# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Wolfgang Weigand' _publ_contact_author_email C8WEWO@UNI-JENA.DE _publ_section_title ; Photochemical behavior of (bisphosphane)(?2-tolane)Pt0 complexes in solution and in the solid state. Part A: Experimental considerations ; loop_ _publ_author_name 'Wolfgang Weigand' 'Daniel Escudero' 'Leticia Gonzalez' 'Helmar Gorls' 'Holm Petzold' 'Thomas Weisheit' data_FO3143 _database_code_depnum_ccdc_archive 'CCDC 743160' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C44 H32 Br2 P2 Pt' _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' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.7128(4) _cell_length_b 11.4086(4) _cell_length_c 16.6238(6) _cell_angle_alpha 100.791(2) _cell_angle_beta 96.609(2) _cell_angle_gamma 107.566(2) _cell_volume 1870.52(12) _cell_formula_units_Z 2 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used 11771 _cell_measurement_theta_min 3.15 _cell_measurement_theta_max 27.47 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.04 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.736 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 948 _exptl_absorpt_coefficient_mu 6.003 _exptl_absorpt_correction_type NONE _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 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 11771 _diffrn_reflns_av_R_equivalents 0.0485 _diffrn_reflns_av_sigmaI/netI 0.0563 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.15 _diffrn_reflns_theta_max 27.47 _reflns_number_total 7820 _reflns_number_gt 6807 _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^)+(0.0815P)^2^+1.4693P] 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 7820 _refine_ls_number_parameters 442 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0577 _refine_ls_R_factor_gt 0.0482 _refine_ls_wR_factor_ref 0.1268 _refine_ls_wR_factor_gt 0.1184 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.048 _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 -0.000412(19) 0.007918(18) 0.277066(12) 0.02760(9) Uani 1 1 d . . . Br1 Br 0.43871(9) -0.22540(8) 0.57797(5) 0.0635(2) Uani 1 1 d . . . Br2 Br -0.35213(15) -0.66138(9) -0.01940(8) 0.1094(5) Uani 1 1 d . . . P1 P 0.09888(14) 0.21324(13) 0.34340(9) 0.0285(3) Uani 1 1 d . . . P2 P -0.15106(14) 0.07615(13) 0.21064(9) 0.0283(3) Uani 1 1 d . . . C1 C -0.0179(6) -0.1771(5) 0.2414(4) 0.0322(11) Uani 1 1 d . . . C2 C 0.0821(6) -0.1234(5) 0.3025(4) 0.0327(12) Uani 1 1 d . . . C3 C 0.1732(6) -0.1464(6) 0.3648(4) 0.0331(12) Uani 1 1 d . . . C4 C 0.2518(7) -0.0498(6) 0.4312(4) 0.0435(15) Uani 1 1 d . . . H4A H 0.2515 0.0339 0.4333 0.052 Uiso 1 1 calc R . . C5 C 0.3308(8) -0.0715(7) 0.4947(4) 0.0493(17) Uani 1 1 d . . . H5A H 0.3822 -0.0043 0.5406 0.059 Uiso 1 1 calc R . . C6 C 0.3336(7) -0.1930(7) 0.4903(4) 0.0446(15) Uani 1 1 d . . . C7 C 0.2642(8) -0.2884(7) 0.4241(5) 0.056(2) Uani 1 1 d . . . H7A H 0.2708 -0.3704 0.4206 0.067 Uiso 1 1 calc R . . C8 C 0.1833(8) -0.2667(6) 0.3613(5) 0.0499(17) Uani 1 1 d . . . H8A H 0.1340 -0.3344 0.3153 0.060 Uiso 1 1 calc R . . C9 C -0.0973(6) -0.2950(5) 0.1805(4) 0.0351(12) Uani 1 1 d . . . C10 C -0.2301(7) -0.3143(6) 0.1489(4) 0.0436(15) Uani 1 1 d . . . H10A H -0.2687 -0.2518 0.1678 0.052 Uiso 1 1 calc R . . C11 C -0.3057(8) -0.4226(7) 0.0906(5) 0.0575(19) Uani 1 1 d . . . H11A H -0.3965 -0.4355 0.0700 0.069 Uiso 1 1 calc R . . C12 C -0.2502(10) -0.5110(7) 0.0626(5) 0.064(2) Uani 1 1 d . . . C13 C -0.1177(9) -0.4942(7) 0.0900(5) 0.057(2) Uani 1 1 d . . . H13A H -0.0790 -0.5552 0.0681 0.069 Uiso 1 1 calc R . . C14 C -0.0429(8) -0.3863(7) 0.1503(4) 0.0476(16) Uani 1 1 d . . . H14A H 0.0473 -0.3748 0.1713 0.057 Uiso 1 1 calc R . . C15 C -0.0211(6) 0.2967(5) 0.3326(3) 0.0309(11) Uani 1 1 d . . . C16 C -0.0087(6) 0.4127(6) 0.3822(4) 0.0413(14) Uani 1 1 d . . . H16A H 0.0617 0.4504 0.4289 0.050 Uiso 1 1 calc R . . C17 C -0.0974(7) 0.4744(6) 0.3646(5) 0.0465(15) Uani 1 1 d . . . H17A H -0.0890 0.5531 0.4000 0.056 Uiso 1 1 calc R . . C18 C -0.1985(7) 0.4223(6) 0.2955(4) 0.0429(14) Uani 1 1 d . . . H18A H -0.2575 0.4664 0.2823 0.051 Uiso 1 1 calc R . . C19 C -0.2133(6) 0.3040(6) 0.2450(4) 0.0391(13) Uani 1 1 d . . . H19A H -0.2822 0.2680 0.1972 0.047 Uiso 1 1 calc R . . C20 C -0.1272(6) 0.2393(5) 0.2648(4) 0.0307(11) Uani 1 1 d . . . C21 C 0.1778(6) 0.2644(5) 0.4526(3) 0.0302(11) Uani 1 1 d . . . C22 C 0.1229(7) 0.1945(6) 0.5074(4) 0.0398(13) Uani 1 1 d . . . H22A H 0.0411 0.1266 0.4884 0.048 Uiso 1 1 calc R . . C23 C 0.1865(7) 0.2230(7) 0.5897(4) 0.0462(15) Uani 1 1 d . . . H23A H 0.1479 0.1740 0.6265 0.055 Uiso 1 1 calc R . . C24 C 0.3030(7) 0.3198(7) 0.6182(4) 0.0447(15) Uani 1 1 d . . . H24A H 0.3470 0.3364 0.6741 0.054 Uiso 1 1 calc R . . C25 C 0.3578(7) 0.3943(7) 0.5664(4) 0.0460(15) Uani 1 1 d . . . H25A H 0.4370 0.4648 0.5874 0.055 Uiso 1 1 calc R . . C26 C 0.2963(6) 0.3658(6) 0.4828(4) 0.0411(14) Uani 1 1 d . . . H26A H 0.3352 0.4156 0.4465 0.049 Uiso 1 1 calc R . . C27 C 0.2291(6) 0.2908(5) 0.2899(3) 0.0319(11) Uani 1 1 d . . . C28 C 0.3183(6) 0.2306(6) 0.2689(4) 0.0394(13) Uani 1 1 d . . . H28A H 0.3115 0.1523 0.2832 0.047 Uiso 1 1 calc R . . C29 C 0.4182(7) 0.2830(8) 0.2271(5) 0.0549(18) Uani 1 1 d . . . H29A H 0.4791 0.2402 0.2131 0.066 Uiso 1 1 calc R . . C30 C 0.4299(8) 0.3957(8) 0.2059(5) 0.059(2) Uani 1 1 d . . . H30A H 0.4983 0.4309 0.1771 0.071 Uiso 1 1 calc R . . C31 C 0.3407(9) 0.4584(8) 0.2268(5) 0.064(2) Uani 1 1 d . . . H31A H 0.3486 0.5371 0.2130 0.077 Uiso 1 1 calc R . . C32 C 0.2403(7) 0.4052(7) 0.2679(5) 0.0489(16) Uani 1 1 d . . . H32A H 0.1784 0.4472 0.2813 0.059 Uiso 1 1 calc R . . C33 C -0.1396(6) 0.0829(6) 0.1029(4) 0.0357(12) Uani 1 1 d . . . C34 C -0.0621(8) 0.1927(7) 0.0840(4) 0.0476(16) Uani 1 1 d . . . H34A H -0.0223 0.2681 0.1264 0.057 Uiso 1 1 calc R . . C35 C -0.0437(10) 0.1910(10) 0.0028(5) 0.066(2) Uani 1 1 d . . . H35A H 0.0072 0.2663 -0.0106 0.079 Uiso 1 1 calc R . . C36 C -0.0982(9) 0.0819(10) -0.0585(5) 0.063(2) Uani 1 1 d . . . H36A H -0.0831 0.0817 -0.1138 0.076 Uiso 1 1 calc R . . C37 C -0.1742(8) -0.0268(10) -0.0406(4) 0.060(2) Uani 1 1 d . . . H37A H -0.2134 -0.1016 -0.0836 0.072 Uiso 1 1 calc R . . C38 C -0.1942(7) -0.0280(8) 0.0410(4) 0.0472(16) Uani 1 1 d . . . H38A H -0.2447 -0.1039 0.0539 0.057 Uiso 1 1 calc R . . C39 C -0.3284(6) -0.0023(5) 0.2079(4) 0.0334(12) Uani 1 1 d . . . C40 C -0.4282(7) 0.0028(7) 0.1481(4) 0.0459(15) Uani 1 1 d . . . H40A H -0.4048 0.0436 0.1045 0.055 Uiso 1 1 calc R . . C41 C -0.5602(7) -0.0510(7) 0.1520(5) 0.0530(18) Uani 1 1 d . . . H41A H -0.6273 -0.0478 0.1106 0.064 Uiso 1 1 calc R . . C42 C -0.5959(7) -0.1094(8) 0.2149(5) 0.0558(19) Uani 1 1 d . . . H42A H -0.6871 -0.1452 0.2179 0.067 Uiso 1 1 calc R . . C43 C -0.4973(8) -0.1153(8) 0.2739(5) 0.0562(19) Uani 1 1 d . . . H43A H -0.5213 -0.1565 0.3172 0.067 Uiso 1 1 calc R . . C44 C -0.3632(7) -0.0617(6) 0.2705(4) 0.0429(14) Uani 1 1 d . . . H44A H -0.2963 -0.0663 0.3114 0.051 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 0.03038(13) 0.02728(13) 0.02713(12) 0.00828(8) 0.00249(8) 0.01227(9) Br1 0.0650(5) 0.0692(5) 0.0602(5) 0.0259(4) -0.0127(4) 0.0300(4) Br2 0.1278(10) 0.0534(5) 0.1046(8) -0.0313(5) -0.0523(8) 0.0258(6) P1 0.0282(7) 0.0283(6) 0.0306(7) 0.0085(5) 0.0037(5) 0.0111(5) P2 0.0304(7) 0.0316(7) 0.0265(6) 0.0084(5) 0.0030(5) 0.0154(6) C1 0.037(3) 0.031(3) 0.032(3) 0.009(2) 0.006(2) 0.016(2) C2 0.038(3) 0.030(3) 0.033(3) 0.009(2) 0.008(2) 0.014(2) C3 0.032(3) 0.036(3) 0.037(3) 0.015(2) 0.008(2) 0.015(2) C4 0.052(4) 0.040(3) 0.040(3) 0.009(3) -0.001(3) 0.022(3) C5 0.056(4) 0.047(4) 0.043(4) 0.003(3) -0.007(3) 0.025(3) C6 0.041(3) 0.058(4) 0.040(3) 0.022(3) -0.004(3) 0.024(3) C7 0.061(4) 0.035(3) 0.068(5) 0.017(3) -0.013(4) 0.017(3) C8 0.056(4) 0.035(3) 0.053(4) 0.009(3) -0.014(3) 0.017(3) C9 0.047(3) 0.027(3) 0.029(3) 0.004(2) 0.001(2) 0.014(2) C10 0.047(4) 0.035(3) 0.047(4) 0.010(3) 0.002(3) 0.013(3) C11 0.055(4) 0.045(4) 0.059(4) 0.007(3) -0.009(4) 0.007(3) C12 0.091(6) 0.032(3) 0.051(4) -0.003(3) -0.019(4) 0.015(4) C13 0.086(6) 0.042(4) 0.048(4) 0.004(3) -0.003(4) 0.034(4) C14 0.055(4) 0.044(4) 0.046(4) 0.009(3) 0.006(3) 0.022(3) C15 0.035(3) 0.027(2) 0.033(3) 0.009(2) 0.006(2) 0.012(2) C16 0.040(3) 0.036(3) 0.045(3) 0.002(3) 0.003(3) 0.014(3) C17 0.050(4) 0.038(3) 0.052(4) -0.001(3) 0.006(3) 0.024(3) C18 0.042(3) 0.038(3) 0.055(4) 0.007(3) 0.006(3) 0.025(3) C19 0.039(3) 0.042(3) 0.040(3) 0.010(3) 0.002(3) 0.021(3) C20 0.034(3) 0.030(3) 0.035(3) 0.012(2) 0.010(2) 0.016(2) C21 0.034(3) 0.032(3) 0.029(3) 0.007(2) 0.005(2) 0.018(2) C22 0.044(3) 0.037(3) 0.042(3) 0.012(3) 0.012(3) 0.014(3) C23 0.060(4) 0.054(4) 0.036(3) 0.017(3) 0.015(3) 0.028(3) C24 0.056(4) 0.055(4) 0.027(3) 0.005(3) 0.002(3) 0.030(3) C25 0.042(3) 0.052(4) 0.036(3) 0.003(3) -0.004(3) 0.013(3) C26 0.041(3) 0.044(3) 0.033(3) 0.014(3) 0.000(3) 0.007(3) C27 0.032(3) 0.033(3) 0.028(3) 0.010(2) 0.001(2) 0.008(2) C28 0.036(3) 0.046(3) 0.039(3) 0.011(3) 0.008(2) 0.019(3) C29 0.039(4) 0.073(5) 0.053(4) 0.012(4) 0.016(3) 0.017(3) C30 0.049(4) 0.073(5) 0.054(4) 0.025(4) 0.021(3) 0.007(4) C31 0.073(5) 0.056(4) 0.066(5) 0.036(4) 0.019(4) 0.011(4) C32 0.053(4) 0.047(4) 0.055(4) 0.022(3) 0.017(3) 0.020(3) C33 0.043(3) 0.044(3) 0.032(3) 0.015(2) 0.006(2) 0.027(3) C34 0.063(4) 0.050(4) 0.045(4) 0.021(3) 0.020(3) 0.031(3) C35 0.094(6) 0.090(6) 0.058(5) 0.051(5) 0.047(5) 0.063(5) C36 0.071(5) 0.118(8) 0.037(4) 0.037(4) 0.024(4) 0.068(5) C37 0.056(4) 0.099(6) 0.031(3) 0.007(4) -0.004(3) 0.043(5) C38 0.051(4) 0.066(4) 0.032(3) 0.010(3) 0.002(3) 0.033(3) C39 0.031(3) 0.031(3) 0.039(3) 0.004(2) 0.005(2) 0.014(2) C40 0.043(4) 0.048(4) 0.045(4) 0.004(3) -0.004(3) 0.021(3) C41 0.037(3) 0.051(4) 0.064(5) -0.002(3) -0.010(3) 0.019(3) C42 0.031(3) 0.058(4) 0.066(5) -0.001(4) 0.010(3) 0.006(3) C43 0.050(4) 0.060(4) 0.047(4) 0.006(3) 0.013(3) 0.004(4) C44 0.041(3) 0.046(3) 0.036(3) 0.004(3) 0.004(3) 0.011(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt C1 2.027(6) . ? Pt C2 2.039(6) . ? Pt P1 2.2569(14) . ? Pt P2 2.2583(14) . ? Br1 C6 1.899(6) . ? Br2 C12 1.909(7) . ? P1 C21 1.818(6) . ? P1 C15 1.828(6) . ? P1 C27 1.831(6) . ? P2 C33 1.823(6) . ? P2 C39 1.831(6) . ? P2 C20 1.837(6) . ? C1 C2 1.295(8) . ? C1 C9 1.469(8) . ? C2 C3 1.454(8) . ? C3 C4 1.384(9) . ? C3 C8 1.400(9) . ? C4 C5 1.382(9) . ? C4 H4A 0.9500 . ? C5 C6 1.383(10) . ? C5 H5A 0.9500 . ? C6 C7 1.350(10) . ? C7 C8 1.386(9) . ? C7 H7A 0.9500 . ? C8 H8A 0.9500 . ? C9 C14 1.383(9) . ? C9 C10 1.395(9) . ? C10 C11 1.375(10) . ? C10 H10A 0.9500 . ? C11 C12 1.355(12) . ? C11 H11A 0.9500 . ? C12 C13 1.384(13) . ? C13 C14 1.386(10) . ? C13 H13A 0.9500 . ? C14 H14A 0.9500 . ? C15 C16 1.381(8) . ? C15 C20 1.403(8) . ? C16 C17 1.378(9) . ? C16 H16A 0.9500 . ? C17 C18 1.384(10) . ? C17 H17A 0.9500 . ? C18 C19 1.402(9) . ? C18 H18A 0.9500 . ? C19 C20 1.392(8) . ? C19 H19A 0.9500 . ? C21 C22 1.386(8) . ? C21 C26 1.397(8) . ? C22 C23 1.389(9) . ? C22 H22A 0.9500 . ? C23 C24 1.356(10) . ? C23 H23A 0.9500 . ? C24 C25 1.377(10) . ? C24 H24A 0.9500 . ? C25 C26 1.402(8) . ? C25 H25A 0.9500 . ? C26 H26A 0.9500 . ? C27 C28 1.375(9) . ? C27 C32 1.395(9) . ? C28 C29 1.388(10) . ? C28 H28A 0.9500 . ? C29 C30 1.370(12) . ? C29 H29A 0.9500 . ? C30 C31 1.393(13) . ? C30 H30A 0.9500 . ? C31 C32 1.387(11) . ? C31 H31A 0.9500 . ? C32 H32A 0.9500 . ? C33 C38 1.389(10) . ? C33 C34 1.392(10) . ? C34 C35 1.384(10) . ? C34 H34A 0.9500 . ? C35 C36 1.370(14) . ? C35 H35A 0.9500 . ? C36 C37 1.369(13) . ? C36 H36A 0.9500 . ? C37 C38 1.400(10) . ? C37 H37A 0.9500 . ? C38 H38A 0.9500 . ? C39 C44 1.372(9) . ? C39 C40 1.396(9) . ? C40 C41 1.376(10) . ? C40 H40A 0.9500 . ? C41 C42 1.372(12) . ? C41 H41A 0.9500 . ? C42 C43 1.382(12) . ? C42 H42A 0.9500 . ? C43 C44 1.393(10) . ? C43 H43A 0.9500 . ? C44 H44A 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Pt C2 37.1(2) . . ? C1 Pt P1 156.50(17) . . ? C2 Pt P1 119.81(17) . . ? C1 Pt P2 118.07(17) . . ? C2 Pt P2 155.17(17) . . ? P1 Pt P2 85.00(5) . . ? C21 P1 C15 105.5(3) . . ? C21 P1 C27 103.9(3) . . ? C15 P1 C27 103.2(3) . . ? C21 P1 Pt 123.06(19) . . ? C15 P1 Pt 108.89(18) . . ? C27 P1 Pt 110.47(19) . . ? C33 P2 C39 104.5(3) . . ? C33 P2 C20 104.9(3) . . ? C39 P2 C20 101.8(3) . . ? C33 P2 Pt 116.0(2) . . ? C39 P2 Pt 119.0(2) . . ? C20 P2 Pt 108.87(18) . . ? C2 C1 C9 145.9(6) . . ? C2 C1 Pt 71.9(3) . . ? C9 C1 Pt 142.2(4) . . ? C1 C2 C3 144.4(6) . . ? C1 C2 Pt 70.9(4) . . ? C3 C2 Pt 142.8(4) . . ? C4 C3 C8 117.1(6) . . ? C4 C3 C2 120.9(6) . . ? C8 C3 C2 121.9(5) . . ? C5 C4 C3 121.9(6) . . ? C5 C4 H4A 119.0 . . ? C3 C4 H4A 119.0 . . ? C4 C5 C6 118.8(6) . . ? C4 C5 H5A 120.6 . . ? C6 C5 H5A 120.6 . . ? C7 C6 C5 121.0(6) . . ? C7 C6 Br1 119.5(5) . . ? C5 C6 Br1 119.4(5) . . ? C6 C7 C8 119.9(6) . . ? C6 C7 H7A 120.1 . . ? C8 C7 H7A 120.1 . . ? C7 C8 C3 121.0(6) . . ? C7 C8 H8A 119.5 . . ? C3 C8 H8A 119.5 . . ? C14 C9 C10 118.3(6) . . ? C14 C9 C1 122.0(6) . . ? C10 C9 C1 119.6(6) . . ? C11 C10 C9 120.7(7) . . ? C11 C10 H10A 119.6 . . ? C9 C10 H10A 119.6 . . ? C12 C11 C10 119.7(8) . . ? C12 C11 H11A 120.1 . . ? C10 C11 H11A 120.1 . . ? C11 C12 C13 121.6(7) . . ? C11 C12 Br2 120.6(7) . . ? C13 C12 Br2 117.7(6) . . ? C12 C13 C14 118.3(7) . . ? C12 C13 H13A 120.8 . . ? C14 C13 H13A 120.8 . . ? C9 C14 C13 121.2(7) . . ? C9 C14 H14A 119.4 . . ? C13 C14 H14A 119.4 . . ? C16 C15 C20 119.7(5) . . ? C16 C15 P1 124.7(5) . . ? C20 C15 P1 115.4(4) . . ? C17 C16 C15 120.7(6) . . ? C17 C16 H16A 119.6 . . ? C15 C16 H16A 119.6 . . ? C16 C17 C18 120.3(6) . . ? C16 C17 H17A 119.8 . . ? C18 C17 H17A 119.8 . . ? C17 C18 C19 119.7(6) . . ? C17 C18 H18A 120.2 . . ? C19 C18 H18A 120.2 . . ? C20 C19 C18 120.0(6) . . ? C20 C19 H19A 120.0 . . ? C18 C19 H19A 120.0 . . ? C19 C20 C15 119.4(5) . . ? C19 C20 P2 123.2(5) . . ? C15 C20 P2 117.3(4) . . ? C22 C21 C26 118.5(5) . . ? C22 C21 P1 118.5(5) . . ? C26 C21 P1 122.9(5) . . ? C21 C22 C23 120.5(6) . . ? C21 C22 H22A 119.7 . . ? C23 C22 H22A 119.7 . . ? C24 C23 C22 120.7(6) . . ? C24 C23 H23A 119.7 . . ? C22 C23 H23A 119.7 . . ? C23 C24 C25 120.4(6) . . ? C23 C24 H24A 119.8 . . ? C25 C24 H24A 119.8 . . ? C24 C25 C26 119.7(6) . . ? C24 C25 H25A 120.1 . . ? C26 C25 H25A 120.1 . . ? C21 C26 C25 120.1(6) . . ? C21 C26 H26A 119.9 . . ? C25 C26 H26A 119.9 . . ? C28 C27 C32 118.8(6) . . ? C28 C27 P1 117.6(5) . . ? C32 C27 P1 123.6(5) . . ? C27 C28 C29 120.7(7) . . ? C27 C28 H28A 119.7 . . ? C29 C28 H28A 119.7 . . ? C30 C29 C28 120.7(7) . . ? C30 C29 H29A 119.7 . . ? C28 C29 H29A 119.7 . . ? C29 C30 C31 119.5(7) . . ? C29 C30 H30A 120.2 . . ? C31 C30 H30A 120.2 . . ? C32 C31 C30 119.6(8) . . ? C32 C31 H31A 120.2 . . ? C30 C31 H31A 120.2 . . ? C31 C32 C27 120.7(7) . . ? C31 C32 H32A 119.6 . . ? C27 C32 H32A 119.6 . . ? C38 C33 C34 119.9(6) . . ? C38 C33 P2 118.8(5) . . ? C34 C33 P2 120.7(5) . . ? C35 C34 C33 119.4(8) . . ? C35 C34 H34A 120.3 . . ? C33 C34 H34A 120.3 . . ? C36 C35 C34 120.8(8) . . ? C36 C35 H35A 119.6 . . ? C34 C35 H35A 119.6 . . ? C37 C36 C35 120.3(7) . . ? C37 C36 H36A 119.8 . . ? C35 C36 H36A 119.8 . . ? C36 C37 C38 120.2(8) . . ? C36 C37 H37A 119.9 . . ? C38 C37 H37A 119.9 . . ? C33 C38 C37 119.4(8) . . ? C33 C38 H38A 120.3 . . ? C37 C38 H38A 120.3 . . ? C44 C39 C40 119.4(6) . . ? C44 C39 P2 117.8(5) . . ? C40 C39 P2 122.7(5) . . ? C41 C40 C39 120.4(7) . . ? C41 C40 H40A 119.8 . . ? C39 C40 H40A 119.8 . . ? C42 C41 C40 120.6(7) . . ? C42 C41 H41A 119.7 . . ? C40 C41 H41A 119.7 . . ? C41 C42 C43 119.1(7) . . ? C41 C42 H42A 120.4 . . ? C43 C42 H42A 120.4 . . ? C42 C43 C44 120.8(7) . . ? C42 C43 H43A 119.6 . . ? C44 C43 H43A 119.6 . . ? C39 C44 C43 119.7(7) . . ? C39 C44 H44A 120.2 . . ? C43 C44 H44A 120.2 . . ? _diffrn_measured_fraction_theta_max 0.914 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.914 _refine_diff_density_max 1.396 _refine_diff_density_min -1.646 _refine_diff_density_rms 0.185 data_FO3398 _database_code_depnum_ccdc_archive 'CCDC 743161' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C46 H36 Br2 P2 Pt' _chemical_formula_sum 'C46 H36 Br2 P2 Pt' _chemical_formula_weight 1005.60 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 orthorhombic _symmetry_space_group_name_H-M 'P b c a' _symmetry_space_group_name_Hall '-P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 20.5293(3) _cell_length_b 16.4027(2) _cell_length_c 23.2611(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7832.85(18) _cell_formula_units_Z 8 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used 48171 _cell_measurement_theta_min 2.65 _cell_measurement_theta_max 27.45 _exptl_crystal_description prism _exptl_crystal_colour 'light yellow' _exptl_crystal_size_max 0.04 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.705 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3920 _exptl_absorpt_coefficient_mu 5.737 _exptl_absorpt_correction_type NONE _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 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 48171 _diffrn_reflns_av_R_equivalents 0.0822 _diffrn_reflns_av_sigmaI/netI 0.0490 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 2.65 _diffrn_reflns_theta_max 27.45 _reflns_number_total 8934 _reflns_number_gt 6750 _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^)+(0.0268P)^2^+18.7354P] 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 8934 _refine_ls_number_parameters 462 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0606 _refine_ls_R_factor_gt 0.0349 _refine_ls_wR_factor_ref 0.0775 _refine_ls_wR_factor_gt 0.0702 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.036 _refine_ls_shift/su_max 0.007 _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 0.759962(8) 0.123049(9) 0.032336(6) 0.01501(5) Uani 1 1 d . . . Br1 Br 0.94128(3) 0.31128(3) -0.21602(2) 0.04274(15) Uani 1 1 d . . . Br2 Br 1.01266(3) -0.05141(4) 0.24890(2) 0.05186(17) Uani 1 1 d . . . P1 P 0.68070(5) 0.15709(7) -0.03000(5) 0.0182(2) Uani 1 1 d . . . P2 P 0.67995(5) 0.07829(6) 0.09019(4) 0.0165(2) Uani 1 1 d . . . C1 C 0.8555(2) 0.1127(2) 0.05702(19) 0.0190(9) Uani 1 1 d . . . C2 C 0.8527(2) 0.1536(3) 0.00910(18) 0.0184(9) Uani 1 1 d . . . C3 C 0.8818(2) 0.1944(3) -0.04008(17) 0.0206(9) Uani 1 1 d . . . C4 C 0.8492(2) 0.2623(3) -0.06282(19) 0.0261(10) Uani 1 1 d . . . H4A H 0.8134 0.2844 -0.0422 0.031 Uiso 1 1 calc R . . C5 C 0.8672(2) 0.2983(3) -0.11391(19) 0.0265(11) Uani 1 1 d . . . H5A H 0.8443 0.3442 -0.1285 0.032 Uiso 1 1 calc R . . C6 C 0.9190(2) 0.2660(3) -0.14309(19) 0.0274(11) Uani 1 1 d . . . C7 C 0.9538(2) 0.2001(3) -0.12164(19) 0.0278(11) Uani 1 1 d . . . H7A H 0.9901 0.1797 -0.1425 0.033 Uiso 1 1 calc R . . C8 C 0.9361(2) 0.1637(3) -0.06981(18) 0.0229(10) Uani 1 1 d . . . C9 C 0.8945(2) 0.0780(3) 0.10309(18) 0.0194(9) Uani 1 1 d . . . C10 C 0.8704(2) 0.0082(3) 0.13112(18) 0.0244(10) Uani 1 1 d . . . H10A H 0.8294 -0.0134 0.1199 0.029 Uiso 1 1 calc R . . C11 C 0.9048(3) -0.0301(3) 0.17461(19) 0.0305(11) Uani 1 1 d . . . H11A H 0.8879 -0.0771 0.1932 0.037 Uiso 1 1 calc R . . C12 C 0.9635(2) 0.0016(3) 