data_[pd(10i)Cl2] _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety C53 H50 Cl2 O5 P2 Pd, 2(C H Cl3) _chemical_formula_sum 'C55 H52 Cl8 O5 P2 Pd' _chemical_formula_weight 1244.91 _chemical_absolute_configuration ad loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 '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' '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 P21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 11.7707(10) _cell_length_b 14.8558(10) _cell_length_c 15.7168(10) _cell_angle_alpha 90.00 _cell_angle_beta 99.1439(10) _cell_angle_gamma 90.00 _cell_volume 2713.4(3) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 12637 _cell_measurement_theta_min 1.75 _cell_measurement_theta_max 27.00 _exptl_crystal_description 'prism' _exptl_crystal_colour ? _exptl_crystal_size_max .3 _exptl_crystal_size_mid .2 _exptl_crystal_size_min .2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.524 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1268 _exptl_absorpt_coefficient_mu 0.843 _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 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method 'Phi/Omega-Scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12637 _diffrn_reflns_av_R_equivalents 0.0394 _diffrn_reflns_av_sigmaI/netI 0.1021 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.75 _diffrn_reflns_theta_max 27.00 _reflns_number_total 9664 _reflns_number_gt 7448 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius COLLECT' _computing_cell_refinement 'Nonius DENZO (Otwinowski, Minor 1997)' _computing_data_reduction 'Nonius DENZO (Otwinowski, Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SCHAKAL99 (E. Keller 1999)' _computing_publication_material 'PLATON (A. L. Spek 1980-2004)' _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^)+(0.0402P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.01(3) _refine_ls_number_reflns 9664 _refine_ls_number_parameters 646 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0710 _refine_ls_R_factor_gt 0.0455 _refine_ls_wR_factor_ref 0.1030 _refine_ls_wR_factor_gt 0.0857 _refine_ls_goodness_of_fit_ref 0.969 _refine_ls_restrained_S_all 0.969 _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 Pd1 Pd 0.25624(4) 0.70098(3) 0.17549(2) 0.01801(11) Uani 1 1 d . . . Cl1 Cl 0.08411(13) 0.62287(9) 0.13417(9) 0.0224(3) Uani 1 1 d . . . Cl2 Cl 0.18496(14) 0.81412(10) 0.07943(10) 0.0311(4) Uani 1 1 d . . . P1 P 0.32906(13) 0.59554(9) 0.26793(9) 0.0162(3) Uani 1 1 d . . . P2 P 0.42042(14) 0.77859(9) 0.20357(9) 0.0181(4) Uani 1 1 d . . . O1 O 0.2933(3) 0.6013(2) 0.3613(2) 0.0178(9) Uani 1 1 d . . . O2 O 0.0443(3) 0.4603(2) 0.3763(2) 0.0214(9) Uani 1 1 d . . . O3 O 0.1728(3) 0.3459(2) 0.3752(2) 0.0192(9) Uani 1 1 d . . . O4 O 0.3063(3) 0.4980(2) 0.2321(2) 0.0167(9) Uani 1 1 d . . . C3 C 0.1768(5) 0.5867(4) 0.3841(3) 0.0187(13) Uani 1 1 d . . . C4 C 0.1338(5) 0.4971(4) 0.3375(3) 0.0180(13) Uani 1 1 d . . . H4 H 0.1074 0.5078 0.2747 0.022 Uiso 1 1 calc R . . C5 C 0.0539(5) 0.3643(4) 0.3795(4) 0.0209(14) Uani 1 1 d . . . C6 C 0.2282(5) 0.4250(3) 