# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Petr Hermann' _publ_contact_author_email PETRH@NATUR.CUNI.CZ _publ_section_title ; Complexes of highly hydrophilic triphenylphosphines modified with gem-bis(phosphonate) moiety. An unusual simultaneous cis and trans arrangements in the Pt(II) dinuclear complex ; loop_ _publ_author_name 'Petr Hermann' 'Ivana Cisarova' 'Bohuslav Drahos' 'Jan Kotek' 'Zbynik Rohlik' # Attachment 'bisp2b2 new.cif' data_bisp2b2 _database_code_depnum_ccdc_archive 'CCDC 705469' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C47 H58 B2 O6 P4, H2 O' _chemical_formula_sum 'C47 H60 B2 O7 P4' _chemical_formula_weight 882.45 _chemical_compound_source 'synthesized by the authors' 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' B B 0.0013 0.0007 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 23.2795(3) _cell_length_b 14.69390(10) _cell_length_c 14.2210(2) _cell_angle_alpha 90.00 _cell_angle_beta 105.9901(6) _cell_angle_gamma 90.00 _cell_volume 4676.32(10) _cell_formula_units_Z 4 _cell_measurement_temperature 150(1) _cell_measurement_reflns_used 10964 _cell_measurement_theta_min 1 _cell_measurement_theta_max 27.48 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.28 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.253 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1872 _exptl_absorpt_coefficient_mu 0.210 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(1) _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 'Nonius KappaCCD area detector' _diffrn_measurement_method '\f and \w scans to fill the Ewald sphere' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20909 _diffrn_reflns_av_R_equivalents 0.0216 _diffrn_reflns_av_sigmaI/netI 0.0299 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.66 _diffrn_reflns_theta_max 27.49 _reflns_number_total 10721 _reflns_number_gt 8525 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Hooft, 1998) and DENZO (Otwinowski & Minor, 1997)' _computing_cell_refinement 'COLLECT and DENZO' _computing_data_reduction 'COLLECT and DENZO' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _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^)+(0.0527P)^2^+3.7343P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10721 _refine_ls_number_parameters 565 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0603 _refine_ls_R_factor_gt 0.0445 _refine_ls_wR_factor_ref 0.1190 _refine_ls_wR_factor_gt 0.1079 _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_restrained_S_all 1.018 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.31813(7) 0.62186(11) 0.51178(12) 0.0206(3) Uani 1 1 d . . . P1A P 0.32706(2) 0.74490(3) 0.53449(3) 0.02349(11) Uani 1 1 d . . . O1A O 0.35464(6) 0.77163(9) 0.63634(10) 0.0301(3) Uani 1 1 d . . . O2A O 0.26144(6) 0.78103(9) 0.49082(10) 0.0344(3) Uani 1 1 d . . . C30A C 0.23542(10) 0.85091(14) 0.53814(17) 0.0367(5) Uani 1 1 d . . . H30P H 0.2474 0.8408 0.6082 0.044 Uiso 1 1 calc R . . H30Q H 0.1922 0.8467 0.5156 0.044 Uiso 1 1 calc R . . C31A C 0.25422(16) 0.94331(16) 0.5172(2) 0.0628(8) Uani 1 1 d . . . H31P H 0.2955 0.9523 0.5518 0.075 Uiso 1 1 calc R . . H31Q H 0.2302 0.9879 0.5382 0.075 Uiso 1 1 calc R . . H31R H 0.2492 0.9496 0.4483 0.075 Uiso 1 1 calc R . . O3A O 0.35850(8) 0.77791(11) 0.45640(11) 0.0452(4) Uani 1 1 d . . . C32A C 0.41199(16) 0.8223(3) 0.4704(2) 0.0862(13) Uani 1 1 d . . . H32P H 0.4433 0.7871 0.5146 0.103 Uiso 1 1 calc R . . H32Q H 0.4098 0.8809 0.5006 0.103 Uiso 1 1 calc R . . C33A C 0.42723(11) 0.83603(17) 0.37698(18) 0.0443(5) Uani 1 1 d . . . H33P H 0.4024 0.8831 0.3400 0.053 Uiso 1 1 calc R . . H33Q H 0.4207 0.7804 0.3401 0.053 Uiso 1 1 calc R . . H33R H 0.4684 0.8534 0.3903 0.053 Uiso 1 1 calc R . . C2A C 0.29520(8) 0.57764(12) 0.59525(13) 0.0219(3) Uani 1 1 d . . . H2A1 H 0.2865 0.5142 0.5786 0.026 Uiso 1 1 calc R . . H2A2 H 0.3278 0.5791 0.6549 0.026 Uiso 1 1 calc R . . C3A C 0.24070(8) 0.61911(11) 0.61752(13) 0.0217(3) Uani 1 1 d . . . C4A C 0.24656(8) 0.65969(13) 0.70845(13) 0.0252(4) Uani 1 1 d . . . H4A H 0.2841 0.6627 0.7533 0.030 Uiso 1 1 calc R . . C5A C 0.19775(8) 0.69547(13) 0.73340(13) 0.0260(4) Uani 1 1 d . . . H5A H 0.2026 0.7206 0.7951 0.031 Uiso 1 1 calc R . . C6A C 0.14125(8) 0.69400(12) 0.66648(13) 0.0222(3) Uani 1 1 d . . . C7A C 0.13478(8) 0.65415(12) 0.57532(13) 0.0241(4) Uani 1 1 d . . . H7A H 0.0975 0.6532 0.5296 0.029 Uiso 1 1 calc R . . C8A C 0.18380(8) 0.61576(12) 0.55249(13) 0.0237(4) Uani 1 1 d . . . H8A H 0.1785 0.5872 0.4924 0.028 Uiso 1 1 calc R . . P2A P 0.07990(2) 0.74815(3) 0.70068(3) 0.02403(11) Uani 1 1 d . . . B2A B 0.08587(11) 0.73245(19) 0.83607(16) 0.0344(5) Uani 1 1 d . . . H1BA H 0.1285(12) 0.7597(18) 0.8764(19) 0.053(7) Uiso 1 1 d . . . H2BA H 0.0472(12) 0.7689(18) 0.8504(19) 0.057(8) Uiso 1 1 d . . . H3BA H 0.0809(12) 0.6559(19) 0.844(2) 0.061(8) Uiso 1 1 d . . . C10A C 0.08049(8) 0.86590(13) 0.66271(14) 0.0286(4) Uani 1 1 d . . . C11A C 0.07942(10) 0.88795(15) 0.56704(15) 0.0358(5) Uani 1 1 d . . . H11A H 0.0785 0.8419 0.5218 0.043 Uiso 1 1 calc R . . C12A C 0.07967(12) 0.97801(16) 0.53907(18) 0.0455(6) Uani 1 1 d . . . H12A H 0.0793 0.9926 0.4753 0.055 Uiso 1 1 calc R . . C13A C 0.08049(13) 1.04658(17) 0.60661(19) 0.0538(7) Uani 1 1 d . . . H13A H 0.0800 1.1072 0.5875 0.065 Uiso 1 1 calc R . . C14A C 0.08197(13) 1.02564(17) 0.70205(19) 0.0546(7) Uani 1 1 d . . . H14A H 0.0829 1.0719 0.7471 0.066 Uiso 1 1 calc R . . C15A C 0.08210(11) 0.93533(15) 0.73020(17) 0.0414(5) Uani 1 1 d . . . H15A H 0.0833 0.9210 0.7944 0.050 Uiso 1 1 calc R . . C20A C 0.01100(8) 0.69981(13) 0.62342(13) 0.0259(4) Uani 1 1 d . . . C21A C -0.03848(9) 0.75472(16) 0.58538(15) 0.0347(4) Uani 1 1 d . . . H21A H -0.0353 0.8175 0.5938 0.042 Uiso 1 1 calc R . . C22A C -0.09265(10) 0.71630(19) 0.53486(17) 0.0438(5) Uani 1 1 d . . . H22A H -0.1259 0.7533 0.5109 0.053 Uiso 1 1 calc R . . C23A C -0.09740(10) 0.62353(19) 0.52009(16) 0.0441(6) Uani 1 1 d . . . H23A H -0.1335 0.5982 0.4848 0.053 Uiso 1 1 calc R . . C24A C -0.04858(10) 0.56849(16) 0.55772(17) 0.0412(5) Uani 1 1 d . . . H24A H -0.0518 0.5059 0.5479 0.049 Uiso 1 1 calc R . . C25A C 0.00540(9) 0.60618(14) 0.61019(15) 0.0334(4) Uani 1 1 d . . . H25A H 0.0380 0.5686 0.6366 0.040 Uiso 1 1 calc R . . P1B P 0.39113(2) 0.56945(3) 0.51817(3) 0.02342(11) Uani 1 1 d . . . O1B O 0.41062(6) 0.57734(10) 0.42875(10) 0.0330(3) Uani 1 1 d . . . O2B O 0.38623(6) 0.46868(9) 0.55231(10) 0.0282(3) Uani 1 1 d . . . C30B C 0.39184(9) 0.38727(13) 0.49607(15) 0.0311(4) Uani 1 1 d . . . H30X H 0.3965 0.4048 0.4328 0.037 Uiso 1 1 calc R . . H30Y H 0.3560 0.3505 0.4853 0.037 Uiso 1 1 calc R . . C31B C 0.44479(10) 0.33358(14) 0.55106(17) 0.0375(5) Uani 1 1 d . . . H31X H 0.4799 0.3711 0.5641 0.045 Uiso 1 1 calc R . . H31Y H 0.4498 0.2819 0.5127 0.045 Uiso 1 1 calc R . . H31Z H 0.4388 0.3131 0.6118 0.045 Uiso 1 1 calc R . . O3B O 0.43199(6) 0.61637(9) 0.61190(10) 0.0317(3) Uani 1 1 d . . . C32B C 0.49113(9) 0.58084(16) 0.65910(16) 0.0372(5) Uani 1 1 d . . . H32X H 0.5077 0.5522 0.6110 0.045 Uiso 1 1 calc R . . H32Y H 0.4887 0.5355 0.7074 0.045 Uiso 1 1 calc R . . C33B C 0.53017(10) 0.65778(19) 0.70729(18) 0.0488(6) Uani 1 1 d . . . H33X H 0.5213 0.7107 0.6663 0.059 Uiso 1 1 calc R . . H33Y H 0.5713 0.6413 0.7173 0.059 Uiso 1 1 calc R . . H33Z H 0.5229 0.6708 0.7692 0.059 Uiso 1 1 calc R . . C2B C 0.27628(8) 0.60949(11) 0.40523(12) 0.0219(3) Uani 1 1 d . . . H2B1 H 0.2367 0.6309 0.4043 0.026 Uiso 1 1 calc R . . H2B2 H 0.2909 0.6487 0.3620 0.026 Uiso 1 1 calc R . . C3B C 0.27024(8) 0.51414(12) 0.36321(13) 0.0224(4) Uani 1 1 d . . . C4B C 0.29500(9) 0.49360(13) 0.28682(13) 0.0268(4) Uani 1 1 d . . . H4B H 0.3145 0.5389 0.2618 0.032 Uiso 1 1 calc R . . C5B C 0.29102(9) 0.40663(13) 0.24772(13) 0.0275(4) Uani 1 1 d . . . H5B H 0.3074 0.3944 0.1964 0.033 Uiso 1 1 calc R . . C6B C 0.26264(8) 0.33744(12) 0.28489(13) 0.0248(4) Uani 1 1 d . . . C7B C 0.23629(8) 0.35784(12) 0.35936(13) 0.0253(4) Uani 1 1 d . . . H7B H 0.2166 0.3126 0.3842 0.030 Uiso 1 1 calc R . . C8B C 0.23940(8) 0.44543(12) 0.39624(13) 0.0240(4) Uani 1 1 d . . . H8B H 0.2204 0.4587 0.4442 0.029 Uiso 1 1 calc R . . P2B P 0.26369(2) 0.22344(3) 0.23649(4) 0.02598(11) Uani 1 1 d . . . B2B B 0.26973(13) 0.22358(18) 0.10548(17) 0.0365(5) Uani 1 1 d . . . H1BB H 0.3148(13) 0.2517(18) 0.1107(19) 0.055(8) Uiso 1 1 d . . . H2BB H 0.2333(12) 0.2645(18) 0.068(2) 0.055(8) Uiso 1 1 d . . . H3BB H 0.2642(12) 0.1523(19) 0.0822(19) 0.058(8) Uiso 1 1 d . . . C10B C 0.32499(9) 0.16402(13) 0.32104(15) 0.0302(4) Uani 1 1 d . . . C11B C 0.32602(10) 0.15070(14) 0.41838(16) 0.0369(5) Uani 1 1 d . . . H11B H 0.2943 0.1709 0.4409 0.044 Uiso 1 1 calc R . . C12B C 0.37421(11) 0.10747(15) 0.48176(18) 0.0449(5) Uani 1 1 d . . . H12B H 0.3746 0.0978 0.5465 0.054 Uiso 1 1 calc R . . C13B C 0.42162(11) 0.07879(16) 0.4489(2) 0.0517(6) Uani 1 1 d . . . H13B H 0.4540 0.0502 0.4919 0.062 Uiso 1 1 calc R . . C14B C 0.42147(11) 0.09214(17) 0.3532(2) 0.0544(7) Uani 1 1 d . . . H14B H 0.4538 0.0732 0.3318 0.065 Uiso 1 1 calc R . . C15B C 0.37285(10) 0.13403(15) 0.28849(19) 0.0430(5) Uani 1 1 d . . . H15B H 0.3723 0.1420 0.2234 0.052 Uiso 1 1 calc R . . C20B C 0.19555(9) 0.16953(13) 0.24640(14) 0.0280(4) Uani 1 1 d . . . C21B C 0.19408(10) 0.07853(14) 0.27186(16) 0.0372(5) Uani 1 1 d . . . H21B H 0.2290 0.0443 0.2874 0.045 Uiso 1 1 calc R . . C22B C 0.14067(12) 0.03867(17) 0.2742(2) 0.0508(6) Uani 1 1 d . . . H22B H 0.1399 -0.0222 0.2918 0.061 Uiso 1 1 calc R . . C23B C 0.08846(11) 0.08885(19) 0.2505(2) 0.0542(7) Uani 1 1 d . . . H23B H 0.0528 0.0621 0.2534 0.065 Uiso 1 1 calc R . . C24B C 0.08931(10) 0.17887(19) 0.22259(19) 0.0500(6) Uani 1 1 d . . . H24B H 0.0540 0.2123 0.2051 0.060 Uiso 1 1 calc R . . C25B C 0.14242(9) 0.21904(16) 0.22069(16) 0.0376(5) Uani 1 1 d . . . H25B H 0.1429 0.2797 0.2021 0.045 Uiso 1 1 calc R . . O1W O 0.42703(9) 0.58225(14) 0.22961(14) 0.0664(6) Uani 1 1 d . . . H1W1 H 0.4239 0.5849 0.2880 0.080 Uiso 1 1 d R . . H1W2 H 0.4071 0.6252 0.2018 0.080 Uiso 1 1 d 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 C1 0.0183(8) 0.0200(8) 0.0234(8) 0.0009(7) 0.0054(7) 0.0000(6) P1A 0.0240(2) 0.0196(2) 0.0257(2) -0.00113(18) 0.00483(18) -0.00250(17) O1A 0.0289(7) 0.0281(7) 0.0296(7) -0.0050(5) 0.0021(6) -0.0020(5) O2A 0.0352(8) 0.0249(7) 0.0362(8) -0.0065(6) -0.0019(6) 0.0097(6) C30A 0.0330(11) 0.0302(10) 0.0458(12) -0.0059(9) 0.0088(9) 0.0058(8) C31A 0.100(2) 0.0261(11) 0.0621(17) 0.0003(11) 0.0213(16) 0.0084(13) O3A 0.0525(10) 0.0477(9) 0.0383(8) -0.0052(7) 0.0174(7) -0.0290(8) C32A 0.089(2) 0.117(3) 