# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Kunio Mochida' _publ_contact_author_email KUNIO.MOCHIDA@GAKUSHUIN.AC.JP _publ_section_title ; Syntheses of Mono- and Dinuclear Silylplatinum Complexes Bearing a Diphosphino Ligand via Stepwise Bond Activation of Unsymmetric Disilanes ; loop_ _publ_author_name 'Kunio Mochida' 'Hidekazu Arii' 'Masato Nanjo' 'Makiko Takahashi' data_complex2a _database_code_depnum_ccdc_archive 'CCDC 761290' #TrackingRef 'CIF.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C35 H48 O P2 Pt Si2' _chemical_formula_weight 797.94 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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)/n ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 13.049(3) _cell_length_b 10.517(2) _cell_length_c 26.795(6) _cell_angle_alpha 90.00 _cell_angle_beta 103.762(3) _cell_angle_gamma 90.00 _cell_volume 3571.8(14) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 9887 _cell_measurement_theta_min 2.51 _cell_measurement_theta_max 27.54 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.484 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1608 _exptl_absorpt_coefficient_mu 4.111 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6383 _exptl_absorpt_correction_T_max 0.7345 _exptl_absorpt_process_details ; SADABS Sheldrick 1996 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker TXS fine-focus rotating anode' _diffrn_radiation_monochromator 'Bruker Helios multilayer confocal mirror' _diffrn_measurement_device_type 'Bruker APEXII CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 8.333 _diffrn_reflns_number 36745 _diffrn_reflns_av_R_equivalents 0.0665 _diffrn_reflns_av_sigmaI/netI 0.0552 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 1.56 _diffrn_reflns_theta_max 27.62 _reflns_number_total 8162 _reflns_number_gt 7265 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker AXS, 2006)' _computing_cell_refinement 'APEX2 (Bruker AXS, 2006)' _computing_data_reduction 'SAINT (Bruker AXS, 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XSHEL (Bruker AXS,2002)' _computing_publication_material 'XCIF (Bruker AXS, 2001)' _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. The minimum residual density locates at 0.8638 0.9342 0.1430 (1.17 _ from H1H). ; _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^)+(0.0500P)^2^+150.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8162 _refine_ls_number_parameters 379 _refine_ls_number_restraints 49 _refine_ls_R_factor_all 0.0966 _refine_ls_R_factor_gt 0.0874 _refine_ls_wR_factor_ref 0.2112 _refine_ls_wR_factor_gt 0.2068 _refine_ls_goodness_of_fit_ref 1.085 _refine_ls_restrained_S_all 1.085 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.86582(3) 0.68923(5) 0.143388(17) 0.02341(15) Uani 1 1 d D . . P1 P 0.8358(2) 0.6036(3) 0.21805(11) 0.0216(6) Uani 1 1 d . . . P2 P 0.8666(2) 0.4835(3) 0.11675(12) 0.0232(6) Uani 1 1 d . . . Si1 Si 0.8820(3) 0.7934(4) 0.06827(14) 0.0280(7) Uani 1 1 d . . . Si2 Si 0.7340(3) 0.9222(4) 0.03551(13) 0.0272(7) Uani 1 1 d . . . O1 O 0.2439(9) 0.7829(10) 0.1661(5) 0.049(3) Uani 1 1 d . . . C1 C 0.8492(11) 0.4300(13) 0.2152(5) 0.035(3) Uani 1 1 d . . . H1A H 0.9243 0.4055 0.2269 0.042 Uiso 1 1 calc R . . H1B H 0.8093 0.3886 0.2379 0.042 Uiso 1 1 calc R . . C2 C 0.8053(10) 0.3866(12) 0.1588(5) 0.029(3) Uani 1 1 d . . . H2A H 0.7277 0.3973 0.1491 0.034 Uiso 1 1 calc R . . H2B H 0.8217 0.2956 0.1552 0.034 Uiso 1 1 calc R . . C3 C 0.6993(9) 0.6220(12) 0.2224(4) 0.024(2) Uani 1 1 d U . . C4 C 0.6281(11) 0.6769(14) 0.1810(5) 0.035(3) Uani 1 1 d . . . H4 H 0.6519 0.7039 0.1519 0.042 Uiso 1 1 calc R . . C5 C 0.5218(11) 0.6932(18) 0.1816(6) 0.048(4) Uani 1 1 d . . . H5 H 0.4738 0.7313 0.1533 0.058 Uiso 1 1 calc R . . C6 C 0.4877(11) 0.6520(17) 0.2249(6) 0.047(4) Uani 1 1 d . . . H6 H 0.4162 0.6635 0.2263 0.056 Uiso 1 1 calc R . . C7 C 0.5573(10) 0.5955(13) 0.2649(5) 0.031(2) Uani 1 1 d U . . H7 H 0.5337 0.5666 0.2938 0.037 Uiso 1 1 calc R . . C8 C 0.6618(9) 0.5802(12) 0.2636(4) 0.026(2) Uani 1 1 d U . . H8 H 0.7089 0.5401 0.2916 0.031 Uiso 1 1 calc R . . C9 C 0.9099(10) 0.6513(13) 0.2811(5) 0.029(3) Uani 1 1 d . . . C10 C 0.9432(11) 0.7775(14) 0.2890(5) 0.036(3) Uani 1 1 d . . . H10 H 0.9300 0.8341 0.2606 0.043 Uiso 1 1 calc R . . C11 C 0.9957(12) 0.8236(16) 0.3375(6) 0.044(3) Uani 1 1 d . . . H11 H 1.0154 0.9105 0.3424 0.052 Uiso 1 1 calc R . . C12 C 1.0178(12) 0.739(2) 0.3780(6) 0.051(5) Uani 1 1 d . . . H12 H 1.0550 0.7680 0.4109 0.061 Uiso 1 1 calc R . . C13 C 0.9868(11) 0.6129(19) 0.3716(6) 0.047(4) Uani 1 1 d . . . H13 H 1.0017 0.5564 0.4000 0.057 Uiso 1 1 calc R . . C14 C 0.9349(11) 0.5702(16) 0.3242(5) 0.040(3) Uani 1 1 d . . . H14 H 0.9150 0.4832 0.3201 0.048 Uiso 1 1 calc R . . C15 C 0.7916(10) 0.4327(17) 0.0534(6) 0.042(3) Uani 1 1 d U . . C16 C 0.8373(11) 0.3680(15) 0.0188(5) 0.036(3) Uani 1 1 d U . . H16 H 0.9102 0.3467 0.0283 0.043 Uiso 1 1 calc R . . C17 C 0.7778(13) 0.3346(16) -0.0291(6) 0.046(3) Uani 1 1 d U . . H17 H 0.8096 0.2898 -0.0523 0.055 Uiso 1 1 calc R . . C18 C 0.6746(14) 0.3653(19) -0.0432(7) 0.060(4) Uani 1 1 d U . . H18 H 0.6337 0.3417 -0.0762 0.072 Uiso 1 1 calc R . . C19 C 0.6286(13) 0.431(2) -0.0100(7) 0.067(4) Uani 1 1 d U . . H19 H 0.5558 0.4515 -0.0199 0.081 Uiso 1 1 calc R . . C20 C 0.6872(11) 0.4663(19) 0.0377(7) 0.055(3) Uani 1 1 d U . . H20 H 0.6553 0.5144 0.0599 0.066 Uiso 1 1 calc R . . C21 C 0.9980(9) 0.4165(13) 0.1239(4) 0.027(3) Uani 1 1 d . . . C22 C 1.0832(10) 0.4985(14) 0.1275(5) 0.032(3) Uani 1 1 d . . . H22 H 1.0719 0.5878 0.1260 0.038 Uiso 1 1 calc R . . C23 C 1.1842(11) 0.4506(17) 0.1334(6) 0.042(4) Uani 1 1 d . . . H23 H 1.2417 0.5075 0.1354 0.051 Uiso 1 1 calc R . . C24 C 1.2021(11) 0.3239(18) 0.1362(6) 0.049(4) Uani 1 1 d . . . H24 H 1.2718 0.2923 0.1405 0.059 Uiso 1 1 calc R . . C25 C 1.1188(11) 0.2403(15) 0.1328(6) 0.042(4) Uani 1 1 d . . . H25 H 1.1314 0.1513 0.1339 0.050 Uiso 1 1 calc R . . C26 C 1.0171(10) 0.2858(12) 0.1279(5) 0.030(3) Uani 1 1 d . . . H26 H 0.9606 0.2283 0.1274 0.036 Uiso 1 1 calc R . . C27 C 0.9959(10) 0.9142(14) 0.0806(6) 0.040(3) Uani 1 1 d . . . H27A H 1.0630 0.8690 0.0845 0.060 Uiso 1 1 calc R . . H27B H 0.9963 0.9621 0.1120 0.060 Uiso 1 1 calc R . . H27C H 0.9863 0.9729 0.0514 0.060 Uiso 1 1 calc R . . C28 C 0.9037(11) 0.6992(14) 0.0126(5) 0.037(3) Uani 1 1 d . . . H28A H 0.9125 0.7572 -0.0147 0.055 Uiso 1 1 calc R . . H28B H 0.8426 0.6440 -0.0004 0.055 Uiso 1 1 calc R . . H28C H 0.9672 0.6469 0.0236 0.055 Uiso 1 1 calc R . . C29 C 0.7406(12) 1.0728(15) 0.0746(6) 0.041(3) Uani 1 1 d . . . H29A H 0.6796 1.1266 0.0597 0.061 Uiso 1 1 calc R . . H29B H 0.8057 1.1189 0.0742 0.061 Uiso 1 1 calc R . . H29C H 0.7399 1.0512 0.1101 0.061 Uiso 1 1 calc R . . C30 C 0.6065(11) 0.8393(14) 0.0336(6) 0.038(3) Uani 1 1 d . . . H30A H 0.5476 0.8952 0.0178 0.057 Uiso 1 1 calc R . . H30B H 0.6022 0.8180 0.0686 0.057 Uiso 1 1 calc R . . H30C H 0.6027 0.7611 0.0133 0.057 Uiso 1 1 calc R . . C31 C 0.7330(11) 0.9756(15) -0.0311(5) 0.034(3) Uani 1 1 d . . . H31A H 0.7300 0.9012 -0.0534 0.052 Uiso 1 1 calc R . . H31B H 0.7974 1.0241 -0.0306 0.052 Uiso 1 1 calc R . . H31C H 0.6712 1.0294 -0.0442 0.052 Uiso 1 1 calc R . . C32 C 0.2913(13) 0.9007(18) 0.1661(7) 0.055(4) Uani 1 1 d . . . H32A H 0.2508 0.9528 0.1373 0.067 Uiso 1 1 calc R . . H32B H 0.3639 0.8901 0.1615 0.067 Uiso 1 1 calc R . . C33 C 0.2941(18) 0.965(3) 0.2160(8) 0.082(5) Uani 1 1 d U . . H33A H 0.3543 0.9363 0.2436 0.098 Uiso 1 1 calc R . . H33B H 0.2957 1.0589 0.2130 0.098 Uiso 1 1 calc R . . C34 C 0.1920(18) 0.919(2) 0.2238(8) 0.079(4) Uani 1 1 d U . . H34A H 0.1330 0.9719 0.2045 0.094 Uiso 1 1 calc R . . H34B H 0.1915 0.9205 0.2607 0.094 Uiso 1 1 calc R . . C35 C 0.1832(18) 0.784(2) 0.2034(8) 0.076(5) Uani 1 1 d U . . H35A H 0.2118 0.7229 0.2313 0.092 Uiso 1 1 calc R . . H35B H 0.1088 0.7620 0.1877 0.092 Uiso 1 1 calc R . . H1H H 0.874(13) 0.828(8) 0.157(7) 0.06(5) Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.0250(2) 0.0246(2) 0.0216(2) 0.00445(19) 0.00724(15) 0.0021(2) P1 0.0227(14) 0.0258(15) 0.0171(13) 0.0032(12) 0.0062(11) 0.0055(12) P2 0.0210(14) 0.0243(15) 0.0274(15) 0.0014(12) 0.0118(12) 0.0009(12) Si1 0.0214(15) 0.0311(19) 0.0325(17) 0.0010(15) 0.0086(13) -0.0066(14) Si2 0.0215(15) 0.0328(19) 0.0265(16) 0.0028(15) 0.0042(13) -0.0010(14) O1 0.050(6) 0.032(6) 0.062(7) -0.009(5) 0.006(5) 0.005(5) C1 0.044(8) 0.030(7) 0.040(7) 0.009(6) 0.025(6) 0.012(6) C2 0.037(7) 0.022(6) 0.034(7) -0.004(5) 0.021(5) -0.009(5) C3 0.026(5) 0.026(5) 0.023(5) 0.002(4) 0.010(4) 0.004(4) C4 0.040(7) 0.036(7) 0.025(6) -0.006(6) 0.001(5) 0.009(6) C5 0.030(7) 0.063(10) 0.042(8) -0.025(8) -0.011(6) 0.004(7) C6 0.025(7) 0.062(11) 0.055(9) -0.026(8) 0.011(6) -0.002(7) C7 0.028(5) 0.036(6) 0.031(5) -0.004(5) 0.011(4) 0.000(5) C8 0.028(5) 0.030(5) 0.020(4) 0.010(4) 0.007(4) 0.007(4) C9 0.024(6) 0.041(7) 0.024(6) 0.006(5) 0.009(5) 0.008(5) C10 0.034(7) 0.041(8) 0.031(7) 0.009(6) 0.005(5) 0.013(6) C11 0.041(8) 0.044(9) 0.042(8) -0.010(7) 0.001(6) -0.002(7) C12 0.030(7) 0.093(14) 0.025(7) -0.001(8) 0.000(6) 0.012(8) C13 0.030(7) 0.080(13) 0.029(7) 0.025(8) 0.000(6) 0.011(8) C14 0.036(7) 0.054(9) 0.029(7) 0.022(7) 0.004(6) 0.007(7) C15 0.019(5) 0.065(8) 0.043(6) -0.024(6) 0.009(5) -0.008(5) C16 0.039(6) 0.046(7) 0.025(5) -0.006(5) 0.011(5) -0.002(5) C17 0.047(6) 0.053(7) 0.035(5) -0.014(5) 0.005(5) -0.004(5) C18 0.055(7) 0.067(8) 0.048(7) -0.022(7) -0.007(6) -0.006(7) C19 0.031(6) 0.100(10) 0.061(8) -0.034(8) -0.007(6) 0.003(7) C20 0.025(5) 0.084(8) 0.052(7) -0.031(6) 0.000(5) 0.000(6) C21 0.024(6) 0.039(7) 0.017(5) 0.005(5) 0.004(4) 0.005(5) C22 0.030(6) 0.041(8) 0.023(6) 0.006(6) 0.003(5) 0.004(6) C23 0.022(6) 0.060(10) 0.043(8) 0.007(8) 0.004(6) 0.004(7) C24 0.025(7) 0.071(12) 0.050(9) 0.004(9) 0.009(6) 0.020(8) C25 0.039(8) 0.039(8) 0.040(8) -0.007(6) -0.006(6) 0.016(6) C26 0.024(6) 0.022(6) 0.042(7) -0.005(5) 0.002(5) 0.006(5) C27 0.023(6) 0.038(8) 0.058(9) 0.019(7) 0.008(6) -0.007(6) C28 0.042(7) 0.037(8) 0.038(7) 0.010(7) 0.023(6) 0.008(6) C29 0.042(8) 0.042(8) 0.038(8) -0.008(7) 0.011(6) 0.001(7) C30 0.030(7) 0.039(8) 0.044(8) 0.005(6) 0.006(6) -0.005(6) C31 0.035(7) 0.045(8) 0.020(6) 0.003(6) -0.001(5) -0.007(6) C32 0.040(9) 0.056(11) 0.069(12) 0.003(9) 0.009(8) 0.009(8) C33 0.077(9) 0.095(12) 0.063(9) -0.008(9) -0.003(8) 0.024(9) C34 0.075(8) 0.100(11) 0.057(8) -0.003(8) 0.007(7) 0.027(9) C35 0.070(9) 0.097(12) 0.061(9) 0.009(9) 0.011(8) 0.019(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 P2 2.279(3) . ? Pt1 P1 2.311(3) . ? Pt1 Si1 2.345(3) . ? Pt1 H1H 1.51(8) . ? P1 C9 1.806(13) . ? P1 C3 1.823(12) . ? P1 C1 1.837(14) . ? P2 C21 1.822(12) . ? P2 C15 1.827(14) . ? P2 C2 1.838(12) . ? Si1 C28 1.868(14) . ? Si1 C27 1.922(13) . ? Si1 Si2 2.351(5) . ? Si2 C31 1.868(13) . ? Si2 C30 1.869(14) . ? Si2 C29 1.890(15) . ? O1 C32 1.38(2) . ? O1 C35 1.42(2) . ? C1 C2 1.551(19) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C8 1.381(16) . ? C3 C4 1.391(17) . ? C4 C5 1.40(2) . ? C4 H4 0.9500 . ? C5 C6 1.41(2) . ? C5 H5 0.9500 . ? C6 C7 1.36(2) . ? C6 H6 0.9500 . ? C7 C8 1.382(17) . ? C7 H7 0.9500 . ? C8 H8 0.9500 . ? C9 C10 1.40(2) . ? C9 C14 1.410(18) . ? C10 C11 1.40(2) . ? C10 H10 0.9500 . ? C11 C12 1.38(2) . ? C11 H11 0.9500 . ? C12 C13 1.39(3) . ? C12 H12 0.9500 . ? C13 C14 1.37(2) . ? C13 H13 0.9500 . ? C14 H14 0.9500 . ? C15 C20 1.37(2) . ? C15 C16 1.392(18) . ? C16 C17 1.379(19) . ? C16 H16 0.9500 . ? C17 C18 1.35(2) . ? C17 H17 0.9500 . ? C18 C19 1.37(3) . ? C18 H18 0.9500 . ? C19 C20 1.38(2) . ? C19 H19 0.9500 . ? C20 H20 0.9500 . ? C21 C22 1.392(18) . ? C21 C26 1.397(18) . ? C22 C23 1.385(18) . ? C22 H22 0.9500 . ? C23 C24 1.35(2) . ? C23 H23 0.9500 . ? C24 C25 1.38(2) . ? C24 H24 0.9500 . ? C25 C26 1.388(18) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 C33 1.49(3) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C34 1.48(3) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 C35 1.51(3) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P2 Pt1 P1 85.13(11) . . ? P2 Pt1 Si1 99.60(12) . . ? P1 Pt1 Si1 173.57(12) . . ? P2 Pt1 H1H 173(7) . . ? P1 Pt1 H1H 101(7) . . ? Si1 Pt1 H1H 75(7) . . ? C9 P1 C3 103.0(5) . . ? C9 P1 C1 106.3(6) . . ? C3 P1 C1 102.3(6) . . ? C9 P1 Pt1 122.6(4) . . ? C3 P1 Pt1 112.5(4) . . ? C1 P1 Pt1 108.3(4) . . ? C21 P2 C15 105.4(6) . . ? C21 P2 C2 104.9(6) . . ? C15 P2 C2 101.1(7) . . ? C21 P2 Pt1 114.1(5) . . ? C15 P2 Pt1 121.9(6) . . ? C2 P2 Pt1 107.4(4) . . ? C28 Si1 C27 103.3(7) . . ? C28 Si1 Pt1 120.0(5) . . ? C27 Si1 Pt1 112.7(5) . . ? C28 Si1 Si2 105.9(5) . . ? C27 Si1 Si2 102.5(5) . . ? Pt1 Si1 Si2 110.85(16) . . ? C31 Si2 C30 108.0(6) . . ? C31 Si2 C29 105.4(7) . . ? C30 Si2 C29 109.2(7) . . ? C31 Si2 Si1 110.4(5) . . ? C30 Si2 Si1 112.9(5) . . ? C29 Si2 Si1 110.6(5) . . ? C32 O1 C35 108.5(15) . . ? C2 C1 P1 108.5(9) . . ? C2 C1 H1A 110.0 . . ? P1 C1 H1A 110.0 . . ? C2 C1 H1B 110.0 . . ? P1 C1 H1B 110.0 . . ? H1A C1 H1B 108.4 . . ? C1 C2 P2 108.7(9) . . ? C1 C2 H2A 110.0 . . ? P2 C2 H2A 110.0 . . ? C1 C2 H2B 110.0 . . ? P2 C2 H2B 110.0 . . ? H2A C2 H2B 108.3 . . ? C8 C3 C4 118.1(11) . . ? C8 C3 P1 123.7(9) . . ? C4 C3 P1 118.1(9) . . ? C3 C4 C5 121.2(14) . . ? C3 C4 H4 119.4 . . ? C5 C4 H4 119.4 . . ? C4 C5 C6 118.7(14) . . ? C4 C5 H5 120.6 . . ? C6 C5 H5 120.6 . . ? C7 C6 C5 119.9(13) . . ? C7 C6 H6 120.0 . . ? C5 C6 H6 120.0 . . ? C6 C7 C8 120.5(12) . . ? C6 C7 H7 119.8 . . ? C8 C7 H7 119.8 . . ? C3 C8 C7 121.5(11) . . ? C3 C8 H8 119.2 . . ? C7 C8 H8 119.2 . . ? C10 C9 C14 116.6(13) . . ? C10 C9 P1 119.0(10) . . ? C14 C9 P1 124.4(12) . . ? C9 C10 C11 122.3(13) . . ? C9 C10 H10 118.8 . . ? C11 C10 H10 118.8 . . ? C12 C11 C10 118.1(16) . . ? C12 