Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2005 data_global _journal_coden_Cambridge 222 _publ_contact_author_name 'Gillian Reid' _publ_contact_author_address ; School of Chemistry University of Southampton Southampton SO17 1BJ, UK ; _publ_contact_author_email gr@soton.ac.uk _publ_contact_author_fax '023 8059 3781' _publ_contact_author_phone '023 8059 3609' loop_ _publ_author_name _publ_author_footnote _publ_author_address 'Brown, Michael D.' ? ; School of Chemistry University of Southampton Southampton SO17 1BJ, UK ; 'Levason, William' ? ; School of Chemistry University of Southampton Southampton SO17 1BJ, UK ; 'Reid, Gillian' ? ; School of Chemistry University of Southampton Southampton SO17 1BJ, UK ; 'Webster, Michael' ? ; School of Chemistry University of Southampton Southampton SO17 1BJ, UK ; _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Preparation, properties and structures of the first series of organometallic Pt(II) and Pt(IV) complexes with stibine co-ligands ; data_05mdb009 _database_code_depnum_ccdc_archive 'CCDC 285688' _audit_creation_method 'SHELXL-97 hand edit' _audit_creation_date 2005-07-01 _chemical_name_systematic ; Iodotrimethyl(1,3-bis(diphenylstibino)propane)platinum(IV) ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H35 I Pt Sb2' _chemical_formula_sum 'C30 H35 I Pt Sb2' _chemical_formula_weight 961.07 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' Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_Int_Tables_number 14 # Superceded ** _symmetry_space_group_name_Hall '-P 2ybc' # Superceded ** loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.611(3) _cell_length_b 12.557(5) _cell_length_c 19.535(5) _cell_angle_alpha 90.00 _cell_angle_beta 105.48(2) _cell_angle_gamma 90.00 _cell_volume 2981.4(16) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 7119 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour yellow _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 2.141 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1792 _exptl_absorpt_coefficient_mu 7.532 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6050 # shelxl 0.4651 _exptl_absorpt_correction_T_max 1.0000 # 0.5841 _exptl_absorpt_process_details 'G.M. Sheldrick, (2003). SADABS. Version 2.10. Bruker AXS Inc.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Nonius rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'area detector, Nonius Kappa ccd' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 41792 _diffrn_reflns_av_R_equivalents 0.1915 _diffrn_reflns_av_sigmaI/netI 0.1707 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 3.07 _diffrn_reflns_theta_max 27.73 _reflns_number_total 6924 _reflns_number_gt 3570 _reflns_threshold_expression I>2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _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 'w=1/[\s^2^(Fo^2^)+(0.0416P)^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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6924 _refine_ls_number_parameters 307 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1687 _refine_ls_R_factor_gt 0.0600 _refine_ls_wR_factor_ref 0.1236 _refine_ls_wR_factor_gt 0.0968 _refine_ls_goodness_of_fit_ref 0.987 _refine_ls_restrained_S_all 0.987 _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 0.16156(4) 0.02955(4) 0.22136(2) 0.02695(14) Uani 1 1 d . . . I1 I 0.30010(7) -0.13823(6) 0.21009(4) 0.0345(2) Uani 1 1 d . . . Sb1 Sb 0.24052(6) 0.02211(7) 0.35871(4) 0.0291(2) Uani 1 1 d . . . Sb2 Sb 0.32488(6) 0.15861(6) 0.21824(4) 0.0294(2) Uani 1 1 d . . . C1 C 0.2362(9) -0.1211(10) 0.4154(6) 0.035(3) Uani 1 1 d . . . C2 C 0.2035(9) -0.2172(10) 0.3801(6) 0.036(3) Uani 1 1 d . . . H2 H 0.1791 -0.2202 0.3297 0.043 Uiso 1 1 calc R . . C3 C 0.2076(9) -0.3067(10) 0.4205(7) 0.040(3) Uani 1 1 d . . . H3 H 0.1900 -0.3733 0.3972 0.048 Uiso 1 1 calc R . . C4 C 0.2360(9) -0.3040(12) 0.4934(8) 0.047(4) Uani 1 1 d . . . H4 H 0.2346 -0.3674 0.5197 0.057 Uiso 1 1 calc R . . C5 C 0.2666(11) -0.2093(12) 0.5280(7) 0.045(4) Uani 1 1 d . . . H5 H 0.2879 -0.2066 0.5784 0.054 Uiso 1 1 calc R . . C6 C 0.2662(9) -0.1185(11) 0.4890(6) 0.037(3) Uani 1 1 d . . . H6 H 0.2867 -0.0526 0.5128 0.045 Uiso 1 1 calc R . . C7 C 0.1597(9) 0.1228(10) 0.4161(6) 0.034(3) Uani 1 1 d . . . C8 C 0.0757(12) 0.0880(13) 0.4386(8) 0.060(4) Uani 1 1 d . . . H8 H 0.0594 0.0140 0.4361 0.072 Uiso 1 1 calc R . . C9 C 0.0105(14) 0.1566(16) 0.4658(10) 0.087(6) Uani 1 1 d . . . H9 H -0.0529 0.1302 0.4776 0.104 Uiso 1 1 calc R . . C10 C 0.0372(11) 0.2603(13) 0.4754(7) 0.050(4) Uani 1 1 d . . . H10 H -0.0049 0.3070 0.4961 0.061 Uiso 1 1 calc R . . C11 C 0.1248(12) 0.2969(13) 0.4551(8) 0.062(4) Uani 1 1 d . . . H11 H 0.1455 0.3697 0.4622 0.074 Uiso 1 1 calc R . . C12 C 0.1845(11) 0.2290(11) 0.4241(7) 0.049(4) Uani 1 1 d . . . H12 H 0.2438 0.2565 0.4081 0.059 Uiso 1 1 calc R . . C13 C 0.4114(9) 0.0650(11) 0.4018(6) 0.040(3) Uani 1 1 d . . . H13A H 0.4150 0.1399 0.4180 0.048 Uiso 1 1 calc R . . H13B H 0.4427 0.0201 0.4440 0.048 Uiso 1 1 calc R . . C14 C 0.4814(12) 0.0537(14) 0.3521(8) 0.069(5) Uani 1 1 d . . . H14A H 0.5587 0.0467 0.3807 0.082 Uiso 1 1 calc R . . H14B H 0.4611 -0.0137 0.3256 0.082 Uiso 1 1 calc R . . C15 C 0.4764(9) 0.1390(11) 0.3006(6) 0.041(3) Uani 1 1 d . . . H15A H 0.5362 0.1270 0.2773 0.049 Uiso 1 1 calc R . . H15B H 0.4925 0.2069 0.3270 0.049 Uiso 1 1 calc R . . C16 C 0.2967(10) 0.3236(10) 0.2233(7) 0.038(3) Uani 1 1 d . . . C17 C 0.3430(14) 0.3835(11) 0.2836(9) 0.068(5) Uani 1 1 d . . . H17 H 0.3898 0.3491 0.3238 0.082 Uiso 1 1 calc R . . C18 C 0.3238(17) 0.4885(14) 0.2871(10) 0.086(7) Uani 1 1 d . . . H18 H 0.3586 0.5283 0.3283 0.103 Uiso 1 1 calc R . . C19 C 0.2497(14) 0.5389(13) 0.2273(12) 0.070(5) Uani 1 1 d . . . H19 H 0.2309 0.6118 0.2300 0.084 Uiso 1 1 calc R . . C20 C 0.2075(13) 0.4843(13) 0.1683(11) 0.072(5) Uani 1 1 d . . . H20 H 0.1615 0.5188 0.1279 0.087 Uiso 1 1 calc R . . C21 C 0.2309(12) 0.3747(12) 0.1656(9) 0.063(4) Uani 1 1 d . . . H21 H 0.2006 0.3359 0.1231 0.075 Uiso 1 1 calc R . . C22 C 0.3857(9) 0.1582(9) 0.1262(6) 0.029(3) Uani 1 1 d . . . C23 C 0.4547(10) 0.2371(10) 0.1175(7) 0.039(3) Uani 1 1 d . . . H23 H 0.4742 0.2926 0.1517 0.047 Uiso 1 1 calc R . . C24 C 0.4972(9) 0.2363(10) 0.0577(7) 0.037(3) Uani 1 1 d . . . H24 H 0.5461 0.2909 0.0518 0.045 Uiso 1 1 calc R . . C25 C 0.4688(9) 0.1581(11) 0.0086(6) 0.037(3) Uani 1 1 d . . . H25 H 0.4963 0.1577 -0.0322 0.045 Uiso 1 1 calc R . . C26 C 0.3981(10) 0.0782(10) 0.0192(6) 0.038(3) Uani 1 1 d . . . H26 H 0.3771 0.0228 -0.0148 0.046 Uiso 1 1 calc R . . C27 C 0.3579(10) 0.0782(10) 0.0786(6) 0.038(3) Uani 1 1 d . . . H27 H 0.3112 0.0224 0.0858 0.046 Uiso 1 1 calc R . . C28 C 0.0913(10) 0.0308(11) 0.1107(6) 0.048(4) Uani 1 1 d . . . H28A H 0.1252 -0.0251 0.0886 0.072 Uiso 1 1 calc R . . H28B H 0.1040 0.1003 0.0915 0.072 Uiso 1 1 calc R . . H28C H 0.0120 0.0178 0.1006 0.072 Uiso 1 1 calc R . . C29 C 0.0308(9) -0.0730(11) 0.2229(6) 0.041(3) Uani 1 1 d . . . H29A H 0.0540 -0.1469 0.2202 0.061 Uiso 1 1 calc R . . H29B H -0.0320 -0.0573 0.1823 0.061 Uiso 1 1 calc R . . H29C H 0.0093 -0.0624 0.2671 0.061 Uiso 1 1 calc R . . C30 C 0.0590(10) 0.1552(11) 0.2286(6) 0.046(4) Uani 1 1 d . . . H30A H 0.0986 0.2225 0.2292 0.069 Uiso 1 1 calc R . . H30B H 0.0356 0.1485 0.2724 0.069 Uiso 1 1 calc R . . H30C H -0.0057 0.1542 0.1875 0.069 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.0271(3) 0.0260(3) 0.0275(2) 0.0015(2) 0.0068(2) 0.0008(2) I1 0.0435(5) 0.0261(5) 0.0356(4) -0.0006(4) 0.0134(4) 0.0055(4) Sb1 0.0307(4) 0.0307(5) 0.0260(4) 0.0002(4) 0.0079(4) 0.0013(4) Sb2 0.0325(5) 0.0238(5) 0.0325(5) -0.0001(4) 0.0094(4) -0.0031(4) C1 0.027(7) 0.046(9) 0.038(8) 0.004(6) 0.019(6) 0.001(6) C2 0.039(7) 0.036(9) 0.033(7) 0.023(6) 0.009(6) 0.011(6) C3 0.032(7) 0.030(8) 0.062(9) 0.012(7) 0.020(7) 0.001(6) C4 0.027(7) 0.053(11) 0.065(10) 0.039(8) 0.019(7) 0.019(7) C5 0.062(9) 0.049(10) 0.027(7) 0.020(7) 0.018(7) 0.004(8) C6 0.035(7) 0.044(9) 0.037(8) -0.003(6) 0.016(6) 0.000(6) C7 0.032(7) 0.037(9) 0.035(7) 0.009(6) 0.017(6) 0.000(6) C8 0.063(10) 0.046(10) 0.079(11) -0.013(9) 0.032(9) 0.002(8) C9 0.077(12) 0.090(16) 0.111(15) -0.023(13) 0.057(12) -0.028(12) C10 0.043(9) 0.061(12) 0.050(9) -0.014(8) 0.017(7) 0.006(8) C11 0.056(10) 0.056(11) 0.075(11) -0.036(9) 0.021(9) 0.001(8) C12 0.053(9) 0.033(9) 0.064(10) -0.002(7) 0.020(8) -0.002(7) C13 0.037(7) 0.045(9) 0.031(7) 0.005(6) 0.000(6) 0.002(6) C14 0.058(10) 0.079(13) 0.059(10) 0.006(9) -0.001(8) -0.015(9) C15 0.027(7) 0.049(9) 0.041(8) -0.004(7) -0.001(6) -0.010(6) C16 0.040(7) 0.028(8) 0.053(9) -0.011(7) 0.023(7) -0.014(6) C17 0.103(13) 0.021(9) 0.083(12) -0.024(8) 0.029(10) -0.002(9) C18 0.135(18) 0.057(13) 0.094(14) -0.057(11) 0.082(14) -0.046(12) C19 0.064(11) 0.033(10) 0.134(17) -0.008(12) 0.060(12) -0.006(9) C20 0.061(11) 0.040(11) 0.115(16) 0.024(11) 0.021(11) 0.017(9) C21 0.053(10) 0.033(10) 0.094(13) 0.010(9) 0.005(9) 0.001(8) C22 0.038(7) 0.009(6) 0.039(7) -0.001(6) 0.012(6) 0.002(6) C23 0.047(8) 0.026(8) 0.042(8) -0.002(6) 0.007(7) -0.017(6) C24 0.028(7) 0.031(8) 0.046(8) 0.017(7) 0.001(6) -0.006(6) C25 0.033(7) 0.045(9) 0.033(7) 0.005(7) 0.005(6) 0.002(7) C26 0.049(8) 0.036(9) 0.026(7) -0.014(6) 0.004(6) -0.002(7) C27 0.051(8) 0.025(8) 