# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email dmatt@chimie.u-strasbg.fr _publ_contact_author_name D.Matt _publ_author_name D.Matt data_dipagchelate_ph2 _database_code_depnum_ccdc_archive 'CCDC 753229' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C33 H33 Ag0.50 B0.50 Cl2 F2 O2 P' _chemical_formula_weight 660.80 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' Cl Cl 0.1484 0.1585 '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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.0076(2) _cell_length_b 16.3137(2) _cell_length_c 17.0857(3) _cell_angle_alpha 63.705(2) _cell_angle_beta 70.812(2) _cell_angle_gamma 66.189(2) _cell_volume 3148.53(8) _cell_formula_units_Z 4 _cell_measurement_temperature 130(2) _cell_measurement_reflns_used 28533 _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 27.1 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.394 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1360 _exptl_absorpt_coefficient_mu 0.599 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 130(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD Saphire 3 Xcalibur' _diffrn_measurement_method 'omega scan' _diffrn_detector_area_resol_mean 19.64 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 43063 _diffrn_reflns_av_R_equivalents 0.0198 _diffrn_reflns_av_sigmaI/netI 0.0254 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.70 _diffrn_reflns_theta_max 27.00 _reflns_number_total 12667 _reflns_number_gt 10742 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd.,Version 1.171.26' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd.,Version 1.171.26' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd.,Version 1.171.26' _computing_structure_solution 'SIR-97_(Altomare& al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'MERCURY(CCDC, 2006)' _computing_publication_material 'WINGX (Farrugia, 1999)' _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. Due to difficulty with ADP for CL3, the instruction DELU was use : DELU 0.01 0.01 CL3 CL4 C72 Convergence was reached after 24 cycles. ; _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^)+(0.1096P)^2^+5.0607P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12667 _refine_ls_number_parameters 739 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0640 _refine_ls_R_factor_gt 0.0562 _refine_ls_wR_factor_ref 0.1723 _refine_ls_wR_factor_gt 0.1681 _refine_ls_goodness_of_fit_ref 1.081 _refine_ls_restrained_S_all 1.082 _refine_ls_shift/su_max 0.008 _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 0.51940(2) 0.210487(19) 0.854053(16) 0.02099(10) Uani 1 1 d . . . P1 P 0.59833(7) 0.23877(6) 0.69929(6) 0.01619(19) Uani 1 1 d . . . P2 P 0.53431(7) 0.16423(7) 1.00642(6) 0.01774(19) Uani 1 1 d . . . O1 O 0.81238(19) -0.13583(18) 0.64424(16) 0.0198(5) Uani 1 1 d . . . O2 O 0.73731(19) -0.18387(18) 0.51839(17) 0.0217(5) Uani 1 1 d . . . O3 O 0.7736(2) -0.34867(19) 0.71620(18) 0.0252(6) Uani 1 1 d . . . O4 O 0.9094(2) -0.32672(19) 0.83024(18) 0.0250(6) Uani 1 1 d . . . C1 C 0.6651(3) 0.1286(2) 0.6757(2) 0.0168(7) Uani 1 1 d . . . C2 C 0.6503(3) 0.1136(3) 0.6069(2) 0.0181(7) Uani 1 1 d . . . H2 H 0.6048 0.1642 0.5676 0.022 Uiso 1 1 calc R . . C3 C 0.7008(3) 0.0256(3) 0.5944(2) 0.0181(7) Uani 1 1 d . . . C4 C 0.7679(3) -0.0477(2) 0.6526(2) 0.0171(7) Uani 1 1 d . . . C5 C 0.7805(3) -0.0363(3) 0.7254(2) 0.0164(6) Uani 1 1 d . . . C6 C 0.7301(3) 0.0522(3) 0.7347(2) 0.0177(7) Uani 1 1 d . . . H6 H 0.7398 0.0615 0.7823 0.021 Uiso 1 1 calc R . . C7 C 0.6760(3) 0.0056(3) 0.5256(2) 0.0214(7) Uani 1 1 d . . . H7A H 0.6390 0.0667 0.4831 0.026 Uiso 1 1 calc R . . H7B H 0.7429 -0.0253 0.4921 0.026 Uiso 1 1 calc R . . C8 C 0.4437(3) -0.0883(3) 0.6680(2) 0.0248(8) Uani 1 1 d . . . H8 H 0.3756 -0.0657 0.7005 0.030 Uiso 1 1 calc R . . C9 C 0.5078(3) -0.0296(3) 0.6214(2) 0.0227(8) Uani 1 1 d . . . H9 H 0.4839 0.0329 0.6236 0.027 Uiso 1 1 calc R . . C10 C 0.6065(3) -0.0599(3) 0.5714(2) 0.0190(7) Uani 1 1 d . . . C11 C 0.6393(3) -0.1518(3) 0.5688(2) 0.0187(7) Uani 1 1 d . . . C12 C 0.5778(3) -0.2142(3) 0.6188(2) 0.0216(7) Uani 1 1 d . . . C13 C 0.4794(3) -0.1806(3) 0.6672(2) 0.0246(8) Uani 1 1 d . . . H13 H 0.4359 -0.2214 0.7002 0.030 Uiso 1 1 calc R . . C14 C 0.6177(3) -0.3179(3) 0.6246(3) 0.0261(8) Uani 1 1 d . . . H14A H 0.5698 -0.3288 0.6011 0.031 Uiso 1 1 calc R . . H14B H 0.6893 -0.3308 0.5876 0.031 Uiso 1 1 calc R . . C15 C 0.5464(3) -0.4902(3) 0.8569(3) 0.0310(9) Uani 1 1 d . . . H15 H 0.4959 -0.5243 0.8886 0.037 Uiso 1 1 calc R . . C16 C 0.6194(3) -0.4964(3) 0.9003(3) 0.0276(8) Uani 1 1 d . . . H16 H 0.6167 -0.5330 0.9620 0.033 Uiso 1 1 calc R . . C17 C 0.6960(3) -0.4492(3) 0.8540(3) 0.0232(8) Uani 1 1 d . . . C18 C 0.6988(3) -0.3972(3) 0.7629(3) 0.0223(7) Uani 1 1 d . . . C19 C 0.6226(3) -0.3862(3) 0.7195(3) 0.0246(8) Uani 1 1 d . . . C20 C 0.5479(3) -0.4346(3) 0.7679(3) 0.0282(8) Uani 1 1 d . . . H20 H 0.4968 -0.4295 0.7393 0.034 Uiso 1 1 calc R . . C21 C 0.7679(3) -0.4454(3) 0.9010(3) 0.0248(8) Uani 1 1 d . . . H21A H 0.8425 -0.4634 0.8705 0.030 Uiso 1 1 calc R . . H21B H 0.7623 -0.4914 0.9630 0.030 Uiso 1 1 calc R . . C22 C 0.4076(3) 0.2078(3) 1.0709(2) 0.0179(7) Uani 1 1 d . . . C23 C 0.3401(3) 0.1507(3) 1.1178(2) 0.0170(7) Uani 1 1 d . . . H23 H 0.3671 0.0843 1.1265 0.020 Uiso 1 1 calc R . . C24 C 0.7657(3) -0.1891(2) 0.8478(2) 0.0168(7) Uani 1 1 d . . . C25 C 0.8034(3) -0.2867(3) 0.8599(2) 0.0183(7) Uani 1 1 d . . . C26 C 0.7350(3) -0.3437(3) 0.9002(2) 0.0207(7) Uani 1 1 d . . . C27 C 0.3688(3) 0.3033(3) 1.0637(2) 0.0206(7) Uani 1 1 d . . . H27 H 0.4147 0.3422 1.0331 0.025 Uiso 1 1 calc R . . C28 C 0.8346(3) -0.1231(3) 0.7974(2) 0.0184(7) Uani 1 1 d . . . H28A H 0.8464 -0.1022 0.8388 0.022 Uiso 1 1 calc R . . H28B H 0.9045 -0.1580 0.7704 0.022 Uiso 1 1 calc R . . C29 C 0.9248(3) -0.1620(3) 0.6105(3) 0.0299(9) Uani 1 1 d . . . H29A H 0.9555 -0.2325 0.6363 0.036 Uiso 1 1 calc R . . H29B H 0.9583 -0.1326 0.6298 0.036 Uiso 1 1 calc R . . C30 C 0.9498(3) -0.1307(3) 0.5125(3) 0.0331(9) Uani 1 1 d . . . H30 H 0.9098 -0.1419 0.4849 0.040 Uiso 1 1 calc R . . C31 C 1.0225(4) -0.0889(4) 0.4603(4) 0.0456(12) Uani 1 1 d . . . H31A H 1.0644 -0.0763 0.4851 0.055 Uiso 1 1 calc R . . H31B H 1.0333 -0.0712 0.3978 0.055 Uiso 1 1 calc R . . C32 C 0.7305(3) -0.1801(3) 0.4347(2) 0.0242(8) Uani 1 1 d . . . H32A H 0.7101 -0.1126 0.3936 0.029 Uiso 1 1 calc R . . H32B H 0.6761 -0.2090 0.4433 0.029 Uiso 1 1 calc R . . C33 C 0.8380(3) -0.2353(3) 0.3964(3) 0.0356(10) Uani 1 1 d . . . H33A H 0.8576 -0.3025 0.4383 0.043 Uiso 1 1 calc R . . H33B H 0.8918 -0.2064 0.3893 0.043 Uiso 1 1 calc R . . C34 C 0.8385(4) -0.2346(4) 0.3069(3) 0.0442(12) Uani 1 1 d . . . H34A H 0.9092 -0.2712 0.2843 0.066 Uiso 1 1 calc R . . H34B H 0.8208 -0.1683 0.2649 0.066 Uiso 1 1 calc R . . H34C H 0.7860 -0.2639 0.3139 0.066 Uiso 1 1 calc R . . C35 C 0.8611(4) -0.3894(4) 0.6589(3) 0.0414(11) Uani 1 1 d . . . H35A H 0.8885 -0.3377 0.6102 0.050 Uiso 1 1 calc R . . H35B H 0.8362 -0.4181 0.6321 0.050 Uiso 1 1 calc R . . C36 C 0.9494(4) -0.4645(4) 0.7057(4) 0.0486(12) Uani 1 1 d . . . H36A H 0.9267 -0.5215 0.7479 0.058 Uiso 1 1 calc R . . H36B H 0.9689 -0.4394 0.7395 0.058 Uiso 1 1 calc R . . C37 C 1.0466(4) -0.4929(5) 0.6351(5) 0.071(2) Uani 1 1 d . . . H37A H 1.1053 -0.5421 0.6649 0.106 Uiso 1 1 calc R . . H37B H 1.0687 -0.4362 0.5936 0.106 Uiso 1 1 calc R . . H37C H 1.0268 -0.5183 0.6024 0.106 Uiso 1 1 calc R . . C38 C 0.9682(3) -0.3871(3) 0.9030(3) 0.0343(10) Uani 1 1 d . . . H38A H 1.0376 -0.4275 0.8812 0.041 Uiso 1 1 calc R . . H38B H 0.9282 -0.4302 0.9504 0.041 Uiso 1 1 calc R . . C39 C 0.9859(3) -0.3288(3) 0.9404(3) 0.0379(10) Uani 1 1 d . . . H39 H 1.0282 -0.2878 0.9027 0.045 Uiso 1 1 calc R . . C40 C 0.9475(4) -0.3302(4) 1.0211(4) 0.0466(12) Uani 1 1 d . . . H40A H 0.9049 -0.3705 1.0607 0.056 Uiso 1 1 calc R . . H40B H 0.9621 -0.2910 1.0406 0.056 Uiso 1 1 calc R . . C41 C 0.5199(3) 0.3219(2) 0.6131(2) 0.0176(7) Uani 1 1 d . . . C42 C 0.5677(3) 0.3529(3) 0.5234(2) 0.0213(7) Uani 1 1 d . . . H42 H 0.6424 0.3291 0.5065 0.026 Uiso 1 1 calc R . . C43 C 0.5062(3) 0.4182(3) 0.4594(2) 0.0249(8) Uani 1 1 d . . . H43 H 0.5389 0.4393 0.3987 0.030 Uiso 1 1 calc R . . C44 C 0.3974(3) 0.4528(3) 0.4836(3) 0.0302(9) Uani 1 1 d . . . H44 H 0.3553 0.4966 0.4395 0.036 Uiso 1 1 calc R . . C45 C 0.3500(3) 0.4238(3) 0.5719(3) 0.0332(9) Uani 1 1 d . . . H45 H 0.2754 0.4487 0.5884 0.040 Uiso 1 1 calc R . . C46 C 0.4110(3) 0.3582(3) 0.6371(3) 0.0254(8) Uani 1 1 d . . . H46 H 0.3780 0.3385 0.6978 0.031 Uiso 1 1 calc R . . C47 C 0.7051(3) 0.2879(2) 0.6761(2) 0.0190(7) Uani 1 1 d . . . C48 C 0.7966(3) 0.2711(3) 0.6135(3) 0.0259(8) Uani 1 1 d . . . H48 H 0.8049 0.2326 0.5817 0.031 Uiso 1 1 calc R . . C49 C 0.8758(3) 0.3104(3) 0.5974(3) 0.0363(10) Uani 1 1 d . . . H49 H 0.9376 0.3004 0.5536 0.044 Uiso 1 1 calc R . . C50 C 0.8636(3) 0.3644(3) 0.6458(3) 0.0369(10) Uani 1 1 d . . . H50 H 0.9183 0.3900 0.6362 0.044 Uiso 1 1 calc R . . C51 C 0.7729(3) 0.3816(3) 0.7080(3) 0.0318(9) Uani 1 1 d . . . H51 H 0.7651 0.4190 0.7406 0.038 Uiso 1 1 calc R . . C52 C 0.6936(3) 0.3439(3) 0.7225(3) 0.0247(8) Uani 1 1 d . . . H52 H 0.6307 0.3564 0.7645 0.030 Uiso 1 1 calc R . . C53 C 0.5811(3) 0.0352(3) 1.0669(2) 0.0186(7) Uani 1 1 d . . . C54 C 0.6336(3) -0.0257(3) 1.0190(2) 0.0256(8) Uani 1 1 d . . . H54 H 0.6409 0.0000 0.9561 0.031 Uiso 1 1 calc R . . C55 C 0.6753(3) -0.1236(3) 1.0619(3) 0.0285(8) Uani 1 1 d . . . H55 H 0.7118 -0.1644 1.0284 0.034 Uiso 1 1 calc R . . C56 C 0.6641(3) -0.1620(3) 1.1533(3) 0.0262(8) Uani 1 1 d . . . H56 H 0.6933 -0.2291 1.1826 0.031 Uiso 1 1 calc R . . C57 C 0.6097(3) -0.1020(3) 1.2023(2) 0.0271(8) Uani 1 1 d . . . H57 H 0.6005 -0.1283 1.2653 0.032 Uiso 1 1 calc R . . C58 C 0.5690(3) -0.0038(3) 1.1592(2) 0.0235(8) Uani 1 1 d . . . H58 H 0.5327 0.0370 1.1928 0.028 Uiso 1 1 calc R . . C59 C 0.6266(3) 0.2103(3) 1.0177(2) 0.0228(7) Uani 1 1 d . . . C60 C 0.6130(3) 0.2338(3) 1.0903(3) 0.0291(8) Uani 1 1 d . . . H60 H 0.5525 0.2280 1.1361 0.035 Uiso 1 1 calc R . . C61 C 0.6877(4) 0.2657(3) 1.0962(3) 0.0374(10) Uani 1 1 d . . . H61 H 0.6782 0.2817 1.1459 0.045 Uiso 1 1 calc R . . C62 C 0.7760(4) 0.2741(4) 1.0296(3) 0.0398(11) Uani 1 1 d . . . H62 H 0.8270 0.2960 1.0335 0.048 Uiso 1 1 calc R . . C63 C 0.7897(4) 0.2507(4) 0.9579(3) 0.0401(11) Uani 1 1 d . . . H63 H 0.8507 0.2561 0.9126 0.048 Uiso 1 1 calc R . . C64 C 0.7156(3) 0.2192(3) 0.9510(3) 0.0317(9) Uani 1 1 d . . . H64 H 0.7255 0.2037 0.9009 0.038 Uiso 1 1 calc R . . B1 B 0.7001(5) 0.5581(4) 0.1738(4) 0.0451(14) Uani 1 1 d . . . F1 F 0.7520(3) 0.5079(2) 0.1178(2) 0.0742(11) Uani 1 1 d . . . F2 F 0.6378(4) 0.5092(4) 0.2449(3) 0.0870(14) Uani 1 1 d . . . F3 F 0.7705(4) 0.5661(4) 0.2078(3) 0.0978(15) Uani 1 1 d . . . F4 F 0.6454(5) 0.6500(3) 0.1298(3) 0.130(3) Uani 1 1 d . . . C71 C 0.8070(14) 0.3033(8) 0.2892(7) 0.171(7) Uani 1 1 d . . . H71A H 0.7348 0.3432 0.2767 0.205 Uiso 1 1 calc R . . H71B H 0.8573 0.3274 0.2350 0.205 Uiso 1 1 calc R . . Cl1 Cl 0.82410(15) 0.32773(19) 0.37282(15) 0.1070(8) Uani 1 1 d . . . Cl2 Cl 0.8213(4) 0.1890(3) 0.3010(4) 0.225(3) Uani 1 1 d . . . C72 C 1.0216(13) -0.0293(12) 0.8789(13) 0.232(10) Uani 1 1 d U . . H72A H 1.0646 -0.0882 0.8652 0.279 Uiso 1 1 calc R . . H72B H 1.0669 -0.0136 0.9008 0.279 Uiso 1 1 calc R . . Cl3 Cl 0.9879(9) 0.0611(7) 0.7843(4) 0.368(6) Uani 1 1 d U . . Cl4 Cl 0.9218(4) -0.0518(5) 0.9579(4) 0.217(2) Uani 1 1 d U . . 