Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Ola Wendt' _publ_contact_author_address ; Organic Chemistry, Department of Chemistry Lund University PO Box 124 Lund 221 00 SWEDEN ; _publ_contact_author_email OLA.WENDT@ORGANIC.LU.SE _publ_section_title ; Synthesis and characterisation of PCsp3P phosphine and phosphinite platinum (II) complexes. Cyclometallation and simple coordination ; loop_ _publ_author_name 'Daniel Olsson' 'Athimoolam Arunachalampillai' 'Ola F. Wendt' data_complex5 _database_code_depnum_ccdc_archive 'CCDC 657410' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H38 Cl2 O2 P2 Pt' _chemical_formula_weight 614.41 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 orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 12.8734(8) _cell_length_b 14.8662(9) _cell_length_c 24.0444(13) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4601.6(5) _cell_formula_units_Z 8 _cell_measurement_temperature 150(3) _cell_measurement_reflns_used 6827 _cell_measurement_theta_min 2.1717 _cell_measurement_theta_max 32.7710 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.774 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2432 _exptl_absorpt_coefficient_mu 6.480 _exptl_absorpt_correction_T_min 0.42775 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.5 (release 28-08-2006 CrysAlis171 .NET) (compiled Aug 28 2006,13:05:05) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _diffrn_ambient_temperature 150(3) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Xcalibur3' _diffrn_measurement_method \w-scan _diffrn_detector_area_resol_mean 16.1829 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.0 _diffrn_reflns_number 43390 _diffrn_reflns_av_R_equivalents 0.1426 _diffrn_reflns_av_sigmaI/netI 0.1697 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 2.26 _diffrn_reflns_theta_max 32.89 _reflns_number_total 8030 _reflns_number_gt 3388 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.26 beta (release 01-03-2005 CrysAlis171 .NET) (compiled Mar 2 2005,09:02:11) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.26 beta (release 01-03-2005 CrysAlis171 .NET) (compiled Mar 2 2005,09:02:11) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.26 beta (release 01-03-2005 CrysAlis171 .NET) (compiled Mar 2 2005,09:02:11) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0589P)^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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8030 _refine_ls_number_parameters 226 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1444 _refine_ls_R_factor_gt 0.0607 _refine_ls_wR_factor_ref 0.1481 _refine_ls_wR_factor_gt 0.1340 _refine_ls_goodness_of_fit_ref 0.925 _refine_ls_restrained_S_all 0.925 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.82322(2) 0.16471(2) 0.634547(12) 0.02889(10) Uani 1 1 d . . . Cl2 Cl 0.67300(17) 0.11979(15) 0.58476(9) 0.0403(5) Uani 1 1 d . . . P1 P 0.96659(17) 0.19149(15) 0.68455(9) 0.0332(5) Uani 1 1 d . . . P2 P 0.84969(16) 0.25630(15) 0.56226(8) 0.0300(5) Uani 1 1 d . . . Cl1 Cl 0.77201(18) 0.06078(16) 0.70431(9) 0.0448(6) Uani 1 1 d . . . O1 O 1.0427(4) 0.2731(4) 0.6679(2) 0.0344(13) Uani 1 1 d . . . O2 O 0.9498(4) 0.3193(3) 0.5611(2) 0.0327(13) Uani 1 1 d . . . C4 C 1.1478(7) 0.4062(6) 0.6000(4) 0.045(2) Uani 1 1 d . . . H4A H 1.1528 0.3436 0.5891 0.054 Uiso 1 1 calc R . . H4B H 1.2122 0.4356 0.5896 0.054 Uiso 1 1 calc R . . C2 C 1.0311(6) 0.3672(6) 0.6795(3) 0.036(2) Uani 1 1 d . . . H2 H 1.0207 0.3754 0.7195 0.043 Uiso 1 1 calc R . . C9 C 0.7339(6) 0.3267(6) 0.5488(3) 0.0350(19) Uani 1 1 d . . . H9 H 0.6808 0.2848 0.5355 0.042 Uiso 1 1 calc R . . C16 C 0.6868(7) 0.3704(6) 0.6004(4) 0.043(2) Uani 1 1 d . . . H16A H 0.6788 0.3260 0.6291 0.064 Uiso 1 1 calc R . . H16B H 0.6201 0.3953 0.5913 0.064 Uiso 1 1 calc R . . H16C H 0.7317 0.4175 0.6133 0.064 Uiso 1 1 calc R . . C1 C 0.9399(6) 0.4073(6) 0.6488(3) 0.035(2) Uani 1 1 d . . . H1A H 0.9287 0.4681 0.6621 0.043 Uiso 1 1 calc R . . H1B H 0.8782 0.3725 0.6574 0.043 Uiso 1 1 calc R . . C8 C 0.9373(7) 0.2030(7) 0.7585(4) 0.046(2) Uani 1 1 d . . . H8 H 0.9148 0.1432 0.7706 0.056 Uiso 1 1 calc R . . C3 C 1.1347(7) 0.4115(7) 0.6625(4) 0.046(2) Uani 1 1 d . . . H3A H 1.1353 0.4740 0.6742 0.056 Uiso 1 1 calc R . . H3B H 1.1920 0.3809 0.6807 0.056 Uiso 1 1 calc R . . C10 C 0.8686(7) 0.1909(6) 0.4984(3) 0.036(2) Uani 1 1 d . . . H10 H 0.7998 0.1698 0.4868 0.043 Uiso 1 1 calc R . . C6 C 0.9546(6) 0.4095(5) 0.5865(4) 0.035(2) Uani 1 1 d . . . H6 H 0.8988 0.4461 0.5705 0.042 Uiso 1 1 calc R . . C13 C 0.8472(7) 0.2654(7) 0.7714(4) 0.051(3) Uani 1 1 d . . . H13A H 0.7884 0.2491 0.7490 0.076 Uiso 1 1 calc R . . H13B H 0.8670 0.3263 0.7633 0.076 Uiso 1 1 calc R . . H13C H 0.8293 0.2603 0.8100 0.076 Uiso 1 1 calc R . . C11 C 1.1268(11) 0.1050(8) 0.6322(5) 0.089(4) Uani 1 1 d . . . H11A H 1.1484 0.1656 0.6247 0.134 Uiso 1 1 calc R . . H11B H 1.0868 0.0828 0.6014 0.134 Uiso 1 1 calc R . . H11C H 1.1869 0.0677 0.6374 0.134 Uiso 1 1 calc R . . C15 C 0.7456(7) 0.3960(7) 0.5025(4) 0.055(3) Uani 1 1 d . . . H15A H 0.7752 0.3678 0.4703 0.083 Uiso 1 1 calc R . . H15B H 0.7903 0.4437 0.5148 0.083 Uiso 1 1 calc R . . H15C H 0.6786 0.4201 0.4932 0.083 Uiso 1 1 calc R . . C7 C 1.0653(7) 0.1034(7) 0.6810(5) 0.058(3) Uani 1 1 d . . . H7 H 1.1145 0.1207 0.7103 0.069 Uiso 1 1 calc R . . C5 C 1.0583(6) 0.4500(6) 0.5686(4) 0.042(2) Uani 1 1 d . . . H5A H 1.0678 0.4412 0.5290 0.050 Uiso 1 1 calc R . . H5B H 1.0581 0.5141 0.5759 0.050 Uiso 1 1 calc R . . C18 C 0.9339(9) 0.1088(8) 0.5078(4) 0.067(3) Uani 1 1 d . . . H18A H 0.9058 0.0746 0.5381 0.101 Uiso 1 1 calc R . . H18B H 1.0037 0.1267 0.5166 0.101 Uiso 1 1 calc R . . H18C H 0.9342 0.0727 0.4747 0.101 Uiso 1 1 calc R . . C14 C 1.0326(7) 0.2261(8) 0.7948(4) 0.062(3) Uani 1 1 d . . . H14A H 1.0882 0.1852 0.7865 0.093 Uiso 1 1 calc R . . H14B H 1.0143 0.2208 0.8334 0.093 Uiso 1 1 calc R . . H14C H 1.0545 0.2865 0.7872 0.093 Uiso 1 1 calc R . . C12 C 1.0324(9) 0.0128(7) 0.6979(5) 0.076(4) Uani 1 1 d . . . H12A H 0.9959 0.0161 0.7327 0.115 Uiso 1 1 calc R . . H12B H 1.0924 -0.0250 0.7020 0.115 Uiso 1 1 calc R . . H12C H 0.9874 -0.0120 0.6700 0.115 Uiso 1 1 calc R . . C17 C 0.9133(10) 