Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0222 _publ_contact_author_name 'Wolfgang Weigand' _publ_contact_author_address ; Friedrich-Schiller-Universitat Jena Jena 07743 GERMANY ; _publ_contact_author_email C8WEWO@UNI-JENA.DE _publ_section_title ; Selective carbon-carbon bond cleavage of 2,2'-dibromotolane via photolysis of its appropriate (bisphosphine)Pt0 complex in solid state ; loop_ _publ_author_name 'Wolfgang Weigand' 'Hergen Breitzke' 'Gerd Buntkowsky' 'Daniel Escudero' 'Leticia Gonzalez' ; H.Gorls ; 'Holm Petzold' 'Thomas Weisheit' data_FO2829?(Compound3)? _database_code_depnum_ccdc_archive 'CCDC 660013' _audit_creation_method SHELXL-97? _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44 H32 Br2 P2 Pt' _chemical_formula_weight 977.55 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' ?'-x+1/2, y+1/2, -z+1/2'? ?'-x, -y, -z'? ?'x-1/2, -y-1/2, z-1/2'? _cell_length_a 11.1456(4) _cell_length_b 22.1637(7) _cell_length_c 15.3986(4) _cell_angle_alpha 90.00 _cell_angle_beta 106.710(2) _cell_angle_gamma 90.00 _cell_volume 3643.3(2) _cell_formula_units_Z 4 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.04 _exptl_crystal_size_mid 0.04? _exptl_crystal_size_min 0.03? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.782 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1896 _exptl_absorpt_coefficient_mu 6.164 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. R.H. Blessing, Acta Cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.2908 _exptl_absorpt_correction_T_max 0.6101 _exptl_special_details ; ? ; _diffrn_ambient_temperature 183(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'phi- + omega-scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23208 _diffrn_reflns_av_R_equivalents 0.0899 _diffrn_reflns_av_sigmaI/netI 0.0755 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.30 _diffrn_reflns_theta_max 27.47 _reflns_number_total 8185 _reflns_number_gt 6160 _reflns_threshold_expression >2sigma(I) _computing_data_collection COLLECT _computing_cell_refinement DENZO _computing_data_reduction DENZO _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL/PC _computing_publication_material SHELXL-97 _refine_special_details ; ?Refinement of F^2^ against ALL reflections.? The weighted R-factor wR and? ?goodness of fit S are based on F^2^, conventional R-factors R are based? ?on F, with F set to zero for negative F^2^. The threshold expression of? ?F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is? ?not relevant to the choice of reflections for refinement.? R-factors based? ?on F^2^ are statistically about twice as large as those based on F, and R- ? ?factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0731P)^2^+15.3334P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8185 _refine_ls_number_parameters 442 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0800 _refine_ls_R_factor_gt 0.0544 _refine_ls_wR_factor_ref 0.1463 _refine_ls_wR_factor_gt 0.1328 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.024 _refine_ls_shift/su_max 0.047 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt Pt 0.01887(3) 0.064956(12) 0.730885(17) 0.02476(11) Uani 1 1 d . . .? Br1 Br 0.47663(8) 0.08648(5) 0.86883(7) 0.0484(2) Uani 1 1 d . . .? Br2 Br 0.30680(12) -0.06205(5) 0.88516(7) 0.0583(3) Uani 1 1 d . . .? P1 P -0.11719(17) 0.13972(8) 0.73101(12) 0.0229(4) Uani 1 1 d . . .? P2 P -0.14619(18) 0.00293(8) 0.72203(12) 0.0257(4) Uani 1 1 d . . .? C1 C 0.1921(7) 0.0334(4) 0.7277(5) 0.0334(17) Uani 1 1 d . . .? C2 C 0.1958(7) 0.0919(3) 0.7377(5) 0.0302(16) Uani 1 1 d . . .? C3 C 0.2704(7) 0.1463(3) 0.7445(5) 0.0283(15) Uani 1 1 d . . .? C4 C 0.2155(8) 0.1982(3) 0.6979(5) 0.0353(17) Uani 1 1 d . . .? H4A H 0.1315 0.1964 0.6602 0.042 Uiso 1 1 calc R . .? C5 C 0.2806(8) 0.2522(4) 0.7054(5) 0.0363(18) Uani 1 1 d . . .? H5A H 0.2407 0.2865 0.6727 0.044 Uiso 1 1 calc R . .? C6 C 0.4041(9) 0.2567(4) 0.7603(6) 0.043(2) Uani 1 1 d . . .? H6A H 0.4496 0.2933 0.7644 0.052 Uiso 1 1 calc R . .? C7 C 0.4581(8) 0.2059(4) 0.8086(5) 0.0371(18) Uani 1 1 d . . .? H7A H 0.5408 0.2082 0.8483 0.045 Uiso 1 1 calc R . .? C8 C 0.3934(7) 0.1525(4) 0.7997(5) 0.0344(17) Uani 1 1 d . . .? C9 C 0.2510(8) -0.0202(4) 0.7032(6) 0.0366(18) Uani 1 1 d . . .? C10 C 0.2430(12) -0.0277(4) 0.6067(9) 0.073(4) Uani 1 1 d . . .? H10A H 0.1954 -0.0010 0.5615 0.088 Uiso 1 1 calc R . .? C11 C 0.3096(12) -0.0766(5) 0.5852(8) 0.061(3) Uani 1 1 d . . .? H11A H 0.3139 -0.0803 0.5247 0.073 Uiso 1 1 calc R . .? C12 C 0.3686(11) -0.1190(5) 0.6472(7) 0.059(3) Uani 1 1 d . . .? H12A H 0.4095 -0.1522 0.6288 0.071 Uiso 1 1 calc R . .? C13 C 0.3686(10) -0.1136(4) 0.7359(8) 0.056(3) Uani 1 1 d . . .? H13A H 0.4096 -0.1432 0.7789 0.067 Uiso 1 1 calc R . .? C14 C 0.3105(9) -0.0664(4) 0.7630(7) 0.044(2) Uani 1 1 d . . .? C15 C -0.2771(7) 0.1102(3) 0.6851(4) 0.0245(14) Uani 1 1 d . . .? C16 C -0.3799(7) 0.1471(3) 0.6556(5) 0.0297(16) Uani 1 1 d . . .? H16A H -0.3711 0.1893 0.6656 0.036 Uiso 1 1 calc R . .? C17 C -0.4971(7) 0.1229(4) 0.6111(5) 0.0335(17) Uani 1 1 d . . .? H17A H -0.5682 0.1485 0.5910 0.040 Uiso 1 1 calc R . .? C18 C -0.5087(8) 0.0609(4) 0.5964(6) 0.041(2) Uani 1 1 d . . .? H18A H -0.5875 0.0441 0.5647 0.050 Uiso 1 1 calc R . .? C19 C -0.4057(7) 0.0239(4) 0.6278(5) 0.0326(17) Uani 1 1 d . . .? H19A H -0.4149 -0.0183 0.6179 0.039 Uiso 1 1 calc R . .? C20 C -0.2900(6) 0.0469(3) 0.6733(4) 0.0246(14) Uani 1 1 d . . .? C21 C -0.1065(7) 0.1720(3) 0.8413(5) 0.0264(15) Uani 1 1 d . . .? C22 C 0.0017(7) 0.2046(3) 0.8858(5) 0.0302(16) Uani 1 1 d . . .? H22A H 0.0641 0.2121 0.8561 0.036 Uiso 1 1 calc R . .? C23 C 0.0176(8) 0.2259(4) 0.9731(5) 0.0350(17) Uani 1 1 d . . .? H23A H 0.0899 0.2488 1.0025 0.042 Uiso 1 1 calc R . .? C24 C -0.0714(8) 0.2137(4) 1.0173(5) 0.0372(19) Uani 1 1 d . . .? H24A H -0.0598 0.2280 1.0773 0.045 Uiso 1 1 calc R . .? C25 C -0.1771(9) 0.1811(4) 0.9744(5) 0.0371(19) Uani 1 1 d . . .? H25A H -0.2375 0.1726 1.0055 0.045 Uiso 1 1 calc R . .? C26 C -0.1961(7) 0.1607(3) 0.8866(5) 0.0279(15) Uani 1 1 d . . .? H26A H -0.2701 0.1390 0.8572 0.033 Uiso 1 1 calc R . .? C27 C -0.1237(7) 0.2040(3) 0.6563(5) 0.0278(15) Uani 1 1 d . . .? C28 C -0.1402(9) 0.2637(4) 0.6795(6) 0.044(2) Uani 1 1 d . . .? H28A H -0.1442 0.2729 0.7388 0.053 Uiso 1 1 calc R . .? C29 C -0.1508(11) 0.3096(4) 0.6172(7) 0.055(3) Uani 1 1 d . . .? H29A H -0.1641 0.3499 0.6333 0.067 Uiso 1 1 calc R . .? C30 C -0.1420(10) 0.2968(4) 0.5310(6) 0.052(2) Uani 1 1 d . . .? H30A H -0.1453 0.3285 0.4890 0.062 Uiso 1 1 calc R . .? C31 C -0.1288(9) 0.2389(5) 0.5069(6) 0.051(2) Uani 1 1 d . . .? H31A H -0.1260 0.2302 0.4471 0.061 Uiso 1 1 calc R . .? C32 C -0.1193(8) 0.1920(4) 0.5688(5) 0.0372(18) Uani 1 1 d . . .? H32A H -0.1097 0.1516 0.5511 0.045 Uiso 1 1 calc R . .? C33 C -0.1660(8) -0.0656(3) 0.6527(5) 0.0300(16) Uani 1 1 d . . .? C34 C -0.2339(10) -0.1145(4) 0.6646(6) 0.047(2) Uani 1 1 d . . .? H34A H -0.2758 -0.1135 0.7103 0.056 Uiso 1 1 calc R . .? C35 C -0.2431(11) -0.1657(4) 0.6113(6) 0.052(3) Uani 1 1 d . . .? H35A H -0.2898 -0.1996 0.6208 0.063 Uiso 1 1 calc R . .? C36 C -0.1844(9) -0.1665(4) 0.5451(6) 0.045(2) Uani 1 1 d . . .? H36A H -0.1916 -0.2012 0.5078 0.054 Uiso 1 1 calc R . .? C37 C -0.1147(10) -0.1182(4) 0.5312(6) 0.052(2) Uani 1 1 d . . .? H37A H -0.0754 -0.1194 0.4840 0.062 Uiso 1 1 calc R . .? C38 C -0.1022(9) -0.0677(4) 0.5863(6) 0.041(2) Uani 1 1 d . . .? H38A H -0.0510 -0.0349 0.5792 0.050 Uiso 1 1 calc R . .? C39 C -0.1672(7) -0.0229(3) 0.8290(5) 0.0267(15) Uani 1 1 d . . .? C40 C -0.2795(8) -0.0169(3) 0.8510(5) 0.0306(16) Uani 1 1 d . . .? H40A H -0.3510 -0.0005 0.8081 0.037 Uiso 1 1 calc R . .? C41 C -0.2866(9) -0.0350(4) 0.9357(5) 0.0384(19) Uani 1 1 d . . .? H41A H -0.3629 -0.0299 0.9507 0.046 Uiso 1 1 calc R . .? C42 C -0.1848(10) -0.0603(3) 0.9983(5) 0.040(2) Uani 1 1 d . . .? H42A H -0.1904 -0.0726 1.0562 0.048 Uiso 1 1 calc R . .? C43 C -0.0741(9) -0.0674(4) 0.9752(6) 0.044(2) Uani 1 1 d . . .? H43A H -0.0036 -0.0850 1.0177 0.053 Uiso 1 1 calc R . .? C44 C -0.0647(8) -0.0494(4) 0.8922(5) 0.0370(18) Uani 1 1 d . . .? H44A H 0.0118 -0.0551 0.8775 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 Pt 0.02381(16) 0.02617(16) 0.02433(16) -0.00160(11) 0.00697(11) 0.00210(11) Br1 0.0332(5) 0.0526(5) 0.0544(5) 0.0071(4) 0.0048(4) 0.0062(4) Br2 0.0785(8) 0.0545(6) 0.0441(5) 0.0116(4) 0.0211(5) 0.0045(5) P1 0.0249(9) 0.0209(9) 0.0233(8) 0.0003(7) 0.0075(7) 0.0000(7) P2 0.0277(10) 0.0240(9) 0.0256(9) -0.0013(7) 0.0082(8) 0.0015(7) C1 0.028(4) 0.034(4) 0.040(4) 0.005(3) 0.012(3) 0.007(3) C2 0.028(4) 0.027(4) 0.032(4) 0.003(3) 0.005(3) -0.007(3) C3 0.030(4) 0.031(4) 0.023(3) 0.001(3) 0.007(3) 0.000(3) C4 0.043(5) 0.032(4) 0.034(4) 0.000(3) 0.016(4) 0.002(4) C5 0.041(5) 0.026(4) 0.043(5) 0.006(3) 0.014(4) 0.004(3) C6 0.062(6) 0.030(4) 0.049(5) -0.009(4) 0.033(5) -0.014(4) C7 0.042(5) 0.039(5) 0.032(4) -0.003(3) 0.012(4) 0.003(4) C8 0.032(4) 0.034(4) 0.039(4) -0.001(3) 0.013(3) 0.007(3) C9 0.037(5) 0.032(4) 0.040(4) -0.001(3) 0.011(4) 0.003(3) C10 0.105(9) 0.032(5) 0.120(10) -0.020(5) 0.092(9) -0.017(5) C11 0.080(8) 0.053(6) 0.060(6) -0.012(5) 0.035(6) -0.005(5) C12 0.079(8) 0.040(5) 0.070(7) -0.001(5) 0.042(6) 0.003(5) C13 0.067(7) 0.031(5) 0.078(7) 0.005(5) 0.035(6) 0.004(5) C14 0.047(5) 0.035(5) 0.054(5) 0.008(4) 0.021(4) -0.001(4) C15 0.032(4) 0.025(3) 0.019(3) 0.000(3) 0.011(3) -0.001(3) C16 0.032(4) 0.029(4) 0.028(4) 0.000(3) 0.008(3) 0.003(3) C17 0.028(4) 0.035(4) 0.034(4) 0.008(3) 0.003(3) 0.006(3) C18 0.032(4) 0.044(5) 0.044(5) 0.002(4) 0.005(4) -0.004(4) C19 0.032(4) 0.030(4) 0.035(4) -0.004(3) 0.008(3) -0.008(3) C20 0.020(3) 0.032(4) 0.020(3) 0.001(3) 0.003(3) 0.002(3) C21 0.033(4) 0.022(4) 0.024(3) 0.003(3) 0.008(3) 0.004(3) C22 0.030(4) 0.033(4) 0.028(4) 0.001(3) 0.009(3) -0.002(3) C23 0.035(4) 0.034(4) 0.031(4) -0.003(3) 0.001(3) 0.000(3) C24 0.057(6) 0.031(4) 0.023(4) -0.001(3) 0.010(4) -0.003(4) C25 0.051(5) 0.036(4) 0.029(4) 0.003(3) 0.019(4) 0.006(4) C26 0.028(4) 0.028(4) 0.028(4) 0.002(3) 0.009(3) 0.003(3) C27 0.026(4) 0.030(4) 0.027(4) 0.001(3) 0.006(3) -0.005(3) C28 0.073(7) 0.024(4) 0.033(4) -0.001(3) 0.010(4) -0.003(4) C29 0.091(8) 0.025(4) 0.051(5) 0.006(4) 0.021(5) -0.002(5)? C30 0.058(6) 0.047(6) 0.050(5) 0.019(4) 0.015(5) -0.006(5)? C31 0.057(6) 0.069(7) 0.035(5) 0.015(4) 0.028(4) 0.003(5)? C32 0.050(5) 0.036(4) 0.033(4) -0.001(3) 0.022(4) -0.003(4) C33 0.037(4) 0.025(4) 0.029(4) -0.007(3) 0.011(3) 0.002(3) C34 0.067(6) 0.036(5) 0.046(5) -0.010(4) 0.030(5) -0.014(4) C35 0.087(8) 0.034(5) 0.043(5) -0.013(4) 0.029(5) -0.018(5) C36 0.056(6) 0.032(5) 0.046(5) -0.012(4) 0.014(4) 0.005(4) C37 0.075(7) 0.040(5) 0.049(5) -0.018(4) 0.031(5) -0.004(5) C38 0.054(6) 0.030(4) 0.045(5) -0.008(3) 0.022(4) -0.001(4) C39 0.040(4) 0.017(3) 0.023(3) 0.000(3) 0.008(3) 0.006(3) C40 0.034(4) 0.026(4) 0.033(4) 0.004(3) 0.012(3) 0.008(3) C41 0.045(5) 0.040(5) 0.033(4) -0.001(3) 0.016(4) 0.000(4) C42 0.068(6) 0.026(4) 0.026(4) 0.000(3) 0.010(4) -0.004(4) C43 0.050(6) 0.041(5) 0.032(4) 0.006(3) -0.006(4) 0.004(4) C44 0.041(5) 0.035(4) 0.034(4) -0.001(3) 0.008(4) 0.004(4) _geom_special_details ; ?All esds (except the esd in the dihedral angle between two l.s. planes)? ?are estimated using the full covariance matrix.? The cell esds are taken? ?into account individually in the estimation of esds in distances, angles? ?and torsion angles; correlations between esds in cell parameters are only? ?used when they are defined by crystal symmetry.? An approximate (isotropic)? ?treatment of cell esds is used for estimating esds involving l.s. planes.? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt C2 2.034(7) . ? Pt C1 2.067(7) . ? Pt P1 2.2466(18) . ? Pt P2 2.2692(19) . ? Br1 C8 1.888(8) . ? Br2 C14 1.896(9) . ? P1 C21 1.814(7) . ? P1 C27 1.819(7) . ? P1 C15 1.839(8) . ? P2 C39 1.821(7) . ? P2 C33 1.833(7) . ? P2 C20 1.841(7) . ? C1 C2 1.303(11) . ? C1 C9 1.459(11) . ? C2 C3 1.451(10) . ? C3 C8 1.397(11) . ? C3 C4 1.401(11) . ? C4 C5 1.386(11) . ? C5 C6 1.396(13) . ? C6 C7 1.387(12) . ? C7 C8 1.373(12) . ? C9 C14 1.410(12) . ? C9 C10 1.472(14) . ? C10 C11 1.406(14) . ? C11 C12 1.367(15) . ? C12 C13 1.373(14) . ? C13 C14 1.356(13) . ? C15 C16 1.373(10) . ? C15 C20 1.417(10) . ? C16 C17 1.396(11) . ? C17 C18 1.393(12) . ? C18 C19 1.380(12) . ? C19 C20 1.376(10) . ? C21 C26 1.396(10) . ? C21 C22 1.404(11) . ? C22 C23 1.387(10) . ? C23 C24 1.382(11) . ? C24 C25 1.378(12) . ? C25 C26 1.383(10) . ? C27 C32 1.388(10) . ? C27 C28 1.397(11) . ? C28 C29 1.379(12) . ? C29 C30 1.388(13) . ? C30 C31 1.355(14) . ? C31 C32 1.395(12) . ? C33 C34 1.363(11) . ? C33 C38 1.405(11) . ? C34 C35 1.386(12) . ? C35 C36 1.360(13) . ? C36 C37 1.376(13) . ? C37 C38 1.386(11) . ? C39 C40 1.394(11) . ? C39 C44 1.400(11) . ? C40 C41 1.388(11) . ? C41 C42 1.379(13) . ? C42 C43 1.388(14) . ? C43 C44 1.372(12) . ? 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 Pt C1 37.0(3) . . ? C2 Pt P1 115.4(2) . . ? C1 Pt P1 152.2(2) . . ? C2 Pt P2 159.7(2) . . ? C1 Pt P2 122.7(2) . . ? P1 Pt P2 84.90(7) . . ? C21 P1 C27 105.2(3) . . ? C21 P1 C15 107.2(3) . . ? C27 P1 C15 100.2(3) . . ? C21 P1 Pt 115.4(2) . . ? C27 P1 Pt 118.8(2) . . ? C15 P1 Pt 108.5(2) . . ? C39 P2 C33 103.9(3) . . ? C39 P2 C20 102.2(3) . . ? C33 P2 C20 104.8(4) . . ? C39 P2 Pt 116.7(3) . . ? C33 P2 Pt 119.8(3) . . ? C20 P2 Pt 107.4(2) . . ? C2 C1 C9 147.0(8) . . ? C2 C1 Pt 70.1(5) . . ? C9 C1 Pt 140.7(6) . . ? C1 C2 C3 146.3(8) . . ? C1 C2 Pt 72.9(5) . . ? C3 C2 Pt 140.7(6) . . ? C8 C3 C4 116.0(7) . . ? C8 C3 C2 124.6(7) . . ? C4 C3 C2 119.3(7) . . ? C5 C4 C3 121.7(8) . . ? C4 C5 C6 120.9(8) . . ? C7 C6 C5 117.9(8) . . ? C8 C7 C6 120.8(8) . . ? C7 C8 C3 122.8(7) . . ? C7 C8 Br1 116.9(6) . . ? C3 C8 Br1 120.3(6) . . ? C14 C9 C1 125.8(8) . . ? C14 C9 C10 117.2(8) . . ? C1 C9 C10 116.9(8) . . ? C11 C10 C9 116.2(11) . . ? C12 C11 C10 123.2(11) . . ? C11 C12 C13 119.8(10) . . ? C14 C13 C12 120.7(10) . . ? C13 C14 C9 122.4(9) . . ? C13 C14 Br2 119.5(7) . . ? C9 C14 Br2 118.1(6) . . ? C16 C15 C20 120.2(7) . . ? C16 C15 P1 122.7(6) . . ? C20 C15 P1 116.9(5) . . ? C15 C16 C17 120.6(7) . . ? C18 C17 C16 119.2(7) . . ? C19 C18 C17 120.0(8) . . ? C18 C19 C20 121.5(7) . . ? C19 C20 C15 118.5(7) . . ? C19 C20 P2 126.2(6) . . ? C15 C20 P2 115.3(5) . . ? C26 C21 C22 119.0(7) . . ? C26 C21 P1 122.3(6) . . ? C22 C21 P1 118.4(5) . . ? C23 C22 C21 120.1(7) . . ? C24 C23 C22 120.1(7) . . ? C23 C24 C25 120.2(7) . . ? C26 C25 C24 120.6(7) . . ? C25 C26 C21 120.0(7) . . ? C32 C27 C28 118.3(7) . . ? C32 C27 P1 117.2(6) . . ? C28 C27 P1 124.4(6) . . ? C29 C28 C27 120.8(8) . . ? C28 C29 C30 119.9(9) . . ? C31 C30 C29 120.0(8) . . ? C30 C31 C32 120.7(8) . . ? C27 C32 C31 120.3(8) . . ? C34 C33 C38 119.2(7) . . ? C34 C33 P2 124.0(6) . . ? C38 C33 P2 116.7(6) . . ? C33 C34 C35 121.4(8) . . ? C36 C35 C34 119.0(9) . . ? C35 C36 C37 121.4(8) . . ? C36 C37 C38 119.7(8) . . ? C37 C38 C33 119.3(8) . . ? C40 C39 C44 118.7(7) . . ? C40 C39 P2 123.3(6) . . ? C44 C39 P2 118.0(6) . . ?? C39 C40 C41 120.0(7) . . ? C42 C41 C40 121.1(8) . . ? C41 C42 C43 118.7(7) . . ? C44 C43 C42 121.3(8) . . ? C43 C44 C39 120.2(8) . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 3.193 _refine_diff_density_min -2.345 _refine_diff_density_rms 0.197 #==== END data_FO2930(Compound4) _database_code_depnum_ccdc_archive 'CCDC 660014' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44 H32 Br2 P2 Pt' _chemical_formula_weight 977.55 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.8929(3) _cell_length_b 10.7362(4) _cell_length_c 21.0258(7) _cell_angle_alpha 80.862(2) _cell_angle_beta 88.179(2) _cell_angle_gamma 68.483(2) _cell_volume 1843.09(11) _cell_formula_units_Z 2 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.761 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 948 _exptl_absorpt_coefficient_mu 6.093 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. R.H. Blessing, Acta Cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.3949 _exptl_absorpt_correction_T_max 0.4449 _exptl_special_details ; ? ; _diffrn_ambient_temperature 183(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'phi- + omega-scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13314 _diffrn_reflns_av_R_equivalents 0.0376 _diffrn_reflns_av_sigmaI/netI 0.0716 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -267 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.57 _diffrn_reflns_theta_max 27.49 _reflns_number_total 8374 _reflns_number_gt 6723 _reflns_threshold_expression >2sigma(I) _computing_data_collection COLLECT? _computing_cell_refinement DENZO _computing_data_reduction DENZO _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL/PC _computing_publication_material SHELXL-97 _refine_special_details ; ?Refinement of F^2^ against ALL reflections.? The weighted R-factor wR and? ?goodness of fit S are based on F^2^, conventional R-factors R are based? ?on F, with F set to zero for negative F^2^. The threshold expression of? ?F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is? ?not relevant to the choice of reflections for refinement.? R-factors based? ?on F^2^ are statistically about twice as large as those based on F, and R- ? ?factors based on ALL data will be even larger.? ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0778P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8374 _refine_ls_number_parameters 442 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0762 _refine_ls_R_factor_gt 0.0560 _refine_ls_wR_factor_ref 0.1501 _refine_ls_wR_factor_gt 0.1408 _refine_ls_goodness_of_fit_ref 1.188 _refine_ls_restrained_S_all 1.188 _refine_ls_shift/su_max 0.014 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt Pt 0.78011(3) 0.87121(3) 0.724572(13) 0.02421(11) Uani 1 1 d . . .? Br1 Br 0.64080(13) 1.15524(14) 0.91333(6) 0.0681(3) Uani 1 1 d . . .? Br2 Br 0.41965(12) 1.12543(11) 0.76616(6) 0.0597(3) Uani 1 1 d . . .? P1 P 0.9075(2) 0.6681(2) 0.78859(9) 0.0249(4) Uani 1 1 d . . .? P2 P 0.7056(2) 0.7524(2) 0.66000(9) 0.0247(4) Uani 1 1 d . . .? C1 C 0.8564(8) 0.9652(8) 0.7855(3) 0.0262(16) Uani 1 1 d . . .? C2 C 0.9117(10) 1.0033(8) 0.8268(4) 0.0327(17) Uani 1 1 d . . .? C3 C 0.9658(10) 1.0557(9) 0.8757(4) 0.0359(18) Uani 1 1 d . . .? C4 C 1.1322(13) 1.0364(11) 0.8818(5) 0.054(3) Uani 1 1 d . . .? H4A H 1.2088 0.9855 0.8541 0.065 Uiso 1 1 calc R . .? C5 C 1.1813(14) 1.0923(12) 0.9279(5) 0.061(3) Uani 1 1 d . . .? H5A H 1.2915 1.0832 0.9300 0.073 Uiso 1 1 calc R . .? C6 C 1.0785(15) 1.1595(12) 0.9703(5) 0.062(3) Uani 1 1 d . . .? H6A H 1.1166 1.1948 1.0024 0.074 Uiso 1 1 calc R . .? C7 C 0.9175(16) 1.1765(11) 0.9667(5) 0.061(3) Uani 1 1 d . . .? H7A H 0.8444 1.2227 0.9967 0.073 Uiso 1 1 calc R . .? C8 C 0.8621(12) 1.1263(9) 0.9193(4) 0.046(2) Uani 1 1 d . . .? C9 C 0.6585(10) 1.0582(9) 0.6683(4) 0.0352(18) Uani 1 1 d . . .? C10 C 0.7200(13) 1.1008(10) 0.6097(4) 0.049(2) Uani 1 1 d . . .? H10A H 0.8192 1.0410 0.5958 0.059 Uiso 1 1 calc R . .? C11 C 0.6461(16) 1.2216(11) 0.5723(5) 0.062(3) Uani 1 1 d . . .? H11A H 0.6930 1.2441 0.5330 0.075 Uiso 1 1 calc R . .? C12 C 0.5065(16) 1.3106(13) 0.5900(5) 0.067(3) Uani 1 1 d . . .? H12A H 0.4558 1.3948 0.5628 0.081 Uiso 1 1 calc R . .? C13 C 0.4356(13) 1.2825(11) 0.6466(6) 0.058(3) Uani 1 1 d . . .? H13A H 0.3365 1.3451 0.6589 0.070 Uiso 1 1 calc R . .? C14 C 0.5164(10) 1.1564(10) 0.6858(5) 0.044(2) Uani 1 1 d . . .? C15 C 0.8876(9) 0.5328(8) 0.7509(4) 0.0281(16) Uani 1 1 d . . .? C16 C 0.9624(10) 0.3947(8) 0.7753(4) 0.0335(17) Uani 1 1 d . . .? H16A H 1.0333 0.3663 0.8120 0.040 Uiso 1 1 calc R . .? C17 C 0.9321(12) 0.3001(9) 0.7453(4) 0.042(2) Uani 1 1 d . . .? H17A H 0.9825 0.2065 0.7622 0.051 Uiso 1 1 calc R . .? C18 C 0.8306(11) 0.3383(9) 0.6917(4) 0.040(2) Uani 1 1 d . . .? H18A H 0.8086 0.2718 0.6729 0.048 Uiso 1 1 calc R . .? C19 C 0.7611(10) 0.4740(8) 0.6656(4) 0.0331(17) Uani 1 1 d . . .? H19A H 0.6941 0.5004 0.6278 0.040 Uiso 1 1 calc R . .? C20 C 0.7888(8) 0.5731(7) 0.6945(3) 0.0258(15) Uani 1 1 d . . .? C21 C 1.1229(9) 0.6146(8) 0.8071(4) 0.0312(17) Uani 1 1 d . . .? C22 C 1.2379(10) 0.5348(10) 0.7710(5) 0.047(2) Uani 1 1 d . . .? H22A H 1.2063 0.5012 0.7366 0.056 Uiso 1 1 calc R . .? C23 C 1.4003(11) 0.5032(11) 0.7844(6) 0.060(3) Uani 1 1 d . . .? H23A H 1.4785 0.4482 0.7586 0.072 Uiso 1 1 calc R . .? C24 C 1.4507(12) 0.5477(11) 0.8329(6) 0.061(3) Uani 1 1 d . . .? H24A H 1.5629 0.5244 0.8412 0.074 Uiso 1 1 calc R . .? C25 C 1.3344(12) 0.6296(11) 0.8712(5) 0.056(3) Uani 1 1 d . . .? H25A H 1.3670 0.6604 0.9064 0.067 Uiso 1 1 calc R . .? C26 C 1.1715(10) 0.6641(9) 0.8565(4) 0.041(2) Uani 1 1 d . . .? H26A H 1.0923 0.7225 0.8806 0.049 Uiso 1 1 calc R . .? C27 C 0.8170(8) 0.6564(8) 0.8665(4) 0.0292(16) Uani 1 1 d . . .? C28 C 0.6812(10) 0.7657(9) 0.8805(4) 0.0343(17) Uani 1 1 d . . .? H28A H 0.6396 0.8463 0.8499 0.041 Uiso 1 1 calc R . .? C29 C 0.6073(11) 0.7548(10) 0.9402(4) 0.043(2) Uani 1 1 d . . .? H29A H 0.5140 0.8279 0.9494 0.051 Uiso 1 1 calc R . .? C30 C 0.6679(11) 0.6404(10) 0.9852(4) 0.046(2) Uani 1 1 d . . .? H30A H 0.6167 0.6343 1.0253 0.055 Uiso 1 1 calc R . .? C31 C 0.8033(13) 0.5344(10) 0.9723(4) 0.050(2) Uani 1 1 d . . .? H31A H 0.8474 0.4562 1.0041 0.060 Uiso 1 1 calc R . .? C32 C 0.8757(12) 0.5406(9) 0.9132(4) 0.045(2) Uani 1 1 d . . .? H32A H 0.9666 0.4652 0.9043 0.054 Uiso 1 1 calc R . .? C33 C 0.4923(9) 0.7869(8) 0.6514(4) 0.0305(17) Uani 1 1 d . . .? C34 C 0.3929(10) 0.8435(9) 0.7000(4) 0.0377(19) Uani 1 1 d . . .? H34A H 0.4372 0.8669 0.7347 0.045 Uiso 1 1 calc R . .? C35 C 0.2303(11) 0.8656(11) 0.6977(5) 0.050(2) Uani 1 1 d . . .? H35A H 0.1630 0.9073 0.7303 0.060 Uiso 1 1 calc R . .? C36 C 0.1644(12) 0.8292(12) 0.6500(5) 0.059(3) Uani 1 1 d . . .? H36A H 0.0525 0.8435 0.6500 0.071 Uiso 1 1 calc R . .? C37 C 0.2599(12) 0.7711(13) 0.6012(5) 0.060(3) Uani 1 1 d . . .? H37A H 0.2137 0.7459 0.5676 0.072 Uiso 1 1 calc R . .? C38 C 0.4243(10) 0.7501(11) 0.6018(4) 0.046(2) Uani 1 1 d . . .? H38A H 0.4903 0.7106 0.5684 0.055 Uiso 1 1 calc R . .? C39 C 0.7804(9) 0.7561(7) 0.5783(3) 0.0264(15) Uani 1 1 d . . .? C40 C 0.9262(10) 0.6600(9) 0.5637(4) 0.0367(18) Uani 1 1 d . . .? H40A H 0.9861 0.5885 0.5965 0.044 Uiso 1 1 calc R . .? C41 C 0.9855(11) 0.6675(10) 0.5014(5) 0.049(2) Uani 1 1 d . . .? H41A H 1.0846 0.6008 0.4918 0.059 Uiso 1 1 calc R . .? C42 C 0.8990(12) 0.7729(11) 0.4538(4) 0.050(2) Uani 1 1 d . . .? H42A H 0.9384 0.7796 0.4113 0.060 Uiso 1 1 calc R . .? C43 C 0.7564(12) 0.8665(11) 0.4688(4) 0.054(3) Uani 1 1 d . . .? H43A H 0.6959 0.9378 0.4361 0.065 Uiso 1 1 calc R . .? C44 C 0.6974(10) 0.8607(9) 0.5304(4) 0.040(2) Uani 1 1 d . . .? H44A H 0.5994 0.9290 0.5398 0.048 Uiso 1 1 calc R . .? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt 0.02268(15) 0.02283(17) 0.02781(17) -0.00701(11) 0.00325(11) -0.00813(12) Br1 0.0512(6) 0.0822(9) 0.0631(7) -0.0312(6) 0.0097(5) -0.0080(6) Br2 0.0466(5) 0.0511(6) 0.0748(7) -0.0197(5) 0.0151(5) -0.0074(5) P1 0.0238(9) 0.0252(10) 0.0270(9) -0.0060(8) -0.0009(7) -0.0096(8) P2 0.0226(9) 0.0260(10) 0.0255(9) -0.0067(8) 0.0024(7) -0.0079(8) C1 0.019(3) 0.029(4) 0.024(4) 0.004(3) 0.004(3) -0.006(3) C2 0.036(4) 0.037(5) 0.032(4) -0.012(3) 0.011(3) -0.019(4) C3 0.045(5) 0.033(5) 0.031(4) 0.000(3) -0.002(4) -0.016(4) C4 0.065(6) 0.062(7) 0.042(5) 0.001(5) -0.021(5) -0.032(6) C5 0.065(7) 0.063(7) 0.065(7) -0.004(6) -0.011(6) -0.038(6) C6 0.079(8) 0.059(7) 0.055(6) -0.016(5) -0.019(6) -0.029(6) C7 0.099(9) 0.046(6) 0.038(5) -0.015(5) -0.007(5) -0.023(6) C8 0.063(6) 0.035(5) 0.040(5) -0.012(4) 0.003(4) -0.016(5) C9 0.041(4) 0.034(5) 0.034(4) -0.014(4) -0.003(4) -0.013(4) C10 0.073(7) 0.039(5) 0.039(5) -0.004(4) -0.010(5) -0.026(5) C11 0.089(9) 0.052(7) 0.044(6) 0.005(5) -0.015(6) -0.028(7) C12 0.084(9) 0.062(8) 0.051(6) 0.003(6) -0.033(6) -0.023(7) C13 0.051(6) 0.040(6) 0.078(8) -0.017(5) -0.008(5) -0.007(5) C14 0.033(4) 0.043(5) 0.052(5) -0.015(4) -0.009(4) -0.006(4) C15 0.028(4) 0.024(4) 0.033(4) -0.006(3) 0.005(3) -0.010(3) C16 0.044(5) 0.024(4) 0.031(4) -0.003(3) -0.002(3) -0.012(4) C17 0.058(6) 0.026(4) 0.040(5) -0.006(4) 0.002(4) -0.012(4) C18 0.054(5) 0.030(5) 0.044(5) -0.015(4) 0.005(4) -0.022(4) C19 0.037(4) 0.036(5) 0.032(4) -0.010(3) 0.001(3) -0.018(4) C20 0.025(3) 0.025(4) 0.031(4) -0.006(3) 0.001(3) -0.012(3) C21 0.025(4) 0.029(4) 0.039(4) -0.004(3) 0.000(3) -0.009(3) C22 0.034(4) 0.049(6) 0.055(6) -0.016(5) -0.002(4) -0.011(4) C23 0.031(5) 0.045(6) 0.093(8) -0.014(6) 0.010(5) -0.001(4) C24 0.034(5) 0.054(7) 0.090(8) 0.016(6) -0.022(5) -0.018(5) C25 0.038(5) 0.068(7) 0.066(7) 0.005(6) -0.015(5) -0.028(5) C26 0.036(4) 0.047(5) 0.045(5) -0.006(4) -0.006(4) -0.022(4) C27 0.022(3) 0.038(4) 0.033(4) -0.011(3) 0.002(3) -0.013(3) C28 0.035(4) 0.031(4) 0.037(4) -0.014(3) 0.004(3) -0.010(4) C29 0.035(4) 0.049(6) 0.039(5) -0.012(4) 0.010(4) -0.009(4) C30 0.050(5) 0.054(6) 0.041(5) -0.014(4) 0.014(4) -0.027(5) C31 0.066(6) 0.042(5) 0.036(5) 0.005(4) 0.005(4) -0.018(5) C32 0.052(5) 0.030(5) 0.041(5) 0.000(4) 0.010(4) -0.004(4) C33 0.022(3) 0.031(4) 0.034(4) 0.002(3) -0.003(3) -0.007(3) C34 0.031(4) 0.038(5) 0.042(5) -0.011(4) 0.009(4) -0.008(4) C35 0.034(4) 0.062(7) 0.053(6) -0.012(5) 0.018(4) -0.018(5) C36 0.033(5) 0.085(8) 0.064(7) 0.000(6) 0.004(5) -0.030(5) C37 0.041(5) 0.098(9) 0.047(6) -0.014(6) -0.004(4) -0.031(6) C38 0.030(4) 0.073(7) 0.038(5) -0.019(5) 0.004(4) -0.019(5) C39 0.031(4) 0.025(4) 0.027(4) -0.008(3) 0.003(3) -0.014(3) C40 0.032(4) 0.033(5) 0.045(5) -0.009(4) 0.010(4) -0.012(4) C41 0.042(5) 0.049(6) 0.058(6) -0.020(5) 0.020(4) -0.014(5) C42 0.064(6) 0.063(7) 0.032(4) -0.012(4) 0.024(4) -0.033(6) C43 0.052(6) 0.065(7) 0.031(5) -0.003(5) 0.001(4) -0.007(5) C44 0.038(4) 0.045(5) 0.029(4) -0.005(4) -0.001(3) -0.005(4) _geom_special_details ; ?All esds (except the esd in the dihedral angle between two l.s. planes)? ?are estimated using the full covariance matrix.? The cell esds are taken? ?into account individually in the estimation of esds in distances, angles? ?and torsion angles; correlations between esds in cell parameters are only? ?used when they are defined by crystal symmetry.? An approximate (isotropic)? ?treatment of cell esds is used for estimating esds involving l.s. planes.? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt C1 2.022(8) . ? Pt C9 2.082(9) . ? Pt P2 2.2667(19) . ? Pt P1 2.2808(19) . ? Br1 C8 1.882(10) . ? Br2 C14 1.909(10) . ? P1 C27 1.809(8) . ? P1 C21 1.822(8) . ? P1 C15 1.826(8) . ? P2 C33 1.804(7) . ? P2 C39 1.822(7) . ? P2 C20 1.823(7) . ? C1 C2 1.203(11) . ? C2 C3 1.422(11) . ? C3 C8 1.385(13) . ? C3 C4 1.424(13) . ? C4 C5 1.377(14) . ? C5 C6 1.349(16) . ? C6 C7 1.378(16) . ? C7 C8 1.386(13) . ? C9 C10 1.411(12) . ? C9 C14 1.400(12) . ? C10 C11 1.347(13) . ? C11 C12 1.344(17) . ? C12 C13 1.372(16) . ? C13 C14 1.414(14) . ? C15 C16 1.400(11) . ? C15 C20 1.410(10) . ? C16 C17 1.384(12) . ? C17 C18 1.378(12) . ? C18 C19 1.384(12) . ? C19 C20 1.403(11) . ? C21 C22 1.368(12) . ? C21 C26 1.385(12) . ? C22 C23 1.384(12) . ? C23 C24 1.344(16) . ? C24 C25 1.414(16) . ? C25 C26 1.389(12) . ? C27 C32 1.397(11) . ? C27 C28 1.403(11) . ? C28 C29 1.407(11) . ? C29 C30 1.368(13) . ? C30 C31 1.376(14) . ? C31 C32 1.385(12) . ? C33 C34 1.393(11) . ? C33 C38 1.399(12) . ? C34 C35 1.378(12) . ? C35 C36 1.353(14) . ? C36 C37 1.387(15) . ? C37 C38 1.395(12) . ? C39 C44 1.378(11) . ? C39 C40 1.390(11) . ? C40 C41 1.398(12) . ? C41 C42 1.387(14) . ? C42 C43 1.364(14) . ? C43 C44 1.383(12) . ? 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 C1 Pt C9 89.7(3) . . ? C1 Pt P2 176.1(2) . . ? C9 Pt P2 94.1(2) . . ? C1 Pt P1 89.8(2) . . ? C9 Pt P1 178.2(2) . . ? P2 Pt P1 86.41(7) . . ? C27 P1 C21 104.4(3) . . ? C27 P1 C15 105.6(3) . . ? C21 P1 C15 105.1(4) . . ? C27 P1 Pt 112.6(3) . . ? C21 P1 Pt 119.0(2) . . ? C15 P1 Pt 109.1(2) . . ? C33 P2 C39 105.5(3) . . ? C33 P2 C20 103.4(3) . . ? C39 P2 C20 103.7(3) . . ? C33 P2 Pt 117.2(3) . . ? C39 P2 Pt 116.9(2) . . ? C20 P2 Pt 108.7(2) . . ? C2 C1 Pt 170.8(7) . . ? C1 C2 C3 175.9(9) . . ? C8 C3 C4 117.1(9) . . ? C8 C3 C2 122.5(8) . . ? C4 C3 C2 120.4(8) . . ? C5 C4 C3 119.5(11) . . ? C6 C5 C4 122.3(11) . . ? C5 C6 C7 119.3(10) . . ? C6 C7 C8 120.1(11) . . ? C3 C8 C7 121.6(10) . . ? C3 C8 Br1 118.9(7) . . ? C7 C8 Br1 119.5(8) . . ? C10 C9 C14 113.5(8) . . ? C10 C9 Pt 121.8(7) . . ? C14 C9 Pt 124.5(6) . . ? C11 C10 C9 123.6(11) . . ? C10 C11 C12 120.6(11) . . ? C13 C12 C11 121.5(11) . . ? C12 C13 C14 117.2(10) . . ? C13 C14 C9 123.5(9) . . ? C13 C14 Br2 115.8(7) . . ? C9 C14 Br2 120.7(7) . . ? C16 C15 C20 119.6(7) . . ? C16 C15 P1 123.7(6) . . ? C20 C15 P1 116.6(6) . . ? C17 C16 C15 119.4(8) . . ? C18 C17 C16 121.6(8) . . ? C17 C18 C19 119.6(8) . . ? C18 C19 C20 120.5(8) . . ? C19 C20 C15 119.2(7) . . ? C19 C20 P2 121.9(6) . . ? C15 C20 P2 118.9(5) . . ? C22 C21 C26 119.1(7) . . ? C22 C21 P1 122.0(6) . . ? C26 C21 P1 118.8(6) . . ? C21 C22 C23 120.0(9) . . ? C24 C23 C22 122.1(10) . . ? C23 C24 C25 119.0(9) . . ? C26 C25 C24 118.7(10) . . ? C21 C26 C25 121.0(9) . . ? C32 