Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2003 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 loop_ _publ_author_name 'Fung-E Hong' 'Chin-Pei Chang' 'Yu-Chang Chang' _publ_contact_author_name 'Prof Fung-E Hong' _publ_contact_author_address ; Department of Chemistry National Chung-Hsing University Taichung 40227 TAIWAN ; _publ_contact_author_email FEHONG@DRAGON.NCHU.EDU.TW _publ_section_title ; Synthesis and Structural Characterization of Novel Palladium Complexes Chelated by Bulky Cobalt-Containing Phosphine Ligands: Unusual Palladium-Cobalt Bond Formations ; data_hong135m _database_code_CSD 209741 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C63 H49 Co4 O11 P5' _chemical_formula_weight 1372.59 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' Co Co 0.3494 0.9721 '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 13.7890(19) _cell_length_b 13.8536(19) _cell_length_c 18.622(2) _cell_angle_alpha 86.151(3) _cell_angle_beta 85.941(3) _cell_angle_gamma 61.916(2) _cell_volume 3128.3(7) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.80 _exptl_crystal_size_mid 0.60 _exptl_crystal_size_min 0.60 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.457 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1396 _exptl_absorpt_coefficient_mu 1.228 _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 293(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_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17491 _diffrn_reflns_av_R_equivalents 0.0389 _diffrn_reflns_av_sigmaI/netI 0.0639 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.96 _diffrn_reflns_theta_max 26.03 _reflns_number_total 12039 _reflns_number_gt 7388 _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^)+(0.1180P)^2^+10.3711P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12039 _refine_ls_number_parameters 748 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1232 _refine_ls_R_factor_gt 0.0662 _refine_ls_wR_factor_ref 0.2255 _refine_ls_wR_factor_gt 0.1697 _refine_ls_goodness_of_fit_ref 0.959 _refine_ls_restrained_S_all 0.959 _refine_ls_shift/su_max 0.062 _refine_ls_shift/su_mean 0.007 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 Co1 Co 0.19289(7) 0.47011(8) 0.26998(5) 0.0429(2) Uani 1 1 d . . . Co2 Co 0.08243(7) 0.42087(8) 0.19205(5) 0.0496(3) Uani 1 1 d . . . Co3 Co 0.49737(8) 0.17304(7) 0.26784(5) 0.0476(3) Uani 1 1 d . . . Co4 Co 0.50959(7) 0.29677(7) 0.16719(4) 0.0415(2) Uani 1 1 d . . . P1 P 0.32659(16) 0.18864(15) 0.26245(10) 0.0508(5) Uani 1 1 d . . . P2 P 0.34453(13) 0.38401(13) 0.11873(8) 0.0376(4) Uani 1 1 d . . . P3 P 0.35365(13) 0.44070(14) 0.31076(9) 0.0402(4) Uani 1 1 d . . . P4 P 0.71067(14) 0.24921(17) 0.26892(11) 0.0531(5) Uani 1 1 d . . . P5 P -0.06537(18) 0.4792(2) 0.26224(13) 0.0750(7) Uani 1 1 d . . . O1 O 0.0846(6) 0.5067(8) 0.4145(3) 0.116(3) Uani 1 1 d . . . O2 O 0.0977(5) 0.6947(5) 0.2093(4) 0.090(2) Uani 1 1 d . . . O3 O 0.0446(6) 0.2576(7) 0.1261(5) 0.123(3) Uani 1 1 d . . . O4 O -0.0175(6) 0.5971(9) 0.0824(5) 0.149(4) Uani 1 1 d . . . O5 O 0.5582(8) 0.0761(7) 0.4121(4) 0.121(3) Uani 1 1 d . . . O6 O 0.6255(7) -0.0451(6) 0.2105(5) 0.124(3) Uani 1 1 d . . . O7 O 0.6024(5) 0.4339(6) 0.0991(3) 0.0825(18) Uani 1 1 d . . . O8 O 0.6338(6) 0.1141(6) 0.0720(4) 0.100(2) Uani 1 1 d . . . O9 O -0.1012(8) 0.5898(12) 0.2971(8) 0.180(6) Uani 1 1 d . . . O10 O -0.0588(6) 0.4036(8) 0.3306(4) 0.133(3) Uani 1 1 d . . . O11 O -0.1799(6) 0.5134(11) 0.2288(5) 0.159(5) Uani 1 1 d . . . C1 C 0.1247(6) 0.4899(8) 0.3589(4) 0.067(2) Uani 1 1 d . . . C2 C 0.1380(6) 0.6090(7) 0.2333(4) 0.0584(19) Uani 1 1 d . . . C3 C 0.0631(7) 0.3180(8) 0.1535(6) 0.079(3) Uani 1 1 d . . . C4 C 0.0234(6) 0.5294(9) 0.1260(5) 0.081(3) Uani 1 1 d . . . C5 C 0.5301(8) 0.1183(7) 0.3572(5) 0.074(2) Uani 1 1 d . . . C6 C 0.5764(8) 0.0418(7) 0.2300(5) 0.080(3) Uani 1 1 d . . . C7 C 0.5667(6) 0.3805(6) 0.1265(4) 0.0527(17) Uani 1 1 d . . . C8 C 0.5859(6) 0.1847(7) 0.1090(4) 0.067(2) Uani 1 1 d . . . C9 C 0.2282(5) 0.3254(5) 0.2371(3) 0.0427(14) Uani 1 1 d . . . C10 C 0.2372(5) 0.3898(5) 0.1807(3) 0.0382(13) Uani 1 1 d . . . C11 C 0.4662(5) 0.3278(5) 0.2689(3) 0.0383(13) Uani 1 1 d . . . C12 C 0.5769(5) 0.2593(5) 0.2616(3) 0.0428(14) Uani 1 1 d . . . C13 C -0.1699(19) 0.6886(16) 0.2953(13) 0.200(9) Uani 1 1 d . . . H13A H -0.1533 0.7257 0.3305 0.301 Uiso 1 1 calc R . . H13B H -0.2422 0.6960 0.3060 0.301 Uiso 1 1 calc R . . H13C H -0.1672 0.7202 0.2482 0.301 Uiso 1 1 calc R . . C14 C -0.1444(11) 0.4182(13) 0.3812(8) 0.151(6) Uani 1 1 d . . . H14A H -0.1178 0.3604 0.4176 0.227 Uiso 1 1 calc R . . H14B H -0.2034 0.4169 0.3575 0.227 Uiso 1 1 calc R . . H14C H -0.1708 0.4874 0.4031 0.227 Uiso 1 1 calc R . . C15 C -0.2001(8) 0.4759(11) 0.1670(6) 0.107(4) Uani 1 1 d . . . H15A H -0.2777 0.5121 0.1597 0.161 Uiso 1 1 calc R . . H15B H -0.1741 0.3983 0.1724 0.161 Uiso 1 1 calc R . . H15C H -0.1623 0.4914 0.1262 0.161 Uiso 1 1 calc R . . C16 C 0.2761(8) 0.1491(8) 0.3459(5) 0.071(2) Uani 1 1 d . . . C17 C 0.3422(9) 0.0459(9) 0.3762(5) 0.086(3) Uani 1 1 d . . . H17A H 0.4087 -0.0005 0.3532 0.104 Uiso 1 1 calc R . . C18 C 0.3093(13) 0.0119(13) 0.4407(8) 0.122(5) Uani 1 1 d . . . H18A H 0.3530 -0.0582 0.4598 0.146 Uiso 1 1 calc R . . C19 C 0.2157(14) 0.0781(14) 0.4759(7) 0.127(5) Uani 1 1 d . . . H19A H 0.1964 0.0545 0.5199 0.153 Uiso 1 1 calc R . . C20 C 0.1467(12) 0.1822(14) 0.4475(6) 0.124(5) Uani 1 1 d . . . H20A H 0.0811 0.2288 0.4715 0.149 Uiso 1 1 calc R . . C21 C 0.1805(10) 0.2139(10) 0.3809(5) 0.088(3) Uani 1 1 d . . . H21A H 0.1349 0.2823 0.3603 0.106 Uiso 1 1 calc R . . C22 C 0.3112(7) 0.1002(7) 0.1981(5) 0.066(2) Uani 1 1 d . . . C23 C 0.3732(7) 0.0766(7) 0.1344(5) 0.070(2) Uani 1 1 d . . . H23A H 0.4235 0.1034 0.1251 0.084 Uiso 1 1 calc R . . C24 C 0.3623(10) 0.0136(8) 0.0836(6) 0.090(3) Uani 1 1 d . . . H24A H 0.4056 -0.0030 0.0410 0.108 Uiso 1 1 calc R . . C25 C 0.2883(11) -0.0226(9) 0.0973(7) 0.100(4) Uani 1 1 d . . . H25A H 0.2792 -0.0625 0.0626 0.120 Uiso 1 1 calc R . . C26 C 0.2252(10) -0.0034(9) 0.1602(7) 0.098(4) Uani 1 1 d . . . H26A H 0.1761 -0.0319 0.1683 0.117 Uiso 1 1 calc R . . C27 C 0.2359(9) 0.0609(8) 0.2131(6) 0.089(3) Uani 1 1 d . . . H27A H 0.1937 0.0759 0.2561 0.107 Uiso 1 1 calc R . . C28 C 0.3423(6) 0.3246(6) 0.0340(4) 0.0485(16) Uani 1 1 d . . . C29 C 0.4197(7) 0.3189(7) -0.0203(4) 0.063(2) Uani 1 1 d . . . H29A H 0.4669 0.3477 -0.0129 0.075 Uiso 1 1 calc R . . C30 C 0.4274(9) 0.2729(9) -0.0828(5) 0.090(3) Uani 1 1 d . . . H30A H 0.4806 0.2692 -0.1178 0.108 Uiso 1 1 calc R . . C31 C 0.3589(10) 0.2315(9) -0.0959(5) 0.093(3) Uani 1 1 d . . . H31A H 0.3656 0.1998 -0.1397 0.111 Uiso 1 1 calc R . . C32 C 0.2795(10) 0.2360(8) -0.0451(6) 0.090(3) Uani 1 1 d . . . H32A H 0.2318 0.2088 -0.0546 0.108 Uiso 1 1 calc R . . C33 C 0.2714(7) 0.2829(7) 0.0225(5) 0.069(2) Uani 1 1 d . . . H33A H 0.2195 0.2853 0.0581 0.083 Uiso 1 1 calc R . . C34 C 0.2952(5) 0.5263(5) 0.0875(3) 0.0417(14) Uani 1 1 d . . . C35 C 0.2155(5) 0.5731(6) 0.0348(4) 0.0485(16) Uani 1 1 d . . . H35A H 0.1901 0.5303 0.0143 0.058 Uiso 1 1 calc R . . C36 C 0.1751(6) 0.6818(6) 0.0133(4) 0.0585(19) Uani 1 1 d . . . H36A H 0.1204 0.7128 -0.0201 0.070 Uiso 1 1 calc R . . C37 C 0.2150(6) 0.7444(6) 0.0410(4) 0.062(2) Uani 1 1 d . . . H37A H 0.1891 0.8172 0.0253 0.075 Uiso 1 1 calc R . . C38 C 0.2926(6) 0.7005(7) 0.0915(4) 0.0619(19) Uani 1 1 d . . . H38A H 0.3190 0.7436 0.1104 0.074 Uiso 1 1 calc R . . C39 C 0.3319(6) 0.5933(6) 0.1147(4) 0.0484(16) Uani 1 1 d . . . H39A H 0.3845 0.5649 0.1495 0.058 Uiso 1 1 calc R . . C40 C 0.3668(5) 0.4099(6) 0.4089(3) 0.0484(16) Uani 1 1 d . . . C41 C 0.3912(7) 0.4672(7) 0.4553(4) 0.064(2) Uani 1 1 d . . . H41A H 0.4013 0.5265 0.4379 0.077 Uiso 1 1 calc R . . C42 C 0.4008(8) 0.4372(10) 0.5278(4) 0.081(3) Uani 1 1 d . . . H42A H 0.4164 0.4775 0.5588 0.097 Uiso 1 1 calc R . . C43 C 0.3879(8) 0.3502(10) 0.5547(4) 0.087(3) Uani 1 1 d . . . H43A H 0.3971 0.3293 0.6033 0.105 Uiso 1 1 calc R . . C44 C 0.3611(9) 0.2935(9) 0.5091(4) 0.083(3) Uani 1 1 d . . . H44A H 0.3510 0.2343 0.5269 0.099 Uiso 1 1 calc R . . C45 C 0.3491(7) 0.3245(7) 0.4366(4) 0.068(2) Uani 1 1 d . . . H45A H 0.3287 0.2872 0.4062 0.082 Uiso 1 1 calc R . . C46 C 0.3863(6) 0.5549(5) 0.3001(4) 0.0473(15) Uani 1 1 d . . . C47 C 0.4909(6) 0.5416(6) 0.2795(4) 0.0494(16) Uani 1 1 d . . . H47A H 0.5487 0.4719 0.2719 0.059 Uiso 1 1 calc R . . C48 C 0.5085(7) 0.6313(7) 0.2705(4) 0.062(2) Uani 1 1 d . . . H48A H 0.5785 0.6212 0.2561 0.075 Uiso 1 1 calc R . . C49 C 0.4273(9) 0.7339(8) 0.2818(5) 0.073(2) Uani 1 1 d . . . H49A H 0.4416 0.7931 0.2752 0.088 Uiso 1 1 calc R . . C50 C 0.3244(8) 0.7500(7) 0.3030(5) 0.075(2) Uani 1 1 d . . . H50A H 0.2681 0.8204 0.3106 0.090 Uiso 1 1 calc R . . C51 C 0.3032(7) 0.6611(6) 0.3133(4) 0.062(2) Uani 1 1 d . . . H51A H 0.2333 0.6724 0.3291 0.075 Uiso 1 1 calc R . . C52 C 0.8017(6) 0.1269(7) 0.2208(4) 0.0579(18) Uani 1 1 d . . . C53 C 0.8184(7) 0.0231(8) 0.2434(6) 0.090(3) Uani 1 1 d . . . H53A H 0.7826 0.0140 0.2855 0.108 Uiso 1 1 calc R . . C54 C 0.8871(10) -0.0663(10) 0.2044(8) 0.116(4) Uani 1 1 d . . . H54A H 0.8983 -0.1356 0.2207 0.139 Uiso 1 1 calc R . . C55 C 0.9391(10) -0.0551(10) 0.1423(8) 0.117(4) Uani 1 1 d . . . H55A H 0.9856 -0.1162 0.1162 0.141 Uiso 1 1 calc R . . C56 C 0.9223(9) 0.0482(12) 0.1180(6) 0.112(4) Uani 1 1 d . . . H56A H 0.9569 0.0567 0.0751 0.135 Uiso 1 1 calc R . . C57 C 0.8540(7) 0.1389(8) 0.1577(5) 0.082(3) Uani 1 1 d . . . H57A H 0.8435 0.2081 0.1416 0.098 Uiso 1 1 calc R . . C58 C 0.7507(6) 0.2074(6) 0.3629(4) 0.0568(18) Uani 1 1 d . . . C59 C 0.8613(7) 0.1482(9) 0.3771(5) 0.086(3) Uani 1 1 d . . . H59A H 0.9136 0.1197 0.3395 0.103 Uiso 1 1 calc R . . C60 C 0.8941(9) 0.1314(11) 0.4482(7) 0.103(4) Uani 1 1 d . . . H60A H 0.9683 0.0913 0.4577 0.124 Uiso 1 1 calc R . . C61 C 0.8190(10) 0.1728(10) 0.5030(6) 0.097(3) Uani 1 1 d . . . H61A H 0.8419 0.1615 0.5500 0.117 Uiso 1 1 calc R . . C62 C 0.7096(9) 0.2311(8) 0.4902(5) 0.083(3) Uani 1 1 d . . . H62A H 0.6581 0.2594 0.5283 0.100 Uiso 1 1 calc R . . C63 C 0.6756(7) 0.2479(7) 0.4194(4) 0.065(2) Uani 1 1 d . . . H63A H 0.6010 0.2872 0.4106 0.079 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 Co1 0.0365(4) 0.0518(5) 0.0410(5) -0.0043(4) 0.0005(3) -0.0212(4) Co2 0.0387(5) 0.0623(6) 0.0524(5) 0.0047(4) -0.0077(4) -0.0276(5) Co3 0.0516(5) 0.0395(5) 0.0539(5) 0.0037(4) -0.0197(4) -0.0214(4) Co4 0.0367(4) 0.0438(5) 0.0394(5) -0.0062(4) -0.0040(3) -0.0141(4) P1 0.0599(11) 0.0481(10) 0.0549(11) 0.0100(8) -0.0211(9) -0.0331(9) P2 0.0376(8) 0.0399(9) 0.0340(8) -0.0029(6) -0.0041(6) -0.0166(7) P3 0.0405(8) 0.0459(9) 0.0374(8) -0.0067(7) -0.0017(6) -0.0222(8) P4 0.0389(9) 0.0578(12) 0.0591(11) 0.0034(9) -0.0132(8) -0.0190(9) P5 0.0466(11) 0.106(2) 0.0694(14) -0.0064(13) 0.0001(10) -0.0328(12) O1 0.088(5) 0.209(9) 0.050(4) -0.028(5) 0.023(3) -0.069(6) O2 0.073(4) 0.046(4) 0.115(5) 0.004(3) 0.002(4) -0.001(3) O3 0.091(5) 0.127(7) 0.169(8) -0.047(6) -0.030(5) -0.058(5) O4 0.065(4) 0.203(10) 0.158(8) 0.120(8) -0.044(5) -0.055(5) O5 0.178(8) 0.119(6) 0.102(6) 0.053(5) -0.088(6) -0.094(6) O6 0.114(6) 0.056(4) 