# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Robin Bedford' 'Helena Dumycz' 'Mairi F. Haddow' 'A Orpen' 'Lukasz T Pilarski' 'Paul Pringle' 'Richard L Wingad' _publ_contact_author_name 'Robin Bedford' _publ_contact_author_email R.BEDFORD@BRISTOL.AC.UK _publ_section_title ; Chiral triaryl phosphite-based palladacycles and platinacycles: synthesis and application to asymmetric Lewis acid catalysis ; # Attachment '10a.cif' data_ltp1b68sad _database_code_depnum_ccdc_archive 'CCDC 727729' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C55 H58 Cl N2 O3 P Pd, 1.5(C H2 Cl2)' _chemical_formula_sum 'C56.50 H61 Cl4 N2 O3 P Pd' _chemical_formula_weight 1095.24 _chemical_absolute_configuration ad 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M P212121 _symmetry_space_group_name_Hall 'P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 14.495(3) _cell_length_b 16.679(3) _cell_length_c 21.684(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5242.4(18) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 25839 _cell_measurement_theta_min 2.241 _cell_measurement_theta_max 27.481 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.388 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2268 _exptl_absorpt_coefficient_mu 0.634 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.789671 _exptl_absorpt_correction_T_max 0.900000 _exptl_absorpt_process_details 'SADABS V2.10 (Bruker AXS 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 60588 _diffrn_reflns_av_R_equivalents 0.0309 _diffrn_reflns_av_sigmaI/netI 0.0233 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.08 _diffrn_reflns_theta_max 27.48 _reflns_number_total 12029 _reflns_number_gt 11636 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART V5.628 (Bruker, 2005)' _computing_cell_refinement 'Bruker SMART V5.628 (Bruker, 2005)' _computing_data_reduction 'Bruker SAINT V6.41A (Bruker, 2002)' _computing_structure_solution 'SHELXS V6.12 (Bruker 2001)' _computing_structure_refinement 'SHELXL V6.12 (Bruker 2001)' _computing_molecular_graphics 'Bruker SHELXTL V6.14 (Bruker AXS, 2003)' _computing_publication_material 'Bruker SHELXTL V6.14 (Bruker AXS, 2003)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0534P)^2^+3.5790P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881, based on 5426 Friedel pairs' _refine_ls_abs_structure_Flack -0.027(15) _refine_ls_number_reflns 12029 _refine_ls_number_parameters 662 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0344 _refine_ls_R_factor_gt 0.0329 _refine_ls_wR_factor_ref 0.0891 _refine_ls_wR_factor_gt 0.0879 _refine_ls_goodness_of_fit_ref 1.074 _refine_ls_restrained_S_all 1.080 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.516892(13) 0.958690(10) 0.131891(8) 0.01607(5) Uani 1 1 d . . . P1 P 0.57920(4) 1.02608(4) 0.05604(3) 0.01665(13) Uani 1 1 d . . . Cl1 Cl 0.54448(6) 1.06947(4) 0.19874(3) 0.02917(15) Uani 1 1 d . . . O1 O 0.55166(12) 1.11719(11) 0.04226(8) 0.0177(3) Uani 1 1 d . . . O2 O 0.69033(13) 1.02858(11) 0.05173(9) 0.0199(4) Uani 1 1 d . . . O3 O 0.55859(14) 0.98083(10) -0.00685(8) 0.0203(4) Uani 1 1 d . . . N1 N 0.53187(15) 0.83165(13) 0.22865(11) 0.0203(5) Uani 1 1 d . . . N2 N 0.38659(16) 0.86130(14) 0.21802(10) 0.0198(4) Uani 1 1 d . . . C1 C 0.59790(18) 1.15936(14) -0.00452(12) 0.0169(5) Uani 1 1 d . . . C2 C 0.54645(18) 1.17583(15) -0.05802(13) 0.0206(5) Uani 1 1 d . . . H2 H 0.4840 1.1590 -0.0614 0.025 Uiso 1 1 calc R . . C3 C 0.5882(2) 1.21642(16) -0.10485(13) 0.0225(5) Uani 1 1 d . . . H3 H 0.5539 1.2288 -0.1410 0.027 Uiso 1 1 calc R . . C4 C 0.6813(2) 1.24040(16) -0.10073(12) 0.0205(5) Uani 1 1 d . . . C5 C 0.7254(2) 1.28163(18) -0.15038(13) 0.0264(6) Uani 1 1 d . . . H5 H 0.6915 1.2935 -0.1867 0.032 Uiso 1 1 calc R . . C6 C 0.8152(2) 1.30401(18) -0.14628(13) 0.0282(6) Uani 1 1 d . . . H6 H 0.8433 1.3321 -0.1794 0.034 Uiso 1 1 calc R . . C7 C 0.8666(2) 1.28592(19) -0.09331(14) 0.0298(7) Uani 1 1 d . . . H7 H 0.9296 1.3014 -0.0911 0.036 Uiso 1 1 calc R . . C8 C 0.8270(2) 1.24614(18) -0.04471(13) 0.0240(6) Uani 1 1 d . . . H8 H 0.8634 1.2334 -0.0096 0.029 Uiso 1 1 calc R . . C9 C 0.73250(19) 1.22358(16) -0.04591(12) 0.0196(5) Uani 1 1 d . . . C10 C 0.68733(17) 1.18382(15) 0.00442(11) 0.0160(5) Uani 1 1 d . . . C11 C 0.73421(17) 1.16590(15) 0.06386(12) 0.0162(5) Uani 1 1 d . . . C12 C 0.77507(17) 1.22717(16) 0.10201(12) 0.0173(5) Uani 1 1 d . . . C13 C 0.76934(18) 1.30985(16) 0.08719(12) 0.0194(5) Uani 1 1 d . . . H13 H 0.7393 1.3259 0.0503 0.023 Uiso 1 1 calc R . . C14 C 0.80644(18) 1.36711(17) 0.12531(13) 0.0222(5) Uani 1 1 d . . . H14 H 0.8017 1.4222 0.1147 0.027 Uiso 1 1 calc R . . C15 C 0.85181(18) 1.34421(18) 0.18056(13) 0.0237(6) Uani 1 1 d . . . H15 H 0.8785 1.3839 0.2065 0.028 Uiso 1 1 calc R . . C16 C 0.85706(18) 1.26526(18) 0.19642(12) 0.0232(6) Uani 1 1 d . . . H16 H 0.8874 1.2505 0.2336 0.028 Uiso 1 1 calc R . . C17 C 0.81818(18) 1.20457(17) 0.15854(12) 0.0204(5) Uani 1 1 d . . . C18 C 0.8188(2) 1.12275(19) 0.17635(13) 0.0262(6) Uani 1 1 d . . . H18 H 0.8491 1.1075 0.2134 0.031 Uiso 1 1 calc R . . C19 C 0.77676(19) 1.06586(17) 0.14149(13) 0.0243(6) Uani 1 1 d . . . H19 H 0.7760 1.0114 0.1544 0.029 Uiso 1 1 calc R . . C20 C 0.73471(18) 1.08863(16) 0.08642(12) 0.0193(5) Uani 1 1 d . . . C36 C 0.4868(2) 0.77788(18) 0.27377(14) 0.0288(6) Uani 1 1 d . . . H36A H 0.5067 0.7903 0.3164 0.035 Uiso 1 1 calc R . . H36B H 0.5004 0.7209 0.2647 0.035 Uiso 1 1 calc R . . C37 C 0.3848(2) 0.79648(17) 0.26457(14) 0.0250(6) Uani 1 1 d . . . H37A H 0.3510 0.7490 0.2491 0.030 Uiso 1 1 calc R . . H37B H 0.3560 0.8149 0.3035 0.030 Uiso 1 1 calc R . . C38 C 0.63084(18) 0.84100(16) 0.22821(12) 0.0187(5) Uani 1 1 d . . . C39 C 0.68511(19) 0.79468(16) 0.18842(12) 0.0209(5) Uani 1 1 d . . . C40 C 0.77935(19) 0.80587(17) 0.18885(13) 0.0229(6) Uani 1 1 d . . . H40 H 0.8163 0.7755 0.1613 0.027 Uiso 1 1 calc R . . C41 C 0.8221(2) 0.86011(18) 0.22827(14) 0.0257(6) Uani 1 1 d . . . C42 C 0.7673(2) 0.90271(17) 0.26912(14) 0.0260(6) Uani 1 1 d . . . H42 H 0.7956 0.9389 0.2972 0.031 Uiso 1 1 calc R . . C43 C 0.6716(2) 0.89404(17) 0.27023(13) 0.0239(5) Uani 1 1 d . . . C44 C 0.6432(2) 0.73269(18) 0.14593(14) 0.0275(6) Uani 1 1 d . . . H44A H 0.6197 0.7591 0.1088 0.041 Uiso 1 1 calc R . . H44B H 0.5924 0.7054 0.1671 0.041 Uiso 1 1 calc R . . H44C H 0.6903 0.6934 0.1344 0.041 Uiso 1 1 calc R . . C45 C 0.9252(2) 0.8716(2) 0.22763(17) 0.0363(7) Uani 1 1 d . . . H45A H 0.9419 0.9154 0.2556 0.054 Uiso 1 1 calc R . . H45B H 0.9454 0.8848 0.1857 0.054 Uiso 1 1 calc R . . H45C H 0.9555 0.8221 0.2411 0.054 Uiso 1 1 calc R . . C46 C 0.6170(2) 0.93966(19) 0.31746(15) 0.0339(7) Uani 1 1 d . . . H46A H 0.5511 0.9350 0.3082 0.051 Uiso 1 1 calc R . . H46B H 0.6351 0.9963 0.3165 0.051 Uiso 1 1 calc R . . H46C H 0.6292 0.9175 0.3585 0.051 Uiso 1 1 calc R . . C47 C 0.30553(19) 0.91032(16) 0.20848(13) 0.0217(5) Uani 1 1 d . . . C48 C 0.23715(19) 0.88485(18) 0.16780(13) 0.0236(6) Uani 1 1 d . . . C49 C 0.1595(2) 0.9332(2) 0.15975(14) 0.0295(6) Uani 1 1 d . . . H49 H 0.1129 0.9168 0.1316 0.035 Uiso 1 1 calc R . . C50 C 0.1484(2) 1.0043(2) 0.19162(15) 0.0321(7) Uani 1 1 d . . . C51 C 0.2155(2) 1.02583(18) 0.23387(15) 0.0333(7) Uani 1 1 d . . . H51 H 0.2074 1.0737 0.2570 0.040 Uiso 1 1 calc R . . C52 C 0.2947(2) 0.98001(17) 0.24383(13) 0.0256(6) Uani 1 1 d . . . C53 C 0.2437(2) 0.80692(19) 0.13328(17) 0.0327(6) Uani 1 1 d . . . H53A H 0.2939 0.8100 0.1031 0.049 Uiso 1 1 calc R . . H53B H 0.1853 0.7966 0.1119 0.049 Uiso 1 1 calc R . . H53C H 0.2560 0.7633 0.1624 0.049 Uiso 1 1 calc R . . C54 C 0.0650(3) 1.0566(2) 0.18028(19) 0.0454(9) Uani 1 1 d . . . H54A H 0.0505 1.0868 0.2178 0.068 Uiso 1 1 calc R . . H54B H 0.0122 1.0228 0.1691 0.068 Uiso 1 1 calc R . . H54C H 0.0781 1.0940 0.1466 0.068 Uiso 1 1 calc R . . C55 C 0.3618(2) 1.00306(19) 0.29280(15) 0.0323(7) Uani 1 1 d . . . H55A H 0.3372 1.0483 0.3165 0.048 Uiso 1 1 calc R . . H55B H 0.4204 1.0186 0.2737 0.048 Uiso 1 1 calc R . . H55C H 0.3720 0.9574 0.3204 0.048 Uiso 1 1 calc R . . C26 C 0.49732(17) 0.87859(14) 