1 1 calc R . . C23 C 0.0127(3) 0.1904(3) 0.4018(3) 0.0469(16) Uani 1 1 d . . . H23A H -0.0083 0.2114 0.3684 0.056 Uiso 1 1 calc R . . H23B H -0.0170 0.1843 0.4332 0.056 Uiso 1 1 calc R . . H23C H 0.0299 0.1436 0.3913 0.056 Uiso 1 1 calc R . . C24 C 0.0784(2) 0.3014(3) 0.3063(2) 0.0342(13) Uani 1 1 d . . . H24 H 0.0412 0.3238 0.3245 0.041 Uiso 1 1 calc R . . C25 C 0.1152(3) 0.3618(3) 0.2782(3) 0.0418(14) Uani 1 1 d . . . H25A H 0.1282 0.3962 0.3077 0.050 Uiso 1 1 calc R . . H25B H 0.0894 0.3862 0.2497 0.050 Uiso 1 1 calc R . . H25C H 0.1517 0.3417 0.2593 0.050 Uiso 1 1 calc R . . C26 C 0.0552(3) 0.2481(3) 0.2617(3) 0.0517(17) Uani 1 1 d . . . H26A H 0.0300 0.2113 0.2806 0.062 Uiso 1 1 calc R . . H26B H 0.0904 0.2253 0.2427 0.062 Uiso 1 1 calc R . . H26C H 0.0302 0.2734 0.2331 0.062 Uiso 1 1 calc R . . C27 C 0.2987(2) 0.2698(3) 0.2884(2) 0.0282(12) Uani 1 1 d . . . C28 C 0.2973(3) 0.3515(3) 0.2862(2) 0.0390(14) Uani 1 1 d . . . H28A H 0.3224 0.3709 0.3176 0.047 Uiso 1 1 calc R . . H28B H 0.2546 0.3682 0.2903 0.047 Uiso 1 1 calc R . . H28C H 0.3139 0.3679 0.2493 0.047 Uiso 1 1 calc R . . C29 C 0.3637(2) 0.2400(3) 0.2835(3) 0.0437(15) Uani 1 1 d . . . H29A H 0.3894 0.2603 0.3140 0.052 Uiso 1 1 calc R . . H29B H 0.3810 0.2529 0.2460 0.052 Uiso 1 1 calc R . . H29C H 0.3625 0.1877 0.2873 0.052 Uiso 1 1 calc R . . C30 C 0.2593(3) 0.2380(3) 0.2400(2) 0.0398(14) Uani 1 1 d . . . H30A H 0.2174 0.2577 0.2422 0.048 Uiso 1 1 calc R . . H30B H 0.2576 0.1857 0.2441 0.048 Uiso 1 1 calc R . . H30C H 0.2776 0.2502 0.2028 0.048 Uiso 1 1 calc R . . C31 C 0.2563(2) 0.2908(3) 0.5307(2) 0.0257(11) Uani 1 1 d . . . C32 C 0.2425(2) 0.2185(3) 0.5256(2) 0.0316(12) Uani 1 1 d . . . C33 C 0.2046(2) 0.1805(3) 0.5611(2) 0.0346(13) Uani 1 1 d . . . C34 C 0.1726(2) 0.2161(3) 0.6035(2) 0.0392(14) Uani 1 1 d . . . C35 C 0.1801(2) 0.2890(3) 0.6089(2) 0.0353(12) Uani 1 1 d . . . C36 C 0.2211(2) 0.3240(3) 0.5735(2) 0.0311(12) Uani 1 1 d . . . C41 C 0.3686(2) 0.2815(3) 0.4736(2) 0.0287(11) Uani 1 1 d . . . C42 C 0.3910(2) 0.2246(3) 0.5064(2) 0.0316(12) Uani 1 1 d . . . C43 C 0.4440(3) 0.1869(3) 0.4947(3) 0.0391(14) Uani 1 1 d . . . C44 C 0.4805(3) 0.2063(3) 0.4496(3) 0.0428(15) Uani 1 1 d . . . C45 C 0.4626(3) 0.2628(3) 0.4168(2) 0.0406(14) Uani 1 1 d . . . C46 C 0.4086(2) 0.2987(3) 0.4295(2) 0.0338(13) Uani 1 1 d . . . C51 C 0.3453(2) 0.3965(3) 0.5281(2) 0.0280(11) Uani 1 1 d . . . C52 C 0.3733(2) 0.4568(3) 0.5041(3) 0.0360(13) Uani 1 1 d . . . C53 C 0.4142(3) 0.5013(3) 0.5325(3) 0.0490(16) Uani 1 1 d . . . C54 C 0.4279(3) 0.4892(3) 0.5885(3) 0.0483(16) Uani 1 1 d . . . C55 C 0.4013(3) 0.4312(3) 0.6160(3) 0.0433(15) Uani 1 1 d . . . C56 C 0.3627(2) 0.3874(3) 0.5850(2) 0.0336(13) Uani 1 1 d . . . B B 0.3081(2) 0.3334(3) 0.4910(2) 0.0263(12) Uani 1 1 d . . . C10S C -0.0234(4) 0.4075(4) 0.6831(3) 0.074(2) Uani 1 1 d . . . H10C H -0.0548 0.4106 0.6529 0.088 Uiso 1 1 calc R . . H10D H -0.0436 0.4036 0.7206 0.088 Uiso 1 1 calc R . . H10E H 0.0024 0.3650 0.6766 0.088 Uiso 1 1 calc R . . C11S C 0.0157(3) 0.4729(4) 0.6818(3) 0.0508(16) Uani 1 1 d . . . C12S C 0.0519(3) 0.4882(4) 0.6342(3) 0.0634(19) Uani 1 1 d . . . H12S H 0.0525 0.4561 0.6025 0.076 Uiso 1 1 calc R . . C13S C 0.0869(4) 0.5495(4) 0.6328(3) 0.071(2) Uani 1 1 d . . . H13S H 0.1121 0.5590 0.6003 0.086 Uiso 1 1 calc R . . C14S C 0.0860(4) 0.5971(4) 0.6772(4) 0.071(2) Uani 1 1 d . . . H14S H 0.1091 0.6403 0.6752 0.086 Uiso 1 1 calc R . . C15S C 0.0514(3) 0.5818(4) 0.7249(3) 0.063(2) Uani 1 1 d . . . H15S H 0.0514 0.6139 0.7566 0.076 Uiso 1 1 calc R . . C16S C 0.0165(3) 0.5199(4) 0.7273(3) 0.0572(18) Uani 1 1 d . . . H16S H -0.0071 0.5096 0.7606 0.069 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 0.02798(9) 0.02364(10) 0.02695(10) -0.00255(9) -0.00085(9) -0.00135(9) P 0.0239(6) 0.0277(7) 0.0278(7) -0.0024(6) -0.0020(5) -0.0011(6) S 0.0266(6) 0.0242(7) 0.0258(7) -0.0030(5) 0.0010(5) 0.0015(5) F32 0.0410(17) 0.0326(18) 0.0361(18) -0.0030(14) 0.0031(14) -0.0010(13) F33 0.058(2) 0.0370(19) 0.058(2) 0.0061(16) 0.0052(18) -0.0150(16) F34 0.052(2) 0.070(3) 0.046(2) 0.0155(18) 0.0127(17) -0.0132(18) F35 0.0480(19) 0.066(2) 0.0328(19) -0.0049(17) 0.0123(15) 0.0032(17) F36 0.0451(18) 0.0340(18) 0.0391(19) -0.0087(14) 0.0069(15) 0.0016(14) F42 0.0390(18) 0.045(2) 0.044(2) 0.0123(16) -0.0056(15) 0.0053(15) F43 0.0435(19) 0.0371(19) 0.081(3) -0.0009(19) -0.0209(19) 0.0116(16) F44 0.0363(19) 0.079(3) 0.080(3) -0.027(2) -0.0037(18) 0.0245(19) F45 0.0363(19) 0.104(3) 0.052(2) -0.003(2) 0.0135(18) 0.003(2) F46 0.0348(17) 0.063(2) 0.046(2) 0.0142(17) 0.0097(15) 0.0002(16) F52 0.0478(19) 0.039(2) 0.052(2) 0.0119(16) -0.0111(17) -0.0130(15) F53 0.059(2) 0.036(2) 0.110(3) 0.012(2) -0.022(2) -0.0191(18) F54 0.076(3) 0.060(3) 0.103(3) -0.025(2) -0.039(3) -0.017(2) F55 0.059(2) 0.083(3) 0.043(2) -0.020(2) -0.0182(18) 0.002(2) F56 0.0500(18) 0.057(2) 0.0303(18) 0.0057(16) -0.0092(15) -0.0066(17) C1 0.026(3) 0.026(3) 0.021(3) 0.003(2) 0.001(2) -0.002(2) C2 0.020(2) 0.026(3) 0.022(3) 0.000(2) 0.001(2) 0.003(2) C3 0.027(3) 0.023(3) 0.023(3) 0.0007(19) -0.003(2) -0.004(2) C3A 0.029(2) 0.022(3) 0.026(3) 0.003(2) 0.001(2) 0.000(2) C4 0.027(3) 0.035(3) 0.039(3) 0.000(3) -0.001(2) -0.003(2) C5 0.036(3) 0.032(3) 0.046(4) -0.003(3) 0.005(3) 0.009(3) C6 0.045(3) 0.026(3) 0.043(4) -0.009(3) 0.004(3) 0.004(2) C7 0.037(3) 0.024(3) 0.028(3) -0.001(2) 0.000(2) -0.004(2) C7A 0.026(3) 0.025(3) 0.025(3) 0.001(2) 0.000(2) -0.001(2) C10 0.038(3) 0.028(3) 0.052(4) -0.002(3) -0.008(3) -0.010(2) C11 0.047(3) 0.019(3) 0.040(3) -0.004(2) -0.005(3) -0.001(3) C12 0.040(3) 0.021(3) 0.039(3) 0.007(2) 0.001(3) -0.002(2) C13 0.044(3) 0.034(3) 0.054(4) 0.008(3) 0.002(3) 0.004(3) C14 0.058(4) 0.030(3) 0.060(4) 0.006(3) 0.026(3) 0.011(3) C15 0.084(5) 0.032(3) 0.034(4) -0.001(3) 0.006(4) 0.008(3) C16 0.065(4) 0.025(3) 0.046(4) -0.003(3) -0.009(3) 0.004(3) C21 0.026(3) 0.033(3) 0.034(3) -0.005(2) 0.005(2) -0.001(2) C22 0.044(3) 0.047(4) 0.034(3) 0.005(3) 0.011(3) -0.003(3) C23 0.035(3) 0.050(4) 0.056(4) -0.010(3) 0.007(3) -0.014(3) C24 0.027(3) 0.039(3) 0.036(3) -0.007(3) -0.006(2) 0.005(2) C25 0.042(3) 0.044(4) 0.040(4) 0.011(3) -0.002(3) 0.007(3) C26 0.059(4) 0.056(4) 0.040(4) -0.004(3) -0.024(3) 0.002(3) C27 0.026(3) 0.027(3) 0.031(3) -0.001(2) 0.007(2) -0.002(2) C28 0.043(3) 0.037(4) 0.037(3) 0.005(3) 0.007(3) -0.003(2) C29 0.041(3) 0.051(4) 0.039(4) 0.002(3) 0.012(3) 0.006(3) C30 0.048(3) 0.045(4) 0.025(3) 0.000(3) -0.003(3) -0.002(3) C31 0.026(2) 0.028(3) 0.023(3) 0.001(2) -0.001(2) -0.002(2) C32 0.033(3) 0.033(3) 0.028(3) 0.002(2) -0.005(2) -0.002(2) C33 0.037(3) 0.032(3) 0.035(3) 0.004(2) -0.005(3) -0.008(2) C34 0.036(3) 0.053(4) 0.029(3) 0.011(3) 0.002(3) -0.007(3) C35 0.032(3) 0.053(4) 0.022(3) 0.004(2) 0.000(3) 0.005(3) C36 0.032(3) 0.034(3) 0.028(3) 0.000(2) 0.002(2) -0.002(2) C41 0.026(3) 0.030(3) 0.030(3) -0.006(2) -0.004(2) -0.004(2) C42 0.028(3) 0.033(3) 0.033(3) -0.004(2) -0.004(2) 0.001(2) C43 0.035(3) 0.034(3) 0.049(4) -0.013(3) -0.013(3) 0.003(2) C44 0.036(3) 0.045(4) 0.048(4) -0.024(3) -0.010(3) 0.013(3) C45 0.035(3) 0.052(4) 0.035(4) -0.012(3) 0.005(3) -0.005(3) C46 0.028(3) 0.042(3) 0.032(3) -0.003(3) -0.006(2) 0.002(2) C51 0.027(2) 0.023(3) 0.034(3) -0.004(2) -0.002(2) 0.002(2) C52 0.031(3) 0.034(3) 0.043(4) -0.001(3) -0.010(3) 0.004(2) C53 0.034(3) 0.031(3) 0.081(5) -0.001(3) -0.011(3) -0.007(3) C54 0.040(3) 0.037(4) 0.068(5) -0.019(3) -0.020(3) -0.002(3) C55 0.043(3) 0.048(4) 0.039(4) -0.016(3) -0.014(3) 0.012(3) C56 0.030(3) 0.032(3) 0.039(3) -0.006(3) 0.000(2) 0.000(2) B 0.030(3) 0.022(3) 0.026(3) 0.004(2) -0.001(2) 0.000(3) C10S 0.091(6) 0.057(5) 0.073(5) 0.011(4) 0.006(4) -0.015(4) C11S 0.053(4) 0.054(4) 0.046(4) 0.007(3) -0.011(3) 0.005(3) C12S 0.083(5) 0.063(5) 0.045(4) 0.000(4) -0.006(4) -0.010(4) C13S 0.082(5) 0.073(5) 0.059(5) 0.016(4) -0.013(4) -0.017(5) C14S 