C27 C28 118.4(7) . . ? C32 C27 P1 122.2(6) . . ? C28 C27 P1 119.4(6) . . ? C27 C28 C29 119.4(8) . . ? C30 C29 C28 120.9(9) . . ? C29 C30 C31 119.8(8) . . ? C30 C31 C32 120.5(8) . . ? C31 C32 C27 120.9(9) . . ? C34 C33 C38 118.6(7) . . ? C34 C33 P2 117.5(6) . . ? C38 C33 P2 123.6(6) . . ? C35 C34 C33 120.2(8) . . ? C36 C35 C34 121.4(9) . . ? C35 C36 C37 120.2(8) . . ? C36 C37 C38 119.5(9) . . ? C37 C38 C33 120.2(8) . . ? C44 C39 C40 118.6(7) . . ? C44 C39 P2 119.9(6) . . ? C40 C39 P2 121.3(6) . . ? C39 C40 C41 120.7(8) . . ? C42 C41 C40 119.7(9) . . ? C43 C42 C41 118.9(8) . . ? C42 C43 C44 121.8(9) . . ? C39 C44 C43 120.2(9) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 5.363 _refine_diff_density_min -2.102 _refine_diff_density_rms 0.202 #==== END data_FO3264(Compound6) _database_code_depnum_ccdc_archive 'CCDC 662326' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C44 H32 Br2 P2 Pt), 3(C4 H8 O)' _chemical_formula_sum 'C50 H44 Br2 O1.50 P2 Pt' _chemical_formula_weight 1085.70 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c _symmetry_space_group_name_Hall -P2ybc 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 21.3703(6) _cell_length_b 13.6258(3) _cell_length_c 15.6040(3) _cell_angle_alpha 90.00 _cell_angle_beta 93.290(1) _cell_angle_gamma 90.00 _cell_volume 4536.20(18) _cell_formula_units_Z 4 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.04 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.590 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2136 _exptl_absorpt_coefficient_mu 4.962 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. R.H. Blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.810 _exptl_absorpt_correction_T_max 0.932 _exptl_special_details ; ? ; _diffrn_ambient_temperature 183(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a? _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'phi- + omega-scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 31809 _diffrn_reflns_av_R_equivalents 0.0757 _diffrn_reflns_av_sigmaI/netI 0.0779 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.77 _diffrn_reflns_theta_max 27.48 _reflns_number_total 10383 _reflns_number_gt 7479 _reflns_threshold_expression >2sigma(I) _computing_data_collection COLLECT _computing_cell_refinement DENZO _computing_data_reduction DENZO _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL/PC _computing_publication_material SHELXL-97 _refine_special_details ; ?Refinement of F^2^ against ALL reflections.? The weighted R-factor wR and? ?goodness of fit S are based on F^2^, conventional R-factors R are based? ?on F, with F set to zero for negative F^2^. The threshold expression of? ?F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is? ?not relevant to the choice of reflections for refinement.? R-factors based? ?on F^2^ are statistically about twice as large as those based on F, and R- ? ?factors based on ALL data will be even larger.? ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0553P)^2^+9.2762P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10383 _refine_ls_number_parameters 506 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0819 _refine_ls_R_factor_gt 0.0488 _refine_ls_wR_factor_ref 0.1194 _refine_ls_wR_factor_gt 0.1059 _refine_ls_goodness_of_fit_ref 1.015 _refine_ls_restrained_S_all 1.015 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt Pt 0.777054(11) 0.091580(16) 0.530298(14) 0.02039(8) Uani 1 1 d . . .? Br1 Br 0.56417(5) -0.10580(7) 0.76797(7) 0.0673(3) Uani 1 1 d . . .? Br2 Br 0.82966(4) -0.05666(5) 0.47624(4) 0.03630(18) Uani 1 1 d . . .? P1 P 0.86621(8) 0.14371(11) 0.60518(10) 0.0226(3) Uani 1 1 d . . .? P2 P 0.73310(8) 0.22873(11) 0.57137(10) 0.0222(3) Uani 1 1 d . . .? C1 C 0.6914(3) 0.0544(4) 0.4675(4) 0.0239(13) Uani 1 1 d . . .? C2 C 0.6698(3) 0.0992(5) 0.3924(4) 0.0313(15) Uani 1 1 d . . .? H2A H 0.6961 0.1446 0.3654 0.038 Uiso 1 1 calc R . .? C3 C 0.6097(4) 0.0794(5) 0.3544(5) 0.0415(18) Uani 1 1 d . . .? H3A H 0.5969 0.1076 0.3006 0.050 Uiso 1 1 calc R . .? C4 C 0.5696(4) 0.0188(5) 0.3959(5) 0.0419(19) Uani 1 1 d . . .? H4A H 0.5282 0.0079 0.3723 0.050 Uiso 1 1 calc R . .? C5 C 0.5898(4) -0.0260(5) 0.4719(5) 0.0413(18) Uani 1 1 d . . .? H5A H 0.5624 -0.0685 0.5002 0.050 Uiso 1 1 calc R . .? C6 C 0.6506(3) -0.0089(4) 0.5076(4) 0.0270(14) Uani 1 1 d . . .? C7 C 0.6688(3) -0.0589(4) 0.5903(4) 0.0280(14) Uani 1 1 d . . .? C8 C 0.6776(4) -0.1039(5) 0.6493(5) 0.0394(18) Uani 1 1 d . . .? C9 C 0.6867(4) -0.1666(5) 0.7252(4) 0.0350(16) Uani 1 1 d . . .? C10 C 0.7416(4) -0.2200(5) 0.7411(5) 0.0465(19) Uani 1 1 d . . .? H10A H 0.7748 -0.2134 0.7035 0.056 Uiso 1 1 calc R . .? C11 C 0.7487(5) -0.2825(6) 0.8108(6) 0.057(2) Uani 1 1 d . . .? H11A H 0.7863 -0.3191 0.8200 0.069 Uiso 1 1 calc R . .? C12 C 0.7008(5) -0.2923(6) 0.8679(5) 0.056(2) Uani 1 1 d . . .? H12A H 0.7057 -0.3354 0.9157 0.067 Uiso 1 1 calc R . .? C13 C 0.6469(5) -0.2391(6) 0.8538(5) 0.055(2) Uani 1 1 d . . .? H13A H 0.6145 -0.2448 0.8927 0.066 Uiso 1 1 calc R . .? C14 C 0.6390(4) -0.1777(5) 0.7845(5) 0.0425(18) Uani 1 1 d . . .? C15 C 0.8439(3) 0.2469(4) 0.6724(4) 0.0251(13) Uani 1 1 d . . .? C16 C 0.8830(3) 0.2880(5) 0.7362(4) 0.0295(14) Uani 1 1 d . . .? H16A H 0.9241 0.2627 0.7469 0.035 Uiso 1 1 calc R . .? C17 C 0.8628(3) 0.3659(5) 0.7849(4) 0.0336(16) Uani 1 1 d . . .? H17A H 0.8898 0.3929 0.8292 0.040 Uiso 1 1 calc R . .? C18 C 0.8035(3) 0.4040(5) 0.7690(4) 0.0297(14) Uani 1 1 d . . .? H18A H 0.7899 0.4576 0.8021 0.036 Uiso 1 1 calc R . .? C19 C 0.7638(3) 0.3644(5) 0.7049(4) 0.0296(14) Uani 1 1 d . . .? H19A H 0.7233 0.3917 0.6936 0.035 Uiso 1 1 calc R . .? C20 C 0.7829(3) 0.2848(4) 0.6570(4) 0.0249(13) Uani 1 1 d . . .? C21 C 0.9068(3) 0.0578(5) 0.6784(4) 0.0272(14) Uani 1 1 d . . .? C22 C 0.8727(3) -0.0228(5) 0.7063(4) 