0.2440(8) 0.4498(4) 0.090(4) Uani 1 1 d . . . H17A H 0.8719 0.2968 0.4436 0.134 Uiso 1 1 calc R . . H17B H 0.9130 0.2073 0.4170 0.134 Uiso 1 1 calc R . . H17C H 0.9833 0.2616 0.4583 0.134 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 0.03664(17) 0.02607(16) 0.02397(15) -0.00116(14) 0.00235(14) -0.00223(15) Cl2 0.0480(12) 0.0357(11) 0.0371(11) -0.0011(9) -0.0020(10) -0.0136(11) P1 0.0330(11) 0.0342(12) 0.0323(11) 0.0048(10) 0.0015(9) 0.0043(10) P2 0.0388(12) 0.0279(12) 0.0234(11) -0.0019(9) 0.0032(8) -0.0008(9) Cl1 0.0587(14) 0.0423(13) 0.0335(11) 0.0086(10) 0.0037(10) -0.0115(11) O1 0.027(3) 0.034(3) 0.041(3) 0.006(3) -0.001(2) 0.006(3) O2 0.028(3) 0.030(3) 0.040(3) 0.001(3) 0.002(2) -0.002(2) C4 0.050(6) 0.035(5) 0.050(6) -0.008(5) 0.000(4) -0.012(4) C2 0.037(5) 0.041(5) 0.030(4) -0.006(4) -0.006(4) 0.003(4) C9 0.035(5) 0.037(5) 0.033(4) -0.002(4) -0.007(4) -0.004(4) C16 0.035(5) 0.041(5) 0.053(6) 0.004(5) 0.006(4) 0.009(4) C1 0.035(5) 0.022(4) 0.050(6) 0.002(4) -0.003(4) 0.002(4) C8 0.045(6) 0.058(6) 0.036(5) 0.011(5) -0.011(4) -0.004(5) C3 0.036(5) 0.048(6) 0.056(6) -0.011(5) -0.001(4) -0.006(4) C10 0.040(5) 0.039(5) 0.028(4) -0.003(4) 0.004(4) -0.007(4) C6 0.038(5) 0.023(4) 0.045(5) -0.006(4) 0.002(4) -0.003(4) C13 0.050(6) 0.062(7) 0.040(5) -0.013(5) 0.011(4) -0.002(5) C11 0.127(11) 0.049(7) 0.091(10) 0.018(7) 0.045(8) 0.051(8) C15 0.051(6) 0.074(8) 0.040(6) 0.015(5) -0.006(5) 0.014(6) C7 0.043(6) 0.050(7) 0.081(8) 0.020(6) 0.018(5) 0.024(5) C5 0.051(6) 0.034(5) 0.041(5) -0.002(4) 0.004(4) -0.009(4) C18 0.091(9) 0.073(8) 0.038(6) -0.001(6) 0.014(5) 0.021(7) C14 0.043(6) 0.100(9) 0.043(6) 0.002(6) -0.010(5) 0.001(6) C12 0.071(8) 0.043(7) 0.114(10) 0.020(7) 0.029(7) 0.013(6) C17 0.168(13) 0.064(8) 0.036(6) 0.006(6) 0.039(7) 0.030(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 P2 2.234(2) . ? Pt1 P1 2.238(2) . ? Pt1 Cl2 2.370(2) . ? Pt1 Cl1 2.374(2) . ? P1 O1 1.609(6) . ? P1 C8 1.825(9) . ? P1 C7 1.826(9) . ? P2 O2 1.593(5) . ? P2 C10 1.833(8) . ? P2 C9 1.850(8) . ? O1 C2 1.434(10) . ? O2 C6 1.473(9) . ? C4 C3 1.515(12) . ? C4 C5 1.522(12) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C2 C1 1.508(10) . ? C2 C3 1.543(11) . ? C2 H2 0.9800 . ? C9 C15 1.524(12) . ? C9 C16 1.526(11) . ? C9 H9 0.9800 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C1 C6 1.511(11) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C8 C13 1.518(12) . ? C8 C14 1.545(12) . ? C8 H8 0.9800 . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C10 C18 1.499(13) . ? C10 C17 1.523(12) . ? C10 H10 0.9800 . ? C6 C5 1.527(11) . ? C6 H6 0.9800 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C11 C7 1.417(14) . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C7 C12 1.470(13) . ? C7 H7 0.9800 . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 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 P2 Pt1 P1 100.58(8) . . ? P2 Pt1 Cl2 84.45(7) . . ? P1 Pt1 Cl2 173.75(8) . . ? P2 Pt1 Cl1 171.40(8) . . ? P1 Pt1 Cl1 88.01(8) . . ? Cl2 Pt1 Cl1 86.96(8) . . ? O1 P1 C8 107.3(4) . . ? O1 P1 C7 96.1(4) . . ? C8 P1 C7 104.8(5) . . ? O1 P1 Pt1 120.2(2) . . ? C8 P1 Pt1 111.7(3) . . ? C7 P1 Pt1 114.9(4) . . ? O2 P2 C10 101.0(3) . . ? O2 P2 C9 108.4(3) . . ? C10 P2 C9 105.1(4) . . ? O2 P2 Pt1 119.7(2) . . ? C10 P2 Pt1 110.4(3) . . ? C9 P2 Pt1 111.0(3) . . ? C2 O1 P1 128.6(5) . . ? C6 O2 P2 124.2(5) . . ? C3 C4 C5 112.7(8) . . ? C3 C4 H4A 109.1 . . ? C5 C4 H4A 109.1 . . ? C3 C4 H4B 109.1 . . ? C5 C4 H4B 109.1 . . ? H4A C4 H4B 107.8 . . ? O1 C2 C1 111.8(7) . . ? O1 C2 C3 106.0(7) . . ? C1 C2 C3 112.0(7) . . ? O1 C2 H2 109.0 . . ? C1 C2 H2 109.0 . . ? C3 C2 H2 109.0 . . ? C15 C9 C16 110.2(7) . . ? C15 C9 P2 115.5(6) . . ? C16 C9 P2 114.8(6) . . ? C15 C9 H9 105.0 . . ? C16 C9 H9 105.0 . . ? P2 C9 H9 105.0 . . ? C9 C16 H16A 109.5 . . ? C9 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C9 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C2 C1 C6 113.3(7) . . ? C2 C1 H1A 108.9 . . ? C6 C1 H1A 108.9 . . ? C2 C1 H1B 108.9 . . ? C6 C1 H1B 108.9 . . ? H1A C1 H1B 107.7 . . ? C13 C8 C14 110.8(8) . . ? C13 C8 P1 114.5(6) . . ? C14 C8 P1 114.1(6) . . ? C13 C8 H8 105.5 . . ? C14 C8 H8 105.5 . . ? P1 C8 H8 105.5 . . ? C4 C3 C2 109.6(7) . . ? C4 C3 H3A 109.7 . . ? C2 C3 H3A 109.7 . . ? C4 C3 H3B 109.7 . . ? C2 C3 H3B 109.7 . . ? H3A C3 H3B 108.2 . . ? C18 C10 C17 109.0(8) . . ? C18 C10 P2 112.3(6) . . ? C17 C10 P2 114.7(7) . . ? C18 C10 H10 106.8 . . ? C17 C10 H10 106.8 . . ? P2 C10 H10 106.8 . . ? O2 C6 C1 112.7(7) . . ? O2 C6 C5 106.2(6) . . ? C1 C6 C5 113.4(7) . . ? O2 C6 H6 108.1 . . ? C1 C6 H6 108.1 . . ? C5 C6 H6 108.1 . . ? C8 C13 H13A 109.5 . . ? C8 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C8 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C7 C11 H11A 109.5 . . ? C7 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C7 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? 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 C7 C12 113.9(10) . . ? C11 C7 P1 114.5(7) . . ? C12 C7 P1 116.4(7) . . ? C11 C7 H7 103.2 . . ? C12 C7 H7 103.2 . . ? P1 C7 H7 103.2 . . ? C4 C5 C6 110.7(7) . . ? C4 C5 H5A 109.5 . . ? C6 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? C6 C5 H5B 109.5 . . ? H5A C5 H5B 108.1 . . ? C10 C18 H18A 109.5 . . ? C10 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C10 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C8 C14 H14A 109.5 . . ? C8 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C8 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C7 C12 H12A 109.5 . . ? C7 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C7 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C10 C17 H17A 109.5 . . ? C10 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C10 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.934 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 4.699 _refine_diff_density_min -1.328 _refine_diff_density_rms 0.262 #===END data_complex6 _database_code_depnum_ccdc_archive 'CCDC 657411' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C90 H192 Cl8 O10 P8 Pt4' _chemical_formula_weight 2746.16 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' 