Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2003 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 loop_ _publ_author_name 'Paul David Newman' 'K.M. Abdul Malik' _publ_contact_author_name 'Dr Paul David Newman' _publ_contact_author_address ; Department of Chemistry Cardiff University PO Box 912 Park Place Cardiff CF10 3TB UNITED KINGDOM ; _publ_contact_author_email NEWMANP1@CARDIFF.AC.UK _publ_section_title ; Ligand ambivalence in pallada(platina)cyclic complexes of a rigid phosphine ; data_phenop_ligand _database_code_CSD 213238 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H37 O P' _chemical_formula_weight 396.53 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' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 7.57200(10) _cell_length_b 10.3049(2) _cell_length_c 28.3367(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2211.08(7) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 'all observed reflections in the data set' _cell_measurement_theta_min 2.93 _cell_measurement_theta_max 27.5 _exptl_crystal_description bloc _exptl_crystal_colour colorless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.191 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 864 _exptl_absorpt_coefficient_mu 0.138 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.850 _exptl_absorpt_correction_T_max 0.980 _exptl_absorpt_process_details 'SORTAV (Blessing, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Nonius kappa CCD area detector' _diffrn_measurement_method 'phi & omega scan to fill Ewald sphere' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14316 _diffrn_reflns_av_R_equivalents 0.0560 _diffrn_reflns_av_sigmaI/netI 0.0590 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 2.93 _diffrn_reflns_theta_max 27.50 _reflns_number_total 4712 _reflns_number_gt 3971 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Hooft, 1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-96 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 for Windows (Farrugia, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0517P)^2^+0.5873P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment 'calculated positions, riding model' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.05(10) _refine_ls_number_reflns 4712 _refine_ls_number_parameters 259 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0620 _refine_ls_R_factor_gt 0.0446 _refine_ls_wR_factor_ref 0.1113 _refine_ls_wR_factor_gt 0.1011 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.055 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group P1 P 0.20988(8) 0.38153(5) 0.381960(19) 0.01925(14) Uani 1 1 d . . . O1 O -0.1595(2) 0.32690(13) 0.40268(5) 0.0201(4) Uani 1 1 d . . . C1 C 0.0700(3) 0.2858(2) 0.34017(7) 0.0194(5) Uani 1 1 d . . . H1 H 0.0735 0.3287 0.3085 0.023 Uiso 1 1 calc R . . C2 C 0.1185(3) 0.1407(2) 0.33404(8) 0.0217(5) Uani 1 1 d . . . H2 H 0.2252 0.1253 0.3140 0.026 Uiso 1 1 calc R . . C3 C 0.1272(3) 0.0763(2) 0.38295(8) 0.0257(5) Uani 1 1 d . . . H3A H 0.1966 0.1297 0.4053 0.031 Uiso 1 1 calc R . . H3B H 0.1802 -0.0113 0.3810 0.031 Uiso 1 1 calc R . . C4 C -0.0690(3) 0.0691(2) 0.39796(8) 0.0246(5) Uani 1 1 d . . . H4A H -0.1060 -0.0219 0.4030 0.029 Uiso 1 1 calc R . . H4B H -0.0896 0.1190 0.4273 0.029 Uiso 1 1 calc R . . C5 C -0.1690(3) 0.1297(2) 0.35630(7) 0.0212(5) Uani 1 1 d . . . C6 C -0.1277(3) 0.27601(19) 0.35663(7) 0.0174(5) Uani 1 1 d . . . H6 H -0.2053 0.3213 0.3333 0.021 Uiso 1 1 calc R . . C7 C -0.0550(3) 0.0835(2) 0.31320(8) 0.0234(5) Uani 1 1 d . . . C8 C -0.1116(3) 0.1412(2) 0.26537(8) 0.0281(6) Uani 1 1 d . . . H8A H -0.1259 0.2353 0.2685 0.042 Uiso 1 1 calc R . . H8B H -0.2239 0.1024 0.2556 0.042 Uiso 1 1 calc R . . H8C H -0.0210 0.1225 0.2416 0.042 Uiso 1 1 calc R . . C9 C -0.0504(4) -0.0637(2) 0.30667(9) 0.0314(6) Uani 1 1 d . . . H9A H 0.0396 -0.0862 0.2832 0.047 Uiso 1 1 calc R . . H9B H -0.1662 -0.0939 0.2958 0.047 Uiso 1 1 calc R . . H9C H -0.0218 -0.1052 0.3368 0.047 Uiso 1 1 calc R . . C10 C -0.3657(3) 0.1002(2) 0.35501(9) 0.0294(5) Uani 1 1 d . . . H10A H -0.4157 0.1315 0.3252 0.044 Uiso 1 1 calc R . . H10B H -0.4243 0.1438 0.3815 0.044 Uiso 1 1 calc R . . H10C H -0.3839 0.0063 0.3575 0.044 Uiso 1 1 calc R . . C11 C -0.1435(3) 0.46523(19) 0.40299(8) 0.0193(5) Uani 1 1 d . . . H11 H -0.2189 0.5030 0.3775 0.023 Uiso 1 1 calc R . . C12 C 0.0502(3) 0.5132(2) 0.39695(7) 0.0198(5) Uani 1 1 d . . . H12 H 0.0525 0.5786 0.3709 0.024 Uiso 1 1 calc R . . C13 C 0.0868(3) 0.5850(2) 0.44421(7) 0.0210(5) Uani 1 1 d . . . H13 H 0.2146 0.5933 0.4526 0.025 Uiso 1 1 calc R . . C14 C -0.0120(3) 0.7144(2) 0.43939(8) 0.0257(5) Uani 1 1 d . . . H14A H 0.0147 0.7571 0.4089 0.031 Uiso 1 1 calc R . . H14B H 0.0180 0.7743 0.4655 0.031 Uiso 1 1 calc R . . C15 C -0.2081(3) 0.6711(2) 0.44196(8) 0.0267(5) Uani 1 1 d . . . H15A H -0.2701 0.6902 0.4120 0.032 Uiso 1 1 calc R . . H15B H -0.2703 0.7156 0.4681 0.032 Uiso 1 1 calc R . . C16 C -0.1990(3) 0.5220(2) 0.45090(8) 0.0223(5) Uani 1 1 d . . . C17 C -0.0270(3) 0.5120(2) 0.48107(8) 0.0209(5) Uani 1 1 d . . . C18 C 0.0334(3) 0.3737(2) 0.49258(7) 0.0251(5) Uani 1 1 d . . . H18A H -0.0546 0.3317 0.5128 0.038 Uiso 1 1 calc R . . H18B H 0.1472 0.3768 0.5090 0.038 Uiso 1 1 calc R . . H18C H 0.0461 0.3242 0.4633 0.038 Uiso 1 1 calc R . . C19 C -0.0420(4) 0.5817(2) 0.52899(8) 0.0299(6) Uani 1 1 d . . . H19A H -0.0836 0.6707 0.5240 0.045 Uiso 1 1 calc R . . H19B H 0.0741 0.5836 0.5443 0.045 Uiso 1 1 calc R . . H19C H -0.1259 0.5351 0.5491 0.045 Uiso 1 1 calc R . . C20 C -0.3676(3) 0.4649(2) 0.47100(9) 0.0304(6) Uani 1 1 d . . . H20A H -0.4637 0.4755 0.4481 0.046 Uiso 1 1 calc R . . H20B H -0.3981 0.5099 0.5004 0.046 Uiso 1 1 calc R . . H20C H -0.3500 0.3724 0.4775 0.046 Uiso 1 1 calc R . . C21 C 0.3547(3) 0.4717(2) 0.34099(8) 0.0222(5) Uani 1 1 d . . . C22 C 0.4355(3) 0.4106(2) 0.30281(8) 0.0265(5) Uani 1 1 d . . . H22 H 0.4078 0.3226 0.2961 0.032 Uiso 1 1 calc R . . C23 C 0.5563(3) 0.4760(3) 0.27435(9) 0.0322(6) Uani 1 1 d . . . H23 H 0.6086 0.4328 0.2482 0.039 Uiso 1 1 calc R . . C24 C 0.6004(3) 0.6032(3) 0.28393(8) 0.0336(6) Uani 1 1 d . . . H24 H 0.6844 0.6475 0.2649 0.040 Uiso 1 1 calc R . . C25 C 0.5208(3) 0.6653(3) 0.32155(9) 0.0335(6) Uani 1 1 d . . . H25 H 0.5485 0.7535 0.3280 0.040 Uiso 1 1 calc R . . C26 C 0.4010(3) 0.6005(2) 0.35003(8) 0.0278(5) Uani 1 1 d . . . H26 H 0.3497 0.6443 0.3761 0.033 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 P1 0.0186(3) 0.0189(3) 0.0202(3) 0.0000(2) -0.0016(2) -0.0010(2) O1 0.0230(9) 0.0151(7) 0.0224(8) -0.0017(6) 0.0017(6) -0.0010(6) C1 0.0191(12) 0.0208(11) 0.0182(10) -0.0007(9) -0.0012(9) -0.0020(9) C2 0.0210(12) 0.0202(11) 0.0240(10) -0.0037(9) -0.0001(9) 0.0003(9) C3 0.0283(13) 0.0206(10) 0.0283(12) -0.0025(10) -0.0059(11) 0.0068(10) C4 0.0330(15) 0.0189(10) 0.0218(11) 0.0021(9) 0.0007(10) 0.0010(10) C5 0.0237(13) 0.0175(10) 0.0224(10) 0.0009(9) -0.0006(9) -0.0013(10) C6 0.0152(11) 0.0183(10) 0.0186(10) -0.0013(9) -0.0023(9) 0.0005(9) C7 0.0275(13) 0.0217(11) 0.0211(10) -0.0029(9) 0.0002(10) -0.0016(10) C8 0.0309(14) 0.0324(13) 0.0210(11) -0.0008(10) -0.0017(10) -0.0074(11) C9 0.0386(16) 0.0224(12) 0.0332(13) -0.0085(10) 0.0004(12) -0.0002(11) C10 0.0289(14) 0.0227(12) 0.0366(13) -0.0040(11) 0.0020(11) -0.0065(11) C11 0.0204(12) 0.0133(9) 0.0241(11) 0.0001(9) -0.0019(9) 0.0010(9) C12 0.0226(12) 0.0153(10) 0.0215(10) 0.0022(9) 0.0004(9) -0.0001(9) C13 0.0221(13) 0.0179(11) 0.0232(10) -0.0003(9) -0.0001(9) -0.0033(9) C14 0.0333(15) 0.0163(11) 0.0274(12) 0.0010(9) 0.0005(11) -0.0015(10) C15 0.0311(14) 0.0181(10) 0.0308(12) -0.0037(9) -0.0009(11) 0.0053(11) C16 0.0231(12) 0.0176(10) 0.0263(11) -0.0018(9) 0.0005(10) 0.0009(10) C17 0.0248(13) 0.0177(11) 0.0203(11) -0.0002(9) -0.0004(9) -0.0028(10) C18 0.0314(14) 0.0210(11) 0.0229(11) 0.0028(10) -0.0024(10) -0.0015(11) C19 0.0400(16) 0.0248(12) 0.0249(12) -0.0022(10) 0.0025(11) -0.0080(11) C20 0.0252(14) 0.0286(12) 0.0374(14) -0.0082(11) 0.0104(11) -0.0016(11) C21 0.0174(12) 0.0271(11) 0.0223(11) 0.0035(9) -0.0030(9) -0.0018(10) C22 0.0253(13) 0.0272(13) 0.0270(11) 0.0032(10) 0.0004(10) 0.0013(11) C23 0.0262(14) 0.0449(15) 0.0254(12) 0.0032(12) 0.0033(11) 0.0078(12) C24 0.0244(14) 0.0437(15) 0.0327(12) 0.0146(13) 0.0012(10) -0.0048(12) C25 0.0330(16) 0.0351(13) 0.0325(13) 0.0033(11) -0.0025(11) -0.0107(12) C26 0.0292(14) 0.0287(12) 0.0255(11) -0.0009(11) -0.0001(10) -0.0073(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 P1 C21 1.848(2) . ? P1 C12 1.866(2) . ? P1 C1 1.870(2) . ? O1 C6 1.427(2) . ? O1 C11 1.431(2) . ? C1 C2 1.550(3) . ? C1 C6 1.571(3) . ? C1 H1 1.0000 . ? C2 C3 1.538(3) . ? C2 C7 1.556(3) . ? C2 H2 1.0000 . ? C3 C4 1.547(3) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.535(3) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C10 1.521(3) . ? C5 C6 1.540(3) . ? C5 C7 1.569(3) . ? C6 H6 1.0000 . ? C7 C9 1.529(3) . ? C7 C8 1.541(3) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C16 1.537(3) . ? C11 C12 1.557(3) . ? C11 H11 1.0000 . ? C12 C13 1.555(3) . ? C12 H12 1.0000 . ? C13 C14 1.536(3) . ? C13 C17 1.549(3) . ? C13 H13 1.0000 . ? C14 C15 1.553(4) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.558(3) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C20 1.517(3) . ? C16 C17 1.562(3) . ? C17 C18 1.532(3) . ? C17 C19 1.540(3) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C22 1.394(3) . ? C21 C26 1.396(3) . ? C22 C23 1.394(4) . ? C22 H22 0.9500 . ? C23 C24 1.379(4) . ? C23 H23 0.9500 . ? C24 C25 1.382(4) . ? C24 H24 0.9500 . ? C25 C26 1.386(3) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C21 P1 C12 99.32(10) . . ? C21 P1 C1 101.74(10) . . ? C12 P1 C1 99.24(10) . . ? C6 O1 C11 110.95(16) . . ? C2 C1 C6 101.33(16) . . ? C2 C1 P1 116.49(16) . . ? C6 C1 P1 112.68(14) . . ? C2 C1 H1 108.6 . . ? C6 C1 H1 108.6 . . ? P1 C1 H1 108.6 . . ? C3 C2 C1 108.98(17) . . ? C3 C2 C7 102.42(18) . . ? C1 C2 C7 102.01(17) . . ? C3 C2 H2 114.1 . . ? C1 C2 H2 114.1 . . ? C7 C2 H2 114.1 . . ? C2 C3 C4 103.13(18) . . ? C2 C3 H3A 111.1 . . ? C4 C3 H3A 111.1 . . ? C2 C3 H3B 111.1 . . ? C4 C3 H3B 111.1 . . ? H3A C3 H3B 109.1 . . ? C5 C4 C3 104.04(18) . . ? C5 C4 H4A 110.9 . . ? C3 C4 H4A 110.9 . . ? C5 C4 H4B 110.9 . . ? C3 C4 H4B 110.9 . . ? H4A C4 H4B 109.0 . . ? C10 C5 C4 114.86(19) . . ? C10 C5 C6 113.26(18) . . ? C4 C5 C6 107.05(18) . . ? C10 C5 C7 117.33(18) . . ? C4 C5 C7 101.78(17) . . ? C6 C5 C7 100.95(17) . . ? O1 C6 C5 109.33(17) . . ? O1 C6 C1 114.12(17) . . ? C5 C6 C1 104.76(16) . . ? O1 C6 H6 109.5 . . ? C5 C6 H6 109.5 . . ? C1 C6 H6 109.5 . . ? C9 C7 C8 106.42(19) . . ? C9 C7 C2 113.7(2) . . ? C8 C7 C2 115.00(19) . . ? C9 C7 C5 114.1(2) . . ? C8 C7 C5 114.51(19) . . ? C2 C7 C5 93.10(16) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C5 C10 H10A 109.5 . . ? C5 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C5 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? O1 C11 C16 111.21(18) . . ? O1 C11 C12 113.26(17) . . ? C16 C11 C12 103.52(18) . . ? O1 C11 H11 109.6 . . ? C16 C11 H11 109.6 . . ? C12 C11 H11 109.6 . . ? C13 C12 C11 102.97(17) . . ? C13 C12 P1 115.24(15) . . ? C11 C12 P1 113.89(14) . . ? C13 C12 H12 108.1 . . ? C11 C12 H12 108.1 . . ? P1 C12 H12 108.1 . . ? C14 C13 C17 102.16(18) . . ? C14 C13 C12 104.48(18) . . ? C17 C13 C12 104.49(17) . . ? C14 C13 H13 114.7 . . ? C17 C13 H13 114.7 . . ? C12 C13 H13 114.7 . . ? C13 C14 C15 102.24(18) . . ? C13 C14 H14A 111.3 . . ? C15 C14 H14A 111.3 . . ? C13 C14 H14B 111.3 . . ? C15 C14 H14B 111.3 . . ? H14A C14 H14B 109.2 . . ? C14 C15 C16 104.4(2) . . ? C14 C15 H15A 110.9 . . ? C16 C15 H15A 110.9 . . ? C14 C15 H15B 110.9 . . ? C16 C15 H15B 110.9 . . ? H15A C15 H15B 108.9 . . ? C20 C16 C11 114.45(19) . . ? C20 C16 C15 114.0(2) . . ? C11 C16 C15 104.11(18) . . ? C20 C16 C17 118.09(19) . . ? C11 C16 C17 103.30(18) . . ? C15 C16 C17 101.03(18) . . ? C18 C17 C19 105.56(18) . . ? C18 C17 C13 115.43(19) . . ? C19 C17 C13 114.14(18) . . ? C18 C17 C16 115.29(18) . . ? C19 C17 C16 112.96(19) . . ? C13 C17 C16 93.60(17) . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C16 C20 H20A 109.5 . . ? C16 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C16 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C22 C21 C26 117.5(2) . . ? C22 C21 P1 121.39(17) . . ? C26 C21 P1 120.78(18) . . ? C21 C22 C23 121.2(2) . . ? C21 C22 H22 119.4 . . ? C23 C22 H22 119.4 . . ? C24 C23 C22 120.3(2) . . ? C24 C23 H23 119.8 . . ? C22 C23 H23 119.8 . . ? C23 C24 C25 119.1(2) . . ? C23 C24 H24 120.5 . . ? C25 C24 H24 120.5 . . ? C24 C25 C26 120.8(2) . . ? C24 C25 H25 119.6 . . ? C26 C25 H25 119.6 . . ? C25 C26 C21 121.1(2) . . ? C25 C26 H26 119.5 . . ? C21 C26 H26 119.5 . . ? _diffrn_measured_fraction_theta_max 0.971 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.971 _refine_diff_density_max 0.295 _refine_diff_density_min -0.365 _refine_diff_density_rms 0.073 data_Compound_7 _database_code_CSD 213239 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C52 H72 Cl2 O2 P2 PD2, 0.5(C3H6O)' _chemical_formula_sum 'C53.50 H75 Cl2 O2.50 P2 Pd2' _chemical_formula_weight 1103.78 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 10.3021(2) _cell_length_b 22.5573(4) _cell_length_c 12.4212(2) _cell_angle_alpha 90.00 _cell_angle_beta 101.0630(8) _cell_angle_gamma 90.00 _cell_volume 2832.89(9) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 'All obs. reflections' _cell_measurement_theta_min 2.97 _cell_measurement_theta_max 27.48 _exptl_crystal_description needle-like _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.294 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1144 _exptl_absorpt_coefficient_mu 0.822 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.865 _exptl_absorpt_correction_T_max 0.924 _exptl_absorpt_process_details 'SORTAV (Blessing, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Nonius kappa CCD area detector' _diffrn_measurement_method 'phi & omega scan to fill ewald sphere' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24754 _diffrn_reflns_av_R_equivalents 0.0549 _diffrn_reflns_av_sigmaI/netI 0.0840 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.97 _diffrn_reflns_theta_max 27.48 _reflns_number_total 9970 _reflns_number_gt 8602 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Hooft, 1998)' _computing_cell_refinement 'HKL scalepack (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO & scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-96 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 for Windows (Farrugia, 1997)' _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. The crystal lattice contained voids which contained several low electron density peaks suggesting that there were some disordered solvent species. These could not be readily modelled and assumed to be partially occupied and disordered acetone. Eight such sites, two oxygens and six carbons, each with occupancy 0.25, were included in the SHELXL-97 refinement, with ISOR = 0.005 restraint. ; _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^)+(0.0617P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment ; The H of the disordered solvent were ignored; other H atoms were included in calculated positions, riding model ; _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.08(3) _refine_ls_number_reflns 9970 _refine_ls_number_parameters 625 _refine_ls_number_restraints 49 _refine_ls_R_factor_all 0.0549 _refine_ls_R_factor_gt 0.0438 _refine_ls_wR_factor_ref 0.1233 _refine_ls_wR_factor_gt 0.1065 _refine_ls_goodness_of_fit_ref 1.075 _refine_ls_restrained_S_all 1.074 _refine_ls_shift/su_max 0.010 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.20071(4) 0.20695(2) 0.29334(4) 0.01980(12) Uani 1 1 d . . . Pd2 Pd 0.33949(4) 0.29052(2) 0.14941(3) 0.01923(12) Uani 1 1 d . . . P1 P 0.26665(14) 0.18210(7) 0.46720(13) 0.0191(3) Uani 1 1 d . . . P2 P 0.30049(14) 0.38585(7) 0.11916(12) 0.0189(3) Uani 1 1 d . . . Cl1 Cl 0.10854(14) 0.25118(8) 0.11796(12) 0.0275(4) Uani 1 1 d . . . Cl2 Cl 0.40798(14) 0.19330(7) 0.21926(13) 0.0257(4) Uani 1 1 d . . . O1 O 0.1124(4) 0.07610(19) 0.4602(3) 0.0209(9) Uani 1 1 d . . . O2 O 0.4126(4) 0.3936(2) -0.0727(3) 0.0235(10) Uani 1 1 d . . . C1 C 0.0227(5) 0.2137(3) 0.3429(5) 0.0214(13) Uani 1 1 d . . . H1 H -0.0309 0.2452 0.2985 0.026 Uiso 1 1 calc R . . C2 C 0.0205(6) 0.2245(3) 0.4640(5) 0.0233(14) Uani 1 1 d . . . H2 H 0.0349 0.2668 0.4874 0.028 Uiso 1 1 calc R . . C3 C 0.1185(5) 0.1813(3) 0.5291(5) 0.0214(13) Uani 1 1 d . . . H3 H 0.1395 0.1917 0.6088 0.026 Uiso 1 1 calc R . . C4 C 0.0442(6) 0.1209(3) 0.5085(5) 0.0240(14) Uani 1 1 d . . . H4 H 0.0236 0.1059 0.5791 0.029 Uiso 1 1 calc R . . C5 C -0.0855(6) 0.1380(3) 0.4305(5) 0.0253(15) Uani 1 1 d . . . C6 C -0.0510(6) 0.1531(3) 0.3186(5) 0.0275(15) Uani 1 1 d . . . H6A H -0.1317 0.1574 0.2612 0.033 Uiso 1 1 calc R . . H6B H 0.0071 0.1226 0.2955 0.033 Uiso 1 1 calc R . . C7 C -0.1159(6) 0.1986(3) 0.4781(5) 0.0272(15) Uani 1 1 d . . . C8 C -0.1388(6) 0.1981(4) 0.5936(5) 0.0361(18) Uani 1 1 d . . . H8A H -0.1527 0.2387 0.6168 0.054 Uiso 1 1 calc R . . H8B H -0.0616 0.1810 0.6421 0.054 Uiso 1 1 calc R . . H8C H -0.2172 0.1742 0.5974 0.054 Uiso 1 1 calc R . . C9 C -0.2369(6) 0.2296(4) 0.4048(7) 0.0417(19) Uani 1 1 d . . . H9A H -0.3182 0.2087 0.4118 0.062 Uiso 1 1 calc R . . H9B H -0.2263 0.2289 0.3281 0.062 Uiso 1 1 calc R . . H9C H -0.2421 0.2708 0.4287 0.062 Uiso 1 1 calc R . . C10 C -0.1926(6) 0.0909(3) 0.4217(6) 0.0334(17) Uani 1 1 d . . . H10A H -0.2735 0.1054 0.3743 0.050 Uiso 1 1 calc R . . H10B H -0.2104 0.0824 0.4949 0.050 Uiso 1 1 calc R . . H10C H -0.1629 0.0547 0.3903 0.050 Uiso 1 1 calc R . . C11 C 0.3441(6) 0.1118(3) 0.5189(5) 0.0235(14) Uani 1 1 d . . . H11 H 0.3915 0.1196 0.5957 0.028 Uiso 1 1 calc R . . C12 C 0.2412(6) 0.0631(3) 0.5264(5) 0.0245(14) Uani 1 1 d . . . H12 H 0.2328 0.0576 0.6046 0.029 Uiso 1 1 calc R . . C13 C 0.3042(6) 0.0086(3) 0.4867(5) 0.0260(14) Uani 1 1 d . . . C14 C 0.4316(6) -0.0029(4) 0.5747(6) 0.0304(15) Uani 1 1 d . . . H14A H 0.4146 0.0033 0.6497 0.036 Uiso 1 1 calc R . . H14B H 0.4646 -0.0438 0.5690 0.036 Uiso 1 1 calc R . . C15 C 0.5306(6) 0.0430(4) 0.5471(7) 0.0360(18) Uani 1 1 d . . . H15A H 0.5685 0.0671 0.6122 0.043 Uiso 1 1 calc R . . H15B H 0.6032 0.0236 0.5185 0.043 Uiso 1 1 calc R . . C16 C 0.4452(6) 0.0804(3) 0.4597(6) 0.0278(15) Uani 1 1 d . . . H16 H 0.4951 0.1074 0.4182 0.033 Uiso 1 1 calc R . . C17 C 0.3618(6) 0.0309(3) 0.3887(6) 0.0283(15) Uani 1 1 d . . . C18 C 0.2607(7) 0.0539(3) 0.2881(5) 0.0308(16) Uani 1 1 d . . . H18A H 0.3076 0.0652 0.2296 0.046 Uiso 1 1 calc R . . H18B H 0.2140 0.0884 0.3097 0.046 Uiso 1 1 calc R . . H18C H 0.1968 0.0225 0.2614 0.046 Uiso 1 1 calc R . . C19 C 0.4469(7) -0.0142(4) 0.3405(7) 0.0413(19) Uani 1 1 d . . . H19A H 0.3896 -0.0444 0.2991 0.062 Uiso 1 1 calc R . . H19B H 0.5091 -0.0332 0.4002 0.062 Uiso 1 1 calc R . . H19C H 0.4963 0.0062 0.2915 0.062 Uiso 1 1 calc R . . C20 C 0.2127(6) -0.0462(3) 0.4660(6) 0.0326(16) Uani 1 1 d . . . H20A H 0.1904 -0.0593 0.5355 0.049 Uiso 1 1 calc R . . H20B H 0.2582 -0.0783 0.4351 0.049 Uiso 1 1 calc R . . H20C H 0.1315 -0.0357 0.4144 0.049 Uiso 1 1 calc R . . C21 C 0.3817(6) 0.2353(3) 0.5430(5) 0.0234(14) Uani 1 1 d . . . C22 C 0.4196(7) 0.2340(4) 0.6561(6) 0.0384(18) Uani 1 1 d . . . H22 H 0.3815 0.2060 0.6980 0.046 Uiso 1 1 calc R . . C23 C 0.5142(7) 0.2741(3) 0.7080(6) 0.0392(19) Uani 1 1 d . . . H23 H 0.5396 0.2733 0.7856 0.047 Uiso 1 1 calc R . . C24 C 0.5713(7) 0.3146(3) 0.6490(6) 0.0356(17) Uani 1 1 d . . . H24 H 0.6385 0.3402 0.6860 0.043 Uiso 1 1 calc R . . C25 C 0.5327(6) 0.3183(3) 0.5379(6) 0.0308(16) Uani 1 1 d . . . H25 H 0.5693 0.3480 0.4983 0.037 Uiso 1 1 calc R . . C26 C 0.4390(6) 0.2785(3) 0.4821(5) 0.0268(15) Uani 1 1 d . . . H26 H 0.4138 0.2802 0.4045 0.032 Uiso 1 1 calc R . . C27 C 0.5325(6) 0.3180(3) 0.1669(5) 0.0209(13) Uani 1 1 d . . . H27 H 0.5890 0.2911 0.2203 0.025 Uiso 1 1 calc R . . C28 C 0.5645(6) 0.3828(3) 0.2034(5) 0.0222(14) Uani 1 1 d . . . H28 H 0.5716 0.3906 0.2835 0.027 Uiso 1 1 calc R . . C29 C 0.4618(6) 0.4212(3) 0.1262(5) 0.0222(13) Uani 1 1 d . . . H29 H 0.4618 0.4631 0.1524 0.027 Uiso 1 1 calc R . . C30 C 0.5082(6) 0.4168(3) 0.0138(5) 0.0257(15) Uani 1 1 d . . . H30 H 0.5361 0.4569 -0.0073 0.031 Uiso 1 1 calc R . . C31 C 0.6293(6) 0.3761(3) 0.0381(5) 0.0225(14) Uani 1 1 d . . . C32 C 0.5794(6) 0.3140(3) 0.0552(5) 0.0295(16) Uani 1 1 d . . . H32A H 0.6511 0.2844 0.0587 0.035 Uiso 1 1 calc R . . H32B H 0.5053 0.3030 -0.0047 0.035 Uiso 1 1 calc R . . C33 C 0.6933(6) 0.3947(3) 0.1573(5) 0.0247(14) Uani 1 1 d . . . C34 C 0.8115(6) 0.3560(4) 0.2090(6) 0.0365(19) Uani 1 1 d . . . H34A H 0.7910 0.3143 0.1916 0.055 Uiso 1 1 calc R . . H34B H 0.8296 0.3615 0.2887 0.055 Uiso 1 1 calc R . . H34C H 0.8895 0.3677 0.1796 0.055 Uiso 1 1 calc R . . C35 C 0.7403(7) 0.4603(3) 0.1677(6) 0.0335(17) Uani 1 1 d . . . H35A H 0.7732 0.4698 0.2451 0.050 Uiso 1 1 calc R . . H35B H 0.6661 0.4864 0.1382 0.050 Uiso 1 1 calc R . . H35C H 0.8114 0.4659 0.1264 0.050 Uiso 1 1 calc R . . C36 C 0.7144(6) 0.3788(4) -0.0497(6) 0.0391(19) Uani 1 1 d . . . H36A H 0.7547 0.4182 -0.0492 0.059 Uiso 1 1 calc R . . H36B H 0.6591 0.3713 -0.1218 0.059 Uiso 1 1 calc R . . H36C H 0.7841 0.3487 -0.0343 0.059 Uiso 1 1 calc R . . C37 C 0.2084(6) 0.4210(3) -0.0054(5) 0.0239(14) Uani 1 1 d . . . H37 H 0.1827 0.4615 0.0158 0.029 Uiso 1 1 calc R . . C38 C 0.2956(6) 0.4293(3) -0.0954(5) 0.0219(14) Uani 1 1 d . . . H38 H 0.3206 0.4720 -0.0994 0.026 Uiso 1 1 calc R . . C39 C 0.2002(6) 0.4116(4) -0.2011(5) 0.0310(17) Uani 1 1 d . . . C40 C 0.0914(6) 0.4609(4) -0.2151(6) 0.0372(18) Uani 1 1 d . . . H40A H 0.0396 0.4615 -0.2910 0.045 Uiso 1 1 calc R . . H40B H 0.1312 0.5005 -0.1973 0.045 Uiso 1 1 calc R . . C41 C 0.0016(6) 0.4425(4) -0.1305(6) 0.0368(18) Uani 1 1 d . . . H41A H -0.0070 0.4752 -0.0794 0.044 Uiso 1 1 calc R . . H41B H -0.0875 0.4299 -0.1686 0.044 Uiso 1 1 calc R . . C42 C 0.0795(6) 0.3907(3) -0.0711(5) 0.0303(16) Uani 1 1 d . . . H42 H 0.0298 0.3662 -0.0255 0.036 Uiso 1 1 calc R . . C43 C 0.1239(6) 0.3570(3) -0.1662(5) 0.0288(16) Uani 1 1 d . . . C44 C 0.2085(6) 0.2995(4) -0.1330(5) 0.0332(17) Uani 1 1 d . . . H44A H 0.2763 0.3077 -0.0678 0.050 Uiso 1 1 calc R . . H44B H 0.2512 0.2876 -0.1936 0.050 Uiso 1 1 calc R . . H44C H 0.1508 0.2675 -0.1168 0.050 Uiso 1 1 calc R . . C45 C 0.0085(7) 0.3365(5) -0.2547(6) 0.052(2) Uani 1 1 d . . . H45A H -0.0519 0.3123 -0.2212 0.078 Uiso 1 1 calc R . . H45B H 0.0424 0.3130 -0.3096 0.078 Uiso 1 1 calc R . . H45C H -0.0389 0.3712 -0.2901 0.078 Uiso 1 1 calc R . . C46 C 0.2640(7) 0.4017(5) -0.3015(5) 0.048(2) Uani 1 1 d . . . H46A H 0.2006 0.3819 -0.3593 0.073 Uiso 1 1 calc R . . H46B H 0.3428 0.3768 -0.2809 0.073 Uiso 1 1 calc R . . H46C H 0.2891 0.4400 -0.3286 0.073 Uiso 1 1 calc R . . C47 C 0.2247(6) 0.4190(3) 0.2254(5) 0.0259(15) Uani 1 1 d . . . C48 C 0.1826(6) 0.3830(4) 0.3034(5) 0.0302(16) Uani 1 1 d . . . H48 H 0.1964 0.3414 0.3031 0.036 Uiso 1 1 calc R . . C49 C 0.1192(7) 0.4091(4) 0.3828(5) 0.0364(19) Uani 1 1 d . . . H49 H 0.0920 0.3847 0.4368 0.044 Uiso 1 1 calc R . . C50 C 0.0961(6) 0.4693(4) 0.3836(6) 0.0369(19) Uani 1 1 d . . . H50 H 0.0510 0.4859 0.4363 0.044 Uiso 1 1 calc R . . C51 C 0.1382(7) 0.5048(4) 0.3083(6) 0.0388(18) Uani 1 1 d . . . H51 H 0.1245 0.5464 0.3095 0.047 Uiso 1 1 calc R . . C52 C 0.2023(7) 0.4794(3) 0.2288(5) 0.0320(16) Uani 1 1 d . . . H52 H 0.2308 0.5043 0.1763 0.038 Uiso 1 1 calc R . . O01 O 0.182(2) 0.1271(11) 0.7832(16) 0.044(5) Uani 0.25 1 d PU . . C02 C 0.273(3) 0.1249(15) 0.886(2) 0.038(7) Uani 0.25 1 d PU . . C03 C 0.151(3) 0.1203(16) 0.885(3) 0.045(8) Uani 0.25 1 d PU . . C04 C 0.380(3) 0.1368(17) 0.926(3) 0.050(8) Uani 0.25 1 d PU . . C05 C 0.139(4) 0.101(2) 0.960(3) 0.067(11) Uani 0.25 1 d PU . . O02 O 0.375(3) 0.5655(17) 0.076(3) 0.091(9) Uani 0.25 1 d PU . . C07 C 0.258(7) 0.594(4) 0.037(6) 0.14(2) Uani 0.25 1 d PU . . C08 C 0.323(4) 0.634(2) -0.058(4) 0.077(12) Uani 0.25 1 d PU . . 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 0.0164(2) 0.0202(3) 0.0231(2) 0.0042(2) 0.00463(17) -0.0002(2) Pd2 0.0166(2) 0.0214(3) 0.0199(2) 0.0019(2) 0.00377(17) -0.0001(2) P1 0.0166(7) 0.0182(9) 0.0228(8) 0.0035(6) 0.0044(6) -0.0013(6) P2 0.0158(7) 0.0213(9) 0.0202(7) 0.0040(7) 0.0045(6) -0.0001(7) Cl1 0.0217(7) 0.0350(10) 0.0251(7) 0.0073(7) 0.0029(6) -0.0052(7) Cl2 0.0244(7) 0.0207(10) 0.0345(8) 0.0064(7) 0.0119(7) 0.0016(6) O1 0.0173(19) 0.017(2) 0.028(2) 0.0017(19) 0.0049(18) 0.0026(18) O2 0.0172(19) 0.034(3) 0.019(2) -0.0010(19) 0.0023(17) 0.0015(19) C1 0.017(3) 0.022(4) 0.028(3) 0.008(3) 0.010(2) 0.008(3) C2 0.024(3) 0.021(4) 0.028(3) 0.005(3) 0.014(3) 0.001(3) C3 0.016(3) 0.025(4) 0.025(3) -0.008(3) 0.010(2) 0.004(3) C4 0.020(3) 0.024(4) 0.028(3) 0.005(3) 0.008(3) -0.003(3) C5 0.014(3) 0.026(4) 0.036(4) 0.010(3) 0.005(3) -0.003(3) C6 0.015(3) 0.034(4) 0.030(3) 0.013(3) -0.004(3) -0.003(3) C7 0.021(3) 0.025(4) 0.039(3) 0.011(3) 0.017(3) 0.000(3) C8 0.027(3) 0.050(5) 0.036(4) -0.009(4) 0.019(3) 0.002(3) C9 0.025(3) 0.040(5) 0.063(5) 0.002(4) 0.016(3) 0.018(3) C10 0.021(3) 0.030(4) 0.049(4) 0.006(3) 0.006(3) -0.003(3) C11 0.018(3) 0.027(4) 0.023(3) 0.006(3) -0.004(2) -0.001(3) C12 0.021(3) 0.023(4) 0.025(3) 0.007(3) -0.008(3) -0.005(3) C13 0.022(3) 0.018(4) 0.038(4) 0.007(3) 0.003(3) 0.001(3) C14 0.019(3) 0.027(4) 0.041(4) 0.013(3) -0.003(3) 0.007(3) C15 0.014(3) 0.031(4) 0.061(5) 0.018(4) 0.003(3) 0.002(3) C16 0.018(3) 0.018(4) 0.049(4) 0.003(3) 0.009(3) 0.004(3) C17 0.024(3) 0.013(4) 0.046(4) 0.008(3) 0.005(3) 0.001(3) C18 0.038(4) 0.032(4) 0.025(3) 0.005(3) 0.012(3) -0.006(3) C19 0.041(4) 0.031(5) 0.059(5) -0.001(4) 0.025(4) 0.007(4) C20 0.026(3) 0.023(4) 0.046(4) 0.009(3) -0.001(3) 0.001(3) C21 0.018(3) 0.029(4) 0.024(3) -0.001(3) 0.006(2) -0.004(3) C22 0.053(4) 0.035(4) 0.031(4) 0.000(3) 0.016(3) -0.019(4) C23 0.053(4) 0.036(5) 0.027(3) -0.002(3) 0.002(3) -0.011(4) C24 0.030(3) 0.035(4) 