0.0346(16) Uani 1 1 d . . .? H22A H 0.8305 -0.0326 0.6857 0.041 Uiso 1 1 calc R . .? C23 C 0.9013(4) -0.0881(6) 0.7640(5) 0.0461(19) Uani 1 1 d . . .? H23A H 0.8784 -0.1429 0.7832 0.055 Uiso 1 1 calc R . .? C24 C 0.9633(4) -0.0742(6) 0.7944(5) 0.047(2) Uani 1 1 d . . .? H24A H 0.9825 -0.1196 0.8339 0.056 Uiso 1 1 calc R . .? C25 C 0.9965(4) 0.0046(6) 0.7674(4) 0.048(2) Uani 1 1 d . . .? H25A H 1.0386 0.0140 0.7889 0.058 Uiso 1 1 calc R . .? C26 C 0.9692(4) 0.0713(5) 0.7087(4) 0.0374(17) Uani 1 1 d . . .? H26A H 0.9926 0.1254 0.6894 0.045 Uiso 1 1 calc R . .? C27 C 0.9254(3) 0.1930(5) 0.5382(4) 0.0255(13) Uani 1 1 d . . .? C28 C 0.9652(3) 0.1286(5) 0.4988(4) 0.0307(15) Uani 1 1 d . . .? H28A H 0.9647 0.0608 0.5130 0.037 Uiso 1 1 calc R . .? C29 C 1.0058(3) 0.1625(5) 0.4388(4) 0.0368(16) Uani 1 1 d . . .? H29A H 1.0334 0.1183 0.4128 0.044 Uiso 1 1 calc R . .? C30 C 1.0058(3) 0.2602(5) 0.4176(5) 0.0393(17) Uani 1 1 d . . .? H30A H 1.0334 0.2835 0.3765 0.047 Uiso 1 1 calc R . .? C31 C 0.9660(4) 0.3248(5) 0.4553(5) 0.0428(18) Uani 1 1 d . . .? H31A H 0.9657 0.3922 0.4395 0.051 Uiso 1 1 calc R . .? C32 C 0.9265(3) 0.2917(5) 0.5161(5) 0.0354(16) Uani 1 1 d . . .? H32A H 0.8999 0.3367 0.5429 0.043 Uiso 1 1 calc R . .? C33 C 0.7295(3) 0.3210(4) 0.4869(4) 0.0271(14) Uani 1 1 d . . .? C34 C 0.7715(3) 0.3126(5) 0.4225(4) 0.0316(15) Uani 1 1 d . . .? H34A H 0.7982 0.2569 0.4207 0.038 Uiso 1 1 calc R . .? C35 C 0.7745(4) 0.3856(6) 0.3608(5) 0.048(2) Uani 1 1 d . . .? H35A H 0.8044 0.3813 0.3182 0.058 Uiso 1 1 calc R . .? C36 C 0.7344(5) 0.4638(6) 0.3615(5) 0.060(3) Uani 1 1 d . . .? H36A H 0.7358 0.5126 0.3181 0.072 Uiso 1 1 calc R . .? C37 C 0.6925(5) 0.4728(6) 0.4234(6) 0.062(3) Uani 1 1 d . . .? H37A H 0.6651 0.5278 0.4233 0.074 Uiso 1 1 calc R . .? C38 C 0.6896(4) 0.4018(5) 0.4868(5) 0.0424(18) Uani 1 1 d . . .? H38A H 0.6605 0.4082 0.5302 0.051 Uiso 1 1 calc R . .? C39 C 0.6560(3) 0.2190(4) 0.6128(4) 0.0310(15) Uani 1 1 d . . .? C40 C 0.6018(3) 0.2273(5) 0.5595(5) 0.0415(18) Uani 1 1 d . . .? H40A H 0.6041 0.2444 0.5008 0.050 Uiso 1 1 calc R . .? C41 C 0.5440(4) 0.2099(6) 0.5939(7) 0.058(2) Uani 1 1 d . . .? H41A H 0.5068 0.2153 0.5578 0.070 Uiso 1 1 calc R . .? C42 C 0.5395(4) 0.1852(6) 0.6791(7) 0.055(2) Uani 1 1 d . . .? H42A H 0.4998 0.1732 0.7013 0.066 Uiso 1 1 calc R . .? C43 C 0.5932(4) 0.1782(6) 0.7314(6) 0.055(2) Uani 1 1 d . . .? H43A H 0.5906 0.1618 0.7903 0.066 Uiso 1 1 calc R . .? C44 C 0.6503(4) 0.1945(5) 0.6994(5) 0.0394(17) Uani 1 1 d . . .? H44A H 0.6870 0.1892 0.7364 0.047 Uiso 1 1 calc R . .? O1TA O 1.1265(5) 0.4558(7) 0.4129(6) 0.116(3) Uiso 1 1 d . . .? C1TA C 1.1216(5) 0.4431(6) 0.5005(6) 0.061(3) Uani 1 1 d . . .? H1TA H 1.0770 0.4393 0.5143 0.074 Uiso 1 1 calc R . .? H1TB H 1.1414 0.4988 0.5326 0.074 Uiso 1 1 calc R . .? C2TA C 1.1547(5) 0.3491(7) 0.5240(6) 0.063(3) Uani 1 1 d . . .? H2TA H 1.1854 0.3591 0.5732 0.075 Uiso 1 1 calc R . .? H2TB H 1.1244 0.2979 0.5393 0.075 Uiso 1 1 calc R . .? C3TA C 1.1862(7) 0.3215(10) 0.4474(8) 0.110(5) Uani 1 1 d . . .? H3TA H 1.2321 0.3195 0.4600 0.131 Uiso 1 1 calc R . .? H3TB H 1.1722 0.2556 0.4277 0.131 Uiso 1 1 calc R . .? C4TA C 1.1709(6) 0.3930(10) 0.3824(7) 0.099(5) Uani 1 1 d . . .? H4TA H 1.2088 0.4303 0.3689 0.119 Uiso 1 1 calc R . .? H4TB H 1.1540 0.3603 0.3293 0.119 Uiso 1 1 calc R . .? O1TB O 0.5692(12) -0.3643(17) 0.5288(15) 0.054(6) Uiso 0.25 1 d P . .? O1TC O 0.6144(9) -0.5004(13) 0.6400(11) 0.031(4) Uiso 0.25 1 d P . .? C2TB C 0.6041(10) -0.3421(14) 0.5852(13) 0.066(5) Uiso 0.50 1 d P . .? H2TC H 0.5843 -0.2872 0.6154 0.080 Uiso 0.50 1 calc PR . .? H2TD H 0.6414 -0.3145 0.5591 0.080 Uiso 0.50 1 calc PR . .? C1TB C 0.6268(8) -0.4091(11) 0.6499(10) 0.046(4) Uiso 0.50 1 d P . .? H1TC H 0.6729 -0.4021 0.6561 0.055 Uiso 0.50 1 calc PR . .? H1TD H 0.6101 -0.3881 0.7049 0.055 Uiso 0.50 1 calc PR . .? C3TB C 0.5306(15) -0.395(2) 0.584(2) 0.118(10) Uiso 0.50 1 d P . .? H3TC H 0.4923 -0.4221 0.5540 0.141 Uiso 0.50 1 calc PR . .? H3TD H 0.5184 -0.3403 0.6212 0.141 Uiso 0.50 1 calc PR . .? C4TB C 0.5653(10) -0.4762(15) 0.6384(13) 0.071(5) Uiso 0.50 1 d P . .? H4TC H 0.5580 -0.4588 0.6986 0.085 Uiso 0.50 1 calc PR . .? H4TD H 0.5406 -0.5365 0.6261 0.085 Uiso 0.50 1 calc PR . .? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt 0.02335(14) 0.01902(12) 0.01856(11) -0.00039(10) -0.00100(8) -0.00007(10) Br1 0.0517(6) 0.0670(6) 0.0844(7) 0.0190(5) 0.0136(5) 0.0033(5) Br2 0.0430(4) 0.0280(3) 0.0371(4) -0.0081(3) -0.0048(3) 0.0081(3) P1 0.0218(9) 0.0228(8) 0.0229(7) -0.0017(6) -0.0019(6) 0.0021(6) P2 0.0220(9) 0.0217(7) 0.0227(7) -0.0019(6) -0.0016(6) 0.0031(6) C1 0.020(3) 0.025(3) 0.027(3) 0.000(3) 0.000(2) -0.005(3) C2 0.029(4) 0.037(4) 0.028(3) -0.003(3) -0.005(3) -0.008(3) C3 0.045(5) 0.047(4) 0.031(3) 0.003(3) -0.015(3) -0.008(4) C4 0.033(4) 0.043(4) 0.048(4) 0.004(4) -0.017(3) -0.007(3) C5 0.043(5) 0.040(4) 0.040(4) 0.000(3) 0.000(3) -0.018(3) C6 0.031(4) 0.024(3) 0.026(3) 0.003(3) 0.000(3) 0.000(3) C7 0.029(4) 0.014(3) 0.041(4) -0.005(3) 0.007(3) -0.012(3) C8 0.038(5) 0.031(4) 0.048(4) -0.010(4) -0.002(3) -0.005(3) C9 0.046(5) 0.025(3) 0.033(3) 0.002(3) -0.006(3) -0.008(3) C10 0.059(6) 0.035(4) 0.045(4) 0.004(4) -0.003(4) 0.003(4) C11 0.069(6) 0.035(4) 0.065(6) 0.006(4) -0.017(5) 0.001(4) C12 0.077(7) 0.047(5) 0.041(4) 0.020(4) -0.004(4) -0.009(5) C13 0.072(7) 0.057(5) 0.035(4) 0.003(4) 0.005(4) -0.020(5) C14 0.052(5) 0.036(4) 0.040(4) 0.004(3) 0.003(4) -0.005(4) C15 0.026(4) 0.027(3) 0.023(3) -0.001(3) 0.003(2) 0.001(3) C16 0.024(4) 0.033(3) 0.031(3) 0.000(3) -0.001(3) 0.002(3) C17 0.043(5) 0.034(4) 0.023(3) -0.008(3) -0.007(3) -0.006(3) C18 0.037(4) 0.024(3) 0.028(3) -0.008(3) 0.002(3) -0.007(3) C19 0.034(4) 0.026(3) 0.029(3) -0.003(3) 0.003(3) 0.005(3) C20 0.035(4) 0.023(3) 0.017(3) -0.002(2) 0.002(3) 