0.047(8) 0.002(6) 0.027(7) -0.008(6) C28 0.040(8) 0.055(10) 0.047(8) 0.011(8) 0.006(7) -0.001(7) C29 0.039(7) 0.050(9) 0.029(7) 0.006(6) 0.003(6) -0.009(7) C30 0.054(9) 0.053(10) 0.035(7) 0.012(7) 0.016(7) 0.004(8) _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 C30 2.069(13) . ? Pt1 C29 2.098(11) . ? Pt1 C28 2.106(12) . ? Pt1 Sb1 2.6025(11) . ? Pt1 Sb2 2.6342(11) . ? Pt1 I1 2.7830(11) . ? Sb1 C1 2.120(12) . ? Sb1 C7 2.122(12) . ? Sb1 C13 2.162(12) . ? Sb2 C16 2.109(13) . ? Sb2 C22 2.136(11) . ? Sb2 C15 2.159(11) . ? C1 C6 1.387(15) . ? C1 C2 1.396(17) . ? C2 C3 1.366(16) . ? C2 H2 0.9500 . ? C3 C4 1.374(17) . ? C3 H3 0.9500 . ? C4 C5 1.372(18) . ? C4 H4 0.9500 . ? C5 C6 1.371(16) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C8 1.325(16) . ? C7 C12 1.370(17) . ? C8 C9 1.39(2) . ? C8 H8 0.9500 . ? C9 C10 1.35(2) . ? C9 H9 0.9500 . ? C10 C11 1.351(18) . ? C10 H10 0.9500 . ? C11 C12 1.379(17) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C14 1.482(17) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.459(18) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C21 1.368(18) . ? C16 C17 1.388(18) . ? C17 C18 1.35(2) . ? C17 H17 0.9500 . ? C18 C19 1.43(2) . ? C18 H18 0.9500 . ? C19 C20 1.32(2) . ? C19 H19 0.9500 . ? C20 C21 1.412(19) . ? C20 H20 0.9500 . ? C21 H21 0.9500 . ? C22 C27 1.349(15) . ? C22 C23 1.359(15) . ? C23 C24 1.411(15) . ? C23 H23 0.9500 . ? C24 C25 1.351(16) . ? C24 H24 0.9500 . ? C25 C26 1.395(17) . ? C25 H25 0.9500 . ? C26 C27 1.384(15) . ? C26 H26 0.9500 . ? C27 H27 0.9500 . ? 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 . ? 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 C30 Pt1 C29 87.7(5) . . ? C30 Pt1 C28 88.0(5) . . ? C29 Pt1 C28 84.4(5) . . ? C30 Pt1 Sb1 91.8(3) . . ? C29 Pt1 Sb1 92.8(3) . . ? C28 Pt1 Sb1 177.2(3) . . ? C30 Pt1 Sb2 92.2(4) . . ? C29 Pt1 Sb2 179.5(3) . . ? C28 Pt1 Sb2 95.1(3) . . ? Sb1 Pt1 Sb2 87.68(3) . . ? C30 Pt1 I1 179.2(3) . . ? C29 Pt1 I1 92.8(4) . . ? C28 Pt1 I1 91.5(4) . . ? Sb1 Pt1 I1 88.79(3) . . ? Sb2 Pt1 I1 87.29(4) . . ? C1 Sb1 C7 98.4(4) . . ? C1 Sb1 C13 99.8(5) . . ? C7 Sb1 C13 102.4(5) . . ? C1 Sb1 Pt1 120.8(3) . . ? C7 Sb1 Pt1 114.7(3) . . ? C13 Sb1 Pt1 117.4(3) . . ? C16 Sb2 C22 98.3(4) . . ? C16 Sb2 C15 101.8(5) . . ? C22 Sb2 C15 100.5(4) . . ? C16 Sb2 Pt1 117.4(3) . . ? C22 Sb2 Pt1 118.5(3) . . ? C15 Sb2 Pt1 117.0(3) . . ? C6 C1 C2 119.7(11) . . ? C6 C1 Sb1 118.9(10) . . ? C2 C1 Sb1 121.4(9) . . ? C3 C2 C1 117.7(12) . . ? C3 C2 H2 121.2 . . ? C1 C2 H2 121.2 . . ? C2 C3 C4 122.6(13) . . ? C2 C3 H3 118.7 . . ? C4 C3 H3 118.7 . . ? C5 C4 C3 119.5(12) . . ? C5 C4 H4 120.2 . . ? C3 C4 H4 120.2 . . ? C6 C5 C4 119.3(12) . . ? C6 C5 H5 120.4 . . ? C4 C5 H5 120.4 . . ? C5 C6 C1 121.1(13) . . ? C5 C6 H6 119.5 . . ? C1 C6 H6 119.5 . . ? C8 C7 C12 117.5(12) . . ? C8 C7 Sb1 121.2(10) . . ? C12 C7 Sb1 120.9(9) . . ? C7 C8 C9 122.0(15) . . ? C7 C8 H8 119.0 . . ? C9 C8 H8 119.0 . . ? C10 C9 C8 120.1(14) . . ? C10 C9 H9 119.9 . . ? C8 C9 H9 119.9 . . ? C9 C10 C11 118.8(14) . . ? C9 C10 H10 120.6 . . ? C11 C10 H10 120.6 . . ? C10 C11 C12 120.2(15) . . ? C10 C11 H11 119.9 . . ? C12 C11 H11 119.9 . . ? C7 C12 C11 121.2(13) . . ? C7 C12 H12 119.4 . . ? C11 C12 H12 119.4 . . ? C14 C13 Sb1 115.3(9) . . ? C14 C13 H13A 108.5 . . ? Sb1 C13 H13A 108.5 . . ? C14 C13 H13B 108.5 . . ? Sb1 C13 H13B 108.5 . . ? H13A C13 H13B 107.5 . . ? C15 C14 C13 117.3(14) . . ? C15 C14 H14A 108.0 . . ? C13 C14 H14A 108.0 . . ? C15 C14 H14B 108.0 . . ? C13 C14 H14B 108.0 . . ? H14A C14 H14B 107.2 . . ? C14 C15 Sb2 117.7(9) . . ? C14 C15 H15A 107.9 . . ? Sb2 C15 H15A 107.9 . . ? C14 C15 H15B 107.9 . . ? Sb2 C15 H15B 107.9 . . ? H15A C15 H15B 107.2 . . ? C21 C16 C17 118.1(13) . . ? C21 C16 Sb2 119.7(10) . . ? C17 C16 Sb2 122.3(11) . . ? C18 C17 C16 122.2(17) . . ? C18 C17 H17 118.9 . . ? C16 C17 H17 118.9 . . ? C17 C18 C19 118.6(16) . . ? C17 C18 H18 120.7 . . ? C19 C18 H18 120.7 . . ? C20 C19 C18 120.2(16) . . ? C20 C19 H19 119.9 . . ? C18 C19 H19 119.9 . . ? C19 C20 C21 119.9(17) . . ? C19 C20 H20 120.1 . . ? C21 C20 H20 120.1 . . ? C16 C21 C20 120.9(16) . . ? C16 C21 H21 119.6 . . ? C20 C21 H21 119.6 . . ? C27 C22 C23 121.0(11) . . ? C27 C22 Sb2 119.7(8) . . ? C23 C22 Sb2 119.2(9) . . ? C22 C23 C24 119.6(11) . . ? C22 C23 H23 120.2 . . ? C24 C23 H23 120.2 . . ? C25 C24 C23 120.4(11) . . ? C25 C24 H24 119.8 . . ? C23 C24 H24 119.8 . . ? C24 C25 C26 118.4(11) . . ? C24 C25 H25 120.8 . . ? C26 C25 H25 120.8 . . ? C27 C26 C25 121.1(12) . . ? C27 C26 H26 119.4 . . ? C25 C26 H26 119.4 . . ? C22 C27 C26 119.4(11) . . ? C22 C27 H27 120.3 . . ? C26 C27 H27 120.3 . . ? Pt1 C28 H28A 109.5 . . ? Pt1 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? Pt1 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? Pt1 C29 H29A 109.5 . . ? Pt1 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? Pt1 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? Pt1 C30 H30A 109.5 . . ? Pt1 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? Pt1 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 27.73 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 1.442 _refine_diff_density_min -1.631 _refine_diff_density_rms 0.281 #===END OF CIF =============================================================== data_05mdb011 _database_code_depnum_ccdc_archive 'CCDC 285689' _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2005-07-01 _chemical_name_systematic ; Iodotrimethyl(1,3-bis(dimethylstibino)propane)platinum(IV) ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C10 H27 I Pt Sb2' _chemical_formula_sum 'C10 H27 I Pt Sb2' _chemical_formula_weight 712.81 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' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sb Sb -0.5866 1.5461 '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 n m a' _symmetry_Int_Tables_number 62 # Superceded ** _symmetry_space_group_name_Hall '-P 2ac 2n' # Superceded ** loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-x, y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z-1/2' 'x, -y-1/2, z' _cell_length_a 14.035(4) _cell_length_b 10.851(3) _cell_length_c 11.349(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1728.4(8) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 2205 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description 'cleaved fragment' _exptl_crystal_colour yellow _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.739 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1280 _exptl_absorpt_coefficient_mu 12.937 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5758 # shelxl 0.3578 _exptl_absorpt_correction_T_max 1.0000 # 0.5107 _exptl_absorpt_process_details 'G.M. Sheldrick, (2003). SADABS. Version 2.10. Bruker AXS Inc.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Nonius rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'area detector, Nonius Kappa ccd' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 10988 _diffrn_reflns_av_R_equivalents 0.0611 _diffrn_reflns_av_sigmaI/netI 0.0527 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.41 _diffrn_reflns_theta_max 27.54 _reflns_number_total 2081 _reflns_number_gt 1607 _reflns_threshold_expression I>2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _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 'w=1/[\s^2^(Fo^2^)+(0.0246P)^2^+3.0691P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2081 _refine_ls_number_parameters 74 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0558 _refine_ls_R_factor_gt 0.0346 _refine_ls_wR_factor_ref 0.0703 _refine_ls_wR_factor_gt 0.0644 _refine_ls_goodness_of_fit_ref 1.066 _refine_ls_restrained_S_all 1.066 _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 0.10432(2) 0.2500 0.40422(3) 0.01936(12) Uani 1 2 d S . . I1 I 0.30201(4) 0.2500 0.42534(6) 0.02788(18) Uani 1 2 d S . . Sb1 Sb 0.12050(3) 0.07971(4) 0.24158(4) 0.01956(13) Uani 1 1 d . . . C1 C 0.2031(5) -0.0767(7) 0.2863(7) 0.0341(18) Uani 1 1 d . . . H1A H 0.2687 -0.0511 0.3031 0.051 Uiso 1 1 calc R . . H1B H 0.2029 -0.1350 0.2204 0.051 Uiso 1 1 calc R . . H1C H 0.1759 -0.1164 0.3562 0.051 Uiso 1 1 calc R . . C2 C -0.0021(5) -0.0084(7) 0.1699(6) 0.0296(17) Uani 1 1 d . . . H2A H -0.0395 0.0516 0.1249 0.044 Uiso 1 1 calc R . . H2B H -0.0411 -0.0418 0.2340 0.044 Uiso 1 1 calc R . . H2C H 0.0179 -0.0757 0.1178 0.044 Uiso 1 1 calc R . . C3 C 0.1870(5) 0.1320(7) 0.0801(6) 0.0262(16) Uani 1 1 d . . . H3A H 0.2560 0.1426 0.0950 0.031 Uiso 1 1 calc R . . H3B H 0.1797 0.0632 0.0235 0.031 Uiso 1 1 calc R . . C4 C 0.1495(7) 0.2500 0.0217(8) 0.023(2) Uani 1 2 d S . . H4A H 0.1682 0.2500 -0.0624 0.027 Uiso 1 2 calc SR . . H4B H 0.0790 0.2500 0.0253 0.027 Uiso 1 2 calc SR . . C5 C -0.0439(7) 0.2500 0.3994(9) 0.030(2) Uani 1 2 d S . . H5A H -0.0657 0.2125 0.3256 0.046 Uiso 0.50 1 calc PR . . H5B H -0.0673 0.3350 0.4042 0.046 Uiso 0.50 1 calc PR . . H5C H -0.0686 0.2025 0.4662 0.046 Uiso 0.50 1 calc PR . . C6 C 0.0931(5) 0.3825(6) 0.5438(6) 0.0248(15) Uani 1 1 d . . . H6A H 0.1204 0.3480 0.6161 0.037 Uiso 1 1 calc R . . H6B H 0.0259 0.4026 0.5570 0.037 Uiso 1 1 calc R . . H6C H 0.1279 0.4574 0.5220 0.037 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.0206(2) 0.0196(2) 0.0179(2) 0.000 0.00024(15) 0.000 I1 0.0210(3) 0.0284(4) 0.0342(4) 0.000 -0.0013(3) 0.000 Sb1 0.0242(2) 0.0152(2) 0.0192(2) 0.00040(18) -0.00073(18) -0.00019(17) C1 0.044(5) 0.020(4) 0.039(4) 0.004(3) -0.007(3) 0.010(3) C2 0.032(4) 0.030(5) 0.026(4) 0.000(3) -0.006(3) -0.006(3) C3 0.027(4) 0.025(4) 0.026(4) -0.001(3) 0.006(3) 0.000(3) C4 0.029(5) 0.021(6) 0.018(5) 0.000 0.000(4) 0.000 C5 0.024(5) 0.033(6) 0.034(6) 0.000 -0.002(4) 0.000 C6 0.026(4) 0.024(4) 0.024(4) -0.006(3) -0.002(3) 0.002(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 C5 2.081(9) . ? Pt1 C6 2.145(6) . ? Pt1 C6 2.145(6) 8_565 ? Pt1 Sb1 2.6217(7) . ? Pt1 Sb1 2.6217(7) 8_565 ? Pt1 I1 2.7850(11) . ? Sb1 C1 2.117(7) . ? Sb1 C2 2.130(6) . ? Sb1 C3 2.133(6) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 C4 1.535(8) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C3 1.535(8) 8_565 ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C5 Pt1 C6 86.9(3) . . ? C5 Pt1 C6 86.9(3) . 