C11 H11 121.0 . . ? C10 C11 H11 121.0 . . ? C11 C12 C13 121.4(15) . . ? C11 C12 H12 119.3 . . ? C13 C12 H12 119.3 . . ? C14 C13 C12 119.7(14) . . ? C14 C13 H13 120.2 . . ? C12 C13 H13 120.2 . . ? C13 C14 C9 122.0(16) . . ? C13 C14 H14 119.0 . . ? C9 C14 H14 119.0 . . ? C20 C15 C16 118.3(14) . . ? C20 C15 P2 118.8(11) . . ? C16 C15 P2 122.8(10) . . ? C17 C16 C15 120.5(14) . . ? C17 C16 H16 119.7 . . ? C15 C16 H16 119.7 . . ? C18 C17 C16 120.2(15) . . ? C18 C17 H17 119.9 . . ? C16 C17 H17 119.9 . . ? C17 C18 C19 120.0(15) . . ? C17 C18 H18 120.0 . . ? C19 C18 H18 120.0 . . ? C18 C19 C20 120.5(16) . . ? C18 C19 H19 119.7 . . ? C20 C19 H19 119.7 . . ? C15 C20 C19 120.4(15) . . ? C15 C20 H20 119.8 . . ? C19 C20 H20 119.8 . . ? C22 C21 C26 118.7(12) . . ? C22 C21 P2 118.9(10) . . ? C26 C21 P2 122.3(10) . . ? C23 C22 C21 120.3(14) . . ? C23 C22 H22 119.8 . . ? C21 C22 H22 119.8 . . ? C24 C23 C22 120.8(15) . . ? C24 C23 H23 119.6 . . ? C22 C23 H23 119.6 . . ? C23 C24 C25 120.1(13) . . ? C23 C24 H24 120.0 . . ? C25 C24 H24 120.0 . . ? C24 C25 C26 120.4(14) . . ? C24 C25 H25 119.8 . . ? C26 C25 H25 119.8 . . ? C25 C26 C21 119.7(13) . . ? C25 C26 H26 120.2 . . ? C21 C26 H26 120.2 . . ? Si1 C27 H27A 109.5 . . ? Si1 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? Si1 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? Si1 C28 H28A 109.5 . . ? Si1 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? Si1 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? Si2 C29 H29A 109.5 . . ? Si2 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? Si2 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? Si2 C30 H30A 109.5 . . ? Si2 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? Si2 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? Si2 C31 H31A 109.5 . . ? Si2 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? Si2 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? O1 C32 C33 108.7(18) . . ? O1 C32 H32A 109.9 . . ? C33 C32 H32A 109.9 . . ? O1 C32 H32B 109.9 . . ? C33 C32 H32B 109.9 . . ? H32A C32 H32B 108.3 . . ? C34 C33 C32 98.4(18) . . ? C34 C33 H33A 112.1 . . ? C32 C33 H33A 112.1 . . ? C34 C33 H33B 112.1 . . ? C32 C33 H33B 112.1 . . ? H33A C33 H33B 109.7 . . ? C33 C34 C35 104.5(19) . . ? C33 C34 H34A 110.9 . . ? C35 C34 H34A 110.9 . . ? C33 C34 H34B 110.9 . . ? C35 C34 H34B 110.9 . . ? H34A C34 H34B 108.9 . . ? O1 C35 C34 104.8(19) . . ? O1 C35 H35A 110.8 . . ? C34 C35 H35A 110.8 . . ? O1 C35 H35B 110.8 . . ? C34 C35 H35B 110.8 . . ? H35A C35 H35B 108.9 . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 27.62 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 2.855 _refine_diff_density_min -8.000 _refine_diff_density_rms 0.219 #===END data_complex2b _database_code_depnum_ccdc_archive 'CCDC 761291' #TrackingRef 'CIF.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H52 P2 Pt Si2' _chemical_formula_weight 942.11 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' 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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/n ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.2600(4) _cell_length_b 41.553(2) _cell_length_c 11.4170(6) _cell_angle_alpha 90.00 _cell_angle_beta 101.692(3) _cell_angle_gamma 90.00 _cell_volume 4301.9(4) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 34573 _cell_measurement_theta_min 2.07 _cell_measurement_theta_max 27.97 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.455 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1904 _exptl_absorpt_coefficient_mu 3.424 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; This compound is synthesized under 243 K to avoid the conversion. Data completeness below 0.90 is attributed to the slight low thermal stability. ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method IP _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 34573 _diffrn_reflns_av_R_equivalents 0.090 _diffrn_reflns_av_sigmaI/netI 0.0590 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 54 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.07 _diffrn_reflns_theta_max 27.97 _reflns_number_total 9176 _reflns_number_gt 7216 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'DIP Image plate' _computing_cell_refinement 'HKL Scalepack' _computing_data_reduction 'maXus (Mackay et al., 1999)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep (Johnson, 1976)' _computing_publication_material ? _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^)+(0.0838P)^2^+8.1255P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9176 _refine_ls_number_parameters 481 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0780 _refine_ls_R_factor_gt 0.0568 _refine_ls_wR_factor_ref 0.1496 _refine_ls_wR_factor_gt 0.1354 _refine_ls_goodness_of_fit_ref 1.075 _refine_ls_restrained_S_all 1.075 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.10452(3) 0.162468(5) 0.91001(2) 0.02493(9) Uani 1 1 d . . . H1 H 0.172(9) 0.1740(18) 1.032(9) 0.030 Uiso 1 1 d . . . P1 P 0.19453(18) 0.20633(4) 0.82484(17) 0.0263(3) Uani 1 1 d . . . P2 P 0.00185(17) 0.14740(4) 0.71851(15) 0.0242(3) Uani 1 1 d . . . Si1 Si 0.02952(19) 0.11957(4) 1.02075(17) 0.0246(3) Uani 1 1 d . . . Si2 Si 0.2433(2) 0.09375(4) 1.12759(18) 0.0286(4) Uani 1 1 d . . . C1 C 0.1594(7) 0.20014(15) 0.6621(7) 0.0307(14) Uani 1 1 d . . . H1A H 0.1568 0.2206 0.6224 0.037 Uiso 1 1 d R . . H1B H 0.2367 0.1872 0.6421 0.037 Uiso 1 1 d R . . C2 C 0.0110(8) 0.18273(15) 0.6209(7) 0.0309(14) Uani 1 1 d . . . H2A H 0.0029 0.1755 0.5399 0.037 Uiso 1 1 d R . . H2B H -0.0688 0.1971 0.6253 0.037 Uiso 1 1 d R . . C3 C 0.3893(7) 0.21662(16) 0.8654(7) 0.0312(14) Uani 1 1 d . . . C4 C 0.4490(8) 0.24071(18) 0.8009(9) 0.0395(17) Uani 1 1 d . . . H4 H 0.3861 0.2521 0.7371 0.047 Uiso 1 1 d R . . C5 C 0.5986(9) 0.2480(2) 0.8300(11) 0.051(2) Uani 1 1 d . . . H5 H 0.6373 0.2649 0.7877 0.062 Uiso 1 1 d R . . C6 C 0.6897(9) 0.2309(2) 0.9207(11) 0.057(3) Uani 1 1 d . . . H6 H 0.7931 0.2358 0.9410 0.068 Uiso 1 1 d R . . C7 C 0.6349(10) 0.2074(2) 0.9806(10) 0.054(2) Uani 1 1 d . . . H7 H 0.6992 0.1953 1.0416 0.065 Uiso 1 1 d R . . C8 C 0.4820(9) 0.1996(2) 0.9554(8) 0.0422(18) Uani 1 1 d . . . H8 H 0.4419 0.1830 0.9980 0.051 Uiso 1 1 d R . . C9 C 0.1023(7) 0.24390(15) 0.8482(7) 0.0288(13) Uani 1 1 d . . . C10 C 0.0133(8) 0.26165(16) 0.7562(7) 0.0341(15) Uani 1 1 d . . . H10 H 0.0013 0.2544 0.6749 0.041 Uiso 1 1 d R . . C11 C -0.0573(9) 0.28937(18) 0.7825(9) 0.0412(18) Uani 1 1 d . . . H11 H -0.1202 0.3012 0.7199 0.049 Uiso 1 1 d R . . C12 C -0.0379(8) 0.30031(16) 0.8992(8) 0.0371(16) Uani 1 1 d . . . H12 H -0.0852 0.3198 0.9167 0.045 Uiso 1 1 d R . . C13 C 0.0508(10) 0.28290(18) 0.9929(9) 0.0434(19) Uani 1 1 d . . . H13 H 0.0641 0.2907 1.0736 0.052 Uiso 1 1 d R . . C14 C 0.1185(9) 0.25498(18) 0.9658(8) 0.0377(16) Uani 1 1 d . . . H14 H 0.1771 0.2430 1.0302 0.045 Uiso 1 1 d R . . C15 C 0.0956(7) 0.11532(14) 0.6534(6) 0.0262(12) Uani 1 1 d . . . C16 C 0.1836(7) 0.09383(15) 0.7336(7) 0.0310(14) Uani 1 1 d . . . H16 H 0.2000 0.0977 0.8182 0.037 Uiso 1 1 d R . . C17 C 0.2461(8) 0.06743(16) 0.6891(8) 0.0355(16) Uani 1 1 d . . . H17 H 0.3022 0.0521 0.7429 0.043 Uiso 1 1 d R . . C18 C 0.2284(8) 0.06248(17) 0.5653(8) 0.0388(17) Uani 1 1 d . . . H18 H 0.2713 0.0439 0.5360 0.047 Uiso 1 1 d R . . C19 C 0.1480(8) 0.08483(18) 0.4872(8) 0.0379(16) Uani 1 1 d . . . H19 H 0.1390 0.0822 0.4025 0.046 Uiso 1 1 d R . . C20 C 0.0801(8) 0.11094(17) 0.5315(7) 0.0327(15) Uani 1 1 d . . . H20 H 0.0230 0.1260 0.4773 0.039 Uiso 1 1 d R . . C21 C -0.1933(7) 0.13766(14) 0.6793(6) 0.0266(12) Uani 1 1 d . . . C22 C -0.2534(7) 0.11369(16) 0.5997(7) 0.0293(13) Uani 1 1 d . . . H22 H -0.1897 0.1002 0.5642 0.035 Uiso 1 1 d R . . C23 C -0.4066(7) 0.10934(15) 0.5725(7) 0.0288(13) Uani 1 1 d . . . H23 H -0.4489 0.0926 0.5183 0.035 Uiso 1 1 d R . . C24 C -0.4975(7) 0.12842(15) 0.6231(7) 0.0300(14) Uani 1 1 d . . . H24 H -0.6024 0.1256 0.6019 0.036 Uiso 1 1 d R . . C25 C -0.4383(8) 0.15186(17) 0.7048(8) 0.0355(15) Uani 1 1 d . . . H25 H -0.5020 0.1651 0.7411 0.043 Uiso 1 1 d R . . C26 C -0.2859(8) 0.15666(16) 0.7339(7) 0.0324(14) Uani 1 1 d . . . H26 H -0.2440 0.1727 0.7913 0.039 Uiso 1 1 d R . . C27 C -0.0970(7) 0.08759(15) 0.9353(7) 0.0284(13) Uani 1 1 d . . . C28 C -0.0414(8) 0.05948(16) 0.8906(7) 0.0345(15) Uani 1 1 d . . . H28 H 0.0632 0.0560 0.9053 0.041 Uiso 1 1 d R . . C29 C -0.1372(10) 0.03674(17) 0.8252(8) 0.0423(18) Uani 1 1 d . . . H29 H -0.0980 0.0177 0.7952 0.051 Uiso 1 1 d R . . C30 C -0.2878(10) 0.0418(2) 0.8039(8) 0.046(2) Uani 1 1 d . . . H30 H -0.3537 0.0260 0.7610 0.055 Uiso 1 1 d R . . C31 C -0.3444(9) 0.0689(2) 0.8448(8) 0.0396(17) Uani 1 1 d . . . H31 H -0.4490 0.0723 0.8284 0.048 Uiso 1 1 d R . . C32 C -0.2498(8) 0.09182(17) 0.9107(7) 0.0335(15) Uani 1 1 d . . . H32 H -0.2916 0.1108 0.9387 0.040 Uiso 1 1 d R . . C33 C -0.0741(7) 0.13178(15) 1.1452(6) 0.0259(12) Uani 1 1 d . . . C34 C -0.0682(9) 0.16306(16) 1.1907(7) 0.0346(15) Uani 1 1 d . . . H34 H -0.0080 0.1790 1.1629 0.042 Uiso 1 1 d R . . C35 C -0.1480(10) 0.17143(18) 1.2782(8) 0.0416(18) Uani 1 1 d . . . H35 H -0.1436 0.1930 1.3089 0.050 Uiso 1 1 d R . . C36 C -0.2338(9) 0.14833(18) 1.3204(8) 0.0390(17) Uani 1 1 d . . . H36 H -0.2915 0.1545 1.3777 0.047 Uiso 1 1 d R . . C37 C -0.2349(8) 0.11707(18) 1.2781(7) 0.0351(15) Uani 1 1 d . . . H37 H -0.2909 0.1008 1.3085 0.042 Uiso 1 1 d R . . C38 C -0.1559(7) 0.10898(16) 1.1922(7) 0.0317(14) Uani 1 1 d . . . H38 H -0.1580 0.0871 1.1651 0.038 Uiso 1 1 d R . . C39 C 0.1931(9) 0.05370(16) 1.1871(7) 0.0349(15) Uani 1 1 d . . . H39A H 0.2804 0.0433 1.2305 0.042 Uiso 1 1 d R . . H39B H 0.1475 0.0403 1.1215 0.042 Uiso 1 1 d R . . H39C H 0.1255 0.0572 1.2394 0.042 Uiso 1 1 d R . . C40 C 0.3927(9) 0.0860(2) 1.0406(8) 0.0419(18) Uani 1 1 d . . . H40A H 0.4742 0.0756 1.0917 0.050 Uiso 1 1 d R . . H40B H 0.4251 0.1060 1.0128 0.050 Uiso 1 1 d R . . H40C H 0.3548 0.0724 0.9734 0.050 Uiso 1 1 d R . . C41 C 0.3245(8) 0.12085(17) 1.2562(8) 0.0375(16) Uani 1 1 d . . . H41A H 0.4120 0.1112 1.3023 0.045 Uiso 1 1 d R . . H41B H 0.2534 0.1238 1.3059 0.045 Uiso 1 1 d R . . H41C H 0.3486 0.1413 1.2263 0.045 Uiso 1 1 d R . . C42 C 0.7392(9) 0.01999(16) 0.2435(8) 0.0354(15) Uani 1 1 d . . . C43 C 0.8574(9) 0.02337(18) 0.3383(9) 0.0438(19) Uani 1 1 d . . . H43 H 0.9565 0.0219 0.3255 0.053 Uiso 1 1 d R . . C44 C 0.8360(9) 0.02885(18) 0.4558(9) 0.0429(19) Uani 1 1 d . . . H44 H 0.9194 0.0317 0.5203 0.052 Uiso 1 1 d R . . C45 C 0.6956(10) 0.03018(19) 0.4788(8) 0.0440(18) Uani 1 1 d . . . H45 H 0.6828 0.0341 0.5590 0.053 Uiso 1 1 d R . . C46 C 0.5752(11) 0.0261(2) 0.3845(9) 0.050(2) Uani 1 1 d . . . H46 H 0.4766 0.0264 0.3990 0.060 Uiso 1 1 d R . . C47 C 0.5976(9) 0.02135(19) 0.2683(9) 0.0427(19) Uani 1 1 d . . . H47 H 0.5127 0.0190 0.2048 0.051 Uiso 1 1 d R . . C48 C 0.7577(13) 0.0144(2) 0.1202(9) 0.053(2) Uani 1 1 d . . . H48A H 0.6621 0.0128 0.0687 0.064 Uiso 1 1 d R . . H48B H 0.8117 -0.0051 0.1160 0.064 Uiso 1 1 d R . . H48C H 0.8103 0.0322 0.0950 0.064 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.02687(13) 0.02480(13) 0.02243(13) -0.00094(9) 0.00334(9) -0.00236(9) P1 0.0257(7) 0.0250(7) 0.0277(8) -0.0012(6) 0.0041(6) -0.0045(6) P2 0.0253(7) 0.0262(7) 0.0205(8) -0.0017(6) 0.0032(6) -0.0007(6) Si1 0.0264(8) 0.0251(7) 0.0225(8) 0.0000(6) 0.0054(6) -0.0018(6) Si2 0.0280(8) 0.0318(8) 0.0261(9) 0.0016(7) 0.0054(7) 0.0004(7) C1 0.027(3) 0.029(3) 0.035(4) -0.004(3) 0.005(3) 0.001(2) C2 0.037(3) 0.029(3) 0.027(3) 0.001(2) 0.007(3) -0.001(2) C3 0.024(3) 0.035(3) 0.037(4) -0.009(3) 0.011(3) 0.001(2) C4 0.028(3) 0.039(4) 0.054(5) -0.001(3) 0.013(3) -0.005(3) C5 0.031(4) 0.048(4) 0.078(7) -0.015(4) 0.020(4) -0.011(3) C6 0.027(3) 0.069(6) 0.077(8) -0.038(5) 0.014(4) -0.014(4) C7 0.040(4) 0.077(6) 0.041(5) -0.014(4) -0.006(4) 0.010(4) C8 0.034(4) 0.064(5) 0.029(4) -0.011(3) 0.007(3) 0.004(3) C9 0.027(3) 0.025(3) 0.035(4) 0.005(2) 0.007(3) -0.003(2) C10 0.038(3) 0.034(3) 0.030(4) 0.000(3) 0.005(3) 0.000(3) C11 0.042(4) 0.035(4) 0.047(5) 0.006(3) 0.011(4) 0.004(3) C12 0.040(4) 0.026(3) 0.049(5) -0.004(3) 0.017(3) 0.001(3) C13 0.052(5) 0.037(4) 0.042(5) -0.010(3) 0.012(4) -0.001(3) C14 0.040(4) 0.043(4) 0.031(4) -0.001(3) 0.011(3) 0.005(3) C15 0.025(3) 0.029(3) 0.025(3) -0.002(2) 0.005(2) -0.003(2) C16 0.027(3) 0.033(3) 0.032(4) -0.001(3) 0.004(3) -0.001(2) C17 0.029(3) 0.029(3) 0.051(5) 0.001(3) 0.014(3) 0.004(2) C18 0.032(3) 0.033(3) 0.053(5) -0.015(3) 0.015(3) -0.003(3) C19 0.034(3) 0.050(4) 0.033(4) -0.015(3) 0.013(3) -0.011(3) C20 0.029(3) 0.038(3) 0.029(4) -0.006(3) 0.003(3) -0.001(3) C21 0.025(3) 0.027(3) 0.027(3) 0.002(2) 0.005(2) 0.005(2) C22 0.027(3) 0.035(3) 0.029(3) -0.002(3) 0.013(3) -0.001(2) C23 0.025(3) 0.033(3) 0.027(3) -0.003(2) 0.004(3) -0.004(2) C24 0.021(3) 0.033(3) 0.034(4) 0.005(3) 0.001(3) 0.000(2) C25 0.032(3) 0.037(3) 0.039(4) -0.002(3) 0.011(3) 0.008(3) C26 0.027(3) 0.033(3) 0.037(4) -0.005(3) 0.004(3) 0.000(2) C27 0.029(3) 0.028(3) 0.029(3) 0.003(2) 0.007(3) -0.002(2) C28 0.039(3) 0.032(3) 0.035(4) -0.008(3) 0.014(3) -0.007(3) C29 0.060(5) 0.030(3) 0.040(4) -0.008(3) 0.016(4) -0.014(3) C30 0.053(5) 0.052(4) 0.034(4) -0.007(3) 0.009(4) -0.028(4) C31 0.033(3) 0.056(4) 0.028(4) 0.005(3) 0.001(3) -0.014(3) C32 0.030(3) 0.038(3) 0.032(4) 0.005(3) 0.004(3) -0.006(3) C33 0.024(3) 0.030(3) 0.021(3) 0.001(2) 0.000(2) 0.002(2) C34 0.045(4) 0.029(3) 0.032(4) 0.002(3) 0.013(3) 0.003(3) C35 0.061(5) 0.035(3) 0.031(4) -0.004(3) 0.015(4) 0.015(3) C36 0.037(4) 0.047(4) 0.030(4) 0.004(3) 0.001(3) 0.017(3) C37 0.034(3) 0.045(4) 0.029(4) -0.005(3) 0.011(3) -0.005(3) C38 0.030(3) 0.036(3) 0.029(4) -0.001(3) 0.004(3) 0.003(3) C39 0.043(4) 0.030(3) 0.033(4) 0.006(3) 