# Copyright The Royal Society of Chemistry, 1998 data_zgp3 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C36 H46 Cl2 N2 O2 Pd2' _chemical_formula_weight 822.45 _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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pd' 'Pd' -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 13.518(3) _cell_length_b 25.105(5) _cell_length_c 10.797(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3664.2(13) _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 ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.491 _exptl_crystal_density_method ? _exptl_crystal_F_000 1672 _exptl_absorpt_coefficient_mu 1.160 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _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 ? _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11888 _diffrn_reflns_av_R_equivalents 0.0226 _diffrn_reflns_av_sigmaI/netI 0.0340 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.62 _diffrn_reflns_theta_max 25.48 _reflns_number_total 6486 _reflns_number_observed 6374 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 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^)+(0.0834P)^2^+0.1718P] 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 ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0400(14) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.67(3) _refine_ls_number_reflns 6486 _refine_ls_number_parameters 399 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0404 _refine_ls_R_factor_obs 0.0378 _refine_ls_wR_factor_all 0.1056 _refine_ls_wR_factor_obs 0.0996 _refine_ls_goodness_of_fit_all 1.044 _refine_ls_goodness_of_fit_obs 0.993 _refine_ls_restrained_S_all 1.044 _refine_ls_restrained_S_obs 0.993 _refine_ls_shift/esd_max 0.003 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Pd1 Pd 0.76490(2) 0.202213(12) 0.65054(3) 0.06304(13) Uani 1 d . . Pd2 Pd 0.58367(2) 0.176832(12) 0.87690(3) 0.06446(13) Uani 1 d . . Cl1 Cl 0.68661(10) 0.25304(5) 0.80353(12) 0.0804(3) Uani 1 d . . Cl2 Cl 0.67702(9) 0.12515(4) 0.73864(11) 0.0753(3) Uani 1 d . . O1 O 0.8747(4) 0.4056(2) 0.5656(5) 0.1067(14) Uani 1 d . . O2 O 0.4370(4) -0.0215(2) 0.8873(7) 0.123(2) Uani 1 d . . N1 N 0.8407(3) 0.1611(2) 0.5185(3) 0.0668(8) Uani 1 d . . N2 N 0.4996(3) 0.2166(2) 1.0027(4) 0.0706(9) Uani 1 d . . C1 C 0.8312(3) 0.3167(2) 0.6029(5) 0.0717(10) Uani 1 d . . H1A H 0.7858(3) 0.3291(2) 0.6649(5) 0.080 Uiso 1 d R . C2 C 0.8382(3) 0.2626(2) 0.5762(4) 0.0667(9) Uani 1 d . . C3 C 0.9045(3) 0.2462(2) 0.4808(4) 0.0701(10) Uani 1 d . . C4 C 0.9612(4) 0.2834(2) 0.4184(6) 0.0870(14) Uani 1 d . . H4A H 1.0058(4) 0.2714(2) 0.3550(6) 0.080 Uiso 1 d R . C5 C 0.9548(4) 0.3363(2) 0.4449(7) 0.0902(15) Uani 1 d . . H5A H 0.9939(4) 0.3619(2) 0.4005(7) 0.080 Uiso 1 d R . C6 C 0.8901(4) 0.3533(2) 0.5358(6) 0.0806(12) Uani 1 d . . C7 C 0.9232(7) 0.4443(3) 0.4903(11) 0.138(4) Uani 1 d . . H7A H 0.9063(7) 0.4794(3) 0.5185(11) 0.080 Uiso 1 d R . H7B H 0.9937(7) 0.4397(3) 0.4941(11) 0.080 Uiso 1 d R . H7C H 0.9013(7) 0.4399(3) 0.4063(11) 0.080 Uiso 1 d R . C8 C 0.9014(4) 0.1894(2) 0.4566(4) 0.0712(10) Uani 1 d . . H8A H 0.9432(4) 0.1736(2) 0.3949(4) 0.080 Uiso 1 d R . C9 C 0.8280(4) 0.1043(2) 0.4900(4) 0.0714(10) Uani 1 d . . H9A H 0.8234(4) 0.0844(2) 0.5657(4) 0.080 Uiso 1 d R . H9B H 0.8848(4) 0.0917(2) 0.4453(4) 0.080 Uiso 1 d R . C10 C 0.7355(4) 0.0944(2) 0.4113(4) 0.0677(9) Uani 1 d . . H10A H 0.6809(4) 0.1084(2) 0.4579(4) 0.080 Uiso 1 d R . C11 C 0.7174(6) 0.0333(2) 0.3954(6) 0.097(2) Uani 1 d . . H11A H 0.6702(6) 0.0224(2) 0.4569(6) 0.080 Uiso 1 d R . H11B H 0.7782(6) 0.0150(2) 0.4125(6) 0.080 Uiso 1 d R . C12 C 0.6781(7) 0.0163(2) 0.2717(8) 0.112(2) Uani 1 d . . H12A H 0.6112(7) 0.0039(2) 0.2801(8) 0.080 Uiso 1 d R . H12B H 0.7176(7) -0.0132(2) 0.2437(8) 0.080 Uiso 1 d R . C13 C 0.6834(5) 0.0600(2) 0.1730(6) 0.093(2) Uani 1 d . . H13A H 0.6627(5) 0.0495(2) 0.0915(6) 0.080 Uiso 1 d R . C14 C 0.6331(4) 0.1102(2) 0.2247(6) 0.0834(14) Uani 1 d . . H14A H 0.5805(4) 0.1033(2) 0.2822(6) 0.080 Uiso 1 d R . H14B H 0.6134(4) 0.1354(2) 0.1625(6) 0.080 Uiso 1 d R . C15 C 0.7346(4) 0.1223(2) 0.2863(4) 0.0687(10) Uani 1 d . . H15A H 0.7519(4) 0.1594(2) 0.2889(4) 0.080 Uiso 1 d R . C16 C 0.7833(5) 0.0903(2) 0.1794(5) 0.0861(14) Uani 1 d . . C17 C 0.7955(7) 0.1271(4) 0.0670(6) 0.134(3) Uani 1 d . . H17A H 0.8578(7) 0.1453(4) 0.0734(6) 0.080 Uiso 1 d R . H17B H 0.7931(7) 0.1076(4) -0.0094(6) 0.080 Uiso 1 d R . H17C H 0.7427(7) 0.1527(4) 0.0688(6) 0.080 Uiso 1 d R . C18 C 0.8794(6) 0.0593(3) 0.1972(7) 0.116(2) Uani 1 d . . H18A H 0.8723(6) 0.0351(3) 0.2655(7) 0.080 Uiso 1 d R . H18B H 0.8951(6) 0.0397(3) 0.1235(7) 0.080 Uiso 1 d R . H18C H 0.9316(6) 0.0841(3) 0.2147(7) 0.080 Uiso 1 d R . C19 C 0.4984(3) 0.1176(2) 0.9307(4) 0.0694(10) Uani 1 d . . C20 C 0.4296(4) 0.1324(2) 1.0241(5) 0.0767(11) Uani 1 d . . C21 C 0.3673(4) 0.0949(3) 1.0766(6) 0.0883(14) Uani 1 d . . H21A H 0.3221(4) 0.1057(3) 1.1403(6) 0.080 Uiso 1 d R . C22 C 0.3669(5) 0.0425(3) 1.0327(7) 0.100(2) Uani 1 d . . H22A H 0.3244(5) 0.0165(3) 1.0706(7) 0.080 Uiso 1 d R . C23 C 0.4318(4) 0.0292(2) 0.9391(6) 0.0877(14) Uani 1 d . . C24 C 0.4978(4) 0.0656(2) 0.8891(5) 0.0780(11) Uani 1 d . . H24A H 0.5432(4) 0.0547(2) 0.8255(5) 0.080 Uiso 1 d R . C25 C 0.3697(8) -0.0596(3) 0.9196(12) 0.148(4) Uani 1 d . . H25A H 0.3833(8) -0.0925(3) 0.8774(12) 0.080 Uiso 1 d R . H25B H 0.3751(8) -0.0650(3) 1.0073(12) 0.080 Uiso 1 d R . H25C H 0.3039(8) -0.0480(3) 0.8997(12) 0.080 Uiso 1 d R . C26 C 0.4339(4) 0.1881(2) 1.0587(5) 0.0781(12) Uani 1 d . . H26A H 0.3906(4) 0.2029(2) 1.1203(5) 0.080 Uiso 1 d R . C27 C 0.5174(4) 0.2724(2) 1.0396(5) 0.0758(11) Uani 1 d . . H27A H 0.4612(4) 0.2856(2) 1.0847(5) 0.080 Uiso 1 d R . H27B H 0.5262(4) 0.2945(2) 0.9679(5) 0.080 Uiso 1 d R . C28 C 0.6086(3) 0.2759(2) 1.1212(5) 0.0731(10) Uani 1 d . . H28A H 0.6545(3) 0.2504(2) 1.0883(5) 0.080 Uiso 1 d R . C29 C 0.5869(5) 0.2586(2) 1.2572(5) 0.0798(12) Uani 1 d . . H29A H 0.5486(5) 0.2274(2) 1.2749(5) 0.080 Uiso 1 d R . C30 C 0.6305(4) 0.2936(2) 1.3603(5) 0.0845(12) Uani 1 d . . H30A H 0.6766(4) 0.2730(2) 1.4079(5) 0.080 Uiso 1 d R . H30B H 0.5782(4) 0.3048(2) 1.4146(5) 0.080 Uiso 1 d R . C31 C 0.6838(4) 0.3426(2) 1.3098(6) 0.0887(14) Uani 1 d . . H31A H 0.7133(4) 0.3654(2) 1.3708(6) 0.080 Uiso 1 d R . C32 C 0.7528(5) 0.3259(4) 1.2030(7) 0.113(2) Uani 1 d . . H32A H 0.7792(5) 0.2906(4) 1.2124(7) 0.080 Uiso 1 d R . H32B H 0.8039(5) 0.3512(4) 1.1845(7) 0.080 Uiso 1 d R . C33 C 0.6620(5) 0.3295(2) 1.1185(5) 0.0896(14) Uani 1 d . . H33A H 0.6756(5) 0.3430(2) 1.0371(5) 0.080 Uiso 1 d R . C34 C 0.6194(5) 0.3721(2) 1.2113(6) 0.091(2) Uani 1 d . . C35 C 0.6573(10) 0.4284(3) 1.1829(10) 0.165(5) Uani 1 d . . H35A H 0.6309(10) 0.4538(3) 1.2406(10) 0.080 Uiso 1 d R . H35B H 0.7282(10) 0.4282(3) 1.1888(10) 0.080 Uiso 1 d R . H35C H 0.6381(10) 0.4381(3) 1.1003(10) 0.080 Uiso 1 d R . C36 C 0.5071(6) 0.3770(2) 1.2298(7) 0.106(2) Uani 1 d . . H36A H 0.4930(6) 0.4044(2) 1.2893(7) 0.080 Uiso 1 d R . H36B H 0.4768(6) 0.3860(2) 1.1521(7) 0.080 Uiso 1 d R . H36C H 0.4812(6) 0.3437(2) 1.2588(7) 0.080 Uiso 1 d 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 0.0578(2) 0.0813(2) 0.0500(2) -0.00373(11) 0.00023(13) 0.00118(12) Pd2 0.0590(2) 0.0821(2) 0.0523(2) -0.00065(12) 0.00096(13) 0.00416(12) Cl1 0.0824(6) 0.0900(6) 0.0688(6) -0.0152(5) 0.0196(6) -0.0094(5) Cl2 0.0778(6) 0.0807(5) 0.0673(6) -0.0022(5) 0.0158(5) 0.0030(5) O1 0.115(3) 