0.18987(19) 0.0280(11) Uani 1 1 d . . . C13 C 0.9887(2) 0.0714(3) 0.16529(19) 0.0288(11) Uani 1 1 d . . . H13A H 1.0291 0.0929 0.1782 0.035 Uiso 1 1 calc R . . C14 C 0.9540(2) 0.1101(3) 0.12107(19) 0.0248(10) Uani 1 1 d . . . C15 C 0.9816(2) 0.1870(3) 0.0961(2) 0.0365(12) Uani 1 1 d . . . H15A H 0.9703 0.1903 0.0552 0.055 Uiso 1 1 calc R . . H15B H 1.0292 0.1866 0.1002 0.055 Uiso 1 1 calc R . . H15C H 0.9636 0.2341 0.1164 0.055 Uiso 1 1 calc R . . C16 C 0.9735(2) 0.0907(3) -0.0480(2) 0.0325(12) Uani 1 1 d . . . H16A H 1.0202 0.1033 -0.0475 0.049 Uiso 1 1 calc R . . H16B H 0.9656 0.0440 -0.0733 0.049 Uiso 1 1 calc R . . H16C H 0.9590 0.0774 -0.0090 0.049 Uiso 1 1 calc R . . C17 C 0.6015(2) 0.1282(2) -0.00024(19) 0.0211(9) Uani 1 1 d . . . C18 C 0.5428(2) 0.1438(3) -0.0273(2) 0.0306(11) Uani 1 1 d . . . H18A H 0.5427 0.1707 -0.0635 0.037 Uiso 1 1 calc R . . C19 C 0.4842(2) 0.1213(3) -0.0029(3) 0.0366(13) Uani 1 1 d . . . H19A H 0.4442 0.1329 -0.0218 0.044 Uiso 1 1 calc R . . C20 C 0.4845(2) 0.0817(3) 0.0493(2) 0.0343(12) Uani 1 1 d . . . H20A H 0.4445 0.0648 0.0660 0.041 Uiso 1 1 calc R . . C21 C 0.5424(2) 0.0663(3) 0.0777(2) 0.0263(10) Uani 1 1 d . . . H21A H 0.5418 0.0397 0.1140 0.032 Uiso 1 1 calc R . . C22 C 0.6014(2) 0.0898(3) 0.05341(18) 0.0202(9) Uani 1 1 d . . . C23 C 0.6688(2) 0.2646(3) -0.04720(18) 0.0200(9) Uani 1 1 d . . . C24 C 0.6533(3) 0.3175(3) -0.0033(2) 0.0319(12) Uani 1 1 d . . . H24A H 0.6454 0.2965 0.0342 0.038 Uiso 1 1 calc R . . C25 C 0.6492(3) 0.4004(3) -0.0127(2) 0.0384(13) Uani 1 1 d . . . H25A H 0.6378 0.4360 0.0179 0.046 Uiso 1 1 calc R . . C26 C 0.6614(3) 0.4313(3) -0.0663(2) 0.0380(13) Uani 1 1 d . . . H26A H 0.6593 0.4884 -0.0728 0.046 Uiso 1 1 calc R . . C27 C 0.6764(3) 0.3803(3) -0.1102(2) 0.0481(16) Uani 1 1 d . . . H27A H 0.6845 0.4019 -0.1475 0.058 Uiso 1 1 calc R . . C28 C 0.6801(3) 0.2974(3) -0.1011(2) 0.0402(14) Uani 1 1 d . . . H28A H 0.6905 0.2623 -0.1323 0.048 Uiso 1 1 calc R . . C29 C 0.6883(2) 0.1060(2) -0.09989(19) 0.0233(10) Uani 1 1 d . . . C30 C 0.7491(2) 0.1083(3) -0.1259(2) 0.0320(13) Uani 1 1 d . . . H30A H 0.7835 0.1367 -0.1073 0.038 Uiso 1 1 calc R . . C31 C 0.7612(3) 0.0708(3) -0.1776(2) 0.0398(13) Uani 1 1 d . . . H31A H 0.8030 0.0742 -0.1950 0.048 Uiso 1 1 calc R . . C32 C 0.7115(3) 0.0280(3) -0.2040(2) 0.0489(16) Uani 1 1 d . . . H32A H 0.7191 0.0017 -0.2397 0.059 Uiso 1 1 calc R . . C33 C 0.6512(3) 0.0235(3) -0.1789(2) 0.0477(15) Uani 1 1 d . . . H33A H 0.6176 -0.0071 -0.1969 0.057 Uiso 1 1 calc R . . C34 C 0.6390(3) 0.0634(3) -0.1271(2) 0.0359(12) Uani 1 1 d . . . H34A H 0.5968 0.0613 -0.1105 0.043 Uiso 1 1 calc R . . C35 C 0.6775(2) -0.0275(2) 0.11448(18) 0.0193(9) Uani 1 1 d . . . C36 C 0.6995(2) -0.0861(3) 0.0764(2) 0.0318(12) Uani 1 1 d . . . H36A H 0.7165 -0.0700 0.0401 0.038 Uiso 1 1 calc R . . C37 C 0.6969(3) -0.1677(3) 0.0907(2) 0.0413(14) Uani 1 1 d . . . H37A H 0.7126 -0.2075 0.0645 0.050 Uiso 1 1 calc R . . C38 C 0.6716(3) -0.1914(3) 0.1428(2) 0.0363(12) Uani 1 1 d . . . H38A H 0.6688 -0.2477 0.1520 0.044 Uiso 1 1 calc R . . C39 C 0.6504(3) -0.1341(3) 0.1817(2) 0.0405(14) Uani 1 1 d . . . H39A H 0.6332 -0.1506 0.2178 0.049 Uiso 1 1 calc R . . C40 C 0.6543(3) -0.0517(3) 0.1677(2) 0.0337(12) Uani 1 1 d . . . H40A H 0.6409 -0.0118 0.1949 0.040 Uiso 1 1 calc R . . C41 C 0.6720(2) 0.1407(2) 0.15488(18) 0.0208(10) Uani 1 1 d . . . C42 C 0.6190(3) 0.1902(3) 0.1666(2) 0.0327(12) Uani 1 1 d . . . H42A H 0.5817 0.1876 0.1426 0.039 Uiso 1 1 calc R . . C43 C 0.6198(3) 0.2434(3) 0.2129(2) 0.0427(14) Uani 1 1 d . . . H43A H 0.5828 0.2764 0.2207 0.051 Uiso 1 1 calc R . . C44 C 0.6736(3) 0.2484(3) 0.2475(2) 0.0408(14) Uani 1 1 d . . . H44A H 0.6746 0.2866 0.2782 0.049 Uiso 1 1 calc R . . C45 C 0.7261(3) 0.1985(3) 0.2378(2) 0.0411(14) Uani 1 1 d . . . H45A H 0.7629 0.2006 0.2626 0.049 Uiso 1 1 calc R . . C46 C 0.7253(3) 0.1444(3) 0.1913(2) 0.0321(12) Uani 1 1 d . . . H46A H 0.7617 0.1098 0.1845 0.038 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 0.01673(8) 0.01324(8) 0.01504(8) 0.00173(7) 0.00131(6) 0.00010(7) Br1 0.0568(4) 0.0458(3) 0.0256(3) 0.0139(2) 0.0102(2) -0.0063(3) Br2 0.0626(4) 0.0524(4) 0.0405(3) 0.0058(3) -0.0245(3) 0.0164(3) P1 0.0217(6) 0.0148(5) 0.0179(5) 0.0017(5) -0.0020(5) 0.0011(5) P2 0.0195(6) 0.0132(5) 0.0168(5) 0.0018(4) 0.0025(4) -0.0006(4) C1 0.014(2) 0.017(2) 0.026(2) 0.0011(18) -0.0032(18) 0.0003(18) C2 0.012(2) 0.018(2) 0.026(2) -0.0042(18) 0.0038(18) -0.0024(18) C3 0.021(2) 0.021(2) 0.020(2) 0.0023(18) 0.0024(18) -0.0061(19) C4 0.021(2) 0.026(3) 0.032(3) 0.007(2) 0.007(2) 0.001(2) C5 0.026(3) 0.027(3) 0.027(2) 0.010(2) -0.005(2) -0.004(2) C6 0.034(3) 0.028(3) 0.021(2) 0.007(2) 0.003(2) -0.008(2) C7 0.030(3) 0.031(3) 0.022(2) 0.000(2) 0.007(2) -0.007(2) C8 0.023(2) 0.023(2) 0.023(2) 0.0000(19) 0.0001(19) -0.004(2) C9 0.020(2) 0.017(2) 0.021(2) -0.0019(18) 0.0010(18) 0.0021(18) C10 0.027(3) 0.022(2) 0.024(2) 0.0030(19) 0.000(2) 0.004(2) C11 0.045(3) 0.025(3) 0.022(2) 0.003(2) 0.003(2) 0.002(2) C12 0.033(3) 0.027(3) 0.024(2) -0.003(2) -0.006(2) 0.012(2) C13 0.029(3) 0.029(3) 0.028(3) -0.009(2) -0.006(2) 0.000(2) C14 0.027(3) 0.023(2) 0.024(2) -0.0014(19) 0.000(2) 0.003(2) C15 0.033(3) 0.034(3) 0.042(3) 0.004(2) 0.001(2) -0.010(2) C16 0.031(3) 0.031(3) 0.035(3) 0.003(2) 0.008(2) 0.010(2) C17 0.024(2) 0.010(2) 0.029(2) -0.0010(18) -0.0026(19) -0.0017(19) C18 0.027(3) 0.020(2) 0.044(3) 0.005(2) -0.010(2) 0.001(2) C19 0.020(3) 0.028(3) 0.062(4) -0.003(3) -0.008(2) 0.007(2) C20 0.020(3) 0.025(3) 0.057(3) -0.004(2) 0.011(2) -0.001(2) C21 0.021(2) 0.019(2) 0.039(3) -0.003(2) 0.004(2) -0.001(2) C22 0.023(2) 0.011(2) 0.027(2) -0.0018(18) 0.0026(19) -0.0022(18) C23 0.022(2) 0.015(2) 0.023(2) 0.0000(17) -0.0027(18) -0.0032(18) C24 0.049(3) 0.022(2) 0.025(2) 0.000(2) 0.000(2) 0.003(2) C25 0.059(4) 0.018(2) 0.039(3) -0.007(2) 0.005(3) 0.000(2) C26 0.045(3) 0.011(2) 0.059(4) 0.004(2) 0.011(3) 0.002(2) C27 0.079(5) 0.027(3) 0.039(3) 0.017(2) 0.020(3) 0.014(3) C28 0.070(4) 0.023(3) 0.028(3) 0.002(2) 0.011(3) 0.012(3) C29 0.037(3) 0.011(2) 0.023(2) 0.0012(17) -0.006(2) 0.0011(19) C30 0.041(3) 0.034(3) 0.021(2) -0.011(2) -0.006(2) 0.010(2) C31 0.052(3) 0.039(3) 0.028(3) -0.006(2) -0.003(3) 0.018(3) C32 0.086(5) 0.036(3) 0.025(3) -0.005(2) -0.009(3) 0.016(3) C33 0.070(4) 0.040(3) 0.033(3) -0.006(3) -0.018(3) -0.008(3) C34 0.049(3) 0.030(3) 0.028(3) 0.000(2) -0.006(2) -0.013(3) C35 0.020(2) 0.014(2) 0.024(2) -0.0011(17) 0.0017(18) 0.0009(18) C36 0.046(3) 0.023(3) 0.026(3) -0.002(2) 0.009(2) 0.000(2) C37 0.062(4) 0.020(3) 0.042(3) -0.007(2) 0.004(3) 0.006(3) C38 0.046(3) 0.014(2) 0.048(3) 0.008(2) -0.006(3) 0.001(2) C39 0.060(4) 0.023(3) 0.038(3) 0.012(2) 0.009(3) -0.003(3) C40 0.047(3) 0.021(3) 0.033(3) 0.004(2) 0.014(2) 0.000(2) C41 0.032(3) 0.011(2) 0.019(2) 0.0037(16) 0.0042(19) -0.0060(18) C42 0.037(3) 0.025(3) 0.036(3) -0.009(2) 0.002(2) 0.006(2) C43 0.059(4) 0.029(3) 0.041(3) -0.014(2) 0.004(3) 0.012(3) C44 0.064(4) 0.028(3) 0.030(3) -0.010(2) 0.003(3) -0.001(3) C45 0.052(4) 0.046(3) 0.025(3) -0.002(2) -0.013(2) -0.006(3) C46 0.034(3) 0.033(3) 0.028(3) 0.001(2) -0.001(2) 0.003(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 Pt C2 2.041(4) . ? Pt C1 2.050(4) . ? Pt P2 2.2467(11) . ? Pt P1 2.2499(11) . ? Br1 C6 1.908(4) . ? Br2 C12 1.914(4) . ? P1 C23 1.824(4) . ? P1 C17 1.830(5) . ? P1 C29 1.835(4) . ? P2 C35 1.826(4) . ? P2 C41 1.828(4) . ? P2 C22 1.835(4) . ? C1 C2 1.302(6) . ? C1 C9 1.454(6) . ? C2 C3 1.454(6) . ? C3 C4 1.403(6) . ? C3 C8 1.405(6) . ? C4 C5 1.377(6) . ? C4 H4A 0.9500 . ? C5 C6 1.369(6) . ? C5 H5A 0.9500 . ? C6 C7 1.388(6) . ? C7 C8 1.394(6) . ? C7 H7A 0.9500 . ? C8 C16 1.511(6) . ? C9 C14 1.396(6) . ? C9 C10 1.407(6) . ? C10 C11 1.384(6) . ? C10 H10A 0.9500 . ? C11 C12 1.358(7) . ? C11 H11A 0.9500 . ? C12 C13 1.380(7) . ? C13 C14 1.403(6) . ? C13 H13A 0.9500 . ? C14 C15 1.500(6) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C18 1.383(6) . ? C17 C22 1.398(6) . ? C18 C19 1.380(7) . ? C18 H18A 0.9500 . ? C19 C20 1.376(7) . ? C19 H19A 0.9500 . ? C20 C21 1.383(7) . ? C20 H20A 0.9500 . ? C21 C22 1.392(6) . ? C21 H21A 0.9500 . ? C23 C24 1.378(6) . ? C23 C28 1.385(6) . ? C24 C25 1.381(7) . ? C24 H24A 0.9500 . ? C25 C26 1.370(7) . ? C25 H25A 0.9500 . ? C26 C27 1.355(7) . ? C26 H26A 0.9500 . ? C27 C28 1.378(6) . ? C27 H27A 0.9500 . ? C28 H28A 0.9500 . ? C29 C34 1.384(6) . ? C29 C30 1.387(7) . ? C30 C31 1.375(7) . ? C30 H30A 0.9500 . ? C31 C32 1.382(8) . ? C31 H31A 0.9500 . ? C32 C33 1.369(8) . ? C32 H32A 0.9500 . ? C33 C34 1.395(7) . ? C33 H33A 0.9500 . ? C34 H34A 0.9500 . ? C35 C36 1.383(6) . ? C35 C40 1.385(6) . ? C36 C37 1.381(7) . ? C36 H36A 0.9500 . ? C37 C38 1.376(7) . ? C37 H37A 0.9500 . ? C38 C39 1.376(7) . ? C38 H38A 0.9500 . ? C39 C40 1.393(6) . ? C39 H39A 0.9500 . ? C40 H40A 0.9500 . ? C41 C42 1.383(6) . ? C41 C46 1.385(7) . ? C42 C43 1.386(6) . ? C42 H42A 0.9500 . ? C43 C44 1.370(8) . ? C43 H43A 0.9500 . ? C44 C45 1.373(7) . ? C44 H44A 0.9500 . ? C45 C46 1.401(7) . ? C45 H45A 0.9500 . ? C46 H46A 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 Pt C1 37.11(17) . . ? C2 Pt P2 157.01(13) . . ? C1 Pt P2 120.29(12) . . ? C2 Pt P1 116.29(13) . . ? C1 Pt P1 153.22(12) . . ? P2 Pt P1 86.47(4) . . ? C23 P1 C17 102.33(19) . . ? C23 P1 C29 104.95(19) . . ? C17 P1 C29 107.0(2) . . ? C23 P1 Pt 118.58(14) . . ? C17 P1 Pt 109.56(15) . . ? C29 P1 Pt 113.33(15) . . ? C35 P2 C41 105.98(18) . . ? C35 P2 C22 102.58(19) . . ? C41 P2 C22 104.3(2) . . ? C35 P2 Pt 121.05(14) . . ? C41 P2 Pt 112.07(14) . . ? C22 P2 Pt 109.24(14) . . ? C2 C1 C9 149.0(4) . . ? C2 C1 Pt 71.1(3) . . ? C9 C1 Pt 140.0(3) . . ? C1 C2 C3 153.2(4) . . ? C1 C2 Pt 71.8(3) . . ? C3 C2 Pt 134.8(3) . . ? C4 C3 C8 118.5(4) . . ? C4 C3 C2 117.9(4) . . ? C8 C3 C2 123.2(4) . . ? C5 C4 C3 122.6(4) . . ? C5 C4 H4A 118.7 . . ? C3 C4 H4A 118.7 . . ? C6 C5 C4 118.0(4) . . ? C6 C5 H5A 121.0 . . ? C4 C5 H5A 121.0 . . ? C5 C6 C7 121.6(4) . . ? C5 C6 Br1 118.4(3) . . ? C7 C6 Br1 120.0(3) . . ? C6 C7 C8 120.7(4) . . ? C6 C7 H7A 119.7 . . ? C8 C7 H7A 119.7 . . ? C7 C8 C3 118.6(4) . . ? C7 C8 C16 119.8(4) . . ? C3 C8 C16 121.5(4) . . ? C14 C9 C10 118.4(4) . . ? C14 C9 C1 123.7(4) . . ? C10 C9 C1 117.9(4) . . ? C11 C10 C9 121.9(4) . . ? C11 C10 H10A 119.0 . . ? C9 C10 H10A 119.0 . . ? C12 C11 C10 118.0(4) . . ? C12 C11 H11A 121.0 . . ? C10 C11 H11A 121.0 . . ? C11 C12 C13 122.8(4) . . ? C11 C12 Br2 118.8(4) . . ? C13 C12 Br2 118.4(4) . . ? C12 C13 C14 119.2(4) . . ? C12 C13 H13A 120.4 . . ? C14 C13 H13A 120.4 . . ? C9 C14 C13 119.6(4) . . ? C9 C14 C15 122.2(4) . . ? C13 C14 C15 118.2(4) . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C8 C16 H16A 109.5 . . ? C8 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C8 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C18 C17 C22 119.3(4) . . ? C18 C17 P1 123.7(4) . . ? C22 C17 P1 117.0(3) . . ? C19 C18 C17 121.5(5) . . ? C19 C18 H18A 119.3 . . ? C17 C18 H18A 119.3 . . ? C20 C19 C18 119.0(5) . . ? C20 C19 H19A 120.5 . . ? C18 C19 H19A 120.5 . . ? C19 C20 C21 120.8(5) . . ? C19 C20 H20A 119.6 . . ? C21 C20 H20A 119.6 . . ? C20 C21 C22 120.2(4) . . ? C20 C21 H21A 119.9 . . ? C22 C21 H21A 119.9 . . ? C21 C22 C17 119.2(4) . . ? C21 C22 P2 123.2(3) . . ? C17 C22 P2 117.5(3) . . ? C24 C23 C28 117.7(4) . . ? C24 C23 P1 118.5(3) . . ? C28 C23 P1 123.5(3) . . ? C23 C24 C25 121.1(4) . . ? C23 C24 H24A 119.4 . . ? C25 C24 H24A 119.4 . . ? C26 C25 C24 119.8(5) . . ? C26 C25 H25A 120.1 . . ? C24 C25 H25A 120.1 . . ? C27 C26 C25 120.0(4) . . ? C27 C26 H26A 120.0 . . ? C25 C26 H26A 120.0 . . ? C26 C27 C28 120.3(5) . . ? C26 C27 H27A 119.8 . . ? C28 C27 H27A 119.8 . . ? C27 C28 C23 120.9(5) . . ? C27 C28 H28A 119.5 . . ? C23 C28 H28A 119.5 . . ? C34 C29 C30 118.2(4) . . ? C34 C29 P1 125.0(4) . . ? C30 C29 P1 116.8(3) . . ? C31 C30 C29 122.1(5) . . ? C31 C30 H30A 118.9 . . ? C29 C30 H30A 118.9 . . ? C30 C31 C32 118.9(5) . . ? C30 C31 H31A 120.6 . . ? C32 C31 H31A 120.6 . . ? C33 C32 C31 120.4(5) . . ? C33 C32 H32A 119.8 . . ? C31 C32 H32A 119.8 . . ? C32 C33 C34 120.3(5) . . ? C32 C33 H33A 119.8 . . ? C34 C33 H33A 119.8 . . ? C29 C34 C33 120.1(5) . . ? C29 C34 H34A 120.0 . . ? C33 C34 H34A 120.0 . . ? C36 C35 C40 119.2(4) . . ? C36 C35 P2 116.9(3) . . ? C40 C35 P2 123.9(3) . . ? C37 C36 C35 120.4(4) . . ? C37 C36 H36A 119.8 . . ? C35 C36 H36A 119.8 . . ? C38 C37 C36 120.1(5) . . ? C38 C37 H37A 119.9 . . ? C36 C37 H37A 119.9 . . ? C37 C38 C39 120.4(4) . . ? C37 C38 H38A 119.8 . . ? C39 C38 H38A 119.8 . . ? C38 C39 C40 119.5(5) . . ? C38 C39 H39A 120.3 . . ? C40 C39 H39A 120.3 . . ? C35 C40 C39 120.4(4) . . ? C35 C40 H40A 119.8 . . ? C39 C40 H40A 119.8 . . ? C42 C41 C46 118.3(4) . . ? C42 C41 P2 124.2(4) . . ? C46 C41 P2 117.1(4) . . ? C41 C42 C43 121.0(5) . . ? C41 C42 H42A 119.5 . . ? C43 C42 H42A 119.5 . . ? C44 C43 C42 120.2(5) . . ? C44 C43 H43A 119.9 . . ? C42 C43 H43A 119.9 . . ? C43 C44 C45 120.1(5) . . ? C43 C44 H44A 120.0 . . ? C45 C44 H44A 120.0 . . ? C44 C45 C46 119.7(5) . . ? C44 C45 H45A 120.2 . . ? C46 C45 H45A 120.2 . . ? C41 C46 C45 120.6(5) . . ? C41 C46 H46A 119.7 . . ? C45 C46 H46A 119.7 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.45 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.298 _refine_diff_density_min -1.458 _refine_diff_density_rms 0.263 data_FO3380 _database_code_depnum_ccdc_archive 'CCDC 743162' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C46 H38 P2 Pt' _chemical_formula_sum 'C46 H38 P2 Pt' _chemical_formula_weight 847.79 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.1682(5) _cell_length_b 12.2745(5) _cell_length_c 15.0911(7) _cell_angle_alpha 79.550(2) _cell_angle_beta 69.759(2) _cell_angle_gamma 69.043(2) _cell_volume 1808.67(14) _cell_formula_units_Z 2 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used 12759 _cell_measurement_theta_min 2.85 _cell_measurement_theta_max 27.48 _exptl_crystal_description prism _exptl_crystal_colour 'light yellow' _exptl_crystal_size_max 0.04 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.557 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 844 _exptl_absorpt_coefficient_mu 4.000 _exptl_absorpt_correction_type NONE _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 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 12759 _diffrn_reflns_av_R_equivalents 0.0447 _diffrn_reflns_av_sigmaI/netI 0.0835 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _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 2.85 _diffrn_reflns_theta_max 27.48 _reflns_number_total 8218 _reflns_number_gt 6772 _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^)+(0.0310P)^2^+2.3756P] 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 8218 _refine_ls_number_parameters 444 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0642 _refine_ls_R_factor_gt 0.0451 _refine_ls_wR_factor_ref 0.0902 _refine_ls_wR_factor_gt 0.0825 _refine_ls_goodness_of_fit_ref 1.020 _refine_ls_restrained_S_all 1.020 _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 0.79527(2) 0.336250(17) 0.733769(15) 0.01823(7) Uani 1 1 d . . . P1 P 0.64428(13) 0.51019(11) 0.71211(10) 0.0200(3) Uani 1 1 d . . . P2 P 0.67591(14) 0.25690(12) 0.68473(10) 0.0208(3) Uani 1 1 d . . . C1 C 0.9586(5) 0.2344(5) 0.7785(4) 0.0244(12) Uani 1 1 d . . . C2 C 0.9432(5) 0.3442(5) 0.7802(4) 0.0233(12) Uani 1 1 d . . . C3 C 0.9914(6) 0.4294(5) 0.8015(4) 0.0300(13) Uani 1 1 d . . . C4 C 0.9689(6) 0.5399(5) 0.7539(5) 0.0360(14) Uani 1 1 d . . . H4A H 0.9226 0.5584 0.7081 0.043 Uiso 1 1 calc R . . C5 C 1.0130(7) 0.6231(6) 0.7723(5) 0.0473(18) Uani 1 1 d . . . H5A H 0.9962 0.6980 0.7394 0.057 Uiso 1 1 calc R . . C6 C 1.0801(7) 0.5981(6) 0.8370(5) 0.050(2) Uani 1 1 d . . . H6A H 1.1110 0.6551 0.8490 0.059 Uiso 1 1 calc R . . C7 C 1.1031(6) 0.4902(6) 0.8851(5) 0.0415(17) Uani 1 1 d . . . H7A H 1.1499 0.4737 0.9304 0.050 Uiso 1 1 calc R . . C8 C 1.0597(6) 0.4037(5) 0.8694(4) 0.0319(14) Uani 1 1 d . . . C9 C 1.0500(6) 0.1178(5) 0.7924(4) 0.0312(13) Uani 1 1 d . . . C10 C 1.1923(7) 0.1000(6) 0.7489(5) 0.050(2) Uani 1 1 d . . . H10A H 1.2204 0.1628 0.7117 0.060 Uiso 1 1 calc R . . C11 C 1.2871(8) -0.0032(7) 0.7591(6) 0.061(2) Uani 1 1 d . . . H11A H 1.3803 -0.0140 0.7293 0.073 Uiso 1 1 calc R . . C12 C 1.2434(9) -0.0908(7) 0.8139(5) 0.058(2) Uani 1 1 d . . . H12A H 1.3096 -0.1629 0.8221 0.069 Uiso 1 1 calc R . . C13 C 1.1129(9) -0.0827(6) 0.8574(5) 0.0531(19) Uani 1 1 d . . . H13A H 1.0890 -0.1473 0.8945 0.064 Uiso 1 1 calc R . . C14 C 1.0094(8) 0.0274(6) 0.8461(5) 0.0482(18) Uani 1 1 d . . . C15 C 0.8680(9) 0.0422(7) 0.8968(6) 0.066(2) Uani 1 1 d . . . H15A H 0.8129 0.0885 0.8563 0.099 Uiso 1 1 calc R . . H15B H 0.8409 0.0827 0.9544 0.099 Uiso 1 1 calc R . . H15C H 0.8551 -0.0347 0.9139 0.099 Uiso 1 1 calc R . . C16 C 1.0821(7) 0.2890(6) 0.9264(5) 0.0411(16) Uani 1 1 d . . . H16A H 1.0013 0.2654 0.9447 0.062 Uiso 1 1 calc R . . H16B H 1.1006 0.2971 0.9834 0.062 Uiso 1 1 calc R . . H16C H 1.1589 0.2296 0.8885 0.062 Uiso 1 1 calc R . . C17 C 0.5223(5) 0.4887(5) 0.6675(4) 0.0252(12) Uani 1 1 d . . . C18 C 0.4225(6) 0.5816(5) 0.6404(4) 0.0314(13) Uani 1 1 d . . . H18A H 0.4207 0.6596 0.6403 0.038 Uiso 1 1 calc R . . C19 C 0.3265(6) 0.5611(6) 0.6138(4) 0.0356(14) Uani 1 1 d . . . H19A H 0.2608 0.6242 0.5930 0.043 Uiso 1 1 calc R . . C20 C 0.3272(6) 0.4468(6) 0.6178(5) 0.0410(16) Uani 1 1 d . . . H20A H 0.2577 0.4326 0.6037 0.049 Uiso 1 1 calc R . . C21 C 0.4269(6) 0.3542(5) 0.6417(4) 0.0339(14) Uani 1 1 d . . . H21A H 0.4264 0.2766 0.6431 0.041 Uiso 1 1 calc R . . C22 C 0.5289(5) 0.3730(4) 0.6639(4) 0.0205(11) Uani 1 1 d . . . C23 C 0.6983(5) 0.6253(4) 0.6303(4) 0.0229(11) Uani 1 1 d . . . C24 C 0.6267(6) 0.7443(5) 0.6430(4) 0.0347(14) Uani 1 1 d . . . H24A H 0.5502 0.7682 0.6968 0.042 Uiso 1 1 calc R . . C25 C 0.6705(7) 0.8266(5) 0.5748(5) 0.0440(17) Uani 1 1 d . . . H25A H 0.6224 0.9074 0.5822 0.053 Uiso 1 1 calc R . . C26 C 0.7812(7) 0.7935(6) 0.4974(5) 0.0423(17) Uani 1 1 d . . . H26A H 0.8095 0.8510 0.4519 0.051 Uiso 1 1 calc R . . C27 C 0.8521(6) 0.6757(5) 0.4853(4) 0.0348(14) Uani 1 1 d . . . H27A H 0.9289 0.6522 0.4316 0.042 Uiso 1 1 calc R . . C28 C 0.8099(6) 0.5925(5) 0.5524(4) 0.0289(13) Uani 1 1 d . . . H28A H 0.8587 0.5119 0.5445 0.035 Uiso 1 1 calc R . . C29 C 0.5419(5) 0.5801(4) 0.8225(4) 0.0233(12) Uani 1 1 d . . . C30 C 0.6012(6) 0.6287(5) 0.8655(4) 0.0315(14) Uani 1 1 d . . . H30A H 0.6895 0.6326 0.8339 0.038 Uiso 1 1 calc R . . C31 C 0.5313(7) 0.6717(5) 0.9546(4) 0.0405(16) Uani 1 1 d . . . H31A H 0.5720 0.7054 0.9834 0.049 Uiso 1 1 calc R . . C32 C 0.4048(7) 0.6659(5) 1.0010(5) 0.0455(18) Uani 1 1 d . . . H32A H 0.3580 0.6952 1.0620 0.055 Uiso 1 1 calc R . . C33 C 0.3448(7) 0.6177(5) 0.9595(4) 0.0423(17) Uani 1 1 d . . . H33A H 0.2567 0.6137 0.9919 0.051 Uiso 1 1 calc R . . C34 C 0.4129(6) 0.5752(5) 0.8709(4) 0.0331(14) Uani 1 1 d . . . H34A H 0.3710 0.5421 0.8426 0.040 Uiso 1 1 calc R . . C35 C 0.6048(6) 0.1470(5) 0.7600(4) 0.0265(12) Uani 1 1 d . . . C36 C 0.4855(6) 0.1808(5) 0.8347(4) 