8_565 ? C6 Pt1 C6 84.2(4) . 8_565 ? C5 Pt1 Sb1 93.91(19) . . ? C6 Pt1 Sb1 177.11(18) . . ? C6 Pt1 Sb1 93.08(19) 8_565 . ? C5 Pt1 Sb1 93.91(19) . 8_565 ? C6 Pt1 Sb1 93.08(19) . 8_565 ? C6 Pt1 Sb1 177.11(19) 8_565 8_565 ? Sb1 Pt1 Sb1 89.63(3) . 8_565 ? C5 Pt1 I1 176.6(3) . . ? C6 Pt1 I1 90.54(18) . . ? C6 Pt1 I1 90.54(18) 8_565 . ? Sb1 Pt1 I1 88.524(16) . . ? Sb1 Pt1 I1 88.524(16) 8_565 . ? C1 Sb1 C2 100.0(3) . . ? C1 Sb1 C3 100.4(3) . . ? C2 Sb1 C3 98.3(3) . . ? C1 Sb1 Pt1 116.3(2) . . ? C2 Sb1 Pt1 121.0(2) . . ? C3 Sb1 Pt1 117.08(19) . . ? Sb1 C1 H1A 109.5 . . ? Sb1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? Sb1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? Sb1 C2 H2A 109.5 . . ? Sb1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? Sb1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C4 C3 Sb1 116.3(5) . . ? C4 C3 H3A 108.2 . . ? Sb1 C3 H3A 108.2 . . ? C4 C3 H3B 108.2 . . ? Sb1 C3 H3B 108.2 . . ? H3A C3 H3B 107.4 . . ? C3 C4 C3 113.0(8) 8_565 . ? C3 C4 H4A 109.0 8_565 . ? C3 C4 H4A 109.0 . . ? C3 C4 H4B 109.0 8_565 . ? C3 C4 H4B 109.0 . . ? H4A C4 H4B 107.8 . . ? Pt1 C5 H5A 109.5 . . ? Pt1 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? Pt1 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? Pt1 C6 H6A 109.5 . . ? Pt1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? Pt1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 27.54 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 1.204 _refine_diff_density_min -1.628 _refine_diff_density_rms 0.263 #===END OF CIF =============================================================== data_05mdb016 _database_code_depnum_ccdc_archive 'CCDC 285690' _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2005-07-02 _chemical_name_systematic ; Iodotrimethyl(1,2-bis(dimethylstibinomethyl)benzene)platinum(IV) ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C15 H29 I Pt Sb2' _chemical_formula_sum 'C15 H29 I Pt Sb2' _chemical_formula_weight 774.87 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' Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_Int_Tables_number 14 # Superceded ** _symmetry_space_group_name_Hall '-P 2ybc' # Superceded ** loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.7559(16) _cell_length_b 9.2374(12) _cell_length_c 19.124(2) _cell_angle_alpha 90.00 _cell_angle_beta 102.258(6) _cell_angle_gamma 90.00 _cell_volume 2029.4(5) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 4746 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.536 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1408 _exptl_absorpt_coefficient_mu 11.030 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7391 # shelxl 0.1771 _exptl_absorpt_correction_T_max 1.0000 # 0.2164 _exptl_absorpt_process_details 'G.M. Sheldrick, (2003). SADABS. Version 2.10. Bruker AXS Inc.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Nonius rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'area detector, Nonius Kappa ccd' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 18921 _diffrn_reflns_av_R_equivalents 0.0336 _diffrn_reflns_av_sigmaI/netI 0.0319 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.33 _diffrn_reflns_theta_max 27.52 _reflns_number_total 4624 _reflns_number_gt 4108 _reflns_threshold_expression I>2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _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 'w=1/[\s^2^(Fo^2^)+(0.0256P)^2^+5.2677P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4624 _refine_ls_number_parameters 172 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0314 _refine_ls_R_factor_gt 0.0252 _refine_ls_wR_factor_ref 0.0598 _refine_ls_wR_factor_gt 0.0573 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.055 _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 0.304452(15) -0.314008(19) 0.341448(9) 0.01302(6) Uani 1 1 d . . . Sb1 Sb 0.30668(3) -0.03055(3) 0.346932(15) 0.01330(8) Uani 1 1 d . . . Sb2 Sb 0.18242(3) -0.34726(3) 0.439210(16) 0.01277(8) Uani 1 1 d . . . I1 I 0.08809(3) -0.27789(4) 0.250382(16) 0.02106(8) Uani 1 1 d . . . C1 C 0.2792(5) 0.0702(6) 0.2452(3) 0.0249(11) Uani 1 1 d . . . H1A H 0.2101 0.0284 0.2138 0.037 Uiso 1 1 calc R . . H1B H 0.3473 0.0546 0.2241 0.037 Uiso 1 1 calc R . . H1C H 0.2673 0.1743 0.2505 0.037 Uiso 1 1 calc R . . C2 C 0.4599(4) 0.0818(6) 0.4012(3) 0.0230(11) Uani 1 1 d . . . H2A H 0.4834 0.0451 0.4502 0.035 Uiso 1 1 calc R . . H2B H 0.4432 0.1856 0.4024 0.035 Uiso 1 1 calc R . . H2C H 0.5229 0.0659 0.3758 0.035 Uiso 1 1 calc R . . C3 C 0.1752(4) 0.0808(5) 0.3895(2) 0.0143(9) Uani 1 1 d . . . H3A H 0.1775 0.1849 0.3777 0.017 Uiso 1 1 calc R . . H3B H 0.0978 0.0431 0.3656 0.017 Uiso 1 1 calc R . . C4 C 0.1887(4) 0.0652(5) 0.4693(2) 0.0146(9) Uani 1 1 d . . . C5 C 0.2480(4) 0.1714(5) 0.5139(3) 0.0190(10) Uani 1 1 d . . . H5 H 0.2807 0.2508 0.4934 0.023 Uiso 1 1 calc R . . C6 C 0.2611(5) 0.1649(6) 0.5876(3) 0.0229(11) Uani 1 1 d . . . H6 H 0.3022 0.2389 0.6171 0.028 Uiso 1 1 calc R . . C7 C 0.2136(4) 0.0495(6) 0.6180(3) 0.0221(11) Uani 1 1 d . . . H7 H 0.2215 0.0440 0.6684 0.027 Uiso 1 1 calc R . . C8 C 0.1547(4) -0.0569(5) 0.5744(2) 0.0186(10) Uani 1 1 d . . . H8 H 0.1229 -0.1361 0.5955 0.022 Uiso 1 1 calc R . . C9 C 0.1405(4) -0.0516(5) 0.4997(2) 0.0149(9) Uani 1 1 d . . . C10 C 0.0731(4) -0.1706(5) 0.4561(3) 0.0163(10) Uani 1 1 d . . . H10A H 0.0330 -0.1312 0.4092 0.020 Uiso 1 1 calc R . . H10B H 0.0128 -0.2068 0.4809 0.020 Uiso 1 1 calc R . . C11 C 0.2680(5) -0.3949(6) 0.5469(3) 0.0254(11) Uani 1 1 d . . . H11A H 0.3284 -0.3222 0.5636 0.038 Uiso 1 1 calc R . . H11B H 0.3038 -0.4910 0.5489 0.038 Uiso 1 1 calc R . . H11C H 0.2111 -0.3932 0.5777 0.038 Uiso 1 1 calc R . . C12 C 0.0583(4) -0.5174(5) 0.4165(3) 0.0213(11) Uani 1 1 d . . . H12A H 0.0129 -0.5069 0.3675 0.032 Uiso 1 1 calc R . . H12B H 0.0060 -0.5128 0.4501 0.032 Uiso 1 1 calc R . . H12C H 0.0987 -0.6108 0.4214 0.032 Uiso 1 1 calc R . . C13 C 0.3045(5) -0.5409(5) 0.3296(3) 0.0246(12) Uani 1 1 d . . . H13A H 0.2335 -0.5711 0.2960 0.037 Uiso 1 1 calc R . . H13B H 0.3074 -0.5868 0.3762 0.037 Uiso 1 1 calc R . . H13C H 0.3728 -0.5704 0.3113 0.037 Uiso 1 1 calc R . . C14 C 0.4640(4) -0.3453(6) 0.4112(3) 0.0259(12) Uani 1 1 d . . . H14A H 0.4518 -0.3584 0.4600 0.039 Uiso 1 1 calc R . . H14B H 0.5137 -0.2606 0.4098 0.039 Uiso 1 1 calc R . . H14C H 0.5018 -0.4316 0.3968 0.039 Uiso 1 1 calc R . . C15 C 0.3983(5) -0.2962(6) 0.2591(3) 0.0269(12) Uani 1 1 d . . . H15A H 0.3440 -0.2793 0.2133 0.040 Uiso 1 1 calc R . . H15B H 0.4416 -0.3859 0.2563 0.040 Uiso 1 1 calc R . . H15C H 0.4530 -0.2150 0.2694 0.040 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.01365(10) 0.01246(10) 0.01340(10) 0.00034(7) 0.00384(7) 0.00145(6) Sb1 0.01741(16) 0.01178(16) 0.01120(15) 0.00051(11) 0.00414(12) -0.00075(11) Sb2 0.01435(15) 0.01136(15) 0.01282(15) 0.00018(11) 0.00336(12) -0.00001(11) I1 0.02095(16) 0.02401(18) 0.01542(16) -0.00196(13) -0.00247(12) 0.00016(13) C1 0.036(3) 0.025(3) 0.015(2) 0.007(2) 0.009(2) 0.001(2) C2 0.017(2) 0.023(3) 0.027(3) -0.002(2) 0.001(2) -0.003(2) C3 0.020(2) 0.009(2) 0.014(2) 0.0024(17) 0.0059(18) 0.0019(18) C4 0.017(2) 0.011(2) 0.016(2) -0.0043(18) 0.0039(18) 0.0069(18) C5 0.019(2) 0.017(3) 0.022(3) 0.0000(19) 0.005(2) 0.0006(18) C6 0.021(3) 0.028(3) 0.020(3) -0.010(2) 0.005(2) 0.000(2) C7 0.027(3) 0.029(3) 0.010(2) -0.003(2) 0.003(2) 0.006(2) C8 0.018(2) 0.021(3) 0.019(2) 0.003(2) 0.0086(19) 0.0056(19) C9 0.012(2) 0.016(2) 0.016(2) -0.0035(19) 0.0032(18) 0.0057(18) C10 0.014(2) 0.015(2) 0.022(3) -0.0022(19) 0.0087(19) 0.0008(17) C11 0.027(3) 0.029(3) 0.019(3) 0.003(2) 0.002(2) 0.003(2) C12 0.022(3) 0.015(2) 0.029(3) -0.001(2) 0.009(2) -0.0048(19) C13 0.042(3) 0.008(2) 0.028(3) 0.000(2) 0.016(2) 0.001(2) C14 0.010(2) 0.033(3) 0.031(3) 0.008(2) -0.003(2) 0.007(2) C15 0.031(3) 0.030(3) 0.022(3) -0.006(2) 0.011(2) 0.010(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 C14 2.078(5) . ? Pt1 C13 2.108(5) . ? Pt1 C15 2.113(5) . ? Pt1 Sb2 2.6052(4) . ? Pt1 Sb1 2.6204(5) . ? Pt1 I1 2.7808(5) . ? Sb1 C1 2.119(5) . ? Sb1 C2 2.146(5) . ? Sb1 C3 2.154(4) . ? Sb2 C12 2.126(5) . ? Sb2 C11 2.138(5) . ? Sb2 C10 2.144(4) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 C4 1.508(6) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.387(6) . ? C4 C9 1.401(7) . ? C5 C6 1.387(7) . ? C5 H5 0.9500 . ? C6 C7 1.387(7) . ? C6 H6 0.9500 . ? C7 C8 1.376(7) . ? C7 H7 0.9500 . ? C8 C9 1.403(6) . ? C8 H8 0.9500 . ? C9 C10 1.501(6) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C14 Pt1 C13 84.8(2) . . ? C14 Pt1 C15 86.9(2) . . ? C13 Pt1 C15 89.2(2) . . ? C14 Pt1 Sb2 94.71(16) . . ? C13 Pt1 Sb2 88.42(14) . . ? C15 Pt1 Sb2 176.95(15) . . ? C14 Pt1 Sb1 96.50(15) . . ? C13 Pt1 Sb1 175.98(14) . . ? C15 Pt1 Sb1 87.11(15) . . ? Sb2 Pt1 Sb1 95.246(11) . . ? C14 Pt1 I1 178.33(16) . . ? C13 Pt1 I1 94.21(15) . . ? C15 Pt1 I1 94.41(15) . . ? Sb2 Pt1 I1 83.901(15) . . ? Sb1 Pt1 I1 84.562(11) . . ? C1 Sb1 C2 100.4(2) . . ? C1 Sb1 C3 98.93(19) . . ? C2 Sb1 C3 100.50(19) . . ? C1 Sb1 Pt1 113.82(15) . . ? C2 Sb1 Pt1 120.18(14) . . ? C3 Sb1 Pt1 119.35(12) . . ? C12 Sb2 C11 101.9(2) . . ? C12 Sb2 C10 100.71(18) . . ? C11 Sb2 C10 100.7(2) . . ? C12 Sb2 Pt1 113.54(14) . . ? C11 Sb2 Pt1 119.84(15) . . ? C10 Sb2 Pt1 117.24(13) . . ? Sb1 C1 H1A 109.5 . . ? Sb1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? Sb1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? Sb1 C2 H2A 109.5 . . ? Sb1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? Sb1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C4 C3 Sb1 114.1(3) . . ? C4 C3 H3A 108.7 . . ? Sb1 C3 H3A 108.7 . . ? C4 C3 H3B 108.7 . . ? Sb1 C3 H3B 108.7 . . ? H3A C3 H3B 107.6 . . ? C5 C4 C9 118.9(4) . . ? C5 C4 C3 119.1(4) . . ? C9 C4 C3 121.9(4) . . ? C6 C5 C4 121.8(5) . . ? C6 C5 H5 119.1 . . ? C4 C5 H5 119.1 . . ? C5 C6 C7 119.4(5) . . ? C5 C6 H6 120.3 . . ? C7 C6 H6 120.3 . . ? C8 C7 C6 119.4(4) . . ? C8 C7 H7 120.3 . . ? C6 C7 H7 120.3 . . ? C7 C8 C9 121.8(5) . . ? C7 C8 H8 119.1 . . ? C9 C8 H8 119.1 . . ? C4 C9 C8 118.6(4) . . ? C4 C9 C10 123.1(4) . . ? C8 C9 C10 118.3(4) . . ? C9 C10 Sb2 112.2(3) . . ? C9 C10 H10A 109.2 . . ? Sb2 C10 H10A 109.2 . . ? C9 C10 H10B 109.2 . . ? Sb2 C10 H10B 109.2 . . ? H10A C10 H10B 107.9 . . ? Sb2 C11 H11A 109.5 . . ? Sb2 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? Sb2 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? Sb2 C12 H12A 109.5 . . ? Sb2 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? Sb2 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? Pt1 C13 H13A 109.5 . . ? Pt1 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? Pt1 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? Pt1 C14 H14A 109.5 . . ? Pt1 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? Pt1 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? Pt1 C15 H15A 109.5 . . ? Pt1 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? Pt1 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 27.52 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 1.056 _refine_diff_density_min -1.402 _refine_diff_density_rms 0.199 #===END OF CIF =============================================================== # 05mdb012a.cif data_05mdb012 _database_code_depnum_ccdc_archive 'CCDC 285691' _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2005-07-04 _chemical_name_systematic ; Iodotrimethylbis(triphenylstibine)platinum(IV) ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C39 H39 I Pt Sb2' _chemical_formula_sum 'C39 H39 I Pt Sb2' _chemical_formula_weight 1073.19 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' Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_Int_Tables_number 2 # Superceded ** _symmetry_space_group_name_Hall '-P 1' # Superceded ** loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.6674(10) _cell_length_b 18.681(3) _cell_length_c 19.993(3) _cell_angle_alpha 81.604(7) _cell_angle_beta 89.966(8) _cell_angle_gamma 83.681(8) _cell_volume 3549.7(7) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 15874 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.008 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2024 _exptl_absorpt_coefficient_mu 6.338 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6729 # shelxl 0.4707 _exptl_absorpt_correction_T_max 1.0000 # 0.7856 _exptl_absorpt_process_details 'G.M. Sheldrick, (2003). SADABS. Version 2.10. Bruker AXS Inc.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Nonius rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'area detector, Nonius Kappa ccd' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 75972 _diffrn_reflns_av_R_equivalents 0.0943 _diffrn_reflns_av_sigmaI/netI 0.0987 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.93 _diffrn_reflns_theta_max 27.62 _reflns_number_total 16313 _reflns_number_gt 10820 _reflns_threshold_expression I>2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _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 'w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+29.4023P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 16313 _refine_ls_number_parameters 777 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1066 _refine_ls_R_factor_gt 0.0572 _refine_ls_wR_factor_ref 0.1031 _refine_ls_wR_factor_gt 0.0906 _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_restrained_S_all 1.058 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.28337(4) 0.24992(2) 0.670754(18) 0.03438(11) Uani 1 1 d . . . Pt2 Pt -0.10824(4) -0.25719(2) 0.828996(18) 0.02996(10) Uani 1 1 d . . . I1 I 0.23832(10) 0.39162(5) 0.63458(5) 0.0373(3) Uani 0.6398(19) 1 d P . . I1A I 0.28427(15) 0.11591(8) 0.70311(8) 0.0322(5) Uani 0.3602(19) 1 d P . . C38A C 0.23832(10) 0.39162(5) 0.63458(5) 0.0373(3) Uani 0.3602(19) 1 d P . . C38 C 0.28427(15) 0.11591(8) 0.70311(8) 0.0322(5) Uani 0.6398(19) 1 d P . . I2 I -0.09525(11) -0.39942(6) 0.86126(5) 0.0332(3) Uani 0.5627(18) 1 d P . . I2A I -0.16336(13) -0.11876(7) 0.79702(7) 0.0318(4) Uani 0.4373(18) 1 d P . . C77A C -0.09525(11) -0.39942(6) 0.86126(5) 0.0332(3) Uani 0.4373(18) 1 d P . . C77 C -0.16336(13) -0.11876(7) 0.79702(7) 0.0318(4) Uani 0.5627(18) 1 d P . . Sb1 Sb 0.42100(6) 0.27034(3) 0.77950(3) 0.02288(14) Uani 1 1 d . . . Sb2 Sb 0.50505(6) 0.22789(3) 0.59397(3) 0.02232(14) Uani 1 1 d . . . Sb3 Sb 0.09864(6) -0.23214(3) 0.90745(3) 0.02231(14) Uani 1 1 d . . . Sb4 Sb 0.04502(6) -0.27538(3) 0.72126(3) 0.02373(14) Uani 1 1 d . . . C1 C 0.4986(9) 0.1804(5) 0.8536(4) 0.027(2) Uani 1 1 d . . . C2 C 0.5654(9) 0.1183(5) 0.8333(5) 0.033(2) Uani 1 1 d . . . H2 H 0.5752 0.1161 0.7864 0.039 Uiso 1 1 calc R . . C3 C 0.6186(11) 0.0592(6) 0.8795(6) 0.046(3) Uani 1 1 d . . . H3 H 0.6658 0.0172 0.8645 0.055 Uiso 1 1 calc R . . C4 C 0.6020(12) 0.0622(6) 0.9475(6) 0.054(3) Uani 1 1 d . . . H4 H 0.6370 0.0216 0.9796 0.065 Uiso 1 1 calc R . . C5 C 0.5347(12) 0.1237(6) 0.9697(5) 0.050(3) Uani 1 1 d . . . H5 H 0.5234 0.1256 1.0166 0.060 Uiso 1 1 calc R . . C6 C 0.4847(10) 0.1820(6) 0.9225(5) 0.040(3) Uani 1 1 d . . . H6 H 0.4394 0.2244 0.9375 0.048 Uiso 1 1 calc R . . C7 C 0.2974(8) 0.3350(5) 0.8415(4) 0.025(2) Uani 1 1 d . . . C8 C 0.1982(9) 0.3046(5) 0.8846(5) 0.032(2) Uani 1 1 d . . . H8 H 0.1873 0.2544 0.8871 0.039 Uiso 1 1 calc R . . C9 C 0.1161(10) 0.3472(5) 0.9234(5) 0.036(2) Uani 1 1 d . . . H9 H 0.0511 0.3261 0.9538 0.043 Uiso 1 1 calc R . . C10 C 0.1293(9) 0.4201(5) 0.9177(5) 0.037(2) Uani 1 1 d . . . H10 H 0.0723 0.4494 0.9442 0.045 Uiso 1 1 calc R . . C11 C 0.2226(10) 0.4519(5) 0.8747(5) 0.038(2) Uani 1 1 d . . . H11 H 0.2304 0.5025 0.8716 0.046 Uiso 1 1 calc R . . C12 C 0.3059(9) 0.4093(5) 0.8356(5) 0.029(2) Uani 1 1 d . . . H12 H 0.3690 0.4312 0.8047 0.035 Uiso 1 1 calc R . . C13 C 0.5966(8) 0.3312(5) 0.7690(4) 0.025(2) Uani 1 1 d . . . C14 C 0.6807(10) 0.3335(6) 0.8230(5) 0.045(3) Uani 1 1 d . . . H14 H 0.6635 0.3070 0.8660 0.054 Uiso 1 1 calc R . . C15 C 0.7916(11) 0.3748(7) 0.8147(5) 0.056(3) Uani 1 1 d . . . H15 H 0.8480 0.3779 0.8528 0.067 Uiso 1 1 calc R . . C16 C 0.8216(10) 0.4107(6) 0.7541(5) 0.041(3) Uani 1 1 d . . . H16 H 0.9000 0.4375 0.7491 0.049 Uiso 1 1 calc R . . C17 C 0.7371(12) 0.4082(6) 0.6994(5) 0.053(3) Uani 1 1 d . . . H17 H 0.7573 0.4336 0.6564 0.063 Uiso 1 1 calc R . . C18 C 0.6231(10) 0.3692(5) 0.7060(5) 0.038(3) Uani 1 1 d . . . H18 H 0.5639 0.3685 0.6683 0.046 Uiso 1 1 calc R . . C19 C 0.6224(9) 0.3113(5) 0.5455(4) 0.024(2) Uani 1 1 d . . . C20 C 0.5503(10) 0.3782(5) 0.5146(5) 0.034(2) Uani 1 1 d . . . H20 H 0.4519 0.3865 0.5173 0.041 Uiso 1 1 calc R . . C21 C 0.6232(10) 0.4303(5) 0.4812(5) 0.037(2) Uani 1 1 d . . . H21 H 0.5745 0.4745 0.4594 0.045 Uiso 1 1 calc R . . C22 C 0.7654(11) 0.4202(5) 0.4783(5) 0.041(3) Uani 1 1 d . . . H22 H 0.8145 0.4577 0.4555 0.049 Uiso 1 1 calc R . . C23 C 0.8374(10) 0.3559(6) 0.5083(5) 0.043(3) Uani 1 1 d . . . H23 H 0.9360 0.3489 0.5062 0.051 Uiso 1 1 calc R . . C24 C 0.7649(9) 0.3009(6) 0.5419(5) 0.037(2) Uani 1 1 d . . . H24 H 0.8143 0.2563 0.5623 0.044 Uiso 1 1 calc R . . C25 C 0.6729(8) 0.1522(5) 0.6388(4) 0.024(2) Uani 1 1 d . . . C26 C 0.6892(10) 0.0815(6) 0.6255(5) 0.043(3) Uani 1 1 d . . . H26 H 0.6258 0.0659 0.5959 0.052 Uiso 1 1 calc R . . C27 C 0.7987(12) 0.0330(6) 0.6557(6) 0.056(3) Uani 1 1 d . . . H27 H 0.8115 -0.0152 0.6451 0.068 Uiso 1 1 calc R . . C28 C 0.8880(10) 0.0535(6) 0.7002(5) 0.043(3) Uani 1 1 d . . . H28 H 0.9610 0.0194 0.7212 0.051 Uiso 1 1 calc R . . C29 C 0.8721(9) 0.1241(6) 0.7148(5) 0.041(3) Uani 1 1 d . . . H29 H 0.9342 0.1387 0.7457 0.049 Uiso 1 1 calc R . . C30 C 0.7646(9) 0.1737(5) 0.6837(4) 0.034(2) Uani 1 1 d . . . H30 H 0.7539 0.2224 0.6933 0.041 Uiso 1 1 calc