0.0686(19) -0.0353(19) 0.0473(18) -0.075(2) C33A 0.0408(13) 0.0488(13) 0.0486(13) -0.0030(11) 0.0214(11) -0.0136(10) C2A 0.0196(8) 0.0220(8) 0.0241(8) 0.0017(7) 0.0061(7) 0.0015(7) C3A 0.0214(9) 0.0195(8) 0.0244(8) 0.0028(7) 0.0068(7) -0.0001(7) C4A 0.0193(9) 0.0315(9) 0.0233(8) 0.0000(7) 0.0030(7) -0.0007(7) C5A 0.0247(9) 0.0312(9) 0.0211(8) -0.0047(7) 0.0049(7) -0.0013(7) C6A 0.0197(8) 0.0228(8) 0.0244(8) 0.0002(7) 0.0068(7) 0.0009(7) C7A 0.0197(9) 0.0280(9) 0.0235(9) -0.0023(7) 0.0042(7) -0.0004(7) C8A 0.0233(9) 0.0246(9) 0.0228(8) -0.0038(7) 0.0056(7) -0.0002(7) P2A 0.0209(2) 0.0294(2) 0.0218(2) -0.00296(18) 0.00583(18) 0.00277(18) B2A 0.0309(12) 0.0515(15) 0.0215(10) -0.0026(10) 0.0083(9) 0.0077(11) C10A 0.0243(9) 0.0297(9) 0.0311(10) -0.0035(8) 0.0062(8) 0.0030(7) C11A 0.0429(12) 0.0335(11) 0.0315(10) -0.0018(8) 0.0110(9) 0.0038(9) C12A 0.0572(15) 0.0388(12) 0.0394(12) 0.0058(10) 0.0112(11) 0.0002(11) C13A 0.0710(18) 0.0313(11) 0.0538(15) 0.0015(11) 0.0081(13) -0.0073(12) C14A 0.078(2) 0.0334(12) 0.0498(15) -0.0128(11) 0.0126(13) -0.0065(12) C15A 0.0516(14) 0.0374(12) 0.0341(11) -0.0077(9) 0.0102(10) -0.0012(10) C20A 0.0216(9) 0.0355(10) 0.0223(8) -0.0014(7) 0.0091(7) -0.0005(7) C21A 0.0269(10) 0.0435(12) 0.0329(10) 0.0009(9) 0.0072(8) 0.0053(9) C22A 0.0215(10) 0.0652(16) 0.0412(12) 0.0061(11) 0.0028(9) 0.0016(10) C23A 0.0275(11) 0.0696(16) 0.0338(11) 0.0013(11) 0.0058(9) -0.0163(11) C24A 0.0382(12) 0.0443(12) 0.0433(12) -0.0034(10) 0.0147(10) -0.0152(10) C25A 0.0277(10) 0.0364(11) 0.0364(11) 0.0026(9) 0.0093(8) -0.0018(8) P1B 0.0193(2) 0.0246(2) 0.0272(2) 0.00211(18) 0.00772(18) 0.00167(17) O1B 0.0273(7) 0.0394(8) 0.0364(8) 0.0053(6) 0.0157(6) 0.0017(6) O2B 0.0311(7) 0.0241(6) 0.0321(7) 0.0028(5) 0.0133(6) 0.0066(5) C30B 0.0295(10) 0.0248(9) 0.0394(11) -0.0046(8) 0.0103(9) 0.0016(8) C31B 0.0349(11) 0.0302(10) 0.0492(13) 0.0032(9) 0.0146(10) 0.0071(9) O3B 0.0200(7) 0.0331(7) 0.0380(8) -0.0039(6) 0.0015(6) 0.0036(5) C32B 0.0252(10) 0.0463(12) 0.0368(11) 0.0052(9) 0.0033(8) 0.0062(9) C33B 0.0302(12) 0.0680(17) 0.0454(13) -0.0162(12) 0.0059(10) -0.0061(11) C2B 0.0228(9) 0.0190(8) 0.0232(8) 0.0008(7) 0.0051(7) -0.0001(7) C3B 0.0214(9) 0.0217(8) 0.0225(8) 0.0005(7) 0.0033(7) 0.0014(7) C4B 0.0300(10) 0.0251(9) 0.0266(9) 0.0012(7) 0.0100(8) -0.0033(7) C5B 0.0312(10) 0.0291(9) 0.0249(9) -0.0013(7) 0.0120(8) 0.0009(8) C6B 0.0249(9) 0.0239(9) 0.0249(9) -0.0030(7) 0.0057(7) 0.0016(7) C7B 0.0261(9) 0.0224(8) 0.0286(9) -0.0003(7) 0.0094(7) -0.0015(7) C8B 0.0237(9) 0.0243(9) 0.0254(9) -0.0018(7) 0.0090(7) 0.0009(7) P2B 0.0268(3) 0.0240(2) 0.0285(2) -0.00557(19) 0.00990(19) -0.00007(18) B2B 0.0455(15) 0.0390(13) 0.0275(11) -0.0076(10) 0.0141(11) -0.0017(11) C10B 0.0267(10) 0.0226(9) 0.0413(11) -0.0056(8) 0.0092(8) -0.0011(7) C11B 0.0325(11) 0.0348(11) 0.0416(12) -0.0036(9) 0.0072(9) 0.0031(9) C12B 0.0450(13) 0.0358(11) 0.0457(13) -0.0022(10) -0.0010(10) 0.0023(10) C13B 0.0378(13) 0.0343(12) 0.0713(18) -0.0041(12) -0.0042(12) 0.0094(10) C14B 0.0371(13) 0.0445(14) 0.082(2) -0.0039(13) 0.0173(13) 0.0139(11) C15B 0.0372(12) 0.0380(12) 0.0580(14) -0.0021(11) 0.0202(11) 0.0078(10) C20B 0.0270(10) 0.0288(9) 0.0285(9) -0.0092(8) 0.0082(8) -0.0016(7) C21B 0.0363(12) 0.0303(10) 0.0452(12) -0.0077(9) 0.0116(10) -0.0047(9) C22B 0.0535(16) 0.0404(13) 0.0635(16) -0.0150(12) 0.0242(13) -0.0186(11) C23B 0.0387(14) 0.0665(17) 0.0649(16) -0.0354(14) 0.0266(12) -0.0258(12) C24B 0.0283(12) 0.0661(17) 0.0557(15) -0.0289(13) 0.0117(10) -0.0023(11) C25B 0.0308(11) 0.0398(11) 0.0407(11) -0.0124(10) 0.0073(9) 0.0016(9) O1W 0.0762(14) 0.0748(13) 0.0553(11) 0.0313(10) 0.0302(10) 0.0459(11) _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 C1 C2B 1.570(2) . ? C1 C2A 1.570(2) . ? C1 P1A 1.8382(17) . ? C1 P1B 1.8449(17) . ? P1A O1A 1.4670(14) . ? P1A O3A 1.5660(15) . ? P1A O2A 1.5744(15) . ? O2A C30A 1.449(2) . ? C30A C31A 1.482(3) . ? C30A H30P 0.9700 . ? C30A H30Q 0.9700 . ? C31A H31P 0.9600 . ? C31A H31Q 0.9600 . ? C31A H31R 0.9600 . ? O3A C32A 1.371(3) . ? C32A C33A 1.480(3) . ? C32A H32P 0.9700 . ? C32A H32Q 0.9700 . ? C33A H33P 0.9600 . ? C33A H33Q 0.9600 . ? C33A H33R 0.9600 . ? C2A C3A 1.517(2) . ? C2A H2A1 0.9700 . ? C2A H2A2 0.9700 . ? C3A C8A 1.392(2) . ? C3A C4A 1.396(2) . ? C4A C5A 1.384(3) . ? C4A H4A 0.9300 . ? C5A C6A 1.395(2) . ? C5A H5A 0.9300 . ? C6A C7A 1.392(2) . ? C6A P2A 1.8144(18) . ? C7A C8A 1.389(2) . ? C7A H7A 0.9300 . ? C8A H8A 0.9300 . ? P2A C10A 1.814(2) . ? P2A C20A 1.8203(19) . ? P2A B2A 1.906(2) . ? B2A H1BA 1.08(3) . ? B2A H2BA 1.11(3) . ? B2A H3BA 1.14(3) . ? C10A C11A 1.392(3) . ? C10A C15A 1.394(3) . ? C11A C12A 1.382(3) . ? C11A H11A 0.9300 . ? C12A C13A 1.389(4) . ? C12A H12A 0.9300 . ? C13A C14A 1.383(4) . ? C13A H13A 0.9300 . ? C14A C15A 1.386(3) . ? C14A H14A 0.9300 . ? C15A H15A 0.9300 . ? C20A C21A 1.388(3) . ? C20A C25A 1.390(3) . ? C21A C22A 1.388(3) . ? C21A H21A 0.9300 . ? C22A C23A 1.379(4) . ? C22A H22A 0.9300 . ? C23A C24A 1.377(3) . ? C23A H23A 0.9300 . ? C24A C25A 1.388(3) . ? C24A H24A 0.9300 . ? C25A H25A 0.9300 . ? P1B O1B 1.4678(14) . ? P1B O3B 1.5679(14) . ? P1B O2B 1.5722(13) . ? O2B C30B 1.465(2) . ? C30B C31B 1.491(3) . ? C30B H30X 0.9700 . ? C30B H30Y 0.9700 . ? C31B H31X 0.9600 . ? C31B H31Y 0.9600 . ? C31B H31Z 0.9600 . ? O3B C32B 1.452(2) . ? C32B C33B 1.493(3) . ? C32B H32X 0.9700 . ? C32B H32Y 0.9700 . ? C33B H33X 0.9600 . ? C33B H33Y 0.9600 . ? C33B H33Z 0.9600 . ? C2B C3B 1.515(2) . ? C2B H2B1 0.9700 . ? C2B H2B2 0.9700 . ? C3B C8B 1.393(2) . ? C3B C4B 1.396(3) . ? C4B C5B 1.387(3) . ? C4B H4B 0.9300 . ? C5B C6B 1.394(3) . ? C5B H5B 0.9300 . ? C6B C7B 1.395(2) . ? C6B P2B 1.8137(18) . ? C7B C8B 1.384(2) . ? C7B H7B 0.9300 . ? C8B H8B 0.9300 . ? P2B C20B 1.813(2) . ? P2B C10B 1.816(2) . ? P2B B2B 1.907(2) . ? B2B H1BB 1.11(3) . ? B2B H2BB 1.06(3) . ? B2B H3BB 1.10(3) . ? C10B C15B 1.391(3) . ? C10B C11B 1.392(3) . ? C11B C12B 1.385(3) . ? C11B H11B 0.9300 . ? C12B C13B 1.378(4) . ? C12B H12B 0.9300 . ? C13B C14B 1.374(4) . ? C13B H13B 0.9300 . ? C14B C15B 1.390(3) . ? C14B H14B 0.9300 . ? C15B H15B 0.9300 . ? C20B C21B 1.388(3) . ? C20B C25B 1.394(3) . ? C21B C22B 1.383(3) . ? C21B H21B 0.9300 . ? C22B C23B 1.382(4) . ? C22B H22B 0.9300 . ? C23B C24B 1.383(4) . ? C23B H23B 0.9300 . ? C24B C25B 1.377(3) . ? C24B H24B 0.9300 . ? C25B H25B 0.9300 . ? O1W H1W1 0.8552 . ? O1W H1W2 0.8184 . ? 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 C2B C1 C2A 115.58(14) . . ? C2B C1 P1A 107.07(11) . . ? C2A C1 P1A 108.65(11) . . ? C2B C1 P1B 108.52(11) . . ? C2A C1 P1B 106.88(11) . . ? P1A C1 P1B 110.11(9) . . ? O1A P1A O3A 117.02(8) . . ? O1A P1A O2A 114.35(8) . . ? O3A P1A O2A 102.01(9) . . ? O1A P1A C1 115.74(8) . . ? O3A P1A C1 103.44(8) . . ? O2A P1A C1 102.24(8) . . ? C30A O2A P1A 122.70(13) . . ? O2A C30A C31A 111.8(2) . . ? O2A C30A H30P 109.2 . . ? C31A C30A H30P 109.2 . . ? O2A C30A H30Q 109.2 . . ? C31A C30A H30Q 109.2 . . ? H30P C30A H30Q 107.9 . . ? C30A C31A H31P 109.5 . . ? C30A C31A H31Q 109.5 . . ? H31P C31A H31Q 109.5 . . ? C30A C31A H31R 109.5 . . ? H31P C31A H31R 109.5 . . ? H31Q C31A H31R 109.5 . . ? C32A O3A P1A 128.87(17) . . ? O3A C32A C33A 111.5(2) . . ? O3A C32A H32P 109.3 . . ? C33A C32A H32P 109.3 . . ? O3A C32A H32Q 109.3 . . ? C33A C32A H32Q 109.3 . . ? H32P C32A H32Q 108.0 . . ? C32A C33A H33P 109.5 . . ? C32A C33A H33Q 109.5 . . ? H33P C33A H33Q 109.5 . . ? C32A C33A H33R 109.5 . . ? H33P C33A H33R 109.5 . . ? H33Q C33A H33R 109.5 . . ? C3A C2A C1 118.01(14) . . ? C3A C2A H2A1 107.8 . . ? C1 C2A H2A1 107.8 . . ? C3A C2A H2A2 107.8 . . ? C1 C2A H2A2 107.8 . . ? H2A1 C2A H2A2 107.1 . . ? C8A C3A C4A 117.56(16) . . ? C8A C3A C2A 122.99(16) . . ? C4A C3A C2A 119.40(16) . . ? C5A C4A C3A 121.47(17) . . ? C5A C4A H4A 119.3 . . ? C3A C4A H4A 119.3 . . ? C4A C5A C6A 120.36(16) . . ? C4A C5A H5A 119.8 . . ? C6A C5A H5A 119.8 . . ? C7A C6A C5A 118.79(16) . . ? C7A C6A P2A 122.87(14) . . ? C5A C6A P2A 118.29(13) . . ? C8A C7A C6A 120.21(16) . . ? C8A C7A H7A 119.9 . . ? C6A C7A H7A 119.9 . . ? C7A C8A C3A 121.54(16) . . ? C7A C8A H8A 119.2 . . ? C3A C8A H8A 119.2 . . ? C10A P2A C6A 105.51(8) . . ? C10A P2A C20A 105.68(9) . . ? C6A P2A C20A 107.15(8) . . ? C10A P2A B2A 114.32(11) . . ? C6A P2A B2A 111.97(9) . . ? C20A P2A B2A 111.68(10) . . ? P2A B2A H1BA 107.0(14) . . ? P2A B2A H2BA 106.8(14) . . ? H1BA B2A H2BA 113(2) . . ? P2A B2A H3BA 103.7(14) . . ? H1BA B2A H3BA 115(2) . . ? H2BA B2A H3BA 110(2) . . ? C11A C10A C15A 119.50(19) . . ? C11A C10A P2A 120.89(15) . . ? C15A C10A P2A 119.61(16) . . ? C12A C11A C10A 120.2(2) . . ? C12A C11A H11A 119.9 . . ? C10A C11A H11A 119.9 . . ? C11A C12A C13A 119.7(2) . . ? C11A C12A H12A 120.1 . . ? C13A C12A H12A 120.1 . . ? C14A C13A C12A 120.6(2) . . ? C14A C13A H13A 119.7 . . ? C12A C13A H13A 119.7 . . ? C13A C14A C15A 119.6(2) . . ? C13A C14A H14A 120.2 . . ? C15A C14A H14A 120.2 . . ? C14A C15A C10A 120.3(2) . . ? C14A C15A H15A 119.9 . . ? C10A C15A H15A 119.9 . . ? C21A C20A C25A 119.06(19) . . ? C21A C20A P2A 120.47(16) . . ? C25A C20A P2A 120.15(15) . . ? C22A C21A C20A 120.2(2) . . ? C22A C21A H21A 119.9 . . ? C20A C21A H21A 119.9 . . ? C23A C22A C21A 120.3(2) . . ? C23A C22A H22A 119.9 . . ? C21A C22A H22A 119.9 . . ? C24A C23A C22A 119.9(2) . . ? C24A C23A H23A 120.1 . . ? C22A C23A H23A 120.1 . . ? C23A C24A C25A 120.2(2) . . ? C23A C24A H24A 119.9 . . ? C25A C24A H24A 119.9 . . ? C24A C25A C20A 120.3(2) . . ? C24A C25A H25A 119.8 . . ? C20A C25A H25A 119.8 . . ? O1B P1B O3B 116.22(8) . . ? O1B P1B O2B 114.08(8) . . ? O3B P1B O2B 103.31(8) . . ? O1B P1B C1 115.14(8) . . ? O3B P1B C1 101.14(8) . . ? O2B P1B C1 105.31(7) . . ? C30B O2B P1B 125.14(12) . . ? O2B C30B C31B 109.34(17) . . ? O2B C30B H30X 109.8 . . ? C31B C30B H30X 109.8 . . ? O2B C30B H30Y 109.8 . . ? C31B C30B H30Y 109.8 . . ? H30X C30B H30Y 108.3 . . ? C30B C31B H31X 109.5 . . ? C30B C31B H31Y 109.5 . . ? H31X C31B H31Y 109.5 . . ? C30B C31B H31Z 109.5 . . ? H31X C31B H31Z 109.5 . . ? H31Y C31B H31Z 109.5 . . ? C32B O3B P1B 120.71(13) . . ? O3B C32B C33B 108.64(19) . . ? O3B C32B H32X 110.0 . . ? C33B C32B H32X 110.0 . . ? O3B C32B H32Y 110.0 . . ? C33B C32B H32Y 110.0 . . ? H32X C32B H32Y 108.3 . . ? C32B C33B H33X 109.5 . . ? C32B C33B H33Y 109.5 . . ? H33X C33B H33Y 109.5 . . ? C32B C33B H33Z 109.5 . . ? H33X C33B H33Z 109.5 . . ? H33Y C33B H33Z 109.5 . . ? C3B C2B C1 116.96(14) . . ? C3B C2B H2B1 108.1 . . ? C1 C2B H2B1 108.1 . . ? C3B C2B H2B2 108.1 . . ? C1 C2B H2B2 108.1 . . ? H2B1 C2B H2B2 107.3 . . ? C8B C3B C4B 117.86(16) . . ? C8B C3B C2B 122.53(16) . . ? C4B C3B C2B 