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 0.02582(15) 0.02030(17) 0.01388(15) -0.00577(12) -0.00376(10) -0.00451(11) P1 0.0209(4) 0.0131(5) 0.0141(4) -0.0048(4) -0.0042(3) -0.0041(3) P2 0.0204(4) 0.0184(5) 0.0138(4) -0.0053(4) -0.0032(3) -0.0058(3) O1 0.0200(12) 0.0150(13) 0.0237(12) -0.0092(11) -0.0032(10) -0.0028(9) O2 0.0210(12) 0.0236(14) 0.0245(13) -0.0152(11) -0.0059(10) -0.0018(10) O3 0.0292(14) 0.0226(15) 0.0270(14) -0.0096(12) -0.0043(11) -0.0107(11) O4 0.0200(12) 0.0186(14) 0.0311(14) -0.0085(12) -0.0076(11) 0.0009(10) C1 0.0215(16) 0.0111(17) 0.0168(16) -0.0042(14) -0.0029(13) -0.0054(13) C2 0.0232(16) 0.0141(18) 0.0153(15) -0.0024(14) -0.0059(13) -0.0051(13) C3 0.0232(16) 0.0173(18) 0.0154(15) -0.0057(15) -0.0037(13) -0.0077(14) C4 0.0194(15) 0.0143(18) 0.0170(16) -0.0052(15) -0.0013(13) -0.0064(13) C5 0.0159(15) 0.0172(18) 0.0155(15) -0.0037(14) -0.0027(12) -0.0070(13) C6 0.0199(16) 0.0191(19) 0.0158(15) -0.0065(15) -0.0046(13) -0.0063(13) C7 0.0302(18) 0.0192(19) 0.0157(16) -0.0067(15) -0.0078(14) -0.0052(15) C8 0.0209(17) 0.030(2) 0.0237(18) -0.0123(17) -0.0057(14) -0.0030(15) C9 0.0259(18) 0.0201(19) 0.0228(18) -0.0104(16) -0.0113(14) 0.0007(14) C10 0.0238(17) 0.0193(19) 0.0163(16) -0.0075(15) -0.0096(13) -0.0029(14) C11 0.0207(16) 0.0200(19) 0.0183(16) -0.0097(15) -0.0068(13) -0.0031(13) C12 0.0270(18) 0.021(2) 0.0212(17) -0.0093(16) -0.0101(14) -0.0055(15) C13 0.0250(18) 0.029(2) 0.0212(17) -0.0073(17) -0.0069(14) -0.0101(15) C14 0.034(2) 0.022(2) 0.0284(19) -0.0138(17) -0.0072(16) -0.0089(16) C15 0.033(2) 0.026(2) 0.037(2) -0.0137(19) -0.0016(17) -0.0123(17) C16 0.035(2) 0.019(2) 0.0254(19) -0.0081(17) -0.0013(16) -0.0089(16) C17 0.0267(18) 0.0136(19) 0.0290(19) -0.0113(16) -0.0033(15) -0.0032(14) C18 0.0281(18) 0.0141(18) 0.0269(18) -0.0109(16) -0.0027(15) -0.0062(14) C19 0.0299(19) 0.0169(19) 0.029(2) -0.0127(17) -0.0054(15) -0.0047(15) C20 0.0296(19) 0.024(2) 0.037(2) -0.0155(19) -0.0061(16) -0.0090(16) C21 0.033(2) 0.0127(19) 0.0255(19) -0.0053(16) -0.0090(15) -0.0030(15) C22 0.0217(16) 0.0192(19) 0.0137(15) -0.0061(14) -0.0047(12) -0.0057(13) C23 0.0225(16) 0.0138(17) 0.0147(15) -0.0051(14) -0.0059(13) -0.0033(13) C24 0.0220(16) 0.0145(17) 0.0139(15) -0.0036(14) -0.0067(12) -0.0046(13) C25 0.0193(16) 0.0154(18) 0.0176(16) -0.0058(15) -0.0073(13) 0.0000(13) C26 0.0275(18) 0.0144(18) 0.0187(16) -0.0047(15) -0.0101(14) -0.0017(14) C27 0.0270(18) 0.0192(19) 0.0158(16) -0.0042(15) -0.0047(13) -0.0089(14) C28 0.0180(15) 0.0167(18) 0.0203(16) -0.0061(15) -0.0062(13) -0.0035(13) C29 0.0204(18) 0.026(2) 0.040(2) -0.0175(19) -0.0008(16) -0.0010(15) C30 0.030(2) 0.034(2) 0.039(2) -0.023(2) -0.0011(17) -0.0059(17) C31 0.040(3) 0.043(3) 0.048(3) -0.022(3) 0.006(2) -0.011(2) C32 0.0260(18) 0.026(2) 0.0213(17) -0.0111(16) -0.0089(14) -0.0017(15) C33 0.029(2) 0.044(3) 0.034(2) -0.025(2) -0.0116(17) 0.0059(18) C34 0.035(2) 0.061(3) 0.039(2) -0.035(2) -0.0106(19) 0.006(2) C35 0.035(2) 0.044(3) 0.049(3) -0.024(2) 0.003(2) -0.017(2) C36 0.043(3) 0.043(3) 0.056(3) -0.017(3) -0.006(2) -0.013(2) C37 0.032(3) 0.056(4) 0.111(6) -0.038(4) 0.012(3) -0.011(3) C38 0.026(2) 0.023(2) 0.045(2) -0.005(2) -0.0202(18) 0.0028(16) C39 0.030(2) 0.033(3) 0.047(3) -0.001(2) -0.022(2) -0.0104(18) C40 0.047(3) 0.043(3) 0.056(3) -0.016(3) -0.018(2) -0.014(2) C41 0.0234(16) 0.0107(17) 0.0195(16) -0.0045(14) -0.0079(13) -0.0038(13) C42 0.0264(18) 0.0207(19) 0.0181(16) -0.0073(16) -0.0036(14) -0.0083(14) C43 0.043(2) 0.019(2) 0.0183(17) -0.0038(16) -0.0114(15) -0.0131(16) C44 0.042(2) 0.017(2) 0.035(2) -0.0021(18) -0.0243(18) -0.0070(16) C45 0.0237(19) 0.026(2) 0.042(2) -0.005(2) -0.0119(17) -0.0039(16) C46 0.0234(18) 0.019(2) 0.0263(19) -0.0036(17) -0.0024(15) -0.0063(15) C47 0.0241(17) 0.0127(18) 0.0195(16) -0.0031(15) -0.0095(13) -0.0034(13) C48 0.0226(18) 0.027(2) 0.031(2) -0.0135(18) -0.0058(15) -0.0062(15) C49 0.0237(19) 0.035(3) 0.052(3) -0.020(2) -0.0058(18) -0.0076(17) C50 0.030(2) 0.028(2) 0.058(3) -0.014(2) -0.016(2) -0.0099(17) C51 0.039(2) 0.021(2) 0.042(2) -0.0124(19) -0.0176(19) -0.0071(17) C52 0.033(2) 0.0166(19) 0.0266(19) -0.0078(16) -0.0090(15) -0.0068(15) C53 0.0188(16) 0.0178(18) 0.0181(16) -0.0054(15) -0.0045(13) -0.0047(13) C54 0.036(2) 0.023(2) 0.0178(17) -0.0081(16) -0.0070(15) -0.0060(16) C55 0.036(2) 0.026(2) 0.0265(19) -0.0132(18) -0.0096(16) -0.0054(17) C56 0.0283(19) 0.019(2) 0.0289(19) -0.0026(17) -0.0115(16) -0.0064(15) C57 0.0262(18) 0.029(2) 0.0182(17) -0.0042(17) -0.0057(14) -0.0043(16) C58 0.0236(17) 0.025(2) 0.0193(17) -0.0088(16) -0.0039(14) -0.0037(15) C59 0.0253(18) 0.0189(19) 0.0217(17) -0.0011(16) -0.0080(14) -0.0083(14) C60 0.032(2) 0.035(2) 0.0244(19) -0.0093(18) -0.0057(16) -0.0151(17) C61 0.042(2) 0.045(3) 0.036(2) -0.013(2) -0.0147(19) -0.019(2) C62 0.034(2) 0.041(3) 0.048(3) -0.005(2) -0.018(2) -0.018(2) C63 0.028(2) 0.050(3) 0.039(2) -0.008(2) -0.0024(18) -0.021(2) C64 0.028(2) 0.038(3) 0.028(2) -0.0104(19) -0.0034(16) -0.0122(18) B1 0.049(3) 0.041(3) 0.029(2) -0.014(2) -0.007(2) 0.005(2) F1 0.096(3) 0.054(2) 0.0456(18) -0.0289(16) -0.0145(18) 0.0167(18) F2 0.099(3) 0.131(4) 0.071(2) -0.056(3) 0.031(2) -0.087(3) F3 0.074(3) 0.157(5) 0.094(3) -0.065(3) 0.013(2) -0.064(3) F4 0.165(5) 0.085(3) 0.057(2) -0.041(2) -0.044(3) 0.078(3) C71 0.290(19) 0.097(8) 0.075(6) -0.010(6) -0.076(9) 0.000(10) Cl1 0.0515(10) 0.135(2) 0.0865(13) -0.0377(13) -0.0105(9) 0.0132(11) Cl2 0.236(4) 0.138(3) 0.314(6) 0.068(3) -0.209(5) -0.111(3) C72 0.128(11) 0.182(16) 0.282(17) 0.039(13) -0.058(9) -0.069(12) Cl3 0.615(16) 0.429(11) 0.193(5) 0.067(6) -0.192(7) -0.392(12) Cl4 0.194(5) 0.292(6) 0.226(5) -0.106(5) -0.024(4) -0.130(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 P1 2.4158(9) . ? Ag1 P2 2.4248(9) . ? Ag1 F4 2.546(4) 2_666 ? P1 C1 1.817(3) . ? P1 C41 1.818(3) . ? P1 C47 1.826(4) . ? P2 C22 1.806(4) . ? P2 C53 1.825(4) . ? P2 C59 1.830(4) . ? O1 C4 1.370(4) . ? O1 C29 1.440(4) . ? O2 C11 1.393(4) . ? O2 C32 1.437(4) . ? O3 C18 1.387(5) . ? O3 C35 1.425(5) . ? O4 C25 1.380(4) . ? O4 C38 1.458(5) . ? C1 C2 1.396(4) . ? C1 C6 1.404(5) . ? C2 C3 1.399(5) . ? C2 H2 0.9500 . ? C3 C4 1.399(5) . ? C3 C7 1.518(4) . ? C4 C5 1.409(4) . ? C5 C6 1.384(5) . ? C5 C28 1.516(5) . ? C6 H6 0.9500 . ? C7 C10 1.517(5) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.380(6) . ? C8 C13 1.387(6) . ? C8 H8 0.9500 . ? C9 C10 1.390(5) . ? C9 H9 0.9500 . ? C10 C11 1.397(5) . ? C11 C12 1.400(5) . ? C12 C13 1.388(5) . ? C12 C14 1.520(5) . ? C13 H13 0.9500 . ? C14 C19 1.513(6) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C20 1.381(6) . ? C15 C16 1.398(6) . ? C15 H15 0.9500 . ? C16 C17 1.393(6) . ? C16 H16 0.9500 . ? C17 C18 1.401(5) . ? C17 C21 1.512(5) . ? C18 C19 1.402(5) . ? C19 C20 1.387(6) . ? C20 H20 0.9500 . ? C21 C26 1.527(5) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C27 1.389(5) . ? C22 C23 1.397(5) . ? C23 C24 1.393(5) 2_657 ? C23 H23 0.9500 . ? C24 C23 1.393(5) 2_657 ? C24 C25 1.399(5) . ? C24 C28 1.517(5) . ? C25 C26 1.405(5) . ? C26 C27 1.388(5) 2_657 ? C27 C26 1.388(5) 2_657 ? C27 H27 0.9500 . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 C30 1.481(6) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 C31 1.313(7) . ? C30 H30 0.9500 . ? C31 H31A 0.9500 . ? C31 H31B 0.9500 . ? C32 C33 1.512(5) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C34 1.521(5) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 C36 1.492(7) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 C37 1.558(8) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 C39 1.485(6) . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C39 C40 1.299(7) . ? C39 H39 0.9500 . ? C40 H40A 0.9500 . ? C40 H40B 0.9500 . ? C41 C46 1.385(5) . ? C41 C42 1.402(5) . ? C42 C43 1.385(5) . ? C42 H42 0.9500 . ? C43 C44 1.382(6) . ? C43 H43 0.9500 . ? C44 C45 1.379(6) . ? C44 H44 0.9500 . ? C45 C46 1.396(5) . ? C45 H45 0.9500 . ? C46 H46 0.9500 . ? C47 C52 1.388(5) . ? C47 C48 1.392(5) . ? C48 C49 1.392(6) . ? C48 H48 0.9500 . ? C49 C50 1.387(6) . ? C49 H49 0.9500 . ? C50 C51 1.383(7) . ? C50 H50 0.9500 . ? C51 C52 1.381(6) . ? C51 H51 0.9500 . ? C52 H52 0.9500 . ? C53 C54 1.391(5) . ? C53 C58 1.394(5) . ? C54 C55 1.386(6) . ? C54 H54 0.9500 . ? C55 C56 1.380(5) . ? C55 H55 0.9500 . ? C56 C57 1.396(6) . ? C56 H56 0.9500 . ? C57 C58 1.388(6) . ? C57 H57 0.9500 . ? C58 H58 0.9500 . ? C59 C60 1.389(5) . ? C59 C64 1.393(6) . ? C60 C61 1.390(6) . ? C60 H60 0.9500 . ? C61 C62 1.384(7) . ? C61 H61 0.9500 . ? C62 C63 1.372(7) . ? C62 H62 0.9500 . ? C63 C64 1.386(6) . ? C63 H63 0.9500 . ? C64 H64 0.9500 . ? B1 F4 1.361(7) . ? B1 F2 1.370(7) . ? B1 F1 1.369(6) . ? B1 F3 1.370(7) . ? F4 Ag1 2.546(4) 2_666 ? C71 Cl2 1.718(13) . ? C71 Cl1 1.751(12) . ? C71 H71A 0.9900 . ? C71 H71B 0.9900 . ? C72 Cl4 1.627(16) . ? C72 Cl3 1.683(16) . ? C72 H72A 0.9900 . ? C72 H72B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P1 Ag1 P2 150.89(3) . . ? P1 Ag1 F4 110.44(9) . 2_666 ? P2 Ag1 F4 90.10(9) . 2_666 ? C1 P1 C41 106.57(15) . . ? C1 P1 C47 104.13(16) . . ? C41 P1 C47 104.86(16) . . ? C1 P1 Ag1 112.86(12) . . ? C41 P1 Ag1 120.57(12) . . ? C47 P1 Ag1 106.36(11) . . ? C22 P2 C53 105.68(16) . . ? C22 P2 C59 106.42(16) . . ? C53 P2 C59 103.67(16) . . ? C22 P2 Ag1 111.01(11) . . ? C53 P2 Ag1 115.37(11) . . ? C59 P2 Ag1 113.88(12) . . ? C4 O1 C29 115.7(3) . . ? C11 O2 C32 113.9(3) . . ? C18 O3 C35 116.6(3) . . ? C25 O4 C38 112.2(3) . . ? C2 C1 C6 118.5(3) . . ? C2 C1 P1 124.2(3) . . ? C6 C1 P1 117.2(2) . . ? C1 C2 C3 121.5(3) . . ? C1 C2 H2 119.3 . . ? C3 C2 H2 119.3 . . ? C4 C3 C2 118.3(3) . . ? C4 C3 C7 119.9(3) . . ? C2 C3 C7 121.5(3) . . ? O1 C4 C3 118.6(3) . . ? O1 C4 C5 119.4(3) . . ? C3 C4 C5 121.6(3) . . ? C6 C5 C4 118.1(3) . . ? C6 C5 C28 121.6(3) . . ? C4 C5 C28 119.7(3) . . ? C5 C6 C1 121.9(3) . . ? C5 C6 H6 119.0 . . ? C1 C6 H6 119.0 . . ? C10 C7 C3 109.7(3) . . ? C10 C7 H7A 109.7 . . ? C3 C7 H7A 109.7 . . ? C10 C7 H7B 109.7 . . ? C3 C7 H7B 109.7 . . ? H7A C7 H7B 108.2 . . ? C9 C8 C13 119.5(3) . . ? C9 C8 H8 120.2 . . ? C13 C8 H8 120.2 . . ? C8 C9 C10 121.5(3) . . ? C8 C9 H9 119.3 . . ? C10 C9 H9 119.3 . . ? C9 C10 C11 118.1(3) . . ? C9 C10 C7 119.2(3) . . ? C11 C10 C7 122.7(3) . . ? O2 C11 C10 119.5(3) . . ? O2 C11 C12 119.1(3) . . ? C10 C11 C12 121.4(3) . . ? C13 C12 C11 118.5(3) . . ? C13 C12 C14 119.5(3) . . ? C11 C12 C14 122.0(3) . . ? C8 C13 C12 121.0(4) . . ? C8 C13 H13 119.5 . . ? C12 C13 H13 119.5 . . ? C19 C14 C12 110.9(3) . . ? C19 C14 H14A 109.5 . . ? C12 C14 H14A 109.5 . . ? C19 C14 H14B 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 108.0 . . ? C20 C15 C16 120.0(4) . . ? C20 C15 H15 120.0 . . ? C16 C15 H15 120.0 . . ? C17 C16 C15 120.6(4) . . ? C17 C16 H16 119.7 . . ? C15 C16 H16 119.7 . . ? C16 C17 C18 118.1(3) . . ? C16 C17 C21 121.7(4) . . ? C18 C17 C21 120.0(3) . . ? O3 C18 C17 118.7(3) . . ? O3 C18 C19 119.2(3) . . ? C17 C18 C19 121.9(3) . . ? C20 C19 C18 118.1(4) . . ? C20 C19 C14 121.1(3) . . ? C18 C19 C14 120.7(3) . . ? C15 C20 C19 121.2(4) . . ? C15 C20 H20 119.4 . . ? C19 C20 H20 119.4 . . ? C17 C21 C26 109.1(3) . . ? C17 C21 H21A 109.9 . . ? C26 C21 H21A 109.9 . . ? C17 C21 H21B 109.9 . . ? C26 C21 H21B 109.9 . . ? H21A C21 H21B 108.3 . . ? C27 C22 C23 118.6(3) . . ? C27 C22 P2 120.1(3) . . ? C23 C22 P2 120.6(3) . . ? C24 C23 C22 121.4(3) 2_657 . ? C24 C23 H23 119.3 2_657 . ? C22 C23 H23 119.3 . . ? C23 C24 C25 118.4(3) 2_657 . ? C23 C24 C28 118.8(3) 2_657 . ? C25 C24 C28 122.8(3) . . ? O4 C25 C24 119.0(3) . . ? O4 C25 C26 119.8(3) . . ? C24 C25 C26 121.2(3) . . ? C27 C26 C25 118.2(3) 2_657 . ? C27 C26 C21 118.8(3) 2_657 . ? C25 C26 C21 123.0(3) . . ? C26 C27 C22 121.9(3) 2_657 . ? C26 C27 H27 119.1 2_657 . ? C22 C27 H27 119.1 . . ? C5 C28 C24 109.6(3) . . ? C5 C28 H28A 109.8 . . ? C24 C28 H28A 109.8 . . ? C5 C28 H28B 109.8 . . ? C24 C28 H28B 109.8 . . ? H28A C28 H28B 108.2 . . ? O1 C29 C30 112.5(3) . . ? O1 C29 H29A 109.1 . . ? C30 C29 H29A 109.1 . . ? O1 C29 H29B 109.1 . . ? C30 C29 H29B 109.1 . . ? H29A C29 H29B 107.8 . . ? C31 C30 C29 125.6(4) . . ? C31 C30 H30 117.2 . . ? C29 C30 H30 117.2 . . ? C30 C31 H31A 120.0 . . ? C30 C31 H31B 120.0 . . ? H31A C31 H31B 120.0 . . ? O2 C32 C33 108.1(3) . . ? O2 C32 H32A 110.1 . . ? C33 C32 H32A 110.1 . . ? O2 C32 H32B 110.1 . . ? C33 C32 H32B 110.1 . . ? H32A C32 H32B 108.4 . . ? C32 C33 C34 111.8(3) . . ? C32 C33 H33A 109.3 . . ? C34 C33 H33A 109.3 . . ? C32 C33 H33B 109.3 . . ? C34 C33 H33B 109.3 . . ? H33A C33 H33B 107.9 . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? O3 C35 C36 113.0(4) . . ? O3 C35 H35A 109.0 . . ? C36 C35 H35A 109.0 . . ? O3 C35 H35B 109.0 . . ? C36 C35 H35B 109.0 . . ? H35A C35 H35B 107.8 . . ? C35 C36 C37 108.6(5) . . ? C35 C36 H36A 110.0 . . ? C37 C36 H36A 110.0 . . ? C35 C36 H36B 110.0 . . ? C37 C36 H36B 110.0 . . ? H36A C36 H36B 108.4 . . ? C36 C37 H37A 109.5 . . ? C36 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C36 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? O4 C38 C39 111.7(3) . . ? O4 C38 H38A 109.3 . . ? C39 C38 H38A 109.3 . . ? O4 C38 H38B 109.3 . . ? C39 C38 H38B 109.3 . . ? H38A C38 H38B 107.9 . . ? C40 C39 C38 124.5(5) . . ? C40 C39 H39 117.7 . . ? C38 C39 H39 117.7 . . ? C39 C40 H40A 120.0 . . ? C39 C40 H40B 120.0 . . ? H40A C40 H40B 120.0 . . ? C46 C41 C42 119.4(3) . . ? C46 C41 P1 119.2(3) . . ? C42 C41 P1 121.4(3) . . ? C43 C42 C41 120.2(3) . . ? C43 C42 H42 119.9 . . ? C41 C42 H42 119.9 . . ? C44 C43 C42 120.1(4) . . ? C44 C43 H43 119.9 . . ? C42 C43 H43 119.9 . . ? C43 C44 C45 120.0(4) . . ? C43 C44 H44 120.0 . . ? C45 C44 H44 120.0 . . ? C44 C45 C46 120.4(4) . . ? C44 C45 H45 119.8 . . ? C46 C45 H45 119.8 . . ? C41 C46 C45 119.8(4) . . ? C41 C46 H46 120.1 . . ? C45 C46 H46 120.1 . . ? C52 C47 C48 119.5(3) . . ? C52 C47 P1 118.5(3) . . ? C48 C47 P1 121.9(3) . . ? C49 C48 C47 120.2(4) . . ? C49 C48 H48 119.9 . . ? C47 C48 H48 119.9 . . ? C50 C49 C48 119.2(4) . . ? C50 C49 H49 120.4 . . ? C48 C49 H49 120.4 . . ? C51 C50 C49 120.9(4) . . ? C51 C50 H50 119.5 . . ? C49 C50 H50 119.5 . . ? C52 C51 C50 119.5(4) . . ? C52 C51 H51 120.2 . . ? C50 C51 H51 120.2 . . ? C51 C52 C47 120.6(4) . . ? C51 C52 H52 119.7 . . ? C47 C52 H52 119.7 . . ? C54 C53 C58 119.1(3) . . ? C54 C53 P2 118.8(3) . . ? C58 C53 P2 122.1(3) . . ? C55 C54 C53 120.7(3) . . ? C55 C54 H54 119.7 . . ? C53 C54 H54 119.7 . . ? C56 C55 C54 120.2(4) . . ? C56 C55 H55 119.9 . . ? C54 C55 H55 119.9 . . ? C55 C56 C57 119.7(4) . . ? C55 C56 H56 120.1 . . ? C57 C56 H56 120.1 . . ? C58 C57 C56 120.1(3) . . ? C58 C57 H57 120.0 . . ? C56 C57 H57 120.0 . . ? C57 C58 C53 120.2(3) . . ? C57 C58 H58 119.9 . . ? C53 C58 H58 119.9 . . ? C60 C59 C64 119.3(4) . . ? C60 C59 P2 123.0(3) . . ? C64 C59 P2 117.7(3) . . ? C59 C60 C61 120.1(4) . . ? C59 C60 H60 119.9 . . ? C61 C60 H60 119.9 . . ? C62 C61 C60 120.1(4) . . ? C62 C61 H61 120.0 . . ? C60 C61 H61 120.0 . . ? C63 C62 C61 119.9(4) . . ? C63 C62 H62 120.1 . . ? C61 C62 H62 120.1 . . ? C62 C63 C64 120.7(4) . . ? C62 C63 H63 119.7 . . ? C64 C63 H63 119.7 . . ? C63 C64 C59 119.9(4) . . ? C63 C64 H64 120.0 . . ? C59 C64 H64 120.0 . . ? F4 B1 F2 113.4(5) . . ? F4 B1 F1 111.2(4) . . ? F2 B1 F1 109.6(5) . . ? F4 B1 F3 105.2(6) . . ? F2 B1 F3 106.4(4) . . ? F1 B1 F3 111.0(5) . . ? B1 F4 Ag1 143.9(4) . 2_666 ? Cl2 C71 Cl1 121.9(6) . . ? Cl2 C71 H71A 106.8 . . ? Cl1 C71 H71A 106.8 . . ? Cl2 C71 H71B 106.8 . . ? Cl1 C71 H71B 106.8 . . ? H71A C71 H71B 106.7 . . ? Cl4 C72 Cl3 114.8(10) . . ? Cl4 C72 H72A 108.6 . . ? Cl3 C72 H72A 108.6 . . ? Cl4 C72 H72B 108.6 . . ? Cl3 C72 H72B 108.6 . . ? H72A C72 H72B 107.6 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag P2 Ag1 P1 C1 78.37(14) . . . . ? F4 Ag1 P1 C1 -149.3(2) 2_666 . . . ? P2 Ag1 P1 C41 -154.14(13) . . . . ? F4 Ag1 P1 C41 -21.8(2) 2_666 . . . ? P2 Ag1 P1 C47 -35.20(14) . . . . ? F4 Ag1 P1 C47 97.1(2) 2_666 . . . ? P1 Ag1 P2 C22 159.85(13) . . . . ? F4 Ag1 P2 C22 23.7(2) 2_666 . . . ? P1 Ag1 P2 C53 -79.97(14) . . . . ? F4 Ag1 P2 C53 143.9(2) 2_666 . . . ? P1 Ag1 P2 C59 39.77(16) . . . . ? F4 Ag1 P2 C59 -96.4(2) 2_666 . . . ? C41 P1 C1 C2 -3.6(4) . . . . ? C47 P1 C1 C2 -114.1(3) . . . . ? Ag1 P1 C1 C2 131.0(3) . . . . ? C41 P1 C1 C6 -179.1(3) . . . . ? C47 P1 C1 C6 70.4(3) . . . . ? Ag1 P1 C1 C6 -44.6(3) . . . . ? C6 C1 C2 C3 -1.8(5) . . . . ? P1 C1 C2 C3 -177.3(3) . . . . ? C1 C2 C3 C4 -0.4(5) . . . . ? C1 C2 C3 C7 173.6(3) . . . . ? C29 O1 C4 C3 109.5(4) . . . . ? C29 O1 C4 C5 -78.0(4) . . . . ? C2 C3 C4 O1 176.0(3) . . . . ? C7 C3 C4 O1 1.9(5) . . . . ? C2 C3 C4 C5 3.6(5) . . . . ? C7 C3 C4 C5 -170.5(3) . . . . ? O1 C4 C5 C6 -176.7(3) . . . . ? C3 C4 C5 C6 -4.4(5) . . . . ? O1 C4 C5 C28 -5.2(5) . . . . ? C3 C4 C5 C28 167.1(3) . . . . ? C4 C5 C6 C1 2.1(5) . . . . ? C28 C5 C6 C1 -169.3(3) . . . . ? C2 C1 C6 C5 1.0(5) . . . . ? P1 C1 C6 C5 176.8(3) . . . . ? C4 C3 C7 C10 69.8(4) . . . . ? C2 C3 C7 C10 -104.1(4) . . . . ? C13 C8 C9 C10 1.8(5) . . . . ? C8 C9 C10 C11 0.5(5) . . . . ? C8 C9 C10 C7 -176.7(3) . . . . ? C3 C7 C10 C9 60.2(4) . . . . ? C3 C7 C10 C11 -116.9(3) . . . . ? C32 O2 C11 C10 -102.0(4) . . . . ? C32 O2 C11 C12 80.8(4) . . . . ? C9 C10 C11 O2 179.3(3) . . . . ? C7 C10 C11 O2 -3.6(5) . . . . ? C9 C10 C11 C12 -3.5(5) . . . . ? C7 C10 C11 C12 173.6(3) . . . . ? O2 C11 C12 C13 -178.7(3) . . . . ? C10 C11 C12 C13 4.1(5) . . . . ? O2 C11 C12 C14 4.1(5) . . . . ? C10 C11 C12 C14 -173.2(3) . . . . ? C9 C8 C13 C12 -1.2(5) . . . . ? C11 C12 C13 C8 -1.6(5) . . . . ? C14 C12 C13 C8 175.7(3) . . . . ? C13 C12 C14 C19 -57.7(4) . . . . ? C11 C12 C14 C19 119.5(4) . . . . ? C20 C15 C16 C17 -2.0(6) . . . . ? C15 C16 C17 C18 -1.1(5) . . . . ? C15 C16 C17 C21 173.1(3) . . . . ? C35 O3 C18 C17 106.2(4) . . . . ? C35 O3 C18 C19 -79.2(4) . . . . ? C16 C17 C18 O3 179.0(3) . . . . ? C21 C17 C18 O3 4.8(5) . . . . ? C16 C17 C18 C19 4.6(5) . . . . ? C21 C17 C18 C19 -169.7(3) . . . . ? O3 C18 C19 C20 -179.3(3) . . . . ? C17 C18 C19 C20 -4.9(5) . . . . ? O3 C18 C19 C14 -3.5(5) . . . . ? C17 C18 C19 C14 170.9(3) . . . . ? C12 C14 C19 C20 105.3(4) . . . . ? C12 C14 C19 C18 -70.4(4) . . . . ? C16 C15 C20 C19 1.7(6) . . . . ? C18 C19 C20 C15 1.7(6) . . . . ? C14 C19 C20 C15 -174.1(4) . . . . ? C16 C17 C21 C26 -108.1(4) . . . . ? C18 C17 C21 C26 65.9(4) . . . . ? C53 P2 C22 C27 156.0(3) . . . . ? C59 P2 C22 C27 46.2(3) . . . . ? Ag1 P2 C22 C27 -78.2(3) . . . . ? C53 P2 C22 C23 -33.9(3) . . . . ? C59 P2 C22 C23 -143.7(3) . . . . ? Ag1 P2 C22 C23 91.9(3) . . . . ? C27 C22 C23 C24 4.0(5) . . . 2_657 ? P2 C22 C23 C24 -166.2(2) . . . 2_657 ? C38 O4 C25 C24 105.9(4) . . . . ? C38 O4 C25 C26 -75.2(4) . . . . ? C23 C24 C25 O4 -176.7(3) 2_657 . . . ? C28 C24 C25 O4 4.5(5) . . . . ? C23 C24 C25 C26 4.4(5) 2_657 . . . ? C28 C24 C25 C26 -174.4(3) . . . . ? O4 C25 C26 C27 174.3(3) . . . 2_657 ? C24 C25 C26 C27 -6.8(5) . . . 2_657 ? O4 C25 C26 C21 -9.5(5) . . . . ? C24 C25 C26 C21 169.4(3) . . . . ? C17 C21 C26 C27 56.7(4) . . . 2_657 ? C17 C21 C26 C25 -119.5(4) . . . . ? C23 C22 C27 C26 -1.5(5) . . . 2_657 ? P2 C22 C27 C26 168.8(3) . . . 2_657 ? C6 C5 C28 C24 103.7(4) . . . . ? C4 C5 C28 C24 -67.5(4) . . . . ? C23 C24 C28 C5 -52.1(4) 2_657 . . . ? C25 C24 C28 C5 126.7(3) . . . . ? C4 O1 C29 C30 -89.6(4) . . . . ? O1 C29 C30 C31 135.0(5) . . . . ? C11 O2 C32 C33 -168.4(3) . . . . ? O2 C32 C33 C34 -179.6(4) . . . . ? C18 O3 C35 C36 -85.6(5) . . . . ? O3 C35 C36 C37 -171.7(4) . . . . ? C25 O4 C38 C39 -74.0(4) . . . . ? O4 C38 C39 C40 116.4(5) . . . . ? C1 P1 C41 C46 120.8(3) . . . . ? C47 P1 C41 C46 -129.1(3) . . . . ? Ag1 P1 C41 C46 -9.4(3) . . . . ? C1 P1 C41 C42 -61.7(3) . . . . ? C47 P1 C41 C42 48.4(3) . . . . ? Ag1 P1 C41 C42 168.0(2) . . . . ? C46 C41 C42 C43 -0.9(5) . . . . ? P1 C41 C42 C43 -178.3(3) . . . . ? C41 C42 C43 C44 -0.3(5) . . . . ? C42 C43 C44 C45 1.3(6) . . . . ? C43 C44 C45 C46 -1.2(6) . . . . ? C42 C41 C46 C45 1.0(5) . . . . ? P1 C41 C46 C45 178.5(3) . . . . ? C44 C45 C46 C41 0.0(6) . . . . ? C1 P1 C47 C52 -151.2(3) . . . . ? C41 P1 C47 C52 97.0(3) . . . . ? Ag1 P1 C47 C52 -31.8(3) . . . . ? C1 P1 C47 C48 29.1(3) . . . . ? C41 P1 C47 C48 -82.7(3) . . . . ? Ag1 P1 C47 C48 148.5(3) . . . . ? C52 C47 C48 C49 -0.2(6) . . . . ? P1 C47 C48 C49 179.5(3) . . . . ? C47 C48 C49 C50 1.5(7) . . . . ? C48 C49 C50 C51 -1.7(7) . . . . ? C49 C50 C51 C52 0.4(7) . . . . ? C50 C51 C52 C47 1.0(6) . . . . ? C48 C47 C52 C51 -1.1(6) . . . . ? P1 C47 C52 C51 179.2(3) . . . . ? C22 P2 C53 C54 141.7(3) . . . . ? C59 P2 C53 C54 -106.6(3) . . . . ? Ag1 P2 C53 C54 18.6(3) . . . . ? C22 P2 C53 C58 -40.5(3) . . . . ? C59 P2 C53 C58 71.3(3) . . . . ? Ag1 P2 C53 C58 -163.5(3) . . . . ? C58 C53 C54 C55 -1.3(6) . . . . ? P2 C53 C54 C55 176.6(3) . . . . ? C53 C54 C55 C56 0.8(6) . . . . ? C54 C55 C56 C57 0.6(6) . . . . ? C55 C56 C57 C58 -1.3(6) . . . . ? C56 C57 C58 C53 0.8(6) . . . . ? C54 C53 C58 C57 0.6(5) . . . . ? P2 C53 C58 C57 -177.3(3) . . . . ? C22 P2 C59 C60 25.7(4) . . . . ? C53 P2 C59 C60 -85.5(4) . . . . ? Ag1 P2 C59 C60 148.3(3) . . . . ? C22 P2 C59 C64 -156.1(3) . . . . ? C53 P2 C59 C64 92.7(3) . . . . ? Ag1 P2 C59 C64 -33.5(4) . . . . ? C64 C59 C60 C61 -0.1(6) . . . . ? P2 C59 C60 C61 178.1(3) . . . . ? C59 C60 C61 C62 0.0(7) . . . . ? C60 C61 C62 C63 -0.2(7) . . . . ? C61 C62 C63 C64 0.4(7) . . . . ? C62 C63 C64 C59 -0.5(7) . . . . ? C60 C59 C64 C63 0.4(6) . . . . ? P2 C59 C64 C63 -177.9(4) . . . . ? F2 B1 F4 Ag1 24.4(11) . . . 2_666 ? F1 B1 F4 Ag1 148.4(6) . . . 2_666 ? F3 B1 F4 Ag1 -91.4(9) . . . 2_666 ? _diffrn_measured_fraction_theta_max 0.921 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.921 _refine_diff_density_max 2.145 _refine_diff_density_min -1.489 _refine_diff_density_rms 0.114 data_cj81010 _database_code_depnum_ccdc_archive 'CCDC 796779' #TrackingRef '- CCDC-796779-rvd3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C64.50 H62.50 Cl5.50 O4 P2 Pd2' _chemical_formula_weight 1371.36 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.9880(3) _cell_length_b 13.2820(3) _cell_length_c 22.6990(5) _cell_angle_alpha 95.162(2) _cell_angle_beta 103.609(2) _cell_angle_gamma 113.390(2) _cell_volume 3155.24(13) _cell_formula_units_Z 2 _cell_measurement_temperature 143(2) _cell_measurement_reflns_used 23798 _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 27.1 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.443 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1394 _exptl_absorpt_coefficient_mu 0.899 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 143(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD Saphire 3 Xcalibur' _diffrn_measurement_method 'omega scan' _diffrn_detector_area_resol_mean 19.64 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 44507 _diffrn_reflns_av_R_equivalents 0.0366 _diffrn_reflns_av_sigmaI/netI 0.0629 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.56 _diffrn_reflns_theta_max 27.00 _reflns_number_total 13748 _reflns_number_gt 9498 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd.,Version 1.171.26' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd.,Version 1.171.26' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd.,Version 1.171.26' _computing_structure_solution 'SIR-97_(Altomare & al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'MERCURY(CCDC, 2006)' _computing_publication_material 'WINGX (Farrugia, 1999)' _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. Due to some difficulties to refine the two disordered groups O2-C32-C33-C34 and O4-C38-C39-C40, it was necessary to use the following restraints : DFIX 1.4 C32A C33A DANG 1.4 C32A C33A DFIX 1.7 C33B C34B DANG 1.7 C33B C34B DFIX 1.5 C33A C34A DANG 1.5 C33A C34A DFIX 1.6 O4 C38B DANG 1.6 O4 C38B DFIX 1.6 C38B C39B DANG 1.6 C38B C39B DFIX 1.3 C39B C40B DANG 1.3 C39B C40B EADP C38A C38B Convergence was reached after 23 cycles with oscillating atom U parameter : Maximum = -0.232 for U23 C39B_b ; _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^)+(0.0901P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13748 _refine_ls_number_parameters 756 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0603 _refine_ls_R_factor_gt 0.0372 _refine_ls_wR_factor_ref 0.1225 _refine_ls_wR_factor_gt 0.1151 _refine_ls_goodness_of_fit_ref 0.834 _refine_ls_restrained_S_all 0.839 _refine_ls_shift/su_max 0.232 _refine_ls_shift/su_mean 0.006 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 0.36212(3) 0.29015(2) 0.810308(13) 0.02014(8) Uani 1 1 d . . . Pd2 Pd 0.22159(3) 0.31592(2) 0.665128(14) 0.02668(9) Uani 1 1 d . . . P1 P 0.55570(9) 0.31002(7) 0.86388(4) 0.01828(19) Uani 1 1 d . . . P2 P 0.29723(10) 0.37428(8) 0.58669(5) 0.0276(2) Uani 1 1 d . . . Cl1 Cl 0.28866(9) 0.18801(8) 0.87982(5) 0.0309(2) Uani 1 1 d . . . Cl2 Cl 0.42179(8) 0.39591(8) 0.73799(4) 0.02426(19) Uani 1 1 d . . . Cl3 Cl 0.15021(9) 0.25608(9) 0.75213(5) 0.0332(2) Uani 1 1 d . . . Cl4 Cl 0.01801(10) 0.24411(10) 0.60106(5) 0.0458(3) Uani 1 1 d . . . O1 O 1.0125(2) 0.5568(2) 0.78128(12) 0.0244(6) Uani 1 1 d . . . O2 O 1.0158(3) 0.7886(2) 0.87745(12) 0.0304(6) Uani 1 1 d . . . O3 O 0.8806(2) 0.9179(2) 0.80515(12) 0.0242(6) Uani 1 1 d . . . O4 O 0.8412(2) 0.6619(2) 0.71904(14) 0.0360(7) Uani 1 1 d D . . C1 C 0.6931(3) 0.3914(3) 0.83946(16) 0.0183(7) Uani 1 1 d . . . C2 C 0.6844(3) 0.3775(3) 0.77675(17) 0.0212(8) Uani 1 1 d . . . H2 H 0.6056 0.3277 0.7473 0.025 Uiso 1 1 calc R . . C3 C 0.7890(3) 0.4353(3) 0.75603(17) 0.0212(8) Uani 1 1 d . . . C4 C 0.9060(3) 0.5018(3) 0.80056(17) 0.0215(8) Uani 1 1 d . . . C5 C 0.9180(3) 0.5182(3) 0.86396(16) 0.0199(7) Uani 1 1 d . . . C6 C 0.8098(3) 0.4633(3) 0.88217(16) 0.0201(7) Uani 1 1 d . . . H6 H 0.8157 0.4751 0.9249 0.024 Uiso 1 1 calc R . . C7 C 1.0431(3) 0.5990(3) 0.91195(18) 0.0256(8) Uani 1 1 d . A . H7A H 1.0806 0.5561 0.9365 0.031 Uiso 1 1 calc R . . H7B H 1.1040 0.6426 0.8908 0.031 Uiso 1 1 calc R . . C8 C 0.9675(4) 0.7227(3) 1.04713(18) 0.0333(9) Uani 1 1 d . . . H8 H 0.9636 0.7115 1.0875 0.040 Uiso 1 1 calc R . . C9 C 1.0072(4) 0.6597(3) 1.01211(18) 0.0298(9) Uani 1 1 