0.3510(3) 0.0164(13) Uani 1 1 d . . . H6 H 0.2885 0.4437 0.4000 0.020 Uiso 1 1 calc R . . C7 C 0.2863(5) 0.4087(4) 0.2699(3) 0.0179(13) Uani 1 1 d . . . C8 C 0.4021(5) 0.3617(4) 0.2897(3) 0.0196(14) Uani 1 1 d . . . C9 C 0.4307(5) 0.3087(4) 0.3629(4) 0.0244(15) Uani 1 1 d . . . H9 H 0.3786 0.3040 0.4031 0.029 Uiso 1 1 calc R . . C10 C 0.5358(6) 0.2620(4) 0.3783(4) 0.0304(17) Uani 1 1 d . . . H10 H 0.5547 0.2268 0.4291 0.036 Uiso 1 1 calc R . . C11 C 0.6110(6) 0.2670(4) 0.3203(4) 0.0336(17) Uani 1 1 d . . . H11 H 0.6818 0.2352 0.3306 0.040 Uiso 1 1 calc R . . C12 C 0.5837(6) 0.3186(4) 0.2466(4) 0.0314(16) Uani 1 1 d . . . H12 H 0.6361 0.3226 0.2066 0.038 Uiso 1 1 calc R . . C13 C 0.4785(6) 0.3649(4) 0.2308(4) 0.0227(14) Uani 1 1 d . . . H13 H 0.4594 0.3989 0.1793 0.027 Uiso 1 1 calc R . . C14 C 0.2090(5) 0.3559(4) 0.1990(3) 0.0168(13) Uani 1 1 d . . . C15 C 0.1958(5) 0.2640(4) 0.2091(3) 0.0206(14) Uani 1 1 d . . . H15 H 0.2354 0.2352 0.2592 0.025 Uiso 1 1 calc R . . C16 C 0.1267(5) 0.2136(4) 0.1482(3) 0.0231(14) Uani 1 1 d . . . H16 H 0.1201 0.1506 0.1562 0.028 Uiso 1 1 calc R . . C17 C 0.0666(5) 0.2542(4) 0.0752(4) 0.0246(15) Uani 1 1 d . . . H17 H 0.0184 0.2197 0.0331 0.029 Uiso 1 1 calc R . . C18 C 0.0783(5) 0.3458(4) 0.0650(4) 0.0254(15) Uani 1 1 d . . . H18 H 0.0374 0.3744 0.0153 0.030 Uiso 1 1 calc R . . C19 C 0.1486(5) 0.3971(4) 0.1259(3) 0.0189(14) Uani 1 1 d . . . H19 H 0.1554 0.4601 0.1177 0.023 Uiso 1 1 calc R . . C20 C 0.0273(6) 0.3336(4) 0.4658(4) 0.0315(17) Uani 1 1 d . . . H20A H 0.0825 0.3606 0.5119 0.047 Uiso 1 1 calc R . . H20B H 0.0329 0.2678 0.4695 0.047 Uiso 1 1 calc R . . H20C H -0.0508 0.3524 0.4718 0.047 Uiso 1 1 calc R . . C21 C -0.0226(5) 0.3223(4) 0.3050(4) 0.0266(15) Uani 1 1 d . . . H21A H -0.1029 0.3381 0.3076 0.040 Uiso 1 1 calc R . . H21B H -0.0138 0.2567 0.3078 0.040 Uiso 1 1 calc R . . H21C H -0.0015 0.3445 0.2510 0.040 Uiso 1 1 calc R . . C22 C 0.1027(5) 0.6675(4) 0.3556(3) 0.0198(15) Uani 1 1 d . . . C23 C 0.1454(6) 0.7537(4) 0.3653(4) 0.0235(15) Uani 1 1 d . . . H23 H 0.2238 0.7625 0.3898 0.028 Uiso 1 1 calc R . . C24 C 0.0772(6) 0.8282(4) 0.3404(4) 0.0287(16) Uani 1 1 d . . . H24 H 0.1084 0.8872 0.3474 0.034 Uiso 1 1 calc R . . C25 C -0.0358(7) 0.8155(4) 0.3056(4) 0.0332(18) Uani 1 1 d . . . H25 H -0.0831 0.8658 0.2868 0.040 Uiso 1 1 calc R . . C26 C -0.0809(6) 0.7300(4) 0.2979(4) 0.0333(18) Uani 1 1 d . . . H26 H -0.1601 0.7219 0.2755 0.040 Uiso 1 1 calc R . . C27 C -0.0130(6) 0.6554(4) 0.3220(4) 0.0245(15) Uani 1 1 d . . . H27 H -0.0450 0.5966 0.3158 0.029 Uiso 1 1 calc R . . C28 C 0.1964(6) 0.5763(3) 0.4822(3) 0.0209(14) Uani 1 1 d . . . C29 C 0.3042(6) 0.5643(3) 0.5308(3) 0.0213(14) Uani 1 1 d . . . H29 H 0.3706 0.5654 0.5035 0.026 Uiso 1 1 calc R . . C30 C 0.3160(6) 0.5507(4) 0.6195(4) 0.0267(15) Uani 1 1 d . . . H30 H 0.3905 0.5432 0.6522 0.032 Uiso 1 1 calc R . . C31 C 0.2205(6) 0.5480(4) 0.6601(4) 0.0320(18) Uani 1 1 d . . . H31 H 0.2282 0.5371 0.7203 0.038 Uiso 1 1 calc R . . C32 C 0.1142(6) 0.5612(4) 0.6118(4) 0.0320(17) Uani 1 1 d . . . H32 H 0.0478 0.5596 0.6392 0.038 Uiso 1 1 