119.59(16) . . ? C5B C4B C3B 121.00(17) . . ? C5B C4B H4B 119.5 . . ? C3B C4B H4B 119.5 . . ? C4B C5B C6B 120.43(17) . . ? C4B C5B H5B 119.8 . . ? C6B C5B H5B 119.8 . . ? C5B C6B C7B 119.00(16) . . ? C5B C6B P2B 118.19(14) . . ? C7B C6B P2B 122.78(14) . . ? C8B C7B C6B 119.96(17) . . ? C8B C7B H7B 120.0 . . ? C6B C7B H7B 120.0 . . ? C7B C8B C3B 121.61(16) . . ? C7B C8B H8B 119.2 . . ? C3B C8B H8B 119.2 . . ? C20B P2B C6B 105.70(8) . . ? C20B P2B C10B 106.45(9) . . ? C6B P2B C10B 106.44(9) . . ? C20B P2B B2B 112.22(11) . . ? C6B P2B B2B 112.47(10) . . ? C10B P2B B2B 113.04(11) . . ? P2B B2B H1BB 104.9(14) . . ? P2B B2B H2BB 103.1(15) . . ? H1BB B2B H2BB 116(2) . . ? P2B B2B H3BB 105.0(14) . . ? H1BB B2B H3BB 114(2) . . ? H2BB B2B H3BB 112(2) . . ? C15B C10B C11B 119.4(2) . . ? C15B C10B P2B 119.16(17) . . ? C11B C10B P2B 121.41(15) . . ? C12B C11B C10B 120.1(2) . . ? C12B C11B H11B 120.0 . . ? C10B C11B H11B 120.0 . . ? C13B C12B C11B 120.0(2) . . ? C13B C12B H12B 120.0 . . ? C11B C12B H12B 120.0 . . ? C14B C13B C12B 120.6(2) . . ? C14B C13B H13B 119.7 . . ? C12B C13B H13B 119.7 . . ? C13B C14B C15B 119.9(2) . . ? C13B C14B H14B 120.0 . . ? C15B C14B H14B 120.0 . . ? C14B C15B C10B 120.0(2) . . ? C14B C15B H15B 120.0 . . ? C10B C15B H15B 120.0 . . ? C21B C20B C25B 119.16(19) . . ? C21B C20B P2B 121.74(16) . . ? C25B C20B P2B 118.92(16) . . ? C22B C21B C20B 120.1(2) . . ? C22B C21B H21B 120.0 . . ? C20B C21B H21B 120.0 . . ? C23B C22B C21B 120.3(2) . . ? C23B C22B H22B 119.8 . . ? C21B C22B H22B 119.8 . . ? C22B C23B C24B 119.9(2) . . ? C22B C23B H23B 120.0 . . ? C24B C23B H23B 120.0 . . ? C25B C24B C23B 120.0(2) . . ? C25B C24B H24B 120.0 . . ? C23B C24B H24B 120.0 . . ? C24B C25B C20B 120.5(2) . . ? C24B C25B H25B 119.7 . . ? C20B C25B H25B 119.7 . . ? H1W1 O1W H1W2 104.2 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.014 _refine_diff_density_min -0.838 _refine_diff_density_rms 0.055 _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla, M.C., Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, p. 435. Coppens, P. (1970). Crystallographic Computing, edited by F.R. Ahmed, S.R.Hall & C.P. Huber, pp. 255-270, Copenhagen, Munksgaard. Hooft, R.W. (1998). COLLECT. Nonius BV, Delft, The Netherlands. Otwinowski, Z. & Minor, W. (1997). Methods Enzymol. 276, 307--326. Sheldrick, G. M. (1997). SHELXL97. University of G\"ottingen, Germany. Spek, A.L. (1999). PLATON. Version 1999. Utrecht University, The Netherlands. ; # Attachment 'pdsq new.cif' data_pdsq _database_code_depnum_ccdc_archive 'CCDC 705470' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C56 H74 Cl2 O12 P6 Pd, 2(C H Cl3)' _chemical_formula_sum 'C58 H76 Cl8 O12 P6 Pd' _chemical_formula_weight 1541.01 _chemical_compound_source 'synthesized by the authors' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.2868(3) _cell_length_b 10.5786(3) _cell_length_c 21.4686(7) _cell_angle_alpha 103.0091(15) _cell_angle_beta 92.2351(16) _cell_angle_gamma 107.8208(18) _cell_volume 1733.86(10) _cell_formula_units_Z 1 _cell_measurement_temperature 150(1) _cell_measurement_reflns_used 36895 _cell_measurement_theta_min 1 _cell_measurement_theta_max 27.10 _exptl_crystal_description rod _exptl_crystal_colour colourless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.476 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 792 _exptl_absorpt_coefficient_mu 0.770 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.80869 _exptl_absorpt_correction_T_max 0.97559 _exptl_absorpt_process_details ; Gaussian integration (Coppens, 1970) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(1) _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 'Nonius KappaCCD area detector' _diffrn_measurement_method '\f and \w scans to fill the Ewald sphere' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 31622 _diffrn_reflns_av_R_equivalents 0.0741 _diffrn_reflns_av_sigmaI/netI 0.0793 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.96 _diffrn_reflns_theta_max 27.08 _reflns_number_total 7631 _reflns_number_gt 5191 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Hooft, 1998) and DENZO (Otwinowski & Minor, 1997)' _computing_cell_refinement 'COLLECT and DENZO' _computing_data_reduction 'COLLECT and DENZO' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _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^)+(0.0691P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7631 _refine_ls_number_parameters 353 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0884 _refine_ls_R_factor_gt 0.0522 _refine_ls_wR_factor_ref 0.1333 _refine_ls_wR_factor_gt 0.1202 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.041 _refine_ls_shift/su_max 0.000 _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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.5000 0.5000 0.5000 0.02565(13) Uani 1 2 d S . . Cl1 Cl 0.35874(10) 0.27624(8) 0.44522(4) 0.0334(2) Uani 1 1 d . . . P1 P 0.38988(10) 0.58761(8) 0.42424(4) 0.0271(2) Uani 1 1 d . . . C1 C 0.5493(4) 0.6676(3) 0.37664(17) 0.0298(8) Uani 1 1 d . . . C2 C 0.7241(4) 0.7037(3) 0.39703(17) 0.0316(8) Uani 1 1 d . . . H21 H 0.7591 0.6889 0.4357 0.038 Uiso 1 1 calc R . . C3 C 0.8441(4) 0.7612(3) 0.35977(17) 0.0332(8) Uani 1 1 d . . . H31 H 0.9594 0.7862 0.3742 0.040 Uiso 1 1 calc R . . C4 C 0.7967(4) 0.7824(3) 0.30184(17) 0.0319(8) Uani 1 1 d . . . C5 C 0.6232(5) 0.7474(4) 0.28177(18) 0.0383(9) Uani 1 1 d . . . H51 H 0.5887 0.7629 0.2432 0.046 Uiso 1 1 calc R . . C6 C 0.5023(4) 0.6899(4) 0.31863(18) 0.0372(9) Uani 1 1 d . . . H61 H 0.3871 0.6658 0.3042 0.045 Uiso 1 1 calc R . . C7 C 0.9297(5) 0.8445(4) 0.26109(18) 0.0356(8) Uani 1 1 d . . . H71 H 1.0076 0.9304 0.2872 0.043 Uiso 1 1 calc R . . H72 H 0.8731 0.8648 0.2260 0.043 Uiso 1 1 calc R . . C8 C 1.0345(4) 0.7500(4) 0.23261(17) 0.0336(8) Uani 1 1 d . . . H81 H 1.0601 0.7071 0.2661 0.040 Uiso 1 1 calc R . . P2 P 1.23566(12) 0.84852(11) 0.21156(5) 0.0404(3) Uani 1 1 d . . . O21 O 1.3314(3) 0.7663(3) 0.17676(13) 0.0495(7) Uani 1 1 d . . . O22 O 1.3241(3) 0.9419(3) 0.27933(14) 0.0513(7) Uani 1 1 d . . . C30 C 1.4789(7) 1.0580(5) 0.2823(2) 0.0764(15) Uani 1 1 d D . . H301 H 1.4482 1.1387 0.2807 0.092 Uiso 1 1 calc R . . H302 H 1.5396 1.0372 0.2457 0.092 Uiso 1 1 calc R . . C31 C 1.5892(6) 1.0851(5) 0.3422(2) 0.0694(14) Uani 1 1 d D . . H311 H 1.5270 1.1015 0.3783 0.104 Uiso 1 1 calc R . . H312 H 1.6873 1.1643 0.3452 0.104 Uiso 1 1 calc R . . H313 H 1.6255 1.0073 0.3424 0.104 Uiso 1 1 calc R . . O23 O 1.1962(3) 0.9511(3) 0.17557(13) 0.0472(7) Uani 1 1 d . . . C32 C 1.2070(8) 0.9340(6) 0.1074(2) 0.0819(17) Uani 1 1 d D . . H321 H 1.1617 0.8373 0.0856 0.098 Uiso 1 1 calc R . . H322 H 1.3256 0.9673 0.1000 0.098 Uiso 1 1 calc R . . C33 C 1.1107(10) 1.0092(7) 0.0808(4) 0.137(3) Uani 1 1 d D . . H331 H 1.1366 1.0995 0.1085 0.206 Uiso 1 1 calc R . . H332 H 0.9907 0.9612 0.0776 0.206 Uiso 1 1 calc R . . H333 H 1.1420 1.0160 0.0388 0.206 Uiso 1 1 calc R . . P3 P 0.91822(14) 0.61462(11) 0.16374(5) 0.0456(3) Uani 1 1 d . . . O31 O 0.8851(4) 0.6644(3) 0.10838(15) 0.0687(9) Uani 1 1 d . . . O32 O 1.0167(4) 0.5071(3) 0.15035(15) 0.0622(8) Uani 1 1 d . . . C40 C 1.1027(8) 0.4825(5) 0.0943(3) 0.0810(17) Uani 1 1 d . . . H401 H 1.2221 0.4983 0.1075 0.097 Uiso 1 1 calc R . . H402 H 1.0968 0.5459 0.0687 0.097 Uiso 1 1 calc R . . C41 C 1.0252(9) 0.3425(6) 0.0558(3) 0.105(2) Uani 1 1 d . . . H411 H 1.0361 0.2798 0.0806 0.158 Uiso 1 1 calc R . . H412 H 1.0818 0.3289 0.0179 0.158 Uiso 1 1 calc R . . H413 H 0.9066 0.3263 0.0436 0.158 Uiso 1 1 calc R . . O33 O 0.7603(4) 0.5395(3) 0.19384(15) 0.0599(8) Uani 1 1 d . . . C42 C 0.6233(9) 0.4370(8) 0.1503(3) 0.139(3) Uani 1 1 d D . . H421 H 0.6687 0.3771 0.1201 0.167 Uiso 1 1 calc R . . H422 H 0.5655 0.4806 0.1259 0.167 Uiso 1 1 calc R . . C43 C 0.5017(10) 0.3561(9) 0.1851(4) 0.177(4) Uani 1 1 d D . . H431 H 0.5298 0.3968 0.2305 0.265 Uiso 1 1 calc R . . H432 H 0.5066 0.2643 0.1758 0.265 Uiso 1 1 calc R . . H433 H 0.3886 0.3539 0.1720 0.265 Uiso 1 1 calc R . . C10 C 0.2940(4) 0.7123(3) 0.46390(17) 0.0287(8) Uani 1 1 d . . . C11 C 0.1782(4) 0.6738(4) 0.50634(18) 0.0356(9) Uani 1 1 d . . . H111 H 0.1580 0.5887 0.5153 0.043 Uiso 1 1 calc R . . C12 C 0.0921(5) 0.7601(4) 0.5356(2) 0.0422(9) Uani 1 1 d . . . H121 H 0.0125 0.7322 0.5633 0.051 Uiso 1 1 calc R . . C13 C 0.1251(5) 0.8876(4) 0.5235(2) 0.0418(10) Uani 1 1 d . . . H131 H 0.0666 0.9453 0.5430 0.050 Uiso 1 1 calc R . . C14 C 0.2431(5) 0.9307(4) 0.48309(19) 0.0405(9) Uani 1 1 d . . . H141 H 0.2670 1.0181 0.4763 0.049 Uiso 1 1 calc R . . C15 C 0.3271(4) 0.8420(3) 0.45216(18) 0.0322(8) Uani 1 1 d . . . H151 H 0.4049 0.8694 0.4238 0.039 Uiso 1 1 calc R . . C20 C 0.2208(4) 0.4707(4) 0.36199(18) 0.0340(8) Uani 1 1 d . . . C21 C 0.2519(5) 0.3626(4) 0.31926(19) 0.0440(10) Uani 1 1 d . . . H211 H 0.3572 0.3493 0.3239 0.053 Uiso 1 1 calc R . . C22 C 0.1298(6) 0.2753(5) 0.2704(2) 0.0591(12) Uani 1 1 d . . . H221 H 0.1527 0.2034 0.2425 0.071 Uiso 1 1 calc R . . C23 C -0.0262(7) 0.2936(5) 0.2626(2) 0.0690(14) Uani 1 1 d . . . H231 H -0.1089 0.2346 0.2296 0.083 Uiso 1 1 calc R . . C24 C -0.0591(5) 0.4001(5) 0.3042(2) 0.0604(13) Uani 1 1 d . . . H241 H -0.1642 0.4131 0.2988 0.073 Uiso 1 1 calc R . . C25 C 0.0625(5) 0.4875(4) 0.3536(2) 0.0415(9) Uani 1 1 d . . . H251 H 0.0381 0.5585 0.3816 0.050 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 0.0249(2) 0.0243(2) 0.0322(2) 0.01054(16) 0.00534(15) 0.01154(16) Cl1 0.0355(5) 0.0229(4) 0.0426(6) 0.0095(4) 0.0021(4) 0.0100(4) P1 0.0256(4) 0.0255(5) 0.0344(5) 0.0120(4) 0.0041(4) 0.0108(4) C1 0.0284(18) 0.0295(19) 0.037(2) 0.0130(16) 0.0053(15) 0.0133(15) C2 0.0312(18) 0.037(2) 0.032(2) 0.0107(16) 0.0028(15) 0.0177(16) C3 0.0257(17) 0.038(2) 0.039(2) 0.0100(17) 0.0056(16) 0.0132(16) C4 0.0325(19) 0.0329(19) 0.034(2) 0.0088(16) 0.0095(16) 0.0145(16) C5 0.040(2) 0.049(2) 0.039(2) 0.0249(19) 0.0091(17) 0.0230(19) C6 0.0280(18) 0.047(2) 0.044(2) 0.0213(19) 0.0050(16) 0.0147(17) C7 0.037(2) 0.037(2) 0.038(2) 0.0139(17) 0.0144(16) 0.0149(17) C8 0.0332(19) 0.040(2) 0.032(2) 0.0124(17) 0.0108(16) 0.0140(17) P2 0.0321(5) 0.0508(6) 0.0411(6) 0.0170(5) 0.0096(4) 0.0129(5) O21 0.0377(15) 0.071(2) 0.0483(18) 0.0204(15) 0.0136(13) 0.0253(15) O22 0.0383(15) 0.0580(18) 0.0511(19) 0.0154(15) 0.0047(13) 0.0051(14) C30 0.079(4) 0.058(3) 0.075(4) 0.017(3) -0.007(3) 0.000(3) C31 0.056(3) 0.057(3) 0.082(4) 0.003(3) 0.009(3) 0.011(2) O23 0.0456(16) 0.0551(18) 0.0486(18) 0.0241(14) 0.0165(13) 0.0177(14) C32 0.114(5) 0.101(4) 0.057(4) 0.043(3) 0.025(3) 0.055(4) C33 0.199(8) 0.128(6) 0.096(6) 0.050(5) -0.030(5) 0.057(6) P3 