0.083(2) 0.123(4) -0.009(2) 0.019(3) -0.007(2) O2 0.105(3) 0.090(2) 0.172(5) -0.009(3) 0.042(4) -0.013(2) N1 0.065(2) 0.083(2) 0.053(2) -0.0051(14) -0.010(2) 0.004(2) N2 0.057(2) 0.097(2) 0.058(2) -0.004(2) -0.002(2) 0.006(2) C1 0.066(2) 0.086(2) 0.063(2) -0.004(2) -0.001(2) 0.002(2) C2 0.059(2) 0.088(2) 0.052(2) -0.003(2) -0.007(2) 0.000(2) C3 0.060(2) 0.094(3) 0.056(2) -0.004(2) 0.003(2) -0.001(2) C4 0.074(3) 0.105(3) 0.082(3) -0.001(3) 0.017(3) -0.006(2) C5 0.074(3) 0.096(3) 0.100(4) 0.007(3) 0.013(3) -0.009(2) C6 0.074(3) 0.086(3) 0.083(3) -0.002(2) -0.006(3) -0.002(2) C7 0.134(7) 0.088(4) 0.191(10) -0.001(4) 0.049(7) -0.017(4) C8 0.066(2) 0.095(3) 0.053(2) -0.006(2) 0.004(2) 0.007(2) C9 0.075(3) 0.081(2) 0.058(2) -0.004(2) -0.001(2) 0.014(2) C10 0.070(2) 0.069(2) 0.064(2) -0.003(2) 0.000(2) 0.005(2) C11 0.121(5) 0.075(2) 0.094(4) 0.014(2) -0.013(4) -0.009(3) C12 0.132(6) 0.074(3) 0.128(6) -0.014(3) -0.033(5) 0.000(3) C13 0.100(4) 0.090(3) 0.088(4) -0.026(3) -0.026(3) 0.013(3) C14 0.083(3) 0.086(3) 0.081(3) -0.008(2) -0.027(3) 0.011(2) C15 0.074(2) 0.062(2) 0.070(2) -0.003(2) -0.014(2) 0.005(2) C16 0.084(3) 0.119(4) 0.055(2) -0.006(2) -0.007(2) 0.011(3) C17 0.117(6) 0.224(9) 0.060(3) 0.026(4) -0.012(4) -0.016(6) C18 0.099(4) 0.169(7) 0.081(4) -0.030(4) -0.002(4) 0.039(4) C19 0.057(2) 0.094(3) 0.058(2) 0.004(2) -0.004(2) 0.007(2) C20 0.063(2) 0.108(3) 0.059(2) 0.001(2) -0.003(2) -0.001(2) C21 0.074(3) 0.120(4) 0.071(3) -0.002(3) 0.012(3) -0.009(3) C22 0.078(3) 0.124(4) 0.098(4) 0.024(3) 0.005(3) -0.016(3) C23 0.070(3) 0.094(3) 0.099(4) 0.010(3) -0.002(3) -0.001(2) C24 0.070(2) 0.087(2) 0.077(3) 0.006(2) 0.007(3) 0.002(2) C25 0.128(6) 0.122(5) 0.195(11) -0.002(6) 0.052(8) -0.036(5) C26 0.065(2) 0.109(3) 0.060(2) -0.007(2) 0.002(2) 0.008(2) C27 0.072(3) 0.084(3) 0.071(3) -0.006(2) 0.002(2) 0.016(2) C28 0.069(2) 0.083(2) 0.068(3) -0.009(2) 0.008(2) 0.011(2) C29 0.092(3) 0.075(2) 0.072(3) 0.001(2) -0.004(3) -0.001(2) C30 0.083(3) 0.101(3) 0.070(3) 0.001(3) -0.004(3) 0.007(2) C31 0.080(3) 0.108(3) 0.078(3) -0.020(3) 0.005(3) -0.015(3) C32 0.081(4) 0.155(6) 0.103(5) -0.033(4) 0.019(3) -0.023(4) C33 0.093(3) 0.111(3) 0.065(3) -0.008(3) 0.022(3) -0.017(3) C34 0.119(4) 0.078(3) 0.075(3) -0.004(2) 0.020(3) -0.012(3) C35 0.258(15) 0.106(5) 0.132(7) 0.001(5) 0.025(9) -0.061(7) C36 0.129(5) 0.092(3) 0.097(4) -0.005(3) -0.001(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 Pd1 C2 1.980(5) . ? Pd1 N1 2.037(4) . ? Pd1 Cl1 2.3403(12) . ? Pd1 Cl2 2.4615(12) . ? Pd2 C19 1.968(5) . ? Pd2 N2 2.034(4) . ? Pd2 Cl2 2.3461(11) . ? Pd2 Cl1 2.4949(13) . ? O1 C6 1.366(7) . ? O1 C7 1.429(9) . ? O2 C23 1.392(8) . ? O2 C25 1.365(8) . ? N1 C8 1.275(6) . ? N1 C9 1.470(6) . ? N2 C26 1.291(7) . ? N2 C27 1.476(6) . ? C1 C6 1.415(7) . ? C1 C2 1.393(7) . ? C2 C3 1.425(6) . ? C3 C4 1.383(7) . ? C3 C8 1.449(7) . ? C4 C5 1.363(8) . ? C5 C6 1.383(9) . ? C9 C10 1.532(7) . ? C10 C15 1.520(6) . ? C10 C11 1.564(6) . ? C11 C12 1.500(10) . ? C12 C13 1.533(10) . ? C13 C14 1.536(7) . ? C13 C16 1.550(9) . ? C14 C15 1.555(7) . ? C15 C16 1.553(7) . ? C16 C18 1.526(9) . ? C16 C17 1.535(9) . ? C19 C24 1.382(7) . ? C19 C20 1.421(7) . ? C20 C21 1.384(8) . ? C20 C26 1.450(8) . ? C21 C22 1.399(10) . ? C22 C23 1.381(10) . ? C23 C24 1.386(7) . ? C27 C28 1.518(7) . ? C28 C33 1.527(7) . ? C28 C29 1.558(7) . ? C29 C30 1.535(7) . ? C30 C31 1.527(8) . ? C31 C32 1.541(9) . ? C31 C34 1.560(9) . ? C32 C33 1.533(10) . ? C33 C34 1.575(8) . ? C34 C36 1.536(11) . ? C34 C35 1.536(8) . ? 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 Pd1 N1 81.5(2) . . ? C2 Pd1 Cl1 95.46(13) . . ? N1 Pd1 Cl1 176.32(11) . . ? C2 Pd1 Cl2 178.10(13) . . ? N1 Pd1 Cl2 96.61(12) . . ? Cl1 Pd1 Cl2 86.42(4) . . ? C19 Pd2 N2 81.2(2) . . ? C19 Pd2 Cl2 94.89(14) . . ? N2 Pd2 Cl2 175.85(12) . . ? C19 Pd2 Cl1 177.86(13) . . ? N2 Pd2 Cl1 98.45(12) . . ? Cl2 Pd2 Cl1 85.53(4) . . ? Pd1 Cl1 Pd2 93.33(4) . . ? Pd2 Cl2 Pd1 94.06(4) . . ? C6 O1 C7 116.8(6) . . ? C23 O2 C25 120.3(7) . . ? C8 N1 C9 120.5(4) . . ? C8 N1 Pd1 114.1(3) . . ? C9 N1 Pd1 125.4(3) . . ? C26 N2 C27 120.8(4) . . ? C26 N2 Pd2 115.1(3) . . ? C27 N2 Pd2 123.8(3) . . ? C6 C1 C2 119.3(5) . . ? C1 C2 C3 118.3(4) . . ? C1 C2 Pd1 129.0(4) . . ? C3 C2 Pd1 112.7(3) . . ? C4 C3 C2 120.4(5) . . ? C4 C3 C8 126.2(4) . . ? C2 C3 C8 113.3(4) . . ? C3 C4 C5 121.4(5) . . ? C6 C5 C4 119.3(5) . . ? O1 C6 C5 124.0(5) . . ? O1 C6 C1 114.7(5) . . ? C5 C6 C1 121.3(5) . . ? N1 C8 C3 118.2(4) . . ? N1 C9 C10 111.5(4) . . ? C15 C10 C9 115.2(4) . . ? C15 C10 C11 110.7(4) . . ? C9 C10 C11 110.3(4) . . ? C12 C11 C10 115.6(5) . . ? C11 C12 C13 113.5(4) . . ? C12 C13 C14 108.3(6) . . ? C12 C13 C16 111.1(5) . . ? C14 C13 C16 88.2(4) . . ? C13 C14 C15 85.7(4) . . ? C10 C15 C16 114.7(4) . . ? C10 C15 C14 107.3(4) . . ? C16 C15 C14 87.4(4) . . ? C18 C16 C15 122.1(5) . . ? C18 C16 C13 119.8(6) . . ? C15 C16 C13 85.3(4) . . ? C18 C16 C17 108.4(7) . . ? C15 C16 C17 108.7(5) . . ? C13 C16 C17 110.7(6) . . ? C24 C19 C20 118.2(5) . . ? C24 C19 Pd2 128.4(4) . . ? C20 C19 Pd2 113.3(4) . . ? C21 C20 C19 120.8(5) . . ? C21 C20 C26 125.1(5) . . ? C19 C20 C26 114.1(5) . . ? C20 C21 C22 120.3(5) . . ? C21 C22 C23 118.2(5) . . ? O2 C23 C24 114.5(5) . . ? O2 C23 C22 123.2(5) . . ? C24 C23 C22 122.3(6) . . ? C19 C24 C23 120.1(5) . . ? N2 C26 C20 116.2(4) . . ? N2 C27 C28 110.1(4) . . ? C27 C28 C33 115.1(4) . . ? C27 C28 C29 112.2(4) . . ? C33 C28 C29 110.6(4) . . ? C28 C29 C30 116.9(4) . . ? C31 C30 C29 112.5(5) . . ? C32 C31 C34 87.6(5) . . ? C32 C31 C30 109.5(5) . . ? C34 C31 C30 111.2(5) . . ? C31 C32 C33 86.8(5) . . ? C28 C33 C32 108.4(5) . . ? C28 C33 C34 114.4(4) . . ? C32 C33 C34 87.3(5) . . ? C31 C34 C36 120.1(5) . . ? C31 C34 C35 112.7(7) . . ? C36 C34 C35 106.4(7) . . ? C31 C34 C33 84.7(4) . . ? C36 C34 C33 119.9(5) . . ? C35 C34 C33 112.1(6) . . ? _refine_diff_density_max 0.838 _refine_diff_density_min -0.757 _refine_diff_density_rms 0.284 #=END data_zgb3 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C36 H48 Br2 N2 O2 Pd2' _chemical_formula_weight 913.38 _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' 'Br' 'Br' -0.2901 2.4595 '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 ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 13.548(3) _cell_length_b 24.965(5) _cell_length_c 10.945(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3701.9(13) _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 ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.639 _exptl_crystal_density_method ? _exptl_crystal_F_000 1824 _exptl_absorpt_coefficient_mu 3.163 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _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 ? _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10561 _diffrn_reflns_av_R_equivalents 0.0651 _diffrn_reflns_av_sigmaI/netI 0.0667 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.03 _diffrn_reflns_theta_max 25.61 _reflns_number_total 6258 _reflns_number_observed 5820 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 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^)+(0.1195P)^2^+1.6518P] 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 ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0133(7) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.48(2) _refine_ls_number_reflns 6258 _refine_ls_number_parameters 398 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0640 _refine_ls_R_factor_obs 0.0607 _refine_ls_wR_factor_all 