0.0322(13) Uani 1 1 d . . . H36A H 0.4376 0.2615 0.8430 0.039 Uiso 1 1 calc R . . C37 C 0.4370(6) 0.0980(6) 0.8961(4) 0.0400(16) Uani 1 1 d . . . H37A H 0.3570 0.1217 0.9476 0.048 Uiso 1 1 calc R . . C38 C 0.5043(7) -0.0196(6) 0.8834(5) 0.0422(17) Uani 1 1 d . . . H38A H 0.4696 -0.0761 0.9261 0.051 Uiso 1 1 calc R . . C39 C 0.6201(8) -0.0557(6) 0.8101(5) 0.0504(19) Uani 1 1 d . . . H39A H 0.6654 -0.1367 0.8017 0.060 Uiso 1 1 calc R . . C40 C 0.6709(7) 0.0273(5) 0.7481(4) 0.0366(15) Uani 1 1 d . . . H40A H 0.7513 0.0026 0.6971 0.044 Uiso 1 1 calc R . . C41 C 0.7631(6) 0.1911(4) 0.5699(4) 0.0262(12) Uani 1 1 d . . . C42 C 0.7025(7) 0.1483(5) 0.5243(4) 0.0363(15) Uani 1 1 d . . . H42A H 0.6121 0.1489 0.5538 0.044 Uiso 1 1 calc R . . C43 C 0.7728(8) 0.1048(6) 0.4359(5) 0.0461(18) Uani 1 1 d . . . H43A H 0.7299 0.0768 0.4047 0.055 Uiso 1 1 calc R . . C44 C 0.9051(8) 0.1018(5) 0.3927(5) 0.0460(18) Uani 1 1 d . . . H44A H 0.9534 0.0711 0.3323 0.055 Uiso 1 1 calc R . . C45 C 0.9660(7) 0.1436(6) 0.4377(4) 0.0448(17) Uani 1 1 d . . . H45A H 1.0568 0.1420 0.4083 0.054 Uiso 1 1 calc R . . C46 C 0.8956(6) 0.1883(5) 0.5262(4) 0.0335(14) Uani 1 1 d . . . H46A H 0.9385 0.2171 0.5569 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 Pt 0.01854(11) 0.01577(10) 0.01914(11) -0.00252(7) -0.00374(7) -0.00534(7) P1 0.0208(7) 0.0163(6) 0.0196(7) -0.0019(6) -0.0021(5) -0.0057(5) P2 0.0238(7) 0.0188(7) 0.0210(7) -0.0031(6) -0.0060(6) -0.0081(6) C1 0.024(3) 0.026(3) 0.024(3) -0.001(2) -0.006(2) -0.009(2) C2 0.018(3) 0.026(3) 0.024(3) 0.000(2) -0.004(2) -0.008(2) C3 0.027(3) 0.029(3) 0.035(3) -0.005(3) -0.005(3) -0.013(3) C4 0.037(4) 0.031(3) 0.040(4) 0.000(3) -0.010(3) -0.014(3) C5 0.052(4) 0.038(4) 0.057(5) -0.005(3) -0.009(4) -0.026(3) C6 0.042(4) 0.057(5) 0.060(5) -0.026(4) 0.001(3) -0.033(4) C7 0.036(4) 0.057(4) 0.039(4) -0.020(4) -0.007(3) -0.022(3) C8 0.026(3) 0.038(3) 0.032(3) -0.014(3) -0.003(3) -0.011(3) C9 0.047(4) 0.022(3) 0.027(3) -0.004(3) -0.019(3) -0.006(3) C10 0.049(4) 0.052(4) 0.046(4) -0.032(4) -0.030(3) 0.017(3) C11 0.057(5) 0.064(5) 0.049(5) -0.017(4) -0.023(4) 0.009(4) C12 0.078(6) 0.052(5) 0.033(4) -0.007(4) -0.020(4) -0.003(4) C13 0.078(6) 0.044(4) 0.038(4) 0.006(3) -0.025(4) -0.018(4) C14 0.077(5) 0.033(4) 0.032(4) 0.000(3) -0.018(4) -0.014(4) C15 0.083(7) 0.051(5) 0.073(6) 0.015(4) -0.037(5) -0.029(5) C16 0.044(4) 0.046(4) 0.035(4) -0.006(3) -0.021(3) -0.006(3) C17 0.024(3) 0.027(3) 0.024(3) -0.006(2) -0.005(2) -0.008(2) C18 0.031(3) 0.029(3) 0.028(3) 0.002(3) -0.008(3) -0.006(3) C19 0.028(3) 0.043(4) 0.029(3) 0.004(3) -0.012(3) -0.004(3) C20 0.035(4) 0.048(4) 0.048(4) -0.003(3) -0.023(3) -0.012(3) C21 0.036(4) 0.035(3) 0.035(4) -0.005(3) -0.016(3) -0.010(3) C22 0.021(3) 0.023(3) 0.019(3) -0.002(2) -0.008(2) -0.007(2) C23 0.029(3) 0.019(3) 0.022(3) 0.003(2) -0.008(2) -0.011(2) C24 0.040(4) 0.024(3) 0.028(3) -0.002(3) 0.002(3) -0.008(3) C25 0.058(5) 0.022(3) 0.043(4) -0.002(3) -0.005(3) -0.013(3) C26 0.058(5) 0.036(4) 0.035(4) 0.012(3) -0.009(3) -0.030(3) C27 0.037(4) 0.041(4) 0.022(3) 0.002(3) 0.000(3) -0.020(3) C28 0.033(3) 0.028(3) 0.026(3) -0.004(3) -0.008(3) -0.011(3) C29 0.026(3) 0.015(2) 0.021(3) 0.000(2) -0.002(2) -0.004(2) C30 0.039(4) 0.029(3) 0.025(3) -0.004(3) -0.006(3) -0.012(3) C31 0.059(4) 0.029(3) 0.029(3) -0.007(3) -0.010(3) -0.010(3) C32 0.054(4) 0.030(3) 0.024(3) -0.004(3) 0.007(3) 0.002(3) C33 0.035(4) 0.036(4) 0.030(4) -0.001(3) 0.005(3) 0.004(3) C34 0.030(3) 0.026(3) 0.034(3) 0.000(3) -0.004(3) -0.006(3) C35 0.031(3) 0.025(3) 0.030(3) 0.000(2) -0.014(3) -0.013(2) C36 0.033(3) 0.033(3) 0.028(3) -0.002(3) -0.007(3) -0.009(3) C37 0.035(4) 0.059(4) 0.027(3) 0.013(3) -0.009(3) -0.023(3) C38 0.063(5) 0.044(4) 0.039(4) 0.014(3) -0.026(3) -0.039(4) C39 0.087(6) 0.024(3) 0.048(4) 0.005(3) -0.023(4) -0.028(4) C40 0.049(4) 0.026(3) 0.026(3) 0.001(3) 0.001(3) -0.015(3) C41 0.038(3) 0.016(3) 0.018(3) 0.002(2) -0.005(2) -0.006(2) C42 0.053(4) 0.033(3) 0.029(3) -0.006(3) -0.012(3) -0.019(3) C43 0.076(5) 0.032(3) 0.040(4) -0.008(3) -0.026(4) -0.016(3) C44 0.070(5) 0.031(3) 0.023(3) -0.003(3) -0.007(3) -0.006(3) C45 0.049(4) 0.043(4) 0.026(3) -0.009(3) 0.007(3) -0.011(3) C46 0.031(3) 0.034(3) 0.030(3) -0.007(3) -0.007(3) -0.003(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt C2 2.042(5) . ? Pt C1 2.064(6) . ? Pt P1 2.2498(14) . ? Pt P2 2.2686(13) . ? P1 C29 1.821(5) . ? P1 C17 1.826(5) . ? P1 C23 1.829(5) . ? P2 C35 1.824(6) . ? P2 C22 1.829(5) . ? P2 C41 1.839(5) . ? C1 C2 1.300(7) . ? C1 C9 1.459(8) . ? C2 C3 1.460(7) . ? C3 C4 1.395(9) . ? C3 C8 1.408(9) . ? C4 C5 1.386(8) . ? C4 H4A 0.9500 . ? C5 C6 1.358(10) . ? C5 H5A 0.9500 . ? C6 C7 1.372(10) . ? C6 H6A 0.9500 . ? C7 C8 1.399(8) . ? C7 H7A 0.9500 . ? C8 C16 1.497(9) . ? C9 C14 1.369(9) . ? C9 C10 1.444(9) . ? C10 C11 1.353(10) . ? C10 H10A 0.9500 . ? C11 C12 1.360(11) . ? C11 H11A 0.9500 . ? C12 C13 1.351(11) . ? C12 H12A 0.9500 . ? C13 C14 1.458(10) . ? C13 H13A 0.9500 . ? C14 C15 1.456(11) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C18 1.395(8) . ? C17 C22 1.406(7) . ? C18 C19 1.379(8) . ? C18 H18A 0.9500 . ? C19 C20 1.390(9) . ? C19 H19A 0.9500 . ? C20 C21 1.374(9) . ? C20 H20A 0.9500 . ? C21 C22 1.394(7) . ? C21 H21A 0.9500 . ? C23 C28 1.378(7) . ? C23 C24 1.403(7) . ? C24 C25 1.396(8) . ? C24 H24A 0.9500 . ? C25 C26 1.369(9) . ? C25 H25A 0.9500 . ? C26 C27 1.388(9) . ? C26 H26A 0.9500 . ? C27 C28 1.390(8) . ? C27 H27A 0.9500 . ? C28 H28A 0.9500 . ? C29 C34 1.389(7) . ? C29 C30 1.392(8) . ? C30 C31 1.391(8) . ? C30 H30A 0.9500 . ? C31 C32 1.363(9) . ? C31 H31A 0.9500 . ? C32 C33 1.378(10) . ? C32 H32A 0.9500 . ? C33 C34 1.380(8) . ? C33 H33A 0.9500 . ? C34 H34A 0.9500 . ? C35 C36 1.398(8) . ? C35 C40 1.401(8) . ? C36 C37 1.375(8) . ? C36 H36A 0.9500 . ? C37 C38 1.383(9) . ? C37 H37A 0.9500 . ? C38 C39 1.367(10) . ? C38 H38A 0.9500 . ? C39 C40 1.392(8) . ? C39 H39A 0.9500 . ? C40 H40A 0.9500 . ? C41 C42 1.384(8) . ? C41 C46 1.386(8) . ? C42 C43 1.384(8) . ? C42 H42A 0.9500 . ? C43 C44 1.384(10) . ? C43 H43A 0.9500 . ? C44 C45 1.372(10) . ? C44 H44A 0.9500 . ? C45 C46 1.391(8) . ? C45 H45A 0.9500 . ? C46 H46A 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 Pt C1 36.9(2) . . ? C2 Pt P1 114.90(15) . . ? C1 Pt P1 151.56(14) . . ? C2 Pt P2 158.85(15) . . ? C1 Pt P2 122.02(14) . . ? P1 Pt P2 86.25(5) . . ? C29 P1 C17 104.0(2) . . ? C29 P1 C23 104.9(2) . . ? C17 P1 C23 103.5(3) . . ? C29 P1 Pt 112.62(19) . . ? C17 P1 Pt 109.56(18) . . ? C23 P1 Pt 120.71(18) . . ? C35 P2 C22 103.4(2) . . ? C35 P2 C41 103.4(2) . . ? C22 P2 C41 103.1(2) . . ? C35 P2 Pt 120.72(18) . . ? C22 P2 Pt 109.06(16) . . ? C41 P2 Pt 115.27(19) . . ? C2 C1 C9 141.2(5) . . ? C2 C1 Pt 70.6(3) . . ? C9 C1 Pt 147.9(4) . . ? C1 C2 C3 146.9(6) . . ? C1 C2 Pt 72.5(3) . . ? C3 C2 Pt 140.7(4) . . ? C4 C3 C8 118.7(5) . . ? C4 C3 C2 119.4(6) . . ? C8 C3 C2 121.9(5) . . ? C5 C4 C3 121.0(7) . . ? C5 C4 H4A 119.5 . . ? C3 C4 H4A 119.5 . . ? C6 C5 C4 120.4(7) . . ? C6 C5 H5A 119.8 . . ? C4 C5 H5A 119.8 . . ? C5 C6 C7 119.7(6) . . ? C5 C6 H6A 120.2 . . ? C7 C6 H6A 120.2 . . ? C6 C7 C8 122.0(7) . . ? C6 C7 H7A 119.0 . . ? C8 C7 H7A 119.0 . . ? C7 C8 C3 118.2(6) . . ? C7 C8 C16 120.0(6) . . ? C3 C8 C16 121.8(5) . . ? C14 C9 C10 118.9(6) . . ? C14 C9 C1 124.2(6) . . ? C10 C9 C1 116.8(6) . . ? C11 C10 C9 122.3(8) . . ? C11 C10 H10A 118.8 . . ? C9 C10 H10A 118.8 . . ? C10 C11 C12 117.3(8) . . ? C10 C11 H11A 121.4 . . ? C12 C11 H11A 121.4 . . ? C13 C12 C11 124.8(8) . . ? C13 C12 H12A 117.6 . . ? C11 C12 H12A 117.6 . . ? C12 C13 C14 118.6(7) . . ? C12 C13 H13A 120.7 . . ? C14 C13 H13A 120.7 . . ? C9 C14 C15 121.5(7) . . ? C9 C14 C13 118.0(7) . . ? C15 C14 C13 120.3(7) . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C8 C16 H16A 109.5 . . ? C8 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C8 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C18 C17 C22 119.9(5) . . ? C18 C17 P1 122.7(4) . . ? C22 C17 P1 117.4(4) . . ? C19 C18 C17 120.5(5) . . ? C19 C18 H18A 119.7 . . ? C17 C18 H18A 119.7 . . ? C18 C19 C20 119.2(6) . . ? C18 C19 H19A 120.4 . . ? C20 C19 H19A 120.4 . . ? C21 C20 C19 121.0(6) . . ? C21 C20 H20A 119.5 . . ? C19 C20 H20A 119.5 . . ? C20 C21 C22 120.5(5) . . ? C20 C21 H21A 119.7 . . ? C22 C21 H21A 119.7 . . ? C21 C22 C17 118.6(5) . . ? C21 C22 P2 124.4(4) . . ? C17 C22 P2 117.0(4) . . ? C28 C23 C24 119.8(5) . . ? C28 C23 P1 118.1(4) . . ? C24 C23 P1 122.0(4) . . ? C25 C24 C23 118.5(5) . . ? C25 C24 H24A 120.7 . . ? C23 C24 H24A 120.7 . . ? C26 C25 C24 121.4(6) . . ? C26 C25 H25A 119.3 . . ? C24 C25 H25A 119.3 . . ? C25 C26 C27 119.9(6) . . ? C25 C26 H26A 120.0 . . ? C27 C26 H26A 120.0 . . ? C26 C27 C28 119.5(5) . . ? C26 C27 H27A 120.3 . . ? C28 C27 H27A 120.3 . . ? C23 C28 C27 120.9(5) . . ? C23 C28 H28A 119.6 . . ? C27 C28 H28A 119.6 . . ? C34 C29 C30 118.4(5) . . ? C34 C29 P1 122.9(4) . . ? C30 C29 P1 118.3(4) . . ? C31 C30 C29 120.1(6) . . ? C31 C30 H30A 120.0 . . ? C29 C30 H30A 120.0 . . ? C32 C31 C30 120.5(6) . . ? C32 C31 H31A 119.7 . . ? C30 C31 H31A 119.7 . . ? C31 C32 C33 120.1(6) . . ? C31 C32 H32A 119.9 . . ? C33 C32 H32A 119.9 . . ? C32 C33 C34 119.9(6) . . ? C32 C33 H33A 120.1 . . ? C34 C33 H33A 120.1 . . ? C33 C34 C29 120.9(6) . . ? C33 C34 H34A 119.5 . . ? C29 C34 H34A 119.5 . . ? C36 C35 C40 118.3(5) . . ? C36 C35 P2 120.1(4) . . ? C40 C35 P2 121.4(4) . . ? C37 C36 C35 120.4(6) . . ? C37 C36 H36A 119.8 . . ? C35 C36 H36A 119.8 . . ? C36 C37 C38 120.3(6) . . ? C36 C37 H37A 119.8 . . ? C38 C37 H37A 119.8 . . ? C39 C38 C37 120.8(6) . . ? C39 C38 H38A 119.6 . . ? C37 C38 H38A 119.6 . . ? C38 C39 C40 119.4(6) . . ? C38 C39 H39A 120.3 . . ? C40 C39 H39A 120.3 . . ? C39 C40 C35 120.8(6) . . ? C39 C40 H40A 119.6 . . ? C35 C40 H40A 119.6 . . ? C42 C41 C46 119.0(5) . . ? C42 C41 P2 123.6(4) . . ? C46 C41 P2 117.3(4) . . ? C41 C42 C43 120.4(6) . . ? C41 C42 H42A 119.8 . . ? C43 C42 H42A 119.8 . . ? C44 C43 C42 120.4(6) . . ? C44 C43 H43A 119.8 . . ? C42 C43 H43A 119.8 . . ? C45 C44 C43 119.5(6) . . ? C45 C44 H44A 120.3 . . ? C43 C44 H44A 120.3 . . ? C44 C45 C46 120.4(6) . . ? C44 C45 H45A 119.8 . . ? C46 C45 H45A 119.8 . . ? C41 C46 C45 120.4(6) . . ? C41 C46 H46A 119.8 . . ? C45 C46 H46A 119.8 . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 1.471 _refine_diff_density_min -1.288 _refine_diff_density_rms 0.175 data_FO3296 _database_code_depnum_ccdc_archive 'CCDC 743163' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C43 H33 N P2 Pt' _chemical_formula_sum 'C43 H33 N P2 Pt' _chemical_formula_weight 820.73 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.3596(4) _cell_length_b 11.5124(3) _cell_length_c 14.0287(5) _cell_angle_alpha 71.401(2) _cell_angle_beta 83.585(2) _cell_angle_gamma 88.476(2) _cell_volume 1727.8(1) _cell_formula_units_Z 2 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used 12393 _cell_measurement_theta_min 3.05 _cell_measurement_theta_max 27.45 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.04 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.578 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 812 _exptl_absorpt_coefficient_mu 4.185 _exptl_absorpt_correction_type NONE _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 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 12393 _diffrn_reflns_av_R_equivalents 0.0494 _diffrn_reflns_av_sigmaI/netI 0.0843 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.05 _diffrn_reflns_theta_max 27.45 _reflns_number_total 7859 _reflns_number_gt 6421 _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^)+(0.0375P)^2^+0.2439P] 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 7859 _refine_ls_number_parameters 424 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0624 _refine_ls_R_factor_gt 0.0420 _refine_ls_wR_factor_ref 0.0912 _refine_ls_wR_factor_gt 0.0818 _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_restrained_S_all 1.018 _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 0.326647(17) 0.241209(17) 0.741193(15) 0.01701(7) Uani 1 1 d . . . P1 P 0.24595(12) 0.10042(12) 0.68535(10) 0.0187(3) Uani 1 1 d . . . P2 P 0.50329(11) 0.15713(12) 0.71238(10) 0.0186(3) Uani 1 1 d . . . N1 N 0.3505(6) 0.5281(5) 0.8887(5) 0.0502(15) Uani 1 1 d . . . C1 C 0.2168(5) 0.3555(5) 0.7924(4) 0.0225(11) Uani 1 1 d . . . C2 C 0.3247(5) 0.3847(5) 0.7972(4) 0.0223(11) Uani 1 1 d . . . C3 C 0.3974(5) 0.4707(5) 0.8203(4) 0.0244(12) Uani 1 1 d . . . C4 C 0.5123(5) 0.4995(5) 0.7733(5) 0.0320(14) Uani 1 1 d . . . H4A H 0.5447 0.4599 0.7265 0.038 Uiso 1 1 calc R . . C5 C 0.5799(6) 0.5851(5) 0.7939(6) 0.0466(18) Uani 1 1 d . . . H5A H 0.6570 0.6063 0.7595 0.056 Uiso 1 1 calc R . . C6 C 0.5348(7) 0.6388(6) 0.8639(6) 0.051(2) Uani 1 1 d . . . H6A H 0.5817 0.6946 0.8813 0.061 Uiso 1 1 calc R . . C7 C 0.4209(8) 0.6109(7) 0.9089(6) 0.055(2) Uani 1 1 d . . . H7A H 0.3893 0.6505 0.9560 0.066 Uiso 1 1 calc R . . C8 C 0.0052(5) 0.3457(5) 0.7689(5) 0.0368(15) Uani 1 1 d . . . H8A H 0.0255 0.2971 0.7260 0.044 Uiso 1 1 calc R . . C9 C 0.0935(5) 0.3881(5) 0.8108(4) 0.0248(12) Uani 1 1 d . . . C10 C 0.0634(5) 0.4609(5) 0.8696(4) 0.0299(13) Uani 1 1 d . . . H10B H 0.1227 0.4927 0.8974 0.036 Uiso 1 1 calc R . . C11 C -0.0522(6) 0.4872(6) 0.8877(5) 0.0452(18) Uani 1 1 d . . . H11A H -0.0723 0.5390 0.9279 0.054 Uiso 1 1 calc R . . C12 C -0.1410(6) 0.4429(6) 0.8510(5) 0.0485(19) Uani 1 1 d . . . H12A H -0.2216 0.4596 0.8680 0.058 Uiso 1 1 calc R . . C13 C -0.1106(6) 0.3735(6) 0.7889(6) 0.0461(17) Uani 1 1 d . . . H13A H -0.1705 0.3446 0.7597 0.055 Uiso 1 1 calc R . . C14 C 0.3634(5) -0.0022(4) 0.6604(4) 0.0228(11) Uani 1 1 d . . . C15 C 0.3413(6) -0.1076(5) 0.6356(4) 0.0323(14) Uani 1 1 d . . . H15A H 0.2622 -0.1312 0.6341 0.039 Uiso 1 1 calc R . . C16 C 0.4353(6) -0.1776(5) 0.6133(5) 0.0387(16) Uani 1 1 d . . . H16A H 0.4199 -0.2501 0.5981 0.046 Uiso 1 1 calc R . . C17 C 0.5500(6) -0.1433(5) 0.6129(4) 0.0349(15) Uani 1 1 d . . . H17A H 0.6135 -0.1898 0.5941 0.042 Uiso 1 1 calc R . . C18 C 0.5740(5) -0.0416(5) 0.6397(4) 0.0290(13) Uani 1 1 d . . . H18A H 0.6536 -0.0196 0.6411 0.035 Uiso 1 1 calc R . . C19 C 0.4801(5) 0.0293(5) 0.6649(4) 0.0220(11) Uani 1 1 d . . . C20 C 0.1288(5) -0.0060(5) 0.7630(4) 0.0214(11) Uani 1 1 d . . . C21 C 0.1568(5) -0.1147(6) 0.8346(5) 0.0395(15) Uani 1 1 d . . . H21A H 0.2374 -0.1374 0.8394 0.047 Uiso 1 1 calc R . . C22 C 0.0691(6) -0.1906(6) 0.8992(6) 0.0516(19) Uani 1 1 d . . . H22A H 0.0898 -0.2646 0.9480 0.062 Uiso 1 1 calc R . . C23 C -0.0493(6) -0.1583(6) 0.8925(5) 0.0418(16) Uani 1 1 d . . . H23A H -0.1100 -0.2103 0.9362 0.050 Uiso 1 1 calc R . . C24 C -0.0773(5) -0.0517(5) 0.8227(5) 0.0341(14) Uani 1 1 d . . . H24A H -0.1581 -0.0295 0.8184 0.041 Uiso 1 1 calc R . . C25 C 0.0103(5) 0.0256(5) 0.7574(4) 0.0266(12) Uani 1 1 d . . . H25A H -0.0111 0.0998 0.7092 0.032 Uiso 1 1 calc R . . C26 C 0.1848(5) 0.1645(5) 0.5643(4) 0.0221(11) Uani 1 1 d . . . C27 C 0.1407(5) 0.0931(5) 0.5125(5) 0.0314(13) Uani 1 1 d . . . H27A H 0.1371 0.0064 0.5418 0.038 Uiso 1 1 calc R . . C28 C 0.1016(5) 0.1484(6) 0.4176(5) 0.0364(15) Uani 1 1 d . . . H28A H 0.0741 0.0990 0.3817 0.044 Uiso 1 1 calc R . . C29 C 0.1028(5) 0.2744(6) 0.3758(5) 0.0405(16) Uani 1 1 d . . . H29A H 0.0748 0.3118 0.3118 0.049 Uiso 1 1 calc R . . C30 C 0.1447(6) 0.3454(6) 0.4270(5) 0.0400(15) Uani 1 1 d . . . H30A H 0.1455 0.4321 0.3985 0.048 Uiso 1 1 calc R . . C31 C 0.1857(5) 0.2909(5) 0.5202(4) 0.0285(12) Uani 1 1 d . . . H31A H 0.2151 0.3411 0.5546 0.034 Uiso 1 1 calc R . . C32 C 0.6207(5) 0.2477(4) 0.6221(4) 0.0217(11) Uani 1 1 d . . . C33 C 0.5899(5) 0.3537(5) 0.5478(4) 0.0250(12) Uani 1 1 d . . . H33A H 0.5100 0.3801 0.5487 0.030 Uiso 1 1 calc R . . C34 C 0.6741(5) 0.4210(5) 0.4728(4) 0.0321(14) Uani 1 1 d . . . H34A H 0.6516 0.4931 0.4229 0.039 Uiso 1 1 calc R . . C35 C 0.7895(6) 0.3841(5) 0.4702(5) 0.0356(14) Uani 1 1 d . . . H35A H 0.8467 0.4295 0.4177 0.043 Uiso 1 1 calc R . . C36 C 0.8231(5) 0.2798(6) 0.5446(5) 0.0364(15) Uani 1 1 d . . . H36A H 0.9036 0.2552 0.5439 0.044 Uiso 1 1 calc R . . C37 C 0.7396(5) 0.2124(5) 0.6193(4) 0.0295(13) Uani 1 1 d . . . H37A H 0.7630 0.1411 0.6695 0.035 Uiso 1 1 calc R . . C38 C 0.5798(5) 0.0865(5) 0.8246(4) 0.0243(12) Uani 1 1 d . . . C39 C 0.6388(5) 0.1633(5) 0.8622(4) 0.0253(12) Uani 1 1 d . . . H39A H 0.6397 0.2493 0.8293 0.030 Uiso 1 1 calc R . . C40 C 0.6969(5) 0.1139(6) 0.9489(4) 0.0324(14) Uani 1 1 d . . . H40A H 0.7407 0.1661 0.9728 0.039 Uiso 1 1 calc R . . C41 C 0.6908(5) -0.0104(5) 1.0000(4) 0.0312(13) Uani 1 1 d . . . H41A H 0.7295 -0.0434 1.0594 0.037 Uiso 1 1 calc R . . C42 C 0.6288(5) -0.0864(5) 0.9650(4) 0.0302(13) Uani 1 1 d . . . H42A H 0.6236 -0.1717 1.0009 0.036 Uiso 1 1 calc R . . C43 C 0.5733(5) -0.0389(5) 0.8770(4) 0.0253(12) Uani 1 1 d . . . H43A H 0.5312 -0.0919 0.8527 0.030 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 0.01618(11) 0.01637(10) 0.01837(11) -0.00585(7) -0.00041(7) -0.00013(7) P1 0.0199(7) 0.0181(6) 0.0178(7) -0.0054(5) -0.0011(5) -0.0027(5) P2 0.0154(7) 0.0181(6) 0.0208(7) -0.0051(5) 0.0009(5) -0.0002(5) N1 0.066(4) 0.043(3) 0.050(4) -0.023(3) -0.018(3) 0.005(3) C1 0.027(3) 0.019(3) 0.021(3) -0.007(2) 0.000(2) -0.001(2) C2 0.025(3) 0.021(3) 0.020(3) -0.007(2) 0.002(2) 0.001(2) C3 0.030(3) 0.017(3) 0.028(3) -0.008(2) -0.006(2) 0.003(2) C4 0.033(3) 0.024(3) 0.038(4) -0.006(3) -0.012(3) -0.002(2) C5 0.035(4) 0.030(3) 0.070(5) -0.003(3) -0.022(4) -0.002(3) C6 0.062(5) 0.029(3) 0.069(5) -0.018(3) -0.035(4) 0.000(3) C7 0.076(6) 0.048(4) 0.058(5) -0.035(4) -0.026(4) 0.007(4) C8 0.032(3) 0.022(3) 0.058(4) -0.015(3) -0.007(3) 0.002(2) C9 0.024(3) 0.025(3) 0.021(3) -0.002(2) 0.001(2) 0.003(2) C10 0.022(3) 0.043(3) 0.031(3) -0.022(3) -0.006(3) 0.012(3) C11 0.039(4) 0.054(4) 0.041(4) -0.015(3) -0.006(3) 0.024(3) C12 0.028(4) 0.055(4) 0.041(4) 0.011(3) 0.007(3) 0.012(3) C13 0.027(3) 0.047(4) 0.054(5) -0.001(3) -0.003(3) -0.001(3) C14 0.027(3) 0.017(2) 0.020(3) -0.002(2) 0.000(2) -0.002(2) C15 0.047(4) 0.027(3) 0.026(3) -0.012(2) -0.007(3) -0.002(3) C16 0.065(5) 0.026(3) 0.032(4) -0.017(3) -0.009(3) 0.007(3) C17 0.047(4) 0.028(3) 0.027(3) -0.009(3) 0.006(3) 0.009(3) C18 0.034(3) 0.024(3) 0.027(3) -0.007(2) 0.001(3) 0.004(2) C19 0.025(3) 0.020(3) 0.020(3) -0.006(2) 0.000(2) 0.002(2) C20 0.023(3) 0.024(3) 0.016(3) -0.006(2) 0.000(2) -0.011(2) C21 0.025(3) 0.046(4) 0.036(4) 0.006(3) -0.010(3) -0.007(3) C22 0.042(4) 0.043(4) 0.048(5) 0.018(3) -0.009(3) -0.013(3) C23 0.037(4) 0.044(4) 0.035(4) -0.001(3) 0.005(3) -0.016(3) C24 0.026(3) 0.035(3) 0.036(4) -0.006(3) 0.006(3) -0.008(3) C25 0.022(3) 0.025(3) 0.030(3) -0.006(2) -0.001(2) 0.000(2) C26 0.019(3) 0.027(3) 0.019(3) -0.006(2) 0.000(2) -0.003(2) C27 0.025(3) 0.035(3) 0.034(4) -0.012(3) -0.001(3) -0.005(2) C28 0.028(3) 0.058(4) 0.027(3) -0.019(3) -0.002(3) -0.014(3) C29 0.029(3) 0.067(5) 0.016(3) 0.002(3) -0.002(3) -0.011(3) C30 0.041(4) 0.044(4) 0.025(3) 0.006(3) -0.010(3) -0.005(3) C31 0.025(3) 0.031(3) 0.028(3) -0.006(2) -0.004(2) -0.003(2) C32 0.020(3) 0.021(3) 0.021(3) -0.006(2) 