0.0504(6) 0.0454(6) 0.0382(6) 0.0064(5) 0.0063(5) 0.0142(5) O31 0.095(3) 0.066(2) 0.0436(19) 0.0076(16) -0.0082(17) 0.0312(19) O32 0.087(2) 0.0525(19) 0.055(2) 0.0099(15) 0.0233(17) 0.0345(18) C40 0.106(4) 0.067(4) 0.077(4) 0.007(3) 0.039(3) 0.043(3) C41 0.155(6) 0.074(4) 0.087(5) 0.006(3) 0.054(4) 0.042(4) O33 0.0445(16) 0.0557(19) 0.060(2) -0.0004(15) 0.0013(14) -0.0004(14) C42 0.099(5) 0.138(7) 0.091(5) -0.003(5) -0.013(4) -0.061(5) C43 0.131(7) 0.165(9) 0.138(8) 0.018(6) -0.029(6) -0.070(6) C10 0.0217(16) 0.0272(18) 0.039(2) 0.0097(16) 0.0011(14) 0.0089(14) C11 0.0307(19) 0.0299(19) 0.053(2) 0.0206(18) 0.0113(17) 0.0115(16) C12 0.032(2) 0.048(2) 0.055(3) 0.018(2) 0.0152(18) 0.0194(18) C13 0.034(2) 0.036(2) 0.059(3) 0.0056(19) 0.0031(18) 0.0211(18) C14 0.040(2) 0.027(2) 0.057(3) 0.0137(18) 0.0003(19) 0.0143(17) C15 0.0265(17) 0.0284(19) 0.044(2) 0.0146(16) 0.0026(15) 0.0077(15) C20 0.036(2) 0.033(2) 0.037(2) 0.0180(17) 0.0038(16) 0.0110(17) C21 0.051(2) 0.039(2) 0.040(2) 0.0077(19) 0.0005(19) 0.0147(19) C22 0.078(3) 0.045(3) 0.042(3) 0.001(2) -0.008(2) 0.011(2) C23 0.077(4) 0.054(3) 0.054(3) 0.006(3) -0.024(3) -0.002(3) C24 0.038(2) 0.062(3) 0.071(3) 0.023(3) -0.019(2) -0.001(2) C25 0.035(2) 0.036(2) 0.051(3) 0.0146(19) -0.0047(18) 0.0060(17) _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 2.3022(8) 2_666 ? Pd1 Cl1 2.3022(8) . ? Pd1 P1 2.3275(8) 2_666 ? Pd1 P1 2.3275(8) . ? P1 C10 1.812(3) . ? P1 C1 1.821(3) . ? P1 C20 1.824(4) . ? C1 C6 1.382(5) . ? C1 C2 1.404(4) . ? C2 C3 1.382(5) . ? C2 H21 0.9300 . ? C3 C4 1.376(5) . ? C3 H31 0.9300 . ? C4 C5 1.394(5) . ? C4 C7 1.517(5) . ? C5 C6 1.381(5) . ? C5 H51 0.9300 . ? C6 H61 0.9300 . ? C7 C8 1.557(5) . ? C7 H71 0.9700 . ? C7 H72 0.9700 . ? C8 P3 1.805(4) . ? C8 P2 1.810(4) . ? C8 H81 0.9800 . ? P2 O21 1.456(3) . ? P2 O23 1.567(3) . ? P2 O22 1.567(3) . ? O22 C30 1.467(5) . ? C30 C31 1.467(4) . ? C30 H301 0.9700 . ? C30 H302 0.9700 . ? C31 H311 0.9600 . ? C31 H312 0.9600 . ? C31 H313 0.9600 . ? O23 C32 1.444(5) . ? C32 C33 1.468(4) . ? C32 H321 0.9700 . ? C32 H322 0.9700 . ? C33 H331 0.9600 . ? C33 H332 0.9600 . ? C33 H333 0.9600 . ? P3 O31 1.452(3) . ? P3 O33 1.557(3) . ? P3 O32 1.575(3) . ? O32 C40 1.436(5) . ? C40 C41 1.454(8) . ? C40 H401 0.9700 . ? C40 H402 0.9700 . ? C41 H411 0.9600 . ? C41 H412 0.9600 . ? C41 H413 0.9600 . ? O33 C42 1.431(6) . ? C42 C43 1.459(4) . ? C42 H421 0.9700 . ? C42 H422 0.9700 . ? C43 H431 0.9600 . ? C43 H432 0.9600 . ? C43 H433 0.9600 . ? C10 C11 1.383(5) . ? C10 C15 1.397(5) . ? C11 C12 1.383(5) . ? C11 H111 0.9300 . ? C12 C13 1.378(5) . ? C12 H121 0.9300 . ? C13 C14 1.375(5) . ? C13 H131 0.9300 . ? C14 C15 1.401(5) . ? C14 H141 0.9300 . ? C15 H151 0.9300 . ? C20 C25 1.388(5) . ? C20 C21 1.394(5) . ? C21 C22 1.373(6) . ? C21 H211 0.9300 . ? C22 C23 1.374(7) . ? C22 H221 0.9300 . ? C23 C24 1.375(7) . ? C23 H231 0.9300 . ? C24 C25 1.379(6) . ? C24 H241 0.9300 . ? C25 H251 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl1 Pd1 Cl1 180.0 2_666 . ? Cl1 Pd1 P1 92.99(3) 2_666 2_666 ? Cl1 Pd1 P1 87.01(3) . 2_666 ? Cl1 Pd1 P1 87.01(3) 2_666 . ? Cl1 Pd1 P1 92.99(3) . . ? P1 Pd1 P1 180.00(3) 2_666 . ? C10 P1 C1 108.82(15) . . ? C10 P1 C20 103.16(16) . . ? C1 P1 C20 101.91(16) . . ? C10 P1 Pd1 109.97(11) . . ? C1 P1 Pd1 113.26(10) . . ? C20 P1 Pd1 118.83(11) . . ? C6 C1 C2 118.2(3) . . ? C6 C1 P1 121.2(3) . . ? C2 C1 P1 120.5(3) . . ? C3 C2 C1 120.1(3) . . ? C3 C2 H21 119.9 . . ? C1 C2 H21 119.9 . . ? C4 C3 C2 121.5(3) . . ? C4 C3 H31 119.3 . . ? C2 C3 H31 119.3 . . ? C3 C4 C5 118.4(3) . . ? C3 C4 C7 121.0(3) . . ? C5 C4 C7 120.6(3) . . ? C6 C5 C4 120.6(3) . . ? C6 C5 H51 119.7 . . ? C4 C5 H51 119.7 . . ? C5 C6 C1 121.2(3) . . ? C5 C6 H61 119.4 . . ? C1 C6 H61 119.4 . . ? C4 C7 C8 113.7(3) . . ? C4 C7 H71 108.8 . . ? C8 C7 H71 108.8 . . ? C4 C7 H72 108.8 . . ? C8 C7 H72 108.8 . . ? H71 C7 H72 107.7 . . ? C7 C8 P3 112.6(2) . . ? C7 C8 P2 111.1(2) . . ? P3 C8 P2 109.92(18) . . ? C7 C8 H81 107.7 . . ? P3 C8 H81 107.7 . . ? P2 C8 H81 107.7 . . ? O21 P2 O23 114.06(16) . . ? O21 P2 O22 115.49(16) . . ? O23 P2 O22 103.64(16) . . ? O21 P2 C8 114.53(17) . . ? O23 P2 C8 106.84(15) . . ? O22 P2 C8 100.85(16) . . ? C30 O22 P2 118.4(3) . . ? O22 C30 C31 109.7(4) . . ? O22 C30 H301 109.7 . . ? C31 C30 H301 109.7 . . ? O22 C30 H302 109.7 . . ? C31 C30 H302 109.7 . . ? H301 C30 H302 108.2 . . ? C30 C31 H311 109.5 . . ? C30 C31 H312 109.5 . . ? H311 C31 H312 109.5 . . ? C30 C31 H313 109.5 . . ? H311 C31 H313 109.5 . . ? H312 C31 H313 109.5 . . ? C32 O23 P2 121.1(3) . . ? O23 C32 C33 110.7(5) . . ? O23 C32 H321 109.5 . . ? C33 C32 H321 109.5 . . ? O23 C32 H322 109.5 . . ? C33 C32 H322 109.5 . . ? H321 C32 H322 108.1 . . ? C32 C33 H331 109.5 . . ? C32 C33 H332 109.5 . . ? H331 C33 H332 109.5 . . ? C32 C33 H333 109.5 . . ? H331 C33 H333 109.5 . . ? H332 C33 H333 109.5 . . ? O31 P3 O33 117.00(19) . . ? O31 P3 O32 114.35(18) . . ? O33 P3 O32 102.44(17) . . ? O31 P3 C8 113.23(18) . . ? O33 P3 C8 100.85(16) . . ? O32 P3 C8 107.51(17) . . ? C40 O32 P3 123.8(3) . . ? O32 C40 C41 110.7(5) . . ? O32 C40 H401 109.5 . . ? C41 C40 H401 109.5 . . ? O32 C40 H402 109.5 . . ? C41 C40 H402 109.5 . . ? H401 C40 H402 108.1 . . ? C40 C41 H411 109.5 . . ? C40 C41 H412 109.5 . . ? H411 C41 H412 109.5 . . ? C40 C41 H413 109.5 . . ? H411 C41 H413 109.5 . . ? H412 C41 H413 109.5 . . ? C42 O33 P3 116.8(3) . . ? O33 C42 C43 110.7(5) . . ? O33 C42 H421 109.5 . . ? C43 C42 H421 109.5 . . ? O33 C42 H422 109.5 . . ? C43 C42 H422 109.5 . . ? H421 C42 H422 108.1 . . ? C42 C43 H431 109.5 . . ? C42 C43 H432 109.5 . . ? H431 C43 H432 109.5 . . ? C42 C43 H433 109.5 . . ? H431 C43 H433 109.5 . . ? H432 C43 H433 109.5 . . ? C11 C10 C15 119.0(3) . . ? C11 C10 P1 117.5(2) . . ? C15 C10 P1 123.4(3) . . ? C10 C11 C12 121.0(3) . . ? C10 C11 H111 119.5 . . ? C12 C11 H111 119.5 . . ? C13 C12 C11 119.5(3) . . ? C13 C12 H121 120.3 . . ? C11 C12 H121 120.3 . . ? C14 C13 C12 121.0(3) . . ? C14 C13 H131 119.5 . . ? C12 C13 H131 119.5 . . ? C13 C14 C15 119.4(3) . . ? C13 C14 H141 120.3 . . ? C15 C14 H141 120.3 . . ? C10 C15 C14 120.0(3) . . ? C10 C15 H151 120.0 . . ? C14 C15 H151 120.0 . . ? C25 C20 C21 117.9(4) . . ? C25 C20 P1 122.6(3) . . ? C21 C20 P1 119.5(3) . . ? C22 C21 C20 121.1(4) . . ? C22 C21 H211 119.4 . . ? C20 C21 H211 119.4 . . ? C21 C22 C23 120.3(4) . . ? C21 C22 H221 119.9 . . ? C23 C22 H221 119.9 . . ? C22 C23 C24 119.5(4) . . ? C22 C23 H231 120.3 . . ? C24 C23 H231 120.3 . . ? C23 C24 C25 120.6(4) . . ? C23 C24 H241 119.7 . . ? C25 C24 H241 119.7 . . ? C24 C25 C20 120.6(4) . . ? C24 C25 H251 119.7 . . ? C20 C25 H251 119.7 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.08 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.583 _refine_diff_density_min -0.635 _refine_diff_density_rms 0.088 _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla, M.C., Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, p. 435. Coppens, P. (1970). Crystallographic Computing, edited by F.R. Ahmed, S.R.Hall & C.P. Huber, pp. 255-270, Copenhagen, Munksgaard. Hooft, R.W. (1998). COLLECT. Nonius BV, Delft, The Netherlands. Otwinowski, Z. & Minor, W. (1997). Methods Enzymol. 276, 307--326. Sheldrick, G. M. (1997). SHELXL97. University of G\"ottingen, Germany. Spek, A.L. (1999). PLATON. Version 1999. Utrecht University, The Netherlands. ; # Attachment 'ptbisp2 new.cif' data_ptbisp2 _database_code_depnum_ccdc_archive 'CCDC 705471' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C94 H104 Cl4 O12 P8 Pt2, 7(C H2 Cl2)' _chemical_formula_sum 'C101 H118 Cl18 O12 P8 Pt2' _chemical_formula_weight 2799.98 _chemical_compound_source 'synthesized by the authors' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 17.5897(2) _cell_length_b 18.3345(3) _cell_length_c 20.9857(3) _cell_angle_alpha 84.3179(7) _cell_angle_beta 68.7386(9) _cell_angle_gamma 69.7078(9) _cell_volume 5912.99(15) _cell_formula_units_Z 2 _cell_measurement_temperature 150(1) _cell_measurement_reflns_used 25286 _cell_measurement_theta_min 1 _cell_measurement_theta_max 27.48 _exptl_crystal_description prism _exptl_crystal_colour 'light yellow' _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.573 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2804 _exptl_absorpt_coefficient_mu 2.933 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.422 _exptl_absorpt_correction_T_max 0.578 _exptl_absorpt_process_details ; Gaussian integration (Coppens, 1970) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(1) _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 'Nonius KappaCCD area detector' _diffrn_measurement_method '\f and \w scans to fill the Ewald sphere' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 50678 _diffrn_reflns_av_R_equivalents 0.0246 _diffrn_reflns_av_sigmaI/netI 0.0377 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.36 _diffrn_reflns_theta_max 27.58 _reflns_number_total 26966 _reflns_number_gt 21505 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Hooft, 1998) and DENZO (Otwinowski & Minor, 1997)' _computing_cell_refinement 'COLLECT and DENZO' _computing_data_reduction 'COLLECT and DENZO' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _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^)+(0.0710P)^2^+40.9412P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 26966 _refine_ls_number_parameters 1265 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.0708 _refine_ls_R_factor_gt 0.0525 _refine_ls_wR_factor_ref 0.1515 _refine_ls_wR_factor_gt 0.1362 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.030 _refine_ls_shift/su_max 0.013 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.342526(14) 0.872113(12) 0.258823(11) 0.02424(6) Uani 1 1 d . . . Cl1 Cl 0.36100(10) 0.90815(9) 0.35594(8) 0.0363(3) Uani 1 1 d . . . Cl2 Cl 0.19522(11) 0.94136(12) 0.31228(9) 0.0487(5) Uani 1 1 d . . . Pt2 Pt 0.770673(14) 0.158974(13) 0.237714(11) 0.02600(7) Uani 1 1 d . . . Cl3 Cl 0.79973(10) 0.02501(8) 0.24267(8) 0.0327(3) Uani 1 1 d . . . Cl4 Cl 0.73010(12) 0.29334(9) 0.23835(8) 0.0392(4) Uani 1 1 d . . . C1 C 0.3577(4) 0.4336(3) 0.1742(3) 0.0255(11) Uani 1 1 d . . . P1A P 0.25079(10) 0.46387(9) 0.16577(9) 0.0317(3) Uani 1 1 d . . . O1A O 0.2570(3) 0.4490(3) 0.0972(3) 0.0543(15) Uani 1 1 d . . . O2A O 0.1962(3) 0.4240(3) 0.2235(3) 0.0480(12) Uani 1 1 d . . . C30A C 0.1845(10) 0.3522(9) 0.2167(7) 0.124(6) Uani 1 1 d D . . H30O H 0.2361 0.3099 0.2171 0.149 Uiso 1 1 calc R . . H30P H 0.1796 0.3502 0.1724 0.149 Uiso 1 1 calc R . . C31A C 0.1085(9) 0.3382(9) 0.2698(10) 0.169(9) Uani 1 1 d D . . H31O H 0.1102 0.3434 0.3142 0.202 