0.176(8) -0.046(5) -0.035(6) -0.008(4) O7 0.077(4) 0.103(5) 0.081(4) 0.015(4) 0.005(3) -0.056(4) O8 0.096(5) 0.084(5) 0.086(5) -0.045(4) -0.002(4) -0.010(4) O9 0.076(6) 0.176(11) 0.237(13) -0.094(11) -0.008(7) -0.005(7) O10 0.088(5) 0.170(8) 0.104(6) 0.039(6) 0.027(4) -0.038(5) O11 0.067(5) 0.306(14) 0.120(7) -0.045(8) 0.013(4) -0.099(7) C1 0.054(4) 0.097(7) 0.056(5) -0.004(4) -0.004(4) -0.040(5) C2 0.037(4) 0.060(5) 0.067(5) -0.013(4) 0.009(3) -0.014(4) C3 0.058(5) 0.088(7) 0.097(7) -0.018(5) -0.014(5) -0.037(5) C4 0.037(4) 0.121(8) 0.079(6) 0.034(6) -0.014(4) -0.035(5) C5 0.097(7) 0.065(5) 0.075(6) 0.020(5) -0.042(5) -0.048(5) C6 0.072(6) 0.055(5) 0.101(7) -0.012(5) -0.037(5) -0.016(5) C7 0.047(4) 0.059(5) 0.050(4) -0.004(3) -0.002(3) -0.023(4) C8 0.054(4) 0.067(5) 0.062(5) -0.024(4) -0.008(4) -0.010(4) C9 0.043(3) 0.051(4) 0.039(3) 0.002(3) -0.011(3) -0.024(3) C10 0.038(3) 0.044(3) 0.033(3) 0.003(3) -0.009(2) -0.019(3) C11 0.044(3) 0.040(3) 0.036(3) 0.000(3) -0.008(3) -0.023(3) C12 0.046(4) 0.034(3) 0.048(4) 0.005(3) -0.018(3) -0.018(3) C13 0.20(2) 0.131(15) 0.29(3) -0.002(17) -0.05(2) -0.094(16) C14 0.125(11) 0.148(13) 0.154(13) 0.017(10) 0.070(10) -0.055(10) C15 0.065(6) 0.157(11) 0.099(8) -0.018(8) -0.011(5) -0.048(7) C16 0.089(6) 0.095(7) 0.064(5) 0.029(5) -0.029(5) -0.072(6) C17 0.109(7) 0.096(7) 0.088(7) 0.044(6) -0.043(6) -0.077(6) C18 0.149(12) 0.147(12) 0.117(10) 0.078(10) -0.063(9) -0.111(11) C19 0.153(13) 0.181(15) 0.086(8) 0.071(9) -0.022(8) -0.116(13) C20 0.125(10) 0.194(15) 0.088(8) 0.037(9) -0.001(7) -0.108(11) C21 0.108(8) 0.129(9) 0.067(6) 0.027(6) -0.011(5) -0.091(8) C22 0.075(5) 0.056(5) 0.082(6) 0.016(4) -0.038(5) -0.040(4) C23 0.077(6) 0.067(5) 0.069(5) -0.013(4) -0.011(4) -0.034(5) C24 0.116(8) 0.076(7) 0.089(7) -0.021(5) -0.011(6) -0.051(6) C25 0.148(11) 0.080(7) 0.090(8) 0.001(6) -0.036(7) -0.065(8) C26 0.135(10) 0.088(7) 0.113(9) 0.014(7) -0.045(8) -0.085(8) C27 0.117(8) 0.091(7) 0.092(7) 0.012(6) -0.040(6) -0.074(7) C28 0.049(4) 0.044(4) 0.045(4) -0.004(3) -0.011(3) -0.014(3) C29 0.069(5) 0.070(5) 0.046(4) -0.005(4) -0.004(4) -0.030(4) C30 0.093(7) 0.104(8) 0.051(5) -0.016(5) -0.003(5) -0.027(6) C31 0.117(9) 0.083(7) 0.056(6) -0.020(5) -0.011(6) -0.026(6) C32 0.114(8) 0.081(7) 0.088(7) -0.015(5) -0.034(6) -0.052(6) C33 0.082(6) 0.069(5) 0.071(5) -0.016(4) -0.009(4) -0.044(5) C34 0.041(3) 0.042(4) 0.037(3) -0.006(3) 0.006(3) -0.016(3) C35 0.044(4) 0.055(4) 0.044(4) 0.002(3) -0.004(3) -0.022(3) C36 0.061(4) 0.056(5) 0.049(4) 0.012(3) -0.006(3) -0.021(4) C37 0.062(5) 0.048(4) 0.074(5) 0.015(4) -0.004(4) -0.025(4) C38 0.063(5) 0.056(5) 0.071(5) 0.002(4) -0.002(4) -0.032(4) C39 0.050(4) 0.049(4) 0.046(4) -0.010(3) 0.000(3) -0.023(3) C40 0.044(4) 0.066(5) 0.040(3) -0.008(3) -0.001(3) -0.029(3) C41 0.076(5) 0.086(6) 0.050(4) -0.013(4) 0.002(4) -0.054(5) C42 0.087(6) 0.143(9) 0.035(4) -0.025(5) 0.009(4) -0.071(7) C43 0.090(7) 0.142(10) 0.037(4) 0.006(5) -0.006(4) -0.061(7) C44 0.114(8) 0.105(8) 0.049(5) 0.012(5) -0.011(5) -0.068(7) C45 0.094(6) 0.086(6) 0.046(4) 0.002(4) -0.012(4) -0.060(5) C46 0.052(4) 0.043(4) 0.048(4) -0.007(3) -0.009(3) -0.022(3) C47 0.052(4) 0.051(4) 0.046(4) -0.011(3) -0.002(3) -0.024(3) C48 0.082(6) 0.078(6) 0.054(4) -0.002(4) -0.002(4) -0.060(5) C49 0.102(7) 0.071(6) 0.069(5) -0.007(4) -0.005(5) -0.059(6) C50 0.094(7) 0.043(4) 0.081(6) -0.011(4) -0.005(5) -0.025(5) C51 0.070(5) 0.045(4) 0.068(5) -0.014(4) 0.004(4) -0.023(4) C52 0.043(4) 0.062(5) 0.058(4) 0.002(4) -0.003(3) -0.017(4) C53 0.053(5) 0.067(6) 0.118(8) 0.011(6) 0.022(5) -0.007(4) C54 0.090(8) 0.077(8) 0.151(12) 0.004(7) 0.027(8) -0.019(6) C55 0.091(8) 0.078(8) 0.133(11) -0.018(8) 0.017(8) 0.000(6) C56 0.084(7) 0.128(11) 0.078(7) -0.002(7) 0.025(6) -0.015(7) C57 0.066(5) 0.078(6) 0.074(6) 0.012(5) 0.002(5) -0.013(5) C58 0.052(4) 0.059(5) 0.062(5) 0.002(4) -0.020(4) -0.027(4) C59 0.054(5) 0.123(8) 0.073(6) 0.010(6) -0.020(4) -0.034(5) C60 0.074(7) 0.139(10) 0.098(8) 0.023(7) -0.044(6) -0.049(7) C61 0.101(8) 0.130(10) 0.080(7) 0.024(7) -0.047(6) -0.067(8) C62 0.105(8) 0.092(7) 0.066(6) -0.002(5) -0.019(5) -0.055(6) C63 0.060(5) 0.076(6) 0.067(5) -0.004(4) -0.014(4) -0.036(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 C2 1.807(9) . ? Co1 C1 1.816(8) . ? Co1 C9 1.957(7) . ? Co1 C10 1.960(6) . ? Co1 P3 2.2367(18) . ? Co1 Co2 2.5131(12) . ? Co2 C3 1.772(10) . ? Co2 C4 1.783(9) . ? Co2 C10 1.967(6) . ? Co2 C9 2.020(6) . ? Co2 P5 2.175(2) . ? Co3 C5 1.779(9) . ? Co3 C6 1.785(9) . ? Co3 C12 1.960(6) . ? Co3 C11 1.979(6) . ? Co3 P1 2.270(2) . ? Co3 Co4 2.5052(13) . ? Co4 C7 1.788(8) . ? Co4 C8 1.793(8) . ? Co4 C11 1.959(6) . ? Co4 C12 1.970(6) . ? Co4 P2 2.2382(17) . ? P1 C9 1.790(7) . ? P1 C16 1.815(9) . ? P1 C22 1.859(8) . ? P2 C10 1.785(6) . ? P2 C34 1.823(7) . ? P2 C28 1.836(7) . ? P3 C11 1.781(6) . ? P3 C46 1.834(7) . ? P3 C40 1.851(7) . ? P4 C12 1.797(6) . ? P4 C52 1.815(8) . ? P4 C58 1.845(8) . ? P5 O9 1.546(12) . ? P5 O10 1.574(8) . ? P5 O11 1.582(8) . ? O1 C1 1.124(9) . ? O2 C2 1.123(9) . ? O3 C3 1.141(11) . ? O4 C4 1.149(10) . ? O5 C5 1.140(10) . ? O6 C6 1.139(10) . ? O7 C7 1.143(9) . ? O8 C8 1.135(9) . ? O9 C13 1.244(19) . ? O10 C14 1.401(12) . ? O11 C15 1.390(13) . ? C9 C10 1.370(9) . ? C11 C12 1.368(9) . ? C16 C21 1.345(14) . ? C16 C17 1.390(13) . ? C17 C18 1.385(15) . ? C18 C19 1.33(2) . ? C19 C20 1.39(2) . ? C20 C21 1.408(13) . ? C22 C23 1.375(12) . ? C22 C27 1.386(12) . ? C23 C24 1.392(12) . ? C24 C25 1.336(15) . ? C25 C26 1.371(16) . ? C26 C27 1.433(13) . ? C28 C33 1.383(10) . ? C28 C29 1.395(10) . ? C29 C30 1.339(12) . ? C30 C31 1.357(15) . ? C31 C32 1.376(15) . ? C32 C33 1.428(12) . ? C34 C39 1.384(9) . ? C34 C35 1.411(9) . ? C35 C36 1.378(10) . ? C36 C37 1.368(11) . ? C37 C38 1.360(11) . ? C38 C39 1.370(10) . ? C40 C45 1.377(11) . ? C40 C41 1.368(10) . ? C41 C42 1.383(11) . ? C42 C43 1.358(14) . ? C43 C44 1.371(13) . ? C44 C45 1.388(11) . ? C46 C51 1.400(10) . ? C46 C47 1.393(10) . ? C47 C48 1.372(10) . ? C48 C49 1.352(12) . ? C49 C50 1.361(13) . ? C50 C51 1.391(11) . ? C52 C53 1.385(12) . ? C52 C57 1.376(11) . ? C53 C54 1.370(15) . ? C54 C55 1.356(17) . ? C55 C56 1.387(17) . ? C56 C57 1.388(15) . ? C58 C63 1.368(11) . ? C58 C59 1.385(11) . ? C59 C60 1.398(13) . ? C60 C61 1.347(15) . ? C61 C62 1.364(14) . ? C62 C63 1.400(11) . ? 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 C2 Co1 C1 102.0(4) . . ? C2 Co1 C9 138.0(3) . . ? C1 Co1 C9 109.8(4) . . ? C2 Co1 C10 100.1(3) . . ? C1 Co1 C10 148.5(3) . . ? C9 Co1 C10 40.9(3) . . ? C2 Co1 P3 102.2(2) . . ? C1 Co1 P3 94.2(2) . . ? C9 Co1 P3 101.99(18) . . ? C10 Co1 P3 102.81(18) . . ? C2 Co1 Co2 93.9(3) . . ? C1 Co1 Co2 105.7(2) . . ? C9 Co1 Co2 51.93(17) . . ? C10 Co1 Co2 50.34(17) . . ? P3 Co1 Co2 151.18(6) . . ? C3 Co2 C4 100.5(5) . . ? C3 Co2 C10 110.9(3) . . ? C4 Co2 C10 100.0(3) . . ? C3 Co2 C9 99.2(4) . . ? C4 Co2 C9 140.0(3) . . ? C10 Co2 C9 40.2(2) . . ? C3 Co2 P5 95.4(3) . . ? C4 Co2 P5 94.7(3) . . ? C10 Co2 P5 146.59(19) . . ? C9 Co2 P5 117.7(2) . . ? C3 Co2 Co1 148.7(3) . . ? C4 Co2 Co1 107.0(3) . . ? C10 Co2 Co1 50.08(18) . . ? C9 Co2 Co1 49.72(18) . . ? P5 Co2 Co1 96.95(8) . . ? C5 Co3 C6 92.5(4) . . ? C5 Co3 C12 97.9(3) . . ? C6 Co3 C12 112.3(4) . . ? C5 Co3 C11 106.3(3) . . ? C6 Co3 C11 147.9(4) . . ? C12 Co3 C11 40.7(3) . . ? C5 Co3 P1 100.8(3) . . ? C6 Co3 P1 99.2(3) . . ? C12 Co3 P1 142.37(19) . . ? C11 Co3 P1 102.35(18) . . ? C5 Co3 Co4 148.3(3) . . ? C6 Co3 Co4 101.4(4) . . ? C12 Co3 Co4 50.57(18) . . ? C11 Co3 Co4 50.13(17) . . ? P1 Co3 Co4 104.76(6) . . ? C7 Co4 C8 94.9(4) . . ? C7 Co4 C11 112.0(3) . . ? C8 Co4 C11 141.2(3) . . ? C7 Co4 C12 101.1(3) . . ? C8 Co4 C12 108.9(3) . . ? C11 Co4 C12 40.8(3) . . ? C7 Co4 P2 98.1(2) . . ? C8 Co4 P2 103.2(3) . . ? C11 Co4 P2 100.09(18) . . ? C12 Co4 P2 140.7(2) . . ? C7 Co4 Co3 151.1(2) . . ? C8 Co4 Co3 92.4(3) . . ? C11 Co4 Co3 50.85(18) . . ? C12 Co4 Co3 50.22(19) . . ? P2 Co4 Co3 107.37(6) . . ? C9 P1 C16 108.1(4) . . ? C9 P1 C22 105.1(3) . . ? C16 P1 C22 100.8(4) . . ? C9 P1 Co3 111.4(2) . . ? C16 P1 Co3 114.0(3) . . ? C22 P1 Co3 116.5(3) . . ? C10 P2 C34 103.3(3) . . ? C10 P2 C28 111.1(3) . . ? C34 P2 C28 99.4(3) . . ? C10 P2 Co4 111.94(19) . . ? C34 P2 Co4 118.2(2) . . ? C28 P2 Co4 112.0(2) . . ? C11 P3 C46 106.1(3) . . ? C11 P3 C40 105.9(3) . . ? C46 P3 C40 101.1(3) . . ? C11 P3 Co1 111.47(19) . . ? C46 P3 Co1 116.8(2) . . ? C40 P3 Co1 114.4(2) . . ? C12 P4 C52 103.5(3) . . ? C12 P4 C58 107.7(3) . . ? C52 P4 C58 102.5(4) . . ? O9 P5 O10 101.2(7) . . ? O9 P5 O11 95.7(6) . . ? O10 P5 O11 106.2(5) . . ? O9 P5 Co2 115.8(5) . . ? O10 P5 Co2 115.6(3) . . ? O11 P5 Co2 119.3(3) . . ? C13 O9 P5 144.0(15) . . ? C14 O10 P5 126.8(9) . . ? C15 O11 P5 128.2(8) . . ? O1 C1 Co1 175.8(9) . . ? O2 C2 Co1 175.2(7) . . ? O3 C3 Co2 175.1(9) . . ? O4 C4 Co2 176.7(10) . . ? O5 C5 Co3 174.5(10) . . ? O6 C6 Co3 175.1(11) . . ? O7 C7 Co4 178.5(7) . . ? O8 C8 Co4 179.7(10) . . ? C10 C9 P1 127.5(5) . . ? C10 C9 Co1 69.6(4) . . ? P1 C9 Co1 133.8(3) . . ? C10 C9 Co2 67.9(3) . . ? P1 C9 Co2 145.8(4) . . ? Co1 C9 Co2 78.4(2) . . ? C9 C10 P2 136.0(5) . . ? C9 C10 Co2 72.0(4) . . ? P2 C10 Co2 145.5(3) . . ? C9 C10 Co1 69.4(4) . . ? P2 C10 Co1 124.6(3) . . ? Co2 C10 Co1 79.6(2) . . ? C12 C11 P3 149.8(5) . . ? C12 C11 Co4 70.0(4) . . ? P3 C11 Co4 131.3(3) . . ? C12 C11 Co3 68.9(4) . . ? P3 C11 Co3 129.5(3) . . ? Co4 C11 Co3 79.0(2) . . ? C11 C12 P4 144.2(5) . . ? C11 C12 Co3 70.4(4) . . ? P4 C12 Co3 143.0(4) . . ? C11 C12 Co4 69.2(3) . . ? P4 C12 Co4 119.2(4) . . ? Co3 C12 Co4 79.2(2) . . ? C21 C16 C17 118.2(9) . . ? C21 C16 P1 124.4(7) . . ? C17 C16 P1 117.4(8) . . ? C18 C17 C16 120.2(12) . . ? C19 C18 C17 121.0(13) . . ? C18 C19 C20 120.9(11) . . ? C19 C20 C21 117.1(13) . . ? C16 C21 C20 122.7(12) . . ? C23 C22 C27 120.2(8) . . ? C23 C22 P1 119.2(6) . . ? C27 C22 P1 120.6(8) . . ? C22 C23 C24 121.4(9) . . ? C25 C24 C23 118.4(11) . . ? C24 C25 C26 123.1(10) . . ? C25 C26 C27 119.0(10) . . ? C22 C27 C26 117.8(11) . . ? C33 C28 C29 119.2(7) . . ? C33 C28 P2 123.8(6) . . ? C29 C28 P2 117.0(5) . . ? C30 C29 C28 121.4(9) . . ? C29 C30 C31 120.9(10) . . ? C30 C31 C32 120.7(9) . . ? C31 C32 C33 119.2(9) . . ? C28 C33 C32 118.7(9) . . ? C39 C34 C35 117.1(6) . . ? C39 C34 P2 122.3(5) . . ? C35 C34 P2 120.5(5) . . ? C36 C35 C34 120.5(7) . . ? C37 C36 C35 120.2(7) . . ? C38 C37 C36 120.2(7) . . ? C37 C38 C39 120.4(7) . . ? C38 C39 C34 121.6(7) . . ? C45 C40 C41 118.5(7) . . ? C45 C40 P3 117.2(5) . . ? C41 C40 P3 124.3(6) . . ? C42 C41 C40 120.2(8) . . ? C43 C42 C41 121.3(8) . . ? C44 C43 C42 119.1(8) . . ? C43 C44 C45 119.9(9) . . ? C40 C45 C44 120.9(8) . . ? C51 C46 C47 117.7(7) . . ? C51 C46 P3 119.2(6) . . ? C47 C46 P3 123.1(5) . . ? C48 C47 C46 119.9(7) . . ? C49 C48 C47 122.1(8) . . ? C50 C49 C48 119.7(8) . . ? C49 C50 C51 120.1(8) . . ? C50 C51 C46 120.5(8) . . ? C53 C52 C57 118.8(8) . . ? C53 C52 P4 123.2(6) . . ? C57 C52 P4 118.0(7) . . ? C54 C53 C52 120.7(10) . . ? C53 C54 C55 120.8(12) . . ? C54 C55 C56 119.5(11) . . ? C57 C56 C55 120.0(10) . . ? C56 C57 C52 120.2(10) . . ? C63 C58 C59 118.8(7) . . ? C63 C58 P4 121.3(6) . . ? C59 C58 P4 119.1(7) . . ? C58 C59 C60 119.8(10) . . ? C61 C60 