0.1740 _refine_ls_wR_factor_obs 0.1695 _refine_ls_goodness_of_fit_all 1.026 _refine_ls_goodness_of_fit_obs 1.036 _refine_ls_restrained_S_all 1.026 _refine_ls_restrained_S_obs 1.036 _refine_ls_shift/esd_max 0.191 _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 0.91886(4) 0.17679(2) 0.38162(5) 0.06965(14) Uani 1 d . . Pd2 Pd 0.73282(4) 0.20435(2) 0.14646(5) 0.06930(14) Uani 1 d . . Br1 Br 0.81983(7) 0.12276(3) 0.23954(8) 0.0826(2) Uani 1 d . . Br2 Br 0.81529(7) 0.25778(3) 0.30452(8) 0.0867(2) Uani 1 d . . O1 O 1.0666(6) -0.0223(3) 0.3858(10) 0.129(3) Uani 1 d . . O2 O 0.6232(5) 0.4086(3) 0.0631(8) 0.113(2) Uani 1 d . . N1 N 1.0017(5) 0.2164(3) 0.5095(6) 0.078(2) Uani 1 d . . N2 N 0.6575(5) 0.1629(3) 0.0149(6) 0.076(2) Uani 1 d . . C1 C 1.0041(6) 0.0643(3) 0.3934(9) 0.084(2) Uani 1 d . . H1A H 0.9586(6) 0.0534(3) 0.3309(9) 0.080 Uiso 1 d R . C2 C 1.0033(6) 0.1171(3) 0.4347(7) 0.076(2) Uani 1 d . . C3 C 1.0695(6) 0.1314(4) 0.5249(8) 0.083(2) Uani 1 d . . C4 C 1.1349(7) 0.0930(4) 0.5757(9) 0.095(3) Uani 1 d . . H4A H 1.1811(7) 0.1041(4) 0.6371(9) 0.080 Uiso 1 d R . C5 C 1.1349(8) 0.0417(5) 0.5335(11) 0.104(3) Uani 1 d . . H5A H 1.1775(8) 0.0156(5) 0.5706(11) 0.080 Uiso 1 d R . C6 C 1.0711(7) 0.0274(4) 0.4415(11) 0.098(3) Uani 1 d . . C7 C 1.1359(12) -0.0597(5) 0.4113(17) 0.159(6) Uani 1 d . . H7A H 1.1224(12) -0.0922(5) 0.3674(17) 0.080 Uiso 1 d R . H7B H 1.2001(12) -0.0466(5) 0.3890(17) 0.080 Uiso 1 d R . H7C H 1.1342(12) -0.0667(5) 0.4975(17) 0.080 Uiso 1 d R . C8 C 1.0664(6) 0.1864(4) 0.5616(8) 0.085(2) Uani 1 d . . H8A H 1.1110(6) 0.2004(4) 0.6218(8) 0.080 Uiso 1 d R . C9 C 0.9859(6) 0.2711(3) 0.5466(8) 0.081(2) Uani 1 d . . H9A H 0.9777(6) 0.2932(3) 0.4757(8) 0.080 Uiso 1 d R . H9B H 1.0421(6) 0.2839(3) 0.5914(8) 0.080 Uiso 1 d R . C10 C 0.8942(6) 0.2750(3) 0.6266(8) 0.080(2) Uani 1 d . . H10A H 0.8488(6) 0.2488(3) 0.5956(8) 0.080 Uiso 1 d R . C11 C 0.9161(8) 0.2585(3) 0.7613(8) 0.088(2) Uani 1 d . . H11A H 0.9865(8) 0.2581(3) 0.7716(8) 0.080 Uiso 1 d R . H11B H 0.8931(8) 0.2226(3) 0.7734(8) 0.080 Uiso 1 d R . C12 C 0.8710(7) 0.2935(4) 0.8622(9) 0.092(2) Uani 1 d . . H12A H 0.9235(7) 0.3059(4) 0.9139(9) 0.080 Uiso 1 d R . H12B H 0.8278(7) 0.2719(4) 0.9112(9) 0.080 Uiso 1 d R . C13 C 0.8162(7) 0.3413(4) 0.8130(10) 0.097(3) Uani 1 d . . H13A H 0.7848(7) 0.3630(4) 0.8741(10) 0.080 Uiso 1 d R . C14 C 0.7487(8) 0.3239(5) 0.7043(10) 0.115(3) Uani 1 d . . H14A H 0.6960(8) 0.3481(5) 0.6846(10) 0.080 Uiso 1 d R . H14B H 0.7250(8) 0.2879(5) 0.7131(10) 0.080 Uiso 1 d R . C15 C 0.8406(8) 0.3286(4) 0.6230(8) 0.101(3) Uani 1 d . . H15A H 0.8269(8) 0.3416(4) 0.5422(8) 0.080 Uiso 1 d R . C16 C 0.8797(9) 0.3713(3) 0.7161(9) 0.098(3) Uani 1 d . . C17 C 0.8409(13) 0.4270(4) 0.6844(15) 0.155(6) Uani 1 d . . H17A H 0.8657(13) 0.4525(4) 0.7424(15) 0.080 Uiso 1 d R . H17B H 0.8600(13) 0.4376(4) 0.6035(15) 0.080 Uiso 1 d R . H17C H 0.7702(13) 0.4257(4) 0.6896(15) 0.080 Uiso 1 d R . C18 C 0.9903(9) 0.3765(4) 0.7362(11) 0.108(3) Uani 1 d . . H18A H 1.0042(9) 0.4045(4) 0.7940(11) 0.080 Uiso 1 d R . H18B H 1.0151(9) 0.3431(4) 0.7668(11) 0.080 Uiso 1 d R . H18C H 1.0217(9) 0.3847(4) 0.6598(11) 0.080 Uiso 1 d R . C19 C 0.6600(5) 0.2656(3) 0.0707(7) 0.071(2) Uani 1 d . . C20 C 0.5959(6) 0.2488(4) -0.0193(7) 0.076(2) Uani 1 d . . C21 C 0.5379(6) 0.2862(4) -0.0828(9) 0.091(3) Uani 1 d . . H21A H 0.4955(6) 0.2742(4) -0.1474(9) 0.080 Uiso 1 d R . C22 C 0.5434(7) 0.3399(4) -0.0556(11) 0.098(3) Uani 1 d . . H22A H 0.5031(7) 0.3655(4) -0.0982(11) 0.080 Uiso 1 d R . C23 C 0.6102(6) 0.3558(4) 0.0350(9) 0.085(2) Uani 1 d . . C24 C 0.6657(6) 0.3195(3) 0.0969(8) 0.079(2) Uani 1 d . . H24A H 0.7100(6) 0.3315(3) 0.1595(8) 0.080 Uiso 1 d R . C25 C 0.5743(14) 0.4485(5) -0.0044(19) 0.164(7) Uani 1 d . . H25A H 0.5926(14) 0.4833(5) 0.0250(19) 0.080 Uiso 1 d R . H25B H 0.5924(14) 0.4453(5) -0.0889(19) 0.080 Uiso 1 d R . H25C H 0.5043(14) 0.4438(5) 0.0039(19) 0.080 Uiso 1 d R . C26 C 0.5974(6) 0.1930(4) -0.0486(8) 0.084(2) Uani 1 d . . H26A H 0.5567(6) 0.1781(4) -0.1119(8) 0.080 Uiso 1 d R . C27 C 0.6701(7) 0.1063(3) -0.0131(7) 0.083(2) Uani 1 d . . H27A H 0.6130(7) 0.0940(3) -0.0569(7) 0.080 Uiso 1 d R . H27B H 0.6750(7) 0.0859(3) 0.0611(7) 0.080 Uiso 1 d R . C28 C 0.7606(6) 0.0971(3) -0.0918(7) 0.074(2) Uani 1 d . . H28A H 0.8144(6) 0.1121(3) -0.0460(7) 0.080 Uiso 1 d R . C29 C 0.7825(9) 0.0357(3) -0.1041(12) 0.109(3) Uani 1 d . . H29A H 0.7240(9) 0.0163(3) -0.0821(12) 0.080 Uiso 1 d R . H29B H 0.8331(9) 0.0266(3) -0.0464(12) 0.080 Uiso 1 d R . C30 C 0.8200(11) 0.0179(4) -0.2321(13) 0.122(4) Uani 1 d . . H30A H 0.7779(11) -0.0107(4) -0.2592(13) 0.080 Uiso 1 d R . H30B H 0.8860(11) 0.0040(4) -0.2271(13) 0.080 Uiso 1 d R . C31 C 0.8152(9) 0.0613(4) -0.3267(11) 0.106(3) Uani 1 d . . H31A H 0.8353(9) 0.0508(4) -0.4073(11) 0.080 Uiso 1 d R . C32 C 0.8622(7) 0.1116(3) -0.2805(8) 0.088(2) Uani 1 d . . H32A H 0.8796(7) 0.1368(3) -0.3431(8) 0.080 Uiso 1 d R . H32B H 0.9161(7) 0.1056(3) -0.2252(8) 0.080 Uiso 1 d R . C33 C 0.7626(6) 0.1237(3) -0.2173(7) 0.072(2) Uani 1 d . . H33A H 0.7444(6) 0.1608(3) -0.2158(7) 0.080 Uiso 1 d R . C34 C 0.7158(9) 0.0898(4) -0.3212(9) 0.103(3) Uani 1 d . . C35 C 0.7015(10) 0.1264(6) -0.4347(10) 0.133(5) Uani 1 d . . H35A H 0.6707(10) 0.1071(6) -0.5002(10) 0.080 Uiso 1 d R . H35B H 0.6602(10) 0.1559(6) -0.4112(10) 0.080 Uiso 1 d R . H35C H 0.7645(10) 0.1397(6) -0.4612(10) 0.080 Uiso 1 d R . C36 C 0.6233(9) 0.0593(5) -0.3026(11) 0.132(4) Uani 1 d . . H36A H 0.6305(9) 0.0355(5) -0.2343(11) 0.080 Uiso 1 d R . H36B H 0.5704(9) 0.0840(5) -0.2869(11) 0.080 Uiso 1 d R . H36C H 0.6086(9) 0.0389(5) -0.3748(11) 0.080 Uiso 1 d 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 0.0660(3) 0.0917(3) 0.0513(3) -0.0004(2) -0.0008(2) -0.0050(2) Pd2 0.0661(3) 0.0942(3) 0.0477(2) -0.0049(2) -0.0008(2) -0.0024(2) Br1 0.0864(5) 0.0955(4) 0.0658(4) -0.0008(4) -0.0126(4) -0.0063(4) Br2 0.0869(5) 0.1057(5) 0.0675(4) -0.0178(4) -0.0168(4) 0.0116(4) O1 0.113(5) 0.105(4) 0.169(8) 0.000(5) -0.053(6) 0.015(4) O2 0.107(5) 0.110(4) 0.123(6) -0.001(4) -0.024(5) 0.006(4) N1 0.066(3) 0.104(4) 0.064(3) -0.007(3) 0.012(3) -0.014(3) N2 0.072(3) 0.099(4) 0.056(3) -0.009(3) 0.017(3) -0.012(3) C1 0.068(4) 0.090(5) 0.095(6) 0.002(4) -0.011(5) -0.001(3) C2 0.066(4) 0.112(5) 0.051(4) 0.005(4) 0.001(3) -0.011(4) C3 0.065(4) 0.121(6) 0.064(4) -0.004(4) -0.001(4) 0.007(4) C4 0.081(5) 0.127(7) 0.077(5) 0.002(5) -0.021(5) 0.009(5) C5 0.088(6) 0.131(7) 0.092(6) 0.015(6) -0.013(6) 0.016(6) C6 0.082(5) 0.098(5) 0.115(8) 0.016(5) -0.008(6) 0.006(4) C7 0.179(12) 0.141(9) 0.157(14) -0.008(9) -0.035(12) 0.057(9) C8 0.066(4) 0.123(6) 0.065(4) -0.005(4) -0.008(4) -0.005(4) C9 0.083(5) 0.099(5) 0.062(4) -0.004(4) -0.010(4) -0.023(4) C10 0.072(4) 0.100(5) 0.069(4) -0.016(4) -0.001(4) 0.001(4) C11 0.109(6) 0.089(4) 0.066(4) 0.005(4) 0.011(5) 0.005(5) C12 0.094(5) 0.108(6) 0.073(5) 0.007(5) 0.002(5) -0.011(4) C13 0.087(5) 0.119(6) 0.083(5) -0.021(5) -0.022(5) 0.019(5) C14 0.098(7) 0.147(8) 0.099(7) -0.026(6) -0.021(6) 0.029(6) C15 0.139(8) 0.109(6) 0.054(4) -0.009(4) -0.028(5) 0.018(6) C16 0.136(8) 0.085(5) 0.072(5) -0.009(4) -0.008(5) 0.010(5) C17 0.231(16) 0.117(7) 0.117(10) 0.005(7) -0.044(12) 0.042(10) C18 0.117(7) 0.112(6) 0.097(7) -0.001(5) -0.014(6) -0.032(6) C19 0.061(4) 0.100(5) 0.053(3) -0.010(3) -0.004(3) 0.000(3) C20 0.065(4) 0.102(5) 0.063(4) -0.011(4) 0.005(4) 0.000(4) C21 0.077(4) 0.119(6) 0.077(5) -0.011(4) -0.035(4) 