0.072(5) 0.061(5) 0.081(6) 0.013(4) -0.025(5) -0.010(4) C15S 0.061(4) 0.057(5) 0.071(5) -0.012(4) -0.023(4) 0.012(4) C16S 0.046(4) 0.060(5) 0.066(5) -0.004(4) -0.008(3) 0.018(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 C10 2.085(5) . ? Pt P 2.2254(13) . ? Pt C11 2.255(5) . ? Pt C12 2.354(5) . ? Pt S 2.3658(12) . ? P C3 1.817(5) . ? P C24 1.848(5) . ? P C21 1.849(5) . ? S C2 1.785(5) . ? S C27 1.910(5) . ? F32 C32 1.369(6) . ? F33 C33 1.351(6) . ? F34 C34 1.345(6) . ? F35 C35 1.341(6) . ? F36 C36 1.355(6) . ? F42 C42 1.353(6) . ? F43 C43 1.355(6) . ? F44 C44 1.353(6) . ? F45 C45 1.353(6) . ? F46 C46 1.354(6) . ? F52 C52 1.360(6) . ? F53 C53 1.343(7) . ? F54 C54 1.345(6) . ? F55 C55 1.336(7) . ? F56 C56 1.361(6) . ? C1 C2 1.513(6) . ? C1 C7A 1.517(6) . ? C1 B 1.701(7) . ? C2 C3 1.354(6) . ? C3 C3A 1.458(6) . ? C3A C4 1.392(7) . ? C3A C7A 1.402(7) . ? C4 C5 1.370(7) . ? C5 C6 1.383(7) . ? C6 C7 1.381(7) . ? C7 C7A 1.390(7) . ? C10 C11 1.451(8) . ? C11 C12 1.416(7) . ? C11 C16 1.424(8) . ? C12 C13 1.408(7) . ? C13 C14 1.361(8) . ? C14 C15 1.397(9) . ? C15 C16 1.355(8) . ? C21 C23 1.507(7) . ? C21 C22 1.508(7) . ? C24 C26 1.522(7) . ? C24 C25 1.528(7) . ? C27 C29 1.517(7) . ? C27 C28 1.523(7) . ? C27 C30 1.533(7) . ? C31 C32 1.385(7) . ? C31 C36 1.398(7) . ? C31 B 1.658(7) . ? C32 C33 1.363(7) . ? C33 C34 1.377(8) . ? C34 C35 1.374(8) . ? C35 C36 1.376(7) . ? C41 C46 1.380(7) . ? C41 C42 1.394(7) . ? C41 B 1.678(7) . ? C42 C43 1.375(7) . ? C43 C44 1.362(8) . ? C44 C45 1.357(8) . ? C45 C46 1.381(7) . ? C51 C56 1.387(7) . ? C51 C52 1.395(7) . ? C51 B 1.668(7) . ? C52 C53 1.382(8) . ? C53 C54 1.356(9) . ? C54 C55 1.380(9) . ? C55 C56 1.373(7) . ? C10S C11S 1.486(9) . ? C11S C16S 1.373(9) . ? C11S C12S 1.386(9) . ? C12S C13S 1.371(10) . ? C13S C14S 1.361(11) . ? C14S C15S 1.370(10) . ? C15S C16S 1.379(9) . ? 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 C10 Pt P 104.42(16) . . ? C10 Pt C11 38.8(2) . . ? P Pt C11 141.31(15) . . ? C10 Pt C12 66.4(2) . . ? P Pt C12 163.64(14) . . ? C11 Pt C12 35.69(18) . . ? C10 Pt S 165.89(16) . . ? P Pt S 89.34(5) . . ? C11 Pt S 128.37(15) . . ? C12 Pt S 99.45(13) . . ? C3 P C24 108.2(2) . . ? C3 P C21 103.5(2) . . ? C24 P C21 104.4(2) . . ? C3 P Pt 104.28(16) . . ? C24 P Pt 119.48(18) . . ? C21 P Pt 115.70(18) . . ? C2 S C27 107.0(2) . . ? C2 S Pt 101.26(15) . . ? C27 S Pt 107.24(16) . . ? C2 C1 C7A 100.1(4) . . ? C2 C1 B 116.0(4) . . ? C7A C1 B 114.2(4) . . ? C3 C2 C1 112.3(4) . . ? C3 C2 S 121.5(4) . . ? C1 C2 S 126.3(3) . . ? C2 C3 C3A 108.9(4) . . ? C2 C3 P 121.1(4) . . ? C3A C3 P 129.9(4) . . ? C4 C3A C7A 121.3(5) . . ? C4 C3A C3 131.0(5) . . ? C7A C3A C3 107.6(4) . . ? C5 C4 C3A 118.7(5) . . ? C4 C5 C6 120.6(5) . . ? C7 C6 C5 121.2(5) . . ? C6 C7 C7A 119.4(5) . . ? C7 C7A C3A 118.8(4) . . ? C7 C7A C1 130.3(4) . . ? C3A C7A C1 110.8(4) . . ? C11 C10 Pt 76.9(3) . . ? C12 C11 C16 118.3(5) . . ? C12 C11 C10 116.8(5) . . ? C16 C11 C10 123.2(5) . . ? C12 C11 Pt 76.0(3) . . ? C16 C11 Pt 118.1(4) . . ? C10 C11 Pt 64.3(3) . . ? C13 C12 C11 119.6(5) . . ? C13 C12 Pt 124.5(4) . . ? C11 C12 Pt 68.3(3) . . ? C14 C13 C12 120.6(6) . . ? C13 C14 C15 119.9(6) . . ? C16 C15 C14 121.7(6) . . ? C15 C16 C11 119.9(6) . . ? C23 C21 C22 112.8(5) . . ? C23 C21 P 112.9(4) . . ? C22 C21 P 108.4(3) . . ? C26 C24 C25 111.1(5) . . ? C26 C24 P 111.4(4) . . ? C25 C24 P 112.5(4) . . ? C29 C27 C28 112.5(4) . . ? C29 C27 C30 108.7(4) . . ? C28 C27 C30 110.5(4) . . ? C29 C27 S 104.4(4) . . ? C28 C27 S 111.1(4) . . ? C30 C27 S 109.5(3) . . ? C32 C31 C36 112.0(5) . . ? C32 C31 B 124.3(5) . . ? C36 C31 B 123.7(4) . . ? C33 C32 F32 114.8(5) . . ? C33 C32 C31 125.6(5) . . ? F32 C32 C31 119.6(5) . . ? F33 C33 C32 121.5(5) . . ? F33 C33 C34 119.2(5) . . ? C32 C33 C34 119.2(5) . . ? F34 C34 C35 120.5(5) . . ? F34 C34 C33 120.6(5) . . ? C35 C34 C33 118.9(5) . . ? F35 C35 C34 119.9(5) . . ? F35 C35 C36 120.7(5) . . ? C34 C35 C36 119.3(5) . . ? F36 C36 C35 115.6(5) . . ? F36 C36 C31 119.8(4) . . ? C35 C36 C31 124.6(5) . . ? C46 C41 C42 111.5(5) . . ? C46 C41 B 122.4(5) . . ? C42 C41 B 125.2(5) . . ? F42 C42 C43 113.8(5) . . ? F42 C42 C41 121.4(5) . . ? C43 C42 C41 124.7(5) . . ? F43 C43 C44 119.2(5) . . ? F43 C43 C42 120.5(5) . . ? C44 C43 C42 120.2(6) . . ? F44 C44 C45 121.2(6) . . ? F44 C44 C43 120.6(6) . . ? C45 C44 C43 118.2(5) . . ? F45 C45 C44 120.1(5) . . ? F45 C45 C46 120.0(6) . . ? C44 C45 C46 119.9(5) . . ? F46 C46 C41 120.5(5) . . ? F46 C46 C45 114.2(5) . . ? C41 C46 C45 125.3(5) . . ? C56 C51 C52 111.3(5) . . ? C56 C51 B 122.7(4) . . ? C52 C51 B 124.8(5) . . ? F52 C52 C53 114.5(5) . . ? F52 C52 C51 120.7(5) . . ? C53 C52 C51 124.8(6) . . ? F53 C53 C54 120.1(5) . . ? F53 C53 C52 119.9(6) . . ? C54 C53 C52 120.0(6) . . ? F54 C54 C53 121.4(6) . . ? F54 C54 C55 119.6(6) . . ? C53 C54 C55 119.0(5) . . ? F55 C55 C56 121.7(6) . . ? F55 C55 C54 119.8(5) . . ? C56 C55 C54 118.5(6) . . ? F56 C56 C55 113.7(5) . . ? F56 C56 C51 119.8(5) . . ? C55 C56 C51 126.4(6) . . ? C31 B C51 112.1(4) . . ? C31 B C41 112.9(4) . . ? C51 B C41 98.8(4) . . ? C31 B C1 105.9(4) . . ? C51 B C1 114.1(4) . . ? C41 B C1 113.3(4) . . ? C16S C11S C12S 118.5(7) . . ? C16S C11S C10S 121.0(7) . . ? C12S C11S C10S 120.5(7) . . ? C13S C12S C11S 120.2(7) . . ? C14S C13S C12S 121.0(8) . . ? C13S C14S C15S 119.2(8) . . ? C14S C15S C16S 120.4(7) . . ? C11S C16S C15S 120.6(7) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C10 Pt P C3 165.0(2) . . . . ? C11 Pt P C3 -179.9(3) . . . . ? C12 Pt P C3 111.1(5) . . . . ? S Pt P C3 -11.78(16) . . . . ? C10 Pt P C24 -74.0(3) . . . . ? C11 Pt P C24 -58.9(3) . . . . ? C12 Pt P C24 -127.9(5) . . . . ? S Pt P C24 109.2(2) . . . . ? C10 Pt P C21 52.1(3) . . . . ? C11 Pt P C21 67.1(3) . . . . ? C12 Pt P C21 -1.8(5) . . . . ? S Pt P C21 -124.74(19) . . . . ? C10 Pt S C2 -153.4(7) . . . . ? P Pt S C2 13.82(16) . . . . ? C11 Pt S C2 -175.6(2) . . . . ? C12 Pt S C2 -152.3(2) . . . . ? C10 Pt S C27 94.7(7) . . . . ? P Pt S C27 -98.09(16) . . . . ? C11 Pt S C27 72.5(2) . . . . ? C12 Pt S C27 95.8(2) . . . . ? C7A C1 C2 C3 -5.8(5) . . . . ? B C1 C2 C3 117.6(5) . . . . ? C7A C1 C2 S 176.1(4) . . . . ? B C1 C2 S -60.5(5) . . . . ? C27 S C2 C3 97.8(4) . . . . ? Pt S C2 C3 -14.3(4) . . . . ? C27 S C2 C1 -84.2(4) . . . . ? Pt S C2 C1 163.6(4) . . . . ? C1 C2 C3 C3A 5.7(6) . . . . ? S C2 C3 C3A -176.1(3) . . . . ? C1 C2 C3 P -172.5(3) . . . . ? S C2 C3 P 5.7(6) . . . . ? C24 P C3 C2 -121.2(4) . . . . ? C21 P C3 C2 128.4(4) . . . . ? Pt P C3 C2 7.0(4) . . . . ? C24 P C3 C3A 61.1(5) . . . . ? C21 P C3 C3A -49.3(5) . . . . ? Pt P C3 C3A -170.7(4) . . . . ? C2 C3 C3A C4 173.4(5) . . . . ? P C3 C3A C4 -8.7(8) . . . . ? C2 C3 C3A C7A -2.9(6) . . . . ? P C3 C3A C7A 175.0(4) . . . . ? C7A C3A C4 C5 0.1(8) . . . . ? C3 C3A C4 C5 -175.8(5) . . . . ? C3A C4 C5 C6 -0.3(8) . . . . ? C4 C5 C6 C7 0.2(9) . . . . ? C5 C6 C7 C7A 0.2(8) . . . . ? C6 C7 C7A C3A -0.4(7) . . . . ? C6 C7 C7A C1 177.0(5) . . . . ? C4 C3A C7A C7 0.3(7) . . . . ? C3 C3A C7A C7 177.0(4) . . . . ? C4 C3A C7A C1 -177.6(5) . . . . ? C3 C3A C7A C1 -0.9(5) . . . . ? C2 C1 C7A C7 -173.8(5) . . . . ? B C1 C7A C7 61.5(7) . . . . ? C2 C1 C7A C3A 3.8(5) . . . . ? B C1 C7A C3A -120.9(5) . . . . ? P Pt C10 C11 165.0(3) . . . . ? C12 Pt C10 C11 -29.4(3) . . . . ? S Pt C10 C11 -28.2(9) . . . . ? Pt C10 C11 C12 57.0(4) . . . . ? Pt C10 C11 C16 -108.0(5) . . . . ? C10 Pt C11 C12 -129.5(5) . . . . ? P Pt C11 C12 -153.2(3) . . . . ? S Pt C11 C12 42.0(4) . . . . ? C10 Pt C11 C16 115.6(6) . . . . ? P Pt C11 C16 91.9(5) . . . . ? C12 Pt C11 C16 -114.9(6) . . . . ? S Pt C11 C16 -72.9(5) . . . . ? P Pt C11 C10 -23.7(4) . . . . ? C12 Pt C11 C10 129.5(5) . . . . ? S Pt C11 C10 171.5(3) . . . . ? C16 C11 C12 C13 -3.7(7) . . . . ? C10 C11 C12 C13 -169.5(5) . . . . ? Pt C11 C12 C13 -118.3(5) . . . . ? C16 C11 C12 Pt 