Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2005 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'P. Pringle' 'R. Angharad Baber' 'Simon Collard' 'Mark Hooper' 'A. Orpen' 'Matthew J. Wilkinson' 'Richard L. Wingad' _publ_contact_author_name 'Prof P. Pringle' _publ_contact_author_address ; School of Chemistry University of Bristol Cantock's Close BRISTOL BS8 1TS UK ; _publ_contact_author_email PAUL.PRINGLE@BRIS.AC.UK _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Bulky triarylarsines are effective ligands for palladium catalysed Heck olefination ; data_4a _database_code_depnum_ccdc_archive 'CCDC 256982' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[PdCl2(2a)2]' _chemical_formula_sum 'C42 H42 As2 Cl2 Pd' _chemical_formula_weight 873.90 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' As As 0.0499 2.0058 '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 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 10.6786(18) _cell_length_b 10.9964(19) _cell_length_c 15.825(3) _cell_angle_alpha 90.00 _cell_angle_beta 93.093(3) _cell_angle_gamma 90.00 _cell_volume 1855.6(5) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.564 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 880 _exptl_absorpt_coefficient_mu 2.443 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.660167 _exptl_absorpt_correction_T_max 0.862073 _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 'omega scans with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19130 _diffrn_reflns_av_R_equivalents 0.0891 _diffrn_reflns_av_sigmaI/netI 0.0773 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.25 _diffrn_reflns_theta_max 27.59 _reflns_number_total 4250 _reflns_number_gt 2943 _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^)+(0.0323P)^2^+1.6081P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4250 _refine_ls_number_parameters 217 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0862 _refine_ls_R_factor_gt 0.0470 _refine_ls_wR_factor_ref 0.0901 _refine_ls_wR_factor_gt 0.0801 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.041 _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 Pd1 Pd 1.0000 0.0000 0.0000 0.01811(13) Uani 1 2 d S . . As1 As 0.90413(4) 0.12067(4) 0.10778(3) 0.01832(12) Uani 1 1 d . . . Cl1 Cl 0.87258(10) -0.15940(10) 0.03469(7) 0.0241(3) Uani 1 1 d . . . C1 C 0.9185(4) 0.0591(4) 0.2229(3) 0.0204(10) Uani 1 1 d . . . C2 C 0.9761(4) -0.0550(4) 0.2341(3) 0.0274(11) Uani 1 1 d . . . H2 H 1.0025 -0.0984 0.1863 0.033 Uiso 1 1 calc R . . C3 C 0.9949(5) -0.1049(5) 0.3138(3) 0.0357(13) Uani 1 1 d . . . H3 H 1.0343 -0.1820 0.3206 0.043 Uiso 1 1 calc R . . C4 C 0.9567(5) -0.0432(5) 0.3832(3) 0.0368(13) Uani 1 1 d . . . H4 H 0.9686 -0.0779 0.4380 0.044 Uiso 1 1 calc R . . C5 C 0.9005(5) 0.0702(5) 0.3730(3) 0.0358(13) Uani 1 1 d . . . H5 H 0.8754 0.1125 0.4216 0.043 Uiso 1 1 calc R . . C6 C 0.8794(4) 0.1244(4) 0.2930(3) 0.0253(10) Uani 1 1 d . . . C7 C 0.8207(5) 0.2484(5) 0.2883(3) 0.0343(12) Uani 1 1 d . . . H7A H 0.8858 0.3097 0.2808 0.051 Uiso 1 1 calc R . . H7B H 0.7791 0.2649 0.3408 0.051 Uiso 1 1 calc R . . H7C H 0.7589 0.2517 0.2403 0.051 Uiso 1 1 calc R . . C8 C 0.9639(4) 0.2869(4) 0.1216(3) 0.0260(11) Uani 1 1 d . . . C9 C 1.0864(4) 0.3071(4) 0.1569(3) 0.0278(11) Uani 1 1 d . . . C10 C 1.1255(6) 0.4292(5) 0.1671(3) 0.0431(15) Uani 1 1 d . . . H10 H 1.2071 0.4458 0.1912 0.052 Uiso 1 1 calc R . . C11 C 1.0486(6) 0.5246(5) 0.1430(4) 0.0499(16) Uani 1 1 d . . . H11 H 1.0775 0.6057 0.1508 0.060 Uiso 1 1 calc R . . C12 C 0.9296(6) 0.5034(5) 0.1076(3) 0.0455(14) Uani 1 1 d . . . H12 H 0.8769 0.5694 0.0902 0.055 Uiso 1 1 calc R . . C13 C 0.8877(5) 0.3832(4) 0.0976(3) 0.0347(12) Uani 1 1 d . . . H13 H 0.8055 0.3680 0.0740 0.042 Uiso 1 1 calc R . . C14 C 1.1747(4) 0.2063(5) 0.1860(3) 0.0349(13) Uani 1 1 d . . . H14A H 1.1480 0.1728 0.2395 0.052 Uiso 1 1 calc R . . H14B H 1.2599 0.2388 0.1942 0.052 Uiso 1 1 calc R . . H14C H 1.1734 0.1420 0.1431 0.052 Uiso 1 1 calc R . . C15 C 0.7240(4) 0.1297(4) 0.0821(3) 0.0216(10) Uani 1 1 d . . . C16 C 0.6427(4) 0.0859(4) 0.1410(3) 0.0255(11) Uani 1 1 d . . . H16 H 0.6754 0.0554 0.1939 0.031 Uiso 1 1 calc R . . C17 C 0.5143(5) 0.0867(4) 0.1227(3) 0.0333(12) Uani 1 1 d . . . H17 H 0.4590 0.0569 0.1630 0.040 Uiso 1 1 calc R . . C18 C 0.4669(5) 0.1310(5) 0.0454(3) 0.0376(13) Uani 1 1 d . . . H18 H 0.3789 0.1334 0.0331 0.045 Uiso 1 1 calc R . . C19 C 0.5475(5) 0.1714(4) -0.0132(3) 0.0351(13) Uani 1 1 d . . . H19 H 0.5138 0.2009 -0.0661 0.042 Uiso 1 1 