d . A . H9 H 1.0263 0.6029 1.0282 0.036 Uiso 1 1 calc R . . C10 C 1.0196(3) 0.6777(3) 0.95432(17) 0.0235(8) Uani 1 1 d . . . C11 C 0.9967(3) 0.7657(3) 0.93287(17) 0.0238(8) Uani 1 1 d . A . C12 C 0.9466(3) 0.8239(3) 0.96456(17) 0.0245(8) Uani 1 1 d . . . C13 C 0.9333(4) 0.8027(3) 1.02242(17) 0.0284(9) Uani 1 1 d . A . H13 H 0.9010 0.8428 1.0450 0.034 Uiso 1 1 calc R . . C14 C 0.8971(4) 0.9015(3) 0.93381(17) 0.0255(8) Uani 1 1 d . A . H14A H 0.8760 0.9439 0.9642 0.031 Uiso 1 1 calc R . . H14B H 0.9634 0.9560 0.9190 0.031 Uiso 1 1 calc R . . C15 C 0.5670(3) 0.6819(3) 0.84269(17) 0.0239(8) Uani 1 1 d . . . H15 H 0.4944 0.6290 0.8509 0.029 Uiso 1 1 calc R . . C16 C 0.6726(4) 0.7528(3) 0.89070(17) 0.0234(8) Uani 1 1 d . A . H16 H 0.6727 0.7474 0.9322 0.028 Uiso 1 1 calc R . . C17 C 0.7792(3) 0.8322(3) 0.87961(16) 0.0209(8) Uani 1 1 d . . . C18 C 0.7759(3) 0.8404(3) 0.81787(17) 0.0209(7) Uani 1 1 d . A . C19 C 0.6716(3) 0.7659(3) 0.76898(16) 0.0207(7) Uani 1 1 d . . . C20 C 0.5678(3) 0.6887(3) 0.78247(17) 0.0223(8) Uani 1 1 d . A . H20 H 0.4952 0.6390 0.7494 0.027 Uiso 1 1 calc R . . C21 C 0.6715(4) 0.7647(3) 0.70177(16) 0.0230(8) Uani 1 1 d . A . H21A H 0.6102 0.7920 0.6805 0.028 Uiso 1 1 calc R . . H21B H 0.7571 0.8149 0.7001 0.028 Uiso 1 1 calc R . . C22 C 0.4674(4) 0.4632(3) 0.61549(16) 0.0243(8) Uani 1 1 d . . . C23 C 0.5092(4) 0.5770(3) 0.63483(16) 0.0235(8) Uani 1 1 d . A . H23 H 0.4509 0.6091 0.6241 0.028 Uiso 1 1 calc R . . C24 C 0.6344(3) 0.6461(3) 0.66966(16) 0.0221(8) Uani 1 1 d . . . C25 C 0.7198(3) 0.5979(3) 0.68219(16) 0.0213(8) Uani 1 1 d . A . C26 C 0.6801(3) 0.4821(3) 0.66346(16) 0.0212(8) Uani 1 1 d . . . C27 C 0.5542(4) 0.4163(3) 0.63048(16) 0.0229(8) Uani 1 1 d . A . H27 H 0.5257 0.3379 0.6177 0.028 Uiso 1 1 calc R . . C28 C 0.7705(4) 0.4312(3) 0.68725(17) 0.0243(8) Uani 1 1 d . A . H28A H 0.8534 0.4736 0.6800 0.029 Uiso 1 1 calc R . . H28B H 0.7351 0.3525 0.6649 0.029 Uiso 1 1 calc R . . C29 C 1.0822(3) 0.4912(3) 0.77813(19) 0.0279(9) Uani 1 1 d . . . H29A H 1.0298 0.4225 0.7455 0.033 Uiso 1 1 calc R . . H29B H 1.1026 0.4686 0.8182 0.033 Uiso 1 1 calc R . . C30 C 1.2020(4) 0.5586(3) 0.76383(18) 0.0295(9) Uani 1 1 d . . . H30 H 1.2579 0.5247 0.7621 0.035 Uiso 1 1 calc R . . C31 C 1.2369(4) 0.6594(4) 0.7535(2) 0.0447(12) Uani 1 1 d . . . H31A H 1.1840 0.6967 0.7547 0.054 Uiso 1 1 calc R . . H31B H 1.3153 0.6960 0.7447 0.054 Uiso 1 1 calc R . . C32A C 1.1438(12) 0.8928(11) 0.8966(6) 0.036(3) Uani 0.538(11) 1 d PD A 1 H32A H 1.1432 0.9464 0.9296 0.043 Uiso 0.538(11) 1 calc PR A 1 H32B H 1.1517 0.9291 0.8606 0.043 Uiso 0.538(11) 1 calc PR A 1 C33A C 1.2576(9) 0.8719(10) 0.9191(5) 0.034(3) Uani 0.538(11) 1 d PD A 1 H33A H 1.2428 0.8223 0.9492 0.041 Uiso 0.538(11) 1 calc PR A 1 H33B H 1.2696 0.8323 0.8837 0.041 Uiso 0.538(11) 1 calc PR A 1 C34A C 1.3794(8) 0.9795(8) 0.9499(4) 0.046(3) Uani 0.538(11) 1 d PD A 1 H34A H 1.4499 0.9604 0.9665 0.060 Uiso 0.538(11) 1 calc PR A 1 H34B H 1.3669 1.0212 0.9837 0.060 Uiso 0.538(11) 1 calc PR A 1 H34C H 1.3993 1.0259 0.9192 0.060 Uiso 0.538(11) 1 calc PR A 1 C32B C 1.1084(15) 0.8888(15) 0.8709(7) 0.045(4) Uani 0.462(11) 1 d P A 2 H32C H 1.1278 0.9495 0.9057 0.054 Uiso 0.462(11) 1 calc PR A 2 H32D H 1.0740 0.9089 0.8320 0.054 Uiso 0.462(11) 1 calc PR A 2 C33B C 1.2245(10) 0.8804(10) 0.8698(5) 0.048(3) Uani 0.462(11) 1 d PD A 2 H33C H 1.2021 0.8083 0.8426 0.058 Uiso 0.462(11) 1 calc PR A 2 H33D H 1.2737 0.9414 0.8513 0.058 Uiso 0.462(11) 1 calc PR A 2 C34B C 1.3128(12) 0.8873(14) 0.9360(7) 0.053(4) Uani 0.462(11) 1 d PD A 2 H34D H 1.3887 0.8801 0.9313 0.074 Uiso 0.462(11) 1 calc PR A 2 H34E H 1.2656 0.8265 0.9545 0.074 Uiso 0.462(11) 1 calc PR A 2 H34F H 1.3385 0.9596 0.9628 0.074 Uiso 0.462(11) 1 calc PR A 2 C35 C 0.8925(4) 1.0315(3) 0.81235(18) 0.0265(8) Uani 1 1 d . . . H35A H 0.9826 1.0839 0.8192 0.032 Uiso 1 1 calc R . . H35B H 0.8685 1.0486 0.8496 0.032 Uiso 1 1 calc R . . C36 C 0.8115(4) 1.0508(3) 0.75768(19) 0.0335(9) Uani 1 1 d . . . H36A H 0.7215 0.9974 0.7499 0.040 Uiso 1 1 calc R . . H36B H 0.8372 1.0366 0.7206 0.040 Uiso 1 1 calc R . . C37 C 0.8238(4) 1.1714(3) 0.7681(2) 0.0393(10) Uani 1 1 d . . . H37A H 0.7699 1.1813 0.7315 0.059 Uiso 1 1 calc R . . H37B H 0.9127 1.2245 0.7751 0.059 Uiso 1 1 calc R . . H37C H 0.7968 1.1853 0.8043 0.059 Uiso 1 1 calc R . . C38A C 0.9284(13) 0.7123(10) 0.6784(9) 0.083 Uani 0.55 1 d P B 1 H38A H 0.9693 0.6640 0.6683 0.100 Uiso 0.548(10) 1 calc PR B 1 H38B H 0.8798 0.7223 0.6394 0.100 Uiso 0.548(10) 1 calc PR B 1 C39A C 1.0279(10) 0.8262(9) 0.7197(7) 0.082(5) Uani 0.548(10) 1 d P B 1 H39 H 1.0641 0.8254 0.7615 0.098 Uiso 0.548(10) 1 calc PR B 1 C40A C 1.0670(13) 0.9203(11) 0.7045(8) 0.112(6) Uani 0.548(10) 1 d P B 1 H40A H 1.0344 0.9264 0.6633 0.135 Uiso 0.548(10) 1 calc PR B 1 H40B H 1.1292 0.9851 0.7343 0.135 Uiso 0.548(10) 1 calc PR B 1 C38B C 0.9365(14) 0.7412(11) 0.6977(9) 0.083 Uani 0.45 1 d PD B 2 H38C H 1.0182 0.7733 0.7313 0.100 Uiso 0.452(10) 1 calc PR B 2 H38D H 0.9130 0.8033 0.6897 0.100 Uiso 0.452(10) 1 calc PR B 2 C39B C 0.957(2) 0.696(2) 0.6404(11) 0.181(14) Uani 0.452(10) 1 d PD B 2 H39B H 0.9674 0.6308 0.6272 0.217 Uiso 0.452(10) 1 calc PR B 2 C40B C 0.954(3) 0.781(3) 0.615(2) 0.30(3) Uani 0.452(10) 1 d PD B 2 H40C H 0.9423 0.8381 0.6376 0.364 Uiso 0.452(10) 1 calc PR B 2 H40D H 0.9647 0.7852 0.5754 0.364 Uiso 0.452(10) 1 calc PR B 2 C41 C 0.5591(4) 0.1744(3) 0.85967(17) 0.0230(8) Uani 1 1 d . . . C42 C 0.4651(4) 0.0833(3) 0.81473(19) 0.0322(9) Uani 1 1 d . . . H42 H 0.3962 0.0913 0.7883 0.039 Uiso 1 1 calc R . . C43 C 0.4707(5) -0.0189(4) 0.8080(2) 0.0457(12) Uani 1 1 d . . . H43 H 0.4069 -0.0803 0.7766 0.055 Uiso 1 1 calc R . . C44 C 0.5702(5) -0.0315(4) 0.8476(2) 0.0465(12) Uani 1 1 d . . . H44 H 0.5730 -0.1022 0.8441 0.056 Uiso 1 1 calc R . . C45 C 0.6652(4) 0.0592(4) 0.8921(2) 0.0378(11) Uani 1 1 d . . . H45 H 0.7334 0.0506 0.9188 0.045 Uiso 1 1 calc R . . C46 C 0.6613(4) 0.1621(3) 0.89767(19) 0.0290(9) Uani 1 1 d . . . H46 H 0.7280 0.2246 0.9274 0.035 Uiso 1 1 calc R . . C47 C 0.5957(3) 0.3739(3) 0.94453(16) 0.0213(8) Uani 1 1 d . . . C48 C 0.5918(4) 0.3139(3) 0.99095(17) 0.0261(8) Uani 1 1 d . . . H48 H 0.5672 0.2356 0.9815 0.031 Uiso 1 1 calc R . . C49 C 0.6241(4) 0.3687(4) 1.05181(18) 0.0332(9) Uani 1 1 d . . . H49 H 0.6231 0.3275 1.0839 0.040 Uiso 1 1 calc R . . C50 C 0.6574(4) 0.4815(4) 1.06628(18) 0.0316(9) Uani 1 1 d . . . H50 H 0.6802 0.5181 1.1081 0.038 Uiso 1 1 calc R . . C51 C 0.6577(4) 0.5414(3) 1.01959(19) 0.0318(9) Uani 1 1 d . . . H51 H 0.6785 0.6191 1.0291 0.038 Uiso 1 1 calc R . . C52 C 0.6275(3) 0.4879(3) 0.95886(18) 0.0258(8) Uani 1 1 d . . . H52 H 0.6286 0.5292 0.9268 0.031 Uiso 1 1 calc R . . C53 C 0.2772(4) 0.2625(4) 0.5268(2) 0.0399(11) Uani 1 1 d . . . C54 C 0.3646(5) 0.2784(4) 0.49396(19) 0.0419(11) Uani 1 1 d . . . H54 H 0.4353 0.3493 0.5020 0.050 Uiso 1 1 calc R . . C55 C 0.3497(6) 0.1919(4) 0.4496(2) 0.0530(13) Uani 1 1 d . . . H55 H 0.4101 0.2034 0.4273 0.064 Uiso 1 1 calc R . . C56 C 0.2491(7) 0.0912(5) 0.4381(3) 0.081(2) Uani 1 1 d . . . H56 H 0.2387 0.0319 0.4075 0.097 Uiso 1 1 calc R . . C57 C 0.1626(8) 0.0741(5) 0.4699(4) 0.106(3) Uani 1 1 d . . . H57 H 0.0921 0.0028 0.4613 0.128 Uiso 1 1 calc R . . C58 C 0.1755(6) 0.1578(5) 0.5141(3) 0.081(2) Uani 1 1 d . . . H58 H 0.1146 0.1443 0.5362 0.098 Uiso 1 1 calc R . . C59 C 0.2333(4) 0.4643(3) 0.55148(18) 0.0305(9) Uani 1 1 d . . . C60 C 0.1821(4) 0.5191(4) 0.5849(2) 0.0388(10) Uani 1 1 d . . . H60 H 0.1716 0.5013 0.6235 0.047 Uiso 1 1 calc R . . C61 C 0.1465(5) 0.5986(4) 0.5628(2) 0.0457(12) Uani 1 1 d . . . H61 H 0.1120 0.6356 0.5859 0.055 Uiso 1 1 calc R . . C62 C 0.1618(5) 0.6236(4) 0.5067(2) 0.0504(13) Uani 1 1 d . . . H62 H 0.1371 0.6781 0.4912 0.060 Uiso 1 1 calc R . . C63 C 0.2112(5) 0.5719(4) 0.4735(2) 0.0546(14) Uani 1 1 d . . . H63 H 0.2216 0.5909 0.4351 0.065 Uiso 1 1 calc R . . C64 C 0.2466(5) 0.4919(4) 0.4951(2) 0.0461(12) Uani 1 1 d . . . H64 H 0.2802 0.4553 0.4712 0.055 Uiso 1 1 calc R . . Cl11 Cl 0.3731(5) 0.1012(3) 0.65030(16) 0.1023(14) Uani 0.50 1 d P . . Cl12 Cl 0.3954(6) -0.1060(4) 0.6257(3) 0.144(2) Uani 0.50 1 d P . . Cl13 Cl 0.5683(5) 0.0955(4) 0.5974(2) 0.142(2) Uani 0.50 1 d P . . C71 C 0.4776 0.0447 0.6511 0.050 Uiso 0.50 1 d P . . H71 H 0.5370 0.0645 0.6939 0.060 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 Pd1 0.01826(15) 0.01825(14) 0.02652(16) 0.00582(11) 0.00942(12) 0.00867(11) Pd2 0.02068(16) 0.02289(16) 0.03195(18) 0.00618(12) 0.00315(13) 0.00741(12) P1 0.0197(5) 0.0166(4) 0.0222(5) 0.0062(4) 0.0092(4) 0.0094(4) P2 0.0266(5) 0.0229(5) 0.0245(5) 0.0008(4) 0.0001(4) 0.0070(4) Cl1 0.0278(5) 0.0304(5) 0.0355(5) 0.0121(4) 0.0172(4) 0.0082(4) Cl2 0.0199(4) 0.0260(5) 0.0271(5) 0.0098(4) 0.0064(4) 0.0095(4) Cl3 0.0197(5) 0.0370(5) 0.0469(6) 0.0178(5) 0.0121(4) 0.0131(4) Cl4 0.0250(5) 0.0440(6) 0.0484(7) 0.0099(5) -0.0065(5) 0.0046(5) O1 0.0208(13) 0.0252(13) 0.0376(15) 0.0136(12) 0.0168(12) 0.0143(11) O2 0.0364(16) 0.0295(15) 0.0334(15) 0.0169(12) 0.0161(13) 0.0168(13) O3 0.0224(13) 0.0163(12) 0.0323(14) 0.0053(11) 0.0090(11) 0.0064(11) O4 0.0216(15) 0.0312(16) 0.0476(18) 0.0002(13) 0.0035(13) 0.0094(13) C1 0.0193(18) 0.0170(17) 0.0243(19) 0.0082(14) 0.0087(15) 0.0115(15) C2 0.0200(18) 0.0208(18) 0.0253(19) 0.0027(15) 0.0067(15) 0.0118(15) C3 0.0237(19) 0.0212(18) 0.0257(19) 0.0067(15) 0.0106(16) 0.0144(16) C4 0.0218(19) 0.0201(18) 0.032(2) 0.0116(15) 0.0143(16) 0.0136(15) C5 0.0178(18) 0.0188(17) 0.0268(19) 0.0074(15) 0.0052(15) 0.0118(15) C6 0.0241(19) 0.0213(18) 0.0184(17) 0.0079(14) 0.0059(15) 0.0128(15) C7 0.0181(19) 0.026(2) 0.032(2) 0.0086(17) 0.0040(16) 0.0096(16) C8 0.037(2) 0.032(2) 0.021(2) 0.0042(17) -0.0004(18) 0.0105(19) C9 0.030(2) 0.027(2) 0.028(2) 0.0101(17) -0.0012(17) 0.0128(18) C10 0.0136(17) 0.0214(18) 0.028(2) 0.0030(15) -0.0024(15) 0.0049(15) C11 0.0166(18) 0.0216(19) 0.025(2) 0.0049(15) -0.0006(15) 0.0042(15) C12 0.0220(19) 0.0184(18) 0.025(2) 0.0020(15) -0.0029(16) 0.0067(15) C13 0.028(2) 0.024(2) 0.025(2) -0.0001(16) 0.0014(17) 0.0083(17) C14 0.026(2) 0.0188(18) 0.026(2) -0.0009(15) 0.0014(16) 0.0087(16) C15 0.0217(19) 0.0219(19) 0.030(2) 0.0041(16) 0.0099(16) 0.0100(16) C16 0.032(2) 0.0219(19) 0.0220(19) 0.0072(15) 0.0096(16) 0.0154(17) C17 0.0228(19) 0.0169(17) 0.0238(19) 0.0015(15) 0.0029(15) 0.0120(15) C18 0.0225(19) 0.0162(17) 0.0262(19) 0.0049(15) 0.0064(15) 0.0109(15) C19 0.0236(19) 0.0178(17) 0.0238(19) 0.0040(15) 0.0060(15) 0.0129(15) C20 0.0221(19) 0.0168(17) 0.026(2) 0.0010(15) 0.0040(15) 0.0092(15) C21 0.027(2) 0.0193(18) 0.025(2) 0.0045(15) 0.0066(16) 0.0121(16) C22 0.029(2) 0.0237(19) 0.0184(18) 0.0043(15) 0.0064(16) 0.0094(16) C23 0.026(2) 0.027(2) 0.0184(18) 0.0043(15) 0.0056(15) 0.0131(17) C24 0.029(2) 0.0217(18) 0.0186(18) 0.0075(15) 0.0105(16) 0.0114(16) C25 0.0214(19) 0.0223(18) 0.0195(18) 0.0030(15) 0.0073(15) 0.0083(15) C26 0.029(2) 0.0247(19) 0.0174(18) 0.0081(15) 0.0128(16) 0.0155(17) C27 0.034(2) 0.0190(18) 0.0174(18) 0.0037(14) 0.0099(16) 0.0117(16) C28 0.029(2) 0.027(2) 0.0232(19) 0.0063(16) 0.0133(16) 0.0143(17) C29 0.024(2) 0.028(2) 0.040(2) 0.0110(18) 0.0149(18) 0.0162(17) C30 0.024(2) 0.035(2) 0.035(2) 0.0022(18) 0.0119(17) 0.0169(18) C31 0.027(2) 0.035(3) 0.076(4) 0.011(2) 0.027(2) 0.011(2) C32A 0.040(8) 0.025(5) 0.044(7) 0.013(6) 0.014(6) 0.015(5) C33A 0.026(6) 0.047(6) 0.026(7) 0.013(5) 0.005(5) 0.012(6) C34A 0.034(5) 0.053(7) 0.049(6) 0.021(5) 0.016(4) 0.012(5) C32B 0.030(9) 0.048(7) 0.060(11) 0.038(9) 0.019(8) 0.012(7) C33B 0.040(6) 0.051(7) 0.059(9) 0.020(6) 0.021(6) 0.020(5) C34B 0.023(8) 0.067(10) 0.053(9) 0.027(7) -0.003(7) 0.009(9) C35 0.029(2) 0.0147(18) 0.033(2) 0.0031(16) 0.0090(17) 0.0066(16) C36 0.040(2) 0.026(2) 0.036(2) 0.0067(18) 0.0105(19) 0.0156(19) C37 0.047(3) 0.028(2) 0.053(3) 0.015(2) 0.021(2) 0.021(2) C38A 0.042 0.047 0.147 -0.015 0.047 0.003 C39A 0.039(6) 0.043(6) 0.146(12) -0.015(7) 0.046(7) -0.003(5) C40A 0.081(10) 0.057(8) 0.161(16) 0.021(9) 0.036(10) -0.009(7) C38B 0.042 0.047 0.147 -0.015 0.047 0.003 C39B 0.065(14) 0.14(2) 0.32(4) 0.02(3) 0.031(19) 0.047(14) C40B 0.15(3) 0.37(6) 0.47(7) 0.29(6) 0.07(3) 0.17(4) C41 0.030(2) 0.0199(18) 0.030(2) 0.0116(16) 0.0192(17) 0.0146(16) C42 0.039(2) 0.022(2) 0.035(2) 0.0035(17) 0.0125(19) 0.0135(18) C43 0.058(3) 0.024(2) 0.058(3) 0.002(2) 0.023(3) 0.020(2) C44 0.074(4) 0.031(2) 0.062(3) 0.019(2) 0.042(3) 0.035(3) C45 0.053(3) 0.045(3) 0.047(3) 0.029(2) 0.031(2) 0.039(2) C46 0.033(2) 0.031(2) 0.036(2) 0.0139(18) 