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 Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 28.8263(11) _cell_length_b 8.7302(2) _cell_length_c 44.3883(10) _cell_angle_alpha 90.00 _cell_angle_beta 96.065(3) _cell_angle_gamma 90.00 _cell_volume 11108.2(6) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5831 _cell_measurement_theta_min 2.1308 _cell_measurement_theta_max 32.7188 _exptl_crystal_description needles _exptl_crystal_colour yellow _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.642 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5520 _exptl_absorpt_coefficient_mu 5.379 _exptl_absorpt_correction_T_min 0.61567 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.5 (release 28-08-2006 CrysAlis171 .NET) (compiled Aug 28 2006,13:05:05) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction XCalibur 3' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.1829 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 40857 _diffrn_reflns_av_R_equivalents 0.0721 _diffrn_reflns_av_sigmaI/netI 0.3097 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 43 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -61 _diffrn_reflns_limit_l_max 64 _diffrn_reflns_theta_min 2.21 _diffrn_reflns_theta_max 32.77 _reflns_number_total 17354 _reflns_number_gt 4742 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.31.5 (release 28-08-2006 CrysAlis171 .NET) (compiled Aug 28 2006,13:05:05) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.5 (release 28-08-2006 CrysAlis171 .NET) (compiled Aug 28 2006,13:05:05) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.5 (release 28-08-2006 CrysAlis171 .NET) (compiled Aug 28 2006,13:05:05) ; _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^)+(0.0794P)^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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 17354 _refine_ls_number_parameters 577 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2152 _refine_ls_R_factor_gt 0.0586 _refine_ls_wR_factor_ref 0.1724 _refine_ls_wR_factor_gt 0.1423 _refine_ls_goodness_of_fit_ref 0.735 _refine_ls_restrained_S_all 0.735 _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 C31 C 0.6165(6) 0.0835(18) 0.3390(7) 0.266(18) Uani 1 1 d . . . H31A H 0.5876 0.1134 0.3278 0.399 Uiso 1 1 calc R . . H31B H 0.6150 0.1032 0.3601 0.399 Uiso 1 1 calc R . . H31C H 0.6217 -0.0238 0.3360 0.399 Uiso 1 1 calc R . . C16 C 0.6973(13) 0.485(2) 0.4898(4) 0.30(2) Uani 1 1 d . . . H16A H 0.6909 0.5931 0.4882 0.446 Uiso 1 1 calc R . . H16B H 0.7296 0.4699 0.4968 0.446 Uiso 1 1 calc R . . H16C H 0.6783 0.4404 0.5040 0.446 Uiso 1 1 calc R . . Pt1 Pt 0.903156(18) 0.48465(4) 0.369174(9) 0.06473(17) Uani 1 1 d . . . Pt2 Pt 0.662897(16) 0.47156(4) 0.380975(9) 0.05600(15) Uani 1 1 d . . . P2 P 0.67306(9) 0.5646(3) 0.43022(6) 0.0434(6) Uani 1 1 d . . . P4 P 0.89113(9) 0.3909(2) 0.31989(5) 0.0406(6) Uani 1 1 d . . . P1 P 0.91803(9) 0.5706(3) 0.41892(6) 0.0462(7) Uani 1 1 d . . . P3 P 0.64665(9) 0.3783(2) 0.33179(5) 0.0396(6) Uani 1 1 d . . . Cl2 Cl 0.88061(16) 0.7259(4) 0.35291(9) 0.1216(15) Uani 1 1 d . . . O5 O 0.74954(19) 0.4103(5) 0.38240(11) 0.0350(14) Uani 1 1 d . . . H5 H 0.7423 0.4827 0.3927 0.052 Uiso 1 1 calc R . . O1 O 0.8820(2) 0.6862(7) 0.43141(14) 0.0573(19) Uani 1 1 d . . . O4 O 0.8453(2) 0.4496(7) 0.29864(13) 0.0536(17) Uani 1 1 d . . . Cl1 Cl 0.9536(2) 0.2717(5) 0.38070(10) 0.158(2) Uani 1 1 d . . . O2 O 0.7149(2) 0.6812(8) 0.43920(14) 0.0608(19) Uani 1 1 d . . . O3 O 0.6793(2) 0.4361(8) 0.30647(14) 0.0585(19) Uani 1 1 d . . . C23 C 0.7622(3) 0.4396(10) 0.3031(2) 0.045(2) Uani 1 1 d . . . H23A H 0.7569 0.4051 0.2822 0.054 Uiso 1 1 calc R . . H23B H 0.7664 0.3499 0.3160 0.054 Uiso 1 1 calc R . . C45 C 0.8131(3) 0.4184(8) 0.37841(15) 0.0280(19) Uani 1 1 d . . . H45A H 0.8285 0.4786 0.3946 0.042 Uiso 1 1 calc R . . H45B H 0.8178 0.4643 0.3593 0.042 Uiso 1 1 calc R . . H45C H 0.8257 0.3166 0.3793 0.042 Uiso 1 1 calc R . . Cl4 Cl 0.6714(2) 0.7202(5) 0.36294(13) 0.174(2) Uani 1 1 d . . . Cl3 Cl 0.6269(3) 0.2549(8) 0.39672(19) 0.251(4) Uani 1 1 d . . . C24 C 0.7204(3) 0.5278(10) 0.3109(2) 0.042(2) Uani 1 1 d . . . C41 C 0.9365(3) 0.4540(12) 0.2960(2) 0.055(3) Uani 1 1 d . . . C33 C 0.5891(4) 0.4444(12) 0.3132(3) 0.062(3) Uani 1 1 d . . . C7 C 0.9177(4) 0.4112(11) 0.4475(2) 0.055(3) Uani 1 1 d . . . C10 C 0.8754(5) 0.3118(14) 0.4386(3) 0.102(5) Uani 1 1 d . . . H10A H 0.8804 0.2528 0.4210 0.153 Uiso 1 1 calc R . . H10B H 0.8484 0.3757 0.4342 0.153 Uiso 1 1 calc R . . H10C H 0.8705 0.2440 0.4550 0.153 Uiso 1 1 calc R . . C28 C 0.8056(3) 0.5365(10) 0.3071(2) 0.043(2) Uani 1 1 d . . . C25 C 0.7142(4) 0.6709(12) 0.2908(2) 0.064(3) Uani 1 1 d . . . H25A H 0.7068 0.6404 0.2699 0.077 Uiso 1 1 calc R . . H25B H 0.6885 0.7316 0.2967 0.077 Uiso 1 1 calc R . . C5 C 0.7496(4) 0.9086(10) 0.4211(2) 0.063(3) Uani 1 1 d . . . H5A H 0.7198 0.9431 0.4111 0.075 Uiso 1 1 calc R . . H5B H 0.7529 0.9487 0.4415 0.075 Uiso 1 1 calc R . . C27 C 0.8002(4) 0.6755(11) 0.2869(2) 0.064(3) Uani 1 1 d . . . H27A H 0.7966 0.6438 0.2659 0.077 Uiso 1 1 calc R . . H27B H 0.8278 0.7392 0.2903 0.077 Uiso 1 1 calc R . . C36 C 0.5877(5) 0.6167(13) 0.3139(3) 0.105(5) Uani 1 1 d . . . H36A H 0.6166 0.6570 0.3084 0.158 Uiso 1 1 calc R . . H36B H 0.5830 0.6505 0.3340 0.158 Uiso 1 1 calc R . . H36C H 0.5624 0.6526 0.2998 0.158 Uiso 1 1 calc R . . C6 C 0.7503(4) 0.7354(10) 0.4221(2) 0.045(3) Uani 1 1 d . . . C1 C 0.7984(3) 0.6777(9) 0.4352(2) 0.044(2) Uani 1 1 d . . . H1A H 0.8045 0.7106 0.4561 0.053 Uiso 1 1 calc R . . H1B H 0.7987 0.5666 0.4349 0.053 Uiso 1 1 calc R . . C15 C 0.6865(5) 0.4115(14) 0.4595(2) 0.083(4) Uani 1 1 d . . . C3 C 0.8361(4) 0.9080(11) 0.4172(2) 0.062(3) Uani 1 1 d . . . H3A H 0.8599 0.9438 0.4049 0.074 Uiso 1 1 calc R . . H3B H 0.8437 0.9463 0.4376 0.074 Uiso 1 1 calc R . . C4 C 0.7884(4) 0.9693(11) 0.4042(3) 0.066(3) Uani 1 1 d . . . H4A H 0.7887 1.0803 0.4053 0.079 Uiso 1 1 calc R . . H4B H 0.7827 0.9405 0.3830 0.079 Uiso 1 1 calc R . . C11 C 0.9708(4) 0.6916(15) 0.4246(3) 0.081(4) Uani 1 1 d . . . C17 C 0.7270(5) 0.3214(14) 0.4506(3) 0.114(6) Uani 1 1 d . . . H17A H 0.7271 0.2218 0.4598 0.172 Uiso 1 1 calc R . . H17B H 0.7555 0.3736 0.4574 0.172 