# Copyright The Royal Society of Chemistry, 1998 # CCDC Number: 186/1182 # Palladium(II) complexes of 2-pyridyldiphenylphosphine # Peter G. Edwards et al data_805102J _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety Pd2(mu-Ph2Ppy)2(O2CCF3)2 _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C78 H68 Cl2 N4 O8 P4 Pd4' _chemical_formula_weight 1809.74 _chemical_melting_point ? _chemical_compound_source ? 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' 'N' 'N' 0.0061 0.0033 '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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M P2(1)/a 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 12.532(2) _cell_length_b 20.159(4) _cell_length_c 14.7610(6) _cell_angle_alpha 90.00 _cell_angle_beta 104.24(3) _cell_angle_gamma 90.00 _cell_volume 3614.7(10) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2)K _cell_measurement_reflns_used 250 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.145 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.663 _exptl_crystal_density_method ? _exptl_crystal_F_000 1812 _exptl_absorpt_coefficient_mu 1.201 _exptl_absorpt_correction_type DIFABS _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2)K _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Nonius FR571 rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'FAST TV Area detector ' _diffrn_measurement_method ' Phi scans' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14885 _diffrn_reflns_av_R_equivalents 0.0959 _diffrn_reflns_av_sigmaI/netI 0.0972 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.75 _diffrn_reflns_theta_max 25.01 _reflns_number_total 5391 _reflns_number_observed 4284 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'MADNES (Pflugrath, 1989)' _computing_cell_refinement 'REFINE in MADNES' _computing_data_reduction ABSURD _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-92 (Sheldrick, 1993)' _computing_molecular_graphics SNPI _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 8 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0491P)^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 'Riding model' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5383 _refine_ls_number_parameters 455 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0630 _refine_ls_R_factor_obs 0.0478 _refine_ls_wR_factor_all 0.1143 _refine_ls_wR_factor_obs 0.1067 _refine_ls_goodness_of_fit_all 1.027 _refine_ls_goodness_of_fit_obs 1.130 _refine_ls_restrained_S_all 1.070 _refine_ls_restrained_S_obs 1.130 _refine_ls_shift/esd_max 0.124 _refine_ls_shift/esd_mean 0.004 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Pd1 Pd 0.21226(3) 0.13004(2) 0.17225(3) 0.01520(14) Uani 1 d . . Pd2 Pd 0.07049(3) 0.03978(2) 0.18422(3) 0.01659(14) Uani 1 d . . N1 N 0.1892(4) -0.0309(2) 0.2495(3) 0.0196(11) Uani 1 d . . N2 N 0.1101(4) 0.1732(2) 0.0508(3) 0.0185(11) Uani 1 d . . P1 P 0.30365(12) 0.07949(7) 0.29966(10) 0.0169(3) Uani 1 d . . P2 P -0.04309(12) 0.12113(7) 0.12659(10) 0.0173(3) Uani 1 d . . O1 O 0.3379(3) 0.2068(2) 0.1810(3) 0.0206(9) Uani 1 d . . O2 O 0.3946(3) 0.1606(2) 0.0654(3) 0.0361(11) Uani 1 d . . O3 O -0.0486(3) -0.0380(2) 0.1698(3) 0.0292(10) Uani 1 d . . O4 O -0.1492(3) 0.0141(2) 0.2506(3) 0.0397(11) Uani 1 d . . C1 C 0.3718(5) -0.0554(3) 0.3352(4) 0.0298(15) Uani 1 d . . H1 H 0.4414(5) -0.0406(3) 0.3666(4) 0.036 Uiso 1 calc R . C2 C 0.3488(5) -0.1224(3) 0.3273(5) 0.034(2) Uani 1 d . . H2 H 0.4029(5) -0.1533(3) 0.3528(5) 0.041 Uiso 1 calc R . C3 C 0.2470(5) -0.1424(3) 0.2822(4) 0.032(2) Uani 1 d . . H3 H 0.2302(5) -0.1874(3) 0.2776(4) 0.038 Uiso 1 calc R . C4 C 0.1677(5) -0.0964(3) 0.2427(4) 0.0280(14) Uani 1 d . . H4 H 0.0982(5) -0.1109(3) 0.2109(4) 0.034 Uiso 1 calc R . C5 C 0.2901(5) -0.0107(3) 0.2959(4) 0.0195(13) Uani 1 d . . C6 C 0.4525(4) 0.0867(3) 0.3242(4) 0.0184(13) Uani 1 d . . C7 C 0.5029(5) 0.0726(3) 0.2520(4) 0.0294(15) Uani 1 d . . H7 H 0.4595(5) 0.0648(3) 0.1921(4) 0.035 Uiso 1 calc R . C8 C 0.6159(5) 0.0700(3) 0.2679(4) 0.033(2) Uani 1 d . . H8 H 0.6486(5) 0.0584(3) 0.2200(4) 0.039 Uiso 1 calc R . C9 C 0.6794(5) 0.0847(3) 0.3552(5) 0.036(2) Uani 1 d . . H9 H 0.7556(5) 0.0836(3) 0.3658(5) 0.043 Uiso 1 calc R . C10 C 0.6334(5) 0.1010(3) 0.4270(5) 0.033(2) Uani 1 d . . H10 H 0.6777(5) 0.1113(3) 0.4856(5) 0.039 Uiso 1 calc R . C11 C 0.5190(5) 0.1018(3) 0.4110(4) 0.0274(14) Uani 1 d . . H11 H 0.4870(5) 0.1127(3) 0.4596(4) 0.033 Uiso 1 calc R . C12 C 0.2676(4) 0.1044(3) 0.4065(4) 0.0192(12) Uani 1 d . . C13 C 0.2882(5) 0.0655(3) 0.4857(4) 0.032(2) Uani 1 d . . H13 H 0.3211(5) 0.0242(3) 0.4853(4) 0.039 Uiso 1 calc R . C14 C 0.2605(6) 0.0874(4) 0.5665(4) 0.040(2) Uani 1 d . . H14 H 0.2736(6) 0.0607(4) 0.6195(4) 0.048 Uiso 1 calc R . C15 C 0.2143(6) 0.1482(3) 0.5671(5) 0.039(2) Uani 1 d . . H15 H 0.1977(6) 0.1635(3) 0.6215(5) 0.047 Uiso 1 calc R . C16 C 0.1915(5) 0.1875(3) 0.4887(4) 0.032(2) Uani 1 d . . H16 H 0.1588(5) 0.2288(3) 0.4901(4) 0.038 Uiso 1 calc R . C17 C 0.2170(5) 0.1657(3) 0.4077(4) 0.0225(13) Uani 1 d . . H17 H 0.2004(5) 0.1920(3) 0.3542(4) 0.027 Uiso 1 calc R . C18 C 0.4003(5) 0.2013(3) 0.1297(4) 0.0254(14) Uani 1 d . . C19 C 0.4959(6) 0.2516(4) 0.1458(5) 0.050(2) Uani 1 d . . H19A H 0.5081(25) 0.2648(18) 0.0867(5) 0.075 Uiso 1 calc R . H19B H 0.5615(10) 0.2314(8) 0.1831(27) 0.075 Uiso 1 calc R . H19C H 0.4776(16) 0.2899(10) 0.1777(29) 0.075 Uiso 1 calc R . C20 C -0.0001(5) 0.1697(3) 0.0367(4) 0.0186(13) Uani 1 d . . C21 C 0.1497(5) 0.2057(3) -0.0132(4) 0.0238(13) Uani 1 d . . H21 H 0.2256(5) 0.2086(3) -0.0046(4) 0.029 Uiso 1 calc R . C22 C 