calc R . . C20 C 0.6766(5) 0.1705(4) 0.0024(3) 0.0263(11) Uani 1 1 d . . . C21 C 0.7580(5) 0.2088(5) -0.0678(3) 0.0447(15) Uani 1 1 d . . . H21A H 0.7720 0.1391 -0.1046 0.067 Uiso 1 1 calc R . . H21B H 0.8387 0.2383 -0.0435 0.067 Uiso 1 1 calc R . . H21C H 0.7161 0.2739 -0.1008 0.067 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 0.0185(3) 0.0191(3) 0.0173(2) -0.0003(2) 0.00603(19) 0.0004(2) As1 0.0184(2) 0.0194(2) 0.0175(2) 0.0002(2) 0.00413(17) 0.0016(2) Cl1 0.0256(6) 0.0240(6) 0.0238(6) 0.0000(5) 0.0110(5) -0.0058(5) C1 0.017(2) 0.023(2) 0.022(2) 0.001(2) 0.0003(18) -0.0032(19) C2 0.020(3) 0.032(3) 0.030(3) 0.001(2) 0.003(2) 0.000(2) C3 0.037(3) 0.033(3) 0.037(3) 0.014(2) -0.007(2) -0.004(2) C4 0.042(3) 0.041(3) 0.027(3) 0.012(2) -0.006(2) -0.008(3) C5 0.039(3) 0.049(4) 0.019(3) -0.002(2) 0.002(2) -0.017(3) C6 0.024(3) 0.028(3) 0.024(2) -0.005(2) 0.0006(19) -0.006(2) C7 0.038(3) 0.041(3) 0.024(3) -0.010(2) 0.010(2) 0.003(3) C8 0.032(3) 0.026(3) 0.021(2) -0.003(2) 0.013(2) -0.003(2) C9 0.026(3) 0.032(3) 0.026(3) -0.005(2) 0.009(2) -0.007(2) C10 0.044(4) 0.044(4) 0.044(3) -0.014(3) 0.016(3) -0.020(3) C11 0.065(4) 0.026(3) 0.061(4) -0.011(3) 0.025(3) -0.016(3) C12 0.059(4) 0.023(3) 0.056(4) 0.001(3) 0.020(3) 0.003(3) C13 0.039(3) 0.025(3) 0.041(3) 0.003(2) 0.012(2) 0.004(2) C14 0.025(3) 0.045(3) 0.035(3) -0.007(2) -0.002(2) -0.006(2) C15 0.018(2) 0.019(2) 0.028(2) -0.007(2) 0.0001(19) 0.0018(19) C16 0.024(3) 0.022(3) 0.030(3) -0.008(2) 0.002(2) -0.001(2) C17 0.029(3) 0.029(3) 0.042(3) -0.011(2) 0.009(2) -0.003(2) C18 0.024(3) 0.031(3) 0.056(4) -0.020(3) -0.011(3) 0.005(2) C19 0.039(3) 0.027(3) 0.038(3) -0.002(2) -0.013(3) 0.008(2) C20 0.032(3) 0.024(3) 0.023(2) -0.006(2) -0.001(2) 0.007(2) C21 0.049(4) 0.055(4) 0.030(3) 0.010(3) -0.001(3) 0.006(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 Cl1 2.3034(11) . ? Pd1 Cl1 2.3034(11) 3_755 ? Pd1 As1 2.4303(5) 3_755 ? Pd1 As1 2.4303(5) . ? As1 C1 1.941(4) . ? As1 C8 1.944(5) . ? As1 C15 1.947(4) . ? C1 C6 1.404(6) . ? C1 C2 1.405(6) . ? C2 C3 1.379(6) . ? C2 H2 0.9500 . ? C3 C4 1.371(7) . ? C3 H3 0.9500 . ? C4 C5 1.390(7) . ? C4 H4 0.9500 . ? C5 C6 1.406(6) . ? C5 H5 0.9500 . ? C6 C7 1.502(7) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 C13 1.376(7) . ? C8 C9 1.412(7) . ? C9 C10 1.413(7) . ? C9 C14 1.510(7) . ? C10 C11 1.373(8) . ? C10 H10 0.9500 . ? C11 C12 1.380(8) . ? C11 H11 0.9500 . ? C12 C13 1.402(7) . ? C12 H12 0.9500 . ? C13 H13 0.9500 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C16 1.393(6) . ? C15 C20 1.408(6) . ? C16 C17 1.386(6) . ? C16 H16 0.9500 . ? C17 C18 1.386(7) . ? C17 H17 0.9500 . ? C18 C19 1.373(7) . ? C18 H18 0.9500 . ? C19 C20 1.388(7) . ? C19 H19 0.9500 . ? C20 C21 1.506(6) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 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 Cl1 Pd1 Cl1 180.00(7) . 3_755 ? Cl1 Pd1 As1 91.63(3) . 3_755 ? Cl1 Pd1 As1 88.37(3) 3_755 3_755 ? Cl1 Pd1 As1 88.37(3) . . ? Cl1 Pd1 As1 91.63(3) 3_755 . ? As1 Pd1 As1 180.000(14) 3_755 . ? C1 As1 C8 102.32(19) . . ? C1 As1 C15 103.92(18) . . ? C8 As1 C15 106.86(19) . . ? C1 As1 Pd1 116.94(13) . . ? C8 As1 Pd1 116.35(12) . . ? C15 As1 Pd1 109.31(13) . . ? C6 C1 C2 120.2(4) . . ? C6 C1 As1 123.5(3) . . ? C2 C1 As1 116.2(3) . . ? C3 C2 C1 120.8(5) . . ? C3 C2 H2 119.6 . . ? C1 C2 H2 119.6 . . ? C4 C3 C2 120.1(5) . . ? C4 C3 H3 120.0 . . ? C2 C3 H3 120.0 . . ? C3 C4 C5 119.7(5) . . ? C3 C4 H4 120.1 . . ? C5 C4 H4 120.1 . . ? C4 C5 C6 122.1(5) . . ? C4 C5 H5 119.0 . . ? C6 C5 H5 119.0 . . ? C1 C6 C5 117.1(4) . . ? C1 C6 C7 124.5(4) . . ? C5 C6 C7 118.4(4) . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C13 C8 C9 120.6(5) . . ? C13 C8 As1 120.4(4) . . ? C9 C8 As1 118.9(4) . . ? C8 C9 C10 117.1(5) . . ? C8 C9 C14 123.7(4) . . ? C10 C9 C14 119.1(5) . . ? C11 C10 C9 121.7(5) . . ? C11 C10 H10 119.1 . . ? C9 C10 H10 119.1 . . ? C10 C11 C12 120.5(5) . . ? C10 C11 H11 119.8 . . ? C12 C11 H11 119.8 . . ? C11 C12 C13 119.1(5) . . ? C11 C12 H12 120.5 . . ? C13 C12 H12 120.5 . . ? C8 C13 C12 120.9(5) . . ? C8 C13 H13 119.5 . . ? C12 C13 H13 119.5 . . ? 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 . . ? C16 C15 C20 120.2(4) . . ? C16 C15 As1 119.2(3) . . ? C20 C15 As1 120.4(3) . . ? C17 C16 C15 120.2(5) . . ? C17 C16 H16 119.9 . . ? C15 C16 H16 119.9 . . ? C18 C17 C16 119.7(5) . . ? C18 C17 H17 120.1 . . ? C16 C17 H17 120.1 . . ? C19 C18 C17 119.9(5) . . ? C19 C18 H18 120.1 . . ? C17 C18 H18 120.1 . . ? C18 C19 C20 122.0(5) . . ? C18 C19 H19 119.0 . . ? C20 C19 H19 119.0 . . ? C19 C20 C15 117.9(4) . . ? C19 C20 C21 118.3(4) . . ? C15 C20 C21 123.8(4) . . ? 