114.6(5) . . . . ? C10 C11 C12 Pt -51.1(4) . . . . ? C10 Pt C12 C13 143.6(6) . . . . ? P Pt C12 C13 -157.8(4) . . . . ? C11 Pt C12 C13 111.8(6) . . . . ? S Pt C12 C13 -36.1(5) . . . . ? C10 Pt C12 C11 31.8(3) . . . . ? P Pt C12 C11 90.4(6) . . . . ? S Pt C12 C11 -147.9(3) . . . . ? C11 C12 C13 C14 2.0(8) . . . . ? Pt C12 C13 C14 -80.7(7) . . . . ? C12 C13 C14 C15 -0.2(9) . . . . ? C13 C14 C15 C16 0.2(9) . . . . ? C14 C15 C16 C11 -2.0(9) . . . . ? C12 C11 C16 C15 3.7(8) . . . . ? C10 C11 C16 C15 168.5(5) . . . . ? Pt C11 C16 C15 92.3(6) . . . . ? C3 P C21 C23 175.9(4) . . . . ? C24 P C21 C23 62.7(5) . . . . ? Pt P C21 C23 -70.7(4) . . . . ? C3 P C21 C22 -58.4(4) . . . . ? C24 P C21 C22 -171.6(4) . . . . ? Pt P C21 C22 55.0(4) . . . . ? C3 P C24 C26 156.0(4) . . . . ? C21 P C24 C26 -94.2(4) . . . . ? Pt P C24 C26 37.0(5) . . . . ? C3 P C24 C25 30.4(5) . . . . ? C21 P C24 C25 140.2(4) . . . . ? Pt P C24 C25 -88.6(4) . . . . ? C2 S C27 C29 133.0(4) . . . . ? Pt S C27 C29 -119.1(3) . . . . ? C2 S C27 C28 11.5(4) . . . . ? Pt S C27 C28 119.5(3) . . . . ? C2 S C27 C30 -110.8(4) . . . . ? Pt S C27 C30 -2.8(4) . . . . ? C36 C31 C32 C33 -6.7(8) . . . . ? B C31 C32 C33 173.3(5) . . . . ? C36 C31 C32 F32 174.6(4) . . . . ? B C31 C32 F32 -5.4(7) . . . . ? F32 C32 C33 F33 0.8(7) . . . . ? C31 C32 C33 F33 -177.9(5) . . . . ? F32 C32 C33 C34 -175.8(5) . . . . ? C31 C32 C33 C34 5.4(8) . . . . ? F33 C33 C34 F34 1.1(8) . . . . ? C32 C33 C34 F34 177.8(5) . . . . ? F33 C33 C34 C35 -177.0(5) . . . . ? C32 C33 C34 C35 -0.3(8) . . . . ? F34 C34 C35 F35 0.8(8) . . . . ? C33 C34 C35 F35 178.9(5) . . . . ? F34 C34 C35 C36 179.2(5) . . . . ? C33 C34 C35 C36 -2.6(8) . . . . ? F35 C35 C36 F36 1.6(7) . . . . ? C34 C35 C36 F36 -176.9(5) . . . . ? F35 C35 C36 C31 179.4(5) . . . . ? C34 C35 C36 C31 0.9(8) . . . . ? C32 C31 C36 F36 -178.9(4) . . . . ? B C31 C36 F36 1.1(7) . . . . ? C32 C31 C36 C35 3.4(7) . . . . ? B C31 C36 C35 -176.6(5) . . . . ? C46 C41 C42 F42 174.9(4) . . . . ? B C41 C42 F42 5.4(7) . . . . ? C46 C41 C42 C43 -3.9(7) . . . . ? B C41 C42 C43 -173.4(5) . . . . ? F42 C42 C43 F43 2.7(7) . . . . ? C41 C42 C43 F43 -178.4(5) . . . . ? F42 C42 C43 C44 -175.9(5) . . . . ? C41 C42 C43 C44 2.9(8) . . . . ? F43 C43 C44 F44 -0.1(8) . . . . ? C42 C43 C44 F44 178.5(5) . . . . ? F43 C43 C44 C45 -179.2(5) . . . . ? C42 C43 C44 C45 -0.6(8) . . . . ? F44 C44 C45 F45 -0.5(8) . . . . ? C43 C44 C45 F45 178.6(5) . . . . ? F44 C44 C45 C46 -179.5(5) . . . . ? C43 C44 C45 C46 -0.4(8) . . . . ? C42 C41 C46 F46 -176.0(4) . . . . ? B C41 C46 F46 -6.2(7) . . . . ? C42 C41 C46 C45 2.9(8) . . . . ? B C41 C46 C45 172.7(5) . . . . ? F45 C45 C46 F46 -0.9(7) . . . . ? C44 C45 C46 F46 178.0(5) . . . . ? F45 C45 C46 C41 -179.9(5) . . . . ? C44 C45 C46 C41 -1.0(9) . . . . ? C56 C51 C52 F52 -178.4(5) . . . . ? B C51 C52 F52 13.8(8) . . . . ? C56 C51 C52 C53 1.3(8) . . . . ? B C51 C52 C53 -166.5(5) . . . . ? F52 C52 C53 F53 -3.0(8) . . . . ? C51 C52 C53 F53 177.2(5) . . . . ? F52 C52 C53 C54 177.2(5) . . . . ? C51 C52 C53 C54 -2.5(9) . . . . ? F53 C53 C54 F54 0.0(9) . . . . ? C52 C53 C54 F54 179.8(5) . . . . ? F53 C53 C54 C55 -178.5(5) . . . . ? C52 C53 C54 C55 1.2(9) . . . . ? F54 C54 C55 F55 -0.4(8) . . . . ? C53 C54 C55 F55 178.2(5) . . . . ? F54 C54 C55 C56 -177.6(5) . . . . ? C53 C54 C55 C56 1.0(9) . . . . ? F55 C55 C56 F56 -1.1(8) . . . . ? C54 C55 C56 F56 176.0(5) . . . . ? F55 C55 C56 C51 -179.4(5) . . . . ? C54 C55 C56 C51 -2.3(9) . . . . ? C52 C51 C56 F56 -177.1(4) . . . . ? B C51 C56 F56 -9.0(7) . . . . ? C52 C51 C56 C55 1.1(8) . . . . ? B C51 C56 C55 169.2(5) . . . . ? C32 C31 B C51 -144.4(5) . . . . ? C36 C31 B C51 35.6(6) . . . . ? C32 C31 B C41 -33.9(7) . . . . ? C36 C31 B C41 146.1(5) . . . . ? C32 C31 B C1 90.6(6) . . . . ? C36 C31 B C1 -89.4(5) . . . . ? C56 C51 B C31 38.5(6) . . . . ? C52 C51 B C31 -155.0(5) . . . . ? C56 C51 B C41 -80.7(5) . . . . ? C52 C51 B C41 85.8(5) . . . . ? C56 C51 B C1 158.8(5) . . . . ? C52 C51 B C1 -34.7(7) . . . . ? C46 C41 B C31 162.7(5) . . . . ? C42 C41 B C31 -28.9(7) . . . . ? C46 C41 B C51 -78.7(5) . . . . ? C42 C41 B C51 89.7(5) . . . . ? C46 C41 B C1 42.4(6) . . . . ? C42 C41 B C1 -149.3(5) . . . . ? C2 C1 B C31 -57.3(5) . . . . ? C7A C1 B C31 58.4(5) . . . . ? C2 C1 B C51 179.0(4) . . . . ? C7A C1 B C51 -65.3(5) . . . . ? C2 C1 B C41 67.0(5) . . . . ? C7A C1 B C41 -177.3(4) . . . . ? C16S C11S C12S C13S -1.0(10) . . . . ? C10S C11S C12S C13S 178.6(7) . . . . ? C11S C12S C13S C14S -1.2(12) . . . . ? C12S C13S C14S C15S 2.6(12) . . . . ? C13S C14S C15S C16S -1.8(11) . . . . ? C12S C11S C16S C15S 1.7(10) . . . . ? C10S C11S C16S C15S -177.9(6) . . . . ? C14S C15S C16S C11S -0.3(10) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.539 _refine_diff_density_min -0.681 _refine_diff_density_rms 0.122 # Attachment 'DAL0802.CIF' data_dal0802 _database_code_depnum_ccdc_archive 'CCDC 687092' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H36 P Pt S, C24 B F20' _chemical_formula_sum 'C50 H36 B F20 P Pt S' _chemical_formula_weight 1285.72 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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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 P2(1)/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 17.6907(18) _cell_length_b 17.3368(18) _cell_length_c 17.7636(18) _cell_angle_alpha 90.00 _cell_angle_beta 117.9280(10) _cell_angle_gamma 90.00 _cell_volume 4813.6(9) _cell_formula_units_Z 4 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 6055 _cell_measurement_theta_min 2.29 _cell_measurement_theta_max 27.29 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.29 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.774 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2520 _exptl_absorpt_coefficient_mu 3.106 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.4272 _exptl_absorpt_correction_T_max 0.6883 _exptl_absorpt_process_details 'Bruker SHELXTL (Bruker, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker PLATFORM diffractometer/SMART 1000 CCD area detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 8.192 _diffrn_standards_number 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 39940 _diffrn_reflns_av_R_equivalents 0.0431 _diffrn_reflns_av_sigmaI/netI 0.0393 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.75 _diffrn_reflns_theta_max 27.53 _reflns_number_total 11034 _reflns_number_gt 9086 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART (Bruker, 1997)' _computing_cell_refinement 'Bruker SAINT (Bruker, 1997)' _computing_data_reduction 'Bruker SAINT (Bruker, 1997)' _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL (Bruker, 1997)' _computing_publication_material 'Bruker SHELXTL (Bruker, 1997)' _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^)+(0.0517P)^2^+3.6180P] 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 11034 _refine_ls_number_parameters 667 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0491 _refine_ls_R_factor_gt 0.0367 _refine_ls_wR_factor_ref 0.0934 _refine_ls_wR_factor_gt 0.0869 _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_restrained_S_all 1.058 _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 0.311817(9) 0.138183(8) 0.135771(9) 0.02606(6) Uani 1 1 d . . . S S 0.16626(6) 0.16381(6) 0.09301(6) 0.0302(2) Uani 1 1 d . . . P P 0.27130(6) 0.04118(5) 0.04430(6) 0.02478(19) Uani 1 1 d . . . C1 C 0.0182(2) 0.0946(2) -0.0518(3) 0.0354(9) Uani 1 1 d . . . H1A H -0.0054 0.1407 -0.0883 0.042 Uiso 1 1 calc R . . H1B H -0.0120 0.0869 -0.0175 0.042 Uiso 1 1 calc R . . C2 C 0.1133(2) 0.1017(2) 0.0040(2) 0.0277(7) Uani 1 1 d . . . C3 C 0.1563(2) 0.0454(2) -0.0121(2) 0.0258(7) Uani 1 1 d . . . C3A C 0.0943(2) -0.0058(2) -0.0793(2) 0.0288(8) Uani 1 1 d . . . C4 C 0.1056(3) -0.0729(2) -0.1148(3) 0.0365(9) Uani 1 1 d . . . H4 H 0.1613 -0.0934 -0.0969 