0.0834(5) 0.2346(3) -0.0906(4) 0.0260(14) Uani 1 d . . H22 H 0.1143(5) 0.2561(3) -0.1337(4) 0.031 Uiso 1 calc R . C23 C -0.0288(5) 0.2318(3) -0.1046(4) 0.0253(14) Uani 1 d . . H23 H -0.0749(5) 0.2519(3) -0.1563(4) 0.030 Uiso 1 calc R . C24 C -0.0714(5) 0.1984(3) -0.0401(4) 0.0229(13) Uani 1 d . . H24 H -0.1471(5) 0.1952(3) -0.0479(4) 0.027 Uiso 1 calc R . C25 C -0.1804(4) 0.0954(3) 0.0635(4) 0.0189(13) Uani 1 d . . C26 C -0.1893(5) 0.0422(3) 0.0018(4) 0.0276(15) Uani 1 d . . H26 H -0.1262(5) 0.0211(3) -0.0061(4) 0.033 Uiso 1 calc R . C27 C -0.2912(5) 0.0211(3) -0.0474(4) 0.034(2) Uani 1 d . . H27 H -0.2971(5) -0.0155(3) -0.0867(4) 0.041 Uiso 1 calc R . C28 C -0.3845(5) 0.0536(3) -0.0388(4) 0.034(2) Uani 1 d . . H28 H -0.4530(5) 0.0396(3) -0.0737(4) 0.041 Uiso 1 calc R . C29 C -0.3780(5) 0.1062(3) 0.0202(4) 0.033(2) Uani 1 d . . H29 H -0.4416(5) 0.1281(3) 0.0256(4) 0.040 Uiso 1 calc R . C30 C -0.2748(4) 0.1271(3) 0.0726(4) 0.0209(13) Uani 1 d . . H30 H -0.2698(4) 0.1626(3) 0.1137(4) 0.025 Uiso 1 calc R . C31 C -0.0603(4) 0.1836(3) 0.2119(4) 0.0178(13) Uani 1 d . . C32 C -0.0620(6) 0.2498(3) 0.1945(5) 0.042(2) Uani 1 d . . H32 H -0.0563(6) 0.2650(3) 0.1364(5) 0.050 Uiso 1 calc R . C33 C -0.0721(6) 0.2950(3) 0.2630(5) 0.052(2) Uani 1 d . . H33 H -0.0707(6) 0.3403(3) 0.2511(5) 0.062 Uiso 1 calc R . C34 C -0.0840(5) 0.2735(3) 0.3470(4) 0.032(2) Uani 1 d . . H34 H -0.0902(5) 0.3039(3) 0.3928(4) 0.038 Uiso 1 calc R . C35 C -0.0869(6) 0.2076(3) 0.3641(5) 0.040(2) Uani 1 d . . H35 H -0.0982(6) 0.1927(3) 0.4207(5) 0.048 Uiso 1 calc R . C36 C -0.0728(5) 0.1623(3) 0.2967(4) 0.035(2) Uani 1 d . . H36 H -0.0719(5) 0.1171(3) 0.3095(4) 0.042 Uiso 1 calc R . C37 C -0.1307(5) -0.0317(3) 0.2020(4) 0.0275(15) Uani 1 d . . C38 C -0.2166(6) -0.0864(3) 0.1760(5) 0.045(2) Uani 1 d . . H38A H -0.1835(11) -0.1283(4) 0.1974(27) 0.067 Uiso 1 calc R . H38B H -0.2445(26) -0.0876(14) 0.1094(6) 0.067 Uiso 1 calc R . H38C H -0.2759(18) -0.0777(12) 0.2050(26) 0.067 Uiso 1 calc R . Cl1S Cl 0.0606(6) -0.0608(4) 0.4499(5) 0.074(2) Uiso 0.50 d P . Cl3S Cl 0.0487(12) -0.0529(8) 0.4708(10) 0.129(5) Uiso 0.40 d P . Cl4S Cl -0.0027(17) 0.0138(12) 0.4570(15) 0.039(5) Uiso 0.10 d P . C1S C 0.0286(9) -0.0187(6) 0.4354(8) 0.043(3) Uiso 0.75 d P . C2S C -0.0064(55) 0.0310(35) 0.4298(50) 0.135(27) Uiso 0.25 d P . 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 0.0143(3) 0.0161(2) 0.0149(2) 0.0011(2) 0.0029(2) -0.0008(2) Pd2 0.0138(3) 0.0158(3) 0.0203(3) 0.0009(2) 0.0045(2) -0.0002(2) N1 0.017(3) 0.021(3) 0.021(3) 0.003(2) 0.005(2) 0.001(2) N2 0.017(3) 0.018(3) 0.021(3) -0.005(2) 0.005(2) -0.000(2) P1 0.0169(9) 0.0163(8) 0.0169(8) 0.0010(6) 0.0031(6) -0.0004(6) P2 0.0165(9) 0.0173(8) 0.0179(8) -0.0003(6) 0.0039(6) 0.0004(6) O1 0.018(2) 0.021(2) 0.018(2) 0.001(2) -0.004(2) -0.005(2) O2 0.027(3) 0.051(3) 0.030(3) -0.006(2) 0.008(2) 0.008(2) O3 0.026(3) 0.018(2) 0.042(3) -0.004(2) 0.006(2) -0.003(2) O4 0.033(3) 0.040(3) 0.049(3) -0.008(2) 0.014(2) -0.003(2) C1 0.027(4) 0.025(4) 0.033(4) 0.001(3) -0.001(3) 0.007(3) C2 0.031(4) 0.019(4) 0.047(4) 0.004(3) 0.003(3) 0.011(3) C3 0.041(5) 0.012(3) 0.040(4) 0.003(3) 0.007(3) 0.003(3) C4 0.029(4) 0.020(3) 0.033(4) 0.003(3) 0.005(3) -0.001(3) C5 0.024(4) 0.020(3) 0.015(3) 0.003(2) 0.006(3) 0.004(2) C6 0.019(4) 0.015(3) 0.019(3) 0.007(2) 0.001(3) 0.003(2) C7 0.022(4) 0.041(4) 0.024(4) 0.001(3) 0.004(3) -0.001(3) C8 0.018(4) 0.051(4) 0.030(4) 0.008(3) 0.010(3) 0.009(3) C9 0.014(4) 0.036(4) 0.055(5) 0.017(3) 0.005(3) 0.004(3) C10 0.015(4) 0.037(4) 0.040(4) 0.011(3) -0.005(3) 0.000(3) C11 0.024(4) 0.030(4) 0.027(4) 0.002(3) 0.005(3) 0.000(3) C12 0.021(3) 0.017(3) 0.019(3) -0.001(2) 0.005(2) -0.004(2) C13 0.045(4) 0.028(4) 0.025(4) -0.002(3) 0.009(3) 0.009(3) C14 0.046(5) 0.054(5) 0.024(4) 0.004(3) 0.013(3) 0.007(3) C15 0.051(5) 0.044(5) 0.025(4) -0.006(3) 0.017(3) 0.006(3) C16 0.033(4) 0.029(4) 0.034(4) -0.007(3) 0.007(3) 0.008(3) C17 0.020(4) 0.022(3) 0.024(3) 0.003(3) 0.003(3) 0.002(2) C18 0.024(4) 0.023(3) 0.023(3) 0.000(3) -0.006(3) 0.000(3) C19 0.043(5) 0.072(6) 0.039(5) -0.004(4) 0.017(4) -0.026(4) C20 0.021(4) 0.013(3) 0.021(3) -0.003(2) 0.004(3) -0.000(2) C21 0.022(4) 0.024(3) 0.027(3) 0.006(3) 0.009(3) -0.005(3) C22 0.033(4) 0.028(4) 0.018(3) 0.003(3) 0.006(3) -0.002(3) C23 0.025(4) 0.026(4) 0.021(3) 0.005(3) -0.003(3) 0.002(3) C24 0.018(3) 0.022(3) 0.027(3) 0.006(3) 0.002(3) 0.004(2) C25 0.017(3) 0.020(3) 0.019(3) 0.000(2) 0.004(3) -0.001(2) C26 0.026(4) 0.033(4) 0.026(4) -0.003(3) 0.010(3) 0.001(3) C27 0.030(4) 0.041(4) 0.027(4) -0.012(3) -0.000(3) -0.005(3) C28 0.016(4) 0.055(5) 0.030(4) -0.009(3) 0.001(3) -0.007(3) C29 0.020(4) 0.047(4) 0.033(4) -0.001(3) 0.005(3) 0.005(3) C30 0.016(4) 0.027(3) 0.020(3) -0.003(2) 0.004(3) 0.003(2) C31 0.007(3) 0.024(3) 0.022(3) -0.003(2) 0.003(2) 0.004(2) C32 0.072(5) 0.031(4) 0.031(4) 0.002(3) 0.027(4) -0.000(3) C33 0.087(6) 0.023(4) 0.054(5) -0.001(3) 0.034(4) 0.006(4) C34 0.028(4) 0.039(4) 0.029(4) -0.012(3) 0.007(3) 0.004(3) C35 0.057(5) 0.040(4) 0.028(4) -0.008(3) 0.018(3) -0.004(3) C36 0.054(5) 0.021(3) 0.032(4) -0.001(3) 0.014(3) -0.005(3) C37 0.042(4) 0.018(3) 0.024(3) 0.004(3) 0.012(3) 0.003(3) C38 0.045(5) 0.043(5) 0.052(5) -0.009(4) 0.024(4) -0.018(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 N2 2.117(5) . ? Pd1 O1 2.189(3) . ? Pd1 P1 2.197(2) . ? Pd1 Pd2 2.5795(7) . ? Pd2 N1 2.114(4) . ? Pd2 O3 2.139(4) . ? Pd2 P2 2.201(2) . ? N1 C5 1.344(7) . ? N1 C4 1.346(7) . ? N2 C21 1.341(6) . ? N2 C20 1.347(7) . ? P1 C12 1.815(5) . ? P1 C6 1.816(6) . ? P1 C5 1.826(6) . ? P2 C25 1.819(6) . ? P2 C31 