0.041(4) -0.008(3) 0.005(3) -0.008(3) C25 0.032(3) 0.026(4) 0.038(4) 0.001(3) 0.014(3) -0.008(3) C26 0.024(3) 0.026(4) 0.030(3) -0.001(3) 0.004(3) -0.002(3) C27 0.020(3) 0.020(3) 0.023(3) -0.001(3) 0.005(2) 0.000(3) C28 0.022(3) 0.023(4) 0.020(3) 0.005(3) 0.001(2) -0.003(3) C29 0.022(3) 0.021(4) 0.024(3) 0.001(3) 0.003(3) -0.001(3) C30 0.021(3) 0.031(4) 0.024(3) 0.008(3) 0.002(3) -0.008(3) C31 0.017(3) 0.027(4) 0.023(3) -0.002(3) 0.004(2) -0.001(3) C32 0.020(3) 0.035(4) 0.034(4) -0.004(3) 0.007(3) -0.003(3) C33 0.019(3) 0.027(4) 0.027(3) -0.009(3) 0.004(3) 0.002(3) C34 0.016(3) 0.046(5) 0.045(4) 0.019(4) -0.001(3) -0.004(3) C35 0.027(3) 0.036(5) 0.036(4) 0.007(3) 0.002(3) -0.012(3) C36 0.021(3) 0.057(6) 0.039(4) -0.005(4) 0.005(3) -0.004(3) C37 0.020(3) 0.024(4) 0.028(3) 0.007(3) 0.006(3) 0.004(3) C38 0.023(3) 0.019(4) 0.024(3) 0.009(3) 0.005(3) 0.000(3) C39 0.023(3) 0.049(5) 0.021(3) 0.007(3) 0.004(3) -0.005(3) C40 0.023(3) 0.045(5) 0.039(4) 0.018(4) -0.006(3) -0.003(3) C41 0.023(3) 0.053(5) 0.033(4) 0.010(4) 0.003(3) 0.011(3) C42 0.017(3) 0.043(5) 0.030(3) 0.012(3) 0.003(3) -0.008(3) C43 0.019(3) 0.039(5) 0.027(3) 0.000(3) 0.002(3) -0.013(3) C44 0.033(3) 0.041(5) 0.025(3) -0.002(3) 0.003(3) -0.003(4) C45 0.036(4) 0.081(7) 0.033(4) 0.011(4) -0.009(3) -0.025(4) C46 0.036(4) 0.089(8) 0.018(3) 0.019(4) 0.001(3) -0.007(4) C47 0.017(3) 0.033(4) 0.024(3) -0.001(3) -0.004(3) 0.004(3) C48 0.030(3) 0.036(5) 0.023(3) 0.006(3) 0.004(3) -0.007(3) C49 0.036(4) 0.057(6) 0.019(3) -0.018(3) 0.012(3) -0.003(4) C50 0.027(3) 0.050(5) 0.036(4) -0.025(4) 0.011(3) 0.002(3) C51 0.036(4) 0.040(5) 0.040(4) -0.007(4) 0.007(3) 0.002(4) C52 0.035(4) 0.034(5) 0.027(3) -0.001(3) 0.009(3) -0.001(3) O01 0.057(7) 0.037(7) 0.034(6) 0.000(5) -0.001(5) -0.002(5) C02 0.044(8) 0.034(8) 0.036(8) 0.006(5) 0.009(5) 0.001(5) C03 0.052(9) 0.037(9) 0.043(9) -0.008(5) 0.005(5) 0.001(5) C04 0.054(9) 0.049(10) 0.046(9) -0.004(5) 0.008(5) 0.002(5) C05 0.070(11) 0.067(12) 0.065(11) -0.003(5) 0.017(5) 0.001(5) O02 0.095(10) 0.089(10) 0.091(10) 0.003(5) 0.021(5) -0.002(5) C07 0.14(3) 0.15(3) 0.14(3) -0.001(5) 0.030(7) 0.001(5) C08 0.079(13) 0.076(13) 0.077(13) 0.005(5) 0.013(5) -0.005(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 C1 2.049(5) . ? Pd1 P1 2.2083(16) . ? Pd1 Cl1 2.4185(16) . ? Pd1 Cl2 2.5010(14) . ? Pd1 Pd2 3.1265(6) . ? Pd2 C27 2.054(6) . ? Pd2 P2 2.2067(17) . ? Pd2 Cl2 2.4135(16) . ? Pd2 Cl1 2.4988(15) . ? P1 C21 1.818(7) . ? P1 C11 1.835(7) . ? P1 C3 1.836(5) . ? P2 C47 1.818(6) . ? P2 C29 1.830(6) . ? P2 C37 1.833(6) . ? O1 C4 1.428(8) . ? O1 C12 1.450(7) . ? O2 C30 1.412(7) . ? O2 C38 1.432(7) . ? C1 C2 1.528(8) . ? C1 C6 1.564(10) . ? C2 C3 1.519(9) . ? C2 C7 1.562(8) . ? C3 C4 1.559(9) . ? C4 C5 1.541(9) . ? C5 C10 1.519(9) . ? C5 C6 1.538(8) . ? C5 C7 1.546(10) . ? C7 C8 1.498(8) . ? C7 C9 1.560(9) . ? C11 C12 1.542(9) . ? C11 C16 1.556(8) . ? C12 C13 1.516(10) . ? C13 C17 1.537(9) . ? C13 C20 1.546(9) . ? C13 C14 1.560(9) . ? C14 C15 1.537(10) . ? C15 C16 1.517(9) . ? C16 C17 1.573(10) . ? C17 C19 1.538(9) . ? C17 C18 1.554(9) . ? C21 C22 1.385(9) . ? C21 C26 1.428(9) . ? C22 C23 1.392(10) . ? C23 C24 1.372(10) . ? C24 C25 1.364(10) . ? C25 C26 1.401(9) . ? C27 C28 1.547(9) . ? C27 C32 1.557(8) . ? C28 C29 1.549(9) . ? C28 C33 1.565(8) . ? C29 C30 1.563(8) . ? C30 C31 1.532(9) . ? C31 C32 1.522(10) . ? C31 C36 1.525(9) . ? C31 C33 1.558(8) . ? C33 C34 1.535(9) . ? C33 C35 1.554(10) . ? C37 C38 1.574(8) . ? C37 C42 1.575(9) . ? C38 C39 1.534(9) . ? C39 C46 1.533(9) . ? C39 C40 1.565(10) . ? C39 C43 1.566(10) . ? C40 C41 1.583(9) . ? C41 C42 1.525(10) . ? C42 C43 1.546(10) . ? C43 C45 1.527(9) . ? C43 C44 1.573(11) . ? C47 C52 1.383(10) . ? C47 C48 1.396(9) . ? C48 C49 1.412(9) . ? C49 C50 1.379(12) . ? C50 C51 1.364(11) . ? C51 C52 1.412(10) . ? O01 C03 1.38(4) . ? O01 C02 1.43(4) . ? C02 C04 1.15(4) . ? C02 C03 1.26(4) . ? C02 C05 1.87(5) . ? C03 C05 1.06(5) . ? O02 C07 1.37(8) . ? C07 C08 1.73(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Pd1 P1 81.37(17) . . ? C1 Pd1 Cl1 91.20(17) . . ? P1 Pd1 Cl1 168.39(6) . . ? C1 Pd1 Cl2 175.01(19) . . ? P1 Pd1 Cl2 101.80(5) . . ? Cl1 Pd1 Cl2 86.26(5) . . ? C1 Pd1 Pd2 131.38(18) . . ? P1 Pd1 Pd2 128.58(4) . . ? Cl1 Pd1 Pd2 51.66(4) . . ? Cl2 Pd1 Pd2 49.27(4) . . ? C27 Pd2 P2 82.24(19) . . ? C27 Pd2 Cl2 91.48(18) . . ? P2 Pd2 Cl2 167.92(6) . . ? C27 Pd2 Cl1 175.57(17) . . ? P2 Pd2 Cl1 100.52(6) . . ? Cl2 Pd2 Cl1 86.41(5) . . ? C27 Pd2 Pd1 131.38(17) . . ? P2 Pd2 Pd1 126.63(4) . . ? Cl2 Pd2 Pd1 51.74(3) . . ? Cl1 Pd2 Pd1 49.39(4) . . ? C21 P1 C11 101.1(3) . . ? C21 P1 C3 107.5(3) . . ? C11 P1 C3 100.7(3) . . ? C21 P1 Pd1 112.7(2) . . ? C11 P1 Pd1 126.4(2) . . ? C3 P1 Pd1 106.7(2) . . ? C47 P2 C29 107.4(3) . . ? C47 P2 C37 102.1(3) . . ? C29 P2 C37 99.8(3) . . ? C47 P2 Pd2 111.5(2) . . ? C29 P2 Pd2 106.4(2) . . ? C37 P2 Pd2 127.8(2) . . ? Pd1 Cl1 Pd2 78.94(4) . . ? Pd2 Cl2 Pd1 79.00(4) . . ? C4 O1 C12 112.0(5) . . ? C30 O2 C38 112.3(5) . . ? C2 C1 C6 103.4(5) . . ? C2 C1 Pd1 119.4(4) . . ? C6 C1 Pd1 107.9(4) . . ? C3 C2 C1 106.7(5) . . ? C3 C2 C7 102.7(5) . . ? C1 C2 C7 103.5(5) . . ? C2 C3 C4 102.6(5) . . ? C2 C3 P1 106.9(4) . . ? C4 C3 P1 111.2(4) . . ? O1 C4 C5 110.4(5) . . ? O1 C4 C3 114.9(4) . . ? C5 C4 C3 103.0(5) . . ? C10 C5 C6 112.4(6) . . ? C10 C5 C4 113.7(6) . . ? C6 C5 C4 107.5(5) . . ? C10 C5 C7 116.6(5) . . ? C6 C5 C7 104.3(5) . . ? C4 C5 C7 101.2(5) . . ? C5 C6 C1 102.0(5) . . ? C8 C7 C5 116.1(6) . . ? C8 C7 C9 107.8(5) . . ? C5 C7 C9 111.8(6) . . ? C8 C7 C2 114.9(6) . . ? C5 C7 C2 92.0(4) . . ? C9 C7 C2 113.7(5) . . ? C12 C11 C16 103.6(5) . . ? C12 C11 P1 112.2(4) . . ? C16 C11 P1 120.9(4) . . ? O1 C12 C13 112.4(5) . . ? O1 C12 C11 112.8(5) . . ? C13 C12 C11 102.5(5) . . ? C12 C13 C17 104.3(5) . . ? C12 C13 C20 114.6(5) . . ? C17 C13 C20 116.4(6) . . ? C12 C13 C14 105.2(6) . . ? C17 C13 C14 102.1(5) . . ? C20 C13 C14 112.8(6) . . ? C15 C14 C13 103.7(5) . . ? C16 C15 C14 102.5(5) . . ? C15 C16 C11 105.3(5) . . ? C15 C16 C17 100.7(6) . . ? C11 C16 C17 104.2(5) . . ? C13 C17 C19 115.3(6) . . ? C13 C17 C18 116.5(5) . . ? C19 C17 C18 104.6(6) . . ? C13 C17 C16 92.3(5) . . ? C19 C17 C16 113.4(5) . . ? C18 C17 C16 115.0(6) . . ? C22 C21 C26 119.1(6) . . ? C22 C21 P1 122.7(5) . . ? C26 C21 P1 118.1(5) . . ? C21 C22 C23 119.5(6) . . ? C24 C23 C22 121.3(7) . . ? C25 C24 C23 120.6(7) . . ? C24 C25 C26 120.0(6) . . ? C25 C26 C21 119.4(6) . . ? C28 C27 C32 103.3(5) . . ? C28 C27 Pd2 117.6(4) . . ? C32 C27 Pd2 110.4(4) . . ? C27 C28 C29 105.4(5) . . ? C27 C28 C33 101.7(5) . . ? C29 C28 C33 101.7(5) . . ? C28 C29 C30 103.1(5) . . ? C28 C29 P2 107.0(4) . . ? C30 C29 P2 111.1(4) . . ? O2 C30 C31 110.6(6) . . ? O2 C30 C29 114.5(5) . . ? C31 C30 C29 103.9(5) . . ? C32 C31 C36 113.1(6) . . ? C32 C31 C30 107.2(5) . . ? C36 C31 C30 113.2(6) . . ? C32 C31 C33 102.0(5) . . ? C36 C31 C33 118.2(5) . . ? C30 C31 C33 101.8(5) . . ? C31 C32 C27 104.0(5) . . ? C34 C33 C35 107.2(5) . . ? C34 C33 C31 113.7(5) . . ? C35 C33 C31 113.8(6) . . ? C34 C33 C28 114.2(5) . . ? C35 C33 C28 113.9(5) . . ? C31 C33 C28 93.9(4) . . ? C38 C37 C42 102.9(5) . . ? C38 C37 P2 112.2(4) . . ? C42 C37 P2 119.8(5) . . ? O2 C38 C39 113.4(5) . . ? O2 C38 C37 111.5(5) . . ? C39 C38 C37 102.6(5) . . ? C46 C39 C38 115.5(5) . . ? C46 C39 C40 115.0(6) . . ? C38 C39 C40 103.7(6) . . ? C46 C39 C43 115.2(7) . . ? C38 C39 C43 104.0(5) . . ? C40 C39 C43 101.7(5) . . ? C39 C40 C41 103.7(6) . . ? C42 C41 C40 101.7(5) . . ? C41 C42 C43 102.2(5) . . ? C41 C42 C37 103.3(6) . . ? C43 C42 C37 105.4(5) . . ? C45 C43 C42 113.3(6) . . ? C45 C43 C39 113.7(6) . . ? C42 C43 C39 93.6(5) . . ? C45 C43 C44 104.8(6) . . ? C42 C43 C44 115.8(5) . . ? C39 C43 C44 116.0(5) . . ? C52 C47 C48 118.4(6) . . ? C52 C47 P2 121.6(5) . . ? C48 C47 P2 119.9(6) . . ? C47 C48 C49 119.3(7) . . ? C50 C49 C48 121.2(7) . . ? C51 C50 C49 119.7(6) . . ? C50 C51 C52 119.6(7) . . ? C47 C52 C51 121.6(7) . . ? C03 O01 C02 53.0(19) . . ? C04 C02 C03 154(4) . . ? C04 C02 O01 141(3) . . ? C03 C02 O01 61(2) . . ? C04 C02 C05 127(3) . . ? C03 C02 C05 32(2) . . ? O01 C02 C05 92(2) . . ? C05 C03 C02 108(4) . . ? C05 C03 O01 161(4) . . ? C02 C03 O01 66(2) . . ? C03 C05 C02 40(3) . . ? O02 C07 C08 93(5) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.883 _refine_diff_density_min -0.610 _refine_diff_density_rms 0.108 data_compound_8 _database_code_CSD 213240 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C52 H72 Cl2 O2 P2 Pt2, 0.5(C3H6O)' _chemical_formula_sum 'C53.50 H75 Cl2 O2.50 P2 Pt2' _chemical_formula_weight 1281.16 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 10.3287(2) _cell_length_b 22.5278(5) _cell_length_c 12.4452(3) _cell_angle_alpha 90.00 _cell_angle_beta 101.0500(11) _cell_angle_gamma 90.00 _cell_volume 2842.10(11) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 'all obs. reflections' _cell_measurement_theta_min 2.97 _cell_measurement_theta_max 26.02 _exptl_crystal_description needle-like _exptl_crystal_colour colorless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.497 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1272 _exptl_absorpt_coefficient_mu 5.103 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.181 _exptl_absorpt_correction_T_max 0.579 _exptl_absorpt_process_details 'SORTAV (Blessing, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Nonius kappa CCD area detector' _diffrn_measurement_method 'phi & omega scan to fill Ewald sphere' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11276 _diffrn_reflns_av_R_equivalents 0.0501 _diffrn_reflns_av_sigmaI/netI 0.0848 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.97 _diffrn_reflns_theta_max 26.02 _reflns_number_total 7768 _reflns_number_gt 7217 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Hooft, 1998)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO & Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-96 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 for Windows (Farrugia, 1997)' _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. The crystal structure contained a half occupied 0.5 acetone solvent molecule per asymmetric unit in a void; four sites (three carbons and one oxygen) these atoms were refined with occupancy 0.5, C-C distance fixed at 1.52 A and an ISOR = 0.003 restraint. C1 and C29 atoms of the complex were also refined with ISOR 0.003. ; _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^)+(0.0958P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment 'calculated positions, riding model' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.006(12) _refine_ls_number_reflns 7768 _refine_ls_number_parameters 591 _refine_ls_number_restraints 39 _refine_ls_R_factor_all 0.0542 _refine_ls_R_factor_gt 0.0494 _refine_ls_wR_factor_ref 0.1513 _refine_ls_wR_factor_gt 0.1330 _refine_ls_goodness_of_fit_ref 1.076 _refine_ls_restrained_S_all 1.074 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.20091(5) 0.20682(2) 0.29592(4) 0.01942(15) Uani 1 1 d . . . Pt2 Pt 0.34163(5) 0.29111(2) 0.15177(4) 0.01911(15) Uani 1 1 d . . . P1 P 0.2680(3) 0.18123(15) 0.4666(3) 0.0184(7) Uani 1 1 d . . . P2 P 0.3005(4) 0.38511(16) 0.1208(3) 0.0203(7) Uani 1 1 d . . . Cl1 Cl 0.1121(3) 0.24950(16) 0.1199(3) 0.0274(8) Uani 1 1 d . . . Cl2 Cl 0.4063(3) 0.19330(14) 0.2186(3) 0.0241(8) Uani 1 1 d . . . O1 O 0.1118(9) 0.0745(4) 0.4597(8) 0.025(2) Uani 1 1 d . . . O2 O 0.4137(10) 0.3929(4) -0.0713(8) 0.024(2) Uani 1 1 d . . . C1 C 0.0196(12) 0.2131(6) 0.3424(10) 0.020(3) Uani 1 1 d U . . H1 H -0.0337 0.2447 0.2979 0.024 Uiso 1 1 calc R . . C2 C 0.0215(14) 0.2248(6) 0.4641(12) 0.026(3) Uani 1 1 d . . . H2 H 0.0371 0.2670 0.4880 0.031 Uiso 1 1 calc R . . C3 C 0.1195(13) 0.1797(6) 0.5256(11) 0.021(3) Uani 1 1 d . . . H3 H 0.1419 0.1904 0.6049 0.025 Uiso 1 1 calc R . . C4 C 0.0435(13) 0.1205(6) 0.5113(13) 0.027(3) Uani 1 1 d . . . H4 H 0.0257 0.1063 0.5832 0.032 Uiso 1 1 calc R . . C5 C -0.0867(15) 0.1360(6) 0.4328(12) 0.027(3) Uani 1 1 d . . . C6 C -0.0489(17) 0.1524(7) 0.3143(13) 0.036(4) Uani 1 1 d . . . H6A H 0.0120 0.1228 0.2924 0.043 Uiso 1 1 calc R . . H6B H -0.1284 0.1560 0.2560 0.043 Uiso 1 1 calc R . . C7 C -0.1105(16) 0.1991(8) 0.4769(15) 0.038(4) Uani 1 1 d . . . C8 C -0.1344(16) 0.1978(9) 0.5958(15) 0.044(4) Uani 1 1 d . . . H8A H -0.1517 0.2382 0.6187 0.065 Uiso 1 1 calc R . . H8B H -0.0562 0.1819 0.6444 0.065 Uiso 1 1 calc R . . H8C H -0.2107 0.1725 0.5995 0.065 Uiso 1 1 calc R . . C9 C -0.2363(16) 0.2309(8) 0.4083(15) 0.041(4) Uani 1 1 d . . . H9A H -0.3159 0.2091 0.4169 0.061 Uiso 1 1 calc R . . H9B H -0.2297 0.2316 0.3308 0.061 Uiso 1 1 calc R . . H9C H -0.2413 0.2716 0.4347 0.061 Uiso 1 1 calc R . . C10 C -0.1956(15) 0.0893(7) 0.4245(14) 0.036(4) Uani 1 1 d . . . H10A H -0.2691 0.1001 0.3656 0.054 Uiso 1 1 calc R . . H10B H -0.2266 0.0873 0.4941 0.054 Uiso 1 1 calc R . . H10C H -0.1606 0.0505 0.4086 0.054 Uiso 1 1 calc R . . C11 C 0.3422(15) 0.1107(7) 0.5133(13) 0.031(4) Uani 1 1 d . . . H11 H 0.3915 