calc R . . C33 C 0.1020(6) 0.5766(4) 0.5251(4) 0.0272(15) Uani 1 1 d . . . H33 H 0.0275 0.5878 0.4936 0.033 Uiso 1 1 calc R . . O34 O 0.4675(3) 0.5959(2) 0.2952(2) 0.0177(9) Uani 1 1 d . . . C35 C 0.5316(5) 0.6677(3) 0.3371(3) 0.0173(14) Uani 1 1 d . . . C36 C 0.5108(5) 0.7557(4) 0.3068(4) 0.0185(14) Uani 1 1 d . . . C37 C 0.5147(5) 0.7585(4) 0.1237(3) 0.0195(14) Uani 1 1 d . . . C38 C 0.6342(6) 0.7644(4) 0.1460(4) 0.0283(16) Uani 1 1 d . . . H38 H 0.6682 0.7692 0.2048 0.034 Uiso 1 1 calc R . . C39 C 0.7033(6) 0.7632(4) 0.0821(4) 0.0327(16) Uani 1 1 d . . . H39 H 0.7846 0.7671 0.0965 0.039 Uiso 1 1 calc R . . C40 C 0.6515(6) 0.7562(4) -0.0025(4) 0.0283(16) Uani 1 1 d . . . H40 H 0.6981 0.7565 -0.0467 0.034 Uiso 1 1 calc R . . C41 C 0.5332(6) 0.7487(4) -0.0250(4) 0.0270(16) Uani 1 1 d . . . H41 H 0.4997 0.7433 -0.0839 0.032 Uiso 1 1 calc R . . C42 C 0.4643(6) 0.7491(3) 0.0375(3) 0.0223(15) Uani 1 1 d . . . H42 H 0.3832 0.7431 0.0224 0.027 Uiso 1 1 calc R . . C43 C 0.4061(5) 0.9008(4) 0.2035(3) 0.0197(14) Uani 1 1 d . . . C44 C 0.4780(5) 0.9546(4) 0.1643(3) 0.0206(14) Uani 1 1 d . . . H44 H 0.5314 0.9280 0.1324 0.025 Uiso 1 1 calc R . . C45 C 0.4725(6) 1.0478(4) 0.1715(4) 0.0263(15) Uani 1 1 d . . . H45 H 0.5211 1.0846 0.1434 0.032 Uiso 1 1 calc R . . C46 C 0.3976(6) 1.0868(4) 0.2186(4) 0.0291(16) Uani 1 1 d . . . H46 H 0.3966 1.1503 0.2252 0.035 Uiso 1 1 calc R . . C47 C 0.3236(6) 1.0339(4) 0.2566(4) 0.0331(18) Uani 1 1 d . . . H47 H 0.2697 1.0613 0.2875 0.040 Uiso 1 1 calc R . . C48 C 0.3273(6) 0.9412(4) 0.2501(4) 0.0289(16) Uani 1 1 d . . . H48 H 0.2767 0.9050 0.2770 0.035 Uiso 1 1 calc R . . C49 C 0.5723(6) 0.8267(4) 0.3514(3) 0.0246(15) Uani 1 1 d . . . H49 H 0.5577 0.8869 0.3323 0.030 Uiso 1 1 calc R . . C50 C 0.6537(6) 0.8098(4) 0.4227(4) 0.0289(16) Uani 1 1 d . . . H50 H 0.6920 0.8584 0.4546 0.035 Uiso 1 1 calc R . . C51 C 0.6794(6) 0.7221(4) 0.4476(3) 0.0262(16) Uani 1 1 d . . . H51 H 0.7385 0.7118 0.4952 0.031 Uiso 1 1 calc R . . C52 C 0.6227(5) 0.6476(4) 0.4061(3) 0.0180(13) Uani 1 1 d . . . C53 C 0.6655(5) 0.5518(4) 0.4286(4) 0.0221(14) Uani 1 1 d . . . C54 C 0.5748(6) 0.4943(4) 0.4637(4) 0.0304(16) Uani 1 1 d . . . H54A H 0.5582 0.5206 0.5176 0.046 Uiso 1 1 calc R . . H54B H 0.6042 0.4330 0.4747 0.046 Uiso 1 1 calc R . . H54C H 0.5041 0.4925 0.4213 0.046 Uiso 1 1 calc R . . C55 C 0.7019(5) 0.5089(4) 0.3490(4) 0.0297(16) Uani 1 1 d . . . H55A H 0.7345 0.4492 0.3638 0.045 Uiso 1 1 calc R . . H55B H 0.7599 0.5469 0.3282 0.045 Uiso 1 1 calc R . . H55C H 0.6347 0.5031 0.3037 0.045 Uiso 1 1 calc R . . C56 C 0.7753(6) 0.5520(4) 0.4991(4) 0.0340(17) Uani 1 1 d . . . H56A H 0.7557 0.5758 0.5531 0.051 Uiso 1 1 calc R . . H56B H 0.8345 0.5901 0.4801 0.051 Uiso 1 1 calc R . . H56C H 0.8045 0.4904 0.5083 0.051 Uiso 1 1 calc R . . Cl3 Cl 0.80251(16) 0.55383(11) -0.00549(11) 0.0389(4) Uani 1 1 d . . . Cl4 Cl 0.59813(16) 0.51952(11) 0.07145(11) 0.0393(4) Uani 1 1 d . . . Cl5 Cl 0.81671(19) 0.44497(16) 0.14700(13) 0.0669(7) Uani 1 1 d . . . C57 C 0.7321(6) 0.4763(4) 0.0502(4) 0.0312(17) Uani 1 1 d . . . H57 H 0.7163 0.4213 0.0136 