1.831(5) . ? P2 C20 1.833(5) . ? O1 C18 1.220(7) . ? O2 C18 1.245(7) . ? O3 C37 1.242(7) . ? O4 C37 1.227(7) . ? C1 C2 1.379(8) . ? C1 C5 1.381(8) . ? C2 C3 1.347(9) . ? C3 C4 1.379(8) . ? C6 C11 1.380(8) . ? C6 C7 1.395(7) . ? C7 C8 1.379(8) . ? C8 C9 1.370(9) . ? C9 C10 1.364(9) . ? C10 C11 1.395(8) . ? C12 C13 1.379(8) . ? C12 C17 1.392(8) . ? C13 C14 1.394(8) . ? C14 C15 1.355(9) . ? C15 C16 1.374(9) . ? C16 C17 1.383(8) . ? C18 C19 1.542(8) . ? C20 C24 1.386(8) . ? C21 C22 1.366(8) . ? C22 C23 1.371(8) . ? C23 C24 1.376(7) . ? C25 C30 1.380(7) . ? C25 C26 1.393(8) . ? C26 C27 1.373(8) . ? C27 C28 1.374(9) . ? C28 C29 1.362(9) . ? C29 C30 1.398(8) . ? C31 C32 1.358(8) . ? C31 C36 1.368(8) . ? C32 C33 1.390(9) . ? C33 C34 1.357(9) . ? C34 C35 1.353(9) . ? C35 C36 1.395(8) . ? C37 C38 1.521(9) . ? Cl1S C1S 0.942(14) . ? Cl1S Cl4S 1.72(2) . ? Cl1S Cl4S 1.95(2) 3_556 ? Cl1S C2S 2.02(7) . ? Cl1S C2S 2.14(7) 3_556 ? Cl3S C1S 0.86(2) . ? Cl3S Cl4S 1.48(3) . ? Cl3S Cl4S 1.55(2) 3_556 ? Cl3S C2S 1.74(7) 3_556 ? Cl3S C2S 1.87(7) . ? Cl4S C2S 0.52(7) . ? Cl4S C1S 0.86(2) . ? Cl4S Cl4S 1.37(4) 3_556 ? Cl4S Cl3S 1.55(2) 3_556 ? Cl4S C1S 1.70(2) 3_556 ? Cl4S C2S 1.88(7) 3_556 ? Cl4S Cl1S 1.95(2) 3_556 ? C1S C2S 1.09(7) . ? C1S Cl4S 1.70(2) 3_556 ? C2S Cl3S 1.74(7) 3_556 ? C2S Cl4S 1.88(7) 3_556 ? C2S Cl1S 2.14(7) 3_556 ? 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 N2 Pd1 O1 92.1(2) . . ? N2 Pd1 P1 174.20(12) . . ? O1 Pd1 P1 93.52(10) . . ? N2 Pd1 Pd2 93.71(12) . . ? O1 Pd1 Pd2 172.90(10) . . ? P1 Pd1 Pd2 80.61(4) . . ? N1 Pd2 O3 86.9(2) . . ? N1 Pd2 P2 173.94(13) . . ? O3 Pd2 P2 97.98(11) . . ? N1 Pd2 Pd1 95.03(12) . . ? O3 Pd2 Pd1 170.34(11) . . ? P2 Pd2 Pd1 80.72(4) . . ? C5 N1 C4 118.8(5) . . ? C5 N1 Pd2 119.7(4) . . ? C4 N1 Pd2 121.5(4) . . ? C21 N2 C20 117.4(5) . . ? C21 N2 Pd1 123.1(4) . . ? C20 N2 Pd1 119.5(3) . . ? C12 P1 C6 105.5(3) . . ? C12 P1 C5 105.1(2) . . ? C6 P1 C5 99.8(2) . . ? C12 P1 Pd1 115.3(2) . . ? C6 P1 Pd1 115.3(2) . . ? C5 P1 Pd1 114.3(2) . . ? C25 P2 C31 106.9(2) . . ? C25 P2 C20 101.1(3) . . ? C31 P2 C20 103.6(2) . . ? C25 P2 Pd2 115.2(2) . . ? C31 P2 Pd2 114.9(2) . . ? C20 P2 Pd2 113.6(2) . . ? C18 O1 Pd1 117.4(4) . . ? C37 O3 Pd2 120.7(4) . . ? C2 C1 C5 119.0(6) . . ? C3 C2 C1 119.2(6) . . ? C2 C3 C4 120.2(6) . . ? N1 C4 C3 121.2(6) . . ? N1 C5 C1 121.5(5) . . ? N1 C5 P1 112.8(4) . . ? C1 C5 P1 125.7(5) . . ? C11 C6 C7 118.1(5) . . ? C11 C6 P1 124.0(4) . . ? C7 C6 P1 117.9(4) . . ? C8 C7 C6 121.1(6) . . ? C9 C8 C7 119.1(6) . . ? C10 C9 C8 121.6(6) . . ? C9 C10 C11 119.0(6) . . ? C6 C11 C10 121.0(6) . . ? C13 C12 C17 119.1(5) . . ? C13 C12 P1 123.0(4) . . ? C17 C12 P1 117.9(4) . . ? C12 C13 C14 120.7(6) . . ? C15 C14 C13 119.3(6) . . ? C14 C15 C16 121.1(6) . . ? C15 C16 C17 120.1(6) . . ? C16 C17 C12 119.7(5) . . ? O1 C18 O2 127.5(6) . . ? O1 C18 C19 115.9(5) . . ? O2 C18 C19 116.6(5) . . ? N2 C20 C24 122.3(5) . . ? N2 C20 P2 112.9(4) . . ? C24 C20 P2 124.7(4) . . ? N2 C21 C22 122.9(5) . . ? C21 C22 C23 119.9(5) . . ? C22 C23 C24 118.3(5) . . ? C23 C24 C20 119.2(5) . . ? C30 C25 C26 119.2(5) . . ? C30 C25 P2 122.9(4) . . ? C26 C25 P2 117.9(4) . . ? C27 C26 C25 119.9(5) . . ? C26 C27 C28 120.3(6) . . ? C29 C28 C27 120.9(6) . . ? C28 C29 C30 119.3(6) . . ? C25 C30 C29 120.4(5) . . ? C32 C31 C36 118.8(5) . . ? C32 C31 P2 123.0(4) . . ? C36 C31 P2 118.2(4) . . ? C31 C32 C33 120.5(6) . . ? C34 C33 C32 120.3(6) . . ? C35 C34 C33 119.9(6) . . ? C34 C35 C36 119.8(6) . . ? C31 C36 C35 120.6(6) . . ? O4 C37 O3 126.4(6) . . ? O4 C37 C38 118.0(6) . . ? O3 C37 C38 115.6(5) . . ? C1S Cl1S Cl4S 17.3(10) . . ? C1S Cl1S Cl4S 60.6(9) . 3_556 ? Cl4S Cl1S Cl4S 43.3(13) . 3_556 ? C1S Cl1S C2S 4.6(23) . . ? Cl4S Cl1S C2S 13.1(22) . . ? Cl4S Cl1S C2S 56.3(22) 3_556 . ? C1S Cl1S C2S 74.3(20) . 3_556 ? Cl4S Cl1S C2S 57.0(20) . 3_556 ? Cl4S Cl1S C2S 13.8(20) 3_556 3_556 ? C2S Cl1S C2S 70.0(31) . 3_556 ? C1S Cl3S Cl4S 30.8(13) . . ? C1S Cl3S Cl4S 84.6(16) . 3_556 ? Cl4S Cl3S Cl4S 53.8(16) . 3_556 ? C1S Cl3S C2S 101.7(28) . 3_556 ? Cl4S Cl3S C2S 70.8(26) . 3_556 ? Cl4S Cl3S C2S 17.1(24) 3_556 3_556 ? C1S Cl3S C2S 18.8(26) . . ? Cl4S Cl3S C2S 12.2(25) . . ? Cl4S Cl3S C2S 65.8(26) 3_556 . ? C2S Cl3S C2S 83.0(34) 3_556 . ? C2S Cl4S C1S 100.4(92) . . ? C2S Cl4S Cl4S 162.2(100) . 3_556 ? C1S Cl4S Cl4S 96.4(29) . 3_556 ? C2S Cl4S Cl3S 131.2(95) . . ? C1S Cl4S Cl3S 30.9(13) . . ? Cl4S Cl4S Cl3S 65.5(19) 3_556 . ? C2S Cl4S Cl3S 102.3(95) . 3_556 ? C1S Cl4S Cl3S 157.1(25) . 3_556 ? Cl4S Cl4S Cl3S 60.7(17) 3_556 3_556 ? Cl3S Cl4S Cl3S 126.2(16) . 3_556 ? C2S Cl4S C1S 132.5(97) . 3_556 ? C1S Cl4S C1S 126.7(23) . 3_556 ? Cl4S Cl4S C1S 30.3(12) 3_556 3_556 ? Cl3S Cl4S C1S 95.8(13) . 3_556 ? Cl3S Cl4S C1S 30.4(8) 3_556 3_556 ? C2S Cl4S Cl1S 119.2(95) . . ? C1S Cl4S Cl1S 18.9(13) . . ? Cl4S Cl4S Cl1S 77.5(20) 3_556 . ? Cl3S Cl4S Cl1S 12.0(7) . . ? Cl3S Cl4S Cl1S 138.2(17) 3_556 . ? C1S Cl4S Cl1S 107.8(14) 3_556 . ? C2S Cl4S C2S 167.1(79) . 3_556 ? C1S Cl4S C2S 91.8(26) . 3_556 ? Cl4S Cl4S C2S 4.9(30) 3_556 3_556 ? Cl3S Cl4S C2S 60.9(22) . 3_556 ? Cl3S Cl4S C2S 65.4(21) 3_556 3_556 ? C1S Cl4S C2S 35.0(21) 3_556 3_556 ? Cl1S Cl4S C2S 72.9(22) . 3_556 ? C2S Cl4S Cl1S 103.9(95) . 3_556 ? C1S Cl4S Cl1S 155.6(24) . 3_556 ? Cl4S Cl4S Cl1S 59.2(16) 3_556 3_556 ? Cl3S Cl4S Cl1S 124.7(14) . 3_556 ? Cl3S Cl4S Cl1S 1.6(8) 3_556 3_556 ? C1S Cl4S Cl1S 28.9(6) 3_556 3_556 ? Cl1S Cl4S Cl1S 136.7(13) . 3_556 ? C2S Cl4S Cl1S 63.8(21) 3_556 3_556 ? Cl4S C1S Cl3S 118.3(24) . . ? Cl4S C1S Cl1S 143.8(22) . . ? Cl3S C1S Cl1S 25.5(12) . . ? Cl4S C1S C2S 28.3(40) . . ? Cl3S C1S C2S 146.4(44) . . ? Cl1S C1S C2S 171.5(43) . . ? Cl4S C1S Cl4S 53.3(23) . 