0.013(3) 0.006(3) C40 0.035(4) 0.056(5) 0.033(4) 0.001(3) 0.002(3) 0.003(3) C41 0.032(3) 0.039(4) 0.038(4) -0.001(3) 0.001(3) -0.003(3) C42 0.041(4) 0.029(3) 0.039(4) 0.002(3) 0.015(3) 0.000(3) C43 0.037(4) 0.041(4) 0.055(6) 0.010(3) 0.015(4) -0.002(3) C44 0.041(4) 0.040(4) 0.045(5) -0.001(3) 0.002(4) -0.009(3) C45 0.055(5) 0.046(4) 0.033(4) -0.005(3) 0.012(4) 0.000(4) C46 0.050(5) 0.058(5) 0.042(5) 0.004(4) 0.013(4) 0.003(4) C47 0.038(4) 0.049(4) 0.039(5) -0.003(3) 0.002(3) -0.004(3) C48 0.079(6) 0.049(4) 0.037(5) 0.005(4) 0.024(4) -0.001(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 P2 2.2877(16) . ? Pt1 P1 2.3000(17) . ? Pt1 Si1 2.3694(18) . ? Pt1 H1 1.49(9) . ? P1 C3 1.820(7) . ? P1 C9 1.825(7) . ? P1 C1 1.838(8) . ? P2 C21 1.817(7) . ? P2 C15 1.829(7) . ? P2 C2 1.855(7) . ? Si1 C27 1.905(7) . ? Si1 C33 1.936(8) . ? Si1 Si2 2.362(2) . ? Si2 C41 1.882(8) . ? Si2 C40 1.886(10) . ? Si2 C39 1.890(7) . ? C1 C2 1.540(9) . ? C1 H1A 0.9601 . ? C1 H1B 0.9599 . ? C2 H2A 0.9600 . ? C2 H2B 0.9601 . ? C3 C8 1.392(11) . ? C3 C4 1.419(11) . ? C4 C5 1.391(10) . ? C4 H4 0.9600 . ? C5 C6 1.391(16) . ? C5 H5 0.9599 . ? C6 C7 1.350(17) . ? C6 H6 0.9600 . ? C7 C8 1.424(12) . ? C7 H7 0.9600 . ? C8 H8 0.9599 . ? C9 C14 1.398(11) . ? C9 C10 1.405(9) . ? C10 C11 1.388(11) . ? C10 H10 0.9600 . ? C11 C12 1.385(13) . ? C11 H11 0.9601 . ? C12 C13 1.410(12) . ? C12 H12 0.9600 . ? C13 C14 1.383(11) . ? C13 H13 0.9600 . ? C14 H14 0.9600 . ? C15 C20 1.382(10) . ? C15 C16 1.413(9) . ? C16 C17 1.384(10) . ? C16 H16 0.9599 . ? C17 C18 1.405(13) . ? C17 H17 0.9601 . ? C18 C19 1.394(12) . ? C18 H18 0.9600 . ? C19 C20 1.399(11) . ? C19 H19 0.9600 . ? C20 H20 0.9602 . ? C21 C22 1.387(9) . ? C21 C26 1.402(10) . ? C22 C23 1.401(9) . ? C22 H22 0.9600 . ? C23 C24 1.367(10) . ? C23 H23 0.9599 . ? C24 C25 1.383(10) . ? C24 H24 0.9600 . ? C25 C26 1.397(10) . ? C25 H25 0.9601 . ? C26 H26 0.9600 . ? C27 C32 1.397(9) . ? C27 C28 1.412(10) . ? C28 C29 1.403(10) . ? C28 H28 0.9600 . ? C29 C30 1.383(13) . ? C29 H29 0.9600 . ? C30 C31 1.366(14) . ? C30 H30 0.9601 . ? C31 C32 1.404(10) . ? C31 H31 0.9600 . ? C32 H32 0.9599 . ? C33 C38 1.387(10) . ? C33 C34 1.397(9) . ? C34 C35 1.402(12) . ? C34 H34 0.9600 . ? C35 C36 1.392(14) . ? C35 H35 0.9603 . ? C36 C37 1.385(11) . ? C36 H36 0.9599 . ? C37 C38 1.379(11) . ? C37 H37 0.9600 . ? C38 H38 0.9599 . ? C39 H39A 0.9600 . ? C39 H39B 0.9598 . ? C39 H39C 0.9599 . ? C40 H40A 0.9599 . ? C40 H40B 0.9599 . ? C40 H40C 0.9602 . ? C41 H41A 0.9600 . ? C41 H41B 0.9600 . ? C41 H41C 0.9598 . ? C42 C43 1.382(12) . ? C42 C47 1.398(12) . ? C42 C48 1.471(13) . ? C43 C44 1.414(14) . ? C43 H43 0.9599 . ? C44 C45 1.379(13) . ? C44 H44 0.9600 . ? C45 C46 1.395(12) . ? C45 H45 0.9600 . ? C46 C47 1.398(14) . ? C46 H46 0.9599 . ? C47 H47 0.9600 . ? C48 H48A 0.9600 . ? C48 H48B 0.9597 . ? C48 H48C 0.9602 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P2 Pt1 P1 85.92(6) . . ? P2 Pt1 Si1 101.19(6) . . ? P1 Pt1 Si1 172.85(6) . . ? P2 Pt1 H1 177(3) . . ? P1 Pt1 H1 91(3) . . ? Si1 Pt1 H1 82(3) . . ? C3 P1 C9 103.4(3) . . ? C3 P1 C1 104.7(4) . . ? C9 P1 C1 106.0(3) . . ? C3 P1 Pt1 120.3(3) . . ? C9 P1 Pt1 113.3(2) . . ? C1 P1 Pt1 108.1(2) . . ? C21 P2 C15 105.5(3) . . ? C21 P2 C2 101.1(3) . . ? C15 P2 C2 104.5(3) . . ? C21 P2 Pt1 119.8(3) . . ? C15 P2 Pt1 116.6(2) . . ? C2 P2 Pt1 107.3(2) . . ? C27 Si1 C33 102.4(3) . . ? C27 Si1 Si2 108.2(2) . . ? C33 Si1 Si2 103.20(19) . . ? C27 Si1 Pt1 117.9(2) . . ? C33 Si1 Pt1 115.9(2) . . ? Si2 Si1 Pt1 108.16(8) . . ? C41 Si2 C40 107.0(4) . . ? C41 Si2 C39 109.5(4) . . ? C40 Si2 C39 107.4(4) . . ? C41 Si2 Si1 106.9(2) . . ? C40 Si2 Si1 115.6(3) . . ? C39 Si2 Si1 110.1(2) . . ? C2 C1 P1 109.8(5) . . ? C2 C1 H1A 109.6 . . ? P1 C1 H1A 109.6 . . ? C2 C1 H1B 109.0 . . ? P1 C1 H1B 109.3 . . ? H1A C1 H1B 109.5 . . ? C1 C2 P2 109.6(5) . . ? C1 C2 H2A 109.3 . . ? P2 C2 H2A 109.2 . . ? C1 C2 H2B 109.8 . . ? P2 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C8 C3 C4 119.7(7) . . ? C8 C3 P1 119.9(6) . . ? C4 C3 P1 120.3(6) . . ? C5 C4 C3 120.3(8) . . ? C5 C4 H4 119.7 . . ? C3 C4 H4 120.1 . . ? C4 C5 C6 119.4(9) . . ? C4 C5 H5 119.6 . . ? C6 C5 H5 121.0 . . ? C7 C6 C5 120.9(8) . . ? C7 C6 H6 119.4 . . ? C5 C6 H6 119.7 . . ? C6 C7 C8 121.5(9) . . ? C6 C7 H7 120.2 . . ? C8 C7 H7 118.2 . . ? C3 C8 C7 118.2(9) . . ? C3 C8 H8 119.7 . . ? C7 C8 H8 122.1 . . ? C14 C9 C10 118.5(7) . . ? C14 C9 P1 117.4(5) . . ? C10 C9 P1 124.1(6) . . ? C11 C10 C9 120.3(8) . . ? C11 C10 H10 120.0 . . ? C9 C10 H10 119.6 . . ? C12 C11 C10 120.4(7) . . ? C12 C11 H11 119.3 . . ? C10 C11 H11 120.3 . . ? C11 C12 C13 120.3(7) . . ? C11 C12 H12 120.1 . . ? C13 C12 H12 119.7 . . ? C14 C13 C12 118.8(8) . . ? C14 C13 H13 121.5 . . ? C12 C13 H13 119.8 . . ? C13 C14 C9 121.7(7) . . ? C13 C14 H14 118.4 . . ? C9 C14 H14 119.9 . . ? C20 C15 C16 119.9(6) . . ? C20 C15 P2 123.0(5) . . ? C16 C15 P2 117.2(6) . . ? C17 C16 C15 119.5(7) . . ? C17 C16 H16 120.5 . . ? C15 C16 H16 120.0 . . ? C16 C17 C18 120.9(7) . . ? C16 C17 H17 120.2 . . ? C18 C17 H17 118.9 . . ? C19 C18 C17 119.0(7) . . ? C19 C18 H18 121.2 . . ? C17 C18 H18 119.8 . . ? C18 C19 C20 120.4(8) . . ? C18 C19 H19 119.6 . . ? C20 C19 H19 120.0 . . ? C15 C20 C19 120.3(7) . . ? C15 C20 H20 119.7 . . ? C19 C20 H20 120.1 . . ? C22 C21 C26 119.7(6) . . ? C22 C21 P2 124.6(5) . . ? C26 C21 P2 115.6(5) . . ? C21 C22 C23 119.5(6) . . ? C21 C22 H22 119.8 . . ? C23 C22 H22 120.8 . . ? C24 C23 C22 120.9(6) . . ? C24 C23 H23 119.1 . . ? C22 C23 H23 120.0 . . ? C23 C24 C25 120.0(6) . . ? C23 C24 H24 120.1 . . ? C25 C24 H24 119.9 . . ? C24 C25 C26 120.3(7) . . ? C24 C25 H25 120.1 . . ? C26 C25 H25 119.6 . . ? C25 C26 C21 119.6(6) . . ? C25 C26 H26 120.7 . . ? C21 C26 H26 119.7 . . ? C32 C27 C28 117.4(6) . . ? C32 C27 Si1 120.5(5) . . ? C28 C27 Si1 122.1(5) . . ? C29 C28 C27 120.8(7) . . ? C29 C28 H28 119.9 . . ? C27 C28 H28 119.4 . . ? C30 C29 C28 119.9(8) . . ? C30 C29 H29 120.2 . . ? C28 C29 H29 120.0 . . ? C31 C30 C29 120.5(7) . . ? C31 C30 H30 119.4 . . ? C29 C30 H30 120.1 . . ? C30 C31 C32 120.2(8) . . ? C30 C31 H31 119.8 . . ? C32 C31 H31 120.0 . . ? C27 C32 C31 121.2(7) . . ? C27 C32 H32 119.8 . . ? C31 C32 H32 119.0 . . ? C38 C33 C34 118.4(7) . . ? C38 C33 Si1 119.7(5) . . ? C34 C33 Si1 121.9(6) . . ? C33 C34 C35 120.6(7) . . ? C33 C34 H34 120.0 . . ? C35 C34 H34 119.3 . . ? C36 C35 C34 119.7(7) . . ? C36 C35 H35 120.2 . . ? C34 C35 H35 120.2 . . ? C37 C36 C35 119.4(9) . . ? C37 C36 H36 121.4 . . ? C35 C36 H36 119.2 . . ? C38 C37 C36 120.6(8) . . ? C38 C37 H37 119.2 . . ? C36 C37 H37 120.2 . . ? C37 C38 C33 121.2(7) . . ? C37 C38 H38 118.7 . . ? C33 C38 H38 120.0 . . ? Si2 C39 H39A 109.7 . . ? Si2 C39 H39B 109.4 . . ? H39A C39 H39B 109.5 . . ? Si2 C39 H39C 109.3 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? Si2 C40 H40A 109.1 . . ? Si2 C40 H40B 109.8 . . ? H40A C40 H40B 109.5 . . ? Si2 C40 H40C 109.4 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? Si2 C41 H41A 109.7 . . ? Si2 C41 H41B 109.0 . . ? H41A C41 H41B 109.5 . . ? Si2 C41 H41C 109.7 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C43 C42 C47 117.6(9) . . ? C43 C42 C48 122.6(9) . . ? C47 C42 C48 119.7(8) . . ? C42 C43 C44 121.3(8) . . ? C42 C43 H43 120.3 . . ? C44 C43 H43 118.5 . . ? C45 C44 C43 120.4(7) . . ? C45 C44 H44 119.5 . . ? C43 C44 H44 120.1 . . ? C44 C45 C46 119.0(9) . . ? C44 C45 H45 119.4 . . ? C46 C45 H45 121.5 . . ? C45 C46 C47 120.1(9) . . ? C45 C46 H46 120.3 . . ? C47 C46 H46 119.6 . . ? C42 C47 C46 121.6(8) . . ? C42 C47 H47 120.1 . . ? C46 C47 H47 118.4 . . ? C42 C48 H48A 109.0 . . ? C42 C48 H48B 110.1 . . ? H48A C48 H48B 109.5 . . ? C42 C48 H48C 109.3 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.887 _diffrn_reflns_theta_full 27.97 _diffrn_measured_fraction_theta_full 0.887 _refine_diff_density_max 0.903 _refine_diff_density_min -3.023 _refine_diff_density_rms 0.196 #===END data_complex2c _database_code_depnum_ccdc_archive 'CCDC 761292' #TrackingRef 'CIF.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C35 H40 P2 Pt Si2' _chemical_formula_weight 773.88 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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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)/n ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.133(4) _cell_length_b 31.933(12) _cell_length_c 11.720(4) _cell_angle_alpha 90.00 _cell_angle_beta 104.992(5) _cell_angle_gamma 90.00 _cell_volume 3302(2) _cell_formula_units_Z 4 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 1177 _cell_measurement_theta_min 2.21 _cell_measurement_theta_max 18.36 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.06 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.557 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1544 _exptl_absorpt_coefficient_mu 4.442 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7764 _exptl_absorpt_correction_T_max 0.9164 _exptl_absorpt_process_details ; SADABS Sheldrick 1996 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker TXS fine-focus rotating anode' _diffrn_radiation_monochromator 'Bruker Helios multilayer confocal mirror' _diffrn_measurement_device_type 'Bruker APEXII CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 8.333 _diffrn_reflns_number 16071 _diffrn_reflns_av_R_equivalents 0.1189 _diffrn_reflns_av_sigmaI/netI 0.1635 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 38 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.28 _diffrn_reflns_theta_max 25.47 _reflns_number_total 6084 _reflns_number_gt 3533 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker AXS, 2006)' _computing_cell_refinement 'APEX2 (Bruker AXS, 2006)' _computing_data_reduction 'SAINT (Bruker AXS, 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XSHEL (Bruker AXS,2002)' _computing_publication_material 'XCIF (Bruker AXS, 2001)' _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. This compound is obtained as a twin crystal. Each reflection peak is separated by the reciprocal space is carried out the refinement. The high Rint originates from the overlap of peaks. ; _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^)+(0.0302P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00061(9) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 6084 _refine_ls_number_parameters 371 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1239 _refine_ls_R_factor_gt 0.0530 _refine_ls_wR_factor_ref 0.1082 _refine_ls_wR_factor_gt 0.0886 _refine_ls_goodness_of_fit_ref 0.934 _refine_ls_restrained_S_all 0.934 _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 C1 C 0.9656(10) 0.2098(3) 0.6075(8) 0.014(2) Uani 1 1 d . . . C2 C 1.0653(11) 0.1945(3) 0.7107(8) 0.017(2) Uani 1 1 d . . . H3 H 1.0266 0.1780 0.7638 0.020 Uiso 1 1 calc R . . C3 C 1.2204(11) 0.2029(3) 0.7369(9) 0.022(3) Uani 1 1 d . . . H28 H 1.2858 0.1929 0.8084 0.027 Uiso 1 1 calc R . . C4 C 1.2781(12) 0.2256(3) 0.6602(9) 0.025(3) Uani 1 1 d . . . H20 H 1.3837 0.2312 0.6780 0.030 Uiso 1 1 calc R . . C5 C 1.1837(12) 0.2404(4) 0.5574(9) 0.030(3) Uani 1 1 d . . . H24 H 1.2245 0.2561 0.5040 0.036 Uiso 1 1 calc R . . C6 C 1.0308(11) 0.2326(3) 0.5309(9) 0.020(2) Uani 1 1 d . . . H7 H 0.9676 0.2430 0.4589 0.024 Uiso 1 1 calc R . . C7 C 0.6802(11) 0.2469(3) 0.6042(9) 0.015(2) Uani 1 1 d . . . C8 C 0.7003(11) 0.2612(3) 0.7179(9) 0.020(3) Uani 1 1 d . . . H8 H 0.7651 0.2460 0.7809 0.024 Uiso 1 1 calc R . . C9 C 0.6283(11) 0.2974(3) 0.7440(9) 0.023(3) Uani 1 1 d . . . H16 H 0.6475 0.3070 0.8232 0.028 Uiso 1 1 calc R . . C10 C 0.5297(12) 0.3191(3) 0.6548(9) 0.024(3) Uani 1 1 d . . . H37 H 0.4785 0.3433 0.6720 0.028 Uiso 1 1 calc R . . C12 C 0.5794(11) 0.2693(3) 0.5125(8) 0.020(3) Uani 1 1 d . . . H36 H 0.5615 0.2600 0.4330 0.024 Uiso 1 1 calc R . . C13 C 0.7044(11) 0.1888(3) 0.4152(8) 0.017(2) Uani 1 1 d . . . H19A H 0.7005 0.2158 0.3732 0.020 Uiso 1 1 calc R . . H19B H 0.7780 0.1703 0.3906 0.020 Uiso 1 1 calc R . . C14 C 0.5462(12) 0.1682(3) 0.3823(8) 0.024(3) Uani 1 1 d . . . H11A H 0.5222 0.1582 0.2996 0.029 Uiso 1 1 calc R . . H11B H 0.4685 0.1890 0.3891 0.029 Uiso 1 1 calc R . . C15 C 0.6191(11) 0.0801(3) 0.4159(9) 0.019(2) Uani 1 1 d . . . C16 C 0.6216(12) 0.0779(4) 0.2972(9) 0.027(3) Uani 1 1 d . . . H21 H 0.5821 0.1004 0.2455 0.033 Uiso 1 1 calc R . . C17 C 0.6816(12) 0.0428(4) 0.2536(10) 0.029(3) Uani 1 1 d . . . H25 H 0.6843 0.0417 0.1732 0.035 Uiso 1 1 calc R . . C18 C 0.7361(12) 0.0104(4) 0.3279(11) 0.033(3) Uani 1 1 d . . . H31 H 0.7761 -0.0135 0.2980 0.040 Uiso 1 1 calc R . . C19 C 0.7348(13) 0.0113(4) 0.4438(10) 0.037(3) Uani 1 1 d . . . H33 H 0.7740 -0.0115 0.4948 0.044 Uiso 1 1 calc R . . C20 C 0.6739(14) 0.0468(4) 0.4867(10) 0.037(3) Uani 1 1 d . . . H12 H 0.6711 0.0475 0.5671 0.044 Uiso 1 1 calc R . . C21 C 0.3416(11) 0.1108(3) 0.4562(9) 0.018(2) Uani 1 1 d . . . C22 C 0.2705(13) 0.1206(3) 0.5451(9) 0.025(3) Uani 1 1 d . . . H14 H 0.3256 0.1338 0.6158 0.030 Uiso 1 1 calc R . . C23 C 0.1209(12) 0.1109(3) 0.5291(9) 0.027(3) Uani 1 1 d . . . H26 H 0.0733 0.1169 0.5902 0.032 Uiso 1 1 calc R . . C24 C 0.0355(12) 0.0921(3) 0.4243(10) 0.029(3) Uani 1 1 d . . . H15 H -0.0685 0.0854 0.4140 0.035 Uiso 1 1 calc R . . C25 C 0.1084(12) 0.0837(3) 0.3361(9) 0.028(3) Uani 1 1 d . . . H22 H 0.0533 0.0716 0.2636 0.033 Uiso 1 1 calc R . . C26 C 0.2589(11) 0.0926(3) 0.3532(9) 0.021(3) Uani 1 1 d . . . H32 H 0.3073 0.0862 0.2927 0.026 Uiso 1 1 calc R . . C27 C 0.5002(11) 0.1121(3) 0.8849(8) 0.019(2) Uani 1 1 d . . . C28 C 0.5668(11) 0.1430(4) 0.9635(8) 0.023(2) Uani 1 1 d . . . H5 H 0.6625 0.1539 0.9604 0.028 Uiso 1 1 calc R . . C29 C 0.4981(12) 0.1585(3) 1.0463(9) 0.028(3) Uani 1 1 d . . . H30 H 0.5494 0.1787 1.1020 0.033 Uiso 1 1 calc R . . C30 