0.004(2) 0.000(2) C33 0.026(3) 0.022(3) 0.025(3) -0.007(2) 0.005(2) -0.002(2) C34 0.037(4) 0.027(3) 0.027(3) -0.003(2) 0.001(3) -0.001(3) C35 0.037(4) 0.040(3) 0.027(3) -0.010(3) 0.010(3) -0.014(3) C36 0.019(3) 0.046(4) 0.037(4) -0.007(3) 0.012(3) -0.007(3) C37 0.025(3) 0.029(3) 0.028(3) -0.001(2) 0.001(2) -0.001(2) C38 0.021(3) 0.027(3) 0.023(3) -0.006(2) 0.002(2) 0.004(2) C39 0.026(3) 0.025(3) 0.023(3) -0.005(2) -0.002(2) -0.002(2) C40 0.029(3) 0.046(4) 0.026(3) -0.016(3) -0.001(3) 0.000(3) C41 0.031(3) 0.040(3) 0.018(3) -0.004(3) 0.006(3) 0.004(3) C42 0.032(3) 0.025(3) 0.024(3) 0.004(2) 0.005(3) 0.008(2) C43 0.021(3) 0.027(3) 0.025(3) -0.006(2) 0.004(2) -0.001(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 Pt C1 2.030(5) . ? Pt C2 2.042(5) . ? Pt P2 2.2565(13) . ? Pt P1 2.2650(13) . ? P1 C26 1.830(5) . ? P1 C20 1.836(5) . ? P1 C14 1.837(5) . ? P2 C32 1.823(5) . ? P2 C38 1.829(6) . ? P2 C19 1.834(5) . ? N1 C7 1.376(9) . ? N1 C3 1.383(7) . ? C1 C2 1.294(8) . ? C1 C9 1.456(7) . ? C2 C3 1.441(7) . ? C3 C4 1.392(8) . ? C4 C5 1.383(8) . ? C4 H4A 0.9500 . ? C5 C6 1.368(10) . ? C5 H5A 0.9500 . ? C6 C7 1.373(11) . ? C6 H6A 0.9500 . ? C7 H7A 0.9500 . ? C8 C13 1.366(8) . ? C8 C9 1.390(8) . ? C8 H8A 0.9500 . ? C9 C10 1.365(7) . ? C10 C11 1.355(8) . ? C10 H10B 0.9500 . ? C11 C12 1.361(10) . ? C11 H11A 0.9500 . ? C12 C13 1.371(10) . ? C12 H12A 0.9500 . ? C13 H13A 0.9500 . ? C14 C19 1.398(8) . ? C14 C15 1.400(7) . ? C15 C16 1.388(8) . ? C15 H15A 0.9500 . ? C16 C17 1.370(9) . ? C16 H16A 0.9500 . ? C17 C18 1.381(8) . ? C17 H17A 0.9500 . ? C18 C19 1.408(7) . ? C18 H18A 0.9500 . ? C20 C21 1.387(8) . ? C20 C25 1.390(7) . ? C21 C22 1.384(9) . ? C21 H21A 0.9500 . ? C22 C23 1.392(9) . ? C22 H22A 0.9500 . ? C23 C24 1.359(8) . ? C23 H23A 0.9500 . ? C24 C25 1.395(8) . ? C24 H24A 0.9500 . ? C25 H25A 0.9500 . ? C26 C31 1.388(7) . ? C26 C27 1.393(8) . ? C27 C28 1.397(9) . ? C27 H27A 0.9500 . ? C28 C29 1.380(9) . ? C28 H28A 0.9500 . ? C29 C30 1.371(9) . ? C29 H29A 0.9500 . ? C30 C31 1.385(8) . ? C30 H30A 0.9500 . ? C31 H31A 0.9500 . ? C32 C33 1.394(7) . ? C32 C37 1.400(7) . ? C33 C34 1.385(8) . ? C33 H33A 0.9500 . ? C34 C35 1.367(8) . ? C34 H34A 0.9500 . ? C35 C36 1.394(9) . ? C35 H35A 0.9500 . ? C36 C37 1.378(8) . ? C36 H36A 0.9500 . ? C37 H37A 0.9500 . ? C38 C39 1.385(8) . ? C38 C43 1.394(7) . ? C39 C40 1.399(8) . ? C39 H39A 0.9500 . ? C40 C41 1.381(8) . ? C40 H40A 0.9500 . ? C41 C42 1.374(9) . ? C41 H41A 0.9500 . ? C42 C43 1.395(8) . ? C42 H42A 0.9500 . ? C43 H43A 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Pt C2 37.1(2) . . ? C1 Pt P2 154.68(16) . . ? C2 Pt P2 117.84(16) . . ? C1 Pt P1 118.49(16) . . ? C2 Pt P1 155.53(16) . . ? P2 Pt P1 86.64(5) . . ? C26 P1 C20 102.8(2) . . ? C26 P1 C14 104.2(2) . . ? C20 P1 C14 103.2(2) . . ? C26 P1 Pt 114.39(17) . . ? C20 P1 Pt 121.72(17) . . ? C14 P1 Pt 108.70(18) . . ? C32 P2 C38 102.5(3) . . ? C32 P2 C19 103.6(2) . . ? C38 P2 C19 103.6(2) . . ? C32 P2 Pt 120.90(16) . . ? C38 P2 Pt 115.27(17) . . ? C19 P2 Pt 109.06(17) . . ? C7 N1 C3 118.2(6) . . ? C2 C1 C9 143.3(5) . . ? C2 C1 Pt 72.0(3) . . ? C9 C1 Pt 144.7(4) . . ? C1 C2 C3 144.3(5) . . ? C1 C2 Pt 71.0(3) . . ? C3 C2 Pt 144.6(4) . . ? N1 C3 C4 119.5(5) . . ? N1 C3 C2 119.0(5) . . ? C4 C3 C2 121.5(5) . . ? C5 C4 C3 120.9(6) . . ? C5 C4 H4A 119.6 . . ? C3 C4 H4A 119.6 . . ? C6 C5 C4 119.5(7) . . ? C6 C5 H5A 120.2 . . ? C4 C5 H5A 120.2 . . ? C5 C6 C7 119.1(6) . . ? C5 C6 H6A 120.5 . . ? C7 C6 H6A 120.5 . . ? C6 C7 N1 122.8(6) . . ? C6 C7 H7A 118.6 . . ? N1 C7 H7A 118.6 . . ? C13 C8 C9 120.3(6) . . ? C13 C8 H8A 119.8 . . ? C9 C8 H8A 119.8 . . ? C10 C9 C8 119.2(5) . . ? C10 C9 C1 120.2(5) . . ? C8 C9 C1 120.6(5) . . ? C11 C10 C9 119.1(6) . . ? C11 C10 H10B 120.5 . . ? C9 C10 H10B 120.5 . . ? C10 C11 C12 123.0(6) . . ? C10 C11 H11A 118.5 . . ? C12 C11 H11A 118.5 . . ? C11 C12 C13 118.0(6) . . ? C11 C12 H12A 121.0 . . ? C13 C12 H12A 121.0 . . ? C8 C13 C12 120.3(7) . . ? C8 C13 H13A 119.8 . . ? C12 C13 H13A 119.8 . . ? C19 C14 C15 119.3(5) . . ? C19 C14 P1 117.4(4) . . ? C15 C14 P1 123.3(4) . . ? C16 C15 C14 119.8(6) . . ? C16 C15 H15A 120.1 . . ? C14 C15 H15A 120.1 . . ? C17 C16 C15 120.8(5) . . ? C17 C16 H16A 119.6 . . ? C15 C16 H16A 119.6 . . ? C16 C17 C18 120.4(5) . . ? C16 C17 H17A 119.8 . . ? C18 C17 H17A 119.8 . . ? C17 C18 C19 119.9(6) . . ? C17 C18 H18A 120.1 . . ? C19 C18 H18A 120.1 . . ? C14 C19 C18 119.7(5) . . ? C14 C19 P2 117.6(4) . . ? C18 C19 P2 122.6(4) . . ? C21 C20 C25 118.5(5) . . ? C21 C20 P1 120.7(4) . . ? C25 C20 P1 120.5(4) . . ? C22 C21 C20 121.1(6) . . ? C22 C21 H21A 119.4 . . ? C20 C21 H21A 119.4 . . ? C21 C22 C23 119.9(6) . . ? C21 C22 H22A 120.1 . . ? C23 C22 H22A 120.1 . . ? C24 C23 C22 119.3(6) . . ? C24 C23 H23A 120.4 . . ? C22 C23 H23A 120.4 . . ? C23 C24 C25 121.4(6) . . ? C23 C24 H24A 119.3 . . ? C25 C24 H24A 119.3 . . ? C20 C25 C24 119.8(5) . . ? C20 C25 H25A 120.1 . . ? C24 C25 H25A 120.1 . . ? C31 C26 C27 118.2(5) . . ? C31 C26 P1 118.3(4) . . ? C27 C26 P1 123.5(4) . . ? C26 C27 C28 120.2(5) . . ? C26 C27 H27A 119.9 . . ? C28 C27 H27A 119.9 . . ? C29 C28 C27 120.3(6) . . ? C29 C28 H28A 119.8 . . ? C27 C28 H28A 119.8 . . ? C30 C29 C28 119.7(6) . . ? C30 C29 H29A 120.1 . . ? C28 C29 H29A 120.1 . . ? C29 C30 C31 120.2(6) . . ? C29 C30 H30A 119.9 . . ? C31 C30 H30A 119.9 . . ? C30 C31 C26 121.3(6) . . ? C30 C31 H31A 119.4 . . ? C26 C31 H31A 119.4 . . ? C33 C32 C37 117.9(5) . . ? C33 C32 P2 118.5(4) . . ? C37 C32 P2 123.4(4) . . ? C34 C33 C32 121.0(5) . . ? C34 C33 H33A 119.5 . . ? C32 C33 H33A 119.5 . . ? C35 C34 C33 120.3(5) . . ? C35 C34 H34A 119.8 . . ? C33 C34 H34A 119.8 . . ? C34 C35 C36 119.9(5) . . ? C34 C35 H35A 120.1 . . ? C36 C35 H35A 120.1 . . ? C37 C36 C35 120.0(5) . . ? C37 C36 H36A 120.0 . . ? C35 C36 H36A 120.0 . . ? C36 C37 C32 120.9(5) . . ? C36 C37 H37A 119.6 . . ? C32 C37 H37A 119.6 . . ? C39 C38 C43 119.4(5) . . ? C39 C38 P2 117.7(4) . . ? C43 C38 P2 122.7(4) . . ? C38 C39 C40 119.9(5) . . ? C38 C39 H39A 120.1 . . ? C40 C39 H39A 120.1 . . ? C41 C40 C39 120.3(6) . . ? C41 C40 H40A 119.9 . . ? C39 C40 H40A 119.9 . . ? C42 C41 C40 120.0(6) . . ? C42 C41 H41A 120.0 . . ? C40 C41 H41A 120.0 . . ? C41 C42 C43 120.3(5) . . ? C41 C42 H42A 119.9 . . ? C43 C42 H42A 119.9 . . ? C38 C43 C42 120.0(5) . . ? C38 C43 H43A 120.0 . . ? C42 C43 H43A 120.0 . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.45 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.078 _refine_diff_density_min -1.469 _refine_diff_density_rms 0.181 data_FO3336 _database_code_depnum_ccdc_archive 'CCDC 743164' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C42 H32 N2 P2 Pt' _chemical_formula_sum 'C42 H32 N2 P2 Pt' _chemical_formula_weight 821.73 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.9010(4) _cell_length_b 11.0800(6) _cell_length_c 19.0760(7) _cell_angle_alpha 103.772(3) _cell_angle_beta 96.509(2) _cell_angle_gamma 107.308(2) _cell_volume 1709.75(14) _cell_formula_units_Z 2 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used 12065 _cell_measurement_theta_min 2.45 _cell_measurement_theta_max 27.47 _exptl_crystal_description prism _exptl_crystal_colour 'light yellow' _exptl_crystal_size_max 0.04 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.596 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 812 _exptl_absorpt_coefficient_mu 4.230 _exptl_absorpt_correction_type NONE _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 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 12065 _diffrn_reflns_av_R_equivalents 0.0502 _diffrn_reflns_av_sigmaI/netI 0.0948 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.45 _diffrn_reflns_theta_max 27.47 _reflns_number_total 7769 _reflns_number_gt 6139 _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^)+(0.0374P)^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 7769 _refine_ls_number_parameters 424 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0741 _refine_ls_R_factor_gt 0.0470 _refine_ls_wR_factor_ref 0.0996 _refine_ls_wR_factor_gt 0.0880 _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_restrained_S_all 1.060 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt Pt -0.91144(3) -0.79357(2) 0.214671(11) 0.01837(8) Uani 1 1 d . . . P1 P -1.00860(16) -0.94458(15) 0.27360(7) 0.0172(3) Uani 1 1 d . . . P2 P -0.72556(17) -0.67932(15) 0.31781(8) 0.0177(3) Uani 1 1 d . . . N1 N -0.6568(7) -0.5234(6) 0.1545(3) 0.0416(16) Uani 1 1 d . . . N2 N -1.2153(7) -0.8411(7) 0.0058(3) 0.0405(16) Uani 1 1 d . . . C1 C -1.0189(7) -0.8165(6) 0.1097(3) 0.0233(13) Uani 1 1 d . . . C2 C -0.8965(7) -0.7079(7) 0.1318(3) 0.0266(14) Uani 1 1 d . . . C3 C -0.7942(7) -0.6010(6) 0.1079(3) 0.0244(14) Uani 1 1 d . . . C4 C -0.8409(8) -0.5837(7) 0.0404(4) 0.0386(18) Uani 1 1 d . . . H4A H -0.9411 -0.6390 0.0095 0.046 Uiso 1 1 calc R . . C5 C -0.7388(10) -0.4840(8) 0.0186(4) 0.051(2) Uani 1 1 d . . . H5A H -0.7684 -0.4703 -0.0275 0.061 Uiso 1 1 calc R . . C6 C -0.5979(9) -0.4070(8) 0.0633(4) 0.048(2) Uani 1 1 d . . . H6A H -0.5247 -0.3404 0.0486 0.057 Uiso 1 1 calc R . . C7 C -0.5619(9) -0.4266(9) 0.1307(5) 0.055(2) Uani 1 1 d . . . H7A H -0.4642 -0.3688 0.1628 0.066 Uiso 1 1 calc R . . C8 C -1.3353(8) -0.9215(10) -0.0500(4) 0.052(2) Uani 1 1 d . . . H8A H -1.3823 -0.8812 -0.0809 0.062 Uiso 1 1 calc R . . C9 C -1.1489(7) -0.9010(7) 0.0489(3) 0.0284(15) Uani 1 1 d . . . C10 C -1.2016(8) -1.0363(8) 0.0357(4) 0.0383(17) Uani 1 1 d . . . H10A H -1.1538 -1.0757 0.0669 0.046 Uiso 1 1 calc R . . C11 C -1.3261(9) -1.1146(9) -0.0241(4) 0.050(2) Uani 1 1 d . . . H11A H -1.3614 -1.2080 -0.0351 0.060 Uiso 1 1 calc R . . C12 C -1.3968(9) -1.0554(10) -0.0668(4) 0.051(2) Uani 1 1 d . . . H12A H -1.4849 -1.1055 -0.1065 0.061 Uiso 1 1 calc R . . C13 C -0.8757(6) -0.8950(6) 0.3646(3) 0.0194(12) Uani 1 1 d . . . C14 C -0.8956(7) -0.9726(7) 0.4141(3) 0.0238(14) Uani 1 1 d . . . H14A H -0.9818 -1.0539 0.4014 0.029 Uiso 1 1 calc R . . C15 C -0.7897(7) -0.9306(7) 0.4811(3) 0.0279(14) Uani 1 1 d . . . H15A H -0.8059 -0.9815 0.5150 0.033 Uiso 1 1 calc R . . C16 C -0.6597(7) -0.8140(7) 0.4988(3) 0.0256(14) Uani 1 1 d . . . H16A H -0.5853 -0.7868 0.5441 0.031 Uiso 1 1 calc R . . C17 C -0.6390(7) -0.7385(6) 0.4512(3) 0.0235(13) Uani 1 1 d . . . H17A H -0.5499 -0.6591 0.4636 0.028 Uiso 1 1 calc R . . C18 C -0.7483(6) -0.7771(6) 0.3841(3) 0.0180(12) Uani 1 1 d . . . C19 C -1.2068(6) -0.9663(6) 0.2958(3) 0.0193(12) Uani 1 1 d . . . C20 C -1.2315(7) -0.9028(6) 0.3630(3) 0.0240(14) Uani 1 1 d . . . H20A H -1.1417 -0.8470 0.4007 0.029 Uiso 1 1 calc R . . C21 C -1.3842(7) -0.9191(7) 0.3762(4) 0.0326(16) Uani 1 1 d . . . H21A H -1.3989 -0.8751 0.4228 0.039 Uiso 1 1 calc R . . C22 C -1.5169(8) -1.0000(7) 0.3215(4) 0.0340(16) Uani 1 1 d . . . H22A H -1.6222 -1.0135 0.3310 0.041 Uiso 1 1 calc R . . C23 C -1.4951(7) -1.0606(7) 0.2532(4) 0.0359(17) Uani 1 1 d . . . H23A H -1.5855 -1.1137 0.2151 0.043 Uiso 1 1 calc R . . C24 C -1.3411(7) -1.0440(7) 0.2403(3) 0.0315(15) Uani 1 1 d . . . H24A H -1.3265 -1.0858 0.1932 0.038 Uiso 1 1 calc R . . C25 C -1.0174(6) -1.1151(6) 0.2342(3) 0.0218(13) Uani 1 1 d . . . C26 C -1.1133(8) -1.2208(7) 0.2532(3) 0.0289(15) Uani 1 1 d . . . H26A H -1.1804 -1.2066 0.2874 0.035 Uiso 1 1 calc R . . C27 C -1.1126(9) -1.3484(7) 0.2228(4) 0.0382(17) Uani 1 1 d . . . H27A H -1.1776 -1.4204 0.2367 0.046 Uiso 1 1 calc R . . C28 C -1.0175(9) -1.3692(8) 0.1726(4) 0.0415(18) Uani 1 1 d . . . H28A H -1.0172 -1.4559 0.1516 0.050 Uiso 1 1 calc R . . C29 C -0.9214(8) -1.2640(8) 0.1523(4) 0.0413(18) Uani 1 1 d . . . H29A H -0.8549 -1.2784 0.1178 0.050 Uiso 1 1 calc R . . C30 C -0.9237(7) -1.1388(7) 0.1828(3) 0.0291(15) Uani 1 1 d . . . H30A H -0.8598 -1.0673 0.1682 0.035 Uiso 1 1 calc R . . C31 C -0.5126(6) -0.6376(6) 0.3141(3) 0.0205(13) Uani 1 1 d . . . C32 C -0.4698(7) -0.7195(7) 0.2589(3) 0.0297(15) Uani 1 1 d . . . H32A H -0.5509 -0.7900 0.2227 0.036 Uiso 1 1 calc R . . C33 C -0.3085(8) -0.6993(7) 0.2561(4) 0.0335(16) Uani 1 1 d . . . H33A H -0.2795 -0.7559 0.2183 0.040 Uiso 1 1 calc R . . C34 C -0.1916(7) -0.5964(8) 0.3087(4) 0.0350(17) Uani 1 1 d . . . H34A H -0.0815 -0.5829 0.3075 0.042 Uiso 1 1 calc R . . C35 C -0.2333(8) -0.5129(8) 0.3631(4) 0.0395(19) Uani 1 1 d . . . H35A H -0.1522 -0.4412 0.3986 0.047 Uiso 1 1 calc R . . C36 C -0.3928(7) -0.5336(7) 0.3659(3) 0.0340(17) Uani 1 1 d . . . H36A H -0.4210 -0.4763 0.4037 0.041 Uiso 1 1 calc R . . C37 C -0.7457(6) -0.5248(6) 0.3666(3) 0.0210(13) Uani 1 1 d . . . C38 C -0.7886(7) -0.5004(6) 0.4359(3) 0.0263(14) Uani 1 1 d . . . H38A H -0.7993 -0.5648 0.4619 0.032 Uiso 1 1 calc R . . C39 C -0.8157(8) -0.3847(7) 0.4672(3) 0.0311(15) Uani 1 1 d . . . H39A H -0.8449 -0.3700 0.5141 0.037 Uiso 1 1 calc R . . C40 C -0.8002(8) -0.2907(7) 0.4298(4) 0.0368(17) Uani 1 1 d . . . H40A H -0.8185 -0.2109 0.4511 0.044 Uiso 1 1 calc R . . C41 C -0.7577(8) -0.3125(7) 0.3609(4) 0.0351(16) Uani 1 1 d . . . H41A H -0.7473 -0.2478 0.3352 0.042 Uiso 1 1 calc R . . C42 C -0.7309(7) -0.4283(6) 0.3302(3) 0.0285(15) Uani 1 1 d . . . H42B H -0.7018 -0.4424 0.2833 0.034 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 0.01481(12) 0.02287(14) 0.01638(12) 0.00638(9) 0.00167(7) 0.00474(9) P1 0.0126(7) 0.0207(9) 0.0172(7) 0.0054(6) 0.0024(5) 0.0044(6) P2 0.0138(7) 0.0190(9) 0.0179(7) 0.0049(6) 0.0012(5) 0.0034(6) N1 0.034(3) 0.046(4) 0.039(3) 0.022(3) 0.002(3) -0.001(3) N2 0.028(3) 0.062(5) 0.032(3) 0.023(3) 0.003(2) 0.009(3) C1 0.025(3) 0.029(4) 0.016(3) 0.006(3) 0.002(2) 0.010(3) C2 0.018(3) 0.033(4) 0.024(3) 0.004(3) -0.002(2) 0.007(3) C3 0.029(3) 0.023(4) 0.025(3) 0.011(3) 0.010(2) 0.010(3) C4 0.035(4) 0.042(5) 0.034(4) 0.017(3) -0.001(3) 0.002(3) C5 0.069(6) 0.051(6) 0.038(4) 0.027(4) 0.018(4) 0.014(4) C6 0.050(5) 0.043(5) 0.055(5) 0.023(4) 0.028(4) 0.010(4) C7 0.038(5) 0.060(6) 0.061(5) 0.029(5) 0.003(4) 0.000(4) C8 0.028(4) 0.101(8) 0.020(3) 0.021(4) 0.000(3) 0.013(4) C9 0.016(3) 0.039(4) 0.025(3) 0.008(3) 0.007(2) 0.002(3) C10 0.031(4) 0.040(5) 0.034(4) 0.002(3) 0.003(3) 0.007(3) C11 0.032(4) 0.043(5) 0.051(5) -0.012(4) 0.009(3) -0.001(4) C12 0.024(4) 0.077(7) 0.026(4) -0.005(4) -0.002(3) -0.002(4) C13 0.013(3) 0.026(3) 0.023(3) 0.007(3) 0.005(2) 0.011(2) C14 0.019(3) 0.031(4) 0.025(3) 0.012(3) 0.005(2) 0.009(3) C15 0.034(4) 0.031(4) 0.023(3) 0.011(3) 0.004(3) 0.015(3) C16 0.023(3) 0.034(4) 0.018(3) 0.003(3) -0.001(2) 0.013(3) C17 0.017(3) 0.029(4) 0.022(3) 0.005(3) -0.001(2) 0.007(3) C18 0.016(3) 0.019(3) 0.018(3) 0.001(2) 0.005(2) 0.008(2) C19 0.016(3) 0.022(3) 0.024(3) 0.009(3) 0.004(2) 0.011(2) C20 0.019(3) 0.030(4) 0.026(3) 0.010(3) 0.003(2) 0.011(3) C21 0.025(3) 0.041(4) 0.033(3) 0.009(3) 0.010(3) 0.012(3) C22 0.021(3) 0.040(4) 0.044(4) 0.015(4) 0.012(3) 0.011(3) C23 0.016(3) 0.039(5) 0.041(4) 0.004(3) 0.000(3) 0.000(3) C24 0.021(3) 0.037(4) 0.030(3) 0.002(3) 0.002(2) 0.007(3) C25 0.015(3) 0.026(4) 0.025(3) 0.006(3) 0.001(2) 0.009(3) C26 0.032(4) 0.026(4) 0.024(3) 0.003(3) 0.005(3) 0.006(3) C27 0.052(5) 0.020(4) 0.035(4) 0.003(3) -0.001(3) 0.009(3) C28 0.055(5) 0.028(4) 0.035(4) -0.005(3) -0.010(3) 0.022(4) C29 0.033(4) 0.053(5) 0.036(4) -0.004(4) 0.005(3) 0.024(4) C30 0.020(3) 0.036(4) 0.027(3) -0.001(3) 0.004(2) 0.010(3) C31 0.012(3) 0.023(3) 0.023(3) 0.012(3) -0.002(2) -0.001(2) C32 0.026(3) 0.031(4) 0.031(3) 0.008(3) 0.007(3) 0.008(3) C33 0.033(4) 0.034(4) 0.041(4) 0.014(3) 0.017(3) 0.015(3) C34 0.010(3) 0.054(5) 0.047(4) 0.027(4) 0.007(3) 0.009(3) C35 0.024(4) 0.038(5) 0.041(4) 0.016(4) -0.002(3) -0.011(3) C36 0.019(3) 0.046(5) 0.027(3) 0.011(3) 0.000(2) -0.001(3) C37 0.013(3) 0.022(3) 0.021(3) 0.000(3) -0.002(2) 0.003(2) C38 0.026(3) 0.023(4) 0.028(3) 0.005(3) 0.005(2) 0.008(3) C39 0.030(4) 0.033(4) 0.027(3) 0.003(3) 0.000(3) 0.013(3) C40 0.038(4) 0.025(4) 0.039(4) -0.005(3) -0.011(3) 0.016(3) C41 0.041(4) 0.021(4) 0.040(4) 0.008(3) -0.003(3) 0.012(3) C42 0.031(4) 0.023(4) 0.026(3) 0.007(3) -0.001(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 Pt C2 2.027(6) . ? Pt C1 2.041(5) . ? Pt P2 2.2452(14) . ? Pt P1 2.2509(14) . ? P1 C19 1.821(6) . ? P1 C25 1.834(7) . ? P1 C13 1.846(5) . ? P2 C37 1.815(6) . ? P2 C31 1.826(6) . ? P2 C18 1.842(5) . ? N1 C3 1.337(8) . ? N1 C7 1.359(9) . ? N2 C8 1.338(9) . ? N2 C9 1.359(8) . ? C1 C2 1.299(8) . ? C1 C9 1.448(8) . ? C2 C3 1.466(8) . ? C3 C4 1.382(8) . ? C4 C5 1.387(9) . ? C4 H4A 0.9500 . ? C5 C6 1.342(11) . ? C5 H5A 0.9500 . ? C6 C7 1.372(10) . ? C6 H6A 0.9500 . ? C7 H7A 0.9500 . ? C8 C12 1.361(12) . ? C8 H8A 0.9500 . ? C9 C10 1.381(10) . ? C10 C11 1.398(9) . ? C10 H10A 0.9500 . ? C11 C12 1.368(12) . ? C11 H11A 0.9500 . ? C12 H12A 0.9500 . ? C13 C18 1.387(8) . ? C13 C14 1.412(8) . ? C14 C15 1.387(8) . ? C14 H14A 0.9500 . ? C15 C16 1.392(9) . ? C15 H15A 0.9500 . ? C16 C17 1.366(8) . ? C16 H16A 0.9500 . ? C17 C18 1.406(7) . ? C17 H17A 0.9500 . ? C19 C20 1.384(8) . ? C19 C24 1.400(8) . ? C20 C21 1.377(8) . ? C20 H20A 0.9500 . ? C21 C22 1.391(9) . ? C21 H21A 0.9500 . ? C22 C23 1.380(9) . ? C22 H22A 0.9500 . ? C23 C24 1.387(9) . ? C23 H23A 0.9500 . ? C24 H24A 0.9500 . ? C25 C26 1.382(8) . ? C25 C30 1.386(8) . ? C26 C27 1.397(10) . ? C26 H26A 0.9500 . ? C27 C28 1.371(10) . ? C27 H27A 0.9500 . ? C28 C29 1.392(10) . ? C28 H28A 0.9500 . ? C29 C30 1.378(10) . ? C29 H29A 0.9500 . ? C30 H30A 0.9500 . ? C31 C32 1.385(9) . ? C31 C36 1.390(8) . ? C32 C33 1.395(9) . ? C32 H32A 0.9500 . ? C33 C34 1.379(10) . ? C33 H33A 0.9500 . ? C34 C35 1.380(11) . ? C34 H34A 0.9500 . ? C35 C36 1.379(9) . ? C35 H35A 0.9500 . ? C36 H36A 0.9500 . ? C37 C42 1.391(8) . ? C37 C38 1.405(8) . ? C38 C39 1.382(9) . ? C38 H38A 0.9500 . ? C39 C40 1.379(9) . ? C39 H39A 0.9500 . ? C40 C41 1.395(10) . ? C40 H40A 0.9500 . ? C41 C42 1.379(10) . ? C41 H41A 0.9500 . ? C42 H42B 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 Pt C1 37.2(2) . . ? C2 Pt P2 114.80(17) . . ? C1 Pt P2 152.01(18) . . ? C2 Pt P1 157.91(17) . . ? C1 Pt P1 120.67(17) . . ? P2 Pt P1 87.29(5) . . ? C19 P1 C25 102.5(3) . . ? C19 P1 C13 103.4(2) . . ? C25 P1 C13 103.0(3) . . ? C19 P1 Pt 118.64(19) . . ? C25 P1 Pt 119.01(19) . . ? C13 P1 Pt 108.28(19) . . ? C37 P2 C31 104.5(3) . . ? C37 P2 C18 104.3(3) . . ? C31 P2 C18 103.2(2) . . ? C37 P2 Pt 114.83(18) . . ? C31 P2 Pt 119.75(19) . . ? C18 P2 Pt 108.69(18) . . ? C3 N1 C7 115.7(6) . . ? C8 N2 C9 115.8(7) . . ? C2 C1 C9 144.6(6) . . ? C2 C1 Pt 70.8(3) . . ? C9 C1 Pt 144.7(5) . . ? C1 C2 C3 144.0(6) . . ? C1 C2 Pt 72.0(4) . . ? C3 C2 Pt 143.3(4) . . ? N1 C3 C4 123.0(6) . . ? N1 C3 C2 116.6(5) . . ? C4 C3 C2 120.4(6) . . ? C3 C4 C5 118.8(6) . . ? C3 C4 H4A 120.6 . . ? C5 C4 H4A 120.6 . . ? C6 C5 C4 119.5(7) . . ? C6 C5 H5A 120.3 . . ? C4 C5 H5A 120.3 . . ? C5 C6 C7 118.6(7) . . ? C5 C6 H6A 120.7 . . ? C7 C6 H6A 120.7 . . ? N1 C7 C6 124.3(7) . . ? N1 C7 H7A 117.9 . . ? C6 C7 H7A 117.9 . . ? N2 C8 C12 126.5(8) . . ? N2 C8 H8A 116.8 . . ? C12 C8 H8A 116.8 . . ? N2 C9 C10 122.0(6) . . ? N2 C9 C1 117.1(6) . . ? C10 C9 C1 120.9(6) . . ? C9 C10 C11 119.1(7) . . ? C9 C10 H10A 120.4 . . ? C11 C10 H10A 120.4 . . ? C12 C11 C10 119.4(8) . . ? C12 C11 H11A 120.3 . . ? C10 C11 H11A 120.3 . . ? C8 C12 C11 117.1(7) . . ? C8 C12 H12A 121.4 . . ? C11 C12 H12A 121.4 . . ? C18 C13 C14 118.8(5) . . ? C18 C13 P1 117.9(4) . . ? C14 C13 P1 123.2(4) . . ? C15 C14 C13 120.3(6) . . ? C15 C14 H14A 119.9 . . ? C13 C14 H14A 119.9 . . ? C14 C15 C16 120.1(5) . . ? C14 C15 H15A 120.0 . . ? C16 C15 H15A 120.0 . . ? C17 C16 C15 120.1(5) . . ? C17 C16 H16A 120.0 . . ? C15 C16 H16A 120.0 . . ? C16 C17 C18 120.7(6) . . ? C16 C17 H17A 119.7 . . ? C18 C17 H17A 119.7 . . ? C13 C18 C17 120.0(5) . . ? C13 C18 P2 117.6(4) . . ? C17 C18 P2 122.4(4) . . ? C20 C19 C24 118.4(5) . . ? C20 C19 P1 123.4(4) . . ? C24 C19 P1 118.1(5) . . ? C21 C20 C19 121.1(6) . . ? C21 C20 H20A 119.5 . . ? C19 C20 H20A 119.5 . . ? C20 C21 C22 120.1(6) . . ? C20 C21 H21A 119.9 . . ? C22 C21 H21A 119.9 . . ? C23 C22 C21 119.8(6) . . ? C23 C22 H22A 120.1 . . ? C21 C22 H22A 120.1 . . ? C22 C23 C24 119.9(6) . . ? C22 C23 H23A 120.1 . . ? C24 C23 H23A 120.1 . . ? C23 C24 C19 120.8(6) . . ? C23 C24 H24A 119.6 . . ? C19 C24 H24A 119.6 . . ? C26 C25 C30 118.6(6) . . ? C26 C25 P1 123.1(5) . . ? C30 C25 P1 118.3(5) . . ? C25 C26 C27 120.7(6) . . ? C25 C26 H26A 119.6 . . ? C27 C26 H26A 119.6 . . ? C28 C27 C26 119.6(7) . . ? C28 C27 H27A 120.2 . . ? C26 C27 H27A 120.2 . . ? C27 C28 C29 120.4(7) . . ? C27 C28 H28A 119.8 . . ? C29 C28 H28A 119.8 . . ? C30 C29 C28 119.2(7) . . ? C30 C29 H29A 120.4 . . ? C28 C29 H29A 120.4 . . ? C29 C30 C25 121.4(6) . . ? C29 C30 H30A 119.3 . . ? C25 C30 H30A 119.3 . . ? C32 C31 C36 119.1(6) . . ? C32 C31 P2 117.5(4) . . ? C36 C31 P2 123.3(5) . . ? C31 C32 C33 120.5(6) . . ? C31 C32 H32A 119.8 . . ? C33 C32 H32A 119.8 . . ? C34 C33 C32 119.4(6) . . ? C34 C33 H33A 120.3 . . ? C32 C33 H33A 120.3 . . ? C35 C34 C33 120.5(6) . . ? C35 C34 H34A 119.8 . . ? C33 C34 H34A 119.8 . . ? C36 C35 C34 120.0(6) . . ? C36 C35 H35A 120.0 . . ? C34 C35 H35A 120.0 . . ? C35 C36 C31 120.6(7) . . ? C35 C36 H36A 119.7 . . ? C31 C36 H36A 119.7 . . ? C42 C37 C38 117.8(6) . . ? C42 C37 P2 117.6(5) . . ? C38 C37 P2 124.4(5) . . ? C39 C38 C37 121.4(6) . . ? C39 C38 H38A 119.3 . . ? C37 C38 H38A 119.3 . . ? C40 C39 C38 119.6(6) . . ? C40 C39 H39A 120.2 . . ? C38 C39 H39A 120.2 . . ? C39 C40 C41 120.1(7) . . ? C39 C40 H40A 119.9 . . ? C41 C40 H40A 119.9 . . ? C42 C41 C40 119.9(6) . . ? C42 C41 H41A 120.1 . . ? C40 C41 H41A 120.1 . . ? C41 C42 C37 121.2(6) . . ? C41 C42 H42B 119.4 . . ? C37 C42 H42B 119.4 . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.094 _refine_diff_density_min -1.133 _refine_diff_density_rms 0.203 data_FO3731 _database_code_depnum_ccdc_archive 'CCDC 743165' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C46 H36 Br2 P2 Pt' _chemical_formula_sum 'C46 H36 Br2 P2 Pt' _chemical_formula_weight 1005.60 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' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.9257(2) _cell_length_b 11.2405(4) _cell_length_c 20.9629(8) _cell_angle_alpha 78.7990(10) _cell_angle_beta 83.363(2) _cell_angle_gamma 69.013(2) _cell_volume 1923.84(11) _cell_formula_units_Z 2 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used 13479 _cell_measurement_theta_min 2.45 _cell_measurement_theta_max 27.48 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.736 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 980 _exptl_absorpt_coefficient_mu 5.840 _exptl_absorpt_correction_type NONE _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 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 13479 _diffrn_reflns_av_R_equivalents 0.0332 _diffrn_reflns_av_sigmaI/netI 0.0744 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.45 _diffrn_reflns_theta_max 27.48 _reflns_number_total 8752 _reflns_number_gt 6971 _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^)+(0.0414P)^2^+2.2532P] 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 8752 _refine_ls_number_parameters 462 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0651 _refine_ls_R_factor_gt 0.0426 _refine_ls_wR_factor_ref 0.0962 _refine_ls_wR_factor_gt 0.0876 _refine_ls_goodness_of_fit_ref 1.008 _refine_ls_restrained_S_all 1.008 _refine_ls_shift/su_max 0.013 _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 1.75070(2) 0.15894(2) 0.274664(10) 0.02135(7) Uani 1 1 d . . . Br1 Br 1.31868(10) -0.19338(8) 0.00709(4) 0.0593(2) Uani 1 1 d . . . Br2 Br 2.14613(11) -0.43525(7) 0.43912(5) 0.0689(3) Uani 1 1 d . . . P1 P 1.62938(15) 0.35797(13) 0.21634(6) 0.0211(3) Uani 1 1 d . . . P2 P 1.81685(15) 0.26257(13) 0.34386(7) 0.0214(3) Uani 1 1 d . . . C1 C 1.6790(6) 0.0756(5) 0.2124(3) 0.0252(12) Uani 1 1 d . . . C2 C 1.6228(6) 0.0362(6) 0.1756(3) 0.0288(12) Uani 1 1 d . . . C3 C 1.5545(7) -0.0167(6) 0.1337(3) 0.0301(13) Uani 1 1 d . . . C4 C 1.6534(7) -0.1126(6) 0.0985(3) 0.0328(13) Uani 1 1 d . . . C5 C 1.5797(8) -0.1639(6) 0.0604(3) 0.0419(16) Uani 1 1 d . . . H5A H 1.6438 -0.2299 0.0366 0.050 Uiso 1 1 calc R . . C6 C 1.4135(8) -0.1184(6) 0.0575(3) 0.0381(15) Uani 1 1 d . . . C7 C 1.3175(8) -0.0229(6) 0.0906(3) 0.0401(15) Uani 1 1 d . . . H7A H 1.2041 0.0072 0.0880 0.048 Uiso 1 1 calc R . . C8 C 1.3880(7) 0.0296(6) 0.1280(3) 0.0370(14) Uani 1 1 d . . . H8A H 1.3224 0.0980 0.1502 0.044 Uiso 1 1 calc R . . C9 C 1.8301(8) -0.1643(7) 0.1037(4) 0.0515(18) Uani 1 1 d . . . H9A H 1.8753 -0.2442 0.0852 0.077 Uiso 1 1 calc R . . H9B H 1.8556 -0.1823 0.1496 0.077 Uiso 1 1 calc R . . H9C H 1.8763 -0.1005 0.0797 0.077 Uiso 1 1 calc R . . C10 C 1.8717(6) -0.0257(5) 0.3245(3) 0.0250(12) Uani 1 1 d . . . C11 C 2.0142(7) -0.1067(6) 0.2984(3) 0.0355(14) Uani 1 1 d . . . C12 C 2.0958(8) -0.2266(7) 0.3341(3) 0.0459(17) Uani 1 1 d . . . H12A H 2.1959 -0.2794 0.3173 0.055 Uiso 1 1 calc R . . C13 C 2.0336(8) -0.2686(6) 0.3925(3) 0.0398(15) Uani 1 1 d . . . C14 C 1.8884(7) -0.1962(6) 0.4180(3) 0.0356(14) Uani 1 1 d . . . H14A H 1.8424 -0.2277 0.4578 0.043 Uiso 1 1 calc R . . C15 C 1.8103(6) -0.0730(6) 0.3825(3) 0.0303(13) Uani 1 1 d . . . H15A H 1.7105 -0.0206 0.3997 0.036 Uiso 1 1 calc R . . C16 C 2.0865(9) -0.0750(8) 0.2313(4) 0.062(2) Uani 1 1 d . . . H16A H 2.1259 -0.1522 0.2104 0.093 Uiso 1 1 calc R . . H16B H 2.1760 -0.0460 0.2349 0.093 Uiso 1 1 calc R . . H16C H 2.0045 -0.0063 0.2049 0.093 Uiso 1 1 calc R . . C17 C 1.6560(6) 0.4807(5) 0.2560(2) 0.0225(11) Uani 1 1 d . . . C18 C 1.5996(6) 0.6124(5) 0.2307(3) 0.0288(12) Uani 1 1 d . . . H18A H 1.5409 0.6420 0.1923 0.035 Uiso 1 1 calc R . . C19 C 1.6285(7) 0.6997(6) 0.2612(3) 0.0322(13) Uani 1 1 d . . . H19A H 1.5893 0.7893 0.2441 0.039 Uiso 1 1 calc R . . C20 C 1.7150(6) 0.6556(6) 0.3168(3) 0.0319(13) Uani 1 1 d . . . H20A H 1.7377 0.7153 0.3372 0.038 Uiso 1 1 calc R . . C21 C 1.7685(6) 0.5267(6) 0.3429(3) 0.0276(12) Uani 1 1 d . . . H21A H 1.8245 0.4984 0.3820 0.033 Uiso 1 1 calc R . . C22 C 1.7415(6) 0.4374(5) 0.3127(3) 0.0238(11) Uani 1 1 d . . . C23 C 1.4146(6) 0.4100(5) 0.2062(3) 0.0247(12) Uani 1 1 d . . . C24 C 1.3605(6) 0.3655(6) 0.1583(3) 0.0299(13) Uani 1 1 d . . . H24A H 1.4351 0.3141 0.1297 0.036 Uiso 1 1 calc R . . C25 C 1.1959(7) 0.3979(6) 0.1532(3) 0.0379(15) Uani 1 1 d . . . H25A H 1.1581 0.3683 0.1209 0.045 Uiso 1 1 calc R . . C26 C 1.0879(7) 0.4720(7) 0.1944(3) 0.0429(17) Uani 1 1 d . . . H26A H 0.9760 0.4939 0.1901 0.051 Uiso 1 1 calc R . . C27 C 1.1401(7) 0.5151(7) 0.2422(4) 0.0470(18) Uani 1 1 d . . . H27A H 1.0652 0.5664 0.2707 0.056 Uiso 1 1 calc R . . C28 C 1.3042(7) 0.4820(6) 0.2476(3) 0.0371(14) Uani 1 1 d . . . H28A H 1.3410 0.5098 0.2808 0.045 Uiso 1 1 calc R . . C29 C 1.7153(6) 0.3824(5) 0.1338(3) 0.0225(11) Uani 1 1 d . . . C30 C 1.6379(7) 0.4828(6) 0.0855(3) 0.0313(13) Uani 1 1 d . . . H30A H 1.5342 0.5416 0.0948 0.038 Uiso 1 1 calc R . . C31 C 1.7103(7) 0.4977(6) 0.0241(3) 0.0324(13) Uani 1 1 d . . . H31A H 1.6568 0.5669 -0.0084 0.039 Uiso 1 1 calc R . . C32 C 1.8631(7) 0.4107(6) 0.0099(3) 0.0341(14) Uani 1 1 d . . . H32A H 1.9126 0.4207 -0.0325 0.041 Uiso 1 1 calc R . . C33 C 1.9411(7) 0.3110(6) 0.0571(3) 0.0336(14) Uani 1 1 d . . . H33A H 2.0452 0.2530 0.0476 0.040 Uiso 1 1 calc R . . C34 C 1.8684(6) 0.2949(6) 0.1185(3) 0.0304(13) Uani 1 1 d . . . H34A H 1.9217 0.2247 0.1507 0.036 Uiso 1 1 calc R . . C35 C 2.0303(6) 0.2258(5) 0.3521(3) 0.0236(11) Uani 1 1 d . . . C36 C 2.0886(6) 0.2561(6) 0.4031(3) 0.0313(13) Uani 1 1 d . . . H36A H 2.0169 0.2930 0.4369 0.038 Uiso 1 1 calc R . . C37 C 2.2516(7) 0.2323(6) 0.4046(3) 0.0382(15) Uani 1 1 d . . . H37A H 2.2915 0.2526 0.4397 0.046 Uiso 1 1 calc R . . C38 C 2.3566(7) 0.1794(7) 0.3555(3) 0.0428(16) Uani 1 1 d . . . H38A H 2.4682 0.1640 0.3566 0.051 Uiso 1 1 calc R . . C39 C 2.2990(7) 0.1491(7) 0.3049(3) 0.0441(17) Uani 1 1 d . . . H39A H 2.3710 0.1118 0.2713 0.053 Uiso 1 1 calc R . . C40 C 2.1366(6) 0.1728(6) 0.3030(3) 0.0339(14) Uani 1 1 d . . . H40A H 2.0974 0.1526 0.2677 0.041 Uiso 1 1 calc R . . C41 C 1.7324(6) 0.2480(5) 0.4269(3) 0.0234(11) Uani 1 1 d . . . C42 C 1.8090(6) 0.1405(6) 0.4725(3) 0.0313(13) Uani 1 1 d . . . H42A H 1.9077 0.0788 0.4602 0.038 Uiso 1 1 calc R . . C43 C 1.7437(7) 0.1222(6) 0.5351(3) 0.0375(15) Uani 1 1 d . . . H43A H 1.7966 0.0483 0.5655 0.045 Uiso 1 1 calc R . . C44 C 1.5990(7) 0.2134(7) 0.5532(3) 0.0415(16) Uani 1 1 d . . . H44A H 1.5543 0.2023 0.5964 0.050 Uiso 1 1 calc R . . C45 C 1.5211(7) 0.3190(6) 0.5089(3) 0.0375(15) Uani 1 1 d . . . H45A H 1.4223 0.3803 0.5213 0.045 Uiso 1 1 calc R . . C46 C 1.5866(6) 0.3362(6) 0.4460(3) 0.0303(13) Uani 1 1 d . . . H46A H 1.5314 0.4090 0.4155 0.036 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 0.02131(11) 0.02126(12) 0.02145(12) -0.00454(8) -0.00245(7) -0.00635(7) Br1 0.0813(5) 0.0508(5) 0.0627(5) -0.0139(4) -0.0284(4) -0.0330(4) Br2 0.0885(6) 0.0296(4) 0.0780(6) 0.0074(4) -0.0400(5) -0.0052(4) P1 0.0213(6) 0.0225(7) 0.0189(7) -0.0040(6) -0.0033(5) -0.0061(5) P2 0.0200(6) 0.0238(7) 0.0197(7) -0.0033(6) -0.0035(5) -0.0061(5) C1 0.019(2) 0.029(3) 0.022(3) 0.004(2) 0.001(2) -0.005(2) C2 0.032(3) 0.030(3) 0.026(3) -0.008(3) -0.001(2) -0.011(2) C3 0.041(3) 0.031(3) 0.022(3) -0.005(3) -0.002(2) -0.017(3) C4 0.036(3) 0.029(3) 0.036(3) -0.008(3) 0.001(2) -0.013(2) C5 0.065(4) 0.032(4) 0.034(4) -0.010(3) -0.004(3) -0.020(3) C6 0.055(4) 0.035(4) 0.033(3) 0.001(3) -0.018(3) -0.024(3) C7 0.043(4) 0.039(4) 0.046(4) -0.009(3) -0.013(3) -0.019(3) C8 0.035(3) 0.033(4) 0.043(4) -0.009(3) -0.005(3) -0.010(3) C9 0.046(4) 0.050(5) 0.060(5) -0.029(4) 0.004(3) -0.011(3) C10 0.025(3) 0.022(3) 0.029(3) -0.010(2) -0.004(2) -0.005(2) C11 0.037(3) 0.031(3) 0.034(3) -0.003(3) -0.003(2) -0.006(2) C12 0.041(4) 0.040(4) 0.052(4) -0.016(3) -0.008(3) -0.002(3) C13 0.062(4) 0.021(3) 0.036(4) -0.004(3) -0.023(3) -0.008(3) C14 0.053(4) 0.033(4) 0.028(3) 0.002(3) -0.013(3) -0.024(3) C15 0.029(3) 0.028(3) 0.035(3) -0.010(3) -0.003(2) -0.008(2) C16 0.051(4) 0.062(5) 0.067(6) -0.013(4) 0.010(4) -0.016(4) C17 0.021(2) 0.025(3) 0.020(3) -0.006(2) -0.0017(19) -0.005(2) C18 0.034(3) 0.026(3) 0.024(3) 0.000(2) -0.005(2) -0.009(2) C19 0.039(3) 0.022(3) 0.030(3) 0.001(3) -0.005(2) -0.006(2) C20 0.035(3) 0.031(3) 0.035(3) -0.016(3) 0.002(2) -0.014(2) C21 0.028(3) 0.031(3) 0.024(3) -0.007(2) -0.006(2) -0.009(2) C22 0.018(2) 0.025(3) 0.026(3) -0.008(2) -0.0006(19) -0.003(2) C23 0.023(3) 0.027(3) 0.022(3) 0.000(2) -0.001(2) -0.007(2) C24 0.028(3) 0.038(3) 0.025(3) 0.000(3) -0.004(2) -0.015(2) C25 0.034(3) 0.050(4) 0.032(3) 0.009(3) -0.015(3) -0.022(3) C26 0.017(3) 0.047(4) 0.060(4) 0.001(3) -0.007(3) -0.009(3) C27 0.023(3) 0.053(4) 0.059(5) -0.012(4) 0.009(3) -0.008(3) C28 0.033(3) 0.041(4) 0.039(4) -0.016(3) 0.002(3) -0.010(3) C29 0.024(3) 0.025(3) 0.023(3) -0.005(2) -0.003(2) -0.013(2) C30 0.037(3) 0.032(3) 0.024(3) -0.005(3) -0.001(2) -0.011(2) C31 0.047(3) 0.030(3) 0.023(3) -0.002(3) -0.007(2) -0.015(3) C32 0.044(3) 0.041(4) 0.021(3) -0.008(3) 0.006(2) -0.021(3) C33 0.029(3) 0.044(4) 0.030(3) -0.013(3) 0.008(2) -0.013(3) C34 0.025(3) 0.039(4) 0.029(3) -0.009(3) -0.004(2) -0.011(2) C35 0.025(3) 0.025(3) 0.020(3) -0.002(2) -0.003(2) -0.008(2) C36 0.028(3) 0.036(3) 0.031(3) -0.011(3) -0.003(2) -0.010(2) C37 0.031(3) 0.051(4) 0.038(4) -0.003(3) -0.007(3) -0.021(3) C38 0.027(3) 0.055(4) 0.049(4) -0.001(3) -0.004(3) -0.020(3) C39 0.021(3) 0.066(5) 0.040(4) -0.013(3) 0.007(2) -0.008(3) C40 0.027(3) 0.048(4) 0.030(3) -0.012(3) 0.000(2) -0.015(3) C41 0.019(2) 0.028(3) 0.025(3) -0.004(2) -0.003(2) -0.010(2) C42 0.027(3) 0.032(3) 0.028(3) -0.002(3) 0.002(2) -0.003(2) C43 0.039(3) 0.038(4) 0.026(3) 0.003(3) 0.001(2) -0.007(3) C44 0.041(3) 0.052(4) 0.028(3) -0.008(3) 0.006(3) -0.014(3) C45 0.028(3) 0.043(4) 0.032(3) -0.006(3) 0.006(2) -0.005(3) C46 0.031(3) 0.028(3) 0.030(3) -0.005(3) -0.004(2) -0.006(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 C1 2.021(6) . ? Pt1 C10 2.092(5) . ? Pt1 P2 2.2708(14) . ? Pt1 P1 2.2761(14) . ? Br1 C6 1.899(6) . ? Br2 C13 1.908(6) . ? P1 C23 1.818(5) . ? P1 C29 1.821(5) . ? P1 C17 1.838(6) . ? P2 C41 1.817(5) . ? P2 C35 1.821(5) . ? P2 C22 1.843(6) . ? C1 C2 1.193(8) . ? C2 C3 1.444(8) . ? C3 C8 1.399(8) . ? C3 C4 1.400(8) . ? C4 C5 1.405(8) . ? C4 C9 1.482(8) . ? C5 C6 1.390(9) . ? C5 H5A 0.9500 . ? C6 C7 1.364(9) . ? C7 C8 1.386(9) . ? C7 H7A 0.9500 . ? C8 H8A 0.9500 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C15 1.366(8) . ? C10 C11 1.396(8) . ? C11 C12 1.391(9) . ? C11 C16 1.512(9) . ? C12 C13 1.356(10) . ? C12 H12A 0.9500 . ? C13 C14 1.371(9) . ? C14 C15 1.409(8) . ? C14 H14A 0.9500 . ? C15 H15A 0.9500 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C18 1.396(7) . ? C17 C22 1.395(7) . ? C18 C19 1.378(8) . ? C18 H18A 0.9500 . ? C19 C20 1.383(8) . ? C19 H19A 0.9500 . ? C20 C21 1.372(8) . ? C20 H20A 0.9500 . ? C21 C22 1.388(8) . ? C21 H21A 0.9500 . ? C23 C28 1.371(8) . ? C23 C24 1.405(8) . ? C24 C25 1.392(8) . ? C24 H24A 0.9500 . ? C25 C26 1.373(9) . ? C25 H25A 0.9500 . ? C26 C27 1.383(10) . ? C26 H26A 0.9500 . ? C27 C28 1.388(8) . ? C27 H27A 0.9500 . ? C28 H28A 0.9500 . ? C29 C30 1.391(8) . ? C29 C34 1.412(7) . ? C30 C31 1.378(8) . ? C30 H30A 0.9500 . ? C31 C32 1.403(8) . ? C31 H31A 0.9500 . ? C32 C33 1.376(8) . ? C32 H32A 0.9500 . ? C33 C34 1.382(8) . ? C33 H33A 0.9500 . ? C34 H34A 0.9500 . ? C35 C40 1.387(8) . ? C35 C36 1.389(8) . ? C36 C37 1.385(8) . ? C36 H36A 0.9500 . ? C37 C38 1.380(9) . ? C37 H37A 0.9500 . ? C38 C39 1.378(9) . ? C38 H38A 0.9500 . ? C39 C40 1.380(8) . ? C39 H39A 0.9500 . ? C40 H40A 0.9500 . ? C41 C42 1.397(8) . ? C41 C46 1.395(7) . ? C42 C43 1.381(8) . ? C42 H42A 0.9500 . ? C43 C44 1.398(8) . ? C43 H43A 0.9500 . ? C44 C45 1.373(9) . ? C44 H44A 0.9500 . ? C45 C46 1.385(8) . ? C45 H45A 0.9500 . ? C46 H46A 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Pt1 C10 88.6(2) . . ? C1 Pt1 P2 176.55(15) . . ? C10 Pt1 P2 94.24(15) . . ? C1 Pt1 P1 90.61(15) . . ? C10 Pt1 P1 177.03(15) . . ? P2 Pt1 P1 86.64(5) . . ? C23 P1 C29 104.2(2) . . ? C23 P1 C17 105.2(2) . . ? C29 P1 C17 105.1(2) . . ? C23 P1 Pt1 118.08(18) . . ? C29 P1 Pt1 114.19(17) . . ? C17 P1 Pt1 109.01(17) . . ? C41 P2 C35 104.8(2) . . ? C41 P2 C22 104.5(2) . . ? C35 P2 C22 103.9(2) . . ? C41 P2 Pt1 117.13(18) . . ? C35 P2 Pt1 116.65(18) . . ? C22 P2 Pt1 108.48(18) . . ? C2 C1 Pt1 173.6(5) . . ? C1 C2 C3 177.1(6) . . ? C8 C3 C4 120.1(5) . . ? C8 C3 C2 119.3(5) . . ? C4 C3 C2 120.6(5) . . ? C3 C4 C5 118.1(5) . . ? C3 C4 C9 121.5(6) . . ? C5 C4 C9 120.4(6) . . ? C6 C5 C4 120.3(6) . . ? C6 C5 H5A 119.9 . . ? C4 C5 H5A 119.9 . . ? C7 C6 C5 121.6(6) . . ? C7 C6 Br1 119.5(5) . . ? C5 C6 Br1 118.9(5) . . ? C6 C7 C8 119.0(6) . . ? C6 C7 H7A 120.5 . . ? C8 C7 H7A 120.5 . . ? C3 C8 C7 120.9(6) . . ? C3 C8 H8A 119.5 . . ? C7 C8 H8A 119.5 . . ? C4 C9 H9A 109.5 . . ? C4 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C4 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C15 C10 C11 117.7(5) . . ? C15 C10 Pt1 121.0(4) . . ? C11 C10 Pt1 121.3(4) . . ? C12 C11 C10 119.9(6) . . ? C12 C11 C16 116.0(6) . . ? C10 C11 C16 124.0(6) . . ? C13 C12 C11 120.5(6) . . ? C13 C12 H12A 119.7 . . ? C11 C12 H12A 119.7 . . ? C12 C13 C14 121.5(6) . . ? C12 C13 Br2 119.4(5) . . ? C14 C13 Br2 119.0(5) . . ? C13 C14 C15 117.2(6) . . ? C13 C14 H14A 121.4 . . ? C15 C14 H14A 121.4 . . ? C10 C15 C14 122.9(5) . . ? C10 C15 H15A 118.6 . . ? C14 C15 H15A 118.6 . . ? C11 C16 H16A 109.5 . . ? C11 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C11 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C18 C17 C22 119.7(5) . . ? C18 C17 P1 122.9(4) . . ? C22 C17 P1 117.4(4) . . ? C19 C18 C17 120.4(5) . . ? C19 C18 H18A 119.8 . . ? C17 C18 H18A 119.8 . . ? C18 C19 C20 119.4(5) . . ? C18 C19 H19A 120.3 . . ? C20 C19 H19A 120.3 . . ? C21 C20 C19 120.8(5) . . ? C21 C20 H20A 119.6 . . ? C19 C20 H20A 119.6 . . ? C20 C21 C22 120.5(5) . . ? C20 C21 H21A 119.7 . . ? C22 C21 H21A 119.7 . . ? C21 C22 C17 119.1(5) . . ? C21 C22 P2 122.4(4) . . ? C17 C22 P2 118.5(4) . . ? C28 C23 C24 119.2(5) . . ? C28 C23 P1 121.8(4) . . ? C24 C23 P1 118.8(4) . . ? C25 C24 C23 119.1(6) . . ? C25 C24 H24A 120.5 . . ? C23 C24 H24A 120.5 . . ? C26 C25 C24 120.6(6) . . ? C26 C25 H25A 119.7 . . ? C24 C25 H25A 119.7 . . ? C25 C26 C27 120.7(5) . . ? C25 C26 H26A 119.6 . . ? C27 C26 H26A 119.6 . . ? C26 C27 C28 118.7(6) . . ? C26 C27 H27A 120.7 . . ? C28 C27 H27A 120.7 . . ? C23 C28 C27 121.8(6) . . ? C23 C28 H28A 119.1 . . ? C27 C28 H28A 119.1 . . ? C30 C29 C34 118.7(5) . . ? C30 C29 P1 123.3(4) . . ? C34 C29 P1 118.0(4) . . ? C31 C30 C29 120.6(5) . . ? C31 C30 H30A 119.7 . . ? C29 C30 H30A 119.7 . . ? C30 C31 C32 120.0(5) . . ? C30 C31 H31A 120.0 . . ? C32 C31 H31A 120.0 . . ? C33 C32 C31 120.0(5) . . ? C33 C32 H32A 120.0 . . ? C31 C32 H32A 120.0 . . ? C32 C33 C34 120.2(5) . . ? C32 C33 H33A 119.9 . . ? C34 C33 H33A 119.9 . . ? C33 C34 C29 120.4(5) . . ? C33 C34 H34A 119.8 . . ? C29 C34 H34A 119.8 . . ? C40 C35 C36 119.3(5) . . ? C40 C35 P2 118.0(4) . . ? C36 C35 P2 122.6(4) . . ? C37 C36 C35 119.8(5) . . ? C37 C36 H36A 120.1 . . ? C35 C36 H36A 120.1 . . ? C38 C37 C36 120.5(6) . . ? C38 C37 H37A 119.7 . . ? C36 C37 H37A 119.7 . . ? C39 C38 C37 119.7(5) . . ? C39 C38 H38A 120.1 . . ? C37 C38 H38A 120.1 . . ? C38 C39 C40 120.1(6) . . ? C38 C39 H39A 119.9 . . ? C40 C39 H39A 119.9 . . ? C39 C40 C35 120.5(6) . . ? C39 C40 H40A 119.8 . . ? C35 C40 H40A 119.8 . . ? C42 C41 C46 118.2(5) . . ? C42 C41 P2 119.5(4) . . ? C46 C41 P2 122.2(4) . . ? C43 C42 C41 121.2(5) . . ? C43 C42 H42A 119.4 . . ? C41 C42 H42A 119.4 . . ? C42 C43 C44 119.3(6) . . ? C42 C43 H43A 120.3 . . ? C44 C43 H43A 120.3 . . ? C45 C44 C43 120.3(6) . . ? C45 C44 H44A 119.9 . . ? C43 C44 H44A 119.9 . . ? C44 C45 C46 120.1(5) . . ? C44 C45 H45A 120.0 . . ? C46 C45 H45A 120.0 . . ? C45 C46 C41 120.9(5) . . ? C45 C46 H46A 119.6 . . ? C41 C46 H46A 119.6 . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.318 _refine_diff_density_min -1.457 _refine_diff_density_rms 0.157 data_FO3697 _database_code_depnum_ccdc_archive 'CCDC 743166' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C46 H36 Br2 P2 Pt, C4 H8 O' _chemical_formula_sum 'C50 H44 Br2 O P2 Pt' _chemical_formula_weight 1077.70 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' 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' 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 15.3444(5) _cell_length_b 15.6009(3) _cell_length_c 21.3260(6) _cell_angle_alpha 90.00 _cell_angle_beta 111.085(2) _cell_angle_gamma 90.00 _cell_volume 4763.4(2) _cell_formula_units_Z 4 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used 31984 _cell_measurement_theta_min 1.93 _cell_measurement_theta_max 27.50 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.06 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.503 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2120 _exptl_absorpt_coefficient_mu 4.724 _exptl_absorpt_correction_type NONE _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 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 31984 _diffrn_reflns_av_R_equivalents 0.0669 _diffrn_reflns_av_sigmaI/netI 0.0774 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.93 _diffrn_reflns_theta_max 27.50 _reflns_number_total 10847 _reflns_number_gt 7025 _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^)+(0.0835P)^2^+1.5850P] 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 10847 _refine_ls_number_parameters 502 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1019 _refine_ls_R_factor_gt 0.0534 _refine_ls_wR_factor_ref 0.1483 _refine_ls_wR_factor_gt 0.1279 _refine_ls_goodness_of_fit_ref 1.004 _refine_ls_restrained_S_all 1.004 _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 Pt1 Pt 0.972561(18) -0.284514(15) 1.624812(13) 0.03670(10) Uani 1 1 d . . . Br1 Br 1.13998(6) -0.32092(6) 1.67526(4) 0.0626(2) Uani 1 1 d . . . Br2 Br 0.83826(11) -0.40093(14) 2.21455(7) 0.1430(7) Uani 1 1 d . . . P1 P 0.98795(12) -0.25933(11) 1.52396(9) 0.0375(4) Uani 1 1 d . . . P2 P 0.82316(12) -0.25221(11) 1.57603(9) 0.0376(4) Uani 1 1 d . . . C1 C 0.9603(5) -0.3069(5) 1.7183(4) 0.0441(17) Uani 1 1 d . . . C2 C 0.9552(5) -0.3814(5) 1.7387(3) 0.0415(16) Uani 1 1 d . . . H2A H 0.9561 -0.4283 1.7104 0.050 Uiso 1 1 calc R . . C3 C 0.9482(5) -0.3991(4) 1.8023(4) 0.0473(18) Uani 1 1 d . . . H3A H 0.9423 -0.4565 1.8151 0.057 Uiso 1 1 calc R . . C4 C 0.9502(5) -0.3304(4) 1.8464(4) 0.0453(17) Uani 1 1 d . . . C5 C 0.9578(5) -0.2465(5) 1.8239(4) 0.0508(18) Uani 1 1 d . . . C6 C 0.9636(5) -0.2359(4) 1.7603(4) 0.0472(18) Uani 1 1 d . . . H6A H 0.9700 -0.1799 1.7451 0.057 Uiso 1 1 calc R . . C7 C 0.9598(7) -0.1713(5) 1.8688(5) 0.068(2) Uani 1 1 d . . . H7A H 0.9466 -0.1185 1.8421 0.103 Uiso 1 1 calc R . . H7B H 1.0217 -0.1672 1.9042 0.103 Uiso 1 1 calc R . . H7C H 0.9124 -0.1793 1.8891 0.103 Uiso 1 1 calc R . . C8 C 0.9418(5) -0.3440(4) 1.9104(4) 0.0484(18) Uani 1 1 d . . . C9 C 0.9296(5) -0.3530(5) 1.9614(4) 0.0489(18) Uani 1 1 d . . . C10 C 0.9095(5) -0.3639(5) 2.0220(4) 0.0530(19) Uani 1 1 d . . . C11 C 0.9046(6) -0.4459(6) 2.0458(5) 0.072(3) Uani 1 1 d . . . H11A H 0.9153 -0.4947 2.0230 0.087 Uiso 1 1 calc R . . C12 C 0.8834(7) -0.4553(8) 2.1040(6) 0.082(3) Uani 1 1 d . . . H12A H 0.8803 -0.5110 2.1211 0.099 Uiso 1 1 calc R . . C13 C 0.8671(7) -0.3851(9) 2.1365(5) 0.083(3) Uani 1 1 d . . . C14 C 0.8684(8) -0.3068(8) 2.1112(5) 0.083(3) Uani 1 1 d . . . H14A H 0.8526 -0.2589 2.1326 0.100 Uiso 1 1 calc R . . C15 C 0.8913(7) -0.2932(6) 2.0561(5) 0.071(3) Uani 1 1 d . . . C16 C 0.8962(11) -0.2048(6) 2.0285(6) 0.113(5) Uani 1 1 d . . . H16A H 0.8602 -0.1645 2.0448 0.170 Uiso 1 1 calc R . . H16B H 0.8700 -0.2066 1.9792 0.170 Uiso 1 1 calc R . . H16C H 0.9614 -0.1861 2.0434 0.170 Uiso 1 1 calc R . . C17 C 0.8723(5) -0.2327(4) 1.4637(4) 0.0388(15) Uani 1 1 d . . . C18 C 0.8583(5) -0.2130(4) 1.3978(4) 0.0466(17) Uani 1 1 d . . . H18A H 0.9092 -0.2142 1.3824 0.056 Uiso 1 1 calc R . . C19 C 0.7682(5) -0.1912(5) 1.3533(4) 0.053(2) Uani 1 1 d . . . H19A H 0.7579 -0.1791 1.3075 0.064 Uiso 1 1 calc R . . C20 C 0.6948(5) -0.1874(5) 1.3763(4) 0.0503(19) Uani 1 1 d . . . H20A H 0.6342 -0.1722 1.3464 0.060 Uiso 1 1 calc R . . C21 C 0.7092(5) -0.2054(4) 1.4427(4) 0.0428(16) Uani 1 1 d . . . H21A H 0.6587 -0.2015 1.4584 0.051 Uiso 1 1 calc R . . C22 C 0.7976(4) -0.2295(4) 1.4867(3) 0.0356(15) Uani 1 1 d . . . C23 C 1.0580(5) -0.1670(4) 1.5219(4) 0.0415(16) Uani 1 1 d . . . C24 C 1.0695(6) -0.1039(5) 1.5702(4) 0.056(2) Uani 1 1 d . . . H24A H 1.0449 -0.1123 1.6047 0.067 Uiso 1 1 calc R . . C25 C 1.1174(7) -0.0276(5) 1.5684(5) 0.071(3) Uani 1 1 d . . . H25A H 1.1246 0.0156 1.6012 0.085 Uiso 1 1 calc R . . C26 C 1.1531(6) -0.0162(6) 1.5196(6) 0.083(3) Uani 1 1 d . . . H26A H 1.1843 0.0359 1.5180 0.099 Uiso 1 1 calc R . . C27 C 1.1451(6) -0.0805(6) 1.4708(5) 0.072(3) Uani 1 1 d . . . H27A H 1.1726 -0.0728 1.4377 0.087 Uiso 1 1 calc R . . C28 C 1.0957(6) -0.1555(5) 1.4725(5) 0.064(2) Uani 1 1 d . . . H28A H 1.0881 -0.1987 1.4395 0.076 Uiso 1 1 calc R . . C29 C 1.0294(5) -0.3456(4) 1.4850(3) 0.0402(15) Uani 1 1 d . . . C30 C 1.1234(5) -0.3619(5) 1.5037(4) 0.0524(19) Uani 1 1 d . . . H30A H 1.1669 -0.3255 1.5355 0.063 Uiso 1 1 calc R . . C31 C 1.1561(6) -0.4310(5) 1.4768(5) 0.063(2) Uani 1 1 d . . . H31A H 1.2212 -0.4403 1.4889 0.076 Uiso 1 1 calc R . . C32 C 1.0925(7) -0.4857(5) 1.4323(4) 0.064(2) Uani 1 1 d . . . H32B H 1.1141 -0.5336 1.4145 0.076 Uiso 1 1 calc R . . C33 C 0.9970(6) -0.4711(5) 1.4137(4) 0.060(2) Uani 1 1 d . . . H33A H 0.9536 -0.5089 1.3833 0.072 Uiso 1 1 calc R . . C34 C 0.9658(6) -0.4019(4) 1.4393(4) 0.0499(18) Uani 1 1 d . . . H34A H 0.9006 -0.3918 1.4260 0.060 Uiso 1 1 calc R . . C35 C 0.7404(5) -0.3347(4) 1.5774(4) 0.051(2) Uani 1 1 d . . . C36 C 0.6968(5) -0.3866(4) 1.5219(4) 0.053(2) Uani 1 1 d . . . H36A H 0.7087 -0.3790 1.4816 0.064 Uiso 1 1 calc R . . C37 C 0.6347(6) -0.4506(5) 1.5266(6) 0.072(3) Uani 1 1 d . . . H37A H 0.6030 -0.4849 1.4883 0.086 Uiso 1 1 calc R . . C38 C 0.6194(6) -0.4644(6) 1.5839(6) 0.083(3) Uani 1 1 d . . . H38A H 0.5778 -0.5086 1.5857 0.099 Uiso 1 1 calc R . . C39 C 0.6639(7) -0.4142(7) 1.6411(6) 0.090(4) Uani 1 1 d . . . H39A H 0.6529 -0.4241 1.6816 0.107 Uiso 1 1 calc R . . C40 C 0.7250(6) -0.3492(6) 1.6376(5) 0.066(2) Uani 1 1 d . . . H40A H 0.7561 -0.3150 1.6760 0.080 Uiso 1 1 calc R . . C41 C 0.7854(5) -0.1570(4) 1.6082(3) 0.0381(15) Uani 1 1 d . . . C42 C 0.6901(6) -0.1449(5) 1.5996(4) 0.056(2) Uani 1 1 d . . . H42A H 0.6445 -0.1864 1.5766 0.067 Uiso 1 1 calc R . . C43 C 0.6646(6) -0.0717(6) 1.6254(5) 0.072(3) Uani 1 1 d . . . H43A H 0.6012 -0.0633 1.6206 0.086 Uiso 1 1 calc R . . C44 C 0.7311(6) -0.0106(5) 1.6582(4) 0.064(2) Uani 1 1 d . . . H44A H 0.7127 0.0394 1.6757 0.077 Uiso 1 1 calc R . . C45 C 0.8218(5) -0.0213(5) 1.6654(4) 0.054(2) Uani 1 1 d . . . H45A H 0.8667 0.0212 1.6876 0.065 Uiso 1 1 calc R . . C46 C 0.8493(5) -0.0950(4) 1.6401(4) 0.0482(18) Uani 1 1 d . . . H46A H 0.9129 -0.1023 1.6451 0.058 Uiso 1 1 calc R . . O1TA O 1.1194(9) -0.1993(8) 1.3072(7) 0.071(3) Uiso 0.50 1 d P . . C1TA C 1.0538(19) -0.2688(15) 1.2853(14) 0.104(8) Uiso 0.50 1 d P . . H1TA H 1.0288 -0.2827 1.3209 0.125 Uiso 0.50 1 calc PR . . H1TB H 1.0010 -0.2515 1.2445 0.125 Uiso 0.50 1 calc PR . . C2TA C 1.0984(12) -0.3426(11) 1.2709(9) 0.065(4) Uiso 0.50 1 d P . . H2TA H 1.0841 -0.3483 1.2220 0.078 Uiso 0.50 1 calc PR . . H2TB H 1.0782 -0.3954 1.2876 0.078 Uiso 0.50 1 calc PR . . C3TA C 1.1962(12) -0.3271(11) 1.3060(9) 0.063(4) Uiso 0.50 1 d P . . H3TA H 1.2317 -0.3369 1.2759 0.075 Uiso 0.50 1 calc PR . . H3TB H 1.2212 -0.3655 1.3454 0.075 Uiso 0.50 1 calc PR . . C4TA C 1.2034(14) -0.2365(12) 1.3276(11) 0.075(5) Uiso 0.50 1 d P . . H4TA H 1.2320 -0.2335 1.3772 0.090 Uiso 0.50 1 calc PR . . H4TB H 1.2444 -0.2051 1.3087 0.090 Uiso 0.50 1 calc PR . . O1TB O 1.3738(10) 0.5102(9) 1.6362(7) 0.087(4) Uiso 0.50 1 d P . . C1TB C 1.3092(16) 0.4660(15) 1.6609(12) 0.092(6) Uiso 0.50 1 d P . . H1TC H 1.2447 0.4880 1.6394 0.110 Uiso 0.50 1 calc PR . . H1TD H 1.3096 0.4034 1.6536 0.110 Uiso 0.50 1 calc PR . . C2TB C 1.345(2) 0.4858(19) 1.7266(15) 0.126(9) Uiso 0.50 1 d P . . H2TC H 1.3829 0.4371 1.7517 0.151 Uiso 0.50 1 calc PR . . H2TD H 1.2930 0.4945 1.7433 0.151 Uiso 0.50 1 calc PR . . C3TB C 1.3990(15) 0.5578(13) 1.7393(11) 0.083(6) Uiso 0.50 1 d P . . H3TC H 1.3620 0.6101 1.7384 0.100 Uiso 0.50 1 calc PR . . H3TD H 1.4517 0.5541 1.7829 0.100 Uiso 0.50 1 calc PR . . C4TB C 1.4262(18) 0.5553(16) 1.6910(13) 0.105(7) Uiso 0.50 1 d P . . H4TC H 1.4901 0.5310 1.7072 0.126 Uiso 0.50 1 calc PR . . H4TD H 1.4308 0.6150 1.6767 0.126 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 Pt1 0.03315(15) 0.03443(15) 0.03715(16) 0.00198(11) 0.00614(11) 0.00122(11) Br1 0.0410(4) 0.0876(6) 0.0498(5) 0.0052(4) 0.0051(4) 0.0107(4) Br2 0.1081(11) 0.254(2) 0.0678(8) 0.0384(10) 0.0333(7) -0.0493(12) P1 0.0326(9) 0.0337(8) 0.0416(10) 0.0020(7) 0.0076(8) -0.0013(7) P2 0.0330(9) 0.0326(8) 0.0445(10) 0.0037(8) 0.0106(8) 0.0003(7) C1 0.028(4) 0.055(4) 0.039(4) -0.011(3) 0.001(3) 0.002(3) C2 0.040(4) 0.047(4) 0.031(4) -0.014(3) 0.005(3) 0.002(3) C3 0.045(4) 0.035(4) 0.063(5) 0.005(3) 0.022(4) 0.000(3) C4 0.036(4) 0.045(4) 0.054(5) 0.001(3) 0.014(3) 0.003(3) C5 0.051(5) 0.042(4) 0.063(5) 0.000(4) 0.025(4) 0.008(3) C6 0.055(5) 0.035(4) 0.053(5) 0.003(3) 0.020(4) 0.005(3) C7 0.096(7) 0.051(5) 0.065(6) -0.016(4) 0.036(5) -0.002(5) C8 0.043(4) 0.046(4) 0.054(5) 0.001(3) 0.016(4) 0.002(3) C9 0.049(5) 0.050(4) 0.049(5) 0.002(3) 0.020(4) -0.002(3) C10 0.044(4) 0.061(5) 0.053(5) 0.004(4) 0.015(4) -0.001(4) C11 0.062(6) 0.067(6) 0.086(7) 0.026(5) 0.024(5) 0.001(4) C12 0.064(6) 0.101(8) 0.078(7) 0.040(6) 0.022(5) -0.014(6) C13 0.053(6) 0.138(10) 0.046(5) 0.016(6) 0.002(4) -0.035(6) C14 0.104(9) 0.104(8) 0.041(5) -0.006(5) 0.026(5) -0.007(6) C15 0.087(7) 0.078(6) 0.054(5) -0.016(4) 0.035(5) -0.013(5) C16 0.204(16) 0.057(6) 0.100(9) -0.006(6) 0.081(10) 0.006(7) C17 0.034(4) 0.034(3) 0.045(4) 0.001(3) 0.009(3) -0.007(3) C18 0.041(4) 0.052(4) 0.044(4) 0.004(3) 0.013(3) -0.002(3) C19 0.049(5) 0.051(4) 0.046(4) 0.010(3) 0.001(4) -0.001(3) C20 0.038(4) 0.041(4) 0.056(5) 0.009(3) -0.002(4) 0.005(3) C21 0.033(4) 0.043(4) 0.047(4) 0.004(3) 0.008(3) -0.005(3) C22 0.026(3) 0.030(3) 0.041(4) 0.001(3) 0.000(3) 0.000(2) C23 0.032(4) 0.040(4) 0.048(4) 0.005(3) 0.009(3) -0.007(3) C24 0.051(5) 0.045(4) 0.065(5) -0.004(4) 0.012(4) -0.010(3) C25 0.066(6) 0.046(5) 0.085(7) -0.004(4) 0.010(5) -0.017(4) C26 0.042(5) 0.054(5) 0.135(10) 0.032(6) 0.012(6) -0.004(4) C27 0.062(6) 0.066(6) 0.095(7) 0.013(5) 0.035(5) -0.012(4) C28 0.061(5) 0.051(5) 0.082(6) 0.004(4) 0.031(5) -0.003(4) C29 0.043(4) 0.038(3) 0.036(4) -0.001(3) 0.010(3) -0.001(3) C30 0.043(4) 0.049(4) 0.060(5) -0.005(4) 0.013(4) 0.000(3) C31 0.063(6) 0.052(5) 0.075(6) -0.001(4) 0.024(5) 0.018(4) C32 0.077(6) 0.059(5) 0.058(5) 0.003(4) 0.028(5) 0.020(4) C33 0.076(6) 0.045(4) 0.050(5) -0.004(4) 0.012(4) -0.005(4) C34 0.048(4) 0.045(4) 0.056(5) 0.001(3) 0.018(4) -0.005(3) C35 0.033(4) 0.041(4) 0.074(6) 0.015(4) 0.012(4) 0.001(3) C36 0.045(4) 0.036(4) 0.072(5) 0.006(4) 0.013(4) 0.004(3) C37 0.053(5) 0.038(4) 0.110(8) 0.007(5) 0.013(5) -0.007(4) C38 0.049(6) 0.076(6) 0.113(9) 0.045(6) 0.016(6) -0.008(5) C39 0.059(6) 0.111(8) 0.091(8) 0.052(7) 0.018(6) -0.014(6) C40 0.062(6) 0.072(5) 0.059(5) 0.024(4) 0.015(4) -0.009(4) C41 0.042(4) 0.030(3) 0.041(4) 0.004(3) 0.013(3) 0.009(3) C42 0.050(5) 0.055(4) 0.057(5) -0.010(4) 0.012(4) 0.008(4) C43 0.049(5) 0.087(6) 0.070(6) -0.015(5) 0.012(4) 0.022(5) C44 0.074(6) 0.057(5) 0.063(6) -0.012(4) 0.027(5) 0.016(4) C45 0.048(5) 0.045(4) 0.064(5) -0.009(4) 0.013(4) 0.002(3) C46 0.038(4) 0.045(4) 0.063(5) 0.004(3) 0.021(4) 0.006(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 C1 2.099(8) . ? Pt1 P2 2.2082(17) . ? Pt1 P1 2.2806(19) . ? Pt1 Br1 2.4679(8) . ? Br2 C13 1.886(10) . ? P1 C23 1.807(7) . ? P1 C29 1.812(7) . ? P1 C17 1.825(7) . ? P2 C41 1.816(6) . ? P2 C35 1.816(7) . ? P2 C22 1.836(7) . ? C1 C2 1.254(10) . ? C1 C6 1.412(10) . ? C2 C3 1.426(10) . ? C2 H2A 0.9500 . ? C3 C4 1.419(10) . ? C3 H3A 0.9500 . ? C4 C5 1.412(10) . ? C4 C8 1.433(11) . ? C5 C6 1.400(11) . ? C5 C7 1.508(11) . ? C6 H6A 0.9500 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 C9 1.176(10) . ? C9 C10 1.442(11) . ? C10 C11 1.389(11) . ? C10 C15 1.403(12) . ? C11 C12 1.400(13) . ? C11 H11A 0.9500 . ? C12 C13 1.366(16) . ? C12 H12A 0.9500 . ? C13 C14 1.339(15) . ? C14 C15 1.358(13) . ? C14 H14A 0.9500 . ? C15 C16 1.513(13) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C18 1.378(10) . ? C17 C22 1.402(10) . ? C18 C19 1.408(10) . ? C18 H18A 0.9500 . ? C19 C20 1.383(11) . ? C19 H19A 0.9500 . ? C20 C21 1.380(10) . ? C20 H20A 0.9500 . ? C21 C22 1.395(9) . ? C21 H21A 0.9500 . ? C23 C28 1.384(11) . ? C23 C24 1.390(10) . ? C24 C25 1.407(11) . ? C24 H24A 0.9500 . ? C25 C26 1.350(14) . ? C25 H25A 0.9500 . ? C26 C27 1.418(15) . ? C26 H26A 0.9500 . ? C27 C28 1.402(11) . ? C27 H27A 0.9500 . ? C28 H28A 0.9500 . ? C29 C30 1.375(10) . ? C29 C34 1.411(10) . ? C30 C31 1.396(11) . ? C30 H30A 0.9500 . ? C31 C32 1.384(12) . ? C31 H31A 0.9500 . ? C32 C33 1.391(12) . ? C32 H32B 0.9500 . ? C33 C34 1.371(11) . ? C33 H33A 0.9500 . ? C34 H34A 0.9500 . ? C35 C36 1.391(11) . ? C35 C40 1.405(12) . ? C36 C37 1.407(11) . ? C36 H36A 0.9500 . ? C37 C38 1.344(14) . ? C37 H37A 0.9500 . ? C38 C39 1.403(15) . ? C38 H38A 0.9500 . ? C39 C40 1.401(12) . ? C39 H39A 0.9500 . ? C40 H40A 0.9500 . ? C41 C46 1.371(10) . ? C41 C42 1.420(10) . ? C42 C43 1.382(11) . ? C42 H42A 0.9500 . ? C43 C44 1.388(12) . ? C43 H43A 0.9500 . ? C44 C45 1.356(11) . ? C44 H44A 0.9500 . ? C45 C46 1.398(10) . ? C45 H45A 0.9500 . ? C46 H46A 0.9500 . ? O1TA C4TA 1.34(2) . ? O1TA C1TA 1.44(3) . ? C1TA C2TA 1.43(3) . ? C1TA H1TA 0.9900 . ? C1TA H1TB 0.9900 . ? C2TA C3TA 1.44(2) . ? C2TA H2TA 0.9900 . ? C2TA H2TB 0.9900 . ? C3TA C4TA 1.48(3) . ? C3TA H3TA 0.9900 . ? C3TA H3TB 0.9900 . ? C4TA H4TA 0.9900 . ? C4TA H4TB 0.9900 . ? O1TB C4TB 1.35(3) . ? O1TB C1TB 1.45(2) . ? C1TB C2TB 1.34(3) . ? C1TB H1TC 0.9900 . ? C1TB H1TD 0.9900 . ? C2TB C3TB 1.36(3) . ? C2TB H2TC 0.9900 . ? C2TB H2TD 0.9900 . ? C3TB C4TB 1.24(3) . ? C3TB H3TC 0.9900 . ? C3TB H3TD 0.9900 . ? C4TB H4TC 0.9900 . ? C4TB H4TD 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Pt1 P2 93.02(19) . . ? C1 Pt1 P1 179.2(2) . . ? P2 Pt1 P1 87.62(6) . . ? C1 Pt1 Br1 89.01(18) . . ? P2 Pt1 Br1 177.92(5) . . ? P1 Pt1 Br1 90.35(5) . . ? C23 P1 C29 105.7(3) . . ? C23 P1 C17 103.7(3) . . ? C29 P1 C17 105.0(3) . . ? C23 P1 Pt1 115.1(2) . . ? C29 P1 Pt1 118.4(2) . . ? C17 P1 Pt1 107.4(2) . . ? C41 P2 C35 104.7(3) . . ? C41 P2 C22 104.8(3) . . ? C35 P2 C22 105.3(3) . . ? C41 P2 Pt1 115.3(2) . . ? C35 P2 Pt1 116.4(2) . . ? C22 P2 Pt1 109.3(2) . . ? C2 C1 C6 120.0(7) . . ? C2 C1 Pt1 121.4(5) . . ? C6 C1 Pt1 118.5(6) . . ? C1 C2 C3 122.9(7) . . ? C1 C2 H2A 118.5 . . ? C3 C2 H2A 118.5 . . ? C4 C3 C2 119.5(6) . . ? C4 C3 H3A 120.2 . . ? C2 C3 H3A 120.2 . . ? C5 C4 C3 117.4(7) . . ? C5 C4 C8 120.5(7) . . ? C3 C4 C8 122.0(6) . . ? C6 C5 C4 118.7(7) . . ? C6 C5 C7 121.9(7) . . ? C4 C5 C7 119.4(7) . . ? C5 C6 C1 121.4(7) . . ? C5 C6 H6A 119.3 . . ? C1 C6 H6A 119.3 . . ? C5 C7 H7A 109.5 . . ? C5 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C5 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C9 C8 C4 175.9(8) . . ? C8 C9 C10 177.1(9) . . ? C11 C10 C15 119.1(8) . . ? C11 C10 C9 119.6(8) . . ? C15 C10 C9 121.3(7) . . ? C10 C11 C12 118.9(10) . . ? C10 C11 H11A 120.6 . . ? C12 C11 H11A 120.6 . . ? C13 C12 C11 120.5(9) . . ? C13 C12 H12A 119.7 . . ? C11 C12 H12A 119.7 . . ? C14 C13 C12 119.7(10) . . ? C14 C13 Br2 121.1(10) . . ? C12 C13 Br2 119.1(9) . . ? C13 C14 C15 122.4(11) . . ? C13 C14 H14A 118.8 . . ? C15 C14 H14A 118.8 . . ? C14 C15 C10 119.3(9) . . ? C14 C15 C16 122.9(9) . . ? C10 C15 C16 117.8(8) . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C18 C17 C22 120.1(6) . . ? C18 C17 P1 121.7(6) . . ? C22 C17 P1 118.2(5) . . ? C17 C18 C19 119.8(7) . . ? C17 C18 H18A 120.1 . . ? C19 C18 H18A 120.1 . . ? C20 C19 C18 119.9(7) . . ? C20 C19 H19A 120.0 . . ? C18 C19 H19A 120.0 . . ? C21 C20 C19 120.3(7) . . ? C21 C20 H20A 119.8 . . ? C19 C20 H20A 119.8 . . ? C20 C21 C22 120.2(7) . . ? C20 C21 H21A 119.9 . . ? C22 C21 H21A 119.9 . . ? C21 C22 C17 119.6(6) . . ? C21 C22 P2 122.9(6) . . ? C17 C22 P2 117.4(5) . . ? C28 C23 C24 119.8(7) . . ? C28 C23 P1 122.5(6) . . ? C24 C23 P1 117.7(6) . . ? C23 C24 C25 120.4(8) . . ? C23 C24 H24A 119.8 . . ? C25 C24 H24A 119.8 . . ? C26 C25 C24 119.6(9) . . ? C26 C25 H25A 120.2 . . ? C24 C25 H25A 120.2 . . ? C25 C26 C27 121.4(8) . . ? C25 C26 H26A 119.3 . . ? C27 C26 H26A 119.3 . . ? C28 C27 C26 118.4(9) . . ? C28 C27 H27A 120.8 . . ? C26 C27 H27A 120.8 . . ? C23 C28 C27 120.4(9) . . ? C23 C28 H28A 119.8 . . ? C27 C28 H28A 119.8 . . ? C30 C29 C34 118.5(7) . . ? C30 C29 P1 120.6(5) . . ? C34 C29 P1 120.6(6) . . ? C29 C30 C31 121.2(7) . . ? C29 C30 H30A 119.4 . . ? C31 C30 H30A 119.4 . . ? C32 C31 C30 119.3(8) . . ? C32 C31 H31A 120.4 . . ? C30 C31 H31A 120.4 . . ? C31 C32 C33 120.3(8) . . ? C31 C32 H32B 119.8 . . ? C33 C32 H32B 119.8 . . ? C34 C33 C32 119.9(8) . . ? C34 C33 H33A 120.1 . . ? C32 C33 H33A 120.1 . . ? C33 C34 C29 120.8(8) . . ? C33 C34 H34A 119.6 . . ? C29 C34 H34A 119.6 . . ? C36 C35 C40 119.8(7) . . ? C36 C35 P2 121.6(6) . . ? C40 C35 P2 118.5(6) . . ? C35 C36 C37 119.0(9) . . ? C35 C36 H36A 120.5 . . ? C37 C36 H36A 120.5 . . ? C38 C37 C36 121.4(9) . . ? C38 C37 H37A 119.3 . . ? C36 C37 H37A 119.3 . . ? C37 C38 C39 120.8(9) . . ? C37 C38 H38A 119.6 . . ? C39 C38 H38A 119.6 . . ? C40 C39 C38 118.9(10) . . ? C40 C39 H39A 120.5 . . ? C38 C39 H39A 120.5 . . ? C39 C40 C35 120.0(9) . . ? C39 C40 H40A 120.0 . . ? C35 C40 H40A 120.0 . . ? C46 C41 C42 119.3(6) . . ? C46 C41 P2 119.7(5) . . ? C42 C41 P2 121.0(5) . . ? C43 C42 C41 119.0(8) . . ? C43 C42 H42A 120.5 . . ? C41 C42 H42A 120.5 . . ? C42 C43 C44 120.4(8) . . ? C42 C43 H43A 119.8 . . ? C44 C43 H43A 119.8 . . ? C45 C44 C43 120.8(8) . . ? C45 C44 H44A 119.6 . . ? C43 C44 H44A 119.6 . . ? C44 C45 C46 119.8(7) . . ? C44 C45 H45A 120.1 . . ? C46 C45 H45A 120.1 . . ? C41 C46 C45 120.8(7) . . ? C41 C46 H46A 119.6 . . ? C45 C46 H46A 119.6 . . ? C4TA O1TA C1TA 105.0(16) . . ? C2TA C1TA O1TA 110(2) . . ? C2TA C1TA H1TA 109.6 . . ? O1TA C1TA H1TA 109.6 . . ? C2TA C1TA H1TB 109.6 . . ? O1TA C1TA H1TB 109.6 . . ? H1TA C1TA H1TB 108.1 . . ? C1TA C2TA C3TA 104.1(17) . . ? C1TA C2TA H2TA 110.9 . . ? C3TA C2TA H2TA 110.9 . . ? C1TA C2TA H2TB 110.9 . . ? C3TA C2TA H2TB 110.9 . . ? H2TA C2TA H2TB 109.0 . . ? C2TA C3TA C4TA 105.6(15) . . ? C2TA C3TA H3TA 110.6 . . ? C4TA C3TA H3TA 110.6 . . ? C2TA C3TA H3TB 110.6 . . ? C4TA C3TA H3TB 110.6 . . ? H3TA C3TA H3TB 108.7 . . ? O1TA C4TA C3TA 111.0(16) . . ? O1TA C4TA H4TA 109.4 . . ? C3TA C4TA H4TA 109.4 . . ? O1TA C4TA H4TB 109.4 . . ? C3TA C4TA H4TB 109.4 . . ? H4TA C4TA H4TB 108.0 . . ? C4TB O1TB C1TB 101.8(18) . . ? C2TB C1TB O1TB 101(2) . . ? C2TB C1TB H1TC 111.5 . . ? O1TB C1TB H1TC 111.5 . . ? C2TB C1TB H1TD 111.5 . . ? O1TB C1TB H1TD 111.5 . . ? H1TC C1TB H1TD 109.4 . . ? C1TB C2TB C3TB 113(3) . . ? C1TB C2TB H2TC 109.1 . . ? C3TB C2TB H2TC 109.1 . . ? C1TB C2TB H2TD 109.1 . . ? C3TB C2TB H2TD 109.1 . . ? H2TC C2TB H2TD 107.8 . . ? C4TB C3TB C2TB 100(2) . . ? C4TB C3TB H3TC 111.8 . . ? C2TB C3TB H3TC 111.8 . . ? C4TB C3TB H3TD 111.8 . . ? C2TB C3TB H3TD 111.8 . . ? H3TC C3TB H3TD 109.5 . . ? C3TB C4TB O1TB 117(2) . . ? C3TB C4TB H4TC 108.0 . . ? O1TB C4TB H4TC 108.0 . . ? C2TB C4TB H4TC 109.6 . . ? C3TB C4TB H4TD 108.0 . . ? O1TB C4TB H4TD 108.0 . . ? C2TB C4TB H4TD 138.7 . . ? H4TC C4TB H4TD 107.2 . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 1.476 _refine_diff_density_min -1.506 _refine_diff_density_rms 0.148 data_FO3730 _database_code_depnum_ccdc_archive 'CCDC 743167' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C50 H40 P2 Pt, C6 H6' _chemical_formula_sum 'C56 H46 P2 Pt' _chemical_formula_weight 975.96 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.8366(5) _cell_length_b 12.6126(5) _cell_length_c 15.7836(9) _cell_angle_alpha 102.484(2) _cell_angle_beta 107.407(3) _cell_angle_gamma 95.895(3) _cell_volume 2159.55(18) _cell_formula_units_Z 2 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used 15004 _cell_measurement_theta_min 2.56 _cell_measurement_theta_max 27.44 _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 1.501 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 980 _exptl_absorpt_coefficient_mu 3.361 _exptl_absorpt_correction_type NONE _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 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 15004 _diffrn_reflns_av_R_equivalents 0.0365 _diffrn_reflns_av_sigmaI/netI 0.0791 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.56 _diffrn_reflns_theta_max 27.44 _reflns_number_total 9765 _reflns_number_gt 7358 _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^)+(0.0528P)^2^+0.3684P] 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 9765 _refine_ls_number_parameters 534 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0769 _refine_ls_R_factor_gt 0.0469 _refine_ls_wR_factor_ref 0.1090 _refine_ls_wR_factor_gt 0.0975 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.023 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.926132(17) 1.340653(16) 0.228686(16) 0.03507(8) Uani 1 1 d . . . P1 P 0.81771(12) 1.47739(11) 0.22342(10) 0.0357(3) Uani 1 1 d . . . P2 P 0.75588(12) 1.22115(11) 0.14017(10) 0.0346(3) Uani 1 1 d . . . C1 C 1.0790(5) 1.2772(4) 0.2736(4) 0.0411(13) Uani 1 1 d . . . C2 C 1.1056(5) 1.3830(5) 0.3054(4) 0.0398(13) Uani 1 1 d . . . C3 C 1.1934(5) 1.4803(5) 0.3620(4) 0.0439(14) Uani 1 1 d . . . C4 C 1.1857(6) 1.5805(5) 0.3363(6) 0.065(2) Uani 1 1 d . . . H4A H 1.1272 1.5801 0.2798 0.078 Uiso 1 1 calc R . . C5 C 1.2591(7) 1.6783(6) 0.3896(7) 0.078(3) Uani 1 1 d . . . H5A H 1.2475 1.7449 0.3721 0.093 Uiso 1 1 calc R . . C6 C 1.3463(7) 1.6793(6) 0.4655(7) 0.084(3) Uani 1 1 d . . . H6A H 1.3973 1.7473 0.5019 0.101 Uiso 1 1 calc R . . C7 C 1.3646(7) 1.5851(7) 0.4925(6) 0.075(2) Uani 1 1 d . . . H7A H 1.4286 1.5882 0.5469 0.090 Uiso 1 1 calc R . . C8 C 1.2890(6) 1.4827(6) 0.4403(5) 0.0648(19) Uani 1 1 d . . . C9 C 1.1172(5) 1.1696(4) 0.2659(4) 0.0383(13) Uani 1 1 d . . . C10 C 1.1542(5) 1.1267(5) 0.3420(5) 0.0468(14) Uani 1 1 d . . . H10A H 1.1542 1.1682 0.3999 0.056 Uiso 1 1 calc R . . C11 C 1.1906(6) 1.0263(5) 0.3358(5) 0.0585(17) Uani 1 1 d . . . H11A H 1.2173 1.0000 0.3892 0.070 Uiso 1 1 calc R . . C12 C 1.1882(6) 0.9644(5) 0.2523(6) 0.065(2) Uani 1 1 d . . . H12A H 1.2136 0.8949 0.2475 0.078 Uiso 1 1 calc R . . C13 C 1.1486(5) 1.0034(5) 0.1747(5) 0.0513(16) Uani 1 1 d . . . H13A H 1.1460 0.9594 0.1169 0.062 Uiso 1 1 calc R . . C14 C 1.1133(5) 1.1036(5) 0.1798(4) 0.0437(14) Uani 1 1 d . . . C15 C 1.0697(6) 1.1434(5) 0.0942(5) 0.0569(17) Uani 1 1 d . . . H15A H 1.0808 1.0918 0.0425 0.085 Uiso 1 1 calc R . . H15B H 1.1157 1.2167 0.1040 0.085 Uiso 1 1 calc R . . H15C H 0.9841 1.1476 0.0806 0.085 Uiso 1 1 calc R . . C16 C 1.3125(7) 1.3806(6) 0.4677(6) 0.077(2) Uani 1 1 d . . . H16A H 1.3236 1.3274 0.4168 0.116 Uiso 1 1 calc R . . H16B H 1.2442 1.3492 0.4828 0.116 Uiso 1 1 calc R . . H16C H 1.3855 1.3973 0.5216 0.116 Uiso 1 1 calc R . . C17 C 0.6654(5) 1.4480(5) 0.2306(4) 0.0393(13) Uani 1 1 d . . . C18 C 0.6190(5) 1.5405(5) 0.2575(4) 0.0470(14) Uani 1 1 d . . . H18A H 0.6634 1.6110 0.2649 0.056 Uiso 1 1 calc R . . C19 C 0.5080(5) 1.5349(5) 0.2745(4) 0.0501(15) Uani 1 1 d . . . H19A H 0.4775 1.6003 0.2912 0.060 Uiso 1 1 calc R . . C20 C 0.4464(5) 1.4354(5) 0.2667(4) 0.0467(14) Uani 1 1 d . . . H20A H 0.3734 1.4315 0.2803 0.056 Uiso 1 1 calc R . . C21 C 0.4876(5) 1.3364(5) 0.2388(4) 0.0432(14) Uani 1 1 d . . . C22 C 0.4196(5) 1.2342(5) 0.2318(4) 0.0489(15) Uani 1 1 d . . . H22A H 0.3475 1.2334 0.2466 0.059 Uiso 1 1 calc R . . C23 C 0.4541(5) 1.1388(5) 0.2048(4) 0.0514(16) Uani 1 1 d . . . H23A H 0.4093 1.0711 0.2034 0.062 Uiso 1 1 calc R . . C24 C 0.5570(5) 1.1396(5) 0.1787(4) 0.0452(14) Uani 1 1 d . . . H24A H 0.5786 1.0709 0.1569 0.054 Uiso 1 1 calc R . . C25 C 0.6287(4) 1.2351(4) 0.1829(4) 0.0372(12) Uani 1 1 d . . . C26 C 0.5978(5) 1.3397(4) 0.2169(4) 0.0364(12) Uani 1 1 d . . . C27 C 0.8889(5) 1.5997(4) 0.3209(4) 0.0380(12) Uani 1 1 d . . . C28 C 0.9178(5) 1.5835(5) 0.4087(4) 0.0472(14) Uani 1 1 d . . . H28A H 0.8929 1.5128 0.4158 0.057 Uiso 1 1 calc R . . C29 C 0.9816(6) 1.6671(6) 0.4854(5) 0.0587(17) Uani 1 1 d . . . H29A H 1.0001 1.6549 0.5450 0.070 Uiso 1 1 calc R . . C30 C 1.0186(6) 1.7702(6) 0.4741(5) 0.0594(18) Uani 1 1 d . . . H30A H 1.0634 1.8287 0.5264 0.071 Uiso 1 1 calc R . . C31 C 0.9911(6) 1.7875(5) 0.3885(5) 0.0550(16) Uani 1 1 d . . . H31A H 1.0174 1.8580 0.3817 0.066 Uiso 1 1 calc R . . C32 C 0.9254(5) 1.7040(5) 0.3116(5) 0.0470(14) Uani 1 1 d . . . H32A H 0.9051 1.7175 0.2524 0.056 Uiso 1 1 calc R . . C33 C 0.7937(5) 1.5279(4) 0.1201(4) 0.0369(12) Uani 1 1 d . . . C34 C 0.8928(5) 1.5499(5) 0.0917(4) 0.0464(14) Uani 1 1 d . . . H34A H 0.9702 1.5431 0.1285 0.056 Uiso 1 1 calc R . . C35 C 0.8807(5) 1.5814(5) 0.0115(4) 0.0455(14) Uani 1 1 d . . . H35A H 0.9498 1.5976 -0.0055 0.055 Uiso 1 1 calc R . . C36 C 0.7702(6) 1.5893(5) -0.0437(4) 0.0498(15) Uani 1 1 d . . . H36A H 0.7616 1.6091 -0.0998 0.060 Uiso 1 1 calc R . . C37 C 0.6712(6) 1.5680(5) -0.0168(5) 0.0551(17) Uani 1 1 d . . . H37A H 0.5940 1.5740 -0.0546 0.066 Uiso 1 1 calc R . . C38 C 0.6828(5) 1.5382(5) 0.0643(4) 0.0467(15) Uani 1 1 d . . . H38A H 0.6137 1.5246 0.0819 0.056 Uiso 1 1 calc R . . C39 C 0.6953(5) 1.2334(4) 0.0228(4) 0.0388(12) Uani 1 1 d . . . C40 C 0.7754(6) 1.2701(5) -0.0185(4) 0.0493(15) Uani 1 1 d . . . H40A H 0.8588 1.2905 0.0159 0.059 Uiso 1 1 calc R . . C41 C 0.7356(8) 1.2772(6) -0.1085(5) 0.067(2) Uani 1 1 d . . . H41A H 0.7912 1.3025 -0.1357 0.081 Uiso 1 1 calc R . . C42 C 0.6156(9) 1.2476(6) -0.1580(5) 0.074(2) Uani 1 1 d . . . H42A H 0.5885 1.2519 -0.2200 0.089 Uiso 1 1 calc R . . C43 C 0.5330(7) 1.2115(6) -0.1198(5) 0.072(2) Uani 1 1 d . . . H43A H 0.4498 1.1915 -0.1550 0.086 Uiso 1 1 calc R . . C44 C 0.5734(6) 1.2048(5) -0.0287(5) 0.0533(16) Uani 1 1 d . . . H44A H 0.5172 1.1806 -0.0017 0.064 Uiso 1 1 calc R . . C45 C 0.7667(5) 1.0751(4) 0.1249(4) 0.0379(13) Uani 1 1 d . . . C46 C 0.7148(5) 0.9948(5) 0.0420(4) 0.0452(14) Uani 1 1 d . . . H46A H 0.6682 1.0143 -0.0109 0.054 Uiso 1 1 calc R . . C47 C 0.7306(6) 0.8873(5) 0.0361(5) 0.0485(15) Uani 1 1 d . . . H47A H 0.6945 0.8331 -0.0209 0.058 Uiso 1 1 calc R . . C48 C 0.7983(6) 0.8570(5) 0.1122(5) 0.0523(16) Uani 1 1 d . . . H48A H 0.8095 0.7826 0.1072 0.063 Uiso 1 1 calc R . . C49 C 0.8496(6) 0.9354(5) 0.1951(5) 0.0527(16) Uani 1 1 d . . . H49A H 0.8946 0.9148 0.2479 0.063 Uiso 1 1 calc R . . C50 C 0.8353(5) 1.0446(5) 0.2015(4) 0.0435(13) Uani 1 1 d . . . H50A H 0.8725 1.0987 0.2583 0.052 Uiso 1 1 calc R . . C1B C 0.5546(7) 2.0072(6) 0.3854(5) 0.070(2) Uani 1 1 d . . . H1BA H 0.5028 2.0595 0.3771 0.083 Uiso 1 1 calc R . . C2B C 0.5179(7) 1.9123(6) 0.4053(5) 0.0617(18) Uani 1 1 d . . . H2BA H 0.4406 1.8992 0.4114 0.074 Uiso 1 1 calc R . . C3B C 0.5913(7) 1.8356(5) 0.4164(5) 0.0625(18) Uani 1 1 d . . . H3BA H 0.5642 1.7696 0.4300 0.075 Uiso 1 1 calc R . . C4B C 0.7026(7) 1.8527(6) 0.4084(5) 0.0648(19) Uani 1 1 d . . . H4BA H 0.7533 1.7994 0.4163 0.078 Uiso 1 1 calc R . . C5B C 0.7408(7) 1.9491(7) 0.3884(6) 0.077(2) Uani 1 1 d . . . H5BA H 0.8181 1.9618 0.3822 0.092 Uiso 1 1 calc R . . C6B C 0.6672(8) 2.0270(7) 0.3774(6) 0.082(2) Uani 1 1 d . . . H6BA H 0.6939 2.0934 0.3644 0.098 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 0.02980(11) 0.03192(12) 0.04236(14) 0.00863(9) 0.01010(9) 0.00842(8) P1 0.0317(7) 0.0324(7) 0.0405(8) 0.0086(6) 0.0083(6) 0.0081(6) P2 0.0301(7) 0.0318(7) 0.0403(8) 0.0074(6) 0.0102(6) 0.0072(6) C1 0.037(3) 0.037(3) 0.048(4) 0.006(3) 0.015(3) 0.009(2) C2 0.038(3) 0.041(3) 0.042(3) 0.010(3) 0.014(3) 0.013(2) C3 0.038(3) 0.037(3) 0.051(4) 0.001(3) 0.014(3) 0.006(2) C4 0.060(4) 0.039(3) 0.093(6) 0.011(4) 0.029(4) 0.000(3) C5 0.054(4) 0.040(4) 0.132(8) 0.009(4) 0.032(5) 0.002(3) C6 0.061(5) 0.052(5) 0.124(8) 0.005(5) 0.024(5) 0.002(4) C7 0.053(4) 0.081(5) 0.071(5) 0.014(4) -0.001(4) -0.002(4) C8 0.060(4) 0.055(4) 0.064(5) 0.002(4) 0.008(4) 0.012(3) C9 0.030(3) 0.032(3) 0.049(4) 0.006(3) 0.012(3) 0.004(2) C10 0.044(3) 0.040(3) 0.052(4) 0.012(3) 0.008(3) 0.015(3) C11 0.054(4) 0.050(4) 0.063(5) 0.018(4) 0.005(3) 0.008(3) C12 0.055(4) 0.038(3) 0.118(7) 0.029(4) 0.040(4) 0.022(3) C13 0.044(3) 0.039(3) 0.068(5) 0.002(3) 0.023(3) 0.007(3) C14 0.035(3) 0.037(3) 0.058(4) 0.004(3) 0.020(3) 0.003(2) C15 0.065(4) 0.046(4) 0.058(4) 0.007(3) 0.024(4) 0.007(3) C16 0.069(5) 0.075(5) 0.071(6) 0.020(4) -0.001(4) 0.002(4) C17 0.032(3) 0.045(3) 0.038(3) 0.009(3) 0.008(2) 0.014(2) C18 0.041(3) 0.044(3) 0.055(4) 0.011(3) 0.013(3) 0.014(3) C19 0.040(3) 0.055(4) 0.053(4) 0.007(3) 0.011(3) 0.027(3) C20 0.034(3) 0.062(4) 0.044(4) 0.009(3) 0.013(3) 0.018(3) C21 0.033(3) 0.056(4) 0.039(3) 0.010(3) 0.011(3) 0.011(3) C22 0.032(3) 0.066(4) 0.050(4) 0.016(3) 0.016(3) 0.006(3) C23 0.039(3) 0.055(4) 0.055(4) 0.011(3) 0.014(3) -0.004(3) C24 0.040(3) 0.039(3) 0.055(4) 0.010(3) 0.014(3) 0.007(3) C25 0.027(2) 0.041(3) 0.038(3) 0.006(3) 0.005(2) 0.006(2) C26 0.031(3) 0.041(3) 0.036(3) 0.010(3) 0.008(2) 0.011(2) C27 0.031(3) 0.031(3) 0.048(4) 0.007(3) 0.007(3) 0.011(2) C28 0.053(4) 0.040(3) 0.049(4) 0.015(3) 0.015(3) 0.012(3) C29 0.064(4) 0.057(4) 0.049(4) 0.008(3) 0.012(3) 0.016(3) C30 0.048(4) 0.053(4) 0.056(5) -0.007(3) 0.003(3) 0.009(3) C31 0.051(4) 0.041(3) 0.061(5) 0.006(3) 0.008(3) 0.006(3) C32 0.047(3) 0.037(3) 0.055(4) 0.010(3) 0.014(3) 0.011(3) C33 0.041(3) 0.024(2) 0.043(3) 0.007(2) 0.011(3) 0.008(2) C34 0.039(3) 0.045(3) 0.055(4) 0.011(3) 0.014(3) 0.013(3) C35 0.045(3) 0.044(3) 0.050(4) 0.017(3) 0.014(3) 0.010(3) C36 0.061(4) 0.040(3) 0.046(4) 0.013(3) 0.017(3) -0.001(3) C37 0.045(3) 0.056(4) 0.056(4) 0.025(3) 0.002(3) -0.005(3) C38 0.034(3) 0.052(3) 0.052(4) 0.023(3) 0.006(3) 0.001(3) C39 0.047(3) 0.028(3) 0.039(3) 0.005(2) 0.014(3) 0.008(2) C40 0.064(4) 0.035(3) 0.049(4) 0.007(3) 0.023(3) 0.009(3) C41 0.102(6) 0.051(4) 0.051(5) 0.013(4) 0.029(5) 0.015(4) C42 0.122(7) 0.052(4) 0.046(5) 0.012(4) 0.019(5) 0.035(5) C43 0.068(5) 0.068(5) 0.059(5) 0.012(4) -0.006(4) 0.019(4) C44 0.051(4) 0.051(4) 0.050(4) 0.011(3) 0.005(3) 0.013(3) C45 0.035(3) 0.033(3) 0.049(4) 0.012(3) 0.016(3) 0.008(2) C46 0.048(3) 0.040(3) 0.048(4) 0.012(3) 0.015(3) 0.010(3) C47 0.056(4) 0.039(3) 0.050(4) 0.006(3) 0.020(3) 0.012(3) C48 0.064(4) 0.033(3) 0.062(4) 0.011(3) 0.022(4) 0.014(3) C49 0.055(4) 0.040(3) 0.065(5) 0.020(3) 0.015(3) 0.012(3) C50 0.043(3) 0.041(3) 0.046(4) 0.011(3) 0.013(3) 0.012(3) C1B 0.081(5) 0.066(5) 0.065(5) 0.022(4) 0.020(4) 0.029(4) C2B 0.061(4) 0.058(4) 0.059(5) 0.003(4) 0.020(4) 0.004(3) C3B 0.072(5) 0.043(4) 0.063(5) 0.008(3) 0.015(4) 0.001(3) C4B 0.071(5) 0.065(4) 0.053(5) 0.010(4) 0.014(4) 0.019(4) C5B 0.074(5) 0.097(6) 0.082(6) 0.040(5) 0.044(5) 0.029(5) C6B 0.086(6) 0.081(6) 0.100(7) 0.047(5) 0.045(5) 0.019(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 C1 2.047(6) . ? Pt1 C2 2.052(6) . ? Pt1 P2 2.2507(14) . ? Pt1 P1 2.2541(14) . ? P1 C33 1.832(6) . ? P1 C27 1.841(6) . ? P1 C17 1.845(5) . ? P2 C39 1.822(6) . ? P2 C45 1.828(5) . ? P2 C25 1.834(5) . ? C1 C2 1.288(8) . ? C1 C9 1.465(7) . ? C2 C3 1.447(8) . ? C3 C8 1.396(9) . ? C3 C4 1.412(9) . ? C4 C5 1.370(9) . ? C4 H4A 0.9500 . ? C5 C6 1.323(12) . ? C5 H5A 0.9500 . ? C6 C7 1.363(11) . ? C6 H6A 0.9500 . ? C7 C8 1.417(10) . ? C7 H7A 0.9500 . ? C8 C16 1.471(10) . ? C9 C10 1.394(8) . ? C9 C14 1.417(8) . ? C10 C11 1.371(9) . ? C10 H10A 0.9500 . ? C11 C12 1.370(10) . ? C11 H11A 0.9500 . ? C12 C13 1.388(10) . ? C12 H12A 0.9500 . ? C13 C14 1.366(8) . ? C13 H13A 0.9500 . ? C14 C15 1.507(9) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C18 1.379(8) . ? C17 C26 1.448(7) . ? C18 C19 1.416(8) . ? C18 H18A 0.9500 . ? C19 C20 1.347(8) . ? C19 H19A 0.9500 . ? C20 C21 1.417(8) . ? C20 H20A 0.9500 . ? C21 C22 1.412(8) . ? C21 C26 1.445(7) . ? C22 C23 1.334(9) . ? C22 H22A 0.9500 . ? C23 C24 1.398(8) . ? C23 H23A 0.9500 . ? C24 C25 1.378(7) . ? C24 H24A 0.9500 . ? C25 C26 1.439(7) . ? C27 C28 1.389(8) . ? C27 C32 1.395(7) . ? C28 C29 1.373(9) . ? C28 H28A 0.9500 . ? C29 C30 1.395(9) . ? C29 H29A 0.9500 . ? C30 C31 1.364(10) . ? C30 H30A 0.9500 . ? C31 C32 1.379(9) . ? C31 H31A 0.9500 . ? C32 H32A 0.9500 . ? C33 C38 1.381(8) . ? C33 C34 1.399(8) . ? C34 C35 1.379(8) . ? C34 H34A 0.9500 . ? C35 C36 1.365(8) . ? C35 H35A 0.9500 . ? C36 C37 1.382(9) . ? C36 H36A 0.9500 . ? C37 C38 1.384(9) . ? C37 H37A 0.9500 . ? C38 H38A 0.9500 . ? C39 C44 1.392(8) . ? C39 C40 1.396(8) . ? C40 C41 1.383(10) . ? C40 H40A 0.9500 . ? C41 C42 1.367(11) . ? C41 H41A 0.9500 . ? C42 C43 1.380(11) . ? C42 H42A 0.9500 . ? C43 C44 1.398(10) . ? C43 H43A 0.9500 . ? C44 H44A 0.9500 . ? C45 C46 1.391(8) . ? C45 C50 1.395(8) . ? C46 C47 1.374(8) . ? C46 H46A 0.9500 . ? C47 C48 1.384(9) . ? C47 H47A 0.9500 . ? C48 C49 1.379(9) . ? C48 H48A 0.9500 . ? C49 C50 1.391(8) . ? C49 H49A 0.9500 . ? C50 H50A 0.9500 . ? C1B C2B 1.362(10) . ? C1B C6B 1.379(11) . ? C1B H1BA 0.9500 . ? C2B C3B 1.370(10) . ? C2B H2BA 0.9500 . ? C3B C4B 1.361(9) . ? C3B H3BA 0.9500 . ? C4B C5B 1.386(10) . ? C4B H4BA 0.9500 . ? C5B C6B 1.383(11) . ? C5B H5BA 0.9500 . ? C6B H6BA 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Pt1 C2 36.6(2) . . ? C1 Pt1 P2 117.72(16) . . ? C2 Pt1 P2 154.35(16) . . ? C1 Pt1 P1 154.01(16) . . ? C2 Pt1 P1 117.51(16) . . ? P2 Pt1 P1 88.10(5) . . ? C33 P1 C27 105.5(2) . . ? C33 P1 C17 104.0(3) . . ? C27 P1 C17 102.1(2) . . ? C33 P1 Pt1 114.62(18) . . ? C27 P1 Pt1 112.24(17) . . ? C17 P1 Pt1 116.95(18) . . ? C39 P2 C45 103.5(3) . . ? C39 P2 C25 102.9(3) . . ? C45 P2 C25 104.2(2) . . ? C39 P2 Pt1 115.22(18) . . ? C45 P2 Pt1 115.42(18) . . ? C25 P2 Pt1 114.00(18) . . ? C2 C1 C9 149.2(6) . . ? C2 C1 Pt1 71.9(4) . . ? C9 C1 Pt1 139.0(4) . . ? C1 C2 C3 149.1(6) . . ? C1 C2 Pt1 71.5(4) . . ? C3 C2 Pt1 139.3(4) . . ? C8 C3 C4 116.4(6) . . ? C8 C3 C2 124.8(6) . . ? C4 C3 C2 118.8(6) . . ? C5 C4 C3 122.7(8) . . ? C5 C4 H4A 118.7 . . ? C3 C4 H4A 118.7 . . ? C6 C5 C4 119.6(8) . . ? C6 C5 H5A 120.2 . . ? C4 C5 H5A 120.2 . . ? C5 C6 C7 121.5(8) . . ? C5 C6 H6A 119.3 . . ? C7 C6 H6A 119.3 . . ? C6 C7 C8 120.6(8) . . ? C6 C7 H7A 119.7 . . ? C8 C7 H7A 119.7 . . ? C3 C8 C7 118.9(7) . . ? C3 C8 C16 120.7(6) . . ? C7 C8 C16 120.3(7) . . ? C10 C9 C14 117.6(5) . . ? C10 C9 C1 121.4(5) . . ? C14 C9 C1 121.0(5) . . ? C11 C10 C9 122.1(6) . . ? C11 C10 H10A 119.0 . . ? C9 C10 H10A 119.0 . . ? C12 C11 C10 119.6(7) . . ? C12 C11 H11A 120.2 . . ? C10 C11 H11A 120.2 . . ? C11 C12 C13 119.8(6) . . ? C11 C12 H12A 120.1 . . ? C13 C12 H12A 120.1 . . ? C14 C13 C12 121.3(6) . . ? C14 C13 H13A 119.3 . . ? C12 C13 H13A 119.3 . . ? C13 C14 C9 119.6(6) . . ? C13 C14 C15 120.2(6) . . ? C9 C14 C15 120.2(5) . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C8 C16 H16A 109.5 . . ? C8 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C8 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C18 C17 C26 119.5(5) . . ? C18 C17 P1 114.4(4) . . ? C26 C17 P1 125.9(4) . . ? C17 C18 C19 122.8(5) . . ? C17 C18 H18A 118.6 . . ? C19 C18 H18A 118.6 . . ? C20 C19 C18 118.9(5) . . ? C20 C19 H19A 120.6 . . ? C18 C19 H19A 120.6 . . ? C19 C20 C21 121.7(5) . . ? C19 C20 H20A 119.1 . . ? C21 C20 H20A 119.1 . . ? C22 C21 C20 119.5(5) . . ? C22 C21 C26 120.1(5) . . ? C20 C21 C26 120.4(5) . . ? C23 C22 C21 121.6(5) . . ? C23 C22 H22A 119.2 . . ? C21 C22 H22A 119.2 . . ? C22 C23 C24 119.2(5) . . ? C22 C23 H23A 120.4 . . ? C24 C23 H23A 120.4 . . ? C25 C24 C23 123.2(6) . . ? C25 C24 H24A 118.4 . . ? C23 C24 H24A 118.4 . . ? C24 C25 C26 118.9(5) . . ? C24 C25 P2 117.5(4) . . ? C26 C25 P2 123.6(4) . . ? C25 C26 C21 116.8(5) . . ? C25 C26 C17 126.6(5) . . ? C21 C26 C17 116.6(5) . . ? C28 C27 C32 118.6(5) . . ? C28 C27 P1 117.2(4) . . ? C32 C27 P1 124.0(5) . . ? C29 C28 C27 121.7(6) . . ? C29 C28 H28A 119.2 . . ? C27 C28 H28A 119.2 . . ? C28 C29 C30 118.7(7) . . ? C28 C29 H29A 120.7 . . ? C30 C29 H29A 120.7 . . ? C31 C30 C29 120.5(6) . . ? C31 C30 H30A 119.8 . . ? C29 C30 H30A 119.8 . . ? C30 C31 C32 120.8(6) . . ? C30 C31 H31A 119.6 . . ? C32 C31 H31A 119.6 . . ? C31 C32 C27 119.9(6) . . ? C31 C32 H32A 120.1 . . ? C27 C32 H32A 120.1 . . ? C38 C33 C34 117.4(5) . . ? C38 C33 P1 124.5(4) . . ? C34 C33 P1 117.9(4) . . ? C35 C34 C33 121.4(6) . . ? C35 C34 H34A 119.3 . . ? C33 C34 H34A 119.3 . . ? C36 C35 C34 120.5(5) . . ? C36 C35 H35A 119.8 . . ? C34 C35 H35A 119.7 . . ? C35 C36 C37 119.0(6) . . ? C35 C36 H36A 120.5 . . ? C37 C36 H36A 120.5 . . ? C36 C37 C38 120.9(6) . . ? C36 C37 H37A 119.5 . . ? C38 C37 H37A 119.5 . . ? C33 C38 C37 120.8(5) . . ? C33 C38 H38A 119.6 . . ? C37 C38 H38A 119.6 . . ? C44 C39 C40 118.3(6) . . ? C44 C39 P2 123.2(5) . . ? C40 C39 P2 118.4(5) . . ? C41 C40 C39 121.2(7) . . ? C41 C40 H40A 119.4 . . ? C39 C40 H40A 119.4 . . ? C42 C41 C40 119.3(7) . . ? C42 C41 H41A 120.3 . . ? C40 C41 H41A 120.3 . . ? C41 C42 C43 121.4(7) . . ? C41 C42 H42A 119.3 . . ? C43 C42 H42A 119.3 . . ? C42 C43 C44 119.1(7) . . ? C42 C43 H43A 120.5 . . ? C44 C43 H43A 120.5 . . ? C39 C44 C43 120.6(7) . . ? C39 C44 H44A 119.7 . . ? C43 C44 H44A 119.7 . . ? C46 C45 C50 118.8(5) . . ? C46 C45 P2 124.3(4) . . ? C50 C45 P2 116.9(4) . . ? C47 C46 C45 120.4(6) . . ? C47 C46 H46A 119.8 . . ? C45 C46 H46A 119.8 . . ? C46 C47 C48 120.9(6) . . ? C46 C47 H47A 119.6 . . ? C48 C47 H47A 119.6 . . ? C49 C48 C47 119.5(6) . . ? C49 C48 H48A 120.2 . . ? C47 C48 H48A 120.2 . . ? C48 C49 C50 120.0(6) . . ? C48 C49 H49A 120.0 . . ? C50 C49 H49A 120.0 . . ? C49 C50 C45 120.5(6) . . ? C49 C50 H50A 119.8 . . ? C45 C50 H50A 119.8 . . ? C2B C1B C6B 119.9(7) . . ? C2B C1B H1BA 120.1 . . ? C6B C1B H1BA 120.1 . . ? C1B C2B C3B 120.6(7) . . ? C1B C2B H2BA 119.7 . . ? C3B C2B H2BA 119.7 . . ? C4B C3B C2B 120.7(7) . . ? C4B C3B H3BA 119.6 . . ? C2B C3B H3BA 119.6 . . ? C3B C4B C5B 119.0(7) . . ? C3B C4B H4BA 120.5 . . ? C5B C4B H4BA 120.5 . . ? C6B C5B C4B 120.5(7) . . ? C6B C5B H5BA 119.8 . . ? C4B C5B H5BA 119.8 . . ? C1B C6B C5B 119.3(7) . . ? C1B C6B H6BA 120.4 . . ? C5B C6B H6BA 120.4 . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 27.44 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 1.530 _refine_diff_density_min -1.432 _refine_diff_density_rms 0.127 data_FO3804 _database_code_depnum_ccdc_archive 'CCDC 743269' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C48 H42 P2 Pt, C6 H6' _chemical_formula_sum 'C54 H48 P2 Pt' _chemical_formula_weight 953.95 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.6006(5) _cell_length_b 12.9579(5) _cell_length_c 15.4685(5) _cell_angle_alpha 91.791(2) _cell_angle_beta 107.389(2) _cell_angle_gamma 103.098(2) _cell_volume 2148.93(14) _cell_formula_units_Z 2 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used 15688 _cell_measurement_theta_min 1.62 _cell_measurement_theta_max 27.47 _exptl_crystal_description prism _exptl_crystal_colour 'light yellow' _exptl_crystal_size_max 0.06 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.474 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 960 _exptl_absorpt_coefficient_mu 3.376 _exptl_absorpt_correction_type NONE _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 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 15688 _diffrn_reflns_av_R_equivalents 0.0470 _diffrn_reflns_av_sigmaI/netI 0.0962 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.62 _diffrn_reflns_theta_max 27.47 _reflns_number_total 9765 _reflns_number_gt 7398 _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^)+(0.0637P)^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 9765 _refine_ls_number_parameters 516 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0827 _refine_ls_R_factor_gt 0.0526 _refine_ls_wR_factor_ref 0.1226 _refine_ls_wR_factor_gt 0.1113 _refine_ls_goodness_of_fit_ref 1.011 _refine_ls_restrained_S_all 1.011 _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 0.73795(2) 0.233384(18) 0.700627(16) 0.02593(9) Uani 1 1 d . . . P1 P 0.86017(14) 0.36428(12) 0.65060(11) 0.0272(3) Uani 1 1 d . . . P2 P 0.55513(14) 0.28281(12) 0.66720(10) 0.0249(3) Uani 1 1 d . . . C1 C 0.7155(6) 0.0939(5) 0.7591(4) 0.0293(13) Uani 1 1 d . . . C2 C 0.8265(5) 0.1172(4) 0.7517(4) 0.0251(13) Uani 1 1 d . . . C3 C 0.9409(6) 0.0824(5) 0.7647(4) 0.0312(14) Uani 1 1 d . . . C4 C 1.0515(6) 0.1577(5) 0.7737(4) 0.0342(15) Uani 1 1 d . . . H4A H 1.0498 0.2301 0.7676 0.041 Uiso 1 1 calc R . . C5 C 1.1643(7) 0.1297(6) 0.7913(5) 0.0417(17) Uani 1 1 d . . . H5A H 1.2391 0.1830 0.7998 0.050 Uiso 1 1 calc R . . C6 C 1.1674(7) 0.0253(7) 0.7965(5) 0.0478(19) Uani 1 1 d . . . H6A H 1.2443 0.0057 0.8084 0.057 Uiso 1 1 calc R . . C7 C 1.0576(7) -0.0521(6) 0.7843(5) 0.0443(17) Uani 1 1 d . . . H7A H 1.0602 -0.1248 0.7861 0.053 Uiso 1 1 calc R . . C8 C 0.9436(6) -0.0257(5) 0.7694(4) 0.0357(15) Uani 1 1 d . . . C9 C 0.6255(6) 0.0221(5) 0.7932(4) 0.0286(13) Uani 1 1 d . . . C10 C 0.5097(6) -0.0325(5) 0.7341(4) 0.0323(14) Uani 1 1 d . . . H10A H 0.4892 -0.0233 0.6711 0.039 Uiso 1 1 calc R . . C11 C 0.4240(6) -0.1000(5) 0.7655(5) 0.0369(16) Uani 1 1 d . . . H11A H 0.3465 -0.1383 0.7237 0.044 Uiso 1 1 calc R . . C12 C 0.4504(7) -0.1120(6) 0.8571(5) 0.0441(18) Uani 1 1 d . . . H12A H 0.3909 -0.1574 0.8788 0.053 Uiso 1 1 calc R . . C13 C 0.5635(7) -0.0575(6) 0.9166(5) 0.0468(18) Uani 1 1 d . . . H13A H 0.5812 -0.0659 0.9796 0.056 Uiso 1 1 calc R . . C14 C 0.6535(6) 0.0100(6) 0.8872(5) 0.0403(16) Uani 1 1 d . . . C15 C 0.7782(8) 0.0680(8) 0.9531(5) 0.067(3) Uani 1 1 d . . . H15A H 0.7748 0.0654 1.0156 0.100 Uiso 1 1 calc R . . H15B H 0.7982 0.1424 0.9404 0.100 Uiso 1 1 calc R . . H15C H 0.8426 0.0338 0.9462 0.100 Uiso 1 1 calc R . . C16 C 0.8275(7) -0.1125(6) 0.7582(5) 0.0454(18) Uani 1 1 d . . . H16A H 0.8476 -0.1820 0.7588 0.068 Uiso 1 1 calc R . . H16B H 0.7647 -0.1098 0.7001 0.068 Uiso 1 1 calc R . . H16C H 0.7946 -0.1020 0.8084 0.068 Uiso 1 1 calc R . . C17 C 0.7889(6) 0.4626(5) 0.5827(4) 0.0320(14) Uani 1 1 d . . . H17A H 0.7637 0.5079 0.6229 0.038 Uiso 1 1 calc R . . H17B H 0.8529 0.5094 0.5616 0.038 Uiso 1 1 calc R . . C18 C 0.6774(6) 0.4146(5) 0.5013(4) 0.0280(13) Uani 1 1 d . . . C19 C 0.6927(6) 0.4035(5) 0.4165(4) 0.0344(15) Uani 1 1 d . . . H19A H 0.7736 0.4293 0.4114 0.041 Uiso 1 1 calc R . . C20 C 0.5972(7) 0.3572(5) 0.3397(5) 0.0412(17) Uani 1 1 d . . . H20A H 0.6119 0.3499 0.2829 0.049 Uiso 1 1 calc R . . C21 C 0.4765(7) 0.3205(5) 0.3462(5) 0.0398(16) Uani 1 1 d . . . H21A H 0.4084 0.2875 0.2940 0.048 Uiso 1 1 calc R . . C22 C 0.4594(6) 0.3333(5) 0.4297(4) 0.0357(15) Uani 1 1 d . . . H22A H 0.3778 0.3090 0.4339 0.043 Uiso 1 1 calc R . . C23 C 0.5562(5) 0.3801(5) 0.5081(4) 0.0258(13) Uani 1 1 d . . . C24 C 0.5307(6) 0.3939(5) 0.5971(4) 0.0306(14) Uani 1 1 d . . . H24A H 0.4435 0.3992 0.5846 0.037 Uiso 1 1 calc R . . H24B H 0.5861 0.4615 0.6321 0.037 Uiso 1 1 calc R . . C25 C 0.9368(6) 0.3169(5) 0.5743(4) 0.0295(14) Uani 1 1 d . . . C26 C 0.8622(6) 0.2447(5) 0.4998(4) 0.0340(15) Uani 1 1 d . . . H26A H 0.7755 0.2198 0.4911 0.041 Uiso 1 1 calc R . . C27 C 0.9135(7) 0.2082(5) 0.4374(5) 0.0403(16) Uani 1 1 d . . . H27A H 0.8613 0.1601 0.3858 0.048 Uiso 1 1 calc R . . C28 C 1.0413(7) 0.2423(6) 0.4508(5) 0.0405(17) Uani 1 1 d . . . H28A H 1.0767 0.2174 0.4088 0.049 Uiso 1 1 calc R . . C29 C 1.1150(6) 0.3123(5) 0.5257(5) 0.0397(16) Uani 1 1 d . . . H29A H 1.2022 0.3352 0.5355 0.048 Uiso 1 1 calc R . . C30 C 1.0646(6) 0.3503(5) 0.5874(4) 0.0322(14) Uani 1 1 d . . . H30A H 1.1171 0.3989 0.6386 0.039 Uiso 1 1 calc R . . C31 C 0.9893(6) 0.4539(5) 0.7397(5) 0.0332(14) Uani 1 1 d . . . C32 C 1.0224(6) 0.4270(6) 0.8274(5) 0.0383(16) Uani 1 1 d . . . H32A H 0.9779 0.3618 0.8409 0.046 Uiso 1 1 calc R . . C33 C 1.1193(7) 0.4927(6) 0.8968(5) 0.0485(19) Uani 1 1 d . . . H33A H 1.1418 0.4719 0.9567 0.058 Uiso 1 1 calc R . . C34 C 1.1834(7) 0.5896(7) 0.8775(6) 0.056(2) Uani 1 1 d . . . H34A H 1.2506 0.6349 0.9241 0.068 Uiso 1 1 calc R . . C35 C 1.1490(7) 0.6189(6) 0.7913(6) 0.053(2) Uani 1 1 d . . . H35A H 1.1916 0.6856 0.7790 0.064 Uiso 1 1 calc R . . C36 C 1.0539(6) 0.5539(5) 0.7218(5) 0.0433(17) Uani 1 1 d . . . H36A H 1.0315 0.5757 0.6623 0.052 Uiso 1 1 calc R . . C37 C 0.5065(6) 0.3212(5) 0.7645(4) 0.0308(14) Uani 1 1 d . . . C38 C 0.4351(7) 0.3935(6) 0.7608(5) 0.0447(18) Uani 1 1 d . . . H38A H 0.4086 0.4258 0.7064 0.054 Uiso 1 1 calc R . . C39 C 0.4013(8) 0.4196(6) 0.8370(6) 0.058(2) Uani 1 1 d . . . H39A H 0.3525 0.4700 0.8342 0.069 Uiso 1 1 calc R . . C40 C 0.4373(8) 0.3740(7) 0.9138(6) 0.058(2) Uani 1 1 d . . . H40A H 0.4141 0.3923 0.9651 0.070 Uiso 1 1 calc R . . C41 C 0.5082(7) 0.3002(7) 0.9189(5) 0.053(2) Uani 1 1 d . . . H41A H 0.5328 0.2674 0.9732 0.063 Uiso 1 1 calc R . . C42 C 0.5436(7) 0.2742(6) 0.8440(5) 0.0432(17) Uani 1 1 d . . . H42A H 0.5930 0.2243 0.8475 0.052 Uiso 1 1 calc R . . C43 C 0.4240(5) 0.1759(5) 0.5998(4) 0.0269(13) Uani 1 1 d . . . C44 C 0.3079(6) 0.1524(5) 0.6134(5) 0.0335(15) Uani 1 1 d . . . H44A H 0.2953 0.1911 0.6616 0.040 Uiso 1 1 calc R . . C45 C 0.2100(6) 0.0725(6) 0.5568(5) 0.0439(17) Uani 1 1 d . . . H45A H 0.1318 0.0558 0.5678 0.053 Uiso 1 1 calc R . . C46 C 0.2255(7) 0.0179(5) 0.4855(5) 0.0436(18) Uani 1 1 d . . . H46A H 0.1578 -0.0351 0.4462 0.052 Uiso 1 1 calc R . . C47 C 0.3409(7) 0.0405(5) 0.4710(5) 0.0403(16) Uani 1 1 d . . . H47A H 0.3521 0.0030 0.4216 0.048 Uiso 1 1 calc R . . C48 C 0.4395(6) 0.1178(5) 0.5286(4) 0.0316(14) Uani 1 1 d . . . H48A H 0.5187 0.1313 0.5193 0.038 Uiso 1 1 calc R . . C1BB C 0.9429(9) -0.2913(8) 0.9410(6) 0.070(3) Uani 1 1 d . . . H1BA H 1.0308 -0.2780 0.9547 0.084 Uiso 1 1 calc R . . C2BB C 0.8652(10) -0.3731(8) 0.8765(6) 0.068(3) Uani 1 1 d . . . H2BA H 0.8988 -0.4180 0.8463 0.082 Uiso 1 1 calc R . . C3BB C 0.7383(10) -0.3891(7) 0.8564(6) 0.066(3) Uani 1 1 d . . . H3BA H 0.6840 -0.4460 0.8125 0.080 Uiso 1 1 calc R . . C4BB C 0.6897(8) -0.3241(8) 0.8988(6) 0.065(3) Uani 1 1 d . . . H4BA H 0.6020 -0.3342 0.8835 0.078 Uiso 1 1 calc R . . C5BB C 0.7691(9) -0.2438(7) 0.9639(6) 0.061(2) Uani 1 1 d . . . H5BA H 0.7368 -0.1979 0.9942 0.073 Uiso 1 1 calc R . . C6BB C 0.8936(9) -0.2309(7) 0.9844(6) 0.064(2) Uani 1 1 d . . . H6BA H 0.9478 -0.1770 1.0311 0.077 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 0.02228(13) 0.02740(14) 0.02666(13) 0.00725(9) 0.00781(9) 0.00252(9) P1 0.0226(8) 0.0264(8) 0.0317(8) 0.0068(7) 0.0099(7) 0.0020(6) P2 0.0238(8) 0.0256(8) 0.0255(8) 0.0052(6) 0.0092(6) 0.0040(6) C1 0.028(3) 0.025(3) 0.026(3) 0.000(3) 0.001(3) 0.000(3) C2 0.026(3) 0.023(3) 0.025(3) 0.008(2) 0.004(3) 0.007(2) C3 0.031(3) 0.042(4) 0.020(3) 0.008(3) 0.011(3) 0.004(3) C4 0.034(4) 0.038(4) 0.028(3) 0.004(3) 0.006(3) 0.010(3) C5 0.035(4) 0.053(5) 0.040(4) 0.001(3) 0.016(3) 0.010(3) C6 0.041(4) 0.073(6) 0.040(4) 0.013(4) 0.014(3) 0.031(4) C7 0.052(5) 0.047(4) 0.038(4) 0.008(3) 0.008(4) 0.028(4) C8 0.039(4) 0.035(4) 0.035(4) 0.009(3) 0.012(3) 0.013(3) C9 0.027(3) 0.024(3) 0.039(4) 0.010(3) 0.016(3) 0.006(3) C10 0.026(3) 0.037(4) 0.030(3) 0.009(3) 0.007(3) 0.002(3) C11 0.024(3) 0.033(4) 0.050(4) 0.009(3) 0.010(3) 0.002(3) C12 0.036(4) 0.042(4) 0.061(5) 0.019(4) 0.024(4) 0.007(3) C13 0.052(5) 0.054(5) 0.038(4) 0.017(3) 0.021(4) 0.011(4) C14 0.039(4) 0.043(4) 0.037(4) 0.011(3) 0.013(3) 0.005(3) C15 0.053(5) 0.092(7) 0.035(4) 0.013(4) 0.004(4) -0.012(5) C16 0.047(4) 0.038(4) 0.054(5) 0.012(3) 0.016(4) 0.015(3) C17 0.033(3) 0.029(3) 0.034(3) 0.008(3) 0.014(3) 0.002(3) C18 0.029(3) 0.023(3) 0.035(3) 0.012(3) 0.014(3) 0.005(3) C19 0.039(4) 0.032(3) 0.040(4) 0.012(3) 0.023(3) 0.011(3) C20 0.059(5) 0.031(4) 0.038(4) 0.009(3) 0.018(4) 0.013(3) C21 0.047(4) 0.032(4) 0.032(4) 0.007(3) 0.002(3) 0.006(3) C22 0.032(3) 0.033(4) 0.039(4) 0.011(3) 0.006(3) 0.005(3) C23 0.027(3) 0.025(3) 0.027(3) 0.010(2) 0.007(3) 0.010(3) C24 0.025(3) 0.026(3) 0.042(4) 0.003(3) 0.012(3) 0.005(3) C25 0.026(3) 0.028(3) 0.036(3) 0.010(3) 0.011(3) 0.005(3) C26 0.032(3) 0.031(3) 0.037(4) 0.003(3) 0.011(3) 0.005(3) C27 0.052(4) 0.033(4) 0.036(4) 0.001(3) 0.011(3) 0.012(3) C28 0.049(4) 0.045(4) 0.038(4) 0.010(3) 0.026(4) 0.017(3) C29 0.035(4) 0.038(4) 0.051(4) 0.008(3) 0.021(3) 0.008(3) C30 0.030(3) 0.032(3) 0.032(3) 0.005(3) 0.010(3) 0.003(3) C31 0.028(3) 0.027(3) 0.040(4) -0.003(3) 0.007(3) 0.003(3) C32 0.032(4) 0.038(4) 0.042(4) -0.001(3) 0.009(3) 0.009(3) C33 0.041(4) 0.058(5) 0.036(4) -0.003(4) -0.002(3) 0.011(4) C34 0.034(4) 0.057(5) 0.058(5) -0.026(4) -0.001(4) -0.004(4) C35 0.030(4) 0.039(4) 0.081(6) -0.004(4) 0.014(4) -0.003(3) C36 0.032(4) 0.035(4) 0.058(5) 0.002(3) 0.015(4) -0.003(3) C37 0.028(3) 0.032(3) 0.031(3) 0.001(3) 0.014(3) -0.002(3) C38 0.059(5) 0.042(4) 0.045(4) 0.008(3) 0.028(4) 0.020(4) C39 0.075(6) 0.043(5) 0.074(6) 0.002(4) 0.049(5) 0.016(4) C40 0.071(6) 0.055(5) 0.046(5) -0.015(4) 0.035(4) -0.007(4) C41 0.046(4) 0.076(6) 0.030(4) 0.005(4) 0.013(3) 0.001(4) C42 0.039(4) 0.055(5) 0.032(4) 0.008(3) 0.011(3) 0.005(3) C43 0.028(3) 0.023(3) 0.026(3) 0.004(2) 0.004(3) 0.004(3) C44 0.029(3) 0.034(4) 0.038(4) 0.000(3) 0.015(3) 0.005(3) C45 0.031(4) 0.039(4) 0.058(5) 0.003(4) 0.013(4) 0.003(3) C46 0.040(4) 0.029(4) 0.042(4) -0.003(3) -0.005(3) -0.004(3) C47 0.051(4) 0.036(4) 0.029(3) 0.001(3) 0.007(3) 0.010(3) C48 0.029(3) 0.033(3) 0.031(3) 0.003(3) 0.010(3) 0.004(3) C1BB 0.054(5) 0.095(8) 0.053(5) -0.012(5) 0.013(5) 0.011(5) C2BB 0.077(7) 0.075(7) 0.058(6) -0.002(5) 0.018(5) 0.035(6) C3BB 0.083(7) 0.059(6) 0.035(4) -0.001(4) 0.003(5) -0.004(5) C4BB 0.052(5) 0.099(7) 0.039(5) 0.017(5) 0.011(4) 0.011(5) C5BB 0.071(6) 0.069(6) 0.054(5) 0.007(5) 0.031(5) 0.024(5) C6BB 0.068(6) 0.066(6) 0.052(5) -0.004(4) 0.028(5) -0.008(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 C1 2.045(6) . ? Pt1 C2 2.059(6) . ? Pt1 P1 2.2658(14) . ? Pt1 P2 2.2707(16) . ? P1 C31 1.836(7) . ? P1 C25 1.841(6) . ? P1 C17 1.858(6) . ? P2 C43 1.824(6) . ? P2 C37 1.849(6) . ? P2 C24 1.851(6) . ? C1 C2 1.295(8) . ? C1 C9 1.468(8) . ? C2 C3 1.457(9) . ? C3 C4 1.391(9) . ? C3 C8 1.412(9) . ? C4 C5 1.388(10) . ? C4 H4A 0.9500 . ? C5 C6 1.365(11) . ? C5 H5A 0.9500 . ? C6 C7 1.389(11) . ? C6 H6A 0.9500 . ? C7 C8 1.395(10) . ? C7 H7A 0.9500 . ? C8 C16 1.506(9) . ? C9 C10 1.392(9) . ? C9 C14 1.414(9) . ? C10 C11 1.381(8) . ? C10 H10A 0.9500 . ? C11 C12 1.379(10) . ? C11 H11A 0.9500 . ? C12 C13 1.373(10) . ? C12 H12A 0.9500 . ? C13 C14 1.397(9) . ? C13 H13A 0.9500 . ? C14 C15 1.509(10) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C18 1.503(9) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C19 1.382(8) . ? C18 C23 1.413(8) . ? C19 C20 1.366(10) . ? C19 H19A 0.9500 . ? C20 C21 1.408(10) . ? C20 H20A 0.9500 . ? C21 C22 1.374(9) . ? C21 H21A 0.9500 . ? C22 C23 1.390(9) . ? C22 H22A 0.9500 . ? C23 C24 1.505(8) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C26 1.386(9) . ? C25 C30 1.396(8) . ? C26 C27 1.396(9) . ? C26 H26A 0.9500 . ? C27 C28 1.397(10) . ? C27 H27A 0.9500 . ? C28 C29 1.373(10) . ? C28 H28A 0.9500 . ? C29 C30 1.390(9) . ? C29 H29A 0.9500 . ? C30 H30A 0.9500 . ? C31 C32 1.374(9) . ? C31 C36 1.422(9) . ? C32 C33 1.388(10) . ? C32 H32A 0.9500 . ? C33 C34 1.398(11) . ? C33 H33A 0.9500 . ? C34 C35 1.364(12) . ? C34 H34A 0.9500 . ? C35 C36 1.377(10) . ? C35 H35A 0.9500 . ? C36 H36A 0.9500 . ? C37 C38 1.375(10) . ? C37 C42 1.385(9) . ? C38 C39 1.405(10) . ? C38 H38A 0.9500 . ? C39 C40 1.340(12) . ? C39 H39A 0.9500 . ? C40 C41 1.385(12) . ? C40 H40A 0.9500 . ? C41 C42 1.395(10) . ? C41 H41A 0.9500 . ? C42 H42A 0.9500 . ? C43 C44 1.393(8) . ? C43 C48 1.393(9) . ? C44 C45 1.395(9) . ? C44 H44A 0.9500 . ? C45 C46 1.369(10) . ? C45 H45A 0.9500 . ? C46 C47 1.391(10) . ? C46 H46A 0.9500 . ? C47 C48 1.386(9) . ? C47 H47A 0.9500 . ? C48 H48A 0.9500 . ? C1BB C6BB 1.338(12) . ? C1BB C2BB 1.377(13) . ? C1BB H1BA 0.9500 . ? C2BB C3BB 1.375(13) . ? C2BB H2BA 0.9500 . ? C3BB C4BB 1.363(13) . ? C3BB H3BA 0.9500 . ? C4BB C5BB 1.376(13) . ? C4BB H4BA 0.9500 . ? C5BB C6BB 1.352(12) . ? C5BB H5BA 0.9500 . ? C6BB H6BA 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Pt1 C2 36.8(2) . . ? C1 Pt1 P1 149.42(18) . . ? C2 Pt1 P1 112.63(16) . . ? C1 Pt1 P2 107.78(18) . . ? C2 Pt1 P2 144.50(16) . . ? P1 Pt1 P2 102.79(5) . . ? C31 P1 C25 103.8(3) . . ? C31 P1 C17 100.6(3) . . ? C25 P1 C17 100.7(3) . . ? C31 P1 Pt1 115.6(2) . . ? C25 P1 Pt1 114.68(19) . . ? C17 P1 Pt1 119.1(2) . . ? C43 P2 C37 104.0(3) . . ? C43 P2 C24 100.4(3) . . ? C37 P2 C24 100.8(3) . . ? C43 P2 Pt1 111.8(2) . . ? C37 P2 Pt1 117.0(2) . . ? C24 P2 Pt1 120.47(19) . . ? C2 C1 C9 146.8(6) . . ? C2 C1 Pt1 72.2(3) . . ? C9 C1 Pt1 140.8(5) . . ? C1 C2 C3 145.5(6) . . ? C1 C2 Pt1 71.0(4) . . ? C3 C2 Pt1 143.3(4) . . ? C4 C3 C8 118.7(6) . . ? C4 C3 C2 119.3(6) . . ? C8 C3 C2 122.0(6) . . ? C5 C4 C3 121.6(7) . . ? C5 C4 H4A 119.2 . . ? C3 C4 H4A 119.2 . . ? C6 C5 C4 119.8(7) . . ? C6 C5 H5A 120.1 . . ? C4 C5 H5A 120.1 . . ? C5 C6 C7 119.7(7) . . ? C5 C6 H6A 120.1 . . ? C7 C6 H6A 120.1 . . ? C6 C7 C8 121.6(7) . . ? C6 C7 H7A 119.2 . . ? C8 C7 H7A 119.2 . . ? C7 C8 C3 118.5(6) . . ? C7 C8 C16 119.6(6) . . ? C3 C8 C16 122.0(6) . . ? C10 C9 C14 118.8(5) . . ? C10 C9 C1 120.6(5) . . ? C14 C9 C1 120.5(6) . . ? C11 C10 C9 121.2(6) . . ? C11 C10 H10A 119.4 . . ? C9 C10 H10A 119.4 . . ? C12 C11 C10 120.3(6) . . ? C12 C11 H11A 119.8 . . ? C10 C11 H11A 119.8 . . ? C13 C12 C11 119.3(6) . . ? C13 C12 H12A 120.3 . . ? C11 C12 H12A 120.3 . . ? C12 C13 C14 122.0(7) . . ? C12 C13 H13A 119.0 . . ? C14 C13 H13A 119.0 . . ? C13 C14 C9 118.3(6) . . ? C13 C14 C15 121.5(6) . . ? C9 C14 C15 120.2(6) . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C8 C16 H16A 109.5 . . ? C8 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C8 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C18 C17 P1 114.7(4) . . ? C18 C17 H17A 108.6 . . ? P1 C17 H17A 108.6 . . ? C18 C17 H17B 108.6 . . ? P1 C17 H17B 108.6 . . ? H17A C17 H17B 107.6 . . ? C19 C18 C23 118.3(6) . . ? C19 C18 C17 119.5(5) . . ? C23 C18 C17 122.2(5) . . ? C20 C19 C18 123.2(6) . . ? C20 C19 H19A 118.4 . . ? C18 C19 H19A 118.4 . . ? C19 C20 C21 118.8(6) . . ? C19 C20 H20A 120.6 . . ? C21 C20 H20A 120.6 . . ? C22 C21 C20 118.6(6) . . ? C22 C21 H21A 120.7 . . ? C20 C21 H21A 120.7 . . ? C21 C22 C23 122.9(6) . . ? C21 C22 H22A 118.6 . . ? C23 C22 H22A 118.6 . . ? C22 C23 C18 118.1(5) . . ? C22 C23 C24 120.3(5) . . ? C18 C23 C24 121.6(5) . . ? C23 C24 P2 112.7(4) . . ? C23 C24 H24A 109.0 . . ? P2 C24 H24A 109.0 . . ? C23 C24 H24B 109.0 . . ? P2 C24 H24B 109.0 . . ? H24A C24 H24B 107.8 . . ? C26 C25 C30 119.0(6) . . ? C26 C25 P1 117.5(5) . . ? C30 C25 P1 123.5(5) . . ? C25 C26 C27 120.5(6) . . ? C25 C26 H26A 119.8 . . ? C27 C26 H26A 119.8 . . ? C26 C27 C28 120.2(6) . . ? C26 C27 H27A 119.9 . . ? C28 C27 H27A 119.9 . . ? C29 C28 C27 119.0(6) . . ? C29 C28 H28A 120.5 . . ? C27 C28 H28A 120.5 . . ? C28 C29 C30 121.3(6) . . ? C28 C29 H29A 119.4 . . ? C30 C29 H29A 119.4 . . ? C29 C30 C25 120.1(6) . . ? C29 C30 H30A 120.0 . . ? C25 C30 H30A 120.0 . . ? C32 C31 C36 118.2(6) . . ? C32 C31 P1 119.9(5) . . ? C36 C31 P1 121.8(5) . . ? C31 C32 C33 121.7(7) . . ? C31 C32 H32A 119.2 . . ? C33 C32 H32A 119.2 . . ? C32 C33 C34 119.3(7) . . ? C32 C33 H33A 120.4 . . ? C34 C33 H33A 120.4 . . ? C35 C34 C33 119.6(7) . . ? C35 C34 H34A 120.2 . . ? C33 C34 H34A 120.2 . . ? C34 C35 C36 121.6(7) . . ? C34 C35 H35A 119.2 . . ? C36 C35 H35A 119.2 . . ? C35 C36 C31 119.6(7) . . ? C35 C36 H36A 120.2 . . ? C31 C36 H36A 120.2 . . ? C38 C37 C42 119.2(6) . . ? C38 C37 P2 122.9(5) . . ? C42 C37 P2 118.0(5) . . ? C37 C38 C39 120.2(7) . . ? C37 C38 H38A 119.9 . . ? C39 C38 H38A 119.9 . . ? C40 C39 C38 120.4(8) . . ? C40 C39 H39A 119.8 . . ? C38 C39 H39A 119.8 . . ? C39 C40 C41 120.3(7) . . ? C39 C40 H40A 119.8 . . ? C41 C40 H40A 119.8 . . ? C40 C41 C42 119.8(7) . . ? C40 C41 H41A 120.1 . . ? C42 C41 H41A 120.1 . . ? C37 C42 C41 120.0(7) . . ? C37 C42 H42A 120.0 . . ? C41 C42 H42A 120.0 . . ? C44 C43 C48 118.4(6) . . ? C44 C43 P2 123.4(5) . . ? C48 C43 P2 118.1(4) . . ? C43 C44 C45 120.4(6) . . ? C43 C44 H44A 119.8 . . ? C45 C44 H44A 119.8 . . ? C46 C45 C44 120.6(6) . . ? C46 C45 H45A 119.7 . . ? C44 C45 H45A 119.7 . . ? C45 C46 C47 119.7(6) . . ? C45 C46 H46A 120.2 . . ? C47 C46 H46A 120.2 . . ? C48 C47 C46 120.0(6) . . ? C48 C47 H47A 120.0 . . ? C46 C47 H47A 120.0 . . ? C47 C48 C43 120.9(6) . . ? C47 C48 H48A 119.6 . . ? C43 C48 H48A 119.6 . . ? C6BB C1BB C2BB 119.4(9) . . ? C6BB C1BB H1BA 120.3 . . ? C2BB C1BB H1BA 120.3 . . ? C3BB C2BB C1BB 119.2(9) . . ? C3BB C2BB H2BA 120.4 . . ? C1BB C2BB H2BA 120.4 . . ? C4BB C3BB C2BB 120.6(8) . . ? C4BB C3BB H3BA 119.7 . . ? C2BB C3BB H3BA 119.7 . . ? C3BB C4BB C5BB 119.3(9) . . ? C3BB C4BB H4BA 120.4 . . ? C5BB C4BB H4BA 120.4 . . ? C6BB C5BB C4BB 119.3(8) . . ? C6BB C5BB H5BA 120.4 . . ? C4BB C5BB H5BA 120.4 . . ? C1BB C6BB C5BB 122.2(9) . . ? C1BB C6BB H6BA 118.9 . . ? C5BB C6BB H6BA 118.9 . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.657 _refine_diff_density_min -1.741 _refine_diff_density_rms 0.160