0.044 Uiso 1 1 calc R . . C5 C 0.0341(3) -0.1098(3) -0.1770(3) 0.0430(10) Uani 1 1 d . . . H5 H 0.0405 -0.1560 -0.2022 0.052 Uiso 1 1 calc R . . C6 C -0.0468(3) -0.0797(3) -0.2027(3) 0.0436(10) Uani 1 1 d . . . H6 H -0.0952 -0.1058 -0.2452 0.052 Uiso 1 1 calc R . . C7 C -0.0584(3) -0.0125(3) -0.1676(3) 0.0415(10) Uani 1 1 d . . . H7 H -0.1140 0.0084 -0.1869 0.050 Uiso 1 1 calc R . . C7A C 0.0116(2) 0.0237(2) -0.1044(3) 0.0323(8) Uani 1 1 d . . . C10 C 0.4429(3) 0.1280(2) 0.1889(3) 0.0368(9) Uani 1 1 d . . . H10A H 0.4689 0.0874 0.2328 0.044 Uiso 1 1 calc R . . H10B H 0.4663 0.1286 0.1481 0.044 Uiso 1 1 calc R . . C11 C 0.4338(2) 0.2032(2) 0.2204(2) 0.0334(8) Uani 1 1 d . . . C12 C 0.4015(3) 0.2056(3) 0.2791(3) 0.0399(10) Uani 1 1 d . . . H12 H 0.4308 0.1683 0.3271 0.048 Uiso 1 1 calc R . . C13 C 0.3858(3) 0.2767(3) 0.3065(3) 0.0448(11) Uani 1 1 d . . . H13 H 0.3669 0.2780 0.3486 0.054 Uiso 1 1 calc R . . C14 C 0.3973(3) 0.3445(2) 0.2734(3) 0.0417(10) Uani 1 1 d . . . H14 H 0.3867 0.3924 0.2925 0.050 Uiso 1 1 calc R . . C15 C 0.4246(3) 0.3427(3) 0.2118(3) 0.0424(10) Uani 1 1 d . . . H15 H 0.4310 0.3896 0.1877 0.051 Uiso 1 1 calc R . . C16 C 0.4425(3) 0.2737(3) 0.1853(3) 0.0389(9) Uani 1 1 d . . . H16 H 0.4608 0.2734 0.1429 0.047 Uiso 1 1 calc R . . C20 C 0.1322(3) 0.2640(2) 0.0507(3) 0.0392(9) Uani 1 1 d . . . C21 C 0.0413(3) 0.2751(3) 0.0358(4) 0.0588(14) Uani 1 1 d . . . H21A H 0.0216 0.3270 0.0133 0.071 Uiso 1 1 calc R . . H21B H 0.0395 0.2687 0.0898 0.071 Uiso 1 1 calc R . . H21C H 0.0040 0.2367 -0.0053 0.071 Uiso 1 1 calc R . . C22 C 0.1422(4) 0.2768(3) -0.0284(4) 0.0603(14) Uani 1 1 d . . . H22A H 0.1236 0.3292 -0.0498 0.072 Uiso 1 1 calc R . . H22B H 0.1070 0.2393 -0.0721 0.072 Uiso 1 1 calc R . . H22C H 0.2023 0.2702 -0.0144 0.072 Uiso 1 1 calc R . . C23 C 0.1924(3) 0.3148(3) 0.1246(4) 0.0568(14) Uani 1 1 d . . . H23A H 0.1796 0.3692 0.1087 0.068 Uiso 1 1 calc R . . H23B H 0.2517 0.3038 0.1380 0.068 Uiso 1 1 calc R . . H23C H 0.1846 0.3040 0.1747 0.068 Uiso 1 1 calc R . . C24 C 0.2999(2) 0.0466(2) -0.0429(2) 0.0320(8) Uani 1 1 d . . . H24 H 0.2670 0.0052 -0.0847 0.038 Uiso 1 1 calc R . . C25 C 0.3941(3) 0.0325(3) -0.0152(3) 0.0436(10) Uani 1 1 d . . . H25A H 0.4042 0.0359 -0.0648 0.052 Uiso 1 1 calc R . . H25B H 0.4102 -0.0189 0.0103 0.052 Uiso 1 1 calc R . . H25C H 0.4286 0.0715 0.0269 0.052 Uiso 1 1 calc R . . C26 C 0.2699(3) 0.1237(3) -0.0892(3) 0.0475(11) Uani 1 1 d . . . H26A H 0.2846 0.1263 -0.1359 0.057 Uiso 1 1 calc R . . H26B H 0.2982 0.1660 -0.0491 0.057 Uiso 1 1 calc R . . H26C H 0.2078 0.1282 -0.1122 0.057 Uiso 1 1 calc R . . C27 C 0.2972(2) -0.0569(2) 0.0898(3) 0.0306(8) Uani 1 1 d . . . H27 H 0.2916 -0.0929 0.0434 0.037 Uiso 1 1 calc R . . C28 C 0.3882(3) -0.0638(2) 0.1623(3) 0.0390(9) Uani 1 1 d . . . H28A H 0.3987 -0.1170 0.1835 0.047 Uiso 1 1 calc R . . H28B H 0.3956 -0.0287 0.2085 0.047 Uiso 1 1 calc R . . H28C H 0.4289 -0.0501 0.1414 0.047 Uiso 1 1 calc R . . C29 C 0.2340(3) -0.0830(3) 0.1209(3) 0.0507(12) Uani 1 1 d . . . H29A H 0.2494 -0.1348 0.1454 0.061 Uiso 1 1 calc R . . H29B H 0.1761 -0.0838 0.0728 0.061 Uiso 1 1 calc R . . H29C H 0.2360 -0.0470 0.1643 0.061 Uiso 1 1 calc R . . F32 F 0.83541(15) 0.26921(13) -0.02134(15) 0.0383(5) Uani 1 1 d . . . F33 F 0.86102(17) 0.24169(15) -0.15595(17) 0.0485(6) Uani 1 1 d . . . F34 F 0.80107(19) 0.34165(18) -0.28939(17) 0.0540(7) Uani 1 1 d . . . F35 F 0.71139(19) 0.46840(17) -0.28687(17) 0.0545(7) Uani 1 1 d . . . F36 F 0.68732(17) 0.49918(15) -0.15487(16) 0.0471(6) Uani 1 1 d . . . F42 F 0.74851(16) 0.39769(14) 0.16792(15) 0.0399(5) Uani 1 1 d . . . F43 F 0.66146(18) 0.30008(16) 0.21555(17) 0.0502(7) Uani 1 1 d . . . F44 F 0.57515(18) 0.17955(16) 0.11371(19) 0.0525(7) Uani 1 1 d . . . F45 F 0.57180(17) 0.16204(15) -0.03896(18) 0.0484(7) Uani 1 1 d . . . F46 F 0.65468(16) 0.25833(14) -0.08987(15) 0.0424(6) Uani 1 1 d . . . F52 F 0.87835(15) 0.30447(14) 0.16688(16) 0.0436(6) Uani 1 1 d . . . F53 F 1.04249(17) 0.33254(18) 0.26442(19) 0.0584(8) Uani 1 1 d . . . F54 F 1.12073(16) 0.45385(18) 0.2315(2) 0.0601(8) Uani 1 1 d . . . F55 F 1.02745(17) 0.54811(16) 0.0971(2) 0.0586(8) Uani 1 1 d . . . F56 F 0.86111(16) 0.52305(13) -0.00041(16) 0.0429(6) Uani 1 1 d . . . F62 F 0.80084(16) 0.55115(16) 0.11770(18) 0.0507(7) Uani 1 1 d . . . F63 F 0.6933(2) 0.66101(17) 0.1045(2) 0.0714(10) Uani 1 1 d . . . F64 F 0.5240(2) 0.6502(2) -0.0097(2) 0.0760(11) Uani 1 1 d . . . F65 F 0.46729(17) 0.5254(2) -0.11540(19) 0.0683(9) Uani 1 1 d . . . F66 F 0.57573(16) 0.41576(16) -0.10736(16) 0.0484(6) Uani 1 1 d . . . C31 C 0.7589(2) 0.3848(2) -0.0804(2) 0.0298(8) Uani 1 1 d . . . C32 C 0.8034(2) 0.3203(2) -0.0864(2) 0.0305(8) Uani 1 1 d . . . C33 C 0.8179(3) 0.3051(2) -0.1544(3) 0.0357(9) Uani 1 1 d . . . C34 C 0.7874(3) 0.3550(3) -0.2222(3) 0.0398(10) Uani 1 1 d . . . C35 C 0.7426(3) 0.4185(3) -0.2204(3) 0.0408(10) Uani 1 1 d . . . C36 C 0.7292(3) 0.4325(2) -0.1507(3) 0.0360(9) Uani 1 1 d . . . C41 C 0.7095(2) 0.3325(2) 0.0378(2) 0.0273(7) Uani 1 1 d . . . C42 C 0.7066(2) 0.3390(2) 0.1145(2) 0.0298(8) Uani 1 1 d . . . C43 C 0.6627(3) 0.2898(2) 0.1408(3) 0.0339(8) Uani 1 1 d . . . C44 C 0.6183(3) 0.2295(2) 0.0894(3) 0.0361(9) Uani 1 1 d . . . C45 C 0.6175(2) 0.2200(2) 0.0126(3) 0.0334(8) Uani 1 1 d . . . C46 C 0.6622(2) 0.2713(2) -0.0118(2) 0.0309(8) Uani 1 1 d . . . C51 C 0.8589(2) 0.4140(2) 0.0785(2) 0.0281(7) Uani 1 1 d . . . C52 C 0.9103(3) 0.3674(2) 0.1466(3) 0.0326(8) Uani 1 1 d . . . C53 C 0.9967(3) 0.3804(3) 0.1990(3) 0.0388(9) Uani 1 1 d . . . C54 C 1.0364(3) 0.4412(3) 0.1821(3) 0.0416(10) Uani 1 1 d . . . C55 C 0.9897(3) 0.4883(2) 0.1147(3) 0.0398(10) Uani 1 1 d . . . C56 C 0.9034(3) 0.4738(2) 0.0651(3) 0.0342(9) Uani 1 1 d . . . C61 C 0.6953(3) 0.4772(2) 0.0043(2) 0.0311(8) Uani 1 1 d . . . C62 C 0.7198(3) 0.5413(2) 0.0566(3) 0.0369(9) Uani 1 1 d . . . C63 C 0.6639(3) 0.5998(3) 0.0519(3) 0.0465(11) Uani 1 1 d . . . C64 C 0.5794(3) 0.5943(3) -0.0051(3) 0.0511(13) Uani 1 1 d . . . C65 C 0.5507(3) 0.5319(3) -0.0584(3) 0.0487(12) Uani 1 1 d . . . C66 C 0.6083(3) 0.4755(3) -0.0522(3) 0.0373(9) Uani 1 1 d . . . B B 0.7562(3) 0.4015(2) 0.0102(3) 0.0283(8) 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 0.02416(8) 0.02872(8) 0.02635(8) 0.00013(6) 0.01270(6) 0.00094(5) S 0.0277(5) 0.0309(4) 0.0351(5) 0.0008(4) 0.0172(4) 0.0038(4) P 0.0215(4) 0.0285(5) 0.0255(5) 0.0019(4) 0.0120(4) 0.0022(3) C1 0.0232(18) 0.037(2) 0.043(2) 0.0045(18) 0.0128(18) 0.0052(15) C2 0.0209(16) 0.0311(19) 0.032(2) 0.0034(15) 0.0128(16) 0.0002(14) C3 0.0200(16) 0.0303(18) 0.0274(18) 0.0039(14) 0.0115(15) -0.0006(13) C3A 0.0244(18) 0.0335(19) 0.0271(19) 0.0034(15) 0.0111(16) -0.0015(14) C4 0.029(2) 0.042(2) 0.035(2) -0.0016(17) 0.0122(18) -0.0017(16) C5 0.043(2) 0.040(2) 0.043(3) -0.0073(19) 0.017(2) -0.0077(19) C6 0.033(2) 0.052(3) 0.034(2) -0.002(2) 0.0058(19) -0.0126(19) C7 0.025(2) 0.054(3) 0.042(2) 0.007(2) 0.0118(19) -0.0009(18) C7A 0.0228(18) 0.036(2) 0.038(2) 0.0069(17) 0.0141(17) 0.0007(15) C10 0.0267(19) 0.042(2) 0.037(2) -0.0055(17) 0.0116(18) 0.0008(16) C11 0.0234(18) 0.041(2) 0.028(2) -0.0023(16) 0.0057(16) 0.0003(15) C12 0.044(2) 0.041(2) 0.032(2) 0.0025(17) 0.015(2) -0.0002(18) C13 0.058(3) 0.045(2) 0.040(2) -0.0047(19) 0.029(2) -0.002(2) C14 0.045(3) 0.035(2) 0.040(2) -0.0108(18) 0.016(2) -0.0052(18) C15 0.042(2) 0.038(2) 0.045(3) -0.0043(19) 0.019(2) -0.0112(18) C16 0.037(2) 0.045(2) 0.040(2) -0.0024(19) 0.022(2) -0.0068(18) C20 0.039(2) 0.030(2) 0.046(3) 0.0032(18) 0.017(2) 0.0085(17) C21 0.039(3) 0.052(3) 0.072(4) -0.008(3) 0.014(3) 0.019(2) C22 0.087(4) 0.036(2) 0.060(3) 0.012(2) 0.036(3) 0.011(3) C23 0.053(3) 0.032(2) 0.070(4) -0.008(2) 0.016(3) 0.006(2) C24 0.032(2) 0.041(2) 0.028(2) -0.0041(16) 0.0179(17) -0.0035(16) C25 0.034(2) 0.064(3) 0.043(2) -0.002(2) 0.027(2) 0.001(2) C26 0.053(3) 0.057(3) 0.041(3) 