# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _publ_contact_author_name 'Mairi F Haddow' _publ_contact_author_email Mairi.Haddow@bristol.ac.uk loop_ _publ_author_name 'Tamara Fanjul' 'Graham Eastham' 'Joelle Floure' 'Sebastian J. K. Forrest' 'Mairi F. Haddow' ; A.Hamilton ; 'Paul G. Pringle' 'A. Guy Orpen' 'Mark Waugh' data_1 _database_code_depnum_ccdc_archive 'CCDC 897390' #TrackingRef '- all.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H44 Cl2 P2 Pt, C H Cl3' _chemical_formula_sum 'C25 H45 Cl5 P2 Pt' _chemical_formula_weight 779.89 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _space_group_name_H-M_alt P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 7.4494(2) _cell_length_b 22.2352(7) _cell_length_c 18.5251(6) _cell_angle_alpha 90.00 _cell_angle_beta 95.723(2) _cell_angle_gamma 90.00 _cell_volume 3053.18(16) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 4969 _cell_measurement_theta_min 2.75 _cell_measurement_theta_max 23.38 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.697 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1552 _exptl_absorpt_coefficient_mu 5.152 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.223543 _exptl_absorpt_correction_T_max 0.434574 _exptl_absorpt_process_details 'TWINABS 2008/4' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Apex II kappa CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 10671 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.1388 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.39 _diffrn_reflns_theta_max 32.43 _reflns_number_total 10671 _reflns_number_gt 6997 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Apex II (Bruker, 2008)' _computing_cell_refinement 'Apex II (Bruker, 2008)' _computing_data_reduction 'SAINT V7.68A (Bruker, 2010)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0715P)^2^+15.6251P] 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 10671 _refine_ls_number_parameters 311 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1424 _refine_ls_R_factor_gt 0.0837 _refine_ls_wR_factor_ref 0.1808 _refine_ls_wR_factor_gt 0.1602 _refine_ls_goodness_of_fit_ref 1.075 _refine_ls_restrained_S_all 1.075 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.57262(5) 0.649781(18) 0.740173(19) 0.02484(10) Uani 1 1 d . . . P1 P 0.7567(5) 0.57709(12) 0.79163(15) 0.0331(7) Uani 1 1 d . . . P2 P 0.7434(3) 0.73616(10) 0.75421(13) 0.0203(5) Uani 1 1 d . . . Cl1 Cl 0.3462(4) 0.70388(16) 0.66921(16) 0.0451(8) Uani 1 1 d . . . Cl2 Cl 0.3516(6) 0.57629(18) 0.7212(2) 0.0635(11) Uani 1 1 d . . . C1 C 0.9921(16) 0.5963(5) 0.8187(6) 0.038(3) Uani 1 1 d . . . H1A H 1.0530 0.5582 0.8343 0.046 Uiso 1 1 calc R . . H1B H 1.0439 0.6090 0.7740 0.046 Uiso 1 1 calc R . . C2 C 1.0525(15) 0.6424(5) 0.8759(5) 0.030(2) Uani 1 1 d . . . C3 C 1.0469(12) 0.7038(4) 0.8630(5) 0.0206(19) Uani 1 1 d . . . C4 C 0.9873(13) 0.7296(5) 0.7890(5) 0.024(2) Uani 1 1 d . . . H4A H 1.0458 0.7052 0.7533 0.028 Uiso 1 1 calc R . . H4B H 1.0394 0.7705 0.7877 0.028 Uiso 1 1 calc R . . C5 C 1.1193(16) 0.7434(4) 0.9180(5) 0.029(2) Uani 1 1 d . . . H5 H 1.1147 0.7855 0.9090 0.034 Uiso 1 1 calc R . . C6 C 1.1961(13) 0.7232(5) 0.9839(5) 0.027(2) Uani 1 1 d . . . H6 H 1.2421 0.7509 1.0203 0.033 Uiso 1 1 calc R . . C7 C 1.2054(17) 0.6623(5) 0.9966(6) 0.040(3) Uani 1 1 d . . . H7 H 1.2602 0.6472 1.0415 0.047 Uiso 1 1 calc R . . C8 C 1.134(2) 0.6232(6) 0.9431(6) 0.048(3) Uani 1 1 d . . . H8 H 1.1400 0.5812 0.9526 0.057 Uiso 1 1 calc R . . C9 C 0.678(3) 0.5414(6) 0.8762(7) 0.060(5) Uani 1 1 d . . . C10 C 0.659(2) 0.5936(7) 0.9298(7) 0.062(4) Uani 1 1 d . . . H10A H 0.6263 0.5776 0.9760 0.093 Uiso 1 1 calc R . . H10B H 0.5655 0.6214 0.9095 0.093 Uiso 1 1 calc R . . H10C H 0.7746 0.6150 0.9380 0.093 Uiso 1 1 calc R . . C11 C 0.810(3) 0.4949(6) 0.9095(8) 0.088(7) Uani 1 1 d . . . H11A H 0.9307 0.5129 0.9175 0.132 Uiso 1 1 calc R . . H11B H 0.8134 0.4606 0.8765 0.132 Uiso 1 1 calc R . . H11C H 0.7722 0.4813 0.9559 0.132 Uiso 1 1 calc R . . C12 C 0.489(3) 0.5125(8) 0.8646(9) 0.089(7) Uani 1 1 d . . . H12A H 0.4898 0.4798 0.8292 0.133 Uiso 1 1 calc R . . H12B H 0.4001 0.5429 0.8464 0.133 Uiso 1 1 calc R . . H12C H 0.4558 0.4964 0.9108 0.133 Uiso 1 1 calc R . . C13 C 0.796(2) 0.5171(5) 0.7212(6) 0.047(3) Uani 1 1 d . . . C14 C 0.962(2) 0.4799(7) 0.7387(8) 0.062(4) Uani 1 1 d . . . H14A H 0.9551 0.4436 0.7087 0.094 Uiso 1 1 calc R . . H14B H 0.9728 0.4686 0.7901 0.094 Uiso 1 1 calc R . . H14C H 1.0686 0.5034 0.7287 0.094 Uiso 1 1 calc R . . C15 C 0.644(3) 0.4690(7) 0.7123(9) 0.086(7) Uani 1 1 d . . . H15A H 0.6525 0.4466 0.6672 0.128 Uiso 1 1 calc R . . H15B H 0.5263 0.4888 0.7106 0.128 Uiso 1 1 calc R . . H15C H 0.6581 0.4412 0.7535 0.128 Uiso 1 1 calc R . . C16 C 0.812(2) 0.5512(6) 0.6494(6) 0.060(5) Uani 1 1 d . . . H16A H 0.8969 0.5847 0.6583 0.090 Uiso 1 1 calc R . . H16B H 0.6934 0.5669 0.6307 0.090 Uiso 1 1 calc R . . H16C H 0.8557 0.5237 0.6137 0.090 Uiso 1 1 calc R . . C17 C 0.6455(13) 0.7897(5) 0.8185(5) 0.024(2) Uani 1 1 d . . . C18 C 0.4441(16) 0.8051(5) 0.7947(6) 0.033(2) Uani 1 1 d . . . H18A H 0.3953 0.8293 0.8324 0.050 Uiso 1 1 calc R . . H18B H 0.3746 0.7678 0.7874 0.050 Uiso 1 1 calc R . . H18C H 0.4359 0.8280 0.7492 0.050 Uiso 1 1 calc R . . C19 C 0.7513(16) 0.8483(5) 0.8287(6) 0.037(2) Uani 1 1 d . . . H19A H 0.7011 0.8728 0.8657 0.056 Uiso 1 1 calc R . . H19B H 0.7429 0.8704 0.7827 0.056 Uiso 1 1 calc R . . H19C H 0.8781 0.8393 0.8442 0.056 Uiso 1 1 calc R . . C20 C 0.6454(16) 0.7565(5) 0.8922(5) 0.031(2) Uani 1 1 d . . . H20A H 0.7689 0.7448 0.9096 0.047 Uiso 1 1 calc R . . H20B H 0.5696 0.7205 0.8858 0.047 Uiso 1 1 calc R . . H20C H 0.5975 0.7833 0.9277 0.047 Uiso 1 1 calc R . . C21 C 0.7790(15) 0.7749(4) 0.6641(5) 0.028(2) Uani 1 1 d . . . C22 C 0.7967(17) 0.7228(5) 0.6085(5) 0.031(2) Uani 1 1 d . . . H22A H 0.6846 0.6994 0.6030 0.047 Uiso 1 1 calc R . . H22B H 0.8972 0.6965 0.6262 0.047 Uiso 1 1 calc R . . H22C H 0.8194 0.7398 0.5615 0.047 Uiso 1 1 calc R . . C23 C 0.6204(18) 0.8149(5) 0.6345(6) 0.043(3) Uani 1 1 d . . . H23A H 0.6169 0.8510 0.6647 0.065 Uiso 1 1 calc R . . H23B H 0.5072 0.7926 0.6353 0.065 Uiso 1 1 calc R . . H23C H 0.6360 0.8267 0.5845 0.065 Uiso 1 1 calc R . . C24 C 0.9525(15) 0.8137(5) 0.6665(5) 0.029(2) Uani 1 1 d . . . H24A H 0.9592 0.8329 0.6192 0.044 Uiso 1 1 calc R . . H24B H 1.0585 0.7880 0.6779 0.044 Uiso 1 1 calc R . . H24C H 0.9494 0.8447 0.7039 0.044 Uiso 1 1 calc R . . C25 C 0.254(2) 0.5887(5) 0.5380(5) 0.040(3) Uani 1 1 d . . . H25 H 0.2655 0.6054 0.5884 0.048 Uiso 1 1 calc R . . Cl3 Cl 0.2708(7) 0.50963(13) 0.54387(16) 0.0572(10) Uani 1 1 d . . . Cl4 Cl 0.4327(5) 0.61719(14) 0.49256(18) 0.0494(8) Uani 1 1 d . . . Cl5 Cl 0.0457(6) 0.61086(17) 0.4953(2) 0.0619(11) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.02812(17) 0.02717(16) 0.01896(14) -0.00157(17) 0.00102(14) -0.0041(2) P1 0.056(2) 0.0174(12) 0.0235(12) 0.0004(10) -0.0081(12) -0.0016(12) P2 0.0257(12) 0.0161(10) 0.0190(11) -0.0001(9) 0.0021(9) -0.0008(9) Cl1 0.0389(16) 0.062(2) 0.0321(14) -0.0157(13) -0.0074(12) 0.0207(14) Cl2 0.075(3) 0.066(2) 0.0490(19) 0.0036(17) 0.0004(18) -0.035(2) C1 0.045(7) 0.022(5) 0.042(6) -0.005(4) -0.022(5) 0.011(5) C2 0.042(6) 0.024(5) 0.023(4) 0.005(4) -0.007(4) 0.001(4) C3 0.019(4) 0.023(4) 0.019(4) 0.001(3) 0.000(3) -0.003(4) C4 0.021(5) 0.029(5) 0.019(4) 0.004(4) -0.003(4) 0.000(4) C5 0.035(6) 0.021(5) 0.029(5) -0.003(4) 0.001(5) -0.003(4) C6 0.019(5) 0.039(6) 0.023(5) -0.009(4) -0.001(4) -0.001(4) C7 0.050(7) 0.038(7) 0.027(5) 0.004(4) -0.012(5) -0.013(5) C8 0.067(9) 0.031(6) 0.041(6) 0.002(5) -0.022(7) 0.007(6) C9 0.109(14) 0.039(7) 0.029(6) 0.011(5) -0.010(7) -0.024(8) C10 0.093(13) 0.060(9) 0.035(7) 0.013(6) 0.014(7) -0.009(9) C11 0.18(2) 0.042(8) 0.036(7) 0.018(6) -0.019(11) 0.011(11) C12 0.119(16) 0.084(13) 0.061(10) 0.043(9) -0.002(11) -0.053(12) C13 0.074(9) 0.023(5) 0.040(6) -0.008(5) -0.009(7) 0.002(6) C14 0.072(10) 0.050(8) 0.059(9) -0.008(7) -0.022(8) 0.036(8) C15 0.15(2) 0.041(8) 0.061(9) -0.028(7) 0.000(11) -0.029(11) C16 0.110(13) 0.040(7) 0.026(5) -0.012(5) -0.004(7) 0.033(8) C17 0.022(5) 0.026(5) 0.024(5) -0.002(4) 0.004(4) 0.004(4) C18 0.038(6) 0.030(5) 0.031(5) -0.003(4) 0.005(5) 0.009(5) C19 0.048(7) 0.026(5) 0.038(6) -0.014(5) 0.005(5) -0.004(6) C20 0.042(7) 0.030(5) 0.023(5) -0.003(4) 0.011(5) 0.006(5) C21 0.033(6) 0.025(5) 0.025(5) 0.001(4) 0.002(5) 0.003(5) C22 0.039(6) 0.033(5) 0.022(5) -0.003(4) 0.000(5) -0.006(5) C23 0.058(8) 0.037(6) 0.033(6) 0.010(5) -0.003(6) 0.012(6) C24 0.037(6) 0.027(5) 0.025(5) 0.007(4) 0.006(4) -0.002(5) C25 0.070(9) 0.025(5) 0.022(5) 0.002(4) -0.009(6) -0.017(6) Cl3 0.110(3) 0.0246(13) 0.0358(15) 0.0001(11) 0.0003(19) -0.0099(18) Cl4 0.068(2) 0.0372(16) 0.0457(17) -0.0014(13) 0.0165(16) -0.0135(15) Cl5 0.063(2) 0.057(2) 0.062(2) 0.0238(18) -0.0132(18) -0.0168(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 P1 2.267(3) . ? Pt1 P2 2.304(2) . ? Pt1 Cl2 2.321(4) . ? Pt1 Cl1 2.362(3) . ? P1 C1 1.826(12) . ? P1 C9 1.902(13) . ? P1 C13 1.909(12) . ? P2 C4 1.872(10) . ? P2 C17 1.882(10) . ? P2 C21 1.920(10) . ? C1 C2 1.509(14) . ? C2 C3 1.387(13) . ? C2 C8 1.395(14) . ? C3 C5 1.412(13) . ? C3 C4 1.511(12) . ? C5 C6 1.372(14) . ? C6 C7 1.376(15) . ? C7 C8 1.385(16) . ? C9 C11 1.52(2) . ? C9 C10 1.54(2) . ? C9 C12 1.54(2) . ? C13 C14 1.501(19) . ? C13 C16 1.547(18) . ? C13 C15 1.55(2) . ? C17 C19 1.523(15) . ? C17 C20 1.552(14) . ? C17 C18 1.559(15) . ? C21 C23 1.537(16) . ? C21 C24 1.551(15) . ? C21 C22 1.565(14) . ? C25 Cl5 1.739(14) . ? C25 Cl4 1.764(14) . ? C25 Cl3 1.766(11) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P1 Pt1 P2 104.06(10) . . ? P1 Pt1 Cl2 87.24(14) . . ? P2 Pt1 Cl2 168.26(13) . . ? P1 Pt1 Cl1 164.91(11) . . ? P2 Pt1 Cl1 89.64(11) . . ? Cl2 Pt1 Cl1 79.51(14) . . ? C1 P1 C9 103.8(7) . . ? C1 P1 C13 98.3(6) . . ? C9 P1 C13 110.6(6) . . ? C1 P1 Pt1 118.2(4) . . ? C9 P1 Pt1 114.8(6) . . ? C13 P1 Pt1 109.7(4) . . ? C4 P2 C17 104.8(5) . . ? C4 P2 C21 96.9(5) . . ? C17 P2 C21 111.2(4) . . ? C4 P2 Pt1 118.7(3) . . ? C17 P2 Pt1 110.8(3) . . ? C21 P2 Pt1 113.5(3) . . ? C2 C1 P1 124.2(9) . . ? C3 C2 C8 117.2(10) . . ? C3 C2 C1 123.1(9) . . ? C8 C2 C1 119.4(10) . . ? C2 C3 C5 119.2(9) . . ? C2 C3 C4 122.1(9) . . ? C5 C3 C4 118.3(9) . . ? C3 C4 P2 122.0(7) . . ? C6 C5 C3 122.2(9) . . ? C5 C6 C7 119.0(10) . . ? C6 C7 C8 119.1(10) . . ? C7 C8 C2 123.3(11) . . ? C11 C9 C10 110.3(12) . . ? C11 C9 C12 108.7(13) . . ? C10 C9 C12 105.4(16) . . ? C11 C9 P1 112.1(13) . . ? C10 C9 P1 105.7(8) . . ? C12 C9 P1 114.3(9) . . ? C14 C13 C16 108.7(13) . . ? C14 C13 C15 102.8(12) . . ? C16 C13 C15 111.5(12) . . ? C14 C13 P1 114.6(9) . . ? C16 C13 P1 105.9(7) . . ? C15 C13 P1 113.4(11) . . ? C19 C17 C20 110.1(9) . . ? C19 C17 C18 108.6(9) . . ? C20 C17 C18 105.6(8) . . ? C19 C17 P2 113.0(7) . . ? C20 C17 P2 106.9(7) . . ? C18 C17 P2 112.5(7) . . ? C23 C21 C24 107.2(9) . . ? C23 C21 C22 107.8(9) . . ? C24 C21 C22 107.8(9) . . ? C23 C21 P2 113.7(8) . . ? C24 C21 P2 114.3(7) . . ? C22 C21 P2 105.6(7) . . ? Cl5 C25 Cl4 111.3(6) . . ? Cl5 C25 Cl3 111.4(7) . . ? Cl4 C25 Cl3 109.4(8) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag P2 Pt1 P1 C1 -8.6(5) . . . . ? Cl2 Pt1 P1 C1 174.6(5) . . . . ? Cl1 Pt1 P1 C1 146.1(6) . . . . ? P2 Pt1 P1 C9 114.5(5) . . . . ? Cl2 Pt1 P1 C9 -62.3(5) . . . . ? Cl1 Pt1 P1 C9 -90.7(6) . . . . ? P2 Pt1 P1 C13 -120.1(5) . . . . ? Cl2 Pt1 P1 C13 63.1(5) . . . . ? Cl1 Pt1 P1 C13 34.6(7) . . . . ? P1 Pt1 P2 C4 8.2(4) . . . . ? Cl2 Pt1 P2 C4 172.3(6) . . . . ? Cl1 Pt1 P2 C4 -165.4(4) . . . . ? P1 Pt1 P2 C17 -113.0(3) . . . . ? Cl2 Pt1 P2 C17 51.1(7) . . . . ? Cl1 Pt1 P2 C17 73.3(3) . . . . ? P1 Pt1 P2 C21 121.0(4) . . . . ? Cl2 Pt1 P2 C21 -74.9(7) . . . . ? Cl1 Pt1 P2 C21 -52.6(4) . . . . ? C9 P1 C1 C2 -65.4(11) . . . . ? C13 P1 C1 C2 -179.1(9) . . . . ? Pt1 P1 C1 C2 63.1(11) . . . . ? P1 C1 C2 C3 -78.6(14) . . . . ? P1 C1 C2 C8 107.5(13) . . . . ? C8 C2 C3 C5 -1.1(16) . . . . ? C1 C2 C3 C5 -175.1(11) . . . . ? C8 C2 C3 C4 171.1(11) . . . . ? C1 C2 C3 C4 -2.9(17) . . . . ? C2 C3 C4 P2 79.3(12) . . . . ? C5 C3 C4 P2 -108.5(10) . . . . ? C17 P2 C4 C3 63.1(9) . . . . ? C21 P2 C4 C3 177.2(8) . . . . ? Pt1 P2 C4 C3 -61.2(9) . . . . ? C2 C3 C5 C6 0.2(16) . . . . ? C4 C3 C5 C6 -172.2(10) . . . . ? C3 C5 C6 C7 1.0(17) . . . . ? C5 C6 C7 C8 -1.3(19) . . . . ? C6 C7 C8 C2 0(2) . . . . ? C3 C2 C8 C7 1(2) . . . . ? C1 C2 C8 C7 175.0(13) . . . . ? C1 P1 C9 C11 -47.3(11) . . . . ? C13 P1 C9 C11 57.3(12) . . . . ? Pt1 P1 C9 C11 -177.8(9) . . . . ? C1 P1 C9 C10 73.0(12) . . . . ? C13 P1 C9 C10 177.5(11) . . . . ? Pt1 P1 C9 C10 -57.6(12) . . . . ? C1 P1 C9 C12 -171.5(12) . . . . ? C13 P1 C9 C12 -67.0(14) . . . . ? Pt1 P1 C9 C12 57.9(13) . . . . ? C1 P1 C13 C14 34.3(12) . . . . ? C9 P1 C13 C14 -73.9(13) . . . . ? Pt1 P1 C13 C14 158.4(10) . . . . ? C1 P1 C13 C16 -85.6(11) . . . . ? C9 P1 C13 C16 166.2(11) . . . . ? Pt1 P1 C13 C16 38.5(12) . . . . ? C1 P1 C13 C15 151.9(11) . . . . ? C9 P1 C13 C15 43.7(13) . . . . ? Pt1 P1 C13 C15 -84.0(10) . . . . ? C4 P2 C17 C19 52.0(8) . . . . ? C21 P2 C17 C19 -51.7(9) . . . . ? Pt1 P2 C17 C19 -178.9(7) . . . . ? C4 P2 C17 C20 -69.2(8) . . . . ? C21 P2 C17 C20 -172.9(7) . . . . ? Pt1 P2 C17 C20 59.9(7) . . . . ? C4 P2 C17 C18 175.4(7) . . . . ? C21 P2 C17 C18 71.7(9) . . . . ? Pt1 P2 C17 C18 -55.5(8) . . . . ? C4 P2 C21 C23 -152.4(8) . . . . ? C17 P2 C21 C23 -43.5(9) . . . . ? Pt1 P2 C21 C23 82.2(8) . . . . ? C4 P2 C21 C24 -28.7(8) . . . . ? C17 P2 C21 C24 80.2(8) . . . . ? Pt1 P2 C21 C24 -154.1(6) . . . . ? C4 P2 C21 C22 89.6(8) . . . . ? C17 P2 C21 C22 -161.5(7) . . . . ? Pt1 P2 C21 C22 -35.8(8) . . . . ? _diffrn_measured_fraction_theta_max 0.962 _diffrn_reflns_theta_full 32.43 _diffrn_measured_fraction_theta_full 0.962 _refine_diff_density_max 5.077 _refine_diff_density_min -4.063 _refine_diff_density_rms 0.313 data_2a _database_code_depnum_ccdc_archive 'CCDC 897391' #TrackingRef '- all.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C23 H42 Cl2 P2 Pt, C H2 Cl2' _chemical_formula_sum 'C24 H44 Cl4 P2 Pt' _chemical_formula_weight 731.42 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.4152(5) _cell_length_b 21.8460(10) _cell_length_c 15.4768(7) _cell_angle_alpha 90.00 _cell_angle_beta 115.504(3) _cell_angle_gamma 90.00 _cell_volume 2873.1(2) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9838 _cell_measurement_theta_min 2.40 _cell_measurement_theta_max 27.53 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.691 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1456 _exptl_absorpt_coefficient_mu 5.379 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4543 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_process_details 'SADABS V2008/1' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Apex II kappa CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 48854 _diffrn_reflns_av_R_equivalents 0.0225 _diffrn_reflns_av_sigmaI/netI 0.0131 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.73 _diffrn_reflns_theta_max 27.54 _reflns_number_total 6613 _reflns_number_gt 5834 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker Apex2' _computing_cell_refinement 'Bruker Apex2' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker ShelXTL' _computing_publication_material 'Bruker ShelXTL' _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^)+(0.0135P)^2^+11.4984P] 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 6613 _refine_ls_number_parameters 292 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0266 _refine_ls_R_factor_gt 0.0216 _refine_ls_wR_factor_ref 0.0566 _refine_ls_wR_factor_gt 0.0545 _refine_ls_goodness_of_fit_ref 1.143 _refine_ls_restrained_S_all 1.143 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 1.112185(14) 0.248331(6) 0.193403(8) 0.01281(4) Uani 1 1 d . . . P1 P 0.86770(10) 0.21420(4) 0.10015(6) 0.01470(16) Uani 1 1 d . . . P2 P 1.07386(10) 0.34700(4) 0.13817(6) 0.01374(16) Uani 1 1 d . . . Cl1 Cl 1.39104(10) 0.25950(5) 0.26413(7) 0.0274(2) Uani 1 1 d . . . Cl2 Cl 1.16995(10) 0.15399(4) 0.27611(6) 0.01982(16) Uani 1 1 d . . . C1 C 0.7807(4) 0.26160(15) -0.0070(2) 0.0186(7) Uani 1 1 d . . . H1A H 0.8497 0.2590 -0.0403 0.022 Uiso 1 1 calc R . . H1B H 0.6786 0.2430 -0.0499 0.022 Uiso 1 1 calc R . . C2 C 0.7518(4) 0.32854(15) 0.0039(2) 0.0155(6) Uani 1 1 d . . . C3 C 0.8683(4) 0.36962(15) 0.0620(2) 0.0152(6) Uani 1 1 d . . . C4 C 0.8229(4) 0.43105(15) 0.0602(3) 0.0195(7) Uani 1 1 d . . . H4 H 0.8998 0.4600 0.0981 0.023 Uiso 1 1 calc R . . C5 C 0.6707(4) 0.45108(16) 0.0055(3) 0.0204(7) Uani 1 1 d . . . H5 H 0.6448 0.4931 0.0059 0.024 Uiso 1 1 calc R . . C6 C 0.5564(4) 0.40963(16) -0.0498(2) 0.0190(7) Uani 1 1 d . . . H6 H 0.4511 0.4227 -0.0867 0.023 Uiso 1 1 calc R . . C7 C 0.5975(4) 0.34889(16) -0.0506(2) 0.0188(7) Uani 1 1 d . . . H7 H 0.5195 0.3204 -0.0888 0.023 Uiso 1 1 calc R . . C8 C 0.7235(4) 0.21283(16) 0.1543(3) 0.0185(7) Uani 1 1 d . . . C9 C 0.7241(5) 0.27700(18) 0.1955(3) 0.0275(8) Uani 1 1 d . . . H9A H 0.6523 0.2776 0.2262 0.041 Uiso 1 1 calc R . . H9B H 0.6896 0.3072 0.1436 0.041 Uiso 1 1 calc R . . H9C H 0.8308 0.2870 0.2428 0.041 Uiso 1 1 calc R . . C10 C 0.5563(4) 0.19755(19) 0.0796(3) 0.0282(8) Uani 1 1 d . . . H10A H 0.5551 0.1564 0.0540 0.042 Uiso 1 1 calc R . . H10B H 0.5234 0.2275 0.0275 0.042 Uiso 1 1 calc R . . H10C H 0.4838 0.1990 0.1098 0.042 Uiso 1 1 calc R . . C11 C 0.7728(5) 0.16832(19) 0.2386(3) 0.0273(8) Uani 1 1 d . . . H11A H 0.7024 0.1730 0.2699 0.041 Uiso 1 1 calc R . . H11B H 0.8812 0.1772 0.2847 0.041 Uiso 1 1 calc R . . H11C H 0.7664 0.1262 0.2152 0.041 Uiso 1 1 calc R . . C12 C 0.8745(4) 0.13844(16) 0.0400(2) 0.0216(7) Uani 1 1 d . . . C13 C 0.7361(5) 0.13231(17) -0.0608(3) 0.0300(9) Uani 1 1 d . . . H13A H 0.7478 0.1628 -0.1037 0.045 Uiso 1 1 calc R . . H13B H 0.6365 0.1391 -0.0565 0.045 Uiso 1 1 calc R . . H13C H 0.7366 0.0912 -0.0859 0.045 Uiso 1 1 calc R . . C14 C 0.8695(5) 0.08164(16) 0.0976(3) 0.0268(8) Uani 1 1 d . . . H14A H 0.8891 0.0448 0.0682 0.040 Uiso 1 1 calc R . . H14B H 0.7657 0.0787 0.0977 0.040 Uiso 1 1 calc R . . H14C H 0.9506 0.0853 0.1636 0.040 Uiso 1 1 calc R . . C15 C 1.0276(5) 0.13742(17) 0.0273(3) 0.0265(8) Uani 1 1 d . . . H15A H 1.1179 0.1359 0.0903 0.040 Uiso 1 1 calc R . . H15B H 1.0340 0.1745 -0.0065 0.040 Uiso 1 1 calc R . . H15C H 1.0286 0.1013 -0.0099 0.040 Uiso 1 1 calc R . . C16 C 1.1780(4) 0.36341(16) 0.0589(3) 0.0203(7) Uani 1 1 d . . . C17 C 1.1819(5) 0.30336(17) 0.0081(3) 0.0287(9) Uani 1 1 d . . . H17A H 1.0740 0.2894 -0.0309 0.043 Uiso 1 1 calc R . . H17B H 1.2388 0.2721 0.0560 0.043 Uiso 1 1 calc R . . H17C H 1.2353 0.3103 -0.0332 0.043 Uiso 1 1 calc R . . C18 C 1.3482(4) 0.3852(2) 0.1170(3) 0.0303(9) Uani 1 1 d . . . H18A H 1.4009 0.3887 0.0747 0.045 Uiso 1 1 calc R . . H18B H 1.4046 0.3556 0.1679 0.045 Uiso 1 1 calc R . . H18C H 1.3476 0.4252 0.1454 0.045 Uiso 1 1 calc R . . C19 C 1.0897(4) 0.41079(16) -0.0193(3) 0.0212(7) Uani 1 1 d . . . H19A H 1.0831 0.4496 0.0106 0.032 Uiso 1 1 calc R . . H19B H 0.9833 0.3958 -0.0595 0.032 Uiso 1 1 calc R . . H19C H 1.1463 0.4172 -0.0589 0.032 Uiso 1 1 calc R . . C20 C 1.1387(4) 0.40351(16) 0.2434(2) 0.0200(7) Uani 1 1 d . . . C21 C 1.2945(5) 0.3840(2) 0.3263(3) 0.0314(9) Uani 1 1 d . . . H21A H 1.3253 0.4144 0.3778 0.047 Uiso 1 1 calc R . . H21B H 1.3765 0.3812 0.3034 0.047 Uiso 1 1 calc R . . H21C H 1.2813 0.3440 0.3505 0.047 Uiso 1 1 calc R . . C22 C 1.1604(5) 0.47083(17) 0.2184(3) 0.0270(8) Uani 1 1 d . . . H22A H 1.2621 0.4864 0.2654 0.040 Uiso 1 1 calc R . . H22B H 1.0756 0.4962 0.2197 0.040 Uiso 1 1 calc R . . H22C H 1.1573 0.4723 0.1543 0.040 Uiso 1 1 calc R . . C23 C 1.0157(5) 0.40053(18) 0.2846(3) 0.0259(8) Uani 1 1 d . . . H23A H 1.0175 0.3597 0.3113 0.039 Uiso 1 1 calc R . . H23B H 0.9108 0.4086 0.2334 0.039 Uiso 1 1 calc R . . H23C H 1.0408 0.4313 0.3351 0.039 Uiso 1 1 calc R . . C24 C 0.4173(5) 0.05541(18) 0.2090(3) 0.0290(8) Uani 1 1 d . . . H24A H 0.5280 0.0573 0.2578 0.035 Uiso 1 1 calc R . . H24B H 0.3681 0.0957 0.2076 0.035 Uiso 1 1 calc R . . Cl3 Cl 0.41266(14) 0.04027(5) 0.09512(8) 0.0367(2) Uani 1 1 d . . . Cl4 Cl 0.31689(15) -0.00147(5) 0.24111(8) 0.0398(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.01244(6) 0.01550(6) 0.01060(6) 0.00284(5) 0.00506(4) 0.00305(5) P1 0.0161(4) 0.0135(4) 0.0128(4) 0.0007(3) 0.0045(3) 0.0018(3) P2 0.0121(4) 0.0151(4) 0.0135(4) 0.0015(3) 0.0050(3) 0.0008(3) Cl1 0.0127(4) 0.0388(5) 0.0281(4) 0.0144(4) 0.0061(3) 0.0041(3) Cl2 0.0219(4) 0.0189(4) 0.0164(4) 0.0052(3) 0.0061(3) 0.0045(3) C1 0.0199(17) 0.0160(16) 0.0165(16) -0.0018(12) 0.0045(13) 0.0026(12) C2 0.0192(16) 0.0144(15) 0.0121(14) 0.0023(12) 0.0060(13) 0.0036(12) C3 0.0145(15) 0.0171(16) 0.0146(15) 0.0047(12) 0.0067(13) 0.0030(12) C4 0.0192(17) 0.0152(16) 0.0237(17) -0.0003(13) 0.0090(14) -0.0020(13) C5 0.0210(17) 0.0147(16) 0.0255(18) 0.0013(13) 0.0100(15) 0.0030(13) C6 0.0179(16) 0.0195(16) 0.0180(16) 0.0037(13) 0.0063(13) 0.0042(13) C7 0.0182(17) 0.0199(16) 0.0155(15) -0.0019(13) 0.0046(13) 0.0006(13) C8 0.0169(16) 0.0170(16) 0.0224(17) -0.0002(13) 0.0091(14) -0.0009(13) C9 0.029(2) 0.0249(19) 0.038(2) -0.0084(16) 0.0242(18) -0.0047(15) C10 0.0156(18) 0.033(2) 0.031(2) 0.0006(17) 0.0051(15) -0.0029(15) C11 0.028(2) 0.032(2) 0.0271(19) 0.0063(16) 0.0165(17) 0.0030(16) C12 0.0285(19) 0.0147(16) 0.0163(16) -0.0029(13) 0.0047(14) 0.0044(14) C13 0.039(2) 0.0166(17) 0.0211(18) -0.0056(14) 0.0010(17) 0.0039(16) C14 0.036(2) 0.0145(16) 0.0263(19) 0.0009(14) 0.0105(17) 0.0035(15) C15 0.037(2) 0.0229(18) 0.0214(18) -0.0030(14) 0.0148(17) 0.0082(16) C16 0.0211(17) 0.0211(17) 0.0239(17) 0.0073(14) 0.0147(15) 0.0033(13) C17 0.043(2) 0.0231(19) 0.033(2) 0.0096(16) 0.0286(19) 0.0113(17) C18 0.0193(18) 0.043(2) 0.031(2) 0.0141(18) 0.0133(16) 0.0022(16) C19 0.0260(19) 0.0194(17) 0.0212(17) 0.0061(13) 0.0131(15) 0.0045(14) C20 0.0207(17) 0.0200(17) 0.0169(16) -0.0016(13) 0.0057(14) -0.0038(13) C21 0.026(2) 0.037(2) 0.0197(18) -0.0017(16) -0.0014(16) -0.0017(17) C22 0.029(2) 0.0209(18) 0.0269(19) -0.0048(15) 0.0087(16) -0.0070(15) C23 0.033(2) 0.0270(19) 0.0193(17) -0.0057(15) 0.0132(16) -0.0038(16) C24 0.028(2) 0.0242(19) 0.034(2) -0.0059(16) 0.0130(17) -0.0049(15) Cl3 0.0427(6) 0.0373(5) 0.0329(5) -0.0016(4) 0.0188(5) -0.0054(5) Cl4 0.0558(7) 0.0306(5) 0.0401(6) -0.0093(4) 0.0274(5) -0.0155(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 P1 2.2531(9) . ? Pt1 P2 2.2895(8) . ? Pt1 Cl2 2.3627(8) . ? Pt1 Cl1 2.3824(9) . ? P1 C1 1.823(3) . ? P1 C8 1.878(4) . ? P1 C12 1.913(3) . ? P2 C3 1.848(3) . ? P2 C16 1.906(3) . ? P2 C20 1.922(4) . ? C1 C2 1.510(4) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C7 1.402(5) . ? C2 C3 1.403(5) . ? C3 C4 1.405(5) . ? C4 C5 1.385(5) . ? C4 H4 0.9500 . ? C5 C6 1.385(5) . ? C5 H5 0.9500 . ? C6 C7 1.384(5) . ? C6 H6 0.9500 . ? C7 H7 0.9500 . ? C8 C11 1.531(5) . ? C8 C10 1.536(5) . ? C8 C9 1.539(5) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C15 1.537(5) . ? C12 C14 1.540(5) . ? C12 C13 1.548(5) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C19 1.536(5) . ? C16 C18 1.537(5) . ? C16 C17 1.538(5) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 C21 1.536(5) . ? C20 C23 1.545(5) . ? C20 C22 1.557(5) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 Cl4 1.757(4) . ? C24 Cl3 1.776(4) . ? C24 H24A 0.9900 . ? C24 H24B 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 P1 Pt1 P2 96.84(3) . . ? P1 Pt1 Cl2 89.52(3) . . ? P2 Pt1 Cl2 170.42(3) . . ? P1 Pt1 Cl1 161.44(3) . . ? P2 Pt1 Cl1 92.32(3) . . ? Cl2 Pt1 Cl1 83.65(3) . . ? C1 P1 C8 106.68(16) . . ? C1 P1 C12 98.33(15) . . ? C8 P1 C12 112.65(16) . . ? C1 P1 Pt1 109.24(12) . . ? C8 P1 Pt1 117.07(11) . . ? C12 P1 Pt1 111.05(12) . . ? C3 P2 C16 103.12(15) . . ? C3 P2 C20 103.43(16) . . ? C16 P2 C20 111.17(16) . . ? C3 P2 Pt1 116.32(11) . . ? C16 P2 Pt1 112.04(11) . . ? C20 P2 Pt1 110.29(11) . . ? C2 C1 P1 118.7(2) . . ? C2 C1 H1A 107.6 . . ? P1 C1 H1A 107.6 . . ? C2 C1 H1B 107.6 . . ? P1 C1 H1B 107.6 . . ? H1A C1 H1B 107.1 . . ? C7 C2 C3 120.3(3) . . ? C7 C2 C1 115.5(3) . . ? C3 C2 C1 124.3(3) . . ? C2 C3 C4 116.9(3) . . ? C2 C3 P2 123.5(2) . . ? C4 C3 P2 119.6(3) . . ? C5 C4 C3 122.7(3) . . ? C5 C4 H4 118.7 . . ? C3 C4 H4 118.7 . . ? C4 C5 C6 119.7(3) . . ? C4 C5 H5 120.1 . . ? C6 C5 H5 120.1 . . ? C7 C6 C5 119.1(3) . . ? C7 C6 H6 120.5 . . ? C5 C6 H6 120.5 . . ? C6 C7 C2 121.4(3) . . ? C6 C7 H7 119.3 . . ? C2 C7 H7 119.3 . . ? C11 C8 C10 109.9(3) . . ? C11 C8 C9 106.2(3) . . ? C10 C8 C9 109.2(3) . . ? C11 C8 P1 112.2(2) . . ? C10 C8 P1 111.8(3) . . ? C9 C8 P1 107.2(2) . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C8 C10 H10A 109.5 . . ? C8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C8 C11 H11A 109.5 . . ? C8 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C8 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C15 C12 C14 109.0(3) . . ? C15 C12 C13 107.4(3) . . ? C14 C12 C13 106.9(3) . . ? C15 C12 P1 107.7(2) . . ? C14 C12 P1 113.6(2) . . ? C13 C12 P1 112.0(2) . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C12 C15 H15A 109.5 . . ? C12 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C12 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C19 C16 C18 109.1(3) . . ? C19 C16 C17 107.2(3) . . ? C18 C16 C17 108.4(3) . . ? C19 C16 P2 112.3(2) . . ? C18 C16 P2 112.2(3) . . ? C17 C16 P2 107.5(2) . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C16 C19 H19A 109.5 . . ? C16 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C16 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C21 C20 C23 105.1(3) . . ? C21 C20 C22 106.8(3) . . ? C23 C20 C22 110.2(3) . . ? C21 C20 P2 111.7(3) . . ? C23 C20 P2 107.5(2) . . ? C22 C20 P2 115.1(2) . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C20 C22 H22A 109.5 . . ? C20 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C20 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C20 C23 H23A 109.5 . . ? C20 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C20 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? Cl4 C24 Cl3 111.3(2) . . ? Cl4 C24 H24A 109.4 . . ? Cl3 C24 H24A 109.4 . . ? Cl4 C24 H24B 109.4 . . ? Cl3 C24 H24B 109.4 . . ? H24A C24 H24B 108.0 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag P2 Pt1 P1 C1 24.86(12) . . . . ? Cl2 Pt1 P1 C1 -162.32(12) . . . . ? Cl1 Pt1 P1 C1 -94.18(15) . . . . ? P2 Pt1 P1 C8 -96.45(13) . . . . ? Cl2 Pt1 P1 C8 76.37(13) . . . . ? Cl1 Pt1 P1 C8 144.50(14) . . . . ? P2 Pt1 P1 C12 132.24(12) . . . . ? Cl2 Pt1 P1 C12 -54.94(12) . . . . ? Cl1 Pt1 P1 C12 13.20(17) . . . . ? P1 Pt1 P2 C3 11.06(12) . . . . ? Cl2 Pt1 P2 C3 -120.3(2) . . . . ? Cl1 Pt1 P2 C3 174.88(12) . . . . ? P1 Pt1 P2 C16 -107.20(13) . . . . ? Cl2 Pt1 P2 C16 121.5(2) . . . . ? Cl1 Pt1 P2 C16 56.63(13) . . . . ? P1 Pt1 P2 C20 128.38(12) . . . . ? Cl2 Pt1 P2 C20 -3.0(2) . . . . ? Cl1 Pt1 P2 C20 -67.79(12) . . . . ? C8 P1 C1 C2 63.7(3) . . . . ? C12 P1 C1 C2 -179.5(3) . . . . ? Pt1 P1 C1 C2 -63.7(3) . . . . ? P1 C1 C2 C7 -125.8(3) . . . . ? P1 C1 C2 C3 55.4(4) . . . . ? C7 C2 C3 C4 -1.7(5) . . . . ? C1 C2 C3 C4 177.0(3) . . . . ? C7 C2 C3 P2 178.7(3) . . . . ? C1 C2 C3 P2 -2.6(5) . . . . ? C16 P2 C3 C2 94.1(3) . . . . ? C20 P2 C3 C2 -150.0(3) . . . . ? Pt1 P2 C3 C2 -28.9(3) . . . . ? C16 P2 C3 C4 -85.4(3) . . . . ? C20 P2 C3 C4 30.5(3) . . . . ? Pt1 P2 C3 C4 151.6(2) . . . . ? C2 C3 C4 C5 1.0(5) . . . . ? P2 C3 C4 C5 -179.4(3) . . . . ? C3 C4 C5 C6 0.4(5) . . . . ? C4 C5 C6 C7 -1.2(5) . . . . ? C5 C6 C7 C2 0.5(5) . . . . ? C3 C2 C7 C6 1.0(5) . . . . ? C1 C2 C7 C6 -177.8(3) . . . . ? C1 P1 C8 C11 173.2(3) . . . . ? C12 P1 C8 C11 66.4(3) . . . . ? Pt1 P1 C8 C11 -64.2(3) . . . . ? C1 P1 C8 C10 49.2(3) . . . . ? C12 P1 C8 C10 -57.6(3) . . . . ? Pt1 P1 C8 C10 171.8(2) . . . . ? C1 P1 C8 C9 -70.5(3) . . . . ? C12 P1 C8 C9 -177.3(2) . . . . ? Pt1 P1 C8 C9 52.1(3) . . . . ? C1 P1 C12 C15 85.5(3) . . . . ? C8 P1 C12 C15 -162.4(2) . . . . ? Pt1 P1 C12 C15 -28.9(3) . . . . ? C1 P1 C12 C14 -153.6(3) . . . . ? C8 P1 C12 C14 -41.6(3) . . . . ? Pt1 P1 C12 C14 92.0(3) . . . . ? C1 P1 C12 C13 -32.3(3) . . . . ? C8 P1 C12 C13 79.7(3) . . . . ? Pt1 P1 C12 C13 -146.7(3) . . . . ? C3 P2 C16 C19 22.6(3) . . . . ? C20 P2 C16 C19 -87.6(3) . . . . ? Pt1 P2 C16 C19 148.4(2) . . . . ? C3 P2 C16 C18 145.9(3) . . . . ? C20 P2 C16 C18 35.6(3) . . . . ? Pt1 P2 C16 C18 -88.3(3) . . . . ? C3 P2 C16 C17 -95.1(3) . . . . ? C20 P2 C16 C17 154.7(3) . . . . ? Pt1 P2 C16 C17 30.7(3) . . . . ? C3 P2 C20 C21 167.6(3) . . . . ? C16 P2 C20 C21 -82.3(3) . . . . ? Pt1 P2 C20 C21 42.6(3) . . . . ? C3 P2 C20 C23 52.8(3) . . . . ? C16 P2 C20 C23 162.8(2) . . . . ? Pt1 P2 C20 C23 -72.3(3) . . . . ? C3 P2 C20 C22 -70.4(3) . . . . ? C16 P2 C20 C22 39.7(3) . . . . ? Pt1 P2 C20 C22 164.6(2) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.54 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.171 _refine_diff_density_min -1.811 _refine_diff_density_rms 0.119 data_2b _database_code_depnum_ccdc_archive 'CCDC 897392' #TrackingRef '- all.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C25 H40 Cl2 O3 P2 Pt, C H2 Cl2' _chemical_formula_sum 'C26 H42 Cl4 O3 P2 Pt' _chemical_formula_weight 801.43 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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 12.461(3) _cell_length_b 15.187(3) _cell_length_c 17.334(4) _cell_angle_alpha 85.45(3) _cell_angle_beta 79.62(3) _cell_angle_gamma 77.63(3) _cell_volume 3148.8(12) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 8278 _cell_measurement_theta_min 2.2 _cell_measurement_theta_max 27.1 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.691 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1592 _exptl_absorpt_coefficient_mu 4.923 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.476 _exptl_absorpt_correction_T_max 0.778 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1998)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'CCD area detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 36228 _diffrn_reflns_av_R_equivalents 0.0564 _diffrn_reflns_av_sigmaI/netI 0.0812 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.20 _diffrn_reflns_theta_max 27.48 _reflns_number_total 14356 _reflns_number_gt 11142 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0339P)^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 14356 _refine_ls_number_parameters 669 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0558 _refine_ls_R_factor_gt 0.0426 _refine_ls_wR_factor_ref 0.0881 _refine_ls_wR_factor_gt 0.0846 _refine_ls_goodness_of_fit_ref 0.913 _refine_ls_restrained_S_all 0.913 _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 0.288857(17) 0.787232(13) 0.257803(12) 0.01527(6) Uani 1 1 d . . . P1 P 0.36558(12) 0.65873(9) 0.31913(8) 0.0169(3) Uani 1 1 d . . . P2 P 0.11127(11) 0.77125(9) 0.30306(8) 0.0167(3) Uani 1 1 d . . . Cl1 Cl 0.24215(11) 0.91070(9) 0.17025(9) 0.0253(3) Uani 1 1 d . . . Cl2 Cl 0.46876(11) 0.81782(9) 0.22066(8) 0.0226(3) Uani 1 1 d . . . O1 O 0.0224(3) 0.8047(2) 0.1713(2) 0.0200(9) Uani 1 1 d . . . O2 O -0.1062(3) 0.8549(3) 0.3532(2) 0.0210(9) Uani 1 1 d . . . O3 O -0.1595(3) 0.8702(3) 0.2285(2) 0.0250(9) Uani 1 1 d . . . C1 C 0.2679(4) 0.5815(4) 0.3381(3) 0.0198(12) Uani 1 1 d . . . H1A H 0.2450 0.5726 0.2879 0.024 Uiso 1 1 calc R . . H1B H 0.3074 0.5222 0.3569 0.024 Uiso 1 1 calc R . . C2 C 0.1650(4) 0.6127(4) 0.3970(3) 0.0177(12) Uani 1 1 d . . . C3 C 0.0909(4) 0.6956(3) 0.3910(3) 0.0174(12) Uani 1 1 d . . . C4 C 0.0027(4) 0.7181(4) 0.4527(3) 0.0206(12) Uani 1 1 d . . . H4 H -0.0483 0.7741 0.4498 0.025 Uiso 1 1 calc R . . C5 C -0.0120(5) 0.6612(4) 0.5177(3) 0.0251(13) Uani 1 1 d . . . H5 H -0.0718 0.6787 0.5596 0.030 Uiso 1 1 calc R . . C6 C 0.0596(5) 0.5786(4) 0.5224(4) 0.0267(14) Uani 1 1 d . . . H6 H 0.0483 0.5384 0.5666 0.032 Uiso 1 1 calc R . . C7 C 0.1471(5) 0.5552(4) 0.4626(3) 0.0217(13) Uani 1 1 d . . . H7 H 0.1967 0.4986 0.4659 0.026 Uiso 1 1 calc R . . C8 C 0.4033(4) 0.6793(4) 0.4153(3) 0.0191(12) Uani 1 1 d . . . C9 C 0.3022(5) 0.7383(4) 0.4639(3) 0.0254(13) Uani 1 1 d . . . H9A H 0.2452 0.7026 0.4829 0.038 Uiso 1 1 calc R . . H9B H 0.2716 0.7898 0.4311 0.038 Uiso 1 1 calc R . . H9C H 0.3254 0.7602 0.5087 0.038 Uiso 1 1 calc R . . C10 C 0.4374(5) 0.5898(4) 0.4602(4) 0.0298(14) Uani 1 1 d . . . H10A H 0.5076 0.5558 0.4322 0.045 Uiso 1 1 calc R . . H10B H 0.3792 0.5545 0.4642 0.045 Uiso 1 1 calc R . . H10C H 0.4472 0.6017 0.5130 0.045 Uiso 1 1 calc R . . C11 C 0.4989(5) 0.7302(4) 0.4052(4) 0.0262(14) Uani 1 1 d . . . H11A H 0.5095 0.7454 0.4568 0.039 Uiso 1 1 calc R . . H11B H 0.4807 0.7858 0.3732 0.039 Uiso 1 1 calc R . . H11C H 0.5675 0.6921 0.3792 0.039 Uiso 1 1 calc R . . C12 C 0.4830(5) 0.5847(4) 0.2523(4) 0.0245(13) Uani 1 1 d . . . C13 C 0.4880(5) 0.4831(4) 0.2733(4) 0.0262(14) Uani 1 1 d . . . H13A H 0.4195 0.4667 0.2642 0.039 Uiso 1 1 calc R . . H13B H 0.4954 0.4707 0.3286 0.039 Uiso 1 1 calc R . . H13C H 0.5523 0.4475 0.2403 0.039 Uiso 1 1 calc R . . C14 C 0.6004(5) 0.6020(4) 0.2545(4) 0.0292(15) Uani 1 1 d . . . H14A H 0.6538 0.5716 0.2114 0.044 Uiso 1 1 calc R . . H14B H 0.6231 0.5785 0.3047 0.044 Uiso 1 1 calc R . . H14C H 0.5985 0.6670 0.2489 0.044 Uiso 1 1 calc R . . C15 C 0.4576(5) 0.6027(4) 0.1686(3) 0.0273(14) Uani 1 1 d . . . H15A H 0.5077 0.5577 0.1342 0.041 Uiso 1 1 calc R . . H15B H 0.4686 0.6632 0.1496 0.041 Uiso 1 1 calc R . . H15C H 0.3801 0.5988 0.1684 0.041 Uiso 1 1 calc R . . C16 C 0.0336(5) 0.7337(4) 0.2316(3) 0.0209(12) Uani 1 1 d . . . C17 C -0.0794(4) 0.7232(4) 0.2740(3) 0.0219(12) Uani 1 1 d . . . H17A H -0.0711 0.6831 0.3214 0.026 Uiso 1 1 calc R . . H17B H -0.1163 0.6948 0.2395 0.026 Uiso 1 1 calc R . . C18 C -0.1509(5) 0.8134(4) 0.2978(4) 0.0233(13) Uani 1 1 d . . . C19 C 0.0025(4) 0.8784(4) 0.3250(3) 0.0193(12) Uani 1 1 d . . . C20 C -0.0114(5) 0.9371(4) 0.2515(3) 0.0222(13) Uani 1 1 d . . . H20A H 0.0609 0.9522 0.2271 0.027 Uiso 1 1 calc R . . H20B H -0.0651 0.9941 0.2651 0.027 Uiso 1 1 calc R . . C21 C -0.0535(5) 0.8878(4) 0.1936(3) 0.0221(13) Uani 1 1 d . . . C22 C 0.0954(4) 0.6487(4) 0.1900(3) 0.0251(14) Uani 1 1 d . . . H22A H 0.0540 0.6369 0.1503 0.038 Uiso 1 1 calc R . . H22B H 0.1024 0.5976 0.2283 0.038 Uiso 1 1 calc R . . H22C H 0.1698 0.6567 0.1646 0.038 Uiso 1 1 calc R . . C23 C -0.2681(5) 0.8076(4) 0.3353(4) 0.0276(14) Uani 1 1 d . . . H23A H -0.3104 0.8679 0.3495 0.041 Uiso 1 1 calc R . . H23B H -0.2662 0.7678 0.3827 0.041 Uiso 1 1 calc R . . H23C H -0.3038 0.7832 0.2982 0.041 Uiso 1 1 calc R . . C24 C 0.0287(5) 0.9304(4) 0.3891(4) 0.0271(14) Uani 1 1 d . . . H24A H -0.0315 0.9830 0.4015 0.041 Uiso 1 1 calc R . . H24B H 0.0990 0.9504 0.3704 0.041 Uiso 1 1 calc R . . H24C H 0.0354 0.8910 0.4363 0.041 Uiso 1 1 calc R . . C25 C -0.0679(5) 0.9423(4) 0.1188(4) 0.0326(15) Uani 1 1 d . . . H25A H -0.0964 0.9083 0.0841 0.049 Uiso 1 1 calc R . . H25B H 0.0042 0.9549 0.0928 0.049 Uiso 1 1 calc R . . H25C H -0.1208 0.9993 0.1306 0.049 Uiso 1 1 calc R . . Pt2 Pt 0.289311(17) 0.284634(13) 0.278592(12) 0.01579(6) Uani 1 1 d . . . P3 P 0.40244(12) 0.15027(10) 0.29877(8) 0.0180(3) Uani 1 1 d . . . P4 P 0.28613(12) 0.26028(9) 0.15169(8) 0.0188(3) Uani 1 1 d . . . Cl3 Cl 0.14244(11) 0.41318(9) 0.28978(8) 0.0221(3) Uani 1 1 d . . . Cl4 Cl 0.31096(12) 0.32599(9) 0.40190(8) 0.0252(3) Uani 1 1 d . . . O4 O 0.0684(3) 0.3019(2) 0.1427(2) 0.0212(9) Uani 1 1 d . . . O5 O 0.2782(3) 0.3357(3) 0.0037(2) 0.0244(9) Uani 1 1 d . . . O6 O 0.0836(3) 0.3583(3) 0.0119(2) 0.0278(10) Uani 1 1 d . . . C26 C 0.3968(5) 0.0712(3) 0.2258(3) 0.0182(12) Uani 1 1 d . . . H26A H 0.4383 0.0107 0.2402 0.022 Uiso 1 1 calc R . . H26B H 0.3182 0.0669 0.2280 0.022 Uiso 1 1 calc R . . C27 C 0.4434(5) 0.0961(4) 0.1435(3) 0.0213(12) Uani 1 1 d . . . C28 C 0.4060(5) 0.1783(4) 0.1043(3) 0.0216(13) Uani 1 1 d . . . C29 C 0.4632(5) 0.1966(4) 0.0292(3) 0.0276(14) Uani 1 1 d . . . H29 H 0.4402 0.2525 0.0024 0.033 Uiso 1 1 calc R . . C30 C 0.5522(5) 0.1345(4) -0.0059(4) 0.0334(16) Uani 1 1 d . . . H30 H 0.5896 0.1481 -0.0568 0.040 Uiso 1 1 calc R . . C31 C 0.5879(5) 0.0531(5) 0.0313(4) 0.0353(16) Uani 1 1 d . . . H31 H 0.6495 0.0106 0.0066 0.042 Uiso 1 1 calc R . . C32 C 0.5331(5) 0.0342(4) 0.1051(4) 0.0289(14) Uani 1 1 d . . . H32 H 0.5570 -0.0224 0.1306 0.035 Uiso 1 1 calc R . . C33 C 0.5532(5) 0.1554(4) 0.2942(4) 0.0258(14) Uani 1 1 d . . . C34 C 0.5915(5) 0.2068(5) 0.2183(4) 0.0401(17) Uani 1 1 d . . . H34A H 0.5383 0.2639 0.2136 0.060 Uiso 1 1 calc R . . H34B H 0.5954 0.1703 0.1733 0.060 Uiso 1 1 calc R . . H34C H 0.6653 0.2190 0.2192 0.060 Uiso 1 1 calc R . . C35 C 0.6249(5) 0.0597(4) 0.2961(4) 0.0415(18) Uani 1 1 d . . . H35A H 0.6115 0.0253 0.2545 0.062 Uiso 1 1 calc R . . H35B H 0.6052 0.0295 0.3472 0.062 Uiso 1 1 calc R . . H35C H 0.7039 0.0631 0.2878 0.062 Uiso 1 1 calc R . . C36 C 0.5710(5) 0.2080(5) 0.3610(4) 0.0417(18) Uani 1 1 d . . . H36A H 0.6491 0.2141 0.3531 0.063 Uiso 1 1 calc R . . H36B H 0.5529 0.1757 0.4112 0.063 Uiso 1 1 calc R . . H36C H 0.5226 0.2681 0.3613 0.063 Uiso 1 1 calc R . . C37 C 0.3424(5) 0.0875(4) 0.3905(3) 0.0225(13) Uani 1 1 d . . . C38 C 0.3759(5) -0.0151(4) 0.3839(4) 0.0312(15) Uani 1 1 d . . . H38A H 0.3498 -0.0445 0.4341 0.047 Uiso 1 1 calc R . . H38B H 0.4572 -0.0329 0.3710 0.047 Uiso 1 1 calc R . . H38C H 0.3420 -0.0334 0.3425 0.047 Uiso 1 1 calc R . . C39 C 0.3790(6) 0.1069(4) 0.4658(4) 0.0392(17) Uani 1 1 d . . . H39A H 0.3622 0.1721 0.4726 0.059 Uiso 1 1 calc R . . H39B H 0.4593 0.0838 0.4625 0.059 Uiso 1 1 calc R . . H39C H 0.3389 0.0771 0.5107 0.059 Uiso 1 1 calc R . . C40 C 0.2164(5) 0.1141(4) 0.3998(4) 0.0357(16) Uani 1 1 d . . . H40A H 0.1829 0.0805 0.4451 0.054 Uiso 1 1 calc R . . H40B H 0.1922 0.1000 0.3523 0.054 Uiso 1 1 calc R . . H40C H 0.1927 0.1790 0.4080 0.054 Uiso 1 1 calc R . . C41 C 0.2735(5) 0.3641(4) 0.0816(3) 0.0245(13) Uani 1 1 d . . . C42 C 0.1621(5) 0.4264(4) 0.1017(3) 0.0273(14) Uani 1 1 d . . . H42A H 0.1599 0.4815 0.0670 0.033 Uiso 1 1 calc R . . H42B H 0.1518 0.4445 0.1566 0.033 Uiso 1 1 calc R . . C43 C 0.0686(5) 0.3813(4) 0.0921(3) 0.0281(14) Uani 1 1 d . . . C44 C 0.1605(5) 0.2263(4) 0.1256(3) 0.0213(12) Uani 1 1 d . . . C45 C 0.1809(5) 0.2096(4) 0.0387(3) 0.0232(13) Uani 1 1 d . . . H45A H 0.1196 0.1841 0.0261 0.028 Uiso 1 1 calc R . . H45B H 0.2515 0.1653 0.0250 0.028 Uiso 1 1 calc R . . C46 C 0.1874(5) 0.2976(4) -0.0093(3) 0.0258(14) Uani 1 1 d . . . C47 C 0.1258(5) 0.1473(4) 0.1743(3) 0.0231(13) Uani 1 1 d . . . H47A H 0.1194 0.1581 0.2301 0.035 Uiso 1 1 calc R . . H47B H 0.1818 0.0924 0.1608 0.035 Uiso 1 1 calc R . . H47C H 0.0537 0.1402 0.1636 0.035 Uiso 1 1 calc R . . C48 C 0.2043(5) 0.2858(4) -0.0962(3) 0.0315(15) Uani 1 1 d . . . H48A H 0.1466 0.2567 -0.1082 0.047 Uiso 1 1 calc R . . H48B H 0.2779 0.2482 -0.1132 0.047 Uiso 1 1 calc R . . H48C H 0.1993 0.3450 -0.1239 0.047 Uiso 1 1 calc R . . C49 C 0.3692(5) 0.4124(4) 0.0802(4) 0.0326(15) Uani 1 1 d . . . H49A H 0.4402 0.3714 0.0626 0.049 Uiso 1 1 calc R . . H49B H 0.3682 0.4316 0.1330 0.049 Uiso 1 1 calc R . . H49C H 0.3608 0.4654 0.0440 0.049 Uiso 1 1 calc R . . C50 C -0.0448(5) 0.4401(4) 0.1110(4) 0.0362(17) Uani 1 1 d . . . H50A H -0.0491 0.4947 0.0767 0.054 Uiso 1 1 calc R . . H50B H -0.0583 0.4568 0.1659 0.054 Uiso 1 1 calc R . . H50C H -0.1011 0.4072 0.1028 0.054 Uiso 1 1 calc R . . C51 C 0.7938(8) 0.2293(6) -0.0032(5) 0.077(3) Uani 1 1 d . . . H51A H 0.7503 0.1826 -0.0065 0.092 Uiso 1 1 calc R . . H51B H 0.8461 0.2310 -0.0533 0.092 Uiso 1 1 calc R . . Cl5 Cl 0.8678(2) 0.1988(2) 0.06987(15) 0.0890(9) Uani 1 1 d . . . Cl6 Cl 0.70254(17) 0.33364(14) 0.00733(13) 0.0638(6) Uani 1 1 d . . . C52 C 0.9053(5) 0.2987(4) 0.3063(4) 0.0393(17) Uani 1 1 d . . . H52A H 0.9609 0.3236 0.3273 0.047 Uiso 1 1 calc R . . H52B H 0.9310 0.2923 0.2492 0.047 Uiso 1 1 calc R . . Cl7 Cl 0.89887(15) 0.19133(12) 0.35138(12) 0.0487(5) Uani 1 1 d . . . Cl8 Cl 0.77736(16) 0.37462(13) 0.32150(13) 0.0547(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.01857(11) 0.01040(11) 0.01741(12) 0.00058(8) -0.00339(8) -0.00430(8) P1 0.0175(7) 0.0135(7) 0.0208(8) 0.0011(6) -0.0048(6) -0.0050(6) P2 0.0186(7) 0.0119(7) 0.0202(8) -0.0017(6) -0.0041(6) -0.0038(6) Cl1 0.0240(7) 0.0176(7) 0.0306(8) 0.0085(6) -0.0013(6) -0.0023(6) Cl2 0.0223(7) 0.0177(7) 0.0284(8) 0.0030(6) -0.0018(6) -0.0091(6) O1 0.023(2) 0.015(2) 0.023(2) -0.0005(16) -0.0087(16) -0.0024(16) O2 0.019(2) 0.023(2) 0.024(2) -0.0050(17) -0.0055(16) -0.0068(17) O3 0.021(2) 0.022(2) 0.033(2) 0.0039(18) -0.0086(17) -0.0057(17) C1 0.024(3) 0.014(3) 0.023(3) -0.002(2) -0.002(2) -0.007(2) C2 0.021(3) 0.015(3) 0.020(3) 0.000(2) -0.003(2) -0.010(2) C3 0.020(3) 0.013(3) 0.023(3) 0.000(2) -0.007(2) -0.009(2) C4 0.018(3) 0.020(3) 0.025(3) -0.004(2) -0.005(2) -0.005(2) C5 0.028(3) 0.028(3) 0.020(3) -0.003(3) 0.000(2) -0.008(3) C6 0.032(3) 0.026(3) 0.025(3) 0.006(3) -0.003(3) -0.015(3) C7 0.026(3) 0.013(3) 0.030(3) 0.000(2) -0.007(2) -0.008(2) C8 0.018(3) 0.018(3) 0.024(3) 0.006(2) -0.007(2) -0.008(2) C9 0.026(3) 0.027(3) 0.026(3) -0.002(3) -0.006(3) -0.011(3) C10 0.036(4) 0.028(3) 0.028(3) 0.011(3) -0.013(3) -0.010(3) C11 0.026(3) 0.024(3) 0.032(4) -0.001(3) -0.007(3) -0.010(3) C12 0.025(3) 0.013(3) 0.033(4) -0.002(2) 0.000(3) -0.002(2) C13 0.025(3) 0.014(3) 0.037(4) -0.002(3) -0.001(3) -0.001(2) C14 0.023(3) 0.021(3) 0.041(4) -0.002(3) 0.000(3) -0.002(3) C15 0.029(3) 0.022(3) 0.027(3) -0.007(3) 0.006(3) -0.003(3) C16 0.026(3) 0.010(3) 0.025(3) 0.002(2) -0.008(2) 0.001(2) C17 0.026(3) 0.020(3) 0.023(3) 0.002(2) -0.007(2) -0.010(2) C18 0.020(3) 0.022(3) 0.030(3) 0.000(3) -0.007(2) -0.009(2) C19 0.018(3) 0.013(3) 0.028(3) -0.007(2) -0.004(2) -0.002(2) C20 0.019(3) 0.013(3) 0.033(3) -0.002(2) -0.002(2) -0.001(2) C21 0.020(3) 0.015(3) 0.029(3) -0.002(2) -0.002(2) -0.001(2) C22 0.014(3) 0.023(3) 0.034(4) -0.005(3) -0.007(2) 0.010(2) C23 0.023(3) 0.029(3) 0.035(4) 0.002(3) -0.007(3) -0.012(3) C24 0.027(3) 0.020(3) 0.035(4) -0.007(3) -0.007(3) -0.003(3) C25 0.033(4) 0.025(3) 0.038(4) 0.004(3) -0.009(3) -0.001(3) Pt2 0.02217(12) 0.01036(11) 0.01584(12) 0.00000(8) -0.00342(8) -0.00549(9) P3 0.0225(8) 0.0146(7) 0.0178(8) -0.0004(6) -0.0045(6) -0.0046(6) P4 0.0286(8) 0.0115(7) 0.0179(8) 0.0011(6) -0.0055(6) -0.0069(6) Cl3 0.0282(7) 0.0143(6) 0.0225(7) 0.0003(5) -0.0039(6) -0.0027(6) Cl4 0.0358(8) 0.0174(7) 0.0232(8) -0.0034(6) -0.0102(6) -0.0015(6) O4 0.030(2) 0.0105(19) 0.021(2) 0.0021(16) -0.0042(17) 0.0006(17) O5 0.038(2) 0.018(2) 0.020(2) 0.0018(17) -0.0057(18) -0.0123(18) O6 0.040(3) 0.020(2) 0.021(2) 0.0017(17) -0.0102(18) 0.0026(19) C26 0.025(3) 0.009(3) 0.023(3) -0.002(2) -0.005(2) -0.007(2) C27 0.025(3) 0.021(3) 0.020(3) -0.006(2) -0.005(2) -0.008(2) C28 0.026(3) 0.017(3) 0.024(3) -0.006(2) -0.003(2) -0.009(2) C29 0.035(4) 0.027(3) 0.021(3) 0.001(3) -0.003(3) -0.008(3) C30 0.041(4) 0.039(4) 0.020(3) 0.000(3) 0.004(3) -0.015(3) C31 0.038(4) 0.036(4) 0.028(4) -0.008(3) 0.005(3) -0.006(3) C32 0.039(4) 0.018(3) 0.030(4) -0.002(3) -0.007(3) -0.005(3) C33 0.016(3) 0.027(3) 0.034(4) -0.004(3) -0.002(2) -0.003(2) C34 0.030(4) 0.043(4) 0.052(5) 0.005(4) -0.005(3) -0.022(3) C35 0.027(4) 0.035(4) 0.057(5) 0.000(3) -0.008(3) 0.004(3) C36 0.028(4) 0.055(5) 0.048(5) -0.021(4) -0.011(3) -0.011(3) C37 0.036(3) 0.011(3) 0.023(3) 0.004(2) -0.004(3) -0.011(2) C38 0.045(4) 0.018(3) 0.028(4) 0.005(3) -0.005(3) -0.004(3) C39 0.071(5) 0.028(4) 0.023(4) 0.004(3) -0.013(3) -0.018(4) C40 0.042(4) 0.027(4) 0.036(4) 0.007(3) 0.000(3) -0.011(3) C41 0.041(4) 0.014(3) 0.021(3) 0.003(2) -0.008(3) -0.012(3) C42 0.050(4) 0.013(3) 0.019(3) 0.004(2) -0.008(3) -0.006(3) C43 0.043(4) 0.015(3) 0.024(3) 0.004(2) -0.008(3) 0.000(3) C44 0.024(3) 0.015(3) 0.024(3) 0.002(2) -0.006(2) -0.002(2) C45 0.033(3) 0.014(3) 0.025(3) 0.002(2) -0.008(3) -0.007(2) C46 0.038(4) 0.017(3) 0.024(3) 0.002(2) -0.012(3) -0.007(3) C47 0.033(3) 0.022(3) 0.015(3) 0.002(2) -0.011(2) -0.003(3) C48 0.045(4) 0.031(4) 0.021(3) 0.002(3) -0.009(3) -0.012(3) C49 0.051(4) 0.022(3) 0.030(4) 0.005(3) -0.009(3) -0.020(3) C50 0.042(4) 0.024(3) 0.033(4) 0.008(3) -0.004(3) 0.007(3) C51 0.078(7) 0.076(7) 0.066(6) -0.011(5) -0.036(5) 0.029(5) Cl5 0.0688(16) 0.115(2) 0.0656(16) 0.0062(15) -0.0260(13) 0.0272(15) Cl6 0.0532(12) 0.0506(13) 0.0715(15) 0.0150(11) -0.0001(11) 0.0094(10) C52 0.027(4) 0.036(4) 0.051(5) 0.006(3) 0.004(3) -0.008(3) Cl7 0.0402(10) 0.0345(10) 0.0649(13) 0.0063(9) 0.0046(9) -0.0074(8) Cl8 0.0410(11) 0.0409(11) 0.0755(15) 0.0070(10) -0.0047(10) -0.0014(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 P1 2.2562(16) . ? Pt1 P2 2.2683(15) . ? Pt1 Cl2 2.3525(15) . ? Pt1 Cl1 2.3574(16) . ? P1 C1 1.836(6) . ? P1 C8 1.877(6) . ? P1 C12 1.907(6) . ? P2 C3 1.849(6) . ? P2 C16 1.892(6) . ? P2 C19 1.896(5) . ? O1 C21 1.439(6) . ? O1 C16 1.442(6) . ? O2 C18 1.437(7) . ? O2 C19 1.464(6) . ? O3 C21 1.421(7) . ? O3 C18 1.428(7) . ? C1 C2 1.502(7) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C7 1.392(8) . ? C2 C3 1.401(7) . ? C3 C4 1.393(7) . ? C4 C5 1.376(8) . ? C4 H4 0.9500 . ? C5 C6 1.381(8) . ? C5 H5 0.9500 . ? C6 C7 1.370(8) . ? C6 H6 0.9500 . ? C7 H7 0.9500 . ? C8 C10 1.530(7) . ? C8 C11 1.532(8) . ? C8 C9 1.534(7) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C15 1.531(8) . ? C12 C13 1.547(8) . ? C12 C14 1.548(8) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.501(8) . ? C16 C22 1.517(7) . ? C17 C18 1.508(8) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C23 1.506(8) . ? C19 C20 1.512(8) . ? C19 C24 1.531(8) . ? C20 C21 1.523(8) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 C25 1.499(8) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? Pt2 P3 2.2596(16) . ? Pt2 P4 2.2681(15) . ? Pt2 Cl4 2.3514(15) . ? Pt2 Cl3 2.3664(15) . ? P3 C26 1.832(5) . ? P3 C33 1.884(6) . ? P3 C37 1.905(6) . ? P4 C28 1.838(5) . ? P4 C44 1.886(6) . ? P4 C41 1.908(6) . ? O4 C43 1.433(7) . ? O4 C44 1.446(6) . ? O5 C46 1.436(7) . ? O5 C41 1.437(7) . ? O6 C46 1.424(7) . ? O6 C43 1.430(7) . ? C26 C27 1.492(8) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 C32 1.399(7) . ? C27 C28 1.403(8) . ? C28 C29 1.404(8) . ? C29 C30 1.374(8) . ? C29 H29 0.9500 . ? C30 C31 1.372(9) . ? C30 H30 0.9500 . ? C31 C32 1.377(8) . ? C31 H31 0.9500 . ? C32 H32 0.9500 . ? C33 C34 1.530(9) . ? C33 C36 1.530(8) . ? C33 C35 1.537(8) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 C40 1.517(8) . ? C37 C39 1.527(8) . ? C37 C38 1.531(7) . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 C42 1.503(8) . ? C41 C49 1.525(8) . ? C42 C43 1.511(9) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 C50 1.496(8) . ? C44 C47 1.505(8) . ? C44 C45 1.515(8) . ? C45 C46 1.527(8) . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C46 C48 1.502(8) . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C49 H49C 0.9800 . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? C51 Cl5 1.677(8) . ? C51 Cl6 1.743(8) . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? C52 Cl8 1.746(6) . ? C52 Cl7 1.763(7) . ? C52 H52A 0.9900 . ? C52 H52B 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 P1 Pt1 P2 94.07(6) . . ? P1 Pt1 Cl2 88.19(6) . . ? P2 Pt1 Cl2 173.35(5) . . ? P1 Pt1 Cl1 166.96(5) . . ? P2 Pt1 Cl1 95.87(6) . . ? Cl2 Pt1 Cl1 82.87(6) . . ? C1 P1 C8 108.2(3) . . ? C1 P1 C12 98.2(2) . . ? C8 P1 C12 113.8(3) . . ? C1 P1 Pt1 110.00(19) . . ? C8 P1 Pt1 112.55(18) . . ? C12 P1 Pt1 113.05(19) . . ? C3 P2 C16 104.6(2) . . ? C3 P2 C19 105.3(2) . . ? C16 P2 C19 93.2(2) . . ? C3 P2 Pt1 116.19(18) . . ? C16 P2 Pt1 117.39(19) . . ? C19 P2 Pt1 117.01(19) . . ? C21 O1 C16 116.6(4) . . ? C18 O2 C19 116.0(4) . . ? C21 O3 C18 110.6(4) . . ? C2 C1 P1 114.8(4) . . ? C2 C1 H1A 108.6 . . ? P1 C1 H1A 108.6 . . ? C2 C1 H1B 108.6 . . ? P1 C1 H1B 108.6 . . ? H1A C1 H1B 107.5 . . ? C7 C2 C3 119.6(5) . . ? C7 C2 C1 116.0(5) . . ? C3 C2 C1 124.3(5) . . ? C4 C3 C2 118.0(5) . . ? C4 C3 P2 121.9(4) . . ? C2 C3 P2 120.1(4) . . ? C5 C4 C3 121.4(5) . . ? C5 C4 H4 119.3 . . ? C3 C4 H4 119.3 . . ? C4 C5 C6 120.3(5) . . ? C4 C5 H5 119.9 . . ? C6 C5 H5 119.9 . . ? C7 C6 C5 119.2(6) . . ? C7 C6 H6 120.4 . . ? C5 C6 H6 120.4 . . ? C6 C7 C2 121.4(5) . . ? C6 C7 H7 119.3 . . ? C2 C7 H7 119.3 . . ? C10 C8 C11 108.3(5) . . ? C10 C8 C9 109.9(5) . . ? C11 C8 C9 106.6(5) . . ? C10 C8 P1 110.3(4) . . ? C11 C8 P1 112.7(4) . . ? C9 C8 P1 108.9(4) . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C8 C10 H10A 109.5 . . ? C8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C8 C11 H11A 109.5 . . ? C8 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C8 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C15 C12 C13 107.5(5) . . ? C15 C12 C14 109.5(5) . . ? C13 C12 C14 106.5(5) . . ? C15 C12 P1 107.1(4) . . ? C13 C12 P1 111.9(4) . . ? C14 C12 P1 114.1(4) . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C12 C15 H15A 109.5 . . ? C12 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C12 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? O1 C16 C17 110.0(4) . . ? O1 C16 C22 106.3(4) . . ? C17 C16 C22 111.3(5) . . ? O1 C16 P2 106.2(4) . . ? C17 C16 P2 108.8(4) . . ? C22 C16 P2 114.0(4) . . ? C16 C17 C18 110.9(5) . . ? C16 C17 H17A 109.5 . . ? C18 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? C18 C17 H17B 109.5 . . ? H17A C17 H17B 108.0 . . ? O3 C18 O2 110.4(5) . . ? O3 C18 C23 106.5(5) . . ? O2 C18 C23 106.5(5) . . ? O3 C18 C17 108.0(5) . . ? O2 C18 C17 112.2(4) . . ? C23 C18 C17 113.1(5) . . ? O2 C19 C20 105.3(4) . . ? O2 C19 C24 107.7(4) . . ? C20 C19 C24 111.4(5) . . ? O2 C19 P2 109.2(3) . . ? C20 C19 P2 111.4(4) . . ? C24 C19 P2 111.6(4) . . ? C19 C20 C21 109.9(5) . . ? C19 C20 H20A 109.7 . . ? C21 C20 H20A 109.7 . . ? C19 C20 H20B 109.7 . . ? C21 C20 H20B 109.7 . . ? H20A C20 H20B 108.2 . . ? O3 C21 O1 110.0(4) . . ? O3 C21 C25 107.4(5) . . ? O1 C21 C25 106.2(4) . . ? O3 C21 C20 108.7(4) . . ? O1 C21 C20 111.8(4) . . ? C25 C21 C20 112.6(5) . . ? C16 C22 H22A 109.5 . . ? C16 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C16 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C18 C23 H23A 109.5 . . ? C18 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C18 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C19 C24 H24A 109.5 . . ? C19 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C19 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C21 C25 H25A 109.5 . . ? C21 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C21 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? P3 Pt2 P4 94.26(6) . . ? P3 Pt2 Cl4 88.39(6) . . ? P4 Pt2 Cl4 170.90(5) . . ? P3 Pt2 Cl3 164.38(5) . . ? P4 Pt2 Cl3 96.10(6) . . ? Cl4 Pt2 Cl3 83.20(6) . . ? C26 P3 C33 107.5(3) . . ? C26 P3 C37 98.4(2) . . ? C33 P3 C37 113.6(3) . . ? C26 P3 Pt2 110.10(18) . . ? C33 P3 Pt2 114.7(2) . . ? C37 P3 Pt2 111.23(18) . . ? C28 P4 C44 104.8(2) . . ? C28 P4 C41 105.5(3) . . ? C44 P4 C41 92.9(3) . . ? C28 P4 Pt2 114.92(19) . . ? C44 P4 Pt2 119.42(19) . . ? C41 P4 Pt2 116.40(19) . . ? C43 O4 C44 117.5(4) . . ? C46 O5 C41 116.8(4) . . ? C46 O6 C43 110.7(4) . . ? C27 C26 P3 114.6(4) . . ? C27 C26 H26A 108.6 . . ? P3 C26 H26A 108.6 . . ? C27 C26 H26B 108.6 . . ? P3 C26 H26B 108.6 . . ? H26A C26 H26B 107.6 . . ? C32 C27 C28 118.8(5) . . ? C32 C27 C26 117.0(5) . . ? C28 C27 C26 124.1(5) . . ? C27 C28 C29 118.4(5) . . ? C27 C28 P4 120.2(4) . . ? C29 C28 P4 121.3(4) . . ? C30 C29 C28 120.9(6) . . ? C30 C29 H29 119.6 . . ? C28 C29 H29 119.6 . . ? C31 C30 C29 121.1(6) . . ? C31 C30 H30 119.5 . . ? C29 C30 H30 119.5 . . ? C30 C31 C32 118.9(6) . . ? C30 C31 H31 120.6 . . ? C32 C31 H31 120.6 . . ? C31 C32 C27 121.9(6) . . ? C31 C32 H32 119.0 . . ? C27 C32 H32 119.0 . . ? C34 C33 C36 105.9(6) . . ? C34 C33 C35 110.0(5) . . ? C36 C33 C35 109.5(5) . . ? C34 C33 P3 108.5(4) . . ? C36 C33 P3 112.5(4) . . ? C35 C33 P3 110.2(4) . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C33 C35 H35A 109.5 . . ? C33 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C33 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C33 C36 H36A 109.5 . . ? C33 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C33 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C40 C37 C39 109.0(5) . . ? C40 C37 C38 108.1(5) . . ? C39 C37 C38 105.3(5) . . ? C40 C37 P3 107.5(4) . . ? C39 C37 P3 114.5(4) . . ? C38 C37 P3 112.3(4) . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C37 C39 H39A 109.5 . . ? C37 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C37 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C37 C40 H40A 109.5 . . ? C37 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C37 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? O5 C41 C42 105.9(5) . . ? O5 C41 C49 108.1(5) . . ? C42 C41 C49 111.7(5) . . ? O5 C41 P4 108.8(4) . . ? C42 C41 P4 111.1(4) . . ? C49 C41 P4 111.0(4) . . ? C41 C42 C43 111.1(5) . . ? C41 C42 H42A 109.4 . . ? C43 C42 H42A 109.4 . . ? C41 C42 H42B 109.4 . . ? C43 C42 H42B 109.4 . . ? H42A C42 H42B 108.0 . . ? O6 C43 O4 110.2(5) . . ? O6 C43 C50 107.2(5) . . ? O4 C43 C50 106.6(5) . . ? O6 C43 C42 108.3(5) . . ? O4 C43 C42 110.8(5) . . ? C50 C43 C42 113.7(5) . . ? O4 C44 C47 105.8(4) . . ? O4 C44 C45 109.2(4) . . ? C47 C44 C45 111.5(5) . . ? O4 C44 P4 106.4(4) . . ? C47 C44 P4 114.3(4) . . ? C45 C44 P4 109.3(4) . . ? C44 C45 C46 110.3(5) . . ? C44 C45 H45A 109.6 . . ? C46 C45 H45A 109.6 . . ? C44 C45 H45B 109.6 . . ? C46 C45 H45B 109.6 . . ? H45A C45 H45B 108.1 . . ? O6 C46 O5 110.8(4) . . ? O6 C46 C48 107.7(5) . . ? O5 C46 C48 106.0(5) . . ? O6 C46 C45 107.3(5) . . ? O5 C46 C45 112.2(5) . . ? C48 C46 C45 112.8(5) . . ? C44 C47 H47A 109.5 . . ? C44 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C44 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C46 C48 H48A 109.5 . . ? C46 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C46 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C41 C49 H49A 109.5 . . ? C41 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C41 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? C43 C50 H50A 109.5 . . ? C43 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C43 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? Cl5 C51 Cl6 114.3(5) . . ? Cl5 C51 H51A 108.7 . . ? Cl6 C51 H51A 108.7 . . ? Cl5 C51 H51B 108.7 . . ? Cl6 C51 H51B 108.7 . . ? H51A C51 H51B 107.6 . . ? Cl8 C52 Cl7 112.9(4) . . ? Cl8 C52 H52A 109.0 . . ? Cl7 C52 H52A 109.0 . . ? Cl8 C52 H52B 109.0 . . ? Cl7 C52 H52B 109.0 . . ? H52A C52 H52B 107.8 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag P2 Pt1 P1 C1 23.72(19) . . . . ? Cl2 Pt1 P1 C1 -162.54(19) . . . . ? Cl1 Pt1 P1 C1 -115.9(3) . . . . ? P2 Pt1 P1 C8 -96.95(19) . . . . ? Cl2 Pt1 P1 C8 76.78(19) . . . . ? Cl1 Pt1 P1 C8 123.4(3) . . . . ? P2 Pt1 P1 C12 132.4(2) . . . . ? Cl2 Pt1 P1 C12 -53.9(2) . . . . ? Cl1 Pt1 P1 C12 -7.3(3) . . . . ? P1 Pt1 P2 C3 20.21(19) . . . . ? Cl1 Pt1 P2 C3 -168.23(19) . . . . ? P1 Pt1 P2 C16 -104.69(19) . . . . ? Cl1 Pt1 P2 C16 66.87(19) . . . . ? P1 Pt1 P2 C19 145.8(2) . . . . ? Cl1 Pt1 P2 C19 -42.7(2) . . . . ? C8 P1 C1 C2 55.8(5) . . . . ? C12 P1 C1 C2 174.2(4) . . . . ? Pt1 P1 C1 C2 -67.5(4) . . . . ? P1 C1 C2 C7 -121.6(5) . . . . ? P1 C1 C2 C3 56.0(7) . . . . ? C7 C2 C3 C4 1.6(8) . . . . ? C1 C2 C3 C4 -175.9(5) . . . . ? C7 C2 C3 P2 -178.3(4) . . . . ? C1 C2 C3 P2 4.2(7) . . . . ? C16 P2 C3 C4 -91.7(5) . . . . ? C19 P2 C3 C4 5.8(5) . . . . ? Pt1 P2 C3 C4 137.1(4) . . . . ? C16 P2 C3 C2 88.2(5) . . . . ? C19 P2 C3 C2 -174.3(4) . . . . ? Pt1 P2 C3 C2 -43.0(5) . . . . ? C2 C3 C4 C5 -0.2(8) . . . . ? P2 C3 C4 C5 179.7(5) . . . . ? C3 C4 C5 C6 -1.5(9) . . . . ? C4 C5 C6 C7 1.8(9) . . . . ? C5 C6 C7 C2 -0.4(9) . . . . ? C3 C2 C7 C6 -1.3(9) . . . . ? C1 C2 C7 C6 176.3(5) . . . . ? C1 P1 C8 C10 49.3(4) . . . . ? C12 P1 C8 C10 -58.7(5) . . . . ? Pt1 P1 C8 C10 171.0(3) . . . . ? C1 P1 C8 C11 170.6(4) . . . . ? C12 P1 C8 C11 62.6(5) . . . . ? Pt1 P1 C8 C11 -67.7(4) . . . . ? C1 P1 C8 C9 -71.3(4) . . . . ? C12 P1 C8 C9 -179.3(4) . . . . ? Pt1 P1 C8 C9 50.4(4) . . . . ? C1 P1 C12 C15 86.7(4) . . . . ? C8 P1 C12 C15 -159.3(4) . . . . ? Pt1 P1 C12 C15 -29.2(4) . . . . ? C1 P1 C12 C13 -30.9(5) . . . . ? C8 P1 C12 C13 83.2(5) . . . . ? Pt1 P1 C12 C13 -146.8(4) . . . . ? C1 P1 C12 C14 -151.9(4) . . . . ? C8 P1 C12 C14 -37.9(5) . . . . ? Pt1 P1 C12 C14 92.2(4) . . . . ? C21 O1 C16 C17 46.8(6) . . . . ? C21 O1 C16 C22 167.4(4) . . . . ? C21 O1 C16 P2 -70.8(5) . . . . ? C3 P2 C16 O1 165.3(3) . . . . ? C19 P2 C16 O1 58.5(4) . . . . ? Pt1 P2 C16 O1 -64.2(3) . . . . ? C3 P2 C16 C17 46.9(4) . . . . ? C19 P2 C16 C17 -59.9(4) . . . . ? Pt1 P2 C16 C17 177.3(3) . . . . ? C3 P2 C16 C22 -78.0(5) . . . . ? C19 P2 C16 C22 175.2(4) . . . . ? Pt1 P2 C16 C22 52.5(5) . . . . ? O1 C16 C17 C18 -48.4(6) . . . . ? C22 C16 C17 C18 -165.9(5) . . . . ? P2 C16 C17 C18 67.7(5) . . . . ? C21 O3 C18 O2 58.4(5) . . . . ? C21 O3 C18 C23 173.6(4) . . . . ? C21 O3 C18 C17 -64.6(5) . . . . ? C19 O2 C18 O3 -57.0(6) . . . . ? C19 O2 C18 C23 -172.3(4) . . . . ? C19 O2 C18 C17 63.5(6) . . . . ? C16 C17 C18 O3 58.0(6) . . . . ? C16 C17 C18 O2 -63.9(6) . . . . ? C16 C17 C18 C23 175.7(5) . . . . ? C18 O2 C19 C20 55.0(5) . . . . ? C18 O2 C19 C24 173.9(4) . . . . ? C18 O2 C19 P2 -64.7(5) . . . . ? C3 P2 C19 O2 -49.4(4) . . . . ? C16 P2 C19 O2 56.8(4) . . . . ? Pt1 P2 C19 O2 179.8(3) . . . . ? C3 P2 C19 C20 -165.3(4) . . . . ? C16 P2 C19 C20 -59.1(4) . . . . ? Pt1 P2 C19 C20 63.9(4) . . . . ? C3 P2 C19 C24 69.6(5) . . . . ? C16 P2 C19 C24 175.7(4) . . . . ? Pt1 P2 C19 C24 -61.2(5) . . . . ? O2 C19 C20 C21 -55.5(5) . . . . ? C24 C19 C20 C21 -171.9(4) . . . . ? P2 C19 C20 C21 62.8(5) . . . . ? C18 O3 C21 O1 61.2(6) . . . . ? C18 O3 C21 C25 176.3(4) . . . . ? C18 O3 C21 C20 -61.6(5) . . . . ? C16 O1 C21 O3 -52.9(6) . . . . ? C16 O1 C21 C25 -168.8(5) . . . . ? C16 O1 C21 C20 68.1(6) . . . . ? C19 C20 C21 O3 61.8(5) . . . . ? C19 C20 C21 O1 -59.9(6) . . . . ? C19 C20 C21 C25 -179.3(5) . . . . ? P4 Pt2 P3 C26 -20.9(2) . . . . ? Cl4 Pt2 P3 C26 167.8(2) . . . . ? Cl3 Pt2 P3 C26 110.6(3) . . . . ? P4 Pt2 P3 C33 100.5(2) . . . . ? Cl4 Pt2 P3 C33 -70.8(2) . . . . ? Cl3 Pt2 P3 C33 -128.1(3) . . . . ? P4 Pt2 P3 C37 -129.0(2) . . . . ? Cl4 Pt2 P3 C37 59.8(2) . . . . ? Cl3 Pt2 P3 C37 2.5(3) . . . . ? P3 Pt2 P4 C28 -23.6(2) . . . . ? Cl3 Pt2 P4 C28 168.1(2) . . . . ? P3 Pt2 P4 C44 102.2(2) . . . . ? Cl3 Pt2 P4 C44 -66.1(2) . . . . ? P3 Pt2 P4 C41 -147.7(2) . . . . ? Cl3 Pt2 P4 C41 44.1(2) . . . . ? C33 P3 C26 C27 -59.3(5) . . . . ? C37 P3 C26 C27 -177.4(4) . . . . ? Pt2 P3 C26 C27 66.3(4) . . . . ? P3 C26 C27 C32 120.2(5) . . . . ? P3 C26 C27 C28 -57.0(7) . . . . ? C32 C27 C28 C29 -2.6(8) . . . . ? C26 C27 C28 C29 174.6(5) . . . . ? C32 C27 C28 P4 178.5(4) . . . . ? C26 C27 C28 P4 -4.3(8) . . . . ? C44 P4 C28 C27 -87.4(5) . . . . ? C41 P4 C28 C27 175.3(5) . . . . ? Pt2 P4 C28 C27 45.6(5) . . . . ? C44 P4 C28 C29 93.7(5) . . . . ? C41 P4 C28 C29 -3.6(6) . . . . ? Pt2 P4 C28 C29 -133.3(5) . . . . ? C27 C28 C29 C30 1.6(9) . . . . ? P4 C28 C29 C30 -179.5(5) . . . . ? C28 C29 C30 C31 -0.2(10) . . . . ? C29 C30 C31 C32 -0.1(10) . . . . ? C30 C31 C32 C27 -1.0(10) . . . . ? C28 C27 C32 C31 2.4(9) . . . . ? C26 C27 C32 C31 -175.0(6) . . . . ? C26 P3 C33 C34 71.9(5) . . . . ? C37 P3 C33 C34 179.7(4) . . . . ? Pt2 P3 C33 C34 -50.8(5) . . . . ? C26 P3 C33 C36 -171.2(5) . . . . ? C37 P3 C33 C36 -63.4(5) . . . . ? Pt2 P3 C33 C36 66.0(5) . . . . ? C26 P3 C33 C35 -48.6(5) . . . . ? C37 P3 C33 C35 59.2(5) . . . . ? Pt2 P3 C33 C35 -171.4(4) . . . . ? C26 P3 C37 C40 -84.7(4) . . . . ? C33 P3 C37 C40 161.9(4) . . . . ? Pt2 P3 C37 C40 30.8(4) . . . . ? C26 P3 C37 C39 154.0(4) . . . . ? C33 P3 C37 C39 40.6(5) . . . . ? Pt2 P3 C37 C39 -90.5(4) . . . . ? C26 P3 C37 C38 34.0(5) . . . . ? C33 P3 C37 C38 -79.4(5) . . . . ? Pt2 P3 C37 C38 149.5(4) . . . . ? C46 O5 C41 C42 -53.4(6) . . . . ? C46 O5 C41 C49 -173.2(4) . . . . ? C46 O5 C41 P4 66.1(5) . . . . ? C28 P4 C41 O5 48.5(4) . . . . ? C44 P4 C41 O5 -57.7(4) . . . . ? Pt2 P4 C41 O5 177.2(3) . . . . ? C28 P4 C41 C42 164.6(4) . . . . ? C44 P4 C41 C42 58.4(4) . . . . ? Pt2 P4 C41 C42 -66.6(5) . . . . ? C28 P4 C41 C49 -70.4(4) . . . . ? C44 P4 C41 C49 -176.6(4) . . . . ? Pt2 P4 C41 C49 58.4(4) . . . . ? O5 C41 C42 C43 54.8(6) . . . . ? C49 C41 C42 C43 172.2(5) . . . . ? P4 C41 C42 C43 -63.2(6) . . . . ? C46 O6 C43 O4 -60.7(6) . . . . ? C46 O6 C43 C50 -176.3(5) . . . . ? C46 O6 C43 C42 60.6(6) . . . . ? C44 O4 C43 O6 52.0(7) . . . . ? C44 O4 C43 C50 168.0(5) . . . . ? C44 O4 C43 C42 -67.8(6) . . . . ? C41 C42 C43 O6 -60.8(6) . . . . ? C41 C42 C43 O4 60.1(6) . . . . ? C41 C42 C43 C50 -179.9(5) . . . . ? C43 O4 C44 C47 -167.0(5) . . . . ? C43 O4 C44 C45 -46.9(6) . . . . ? C43 O4 C44 P4 71.0(5) . . . . ? C28 P4 C44 O4 -164.5(3) . . . . ? C41 P4 C44 O4 -57.6(4) . . . . ? Pt2 P4 C44 O4 65.0(4) . . . . ? C28 P4 C44 C47 79.0(4) . . . . ? C41 P4 C44 C47 -174.1(4) . . . . ? Pt2 P4 C44 C47 -51.4(4) . . . . ? C28 P4 C44 C45 -46.7(4) . . . . ? C41 P4 C44 C45 60.2(4) . . . . ? Pt2 P4 C44 C45 -177.2(3) . . . . ? O4 C44 C45 C46 49.5(6) . . . . ? C47 C44 C45 C46 166.0(5) . . . . ? P4 C44 C45 C46 -66.6(5) . . . . ? C43 O6 C46 O5 -57.3(6) . . . . ? C43 O6 C46 C48 -172.8(5) . . . . ? C43 O6 C46 C45 65.5(6) . . . . ? C41 O5 C46 O6 55.8(6) . . . . ? C41 O5 C46 C48 172.4(4) . . . . ? C41 O5 C46 C45 -64.1(6) . . . . ? C44 C45 C46 O6 -59.9(6) . . . . ? C44 C45 C46 O5 62.0(6) . . . . ? C44 C45 C46 C48 -178.4(5) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 3.402 _refine_diff_density_min -2.557 _refine_diff_density_rms 0.185 data_3c _database_code_depnum_ccdc_archive 'CCDC 897393' #TrackingRef '- all.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C27.87 H36.61 Cl1.13 P2 Pt' _chemical_formula_sum 'C27.87 H36.61 Cl1.13 P2 Pt' _chemical_formula_weight 668.70 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' _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 11.4182(1) _cell_length_b 15.7441(1) _cell_length_c 15.0578(1) _cell_angle_alpha 90.00 _cell_angle_beta 103.5301(8) _cell_angle_gamma 90.00 _cell_volume 2631.80(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 74574 _cell_measurement_theta_min 2.2394 _cell_measurement_theta_max 29.9997 _exptl_crystal_description rhomboid _exptl_crystal_colour colourless _exptl_crystal_size_max 0.4885 _exptl_crystal_size_mid 0.4704 _exptl_crystal_size_min 0.1501 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.688 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1323.9 _exptl_absorpt_coefficient_mu 5.582 _exptl_absorpt_correction_type gaussian _exptl_absorpt_correction_T_min 0.091 _exptl_absorpt_correction_T_max 0.485 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) Numerical absorption correction based on gaussian integration over a multifaceted crystal model ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'Oxford diffraction Gemini R Ultra' _diffrn_measurement_method 'Narrow scans in Omega, 1 degree width' _diffrn_detector_area_resol_mean 10.4752 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 142333 _diffrn_reflns_av_R_equivalents 0.0458 _diffrn_reflns_av_sigmaI/netI 0.0183 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.24 _diffrn_reflns_theta_max 30.10 _reflns_number_total 7730 _reflns_number_gt 6455 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0184P)^2^+7.6866P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00014(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 7730 _refine_ls_number_parameters 301 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0360 _refine_ls_R_factor_gt 0.0254 _refine_ls_wR_factor_ref 0.0592 _refine_ls_wR_factor_gt 0.0518 _refine_ls_goodness_of_fit_ref 1.143 _refine_ls_restrained_S_all 1.143 _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 0.021841(10) 0.214045(7) 0.367726(7) 0.01583(4) Uani 1 1 d . . . P2 P -0.09910(7) 0.25246(5) 0.45558(5) 0.01428(13) Uani 1 1 d . A . P1 P 0.15895(7) 0.32190(5) 0.41777(5) 0.01516(14) Uani 1 1 d . A . C12 C 0.3015(3) 0.28728(19) 0.4999(2) 0.0181(5) Uani 1 1 d . . . C4 C -0.0665(3) 0.2862(2) 0.6427(2) 0.0206(6) Uani 1 1 d . A . H4 H -0.1226 0.2432 0.6418 0.025 Uiso 1 1 calc R . . C3 C -0.0328(3) 0.30779(18) 0.5621(2) 0.0159(5) Uani 1 1 d . . . C22 C -0.2201(3) 0.32387(18) 0.3998(2) 0.0169(5) Uani 1 1 d . . . C2 C 0.0513(3) 0.37321(18) 0.5638(2) 0.0160(5) Uani 1 1 d . A . C27 C -0.2428(3) 0.3353(2) 0.3056(2) 0.0241(6) Uani 1 1 d . A . H27 H -0.1959 0.3070 0.2722 0.029 Uiso 1 1 calc R . . C5 C -0.0175(3) 0.3279(2) 0.7240(2) 0.0253(7) Uani 1 1 d . . . H5 H -0.0405 0.3127 0.7771 0.030 Uiso 1 1 calc R A . C21 C -0.2988(3) 0.1536(2) 0.4770(2) 0.0217(6) Uani 1 1 d . A . H21 H -0.3483 0.1975 0.4486 0.026 Uiso 1 1 calc R . . C8 C 0.1858(3) 0.3904(2) 0.3206(2) 0.0205(6) Uani 1 1 d . . . C17 C -0.1016(3) 0.0946(2) 0.5350(2) 0.0221(6) Uani 1 1 d . A . H17 H -0.0183 0.0988 0.5449 0.027 Uiso 1 1 calc R . . C1 C 0.0912(3) 0.40197(18) 0.4801(2) 0.0166(5) Uani 1 1 d . . . H1A H 0.1493 0.4474 0.4982 0.020 Uiso 1 1 calc R A . H1B H 0.0219 0.4260 0.4378 0.020 Uiso 1 1 calc R . . C16 C -0.1741(3) 0.16157(18) 0.4930(2) 0.0165(5) Uani 1 1 d . . . C23 C -0.2907(3) 0.3660(2) 0.4493(2) 0.0221(6) Uani 1 1 d . A . H23 H -0.2758 0.3592 0.5123 0.026 Uiso 1 1 calc R . . C13 C 0.2639(3) 0.2303(2) 0.5713(2) 0.0282(7) Uani 1 1 d . A . H13A H 0.3345 0.2078 0.6121 0.042 Uiso 1 1 calc R . . H13B H 0.2151 0.1844 0.5410 0.042 Uiso 1 1 calc R . . H13C H 0.2186 0.2631 0.6053 0.042 Uiso 1 1 calc R . . C20 C -0.3493(3) 0.0799(2) 0.5034(3) 0.0294(7) Uani 1 1 d . . . H20 H -0.4326 0.0747 0.4923 0.035 Uiso 1 1 calc R A . C14 C 0.3769(3) 0.3614(2) 0.5483(2) 0.0272(7) Uani 1 1 d . A . H14A H 0.3300 0.3939 0.5814 0.041 Uiso 1 1 calc R . . H14B H 0.4007 0.3970 0.5039 0.041 Uiso 1 1 calc R . . H14C H 0.4474 0.3398 0.5901 0.041 Uiso 1 1 calc R . . C24 C -0.3835(3) 0.4185(2) 0.4044(3) 0.0265(7) Uani 1 1 d . . . H24 H -0.4314 0.4463 0.4374 0.032 Uiso 1 1 calc R A . C25 C -0.4052(3) 0.4296(2) 0.3111(3) 0.0284(7) Uani 1 1 d . A . H25 H -0.4676 0.4648 0.2815 0.034 Uiso 1 1 calc R . . C6 C 0.0654(3) 0.3920(2) 0.7260(2) 0.0223(6) Uani 1 1 d . A . H6 H 0.0984 0.4202 0.7803 0.027 Uiso 1 1 calc R . . C10 C 0.2782(3) 0.3508(2) 0.2737(2) 0.0295(7) Uani 1 1 d . A . H10A H 0.2742 0.3787 0.2164 0.044 Uiso 1 1 calc R . . H10B H 0.2608 0.2915 0.2632 0.044 Uiso 1 1 calc R . . H10C H 0.3576 0.3573 0.3122 0.044 Uiso 1 1 calc R . . C11 C 0.0638(3) 0.3942(2) 0.2505(2) 0.0256(7) Uani 1 1 d . A . H11A H 0.0703 0.4311 0.2012 0.038 Uiso 1 1 calc R . . H11B H 0.0034 0.4157 0.2796 0.038 Uiso 1 1 calc R . . H11C H 0.0417 0.3383 0.2272 0.038 Uiso 1 1 calc R . . C9 C 0.2256(3) 0.4816(2) 0.3495(2) 0.0287(7) Uani 1 1 d . A . H9A H 0.2968 0.4799 0.3983 0.043 Uiso 1 1 calc R . . H9B H 0.1624 0.5102 0.3698 0.043 Uiso 1 1 calc R . . H9C H 0.2427 0.5115 0.2984 0.043 Uiso 1 1 calc R . . C19 C -0.2766(3) 0.0149(2) 0.5459(3) 0.0286(7) Uani 1 1 d . A . H19 H -0.3109 -0.0339 0.5637 0.034 Uiso 1 1 calc R . . C18 C -0.1524(3) 0.0220(2) 0.5621(2) 0.0275(7) Uani 1 1 d . . . H18 H -0.1034 -0.0218 0.5910 0.033 Uiso 1 1 calc R A . C26 C -0.3347(3) 0.3886(2) 0.2615(3) 0.0299(7) Uani 1 1 d . . . H26 H -0.3488 0.3966 0.1987 0.036 Uiso 1 1 calc R A . C15 C 0.3798(3) 0.2330(2) 0.4518(2) 0.0272(7) Uani 1 1 d . A . H15A H 0.4193 0.2690 0.4164 0.041 Uiso 1 1 calc R . . H15B H 0.3299 0.1928 0.4122 0.041 Uiso 1 1 calc R . . H15C H 0.4392 0.2032 0.4966 0.041 Uiso 1 1 calc R . . Cl2 Cl 0.13360(8) 0.15211(6) 0.27050(6) 0.02937(17) Uani 1 1 d . A . C28 C -0.1150(7) 0.1237(5) 0.3115(5) 0.0208(13) Uani 0.870(6) 1 d P A 1 H28A H -0.1022 0.0726 0.3474 0.031 Uiso 0.870(6) 1 calc PR A 1 H28B H -0.1118 0.1108 0.2498 0.031 Uiso 0.870(6) 1 calc PR A 1 H28C H -0.1926 0.1469 0.3121 0.031 Uiso 0.870(6) 1 calc PR A 1 Cl1 Cl -0.1039(17) 0.1132(12) 0.3021(12) 0.02937(17) Uani 0.130(6) 1 d P A 2 C7 C 0.0992(3) 0.4141(2) 0.6465(2) 0.0194(6) Uani 1 1 d . . . H7 H 0.1553 0.4573 0.6483 0.023 Uiso 1 1 calc R A . 