0.06144(11) 0.0169(5) Uani 1 1 d . . . C25 C 0.46229(17) 0.80055(15) 0.06624(12) 0.0177(5) Uani 1 1 d . . . H25 H 0.4479 0.7803 0.1060 0.021 Uiso 1 1 calc R . . C24 C 0.44772(18) 0.75142(15) 0.01524(12) 0.0178(5) Uani 1 1 d . . . C23 C 0.46936(17) 0.78209(15) -0.04283(12) 0.0185(5) Uani 1 1 d . . . H23 H 0.4583 0.7494 -0.0779 0.022 Uiso 1 1 calc R . . C22 C 0.50652(17) 0.85848(14) -0.05194(11) 0.0161(5) Uani 1 1 d . . . C21 C 0.51966(19) 0.90357(14) 0.00157(11) 0.0162(4) Uani 1 1 d . . . C31 C 0.4071(2) 0.66625(16) 0.01967(13) 0.0241(6) Uani 1 1 d . . . C34 C 0.4068(2) 0.63460(17) 0.08598(14) 0.0301(6) Uani 1 1 d . . . H34A H 0.3811 0.5803 0.0866 0.045 Uiso 1 1 calc R . . H34B H 0.3690 0.6698 0.1119 0.045 Uiso 1 1 calc R . . H34C H 0.4701 0.6335 0.1019 0.045 Uiso 1 1 calc R . . C32 C 0.3080(2) 0.6672(2) -0.00528(15) 0.0363(8) Uani 1 1 d . . . H32A H 0.3077 0.6899 -0.0470 0.054 Uiso 1 1 calc R . . H32B H 0.2691 0.7000 0.0218 0.054 Uiso 1 1 calc R . . H32C H 0.2840 0.6123 -0.0066 0.054 Uiso 1 1 calc R . . C33 C 0.4646(3) 0.60787(18) -0.01948(17) 0.0446(10) Uani 1 1 d . . . H33A H 0.5287 0.6086 -0.0053 0.067 Uiso 1 1 calc R . . H33B H 0.4620 0.6242 -0.0629 0.067 Uiso 1 1 calc R . . H33C H 0.4395 0.5536 -0.0152 0.067 Uiso 1 1 calc R . . C27 C 0.53007(18) 0.89057(15) -0.11651(11) 0.0189(5) Uani 1 1 d . . . C30 C 0.5105(2) 0.82782(16) -0.16618(12) 0.0240(5) Uani 1 1 d . . . H30A H 0.5473 0.7797 -0.1581 0.036 Uiso 1 1 calc R . . H30B H 0.5267 0.8496 -0.2067 0.036 Uiso 1 1 calc R . . H30C H 0.4448 0.8139 -0.1656 0.036 Uiso 1 1 calc R . . C28 C 0.6339(2) 0.91158(17) -0.12109(13) 0.0245(6) Uani 1 1 d . . . H28A H 0.6708 0.8645 -0.1100 0.037 Uiso 1 1 calc R . . H28B H 0.6481 0.9556 -0.0927 0.037 Uiso 1 1 calc R . . H28C H 0.6485 0.9279 -0.1634 0.037 Uiso 1 1 calc R . . C29 C 0.47130(19) 0.96461(16) -0.13107(13) 0.0264(5) Uani 1 1 d . . . H29A H 0.4881 0.9855 -0.1718 0.040 Uiso 1 1 calc R . . H29B H 0.4823 1.0059 -0.0998 0.040 Uiso 1 1 calc R . . H29C H 0.4059 0.9497 -0.1310 0.040 Uiso 1 1 calc R . . C35 C 0.47255(18) 0.87949(15) 0.19926(11) 0.0174(5) Uani 1 1 d . . . C56 C 0.4384(5) 0.8894(5) 0.5032(3) 0.050(2) Uani 0.50 1 d PD A 1 H56A H 0.3972 0.8466 0.5186 0.060 Uiso 0.50 1 calc PR A 1 H56B H 0.4064 0.9413 0.5094 0.060 Uiso 0.50 1 calc PR A 1 Cl2 Cl 0.53974(13) 0.88916(11) 0.54712(9) 0.0452(4) Uani 0.50 1 d PD A 1 Cl3 Cl 0.45466(18) 0.8759(4) 0.42826(11) 0.133(2) Uani 0.50 1 d PD A 1 C57 C 0.2241(9) 0.9994(6) 0.5226(5) 0.068(3) Uani 0.50 1 d P B 2 H57A H 0.1756 0.9645 0.5050 0.082 Uiso 0.50 1 calc PR B 2 H57B H 0.2045 1.0154 0.5645 0.082 Uiso 0.50 1 calc PR B 2 Cl4 Cl 0.3327(3) 0.94359(16) 0.52720(13) 0.0887(10) Uani 0.50 1 d P B 2 Cl5 Cl 0.2361(2) 1.0821(2) 0.47814(16) 0.0793(8) Uani 0.50 1 d P B 2 C58 C 0.2148(6) 1.0541(6) 0.5158(4) 0.050(2) Uani 0.50 1 d P C 3 H58A H 0.2488 1.0790 0.5505 0.060 Uiso 0.50 1 calc PR C 3 H58B H 0.1584 1.0861 0.5085 0.060 Uiso 0.50 1 calc PR C 3 Cl6 Cl 0.28551(16) 1.05732(14) 0.44806(11) 0.0604(6) Uani 0.50 1 d P C 3 Cl7 Cl 0.18468(15) 0.96110(14) 0.53550(9) 0.0490(4) Uani 0.50 1 d P C 3 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 0.02132(9) 0.01058(8) 0.01632(8) -0.00130(7) 0.00518(7) -0.00302(7) P1 0.0206(3) 0.0105(3) 0.0188(3) -0.0010(2) 0.0050(2) -0.0030(2) Cl1 0.0464(4) 0.0160(3) 0.0252(3) -0.0072(2) 0.0096(3) -0.0080(3) O1 0.0173(8) 0.0130(8) 0.0229(9) 0.0012(7) 0.0049(7) -0.0025(7) O2 0.0215(9) 0.0117(9) 0.0266(9) -0.0011(7) 0.0045(7) -0.0005(7) O3 0.0301(10) 0.0122(8) 0.0186(9) -0.0019(7) 0.0057(7) -0.0073(7) N1 0.0221(12) 0.0153(10) 0.0236(11) 0.0029(8) 0.0067(9) -0.0005(8) N2 0.0233(11) 0.0165(11) 0.0195(11) 0.0039(9) 0.0063(9) -0.0018(9) C1 0.0207(12) 0.0092(11) 0.0209(12) 0.0002(9) 0.0041(10) -0.0024(9) C2 0.0186(11) 0.0151(11) 0.0280(13) -0.0022(10) -0.0026(10) -0.0024(9) C3 0.0287(14) 0.0175(12) 0.0213(12) -0.0023(10) -0.0068(11) -0.0007(10) C4 0.0302(14) 0.0144(12) 0.0170(12) -0.0010(10) 0.0012(10) -0.0022(10) C5 0.0428(18) 0.0196(14) 0.0168(12) 0.0023(10) 0.0011(11) -0.0033(12) C6 0.0406(17) 0.0236(14) 0.0204(14) -0.0005(10) 0.0116(12) -0.0110(12) C7 0.0315(15) 0.0316(16) 0.0262(14) -0.0072(12) 0.0104(12) -0.0171(13) C8 0.0239(13) 0.0304(15) 0.0178(12) -0.0034(11) 0.0021(10) -0.0098(11) C9 0.0229(13) 0.0162(12) 0.0197(12) -0.0018(10) 0.0025(10) -0.0047(10) C10 0.0187(12) 0.0121(11) 0.0173(11) -0.0016(9) 0.0007(9) -0.0019(9) C11 0.0157(11) 0.0160(11) 0.0168(11) -0.0003(9) 0.0025(9) -0.0012(9) C12 0.0158(11) 0.0204(13) 0.0157(11) -0.0012(10) 0.0025(9) -0.0028(9) C13 0.0202(12) 0.0198(12) 0.0183(12) -0.0004(10) 0.0021(9) -0.0062(10) C14 0.0210(12) 0.0226(13) 0.0230(13) -0.0052(11) 0.0054(11) -0.0070(10) C15 0.0169(12) 0.0308(15) 0.0233(13) -0.0102(11) 0.0021(10) -0.0037(11) C16 0.0172(12) 0.0352(16) 0.0170(12) -0.0048(11) -0.0014(10) 0.0007(11) C17 0.0156(11) 0.0255(14) 0.0201(12) -0.0020(11) 0.0011(10) 0.0017(10) C18 0.0222(13) 0.0345(16) 0.0219(13) 0.0028(12) -0.0026(11) 0.0071(12) C19 0.0255(13) 0.0201(12) 0.0274(14) 0.0064(11) 0.0017(11) 0.0054(10) C20 0.0185(12) 0.0181(12) 0.0214(12) -0.0016(10) 0.0038(10) -0.0002(10) C36 0.0266(13) 0.0268(14) 0.0330(14) 0.0140(12) 0.0045(13) -0.0021(12) C37 0.0247(13) 0.0240(14) 0.0265(14) 0.0106(11) 0.0090(11) 0.0014(11) C38 0.0206(12) 0.0156(12) 0.0199(12) 0.0025(10) 0.0014(10) -0.0019(10) C39 0.0229(13) 0.0191(12) 0.0206(12) 0.0016(10) -0.0015(10) 0.0013(10) C40 0.0231(13) 0.0247(14) 0.0209(13) 0.0010(11) 0.0033(10) 0.0042(11) C41 0.0244(14) 0.0250(14) 0.0275(14) 0.0064(12) -0.0028(11) -0.0008(11) C42 0.0340(15) 0.0176(12) 0.0263(14) -0.0023(11) -0.0045(12) -0.0037(11) C43 0.0304(14) 0.0168(12) 0.0245(13) -0.0011(10) -0.0009(11) 0.0005(11) C44 0.0257(14) 0.0255(14) 0.0315(16) -0.0103(12) -0.0039(11) 0.0046(11) C45 0.0250(15) 0.0385(18) 0.0453(19) 0.0004(15) -0.0043(13) -0.0072(13) C46 0.0417(17) 0.0298(16) 0.0303(15) -0.0110(13) 0.0009(13) 0.0016(13) C47 0.0249(13) 0.0195(13) 0.0207(12) 0.0046(10) 0.0092(10) 0.0004(10) C48 0.0213(13) 0.0261(14) 0.0236(13) 0.0044(11) 0.0070(10) -0.0013(11) C49 0.0229(14) 0.0375(17) 0.0280(14) 0.0095(13) 0.0076(11) 0.0005(12) C50 0.0331(16) 0.0298(16) 0.0333(16) 0.0133(13) 0.0158(13) 0.0109(13) C51 0.0463(18) 0.0198(15) 0.0338(16) 0.0083(12) 0.0196(14) 0.0059(13) C52 0.0330(14) 0.0182(13) 0.0257(14) 0.0033(11) 0.0148(11) -0.0033(11) C53 0.0254(14) 0.0334(16) 0.0394(16) -0.0095(15) 0.0015(14) -0.0041(12) C54 0.0425(19) 0.042(2) 0.052(2) 0.0165(17) 0.0140(16) 0.0208(16) C55 0.0401(17) 0.0274(15) 0.0294(15) -0.0079(12) 0.0110(13) -0.0034(13) C26 0.0203(14) 0.0132(10) 0.0174(11) -0.0021(9) 0.0011(9) -0.0010(9) C25 0.0193(13) 0.0150(11) 0.0188(11) 0.0005(9) 0.0035(9) -0.0023(9) C24 0.0195(11) 0.0132(11) 0.0206(12) 0.0015(9) 0.0007(10) -0.0028(9) C23 0.0206(13) 0.0147(11) 0.0200(12) -0.0025(9) 0.0001(9) -0.0017(9) C22 0.0159(12) 0.0136(10) 0.0186(11) 0.0014(9) 0.0012(9) -0.0003(9) C21 0.0167(10) 0.0100(10) 0.0218(11) 0.0006(8) 0.0042(10) -0.0023(10) C31 0.0346(15) 0.0136(12) 0.0242(13) -0.0014(10) 0.0066(11) -0.0084(11) C34 0.0483(18) 0.0150(13) 0.0270(14) 0.0040(11) -0.0019(13) -0.0107(12) C32 0.0427(19) 0.0393(18) 0.0269(15) 0.0025(13) -0.0021(13) -0.0229(15) C33 0.075(3) 0.0153(13) 0.0430(18) -0.0037(13) 0.0218(18) -0.0061(15) C27 0.0243(13) 0.0159(11) 0.0164(11) 0.0007(9) 0.0030(9) -0.0005(10) C30 0.0313(14) 0.0229(12) 0.0179(12) -0.0002(10) 0.0028(11) -0.0017(11) C28 0.0263(13) 0.0239(14) 0.0232(14) -0.0008(10) 0.0088(10) -0.0039(10) C29 0.0328(14) 0.0215(12) 0.0249(12) 0.0047(11) -0.0024(11) 0.0045(11) C35 0.0226(12) 0.0130(10) 0.0165(11) -0.0052(8) 0.0056(10) -0.0012(10) C56 0.045(4) 0.040(4) 0.065(5) 0.008(4) -0.036(4) -0.003(3) Cl2 0.0455(10) 0.0369(9) 0.0532(10) -0.0018(8) -0.0112(8) 0.0031(7) Cl3 0.0454(13) 0.317(7) 0.0364(11) 0.007(2) 0.0000(10) 0.022(2) C57 0.110(9) 0.030(5) 0.064(6) 0.000(4) 0.007(6) -0.039(6) Cl4 0.149(3) 0.0510(14) 0.0661(15) -0.0032(12) -0.0385(17) -0.0207(16) Cl5 0.0621(15) 0.099(2) 0.0771(18) -0.0155(18) -0.0062(14) 0.0211(15) C58 0.061(5) 0.061(6) 0.027(4) 0.010(4) 0.009(3) -0.021(4) Cl6 0.0584(12) 0.0557(13) 