C59 120.5(10) . . ? C60 C61 C62 120.6(9) . . ? C61 C62 C63 119.5(10) . . ? C58 C63 C62 120.8(8) . . ? _diffrn_measured_fraction_theta_max 0.977 _diffrn_reflns_theta_full 26.03 _diffrn_measured_fraction_theta_full 0.977 _refine_diff_density_max 1.088 _refine_diff_density_min -0.835 _refine_diff_density_rms 0.102 data_hong154m _database_code_CSD 209742 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C61 H40 Cl2 Co4 O9 P4 Pd' _chemical_formula_weight 1453.83 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 15.029(4) _cell_length_b 23.761(7) _cell_length_c 17.180(5) _cell_angle_alpha 90.00 _cell_angle_beta 98.846(7) _cell_angle_gamma 90.00 _cell_volume 6062(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3819 _cell_measurement_theta_min 2.196 _cell_measurement_theta_max 22.202 _exptl_crystal_description parallelepiped _exptl_crystal_colour brown _exptl_crystal_size_max 0.49 _exptl_crystal_size_mid 0.45 _exptl_crystal_size_min 0.34 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.593 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2904 _exptl_absorpt_coefficient_mu 1.611 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.227867 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 33858 _diffrn_reflns_av_R_equivalents 0.2175 _diffrn_reflns_av_sigmaI/netI 0.2428 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.68 _diffrn_reflns_theta_max 25.98 _reflns_number_total 11746 _reflns_number_gt 4405 _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^)+(0.1525P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11746 _refine_ls_number_parameters 730 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2518 _refine_ls_R_factor_gt 0.0889 _refine_ls_wR_factor_ref 0.3144 _refine_ls_wR_factor_gt 0.2158 _refine_ls_goodness_of_fit_ref 0.986 _refine_ls_restrained_S_all 0.986 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd Pd 0.03567(7) 0.11158(4) 0.23567(8) 0.0523(4) Uani 1 1 d . . . Co1 Co -0.42130(13) 0.15031(7) 0.13384(12) 0.0499(6) Uani 1 1 d . . . Co2 Co -0.48516(14) 0.14537(8) 0.25909(13) 0.0550(6) Uani 1 1 d . . . Co3 Co -0.17516(12) 0.23314(7) 0.21399(12) 0.0465(5) Uani 1 1 d . . . Co4 Co -0.14123(13) 0.12809(7) 0.23109(12) 0.0457(5) Uani 1 1 d . . . P1 P -0.3059(3) 0.24555(14) 0.2612(2) 0.0512(10) Uani 1 1 d . . . P2 P -0.2660(3) 0.08417(14) 0.2610(2) 0.0477(10) Uani 1 1 d . . . P3 P -0.3049(3) 0.16572(14) 0.0692(2) 0.0474(10) Uani 1 1 d . . . P4 P -0.0007(3) 0.17406(14) 0.1415(2) 0.0484(10) Uani 1 1 d . . . Cl1 Cl 0.0628(3) 0.04755(15) 0.3434(3) 0.0728(13) Uani 1 1 d . . . Cl2 Cl 0.1866(3) 0.11232(19) 0.2151(3) 0.0824(14) Uani 1 1 d . . . O1 O -0.5550(9) 0.2202(5) 0.0352(8) 0.096(4) Uani 1 1 d . . . O2 O -0.4955(8) 0.0422(5) 0.0698(8) 0.089(4) Uani 1 1 d . . . O3 O -0.4916(10) 0.1769(6) 0.4212(9) 0.109(5) Uani 1 1 d . . . O4 O -0.5613(10) 0.0317(5) 0.2604(9) 0.114(5) Uani 1 1 d . . . O5 O -0.1707(9) 0.3345(5) 0.1175(8) 0.092(4) Uani 1 1 d . . . O6 O -0.0504(9) 0.2834(5) 0.3434(8) 0.094(4) Uani 1 1 d . . . O7 O -0.0838(7) 0.0180(4) 0.1782(7) 0.066(3) Uani 1 1 d . . . O8 O -0.0649(8) 0.1555(4) 0.3943(8) 0.077(3) Uani 1 1 d . . . O9 O -0.6478(9) 0.2110(6) 0.2052(9) 0.111(5) Uani 1 1 d . . . C1 C -0.5010(11) 0.1952(7) 0.0731(10) 0.061(4) Uani 1 1 d . . . C2 C -0.4631(10) 0.0845(6) 0.0925(10) 0.060(4) Uani 1 1 d . . . C3 C -0.4850(11) 0.1652(6) 0.3591(12) 0.065(5) Uani 1 1 d . . . C4 C -0.5305(11) 0.0748(7) 0.2601(10) 0.068(5) Uani 1 1 d . . . C5 C -0.1784(10) 0.2951(7) 0.1549(10) 0.061(4) Uani 1 1 d . . . C6 C -0.0978(11) 0.2630(6) 0.2945(12) 0.066(5) Uani 1 1 d . . . C7 C -0.0964(9) 0.0628(6) 0.2043(9) 0.050(4) Uani 1 1 d . . . C8 C -0.0896(11) 0.1442(5) 0.3303(11) 0.054(4) Uani 1 1 d . . . C9 C -0.3774(9) 0.1857(5) 0.2359(8) 0.049(4) Uani 1 1 d . . . C10 C -0.3628(9) 0.1294(5) 0.2374(8) 0.046(3) Uani 1 1 d . . . C11 C -0.2024(10) 0.1708(5) 0.1367(8) 0.048(4) Uani 1 1 d . . . C12 C -0.1127(10) 0.1847(6) 0.1492(9) 0.055(4) Uani 1 1 d . . . C13 C -0.5857(11) 0.1846(7) 0.2243(11) 0.069(5) Uani 1 1 d . . . C14 C -0.3723(11) 0.3080(5) 0.2274(10) 0.057(4) Uani 1 1 d . . . C15 C -0.3293(10) 0.3607(6) 0.2256(11) 0.071(5) Uani 1 1 d . . . H15A H -0.2683 0.3644 0.2447 0.086 Uiso 1 1 calc R . . C16 C -0.3772(15) 0.4049(7) 0.1961(14) 0.094(7) Uani 1 1 d . . . H16A H -0.3482 0.4393 0.1935 0.113 Uiso 1 1 calc R . . C17 C -0.4648(17) 0.4018(7) 0.1705(12) 0.103(7) Uani 1 1 d . . . H17A H -0.4949 0.4340 0.1501 0.123 Uiso 1 1 calc R . . C18 C -0.5143(13) 0.3518(7) 0.1728(12) 0.087(6) Uani 1 1 d . . . H18A H -0.5760 0.3498 0.1557 0.105 Uiso 1 1 calc R . . C19 C -0.4638(11) 0.3058(7) 0.2024(10) 0.067(5) Uani 1 1 d . . . H19A H -0.4932 0.2716 0.2057 0.081 Uiso 1 1 calc R . . C20 C -0.2929(9) 0.2505(7) 0.3690(9) 0.057(4) Uani 1 1 d . . . C21 C -0.3002(11) 0.3016(7) 0.4075(12) 0.077(5) Uani 1 1 d . . . H21A H -0.3146 0.3341 0.3780 0.092 Uiso 1 1 calc R . . C22 C -0.2865(13) 0.3048(10) 0.4875(15) 0.091(7) Uani 1 1 d . . . H22A H -0.2914 0.3392 0.5123 0.109 Uiso 1 1 calc R . . C23 C -0.2659(14) 0.2578(13) 0.5309(14) 0.113(9) Uani 1 1 d . . . H23A H -0.2582 0.2599 0.5855 0.135 Uiso 1 1 calc R . . C24 C -0.2562(13) 0.2067(10) 0.4950(11) 0.097(7) Uani 1 1 d . . . H24A H -0.2395 0.1749 0.5255 0.117 Uiso 1 1 calc R . . C25 C -0.2711(12) 0.2028(7) 0.4139(10) 0.077(5) Uani 1 1 d . . . H25A H -0.2666 0.1681 0.3896 0.093 Uiso 1 1 calc R . . C26 C -0.3029(9) 0.0190(5) 0.2098(10) 0.054(4) Uani 1 1 d . . . C27 C -0.2869(11) 0.0069(5) 0.1346(10) 0.063(5) Uani 1 1 d . . . H27A H -0.2537 0.0324 0.1098 0.076 Uiso 1 1 calc R . . C28 C -0.3180(11) -0.0416(6) 0.0942(11) 0.070(5) Uani 1 1 d . . . H28A H -0.3041 -0.0486 0.0441 0.085 Uiso 1 1 calc R . . C29 C -0.3679(12) -0.0781(7) 0.1277(13) 0.078(5) Uani 1 1 d . . . H29A H -0.3904 -0.1099 0.0996 0.093 Uiso 1 1 calc R . . C30 C -0.3867(12) -0.0702(6) 0.2020(13) 0.083(6) Uani 1 1 d . . . H30A H -0.4214 -0.0960 0.2247 0.099 Uiso 1 1 calc R . . C31 C -0.3519(10) -0.0213(6) 0.2442(10) 0.063(4) Uani 1 1 d . . . H31A H -0.3620 -0.0163 0.2958 0.076 Uiso 1 1 calc R . . C32 C -0.2547(12) 0.0606(6) 0.3634(10) 0.063(4) Uani 1 1 d . . . C33 C -0.1717(11) 0.0372(6) 0.3961(10) 0.067(5) Uani 1 1 d . . . H33A H -0.1251 0.0363 0.3662 0.080 Uiso 1 1 calc R . . C34 C -0.1575(14) 0.0155(9) 0.4719(12) 0.094(7) Uani 1 1 d . . . H34A H -0.1018 0.0011 0.4940 0.113 Uiso 1 1 calc R . . C35 C -0.2317(18) 0.0159(10) 0.5147(13) 0.120(8) Uani 1 1 d . . . H35A H -0.2249 -0.0006 0.5644 0.144 Uiso 1 1 calc R . . C36 C -0.3122(16) 0.0399(10) 0.4849(12) 0.116(8) Uani 1 1 d . . . H36A H -0.3588 0.0422 0.5146 0.139 Uiso 1 1 calc R . . C37 C -0.3223(12) 0.0611(7) 0.4069(12) 0.081(6) Uani 1 1 d . . . H37A H -0.3777 0.0760 0.3848 0.097 Uiso 1 1 calc R . . C38 C -0.3057(8) 0.2307(6) 0.0127(9) 0.049(4) Uani 1 1 d . . . C39 C -0.2510(11) 0.2339(6) -0.0462(10) 0.064(4) Uani 1 1 d . . . H39A H -0.2164 0.2032 -0.0567 0.077 Uiso 1 1 calc R . . C40 C -0.2488(12) 0.2843(8) -0.0896(11) 0.081(5) Uani 1 1 d . . . H40A H -0.2140 0.2863 -0.1298 0.098 Uiso 1 1 calc R . . C41 C -0.2983(12) 0.3307(7) -0.0726(12) 0.076(5) Uani 1 1 d . . . H41A H -0.2947 0.3641 -0.1002 0.091 Uiso 1 1 calc R . . C42 C -0.3507(12) 0.3280(6) -0.0172(11) 0.071(5) Uani 1 1 d . . . H42A H -0.3843 0.3592 -0.0071 0.085 Uiso 1 1 calc R . . C43 C -0.3558(10) 0.2775(6) 0.0270(10) 0.059(4) Uani 1 1 d . . . H43A H -0.3930 0.2760 0.0655 0.071 Uiso 1 1 calc R . . C44 C -0.2899(9) 0.1132(5) -0.0039(8) 0.045(3) Uani 1 1 d . . . C45 C -0.3636(11) 0.1001(6) -0.0610(10) 0.064(4) Uani 1 1 d . . . H45A H -0.4177 0.1188 -0.0593 0.077 Uiso 1 1 calc R . . C46 C -0.3603(12) 0.0623(7) -0.1176(11) 0.076(5) Uani 1 1 d . . . H46A H -0.4112 0.0544 -0.1540 0.091 Uiso 1 1 calc R . . C47 C -0.2782(14) 0.0344(7) -0.1214(12) 0.082(6) Uani 1 1 d . . . H47A H -0.2749 0.0076 -0.1604 0.099 Uiso 1 1 calc R . . C48 C -0.2054(12) 0.0463(6) -0.0694(11) 0.071(5) Uani 1 1 d . . . H48A H -0.1511 0.0285 -0.0729 0.085 Uiso 1 1 calc R . . C49 C -0.2102(10) 0.0864(6) -0.0081(9) 0.056(4) Uani 1 1 d . . . H49A H -0.1595 0.0943 0.0286 0.067 Uiso 1 1 calc R . . C50 C 0.0538(9) 0.2425(6) 0.1587(9) 0.052(4) Uani 1 1 d . . . C51 C 0.1114(12) 0.2526(6) 0.2263(12) 0.092(7) Uani 1 1 d . . . H51A H 0.1269 0.2228 0.2608 0.110 Uiso 1 1 calc R . . C52 C 0.1473(16) 0.3040(8) 0.2457(14) 0.126(10) Uani 1 1 d . . . H52A H 0.1824 0.3100 0.2945 0.151 Uiso 1 1 calc R . . C53 C 0.1310(14) 0.3467(8) 0.1922(14) 0.094(6) Uani 1 1 d . . . H53A H 0.1612 0.3808 0.2017 0.113 Uiso 1 1 calc R . . C54 C 0.0703(16) 0.3397(7) 0.1249(14) 0.103(7) Uani 1 1 d . . . H54A H 0.0544 0.3698 0.0909 0.123 Uiso 1 1 calc R . . C55 C 0.0336(13) 0.2875(7) 0.1083(11) 0.090(6) Uani 1 1 d . . . H55A H -0.0061 0.2822 0.0618 0.108 Uiso 1 1 calc R . . C56 C 0.0080(9) 0.1495(5) 0.0410(9) 0.049(4) Uani 1 1 d . . . C57 C -0.0289(11) 0.1793(6) -0.0243(11) 0.069(5) Uani 1 1 d . . . H57A H -0.0554 0.2141 -0.0180 0.082 Uiso 1 1 calc R . . C58 C -0.0275(12) 0.1591(8) -0.0984(12) 0.080(5) Uani 1 1 d . . . H58A H -0.0517 0.1800 -0.1423 0.096 Uiso 1 1 calc R . . C59 C 0.0108(13) 0.1066(8) -0.1075(12) 0.082(6) Uani 1 1 d . . . H59A H 0.0134 0.0916 -0.1571 0.098 Uiso 1 1 calc R . . C60 C 0.0445(14) 0.0780(7) -0.0398(13) 0.089(6) Uani 1 1 d . . . H60A H 0.0686 0.0425 -0.0457 0.106 Uiso 1 1 calc R . . C61 C 0.0457(11) 0.0969(6) 0.0343(11) 0.068(5) Uani 1 1 d . . . H61A H 0.0703 0.0760 0.0781 0.081 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 Pd 0.0567(7) 0.0342(6) 0.0607(9) 0.0031(5) -0.0078(6) 0.0042(5) Co1 0.0573(12) 0.0369(10) 0.0504(14) -0.0033(9) -0.0084(10) 0.0027(9) Co2 0.0605(13) 0.0459(11) 0.0544(15) -0.0038(10) -0.0043(10) 0.0041(10) Co3 0.0564(12) 0.0266(9) 0.0520(14) -0.0053(8) -0.0064(10) 0.0024(8) Co4 0.0562(12) 0.0261(9) 0.0494(14) -0.0014(8) -0.0092(10) 0.0044(8) P1 0.064(2) 0.0303(17) 0.055(3) -0.0083(17) -0.003(2) 0.0045(17) P2 0.060(2) 0.0293(17) 0.048(3) -0.0017(16) -0.0092(19) 0.0043(16) P3 0.057(2) 0.0331(18) 0.047(3) -0.0022(16) -0.007(2) 0.0049(16) P4 0.056(2) 0.0331(18) 0.054(3) -0.0010(17) 0.000(2) 0.0033(16) Cl1 0.081(3) 0.045(2) 0.081(3) 0.022(2) -0.023(2) 0.0014(19) Cl2 0.056(2) 0.077(3) 0.111(4) -0.003(3) 0.004(3) 0.007(2) O1 0.092(9) 0.084(9) 0.100(11) 0.030(8) -0.019(8) 0.028(7) O2 0.099(9) 0.067(8) 0.093(10) -0.022(7) -0.007(7) -0.010(7) O3 0.118(11) 0.133(13) 0.072(11) -0.022(9) 0.006(9) 0.015(9) O4 0.137(12) 0.064(8) 0.138(14) -0.009(8) 0.015(10) -0.046(8) O5 0.110(10) 0.051(7) 0.106(11) 0.022(7) -0.007(8) -0.013(7) O6 0.123(11) 0.061(7) 0.082(10) -0.017(7) -0.033(8) -0.003(7) O7 0.074(7) 0.036(5) 0.082(9) -0.020(5) 0.000(6) 0.014(5) O8 0.113(10) 0.054(7) 0.055(9) 0.009(6) -0.018(7) 0.003(6) O9 0.072(9) 0.124(12) 0.134(13) 0.046(10) 0.004(8) 0.039(8) C1 0.056(10) 0.069(10) 0.057(12) 0.000(9) 0.005(9) -0.001(9) C2 0.060(10) 0.048(9) 0.066(12) 0.007(8) -0.011(8) -0.009(8) C3 0.083(12) 0.037(8) 0.072(14) -0.015(8) 0.004(11) 0.013(8) C4 0.069(11) 0.064(11) 0.074(13) -0.005(9) 0.020(9) -0.013(9) C5 0.062(10) 0.054(9) 0.062(12) -0.004(8) -0.002(9) 0.009(8) C6 0.076(11) 0.030(7) 0.087(15) -0.010(8) -0.002(10) 0.008(7) C7 0.041(8) 0.051(8) 0.055(10) 0.004(7) -0.001(7) 0.016(7) C8 0.075(11) 0.031(7) 