0.1182 0.5894 0.038 Uiso 1 1 calc R . . C12 C 0.2387(14) 0.0619(6) 0.5256(12) 0.024(3) Uani 1 1 d . . . H12 H 0.2315 0.0575 0.6042 0.029 Uiso 1 1 calc R . . C13 C 0.3019(14) 0.0065(6) 0.4863(13) 0.025(3) Uani 1 1 d . . . C14 C 0.4259(16) -0.0052(7) 0.5708(15) 0.033(4) Uani 1 1 d . . . H14A H 0.4582 -0.0462 0.5645 0.039 Uiso 1 1 calc R . . H14B H 0.4100 0.0010 0.6459 0.039 Uiso 1 1 calc R . . C15 C 0.5274(14) 0.0420(8) 0.5414(15) 0.036(4) Uani 1 1 d . . . H15A H 0.5652 0.0666 0.6057 0.044 Uiso 1 1 calc R . . H15B H 0.5998 0.0226 0.5128 0.044 Uiso 1 1 calc R . . C16 C 0.4418(13) 0.0784(6) 0.4546(12) 0.023(3) Uani 1 1 d . . . H16 H 0.4912 0.1051 0.4125 0.027 Uiso 1 1 calc R . . C17 C 0.3584(16) 0.0316(6) 0.3861(13) 0.031(4) Uani 1 1 d . . . C18 C 0.2583(17) 0.0519(7) 0.2864(12) 0.035(4) Uani 1 1 d . . . H18A H 0.3049 0.0687 0.2318 0.052 Uiso 1 1 calc R . . H18B H 0.2006 0.0822 0.3086 0.052 Uiso 1 1 calc R . . H18C H 0.2052 0.0179 0.2547 0.052 Uiso 1 1 calc R . . C19 C 0.4470(18) -0.0151(7) 0.3383(15) 0.043(4) Uani 1 1 d . . . H19A H 0.3902 -0.0443 0.2935 0.064 Uiso 1 1 calc R . . H19B H 0.5047 -0.0355 0.3988 0.064 Uiso 1 1 calc R . . H19C H 0.5008 0.0054 0.2931 0.064 Uiso 1 1 calc R . . C20 C 0.2116(15) -0.0476(6) 0.4631(14) 0.034(4) Uani 1 1 d . . . H20A H 0.1633 -0.0529 0.5229 0.050 Uiso 1 1 calc R . . H20B H 0.2649 -0.0831 0.4572 0.050 Uiso 1 1 calc R . . H20C H 0.1488 -0.0416 0.3942 0.050 Uiso 1 1 calc R . . C21 C 0.3815(14) 0.2351(6) 0.5422(11) 0.019(3) Uani 1 1 d . . . C22 C 0.417(2) 0.2329(8) 0.6569(15) 0.047(5) Uani 1 1 d . . . H22 H 0.3745 0.2053 0.6966 0.057 Uiso 1 1 calc R . . C23 C 0.5134(16) 0.2710(7) 0.7131(13) 0.035(4) Uani 1 1 d . . . H23 H 0.5402 0.2684 0.7903 0.042 Uiso 1 1 calc R . . C24 C 0.5693(16) 0.3125(7) 0.6543(15) 0.038(4) Uani 1 1 d . . . H24 H 0.6331 0.3392 0.6924 0.045 Uiso 1 1 calc R . . C25 C 0.5350(15) 0.3163(7) 0.5418(12) 0.027(3) Uani 1 1 d . . . H25 H 0.5754 0.3449 0.5027 0.033 Uiso 1 1 calc R . . C26 C 0.4385(14) 0.2769(6) 0.4860(11) 0.026(3) Uani 1 1 d . . . H26 H 0.4130 0.2793 0.4086 0.031 Uiso 1 1 calc R . . C27 C 0.5338(13) 0.3178(6) 0.1683(11) 0.021(3) Uani 1 1 d . . . H27 H 0.5893 0.2912 0.2229 0.025 Uiso 1 1 calc R . . C28 C 0.5634(13) 0.3820(7) 0.2042(11) 0.024(3) Uani 1 1 d . . . H28 H 0.5702 0.3896 0.2843 0.029 Uiso 1 1 calc R . . C29 C 0.4634(13) 0.4206(6) 0.1288(10) 0.017(3) Uani 1 1 d U . . H29 H 0.4638 0.4624 0.1557 0.020 Uiso 1 1 calc R . . C30 C 0.5084(15) 0.4167(6) 0.0152(11) 0.022(3) Uani 1 1 d . . . H30 H 0.5348 0.4571 -0.0059 0.027 Uiso 1 1 calc R . . C31 C 0.6311(14) 0.3766(6) 0.0388(10) 0.021(3) Uani 1 1 d . . . C32 C 0.5826(14) 0.3126(6) 0.0595(13) 0.026(3) Uani 1 1 d . . . H32A H 0.5102 0.3002 -0.0004 0.032 Uiso 1 1 calc R . . H32B H 0.6556 0.2836 0.0655 0.032 Uiso 1 1 calc R . . C33 C 0.6950(13) 0.3960(6) 0.1571(12) 0.023(3) Uani 1 1 d . . . C34 C 0.8114(13) 0.3573(7) 0.2103(12) 0.027(3) Uani 1 1 d . . . H34A H 0.7833 0.3157 0.2093 0.040 Uiso 1 1 calc R . . H34B H 0.8424 0.3701 0.2861 0.040 Uiso 1 1 calc R . . H34C H 0.8832 0.3613 0.1694 0.040 Uiso 1 1 calc R . . C35 C 0.7404(16) 0.4595(7) 0.1717(15) 0.037(4) Uani 1 1 d . . . H35A H 0.7606 0.4692 0.2498 0.056 Uiso 1 1 calc R . . H35B H 0.6704 0.4858 0.1344 0.056 Uiso 1 1 calc R . . H35C H 0.8196 0.4649 0.1402 0.056 Uiso 1 1 calc R . . C36 C 0.7131(16) 0.3807(8) -0.0468(13) 0.032(4) Uani 1 1 d . . . H36A H 0.7505 0.4207 -0.0465 0.048 Uiso 1 1 calc R . . H36B H 0.6582 0.3726 -0.1187 0.048 Uiso 1 1 calc R . . H36C H 0.7847 0.3515 -0.0317 0.048 Uiso 1 1 calc R . . C37 C 0.2092(14) 0.4186(6) -0.0023(12) 0.024(3) Uani 1 1 d . . . H37 H 0.1827 0.4591 0.0184 0.028 Uiso 1 1 calc R . . C38 C 0.2963(14) 0.4276(7) -0.0914(11) 0.024(3) Uani 1 1 d . . . H38 H 0.3201 0.4705 -0.0946 0.029 Uiso 1 1 calc R . . C39 C 0.2035(13) 0.4098(7) -0.1999(11) 0.024(3) Uani 1 1 d . . . C40 C 0.0914(14) 0.4588(8) -0.2128(12) 0.032(4) Uani 1 1 d . . . H40A H 0.0393 0.4588 -0.2883 0.038 Uiso 1 1 calc R . . H40B H 0.1304 0.4987 -0.1964 0.038 Uiso 1 1 calc R . . C41 C 0.0009(15) 0.4416(7) -0.1276(15) 0.037(4) Uani 1 1 d . . . H41A H -0.0055 0.4744 -0.0757 0.044 Uiso 1 1 calc R . . H41B H -0.0887 0.4294 -0.1645 0.044 Uiso 1 1 calc R . . C42 C 0.0818(13) 0.3889(6) -0.0710(11) 0.021(3) Uani 1 1 d . . . H42 H 0.0325 0.3636 -0.0265 0.025 Uiso 1 1 calc R . . C43 C 0.1246(15) 0.3558(7) -0.1657(13) 0.029(3) Uani 1 1 d . . . C44 C 0.2087(18) 0.2995(7) -0.1327(11) 0.036(4) Uani 1 1 d . . . H44A H 0.2599 0.3043 -0.0583 0.053 Uiso 1 1 calc R . . H44B H 0.2688 0.2935 -0.1838 0.053 Uiso 1 1 calc R . . H44C H 0.1505 0.2649 -0.1350 0.053 Uiso 1 1 calc R . . C45 C 0.0104(17) 0.3351(9) -0.2545(15) 0.048(5) Uani 1 1 d . . . H45A H -0.0568 0.3160 -0.2203 0.072 Uiso 1 1 calc R . . H45B H 0.0430 0.3066 -0.3026 0.072 Uiso 1 1 calc R . . H45C H -0.0283 0.3694 -0.2975 0.072 Uiso 1 1 calc R . . C46 C 0.2700(19) 0.4030(10) -0.3014(13) 0.048(5) Uani 1 1 d . . . H46A H 0.2027 0.3936 -0.3661 0.071 Uiso 1 1 calc R . . H46B H 0.3351 0.3709 -0.2884 0.071 Uiso 1 1 calc R . . H46C H 0.3141 0.4402 -0.3138 0.071 Uiso 1 1 calc R . . C47 C 0.2248(13) 0.4181(6) 0.2271(12) 0.021(3) Uani 1 1 d . . . C48 C 0.1864(14) 0.3821(7) 0.3034(11) 0.026(4) Uani 1 1 d . . . H48 H 0.2027 0.3406 0.3030 0.031 Uiso 1 1 calc R . . C49 C 0.1194(16) 0.4082(8) 0.3862(12) 0.032(4) Uani 1 1 d . . . H49 H 0.0948 0.3840 0.4416 0.039 Uiso 1 1 calc R . . C50 C 0.0931(15) 0.4672(8) 0.3827(13) 0.037(4) Uani 1 1 d . . . H50 H 0.0457 0.4843 0.4332 0.045 Uiso 1 1 calc R . . C51 C 0.1350(15) 0.5017(7) 0.3063(14) 0.031(4) Uani 1 1 d . . . H51 H 0.1187 0.5432 0.3074 0.037 Uiso 1 1 calc R . . C52 C 0.1989(16) 0.4803(7) 0.2283(13) 0.031(4) Uani 1 1 d . . . H52 H 0.2256 0.5061 0.1762 0.037 Uiso 1 1 calc R . . O01 O 0.174(3) 0.1248(16) 0.780(3) 0.071(9) Uani 0.50 1 d PU . . C01 C 0.367(3) 0.135(2) 0.933(4) 0.063(11) Uani 0.50 1 d PDU . . H01A H 0.4256 0.1128 0.8951 0.094 Uiso 0.50 1 calc PR . . H01B H 0.3858 0.1253 1.0112 0.094 Uiso 0.50 1 calc PR . . H01C H 0.3811 0.1779 0.9242 0.094 Uiso 0.50 1 calc PR . . C02 C 0.224(3) 0.120(2) 0.885(4) 0.077(14) Uani 0.50 1 d PDU . . C03 C 0.124(6) 0.104(3) 0.955(5) 0.13(2) Uani 0.50 1 d PDU . . H03A H 0.0372 0.0987 0.9081 0.194 Uiso 0.50 1 calc PR . . H03B H 0.1191 0.1366 1.0070 0.194 Uiso 0.50 1 calc PR . . H03C H 0.1508 0.0676 0.9954 0.194 Uiso 0.50 1 calc PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.0206(3) 0.0131(3) 0.0253(3) 0.0034(2) 0.0060(2) -0.0007(2) Pt2 0.0212(3) 0.0152(3) 0.0213(3) 0.0015(2) 0.0050(2) -0.0002(2) P1 0.0188(17) 0.0138(16) 0.0232(18) -0.0019(14) 0.0050(14) 0.0025(15) P2 0.0213(18) 0.0177(18) 0.0204(17) 0.0012(14) 0.0002(14) -0.0007(15) Cl1 0.0266(18) 0.0260(19) 0.0287(18) 0.0082(15) 0.0031(15) -0.0054(16) Cl2 0.0262(18) 0.0168(18) 0.0326(18) 0.0055(14) 0.0140(15) 0.0013(14) O1 0.028(5) 0.016(5) 0.028(5) 0.003(4) -0.002(4) 0.002(4) O2 0.028(5) 0.020(5) 0.027(5) 0.007(4) 0.010(4) -0.002(4) C1 0.019(4) 0.019(4) 0.024(4) -0.004(3) 0.006(3) 0.007(3) C2 0.028(8) 0.021(8) 0.031(8) 0.000(6) 0.014(6) -0.009(6) C3 0.020(7) 0.020(7) 0.022(7) 0.002(6) 0.005(6) -0.002(6) C4 0.019(7) 0.011(7) 0.053(10) 0.000(7) 0.012(7) 0.003(6) C5 0.030(8) 0.020(8) 0.031(8) 0.000(6) 0.004(6) 0.000(6) C6 0.042(10) 0.021(8) 0.037(9) 0.004(7) -0.007(7) -0.005(7) C7 0.025(8) 0.035(10) 0.063(11) 0.015(9) 0.026(8) 0.005(7) C8 0.031(9) 0.046(11) 0.055(11) -0.003(9) 0.013(8) -0.004(8) C9 0.034(9) 0.040(9) 0.055(11) 0.019(8) 0.025(8) 0.011(8) C10 0.030(9) 0.025(8) 0.052(10) -0.012(8) 0.006(8) -0.005(7) C11 0.025(8) 0.022(8) 0.039(9) 0.016(7) -0.014(7) -0.010(6) C12 0.026(8) 0.007(6) 0.036(8) 0.004(6) -0.001(6) -0.001(6) C13 0.016(7) 0.020(7) 0.040(9) 0.010(6) 0.002(6) 0.002(6) C14 0.037(9) 0.015(7) 0.048(9) 0.012(6) 0.013(7) 0.011(6) C15 0.020(8) 0.031(9) 0.056(11) 0.007(8) 0.003(7) 0.006(7) C16 0.020(7) 0.016(7) 0.037(8) 0.012(6) 0.020(6) 0.003(6) C17 0.042(9) 0.010(7) 0.046(9) -0.013(7) 0.025(8) 0.001(7) C18 0.048(10) 0.026(9) 0.035(9) 0.011(7) 0.022(8) -0.008(8) C19 0.054(11) 0.026(9) 0.044(10) -0.002(8) 0.000(8) 0.025(8) C20 0.029(8) 0.016(7) 0.053(10) 0.012(7) 0.002(7) 0.003(7) C21 0.025(7) 0.016(6) 0.021(7) -0.008(5) 0.014(6) -0.004(6) C22 0.068(13) 0.033(9) 0.040(10) -0.003(8) 0.010(9) -0.024(9) C23 0.053(11) 0.022(8) 0.035(9) -0.010(6) 0.022(8) -0.012(7) C24 0.037(9) 0.024(8) 0.054(11) -0.020(7) 0.013(8) -0.014(7) C25 0.036(9) 0.026(8) 0.027(8) -0.007(6) 0.022(7) 0.001(7) C26 0.028(8) 0.033(9) 0.022(7) -0.002(6) 0.017(6) -0.015(6) C27 0.018(7) 0.015(6) 0.029(7) -0.014(6) 0.001(6) 0.010(6) C28 0.019(7) 0.031(8) 0.021(7) 0.005(6) 0.002(5) -0.019(6) C29 0.015(4) 0.017(4) 0.018(4) -0.001(3) 0.005(3) -0.003(3) C30 0.034(8) 0.017(7) 0.018(7) 0.008(6) 0.008(6) 0.001(6) C31 0.032(8) 0.016(7) 0.013(6) 0.004(6) 0.000(6) -0.007(6) C32 0.016(7) 0.024(8) 0.038(8) -0.011(6) 0.003(6) 0.011(6) C33 0.012(7) 0.022(7) 0.033(8) -0.017(6) 0.000(6) 0.011(6) C34 0.014(7) 0.032(9) 0.030(8) 0.006(6) -0.007(6) -0.008(6) C35 0.034(9) 0.023(8) 0.051(10) 0.005(7) -0.001(8) -0.020(7) C36 0.034(9) 0.033(9) 0.036(9) 0.006(7) 0.021(7) 0.000(8) C37 0.018(7) 0.016(7) 0.039(8) 0.003(6) 0.012(6) 0.001(6) C38 0.024(8) 0.024(8) 0.024(7) 0.017(6) 0.003(6) -0.004(6) C39 0.019(8) 0.028(8) 0.029(8) 0.023(6) 0.013(6) 0.000(6) C40 0.019(7) 0.049(10) 0.025(8) 0.017(7) -0.001(6) -0.007(7) C41 0.019(8) 0.027(9) 0.059(11) 0.020(8) -0.006(7) -0.002(7) C42 0.017(7) 0.026(8) 0.022(7) 0.010(6) 0.010(6) 0.011(6) C43 0.023(8) 0.026(8) 0.037(9) 0.002(7) 0.002(6) 0.007(7) C44 0.064(11) 0.022(8) 0.016(7) 0.001(6) -0.006(7) 0.016(8) C45 0.038(10) 0.056(11) 0.045(11) 0.016(9) -0.007(8) -0.026(9) C46 0.045(11) 0.073(14) 0.027(9) 0.019(9) 0.013(8) -0.017(10) C47 0.015(7) 0.006(6) 0.043(9) 0.003(6) 0.007(6) 0.004(5) C48 0.026(8) 0.027(8) 0.021(7) -0.009(7) -0.007(6) 0.013(7) C49 0.031(9) 0.044(10) 0.021(8) -0.002(7) 0.005(6) -0.005(8) C50 0.032(9) 0.050(11) 0.035(9) -0.022(8) 0.020(7) -0.004(8) C51 0.026(8) 0.022(8) 0.046(10) -0.019(7) 0.011(7) 0.005(7) C52 0.044(10) 0.017(8) 0.034(9) -0.004(6) 0.015(7) 0.011(7) O01 0.073(9) 0.070(9) 0.071(9) 0.000(3) 0.013(3) 0.000(3) C01 0.063(12) 0.062(12) 0.062(12) 0.000(3) 0.012(4) 0.000(3) C02 0.078(14) 0.077(14) 0.077(14) -0.001(3) 0.015(4) 0.001(3) C03 0.13(2) 0.13(2) 0.13(2) -0.001(3) 0.024(6) 0.000(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 C1 2.068(12) . ? Pt1 P1 2.182(4) . ? Pt1 Cl1 2.407(3) . ? Pt1 Cl2 2.510(3) . ? Pt1 Pt2 3.1521(7) . ? Pt2 C27 2.046(14) . ? Pt2 P2 2.180(4) . ? Pt2 Cl2 2.404(3) . ? Pt2 Cl1 2.509(3) . ? P1 C11 1.811(15) . ? P1 C21 1.819(14) . ? P1 C3 1.823(14) . ? P2 C37 1.804(15) . ? P2 C47 1.819(15) . ? P2 C29 1.848(13) . ? O1 C12 1.435(16) . ? O1 C4 1.469(17) . ? O2 C30 1.413(17) . ? O2 C38 1.423(17) . ? C1 C2 1.534(18) . ? C1 C6 1.55(2) . ? C2 C7 1.52(2) . ? C2 C3 1.53(2) . ? C3 C4 1.540(19) . ? C4 C5 1.54(2) . ? C5 C10 1.53(2) . ? C5 C7 1.56(2) . ? C5 C6 1.64(2) . ? C7 C8 1.55(2) . ? C7 C9 1.58(2) . ? C11 C16 1.55(2) . ? C11 C12 1.560(19) . ? C12 C13 1.53(2) . ? C13 C14 1.52(2) . ? C13 C20 1.53(2) . ? C13 C17 1.58(2) . ? C14 C15 1.58(2) . ? C15 C16 1.50(2) . ? C16 C17 1.52(2) . ? C17 C18 1.52(2) . ? C17 C19 1.58(2) . ? C21 C26 1.371(19) . ? C21 C22 1.40(2) . ? C22 C23 1.40(2) . ? C23 C24 1.38(2) . ? C24 C25 1.38(2) . ? C25 C26 1.41(2) . ? C27 C28 1.53(2) . ? C27 C32 1.54(2) . ? C28 C29 1.527(19) . ? C28 C33 1.612(19) . ? C29 C30 1.572(18) . ? C30 C31 1.54(2) . ? C31 C36 1.484(19) . ? C31 C33 1.557(18) . ? C31 C32 1.56(2) . ? C33 C35 1.51(2) . ? C33 C34 1.529(19) . ? C37 C38 1.570(19) . ? C37 C42 1.58(2) . ? C38 C39 1.55(2) . ? C39 C46 1.56(2) . ? C39 C43 1.57(2) . ? C39 C40 1.58(2) . ? C40 C41 1.59(2) . ? C41 C42 1.543(19) . ? C42 C43 1.53(2) . ? C43 C45 1.53(2) . ? C43 C44 1.55(2) . ? C47 C48 1.36(2) . ? C47 C52 1.428(19) . ? C48 C49 1.47(2) . ? C49 C50 1.36(3) . ? C50 C51 1.36(2) . ? C51 C52 1.36(2) . ? O01 C02 1.31(5) . ? C01 C02 1.520(5) . ? C02 C03 1.520(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Pt1 P1 83.2(4) . . ? C1 Pt1 Cl1 91.1(4) . . ? P1 Pt1 Cl1 170.41(13) . . ? C1 Pt1 Cl2 173.0(4) . . ? P1 Pt1 Cl2 101.96(12) . . ? Cl1 Pt1 Cl2 84.40(12) . . ? C1 Pt1 Pt2 131.2(4) . . ? P1 Pt1 Pt2 128.18(9) . . ? Cl1 Pt1 Pt2 51.57(8) . . ? Cl2 Pt1 Pt2 48.63(7) . . ? C27 Pt2 P2 83.4(4) . . ? C27 Pt2 Cl2 92.0(4) . . ? P2 Pt2 Cl2 169.55(13) . . ? C27 Pt2 Cl1 174.0(3) . . ? P2 Pt2 Cl1 100.88(13) . . ? Cl2 Pt2 Cl1 84.47(12) . . ? C27 Pt2 Pt1 131.6(4) . . ? P2 Pt2 Pt1 126.18(10) . . ? Cl2 Pt2 Pt1 51.60(8) . . ? Cl1 Pt2 Pt1 48.70(8) . . ? C11 P1 C21 103.2(7) . . ? C11 P1 C3 101.0(7) . . ? C21 P1 C3 108.2(6) . . ? C11 P1 Pt1 125.5(6) . . ? C21 P1 Pt1 112.3(5) . . ? C3 P1 Pt1 105.2(5) . . ? C37 P2 C47 102.6(6) . . ? C37 P2 C29 100.8(6) . . ? C47 P2 C29 107.4(6) . . ? C37 P2 Pt2 127.5(5) . . ? C47 P2 Pt2 111.4(4) . . ? C29 P2 Pt2 105.4(5) . . ? Pt1 Cl1 Pt2 79.73(10) . . ? Pt2 Cl2 Pt1 79.77(10) . . ? C12 O1 C4 110.6(10) . . ? C30 O2 C38 111.6(11) . . ? C2 C1 C6 107.1(12) . . ? C2 C1 Pt1 116.5(9) . . ? C6 C1 Pt1 