0.005(4) C22 0.084(5) 0.114(6) 0.096(6) 0.008(5) -0.019(5) 0.018(5) C23 0.069(4) 0.100(5) 0.087(6) -0.013(4) 0.008(4) 0.000(4) C24 0.068(4) 0.104(5) 0.066(4) 0.003(4) 0.004(4) 0.004(4) C25 0.189(15) 0.119(9) 0.183(18) -0.010(10) -0.037(15) 0.023(10) C26 0.071(4) 0.119(6) 0.062(4) -0.002(4) 0.003(4) -0.003(4) C27 0.096(5) 0.101(5) 0.051(4) 0.003(3) 0.007(4) -0.027(4) C28 0.079(4) 0.083(4) 0.060(4) 0.004(3) -0.003(4) -0.009(4) C29 0.123(8) 0.082(5) 0.123(8) 0.015(5) 0.007(7) 0.003(5) C30 0.138(9) 0.089(5) 0.137(10) -0.012(6) 0.023(9) -0.007(6) C31 0.125(7) 0.096(5) 0.097(7) -0.019(5) 0.036(6) -0.023(5) C32 0.098(6) 0.093(5) 0.074(5) -0.005(4) 0.028(5) -0.018(4) C33 0.085(4) 0.074(4) 0.058(4) -0.003(3) 0.014(4) -0.012(3) C34 0.117(7) 0.132(7) 0.060(5) -0.003(5) 0.003(5) -0.028(6) C35 0.121(9) 0.217(14) 0.062(5) 0.011(7) 0.006(6) -0.007(9) C36 0.125(8) 0.202(11) 0.068(5) -0.037(6) 0.011(6) -0.061(8) _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 C2 1.967(8) . ? Pd1 N1 2.048(7) . ? Pd1 Br1 2.4572(10) . ? Pd1 Br2 2.6018(11) . ? Pd2 C19 1.999(8) . ? Pd2 N2 2.045(7) . ? Pd2 Br2 2.4538(10) . ? Pd2 Br1 2.5644(11) . ? O1 C7 1.353(14) . ? O1 C6 1.384(13) . ? O2 C23 1.365(11) . ? O2 C25 1.41(2) . ? N1 C8 1.285(11) . ? N1 C9 1.441(10) . ? N2 C26 1.308(11) . ? N2 C27 1.457(11) . ? C1 C2 1.392(12) . ? C1 C6 1.396(12) . ? C2 C3 1.381(12) . ? C3 C4 1.419(13) . ? C3 C8 1.432(13) . ? C4 C5 1.360(15) . ? C5 C6 1.37(2) . ? C9 C10 1.524(12) . ? C10 C15 1.523(12) . ? C10 C11 1.559(12) . ? C11 C12 1.534(12) . ? C12 C13 1.506(13) . ? C13 C16 1.56(2) . ? C13 C14 1.562(14) . ? C14 C15 1.53(2) . ? C15 C16 1.567(13) . ? C16 C18 1.52(2) . ? C16 C17 1.526(14) . ? C19 C24 1.378(11) . ? C19 C20 1.379(11) . ? C20 C21 1.405(12) . ? C20 C26 1.430(13) . ? C21 C22 1.375(13) . ? C22 C23 1.400(14) . ? C23 C24 1.358(12) . ? C27 C28 1.516(12) . ? C28 C33 1.525(10) . ? C28 C29 1.568(11) . ? C29 C30 1.56(2) . ? C30 C31 1.50(2) . ? C31 C32 1.495(13) . ? C31 C34 1.52(2) . ? C32 C33 1.547(12) . ? C33 C34 1.552(12) . ? C34 C36 1.481(15) . ? C34 C35 1.55(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 C2 Pd1 N1 81.1(3) . . ? C2 Pd1 Br1 95.1(2) . . ? N1 Pd1 Br1 175.2(2) . . ? C2 Pd1 Br2 176.9(2) . . ? N1 Pd1 Br2 98.2(2) . . ? Br1 Pd1 Br2 85.81(3) . . ? C19 Pd2 N2 81.3(3) . . ? C19 Pd2 Br2 95.8(2) . . ? N2 Pd2 Br2 176.7(2) . . ? C19 Pd2 Br1 177.3(2) . . ? N2 Pd2 Br1 96.2(2) . . ? Br2 Pd2 Br1 86.70(3) . . ? Pd1 Br1 Pd2 93.81(3) . . ? Pd2 Br2 Pd1 92.97(3) . . ? C7 O1 C6 119.8(10) . . ? C23 O2 C25 120.4(10) . . ? C8 N1 C9 121.8(7) . . ? C8 N1 Pd1 113.4(6) . . ? C9 N1 Pd1 124.7(5) . . ? C26 N2 C27 121.2(7) . . ? C26 N2 Pd2 113.2(6) . . ? C27 N2 Pd2 125.5(5) . . ? C2 C1 C6 120.4(9) . . ? C3 C2 C1 118.2(8) . . ? C3 C2 Pd1 113.1(6) . . ? C1 C2 Pd1 128.7(6) . . ? C2 C3 C4 120.7(9) . . ? C2 C3 C8 115.4(8) . . ? C4 C3 C8 123.9(8) . . ? C5 C4 C3 120.2(9) . . ? C4 C5 C6 119.5(9) . . ? C5 C6 O1 125.7(9) . . ? C5 C6 C1 120.9(10) . . ? O1 C6 C1 113.4(9) . . ? N1 C8 C3 117.0(8) . . ? N1 C9 C10 110.1(6) . . ? C15 C10 C9 115.5(8) . . ? C15 C10 C11 110.3(7) . . ? C9 C10 C11 111.8(7) . . ? C12 C11 C10 117.1(7) . . ? C13 C12 C11 112.9(8) . . ? C12 C13 C16 110.6(8) . . ? C12 C13 C14 109.9(8) . . ? C16 C13 C14 86.5(8) . . ? C15 C14 C13 86.9(8) . . ? C10 C15 C14 107.7(8) . . ? C10 C15 C16 114.8(8) . . ? C14 C15 C16 87.1(8) . . ? C18 C16 C17 107.1(10) . . ? C18 C16 C13 119.2(9) . . ? C17 C16 C13 113.7(10) . . ? C18 C16 C15 119.0(9) . . ? C17 C16 C15 110.8(9) . . ? C13 C16 C15 85.9(7) . . ? C24 C19 C20 118.7(7) . . ? C24 C19 Pd2 129.3(6) . . ? C20 C19 Pd2 112.0(6) . . ? C19 C20 C21 120.2(8) . . ? C19 C20 C26 116.6(8) . . ? C21 C20 C26 123.0(8) . . ? C22 C21 C20 120.8(8) . . ? C21 C22 C23 117.6(9) . . ? C24 C23 O2 117.4(9) . . ? C24 C23 C22 121.5(9) . . ? O2 C23 C22 121.1(9) . . ? C23 C24 C19 121.1(8) . . ? N2 C26 C20 116.6(8) . . ? N2 C27 C28 111.1(6) . . ? C27 C28 C33 117.4(7) . . ? C27 C28 C29 110.4(7) . . ? C33 C28 C29 110.1(7) . . ? C28 C29 C30 114.8(9) . . ? C31 C30 C29 113.6(8) . . ? C30 C31 C32 110.8(10) . . ? C30 C31 C34 110.4(10) . . ? C32 C31 C34 88.4(7) . . ? C31 C32 C33 86.7(7) . . ? C28 C33 C32 109.5(7) . . ? C28 C33 C34 114.6(6) . . ? C32 C33 C34 85.6(7) . . ? C36 C34 C31 120.9(10) . . ? C36 C34 C35 107.8(10) . . ? C31 C34 C35 110.7(9) . . ? C36 C34 C33 121.7(9) . . ? C31 C34 C33 85.5(8) . . ? C35 C34 C33 108.5(8) . . ? _refine_diff_density_max 0.870 _refine_diff_density_min -0.926 _refine_diff_density_rms 0.106 #=END data_zgp2 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C36 H49 Cl N O P Pd' _chemical_formula_weight 684.58 _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' 'Cl' 'Cl' 0.1484 0.1585 '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 ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' _cell_length_a 12.138(2) _cell_length_b 13.909(3) _cell_length_c 10.066(2) _cell_angle_alpha 91.75(3) _cell_angle_beta 97.35(3) _cell_angle_gamma 104.22(3) _cell_volume 1630.4(5) _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 ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.394 _exptl_crystal_density_method ? _exptl_crystal_F_000 716 _exptl_absorpt_coefficient_mu 0.729 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _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 ? _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6049 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0532 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.00 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6049 _reflns_number_observed 4757 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 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^)+(0.0319P)^2^+0.2074P] 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 ? _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 -0.03(3) _refine_ls_number_reflns 6049 _refine_ls_number_parameters 739 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0494 _refine_ls_R_factor_obs 0.0316 _refine_ls_wR_factor_all 0.0878 _refine_ls_wR_factor_obs 0.0788 _refine_ls_goodness_of_fit_all 1.021 _refine_ls_goodness_of_fit_obs 1.051 _refine_ls_restrained_S_all 1.020 _refine_ls_restrained_S_obs 1.051 _refine_ls_shift/esd_max 0.077 _refine_ls_shift/esd_mean 0.006 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Pd1 Pd 0.27446(2) -0.00596(2) 0.93027(2) 0.04410(10) Uani 1 d . . Cl1 Cl 0.14912(11) 0.05454(11) 1.05537(14) 0.0677(4) Uani 1 d . . P1 P 0.42207(10) 0.03503(9) 1.10061(11) 0.0397(3) Uani 1 d . . N1 N 0.1519(3) -0.0437(3) 0.7600(4) 0.0474(11) Uani 1 d . . O1 O 0.6210(4) -0.1489(3) 0.7541(4) 0.0880(15) Uani 1 d . . C1 C 0.3569(4) -0.0714(3) 0.8077(4) 0.0420(12) Uani 1 d . . C2 C 0.4682(4) -0.0886(4) 0.8387(4) 0.0513(15) Uani 1 d . . H2A H 0.5117(4) -0.0751(4) 0.9268(4) 0.080 Uiso 1 d R . C3 C 0.5138(4) -0.1315(4) 0.7371(6) 0.059(2) Uani 1 d . . C4 C 0.4529(6) -0.1578(4) 0.6063(5) 0.074(2) Uani 1 d . . H4A H 0.4891(6) -0.1864(4) 0.5415(5) 0.080 Uiso 1 d R . C5 C 0.3438(5) -0.1438(4) 0.5809(5) 0.060(2) Uani 1 d . . H5A H 0.3011(5) -0.1598(4) 0.4925(5) 0.080 Uiso 1 d R . C6 C 0.2985(4) -0.1016(3) 0.6842(4) 0.0416(13) Uani 1 d . . C7 C 0.1836(4) -0.0835(4) 0.6577(5) 0.057(2) Uani 1 d . . H7A H 0.1333(4) -0.1076(4) 0.5755(5) 0.080 Uiso 1 d R . C8 C 0.0335(4) -0.0251(4) 0.7460(6) 0.060(2) Uani 1 d . . H8A H -0.0003(4) -0.0443(4) 0.8254(6) 0.080 Uiso 1 d R . H8B H -0.0160(4) -0.0625(4) 0.6700(6) 0.080 Uiso 1 d R . C9 C 0.0388(5) 0.0834(4) 