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 . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 27.59 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.651 _refine_diff_density_min -0.720 _refine_diff_density_rms 0.126 data_3d.3CH2Cl2robots _database_code_depnum_ccdc_archive 'CCDC 256983' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C60 H78 As2 Cl2 O6 Pt,3(CH2Cl2)' _chemical_formula_sum 'C63 H84 As2 Cl8 O6 Pt' _chemical_formula_weight 1565.83 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' As As 0.0499 2.0058 '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/n _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 14.116(3) _cell_length_b 24.806(5) _cell_length_c 19.594(4) _cell_angle_alpha 90.00 _cell_angle_beta 99.57(3) _cell_angle_gamma 90.00 _cell_volume 6766(2) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 10948 _cell_measurement_theta_min 2.2625 _cell_measurement_theta_max 27.4835 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.537 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3160 _exptl_absorpt_coefficient_mu 3.408 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.49 _exptl_absorpt_correction_T_max 0.51 _exptl_absorpt_process_details 'SADABS (Sheldrick 1996)' _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 '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 47826 _diffrn_reflns_av_R_equivalents 0.0553 _diffrn_reflns_av_sigmaI/netI 0.0657 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.34 _diffrn_reflns_theta_max 27.48 _reflns_number_total 15511 _reflns_number_gt 13305 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _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^)+(0.0497P)^2^+93.9988P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 15511 _refine_ls_number_parameters 739 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0781 _refine_ls_R_factor_gt 0.0654 _refine_ls_wR_factor_ref 0.1636 _refine_ls_wR_factor_gt 0.1558 _refine_ls_goodness_of_fit_ref 1.096 _refine_ls_restrained_S_all 1.096 _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 0.000355(18) 0.848569(10) 0.261699(13) 0.01023(8) Uani 1 1 d . . . As1 As -0.15991(5) 0.84364(3) 0.29025(3) 0.01088(14) Uani 1 1 d . . . As2 As 0.15616(5) 0.86114(3) 0.22746(4) 0.01048(14) Uani 1 1 d . . . Cl1 Cl 0.02027(13) 0.75694(7) 0.26873(10) 0.0201(4) Uani 1 1 d . . . Cl2 Cl -0.01787(12) 0.94121(7) 0.25677(9) 0.0159(3) Uani 1 1 d . . . C14 C -0.1418(6) 0.8042(4) 0.0872(4) 0.0245(17) Uani 1 1 d . . . H14A H -0.1695 0.8230 0.0446 0.037 Uiso 1 1 calc R . . H14B H -0.1151 0.7695 0.0756 0.037 Uiso 1 1 calc R . . H14C H -0.0906 0.8263 0.1133 0.037 Uiso 1 1 calc R . . C15 C -0.2941(6) 0.7543(3) 0.0954(4) 0.0242(17) Uani 1 1 d . . . H15A H -0.3483 0.7519 0.1207 0.036 Uiso 1 1 calc R . . H15B H -0.2641 0.7188 0.0941 0.036 Uiso 1 1 calc R . . H15C H -0.3173 0.7666 0.0480 0.036 Uiso 1 1 calc R . . C29 C -0.3488(5) 0.7124(3) 0.2904(4) 0.0185(15) Uani 1 1 d . . . H29 H -0.4050 0.7001 0.2610 0.022 Uiso 1 1 calc R . . C45 C 0.3213(6) 0.8014(3) 0.4351(4) 0.0249(17) Uani 1 1 d . . . H45A H 0.3735 0.7980 0.4080 0.037 Uiso 1 1 calc R . . H45B H 0.2997 0.7654 0.4463 0.037 Uiso 1 1 calc R . . H45C H 0.3445 0.8211 0.4780 0.037 Uiso 1 1 calc R . . C32 C -0.1772(5) 0.7459(3) 0.3740(4) 0.0156(14) Uani 1 1 d . . . C65 C 0.0675(6) 0.7049(3) 0.1071(4) 0.0237(17) Uani 1 1 d . . . H65A H 0.1051 0.6804 0.0828 0.036 Uiso 1 1 calc R . . H65B H 0.0022 0.7080 0.0809 0.036 Uiso 1 1 calc R . . H65C H 0.0646 0.6906 0.1533 0.036 Uiso 1 1 calc R . . C56 C 0.1748(6) 0.9922(4) -0.0844(5) 0.0290(19) Uani 1 1 d . . . H56A H 0.2084 1.0196 -0.0534 0.044 Uiso 1 1 calc R . . H56B H 0.1483 1.0089 -0.1288 0.044 Uiso 1 1 calc R . . H56C H 0.2199 0.9637 -0.0919 0.044 Uiso 1 1 calc R . . C50 C 0.1217(6) 0.9465(3) 0.0094(4) 0.0193(15) Uani 1 1 d . . . C58 C 0.3290(5) 0.7974(3) 0.2534(4) 0.0169(15) Uani 1 1 d . . . H58 H 0.3480 0.8246 0.2870 0.020 Uiso 1 1 calc R . . C27 C -0.2163(5) 0.7762(3) 0.3139(4) 0.0116(13) Uani 1 1 d . . . O16 O 0.4314(4) 0.6774(2) 0.1912(3) 0.0308(15) Uani 1 1 d . . . C10 C -0.3589(5) 0.9263(3) 0.1007(4) 0.0176(15) Uani 1 1 d . . . C47 C 0.1504(5) 0.9003(3) 0.1401(3) 0.0124(13) Uani 1 1 d . . . C44 C 0.1576(5) 0.8417(3) 0.4359(4) 0.0203(16) Uani 1 1 d . . . H44A H 0.1837 0.8620 0.4777 0.030 Uiso 1 1 calc R . . H44B H 0.1330 0.8069 0.4489 0.030 Uiso 1 1 calc R . . H44C H 0.1053 0.8623 0.4086 0.030 