Uiso 1 1 calc R . . H17C H 0.7243 0.3107 0.4290 0.172 Uiso 1 1 calc R . . C44 C 0.9856(4) 0.4071(14) 0.3110(3) 0.085(4) Uani 1 1 d . . . H44A H 1.0083 0.4247 0.2970 0.127 Uiso 1 1 calc R . . H44B H 0.9855 0.3004 0.3162 0.127 Uiso 1 1 calc R . . H44C H 0.9934 0.4671 0.3289 0.127 Uiso 1 1 calc R . . C22 C 0.5771(5) 0.594(2) 0.4364(4) 0.165(8) Uani 1 1 d . . . H22A H 0.5510 0.6618 0.4377 0.248 Uiso 1 1 calc R . . H22B H 0.5791 0.5234 0.4530 0.248 Uiso 1 1 calc R . . H22C H 0.5729 0.5391 0.4176 0.248 Uiso 1 1 calc R . . C37 C 0.8825(4) 0.1763(10) 0.3188(2) 0.058(3) Uani 1 1 d . . . C13 C 1.0144(5) 0.5971(18) 0.4170(4) 0.128(6) Uani 1 1 d . . . H13A H 1.0065 0.5398 0.3987 0.191 Uiso 1 1 calc R . . H13B H 1.0237 0.5280 0.4333 0.191 Uiso 1 1 calc R . . H13C H 1.0396 0.6658 0.4143 0.191 Uiso 1 1 calc R . . C19 C 0.6223(5) 0.689(2) 0.4378(4) 0.106(5) Uani 1 1 d . . . C2 C 0.8357(3) 0.7368(9) 0.4176(2) 0.040(2) Uani 1 1 d . . . H2 H 0.8306 0.6985 0.3967 0.048 Uiso 1 1 calc R . . C9 C 0.9115(10) 0.4753(17) 0.4785(3) 0.203(12) Uani 1 1 d . . . H9A H 0.8997 0.3967 0.4908 0.305 Uiso 1 1 calc R . . H9B H 0.8898 0.5591 0.4764 0.305 Uiso 1 1 calc R . . H9C H 0.9410 0.5110 0.4880 0.305 Uiso 1 1 calc R . . C38 C 0.8500(4) 0.1366(12) 0.3413(3) 0.097(5) Uani 1 1 d . . . H38A H 0.8448 0.0280 0.3411 0.145 Uiso 1 1 calc R . . H38B H 0.8209 0.1887 0.3363 0.145 Uiso 1 1 calc R . . H38C H 0.8632 0.1674 0.3611 0.145 Uiso 1 1 calc R . . C26 C 0.7579(4) 0.7659(12) 0.2937(3) 0.075(4) Uani 1 1 d . . . H26A H 0.7631 0.8062 0.3142 0.090 Uiso 1 1 calc R . . H26B H 0.7537 0.8520 0.2799 0.090 Uiso 1 1 calc R . . C42 C 0.9361(5) 0.6286(13) 0.2954(4) 0.120(6) Uani 1 1 d . . . H42A H 0.9568 0.6644 0.2814 0.181 Uiso 1 1 calc R . . H42B H 0.9462 0.6671 0.3153 0.181 Uiso 1 1 calc R . . H42C H 0.9050 0.6641 0.2892 0.181 Uiso 1 1 calc R . . C34 C 0.5498(4) 0.3869(15) 0.3311(4) 0.113(5) Uani 1 1 d . . . H34A H 0.5542 0.2798 0.3355 0.169 Uiso 1 1 calc R . . H34B H 0.5203 0.4018 0.3193 0.169 Uiso 1 1 calc R . . H34C H 0.5504 0.4430 0.3497 0.169 Uiso 1 1 calc R . . C29 C 0.6525(4) 0.1660(11) 0.3290(2) 0.068(3) Uani 1 1 d . . . C18 C 0.6497(7) 0.2999(18) 0.4626(5) 0.175(9) Uani 1 1 d . . . H18A H 0.6507 0.2217 0.4474 0.263 Uiso 1 1 calc R . . H18B H 0.6199 0.3501 0.4599 0.263 Uiso 1 1 calc R . . H18C H 0.6542 0.2542 0.4823 0.263 Uiso 1 1 calc R . . C40 C 0.9232(6) 0.0869(16) 0.3210(6) 0.231(14) Uani 1 1 d . . . H40A H 0.9427 0.1140 0.3391 0.347 Uiso 1 1 calc R . . H40B H 0.9397 0.1052 0.3037 0.347 Uiso 1 1 calc R . . H40C H 0.9150 -0.0195 0.3218 0.347 Uiso 1 1 calc R . . C8 C 0.9603(6) 0.3142(18) 0.4491(5) 0.191(10) Uani 1 1 d . . . H8A H 0.9664 0.2720 0.4691 0.286 Uiso 1 1 calc R . . H8B H 0.9864 0.3755 0.4447 0.286 Uiso 1 1 calc R . . H8C H 0.9556 0.2326 0.4346 0.286 Uiso 1 1 calc R . . C39 C 0.8525(9) 0.1423(18) 0.2868(3) 0.218(13) Uani 1 1 d . . . H39A H 0.8732 0.1286 0.2714 0.327 Uiso 1 1 calc R . . H39B H 0.8320 0.2270 0.2814 0.327 Uiso 1 1 calc R . . H39C H 0.8344 0.0509 0.2883 0.327 Uiso 1 1 calc R . . C43 C 0.9292(5) 0.3943(18) 0.2637(3) 0.113(5) Uani 1 1 d . . . H43A H 0.8972 0.4087 0.2558 0.170 Uiso 1 1 calc R . . H43B H 0.9367 0.2872 0.2635 0.170 Uiso 1 1 calc R . . H43C H 0.9490 0.4493 0.2514 0.170 Uiso 1 1 calc R . . C20 C 0.6171(6) 0.8078(14) 0.4143(5) 0.172(10) Uani 1 1 d . . . H20A H 0.6021 0.7651 0.3958 0.258 Uiso 1 1 calc R . . H20B H 0.6474 0.8460 0.4109 0.258 Uiso 1 1 calc R . . H20C H 0.5985 0.8903 0.4208 0.258 Uiso 1 1 calc R . . C12 C 0.9797(6) 0.7506(19) 0.4589(3) 0.154(8) Uani 1 1 d . . . H12A H 1.0022 0.8320 0.4601 0.230 Uiso 1 1 calc R . . H12B H 0.9913 0.6677 0.4717 0.230 Uiso 1 1 calc R . . H12C H 0.9510 0.7876 0.4653 0.230 Uiso 1 1 calc R . . C30 C 0.6995(4) 0.1262(13) 0.3439(3) 0.104(5) Uani 1 1 d . . . H30A H 0.7051 0.1803 0.3627 0.156 Uiso 1 1 calc R . . H30B H 0.7227 0.1547 0.3308 0.156 Uiso 1 1 calc R . . H30C H 0.7012 0.0179 0.3476 0.156 Uiso 1 1 calc R . . C14 C 0.9646(5) 0.8205(14) 0.4014(4) 0.133(7) Uani 1 1 d . . . H14A H 0.9942 0.8675 0.3995 0.199 Uiso 1 1 calc R . . H14B H 0.9435 0.8956 0.4079 0.199 Uiso 1 1 calc R . . H14C H 0.9521 0.7795 0.3821 0.199 Uiso 1 1 calc R . . C21 C 0.6316(7) 0.761(3) 0.4702(5) 0.240(14) Uani 1 1 d . . . H21A H 0.6614 0.8111 0.4722 0.360 Uiso 1 1 calc R . . H21B H 0.6313 0.6822 0.4852 0.360 Uiso 1 1 calc R . . H21C H 0.6077 0.8349 0.4730 0.360 Uiso 1 1 calc R . . C35 C 0.5808(5) 0.390(2) 0.2799(3) 0.136(7) Uani 1 1 d . . . H35A H 0.5492 0.4122 0.2720 0.204 Uiso 1 1 calc R . . H35B H 0.5861 0.2817 0.2789 0.204 Uiso 1 1 calc R . . H35C H 0.6018 0.4425 0.2680 0.204 Uiso 1 1 calc R . . H28 H 0.809(2) 0.561(7) 0.3274(16) 0.019(19) Uiso 1 1 d . . . H6 H 0.752(2) 0.693(7) 0.4003(15) 0.015(17) Uiso 1 1 d . . . H24 H 0.724(3) 0.556(8) 0.3353(17) 0.03(2) Uiso 1 1 d . . . C32 C 0.6534(11) 0.1218(18) 0.2956(4) 0.30(2) Uani 1 1 d . . . H32A H 0.6790 0.1727 0.2876 0.449 Uiso 1 1 calc R . . H32B H 0.6247 0.1523 0.2843 0.449 Uiso 1 1 calc R . . H32C H 0.6572 0.0130 0.2940 0.449 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 C31 0.081(13) 0.081(11) 0.62(5) 0.13(2) -0.01(2) -0.021(10) C16 0.67(6) 0.116(15) 0.075(12) 0.001(11) -0.09(2) 0.10(2) Pt1 0.1066(4) 0.0433(2) 0.0411(2) -0.00231(18) -0.0072(2) 0.0115(2) Pt2 0.0824(4) 0.0414(2) 0.0444(2) -0.00435(18) 0.0077(2) -0.0092(2) P2 0.0459(17) 0.0416(13) 0.0436(15) -0.0019(11) 0.0082(13) 0.0005(11) P4 0.0442(16) 0.0392(12) 0.0386(14) 0.0008(10) 0.0054(12) 0.0018(11) P1 0.0479(17) 0.0485(14) 0.0412(14) -0.0018(11) -0.0006(13) 0.0008(12) P3 0.0355(15) 0.0401(12) 0.0422(14) -0.0057(10) -0.0004(12) 0.0011(10) Cl2 0.166(4) 0.081(2) 0.113(3) 0.003(2) -0.008(3) -0.002(2) O5 0.055(4) 0.027(3) 0.019(3) -0.010(2) -0.011(3) 0.003(3) O1 0.062(5) 0.047(4) 0.058(4) -0.014(3) -0.013(4) 0.017(3) O4 0.052(4) 0.077(4) 0.032(3) -0.006(3) 0.003(3) 0.020(4) Cl1 0.214(6) 0.126(4) 0.129(4) 0.008(3) 0.004(4) 0.066(4) O2 0.065(5) 0.075(5) 0.046(4) -0.022(3) 0.026(4) -0.022(4) O3 0.042(4) 0.087(5) 0.046(4) 0.000(4) 0.003(3) -0.017(4) C23 0.047(6) 0.041(5) 0.047(6) 0.000(4) 0.007(5) -0.006(4) C45 0.045(6) 0.031(4) 0.009(3) -0.009(3) 0.008(4) -0.006(4) Cl4 0.218(6) 0.113(4) 0.189(5) 0.007(3) 0.003(4) 