0.037 Uiso 1 1 calc R . . Cl6 Cl 0.91957(17) 0.01314(12) 0.12222(11) 0.0457(5) Uani 1 1 d . . . Cl7 Cl 0.69329(16) 0.03174(12) 0.02031(11) 0.0427(5) Uani 1 1 d . . . Cl8 Cl 0.78816(16) 0.17556(10) 0.13434(10) 0.0387(5) Uani 1 1 d . . . C58 C 0.8205(5) 0.0889(4) 0.0654(4) 0.0325(17) Uani 1 1 d . . . H58 H 0.8558 0.1162 0.0177 0.039 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.0204(3) 0.0187(2) 0.01440(19) 0.00279(19) 0.00104(17) 0.0002(2) Cl1 0.0206(9) 0.0261(8) 0.0197(7) 0.0023(6) 0.0005(6) -0.0017(7) Cl2 0.0280(11) 0.0306(8) 0.0314(9) 0.0151(7) -0.0055(7) 0.0000(7) P1 0.0170(9) 0.0171(7) 0.0142(7) 0.0002(6) 0.0018(6) 0.0016(7) P2 0.0247(10) 0.0168(7) 0.0128(7) 0.0004(6) 0.0026(7) -0.0003(7) O1 0.020(2) 0.020(2) 0.0138(19) -0.0005(15) 0.0047(17) -0.0024(18) O2 0.018(3) 0.019(2) 0.028(2) 0.0024(17) 0.0092(19) -0.0002(18) O3 0.019(3) 0.019(2) 0.020(2) 0.0040(16) 0.0043(18) -0.0012(18) O4 0.019(3) 0.020(2) 0.0107(18) 0.0046(16) 0.0025(17) -0.0009(18) C3 0.013(3) 0.027(3) 0.019(3) 0.001(2) 0.010(2) -0.004(3) C4 0.017(4) 0.022(3) 0.015(3) -0.001(2) 0.002(2) 0.000(3) C5 0.021(4) 0.022(3) 0.021(3) 0.004(2) 0.007(3) 0.000(3) C6 0.015(4) 0.019(3) 0.015(3) -0.001(2) 0.003(2) -0.003(3) C7 0.024(4) 0.015(3) 0.016(3) 0.005(2) 0.007(3) -0.001(3) C8 0.023(4) 0.019(3) 0.016(3) -0.007(2) 0.002(3) -0.003(3) C9 0.026(4) 0.022(3) 0.025(3) 0.001(3) 0.005(3) 0.002(3) C10 0.038(5) 0.024(3) 0.027(4) -0.003(3) 0.000(3) 0.011(3) C11 0.026(4) 0.023(3) 0.051(4) -0.008(3) 0.002(4) 0.012(3) C12 0.028(4) 0.025(3) 0.043(4) -0.004(3) 0.012(3) 0.000(3) C13 0.028(4) 0.020(3) 0.021(3) -0.001(2) 0.009(3) 0.005(3) C14 0.015(3) 0.021(3) 0.017(3) -0.001(2) 0.010(2) -0.005(3) C15 0.020(4) 0.027(3) 0.018(3) 0.000(2) 0.011(3) -0.002(3) C16 0.026(4) 0.021(3) 0.023(3) -0.001(3) 0.008(3) -0.004(3) C17 0.021(4) 0.032(4) 0.023(3) -0.009(3) 0.007(3) -0.005(3) C18 0.028(4) 0.029(3) 0.019(3) 0.001(3) 0.003(3) 0.001(3) C19 0.019(4) 0.023(3) 0.015(3) 0.004(2) 0.006(3) -0.001(3) C20 0.040(5) 0.031(4) 0.026(3) 0.008(3) 0.011(3) 0.005(3) C21 0.022(4) 0.030(3) 0.028(3) -0.003(3) 0.005(3) 0.001(3) C22 0.025(4) 0.018(3) 0.015(3) -0.003(2) 0.000(3) 0.009(3) C23 0.030(4) 0.022(3) 0.020(3) -0.006(2) 0.008(3) 0.005(3) C24 0.045(5) 0.016(3) 0.029(3) 0.003(3) 0.018(3) 0.001(3) C25 0.049(5) 0.026(4) 0.028(4) 0.004(3) 0.016(3) 0.021(3) C26 0.031(4) 0.038(4) 0.029(4) 0.001(3) -0.001(3) 0.012(3) C27 0.020(4) 0.028(3) 0.027(3) 0.001(3) 0.008(3) 0.001(3) C28 0.030(4) 0.017(3) 0.015(3) -0.005(2) 0.002(3) 0.000(3) C29 0.034(4) 0.015(3) 0.016(3) -0.004(2) 0.009(3) 0.002(3) C30 0.040(5) 0.018(3) 0.021(3) -0.004(2) 0.001(3) -0.001(3) C31 0.059(6) 0.024(3) 0.017(3) -0.005(2) 0.019(3) -0.010(3) C32 0.040(5) 0.035(4) 0.025(3) -0.002(3) 0.018(3) -0.006(3) C33 0.029(4) 0.032(4) 0.021(3) -0.001(3) 0.005(3) 0.001(3) O34 0.016(2) 0.018(2) 0.019(2) -0.0006(16) 0.0014(17) 0.0005(18) C35 0.020(4) 0.017(3) 0.017(3) -0.003(2) 0.007(3) 0.002(3) C36 0.021(4) 0.019(3) 0.017(3) -0.001(2) 0.006(3) -0.005(3) C37 0.021(4) 0.018(3) 0.019(3) 0.004(2) 0.000(3) -0.001(3) C38 0.035(5) 0.025(3) 0.025(3) 0.001(3) 0.004(3) 