0.015(2) 0.030(2) 0.005(2) C27 0.0304(19) 0.0271(18) 0.032(2) 0.0027(15) 0.0125(17) 0.0037(14) C28 0.035(2) 0.038(2) 0.038(2) 0.0037(18) 0.0120(19) 0.0066(17) C29 0.041(2) 0.053(3) 0.058(3) 0.028(2) 0.024(2) 0.005(2) F32 0.0416(13) 0.0352(12) 0.0408(14) 0.0040(10) 0.0215(12) 0.0067(10) F33 0.0505(15) 0.0484(15) 0.0565(17) -0.0108(12) 0.0333(14) 0.0009(12) F34 0.0608(18) 0.0750(19) 0.0399(15) -0.0122(13) 0.0349(15) -0.0147(14) F35 0.0635(18) 0.0659(18) 0.0364(15) 0.0155(13) 0.0254(14) -0.0007(14) F36 0.0607(17) 0.0435(14) 0.0397(14) 0.0158(11) 0.0257(13) 0.0164(12) F42 0.0475(14) 0.0423(13) 0.0289(12) -0.0080(10) 0.0169(11) -0.0068(11) F43 0.0576(17) 0.0657(17) 0.0379(14) -0.0011(12) 0.0311(13) -0.0055(13) F44 0.0535(16) 0.0529(16) 0.0679(19) 0.0018(14) 0.0423(16) -0.0130(13) F45 0.0498(15) 0.0391(13) 0.0632(18) -0.0179(12) 0.0322(15) -0.0164(12) F46 0.0502(15) 0.0459(14) 0.0363(13) -0.0152(11) 0.0247(12) -0.0167(11) F52 0.0365(13) 0.0414(13) 0.0467(15) 0.0161(11) 0.0144(12) 0.0024(10) F53 0.0373(14) 0.0697(18) 0.0474(17) 0.0180(14) 0.0025(13) 0.0112(13) F54 0.0248(13) 0.0706(19) 0.069(2) -0.0076(15) 0.0083(13) -0.0046(12) F55 0.0443(15) 0.0477(16) 0.081(2) 0.0020(15) 0.0265(16) -0.0166(12) F56 0.0424(14) 0.0326(12) 0.0492(15) 0.0087(11) 0.0178(12) -0.0019(10) F62 0.0404(14) 0.0450(15) 0.0554(17) -0.0215(12) 0.0131(13) 0.0006(11) F63 0.093(3) 0.0458(16) 0.090(3) -0.0153(16) 0.056(2) 0.0158(16) F64 0.078(2) 0.085(2) 0.082(2) 0.0264(18) 0.052(2) 0.0542(19) F65 0.0338(15) 0.117(3) 0.0478(17) 0.0225(17) 0.0140(14) 0.0255(16) F66 0.0328(13) 0.0652(17) 0.0333(13) -0.0010(12) 0.0038(11) -0.0045(12) C31 0.0267(18) 0.0341(19) 0.028(2) -0.0010(15) 0.0122(17) -0.0037(15) C32 0.0301(19) 0.033(2) 0.029(2) -0.0007(15) 0.0141(17) -0.0044(15) C33 0.033(2) 0.036(2) 0.039(2) -0.0088(17) 0.0177(19) -0.0070(16) C34 0.040(2) 0.054(3) 0.032(2) -0.0126(19) 0.023(2) -0.0162(19) C35 0.040(2) 0.050(2) 0.030(2) 0.0053(18) 0.0140(19) -0.0090(19) C36 0.037(2) 0.036(2) 0.032(2) 0.0040(17) 0.0140(18) 0.0000(17) C41 0.0244(18) 0.0281(17) 0.0274(19) 0.0002(15) 0.0104(16) 0.0022(14) C42 0.0280(19) 0.0309(18) 0.029(2) -0.0003(15) 0.0126(17) 0.0023(15) C43 0.032(2) 0.042(2) 0.031(2) 0.0049(17) 0.0171(18) 0.0037(16) C44 0.033(2) 0.034(2) 0.051(3) 0.0061(18) 0.028(2) 0.0033(16) C45 0.0278(19) 0.0314(19) 0.043(2) -0.0050(17) 0.0187(18) -0.0022(15) C46 0.0294(19) 0.033(2) 0.031(2) -0.0046(15) 0.0144(17) -0.0015(15) C51 0.0272(18) 0.0271(17) 0.0281(19) -0.0040(15) 0.0114(16) 0.0011(14) C52 0.031(2) 0.032(2) 0.033(2) 0.0021(16) 0.0135(18) 0.0006(15) C53 0.031(2) 0.045(2) 0.032(2) 0.0018(18) 0.0077(18) 0.0090(17) C54 0.0234(19) 0.050(3) 0.043(2) -0.012(2) 0.0085(19) -0.0022(17) C55 0.036(2) 0.035(2) 0.050(3) -0.0091(19) 0.021(2) -0.0073(17) C56 0.034(2) 0.0277(19) 0.038(2) 0.0007(16) 0.0138(18) 0.0031(15) C61 0.033(2) 0.0322(19) 0.028(2) 0.0038(15) 0.0147(17) 0.0045(15) C62 0.040(2) 0.035(2) 0.036(2) -0.0007(17) 0.0185(19) 0.0052(17) C63 0.061(3) 0.039(2) 0.051(3) 0.002(2) 0.036(3) 0.014(2) C64 0.056(3) 0.058(3) 0.053(3) 0.019(2) 0.037(3) 0.030(2) C65 0.032(2) 0.076(3) 0.040(3) 0.028(2) 0.020(2) 0.020(2) C66 0.034(2) 0.049(2) 0.029(2) 0.0078(18) 0.0152(18) 0.0055(18) B 0.031(2) 0.026(2) 0.026(2) 0.0001(16) 0.0118(18) -0.0003(16) _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 C10 2.061(4) . ? Pt P 2.2116(10) . ? Pt C11 2.269(4) . ? Pt S 2.3608(10) . ? Pt C12 2.566(4) . ? S C2 1.775(4) . ? S C20 1.877(4) . ? P C3 1.800(4) . ? P C24 1.844(4) . ? P C27 1.846(4) . ? C1 C2 1.505(5) . ? C1 C7A 1.515(6) . ? C2 C3 1.347(5) . ? C3 C3A 1.480(5) . ? C3A C4 1.382(6) . ? C3A C7A 1.411(5) . ? C4 C5 1.387(6) . ? C5 C6 1.384(6) . ? C6 C7 1.381(7) . ? C7 C7A 1.373(6) . ? C10 C11 1.456(6) . ? C11 C12 1.407(6) . ? C11 C16 1.411(6) . ? C12 C13 1.400(6) . ? C13 C14 1.371(6) . ? C14 C15 1.388(6) . ? C15 C16 1.375(6) . ? C20 C22 1.512(7) . ? C20 C21 1.515(6) . ? C20 C23 1.524(6) . ? C24 C25 1.519(6) . ? C24 C26 1.528(6) . ? C27 C28 1.524(5) . ? C27 C29 1.529(6) . ? F32 C32 1.352(4) . ? F33 C33 1.346(5) . ? F34 C34 1.344(5) . ? F35 C35 1.356(5) . ? F36 C36 1.356(5) . ? F42 C42 1.351(4) . ? F43 C43 1.349(5) . ? F44 C44 1.352(4) . ? F45 C45 1.344(5) . ? F46 C46 1.348(4) . ? F52 C52 1.353(4) . ? F53 C53 1.348(5) . ? F54 C54 1.348(5) . ? F55 C55 1.348(5) . ? F56 C56 1.352(5) . ? F62 C62 1.343(5) . ? F63 C63 1.347(6) . ? F64 C64 1.353(5) . ? F65 C65 1.348(5) . ? F66 C66 1.356(5) . ? C31 C36 1.380(6) . ? C31 C32 1.401(6) . ? C31 B 1.659(6) . ? C32 C33 1.372(5) . ? C33 C34 1.373(6) . ? C34 C35 1.366(7) . ? C35 C36 1.386(6) . ? C41 C46 1.383(5) . ? C41 C42 1.392(5) . ? C41 B 1.652(6) . ? C42 C43 1.375(5) . ? C43 C44 1.368(6) . ? C44 C45 1.369(6) . ? C45 C46 1.388(5) . ? C51 C52 1.383(5) . ? C51 C56 1.388(5) . ? C51 B 1.660(6) . ? C52 C53 1.386(6) . ? C53 C54 1.373(6) . ? C54 C55 1.363(6) . ? C55 C56 1.382(6) . ? C61 C62 1.381(6) . ? C61 C66 1.389(6) . ? C61 B 1.670(6) . ? C62 C63 1.393(6) . ? C63 C64 1.360(7) . ? C64 C65 1.369(8) . ? C65 C66 1.378(6) . ? 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 C10 Pt P 100.35(12) . . ? C10 Pt C11 38.91(15) . . ? P Pt C11 138.13(10) . . ? C10 Pt S 170.75(12) . . ? P Pt S 88.70(3) . . ? C11 Pt S 132.50(10) . . ? C10 Pt C12 62.90(15) . . ? P Pt C12 155.88(10) . . ? C11 Pt C12 33.12(14) . . ? S Pt C12 107.92(10) . . ? C2 S C20 105.60(19) . . ? C2 S Pt 102.35(12) . . ? C20 S Pt 113.60(14) . . ? C3 P C24 102.36(17) . . ? C3 P C27 105.40(17) . . ? C24 P C27 107.77(18) . . ? C3 P Pt 105.70(12) . . ? C24 P Pt 117.15(13) . . ? C27 P Pt 116.77(13) . . ? C2 C1 C7A 102.2(3) . . ? C3 C2 C1 111.7(3) . . ? C3 C2 S 120.9(3) . . ? C1 C2 S 126.7(3) . . ? C2 C3 C3A 109.1(3) . . ? C2 C3 P 121.0(3) . . ? C3A C3 P 129.9(3) . . ? C4 C3A C7A 120.8(4) . . ? C4 C3A C3 131.5(3) . . ? C7A C3A C3 107.7(3) . . ? C3A C4 C5 118.6(4) . . ? C6 C5 C4 120.4(4) . . ? C7 C6 C5 121.2(4) . . ? C7A C7 C6 119.1(4) . . ? C7 C7A C3A 119.8(4) . . ? C7 C7A C1 130.8(4) . . ? C3A C7A C1 109.3(3) . . ? C11 C10 Pt 78.3(2) . . ? C12 C11 C16 117.8(4) . . ? C12 C11 C10 117.9(4) . . ? C16 C11 C10 123.5(4) . . ? C12 C11 Pt 85.1(3) . . ? C16 C11 Pt 113.8(3) . . ? C10 C11 Pt 62.8(2) . . ? C13 C12 C11 120.1(4) . . ? C13 C12 Pt 128.0(3) . . ? C11 C12 Pt 61.8(2) . . ? C14 C13 C12 120.7(4) . . ? C13 C14 C15 119.8(4) . . ? C16 C15 C14 120.6(4) . . ? C15 C16 C11 120.9(4) . . ? C22 C20 C21 113.3(4) . . ? C22 C20 C23 112.2(4) . . ? C21 C20 C23 109.5(4) . . ? C22 C20 S 110.6(3) . . ? C21 C20 S 107.6(3) . . ? C23 C20 S 103.1(3) . . ? C25 C24 C26 111.5(4) . . ? C25 C24 P 114.2(3) . . ? C26 C24 P 109.5(3) . . ? C28 C27 C29 109.5(3) . . ? C28 C27 P 112.9(3) . . ? C29 C27 P 110.8(3) . . ? C36 C31 C32 113.5(4) . . ? C36 C31 B 127.0(4) . . ? C32 C31 B 119.1(3) . . ? F32 C32 C33 116.8(3) . . ? F32 C32 C31 118.9(3) . . ? C33 C32 C31 124.3(4) . . ? F33 C33 C32 121.1(4) . . ? F33 C33 C34 119.3(4) . . ? C32 C33 C34 119.6(4) . . ? F34 C34 C35 120.5(4) . . ? F34 C34 C33 120.7(4) . . ? C35 C34 C33 118.7(4) . . ? F35 C35 C34 119.8(4) . . ? F35 C35 C36 119.7(4) . . ? C34 C35 C36 120.4(4) . . ? F36 C36 C31 121.8(4) . . ? F36 C36 C35 114.8(4) . . ? C31 C36 C35 123.4(4) . . ? C46 C41 C42 113.4(3) . . ? C46 C41 B 127.2(3) . . ? C42 C41 B 118.9(3) . . ? F42 C42 C43 116.1(3) . . ? F42 C42 C41 119.2(3) . . ? C43 C42 C41 124.6(4) . . ? F43 C43 C44 119.3(4) . . ? F43 C43 C42 121.6(4) . . ? C44 C43 C42 119.1(4) . . ? F44 C44 C43 120.7(4) . . ? F44 C44 C45 119.8(4) . . ? C43 C44 C45 119.5(4) . . ? F45 C45 C44 119.4(4) . . ? F45 C45 C46 121.0(4) . . ? C44 C45 C46 119.5(4) . . ? F46 C46 C41 121.5(3) . . ? F46 C46 C45 114.7(3) . . ? C41 C46 C45 123.8(4) . . ? C52 C51 C56 113.1(3) . . ? C52 C51 B 127.5(3) . . ? C56 C51 B 119.2(3) . . ? F52 C52 C51 121.2(3) . . ? F52 C52 C53 114.8(4) . . ? C51 C52 C53 123.9(4) . . ? F53 C53 C54 119.9(4) . . ? F53 C53 C52 120.4(4) . . ? C54 