3_556 ? Cl3S C1S Cl4S 65.0(13) . 3_556 ? Cl1S C1S Cl4S 90.5(11) . 3_556 ? C2S C1S Cl4S 81.4(43) . 3_556 ? Cl4S C2S C1S 51.3(72) . . ? Cl4S C2S Cl3S 60.6(85) . 3_556 ? C1S C2S Cl3S 111.8(51) . 3_556 ? Cl4S C2S Cl3S 36.6(75) . . ? C1S C2S Cl3S 14.8(19) . . ? Cl3S C2S Cl3S 97.0(34) 3_556 . ? Cl4S C2S Cl4S 12.9(79) . 3_556 ? C1S C2S Cl4S 63.6(36) . 3_556 ? Cl3S C2S Cl4S 48.3(18) 3_556 3_556 ? Cl3S C2S Cl4S 48.8(19) . 3_556 ? Cl4S C2S Cl1S 47.7(80) . . ? C1S C2S Cl1S 4.0(20) . . ? Cl3S C2S Cl1S 108.1(35) 3_556 . ? Cl3S C2S Cl1S 11.1(7) . . ? Cl4S C2S Cl1S 59.9(21) 3_556 . ? Cl4S C2S Cl1S 62.4(87) . 3_556 ? C1S C2S Cl1S 113.6(48) . 3_556 ? Cl3S C2S Cl1S 1.8(9) 3_556 3_556 ? Cl3S C2S Cl1S 98.9(31) . 3_556 ? Cl4S C2S Cl1S 50.1(16) 3_556 3_556 ? Cl1S C2S Cl1S 110.0(31) . 3_556 ? _refine_diff_density_max 1.956 _refine_diff_density_min -0.992 _refine_diff_density_rms 0.196 #=END data_2 _audit_creation_method SHELXL _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety Pd2(mu-Ph2Ppy)2(OAc)2 _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C19.25 H14 Cl0.50 F3 N O2 P Pd' _chemical_formula_weight 503.41 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pd' 'Pd' -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M P2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 12.413(9) _cell_length_b 20.703(10) _cell_length_c 15.580(9) _cell_angle_alpha 90.00 _cell_angle_beta 108.53(10) _cell_angle_gamma 90.00 _cell_volume 3796.3(40) _cell_formula_units_Z 8 _cell_measurement_temperature 120(2)K _cell_measurement_reflns_used 250 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.762 _exptl_crystal_density_method ? _exptl_crystal_F_000 1992 _exptl_absorpt_coefficient_mu 1.176 _exptl_absorpt_correction_type DIFABS _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Nonius FR571 rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'FAST TV Area Detector' _diffrn_measurement_method 'Phi Scans' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16331 _diffrn_reflns_av_R_equivalents 0.0689 _diffrn_reflns_av_sigmaI/netI 0.0681 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.84 _diffrn_reflns_theta_max 25.03 _reflns_number_total 9636 _reflns_number_observed 8930 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'MADNES (Pflugrath, 1989)' _computing_cell_refinement 'REFINE in MADNES' _computing_data_reduction ABSURD _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-92 (Sheldrick, 1993)' _computing_molecular_graphics SNPI _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 8 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 fullcycle _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0598P)^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 'Riding model' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.02(3) _refine_ls_number_reflns 9628 _refine_ls_number_parameters 1000 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0472 _refine_ls_R_factor_obs 0.0438 _refine_ls_wR_factor_all 0.1112 _refine_ls_wR_factor_obs 0.1078 _refine_ls_goodness_of_fit_all 1.059 _refine_ls_goodness_of_fit_obs 1.092 _refine_ls_restrained_S_all 1.081 _refine_ls_restrained_S_obs 1.092 _refine_ls_shift/esd_max -0.071 _refine_ls_shift/esd_mean 0.013 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Cl1 Cl -0.2682(3) 0.3866(2) -0.6759(2) 0.0613(8) Uani 1 d . . Cl2 Cl -0.2101(2) 0.3083(2) 0.1901(2) 0.0624(8) Uani 1 d . . C80 C -0.2701(10) 0.3815(5) -0.7891(6) 0.049(3) Uani 1 d . . F1 F -0.0659(4) 0.5149(2) -0.4568(4) 0.0357(13) Uani 1 d . . F2 F 0.0330(5) 0.4690(3) -0.3337(3) 0.0421(15) Uani 1 d . . F3 F 0.0647(4) 0.4464(3) -0.4563(4) 0.0347(13) Uani 1 d . . F4 F -0.7322(8) 0.0796(5) -0.4560(7) 0.127(4) Uani 1 d . . F5 F -0.6828(9) 0.0745(5) -0.3259(7) 0.133(4) Uani 1 d . . F6 F -0.8184(7) 0.1329(4) -0.3961(11) 0.162(6) Uani 1 d . . F7 F -0.2528(7) 0.1281(3) 0.1824(4) 0.074(2) Uani 1 d . . F8 F -0.2228(4) 0.1770(3) 0.0686(4) 0.0388(13) Uani 1 d . . F9 F -0.3534(5) 0.1063(3) 0.0498(5) 0.059(2) Uani 1 d . . F10 F 0.5516(5) -0.1922(3) 0.0189(5) 0.063(2) Uani 1 d . . F11 F 0.5221(5) -0.2101(3) 0.1434(4) 0.062(2) Uani 1 d . . F12 F 0.4251(5) -0.2587(3) 0.0249(5) 0.067(2) Uani 1 d . . Pd1 Pd -0.45241(5) 0.25244(7) -0.41013(4) 0.0271(2) Uani 1 d . . Pd2 Pd -0.31113(5) 0.34005(7) -0.41999(4) 0.01621(15) Uani 1 d . . Pd3 Pd 0.02632(5) 0.00080(7) 0.05869(4) 0.0168(2) Uani 1 d . . Pd4 Pd 0.17370(5) -0.08383(7) 0.05215(4) 0.0178(2) Uani 1 d . . P1 P -0.5547(2) 0.29944(12) -0.53605(14) 0.0212(5) Uani 1 d . . P2 P -0.1904(2) 0.26049(12) -0.36225(13) 0.0166(5) Uani 1 d . . P3 P 0.2888(2) -0.00236(12) 0.11257(13) 0.0199(5) Uani 1 d . . P4 P -0.0644(2) -0.04572(12) -0.07125(14) 0.0173(5) Uani 1 d . . O1 O -0.1860(4) 0.4165(3) -0.4079(4) 0.0245(13) Uani 1 d . . O2 O -0.0912(5) 0.3566(3) -0.4796(4) 0.0295(15) Uani 1 d . . O3 O -0.5772(6) 0.1670(4) -0.4293(5) 0.055(2) Uani 1 d . . O4 O -0.6411(8) 0.2131(5) -0.3242(7) 0.087(3) Uani 1 d . . O5 O -0.0987(4) 0.0774(3) 0.0549(3) 0.0198(13) Uani 1 d . . O6 O -0.1734(5) 0.0164(3) 0.1406(4) 0.036(2) Uani 1 d . . O7 O 0.3007(4) -0.1582(3) 0.0670(4) 0.0222(13) Uani 1 d . . O8 O 0.3960(5) -0.1029(3) -0.0102(4) 0.0242(14) Uani 1 d . . N1 N -0.4384(5) 0.4080(3) -0.4839(4) 0.020(2) Uani 1 d . . N2 N -0.3417(6) 0.2130(4) -0.2894(4) 0.024(2) Uani 1 d . . N3 N 0.0514(5) -0.1546(3) -0.0136(4) 0.0181(14) Uani 1 d . . N4 N 0.1310(5) 0.0395(3) 0.1841(4) 0.021(2) Uani 1 d . . C1 C -0.4182(8) 0.4729(4) -0.4736(6) 0.032(2) Uani 1 d . . H1 H -0.3449(8) 0.4874(4) -0.4439(6) 0.038 Uiso 1 calc