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 0.01831(6) 0.01548(5) 0.01405(6) -0.00046(4) 0.00453(4) 0.00185(4) P2 0.0140(3) 0.0144(3) 0.0146(3) 0.0000(3) 0.0037(3) 0.0003(3) P1 0.0148(3) 0.0157(3) 0.0159(3) 0.0009(3) 0.0054(3) 0.0006(3) Cl1 0.0308(4) 0.0310(4) 0.0288(4) -0.0042(3) 0.0120(3) 0.0042(3) C12 0.0172(13) 0.0198(13) 0.0181(13) 0.0014(11) 0.0057(11) 0.0014(11) C1 0.0180(14) 0.0166(13) 0.0158(13) -0.0005(10) 0.0053(11) -0.0009(10) C2 0.0145(13) 0.0176(13) 0.0160(13) 0.0009(10) 0.0037(10) 0.0012(10) C3 0.0139(13) 0.0190(13) 0.0146(13) 0.0005(10) 0.0031(10) 0.0016(10) C4 0.0211(14) 0.0246(14) 0.0170(14) 0.0006(12) 0.0063(11) -0.0038(12) C5 0.0282(17) 0.0319(17) 0.0164(15) 0.0031(13) 0.0068(13) 0.0013(14) C6 0.0230(15) 0.0278(15) 0.0151(14) -0.0046(12) 0.0025(12) 0.0018(12) C7 0.0163(14) 0.0210(14) 0.0210(15) -0.0029(11) 0.0045(11) 0.0002(11) C8 0.0227(15) 0.0219(14) 0.0190(14) 0.0031(11) 0.0089(12) 0.0002(12) C9 0.0339(19) 0.0247(16) 0.0285(18) 0.0062(13) 0.0094(15) -0.0063(14) C10 0.0317(18) 0.0351(18) 0.0269(17) 0.0071(14) 0.0170(15) 0.0053(15) C11 0.0293(17) 0.0282(16) 0.0202(15) 0.0058(13) 0.0073(13) 0.0020(13) Cl2 0.0308(4) 0.0310(4) 0.0288(4) -0.0042(3) 0.0120(3) 0.0042(3) C13 0.0238(16) 0.0359(19) 0.0256(17) 0.0118(14) 0.0069(13) 0.0077(14) C14 0.0211(16) 0.0332(17) 0.0249(17) -0.0045(14) 0.0006(13) -0.0007(13) C15 0.0230(16) 0.0304(17) 0.0277(17) 0.0002(13) 0.0049(13) 0.0066(13) C16 0.0159(13) 0.0171(13) 0.0176(14) -0.0007(10) 0.0062(11) -0.0005(10) C17 0.0199(15) 0.0216(14) 0.0249(16) 0.0029(12) 0.0053(12) 0.0020(12) C18 0.0316(18) 0.0196(15) 0.0321(18) 0.0066(13) 0.0089(15) 0.0034(13) C19 0.0353(19) 0.0174(14) 0.0366(19) 0.0016(13) 0.0155(16) -0.0035(13) C20 0.0231(17) 0.0235(16) 0.043(2) 0.0011(14) 0.0107(15) -0.0034(13) C21 0.0167(14) 0.0188(14) 0.0299(17) 0.0020(12) 0.0059(12) 0.0003(11) C22 0.0165(13) 0.0145(12) 0.0189(14) 0.0024(10) 0.0028(11) -0.0007(10) C23 0.0225(15) 0.0184(14) 0.0251(16) 0.0000(12) 0.0051(13) 0.0013(12) C24 0.0186(15) 0.0195(14) 0.043(2) 0.0012(13) 0.0100(14) 0.0025(12) C25 0.0176(15) 0.0205(15) 0.044(2) 0.0098(14) 0.0006(14) 0.0000(12) C26 0.0278(18) 0.0314(17) 0.0259(17) 0.0093(14) -0.0026(14) 0.0015(14) C27 0.0237(16) 0.0266(16) 0.0205(15) -0.0005(12) 0.0019(12) 0.0014(13) C28 0.017(2) 0.028(3) 0.019(3) -0.0080(19) 0.0075(17) -0.0023(19) _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 C28 2.136(8) . ? Pt1 P2 2.2085(7) . ? Pt1 Cl1 2.21(2) . ? Pt1 P1 2.3131(8) . ? Pt1 Cl2 2.3658(8) . ? P2 C16 1.823(3) . ? P2 C22 1.827(3) . ? P2 C3 1.827(3) . ? P1 C1 1.846(3) . ? P1 C12 1.880(3) . ? P1 C8 1.900(3) . ? C12 C14 1.530(5) . ? C12 C13 1.536(4) . ? C12 C15 1.536(4) . ? C4 C5 1.386(5) . ? C4 C3 1.398(4) . ? C4 H4 0.9300 . ? C3 C2 1.404(4) . ? C22 C23 1.389(4) . ? C22 C27 1.392(4) . ? C2 C7 1.395(4) . ? C2 C1 1.506(4) . ? C27 C26 1.385(5) . ? C27 H27 0.9300 . ? C5 C6 1.379(5) . ? C5 H5 0.9300 . ? C21 C16 1.393(4) . ? C21 C20 1.395(4) . ? C21 H21 0.9300 . ? C8 C10 1.532(5) . ? C8 C9 1.538(5) . ? C8 C11 1.538(5) . ? C17 C18 1.386(5) . ? C17 C16 1.397(4) . ? C17 H17 0.9300 . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C23 C24 1.388(4) . ? C23 H23 0.9300 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C20 C19 1.378(5) . ? C20 H20 0.9300 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C24 C25 1.380(5) . ? C24 H24 0.9300 . ? C25 C26 1.381(5) . ? C25 H25 0.9300 . ? C6 C7 1.385(4) . ? C6 H6 0.9300 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C19 C18 1.386(5) . ? C19 H19 0.9300 . ? C18 H18 0.9300 . ? C26 H26 0.9300 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C7 H7 0.9300 . ? 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 C28 Pt1 P2 85.28(17) . . ? C28 Pt1 Cl1 6.8(5) . . ? P2 Pt1 Cl1 91.9(4) . . ? C28 Pt1 P1 174.1(2) . . ? P2 Pt1 P1 94.26(3) . . ? Cl1 Pt1 P1 172.5(4) . . ? C28 Pt1 Cl2 86.04(17) . . ? P2 Pt1 Cl2 170.73(3) . . ? Cl1 Pt1 Cl2 79.4(4) . . ? P1 Pt1 Cl2 94.72(3) . . ? C16 P2 C22 105.43(14) . . ? C16 P2 C3 103.34(14) . . ? C22 P2 C3 102.95(13) . . ? C16 P2 Pt1 112.03(10) . . ? C22 P2 Pt1 113.87(10) . . ? C3 P2 Pt1 117.89(10) . . ? C1 P1 C12 105.34(14) . . ? C1 P1 C8 99.59(14) . . ? C12 P1 C8 113.63(14) . . ? C1 P1 Pt1 109.56(10) . . ? C12 P1 Pt1 114.66(10) . . ? C8 P1 Pt1 112.61(10) . . ? C14 C12 C13 109.3(3) . . ? C14 C12 C15 108.9(3) . . ? C13 C12 C15 107.1(3) . . ? C14 C12 P1 113.4(2) . . ? C13 C12 P1 106.8(2) . . ? C15 C12 P1 111.1(2) . . ? C5 C4 C3 121.0(3) . . ? C5 C4 H4 119.5 . . ? C3 C4 H4 119.5 . . ? C4 C3 C2 119.2(3) . . ? C4 C3 P2 120.3(2) . . ? C2 C3 P2 120.4(2) . . ? C23 C22 C27 119.5(3) . . ? C23 C22 P2 121.2(2) . . ? C27 C22 P2 119.3(2) . . ? C7 C2 C3 118.6(3) . . ? C7 C2 C1 118.4(3) . . ? C3 C2 C1 123.0(3) . . ? C26 C27 C22 120.5(3) . . ? C26 C27 H27 119.8 . . ? C22 C27 H27 119.8 . . ? C6 C5 C4 119.9(3) . . ? C6 C5 H5 120.0 . . ? C4 C5 H5 120.0 . . ? C16 C21 C20 119.9(3) . . ? C16 C21 H21 120.0 . . ? C20 C21 H21 120.0 . . ? C10 C8 C9 108.7(3) . . ? C10 C8 C11 108.1(3) . . ? C9 C8 C11 108.5(3) . . ? C10 C8 P1 112.1(2) . . ? C9 C8 P1 113.7(2) . . ? C11 C8 P1 105.5(2) . . ? C18 C17 C16 120.7(3) . . ? C18 C17 H17 119.6 . . ? C16 C17 H17 119.6 . . ? C2 C1 P1 117.7(2) . . ? C2 C1 H1A 107.9 . . ? P1 C1 H1A 107.9 . . ? C2 C1 H1B 107.9 . . ? P1 C1 H1B 107.9 . . ? H1A C1 H1B 107.2 . . ? C21 C16 C17 119.0(3) . . ? C21 C16 P2 123.5(2) . . ? C17 C16 P2 117.4(2) . . ? C24 C23 C22 119.7(3) . . ? C24 C23 H23 120.2 . . ? C22 C23 H23 120.2 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C19 C20 C21 120.4(3) . . ? C19 C20 H20 119.8 . . ? C21 C20 H20 119.8 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C25 C24 C23 120.4(3) . . ? C25 C24 H24 119.8 . . ? C23 C24 H24 119.8 . . ? C24 C25 C26 120.2(3) . . ? C24 C25 H25 119.9 . . ? C26 C25 H25 119.9 . . ? C5 C6 C7 119.6(3) . . ? C5 C6 H6 120.2 . . ? C7 C6 H6 120.2 . . ? C8 C10 H10A 109.5 . . ? C8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C8 C11 H11A 109.5 . . ? C8 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C8 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C20 C19 C18 120.2(3) . . ? C20 C19 H19 119.9 . . ? C18 C19 H19 119.9 . . ? C17 C18 C19 119.7(3) . . ? C17 C18 H18 120.1 . . ? C19 C18 H18 120.1 . . ? C25 C26 C27 119.7(3) . . ? C25 C26 H26 120.2 . . ? C27 C26 H26 120.2 . . ? C12 C15 H15A 109.5 . . ? C12 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C12 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? Pt1 C28 H28A 109.5 . . ? Pt1 C28 H28B 109.5 . . ? Pt1 C28 H28C 109.5 . . ? C6 C7 C2 121.7(3) . . ? C6 C7 H7 119.2 . . ? C2 C7 H7 119.2 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C28 Pt1 P2 C16 38.6(3) . . . . ? Cl1 Pt1 P2 C16 37.0(5) . . . . ? P1 Pt1 P2 C16 -147.36(11) . . . . ? Cl2 Pt1 P2 C16 18.1(2) . . . . ? C28 Pt1 P2 C22 -80.9(3) . . . . ? Cl1 Pt1 P2 C22 -82.5(5) . . . . ? P1 Pt1 P2 C22 93.11(11) . . . . ? Cl2 Pt1 P2 C22 -101.4(2) . . . . ? C28 Pt1 P2 C3 158.3(3) . . . . ? Cl1 Pt1 P2 C3 156.7(5) . . . . ? P1 Pt1 P2 C3 -27.65(11) . . . . ? Cl2 Pt1 P2 C3 137.8(2) . . . . ? C28 Pt1 P1 C1 71.2(16) . . . . ? P2 Pt1 P1 C1 -14.08(10) . . . . ? Cl1 Pt1 P1 C1 130(3) . . . . ? Cl2 Pt1 P1 C1 168.24(10) . . . . ? C28 Pt1 P1 C12 -170.6(16) . . . . ? P2 Pt1 P1 C12 104.09(11) . . . . ? Cl1 Pt1 P1 C12 -112(3) . . . . ? Cl2 Pt1 P1 C12 -73.59(11) . . . . ? C28 Pt1 P1 C8 -38.6(16) . . . . ? P2 Pt1 P1 C8 -123.92(11) . . . . ? Cl1 Pt1 P1 C8 20(3) . . . . ? Cl2 Pt1 P1 C8 58.40(11) . . . . ? C1 P1 C12 C14 -46.3(3) . . . . ? C8 P1 C12 C14 61.7(3) . . . . ? Pt1 P1 C12 C14 -166.82(19) . . . . ? C1 P1 C12 C13 74.1(2) . . . . ? C8 P1 C12 C13 -177.9(2) . . . . ? Pt1 P1 C12 C13 -46.4(2) . . . . ? C1 P1 C12 C15 -169.4(2) . . . . ? C8 P1 C12 C15 -61.4(3) . . . . ? Pt1 P1 C12 C15 70.1(2) . . . . ? C5 C4 C3 C2 -0.5(5) . . . . ? C5 C4 C3 P2 -179.6(3) . . . . ? C16 P2 C3 C4 -12.5(3) . . . . ? C22 P2 C3 C4 97.1(3) . . . . ? Pt1 P2 C3 C4 -136.7(2) . . . . ? C16 P2 C3 C2 168.4(2) . . . . ? C22 P2 C3 C2 -82.0(3) . . . . ? Pt1 P2 C3 C2 44.2(3) . . . . ? C16 P2 C22 C23 68.5(3) . . . . ? C3 P2 C22 C23 -39.5(3) . . . . ? Pt1 P2 C22 C23 -168.3(2) . . . . ? C16 P2 C22 C27 -110.7(3) . . . . ? C3 P2 C22 C27 141.3(3) . . . . ? Pt1 P2 C22 C27 12.5(3) . . . . ? C4 C3 C2 C7 0.6(4) . . . . ? P2 C3 C2 C7 179.7(2) . . . . ? C4 C3 C2 C1 -178.8(3) . . . . ? P2 C3 C2 C1 0.3(4) . . . . ? C23 C22 C27 C26 0.2(5) . . . . ? P2 C22 C27 C26 179.5(3) . . . . ? C3 C4 C5 C6 0.3(5) . . . . ? C1 P1 C8 C10 161.2(2) . . . . ? C12 P1 C8 C10 49.7(3) . . . . ? Pt1 P1 C8 C10 -82.8(2) . . . . ? C1 P1 C8 C9 37.4(3) . . . . ? C12 P1 C8 C9 -74.1(3) . . . . ? Pt1 P1 C8 C9 153.4(2) . . . . ? C1 P1 C8 C11 -81.4(2) . . . . ? C12 P1 C8 C11 167.1(2) . . . . ? Pt1 P1 C8 C11 34.6(2) . . . . ? C7 C2 C1 P1 123.0(3) . . . . ? C3 C2 C1 P1 -57.6(4) . . . . ? C12 P1 C1 C2 -63.9(2) . . . . ? C8 P1 C1 C2 178.2(2) . . . . ? Pt1 P1 C1 C2 59.9(2) . . . . ? C20 C21 C16 C17 0.6(5) . . . . ? C20 C21 C16 P2 176.5(3) . . . . ? C18 C17 C16 C21 -1.4(5) . . . . ? C18 C17 C16 P2 -177.5(3) . . . . ? C22 P2 C16 C21 1.3(3) . . . . ? C3 P2 C16 C21 109.1(3) . . . . ? Pt1 P2 C16 C21 -123.0(3) . . . . ? C22 P2 C16 C17 177.3(2) . . . . ? C3 P2 C16 C17 -75.0(3) . . . . ? Pt1 P2 C16 C17 52.9(3) . . . . ? C27 C22 C23 C24 0.5(5) . . . . ? P2 C22 C23 C24 -178.7(2) . . . . ? C16 C21 C20 C19 0.3(5) . . . . ? C22 C23 C24 C25 -0.7(5) . . . . ? C23 C24 C25 C26 0.0(5) . . . . ? C4 C5 C6 C7 -0.1(5) . . . . ? C21 C20 C19 C18 -0.5(6) . . . . ? C16 C17 C18 C19 1.2(5) . . . . ? C20 C19 C18 C17 -0.3(6) . . . . ? C24 C25 C26 C27 0.8(5) . . . . ? C22 C27 C26 C25 -0.9(5) . . . . ? C5 C6 C7 C2 0.2(5) . . . . ? C3 C2 C7 C6 -0.4(4) . . . . ? C1 C2 C7 C6 179.0(3) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 30.10 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 3.368 _refine_diff_density_min -1.200 _refine_diff_density_rms 0.139 data_3d4d _database_code_depnum_ccdc_archive 'CCDC 897394' #TrackingRef '- all.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H41 Cl P2 Pt' _chemical_formula_sum 'C30 H41 Cl P2 Pt' _chemical_formula_weight 694.10 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.9460(5) _cell_length_b 15.7116(6) _cell_length_c 18.9402(7) _cell_angle_alpha 90.00 _cell_angle_beta 120.965(3) _cell_angle_gamma 90.00 _cell_volume 2793.1(2) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9967 _cell_measurement_theta_min 2.173 _cell_measurement_theta_max 25.894 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.651 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1384 _exptl_absorpt_coefficient_mu 5.251 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5420 _exptl_absorpt_correction_T_max 0.6487 _exptl_absorpt_process_details 'SADABS V2008/1' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-AXS Kappa with CCD area detector' _diffrn_measurement_method '\w & \f scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 81357 _diffrn_reflns_av_R_equivalents 0.0610 _diffrn_reflns_av_sigmaI/netI 0.0277 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.51 _diffrn_reflns_theta_max 27.58 _reflns_number_total 6438 _reflns_number_gt 5569 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Apex II (Bruker-AXS, 2007)' _computing_cell_refinement 'Apex II (Bruker-AXS, 2007)' _computing_data_reduction ; SAINT v7.34A (Bruker-AXS, 2007) & XPREP v2005/4 (Bruker-AXS, 2005) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0232P)^2^+14.4297P] 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 6438 _refine_ls_number_parameters 348 _refine_ls_number_restraints 216 _refine_ls_R_factor_all 0.0489 _refine_ls_R_factor_gt 0.0393 _refine_ls_wR_factor_ref 0.0871 _refine_ls_wR_factor_gt 0.0844 _refine_ls_goodness_of_fit_ref 1.199 _refine_ls_restrained_S_all 1.179 _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 0.41393(2) 0.865972(12) 0.793858(12) 0.02546(7) Uani 1 1 d . . . P1 P 0.40501(15) 0.91497(8) 0.67724(8) 0.0254(3) Uani 1 1 d . A . P2 P 0.19137(14) 0.91275(8) 0.75385(8) 0.0213(3) Uani 1 1 d . A . Cl1A Cl 0.6476(2) 0.81944(16) 0.85967(15) 0.0422(8) Uani 0.586(7) 1 d P A 1 C1A C 0.4442(4) 0.80953(18) 0.91289(18) 0.0451(10) Uani 0.586(7) 1 d P A 1 H1A1 H 0.4721 0.8546 0.9541 0.068 Uiso 0.586(7) 1 calc PR A 1 H1A2 H 0.5187 0.7659 0.9335 0.068 Uiso 0.586(7) 1 calc PR A 1 H1A3 H 0.3546 0.7838 0.9021 0.068 Uiso 0.586(7) 1 calc PR A 1 Cl1B Cl 0.4442(4) 0.80953(18) 0.91289(18) 0.0451(10) Uani 0.414(7) 1 d P A 2 C1B C 0.6476(2) 0.81944(16) 0.85967(15) 0.0422(8) Uani 0.414(7) 1 d P A 2 H1B1 H 0.6496 0.7588 0.8484 0.063 Uiso 0.414(7) 1 calc PR A 2 H1B2 H 0.6921 0.8282 0.9191 0.063 Uiso 0.414(7) 1 calc PR A 2 H1B3 H 0.7000 0.8517 0.8394 0.063 Uiso 0.414(7) 1 calc PR A 2 C2 C 0.2229(6) 0.9525(4) 0.6024(3) 0.0318(12) Uani 1 1 d . . . H2A H 0.2220 0.9721 0.5524 0.038 Uiso 1 1 calc R A . H2B H 0.1577 0.9031 0.5862 0.038 Uiso 1 1 calc R . . C3 C 0.1630(6) 1.0226(4) 0.6295(3) 0.0333(13) Uani 1 1 d . A . C4 C 0.1442(6) 1.0134(3) 0.6970(3) 0.0295(12) Uani 1 1 d . . . C5 C 0.0856(7) 1.0805(4) 0.7187(4) 0.0404(15) Uani 1 1 d . A . H5 H 0.0705 1.0743 0.7635 0.049 Uiso 1 1 calc R . . C6 C 0.0496(8) 1.1559(4) 0.6744(5) 0.056(2) Uani 1 1 d . . . H6 H 0.0118 1.2018 0.6900 0.067 Uiso 1 1 calc R A . C7 C 0.0679(8) 1.1651(4) 0.6088(5) 0.058(2) Uani 1 1 d . A . H7 H 0.0421 1.2169 0.5786 0.069 Uiso 1 1 calc R . . C8 C 0.1244(7) 1.0987(4) 0.5862(4) 0.0454(16) Uani 1 1 d . . . H8 H 0.1368 1.1055 0.5405 0.054 Uiso 1 1 calc R A . C9 C 0.5247(6) 1.0094(4) 0.6953(4) 0.0335(13) Uani 1 1 d . . . C10 C 0.5169(8) 1.0662(4) 0.7586(4) 0.0501(18) Uani 1 1 d . A . H10A H 0.5853 1.1130 0.7743 0.075 Uiso 1 1 calc R . . H10B H 0.5400 1.0325 0.8075 0.075 Uiso 1 1 calc R . . H10C H 0.4204 1.0895 0.7345 0.075 Uiso 1 1 calc R . . C11 C 0.4809(9) 1.0616(4) 0.6185(4) 0.0523(19) Uani 1 1 d . A . H11A H 0.5476 1.1089 0.6321 0.078 Uiso 1 1 calc R . . H11B H 0.3846 1.0841 0.5972 0.078 Uiso 1 1 calc R . . H11C H 0.4820 1.0255 0.5767 0.078 Uiso 1 1 calc R . . C12 C 0.6794(8) 0.9815(5) 0.7326(6) 0.070(3) Uani 1 1 d . A . H12A H 0.6902 0.9506 0.6912 0.105 Uiso 1 1 calc R . . H12B H 0.7061 0.9443 0.7799 0.105 Uiso 1 1 calc R . . H12C H 0.7413 1.0318 0.7507 0.105 Uiso 1 1 calc R . . C13 C 0.4257(8) 0.8294(4) 0.6130(4) 0.0393(15) Uani 1 1 d . . . C14 C 0.4115(12) 0.8645(5) 0.5341(5) 0.075(3) Uani 1 1 d . A . H14A H 0.4877 0.9058 0.5480 0.113 Uiso 1 1 calc R . . H14B H 0.3188 0.8925 0.5013 0.113 Uiso 1 1 calc R . . H14C H 0.4189 0.8177 0.5023 0.113 Uiso 1 1 calc R . . C15 C 0.5640(9) 0.7806(5) 0.6607(5) 0.063(2) Uani 1 1 d . A . H15A H 0.5650 0.7338 0.6268 0.094 Uiso 1 1 calc R . . H15B H 0.5724 0.7576 0.7111 0.094 Uiso 1 1 calc R . . H15C H 0.6442 0.8189 0.6752 0.094 Uiso 1 1 calc R . . C16 C 0.3057(9) 0.7647(4) 0.5901(5) 0.057(2) Uani 1 1 d . A . H16A H 0.3197 0.7152 0.5636 0.086 Uiso 1 1 calc R . . H16B H 0.2136 0.7912 0.5521 0.086 Uiso 1 1 calc R . . H16C H 0.3072 0.7466 0.6401 0.086 Uiso 1 1 calc R . . C17 C 0.1603(6) 0.9338(3) 0.8385(3) 0.0248(11) Uani 1 1 d . . . C18 C 0.2538(6) 0.9879(3) 0.9040(3) 0.0261(11) Uani 1 1 d . A . C19 C 0.2346(6) 0.9959(4) 0.9708(4) 0.0332(13) Uani 1 1 d . . . H19 H 0.2970 1.0315 1.0155 0.040 Uiso 1 1 calc R A . C20 C 0.1268(7) 0.9532(4) 0.9736(4) 0.0383(14) Uani 1 1 d . A . H20 H 0.1173 0.9588 1.0204 0.046 Uiso 1 1 calc R . . C21 C 0.0330(7) 0.9024(4) 0.9086(4) 0.0390(14) Uani 1 1 d . . . H21 H -0.0430 0.8745 0.9097 0.047 Uiso 1 1 calc R A . C22 C 0.0512(6) 0.8928(3) 0.8420(3) 0.0288(12) Uani 1 1 d . A . H22 H -0.0126 0.8572 0.7976 0.035 Uiso 1 1 calc R . . C23 C 0.3689(6) 1.0382(3) 0.9025(3) 0.0308(12) Uani 1 1 d . . . H23A H 0.3260 1.0847 0.8626 0.046 Uiso 1 1 calc R A . H23B H 0.4225 1.0010 0.8865 0.046 Uiso 1 1 calc R . . H23C H 0.4334 1.0618 0.9573 0.046 Uiso 1 1 calc R . . C24A C 0.0551(8) 0.8363(4) 0.6819(5) 0.0219(19) Uani 0.650(11) 1 d PGU A 1 C25A C -0.0868(9) 0.8547(4) 0.6252(6) 0.029(2) Uani 0.650(11) 1 d PGU A 1 C26A C -0.1776(7) 0.7907(5) 0.5749(5) 0.035(2) Uani 0.650(11) 1 d PGU A 1 H26A H -0.2745 0.8032 0.5362 0.042 Uiso 0.650(11) 1 calc PR A 1 C27A C -0.1264(8) 0.7083(4) 0.5812(5) 0.040(3) Uani 0.650(11) 1 d PGU A 1 H27A H -0.1884 0.6646 0.5468 0.048 Uiso 0.650(11) 1 calc PR A 1 C28A C 0.0155(9) 0.6900(3) 0.6379(5) 0.039(3) Uani 0.650(11) 1 d PGU A 1 H28A H 0.0505 0.6337 0.6422 0.046 Uiso 0.650(11) 1 calc PR A 1 C29A C 0.1063(7) 0.7540(4) 0.6882(4) 0.032(2) Uani 0.650(11) 1 d PGU A 1 H29A H 0.2033 0.7415 0.7269 0.038 Uiso 0.650(11) 1 calc PR A 1 C30A C -0.1521(10) 0.9427(6) 0.6163(6) 0.038(2) Uani 0.650(11) 1 d PU A 1 H30A H -0.1238 0.9651 0.6709 0.057 Uiso 0.650(11) 1 calc PR A 1 H30B H -0.2561 0.9384 0.5831 0.057 Uiso 0.650(11) 1 calc PR A 1 H30C H -0.1182 0.9810 0.5892 0.057 Uiso 0.650(11) 1 calc PR A 1 C24B C 0.0385(13) 0.8404(6) 0.6908(10) 0.0219(19) Uani 0.350(11) 1 d PGU A 2 C25B C 0.0556(10) 0.7526(6) 0.6926(7) 0.026(4) Uani 0.350(11) 1 d PGU A 2 C26B C -0.0540(13) 0.7018(7) 0.6343(7) 0.032(4) Uani 0.350(11) 1 d PGU A 2 H26B H -0.0423 0.6418 0.6356 0.038 Uiso 0.350(11) 1 calc PR A 2 C27B C -0.1808(13) 0.7388(9) 0.5743(7) 0.038(5) Uani 0.350(11) 1 d PGU A 2 H27B H -0.2557 0.7041 0.5345 0.045 Uiso 0.350(11) 1 calc PR A 2 C28B C -0.1979(13) 0.8266(10) 0.5725(10) 0.042(5) Uani 0.350(11) 1 d PGU A 2 H28B H -0.2845 0.8518 0.5314 0.050 Uiso 0.350(11) 1 calc PR A 2 C29B C -0.0883(16) 0.8774(7) 0.6307(12) 0.025(4) Uani 0.350(11) 1 d PGU A 2 H29B H -0.1000 0.9374 0.6295 0.030 Uiso 0.350(11) 1 calc PR A 2 C30B C 0.1848(12) 0.7097(9) 0.7681(9) 0.046(5) Uani 0.350(11) 1 d PGU A 2 H30D H 0.2713 0.7199 0.7661 0.070 Uiso 0.350(11) 1 calc PR A 2 H30E H 0.1680 0.6483 0.7667 0.070 Uiso 0.350(11) 1 calc PR A 2 H30F H 0.1967 0.7337 0.8189 0.070 Uiso 0.350(11) 1 calc PR A 2 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 0.03037(11) 0.01866(9) 0.02157(10) 0.00103(8) 0.00924(8) 0.00292(9) P1 0.0340(7) 0.0201(6) 0.0213(6) 0.0014(5) 0.0136(6) -0.0003(5) P2 0.0250(6) 0.0137(6) 0.0211(6) 0.0008(5) 0.0088(5) 0.0008(5) Cl1A 0.0324(12) 0.0514(14) 0.0439(13) 0.0080(10) 0.0204(10) 0.0144(10) C1A 0.070(2) 0.0383(15) 0.0498(18) 0.0222(13) 0.0469(17) 0.0270(14) Cl1B 0.070(2) 0.0383(15) 0.0498(18) 0.0222(13) 0.0469(17) 0.0270(14) C1B 0.0324(12) 0.0514(14) 0.0439(13) 0.0080(10) 0.0204(10) 0.0144(10) C2 0.032(3) 0.038(3) 0.019(2) 0.007(2) 0.008(2) -0.003(2) C3 0.031(3) 0.028(3) 0.027(3) 0.007(2) 0.005(2) -0.003(2) C4 0.033(3) 0.015(2) 0.028(3) 0.001(2) 0.007(2) 0.001(2) C5 0.049(4) 0.025(3) 0.032(3) -0.001(2) 0.010(3) 0.010(3) C6 0.067(5) 0.021(3) 0.046(4) 0.001(3) 0.006(4) 0.015(3) C7 0.054(4) 0.026(3) 0.058(5) 0.014(3) 0.004(4) 0.003(3) C8 0.039(3) 0.042(3) 0.035(3) 0.019(3) 0.005(3) 0.003(3) C9 0.035(3) 0.026(3) 0.039(3) 0.002(2) 0.019(3) -0.001(2) C10 0.068(5) 0.038(3) 0.052(4) -0.015(3) 0.036(4) -0.023(3) C11 0.072(5) 0.040(4) 0.048(4) 0.006(3) 0.034(4) -0.016(3) C12 0.037(4) 0.044(4) 0.109(7) 0.012(4) 0.023(4) -0.003(3) C13 0.067(4) 0.028(3) 0.031(3) -0.002(2) 0.031(3) 0.003(3) C14 0.158(10) 0.046(4) 0.052(4) -0.003(4) 0.076(6) 0.007(5) C15 0.084(6) 0.058(5) 0.064(5) -0.002(4) 0.050(5) 0.017(4) C16 0.085(6) 0.028(3) 0.058(4) -0.011(3) 0.035(4) -0.007(3) C17 0.028(3) 0.019(2) 0.028(3) -0.001(2) 0.014(2) 0.005(2) C18 0.028(3) 0.018(2) 0.028(3) -0.002(2) 0.011(2) 0.007(2) C19 0.036(3) 0.029(3) 0.030(3) -0.004(2) 0.014(3) 0.011(2) C20 0.042(3) 0.039(3) 0.043(3) 0.003(3) 0.028(3) 0.017(3) C21 0.034(3) 0.037(3) 0.055(4) 0.002(3) 0.030(3) 0.007(3) C22 0.028(3) 0.026(3) 0.034(3) -0.001(2) 0.016(2) 0.007(2) C23 0.034(3) 0.023(3) 0.029(3) -0.005(2) 0.011(2) -0.002(2) C24A 0.028(3) 0.023(2) 0.019(3) -0.003(2) 0.016(2) -0.008(2) C25A 0.041(5) 0.027(4) 0.021(5) -0.001(4) 0.017(4) -0.002(4) C26A 0.041(5) 0.036(6) 0.022(4) 0.005(5) 0.012(4) -0.012(4) C27A 0.053(6) 0.025(5) 0.027(5) 0.003(4) 0.009(5) -0.016(4) C28A 0.052(6) 0.021(4) 0.041(5) -0.001(3) 0.023(5) -0.012(4) C29A 0.035(5) 0.027(4) 0.035(5) -0.002(3) 0.018(4) -0.008(4) C30A 0.036(5) 0.041(5) 0.034(5) 0.003(4) 0.016(4) 0.000(4) C24B 0.028(3) 0.023(2) 0.019(3) -0.003(2) 0.016(2) -0.008(2) C25B 0.015(7) 0.024(6) 0.044(8) -0.007(6) 0.018(6) -0.007(5) C26B 0.036(9) 0.028(7) 0.042(8) -0.013(6) 0.027(7) -0.021(6) C27B 0.046(9) 0.043(10) 0.015(7) -0.005(8) 0.009(6) -0.022(8) C28B 0.036(8) 0.047(10) 0.030(8) 0.012(9) 0.008(6) -0.018(7) C29B 0.018(7) 0.034(8) 0.026(8) -0.004(7) 0.013(6) -0.003(5) C30B 0.021(8) 0.032(8) 0.077(12) 0.008(8) 0.019(7) 0.003(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 P2 2.2692(13) . ? Pt1 C1A 2.283(3) . ? Pt1 P1 2.2932(14) . ? Pt1 Cl1A 2.313(2) . ? P1 C2 1.850(6) . ? P1 C9 1.891(6) . ? P1 C13 1.904(6) . ? P2 C17 1.832(5) . ? P2 C4 1.832(5) . ? P2 C24A 1.852(6) . ? P2 C24B 1.861(10) . ? C1A H1A1 0.9800 . ? C1A H1A2 0.9800 . ? C1A H1A3 0.9800 . ? C2 C3 1.502(9) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C8 1.387(8) . ? C3 C4 1.402(8) . ? C4 C5 1.400(8) . ? C5 C6 1.387(9) . ? C5 H5 0.9500 . ? C6 C7 1.365(11) . ? C6 H6 0.9500 . ? C7 C8 1.387(11) . ? C7 H7 0.9500 . ? C8 H8 0.9500 . ? C9 C11 1.515(9) . ? C9 C12 1.526(9) . ? C9 C10 1.532(9) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C15 1.513(10) . ? C13 C14 1.523(9) . ? C13 C16 1.537(10) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? 