C53 C52 119.6(4) . . ? F54 C54 C55 120.3(4) . . ? F54 C54 C53 120.4(4) . . ? C55 C54 C53 119.3(4) . . ? F55 C55 C54 120.2(4) . . ? F55 C55 C56 120.8(4) . . ? C54 C55 C56 119.0(4) . . ? F56 C56 C55 115.8(4) . . ? F56 C56 C51 119.3(3) . . ? C55 C56 C51 124.9(4) . . ? C62 C61 C66 113.3(4) . . ? C62 C61 B 126.8(4) . . ? C66 C61 B 119.5(3) . . ? F62 C62 C61 121.8(4) . . ? F62 C62 C63 114.5(4) . . ? C61 C62 C63 123.7(4) . . ? F63 C63 C64 120.3(4) . . ? F63 C63 C62 120.0(4) . . ? C64 C63 C62 119.7(4) . . ? F64 C64 C63 120.4(5) . . ? F64 C64 C65 120.1(5) . . ? C63 C64 C65 119.5(4) . . ? F65 C65 C64 120.4(4) . . ? F65 C65 C66 120.6(5) . . ? C64 C65 C66 119.0(4) . . ? F66 C66 C65 115.9(4) . . ? F66 C66 C61 119.4(4) . . ? C65 C66 C61 124.7(4) . . ? C41 B C31 114.0(3) . . ? C41 B C51 114.0(3) . . ? C31 B C51 102.2(3) . . ? C41 B C61 101.0(3) . . ? C31 B C61 112.8(3) . . ? C51 B C61 113.4(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C10 Pt S C2 -177.1(8) . . . . ? P Pt S C2 -8.71(13) . . . . ? C11 Pt S C2 162.94(19) . . . . ? C12 Pt S C2 -170.91(16) . . . . ? C10 Pt S C20 69.5(8) . . . . ? P Pt S C20 -122.05(16) . . . . ? C11 Pt S C20 49.6(2) . . . . ? C12 Pt S C20 75.76(19) . . . . ? C10 Pt P C3 -177.10(18) . . . . ? C11 Pt P C3 -166.00(19) . . . . ? S Pt P C3 4.78(12) . . . . ? C12 Pt P C3 139.4(3) . . . . ? C10 Pt P C24 -63.9(2) . . . . ? C11 Pt P C24 -52.8(2) . . . . ? S Pt P C24 117.99(15) . . . . ? C12 Pt P C24 -107.4(3) . . . . ? C10 Pt P C27 66.11(19) . . . . ? C11 Pt P C27 77.2(2) . . . . ? S Pt P C27 -112.01(14) . . . . ? C12 Pt P C27 22.6(3) . . . . ? C7A C1 C2 C3 0.1(4) . . . . ? C7A C1 C2 S -169.8(3) . . . . ? C20 S C2 C3 132.1(3) . . . . ? Pt S C2 C3 13.0(3) . . . . ? C20 S C2 C1 -58.8(4) . . . . ? Pt S C2 C1 -178.0(3) . . . . ? C1 C2 C3 C3A -1.0(4) . . . . ? S C2 C3 C3A 169.6(3) . . . . ? C1 C2 C3 P 178.7(3) . . . . ? S C2 C3 P -10.7(4) . . . . ? C24 P C3 C2 -121.3(3) . . . . ? C27 P C3 C2 126.1(3) . . . . ? Pt P C3 C2 1.8(3) . . . . ? C24 P C3 C3A 58.3(4) . . . . ? C27 P C3 C3A -54.3(4) . . . . ? Pt P C3 C3A -178.5(3) . . . . ? C2 C3 C3A C4 -176.4(4) . . . . ? P C3 C3A C4 3.9(6) . . . . ? C2 C3 C3A C7A 1.5(4) . . . . ? P C3 C3A C7A -178.2(3) . . . . ? C7A C3A C4 C5 1.3(6) . . . . ? C3 C3A C4 C5 179.0(4) . . . . ? C3A C4 C5 C6 -0.1(7) . . . . ? C4 C5 C6 C7 0.3(7) . . . . ? C5 C6 C7 C7A -1.9(7) . . . . ? C6 C7 C7A C3A 3.1(6) . . . . ? C6 C7 C7A C1 -176.4(4) . . . . ? C4 C3A C7A C7 -2.9(6) . . . . ? C3 C3A C7A C7 178.9(4) . . . . ? C4 C3A C7A C1 176.7(4) . . . . ? C3 C3A C7A C1 -1.4(4) . . . . ? C2 C1 C7A C7 -179.6(4) . . . . ? C2 C1 C7A C3A 0.9(4) . . . . ? P Pt C10 C11 168.2(2) . . . . ? S Pt C10 C11 -23.6(10) . . . . ? C12 Pt C10 C11 -30.2(2) . . . . ? Pt C10 C11 C12 67.6(3) . . . . ? Pt C10 C11 C16 -101.8(4) . . . . ? C10 Pt C11 C12 -124.9(4) . . . . ? P Pt C11 C12 -142.4(2) . . . . ? S Pt C11 C12 50.1(3) . . . . ? C10 Pt C11 C16 116.9(4) . . . . ? P Pt C11 C16 99.3(3) . . . . ? S Pt C11 C16 -68.1(3) . . . . ? C12 Pt C11 C16 -118.3(4) . . . . ? P Pt C11 C10 -17.6(3) . . . . ? S Pt C11 C10 175.0(2) . . . . ? C12 Pt C11 C10 124.9(4) . . . . ? C16 C11 C12 C13 -5.3(6) . . . . ? C10 C11 C12 C13 -175.4(4) . . . . ? Pt C11 C12 C13 -119.7(4) . . . . ? C16 C11 C12 Pt 114.4(4) . . . . ? C10 C11 C12 Pt -55.6(3) . . . . ? C10 Pt C12 C13 143.0(4) . . . . ? P Pt C12 C13 -167.5(3) . . . . ? C11 Pt C12 C13 107.6(5) . . . . ? S Pt C12 C13 -35.9(4) . . . . ? C10 Pt C12 C11 35.4(3) . . . . ? P Pt C12 C11 84.9(3) . . . . ? S Pt C12 C11 -143.5(2) . . . . ? C11 C12 C13 C14 3.4(7) . . . . ? Pt C12 C13 C14 -72.6(6) . . . . ? C12 C13 C14 C15 0.2(7) . . . . ? C13 C14 C15 C16 -1.8(7) . . . . ? C14 C15 C16 C11 -0.3(7) . . . . ? C12 C11 C16 C15 3.8(6) . . . . ? C10 C11 C16 C15 173.3(4) . . . . ? Pt C11 C16 C15 101.2(4) . . . . ? C2 S C20 C22 -49.1(4) . . . . ? Pt S C20 C22 62.3(4) . . . . ? C2 S C20 C21 75.2(4) . . . . ? Pt S C20 C21 -173.5(3) . . . . ? C2 S C20 C23 -169.2(3) . . . . ? Pt S C20 C23 -57.8(3) . . . . ? C3 P C24 C25 -171.5(3) . . . . ? C27 P C24 C25 -60.7(4) . . . . ? Pt P C24 C25 73.4(3) . . . . ? C3 P C24 C26 62.6(3) . . . . ? C27 P C24 C26 173.5(3) . . . . ? Pt P C24 C26 -52.4(3) . . . . ? C3 P C27 C28 -161.4(3) . . . . ? C24 P C27 C28 89.9(3) . . . . ? Pt P C27 C28 -44.4(3) . . . . ? C3 P C27 C29 -38.1(3) . . . . ? C24 P C27 C29 -146.8(3) . . . . ? Pt P C27 C29 78.9(3) . . . . ? C36 C31 C32 F32 -179.9(3) . . . . ? B C31 C32 F32 6.6(5) . . . . ? C36 C31 C32 C33 0.8(6) . . . . ? B C31 C32 C33 -172.7(4) . . . . ? F32 C32 C33 F33 0.8(5) . . . . ? C31 C32 C33 F33 -179.9(4) . . . . ? F32 C32 C33 C34 -179.6(4) . . . . ? C31 C32 C33 C34 -0.3(6) . . . . ? F33 C33 C34 F34 -0.8(6) . . . . ? C32 C33 C34 F34 179.6(4) . . . . ? F33 C33 C34 C35 179.1(4) . . . . ? C32 C33 C34 C35 -0.5(6) . . . . ? F34 C34 C35 F35 0.3(6) . . . . ? C33 C34 C35 F35 -179.6(4) . . . . ? F34 C34 C35 C36 -179.4(4) . . . . ? C33 C34 C35 C36 0.7(6) . . . . ? C32 C31 C36 F36 -177.7(4) . . . . ? B C31 C36 F36 -4.8(6) . . . . ? C32 C31 C36 C35 -0.6(6) . . . . ? B C31 C36 C35 172.3(4) . . . . ? F35 C35 C36 F36 -2.6(6) . . . . ? C34 C35 C36 F36 177.1(4) . . . . ? F35 C35 C36 C31 -179.9(4) . . . . ? C34 C35 C36 C31 -0.2(7) . . . . ? C46 C41 C42 F42 -178.3(3) . . . . ? B C41 C42 F42 -5.8(5) . . . . ? C46 C41 C42 C43 0.8(6) . . . . ? B C41 C42 C43 173.3(4) . . . . ? F42 C42 C43 F43 0.2(6) . . . . ? C41 C42 C43 F43 -179.0(4) . . . . ? F42 C42 C43 C44 179.5(3) . . . . ? C41 C42 C43 C44 0.3(6) . . . . ? F43 C43 C44 F44 -1.5(6) . . . . ? C42 C43 C44 F44 179.3(4) . . . . ? F43 C43 C44 C45 178.3(4) . . . . ? C42 C43 C44 C45 -0.9(6) . . . . ? F44 C44 C45 F45 1.7(6) . . . . ? C43 C44 C45 F45 -178.0(4) . . . . ? F44 C44 C45 C46 -179.8(4) . . . . ? C43 C44 C45 C46 0.4(6) . . . . ? C42 C41 C46 F46 177.1(3) . . . . ? B C41 C46 F46 5.4(6) . . . . ? C42 C41 C46 C45 -1.4(6) . . . . ? B C41 C46 C45 -173.1(4) . . . . ? F45 C45 C46 F46 0.7(5) . . . . ? C44 C45 C46 F46 -177.8(4) . . . . ? F45 C45 C46 C41 179.3(4) . . . . ? C44 C45 C46 C41 0.8(6) . . . . ? C56 C51 C52 F52 -177.5(4) . . . . ? B C51 C52 F52 -2.6(6) . . . . ? C56 C51 C52 C53 2.7(6) . . . . ? B C51 C52 C53 177.6(4) . . . . ? F52 C52 C53 F53 -0.2(6) . . . . ? C51 C52 C53 F53 179.7(4) . . . . ? F52 C52 C53 C54 177.6(4) . . . . ? C51 C52 C53 C54 -2.5(7) . . . . ? F53 C53 C54 F54 -1.0(7) . . . . ? C52 C53 C54 F54 -178.8(4) . . . . ? F53 C53 C54 C55 178.8(4) . . . . ? C52 C53 C54 C55 0.9(7) . . . . ? F54 C54 C55 F55 -0.1(6) . . . . ? C53 C54 C55 F55 -179.9(4) . . . . ? F54 C54 C55 C56 179.9(4) . . . . ? C53 C54 C55 C56 0.2(7) . . . . ? F55 C55 C56 F56 -0.1(6) . . . . ? C54 C55 C56 F56 179.8(4) . . . . ? F55 C55 C56 C51 -179.8(4) . . . . ? C54 C55 C56 C51 0.2(7) . . . . ? C52 C51 C56 F56 178.8(3) . . . . ? B C51 C56 F56 3.5(5) . . . . ? C52 C51 C56 C55 -1.5(6) . . . . ? B C51 C56 C55 -176.9(4) . . . . ? C66 C61 C62 F62 177.2(4) . . . . ? B C61 C62 F62 3.9(6) . . . . ? C66 C61 C62 C63 -1.8(6) . . . . ? B C61 C62 C63 -175.1(4) . . . . ? F62 C62 C63 F63 2.0(6) . . . . ? C61 C62 C63 F63 -179.0(4) . . . . ? F62 C62 C63 C64 -177.2(4) . . . . ? C61 C62 C63 C64 1.9(7) . . . . ? F63 C63 C64 F64 0.0(7) . . . . ? C62 C63 C64 F64 179.1(4) . . . . ? F63 C63 C64 C65 179.6(4) . . . . ? C62 C63 C64 C65 -1.2(7) . . . . ? F64 C64 C65 F65 -0.3(7) . . . . ? C63 C64 C65 F65 -179.9(4) . . . . ? F64 C64 C65 C66 -179.7(4) . . . . ? C63 C64 C65 C66 0.7(7) . . . . ? F65 C65 C66 F66 1.2(6) . . . . ? C64 C65 C66 F66 -179.4(4) . . . . ? F65 C65 C66 C61 179.9(4) . . . . ? C64 C65 C66 C61 -0.7(7) . . . . ? C62 C61 C66 F66 179.9(3) . . . . ? B C61 C66 F66 -6.3(6) . . . . ? C62 C61 C66 C65 1.2(6) . . . . ? B C61 C66 C65 175.1(4) . . . . ? C46 C41 B C31 -11.2(5) . . . . ? C42 C41 B C31 177.5(3) . . . . ? C46 C41 B C51 -128.1(4) . . . . ? C42 C41 B C51 60.6(4) . . . . ? C46 C41 B C61 