C 0.3546(12) 0.1450(4) 1.0493(8) 0.030(3) Uani 1 1 d . . . H10 H 0.3063 0.1564 1.1049 0.036 Uiso 1 1 calc R . . C31 C 0.2836(13) 0.1148(3) 0.9707(10) 0.031(3) Uani 1 1 d . . . H34 H 0.1852 0.1054 0.9717 0.037 Uiso 1 1 calc R . . C32 C 0.3547(12) 0.0980(4) 0.8898(9) 0.027(3) Uani 1 1 d . . . H23 H 0.3053 0.0767 0.8370 0.032 Uiso 1 1 calc R . . C33 C 0.9321(12) 0.0334(4) 0.7901(9) 0.032(3) Uani 1 1 d . . . H27A H 1.0130 0.0160 0.8387 0.049 Uiso 1 1 calc R . . H27B H 0.9756 0.0594 0.7692 0.049 Uiso 1 1 calc R . . H27C H 0.8822 0.0181 0.7179 0.049 Uiso 1 1 calc R . . C34 C 0.8928(11) 0.0738(4) 1.0140(8) 0.027(3) Uani 1 1 d . . . H39A H 0.8243 0.0785 1.0648 0.040 Uiso 1 1 calc R . . H39B H 0.9297 0.1008 0.9931 0.040 Uiso 1 1 calc R . . H39C H 0.9789 0.0567 1.0561 0.040 Uiso 1 1 calc R . . C35 C 0.7114(13) -0.0033(3) 0.9188(10) 0.038(3) Uani 1 1 d . . . H40A H 0.7948 -0.0208 0.9634 0.058 Uiso 1 1 calc R . . H40B H 0.6561 -0.0182 0.8477 0.058 Uiso 1 1 calc R . . H40C H 0.6424 0.0030 0.9681 0.058 Uiso 1 1 calc R . . C11S C 0.5064(11) 0.3050(3) 0.5385(9) 0.020(3) Uani 1 1 d . . . H38S H 0.4398 0.3200 0.4762 0.024 Uiso 1 1 calc R . . H1S H 0.780(10) 0.157(3) 0.788(7) 0.024 Uiso 1 1 d . . . P1 P 0.7665(3) 0.19765(9) 0.5757(2) 0.0164(6) Uani 1 1 d . . . P2 P 0.5443(3) 0.12376(9) 0.4824(2) 0.0171(6) Uani 1 1 d . . . Pt1 Pt 0.68183(5) 0.142428(13) 0.66509(3) 0.01602(14) Uani 1 1 d . . . Si1 Si 0.5946(3) 0.08965(9) 0.7712(3) 0.0192(7) Uani 1 1 d . . . Si2 Si 0.7884(3) 0.04597(10) 0.8761(3) 0.0232(7) Uani 1 1 d . . . H2S H 0.480(10) 0.060(3) 0.698(7) 0.028 Uiso 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 C1 0.010(5) 0.020(6) 0.014(5) -0.004(5) 0.007(4) 0.001(5) C2 0.021(6) 0.025(7) 0.007(5) -0.002(5) 0.007(4) -0.002(5) C3 0.012(6) 0.030(7) 0.024(6) -0.012(5) 0.002(5) 0.006(5) C4 0.023(7) 0.032(7) 0.027(7) -0.021(6) 0.016(5) -0.011(5) C5 0.020(7) 0.040(8) 0.028(7) -0.002(6) 0.006(5) -0.007(6) C6 0.022(6) 0.019(6) 0.021(6) 0.001(5) 0.010(5) 0.003(5) C7 0.006(5) 0.026(7) 0.015(6) -0.006(5) 0.004(4) -0.009(5) C8 0.021(6) 0.019(7) 0.022(6) 0.004(5) 0.008(5) -0.004(5) C9 0.014(6) 0.040(8) 0.017(6) -0.006(5) 0.007(5) -0.006(5) C10 0.021(6) 0.019(7) 0.031(7) 0.001(5) 0.007(5) -0.005(5) C12 0.017(6) 0.028(7) 0.011(5) -0.004(5) -0.002(5) -0.005(5) C13 0.022(6) 0.015(6) 0.014(5) 0.001(5) 0.007(5) -0.002(5) C14 0.033(7) 0.029(7) 0.013(6) 0.003(5) 0.010(5) 0.001(6) C15 0.014(6) 0.019(7) 0.021(6) 0.002(5) 0.003(5) 0.000(5) C16 0.022(7) 0.032(8) 0.027(7) 0.003(6) 0.006(5) -0.009(6) C17 0.029(7) 0.037(8) 0.025(7) -0.014(6) 0.012(5) -0.008(6) C18 0.025(7) 0.026(7) 0.056(9) -0.010(7) 0.022(6) -0.002(6) C19 0.041(8) 0.036(8) 0.042(8) 0.009(7) 0.025(6) 0.004(6) C20 0.046(8) 0.037(8) 0.033(7) -0.011(6) 0.022(6) 0.001(7) C21 0.014(6) 0.024(7) 0.018(6) 0.004(5) 0.007(5) 0.007(5) C22 0.035(7) 0.012(6) 0.031(7) -0.008(5) 0.015(6) -0.010(5) C23 0.023(7) 0.032(8) 0.029(7) -0.007(6) 0.013(5) 0.002(5) C24 0.016(7) 0.023(7) 0.046(8) 0.000(6) 0.003(6) 0.003(5) C25 0.032(7) 0.020(7) 0.026(7) -0.006(5) -0.001(6) -0.005(5) C26 0.018(6) 0.021(7) 0.028(6) 0.000(5) 0.012(5) -0.003(5) C27 0.015(6) 0.027(7) 0.013(6) -0.002(5) 0.002(5) -0.001(5) C28 0.022(6) 0.031(7) 0.021(6) 0.011(6) 0.011(4) 0.004(6) C29 0.029(7) 0.025(7) 0.028(7) -0.003(5) 0.006(5) -0.003(5) C30 0.040(7) 0.033(7) 0.021(6) 0.012(6) 0.014(5) 0.026(7) C31 0.027(7) 0.028(8) 0.045(8) 0.004(6) 0.026(6) 0.002(6) C32 0.032(7) 0.022(7) 0.021(6) 0.001(5) -0.001(5) -0.007(6) C33 0.025(7) 0.040(8) 0.032(7) -0.004(6) 0.005(5) 0.012(6) C34 0.014(6) 0.045(8) 0.021(6) 0.014(6) 0.005(5) -0.003(5) C35 0.032(8) 0.025(8) 0.047(8) 0.004(6) -0.010(6) 0.008(6) C11S 0.014(6) 0.016(6) 0.033(7) 0.013(5) 0.008(5) 0.010(5) P1 0.0133(15) 0.0177(17) 0.0183(15) -0.0008(13) 0.0041(12) -0.0006(12) P2 0.0154(15) 0.0163(15) 0.0208(15) 0.0001(12) 0.0066(12) 0.0003(12) Pt1 0.0145(2) 0.0185(2) 0.0155(2) 0.0008(2) 0.00471(14) -0.0001(2) Si1 0.0181(17) 0.0166(17) 0.0230(17) -0.0009(14) 0.0057(13) -0.0014(13) Si2 0.0219(18) 0.0243(19) 0.0245(17) 0.0041(14) 0.0082(14) 0.0009(15) _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 C1 C2 1.401(12) . ? C1 C6 1.404(12) . ? C1 P1 1.801(10) . ? C2 C3 1.396(13) . ? C2 H3 0.9500 . ? C3 C4 1.362(13) . ? C3 H28 0.9500 . ? C4 C5 1.371(14) . ? C4 H20 0.9500 . ? C5 C6 1.372(13) . ? C5 H24 0.9500 . ? C6 H7 0.9500 . ? C7 C8 1.376(12) . ? C7 C12 1.416(13) . ? C7 P1 1.827(10) . ? C8 C9 1.403(14) . ? C8 H8 0.9500 . ? C9 C10 1.377(14) . ? C9 H16 0.9500 . ? C10 C11S 1.400(13) . ? C10 H37 0.9500 . ? C12 C11S 1.394(13) . ? C12 H36 0.9500 . ? C13 C14 1.543(13) . ? C13 P1 1.841(9) . ? C13 H19A 0.9900 . ? C13 H19B 0.9900 . ? C14 P2 1.844(10) . ? C14 H11A 0.9900 . ? C14 H11B 0.9900 . ? C15 C20 1.362(14) . ? C15 C16 1.399(13) . ? C15 P2 1.815(10) . ? C16 C17 1.399(14) . ? C16 H21 0.9500 . ? C17 C18 1.362(15) . ? C17 H25 0.9500 . ? C18 C19 1.363(14) . ? C18 H31 0.9500 . ? C19 C20 1.411(15) . ? C19 H33 0.9500 . ? C20 H12 0.9500 . ? C21 C26 1.376(13) . ? C21 C22 1.398(13) . ? C21 P2 1.844(10) . ? C22 C23 1.366(14) . ? C22 H14 0.9500 . ? C23 C24 1.407(14) . ? C23 H26 0.9500 . ? C24 C25 1.394(14) . ? C24 H15 0.9500 . ? C25 C26 1.366(14) . ? C25 H22 0.9500 . ? C26 H32 0.9500 . ? C27 C28 1.380(14) . ? C27 C32 1.418(14) . ? C27 Si1 1.905(10) . ? C28 C29 1.377(13) . ? C28 H5 0.9500 . ? C29 C30 1.389(14) . ? C29 H30 0.9500 . ? C30 C31 1.374(15) . ? C30 H10 0.9500 . ? C31 C32 1.389(14) . ? C31 H34 0.9500 . ? C32 H23 0.9500 . ? C33 Si2 1.894(10) . ? C33 H27A 0.9800 . ? C33 H27B 0.9800 . ? C33 H27C 0.9800 . ? C34 Si2 1.874(10) . ? C34 H39A 0.9800 . ? C34 H39B 0.9800 . ? C34 H39C 0.9800 . ? C35 Si2 1.843(11) . ? C35 H40A 0.9800 . ? C35 H40B 0.9800 . ? C35 H40C 0.9800 . ? C11S H38S 0.9500 . ? P1 Pt1 2.286(3) . ? P2 Pt1 2.264(3) . ? Pt1 Si1 2.352(3) . ? Pt1 H1S 1.56(8) . ? Si1 Si2 2.337(4) . ? Si1 H2S 1.50(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 C2 C1 C6 116.5(9) . . ? C2 C1 P1 119.9(7) . . ? C6 C1 P1 123.5(7) . . ? C3 C2 C1 121.2(9) . . ? C3 C2 H3 119.4 . . ? C1 C2 H3 119.4 . . ? C4 C3 C2 120.1(10) . . ? C4 C3 H28 120.0 . . ? C2 C3 H28 120.0 . . ? C3 C4 C5 120.0(10) . . ? C3 C4 H20 120.0 . . ? C5 C4 H20 120.0 . . ? C6 C5 C4 120.6(10) . . ? C6 C5 H24 119.7 . . ? C4 C5 H24 119.7 . . ? C5 C6 C1 121.6(10) . . ? C5 C6 H7 119.2 . . ? C1 C6 H7 119.2 . . ? C8 C7 C12 117.7(9) . . ? C8 C7 P1 120.5(8) . . ? C12 C7 P1 121.5(7) . . ? C7 C8 C9 122.2(10) . . ? C7 C8 H8 118.9 . . ? C9 C8 H8 118.9 . . ? C10 C9 C8 120.1(10) . . ? C10 C9 H16 119.9 . . ? C8 C9 H16 119.9 . . ? C9 C10 C11S 118.8(10) . . ? C9 C10 H37 120.6 . . ? C11S C10 H37 120.6 . . ? C11S C12 C7 120.1(9) . . ? C11S C12 H36 119.9 . . ? C7 C12 H36 119.9 . . ? C14 C13 P1 110.1(6) . . ? C14 C13 H19A 109.6 . . ? P1 C13 H19A 109.6 . . ? C14 C13 H19B 109.6 . . ? P1 C13 H19B 109.6 . . ? H19A C13 H19B 108.2 . . ? C13 C14 P2 109.3(7) . . ? C13 C14 H11A 109.8 . . ? P2 C14 H11A 109.8 . . ? C13 C14 H11B 109.8 . . ? P2 C14 H11B 109.8 . . ? H11A C14 H11B 108.3 . . ? C20 C15 C16 117.9(10) . . ? C20 C15 P2 117.3(8) . . ? C16 C15 P2 124.8(8) . . ? C17 C16 C15 120.8(11) . . ? C17 C16 H21 119.6 . . ? C15 C16 H21 119.6 . . ? C18 C17 C16 119.2(10) . . ? C18 C17 H25 120.4 . . ? C16 C17 H25 120.4 . . ? C17 C18 C19 121.7(11) . . ? C17 C18 H31 119.2 . . ? C19 C18 H31 119.2 . . ? C18 C19 C20 118.6(11) . . ? C18 C19 H33 120.7 . . ? C20 C19 H33 120.7 . . ? C15 C20 C19 121.8(11) . . ? C15 C20 H12 119.1 . . ? C19 C20 H12 119.1 . . ? C26 C21 C22 119.5(10) . . ? C26 C21 P2 122.7(8) . . ? C22 C21 P2 117.7(8) . . ? C23 C22 C21 119.1(10) . . ? C23 C22 H14 120.4 . . ? C21 C22 H14 120.4 . . ? C22 C23 C24 121.7(10) . . ? C22 C23 H26 119.1 . . ? C24 C23 H26 119.1 . . ? C25 C24 C23 117.8(10) . . ? C25 C24 H15 121.1 . . ? C23 C24 H15 121.1 . . ? C26 C25 C24 120.4(10) . . ? C26 C25 H22 119.8 . . ? C24 C25 H22 119.8 . . ? C25 C26 C21 121.4(10) . . ? C25 C26 H32 119.3 . . ? C21 C26 H32 119.3 . . ? C28 C27 C32 117.2(9) . . ? C28 C27 Si1 122.3(7) . . ? C32 C27 Si1 120.4(8) . . ? C29 C28 C27 121.7(10) . . ? C29 C28 H5 119.2 . . ? C27 C28 H5 119.2 . . ? C28 C29 C30 120.7(10) . . ? C28 C29 H30 119.7 . . ? C30 C29 H30 119.7 . . ? C31 C30 C29 119.2(10) . . ? C31 C30 H10 120.4 . . ? C29 C30 H10 120.4 . . ? C30 C31 C32 120.4(10) . . ? C30 C31 H34 119.8 . . ? C32 C31 H34 119.8 . . ? C31 C32 C27 120.8(10) . . ? C31 C32 H23 119.6 . . ? C27 C32 H23 119.6 . . ? Si2 C33 H27A 109.5 . . ? Si2 C33 H27B 109.5 . . ? H27A C33 H27B 109.5 . . ? Si2 C33 H27C 109.5 . . ? H27A C33 H27C 109.5 . . ? H27B C33 H27C 109.5 . . ? Si2 C34 H39A 109.5 . . ? Si2 C34 H39B 109.5 . . ? H39A C34 H39B 109.5 . . ? Si2 C34 H39C 109.5 . . ? H39A C34 H39C 109.5 . . ? H39B C34 H39C 109.5 . . ? Si2 C35 H40A 109.5 . . ? Si2 C35 H40B 109.5 . . ? H40A C35 H40B 109.5 . . ? Si2 C35 H40C 109.5 . . ? H40A C35 H40C 109.5 . . ? H40B C35 H40C 109.5 . . ? C12 C11S C10 121.1(9) . . ? C12 C11S H38S 119.5 . . ? C10 C11S H38S 119.5 . . ? C1 P1 C7 103.7(4) . . ? C1 P1 C13 105.8(4) . . ? C7 P1 C13 106.6(5) . . ? C1 P1 Pt1 121.0(3) . . ? C7 P1 Pt1 111.5(3) . . ? C13 P1 Pt1 107.3(3) . . ? C15 P2 C14 104.5(5) . . ? C15 P2 C21 103.2(5) . . ? C14 P2 C21 104.0(5) . . ? C15 P2 Pt1 115.5(3) . . ? C14 P2 Pt1 107.8(3) . . ? C21 P2 Pt1 120.3(3) . . ? P2 Pt1 P1 86.60(10) . . ? P2 Pt1 Si1 97.49(10) . . ? P1 Pt1 Si1 174.87(10) . . ? P2 Pt1 H1S 177(3) . . ? P1 Pt1 H1S 90(3) . . ? Si1 Pt1 H1S 86(3) . . ? C27 Si1 Si2 105.9(3) . . ? C27 Si1 Pt1 112.1(3) . . ? Si2 Si1 Pt1 113.08(14) . . ? C27 Si1 H2S 105(3) . . ? Si2 Si1 H2S 104(3) . . ? Pt1 Si1 H2S 115(3) . . ? C35 Si2 C34 108.4(5) . . ? C35 Si2 C33 109.2(5) . . ? C34 Si2 C33 106.9(5) . . ? C35 Si2 Si1 111.2(4) . . ? C34 Si2 Si1 108.5(4) . . ? C33 Si2 Si1 112.4(4) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.47 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.572 _refine_diff_density_min -1.834 _refine_diff_density_rms 0.210 #===END data_complex3a _database_code_depnum_ccdc_archive 'CCDC 761293' #TrackingRef 'CIF.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C31 H40 P2 Pt Si2' _chemical_formula_weight 725.84 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' 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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.4840(4) _cell_length_b 11.5970(8) _cell_length_c 16.3770(11) _cell_angle_alpha 107.605(3) _cell_angle_beta 98.424(4) _cell_angle_gamma 107.803(4) _cell_volume 1576.97(17) _cell_formula_units_Z 2 _cell_measurement_temperature 133(2) _cell_measurement_reflns_used 15156 _cell_measurement_theta_min 2.37 _cell_measurement_theta_max 27.96 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.529 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 724 _exptl_absorpt_coefficient_mu 4.645 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 133(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method IP _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 15156 _diffrn_reflns_av_R_equivalents 0.042 _diffrn_reflns_av_sigmaI/netI 0.0376 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.37 _diffrn_reflns_theta_max 27.96 _reflns_number_total 6961 _reflns_number_gt 6513 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'DIP Image plate' _computing_cell_refinement 'HKL Scalepack' _computing_data_reduction 'maXus (Mackay et al., 1999)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep (Johnson, 1976)' _computing_publication_material ? _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. The bond distance of Si1-C29B is restrained to the standard value. ; _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^)+(0.0874P)^2^+1.5473P] 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 6961 _refine_ls_number_parameters 361 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0525 _refine_ls_R_factor_gt 0.0495 _refine_ls_wR_factor_ref 0.1235 _refine_ls_wR_factor_gt 0.1205 _refine_ls_goodness_of_fit_ref 1.082 _refine_ls_restrained_S_all 1.082 _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 Si2A Si 0.7917(4) 0.4492(3) 0.2968(2) 0.0312(7) Uani 0.656(10) 1 d P A 1 C29A C 0.8279(18) 0.5194(12) 0.4220(7) 0.063(3) Uani 0.656(10) 1 d P A 1 H29A H 0.9385 0.5552 0.4498 0.095 Uiso 0.656(10) 1 calc PR A 1 H29B H 0.7769 0.4504 0.4426 0.095 Uiso 0.656(10) 1 calc PR A 1 H29C H 0.7869 0.5887 0.4383 0.095 Uiso 0.656(10) 1 calc PR A 1 C30A C 0.9111(14) 0.5866(10) 0.2671(10) 0.067(4) Uani 0.656(10) 1 d P A 1 H30A H 0.8982 0.5564 0.2028 0.100 Uiso 0.656(10) 1 calc PR A 1 H30B H 1.0195 0.6144 0.2977 0.100 Uiso 0.656(10) 1 calc PR A 1 H30C H 0.8774 0.6602 0.2856 0.100 Uiso 0.656(10) 1 calc PR A 1 C31A C 0.5935(8) 0.4378(6) 0.2455(4) 0.051(2) Uani 0.656(10) 1 d P A 1 H31A H 0.5788 0.5181 0.2768 0.076 Uiso 0.656(10) 1 calc PR A 1 H31B H 0.5160 0.3634 0.2502 0.076 Uiso 0.656(10) 1 calc PR A 1 H31C H 0.5829 0.4261 0.1828 0.076 Uiso 0.656(10) 1 calc PR A 1 Si2B Si 0.8451(8) 0.4687(5) 0.2803(4) 0.0386(16) Uani 0.344(10) 1 d PR A 2 C29B C 0.5544(9) 0.2963(9) 0.3596(5) 0.042(4) Uani 0.344(10) 1 d PRD A 2 H29D H 0.6239 0.3425 0.4195 0.063 Uiso 0.344(10) 1 calc PR A 2 H29E H 0.4505 0.2532 0.3633 0.063 Uiso 0.344(10) 1 calc PR A 2 H29F H 0.5534 0.3587 0.3305 0.063 Uiso 0.344(10) 1 calc PR A 2 C30B C 0.660(3) 0.485(3) 0.2294(19) 0.071(7) Uani 0.344(10) 1 d P A 2 H30D H 0.6628 0.5728 0.2606 0.106 Uiso 0.344(10) 1 calc PR A 2 H30E H 0.5713 0.4204 0.2352 0.106 Uiso 0.344(10) 1 calc PR A 2 H30F H 0.6514 0.4706 0.1664 0.106 Uiso 0.344(10) 1 calc PR A 2 C31B C 0.911(3) 0.568(2) 0.4042(14) 0.059(6) Uani 0.344(10) 1 d P A 2 H31D H 0.9040 0.6539 0.4147 0.088 Uiso 0.344(10) 1 calc PR A 2 H31E H 1.0177 0.5795 0.4273 0.088 Uiso 0.344(10) 1 calc PR A 2 H31F H 0.8455 0.5229 0.4346 0.088 Uiso 0.344(10) 1 calc PR A 2 Pt1 Pt 0.849841(19) 