0.050(11) 0.007(7) -0.011(9) 0.003(7) C9 0.064(10) 0.036(7) 0.044(10) -0.004(6) 0.005(8) 0.003(7) C10 0.060(9) 0.039(7) 0.034(9) -0.009(6) -0.008(7) 0.003(6) C11 0.068(10) 0.027(6) 0.047(10) -0.009(6) 0.005(8) -0.002(6) C12 0.074(11) 0.047(8) 0.038(10) -0.005(7) -0.009(8) -0.015(8) C13 0.058(11) 0.073(11) 0.074(14) 0.011(10) 0.003(10) 0.011(9) C14 0.071(11) 0.034(7) 0.062(11) -0.006(7) 0.002(9) 0.007(7) C15 0.055(10) 0.047(9) 0.107(16) -0.001(9) -0.003(10) 0.006(8) C16 0.109(17) 0.044(10) 0.12(2) 0.008(11) 0.003(15) 0.018(11) C17 0.16(2) 0.051(11) 0.083(16) -0.002(10) -0.026(15) 0.051(13) C18 0.086(13) 0.047(10) 0.120(18) -0.006(10) -0.011(12) 0.026(9) C19 0.064(11) 0.056(9) 0.077(13) -0.017(9) 0.001(9) 0.017(8) C20 0.044(9) 0.074(11) 0.052(11) -0.018(9) 0.001(8) 0.002(8) C21 0.077(12) 0.071(11) 0.074(15) -0.031(10) -0.014(10) 0.011(9) C22 0.080(14) 0.099(16) 0.089(19) -0.054(14) 0.001(13) 0.002(12) C23 0.091(16) 0.17(3) 0.070(18) -0.069(19) -0.008(13) -0.015(17) C24 0.108(15) 0.137(19) 0.035(13) 0.024(12) -0.027(11) -0.022(14) C25 0.113(15) 0.068(11) 0.043(12) -0.008(9) -0.012(10) 0.011(10) C26 0.054(9) 0.027(7) 0.070(12) 0.004(7) -0.021(8) 0.001(6) C27 0.106(13) 0.021(7) 0.056(12) -0.004(7) -0.010(10) -0.002(7) C28 0.088(12) 0.052(9) 0.065(13) -0.013(8) -0.007(10) -0.008(9) C29 0.087(13) 0.049(10) 0.088(16) -0.015(10) -0.014(12) -0.010(9) C30 0.093(14) 0.034(8) 0.110(18) 0.009(10) -0.020(13) -0.004(8) C31 0.063(10) 0.050(9) 0.077(13) 0.004(8) 0.012(9) -0.011(8) C32 0.077(12) 0.048(9) 0.057(12) 0.006(8) -0.006(9) 0.010(8) C33 0.081(12) 0.049(9) 0.067(13) 0.024(8) -0.001(9) 0.013(8) C34 0.087(14) 0.119(17) 0.073(15) 0.043(13) -0.004(12) 0.029(12) C35 0.15(2) 0.127(19) 0.066(17) 0.036(14) -0.024(16) 0.045(17) C36 0.15(2) 0.14(2) 0.052(15) 0.029(13) 0.011(14) 0.070(17) C37 0.064(11) 0.082(13) 0.089(16) 0.012(11) -0.015(11) 0.027(10) C38 0.029(7) 0.045(8) 0.068(11) 0.003(7) -0.006(7) 0.002(6) C39 0.073(11) 0.050(9) 0.064(12) 0.001(8) -0.005(9) 0.007(8) C40 0.098(14) 0.072(12) 0.073(14) 0.018(10) 0.009(11) -0.006(11) C41 0.085(13) 0.049(10) 0.088(15) 0.016(9) -0.005(11) -0.001(9) C42 0.097(14) 0.048(9) 0.065(13) 0.004(8) -0.001(11) 0.021(9) C43 0.062(10) 0.052(9) 0.063(11) 0.004(8) 0.007(8) 0.005(8) C44 0.059(9) 0.043(7) 0.032(9) -0.007(6) 0.002(7) -0.003(7) C45 0.074(11) 0.054(9) 0.058(12) -0.012(8) -0.012(9) 0.003(8) C46 0.092(13) 0.055(10) 0.070(14) -0.018(9) -0.021(10) 0.000(10) C47 0.102(15) 0.062(11) 0.079(15) -0.029(10) 0.000(12) -0.001(11) C48 0.071(12) 0.058(10) 0.082(14) -0.008(9) 0.010(11) 0.020(9) C49 0.056(9) 0.050(8) 0.058(11) -0.013(8) -0.002(8) 0.007(7) C50 0.056(9) 0.045(8) 0.047(10) 0.018(7) -0.016(8) -0.008(7) C51 0.125(16) 0.035(8) 0.093(16) 0.003(9) -0.053(13) -0.007(9) C52 0.18(2) 0.051(11) 0.11(2) 0.008(12) -0.079(17) -0.028(13) C53 0.096(15) 0.081(14) 0.102(18) -0.012(13) 0.008(13) -0.036(12) C54 0.15(2) 0.053(11) 0.100(18) 0.021(10) 0.008(16) -0.047(12) C55 0.133(17) 0.063(11) 0.064(13) 0.021(10) -0.019(11) -0.022(11) C56 0.057(9) 0.035(7) 0.054(10) -0.018(7) 0.006(8) 0.006(7) C57 0.088(12) 0.042(8) 0.072(14) -0.002(9) 0.001(10) 0.019(8) C58 0.094(14) 0.080(13) 0.067(14) -0.001(10) 0.017(11) -0.003(11) C59 0.110(15) 0.069(12) 0.075(15) -0.027(11) 0.040(13) -0.005(11) C60 0.136(17) 0.053(11) 0.081(16) -0.020(10) 0.031(14) 0.014(11) C61 0.082(12) 0.061(10) 0.064(13) 0.000(9) 0.022(10) 0.016(9) _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 Pd P4 2.202(4) . ? Pd C7 2.290(14) . ? Pd Cl2 2.350(4) . ? Pd Cl1 2.382(4) . ? Pd Co4 2.677(2) . ? Co1 C2 1.791(16) . ? Co1 C1 1.811(18) . ? Co1 C10 1.924(14) . ? Co1 C9 1.965(14) . ? Co1 P3 2.242(4) . ? Co1 Co2 2.490(3) . ? Co2 C3 1.782(19) . ? Co2 C13 1.797(18) . ? Co2 C4 1.811(17) . ? Co2 C10 1.969(14) . ? Co2 C9 1.975(14) . ? Co3 C5 1.785(17) . ? Co3 C6 1.809(19) . ? Co3 C12 1.941(15) . ? Co3 C11 1.990(13) . ? Co3 P1 2.257(4) . ? Co3 Co4 2.555(2) . ? Co4 C7 1.780(14) . ? Co4 C8 1.802(18) . ? Co4 C11 2.011(14) . ? Co4 C12 2.038(15) . ? Co4 P2 2.273(4) . ? P1 C9 1.795(14) . ? P1 C14 1.832(14) . ? P1 C20 1.836(16) . ? P2 C10 1.804(14) . ? P2 C26 1.825(14) . ? P2 C32 1.830(17) . ? P3 C11 1.784(16) . ? P3 C44 1.809(13) . ? P3 C38 1.823(14) . ? P4 C12 1.728(16) . ? P4 C50 1.825(14) . ? P4 C56 1.847(14) . ? O1 C1 1.126(17) . ? O2 C2 1.158(16) . ? O3 C3 1.122(18) . ? O4 C4 1.125(18) . ? O5 C5 1.151(17) . ? O6 C6 1.126(18) . ? O7 C7 1.182(15) . ? O8 C8 1.136(17) . ? O9 C13 1.131(17) . ? C9 C10 1.356(17) . ? C11 C12 1.372(19) . ? C14 C19 1.38(2) . ? C14 C15 1.410(19) . ? C15 C16 1.33(2) . ? C16 C17 1.32(3) . ? C17 C18 1.40(3) . ? C18 C19 1.38(2) . ? C20 C25 1.38(2) . ? C20 C21 1.40(2) . ? C21 C22 1.36(3) . ? C22 C23 1.35(3) . ? C23 C24 1.38(3) . ? C24 C25 1.38(2) . ? C26 C27 1.38(2) . ? C26 C31 1.395(19) . ? C27 C28 1.389(19) . ? C28 C29 1.33(2) . ? C29 C30 1.36(2) . ? C30 C31 1.42(2) . ? C32 C37 1.35(2) . ? C32 C33 1.40(2) . ? C33 C34 1.39(2) . ? C34 C35 1.43(3) . ? C35 C36 1.36(3) . ? C36 C37 1.42(2) . ? C38 C43 1.386(18) . ? C38 C39 1.40(2) . ? C39 C40 1.41(2) . ? C40 C41 1.39(2) . ? C41 C42 1.33(2) . ? C42 C43 1.43(2) . ? C44 C49 1.367(18) . ? C44 C45 1.40(2) . ? C45 C46 1.33(2) . ? C46 C47 1.41(2) . ? C47 C48 1.33(2) . ? C48 C49 1.43(2) . ? C50 C51 1.36(2) . ? C50 C55 1.38(2) . ? C51 C52 1.36(2) . ? C52 C53 1.37(3) . ? C53 C54 1.37(3) . ? C54 C55 1.37(2) . ? C56 C57 1.37(2) . ? C56 C61 1.384(18) . ? C57 C58 1.36(2) . ? C58 C59 1.39(2) . ? C59 C60 1.37(2) . ? C60 C61 1.35(2) . ? 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 P4 Pd C7 93.4(4) . . ? P4 Pd Cl2 91.18(16) . . ? C7 Pd Cl2 142.2(4) . . ? P4 Pd Cl1 174.27(16) . . ? C7 Pd Cl1 84.2(4) . . ? Cl2 Pd Cl1 93.90(17) . . ? P4 Pd Co4 75.31(11) . . ? C7 Pd Co4 41.1(3) . . ? Cl2 Pd Co4 166.49(14) . . ? Cl1 Pd Co4 99.61(12) . . ? C2 Co1 C1 97.2(7) . . ? C2 Co1 C10 102.9(6) . . ? C1 Co1 C10 148.5(6) . . ? C2 Co1 C9 141.0(6) . . ? C1 Co1 C9 111.3(6) . . ? C10 Co1 C9 40.8(5) . . ? C2 Co1 P3 101.5(5) . . ? C1 Co1 P3 96.7(5) . . ? C10 Co1 P3 102.7(4) . . ? C9 Co1 P3 101.0(4) . . ? C2 Co1 Co2 98.2(5) . . ? C1 Co1 Co2 102.5(5) . . ? C10 Co1 Co2 51.0(4) . . ? C9 Co1 Co2 51.0(4) . . ? P3 Co1 Co2 150.43(14) . . ? C3 Co2 C13 93.5(8) . . ? C3 Co2 C4 100.4(7) . . ? C13 Co2 C4 100.7(8) . . ? C3 Co2 C10 111.8(7) . . ? C13 Co2 C10 143.0(7) . . ? C4 Co2 C10 100.8(6) . . ? C3 Co2 C9 100.8(7) . . ? C13 Co2 C9 110.8(7) . . ? C4 Co2 C9 140.6(6) . . ? C10 Co2 C9 40.2(5) . . ? C3 Co2 Co1 151.3(6) . . ? C13 Co2 Co1 96.0(6) . . ? C4 Co2 Co1 104.3(5) . . ? C10 Co2 Co1 49.4(4) . . ? C9 Co2 Co1 50.6(4) . . ? C5 Co3 C6 94.0(7) . . ? C5 Co3 C12 97.9(6) . . ? C6 Co3 C12 111.2(7) . . ? C5 Co3 C11 104.5(6) . . ? C6 Co3 C11 147.6(6) . . ? C12 Co3 C11 40.8(5) . . ? C5 Co3 P1 98.5(5) . . ? C6 Co3 P1 99.6(5) . . ? C12 Co3 P1 143.9(4) . . ? C11 Co3 P1 103.6(4) . . ? C5 Co3 Co4 149.2(5) . . ? C6 Co3 Co4 101.7(4) . . ? C12 Co3 Co4 51.7(4) . . ? C11 Co3 Co4 50.7(4) . . ? P1 Co3 Co4 104.81(12) . . ? C7 Co4 C8 107.8(6) . . ? C7 Co4 C11 112.0(6) . . ? C8 Co4 C11 137.1(5) . . ? C7 Co4 C12 105.6(6) . . ? C8 Co4 C12 114.0(6) . . ? C11 Co4 C12 39.6(5) . . ? C7 Co4 P2 91.0(5) . . ? C8 Co4 P2 97.7(5) . . ? C11 Co4 P2 97.1(4) . . ? C12 Co4 P2 136.6(5) . . ? C7 Co4 Co3 153.9(5) . . ? C8 Co4 Co3 87.1(4) . . ? C11 Co4 Co3 49.9(3) . . ? C12 Co4 Co3 48.4(4) . . ? P2 Co4 Co3 108.51(12) . . ? C7 Co4 Pd 57.7(4) . . ? C8 Co4 Pd 73.9(5) . . ? C11 Co4 Pd 115.2(4) . . ? C12 Co4 Pd 78.7(4) . . ? P2 Co4 Pd 140.93(11) . . ? Co3 Co4 Pd 109.04(8) . . ? C9 P1 C14 106.7(7) . . ? C9 P1 C20 105.2(7) . . ? C14 P1 C20 103.6(7) . . ? C9 P1 Co3 109.4(5) . . ? C14 P1 Co3 117.0(5) . . ? C20 P1 Co3 114.0(5) . . ? C10 P2 C26 102.8(6) . . ? C10 P2 C32 110.6(7) . . ? C26 P2 C32 100.4(7) . . ? C10 P2 Co4 109.9(5) . . ? C26 P2 Co4 118.7(6) . . ? C32 P2 Co4 113.6(6) . . ? C11 P3 C44 108.0(6) . . ? C11 P3 C38 102.9(6) . . ? C44 P3 C38 101.9(7) . . ? C11 P3 Co1 110.5(5) . . ? C44 P3 Co1 114.9(5) . . ? C38 P3 Co1 117.4(5) . . ? C12 P4 C50 106.0(7) . . ? C12 P4 C56 109.1(7) . . ? C50 P4 C56 109.8(7) . . ? C12 P4 Pd 100.2(5) . . ? C50 P4 Pd 115.3(5) . . ? C56 P4 Pd 115.4(5) . . ? O1 C1 Co1 175.1(15) . . ? O2 C2 Co1 174.3(16) . . ? O3 C3 Co2 174.8(17) . . ? O4 C4 Co2 177.8(16) . . ? O5 C5 Co3 172.7(14) . . ? O6 C6 Co3 177.6(15) . . ? O7 C7 Co4 166.5(12) . . ? O7 C7 Pd 111.2(10) . . ? Co4 C7 Pd 81.2(6) . . ? O8 C8 Co4 173.6(15) . . ? C10 C9 P1 133.5(12) . . ? C10 C9 Co1 68.0(8) . . ? P1 C9 Co1 131.4(8) . . ? C10 C9 Co2 69.6(8) . . ? P1 C9 Co2 144.6(8) . . ? Co1 C9 Co2 78.4(5) . . ? C9 C10 P2 135.6(11) . . ? C9 C10 Co1 71.2(9) . . ? P2 C10 Co1 126.9(7) . . ? C9 C10 Co2 70.1(8) . . ? P2 C10 Co2 144.7(8) . . ? Co1 C10 Co2 79.5(5) . . ? C12 C11 P3 147.9(12) . . ? C12 C11 Co3 67.7(8) . . ? P3 C11 Co3 123.5(7) . . ? C12 C11 Co4 71.3(9) . . ? P3 C11 Co4 137.1(7) . . ? Co3 C11 Co4 79.4(5) . . ? C11 C12 P4 153.9(11) . . ? C11 C12 Co3 71.5(9) . . ? P4 C12 Co3 133.9(8) . . ? C11 C12 Co4 69.1(8) . . ? P4 C12 Co4 105.5(7) . . ? Co3 C12 Co4 79.9(6) . . ? O9 C13 Co2 176.7(18) . . ? C19 C14 C15 117.7(14) . . ? C19 C14 P1 122.5(11) . . ? C15 C14 P1 119.8(12) . . ? C16 C15 C14 119.2(16) . . ? C17 C16 C15 122.2(18) . . ? C16 C17 C18 122.8(16) . . ? C19 C18 C17 114.6(17) . . ? C14 C19 C18 123.3(16) . . ? C25 C20 C21 118.5(16) . . ? C25 C20 P1 119.3(12) . . ? C21 C20 P1 122.1(14) . . ? C22 C21 C20 121.2(19) . . ? C23 C22 C21 120(2) . . ? C22 C23 C24 121(2) . . ? C23 C24 C25 120(2) . . ? C24 C25 C20 119.8(17) . . ? C27 C26 C31 115.7(13) . . ? C27 C26 P2 123.0(11) . . ? C31 C26 P2 121.3(13) . . ? C26 C27 C28 123.2(16) . . ? C29 C28 C27 119.5(17) . . ? C28 C29 C30 121.7(16) . . ? C29 C30 C31 118.5(17) . . ? C26 C31 C30 121.3(17) . . ? C37 C32 C33 118.8(16) . . ? C37 C32 P2 124.2(14) . . ? C33 C32 P2 116.8(14) . . ? C34 C33 C32 121.5(17) . . ? C33 C34 C35 117.5(17) . . ? C36 C35 C34 122(2) . . ? C35 C36 C37 118(2) . . ? C32 C37 C36 122.6(17) . . ? C43 C38 C39 118.7(14) . . ? C43 C38 P3 122.9(12) . . ? C39 C38 P3 118.4(11) . . ? C38 C39 C40 119.4(15) . . ? C41 C40 C39 120.5(17) . . ? C42 C41 C40 120.5(17) . . ? C41 C42 C43 120.6(16) . . ? C38 C43 C42 120.2(15) . . ? C49 C44 C45 117.7(13) . . ? C49 C44 P3 124.2(11) . . ? C45 C44 P3 118.1(11) . . ? C46 C45 C44 123.3(15) . . ? C45 C46 C47 118.8(16) . . ? C48 C47 C46 120.1(16) . . ? C47 C48 C49 120.4(15) . . ? C44 C49 C48 119.6(14) . . ? C51 C50 C55 116.7(14) . . ? C51 C50 P4 120.4(11) . . ? C55 C50 P4 122.6(12) . . ? C52 C51 C50 123.1(16) . . ? C51 C52 C53 118.7(19) . . ? C52 C53 C54 120.3(17) . . ? C53 C54 C55 118.7(18) . . ? C54 C55 C50 121.9(18) . . ? C57 C56 C61 121.2(14) . . ? C57 C56 P4 121.6(11) . . ? C61 C56 P4 116.8(12) . . ? C58 C57 C56 121.3(15) . . ? C57 C58 C59 119.1(18) . . ? C60 C59 C58 116.9(17) . . ? C61 C60 C59 125.8(17) . . ? C60 C61 C56 115.6(17) . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 25.98 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 2.254 _refine_diff_density_min -1.676 _refine_diff_density_rms 0.170 data_hong140m _database_code_CSD 209743 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C66 H57 Cl6 Co4 O12 P5 Pd' _chemical_formula_weight 1751.74 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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c 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 16.5696(12) _cell_length_b 19.5107(13) _cell_length_c 23.8716(17) _cell_angle_alpha 90.00 _cell_angle_beta 109.1480(10) _cell_angle_gamma 90.00 _cell_volume 7290.4(9) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.67 _exptl_crystal_size_mid 0.59 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.597 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3502 _exptl_absorpt_coefficient_mu 1.520 _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 293(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_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 40766 _diffrn_reflns_av_R_equivalents 0.0473 _diffrn_reflns_av_sigmaI/netI 0.0590 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.38 _diffrn_reflns_theta_max 26.00 _reflns_number_total 14302 _reflns_number_gt 8545 _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^)+(0.1129P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 14302 _refine_ls_number_parameters 865 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0955 _refine_ls_R_factor_gt 0.0494 _refine_ls_wR_factor_ref 0.1732 _refine_ls_wR_factor_gt 0.1409 _refine_ls_goodness_of_fit_ref 0.906 _refine_ls_restrained_S_all 0.906 _refine_ls_shift/su_max 0.394 _refine_ls_shift/su_mean 0.036 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 Pd Pd 0.49092(3) 0.16797(3) 0.277585(19) 0.05761(15) Uani 1 1 d . . . Co1 Co 0.88304(4) 0.23704(3) 0.24469(3) 0.04180(18) Uani 1 1 d . . . Co2 Co 0.99237(4) 0.17655(4) 0.32791(3) 0.0480(2) Uani 1 1 d . . . Co3 Co 0.67924(4) 0.09402(3) 0.20941(3) 0.04129(18) Uani 1 1 d . . . Co4 Co 0.65716(4) 0.17333(3) 0.28788(3) 0.03949(17) Uani 1 1 d . . . P1 P 0.82111(8) 0.06754(7) 0.23821(6) 0.0427(3) Uani 1 1 d . . . P2 P 0.79156(8) 0.19817(7) 0.34674(6) 0.0419(3) Uani 1 1 d . . . P3 P 0.74698(8) 0.25241(6) 0.18945(6) 0.0404(3) Uani 1 1 d . . . P4 P 0.48941(9) 0.17314(7) 0.18533(6) 0.0469(3) Uani 1 1 d . . . P5 P 1.09973(11) 0.16016(10) 0.29578(10) 0.0747(5) Uani 1 1 d . . . Cl1 Cl 0.49837(12) 0.15773(10) 0.37875(7) 0.0813(5) Uani 1 1 d . . . Cl2 Cl 0.34246(11) 0.16171(14) 0.24307(10) 0.1062(7) Uani 1 1 d . . . O1 O 0.9545(3) 0.2460(3) 0.1477(2) 0.0904(15) Uani 1 1 d . . . O2 O 0.9314(3) 0.3769(2) 0.2883(2) 0.0831(14) Uani 1 1 d . . . O3 O 1.0636(4) 0.0760(4) 0.4212(3) 0.136(3) Uani 1 1 d . . . O4 O 1.0673(4) 0.2944(3) 0.4037(3) 0.123(2) Uani 1 1 d . . . O5 O 0.6339(4) 0.0572(3) 0.0847(2) 0.0957(16) Uani 1 1 d . . . O6 O 0.5972(4) -0.0284(3) 0.2368(3) 0.1033(18) Uani 1 1 d . . . O7 O 0.5937(3) 0.2950(2) 0.33320(19) 0.0663(11) Uani 1 1 d . . . O8 O 0.6405(3) 0.0508(2) 0.3565(2) 0.0827(14) Uani 1 1 d . . . O9 O 1.1846(4) 0.1559(6) 0.3475(5) 0.203(5) Uani 1 1 d . . . O10 O 1.1212(5) 0.2082(5) 0.2533(5) 0.202(5) Uani 1 1 d . . . O11 O 1.0951(4) 0.0914(4) 0.2613(4) 0.156(3) Uani 1 1 d . . . C1 C 0.9272(4) 0.2407(3) 0.1858(3) 0.0565(14) Uani 1 1 d . . . C2 C 0.9099(4) 0.3232(3) 0.2722(3) 0.0546(14) Uani 1 1 d . . . C3 C 1.0326(4) 0.1135(4) 0.3834(3) 0.083(2) Uani 1 1 d . . . C4 C 1.0374(4) 0.2485(4) 0.3739(3) 0.0743(19) Uani 1 1 d . . . C5 C 0.6556(4) 0.0722(3) 0.1325(3) 0.0561(14) Uani 1 1 d . . . C6 C 0.6310(4) 0.0185(3) 0.2264(3) 0.0608(15) Uani 1 1 d . . . C7 C 0.6106(3) 0.2446(3) 0.3147(2) 0.0500(13) Uani 1 1 d . . . C8 C 0.6441(4) 0.0992(3) 0.3310(3) 0.0602(15) Uani 1 1 d . . . C9 C 0.8831(3) 0.1415(3) 0.2708(2) 0.0424(11) Uani 1 1 d . . . C10 C 0.8695(3) 0.1851(2) 0.3113(2) 0.0399(11) Uani 1 1 d . . . C11 C 0.6782(3) 0.1958(2) 0.2123(2) 0.0378(11) Uani 1 1 d . . . C12 C 0.5997(3) 0.1684(2) 0.1974(2) 0.0396(11) Uani 1 1 d . . . C13 C 1.2552(9) 0.1497(7) 0.3730(6) 0.209(8) Uani 1 1 d . . . H13A H 1.2646 0.1549 0.4147 0.313 Uiso 1 1 calc R . . H13B H 1.2871 0.1839 0.3604 0.313 Uiso 1 1 calc R . . H13C H 1.2737 0.1050 0.3657 0.313 Uiso 1 1 calc R . . C14 C 1.1408(8) 0.2755(6) 0.2576(7) 0.217(9) Uani 1 1 d . . . H14A H 1.1503 0.2905 0.2220 0.325 Uiso 1 1 calc R . . H14B H 1.1916 0.2829 0.2909 0.325 Uiso 1 1 calc R . . H14C H 1.0945 0.3011 0.2631 0.325 Uiso 1 1 calc R . . C15 C 1.1449(6) 0.0701(6) 0.2259(4) 0.130(4) Uani 1 1 d . . . H15A H 1.1273 0.0250 0.2105 0.195 Uiso 1 1 calc R . . H15B H 1.2042 0.0692 0.2497 0.195 Uiso 1 1 calc R . . H15C H 1.1368 0.1016 0.1936 0.195 Uiso 1 1 calc R . . C16 C 0.8546(3) 0.0359(3) 0.1774(2) 0.0516(13) Uani 1 1 d . . . C17 C 0.8151(5) -0.0230(3) 0.1484(3) 0.078(2) Uani 1 1 d . . . H17A H 0.7734 -0.0442 0.1606 0.093 Uiso 1 1 calc R . . C18 C 0.8364(6) -0.0504(4) 0.1022(4) 0.100(3) Uani 1 1 d . . . H18A H 0.8092 -0.0899 0.0834 0.120 Uiso 1 1 calc R . . C19 C 0.8978(6) -0.0197(5) 0.0838(4) 0.101(3) Uani 1 1 d . . . H19A H 0.9119 -0.0378 0.0522 0.121 Uiso 1 1 calc R . . C20 C 0.9382(5) 0.0383(5) 0.1126(3) 0.094(2) Uani 1 1 d . . . H20A H 0.9804 0.0592 0.1008 0.113 Uiso 1 1 calc R . . C21 C 0.9159(4) 0.0656(3) 0.1596(3) 0.0648(16) Uani 1 1 d . . . H21A H 0.9435 0.1047 0.1789 0.078 Uiso 1 1 calc R . . C22 C 0.8647(4) -0.0013(3) 0.2917(2) 0.0500(13) Uani 1 1 d . . . C23 C 0.8207(4) -0.0300(4) 0.3252(3) 0.0766(19) Uani 1 1 d . . . H23A H 0.7659 -0.0146 0.3208 0.092 Uiso 1 1 calc R . . C24 C 0.8566(6) -0.0820(4) 0.3660(4) 0.100(3) Uani 1 1 d . . . H24A H 0.8252 -0.1013 0.3880 0.120 Uiso 1 1 calc R . . C25 C 0.9364(5) -0.1043(4) 0.3737(4) 0.089(2) Uani 1 1 d . . . H25A H 0.9606 -0.1384 0.4013 0.107 Uiso 1 1 calc R . . C26 C 0.9818(5) -0.0765(4) 0.3407(4) 0.090(2) Uani 1 1 d . . . H26A H 1.0365 -0.0924 0.3452 0.108 Uiso 1 1 calc R . . C27 C 0.9467(4) -0.0252(3) 0.3007(3) 0.0688(17) Uani 1 1 d . . . H27A H 0.9787 -0.0061 0.2792 0.083 Uiso 1 1 calc R . . C28 C 0.8148(4) 0.1451(3) 0.4139(2) 0.0519(13) Uani 1 1 d . . . C29 C 0.7699(5) 0.1602(4) 0.4524(3) 0.083(2) Uani 1 1 d . . . H29A H 0.7332 0.1976 0.4450 0.099 Uiso 1 1 calc R . . C30 C 0.7798(6) 0.1198(5) 0.5014(3) 0.104(3) Uani 1 1 d . . . H30A H 0.7488 0.1299 0.5266 0.124 Uiso 1 1 calc R . . C31 C 0.8325(6) 0.0668(5) 0.5133(3) 0.100(3) Uani 1 1 d . . . H31A H 0.8401 0.0406 0.5471 0.120 Uiso 1 1 calc R . . C32 C 0.8757(5) 0.0511(4) 0.4752(4) 0.103(3) Uani 1 1 d . . . H32A H 0.9121 0.0134 0.4832 0.124 Uiso 1 1 calc R . . C33 C 0.8667(4) 0.0899(3) 0.4251(3) 0.0679(17) Uani 1 1 d . . . H33A H 0.8961 0.0781 0.3994 0.081 Uiso 1 1 calc R . . C34 C 0.8181(3) 0.2839(3) 0.3786(2) 0.0524(14) Uani 1 1 d . . . C35 C 0.7808(4) 0.3419(3) 0.3477(3) 0.0629(16) Uani 1 1 d . . . H35A H 0.7375 0.3371 0.3114 0.076 Uiso 1 1 calc R . . C36 C 0.8061(5) 0.4061(3) 0.3692(4) 0.083(2) Uani 1 1 d . . . H36A H 0.7807 0.4445 0.3475 0.100 Uiso 1 1 calc R . . C37 C 0.8695(6) 0.4135(5) 0.4235(5) 0.107(3) Uani 1 1 d . . . H37A H 0.8862 0.4570 0.4389 0.129 Uiso 1 1 calc R . . C38 C 0.9087(6) 0.3552(5) 0.4553(4) 0.108(3) Uani 1 1 d . . . H38A H 0.9524 0.3601 0.4913 0.130 Uiso 1 1 calc R . . C39 C 0.8827(4) 0.2907(4) 0.4334(3) 0.081(2) Uani 1 1 d . . . H39A H 0.9079 0.2520 0.4548 0.097 Uiso 1 1 calc R . . C40 C 0.7155(3) 0.2336(3) 0.1095(2) 0.0494(13) Uani 1 1 d . . . C41 C 0.6452(4) 0.2666(4) 0.0696(3) 0.0734(18) Uani 1 1 d . . . H41A H 0.6164 0.3004 0.0829 0.088 Uiso 1 1 calc R . . C42 C 0.6183(6) 0.2490(5) 0.0099(3) 0.100(3) Uani 1 1 d . . . H42A H 0.5712 0.2704 -0.0168 0.119 Uiso 1 1 calc R . . C43 C 0.6625(6) 0.1994(4) -0.0089(3) 0.089(3) Uani 1 1 d . . . H43A H 0.6444 0.1870 -0.0488 0.106 Uiso 1 1 calc R . . C44 C 0.7319(5) 0.1682(4) 0.0293(3) 0.081(2) Uani 1 1 d . . . H44A H 0.7616 0.1353 0.0156 0.098 Uiso 1 1 calc R . . C45 C 0.7585(4) 0.1853(3) 0.0889(3) 0.0624(16) Uani 1 1 d . . . H45A H 0.8060 0.1637 0.1151 0.075 Uiso 1 1 calc R . . C46 C 0.7052(4) 0.3396(3) 0.1874(2) 0.0517(14) Uani 1 1 d . . . C47 C 0.6319(4) 0.3552(3) 0.2002(3) 0.0603(15) Uani 1 1 d . . . H47A H 0.6017 0.3205 0.2112 0.072 Uiso 1 1 calc R . . C48 C 0.6029(5) 0.4221(4) 0.1968(3) 0.080(2) Uani 1 1 d . . . H48A H 0.5536 0.4326 0.2056 0.096 Uiso 1 1 calc R . . C49 C 0.6474(6) 0.4722(4) 0.1803(4) 0.103(3) Uani 1 1 d . . . H49A H 0.6282 0.5172 0.1781 0.124 Uiso 1 1 calc R . . C50 C 0.7192(6) 0.4579(4) 0.1668(4) 0.099(3) Uani 1 1 d . . . H50A H 0.7480 0.4930 0.1550 0.119 Uiso 1 1 calc R . . C51 C 0.7498(5) 0.3915(3) 0.1707(3) 0.0728(18) Uani 1 1 d . . . H51A H 0.7996 0.3818 0.1623 0.087 Uiso 1 1 calc R . . C52 C 0.4422(4) 0.0998(3) 0.1396(3) 0.0654(17) Uani 1 1 d . . . C53 C 0.4180(5) 0.0437(4) 0.1651(4) 0.103(3) Uani 1 1 d . . . H53A H 0.4204 0.0458 0.2046 0.123 Uiso 1 1 calc R . . C54 C 0.3904(7) -0.0154(5) 0.1332(7) 0.147(5) Uani 1 1 d . . . H54A H 0.3788 -0.0545 0.1515 0.176 Uiso 1 1 calc R . . C55 C 0.3805(8) -0.0153(7) 0.0739(7) 0.164(6) Uani 1 1 d . . . H55A H 0.3579 -0.0537 0.0511 0.197 Uiso 1 1 calc R . . C56 C 0.4026(10) 0.0387(6) 0.0488(5) 0.182(7) Uani 1 1 d . . . H56A H 0.3966 0.0374 0.0087 0.218 Uiso 1 1 calc R . . C57 C 0.4347(7) 0.0974(4) 0.0815(4) 0.126(4) Uani 1 1 d . . . H57A H 0.4509 0.1348 0.0635 0.152 Uiso 1 1 calc R . . C58 C 0.4448(3) 0.2514(3) 0.1464(3) 0.0567(15) Uani 1 1 d . . . C59 C 0.4063(5) 0.2983(4) 0.1735(4) 0.088(2) Uani 1 1 d . . . H59A H 0.4028 0.2892 0.2109 0.106 Uiso 1 1 calc R . . C60 C 0.3732(6) 0.3589(5) 0.1441(6) 0.128(4) Uani 1 1 d . . . H60A H 0.3479 0.3904 0.1625 0.154 Uiso 1 1 calc R . . C61 C 0.3767(7) 0.3733(6) 0.0900(6) 0.133(4) Uani 1 1 d . . . H61A H 0.3522 0.4134 0.0708 0.159 Uiso 1 1 calc R . . C62 C 0.4160(8) 0.3290(5) 0.0630(5) 0.129(4) Uani 1 1 d . . . H62A H 0.4202 0.3394 0.0261 0.155 Uiso 1 1 calc R . . C63 C 0.4505(5) 0.2669(4) 0.0921(3) 0.086(2) Uani 1 1 d . . . H63A H 0.4773 0.2365 0.0739 0.104 Uiso 1 1 calc R . . C100 C 0.598(2) -0.1891(17) 0.1152(11) 0.481(7) Uani 1 1 d . . . Cl3 Cl 0.6381(7) -0.1521(4) 0.1766(4) 0.198(3) Uani 0.60 1 d P . . Cl3' Cl 0.5649(10) -0.1172(7) 0.1061(11) 0.252(8) Uani 0.40 1 d P . . Cl4 Cl 0.5952(19) -0.1483(16) 0.0626(10) 0.191(9) Uani 0.20 1 d P . . Cl4' Cl 0.6578(5) -0.1919(3) 0.0634(3) 0.208(3) Uani 0.80 1 d P . . C101 C 1.2143(9) 0.2986(10) 0.5685(12) 0.367(19) Uani 1 1 d . . . H10A H 1.2361 0.2913 0.5359 0.441 Uiso 1 1 calc R . . H10B H 1.2593 0.2893 0.6057 0.441 Uiso 1 1 calc R . . Cl5 Cl 1.1707(4) 0.3882(3) 0.5672(2) 0.267(3) Uani 1 1 d . . . Cl6 Cl 1.1396(7) 0.2568(4) 0.5622(4) 0.498(9) Uani 1 1 d . . . C102 C 0.531(3) 0.0242(13) 0.4872(14) 0.321(17) Uani 1 1 d . . . O101 O 0.5919(8) 0.0135(8) 0.5168(4) 0.189(6) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd 0.0413(3) 0.0799(3) 0.0523(3) -0.0066(2) 0.0162(2) -0.0062(2) Co1 0.0397(4) 0.0371(4) 0.0455(4) 0.0027(3) 0.0098(3) -0.0021(3) Co2 0.0369(4) 0.0458(4) 0.0551(4) 0.0049(3) 0.0067(3) 0.0013(3) Co3 0.0409(4) 0.0354(4) 0.0462(4) -0.0031(3) 0.0124(3) -0.0008(3) Co4 0.0383(4) 0.0397(4) 0.0389(4) -0.0002(3) 0.0106(3) 0.0002(3) P1 0.0433(7) 0.0336(7) 0.0515(8) -0.0005(6) 0.0160(6) 0.0010(6) P2 0.0420(7) 0.0425(7) 0.0373(7) 0.0005(6) 0.0077(6) 0.0041(6) P3 0.0416(7) 0.0362(7) 0.0397(7) 0.0032(5) 0.0083(5) -0.0013(5) P4 0.0368(7) 0.0528(8) 0.0463(7) -0.0054(6) 0.0073(6) -0.0024(6) P5 0.0426(9) 0.0858(13) 0.0980(14) 0.0058(11) 0.0261(9) -0.0025(9) Cl1 0.0789(12) 0.1127(15) 0.0597(9) -0.0074(9) 0.0329(9) -0.0101(10) Cl2 0.0426(9) 0.171(2) 