0.005(4) Cl3 0.301(10) 0.161(6) 0.289(9) -0.001(6) 0.026(7) -0.051(6) C24 0.033(6) 0.049(5) 0.044(5) -0.003(4) 0.002(5) -0.001(4) C41 0.025(6) 0.078(7) 0.063(7) 0.006(6) 0.008(5) 0.000(5) C33 0.041(7) 0.074(7) 0.072(8) 0.007(6) 0.016(6) 0.008(6) C7 0.069(8) 0.064(6) 0.033(6) 0.018(5) 0.007(5) 0.014(6) C10 0.099(11) 0.073(8) 0.134(12) 0.050(8) 0.011(9) 0.000(8) C28 0.037(6) 0.049(5) 0.042(6) -0.001(5) 0.004(5) 0.011(5) C25 0.043(7) 0.079(7) 0.073(8) 0.027(6) 0.013(6) 0.015(6) C5 0.063(8) 0.047(6) 0.076(8) -0.010(5) -0.001(6) 0.014(5) C27 0.047(7) 0.073(7) 0.073(8) 0.030(6) 0.017(6) 0.001(6) C36 0.080(10) 0.079(9) 0.160(14) 0.047(9) 0.028(9) 0.028(7) C6 0.059(7) 0.046(5) 0.033(5) -0.014(4) 0.014(5) -0.008(5) C1 0.038(6) 0.041(5) 0.049(6) -0.010(4) -0.008(5) 0.004(4) C15 0.131(13) 0.067(7) 0.049(7) 0.002(6) 0.000(8) -0.011(8) C3 0.060(8) 0.054(6) 0.071(7) 0.013(5) 0.001(6) -0.006(5) C4 0.059(7) 0.047(5) 0.096(9) 0.007(6) 0.026(7) -0.004(5) C11 0.063(9) 0.109(10) 0.076(9) 0.000(7) 0.024(7) -0.020(7) C17 0.110(13) 0.079(9) 0.152(14) 0.056(9) 0.003(11) 0.024(9) C44 0.048(8) 0.089(9) 0.123(11) 0.020(8) 0.034(8) -0.001(6) C22 0.059(11) 0.207(19) 0.24(2) 0.010(17) 0.069(13) 0.021(12) C37 0.078(8) 0.040(5) 0.056(7) -0.012(5) 0.012(6) 0.009(5) C13 0.052(10) 0.145(14) 0.181(17) -0.002(13) -0.008(10) -0.019(9) C19 0.047(9) 0.147(14) 0.127(13) -0.058(11) 0.028(8) 0.020(9) C2 0.026(5) 0.036(5) 0.059(6) -0.010(4) 0.008(5) -0.002(4) C9 0.45(4) 0.104(13) 0.055(9) 0.002(9) 0.013(15) -0.044(17) C38 0.073(9) 0.060(7) 0.169(14) 0.047(8) 0.066(9) 0.020(6) C26 0.052(8) 0.063(7) 0.113(10) 0.035(7) 0.029(7) 0.011(6) C42 0.083(11) 0.076(9) 0.199(17) 0.069(10) 0.000(10) -0.017(8) C34 0.058(9) 0.079(9) 0.197(16) 0.013(10) -0.005(10) 0.010(7) C29 0.088(9) 0.044(6) 0.066(7) -0.001(5) -0.016(7) -0.008(6) C18 0.18(2) 0.109(13) 0.26(2) 0.061(14) 0.143(18) 0.003(13) C40 0.129(16) 0.057(9) 0.53(4) 0.072(16) 0.14(2) 0.047(10) C8 0.129(16) 0.107(13) 0.33(3) 0.102(16) 0.020(17) 0.045(12) C39 0.48(4) 0.093(12) 0.074(11) -0.026(9) -0.001(17) -0.111(18) C43 0.104(12) 0.177(15) 0.058(8) 0.011(9) 0.010(8) -0.046(11) C20 0.118(15) 0.047(8) 0.33(3) 0.006(12) -0.057(16) 0.024(8) C12 0.196(19) 0.187(17) 0.083(11) -0.046(11) 0.041(12) -0.125(15) C30 0.091(11) 0.072(8) 0.145(13) 0.037(8) -0.010(9) 0.034(7) C14 0.091(12) 0.073(9) 0.24(2) 0.069(11) 0.047(12) -0.011(8) C21 0.22(3) 0.30(3) 0.21(2) -0.15(2) 0.055(18) 0.12(2) C35 0.132(14) 0.198(17) 0.072(10) -0.005(11) -0.015(10) 0.086(13) C32 0.67(6) 0.082(12) 0.105(13) -0.055(10) -0.14(2) 0.15(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C31 C29 1.37(2) . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? C16 C15 1.495(19) . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? Pt1 Cl2 2.298(4) . ? Pt1 P4 2.327(2) . ? Pt1 P1 2.329(2) . ? Pt1 Cl1 2.382(4) . ? Pt2 Cl3 2.301(7) . ? Pt2 P2 2.321(2) . ? Pt2 P3 2.331(2) . ? Pt2 Cl4 2.335(5) . ? P2 O2 1.595(7) . ? P2 C15 1.876(12) . ? P2 C19 1.881(13) . ? P4 O4 1.623(6) . ? P4 C41 1.852(10) . ? P4 C37 1.890(9) . ? P1 O1 1.589(7) . ? P1 C11 1.847(12) . ? P1 C7 1.885(9) . ? P3 O3 1.621(7) . ? P3 C33 1.864(11) . ? P3 C29 1.866(10) . ? O5 C45 1.860(10) . ? O5 H5 0.8200 . ? O1 C2 1.477(10) . ? O4 C28 1.455(11) . ? O2 C6 1.417(11) . ? O3 C24 1.426(10) . ? C23 C24 1.500(13) . ? C23 C28 1.507(13) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C45 H45A 0.9600 . ? C45 H45B 0.9600 . ? C45 H45C 0.9600 . ? C24 C25 1.535(12) . ? C24 H24 1.11(7) . ? C41 C43 1.521(14) . ? C41 C42 1.524(15) . ? C41 C44 1.553(14) . ? C33 C36 1.506(15) . ? C33 C34 1.536(16) . ? C33 C35 1.548(16) . ? C7 C8 1.487(17) . ? C7 C9 1.512(17) . ? C7 C10 1.515(15) . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C28 C27 1.508(12) . ? C28 H28 0.92(7) . ? C25 C26 1.500(14) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C5 C4 1.507(14) . ? C5 C6 1.513(12) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C27 C26 1.509(14) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? C6 C1 1.532(12) . ? C6 H6 1.04(6) . ? C1 C2 1.488(12) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C15 C18 1.458(19) . ? C15 C17 1.493(18) . ? C3 C2 1.494(12) . ? C3 C4 1.530(14) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C11 C14 1.525(17) . ? C11 C13 1.569(18) . ? C11 C12 1.600(16) . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C44 H44A 0.9600 . ? C44 H44B 0.9600 . ? C44 H44C 0.9600 . ? C22 C19 1.54(2) . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C37 C40 1.404(17) . ? C37 C38 1.481(14) . ? C37 C39 1.613(18) . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C19 C20 1.47(2) . ? C19 C21 1.57(2) . ? C2 H2 0.9800 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C42 H42A 0.9600 . ? C42 H42B 0.9600 . ? C42 H42C 0.9600 . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C29 C30 1.485(15) . ? C29 C32 1.536(19) . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C40 H40A 0.9600 . ? C40 H40B 0.9600 . ? C40 H40C 0.9600 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C39 H39A 0.9600 . ? C39 H39B 0.9600 . ? C39 H39C 0.9600 . ? C43 H43A 0.9600 . ? C43 H43B 0.9600 . ? C43 H43C 0.9600 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 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 C29 C31 H31A 109.5 . . ? C29 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C29 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? Cl2 Pt1 P4 91.03(11) . . ? Cl2 Pt1 P1 91.16(12) . . ? P4 Pt1 P1 177.36(9) . . ? Cl2 Pt1 Cl1 158.25(19) . . ? P4 Pt1 Cl1 87.37(13) . . ? P1 Pt1 Cl1 90.05(13) . . ? Cl3 Pt2 P2 91.0(2) . . ? Cl3 Pt2 P3 86.8(2) . . ? P2 Pt2 P3 175.68(9) . . ? Cl3 Pt2 Cl4 159.3(3) . . ? P2 Pt2 Cl4 89.44(15) . . ? P3 Pt2 Cl4 91.23(15) . . ? O2 P2 C15 100.7(5) . . ? O2 P2 C19 99.7(6) . . ? C15 P2 C19 113.2(8) . . ? O2 P2 Pt2 118.4(3) . . ? C15 P2 Pt2 113.6(4) . . ? C19 P2 Pt2 110.3(5) . . ? O4 P4 C41 98.9(4) . . ? O4 P4 C37 101.6(4) . . ? C41 P4 C37 112.3(5) . . ? O4 P4 Pt1 117.8(2) . . ? C41 P4 Pt1 112.9(3) . . ? C37 P4 Pt1 112.3(3) . . ? O1 P1 C11 98.5(5) . . ? O1 P1 C7 100.6(4) . . ? C11 P1 C7 113.1(6) . . ? O1 P1 Pt1 118.3(2) . . ? C11 P1 Pt1 112.4(4) . . ? C7 P1 Pt1 112.8(3) . . ? O3 P3 C33 98.7(4) . . ? O3 P3 C29 