0.256126(15) 0.249580(11) 0.03109(8) Uani 1 1 d . . . P1 P 0.89779(16) 0.06494(12) 0.21232(9) 0.0325(3) Uani 1 1 d . A . P2 P 1.06863(16) 0.33510(13) 0.20417(10) 0.0347(3) Uani 1 1 d . A . Si1 Si 0.62274(18) 0.16994(15) 0.29265(10) 0.0358(3) Uani 1 1 d D A . C1 C 1.0381(6) 0.0785(5) 0.1454(4) 0.0390(11) Uani 1 1 d . . . H1A H 1.0800 0.0121 0.1417 0.047 Uiso 1 1 d R A . H1B H 0.9875 0.0677 0.0868 0.047 Uiso 1 1 d R . . C2 C 1.1645(6) 0.2152(5) 0.1903(4) 0.0424(12) Uani 1 1 d . A . H2A H 1.2365 0.2309 0.1557 0.051 Uiso 1 1 d R . . H2B H 1.2178 0.2248 0.2480 0.051 Uiso 1 1 d R . . C3 C 1.0004(7) 0.0395(6) 0.3039(4) 0.0416(12) Uani 1 1 d . . . C4 C 1.0520(9) -0.0640(7) 0.2902(5) 0.0571(17) Uani 1 1 d . A . H4 H 1.0253 -0.1276 0.2314 0.068 Uiso 1 1 d R . . C5 C 1.1401(11) -0.0749(8) 0.3607(6) 0.072(2) Uani 1 1 d . . . H5 H 1.1781 -0.1444 0.3514 0.086 Uiso 1 1 d R A . C6 C 1.1747(10) 0.0137(9) 0.4446(6) 0.073(2) Uani 1 1 d . A . H6 H 1.2309 0.0025 0.4934 0.088 Uiso 1 1 d R . . C7 C 1.1278(11) 0.1183(9) 0.4602(5) 0.070(2) Uani 1 1 d . . . H7 H 1.1595 0.1836 0.5188 0.084 Uiso 1 1 d R A . C8 C 1.0393(8) 0.1299(6) 0.3901(4) 0.0509(14) Uani 1 1 d . A . H8 H 1.0041 0.2012 0.4012 0.061 Uiso 1 1 d R . . C9 C 0.7461(6) -0.0906(5) 0.1431(4) 0.0375(11) Uani 1 1 d . . . C10 C 0.6788(7) -0.1053(5) 0.0566(4) 0.0413(11) Uani 1 1 d . A . H10 H 0.7155 -0.0358 0.0355 0.050 Uiso 1 1 d R . . C11 C 0.5587(7) -0.2201(6) 0.0003(4) 0.0498(14) Uani 1 1 d . . . H11 H 0.5141 -0.2291 -0.0589 0.060 Uiso 1 1 d R A . C12 C 0.5050(7) -0.3202(6) 0.0313(5) 0.0550(17) Uani 1 1 d . A . H12 H 0.4247 -0.4001 -0.0086 0.066 Uiso 1 1 d R . . C13 C 0.5654(7) -0.3068(5) 0.1163(5) 0.0512(15) Uani 1 1 d . . . H13 H 0.5238 -0.3762 0.1367 0.061 Uiso 1 1 d R A . C14 C 0.6880(7) -0.1906(5) 0.1739(4) 0.0431(12) Uani 1 1 d . A . H14 H 0.7313 -0.1803 0.2336 0.052 Uiso 1 1 d R . . C15 C 1.2243(7) 0.4889(5) 0.2739(4) 0.0429(12) Uani 1 1 d . . . C16 C 1.2791(7) 0.5920(5) 0.2462(5) 0.0462(13) Uani 1 1 d . A . H16 H 1.2388 0.5818 0.1861 0.055 Uiso 1 1 d R . . C17 C 1.3929(8) 0.7104(6) 0.3050(6) 0.0604(18) Uani 1 1 d . . . H17 H 1.4296 0.7816 0.2854 0.073 Uiso 1 1 d R A . C18 C 1.4490(10) 0.7242(8) 0.3906(6) 0.079(3) Uani 1 1 d . A . H18 H 1.5269 0.8045 0.4318 0.095 Uiso 1 1 d R . . C19 C 1.3987(13) 0.6220(10) 0.4186(7) 0.101(4) Uani 1 1 d . . . H19 H 1.4396 0.6339 0.4790 0.121 Uiso 1 1 d R A . C20 C 1.2852(10) 0.5033(8) 0.3608(5) 0.073(2) Uani 1 1 d . A . H20 H 1.2511 0.4313 0.3800 0.087 Uiso 1 1 d R . . C21 C 1.0310(6) 0.3370(5) 0.0921(4) 0.0363(10) Uani 1 1 d . . . C22 C 1.1464(7) 0.3631(6) 0.0489(4) 0.0419(12) Uani 1 1 d . A . H22 H 1.2511 0.3852 0.0792 0.050 Uiso 1 1 d R . . C23 C 1.1121(8) 0.3579(6) -0.0373(4) 0.0504(14) Uani 1 1 d . . . H23 H 1.1930 0.3797 -0.0655 0.060 Uiso 1 1 d R A . C24 C 0.9608(8) 0.3217(7) -0.0834(4) 0.0493(14) Uani 1 1 d . A . H24 H 0.9374 0.3158 -0.1439 0.059 Uiso 1 1 d R . . C25 C 0.8431(8) 0.2927(6) -0.0422(4) 0.0479(13) Uani 1 1 d . . . H25 H 0.7383 0.2681 -0.0735 0.057 Uiso 1 1 d R A . C26 C 0.8786(7) 0.3004(5) 0.0455(4) 0.0414(11) Uani 1 1 d . A . H26 H 0.7978 0.2800 0.0740 0.050 Uiso 1 1 d R . . C27 C 0.6449(8) 0.0809(7) 0.3711(5) 0.0522(14) Uani 1 1 d . . . H27A H 0.5490 0.0493 0.3851 0.063 Uiso 1 1 d R A . H27B H 0.7230 0.1396 0.4247 0.063 Uiso 1 1 d R . . H27C H 0.6731 0.0087 0.3433 0.063 Uiso 1 1 d R . . C28 C 0.4565(8) 0.0514(7) 0.1957(5) 0.0512(15) Uani 1 1 d . . . H28A H 0.3681 0.0194 0.2162 0.061 Uiso 1 1 d R A . H28B H 0.4828 -0.0203 0.1644 0.061 Uiso 1 1 d R . . H28C H 0.4340 0.0944 0.1567 0.061 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Si2A 0.0319(15) 0.0239(11) 0.0398(14) 0.0115(9) 0.0120(10) 0.0120(10) C29A 0.080(9) 0.044(6) 0.047(5) 0.001(5) -0.009(6) 0.024(6) C30A 0.074(7) 0.038(5) 0.123(10) 0.050(6) 0.061(8) 0.032(5) C31A 0.035(5) 0.046(5) 0.071(7) 0.020(5) 0.002(5) 0.021(4) Si2B 0.050(4) 0.028(2) 0.045(3) 0.0149(19) 0.014(3) 0.023(3) C29B 0.026(7) 0.059(10) 0.050(9) 0.019(7) 0.019(7) 0.023(6) C30B 0.076(18) 0.094(19) 0.082(16) 0.043(15) 0.039(15) 0.064(16) C31B 0.081(16) 0.035(9) 0.046(10) 0.001(8) 0.000(10) 0.022(10) Pt1 0.03067(14) 0.02383(11) 0.03933(12) 0.01243(8) 0.00617(9) 0.01149(8) P1 0.0310(7) 0.0243(5) 0.0442(6) 0.0138(5) 0.0076(5) 0.0130(5) P2 0.0266(7) 0.0272(6) 0.0483(7) 0.0151(5) 0.0070(5) 0.0073(5) Si1 0.0330(8) 0.0356(7) 0.0421(7) 0.0159(6) 0.0115(6) 0.0149(6) C1 0.034(3) 0.033(2) 0.055(3) 0.019(2) 0.012(2) 0.016(2) C2 0.033(3) 0.038(3) 0.062(3) 0.023(2) 0.012(2) 0.018(2) C3 0.041(3) 0.037(3) 0.051(3) 0.020(2) 0.006(2) 0.020(2) C4 0.067(5) 0.050(4) 0.066(4) 0.025(3) 0.011(3) 0.036(3) C5 0.078(6) 0.063(4) 0.087(5) 0.036(4) 0.004(4) 0.042(4) C6 0.062(5) 0.085(6) 0.082(5) 0.049(5) -0.004(4) 0.034(4) C7 0.071(6) 0.066(5) 0.059(4) 0.023(4) -0.015(4) 0.025(4) C8 0.051(4) 0.046(3) 0.052(3) 0.017(3) -0.001(3) 0.021(3) C9 0.032(3) 0.025(2) 0.055(3) 0.013(2) 0.012(2) 0.0122(18) C10 0.038(3) 0.032(2) 0.049(3) 0.012(2) 0.009(2) 0.012(2) C11 0.040(3) 0.041(3) 0.053(3) 0.005(2) 0.008(3) 0.009(2) C12 0.039(3) 0.033(3) 0.077(4) 0.003(3) 0.017(3) 0.008(2) C13 0.046(3) 0.029(3) 0.080(4) 0.018(3) 0.029(3) 0.014(2) C14 0.043(3) 0.029(2) 0.064(3) 0.020(2) 0.020(3) 0.017(2) C15 0.033(3) 0.034(3) 0.054(3) 0.014(2) 0.004(2) 0.007(2) C16 0.040(3) 0.031(3) 0.062(3) 0.011(2) 0.018(3) 0.009(2) C17 0.047(4) 0.033(3) 0.086(5) 0.008(3) 0.021(4) 0.005(2) C18 0.060(5) 0.051(4) 0.085(6) 0.001(4) 0.007(4) -0.005(3) C19 0.087(7) 0.080(6) 0.074(6) 0.015(5) -0.027(5) -0.016(5) C20 0.065(5) 0.059(4) 0.060(4) 0.020(3) -0.011(4) -0.008(4) C21 0.034(3) 0.026(2) 0.046(3) 0.0110(19) 0.007(2) 0.0108(18) C22 0.031(3) 0.037(3) 0.056(3) 0.014(2) 0.013(2) 0.015(2) C23 0.054(4) 0.046(3) 0.058(3) 0.019(3) 0.025(3) 0.023(3) C24 0.058(4) 0.056(3) 0.043(3) 0.017(3) 0.017(3) 0.032(3) C25 0.048(4) 0.050(3) 0.049(3) 0.017(3) 0.013(3) 0.023(3) C26 0.037(3) 0.035(3) 0.051(3) 0.015(2) 0.011(2) 0.014(2) C27 0.056(4) 0.047(3) 0.059(4) 0.028(3) 0.014(3) 0.020(3) C28 0.038(3) 0.047(3) 0.060(4) 0.012(3) 0.006(3) 0.014(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Si2A C31A 1.891(6) . ? Si2A C30A 1.894(10) . ? Si2A C29A 1.896(12) . ? Si2A Pt1 2.398(3) . ? C29A H29A 0.9800 . ? C29A H29B 0.9800 . ? C29A H29C 0.9800 . ? C30A H30A 0.9800 . ? C30A H30B 0.9800 . ? C30A H30C 0.9800 . ? C31A H31A 0.9800 . ? C31A H31B 0.9800 . ? C31A H31C 0.9800 . ? Si2B C31B 1.90(2) . ? Si2B C30B 1.92(3) . ? Si2B Pt1 2.378(5) . ? C29B Si1 1.894(8) . ? C29B H29D 0.9800 . ? C29B H29E 0.9800 . ? C29B H29F 0.9800 . ? C30B H30D 0.9800 . ? C30B H30E 0.9800 . ? C30B H30F 0.9800 . ? C31B H31D 0.9800 . ? C31B H31E 0.9800 . ? C31B H31F 0.9800 . ? Pt1 P1 2.3183(12) . ? Pt1 P2 2.3237(13) . ? Pt1 Si1 2.3855(15) . ? P1 C3 1.816(6) . ? P1 C9 1.819(5) . ? P1 C1 1.844(6) . ? P2 C15 1.824(6) . ? P2 C21 1.826(6) . ? P2 C2 1.859(6) . ? Si1 C28 1.875(7) . ? Si1 C27 1.903(6) . ? C1 C2 1.538(8) . ? C1 H1A 0.9601 . ? C1 H1B 0.9599 . ? C2 H2A 0.9600 . ? C2 H2B 0.9600 . ? C3 C8 1.395(9) . ? C3 C4 1.399(8) . ? C4 C5 1.385(10) . ? C4 H4 0.9601 . ? C5 C6 1.364(13) . ? C5 H5 0.9601 . ? C6 C7 1.382(12) . ? C6 H6 0.9601 . ? C7 C8 1.386(9) . ? C7 H7 0.9601 . ? C8 H8 0.9601 . ? C9 C14 1.395(7) . ? C9 C10 1.403(8) . ? C10 C11 1.394(8) . ? C10 H10 0.9602 . ? C11 C12 1.391(10) . ? C11 H11 0.9598 . ? C12 C13 1.369(11) . ? C12 H12 0.9600 . ? C13 C14 1.417(8) . ? C13 H13 0.9599 . ? C14 H14 0.9599 . ? C15 C16 1.386(8) . ? C15 C20 1.394(10) . ? C16 C17 1.403(8) . ? C16 H16 0.9600 . ? C17 C18 1.368(13) . ? C17 H17 0.9600 . ? C18 C19 1.374(14) . ? C18 H18 0.9600 . ? C19 C20 1.399(10) . ? C19 H19 0.9601 . ? C20 H20 0.9600 . ? C21 C22 1.395(8) . ? C21 C26 1.400(8) . ? C22 C23 1.379(9) . ? C22 H22 0.9600 . ? C23 C24 1.388(10) . ? C23 H23 0.9601 . ? C24 C25 1.395(9) . ? C24 H24 0.9600 . ? C25 C26 1.395(9) . ? C25 H25 0.9600 . ? C26 H26 0.9600 . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C28 H28A 0.9601 . ? C28 H28B 0.9601 . ? C28 H28C 0.9599 . ? 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 C31A Si2A C30A 99.3(5) . . ? C31A Si2A C29A 107.9(5) . . ? C30A Si2A C29A 105.3(6) . . ? C31A Si2A Pt1 117.6(2) . . ? C30A Si2A Pt1 114.0(3) . . ? C29A Si2A Pt1 111.5(4) . . ? C31B Si2B C30B 109.4(12) . . ? C31B Si2B Pt1 111.6(7) . . ? C30B Si2B Pt1 118.4(10) . . ? Si1 C29B H29D 109.5 . . ? Si1 C29B H29E 109.5 . . ? H29D C29B H29E 109.5 . . ? Si1 C29B H29F 109.5 . . ? H29D C29B H29F 109.5 . . ? H29E C29B H29F 109.5 . . ? Si2B C30B H30D 109.5 . . ? Si2B C30B H30E 109.5 . . ? H30D C30B H30E 109.5 . . ? Si2B C30B H30F 109.5 . . ? H30D C30B H30F 109.5 . . ? H30E C30B H30F 109.5 . . ? Si2B C31B H31D 109.5 . . ? Si2B C31B H31E 109.5 . . ? H31D C31B H31E 109.5 . . ? Si2B C31B H31F 109.5 . . ? H31D C31B H31F 109.5 . . ? H31E C31B H31F 109.5 . . ? P1 Pt1 P2 84.13(5) . . ? P1 Pt1 Si2B 169.0(2) . . ? P2 Pt1 Si2B 84.9(2) . . ? P1 Pt1 Si1 94.83(5) . . ? P2 Pt1 Si1 178.46(4) . . ? Si2B Pt1 Si1 96.2(2) . . ? P1 Pt1 Si2A 175.51(9) . . ? P2 Pt1 Si2A 99.73(10) . . ? Si2B Pt1 Si2A 14.97(14) . . ? Si1 Pt1 Si2A 81.36(10) . . ? C3 P1 C9 107.0(3) . . ? C3 P1 C1 100.8(3) . . ? C9 P1 C1 102.2(3) . . ? C3 P1 Pt1 115.62(19) . . ? C9 P1 Pt1 120.93(17) . . ? C1 P1 Pt1 107.56(17) . . ? C15 P2 C21 106.7(3) . . ? C15 P2 C2 103.1(3) . . ? C21 P2 C2 100.8(3) . . ? C15 P2 Pt1 121.3(2) . . ? C21 P2 Pt1 114.56(18) . . ? C2 P2 Pt1 107.91(19) . . ? C28 Si1 C29B 107.0(3) . . ? C28 Si1 C27 105.9(3) . . ? C29B Si1 C27 100.9(3) . . ? C28 Si1 Pt1 112.9(2) . . ? C29B Si1 Pt1 114.9(3) . . ? C27 Si1 Pt1 114.2(2) . . ? C2 C1 P1 108.0(4) . . ? C2 C1 H1A 111.1 . . ? P1 C1 H1A 109.5 . . ? C2 C1 H1B 109.6 . . ? P1 C1 H1B 109.2 . . ? H1A C1 H1B 109.5 . . ? C1 C2 P2 107.3(4) . . ? C1 C2 H2A 111.8 . . ? P2 C2 H2A 109.9 . . ? C1 C2 H2B 109.6 . . ? P2 C2 H2B 108.7 . . ? H2A C2 H2B 109.5 . . ? C8 C3 C4 118.1(6) . . ? C8 C3 P1 119.7(4) . . ? C4 C3 P1 122.0(5) . . ? C5 C4 C3 120.5(7) . . ? C5 C4 H4 120.2 . . ? C3 C4 H4 119.2 . . ? C6 C5 C4 120.1(7) . . ? C6 C5 H5 119.1 . . ? C4 C5 H5 120.8 . . ? C5 C6 C7 120.8(7) . . ? C5 C6 H6 119.5 . . ? C7 C6 H6 119.7 . . ? C6 C7 C8 119.4(8) . . ? C6 C7 H7 119.9 . . ? C8 C7 H7 120.6 . . ? C7 C8 C3 120.9(6) . . ? C7 C8 H8 119.4 . . ? C3 C8 H8 119.7 . . ? C14 C9 C10 119.3(5) . . ? C14 C9 P1 123.3(5) . . ? C10 C9 P1 117.2(4) . . ? C11 C10 C9 120.8(6) . . ? C11 C10 H10 119.3 . . ? C9 C10 H10 120.0 . . ? C12 C11 C10 119.1(6) . . ? C12 C11 H11 120.9 . . ? C10 C11 H11 120.0 . . ? C13 C12 C11 121.3(6) . . ? C13 C12 H12 120.1 . . ? C11 C12 H12 118.6 . . ? C12 C13 C14 120.0(6) . . ? C12 C13 H13 119.6 . . ? C14 C13 H13 120.4 . . ? C9 C14 C13 119.5(6) . . ? C9 C14 H14 119.9 . . ? C13 C14 H14 120.6 . . ? C16 C15 C20 119.3(6) . . ? C16 C15 P2 123.7(5) . . ? C20 C15 P2 117.0(5) . . ? C15 C16 C17 120.7(7) . . ? C15 C16 H16 119.5 . . ? C17 C16 H16 119.8 . . ? C18 C17 C16 119.4(7) . . ? C18 C17 H17 120.4 . . ? C16 C17 H17 120.2 . . ? C17 C18 C19 120.7(7) . . ? C17 C18 H18 120.5 . . ? C19 C18 H18 118.8 . . ? C18 C19 C20 120.6(9) . . ? C18 C19 H19 119.2 . . ? C20 C19 H19 120.1 . . ? C15 C20 C19 119.3(8) . . ? C15 C20 H20 120.0 . . ? C19 C20 H20 120.7 . . ? C22 C21 C26 118.9(5) . . ? C22 C21 P2 122.6(5) . . ? C26 C21 P2 118.3(4) . . ? C23 C22 C21 120.7(6) . . ? C23 C22 H22 119.4 . . ? C21 C22 H22 119.9 . . ? C22 C23 C24 120.3(6) . . ? C22 C23 H23 120.0 . . ? C24 C23 H23 119.7 . . ? C23 C24 C25 120.0(6) . . ? C23 C24 H24 119.9 . . ? C25 C24 H24 120.1 . . ? C24 C25 C26 119.5(6) . . ? C24 C25 H25 120.5 . . ? C26 C25 H25 119.9 . . ? C25 C26 C21 120.5(6) . . ? C25 C26 H26 119.8 . . ? C21 C26 H26 119.7 . . ? Si1 C27 H27A 109.0 . . ? Si1 C27 H27B 109.6 . . ? H27A C27 H27B 109.5 . . ? Si1 C27 H27C 109.8 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? Si1 C28 H28A 109.8 . . ? Si1 C28 H28B 109.3 . . ? H28A C28 H28B 109.5 . . ? Si1 C28 H28C 109.2 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.916 _diffrn_reflns_theta_full 27.96 _diffrn_measured_fraction_theta_full 0.916 _refine_diff_density_max 1.101 _refine_diff_density_min -4.354 _refine_diff_density_rms 0.194 #===END data_complex3b _database_code_depnum_ccdc_archive 'CCDC 761294' #TrackingRef 'CIF.