0.7224(5) 0.059(2) Uani 1 d . . H9A H 0.0975(5) 0.1192(4) 0.7919(5) 0.080 Uiso 1 d R . C10 C -0.0750(5) 0.1109(4) 0.7494(5) 0.077(2) Uani 1 d . . H10A H -0.0684(5) 0.1366(4) 0.8404(5) 0.080 Uiso 1 d R . H10B H -0.1358(5) 0.0510(4) 0.7380(5) 0.080 Uiso 1 d R . C11 C -0.1155(5) 0.1800(5) 0.6525(6) 0.094(2) Uani 1 d . . H11A H -0.0980(5) 0.2435(5) 0.7012(6) 0.080 Uiso 1 d R . H11B H -0.1971(5) 0.1590(5) 0.6269(6) 0.080 Uiso 1 d R . C12 C -0.0540(5) 0.1948(4) 0.5346(6) 0.077(2) Uani 1 d . . H12A H -0.0801(5) 0.2375(4) 0.4713(6) 0.080 Uiso 1 d R . C13 C 0.0792(5) 0.2311(4) 0.5892(6) 0.079(2) Uani 1 d . . H13A H 0.0959(5) 0.2648(4) 0.6768(6) 0.080 Uiso 1 d R . H13B H 0.1253(5) 0.2679(4) 0.5280(6) 0.080 Uiso 1 d R . C14 C 0.0758(5) 0.1186(3) 0.5902(5) 0.0563(14) Uani 1 d . . H14A H 0.1439(5) 0.1027(3) 0.5672(5) 0.080 Uiso 1 d R . C15 C -0.0288(5) 0.1007(4) 0.4733(5) 0.071(2) Uani 1 d . . C16 C 0.0171(6) 0.1151(5) 0.3397(5) 0.094(2) Uani 1 d . . H16A H -0.0452(6) 0.1038(5) 0.2673(5) 0.080 Uiso 1 d R . H16B H 0.0630(6) 0.1821(5) 0.3409(5) 0.080 Uiso 1 d R . H16C H 0.0636(6) 0.0696(5) 0.3273(5) 0.080 Uiso 1 d R . C17 C -0.1258(6) 0.0102(5) 0.4614(7) 0.104(3) Uani 1 d . . H17A H -0.1803(6) 0.0118(5) 0.3840(7) 0.080 Uiso 1 d R . H17B H -0.1008(6) -0.0500(5) 0.4557(7) 0.080 Uiso 1 d R . H17C H -0.1611(6) 0.0125(5) 0.5411(7) 0.080 Uiso 1 d R . C18 C 0.6924(5) -0.1236(5) 0.8854(7) 0.090(2) Uani 1 d . . H18A H 0.7601(5) -0.1470(5) 0.8818(7) 0.080 Uiso 1 d R . H18B H 0.7125(5) -0.0522(5) 0.8906(7) 0.080 Uiso 1 d R . H18C H 0.6583(5) -0.1469(5) 0.9631(7) 0.080 Uiso 1 d R . C19 C 0.5512(4) 0.1116(4) 1.0555(5) 0.0502(14) Uani 1 d . . C20 C 0.5604(4) 0.1356(3) 0.9205(4) 0.0524(13) Uani 1 d . . H20A H 0.4930(4) 0.1147(3) 0.8550(4) 0.080 Uiso 1 d R . C21 C 0.6665(5) 0.1898(4) 0.8898(6) 0.071(2) Uani 1 d . . H21A H 0.6720(5) 0.2066(4) 0.7987(6) 0.080 Uiso 1 d R . C22 C 0.7593(5) 0.2284(4) 0.9867(7) 0.086(2) Uani 1 d . . H22A H 0.8320(5) 0.2609(4) 0.9609(7) 0.080 Uiso 1 d R . C23 C 0.7530(5) 0.2118(4) 1.1153(7) 0.084(2) Uani 1 d . . H23A H 0.8181(5) 0.2392(4) 1.1820(7) 0.080 Uiso 1 d R . C24 C 0.6493(5) 0.1536(5) 1.1517(7) 0.078(2) Uani 1 d . . H24A H 0.6430(5) 0.1470(5) 1.2453(7) 0.080 Uiso 1 d R . C25 C 0.4557(4) -0.0764(3) 1.1679(4) 0.0429(13) Uani 1 d . . C26 C 0.3666(5) -0.1614(4) 1.1577(5) 0.069(2) Uani 1 d . . H26A H 0.2913(5) -0.1553(4) 1.1234(5) 0.080 Uiso 1 d R . C27 C 0.3850(6) -0.2519(4) 1.2094(6) 0.071(2) Uani 1 d . . H27A H 0.3203(6) -0.3087(4) 1.2031(6) 0.080 Uiso 1 d R . C28 C 0.4894(6) -0.2535(4) 1.2658(6) 0.087(2) Uani 1 d . . H28A H 0.4999(6) -0.3139(4) 1.3029(6) 0.080 Uiso 1 d R . C29 C 0.5782(6) -0.1675(5) 1.2681(7) 0.090(2) Uani 1 d . . H29A H 0.6547(6) -0.1702(5) 1.3032(7) 0.080 Uiso 1 d R . C30 C 0.5611(5) -0.0856(4) 1.2217(6) 0.074(2) Uani 1 d . . H30A H 0.6245(5) -0.0278(4) 1.2286(6) 0.080 Uiso 1 d R . C31 C 0.4040(4) 0.1090(3) 1.2495(4) 0.0461(14) Uani 1 d . . C32 C 0.4065(4) 0.0720(4) 1.3781(5) 0.055(2) Uani 1 d . . H32A H 0.4325(4) 0.0135(4) 1.3980(5) 0.080 Uiso 1 d R . C33 C 0.3910(6) 0.1258(4) 1.4869(6) 0.082(2) Uani 1 d . . H33A H 0.3732(6) 0.0993(4) 1.5708(6) 0.080 Uiso 1 d R . C34 C 0.3657(5) 0.2188(5) 1.4579(7) 0.097(3) Uani 1 d . . H34A H 0.3721(5) 0.2646(5) 1.5335(7) 0.080 Uiso 1 d R . C35 C 0.3651(5) 0.2533(5) 1.3359(7) 0.074(2) Uani 1 d . . H35A H 0.3357(5) 0.3107(5) 1.3209(7) 0.080 Uiso 1 d R . C36 C 0.3814(4) 0.1993(3) 1.2312(5) 0.0561(15) Uani 1 d . . H36A H 0.3867(4) 0.2252(3) 1.1443(5) 0.080 Uiso 1 d R . Pd2 Pd 1.16389(2) 0.58651(2) 1.53476(2) 0.04439(11) Uani 1 d . . Cl2 Cl 1.29326(13) 0.52951(14) 1.4148(2) 0.0758(6) Uani 1 d . . P2 P 1.01955(12) 0.54657(10) 1.36273(13) 0.0455(4) Uani 1 d . . N2 N 1.2861(4) 0.6253(3) 1.7091(5) 0.058(2) Uani 1 d . . O2 O 0.8127(3) 0.7303(3) 1.7063(4) 0.0743(14) Uani 1 d . . C41 C 1.0686(5) 0.6508(4) 1.6482(5) 0.0456(15) Uani 1 d . . C42 C 0.9643(4) 0.6694(3) 1.6281(5) 0.0480(15) Uani 1 d . . H42A H 0.9215(4) 0.6488(3) 1.5406(5) 0.080 Uiso 1 d R . C43 C 0.9166(5) 0.7108(4) 1.7262(5) 0.058(2) Uani 1 d . . C44 C 0.9792(5) 0.7380(4) 1.8499(6) 0.061(2) Uani 1 d . . H44A H 0.9477(5) 0.7632(4) 1.9222(6) 0.080 Uiso 1 d R . C45 C 1.0848(7) 0.7228(4) 1.8759(6) 0.074(2) Uani 1 d . . H45A H 1.1325(7) 0.7494(4) 1.9588(6) 0.080 Uiso 1 d R . C46 C 1.1341(5) 0.6786(4) 1.7801(6) 0.063(2) Uani 1 d . . C47 C 1.2486(5) 0.6686(4) 1.7969(5) 0.056(2) Uani 1 d . . H47A H 1.2939(5) 0.6845(4) 1.8838(5) 0.080 Uiso 1 d R . C48 C 1.3972(5) 0.6062(4) 1.7318(6) 0.061(2) Uani 1 d . . H48A H 1.4411(5) 0.6494(4) 1.8064(6) 0.080 Uiso 1 d R . H48B H 1.4352(5) 0.6220(4) 1.6543(6) 0.080 Uiso 1 d R . C49 C 1.3904(5) 0.4964(4) 1.7635(7) 0.078(2) Uani 1 d . . H49A H 1.3394(5) 0.4537(4) 1.6929(7) 0.080 Uiso 1 d R . C50 C 1.5061(5) 0.4751(4) 1.7705(6) 0.069(2) Uani 1 d . . H50A H 1.5462(5) 0.4944(4) 1.6954(6) 0.080 Uiso 1 d R . C51 C 1.5807(5) 0.4941(4) 1.9093(5) 0.0673(15) Uani 1 d . . C52 C 1.5023(6) 0.3938(5) 1.9476(7) 0.084(2) Uani 1 d . . H52A H 1.5431(6) 0.3574(5) 2.0068(7) 0.080 Uiso 1 d R . C53 C 1.3943(6) 0.4063(6) 1.9884(8) 0.143(3) Uani 1 d . . H53A H 1.4044(6) 0.4293(6) 2.0811(8) 0.080 Uiso 1 d R . H53B H 1.3419(6) 0.3416(6) 1.9773(8) 0.080 Uiso 1 d R . C54 C 1.3368(6) 0.4692(6) 1.8883(8) 0.139(3) Uani 1 d . . H54A H 1.2552(6) 0.4434(6) 1.8675(8) 0.080 Uiso 1 d R . H54B H 1.3510(6) 0.5320(6) 1.9381(8) 0.080 Uiso 1 d R . C55 C 1.4857(7) 0.3616(5) 1.8033(7) 0.110(3) Uani 1 d . . H55A H 1.5410(7) 0.3272(5) 1.7805(7) 0.080 Uiso 1 d R . H55B H 1.4089(7) 0.3230(5) 1.7728(7) 0.080 Uiso 1 d R . C56 C 1.7040(5) 0.4886(5) 1.9024(8) 0.114(3) Uani 1 d . . H56A H 1.7014(5) 0.4328(5) 1.8426(8) 0.080 Uiso 1 d R . H56B H 1.7473(5) 0.5482(5) 1.8695(8) 0.080 Uiso 1 d R . H56C H 1.7399(5) 0.4793(5) 1.9901(8) 0.080 Uiso 1 d R . C57 C 1.5852(7) 0.5884(5) 1.9989(7) 0.116(3) Uani 1 d . . H57A H 1.6294(7) 0.5892(5) 2.0852(7) 0.080 Uiso 1 d R . H57B H 1.6119(7) 0.6504(5) 1.9595(7) 0.080 Uiso 1 d R . H57C H 1.5057(7) 0.5792(5) 2.0091(7) 0.080 Uiso 1 d R . C58 C 0.7468(6) 0.7006(6) 1.5864(8) 0.100(3) Uani 1 d . . H58A H 0.6720(6) 0.7127(6) 1.5829(8) 0.080 Uiso 1 d R . H58B H 0.7919(6) 0.7465(6) 1.5330(8) 0.080 Uiso 1 d R . H58C H 0.7396(6) 0.6338(6) 1.5520(8) 0.080 Uiso 1 d R . C59 C 1.0427(4) 0.4819(4) 1.2163(6) 0.0469(15) Uani 1 d . . C60 C 1.0673(5) 0.3882(5) 1.2322(6) 0.069(2) Uani 1 d . . H60A H 1.0845(5) 0.3653(5) 1.3195(6) 0.080 Uiso 1 d R . C61 C 1.0820(6) 0.3299(4) 1.1218(7) 0.076(2) Uani 1 d . . H61A H 1.0821(6) 0.2615(4) 1.1314(7) 0.080 Uiso 1 d R . C62 C 1.0659(6) 0.3635(5) 0.9940(6) 0.069(2) Uani 1 d . . H62A H 1.0933(6) 0.3329(5) 0.9225(6) 0.080 Uiso 1 d R . C63 C 1.0430(6) 0.4499(6) 0.9797(6) 0.083(3) Uani 1 d . . H63A H 1.0160(6) 0.4687(6) 0.8930(6) 0.080 Uiso 1 d R . C64 C 1.0273(6) 0.5134(5) 1.0890(6) 0.073(2) Uani 1 d . . H64A H 1.0236(6) 0.5811(5) 1.0809(6) 0.080 Uiso 1 d R . C65 C 0.8821(4) 0.4669(3) 1.4010(5) 0.0467(15) Uani 1 d . . C66 C 0.7915(5) 0.4339(4) 1.3045(6) 0.068(2) Uani 1 d . . H66A H 0.8005(5) 0.4480(4) 1.2132(6) 0.080 Uiso 1 d R . C67 C 0.6914(6) 0.3836(6) 1.3357(8) 0.092(3) Uani 1 d . . H67A H 0.6239(6) 0.3728(6) 1.2704(8) 0.080 Uiso 1 d R . C68 C 0.6800(5) 0.3579(5) 1.4675(9) 0.098(3) Uani 1 d . . H68A H 0.6119(5) 0.3126(5) 1.4886(9) 0.080 Uiso 1 d R . C69 C 0.7733(6) 0.3807(5) 1.5643(8) 0.084(2) Uani 1 d . . H69A H 0.7663(6) 0.3624(5) 1.6546(8) 0.080 Uiso 1 d R . C70 C 0.8755(5) 0.4397(4) 1.5295(7) 0.061(2) Uani 1 d . . H70A H 