110.0(4) . . . . ? C42 C41 B C61 -61.4(4) . . . . ? C36 C31 B C41 125.7(4) . . . . ? C32 C31 B C41 -61.8(5) . . . . ? C36 C31 B C51 -110.8(4) . . . . ? C32 C31 B C51 61.7(4) . . . . ? C36 C31 B C61 11.3(5) . . . . ? C32 C31 B C61 -176.2(3) . . . . ? C52 C51 B C41 9.8(5) . . . . ? C56 C51 B C41 -175.6(3) . . . . ? C52 C51 B C31 -113.7(4) . . . . ? C56 C51 B C31 60.9(4) . . . . ? C52 C51 B C61 124.6(4) . . . . ? C56 C51 B C61 -60.8(5) . . . . ? C62 C61 B C41 113.4(4) . . . . ? C66 C61 B C41 -59.5(4) . . . . ? C62 C61 B C31 -124.5(4) . . . . ? C66 C61 B C31 62.6(5) . . . . ? C62 C61 B C51 -8.9(6) . . . . ? C66 C61 B C51 178.1(3) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.53 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 2.882 _refine_diff_density_min -0.537 _refine_diff_density_rms 0.138 # Attachment 'damskh0704.cif' data_damskh0704 _database_code_depnum_ccdc_archive 'CCDC 687093' # SUBMISSION DETAILS _audit_creation_method 'manual editing of SHELXL template' _publ_section_acknowledgements ; NSERC, CFI ; # CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H36 Cl P Pt S' _chemical_formula_sum 'C26 H36 Cl P Pt S' _chemical_formula_weight 642.12 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 13.1479(3) _cell_length_b 12.5326(4) _cell_length_c 15.8100(5) _cell_angle_alpha 90.00 _cell_angle_beta 98.1364(17) _cell_angle_gamma 90.00 _cell_volume 2578.91(13) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 5980 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.48 _exptl_crystal_description plate _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.654 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1272 _exptl_absorpt_coefficient_mu 5.699 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5245 _exptl_absorpt_correction_T_max 0.5245 _exptl_absorpt_process_details 'HKL Scalepack (Otwinowski & Minor 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Nonius FR590D, fine-focus sealed tube' _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type 'KappaCCD (BruKer AXS-Nonius, FR540C)' _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 'no decay' _diffrn_reflns_number 10055 _diffrn_reflns_av_R_equivalents 0.0389 _diffrn_reflns_av_sigmaI/netI 0.0505 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.07 _diffrn_reflns_theta_max 26.37 _reflns_number_total 5271 _reflns_number_gt 4253 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT, Bruker AXS/Nonius' _computing_cell_refinement 'HKL DENZO and SCALEPACK, Bruker AXS/Nonius' _computing_data_reduction 'HKL DENZO and SCALEPACK, Bruker AXS/Nonius' _computing_structure_solution ; SIR-97 (A. Altomare, G. Cascarano, C. Giacovazzo et al., 1999) ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; Cameron (WinGX v1.70-01), Ortep (SHELXTL-NT v6.14, Bruker AXS) ; _computing_publication_material 'WinGX v1.70.01 (L. J. Farrugia)' # REFINEMENT DATA _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^)+(0.0300P)^2^+3.5261P] 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 SHELXL _refine_ls_extinction_coef 0.00176(13) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 5271 _refine_ls_number_parameters 279 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0473 _refine_ls_R_factor_gt 0.0335 _refine_ls_wR_factor_ref 0.0810 _refine_ls_wR_factor_gt 0.0744 _refine_ls_goodness_of_fit_ref 1.081 _refine_ls_restrained_S_all 1.081 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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 0.268696(14) 0.589411(16) 0.318113(12) 0.02401(9) Uani 1 1 d . . . Cl1 Cl 0.33531(12) 0.76282(11) 0.34957(10) 0.0394(3) Uani 1 1 d . . . S1 S 0.42660(10) 0.51611(11) 0.38227(9) 0.0267(3) Uani 1 1 d . . . P1 P 0.20308(10) 0.42658(11) 0.30555(9) 0.0237(3) Uani 1 1 d . . . C1 C 0.4651(4) 0.2969(5) 0.4343(4) 0.0357(13) Uani 1 1 d . . . H1A H 0.5259 0.2800 0.4063 0.043 Uiso 1 1 calc R . . H1B H 0.4883 0.3211 0.4935 0.043 Uiso 1 1 calc R . . C2 C 0.3983(4) 0.3792(4) 0.3846(3) 0.0261(11) Uani 1 1 d . . . C3 C 0.3040(4) 0.3380(4) 0.3538(4) 0.0293(12) Uani 1 1 d . . . C3A C 0.3016(4) 0.2257(4) 0.3824(3) 0.0278(11) Uani 1 1 d . . . C4 C 0.2258(5) 0.1473(5) 0.3692(4) 0.0384(14) Uani 1 1 d . . . H4 H 0.1614 0.1619 0.3358 0.046 Uiso 1 1 calc . . . C5 C 0.2465(5) 0.0467(5) 0.4060(4) 0.0422(15) Uani 1 1 d . . . H5 H 0.1966 -0.0082 0.3951 0.051 Uiso 1 1 calc . . . C6 C 0.3371(5) 0.0258(5) 0.4573(4) 0.0413(15) Uani 1 1 d . . . H6 H 0.3483 -0.0424 0.4830 0.050 Uiso 1 1 calc . . . C7 C 0.4138(5) 0.1044(5) 0.4724(5) 0.0451(16) Uani 1 1 d . . . H7 H 0.4766 0.0907 0.5083 0.054 Uiso 1 1 calc . . . C7A C 0.3944(4) 0.2030(4) 0.4327(4) 0.0322(13) Uani 1 1 d . . . C21 C 0.1579(4) 0.3820(5) 0.1960(4) 0.0309(12) Uani 1 1 d . . . H21 H 0.0983 0.4289 0.1741 0.037 Uiso 1 1 calc R . . C22 C 0.2392(5) 0.4018(5) 0.1385(4) 0.0424(15) Uani 1 1 d . . . H22A H 0.3016 0.3619 0.1602 0.051 Uiso 1 1 calc R . . H22B H 0.2550 0.4782 0.1379 0.051 Uiso 1 1 calc R . . H22C H 0.2135 0.3781 0.0803 0.051 Uiso 1 1 calc R . . C23 C 0.1186(5) 0.2670(5) 0.1858(4) 0.0419(15) Uani 1 1 d . . . H23A H 0.0883 0.2547 0.1264 0.050 Uiso 1 1 calc R . . H23B H 0.0665 0.2551 0.2234 0.050 Uiso 1 1 calc R . . H23C H 0.1760 0.2175 0.2012 0.050 Uiso 1 1 calc R . . C24 C 0.0986(4) 0.3954(5) 0.3690(4) 0.0388(14) Uani 1 1 d . . . H24 H 0.0895 0.3162 0.3671 0.047 Uiso 1 1 calc R . . C25 C 0.1325(6) 0.4251(7) 0.4630(4) 0.063(2) Uani 1 1 d . . . H25A H 0.1433 0.5024 0.4678 0.075 Uiso 1 1 calc R . . H25B H 0.1968 0.3881 0.4841 0.075 Uiso 1 1 calc R . . H25C H 0.0792 0.4039 0.4971 0.075 Uiso 1 1 calc R . . C26 C -0.0053(5) 0.4436(6) 0.3364(5) 0.056(2) Uani 1 1 d . . . H26A H -0.0581 0.4104 0.3657 0.067 Uiso 1 1 calc R . . H26B H -0.0215 0.4311 0.2747 0.067 Uiso 1 1 calc R . . H26C H -0.0035 0.5205 0.3475 0.067 Uiso 1 1 calc R . . C31 C 0.5329(4) 0.5274(5) 0.3140(4) 0.0374(14) Uani 1 1 d . . . C32 C 0.5528(7) 0.6446(6) 0.3053(7) 0.085(3) Uani 1 1 d . . . H32A H 0.5766 0.6749 0.3617 0.102 Uiso 1 1 calc R . . H32B H 0.4892 0.6802 0.2804 0.102 Uiso 1 1 calc R . . H32C H 0.6055 0.6551 0.2680 0.102 Uiso 1 1 calc R . . C33 C 0.6263(5) 0.4735(9) 0.3588(7) 0.106(4) Uani 1 1 d . . . H33A H 0.6852 0.4897 0.3295 0.128 Uiso 1 1 calc R . . H33B H 0.6150 0.3961 0.3586 0.128 Uiso 1 1 calc R . . H33C H 0.6399 0.4990 0.4180 0.128 Uiso 1 1 calc R . . C34 C 0.5003(7) 0.4772(9) 0.2284(6) 0.095(4) Uani 1 1 d . . . H34A H 0.5557 0.4843 0.1932 0.114 Uiso 1 1 calc R . . H34B H 0.4385 0.5130 0.2000 0.114 Uiso 1 1 calc R . . H34C H 0.4856 0.4014 0.2359 0.114 Uiso 1 1 calc R . . C41 C 0.1334(4) 0.6624(5) 0.2594(3) 0.0319(13) Uani 1 1 d . . . H41A H 0.0736 0.6198 0.2713 0.038 Uiso 1 1 calc R . . H41B H 0.1277 0.7342 0.2843 0.038 Uiso 1 1 calc R . . C42 C 0.1307(4) 0.6725(5) 0.1648(4) 0.0320(13) Uani 1 1 d . . . C43 C 0.0525(4) 0.6275(5) 0.1077(4) 0.0407(15) Uani 1 1 d . . . H43 H 0.0006 0.5872 0.1293 0.049 Uiso 1 1 calc . . . C44 C 0.0480(5) 0.6399(6) 0.0200(4) 0.0459(16) Uani 1 1 d . . . H44 H -0.0067 0.6089 -0.0177 0.055 Uiso 1 1 calc . . . C45 C 0.1225(6) 0.6969(6) -0.0117(4) 0.0510(18) Uani 1 1 d . . . H45 H 0.1198 0.7050 -0.0717 0.061 Uiso 1 1 calc . . . C46 C 0.2021(5) 0.7430(5) 0.0431(4) 0.0426(15) Uani 1 1 d . . . H46 H 0.2531 0.7837 0.0208 0.051 Uiso 1 1 calc . . . C47 C 0.2068(4) 0.7297(5) 0.1295(4) 0.0351(13) Uani 1 1 d . . . H47 H 0.2627 0.7596 0.1665 0.042 Uiso 1 1 calc . . . 