0.003(3) C39 0.026(4) 0.040(4) 0.034(4) -0.003(3) 0.010(3) -0.003(3) C40 0.037(5) 0.028(3) 0.024(3) 0.001(3) 0.017(3) -0.001(3) C41 0.040(5) 0.026(3) 0.017(3) 0.002(3) 0.011(3) 0.001(3) C42 0.028(4) 0.018(3) 0.022(3) 0.000(2) 0.006(3) -0.003(3) C43 0.026(4) 0.017(3) 0.014(3) 0.002(2) -0.003(3) 0.001(3) C44 0.021(4) 0.022(3) 0.019(3) 0.002(2) 0.004(3) 0.001(3) C45 0.032(4) 0.023(3) 0.024(3) 0.005(3) 0.005(3) -0.001(3) C46 0.031(4) 0.027(3) 0.027(4) -0.004(3) -0.004(3) 0.004(3) C47 0.038(5) 0.030(4) 0.033(4) -0.004(3) 0.010(3) 0.008(3) C48 0.038(5) 0.023(3) 0.027(4) 0.004(3) 0.009(3) 0.002(3) C49 0.039(4) 0.018(3) 0.017(3) -0.001(2) 0.005(3) -0.001(3) C50 0.038(5) 0.025(3) 0.022(3) -0.004(3) -0.002(3) -0.006(3) C51 0.031(4) 0.029(4) 0.016(3) -0.004(2) -0.006(3) -0.001(3) C52 0.015(4) 0.026(3) 0.015(3) -0.001(2) 0.009(3) 0.001(3) C53 0.018(4) 0.023(3) 0.025(3) -0.001(3) 0.001(3) 0.004(3) C54 0.032(4) 0.027(3) 0.030(4) 0.008(3) -0.005(3) -0.001(3) C55 0.017(4) 0.034(4) 0.039(4) -0.008(3) 0.006(3) 0.007(3) C56 0.031(5) 0.037(4) 0.031(4) 0.002(3) -0.004(3) 0.007(3) Cl3 0.0393(12) 0.0391(9) 0.0415(10) 0.0103(8) 0.0162(8) -0.0006(9) Cl4 0.0330(12) 0.0459(10) 0.0408(10) 0.0089(8) 0.0115(8) 0.0033(9) Cl5 0.0422(14) 0.1103(18) 0.0504(12) 0.0433(12) 0.0143(10) 0.0251(13) C57 0.041(5) 0.022(3) 0.034(4) -0.001(3) 0.017(3) 0.001(3) Cl6 0.0417(13) 0.0481(11) 0.0463(11) -0.0053(8) 0.0038(9) 0.0060(9) Cl7 0.0315(11) 0.0541(11) 0.0437(10) -0.0124(8) 0.0099(8) -0.0085(9) Cl8 0.0495(13) 0.0369(10) 0.0297(8) -0.0012(7) 0.0059(8) -0.0016(8) C58 0.028(4) 0.044(4) 0.026(3) -0.005(3) 0.008(3) -0.009(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 P1 2.2143(14) . ? Pd1 P2 2.2333(16) . ? Pd1 Cl2 2.3251(14) . ? Pd1 Cl1 2.3356(15) . ? P1 O4 1.563(4) . ? P1 O1 1.593(4) . ? P1 O34 1.618(4) . ? P2 C43 1.823(5) . ? P2 C36 1.825(6) . ? P2 C37 1.827(6) . ? O1 C3 1.487(7) . ? O2 C4 1.408(7) . ? O2 C5 1.432(6) . ? O3 C6 1.424(6) . ? O3 C5 1.437(7) . ? O4 C7 1.487(6) . ? C3 C22 1.509(8) . ? C3 C28 1.531(7) . ? C3 C4 1.564(7) . ? C4 C6 1.533(8) . ? C5 C21 1.495(8) . ? C5 C20 1.510(8) . ? C6 C7 1.559(8) . ? C7 C8 1.519(8) . ? C7 C14 1.536(7) . ? C8 C9 1.390(7) . ? C8 C13 1.392(8) . ? C9 C10 1.405(8) . ? C10 C11 1.371(9) . ? C11 C12 1.383(9) . ? C12 C13 1.403(8) . ? C14 C15 1.387(7) . ? C14 C19 1.393(7) . ? C15 C16 1.374(7) . ? C16 C17 1.387(7) . ? C17 C18 1.379(8) . ? C18 C19 1.389(7) . ? C22 C23 1.376(8) . ? C22 C27 1.391(8) . ? C23 C24 1.387(8) . ? C24 C25 1.368(9) . ? C25 C26 1.376(9) . ? C26 C27 1.384(8) . ? C28 C29 1.385(8) . ? C28 C33 1.387(8) . ? C29 C30 1.393(8) . ? C30 C31 1.379(9) . ? C31 C32 1.370(9) . ? C32 C33 1.368(8) . ? O34 C35 1.408(6) . ? C35 C36 1.399(7) . ? C35 C52 1.430(8) . ? C36 C49 1.403(8) . ? C37 C38 1.397(8) . ? C37 C42 1.398(7) . ? C38 C39 1.389(9) . ? C39 C40 1.376(8) . ? C40 C41 1.386(9) . ? C41 C42 1.368(8) . ? C43 C44 1.379(8) . ? C43 C48 1.405(9) . ? C44 C45 1.392(8) . ? C45 C46 1.367(9) . ? C46 C47 1.378(9) . ? C47 C48 1.381(8) . ? C49 C50 1.376(8) . ? C50 C51 1.381(8) . ? C51 C52 1.398(7) . ? C52 C53 1.533(8) . ? C53 C55 