0.9387(5) 0.4632(4) 1.6000(7) 0.080 Uiso 1 d R . C71 C 0.9890(5) 0.6616(4) 1.2982(5) 0.050(2) Uani 1 d . . C72 C 0.8781(5) 0.6697(4) 1.2508(6) 0.061(2) Uani 1 d . . H72A H 0.8131(5) 0.6143(4) 1.2522(6) 0.080 Uiso 1 d R . C73 C 0.8649(5) 0.7630(4) 1.1979(6) 0.069(2) Uani 1 d . . H73A H 0.7903(5) 0.7721(4) 1.1663(6) 0.080 Uiso 1 d R . C74 C 0.9572(6) 0.8379(4) 1.1975(6) 0.072(2) Uani 1 d . . H74A H 0.9476(6) 0.8991(4) 1.1624(6) 0.080 Uiso 1 d R . C75 C 1.0680(6) 0.8241(5) 1.2419(7) 0.076(2) Uani 1 d . . H75A H 1.1319(6) 0.8802(5) 1.2384(7) 0.080 Uiso 1 d R . C76 C 1.0802(5) 0.7380(4) 1.2903(6) 0.055(2) Uani 1 d . . H76A H 1.1563(5) 0.7347(4) 1.3263(6) 0.080 Uiso 1 d 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 0.0440(2) 0.0455(2) 0.0445(2) 0.00559(14) 0.0044(2) 0.01515(15) Cl1 0.0558(7) 0.0862(8) 0.0695(8) -0.0008(7) 0.0132(6) 0.0320(6) P1 0.0360(5) 0.0425(6) 0.0396(6) 0.0023(5) 0.0046(5) 0.0087(5) N1 0.041(2) 0.052(2) 0.054(2) 0.012(2) 0.002(2) 0.023(2) O1 0.099(3) 0.114(3) 0.072(2) 0.005(2) 0.031(2) 0.058(2) C1 0.046(2) 0.043(2) 0.046(2) 0.008(2) 0.010(2) 0.026(2) C2 0.057(3) 0.064(3) 0.038(2) 0.000(2) 0.020(2) 0.018(2) C3 0.056(2) 0.047(2) 0.085(4) 0.004(2) 0.026(3) 0.025(2) C4 0.123(4) 0.078(3) 0.032(2) -0.001(2) 0.004(3) 0.048(3) C5 0.074(3) 0.054(3) 0.049(3) -0.005(2) 0.018(2) 0.011(3) C6 0.052(2) 0.044(2) 0.029(2) 0.003(2) 0.013(2) 0.009(2) C7 0.066(3) 0.058(3) 0.052(3) 0.029(2) 0.004(2) 0.021(2) C8 0.037(2) 0.075(3) 0.075(3) 0.021(3) 0.005(2) 0.027(2) C9 0.078(3) 0.053(3) 0.047(3) 0.003(2) -0.003(2) 0.022(2) C10 0.094(3) 0.087(3) 0.070(3) 0.000(3) 0.036(3) 0.046(3) C11 0.113(4) 0.112(4) 0.095(4) 0.031(3) 0.048(3) 0.078(3) C12 0.107(4) 0.076(3) 0.070(3) 0.010(3) 0.017(3) 0.063(3) C13 0.101(4) 0.067(3) 0.073(3) 0.016(3) 0.021(3) 0.024(3) C14 0.070(3) 0.049(2) 0.053(3) 0.003(2) 0.003(2) 0.023(2) C15 0.084(3) 0.077(3) 0.057(3) -0.006(2) 0.003(3) 0.035(3) C16 0.141(5) 0.099(4) 0.061(3) 0.006(3) 0.018(3) 0.061(4) C17 0.087(4) 0.130(5) 0.093(5) 0.029(4) -0.016(4) 0.031(4) C18 0.051(3) 0.130(5) 0.097(5) 0.010(4) 0.004(3) 0.044(3) C19 0.047(2) 0.055(3) 0.053(3) -0.010(2) 0.008(2) 0.022(2) C20 0.082(3) 0.038(2) 0.051(2) 0.017(2) 0.043(2) 0.022(2) C21 0.073(3) 0.049(3) 0.092(3) 0.002(3) 0.049(3) -0.001(3) C22 0.078(3) 0.068(3) 0.132(5) 0.032(3) 0.066(3) 0.026(3) C23 0.049(3) 0.069(4) 0.124(5) -0.019(4) 0.032(3) -0.008(3) C24 0.064(3) 0.080(4) 0.090(4) 0.005(3) 0.018(3) 0.016(3) C25 0.045(2) 0.041(2) 0.041(2) -0.003(2) 0.010(2) 0.005(2) C26 0.075(3) 0.051(3) 0.071(3) 0.003(3) -0.027(3) 0.016(3) C27 0.097(4) 0.041(3) 0.073(3) 0.007(2) 0.004(3) 0.018(3) C28 0.141(5) 0.075(3) 0.054(3) -0.011(3) -0.007(4) 0.057(4) C29 0.080(4) 0.082(4) 0.114(5) 0.009(4) 0.004(4) 0.037(3) C30 0.055(3) 0.068(3) 0.092(4) 0.011(3) -0.008(3) 0.013(3) C31 0.044(2) 0.045(2) 0.041(2) -0.006(2) 0.009(2) -0.003(2) C32 0.059(3) 0.056(3) 0.047(3) 0.002(2) 0.001(2) 0.011(2) C33 0.097(4) 0.076(4) 0.070(3) -0.020(3) 0.033(3) 0.011(3) C34 0.076(4) 0.084(4) 0.116(5) -0.039(4) 0.034(4) -0.016(4) C35 0.045(3) 0.067(3) 0.103(5) -0.003(3) 0.006(3) 0.004(3) C36 0.057(3) 0.047(2) 0.072(3) -0.006(2) 0.019(2) 0.023(2) Pd2 0.0404(2) 0.0483(2) 0.0467(2) 0.0069(2) 0.0034(2) 0.0163(2) Cl2 0.0560(8) 0.1152(13) 0.0658(9) 0.0011(9) 0.0099(7) 0.0399(8) P2 0.0466(7) 0.0450(7) 0.0474(7) 0.0034(6) 0.0101(6) 0.0145(6) N2 0.059(3) 0.044(2) 0.059(3) 0.012(2) -0.013(2) 0.002(2) O2 0.064(2) 0.088(3) 0.084(3) -0.017(2) 0.015(2) 0.044(2) C41 0.053(3) 0.042(3) 0.035(2) 0.000(2) -0.005(2) 0.004(2) C42 0.053(3) 0.040(2) 0.055(3) 0.004(2) 0.000(2) 0.025(2) C43 0.083(4) 0.059(3) 0.035(3) 0.006(2) 0.010(3) 0.024(3) C44 0.073(3) 0.046(3) 0.072(4) 0.003(3) 0.035(3) 0.018(3) C45 0.117(5) 0.060(3) 0.040(3) 0.008(3) -0.011(3) 0.026(4) C46 0.071(4) 0.042(3) 0.075(4) 0.008(3) -0.008(3) 0.019(3) C47 0.071(4) 0.041(3) 0.045(3) -0.004(2) -0.016(3) 0.005(3) C48 0.055(3) 0.039(3) 0.078(4) 0.005(3) -0.010(3) 0.003(2) C49 0.038(3) 0.060(3) 0.126(5) 0.020(3) -0.020(3) 0.010(3) C50 0.082(3) 0.070(3) 0.063(3) -0.006(3) 0.008(3) 0.037(3) C51 0.076(3) 0.072(3) 0.058(3) -0.004(2) -0.006(3) 0.036(2) C52 0.092(4) 0.098(4) 0.075(4) 0.041(3) 0.012(4) 0.045(4) C53 0.118(5) 0.174(5) 0.183(6) 0.134(4) 0.059(5) 0.088(4) C54 0.089(5) 0.145(5) 0.212(7) 0.124(5) 0.065(5) 0.051(4) C55 0.143(5) 0.081(4) 0.112(5) -0.011(4) -0.035(5) 0.070(4) C56 0.071(3) 0.141(5) 0.146(6) 0.050(5) 0.004(4) 0.055(4) C57 0.146(6) 0.079(4) 0.110(5) -0.049(3) -0.076(4) 0.056(4) C58 0.088(4) 0.101(4) 0.129(6) -0.029(4) 0.031(4) 0.052(4) C59 0.039(2) 0.037(2) 0.068(3) 0.001(2) 0.009(2) 0.013(2) C60 0.072(4) 0.065(4) 0.064(4) 0.001(3) 0.010(3) 0.008(3) C61 0.096(4) 0.052(3) 0.089(4) -0.018(3) 0.043(3) 0.022(3) C62 0.078(4) 0.074(4) 0.052(3) -0.018(3) 0.026(3) 0.008(3) C63 0.086(5) 0.108(5) 0.042(3) 0.015(3) 0.016(3) -0.004(4) C64 0.095(5) 0.072(4) 0.051(3) -0.001(3) 0.027(3) 0.009(4) C65 0.047(3) 0.032(2) 0.058(3) 0.011(2) 0.015(2) 0.000(2) C66 0.053(3) 0.067(4) 0.067(4) -0.013(3) 0.006(3) -0.016(3) C67 0.053(4) 0.100(5) 0.108(5) 0.016(4) 0.002(4) -0.005(4) C68 0.040(3) 0.072(4) 0.164(7) -0.024(5) 0.025(4) -0.017(3) C69 0.105(4) 0.069(3) 0.106(5) 0.037(3) 0.058(4) 0.046(3) C70 0.041(3) 0.048(3) 0.090(4) -0.007(3) 0.003(3) 0.010(2) C71 0.056(3) 0.056(3) 0.043(3) 0.004(2) -0.008(2) 0.028(2) C72 0.060(3) 0.073(3) 0.063(3) 0.020(3) 0.015(3) 0.037(3) C73 0.081(3) 0.084(3) 0.064(3) 0.022(3) 0.005(3) 0.062(3) C74 0.107(4) 0.055(3) 0.071(4) 0.024(3) 0.023(3) 0.045(3) C75 0.086(4) 0.056(3) 0.080(4) 0.002(3) 0.004(4) 0.010(3) C76 0.052(3) 0.043(3) 0.067(3) 0.012(2) 0.011(3) 0.007(2) _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 C1 2.011(5) . ? Pd1 N1 2.082(4) . ? Pd1 P1 2.2644(14) . ? Pd1 Cl1 2.380(2) . ? P1 C19 1.785(5) . ? P1 C25 1.825(5) . ? P1 C31 1.858(5) . ? N1 C7 1.299(7) . ? N1 C8 1.511(6) . ? O1 C3 1.372(7) . ? O1 C18 1.466(7) . ? C1 C6 1.350(6) . ? C1 C2 1.427(7) . ? C2 C3 1.406(7) . ? C3 C4 1.415(7) . ? C4 C5 1.378(9) . ? C5 C6 1.413(7) . ? C6 C7 1.470(7) . ? C8 C9 1.522(7) . ? C9 C14 1.515(7) . ? C9 C10 1.573(8) . ? C10 C11 1.511(8) . ? C11 C12 1.474(8) . ? C12 C15 1.544(8) . ? C12 C13 1.590(8) . ? C13 C14 1.555(7) . ? C14 C15 1.582(7) . ? C15 C17 1.487(8) . ? C15 C16 1.521(8) . ? C19 C20 1.421(7) . ? C19 C24 1.424(7) . ? C20 C21 1.401(7) . ? C21 C22 1.378(8) . ? C22 C23 1.330(10) . ? C23 C24 1.417(8) . ? C25 C30 1.362(7) . ? C25 C26 1.385(6) . ? C26 C27 1.433(8) . ? C27 C28 1.327(9) . ? C28 C29 1.397(9) . ? C29 C30 1.297(9) . ? C31 C36 1.362(7) . ? C31 C32 1.408(7) . ? C32 C33 1.367(8) . ? C33 C34 1.431(10) . ? C34 C35 1.332(9) . ? C35 C36 1.338(8) . ? Pd2 C41 2.055(6) . ? Pd2 N2 2.111(4) . ? Pd2 P2 2.250(2) . ? Pd2 Cl2 2.364(2) . ? P2 C59 1.792(6) . ? P2 C71 1.847(6) . ? P2 C65 1.856(5) . ? N2 C47 1.247(8) . ? N2 C48 1.429(8) . ? O2 C43 1.345(8) . ? O2 C58 1.352(8) . ? C41 C42 1.345(8) . ? C41 C46 1.446(7) . ? C42 C43 1.385(8) . ? C43 C44 1.364(8) . ? C44 C45 1.343(9) . ? C45 C46 1.399(9) . ? C46 C47 1.420(9) . ? C48 C49 1.555(8) . ? C49 C50 1.498(9) . ? C49 C54 1.504(10) . ? C50 C51 1.542(7) . ? C50 C55 1.589(8) . ? C51 C56 1.527(8) . ? C51 C57 1.555(8) . ? C51 C52 1.573(8) . ? C52 C53 1.471(10) . ? C52 C55 1.481(9) . ? C53 C54 1.563(10) . ? C59 C64 1.372(8) . ? C59 C60 1.416(8) . ? C60 C61 1.411(9) . ? C61 C62 1.388(9) . ? C62 C63 1.307(10) . ? C63 C64 1.450(9) . ? C65 C66 1.347(7) . ? C65 C70 1.365(8) . ? C66 C67 1.327(9) . ? C67 C68 1.399(11) . ? C68 C69 1.362(10) . ? C69 C70 1.402(9) . ? C71 C76 1.347(7) . ? C71 C72 1.402(8) . ? C72 C73 1.455(8) . ? C73 C74 1.330(8) . ? C74 C75 1.422(10) . ? C75 C76 1.341(8) . ? 