106.0(10) . . ? C7 C2 C3 102.4(11) . . ? C7 C2 C1 101.3(12) . . ? C3 C2 C1 105.2(11) . . ? C2 C3 C4 104.1(11) . . ? C2 C3 P1 108.2(9) . . ? C4 C3 P1 114.8(10) . . ? O1 C4 C3 112.6(11) . . ? O1 C4 C5 108.4(12) . . ? C3 C4 C5 103.9(11) . . ? C10 C5 C4 115.3(13) . . ? C10 C5 C7 119.2(13) . . ? C4 C5 C7 99.2(12) . . ? C10 C5 C6 113.1(13) . . ? C4 C5 C6 106.9(12) . . ? C7 C5 C6 101.2(12) . . ? C1 C6 C5 99.9(12) . . ? C2 C7 C8 114.8(15) . . ? C2 C7 C5 96.0(12) . . ? C8 C7 C5 112.7(14) . . ? C2 C7 C9 115.6(13) . . ? C8 C7 C9 105.0(13) . . ? C5 C7 C9 113.0(15) . . ? C16 C11 C12 104.1(12) . . ? C16 C11 P1 122.5(10) . . ? C12 C11 P1 113.2(10) . . ? O1 C12 C13 112.2(12) . . ? O1 C12 C11 111.9(11) . . ? C13 C12 C11 101.6(12) . . ? C14 C13 C20 113.4(12) . . ? C14 C13 C12 106.0(13) . . ? C20 C13 C12 115.4(12) . . ? C14 C13 C17 102.6(12) . . ? C20 C13 C17 116.1(13) . . ? C12 C13 C17 101.7(11) . . ? C13 C14 C15 103.4(12) . . ? C16 C15 C14 102.0(11) . . ? C15 C16 C17 102.7(13) . . ? C15 C16 C11 105.6(12) . . ? C17 C16 C11 103.5(11) . . ? C16 C17 C18 118.3(12) . . ? C16 C17 C13 93.5(11) . . ? C18 C17 C13 117.0(13) . . ? C16 C17 C19 111.5(13) . . ? C18 C17 C19 104.1(13) . . ? C13 C17 C19 112.6(12) . . ? C26 C21 C22 119.4(13) . . ? C26 C21 P1 119.4(10) . . ? C22 C21 P1 121.1(11) . . ? C23 C22 C21 120.4(15) . . ? C24 C23 C22 118.8(16) . . ? C25 C24 C23 121.9(15) . . ? C24 C25 C26 118.6(14) . . ? C21 C26 C25 120.8(13) . . ? C28 C27 C32 104.4(12) . . ? C28 C27 Pt2 116.3(9) . . ? C32 C27 Pt2 111.4(9) . . ? C29 C28 C27 106.6(11) . . ? C29 C28 C33 100.6(10) . . ? C27 C28 C33 102.4(11) . . ? C28 C29 C30 103.9(11) . . ? C28 C29 P2 106.8(9) . . ? C30 C29 P2 110.5(9) . . ? O2 C30 C31 110.3(11) . . ? O2 C30 C29 115.2(12) . . ? C31 C30 C29 103.7(10) . . ? C36 C31 C30 112.9(12) . . ? C36 C31 C33 117.7(12) . . ? C30 C31 C33 101.5(11) . . ? C36 C31 C32 114.9(12) . . ? C30 C31 C32 107.1(11) . . ? C33 C31 C32 101.2(11) . . ? C27 C32 C31 104.2(11) . . ? C35 C33 C34 106.8(12) . . ? C35 C33 C31 116.5(13) . . ? C34 C33 C31 113.8(11) . . ? C35 C33 C28 114.0(12) . . ? C34 C33 C28 112.3(12) . . ? C31 C33 C28 93.2(10) . . ? C38 C37 C42 101.7(11) . . ? C38 C37 P2 112.1(9) . . ? C42 C37 P2 121.9(9) . . ? O2 C38 C39 112.1(12) . . ? O2 C38 C37 113.0(11) . . ? C39 C38 C37 103.8(11) . . ? C38 C39 C46 115.9(12) . . ? C38 C39 C43 103.4(10) . . ? C46 C39 C43 118.4(14) . . ? C38 C39 C40 103.1(12) . . ? C46 C39 C40 114.4(12) . . ? C43 C39 C40 99.2(10) . . ? C39 C40 C41 106.0(11) . . ? C42 C41 C40 98.9(12) . . ? C43 C42 C41 103.6(12) . . ? C43 C42 C37 106.9(11) . . ? C41 C42 C37 104.0(11) . . ? C45 C43 C42 114.1(14) . . ? C45 C43 C44 105.0(14) . . ? C42 C43 C44 115.1(12) . . ? C45 C43 C39 114.2(13) . . ? C42 C43 C39 94.2(11) . . ? C44 C43 C39 114.5(13) . . ? C48 C47 C52 119.7(13) . . ? C48 C47 P2 119.1(10) . . ? C52 C47 P2 121.1(11) . . ? C47 C48 C49 119.3(14) . . ? C50 C49 C48 119.2(15) . . ? C49 C50 C51 119.7(14) . . ? C50 C51 C52 123.8(15) . . ? C51 C52 C47 118.2(15) . . ? O01 C02 C01 123(4) . . ? O01 C02 C03 114(4) . . ? C01 C02 C03 123(5) . . ? _diffrn_measured_fraction_theta_max 0.954 _diffrn_reflns_theta_full 26.02 _diffrn_measured_fraction_theta_full 0.954 _refine_diff_density_max 2.740 _refine_diff_density_min -1.911 _refine_diff_density_rms 0.254 data_compound_9 _database_code_CSD 213241 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C52 H68 Cl2 O2 Pd2, 2(C7H8)' _chemical_formula_sum 'C66 H84 Cl2 O2 P2 Pd2' _chemical_formula_weight 1254.97 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 Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 15.8838(4) _cell_length_b 17.5364(5) _cell_length_c 25.2450(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7031.9(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 'all obs. reflections' _cell_measurement_theta_min 2.93 _cell_measurement_theta_max 27.45 _exptl_crystal_description 'irregular bloc' _exptl_crystal_colour yellow _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.185 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2608 _exptl_absorpt_coefficient_mu 0.670 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.740 _exptl_absorpt_correction_T_max 0.852 _exptl_absorpt_process_details 'SORTAV (Blessing, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Nonius kappa CCD area detector' _diffrn_measurement_method 'phi & omega scan to fill Ewald sphere' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29630 _diffrn_reflns_av_R_equivalents 0.0623 _diffrn_reflns_av_sigmaI/netI 0.0987 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 2.93 _diffrn_reflns_theta_max 27.45 _reflns_number_total 13557 _reflns_number_gt 10244 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Hooft, 1998)' _computing_cell_refinement 'HKL Scalepack, (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO & Scalepack, (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-96 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 for Windows (Farrugia, 1997)' _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. The complex contained one fully occupied, one half occupied and two quarter occupied toluene solvent molecules (two per asymmetric unit) in the lattice. These molecules were ridealised (phenyl ring C-C = 1.39 A, phenyl-methyl = 1.52 A) and and refined with ISOR = 0.01 restaint for all solvent atoms. ; _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^)+(0.0911P)^2^+5.6226P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment 'calculated positions, riding model' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.06(4) _refine_ls_number_reflns 13557 _refine_ls_number_parameters 761 _refine_ls_number_restraints 129 _refine_ls_R_factor_all 0.0924 _refine_ls_R_factor_gt 0.0593 _refine_ls_wR_factor_ref 0.1697 _refine_ls_wR_factor_gt 0.1501 _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_restrained_S_all 1.057 _refine_ls_shift/su_max 0.010 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.50323(4) 0.35495(3) 0.084243(19) 0.02178(14) Uani 1 1 d . . . Pd2 Pd 0.37723(4) 0.21422(3) 0.17050(2) 0.02169(14) Uani 1 1 d . . . Cl1 Cl 0.59047(12) 0.35592(12) 0.00837(7) 0.0322(4) Uani 1 1 d . . . Cl2 Cl 0.39899(14) 0.13044(10) 0.24215(7) 0.0340(5) Uani 1 1 d . . . P1 P 0.54405(13) 0.46296(11) 0.13014(7) 0.0234(4) Uani 1 1 d . . . P2 P 0.26069(13) 0.16436(10) 0.12705(7) 0.0231(4) Uani 1 1 d . . . O1 O 0.6031(3) 0.3823(3) 0.22018(18) 0.0220(11) Uani 1 1 d . . . O2 O 0.3485(3) 0.1281(3) 0.03376(19) 0.0256(12) Uani 1 1 d . . . C1 C 0.6439(5) 0.4913(4) 0.1628(3) 0.0240(17) Uani 1 1 d . . . H1 H 0.6385 0.5464 0.1727 0.029 Uiso 1 1 calc R . . C2 C 0.7280(5) 0.4821(4) 0.1329(3) 0.0293(18) Uani 1 1 d . . . H2 H 0.7240 0.4893 0.0937 0.035 Uiso 1 1 calc R . . C3 C 0.7881(5) 0.5369(4) 0.1608(3) 0.0314(19) Uani 1 1 d . . . H3A H 0.7624 0.5880 0.1653 0.038 Uiso 1 1 calc R . . H3B H 0.8417 0.5422 0.1410 0.038 Uiso 1 1 calc R . . C4 C 0.8018(5) 0.4967(5) 0.2151(3) 0.0325(19) Uani 1 1 d . . . H4A H 0.8624 0.4868 0.2215 0.039 Uiso 1 1 calc R . . H4B H 0.7795 0.5281 0.2445 0.039 Uiso 1 1 calc R . . C5 C 0.7522(5) 0.4206(4) 0.2101(3) 0.0311(19) Uani 1 1 d . . . C6 C 0.6594(5) 0.4455(4) 0.2153(3) 0.0229(16) Uani 1 1 d . . . H6 H 0.6529 0.4802 0.2465 0.027 Uiso 1 1 calc R . . C7 C 0.7621(5) 0.4038(4) 0.1502(3) 0.0223(16) Uani 1 1 d . . . C8 C 0.8533(6) 0.3900(5) 0.1333(3) 0.038(2) Uani 1 1 d . . . H8A H 0.8555 0.3813 0.0950 0.057 Uiso 1 1 calc R . . H8B H 0.8755 0.3452 0.1518 0.057 Uiso 1 1 calc R . . H8C H 0.8875 0.4347 0.1422 0.057 Uiso 1 1 calc R . . C9 C 0.7131(5) 0.3332(4) 0.1303(3) 0.0306(18) Uani 1 1 d . . . H9A H 0.7178 0.3298 0.0917 0.046 Uiso 1 1 calc R . . H9B H 0.6537 0.3379 0.1403 0.046 Uiso 1 1 calc R . . H9C H 0.7368 0.2871 0.1464 0.046 Uiso 1 1 calc R . . C10 C 0.7774(5) 0.3588(5) 0.2496(3) 0.0363(19) Uani 1 1 d . . . H10A H 0.7438 0.3128 0.2432 0.055 Uiso 1 1 calc R . . H10B H 0.7673 0.3770 0.2857 0.055 Uiso 1 1 calc R . . H10C H 0.8373 0.3468 0.2452 0.055 Uiso 1 1 calc R . . C11 C 0.5208(5) 0.4093(4) 0.2333(3) 0.031(2) Uani 1 1 d . . . H11 H 0.5243 0.4411 0.2661 0.037 Uiso 1 1 calc R . . C12 C 0.4749(5) 0.4571(4) 0.1880(3) 0.0249(17) Uani 1 1 d . . . H12 H 0.4608 0.5093 0.2011 0.030 Uiso 1 1 calc R . . C13 C 0.3912(5) 0.4085(4) 0.1794(3) 0.0268(17) Uani 1 1 d . . . H13 H 0.3443 0.4357 0.1609 0.032 Uiso 1 1 calc R . . C14 C 0.4240(4) 0.3341(4) 0.1512(3) 0.0186(15) Uani 1 1 d . . . C15 C 0.4688(5) 0.2936(4) 0.1928(2) 0.0202(15) Uani 1 1 d . . . H15 H 0.5278 0.2788 0.1836 0.024 Uiso 1 1 calc R . . C16 C 0.4605(5) 0.3408(4) 0.2435(3) 0.0245(16) Uani 1 1 d . . . C17 C 0.3720(5) 0.3820(4) 0.2371(3) 0.0263(17) Uani 1 1 d . . . C18 C 0.2952(5) 0.3311(4) 0.2418(3) 0.0283(18) Uani 1 1 d . . . H18A H 0.3002 0.2993 0.2736 0.042 Uiso 1 1 calc R . . H18B H 0.2912 0.2983 0.2105 0.042 Uiso 1 1 calc R . . H18C H 0.2445 0.3627 0.2444 0.042 Uiso 1 1 calc R . . C19 C 0.3593(6) 0.4479(4) 0.2760(3) 0.036(2) Uani 1 1 d . . . H19A H 0.3100 0.4778 0.2654 0.054 Uiso 1 1 calc R . . H19B H 0.4093 0.4807 0.2759 0.054 Uiso 1 1 calc R . . H19C H 0.3505 0.4275 0.3117 0.054 Uiso 1 1 calc R . . C20 C 0.4780(5) 0.3001(4) 0.2945(3) 0.0250(17) Uani 1 1 d . . . H20A H 0.4421 0.2548 0.2971 0.037 Uiso 1 1 calc R . . H20B H 0.4662 0.3342 0.3244 0.037 Uiso 1 1 calc R . . H20C H 0.5373 0.2846 0.2956 0.037 Uiso 1 1 calc R . . C21 C 0.5149(5) 0.5501(4) 0.0952(3) 0.0261(17) Uani 1 1 d . . . C22 C 0.4911(6) 0.6172(4) 0.1211(3) 0.0344(19) Uani 1 1 d . . . H22 H 0.4921 0.6185 0.1587 0.041 Uiso 1 1 calc R . . C23 C 0.4663(7) 0.6813(5) 0.0940(4) 0.056(3) Uani 1 1 d . . . H23 H 0.4467 0.7256 0.1119 0.067 Uiso 1 1 calc R . . C24 C 0.4713(8) 0.6780(5) 0.0393(4) 0.065(4) Uani 1 1 d . . . H24 H 0.4588 0.7226 0.0196 0.078 Uiso 1 1 calc R . . C25 C 0.4932(8) 0.6135(5) 0.0125(3) 0.057(3) Uani 1 1 d . . . H25 H 0.4922 0.6131 -0.0251 0.068 Uiso 1 1 calc R . . C26 C 0.5169(6) 0.5491(5) 0.0398(3) 0.037(2) Uani 1 1 d . . . H26 H 0.5344 0.5047 0.0213 0.045 Uiso 1 1 calc R . . C27 C 0.2384(5) 0.0752(4) 0.0905(3) 0.0299(18) Uani 1 1 d . . . H27 H 0.1769 0.0753 0.0819 0.036 Uiso 1 1 calc R . . C28 C 0.2582(6) -0.0034(4) 0.1187(3) 0.0318(19) Uani 1 1 d . . . H28 H 0.2506 -0.0035 0.1580 0.038 Uiso 1 1 calc R . . C29 C 0.2026(6) -0.0604(4) 0.0884(4) 0.040(2) Uani 1 1 d . . . H29A H 0.1440 -0.0415 0.0856 0.048 Uiso 1 1 calc R . . H29B H 0.2023 -0.1108 0.1061 0.048 Uiso 1 1 calc R . . C30 C 0.2445(6) -0.0652(4) 0.0332(3) 0.038(2) Uani 1 1 d . . . H30A H 0.2060 -0.0465 0.0052 0.045 Uiso 1 1 calc R . . H30B H 0.2613 -0.1183 0.0249 0.045 Uiso 1 1 calc R . . C31 C 0.3231(5) -0.0126(4) 0.0383(3) 0.0318(19) Uani 1 1 d . . . C32 C 0.2862(5) 0.0687(4) 0.0377(3) 0.0256(17) Uani 1 1 d . . . H32 H 0.2455 0.0735 0.0076 0.031 Uiso 1 1 calc R . . C33 C 0.3454(5) -0.0240(4) 0.0998(3) 0.0301(19) Uani 1 1 d . . . C34 C 0.4170(6) 0.0260(5) 0.1188(3) 0.036(2) Uani 1 1 d . . . H34A H 0.4009 0.0798 0.1156 0.054 Uiso 1 1 calc R . . H34B H 0.4672 0.0164 0.0972 0.054 Uiso 1 1 calc R . . H34C H 0.4294 0.0143 0.1560 0.054 Uiso 1 1 calc R . . C35 C 0.3705(7) -0.1076(5) 0.1120(4) 0.043(2) Uani 1 1 d . . . H35A H 0.3723 -0.1152 0.1504 0.064 Uiso 1 1 calc R . . H35B H 0.4262 -0.1182 0.0969 0.064 Uiso 1 1 calc R . . H35C H 0.3290 -0.1423 0.0964 0.064 Uiso 1 1 calc R . . C36 C 0.3922(5) -0.0266(5) -0.0026(3) 0.038(2) Uani 1 1 d . . . H36A H 0.3684 -0.0222 -0.0383 0.057 Uiso 1 1 calc R . . H36B H 0.4155 -0.0779 0.0023 0.057 Uiso 1 1 calc R . . H36C H 0.4369 0.0113 0.0019 0.057 Uiso 1 1 calc R . . C37 C 0.3068(5) 0.1987(4) 0.0230(3) 0.0241(17) Uani 1 1 d . . . H37 H 0.2698 0.1931 -0.0089 0.029 Uiso 1 1 calc R . . C38 C 0.2550(5) 0.2307(4) 0.0701(3) 0.0261(17) Uani 1 1 d . . . H38 H 0.1950 0.2372 0.0591 0.031 Uiso 1 1 calc R . . C39 C 0.2952(5) 0.3111(4) 0.0808(3) 0.0238(16) Uani 1 1 d . . . H39 H 0.2594 0.3480 0.1009 0.029 Uiso 1 1 calc R . . C40 C 0.3817(5) 0.2924(4) 0.1057(2) 0.0206(15) Uani 1 1 d . . . C41 C 0.4303(5) 0.2604(4) 0.0617(3) 0.0219(16) Uani 1 1 d . . . H41 H 0.4567 0.2097 0.0690 0.026 Uiso 1 1 calc R . . C42 C 0.3721(5) 0.2626(4) 0.0136(3) 0.0258(17) Uani 1 1 d . . . C43 C 0.3158(5) 0.3336(4) 0.0226(3) 0.0256(18) Uani 1 1 d . . . C44 C 0.2386(6) 0.3376(5) -0.0137(3) 0.038(2) Uani 1 1 d . . . H44A H 0.2570 0.3410 -0.0507 0.057 Uiso 1 1 calc R . . H44B H 0.2051 0.3828 -0.0048 0.057 Uiso 1 1 calc R . . H44C H 0.2042 0.2917 -0.0089 0.057 Uiso 1 1 calc R . . C45 C 0.3592(5) 0.4132(4) 0.0177(3) 0.0278(18) Uani 1 1 d . . . H45A H 0.3848 0.4182 -0.0174 0.042 Uiso 1 1 calc R . . H45B H 0.4029 0.4179 0.0449 0.042 Uiso 1 1 calc R . . H45C H 0.3171 0.4535 0.0226 0.042 Uiso 1 1 calc R . . C46 C 0.4165(6) 0.2572(5) -0.0401(3) 0.034(2) Uani 1 1 d . . . H46A H 0.4559 0.2999 -0.0438 0.051 Uiso 1 1 calc R . . H46B H 0.3746 0.2594 -0.0685 0.051 Uiso 1 1 calc R . . H46C H 0.4474 0.2090 -0.0422 0.051 Uiso 1 1 calc R . . C47 C 0.1649(5) 0.1780(4) 0.1650(3) 0.0263(17) Uani 1 1 d . . . C48 C 0.1688(5) 0.1783(4) 0.2205(3) 0.0278(18) Uani 1 1 d . . . H48 H 