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 C22 1.390(8) . ? C17 C18 1.415(7) . ? C18 C19 1.391(8) . ? C18 C23 1.500(8) . ? C19 C20 1.381(9) . ? C19 H19 0.9500 . ? C20 C21 1.380(9) . ? C20 H20 0.9500 . ? C21 C22 1.383(8) . ? C21 H21 0.9500 . ? C22 H22 0.9500 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24A C25A 1.3900 . ? C24A C29A 1.3900 . ? C25A C26A 1.3900 . ? C25A C30A 1.525(11) . ? C26A C27A 1.3900 . ? C26A H26A 0.9500 . ? C27A C28A 1.3900 . ? C27A H27A 0.9500 . ? C28A C29A 1.3900 . ? C28A H28A 0.9500 . ? C29A H29A 0.9500 . ? C30A H30A 0.9800 . ? C30A H30B 0.9800 . ? C30A H30C 0.9800 . ? C24B C25B 1.3900 . ? C24B C29B 1.3900 . ? C25B C26B 1.3900 . ? C25B C30B 1.5556 . ? C26B C27B 1.3900 . ? C26B H26B 0.9500 . ? C27B C28B 1.3900 . ? C27B H27B 0.9500 . ? C28B C29B 1.3900 . ? C28B H28B 0.9500 . ? C29B H29B 0.9500 . ? C30B H30D 0.9800 . ? C30B H30E 0.9800 . ? C30B H30F 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P2 Pt1 C1A 92.34(8) . . ? P2 Pt1 P1 93.63(5) . . ? C1A Pt1 P1 173.91(8) . . ? P2 Pt1 Cl1A 169.06(7) . . ? C1A Pt1 Cl1A 77.68(10) . . ? P1 Pt1 Cl1A 96.46(7) . . ? C2 P1 C9 105.1(3) . . ? C2 P1 C13 99.8(3) . . ? C9 P1 C13 111.8(3) . . ? C2 P1 Pt1 109.90(19) . . ? C9 P1 Pt1 114.03(19) . . ? C13 P1 Pt1 114.76(19) . . ? C17 P2 C4 103.6(3) . . ? C17 P2 C24A 108.6(4) . . ? C4 P2 C24A 104.5(3) . . ? C17 P2 C24B 99.3(7) . . ? C4 P2 C24B 105.2(4) . . ? C24A P2 C24B 9.7(9) . . ? C17 P2 Pt1 114.65(17) . . ? C4 P2 Pt1 113.9(2) . . ? C24A P2 Pt1 110.8(3) . . ? C24B P2 Pt1 118.2(4) . . ? Pt1 C1A H1A1 109.5 . . ? Pt1 C1A H1A2 109.5 . . ? H1A1 C1A H1A2 109.5 . . ? Pt1 C1A H1A3 109.5 . . ? H1A1 C1A H1A3 109.5 . . ? H1A2 C1A H1A3 109.5 . . ? C3 C2 P1 117.4(4) . . ? C3 C2 H2A 108.0 . . ? P1 C2 H2A 108.0 . . ? C3 C2 H2B 108.0 . . ? P1 C2 H2B 108.0 . . ? H2A C2 H2B 107.2 . . ? C8 C3 C4 119.0(6) . . ? C8 C3 C2 118.9(6) . . ? C4 C3 C2 122.1(5) . . ? C5 C4 C3 119.6(5) . . ? C5 C4 P2 120.7(5) . . ? C3 C4 P2 119.7(4) . . ? C6 C5 C4 119.8(7) . . ? C6 C5 H5 120.1 . . ? C4 C5 H5 120.1 . . ? C7 C6 C5 120.8(7) . . ? C7 C6 H6 119.6 . . ? C5 C6 H6 119.6 . . ? C6 C7 C8 119.9(6) . . ? C6 C7 H7 120.1 . . ? C8 C7 H7 120.1 . . ? C3 C8 C7 121.0(7) . . ? C3 C8 H8 119.5 . . ? C7 C8 H8 119.5 . . ? C11 C9 C12 109.1(6) . . ? C11 C9 C10 108.6(5) . . ? C12 C9 C10 107.5(6) . . ? C11 C9 P1 113.8(4) . . ? C12 C9 P1 111.0(4) . . ? C10 C9 P1 106.6(4) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C11 H11A 109.5 . . ? C9 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C9 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C9 C12 H12A 109.5 . . ? C9 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C9 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C15 C13 C14 109.6(7) . . ? C15 C13 C16 106.3(6) . . ? C14 C13 C16 108.8(6) . . ? C15 C13 P1 112.8(5) . . ? C14 C13 P1 112.7(4) . . ? C16 C13 P1 106.3(5) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C13 C16 H16A 109.5 . . ? C13 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C13 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C22 C17 C18 119.2(5) . . ? C22 C17 P2 120.6(4) . . ? C18 C17 P2 120.0(4) . . ? C19 C18 C17 118.2(5) . . ? C19 C18 C23 119.4(5) . . ? C17 C18 C23 122.4(5) . . ? C20 C19 C18 121.5(6) . . ? C20 C19 H19 119.2 . . ? C18 C19 H19 119.2 . . ? C21 C20 C19 120.3(6) . . ? C21 C20 H20 119.8 . . ? C19 C20 H20 119.8 . . ? C20 C21 C22 119.1(6) . . ? C20 C21 H21 120.5 . . ? C22 C21 H21 120.5 . . ? C21 C22 C17 121.6(5) . . ? C21 C22 H22 119.2 . . ? C17 C22 H22 119.2 . . ? C18 C23 H23A 109.5 . . ? C18 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C18 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C25A C24A C29A 120.0 . . ? C25A C24A P2 126.2(4) . . ? C29A C24A P2 113.8(4) . . ? C26A C25A C24A 120.0 . . ? C26A C25A C30A 116.8(6) . . ? C24A C25A C30A 123.2(6) . . ? C25A C26A C27A 120.0 . . ? C25A C26A H26A 120.0 . . ? C27A C26A H26A 120.0 . . ? C28A C27A C26A 120.0 . . ? C28A C27A H27A 120.0 . . ? C26A C27A H27A 120.0 . . ? C27A C28A C29A 120.0 . . ? C27A C28A H28A 120.0 . . ? C29A C28A H28A 120.0 . . ? C28A C29A C24A 120.0 . . ? C28A C29A H29A 120.0 . . ? C24A C29A H29A 120.0 . . ? C25B C24B C29B 120.0 . . ? C25B C24B P2 121.7(6) . . ? C29B C24B P2 117.3(6) . . ? C26B C25B C24B 120.0 . . ? C26B C25B C30B 119.1 . . ? C24B C25B C30B 120.0 . . ? C25B C26B C27B 120.0 . . ? C25B C26B H26B 120.0 . . ? C27B C26B H26B 120.0 . . ? C26B C27B C28B 120.0 . . ? C26B C27B H27B 120.0 . . ? C28B C27B H27B 120.0 . . ? C29B C28B C27B 120.0 . . ? C29B C28B H28B 120.0 . . ? C27B C28B H28B 120.0 . . ? C28B C29B C24B 120.0 . . ? C28B C29B H29B 120.0 . . ? C24B C29B H29B 120.0 . . ? C25B C30B H30D 109.5 . . ? C25B C30B H30E 109.5 . . ? H30D C30B H30E 109.5 . . ? C25B C30B H30F 109.5 . . ? H30D C30B H30F 109.5 . . ? H30E C30B H30F 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag P2 Pt1 P1 C2 -8.2(2) . . . . ? C1A Pt1 P1 C2 160.2(9) . . . . ? Cl1A Pt1 P1 C2 176.0(2) . . . . ? P2 Pt1 P1 C9 109.6(2) . . . . ? C1A Pt1 P1 C9 -82.1(9) . . . . ? Cl1A Pt1 P1 C9 -66.2(2) . . . . ? P2 Pt1 P1 C13 -119.7(3) . . . . ? C1A Pt1 P1 C13 48.7(9) . . . . ? Cl1A Pt1 P1 C13 64.5(3) . . . . ? C1A Pt1 P2 C17 26.5(2) . . . . ? P1 Pt1 P2 C17 -154.78(19) . . . . ? Cl1A Pt1 P2 C17 2.5(4) . . . . ? C1A Pt1 P2 C4 145.6(2) . . . . ? P1 Pt1 P2 C4 -35.7(2) . . . . ? Cl1A Pt1 P2 C4 121.6(4) . . . . ? C1A Pt1 P2 C24A -97.0(3) . . . . ? P1 Pt1 P2 C24A 81.8(3) . . . . ? Cl1A Pt1 P2 C24A -120.9(5) . . . . ? C1A Pt1 P2 C24B -90.2(7) . . . . ? P1 Pt1 P2 C24B 88.6(7) . . . . ? Cl1A Pt1 P2 C24B -114.2(8) . . . . ? C9 P1 C2 C3 -64.2(5) . . . . ? C13 P1 C2 C3 180.0(4) . . . . ? Pt1 P1 C2 C3 59.0(5) . . . . ? P1 C2 C3 C8 119.8(5) . . . . ? P1 C2 C3 C4 -60.5(7) . . . . ? C8 C3 C4 C5 0.7(8) . . . . ? C2 C3 C4 C5 -178.9(5) . . . . ? C8 C3 C4 P2 178.9(4) . . . . ? C2 C3 C4 P2 -0.8(7) . . . . ? C17 P2 C4 C5 -5.6(5) . . . . ? C24A P2 C4 C5 108.1(6) . . . . ? C24B P2 C4 C5 98.1(8) . . . . ? Pt1 P2 C4 C5 -130.8(5) . . . . ? C17 P2 C4 C3 176.3(4) . . . . ? C24A P2 C4 C3 -70.0(6) . . . . ? C24B P2 C4 C3 -80.0(8) . . . . ? Pt1 P2 C4 C3 51.1(5) . . . . ? C3 C4 C5 C6 -1.4(9) . . . . ? P2 C4 C5 C6 -179.5(5) . . . . ? C4 C5 C6 C7 1.3(11) . . . . ? C5 C6 C7 C8 -0.6(11) . . . . ? C4 C3 C8 C7 0.0(9) . . . . ? C2 C3 C8 C7 179.7(6) . . . . ? C6 C7 C8 C3 -0.1(11) . . . . ? C2 P1 C9 C11 -37.9(6) . . . . ? C13 P1 C9 C11 69.5(6) . . . . ? Pt1 P1 C9 C11 -158.3(4) . . . . ? C2 P1 C9 C12 -161.5(5) . . . . ? C13 P1 C9 C12 -54.1(6) . . . . ? Pt1 P1 C9 C12 78.1(6) . . . . ? C2 P1 C9 C10 81.8(5) . . . . ? C13 P1 C9 C10 -170.9(4) . . . . ? Pt1 P1 C9 C10 -38.7(5) . . . . ? C2 P1 C13 C15 -175.6(5) . . . . ? C9 P1 C13 C15 73.7(6) . . . . ? Pt1 P1 C13 C15 -58.2(6) . . . . ? C2 P1 C13 C14 59.7(6) . . . . ? C9 P1 C13 C14 -51.1(7) . . . . ? Pt1 P1 C13 C14 177.1(5) . . . . ? C2 P1 C13 C16 -59.4(5) . . . . ? C9 P1 C13 C16 -170.2(4) . . . . ? Pt1 P1 C13 C16 58.0(5) . . . . ? C4 P2 C17 C22 112.5(4) . . . . ? C24A P2 C17 C22 1.8(5) . . . . ? C24B P2 C17 C22 4.3(6) . . . . ? Pt1 P2 C17 C22 -122.7(4) . . . . ? C4 P2 C17 C18 -71.8(4) . . . . ? C24A P2 C17 C18 177.5(4) . . . . ? C24B P2 C17 C18 180.0(5) . . . . ? Pt1 P2 C17 C18 52.9(4) . . . . ? C22 C17 C18 C19 1.7(7) . . . . ? P2 C17 C18 C19 -174.0(4) . . . . ? C22 C17 C18 C23 -176.5(5) . . . . ? P2 C17 C18 C23 7.8(7) . . . . ? C17 C18 C19 C20 -0.6(8) . . . . ? C23 C18 C19 C20 177.7(5) . . . . ? C18 C19 C20 C21 -1.3(9) . . . . ? C19 C20 C21 C22 2.0(9) . . . . ? C20 C21 C22 C17 -0.9(9) . . . . ? C18 C17 C22 C21 -1.0(8) . . . . ? P2 C17 C22 C21 174.7(4) . . . . ? C17 P2 C24A C25A 75.8(5) . . . . ? C4 P2 C24A C25A -34.3(6) . . . . ? C24B P2 C24A C25A 61(3) . . . . ? Pt1 P2 C24A C25A -157.4(4) . . . . ? C17 P2 C24A C29A -104.2(5) . . . . ? C4 P2 C24A C29A 145.8(5) . . . . ? C24B P2 C24A C29A -119(4) . . . . ? Pt1 P2 C24A C29A 22.7(6) . . . . ? C29A C24A C25A C26A 0.0 . . . . ? P2 C24A C25A C26A -179.9(7) . . . . ? C29A C24A C25A C30A 178.1(11) . . . . ? P2 C24A C25A C30A -1.8(9) . . . . ? C24A C25A C26A C27A 0.0 . . . . ? C30A C25A C26A C27A -178.3(10) . . . . ? C25A C26A C27A C28A 0.0 . . . . ? C26A C27A C28A C29A 0.0 . . . . ? C27A C28A C29A C24A 0.0 . . . . ? C25A C24A C29A C28A 0.0 . . . . ? P2 C24A C29A C28A 179.9(6) . . . . ? C17 P2 C24B C25B -100.8(11) . . . . ? C4 P2 C24B C25B 152.3(10) . . . . ? C24A P2 C24B C25B 65(3) . . . . ? Pt1 P2 C24B C25B 23.8(14) . . . . ? C17 P2 C24B C29B 90.6(5) . . . . ? C4 P2 C24B C29B -16.3(6) . . . . ? C24A P2 C24B C29B -104(4) . . . . ? Pt1 P2 C24B C29B -144.8(5) . . . . ? C29B C24B C25B C26B 0.0 . . . . ? P2 C24B C25B C26B -168.3(13) . . . . ? C29B C24B C25B C30B -169.0 . . . . ? P2 C24B C25B C30B 22.7(13) . . . . ? C24B C25B C26B C27B 0.0 . . . . ? C30B C25B C26B C27B 169.1 . . . . ? C25B C26B C27B C28B 0.0 . . . . ? C26B C27B C28B C29B 0.0 . . . . ? C27B C28B C29B C24B 0.0 . . . . ? C25B C24B C29B C28B 0.0 . . . . ? P2 C24B C29B C28B 168.8(13) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.58 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.600 _refine_diff_density_min -2.065 _refine_diff_density_rms 0.130 data_4a _database_code_depnum_ccdc_archive 'CCDC 897395' #TrackingRef '- all.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H45 Cl P2 Pt' _chemical_formula_sum 'C48 H90 Cl2 P4 Pt2' _chemical_formula_weight 1252.16 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 15.9715(7) _cell_length_b 20.0553(8) _cell_length_c 18.7186(8) _cell_angle_alpha 90.00 _cell_angle_beta 118.759(3) _cell_angle_gamma 90.00 _cell_volume 5256.2(4) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 4496 _cell_measurement_theta_min 2.46 _cell_measurement_theta_max 25.36 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.582 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2512 _exptl_absorpt_coefficient_mu 5.571 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5930 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_process_details 'SADABS V2008/1' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 54476 _diffrn_reflns_av_R_equivalents 0.0814 _diffrn_reflns_av_sigmaI/netI 0.0683 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.45 _diffrn_reflns_theta_max 27.52 _reflns_number_total 12047 _reflns_number_gt 8095 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Apex II (Bruker-AXS, 2007)' _computing_cell_refinement 'Apex II (Bruker-AXS, 2007)' _computing_data_reduction ; SAINT v7.34A (Bruker-AXS, 2007) & XPREP v2005/4 (Bruker-AXS, 2005) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0352P)^2^+0.9343P] 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 12047 _refine_ls_number_parameters 531 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0775 _refine_ls_R_factor_gt 0.0405 _refine_ls_wR_factor_ref 0.0954 _refine_ls_wR_factor_gt 0.0830 _refine_ls_goodness_of_fit_ref 1.016 _refine_ls_restrained_S_all 1.016 _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 0.624498(16) 0.741757(11) 0.427387(14) 0.01902(7) Uani 1 1 d . . . P1 P 0.59960(12) 0.78193(7) 0.30761(10) 0.0194(3) Uani 1 1 d . . . P2 P 0.67197(11) 0.63175(7) 0.41245(10) 0.0162(3) Uani 1 1 d . . . Cl1 Cl 0.68254(11) 0.72954(8) 0.57123(9) 0.0258(3) Uani 1 1 d . . . C1 C 0.5658(5) 0.8291(3) 0.4499(4) 0.0285(16) Uani 1 1 d . . . H1A H 0.6175 0.8595 0.4848 0.043 Uiso 1 1 calc R . . H1B H 0.5289 0.8170 0.4773 0.043 Uiso 1 1 calc R . . H1C H 0.5239 0.8513 0.3981 0.043 Uiso 1 1 calc R . . C2 C 0.6688(4) 0.7335(3) 0.2713(4) 0.0184(12) Uani 1 1 d . . . H2A H 0.6604 0.7548 0.2206 0.022 Uiso 1 1 calc R . . H2B H 0.7371 0.7382 0.3122 0.022 Uiso 1 1 calc R . . C3 C 0.6491(4) 0.6594(3) 0.2538(4) 0.0196(14) Uani 1 1 d . . . C4 C 0.6543(4) 0.6111(3) 0.3103(4) 0.0174(13) Uani 1 1 d . . . C5 C 0.6425(5) 0.5443(3) 0.2843(4) 0.0237(14) Uani 1 1 d . . . H5 H 0.6484 0.5103 0.3219 0.028 Uiso 1 1 calc R . . C6 C 0.6226(5) 0.5258(3) 0.2068(4) 0.0280(16) Uani 1 1 d . . . H6 H 0.6144 0.4800 0.1919 0.034 Uiso 1 1 calc R . . C7 C 0.6144(5) 0.5734(3) 0.1507(4) 0.0292(16) Uani 1 1 d . . . H7 H 0.5988 0.5614 0.0966 0.035 Uiso 1 1 calc R . . C8 C 0.6299(5) 0.6399(3) 0.1758(4) 0.0265(16) Uani 1 1 d . . . H8 H 0.6273 0.6731 0.1385 0.032 Uiso 1 1 calc R . . C9 C 0.4734(5) 0.7826(3) 0.2216(4) 0.0249(14) Uani 1 1 d . . . C10 C 0.4643(5) 0.8108(3) 0.1419(4) 0.0339(17) Uani 1 1 d . . . H10A H 0.5089 0.7875 0.1284 0.051 Uiso 1 1 calc R . . H10B H 0.4795 0.8586 0.1485 0.051 Uiso 1 1 calc R . . H10C H 0.3988 0.8044 0.0978 0.051 Uiso 1 1 calc R . . C11 C 0.4057(5) 0.8205(3) 0.2450(4) 0.0363(18) Uani 1 1 d . . . H11A H 0.4219 0.8681 0.2514 0.055 Uiso 1 1 calc R . . H11B H 0.4129 0.8028 0.2964 0.055 Uiso 1 1 calc R . . H11C H 0.3395 0.8147 0.2020 0.055 Uiso 1 1 calc R . . C12 C 0.4389(5) 0.7102(3) 0.2066(4) 0.0311(17) Uani 1 1 d . . . H12A H 0.3698 0.7092 0.1698 0.047 Uiso 1 1 calc R . . H12B H 0.4531 0.6893 0.2586 0.047 Uiso 1 1 calc R . . H12C H 0.4717 0.6858 0.1819 0.047 Uiso 1 1 calc R . . C13 C 0.6597(5) 0.8658(3) 0.3165(4) 0.0265(15) Uani 1 1 d . . . C14 C 0.7510(5) 0.8663(3) 0.3998(4) 0.0319(17) Uani 1 1 d . . . H14A H 0.7955 0.8325 0.4001 0.048 Uiso 1 1 calc R . . H14B H 0.7347 0.8564 0.4428 0.048 Uiso 1 1 calc R . . H14C H 0.7811 0.9103 0.4093 0.048 Uiso 1 1 calc R . . C15 C 0.6910(6) 0.8778(3) 0.2520(4) 0.0357(18) Uani 1 1 d . . . H15A H 0.7125 0.9241 0.2554 0.054 Uiso 1 1 calc R . . H15B H 0.6370 0.8696 0.1977 0.054 Uiso 1 1 calc R . . H15C H 0.7435 0.8475 0.2615 0.054 Uiso 1 1 calc R . . C16 C 0.5971(5) 0.9260(3) 0.3139(5) 0.0361(18) Uani 1 1 d . . . H16A H 0.6342 0.9672 0.3248 0.054 Uiso 1 1 calc R . . H16B H 0.5770 0.9201 0.3554 0.054 Uiso 1 1 calc R . . H16C H 0.5406 0.9287 0.2599 0.054 Uiso 1 1 calc R . . C17 C 0.5964(4) 0.5667(3) 0.4320(4) 0.0214(14) Uani 1 1 d . . . C18 C 0.4968(4) 0.5668(3) 0.3566(4) 0.0239(14) Uani 1 1 d . . . H18A H 0.4544 0.5371 0.3661 0.036 Uiso 1 1 calc R . . H18B H 0.5016 0.5511 0.3091 0.036 Uiso 1 1 calc R . . H18C H 0.4707 0.6121 0.3465 0.036 Uiso 1 1 calc R . . C19 C 0.5829(5) 0.5891(3) 0.5043(4) 0.0291(16) Uani 1 1 d . . . H19A H 0.5516 0.6328 0.4923 0.044 Uiso 1 1 calc R . . H19B H 0.6453 0.5922 0.5533 0.044 Uiso 1 1 calc R . . H19C H 0.5430 0.5566 0.5132 0.044 Uiso 1 1 calc R . . C20 C 0.6355(5) 0.4942(3) 0.4517(4) 0.0257(15) Uani 1 1 d . . . H20A H 0.5895 0.4658 0.4579 0.039 Uiso 1 1 calc R . . H20B H 0.6964 0.4939 0.5025 0.039 Uiso 1 1 calc R . . H20C H 0.6453 0.4772 0.4072 0.039 Uiso 1 1 calc R . . C21 C 0.8041(4) 0.6140(3) 0.4806(4) 0.0196(13) Uani 1 1 d . . . C22 C 0.8278(5) 0.6022(3) 0.5694(4) 0.0234(14) Uani 1 1 d . . . H22A H 0.8972 0.5986 0.6038 0.035 Uiso 1 1 calc R . . H22B H 0.7974 0.5608 0.5731 0.035 Uiso 1 1 calc R . . H22C H 0.8039 0.6396 0.5882 0.035 Uiso 1 1 calc R . . C23 C 0.8409(5) 0.5541(3) 0.4528(4) 0.0293(16) Uani 1 1 d . . . H23A H 0.8304 0.5621 0.3974 0.044 Uiso 1 1 calc R . . H23B H 0.8066 0.5138 0.4534 0.044 Uiso 1 1 calc R . . H23C H 0.9094 0.5483 0.4899 0.044 Uiso 1 1 calc R . . C24 C 0.8572(4) 0.6764(3) 0.4766(4) 0.0247(14) Uani 1 1 d . . . H24A H 0.9259 0.6707 0.5128 0.037 Uiso 1 1 calc R . . H24B H 0.8345 0.7153 0.4940 0.037 Uiso 1 1 calc R . . H24C H 0.8451 0.6830 0.4206 0.037 Uiso 1 1 calc R . . Pt2 Pt 0.131882(16) 0.747886(10) 0.418507(13) 0.01647(7) Uani 1 1 d . . . P3 P 0.12386(11) 0.71102(7) 0.30305(10) 0.0162(3) Uani 1 1 d . . . P4 P 0.14682(12) 0.86401(7) 0.39779(10) 0.0169(3) Uani 1 1 d . . . Cl2 Cl 0.17856(11) 0.76221(7) 0.55982(9) 0.0213(3) Uani 1 1 d . . . C25 C 0.1005(5) 0.6506(3) 0.4449(4) 0.0220(14) Uani 1 1 d . . . H25A H 0.0768 0.6228 0.3960 0.033 Uiso 1 1 calc R . . H25B H 0.0516 0.6537 0.4622 0.033 Uiso 1 1 calc R . . H25C H 0.1585 0.6307 0.4887 0.033 Uiso 1 1 calc R . . C26 C 0.1800(4) 0.7715(3) 0.2661(4) 0.0151(12) Uani 1 1 d . . . H26A H 0.2482 0.7739 0.3077 0.018 Uiso 1 1 calc R . . H26B H 0.1776 0.7521 0.2165 0.018 Uiso 1 1 calc R . . C27 C 0.1447(4) 0.8429(3) 0.2453(4) 0.0161(13) Uani 1 1 d . . . C28 C 0.1335(4) 0.8875(3) 0.2973(4) 0.0167(13) Uani 1 1 d . . . C29 C 0.1098(5) 0.9537(3) 0.2699(4) 0.0250(15) Uani 1 1 d . . . H29 H 0.1034 0.9852 0.3049 0.030 Uiso 1 1 calc R . . C30 C 0.0953(5) 0.9749(3) 0.1948(4) 0.0242(15) Uani 1 1 d . . . H30 H 0.0807 1.0203 0.1792 0.029 Uiso 1 1 calc R . . C31 C 0.1023(4) 0.9295(3) 0.1421(4) 0.0213(14) Uani 1 1 d . . . H31 H 0.0895 0.9424 0.0889 0.026 Uiso 1 1 calc R . . C32 C 0.1285(4) 0.8646(3) 0.1695(4) 0.0186(13) Uani 1 1 d . . . H32 H 0.1357 0.8335 0.1345 0.022 Uiso 1 1 calc R . . C33 C 0.0024(4) 0.6943(3) 0.2154(4) 0.0219(14) Uani 1 1 d . . . C34 C 0.0040(5) 0.6703(3) 0.1389(4) 0.0323(17) Uani 1 1 d . . . H34A H -0.0616 0.6666 0.0942 0.048 Uiso 1 1 calc R . . H34B H 0.0351 0.6265 0.1493 0.048 Uiso 1 1 calc R . . H34C H 0.0395 0.7022 0.1241 0.048 Uiso 1 1 calc R . . C35 C -0.0541(5) 0.6442(3) 0.2381(4) 0.0299(16) Uani 1 1 d . . . H35A H -0.0591 0.6611 0.2850 0.045 Uiso 1 1 calc R . . H35B H -0.0208 0.6012 0.2519 0.045 Uiso 1 1 calc R . . H35C H -0.1182 0.6385 0.1916 0.045 Uiso 1 1 calc R . . C36 C -0.0522(5) 0.7601(3) 0.1952(4) 0.0347(17) Uani 1 1 d . . . H36A H -0.0221 0.7920 0.1750 0.052 Uiso 1 1 calc R . . H36B H -0.0511 0.7779 0.2444 0.052 Uiso 1 1 calc R . . H36C H -0.1185 0.7525 0.1533 0.052 Uiso 1 1 calc R . . C37 C 0.2085(5) 0.6380(3) 0.3193(4) 0.0216(14) Uani 1 1 d . . . C38 C 0.2955(5) 0.6476(3) 0.4025(4) 0.0281(16) Uani 1 1 d . . . H38A H 0.2769 0.6424 0.4450 0.042 Uiso 1 1 calc R . . H38B H 0.3217 0.6924 0.4058 0.042 Uiso 1 1 calc R . . H38C H 0.3440 0.6143 0.4103 0.042 Uiso 1 1 calc R . . C39 C 0.2442(5) 0.6365(3) 0.2557(4) 0.0293(16) Uani 1 1 d . . . H39A H 0.2839 0.6758 0.2629 0.044 Uiso 1 1 calc R . . H39B H 0.1893 0.6367 0.2007 0.044 Uiso 1 1 calc R . . H39C H 0.2820 0.5961 0.2634 0.044 Uiso 1 1 calc R . . C40 C 0.1653(5) 0.5698(3) 0.3174(4) 0.0310(17) Uani 1 1 d . . . H40A H 0.2132 0.5351 0.3286 0.047 Uiso 1 1 calc R . . H40B H 0.1102 0.5624 0.2635 0.047 Uiso 1 1 calc R . . H40C H 0.1446 0.5682 0.3589 0.047 Uiso 1 1 calc R . . C41 C 0.0465(5) 0.9129(3) 0.4035(4) 0.0237(14) Uani 1 1 d . . . C42 C -0.0467(4) 0.9051(3) 0.3219(4) 0.0296(16) Uani 1 1 d . . . H42A H -0.0615 0.8576 0.3102 0.044 Uiso 1 1 calc R . . H42B H -0.0387 0.9256 0.2781 0.044 Uiso 1 1 calc R . . H42C H -0.0992 0.9271 0.3258 0.044 Uiso 1 1 calc R . . C43 C 0.0292(5) 0.8813(3) 0.4707(4) 0.0298(16) Uani 1 1 d . . . H43A H -0.0240 0.9042 0.4725 0.045 Uiso 1 1 calc R . . H43B H 0.0870 0.8858 0.5236 0.045 Uiso 1 1 calc R . . H43C H 0.0135 0.8340 0.4586 0.045 Uiso 1 1 calc R . . C44 C 0.0632(5) 0.9879(3) 0.4243(4) 0.0302(16) Uani 1 1 d . . . H44A H 0.0125 1.0051 0.4345 0.045 Uiso 1 1 calc R . . H44B H 0.0625 1.0121 0.3785 0.045 Uiso 1 1 calc R . . H44C H 0.1252 0.9941 0.4731 0.045 Uiso 1 1 calc R . . C45 C 0.2688(5) 0.9004(3) 0.4716(4) 0.0252(15) Uani 1 1 d . . . C46 C 0.2815(5) 0.9099(3) 0.5568(4) 0.0296(16) Uani 1 1 d . . . H46A H 0.2665 0.8681 0.5754 0.044 Uiso 1 1 calc R . . H46B H 0.2385 0.9451 0.5560 0.044 Uiso 1 1 calc R . . H46C H 0.3478 0.9225 0.5942 0.044 Uiso 1 1 calc R . . C47 C 0.2905(5) 0.9667(3) 0.4436(4) 0.0392(19) Uani 1 1 d . . . H47A H 0.2421 0.9997 0.4372 0.059 Uiso 1 1 calc R . . H47B H 0.2896 0.9604 0.3913 0.059 Uiso 1 1 calc R . . H47C H 0.3537 0.9826 0.4843 0.059 Uiso 1 1 calc R . . C48 C 0.3407(5) 0.8486(3) 0.4753(5) 0.0362(18) Uani 1 1 d . . . H48A H 0.4057 0.8648 0.5106 0.054 Uiso 1 1 calc R . . H48B H 0.3318 0.8409 0.4203 0.054 Uiso 1 1 calc R . . H48C H 0.3309 0.8067 0.4972 0.054 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 0.01641(13) 0.01993(12) 0.01869(13) -0.00297(10) 0.00682(11) 0.00245(10) P1 0.0190(9) 0.0143(8) 0.0213(9) -0.0025(6) 0.0069(7) 0.0014(6) P2 0.0172(9) 0.0165(7) 0.0160(8) -0.0009(6) 0.0087(7) -0.0002(6) Cl1 0.0249(9) 0.0312(8) 0.0192(8) -0.0035(6) 0.0088(7) 0.0057(7) C1 0.026(4) 0.037(4) 0.018(4) -0.004(3) 0.008(3) 0.010(3) C2 0.014(3) 0.015(3) 0.022(3) -0.002(2) 0.006(3) 0.000(2) C3 0.019(3) 0.012(3) 0.031(4) 0.001(2) 0.015(3) 0.002(2) C4 0.016(3) 0.015(3) 0.021(3) -0.003(2) 0.009(3) -0.003(2) C5 0.036(4) 0.018(3) 0.024(4) 0.002(2) 0.020(3) -0.003(3) C6 0.043(5) 0.014(3) 0.033(4) -0.006(3) 0.023(4) -0.004(3) C7 0.042(4) 0.025(3) 0.025(4) -0.007(3) 0.021(4) 0.001(3) C8 0.039(5) 0.019(3) 0.030(4) 0.004(3) 0.023(4) 0.002(3) C9 0.022(4) 0.028(3) 0.021(4) 0.005(3) 0.008(3) 0.005(3) C10 0.031(4) 0.037(4) 0.018(4) 0.006(3) -0.002(3) 0.007(3) C11 0.025(4) 0.046(4) 0.032(4) -0.005(3) 0.009(4) 0.009(3) C12 0.019(4) 0.023(3) 0.034(4) 0.001(3) -0.001(3) -0.003(3) C13 0.032(4) 0.022(3) 0.023(4) 0.003(3) 0.011(3) 0.003(3) C14 0.023(4) 0.033(4) 0.030(4) -0.007(3) 0.005(3) -0.011(3) C15 0.051(5) 0.020(3) 0.037(5) -0.003(3) 0.022(4) -0.008(3) C16 0.042(5) 0.015(3) 0.045(5) -0.002(3) 0.015(4) 0.005(3) C17 0.022(4) 0.020(3) 0.024(4) 0.000(2) 0.013(3) -0.007(2) C18 0.014(3) 0.030(4) 0.024(4) 0.000(3) 0.007(3) -0.005(3) C19 0.029(4) 0.036(4) 0.027(4) -0.003(3) 0.017(3) -0.012(3) C20 0.028(4) 0.022(3) 0.024(4) 0.002(3) 0.009(3) -0.003(3) C21 0.015(3) 0.020(3) 0.019(3) -0.002(2) 0.005(3) 0.007(2) C22 0.022(4) 0.022(3) 0.020(4) 0.005(2) 0.006(3) 0.002(3) C23 0.020(4) 0.030(4) 0.029(4) -0.004(3) 0.005(3) 0.006(3) C24 0.014(3) 0.037(4) 0.023(4) 0.003(3) 0.008(3) -0.004(3) Pt2 0.01700(13) 0.01604(11) 0.01711(12) 0.00152(9) 0.00881(10) 0.00018(9) P3 0.0173(8) 0.0127(7) 0.0189(8) 0.0020(6) 0.0089(7) 0.0003(6) P4 0.0220(9) 0.0143(7) 0.0171(9) 0.0015(6) 0.0114(7) 0.0010(6) Cl2 0.0259(8) 0.0215(7) 0.0166(7) 0.0018(6) 0.0103(7) -0.0022(6) C25 0.035(4) 0.017(3) 0.021(4) -0.002(2) 0.020(3) -0.005(3) C26 0.013(3) 0.011(3) 0.023(3) 0.001(2) 0.009(3) 0.002(2) C27 0.011(3) 0.016(3) 0.020(3) 0.000(2) 0.006(3) -0.003(2) C28 0.018(3) 0.019(3) 0.016(3) 0.002(2) 0.011(3) -0.001(2) C29 0.036(4) 0.011(3) 0.032(4) 0.000(3) 0.020(4) 0.006(3) C30 0.034(4) 0.018(3) 0.030(4) 0.008(3) 0.022(3) 0.007(3) C31 0.026(4) 0.026(3) 0.016(3) 0.004(2) 0.013(3) -0.003(3) C32 0.016(3) 0.021(3) 0.020(4) -0.002(2) 0.009(3) -0.001(2) C33 0.021(3) 0.019(3) 0.022(4) 0.006(2) 0.007(3) -0.005(2) C34 0.034(4) 0.035(4) 0.016(4) -0.003(3) 0.003(3) -0.006(3) C35 0.024(4) 0.035(4) 0.028(4) 0.000(3) 0.010(3) -0.012(3) C36 0.018(3) 0.035(4) 0.035(4) 0.005(3) 0.000(3) -0.002(3) C37 0.024(4) 0.019(3) 0.021(4) 0.002(2) 0.010(3) 0.003(3) C38 0.026(4) 0.023(3) 0.027(4) 0.005(3) 0.006(3) 0.012(3) C39 0.039(4) 0.025(3) 0.025(4) 0.004(3) 0.016(4) 0.015(3) C40 0.040(4) 0.014(3) 0.039(5) 0.005(3) 0.019(4) 0.009(3) C41 0.031(4) 0.024(3) 0.023(4) 0.004(3) 0.018(3) 0.007(3) C42 0.018(4) 0.041(4) 0.029(4) 0.000(3) 0.011(3) 0.008(3) C43 0.038(4) 0.030(4) 0.031(4) 0.005(3) 0.024(4) 0.005(3) C44 0.047(5) 0.020(3) 0.034(4) 0.001(3) 0.027(4) 0.010(3) C45 0.027(4) 0.024(3) 0.022(4) -0.001(3) 0.011(3) -0.003(3) C46 0.035(4) 0.023(3) 0.024(4) 0.001(3) 0.008(3) -0.002(3) C47 0.043(5) 0.043(4) 0.028(4) -0.003(3) 0.014(4) -0.020(4) C48 0.017(4) 0.045(4) 0.042(5) -0.008(3) 0.011(4) -0.012(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 2.123(6) . ? Pt1 P1 2.2307(17) . ? Pt1 P2 2.3926(15) . ? Pt1 Cl1 2.4015(16) . ? P1 C2 1.832(6) . ? P1 C9 1.880(7) . ? P1 C13 1.904(7) . ? P2 C4 1.840(6) . ? P2 C21 1.902(6) . ? P2 C17 1.927(6) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C3 1.520(7) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C8 1.395(8) . ? C3 C4 1.408(8) . ? C4 C5 1.408(8) . ? C5 C6 1.378(8) . ? C5 H5 0.9500 . ? C6 C7 1.379(9) . ? C6 H6 0.9500 . ? C7 C8 1.396(8) . ? C7 H7 0.9500 . ? C8 H8 0.9500 . ? C9 C12 1.530(8) . ? C9 C10 1.537(9) . ? C9 C11 1.547(9) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C15 1.532(9) . ? C13 C14 1.540(9) . ? C13 C16 1.554(8) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? 