Uiso 1 1 calc R . . H31P H 0.1096 0.2867 0.2633 0.202 Uiso 1 1 calc R . . H31Q H 0.0563 0.3756 0.2661 0.202 Uiso 1 1 calc R . . O3A O 0.2067(3) 0.5500(3) 0.1917(3) 0.0433(11) Uani 1 1 d . . . C32A C 0.1436(5) 0.6066(5) 0.1672(5) 0.071(3) Uani 1 1 d D . . H32O H 0.1548 0.5926 0.1205 0.086 Uiso 1 1 calc R . . H32P H 0.1498 0.6572 0.1670 0.086 Uiso 1 1 calc R . . C33A C 0.0537(6) 0.6118(13) 0.2100(9) 0.218(14) Uani 1 1 d D . . H33O H 0.0506 0.5604 0.2190 0.261 Uiso 1 1 calc R . . H33P H 0.0153 0.6396 0.1862 0.261 Uiso 1 1 calc R . . H33Q H 0.0371 0.6388 0.2524 0.261 Uiso 1 1 calc R . . C2A C 0.4115(4) 0.4843(3) 0.1292(3) 0.0293(12) Uani 1 1 d . . . H2A1 H 0.4696 0.4615 0.1304 0.035 Uiso 1 1 calc R . . H2A2 H 0.4159 0.4784 0.0825 0.035 Uiso 1 1 calc R . . C3A C 0.3828(4) 0.5705(3) 0.1445(3) 0.0249(11) Uani 1 1 d . . . C4A C 0.3984(4) 0.5995(3) 0.1952(3) 0.0299(12) Uani 1 1 d . . . H4A H 0.4229 0.5652 0.2237 0.036 Uiso 1 1 calc R . . C5A C 0.3782(4) 0.6794(3) 0.2044(3) 0.0279(12) Uani 1 1 d . . . H5A H 0.3886 0.6976 0.2392 0.033 Uiso 1 1 calc R . . C6A C 0.3426(4) 0.7317(3) 0.1615(3) 0.0250(11) Uani 1 1 d . . . C7A C 0.3239(4) 0.7028(3) 0.1119(3) 0.0274(12) Uani 1 1 d . . . H7A H 0.2973 0.7373 0.0845 0.033 Uiso 1 1 calc R . . C8A C 0.3445(4) 0.6237(3) 0.1029(3) 0.0297(12) Uani 1 1 d . . . H8A H 0.3328 0.6055 0.0688 0.036 Uiso 1 1 calc R . . P2A P 0.31731(9) 0.83571(8) 0.17137(7) 0.0233(3) Uani 1 1 d . . . C10A C 0.2049(4) 0.8710(4) 0.1748(3) 0.0310(13) Uani 1 1 d . . . C11A C 0.1772(5) 0.9263(4) 0.1304(4) 0.0419(16) Uani 1 1 d . . . H11A H 0.2157 0.9472 0.0978 0.050 Uiso 1 1 calc R . . C12A C 0.0902(5) 0.9501(5) 0.1355(5) 0.057(2) Uani 1 1 d . . . H12A H 0.0714 0.9869 0.1059 0.069 Uiso 1 1 calc R . . C13A C 0.0332(5) 0.9205(6) 0.1828(5) 0.062(2) Uani 1 1 d . . . H13A H -0.0243 0.9374 0.1857 0.074 Uiso 1 1 calc R . . C14A C 0.0608(5) 0.8646(6) 0.2273(4) 0.059(2) Uani 1 1 d . . . H14A H 0.0221 0.8438 0.2598 0.071 Uiso 1 1 calc R . . C15A C 0.1479(5) 0.8402(5) 0.2221(4) 0.0426(16) Uani 1 1 d . . . H15A H 0.1670 0.8026 0.2511 0.051 Uiso 1 1 calc R . . C20A C 0.3741(4) 0.8715(3) 0.0899(3) 0.0255(11) Uani 1 1 d . . . C21A C 0.3679(4) 0.9496(3) 0.0903(3) 0.0318(13) Uani 1 1 d . . . H21A H 0.3394 0.9789 0.1311 0.038 Uiso 1 1 calc R . . C22A C 0.4039(5) 0.9828(4) 0.0307(4) 0.0387(15) Uani 1 1 d . . . H22A H 0.3996 1.0348 0.0312 0.046 Uiso 1 1 calc R . . C23A C 0.4469(5) 0.9395(4) -0.0303(3) 0.0384(15) Uani 1 1 d . . . H23A H 0.4700 0.9628 -0.0707 0.046 Uiso 1 1 calc R . . C24A C 0.4551(4) 0.8622(4) -0.0310(3) 0.0346(14) Uani 1 1 d . . . H24A H 0.4849 0.8330 -0.0718 0.041 Uiso 1 1 calc R . . C25A C 0.4189(4) 0.8275(3) 0.0294(3) 0.0280(12) Uani 1 1 d . . . H25A H 0.4248 0.7751 0.0289 0.034 Uiso 1 1 calc R . . P1B P 0.35089(11) 0.42623(9) 0.26375(8) 0.0298(3) Uani 1 1 d . . . O1B O 0.3296(3) 0.3581(3) 0.2981(2) 0.0396(11) Uani 1 1 d . . . O2B O 0.4433(3) 0.4268(2) 0.2551(2) 0.0339(10) Uani 1 1 d . . . C30B C 0.4781(6) 0.4050(4) 0.3104(4) 0.0471(18) Uani 1 1 d . . . H30R H 0.5369 0.3688 0.2927 0.057 Uiso 1 1 calc R . . H30S H 0.4434 0.3792 0.3454 0.057 Uiso 1 1 calc R . . C31B C 0.4777(7) 0.4751(6) 0.3407(5) 0.064(3) Uani 1 1 d . . . H31R H 0.5238 0.4921 0.3103 0.077 Uiso 1 1 calc R . . H31S H 0.4858 0.4625 0.3838 0.077 Uiso 1 1 calc R . . H31T H 0.4233 0.5158 0.3476 0.077 Uiso 1 1 calc R . . O3B O 0.2863(3) 0.5063(3) 0.2998(2) 0.0417(11) Uani 1 1 d . . . C32B C 0.2148(8) 0.5129(6) 0.3607(6) 0.108(5) Uani 1 1 d D . . H32R H 0.2324 0.5137 0.3994 0.130 Uiso 1 1 calc R . . H32S H 0.1977 0.4673 0.3641 0.130 Uiso 1 1 calc R . . C33B C 0.1389(8) 0.5834(8) 0.3652(7) 0.129(6) Uani 1 1 d D . . H33R H 0.1544 0.6290 0.3644 0.155 Uiso 1 1 calc R . . H33S H 0.0922 0.5837 0.4071 0.155 Uiso 1 1 calc R . . H33T H 0.1211 0.5833 0.3271 0.155 Uiso 1 1 calc R . . C2B C 0.4024(4) 0.3484(3) 0.1416(3) 0.0276(12) Uani 1 1 d . . . H2B1 H 0.3672 0.3174 0.1675 0.033 Uiso 1 1 calc R . . H2B2 H 0.4013 0.3510 0.0955 0.033 Uiso 1 1 calc R . . C3B C 0.4949(4) 0.3055(3) 0.1378(3) 0.0252(11) Uani 1 1 d . . . C4B C 0.5120(4) 0.2534(3) 0.1882(3) 0.0271(12) Uani 1 1 d . . . H4B H 0.4662 0.2467 0.2253 0.032 Uiso 1 1 calc R . . C5B C 0.5966(4) 0.2115(3) 0.1833(3) 0.0283(12) Uani 1 1 d . . . H5B H 0.6068 0.1780 0.2178 0.034 Uiso 1 1 calc R . . C6B C 0.6664(4) 0.2191(3) 0.1273(3) 0.0276(12) Uani 1 1 d . . . C7B C 0.6491(4) 0.2715(3) 0.0769(3) 0.0275(12) Uani 1 1 d . . . H7B H 0.6945 0.2785 0.0396 0.033 Uiso 1 1 calc R . . C8B C 0.5644(4) 0.3129(3) 0.0826(3) 0.0271(12) Uani 1 1 d . . . H8B H 0.5539 0.3466 0.0483 0.033 Uiso 1 1 calc R . . P2B P 0.77539(10) 0.16299(9) 0.12606(8) 0.0272(3) Uani 1 1 d . . . C10B C 0.8026(4) 0.0695(3) 0.0856(3) 0.0315(13) Uani 1 1 d . . . C11B C 0.7450(4) 0.0464(4) 0.0698(4) 0.0377(15) Uani 1 1 d . . . H11B H 0.6885 0.0799 0.0790 0.045 Uiso 1 1 calc R . . C12B C 0.7707(6) -0.0269(4) 0.0401(4) 0.0518(19) Uani 1 1 d . . . H12B H 0.7312 -0.0420 0.0297 0.062 Uiso 1 1 calc R . . C13B C 0.8539(6) -0.0771(4) 0.0262(4) 0.055(2) Uani 1 1 d . . . H13B H 0.8705 -0.1262 0.0069 0.066 Uiso 1 1 calc R . . C14B C 0.9125(5) -0.0545(4) 0.0409(4) 0.052(2) Uani 1 1 d . . . H14B H 0.9692 -0.0881 0.0310 0.062 Uiso 1 1 calc R . . C15B C 0.8877(4) 0.0178(4) 0.0704(4) 0.0429(16) Uani 1 1 d . . . H15B H 0.9278 0.0326 0.0803 0.051 Uiso 1 1 calc R . . C20B C 0.8479(4) 0.2069(4) 0.0619(3) 0.0320(13) Uani 1 1 d . . . C21B C 0.8613(4) 0.1993(4) -0.0075(3) 0.0379(15) Uani 1 1 d . . . H21B H 0.8352 0.1702 -0.0207 0.045 Uiso 1 1 calc R . . C22B C 0.9130(5) 0.2348(4) -0.0561(4) 0.0460(18) Uani 1 1 d . . . H22B H 0.9203 0.2308 -0.1019 0.055 Uiso 1 1 calc R . . C23B C 0.9537(6) 0.2759(5) -0.0374(5) 0.062(2) Uani 1 1 d . . . H23B H 0.9883 0.3000 -0.0704 0.074 Uiso 1 1 calc R . . C24B C 0.9435(6) 0.2818(6) 0.0307(5) 0.064(2) Uani 1 1 d . . . H24B H 0.9718 0.3092 0.0431 0.076 Uiso 1 1 calc R . . C25B C 0.8906(5) 0.2465(5) 0.0809(4) 0.0473(17) Uani 1 1 d . . . H25B H 0.8844 0.2498 0.1266 0.057 Uiso 1 1 calc R . . C1C C 0.6973(4) 0.5410(3) 0.4128(3) 0.0280(12) Uani 1 1 d . . . P1C P 0.65508(11) 0.62893(9) 0.46734(8) 0.0298(3) Uani 1 1 d . . . O1C O 0.5728(3) 0.6345(3) 0.5222(2) 0.0384(10) Uani 1 1 d . . . O2C O 0.6508(3) 0.7016(2) 0.4210(2) 0.0372(10) Uani 1 1 d . . . C30C C 0.5722(6) 0.7702(4) 0.4388(5) 0.059(2) Uani 1 1 d D . . H30U H 0.5550 0.7864 0.4861 0.071 Uiso 1 1 calc R . . H30V H 0.5253 0.7578 0.4337 0.071 Uiso 1 1 calc R . . C31C C 0.5899(10) 0.8337(5) 0.3929(7) 0.126(6) Uani 1 1 d D . . H31U H 0.5652 0.8382 0.3582 0.151 Uiso 1 1 calc R . . H31V H 0.6514 0.8222 0.3718 0.151 Uiso 1 1 calc R . . H31W H 0.5648 0.8818 0.4190 0.151 Uiso 1 1 calc R . . O3C O 0.7344(3) 0.6175(3) 0.4906(2) 0.0382(10) Uani 1 1 d . . . C32C C 0.7330(5) 0.6776(4) 0.5317(4) 0.0476(18) Uani 1 1 d . . . H32U H 0.6980 0.6745 0.5791 0.057 Uiso 1 1 calc R . . H32V H 0.7077 0.7285 0.5157 0.057 Uiso 1 1 calc R . . C33C C 0.8231(7) 0.6662(6) 0.5259(7) 0.081(3) Uani 1 1 d . . . H33U H 0.8620 0.6207 0.4977 0.097 Uiso 1 1 calc R . . H33V H 0.8273 0.6597 0.5706 0.097 Uiso 1 1 calc R . . H33W H 0.8382 0.7109 0.5056 0.097 Uiso 1 1 calc R . . C2C C 0.6295(4) 0.5425(3) 0.3800(3) 0.0295(12) Uani 1 1 d . . . H2C1 H 0.6543 0.4963 0.3505 0.035 Uiso 1 1 calc R . . H2C2 H 0.5790 0.5372 0.4167 0.035 Uiso 1 1 calc R . . C3C C 0.5979(4) 0.6112(3) 0.3388(3) 0.0277(12) Uani 1 1 d . . . C4C C 0.5106(4) 0.6571(4) 0.3623(3) 0.0307(13) Uani 1 1 d . . . H4C H 0.4738 0.6461 0.4037 0.037 Uiso 1 1 calc R . . C5C C 0.4774(4) 0.7189(3) 0.3253(3) 0.0286(12) Uani 1 1 d . . . H5C H 0.4189 0.7487 0.3422 0.034 Uiso 1 1 calc R . . C6C C 0.5311(4) 0.7367(3) 0.2630(3) 0.0249(11) Uani 1 1 d . . . C7C C 0.6184(4) 0.6896(3) 0.2382(3) 0.0305(13) Uani 1 1 d . . . H7C H 0.6548 0.6994 0.1959 0.037 Uiso 1 1 calc R . . C8C C 0.6509(4) 0.6287(4) 0.2759(3) 0.0307(13) Uani 1 1 d . . . H8C H 0.7092 0.5987 0.2589 0.037 Uiso 1 1 calc R . . P2C P 0.48887(9) 0.81978(8) 0.21556(7) 0.0236(3) Uani 1 1 d . . . C10C C 0.5345(4) 0.8934(3) 0.2213(3) 0.0280(12) Uani 1 1 d . . . C11C C 0.4891(5) 0.9710(4) 0.2190(4) 0.0425(16) Uani 1 1 d . . . H11C H 0.4348 0.9860 0.2151 0.051 Uiso 1 1 calc R . . C12C C 0.5242(6) 1.0271(4) 0.2225(5) 0.052(2) Uani 1 1 d . . . H12C H 0.4932 1.0794 0.2204 0.062 Uiso 1 1 calc R . . C13C C 0.6030(6) 1.0069(5) 0.2291(4) 0.0511(19) Uani 1 1 d . . . H13C H 0.6249 1.0450 0.2332 0.061 Uiso 1 1 calc R . . C14C C 0.6493(6) 0.9303(5) 0.2295(6) 0.072(3) Uani 1 1 d . . . H14C H 0.7040 0.9156 0.2325 0.086 Uiso 1 1 calc R . . C15C C 0.6158(6) 0.8744(5) 0.2254(6) 0.066(3) Uani 1 1 d . . . H15C H 0.6486 0.8222 0.2254 0.079 Uiso 1 1 calc R . . C20C C 0.5498(4) 0.7836(3) 0.1266(3) 0.0254(11) Uani 1 1 d . . . C21C C 0.5619(4) 0.7086(3) 0.1076(3) 0.0300(12) Uani 1 1 d . . . H21C H 0.5357 0.6778 0.1396 0.036 Uiso 1 1 calc R . . C22C C 0.6126(4) 0.6792(4) 0.0414(3) 0.0345(14) Uani 1 1 d . . . H22C H 0.6202 0.6290 0.0293 0.041 Uiso 1 1 calc R . . C23C C 0.6518(4) 0.7248(4) -0.0066(3) 0.0372(14) Uani 1 1 d . . . H23C H 0.6856 0.7053 -0.0509 0.045 Uiso 1 1 calc R . . C24C C 0.6406(4) 0.7998(4) 0.0117(3) 0.0376(14) Uani 1 1 d . . . H24C H 0.6674 0.8302 -0.0204 0.045 Uiso 1 1 calc R . . C25C C 0.5893(4) 0.8291(3) 0.0777(3) 0.0319(13) Uani 1 1 d . . . H25C H 0.5811 0.8795 0.0894 0.038 Uiso 1 1 calc R . . P1D P 0.80520(11) 0.52991(11) 0.34859(10) 0.0383(4) Uani 1 1 d . . . O1D O 0.8193(4) 0.6035(3) 0.3202(3) 0.0568(14) Uani 1 1 d . . . O2D O 0.8092(3) 0.4744(3) 0.2944(3) 0.0458(12) Uani 1 1 d . . . C30D C 0.8895(7) 0.4509(9) 0.2350(6) 0.101(4) Uani 1 1 d D . . H30X H 0.9375 0.4224 0.2501 0.121 Uiso 1 1 calc R . . H30Y H 0.9004 0.4968 0.2122 0.121 Uiso 1 1 calc R . . C31D C 0.8840(14) 0.4016(17) 0.1866(11) 0.29(2) Uani 1 1 d D . . H31X H 0.8263 0.3996 0.2015 0.345 Uiso 1 1 calc R . . H31Y H 0.9243 0.3500 0.1848 0.345 Uiso 1 1 calc R . . H31Z H 0.8978 0.4231 0.1419 0.345 Uiso 1 1 calc R . . O3D O 0.8738(3) 0.4801(3) 0.3803(3) 0.0552(14) Uani 1 1 d . . . C32D C 0.9369(7) 0.5055(8) 0.3911(7) 0.098(4) Uani 1 1 d . . . H32X H 0.9101 0.5578 0.4111 0.117 Uiso 1 1 calc R . . H32Y H 0.9828 0.5056 0.3480 0.117 Uiso 1 1 calc R . . C33D C 0.9719(12) 0.4503(13) 0.4379(10) 0.182(10) Uani 1 1 d . . . H33X H 0.9416 0.4135 0.4521 0.219 Uiso 1 1 calc R . . H33Y H 0.9644 0.4783 0.4773 0.219 Uiso 1 1 calc R . . H33Z H 1.0324 0.4232 0.4148 0.219 Uiso 1 1 calc R . . C2D C 0.7009(5) 0.4727(3) 0.4647(3) 0.0341(14) Uani 1 1 d . . . H2D1 H 0.7497 0.4650 0.4790 0.041 Uiso 1 1 calc R . . H2D2 H 0.6489 0.4891 0.5050 0.041 Uiso 1 1 calc R . . C3D C 0.7088(4) 0.3950(3) 0.4391(3) 0.0337(14) Uani 1 1 d . . . C4D C 0.6356(4) 