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C41 H44 P2 Pt Si2' _chemical_formula_weight 849.97 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' 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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C 2/c ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 40.4880(14) _cell_length_b 10.2430(6) _cell_length_c 20.5200(11) _cell_angle_alpha 90.00 _cell_angle_beta 115.089(3) _cell_angle_gamma 90.00 _cell_volume 7707.1(7) _cell_formula_units_Z 8 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 34652 _cell_measurement_theta_min 2.06 _cell_measurement_theta_max 27.94 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.465 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3408 _exptl_absorpt_coefficient_mu 3.814 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method IP _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 34652 _diffrn_reflns_av_R_equivalents 0.061 _diffrn_reflns_av_sigmaI/netI 0.0411 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 53 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.06 _diffrn_reflns_theta_max 27.94 _reflns_number_total 8848 _reflns_number_gt 7518 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'DIP Image plate' _computing_cell_refinement 'HKL Scalepack' _computing_data_reduction 'maXus (Mackay et al., 1999)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep (Johnson, 1976)' _computing_publication_material ? _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^)+(0.0642P)^2^+16.3700P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8848 _refine_ls_number_parameters 418 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0507 _refine_ls_R_factor_gt 0.0405 _refine_ls_wR_factor_ref 0.1028 _refine_ls_wR_factor_gt 0.0967 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.035 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.119058(4) 0.178881(15) -0.047370(8) 0.01757(6) Uani 1 1 d . . . P1 P 0.14190(3) 0.23023(12) -0.13147(6) 0.0197(2) Uani 1 1 d . . . P2 P 0.11208(3) 0.40265(11) -0.04239(6) 0.0201(2) Uani 1 1 d . . . Si1 Si 0.13600(3) -0.04341(12) -0.03235(6) 0.0204(2) Uani 1 1 d D . . H1 H 0.1204(13) -0.120(4) 0.005(2) 0.025 Uiso 1 1 d D . . Si2 Si 0.08683(3) 0.12072(13) 0.02308(7) 0.0221(2) Uani 1 1 d . . . C1 C 0.15637(13) 0.4023(5) -0.1160(3) 0.0263(9) Uani 1 1 d . . . H1A H 0.1789 0.4088 -0.0736 0.032 Uiso 1 1 d R . . H1B H 0.1597 0.4346 -0.1567 0.032 Uiso 1 1 d R . . C2 C 0.12711(13) 0.4833(5) -0.1058(3) 0.0261(9) Uani 1 1 d . . . H2A H 0.1067 0.4936 -0.1517 0.031 Uiso 1 1 d R . . H2B H 0.1371 0.5674 -0.0872 0.031 Uiso 1 1 d R . . C3 C 0.18030(12) 0.1539(5) -0.1407(3) 0.0240(9) Uani 1 1 d . . . C4 C 0.17844(14) 0.1094(5) -0.2067(3) 0.0314(11) Uani 1 1 d . . . H4 H 0.1562 0.1192 -0.2495 0.038 Uiso 1 1 d R . . C5 C 0.20884(16) 0.0511(6) -0.2100(3) 0.0422(13) Uani 1 1 d . . . H5 H 0.2076 0.0220 -0.2555 0.051 Uiso 1 1 d R . . C6 C 0.24077(16) 0.0350(6) -0.1482(4) 0.0488(15) Uani 1 1 d . . . H6 H 0.2615 -0.0057 -0.1507 0.059 Uiso 1 1 d R . . C7 C 0.24279(14) 0.0796(6) -0.0822(4) 0.0430(14) Uani 1 1 d . . . H7 H 0.2649 0.0680 -0.0393 0.052 Uiso 1 1 d R . . C8 C 0.21288(14) 0.1399(6) -0.0786(3) 0.0335(11) Uani 1 1 d . . . H8 H 0.2145 0.1715 -0.0332 0.040 Uiso 1 1 d R . . C9 C 0.10502(12) 0.2277(5) -0.2220(2) 0.0249(9) Uani 1 1 d . . . C10 C 0.10280(16) 0.3145(6) -0.2757(3) 0.0376(13) Uani 1 1 d . . . H10 H 0.1209 0.3814 -0.2652 0.045 Uiso 1 1 d R . . C11 C 0.07438(17) 0.3046(7) -0.3445(3) 0.0470(16) Uani 1 1 d . . . H11 H 0.0727 0.3651 -0.3815 0.056 Uiso 1 1 d R . . C12 C 0.04820(17) 0.2085(7) -0.3598(3) 0.0496(16) Uani 1 1 d . . . H12 H 0.0288 0.2022 -0.4073 0.060 Uiso 1 1 d R . . C13 C 0.05004(17) 0.1220(7) -0.3072(3) 0.0483(15) Uani 1 1 d . . . H13 H 0.0322 0.0538 -0.3179 0.058 Uiso 1 1 d R . . C14 C 0.07821(14) 0.1317(5) -0.2379(3) 0.0339(11) Uani 1 1 d . . . H14 H 0.0789 0.0729 -0.2009 0.041 Uiso 1 1 d R . . C15 C 0.06676(12) 0.4723(5) -0.0709(2) 0.0245(9) Uani 1 1 d . . . C16 C 0.05818(14) 0.5752(5) -0.0364(3) 0.0332(11) Uani 1 1 d . . . H16 H 0.0772 0.6150 0.0048 0.040 Uiso 1 1 d R . . C17 C 0.02242(15) 0.6201(6) -0.0616(3) 0.0369(12) Uani 1 1 d . . . H17 H 0.0165 0.6908 -0.0377 0.044 Uiso 1 1 d R . . C18 C -0.00480(14) 0.5630(6) -0.1210(3) 0.0386(13) Uani 1 1 d . . . H18 H -0.0295 0.5928 -0.1375 0.046 Uiso 1 1 d R . . C19 C 0.00323(14) 0.4624(6) -0.1567(3) 0.0377(12) Uani 1 1 d . . . H19 H -0.0156 0.4254 -0.1993 0.045 Uiso 1 1 d R . . C20 C 0.03902(13) 0.4158(5) -0.1309(3) 0.0298(10) Uani 1 1 d . . . H20 H 0.0446 0.3437 -0.1544 0.036 Uiso 1 1 d R . . C21 C 0.14028(12) 0.4729(4) 0.0455(2) 0.0227(9) Uani 1 1 d . . . C22 C 0.15504(12) 0.3922(5) 0.1060(3) 0.0259(9) Uani 1 1 d . . . H22 H 0.1513 0.2995 0.1009 0.031 Uiso 1 1 d R . . C23 C 0.17532(13) 0.4446(5) 0.1736(3) 0.0301(10) Uani 1 1 d . . . H23 H 0.1858 0.3883 0.2148 0.036 Uiso 1 1 d R . . C24 C 0.18071(13) 0.5788(5) 0.1825(3) 0.0275(10) Uani 1 1 d . . . H24 H 0.1942 0.6146 0.2297 0.033 Uiso 1 1 d R . . C25 C 0.16630(14) 0.6598(5) 0.1226(3) 0.0296(10) Uani 1 1 d . . . H25 H 0.1695 0.7527 0.1278 0.036 Uiso 1 1 d R . . C26 C 0.14726(13) 0.6086(5) 0.0553(2) 0.0260(9) Uani 1 1 d . . . H26 H 0.1385 0.6658 0.0144 0.031 Uiso 1 1 d R . . C27 C 0.12522(13) -0.1427(4) -0.1171(2) 0.0244(9) Uani 1 1 d . . . C28 C 0.09007(15) -0.1937(5) -0.1534(3) 0.0324(11) Uani 1 1 d . . . H28 H 0.0727 -0.1816 -0.1334 0.039 Uiso 1 1 d R . . C29 C 0.07951(17) -0.2613(6) -0.2179(3) 0.0416(13) Uani 1 1 d . . . H29 H 0.0552 -0.2956 -0.2420 0.050 Uiso 1 1 d R . . C30 C 0.10444(19) -0.2799(6) -0.2478(3) 0.0438(15) Uani 1 1 d . . . H30 H 0.0972 -0.3263 -0.2924 0.053 Uiso 1 1 d R . . C31 C 0.13939(18) -0.2308(6) -0.2124(3) 0.0406(13) Uani 1 1 d . . . H31 H 0.1567 -0.2436 -0.2325 0.049 Uiso 1 1 d R . . C32 C 0.15009(16) -0.1622(5) -0.1480(3) 0.0301(10) Uani 1 1 d . . . H32 H 0.1744 -0.1283 -0.1246 0.036 Uiso 1 1 d R . . C33 C 0.18669(12) -0.0570(5) 0.0290(2) 0.0257(9) Uani 1 1 d . . . C34 C 0.20786(14) -0.1663(5) 0.0307(3) 0.0298(10) Uani 1 1 d . . . H34 H 0.1968 -0.2385 -0.0009 0.036 Uiso 1 1 d R . . C35 C 0.24504(15) -0.1738(6) 0.0771(3) 0.0361(12) Uani 1 1 d . . . H35 H 0.2589 -0.2502 0.0776 0.043 Uiso 1 1 d R . . C36 C 0.26156(14) -0.0703(6) 0.1225(3) 0.0388(13) Uani 1 1 d . . . H36 H 0.2870 -0.0740 0.1549 0.047 Uiso 1 1 d R . . C37 C 0.24152(15) 0.0395(6) 0.1225(3) 0.0427(13) Uani 1 1 d . . . H37 H 0.2534 0.1116 0.1535 0.051 Uiso 1 1 d R . . C38 C 0.20431(14) 0.0452(5) 0.0763(3) 0.0329(11) Uani 1 1 d . . . H38 H 0.1908 0.1215 0.0775 0.039 Uiso 1 1 d R . . C39 C 0.06242(14) 0.2575(5) 0.0469(3) 0.0300(10) Uani 1 1 d . . . H39A H 0.0505 0.2232 0.0750 0.036 Uiso 1 1 d R . . H39B H 0.0446 0.2957 0.0036 0.036 Uiso 1 1 d R . . H39C H 0.0797 0.3229 0.0742 0.036 Uiso 1 1 d R . . C40 C 0.04757(12) 0.0056(5) -0.0289(3) 0.0321(11) Uani 1 1 d . . . H40A H 0.0350 -0.0165 0.0001 0.038 Uiso 1 1 d R . . H40B H 0.0569 -0.0723 -0.0409 0.038 Uiso 1 1 d R . . H40C H 0.0310 0.0477 -0.0722 0.038 Uiso 1 1 d R . . C41 C 0.11576(14) 0.0441(5) 0.1134(2) 0.0292(10) Uani 1 1 d . . . H41A H 0.1008 0.0240 0.1379 0.035 Uiso 1 1 d R . . H41B H 0.1346 0.1039 0.1419 0.035 Uiso 1 1 d R . . H41C H 0.1266 -0.0347 0.1061 0.035 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.01858(9) 0.01662(9) 0.01840(9) 0.00060(6) 0.00870(6) 0.00252(6) P1 0.0197(5) 0.0216(5) 0.0195(5) 0.0003(4) 0.0100(4) 0.0009(4) P2 0.0238(5) 0.0169(5) 0.0208(5) 0.0016(4) 0.0107(4) 0.0042(4) Si1 0.0218(5) 0.0182(5) 0.0211(6) 0.0005(4) 0.0089(4) 0.0034(5) Si2 0.0225(6) 0.0239(6) 0.0226(6) 0.0029(5) 0.0123(5) 0.0025(5) C1 0.028(2) 0.021(2) 0.033(3) 0.0025(18) 0.0162(19) 0.0015(19) C2 0.032(2) 0.021(2) 0.029(2) 0.0003(17) 0.0154(19) 0.0046(18) C3 0.021(2) 0.025(2) 0.028(2) 0.0025(17) 0.0127(17) 0.0039(18) C4 0.032(2) 0.036(3) 0.030(3) 0.000(2) 0.017(2) 0.007(2) C5 0.041(3) 0.047(3) 0.052(3) 0.000(3) 0.032(3) 0.011(3) C6 0.039(3) 0.043(3) 0.079(5) 0.004(3) 0.039(3) 0.010(3) C7 0.024(2) 0.042(3) 0.060(4) 0.001(3) 0.015(2) 0.007(2) C8 0.027(2) 0.039(3) 0.032(3) -0.001(2) 0.011(2) 0.002(2) C9 0.024(2) 0.029(2) 0.021(2) -0.0018(18) 0.0101(17) 0.0051(19) C10 0.034(3) 0.050(4) 0.033(3) 0.011(2) 0.019(2) 0.004(2) C11 0.045(3) 0.069(4) 0.026(3) 0.017(3) 0.014(2) 0.016(3) C12 0.039(3) 0.068(4) 0.027(3) -0.003(3) 0.001(2) 0.013(3) C13 0.043(3) 0.045(4) 0.038(3) -0.009(3) 0.000(2) 0.001(3) C14 0.029(2) 0.033(3) 0.032(3) -0.001(2) 0.005(2) 0.002(2) C15 0.030(2) 0.023(2) 0.022(2) 0.0037(17) 0.0134(17) 0.0045(19) C16 0.030(2) 0.037(3) 0.034(3) -0.003(2) 0.014(2) 0.006(2) C17 0.034(3) 0.034(3) 0.044(3) -0.005(2) 0.018(2) 0.015(2) C18 0.030(2) 0.049(3) 0.035(3) 0.008(2) 0.012(2) 0.014(2) C19 0.029(2) 0.052(3) 0.027(3) -0.003(2) 0.006(2) 0.007(2) C20 0.026(2) 0.033(3) 0.026(2) -0.0013(19) 0.0062(18) 0.008(2) C21 0.026(2) 0.020(2) 0.024(2) -0.0011(17) 0.0120(17) 0.0040(18) C22 0.028(2) 0.022(2) 0.029(2) -0.0019(18) 0.0134(18) -0.0019(19) C23 0.033(2) 0.035(3) 0.022(2) 0.0025(19) 0.0113(19) -0.001(2) C24 0.025(2) 0.032(3) 0.025(2) -0.0053(18) 0.0103(18) -0.0031(19) C25 0.031(2) 0.023(2) 0.032(3) -0.0047(19) 0.010(2) -0.0002(19) C26 0.030(2) 0.025(2) 0.022(2) 0.0020(17) 0.0099(18) 0.0039(19) C27 0.028(2) 0.016(2) 0.022(2) 0.0004(16) 0.0040(17) 0.0081(17) C28 0.033(3) 0.024(2) 0.031(3) 0.0005(19) 0.004(2) 0.005(2) C29 0.052(3) 0.032(3) 0.027(3) -0.005(2) 0.003(2) 0.000(3) C30 0.069(4) 0.028(3) 0.024(3) 0.001(2) 0.009(3) 0.009(3) C31 0.066(4) 0.031(3) 0.032(3) 0.003(2) 0.028(3) 0.013(3) C32 0.042(3) 0.023(2) 0.029(2) 0.0022(18) 0.018(2) 0.005(2) C33 0.026(2) 0.029(2) 0.023(2) 0.0018(17) 0.0102(17) 0.0021(19) C34 0.030(2) 0.028(3) 0.033(3) 0.0046(19) 0.014(2) 0.005(2) C35 0.029(3) 0.041(3) 0.044(3) 0.010(2) 0.021(2) 0.010(2) C36 0.027(2) 0.050(4) 0.032(3) 0.012(2) 0.006(2) 0.000(2) C37 0.031(3) 0.050(3) 0.031(3) -0.002(2) -0.002(2) -0.002(3) C38 0.033(2) 0.032(3) 0.026(2) 0.000(2) 0.0056(19) 0.007(2) C39 0.034(2) 0.032(3) 0.033(3) 0.008(2) 0.022(2) 0.009(2) C40 0.0172(19) 0.037(3) 0.045(3) -0.002(2) 0.0156(19) -0.003(2) C41 0.038(3) 0.027(2) 0.026(2) 0.0037(19) 0.0168(19) 0.000(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 P2 2.3170(12) . ? Pt1 P1 2.3375(11) . ? Pt1 Si1 2.3602(12) . ? Pt1 Si2 2.3973(12) . ? P1 C3 1.820(5) . ? P1 C9 1.825(5) . ? P1 C1 1.842(5) . ? P2 C15 1.819(5) . ? P2 C21 1.824(5) . ? P2 C2 1.849(5) . ? Si1 C27 1.899(5) . ? Si1 C33 1.904(5) . ? Si1 H1 1.419(19) . ? Si2 C41 1.892(5) . ? Si2 C39 1.895(5) . ? Si2 C40 1.901(5) . ? C1 C2 1.530(6) . ? C1 H1A 0.9599 . ? C1 H1B 0.9599 . ? C2 H2A 0.9599 . ? C2 H2B 0.9600 . ? C3 C4 1.400(7) . ? C3 C8 1.400(7) . ? C4 C5 1.395(7) . ? C4 H4 0.9600 . ? C5 C6 1.385(9) . ? C5 H5 0.9601 . ? C6 C7 1.399(9) . ? C6 H6 0.9597 . ? C7 C8 1.389(7) . ? C7 H7 0.9600 . ? C8 H8 0.9600 . ? C9 C10 1.388(7) . ? C9 C14 1.397(7) . ? C10 C11 1.397(8) . ? C10 H10 0.9601 . ? C11 C12 1.382(10) . ? C11 H11 0.9601 . ? C12 C13 1.374(9) . ? C12 H12 0.9599 . ? C13 C14 1.400(7) . ? C13 H13 0.9601 . ? C14 H14 0.9599 . ? C15 C20 1.393(6) . ? C15 C16 1.393(7) . ? C16 C17 1.393(7) . ? C16 H16 0.9601 . ? C17 C18 1.379(8) . ? C17 H17 0.9600 . ? C18 C19 1.382(8) . ? C18 H18 0.9601 . ? C19 C20 1.399(7) . ? C19 H19 0.9599 . ? C20 H20 0.9600 . ? C21 C22 1.397(6) . ? C21 C26 1.415(6) . ? C22 C23 1.386(7) . ? C22 H22 0.9600 . ? C23 C24 1.392(7) . ? C23 H23 0.9600 . ? C24 C25 1.389(7) . ? C24 H24 0.9600 . ? C25 C26 1.369(7) . ? C25 H25 0.9600 . ? C26 H26 0.9600 . ? C27 C28 1.398(7) . ? C27 C32 1.413(7) . ? C28 C29 1.392(7) . ? C28 H28 0.9599 . ? C29 C30 1.398(9) . ? C29 H29 0.9599 . ? C30 C31 1.383(9) . ? C30 H30 0.9600 . ? C31 C32 1.393(7) . ? C31 H31 0.9603 . ? C32 H32 0.9600 . ? C33 C38 1.400(7) . ? C33 C34 1.401(7) . ? C34 C35 1.401(7) . ? C34 H34 0.9600 . ? C35 C36 1.382(8) . ? C35 H35 0.9601 . ? C36 C37 1.387(8) . ? C36 H36 0.9601 . ? C37 C38 1.400(7) . ? C37 H37 0.9601 . ? C38 H38 0.9595 . ? C39 H39A 0.9601 . ? C39 H39B 0.9600 . ? C39 H39C 0.9599 . ? C40 H40A 0.9600 . ? C40 H40B 0.9601 . ? C40 H40C 0.9599 . ? C41 H41A 0.9602 . ? C41 H41B 0.9599 . ? C41 H41C 0.9599 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P2 Pt1 P1 84.48(4) . . ? P2 Pt1 Si1 169.33(4) . . ? P1 Pt1 Si1 97.44(4) . . ? P2 Pt1 Si2 96.41(4) . . ? P1 Pt1 Si2 171.13(4) . . ? Si1 Pt1 Si2 83.33(4) . . ? C3 P1 C9 104.7(2) . . ? C3 P1 C1 101.9(2) . . ? C9 P1 C1 104.6(2) . . ? C3 P1 Pt1 127.09(16) . . ? C9 P1 Pt1 109.85(15) . . ? C1 P1 Pt1 106.51(15) . . ? C15 P2 C21 106.6(2) . . ? C15 P2 C2 100.8(2) . . ? C21 P2 C2 105.4(2) . . ? C15 P2 Pt1 119.93(16) . . ? C21 P2 Pt1 113.38(15) . . ? C2 P2 Pt1 109.15(15) . . ? C27 Si1 C33 109.3(2) . . ? C27 Si1 Pt1 117.11(14) . . ? C33 Si1 Pt1 109.20(16) . . ? C27 Si1 H1 102(2) . . ? C33 Si1 H1 102(2) . . ? Pt1 Si1 H1 116(2) . . ? C41 Si2 C39 103.2(2) . . ? C41 Si2 C40 108.4(2) . . ? C39 Si2 C40 101.5(2) . . ? C41 Si2 Pt1 115.10(16) . . ? C39 Si2 Pt1 116.68(16) . . ? C40 Si2 Pt1 110.83(16) . . ? C2 C1 P1 109.5(3) . . ? C2 C1 H1A 109.5 . . ? P1 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? P1 C1 H1B 109.3 . . ? H1A C1 H1B 109.5 . . ? C1 C2 P2 111.0(3) . . ? C1 C2 H2A 108.8 . . ? P2 C2 H2A 109.6 . . ? C1 C2 H2B 108.7 . . ? P2 C2 H2B 109.2 . . ? H2A C2 H2B 109.5 . . ? C4 C3 C8 119.4(4) . . ? C4 C3 P1 122.9(4) . . ? C8 C3 P1 117.7(4) . . ? C5 C4 C3 120.0(5) . . ? C5 C4 H4 120.3 . . ? C3 C4 H4 119.7 . . ? C6 C5 C4 120.4(5) . . ? C6 C5 H5 119.8 . . ? C4 C5 H5 119.8 . . ? C5 C6 C7 119.8(5) . . ? C5 C6 H6 120.1 . . ? C7 C6 H6 120.1 . . ? C8 C7 C6 120.2(5) . . ? C8 C7 H7 120.1 . . ? C6 C7 H7 119.7 . . ? C7 C8 C3 120.2(5) . . ? C7 C8 H8 119.8 . . ? C3 C8 H8 120.0 . . ? C10 C9 C14 118.9(5) . . ? C10 C9 P1 123.3(4) . . ? C14 C9 P1 117.8(4) . . ? C9 C10 C11 120.3(6) . . ? C9 C10 H10 119.6 . . ? C11 C10 H10 120.1 . . ? C12 C11 C10 120.3(6) . . ? C12 C11 H11 119.4 . . ? C10 C11 H11 120.3 . . ? C13 C12 C11 120.0(5) . . ? C13 C12 H12 120.2 . . ? C11 C12 H12 119.8 . . ? C12 C13 C14 120.1(6) . . ? C12 C13 H13 120.3 . . ? C14 C13 H13 119.6 . . ? C9 C14 C13 120.3(5) . . ? C9 C14 H14 120.0 . . ? C13 C14 H14 119.7 . . ? C20 C15 C16 118.8(4) . . ? C20 C15 P2 116.5(3) . . ? C16 C15 P2 124.6(4) . . ? C17 C16 C15 120.3(5) . . ? C17 C16 H16 120.4 . . ? C15 C16 H16 119.3 . . ? C18 C17 C16 120.2(5) . . ? C18 C17 H17 119.5 . . ? C16 C17 H17 120.2 . . ? C17 C18 C19 120.4(5) . . ? C17 C18 H18 120.0 . . ? C19 C18 H18 119.6 . . ? C18 C19 C20 119.5(5) . . ? C18 C19 H19 120.2 . . ? C20 C19 H19 120.3 . . ? C15 C20 C19 120.7(5) . . ? C15 C20 H20 119.4 . . ? C19 C20 H20 119.9 . . ? C22 C21 C26 118.1(4) . . ? C22 C21 P2 119.8(3) . . ? C26 C21 P2 122.1(3) . . ? C23 C22 C21 120.5(5) . . ? C23 C22 H22 119.4 . . ? C21 C22 H22 120.0 . . ? C22 C23 C24 120.5(5) . . ? C22 C23 H23 120.0 . . ? C24 C23 H23 119.5 . . ? C25 C24 C23 119.3(4) . . ? C25 C24 H24 120.7 . . ? C23 C24 H24 120.0 . . ? C26 C25 C24 120.6(5) . . ? C26 C25 H25 119.0 . . ? C24 C25 H25 120.4 . . ? C25 C26 C21 120.9(4) . . ? C25 C26 H26 119.3 . . ? C21 C26 H26 119.8 . . ? C28 C27 C32 117.8(5) . . ? C28 C27 Si1 118.3(4) . . ? C32 C27 Si1 123.8(4) . . ? C29 C28 C27 121.7(6) . . ? C29 C28 H28 119.1 . . ? C27 C28 H28 119.2 . . ? C28 C29 C30 119.8(6) . . ? C28 C29 H29 120.4 . . ? C30 C29 H29 119.7 . . ? C31 C30 C29 119.2(5) . . ? C31 C30 H30 120.8 . . ? C29 C30 H30 120.0 . . ? C30 C31 C32 121.3(6) . . ? C30 C31 H31 119.6 . . ? C32 C31 H31 119.1 . . ? C31 C32 C27 120.2(5) . . ? C31 C32 H32 119.8 . . ? C27 C32 H32 120.0 . . ? C38 C33 C34 117.0(4) . . ? C38 C33 Si1 119.6(4) . . ? C34 C33 Si1 123.5(4) . . ? C35 C34 C33 122.1(5) . . ? C35 C34 H34 118.5 . . ? C33 C34 H34 119.5 . . ? C36 C35 C34 119.3(5) . . ? C36 C35 H35 120.4 . . ? C34 C35 H35 120.4 . . ? C35 C36 C37 120.4(5) . . ? C35 C36 H36 120.4 . . ? C37 C36 H36 119.2 . . ? C36 C37 C38 119.7(5) . . ? C36 C37 H37 119.6 . . ? C38 C37 H37 120.7 . . ? C33 C38 C37 121.6(5) . . ? C33 C38 H38 119.9 . . ? C37 C38 H38 118.5 . . ? Si2 C39 H39A 109.5 . . ? Si2 C39 H39B 109.4 . . ? H39A C39 H39B 109.5 . . ? Si2 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? Si2 C40 H40A 109.7 . . ? Si2 C40 H40B 109.4 . . ? H40A C40 H40B 109.5 . . ? Si2 C40 H40C 109.3 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? Si2 C41 H41A 109.6 . . ? Si2 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? Si2 C41 H41C 109.3 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.954 _diffrn_reflns_theta_full 27.94 _diffrn_measured_fraction_theta_full 0.954 _refine_diff_density_max 0.894 _refine_diff_density_min -2.173 _refine_diff_density_rms 0.156 #===END data_complex4c _database_code_depnum_ccdc_archive 'CCDC 761295' #TrackingRef 'CIF.