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 C19 1.537(8) . ? C17 C18 1.538(8) . ? C17 C20 1.555(8) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C24 1.533(8) . ? C21 C23 1.534(8) . ? C21 C22 1.536(8) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? Pt2 C25 2.131(5) . ? Pt2 P3 2.2288(16) . ? Pt2 P4 2.3916(14) . ? Pt2 Cl2 2.3953(14) . ? P3 C26 1.831(5) . ? P3 C33 1.872(6) . ? P3 C37 1.916(6) . ? P4 C28 1.850(6) . ? P4 C45 1.910(7) . ? P4 C41 1.924(6) . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 C27 1.519(7) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 C32 1.384(8) . ? C27 C28 1.395(8) . ? C28 C29 1.408(8) . ? C29 C30 1.379(8) . ? C29 H29 0.9500 . ? C30 C31 1.386(8) . ? C30 H30 0.9500 . ? C31 C32 1.388(8) . ? C31 H31 0.9500 . ? C32 H32 0.9500 . ? C33 C34 1.523(9) . ? C33 C36 1.525(8) . ? C33 C35 1.539(8) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 C38 1.519(9) . ? C37 C40 1.524(8) . ? C37 C39 1.548(8) . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 C43 1.549(8) . ? C41 C44 1.545(8) . ? C41 C42 1.544(9) . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 C46 1.521(9) . ? C45 C48 1.526(9) . ? C45 C47 1.528(8) . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Pt1 P1 91.11(18) . . ? C1 Pt1 P2 168.32(19) . . ? P1 Pt1 P2 97.41(5) . . ? C1 Pt1 Cl1 80.24(18) . . ? P1 Pt1 Cl1 161.75(6) . . ? P2 Pt1 Cl1 93.66(5) . . ? C2 P1 C9 106.0(3) . . ? C2 P1 C13 97.6(3) . . ? C9 P1 C13 110.8(3) . . ? C2 P1 Pt1 109.5(2) . . ? C9 P1 Pt1 117.6(2) . . ? C13 P1 Pt1 113.1(2) . . ? C4 P2 C21 102.7(3) . . ? C4 P2 C17 104.3(3) . . ? C21 P2 C17 109.9(3) . . ? C4 P2 Pt1 115.48(19) . . ? C21 P2 Pt1 113.96(18) . . ? C17 P2 Pt1 109.84(19) . . ? Pt1 C1 H1A 109.5 . . ? Pt1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? Pt1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C3 C2 P1 119.9(4) . . ? C3 C2 H2A 107.3 . . ? P1 C2 H2A 107.3 . . ? C3 C2 H2B 107.3 . . ? P1 C2 H2B 107.3 . . ? H2A C2 H2B 106.9 . . ? C8 C3 C4 119.8(5) . . ? C8 C3 C2 114.7(5) . . ? C4 C3 C2 125.4(5) . . ? C5 C4 C3 116.5(5) . . ? C5 C4 P2 120.1(4) . . ? C3 C4 P2 123.4(4) . . ? C6 C5 C4 123.0(6) . . ? C6 C5 H5 118.5 . . ? C4 C5 H5 118.5 . . ? C7 C6 C5 120.3(6) . . ? C7 C6 H6 119.9 . . ? C5 C6 H6 119.9 . . ? C6 C7 C8 118.0(6) . . ? C6 C7 H7 121.0 . . ? C8 C7 H7 121.0 . . ? C7 C8 C3 122.3(6) . . ? C7 C8 H8 118.9 . . ? C3 C8 H8 118.9 . . ? C12 C9 C10 108.3(6) . . ? C12 C9 C11 106.2(5) . . ? C10 C9 C11 110.0(5) . . ? C12 C9 P1 107.0(4) . . ? C10 C9 P1 113.3(5) . . ? C11 C9 P1 111.6(5) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C11 H11A 109.5 . . ? C9 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C9 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C9 C12 H12A 109.5 . . ? C9 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C9 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C15 C13 C14 106.7(6) . . ? C15 C13 C16 107.6(5) . . ? C14 C13 C16 108.0(5) . . ? C15 C13 P1 114.3(4) . . ? C14 C13 P1 106.6(4) . . ? C16 C13 P1 113.2(5) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C13 C16 H16A 109.5 . . ? C13 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C13 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C19 C17 C18 106.6(5) . . ? C19 C17 C20 106.0(5) . . ? C18 C17 C20 109.8(5) . . ? C19 C17 P2 109.6(4) . . ? C18 C17 P2 107.0(4) . . ? C20 C17 P2 117.5(4) . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C17 C20 H20A 109.5 . . ? C17 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C17 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C24 C21 C23 108.1(5) . . ? C24 C21 C22 108.9(5) . . ? C23 C21 C22 108.1(5) . . ? C24 C21 P2 106.0(4) . . ? C23 C21 P2 113.7(4) . . ? C22 C21 P2 111.8(4) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C21 C24 H24A 109.5 . . ? C21 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C21 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C25 Pt2 P3 90.66(16) . . ? C25 Pt2 P4 169.12(17) . . ? P3 Pt2 P4 97.44(5) . . ? C25 Pt2 Cl2 80.57(17) . . ? P3 Pt2 Cl2 162.31(5) . . ? P4 Pt2 Cl2 93.44(5) . . ? C26 P3 C33 106.1(3) . . ? C26 P3 C37 97.5(3) . . ? C33 P3 C37 110.9(3) . . ? C26 P3 Pt2 109.66(19) . . ? C33 P3 Pt2 117.5(2) . . ? C37 P3 Pt2 113.1(2) . . ? C28 P4 C45 102.5(3) . . ? C28 P4 C41 103.6(3) . . ? C45 P4 C41 110.6(3) . . ? C28 P4 Pt2 116.18(19) . . ? C45 P4 Pt2 113.7(2) . . ? C41 P4 Pt2 109.65(19) . . ? Pt2 C25 H25A 109.5 . . ? Pt2 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? Pt2 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C27 C26 P3 122.2(4) . . ? C27 C26 H26A 106.8 . . ? P3 C26 H26A 106.8 . . ? C27 C26 H26B 106.8 . . ? P3 C26 H26B 106.8 . . ? H26A C26 H26B 106.6 . . ? C32 C27 C28 119.4(5) . . ? C32 C27 C26 115.0(5) . . ? C28 C27 C26 125.5(5) . . ? C27 C28 C29 116.9(5) . . ? C27 C28 P4 123.8(4) . . ? C29 C28 P4 119.3(4) . . ? C30 C29 C28 123.1(6) . . ? C30 C29 H29 118.5 . . ? C28 C29 H29 118.5 . . ? C29 C30 C31 119.4(5) . . ? C29 C30 H30 120.3 . . ? C31 C30 H30 120.3 . . ? C32 C31 C30 117.9(6) . . ? C32 C31 H31 121.1 . . ? C30 C31 H31 121.1 . . ? C31 C32 C27 123.2(6) . . ? C31 C32 H32 118.4 . . ? C27 C32 H32 118.4 . . ? C34 C33 C36 107.9(5) . . ? C34 C33 C35 109.2(5) . . ? C36 C33 C35 107.0(5) . . ? C34 C33 P3 113.7(5) . . ? C36 C33 P3 106.9(4) . . ? C35 C33 P3 111.9(4) . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C33 C35 H35A 109.5 . . ? C33 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C33 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C33 C36 H36A 109.5 . . ? C33 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C33 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C38 C37 C40 108.6(5) . . ? C38 C37 C39 107.3(5) . . ? C40 C37 C39 107.2(5) . . ? C38 C37 P3 107.0(4) . . ? C40 C37 P3 113.9(4) . . ? C39 C37 P3 112.6(4) . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C37 C39 H39A 109.5 . . ? C37 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C37 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C37 C40 H40A 109.5 . . ? C37 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C37 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C43 C41 C44 105.6(5) . . ? C43 C41 C42 107.3(5) . . ? C44 C41 C42 108.4(5) . . ? C43 C41 P4 108.5(4) . . ? C44 C41 P4 117.6(5) . . ? C42 C41 P4 109.1(4) . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C41 C43 H43A 109.5 . . ? C41 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C41 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C41 C44 H44A 109.5 . . ? C41 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C41 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C46 C45 C48 108.6(6) . . ? C46 C45 C47 108.3(5) . . ? C48 C45 C47 108.6(6) . . ? C46 C45 P4 112.4(5) . . ? C48 C45 P4 104.8(4) . . ? C47 C45 P4 113.9(5) . . ? C45 C46 H46A 109.5 . . ? C45 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C45 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C45 C47 H47A 109.5 . . ? C45 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C45 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C45 C48 H48A 109.5 . . ? C45 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C45 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 Pt1 P1 C2 164.6(3) . . . . ? P2 Pt1 P1 C2 -23.4(2) . . . . ? Cl1 Pt1 P1 C2 103.5(2) . . . . ? C1 Pt1 P1 C9 -74.4(3) . . . . ? P2 Pt1 P1 C9 97.6(2) . . . . ? Cl1 Pt1 P1 C9 -135.5(3) . . . . ? C1 Pt1 P1 C13 56.9(3) . . . . ? P2 Pt1 P1 C13 -131.1(2) . . . . ? Cl1 Pt1 P1 C13 -4.2(3) . . . . ? C1 Pt1 P2 C4 126.8(9) . . . . ? P1 Pt1 P2 C4 -9.7(2) . . . . ? Cl1 Pt1 P2 C4 -175.2(2) . . . . ? C1 Pt1 P2 C21 -114.6(9) . . . . ? P1 Pt1 P2 C21 108.9(2) . . . . ? Cl1 Pt1 P2 C21 -56.6(2) . . . . ? C1 Pt1 P2 C17 9.1(9) . . . . ? P1 Pt1 P2 C17 -127.4(2) . . . . ? Cl1 Pt1 P2 C17 67.2(2) . . . . ? C9 P1 C2 C3 -65.8(5) . . . . ? C13 P1 C2 C3 179.8(5) . . . . ? Pt1 P1 C2 C3 61.9(5) . . . . ? P1 C2 C3 C8 125.8(5) . . . . ? P1 C2 C3 C4 -58.0(8) . . . . ? C8 C3 C4 C5 2.0(9) . . . . ? C2 C3 C4 C5 -174.0(6) . . . . ? C8 C3 C4 P2 -176.2(5) . . . . ? C2 C3 C4 P2 7.9(9) . . . . ? C21 P2 C4 C5 80.8(5) . . . . ? C17 P2 C4 C5 -33.9(6) . . . . ? Pt1 P2 C4 C5 -154.6(4) . . . . ? C21 P2 C4 C3 -101.1(5) . . . . ? C17 P2 C4 C3 144.2(5) . . . . ? Pt1 P2 C4 C3 23.5(6) . . . . ? C3 C4 C5 C6 -2.7(10) . . . . ? P2 C4 C5 C6 175.5(5) . . . . ? C4 C5 C6 C7 0.7(11) . . . . ? C5 C6 C7 C8 2.0(10) . . . . ? C6 C7 C8 C3 -2.7(10) . . . . ? C4 C3 C8 C7 0.7(10) . . . . ? C2 C3 C8 C7 177.1(6) . . . . ? C2 P1 C9 C12 62.5(5) . . . . ? C13 P1 C9 C12 167.4(4) . . . . ? Pt1 P1 C9 C12 -60.3(5) . . . . ? C2 P1 C9 C10 -56.8(5) . . . . ? C13 P1 C9 C10 48.1(5) . . . . ? Pt1 P1 C9 C10 -179.6(4) . . . . ? C2 P1 C9 C11 178.3(4) . . . . ? C13 P1 C9 C11 -76.8(5) . . . . ? Pt1 P1 C9 C11 55.5(5) . . . . ? C2 P1 C13 C15 34.1(6) . . . . ? C9 P1 C13 C15 -76.4(6) . . . . ? Pt1 P1 C13 C15 149.1(4) . . . . ? C2 P1 C13 C14 -83.6(5) . . . . ? C9 P1 C13 C14 166.0(4) . . . . ? Pt1 P1 C13 C14 31.5(5) . . . . ? C2 P1 C13 C16 157.8(5) . . . . ? C9 P1 C13 C16 47.4(6) . . . . ? Pt1 P1 C13 C16 -87.1(5) . . . . ? C4 P2 C17 C19 -164.9(4) . . . . ? C21 P2 C17 C19 85.6(5) . . . . ? Pt1 P2 C17 C19 -40.6(5) . . . . ? C4 P2 C17 C18 -49.7(5) . . . . ? C21 P2 C17 C18 -159.3(4) . . . . ? Pt1 P2 C17 C18 74.6(4) . . . . ? C4 P2 C17 C20 74.2(5) . . . . ? C21 P2 C17 C20 -35.4(5) . . . . ? Pt1 P2 C17 C20 -161.5(4) . . . . ? C4 P2 C21 C24 82.9(4) . . . . ? C17 P2 C21 C24 -166.5(4) . . . . ? Pt1 P2 C21 C24 -42.7(4) . . . . ? C4 P2 C21 C23 -35.7(5) . . . . ? C17 P2 C21 C23 74.9(5) . . . . ? Pt1 P2 C21 C23 -161.4(4) . . . . ? C4 P2 C21 C22 -158.5(4) . . . . ? C17 P2 C21 C22 -47.9(5) . . . . ? Pt1 P2 C21 C22 75.8(4) . . . . ? C25 Pt2 P3 C26 -163.7(3) . . . . ? P4 Pt2 P3 C26 23.6(2) . . . . ? Cl2 Pt2 P3 C26 -103.9(2) . . . . ? C25 Pt2 P3 C33 75.2(3) . . . . ? P4 Pt2 P3 C33 -97.5(2) . . . . ? Cl2 Pt2 P3 C33 135.0(2) . . . . ? C25 Pt2 P3 C37 -56.0(3) . . . . ? P4 Pt2 P3 C37 131.3(2) . . . . ? Cl2 Pt2 P3 C37 3.8(3) . . . . ? C25 Pt2 P4 C28 -131.1(10) . . . . ? P3 Pt2 P4 C28 6.7(2) . . . . ? Cl2 Pt2 P4 C28 172.7(2) . . . . ? C25 Pt2 P4 C45 110.3(10) . . . . ? P3 Pt2 P4 C45 -111.9(2) . . . . ? Cl2 Pt2 P4 C45 54.1(2) . . . . ? C25 Pt2 P4 C41 -14.1(10) . . . . ? P3 Pt2 P4 C41 123.7(2) . . . . ? Cl2 Pt2 P4 C41 -70.3(2) . . . . ? C33 P3 C26 C27 68.1(5) . . . . ? C37 P3 C26 C27 -177.5(5) . . . . ? Pt2 P3 C26 C27 -59.7(5) . . . . ? P3 C26 C27 C32 -129.4(5) . . . . ? P3 C26 C27 C28 54.6(8) . . . . ? C32 C27 C28 C29 -2.6(9) . . . . ? C26 C27 C28 C29 173.3(6) . . . . ? C32 C27 C28 P4 176.8(4) . . . . ? C26 C27 C28 P4 -7.4(8) . . . . ? C45 P4 C28 C27 104.4(5) . . . . ? C41 P4 C28 C27 -140.5(5) . . . . ? Pt2 P4 C28 C27 -20.2(6) . . . . ? C45 P4 C28 C29 -76.3(5) . . . . ? C41 P4 C28 C29 38.8(6) . . . . ? Pt2 P4 C28 C29 159.1(4) . . . . ? C27 C28 C29 C30 1.6(10) . . . . ? P4 C28 C29 C30 -177.7(5) . . . . ? C28 C29 C30 C31 1.3(10) . . . . ? C29 C30 C31 C32 -3.2(9) . . . . ? C30 C31 C32 C27 2.2(9) . . . . ? C28 C27 C32 C31 0.7(9) . . . . ? C26 C27 C32 C31 -175.6(5) . . . . ? C26 P3 C33 C34 56.2(5) . . . . ? C37 P3 C33 C34 -48.6(5) . . . . ? Pt2 P3 C33 C34 179.2(4) . . . . ? C26 P3 C33 C36 -62.7(5) . . . . ? C37 P3 C33 C36 -167.5(4) . . . . ? Pt2 P3 C33 C36 60.3(5) . . . . ? C26 P3 C33 C35 -179.5(4) . . . . ? C37 P3 C33 C35 75.7(5) . . . . ? Pt2 P3 C33 C35 -56.5(5) . . . . ? C26 P3 C37 C38 83.5(5) . . . . ? C33 P3 C37 C38 -166.1(4) . . . . ? Pt2 P3 C37 C38 -31.7(5) . . . . ? C26 P3 C37 C40 -156.5(5) . . . . ? C33 P3 C37 C40 -46.1(5) . . . . ? Pt2 P3 C37 C40 88.3(5) . . . . ? C26 P3 C37 C39 -34.2(5) . . . . ? C33 P3 C37 C39 76.2(5) . . . . ? Pt2 P3 C37 C39 -149.4(4) . . . . ? C28 P4 C41 C43 162.3(4) . . . . ? C45 P4 C41 C43 -88.5(5) . . . . ? Pt2 P4 C41 C43 37.7(5) . . . . ? C28 P4 C41 C44 -78.0(5) . . . . ? C45 P4 C41 C44 31.1(6) . . . . ? Pt2 P4 C41 C44 157.3(4) . . . . ? C28 P4 C41 C42 45.8(5) . . . . ? C45 P4 C41 C42 155.0(4) . . . . ? Pt2 P4 C41 C42 -78.9(4) . . . . ? C28 P4 C45 C46 159.5(4) . . . . ? C41 P4 C45 C46 49.6(5) . . . . ? Pt2 P4 C45 C46 -74.3(4) . . . . ? C28 P4 C45 C48 -82.7(5) . . . . ? C41 P4 C45 C48 167.4(4) . . . . ? Pt2 P4 C45 C48 43.5(5) . . . . ? C28 P4 C45 C47 35.9(5) . . . . ? C41 P4 C45 C47 -74.1(5) . . . . ? Pt2 P4 C45 C47 162.1(4) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.52 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.792 _refine_diff_density_min -1.340 _refine_diff_density_rms 0.171 data_4b _database_code_depnum_ccdc_archive 'CCDC 897396' #TrackingRef '- all.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H43 Cl O3 P2 Pt' _chemical_formula_sum 'C26 H43 Cl O3 P2 Pt' _chemical_formula_weight 696.07 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.0658(1) _cell_length_b 14.8858(1) _cell_length_c 17.0888(2) _cell_angle_alpha 90.00 _cell_angle_beta 102.379(1) _cell_angle_gamma 90.00 _cell_volume 2749.48(4) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 61490 _cell_measurement_theta_min 2.0104 _cell_measurement_theta_max 30.000 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.682 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1392 _exptl_absorpt_coefficient_mu 5.342 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.67357 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) Numerical absorption correction based on gaussian integration over a multifaceted crystal model ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Oxford Diff - Gemini' _diffrn_measurement_method w/scans _diffrn_detector_area_resol_mean 10.4752 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 140525 _diffrn_reflns_av_R_equivalents 0.0468 _diffrn_reflns_av_sigmaI/netI 0.0286 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.43 _diffrn_reflns_theta_max 30.11 _reflns_number_total 8071 _reflns_number_gt 6276 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis RED, Ox Diff Ltd. V 1.171.32.5' _computing_cell_refinement 'CrysAlis CCD, Ox Diff Ltd. V 1.171.32.5' _computing_data_reduction 'CrysAlis CCD, Ox Diff Ltd. V 1.171.32.5' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0370P)^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 8071 _refine_ls_number_parameters 318 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0348 _refine_ls_R_factor_gt 0.0243 _refine_ls_wR_factor_ref 0.0637 _refine_ls_wR_factor_gt 0.0590 _refine_ls_goodness_of_fit_ref 1.094 _refine_ls_restrained_S_all 1.094 _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 0.327825(9) 0.202423(6) 0.240097(6) 0.01594(4) Uani 1 1 d . . . P1 P 0.45799(6) 0.28193(4) 0.33276(4) 0.01437(14) Uani 1 1 d . . . P2 P 0.17845(6) 0.31632(4) 0.20912(4) 0.01293(13) Uani 1 1 d . . . Cl1A Cl 0.2432(3) 0.1052(2) 0.13106(18) 0.0373(6) Uani 0.85 1 d P . . Cl1B Cl 0.2259(19) 0.0954(13) 0.1534(10) 0.032(3) Uani 0.15 1 d P . . O1 O -0.07527(16) 0.34638(12) 0.16457(11) 0.0164(4) Uani 1 1 d . . . O2 O -0.07715(16) 0.38034(12) 0.02995(10) 0.0162(4) Uani 1 1 d . . . O3 O 0.13807(16) 0.35653(12) 0.05109(10) 0.0156(4) Uani 1 1 d . . . C2 C 0.4107(2) 0.40137(17) 0.32712(16) 0.0175(5) Uani 1 1 d . . . H2A H 0.4718 0.4350 0.3651 0.021 Uiso 1 1 calc R . . H2B H 0.4126 0.4235 0.2740 0.021 Uiso 1 1 calc R . . C3 C 0.2850(2) 0.42120(17) 0.34351(16) 0.0173(5) Uani 1 1 d . . . C8 C 0.2786(3) 0.47895(19) 0.40711(17) 0.0230(6) Uani 1 1 d . . . H8 H 0.3512 0.5046 0.4360 0.028 Uiso 1 1 calc R . . C7 C 0.1680(3) 0.4992(2) 0.42860(17) 0.0246(6) Uani 1 1 d . . . H7 H 0.1670 0.5374 0.4715 0.029 Uiso 1 1 calc R . . C6 C 0.0593(3) 0.46247(19) 0.38591(16) 0.0206(6) Uani 1 1 d . . . H6 H -0.0154 0.4747 0.4003 0.025 Uiso 1 1 calc R . . C5 C 0.0630(2) 0.40717(18) 0.32150(15) 0.0164(5) Uani 1 1 d . . . H5 H -0.0107 0.3830 0.2926 0.020 Uiso 1 1 calc R . . C4 C 0.1740(2) 0.38613(17) 0.29803(15) 0.0145(5) Uani 1 1 d . . . C17 C 0.1640(2) 0.40382(17) 0.12645(15) 0.0147(5) Uani 1 1 d . . . C23 C 0.2820(2) 0.45573(18) 0.12715(16) 0.0177(5) Uani 1 1 d . . . H23A H 0.3478 0.4145 0.1248 0.026 Uiso 1 1 calc R . . H23B H 0.3033 0.4905 0.1755 0.026 Uiso 1 1 calc R . . H23C H 0.2698 0.4951 0.0817 0.026 Uiso 1 1 calc R . . C18 C 0.0560(2) 0.46607(17) 0.12932(15) 0.0152(5) Uani 1 1 d . . . H18A H 0.0665 0.4915 0.1826 0.018 Uiso 1 1 calc R . . H18B H 0.0554 0.5151 0.0918 0.018 Uiso 1 1 calc R . . C19 C -0.0665(2) 0.41651(18) 0.10847(15) 0.0157(5) Uani 1 1 d . . . C24 C -0.1767(2) 0.47688(19) 0.10692(17) 0.0213(6) Uani 1 1 d . . . H24A H -0.1753 0.5255 0.0702 0.032 Uiso 1 1 calc R . . H24B H -0.1733 0.5006 0.1596 0.032 Uiso 1 1 calc R . . H24C H -0.2515 0.4430 0.0900 0.032 Uiso 1 1 calc R . . C22 C 0.0185(2) 0.31536(17) 0.02882(16) 0.0156(5) Uani 1 1 d . . . C26 C 0.0068(3) 0.28546(18) -0.05667(16) 0.0196(6) Uani 1 1 d . . . H26A H 0.0193 0.3360 -0.0890 0.029 Uiso 1 1 calc R . . H26B H -0.0743 0.2610 -0.0765 0.029 Uiso 1 1 calc R . . H26C H 0.0679 0.2404 -0.0591 0.029 Uiso 1 1 calc R . . C21 C 0.0051(2) 0.23968(18) 0.08481(15) 0.0160(5) Uani 1 1 d . . . H21A H 0.0691 0.1953 0.0845 0.019 Uiso 1 1 calc R . . H21B H -0.0746 0.2108 0.0666 0.019 Uiso 1 1 calc R . . C20 C 0.0153(2) 0.27490(18) 0.16983(16) 0.0152(5) Uani 1 1 d . . . C25 C -0.0193(3) 0.20249(18) 0.22298(17) 0.0194(6) Uani 1 1 d . . . H25A H -0.0017 0.2229 0.2775 0.029 Uiso 1 1 calc R . . H25B H 0.0278 0.1492 0.2188 0.029 Uiso 1 1 calc R . . H25C H -0.1060 0.1893 0.2064 0.029 Uiso 1 1 calc R . . C13 C 0.4725(3) 0.25050(19) 0.44203(17) 0.0222(6) Uani 1 1 d . . . C14 C 0.3428(3) 0.2213(2) 0.4502(2) 0.0315(7) Uani 1 1 d . . . H14A H 0.3214 0.1657 0.4220 0.047 Uiso 1 1 calc R . . H14B H 0.2838 0.2667 0.4278 0.047 Uiso 1 1 calc R . . H14C H 0.3419 0.2131 0.5058 0.047 Uiso 1 1 calc R . . C15 C 0.5131(3) 0.3307(2) 0.49909(18) 0.0297(7) Uani 1 1 d . . . H15A H 0.4512 0.3768 0.4883 0.045 Uiso 1 1 calc R . . H15B H 0.5903 0.3540 0.4908 0.045 Uiso 1 1 calc R . . H15C H 0.5230 0.3109 0.5536 0.045 Uiso 1 1 calc R . . C16 C 0.5649(3) 0.1747(2) 0.47263(19) 0.0339(8) Uani 1 1 d . . . H16A H 0.5649 0.1624 0.5278 0.051 Uiso 1 1 calc R . . H16B H 0.6463 0.1927 0.4679 0.051 Uiso 1 1 calc R . . H21C H 0.5412 0.1215 0.4413 0.051 Uiso 1 1 calc R . . C9 C 0.6151(2) 0.29166(18) 0.30560(17) 0.0186(6) Uani 1 1 d . . . C11 C 0.7026(3) 0.3546(2) 0.36214(19) 0.0267(7) Uani 1 1 d . . . H11A H 0.7208 0.3295 0.4151 0.040 Uiso 1 1 calc R . . H11B H 0.6639 0.4121 0.3632 0.040 Uiso 1 1 calc R . . H11C H 0.7779 0.3615 0.3435 0.040 Uiso 1 1 calc R . . C12 C 0.6790(3) 0.20053(18) 0.30366(19) 0.0222(6) Uani 1 1 d . . . H12A H 0.7581 0.2093 0.2903 0.033 Uiso 1 1 calc R . . H12B H 0.6287 0.1627 0.2641 0.033 Uiso 1 1 calc R . . H12C H 0.6901 0.1725 0.3553 0.033 Uiso 1 1 calc R . . C10 C 0.5921(3) 0.3297(2) 0.21967(18) 0.0258(6) Uani 1 1 d . . . H10A H 0.5603 0.3897 0.2193 0.039 Uiso 1 1 calc R . . H10B H 0.5332 0.2925 0.1847 0.039 Uiso 1 1 calc R . . H10C H 0.6685 0.3304 0.2016 0.039 Uiso 1 1 calc R . . C1 C 0.4292(2) 0.08340(17) 0.28044(17) 0.0179(6) Uani 1 1 d . . . H1A H 0.4918 0.0967 0.3272 0.027 Uiso 1 1 calc R . . H1B H 0.4674 0.0611 0.2389 0.027 Uiso 1 1 calc R . . H1C H 0.3739 0.0387 0.2933 0.027 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 0.01213(5) 0.01211(6) 0.02301(6) -0.00264(4) 0.00254(4) -0.00040(4) P1 0.0114(3) 0.0146(3) 0.0165(3) 0.0011(2) 0.0016(3) 0.0000(2) P2 0.0115(3) 0.0140(3) 0.0130(3) -0.0003(2) 0.0019(2) -0.0004(2) Cl1A 0.0313(11) 0.0288(12) 0.0436(15) -0.0201(10) -0.0099(8) 0.0095(8) Cl1B 0.027(5) 0.017(4) 0.044(8) -0.014(5) -0.009(5) -0.001(3) O1 0.0148(9) 0.0185(10) 0.0163(9) 0.0021(7) 0.0044(7) 0.0008(7) O2 0.0153(9) 0.0210(10) 0.0114(9) -0.0012(7) 0.0004(7) 0.0022(8) O3 0.0164(9) 0.0182(9) 0.0127(9) -0.0021(7) 0.0043(7) -0.0030(7) C2 0.0189(13) 0.0123(12) 0.0200(13) -0.0021(10) 0.0011(11) -0.0021(10) C3 0.0176(13) 0.0128(12) 0.0203(14) 0.0019(10) 0.0014(11) 0.0027(10) C8 0.0236(15) 0.0201(14) 0.0210(14) -0.0049(11) -0.0048(12) 0.0018(12) C7 0.0307(16) 0.0219(15) 0.0193(14) -0.0065(11) 0.0013(12) 0.0066(13) C6 0.0235(14) 0.0231(15) 0.0164(13) 0.0008(11) 0.0069(11) 0.0060(12) C5 0.0163(12) 0.0190(13) 0.0123(12) -0.0006(10) -0.0005(10) 0.0015(10) C4 0.0190(13) 0.0111(12) 0.0126(12) 0.0029(10) 0.0014(10) 0.0021(10) C17 0.0150(12) 0.0161(13) 0.0124(12) -0.0008(10) 0.0014(10) -0.0012(10) C23 0.0184(13) 0.0169(13) 0.0169(13) 0.0026(10) 0.0019(11) -0.0042(11) C18 0.0190(13) 0.0142(12) 0.0119(12) 0.0008(10) 0.0020(10) 0.0012(10) C19 0.0170(13) 0.0163(13) 0.0129(12) 0.0014(10) 0.0014(10) 0.0027(10) C24 0.0190(13) 0.0244(15) 0.0203(14) 0.0023(11) 0.0035(11) 0.0080(11) C22 0.0132(12) 0.0179(13) 0.0149(13) -0.0022(10) 0.0013(10) -0.0008(10) C26 0.0164(13) 0.0243(15) 0.0173(14) -0.0042(11) 0.0015(11) -0.0023(11) C21 0.0151(13) 0.0174(13) 0.0143(13) -0.0026(10) 0.0008(10) -0.0034(10) C20 0.0139(12) 0.0170(13) 0.0145(13) 0.0006(10) 0.0030(10) -0.0006(10) C25 0.0144(12) 0.0236(14) 0.0201(14) 0.0014(11) 0.0035(11) -0.0057(11) C13 0.0214(14) 0.0242(16) 0.0206(14) 0.0040(12) 0.0035(12) 0.0040(12) C14 0.0319(18) 0.0396(19) 0.0262(17) 0.0047(14) 0.0132(14) -0.0059(14) C15 0.0319(17) 0.0354(17) 0.0193(15) -0.0005(13) 0.0001(13) 0.0040(15) C16 0.046(2) 0.0301(17) 0.0254(17) 0.0097(14) 0.0069(15) 0.0098(16) C9 0.0112(12) 0.0206(14) 0.0237(14) -0.0011(11) 0.0031(11) -0.0031(10) C11 0.0152(14) 0.0276(16) 0.0363(17) -0.0042(13) 0.0029(12) -0.0051(12) C12 0.0159(13) 0.0204(14) 0.0318(17) -0.0004(12) 0.0084(12) 0.0020(11) C10 0.0195(14) 0.0328(16) 0.0270(16) 0.0033(13) 0.0093(12) -0.0003(13) C1 0.0083(11) 0.0118(12) 0.0309(15) -0.0027(11) -0.0018(11) 0.0020(10) _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 2.131(2) . ? Pt1 P1 2.2372(7) . ? Pt1 Cl1B 2.30(2) . ? Pt1 P2 2.3478(7) . ? Pt1 Cl1A 2.386(4) . ? P1 C2 1.850(3) . ? P1 C13 1.898(3) . ? P1 C9 1.898(3) . ? P2 C4 1.850(3) . ? P2 C20 1.890(3) . ? P2 C17 1.903(3) . ? O1 C19 1.435(3) . ? O1 C20 1.451(3) . ? O2 C19 1.427(3) . ? O2 C22 1.437(3) . ? O3 C22 1.434(3) . ? O3 C17 1.441(3) . ? C2 C3 1.506(4) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C8 1.399(4) . ? C3 C4 1.406(4) . ? C8 C7 1.384(4) . ? C8 H8 0.9300 . ? C7 C6 1.379(4) . ? C7 H7 0.9300 . ? C6 C5 1.382(4) . ? C6 H6 0.9300 . ? C5 C4 1.407(4) . ? C5 H5 0.9300 . ? C17 C23 1.515(3) . ? C17 C18 1.521(3) . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C18 C19 1.517(4) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 C24 1.510(4) . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C22 C21 1.506(4) . ? C22 C26 1.506(4) . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C21 C20 1.526(4) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C20 C25 1.511(4) . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C13 C14 1.535(4) . ? C13 C16 1.538(4) . ? C13 C15 1.545(4) . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H21C 0.9600 . ? C9 C11 1.532(4) . ? C9 C12 1.533(4) . ? C9 C10 1.543(4) . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? 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 P1 89.80(7) . . ? C1 Pt1 Cl1B 77.5(5) . . ? P1 Pt1 Cl1B 167.1(5) . . ? C1 Pt1 P2 165.86(8) . . ? P1 Pt1 P2 95.33(2) . . ? Cl1B Pt1 P2 97.5(5) . . ? C1 Pt1 Cl1A 80.78(12) . . ? P1 Pt1 Cl1A 163.50(8) . . ? Cl1B Pt1 Cl1A 11.7(3) . . ? P2 Pt1 Cl1A 97.02(9) . . ? C2 P1 C13 104.57(13) . . ? C2 P1 C9 100.22(12) . . ? C13 P1 C9 111.74(13) . . ? C2 P1 Pt1 109.85(9) . . ? C13 P1 Pt1 118.15(10) . . ? C9 P1 Pt1 110.59(9) . . ? C4 P2 C20 106.46(12) . . ? C4 P2 C17 102.27(11) . . ? C20 P2 C17 92.16(11) . . ? C4 P2 Pt1 111.22(8) . . ? C20 P2 Pt1 114.66(9) . . ? C17 P2 Pt1 127.22(8) . . ? C19 O1 C20 115.48(19) . . ? C19 O2 C22 110.74(18) . . ? C22 O3 C17 116.20(19) . . ? C3 C2 P1 116.16(19) . . ? C3 C2 H2A 108.2 . . ? P1 C2 H2A 108.2 . . ? C3 C2 H2B 108.2 . . ? P1 C2 H2B 108.2 . . ? H2A C2 H2B 107.4 . . ? C8 C3 C4 118.2(2) . . ? C8 C3 C2 117.9(2) . . ? C4 C3 C2 123.9(2) . . ? C7 C8 C3 122.4(3) . . ? C7 C8 H8 118.8 . . ? C3 C8 H8 118.8 . . ? C6 C7 C8 119.6(3) . . ? C6 C7 H7 120.2 . . ? C8 C7 H7 120.2 . . ? C7 C6 C5 119.1(3) . . ? C7 C6 H6 120.4 . . ? C5 C6 H6 120.4 . . ? C6 C5 C4 122.4(2) . . ? C6 C5 H5 118.8 . . ? C4 C5 H5 118.8 . . ? C3 C4 C5 118.2(2) . . ? C3 C4 P2 119.2(2) . . ? C5 C4 P2 122.55(19) . . ? O3 C17 C23 105.2(2) . . ? O3 C17 C18 108.6(2) . . ? C23 C17 C18 111.8(2) . . ? O3 C17 P2 107.33(16) . . ? C23 C17 P2 114.08(17) . . ? C18 C17 P2 109.55(17) . . ? C17 C23 H23A 109.5 . . ? C17 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C17 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C19 C18 C17 111.4(2) . . ? C19 C18 H18A 109.3 . . ? C17 C18 H18A 109.3 . . ? C19 C18 H18B 109.3 . . ? C17 C18 H18B 109.3 . . ? H18A C18 H18B 108.0 . . ? O2 C19 O1 110.5(2) . . ? O2 C19 C24 107.7(2) . . ? O1 C19 C24 106.0(2) . . ? O2 C19 C18 107.1(2) . . ? O1 C19 C18 112.4(2) . . ? C24 C19 C18 113.1(2) . . ? C19 C24 H24A 109.5 . . ? C19 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C19 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? O3 C22 O2 110.4(2) . . ? O3 C22 C21 111.2(2) . . ? O2 C22 C21 108.8(2) . . ? O3 C22 C26 105.5(2) . . ? O2 C22 C26 107.5(2) . . ? C21 C22 C26 113.3(2) . . ? C22 C26 H26A 109.5 . . ? C22 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C22 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C22 C21 C20 110.5(2) . . ? C22 C21 H21A 109.5 . . ? C20 C21 H21A 109.5 . . ? C22 C21 H21B 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 108.1 . . ? O1 C20 C25 107.4(2) . . ? O1 C20 C21 106.5(2) . . ? C25 C20 C21 110.5(2) . . ? O1 C20 P2 112.16(17) . . ? C25 C20 P2 111.42(18) . . ? C21 C20 P2 108.70(18) . . ? C20 C25 H25A 109.5 . . ? C20 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C20 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C14 C13 C16 109.2(3) . . ? C14 C13 C15 108.2(3) . . ? C16 C13 C15 105.7(3) . . ? C14 C13 P1 106.0(2) . . ? C16 C13 P1 115.2(2) . . ? C15 C13 P1 112.5(2) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C13 C16 H16A 109.5 . . ? C13 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C13 C16 H21C 109.5 . . ? H16A C16 H21C 109.5 . . ? H16B C16 H21C 109.5 . . ? C11 C9 C12 108.8(2) . . ? C11 C9 C10 109.2(2) . . ? C12 C9 C10 106.6(2) . . ? C11 C9 P1 112.4(2) . . ? C12 C9 P1 112.86(18) . . ? C10 C9 P1 106.74(18) . . ? C9 C11 H11A 109.5 . . ? C9 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C9 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C9 C12 H12A 109.5 . . ? C9 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C9 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? Pt1 C1 H1A 109.5 . . ? Pt1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? Pt1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 Pt1 P1 C2 -179.13(12) . . . . ? Cl1B Pt1 P1 C2 171.4(14) . . . . ? P2 Pt1 P1 C2 -12.33(10) . . . . ? Cl1A Pt1 P1 C2 126.0(3) . . . . ? C1 Pt1 P1 C13 -59.36(13) . . . . ? Cl1B Pt1 P1 C13 -68.9(14) . . . . ? P2 Pt1 P1 C13 107.44(10) . . . . ? Cl1A Pt1 P1 C13 -114.2(3) . . . . ? C1 Pt1 P1 C9 71.16(12) . . . . ? Cl1B Pt1 P1 C9 61.7(14) . . . . ? P2 Pt1 P1 C9 -122.04(9) . . . . ? Cl1A Pt1 P1 C9 16.3(3) . . . . ? C1 Pt1 P2 C4 78.7(3) . . . . ? P1 Pt1 P2 C4 -32.19(9) . . . . ? Cl1B Pt1 P2 C4 147.0(3) . . . . ? Cl1A Pt1 P2 C4 158.77(11) . . . . ? C1 Pt1 P2 C20 -42.2(3) . . . . ? P1 Pt1 P2 C20 -153.03(9) . . . . ? Cl1B Pt1 P2 C20 26.1(3) . . . . ? Cl1A Pt1 P2 C20 37.93(11) . . . . ? C1 Pt1 P2 C17 -155.8(3) . . . . ? P1 Pt1 P2 C17 93.33(10) . . . . ? Cl1B Pt1 P2 C17 -87.5(3) . . . . ? Cl1A Pt1 P2 C17 -75.71(12) . . . . ? C13 P1 C2 C3 -65.6(2) . . . . ? C9 P1 C2 C3 178.6(2) . . . . ? Pt1 P1 C2 C3 62.1(2) . . . . ? P1 C2 C3 C8 120.7(2) . . . . ? P1 C2 C3 C4 -60.3(3) . . . . ? C4 C3 C8 C7 2.9(4) . . . . ? C2 C3 C8 C7 -178.0(3) . . . . ? C3 C8 C7 C6 -0.7(4) . . . . ? C8 C7 C6 C5 -1.1(4) . . . . ? C7 C6 C5 C4 0.6(4) . . . . ? C8 C3 C4 C5 -3.3(4) . . . . ? C2 C3 C4 C5 177.6(2) . . . . ? C8 C3 C4 P2 175.6(2) . . . . ? C2 C3 C4 P2 -3.5(4) . . . . ? C6 C5 C4 C3 1.7(4) . . . . ? C6 C5 C4 P2 -177.2(2) . . . . ? C20 P2 C4 C3 175.6(2) . . . . ? C17 P2 C4 C3 -88.5(2) . . . . ? Pt1 P2 C4 C3 50.0(2) . . . . ? C20 P2 C4 C5 -5.6(2) . . . . ? C17 P2 C4 C5 90.4(2) . . . . ? Pt1 P2 C4 C5 -131.2(2) . . . . ? C22 O3 C17 C23 -168.7(2) . . . . ? C22 O3 C17 C18 -48.9(3) . . . . ? C22 O3 C17 P2 69.4(2) . . . . ? C4 P2 C17 O3 -167.15(16) . . . . ? C20 P2 C17 O3 -59.79(17) . . . . ? Pt1 P2 C17 O3 63.78(18) . . . . ? C4 P2 C17 C23 76.7(2) . . . . ? C20 P2 C17 C23 -175.9(2) . . . . ? Pt1 P2 C17 C23 -52.3(2) . . . . ? C4 P2 C17 C18 -49.40(19) . . . . ? C20 P2 C17 C18 57.95(18) . . . . ? Pt1 P2 C17 C18 -178.47(13) . . . . ? O3 C17 C18 C19 50.6(3) . . . . ? C23 C17 C18 C19 166.2(2) . . . . ? P2 C17 C18 C19 -66.4(2) . . . . ? C22 O2 C19 O1 -59.1(3) . . . . ? C22 O2 C19 C24 -174.4(2) . . . . ? C22 O2 C19 C18 63.6(2) . . . . ? C20 O1 C19 O2 57.7(3) . . . . ? C20 O1 C19 C24 174.1(2) . . . . ? C20 O1 C19 C18 -61.9(3) . . . . ? C17 C18 C19 O2 -58.9(3) . . . . ? C17 C18 C19 O1 62.7(3) . . . . ? C17 C18 C19 C24 -177.4(2) . . . . ? C17 O3 C22 O2 54.4(3) . . . . ? C17 O3 C22 C21 -66.4(3) . . . . ? C17 O3 C22 C26 170.4(2) . . . . ? C19 O2 C22 O3 -61.4(3) . . . . ? C19 O2 C22 C21 61.0(3) . . . . ? C19 O2 C22 C26 -176.0(2) . . . . ? O3 C22 C21 C20 62.5(3) . . . . ? O2 C22 C21 C20 -59.3(3) . . . . ? C26 C22 C21 C20 -178.9(2) . . . . ? C19 O1 C20 C25 -172.6(2) . . . . ? C19 O1 C20 C21 -54.2(3) . . . . ? C19 O1 C20 P2 64.6(2) . . . . ? C22 C21 C20 O1 54.1(3) . . . . ? C22 C21 C20 C25 170.5(2) . . . . ? C22 C21 C20 P2 -66.9(2) . . . . ? C4 P2 C20 O1 46.8(2) . . . . ? C17 P2 C20 O1 -56.62(18) . . . . ? Pt1 P2 C20 O1 170.27(13) . . . . ? C4 P2 C20 C25 -73.6(2) . . . . ? C17 P2 C20 C25 -177.1(2) . . . . ? Pt1 P2 C20 C25 49.8(2) . . . . ? C4 P2 C20 C21 164.31(17) . . . . ? C17 P2 C20 C21 60.85(19) . . . . ? Pt1 P2 C20 C21 -72.26(19) . . . . ? C2 P1 C13 C14 86.8(2) . . . . ? C9 P1 C13 C14 -165.66(19) . . . . ? Pt1 P1 C13 C14 -35.7(2) . . . . ? C2 P1 C13 C16 -152.4(2) . . . . ? C9 P1 C13 C16 -44.9(3) . . . . ? Pt1 P1 C13 C16 85.1(2) . . . . ? C2 P1 C13 C15 -31.2(2) . . . . ? C9 P1 C13 C15 76.3(2) . . . . ? Pt1 P1 C13 C15 -153.72(18) . . . . ? C2 P1 C9 C11 57.5(2) . . . . ? C13 P1 C9 C11 -52.8(2) . . . . ? Pt1 P1 C9 C11 173.40(17) . . . . ? C2 P1 C9 C12 -179.0(2) . . . . ? C13 P1 C9 C12 70.7(2) . . . . ? Pt1 P1 C9 C12 -63.1(2) . . . . ? C2 P1 C9 C10 -62.2(2) . . . . ? C13 P1 C9 C10 -172.47(19) . . . . ? Pt1 P1 C9 C10 53.7(2) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 30.11 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 3.137 _refine_diff_density_min -0.947 _refine_diff_density_rms 0.125 data_4f _database_code_depnum_ccdc_archive 'CCDC 897397' #TrackingRef '- all.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H41 Cl O6 P2 Pt, C H2 Cl2' _chemical_formula_sum 'C29 H43 Cl3 O6 P2 Pt' _chemical_formula_weight 851.01 _chemical_absolute_configuration ad loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 10.588(4) _cell_length_b 14.583(5) _cell_length_c 11.873(4) _cell_angle_alpha 90.00 _cell_angle_beta 116.01(2) _cell_angle_gamma 90.00 _cell_volume 1647.6(10) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9958 _cell_measurement_theta_min 30.4935 _cell_measurement_theta_max 2.5675 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.715 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 848 _exptl_absorpt_coefficient_mu 4.638 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.248 _exptl_absorpt_correction_T_max 0.690 _exptl_absorpt_process_details 'SADABS V2008/1' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 24888 _diffrn_reflns_av_R_equivalents 0.0262 _diffrn_reflns_av_sigmaI/netI 0.0563 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.57 _diffrn_reflns_theta_max 30.52 _reflns_number_total 9839 _reflns_number_gt 9295 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Apex II (Bruker-AXS, 2007)' _computing_cell_refinement 'Apex II (Bruker-AXS, 2007)' _computing_data_reduction ; SAINT v7.34A (Bruker-AXS, 2007) & XPREP v2005/4 (Bruker-AXS, 2005) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0000P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.006(3) _refine_ls_number_reflns 9839 _refine_ls_number_parameters 380 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0216 _refine_ls_R_factor_gt 0.0197 _refine_ls_wR_factor_ref 0.0402 _refine_ls_wR_factor_gt 0.0397 _refine_ls_goodness_of_fit_ref 0.778 _refine_ls_restrained_S_all 0.778 _refine_ls_shift/su_max 0.003 _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 -0.016108(8) 0.748258(9) 0.857071(7) 0.00991(2) Uani 1 1 d . . . P1 P 0.15892(7) 0.84180(4) 0.96689(7) 0.00972(13) Uani 1 1 d . . . P2 P -0.17235(8) 0.87033(4) 0.75277(7) 0.00976(14) Uani 1 1 d . . . Cl1 Cl -0.19527(8) 0.63464(4) 0.78479(7) 0.01834(16) Uani 1 1 d . . . O1 O 0.38146(16) 0.73821(15) 1.12989(16) 0.0146(4) Uani 1 1 d . . . O2 O 0.38558(18) 0.94283(11) 0.99564(17) 0.0141(4) Uani 1 1 d . . . O3 O 0.5557(2) 0.83973(12) 1.1303(2) 0.0165(4) Uani 1 1 d . . . O4 O -0.37966(19) 0.93652(11) 0.53063(18) 0.0132(4) Uani 1 1 d . . . O5 O -0.41518(18) 0.81784(11) 0.75787(17) 0.0122(3) Uani 1 1 d . . . O6 O -0.56948(18) 0.88389(10) 0.56541(18) 0.0149(4) Uani 1 1 d . . . C1 C 0.1151(3) 0.63415(17) 0.9279(3) 0.0163(6) Uani 1 1 d . . . H1A H 0.2090 0.6545 0.9873 0.024 Uiso 1 1 calc R . . H1B H 0.1213 0.6009 0.8587 0.024 Uiso 1 1 calc R . . H1C H 0.0763 0.5936 0.9707 0.024 Uiso 1 1 calc R . . C2 C 0.0831(3) 0.94917(15) 0.9909(2) 0.0133(5) Uani 1 1 d . . . H2A H 0.0065 0.9346 1.0144 0.016 Uiso 1 1 calc R . . H2B H 0.1562 0.9836 1.0610 0.016 Uiso 1 1 calc R . . C3 C 0.0262(3) 1.00804(15) 0.8760(2) 0.0121(5) Uani 1 1 d . . . C4 C -0.0870(3) 0.98208(14) 0.7614(2) 0.0112(5) Uani 1 1 d . . . C5 C -0.1229(3) 1.04018(18) 0.6572(3) 0.0146(5) Uani 1 1 d . . . H5 H -0.1970 1.0232 0.5789 0.018 Uiso 1 1 calc R . . C6 C -0.0515(3) 1.12226(15) 0.6671(3) 0.0161(5) Uani 1 1 d . . . H6 H -0.0771 1.1606 0.5957 0.019 Uiso 1 1 calc R . . C7 C 0.0569(3) 1.14825(15) 0.7809(3) 0.0168(5) Uani 1 1 d . . . H7 H 0.1046 1.2047 0.7878 0.020 Uiso 1 1 calc R . . C8 C 0.0949(3) 1.09197(15) 0.8833(3) 0.0142(5) Uani 1 1 d . . . H8 H 0.1692 1.1101 0.9610 0.017 Uiso 1 1 calc R . . C9 C 0.2973(3) 0.87070(15) 0.9154(2) 0.0126(5) Uani 1 1 d . . . C10 C 0.3850(3) 0.78360(16) 0.9327(3) 0.0145(5) Uani 1 1 d . . . H10A H 0.3218 0.7315 0.8908 0.017 Uiso 1 1 calc R . . H10B H 0.4490 0.7922 0.8929 0.017 Uiso 1 1 calc R . . C11 C 0.4709(2) 0.76162(15) 1.0714(2) 0.0148(6) Uani 1 1 d . . . C12 C 0.2892(3) 0.81072(16) 1.1317(2) 0.0131(5) Uani 1 1 d . . . C13 C 0.3834(3) 0.89353(16) 1.1932(2) 0.0149(5) Uani 1 1 d . . . H13A H 0.3246 0.9466 1.1920 0.018 Uiso 1 1 calc R . . H13B H 0.4468 0.8791 1.2817 0.018 Uiso 1 1 calc R . . C14 C 0.4704(3) 0.91797(16) 1.1235(3) 0.0150(5) Uani 1 1 d . . . C15 C 0.2404(3) 0.90575(17) 0.7816(3) 0.0170(5) Uani 1 1 d . . . H15A H 0.1979 0.9663 0.7760 0.025 Uiso 1 1 calc R . . H15B H 0.1693 0.8630 0.7252 0.025 Uiso 1 1 calc R . . H15C H 0.3174 0.9105 0.7571 0.025 Uiso 1 1 calc R . . C16 C 0.5684(3) 0.68119(19) 1.0941(3) 0.0241(7) Uani 1 1 d . . . H16A H 0.6308 0.6928 1.0543 0.036 Uiso 1 1 calc R . . H16B H 0.5132 0.6257 1.0583 0.036 Uiso 1 1 calc R . . H16C H 0.6248 0.6728 1.1845 0.036 Uiso 1 1 calc R . . C17 C 0.2161(3) 0.77426(17) 1.2065(3) 0.0187(5) Uani 1 1 d . . . H17A H 0.1583 0.7212 1.1633 0.028 Uiso 1 1 calc R . . H17B H 0.1561 0.8222 1.2151 0.028 Uiso 1 1 calc R . . H17C H 0.2864 0.7556 1.2898 0.028 Uiso 1 1 calc R . . C18 C 0.5688(3) 0.99756(17) 1.1819(3) 0.0203(6) Uani 1 1 d . . . H18A H 0.6304 1.0051 1.1405 0.030 Uiso 1 1 calc R . . H18B H 0.6259 0.9855 1.2713 0.030 Uiso 1 1 calc R . . H18C H 0.5139 1.0537 1.1718 0.030 Uiso 1 1 calc R . . C19 C -0.2940(3) 0.85512(14) 0.5811(2) 0.0112(5) Uani 1 1 d . . . C20 C -0.3967(3) 0.77747(15) 0.5667(2) 0.0126(5) Uani 1 1 d . . . H20A H -0.4540 0.7643 0.4766 0.015 Uiso 1 1 calc R . . H20B H -0.3435 0.7213 0.6069 0.015 Uiso 1 1 calc R . . C21 C -0.4924(3) 0.80271(15) 0.6262(2) 0.0130(5) Uani 1 1 d . . . C22 C -0.3209(3) 0.89569(14) 0.7955(2) 0.0125(5) Uani 1 1 d . . . C23 C -0.4009(3) 0.97965(15) 0.7227(3) 0.0148(5) Uani 1 1 d . . . H23A H -0.3346 1.0312 0.7377 0.018 Uiso 1 1 calc R . . H23B H -0.4709 0.9983 0.7527 0.018 Uiso 1 1 calc R . . C24 C -0.4755(3) 0.95877(15) 0.5826(3) 0.0136(5) Uani 1 1 d . . . C25 C -0.2141(3) 0.83706(16) 0.5043(3) 0.0159(5) Uani 1 1 d . . . H25A H -0.2806 0.8315 0.4157 0.024 Uiso 1 1 calc R . . H25B H -0.1605 0.7800 0.5327 0.024 Uiso 1 1 calc R . . H25C H -0.1495 0.8880 0.5150 0.024 Uiso 1 1 calc R . . C26 C -0.6005(3) 0.72979(14) 0.6116(3) 0.0175(6) Uani 1 1 d . . . H26A H -0.5526 0.6727 0.6510 0.026 Uiso 1 1 calc R . . H26B H -0.6603 0.7190 0.5223 0.026 Uiso 1 1 calc R . . H26C H -0.6587 0.7505 0.6521 0.026 Uiso 1 1 calc R . . C27 C -0.2731(3) 0.90498(16) 0.9349(3) 0.0161(5) Uani 1 1 d . . . H27A H -0.3552 0.9107 0.9520 0.024 Uiso 1 1 calc R . . H27B H -0.2141 0.9597 0.9655 0.024 Uiso 1 1 calc R . . H27C H -0.2188 0.8506 0.9776 0.024 Uiso 1 1 calc R . . C28 C -0.5609(3) 1.03854(17) 0.5068(3) 0.0223(7) Uani 1 1 d . . . H28A H -0.6106 1.0206 0.4185 0.033 Uiso 1 1 calc R . . H28B H -0.4985 1.0903 0.5149 0.033 Uiso 1 1 calc R . . H28C H -0.6293 1.0566 0.5376 0.033 Uiso 1 1 calc R . . C29 C 0.0862(3) 0.9618(2) 0.3663(3) 0.0250(7) Uani 1 1 d . . . H29A H 0.1641 0.9183 0.4106 0.030 Uiso 1 1 calc R . . H29B H 0.1117 1.0004 0.3109 0.030 Uiso 1 1 calc R . . Cl2 Cl -0.06989(8) 0.89991(5) 0.27474(8) 0.02988(17) Uani 1 1 d . . . Cl3 Cl 0.06240(10) 1.03187(6) 0.47675(9) 0.0398(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.01021(4) 0.00822(3) 0.00996(4) 0.00039(5) 0.00319(3) -0.00001(5) P1 0.0086(3) 0.0095(2) 0.0103(3) 0.0005(2) 0.0035(3) 0.0012(2) P2 0.0089(3) 0.0093(2) 0.0099(3) 0.0000(2) 0.0031(3) -0.0012(2) Cl1 0.0161(3) 0.0111(2) 0.0186(4) 0.0019(2) -0.0009(3) -0.0033(2) O1 0.0119(7) 0.0140(8) 0.0174(8) 0.0027(9) 0.0058(6) 0.0046(8) O2 0.0137(9) 0.0136(7) 0.0121(9) -0.0016(7) 0.0028(7) -0.0029(6) O3 0.0089(9) 0.0170(8) 0.0209(11) -0.0005(8) 0.0039(8) -0.0007(7) O4 0.0124(9) 0.0132(7) 0.0134(10) 0.0039(7) 0.0050(8) 0.0011(6) O5 0.0122(8) 0.0112(6) 0.0114(9) -0.0017(6) 0.0037(7) -0.0041(6) O6 0.0095(9) 0.0128(7) 0.0195(10) 0.0014(7) 0.0035(7) -0.0011(6) C1 0.0122(13) 0.0093(10) 0.0249(17) 0.0004(10) 0.0058(12) -0.0015(9) C2 0.0113(11) 0.0117(9) 0.0135(12) 0.0004(9) 0.0022(10) 0.0017(8) C3 0.0096(11) 0.0113(9) 0.0141(12) 0.0006(9) 0.0041(9) 0.0015(8) C4 0.0100(11) 0.0103(8) 0.0136(12) -0.0007(8) 0.0055(9) 0.0001(8) C5 0.0136(13) 0.0151(10) 0.0165(14) 0.0011(10) 0.0078(11) -0.0008(9) C6 0.0155(12) 0.0138(10) 0.0216(14) 0.0045(10) 0.0106(11) 0.0015(9) C7 0.0163(12) 0.0098(9) 0.0267(15) -0.0005(10) 0.0117(11) -0.0013(8) C8 0.0108(11) 0.0118(9) 0.0179(13) -0.0011(9) 0.0045(10) 0.0005(8) C9 0.0115(11) 0.0140(9) 0.0118(12) -0.0021(9) 0.0047(10) -0.0007(8) C10 0.0140(12) 0.0144(9) 0.0161(13) -0.0017(9) 0.0073(10) 0.0010(9) C11 0.0100(10) 0.0161(15) 0.0175(11) -0.0002(9) 0.0053(9) 0.0020(8) C12 0.0104(11) 0.0150(9) 0.0126(12) 0.0023(9) 0.0038(9) 0.0026(8) C13 0.0110(12) 0.0196(10) 0.0118(12) 0.0005(9) 0.0029(10) 0.0023(8) C14 0.0103(11) 0.0161(10) 0.0160(13) -0.0017(9) 0.0034(10) 0.0005(8) C15 0.0182(13) 0.0195(10) 0.0146(13) 0.0006(10) 0.0084(11) -0.0008(9) C16 0.0182(15) 0.0218(13) 0.0282(18) -0.0016(12) 0.0065(13) 0.0049(11) C17 0.0167(12) 0.0262(11) 0.0136(12) 0.0056(9) 0.0070(10) 0.0028(9) C18 0.0160(13) 0.0205(11) 0.0185(14) -0.0030(10) 0.0022(11) -0.0056(9) C19 0.0118(11) 0.0112(9) 0.0086(11) 0.0022(8) 0.0026(9) 0.0014(8) C20 0.0129(11) 0.0125(8) 0.0093(11) -0.0006(8) 0.0022(9) -0.0020(8) C21 0.0131(12) 0.0123(9) 0.0126(13) 0.0004(8) 0.0048(10) -0.0009(8) C22 0.0131(12) 0.0116(9) 0.0131(12) -0.0018(9) 0.0061(10) -0.0014(8) C23 0.0122(12) 0.0128(9) 0.0203(14) -0.0022(9) 0.0081(10) 0.0000(8) C24 0.0116(12) 0.0125(9) 0.0166(13) 0.0019(9) 0.0060(10) -0.0002(8) C25 0.0157(12) 0.0189(10) 0.0138(13) -0.0005(9) 0.0072(10) -0.0009(9) C26 0.0164(12) 0.0178(15) 0.0161(12) -0.0029(9) 0.0051(10) -0.0054(8) C27 0.0179(13) 0.0177(10) 0.0152(13) -0.0033(9) 0.0095(11) -0.0049(9) C28 0.0154(14) 0.0165(11) 0.0291(18) 0.0059(11) 0.0042(13) 0.0058(10) C29 0.0235(17) 0.0276(13) 0.0273(18) -0.0026(13) 0.0142(14) 0.0004(12) Cl2 0.0278(4) 0.0282(3) 0.0347(4) -0.0075(3) 0.0147(3) -0.0048(3) Cl3 0.0375(5) 0.0516(4) 0.0358(5) -0.0210(4) 0.0211(4) -0.0081(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 C1 2.093(3) . ? Pt1 P1 2.2082(9) . ? Pt1 P2 2.3754(9) . ? Pt1 Cl1 2.3775(9) . ? P1 C2 1.838(2) . ? P1 C9 1.867(3) . ? P1 C12 1.889(3) . ? P2 C4 1.844(2) . ? P2 C19 1.887(3) . ? P2 C22 1.889(3) . ? O1 C11 1.439(3) . ? O1 C12 1.446(3) . ? O2 C14 1.431(3) . ? O2 C9 1.451(3) . ? O3 C11 1.429(3) . ? O3 C14 1.436(3) . ? O4 C24 1.437(3) . ? O4 C19 1.454(3) . ? O5 C21 1.429(3) . ? O5 C22 1.447(3) . ? O6 C24 1.430(3) . ? O6 C21 1.439(3) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C3 1.496(3) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C8 1.407(3) . ? C3 C4 1.415(3) . ? C4 C5 1.407(4) . ? C5 C6 1.393(3) . ? C5 H5 0.9500 . ? C6 C7 1.388(4) . ? C6 H6 0.9500 . ? C7 C8 1.374(4) . ? C7 H7 0.9500 . ? C8 H8 0.9500 . ? C9 C15 1.520(4) . ? C9 C10 1.533(3) . ? C10 C11 1.526(4) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C16 1.507(4) . ? C12 C17 1.508(4) . ? C12 C13 1.532(3) . ? C13 C14 1.526(4) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C18 1.510(3) . ? 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 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C25 1.514(4) . ? C19 C20 1.527(3) . ? C20 C21 1.512(4) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 C26 1.516(3) . ? C22 C27 1.510(4) . ? C22 C23 1.523(3) . ? C23 C24 1.527(4) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 C28 1.506(3) . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 Cl3 1.765(3) . ? C29 Cl2 1.775(3) . ? C29 H29A 0.9900 . ? C29 H29B 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 P1 90.96(9) . . ? C1 Pt1 P2 173.20(9) . . ? P1 Pt1 P2 93.27(4) . . ? C1 Pt1 Cl1 82.81(8) . . ? P1 Pt1 Cl1 166.87(3) . . ? P2 Pt1 Cl1 94.08(4) . . ? C2 P1 C9 108.51(12) . . ? C2 P1 C12 102.38(12) . . ? C9 P1 C12 94.10(12) . . ? C2 P1 Pt1 107.89(9) . . ? C9 P1 Pt1 121.49(8) . . ? C12 P1 Pt1 120.39(8) . . ? C4 P2 C19 104.45(11) . . ? C4 P2 C22 104.93(11) . . ? C19 P2 C22 93.35(12) . . ? C4 P2 Pt1 114.90(8) . . ? C19 P2 Pt1 117.68(8) . . ? C22 P2 Pt1 118.58(8) . . ? C11 O1 C12 115.2(2) . . ? C14 O2 C9 115.89(18) . . ? C11 O3 C14 111.17(19) . . ? C24 O4 C19 115.97(19) . . ? C21 O5 C22 116.42(18) . . ? C24 O6 C21 110.50(18) . . ? Pt1 C1 H1A 109.5 . . ? Pt1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? Pt1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C3 C2 P1 112.09(19) . . ? C3 C2 H2A 109.2 . . ? P1 C2 H2A 109.2 . . ? C3 C2 H2B 109.2 . . ? P1 C2 H2B 109.2 . . ? H2A C2 H2B 107.9 . . ? C8 C3 C4 119.3(2) . . ? C8 C3 C2 116.9(2) . . ? C4 C3 C2 123.7(2) . . ? C5 C4 C3 118.2(2) . . ? C5 C4 P2 123.13(19) . . ? C3 C4 P2 118.54(18) . . ? C6 C5 C4 121.1(3) . . ? C6 C5 H5 119.5 . . ? C4 C5 H5 119.5 . . ? C7 C6 C5 120.2(3) . . ? C7 C6 H6 119.9 . . ? C5 C6 H6 119.9 . . ? C8 C7 C6 119.7(2) . . ? C8 C7 H7 120.2 . . ? C6 C7 H7 120.2 . . ? C7 C8 C3 121.5(2) . . ? C7 C8 H8 119.3 . . ? C3 C8 H8 119.3 . . ? O2 C9 C15 106.76(19) . . ? O2 C9 C10 109.6(2) . . ? C15 C9 C10 111.0(2) . . ? O2 C9 P1 108.71(17) . . ? C15 C9 P1 114.20(18) . . ? C10 C9 P1 106.58(17) . . ? C11 C10 C9 111.0(2) . . ? C11 C10 H10A 109.4 . . ? C9 C10 H10A 109.4 . . ? C11 C10 H10B 109.4 . . ? C9 C10 H10B 109.4 . . ? H10A C10 H10B 108.0 . . ? O3 C11 O1 111.0(2) . . ? O3 C11 C16 107.4(2) . . ? O1 C11 C16 105.9(2) . . ? O3 C11 C10 108.04(19) . . ? O1 C11 C10 111.30(19) . . ? C16 C11 C10 113.2(2) . . ? O1 C12 C17 106.0(2) . . ? O1 C12 C13 106.3(2) . . ? C17 C12 C13 113.1(2) . . ? O1 C12 P1 110.57(17) . . ? C17 C12 P1 111.36(18) . . ? C13 C12 P1 109.37(16) . . ? C14 C13 C12 110.3(2) . . ? C14 C13 H13A 109.6 . . ? C12 C13 H13A 109.6 . . ? C14 C13 H13B 109.6 . . ? C12 C13 H13B 109.6 . . ? H13A C13 H13B 108.1 . . ? O2 C14 O3 110.3(2) . . ? O2 C14 C18 106.2(2) . . ? O3 C14 C18 107.1(2) . . ? O2 C14 C13 112.8(2) . . ? O3 C14 C13 107.4(2) . . ? C18 C14 C13 112.9(2) . . ? C9 C15 H15A 109.5 . . ? C9 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C9 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? 