0.3748(3) 0.4517(3) 0.0315(13) Uani 1 1 d . . . H4D H 0.5816 0.4097 0.4760 0.038 Uiso 1 1 calc R . . C5D C 0.6407(4) 0.3043(3) 0.4291(3) 0.0317(13) Uani 1 1 d . . . H5D H 0.5906 0.2924 0.4381 0.038 Uiso 1 1 calc R . . C6D C 0.7216(4) 0.2509(3) 0.3926(3) 0.0292(12) Uani 1 1 d . . . C7D C 0.7953(4) 0.2704(4) 0.3809(4) 0.0381(15) Uani 1 1 d . . . H7D H 0.8494 0.2352 0.3570 0.046 Uiso 1 1 calc R . . C8D C 0.7899(4) 0.3402(4) 0.4038(4) 0.0382(15) Uani 1 1 d . . . H8D H 0.8402 0.3514 0.3958 0.046 Uiso 1 1 calc R . . P2D P 0.73707(10) 0.15961(8) 0.35466(8) 0.0264(3) Uani 1 1 d . . . C10D C 0.6348(4) 0.1408(3) 0.3846(3) 0.0304(12) Uani 1 1 d . . . C11D C 0.5678(4) 0.1900(4) 0.3649(3) 0.0371(14) Uani 1 1 d . . . H11D H 0.5722 0.2366 0.3447 0.044 Uiso 1 1 calc R . . C12D C 0.4947(5) 0.1719(5) 0.3745(4) 0.0472(18) Uani 1 1 d . . . H12D H 0.4501 0.2062 0.3615 0.057 Uiso 1 1 calc R . . C13D C 0.4884(5) 0.1023(5) 0.4037(4) 0.056(2) Uani 1 1 d . . . H13D H 0.4397 0.0892 0.4097 0.067 Uiso 1 1 calc R . . C14D C 0.5537(6) 0.0527(5) 0.4237(4) 0.054(2) Uani 1 1 d . . . H14D H 0.5490 0.0060 0.4435 0.065 Uiso 1 1 calc R . . C15D C 0.6273(5) 0.0714(4) 0.4147(4) 0.0440(16) Uani 1 1 d . . . H15D H 0.6712 0.0375 0.4287 0.053 Uiso 1 1 calc R . . C20D C 0.8113(4) 0.0900(3) 0.3914(3) 0.0298(12) Uani 1 1 d . . . C21D C 0.7872(5) 0.0824(4) 0.4623(3) 0.0387(15) Uani 1 1 d . . . H21D H 0.7311 0.1096 0.4904 0.046 Uiso 1 1 calc R . . C22D C 0.8457(6) 0.0351(4) 0.4905(4) 0.0490(19) Uani 1 1 d . . . H22D H 0.8290 0.0297 0.5377 0.059 Uiso 1 1 calc R . . C23D C 0.9301(6) -0.0050(4) 0.4483(4) 0.053(2) Uani 1 1 d . . . H23D H 0.9698 -0.0368 0.4676 0.064 Uiso 1 1 calc R . . C24D C 0.9551(5) 0.0024(4) 0.3787(4) 0.0473(18) Uani 1 1 d . . . H24D H 1.0116 -0.0243 0.3510 0.057 Uiso 1 1 calc R . . C25D C 0.8959(4) 0.0497(4) 0.3492(3) 0.0361(14) Uani 1 1 d . . . H25D H 0.9126 0.0544 0.3020 0.043 Uiso 1 1 calc R . . C1E C 0.6730(9) 0.4306(6) 0.1259(5) 0.080(3) Uani 1 1 d . . . H1E H 0.6242 0.4119 0.1427 0.096 Uiso 1 1 calc R . . H2E H 0.7235 0.3885 0.1286 0.096 Uiso 1 1 calc R . . Cl1E Cl 0.6906(3) 0.45569(16) 0.04056(15) 0.1036(12) Uani 1 1 d . . . Cl2E Cl 0.6531(2) 0.50679(17) 0.17723(15) 0.0921(9) Uani 1 1 d . . . C1F C 0.2049(10) 0.7738(9) 0.4374(6) 0.109(5) Uani 1 1 d . . . H1F H 0.2147 0.8182 0.4108 0.131 Uiso 1 1 calc R . . H2F H 0.2205 0.7733 0.4773 0.131 Uiso 1 1 calc R . . Cl1F Cl 0.0933(3) 0.7858(3) 0.4647(4) 0.206(3) Uani 1 1 d . . . Cl2F Cl 0.2679(2) 0.6946(3) 0.3915(2) 0.1255(14) Uani 1 1 d . . . C1G C 0.1719(10) 0.1243(8) 0.6060(9) 0.131(6) Uani 1 1 d . . . H1G H 0.1462 0.0865 0.6026 0.157 Uiso 1 1 calc R . . H2G H 0.1949 0.1094 0.6427 0.157 Uiso 1 1 calc R . . Cl1G Cl 0.2544(3) 0.1230(2) 0.5311(3) 0.1491(19) Uani 1 1 d . . . Cl2G Cl 0.0950(7) 0.2127(5) 0.6247(5) 0.352(8) Uani 1 1 d . . . C1H C 0.1809(9) 0.2772(7) 0.7667(7) 0.107(5) Uani 1 1 d . . . H1H H 0.2429 0.2555 0.7429 0.129 Uiso 1 1 calc R . . H2H H 0.1560 0.3157 0.7382 0.129 Uiso 1 1 calc R . . Cl1H Cl 0.1597(4) 0.3171(6) 0.8416(4) 0.241(4) Uani 1 1 d . . . Cl2H Cl 0.1275(6) 0.1932(5) 0.7877(7) 0.301(6) Uani 1 1 d . . . C1I C 0.1415(9) 0.4380(9) 0.0086(9) 0.120(5) Uani 1 1 d . . . H1I H 0.1471 0.4434 -0.0392 0.143 Uiso 1 1 calc R . . H2I H 0.1938 0.4394 0.0134 0.143 Uiso 1 1 calc R . . Cl1I Cl 0.0460(3) 0.5137(3) 0.0621(3) 0.1516(19) Uani 1 1 d . . . Cl2I Cl 0.1205(3) 0.3510(3) 0.0412(5) 0.223(4) Uani 1 1 d . . . C1J C 0.2342(11) 0.1077(10) 0.3605(9) 0.135(6) Uiso 1 1 d . . . H1J H 0.2550 0.0756 0.3943 0.162 Uiso 1 1 calc R . . H2J H 0.2453 0.0737 0.3232 0.162 Uiso 1 1 calc R . . Cl1J Cl 0.2951(2) 0.1749(2) 0.3275(2) 0.1173(12) Uani 1 1 d . . . Cl2J Cl 0.1200(3) 0.1556(3) 0.3984(3) 0.1371(15) Uani 1 1 d . . . C1K C 0.1016(10) 0.1169(9) 0.2202(9) 0.130(6) Uani 1 1 d . . . H1K H 0.0969 0.1290 0.2657 0.156 Uiso 1 1 calc R . . H2K H 0.1117 0.0616 0.2176 0.156 Uiso 1 1 calc R . . Cl1K Cl 0.0056(3) 0.1666(3) 0.2095(3) 0.170(2) Uani 1 1 d . . . Cl2K Cl 0.1884(5) 0.1357(4) 0.1630(6) 0.349(8) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.02574(11) 0.02109(11) 0.02472(11) -0.00457(8) -0.01213(9) -0.00162(8) Cl1 0.0370(8) 0.0397(8) 0.0299(7) -0.0110(6) -0.0153(6) -0.0033(6) Cl2 0.0295(8) 0.0618(11) 0.0448(9) -0.0271(8) -0.0154(7) 0.0066(7) Pt2 0.02596(11) 0.02435(11) 0.02725(12) 0.00094(8) -0.01323(9) -0.00389(8) Cl3 0.0345(7) 0.0281(7) 0.0363(8) -0.0003(6) -0.0173(6) -0.0061(6) Cl4 0.0536(10) 0.0276(7) 0.0361(8) 0.0043(6) -0.0207(7) -0.0088(7) C1 0.032(3) 0.019(3) 0.027(3) -0.001(2) -0.015(2) -0.005(2) P1A 0.0284(8) 0.0282(8) 0.0366(9) -0.0018(6) -0.0159(7) -0.0016(6) O1A 0.039(3) 0.070(4) 0.045(3) -0.016(3) -0.024(2) 0.008(3) O2A 0.034(3) 0.057(3) 0.058(3) 0.004(3) -0.023(2) -0.014(2) C30A 0.144(13) 0.109(11) 0.119(11) -0.025(9) 0.014(9) -0.097(10) C31A 0.094(11) 0.101(12) 0.29(3) -0.002(14) -0.013(14) -0.060(10) O3A 0.039(3) 0.029(2) 0.055(3) -0.004(2) -0.021(2) 0.004(2) C32A 0.056(5) 0.050(5) 0.089(7) 0.000(5) -0.038(5) 0.019(4) C33A 0.054(8) 0.34(3) 0.134(14) 0.111(17) -0.016(8) 0.039(12) C2A 0.033(3) 0.023(3) 0.029(3) -0.003(2) -0.010(2) -0.006(2) C3A 0.030(3) 0.020(3) 0.025(3) 0.001(2) -0.009(2) -0.009(2) C4A 0.038(3) 0.023(3) 0.034(3) 0.006(2) -0.021(3) -0.009(2) C5A 0.035(3) 0.026(3) 0.027(3) 0.002(2) -0.017(2) -0.011(2) C6A 0.029(3) 0.018(2) 0.027(3) 0.001(2) -0.012(2) -0.005(2) C7A 0.037(3) 0.022(3) 0.027(3) 0.002(2) -0.019(3) -0.008(2) C8A 0.042(3) 0.025(3) 0.027(3) -0.002(2) -0.016(3) -0.012(3) P2A 0.0260(7) 0.0190(6) 0.0264(7) -0.0019(5) -0.0133(6) -0.0043(5) C10A 0.027(3) 0.029(3) 0.035(3) -0.011(2) -0.015(3) -0.001(2) C11A 0.036(4) 0.043(4) 0.045(4) 0.002(3) -0.022(3) -0.003(3) C12A 0.040(4) 0.063(5) 0.065(5) -0.005(4) -0.031(4) 0.002(4) C13A 0.035(4) 0.077(6) 0.069(6) -0.027(5) -0.029(4) 0.005(4) C14A 0.036(4) 0.088(7) 0.051(5) -0.026(5) 0.000(3) -0.026(4) C15A 0.039(4) 0.050(4) 0.041(4) 0.002(3) -0.012(3) -0.020(3) C20A 0.028(3) 0.023(3) 0.029(3) 0.000(2) -0.015(2) -0.006(2) C21A 0.040(3) 0.021(3) 0.037(3) 0.002(2) -0.020(3) -0.008(2) C22A 0.053(4) 0.025(3) 0.045(4) 0.008(3) -0.023(3) -0.018(3) C23A 0.042(4) 0.046(4) 0.031(3) 0.011(3) -0.015(3) -0.021(3) C24A 0.043(4) 0.034(3) 0.031(3) -0.002(3) -0.016(3) -0.014(3) C25A 0.034(3) 0.024(3) 0.029(3) -0.001(2) -0.018(2) -0.007(2) P1B 0.0380(8) 0.0240(7) 0.0284(8) -0.0001(6) -0.0152(7) -0.0076(6) O1B 0.053(3) 0.035(2) 0.036(3) 0.007(2) -0.020(2) -0.018(2) O2B 0.047(3) 0.026(2) 0.036(2) 0.0011(18) -0.026(2) -0.0091(19) C30B 0.065(5) 0.041(4) 0.052(4) 0.014(3) -0.040(4) -0.020(4) C31B 0.099(7) 0.076(6) 0.055(5) 0.016(4) -0.051(5) -0.052(6) O3B 0.050(3) 0.032(2) 0.036(3) -0.008(2) -0.014(2) -0.004(2) C32B 0.114(10) 0.063(7) 0.070(7) -0.003(6) 0.028(7) 0.000(7) C33B 0.082(9) 0.159(15) 0.096(10) -0.041(10) 0.005(8) -0.005(9) C2B 0.034(3) 0.021(3) 0.032(3) -0.002(2) -0.018(3) -0.006(2) C3B 0.033(3) 0.018(2) 0.027(3) -0.005(2) -0.015(2) -0.004(2) C4B 0.028(3) 0.020(3) 0.035(3) 0.001(2) -0.012(2) -0.008(2) C5B 0.034(3) 0.021(3) 0.030(3) 0.005(2) -0.015(2) -0.007(2) C6B 0.030(3) 0.020(3) 0.031(3) -0.004(2) -0.013(2) -0.003(2) C7B 0.030(3) 0.024(3) 0.026(3) -0.003(2) -0.014(2) -0.002(2) C8B 0.035(3) 0.020(3) 0.027(3) 0.001(2) -0.017(2) -0.004(2) P2B 0.0266(7) 0.0256(7) 0.0278(8) 0.0004(6) -0.0134(6) -0.0030(6) C10B 0.032(3) 0.027(3) 0.030(3) 0.000(2) -0.012(3) -0.001(2) C11B 0.035(3) 0.031(3) 0.044(4) -0.004(3) -0.020(3) 0.000(3) C12B 0.059(5) 0.034(4) 0.066(5) -0.009(3) -0.034(4) -0.005(3) C13B 0.070(5) 0.027(3) 0.057(5) -0.008(3) -0.026(4) 0.002(3) C14B 0.042(4) 0.036(4) 0.063(5) -0.004(3) -0.018(4) 0.007(3) C15B 0.034(3) 0.036(4) 0.050(4) -0.005(3) -0.019(3) 0.003(3) C20B 0.030(3) 0.031(3) 0.031(3) 0.003(2) -0.012(3) -0.006(2) C21B 0.033(3) 0.034(3) 0.035(3) 0.003(3) -0.012(3) 0.001(3) C22B 0.043(4) 0.041(4) 0.037(4) 0.006(3) -0.007(3) -0.003(3) C23B 0.054(5) 0.057(5) 0.056(5) 0.002(4) 0.004(4) -0.021(4) C24B 0.058(5) 0.076(6) 0.061(6) -0.006(5) -0.007(4) -0.040(5) C25B 0.042(4) 0.057(5) 0.043(4) -0.004(3) -0.010(3) -0.021(4) C1C 0.034(3) 0.022(3) 0.028(3) 0.001(2) -0.017(2) -0.003(2) P1C 0.0360(8) 0.0216(7) 0.0335(8) -0.0015(6) -0.0186(7) -0.0041(6) O1C 0.037(2) 0.030(2) 0.041(3) -0.0084(19) -0.010(2) -0.0033(19) O2C 0.048(3) 0.024(2) 0.040(3) 0.0009(18) -0.021(2) -0.0070(19) C30C 0.068(5) 0.024(3) 0.094(7) 0.001(4) -0.052(5) -0.003(3) C31C 0.152(13) 0.035(5) 0.116(11) 0.023(6) -0.003(9) 0.007(6) O3C 0.048(3) 0.030(2) 0.044(3) -0.0053(19) -0.028(2) -0.007(2) C32C 0.063(5) 0.036(4) 0.058(5) -0.005(3) -0.039(4) -0.013(3) C33C 0.080(7) 0.060(6) 0.137(10) -0.016(6) -0.071(7) -0.025(5) C2C 0.037(3) 0.025(3) 0.032(3) 0.004(2) -0.021(3) -0.009(2) C3C 0.032(3) 0.025(3) 0.029(3) 0.000(2) -0.017(2) -0.007(2) C4C 0.033(3) 0.033(3) 0.026(3) 0.003(2) -0.014(2) -0.009(3) C5C 0.026(3) 0.028(3) 0.031(3) 0.002(2) -0.015(2) -0.004(2) C6C 0.030(3) 0.020(3) 0.027(3) -0.001(2) -0.015(2) -0.006(2) C7C 0.026(3) 0.028(3) 0.032(3) 0.002(2) -0.011(2) -0.003(2) C8C 0.027(3) 0.028(3) 0.033(3) -0.002(2) -0.013(2) -0.001(2) P2C 0.0264(7) 0.0203(6) 0.0247(7) -0.0002(5) -0.0127(6) -0.0044(5) C10C 0.031(3) 0.025(3) 0.028(3) -0.002(2) -0.009(2) -0.010(2) C11C 0.050(4) 0.029(3) 0.058(5) 0.006(3) -0.032(4) -0.012(3) C12C 0.071(5) 0.027(3) 0.072(6) 0.007(3) -0.039(5) -0.020(4) C13C 0.064(5) 0.047(4) 0.056(5) -0.003(4) -0.023(4) -0.032(4) C14C 0.057(5) 0.047(5) 0.134(10) 0.001(5) -0.055(6) -0.021(4) C15C 0.048(5) 0.038(4) 0.125(9) -0.007(5) -0.045(5) -0.012(4) C20C 0.027(3) 0.024(3) 0.025(3) 0.000(2) -0.014(2) -0.003(2) C21C 0.032(3) 0.023(3) 0.033(3) 0.000(2) -0.014(3) -0.004(2) C22C 0.039(3) 0.026(3) 0.035(3) -0.007(3) -0.016(3) -0.001(3) C23C 0.039(3) 0.038(3) 0.029(3) -0.006(3) -0.011(3) -0.005(3) C24C 0.039(3) 0.035(3) 0.033(3) 0.004(3) -0.008(3) -0.010(3) C25C 0.037(3) 0.023(3) 0.034(3) 0.000(2) -0.014(3) -0.006(2) P1D 0.0313(8) 0.0399(9) 0.0404(9) -0.0057(7) -0.0173(7) -0.0013(7) O1D 0.049(3) 0.049(3) 0.060(4) 0.003(3) -0.009(3) -0.011(3) O2D 0.038(3) 0.048(3) 0.041(3) -0.013(2) -0.016(2) 0.004(2) C30D 0.051(6) 0.138(12) 0.080(8) -0.042(8) -0.005(5) 0.000(7) C31D 0.20(2) 0.39(4) 0.23(2) -0.24(3) 0.136(19) -0.21(3) O3D 0.039(3) 0.063(4) 0.065(4) -0.008(3) -0.032(3) -0.001(3) C32D 0.054(6) 0.125(11) 0.122(10) -0.026(8) -0.044(7) -0.017(6) C33D 0.142(15) 0.29(3) 0.187(19) 0.065(18) -0.140(16) -0.085(17) C2D 0.047(4) 0.024(3) 0.032(3) 0.000(2) -0.024(3) -0.002(3) C3D 0.045(4) 0.023(3) 0.035(3) 0.004(2) -0.026(3) -0.003(3) C4D 0.036(3) 0.022(3) 0.030(3) 0.000(2) -0.013(3) -0.001(2) C5D 0.033(3) 0.026(3) 0.031(3) 0.003(2) -0.013(3) -0.004(2) C6D 0.032(3) 0.021(3) 0.030(3) -0.002(2) -0.015(2) 