R . . C31 C 0.4673(9) 0.1774(5) 0.5065(4) 0.026(2) Uani 1 1 d . . . C32 C 0.5314(9) 0.1984(5) 0.4470(5) 0.035(2) Uani 1 1 d . . . H32 H 0.5897 0.2364 0.4442 0.042 Uiso 1 1 calc R . . C33 C 0.5127(9) 0.1655(6) 0.3916(5) 0.041(3) Uani 1 1 d . . . H33 H 0.5592 0.1799 0.3508 0.049 Uiso 1 1 calc R . . C34 C 0.4255(11) 0.1109(6) 0.3952(5) 0.050(3) Uani 1 1 d . . . H34 H 0.4109 0.0889 0.3562 0.060 Uiso 1 1 calc R . . C35 C 0.3606(15) 0.0886(7) 0.4539(6) 0.078(5) Uani 1 1 d . . . H35 H 0.3033 0.0501 0.4567 0.094 Uiso 1 1 calc R . . C36 C 0.3803(13) 0.1239(7) 0.5100(5) 0.065(4) Uani 1 1 d . . . H36 H 0.3328 0.1105 0.5508 0.078 Uiso 1 1 calc R . . C37 C 0.1485(10) 0.2382(8) 0.5914(5) 0.077(5) Uani 1 1 d . . . H37A H 0.2027 0.2317 0.5509 0.116 Uiso 1 1 calc R . . H37B H 0.0815 0.2819 0.5818 0.116 Uiso 1 1 calc R . . H37C H 0.0985 0.1956 0.6046 0.116 Uiso 1 1 calc R . . C39 C 0.1020(10) 0.2604(8) 0.7295(5) 0.065(4) Uani 1 1 d . . . H39A H 0.1279 0.2676 0.7753 0.097 Uiso 1 1 calc R . . H39B H 0.0554 0.2162 0.7318 0.097 Uiso 1 1 calc R . . H39C H 0.0389 0.3024 0.7087 0.097 Uiso 1 1 calc R . . C40 C 0.0359(8) -0.1792(5) 0.9922(4) 0.0229(19) Uani 1 1 d . . . C41 C -0.0791(12) -0.1293(6) 0.9904(5) 0.061(4) Uani 1 1 d . . . H41 H -0.1362 -0.1183 0.9507 0.073 Uiso 1 1 calc R . . C42 C -0.1128(14) -0.0951(7) 1.0453(6) 0.075(5) Uani 1 1 d . . . H42 H -0.1943 -0.0614 1.0436 0.090 Uiso 1 1 calc R . . C43 C -0.0312(12) -0.1086(6) 1.1025(5) 0.052(3) Uani 1 1 d . . . H43 H -0.0539 -0.0834 1.1397 0.063 Uiso 1 1 calc R . . C44 C 0.0819(11) -0.1581(6) 1.1054(5) 0.043(3) Uani 1 1 d . . . H44 H 0.1393 -0.1682 1.1450 0.051 Uiso 1 1 calc R . . C45 C 0.1141(9) -0.1939(5) 1.0510(5) 0.035(2) Uani 1 1 d . . . H45 H 0.1925 -0.2298 1.0542 0.042 Uiso 1 1 calc R . . C46 C 0.2470(9) -0.3157(5) 0.9589(4) 0.025(2) Uani 1 1 d . . . C47 C 0.2041(10) -0.3834(5) 0.9844(4) 0.030(2) Uani 1 1 d . . . H47 H 0.1115 -0.3928 0.9762 0.036 Uiso 1 1 calc R . . C48 C 0.2952(11) -0.4366(5) 1.0211(5) 0.041(3) Uani 1 1 d . . . H48 H 0.2645 -0.4819 1.0395 0.049 Uiso 1 1 calc R . . C49 C 0.4323(10) -0.4239(6) 1.0314(5) 0.041(3) Uani 1 1 d . . . H49 H 0.4950 -0.4607 1.0567 0.049 Uiso 1 1 calc R . . C50 C 0.4778(10) -0.3585(5) 1.0053(5) 0.037(2) Uani 1 1 d . . . H50 H 0.5716 -0.3502 1.0121 0.044 Uiso 1 1 calc R . . C51 C 0.3854(9) -0.3044(5) 0.9688(4) 0.030(2) Uani 1 1 d . . . H51 H 0.4169 -0.2593 0.9504 0.035 Uiso 1 1 calc R . . C52 C 0.2375(8) -0.1572(5) 0.8635(4) 0.025(2) Uani 1 1 d . . . C53 C 0.2158(10) -0.0834(5) 0.8730(5) 0.037(2) Uani 1 1 d . . . H53 H 0.1414 -0.0667 0.8999 0.044 Uiso 1 1 calc R . . C54 C 0.3046(11) -0.0358(6) 0.8426(5) 0.047(3) Uani 1 1 d . . . H54 H 0.2922 0.0136 0.8498 0.056 Uiso 1 1 calc R . . C55 C 0.4096(10) -0.0583(5) 0.8025(5) 0.039(2) Uani 1 1 d . . . H55 H 0.4679 -0.0242 0.7814 0.046 Uiso 1 1 calc R . . C56 C 0.4318(9) -0.1284(5) 0.7925(5) 0.035(2) Uani 1 1 d . . . H56 H 0.5073 -0.1438 0.7656 0.043 Uiso 1 1 calc R . . C58 C 0.2465(9) -0.3354(5) 0.7320(5) 0.027(2) Uani 1 1 d . . . C57 C 0.3436(9) -0.1784(5) 0.8217(5) 0.031(2) Uani 1 1 d . . . H57 H 0.3566 -0.2273 0.8128 0.038 Uiso 1 1 calc R . . C59 C 0.2992(10) -0.3655(5) 0.7957(5) 0.035(2) Uani 1 1 d . . . H59 H 0.2444 -0.3595 0.8343 0.042 Uiso 1 1 calc R . . C60 C 0.4319(10) -0.4045(5) 0.8041(5) 0.039(2) Uani 1 1 d . . . H60 H 0.4668 -0.4249 0.8480 0.047 Uiso 1 1 calc R . . C61 C 0.5117(10) -0.4129(6) 0.7475(6) 0.043(3) Uani 1 1 d . . . H61 H 0.6035 -0.4371 0.7524 0.052 Uiso 1 1 calc R . . C62 C 0.4570(10) -0.3859(7) 0.6842(6) 0.053(3) Uani 1 1 d . . . H62 H 0.5100 -0.3941 0.6455 0.064 Uiso 1 1 calc R . . C63 C 0.3270(9) -0.3472(6) 0.6759(5) 0.039(3) Uani 1 1 d . . . H63 H 0.2918 -0.3284 0.6317 0.046 Uiso 1 1 calc R . . C64 C 0.0835(8) -0.1836(5) 0.6483(4) 0.025(2) Uani 1 1 d . . . C65 C 0.1263(9) -0.1229(5) 0.6708(5) 0.029(2) Uani 1 1 d . . . H65 H 0.1390 -0.1221 0.7178 0.035 Uiso 1 1 calc R . . C66 C 0.1508(10) -0.0629(5) 0.6237(6) 0.044(3) Uani 1 1 d . . . H66 H 0.1799 -0.0211 0.6391 0.053 Uiso 1 1 calc R . . C67 C 0.1336(11) -0.0630(6) 0.5552(6) 0.046(3) Uani 1 1 d . . . H67 H 0.1501 -0.0218 0.5236 0.055 Uiso 1 1 calc R . . C68 C 0.0919(11) -0.1243(6) 0.5339(5) 0.047(3) Uani 1 1 d . . . H68 H 0.0791 -0.1250 0.4869 0.057 Uiso 1 1 calc R . . C69 C 0.0684(10) -0.1850(5) 0.5795(5) 0.038(2) Uani 1 1 d . . . H69 H 0.0420 -0.2272 0.5637 0.045 Uiso 1 1 calc R . . C70 C -0.0495(9) -0.3390(5) 0.6577(4) 0.025(2) Uani 1 1 d . . . C71 C -0.0051(9) -0.4122(5) 0.6588(5) 0.030(2) Uani 1 1 d . . . H71 H 0.0704 -0.4348 0.6875 0.036 Uiso 1 1 calc R . . C72 C -0.0708(9) -0.4525(5) 0.6178(4) 0.030(2) Uani 1 1 d . . . H72 H -0.0395 -0.5026 0.6182 0.036 Uiso 1 1 calc R . . C73 C -0.1807(10) -0.4202(5) 0.5767(5) 0.035(2) Uani 1 1 d . . . H73 H -0.2252 -0.4481 0.5488 0.042 Uiso 1 1 calc R . . C74 C -0.2266(10) -0.3484(6) 0.5756(5) 0.039(2) Uani 1 1 d . . . H74 H -0.3026 -0.3265 0.5469 0.047 Uiso 1 1 calc R . . C75 C -0.1627(9) -0.3070(5) 0.6164(4) 0.029(2) Uani 1 1 d . . . H75 H -0.1959 -0.2572 0.6161 0.035 Uiso 1 1 calc R . . C76 C -0.2814(9) -0.2670(7) 0.7688(5) 0.058(4) Uani 1 1 d . . . H76A H -0.2512 -0.2716 0.7227 0.087 Uiso 1 1 calc R . . H76B H -0.3488 -0.2236 0.7680 0.087 Uiso 1 1 calc R . . H76C H -0.3250 -0.3103 0.7878 0.087 Uiso 1 1 calc R . . C78 C -0.2518(11) -0.2503(7) 0.9072(5) 0.059(3) Uani 1 1 d . . . H78A H -0.2028 -0.2448 0.9487 0.088 Uiso 1 1 calc R . . H78B H -0.2983 -0.2947 0.9147 0.088 Uiso 1 1 calc R . . H78C H -0.3212 -0.2081 0.8946 0.088 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.02231(19) 0.0595(3) 0.0219(2) -0.00756(19) -0.00067(15) -0.00482(18) Pt2 0.02409(19) 0.0458(3) 0.0220(2) -0.00843(18) 0.00361(15) -0.00832(17) I1 0.0413(6) 0.0335(6) 0.0319(6) 0.0043(4) 0.0059(4) 0.0076(4) I1A 0.0333(9) 0.0342(10) 0.0302(9) -0.0045(7) 0.0024(7) -0.0089(7) C38A 0.0413(6) 0.0335(6) 0.0319(6) 0.0043(4) 0.0059(4) 0.0076(4) C38 0.0333(9) 0.0342(10) 0.0302(9) -0.0045(7) 0.0024(7) -0.0089(7) I2 0.0356(6) 0.0297(7) 0.0328(7) 0.0009(5) -0.0010(5) -0.0043(5) I2A 0.0299(7) 0.0341(8) 0.0306(8) -0.0043(6) -0.0017(6) -0.0001(6) C77A 0.0356(6) 0.0297(7) 0.0328(7) 0.0009(5) -0.0010(5) -0.0043(5) C77 0.0299(7) 0.0341(8) 0.0306(8) -0.0043(6) -0.0017(6) -0.0001(6) Sb1 0.0258(3) 0.0215(3) 0.0209(3) -0.0021(3) -0.0001(2) -0.0014(2) Sb2 0.0238(3) 0.0224(3) 0.0215(3) -0.0039(3) -0.0004(2) -0.0048(2) Sb3 0.0227(3) 0.0230(3) 0.0208(3) -0.0037(3) 0.0014(2) 0.0001(2) Sb4 0.0291(3) 0.0219(3) 0.0207(3) -0.0036(3) 0.0028(3) -0.0044(3) C1 0.031(5) 0.028(5) 0.024(5) -0.001(4) 0.003(4) -0.012(4) C2 0.031(5) 0.023(5) 0.045(6) -0.002(5) -0.007(5) -0.005(4) C3 0.056(7) 0.035(6) 0.045(7) 0.001(5) -0.012(6) -0.006(5) C4 0.063(8) 0.043(7) 0.051(8) 0.015(6) -0.016(6) -0.009(6) C5 0.072(8) 0.050(8) 0.022(6) 0.008(5) -0.005(5) -0.003(6) C6 0.042(6) 0.037(6) 0.040(6) 0.000(5) -0.005(5) -0.004(5) C7 0.023(4) 0.026(5) 0.028(5) -0.006(4) 0.004(4) -0.010(4) C8 0.033(5) 0.026(5) 0.037(6) -0.003(4) -0.003(4) -0.006(4) C9 0.042(6) 0.040(6) 0.029(6) -0.016(5) 0.004(5) -0.012(5) C10 0.031(5) 0.042(6) 0.042(6) -0.021(5) 0.010(5) 0.002(5) C11 0.039(6) 0.023(5) 0.055(7) -0.011(5) 0.017(5) -0.006(4) C12 0.027(5) 0.018(5) 0.042(6) -0.002(4) 0.008(4) -0.003(4) C13 0.024(5) 0.021(5) 0.030(5) -0.008(4) 0.002(4) -0.001(4) C14 0.037(6) 0.062(8) 0.033(6) 0.009(5) 0.002(5) -0.018(5) C15 0.038(6) 0.096(10) 0.033(7) 0.004(6) -0.012(5) -0.020(6) C16 0.043(6) 0.046(7) 0.037(6) -0.005(5) 0.006(5) -0.016(5) C17 0.077(8) 0.050(7) 0.034(6) 0.004(5) -0.004(6) -0.037(6) C18 0.057(7) 0.029(6) 0.034(6) -0.004(5) -0.001(5) -0.024(5) C19 0.028(5) 0.020(5) 0.027(5) -0.008(4) 0.002(4) -0.012(4) C20 0.036(5) 0.037(6) 0.032(6) -0.008(5) 0.007(4) -0.016(5) C21 0.050(6) 0.035(6) 0.026(5) -0.004(5) 0.013(5) -0.002(5) C22 0.055(7) 0.018(5) 0.051(7) -0.008(5) 0.028(5) -0.006(5) C23 0.028(5) 0.038(6) 0.062(8) -0.008(6) 0.010(5) -0.004(5) C24 0.027(5) 0.042(6) 0.039(6) -0.007(5) 0.015(4) 0.004(4) C25 0.023(4) 0.028(5) 0.019(5) 0.005(4) -0.001(4) -0.010(4) C26 0.045(6) 0.040(7) 0.047(7) -0.010(5) -0.019(5) -0.007(5) C27 0.064(8) 0.029(6) 0.075(9) -0.014(6) -0.019(7) 0.006(6) C28 0.032(6) 0.054(7) 0.039(6) -0.006(5) -0.007(5) 0.008(5) C29 0.027(5) 0.053(7) 0.044(7) -0.016(6) -0.003(5) 0.003(5) C30 0.032(5) 0.041(6) 0.028(5) -0.012(5) -0.006(4) 0.003(5) C31 0.029(5) 0.025(5) 0.025(5) -0.007(4) -0.002(4) 0.000(4) C32 0.030(5) 0.040(6) 0.040(6) -0.019(5) 0.005(5) -0.007(4) C33 0.031(5) 0.054(7) 0.043(7) -0.023(6) 0.016(5) -0.009(5) C34 0.064(7) 0.058(8) 0.037(7) -0.022(6) -0.006(6) -0.021(6) C35 0.133(12) 0.093(11) 0.031(7) -0.027(7) 0.023(7) -0.084(10) C36 0.098(10) 0.086(10) 0.029(6) -0.025(6) 0.025(6) -0.065(8) C37 0.027(6) 0.181(15) 0.033(7) -0.032(8) -0.012(5) -0.027(7) C39 0.027(6) 0.130(12) 0.042(7) -0.024(7) 0.008(5) -0.013(6) C40 0.025(5) 0.023(5) 0.022(5) -0.009(4) 0.002(4) -0.001(4) C41 0.074(8) 0.069(9) 0.031(6) -0.023(6) -0.021(6) 0.046(7) C42 0.105(10) 0.063(9) 0.045(8) -0.025(7) -0.020(7) 0.067(8) C43 0.067(8) 0.057(8) 0.034(7) -0.024(6) -0.001(6) 0.014(6) C44 0.052(7) 0.047(7) 0.032(6) -0.020(5) -0.004(5) -0.001(5) C45 0.029(5) 0.039(6) 0.040(6) -0.022(5) 0.005(4) 0.001(4) C46 0.040(5) 0.020(5) 0.014(4) 0.000(4) 0.003(4) -0.005(4) C47 0.036(5) 0.027(5) 0.024(5) 0.000(4) 0.002(4) 