R . C2 C -0.5043(8) 0.5173(4) -0.5063(7) 0.040(2) Uani 1 d . . H2 H -0.4887(8) 0.5612(4) -0.4983(7) 0.048 Uiso 1 calc R . C3 C -0.6129(8) 0.4969(4) -0.5506(6) 0.038(2) Uani 1 d . . H3 H -0.6712(8) 0.5268(4) -0.5724(6) 0.045 Uiso 1 calc R . C4 C -0.6352(7) 0.4306(4) -0.5629(6) 0.030(2) Uani 1 d . . H4 H -0.7085(7) 0.4159(4) -0.5925(6) 0.037 Uiso 1 calc R . C5 C -0.5466(6) 0.3870(4) -0.5302(5) 0.021(2) Uani 1 d . . C6 C -0.7079(6) 0.2877(4) -0.5628(5) 0.017(2) Uani 1 d . . C7 C -0.7556(7) 0.2991(4) -0.4958(6) 0.027(2) Uani 1 d . . H7 H -0.7087(7) 0.3080(4) -0.4373(6) 0.032 Uiso 1 calc R . C8 C -0.8727(7) 0.2977(4) -0.5139(6) 0.032(2) Uani 1 d . . H8 H -0.9044(7) 0.3070(4) -0.4686(6) 0.038 Uiso 1 calc R . C9 C -0.9422(7) 0.2822(5) -0.6014(6) 0.038(2) Uani 1 d . . H9 H -1.0206(7) 0.2817(5) -0.6141(6) 0.045 Uiso 1 calc R . C10 C -0.8969(7) 0.2676(4) -0.6693(6) 0.029(2) Uani 1 d . . H10 H -0.9439(7) 0.2560(4) -0.7266(6) 0.035 Uiso 1 calc R . C11 C -0.7789(6) 0.2706(4) -0.6501(5) 0.024(2) Uani 1 d . . H11 H -0.7471(6) 0.2613(4) -0.6952(5) 0.029 Uiso 1 calc R . C12 C -0.5257(6) 0.2771(4) -0.6403(5) 0.021(2) Uani 1 d . . C13 C -0.4804(7) 0.2151(4) -0.6438(6) 0.030(2) Uani 1 d . . H13 H -0.4611(7) 0.1884(4) -0.5932(6) 0.036 Uiso 1 calc R . C14 C -0.4650(7) 0.1946(4) -0.7232(6) 0.033(2) Uani 1 d . . H14 H -0.4350(7) 0.1538(4) -0.7263(6) 0.040 Uiso 1 calc R . C15 C -0.4944(7) 0.2348(5) -0.7989(6) 0.036(2) Uani 1 d . . H15 H -0.4837(7) 0.2209(5) -0.8523(6) 0.043 Uiso 1 calc R . C16 C -0.5388(8) 0.2947(5) -0.7947(6) 0.037(2) Uani 1 d . . H16 H -0.5597(8) 0.3210(5) -0.8458(6) 0.044 Uiso 1 calc R . C17 C -0.5527(7) 0.3159(4) -0.7165(5) 0.026(2) Uani 1 d . . H17 H -0.5807(7) 0.3573(4) -0.7140(5) 0.032 Uiso 1 calc R . C18 C -0.6334(9) 0.1739(7) -0.3843(8) 0.060(3) Uani 1 d . . C19 C -0.7198(8) 0.1167(5) -0.3897(6) 0.034(2) Uani 1 d . . C20 C -0.3782(7) 0.1832(4) -0.2274(6) 0.031(2) Uani 1 d . . H20 H -0.4551(7) 0.1844(4) -0.2333(6) 0.037 Uiso 1 calc R . C21 C -0.3032(8) 0.1501(4) -0.1538(6) 0.032(2) Uani 1 d . . H21 H -0.3312(8) 0.1287(4) -0.1129(6) 0.038 Uiso 1 calc R . C22 C -0.1907(8) 0.1491(4) -0.1421(5) 0.024(2) Uani 1 d . . H22 H -0.1407(8) 0.1263(4) -0.0945(5) 0.028 Uiso 1 calc R . C23 C -0.1513(8) 0.1835(4) -0.2039(6) 0.029(2) Uani 1 d . . H23 H -0.0739(8) 0.1863(4) -0.1957(6) 0.035 Uiso 1 calc R . C24 C -0.2277(7) 0.2129(4) -0.2759(5) 0.018(2) Uani 1 d . . C25 C -0.1784(7) 0.2008(4) -0.4450(5) 0.018(2) Uani 1 d . . C26 C -0.1548(8) 0.1359(4) -0.4226(6) 0.032(2) Uani 1 d . . H26 H -0.1452(8) 0.1213(4) -0.3642(6) 0.038 Uiso 1 calc R . C27 C -0.1459(8) 0.0926(4) -0.4904(6) 0.038(2) Uani 1 d . . H27 H -0.1260(8) 0.0498(4) -0.4755(6) 0.046 Uiso 1 calc R . C28 C -0.1658(8) 0.1128(5) -0.5754(6) 0.035(2) Uani 1 d . . H28 H -0.1659(8) 0.0833(5) -0.6204(6) 0.042 Uiso 1 calc R . C29 C -0.1863(7) 0.1779(4) -0.5968(5) 0.027(2) Uani 1 d . . H29 H -0.1931(7) 0.1923(4) -0.6548(5) 0.032 Uiso 1 calc R . C30 C -0.1966(7) 0.2206(4) -0.5335(5) 0.024(2) Uani 1 d . . H30 H -0.2159(7) 0.2633(4) -0.5497(5) 0.028 Uiso 1 calc R . C31 C -0.0479(7) 0.2855(4) -0.2988(5) 0.020(2) Uani 1 d . . C32 C 0.0507(7) 0.2598(4) -0.3089(5) 0.021(2) Uani 1 d . . H32 H 0.0461(7) 0.2271(4) -0.3508(5) 0.026 Uiso 1 calc R . C33 C 0.1552(7) 0.2827(4) -0.2569(6) 0.026(2) Uani 1 d . . H33 H 0.2210(7) 0.2652(4) -0.2637(6) 0.031 Uiso 1 calc R . C34 C 0.1632(7) 0.3324(5) -0.1938(5) 0.031(2) Uani 1 d . . H34 H 0.2341(7) 0.3477(5) -0.1591(5) 0.038 Uiso 1 calc R . C35 C 0.0656(7) 0.3586(4) -0.1831(5) 0.028(2) Uani 1 d . . H35 H 0.0712(7) 0.3917(4) -0.1415(5) 0.034 Uiso 1 calc R . C36 C -0.0372(7) 0.3365(4) -0.2327(5) 0.025(2) Uani 1 d . . H36 H -0.1022(7) 0.3540(4) -0.2244(5) 0.030 Uiso 1 calc R . C37 C -0.1075(7) 0.4042(4) -0.4392(5) 0.019(2) Uani 1 d . . C38 C -0.0188(7) 0.4589(4) -0.4204(6) 0.025(2) Uani 1 d . . C40 C 0.0727(7) -0.2171(4) -0.0082(5) 0.027(2) Uani 1 d . . H40 H 0.1452(7) -0.2311(4) 0.0250(5) 0.032 Uiso 1 calc R . C41 C -0.0095(7) -0.2636(4) -0.0505(6) 0.029(2) Uani 1 d . . H41 H 0.0068(7) -0.3075(4) -0.0440(6) 0.034 Uiso 1 calc R . C42 C -0.1129(7) -0.2423(4) -0.1008(5) 0.024(2) Uani 1 d . . H42 H -0.1685(7) -0.2719(4) -0.1307(5) 0.029 Uiso 1 calc R . C43 C -0.1374(7) -0.1758(4) -0.1086(5) 0.026(2) Uani 1 d . . H43 H -0.2091(7) -0.1609(4) -0.1423(5) 0.031 Uiso 1 calc R . C44 C -0.0533(6) -0.1339(4) -0.0655(5) 0.017(2) Uani 1 d . . C45 C -0.2174(7) -0.0336(4) -0.1107(6) 0.023(2) Uani 1 d . . C46 C -0.2780(7) -0.0113(4) -0.1967(5) 0.024(2) Uani 1 d . . H46 H -0.2398(7) -0.0014(4) -0.2376(5) 0.028 Uiso 1 calc R . C47 C -0.3947(7) -0.0038(4) -0.2219(6) 0.035(2) Uani 1 d . . H47 H -0.4342(7) 0.0129(4) -0.2786(6) 0.043 Uiso 1 calc R . C48 C -0.4529(8) -0.0210(4) -0.1629(8) 0.044(3) Uani 1 d . . H48 H -0.5316(8) -0.0175(4) -0.1811(8) 0.052 Uiso 1 calc R . C49 C -0.3959(8) -0.0429(4) -0.0791(8) 0.043(3) Uani 1 d . . H49 H -0.4351(8) -0.0535(4) -0.0392(8) 0.052 Uiso 1 calc R . C50 C -0.2762(7) -0.0495(4) -0.0522(6) 0.031(2) Uani 1 d . . H50 H -0.2371(7) -0.0648(4) 0.0054(6) 0.037 Uiso 1 calc R . C51 C -0.0174(6) -0.0258(4) -0.1671(5) 0.015(2) Uani 1 d . . C52 C 0.0426(7) 0.0311(4) -0.1646(6) 0.025(2) Uani 1 d . . H52 H 0.0594(7) 0.0577(4) -0.1139(6) 0.030 Uiso 1 calc R . C53 C 0.0776(7) 0.0485(4) -0.2382(6) 0.032(2) Uani 1 d . . H53 H 0.1170(7) 0.0870(4) -0.2365(6) 0.038 Uiso 1 calc R . C54 C 0.0550(8) 0.0102(4) -0.3113(5) 0.032(2) Uani 1 d . . H54 H 0.0790(8) 0.0224(4) -0.3597(5) 0.039 Uiso 1 calc R . C55 C -0.0046(8) -0.0481(4) -0.3155(5) 0.032(2) Uani 1 d . . H55 H -0.0212(8) -0.0744(4) -0.3665(5) 