0.001(2) C7D 0.034(3) 0.028(3) 0.049(4) -0.007(3) -0.020(3) 0.002(3) C8D 0.034(3) 0.034(3) 0.052(4) -0.003(3) -0.026(3) -0.005(3) P2D 0.0290(7) 0.0209(7) 0.0274(7) -0.0006(6) -0.0128(6) -0.0026(6) C10D 0.035(3) 0.026(3) 0.027(3) -0.003(2) -0.010(2) -0.007(2) C11D 0.037(3) 0.041(4) 0.034(3) -0.003(3) -0.013(3) -0.013(3) C12D 0.036(4) 0.062(5) 0.041(4) -0.013(4) -0.007(3) -0.016(3) C13D 0.042(4) 0.071(6) 0.052(5) -0.021(4) 0.003(4) -0.031(4) C14D 0.058(5) 0.044(4) 0.054(5) -0.002(4) -0.003(4) -0.026(4) C15D 0.045(4) 0.032(3) 0.046(4) 0.000(3) -0.009(3) -0.011(3) C20D 0.036(3) 0.021(3) 0.030(3) -0.002(2) -0.017(3) -0.001(2) C21D 0.047(4) 0.028(3) 0.032(3) -0.002(3) -0.014(3) 0.000(3) C22D 0.071(5) 0.036(4) 0.037(4) 0.002(3) -0.032(4) -0.001(4) C23D 0.061(5) 0.041(4) 0.063(5) -0.003(4) -0.045(4) 0.003(4) C24D 0.039(4) 0.043(4) 0.054(5) -0.009(3) -0.026(3) 0.005(3) C25D 0.033(3) 0.039(3) 0.034(3) -0.005(3) -0.018(3) 0.000(3) C1E 0.149(11) 0.060(6) 0.062(6) 0.015(5) -0.064(7) -0.048(7) Cl1E 0.214(4) 0.0655(16) 0.0730(17) 0.0210(13) -0.087(2) -0.063(2) Cl2E 0.143(3) 0.0638(15) 0.0741(17) -0.0093(13) -0.0445(18) -0.0301(17) C1F 0.160(14) 0.123(11) 0.061(7) 0.008(7) -0.021(8) -0.088(11) Cl1F 0.088(3) 0.120(4) 0.341(9) -0.030(5) -0.024(4) 0.002(3) Cl2F 0.092(2) 0.152(4) 0.118(3) -0.035(3) 0.003(2) -0.056(2) C1G 0.106(11) 0.076(9) 0.166(16) 0.017(9) -0.012(11) -0.018(8) Cl1G 0.152(4) 0.085(2) 0.150(4) 0.050(3) -0.015(3) -0.019(2) Cl2G 0.373(13) 0.168(6) 0.262(9) 0.000(6) 0.168(9) -0.083(8) C1H 0.110(10) 0.080(8) 0.076(8) 0.013(6) -0.014(7) 0.014(7) Cl1H 0.108(4) 0.420(13) 0.184(6) 0.032(7) -0.018(4) -0.118(6) Cl2H 0.199(8) 0.164(6) 0.482(17) 0.022(8) -0.037(9) -0.082(6) C1I 0.096(10) 0.135(13) 0.141(13) -0.023(11) -0.066(10) -0.023(9) Cl1I 0.119(3) 0.113(3) 0.240(6) -0.027(3) -0.099(4) -0.014(3) Cl2I 0.081(3) 0.155(4) 0.453(12) -0.107(6) -0.108(5) -0.018(3) Cl1J 0.091(2) 0.110(3) 0.123(3) -0.015(2) -0.032(2) -0.001(2) Cl2J 0.115(3) 0.119(3) 0.153(4) -0.006(3) -0.025(3) -0.031(3) C1K 0.117(12) 0.092(10) 0.168(16) -0.046(10) -0.057(12) 0.004(9) Cl1K 0.114(3) 0.163(4) 0.197(5) 0.082(4) -0.063(3) -0.015(3) Cl2K 0.179(6) 0.125(5) 0.515(16) -0.098(7) 0.158(8) -0.047(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 P2A 2.2469(14) . ? Pt1 P2C 2.2661(15) . ? Pt1 Cl2 2.3401(16) . ? Pt1 Cl1 2.3648(15) . ? Pt2 P2D 2.3069(15) . ? Pt2 P2B 2.3091(15) . ? Pt2 Cl4 2.3148(16) . ? Pt2 Cl3 2.3286(15) . ? C1 C2A 1.562(8) . ? C1 C2B 1.581(8) . ? C1 P1B 1.833(6) . ? C1 P1A 1.837(6) . ? P1A O1A 1.449(5) . ? P1A O2A 1.546(6) . ? P1A O3A 1.552(5) . ? O2A C30A 1.430(12) . ? C30A C31A 1.482(5) . ? C30A H30O 0.9700 . ? C30A H30P 0.9700 . ? C31A H31O 0.9600 . ? C31A H31P 0.9600 . ? C31A H31Q 0.9600 . ? O3A C32A 1.443(9) . ? C32A C33A 1.483(5) . ? C32A H32O 0.9700 . ? C32A H32P 0.9700 . ? C33A H33O 0.9600 . ? C33A H33P 0.9600 . ? C33A H33Q 0.9600 . ? C2A C3A 1.511(8) . ? C2A H2A1 0.9700 . ? C2A H2A2 0.9700 . ? C3A C4A 1.384(8) . ? C3A C8A 1.405(8) . ? C4A C5A 1.397(8) . ? C4A H4A 0.9300 . ? C5A C6A 1.395(8) . ? C5A H5A 0.9300 . ? C6A C7A 1.398(8) . ? C6A P2A 1.816(6) . ? C7A C8A 1.383(8) . ? C7A H7A 0.9300 . ? C8A H8A 0.9300 . ? P2A C10A 1.830(6) . ? P2A C20A 1.829(6) . ? C10A C15A 1.367(10) . ? C10A C11A 1.391(9) . ? C11A C12A 1.403(10) . ? C11A H11A 0.9300 . ? C12A C13A 1.355(14) . ? C12A H12A 0.9300 . ? C13A C14A 1.396(14) . ? C13A H13A 0.9300 . ? C14A C15A 1.405(11) . ? C14A H14A 0.9300 . ? C15A H15A 0.9300 . ? C20A C25A 1.386(8) . ? C20A C21A 1.398(8) . ? C21A C22A 1.371(9) . ? C21A H21A 0.9300 . ? C22A C23A 1.388(10) . ? C22A H22A 0.9300 . ? C23A C24A 1.374(9) . ? C23A H23A 0.9300 . ? C24A C25A 1.397(9) . ? C24A H24A 0.9300 . ? C25A H25A 0.9300 . ? P1B O1B 1.472(5) . ? P1B O3B 1.568(5) . ? P1B O2B 1.573(5) . ? O2B C30B 1.460(8) . ? C30B C31B 1.487(11) . ? C30B H30R 0.9700 . ? C30B H30S 0.9700 . ? C31B H31R 0.9600 . ? C31B H31S 0.9600 . ? C31B H31T 0.9600 . ? O3B C32B 1.411(11) . ? C32B C33B 1.483(5) . ? C32B H32R 0.9700 . ? C32B H32S 0.9700 . ? C33B H33R 0.9600 . ? C33B H33S 0.9600 . ? C33B H33T 0.9600 . ? C2B C3B 1.518(8) . ? C2B H2B1 0.9700 . ? C2B H2B2 0.9700 . ? C3B C8B 1.382(9) . ? C3B C4B 1.397(8) . ? C4B C5B 1.388(8) . ? C4B H4B 0.9300 . ? C5B C6B 1.396(9) . ? C5B H5B 0.9300 . ? C6B C7B 1.402(8) . ? C6B P2B 1.826(6) . ? C7B C8B 1.383(8) . ? C7B H7B 0.9300 . ? C8B H8B 0.9300 . ? P2B C10B 1.820(6) . ? P2B C20B 1.828(7) . ? C10B C11B 1.372(9) . ? C10B C15B 1.403(9) . ? C11B C12B 1.393(10) . ? C11B H11B 0.9300 . ? C12B C13B 1.372(11) . ? C12B H12B 0.9300 . ? C13B C14B 1.372(12) . ? C13B H13B 0.9300 . ? C14B C15B 1.378(10) . ? C14B H14B 0.9300 . ? C15B H15B 0.9300 . ? C20B C25B 1.380(10) . ? C20B C21B 1.401(9) . ? C21B C22B 1.377(10) . ? C21B H21B 0.9300 . ? C22B C23B 1.368(13) . ? C22B H22B 0.9300 . ? C23B C24B 1.383(13) . ? C23B H23B 0.9300 . ? C24B C25B 1.402(11) . ? C24B H24B 0.9300 . ? C25B H25B 0.9300 . ? C1C C2C 1.572(8) . ? C1C C2D 1.576(8) . ? C1C P1C 1.837(6) . ? C1C P1D 1.841(7) . ? P1C O1C 1.464(5) . ? P1C O2C 1.567(5) . ? P1C O3C 1.582(5) . ? O2C C30C 1.465(9) . ? C30C C31C 1.481(5) . ? C30C H30U 0.9700 . ? C30C H30V 0.9700 . ? C31C H31U 0.9600 . ? C31C H31V 0.9600 . ? C31C H31W 0.9600 . ? O3C C32C 1.452(8) . ? C32C C33C 1.486(12) . ? C32C H32U 0.9700 . ? C32C H32V 0.9700 . ? C33C H33U 0.9600 . ? C33C H33V 0.9600 . ? C33C H33W 0.9600 . ? C2C C3C 1.514(8) . ? C2C H2C1 0.9700 . ? C2C H2C2 0.9700 . ? C3C C8C 1.395(9) . ? C3C C4C 1.395(8) . ? C4C C5C 1.387(8) . ? C4C H4C 0.9300 . ? C5C C6C 1.393(8) . ? C5C H5C 0.9300 . ? C6C C7C 1.402(8) . ? C6C P2C 1.821(6) . ? C7C C8C 1.382(8) . ? C7C H7C 0.9300 . ? C8C H8C 0.9300 . ? P2C C10C 1.826(6) . ? P2C C20C 1.838(6) . ? C10C C11C 1.375(9) . ? C10C C15C 1.382(10) . ? C11C C12C 1.390(10) . ? C11C H11C 0.9300 . ? C12C C13C 1.361(12) . ? C12C H12C 0.9300 . ? C13C C14C 1.359(12) . ? C13C H13C 0.9300 . ? C14C C15C 1.369(11) . ? C14C H14C 0.9300 . ? C15C H15C 0.9300 . ? C20C C25C 1.394(9) . ? C20C C21C 1.393(8) . ? C21C C22C 1.390(9) . ? C21C H21C 0.9300 . ? C22C C23C 1.384(10) . ? C22C H22C 0.9300 . ? C23C C24C 1.391(10) . ? C23C H23C 0.9300 . ? C24C C25C 1.389(9) . ? C24C H24C 0.9300 . ? C25C H25C 0.9300 . ? P1D O1D 1.484(6) . ? P1D O3D 1.559(5) . ? P1D O2D 1.566(5) . ? O2D C30D 1.464(11) . ? C30D C31D 1.474(5) . ? C30D H30X 0.9700 . ? C30D H30Y 0.9700 . ? C31D H31X 0.9600 . ? C31D H31Y 0.9600 . ? C31D H31Z 0.9600 . ? O3D C32D 1.435(12) . ? C32D C33D 1.48(2) . ? C32D H32X 0.9700 . ? C32D H32Y 0.9700 . ? C33D H33X 0.9600 . ? C33D H33Y 0.9600 . ? C33D H33Z 0.9600 . ? C2D C3D 1.516(9) . ? C2D H2D1 0.9700 . ? C2D H2D2 0.9700 . ? C3D C4D 1.388(9) . ? C3D C8D 1.406(9) . ? C4D C5D 1.384(9) . ? C4D H4D 0.9300 . ? C5D C6D 1.400(8) . ? C5D H5D 0.9300 . ? C6D C7D 1.393(9) . ? C6D P2D 1.817(6) . ? C7D C8D 1.372(9) . ? C7D H7D 0.9300 . ? C8D H8D 0.9300 . ? P2D C20D 1.819(6) . ? P2D C10D 1.821(7) . ? C10D C11D 1.385(9) . ? C10D C15D 1.390(9) . ? C11D C12D 1.378(10) . ? C11D H11D 0.9300 . ? C12D C13D 1.383(12) . ? C12D H12D 0.9300 . ? C13D C14D 1.370(13) . ? C13D H13D 0.9300 . ? C14D C15D 1.395(11) . ? C14D H14D 0.9300 . ? C15D H15D 0.9300 . ? C20D C21D 1.397(9) . ? C20D C25D 1.399(9) . ? C21D C22D 1.373(9) . ? C21D H21D 0.9300 . ? C22D C23D 1.396(12) . ? C22D H22D 0.9300 . ? C23D C24D 1.372(11) . ? C23D H23D 0.9300 . ? C24D C25D 1.398(9) . ? C24D H24D 0.9300 . ? C25D H25D 0.9300 . ? C1E Cl2E 1.708(10) . ? C1E Cl1E 1.746(10) . ? C1E H1E 0.9700 . ? C1E H2E 0.9700 . ? C1F Cl2F 1.629(15) . ? C1F Cl1F 1.772(16) . ? C1F H1F 0.9700 . ? C1F H2F 0.9700 . ? C1G Cl2G 1.682(15) . ? C1G Cl1G 1.704(16) . ? C1G H1G 0.9700 . ? C1G H2G 0.9700 . ? C1H Cl1H 1.660(15) . ? C1H Cl2H 2.005(17) . ? C1H H1H 0.9700 . ? C1H H2H 0.9700 . ? C1I Cl2I 1.777(18) . ? C1I Cl1I 1.826(15) . ? C1I H1I 0.9700 . ? C1I H2I 0.9700 . ? C1J Cl1J 1.831(18) . ? C1J Cl2J 1.787(18) . ? C1J H1J 0.9700 . ? C1J H2J 0.9700 . ? C1K Cl2K 1.686(19) . ? C1K Cl1K 1.703(16) . ? C1K H1K 0.9700 . ? C1K H2K 0.9700 . ? 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 P2A Pt1 P2C 96.95(5) . . ? P2A Pt1 Cl2 91.24(6) . . ? P2C Pt1 Cl2 170.56(6) . . ? P2A Pt1 Cl1 176.13(6) . . ? P2C Pt1 Cl1 85.97(5) . . ? Cl2 Pt1 Cl1 86.07(6) . . ? P2D Pt2 P2B 168.64(5) . . ? P2D Pt2 Cl4 90.69(5) . . ? P2B Pt2 Cl4 88.08(6) . . ? P2D Pt2 Cl3 87.16(5) . . ? P2B Pt2 Cl3 93.20(5) . . ? Cl4 Pt2 Cl3 175.28(6) . . ? C2A C1 C2B 107.5(5) . . ? C2A C1 P1B 115.3(4) . . ? C2B C1 P1B 107.2(4) . . ? C2A C1 P1A 110.5(4) . . ? C2B C1 P1A 102.8(4) . . ? P1B C1 P1A 112.4(3) . . ? O1A P1A O2A 115.5(3) . . ? O1A P1A O3A 115.8(3) . . ? O2A P1A O3A 101.1(3) . . ? O1A P1A C1 112.0(3) . . ? O2A P1A C1 106.2(3) . . ? O3A P1A C1 105.0(3) . . ? C30A O2A P1A 125.7(6) . . ? O2A C30A C31A 116.0(11) . . ? O2A C30A H30O 108.3 . . ? C31A C30A H30O 108.3 . . ? O2A C30A H30P 108.3 . . ? C31A C30A H30P 108.3 . . ? H30O C30A H30P 107.4 . . ? C30A C31A H31O 109.5 . . ? C30A C31A H31P 109.5 . . ? H31O C31A H31P 109.5 . . ? C30A C31A H31Q 109.5 . . ? H31O C31A H31Q 109.5 . . ? H31P C31A H31Q 109.5 . . ? C32A O3A P1A 123.5(6) . . ? O3A C32A C33A 112.1(8) . . ? O3A C32A H32O 109.2 . . ? C33A C32A H32O 109.2 . . ? O3A C32A H32P 109.2 . . ? C33A C32A H32P 109.2 . . ? H32O C32A H32P 107.9 . . ? C32A C33A H33O 109.5 . . ? C32A C33A H33P 109.5 . . ? H33O C33A H33P 109.5 . . ? C32A C33A H33Q 109.5 . . ? H33O C33A H33Q 109.5 . . ? H33P C33A H33Q 109.5 . . ? C3A C2A C1 120.8(5) . . ? C3A C2A H2A1 107.1 . . ? C1 C2A H2A1 107.1 . . ? C3A C2A H2A2 107.1 . . ? C1 C2A H2A2 107.1 . . ? H2A1 C2A H2A2 106.8 . . ? C4A C3A C8A 118.1(5) . . ? C4A C3A C2A 122.4(5) . . ? C8A C3A C2A 119.3(5) . . ? C3A C4A C5A 121.5(5) . . ? C3A C4A H4A 119.3 . . ? C5A C4A H4A 119.3 . . ? C4A C5A C6A 120.1(5) . . ? C4A C5A H5A 120.0 . . ? C6A C5A H5A 120.0 . . ? C5A C6A C7A 118.6(5) . . ? C5A C6A P2A 121.1(4) . . ? C7A C6A P2A 120.2(4) . . ? C8A C7A C6A 120.8(5) . . ? C8A C7A H7A 119.6 . . ? C6A C7A H7A 119.6 . . ? C7A C8A C3A 120.8(5) . . ? C7A C8A H8A 119.6 . . ? C3A C8A H8A 119.6 . . ? C6A P2A C10A 100.2(3) . . ? C6A P2A C20A 108.5(3) . . ? C10A P2A C20A 103.0(3) . . ? C6A P2A Pt1 115.26(19) . . ? C10A P2A Pt1 116.8(2) . . ? C20A P2A Pt1 111.81(19) . . ? C15A C10A C11A 119.9(6) . . ? C15A C10A P2A 118.0(5) . . ? C11A C10A P2A 122.1(5) . . ? C10A C11A C12A 119.0(7) . . ? C10A C11A H11A 120.5 . . ? C12A C11A H11A 120.5 . . ? C13A C12A C11A 121.3(8) . . ? C13A C12A H12A 119.3 . . ? C11A C12A H12A 119.3 . . ? C12A C13A C14A 120.0(7) . . ? C12A C13A H13A 120.0 . . ? C14A C13A H13A 120.0 . . ? C13A C14A C15A 118.9(8) . . ? C13A C14A H14A 120.5 . . ? C15A C14A H14A 120.5 . . ? C10A