0.000(4) C48 0.056(7) 0.029(6) 0.035(6) 0.000(5) 0.001(5) -0.002(5) C49 0.042(6) 0.035(6) 0.046(7) -0.009(5) -0.010(5) 0.003(5) C50 0.035(5) 0.039(6) 0.034(6) 0.002(5) -0.017(5) 0.000(5) C51 0.035(5) 0.022(5) 0.032(5) -0.001(4) -0.009(4) -0.008(4) C52 0.026(5) 0.025(5) 0.023(5) -0.001(4) 0.001(4) -0.002(4) C53 0.039(6) 0.029(6) 0.043(6) -0.005(5) 0.016(5) -0.007(5) C54 0.058(7) 0.032(6) 0.053(7) -0.010(5) 0.022(6) -0.015(5) C55 0.048(6) 0.024(6) 0.045(7) -0.005(5) 0.010(5) -0.009(5) C56 0.028(5) 0.042(6) 0.038(6) -0.002(5) 0.013(4) -0.013(5) C58 0.025(5) 0.028(5) 0.029(5) -0.002(4) -0.003(4) -0.007(4) C57 0.027(5) 0.032(6) 0.036(6) -0.010(5) 0.003(4) -0.004(4) C59 0.045(6) 0.030(6) 0.029(6) -0.007(4) 0.004(5) 0.005(5) C60 0.047(6) 0.031(6) 0.033(6) 0.006(5) -0.004(5) 0.002(5) C61 0.025(5) 0.049(7) 0.053(7) -0.009(6) -0.009(5) 0.005(5) C62 0.030(6) 0.087(10) 0.045(7) -0.022(7) 0.007(5) -0.003(6) C63 0.031(5) 0.062(7) 0.023(5) -0.005(5) 0.000(4) -0.003(5) C64 0.024(5) 0.023(5) 0.027(5) 0.000(4) 0.010(4) -0.001(4) C65 0.039(5) 0.020(5) 0.029(5) -0.003(4) 0.004(4) -0.007(4) C66 0.038(6) 0.029(6) 0.066(8) -0.007(6) 0.005(6) -0.009(5) C67 0.058(7) 0.028(6) 0.047(7) 0.011(5) 0.014(6) -0.004(5) C68 0.069(8) 0.041(7) 0.032(6) 0.004(5) 0.011(5) -0.018(6) C69 0.047(6) 0.036(6) 0.029(6) 0.002(5) -0.004(5) -0.008(5) C70 0.029(5) 0.035(6) 0.013(4) -0.004(4) 0.004(4) -0.007(4) C71 0.036(5) 0.024(5) 0.029(5) 0.003(4) -0.001(4) -0.011(4) C72 0.029(5) 0.030(5) 0.030(5) -0.003(4) 0.013(4) -0.005(4) C73 0.037(6) 0.040(6) 0.030(6) -0.005(5) 0.000(5) -0.009(5) C74 0.038(6) 0.037(6) 0.040(6) -0.003(5) -0.011(5) -0.004(5) C75 0.042(6) 0.015(5) 0.031(5) -0.005(4) -0.004(4) -0.004(4) C76 0.021(5) 0.119(11) 0.044(7) -0.042(7) 0.003(5) -0.016(6) C78 0.043(6) 0.109(11) 0.029(6) -0.020(7) 0.018(5) -0.019(7) _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 C37 2.104(9) . ? Pt1 C39 2.117(9) . ? Pt1 I1A 2.4915(17) . ? Pt1 I1 2.6283(11) . ? Pt1 Sb1 2.6457(7) . ? Pt1 Sb2 2.6656(7) . ? Pt2 C78 2.098(9) . ? Pt2 C76 2.102(9) . ? Pt2 I2A 2.5679(14) . ? Pt2 I2 2.6302(12) . ? Pt2 Sb4 2.6551(7) . ? Pt2 Sb3 2.6651(7) . ? Sb1 C7 2.131(8) . ? Sb1 C13 2.138(8) . ? Sb1 C1 2.139(9) . ? Sb2 C25 2.136(8) . ? Sb2 C19 2.145(8) . ? Sb2 C31 2.153(8) . ? Sb3 C40 2.137(8) . ? Sb3 C52 2.143(8) . ? Sb3 C46 2.143(9) . ? Sb4 C70 2.131(8) . ? Sb4 C58 2.132(9) . ? Sb4 C64 2.149(8) . ? C1 C2 1.379(12) . ? C1 C6 1.388(12) . ? C2 C3 1.383(13) . ? C2 H2 0.9500 . ? C3 C4 1.378(14) . ? C3 H3 0.9500 . ? C4 C5 1.388(15) . ? C4 H4 0.9500 . ? C5 C6 1.376(13) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C12 1.386(11) . ? C7 C8 1.401(12) . ? C8 C9 1.380(12) . ? C8 H8 0.9500 . ? C9 C10 1.371(13) . ? C9 H9 0.9500 . ? C10 C11 1.368(13) . ? C10 H10 0.9500 . ? C11 C12 1.390(12) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C14 1.361(12) . ? C13 C18 1.390(12) . ? C14 C15 1.385(14) . ? C14 H14 0.9500 . ? C15 C16 1.345(13) . ? C15 H15 0.9500 . ? C16 C17 1.375(14) . ? C16 H16 0.9500 . ? C17 C18 1.382(13) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 C24 1.373(11) . ? C19 C20 1.418(13) . ? C20 C21 1.362(12) . ? C20 H20 0.9500 . ? C21 C22 1.369(13) . ? C21 H21 0.9500 . ? C22 C23 1.376(13) . ? C22 H22 0.9500 . ? C23 C24 1.398(13) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C25 C26 1.377(12) . ? C25 C30 1.393(12) . ? C26 C27 1.392(14) . ? C26 H26 0.9500 . ? C27 C28 1.362(14) . ? C27 H27 0.9500 . ? C28 C29 1.384(14) . ? C28 H28 0.9500 . ? C29 C30 1.395(13) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? C31 C32 1.367(12) . ? C31 C36 1.370(13) . ? C32 C33 1.364(12) . ? C32 H32 0.9500 . ? C33 C34 1.387(13) . ? C33 H33 0.9500 . ? C34 C35 1.364(14) . ? C34 H34 0.9500 . ? C35 C36 1.405(14) . ? C35 H35 0.9500 . ? C36 H36 0.9500 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 C41 1.367(12) . ? C40 C45 1.376(12) . ? C41 C42 1.372(14) . ? C41 H41 0.9500 . ? C42 C43 1.366(15) . ? C42 H42 0.9500 . ? C43 C44 1.347(14) . ? C43 H43 0.9500 . ? C44 C45 1.378(12) . ? C44 H44 0.9500 . ? C45 H45 0.9500 . ? C46 C51 1.396(12) . ? C46 C47 1.399(12) . ? C47 C48 1.378(12) . ? C47 H47 0.9500 . ? C48 C49 1.393(13) . ? C48 H48 0.9500 . ? C49 C50 1.375(13) . ? C49 H49 0.9500 . ? C50 C51 1.391(12) . ? C50 H50 0.9500 . ? C51 H51 0.9500 . ? C52 C57 1.383(11) . ? C52 C53 1.412(12) . ? C53 C54 1.380(13) . ? C53 H53 0.9500 . ? C54 C55 1.361(13) . ? C54 H54 0.9500 . ? C55 C56 1.348(12) . ? C55 H55 0.9500 . ? C56 C57 1.399(12) . ? C56 H56 0.9500 . ? C58 C59 1.387(12) . ? C58 C63 1.396(12) . ? C57 H57 0.9500 . ? C59 C60 1.401(13) . ? C59 H59 0.9500 . ? C60 C61 1.387(13) . ? C60 H60 0.9500 . ? C61 C62 1.375(14) . ? C61 H61 0.9500 . ? C62 C63 1.377(13) . ? C62 H62 0.9500 . ? C63 H63 0.9500 . ? C64 C65 1.382(12) . ? C64 C69 1.388(12) . ? C65 C66 1.397(13) . ? C65 H65 0.9500 . ? C66 C67 1.379(14) . ? C66 H66 0.9500 . ? C67 C68 1.380(14) . ? C67 H67 0.9500 . ? C68 C69 1.386(13) . ? C68 H68 0.9500 . ? C69 H69 0.9500 . ? C70 C71 1.385(12) . ? C70 C75 1.397(12) . ? C71 C72 1.387(12) . ? C71 H71 0.9500 . ? C72 C73 1.373(12) . ? C72 H72 0.9500 . ? C73 C74 1.362(13) . ? C73 H73 0.9500 . ? C74 C75 1.390(12) . ? C74 H74 0.9500 . ? C75 H75 0.9500 . ? C76 H76A 0.9800 . ? C76 H76B 0.9800 . ? C76 H76C 0.9800 . ? C78 H78A 0.9800 . ? C78 H78B 0.9800 . ? C78 H78C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C37 Pt1 C39 86.0(4) . . ? C37 Pt1 I1A 85.3(4) . . ? C39 Pt1 I1A 86.5(4) . . ? C37 Pt1 I1 88.2(4) . . ? C39 Pt1 I1 86.4(4) . . ? I1A Pt1 I1 170.67(4) . . ? C37 Pt1 Sb1 172.0(3) . . ? C39 Pt1 Sb1 86.1(3) . . ? I1A Pt1 Sb1 95.76(4) . . ? I1 Pt1 Sb1 89.78(3) . . ? C37 Pt1 Sb2 91.2(3) . . ? C39 Pt1 Sb2 175.8(3) . . ? I1A Pt1 Sb2 90.11(4) . . ? I1 Pt1 Sb2 96.71(3) . . ? Sb1 Pt1 Sb2 96.74(2) . . ? C78 Pt2 C76 85.3(4) . . ? C78 Pt2 I2A 87.4(4) . . ? C76 Pt2 I2A 87.0(4) . . ? C78 Pt2 I2 86.8(4) . . ? C76 Pt2 I2 85.5(4) . . ? I2A Pt2 I2 170.81(4) . . ? C78 Pt2 Sb4 171.4(3) . . ? C76 Pt2 Sb4 86.7(3) . . ? I2A Pt2 Sb4 95.31(3) . . ? I2 Pt2 Sb4 89.46(3) . . ? C78 Pt2 Sb3 91.7(3) . . ? C76 Pt2 Sb3 174.3(3) . . ? I2A Pt2 Sb3 88.07(3) . . ? I2 Pt2 Sb3 99.21(3) . . ? Sb4 Pt2 Sb3 96.48(2) . . ? C7 Sb1 C13 98.5(3) . . ? C7 Sb1 C1 100.3(3) . . ? C13 Sb1 C1 101.0(3) . . ? C7 Sb1 Pt1 112.3(2) . . ? C13 Sb1 Pt1 119.9(2) . . ? C1 Sb1 Pt1 121.0(2) . . ? C25 Sb2 C19 99.1(3) . . ? C25 Sb2 C31 98.8(3) . . ? C19 Sb2 C31 97.9(3) . . ? C25 Sb2 Pt1 116.5(2) . . ? C19 Sb2 Pt1 125.3(2) . . ? C31 Sb2 Pt1 114.7(2) . . ? C40 Sb3 C52 98.1(3) . . ? C40 Sb3 C46 98.1(3) . . ? C52 Sb3 C46 99.6(3) . . ? C40 Sb3 Pt2 115.3(2) . . ? C52 Sb3 Pt2 117.1(2) . . ? C46 Sb3 Pt2 124.0(2) . . ? C70 Sb4 C58 98.8(3) . . ? C70 Sb4 C64 100.2(3) . . ? C58 Sb4 C64 101.3(3) . . ? C70 Sb4 Pt2 111.4(2) . . ? C58 Sb4 Pt2 120.7(2) . . ? C64 Sb4 Pt2 120.6(2) . . ? C2 C1 C6 117.9(9) . . ? C2 C1 Sb1 119.8(7) . . ? C6 C1 Sb1 122.3(7) . . ? C1 C2 C3 121.8(10) . . ? C1 C2 H2 119.1 . . ? C3 C2 H2 119.1 . . ? C4 C3 C2 118.9(11) . . ? C4 C3 H3 120.6 . . ? C2 C3 H3 120.6 . . ? C3 C4 C5 120.8(10) . . ? C3 C4 H4 119.6 . . ? C5 C4 H4 119.6 . . ? C6 C5 C4 118.8(10) . . ? C6 C5 H5 120.6 . . ? C4 C5 H5 120.6 . . ? C5 C6 C1 121.8(10) . . ? C5 C6 H6 119.1 . . ? C1 C6 H6 119.1 . . ? C12 C7 C8 118.8(8) . . ? C12 C7 Sb1 120.3(6) . . ? C8 C7 Sb1 120.7(6) . . ? C9 C8 C7 120.4(9) . . ? C9 C8 H8 119.8 . . ? C7 C8 H8 119.8 . . ? C10 C9 C8 119.3(9) . . ? C10 C9 H9 120.3 . . ? C8 C9 H9 120.3 . . ? C11 C10 C9 121.6(9) . . ? C11 C10 H10 119.2 . . ? C9 C10 H10 119.2 . . ? C10 C11 C12 119.3(9) . . ? C10 C11 H11 120.3 . . ? C12 C11 H11 120.3 . . ? C7 C12 C11 120.4(8) . . ? C7 C12 H12 119.8 . . ? C11 C12 H12 119.8 . . ? C14 C13 C18 120.2(9) . . ? C14 C13 Sb1 120.8(7) . . ? C18 C13 Sb1 119.0(6) . . ? C13 C14 C15 119.2(9) . . ? C13 C14 H14 120.4 . . ? C15 C14 H14 120.4 . . ? C16 C15 C14 121.8(10) . . ? C16 C15 H15 119.1 . . ? C14 C15 H15 119.1 . . ? C15 C16 C17 119.0(10) . . ? C15 C16 H16 120.5 . . ? C17 C16 H16 120.5 . . ? C16 C17 C18 121.0(10) . . ? C16 C17 H17 119.5 . . ? C18 C17 H17 119.5 . . ? C17 C18 C13 118.8(9) . . ? C17 C18 H18 120.6 . . ? C13 C18 H18 120.6 . . ? C24 C19 C20 119.2(8) . . ? C24 C19 Sb2 121.8(7) . . ? C20 C19 Sb2 119.0(6) . . ? C21 C20 C19 119.5(9) . . ? C21 C20 H20 120.2 . . ? C19 C20 H20 120.2 . . ? C20 C21 C22 121.2(10) . . ? C20 C21 H21 119.4 . . ? C22 C21 H21 119.4 . . ? C21 C22 C23 120.2(9) . . ? C21 C22 H22 119.9 . . ? C23 C22 H22 119.9 . . ? C22 C23 C24 119.8(9) . . ? C22 C23 H23 120.1 . . ? C24 C23 H23 120.1 . . ? C19 C24 C23 120.1(9) . . ? C19 C24 H24 120.0 . . ? C23 C24 H24 120.0 . . ? C26 C25 C30 119.4(8) . . ? C26 C25 Sb2 120.8(6) . . ? C30 C25 Sb2 119.8(7) . . ? C25 C26 C27 119.8(9) . . ? C25 C26 H26 120.1 . . ? C27 C26 H26 120.1 . . ? C28 C27 C26 121.1(10) . . ? C28 C27 H27 119.5 . . ? C26 C27 H27 119.5 . . ? C27 C28 C29 119.8(10) . . ? C27 C28 H28 120.1 . . ? C29 C28 H28 120.1 . . ? C28 C29 C30 119.7(9) . . ? C28 C29 H29 120.2 . . ? C30 C29 H29 120.2 . . ? C25 C30 C29 120.2(9) . . ? C25 C30 H30 119.9 . . ? C29 C30 H30 119.9 . . ? C32 C31 C36 119.5(9) . . ? C32 C31 Sb2 119.9(7) . . ? C36 C31 Sb2 120.6(7) . . ? C33 C32 C31 120.9(9) . . ? C33 C32 H32 119.5 . . ? C31 C32 H32 119.5 . . ? C32 C33 C34 119.7(9) . . ? C32 C33 H33 120.2 . . ? C34 C33 H33 120.2 . . ? C35 C34 C33 120.8(10) . . ? C35 