0.038 Uiso 1 calc R . C56 C -0.0379(7) -0.0653(4) -0.2425(5) 0.027(2) Uani 1 d . . H56 H -0.0751(7) -0.1044(4) -0.2437(5) 0.032 Uiso 1 calc R . C57 C -0.1641(7) 0.0658(4) 0.0983(5) 0.023(2) Uani 1 d . . C58 C -0.2466(8) 0.1219(4) 0.1036(6) 0.033(2) Uani 1 d . . C59 C 0.2467(7) 0.0416(4) 0.1995(6) 0.026(2) Uani 1 d . . C60 C 0.3166(8) 0.0755(4) 0.2688(6) 0.035(2) Uani 1 d . . H60 H 0.3934(8) 0.0792(4) 0.2749(6) 0.042 Uiso 1 calc R . C61 C 0.2726(8) 0.1055(4) 0.3321(6) 0.035(2) Uani 1 d . . H61 H 0.3197(8) 0.1280(4) 0.3815(6) 0.042 Uiso 1 calc R . C62 C 0.1593(7) 0.1004(4) 0.3185(5) 0.023(2) Uani 1 d . . H62 H 0.1288(7) 0.1192(4) 0.3598(5) 0.028 Uiso 1 calc R . C63 C 0.0889(7) 0.0680(4) 0.2451(5) 0.028(2) Uani 1 d . . H63 H 0.0115(7) 0.0655(4) 0.2372(5) 0.033 Uiso 1 calc R . C64 C 0.3039(7) 0.0617(4) 0.0366(5) 0.021(2) Uani 1 d . . C65 C 0.3563(9) 0.0501(5) -0.0279(6) 0.040(3) Uani 1 d . . H65 H 0.3856(9) 0.0092(5) -0.0311(6) 0.048 Uiso 1 calc R . C66 C 0.3666(8) 0.0960(4) -0.0865(6) 0.037(2) Uani 1 d . . H66 H 0.4076(8) 0.0871(4) -0.1258(6) 0.044 Uiso 1 calc R . C67 C 0.3174(8) 0.1552(5) -0.0886(6) 0.035(2) Uani 1 d . . H67 H 0.3228(8) 0.1866(5) -0.1298(6) 0.042 Uiso 1 calc R . C68 C 0.2594(10) 0.1673(5) -0.0276(7) 0.056(3) Uani 1 d . . H68 H 0.2241(10) 0.2070(5) -0.0279(7) 0.067 Uiso 1 calc R . C69 C 0.2544(9) 0.1210(5) 0.0325(7) 0.044(3) Uani 1 d . . H69 H 0.2152(9) 0.1301(5) 0.0730(7) 0.052 Uiso 1 calc R . C70 C 0.4309(6) -0.0281(4) 0.1802(5) 0.018(2) Uani 1 d . . C71 C 0.4366(7) -0.0796(4) 0.2396(5) 0.027(2) Uani 1 d . . H71 H 0.3701(7) -0.0995(4) 0.2412(5) 0.033 Uiso 1 calc R . C72 C 0.5389(7) -0.1007(5) 0.2950(6) 0.033(2) Uani 1 d . . H72 H 0.5421(7) -0.1354(5) 0.3337(6) 0.039 Uiso 1 calc R . C73 C 0.6404(8) -0.0702(5) 0.2942(6) 0.038(2) Uani 1 d . . H73 H 0.7101(8) -0.0839(5) 0.3333(6) 0.045 Uiso 1 calc R . C74 C 0.6352(7) -0.0212(5) 0.2362(6) 0.033(2) Uani 1 d . . H74 H 0.7020(7) -0.0024(5) 0.2333(6) 0.040 Uiso 1 calc R . C75 C 0.5293(7) 0.0021(5) 0.1798(5) 0.029(2) Uani 1 d . . H75 H 0.5263(7) 0.0376(5) 0.1425(5) 0.034 Uiso 1 calc R . C76 C 0.3818(6) -0.1471(4) 0.0342(5) 0.018(2) Uani 1 d . . C77 C 0.4708(7) -0.2030(4) 0.0553(5) 0.023(2) Uani 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 Cl1 0.071(2) 0.069(2) 0.0358(13) 0.0008(13) 0.0063(13) -0.020(2) Cl2 0.057(2) 0.049(2) 0.075(2) 0.000(2) 0.011(2) 0.0135(14) C80 0.069(7) 0.037(6) 0.030(5) -0.007(5) -0.002(5) 0.004(5) F1 0.035(3) 0.011(3) 0.061(3) 0.005(2) 0.015(3) 0.000(2) F2 0.055(4) 0.046(4) 0.023(2) -0.004(2) 0.010(3) -0.023(3) F3 0.030(3) 0.026(3) 0.056(3) 0.000(2) 0.024(3) -0.003(2) F4 0.117(8) 0.121(8) 0.161(9) -0.079(7) 0.070(7) -0.094(7) F5 0.120(8) 0.119(8) 0.149(9) 0.066(7) 0.028(7) -0.035(6) F6 0.059(6) 0.053(6) 0.400(20) -0.025(8) 0.111(9) -0.014(4) F7 0.129(7) 0.058(5) 0.066(4) -0.006(4) 0.073(5) 0.019(4) F8 0.035(3) 0.024(3) 0.062(3) 0.007(3) 0.023(3) 0.005(2) F9 0.029(3) 0.052(4) 0.090(5) 0.019(4) 0.010(3) 0.006(3) F10 0.051(4) 0.061(5) 0.096(5) 0.026(4) 0.053(4) 0.026(3) F11 0.059(4) 0.072(5) 0.049(4) 0.003(3) 0.008(3) 0.038(4) F12 0.040(4) 0.022(4) 0.128(6) -0.018(3) 0.011(4) 0.008(3) Pd1 0.0168(3) 0.0303(4) 0.0330(4) 0.0146(3) 0.0063(3) -0.0039(3) Pd2 0.0144(3) 0.0144(4) 0.0211(3) 0.0011(3) 0.0075(2) 0.0003(2) Pd3 0.0174(3) 0.0161(4) 0.0201(3) 0.0025(3) 0.0104(3) 0.0021(3) Pd4 0.0152(3) 0.0154(4) 0.0250(3) 0.0023(3) 0.0097(3) 0.0012(2) P1 0.0167(11) 0.0220(14) 0.0240(11) 0.0025(9) 0.0053(9) -0.0008(9) P2 0.0174(11) 0.0149(12) 0.0186(10) 0.0011(9) 0.0070(9) 0.0014(8) P3 0.0179(11) 0.0182(13) 0.0259(11) 0.0021(10) 0.0100(9) 0.0006(9) P4 0.0173(11) 0.0144(13) 0.0233(11) 0.0011(9) 0.0106(9) 0.0013(9) O1 0.016(3) 0.014(3) 0.042(3) -0.001(3) 0.007(3) 0.005(3) O2 0.020(3) 0.039(4) 0.033(3) -0.008(3) 0.014(3) -0.004(3) O3 0.040(4) 0.056(5) 0.072(5) 0.027(4) 0.023(4) 0.014(4) O4 0.076(7) 0.069(7) 0.100(7) -0.029(6) 0.005(6) -0.009(5) O5 0.021(3) 0.023(3) 0.015(3) 0.001(2) 0.006(2) 0.000(2) O6 0.033(4) 0.045(4) 0.038(3) 0.012(3) 0.020(3) 0.010(3) O7 0.019(3) 0.019(3) 0.030(3) 0.006(3) 0.009(2) 0.006(3) O8 0.022(3) 0.021(4) 0.033(3) 0.007(2) 0.014(3) 0.003(2) N1 0.021(4) 0.015(4) 0.027(3) 0.001(3) 0.012(3) -0.002(3) N2 0.030(4) 0.022(4) 0.025(4) 0.005(3) 0.014(3) 0.004(3) N3 0.012(3) 0.017(4) 0.027(3) 0.007(3) 0.008(3) -0.002(3) N4 0.018(4) 0.025(4) 0.021(3) 0.002(3) 0.008(3) 0.002(3) C1 0.037(5) 0.020(6) 0.041(5) -0.006(4) 0.015(4) -0.004(4) C2 0.043(6) 0.010(5) 0.051(6) -0.005(4) -0.005(5) 0.017(4) C3 0.036(6) 0.023(6) 0.055(6) -0.001(5) 0.014(5) 0.017(4) C4 0.022(5) 0.032(6) 0.035(5) 0.003(4) 0.006(4) 0.011(4) C5 0.016(4) 0.024(5) 0.026(4) 0.000(4) 0.010(4) -0.002(3) C6 0.009(4) 0.014(4) 0.027(4) 0.002(3) 0.004(3) -0.001(3) C7 0.026(5) 0.024(5) 0.032(5) -0.001(4) 0.011(4) 0.000(4) C8 0.024(5) 0.035(6) 0.042(5) 0.003(4) 0.017(4) 0.005(4) C9 0.017(5) 0.052(7) 0.038(5) 0.003(5) -0.001(4) 0.001(4) C10 0.016(4) 0.032(6) 0.034(5) 0.004(4) -0.002(4) -0.005(4) C11 0.013(4) 0.030(5) 0.030(4) 0.000(4) 0.008(4) 0.000(3) C12 0.020(4) 0.016(5) 0.028(4) -0.002(4) 0.009(4) 0.006(3) C13 0.020(5) 0.027(5) 0.043(5) 0.013(4) 0.009(4) -0.005(4) C14 0.028(5) 0.029(6) 0.047(6) -0.015(5) 0.017(4) -0.001(4) C15 0.033(5) 0.042(7) 0.035(5) -0.009(5) 0.013(4) 0.008(4) C16 0.038(6) 0.042(7) 0.031(5) 0.007(5) 0.014(4) 0.001(5) C17 0.029(5) 0.016(5) 0.035(5) -0.003(4) 0.010(4) 0.003(4) C18 0.028(6) 0.101(11) 0.050(7) 0.026(7) 0.013(5) 0.039(6) C19 0.026(5) 0.062(7) 0.020(4) -0.006(5) 0.015(4) -0.014(5) C20 0.027(5) 0.030(5) 0.039(5) 0.001(4) 0.016(4) -0.005(4) C21 0.050(6) 0.025(6) 0.025(5) 0.000(4) 