C15A C14A 120.9(7) . . ? C10A C15A H15A 119.6 . . ? C14A C15A H15A 119.6 . . ? C25A C20A C21A 119.6(6) . . ? C25A C20A P2A 124.5(4) . . ? C21A C20A P2A 115.9(5) . . ? C22A C21A C20A 120.0(6) . . ? C22A C21A H21A 120.0 . . ? C20A C21A H21A 120.0 . . ? C21A C22A C23A 120.5(6) . . ? C21A C22A H22A 119.7 . . ? C23A C22A H22A 119.7 . . ? C24A C23A C22A 120.0(6) . . ? C24A C23A H23A 120.0 . . ? C22A C23A H23A 120.0 . . ? C23A C24A C25A 120.2(6) . . ? C23A C24A H24A 119.9 . . ? C25A C24A H24A 119.9 . . ? C20A C25A C24A 119.7(6) . . ? C20A C25A H25A 120.1 . . ? C24A C25A H25A 120.1 . . ? O1B P1B O3B 114.3(3) . . ? O1B P1B O2B 115.2(3) . . ? O3B P1B O2B 105.3(3) . . ? O1B P1B C1 114.3(3) . . ? O3B P1B C1 106.3(3) . . ? O2B P1B C1 100.1(3) . . ? C30B O2B P1B 121.8(5) . . ? O2B C30B C31B 110.3(6) . . ? O2B C30B H30R 109.6 . . ? C31B C30B H30R 109.6 . . ? O2B C30B H30S 109.6 . . ? C31B C30B H30S 109.6 . . ? H30R C30B H30S 108.1 . . ? C30B C31B H31R 109.5 . . ? C30B C31B H31S 109.5 . . ? H31R C31B H31S 109.5 . . ? C30B C31B H31T 109.5 . . ? H31R C31B H31T 109.5 . . ? H31S C31B H31T 109.5 . . ? C32B O3B P1B 123.1(6) . . ? O3B C32B C33B 113.6(9) . . ? O3B C32B H32R 108.8 . . ? C33B C32B H32R 108.8 . . ? O3B C32B H32S 108.8 . . ? C33B C32B H32S 108.8 . . ? H32R C32B H32S 107.7 . . ? C32B C33B H33R 109.5 . . ? C32B C33B H33S 109.5 . . ? H33R C33B H33S 109.5 . . ? C32B C33B H33T 109.5 . . ? H33R C33B H33T 109.5 . . ? H33S C33B H33T 109.5 . . ? C3B C2B C1 117.4(5) . . ? C3B C2B H2B1 108.0 . . ? C1 C2B H2B1 108.0 . . ? C3B C2B H2B2 108.0 . . ? C1 C2B H2B2 108.0 . . ? H2B1 C2B H2B2 107.2 . . ? C8B C3B C4B 118.1(5) . . ? C8B C3B C2B 121.3(5) . . ? C4B C3B C2B 120.5(5) . . ? C5B C4B C3B 120.6(6) . . ? C5B C4B H4B 119.7 . . ? C3B C4B H4B 119.7 . . ? C4B C5B C6B 120.9(5) . . ? C4B C5B H5B 119.5 . . ? C6B C5B H5B 119.5 . . ? C5B C6B C7B 118.3(5) . . ? C5B C6B P2B 117.8(4) . . ? C7B C6B P2B 123.9(5) . . ? C8B C7B C6B 120.0(6) . . ? C8B C7B H7B 120.0 . . ? C6B C7B H7B 120.0 . . ? C3B C8B C7B 122.0(5) . . ? C3B C8B H8B 119.0 . . ? C7B C8B H8B 119.0 . . ? C10B P2B C6B 105.5(3) . . ? C10B P2B C20B 102.4(3) . . ? C6B P2B C20B 106.0(3) . . ? C10B P2B Pt2 115.8(2) . . ? C6B P2B Pt2 106.9(2) . . ? C20B P2B Pt2 119.1(2) . . ? C11B C10B C15B 118.3(6) . . ? C11B C10B P2B 124.1(5) . . ? C15B C10B P2B 117.6(5) . . ? C10B C11B C12B 120.5(6) . . ? C10B C11B H11B 119.8 . . ? C12B C11B H11B 119.8 . . ? C13B C12B C11B 120.5(7) . . ? C13B C12B H12B 119.7 . . ? C11B C12B H12B 119.7 . . ? C14B C13B C12B 119.7(7) . . ? C14B C13B H13B 120.1 . . ? C12B C13B H13B 120.1 . . ? C13B C14B C15B 120.1(7) . . ? C13B C14B H14B 119.9 . . ? C15B C14B H14B 119.9 . . ? C14B C15B C10B 120.8(7) . . ? C14B C15B H15B 119.6 . . ? C10B C15B H15B 119.6 . . ? C25B C20B C21B 119.6(6) . . ? C25B C20B P2B 120.8(5) . . ? C21B C20B P2B 119.6(5) . . ? C22B C21B C20B 120.2(7) . . ? C22B C21B H21B 119.9 . . ? C20B C21B H21B 119.9 . . ? C23B C22B C21B 120.4(8) . . ? C23B C22B H22B 119.8 . . ? C21B C22B H22B 119.8 . . ? C22B C23B C24B 120.1(8) . . ? C22B C23B H23B 120.0 . . ? C24B C23B H23B 120.0 . . ? C23B C24B C25B 120.3(8) . . ? C23B C24B H24B 119.8 . . ? C25B C24B H24B 119.8 . . ? C20B C25B C24B 119.3(7) . . ? C20B C25B H25B 120.4 . . ? C24B C25B H25B 120.4 . . ? C2C C1C C2D 107.4(5) . . ? C2C C1C P1C 109.2(4) . . ? C2D C1C P1C 103.9(4) . . ? C2C C1C P1D 112.7(4) . . ? C2D C1C P1D 111.4(4) . . ? P1C C1C P1D 111.8(3) . . ? O1C P1C O2C 113.8(3) . . ? O1C P1C O3C 116.0(3) . . ? O2C P1C O3C 104.7(3) . . ? O1C P1C C1C 112.0(3) . . ? O2C P1C C1C 108.9(3) . . ? O3C P1C C1C 100.3(3) . . ? C30C O2C P1C 120.0(5) . . ? O2C C30C C31C 108.7(8) . . ? O2C C30C H30U 109.9 . . ? C31C C30C H30U 109.9 . . ? O2C C30C H30V 109.9 . . ? C31C C30C H30V 109.9 . . ? H30U C30C H30V 108.3 . . ? C30C C31C H31U 109.5 . . ? C30C C31C H31V 109.5 . . ? H31U C31C H31V 109.5 . . ? C30C C31C H31W 109.5 . . ? H31U C31C H31W 109.5 . . ? H31V C31C H31W 109.5 . . ? C32C O3C P1C 120.2(4) . . ? O3C C32C C33C 108.8(7) . . ? O3C C32C H32U 109.9 . . ? C33C C32C H32U 109.9 . . ? O3C C32C H32V 109.9 . . ? C33C C32C H32V 109.9 . . ? H32U C32C H32V 108.3 . . ? C32C C33C H33U 109.5 . . ? C32C C33C H33V 109.5 . . ? H33U C33C H33V 109.5 . . ? C32C C33C H33W 109.5 . . ? H33U C33C H33W 109.5 . . ? H33V C33C H33W 109.5 . . ? C3C C2C C1C 120.0(5) . . ? C3C C2C H2C1 107.3 . . ? C1C C2C H2C1 107.3 . . ? C3C C2C H2C2 107.3 . . ? C1C C2C H2C2 107.3 . . ? H2C1 C2C H2C2 106.9 . . ? C8C C3C C4C 117.7(5) . . ? C8C C3C C2C 123.1(5) . . ? C4C C3C C2C 119.1(6) . . ? C5C C4C C3C 121.6(6) . . ? C5C C4C H4C 119.2 . . ? C3C C4C H4C 119.2 . . ? C4C C5C C6C 120.3(5) . . ? C4C C5C H5C 119.8 . . ? C6C C5C H5C 119.8 . . ? C5C C6C C7C 118.5(5) . . ? C5C C6C P2C 120.6(4) . . ? C7C C6C P2C 120.9(5) . . ? C8C C7C C6C 120.6(6) . . ? C8C C7C H7C 119.7 . . ? C6C C7C H7C 119.7 . . ? C7C C8C C3C 121.3(6) . . ? C7C C8C H8C 119.3 . . ? C3C C8C H8C 119.3 . . ? C6C P2C C10C 107.2(3) . . ? C6C P2C C20C 101.9(3) . . ? C10C P2C C20C 101.9(3) . . ? C6C P2C Pt1 112.6(2) . . ? C10C P2C Pt1 108.5(2) . . ? C20C P2C Pt1 123.25(18) . . ? C11C C10C C15C 117.5(6) . . ? C11C C10C P2C 120.0(5) . . ? C15C C10C P2C 122.5(5) . . ? C10C C11C C12C 120.1(7) . . ? C10C C11C H11C 119.9 . . ? C12C C11C H11C 119.9 . . ? C13C C12C C11C 121.2(7) . . ? C13C C12C H12C 119.4 . . ? C11C C12C H12C 119.4 . . ? C12C C13C C14C 118.9(7) . . ? C12C C13C H13C 120.5 . . ? C14C C13C H13C 120.5 . . ? C13C C14C C15C 120.4(8) . . ? C13C C14C H14C 119.8 . . ? C15C C14C H14C 119.8 . . ? C14C C15C C10C 121.8(8) . . ? C14C C15C H15C 119.1 . . ? C10C C15C H15C 119.1 . . ? C25C C20C C21C 118.7(5) . . ? C25C C20C P2C 120.6(4) . . ? C21C C20C P2C 120.7(5) . . ? C22C C21C C20C 120.9(6) . . ? C22C C21C H21C 119.6 . . ? C20C C21C H21C 119.6 . . ? C23C C22C C21C 119.8(6) . . ? C23C C22C H22C 120.1 . . ? C21C C22C H22C 120.1 . . ? C22C C23C C24C 120.0(6) . . ? C22C C23C H23C 120.0 . . ? C24C C23C H23C 120.0 . . ? C25C C24C C23C 119.9(6) . . ? C25C C24C H24C 120.0 . . ? C23C C24C H24C 120.0 . . ? C24C C25C C20C 120.7(6) . . ? C24C C25C H25C 119.7 . . ? C20C C25C H25C 119.7 . . ? O1D P1D O3D 112.9(3) . . ? O1D P1D O2D 113.9(3) . . ? O3D P1D O2D 105.1(3) . . ? O1D P1D C1C 115.4(3) . . ? O3D P1D C1C 107.6(3) . . ? O2D P1D C1C 100.8(3) . . ? C30D O2D P1D 116.0(6) . . ? O2D C30D C31D 110.9(10) . . ? O2D C30D H30X 109.5 . . ? C31D C30D H30X 109.4 . . ? O2D C30D H30Y 109.5 . . ? C31D C30D H30Y 109.5 . . ? H30X C30D H30Y 108.0 . . ? C30D C31D H31X 109.5 . . ? C30D C31D H31Y 109.5 . . ? H31X C31D H31Y 109.5 . . ? C30D C31D H31Z 109.5 . . ? H31X C31D H31Z 109.5 . . ? H31Y C31D H31Z 109.5 . . ? C32D O3D P1D 125.0(7) . . ? O3D C32D C33D 106.7(12) . . ? O3D C32D H32X 110.4 . . ? C33D C32D H32X 110.4 . . ? O3D C32D H32Y 110.4 . . ? C33D C32D H32Y 110.4 . . ? H32X C32D H32Y 108.6 . . ? C32D C33D H33X 109.5 . . ? C32D C33D H33Y 109.5 . . ? H33X C33D H33Y 109.5 . . ? C32D C33D H33Z 109.5 . . ? H33X C33D H33Z 109.5 . . ? H33Y C33D H33Z 109.5 . . ? C3D C2D C1C 116.7(5) . . ? C3D C2D H2D1 108.1 . . ? C1C C2D H2D1 108.1 . . ? C3D C2D H2D2 108.1 . . ? C1C C2D H2D2 108.1 . . ? H2D1 C2D H2D2 107.3 . . ? C4D C3D C8D 117.8(6) . . ? C4D C3D C2D 120.6(6) . . ? C8D C3D C2D 121.6(6) . . ? C5D C4D C3D 122.0(6) . . ? C5D C4D H4D 119.0 . . ? C3D C4D H4D 119.0 . . ? C4D C5D C6D 119.8(6) . . ? C4D C5D H5D 120.1 . . ? C6D C5D H5D 120.1 . . ? C7D C6D C5D 118.4(6) . . ? C7D C6D P2D 117.1(5) . . ? C5D C6D P2D 124.3(5) . . ? C8D C7D C6D 121.5(6) . . ? C8D C7D H7D 119.2 . . ? C6D C7D H7D 119.2 . . ? C7D C8D C3D 120.5(6) . . ? C7D C8D H8D 119.8 . . ? C3D C8D H8D 119.8 . . ? C6D P2D C20D 101.7(3) . . ? C6D P2D C10D 109.5(3) . . ? C20D P2D C10D 109.3(3) . . ? C6D P2D Pt2 115.2(2) . . ? C20D P2D Pt2 119.4(2) . . ? C10D P2D Pt2 101.6(2) . . ? C11D C10D C15D 118.4(6) . . ? C11D C10D P2D 118.3(5) . . ? C15D C10D P2D 122.0(5) . . ? C12D C11D C10D 121.7(7) . . ? C12D C11D H11D 119.1 . . ? C10D C11D H11D 119.1 . . ? C11D C12D C13D 119.4(8) . . ? C11D C12D H12D 120.3 . . ? C13D C12D H12D 120.3 . . ? C14D C13D C12D 120.0(7) . . ? C14D C13D H13D 120.0 . . ? C12D C13D H13D 120.0 . . ? C13D C14D C15D 120.7(7) . . ? C13D C14D H14D 119.7 . . ? C15D C14D H14D 119.7 . . ? C10D C15D C14D 119.8(7) . . ? C10D C15D H15D 120.1 . . ? C14D C15D H15D 120.1 . . ? C21D C20D C25D 119.6(6) . . ? C21D C20D P2D 120.3(5) . . ? C25D C20D P2D 119.7(5) . . ? C22D C21D C20D 120.4(7) . . ? C22D C21D H21D 119.8 . . ? C20D C21D H21D 119.8 . . ? C21D C22D C23D 119.8(7) . . ? C21D C22D H22D 120.1 . . ? C23D C22D H22D 120.1 . . ? C24D C23D C22D 120.5(6) . . ? C24D C23D H23D 119.8 . . ? C22D C23D H23D 119.8 . . ? C23D C24D C25D 120.3(7) . . ? C23D C24D H24D 119.9 . . ? C25D C24D H24D 119.9 . . ? C20D C25D C24D 119.3(6) . . ? C20D C25D H25D 120.3 . . ? C24D C25D H25D 120.3 . . ? Cl2E C1E Cl1E 112.7(5) . . ? Cl2E C1E H1E 109.1 . . ? Cl1E C1E H1E 109.1 . . ? Cl2E C1E H2E 109.1 . . ? Cl1E C1E H2E 109.1 . . ? H1E C1E H2E 107.8 . . ? Cl2F C1F Cl1F 113.7(8) . . ? Cl2F C1F H1F 108.8 . . ? Cl1F C1F H1F 108.8 . . ? Cl2F C1F H2F 108.8 . . ? Cl1F C1F H2F 108.8 . . ? H1F C1F H2F 107.7 . . ? Cl2G C1G Cl1G 111.9(9) . . ? Cl2G C1G H1G 109.2 . . ? Cl1G C1G H1G 109.2 . . ? Cl2G C1G H2G 109.2 . . ? Cl1G C1G H2G 109.2 . . ? H1G C1G H2G 107.9 . . ? Cl1H C1H Cl2H 106.1(8) . . ? Cl1H C1H H1H 110.5 . . ? Cl2H C1H H1H 110.5 . . ? Cl1H C1H H2H 110.5 . . ? Cl2H C1H H2H 110.5 . . ? H1H C1H H2H 108.7 . . ? Cl2I C1I Cl1I 102.9(9) . . ? Cl2I C1I H1I 111.2 . . ? Cl1I C1I H1I 111.2 . . ? Cl2I C1I H2I 111.2 . . ? Cl1I C1I H2I 111.2 . . ? H1I C1I H2I 109.1 . . ? Cl1J C1J Cl2J 113.4(10) . . ? Cl1J C1J H1J 108.9 . . ? Cl2J C1J H1J 108.9 . . ? Cl1J C1J H2J 108.9 . . ? Cl2J C1J H2J 108.9 . . ? H1J C1J H2J 107.7 . . ? Cl2K C1K Cl1K 115.2(12) . . ? Cl2K C1K H1K 108.5 . . ? Cl1K C1K H1K 108.5 . . ? Cl2K C1K H2K 108.5 . . ? Cl1K C1K H2K 108.5 . . ? H1K C1K H2K 107.5 . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 27.58 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 4.237 _refine_diff_density_min -1.945 _refine_diff_density_rms 0.160 _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla, M.C., Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, p. 435. Coppens, P. (1970). Crystallographic Computing, edited by F.R. Ahmed, S.R.Hall & C.P. Huber, pp. 255-270, Copenhagen, Munksgaard. Hooft, R.W. (1998). COLLECT. Nonius BV, Delft, The Netherlands. Otwinowski, Z. & Minor, W. (1997). Methods Enzymol. 276, 307--326. Sheldrick, G. M. (1997). SHELXL97. University of G\"ottingen, Germany. Spek, A.L. (1999). PLATON. Version 1999. Utrecht University, The Netherlands. ;