101.6(5) . . ? C33 P3 C29 111.1(5) . . ? O3 P3 Pt2 117.8(2) . . ? C33 P3 Pt2 112.8(4) . . ? C29 P3 Pt2 113.5(3) . . ? C45 O5 H5 109.5 . . ? C2 O1 P1 129.8(5) . . ? C28 O4 P4 128.9(5) . . ? C6 O2 P2 130.3(6) . . ? C24 O3 P3 127.9(6) . . ? C24 C23 C28 111.2(7) . . ? C24 C23 H23A 109.4 . . ? C28 C23 H23A 109.4 . . ? C24 C23 H23B 109.4 . . ? C28 C23 H23B 109.4 . . ? H23A C23 H23B 108.0 . . ? O5 C45 H45A 109.5 . . ? O5 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? O5 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? O3 C24 C23 110.8(7) . . ? O3 C24 C25 109.5(7) . . ? C23 C24 C25 109.3(8) . . ? O3 C24 H24 104(4) . . ? C23 C24 H24 111(4) . . ? C25 C24 H24 112(4) . . ? C43 C41 C42 109.0(11) . . ? C43 C41 C44 110.0(10) . . ? C42 C41 C44 106.1(9) . . ? C43 C41 P4 113.7(8) . . ? C42 C41 P4 107.7(8) . . ? C44 C41 P4 110.1(7) . . ? C36 C33 C34 107.0(10) . . ? C36 C33 C35 108.9(11) . . ? C34 C33 C35 110.3(11) . . ? C36 C33 P3 109.0(8) . . ? C34 C33 P3 109.9(8) . . ? C35 C33 P3 111.7(8) . . ? C8 C7 C9 110.1(14) . . ? C8 C7 C10 109.0(11) . . ? C9 C7 C10 106.3(13) . . ? C8 C7 P1 112.9(9) . . ? C9 C7 P1 110.4(8) . . ? C10 C7 P1 107.9(7) . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? O4 C28 C23 110.0(8) . . ? O4 C28 C27 107.5(8) . . ? C23 C28 C27 110.3(8) . . ? O4 C28 H28 111(4) . . ? C23 C28 H28 105(5) . . ? C27 C28 H28 113(4) . . ? C26 C25 C24 110.8(8) . . ? C26 C25 H25A 109.5 . . ? C24 C25 H25A 109.5 . . ? C26 C25 H25B 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 108.1 . . ? C4 C5 C6 111.0(9) . . ? C4 C5 H5A 109.4 . . ? C6 C5 H5A 109.4 . . ? C4 C5 H5B 109.4 . . ? C6 C5 H5B 109.4 . . ? H5A C5 H5B 108.0 . . ? C28 C27 C26 109.7(8) . . ? C28 C27 H27A 109.7 . . ? C26 C27 H27A 109.7 . . ? C28 C27 H27B 109.7 . . ? C26 C27 H27B 109.7 . . ? H27A C27 H27B 108.2 . . ? 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 . . ? O2 C6 C5 110.0(8) . . ? O2 C6 C1 111.2(8) . . ? C5 C6 C1 110.4(8) . . ? O2 C6 H6 119(4) . . ? C5 C6 H6 109(3) . . ? C1 C6 H6 96(4) . . ? C2 C1 C6 111.2(7) . . ? C2 C1 H1A 109.4 . . ? C6 C1 H1A 109.4 . . ? C2 C1 H1B 109.4 . . ? C6 C1 H1B 109.4 . . ? H1A C1 H1B 108.0 . . ? C18 C15 C17 105.6(12) . . ? C18 C15 C16 106.8(17) . . ? C17 C15 C16 111.8(17) . . ? C18 C15 P2 116.2(12) . . ? C17 C15 P2 107.6(9) . . ? C16 C15 P2 109.0(9) . . ? C2 C3 C4 110.3(8) . . ? C2 C3 H3A 109.6 . . ? C4 C3 H3A 109.6 . . ? C2 C3 H3B 109.6 . . ? C4 C3 H3B 109.6 . . ? H3A C3 H3B 108.1 . . ? C5 C4 C3 112.1(9) . . ? C5 C4 H4A 109.2 . . ? C3 C4 H4A 109.2 . . ? C5 C4 H4B 109.2 . . ? C3 C4 H4B 109.2 . . ? H4A C4 H4B 107.9 . . ? C14 C11 C13 106.3(11) . . ? C14 C11 C12 113.6(12) . . ? C13 C11 C12 108.8(12) . . ? C14 C11 P1 107.0(9) . . ? C13 C11 P1 109.6(9) . . ? C12 C11 P1 111.2(8) . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 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 . . ? C19 C22 H22A 109.5 . . ? C19 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C19 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C40 C37 C38 114.0(12) . . ? C40 C37 C39 109.0(15) . . ? C38 C37 C39 103.5(12) . . ? C40 C37 P4 116.3(10) . . ? C38 C37 P4 107.8(7) . . ? C39 C37 P4 105.2(8) . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C20 C19 C22 109.2(14) . . ? C20 C19 C21 111.1(16) . . ? C22 C19 C21 108.4(15) . . ? C20 C19 P2 107.6(11) . . ? C22 C19 P2 110.9(11) . . ? C21 C19 P2 109.6(10) . . ? O1 C2 C1 110.4(7) . . ? O1 C2 C3 107.2(7) . . ? C1 C2 C3 111.1(8) . . ? O1 C2 H2 109.3 . . ? C1 C2 H2 109.3 . . ? C3 C2 H2 109.3 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? 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 . . ? C25 C26 C27 112.4(9) . . ? C25 C26 H26A 109.1 . . ? C27 C26 H26A 109.1 . . ? C25 C26 H26B 109.1 . . ? C27 C26 H26B 109.1 . . ? H26A C26 H26B 107.8 . . ? 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 . . ? 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 . . ? C31 C29 C30 114.9(12) . . ? C31 C29 C32 105.7(17) . . ? C30 C29 C32 105.1(14) . . ? C31 C29 P3 115.1(12) . . ? C30 C29 P3 106.7(8) . . ? C32 C29 P3 108.9(9) . . ? C15 C18 H18A 109.5 . . ? C15 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C15 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 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 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 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 . . ? 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 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C11 C14 H14A 109.5 . . ? C11 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C11 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 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 . . ? C29 C32 H32A 109.5 . . ? C29 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C29 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.844 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.941 _refine_diff_density_max 2.423 _refine_diff_density_min -1.636 _refine_diff_density_rms 0.166 #===END data_complex7 _database_code_depnum_ccdc_archive 'CCDC 657412' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H49 Cl P2 Pt' _chemical_formula_weight 630.11 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.0176(8) _cell_length_b 14.8027(9) _cell_length_c 15.7279(9) _cell_angle_alpha 90.00 _cell_angle_beta 100.786(5) _cell_angle_gamma 90.00 _cell_volume 2748.5(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2300 _cell_measurement_theta_min 2.2020 _cell_measurement_theta_max 32.6459 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.11878 _exptl_crystal_size_mid 0.06810 _exptl_crystal_size_min 0.03399 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.523 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1272 _exptl_absorpt_coefficient_mu 5.327 _exptl_absorpt_correction_T_min 0.45151 _exptl_absorpt_correction_T_max 0.72269 _exptl_absorpt_correction_type 'numeric analytical' _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.26 beta (release 01-03-2005 CrysAlis171 .NET) (compiled Mar 2 2005,09:02:11) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Xcalibur3' _diffrn_measurement_method \w-scan _diffrn_detector_area_resol_mean 16.1829 