0.018(4) -0.014(4) C22 0.038(5) 0.014(5) 0.018(4) 0.002(3) 0.008(4) -0.003(4) C23 0.024(5) 0.022(5) 0.035(5) -0.006(4) 0.002(4) -0.004(4) C24 0.020(4) 0.019(5) 0.015(4) 0.004(3) 0.008(3) -0.004(4) C25 0.019(4) 0.016(5) 0.021(4) -0.005(3) 0.009(3) -0.003(3) C26 0.043(6) 0.023(6) 0.031(5) 0.003(4) 0.016(4) 0.011(4) C27 0.051(6) 0.021(5) 0.047(6) 0.007(5) 0.023(5) 0.018(5) C28 0.040(6) 0.033(7) 0.040(5) -0.010(5) 0.023(5) 0.014(4) C29 0.035(5) 0.025(6) 0.022(4) 0.002(4) 0.012(4) 0.002(4) C30 0.026(5) 0.021(5) 0.018(4) -0.003(4) -0.002(4) 0.000(4) C31 0.026(5) 0.012(5) 0.020(4) 0.001(3) 0.003(4) -0.004(3) C32 0.028(5) 0.021(5) 0.017(4) 0.006(4) 0.012(4) 0.016(4) C33 0.017(5) 0.023(5) 0.035(5) 0.002(4) 0.006(4) 0.002(4) C34 0.017(4) 0.050(7) 0.024(4) 0.003(5) 0.001(4) -0.007(4) C35 0.035(5) 0.022(5) 0.022(4) -0.003(4) 0.002(4) -0.008(4) C36 0.024(5) 0.029(5) 0.024(4) 0.000(4) 0.010(4) 0.004(4) C37 0.022(4) 0.017(5) 0.016(4) 0.007(3) 0.005(3) 0.003(3) C38 0.032(5) 0.012(5) 0.040(5) 0.003(4) 0.024(4) -0.007(4) C40 0.021(5) 0.028(5) 0.032(5) 0.013(4) 0.010(4) 0.004(4) C41 0.038(5) 0.014(5) 0.037(5) 0.007(4) 0.017(4) 0.002(4) C42 0.033(5) 0.017(5) 0.022(4) -0.001(4) 0.006(4) -0.008(4) C43 0.026(5) 0.027(6) 0.026(4) 0.008(4) 0.011(4) 0.004(4) C44 0.016(4) 0.024(5) 0.014(3) 0.004(3) 0.011(3) 0.000(3) C45 0.020(4) 0.010(5) 0.039(5) -0.006(4) 0.010(4) 0.003(3) C46 0.025(5) 0.018(5) 0.029(4) -0.006(4) 0.012(4) 0.002(3) C47 0.031(5) 0.024(5) 0.043(5) -0.003(5) 0.000(4) 0.002(4) C48 0.017(5) 0.026(6) 0.078(8) -0.020(5) 0.001(5) -0.004(4) C49 0.025(5) 0.029(6) 0.088(8) -0.010(6) 0.036(6) -0.006(4) C50 0.022(5) 0.023(5) 0.048(5) -0.001(4) 0.013(4) -0.002(4) C51 0.015(4) 0.012(4) 0.019(4) 0.003(3) 0.007(3) 0.003(3) C52 0.024(5) 0.021(5) 0.032(5) -0.002(4) 0.011(4) -0.004(4) C53 0.036(5) 0.026(6) 0.031(5) 0.008(4) 0.007(4) -0.011(4) C54 0.049(6) 0.032(6) 0.020(4) 0.009(4) 0.015(4) -0.003(4) C55 0.045(6) 0.033(6) 0.022(4) -0.003(4) 0.017(4) -0.003(4) C56 0.028(5) 0.021(5) 0.032(4) 0.008(4) 0.009(4) 0.001(4) C57 0.036(5) 0.015(5) 0.015(4) 0.008(3) 0.003(4) 0.007(4) C58 0.053(6) 0.014(5) 0.038(5) 0.003(4) 0.022(5) 0.014(4) C59 0.031(5) 0.022(5) 0.028(5) 0.004(4) 0.014(4) -0.005(4) C60 0.032(5) 0.023(6) 0.053(6) -0.019(5) 0.019(5) -0.009(4) C61 0.050(6) 0.013(5) 0.042(5) -0.013(4) 0.016(5) -0.008(4) C62 0.027(5) 0.025(5) 0.023(4) 0.002(4) 0.013(4) 0.004(4) C63 0.033(5) 0.029(5) 0.024(4) 0.002(4) 0.013(4) 0.010(4) C64 0.030(5) 0.010(5) 0.023(4) -0.004(3) 0.011(4) -0.009(4) C65 0.057(7) 0.027(6) 0.037(5) 0.009(5) 0.017(5) 0.013(5) C66 0.052(6) 0.024(6) 0.041(5) 0.011(4) 0.025(5) 0.005(5) C67 0.034(6) 0.036(6) 0.033(5) 0.006(4) 0.010(4) -0.003(4) C68 0.097(9) 0.019(6) 0.071(7) 0.014(5) 0.056(7) 0.012(6) C69 0.065(7) 0.032(6) 0.050(6) 0.010(5) 0.041(6) 0.013(5) C70 0.012(4) 0.027(5) 0.016(4) -0.006(3) 0.006(3) -0.003(3) C71 0.021(5) 0.036(6) 0.032(5) -0.005(5) 0.018(4) -0.006(4) C72 0.024(5) 0.042(7) 0.035(5) 0.012(4) 0.014(4) 0.009(4) C73 0.029(5) 0.045(7) 0.026(5) 0.000(5) -0.007(4) 0.007(5) C74 0.016(5) 0.056(7) 0.027(5) 0.008(5) 0.006(4) -0.006(4) C75 0.034(5) 0.029(6) 0.024(4) 0.003(4) 0.011(4) -0.004(4) C76 0.016(4) 0.021(5) 0.018(4) -0.005(3) 0.004(3) 0.001(3) C77 0.021(5) 0.032(6) 0.018(4) -0.001(4) 0.009(4) -0.001(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 Cl1 C80 1.760(10) . ? Cl2 C80 1.764(11) 1_556 ? C80 Cl2 1.764(11) 1_554 ? F1 C38 1.340(8) . ? F2 C38 1.316(9) . ? F3 C38 1.350(8) . ? F4 C19 1.256(12) . ? F5 C19 1.293(12) . ? F6 C19 1.242(12) . ? F7 C58 1.262(9) . ? F8 C58 1.337(9) . ? F9 C58 1.363(10) . ? F10 C77 1.317(8) . ? F11 C77 1.326(8) . ? F12 C77 1.306(9) . ? Pd1 N2 2.110(7) . ? Pd1 P1 2.197(3) . ? Pd1 O3 2.307(8) . ? Pd1 Pd2 2.5613(14) . ? Pd2 N1 2.114(7) . ? Pd2 O1 2.183(6) . ? Pd2 P2 2.216(2) . ? Pd3 N4 2.130(7) . ? Pd3 P4 2.201(3) . ? Pd3 O5 2.207(6) . ? Pd3 Pd4 2.5584(14) . ? Pd4 N3 2.125(7) . ? Pd4 O7 2.163(5) . ? Pd4 P3 2.217(3) . ? P1 C5 1.817(8) . ? P1 C6 1.828(7) . ? P1 C12 1.832(8) . ? P2 C31 1.805(8) . ? P2 C25 1.825(7) . ? P2 C24 1.841(7) . ? P3 C70 1.823(8) . ? P3 C64 1.826(8) . ? P3 C59 1.839(9) . ? P4 C51 1.815(7) . ? P4 C45 1.818(8) . ? P4 C44 1.831(8) . ? O1 C37 1.247(8) . ? O2 C37 1.220(8) . ? O3 C18 1.143(12) . ? O4 C18 1.267(14) . ? O5 C57 1.234(8) . ? O6 C57 1.241(8) . ? O7 C76 1.286(8) . ? O8 C76 1.194(8) . ? N1 C1 1.367(11) . ? N1 C5 1.378(10) . ? N2 C20 1.340(10) . ? N2 C24 1.363(8) . ? N3 C40 1.319(8) . ? N3 C44 1.363(7) . ? N4 C63 1.356(8) . ? N4 C59 1.380(9) . ? C1 C2 1.378(12) . ? C2 C3 1.371(13) . ? C3 C4 1.402(13) . ? C4 C5 1.387(11) . ? C6 C7 1.375(11) . ? C6 C11 1.410(11) . ? C7 C8 1.390(11) . ? C8 C9 1.400(12) . ? C9 C10 1.380(12) . ? C10 C11 1.401(11) . ? C12 C17 1.384(11) . ? C12 C13 1.409(12) . ? C13 C14 1.376(12) . ? C14 C15 1.395(13) . ? C15 C16 1.366(12) . ? C16 C17 1.357(12) . ? C18 C19 1.58(2) . ? C20 C21 1.404(9) . ? C21 C22 1.349(12) . ? C22 C23 1.405(12) . ? C23 C24 1.361(12) . ? C25 C30 1.387(11) . ? C25 C26 1.396(12) . ? C26 C27 1.416(12) . ? C27 C28 1.335(12) . ? C28 C29 1.392(13) . ? C29 C30 1.360(11) . ? C31 C32 1.388(11) . ? C31 C36 1.451(11) . ? C32 C33 1.377(11) . ? C33 C34 1.405(12) . ? C34 C35 1.385(12) . ? C35 C36 1.345(12) . ? C37 C38 1.541(11) . ? C40 C41 1.404(11) . ? C41 C42 1.347(12) . ? C42 C43 1.408(12) . ? C43 C44 1.359(11) . ? C45 C50 1.376(12) . ? C45 C46 1.391(11) . ? C46 C47 1.385(12) . ? C47 C48 1.384(14) . ? C48 C49 1.350(14) . ? C49 C50 1.417(12) . ? C51 C56 1.386(11) . ? C51 C52 1.388(11) . ? C52 C53 1.397(11) . ? C53 C54 1.343(12) . ? C54 C55 1.407(12) . ? C55 C56 1.375(11) . ? C57 C58 1.569(11) . ? C59 C60 1.348(12) . ? C60 C61 1.414(12) . ? C61 C62 1.358(13) . ? C62 C63 1.373(12) . ? C64 C69 1.366(13) . ? C64 C65 1.380(12) . ? C65 C66 1.352(12) . ? C66 C67 1.366(13) . ? C67 C68 1.385(13) . ? C68 C69 1.356(13) . ? C70 C75 1.374(11) . ? C70 C71 1.398(12) . ? C71 C72 1.362(12) . ? C72 C73 1.412(13) . ? C73 C74 1.347(13) . ? C74 C75 1.414(12) . ? C76 C77 1.560(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 Cl1 C80 Cl2 111.3(6) . 