1.526(8) . ? C53 C54 1.537(8) . ? C53 C56 1.563(7) . ? Cl3 C57 1.735(6) . ? Cl4 C57 1.782(7) . ? Cl5 C57 1.744(6) . ? Cl6 C58 1.758(6) . ? Cl7 C58 1.769(6) . ? Cl8 C58 1.763(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 P1 Pd1 P2 90.17(5) . . ? P1 Pd1 Cl2 178.26(6) . . ? P2 Pd1 Cl2 88.09(5) . . ? P1 Pd1 Cl1 93.40(5) . . ? P2 Pd1 Cl1 175.27(5) . . ? Cl2 Pd1 Cl1 88.34(5) . . ? O4 P1 O1 109.1(2) . . ? O4 P1 O34 101.9(2) . . ? O1 P1 O34 99.11(19) . . ? O4 P1 Pd1 113.19(14) . . ? O1 P1 Pd1 115.79(15) . . ? O34 P1 Pd1 116.11(14) . . ? C43 P2 C36 103.1(2) . . ? C43 P2 C37 103.2(3) . . ? C36 P2 C37 104.4(3) . . ? C43 P2 Pd1 115.9(2) . . ? C36 P2 Pd1 116.3(2) . . ? C37 P2 Pd1 112.41(19) . . ? C3 O1 P1 127.0(3) . . ? C4 O2 C5 109.9(4) . . ? C6 O3 C5 110.3(4) . . ? C7 O4 P1 135.4(3) . . ? O1 C3 C22 108.9(4) . . ? O1 C3 C28 105.1(4) . . ? C22 C3 C28 111.5(5) . . ? O1 C3 C4 104.7(4) . . ? C22 C3 C4 114.2(4) . . ? C28 C3 C4 111.8(4) . . ? O2 C4 C6 104.2(4) . . ? O2 C4 C3 109.7(4) . . ? C6 C4 C3 110.9(4) . . ? O2 C5 O3 105.1(4) . . ? O2 C5 C21 110.7(5) . . ? O3 C5 C21 110.8(5) . . ? O2 C5 C20 107.8(5) . . ? O3 C5 C20 109.1(5) . . ? C21 C5 C20 113.0(5) . . ? O3 C6 C4 105.1(5) . . ? O3 C6 C7 111.7(4) . . ? C4 C6 C7 113.4(4) . . ? O4 C7 C8 107.3(5) . . ? O4 C7 C14 106.2(4) . . ? C8 C7 C14 108.8(4) . . ? O4 C7 C6 107.8(4) . . ? C8 C7 C6 113.6(4) . . ? C14 C7 C6 112.8(5) . . ? C9 C8 C13 118.3(6) . . ? C9 C8 C7 121.4(5) . . ? C13 C8 C7 120.1(5) . . ? C8 C9 C10 120.9(6) . . ? C11 C10 C9 120.1(6) . . ? C10 C11 C12 119.9(6) . . ? C11 C12 C13 120.1(6) . . ? C8 C13 C12 120.7(5) . . ? C15 C14 C19 118.3(5) . . ? C15 C14 C7 118.9(5) . . ? C19 C14 C7 122.7(5) . . ? C16 C15 C14 121.4(5) . . ? C15 C16 C17 120.5(5) . . ? C18 C17 C16 118.5(5) . . ? C17 C18 C19 121.3(5) . . ? C18 C19 C14 119.9(5) . . ? C23 C22 C27 118.8(5) . . ? C23 C22 C3 121.6(5) . . ? C27 C22 C3 119.6(5) . . ? C22 C23 C24 121.8(6) . . ? C25 C24 C23 119.1(6) . . ? C24 C25 C26 120.0(6) . . ? C25 C26 C27 121.2(6) . . ? C26 C27 C22 119.2(6) . . ? C29 C28 C33 117.9(5) . . ? C29 C28 C3 123.1(6) . . ? C33 C28 C3 119.0(5) . . ? C28 C29 C30 120.5(6) . . ? C31 C30 C29 120.5(6) . . ? C32 C31 C30 118.7(6) . . ? C33 C32 C31 121.2(7) . . ? C32 C33 C28 121.2(6) . . ? C35 O34 P1 124.6(3) . . ? C36 C35 O34 119.8(5) . . ? C36 C35 C52 121.5(5) . . ? O34 C35 C52 118.5(4) . . ? C35 C36 C49 118.9(5) . . ? C35 C36 P2 121.5(4) . . ? C49 C36 P2 119.1(4) . . ? C38 C37 C42 120.3(6) . . ? C38 C37 P2 121.0(4) . . ? C42 C37 P2 118.1(5) . . ? C39 C38 C37 120.0(6) . . ? C40 C39 C38 118.7(6) . . ? C39 C40 C41 121.6(6) . . ? C42 C41 C40 120.2(6) . . ? C41 C42 C37 119.2(6) . . ? C44 C43 C48 119.2(5) . . ? C44 C43 P2 121.0(5) . . ? C48 C43 P2 119.6(5) . . ? C43 C44 C45 120.0(6) . . ? C46 C45 C44 120.6(6) . . ? C45 C46 C47 120.0(6) . . ? C46 C47 C48 120.5(7) . . ? C47 C48 C43 119.7(6) . . ? C50 C49 C36 120.5(5) . . ? C49 C50 C51 119.7(5) . . ? C50 C51 C52 123.2(5) . . ? C51 C52 C35 115.7(5) . . ? C51 C52 C53 120.8(5) . . ? C35 C52 C53 123.2(5) . . ? C55 C53 C52 108.8(5) . . ? C55 C53 C54 111.4(5) . . ? C52 C53 C54 