0.0671(13) 0.0128(11) 0.0242(11) 0.0016(10) Cl7 0.0572(11) 0.0375(10) 0.0523(10) 0.0037(9) 0.0178(8) 0.0053(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 C26 2.049(2) . ? Pd1 C35 2.072(3) . ? Pd1 P1 2.1873(7) . ? Pd1 Cl1 2.3822(7) . ? P1 O3 1.5870(19) . ? P1 O1 1.5993(19) . ? P1 O2 1.6140(19) . ? O1 C1 1.405(3) . ? O2 C20 1.408(3) . ? O3 C21 1.419(3) . ? N1 C35 1.335(4) . ? N1 C38 1.443(3) . ? N1 C36 1.479(3) . ? N2 C35 1.346(3) . ? N2 C47 1.446(4) . ? N2 C37 1.479(3) . ? C1 C10 1.373(4) . ? C1 C2 1.406(4) . ? C2 C3 1.362(4) . ? C2 H2 0.9500 . ? C3 C4 1.411(4) . ? C3 H3 0.9500 . ? C4 C5 1.428(4) . ? C4 C9 1.429(4) . ? C5 C6 1.357(5) . ? C5 H5 0.9500 . ? C6 C7 1.402(5) . ? C6 H6 0.9500 . ? C7 C8 1.371(4) . ? C7 H7 0.9500 . ? C8 C9 1.421(4) . ? C8 H8 0.9500 . ? C9 C10 1.435(4) . ? C10 C11 1.487(4) . ? C11 C20 1.379(4) . ? C11 C12 1.442(4) . ? C12 C13 1.418(4) . ? C12 C17 1.427(4) . ? C13 C14 1.373(4) . ? C13 H13 0.9500 . ? C14 C15 1.419(4) . ? C14 H14 0.9500 . ? C15 C16 1.363(4) . ? C15 H15 0.9500 . ? C16 C17 1.420(4) . ? C16 H16 0.9500 . ? C17 C18 1.418(4) . ? C18 C19 1.357(4) . ? C18 H18 0.9500 . ? C19 C20 1.393(4) . ? C19 H19 0.9500 . ? C36 C37 1.523(4) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 C39 1.400(4) . ? C38 C43 1.401(4) . ? C39 C40 1.379(4) . ? C39 C44 1.512(4) . ? C40 C41 1.391(4) . ? C40 H40 0.9500 . ? C41 C42 1.387(4) . ? C41 C45 1.507(4) . ? C42 C43 1.394(4) . ? C42 H42 0.9500 . ? C43 C46 1.501(4) . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 C48 1.393(4) . ? C47 C52 1.401(4) . ? C48 C49 1.396(4) . ? C48 C53 1.503(4) . ? C49 C50 1.382(5) . ? C49 H49 0.9500 . ? C50 C51 1.384(5) . ? C50 C54 1.511(4) . ? C51 C52 1.395(5) . ? C51 H51 0.9500 . ? C52 C55 1.491(5) . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? C26 C25 1.401(3) . ? C26 C21 1.401(3) . ? C25 C24 1.392(4) . ? C25 H25 0.9500 . ? C24 C23 1.395(4) . ? C24 C31 1.541(3) . ? C23 C22 1.397(3) . ? C23 H23 0.9500 . ? C22 C21 1.396(3) . ? C22 C27 1.537(3) . ? C31 C34 1.532(4) . ? C31 C32 1.535(5) . ? C31 C33 1.537(4) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C27 C30 1.528(4) . ? C27 C29 1.533(4) . ? C27 C28 1.549(4) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C56 Cl3 1.657(7) . ? C56 Cl2 1.752(6) . ? C56 H56A 0.9900 . ? C56 H56B 0.9900 . ? C57 Cl5 1.691(11) . ? C57 Cl4 1.832(13) . ? C57 H57A 0.9900 . ? C57 H57B 0.9900 . ? C58 Cl7 1.667(10) . ? C58 Cl6 1.792(8) . ? C58 H58A 0.9900 . ? C58 H58B 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 C26 Pd1 C35 93.84(10) . . ? C26 Pd1 P1 80.31(7) . . ? C35 Pd1 P1 170.39(7) . . ? C26 Pd1 Cl1 169.28(7) . . ? C35 Pd1 Cl1 96.75(7) . . ? P1 Pd1 Cl1 89.41(3) . . ? O3 P1 O1 104.13(10) . . ? O3 P1 O2 98.65(10) . . ? O1 P1 O2 102.34(10) . . ? O3 P1 Pd1 108.91(7) . . ? O1 P1 Pd1 121.71(7) . . ? O2 P1 Pd1 117.97(8) . . ? C1 O1 P1 119.44(16) . . ? C20 O2 P1 116.32(16) . . ? C21 O3 P1 113.34(15) . . ? C35 N1 C38 124.9(2) . . ? C35 N1 C36 113.2(2) . . ? C38 N1 C36 120.6(2) . . ? C35 N2 C47 125.6(2) . . ? C35 N2 C37 112.8(2) . . ? C47 N2 C37 119.8(2) . . ? C10 C1 O1 119.8(2) . . ? C10 C1 C2 124.0(2) . . ? O1 C1 C2 116.1(2) . . ? C3 C2 C1 118.5(2) . . ? C3 C2 H2 120.8 . . ? C1 C2 H2 120.8 . . ? C2 C3 C4 121.2(3) . . ? C2 C3 H3 119.4 . . ? C4 C3 H3 119.4 . . ? C3 C4 C5 121.1(3) . . ? C3 C4 C9 119.6(2) . . ? C5 C4 C9 119.3(3) . . ? C6 C5 C4 120.8(3) . . ? C6 C5 H5 119.6 . . ? C4 C5 H5 119.6 . . ? C5 C6 C7 120.3(3) . . ? C5 C6 H6 119.9 . . ? C7 C6 H6 119.9 . . ? C8 C7 C6 120.8(3) . . ? C8 C7 H7 119.6 . . ? C6 C7 H7 119.6 . . ? C7 C8 C9 121.2(3) . . ? C7 C8 H8 119.4 . . ? C9 C8 H8 119.4 . . ? C8 C9 C4 117.6(2) . . ? C8 C9 C10 123.3(2) . . ? C4 C9 C10 119.1(2) . . ? C1 C10 C9 117.4(2) . . ? C1 C10 C11 119.6(2) . . ? C9 C10 C11 122.9(2) . . ? C20 C11 C12 117.2(2) . . ? C20 C11 C10 119.9(2) . . ? C12 C11 C10 122.8(2) . . ? C13 C12 C17 118.5(2) . . ? C13 C12 C11 122.3(2) . . ? C17 C12 C11 119.1(2) . . ? C14 C13 C12 121.1(3) . . ? C14 C13 H13 119.4 . . ? C12 C13 H13 119.4 . . ? C13 C14 C15 120.2(3) . . ? C13 C14 H14 119.9 . . ? C15 C14 H14 119.9 . . ? C16 C15 C14 119.9(3) . . ? C16 C15 H15 120.0 . . ? C14 C15 H15 120.0 . . ? C15 C16 C17 121.4(3) . . ? C15 C16 H16 119.3 . . ? C17 C16 H16 119.3 . . ? C18 C17 C16 121.7(3) . . ? C18 C17 C12 119.4(3) . . ? C16 C17 C12 118.8(3) . . ? C19 C18 C17 121.2(3) . . ? C19 C18 H18 119.4 . . ? C17 C18 H18 119.4 . . ? C18 C19 C20 118.9(3) . . ? C18 C19 H19 120.6 . . ? C20 C19 H19 120.6 . . ? C11 C20 C19 124.1(3) . . ? C11 C20 O2 118.2(2) . . ? C19 C20 O2 117.6(2) . . ? N1 C36 C37 102.6(2) . . ? N1 C36 H36A 111.2 . . ? C37 C36 H36A 111.2 . . ? N1 C36 H36B 111.2 . . ? C37 C36 H36B 111.2 . . ? H36A C36 H36B 109.2 . . ? N2 C37 C36 102.8(2) . . ? N2 C37 H37A 111.2 . . ? C36 C37 H37A 111.2 . . ? N2 C37 H37B 111.2 . . ? C36 C37 H37B 111.2 . . ? H37A C37 H37B 109.1 . . ? C39 C38 C43 120.8(3) . . ? C39 C38 N1 120.2(2) . . ? C43 C38 N1 118.9(2) . . ? C40 C39 C38 118.5(3) . . ? C40 C39 C44 119.7(3) . . ? C38 C39 C44 121.8(2) . . ? C39 C40 C41 122.3(3) . . ? C39 C40 H40 118.9 . . ? C41 C40 H40 118.9 . . ? C42 C41 C40 118.0(3) . . ? C42 C41 C45 120.7(3) . . ? C40 C41 C45 121.3(3) . . ? C41 C42 C43 121.9(3) . . ? C41 C42 H42 119.0 . . ? C43 C42 H42 119.0 . . ? C42 C43 C38 118.3(3) . . ? C42 C43 C46 118.9(3) . . ? C38 C43 C46 122.8(3) . . ? C39 C44 H44A 109.5 . . ? C39 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C39 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C41 C45 H45A 109.5 . . ? C41 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C41 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C43 C46 H46A 109.5 . . ? C43 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C43 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C48 C47 C52 121.3(3) . . ? C48 C47 N2 119.7(2) . . ? C52 C47 N2 118.8(3) . . ? C47 C48 C49 118.5(3) . . ? C47 C48 C53 122.3(3) . . ? C49 C48 C53 119.2(3) . . ? C50 C49 C48 121.8(3) . . ? C50 C49 H49 119.1 . . ? C48 C49 H49 119.1 . . ? C49 C50 C51 118.2(3) . . ? C49 C50 C54 120.4(3) . . ? C51 C50 C54 121.4(3) . . ? C50 C51 C52 122.6(3) . . ? C50 C51 H51 118.7 . . ? C52 C51 H51 118.7 . . ? C51 C52 C47 117.5(3) . . ? C51 C52 C55 120.4(3) . . ? C47 C52 C55 122.0(3) . . ? C48 C53 H53A 109.5 . . ? C48 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C48 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C50 C54 H54A 109.5 . . ? C50 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C50 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C52 C55 H55A 109.5 . . ? C52 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? C52 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? C25 C26 C21 115.4(2) . . ? C25 C26 Pd1 126.91(19) . . ? C21 C26 Pd1 117.69(17) . . ? C24 C25 C26 122.9(2) . . ? C24 C25 H25 118.6 . . ? C26 C25 H25 118.6 . . ? C25 C24 C23 117.8(2) . . ? C25 C24 C31 123.4(2) . . ? C23 C24 C31 118.7(2) . . ? C24 C23 C22 123.3(2) . . ? C24 C23 H23 118.4 . . ? C22 C23 H23 118.4 . . ? C21 C22 C23 115.2(2) . . ? C21 C22 C27 122.6(2) . . ? C23 C22 C27 122.1(2) . . ? C22 C21 C26 125.3(2) . . ? C22 C21 O3 115.9(2) . . ? C26 C21 O3 118.8(2) . . ? C34 C31 C32 109.4(2) . . ? C34 C31 C33 107.6(3) . . ? C32 C31 C33 108.6(3) . . ? C34 C31 C24 112.2(2) . . ? C32 C31 C24 109.0(2) . . ? C33 C31 C24 110.1(2) . . ? C31 C34 H34A 109.5 . . ? C31 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C31 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C31 C33 H33A 109.5 . . ? C31 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C31 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C30 C27 C29 107.6(2) . . ? C30 C27 C22 111.2(2) . . ? C29 C27 C22 110.2(2) . . ? C30 C27 C28 106.9(2) . . ? C29 C27 C28 110.2(2) . . ? C22 C27 C28 110.7(2) . . ? C27 C30 H30A 109.5 . . ? C27 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C27 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? N1 C35 N2 108.5(2) . . ? N1 C35 Pd1 121.20(19) . . ? N2 C35 Pd1 130.1(2) . . ? Cl3 C56 Cl2 114.4(4) . . ? Cl3 C56 H56A 108.7 . . ? Cl2 C56 H56A 108.7 . . ? Cl3 C56 H56B 108.7 . . ? Cl2 C56 H56B 108.7 . . ? H56A C56 H56B 107.6 . . ? Cl5 C57 Cl4 110.9(6) . . ? Cl5 C57 H57A 109.5 . . ? Cl4 C57 H57A 109.5 . . ? Cl5 C57 H57B 109.5 . . ? Cl4 C57 H57B 109.5 . . ? H57A C57 H57B 108.0 . . ? Cl7 C58 Cl6 112.8(6) . . ? Cl7 C58 H58A 109.0 . . ? Cl6 C58 H58A 109.0 . . ? Cl7 C58 H58B 109.0 . . ? Cl6 C58 H58B 109.0 . . ? H58A C58 H58B 107.8 . . ? 