Uiso 1 1 calc R . . C57 C 0.2371(5) 0.7995(3) 0.2135(4) 0.0112(13) Uani 1 1 d . . . C17 C -0.1803(5) 0.8889(3) 0.3684(3) 0.0110(13) Uani 1 1 d . . . C49 C 0.0421(5) 0.9316(3) 0.0398(4) 0.0164(14) Uani 1 1 d . . . H49 H -0.0215 0.9367 0.0158 0.020 Uiso 1 1 calc R . . C37 C 0.2364(5) 0.9044(3) 0.2974(4) 0.0139(14) Uani 1 1 d . . . C48 C 0.0584(6) 0.9096(3) 0.1049(4) 0.0164(14) Uani 1 1 d . . . H48 H 0.0051 0.9004 0.1264 0.020 Uiso 1 1 calc R . . C38 C 0.2594(5) 0.9560(3) 0.2788(4) 0.0155(14) Uani 1 1 d . . . H38 H 0.2345 0.9689 0.2337 0.019 Uiso 1 1 calc R . . C64 C 0.1267(6) 0.7812(3) 0.0421(4) 0.0234(17) Uani 1 1 d . . . H64A H 0.1528 0.8178 0.0465 0.035 Uiso 1 1 calc R . . H64B H 0.0641 0.7815 0.0117 0.035 Uiso 1 1 calc R . . H64C H 0.1709 0.7576 0.0223 0.035 Uiso 1 1 calc R . . C12 C -0.2647(5) 0.8489(3) 0.1466(4) 0.0128(13) Uani 1 1 d . . . C8 C -0.2819(5) 0.9255(3) 0.2184(4) 0.0166(14) Uani 1 1 d . . . H8 H -0.2663 0.9432 0.2619 0.020 Uiso 1 1 calc R . . C24 C -0.4398(6) 0.9187(3) 0.3396(4) 0.0229(17) Uani 1 1 d . . . H24A H -0.5005 0.9034 0.3160 0.034 Uiso 1 1 calc R . . H24B H -0.4170 0.9459 0.3099 0.034 Uiso 1 1 calc R . . H24C H -0.4497 0.9354 0.3832 0.034 Uiso 1 1 calc R . . C63 C 0.1147(5) 0.7601(3) 0.1137(4) 0.0160(14) Uani 1 1 d . . . H63 H 0.0708 0.7853 0.1331 0.019 Uiso 1 1 calc R . . C11 C -0.3231(5) 0.8753(3) 0.0926(4) 0.0181(15) Uani 1 1 d . . . H11 H -0.3387 0.8579 0.0491 0.022 Uiso 1 1 calc R . . C28 C -0.3014(5) 0.7586(3) 0.2742(4) 0.0136(13) Uani 1 1 d . . . H28 H -0.3281 0.7789 0.2345 0.016 Uiso 1 1 calc R . . C18 C -0.0972(5) 0.9102(3) 0.4069(4) 0.0132(13) Uani 1 1 d . . . H18 H -0.0379 0.9056 0.3907 0.016 Uiso 1 1 calc R . . C9 C -0.3382(5) 0.9520(3) 0.1653(4) 0.0155(14) Uani 1 1 d . . . H9 H -0.3627 0.9870 0.1720 0.019 Uiso 1 1 calc R . . C33 C -0.0856(5) 0.7629(3) 0.4217(4) 0.0177(15) Uani 1 1 d . . . H33 H -0.0534 0.7917 0.3980 0.021 Uiso 1 1 calc R . . C60 C 0.3658(6) 0.7168(3) 0.1958(4) 0.0223(16) Uani 1 1 d . . . C25 C -0.4014(6) 0.8295(3) 0.3979(4) 0.0222(16) Uani 1 1 d . . . H25A H -0.3533 0.8008 0.4070 0.033 Uiso 1 1 calc R . . H25B H -0.4615 0.8147 0.3726 0.033 Uiso 1 1 calc R . . H25C H -0.4131 0.8447 0.4420 0.033 Uiso 1 1 calc R . . C43 C 0.2370(5) 0.8323(3) 0.3927(4) 0.0166(14) Uani 1 1 d . . . H43 H 0.2099 0.8095 0.3520 0.020 Uiso 1 1 calc R . . C23 C -0.3648(5) 0.8737(3) 0.3549(4) 0.0152(14) Uani 1 1 d . . . H23 H -0.3546 0.8576 0.3099 0.018 Uiso 1 1 calc R . . C40 C 0.3517(5) 0.9714(3) 0.3911(4) 0.0164(15) Uani 1 1 d . . . C41 C 0.3235(5) 0.9207(3) 0.4108(4) 0.0177(15) Uani 1 1 d . . . H41 H 0.3444 0.9092 0.4571 0.021 Uiso 1 1 calc R . . C39 C 0.3185(5) 0.9896(3) 0.3249(4) 0.0168(14) Uani 1 1 d . . . H39 H 0.3355 1.0244 0.3108 0.020 Uiso 1 1 calc R . . C7 C -0.2460(5) 0.8731(3) 0.2115(4) 0.0136(13) Uani 1 1 d . . . C20 C -0.1845(5) 0.9440(3) 0.4924(4) 0.0164(14) Uani 1 1 d . . . C26 C -0.1169(5) 1.0009(3) 0.5861(4) 0.0223(16) Uani 1 1 d . . . H26A H -0.0589 0.9787 0.5967 0.033 Uiso 1 1 calc R . . H26B H -0.1330 1.0157 0.6292 0.033 Uiso 1 1 calc R . . H26C H -0.1053 1.0305 0.5555 0.033 Uiso 1 1 calc R . . C19 C -0.0977(5) 0.9381(3) 0.4685(4) 0.0153(14) Uani 1 1 d . . . H19 H -0.0400 0.9528 0.4936 0.018 Uiso 1 1 calc R . . C21 C -0.2679(5) 0.9233(3) 0.4540(4) 0.0196(16) Uani 1 1 d . . . H21 H -0.3270 0.9283 0.4705 0.024 Uiso 1 1 calc R . . C35 C -0.0167(6) 0.7147(3) 0.4362(4) 0.0240(17) Uani 1 1 d . . . H35A H -0.0457 0.6871 0.4622 0.036 Uiso 1 1 calc R . . H35B H 0.0441 0.7267 0.4635 0.036 Uiso 1 1 calc R . . H35C H -0.0048 0.6994 0.3923 0.036 Uiso 1 1 calc R . . C46 C 0.4415(6) 1.0512(3) 0.4210(4) 0.0278(19) Uani 1 1 d . . . H46A H 0.4754 1.0474 0.3814 0.042 Uiso 1 1 calc R . . H46B H 0.4847 1.0674 0.4599 0.042 Uiso 1 1 calc R . . H46C H 0.3851 1.0743 0.4081 0.042 Uiso 1 1 calc R . . C61 C 0.2749(5) 0.7190(3) 0.1550(4) 0.0162(14) Uani 1 1 d . . . H61 H 0.2568 0.6919 0.1211 0.019 Uiso 1 1 calc R . . C13 C -0.2205(5) 0.7944(3) 0.1317(4) 0.0171(15) Uani 1 1 d . . . H13 H -0.1897 0.7783 0.1767 0.021 Uiso 1 1 calc R . . C22 C -0.2683(5) 0.8953(3) 0.3921(4) 0.0127(13) Uani 1 1 d . . . C51 C 0.2130(6) 0.9379(3) 0.0439(4) 0.0172(14) Uani 1 1 d . . . H51 H 0.2662 0.9483 0.0228 0.021 Uiso 1 1 calc R . . O15 O 0.4115(4) 0.9992(2) 0.4407(3) 0.0220(12) Uani 1 1 d . . . O17 O -0.1947(4) 0.9686(2) 0.5527(3) 0.0217(12) Uani 1 1 d . . . O14 O 0.0993(4) 0.9699(2) -0.0543(3) 0.0241(12) Uani 1 1 d . . . C62 C 0.2102(5) 0.7598(3) 0.1626(4) 0.0163(14) Uani 1 1 d . . . C42 C 0.2660(5) 0.8863(3) 0.3654(4) 