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 0.02794(12) 0.02081(12) 0.02466(12) -0.00026(9) 0.00846(8) 0.00022(8) Cl1 0.0512(8) 0.0213(7) 0.0471(8) -0.0044(6) 0.0117(7) -0.0054(6) S1 0.0275(6) 0.0238(7) 0.0286(7) -0.0018(5) 0.0036(6) -0.0023(5) P1 0.0228(6) 0.0239(7) 0.0249(7) 0.0008(5) 0.0056(5) -0.0026(5) C1 0.035(3) 0.030(3) 0.039(3) 0.001(3) -0.005(3) 0.005(2) C2 0.031(3) 0.024(3) 0.025(3) 0.003(2) 0.008(2) 0.001(2) C3 0.029(3) 0.026(3) 0.033(3) 0.003(2) 0.004(2) -0.003(2) C3A 0.035(3) 0.027(3) 0.022(3) -0.001(2) 0.005(2) -0.001(2) C4 0.040(3) 0.031(3) 0.045(4) 0.003(3) 0.009(3) -0.001(3) C5 0.051(4) 0.022(3) 0.055(4) 0.005(3) 0.013(3) -0.002(3) C6 0.052(4) 0.021(3) 0.054(4) 0.008(3) 0.019(3) 0.007(3) C7 0.046(4) 0.035(4) 0.052(4) 0.005(3) 0.003(3) 0.011(3) C7A 0.038(3) 0.026(3) 0.033(3) 0.000(2) 0.006(3) 0.004(2) C21 0.029(3) 0.033(3) 0.028(3) -0.001(2) -0.003(2) 0.004(2) C22 0.047(4) 0.049(4) 0.032(3) -0.003(3) 0.008(3) -0.006(3) C23 0.042(3) 0.034(3) 0.048(4) -0.005(3) -0.002(3) -0.009(3) C24 0.038(3) 0.038(4) 0.045(4) -0.003(3) 0.019(3) -0.004(3) C25 0.061(4) 0.093(6) 0.041(4) -0.007(4) 0.029(4) -0.007(4) C26 0.034(3) 0.054(4) 0.086(6) 0.003(4) 0.029(4) -0.002(3) C31 0.033(3) 0.036(3) 0.046(4) -0.001(3) 0.017(3) -0.006(3) C32 0.093(6) 0.037(4) 0.142(9) -0.007(5) 0.079(7) -0.016(4) C33 0.030(4) 0.159(11) 0.137(9) 0.086(8) 0.034(5) 0.033(5) C34 0.079(6) 0.141(9) 0.078(7) -0.047(6) 0.059(5) -0.050(6) C41 0.037(3) 0.028(3) 0.034(3) 0.008(2) 0.014(3) 0.008(2) C42 0.032(3) 0.026(3) 0.038(3) 0.008(2) 0.006(3) 0.009(2) C43 0.030(3) 0.035(3) 0.055(4) 0.008(3) -0.003(3) 0.000(3) C44 0.047(4) 0.040(4) 0.046(4) 0.002(3) -0.013(3) 0.002(3) C45 0.063(4) 0.058(5) 0.028(3) 0.006(3) -0.004(3) 0.013(4) C46 0.043(3) 0.047(4) 0.039(3) 0.006(3) 0.010(3) -0.002(3) C47 0.034(3) 0.029(3) 0.041(3) 0.002(3) 0.004(3) -0.004(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. ; # MOLECULAR GEOMETRY 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 C41 2.096(5) . ? Pt1 P1 2.2135(14) . ? Pt1 S1 2.3637(14) . ? Pt1 Cl1 2.3695(14) . ? S1 C2 1.757(5) . ? S1 C31 1.889(5) . ? P1 C3 1.814(6) . ? P1 C21 1.837(6) . ? P1 C24 1.854(5) . ? C1 C7A 1.498(8) . ? C1 C2 1.502(7) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C3 1.368(7) . ? C3 C3A 1.479(8) . ? C3A C7A 1.388(8) . ? C3A C4 1.394(8) . ? C4 C5 1.399(9) . ? C4 H4 0.9500 . ? C5 C6 1.368(9) . ? C5 H5 0.9500 . ? C6 C7 1.405(9) . ? C6 H6 0.9500 . ? C7 C7A 1.393(8) . ? C7 H7 0.9500 . ? C21 C22 1.518(8) . ? C21 C23 1.532(8) . ? C21 H21 1.0000 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 C26 1.516(9) . ? C24 C25 1.536(9) . ? C24 H24 1.0000 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C31 C33 1.490(10) . ? C31 C34 1.499(10) . ? C31 C32 1.501(9) . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C41 C42 1.497(8) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 C43 1.389(9) . ? C42 C47 1.408(8) . ? C43 C44 1.388(9) . ? C43 H43 0.9500 . ? C44 C45 1.363(10) . ? C44 H44 0.9500 . ? C45 C46 1.387(9) . ? C45 H45 0.9500 . ? C46 C47 1.369(8) . ? C46 H46 0.9500 . ? C47 H47 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 C41 Pt1 P1 93.84(17) . . ? C41 Pt1 S1 176.63(16) . . ? P1 Pt1 S1 89.29(5) . . ? C41 Pt1 Cl1 87.59(17) . . ? P1 Pt1 Cl1 172.85(5) . . ? S1 Pt1 Cl1 89.44(5) . . ? C2 S1 C31 105.1(3) . . ? C2 S1 Pt1 102.30(19) . . ? C31 S1 Pt1 113.7(2) . . ? C3 P1 C21 109.3(3) . . ? C3 P1 C24 101.4(3) . . ? C21 P1 C24 106.3(3) . . ? C3 P1 Pt1 105.90(18) . . ? C21 P1 Pt1 115.77(19) . . ? C24 P1 Pt1 117.1(2) . . ? C7A C1 C2 102.4(4) . . ? C7A C1 H1A 111.3 . . ? C2 C1 H1A 111.3 . . ? C7A C1 H1B 111.3 . . ? C2 C1 H1B 111.3 . . ? H1A C1 H1B 109.2 . . ? C3 C2 C1 111.1(5) . . ? C3 C2 S1 123.0(4) . . ? C1 C2 S1 124.9(4) . . ? C2 C3 C3A 108.0(5) . . ? C2 C3 P1 119.4(4) . . ? C3A C3 P1 131.6(4) . . ? C7A C3A C4 119.5(5) . . ? C7A C3A C3 108.3(5) . . ? C4 C3A C3 132.1(5) . . ? C3A C4 C5 118.7(6) . . ? C3A C4 H4 120.7 . . ? C5 C4 H4 120.7 . . ? C6 C5 C4 121.4(6) . . ? C6 C5 H5 119.3 . . ? C4 C5 H5 119.3 . . ? C5 C6 C7 120.7(6) . . ? C5 C6 H6 119.7 . . ? C7 C6 H6 119.7 . . ? C7A C7 C6 117.7(6) . . ? C7A C7 H7 121.2 . . ? C6 C7 H7 121.2 . . ? C3A C7A C7 122.0(6) . . ? C3A C7A C1 110.0(5) . . ? C7 C7A C1 128.0(6) . . ? C22 C21 C23 110.3(5) . . ? C22 C21 P1 110.7(4) . . ? C23 C21 P1 116.4(4) . . ? C22 C21 H21 106.3 . . ? C23 C21 H21 106.3 . . ? P1 C21 H21 106.3 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C26 C24 C25 111.0(6) . . ? C26 C24 P1 115.6(5) . . ? C25 C24 P1 109.6(4) . . ? C26 C24 H24 106.7 . . ? C25 C24 H24 106.7 . . ? P1 C24 H24 106.7 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C33 C31 C34 110.5(8) . . ? C33 C31 C32 110.2(7) . . ? C34 C31 C32 111.1(7) . . ? C33 C31 S1 108.6(5) . . ? C34 C31 S1 110.1(4) . . ? C32 C31 S1 106.1(4) . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C31 C33 H33A 109.5 . . ? C31 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C31 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C31 C34 H34A 109.5 . . ? C31 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C31 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C42 C41 Pt1 112.2(3) . . ? C42 C41 H41A 109.2 . . ? Pt1 C41 H41A 109.2 . . ? C42 C41 H41B 109.2 . . ? Pt1 C41 H41B 109.2 . . ? H41A C41 H41B 107.9 . . ? C43 C42 C47 116.9(6) . . ? C43 C42 C41 121.7(5) . . ? C47 C42 C41 121.4(6) . . ? C44 C43 C42 121.8(6) . . ? C44 C43 H43 119.1 . . ? C42 C43 H43 119.1 . . ? C45 C44 C43 119.6(6) . . ? C45 C44 H44 120.2 . . ? C43 C44 H44 120.2 . . ? C44 C45 C46 120.5(6) . . ? C44 C45 H45 119.8 . . ? C46 C45 H45 119.8 . . ? C47 C46 C45 119.7(6) . . ? C47 C46 H46 120.1 . . ? C45 C46 H46 120.1 . . ? C46 C47 C42 121.5(6) . . ? C46 C47 H47 119.2 . . ? C42 C47 H47 119.2 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag P1 Pt1 S1 C2 -1.44(18) . . . . ? Cl1 Pt1 S1 C2 171.53(18) . . . . ? P1 Pt1 S1 C31 111.3(2) . . . . ? Cl1 Pt1 S1 C31 -75.7(2) . . . . ? C41 Pt1 P1 C3 -179.2(2) . . . . ? S1 Pt1 P1 C3 2.08(18) . . . . ? C41 Pt1 P1 C21 59.6(2) . . . . ? S1 Pt1 P1 C21 -119.2(2) . . . . ? C41 Pt1 P1 C24 -67.1(3) . . . . ? S1 Pt1 P1 C24 114.2(2) . . . . ? C7A C1 C2 C3 -3.2(6) . . . . ? C7A C1 C2 S1 165.7(4) . . . . ? C31 S1 C2 C3 -118.8(5) . . . . ? Pt1 S1 C2 C3 0.2(5) . . . . ? C31 S1 C2 C1 73.6(5) . . . . ? Pt1 S1 C2 C1 -167.4(4) . . . . ? C1 C2 C3 C3A 0.9(6) . . . . ? S1 C2 C3 C3A -168.3(4) . . . . ? C1 C2 C3 P1 170.8(4) . . . . ? S1 C2 C3 P1 1.7(6) . . . . ? C21 P1 C3 C2 122.7(4) . . . . ? C24 P1 C3 C2 -125.4(5) . . . . ? Pt1 P1 C3 C2 -2.7(5) . . . . ? C21 P1 C3 C3A -70.2(6) . . . . ? C24 P1 C3 C3A 41.8(6) . . . . ? Pt1 P1 C3 C3A 164.4(5) . . . . ? C2 C3 C3A C7A 2.1(6) . . . . ? P1 C3 C3A C7A -166.2(4) . . . . ? C2 C3 C3A C4 -179.7(6) . . . . ? P1 C3 C3A C4 12.1(9) . . . . ? C7A C3A C4 C5 -1.2(8) . . . . ? C3 C3A C4 C5 -179.3(6) . . . . ? C3A C4 C5 C6 3.0(9) . . . . ? C4 C5 C6 C7 -2.1(10) . . . . ? C5 C6 C7 C7A -0.6(9) . . . . ? C4 C3A C7A C7 -1.4(8) . . . . ? C3 C3A C7A C7 177.1(5) . . . . ? C4 C3A C7A C1 177.3(5) . . . . ? C3 C3A C7A C1 -4.2(6) . . . . ? C6 C7 C7A C3A 2.3(9) . . . . ? C6 C7 C7A C1 -176.2(6) . . . . ? C2 C1 C7A C3A 4.5(6) . . . . ? C2 C1 C7A C7 -176.9(6) . . . . ? C3 P1 C21 C22 -70.1(5) . . . . ? C24 P1 C21 C22 -178.8(4) . . . . ? Pt1 P1 C21 C22 49.3(4) . . . . ? C3 P1 C21 C23 56.8(5) . . . . ? C24 P1 C21 C23 -51.9(5) . . . . ? Pt1 P1 C21 C23 176.2(4) . . . . ? C3 P1 C24 C26 -170.7(5) . . . . ? C21 P1 C24 C26 -56.5(6) . . . . ? Pt1 P1 C24 C26 74.6(5) . . . . ? C3 P1 C24 C25 62.9(5) . . . . ? C21 P1 C24 C25 177.1(5) . . . . ? Pt1 P1 C24 C25 -51.7(6) . . . . ? C2 S1 C31 C33 -65.8(7) . . . . ? Pt1 S1 C31 C33 -176.9(6) . . . . ? C2 S1 C31 C34 55.3(7) . . . . ? Pt1 S1 C31 C34 -55.8(6) . . . . ? C2 S1 C31 C32 175.6(6) . . . . ? Pt1 S1 C31 C32 64.6(6) . . . . ? P1 Pt1 C41 C42 -90.6(4) . . . . ? Cl1 Pt1 C41 C42 96.4(4) . . . . ? Pt1 C41 C42 C43 121.9(5) . . . . ? Pt1 C41 C42 C47 -59.1(6) . . . . ? C47 C42 C43 C44 -1.3(9) . . . . ? C41 C42 C43 C44 177.8(6) . . . . ? C42 C43 C44 C45 0.5(10) . . . . ? C43 C44 C45 C46 -0.4(11) . . . . ? C44 C45 C46 C47 1.1(11) . . . . ? C45 C46 C47 C42 -1.9(10) . . . . ? C43 C42 C47 C46 2.0(9) . . . . ? C41 C42 C47 C46 -177.1(6) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.897 _refine_diff_density_min -0.924 _refine_diff_density_rms 0.141