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 C26 Pd1 P1 O3 8.56(11) . . . . ? Cl1 Pd1 P1 O3 -168.39(8) . . . . ? C26 Pd1 P1 O1 129.56(11) . . . . ? Cl1 Pd1 P1 O1 -47.39(9) . . . . ? C26 Pd1 P1 O2 -102.66(11) . . . . ? Cl1 Pd1 P1 O2 80.39(8) . . . . ? O3 P1 O1 C1 -60.7(2) . . . . ? O2 P1 O1 C1 41.6(2) . . . . ? Pd1 P1 O1 C1 176.00(15) . . . . ? O3 P1 O2 C20 157.15(18) . . . . ? O1 P1 O2 C20 50.53(19) . . . . ? Pd1 P1 O2 C20 -85.98(18) . . . . ? O1 P1 O3 C21 -140.91(17) . . . . ? O2 P1 O3 C21 113.94(18) . . . . ? Pd1 P1 O3 C21 -9.67(19) . . . . ? P1 O1 C1 C10 -72.7(3) . . . . ? P1 O1 C1 C2 109.1(2) . . . . ? C10 C1 C2 C3 2.1(4) . . . . ? O1 C1 C2 C3 -179.8(2) . . . . ? C1 C2 C3 C4 1.1(4) . . . . ? C2 C3 C4 C5 178.8(3) . . . . ? C2 C3 C4 C9 -1.5(4) . . . . ? C3 C4 C5 C6 -179.5(3) . . . . ? C9 C4 C5 C6 0.8(4) . . . . ? C4 C5 C6 C7 0.9(5) . . . . ? C5 C6 C7 C8 -0.6(5) . . . . ? C6 C7 C8 C9 -1.3(5) . . . . ? C7 C8 C9 C4 2.9(4) . . . . ? C7 C8 C9 C10 -178.3(3) . . . . ? C3 C4 C9 C8 177.7(3) . . . . ? C5 C4 C9 C8 -2.6(4) . . . . ? C3 C4 C9 C10 -1.2(4) . . . . ? C5 C4 C9 C10 178.5(2) . . . . ? O1 C1 C10 C9 177.3(2) . . . . ? C2 C1 C10 C9 -4.6(4) . . . . ? O1 C1 C10 C11 -0.5(4) . . . . ? C2 C1 C10 C11 177.6(2) . . . . ? C8 C9 C10 C1 -174.7(3) . . . . ? C4 C9 C10 C1 4.0(4) . . . . ? C8 C9 C10 C11 3.0(4) . . . . ? C4 C9 C10 C11 -178.2(2) . . . . ? C1 C10 C11 C20 51.6(3) . . . . ? C9 C10 C11 C20 -126.1(3) . . . . ? C1 C10 C11 C12 -124.3(3) . . . . ? C9 C10 C11 C12 58.1(4) . . . . ? C20 C11 C12 C13 -172.6(2) . . . . ? C10 C11 C12 C13 3.4(4) . . . . ? C20 C11 C12 C17 3.7(4) . . . . ? C10 C11 C12 C17 179.6(2) . . . . ? C17 C12 C13 C14 1.7(4) . . . . ? C11 C12 C13 C14 178.0(2) . . . . ? C12 C13 C14 C15 0.2(4) . . . . ? C13 C14 C15 C16 -1.2(4) . . . . ? C14 C15 C16 C17 0.3(4) . . . . ? C15 C16 C17 C18 -176.4(3) . . . . ? C15 C16 C17 C12 1.7(4) . . . . ? C13 C12 C17 C18 175.5(2) . . . . ? C11 C12 C17 C18 -0.9(4) . . . . ? C13 C12 C17 C16 -2.6(4) . . . . ? C11 C12 C17 C16 -179.0(2) . . . . ? C16 C17 C18 C19 176.2(3) . . . . ? C12 C17 C18 C19 -1.9(4) . . . . ? C17 C18 C19 C20 1.8(4) . . . . ? C12 C11 C20 C19 -4.0(4) . . . . ? C10 C11 C20 C19 179.9(2) . . . . ? C12 C11 C20 O2 176.2(2) . . . . ? C10 C11 C20 O2 0.2(4) . . . . ? C18 C19 C20 C11 1.3(4) . . . . ? C18 C19 C20 O2 -179.0(2) . . . . ? P1 O2 C20 C11 -77.6(3) . . . . ? P1 O2 C20 C19 102.7(2) . . . . ? C35 N1 C36 C37 3.7(3) . . . . ? C38 N1 C36 C37 171.4(2) . . . . ? C35 N2 C37 C36 1.6(3) . . . . ? C47 N2 C37 C36 -163.6(2) . . . . ? N1 C36 C37 N2 -3.0(3) . . . . ? C35 N1 C38 C39 -98.9(3) . . . . ? C36 N1 C38 C39 95.0(3) . . . . ? C35 N1 C38 C43 84.3(3) . . . . ? C36 N1 C38 C43 -81.8(3) . . . . ? C43 C38 C39 C40 -3.9(4) . . . . ? N1 C38 C39 C40 179.3(2) . . . . ? C43 C38 C39 C44 175.5(3) . . . . ? N1 C38 C39 C44 -1.3(4) . . . . ? C38 C39 C40 C41 1.4(4) . . . . ? C44 C39 C40 C41 -177.9(3) . . . . ? C39 C40 C41 C42 1.3(4) . . . . ? C39 C40 C41 C45 -179.7(3) . . . . ? C40 C41 C42 C43 -1.8(4) . . . . ? C45 C41 C42 C43 179.2(3) . . . . ? C41 C42 C43 C38 -0.5(4) . . . . ? C41 C42 C43 C46 177.6(3) . . . . ? C39 C38 C43 C42 3.4(4) . . . . ? N1 C38 C43 C42 -179.7(2) . . . . ? C39 C38 C43 C46 -174.6(3) . . . . ? N1 C38 C43 C46 2.2(4) . . . . ? C35 N2 C47 C48 110.5(3) . . . . ? C37 N2 C47 C48 -86.2(3) . . . . ? C35 N2 C47 C52 -73.9(3) . . . . ? C37 N2 C47 C52 89.4(3) . . . . ? C52 C47 C48 C49 4.2(4) . . . . ? N2 C47 C48 C49 179.7(2) . . . . ? C52 C47 C48 C53 -174.9(3) . . . . ? N2 C47 C48 C53 0.6(4) . . . . ? C47 C48 C49 C50 -1.0(4) . . . . ? C53 C48 C49 C50 178.1(3) . . . . ? C48 C49 C50 C51 -2.1(4) . . . . ? C48 C49 C50 C54 178.0(3) . . . . ? C49 C50 C51 C52 2.2(4) . . . . ? C54 C50 C51 C52 -177.9(3) . . . . ? C50 C51 C52 C47 0.8(4) . . . . ? C50 C51 C52 C55 -176.0(3) . . . . ? C48 C47 C52 C51 -4.1(4) . . . . ? N2 C47 C52 C51 -179.6(2) . . . . ? C48 C47 C52 C55 172.7(3) . . . . ? N2 C47 C52 C55 -2.8(4) . . . . ? C35 Pd1 C26 C25 1.8(2) . . . . ? P1 Pd1 C26 C25 174.1(2) . . . . ? Cl1 Pd1 C26 C25 -169.3(3) . . . . ? C35 Pd1 C26 C21 -179.2(2) . . . . ? P1 Pd1 C26 C21 -6.86(19) . . . . ? Cl1 Pd1 C26 C21 9.7(5) . . . . ? C21 C26 C25 C24 -1.9(4) . . . . ? Pd1 C26 C25 C24 177.19(19) . . . . ? C26 C25 C24 C23 0.1(4) . . . . ? C26 C25 C24 C31 -178.5(2) . . . . ? C25 C24 C23 C22 1.4(4) . . . . ? C31 C24 C23 C22 -179.9(2) . . . . ? C24 C23 C22 C21 -0.9(4) . . . . ? C24 C23 C22 C27 179.7(2) . . . . ? C23 C22 C21 C26 -1.1(4) . . . . ? C27 C22 C21 C26 178.2(2) . . . . ? C23 C22 C21 O3 179.1(2) . . . . ? C27 C22 C21 O3 -1.5(4) . . . . ? C25 C26 C21 C22 2.5(4) . . . . ? Pd1 C26 C21 C22 -176.7(2) . . . . ? C25 C26 C21 O3 -177.8(2) . . . . ? Pd1 C26 C21 O3 3.1(3) . . . . ? P1 O3 C21 C22 -175.33(19) . . . . ? P1 O3 C21 C26 4.9(3) . . . . ? C25 C24 C31 C34 -13.9(4) . . . . ? C23 C24 C31 C34 167.6(3) . . . . ? C25 C24 C31 C32 107.4(3) . . . . ? C23 C24 C31 C32 -71.1(3) . . . . ? C25 C24 C31 C33 -133.6(3) . . . . ? C23 C24 C31 C33 47.9(4) . . . . ? C21 C22 C27 C30 178.9(2) . . . . ? C23 C22 C27 C30 -1.8(3) . . . . ? C21 C22 C27 C29 -61.9(3) . . . . ? C23 C22 C27 C29 117.4(3) . . . . ? C21 C22 C27 C28 60.2(3) . . . . ? C23 C22 C27 C28 -120.5(3) . . . . ? C38 N1 C35 N2 -169.9(2) . . . . ? C36 N1 C35 N2 -2.9(3) . . . . ? C38 N1 C35 Pd1 14.6(3) . . . . ? C36 N1 C35 Pd1 -178.36(19) . . . . ? C47 N2 C35 N1 164.9(2) . . . . ? C37 N2 C35 N1 0.7(3) . . . . ? C47 N2 C35 Pd1 -20.1(4) . . . . ? C37 N2 C35 Pd1 175.61(19) . . . . ? C26 Pd1 C35 N1 91.4(2) . . . . ? Cl1 Pd1 C35 N1 -90.3(2) . . . . ? C26 Pd1 C35 N2 -83.0(2) . . . . ? Cl1 Pd1 C35 N2 95.3(2) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.574 _refine_diff_density_min -0.629 _refine_diff_density_rms 0.078 # Attachment '17.cif' data_choclatsad _database_code_depnum_ccdc_archive 'CCDC 727730' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C68 H64 Cl2 O6 P2 Pt2' _chemical_formula_sum 'C68 H64 Cl2 O6 P2 Pt2' _chemical_formula_weight 1500.21 _chemical_absolute_configuration ad loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2 _symmetry_space_group_name_Hall C2y loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' _cell_length_a 17.724(3) _cell_length_b 10.2340(16) _cell_length_c 17.561(3) _cell_angle_alpha 90.00 _cell_angle_beta 108.246(3) _cell_angle_gamma 90.00 _cell_volume 3025.2(9) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 143 _cell_measurement_theta_min 2.33 _cell_measurement_theta_max 27.51 _exptl_crystal_description rod _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.647 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1480 _exptl_absorpt_coefficient_mu 4.812 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.384 _exptl_absorpt_correction_T_max 0.618 _exptl_absorpt_process_details 'SADABS V2.05' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 9873 _diffrn_reflns_av_R_equivalents 0.0296 _diffrn_reflns_av_sigmaI/netI 0.0704 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.33 _diffrn_reflns_theta_max 27.51 _reflns_number_total 6748 _reflns_number_gt 5712 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0393P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881, based on 3084 Friedel pairs' _refine_ls_abs_structure_Flack -0.009(9) _refine_ls_number_reflns 6748 _refine_ls_number_parameters 368 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0524 _refine_ls_R_factor_gt 0.0376 _refine_ls_wR_factor_ref 0.0824 _refine_ls_wR_factor_gt 0.0770 _refine_ls_goodness_of_fit_ref 0.968 _refine_ls_restrained_S_all 0.968 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.487008(12) -0.00185(5) 0.096795(12) 0.02100(7) Uani 1 1 d . . . P1 P 0.55263(10) 0.03562(16) 0.21852(11) 0.0218(5) Uani 1 1 d . . . Cl1 