1_554 ? N2 Pd1 P1 174.7(2) . . ? N2 Pd1 O3 92.2(3) . . ? P1 Pd1 O3 92.9(2) . . ? N2 Pd1 Pd2 93.6(2) . . ? P1 Pd1 Pd2 81.11(9) . . ? O3 Pd1 Pd2 168.4(2) . . ? N1 Pd2 O1 87.9(2) . . ? N1 Pd2 P2 173.6(2) . . ? O1 Pd2 P2 97.6(2) . . ? N1 Pd2 Pd1 94.4(2) . . ? O1 Pd2 Pd1 171.92(15) . . ? P2 Pd2 Pd1 80.62(8) . . ? N4 Pd3 P4 173.3(2) . . ? N4 Pd3 O5 88.4(2) . . ? P4 Pd3 O5 98.0(2) . . ? N4 Pd3 Pd4 93.4(2) . . ? P4 Pd3 Pd4 80.03(9) . . ? O5 Pd3 Pd4 175.46(13) . . ? N3 Pd4 O7 86.9(2) . . ? N3 Pd4 P3 174.0(2) . . ? O7 Pd4 P3 98.4(2) . . ? N3 Pd4 Pd3 94.6(2) . . ? O7 Pd4 Pd3 171.64(14) . . ? P3 Pd4 Pd3 80.47(8) . . ? C5 P1 C6 100.5(4) . . ? C5 P1 C12 105.8(4) . . ? C6 P1 C12 104.3(4) . . ? C5 P1 Pd1 113.0(3) . . ? C6 P1 Pd1 114.1(3) . . ? C12 P1 Pd1 117.3(3) . . ? C31 P2 C25 107.2(4) . . ? C31 P2 C24 100.6(3) . . ? C25 P2 C24 104.4(4) . . ? C31 P2 Pd2 115.3(3) . . ? C25 P2 Pd2 114.4(3) . . ? C24 P2 Pd2 113.5(3) . . ? C70 P3 C64 107.9(4) . . ? C70 P3 C59 99.7(4) . . ? C64 P3 C59 103.3(4) . . ? C70 P3 Pd4 113.4(3) . . ? C64 P3 Pd4 117.5(2) . . ? C59 P3 Pd4 113.2(3) . . ? C51 P4 C45 105.4(4) . . ? C51 P4 C44 103.2(3) . . ? C45 P4 C44 102.0(3) . . ? C51 P4 Pd3 117.0(2) . . ? C45 P4 Pd3 115.1(3) . . ? C44 P4 Pd3 112.5(2) . . ? C37 O1 Pd2 116.2(4) . . ? C18 O3 Pd1 109.9(9) . . ? C57 O5 Pd3 115.1(4) . . ? C76 O7 Pd4 117.8(4) . . ? C1 N1 C5 118.9(7) . . ? C1 N1 Pd2 121.2(6) . . ? C5 N1 Pd2 119.7(5) . . ? C20 N2 C24 117.4(6) . . ? C20 N2 Pd1 123.2(6) . . ? C24 N2 Pd1 119.2(4) . . ? C40 N3 C44 118.7(5) . . ? C40 N3 Pd4 123.2(4) . . ? C44 N3 Pd4 118.0(4) . . ? C63 N4 C59 118.5(5) . . ? C63 N4 Pd3 123.2(4) . . ? C59 N4 Pd3 117.9(4) . . ? N1 C1 C2 121.4(8) . . ? C3 C2 C1 120.2(8) . . ? C2 C3 C4 119.4(8) . . ? C5 C4 C3 119.1(8) . . ? N1 C5 C4 121.0(8) . . ? N1 C5 P1 111.7(6) . . ? C4 C5 P1 127.2(6) . . ? C7 C6 C11 119.1(7) . . ? C7 C6 P1 118.1(6) . . ? C11 C6 P1 122.6(6) . . ? C6 C7 C8 121.2(8) . . ? C7 C8 C9 118.9(8) . . ? C10 C9 C8 121.5(8) . . ? C9 C10 C11 118.7(8) . . ? C10 C11 C6 120.6(8) . . ? C17 C12 C13 119.1(7) . . ? C17 C12 P1 123.5(6) . . ? C13 C12 P1 117.3(6) . . ? C14 C13 C12 119.2(8) . . ? C13 C14 C15 120.1(8) . . ? C16 C15 C14 120.2(8) . . ? C17 C16 C15 120.3(9) . . ? C16 C17 C12 121.1(8) . . ? O3 C18 O4 137.5(14) . . ? O3 C18 C19 114.2(12) . . ? O4 C18 C19 108.0(10) . . ? F6 C19 F4 103.8(10) . . ? F6 C19 F5 110.2(10) . . ? F4 C19 F5 98.1(11) . . ? F6 C19 C18 115.9(10) . . ? F4 C19 C18 113.8(8) . . ? F5 C19 C18 113.3(8) . . ? N2 C20 C21 121.7(7) . . ? C22 C21 C20 120.4(7) . . ? C21 C22 C23 118.0(8) . . ? C24 C23 C22 119.3(8) . . ? C23 C24 N2 123.0(7) . . ? C23 C24 P2 124.7(6) . . ? N2 C24 P2 112.2(5) . . ? C30 C25 C26 119.2(7) . . ? C30 C25 P2 118.6(6) . . ? C26 C25 P2 122.2(6) . . ? C25 C26 C27 118.9(8) . . ? C28 C27 C26 120.5(8) . . ? C27 C28 C29 120.2(8) . . ? C30 C29 C28 120.5(8) . . ? C29 C30 C25 120.4(8) . . ? C32 C31 C36 118.2(7) . . ? C32 C31 P2 125.0(6) . . ? C36 C31 P2 116.8(6) . . ? C33 C32 C31 120.1(8) . . ? C32 C33 C34 120.5(8) . . ? C35 C34 C33 120.1(8) . . ? C36 C35 C34 120.2(8) . . ? C35 C36 C31 120.8(8) . . ? O2 C37 O1 130.1(7) . . ? O2 C37 C38 117.8(7) . . ? O1 C37 C38 112.1(6) . . ? F2 C38 F1 107.6(6) . . ? F2 C38 F3 105.5(6) . . ? F1 C38 F3 106.3(5) . . ? F2 C38 C37 113.5(6) . . ? F1 C38 C37 111.5(6) . . ? F3 C38 C37 112.1(6) . . ? N3 C40 C41 122.7(7) . . ? C42 C41 C40 117.7(8) . . ? C41 C42 C43 120.7(8) . . ? C44 C43 C42 118.0(8) . . ? C43 C44 N3 122.0(7) . . ? C43 C44 P4 125.3(6) . . ? N3 C44 P4 112.6(5) . . ? C50 C45 C46 118.6(8) . . ? C50 C45 P4 117.4(6) . . ? C46 C45 P4 123.9(6) . . ? C47 C46 C45 120.5(8) . . ? C46 C47 C48 120.2(9) . . ? C49 C48 C47 120.4(9) . . ? C48 C49 C50 119.8(9) . . ? C45 C50 C49 120.5(9) . . ? C56 C51 C52 118.5(7) . . ? C56 C51 P4 122.9(6) . . ? C52 C51 P4 118.6(6) . . ? C51 C52 C53 120.0(8) . . ? C54 C53 C52 120.6(8) . . ? C53 C54 C55 120.8(8) . . ? C56 C55 C54 118.4(8) . . ? C55 C56 C51 121.7(8) . . ? O5 C57 O6 129.9(7) . . ? O5 C57 C58 116.0(6) . . ? O6 C57 C58 114.1(7) . . ? F7 C58 F8 113.6(6) . . ? F7 C58 F9 105.9(7) . . ? F8 C58 F9 104.5(6) . . ? F7 C58 C57 111.7(6) . . ? F8 C58 C57 112.2(7) . . ? F9 C58 C57 108.4(6) . . ? C60 C59 N4 121.7(7) . . ? C60 C59 P3 125.9(7) . . ? N4 C59 P3 112.4(5) . . ? C59 C60 C61 119.6(9) . . ? C62 C61 C60 117.8(8) . . ? C61 C62 C63 121.5(8) . . ? N4 C63 C62 120.7(7) . . ? C69 C64 C65 115.6(8) . . ? C69 C64 P3 123.1(7) . . ? C65 C64 P3 121.0(7) . . ? C66 C65 C64 122.5(9) . . ? C65 C66 C67 120.6(9) . . ? C66 C67 C68 118.2(9) . . ? C69 C68 C67 119.6(9) . . ? C68 C69 C64 123.3(9) . . ? C75 C70 C71 119.4(8) . . ? C75 C70 P3 124.2(6) . . ? C71 C70 P3 116.2(6) . . ? C72 C71 C70 120.4(8) . . ? C71 C72 C73 120.4(8) . . ? C74 C73 C72 119.4(8) . . ? C73 C74 C75 120.7(8) . . ? C70 C75 C74 119.6(8) . . ? O8 C76 O7 130.2(6) . . ? O8 C76 C77 117.7(6) . . ? O7 C76 C77 112.1(6) . . ? F12 C77 F10 107.2(6) . . ? F12 C77 F11 106.7(6) . . ? F10 C77 F11 106.5(6) . . ? F12 C77 C76 112.4(6) . . ? F10 C77 C76 111.7(6) . . ? F11 C77 C76 112.0(6) . . ? _refine_diff_density_max 1.436 _refine_diff_density_min -0.874 _refine_diff_density_rms 0.138