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 . . ? C12 C17 H17A 109.5 . . ? C12 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C12 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C14 C18 H18A 109.5 . . ? C14 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C14 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? O4 C19 C25 107.8(2) . . ? O4 C19 C20 105.93(19) . . ? C25 C19 C20 111.3(2) . . ? O4 C19 P2 110.86(16) . . ? C25 C19 P2 111.95(18) . . ? C20 C19 P2 108.85(17) . . ? C21 C20 C19 110.94(19) . . ? C21 C20 H20A 109.5 . . ? C19 C20 H20A 109.5 . . ? C21 C20 H20B 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 108.0 . . ? O5 C21 O6 110.36(18) . . ? O5 C21 C20 111.7(2) . . ? O6 C21 C20 108.4(2) . . ? O5 C21 C26 105.9(2) . . ? O6 C21 C26 106.60(19) . . ? C20 C21 C26 113.8(2) . . ? O5 C22 C27 105.3(2) . . ? O5 C22 C23 108.61(19) . . ? C27 C22 C23 112.7(2) . . ? O5 C22 P2 107.85(15) . . ? C27 C22 P2 113.14(18) . . ? C23 C22 P2 109.06(18) . . ? C22 C23 C24 110.53(19) . . ? C22 C23 H23A 109.5 . . ? C24 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? C24 C23 H23B 109.5 . . ? H23A C23 H23B 108.1 . . ? O6 C24 O4 110.15(19) . . ? O6 C24 C28 107.9(2) . . ? O4 C24 C28 105.7(2) . . ? O6 C24 C23 107.6(2) . . ? O4 C24 C23 112.8(2) . . ? C28 C24 C23 112.7(2) . . ? C19 C25 H25A 109.5 . . ? C19 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C19 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C21 C26 H26A 109.5 . . ? C21 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C21 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C22 C27 H27A 109.5 . . ? C22 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C22 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C24 C28 H28A 109.5 . . ? C24 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C24 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? Cl3 C29 Cl2 110.60(18) . . ? Cl3 C29 H29A 109.5 . . ? Cl2 C29 H29A 109.5 . . ? Cl3 C29 H29B 109.5 . . ? Cl2 C29 H29B 109.5 . . ? H29A C29 H29B 108.1 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 Pt1 P1 C2 -155.82(14) . . . . ? P2 Pt1 P1 C2 29.49(10) . . . . ? Cl1 Pt1 P1 C2 -94.46(15) . . . . ? C1 Pt1 P1 C9 78.09(13) . . . . ? P2 Pt1 P1 C9 -96.59(9) . . . . ? Cl1 Pt1 P1 C9 139.46(14) . . . . ? C1 Pt1 P1 C12 -39.06(13) . . . . ? P2 Pt1 P1 C12 146.26(10) . . . . ? Cl1 Pt1 P1 C12 22.31(17) . . . . ? C1 Pt1 P2 C4 -111.6(7) . . . . ? P1 Pt1 P2 C4 16.88(10) . . . . ? Cl1 Pt1 P2 C4 -174.01(10) . . . . ? C1 Pt1 P2 C19 12.1(7) . . . . ? P1 Pt1 P2 C19 140.53(10) . . . . ? Cl1 Pt1 P2 C19 -50.36(10) . . . . ? C1 Pt1 P2 C22 123.2(7) . . . . ? P1 Pt1 P2 C22 -108.31(9) . . . . ? Cl1 Pt1 P2 C22 60.80(9) . . . . ? C9 P1 C2 C3 56.3(2) . . . . ? C12 P1 C2 C3 154.97(18) . . . . ? Pt1 P1 C2 C3 -77.08(18) . . . . ? P1 C2 C3 C8 -113.7(2) . . . . ? P1 C2 C3 C4 63.6(3) . . . . ? C8 C3 C4 C5 2.5(4) . . . . ? C2 C3 C4 C5 -174.7(3) . . . . ? C8 C3 C4 P2 178.40(19) . . . . ? C2 C3 C4 P2 1.1(3) . . . . ? C19 P2 C4 C5 4.6(3) . . . . ? C22 P2 C4 C5 -92.9(2) . . . . ? Pt1 P2 C4 C5 135.0(2) . . . . ? C19 P2 C4 C3 -171.1(2) . . . . ? C22 P2 C4 C3 91.4(2) . . . . ? Pt1 P2 C4 C3 -40.6(2) . . . . ? C3 C4 C5 C6 -1.6(4) . . . . ? P2 C4 C5 C6 -177.3(2) . . . . ? C4 C5 C6 C7 -0.1(4) . . . . ? C5 C6 C7 C8 1.0(4) . . . . ? C6 C7 C8 C3 0.0(4) . . . . ? C4 C3 C8 C7 -1.8(4) . . . . ? C2 C3 C8 C7 175.7(2) . . . . ? C14 O2 C9 C15 -168.9(2) . . . . ? C14 O2 C9 C10 -48.7(3) . . . . ? C14 O2 C9 P1 67.4(2) . . . . ? C2 P1 C9 O2 46.20(18) . . . . ? C12 P1 C9 O2 -58.32(16) . . . . ? Pt1 P1 C9 O2 172.00(11) . . . . ? C2 P1 C9 C15 -72.88(19) . . . . ? C12 P1 C9 C15 -177.39(17) . . . . ? Pt1 P1 C9 C15 52.92(19) . . . . ? C2 P1 C9 C10 164.23(17) . . . . ? C12 P1 C9 C10 59.72(18) . . . . ? Pt1 P1 C9 C10 -69.97(18) . . . . ? O2 C9 C10 C11 48.5(3) . . . . ? C15 C9 C10 C11 166.1(2) . . . . ? P1 C9 C10 C11 -69.0(2) . . . . ? C14 O3 C11 O1 -59.3(3) . . . . ? C14 O3 C11 C16 -174.6(2) . . . . ? C14 O3 C11 C10 63.0(3) . . . . ? C12 O1 C11 O3 57.1(3) . . . . ? C12 O1 C11 C16 173.3(2) . . . . ? C12 O1 C11 C10 -63.3(2) . . . . ? C9 C10 C11 O3 -56.3(3) . . . . ? C9 C10 C11 O1 65.8(3) . . . . ? C9 C10 C11 C16 -175.1(2) . . . . ? C11 O1 C12 C17 -175.0(2) . . . . ? C11 O1 C12 C13 -54.5(3) . . . . ? C11 O1 C12 P1 64.1(2) . . . . ? C2 P1 C12 O1 -167.80(17) . . . . ? C9 P1 C12 O1 -57.82(18) . . . . ? Pt1 P1 C12 O1 72.65(19) . . . . ? C2 P1 C12 C17 74.6(2) . . . . ? C9 P1 C12 C17 -175.39(18) . . . . ? Pt1 P1 C12 C17 -44.9(2) . . . . ? C2 P1 C12 C13 -51.1(2) . . . . ? C9 P1 C12 C13 58.91(19) . . . . ? Pt1 P1 C12 C13 -170.62(14) . . . . ? O1 C12 C13 C14 55.7(3) . . . . ? C17 C12 C13 C14 171.6(2) . . . . ? P1 C12 C13 C14 -63.7(2) . . . . ? C9 O2 C14 O3 55.1(3) . . . . ? C9 O2 C14 C18 170.8(2) . . . . ? C9 O2 C14 C13 -65.0(3) . . . . ? C11 O3 C14 O2 -62.0(3) . . . . ? C11 O3 C14 C18 -177.2(2) . . . . ? C11 O3 C14 C13 61.2(3) . . . . ? C12 C13 C14 O2 61.3(2) . . . . ? C12 C13 C14 O3 -60.5(3) . . . . ? C12 C13 C14 C18 -178.3(2) . . . . ? C24 O4 C19 C25 173.3(2) . . . . ? C24 O4 C19 C20 54.1(3) . . . . ? C24 O4 C19 P2 -63.9(2) . . . . ? C4 P2 C19 O4 -49.7(2) . . . . ? C22 P2 C19 O4 56.68(18) . . . . ? Pt1 P2 C19 O4 -178.44(13) . . . . ? C4 P2 C19 C25 70.78(17) . . . . ? C22 P2 C19 C25 177.13(16) . . . . ? Pt1 P2 C19 C25 -57.99(17) . . . . ? C4 P2 C19 C20 -165.82(16) . . . . ? C22 P2 C19 C20 -59.46(17) . . . . ? Pt1 P2 C19 C20 65.42(18) . . . . ? O4 C19 C20 C21 -53.9(3) . . . . ? C25 C19 C20 C21 -170.8(2) . . . . ? P2 C19 C20 C21 65.4(2) . . . . ? C22 O5 C21 O6 -54.9(3) . . . . ? C22 O5 C21 C20 65.7(2) . . . . ? C22 O5 C21 C26 -169.90(19) . . . . ? C24 O6 C21 O5 61.1(3) . . . . ? C24 O6 C21 C20 -61.5(3) . . . . ? C24 O6 C21 C26 175.7(2) . . . . ? C19 C20 C21 O5 -62.1(2) . . . . ? C19 C20 C21 O6 59.7(3) . . . . ? C19 C20 C21 C26 178.1(2) . . . . ? C21 O5 C22 C27 170.73(19) . . . . ? C21 O5 C22 C23 49.9(3) . . . . ? C21 O5 C22 P2 -68.2(2) . . . . ? C4 P2 C22 O5 164.51(16) . . . . ? C19 P2 C22 O5 58.59(17) . . . . ? Pt1 P2 C22 O5 -65.58(17) . . . . ? C4 P2 C22 C27 -79.49(18) . . . . ? C19 P2 C22 C27 174.59(16) . . . . ? Pt1 P2 C22 C27 50.41(18) . . . . ? C4 P2 C22 C23 46.73(19) . . . . ? C19 P2 C22 C23 -59.19(17) . . . . ? Pt1 P2 C22 C23 176.63(13) . . . . ? O5 C22 C23 C24 -50.7(3) . . . . ? C27 C22 C23 C24 -166.9(2) . . . . ? P2 C22 C23 C24 66.6(2) . . . . ? C21 O6 C24 O4 59.7(3) . . . . ? C21 O6 C24 C28 174.6(2) . . . . ? C21 O6 C24 C23 -63.6(2) . . . . ? C19 O4 C24 O6 -58.1(3) . . . . ? C19 O4 C24 C28 -174.33(19) . . . . ? C19 O4 C24 C23 62.2(2) . . . . ? C22 C23 C24 O6 59.0(3) . . . . ? C22 C23 C24 O4 -62.7(3) . . . . ? C22 C23 C24 C28 177.7(2) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 30.52 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.666 _refine_diff_density_min -0.920 _refine_diff_density_rms 0.087 data_2b_Pd _database_code_depnum_ccdc_archive 'CCDC 897398' #TrackingRef '- all.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C25 H40 Cl2 O3 P2 Pd' _chemical_formula_sum 'C25 H40 Cl2 O3 P2 Pd' _chemical_formula_weight 627.81 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.7707(11) _cell_length_b 15.2847(14) _cell_length_c 15.9116(15) _cell_angle_alpha 90.00 _cell_angle_beta 103.716(2) _cell_angle_gamma 90.00 _cell_volume 2781.0(4) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 920 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 27.4 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.499 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1296 _exptl_absorpt_coefficient_mu 0.999 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.804 _exptl_absorpt_correction_T_max 0.950 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1998)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'CCD area detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 18043 _diffrn_reflns_av_R_equivalents 0.0398 _diffrn_reflns_av_sigmaI/netI 0.0556 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.22 _diffrn_reflns_theta_max 27.48 _reflns_number_total 6349 _reflns_number_gt 4719 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0383P)^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 6349 _refine_ls_number_parameters 308 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0495 _refine_ls_R_factor_gt 0.0297 _refine_ls_wR_factor_ref 0.0679 _refine_ls_wR_factor_gt 0.0627 _refine_ls_goodness_of_fit_ref 0.829 _refine_ls_restrained_S_all 0.829 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.133988(16) 0.912907(11) 0.246245(13) 0.01841(6) Uani 1 1 d . . . P1 P -0.03026(6) 0.83733(4) 0.18163(4) 0.01914(14) Uani 1 1 d . . . P2 P 0.25478(6) 0.79304(4) 0.25705(4) 0.01937(14) Uani 1 1 d . . . Cl1 Cl 0.25512(6) 1.00333(4) 0.35304(5) 0.03473(17) Uani 1 1 d . . . Cl2 Cl 0.03765(6) 1.04166(4) 0.19301(5) 0.03510(17) Uani 1 1 d . . . O1 O 0.37646(16) 0.78918(11) 0.42380(12) 0.0301(4) Uani 1 1 d . . . O2 O 0.47606(15) 0.74372(11) 0.24783(13) 0.0282(4) Uani 1 1 d . . . O3 O 0.55636(16) 0.74372(12) 0.39792(14) 0.0364(5) Uani 1 1 d . . . C1 C -0.0034(2) 0.71976(15) 0.20045(17) 0.0202(5) Uani 1 1 d . . . H1A H 0.0222 0.7098 0.2636 0.024 Uiso 1 1 calc R . . H1B H -0.0782 0.6883 0.1794 0.024 Uiso 1 1 calc R . . C2 C 0.0864(2) 0.68026(15) 0.15802(16) 0.0204(5) Uani 1 1 d . . . C3 C 0.2027(2) 0.70950(15) 0.17359(16) 0.0202(5) Uani 1 1 d . . . C4 C 0.2749(2) 0.67358(17) 0.12360(17) 0.0265(6) Uani 1 1 d . . . H4 H 0.3534 0.6934 0.1323 0.032 Uiso 1 1 calc R . . C5 C 0.2340(3) 0.60992(17) 0.06188(19) 0.0319(7) Uani 1 1 d . . . H5 H 0.2832 0.5881 0.0272 0.038 Uiso 1 1 calc R . . C6 C 0.1225(3) 0.57847(17) 0.05091(18) 0.0313(6) Uani 1 1 d . . . H6 H 0.0955 0.5331 0.0103 0.038 Uiso 1 1 calc R . . C7 C 0.0494(2) 0.61251(16) 0.09863(17) 0.0265(6) Uani 1 1 d . . . H7 H -0.0274 0.5896 0.0911 0.032 Uiso 1 1 calc R . . C8 C -0.0897(2) 0.84990(17) 0.06164(17) 0.0262(6) Uani 1 1 d . . . C9 C 0.0166(3) 0.8522(2) 0.02235(19) 0.0415(8) Uani 1 1 d . . . H9A H 0.0595 0.7969 0.0345 0.062 Uiso 1 1 calc R . . H9B H 0.0678 0.9007 0.0476 0.062 Uiso 1 1 calc R . . H9C H -0.0093 0.8604 -0.0404 0.062 Uiso 1 1 calc R . . C10 C -0.1688(3) 0.77259(19) 0.0237(2) 0.0444(8) Uani 1 1 d . . . H10A H -0.1952 0.7796 -0.0392 0.067 Uiso 1 1 calc R . . H10B H -0.2367 0.7710 0.0493 0.067 Uiso 1 1 calc R . . H10C H -0.1248 0.7178 0.0367 0.067 Uiso 1 1 calc R . . C11 C -0.1611(3) 0.93383(18) 0.0349(2) 0.0403(8) Uani 1 1 d . . . H11A H -0.1183 0.9840 0.0653 0.060 Uiso 1 1 calc R . . H11B H -0.2368 0.9286 0.0501 0.060 Uiso 1 1 calc R . . H11C H -0.1737 0.9424 -0.0276 0.060 Uiso 1 1 calc R . . C12 C -0.1431(2) 0.85703(17) 0.2475(2) 0.0301(6) Uani 1 1 d . . . C13 C -0.2355(3) 0.7868(2) 0.2322(3) 0.0917(19) Uani 1 1 d . . . H13A H -0.2917 0.7989 0.2674 0.138 Uiso 1 1 calc R . . H13B H -0.1986 0.7298 0.2485 0.138 Uiso 1 1 calc R . . H13C H -0.2762 0.7861 0.1709 0.138 Uiso 1 1 calc R . . C14 C -0.2032(3) 0.9457(2) 0.2326(2) 0.0489(9) Uani 1 1 d . . . H14A H -0.2531 0.9480 0.1738 0.073 Uiso 1 1 calc R . . H14B H -0.1440 0.9919 0.2398 0.073 Uiso 1 1 calc R . . H14C H -0.2512 0.9542 0.2745 0.073 Uiso 1 1 calc R . . C15 C -0.0753(3) 0.8555(3) 0.3426(2) 0.0731(14) Uani 1 1 d . . . H15A H -0.1285 0.8693 0.3797 0.110 Uiso 1 1 calc R . . H15B H -0.0124 0.8989 0.3517 0.110 Uiso 1 1 calc R . . H15C H -0.0418 0.7972 0.3571 0.110 Uiso 1 1 calc R . . C16 C 0.3088(2) 0.73018(16) 0.36148(17) 0.0234(6) Uani 1 1 d . . . C17 C 0.3881(2) 0.65610(16) 0.34439(18) 0.0260(6) Uani 1 1 d . . . H17A H 0.4079 0.6172 0.3955 0.031 Uiso 1 1 calc R . . H17B H 0.3459 0.6210 0.2944 0.031 Uiso 1 1 calc R . . C18 C 0.4999(2) 0.69234(17) 0.32575(19) 0.0296(6) Uani 1 1 d . . . C19 C 0.4086(2) 0.82265(16) 0.2483(2) 0.0284(6) Uani 1 1 d . . . C20 C 0.4683(2) 0.87452(17) 0.3289(2) 0.0342(7) Uani 1 1 d . . . H20A H 0.5449 0.8963 0.3223 0.041 Uiso 1 1 calc R . . H20B H 0.4195 0.9258 0.3352 0.041 Uiso 1 1 calc R . . C21 C 0.4863(2) 0.81805(18) 0.4095(2) 0.0366(7) Uani 1 1 d . . . C22 C 0.2120(2) 0.69789(18) 0.40029(17) 0.0286(6) Uani 1 1 d . . . H22A H 0.2455 0.6716 0.4569 0.043 Uiso 1 1 calc R . . H22B H 0.1658 0.6540 0.3620 0.043 Uiso 1 1 calc R . . H22C H 0.1615 0.7470 0.4072 0.043 Uiso 1 1 calc R . . C23 C 0.5835(2) 0.62154(18) 0.3134(2) 0.0394(8) Uani 1 1 d . . . H23A H 0.6554 0.6482 0.3045 0.059 Uiso 1 1 calc R . . H23B H 0.5472 0.5862 0.2628 0.059 Uiso 1 1 calc R . . H23C H 0.6021 0.5842 0.3649 0.059 Uiso 1 1 calc R . . C24 C 0.4069(3) 0.87169(19) 0.1656(2) 0.0394(8) Uani 1 1 d . . . H24A H 0.4873 0.8850 0.1625 0.059 Uiso 1 1 calc R . . H24B H 0.3630 0.9263 0.1647 0.059 Uiso 1 1 calc R . . H24C H 0.3694 0.8355 0.1159 0.059 Uiso 1 1 calc R . . C25 C 0.5484(3) 0.8639(2) 0.4903(2) 0.0524(10) Uani 1 1 d . . . H25A H 0.5031 0.9152 0.4997 0.079 Uiso 1 1 calc R . . H25B H 0.6260 0.8825 0.4847 0.079 Uiso 1 1 calc R . . H25C H 0.5569 0.8239 0.5396 0.079 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 Pd1 0.01880(10) 0.01450(9) 0.02039(11) -0.00123(8) 0.00157(7) -0.00024(8) P1 0.0174(3) 0.0180(3) 0.0210(4) 0.0007(3) 0.0025(3) -0.0002(3) P2 0.0163(3) 0.0162(3) 0.0243(4) -0.0011(3) 0.0024(3) -0.0014(2) Cl1 0.0312(4) 0.0272(3) 0.0393(4) -0.0126(3) -0.0044(3) -0.0015(3) Cl2 0.0416(4) 0.0191(3) 0.0381(4) -0.0001(3) -0.0034(3) 0.0078(3) O1 0.0262(10) 0.0289(10) 0.0291(11) -0.0113(8) -0.0059(8) 0.0002(8) O2 0.0190(10) 0.0218(9) 0.0442(13) 0.0008(9) 0.0084(9) 0.0033(7) O3 0.0218(10) 0.0290(10) 0.0497(14) -0.0113(10) -0.0090(9) 0.0050(8) C1 0.0170(13) 0.0187(12) 0.0233(14) 0.0007(10) 0.0018(10) -0.0022(10) C2 0.0232(13) 0.0156(12) 0.0217(14) 0.0031(10) 0.0036(11) 0.0010(10) C3 0.0210(13) 0.0187(12) 0.0202(14) 0.0007(10) 0.0034(11) -0.0004(10) C4 0.0256(14) 0.0275(14) 0.0270(15) 0.0006(12) 0.0073(12) -0.0009(11) C5 0.0391(17) 0.0309(15) 0.0286(16) -0.0042(12) 0.0138(14) 0.0036(13) C6 0.0441(17) 0.0227(14) 0.0257(15) -0.0061(12) 0.0056(13) -0.0015(13) C7 0.0288(15) 0.0199(13) 0.0285(16) -0.0023(11) 0.0020(12) -0.0055(11) C8 0.0260(15) 0.0273(14) 0.0206(14) 0.0013(11) -0.0039(11) -0.0013(11) C9 0.0441(19) 0.059(2) 0.0221(16) 0.0073(15) 0.0088(14) 0.0052(16) C10 0.047(2) 0.0367(17) 0.0374(19) -0.0015(14) -0.0145(15) -0.0048(14) C11 0.0484(19) 0.0351(17) 0.0292(17) 0.0032(13) -0.0075(14) 0.0078(14) C12 0.0259(15) 0.0291(14) 0.0399(18) 0.0040(13) 0.0167(13) 0.0051(12) C13 0.070(3) 0.059(3) 0.178(5) -0.044(3) 0.095(4) -0.029(2) C14 0.050(2) 0.0450(19) 0.061(2) 0.0114(17) 0.0309(19) 0.0218(16) C15 0.063(3) 0.126(4) 0.038(2) 0.020(2) 0.028(2) 0.048(3) C16 0.0221(14) 0.0210(13) 0.0230(14) -0.0036(11) -0.0028(11) -0.0005(10) C17 0.0254(14) 0.0194(13) 0.0290(16) -0.0018(11) -0.0017(12) 0.0011(11) C18 0.0221(14) 0.0231(14) 0.0393(18) -0.0028(12) -0.0015(12) 0.0052(11) C19 0.0185(13) 0.0191(13) 0.0476(19) 0.0007(12) 0.0075(12) 0.0003(11) C20 0.0181(14) 0.0202(13) 0.062(2) -0.0070(14) 0.0049(14) -0.0040(11) C21 0.0194(14) 0.0296(15) 0.054(2) -0.0136(14) -0.0037(14) 0.0018(12) C22 0.0306(15) 0.0331(15) 0.0201(15) 0.0022(12) 0.0019(12) -0.0012(12) C23 0.0288(16) 0.0260(14) 0.060(2) -0.0031(15) 0.0041(15) 0.0062(12) C24 0.0332(17) 0.0279(15) 0.061(2) 0.0128(15) 0.0181(16) -0.0040(13) C25 0.0307(18) 0.0417(19) 0.072(3) -0.0273(18) -0.0131(17) 0.0024(14) _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 Pd1 P1 2.2775(7) . ? Pd1 P2 2.3004(7) . ? Pd1 Cl2 2.3282(7) . ? Pd1 Cl1 2.3837(7) . ? P1 C1 1.837(2) . ? P1 C8 1.881(3) . ? P1 C12 1.901(3) . ? P2 C3 1.839(3) . ? P2 C16 1.894(3) . ? P2 C19 1.903(3) . ? O1 C16 1.434(3) . ? O1 C21 1.435(3) . ? O2 C18 1.438(3) . ? O2 C19 1.445(3) . ? O3 C18 1.419(3) . ? O3 C21 1.441(3) . ? C1 C2 1.509(3) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C7 1.400(3) . ? C2 C3 1.405(3) . ? C3 C4 1.406(3) . ? C4 C5 1.385(4) . ? C4 H4 0.9500 . ? C5 C6 1.369(4) . ? C5 H5 0.9500 . ? C6 C7 1.377(4) . ? C6 H6 0.9500 . ? C7 H7 0.9500 . ? C8 C9 1.526(4) . ? C8 C10 1.536(4) . ? C8 C11 1.537(4) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C13 1.506(4) . ? C12 C14 1.520(4) . ? C12 C15 1.534(5) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C22 1.502(4) . ? C16 C17 1.532(3) . ? C17 C18 1.521(4) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C23 1.506(4) . ? C19 C24 1.511(4) . ? C19 C20 1.530(4) . ? C20 C21 1.518(4) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 C25 1.495(4) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P1 Pd1 P2 94.20(2) . . ? P1 Pd1 Cl2 88.65(3) . . ? P2 Pd1 Cl2 159.96(3) . . ? P1 Pd1 Cl1 156.38(3) . . ? P2 Pd1 Cl1 98.85(2) . . ? Cl2 Pd1 Cl1 85.80(3) . . ? C1 P1 C8 105.88(12) . . ? C1 P1 C12 100.42(11) . . ? C8 P1 C12 113.77(13) . . ? C1 P1 Pd1 109.13(8) . . ? C8 P1 Pd1 118.56(8) . . ? C12 P1 Pd1 107.47(10) . . ? C3 P2 C16 105.44(11) . . ? C3 P2 C19 105.80(12) . . ? C16 P2 C19 93.31(12) . . ? C3 P2 Pd1 113.87(8) . . ? C16 P2 Pd1 122.85(8) . . ? C19 P2 Pd1 112.77(8) . . ? C16 O1 C21 117.2(2) . . ? C18 O2 C19 116.5(2) . . ? C18 O3 C21 111.6(2) . . ? C2 C1 P1 115.49(17) . . ? C2 C1 H1A 108.4 . . ? P1 C1 H1A 108.4 . . ? C2 C1 H1B 108.4 . . ? P1 C1 H1B 108.4 . . ? H1A C1 H1B 107.5 . . ? C7 C2 C3 119.3(2) . . ? C7 C2 C1 117.3(2) . . ? C3 C2 C1 123.4(2) . . ? C2 C3 C4 118.1(2) . . ? C2 C3 P2 119.49(18) . . ? C4 C3 P2 122.44(19) . . ? C5 C4 C3 121.3(3) . . ? C5 C4 H4 119.4 . . ? C3 C4 H4 119.4 . . ? C6 C5 C4 119.9(3) . . ? C6 C5 H5 120.0 . . ? C4 C5 H5 120.0 . . ? C5 C6 C7 120.1(3) . . ? C5 C6 H6 119.9 . . ? C7 C6 H6 119.9 . . ? C6 C7 C2 121.1(2) . . ? C6 C7 H7 119.5 . . ? C2 C7 H7 119.5 . . ? C9 C8 C10 109.6(2) . . ? C9 C8 C11 108.4(2) . . ? C10 C8 C11 107.0(2) . . ? C9 C8 P1 105.93(18) . . ? C10 C8 P1 111.43(19) . . ? C11 C8 P1 114.40(19) . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C8 C10 H10A 109.5 . . ? C8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C8 C11 H11A 109.5 . . ? C8 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C8 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C13 C12 C14 108.6(3) . . ? C13 C12 C15 109.6(3) . . ? C14 C12 C15 106.4(3) . . ? C13 C12 P1 111.7(2) . . ? C14 C12 P1 114.5(2) . . ? C15 C12 P1 105.8(2) . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C12 C15 H15A 109.5 . . ? C12 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C12 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? O1 C16 C22 105.9(2) . . ? O1 C16 C17 109.0(2) . . ? C22 C16 C17 112.5(2) . . ? O1 C16 P2 107.67(16) . . ? C22 C16 P2 113.44(18) . . ? C17 C16 P2 108.12(18) . . ? C18 C17 C16 110.9(2) . . ? C18 C17 H17A 109.5 . . ? C16 C17 H17A 109.5 . . ? C18 C17 H17B 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 108.0 . . ? O3 C18 O2 110.7(2) . . ? O3 C18 C23 108.0(2) . . ? O2 C18 C23 106.3(2) . . ? O3 C18 C17 107.7(2) . . ? O2 C18 C17 111.5(2) . . ? C23 C18 C17 112.7(2) . . ? O2 C19 C24 107.6(2) . . ? O2 C19 C20 107.0(2) . . ? C24 C19 C20 112.5(2) . . ? O2 C19 P2 109.60(16) . . ? C24 C19 P2 111.5(2) . . ? C20 C19 P2 108.52(19) . . ? C21 C20 C19 111.0(2) . . ? C21 C20 H20A 109.4 . . ? C19 C20 H20A 109.4 . . ? C21 C20 H20B 109.4 . . ? C19 C20 H20B 109.4 . . ? H20A C20 H20B 108.0 . . ? O1 C21 O3 110.0(2) . . ? O1 C21 C25 106.4(3) . . ? O3 C21 C25 107.6(2) . . ? O1 C21 C20 111.0(2) . . ? O3 C21 C20 108.1(2) . . ? C25 C21 C20 113.7(3) . . ? C16 C22 H22A 109.5 . . ? C16 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C16 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C18 C23 H23A 109.5 . . ? C18 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C18 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C19 C24 H24A 109.5 . . ? C19 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C19 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C21 C25 H25A 109.5 . . ? C21 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C21 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag P2 Pd1 P1 C1 18.26(9) . . . . ? Cl2 Pd1 P1 C1 178.39(9) . . . . ? Cl1 Pd1 P1 C1 -105.32(10) . . . . ? P2 Pd1 P1 C8 -102.98(10) . . . . ? Cl2 Pd1 P1 C8 57.16(10) . . . . ? Cl1 Pd1 P1 C8 133.45(11) . . . . ? P2 Pd1 P1 C12 126.30(9) . . . . ? Cl2 Pd1 P1 C12 -73.56(9) . . . . ? Cl1 Pd1 P1 C12 2.73(12) . . . . ? P1 Pd1 P2 C3 27.42(9) . . . . ? Cl2 Pd1 P2 C3 -70.18(12) . . . . ? Cl1 Pd1 P2 C3 -172.33(9) . . . . ? P1 Pd1 P2 C16 -101.81(10) . . . . ? Cl2 Pd1 P2 C16 160.59(11) . . . . ? Cl1 Pd1 P2 C16 58.44(10) . . . . ? P1 Pd1 P2 C19 147.98(11) . . . . ? Cl2 Pd1 P2 C19 50.39(13) . . . . ? Cl1 Pd1 P2 C19 -51.76(11) . . . . ? C8 P1 C1 C2 62.6(2) . . . . ? C12 P1 C1 C2 -178.83(19) . . . . ? Pd1 P1 C1 C2 -66.1(2) . . . . ? P1 C1 C2 C7 -120.1(2) . . . . ? P1 C1 C2 C3 58.3(3) . . . . ? C7 C2 C3 C4 4.7(4) . . . . ? C1 C2 C3 C4 -173.6(2) . . . . ? C7 C2 C3 P2 -175.71(19) . . . . ? C1 C2 C3 P2 6.0(3) . . . . ? C16 P2 C3 C2 88.1(2) . . . . ? C19 P2 C3 C2 -173.8(2) . . . . ? Pd1 P2 C3 C2 -49.4(2) . . . . ? C16 P2 C3 C4 -92.3(2) . . . . ? C19 P2 C3 C4 5.7(2) . . . . ? Pd1 P2 C3 C4 130.1(2) . . . . ? C2 C3 C4 C5 -1.3(4) . . . . ? P2 C3 C4 C5 179.2(2) . . . . ? C3 C4 C5 C6 -2.5(4) . . . . ? C4 C5 C6 C7 2.7(4) . . . . ? C5 C6 C7 C2 0.9(4) . . . . ? C3 C2 C7 C6 -4.6(4) . . . . ? C1 C2 C7 C6 173.8(2) . . . . ? C1 P1 C8 C9 -83.1(2) . . . . ? C12 P1 C8 C9 167.63(18) . . . . ? Pd1 P1 C8 C9 39.8(2) . . . . ? C1 P1 C8 C10 36.1(2) . . . . ? C12 P1 C8 C10 -73.2(2) . . . . ? Pd1 P1 C8 C10 158.97(17) . . . . ? C1 P1 C8 C11 157.6(2) . . . . ? C12 P1 C8 C11 48.3(2) . . . . ? Pd1 P1 C8 C11 -79.5(2) . . . . ? C1 P1 C12 C13 -44.8(3) . . . . ? C8 P1 C12 C13 67.8(3) . . . . ? Pd1 P1 C12 C13 -158.8(3) . . . . ? C1 P1 C12 C14 -168.8(2) . . . . ? C8 P1 C12 C14 -56.1(3) . . . . ? Pd1 P1 C12 C14 77.2(2) . . . . ? C1 P1 C12 C15 74.4(2) . . . . ? C8 P1 C12 C15 -173.0(2) . . . . ? Pd1 P1 C12 C15 -39.6(2) . . . . ? C21 O1 C16 C22 169.6(2) . . . . ? C21 O1 C16 C17 48.3(3) . . . . ? C21 O1 C16 P2 -68.8(2) . . . . ? C3 P2 C16 O1 165.79(16) . . . . ? C19 P2 C16 O1 58.40(18) . . . . ? Pd1 P2 C16 O1 -61.52(18) . . . . ? C3 P2 C16 C22 -77.4(2) . . . . ? C19 P2 C16 C22 175.19(19) . . . . ? Pd1 P2 C16 C22 55.3(2) . . . . ? C3 P2 C16 C17 48.15(19) . . . . ? C19 P2 C16 C17 -59.24(18) . . . . ? Pd1 P2 C16 C17 -179.15(13) . . . . ? O1 C16 C17 C18 -49.4(3) . . . . ? C22 C16 C17 C18 -166.5(2) . . . . ? P2 C16 C17 C18 67.4(2) . . . . ? C21 O3 C18 O2 58.7(3) . . . . ? C21 O3 C18 C23 174.7(2) . . . . ? C21 O3 C18 C17 -63.4(3) . . . . ? C19 O2 C18 O3 -55.7(3) . . . . ? C19 O2 C18 C23 -172.7(2) . . . . ? C19 O2 C18 C17 64.2(3) . . . . ? C16 C17 C18 O3 57.9(3) . . . . ? C16 C17 C18 O2 -63.8(3) . . . . ? C16 C17 C18 C23 176.8(2) . . . . ? C18 O2 C19 C24 173.0(2) . . . . ? C18 O2 C19 C20 51.9(3) . . . . ? C18 O2 C19 P2 -65.6(3) . . . . ? C3 P2 C19 O2 -49.8(2) . . . . ? C16 P2 C19 O2 57.3(2) . . . . ? Pd1 P2 C19 O2 -174.90(15) . . . . ? C3 P2 C19 C24 69.2(2) . . . . ? C16 P2 C19 C24 176.3(2) . . . . ? Pd1 P2 C19 C24 -55.8(2) . . . . ? C3 P2 C19 C20 -166.39(18) . . . . ? C16 P2 C19 C20 -59.32(19) . . . . ? Pd1 P2 C19 C20 68.5(2) . . . . ? O2 C19 C20 C21 -52.6(3) . . . . ? C24 C19 C20 C21 -170.6(2) . . . . ? P2 C19 C20 C21 65.6(2) . . . . ? C16 O1 C21 O3 -53.3(3) . . . . ? C16 O1 C21 C25 -169.5(2) . . . . ? C16 O1 C21 C20 66.3(3) . . . . ? C18 O3 C21 O1 60.2(3) . . . . ? C18 O3 C21 C25 175.7(3) . . . . ? C18 O3 C21 C20 -61.1(3) . . . . ? C19 C20 C21 O1 -62.2(3) . . . . ? C19 C20 C21 O3 58.5(3) . . . . ? C19 C20 C21 C25 177.8(2) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.494 _refine_diff_density_min -0.461 _refine_diff_density_rms 0.077