Cl 0.40637(9) -0.0279(3) -0.03932(9) 0.0309(7) Uani 1 1 d . . . O1 O 0.6194(3) -0.0624(5) 0.2708(3) 0.0229(10) Uani 1 1 d . . . O2 O 0.5968(3) 0.1738(5) 0.2327(3) 0.0259(11) Uani 1 1 d . . . O3 O 0.4949(3) 0.0362(5) 0.2716(3) 0.0286(15) Uani 1 1 d . . . C1 C 0.6928(4) -0.0582(7) 0.2530(4) 0.0218(15) Uani 1 1 d . . . C2 C 0.7085(4) -0.1627(7) 0.2078(4) 0.0247(16) Uani 1 1 d . . . H2 H 0.6720 -0.2328 0.1908 0.030 Uiso 1 1 calc R . . C3 C 0.7774(5) -0.1602(8) 0.1891(4) 0.0307(17) Uani 1 1 d . . . H3 H 0.7894 -0.2308 0.1597 0.037 Uiso 1 1 calc R . . C4 C 0.8311(4) -0.0564(7) 0.2121(4) 0.0285(17) Uani 1 1 d . . . C5 C 0.9026(5) -0.0520(9) 0.1917(5) 0.041(2) Uani 1 1 d . . . H5 H 0.9164 -0.1235 0.1643 0.049 Uiso 1 1 calc R . . C6 C 0.9515(5) 0.0543(10) 0.2113(5) 0.044(2) Uani 1 1 d . . . H6 H 1.0004 0.0542 0.1997 0.053 Uiso 1 1 calc R . . C7 C 0.9304(5) 0.1632(10) 0.2480(5) 0.040(2) Uani 1 1 d . . . H7 H 0.9629 0.2390 0.2572 0.048 Uiso 1 1 calc R . . C8 C 0.8636(4) 0.1617(8) 0.2707(4) 0.0305(18) Uani 1 1 d . . . H8 H 0.8507 0.2356 0.2969 0.037 Uiso 1 1 calc R . . C9 C 0.8132(4) 0.0511(7) 0.2555(4) 0.0251(16) Uani 1 1 d . . . C10 C 0.7434(4) 0.0454(7) 0.2809(4) 0.0227(16) Uani 1 1 d . . . C11 C 0.7237(4) 0.1457(7) 0.3327(4) 0.0228(15) Uani 1 1 d . . . C12 C 0.7765(4) 0.1774(7) 0.4112(4) 0.0228(15) Uani 1 1 d . . . C13 C 0.8508(4) 0.1150(8) 0.4459(4) 0.0288(17) Uani 1 1 d . . . H13 H 0.8673 0.0486 0.4168 0.035 Uiso 1 1 calc R . . C14 C 0.8991(5) 0.1489(9) 0.5204(4) 0.035(2) Uani 1 1 d . . . H14 H 0.9487 0.1061 0.5425 0.042 Uiso 1 1 calc R . . C15 C 0.8759(5) 0.2473(9) 0.5651(4) 0.040(2) Uani 1 1 d . . . H15 H 0.9098 0.2707 0.6168 0.049 Uiso 1 1 calc R . . C16 C 0.8050(5) 0.3081(9) 0.5338(4) 0.0362(19) Uani 1 1 d . . . H16 H 0.7902 0.3752 0.5637 0.043 Uiso 1 1 calc R . . C17 C 0.7520(5) 0.2736(8) 0.4570(4) 0.0299(17) Uani 1 1 d . . . C18 C 0.6777(4) 0.3342(8) 0.4267(5) 0.0335(18) Uani 1 1 d . . . H18 H 0.6625 0.3993 0.4576 0.040 Uiso 1 1 calc R . . C19 C 0.6271(4) 0.3007(7) 0.3533(4) 0.0284(17) Uani 1 1 d . . . H19 H 0.5766 0.3414 0.3329 0.034 Uiso 1 1 calc R . . C20 C 0.6509(4) 0.2052(7) 0.3088(4) 0.0255(16) Uani 1 1 d . . . C21 C 0.3972(3) 0.0076(13) 0.1433(3) 0.0217(15) Uani 1 1 d . . . C22 C 0.3177(3) -0.0141(12) 0.0981(4) 0.0249(16) Uani 1 1 d . . . H22 H 0.3047 -0.0290 0.0421 0.030 Uiso 1 1 calc R . . C23 C 0.2572(3) -0.0146(11) 0.1330(3) 0.0214(15) Uani 1 1 d . . . C24 C 0.2776(4) 0.0118(11) 0.2148(4) 0.0244(17) Uani 1 1 d . . . H24 H 0.2363 0.0140 0.2386 0.029 Uiso 1 1 calc R . . C25 C 0.3553(4) 0.0350(6) 0.2637(4) 0.0208(17) Uani 1 1 d . . . C26 C 0.4124(4) 0.0259(7) 0.2248(4) 0.025(2) Uani 1 1 d . . . C27 C 0.1712(4) -0.0371(7) 0.0779(4) 0.027(2) Uani 1 1 d . . . C28 C 0.1663(5) -0.1718(10) 0.0400(6) 0.052(3) Uani 1 1 d . . . H28A H 0.1110 -0.1913 0.0096 0.078 Uiso 1 1 calc R . . H28B H 0.1861 -0.2375 0.0822 0.078 Uiso 1 1 calc R . . H28C H 0.1988 -0.1733 0.0039 0.078 Uiso 1 1 calc R . . C29 C 0.1476(5) 0.0706(10) 0.0151(5) 0.043(2) Uani 1 1 d . . . H29A H 0.1868 0.0757 -0.0136 0.065 Uiso 1 1 calc R . . H29B H 0.1456 0.1543 0.0415 0.065 Uiso 1 1 calc R . . H29C H 0.0952 0.0511 -0.0229 0.065 Uiso 1 1 calc R . . C30 C 0.1121(4) -0.0332(11) 0.1266(5) 0.047(3) Uani 1 1 d . . . H30A H 0.0577 -0.0409 0.0900 0.071 Uiso 1 1 calc R . . H30B H 0.1179 0.0497 0.1558 0.071 Uiso 1 1 calc R . . H30C H 0.1232 -0.1059 0.1648 0.071 Uiso 1 1 calc R . . C31 C 0.3747(4) 0.0674(8) 0.3539(4) 0.0282(17) Uani 1 1 d . . . C32 C 0.2991(4) 0.0863(9) 0.3767(5) 0.038(2) Uani 1 1 d . . . H32A H 0.2677 0.0056 0.3659 0.057 Uiso 1 1 calc R . . H32B H 0.2678 0.1579 0.3451 0.057 Uiso 1 1 calc R . . H32C H 0.3132 0.1074 0.4339 0.057 Uiso 1 1 calc R . . C33 C 0.4227(5) 0.1944(8) 0.3742(5) 0.040(2) Uani 1 1 d . . . H33A H 0.4290 0.2193 0.4297 0.060 Uiso 1 1 calc R . . H33B H 0.3947 0.2639 0.3379 0.060 Uiso 1 1 calc R . . H33C H 0.4752 0.1810 0.3679 0.060 Uiso 1 1 calc R . . C34 C 0.4220(5) -0.0429(7) 0.4049(4) 0.035(2) Uani 1 1 d . . . H34A H 0.4349 -0.0200 0.4617 0.053 Uiso 1 1 calc R . . H34B H 0.4711 -0.0565 0.3916 0.053 Uiso 1 1 calc R . . H34C H 0.3903 -0.1232 0.3942 0.053 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.01577(10) 0.03510(13) 0.01221(10) 0.0001(2) 0.00452(7) -0.0022(2) P1 0.0157(8) 0.0324(14) 0.0170(8) 0.0000(7) 0.0046(6) -0.0025(7) Cl1 0.0185(7) 0.061(2) 0.0137(7) -0.0040(9) 0.0053(6) -0.0026(9) O1 0.019(2) 0.030(3) 0.020(2) -0.001(2) 0.005(2) -0.001(2) O2 0.021(2) 0.035(3) 0.017(2) 0.002(2) -0.001(2) 0.000(2) O3 0.016(2) 0.058(5) 0.015(2) -0.005(2) 0.0095(18) -0.008(2) C1 0.019(3) 0.031(4) 0.013(3) 0.006(3) 0.000(3) 0.004(3) C2 0.027(4) 0.022(4) 0.019(4) -0.007(3) -0.001(3) 0.000(3) C3 0.034(4) 0.032(4) 0.024(4) 0.003(3) 0.006(3) 0.008(4) C4 0.020(4) 0.040(4) 0.022(4) 0.005(3) 0.001(3) 0.012(3) C5 0.033(4) 0.066(6) 0.028(4) 0.000(4) 0.017(4) 0.011(4) C6 0.026(4) 0.078(7) 0.030(5) 0.005(4) 0.012(4) 0.014(4) C7 0.026(4) 0.069(6) 0.026(4) 0.001(4) 0.008(3) -0.008(4) C8 0.024(4) 0.046(5) 0.022(4) 0.000(3) 0.007(3) -0.007(3) C9 0.021(4) 0.040(4) 0.017(4) 0.006(3) 0.009(3) 0.002(3) C10 0.018(3) 0.031(4) 0.017(3) -0.001(3) 0.003(3) 0.002(3) C11 0.020(3) 0.032(4) 0.013(3) 0.002(3) 0.001(3) -0.003(3) C12 0.017(3) 0.033(4) 0.019(4) -0.005(3) 0.006(3) -0.007(3) C13 0.022(4) 0.050(5) 0.016(4) -0.004(3) 0.008(3) -0.003(3) C14 0.024(4) 0.054(5) 0.022(4) 0.012(4) -0.001(3) -0.007(4) C15 0.040(5) 0.067(6) 0.013(4) -0.009(4) 0.006(3) -0.020(4) C16 0.040(5) 0.053(5) 0.018(4) -0.006(4) 0.012(3) -0.010(4) C17 0.035(4) 0.040(5) 0.018(4) -0.008(3) 0.014(3) -0.012(4) C18 0.030(4) 0.042(5) 0.032(4) -0.010(4) 0.014(3) -0.009(4) C19 0.023(4) 0.033(4) 0.032(4) -0.002(3) 0.013(3) -0.002(3) C20 0.021(4) 0.033(4) 0.020(4) -0.002(3) 0.003(3) -0.005(3) C21 0.021(3) 0.027(4) 0.020(3) 0.008(5) 0.011(2) 0.003(5) C22 0.022(3) 0.037(5) 0.016(3) 0.001(4) 0.007(2) -0.005(5) C23 0.019(3) 0.024(4) 0.020(3) -0.003(4) 0.005(2) -0.002(4) C24 0.022(3) 0.032(5) 0.023(3) 0.002(4) 0.013(2) -0.002(4) C25 0.027(3) 0.029(5) 0.010(3) 0.000(2) 0.010(3) -0.004(3) C26 0.015(3) 0.031(6) 0.029(3) -0.006(3) 0.006(3) -0.005(3) C27 0.022(3) 0.038(6) 0.023(4) -0.005(3) 0.009(3) -0.005(3) C28 0.034(5) 0.060(7) 0.056(6) -0.024(5) 0.006(5) -0.010(5) C29 0.032(5) 0.069(6) 0.022(4) 0.004(4) -0.001(4) -0.003(4) C30 0.021(3) 0.088(10) 0.033(4) -0.003(5) 0.008(3) -0.015(4) C31 0.027(4) 0.049(5) 0.007(3) 0.005(3) 0.004(3) 0.007(3) C32 0.030(4) 0.065(6) 0.023(4) 0.002(4) 0.014(3) 0.003(4) C33 0.054(5) 0.050(5) 0.020(4) -0.011(4) 0.015(4) -0.014(4) C34 0.035(4) 0.051(6) 0.019(4) 0.005(3) 0.006(3) 0.010(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 C21 2.006(6) . ? Pt1 P1 2.1243(18) . ? Pt1 Cl1 2.3849(16) . ? Pt1 Cl1 2.4197(16) 2_655 ? P1 O3 1.585(5) . ? P1 O2 1.598(5) . ? P1 O1 1.603(5) . ? Cl1 Pt1 2.4198(16) 2_655 ? O1 C1 1.429(8) . ? O2 C20 1.417(8) . ? O3 C26 1.440(7) . ? C1 C10 1.376(9) . ? C1 C2 1.412(10) . ? C2 C3 1.359(11) . ? C2 H2 0.9500 . ? C3 C4 1.399(11) . ? C3 H3 0.9500 . ? C4 C5 1.421(11) . ? C4 C9 1.429(10) . ? C5 C6 1.367(12) . ? C5 H5 0.9500 . ? C6 C7 1.396(12) . ? C6 H6 0.9500 . ? C7 C8 1.363(11) . ? C7 H7 0.9500 . ? C8 C9 1.415(10) . ? C8 H8 0.9500 . ? C9 C10 1.443(10) . ? C10 C11 1.484(10) . ? C11 C20 1.368(9) . ? C11 C12 1.440(9) . ? C12 C13 1.418(10) . ? C12 C17 1.422(10) . ? C13 C14 1.366(10) . ? C13 H13 0.9500 . ? C14 C15 1.414(12) . ? C14 H14 0.9500 . ? C15 C16 1.355(12) . ? C15 H15 0.9500 . ? C16 C17 1.426(10) . ? C16 H16 0.9500 . ? C17 C18 1.401(11) . ? C18 C19 1.363(10) . ? C18 H18 0.9500 . ? C19 C20 1.396(10) . ? C19 H19 0.9500 . ? C21 C26 1.384(9) . ? C21 C22 1.402(8) . ? C22 C23 1.391(8) . ? C22 H22 0.9500 . ? C23 C24 1.394(9) . ? C23 C27 1.546(9) . ? C24 C25 1.396(9) . ? C24 H24 0.9500 . ? C25 C26 1.389(9) . ? C25 C31 1.548(9) . ? C27 C28 1.521(11) . ? C27 C29 1.522(11) . ? C27 C30 1.546(10) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 C34 1.519(10) . ? C31 C32 1.527(10) . ? C31 C33 1.533(11) . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 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 C21 Pt1 P1 80.53(19) . . ? C21 Pt1 Cl1 96.36(17) . . ? P1 Pt1 Cl1 175.01(8) . . ? C21 Pt1 Cl1 176.4(4) . 2_655 ? P1 Pt1 Cl1 100.76(6) . 2_655 ? Cl1 Pt1 Cl1 82.58(6) . 2_655 ? O3 P1 O2 106.3(3) . . ? O3 P1 O1 99.4(3) . . ? O2 P1 O1 103.1(3) . . ? O3 P1 Pt1 109.96(18) . . ? O2 P1 Pt1 113.79(19) . . ? O1 P1 Pt1 122.45(19) . . ? Pt1 Cl1 Pt1 96.00(6) . 2_655 ? C1 O1 P1 114.5(4) . . ? C20 O2 P1 120.1(4) . . ? C26 O3 P1 113.1(4) . . ? C10 C1 C2 124.2(7) . . ? C10 C1 O1 118.8(6) . . ? C2 C1 O1 117.0(6) . . ? C3 C2 C1 118.2(7) . . ? C3 C2 H2 120.9 . . ? C1 C2 H2 120.9 . . ? C2 C3 C4 121.7(7) . . ? C2 C3 H3 119.1 . . ? C4 C3 H3 119.1 . . ? C3 C4 C5 122.1(8) . . ? C3 C4 C9 119.6(7) . . ? C5 C4 C9 118.3(7) . . ? C6 C5 C4 120.5(8) . . ? C6 C5 H5 119.7 . . ? C4 C5 H5 119.7 . . ? C5 C6 C7 120.7(8) . . ? C5 C6 H6 119.7 . . ? C7 C6 H6 119.7 . . ? C8 C7 C6 120.7(9) . . ? C8 C7 H7 119.7 . . ? C6 C7 H7 119.7 . . ? C7 C8 C9 120.5(8) . . ? C7 C8 H8 119.7 . . ? C9 C8 H8 119.7 . . ? C8 C9 C4 119.0(7) . . ? C8 C9 C10 121.7(7) . . ? C4 C9 C10 119.3(7) . . ? C1 C10 C9 116.6(6) . . ? C1 C10 C11 119.9(6) . . ? C9 C10 C11 123.4(6) . . ? C20 C11 C12 117.5(7) . . ? C20 C11 C10 120.0(6) . . ? C12 C11 C10 122.4(6) . . ? C13 C12 C17 118.4(6) . . ? C13 C12 C11 123.3(7) . . ? C17 C12 C11 118.3(6) . . ? C14 C13 C12 121.1(7) . . ? C14 C13 H13 119.4 . . ? C12 C13 H13 119.4 . . ? C13 C14 C15 120.6(8) . . ? C13 C14 H14 119.7 . . ? C15 C14 H14 119.7 . . ? C16 C15 C14 119.7(7) . . ? C16 C15 H15 120.1 . . ? C14 C15 H15 120.1 . . ? C15 C16 C17 121.5(8) . . ? C15 C16 H16 119.2 . . ? C17 C16 H16 119.2 . . ? C18 C17 C12 120.6(7) . . ? C18 C17 C16 120.8(7) . . ? C12 C17 C16 118.6(7) . . ? C19 C18 C17 120.6(7) . . ? C19 C18 H18 119.7 . . ? C17 C18 H18 119.7 . . ? C18 C19 C20 118.7(7) . . ? C18 C19 H19 120.7 . . ? C20 C19 H19 120.7 . . ? C11 C20 C19 124.1(6) . . ? C11 C20 O2 118.9(6) . . ? C19 C20 O2 117.0(6) . . ? C26 C21 C22 116.3(5) . . ? C26 C21 Pt1 120.4(4) . . ? C22 C21 Pt1 123.1(5) . . ? C23 C22 C21 121.8(6) . . ? C23 C22 H22 119.1 . . ? C21 C22 H22 119.1 . . ? C22 C23 C24 117.8(6) . . ? C22 C23 C27 118.1(5) . . ? C24 C23 C27 124.0(5) . . ? C23 C24 C25 123.7(6) . . ? C23 C24 H24 118.2 . . ? C25 C24 H24 118.2 . . ? C26 C25 C24 114.6(6) . . ? C26 C25 C31 123.6(6) . . ? C24 C25 C31 121.7(6) . . ? C21 C26 C25 125.6(6) . . ? C21 C26 O3 115.7(5) . . ? C25 C26 O3 118.8(6) . . ? C28 C27 C29 111.9(7) . . ? C28 C27 C30 108.1(7) . . ? C29 C27 C30 107.6(7) . . ? C28 C27 C23 108.6(7) . . ? C29 C27 C23 109.8(6) . . ? C30 C27 C23 110.9(5) . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C27 C30 H30A 109.5 . . ? C27 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C27 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C34 C31 C32 107.8(6) . . ? C34 C31 C33 109.2(6) . . ? C32 C31 C33 107.5(7) . . ? C34 C31 C25 110.4(6) . . ? C32 C31 C25 111.3(6) . . ? C33 C31 C25 110.4(6) . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C31 C33 H33A 109.5 . . ? C31 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C31 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C31 C34 H34A 109.5 . . ? C31 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C31 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 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 C21 Pt1 P1 O3 4.7(4) . . . . ? Cl1 Pt1 P1 O3 -171.9(2) 2_655 . . . ? C21 Pt1 P1 O2 -114.4(4) . . . . ? Cl1 Pt1 P1 O2 69.0(2) 2_655 . . . ? C21 Pt1 P1 O1 120.6(4) . . . . ? Cl1 Pt1 P1 O1 -56.0(2) 2_655 . . . ? C21 Pt1 Cl1 Pt1 170.8(4) . . . 2_655 ? Cl1 Pt1 Cl1 Pt1 -12.63(14) 2_655 . . 2_655 ? O3 P1 O1 C1 -163.2(4) . . . . ? O2 P1 O1 C1 -53.9(5) . . . . ? Pt1 P1 O1 C1 75.8(5) . . . . ? O3 P1 O2 C20 66.9(5) . . . . ? O1 P1 O2 C20 -37.1(5) . . . . ? Pt1 P1 O2 C20 -171.9(4) . . . . ? O2 P1 O3 C26 117.3(4) . . . . ? O1 P1 O3 C26 -136.0(5) . . . . ? Pt1 P1 O3 C26 -6.3(5) . . . . ? P1 O1 C1 C10 75.7(7) . . . . ? P1 O1 C1 C2 -104.6(6) . . . . ? C10 C1 C2 C3 -1.2(10) . . . . ? O1 C1 C2 C3 179.1(6) . . . . ? C1 C2 C3 C4 -1.4(11) . . . . ? C2 C3 C4 C5 -179.0(7) . . . . ? C2 C3 C4 C9 -0.7(11) . . . . ? C3 C4 C5 C6 176.3(7) . . . . ? C9 C4 C5 C6 -1.9(11) . . . . ? C4 C5 C6 C7 -3.2(13) . . . . ? C5 C6 C7 C8 5.1(13) . . . . ? C6 C7 C8 C9 -1.7(12) . . . . ? C7 C8 C9 C4 -3.4(11) . . . . ? C7 C8 C9 C10 178.2(7) . . . . ? C3 C4 C9 C8 -173.2(7) . . . . ? C5 C4 C9 C8 5.1(10) . . . . ? C3 C4 C9 C10 5.3(10) . . . . ? C5 C4 C9 C10 -176.4(7) . . . . ? C2 C1 C10 C9 5.7(10) . . . . ? O1 C1 C10 C9 -174.7(6) . . . . ? C2 C1 C10 C11 -175.8(6) . . . . ? O1 C1 C10 C11 3.8(9) . . . . ? C8 C9 C10 C1 170.9(6) . . . . ? C4 C9 C10 C1 -7.5(9) . . . . ? C8 C9 C10 C11 -7.5(11) . . . . ? C4 C9 C10 C11 174.0(6) . . . . ? C1 C10 C11 C20 -51.9(9) . . . . ? C9 C10 C11 C20 126.4(8) . . . . ? C1 C10 C11 C12 123.4(7) . . . . ? C9 C10 C11 C12 -58.2(10) . . . . ? C20 C11 C12 C13 174.7(7) . . . . ? C10 C11 C12 C13 -0.7(11) . . . . ? C20 C11 C12 C17 -3.6(10) . . . . ? C10 C11 C12 C17 -179.1(7) . . . . ? C17 C12 C13 C14 -2.0(11) . . . . ? C11 C12 C13 C14 179.7(7) . . . . ? C12 C13 C14 C15 0.2(12) . . . . ? C13 C14 C15 C16 0.3(12) . . . . ? C14 C15 C16 C17 1.2(12) . . . . ? C13 C12 C17 C18 -177.4(7) . . . . ? C11 C12 C17 C18 1.0(11) . . . . ? C13 C12 C17 C16 3.3(11) . . . . ? C11 C12 C17 C16 -178.2(7) . . . . ? C15 C16 C17 C18 177.7(8) . . . . ? C15 C16 C17 C12 -3.0(12) . . . . ? C12 C17 C18 C19 1.0(12) . . . . ? C16 C17 C18 C19 -179.8(7) . . . . ? C17 C18 C19 C20 -0.3(12) . . . . ? C12 C11 C20 C19 4.5(11) . . . . ? C10 C11 C20 C19 -179.9(7) . . . . ? C12 C11 C20 O2 -178.5(6) . . . . ? C10 C11 C20 O2 -2.9(10) . . . . ? C18 C19 C20 C11 -2.6(12) . . . . ? C18 C19 C20 O2 -179.6(7) . . . . ? P1 O2 C20 C11 73.2(8) . . . . ? P1 O2 C20 C19 -109.6(7) . . . . ? P1 Pt1 C21 C26 -2.7(9) . . . . ? Cl1 Pt1 C21 C26 -178.8(9) . . . . ? P1 Pt1 C21 C22 -177.3(11) . . . . ? Cl1 Pt1 C21 C22 6.6(11) . . . . ? C26 C21 C22 C23 1.3(18) . . . . ? Pt1 C21 C22 C23 176.1(9) . . . . ? C21 C22 C23 C24 2.1(19) . . . . ? C21 C22 C23 C27 179.0(10) . . . . ? C22 C23 C24 C25 -1.7(18) . . . . ? C27 C23 C24 C25 -178.4(8) . . . . ? C23 C24 C25 C26 -2.0(14) . . . . ? C23 C24 C25 C31 178.4(10) . . . . ? C22 C21 C26 C25 -5.6(16) . . . . ? Pt1 C21 C26 C25 179.5(6) . . . . ? C22 C21 C26 O3 174.6(9) . . . . ? Pt1 C21 C26 O3 -0.4(12) . . . . ? C24 C25 C26 C21 5.8(12) . . . . ? C31 C25 C26 C21 -174.5(9) . . . . ? C24 C25 C26 O3 -174.3(7) . . . . ? C31 C25 C26 O3 5.4(10) . . . . ? P1 O3 C26 C21 4.6(9) . . . . ? P1 O3 C26 C25 -175.3(5) . . . . ? C22 C23 C27 C28 61.9(12) . . . . ? C24 C23 C27 C28 -121.4(11) . . . . ? C22 C23 C27 C29 -60.8(12) . . . . ? C24 C23 C27 C29 116.0(11) . . . . ? C22 C23 C27 C30 -179.5(10) . . . . ? C24 C23 C27 C30 -2.8(14) . . . . ? C26 C25 C31 C34 -66.9(9) . . . . ? C24 C25 C31 C34 112.7(9) . . . . ? C26 C25 C31 C32 173.3(7) . . . . ? C24 C25 C31 C32 -7.1(11) . . . . ? C26 C25 C31 C33 54.0(9) . . . . ? C24 C25 C31 C33 -126.4(8) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.165 _refine_diff_density_min -1.132 _refine_diff_density_rms 0.132 # Attachment '8.cif' data_berwicksad _database_code_depnum_ccdc_archive 'CCDC 727731' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C68 H64 Cl2 O6 P2 Pd2' _chemical_formula_sum 'C68 H64 Cl2 O6 P2 Pd2' _chemical_formula_weight 1322.83 _chemical_absolute_configuration ad 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 monoclinic _symmetry_space_group_name_H-M C2 _symmetry_space_group_name_Hall C2y loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' _cell_length_a 17.694(4) _cell_length_b 10.290(2) _cell_length_c 17.527(4) _cell_angle_alpha 90.00 _cell_angle_beta 108.220(3) _cell_angle_gamma 90.00 _cell_volume 3031.0(10) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 43 _cell_measurement_theta_min 2.32 _cell_measurement_theta_max 27.47 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.449 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1352 _exptl_absorpt_coefficient_mu 0.786 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.759 _exptl_absorpt_correction_T_max 