0.0209(18) 0.0185(18) C47 0.0184(18) 0.0247(19) 0.0241(19) 0.0040(15) 0.0084(15) 0.0116(15) C48 0.031(2) 0.029(2) 0.027(2) 0.0092(16) 0.0158(17) 0.0173(18) C49 0.038(2) 0.049(3) 0.026(2) 0.0143(19) 0.0169(18) 0.027(2) C50 0.029(2) 0.043(2) 0.026(2) 0.0000(18) 0.0093(17) 0.0185(19) C51 0.028(2) 0.030(2) 0.038(2) -0.0002(18) 0.0125(18) 0.0135(18) C52 0.027(2) 0.025(2) 0.030(2) 0.0040(16) 0.0095(17) 0.0156(17) C53 0.045(3) 0.030(2) 0.033(2) -0.0023(19) 0.001(2) 0.012(2) C54 0.064(3) 0.033(2) 0.025(2) 0.0041(18) 0.006(2) 0.023(2) C55 0.083(4) 0.049(3) 0.028(2) 0.002(2) 0.010(3) 0.035(3) C56 0.113(6) 0.042(3) 0.065(4) -0.020(3) 0.019(4) 0.022(4) C57 0.106(6) 0.047(4) 0.123(6) -0.039(4) 0.052(5) -0.009(4) C58 0.073(4) 0.039(3) 0.096(5) -0.026(3) 0.033(4) -0.009(3) C59 0.026(2) 0.028(2) 0.027(2) 0.0017(17) -0.0028(17) 0.0078(17) C60 0.040(3) 0.048(3) 0.031(2) 0.012(2) 0.008(2) 0.023(2) C61 0.049(3) 0.049(3) 0.048(3) 0.015(2) 0.013(2) 0.030(2) C62 0.057(3) 0.052(3) 0.047(3) 0.018(2) 0.001(2) 0.035(3) C63 0.080(4) 0.062(3) 0.030(3) 0.018(2) 0.008(3) 0.042(3) C64 0.063(3) 0.050(3) 0.028(2) 0.007(2) 0.010(2) 0.029(3) Cl11 0.170(4) 0.058(2) 0.065(2) 0.0147(16) 0.023(2) 0.042(2) Cl12 0.155(5) 0.068(3) 0.194(5) -0.004(3) 0.057(4) 0.039(3) Cl13 0.161(5) 0.092(3) 0.138(4) -0.037(3) 0.007(4) 0.052(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 P1 2.2498(9) . ? Pd1 Cl1 2.2795(9) . ? Pd1 Cl2 2.3128(9) . ? Pd1 Cl3 2.4090(10) . ? Pd2 P2 2.2457(11) . ? Pd2 Cl4 2.2832(10) . ? Pd2 Cl2 2.3271(9) . ? Pd2 Cl3 2.4087(10) . ? P1 C41 1.812(4) . ? P1 C47 1.812(4) . ? P1 C1 1.821(3) . ? P2 C59 1.808(4) . ? P2 C22 1.818(4) . ? P2 C53 1.820(4) . ? O1 C4 1.391(4) . ? O1 C29 1.435(4) . ? O2 C11 1.370(4) . ? O2 C32B 1.402(16) . ? O2 C32A 1.533(14) . ? O3 C18 1.385(4) . ? O3 C35 1.449(4) . ? O4 C38B 1.431(12) . ? O4 C25 1.362(4) . ? O4 C38A 1.550(15) . ? C1 C6 1.394(5) . ? C1 C2 1.392(5) . ? C2 C3 1.400(5) . ? C2 H2 0.9500 . ? C3 C4 1.400(5) . ? C3 C28 1.517(5) . ? C4 C5 1.400(5) . ? C5 C6 1.393(5) . ? C5 C7 1.526(5) . ? C6 H6 0.9500 . ? C7 C10 1.509(5) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.390(6) . ? C8 C13 1.399(5) . ? C8 H8 0.9500 . ? C9 C10 1.385(5) . ? C9 H9 0.9500 . ? C10 C11 1.405(5) . ? C11 C12 1.395(5) . ? C12 C13 1.399(5) . ? C12 C14 1.525(5) . ? C13 H13 0.9500 . ? C14 C17 1.518(5) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.377(5) . ? C15 C20 1.380(5) . ? C15 H15 0.9500 . ? C16 C17 1.392(5) . ? C16 H16 0.9500 . ? C17 C18 1.408(5) . ? C18 C19 1.393(5) . ? C19 C20 1.385(5) . ? C19 C21 1.524(5) . ? C20 H20 0.9500 . ? C21 C24 1.515(5) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C23 1.380(5) . ? C22 C27 1.405(5) . ? C23 C24 1.392(5) . ? C23 H23 0.9500 . ? C24 C25 1.398(5) . ? C25 C26 1.408(5) . ? C26 C27 1.381(5) . ? C26 C28 1.514(5) . ? C27 H27 0.9500 . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 C30 1.490(5) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 C31 1.297(6) . ? C30 H30 0.9500 . ? C31 H31A 0.9500 . ? C31 H31B 0.9500 . ? C32A C33A 1.483(12) . ? C32A H32A 0.9900 . ? C32A H32B 0.9900 . ? C33A C34A 1.532(11) . ? C33A H33A 0.9900 . ? C33A H33B 0.9900 . ? C34A H34A 0.9800 . ? C34A H34B 0.9800 . ? C34A H34C 0.9800 . ? C32B C33B 1.446(19) . ? C32B H32C 0.9900 . ? C32B H32D 0.9900 . ? C33B C34B 1.592(12) . ? C33B H33C 0.9900 . ? C33B H33D 0.9900 . ? C34B H34D 0.9800 . ? C34B H34E 0.9800 . ? C34B H34F 0.9800 . ? C35 C36 1.495(5) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 C37 1.540(5) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38A C39A 1.542(16) . ? C38A H38A 0.9900 . ? C38A H38B 0.9900 . ? C39A C40A 1.260(17) . ? C39A H39 0.9500 . ? C40A H40A 0.9500 . ? C40A H40B 0.9500 . ? C38B C39B 1.499(16) . ? C38B H38C 0.9900 . ? C38B H38D 0.9900 . ? C39B C40B 1.319(16) . ? C39B H39B 0.9500 . ? C40B H40C 0.9500 . ? C40B H40D 0.9500 . ? C41 C42 1.389(5) . ? C41 C46 1.399(5) . ? C42 C43 1.382(6) . ? C42 H42 0.9500 . ? C43 C44 1.392(7) . ? C43 H43 0.9500 . ? C44 C45 1.385(7) . ? C44 H44 0.9500 . ? C45 C46 1.382(5) . ? C45 H45 0.9500 . ? C46 H46 0.9500 . ? C47 C48 1.375(5) . ? C47 C52 1.392(5) . ? C48 C49 1.390(5) . ? C48 H48 0.9500 . ? C49 C50 1.373(6) . ? C49 H49 0.9500 . ? C50 C51 1.381(6) . ? C50 H50 0.9500 . ? C51 C52 1.386(5) . ? C51 H51 0.9500 . ? C52 H52 0.9500 . ? C53 C54 1.385(7) . ? C53 C58 1.385(7) . ? C54 C55 1.382(6) . ? C54 H54 0.9500 . ? C55 C56 1.349(8) . ? C55 H55 0.9500 . ? C56 C57 1.359(9) . ? C56 H56 0.9500 . ? C57 C58 1.361(8) . ? C57 H57 0.9500 . ? C58 H58 0.9500 . ? C59 C60 1.399(6) . ? C59 C64 1.389(6) . ? C60 C61 1.378(6) . ? C60 H60 0.9500 . ? C61 C62 1.379(7) . ? C61 H61 0.9500 . ? C62 C63 1.353(7) . ? C62 H62 0.9500 . ? C63 C64 1.381(7) . ? C63 H63 0.9500 . ? C64 H64 0.9500 . ? Cl11 C71 1.694(5) . ? Cl12 C71 1.808(4) . ? Cl13 C71 1.819(6) . ? C71 H71 1.0000 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P1 Pd1 Cl1 85.97(3) . . ? P1 Pd1 Cl2 98.37(3) . . ? Cl1 Pd1 Cl2 175.36(3) . . ? P1 Pd1 Cl3 176.33(4) . . ? Cl1 Pd1 Cl3 91.94(4) . . ? Cl2 Pd1 Cl3 83.81(3) . . ? P2 Pd2 Cl4 90.36(4) . . ? P2 Pd2 Cl2 93.94(4) . . ? Cl4 Pd2 Cl2 174.18(4) . . ? P2 Pd2 Cl3 177.41(4) . . ? Cl4 Pd2 Cl3 92.22(4) . . ? Cl2 Pd2 Cl3 83.51(3) . . ? C41 P1 C47 108.76(17) . . ? C41 P1 C1 102.34(15) . . ? C47 P1 C1 104.94(17) . . ? C41 P1 Pd1 110.05(13) . . ? C47 P1 Pd1 110.96(11) . . ? C1 P1 Pd1 119.10(11) . . ? C59 P2 C22 103.48(18) . . ? C59 P2 C53 109.4(2) . . ? C22 P2 C53 105.7(2) . . ? C59 P2 Pd2 112.56(14) . . ? C22 P2 Pd2 110.16(12) . . ? C53 P2 Pd2 114.68(16) . . ? Pd1 Cl2 Pd2 95.86(3) . . ? Pd2 Cl3 Pd1 91.27(3) . . ? C4 O1 C29 111.7(3) . . ? C11 O2 C32B 124.3(8) . . ? C11 O2 C32A 103.5(6) . . ? C32B O2 C32A 23.8(6) . . ? C18 O3 C35 115.3(3) . . ? C38B O4 C25 122.9(9) . . ? C38B O4 C38A 19.6(7) . . ? C25 O4 C38A 109.6(7) . . ? C6 C1 C2 118.7(3) . . ? C6 C1 P1 121.7(3) . . ? C2 C1 P1 119.5(3) . . ? C3 C2 C1 121.5(3) . . ? C3 C2 H2 119.2 . . ? C1 C2 H2 119.2 . . ? C2 C3 C4 118.0(3) . . ? C2 C3 C28 119.7(3) . . ? C4 C3 C28 122.2(3) . . ? O1 C4 C3 119.2(3) . . ? O1 C4 C5 118.9(3) . . ? C3 C4 C5 121.8(3) . . ? C6 C5 C4 118.0(3) . . ? C6 C5 C7 120.3(3) . . ? C4 C5 C7 121.6(3) . . ? C1 C6 C5 121.9(3) . . ? C1 C6 H6 119.1 . . ? C5 C6 H6 119.1 . . ? C10 C7 C5 109.8(3) . . ? C10 C7 H7A 109.7 . . ? C5 C7 H7A 109.7 . . ? C10 C7 H7B 109.7 . . ? C5 C7 H7B 109.7 . . ? H7A C7 H7B 108.2 . . ? C9 C8 C13 119.4(4) . . ? C9 C8 H8 120.3 . . ? C13 C8 H8 120.3 . . ? C8 C9 C10 121.6(4) . . ? C8 C9 H9 119.2 . . ? C10 C9 H9 119.2 . . ? C9 C10 C11 118.1(3) . . ? C9 C10 C7 122.0(3) . . ? C11 C10 C7 119.7(3) . . ? O2 C11 C12 120.0(3) . . ? O2 C11 C10 118.6(3) . . ? C12 C11 C10 121.2(3) . . ? C11 C12 C13 119.0(3) . . ? C11 C12 C14 120.0(3) . . ? C13 C12 C14 120.8(3) . . ? C12 C13 C8 120.1(4) . . ? C12 C13 H13 120.0 . . ? C8 C13 H13 120.0 . . ? C17 C14 C12 109.2(3) . . ? C17 C14 H14A 109.8 . . ? C12 C14 H14A 109.8 . . ? C17 C14 H14B 109.8 . . ? C12 C14 H14B 109.8 . . ? H14A C14 H14B 108.3 . . ? C16 C15 C20 119.3(3) . . ? C16 C15 H15 120.3 . . ? C20 C15 H15 120.3 . . ? C15 C16 C17 121.2(3) . . ? C15 C16 H16 119.4 . . ? C17 C16 H16 119.4 . . ? C16 C17 C18 118.4(3) . . ? C16 C17 C14 119.1(3) . . ? C18 C17 C14 122.4(3) . . ? C19 C18 O3 119.3(3) . . ? C19 C18 C17 120.6(3) . . ? O3 C18 C17 119.9(3) . . ? C18 C19 C20 118.6(3) . . ? C18 C19 C21 121.7(3) . . ? C20 C19 C21 119.6(3) . . ? C15 C20 C19 121.7(3) . . ? C15 C20 H20 119.2 . . ? C19 C20 H20 119.2 . . ? C24 C21 C19 109.2(3) . . ? C24 C21 H21A 109.8 . . ? C19 C21 H21A 109.8 . . ? C24 C21 H21B 109.8 . . ? C19 C21 H21B 109.8 . . ? H21A C21 H21B 108.3 . . ? C23 C22 C27 119.0(3) . . ? C23 C22 P2 118.9(3) . . ? C27 C22 P2 120.7(3) . . ? C22 C23 C24 121.7(3) . . ? C22 C23 H23 119.1 . . ? C24 C23 H23 119.1 . . ? C23 C24 C25 118.0(3) . . ? C23 C24 C21 120.7(3) . . ? C25 C24 C21 120.5(3) . . ? O4 C25 C24 119.4(3) . . ? O4 C25 C26 118.6(3) . . ? C24 C25 C26 121.6(3) . . ? C27 C26 C25 118.3(3) . . ? C27 C26 C28 121.7(3) . . ? C25 C26 C28 119.4(3) . . ? C26 C27 C22 121.2(3) . . ? C26 C27 H27 119.4 . . ? C22 C27 H27 119.4 . . ? C26 C28 C3 109.0(3) . . ? C26 C28 H28A 109.9 . . ? C3 C28 H28A 109.9 . . ? C26 C28 H28B 109.9 . . ? C3 C28 H28B 109.9 . . ? H28A C28 H28B 108.3 . . ? O1 C29 C30 109.5(3) . . ? O1 C29 H29A 109.8 . . ? C30 C29 H29A 109.8 . . ? O1 C29 H29B 109.8 . . ? C30 C29 H29B 109.8 . . ? H29A C29 H29B 108.2 . . ? C31 C30 C29 125.9(4) . . ? C31 C30 H30 117.1 . . ? C29 C30 H30 117.1 . . ? C30 C31 H31A 120.0 . . ? C30 C31 H31B 120.0 . . ? H31A C31 H31B 120.0 . . ? O2 C32A C33A 115.3(9) . . ? O2 C32A H32A 108.4 . . ? C33A C32A H32A 108.4 . . ? O2 C32A H32B 108.4 . . ? C33A C32A H32B 108.4 . . ? H32A C32A H32B 107.5 . . ? C34A C33A C32A 113.1(10) . . ? C34A C33A H33A 109.0 . . ? C32A C33A H33A 109.0 . . ? C34A C33A H33B 109.0 . . ? C32A C33A H33B 109.0 . . ? H33A C33A H33B 107.8 . . ? C33A C34A H34A 109.5 . . ? C33A C34A H34B 109.5 . . ? H34A C34A H34B 109.5 . . ? C33A C34A H34C 109.5 . . ? H34A C34A H34C 109.5 . . ? H34B C34A H34C 109.5 . . ? O2 C32B C33B 112.3(12) . . ? O2 C32B H32C 109.1 . . ? C33B C32B H32C 109.1 . . ? O2 C32B H32D 109.1 . . ? C33B C32B H32D 109.1 . . ? H32C C32B H32D 107.9 . . ? C34B C33B C32B 114.4(11) . . ? C34B C33B H33C 108.6 . . ? C32B C33B H33C 108.7 . . ? C34B C33B H33D 108.7 . . ? C32B C33B H33D 108.7 . . ? H33C C33B H33D 107.6 . . ? C33B C34B H34D 109.5 . . ? C33B C34B H34E 109.5 . . ? H34D C34B H34E 109.5 . . ? C33B C34B H34F 109.5 . . ? H34D C34B H34F 109.5 . . ? H34E C34B H34F 109.5 . . ? O3 C35 C36 113.3(3) . . ? O3 C35 H35A 108.9 . . ? C36 C35 H35A 108.9 . . ? O3 C35 H35B 108.9 . . ? C36 C35 H35B 108.9 . . ? H35A C35 H35B 107.7 . . ? C35 C36 C37 111.6(3) . . ? C35 C36 H36A 109.3 . . ? C37 C36 H36A 109.3 . . ? C35 C36 H36B 109.3 . . ? C37 C36 H36B 109.3 . . ? H36A C36 H36B 108.0 . . ? C36 C37 H37A 109.5 . . ? C36 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C36 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C39A C38A O4 103.2(10) . . ? C39A C38A H38A 111.1 . . ? O4 C38A H38A 111.1 . . ? C39A C38A H38B 111.1 . . ? O4 C38A H38B 111.1 . . ? H38A C38A H38B 109.1 . . ? C40A C39A C38A 127.7(16) . . ? C40A C39A H39 116.1 . . ? C38A C39A H39 116.2 . . ? C39A C40A H40A 120.0 . . ? C39A C40A H40B 120.0 . . ? H40A C40A H40B 120.0 . . ? O4 C38B C39B 115.3(14) . . ? O4 C38B H38C 108.5 . . ? C39B C38B H38C 108.6 . . ? O4 C38B H38D 108.5 . . ? C39B C38B H38D 108.2 . . ? H38C C38B H38D 107.5 . . ? C40B C39B C38B 91(3) . . ? C40B C39B H39B 134.6 . . ? C38B C39B H39B 133.9 . . ? C39B C40B H40C 120.4 . . ? C39B C40B H40D 119.6 . . ? H40C C40B H40D 120.0 . . ? C42 C41 C46 119.1(3) . . ? C42 C41 P1 119.9(3) . . ? C46 C41 P1 120.8(3) . . ? C41 C42 C43 120.8(4) . . ? C41 C42 H42 119.6 . . ? C43 C42 H42 119.6 . . ? C44 C43 C42 119.7(4) . . ? C44 C43 H43 120.2 . . ? C42 C43 H43 120.2 . . ? C45 C44 C43 120.0(4) . . ? C45 C44 H44 120.0 . . ? C43 C44 H44 120.0 . . ? C44 C45 C46 120.3(4) . . ? C44 C45 H45 119.9 . . ? C46 C45 H45 119.9 . . ? C45 C46 C41 120.1(4) . . ? C45 C46 H46 119.9 . . ? C41 C46 H46 119.9 . . ? C48 C47 C52 119.5(3) . . ? C48 C47 P1 122.8(3) . . ? C52 C47 P1 117.6(3) . . ? C47 C48 C49 119.6(4) . . ? C47 C48 H48 120.2 . . ? C49 C48 H48 120.2 . . ? C50 C49 C48 121.1(4) . . ? C50 C49 H49 119.5 . . ? C48 C49 H49 119.5 . . ? C49 C50 C51 119.6(4) . . ? C49 C50 H50 120.2 . . ? C51 C50 H50 120.2 . . ? C52 C51 C50 119.8(4) . . ? C52 C51 H51 120.1 . . ? C50 C51 H51 120.1 . . ? C51 C52 C47 120.5(4) . . ? C51 C52 H52 119.8 . . ? C47 C52 H52 119.8 . . ? C54 C53 C58 118.1(5) . . ? C54 C53 P2 121.2(3) . . ? C58 C53 P2 120.7(4) . . ? C53 C54 C55 120.6(5) . . ? C53 C54 H54 119.7 . . ? C55 C54 H54 119.7 . . ? C56 C55 C54 119.7(6) . . ? C56 C55 H55 120.2 . . ? C54 C55 H55 120.2 . . ? C57 C56 C55 120.5(5) . . ? C57 C56 H56 119.8 . . ? C55 C56 H56 119.8 . . ? C56 C57 C58 120.9(6) . . ? C56 C57 H57 119.6 . . ? C58 C57 H57 119.6 . . ? C57 C58 C53 120.2(6) . . ? C57 C58 H58 119.9 . . ? C53 C58 H58 119.9 . . ? C60 C59 C64 118.1(4) . . ? C60 C59 P2 119.3(3) . . ? C64 C59 P2 122.2(3) . . ? C61 C60 C59 121.0(4) . . ? C61 C60 H60 119.5 . . ? C59 C60 H60 119.5 . . ? C62 C61 C60 118.9(5) . . ? C62 C61 H61 120.5 . . ? C60 C61 H61 120.5 . . ? C61 C62 C63 121.2(4) . . ? C61 C62 H62 119.4 . . ? C63 C62 H62 119.4 . . ? C62 C63 C64 120.3(5) . . ? C62 C63 H63 119.9 . . ? C64 C63 H63 119.9 . . ? C63 C64 C59 120.5(5) . . ? C63 C64 H64 119.8 . . ? C59 C64 H64 119.8 . . ? Cl11 C71 Cl12 111.0(2) . . ? Cl11 C71 Cl13 