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C71 H68 P4 Pt2 Si2' _chemical_formula_weight 1491.49 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' 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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 12.6750(3) _cell_length_b 16.3880(6) _cell_length_c 29.9580(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6222.8(3) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 54920 _cell_measurement_theta_min 2.10 _cell_measurement_theta_max 27.94 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.592 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2952 _exptl_absorpt_coefficient_mu 4.674 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method IP _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 54920 _diffrn_reflns_av_R_equivalents 0.089 _diffrn_reflns_av_sigmaI/netI 0.0339 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 39 _diffrn_reflns_theta_min 2.10 _diffrn_reflns_theta_max 27.94 _reflns_number_total 8147 _reflns_number_gt 7475 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'DIP Image plate' _computing_cell_refinement 'HKL Scalepack' _computing_data_reduction 'maXus (Mackay et al., 1999)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep (Johnson, 1976)' _computing_publication_material ? _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. The bond distance of Si1-H1 and the anisotropic displacements for C44-C46 and C53-C58 are restrained. ; _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^)+(0.0888P)^2^+41.2228P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.480(12) _refine_ls_number_reflns 8147 _refine_ls_number_parameters 719 _refine_ls_number_restraints 49 _refine_ls_R_factor_all 0.0583 _refine_ls_R_factor_gt 0.0526 _refine_ls_wR_factor_ref 0.1396 _refine_ls_wR_factor_gt 0.1349 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.021 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.15084(3) 0.18867(3) 0.186815(14) 0.02526(10) Uani 1 1 d . . . Pt2 Pt 0.43565(3) 0.10054(3) 0.188532(15) 0.02605(11) Uani 1 1 d . . . P1 P 0.0284(2) 0.2204(2) 0.24130(10) 0.0271(6) Uani 1 1 d . . . P2 P 0.0350(2) 0.2546(2) 0.13836(9) 0.0275(6) Uani 1 1 d . . . P3 P 0.5721(2) 0.08113(19) 0.23959(10) 0.0277(6) Uani 1 1 d . . . P4 P 0.5684(2) 0.1004(2) 0.13610(9) 0.0265(5) Uani 1 1 d . . . Si1 Si 0.2686(3) 0.0966(2) 0.22581(11) 0.0338(7) Uani 1 1 d D . . H1 H 0.217(5) 0.025(3) 0.218(2) -0.016(15) Uiso 1 1 d D . . Si2 Si 0.2978(2) 0.1481(2) 0.14120(11) 0.0289(7) Uani 1 1 d . . . H2 H 0.343(11) 0.207(8) 0.116(4) 0.035 Uiso 1 1 d . . . C1 C -0.0960(9) 0.2453(9) 0.2109(4) 0.035(3) Uani 1 1 d . . . H1A H -0.1276 0.1957 0.2002 0.041 Uiso 1 1 d R . . H1B H -0.1441 0.2724 0.2307 0.041 Uiso 1 1 d R . . C2 C -0.0761(10) 0.2991(7) 0.1714(4) 0.030(2) Uani 1 1 d . . . H2A H -0.0570 0.3529 0.1812 0.035 Uiso 1 1 d R . . H2B H -0.1379 0.3022 0.1530 0.035 Uiso 1 1 d R . . C3 C -0.0196(10) 0.1428(8) 0.2803(4) 0.031(2) Uani 1 1 d . . . C4 C -0.0411(9) 0.0673(8) 0.2630(4) 0.033(3) Uani 1 1 d . . . H4 H -0.0240 0.0559 0.2324 0.040 Uiso 1 1 d R . . C5 C -0.0867(12) 0.0064(8) 0.2895(5) 0.041(3) Uani 1 1 d . . . H5 H -0.1045 -0.0458 0.2770 0.049 Uiso 1 1 d R . . C6 C -0.1078(10) 0.0229(8) 0.3338(5) 0.038(3) Uani 1 1 d . . . H6 H -0.1402 -0.0179 0.3523 0.045 Uiso 1 1 d R . . C7 C -0.0814(12) 0.0982(9) 0.3520(4) 0.042(3) Uani 1 1 d . . . H7 H -0.0970 0.1095 0.3828 0.050 Uiso 1 1 d R . . C8 C -0.0337(10) 0.1567(7) 0.3247(4) 0.030(2) Uani 1 1 d . . . H8 H -0.0096 0.2067 0.3380 0.037 Uiso 1 1 d R . . C9 C 0.0512(9) 0.3079(7) 0.2777(3) 0.026(2) Uani 1 1 d . . . C10 C 0.1539(11) 0.3150(9) 0.2954(4) 0.039(3) Uani 1 1 d . . . H10 H 0.2086 0.2795 0.2847 0.047 Uiso 1 1 d R . . C11 C 0.1775(13) 0.3712(8) 0.3281(5) 0.047(3) Uani 1 1 d . . . H11 H 0.2474 0.3736 0.3405 0.057 Uiso 1 1 d R . . C12 C 0.0989(12) 0.4252(9) 0.3424(5) 0.044(3) Uani 1 1 d . . . H12 H 0.1148 0.4650 0.3650 0.053 Uiso 1 1 d R . . C13 C -0.0021(14) 0.4219(9) 0.3235(5) 0.051(4) Uani 1 1 d . . . H13 H -0.0547 0.4605 0.3328 0.061 Uiso 1 1 d R . . C14 C -0.0237(10) 0.3612(8) 0.2921(4) 0.036(3) Uani 1 1 d . . . H14 H -0.0943 0.3578 0.2806 0.043 Uiso 1 1 d R . . C15 C -0.0294(9) 0.1851(8) 0.0990(4) 0.030(2) Uani 1 1 d . . . C16 C 0.0103(9) 0.1071(8) 0.0946(4) 0.033(2) Uani 1 1 d . . . H16 H 0.0667 0.0893 0.1137 0.040 Uiso 1 1 d R . . C17 C -0.0305(11) 0.0536(8) 0.0622(5) 0.039(3) Uani 1 1 d . . . H17 H -0.0024 -0.0006 0.0594 0.047 Uiso 1 1 d R . . C18 C -0.1106(10) 0.0796(8) 0.0346(4) 0.035(3) Uani 1 1 d . . . H18 H -0.1382 0.0445 0.0118 0.041 Uiso 1 1 d R . . C19 C -0.1537(11) 0.1562(9) 0.0395(4) 0.040(3) Uani 1 1 d . . . H19 H -0.2107 0.1734 0.0205 0.048 Uiso 1 1 d R . . C20 C -0.1125(10) 0.2086(8) 0.0716(4) 0.035(3) Uani 1 1 d . . . H20 H -0.1433 0.2617 0.0750 0.043 Uiso 1 1 d R . . C21 C 0.0725(10) 0.3404(7) 0.1023(4) 0.028(2) Uani 1 1 d . . . C22 C 0.1785(10) 0.3507(8) 0.0914(4) 0.034(3) Uani 1 1 d . . . H22 H 0.2303 0.3128 0.1023 0.040 Uiso 1 1 d R . . C23 C 0.2108(13) 0.4141(9) 0.0645(4) 0.044(3) Uani 1 1 d . . . H23 H 0.2845 0.4203 0.0580 0.053 Uiso 1 1 d R . . C24 C 0.1386(12) 0.4687(8) 0.0473(4) 0.040(3) Uani 1 1 d . . . H24 H 0.1606 0.5118 0.0278 0.048 Uiso 1 1 d R . . C25 C 0.0325(14) 0.4618(9) 0.0582(5) 0.048(3) Uani 1 1 d . . . H25 H -0.0177 0.5004 0.0468 0.057 Uiso 1 1 d R . . C26 C -0.0010(11) 0.3987(9) 0.0860(5) 0.041(3) Uani 1 1 d . . . H26 H -0.0744 0.3939 0.0934 0.049 Uiso 1 1 d R . . C27 C 0.6941(9) 0.0571(7) 0.2066(4) 0.029(2) Uani 1 1 d . . . H27A H 0.7553 0.0659 0.2249 0.035 Uiso 1 1 d R . . H27B H 0.6918 0.0011 0.1974 0.035 Uiso 1 1 d R . . C28 C 0.6951(9) 0.1114(9) 0.1661(4) 0.035(3) Uani 1 1 d . . . H28A H 0.7521 0.0967 0.1465 0.042 Uiso 1 1 d R . . H28B H 0.7033 0.1671 0.1753 0.042 Uiso 1 1 d R . . C29 C 0.5809(10) 0.0040(8) 0.2838(4) 0.033(3) Uani 1 1 d . . . C30 C 0.6411(11) -0.0657(9) 0.2802(5) 0.040(3) Uani 1 1 d . . . H30 H 0.6850 -0.0736 0.2545 0.048 Uiso 1 1 d R . . C31 C 0.6393(11) -0.1249(8) 0.3131(6) 0.045(3) Uani 1 1 d . . . H31 H 0.6834 -0.1723 0.3103 0.054 Uiso 1 1 d R . . C32 C 0.5763(12) -0.1149(10) 0.3500(5) 0.049(4) Uani 1 1 d . . . H32 H 0.5728 -0.1566 0.3724 0.059 Uiso 1 1 d R . . C33 C 0.5158(14) -0.0469(11) 0.3543(6) 0.059(5) Uani 1 1 d . . . H33 H 0.4720 -0.0403 0.3802 0.070 Uiso 1 1 d R . . C34 C 0.5198(12) 0.0130(10) 0.3215(4) 0.046(3) Uani 1 1 d . . . H34 H 0.4792 0.0618 0.3257 0.056 Uiso 1 1 d R . . C35 C 0.6084(9) 0.1761(8) 0.2660(4) 0.029(2) Uani 1 1 d . . . C36 C 0.6779(10) 0.1805(9) 0.3018(4) 0.038(3) Uani 1 1 d . . . H36 H 0.7034 0.1311 0.3153 0.045 Uiso 1 1 d R . . C37 C 0.7103(12) 0.2562(9) 0.3183(6) 0.049(3) Uani 1 1 d . . . H37 H 0.7612 0.2592 0.3420 0.059 Uiso 1 1 d R . . C38 C 0.6710(13) 0.3276(9) 0.3002(5) 0.050(4) Uani 1 1 d . . . H38 H 0.6900 0.3790 0.3132 0.060 Uiso 1 1 d R . . C39 C 0.6011(13) 0.3249(10) 0.2643(6) 0.057(4) Uani 1 1 d . . . H39 H 0.5790 0.3749 0.2504 0.069 Uiso 1 1 d R . . C40 C 0.5688(13) 0.2477(8) 0.2479(5) 0.044(3) Uani 1 1 d . . . H40 H 0.5169 0.2454 0.2246 0.053 Uiso 1 1 d R . . C41 C 0.5824(10) 0.0025(7) 0.1078(4) 0.032(3) Uani 1 1 d . . . C42 C 0.6709(11) -0.0126(8) 0.0804(4) 0.039(3) Uani 1 1 d . . . H42 H 0.7219 0.0299 0.0755 0.047 Uiso 1 1 d R . . C43 C 0.6810(13) -0.0894(9) 0.0600(4) 0.046(4) Uani 1 1 d . . . H43 H 0.7410 -0.1009 0.0415 0.055 Uiso 1 1 d R . . C44 C 0.6054(14) -0.1492(10) 0.0663(7) 0.062(4) Uani 1 1 d U . . H44 H 0.6116 -0.2014 0.0520 0.075 Uiso 1 1 d R . . C45 C 0.5177(15) -0.1335(11) 0.0949(7) 0.066(4) Uani 1 1 d U . . H45 H 0.4667 -0.1758 0.0999 0.080 Uiso 1 1 d R . . C46 C 0.5081(14) -0.0578(10) 0.1154(7) 0.063(4) Uani 1 1 d U . . H46 H 0.4496 -0.0456 0.1347 0.076 Uiso 1 1 d R . . C47 C 0.5783(9) 0.1768(8) 0.0925(4) 0.029(2) Uani 1 1 d . . . C48 C 0.6145(11) 0.2555(9) 0.1018(4) 0.038(3) Uani 1 1 d . . . H48 H 0.6345 0.2693 0.1317 0.046 Uiso 1 1 d R . . C49 C 0.6211(11) 0.3128(9) 0.0687(5) 0.043(3) Uani 1 1 d . . . H49 H 0.6482 0.3661 0.0753 0.051 Uiso 1 1 d R . . C50 C 0.5906(11) 0.2944(9) 0.0248(4) 0.044(3) Uani 1 1 d . . . H50 H 0.5936 0.3358 0.0022 0.052 Uiso 1 1 d R . . C51 C 0.5546(13) 0.2205(10) 0.0153(4) 0.048(3) Uani 1 1 d . . . H51 H 0.5357 0.2067 -0.0148 0.057 Uiso 1 1 d R . . C52 C 0.5484(12) 0.1596(8) 0.0480(4) 0.038(3) Uani 1 1 d . . . H52 H 0.5226 0.1062 0.0406 0.045 Uiso 1 1 d R . . C53 C 0.2707(14) 0.1035(16) 0.2885(5) 0.068(3) Uani 1 1 d U . . C54 C 0.3304(14) 0.1656(15) 0.3100(6) 0.071(3) Uani 1 1 d U . . H54 H 0.3666 0.2048 0.2923 0.085 Uiso 1 1 calc R . . C55 C 0.3370(16) 0.1702(16) 0.3568(6) 0.078(3) Uani 1 1 d U . . H55 H 0.3792 0.2094 0.3718 0.094 Uiso 1 1 calc R . . C56 C 0.2748(17) 0.1107(18) 0.3801(7) 0.082(3) Uani 1 1 d U . . H56 H 0.2694 0.1167 0.4115 0.098 Uiso 1 1 calc R . . C57 C 0.2248(16) 0.0491(17) 0.3621(6) 0.079(3) Uani 1 1 d U . . H57 H 0.1952 0.0067 0.3797 0.095 Uiso 1 1 calc R . . C58 C 0.2173(14) 0.0491(15) 0.3154(6) 0.075(3) Uani 1 1 d U . . H58 H 0.1731 0.0097 0.3016 0.090 Uiso 1 1 calc R . . C59 C 0.2715(11) 0.0725(8) 0.0944(4) 0.034(3) Uani 1 1 d . . . C60 C 0.2820(12) 0.0980(12) 0.0493(5) 0.049(4) Uani 1 1 d . . . H60 H 0.2956 0.1545 0.0431 0.059 Uiso 1 1 d R . . C61 C 0.2699(14) 0.0389(13) 0.0152(6) 0.063(5) Uani 1 1 d . . . H61 H 0.2833 0.0536 -0.0153 0.075 Uiso 1 1 d R . . C62 C 0.2438(15) -0.0392(11) 0.0237(6) 0.060(5) Uani 1 1 d . . . H62 H 0.2316 -0.0761 -0.0007 0.072 Uiso 1 1 d R . . C63 C 0.2314(14) -0.0655(12) 0.0677(6) 0.060(5) Uani 1 1 d . . . H63 H 0.2150 -0.1215 0.0738 0.072 Uiso 1 1 d R . . C64 C 0.2449(12) -0.0089(10) 0.1033(5) 0.044(3) Uani 1 1 d . . . H64 H 0.2360 -0.0262 0.1337 0.053 Uiso 1 1 d R . . C65 C 0.420(2) 0.7144(12) -0.0111(8) 0.078(6) Uani 1 1 d . . . C66 C 0.331(2) 0.7317(14) 0.0131(9) 0.086(7) Uani 1 1 d . . . H66 H 0.2825 0.7725 0.0032 0.104 Uiso 1 1 d R . . C67 C 0.313(3) 0.6908(19) 0.0510(9) 0.097(8) Uani 1 1 d . . . H67 H 0.2544 0.7066 0.0696 0.116 Uiso 1 1 d R . . C68 C 0.367(3) 0.631(2) 0.0654(8) 0.111(10) Uani 1 1 d . . . H68 H 0.3405 0.6019 0.0909 0.134 Uiso 1 1 d R . . C69 C 0.462(3) 0.6130(19) 0.0404(11) 0.113(10) Uani 1 1 d . . . H69 H 0.5099 0.5739 0.0528 0.136 Uiso 1 1 d R . . C70 C 0.4844(18) 0.6537(14) 0.0032(8) 0.078(6) Uani 1 1 d . . . H70 H 0.5446 0.6400 -0.0147 0.093 Uiso 1 1 d R . . C71 C 0.441(4) 0.762(2) -0.0555(10) 0.159(17) Uani 1 1 d . . . H71A H 0.5060 0.7411 -0.0671 0.191 Uiso 1 1 d R . . H71B H 0.4478 0.8199 -0.0505 0.191 Uiso 1 1 d R . . H71C H 0.3853 0.7527 -0.0766 0.191 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.02089(17) 0.0339(2) 0.02100(17) 0.00076(17) -0.00127(16) 0.00058(15) Pt2 0.02169(17) 0.0335(2) 0.02301(18) -0.00013(18) -0.00214(17) 0.00244(15) P1 0.0242(13) 0.0334(14) 0.0238(13) -0.0003(11) -0.0002(10) 0.0000(12) P2 0.0245(13) 0.0377(15) 0.0203(12) 0.0027(11) -0.0027(10) 0.0000(12) P3 0.0222(12) 0.0350(15) 0.0260(13) 0.0024(11) -0.0039(11) 0.0024(11) P4 0.0216(12) 0.0329(14) 0.0249(12) -0.0009(11) 0.0028(10) 0.0011(12) Si1 0.0302(15) 0.0372(17) 0.0340(16) 0.0027(14) -0.0002(13) 0.0008(15) Si2 0.0225(14) 0.0391(18) 0.0251(14) 0.0014(13) -0.0014(11) -0.0010(13) C1 0.027(6) 0.046(7) 0.031(6) -0.005(5) -0.002(5) 0.010(5) C2 0.033(6) 0.032(6) 0.024(5) 0.005(4) -0.005(4) 0.002(5) C3 0.032(6) 0.040(6) 0.022(5) -0.001(5) -0.007(4) -0.005(5) C4 0.031(6) 0.037(6) 0.032(6) 0.007(5) -0.010(5) -0.007(5) C5 0.048(8) 0.031(6) 0.044(7) 0.008(5) -0.008(6) 0.002(6) C6 0.033(6) 0.034(6) 0.046(7) 0.021(6) 0.004(5) -0.003(5) C7 0.056(8) 0.040(7) 0.030(6) 0.006(5) 0.013(6) 0.008(7) C8 0.043(6) 0.022(5) 0.026(5) 0.001(4) 0.007(5) -0.002(5) C9 0.031(5) 0.023(5) 0.023(5) 0.005(4) -0.003(4) 0.004(4) C10 0.035(6) 0.038(6) 0.044(6) -0.003(6) -0.005(5) 0.006(6) C11 0.056(9) 0.035(7) 0.051(8) -0.001(6) -0.015(7) -0.005(6) C12 0.053(8) 0.044(7) 0.036(6) -0.004(6) 0.002(6) -0.008(6) C13 0.067(10) 0.042(7) 0.044(8) -0.015(6) 0.009(7) -0.003(7) C14 0.027(5) 0.046(7) 0.035(6) -0.003(5) 0.007(5) -0.007(5) C15 0.024(5) 0.038(6) 0.030(5) 0.005(5) -0.003(4) -0.001(5) C16 0.025(5) 0.042(7) 0.032(6) 0.004(5) -0.003(4) 0.006(5) C17 0.040(7) 0.032(6) 0.045(7) 0.004(5) 0.001(6) -0.002(5) C18 0.030(6) 0.039(7) 0.035(6) 0.003(5) -0.007(5) -0.006(5) C19 0.031(6) 0.052(8) 0.038(6) 0.004(6) -0.011(5) -0.006(6) C20 0.035(6) 0.038(7) 0.033(6) 0.004(5) 0.000(5) 0.002(5) C21 0.030(5) 0.032(5) 0.022(5) 0.001(4) 0.004(4) -0.006(5) C22 0.034(6) 0.039(6) 0.027(5) -0.006(5) -0.002(5) 