0.1040(15) -0.0125(14) 0.0232(9) -0.0146(11) O1 0.099(4) 0.103(4) 0.088(3) -0.005(3) 0.055(3) -0.022(3) O2 0.089(3) 0.049(3) 0.105(4) -0.013(3) 0.022(3) -0.019(2) O3 0.086(4) 0.154(6) 0.144(5) 0.098(5) 0.007(4) 0.023(4) O4 0.116(5) 0.101(4) 0.122(5) -0.046(4) -0.001(4) -0.025(4) O5 0.125(4) 0.097(4) 0.056(3) -0.028(3) 0.017(3) -0.020(3) O6 0.112(4) 0.071(3) 0.129(5) 0.006(3) 0.042(4) -0.036(3) O7 0.063(3) 0.063(3) 0.073(3) -0.019(2) 0.023(2) 0.005(2) O8 0.111(4) 0.061(3) 0.089(3) 0.024(3) 0.051(3) 0.003(3) O9 0.042(4) 0.295(12) 0.244(10) 0.043(9) 0.011(5) 0.027(5) O10 0.148(7) 0.207(9) 0.308(12) 0.132(9) 0.152(8) 0.049(7) O11 0.102(5) 0.185(7) 0.214(8) -0.095(6) 0.096(5) -0.023(5) C1 0.056(4) 0.055(3) 0.058(3) 0.006(3) 0.018(3) -0.009(3) C2 0.053(3) 0.053(4) 0.055(3) 0.006(3) 0.013(3) -0.002(3) C3 0.044(4) 0.093(5) 0.102(5) 0.035(5) 0.011(4) 0.006(4) C4 0.059(4) 0.078(5) 0.074(4) -0.008(4) 0.006(3) -0.008(3) C5 0.060(4) 0.047(3) 0.057(4) -0.008(3) 0.012(3) -0.004(3) C6 0.059(4) 0.052(4) 0.070(4) -0.007(3) 0.021(3) -0.007(3) C7 0.049(3) 0.055(3) 0.044(3) 0.001(3) 0.013(2) 0.002(3) C8 0.056(4) 0.063(4) 0.062(4) -0.003(3) 0.020(3) -0.003(3) C9 0.034(3) 0.039(3) 0.051(3) 0.003(2) 0.009(2) 0.001(2) C10 0.038(3) 0.035(3) 0.043(3) 0.003(2) 0.009(2) 0.002(2) C11 0.036(3) 0.035(3) 0.039(3) 0.003(2) 0.008(2) 0.003(2) C12 0.038(3) 0.044(3) 0.035(2) -0.002(2) 0.010(2) 0.004(2) C13 0.187(15) 0.161(12) 0.174(13) -0.049(9) -0.084(11) 0.037(10) C14 0.151(11) 0.115(9) 0.32(2) 0.122(12) -0.008(11) -0.023(8) C15 0.093(6) 0.190(11) 0.121(7) -0.026(7) 0.056(6) 0.020(7) C16 0.050(3) 0.046(3) 0.060(3) -0.007(3) 0.019(3) 0.004(3) C17 0.083(5) 0.064(4) 0.096(5) -0.034(4) 0.042(4) -0.007(4) C18 0.092(6) 0.095(6) 0.112(6) -0.048(5) 0.032(5) 0.000(5) C19 0.102(7) 0.122(7) 0.083(5) -0.036(5) 0.037(5) 0.016(6) C20 0.087(6) 0.124(7) 0.088(5) 0.000(5) 0.049(5) 0.011(5) C21 0.066(4) 0.067(4) 0.068(4) -0.010(3) 0.030(3) 0.002(3) C22 0.057(3) 0.033(3) 0.059(3) 0.004(2) 0.017(3) 0.004(2) C23 0.062(4) 0.080(5) 0.090(5) 0.029(4) 0.028(4) 0.014(3) C24 0.097(6) 0.095(6) 0.112(6) 0.054(5) 0.040(5) 0.007(5) C25 0.092(6) 0.065(5) 0.100(6) 0.035(4) 0.020(5) 0.020(4) C26 0.080(5) 0.077(5) 0.106(6) 0.018(4) 0.022(4) 0.025(4) C27 0.067(4) 0.060(4) 0.085(5) 0.018(3) 0.032(3) 0.020(3) C28 0.054(3) 0.061(3) 0.036(3) 0.006(2) 0.008(2) 0.007(3) C29 0.103(6) 0.095(5) 0.062(4) 0.020(4) 0.043(4) 0.050(4) C30 0.136(7) 0.135(7) 0.055(4) 0.024(5) 0.051(5) 0.045(6) C31 0.119(7) 0.126(7) 0.061(4) 0.049(5) 0.036(4) 0.044(6) C32 0.111(6) 0.110(6) 0.098(6) 0.053(5) 0.047(5) 0.053(5) C33 0.068(4) 0.072(4) 0.070(4) 0.024(3) 0.031(3) 0.024(3) C34 0.047(3) 0.053(3) 0.055(3) -0.015(3) 0.012(3) 0.002(3) C35 0.064(4) 0.047(3) 0.074(4) -0.009(3) 0.018(3) -0.005(3) C36 0.087(5) 0.051(4) 0.117(6) -0.013(4) 0.039(5) -0.008(4) C37 0.091(6) 0.079(6) 0.161(9) -0.056(6) 0.054(6) -0.029(5) C38 0.096(6) 0.110(7) 0.092(6) -0.053(5) -0.006(5) -0.015(5) C39 0.077(5) 0.078(5) 0.068(4) -0.027(4) -0.001(4) 0.003(4) C40 0.051(3) 0.052(3) 0.044(3) 0.006(3) 0.014(2) -0.009(3) C41 0.077(5) 0.076(5) 0.056(4) 0.010(3) 0.007(3) 0.009(4) C42 0.120(7) 0.113(7) 0.044(4) 0.008(4) -0.002(4) -0.015(6) C43 0.130(7) 0.098(6) 0.038(4) -0.007(4) 0.028(4) -0.047(5) C44 0.098(6) 0.091(5) 0.059(4) -0.023(4) 0.031(4) -0.027(4) C45 0.067(4) 0.064(4) 0.053(3) -0.006(3) 0.013(3) -0.012(3) C46 0.055(3) 0.041(3) 0.049(3) 0.003(2) 0.003(3) -0.002(3) C47 0.058(4) 0.045(3) 0.068(4) -0.008(3) 0.007(3) 0.006(3) C48 0.083(5) 0.056(4) 0.093(5) -0.007(4) 0.017(4) 0.018(4) C49 0.116(7) 0.055(5) 0.123(7) -0.002(5) 0.017(6) 0.025(5) C50 0.112(7) 0.049(4) 0.133(7) 0.022(4) 0.035(6) -0.002(4) C51 0.080(5) 0.043(3) 0.088(5) 0.022(3) 0.017(4) 0.000(3) C52 0.050(4) 0.058(4) 0.074(4) -0.013(3) 0.000(3) -0.007(3) C53 0.091(6) 0.078(5) 0.141(8) -0.018(5) 0.041(5) -0.032(5) C54 0.114(9) 0.070(6) 0.247(16) -0.016(9) 0.048(10) -0.036(6) C55 0.128(9) 0.091(8) 0.203(14) -0.056(10) -0.040(10) -0.027(7) C56 0.285(18) 0.091(8) 0.101(8) -0.038(7) -0.028(9) -0.011(9) C57 0.213(11) 0.072(5) 0.069(5) -0.026(4) 0.011(6) -0.035(6) C58 0.042(3) 0.056(4) 0.059(4) -0.008(3) -0.001(3) 0.002(3) C59 0.078(5) 0.092(5) 0.085(5) -0.021(4) 0.013(4) 0.025(4) C60 0.104(7) 0.092(7) 0.172(11) -0.022(7) 0.022(7) 0.047(6) C61 0.130(9) 0.089(7) 0.142(10) 0.012(7) -0.006(8) 0.037(6) C62 0.189(12) 0.078(6) 0.098(7) 0.019(5) 0.017(7) 0.013(7) C63 0.113(6) 0.062(4) 0.080(5) 0.004(4) 0.026(4) 0.010(4) C100 0.73(3) 0.58(3) 0.24(2) -0.24(2) 0.30(3) -0.560 Cl3 0.274(9) 0.149(5) 0.226(7) -0.050(5) 0.155(7) -0.048(6) Cl3' 0.244(14) 0.184(11) 0.36(2) -0.119(15) 0.146(16) -0.073(11) Cl4 0.23(3) 0.21(3) 0.143(16) -0.005(17) 0.077(17) -0.02(2) Cl4' 0.301(9) 0.178(5) 0.151(4) 0.042(4) 0.080(5) 0.003(5) C101 0.081(9) 0.27(2) 0.61(4) 0.26(3) -0.067(16) -0.001(12) Cl5 0.330(7) 0.211(5) 0.194(4) 0.038(4) -0.002(4) 0.024(5) Cl6 0.448(13) 0.361(10) 0.470(12) 0.276(10) -0.142(10) -0.190(10) C102 0.59(6) 0.195(19) 0.28(3) 0.12(2) 0.29(3) 0.06(3) O101 0.217(10) 0.234(14) 0.069(5) -0.015(6) -0.015(5) -0.099(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 Pd P4 2.1966(15) . ? Pd Cl2 2.3270(18) . ? Pd Cl1 2.3857(17) . ? Pd C7 2.409(6) . ? Pd Co4 2.6861(8) . ? Co1 C1 1.786(6) . ? Co1 C2 1.806(6) . ? Co1 C10 1.961(5) . ? Co1 C9 1.966(5) . ? Co1 P3 2.2274(14) . ? Co1 Co2 2.5020(10) . ? Co2 C3 1.769(7) . ? Co2 C4 1.787(7) . ? Co2 C10 1.950(5) . ? Co2 C9 1.996(5) . ? Co2 P5 2.1794(19) . ? Co3 C6 1.785(6) . ? Co3 C5 1.798(6) . ? Co3 C12 1.918(5) . ? Co3 C11 1.987(5) . ? Co3 P1 2.2816(15) . ? Co3 Co4 2.5468(9) . ? Co4 C7 1.806(6) . ? Co4 C8 1.828(7) . ? Co4 C11 1.995(5) . ? Co4 C12 2.057(5) . ? Co4 P2 2.2618(15) . ? P1 C9 1.794(5) . ? P1 C22 1.830(5) . ? P1 C16 1.824(5) . ? P2 C10 1.778(5) . ? P2 C34 1.831(6) . ? P2 C28 1.841(5) . ? P3 C11 1.796(5) . ? P3 C46 1.830(5) . ? P3 C40 1.843(5) . ? P4 C12 1.757(5) . ? P4 C52 1.813(6) . ? P4 C58 1.813(6) . ? P5 O10 1.507(8) . ? P5 O11 1.562(7) . ? P5 O9 1.540(9) . ? O1 C1 1.146(7) . ? O2 C2 1.131(6) . ? O3 C3 1.145(7) . ? O4 C4 1.150(8) . ? O5 C5 1.117(6) . ? O6 C6 1.141(7) . ? O7 C7 1.149(6) . ? O8 C8 1.136(7) . ? O9 C13 1.134(13) . ? O10 C14 1.349(14) . ? O11 C15 1.423(9) . ? C9 C10 1.362(7) . ? C11 C12 1.341(7) . ? C16 C21 1.352(8) . ? C16 C17 1.390(8) . ? C17 C18 1.371(10) . ? C18 C19 1.372(12) . ? C19 C20 1.379(11) . ? C20 C21 1.397(9) . ? C22 C23 1.367(8) . ? C22 C27 1.384(8) . ? C23 C24 1.397(9) . ? C24 C25 1.347(11) . ? C25 C26 1.367(10) . ? C26 C27 1.373(9) . ? C28 C33 1.349(8) . ? C28 C29 1.390(8) . ? C29 C30 1.375(9) . ? C30 C31 1.324(10) . ? C31 C32 1.362(10) . ? C32 C33 1.381(9) . ? C34 C35 1.381(8) . ? C34 C39 1.399(8) . ? C35 C36 1.367(8) . ? C36 C37 1.383(11) . ? C37 C38 1.403(12) . ? C38 C39 1.377(10) . ? C40 C45 1.368(8) . ? C40 C41 1.396(8) . ? C41 C42 1.388(9) . ? C42 C43 1.375(12) . ? C43 C44 1.357(11) . ? C44 C45 1.383(8) . ? C46 C47 1.380(8) . ? C46 C51 1.387(8) . ? C47 C48 1.384(8) . ? C48 C49 1.359(11) . ? C49 C50 1.359(12) . ? C50 C51 1.384(10) . ? C52 C57 1.352(10) . ? C52 C53 1.374(10) . ? C53 C54 1.375(13) . ? C54 C55 1.370(17) . ? C55 C56 1.322(18) . ? C56 C57 1.389(12) . ? C58 C63 1.366(9) . ? C58 C59 1.391(9) . ? C59 C60 1.394(12) . ? C60 C61 1.342(14) . ? C61 C62 1.363(14) . ? C62 C63 1.420(11) . ? C100 Cl4 1.48(3) . ? C100 Cl3 1.57(2) . ? C100 Cl3' 1.49(4) . ? C100 Cl4' 1.83(3) . ? Cl3 Cl3' 1.85(2) . ? Cl3' Cl4 1.43(3) . ? Cl4 Cl4' 1.34(3) . ? C101 Cl6 1.449(16) . ? C101 Cl5 1.89(2) . ? C102 O101 1.05(4) . ? C102 C102 1.65(5) 3_656 ? 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 P4 Pd Cl2 89.10(7) . . ? P4 Pd Cl1 176.92(7) . . ? Cl2 Pd Cl1 92.97(7) . . ? P4 Pd C7 94.46(13) . . ? Cl2 Pd C7 144.11(15) . . ? Cl1 Pd C7 85.20(13) . . ? P4 Pd Co4 76.35(4) . . ? Cl2 Pd Co4 165.39(6) . . ? Cl1 Pd Co4 101.52(5) . . ? C7 Pd Co4 41.08(14) . . ? C1 Co1 C2 97.6(3) . . ? C1 Co1 C10 147.6(2) . . ? C2 Co1 C10 105.5(2) . . ? C1 Co1 C9 109.2(2) . . ? C2 Co1 C9 142.5(2) . . ? C10 Co1 C9 40.6(2) . . ? C1 Co1 P3 97.19(19) . . ? C2 Co1 P3 99.84(19) . . ? C10 Co1 P3 100.76(15) . . ? C9 Co1 P3 102.17(14) . . ? C1 Co1 Co2 105.46(19) . . ? C2 Co1 Co2 97.03(18) . . ? C10 Co1 Co2 50.05(14) . . ? C9 Co1 Co2 51.38(14) . . ? P3 Co1 Co2 149.57(5) . . ? C3 Co2 C4 96.2(4) . . ? C3 Co2 C10 108.8(3) . . ? C4 Co2 C10 104.8(3) . . ? C3 Co2 C9 107.9(3) . . ? C4 Co2 C9 142.3(3) . . ? C10 Co2 C9 40.4(2) . . ? C3 Co2 P5 90.6(2) . . ? C4 Co2 P5 96.1(2) . . ? C10 Co2 P5 149.29(16) . . ? C9 Co2 P5 111.79(16) . . ? C3 Co2 Co1 156.8(2) . . ? C4 Co2 Co1 99.5(2) . . ? C10 Co2 Co1 50.41(14) . . ? C9 Co2 Co1 50.30(14) . . ? P5 Co2 Co1 104.59(6) . . ? C6 Co3 C5 94.2(3) . . ? C6 Co3 C12 108.7(2) . . ? C5 Co3 C12 96.7(2) . . ? C6 Co3 C11 143.8(2) . . ? C5 Co3 C11 105.7(2) . . ? C12 Co3 C11 40.1(2) . . ? C6 Co3 P1 103.8(2) . . ? C5 Co3 P1 96.40(19) . . ? C12 Co3 P1 143.70(15) . . ? C11 Co3 P1 103.62(14) . . ? C6 Co3 Co4 98.7(2) . . ? C5 Co3 Co4 149.20(19) . . ? C12 Co3 Co4 52.61(14) . . ? C11 Co3 Co4 50.37(14) . . ? P1 Co3 Co4 107.36(4) . . ? C7 Co4 C8 105.4(3) . . ? C7 Co4 C11 111.9(2) . . ? C8 Co4 C11 140.4(2) . . ? C7 Co4 C12 107.7(2) . . ? C8 Co4 C12 117.0(2) . . ? C11 Co4 C12 38.63(19) . . ? C7 Co4 P2 93.58(18) . . ? C8 Co4 P2 95.40(19) . . ? C11 Co4 P2 94.94(14) . . ? C12 Co4 P2 133.19(14) . . ? C7 Co4 Co3 155.47(17) . . ? C8 Co4 Co3 90.29(19) . . ? C11 Co4 Co3 50.09(14) . . ? C12 Co4 Co3 47.79(13) . . ? P2 Co4 Co3 103.74(4) . . ? C7 Co4 Pd 61.20(18) . . ? C8 Co4 Pd 73.36(19) . . ? C11 Co4 Pd 113.84(14) . . ? C12 Co4 Pd 78.16(14) . . ? P2 Co4 Pd 146.76(5) . . ? Co3 Co4 Pd 107.42(3) . . ? C9 P1 C22 104.4(2) . . ? C9 P1 C16 109.7(3) . . ? C22 P1 C16 98.8(3) . . ? C9 P1 Co3 109.62(17) . . ? C22 P1 Co3 120.55(19) . . ? C16 P1 Co3 112.92(18) . . ? C10 P2 C34 102.5(2) . . ? C10 P2 C28 110.9(2) . . ? C34 P2 C28 101.5(3) . . ? C10 P2 Co4 113.22(17) . . ? C34 P2 Co4 120.48(18) . . ? C28 P2 Co4 107.62(19) . . ? C11 P3 C46 107.9(2) . . ? C11 P3 C40 101.5(2) . . ? C46 P3 C40 100.4(2) . . ? C11 P3 Co1 110.91(16) . . ? C46 P3 Co1 116.17(18) . . ? C40 P3 Co1 118.32(19) . . ? C12 P4 C52 106.1(3) . . ? C12 P4 C58 110.8(3) . . ? C52 P4 C58 109.5(3) . . ? C12 P4 Pd 99.45(16) . . ? C52 P4 Pd 115.3(2) . . ? C58 P4 Pd 114.9(2) . . ? O10 P5 O11 99.3(6) . . ? O10 P5 O9 102.6(6) . . ? O11 P5 O9 104.5(5) . . ? O10 P5 Co2 123.1(3) . . ? O11 P5 Co2 114.0(2) . . ? O9 P5 Co2 111.3(4) . . ? C13 O9 P5 161.2(14) . . ? C14 O10 P5 131.1(12) . . ? C15 O11 P5 128.8(7) . . ? O1 C1 Co1 176.9(6) . . ? O2 C2 Co1 175.4(6) . . ? O3 C3 Co2 174.8(7) . . ? O4 C4 Co2 179.3(8) . . ? O5 C5 Co3 173.8(6) . . ? O6 C6 Co3 177.4(6) . . ? O7 C7 Co4 168.8(5) . . ? O7 C7 Pd 113.4(4) . . ? Co4 C7 Pd 77.7(2) . . ? O8 C8 Co4 174.9(6) . . ? C10 C9 P1 127.2(4) . . ? C10 C9 Co1 69.5(3) . . ? P1 C9 Co1 133.2(3) . . ? C10 C9 Co2 68.0(3) . . ? P1 C9 Co2 146.5(3) . . ? Co1 C9 Co2 78.32(18) . . ? C9 C10 P2 138.0(4) . . ? C9 C10 Co2 71.6(3) . . ? P2 C10 Co2 142.0(3) . . ? C9 C10 Co1 69.9(3) . . ? P2 C10 Co1 127.3(3) . . ? Co2 C10 Co1 79.55(19) . . ? C12 C11 P3 145.1(4) . . ? C12 C11 Co3 67.2(3) . . ? P3 C11 Co3 126.2(3) . . ? C12 C11 Co4 73.2(3) . . ? P3 C11 Co4 136.6(3) . . ? Co3 C11 Co4 