0.001(3) C21 0.028(4) 0.030(3) 0.024(3) -0.007(3) 0.000(3) 0.011(3) C22 0.033(4) 0.041(4) 0.029(3) 0.002(3) 0.005(3) 0.012(3) C23 0.056(5) 0.040(4) 0.042(4) 0.008(4) 0.004(4) 0.013(4) C24 0.063(6) 0.045(5) 0.032(4) 0.011(3) 0.001(4) 0.019(4) C25 0.044(5) 0.071(6) 0.027(4) -0.014(4) -0.010(3) 0.031(4) C26 0.037(4) 0.037(4) 0.037(4) -0.003(3) -0.005(3) 0.010(3) C27 0.021(3) 0.033(3) 0.022(3) -0.002(3) -0.003(2) 0.003(3) C28 0.031(4) 0.027(3) 0.035(3) 0.003(3) 0.009(3) 0.000(3) C29 0.030(4) 0.043(4) 0.038(4) -0.003(3) 0.002(3) 0.005(3) C30 0.031(4) 0.049(4) 0.039(4) 0.000(4) 0.007(3) -0.006(3) C31 0.049(5) 0.032(4) 0.048(4) 0.009(3) 0.013(4) -0.006(3) C32 0.026(4) 0.036(4) 0.045(4) 0.001(3) 0.007(3) 0.001(3) C33 0.034(4) 0.021(3) 0.025(3) -0.004(3) -0.008(3) -0.001(3) C34 0.040(4) 0.029(3) 0.025(3) 0.004(3) -0.003(3) -0.003(3) C35 0.070(6) 0.042(4) 0.030(4) 0.009(3) -0.004(4) -0.010(4) C36 0.101(8) 0.038(5) 0.039(4) 0.016(4) -0.016(5) -0.001(5) C37 0.094(8) 0.038(4) 0.053(5) 0.006(4) -0.013(5) 0.019(5) C38 0.055(5) 0.032(4) 0.040(4) -0.002(3) -0.002(4) 0.013(4) C39 0.026(4) 0.020(3) 0.048(4) -0.009(3) 0.003(3) 0.004(3) C40 0.028(4) 0.044(4) 0.052(4) -0.013(4) -0.002(3) 0.005(3) C41 0.022(4) 0.052(5) 0.098(7) -0.023(5) -0.007(4) -0.002(4) C42 0.032(5) 0.036(4) 0.099(7) -0.014(5) 0.026(5) -0.007(4) C43 0.051(6) 0.049(5) 0.065(6) -0.004(4) 0.022(5) -0.005(4) C44 0.033(4) 0.039(4) 0.047(4) 0.001(3) 0.007(3) 0.004(3) C1TA 0.076(7) 0.042(4) 0.066(6) -0.005(4) -0.006(5) 0.003(5) C2TA 0.079(7) 0.056(5) 0.054(5) 0.012(4) -0.001(5) 0.007(5) C3TA 0.143(13) 0.105(9) 0.084(8) 0.044(7) 0.038(8) 0.075(9) C4TA 0.088(9) 0.142(11) 0.070(7) 0.055(7) 0.038(6) 0.050(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 Pt C1 2.089(6) . ? Pt P2 2.2033(16) . ? Pt P1 2.2900(16) . ? Pt Br2 2.4827(7) . ? Br1 C14 1.880(8) . ? P1 C27 1.816(7) . ? P1 C21 1.821(6) . ? P1 C15 1.834(6) . ? P2 C39 1.809(7) . ? P2 C33 1.820(6) . ? P2 C20 1.827(6) . ? C1 C2 1.378(9) . ? C1 C6 1.399(9) . ? C2 C3 1.408(9) . ? C3 C4 1.377(10) . ? C4 C5 1.380(10) . ? C5 C6 1.403(10) . ? C6 C7 1.492(9) . ? C7 C8 1.113(10) . ? C8 C9 1.463(10) . ? C9 C10 1.392(11) . ? C9 C14 1.423(11) . ? C10 C11 1.382(11) . ? C11 C12 1.400(13) . ? C12 C13 1.368(13) . ? C13 C14 1.371(11) . ? C15 C16 1.382(9) . ? C15 C20 1.409(9) . ? C16 C17 1.388(9) . ? C17 C18 1.378(10) . ? C18 C19 1.383(9) . ? C19 C20 1.392(8) . ? C21 C26 1.400(10) . ? C21 C22 1.400(10) . ? C22 C23 1.383(10) . ? C23 C24 1.394(12) . ? C24 C25 1.367(12) . ? C25 C26 1.395(10) . ? C27 C28 1.389(9) . ? C27 C32 1.389(9) . ? C28 C29 1.392(10) . ? C29 C30 1.371(10) . ? C30 C31 1.381(10) . ? C31 C32 1.381(10) . ? C33 C34 1.389(9) . ? C33 C38 1.392(9) . ? C34 C35 1.389(9) . ? C35 C36 1.368(12) . ? C36 C37 1.360(13) . ? C37 C38 1.388(11) . ? C39 C40 1.391(9) . ? C39 C44 1.404(10) . ? C40 C41 1.394(12) . ? C41 C42 1.380(13) . ? C42 C43 1.373(12) . ? C43 C44 1.362(11) . ? O1TA C4TA 1.382(14) . ? O1TA C1TA 1.387(12) . ? C1TA C2TA 1.499(12) . ? C2TA C3TA 1.455(14) . ? C3TA C4TA 1.431(14) . ? O1TB C2TB 1.16(3) . ? O1TB C3TB 1.29(4) . ? O1TC C4TB 1.10(2) . ? O1TC C1TB 1.28(2) . ? C2TB C1TB 1.43(2) . ? C3TB C4TB 1.56(3) . ? 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 C1 Pt P2 88.00(18) . . ? C1 Pt P1 174.71(18) . . ? P2 Pt P1 86.82(6) . . ? C1 Pt Br2 92.60(17) . . ? P2 Pt Br2 176.18(5) . . ? P1 Pt Br2 92.64(4) . . ? C27 P1 C21 106.1(3) . . ? C27 P1 C15 105.0(3) . . ? C21 P1 C15 105.3(3) . . ? C27 P1 Pt 114.06(19) . . ? C21 P1 Pt 118.2(2) . . ? C15 P1 Pt 107.1(2) . . ? C39 P2 C33 107.9(3) . . ? C39 P2 C20 105.9(3) . . ? C33 P2 C20 103.8(3) . . ? C39 P2 Pt 117.0(2) . . ? C33 P2 Pt 112.1(2) . . ? C20 P2 Pt 109.1(2) . . ? C2 C1 C6 117.8(6) . . ? C2 C1 Pt 122.3(5) . . ? C6 C1 Pt 119.5(4) . . ? C1 C2 C3 121.7(6) . . ? C4 C3 C2 119.6(6) . . ? C3 C4 C5 119.8(7) . . ? C4 C5 C6 120.2(7) . . ? C5 C6 C1 120.8(6) . . ? C5 C6 C7 117.2(6) . . ? C1 C6 C7 122.0(6) . . ? C8 C7 C6 172.2(7) . . ? C7 C8 C9 177.0(8) . . ? C10 C9 C14 117.2(7) . . ? C10 C9 C8 121.4(7) . . ? C14 C9 C8 121.4(7) . . ? C11 C10 C9 121.0(8) . . ? C10 C11 C12 120.6(9) . . ? C13 C12 C11 119.0(8) . . ? C14 C13 C12 121.0(9) . . ? C13 C14 C9 121.1(8) . . ? C13 C14 Br1 119.5(7) . . ? C9 C14 Br1 119.4(5) . . ? C16 C15 C20 119.3(6) . . ? C16 C15 P1 123.8(5) . . ? C20 C15 P1 116.9(4) . . ? C15 C16 C17 120.6(6) . . ? C18 C17 C16 120.1(6) . . ? C17 C18 C19 120.2(6) . . ? C18 C19 C20 120.4(6) . . ? C19 C20 C15 119.4(6) . . ? C19 C20 P2 122.8(5) . . ? C15 C20 P2 117.8(4) . . ? C26 C21 C22 120.0(6) . . ? C26 C21 P1 122.5(5) . . ? C22 C21 P1 117.5(5) . . ? C23 C22 C21 119.3(7) . . ? C22 C23 C24 120.6(8) . . ? C25 C24 C23 120.2(7) . . ? C24 C25 C26 120.5(8) . . ? C25 C26 C21 119.4(8) . . ? C28 C27 C32 118.9(6) . . ? C28 C27 P1 119.0(5) . . ? C32 C27 P1 121.5(5) . . ? C27 C28 C29 120.6(6) . . ? C30 C29 C28 119.6(7) . . ? C29 C30 C31 120.5(7) . . ? C32 C31 C30 120.0(7) . . ? C31 C32 C27 120.4(7) . . ? C34 C33 C38 119.1(6) . . ? C34 C33 P2 117.7(5) . . ? C38 C33 P2 123.1(6) . . ? C33 C34 C35 120.0(7) . . ? C36 C35 C34 119.9(8) . . ? C37 C36 C35 121.0(7) . . ? C36 C37 C38 120.1(8) . . ? C37 C38 C33 120.0(8) . . ? C40 C39 C44 118.6(7) . . ? C40 C39 P2 121.7(6) . . ? C44 C39 P2 119.5(5) . . ? C39 C40 C41 118.8(8) . . ? C42 C41 C40 121.6(8) . . ? C43 C42 C41 119.2(8) . . ? C44 C43 C42 120.3(8) . . ? C43 C44 C39 121.4(7) . . ? C4TA O1TA C1TA 110.8(9) . . ? O1TA C1TA C2TA 106.6(8) . . ? C3TA C2TA C1TA 104.8(8) . . ? C4TA C3TA C2TA 107.9(9) . . ? O1TA C4TA C3TA 108.1(9) . . ? C2TB O1TB C3TB 89(2) . . ? C4TB O1TC C1TB 84.3(18) . . ? O1TB C2TB C1TB 123(2) . . ? O1TC C1TB C2TB 118.5(16) . . ? O1TB C3TB C4TB 107(3) . . ? O1TC C4TB C3TB 131(2) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.561 _refine_diff_density_min -1.758 _refine_diff_density_rms 0.167