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.0 _diffrn_reflns_number 24215 _diffrn_reflns_av_R_equivalents 0.0410 _diffrn_reflns_av_sigmaI/netI 0.1044 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.21 _diffrn_reflns_theta_max 32.72 _reflns_number_total 9275 _reflns_number_gt 4711 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.26 beta (release 01-03-2005 CrysAlis171 .NET) (compiled Mar 2 2005,09:02:11) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.26 beta (release 01-03-2005 CrysAlis171 .NET) (compiled Mar 2 2005,09:02:11) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.26 beta (release 01-03-2005 CrysAlis171 .NET) (compiled Mar 2 2005,09:02:11) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0290P)^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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9275 _refine_ls_number_parameters 253 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1031 _refine_ls_R_factor_gt 0.0347 _refine_ls_wR_factor_ref 0.0878 _refine_ls_wR_factor_gt 0.0629 _refine_ls_goodness_of_fit_ref 0.984 _refine_ls_restrained_S_all 0.984 _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 0.895249(15) 0.060449(13) 0.248994(11) 0.03535(7) Uani 1 1 d . . . P1 P 1.09014(10) 0.06112(10) 0.28307(8) 0.0387(3) Uani 1 1 d . . . Cl1 Cl 0.86725(11) 0.17425(10) 0.35472(8) 0.0574(4) Uani 1 1 d . . . C1 C 0.9187(4) -0.0282(3) 0.1525(3) 0.0396(12) Uani 1 1 d . . . H1 H 0.9210 0.0097 0.1018 0.047 Uiso 1 1 calc R . . P2 P 0.70611(10) 0.04239(9) 0.18899(8) 0.0369(3) Uani 1 1 d . . . C2 C 1.0318(4) -0.0792(3) 0.1693(3) 0.0440(13) Uani 1 1 d . . . H2 H 1.0293 -0.1217 0.2167 0.053 Uiso 1 1 calc R . . C3 C 1.0486(5) -0.1349(4) 0.0912(3) 0.0573(16) Uani 1 1 d . . . H3A H 1.0533 -0.0948 0.0432 0.069 Uiso 1 1 calc R . . H3B H 1.1194 -0.1679 0.1051 0.069 Uiso 1 1 calc R . . C4 C 0.9519(5) -0.2009(4) 0.0646(3) 0.0645(17) Uani 1 1 d . . . H4A H 0.9525 -0.2449 0.1103 0.077 Uiso 1 1 calc R . . H4B H 0.9626 -0.2329 0.0129 0.077 Uiso 1 1 calc R . . C5 C 0.8378(5) -0.1527(4) 0.0469(3) 0.0559(15) Uani 1 1 d . . . H5A H 0.7777 -0.1972 0.0348 0.067 Uiso 1 1 calc R . . H5B H 0.8334 -0.1147 -0.0039 0.067 Uiso 1 1 calc R . . C6 C 0.8205(4) -0.0946(3) 0.1237(3) 0.0422(12) Uani 1 1 d . . . H6 H 0.8177 -0.1353 0.1724 0.051 Uiso 1 1 calc R . . C7 C 0.7091(4) -0.0433(3) 0.1050(3) 0.0472(14) Uani 1 1 d . . . H7A H 0.6466 -0.0851 0.1036 0.057 Uiso 1 1 calc R . . H7B H 0.7005 -0.0144 0.0488 0.057 Uiso 1 1 calc R . . C8 C 1.1302(4) -0.0141(4) 0.2001(3) 0.0495(14) Uani 1 1 d . . . H8A H 1.1457 0.0214 0.1517 0.059 Uiso 1 1 calc R . . H8B H 1.1980 -0.0477 0.2243 0.059 Uiso 1 1 calc R . . C9 C 0.6389(4) 0.1438(4) 0.1288(3) 0.0477(14) Uani 1 1 d . . . C10 C 0.6132(4) -0.0086(3) 0.2597(3) 0.0418(12) Uani 1 1 d . . . C11 C 1.1581(4) 0.0101(4) 0.3897(3) 0.0507(14) Uani 1 1 d . . . C12 C 1.1569(4) 0.1739(4) 0.2638(3) 0.0522(14) Uani 1 1 d . . . C13 C 0.7310(5) 0.1843(4) 0.0845(4) 0.0766(19) Uani 1 1 d . . . H13A H 0.7523 0.1408 0.0452 0.115 Uiso 1 1 calc R . . H13B H 0.7959 0.1997 0.1275 0.115 Uiso 1 1 calc R . . H13C H 0.7022 0.2376 0.0532 0.115 Uiso 1 1 calc R . . C14 C 0.6080(5) 0.2145(4) 0.1894(4) 0.0721(19) Uani 1 1 d . . . H14A H 0.5505 0.1911 0.2182 0.108 Uiso 1 1 calc R . . H14B H 0.5801 0.2674 0.1569 0.108 Uiso 1 1 calc R . . H14C H 0.6739 0.2300 0.2315 0.108 Uiso 1 1 calc R . . C15 C 0.5354(5) 0.1229(4) 0.0585(4) 0.078(2) Uani 1 1 d . . . H15A H 0.5553 0.0785 0.0195 0.118 Uiso 1 1 calc R . . H15B H 0.5107 0.1772 0.0271 0.118 Uiso 1 1 calc R . . H15C H 0.4753 0.1000 0.0850 0.118 Uiso 1 1 calc R . . C16 C 0.6711(5) -0.0987(4) 0.2945(4) 0.0676(18) Uani 1 1 d . . . H16A H 0.7474 -0.0869 0.3232 0.101 Uiso 1 1 calc R . . H16B H 0.6718 -0.1394 0.2471 0.101 Uiso 1 1 calc R . . H16C H 0.6297 -0.1255 0.3347 0.101 Uiso 1 1 calc R . . C17 C 0.4936(5) -0.0295(4) 0.2140(4) 0.0722(19) Uani 1 1 d . . . H17A H 0.4960 -0.0679 0.1651 0.108 Uiso 1 1 calc R . . H17B H 0.4553 0.0258 0.1945 0.108 Uiso 1 1 calc R . . H17C H 0.4537 -0.0596 0.2533 0.108 Uiso 1 1 calc R . . C18 C 0.6086(5) 0.0524(4) 0.3369(4) 0.0636(16) Uani 1 1 d . . . H18A H 0.6843 0.0653 0.3665 0.095 Uiso 1 1 calc R . . H18B H 0.5677 0.0226 0.3757 0.095 Uiso 1 1 calc R . . H18C H 0.5710 0.1078 0.3170 0.095 Uiso 1 1 calc R . . C19 C 1.1213(5) 0.0612(4) 0.4638(3) 0.0631(16) Uani 1 1 d . . . H19A H 1.0401 0.0644 0.4540 0.095 Uiso 1 1 calc R . . H19B H 1.1522 0.1212 0.4669 0.095 Uiso 1 1 calc R . . H19C H 1.1484 0.0301 0.5173 0.095 Uiso 1 1 calc R . . C20 C 1.2887(5) 0.0065(6) 0.4052(4) 0.088(2) Uani 1 1 d . . . H20A H 1.3123 -0.0260 0.3588 0.132 Uiso 1 1 calc R . . H20B H 1.3167 -0.0236 0.4590 0.132 Uiso 1 1 calc R . . H20C H 1.3184 0.0668 0.4074 0.132 Uiso 1 1 calc R . . C21 C 1.1116(6) -0.0862(4) 0.3904(4) 0.0715(19) Uani 1 1 d . . . H21A H 1.0304 -0.0843 0.3811 0.107 Uiso 1 1 calc R . . H21B H 1.1403 -0.1138 0.4454 0.107 Uiso 1 1 calc R . . H21C H 1.1350 -0.1208 0.3452 0.107 Uiso 1 1 calc R . . C22 C 1.1562(5) 0.2387(4) 0.3386(4) 0.0681(18) Uani 1 1 d . . . H22A H 1.2036 0.2153 0.3898 0.102 Uiso 1 1 calc R . . H22B H 1.0802 0.2453 0.3485 0.102 Uiso 1 1 calc R . . H22C H 1.1844 0.2965 0.3247 0.102 Uiso 1 1 calc R . . C23 C 1.2768(5) 0.1660(4) 0.2449(4) 0.077(2) Uani 1 1 d . . . H23A H 1.3260 0.1406 0.2942 0.116 Uiso 1 1 calc R . . H23B H 1.3037 0.2249 0.2330 0.116 Uiso 1 1 calc R . . H23C H 1.2758 0.1277 0.1955 0.116 Uiso 1 1 calc R . . C24 C 1.0790(5) 0.2160(4) 0.1845(4) 0.0734(19) Uani 1 1 d . . . H24A H 1.0769 0.1774 0.1352 0.110 Uiso 1 1 calc R . . H24B H 1.1077 0.2742 0.1727 0.110 Uiso 1 1 calc R . . H24C H 1.0039 0.2224 0.1964 0.110 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 0.03177(10) 0.03840(12) 0.03543(10) -0.00339(10) 0.00513(7) 0.00168(10) P1 0.0298(6) 0.0448(8) 0.0417(7) -0.0013(7) 0.0070(5) 0.0018(6) Cl1 0.0457(8) 0.0652(10) 0.0593(8) -0.0271(8) 0.0052(7) 0.0014(7) C1 0.047(3) 0.042(3) 0.030(2) -0.001(2) 0.009(2) 0.010(2) P2 0.0308(7) 0.0367(8) 0.0402(7) -0.0020(6) -0.0011(6) 0.0017(6) C2 0.051(3) 0.046(4) 0.035(3) 0.000(2) 0.009(2) 0.009(3) C3 0.067(4) 0.060(4) 0.045(3) -0.003(3) 0.012(3) 0.025(3) C4 0.096(5) 0.053(4) 0.046(3) -0.011(3) 0.015(3) 0.019(4) C5 0.068(4) 0.054(4) 