C34 H34 119.6 . . ? C33 C34 H34 119.6 . . ? C34 C35 C36 118.4(10) . . ? C34 C35 H35 120.8 . . ? C36 C35 H35 120.8 . . ? C31 C36 C35 120.7(10) . . ? C31 C36 H36 119.7 . . ? C35 C36 H36 119.7 . . ? Pt1 C37 H37A 109.5 . . ? Pt1 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? Pt1 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? Pt1 C39 H39A 109.5 . . ? Pt1 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? Pt1 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C41 C40 C45 117.5(8) . . ? C41 C40 Sb3 122.6(7) . . ? C45 C40 Sb3 119.9(6) . . ? C40 C41 C42 120.5(10) . . ? C40 C41 H41 119.7 . . ? C42 C41 H41 119.7 . . ? C43 C42 C41 121.1(10) . . ? C43 C42 H42 119.4 . . ? C41 C42 H42 119.4 . . ? C44 C43 C42 119.2(10) . . ? C44 C43 H43 120.4 . . ? C42 C43 H43 120.4 . . ? C43 C44 C45 119.8(10) . . ? C43 C44 H44 120.1 . . ? C45 C44 H44 120.1 . . ? C40 C45 C44 121.8(9) . . ? C40 C45 H45 119.1 . . ? C44 C45 H45 119.1 . . ? C51 C46 C47 118.7(8) . . ? C51 C46 Sb3 122.0(6) . . ? C47 C46 Sb3 119.3(6) . . ? C48 C47 C46 120.5(9) . . ? C48 C47 H47 119.7 . . ? C46 C47 H47 119.7 . . ? C47 C48 C49 119.9(9) . . ? C47 C48 H48 120.0 . . ? C49 C48 H48 120.1 . . ? C50 C49 C48 120.5(9) . . ? C50 C49 H49 119.7 . . ? C48 C49 H49 119.7 . . ? C49 C50 C51 119.6(9) . . ? C49 C50 H50 120.2 . . ? C51 C50 H50 120.2 . . ? C50 C51 C46 120.7(8) . . ? C50 C51 H51 119.7 . . ? C46 C51 H51 119.7 . . ? C57 C52 C53 118.7(8) . . ? C57 C52 Sb3 121.1(7) . . ? C53 C52 Sb3 120.0(6) . . ? C54 C53 C52 118.8(9) . . ? C54 C53 H53 120.6 . . ? C52 C53 H53 120.6 . . ? C55 C54 C53 121.4(10) . . ? C55 C54 H54 119.3 . . ? C53 C54 H54 119.3 . . ? C56 C55 C54 120.7(9) . . ? C56 C55 H55 119.6 . . ? C54 C55 H55 119.6 . . ? C55 C56 C57 119.9(9) . . ? C55 C56 H56 120.0 . . ? C57 C56 H56 120.0 . . ? C59 C58 C63 118.3(8) . . ? C59 C58 Sb4 120.2(7) . . ? C63 C58 Sb4 121.5(7) . . ? C52 C57 C56 120.3(9) . . ? C52 C57 H57 119.8 . . ? C56 C57 H57 119.8 . . ? C58 C59 C60 121.3(9) . . ? C58 C59 H59 119.4 . . ? C60 C59 H59 119.4 . . ? C61 C60 C59 119.1(9) . . ? C61 C60 H60 120.5 . . ? C59 C60 H60 120.5 . . ? C62 C61 C60 119.6(9) . . ? C62 C61 H61 120.2 . . ? C60 C61 H61 120.2 . . ? C61 C62 C63 121.3(10) . . ? C61 C62 H62 119.4 . . ? C63 C62 H62 119.4 . . ? C62 C63 C58 120.3(9) . . ? C62 C63 H63 119.8 . . ? C58 C63 H63 119.8 . . ? C65 C64 C69 120.0(8) . . ? C65 C64 Sb4 118.9(7) . . ? C69 C64 Sb4 121.1(7) . . ? C64 C65 C66 119.1(9) . . ? C64 C65 H65 120.4 . . ? C66 C65 H65 120.4 . . ? C67 C66 C65 121.5(10) . . ? C67 C66 H66 119.3 . . ? C65 C66 H66 119.3 . . ? C66 C67 C68 118.4(9) . . ? C66 C67 H67 120.8 . . ? C68 C67 H67 120.8 . . ? C67 C68 C69 121.4(10) . . ? C67 C68 H68 119.3 . . ? C69 C68 H68 119.3 . . ? C68 C69 C64 119.5(9) . . ? C68 C69 H69 120.2 . . ? C64 C69 H69 120.2 . . ? C71 C70 C75 119.3(8) . . ? C71 C70 Sb4 121.4(6) . . ? C75 C70 Sb4 119.3(6) . . ? C70 C71 C72 120.0(9) . . ? C70 C71 H71 120.0 . . ? C72 C71 H71 120.0 . . ? C73 C72 C71 120.2(9) . . ? C73 C72 H72 119.9 . . ? C71 C72 H72 119.9 . . ? C74 C73 C72 120.5(9) . . ? C74 C73 H73 119.7 . . ? C72 C73 H73 119.7 . . ? C73 C74 C75 120.3(9) . . ? C73 C74 H74 119.9 . . ? C75 C74 H74 119.9 . . ? C74 C75 C70 119.7(8) . . ? C74 C75 H75 120.1 . . ? C70 C75 H75 120.1 . . ? Pt2 C76 H76A 109.5 . . ? Pt2 C76 H76B 109.5 . . ? H76A C76 H76B 109.5 . . ? Pt2 C76 H76C 109.5 . . ? H76A C76 H76C 109.5 . . ? H76B C76 H76C 109.5 . . ? Pt2 C78 H78A 109.5 . . ? Pt2 C78 H78B 109.5 . . ? H78A C78 H78B 109.5 . . ? Pt2 C78 H78C 109.5 . . ? H78A C78 H78C 109.5 . . ? H78B C78 H78C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 27.62 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 1.587 _refine_diff_density_min -2.743 _refine_diff_density_rms 0.220 #===END OF CIF =============================================================== data_05mdb015 _database_code_depnum_ccdc_archive 'CCDC 285692' _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2005-07-01 _chemical_name_systematic ; Bis(iodotrimethylplatinum(IV))-mu-bis(diphenylstibino)methane ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C31 H40 I2 Pt2 Sb2' _chemical_formula_sum 'C31 H40 I2 Pt2 Sb2' _chemical_formula_weight 1300.11 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' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_Int_Tables_number 2 # Superceded ** _symmetry_space_group_name_Hall '-P 1' # Superceded ** loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.7960(10) _cell_length_b 11.7470(10) _cell_length_c 15.3850(10) _cell_angle_alpha 103.790(6) _cell_angle_beta 93.514(5) _cell_angle_gamma 90.628(4) _cell_volume 1715.5(3) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 7625 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.517 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1180 _exptl_absorpt_coefficient_mu 11.504 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6357 # shelxl 0.1298 _exptl_absorpt_correction_T_max 1.0000 # 0.2069 _exptl_absorpt_process_details 'G.M. Sheldrick, (2003). SADABS. Version 2.10. Bruker AXS Inc.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Nonius rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'area detector, Nonius Kappa ccd' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 33362 _diffrn_reflns_av_R_equivalents 0.0299 _diffrn_reflns_av_sigmaI/netI 0.0291 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.33 _diffrn_reflns_theta_max 27.54 _reflns_number_total 7793 _reflns_number_gt 7221 _reflns_threshold_expression I>2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _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 'w=1/[\s^2^(Fo^2^)+(0.0585P)^2^+4.6468P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7793 _refine_ls_number_parameters 334 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0320 _refine_ls_R_factor_gt 0.0284 _refine_ls_wR_factor_ref 0.0879 _refine_ls_wR_factor_gt 0.0851 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.021 _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 Pt1 Pt 0.87988(2) 0.186168(17) 0.352035(12) 0.01589(7) Uani 1 1 d . . . Pt2 Pt 0.77925(2) 0.448778(18) 0.227834(13) 0.01716(7) Uani 1 1 d . . . I1 I 0.84129(4) 0.42803(3) 0.40311(2) 0.01915(9) Uani 1 1 d . . . I2 I 0.79429(3) 0.20380(3) 0.17931(2) 0.01927(9) Uani 1 1 d . . . Sb1 Sb 1.13686(3) 0.23161(3) 0.32325(2) 0.01439(8) Uani 1 1 d . . . Sb2 Sb 1.04642(3) 0.45075(3) 0.19976(2) 0.01536(8) Uani 1 1 d . . . C1 C 0.6797(6) 0.1468(5) 0.3714(4) 0.0267(12) Uani 1 1 d . . . H1A H 0.6230 0.1419 0.3158 0.040 Uiso 1 1 calc R . . H1B H 0.6459 0.2083 0.4195 0.040 Uiso 1 1 calc R . . H1C H 0.6753 0.0713 0.3880 0.040 Uiso 1 1 calc R . . C2 C 0.9277(6) 0.1813(5) 0.4832(4) 0.0253(12) Uani 1 1 d . . . H2A H 0.9259 0.2608 0.5216 0.038 Uiso 1 1 calc R . . H2B H 1.0193 0.1499 0.4884 0.038 Uiso 1 1 calc R . . H2C H 0.8607 0.1310 0.5019 0.038 Uiso 1 1 calc R . . C3 C 0.9016(7) 0.0066(5) 0.3161(4) 0.0271(12) Uani 1 1 d . . . H3A H 0.8840 -0.0217 0.2511 0.041 Uiso 1 1 calc R . . H3B H 0.8362 -0.0312 0.3468 0.041 Uiso 1 1 calc R . . H3C H 0.9950 -0.0125 0.3334 0.041 Uiso 1 1 calc R . . C4 C 1.2896(5) 0.2349(4) 0.4287(3) 0.0160(10) Uani 1 1 d . . . C5 C 1.3001(7) 0.1412(5) 0.4695(4) 0.0292(13) Uani 1 1 d . . . H5 H 1.2404 0.0747 0.4488 0.035 Uiso 1 1 calc R . . C6 C 1.3957(7) 0.1437(6) 0.5393(4) 0.0336(14) Uani 1 1 d . . . H6 H 1.4026 0.0786 0.5658 0.040 Uiso 1 1 calc R . . C7 C 1.4823(6) 0.2412(6) 0.5710(4) 0.0314(14) Uani 1 1 d . . . H7 H 1.5476 0.2437 0.6197 0.038 Uiso 1 1 calc R . . C8 C 1.4727(7) 0.3328(6) 0.5316(4) 0.0307(13) Uani 1 1 d . . . H8 H 1.5322 0.3992 0.5531 0.037 Uiso 1 1 calc R . . C9 C 1.3768(6) 0.3313(5) 0.4601(4) 0.0250(12) Uani 1 1 d . . . H9 H 1.3717 0.3961 0.4332 0.030 Uiso 1 1 calc R . . C10 C 1.2276(5) 0.1197(4) 0.2126(3) 0.0169(10) Uani 1 1 d . . . C11 C 1.3693(5) 0.1183(4) 0.2086(3) 0.0164(10) Uani 1 1 d . . . H11 H 1.4259 0.1657 0.2562 0.020 Uiso 1 1 calc R . . C12 C 1.4284(6) 0.0475(5) 0.1354(4) 0.0219(11) Uani 1 1 d . . . H12 H 1.5250 0.0459 0.1330 0.026 Uiso 1 1 calc R . . C13 C 1.3441(6) -0.0212(5) 0.0652(3) 0.0217(11) Uani 1 1 d . . . H13 H 1.3833 -0.0699 0.0150 0.026 Uiso 1 1 calc R . . C14 C 1.2041(6) -0.0180(5) 0.0691(4) 0.0214(11) Uani 1 1 d . . . H14 H 1.1471 -0.0642 0.0212 0.026 Uiso 1 1 calc R . . C15 C 1.1454(6) 0.0520(5) 0.1422(4) 0.0199(11) Uani 1 1 d . . . H15 H 1.0487 0.0535 0.1441 0.024 Uiso 1 1 calc R . . C16 C 1.1803(5) 0.3992(4) 0.2980(3) 0.0162(10) Uani 1 1 d . . . H16A H 1.2748 0.3994 0.2786 0.019 Uiso 1 1 calc R . . H16B H 1.1777 0.4593 0.3552 0.019 Uiso 1 1 calc R . . C17 C 1.1188(5) 0.3459(4) 0.0804(3) 0.0164(10) Uani 1 1 d . . . C18 C 1.2564(6) 0.3173(5) 0.0753(4) 0.0206(11) Uani 1 1 d . . . H18 H 1.3185 0.3450 0.1261 0.025 Uiso 1 1 calc R . . C19 C 1.3038(6) 0.2487(5) -0.0035(4) 0.0251(12) Uani 1 1 d . . . H19 H 1.3980 0.2307 -0.0064 0.030 Uiso 1 1 calc R . . C20 C 1.2132(7) 0.2067(5) -0.0779(4) 0.0271(12) Uani 1 1 d . . . H20 H 1.2454 0.1595 -0.1314 0.033 Uiso 1 1 calc R . . C21 C 1.0753(7) 0.2337(5) -0.0739(4) 0.0308(14) Uani 1 1 d . . . H21 H 1.0132 0.2045 -0.1244 0.037 Uiso 1 1 calc R . . C22 C 1.0295(6) 0.3030(5) 0.0038(4) 0.0231(11) Uani 1 1 d . . . H22 H 0.9356 0.3223 0.0058 0.028 Uiso 1 1 calc R . . C23 C 1.1574(5) 0.6115(4) 0.2081(3) 0.0173(10) Uani 1 1 d . . . C24 C 1.2534(6) 0.6220(5) 0.1478(4) 0.0254(12) Uani 1 1 d . . . H24 H 1.2683 0.5579 0.0987 0.031 Uiso 1 1 calc R . . C25 C 1.3281(7) 0.7268(5) 0.1594(4) 0.0332(14) Uani 1 1 d . . . H25 H 1.3932 0.7342 0.1177 0.040 Uiso 1 1 calc R . . C26 C 1.3079(7) 0.8210(5) 0.2319(4) 0.0294(13) Uani 1 1 d . . . H26 H 1.3598 0.8921 0.2403 0.035 Uiso 1 1 calc R . . C27 C 1.2111(6) 0.8092(5) 0.2910(4) 0.0266(13) Uani 1 1 d . . . H27 H 1.1961 0.8732 0.3401 0.032 Uiso 1 1 calc R . . C28 C 1.1354(6) 0.7054(5) 0.2800(4) 0.0244(12) Uani 1 1 d . . . H28 H 1.0693 0.6985 0.3212 0.029 Uiso 1 1 calc R . . C29 C 0.7204(6) 0.4650(6) 0.0995(4) 0.0286(13) Uani 1 1 d . . . H29A H 0.7150 0.3872 0.0581 0.043 Uiso 1 1 calc R . . H29B H 0.7878 0.5144 0.0801 0.043 Uiso 1 1 calc R . . H29C H 0.6306 0.5010 0.0997 0.043 Uiso 1 1 calc R . . C30 C 0.7660(6) 0.6294(5) 0.2643(4) 0.0258(12) Uani 1 1 d . . . H30A H 0.8560 0.6655 0.2619 0.039 Uiso 1 1 calc R . . H30B H 0.7359 0.6535 0.3254 0.039 Uiso 1 1 calc R . . H30C H 0.6999 0.6549 0.2228 0.039 Uiso 1 1 calc R . . C31 C 0.5726(6) 0.4382(6) 0.2469(4) 0.0295(13) Uani 1 1 d . . . H31A H 0.5427 0.3556 0.2339 0.044 Uiso 1 1 calc R . . H31B H 0.5209 0.4776 0.2065 0.044 Uiso 1 1 calc R . . H31C H 0.5563 0.4762 0.3092 0.044 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.01363(11) 0.01985(11) 0.01363(11) 0.00248(8) 0.00261(8) 0.00039(8) Pt2 0.01221(11) 0.02398(12) 0.01510(11) 0.00453(8) -0.00015(8) 0.00161(8) I1 0.02051(18) 0.02151(17) 0.01362(16) 0.00037(13) 0.00169(13) 0.00331(13) I2 0.01638(17) 0.02441(18) 0.01427(16) -0.00019(13) -0.00086(12) -0.00326(13) Sb1 0.01252(17) 0.01703(16) 0.01223(16) 0.00101(12) 0.00001(12) -0.00041(12) Sb2 0.01238(17) 0.02028(17) 0.01317(16) 0.00373(12) -0.00001(12) 0.00027(13) C1 0.022(3) 0.030(3) 0.030(3) 0.009(2) 0.006(2) 0.001(2) C2 0.030(3) 0.033(3) 0.016(3) 0.012(2) 0.003(2) -0.001(2) C3 0.029(3) 0.021(3) 0.030(3) 0.005(2) 0.007(2) 0.003(2) C4 0.017(3) 0.017(2) 0.014(2) 0.0024(18) 0.0020(19) 0.0042(19) C5 0.031(3) 0.025(3) 0.033(3) 0.012(2) -0.007(3) -0.008(2) C6 0.040(4) 0.038(3) 0.026(3) 0.017(3) -0.002(3) 0.008(3) C7 0.024(3) 0.054(4) 0.016(3) 0.009(3) -0.004(2) 0.010(3) C8 0.030(3) 0.031(3) 0.025(3) -0.002(2) -0.012(2) -0.003(3) C9 0.022(3) 0.027(3) 0.025(3) 0.006(2) -0.006(2) 0.003(2) C10 0.019(3) 0.017(2) 0.014(2) 0.0013(18) 0.0005(19) 0.0003(19) C11 0.014(2) 0.019(2) 0.017(2) 0.0056(19) 0.0020(19) -0.0037(19) C12 0.016(3) 0.025(3) 0.026(3) 0.006(2) 0.002(2) -0.002(2) C13 0.029(3) 0.023(3) 0.016(2) 0.006(2) 0.011(2) 0.000(2) C14 0.021(3) 0.021(3) 0.019(3) -0.002(2) -0.003(2) -0.002(2) C15 0.018(3) 0.021(3) 0.021(3) 0.003(2) 0.003(2) 0.001(2) C16 0.013(2) 0.012(2) 0.024(3) 0.0069(19) 0.002(2) -0.0031(18) C17 0.017(3) 0.021(2) 0.012(2) 0.0038(18) 0.0032(19) -0.004(2) C18 0.019(3) 0.027(3) 0.018(3) 0.008(2) 0.003(2) 0.000(2) C19 0.021(3) 0.032(3) 0.025(3) 0.012(2) 0.006(2) 0.004(2) C20 0.035(3) 0.025(3) 0.022(3) 0.004(2) 0.007(2) 0.002(2) C21 0.044(4) 0.024(3) 0.021(3) 0.001(2) -0.004(3) 0.001(3) C22 0.024(3) 0.026(3) 0.021(3) 0.009(2) -0.003(2) 0.001(2) C23 0.020(3) 0.017(2) 0.015(2) 0.0069(19) -0.0042(19) 0.000(2) C24 0.034(3) 0.021(3) 0.022(3) 0.005(2) 0.004(2) -0.001(2) C25 0.046(4) 0.028(3) 0.030(3) 0.015(3) 0.007(3) -0.008(3) C26 0.041(4) 0.021(3) 0.029(3) 0.014(2) -0.003(3) -0.003(2) C27 0.035(3) 0.019(3) 0.022(3) -0.001(2) -0.010(2) 0.003(2) C28 0.024(3) 0.026(3) 0.022(3) 0.006(2) -0.002(2) 0.005(2) C29 0.026(3) 0.040(3) 0.020(3) 0.010(2) -0.005(2) 0.001(3) C30 0.020(3) 0.025(3) 0.031(3) 0.006(2) 0.003(2) 0.006(2) C31 0.011(3) 0.039(3) 0.038(3) 0.009(3) 0.001(2) -0.002(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 C2 2.057(5) . ? Pt1 C1 2.065(6) . ? Pt1 C3 2.066(6) . ? Pt1 Sb1 2.6530(5) . ? Pt1 I2 2.7929(4) . ? Pt1 I1 2.7979(5) . ? Pt2 C30 2.070(6) . ? Pt2 C31 2.070(6) . ? Pt2 C29 2.076(6) . ? Pt2 Sb2 2.6793(5) . ? Pt2 I1 2.7957(4) . ? Pt2 I2 2.8034(5) . ? Sb1 C4 2.132(5) . ? Sb1 C10 2.136(5) . ? Sb1 C16 2.139(5) . ? Sb2 C17 2.120(5) . ? Sb2 C16 2.140(5) . ? Sb2 C23 2.142(5) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 C9 1.383(8) . ? C4 C5 1.392(8) . ? C5 C6 1.376(8) . ? C5 H5 0.9500 . ? C6 C7 1.390(10) . ? C6 H6 0.9500 . ? C7 C8 1.355(9) . ? C7 H7 0.9500 . ? C8 C9 1.399(8) . ? C8 H8 0.9500 . ? C9 H9 0.9500 . ? C10 C15 1.387(7) . ? C10 C11 1.393(7) . ? C11 C12 1.393(7) . ? C11 H11 0.9500 . ? C12 C13 1.400(8) . ? C12 H12 0.9500 . ? C13 C14 1.377(8) . ? C13 H13 0.9500 . ? C14 C15 1.385(7) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.395(8) . ? C17 C22 1.409(7) . ? C18 C19 1.396(8) . ? C18 H18 0.9500 . ? C19 C20 1.392(8) . ? C19 H19 0.9500 . ? C20 C21 1.392(9) . ? C20 H20 0.9500 . ? C21 C22 1.380(8) . ? C21 H21 0.9500 . ? C22 H22 0.9500 . ? C23 C24 1.385(8) . ? C23 C28 1.392(8) . ? C24 C25 1.394(8) . ? C24 H24 0.9500 . ? C25 C26 1.397(9) . ? C25 H25 0.9500 . ? C26 C27 1.382(9) . ? C26 H26 0.9500 . ? C27 C28 1.391(8) . ? C27 H27 0.9500 . ? C28 H28 0.9500 . ? 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 . ? 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 Pt1 C1 87.7(2) . . ? C2 Pt1 C3 88.5(2) . . ? C1 Pt1 C3 85.0(2) . . ? C2 Pt1 Sb1 93.22(17) . . ? C1 Pt1 Sb1 178.38(17) . . ? C3 Pt1 Sb1 93.66(18) . . ? C2 Pt1 I2 174.89(18) . . ? C1 Pt1 I2 88.56(17) . . ? C3 Pt1 I2 94.67(17) . . ? Sb1 Pt1 I2 90.593(12) . . ? C2 Pt1 I1 90.99(17) . . ? C1 Pt1 I1 92.92(17) . . ? C3 Pt1 I1 177.92(18) . . ? Sb1 Pt1 I1 88.383(12) . . ? I2 Pt1 I1 85.713(12) . . ? C30 Pt2 C31 88.0(2) . . ? C30 Pt2 C29 85.1(3) . . ? C31 Pt2 C29 86.5(3) . . ? C30 Pt2 Sb2 94.88(17) . . ? C31 Pt2 Sb2 177.09(18) . . ? C29 Pt2 Sb2 93.34(18) . . ? C30 Pt2 I1 94.26(17) . . ? C31 Pt2 I1 89.94(18) . . ? C29 Pt2 I1 176.42(18) . . ? Sb2 Pt2 I1 90.224(12) . . ? C30 Pt2 I2 179.34(17) . . ? C31 Pt2 I2 91.36(18) . . ? C29 Pt2 I2 95.00(18) . . ? Sb2 Pt2 I2 85.759(12) . . ? I1 Pt2 I2 85.556(12) . . ? Pt2 I1 Pt1 94.184(12) . . ? Pt1 I2 Pt2 94.123(12) . . ? C4 Sb1 C10 101.04(19) . . ? C4 Sb1 C16 99.01(19) . . ? C10 Sb1 C16 100.3(2) . . ? C4 Sb1 Pt1 117.90(14) . . ? C10 Sb1 Pt1 118.30(14) . . ? C16 Sb1 Pt1 116.88(14) . . ? C17 Sb2 C16 100.4(2) . . ? C17 Sb2 C23 100.29(19) . . ? C16 Sb2 C23 93.96(18) . . ? C17 Sb2 Pt2 120.13(14) . . ? C16 Sb2 Pt2 115.89(14) . . ? C23 Sb2 Pt2 121.29(14) . . ? Pt1 C1 H1A 109.5 . . ? Pt1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? Pt1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? Pt1 C2 H2A 109.5 . . ? Pt1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? Pt1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? Pt1 C3 H3A 109.5 . . ? Pt1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? Pt1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C9 C4 C5 118.7(5) . . ? C9 C4 Sb1 120.9(4) . . ? C5 C4 Sb1 120.3(4) . . ? C6 C5 C4 120.9(6) . . ? C6 C5 H5 119.5 . . ? C4 C5 H5 119.5 . . ? C5 C6 C7 120.1(6) . . ? C5 C6 H6 120.0 . . ? C7 C6 H6 120.0 . . ? C8 C7 C6 119.3(5) . . ? C8 C7 H7 120.3 . . ? C6 C7 H7 120.3 . . ? C7 C8 C9 121.3(6) . . ? C7 C8 H8 119.3 . . ? C9 C8 H8 119.3 . . ? C4 C9 C8 119.7(5) . . ? C4 C9 H9 120.2 . . ? C8 C9 H9 120.2 . . ? C15 C10 C11 119.6(5) . . ? C15 C10 Sb1 120.1(4) . . ? C11 C10 Sb1 120.3(4) . . ? C12 C11 C10 120.3(5) . . ? C12 C11 H11 119.8 . . ? C10 C11 H11 119.8 . . ? C11 C12 C13 119.4(5) . . ? C11 C12 H12 120.3 . . ? C13 C12 H12 120.3 . . ? C14 C13 C12 119.8(5) . . ? C14 C13 H13 120.1 . . ? C12 C13 H13 120.1 . . ? C13 C14 C15 120.7(5) . . ? C13 C14 H14 119.6 . . ? C15 C14 H14 119.6 . . ? C14 C15 C10 120.1(5) . . ? C14 C15 H15 119.9 . . ? C10 C15 H15 119.9 . . ? Sb1 C16 Sb2 116.2(2) . . ? Sb1 C16 H16A 108.2 . . ? Sb2 C16 H16A 108.2 . . ? Sb1 C16 H16B 108.2 . . ? Sb2 C16 H16B 108.2 . . ? H16A C16 H16B 107.4 . . ? C18 C17 C22 118.1(5) . . ? C18 C17 Sb2 120.9(4) . . ? C22 C17 Sb2 121.1(4) . . ? C19 C18 C17 120.7(5) . . ? C19 C18 H18 119.6 . . ? C17 C18 H18 119.6 . . ? C20 C19 C18 120.0(5) . . ? C20 C19 H19 120.0 . . ? C18 C19 H19 120.0 . . ? C21 C20 C19 120.1(5) . . ? C21 C20 H20 120.0 . . ? C19 C20 H20 120.0 . . ? C22 C21 C20 119.6(6) . . ? C22 C21 H21 120.2 . . ? C20 C21 H21 120.2 . . ? C21 C22 C17 121.5(6) . . ? C21 C22 H22 119.2 . . ? C17 C22 H22 119.2 . . ? C24 C23 C28 120.1(5) . . ? C24 C23 Sb2 122.2(4) . . ? C28 C23 Sb2 117.5(4) . . ? C23 C24 C25 119.8(5) . . ? C23 C24 H24 120.1 . . ? C25 C24 H24 120.1 . . ? C24 C25 C26 120.6(6) . . ? C24 C25 H25 119.7 . . ? C26 C25 H25 119.7 . . ? C27 C26 C25 118.9(5) . . ? C27 C26 H26 120.6 . . ? C25 C26 H26 120.6 . . ? C26 C27 C28 121.2(5) . . ? C26 C27 H27 119.4 . . ? C28 C27 H27 119.4 . . ? C27 C28 C23 119.5(5) . . ? C27 C28 H28 120.3 . . ? C23 C28 H28 120.3 . . ? Pt2 C29 H29A 109.5 . . ? Pt2 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? Pt2 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? Pt2 C30 H30A 109.5 . . ? Pt2 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? Pt2 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? Pt2 C31 H31A 109.5 . . ? Pt2 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? Pt2 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 27.54 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 1.161 _refine_diff_density_min -2.134 _refine_diff_density_rms 0.262 #===END OF FILE ==============================================================