0.2211 0.1695 0.2377 0.033 Uiso 1 1 calc R . . C49 C 0.0979(6) 0.1913(5) 0.2502(3) 0.041(2) Uani 1 1 d . . . H49 H 0.1028 0.1929 0.2876 0.049 Uiso 1 1 calc R . . C50 C 0.0210(5) 0.2019(5) 0.2278(3) 0.041(2) Uani 1 1 d . . . H50 H -0.0272 0.2106 0.2492 0.049 Uiso 1 1 calc R . . C51 C 0.0140(6) 0.1996(5) 0.1716(4) 0.048(2) Uani 1 1 d . . . H51 H -0.0392 0.2059 0.1550 0.058 Uiso 1 1 calc R . . C52 C 0.0864(5) 0.1882(5) 0.1411(3) 0.034(2) Uani 1 1 d . . . H52 H 0.0821 0.1874 0.1036 0.040 Uiso 1 1 calc R . . C53 C 0.6398(3) 0.1504(3) 0.2347(2) 0.042(2) Uani 1 1 d G . . H53 H 0.5820 0.1624 0.2395 0.051 Uiso 1 1 calc R . . C54 C 0.6938(5) 0.1491(4) 0.27799(19) 0.063(3) Uani 1 1 d G . . H54 H 0.6729 0.1601 0.3124 0.076 Uiso 1 1 calc R . . C55 C 0.7785(4) 0.1316(4) 0.2710(3) 0.080(4) Uani 1 1 d G . . H55 H 0.8154 0.1307 0.3006 0.096 Uiso 1 1 calc R . . C56 C 0.8091(3) 0.1155(4) 0.2206(3) 0.061(3) Uani 1 1 d G . . H56 H 0.8669 0.1036 0.2158 0.073 Uiso 1 1 calc R . . C57 C 0.7551(4) 0.1168(4) 0.1773(2) 0.055(3) Uani 1 1 d G . . H57 H 0.7760 0.1058 0.1429 0.066 Uiso 1 1 calc R . . C58 C 0.6704(4) 0.1343(3) 0.1843(2) 0.044(2) Uani 1 1 d G . . C59 C 0.6110(6) 0.1353(6) 0.1384(4) 0.050(2) Uani 1 1 d . . . H59A H 0.6241 0.1788 0.1155 0.075 Uiso 1 1 calc R . . H59B H 0.5531 0.1399 0.1514 0.075 Uiso 1 1 calc R . . H59C H 0.6169 0.0879 0.1182 0.075 Uiso 1 1 calc R . . C60 C 0.0415(9) 0.5216(7) 0.1808(6) 0.054(5) Uani 0.50 1 d PGU . . H60 H 0.0261 0.5615 0.2043 0.065 Uiso 0.50 1 calc PR . . C61 C 0.0427(9) 0.5344(6) 0.1265(6) 0.069(6) Uani 0.50 1 d PGU . . H61 H 0.0281 0.5832 0.1129 0.083 Uiso 0.50 1 calc PR . . C62 C 0.0653(10) 0.4760(9) 0.0922(4) 0.085(8) Uani 0.50 1 d PGU . . H62 H 0.0661 0.4847 0.0550 0.102 Uiso 0.50 1 calc PR . . C63 C 0.0866(8) 0.4047(8) 0.1121(5) 0.061(6) Uani 0.50 1 d PGU . . H63 H 0.1020 0.3647 0.0886 0.073 Uiso 0.50 1 calc PR . . C64 C 0.0854(8) 0.3918(6) 0.1664(6) 0.043(4) Uani 0.50 1 d PGU . . H64 H 0.0999 0.3431 0.1801 0.052 Uiso 0.50 1 calc PR . . C65 C 0.0628(9) 0.4503(8) 0.2008(4) 0.075(7) Uani 0.50 1 d PGDU . . C66 C 0.045(3) 0.443(3) 0.2590(6) 0.20(2) Uani 0.50 1 d PDU . . H66A H 0.0051 0.4012 0.2649 0.305 Uiso 0.50 1 calc PR . . H66B H 0.0211 0.4907 0.2723 0.305 Uiso 0.50 1 calc PR . . H66C H 0.0977 0.4319 0.2779 0.305 Uiso 0.50 1 calc PR . . C67 C 0.2092(13) 0.6247(11) 0.0264(6) 0.017(6) Uani 0.25 1 d PGDU . . C68 C 0.2062(15) 0.7033(10) 0.0196(7) 0.041(8) Uani 0.25 1 d PGU . . H68 H 0.2291 0.7361 0.0459 0.049 Uiso 0.25 1 calc PR . . C69 C 0.1697(18) 0.7340(9) -0.0256(9) 0.072(13) Uani 0.25 1 d PGU . . H69 H 0.1676 0.7878 -0.0303 0.086 Uiso 0.25 1 calc PR . . C70 C 0.1362(15) 0.6861(12) -0.0641(7) 0.042(8) Uani 0.25 1 d PGU . . H70 H 0.1113 0.7071 -0.0951 0.051 Uiso 0.25 1 calc PR . . C71 C 0.1393(14) 0.6075(11) -0.0573(7) 0.035(8) Uani 0.25 1 d PGU . . H71 H 0.1164 0.5748 -0.0836 0.042 Uiso 0.25 1 calc PR . . C72 C 0.1758(16) 0.5768(8) -0.0121(8) 0.050(10) Uani 0.25 1 d PGU . . H72 H 0.1778 0.5231 -0.0074 0.060 Uiso 0.25 1 calc PR . . C73 C 0.257(2) 0.5994(18) 0.0746(9) 0.037(8) Uani 0.25 1 d PDU . . H73A H 0.3144 0.5862 0.0647 0.056 Uiso 0.25 1 calc PR . . H73B H 0.2288 0.5546 0.0899 0.056 Uiso 0.25 1 calc PR . . H73C H 0.2574 0.6408 0.1007 0.056 Uiso 0.25 1 calc PR . . C74 C 0.3573(19) 0.7460(18) -0.0946(12) 0.087(16) Uani 0.25 1 d PGDU . . C75 C 0.3419(15) 0.6739(19) -0.1154(13) 0.068(13) Uani 0.25 1 d PGU . . H75 H 0.2871 0.6524 -0.1131 0.081 Uiso 0.25 1 calc PR . . C76 C 0.407(2) 0.6332(14) -0.1393(12) 0.073(13) Uani 0.25 1 d PGU . . H76 H 0.3960 0.5840 -0.1535 0.088 Uiso 0.25 1 calc PR . . C77 C 0.4868(17) 0.6647(18) -0.1426(12) 0.065(11) Uani 0.25 1 d PGU . . H77 H 0.5310 0.6369 -0.1590 0.078 Uiso 0.25 1 calc PR . . C78 C 0.5022(17) 0.7367(19) -0.1219(13) 0.12(2) Uani 0.25 1 d PGU . . H78 H 0.5570 0.7582 -0.1242 0.141 Uiso 0.25 1 calc PR . . C79 C 0.438(2) 0.7774(15) -0.0979(13) 0.079(14) Uani 0.25 1 d PGU . . H79 H 0.4481 0.8267 -0.0838 0.095 Uiso 0.25 1 calc PR . . C80 C 0.267(2) 0.770(4) -0.089(3) 0.11(2) Uani 0.25 1 d PDU . . H80A H 0.2485 0.7955 -0.1213 0.167 Uiso 0.25 1 calc PR . . H80B H 0.2625 0.8061 -0.0589 0.167 Uiso 0.25 1 calc PR . . H80C H 0.2321 0.7256 -0.0818 0.167 Uiso 0.25 1 calc PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.0268(3) 0.0180(3) 0.0206(2) -0.0019(2) 0.0017(3) -0.0024(3) Pd2 0.0267(3) 0.0167(3) 0.0217(2) 0.0011(2) -0.0010(3) -0.0019(2) Cl1 0.0301(11) 0.0384(11) 0.0281(9) -0.0042(8) 0.0074(8) -0.0058(9) Cl2 0.0492(14) 0.0229(10) 0.0298(9) 0.0082(7) -0.0075(9) -0.0057(9) P1 0.0298(12) 0.0174(10) 0.0230(9) -0.0022(7) 0.0020(9) -0.0020(8) P2 0.0261(11) 0.0202(10) 0.0229(8) 0.0019(7) -0.0023(8) -0.0022(8) O1 0.024(3) 0.017(3) 0.024(2) -0.0014(19) 0.002(2) -0.001(2) O2 0.030(3) 0.020(3) 0.028(2) -0.002(2) -0.001(2) -0.001(2) C1 0.028(4) 0.022(4) 0.023(3) -0.007(3) -0.004(3) -0.006(3) C2 0.041(5) 0.023(4) 0.024(4) -0.002(3) -0.004(4) -0.003(4) C3 0.032(5) 0.027(4) 0.036(4) -0.006(3) 0.008(4) -0.008(4) C4 0.032(5) 0.028(4) 0.037(4) -0.010(3) -0.005(4) -0.007(4) C5 0.032(5) 0.025(4) 0.036(4) -0.012(3) 0.006(4) -0.005(4) C6 0.027(4) 0.015(4) 0.027(4) -0.007(3) -0.001(3) -0.004(3) C7 0.014(4) 0.027(4) 0.025(3) -0.003(3) -0.002(3) -0.002(3) C8 0.046(6) 0.032(5) 0.037(4) -0.003(4) -0.001(4) -0.005(4) C9 0.027(5) 0.025(4) 0.039(4) -0.005(3) 0.002(4) -0.004(3) C10 0.035(5) 0.031(5) 0.043(5) 0.002(4) -0.002(4) 0.002(4) C11 0.053(6) 0.016(4) 0.023(3) -0.008(3) 0.003(4) -0.004(4) C12 0.034(5) 0.014(4) 0.026(3) -0.001(3) 0.010(3) 0.000(3) C13 0.042(5) 0.014(3) 0.024(4) 0.001(3) 0.000(4) -0.001(3) C14 0.014(4) 0.022(4) 0.020(3) 0.001(3) 0.007(3) -0.001(3) C15 0.022(4) 0.020(4) 0.018(3) -0.001(3) 0.003(3) -0.010(3) C16 0.032(4) 0.017(4) 0.025(3) 0.004(3) -0.003(3) -0.001(3) C17 0.032(5) 0.025(4) 0.022(3) -0.006(3) -0.002(4) -0.003(4) C18 0.029(5) 0.028(4) 0.028(4) -0.005(3) 0.011(4) -0.007(3) C19 0.057(6) 0.022(4) 0.029(4) -0.004(3) 0.011(4) 0.003(4) C20 0.032(5) 0.023(4) 0.020(3) -0.002(3) 0.002(3) -0.002(3) C21 0.027(5) 0.025(4) 0.027(4) -0.002(3) -0.007(3) -0.004(3) C22 0.043(5) 0.031(4) 0.029(4) 0.004(3) -0.004(4) -0.005(4) C23 0.095(9) 0.026(5) 0.046(5) -0.003(4) -0.014(5) 0.016(5) C24 0.122(11) 0.035(6) 0.040(5) 0.018(4) -0.027(6) 0.007(6) C25 0.108(9) 0.025(5) 0.036(4) 0.011(3) -0.007(6) 0.004(6) C26 0.054(6) 0.029(4) 0.030(4) 0.002(3) 0.003(4) -0.004(4) C27 0.032(5) 0.021(4) 0.037(4) -0.001(3) -0.012(4) -0.006(3) C28 0.050(6) 0.016(4) 0.030(4) 0.004(3) 0.002(4) -0.004(4) C29 0.046(6) 0.021(4) 0.051(5) 0.001(4) 0.003(5) -0.011(4) C30 0.052(6) 0.018(4) 0.044(5) -0.007(3) -0.007(4) -0.003(4) C31 0.043(5) 0.019(4) 0.033(4) -0.003(3) -0.011(4) 0.007(4) C32 0.032(5) 0.019(4) 0.026(4) 0.001(3) -0.009(3) -0.003(3) C33 0.033(5) 0.017(4) 0.040(4) 0.009(3) -0.005(4) 0.001(3) C34 0.044(5) 0.028(5) 0.036(4) -0.003(3) -0.005(4) 0.009(4) C35 0.054(6) 0.025(4) 0.050(5) 0.011(4) -0.010(5) 0.001(4) C36 0.039(6) 0.035(5) 0.041(4) -0.011(4) 0.001(4) 0.007(4) C37 0.026(4) 0.026(4) 0.020(3) 0.002(3) -0.004(3) -0.004(3) C38 0.025(4) 0.024(4) 0.029(4) -0.001(3) -0.007(3) -0.006(3) C39 0.030(4) 0.018(4) 0.024(3) 0.000(3) -0.001(3) -0.005(3) C40 0.027(4) 0.014(3) 0.021(3) 0.002(3) 0.000(3) -0.007(3) C41 0.034(5) 0.011(3) 0.021(3) 0.001(3) -0.002(3) -0.001(3) C42 0.033(5) 0.023(4) 0.022(3) 0.001(3) 0.000(4) -0.004(3) C43 0.034(5) 0.022(4) 0.021(3) 0.007(3) -0.003(3) -0.001(3) C44 0.048(6) 0.030(5) 0.036(4) 0.006(3) -0.013(4) -0.004(4) C45 0.023(5) 0.033(4) 0.028(4) 0.006(3) -0.006(3) -0.003(3) C46 0.040(5) 0.037(5) 0.026(4) 0.002(3) 0.000(4) -0.014(4) C47 0.032(5) 0.021(4) 0.026(4) 0.004(3) 0.006(4) -0.002(3) C48 0.030(5) 0.027(4) 0.026(4) 0.004(3) -0.003(4) -0.005(3) C49 0.056(7) 0.043(5) 0.025(4) -0.002(3) 0.000(4) -0.004(4) C50 0.027(5) 0.054(6) 0.042(5) 0.002(4) 0.017(4) -0.005(4) C51 0.030(5) 0.060(6) 0.054(5) 0.005(5) 0.004(5) 0.004(4) C52 0.032(5) 0.041(5) 0.028(4) 0.004(3) -0.007(4) -0.003(4) C53 0.048(6) 0.022(4) 0.056(5) 0.000(4) -0.008(5) 0.000(4) C54 0.079(9) 0.058(7) 0.053(6) 0.001(5) -0.009(6) 0.006(7) C55 0.074(10) 0.076(9) 0.091(10) 0.027(7) -0.023(8) -0.010(7) C56 0.041(7) 0.066(8) 0.075(8) 0.034(6) 0.002(6) -0.002(5) C57 0.042(6) 0.052(6) 0.070(7) 0.014(5) 0.007(6) -0.005(5) C58 0.057(7) 0.019(4) 0.055(6) 0.010(4) -0.005(5) -0.005(4) C59 0.050(6) 0.043(6) 0.057(6) -0.003(4) -0.003(5) 0.009(5) C60 0.038(8) 0.052(8) 0.072(9) -0.010(7) -0.001(7) -0.012(7) C61 0.048(9) 0.066(10) 0.094(10) -0.002(8) -0.010(8) -0.008(8) C62 0.072(11) 0.094(11) 0.089(11) 0.014(9) 0.001(9) -0.015(9) C63 0.037(8) 0.064(9) 0.082(10) -0.011(8) 0.006(8) 0.006(7) C64 0.029(7) 0.040(7) 0.061(8) -0.011(7) -0.002(7) 0.006(6) C65 0.069(10) 0.074(10) 0.082(10) -0.011(8) -0.005(8) -0.021(8) C66 0.20(2) 0.20(2) 0.21(2) -0.006(10) -0.015(10) -0.006(10) C67 0.015(9) 0.022(9) 0.014(8) 0.003(7) -0.008(7) 0.008(8) C68 0.039(12) 0.042(12) 0.043(11) -0.016(9) 0.007(9) -0.007(9) C69 0.073(16) 0.060(15) 0.082(16) -0.004(9) 0.001(10) 0.004(10) C70 0.043(12) 0.039(11) 0.045(11) -0.005(8) -0.020(9) 0.016(9) C71 0.031(11) 0.037(11) 0.036(10) 0.000(8) 0.004(9) -0.015(9) C72 0.048(13) 0.042(12) 0.060(13) 0.001(9) -0.002(9) 0.003(9) C73 0.039(11) 0.041(11) 0.031(10) -0.009(8) 0.000(9) 0.002(9) C74 0.089(18) 0.095(18) 0.075(17) 0.020(10) 0.001(10) -0.002(10) C75 0.067(15) 0.071(15) 0.065(15) 0.014(9) 0.000(10) 0.013(9) C76 0.074(16) 0.077(16) 0.069(15) 0.007(10) -0.013(10) 0.004(10) C77 0.074(15) 0.066(14) 0.056(13) 0.015(9) -0.005(9) 0.009(10) C78 0.12(2) 0.12(2) 0.11(2) 0.015(10) -0.010(10) 0.000(10) C79 0.089(17) 0.078(16) 0.071(16) 0.012(10) -0.008(10) 0.003(10) C80 0.12(2) 0.11(2) 0.10(2) 0.007(10) 0.004(10) -0.003(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 C41 2.100(7) . ? Pd1 C14 2.138(6) . ? Pd1 C40 2.286(7) . ? Pd1 P1 2.3131(19) . ? Pd1 Cl1 2.3641(18) . ? Pd2 C15 2.090(7) . ? Pd2 C40 2.134(6) . ? Pd2 C14 2.282(7) . ? Pd2 P2 2.323(2) . ? Pd2 Cl2 2.3559(18) . ? P1 C21 1.824(8) . ? P1 C12 1.830(7) . ? P1 C1 1.856(7) . ? P2 C47 1.813(8) . ? P2 C27 1.849(7) . ? P2 C38 1.851(7) . ? O1 C11 1.429(10) . ? O1 C6 1.431(8) . ? O2 C37 1.430(9) . ? O2 C32 1.439(9) . ? C1 C2 1.542(11) . ? C1 C6 1.570(10) . ? C2 C3 1.527(10) . ? C2 C7 1.540(10) . ? C3 C4 1.559(11) . ? C4 C5 1.554(11) . ? C5 C10 1.527(11) . ? C5 C6 1.542(11) . ? C5 C7 1.548(10) . ? C7 C8 1.530(12) . ? C7 C9 1.546(10) . ? C11 C16 1.558(10) . ? C11 C12 1.594(10) . ? C12 C13 1.593(11) . ? C13 C17 1.560(9) . ? C13 C14 1.576(9) . ? C14 C15 1.454(9) . ? C14 C40 1.517(9) . ? C15 C16 1.530(9) . ? C16 C20 1.499(9) . ? C16 C17 1.589(11) . ? C17 C18 1.516(10) . ? C17 C19 1.531(9) . ? C21 C22 1.397(11) . ? C21 C26 1.399(10) . ? C22 C23 1.374(11) . ? C23 C24 1.384(13) . ? C24 C25 1.362(13) . ? C25 C26 1.375(11) . ? C27 C32 1.540(11) . ? C27 C28 1.582(10) . ? C28 C33 1.509(12) . ? C28 C29 1.537(11) . ? C29 C30 1.546(12) . ? C30 C31 1.557(12) . ? C31 C36 1.527(12) . ? C31 C32 1.543(10) . ? C31 C33 1.603(11) . ? C33 C34 1.515(11) . ? C33 C35 1.552(10) . ? C37 C42 1.546(10) . ? C37 C38 1.552(10) . ? C38 C39 1.571(10) . ? C39 C40 1.546(11) . ? C39 C43 1.555(10) . ? C40 C41 1.464(9) . ? C41 C42 1.529(10) . ? C42 C46 1.529(10) . ? C42 C43 1.550(10) . ? C43 C44 1.532(11) . ? C43 C45 1.562(10) . ? C47 C52 1.398(11) . ? C47 C48 1.402(10) . ? C48 C49 1.372(12) . ? C49 C50 1.359(12) . ? C50 C51 1.423(12) . ? C51 C52 1.398(12) . ? C53 C54 1.3900 . ? C53 C58 1.3900 . ? C54 C55 1.3900 . ? C55 C56 1.3900 . ? C56 C57 1.3900 . ? C57 C58 1.3900 . ? C58 C59 1.495(10) . ? C60 C61 1.3900 . ? C60 C65 1.3900 . ? C61 C62 1.3900 . ? C62 C63 1.3900 . ? C63 C64 1.3900 . ? C64 C65 1.3900 . ? C65 C66 1.501(5) . ? C67 C68 1.3900 . ? C67 C72 1.3900 . ? C67 C73 1.497(5) . ? C68 C69 1.3900 . ? C69 C70 1.3900 . ? C70 C71 1.3900 . ? C71 C72 1.3900 . ? C74 C75 1.3900 . ? C74 C79 1.3900 . ? C74 C80 1.500(5) . ? C75 C76 1.3900 . ? C76 C77 1.3900 . ? C77 C78 1.3900 . ? C78 C79 1.3900 . ? 