0.043(3) -0.015(3) 0.005(3) 0.007(3) C6 0.046(3) 0.040(3) 0.040(3) -0.005(2) 0.005(2) 0.003(2) C7 0.045(3) 0.051(4) 0.043(3) -0.007(3) 0.002(2) 0.001(3) C8 0.051(3) 0.054(4) 0.046(3) 0.003(3) 0.015(3) 0.013(3) C9 0.044(3) 0.042(3) 0.051(3) 0.006(3) -0.007(3) 0.006(3) C10 0.036(3) 0.037(3) 0.054(3) -0.007(3) 0.011(2) -0.004(2) C11 0.044(3) 0.064(4) 0.042(3) 0.004(3) 0.003(3) 0.007(3) C12 0.041(3) 0.056(4) 0.062(3) 0.005(3) 0.014(3) -0.009(3) C13 0.085(5) 0.068(5) 0.074(4) 0.031(4) 0.009(4) 0.011(4) C14 0.081(5) 0.040(4) 0.087(5) -0.005(3) -0.008(4) 0.017(3) C15 0.067(4) 0.070(5) 0.080(4) 0.001(4) -0.032(4) 0.006(4) C16 0.064(4) 0.058(4) 0.086(4) 0.014(4) 0.026(4) 0.006(3) C17 0.047(4) 0.083(5) 0.085(5) -0.012(4) 0.008(3) -0.014(3) C18 0.067(4) 0.066(4) 0.064(4) -0.010(3) 0.028(3) -0.007(3) C19 0.074(4) 0.072(4) 0.044(3) -0.002(3) 0.013(3) -0.008(4) C20 0.043(4) 0.152(7) 0.066(4) 0.025(5) 0.003(3) 0.020(4) C21 0.097(5) 0.068(5) 0.046(3) 0.010(3) 0.003(3) 0.010(4) C22 0.058(4) 0.070(5) 0.077(4) -0.008(4) 0.015(3) -0.014(3) C23 0.054(4) 0.069(5) 0.118(6) 0.012(4) 0.040(4) -0.002(3) C24 0.076(5) 0.066(5) 0.075(4) 0.019(4) 0.006(4) -0.010(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 2.065(4) . ? Pt1 P1 2.3028(12) . ? Pt1 P2 2.3078(12) . ? Pt1 Cl1 2.4342(13) . ? P1 C8 1.847(5) . ? P1 C11 1.881(5) . ? P1 C12 1.901(6) . ? C1 C2 1.535(7) . ? C1 C6 1.537(7) . ? C1 H1 0.9800 . ? P2 C7 1.837(5) . ? P2 C9 1.875(5) . ? P2 C10 1.876(5) . ? C2 C3 1.524(6) . ? C2 C8 1.533(7) . ? C2 H2 0.9800 . ? C3 C4 1.516(8) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 C5 1.525(7) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C6 1.529(6) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 C7 1.519(7) . ? C6 H6 0.9800 . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C14 1.508(7) . ? C9 C15 1.532(7) . ? C9 C13 1.535(7) . ? C10 C17 1.514(7) . ? C10 C18 1.522(7) . ? C10 C16 1.555(7) . ? C11 C19 1.523(7) . ? C11 C21 1.531(8) . ? C11 C20 1.544(7) . ? C12 C22 1.519(7) . ? C12 C23 1.529(7) . ? C12 C24 1.543(7) . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? 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 H16C 0.9600 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 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 84.32(14) . . ? C1 Pt1 P2 83.41(14) . . ? P1 Pt1 P2 167.60(5) . . ? C1 Pt1 Cl1 175.60(14) . . ? P1 Pt1 Cl1 95.89(5) . . ? P2 Pt1 Cl1 96.20(4) . . ? C8 P1 C11 105.1(2) . . ? C8 P1 C12 104.0(2) . . ? C11 P1 C12 111.7(3) . . ? C8 P1 Pt1 102.79(17) . . ? C11 P1 Pt1 117.32(17) . . ? C12 P1 Pt1 114.07(18) . . ? C2 C1 C6 110.0(4) . . ? C2 C1 Pt1 115.1(3) . . ? C6 C1 Pt1 114.8(3) . . ? C2 C1 H1 105.3 . . ? C6 C1 H1 105.3 . . ? Pt1 C1 H1 105.3 . . ? C7 P2 C9 104.7(2) . . ? C7 P2 C10 104.0(2) . . ? C9 P2 C10 111.9(2) . . ? C7 P2 Pt1 102.93(17) . . ? C9 P2 Pt1 114.33(17) . . ? C10 P2 Pt1 116.99(16) . . ? C3 C2 C8 112.6(4) . . ? C3 C2 C1 112.0(4) . . ? C8 C2 C1 110.5(4) . . ? C3 C2 H2 107.1 . . ? C8 C2 H2 107.1 . . ? C1 C2 H2 107.1 . . ? C4 C3 C2 111.1(5) . . ? C4 C3 H3A 109.4 . . ? C2 C3 H3A 109.4 . . ? C4 C3 H3B 109.4 . . ? C2 C3 H3B 109.4 . . ? H3A C3 H3B 108.0 . . ? C3 C4 C5 111.5(5) . . ? C3 C4 H4A 109.3 . . ? C5 C4 H4A 109.3 . . ? C3 C4 H4B 109.3 . . ? C5 C4 H4B 109.3 . . ? H4A C4 H4B 108.0 . . ? C4 C5 C6 111.7(4) . . ? C4 C5 H5A 109.3 . . ? C6 C5 H5A 109.3 . . ? C4 C5 H5B 109.3 . . ? C6 C5 H5B 109.3 . . ? H5A C5 H5B 107.9 . . ? C7 C6 C5 111.9(4) . . ? C7 C6 C1 109.7(4) . . ? C5 C6 C1 112.5(4) . . ? C7 C6 H6 107.5 . . ? C5 C6 H6 107.5 . . ? C1 C6 H6 107.5 . . ? C6 C7 P2 109.9(3) . . ? C6 C7 H7A 109.7 . . ? P2 C7 H7A 109.7 . . ? C6 C7 H7B 109.7 . . ? P2 C7 H7B 109.7 . . ? H7A C7 H7B 108.2 . . ? C2 C8 P1 108.3(3) . . ? C2 C8 H8A 110.0 . . ? P1 C8 H8A 110.0 . . ? C2 C8 H8B 110.0 . . ? P1 C8 H8B 110.0 . . ? H8A C8 H8B 108.4 . . ? C14 C9 C15 109.4(5) . . ? C14 C9 C13 107.4(5) . . ? C15 C9 C13 107.9(5) . . ? C14 C9 P2 111.7(4) . . ? C15 C9 P2 114.7(4) . . ? C13 C9 P2 105.2(4) . . ? C17 C10 C18 109.1(4) . . ? C17 C10 C16 108.3(5) . . ? C18 C10 C16 108.0(4) . . ? C17 C10 P2 114.7(4) . . ? C18 C10 P2 110.4(3) . . ? C16 C10 P2 106.1(3) . . ? C19 C11 C21 107.3(5) . . ? C19 C11 C20 109.2(5) . . ? C21 C11 C20 109.2(5) . . ? C19 C11 P1 110.1(4) . . ? C21 C11 P1 106.4(4) . . ? C20 C11 P1 114.4(4) . . ? C22 C12 C23 109.9(5) . . ? C22 C12 C24 106.3(5) . . ? C23 C12 C24 109.0(5) . . ? C22 C12 P1 111.5(4) . . ? C23 C12 P1 113.9(4) . . ? C24 C12 P1 105.8(4) . . ? C9 C13 H13A 109.5 . . ? C9 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C9 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C9 C14 H14A 109.5 . . ? C9 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C9 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? 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 . . ? C10 C16 H16A 109.5 . . ? C10 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C10 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C10 C17 H17A 109.5 . . ? C10 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C10 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C10 C18 H18A 109.5 . . ? C10 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C10 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C11 C19 H19A 109.5 . . ? C11 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C11 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C11 C20 H20A 109.5 . . ? C11 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C11 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C11 C21 H21A 109.5 . . ? C11 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C11 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C12 C22 H22A 109.5 . . ? C12 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C12 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C12 C23 H23A 109.5 . . ? C12 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C12 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C12 C24 H24A 109.5 . . ? C12 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C12 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.916 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 2.658 _refine_diff_density_min -0.847 _refine_diff_density_rms 0.250