110.8(2) . . ? Cl12 C71 Cl13 106.1(2) . . ? Cl11 C71 H71 109.6 . . ? Cl12 C71 H71 109.6 . . ? Cl13 C71 H71 109.6 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Cl1 Pd1 P1 C41 62.98(12) . . . . ? Cl2 Pd1 P1 C41 -118.66(12) . . . . ? Cl3 Pd1 P1 C41 7.6(6) . . . . ? Cl1 Pd1 P1 C47 -57.45(13) . . . . ? Cl2 Pd1 P1 C47 120.91(13) . . . . ? Cl3 Pd1 P1 C47 -112.8(6) . . . . ? Cl1 Pd1 P1 C1 -179.40(13) . . . . ? Cl2 Pd1 P1 C1 -1.04(13) . . . . ? Cl3 Pd1 P1 C1 125.2(5) . . . . ? Cl4 Pd2 P2 C59 55.90(14) . . . . ? Cl2 Pd2 P2 C59 -120.16(14) . . . . ? Cl3 Pd2 P2 C59 -129.1(8) . . . . ? Cl4 Pd2 P2 C22 170.83(14) . . . . ? Cl2 Pd2 P2 C22 -5.24(14) . . . . ? Cl3 Pd2 P2 C22 -14.1(9) . . . . ? Cl4 Pd2 P2 C53 -70.08(17) . . . . ? Cl2 Pd2 P2 C53 113.86(17) . . . . ? Cl3 Pd2 P2 C53 105.0(9) . . . . ? P1 Pd1 Cl2 Pd2 158.91(3) . . . . ? Cl1 Pd1 Cl2 Pd2 -41.7(5) . . . . ? Cl3 Pd1 Cl2 Pd2 -18.11(4) . . . . ? P2 Pd2 Cl2 Pd1 -161.47(4) . . . . ? Cl4 Pd2 Cl2 Pd1 61.1(4) . . . . ? Cl3 Pd2 Cl2 Pd1 18.13(3) . . . . ? P2 Pd2 Cl3 Pd1 -8.4(9) . . . . ? Cl4 Pd2 Cl3 Pd1 166.68(4) . . . . ? Cl2 Pd2 Cl3 Pd1 -17.29(3) . . . . ? P1 Pd1 Cl3 Pd2 -109.2(5) . . . . ? Cl1 Pd1 Cl3 Pd2 -164.47(4) . . . . ? Cl2 Pd1 Cl3 Pd2 17.39(3) . . . . ? C41 P1 C1 C6 -98.2(3) . . . . ? C47 P1 C1 C6 15.4(3) . . . . ? Pd1 P1 C1 C6 140.3(2) . . . . ? C41 P1 C1 C2 78.2(3) . . . . ? C47 P1 C1 C2 -168.2(3) . . . . ? Pd1 P1 C1 C2 -43.3(3) . . . . ? C6 C1 C2 C3 -1.1(5) . . . . ? P1 C1 C2 C3 -177.6(3) . . . . ? C1 C2 C3 C4 4.5(5) . . . . ? C1 C2 C3 C28 -170.9(3) . . . . ? C29 O1 C4 C3 -92.4(4) . . . . ? C29 O1 C4 C5 90.1(4) . . . . ? C2 C3 C4 O1 177.7(3) . . . . ? C28 C3 C4 O1 -7.1(5) . . . . ? C2 C3 C4 C5 -4.9(5) . . . . ? C28 C3 C4 C5 170.4(3) . . . . ? O1 C4 C5 C6 179.3(3) . . . . ? C3 C4 C5 C6 1.9(5) . . . . ? O1 C4 C5 C7 2.9(5) . . . . ? C3 C4 C5 C7 -174.5(3) . . . . ? C2 C1 C6 C5 -2.1(5) . . . . ? P1 C1 C6 C5 174.3(3) . . . . ? C4 C5 C6 C1 1.7(5) . . . . ? C7 C5 C6 C1 178.2(3) . . . . ? C6 C5 C7 C10 -47.2(4) . . . . ? C4 C5 C7 C10 129.2(3) . . . . ? C13 C8 C9 C10 3.1(6) . . . . ? C8 C9 C10 C11 3.1(6) . . . . ? C8 C9 C10 C7 -170.6(4) . . . . ? C5 C7 C10 C9 98.5(4) . . . . ? C5 C7 C10 C11 -75.1(4) . . . . ? C32B O2 C11 C12 69.2(9) . . . . ? C32A O2 C11 C12 82.0(6) . . . . ? C32B O2 C11 C10 -115.5(9) . . . . ? C32A O2 C11 C10 -102.7(5) . . . . ? C9 C10 C11 O2 176.2(3) . . . . ? C7 C10 C11 O2 -10.0(5) . . . . ? C9 C10 C11 C12 -8.5(5) . . . . ? C7 C10 C11 C12 165.3(3) . . . . ? O2 C11 C12 C13 -177.1(3) . . . . ? C10 C11 C12 C13 7.7(5) . . . . ? O2 C11 C12 C14 8.0(5) . . . . ? C10 C11 C12 C14 -167.2(3) . . . . ? C11 C12 C13 C8 -1.3(6) . . . . ? C14 C12 C13 C8 173.5(3) . . . . ? C9 C8 C13 C12 -4.0(6) . . . . ? C11 C12 C14 C17 67.2(4) . . . . ? C13 C12 C14 C17 -107.6(4) . . . . ? C20 C15 C16 C17 1.0(5) . . . . ? C15 C16 C17 C18 1.4(5) . . . . ? C15 C16 C17 C14 -174.9(3) . . . . ? C12 C14 C17 C16 61.6(4) . . . . ? C12 C14 C17 C18 -114.6(4) . . . . ? C35 O3 C18 C19 103.7(4) . . . . ? C35 O3 C18 C17 -81.0(4) . . . . ? C16 C17 C18 C19 -4.2(5) . . . . ? C14 C17 C18 C19 172.0(3) . . . . ? C16 C17 C18 O3 -179.5(3) . . . . ? C14 C17 C18 O3 -3.3(5) . . . . ? O3 C18 C19 C20 179.8(3) . . . . ? C17 C18 C19 C20 4.4(5) . . . . ? O3 C18 C19 C21 2.1(5) . . . . ? C17 C18 C19 C21 -173.2(3) . . . . ? C16 C15 C20 C19 -0.8(5) . . . . ? C18 C19 C20 C15 -1.9(5) . . . . ? C21 C19 C20 C15 175.8(3) . . . . ? C18 C19 C21 C24 128.3(3) . . . . ? C20 C19 C21 C24 -49.4(4) . . . . ? C59 P2 C22 C23 31.5(3) . . . . ? C53 P2 C22 C23 146.5(3) . . . . ? Pd2 P2 C22 C23 -89.1(3) . . . . ? C59 P2 C22 C27 -162.1(3) . . . . ? C53 P2 C22 C27 -47.0(3) . . . . ? Pd2 P2 C22 C27 77.4(3) . . . . ? C27 C22 C23 C24 -1.1(5) . . . . ? P2 C22 C23 C24 165.5(3) . . . . ? C22 C23 C24 C25 3.2(5) . . . . ? C22 C23 C24 C21 -166.9(3) . . . . ? C19 C21 C24 C23 96.4(4) . . . . ? C19 C21 C24 C25 -73.4(4) . . . . ? C38B O4 C25 C24 -77.1(8) . . . . ? C38A O4 C25 C24 -93.2(7) . . . . ? C38B O4 C25 C26 109.9(8) . . . . ? C38A O4 C25 C26 93.8(7) . . . . ? C23 C24 C25 O4 -176.4(3) . . . . ? C21 C24 C25 O4 -6.2(5) . . . . ? C23 C24 C25 C26 -3.5(5) . . . . ? C21 C24 C25 C26 166.6(3) . . . . ? O4 C25 C26 C27 174.7(3) . . . . ? C24 C25 C26 C27 1.8(5) . . . . ? O4 C25 C26 C28 3.1(5) . . . . ? C24 C25 C26 C28 -169.8(3) . . . . ? C25 C26 C27 C22 0.3(5) . . . . ? C28 C26 C27 C22 171.7(3) . . . . ? C23 C22 C27 C26 -0.7(5) . . . . ? P2 C22 C27 C26 -167.1(3) . . . . ? C27 C26 C28 C3 -102.4(4) . . . . ? C25 C26 C28 C3 68.9(4) . . . . ? C2 C3 C28 C26 61.6(4) . . . . ? C4 C3 C28 C26 -113.6(4) . . . . ? C4 O1 C29 C30 -174.1(3) . . . . ? O1 C29 C30 C31 -2.3(6) . . . . ? C11 O2 C32A C33A 76.2(10) . . . . ? C32B O2 C32A C33A -131(3) . . . . ? O2 C32A C33A C34A -168.1(9) . . . . ? C11 O2 C32B C33B 95.2(13) . . . . ? C32A O2 C32B C33B 63(2) . . . . ? O2 C32B C33B C34B -77.4(16) . . . . ? C18 O3 C35 C36 -81.4(4) . . . . ? O3 C35 C36 C37 178.2(3) . . . . ? C38B O4 C38A C39A 12(3) . . . . ? C25 O4 C38A C39A 147.6(9) . . . . ? O4 C38A C39A C40A -133.7(14) . . . . ? C25 O4 C38B C39B -54.0(18) . . . . ? C38A O4 C38B C39B -3(3) . . . . ? O4 C38B C39B C40B 133(2) . . . . ? C47 P1 C41 C42 138.3(3) . . . . ? C1 P1 C41 C42 -111.0(3) . . . . ? Pd1 P1 C41 C42 16.6(3) . . . . ? C47 P1 C41 C46 -47.2(3) . . . . ? C1 P1 C41 C46 63.4(3) . . . . ? Pd1 P1 C41 C46 -169.0(3) . . . . ? C46 C41 C42 C43 1.0(6) . . . . ? P1 C41 C42 C43 175.6(3) . . . . ? C41 C42 C43 C44 1.3(7) . . . . ? C42 C43 C44 C45 -2.1(7) . . . . ? C43 C44 C45 C46 0.5(7) . . . . ? C44 C45 C46 C41 1.9(6) . . . . ? C42 C41 C46 C45 -2.7(5) . . . . ? P1 C41 C46 C45 -177.2(3) . . . . ? C41 P1 C47 C48 -16.9(4) . . . . ? C1 P1 C47 C48 -125.8(3) . . . . ? Pd1 P1 C47 C48 104.3(3) . . . . ? C41 P1 C47 C52 165.3(3) . . . . ? C1 P1 C47 C52 56.4(3) . . . . ? Pd1 P1 C47 C52 -73.5(3) . . . . ? C52 C47 C48 C49 -2.3(5) . . . . ? P1 C47 C48 C49 179.8(3) . . . . ? C47 C48 C49 C50 1.4(6) . . . . ? C48 C49 C50 C51 0.7(6) . . . . ? C49 C50 C51 C52 -1.7(6) . . . . ? C50 C51 C52 C47 0.7(6) . . . . ? C48 C47 C52 C51 1.3(5) . . . . ? P1 C47 C52 C51 179.3(3) . . . . ? C59 P2 C53 C54 84.2(4) . . . . ? C22 P2 C53 C54 -26.6(4) . . . . ? Pd2 P2 C53 C54 -148.2(3) . . . . ? C59 P2 C53 C58 -97.6(5) . . . . ? C22 P2 C53 C58 151.6(5) . . . . ? Pd2 P2 C53 C58 30.0(5) . . . . ? C58 C53 C54 C55 0.3(7) . . . . ? P2 C53 C54 C55 178.5(4) . . . . ? C53 C54 C55 C56 0.1(8) . . . . ? C54 C55 C56 C57 -0.2(10) . . . . ? C55 C56 C57 C58 -0.1(13) . . . . ? C56 C57 C58 C53 0.6(13) . . . . ? C54 C53 C58 C57 -0.6(10) . . . . ? P2 C53 C58 C57 -178.9(6) . . . . ? C22 P2 C59 C60 -98.0(4) . . . . ? C53 P2 C59 C60 149.6(3) . . . . ? Pd2 P2 C59 C60 20.9(4) . . . . ? C22 P2 C59 C64 74.2(4) . . . . ? C53 P2 C59 C64 -38.1(4) . . . . ? Pd2 P2 C59 C64 -166.9(3) . . . . ? C64 C59 C60 C61 -0.4(7) . . . . ? P2 C59 C60 C61 172.1(4) . . . . ? C59 C60 C61 C62 0.2(7) . . . . ? C60 C61 C62 C63 -0.3(8) . . . . ? C61 C62 C63 C64 0.6(8) . . . . ? C62 C63 C64 C59 -0.8(8) . . . . ? C60 C59 C64 C63 0.7(7) . . . . ? P2 C59 C64 C63 -171.6(4) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.217 _refine_diff_density_min -1.380 _refine_diff_density_rms 0.098 data_matt_au_cl _database_code_depnum_ccdc_archive 'CCDC 809315' #TrackingRef 'the_cif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C64 H62 Au2 Cl2 O4 P2' _chemical_formula_sum 'C64 H62 Au2 Cl2 O4 P2' _chemical_formula_weight 1421.91 _chemical_absolute_configuration . 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' Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 22.808(7) _cell_length_b 15.115(5) _cell_length_c 17.830(6) _cell_angle_alpha 90.00 _cell_angle_beta 95.811(10) _cell_angle_gamma 90.00 _cell_volume 6115(3) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 107496 _cell_measurement_theta_min 0.90 _cell_measurement_theta_max 27.57 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.544 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2800 _exptl_absorpt_coefficient_mu 4.976 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method '\p scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 107496 _diffrn_reflns_av_R_equivalents 0.1159 _diffrn_reflns_av_sigmaI/netI 0.1022 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 0.90 _diffrn_reflns_theta_max 27.57 _reflns_number_total 14099 _reflns_number_gt 8680 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V., 1998)' _computing_cell_refinement 'Denzo (Nonius B.V., 1998)' _computing_data_reduction 'Denzo (Nonius B.V., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON 98 (Spek, 1998)' _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. ; # start Validation Reply Form _vrf_PLAT220_matt_au_cl ; PROBLEM: Large Non-Solvent C Ueq(max)/Ueq(min) ... 5.59 Ratio RESPONSE: small disorder of the terminal groups ; _vrf_PLAT241_matt_au_cl ; PROBLEM: Check High Ueq as Compared to Neighbors for C54 RESPONSE: small disorder of the terminal groups ; _vrf_PLAT601_matt_au_cl ; PROBLEM: Structure Contains Solvent Accessible VOIDS of . 238.00 A**3 RESPONSE: disordered solvent molecule has been removed with squeeze procedure with PLATON software ; # end Validation Reply Form _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^)+(0.0429P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 14099 _refine_ls_number_parameters 667 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1121 _refine_ls_R_factor_gt 0.0556 _refine_ls_wR_factor_ref 0.1101 _refine_ls_wR_factor_gt 0.0957 _refine_ls_goodness_of_fit_ref 0.981 _refine_ls_restrained_S_all 0.985 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Au1 Au 0.172654(15) -0.13817(2) -0.135725(18) 0.04387(10) Uani 1 1 d . . . Au2 Au 0.403986(13) 0.167976(18) 0.077939(16) 0.03297(8) Uani 1 1 d . . . Cl1 Cl 0.39371(10) 0.05606(13) 0.16143(11) 0.0527(6) Uani 1 1 d . . . Cl2 Cl 0.10679(11) -0.19996(19) -0.22496(15) 0.0804(8) Uani 1 1 d . . . P1 P 0.23577(9) -0.07326(12) -0.04936(10) 0.0334(5) Uani 1 1 d . . . P2 P 0.41966(8) 0.28419(12) 0.00534(10) 0.0290(4) Uani 1 1 d . . . O1 O 0.1984(2) 0.4494(3) -0.1340(2) 0.0314(11) Uani 1 1 d . . . O2 O 0.15571(19) 0.2979(3) -0.0097(2) 0.0269(11) Uani 1 1 d . . . O3 O 0.1337(2) 0.3657(3) 0.1554(2) 0.0302(11) Uani 1 1 d . . . O4 O 0.2017(2) 0.5009(3) 0.0441(2) 0.0306(11) Uani 1 1 d . . . C1 C 0.3118(3) -0.0737(4) -0.0765(3) 0.0285(16) Uani 1 1 d . . . C2 C 0.3469(4) -0.0027(6) -0.0718(4) 0.051(2) Uani 1 1 d . . . H2 H 0.3329 0.0512 -0.0528 0.062 Uiso 1 1 calc . . . C3 C 0.4037(4) -0.0063(6) -0.0944(5) 0.061(3) Uani 1 1 d . . . H3 H 0.4280 0.0448 -0.0913 0.074 Uiso 1 1 calc . . . C4 C 0.4240(4) -0.0852(8) -0.1213(5) 0.058(3) Uani 1 1 d . . . H4 H 0.4623 -0.0887 -0.1376 0.070 Uiso 1 1 calc . . . C5 C 0.3877(5) -0.1593(7) -0.1241(5) 0.064(3) Uani 1 1 d . . . H5 H 0.4018 -0.2144 -0.1404 0.077 Uiso 1 1 calc . . . C6 C 0.3310(4) -0.1530(5) -0.1032(4) 0.048(2) Uani 1 1 d . . . H6 H 0.3057 -0.2030 -0.1072 0.058 Uiso 1 1 calc . . . C7 C 0.2405(4) -0.1250(5) 0.0417(4) 0.0391(19) Uani 1 1 d . . . C8 C 0.2871(4) -0.1050(5) 0.0962(4) 0.051(2) Uani 1 1 d . . . H8 H 0.3173 -0.0657 0.0844 0.061 Uiso 1 1 calc . . . C9 C 0.2891(4) -0.1419(6) 0.1669(5) 0.060(3) Uani 1 1 d . . . H9 H 0.3203 -0.1272 0.2041 0.072 Uiso 1 1 calc . . . C10 C 0.2462(5) -0.2000(6) 0.1838(5) 0.066(3) Uani 1 1 d . . . H10 H 0.2488 -0.2272 0.2321 0.080 Uiso 1 1 calc . . . C11 C 0.1986(5) -0.2194(6) 0.1308(6) 0.070(3) Uani 1 1 d . . . H11 H 0.1681 -0.2581 0.1429 0.084 Uiso 1 1 calc . . . C12 C 0.1969(4) -0.1818(5) 0.0612(5) 0.054(2) Uani 1 1 d . . . H12 H 0.1647 -0.1949 0.0248 0.065 Uiso 1 1 calc . . . C13 C 0.4602(3) 0.3648(5) 0.0658(4) 0.0309(16) Uani 1 1 d . . . C14 C 0.4314(3) 0.3997(5) 0.1244(4) 0.045(2) Uani 1 1 d . . . H14 H 0.3916 0.3846 0.1291 0.054 Uiso 1 1 calc . . . C15 C 0.4617(4) 0.4573(5) 0.1761(4) 0.053(2) Uani 1 1 d . . . H15 H 0.4422 0.4820 0.2158 0.064 Uiso 1 1 calc . . . C16 C 0.5189(4) 0.4781(5) 0.1698(5) 0.052(2) Uani 1 1 d . . . H16 H 0.5393 0.5169 0.2053 0.062 Uiso 1 1 calc . . . C17 C 0.5477(4) 0.4424(6) 0.1113(5) 0.057(2) Uani 1 1 d . . . H17 H 0.5879 0.4563 0.1075 0.069 Uiso 1 1 calc . . . C18 C 0.5178(4) 0.3869(5) 0.0588(4) 0.046(2) Uani 1 1 d . . . H18 H 0.5371 0.3642 0.0180 0.055 Uiso 1 1 calc . . . C19 C 0.4620(3) 0.2572(5) -0.0719(4) 0.0320(17) Uani 1 1 d . . . C20 C 0.4497(3) 0.2929(5) -0.1430(4) 0.0377(18) Uani 1 1 d . . . H20 H 0.4193 0.3356 -0.1520 0.045 Uiso 1 1 calc . . . C21 C 0.4817(4) 0.2666(6) -0.2011(4) 0.051(2) Uani 1 1 d . . . H21 H 0.4734 0.2917 -0.2498 0.061 Uiso 1 1 calc . . . C22 C 0.5255(4) 0.2041(6) -0.1886(5) 0.053(2) Uani 1 1 d . . . H22 H 0.5463 0.1843 -0.2290 0.063 Uiso 1 1 calc . . . C23 C 0.5388(4) 0.1708(6) -0.1181(6) 0.058(2) Uani 1 1 d . . . H23 H 0.5705 0.1300 -0.1092 0.070 Uiso 1 1 calc . . . C24 C 0.5078(3) 0.1947(5) -0.0603(4) 0.042(2) Uani 1 1 d . . . H24 H 0.5171 0.1692 -0.0118 0.050 Uiso 1 1 calc . . . C25 C 0.3539(3) 0.3385(4) -0.0365(4) 0.0263(15) Uani 1 1 d . . . C26 C 0.3446(3) 0.4287(4) -0.0309(4) 0.0276(16) Uani 1 1 d . . . H26 H 0.3736 0.4646 -0.0038 0.033 Uiso 1 1 calc . . . C27 C 0.2925(3) 0.4675(4) -0.0651(3) 0.0275(16) Uani 1 1 d . . . C28 C 0.2505(3) 0.4134(4) -0.1029(3) 0.0246(15) Uani 1 1 d . . . C29 C 0.2577(3) 0.3211(4) -0.1064(3) 0.0233(15) Uani 1 1 d . . . C30 C 0.3095(3) 0.2861(4) -0.0731(3) 0.0255(15) Uani 1 1 d . . . H30 H 0.3153 0.2239 -0.0750 0.031 Uiso 1 1 calc . . . C31 C 0.2092(3) 0.2604(4) -0.1399(3) 0.0261(15) Uani 1 1 d . . . H31A H 0.1725 0.2947 -0.1522 0.031 Uiso 1 1 calc . . . H31B H 0.2206 0.2337 -0.1870 0.031 Uiso 1 1 calc . . . C32 C 0.1987(3) 0.1883(4) -0.0840(3) 0.0221(14) Uani 1 1 d . . . C33 C 0.2176(3) 0.1023(4) -0.0918(4) 0.0276(16) Uani 1 1 d . . . H33 H 0.2320 0.0846 -0.1376 0.033 Uiso 1 1 calc . . . C34 C 0.2160(3) 0.0411(4) -0.0340(4) 0.0263(15) Uani 1 1 d . . . C35 C 0.1951(3) 0.0679(4) 0.0331(4) 0.0303(16) Uani 1 1 d . . . H35 H 0.1951 0.0271 0.0736 0.036 Uiso 1 1 calc . . . C36 C 0.1740(3) 0.1536(4) 0.0418(3) 0.0243(15) Uani 1 1 d . . . C37 C 0.1749(3) 0.2119(5) -0.0175(3) 0.0273(16) Uani 1 1 d . . . C38 C 0.1579(3) 0.1864(4) 0.1176(3) 0.0294(16) Uani 1 1 d . . . H38A H 0.1198 0.2181 0.1105 0.035 Uiso 1 1 calc . . . H38B H 0.1533 0.1353 0.1511 0.035 Uiso 1 1 calc . . . C39 C 0.2048(3) 0.2480(4) 0.1542(3) 0.0238(15) Uani 1 1 d . . . C40 C 0.2620(3) 0.2187(4) 0.1715(4) 0.0292(16) Uani 1 1 d . . . H40 H 0.2716 0.1590 0.1614 0.035 Uiso 1 1 calc . . . C41 C 0.3058(3) 0.2756(5) 0.2036(4) 0.0337(18) Uani 1 1 d . . . H41 H 0.3446 0.2545 0.2173 0.040 Uiso 1 1 calc . . . C42 C 0.2918(3) 0.3638(5) 0.2151(4) 0.0354(18) Uani 1 1 d . . . H42 H 0.3218 0.4029 0.2357 0.042 Uiso 1 1 calc . . . C43 C 0.2353(3) 0.3962(5) 0.1975(3) 0.0286(16) Uani 1 1 d . . . C44 C 0.1917(3) 0.3357(5) 0.1684(3) 0.0264(15) Uani 1 1 d . . . C45 C 0.2231(3) 0.4934(5) 0.2050(4) 0.0373(19) Uani 1 1 d . . . H45A H 0.2318 0.5114 0.2584 0.045 Uiso 1 1 calc . . . H45B H 0.1809 0.5050 0.1898 0.045 Uiso 1 1 calc . . . C46 C 0.2603(3) 0.5472(5) 0.1564(4) 0.0366(18) Uani 1 1 d . . . C47 C 0.3104(4) 0.5927(5) 0.1877(4) 0.048(2) Uani 1 1 d . . . H47 H 0.3190 0.5938 0.2410 0.057 Uiso 1 1 calc . . . C48 C 0.3475(4) 0.6357(5) 0.1438(5) 0.050(2) Uani 1 1 d . . . H48 H 0.3796 0.6694 0.1667 0.060 Uiso 1 1 calc . . . C49 C 0.3381(3) 0.6301(5) 0.0673(5) 0.0400(19) Uani 1 1 d . . . H49 H 0.3650 0.6571 0.0370 0.048 Uiso 1 1 calc . . . C50 C 0.2886(3) 0.5843(4) 0.0329(4) 0.0309(17) Uani 1 1 d . . . C51 C 0.2497(3) 0.5471(4) 0.0786(4) 0.0277(16) Uani 1 1 d . . . C52 C 0.2816(3) 0.5659(4) -0.0522(4) 0.0340(17) Uani 1 1 d . . . H52A H 0.2413 0.5821 -0.0738 0.041 Uiso 1 1 calc . . . H52B H 0.3101 0.6019 -0.0774 0.041 Uiso 1 1 calc . . . C53 C 0.1990(4) 0.4773(5) -0.2106(4) 0.045(2) Uani 1 1 d . . . H53A H 0.2229 0.5317 -0.2131 0.054 Uiso 1 1 calc . . . H53B H 0.2164 0.4305 -0.2404 0.054 Uiso 1 1 calc . . . C54 C 0.1395(5) 0.4938(9) -0.2398(5) 0.123(6) Uani 1 1 d D . . H54 H 0.1143 0.4446 -0.2343 0.147 Uiso 1 1 calc . . . C55 C 0.1108(5) 0.5640(8) -0.2737(6) 0.096(4) Uani 1 1 d D . . H55A H 0.1317 0.6168 -0.2821 0.116 Uiso 1 1 calc . . . H55B H 0.0697 0.5603 -0.2891 0.116 Uiso 1 1 calc . . . C56 C 0.0913(3) 0.3069(5) -0.0188(4) 0.0391(19) Uani 1 1 d . . . H56A H 0.0790 0.3493 0.0189 0.047 Uiso 1 1 calc . . . H56B H 0.0731 0.2489 -0.0096 0.047 Uiso 1 1 calc . . . C57 C 0.0701(4) 0.3379(6) -0.0951(4) 0.050(2) Uani 1 1 d . . . H57 H 0.0863 0.3909 -0.1129 0.060 Uiso 1 1 calc . . . C58 C 0.0300(4) 0.2961(7) -0.1396(5) 0.068(3) Uani 1 1 d . . . H58A H 0.0131 0.2430 -0.1231 0.082 Uiso 1 1 calc . . . H58B H 0.0178 0.3189 -0.1883 0.082 Uiso 1 1 calc . . . C59 C 0.1017(3) 0.3545(5) 0.2212(4) 0.045(2) Uani 1 1 d . . . H59A H 0.1172 0.3957 0.2616 0.054 Uiso 1 1 calc . . . H59B H 0.1067 0.2933 0.2406 0.054 Uiso 1 1 calc . . . C60 C 0.0363(4) 0.3735(6) 0.1984(5) 0.061(3) Uani 1 1 d . . . H60A H 0.0220 0.3342 0.1560 0.073 Uiso 1 1 calc . . . H60B H 0.0136 0.3597 0.2414 0.073 Uiso 1 1 calc . . . C61 C 0.0254(4) 0.4670(7) 0.1755(6) 0.078(3) Uani 1 1 d . . . H61A H 0.0453 0.5064 0.2137 0.116 Uiso 1 1 calc . . . H61B H -0.0171 0.4788 0.1707 0.116 Uiso 1 1 calc . . . H61C H 0.0408 0.4776 0.1269 0.116 Uiso 1 1 calc . . . C62 C 0.1467(3) 0.5464(5) 0.0440(4) 0.044(2) Uani 1 1 d . . . H62A H 0.1472 0.5807 0.0913 0.053 Uiso 1 1 calc . . . H62B H 0.1148 0.5020 0.0438 0.053 Uiso 1 1 calc . . . C63 C 0.1328(4) 0.6073(6) -0.0204(4) 0.050(2) Uani 1 1 d . . . H63A H 0.1315 0.5735 -0.0681 0.060 Uiso 1 1 calc . . . H63B H 0.1644 0.6522 -0.0207 0.060 Uiso 1 1 calc . . . C64 C 0.0743(4) 0.6534(7) -0.0162(5) 0.073(3) Uani 1 1 d . . . H64A H 0.0464 0.6121 0.0032 0.109 Uiso 1 1 calc . . . H64B H 0.0589 0.6734 -0.0667 0.109 Uiso 1 1 calc . . . H64C H 0.0799 0.7045 0.0176 0.109 Uiso 1 1 calc . . . 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 Au1 0.0458(2) 0.04011(19) 0.04554(19) -0.01339(14) 0.00408(15) -0.00271(15) Au2 0.03244(17) 0.03100(16) 0.03392(15) 0.00216(13) -0.00418(12) 0.00413(14) Cl1 0.0661(15) 0.0434(12) 0.0462(12) 0.0123(9) -0.0069(10) 0.0051(11) Cl2 0.0634(17) 0.094(2) 0.0812(18) -0.0457(15) -0.0080(14) -0.0074(15) P1 0.0408(12) 0.0273(10) 0.0323(10) -0.0020(8) 0.0044(9) 0.0009(9) P2 0.0234(10) 0.0296(10) 0.0331(10) -0.0018(8) -0.0012(8) 0.0030(8) O1 0.024(3) 0.042(3) 0.029(3) 0.008(2) 0.007(2) 0.014(2) O2 0.023(3) 0.033(3) 0.024(2) 0.001(2) 0.002(2) 0.005(2) O3 0.029(3) 0.040(3) 0.022(2) 0.003(2) 0.006(2) 0.008(2) O4 0.029(3) 0.030(3) 0.033(3) 0.000(2) 0.006(2) 0.003(2) C1 0.035(4) 0.029(4) 0.020(3) -0.002(3) -0.001(3) 0.005(3) C2 0.037(5) 0.070(6) 0.048(5) -0.004(4) 0.009(4) 0.016(5) C3 0.041(6) 0.072(7) 0.072(7) 0.001(5) 0.009(5) -0.007(5) C4 0.039(6) 0.093(8) 0.041(5) 0.007(5) -0.001(4) 0.023(6) C5 0.064(7) 0.077(7) 0.050(6) -0.007(5) 0.000(5) 0.047(6) C6 0.053(6) 0.051(6) 0.040(5) 0.003(4) 0.005(4) 0.015(4) C7 0.052(5) 0.025(4) 0.042(5) 0.000(3) 0.014(4) 0.009(4) C8 0.062(6) 0.050(5) 0.042(5) 0.016(4) 0.011(4) 0.011(5) C9 0.061(7) 0.072(7) 0.047(5) 0.011(5) 0.003(5) 0.027(5) C10 0.107(9) 0.047(6) 0.049(6) 0.023(5) 0.029(6) 0.035(6) C11 0.116(10) 0.038(5) 0.062(7) -0.003(5) 0.037(6) -0.008(6) C12 0.077(7) 0.040(5) 0.047(5) -0.001(4) 0.008(5) -0.009(5) C13 0.024(4) 0.037(4) 0.031(4) 0.005(3) 0.001(3) -0.004(3) C14 0.035(5) 0.059(5) 0.042(5) -0.008(4) 0.009(4) -0.012(4) C15 0.068(7) 0.048(5) 0.040(5) -0.012(4) -0.010(4) -0.002(5) C16 0.060(6) 0.050(5) 0.043(5) -0.001(4) -0.012(4) -0.025(5) C17 0.038(5) 0.076(7) 0.058(6) 0.010(5) 0.004(4) -0.028(5) C18 0.040(5) 0.057(6) 0.041(5) -0.001(4) 0.005(4) -0.009(4) C19 0.022(4) 0.031(4) 0.043(4) -0.003(3) 0.002(3) 0.001(3) C20 0.023(4) 0.041(5) 0.048(5) -0.001(4) -0.001(4) 0.005(3) C21 0.044(6) 0.066(6) 0.044(5) -0.001(4) 0.011(4) 0.000(5) C22 0.044(6) 0.065(6) 0.052(6) -0.027(5) 0.022(4) -0.008(5) C23 0.037(5) 0.050(6) 0.089(7) -0.017(5) 0.010(5) 0.012(4) C24 0.033(5) 0.043(5) 0.050(5) -0.006(4) 0.008(4) 0.007(4) C25 0.019(4) 0.030(4) 0.030(4) -0.003(3) 0.005(3) -0.001(3) C26 0.030(4) 0.028(4) 0.027(4) -0.003(3) 0.013(3) -0.006(3) C27 0.038(4) 0.026(4) 0.022(3) 0.003(3) 0.017(3) 0.002(3) C28 0.025(4) 0.029(4) 0.021(3) 0.000(3) 0.009(3) 0.007(3) C29 0.023(4) 0.027(4) 0.021(3) 0.001(3) 0.005(3) 0.003(3) C30 0.031(4) 0.026(4) 0.020(3) -0.002(3) 0.005(3) 0.004(3) C31 0.028(4) 0.031(4) 0.019(3) 0.000(3) -0.001(3) 0.002(3) C32 0.023(4) 0.024(4) 0.018(3) -0.002(3) -0.004(3) 0.000(3) C33 0.026(4) 0.029(4) 0.027(4) -0.003(3) -0.001(3) -0.004(3) C34 0.026(4) 0.026(4) 0.028(4) -0.001(3) 0.005(3) 0.000(3) C35 0.033(4) 0.026(4) 0.032(4) 0.004(3) 0.004(3) -0.001(3) C36 0.021(4) 0.030(4) 0.023(3) 0.000(3) 0.006(3) -0.004(3) C37 0.023(4) 0.037(4) 0.021(3) -0.001(3) 0.001(3) 0.000(3) C38 0.036(4) 0.032(4) 0.021(3) 0.005(3) 0.011(3) 0.007(3) C39 0.031(4) 0.028(4) 0.014(3) -0.003(3) 0.008(3) 0.005(3) C40 0.037(5) 0.027(4) 0.025(4) 0.002(3) 0.009(3) 0.006(3) C41 0.034(5) 0.045(5) 0.023(4) 0.001(3) 0.010(3) 0.013(4) C42 0.042(5) 0.041(4) 0.024(4) -0.004(3) 0.006(3) -0.006(4) C43 0.032(4) 0.038(4) 0.017(3) -0.001(3) 0.009(3) 0.012(3) C44 0.026(4) 0.038(4) 0.016(3) 0.006(3) 0.002(3) 0.008(3) C45 0.050(5) 0.034(4) 0.028(4) -0.007(3) 0.009(4) 0.004(4) C46 0.048(5) 0.030(4) 0.032(4) -0.008(3) 0.011(4) 0.003(4) C47 0.061(6) 0.033(5) 0.046(5) -0.016(4) -0.008(4) 0.001(4) C48 0.049(6) 0.041(5) 0.061(6) -0.011(4) 0.005(5) -0.013(4) C49 0.038(5) 0.025(4) 0.060(5) -0.007(4) 0.016(4) -0.008(4) C50 0.036(4) 0.017(4) 0.041(4) -0.007(3) 0.006(3) 0.009(3) C51 0.039(4) 0.015(3) 0.030(4) -0.001(3) 0.007(3) 0.002(3) C52 0.036(5) 0.023(4) 0.045(4) 0.003(3) 0.012(4) -0.001(3) C53 0.051(6) 0.057(5) 0.028(4) 0.003(4) 0.008(4) 0.017(4) C54 0.103(10) 0.232(16) 0.039(6) 0.039(8) 0.031(6) 0.091(11) C55 0.078(9) 0.133(11) 0.079(8) 0.040(7) 0.018(6) 0.006(8) C56 0.031(5) 0.050(5) 0.037(4) -0.001(3) 0.002(3) 0.020(4) C57 0.036(5) 0.069(6) 0.045(5) 0.011(4) 0.004(4) 0.018(5) C58 0.053(6) 0.099(8) 0.049(6) -0.011(5) -0.012(5) 0.016(6) C59 0.035(5) 0.070(6) 0.030(4) 0.011(4) 0.010(3) 0.022(4) C60 0.048(6) 0.065(6) 0.072(6) 0.014(5) 0.020(5) 0.018(5) C61 0.063(7) 0.072(7) 0.103(8) 0.026(6) 0.033(6) 0.029(6) C62 0.039(5) 0.050(5) 0.044(5) -0.003(4) 0.004(4) 0.002(4) C63 0.035(5) 0.067(6) 0.049(5) 0.005(4) 0.007(4) 0.014(4) C64 0.056(7) 0.088(8) 0.073(7) 0.001(5) -0.002(5) 0.033(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Au1 P1 2.227(2) . ? Au1 Cl2 2.275(2) . ? Au2 P2 2.2322(19) . ? Au2 Cl1 2.281(2) . ? P1 C7 1.796(7) . ? P1 C34 1.814(7) . ? P1 C1 1.846(7) . ? P2 C25 1.804(7) . ? P2 C19 1.807(7) . ? P2 C13 1.817(7) . ? O1 C28 1.371(7) . ? O1 C53 1.432(8) . ? O2 C37 1.383(8) . ? O2 C56 1.468(8) . ? O3 C44 1.394(7) . ? O3 C59 1.454(8) . ? O4 C51 1.388(8) . ? O4 C62 1.430(8) . ? C1 C2 1.336(10) . ? C1 C6 1.378(10) . ? C2 C3 1.396(11) . ? C2 H2 0.9500 . ? C3 C4 1.382(12) . ? C3 H3 0.9500 . ? C4 C5 1.391(13) . ? C4 H4 0.9500 . ? C5 C6 1.383(12) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C12 1.384(11) . ? C7 C8 1.398(11) . ? C8 C9 1.375(11) . ? C8 H8 0.9500 . ? C9 C10 1.370(13) . ? C9 H9 0.9500 . ? C10 C11 1.396(14) . ? C10 H10 0.9500 . ? C11 C12 1.362(12) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C18 1.374(10) . ? C13 C14 1.391(10) . ? C14 C15 1.399(10) . ? C14 H14 0.9500 . ? C15 C16 1.355(12) . ? C15 H15 0.9500 . ? C16 C17 1.396(12) . ? C16 H16 0.9500 . ? C17 C18 1.384(11) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 C20 1.381(9) . ? C19 C24 1.408(9) . ? C20 C21 1.385(10) . ? C20 H20 0.9500 . ? C21 C22 1.377(11) . ? C21 H21 0.9500 . ? C22 C23 1.359(12) . ? C22 H22 0.9500 . ? C23 C24 1.358(11) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C25 C26 1.384(9) . ? C25 C30 1.395(9) . ? C26 C27 1.407(9) . ? C26 H26 0.9500 . ? C27 C28 1.383(9) . ? C27 C52 1.529(9) . ? C28 C29 1.406(9) . ? C29 C30 1.374(9) . ? C29 C31 1.512(9) . ? C30 H30 0.9500 . ? C31 C32 1.511(8) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 C33 1.382(9) . ? C32 C37 1.401(8) . ? C33 C34 1.387(9) . ? C33 H33 0.9500 . ? C34 C35 1.392(9) . ? C35 C36 1.396(9) . ? C35 H35 0.9500 . ? C36 C37 1.378(8) . ? C36 C38 1.519(8) . ? C38 C39 1.515(9) . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C39 C40 1.381(9) . ? C39 C44 1.389(9) . ? C40 C41 1.397(9) . ? C40 H40 0.9500 . ? C41 C42 1.391(10) . ? C41 H41 0.9500 . ? C42 C43 1.384(9) . ? C42 H42 0.9500 . ? C43 C44 1.411(9) . ? C43 C45 1.504(9) . ? C45 C46 1.511(10) . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C46 C51 1.384(9) . ? C46 C47 1.400(10) . ? C47 C48 1.374(11) . ? C47 H47 0.9500 . ? C48 C49 1.361(11) . ? C48 H48 0.9500 . ? C49 C50 1.411(10) . ? C49 H49 0.9500 . ? C50 C51 1.384(9) . ? C50 C52 1.535(9) . ? C52 H52A 0.9900 . ? C52 H52B 0.9900 . ? C53 C54 1.426(13) . ? C53 H53A 0.9900 . ? C53 H53B 0.9900 . ? C54 C55 1.357(8) . ? C54 H54 0.9500 . ? C55 H55A 0.9500 . ? C55 H55B 0.9500 . ? C56 C57 1.473(10) . ? C56 H56A 0.9900 . ? C56 H56B 0.9900 . ? C57 C58 1.310(12) . ? C57 H57 0.9500 . ? C58 H58A 0.9500 . ? C58 H58B 0.9500 . ? C59 C60 1.532(11) . ? C59 H59A 0.9900 . ? C59 H59B 0.9900 . ? C60 C61 1.486(12) . ? C60 H60A 0.9900 . ? C60 H60B 0.9900 . ? C61 H61A 0.9800 . ? C61 H61B 0.9800 . ? C61 H61C 0.9800 . ? C62 C63 1.481(10) . ? C62 H62A 0.9900 . ? C62 H62B 0.9900 . ? C63 C64 1.512(11) . ? C63 H63A 0.9900 . ? C63 H63B 0.9900 . ? C64 H64A 0.9800 . ? C64 H64B 0.9800 . ? C64 H64C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P1 Au1 Cl2 178.07(9) . . ? P2 Au2 Cl1 174.33(7) . . ? C7 P1 C34 105.8(3) . . ? C7 P1 C1 105.3(3) . . ? C34 P1 C1 107.3(3) . . ? C7 P1 Au1 114.1(3) . . ? C34 P1 Au1 111.8(2) . . ? C1 P1 Au1 112.0(2) . . ? C25 P2 C19 105.9(3) . . ? C25 P2 C13 106.9(3) . . ? C19 P2 C13 108.9(3) . . ? C25 P2 Au2 115.0(2) . . ? C19 P2 Au2 113.2(2) . . ? C13 P2 Au2 106.6(2) . . ? C28 O1 C53 114.2(5) . . ? C37 O2 C56 113.5(5) . . ? C44 O3 C59 111.9(5) . . ? C51 O4 C62 114.3(5) . . ? C2 C1 C6 120.7(8) . . ? C2 C1 P1 123.6(6) . . ? C6 C1 P1 115.8(6) . . ? C1 C2 C3 121.2(8) . . ? C1 C2 H2 119.4 . . ? C3 C2 H2 119.4 . . ? C4 C3 C2 119.2(9) . . ? C4 C3 H3 120.4 . . ? C2 C3 H3 120.4 . . ? C3 C4 C5 119.1(8) . . ? C3 C4 H4 120.4 . . ? C5 C4 H4 120.4 . . ? C6 C5 C4 120.3(8) . . ? C6 C5 H5 119.8 . . ? C4 C5 H5 119.8 . . ? C1 C6 C5 119.5(8) . . ? C1 C6 H6 120.3 . . ? C5 C6 H6 120.3 . . ? C12 C7 C8 118.4(7) . . ? C12 C7 P1 121.2(7) . . ? C8 C7 P1 120.4(6) . . ? C9 C8 C7 120.1(8) . . ? C9 C8 H8 120.0 . . ? C7 C8 H8 120.0 . . ? C10 C9 C8 120.3(9) . . ? C10 C9 H9 119.9 . . ? C8 C9 H9 119.9 . . ? C9 C10 C11 120.6(8) . . ? C9 C10 H10 119.7 . . ? C11 C10 H10 119.7 . . ? C12 C11 C10 118.6(9) . . ? C12 C11 H11 120.7 . . ? C10 C11 H11 120.7 . . ? C11 C12 C7 122.1(9) . . ? C11 C12 H12 118.9 . . ? C7 C12 H12 118.9 . . ? C18 C13 C14 120.3(7) . . ? C18 C13 P2 122.8(6) . . ? C14 C13 P2 116.7(5) . . ? C13 C14 C15 119.5(7) . . ? C13 C14 H14 120.3 . . ? C15 C14 H14 120.3 . . ? C16 C15 C14 120.2(8) . . ? C16 C15 H15 119.9 . . ? C14 C15 H15 119.9 . . ? C15 C16 C17 120.1(7) . . ? C15 C16 H16 119.9 . . ? C17 C16 H16 119.9 . . ? C18 C17 C16 120.2(8) . . ? C18 C17 H17 119.9 . . ? C16 C17 H17 119.9 . . ? C13 C18 C17 119.6(8) . . ? C13 C18 H18 120.2 . . ? C17 C18 H18 120.2 . . ? C20 C19 C24 118.4(7) . . ? C20 C19 P2 122.5(5) . . ? C24 C19 P2 119.1(5) . . ? C19 C20 C21 120.1(7) . . ? C19 C20 H20 119.9 . . ? C21 C20 H20 119.9 . . ? C22 C21 C20 120.3(8) . . ? C22 C21 H21 119.8 . . ? C20 C21 H21 119.8 . . ? C23 C22 C21 119.6(7) . . ? C23 C22 H22 120.2 . . ? C21 C22 H22 120.2 . . ? C24 C23 C22 121.3(8) . . ? C24 C23 H23 119.4 . . ? C22 C23 H23 119.4 . . ? C23 C24 C19 120.2(8) . . ? C23 C24 H24 119.9 . . ? C19 C24 H24 119.9 . . ? C26 C25 C30 118.9(6) . . ? C26 C25 P2 123.1(5) . . ? C30 C25 P2 117.9(5) . . ? C25 C26 C27 120.6(6) . . ? C25 C26 H26 119.7 . . ? C27 C26 H26 119.7 . . ? C28 C27 C26 118.5(6) . . ? C28 C27 C52 122.2(6) . . ? C26 C27 C52 119.0(6) . . ? O1 C28 C27 119.4(6) . . ? O1 C28 C29 118.4(6) . . ? C27 C28 C29 122.0(6) . . ? C30 C29 C28 117.5(6) . . ? C30 C29 C31 120.0(6) . . ? C28 C29 C31 122.3(6) . . ? C29 C30 C25 122.4(6) . . ? C29 C30 H30 118.8 . . ? C25 C30 H30 118.8 . . ? C32 C31 C29 109.6(5) . . ? C32 C31 H31A 109.8 . . ? C29 C31 H31A 109.8 . . ? C32 C31 H31B 109.8 . . ? C29 C31 H31B 109.8 . . ? H31A C31 H31B 108.2 . . ? C33 C32 C37 118.4(6) . . ? C33 C32 C31 122.8(6) . . ? C37 C32 C31 118.4(6) . . ? C32 C33 C34 121.4(6) . . ? C32 C33 H33 119.3 . . ? C34 C33 H33 119.3 . . ? C33 C34 C35 118.7(6) . . ? C33 C34 P1 119.8(5) . . ? C35 C34 P1 121.3(5) . . ? C34 C35 C36 121.2(6) . . ? C34 C35 H35 119.4 . . ? C36 C35 H35 119.4 . . ? C37 C36 C35 118.4(6) . . ? C37 C36 C38 119.8(6) . . ? C35 C36 C38 121.3(6) . . ? C36 C37 O2 119.6(6) . . ? C36 C37 C32 121.6(6) . . ? O2 C37 C32 118.6(6) . . ? C39 C38 C36 111.1(5) . . ? C39 C38 H38A 109.4 . . ? C36 C38 H38A 109.4 . . ? C39 C38 H38B 109.4 . . ? C36 C38 H38B 109.4 . . ? H38A C38 H38B 108.0 . . ? C40 C39 C44 118.8(6) . . ? C40 C39 C38 120.6(6) . . ? C44 C39 C38 120.5(6) . . ? C39 C40 C41 120.9(6) . . ? C39 C40 H40 119.5 . . ? C41 C40 H40 119.5 . . ? C42 C41 C40 119.0(6) . . ? C42 C41 H41 120.5 . . ? C40 C41 H41 120.5 . . ? C43 C42 C41 121.9(7) . . ? C43 C42 H42 119.1 . . ? C41 C42 H42 119.1 . . ? C42 C43 C44 117.4(6) . . ? C42 C43 C45 120.1(7) . . ? C44 C43 C45 122.4(6) . . ? C39 C44 O3 119.9(6) . . ? C39 C44 C43 121.9(6) . . ? O3 C44 C43 118.2(6) . . ? C43 C45 C46 110.8(6) . . ? C43 C45 H45A 109.5 . . ? C46 C45 H45A 109.5 . . ? C43 C45 H45B 109.5 . . ? C46 C45 H45B 109.5 . . ? H45A C45 H45B 108.1 . . ? C51 C46 C47 116.9(7) . . ? C51 C46 C45 121.5(7) . . ? C47 C46 C45 121.3(7) . . ? C48 C47 C46 122.0(7) . . ? C48 C47 H47 119.0 . . ? C46 C47 H47 119.0 . . ? C49 C48 C47 119.9(7) . . ? C49 C48 H48 120.1 . . ? C47 C48 H48 120.1 . . ? C48 C49 C50 120.3(7) . . ? C48 C49 H49 119.9 . . ? C50 C49 H49 119.9 . . ? C51 C50 C49 118.5(7) . . ? C51 C50 C52 119.9(6) . . ? C49 C50 C52 121.2(7) . . ? C46 C51 C50 122.1(7) . . ? C46 C51 O4 119.7(6) . . ? C50 C51 O4 117.8(6) . . ? C27 C52 C50 108.8(5) . . ? C27 C52 H52A 109.9 . . ? C50 C52 H52A 109.9 . . ? C27 C52 H52B 109.9 . . ? C50 C52 H52B 109.9 . . ? H52A C52 H52B 108.3 . . ? C54 C53 O1 107.4(7) . . ? C54 C53 H53A 110.2 . . ? O1 C53 H53A 110.2 . . ? C54 C53 H53B 110.2 . . ? O1 C53 H53B 110.2 . . ? H53A C53 H53B 108.5 . . ? C55 C54 C53 134.3(14) . . ? C55 C54 H54 112.9 . . ? C53 C54 H54 112.9 . . ? C54 C55 H55A 120.0 . . ? C54 C55 H55B 120.0 . . ? H55A C55 H55B 120.0 . . ? O2 C56 C57 111.3(6) . . ? O2 C56 H56A 109.4 . . ? C57 C56 H56A 109.4 . . ? O2 C56 H56B 109.4 . . ? C57 C56 H56B 109.4 . . ? H56A C56 H56B 108.0 . . ? C58 C57 C56 123.3(9) . . ? C58 C57 H57 118.3 . . ? C56 C57 H57 118.3 . . ? C57 C58 H58A 120.0 . . ? C57 C58 H58B 120.0 . . ? H58A C58 H58B 120.0 . . ? O3 C59 C60 108.6(6) . . ? O3 C59 H59A 110.0 . . ? C60 C59 H59A 110.0 . . ? O3 C59 H59B 110.0 . . ? C60 C59 H59B 110.0 . . ? H59A C59 H59B 108.4 . . ? C61 C60 C59 112.5(8) . . ? C61 C60 H60A 109.1 . . ? C59 C60 H60A 109.1 . . ? C61 C60 H60B 109.1 . . ? C59 C60 H60B 109.1 . . ? H60A C60 H60B 107.8 . . ? C60 C61 H61A 109.5 . . ? C60 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? C60 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? O4 C62 C63 114.8(6) . . ? O4 C62 H62A 108.6 . . ? C63 C62 H62A 108.6 . . ? O4 C62 H62B 108.6 . . ? C63 C62 H62B 108.6 . . ? H62A C62 H62B 107.5 . . ? C62 C63 C64 111.7(7) . . ? C62 C63 H63A 109.3 . . ? C64 C63 H63A 109.3 . . ? C62 C63 H63B 109.3 . . ? C64 C63 H63B 109.3 . . ? H63A C63 H63B 107.9 . . ? C63 C64 H64A 109.5 . . ? C63 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? C63 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Cl2 Au1 P1 C7 130(3) . . . . ? Cl2 Au1 P1 C34 10(3) . . . . ? Cl2 Au1 P1 C1 -110(3) . . . . ? Cl1 Au2 P2 C25 -124.4(8) . . . . ? Cl1 Au2 P2 C19 113.6(8) . . . . ? Cl1 Au2 P2 C13 -6.1(9) . . . . ? C7 P1 C1 C2 -101.9(7) . . . . ? C34 P1 C1 C2 10.4(7) . . . . ? Au1 P1 C1 C2 133.5(6) . . . . ? C7 P1 C1 C6 78.5(6) . . . . ? C34 P1 C1 C6 -169.2(5) . . . . ? Au1 P1 C1 C6 -46.1(6) . . . . ? C6 C1 C2 C3 0.7(12) . . . . ? P1 C1 C2 C3 -178.9(6) . . . . ? C1 C2 C3 C4 -0.7(13) . . . . ? C2 C3 C4 C5 -1.0(13) . . . . ? C3 C4 C5 C6 2.7(13) . . . . ? C2 C1 C6 C5 1.1(11) . . . . ? P1 C1 C6 C5 -179.3(6) . . . . ? C4 C5 C6 C1 -2.8(12) . . . . ? C34 P1 C7 C12 105.2(7) . . . . ? C1 P1 C7 C12 -141.4(6) . . . . ? Au1 P1 C7 C12 -18.1(7) . . . . ? C34 P1 C7 C8 -71.3(7) . . . . ? C1 P1 C7 C8 42.1(7) . . . . ? Au1 P1 C7 C8 165.4(5) . . . . ? C12 C7 C8 C9 0.6(12) . . . . ? P1 C7 C8 C9 177.2(6) . . . . ? C7 C8 C9 C10 1.3(13) . . . . ? C8 C9 C10 C11 -2.7(14) . . . . ? C9 C10 C11 C12 2.1(14) . . . . ? C10 C11 C12 C7 -0.2(14) . . . . ? C8 C7 C12 C11 -1.2(13) . . . . ? P1 C7 C12 C11 -177.8(7) . . . . ? C25 P2 C13 C18 -124.6(6) . . . . ? C19 P2 C13 C18 -10.5(7) . . . . ? Au2 P2 C13 C18 111.9(6) . . . . ? C25 P2 C13 C14 59.9(6) . . . . ? C19 P2 C13 C14 173.9(6) . . . . ? Au2 P2 C13 C14 -63.6(6) . . . . ? C18 C13 C14 C15 -0.2(12) . . . . ? P2 C13 C14 C15 175.5(6) . . . . ? C13 C14 C15 C16 -0.8(13) . . . . ? C14 C15 C16 C17 0.4(13) . . . . ? C15 C16 C17 C18 1.0(14) . . . . ? C14 C13 C18 C17 1.6(12) . . . . ? P2 C13 C18 C17 -173.8(6) . . . . ? C16 C17 C18 C13 -2.0(13) . . . . ? C25 P2 C19 C20 13.7(7) . . . . ? C13 P2 C19 C20 -101.0(6) . . . . ? Au2 P2 C19 C20 140.6(6) . . . . ? C25 P2 C19 C24 -163.6(6) . . . . ? C13 P2 C19 C24 81.7(6) . . . . ? Au2 P2 C19 C24 -36.7(6) . . . . ? C24 C19 C20 C21 0.6(11) . . . . ? P2 C19 C20 C21 -176.7(6) . . . . ? C19 C20 C21 C22 0.6(12) . . . . ? C20 C21 C22 C23 -2.6(13) . . . . ? C21 C22 C23 C24 3.3(14) . . . . ? C22 C23 C24 C19 -2.0(13) . . . . ? C20 C19 C24 C23 0.0(11) . . . . ? P2 C19 C24 C23 177.5(6) . . . . ? C19 P2 C25 C26 -106.2(6) . . . . ? C13 P2 C25 C26 9.9(6) . . . . ? Au2 P2 C25 C26 128.0(5) . . . . ? C19 P2 C25 C30 76.8(6) . . . . ? C13 P2 C25 C30 -167.1(5) . . . . ? Au2 P2 C25 C30 -49.0(6) . . . . ? C30 C25 C26 C27 -3.4(10) . . . . ? P2 C25 C26 C27 179.6(5) . . . . ? C25 C26 C27 C28 1.4(9) . . . . ? C25 C26 C27 C52 175.0(6) . . . . ? C53 O1 C28 C27 91.2(7) . . . . ? C53 O1 C28 C29 -92.9(7) . . . . ? C26 C27 C28 O1 177.3(5) . . . . ? C52 C27 C28 O1 4.0(9) . . . . ? C26 C27 C28 C29 1.6(9) . . . . ? C52 C27 C28 C29 -171.7(6) . . . . ? O1 C28 C29 C30 -178.2(5) . . . . ? C27 C28 C29 C30 -2.4(9) . . . . ? O1 C28 C29 C31 -2.8(9) . . . . ? C27 C28 C29 C31 172.9(6) . . . . ? C28 C29 C30 C25 0.3(9) . . . . ? C31 C29 C30 C25 -175.2(6) . . . . ? C26 C25 C30 C29 2.6(10) . . . . ? P2 C25 C30 C29 179.7(5) . . . . ? C30 C29 C31 C32 48.2(8) . . . . ? C28 C29 C31 C32 -127.0(6) . . . . ? C29 C31 C32 C33 -105.1(7) . . . . ? C29 C31 C32 C37 67.5(7) . . . . ? C37 C32 C33 C34 -3.1(10) . . . . ? C31 C32 C33 C34 169.4(6) . . . . ? C32 C33 C34 C35 -0.3(10) . . . . ? C32 C33 C34 P1 175.2(5) . . . . ? C7 P1 C34 C33 170.2(6) . . . . ? C1 P1 C34 C33 58.2(6) . . . . ? Au1 P1 C34 C33 -65.0(6) . . . . ? C7 P1 C34 C35 -14.4(7) . . . . ? C1 P1 C34 C35 -126.4(6) . . . . ? Au1 P1 C34 C35 110.4(5) . . . . ? C33 C34 C35 C36 2.2(10) . . . . ? P1 C34 C35 C36 -173.2(5) . . . . ? C34 C35 C36 C37 -0.6(10) . . . . ? C34 C35 C36 C38 -172.7(6) . . . . ? C35 C36 C37 O2 -178.4(6) . . . . ? C38 C36 C37 O2 -6.1(9) . . . . ? C35 C36 C37 C32 -3.0(10) . . . . ? C38 C36 C37 C32 169.3(6) . . . . ? C56 O2 C37 C36 -79.5(7) . . . . ? C56 O2 C37 C32 105.0(7) . . . . ? C33 C32 C37 C36 4.8(10) . . . . ? C31 C32 C37 C36 -168.0(6) . . . . ? C33 C32 C37 O2 -179.7(6) . . . . ? C31 C32 C37 O2 7.4(9) . . . . ? C37 C36 C38 C39 -67.8(8) . . . . ? C35 C36 C38 C39 104.2(7) . . . . ? C36 C38 C39 C40 -60.3(8) . . . . ? C36 C38 C39 C44 117.2(6) . . . . ? C44 C39 C40 C41 0.9(9) . . . . ? C38 C39 C40 C41 178.4(6) . . . . ? C39 C40 C41 C42 -2.7(10) . . . . ? C40 C41 C42 C43 1.7(10) . . . . ? C41 C42 C43 C44 1.1(10) . . . . ? C41 C42 C43 C45 -175.0(6) . . . . ? C40 C39 C44 O3 -176.5(5) . . . . ? C38 C39 C44 O3 6.0(9) . . . . ? C40 C39 C44 C43 2.0(9) . . . . ? C38 C39 C44 C43 -175.5(6) . . . . ? C59 O3 C44 C39 88.9(7) . . . . ? C59 O3 C44 C43 -89.6(7) . . . . ? C42 C43 C44 C39 -3.0(9) . . . . ? C45 C43 C44 C39 173.0(6) . . . . ? C42 C43 C44 O3 175.5(5) . . . . ? C45 C43 C44 O3 -8.5(9) . . . . ? C42 C43 C45 C46 58.5(8) . . . . ? C44 C43 C45 C46 -117.4(7) . . . . ? C43 C45 C46 C51 70.9(9) . . . . ? C43 C45 C46 C47 -103.0(8) . . . . ? C51 C46 C47 C48 0.2(11) . . . . ? C45 C46 C47 C48 174.4(7) . . . . ? C46 C47 C48 C49 -4.3(13) . . . . ? C47 C48 C49 C50 3.5(12) . . . . ? C48 C49 C50 C51 1.2(11) . . . . ? C48 C49 C50 C52 -171.4(7) . . . . ? C47 C46 C51 C50 4.6(10) . . . . ? C45 C46 C51 C50 -169.5(6) . . . . ? C47 C46 C51 O4 178.1(6) . . . . ? C45 C46 C51 O4 4.0(10) . . . . ? C49 C50 C51 C46 -5.4(10) . . . . ? C52 C50 C51 C46 167.3(6) . . . . ? C49 C50 C51 O4 -179.0(6) . . . . ? C52 C50 C51 O4 -6.2(9) . . . . ? C62 O4 C51 C46 79.9(7) . . . . ? C62 O4 C51 C50 -106.3(7) . . . . ? C28 C27 C52 C50 121.2(7) . . . . ? C26 C27 C52 C50 -52.1(8) . . . . ? C51 C50 C52 C27 -65.3(8) . . . . ? C49 C50 C52 C27 107.2(7) . . . . ? C28 O1 C53 C54 167.0(8) . . . . ? O1 C53 C54 C55 125.4(13) . . . . ? C37 O2 C56 C57 -99.4(7) . . . . ? O2 C56 C57 C58 125.5(9) . . . . ? C44 O3 C59 C60 -170.3(6) . . . . ? O3 C59 C60 C61 -64.9(9) . . . . ? C51 O4 C62 C63 87.1(8) . . . . ? O4 C62 C63 C64 -179.5(7) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.57 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.006 _refine_diff_density_min -1.030 _refine_diff_density_rms 0.138 # Attachment 'squeezeforCCDC809315.sqz' # Accepted Reflns Hmax Kmax Lmax