112.2(5) . . ? C55 C53 C56 105.9(5) . . ? C52 C53 C56 111.5(5) . . ? C54 C53 C56 106.9(5) . . ? Cl3 C57 Cl5 111.4(4) . . ? Cl3 C57 Cl4 111.3(3) . . ? Cl5 C57 Cl4 109.4(3) . . ? Cl6 C58 Cl8 110.3(3) . . ? Cl6 C58 Cl7 110.3(3) . . ? Cl8 C58 Cl7 110.2(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag P2 Pd1 P1 O4 -134.32(18) . . . . ? Cl2 Pd1 P1 O4 -135(2) . . . . ? Cl1 Pd1 P1 O4 42.57(18) . . . . ? P2 Pd1 P1 O1 98.67(17) . . . . ? Cl2 Pd1 P1 O1 98(2) . . . . ? Cl1 Pd1 P1 O1 -84.43(17) . . . . ? P2 Pd1 P1 O34 -16.97(16) . . . . ? Cl2 Pd1 P1 O34 -18(2) . . . . ? Cl1 Pd1 P1 O34 159.93(16) . . . . ? P1 Pd1 P2 C43 -144.2(2) . . . . ? Cl2 Pd1 P2 C43 35.8(2) . . . . ? Cl1 Pd1 P2 C43 76.8(8) . . . . ? P1 Pd1 P2 C36 -22.8(2) . . . . ? Cl2 Pd1 P2 C36 157.2(2) . . . . ? Cl1 Pd1 P2 C36 -161.8(7) . . . . ? P1 Pd1 P2 C37 97.46(19) . . . . ? Cl2 Pd1 P2 C37 -82.6(2) . . . . ? Cl1 Pd1 P2 C37 -41.5(8) . . . . ? O4 P1 O1 C3 -61.7(4) . . . . ? O34 P1 O1 C3 -167.7(4) . . . . ? Pd1 P1 O1 C3 67.3(4) . . . . ? O1 P1 O4 C7 -16.8(6) . . . . ? O34 P1 O4 C7 87.3(5) . . . . ? Pd1 P1 O4 C7 -147.3(5) . . . . ? P1 O1 C3 C22 -74.6(5) . . . . ? P1 O1 C3 C28 165.9(3) . . . . ? P1 O1 C3 C4 48.0(5) . . . . ? C5 O2 C4 C6 -23.4(5) . . . . ? C5 O2 C4 C3 -142.2(4) . . . . ? O1 C3 C4 O2 160.2(4) . . . . ? C22 C3 C4 O2 -80.7(6) . . . . ? C28 C3 C4 O2 47.0(6) . . . . ? O1 C3 C4 C6 45.7(5) . . . . ? C22 C3 C4 C6 164.8(5) . . . . ? C28 C3 C4 C6 -67.5(6) . . . . ? C4 O2 C5 O3 22.9(5) . . . . ? C4 O2 C5 C21 -96.7(6) . . . . ? C4 O2 C5 C20 139.2(5) . . . . ? C6 O3 C5 O2 -12.5(5) . . . . ? C6 O3 C5 C21 107.0(5) . . . . ? C6 O3 C5 C20 -127.9(5) . . . . ? C5 O3 C6 C4 -1.3(5) . . . . ? C5 O3 C6 C7 -124.7(5) . . . . ? O2 C4 C6 O3 14.8(5) . . . . ? C3 C4 C6 O3 132.7(4) . . . . ? O2 C4 C6 C7 137.1(4) . . . . ? C3 C4 C6 C7 -105.0(5) . . . . ? P1 O4 C7 C8 -93.7(6) . . . . ? P1 O4 C7 C14 150.0(4) . . . . ? P1 O4 C7 C6 28.9(7) . . . . ? O3 C6 C7 O4 161.2(4) . . . . ? C4 C6 C7 O4 42.7(6) . . . . ? O3 C6 C7 C8 -80.0(6) . . . . ? C4 C6 C7 C8 161.4(4) . . . . ? O3 C6 C7 C14 44.3(6) . . . . ? C4 C6 C7 C14 -74.2(5) . . . . ? O4 C7 C8 C9 142.6(5) . . . . ? C14 C7 C8 C9 -102.9(6) . . . . ? C6 C7 C8 C9 23.5(7) . . . . ? O4 C7 C8 C13 -42.7(6) . . . . ? C14 C7 C8 C13 71.8(6) . . . . ? C6 C7 C8 C13 -161.8(5) . . . . ? C13 C8 C9 C10 2.0(8) . . . . ? C7 C8 C9 C10 176.8(5) . . . . ? C8 C9 C10 C11 -1.0(9) . . . . ? C9 C10 C11 C12 0.3(9) . . . . ? C10 C11 C12 C13 -0.6(9) . . . . ? C9 C8 C13 C12 -2.3(8) . . . . ? C7 C8 C13 C12 -177.2(5) . . . . ? C11 C12 C13 C8 1.7(9) . . . . ? O4 C7 C14 C15 166.5(5) . . . . ? C8 C7 C14 C15 51.2(7) . . . . ? C6 C7 C14 C15 -75.7(7) . . . . ? O4 C7 C14 C19 -15.6(8) . . . . ? C8 C7 C14 C19 -130.8(6) . . . . ? C6 C7 C14 C19 102.2(6) . . . . ? C19 C14 C15 C16 1.2(9) . . . . ? C7 C14 C15 C16 179.2(5) . . . . ? C14 C15 C16 C17 -1.0(9) . . . . ? C15 C16 C17 C18 0.3(9) . . . . ? C16 C17 C18 C19 0.1(10) . . . . ? C17 C18 C19 C14 0.1(10) . . . . ? C15 C14 C19 C18 -0.7(9) . . . . ? C7 C14 C19 C18 -178.7(6) . . . . ? O1 C3 C22 C23 -40.4(7) . . . . ? C28 C3 C22 C23 75.1(7) . . . . ? C4 