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 C41 Pd1 C14 75.8(3) . . ? C41 Pd1 C40 38.7(2) . . ? C14 Pd1 C40 39.9(2) . . ? C41 Pd1 P1 159.4(2) . . ? C14 Pd1 P1 84.81(19) . . ? C40 Pd1 P1 120.73(17) . . ? C41 Pd1 Cl1 96.3(2) . . ? C14 Pd1 Cl1 170.52(19) . . ? C40 Pd1 Cl1 133.68(16) . . ? P1 Pd1 Cl1 103.63(7) . . ? C15 Pd2 C40 75.9(3) . . ? C15 Pd2 C14 38.5(2) . . ? C40 Pd2 C14 40.0(2) . . ? C15 Pd2 P2 158.8(2) . . ? C40 Pd2 P2 84.62(19) . . ? C14 Pd2 P2 120.34(18) . . ? C15 Pd2 Cl2 96.11(19) . . ? C40 Pd2 Cl2 169.6(2) . . ? C14 Pd2 Cl2 133.70(18) . . ? P2 Pd2 Cl2 104.17(7) . . ? C21 P1 C12 106.3(3) . . ? C21 P1 C1 101.9(3) . . ? C12 P1 C1 100.0(3) . . ? C21 P1 Pd1 111.9(2) . . ? C12 P1 Pd1 100.7(2) . . ? C1 P1 Pd1 133.0(3) . . ? C47 P2 C27 102.4(4) . . ? C47 P2 C38 106.7(4) . . ? C27 P2 C38 97.8(3) . . ? C47 P2 Pd2 111.7(3) . . ? C27 P2 Pd2 134.9(3) . . ? C38 P2 Pd2 99.7(2) . . ? C11 O1 C6 109.6(5) . . ? C37 O2 C32 108.7(5) . . ? C2 C1 C6 102.9(6) . . ? C2 C1 P1 119.6(5) . . ? C6 C1 P1 111.9(5) . . ? C3 C2 C7 102.1(6) . . ? C3 C2 C1 104.5(6) . . ? C7 C2 C1 105.0(6) . . ? C2 C3 C4 102.0(6) . . ? C5 C4 C3 104.2(6) . . ? C10 C5 C6 113.3(7) . . ? C10 C5 C7 118.4(6) . . ? C6 C5 C7 103.6(6) . . ? C10 C5 C4 115.0(7) . . ? C6 C5 C4 103.6(6) . . ? C7 C5 C4 101.0(6) . . ? O1 C6 C5 112.6(6) . . ? O1 C6 C1 111.8(6) . . ? C5 C6 C1 102.9(6) . . ? C8 C7 C2 113.3(6) . . ? C8 C7 C9 105.0(6) . . ? C2 C7 C9 116.4(6) . . ? C8 C7 C5 113.5(6) . . ? C2 C7 C5 94.1(6) . . ? C9 C7 C5 114.7(6) . . ? O1 C11 C16 110.2(6) . . ? O1 C11 C12 115.2(6) . . ? C16 C11 C12 104.1(6) . . ? C13 C12 C11 101.5(5) . . ? C13 C12 P1 115.0(5) . . ? C11 C12 P1 109.1(5) . . ? C17 C13 C14 103.8(5) . . ? C17 C13 C12 101.3(6) . . ? C14 C13 C12 103.2(6) . . ? C15 C14 C40 121.9(6) . . ? C15 C14 C13 103.8(5) . . ? C40 C14 C13 126.5(6) . . ? C15 C14 Pd1 111.5(5) . . ? C40 C14 Pd1 75.3(4) . . ? C13 C14 Pd1 114.2(4) . . ? C15 C14 Pd2 63.6(4) . . ? C40 C14 Pd2 64.8(3) . . ? C13 C14 Pd2 124.0(4) . . ? Pd1 C14 Pd2 121.2(3) . . ? C14 C15 C16 107.4(6) . . ? C14 C15 Pd2 77.9(4) . . ? C16 C15 Pd2 121.7(5) . . ? C20 C16 C15 116.4(6) . . ? C20 C16 C11 113.3(6) . . ? C15 C16 C11 103.0(6) . . ? C20 C16 C17 118.0(6) . . ? C15 C16 C17 103.6(6) . . ? C11 C16 C17 100.2(6) . . ? C18 C17 C19 106.8(6) . . ? C18 C17 C13 114.0(6) . . ? C19 C17 C13 113.6(6) . . ? C18 C17 C16 115.9(6) . . ? C19 C17 C16 113.2(6) . . ? C13 C17 C16 93.3(6) . . ? C22 C21 C26 118.9(7) . . ? C22 C21 P1 123.2(5) . . ? C26 C21 P1 117.8(6) . . ? C23 C22 C21 122.3(7) . . ? C22 C23 C24 116.4(8) . . ? C25 C24 C23 123.1(8) . . ? C24 C25 C26 120.2(8) . . ? C25 C26 C21 118.9(8) . . ? C32 C27 C28 103.1(6) . . ? C32 C27 P2 113.6(5) . . ? C28 C27 P2 118.3(5) . . ? C33 C28 C29 102.4(6) . . ? C33 C28 C27 104.4(6) . . ? C29 C28 C27 103.2(6) . . ? C28 C29 C30 103.7(6) . . ? C29 C30 C31 103.8(6) . . ? C36 C31 C32 114.4(7) . . ? C36 C31 C30 115.1(6) . . ? C32 C31 C30 104.0(7) . . ? C36 C31 C33 118.5(7) . . ? C32 C31 C33 102.1(6) . . ? C30 C31 C33 100.6(6) . . ? O2 C32 C27 110.2(6) . . ? O2 C32 C31 114.1(7) . . ? C27 C32 C31 104.3(6) . . ? C28 C33 C34 116.8(7) . . ? C28 C33 C35 113.5(7) . . ? C34 C33 C35 106.9(7) . . ? C28 C33 C31 94.3(6) . . ? C34 C33 C31 113.7(7) . . ? C35 C33 C31 111.5(6) . . ? O2 C37 C42 110.3(6) . . ? O2 C37 C38 114.3(6) . . ? C42 C37 C38 102.2(6) . . ? C37 C38 C39 103.9(6) . . ? C37 C38 P2 110.0(5) . . ? C39 C38 P2 114.3(5) . . ? C40 C39 C43 104.7(6) . . ? C40 C39 C38 103.9(5) . . ? C43 C39 C38 98.7(5) . . ? C41 C40 C14 121.6(6) . . ? C41 C40 C39 103.9(6) . . ? C14 C40 C39 126.8(6) . . ? C41 C40 Pd2 110.7(5) . . ? C14 C40 Pd2 75.2(4) . . ? C39 C40 Pd2 114.8(5) . . ? C41 C40 Pd1 63.8(4) . . ? C14 C40 Pd1 64.8(3) . . ? C39 C40 Pd1 123.4(4) . . ? Pd2 C40 Pd1 121.2(3) . . ? C40 C41 C42 105.9(6) . . ? C40 C41 Pd1 77.5(4) . . ? C42 C41 Pd1 121.9(5) . . ? C41 C42 C46 115.1(7) . . ? C41 C42 C37 105.4(5) . . ? C46 C42 C37 113.6(6) . . ? C41 C42 C43 104.7(5) . . ? C46 C42 C43 116.5(6) . . ? C37 C42 C43 99.9(6) . . ? C44 C43 C42 114.3(6) . . ? C44 C43 C39 114.1(7) . . ? C42 C43 C39 93.2(5) . . ? C44 C43 C45 105.4(6) . . ? C42 C43 C45 116.8(6) . . ? C39 C43 C45 113.1(6) . . ? C52 C47 C48 118.0(7) . . ? C52 C47 P2 122.5(6) . . ? C48 C47 P2 119.4(6) . . ? C49 C48 C47 120.7(8) . . ? C50 C49 C48 122.3(7) . . ? C49 C50 C51 118.7(8) . . ? C52 C51 C50 119.3(8) . . ? C47 C52 C51 121.0(7) . . ? C54 C53 C58 120.0 . . ? C55 C54 C53 120.0 . . ? C54 C55 C56 120.0 . . ? C55 C56 C57 120.0 . . ? C58 C57 C56 120.0 . . ? C57 C58 C53 120.0 . . ? C57 C58 C59 120.9(6) . . ? C53 C58 C59 119.1(6) . . ? C61 C60 C65 120.0 . . ? C62 C61 C60 120.0 . . ? C61 C62 C63 120.0 . . ? C64 C63 C62 120.0 . . ? C63 C64 C65 120.0 . . ? C64 C65 C60 120.0 . . ? C64 C65 C66 127(2) . . ? C60 C65 C66 113(2) . . ? C68 C67 C72 120.0 . . ? C68 C67 C73 114.3(18) . . ? C72 C67 C73 125.5(18) . . ? C67 C68 C69 120.0 . . ? C68 C69 C70 120.0 . . ? C71 C70 C69 120.0 . . ? C70 C71 C72 120.0 . . ? C71 C72 C67 120.0 . . ? C75 C74 C79 120.0 . . ? C75 C74 C80 97(3) . . ? C79 C74 C80 140(3) . . ? C76 C75 C74 120.0 . . ? C75 C76 C77 120.0 . . ? C78 C77 C76 120.0 . . ? C79 C78 C77 120.0 . . ? C78 C79 C74 120.0 . . ? _diffrn_measured_fraction_theta_max 0.944 _diffrn_reflns_theta_full 27.45 _diffrn_measured_fraction_theta_full 0.944 _refine_diff_density_max 0.803 _refine_diff_density_min -0.698 _refine_diff_density_rms 0.124 #===END data_compound11 _database_code_CSD 213242 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C54 H74 Ag2 F6 O8 P2 S2' _chemical_formula_weight 1306.93 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' F F 0.0171 0.0103 '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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 16.6065(2) _cell_length_b 17.2601(2) _cell_length_c 20.6222(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5910.94(13) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 'all observed reflections in the data set' _cell_measurement_theta_min 3.08 _cell_measurement_theta_max 26.00 _exptl_crystal_description needle-like _exptl_crystal_colour colorless _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.469 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2688 _exptl_absorpt_coefficient_mu 0.855 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.679 _exptl_absorpt_correction_T_max 0.706 _exptl_absorpt_process_details 'SORTAV (Blessing, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Nonius kappa CCD area detector' _diffrn_measurement_method 'phi & omega scan to fill Ewald sphere' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 43065 _diffrn_reflns_av_R_equivalents 0.0619 _diffrn_reflns_av_sigmaI/netI 0.0591 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 3.08 _diffrn_reflns_theta_max 26.00 _reflns_number_total 11592 _reflns_number_gt 8219 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Hooft, 1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-96 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 for Windows (Farrugia, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The atoms F1 to F6, O3 to O6, C1, C21, C22 and C28 were refined with ISOR = 0.01. ; _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^)+(0.0849P)^2^+5.1475P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment 'calculated positions, riding model' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.02(4) _refine_ls_number_reflns 11592 _refine_ls_number_parameters 679 _refine_ls_number_restraints 84 _refine_ls_R_factor_all 0.0902 _refine_ls_R_factor_gt 0.0598 _refine_ls_wR_factor_ref 0.1646 _refine_ls_wR_factor_gt 0.1463 _refine_ls_goodness_of_fit_ref 1.009 _refine_ls_restrained_S_all 1.064 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.20393(4) 0.18443(3) 0.33963(3) 0.0715(2) Uani 1 1 d . . . Ag2 Ag 0.43772(4) 0.17109(3) 0.26587(4) 0.0808(2) Uani 1 1 d . . . S1 S 0.29272(13) 0.05525(10) 0.22862(10) 0.0662(5) Uani 1 1 d . . . S2 S 0.37862(17) 0.14668(16) 0.42490(13) 0.0897(7) Uani 1 1 d . . . P1 P 0.08747(12) 0.25180(10) 0.37319(9) 0.0557(5) Uani 1 1 d . . . P2 P 0.53590(12) 0.26976(9) 0.24720(8) 0.0517(4) Uani 1 1 d . . . F1 F 0.1852(9) 0.0701(10) 0.1400(7) 0.247(6) Uani 1 1 d U . . F2 F 0.2870(8) 0.0048(5) 0.1122(4) 0.179(4) Uani 1 1 d U . . F3 F 0.2921(9) 0.1252(7) 0.1201(5) 0.197(4) Uani 1 1 d U . . F4 F 0.2642(8) 0.0775(7) 0.4839(6) 0.207(4) Uani 1 1 d U . . F5 F 0.3086(8) 0.0147(6) 0.4159(6) 0.191(4) Uani 1 1 d U . . F6 F 0.3773(7) 0.0294(6) 0.4979(6) 0.210(4) Uani 1 1 d U . . O1 O 0.2629(6) 0.1252(4) 0.2547(4) 0.138(4) Uani 1 1 d . . . O2 O 0.3777(4) 0.0561(4) 0.2248(5) 0.120(3) Uani 1 1 d . . . O3 O 0.2611(5) -0.0139(5) 0.2513(4) 0.131(3) Uani 1 1 d U . . O4 O 0.3345(6) 0.1762(7) 0.3782(6) 0.172(4) Uani 1 1 d U . . O5 O 0.4317(11) 0.1047(10) 0.3761(9) 0.248(7) Uani 1 1 d U . . O6 O 0.4164(10) 0.1864(8) 0.4688(7) 0.229(6) Uani 1 1 d U . . O7 O -0.0483(3) 0.1497(3) 0.3415(2) 0.0610(12) Uani 1 1 d . . . O8 O 0.4851(3) 0.3572(3) 0.1326(2) 0.0560(12) Uani 1 1 d . . . C1 C 0.2596(11) 0.0596(11) 0.1447(8) 0.140(5) Uani 1 1 d U . . C2 C 0.3413(10) 0.0604(8) 0.4547(6) 0.116(4) Uani 1 1 d . . . C3 C 0.1158(5) 0.3443(4) 0.4093(4) 0.0617(19) Uani 1 1 d . . . C4 C 0.1963(6) 0.3638(5) 0.4173(4) 0.075(2) Uani 1 1 d . . . H4 H 0.2369 0.3275 0.4057 0.090 Uiso 1 1 calc R . . C5 C 0.2182(7) 0.4358(6) 0.4420(5) 0.090(3) Uani 1 1 d . . . H5 H 0.2738 0.4479 0.4458 0.108 Uiso 1 1 calc R . . C6 C 0.1648(7) 0.4877(6) 0.4604(5) 0.092(3) Uani 1 1 d . . . H6 H 0.1816 0.5367 0.4764 0.110 Uiso 1 1 calc R . . C7 C 0.0826(8) 0.4696(6) 0.4559(6) 0.105(4) Uani 1 1 d . . . H7 H 0.0432 0.5063 0.4691 0.126 Uiso 1 1 calc R . . C8 C 0.0592(6) 0.3975(5) 0.4320(5) 0.086(3) Uani 1 1 d . . . H8 H 0.0037 0.3843 0.4312 0.104 Uiso 1 1 calc R . . C9 C 0.0272(4) 0.2021(4) 0.4360(3) 0.0540(17) Uani 1 1 d . . . H9 H 0.0075 0.2432 0.4664 0.065 Uiso 1 1 calc R . . C10 C 0.0705(5) 0.1403(4) 0.4782(3) 0.0591(18) Uani 1 1 d . . . H10 H 0.1296 0.1487 0.4846 0.071 Uiso 1 1 calc R . . C11 C 0.0201(6) 0.1364(5) 0.5407(3) 0.075(2) Uani 1 1 d . . . H11A H 0.0464 0.1033 0.5737 0.090 Uiso 1 1 calc R . . H11B H 0.0113 0.1887 0.5591 0.090 Uiso 1 1 calc R . . C12 C -0.0580(6) 0.1010(5) 0.5174(4) 0.074(2) Uani 1 1 d . . . H12A H -0.1029 0.1384 0.5221 0.089 Uiso 1 1 calc R . . H12B H -0.0710 0.0539 0.5427 0.089 Uiso 1 1 calc R . . C13 C -0.0443(5) 0.0804(4) 0.4448(3) 0.0615(19) Uani 1 1 d . . . C14 C -0.0476(4) 0.1605(4) 0.4099(3) 0.0549(16) Uani 1 1 d . . . H14 H -0.0971 0.1891 0.4236 0.066 Uiso 1 1 calc R . . C15 C 0.0469(5) 0.0623(4) 0.4450(3) 0.0604(19) Uani 1 1 d . . . C16 C 0.0703(6) -0.0088(5) 0.4869(5) 0.084(3) Uani 1 1 d . . . H16A H 0.0483 -0.0560 0.4672 0.127 Uiso 1 1 calc R . . H16B H 0.0481 -0.0026 0.5307 0.127 Uiso 1 1 calc R . . H16C H 0.1290 -0.0128 0.4894 0.127 Uiso 1 1 calc R . . C17 C 0.0856(6) 0.0466(4) 0.3794(4) 0.071(2) Uani 1 1 d . . . H17A H 0.0576 0.0036 0.3581 0.107 Uiso 1 1 calc R . . H17B H 0.1424 0.0331 0.3856 0.107 Uiso 1 1 calc R . . H17C H 0.0816 0.0931 0.3523 0.107 Uiso 1 1 calc R . . C18 C -0.1020(6) 0.0213(5) 0.4173(5) 0.088(3) Uani 1 1 d . . . H18A H -0.1564 0.0431 0.4163 0.133 Uiso 1 1 calc R . . H18B H -0.1016 -0.0252 0.4445 0.133 Uiso 1 1 calc R . . H18C H -0.0853 0.0076 0.3731 0.133 Uiso 1 1 calc R . . C19 C 0.0085(5) 0.2803(4) 0.3139(4) 0.0619(19) Uani 1 1 d . . . H19 H -0.0150 0.3299 0.3303 0.074 Uiso 1 1 calc R . . C20 C 0.0315(6) 0.2949(6) 0.2437(4) 0.088(3) Uani 1 1 d . . . H20 H 0.0622 0.3441 0.2372 0.106 Uiso 1 1 calc R . . C21 C 0.0716(7) 0.2262(7) 0.2146(5) 0.104(3) Uani 1 1 d U . . H21A H 0.1163 0.2077 0.2424 0.125 Uiso 1 1 calc R . . H21B H 0.0929 0.2382 0.1709 0.125 Uiso 1 1 calc R . . C22 C 0.0048(8) 0.1670(7) 0.2111(4) 0.103(3) Uani 1 1 d U . . H22A H 0.0165 0.1222 0.2396 0.124 Uiso 1 1 calc R . . H22B H -0.0025 0.1483 0.1661 0.124 Uiso 1 1 calc R . . C23 C -0.0724(6) 0.2120(5) 0.2352(4) 0.087(3) Uani 1 1 d . . . C24 C -0.0621(5) 0.2224(4) 0.3094(3) 0.0611(18) Uani 1 1 d . . . H24 H -0.1118 0.2469 0.3276 0.073 Uiso 1 1 calc R . . C25 C -0.0526(6) 0.2955(6) 0.2114(4) 0.082(3) Uani 1 1 d . . . C26 C -0.1118(7) 0.3575(6) 0.2339(5) 0.109(4) Uani 1 1 d . . . H26A H -0.1024 0.4054 0.2095 0.164 Uiso 1 1 calc R . . H26B H -0.1039 0.3674 0.2803 0.164 Uiso 1 1 calc R . . H26C H -0.1670 0.3397 0.2264 0.164 Uiso 1 1 calc R . . C27 C -0.0481(7) 0.3009(7) 0.1365(4) 0.110(4) Uani 1 1 d . . . H27A H 0.0084 0.3045 0.1231 0.165 Uiso 1 1 calc R . . H27B H -0.0773 0.3469 0.1218 0.165 Uiso 1 1 calc R . . H27C H -0.0724 0.2545 0.1174 0.165 Uiso 1 1 calc R . . C28 C -0.1554(8) 0.1764(8) 0.2186(6) 0.128(4) Uani 1 1 d U . . H28A H -0.1537 0.1203 0.2258 0.192 Uiso 1 1 calc R . . H28B H -0.1684 0.1868 0.1731 0.192 Uiso 1 1 calc R . . H28C H -0.1968 0.1994 0.2465 0.192 Uiso 1 1 calc R . . C29 C 0.6118(4) 0.2626(4) 0.3116(3) 0.0485(16) Uani 1 1 d . . . C30 C 0.6704(5) 0.3193(5) 0.3203(3) 0.0615(18) Uani 1 1 d . . . H30 H 0.6729 0.3623 0.2916 0.074 Uiso 1 1 calc R . . C31 C 0.7250(5) 0.3131(6) 0.3708(4) 0.077(2) Uani 1 1 d . . . H31 H 0.7646 0.3521 0.3773 0.093 Uiso 1 1 calc R . . C32 C 0.7212(5) 0.2481(6) 0.4128(4) 0.076(2) Uani 1 1 d . . . H32 H 0.7590 0.2428 0.4470 0.091 Uiso 1 1 calc R . . C33 C 0.6630(6) 0.1934(5) 0.4039(4) 0.074(2) Uani 1 1 d . . . H33 H 0.6593 0.1503 0.4324 0.088 Uiso 1 1 calc R . . C34 C 0.6100(5) 0.2009(4) 0.3535(3) 0.0623(19) Uani 1 1 d . . . H34 H 0.5703 0.1619 0.3473 0.075 Uiso 1 1 calc R . . C35 C 0.5990(5) 0.2765(4) 0.1736(3) 0.0594(18) Uani 1 1 d . . . H35 H 0.6526 0.2977 0.1869 0.071 Uiso 1 1 calc R . . C36 C 0.6143(7) 0.2011(5) 0.1345(4) 0.082(3) Uani 1 1 d . . . H36 H 0.6527 0.1644 0.1558 0.099 Uiso 1 1 calc R . . C37 C 0.5354(8) 0.1641(5) 0.1141(4) 0.098(3) Uani 1 1 d . . . H37A H 0.4981 0.1596 0.1514 0.117 Uiso 1 1 calc R . . H37B H 0.5445 0.1120 0.0955 0.117 Uiso 1 1 calc R . . C38 C 0.5019(7) 0.2202(5) 0.0626(4) 0.087(3) Uani 1 1 d . . . H38A H 0.4942 0.1935 0.0206 0.105 Uiso 1 1 calc R . . H38B H 0.4499 0.2426 0.0767 0.105 Uiso 1 1 calc R . . C39 C 0.5668(6) 0.2829(4) 0.0573(3) 0.072(2) Uani 1 1 d . . . C40 