0.0131(13) Uani 1 1 d . . . Cl7 Cl 0.7587(6) 0.3428(2) 0.5955(2) 0.154(3) Uani 1 1 d . . . C69 C 0.7834(10) 0.3347(5) 0.6816(6) 0.054(3) Uani 1 1 d . . . H69A H 0.7423 0.3059 0.6961 0.065 Uiso 1 1 calc R . . H69B H 0.8514 0.3241 0.6957 0.065 Uiso 1 1 calc R . . O12 O -0.3547(5) 0.6405(3) 0.3744(4) 0.0407(19) Uani 1 1 d . . . C53 C 0.3344(5) 0.9049(3) 0.1425(4) 0.0170(15) Uani 1 1 d . . . H53 H 0.3352 0.8920 0.1910 0.020 Uiso 1 1 calc R . . C54 C 0.3821(6) 0.8615(3) 0.1045(4) 0.0242(17) Uani 1 1 d . . . H54A H 0.3459 0.8277 0.1043 0.036 Uiso 1 1 calc R . . H54B H 0.4481 0.8558 0.1281 0.036 Uiso 1 1 calc R . . H54C H 0.3827 0.8730 0.0568 0.036 Uiso 1 1 calc R . . C52 C 0.2298(5) 0.9139(3) 0.1099(4) 0.0138(14) Uani 1 1 d . . . C59 C 0.3928(5) 0.7565(3) 0.2451(4) 0.0213(16) Uani 1 1 d . . . H59 H 0.4547 0.7557 0.2729 0.026 Uiso 1 1 calc R . . C31 C -0.2270(5) 0.7011(3) 0.3909(4) 0.0204(16) Uani 1 1 d . . . H31 H -0.2020 0.6812 0.4313 0.025 Uiso 1 1 calc R . . C55 C 0.3936(6) 0.9571(4) 0.1463(4) 0.0254(17) Uani 1 1 d . . . H55A H 0.3930 0.9712 0.0995 0.038 Uiso 1 1 calc R . . H55B H 0.4599 0.9496 0.1681 0.038 Uiso 1 1 calc R . . H55C H 0.3656 0.9839 0.1739 0.038 Uiso 1 1 calc R . . C30 C -0.3122(6) 0.6846(3) 0.3507(5) 0.0248(18) Uani 1 1 d . . . C66 C 0.4017(7) 0.6307(4) 0.1509(5) 0.034(2) Uani 1 1 d . . . H66A H 0.3476 0.6137 0.1681 0.052 Uiso 1 1 calc R . . H66B H 0.4553 0.6051 0.1545 0.052 Uiso 1 1 calc R . . H66C H 0.3819 0.6411 0.1024 0.052 Uiso 1 1 calc R . . C34 C -0.1086(6) 0.7857(4) 0.4897(4) 0.0292(19) Uani 1 1 d . . . H34A H -0.1545 0.8154 0.4797 0.044 Uiso 1 1 calc R . . H34B H -0.0494 0.7990 0.5180 0.044 Uiso 1 1 calc R . . H34C H -0.1365 0.7573 0.5149 0.044 Uiso 1 1 calc R . . C36 C -0.4543(9) 0.6321(6) 0.3462(10) 0.110(8) Uani 1 1 d . . . H36A H -0.4886 0.6665 0.3444 0.165 Uiso 1 1 calc R . . H36B H -0.4824 0.6068 0.3757 0.165 Uiso 1 1 calc R . . H36C H -0.4596 0.6172 0.2994 0.165 Uiso 1 1 calc R . . Cl6 Cl 0.6668(4) 0.56698(18) 0.2426(2) 0.0913(14) Uani 1 1 d . . . Cl5 Cl 0.6318(3) 0.58022(18) 0.0945(2) 0.0831(12) Uani 1 1 d . . . Cl3 Cl 0.8699(4) 0.6252(3) 0.1612(4) 0.133(2) Uani 1 1 d . . . O13 O -0.4152(4) 0.9555(2) 0.0505(3) 0.0220(12) Uani 1 1 d . . . C16 C -0.4413(6) 0.9318(3) -0.0157(4) 0.0236(17) Uani 1 1 d . . . H16A H -0.3832 0.9237 -0.0351 0.035 Uiso 1 1 calc R . . H16B H -0.4818 0.9568 -0.0463 0.035 Uiso 1 1 calc R . . H16C H -0.4769 0.8983 -0.0115 0.035 Uiso 1 1 calc R . . Cl8 Cl 0.7625(11) 0.3930(2) 0.7197(4) 0.284(8) Uani 1 1 d . . . Cl4 Cl 0.9506(9) 0.5934(3) 0.3000(6) 0.264(7) Uani 1 1 d . . . C68 C 0.6747(12) 0.5366(6) 0.1603(7) 0.076(5) Uani 1 1 d . . . H68A H 0.7424 0.5275 0.1582 0.092 Uiso 1 1 calc R . . H68B H 0.6367 0.5029 0.1549 0.092 Uiso 1 1 calc R . . C67 C 0.8868(16) 0.6240(16) 0.2478(10) 0.23(2) Uani 1 1 d . . . H67A H 0.9006 0.6621 0.2611 0.274 Uiso 1 1 calc R . . H67B H 0.8219 0.6167 0.2586 0.274 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 0.00957(12) 0.01245(13) 0.00897(13) -0.00105(9) 0.00239(9) 0.00021(9) As1 0.0105(3) 0.0125(3) 0.0097(3) -0.0016(2) 0.0017(2) -0.0003(2) As2 0.0114(3) 0.0108(3) 0.0097(3) -0.0007(2) 0.0029(2) 0.0011(2) Cl1 0.0198(9) 0.0165(8) 0.0260(10) -0.0002(7) 0.0098(7) 0.0004(7) Cl2 0.0158(8) 0.0160(8) 0.0170(8) -0.0014(6) 0.0055(6) 0.0014(6) C14 0.020(4) 0.033(5) 0.021(4) -0.006(3) 0.005(3) 0.003(3) C15 0.024(4) 0.024(4) 0.024(4) -0.002(3) 0.001(3) 0.005(3) C29 0.015(3) 0.015(3) 0.024(4) 0.005(3) -0.002(3) -0.002(3) C45 0.019(4) 0.029(4) 0.026(4) 0.007(3) 0.004(3) 0.005(3) C32 0.014(3) 0.015(3) 0.018(4) 0.003(3) 0.004(3) 0.001(3) C65 0.021(4) 0.024(4) 0.026(4) -0.010(3) 0.002(3) -0.001(3) C56 0.027(4) 0.033(5) 0.029(5) 0.009(4) 0.011(4) 0.001(4) C50 0.029(4) 0.016(4) 0.014(4) 0.001(3) 0.007(3) 0.003(3) C58 0.018(4) 0.021(4) 0.013(3) -0.004(3) 0.005(3) 0.000(3) C27 0.007(3) 0.014(3) 0.015(3) 0.001(3) 0.005(2) 0.004(2) O16 0.025(3) 0.031(3) 0.032(3) -0.015(3) -0.006(3) 0.019(3) C10 0.018(4) 0.017(4) 0.017(4) 0.006(3) 0.000(3) 0.000(3) C47 0.017(3) 0.015(3) 0.005(3) 0.000(2) 0.003(3) 0.002(3) C44 0.018(4) 0.026(4) 0.018(4) 0.006(3) 0.005(3) -0.004(3) C57 0.011(3) 0.010(3) 0.014(3) -0.002(2) 0.008(3) 0.005(2) C17 0.014(3) 0.016(3) 0.004(3) -0.003(2) 0.006(2) 0.000(3) C49 0.018(4) 0.017(4) 0.015(4) -0.003(3) 0.005(3) 0.002(3) C37 0.014(3) 0.015(3) 0.013(3) -0.001(3) 0.002(3) 0.004(3) C48 0.025(4) 0.014(3) 0.011(3) -0.002(3) 0.006(3) 0.004(3) C38 0.014(3) 0.021(4) 0.013(3) 0.001(3) 0.006(3) -0.004(3) C64 0.027(4) 0.025(4) 0.016(4) -0.004(3) -0.002(3) 