0.961 _exptl_absorpt_process_details 'SADABS V2.05' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 9750 _diffrn_reflns_av_R_equivalents 0.1106 _diffrn_reflns_av_sigmaI/netI 0.2131 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.32 _diffrn_reflns_theta_max 27.47 _reflns_number_total 5548 _reflns_number_gt 3085 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0416P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881, based on 1944 Friedel pairs' _refine_ls_abs_structure_Flack -0.03(6) _refine_ls_number_reflns 5548 _refine_ls_number_parameters 362 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1599 _refine_ls_R_factor_gt 0.0671 _refine_ls_wR_factor_ref 0.1355 _refine_ls_wR_factor_gt 0.1069 _refine_ls_goodness_of_fit_ref 0.959 _refine_ls_restrained_S_all 0.959 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.48607(4) -0.01530(9) 0.09500(4) 0.0220(2) Uani 1 1 d . . . P1 P 0.55212(15) 0.0220(3) 0.21760(15) 0.0242(8) Uani 1 1 d . . . O1 O 0.6200(3) -0.0761(6) 0.2696(4) 0.0230(17) Uani 1 1 d . . . O2 O 0.5958(4) 0.1597(6) 0.2312(4) 0.0231(16) Uani 1 1 d . . . O3 O 0.4960(3) 0.0214(6) 0.2726(3) 0.026(2) Uani 1 1 d . . . Cl1 Cl 0.40370(13) -0.0385(4) -0.04182(14) 0.0356(10) Uani 1 1 d . . . C1 C 0.6933(6) -0.0705(9) 0.2521(6) 0.018(2) Uani 1 1 d . . . C2 C 0.7088(6) -0.1747(10) 0.2103(6) 0.028(3) Uani 1 1 d . . . H2 H 0.6724 -0.2452 0.1956 0.034 Uiso 1 1 calc R . . C3 C 0.7777(7) -0.1749(10) 0.1904(6) 0.034(3) Uani 1 1 d . . . H3 H 0.7894 -0.2455 0.1610 0.040 Uiso 1 1 calc R . . C4 C 0.8327(6) -0.0668(10) 0.2143(6) 0.029(3) Uani 1 1 d . . . C5 C 0.9052(6) -0.0631(12) 0.1929(7) 0.041(3) Uani 1 1 d . . . H5 H 0.9198 -0.1340 0.1657 0.050 Uiso 1 1 calc R . . C6 C 0.9521(7) 0.0444(13) 0.2125(7) 0.045(3) Uani 1 1 d . . . H6 H 1.0009 0.0450 0.2005 0.054 Uiso 1 1 calc R . . C7 C 0.9325(6) 0.1527(12) 0.2490(6) 0.038(3) Uani 1 1 d . . . H7 H 0.9655 0.2277 0.2586 0.046 Uiso 1 1 calc R . . C8 C 0.8637(6) 0.1502(12) 0.2713(6) 0.033(3) Uani 1 1 d . . . H8 H 0.8492 0.2235 0.2965 0.040 Uiso 1 1 calc R . . C9 C 0.8153(6) 0.0366(11) 0.2560(6) 0.027(3) Uani 1 1 d . . . C10 C 0.7429(6) 0.0316(10) 0.2813(6) 0.023(3) Uani 1 1 d . . . C11 C 0.7214(6) 0.1333(10) 0.3314(6) 0.023(2) Uani 1 1 d . . . C12 C 0.7743(6) 0.1636(10) 0.4104(6) 0.023(2) Uani 1 1 d . . . C13 C 0.8501(5) 0.1013(10) 0.4466(6) 0.029(3) Uani 1 1 d . . . H13 H 0.8675 0.0353 0.4180 0.035 Uiso 1 1 calc R . . C14 C 0.8973(6) 0.1362(12) 0.5215(6) 0.035(3) Uani 1 1 d . . . H14 H 0.9461 0.0915 0.5448 0.041 Uiso 1 1 calc R . . C15 C 0.8756(7) 0.2362(13) 0.5650(6) 0.046(4) Uani 1 1 d . . . H15 H 0.9107 0.2622 0.6157 0.055 Uiso 1 1 calc R . . C16 C 0.8019(7) 0.2973(12) 0.5327(6) 0.042(3) Uani 1 1 d . . . H16 H 0.7859 0.3633 0.5623 0.050 Uiso 1 1 calc R . . C17 C 0.7509(7) 0.2609(10) 0.4558(6) 0.030(3) Uani 1 1 d . . . C18 C 0.6759(6) 0.3205(11) 0.4235(6) 0.033(3) Uani 1 1 d . . . H18 H 0.6605 0.3865 0.4535 0.039 Uiso 1 1 calc R . . C19 C 0.6250(6) 0.2866(9) 0.3506(6) 0.027(3) Uani 1 1 d . . . H19 H 0.5744 0.3270 0.3302 0.032 Uiso 1 1 calc R . . C20 C 0.6493(6) 0.1895(9) 0.3059(6) 0.022(2) Uani 1 1 d . . . C21 C 0.3972(4) -0.0070(16) 0.1444(5) 0.023(2) Uani 1 1 d . . . C22 C 0.3183(4) -0.0240(15) 0.0974(5) 0.028(2) Uani 1 1 d . . . H22 H 0.3056 -0.0338 0.0408 0.033 Uiso 1 1 calc R . . C23 C 0.2574(4) -0.0267(13) 0.1332(5) 0.0216(17) Uani 1 1 d . . . C24 C 0.2774(5) -0.0022(13) 0.2144(5) 0.025(2) Uani 1 1 d . . . H24 H 0.2358 -0.0010 0.2380 0.030 Uiso 1 1 calc R . . C25 C 0.3571(5) 0.0218(9) 0.2656(5) 0.024(3) Uani 1 1 d . . . C26 C 0.4130(5) 0.0116(9) 0.2241(5) 0.0216(17) Uani 1 1 d . . . C27 C 0.1713(5) -0.0487(11) 0.0770(6) 0.031(3) Uani 1 1 d . . . C28 C 0.1473(7) 0.0587(12) 0.0139(7) 0.046(4) Uani 1 1 d . . . H28A H 0.1822 0.0565 -0.0198 0.068 Uiso 1 1 calc R . . H28B H 0.1521 0.1433 0.0408 0.068 Uiso 1 1 calc R . . H28C H 0.0920 0.0454 -0.0196 0.068 Uiso 1 1 calc R . . C29 C 0.1661(7) -0.1808(13) 0.0377(8) 0.052(4) Uani 1 1 d . . . H29A H 0.1102 -0.2019 0.0100 0.079 Uiso 1 1 calc R . . H29B H 0.1890 -0.2466 0.0789 0.079 Uiso 1 1 calc R . . H29C H 0.1957 -0.1795 -0.0012 0.079 Uiso 1 1 calc R . . C30 C 0.1123(5) -0.0461(14) 0.1270(6) 0.047(4) Uani 1 1 d . . . H30A H 0.0576 -0.0402 0.0906 0.070 Uiso 1 1 calc R . . H30B H 0.1238 0.0294 0.1629 0.070 Uiso 1 1 calc R . . H30C H 0.1184 -0.1258 0.1589 0.070 Uiso 1 1 calc R . . C31 C 0.3765(6) 0.0528(10) 0.3548(6) 0.030(3) Uani 1 1 d . . . C32 C 0.4231(6) 0.1810(11) 0.3780(7) 0.038(3) Uani 1 1 d . . . H32A H 0.4350 0.1962 0.4357 0.058 Uiso 1 1 calc R . . H32B H 0.3909 0.2530 0.3481 0.058 Uiso 1 1 calc R . . H32C H 0.4729 0.1754 0.3648 0.058 Uiso 1 1 calc R . . C33 C 0.4210(6) -0.0562(10) 0.4052(6) 0.031(3) Uani 1 1 d . . . H33A H 0.4286 -0.0377 0.4619 0.046 Uiso 1 1 calc R . . H33B H 0.4730 -0.0657 0.3968 0.046 Uiso 1 1 calc R . . H33C H 0.3907 -0.1370 0.3898 0.046 Uiso 1 1 calc R . . C34 C 0.2986(6) 0.0727(11) 0.3767(6) 0.039(3) Uani 1 1 d . . . H34A H 0.2660 -0.0061 0.3635 0.059 Uiso 1 1 calc R . . H34B H 0.2688 0.1463 0.3462 0.059 Uiso 1 1 calc R . . H34C H 0.3119 0.0906 0.4343 0.059 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.0114(3) 0.0379(4) 0.0187(3) 0.0005(5) 0.0080(3) -0.0013(6) P1 0.0158(13) 0.037(2) 0.0203(14) 0.0009(12) 0.0063(11) -0.0006(12) O1 0.013(3) 0.036(4) 0.018(4) 0.007(3) 0.002(3) 0.000(3) O2 0.016(4) 0.033(4) 0.015(4) 0.003(3) -0.003(3) -0.001(3) O3 0.011(3) 0.051(6) 0.014(3) -0.003(3) 0.001(3) -0.009(3) Cl1 0.0131(11) 0.076(3) 0.0196(12) -0.0098(17) 0.0075(9) -0.0114(17) C1 0.021(5) 0.022(6) 0.017(5) 0.008(4) 0.013(4) 0.009(5) C2 0.028(6) 0.026(7) 0.031(7) -0.006(5) 0.010(5) 0.009(5) C3 0.043(7) 0.020(7) 0.035(7) -0.007(5) 0.008(6) 0.012(6) C4 0.016(5) 0.049(8) 0.016(6) 0.004(5) -0.002(5) 0.001(5) C5 0.022(6) 0.053(9) 0.053(8) 0.002(6) 0.018(6) 0.016(6) C6 0.027(7) 0.071(10) 0.044(8) -0.006(6) 0.020(6) -0.009(7) C7 0.023(6) 0.057(9) 0.034(7) 0.008(6) 0.007(5) -0.001(6) C8 0.017(6) 0.052(8) 0.034(7) 0.007(6) 0.013(5) 0.008(6) C9 0.018(5) 0.057(8) 0.011(5) -0.002(5) 0.011(4) 0.004(5) C10 0.017(5) 0.026(7) 0.023(6) 0.002(4) 0.003(5) 0.003(5) C11 0.022(6) 0.028(6) 0.023(6) 0.002(5) 0.014(5) -0.007(5) C12 0.016(5) 0.036(7) 0.023(6) 0.004(5) 0.015(5) -0.003(5) C13 0.015(6) 0.046(8) 0.031(7) 0.013(5) 0.014(5) 0.001(5) C14 0.015(6) 0.056(8) 0.027(7) 0.010(6) -0.002(5) -0.003(6) C15 0.042(8) 0.072(10) 0.014(6) 0.002(6) -0.005(6) -0.022(7) C16 0.050(8) 0.062(9) 0.022(7) -0.001(6) 0.023(6) -0.023(7) C17 0.032(6) 0.031(7) 0.033(7) -0.001(5) 0.020(5) -0.006(5) C18 0.035(7) 0.032(7) 0.037(7) -0.006(5) 0.020(6) -0.002(6) C19 0.018(6) 0.028(7) 0.040(7) 0.004(5) 0.018(5) 0.007(5) C20 0.024(6) 0.018(6) 0.024(6) 0.002(5) 0.008(5) 0.001(5) C21 0.010(4) 0.041(7) 0.021(5) 0.007(8) 0.010(3) -0.006(8) C22 0.011(4) 0.050(7) 0.026(5) 0.004(8) 0.010(3) 0.007(8) C23 0.018(3) 0.022(5) 0.021(3) -0.001(4) 0.001(3) 0.001(4) C24 0.017(4) 0.030(7) 0.032(5) -0.013(7) 0.013(4) -0.009(6) C25 0.020(5) 0.031(8) 0.020(5) 0.002(4) 0.006(4) 0.005(4) C26 0.018(3) 0.022(5) 0.021(3) -0.001(4) 0.001(3) 0.001(4) C27 0.013(5) 0.051(11) 0.031(6) -0.002(6) 0.010(4) -0.004(5) C28 0.021(7) 0.074(10) 0.040(8) 0.006(7) 0.007(6) 0.006(6) C29 0.023(7) 0.066(10) 0.070(10) -0.033(8) 0.017(7) -0.004(7) C30 0.014(5) 0.097(13) 0.034(6) -0.014(7) 0.016(4) -0.010(7) C31 0.041(7) 0.045(7) 0.006(5) 0.009(5) 0.009(5) 0.007(6) C32 0.034(7) 0.038(8) 0.049(8) -0.007(6) 0.021(6) -0.005(6) C33 0.021(5) 0.036(8) 0.037(6) 0.006(5) 0.012(5) 0.000(5) C34 0.041(7) 0.056(8) 0.032(7) -0.005(6) 0.027(6) 0.001(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 Pd1 C21 2.019(8) . ? Pd1 P1 2.135(3) . ? Pd1 Cl1 2.397(2) . ? Pd1 Cl1 2.422(2) 2_655 ? P1 O3 1.585(7) . ? P1 O2 1.595(7) . ? P1 O1 1.614(6) . ? O1 C1 1.425(11) . ? O2 C20 1.390(10) . ? O3 C26 1.453(9) . ? Cl1 Pd1 2.422(2) 2_655 ? C1 C10 1.362(12) . ? C1 C2 1.373(13) . ? C2 C3 1.369(15) . ? C2 H2 0.9500 . ? C3 C4 1.452(14) . ? C3 H3 0.9500 . ? C4 C9 1.379(13) . ? C4 C5 1.445(14) . ? C5 C6 1.361(14) . ? C5 H5 0.9500 . ? C6 C7 1.382(16) . ? C6 H6 0.9500 . ? C7 C8 1.390(14) . ? C7 H7 0.9500 . ? C8 C9 1.424(14) . ? C8 H8 0.9500 . ? C9 C10 1.482(14) . ? C10 C11 1.491(14) . ? C11 C20 1.343(13) . ? C11 C12 1.441(12) . ? C12 C17 1.420(14) . ? C12 C13 1.443(13) . ? C13 C14 1.365(13) . ? C13 H13 0.9500 . ? C14 C15 1.403(16) . ? C14 H14 0.9500 . ? C15 C16 1.399(16) . ? C15 H15 0.9500 . ? C16 C17 1.417(14) . ? C16 H16 0.9500 . ? C17 C18 1.410(14) . ? C18 C19 1.357(13) . ? C18 H18 0.9500 . ? C19 C20 1.417(13) . ? C19 H19 0.9500 . ? C21 C26 1.349(11) . ? C21 C22 1.393(10) . ? C22 C23 1.408(10) . ? C22 H22 0.9500 . ? C23 C24 1.378(11) . ? C23 C27 1.550(11) . ? C24 C25 1.437(11) . ? C24 H24 0.9500 . ? C25 C26 1.403(13) . ? C25 C31 1.526(13) . ? C27 C29 1.513(15) . ? C27 C28 1.526(14) . ? C27 C30 1.560(12) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 C33 1.491(13) . ? C31 C32 1.542(14) . ? C31 C34 1.555(14) . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 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 C21 Pd1 P1 79.4(3) . . ? C21 Pd1 Cl1 97.0(2) . . ? P1 Pd1 Cl1 174.17(13) . . ? C21 Pd1 Cl1 175.9(4) . 2_655 ? P1 Pd1 Cl1 98.73(9) . 2_655 ? Cl1 Pd1 Cl1 85.18(8) . 2_655 ? O3 P1 O2 106.2(4) . . ? O3 P1 O1 98.7(3) . . ? O2 P1 O1 103.4(3) . . ? O3 P1 Pd1 111.2(2) . . ? O2 P1 Pd1 113.4(3) . . ? O1 P1 Pd1 122.2(3) . . ? C1 O1 P1 114.8(5) . . ? C20 O2 P1 119.5(6) . . ? C26 O3 P1 110.8(5) . . ? Pd1 Cl1 Pd1 93.69(8) . 2_655 ? C10 C1 C2 126.2(9) . . ? C10 C1 O1 118.2(8) . . ? C2 C1 O1 115.4(9) . . ? C3 C2 C1 118.6(10) . . ? C3 C2 H2 120.7 . . ? C1 C2 H2 120.7 . . ? C2 C3 C4 119.7(10) . . ? C2 C3 H3 120.1 . . ? C4 C3 H3 120.1 . . ? C9 C4 C5 118.8(10) . . ? C9 C4 C3 120.2(10) . . ? C5 C4 C3 121.0(10) . . ? C6 C5 C4 118.4(10) . . ? C6 C5 H5 120.8 . . ? C4 C5 H5 120.8 . . ? C5 C6 C7 123.4(11) . . ? C5 C6 H6 118.3 . . ? C7 C6 H6 118.3 . . ? C6 C7 C8 118.9(11) . . ? C6 C7 H7 120.5 . . ? C8 C7 H7 120.5 . . ? C7 C8 C9 119.4(11) . . ? C7 C8 H8 120.3 . . ? C9 C8 H8 120.3 . . ? C4 C9 C8 120.8(9) . . ? C4 C9 C10 119.3(10) . . ? C8 C9 C10 119.9(9) . . ? C1 C10 C9 115.4(9) . . ? C1 C10 C11 120.7(9) . . ? C9 C10 C11 123.8(9) . . ? C20 C11 C12 119.4(9) . . ? C20 C11 C10 119.8(9) . . ? C12 C11 C10 120.5(9) . . ? C17 C12 C11 118.4(9) . . ? C17 C12 C13 117.4(9) . . ? C11 C12 C13 124.2(10) . . ? C14 C13 C12 120.8(10) . . ? C14 C13 H13 119.6 . . ? C12 C13 H13 119.6 . . ? C13 C14 C15 121.7(10) . . ? C13 C14 H14 119.1 . . ? C15 C14 H14 119.1 . . ? C16 C15 C14 119.3(10) . . ? C16 C15 H15 120.4 . . ? C14 C15 H15 120.4 . . ? C15 C16 C17 120.1(11) . . ? C15 C16 H16 119.9 . . ? C17 C16 H16 119.9 . . ? C18 C17 C16 120.5(10) . . ? C18 C17 C12 118.9(10) . . ? C16 C17 C12 120.6(10) . . ? C19 C18 C17 122.1(10) . . ? C19 C18 H18 119.0 . . ? C17 C18 H18 119.0 . . ? C18 C19 C20 118.3(9) . . ? C18 C19 H19 120.8 . . ? C20 C19 H19 120.8 . . ? C11 C20 O2 121.0(9) . . ? C11 C20 C19 122.7(9) . . ? O2 C20 C19 116.2(8) . . ? C26 C21 C22 118.3(8) . . ? C26 C21 Pd1 120.9(6) . . ? C22 C21 Pd1 120.8(6) . . ? C21 C22 C23 120.3(7) . . ? C21 C22 H22 119.9 . . ? C23 C22 H22 119.9 . . ? C24 C23 C22 118.2(7) . . ? C24 C23 C27 124.6(7) . . ? C22 C23 C27 117.1(7) . . ? C23 C24 C25 124.1(8) . . ? C23 C24 H24 117.9 . . ? C25 C24 H24 117.9 . . ? C26 C25 C24 112.1(8) . . ? C26 C25 C31 125.4(8) . . ? C24 C25 C31 122.5(9) . . ? C21 C26 C25 126.7(8) . . ? C21 C26 O3 117.3(8) . . ? C25 C26 O3 116.0(7) . . ? C29 C27 C28 111.0(10) . . ? C29 C27 C23 109.2(9) . . ? C28 C27 C23 110.6(9) . . ? C29 C27 C30 108.3(10) . . ? C28 C27 C30 108.0(9) . . ? C23 C27 C30 109.7(8) . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C27 C30 H30A 109.5 . . ? C27 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C27 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C33 C31 C25 110.9(9) . . ? C33 C31 C32 110.4(8) . . ? C25 C31 C32 112.3(8) . . ? C33 C31 C34 107.3(9) . . ? C25 C31 C34 110.4(8) . . ? C32 C31 C34 105.3(9) . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C31 C33 H33A 109.5 . . ? C31 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C31 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C31 C34 H34A 109.5 . . ? C31 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C31 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 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 C21 Pd1 P1 O3 4.8(5) . . . . ? Cl1 Pd1 P1 O3 -171.5(3) 2_655 . . . ? C21 Pd1 P1 O2 -114.7(5) . . . . ? Cl1 Pd1 P1 O2 69.0(3) 2_655 . . . ? C21 Pd1 P1 O1 120.6(5) . . . . ? Cl1 Pd1 P1 O1 -55.7(3) 2_655 . . . ? O3 P1 O1 C1 -162.0(6) . . . . ? O2 P1 O1 C1 -53.0(7) . . . . ? Pd1 P1 O1 C1 76.1(6) . . . . ? O3 P1 O2 C20 66.2(7) . . . . ? O1 P1 O2 C20 -37.2(7) . . . . ? Pd1 P1 O2 C20 -171.5(6) . . . . ? O2 P1 O3 C26 116.7(6) . . . . ? O1 P1 O3 C26 -136.6(6) . . . . ? Pd1 P1 O3 C26 -7.0(6) . . . . ? C21 Pd1 Cl1 Pd1 172.2(5) . . . 2_655 ? Cl1 Pd1 Cl1 Pd1 -11.3(2) 2_655 . . 2_655 ? P1 O1 C1 C10 76.2(9) . . . . ? P1 O1 C1 C2 -107.3(8) . . . . ? C10 C1 C2 C3 -4.8(16) . . . . ? O1 C1 C2 C3 179.0(8) . . . . ? C1 C2 C3 C4 0.7(15) . . . . ? C2 C3 C4 C9 -0.9(15) . . . . ? C2 C3 C4 C5 -178.9(10) . . . . ? C9 C4 C5 C6 -2.1(15) . . . . ? C3 C4 C5 C6 175.9(10) . . . . ? C4 C5 C6 C7 -2.8(18) . . . . ? C5 C6 C7 C8 3.9(18) . . . . ? C6 C7 C8 C9 -0.1(16) . . . . ? C5 C4 C9 C8 5.7(15) . . . . ? C3 C4 C9 C8 -172.3(9) . . . . ? C5 C4 C9 C10 -177.4(9) . . . . ? C3 C4 C9 C10 4.6(14) . . . . ? C7 C8 C9 C4 -4.6(15) . . . . ? C7 C8 C9 C10 178.5(9) . . . . ? C2 C1 C10 C9 8.2(14) . . . . ? O1 C1 C10 C9 -175.7(8) . . . . ? C2 C1 C10 C11 -175.1(10) . . . . ? O1 C1 C10 C11 1.0(13) . . . . ? C4 C9 C10 C1 -7.9(13) . . . . ? C8 C9 C10 C1 169.0(9) . . . . ? C4 C9 C10 C11 175.5(9) . . . . ? C8 C9 C10 C11 -7.5(14) . . . . ? C1 C10 C11 C20 -50.0(14) . . . . ? C9 C10 C11 C20 126.4(10) . . . . ? C1 C10 C11 C12 124.3(10) . . . . ? C9 C10 C11 C12 -59.3(13) . . . . ? C20 C11 C12 C17 -5.4(14) . . . . ? C10 C11 C12 C17 -179.8(9) . . . . ? C20 C11 C12 C13 174.7(9) . . . . ? C10 C11 C12 C13 0.3(15) . . . . ? C17 C12 C13 C14 -0.5(14) . . . . ? C11 C12 C13 C14 179.4(9) . . . . ? C12 C13 C14 C15 -2.3(16) . . . . ? C13 C14 C15 C16 3.5(17) . . . . ? C14 C15 C16 C17 -1.9(17) . . . . ? C15 C16 C17 C18 179.0(10) . . . . ? C15 C16 C17 C12 -0.8(16) . . . . ? C11 C12 C17 C18 2.3(14) . . . . ? C13 C12 C17 C18 -177.8(9) . . . . ? C11 C12 C17 C16 -177.9(9) . . . . ? C13 C12 C17 C16 2.0(15) . . . . ? C16 C17 C18 C19 -178.9(10) . . . . ? C12 C17 C18 C19 0.8(16) . . . . ? C17 C18 C19 C20 -1.0(16) . . . . ? C12 C11 C20 O2 -178.0(8) . . . . ? C10 C11 C20 O2 -3.6(14) . . . . ? C12 C11 C20 C19 5.5(15) . . . . ? C10 C11 C20 C19 179.9(9) . . . . ? P1 O2 C20 C11 72.7(11) . . . . ? P1 O2 C20 C19 -110.6(8) . . . . ? C18 C19 C20 C11 -2.3(16) . . . . ? C18 C19 C20 O2 -178.9(9) . . . . ? P1 Pd1 C21 C26 -2.0(11) . . . . ? Cl1 Pd1 C21 C26 -177.4(11) . . . . ? P1 Pd1 C21 C22 179.8(14) . . . . ? Cl1 Pd1 C21 C22 4.4(14) . . . . ? C26 C21 C22 C23 -2(2) . . . . ? Pd1 C21 C22 C23 175.7(12) . . . . ? C21 C22 C23 C24 5(2) . . . . ? C21 C22 C23 C27 -178.8(13) . . . . ? C22 C23 C24 C25 -2(2) . . . . ? C27 C23 C24 C25 -178.1(11) . . . . ? C23 C24 C25 C26 -2.6(17) . . . . ? C23 C24 C25 C31 178.0(11) . . . . ? C22 C21 C26 C25 -3(2) . . . . ? Pd1 C21 C26 C25 178.7(8) . . . . ? C22 C21 C26 O3 176.4(12) . . . . ? Pd1 C21 C26 O3 -1.8(16) . . . . ? C24 C25 C26 C21 5.5(16) . . . . ? C31 C25 C26 C21 -175.2(12) . . . . ? C24 C25 C26 O3 -174.1(9) . . . . ? C31 C25 C26 O3 5.2(14) . . . . ? P1 O3 C26 C21 5.8(12) . . . . ? P1 O3 C26 C25 -174.5(7) . . . . ? C24 C23 C27 C29 -121.6(14) . . . . ? C22 C23 C27 C29 62.5(16) . . . . ? C24 C23 C27 C28 116.1(14) . . . . ? C22 C23 C27 C28 -59.9(15) . . . . ? C24 C23 C27 C30 -3.0(18) . . . . ? C22 C23 C27 C30 -178.9(12) . . . . ? C26 C25 C31 C33 -68.2(12) . . . . ? C24 C25 C31 C33 111.0(11) . . . . ? C26 C25 C31 C32 55.8(13) . . . . ? C24 C25 C31 C32 -125.0(11) . . . . ? C26 C25 C31 C34 173.0(9) . . . . ? C24 C25 C31 C34 -7.8(14) . . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.871 _refine_diff_density_min -1.269 _refine_diff_density_rms 0.153