79.53(17) . . ? C11 C12 P4 152.7(4) . . ? C11 C12 Co3 72.7(3) . . ? P4 C12 Co3 133.7(3) . . ? C11 C12 Co4 68.2(3) . . ? P4 C12 Co4 105.5(2) . . ? Co3 C12 Co4 79.60(17) . . ? C21 C16 C17 118.6(6) . . ? C21 C16 P1 124.1(4) . . ? C17 C16 P1 117.3(5) . . ? C18 C17 C16 121.3(7) . . ? C17 C18 C19 120.1(8) . . ? C18 C19 C20 119.2(7) . . ? C19 C20 C21 120.0(8) . . ? C16 C21 C20 120.8(7) . . ? C23 C22 C27 117.0(5) . . ? C23 C22 P1 123.0(5) . . ? C27 C22 P1 119.9(4) . . ? C22 C23 C24 121.3(7) . . ? C25 C24 C23 120.2(7) . . ? C24 C25 C26 119.7(7) . . ? C25 C26 C27 120.1(7) . . ? C22 C27 C26 121.7(6) . . ? C33 C28 C29 118.9(5) . . ? C33 C28 P2 124.0(5) . . ? C29 C28 P2 116.9(4) . . ? C30 C29 C28 120.1(6) . . ? C31 C30 C29 121.0(7) . . ? C30 C31 C32 119.1(7) . . ? C33 C32 C31 121.6(7) . . ? C28 C33 C32 119.3(6) . . ? C35 C34 C39 119.6(6) . . ? C35 C34 P2 121.4(4) . . ? C39 C34 P2 118.7(5) . . ? C34 C35 C36 121.4(6) . . ? C37 C36 C35 119.6(8) . . ? C36 C37 C38 119.8(7) . . ? C37 C38 C39 120.3(7) . . ? C34 C39 C38 119.3(7) . . ? C45 C40 C41 119.2(5) . . ? C45 C40 P3 120.4(4) . . ? C41 C40 P3 120.3(5) . . ? C40 C41 C42 120.1(7) . . ? C43 C42 C41 118.9(7) . . ? C44 C43 C42 121.3(7) . . ? C43 C44 C45 119.9(7) . . ? C40 C45 C44 120.5(6) . . ? C47 C46 C51 119.5(6) . . ? C47 C46 P3 123.5(4) . . ? C51 C46 P3 117.0(5) . . ? C46 C47 C48 120.7(6) . . ? C49 C48 C47 119.0(8) . . ? C50 C49 C48 121.5(7) . . ? C49 C50 C51 120.4(8) . . ? C50 C51 C46 119.0(7) . . ? C57 C52 C53 119.0(7) . . ? C57 C52 P4 121.4(6) . . ? C53 C52 P4 119.5(6) . . ? C54 C53 C52 121.0(10) . . ? C53 C54 C55 118.4(11) . . ? C56 C55 C54 120.8(11) . . ? C55 C56 C57 120.9(12) . . ? C52 C57 C56 119.6(10) . . ? C63 C58 C59 118.8(7) . . ? C63 C58 P4 122.0(5) . . ? C59 C58 P4 119.2(5) . . ? C60 C59 C58 119.3(8) . . ? C59 C60 C61 121.8(9) . . ? C60 C61 C62 120.1(10) . . ? C61 C62 C63 119.3(10) . . ? C58 C63 C62 120.7(8) . . ? Cl4 C100 Cl3 115.4(19) . . ? Cl4 C100 Cl3' 58(2) . . ? Cl3 C100 Cl3' 74.2(16) . . ? Cl4 C100 Cl4' 46.3(15) . . ? Cl3 C100 Cl4' 118.9(14) . . ? Cl3' C100 Cl4' 100.5(16) . . ? C100 Cl3 Cl3' 50.9(17) . . ? Cl4 Cl3' C100 60.7(14) . . ? Cl4 Cl3' Cl3 102.9(16) . . ? C100 Cl3' Cl3 54.9(13) . . ? Cl4' Cl4 Cl3' 136(2) . . ? Cl4' Cl4 C100 81(3) . . ? Cl3' Cl4 C100 61.8(19) . . ? Cl4 Cl4' C100 52.9(17) . . ? Cl6 C101 Cl5 102.1(12) . . ? O101 C102 C102 102(3) . 3_656 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.811 _refine_diff_density_min -0.627 _refine_diff_density_rms 0.110 data_hong158m _database_code_CSD 209744 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C56 H44 Cl4 Co2 O5 P4 Pd' _chemical_formula_weight 1286.85 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' Co Co 0.3494 0.9721 '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 11.1922(8) _cell_length_b 13.1178(9) _cell_length_c 19.4159(14) _cell_angle_alpha 94.9880(10) _cell_angle_beta 100.917(2) _cell_angle_gamma 101.4100(10) _cell_volume 2720.7(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 7517 _cell_measurement_theta_min 2.198 _cell_measurement_theta_max 26.014 _exptl_crystal_description parallelepiped _exptl_crystal_colour red-brown _exptl_crystal_size_max 0.64 _exptl_crystal_size_mid 0.54 _exptl_crystal_size_min 0.33 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.571 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1296 _exptl_absorpt_coefficient_mu 1.291 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.574474 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15536 _diffrn_reflns_av_R_equivalents 0.0225 _diffrn_reflns_av_sigmaI/netI 0.0369 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.81 _diffrn_reflns_theta_max 26.04 _reflns_number_total 10576 _reflns_number_gt 8214 _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^)+(0.0705P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10576 _refine_ls_number_parameters 657 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0542 _refine_ls_R_factor_gt 0.0385 _refine_ls_wR_factor_ref 0.1096 _refine_ls_wR_factor_gt 0.0993 _refine_ls_goodness_of_fit_ref 0.983 _refine_ls_restrained_S_all 0.983 _refine_ls_shift/su_max 0.045 _refine_ls_shift/su_mean 0.002 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 Pd Pd 0.58144(2) 0.836680(19) 0.172953(14) 0.03847(9) Uani 1 1 d . . . Co1 Co 0.25552(4) 0.61794(3) 0.20245(2) 0.03439(11) Uani 1 1 d . . . Co2 Co 0.48822(4) 0.67166(3) 0.22803(2) 0.03149(11) Uani 1 1 d . . . Cl1 Cl 0.77198(9) 0.78751(7) 0.15947(5) 0.0520(2) Uani 1 1 d . . . Cl2 Cl 0.63033(10) 0.99758(8) 0.13119(6) 0.0643(3) Uani 1 1 d . . . P1 P 0.37115(8) 0.69523(6) 0.38117(4) 0.03714(19) Uani 1 1 d . . . P2 P 0.40817(8) 0.87016(6) 0.19847(5) 0.03513(19) Uani 1 1 d . . . P3 P 0.24942(8) 0.44872(6) 0.21459(4) 0.03611(19) Uani 1 1 d . . . P4 P 0.52767(8) 0.51709(6) 0.25590(4) 0.03144(17) Uani 1 1 d . . . O1 O 0.1690(3) 0.6165(3) 0.04964(15) 0.0746(9) Uani 1 1 d . . . O2 O 0.0094(3) 0.6146(3) 0.2334(2) 0.0906(11) Uani 1 1 d . . . O3 O 0.7202(3) 0.7888(2) 0.32388(14) 0.0561(7) Uani 1 1 d . . . O4 O 0.4784(2) 0.6264(2) 0.07550(12) 0.0520(6) Uani 1 1 d . . . O5 O 0.3607(2) 0.58826(17) 0.40192(12) 0.0449(6) Uani 1 1 d . . . C1 C 0.3700(3) 0.6972(2) 0.28902(16) 0.0337(7) Uani 1 1 d . . . C2 C 0.3549(3) 0.7563(2) 0.23596(16) 0.0344(7) Uani 1 1 d . . . C3 C 0.2441(3) 0.7530(3) 0.39904(18) 0.0416(8) Uani 1 1 d . . . C4 C 0.1799(5) 0.8074(4) 0.3545(2) 0.0685(13) Uani 1 1 d . . . H4A H 0.2034 0.8194 0.3119 0.082 Uiso 1 1 calc R . . C5 C 0.0810(5) 0.8452(4) 0.3709(3) 0.0873(16) Uani 1 1 d . . . H5B H 0.0382 0.8818 0.3395 0.105 Uiso 1 1 calc R . . C6 C 0.0459(5) 0.8289(4) 0.4334(3) 0.0749(14) Uani 1 1 d . . . H6A H -0.0218 0.8533 0.4442 0.090 Uiso 1 1 calc R . . C7 C 0.1096(4) 0.7775(3) 0.4792(3) 0.0679(12) Uani 1 1 d . . . H7A H 0.0867 0.7681 0.5222 0.082 Uiso 1 1 calc R . . C8 C 0.2094(4) 0.7381(3) 0.4633(2) 0.0538(10) Uani 1 1 d . . . H8A H 0.2525 0.7023 0.4952 0.065 Uiso 1 1 calc R . . C9 C 0.5125(3) 0.7814(3) 0.43132(18) 0.0438(8) Uani 1 1 d . . . C10 C 0.6028(4) 0.7356(3) 0.4676(2) 0.0617(11) Uani 1 1 d . . . H10A H 0.5884 0.6630 0.4655 0.074 Uiso 1 1 calc R . . C11 C 0.7140(5) 0.7966(4) 0.5068(3) 0.0805(14) Uani 1 1 d . . . H11A H 0.7744 0.7654 0.5308 0.097 Uiso 1 1 calc R . . C12 C 0.7339(5) 0.9029(5) 0.5098(3) 0.0852(16) Uani 1 1 d . . . H12A H 0.8087 0.9442 0.5360 0.102 Uiso 1 1 calc R . . C13 C 0.6466(5) 0.9499(4) 0.4751(3) 0.0770(14) Uani 1 1 d . . . H13A H 0.6618 1.0226 0.4779 0.092 Uiso 1 1 calc R . . C14 C 0.5350(4) 0.8891(3) 0.4357(2) 0.0566(10) Uani 1 1 d . . . H14A H 0.4751 0.9212 0.4121 0.068 Uiso 1 1 calc R . . C15 C 0.2822(3) 0.8756(2) 0.12583(17) 0.0386(7) Uani 1 1 d . . . C16 C 0.3083(4) 0.8987(3) 0.06090(19) 0.0458(8) Uani 1 1 d . . . H16A H 0.3902 0.9128 0.0549 0.055 Uiso 1 1 calc R . . C17 C 0.2114(4) 0.9006(3) 0.0056(2) 0.0580(10) Uani 1 1 d . . . H17A H 0.2284 0.9152 -0.0381 0.070 Uiso 1 1 calc R . . C18 C 0.0902(4) 0.8811(3) 0.0140(2) 0.0619(11) Uani 1 1 d . . . H18A H 0.0259 0.8826 -0.0237 0.074 Uiso 1 1 calc R . . C19 C 0.0637(4) 0.8591(3) 0.0790(2) 0.0572(10) Uani 1 1 d . . . H19A H -0.0182 0.8465 0.0851 0.069 Uiso 1 1 calc R . . C20 C 0.1601(3) 0.8560(3) 0.1342(2) 0.0476(8) Uani 1 1 d . . . H20A H 0.1427 0.8406 0.1776 0.057 Uiso 1 1 calc R . . C21 C 0.4356(3) 0.9885(2) 0.26087(18) 0.0403(8) Uani 1 1 d . . . C22 C 0.3405(4) 1.0358(3) 0.2721(2) 0.0657(12) Uani 1 1 d . . . H22A H 0.2597 1.0076 0.2467 0.079 Uiso 1 1 calc R . . C23 C 0.3635(6) 1.1250(4) 0.3207(3) 0.0816(15) Uani 1 1 d . . . H23A H 0.2983 1.1556 0.3287 0.098 Uiso 1 1 calc R . . C24 C 0.4827(6) 1.1675(4) 0.3568(3) 0.0791(15) Uani 1 1 d . . . H24A H 0.4984 1.2271 0.3896 0.095 Uiso 1 1 calc R . . C25 C 0.5786(5) 1.1239(4) 0.3454(3) 0.0765(14) Uani 1 1 d . . . H25A H 0.6597 1.1547 0.3691 0.092 Uiso 1 1 calc R . . C26 C 0.5553(4) 1.0332(3) 0.2981(2) 0.0669(12) Uani 1 1 d . . . H26A H 0.6208 1.0022 0.2915 0.080 Uiso 1 1 calc R . . C27 C 0.2052(4) 0.6155(3) 0.1079(2) 0.0480(9) Uani 1 1 d . . . C28 C 0.1054(4) 0.6170(3) 0.2225(2) 0.0530(9) Uani 1 1 d . . . C29 C 0.6339(3) 0.7475(2) 0.28325(18) 0.0399(7) Uani 1 1 d . . . C30 C 0.4907(3) 0.6511(3) 0.13510(19) 0.0410(8) Uani 1 1 d . . . C31 C 0.1201(3) 0.3877(3) 0.2529(2) 0.0439(8) Uani 1 1 d . . . C32 C 0.0040(4) 0.3532(4) 0.2094(3) 0.0696(13) Uani 1 1 d . . . H32A H -0.0059 0.3540 0.1608 0.084 Uiso 1 1 calc R . . C33 C -0.0994(4) 0.3167(4) 0.2388(3) 0.0848(16) Uani 1 1 d . . . H33A H -0.1779 0.2935 0.2094 0.102 Uiso 1 1 calc R . . C34 C -0.0865(5) 0.3149(4) 0.3087(3) 0.0761(14) Uani 1 1 d . . . H34A H -0.1560 0.2916 0.3276 0.091 Uiso 1 1 calc R . . C35 C 0.0275(5) 0.3468(4) 0.3519(3) 0.0789(15) Uani 1 1 d . . . H35A H 0.0362 0.3441 0.4002 0.095 Uiso 1 1 calc R . . C36 C 0.1327(4) 0.3839(3) 0.3245(2) 0.0634(11) Uani 1 1 d . . . H36A H 0.2107 0.4060 0.3545 0.076 Uiso 1 1 calc R . . C37 C 0.2443(3) 0.3521(3) 0.13965(17) 0.0391(7) Uani 1 1 d . . . C38 C 0.2219(4) 0.2464(3) 0.1478(2) 0.0515(9) Uani 1 1 d . . . H38A H 0.2001 0.2250 0.1891 0.062 Uiso 1 1 calc R . . C39 C 0.2319(4) 0.1728(3) 0.0953(2) 0.0578(10) Uani 1 1 d . . . H39A H 0.2179 0.1023 0.1017 0.069 Uiso 1 1 calc R . . C40 C 0.2623(4) 0.2028(3) 0.0336(2) 0.0610(11) Uani 1 1 d . . . H40A H 0.2681 0.1528 -0.0018 0.073 Uiso 1 1 calc R . . C41 C 0.2840(4) 0.3071(3) 0.0246(2) 0.0582(10) Uani 1 1 d . . . H41A H 0.3047 0.3278 -0.0170 0.070 Uiso 1 1 calc R . . C42 C 0.2751(4) 0.3820(3) 0.07796(19) 0.0493(9) Uani 1 1 d . . . H42A H 0.2901 0.4526 0.0717 0.059 Uiso 1 1 calc R . . C43 C 0.6504(3) 0.5199(2) 0.33336(17) 0.0366(7) Uani 1 1 d . . . C44 C 0.6258(4) 0.4891(3) 0.39672(18) 0.0483(9) Uani 1 1 d . . . H44A H 0.5440 0.4639 0.4007 0.058 Uiso 1 1 calc R . . C45 C 0.7239(4) 0.4960(3) 0.4545(2) 0.0601(11) Uani 1 1 d . . . H45A H 0.7074 0.4768 0.4973 0.072 Uiso 1 1 calc R . . C46 C 0.8429(4) 0.5308(4) 0.4481(2) 0.0677(12) Uani 1 1 d . . . H46A H 0.9080 0.5350 0.4867 0.081 Uiso 1 1 calc R . . C47 C 0.8688(4) 0.5598(3) 0.3860(2) 0.0632(11) Uani 1 1 d . . . H47A H 0.9511 0.5823 0.3820 0.076 Uiso 1 1 calc R . . C48 C 0.7726(3) 0.5558(3) 0.32867(19) 0.0487(9) Uani 1 1 d . . . H48A H 0.7905 0.5774 0.2867 0.058 Uiso 1 1 calc R . . C49 C 0.5766(3) 0.4383(2) 0.18894(16) 0.0374(7) Uani 1 1 d . . . C50 C 0.5430(3) 0.3299(3) 0.1790(2) 0.0496(9) Uani 1 1 d . . . H50A H 0.4938 0.2951 0.2071 0.059 Uiso 1 1 calc R . . C51 C 0.5824(4) 0.2727(3) 0.1274(2) 0.0640(12) Uani 1 1 d . . . H51A H 0.5580 0.2000 0.1202 0.077 Uiso 1 1 calc R . . C52 C 0.6574(5) 0.3234(4) 0.0869(2) 0.0742(14) Uani 1 1 d . . . H52A H 0.6830 0.2849 0.0521 0.089 Uiso 1 1 calc R . . C53 C 0.6945(5) 0.4300(4) 0.0973(2) 0.0670(12) Uani 1 1 d . . . H53A H 0.7466 0.4638 0.0703 0.080 Uiso 1 1 calc R . . C54 C 0.6549(4) 0.4884(3) 0.14810(18) 0.0474(9) Uani 1 1 d . . . H54A H 0.6806 0.5611 0.1550 0.057 Uiso 1 1 calc R . . C55 C 0.3887(3) 0.4383(3) 0.27651(18) 0.0365(7) Uani 1 1 d . . . H55A H 0.384(3) 0.470(3) 0.318(2) 0.045(10) Uiso 1 1 d . . . H55B H 0.389(3) 0.367(3) 0.2767(18) 0.046(10) Uiso 1 1 d . . . C100 C -0.1066(5) 1.0354(4) 0.2708(3) 0.0842(15) Uani 1 1 d . . . H10B H -0.1449 0.9624 0.2536 0.101 Uiso 1 1 calc R . . H10C H -0.1623 1.0773 0.2494 