0.004(3) C12 0.011(3) 0.016(3) 0.010(3) 0.001(3) -0.001(2) 0.000(3) C8 0.018(4) 0.015(3) 0.018(4) 0.000(3) 0.004(3) -0.004(3) C24 0.016(4) 0.029(4) 0.022(4) -0.007(3) 0.000(3) 0.009(3) C63 0.014(3) 0.020(4) 0.014(3) -0.001(3) 0.003(3) 0.003(3) C11 0.022(4) 0.016(4) 0.018(4) -0.001(3) 0.005(3) -0.005(3) C28 0.013(3) 0.017(3) 0.011(3) 0.002(3) 0.001(3) 0.002(3) C18 0.007(3) 0.020(4) 0.013(3) 0.000(3) 0.003(2) 0.002(3) C9 0.022(4) 0.007(3) 0.017(4) 0.000(3) 0.003(3) 0.000(3) C33 0.018(4) 0.016(4) 0.017(4) 0.006(3) -0.004(3) 0.005(3) C60 0.021(4) 0.026(4) 0.020(4) -0.002(3) 0.003(3) 0.008(3) C25 0.019(4) 0.029(4) 0.020(4) -0.002(3) 0.007(3) -0.008(3) C43 0.020(4) 0.015(3) 0.015(4) 0.002(3) 0.003(3) 0.000(3) C23 0.009(3) 0.025(4) 0.011(3) -0.003(3) 0.002(3) 0.001(3) C40 0.011(3) 0.022(4) 0.016(4) -0.008(3) 0.001(3) -0.007(3) C41 0.016(3) 0.020(4) 0.018(4) 0.002(3) 0.006(3) 0.002(3) C39 0.020(4) 0.015(3) 0.016(4) -0.003(3) 0.007(3) -0.003(3) C7 0.015(3) 0.016(3) 0.011(3) -0.001(3) 0.003(3) -0.004(3) C20 0.019(4) 0.016(3) 0.015(3) -0.003(3) 0.006(3) 0.000(3) C26 0.016(4) 0.031(4) 0.020(4) -0.012(3) 0.003(3) -0.001(3) C19 0.015(3) 0.018(3) 0.011(3) -0.003(3) -0.002(3) -0.003(3) C21 0.016(4) 0.025(4) 0.019(4) -0.006(3) 0.007(3) 0.000(3) C35 0.016(4) 0.028(4) 0.026(4) 0.007(3) -0.003(3) -0.001(3) C46 0.031(4) 0.028(4) 0.024(4) -0.011(3) 0.002(3) -0.013(4) C61 0.017(4) 0.015(3) 0.016(4) -0.005(3) 0.000(3) 0.000(3) C13 0.022(4) 0.016(3) 0.012(3) 0.002(3) -0.002(3) 0.006(3) C22 0.012(3) 0.014(3) 0.013(3) 0.000(3) 0.004(3) 0.000(3) C51 0.023(4) 0.016(3) 0.015(4) 0.000(3) 0.009(3) 0.001(3) O15 0.021(3) 0.023(3) 0.021(3) -0.007(2) 0.000(2) -0.007(2) O17 0.017(3) 0.028(3) 0.021(3) -0.011(2) 0.009(2) -0.006(2) O14 0.030(3) 0.029(3) 0.014(3) 0.013(2) 0.009(2) 0.004(2) C62 0.019(4) 0.013(3) 0.017(4) 0.002(3) 0.003(3) 0.001(3) C42 0.015(3) 0.013(3) 0.012(3) -0.003(3) 0.006(3) 0.002(3) Cl7 0.290(9) 0.118(4) 0.044(2) -0.002(2) 0.002(4) -0.114(5) C69 0.064(8) 0.053(7) 0.047(7) 0.011(6) 0.013(6) 0.011(6) O12 0.027(3) 0.034(4) 0.054(4) 0.031(3) -0.012(3) -0.017(3) C53 0.013(3) 0.022(4) 0.017(4) 0.001(3) 0.006(3) -0.002(3) C54 0.026(4) 0.022(4) 0.029(4) -0.001(3) 0.015(3) 0.000(3) C52 0.017(3) 0.012(3) 0.014(3) -0.004(3) 0.006(3) 0.000(3) C59 0.015(4) 0.027(4) 0.021(4) -0.003(3) 0.001(3) 0.004(3) C31 0.015(4) 0.023(4) 0.021(4) 0.008(3) -0.003(3) 0.000(3) C55 0.022(4) 0.031(4) 0.025(4) 0.004(3) 0.012(3) -0.006(3) C30 0.019(4) 0.023(4) 0.032(5) 0.011(3) 0.001(3) -0.008(3) C66 0.035(5) 0.030(5) 0.035(5) -0.016(4) -0.006(4) 0.019(4) C34 0.028(4) 0.039(5) 0.019(4) 0.003(4) 0.000(3) -0.001(4) C36 0.048(8) 0.099(12) 0.158(17) 0.100(12) -0.055(9) -0.059(8) Cl6 0.137(4) 0.077(3) 0.061(2) -0.003(2) 0.022(2) -0.028(3) Cl5 0.092(3) 0.081(3) 0.073(3) 0.013(2) 0.004(2) -0.023(2) Cl3 0.091(4) 0.122(5) 0.197(7) -0.007(5) 0.056(4) -0.009(3) O13 0.025(3) 0.020(3) 0.018(3) 0.003(2) -0.004(2) 0.004(2) C16 0.027(4) 0.024(4) 0.017(4) 0.006(3) -0.005(3) 0.001(3) Cl8 0.69(2) 0.081(4) 0.113(5) -0.050(4) 0.168(9) -0.146(8) Cl4 0.390(15) 0.103(5) 0.227(10) 0.024(6) -0.163(10) -0.025(7) C68 0.099(12) 0.068(9) 0.056(9) -0.019(7) -0.005(8) 0.008(8) C67 0.098(17) 0.52(6) 0.058(12) 0.09(2) -0.023(11) -0.12(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 Cl1 2.2915(19) . ? Pt1 Cl2 2.3127(18) . ? Pt1 As1 2.4221(9) . ? Pt1 As2 2.4238(9) . ? As1 C7 1.941(7) . ? As1 C27 1.943(7) . ? As1 C17 1.958(6) . ? As2 C37 1.950(7) . ? As2 C57 1.954(6) . ? As2 C47 1.958(7) . ? C14 C13 1.540(11) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C13 1.526(11) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C29 C30 1.390(11) . ? C29 C28 1.391(10) . ? C29 H29 0.9500 . ? C45 C43 1.538(10) . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C32 C31 1.383(10) . ? C32 C27 1.427(10) . ? C32 C33 1.524(10) . ? C65 C63 1.519(11) . ? C65 H65A 0.9800 . ? C65 H65B 0.9800 . ? C65 H65C 0.9800 . ? C56 O14 1.414(10) . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? C50 O14 1.365(9) . ? C50 C51 1.369(11) . ? C50 C49 1.406(10) . ? C58 C59 1.384(10) . ? C58 C57 1.400(10) . ? C58 H58 0.9500 . ? C27 C28 1.389(9) . ? O16 C60 1.360(9) . ? O16 C66 1.427(10) . ? C10 O13 1.364(8) . ? C10 C11 1.381(11) . ? C10 C9 1.405(10) . ? C47 C48 1.384(10) . ? C47 C52 1.393(10) . ? C44 C43 1.531(10) . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C57 C62 1.409(10) . ? C17 C18 1.390(9) . ? C17 C22 1.405(9) . ? C49 C48 1.371(10) . ? C49 H49 0.9500 . ? C37 C38 1.384(10) . ? C37 C42 1.402(10) . ? C48 H48 0.9500 . ? C38 C39 1.398(10) . ? C38 H38 0.9500 . ? C64 C63 1.531(11) . ? C64 H64A 0.9800 . ? C64 H64B 0.9800 . ? C64 H64C 0.9800 . ? C12 C7 1.390(10) . ? C12 C11 1.393(10) . ? C12 C13 1.537(10) . ? C8 C9 1.368(10) . ? C8 C7 1.411(10) . ? C8 H8 0.9500 . ? C24 C23 1.533(10) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C63 C62 1.518(10) . ? C63 H63 1.0000 . ? C11 H11 0.9500 . ? C28 H28 0.9500 . ? C18 C19 1.391(10) . ? C18 H18 0.9500 . ? C9 H9 0.9500 . ? C33 C34 1.531(11) . ? C33 C35 1.539(10) . ? C33 H33 1.0000 . ? C60 C59 1.387(11) . ? C60 C61 1.396(10) . ? C25 C23 1.524(11) . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C43 C42 1.522(10) . ? C43 H43 1.0000 . ? C23 C22 1.530(9) . ? C23 H23 1.0000 . ? C40 O15 1.364(8) . ? C40 C39 1.380(10) . ? C40 C41 1.394(10) . ? C41 C42 1.393(10) . ? C41 H41 0.9500 . ? C39 H39 0.9500 . ? C20 O17 1.360(9) . ? C20 C21 1.387(10) . ? C20 C19 1.390(10) . ? C26 O17 1.427(9) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C19 H19 0.9500 . ? C21 C22 1.398(10) . ? C21 H21 0.9500 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C46 O15 1.429(10) . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C61 C62 1.388(10) . ? C61 H61 0.9500 . ? C13 H13 1.0000 . ? C51 C52 1.407(10) . ? C51 H51 0.9500 . ? Cl7 C69 1.678(12) . ? C69 Cl8 1.675(14) . ? C69 H69A 0.9900 . ? C69 H69B 0.9900 . ? O12 C30 1.365(9) . ? O12 C36 1.437(12) . ? C53 C52 1.525(10) . ? C53 C54 1.527(10) . ? C53 C55 1.538(11) . ? C53 H53 1.0000 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C59 H59 0.9500 . ? C31 C30 1.386(11) . ? C31 H31 0.9500 . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? C66 H66A 0.9800 . ? C66 H66B 0.9800 . ? C66 H66C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? Cl6 C68 1.801(14) . ? Cl5 C68 1.714(15) . ? Cl3 C67 1.67(2) . ? O13 C16 1.416(9) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? Cl4 C67 1.46(3) . ? C68 H68A 0.9900 . ? C68 H68B 0.9900 . ? C67 H67A 0.9900 . ? C67 H67B 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 Cl1 Pt1 Cl2 178.85(7) . . ? Cl1 Pt1 As1 92.64(5) . . ? Cl2 Pt1 As1 87.60(5) . . ? Cl1 Pt1 As2 92.09(5) . . ? Cl2 Pt1 As2 87.73(5) . . ? As1 Pt1 As2 174.71(3) . . ? C7 As1 C27 106.7(3) . . ? C7 As1 C17 104.6(3) . . ? C27 As1 C17 100.8(3) . . ? C7 As1 Pt1 106.4(2) . . ? C27 As1 Pt1 122.28(19) . . ? C17 As1 Pt1 114.6(2) . . ? C37 As2 C57 104.1(3) . . ? C37 As2 C47 106.0(3) . . ? C57 As2 C47 101.9(3) . . ? C37 As2 Pt1 108.9(2) . . ? C57 As2 Pt1 121.1(2) . . ? C47 As2 Pt1 113.4(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 . . ? C30 C29 C28 118.5(7) . . ? C30 C29 H29 120.7 . . ? C28 C29 H29 120.7 . . ? C43 C45 H45A 109.5 . . ? C43 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C43 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C31 C32 C27 118.6(7) . . ? C31 C32 C33 119.2(7) . . ? C27 C32 C33 122.1(6) . . ? C63 C65 H65A 109.5 . . ? C63 C65 H65B 109.5 . . ? H65A C65 H65B 109.5 . . ? C63 C65 H65C 109.5 . . ? H65A C65 H65C 109.5 . . ? H65B C65 H65C 109.5 . . ? O14 C56 H56A 109.5 . . ? O14 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? O14 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? O14 C50 C51 125.0(7) . . ? O14 C50 C49 114.7(7) . . ? C51 C50 C49 120.3(7) . . ? C59 C58 C57 121.6(7) . . ? C59 C58 H58 119.2 . . ? C57 C58 H58 119.2 . . ? C28 C27 C32 118.5(6) . . ? C28 C27 As1 119.1(5) . . ? C32 C27 As1 122.2(5) . . ? C60 O16 C66 118.7(6) . . ? O13 C10 C11 125.7(7) . . ? O13 C10 C9 114.7(7) . . ? C11 C10 C9 119.5(7) . . ? C48 C47 C52 120.2(6) . . ? C48 C47 As2 114.7(5) . . ? C52 C47 As2 124.8(5) . . ? C43 C44 H44A 109.5 . . ? C43 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C43 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C58 C57 C62 119.0(6) . . ? C58 C57 As2 117.5(5) . . ? C62 C57 As2 123.4(5) . . ? C18 C17 C22 119.4(6) . . ? C18 C17 As1 115.0(5) . . ? C22 C17 As1 125.1(5) . . ? C48 C49 C50 118.4(7) . . ? C48 C49 H49 120.8 . . ? C50 C49 H49 120.8 . . ? C38 C37 C42 120.1(7) . . ? C38 C37 As2 117.2(5) . . ? C42 C37 As2 122.5(5) . . ? C49 C48 C47 121.9(7) . . ? C49 C48 H48 119.1 . . ? C47 C48 H48 119.1 . . ? C37 C38 C39 121.4(7) . . ? C37 C38 H38 119.3 . . ? C39 C38 H38 119.3 . . ? C63 C64 H64A 109.5 . . ? C63 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? C63 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? C7 C12 C11 119.3(7) . . ? C7 C12 C13 122.2(6) . . ? C11 C12 C13 118.5(6) . . ? C9 C8 C7 122.8(7) . . ? C9 C8 H8 118.6 . . ? C7 C8 H8 118.6 . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C62 C63 C65 112.4(6) . . ? C62 C63 C64 111.0(6) . . ? C65 C63 C64 110.1(6) . . ? C62 C63 H63 107.7 . . ? C65 C63 H63 107.7 . . ? C64 C63 H63 107.7 . . ? C10 C11 C12 121.8(7) . . ? C10 C11 H11 119.1 . . ? C12 C11 H11 119.1 . . ? C27 C28 C29 122.3(7) . . ? C27 C28 H28 118.8 . . ? C29 C28 H28 118.8 . . ? C17 C18 C19 122.3(6) . . ? C17 C18 H18 118.8 . . ? C19 C18 H18 118.8 . . ? C8 C9 C10 118.4(7) . . ? C8 C9 H9 120.8 . . ? C10 C9 H9 120.8 . . ? C32 C33 C34 110.8(6) . . ? C32 C33 C35 110.1(6) . . ? C34 C33 C35 110.2(6) . . ? C32 C33 H33 108.6 . . ? C34 C33 H33 108.6 . . ? C35 C33 H33 108.6 . . ? O16 C60 C59 116.4(7) . . ? O16 C60 C61 124.1(7) . . ? C59 C60 C61 119.5(7) . . ? C23 C25 H25A 109.5 . . ? C23 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C23 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C42 C43 C44 108.9(6) . . ? C42 C43 C45 113.5(6) . . ? C44 C43 C45 110.4(6) . . ? C42 C43 H43 107.9 . . ? C44 C43 H43 107.9 . . ? C45 C43 H43 107.9 . . ? C25 C23 C22 110.2(6) . . ? C25 C23 C24 110.1(6) . . ? C22 C23 C24 111.6(6) . . ? C25 C23 H23 108.3 . . ? C22 C23 H23 108.3 . . ? C24 C23 H23 108.3 . . ? O15 C40 C39 125.3(7) . . ? O15 C40 C41 115.4(7) . . ? C39 C40 C41 119.2(7) . . ? C42 C41 C40 122.6(7) . . ? C42 C41 H41 118.7 . . ? C40 C41 H41 118.7 . . ? C40 C39 C38 119.1(7) . . ? C40 C39 H39 120.5 . . ? C38 C39 H39 120.5 . . ? C12 C7 C8 118.0(7) . . ? C12 C7 As1 124.3(5) . . ? C8 C7 As1 117.2(5) . . ? O17 C20 C21 115.7(7) . . ? O17 C20 C19 124.6(7) . . ? C21 C20 C19 119.7(7) . . ? O17 C26 H26A 109.5 . . ? O17 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? O17 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C20 C19 C18 118.4(6) . . ? C20 C19 H19 120.8 . . ? C18 C19 H19 120.8 . . ? C20 C21 C22 122.4(7) . . ? C20 C21 H21 118.8 . . ? C22 C21 H21 118.8 . . ? 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 . . ? O15 C46 H46A 109.5 . . ? O15 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? O15 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C62 C61 C60 121.7(7) . . ? C62 C61 H61 119.2 . . ? C60 C61 H61 119.2 . . ? C15 C13 C12 113.2(6) . . ? C15 C13 C14 109.8(6) . . ? C12 C13 C14 108.8(6) . . ? C15 C13 H13 108.3 . . ? C12 C13 H13 108.3 . . ? C14 C13 H13 108.3 . . ? C21 C22 C17 117.8(6) . . ? C21 C22 C23 117.5(6) . . ? C17 C22 C23 124.7(6) . . ? C50 C51 C52 121.3(7) . . ? C50 C51 H51 119.3 . . ? C52 C51 H51 119.3 . . ? C40 O15 C46 116.1(6) . . ? C20 O17 C26 117.8(6) . . ? C50 O14 C56 118.2(7) . . ? C61 C62 C57 118.8(7) . . ? C61 C62 C63 117.7(6) . . ? C57 C62 C63 123.5(6) . . ? C41 C42 C37 117.4(7) . . ? C41 C42 C43 118.5(6) . . ? C37 C42 C43 124.1(6) . . ? Cl8 C69 Cl7 108.8(8) . . ? Cl8 C69 H69A 109.9 . . ? Cl7 C69 H69A 109.9 . . ? Cl8 C69 H69B 109.9 . . ? Cl7 C69 H69B 109.9 . . ? H69A C69 H69B 108.3 . . ? C30 O12 C36 116.3(7) . . ? C52 C53 C54 112.0(6) . . ? C52 C53 C55 112.1(6) . . ? C54 C53 C55 109.8(6) . . ? C52 C53 H53 107.6 . . ? C54 C53 H53 107.6 . . ? C55 C53 H53 107.6 . . ? C53 C54 H54A 109.5 . . ? C53 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C53 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C47 C52 C51 117.9(7) . . ? C47 C52 C53 125.3(6) . . ? C51 C52 C53 116.7(6) . . ? C58 C59 C60 119.5(7) . . ? C58 C59 H59 120.2 . . ? C60 C59 H59 120.2 . . ? C32 C31 C30 121.9(7) . . ? C32 C31 H31 119.1 . . ? C30 C31 H31 119.1 . . ? C53 C55 H55A 109.5 . . ? C53 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? C53 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? O12 C30 C31 115.6(7) . . ? O12 C30 C29 124.3(7) . . ? C31 C30 C29 120.1(7) . . ? O16 C66 H66A 109.5 . . ? O16 C66 H66B 109.5 . . ? H66A C66 H66B 109.5 . . ? O16 C66 H66C 109.5 . . ? H66A C66 H66C 109.5 . . ? H66B C66 H66C 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 . . ? O12 C36 H36A 109.5 . . ? O12 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? O12 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C10 O13 C16 118.2(6) . . ? O13 C16 H16A 109.5 . . ? O13 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? O13 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? Cl5 C68 Cl6 110.1(8) . . ? Cl5 C68 H68A 109.6 . . ? Cl6 C68 H68A 109.6 . . ? Cl5 C68 H68B 109.6 . . ? Cl6 C68 H68B 109.6 . . ? H68A C68 H68B 108.2 . . ? Cl4 C67 Cl3 133(3) . . ? Cl4 C67 H67A 103.9 . . ? Cl3 C67 H67A 103.9 . . ? Cl4 C67 H67B 103.9 . . ? Cl3 C67 H67B 103.9 . . ? H67A C67 H67B 105.4 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 2.697 _refine_diff_density_min -2.370 _refine_diff_density_rms 0.215