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 C1 Pd1 N1 78.8(2) . . ? C1 Pd1 P1 95.65(13) . . ? N1 Pd1 P1 173.86(11) . . ? C1 Pd1 Cl1 170.66(12) . . ? N1 Pd1 Cl1 92.93(12) . . ? P1 Pd1 Cl1 92.82(5) . . ? C19 P1 C25 107.5(2) . . ? C19 P1 C31 100.7(2) . . ? C25 P1 C31 104.8(2) . . ? C19 P1 Pd1 114.3(2) . . ? C25 P1 Pd1 110.67(14) . . ? C31 P1 Pd1 117.9(2) . . ? C7 N1 C8 118.9(4) . . ? C7 N1 Pd1 115.7(3) . . ? C8 N1 Pd1 125.4(3) . . ? C3 O1 C18 119.0(5) . . ? C6 C1 C2 118.1(4) . . ? C6 C1 Pd1 115.1(3) . . ? C2 C1 Pd1 126.8(3) . . ? C3 C2 C1 118.4(4) . . ? O1 C3 C2 123.6(5) . . ? O1 C3 C4 114.3(5) . . ? C2 C3 C4 122.1(5) . . ? C5 C4 C3 118.1(5) . . ? C4 C5 C6 119.2(5) . . ? C1 C6 C5 123.9(5) . . ? C1 C6 C7 116.1(4) . . ? C5 C6 C7 119.9(4) . . ? N1 C7 C6 114.2(4) . . ? N1 C8 C9 111.1(4) . . ? C14 C9 C8 115.6(5) . . ? C14 C9 C10 112.4(5) . . ? C8 C9 C10 111.5(4) . . ? C11 C10 C9 114.9(5) . . ? C12 C11 C10 113.8(5) . . ? C11 C12 C15 115.4(5) . . ? C11 C12 C13 107.2(5) . . ? C15 C12 C13 87.3(4) . . ? C14 C13 C12 85.4(4) . . ? C9 C14 C13 107.1(4) . . ? C9 C14 C15 112.4(4) . . ? C13 C14 C15 87.2(4) . . ? C17 C15 C16 109.7(5) . . ? C17 C15 C12 114.7(5) . . ? C16 C15 C12 113.8(5) . . ? C17 C15 C14 121.8(5) . . ? C16 C15 C14 109.1(5) . . ? C12 C15 C14 86.1(4) . . ? C20 C19 C24 116.2(5) . . ? C20 C19 P1 121.3(3) . . ? C24 C19 P1 122.5(4) . . ? C21 C20 C19 118.6(5) . . ? C22 C21 C20 122.7(6) . . ? C23 C22 C21 120.7(6) . . ? C22 C23 C24 119.1(6) . . ? C23 C24 C19 122.5(6) . . ? C30 C25 C26 116.4(5) . . ? C30 C25 P1 126.5(4) . . ? C26 C25 P1 117.0(4) . . ? C25 C26 C27 120.8(5) . . ? C28 C27 C26 118.9(5) . . ? C27 C28 C29 118.5(6) . . ? C30 C29 C28 122.3(7) . . ? C29 C30 C25 122.9(5) . . ? C36 C31 C32 119.5(5) . . ? C36 C31 P1 118.6(4) . . ? C32 C31 P1 121.9(4) . . ? C33 C32 C31 121.7(5) . . ? C32 C33 C34 114.8(6) . . ? C35 C34 C33 122.5(7) . . ? C34 C35 C36 121.3(6) . . ? C35 C36 C31 120.0(5) . . ? C41 Pd2 N2 82.4(2) . . ? C41 Pd2 P2 91.92(14) . . ? N2 Pd2 P2 173.93(15) . . ? C41 Pd2 Cl2 172.78(14) . . ? N2 Pd2 Cl2 92.3(2) . . ? P2 Pd2 Cl2 93.58(6) . . ? C59 P2 C71 103.5(2) . . ? C59 P2 C65 102.2(2) . . ? C71 P2 C65 107.1(3) . . ? C59 P2 Pd2 117.6(2) . . ? C71 P2 Pd2 109.2(2) . . ? C65 P2 Pd2 116.0(2) . . ? C47 N2 C48 121.7(5) . . ? C47 N2 Pd2 110.7(4) . . ? C48 N2 Pd2 127.6(4) . . ? C43 O2 C58 118.1(5) . . ? C42 C41 C46 116.8(5) . . ? C42 C41 Pd2 135.3(4) . . ? C46 C41 Pd2 107.8(4) . . ? C41 C42 C43 123.9(5) . . ? O2 C43 C44 116.8(5) . . ? O2 C43 C42 124.2(5) . . ? C44 C43 C42 119.0(6) . . ? C45 C44 C43 120.0(6) . . ? C44 C45 C46 122.3(5) . . ? C45 C46 C47 125.1(5) . . ? C45 C46 C41 117.9(6) . . ? C47 C46 C41 116.6(6) . . ? N2 C47 C46 121.8(5) . . ? N2 C48 C49 111.9(4) . . ? C50 C49 C54 111.8(6) . . ? C50 C49 C48 110.9(5) . . ? C54 C49 C48 112.2(6) . . ? C49 C50 C51 116.2(5) . . ? C49 C50 C55 105.1(5) . . ? C51 C50 C55 83.9(4) . . ? C56 C51 C50 112.5(5) . . ? C56 C51 C57 107.9(5) . . ? C50 C51 C57 119.6(5) . . ? C56 C51 C52 112.9(5) . . ? C50 C51 C52 86.8(4) . . ? C57 C51 C52 116.2(5) . . ? C53 C52 C55 110.6(6) . . ? C53 C52 C51 112.4(6) . . ? C55 C52 C51 86.5(5) . . ? C52 C53 C54 111.1(6) . . ? C49 C54 C53 117.4(7) . . ? C52 C55 C50 88.3(5) . . ? C64 C59 C60 118.4(6) . . ? C64 C59 P2 123.8(5) . . ? C60 C59 P2 117.5(4) . . ? C61 C60 C59 121.6(6) . . ? C62 C61 C60 118.8(6) . . ? C63 C62 C61 119.4(6) . . ? C62 C63 C64 124.4(6) . . ? C59 C64 C63 117.3(6) . . ? C66 C65 C70 120.3(5) . . ? C66 C65 P2 121.3(4) . . ? C70 C65 P2 118.3(4) . . ? C67 C66 C65 120.3(6) . . ? C66 C67 C68 120.7(6) . . ? C69 C68 C67 120.1(7) . . ? C68 C69 C70 117.3(7) . . ? C65 C70 C69 120.7(5) . . ? C76 C71 C72 119.9(5) . . ? C76 C71 P2 116.7(4) . . ? C72 C71 P2 123.3(4) . . ? C71 C72 C73 118.4(5) . . ? C74 C73 C72 119.5(6) . . ? C73 C74 C75 119.7(6) . . ? C76 C75 C74 120.8(6) . . ? C75 C76 C71 121.6(6) . . ? _refine_diff_density_max 0.285 _refine_diff_density_min -0.380 _refine_diff_density_rms 0.056 #=END data_zgb17 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C35.50 H38 Br Cl Fe0.50 N O P Pd' _chemical_formula_weight 775.32 _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' 'Br' 'Br' -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' 0.3463 0.8444 '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 ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 16.730(3) _cell_length_b 16.415(3) _cell_length_c 25.250(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.70(3) _cell_angle_gamma 90.00 _cell_volume 6933.7(22) _cell_formula_units_Z 8 _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 ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.485 _exptl_crystal_density_method ? _exptl_crystal_F_000 3136 _exptl_absorpt_coefficient_mu 2.040 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _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 ? _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20315 _diffrn_reflns_av_R_equivalents 0.0624 _diffrn_reflns_av_sigmaI/netI 0.0784 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.22 _diffrn_reflns_theta_max 25.50 _reflns_number_total 12097 _reflns_number_observed 10414 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 5 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^)+(0.0889P)^2^+5.1309P] 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 ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00220(8) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.08(2) _refine_ls_number_reflns 12092 _refine_ls_number_parameters 1514 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0834 _refine_ls_R_factor_obs 0.0694 _refine_ls_wR_factor_all 0.1797 _refine_ls_wR_factor_obs 0.1667 _refine_ls_goodness_of_fit_all 1.108 _refine_ls_goodness_of_fit_obs 1.142 _refine_ls_restrained_S_all 1.136 _refine_ls_restrained_S_obs 1.142 _refine_ls_shift/esd_max 0.055 _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 0.03359(3) 0.43352(3) -0.37030(2) 0.06554(13) Uani 1 d . . Pd2 Pd 0.19255(3) 0.52197(3) -0.69007(2) 0.05913(11) Uani 1 d . . Fe1 Fe 0.13521(5) 0.51984(6) -0.52306(3) 0.0645(2) Uani 1 d . . Br1 Br 0.05239(5) 0.31840(5) -0.43552(3) 0.0892(2) Uani 1 d . . Br2 Br 0.27356(4) 0.39123(4) -0.68539(3) 0.0758(2) Uani 1 d . . P1 P 0.15579(9) 0.48760(10) -0.38613(6) 0.0612(4) Uani 1 d . . P2 P 0.08539(9) 0.46174(10) -0.65250(6) 0.0608(4) Uani 1 d . . O1 O 0.0862(4) 0.6158(4) -0.1858(2) 0.110(2) Uani 1 d . . O2 O -0.0462(3) 0.7522(4) -0.7291(2) 0.107(2) Uani 1 d . . N1 N -0.0852(3) 0.4010(4) -0.3588(2) 0.083(2) Uani 1 d . . N2 N 0.2915(3) 0.5910(4) -0.7157(2) 0.071(2) Uani 1 d . . C1 C 0.1918(4) 0.4949(4) -0.4535(2) 0.071(2) Uani 1 d . . C2 C 0.2212(4) 0.5678(5) -0.4773(2) 0.083(2) Uani 1 d . . H2 H 0.2193(4) 0.6197(5) -0.4627(2) 0.099 Uiso 1 calc R . C3 C 0.2541(4) 0.5469(5) -0.5276(2) 0.082(2) Uani 1 d . . H3 H 0.2790(4) 0.5826(5) -0.5507(2) 0.098 Uiso 1 calc R . C4 C 0.2424(4) 0.4654(5) -0.5357(2) 0.084(2) Uani 1 d . . H4 H 0.2568(4) 0.4368(5) -0.5658(2) 0.100 Uiso 1 calc R . C5 C 0.2048(4) 0.4313(5) -0.4906(2) 0.079(2) Uani 1 d . . H5 H 0.1910(4) 0.3768(5) -0.4861(2) 0.095 Uiso 1 calc R . C6 C 0.0653(4) 0.5064(4) -0.5890(2) 0.070(2) Uani 1 d . . C7 C 0.0789(4) 0.5920(4) -0.5783(2) 0.073(2) Uani 1 d . . H7 H 0.1040(4) 0.6288(4) -0.6007(2) 0.087 Uiso 1 calc R . C8 C 0.0474(4) 