0.101 Uiso 1 1 calc R . . Cl3 Cl 0.03036(19) 1.06660(15) 0.24296(16) 0.1620(10) Uani 1 1 d . . . Cl4 Cl -0.09347(18) 1.05404(13) 0.36101(10) 0.1134(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd 0.04165(16) 0.03786(14) 0.04263(16) 0.01327(11) 0.02021(12) 0.01025(11) Co1 0.0380(2) 0.0355(2) 0.0322(2) 0.00873(17) 0.01057(18) 0.00913(18) Co2 0.0381(2) 0.0313(2) 0.0282(2) 0.00692(16) 0.01205(18) 0.00874(17) Cl1 0.0465(5) 0.0571(5) 0.0575(6) 0.0021(4) 0.0249(4) 0.0123(4) Cl2 0.0645(6) 0.0556(5) 0.0845(8) 0.0393(5) 0.0314(6) 0.0123(5) P1 0.0497(5) 0.0371(4) 0.0287(4) 0.0061(3) 0.0160(4) 0.0109(4) P2 0.0408(5) 0.0331(4) 0.0366(5) 0.0108(3) 0.0155(4) 0.0106(3) P3 0.0386(5) 0.0355(4) 0.0345(4) 0.0081(3) 0.0095(4) 0.0056(3) P4 0.0368(4) 0.0317(4) 0.0269(4) 0.0046(3) 0.0080(3) 0.0084(3) O1 0.104(3) 0.086(2) 0.0349(16) 0.0094(14) 0.0022(15) 0.0346(19) O2 0.059(2) 0.099(3) 0.129(3) 0.018(2) 0.046(2) 0.0277(18) O3 0.0550(17) 0.0568(15) 0.0470(16) 0.0000(12) 0.0035(13) 0.0000(13) O4 0.0638(17) 0.0637(16) 0.0293(14) 0.0065(11) 0.0133(12) 0.0125(13) O5 0.0627(16) 0.0411(12) 0.0349(13) 0.0099(10) 0.0173(11) 0.0119(11) C1 0.0428(18) 0.0321(15) 0.0304(16) 0.0047(12) 0.0158(14) 0.0105(13) C2 0.0395(18) 0.0350(15) 0.0339(17) 0.0062(13) 0.0148(14) 0.0126(13) C3 0.046(2) 0.0401(17) 0.0414(19) 0.0016(15) 0.0179(16) 0.0076(15) C4 0.091(3) 0.079(3) 0.060(3) 0.023(2) 0.041(3) 0.047(3) C5 0.103(4) 0.099(4) 0.088(4) 0.028(3) 0.036(3) 0.066(3) C6 0.071(3) 0.071(3) 0.097(4) 0.002(3) 0.042(3) 0.028(2) C7 0.076(3) 0.068(3) 0.066(3) 0.001(2) 0.044(3) 0.006(2) C8 0.066(3) 0.058(2) 0.043(2) 0.0069(17) 0.0246(19) 0.0142(19) C9 0.046(2) 0.051(2) 0.0335(18) -0.0032(15) 0.0129(15) 0.0087(16) C10 0.067(3) 0.063(3) 0.052(2) -0.0046(19) 0.005(2) 0.022(2) C11 0.065(3) 0.101(4) 0.067(3) -0.009(3) -0.006(2) 0.025(3) C12 0.063(3) 0.102(4) 0.072(3) -0.020(3) 0.004(3) -0.004(3) C13 0.079(4) 0.057(3) 0.081(3) -0.010(2) 0.017(3) -0.010(2) C14 0.060(3) 0.050(2) 0.060(3) 0.0064(18) 0.016(2) 0.0097(18) C15 0.047(2) 0.0345(16) 0.0382(18) 0.0101(14) 0.0129(15) 0.0113(14) C16 0.051(2) 0.0489(19) 0.042(2) 0.0103(16) 0.0180(17) 0.0133(16) C17 0.070(3) 0.070(3) 0.037(2) 0.0135(18) 0.0151(19) 0.018(2) C18 0.059(3) 0.074(3) 0.049(2) 0.014(2) -0.0020(19) 0.017(2) C19 0.046(2) 0.064(2) 0.063(3) 0.013(2) 0.0084(19) 0.0144(18) C20 0.054(2) 0.051(2) 0.045(2) 0.0153(16) 0.0180(17) 0.0180(17) C21 0.052(2) 0.0322(16) 0.0394(19) 0.0104(14) 0.0141(16) 0.0093(14) C22 0.076(3) 0.067(3) 0.056(3) -0.007(2) 0.004(2) 0.035(2) C23 0.106(4) 0.076(3) 0.068(3) -0.013(2) 0.007(3) 0.052(3) C24 0.124(5) 0.053(3) 0.059(3) -0.003(2) 0.020(3) 0.021(3) C25 0.077(3) 0.063(3) 0.075(3) -0.017(2) 0.018(3) -0.011(2) C26 0.063(3) 0.057(2) 0.079(3) -0.004(2) 0.025(2) 0.005(2) C27 0.055(2) 0.050(2) 0.041(2) 0.0090(16) 0.0103(17) 0.0162(17) C28 0.051(2) 0.054(2) 0.059(2) 0.0148(18) 0.0182(19) 0.0145(18) C29 0.048(2) 0.0367(17) 0.0399(19) 0.0079(14) 0.0174(16) 0.0106(15) C30 0.0425(19) 0.0441(18) 0.041(2) 0.0124(15) 0.0124(15) 0.0129(15) C31 0.042(2) 0.0363(17) 0.057(2) 0.0134(16) 0.0184(17) 0.0065(14) C32 0.039(2) 0.096(3) 0.074(3) 0.041(3) 0.006(2) 0.008(2) C33 0.038(2) 0.110(4) 0.111(4) 0.055(3) 0.013(2) 0.012(2) C34 0.061(3) 0.071(3) 0.110(4) 0.033(3) 0.048(3) 0.010(2) C35 0.078(4) 0.085(3) 0.069(3) 0.002(3) 0.038(3) -0.012(3) C36 0.065(3) 0.066(3) 0.052(2) 0.005(2) 0.023(2) -0.011(2) C37 0.0394(18) 0.0403(17) 0.0340(18) 0.0021(14) 0.0034(14) 0.0052(14) C38 0.063(3) 0.0435(19) 0.043(2) 0.0059(16) 0.0066(18) 0.0043(17) C39 0.068(3) 0.0361(19) 0.059(3) -0.0037(17) 0.001(2) 0.0050(17) C40 0.060(3) 0.064(3) 0.051(2) -0.015(2) 0.0027(19) 0.012(2) C41 0.071(3) 0.064(3) 0.039(2) 0.0000(18) 0.0136(19) 0.014(2) C42 0.058(2) 0.048(2) 0.041(2) 0.0041(16) 0.0125(17) 0.0092(17) C43 0.0438(19) 0.0335(16) 0.0328(17) 0.0035(13) 0.0061(14) 0.0116(14) C44 0.059(2) 0.053(2) 0.0374(19) 0.0126(16) 0.0116(17) 0.0200(18) C45 0.080(3) 0.071(3) 0.035(2) 0.0159(18) 0.0062(19) 0.033(2) C46 0.072(3) 0.082(3) 0.044(2) -0.005(2) -0.012(2) 0.034(2) C47 0.042(2) 0.077(3) 0.062(3) -0.004(2) 0.0004(19) 0.010(2) C48 0.047(2) 0.059(2) 0.0367(19) 0.0028(16) 0.0048(16) 0.0092(17) C49 0.0454(19) 0.0392(17) 0.0287(16) 0.0003(13) 0.0041(14) 0.0168(14) C50 0.046(2) 0.046(2) 0.054(2) -0.0032(17) 0.0029(17) 0.0145(16) C51 0.072(3) 0.052(2) 0.063(3) -0.016(2) -0.003(2) 0.029(2) C52 0.095(4) 0.092(4) 0.044(2) -0.013(2) 0.009(2) 0.056(3) C53 0.086(3) 0.088(3) 0.047(2) 0.014(2) 0.029(2) 0.047(3) C54 0.060(2) 0.053(2) 0.0380(19) 0.0080(16) 0.0169(17) 0.0240(18) C55 0.0439(19) 0.0339(17) 0.0314(18) 0.0055(14) 0.0089(14) 0.0070(14) C100 0.065(3) 0.072(3) 0.110(4) -0.008(3) 0.022(3) 0.007(2) Cl3 0.1152(15) 0.1141(13) 0.294(3) 0.0442(16) 0.1271(19) 0.0252(11) Cl4 0.1421(15) 0.0909(10) 0.1132(13) 0.0019(9) 0.0194(11) 0.0517(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 Pd P2 2.2050(9) . ? Pd Cl2 2.3282(9) . ? Pd Cl1 2.3997(9) . ? Pd C30 2.434(3) . ? Pd C29 2.556(3) . ? Pd Co2 2.6171(5) . ? Co1 C28 1.793(4) . ? Co1 C27 1.810(4) . ? Co1 C2 1.917(3) . ? Co1 C1 1.975(3) . ? Co1 P3 2.2416(9) . ? Co1 Co2 2.4999(6) . ? Co2 C30 1.807(4) . ? Co2 C29 1.819(4) . ? Co2 C1 1.991(3) . ? Co2 C2 2.049(3) . ? Co2 P4 2.2480(9) . ? P1 O5 1.482(2) . ? P1 C1 1.789(3) . ? P1 C9 1.802(4) . ? P1 C3 1.813(3) . ? P2 C2 1.766(3) . ? P2 C15 1.813(4) . ? P2 C21 1.821(3) . ? P3 C55 1.816(4) . ? P3 C37 1.829(3) . ? P3 C31 1.828(3) . ? P4 C49 1.822(3) . ? P4 C43 1.827(3) . ? P4 C55 1.822(3) . ? O1 C27 1.130(4) . ? O2 C28 1.129(5) . ? O3 C29 1.131(4) . ? O4 C30 1.149(4) . ? C1 C2 1.348(4) . ? C3 C4 1.359(5) . ? C3 C8 1.392(5) . ? C4 C5 1.376(6) . ? C5 C6 1.365(7) . ? C6 C7 1.346(7) . ? C7 C8 1.394(6) . ? C9 C14 1.378(5) . ? C9 C10 1.386(6) . ? C10 C11 1.381(6) . ? C11 C12 1.363(7) . ? C12 C13 1.359(7) . ? C13 C14 1.385(6) . ? C15 C20 1.383(5) . ? C15 C16 1.392(4) . ? C16 C17 1.380(5) . ? C17 C18 1.374(6) . ? C18 C19 1.391(5) . ? C19 C20 1.379(5) . ? C21 C22 1.375(5) . ? C21 C26 1.382(6) . ? C22 C23 1.388(6) . ? C23 C24 1.367(7) . ? C24 C25 1.357(7) . ? C25 C26 1.386(6) . ? C31 C32 1.376(5) . ? C31 C36 1.376(5) . ? C32 C33 1.406(6) . ? C33 C34 1.341(7) . ? C34 C35 1.352(7) . ? C35 C36 1.400(6) . ? C37 C42 1.376(5) . ? C37 C38 1.389(5) . ? C38 C39 1.377(5) . ? C39 C40 1.375(6) . ? C40 C41 1.374(6) . ? C41 C42 1.396(5) . ? C43 C48 1.379(5) . ? C43 C44 1.387(5) . ? C44 C45 1.396(5) . ? C45 C46 1.353(6) . ? C46 C47 1.362(6) . ? C47 C48 1.383(5) . ? C49 C50 1.383(5) . ? C49 C54 1.398(5) . ? C50 C51 1.390(5) . ? C51 C52 1.372(7) . ? C52 C53 1.363(7) . ? C53 C54 1.386(5) . ? C100 Cl3 1.707(5) . ? C100 Cl4 1.721(6) . ? 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 P2 Pd Cl2 92.04(3) . . ? P2 Pd Cl1 171.98(3) . . ? Cl2 Pd Cl1 94.58(4) . . ? P2 Pd C30 93.74(8) . . ? Cl2 Pd C30 143.00(9) . . ? Cl1 Pd C30 83.69(8) . . ? P2 Pd C29 93.99(8) . . ? Cl2 Pd C29 140.80(9) . . ? Cl1 Pd C29 78.02(8) . . ? C30 Pd C29 75.12(11) . . ? P2 Pd Co2 75.90(2) . . ? Cl2 Pd Co2 167.85(3) . . ? Cl1 Pd Co2 97.33(3) . . ? C30 Pd Co2 41.73(8) . . ? C29 Pd Co2 41.15(8) . . ? C28 Co1 C27 95.68(18) . . ? C28 Co1 C2 106.33(15) . . ? C27 Co1 C2 105.41(15) . . ? C28 Co1 C1 102.32(16) . . ? C27 Co1 C1 144.78(15) . . ? C2 Co1 C1 40.48(13) . . ? C28 Co1 P3 94.99(12) . . ? C27 Co1 P3 103.15(12) . . ? C2 Co1 P3 142.10(10) . . ? C1 Co1 P3 105.11(9) . . ? C28 Co1 Co2 153.40(13) . . ? C27 Co1 Co2 105.84(12) . . ? C2 Co1 Co2 53.30(9) . . ? C1 Co1 Co2 51.22(9) . . ? P3 Co1 Co2 95.12(3) . . ? C30 Co2 C29 114.12(15) . . ? C30 Co2 C1 138.93(15) . . ? C29 Co2 C1 100.08(14) . . ? C30 Co2 C2 106.25(14) . . ? C29 Co2 C2 107.03(14) . . ? C1 Co2 C2 38.94(12) . . ? C30 Co2 P4 97.66(11) . . ? C29 Co2 P4 93.69(11) . . ? C1 Co2 P4 102.28(9) . . ? C2 Co2 P4 137.71(9) . . ? C30 Co2 Co1 91.64(11) . . ? C29 Co2 Co1 150.31(10) . . ? C1 Co2 Co1 50.63(9) . . ? C2 Co2 Co1 48.62(9) . . ? P4 Co2 Co1 97.35(3) . . ? C30 Co2 Pd 63.70(11) . . ? C29 Co2 Pd 67.62(10) . . ? C1 Co2 Pd 113.99(9) . . ? C2 Co2 Pd 81.07(8) . . ? P4 Co2 Pd 141.21(3) . . ? Co1 Co2 Pd 115.846(19) . . ? O5 P1 C1 112.52(13) . . ? O5 P1 C9 110.44(16) . . ? C1 P1 C9 108.58(15) . . ? O5 P1 C3 111.92(15) . . ? C1 P1 C3 106.81(16) . . ? C9 P1 C3 106.29(16) . . ? C2 P2 C15 105.44(15) . . ? C2 P2 C21 111.77(14) . . ? C15 P2 C21 107.90(15) . . ? C2 P2 Pd 100.36(10) . . ? C15 P2 Pd 118.08(11) . . ? C21 P2 Pd 112.84(12) . . ? C55 P3 C37 102.50(16) . . ? C55 P3 C31 104.70(16) . . ? C37 P3 C31 103.27(16) . . ? C55 P3 Co1 109.28(11) . . ? C37 P3 Co1 121.79(11) . . ? C31 P3 Co1 113.57(11) . . ? C49 P4 C43 101.11(15) . . ? C49 P4 C55 107.80(16) . . ? C43 P4 C55 104.04(15) . . ? C49 P4 Co2 116.34(11) . . ? C43 P4 Co2 117.40(10) . . ? C55 P4 Co2 109.06(12) . . ? C2 C1 P1 143.2(2) . . ? C2 C1 Co1 67.45(19) . . ? P1 C1 Co1 132.90(17) . . ? C2 C1 Co2 72.82(18) . . ? P1 C1 Co2 134.14(18) . . ? Co1 C1 Co2 78.14(11) . . ? C1 C2 P2 149.1(3) . . ? C1 C2 Co1 72.07(19) . . ? P2 C2 Co1 136.81(19) . . ? C1 C2 Co2 68.24(18) . . ? P2 C2 Co2 102.65(14) . . ? Co1 C2 Co2 78.08(11) . . ? C4 C3 C8 118.3(3) . . ? C4 C3 P1 125.2(3) . . ? C8 C3 P1 116.5(3) . . ? C3 C4 C5 121.5(4) . . ? C6 C5 C4 120.0(5) . . ? C7 C6 C5 119.7(4) . . ? C6 C7 C8 121.0(4) . . ? C3 C8 C7 119.4(4) . . ? C14 C9 C10 118.8(4) . . ? C14 C9 P1 123.7(3) . . ? C10 C9 P1 117.5(3) . . ? C11 C10 C9 120.8(4) . . ? C12 C11 C10 119.1(5) . . ? C13 C12 C11 121.3(5) . . ? C12 C13 C14 119.8(5) . . ? C9 C14 C13 120.2(4) . . ? C20 C15 C16 119.7(3) . . ? C20 C15 P2 120.5(3) . . ? C16 C15 P2 119.8(3) . . ? C17 C16 C15 119.3(3) . . ? C18 C17 C16 120.9(4) . . ? C17 C18 C19 120.1(4) . . ? C20 C19 C18 119.2(4) . . ? C19 C20 C15 120.9(3) . . ? C22 C21 C26 118.4(4) . . ? C22 C21 P2 122.0(3) . . ? C26 C21 P2 119.6(3) . . ? C21 C22 C23 120.9(4) . . ? C24 C23 C22 119.4(5) . . ? C25 C24 C23 120.8(4) . . ? C24 C25 C26 119.8(5) . . ? C21 C26 C25 120.6(4) . . ? O1 C27 Co1 176.4(4) . . ? O2 C28 Co1 178.1(4) . . ? O3 C29 Co2 171.9(3) . . ? O3 C29 Pd 116.4(2) . . ? Co2 C29 Pd 71.24(12) . . ? O4 C30 Co2 170.3(3) . . ? O4 C30 Pd 114.1(2) . . ? Co2 C30 Pd 74.57(12) . . ? C32 C31 C36 119.1(3) . . ? C32 C31 P3 118.5(3) . . ? C36 C31 P3 122.2(3) . . ? C31 C32 C33 119.5(4) . . ? C34 C33 C32 120.9(5) . . ? C33 C34 C35 120.0(4) . . ? C34 C35 C36 120.7(5) . . ? C31 C36 C35 119.8(4) . . ? C42 C37 C38 118.9(3) . . ? C42 C37 P3 121.6(3) . . ? C38 C37 P3 119.2(3) . . ? C39 C38 C37 120.5(4) . . ? C40 C39 C38 120.5(4) . . ? C39 C40 C41 119.7(4) . . ? C40 C41 C42 120.0(4) . . ? C37 C42 C41 120.4(3) . . ? C48 C43 C44 118.8(3) . . ? C48 C43 P4 118.3(3) . . ? C44 C43 P4 122.9(3) . . ? C43 C44 C45 120.0(4) . . ? C46 C45 C44 119.9(4) . . ? C45 C46 C47 120.9(4) . . ? C46 C47 C48 120.0(4) . . ? C43 C48 C47 120.5(4) . . ? C50 C49 C54 118.7(3) . . ? C50 C49 P4 122.1(3) . . ? C54 C49 P4 119.1(2) . . ? C49 C50 C51 120.3(4) . . ? C52 C51 C50 120.2(4) . . ? C53 C52 C51 120.4(4) . . ? C52 C53 C54 120.3(4) . . ? C53 C54 C49 120.2(4) . . ? P3 C55 P4 110.83(17) . . ? Cl3 C100 Cl4 115.2(3) . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 26.04 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.964 _refine_diff_density_min -0.613 _refine_diff_density_rms 0.086