C 0.5633(5) 0.3320(4) 0.1203(3) 0.0554(17) Uani 1 1 d . . . H40 H 0.5994 0.3780 0.1154 0.067 Uiso 1 1 calc R . . C41 C 0.6459(7) 0.2357(5) 0.0683(4) 0.084(3) Uani 1 1 d . . . C42 C 0.7229(7) 0.2842(8) 0.0741(5) 0.120(4) Uani 1 1 d . . . H42A H 0.7093 0.3360 0.0902 0.180 Uiso 1 1 calc R . . H42B H 0.7485 0.2887 0.0314 0.180 Uiso 1 1 calc R . . H42C H 0.7601 0.2591 0.1044 0.180 Uiso 1 1 calc R . . C43 C 0.6622(9) 0.1755(7) 0.0149(5) 0.129(5) Uani 1 1 d . . . H43A H 0.6930 0.1323 0.0331 0.194 Uiso 1 1 calc R . . H43B H 0.6931 0.1997 -0.0201 0.194 Uiso 1 1 calc R . . H43C H 0.6109 0.1563 -0.0022 0.194 Uiso 1 1 calc R . . C44 C 0.5617(7) 0.3317(5) -0.0039(4) 0.089(3) Uani 1 1 d . . . H44A H 0.5641 0.2978 -0.0420 0.134 Uiso 1 1 calc R . . H44B H 0.6069 0.3682 -0.0050 0.134 Uiso 1 1 calc R . . H44C H 0.5109 0.3606 -0.0041 0.134 Uiso 1 1 calc R . . C45 C 0.4970(4) 0.3708(4) 0.2532(3) 0.0510(16) Uani 1 1 d . . . H45 H 0.5383 0.4022 0.2767 0.061 Uiso 1 1 calc R . . C46 C 0.4154(5) 0.3826(4) 0.2883(3) 0.0614(19) Uani 1 1 d . . . H46 H 0.4041 0.3441 0.3233 0.074 Uiso 1 1 calc R . . C47 C 0.4164(6) 0.4691(5) 0.3117(4) 0.078(2) Uani 1 1 d . . . H47A H 0.4672 0.4821 0.3344 0.094 Uiso 1 1 calc R . . H47B H 0.3701 0.4809 0.3403 0.094 Uiso 1 1 calc R . . C48 C 0.4096(6) 0.5120(4) 0.2444(4) 0.070(2) Uani 1 1 d . . . H48A H 0.3626 0.5473 0.2439 0.084 Uiso 1 1 calc R . . H48B H 0.4589 0.5424 0.2354 0.084 Uiso 1 1 calc R . . C49 C 0.3991(5) 0.4470(4) 0.1943(4) 0.0636(19) Uani 1 1 d . . . C50 C 0.4819(5) 0.4102(4) 0.1861(3) 0.0547(17) Uani 1 1 d . . . H50 H 0.5229 0.4519 0.1794 0.066 Uiso 1 1 calc R . . C51 C 0.3504(5) 0.3843(5) 0.2323(4) 0.069(2) Uani 1 1 d . . . C52 C 0.2662(6) 0.4130(6) 0.2547(5) 0.096(3) Uani 1 1 d . . . H52A H 0.2303 0.4170 0.2171 0.143 Uiso 1 1 calc R . . H52B H 0.2715 0.4640 0.2752 0.143 Uiso 1 1 calc R . . H52C H 0.2437 0.3762 0.2860 0.143 Uiso 1 1 calc R . . C53 C 0.3351(5) 0.3080(5) 0.1982(5) 0.086(3) Uani 1 1 d . . . H53A H 0.2886 0.3133 0.1693 0.128 Uiso 1 1 calc R . . H53B H 0.3241 0.2677 0.2305 0.128 Uiso 1 1 calc R . . H53C H 0.3826 0.2936 0.1728 0.128 Uiso 1 1 calc R . . C54 C 0.3622(6) 0.4756(5) 0.1296(4) 0.077(2) Uani 1 1 d . . . H54A H 0.4005 0.5099 0.1077 0.115 Uiso 1 1 calc R . . H54B H 0.3123 0.5041 0.1385 0.115 Uiso 1 1 calc R . . H54C H 0.3503 0.4310 0.1018 0.115 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 Ag1 0.0664(4) 0.0611(3) 0.0869(4) 0.0023(3) 0.0244(3) 0.0143(3) Ag2 0.0787(4) 0.0590(3) 0.1047(5) 0.0206(3) -0.0188(4) -0.0232(3) S1 0.0595(11) 0.0561(10) 0.0831(12) -0.0276(10) 0.0085(11) -0.0038(9) S2 0.0873(16) 0.0963(17) 0.0854(15) 0.0240(14) -0.0210(14) -0.0139(14) P1 0.0594(11) 0.0475(9) 0.0602(10) -0.0009(8) 0.0192(9) 0.0049(8) P2 0.0673(11) 0.0411(8) 0.0467(9) 0.0048(7) -0.0097(8) -0.0098(8) F1 0.209(8) 0.323(10) 0.207(8) -0.028(8) -0.085(7) 0.020(8) F2 0.256(8) 0.162(6) 0.119(5) -0.069(5) 0.026(6) -0.021(6) F3 0.271(9) 0.187(7) 0.133(6) 0.003(6) -0.018(6) -0.011(7) F4 0.188(8) 0.211(8) 0.223(8) 0.032(7) 0.056(7) -0.008(7) F5 0.227(8) 0.143(6) 0.201(7) -0.016(6) -0.002(7) -0.057(6) F6 0.201(8) 0.202(7) 0.226(8) 0.129(7) -0.064(6) -0.019(6) O1 0.206(9) 0.116(5) 0.090(5) -0.041(4) 0.002(5) 0.088(6) O2 0.065(4) 0.111(5) 0.185(8) 0.000(6) -0.006(5) -0.015(4) O3 0.145(6) 0.114(5) 0.135(6) -0.025(5) 0.043(5) -0.059(5) O4 0.148(7) 0.166(7) 0.202(7) 0.061(7) -0.077(6) -0.023(6) O5 0.229(10) 0.248(10) 0.266(10) 0.016(9) 0.096(8) 0.006(8) O6 0.273(10) 0.195(9) 0.220(9) -0.014(7) -0.117(8) -0.065(8) O7 0.069(3) 0.060(3) 0.054(3) 0.005(2) -0.009(2) 0.003(2) O8 0.077(3) 0.047(2) 0.045(2) -0.001(2) -0.008(2) -0.008(2) C1 0.132(8) 0.157(9) 0.131(8) -0.034(8) 0.019(7) 0.010(8) C2 0.162(12) 0.116(9) 0.069(6) 0.014(7) 0.006(7) 0.005(9) C3 0.078(5) 0.046(4) 0.061(4) 0.003(3) 0.026(4) 0.000(4) C4 0.077(6) 0.075(5) 0.072(5) -0.002(4) 0.015(5) 0.005(5) C5 0.088(7) 0.096(7) 0.087(6) -0.012(5) 0.007(5) -0.009(6) C6 0.108(8) 0.069(6) 0.099(7) -0.011(5) 0.016(6) -0.032(6) C7 0.122(9) 0.076(6) 0.118(8) -0.040(6) 0.030(7) -0.008(6) C8 0.078(6) 0.067(5) 0.114(7) -0.022(5) 0.027(6) -0.010(5) C9 0.064(4) 0.046(4) 0.052(4) -0.004(3) 0.017(3) 0.002(3) C10 0.063(4) 0.061(4) 0.054(4) -0.003(3) -0.002(4) -0.006(4) C11 0.096(6) 0.089(6) 0.040(4) 0.002(4) -0.002(4) -0.018(5) C12 0.093(6) 0.080(5) 0.050(4) 0.009(4) 0.008(4) -0.019(5) C13 0.074(5) 0.056(4) 0.055(4) 0.007(3) -0.009(4) -0.016(4) C14 0.055(4) 0.059(4) 0.051(4) 0.003(3) 0.003(3) -0.004(3) C15 0.077(5) 0.049(4) 0.055(4) 0.008(3) -0.002(4) -0.003(4) C16 0.100(7) 0.059(5) 0.094(6) 0.020(4) -0.009(5) 0.006(5) C17 0.089(6) 0.051(4) 0.074(5) -0.005(4) 0.007(4) 0.009(4) C18 0.100(7) 0.071(5) 0.094(6) -0.001(5) -0.019(5) -0.025(5) C19 0.071(5) 0.050(4) 0.065(4) 0.010(3) 0.024(4) 0.016(3) C20 0.090(6) 0.103(7) 0.072(5) 0.025(5) 0.025(5) 0.029(5) C21 0.103(6) 0.130(7) 0.079(5) -0.007(5) 0.020(5) 0.035(6) C22 0.148(8) 0.104(6) 0.058(4) 0.003(5) -0.002(5) 0.034(6) C23 0.105(7) 0.095(6) 0.060(5) 0.019(4) -0.013(5) 0.029(6) C24 0.063(4) 0.062(4) 0.058(4) 0.017(3) 0.002(4) 0.011(4) C25 0.088(6) 0.093(6) 0.065(5) 0.021(4) 0.017(4) 0.027(5) C26 0.127(9) 0.111(7) 0.090(6) 0.044(6) 0.019(6) 0.064(7) C27 0.131(9) 0.134(9) 0.065(5) 0.038(6) 0.006(6) 0.042(8) C28 0.143(8) 0.138(8) 0.103(6) 0.022(6) -0.037(6) -0.019(7) C29 0.061(4) 0.049(4) 0.035(3) -0.004(3) -0.004(3) 0.000(3) C30 0.071(4) 0.059(4) 0.055(4) -0.003(4) 0.001(3) -0.014(4) C31 0.066(5) 0.094(6) 0.071(5) -0.033(5) -0.004(4) -0.010(5) C32 0.065(5) 0.113(7) 0.051(4) -0.017(5) -0.018(4) 0.010(5) C33 0.094(6) 0.069(5) 0.058(4) 0.001(4) -0.019(4) 0.013(5) C34 0.081(5) 0.052(4) 0.054(4) 0.001(3) -0.006(4) -0.001(4) C35 0.081(5) 0.048(4) 0.049(4) 0.003(3) -0.006(4) -0.001(4) C36 0.136(8) 0.060(5) 0.051(4) -0.003(4) -0.010(5) 0.031(5) C37 0.180(11) 0.047(4) 0.066(5) -0.019(4) -0.017(6) -0.003(6) C38 0.142(9) 0.061(5) 0.059(5) -0.012(4) -0.010(5) -0.025(5) C39 0.119(7) 0.057(4) 0.039(3) -0.005(3) -0.006(4) -0.003(5) C40 0.079(5) 0.040(3) 0.047(3) 0.000(3) -0.004(3) -0.008(4) C41 0.127(9) 0.071(5) 0.054(4) -0.013(4) -0.010(5) 0.026(6) C42 0.101(8) 0.181(12) 0.077(6) -0.032(7) 0.019(6) 0.007(8) C43 0.196(13) 0.121(9) 0.072(6) -0.027(6) 0.010(7) 0.072(10) C44 0.151(9) 0.067(5) 0.050(4) -0.001(4) -0.014(5) 0.006(6) C45 0.067(4) 0.038(3) 0.048(4) 0.000(3) 0.003(3) -0.011(3) C46 0.080(5) 0.058(4) 0.046(4) 0.015(3) 0.005(4) -0.003(4) C47 0.089(6) 0.077(5) 0.068(5) 0.010(4) 0.002(5) 0.009(5) C48 0.090(6) 0.058(4) 0.063(4) 0.001(4) -0.006(4) 0.013(4) C49 0.083(5) 0.049(4) 0.059(4) 0.005(3) -0.004(4) -0.005(4) C50 0.075(5) 0.039(3) 0.051(4) 0.005(3) -0.003(3) -0.008(3) C51 0.066(5) 0.073(5) 0.069(5) 0.013(4) -0.018(4) -0.001(4) C52 0.069(6) 0.120(8) 0.098(7) 0.016(6) 0.013(5) 0.004(5) C53 0.074(5) 0.085(6) 0.098(6) 0.032(5) -0.024(5) -0.024(5) C54 0.099(6) 0.070(5) 0.062(4) 0.006(4) -0.010(5) 0.013(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 O1 2.252(6) . ? Ag1 O4 2.314(10) . ? Ag1 P1 2.3604(19) . ? Ag2 O2 2.376(8) . ? Ag2 P2 2.3889(18) . ? Ag2 O5 2.547(17) . ? S1 O3 1.385(7) . ? S1 O1 1.411(6) . ? S1 O2 1.414(7) . ? S1 C1 1.817(17) . ? S2 O6 1.297(11) . ? S2 O4 1.313(9) . ? S2 O5 1.522(16) . ? S2 C2 1.725(14) . ? P1 C3 1.823(8) . ? P1 C9 1.849(7) . ? P1 C19 1.859(8) . ? P2 C29 1.836(6) . ? P2 C35 1.847(8) . ? P2 C45 1.863(7) . ? F1 C1 1.253(18) . ? F2 C1 1.244(16) . ? F3 C1 1.352(19) . ? F4 C2 1.446(17) . ? F5 C2 1.247(15) . ? F6 C2 1.200(14) . ? O7 C14 1.423(8) . ? O7 C24 1.436(8) . ? O8 C40 1.394(9) . ? O8 C50 1.433(8) . ? C3 C4 1.388(12) . ? C3 C8 1.395(12) . ? C4 C5 1.392(13) . ? C5 C6 1.317(14) . ? C6 C7 1.402(16) . ? C7 C8 1.395(13) . ? C9 C14 1.532(10) . ? C9 C10 1.554(10) . ? C10 C11 1.538(11) . ? C10 C15 1.561(10) . ? C11 C12 1.513(12) . ? C12 C13 1.557(11) . ? C13 C18 1.510(11) . ? C13 C15 1.547(12) . ? C13 C14 1.559(10) . ? C15 C17 1.520(11) . ? C15 C16 1.551(10) . ? C19 C20 1.519(11) . ? C19 C24 1.544(11) . ? C20 C21 1.485(13) . ? C20 C25 1.547(14) . ? C21 C22 1.510(16) . ? C22 C23 1.579(14) . ? C23 C28 1.548(16) . ? C23 C24 1.551(11) . ? C23 C25 1.558(13) . ? C25 C26 1.526(12) . ? C25 C27 1.548(12) . ? C29 C34 1.371(9) . ? C29 C30 1.391(10) . ? C30 C31 1.385(11) . ? C31 C32 1.419(13) . ? C32 C33 1.364(12) . ? C33 C34 1.369(11) . ? C35 C36 1.552(10) . ? C35 C40 1.574(10) . ? C36 C37 1.516(16) . ? C36 C41 1.581(13) . ? C37 C38 1.541(13) . ? C38 C39 1.531(13) . ? C39 C44 1.520(10) . ? C39 C40 1.550(9) . ? C39 C41 1.563(13) . ? C41 C42 1.534(16) . ? C41 C43 1.536(12) . ? C45 C46 1.550(11) . ? C45 C50 1.563(9) . ? C46 C47 1.568(11) . ? C46 C51 1.580(11) . ? C47 C48 1.577(11) . ? C48 C49 1.535(10) . ? C49 C50 1.525(11) . ? C49 C54 1.548(11) . ? C49 C51 1.562(11) . ? C51 C53 1.515(12) . ? C51 C52 1.554(12) . ? 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 O1 Ag1 O4 80.3(4) . . ? O1 Ag1 P1 143.9(2) . . ? O4 Ag1 P1 134.2(3) . . ? O2 Ag2 P2 145.5(2) . . ? O2 Ag2 O5 85.8(5) . . ? P2 Ag2 O5 119.4(4) . . ? O3 S1 O1 118.4(5) . . ? O3 S1 O2 114.0(6) . . ? O1 S1 O2 111.2(6) . . ? O3 S1 C1 104.0(7) . . ? O1 S1 C1 102.8(7) . . ? O2 S1 C1 104.4(7) . . ? O6 S2 O4 125.2(9) . . ? O6 S2 O5 115.6(11) . . ? O4 S2 O5 91.3(10) . . ? O6 S2 C2 112.4(8) . . ? O4 S2 C2 113.3(7) . . ? O5 S2 C2 91.9(8) . . ? C3 P1 C9 105.0(3) . . ? C3 P1 C19 102.6(4) . . ? C9 P1 C19 101.6(3) . . ? C3 P1 Ag1 109.9(3) . . ? C9 P1 Ag1 114.9(2) . . ? C19 P1 Ag1 121.0(2) . . ? C29 P2 C35 102.1(3) . . ? C29 P2 C45 104.6(3) . . ? C35 P2 C45 101.1(3) . . ? C29 P2 Ag2 107.7(2) . . ? C35 P2 Ag2 124.3(2) . . ? C45 P2 Ag2 114.8(2) . . ? S1 O1 Ag1 146.8(6) . . ? S1 O2 Ag2 114.1(5) . . ? S2 O4 Ag1 143.0(7) . . ? S2 O5 Ag2 113.5(9) . . ? C14 O7 C24 110.2(5) . . ? C40 O8 C50 111.9(5) . . ? F2 C1 F1 115.4(18) . . ? F2 C1 F3 106.8(13) . . ? F1 C1 F3 104.0(18) . . ? F2 C1 S1 111.8(13) . . ? F1 C1 S1 112.2(12) . . ? F3 C1 S1 105.7(12) . . ? F6 C2 F5 114.2(14) . . ? F6 C2 F4 102.9(11) . . ? F5 C2 F4 90.6(13) . . ? F6 C2 S2 118.1(13) . . ? F5 C2 S2 118.3(9) . . ? F4 C2 S2 106.9(10) . . ? C4 C3 C8 116.7(7) . . ? C4 C3 P1 120.6(6) . . ? C8 C3 P1 122.7(7) . . ? C3 C4 C5 120.8(8) . . ? C6 C5 C4 122.4(10) . . ? C5 C6 C7 119.0(9) . . ? C8 C7 C6 119.5(10) . . ? C3 C8 C7 121.2(10) . . ? C14 C9 C10 104.5(6) . . ? C14 C9 P1 114.2(5) . . ? C10 C9 P1 117.4(5) . . ? C11 C10 C9 104.3(6) . . ? C11 C10 C15 101.2(6) . . ? C9 C10 C15 103.3(6) . . ? C12 C11 C10 102.6(6) . . ? C11 C12 C13 105.8(7) . . ? C18 C13 C15 119.0(7) . . ? C18 C13 C12 115.0(7) . . ? C15 C13 C12 100.8(6) . . ? C18 C13 C14 113.8(6) . . ? C15 C13 C14 102.3(6) . . ? C12 C13 C14 103.7(6) . . ? O7 C14 C9 114.6(6) . . ? O7 C14 C13 110.0(6) . . ? C9 C14 C13 103.1(6) . . ? C17 C15 C13 116.6(7) . . ? C17 C15 C16 104.5(7) . . ? C13 C15 C16 113.9(7) . . ? C17 C15 C10 116.0(6) . . ? C13 C15 C10 94.2(6) . . ? C16 C15 C10 112.0(6) . . ? C20 C19 C24 104.0(7) . . ? C20 C19 P1 119.5(6) . . ? C24 C19 P1 113.8(5) . . ? C21 C20 C19 111.4(8) . . ? C21 C20 C25 103.7(9) . . ? C19 C20 C25 100.6(7) . . ? C20 C21 C22 103.3(9) . . ? C21 C22 C23 104.4(8) . . ? C28 C23 C24 111.2(8) . . ? C28 C23 C25 119.1(8) . . ? C24 C23 C25 100.4(7) . . ? C28 C23 C22 117.3(9) . . ? C24 C23 C22 106.2(7) . . ? C25 C23 C22 100.6(8) . . ? O7 C24 C19 114.6(6) . . ? O7 C24 C23 111.8(6) . . ? C19 C24 C23 102.5(6) . . ? C26 C25 C20 117.1(9) . . ? C26 C25 C27 107.0(8) . . ? C20 C25 C27 112.7(8) . . ? C26 C25 C23 114.7(8) . . ? C20 C25 C23 92.8(7) . . ? C27 C25 C23 112.3(9) . . ? C34 C29 C30 118.7(6) . . ? C34 C29 P2 119.5(5) . . ? C30 C29 P2 121.7(5) . . ? C31 C30 C29 120.0(7) . . ? C30 C31 C32 119.4(8) . . ? C33 C32 C31 119.8(7) . . ? C32 C33 C34 119.5(8) . . ? C33 C34 C29 122.6(8) . . ? C36 C35 C40 102.0(5) . . ? C36 C35 P2 117.9(6) . . ? C40 C35 P2 113.5(5) . . ? C37 C36 C35 110.8(8) . . ? C37 C36 C41 101.9(7) . . ? C35 C36 C41 100.8(6) . . ? C36 C37 C38 103.8(7) . . ? C39 C38 C37 103.9(8) . . ? C44 C39 C38 114.3(7) . . ? C44 C39 C40 113.0(6) . . ? C38 C39 C40 107.5(7) . . ? C44 C39 C41 117.1(8) . . ? C38 C39 C41 102.2(7) . . ? C40 C39 C41 101.3(6) . . ? O8 C40 C39 111.0(6) . . ? O8 C40 C35 114.4(6) . . ? C39 C40 C35 103.8(5) . . ? C42 C41 C43 106.2(10) . . ? C42 C41 C39 115.3(8) . . ? C43 C41 C39 113.4(8) . . ? C42 C41 C36 114.6(8) . . ? C43 C41 C36 114.9(8) . . ? C39 C41 C36 92.4(7) . . ? C46 C45 C50 102.5(6) . . ? C46 C45 P2 117.3(4) . . ? C50 C45 P2 113.8(4) . . ? C45 C46 C47 105.1(6) . . ? C45 C46 C51 105.0(6) . . ? C47 C46 C51 102.4(6) . . ? C46 C47 C48 100.1(6) . . ? C49 C48 C47 104.9(6) . . ? C50 C49 C48 106.1(6) . . ? C50 C49 C54 113.3(7) . . ? C48 C49 C54 113.1(6) . . ? C50 C49 C51 103.5(6) . . ? C48 C49 C51 103.1(6) . . ? C54 C49 C51 116.6(7) . . ? O8 C50 C49 112.6(6) . . ? O8 C50 C45 113.5(5) . . ? C49 C50 C45 103.2(6) . . ? C53 C51 C52 105.3(7) . . ? C53 C51 C49 117.2(7) . . ? C52 C51 C49 113.2(7) . . ? C53 C51 C46 116.0(6) . . ? C52 C51 C46 113.7(7) . . ? C49 C51 C46 91.5(6) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.694 _refine_diff_density_min -0.657 _refine_diff_density_rms 0.075