0.000(5) C23 0.058(8) 0.046(8) 0.028(6) 0.003(5) 0.005(6) -0.003(7) C24 0.061(9) 0.033(6) 0.026(5) 0.003(5) 0.005(6) 0.000(6) C25 0.063(9) 0.044(7) 0.036(7) 0.010(6) -0.012(7) 0.007(7) C26 0.036(6) 0.039(7) 0.047(7) 0.002(6) -0.006(6) 0.000(6) C27 0.028(5) 0.032(6) 0.028(5) -0.001(4) -0.009(4) 0.012(5) C28 0.027(5) 0.046(7) 0.032(6) 0.003(5) 0.000(5) 0.004(5) C29 0.032(6) 0.037(6) 0.030(5) 0.002(5) 0.000(5) 0.004(5) C30 0.034(6) 0.042(7) 0.043(7) 0.003(6) 0.002(6) -0.001(6) C31 0.038(6) 0.040(7) 0.057(8) 0.009(7) -0.011(8) 0.000(5) C32 0.041(7) 0.055(9) 0.051(8) 0.021(7) -0.009(6) 0.003(7) C33 0.055(9) 0.071(11) 0.051(9) 0.026(8) 0.017(7) 0.025(9) C34 0.044(7) 0.056(8) 0.039(7) 0.018(6) 0.003(6) 0.018(7) C35 0.029(5) 0.036(6) 0.023(5) -0.005(4) 0.000(4) -0.003(5) C36 0.033(6) 0.042(7) 0.038(6) -0.002(5) -0.003(5) 0.002(5) C37 0.047(8) 0.047(8) 0.055(9) -0.007(7) -0.003(7) -0.008(6) C38 0.054(9) 0.036(7) 0.059(9) -0.012(6) -0.007(7) -0.002(6) C39 0.054(9) 0.038(8) 0.080(12) -0.003(8) -0.014(9) 0.010(7) C40 0.051(8) 0.035(6) 0.045(7) -0.003(6) -0.009(7) 0.000(6) C41 0.032(6) 0.023(5) 0.042(6) -0.001(5) -0.010(5) 0.000(4) C42 0.050(8) 0.038(7) 0.031(6) 0.006(5) 0.012(5) 0.016(6) C43 0.067(10) 0.043(7) 0.029(6) -0.001(5) 0.008(6) 0.025(7) C44 0.050(7) 0.041(6) 0.096(10) -0.024(7) 0.003(7) 0.003(6) C45 0.051(6) 0.043(6) 0.106(10) -0.020(6) 0.009(7) -0.003(5) C46 0.046(7) 0.042(7) 0.102(10) -0.019(7) 0.011(7) -0.007(6) C47 0.027(5) 0.034(6) 0.027(5) 0.004(5) 0.002(4) 0.004(5) C48 0.042(7) 0.041(7) 0.031(6) 0.000(5) 0.002(5) 0.005(6) C49 0.042(7) 0.036(6) 0.050(8) 0.000(6) 0.006(6) 0.005(6) C50 0.046(8) 0.049(8) 0.035(6) 0.015(6) 0.009(6) 0.019(6) C51 0.057(9) 0.060(9) 0.026(6) 0.009(6) 0.000(6) 0.009(8) C52 0.052(8) 0.037(6) 0.025(5) 0.003(5) -0.008(5) 0.006(6) C53 0.042(5) 0.121(9) 0.040(5) 0.012(5) 0.002(4) 0.021(6) C54 0.049(5) 0.121(8) 0.043(5) 0.005(6) -0.003(4) 0.025(5) C55 0.058(5) 0.127(9) 0.050(5) 0.004(6) -0.003(5) 0.025(6) C56 0.063(5) 0.131(9) 0.051(5) 0.009(6) -0.001(5) 0.021(6) C57 0.058(5) 0.131(9) 0.049(5) 0.015(6) 0.000(5) 0.018(6) C58 0.051(5) 0.128(9) 0.046(5) 0.016(6) 0.002(4) 0.017(6) C59 0.034(6) 0.039(6) 0.029(6) -0.003(5) -0.003(5) -0.001(5) C60 0.038(7) 0.070(10) 0.039(7) 0.003(7) 0.001(6) 0.011(8) C61 0.049(9) 0.092(14) 0.046(9) -0.016(9) -0.007(7) 0.006(10) C62 0.058(10) 0.060(10) 0.062(10) -0.029(8) -0.021(8) 0.017(9) C63 0.055(9) 0.060(10) 0.064(11) -0.026(9) -0.006(8) 0.009(8) C64 0.043(7) 0.051(8) 0.038(7) -0.005(6) -0.005(6) -0.002(7) C65 0.096(17) 0.046(10) 0.092(15) -0.008(10) -0.002(14) -0.003(11) C66 0.085(16) 0.062(13) 0.11(2) -0.034(13) -0.022(15) 0.015(12) C67 0.12(2) 0.10(2) 0.070(15) -0.026(15) 0.011(15) 0.014(18) C68 0.15(3) 0.12(3) 0.056(13) 0.004(14) 0.001(17) -0.01(2) C69 0.13(3) 0.086(19) 0.12(2) -0.001(18) -0.02(2) 0.00(2) C70 0.065(12) 0.080(14) 0.089(15) -0.024(12) -0.005(11) 0.013(11) C71 0.25(5) 0.13(3) 0.10(2) 0.01(2) 0.02(3) -0.03(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 P1 2.311(3) . ? Pt1 P2 2.331(3) . ? Pt1 Si2 2.404(3) . ? Pt1 Si1 2.422(4) . ? Pt2 P4 2.302(3) . ? Pt2 P3 2.330(3) . ? Pt2 Si2 2.382(3) . ? Pt2 Si1 2.394(3) . ? P1 C9 1.823(12) . ? P1 C3 1.832(13) . ? P1 C1 1.866(12) . ? P2 C15 1.832(13) . ? P2 C21 1.835(12) . ? P2 C2 1.869(12) . ? P3 C35 1.805(12) . ? P3 C29 1.834(13) . ? P3 C27 1.877(12) . ? P4 C47 1.815(12) . ? P4 C41 1.823(12) . ? P4 C28 1.849(12) . ? Si1 C53 1.883(17) . ? Si1 Si2 2.697(5) . ? Si1 H1 1.36(2) . ? Si2 C59 1.902(13) . ? Si2 H2 1.34(14) . ? C1 C2 1.498(16) . ? C1 H1A 0.9600 . ? C1 H1B 0.9601 . ? C2 H2A 0.9601 . ? C2 H2B 0.9598 . ? C3 C8 1.361(16) . ? C3 C4 1.368(17) . ? C4 C5 1.401(18) . ? C4 H4 0.9602 . ? C5 C6 1.382(19) . ? C5 H5 0.9600 . ? C6 C7 1.39(2) . ? C6 H6 0.9600 . ? C7 C8 1.398(17) . ? C7 H7 0.9603 . ? C8 H8 0.9600 . ? C9 C14 1.361(17) . ? C9 C10 1.410(17) . ? C10 C11 1.378(19) . ? C10 H10 0.9599 . ? C11 C12 1.40(2) . ? C11 H11 0.9601 . ? C12 C13 1.40(2) . ? C12 H12 0.9601 . ? C13 C14 1.397(19) . ? C13 H13 0.9599 . ? C14 H14 0.9600 . ? C15 C16 1.381(18) . ? C15 C20 1.389(16) . ? C16 C17 1.407(19) . ? C16 H16 0.9601 . ? C17 C18 1.376(18) . ? C17 H17 0.9601 . ? C18 C19 1.38(2) . ? C18 H18 0.9602 . ? C19 C20 1.392(19) . ? C19 H19 0.9602 . ? C20 H20 0.9601 . ? C21 C22 1.394(17) . ? C21 C26 1.420(18) . ? C22 C23 1.377(18) . ? C22 H22 0.9600 . ? C23 C24 1.38(2) . ? C23 H23 0.9601 . ? C24 C25 1.39(2) . ? C24 H24 0.9600 . ? C25 C26 1.40(2) . ? C25 H25 0.9600 . ? C26 H26 0.9600 . ? C27 C28 1.506(16) . ? C27 H27A 0.9600 . ? C27 H27B 0.9598 . ? C28 H28A 0.9599 . ? C28 H28B 0.9600 . ? C29 C34 1.377(18) . ? C29 C30 1.378(18) . ? C30 C31 1.383(19) . ? C30 H30 0.9600 . ? C31 C32 1.37(2) . ? C31 H31 0.9600 . ? C32 C33 1.36(2) . ? C32 H32 0.9601 . ? C33 C34 1.391(19) . ? C33 H33 0.9599 . ? C34 H34 0.9598 . ? C35 C40 1.387(18) . ? C35 C36 1.390(16) . ? C36 C37 1.398(19) . ? C36 H36 0.9599 . ? C37 C38 1.38(2) . ? C37 H37 0.9599 . ? C38 C39 1.39(2) . ? C38 H38 0.9600 . ? C39 C40 1.42(2) . ? C39 H39 0.9601 . ? C40 H40 0.9600 . ? C41 C46 1.38(2) . ? C41 C42 1.412(18) . ? C42 C43 1.405(18) . ? C42 H42 0.9600 . ? C43 C44 1.38(2) . ? C43 H43 0.9600 . ? C44 C45 1.43(3) . ? C44 H44 0.9601 . ? C45 C46 1.39(2) . ? C45 H45 0.9600 . ? C46 H46 0.9599 . ? C47 C48 1.397(18) . ? C47 C52 1.414(16) . ? C48 C49 1.367(19) . ? C48 H48 0.9598 . ? C49 C50 1.40(2) . ? C49 H49 0.9600 . ? C50 C51 1.32(2) . ? C50 H50 0.9599 . ? C51 C52 1.401(18) . ? C51 H51 0.9600 . ? C52 H52 0.9600 . ? C53 C58 1.38(3) . ? C53 C54 1.42(3) . ? C54 C55 1.41(2) . ? C54 H54 0.9500 . ? C55 C56 1.43(3) . ? C55 H55 0.9500 . ? C56 C57 1.31(3) . ? C56 H56 0.9500 . ? C57 C58 1.40(2) . ? C57 H57 0.9500 . ? C58 H58 0.9500 . ? C59 C64 1.40(2) . ? C59 C60 1.420(19) . ? C60 C61 1.42(2) . ? C60 H60 0.9600 . ? C61 C62 1.35(3) . ? C61 H61 0.9600 . ? C62 C63 1.40(3) . ? C62 H62 0.9600 . ? C63 C64 1.42(2) . ? C63 H63 0.9599 . ? C64 H64 0.9600 . ? C65 C70 1.36(3) . ? C65 C66 1.37(3) . ? C65 C71 1.57(4) . ? C66 C67 1.34(4) . ? C66 H66 0.9599 . ? C67 C68 1.28(4) . ? C67 H67 0.9602 . ? C68 C69 1.44(4) . ? C68 H68 0.9600 . ? C69 C70 1.33(4) . ? C69 H69 0.9598 . ? C70 H70 0.9599 . ? C71 H71A 0.9601 . ? C71 H71B 0.9600 . ? C71 H71C 0.9601 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P1 Pt1 P2 84.97(10) . . ? P1 Pt1 Si2 169.69(11) . . ? P2 Pt1 Si2 105.21(11) . . ? P1 Pt1 Si1 102.32(11) . . ? P2 Pt1 Si1 167.79(12) . . ? Si2 Pt1 Si1 67.95(11) . . ? P4 Pt2 P3 84.56(10) . . ? P4 Pt2 Si2 97.50(11) . . ? P3 Pt2 Si2 168.49(11) . . ? P4 Pt2 Si1 164.70(11) . . ? P3 Pt2 Si1 110.26(11) . . ? Si2 Pt2 Si1 68.76(11) . . ? C9 P1 C3 102.5(5) . . ? C9 P1 C1 104.7(6) . . ? C3 P1 C1 100.5(6) . . ? C9 P1 Pt1 119.5(4) . . ? C3 P1 Pt1 121.2(4) . . ? C1 P1 Pt1 105.8(4) . . ? C15 P2 C21 102.3(5) . . ? C15 P2 C2 104.4(5) . . ? C21 P2 C2 102.0(5) . . ? C15 P2 Pt1 113.2(4) . . ? C21 P2 Pt1 123.9(4) . . ? C2 P2 Pt1 109.0(3) . . ? C35 P3 C29 105.1(6) . . ? C35 P3 C27 101.6(6) . . ? C29 P3 C27 100.7(5) . . ? C35 P3 Pt2 111.1(4) . . ? C29 P3 Pt2 127.8(4) . . ? C27 P3 Pt2 107.2(4) . . ? C47 P4 C41 105.4(6) . . ? C47 P4 C28 102.8(6) . . ? C41 P4 C28 103.2(6) . . ? C47 P4 Pt2 122.8(4) . . ? C41 P4 Pt2 112.9(4) . . ? C28 P4 Pt2 107.7(4) . . ? C53 Si1 Pt2 116.8(6) . . ? C53 Si1 Pt1 116.9(7) . . ? Pt2 Si1 Pt1 107.66(13) . . ? C53 Si1 Si2 156.5(8) . . ? Pt2 Si1 Si2 55.40(10) . . ? Pt1 Si1 Si2 55.70(10) . . ? C53 Si1 H1 103(3) . . ? Pt2 Si1 H1 111(3) . . ? Pt1 Si1 H1 99(3) . . ? Si2 Si1 H1 100(3) . . ? C59 Si2 Pt2 110.7(4) . . ? C59 Si2 Pt1 117.6(4) . . ? Pt2 Si2 Pt1 108.70(13) . . ? C59 Si2 Si1 117.7(4) . . ? Pt2 Si2 Si1 55.85(10) . . ? Pt1 Si2 Si1 56.36(10) . . ? C59 Si2 H2 98(6) . . ? Pt2 Si2 H2 105(6) . . ? Pt1 Si2 H2 117(6) . . ? Si1 Si2 H2 143(6) . . ? C2 C1 P1 111.8(9) . . ? C2 C1 H1A 107.7 . . ? P1 C1 H1A 109.3 . . ? C2 C1 H1B 108.8 . . ? P1 C1 H1B 109.6 . . ? H1A C1 H1B 109.5 . . ? C1 C2 P2 108.4(8) . . ? C1 C2 H2A 110.0 . . ? P2 C2 H2A 109.3 . . ? C1 C2 H2B 110.3 . . ? P2 C2 H2B 109.2 . . ? H2A C2 H2B 109.5 . . ? C8 C3 C4 119.8(12) . . ? C8 C3 P1 123.4(10) . . ? C4 C3 P1 116.8(9) . . ? C3 C4 C5 120.7(12) . . ? C3 C4 H4 119.6 . . ? C5 C4 H4 119.6 . . ? C6 C5 C4 119.0(13) . . ? C6 C5 H5 120.3 . . ? C4 C5 H5 120.6 . . ? C5 C6 C7 120.3(12) . . ? C5 C6 H6 120.0 . . ? C7 C6 H6 119.7 . . ? C6 C7 C8 118.9(12) . . ? C6 C7 H7 119.8 . . ? C8 C7 H7 121.3 . . ? C3 C8 C7 120.9(12) . . ? C3 C8 H8 120.4 . . ? C7 C8 H8 118.7 . . ? C14 C9 C10 118.1(11) . . ? C14 C9 P1 125.7(9) . . ? C10 C9 P1 115.8(9) . . ? C11 C10 C9 121.6(13) . . ? C11 C10 H10 118.9 . . ? C9 C10 H10 119.4 . . ? C10 C11 C12 119.0(14) . . ? C10 C11 H11 120.2 . . ? C12 C11 H11 120.8 . . ? C11 C12 C13 120.2(13) . . ? C11 C12 H12 119.7 . . ? C13 C12 H12 120.1 . . ? C14 C13 C12 118.6(14) . . ? C14 C13 H13 121.8 . . ? C12 C13 H13 119.6 . . ? C9 C14 C13 122.3(13) . . ? C9 C14 H14 119.9 . . ? C13 C14 H14 117.8 . . ? C16 C15 C20 118.5(12) . . ? C16 C15 P2 118.3(9) . . ? C20 C15 P2 123.1(10) . . ? C15 C16 C17 120.5(11) . . ? C15 C16 H16 119.7 . . ? C17 C16 H16 119.7 . . ? C18 C17 C16 119.5(12) . . ? C18 C17 H17 120.6 . . ? C16 C17 H17 119.9 . . ? C17 C18 C19 120.8(12) . . ? C17 C18 H18 120.7 . . ? C19 C18 H18 118.5 . . ? C18 C19 C20 119.1(12) . . ? C18 C19 H19 120.2 . . ? C20 C19 H19 120.7 . . ? C15 C20 C19 121.5(13) . . ? C15 C20 H20 119.8 . . ? C19 C20 H20 118.7 . . ? C22 C21 C26 118.0(11) . . ? C22 C21 P2 118.8(10) . . ? C26 C21 P2 123.2(10) . . ? C23 C22 C21 121.0(13) . . ? C23 C22 H22 118.9 . . ? C21 C22 H22 120.1 . . ? C22 C23 C24 120.7(14) . . ? C22 C23 H23 119.3 . . ? C24 C23 H23 120.1 . . ? C23 C24 C25 120.2(13) . . ? C23 C24 H24 120.9 . . ? C25 C24 H24 118.9 . . ? C24 C25 C26 119.6(13) . . ? C24 C25 H25 120.4 . . ? C26 C25 H25 120.0 . . ? C25 C26 C21 120.3(13) . . ? C25 C26 H26 119.5 . . ? C21 C26 H26 120.1 . . ? C28 C27 P3 107.9(7) . . ? C28 C27 H27A 111.4 . . ? P3 C27 H27A 109.5 . . ? C28 C27 H27B 109.4 . . ? P3 C27 H27B 109.1 . . ? H27A C27 H27B 109.5 . . ? C27 C28 P4 109.1(9) . . ? C27 C28 H28A 110.5 . . ? P4 C28 H28A 109.5 . . ? C27 C28 H28B 109.3 . . ? P4 C28 H28B 109.1 . . ? H28A C28 H28B 109.5 . . ? C34 C29 C30 117.6(12) . . ? C34 C29 P3 119.0(10) . . ? C30 C29 P3 123.3(10) . . ? C29 C30 C31 121.2(13) . . ? C29 C30 H30 119.7 . . ? C31 C30 H30 119.1 . . ? C32 C31 C30 119.9(13) . . ? C32 C31 H31 120.4 . . ? C30 C31 H31 119.7 . . ? C33 C32 C31 120.3(13) . . ? C33 C32 H32 119.3 . . ? C31 C32 H32 120.3 . . ? C32 C33 C34 119.3(14) . . ? C32 C33 H33 119.9 . . ? C34 C33 H33 120.8 . . ? C29 C34 C33 121.7(14) . . ? C29 C34 H34 119.9 . . ? C33 C34 H34 118.4 . . ? C40 C35 C36 119.1(12) . . ? C40 C35 P3 117.8(9) . . ? C36 C35 P3 123.0(10) . . ? C35 C36 C37 120.3(13) . . ? C35 C36 H36 119.6 . . ? C37 C36 H36 120.1 . . ? C38 C37 C36 120.4(14) . . ? C38 C37 H37 119.3 . . ? C36 C37 H37 120.3 . . ? C37 C38 C39 120.4(14) . . ? C37 C38 H38 119.5 . . ? C39 C38 H38 120.0 . . ? C38 C39 C40 118.6(14) . . ? C38 C39 H39 119.5 . . ? C40 C39 H39 121.8 . . ? C35 C40 C39 121.1(13) . . ? C35 C40 H40 120.0 . . ? C39 C40 H40 118.9 . . ? C46 C41 C42 120.8(13) . . ? C46 C41 P4 119.0(11) . . ? C42 C41 P4 120.1(10) . . ? C43 C42 C41 118.8(14) . . ? C43 C42 H42 121.4 . . ? C41 C42 H42 119.8 . . ? C44 C43 C42 120.8(14) . . ? C44 C43 H43 119.2 . . ? C42 C43 H43 119.9 . . ? C43 C44 C45 119.6(14) . . ? C43 C44 H44 120.9 . . ? C45 C44 H44 119.5 . . ? C46 C45 C44 119.6(17) . . ? C46 C45 H45 121.1 . . ? C44 C45 H45 119.3 . . ? C41 C46 C45 120.3(17) . . ? C41 C46 H46 118.4 . . ? C45 C46 H46 121.3 . . ? C48 C47 C52 117.4(11) . . ? C48 C47 P4 121.1(9) . . ? C52 C47 P4 121.5(10) . . ? C49 C48 C47 120.6(13) . . ? C49 C48 H48 120.0 . . ? C47 C48 H48 119.3 . . ? C48 C49 C50 121.0(14) . . ? C48 C49 H49 119.8 . . ? C50 C49 H49 119.2 . . ? C51 C50 C49 119.5(13) . . ? C51 C50 H50 120.5 . . ? C49 C50 H50 119.9 . . ? C50 C51 C52 121.3(13) . . ? C50 C51 H51 120.2 . . ? C52 C51 H51 118.3 . . ? C51 C52 C47 120.1(13) . . ? C51 C52 H52 120.4 . . ? C47 C52 H52 119.4 . . ? C58 C53 C54 117.4(17) . . ? C58 C53 Si1 122.5(18) . . ? C54 C53 Si1 120.1(16) . . ? C55 C54 C53 121(2) . . ? C55 C54 H54 119.3 . . ? C53 C54 H54 119.3 . . ? C54 C55 C56 115(2) . . ? C54 C55 H55 122.7 . . ? C56 C55 H55 122.7 . . ? C57 C56 C55 126(2) . . ? C57 C56 H56 116.9 . . ? C55 C56 H56 116.9 . . ? C56 C57 C58 116(2) . . ? C56 C57 H57 121.8 . . ? C58 C57 H57 121.8 . . ? C53 C58 C57 123(2) . . ? C53 C58 H58 118.3 . . ? C57 C58 H58 118.3 . . ? C64 C59 C60 119.0(13) . . ? C64 C59 Si2 121.4(10) . . ? C60 C59 Si2 119.6(11) . . ? C61 C60 C59 118.3(17) . . ? C61 C60 H60 122.8 . . ? C59 C60 H60 118.9 . . ? C62 C61 C60 122.7(17) . . ? C62 C61 H61 117.5 . . ? C60 C61 H61 119.7 . . ? C61 C62 C63 120.0(16) . . ? C61 C62 H62 119.7 . . ? C63 C62 H62 120.4 . . ? C62 C63 C64 119.6(17) . . ? C62 C63 H63 119.9 . . ? C64 C63 H63 120.5 . . ? C59 C64 C63 120.4(15) . . ? C59 C64 H64 119.5 . . ? C63 C64 H64 120.2 . . ? C70 C65 C66 119(2) . . ? C70 C65 C71 122(3) . . ? C66 C65 C71 119(3) . . ? C67 C66 C65 120(2) . . ? C67 C66 H66 119.7 . . ? C65 C66 H66 120.7 . . ? C68 C67 C66 125(3) . . ? C68 C67 H67 115.3 . . ? C66 C67 H67 119.6 . . ? C67 C68 C69 115(3) . . ? C67 C68 H68 117.3 . . ? C69 C68 H68 127.2 . . ? C70 C69 C68 121(3) . . ? C70 C69 H69 121.5 . . ? C68 C69 H69 117.6 . . ? C69 C70 C65 120(3) . . ? C69 C70 H70 121.5 . . ? C65 C70 H70 118.3 . . ? C65 C71 H71A 105.7 . . ? C65 C71 H71B 112.0 . . ? H71A C71 H71B 109.5 . . ? C65 C71 H71C 110.6 . . ? H71A C71 H71C 109.5 . . ? H71B C71 H71C 109.5 . . ? _chemical_absolute_configuration unk _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.94 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.882 _refine_diff_density_min -2.878 _refine_diff_density_rms 0.203