C3 C22 C23 -157.1(6) . . . . ? O1 C3 C22 C27 142.5(5) . . . . ? C28 C3 C22 C27 -102.1(6) . . . . ? C4 C3 C22 C27 25.8(8) . . . . ? C27 C22 C23 C24 -1.8(10) . . . . ? C3 C22 C23 C24 -179.0(5) . . . . ? C22 C23 C24 C25 0.3(10) . . . . ? C23 C24 C25 C26 1.7(9) . . . . ? C24 C25 C26 C27 -2.2(10) . . . . ? C25 C26 C27 C22 0.7(10) . . . . ? C23 C22 C27 C26 1.3(9) . . . . ? C3 C22 C27 C26 178.5(6) . . . . ? O1 C3 C28 C29 -12.2(7) . . . . ? C22 C3 C28 C29 -130.1(6) . . . . ? C4 C3 C28 C29 100.8(6) . . . . ? O1 C3 C28 C33 169.4(5) . . . . ? C22 C3 C28 C33 51.6(7) . . . . ? C4 C3 C28 C33 -77.6(6) . . . . ? C33 C28 C29 C30 1.7(8) . . . . ? C3 C28 C29 C30 -176.7(5) . . . . ? C28 C29 C30 C31 0.7(8) . . . . ? C29 C30 C31 C32 -1.6(9) . . . . ? C30 C31 C32 C33 0.1(9) . . . . ? C31 C32 C33 C28 2.3(9) . . . . ? C29 C28 C33 C32 -3.2(8) . . . . ? C3 C28 C33 C32 175.3(5) . . . . ? O4 P1 O34 C35 -175.4(4) . . . . ? O1 P1 O34 C35 -63.6(4) . . . . ? Pd1 P1 O34 C35 61.1(4) . . . . ? P1 O34 C35 C36 -47.3(7) . . . . ? P1 O34 C35 C52 137.3(5) . . . . ? O34 C35 C36 C49 177.5(5) . . . . ? C52 C35 C36 C49 -7.2(10) . . . . ? O34 C35 C36 P2 -10.7(9) . . . . ? C52 C35 C36 P2 164.6(5) . . . . ? C43 P2 C36 C35 172.3(6) . . . . ? C37 P2 C36 C35 -80.2(6) . . . . ? Pd1 P2 C36 C35 44.3(6) . . . . ? C43 P2 C36 C49 -15.9(6) . . . . ? C37 P2 C36 C49 91.6(6) . . . . ? Pd1 P2 C36 C49 -143.9(5) . . . . ? C43 P2 C37 C38 83.8(5) . . . . ? C36 P2 C37 C38 -23.7(5) . . . . ? Pd1 P2 C37 C38 -150.6(4) . . . . ? C43 P2 C37 C42 -87.8(5) . . . . ? C36 P2 C37 C42 164.8(4) . . . . ? Pd1 P2 C37 C42 37.8(5) . . . . ? C42 C37 C38 C39 1.7(8) . . . . ? P2 C37 C38 C39 -169.7(4) . . . . ? C37 C38 C39 C40 0.0(9) . . . . ? C38 C39 C40 C41 -1.2(9) . . . . ? C39 C40 C41 C42 0.7(9) . . . . ? C40 C41 C42 C37 1.0(8) . . . . ? C38 C37 C42 C41 -2.1(8) . . . . ? P2 C37 C42 C41 169.5(4) . . . . ? C36 P2 C43 C44 95.2(5) . . . . ? C37 P2 C43 C44 -13.2(5) . . . . ? Pd1 P2 C43 C44 -136.5(4) . . . . ? C36 P2 C43 C48 -79.5(5) . . . . ? C37 P2 C43 C48 172.1(5) . . . . ? Pd1 P2 C43 C48 48.8(5) . . . . ? C48 C43 C44 C45 0.4(8) . . . . ? P2 C43 C44 C45 -174.3(4) . . . . ? C43 C44 C45 C46 1.2(9) . . . . ? C44 C45 C46 C47 -2.6(9) . . . . ? C45 C46 C47 C48 2.4(9) . . . . ? C46 C47 C48 C43 -0.8(9) . . . . ? C44 C43 C48 C47 -0.6(9) . . . . ? P2 C43 C48 C47 174.2(5) . . . . ? C35 C36 C49 C50 1.5(10) . . . . ? P2 C36 C49 C50 -170.5(5) . . . . ? C36 C49 C50 C51 3.6(11) . . . . ? C49 C50 C51 C52 -3.1(11) . . . . ? C50 C51 C52 C35 -2.4(9) . . . . ? C50 C51 C52 C53 171.8(6) . . . . ? C36 C35 C52 C51 7.6(9) . . . . ? O34 C35 C52 C51 -177.1(5) . . . . ? C36 C35 C52 C53 -166.4(6) . . . . ? O34 C35 C52 C53 8.9(9) . . . . ? C51 C52 C53 C55 -117.3(6) . . . . ? C35 C52 C53 C55 56.5(8) . . . . ? C51 C52 C53 C54 119.0(6) . . . . ? C35 C52 C53 C54 -67.3(7) . . . . ? C51 C52 C53 C56 -0.8(8) . . . . ? C35 C52 C53 C56 172.9(6) . . . . ? _diffrn_measured_fraction_theta_max 0.949 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.949 _refine_diff_density_max 0.594 _refine_diff_density_min -0.733 _refine_diff_density_rms 0.096