0.6097(4) -0.5282(3) 0.076(2) Uani 1 d . . H8 H 0.0475(4) 0.6609(4) -0.5124(3) 0.092 Uiso 1 calc R . C9 C 0.0167(4) 0.5403(4) -0.5061(3) 0.078(2) Uani 1 d . . H9 H -0.0058(4) 0.5361(4) -0.4727(3) 0.094 Uiso 1 calc R . C10 C 0.0251(3) 0.4766(5) -0.5431(2) 0.075(2) Uani 1 d . . H10 H 0.0074(3) 0.4234(5) -0.5384(2) 0.091 Uiso 1 calc R . C11 C -0.0661(4) 0.4889(4) -0.2865(2) 0.071(2) Uani 1 d . . C12 C 0.0104(3) 0.4991(4) -0.3034(2) 0.064(2) Uani 1 d . . C13 C 0.0622(4) 0.5438(4) -0.2697(2) 0.069(2) Uani 1 d . . H13 H 0.1141(4) 0.5541(4) -0.2806(2) 0.083 Uiso 1 calc R . C14 C 0.0376(5) 0.5732(4) -0.2204(2) 0.079(2) Uani 1 d . . C15 C -0.0393(4) 0.5649(4) -0.2044(2) 0.082(2) Uani 1 d . . H15 H -0.0558(4) 0.5865(4) -0.1722(2) 0.098 Uiso 1 calc R . C16 C -0.0948(4) 0.5218(5) -0.2384(3) 0.093(2) Uani 1 d . . H16 H -0.1481(4) 0.5157(5) -0.2291(3) 0.112 Uiso 1 calc R . C17 C -0.1180(4) 0.4388(4) -0.3178(2) 0.076(2) Uani 1 d . . H17 H -0.1719(4) 0.4329(4) -0.3100(2) 0.091 Uiso 1 calc R . C18 C -0.1399(4) 0.3543(4) -0.3930(3) 0.082(2) Uani 1 d . . H18A H -0.1906(4) 0.3476(4) -0.3753(3) 0.099 Uiso 1 calc R . H18B H -0.1176(4) 0.3006(4) -0.3991(3) 0.099 Uiso 1 calc R . C19 C -0.1540(4) 0.3986(5) -0.4479(2) 0.075(2) Uani 1 d . . H19 H -0.1010(4) 0.4097(5) -0.4623(2) 0.090 Uiso 1 calc R . C20 C -0.1946(5) 0.4820(5) -0.4399(3) 0.089(2) Uani 1 d . . H20A H -0.2151(5) 0.4841(5) -0.4042(3) 0.107 Uiso 1 calc R . H20B H -0.1543(5) 0.5241(5) -0.4429(3) 0.107 Uiso 1 calc R . C21 C -0.2631(5) 0.5019(6) -0.4785(4) 0.115(3) Uani 1 d . . H21A H -0.2494(5) 0.5500(6) -0.4989(4) 0.137 Uiso 1 calc R . H21B H -0.3109(5) 0.5140(6) -0.4587(4) 0.137 Uiso 1 calc R . C22 C -0.2803(5) 0.4287(7) -0.5175(3) 0.124(3) Uani 1 d . . H22 H -0.3218(5) 0.4386(7) -0.5444(3) 0.149 Uiso 1 calc R . C23 C -0.2041(5) 0.3991(8) -0.5377(3) 0.120(4) Uani 1 d . . H23A H -0.1634(5) 0.4409(8) -0.5404(3) 0.143 Uiso 1 calc R . H23B H -0.2090(5) 0.3684(8) -0.5704(3) 0.143 Uiso 1 calc R . C24 C -0.1957(4) 0.3440(6) -0.4865(3) 0.092(3) Uani 1 d . . H24 H -0.1736(4) 0.2892(6) -0.4911(3) 0.110 Uiso 1 calc R . C25 C -0.2905(5) 0.3521(5) -0.4853(3) 0.087(2) Uani 1 d . . C26 C -0.3293(5) 0.3506(5) -0.4307(3) 0.104(3) Uani 1 d . . H26A H -0.3078(5) 0.3940(5) -0.4093(3) 0.156 Uiso 1 calc R . H26B H -0.3183(5) 0.2993(5) -0.4138(3) 0.156 Uiso 1 calc R . H26C H -0.3860(5) 0.3575(5) -0.4346(3) 0.156 Uiso 1 calc R . C27 C -0.3254(6) 0.2839(8) -0.5174(4) 0.149(4) Uani 1 d . . H27A H -0.3311(6) 0.2365(8) -0.4955(4) 0.224 Uiso 1 calc R . H27B H -0.2907(6) 0.2716(8) -0.5463(4) 0.224 Uiso 1 calc R . H27C H -0.3769(6) 0.2998(8) -0.5311(4) 0.224 Uiso 1 calc R . C28 C 0.1637(6) 0.6320(8) -0.2020(3) 0.140(4) Uani 1 d . . H28A H 0.1915(6) 0.6619(8) -0.1749(3) 0.210 Uiso 1 calc R . H28B H 0.1620(6) 0.6637(8) -0.2340(3) 0.210 Uiso 1 calc R . H28C H 0.1910(6) 0.5817(8) -0.2085(3) 0.210 Uiso 1 calc R . C29 C 0.1933(4) 0.6842(5) -0.7316(2) 0.080(2) Uani 1 d . . C30 C 0.1371(3) 0.6294(4) -0.7096(2) 0.068(2) Uani 1 d . . C31 C 0.0564(4) 0.6528(4) -0.7059(2) 0.077(2) Uani 1 d . . H31 H 0.0197(4) 0.6199(4) -0.6887(2) 0.092 Uiso 1 calc R . C32 C 0.0328(4) 0.7269(4) -0.7285(2) 0.076(2) Uani 1 d . . C33 C 0.0856(5) 0.7765(4) -0.7510(2) 0.087(2) Uani 1 d . . H33 H 0.0676(5) 0.8252(4) -0.7658(2) 0.104 Uiso 1 calc R . C34 C 0.1637(5) 0.7586(4) -0.7530(3) 0.083(2) Uani 1 d . . H34 H 0.1988(5) 0.7952(4) -0.7684(3) 0.099 Uiso 1 calc R . C35 C 0.2717(4) 0.6621(4) -0.7329(2) 0.072(2) Uani 1 d . . H35 H 0.3101(4) 0.6975(4) -0.7460(2) 0.086 Uiso 1 calc R . C36 C 0.3757(3) 0.5686(4) -0.7118(2) 0.073(2) Uani 1 d . . H36A H 0.4077(3) 0.6075(4) -0.7312(2) 0.088 Uiso 1 calc R . H36B H 0.3836(3) 0.5152(4) -0.7274(2) 0.088 Uiso 1 calc R . C37 C 0.4026(4) 0.5673(5) -0.6531(3) 0.077(2) Uani 1 d . . H37 H 0.3626(4) 0.5354(5) -0.6340(3) 0.093 Uiso 1 calc R . C38 C 0.4032(5) 0.6508(5) -0.6288(3) 0.092(2) Uani 1 d . . H38A H 0.3523(5) 0.6589(5) -0.6116(3) 0.111 Uiso 1 calc R . H38B H 0.4062(5) 0.6903(5) -0.6573(3) 0.111 Uiso 1 calc R . C39 C 0.4692(5) 0.6709(8) -0.5886(4) 0.160(4) Uani 1 d . . H39A H 0.4463(5) 0.6767(8) -0.5537(4) 0.192 Uiso 1 calc R . H39B H 0.4940(5) 0.7222(8) -0.5980(4) 0.192 Uiso 1 calc R . C40 C 0.5345(5) 0.6014(7) -0.5874(3) 0.111(3) Uani 1 d . . H40 H 0.5792(5) 0.6117(7) -0.5628(3) 0.133 Uiso 1 calc R . C41 C 0.4999(4) 0.5226(8) -0.5826(3) 0.115(3) Uani 1 d . . H41A H 0.4521(4) 0.5213(8) -0.5612(3) 0.138 Uiso 1 calc R . H41B H 0.5374(4) 0.4806(8) -0.5717(3) 0.138 Uiso 1 calc R . C42 C 0.4828(4) 0.5253(5) -0.6439(3) 0.084(2) Uani 1 d . . H42 H 0.4893(4) 0.4732(5) -0.6623(3) 0.101 Uiso 1 calc R . C43 C 0.5596(5) 0.5839(8) -0.6444(4) 0.119(4) Uani 1 d . . C44 C 0.6337(5) 0.5265(9) -0.6456(4) 0.165(5) Uani 1 d . . H44A H 0.6302(5) 0.4875(9) -0.6174(4) 0.247 Uiso 1 calc R . H44B H 0.6816(5) 0.5582(9) -0.6413(4) 0.247 Uiso 1 calc R . H44C H 0.6349(5) 0.4984(9) -0.6790(4) 0.247 Uiso 1 calc R . C45 C 0.5636(6) 0.6465(6) -0.6890(4) 0.116(3) Uani 1 d . . H45A H 0.5809(6) 0.6203(6) -0.7209(4) 0.174 Uiso 1 calc R . H45B H 0.6008(6) 0.6887(6) -0.6794(4) 0.174 Uiso 1 calc R . H45C H 0.5116(6) 0.6699(6) -0.6948(4) 0.174 Uiso 1 calc R . C46 C -0.1038(5) 0.7031(6) -0.7030(4) 0.125(4) Uani 1 d . . H46A H -0.1557(5) 0.7277(6) -0.7066(4) 0.188 Uiso 1 calc R . H46B H -0.0898(5) 0.6985(6) -0.6661(4) 0.188 Uiso 1 calc R . H46C H -0.1049(5) 0.6498(6) -0.7187(4) 0.188 Uiso 1 calc R . C47 C 0.2370(4) 0.4342(3) -0.3513(2) 0.063(2) Uani 1 d . . C48 C 0.3101(4) 0.4251(5) -0.3703(3) 0.090(2) Uani 1 d . . H48 H 0.3221(4) 0.4486(5) -0.4028(3) 0.108 Uiso 1 calc R . C49 C 0.3693(5) 0.3816(6) -0.3436(3) 0.104(3) Uani 1 d . . H49 H 0.4176(5) 0.3695(6) -0.3596(3) 0.125 Uiso 1 calc R . C50 C 0.3536(5) 0.3573(5) -0.2928(3) 0.101(3) Uani 1 d . . H50 H 0.3943(5) 0.3343(5) -0.2723(3) 0.122 Uiso 1 calc R . C51 C 0.2824(5) 0.3660(5) -0.2727(3) 0.112(3) Uani 1 d . . H51 H 0.2729(5) 0.3484(5) -0.2383(3) 0.134 Uiso 1 calc R . C52 C 0.2218(5) 0.4006(5) -0.3015(3) 0.090(2) Uani 1 d . . H52 H 0.1703(5) 0.4018(5) -0.2881(3) 0.108 Uiso 1 calc R . C53 C 0.1663(4) 0.5927(4) -0.3667(2) 0.063(2) Uani 1 d . . C54 C 0.2365(4) 0.6246(4) -0.3418(3) 0.077(2) Uani 1 d . . H54 H 0.2792(4) 0.5905(4) -0.3334(3) 0.093 Uiso 1 calc R . C55 C 0.2403(4) 0.7095(6) -0.3300(3) 0.097(3) Uani 1 d . . H55 H 0.2856(4) 0.7315(6) -0.3138(3) 0.117 Uiso 1 calc R . C56 C 0.1777(5) 0.7570(5) -0.3426(3) 0.095(2) Uani 1 d . . H56 H 0.1809(5) 0.8123(5) -0.3349(3) 0.114 Uiso 1 calc R . C57 C 0.1100(5) 0.7287(4) -0.3659(3) 0.092(3) Uani 1 d . . H57 H 0.0680(5) 0.7643(4) -0.3731(3) 0.111 Uiso 1 calc R . C58 C 0.1025(4) 0.6466(5) -0.3793(2) 0.078(2) Uani 1 d . . H58 H 0.0564(4) 0.6275(5) -0.3961(2) 0.093 Uiso 1 calc R . C59 C -0.0093(4) 0.4695(4) -0.6893(2) 0.070(2) Uani 1 d . . C60 C -0.0819(4) 0.4751(4) -0.6634(3) 0.080(2) Uani 1 d . . H60 H -0.0822(4) 0.4758(4) -0.6266(3) 0.096 Uiso 1 calc R . C61 C -0.1567(4) 0.4799(5) -0.6921(3) 0.095(3) Uani 1 d . . H61 H -0.2049(4) 0.4825(5) -0.6741(3) 0.114 Uiso 1 calc R . C62 C -0.1556(6) 0.4806(6) -0.7439(4) 0.123(3) Uani 1 d . . H62 H -0.2033(6) 0.4876(6) -0.7625(4) 0.148 Uiso 1 calc R . C63 C -0.0812(6) 0.4705(8) -0.7735(4) 0.135(4) Uani 1 d . . H63 H -0.0817(6) 0.4645(8) -0.8101(4) 0.162 Uiso 1 calc R . C64 C -0.0090(5) 0.4704(6) -0.7441(3) 0.099(3) Uani 1 d . . H64 H 0.0394(5) 0.4709(6) -0.7617(3) 0.119 Uiso 1 calc R . C65 C 0.0939(4) 0.3537(4) -0.6423(2) 0.071(2) Uani 1 d . . C66 C 0.0815(4) 0.2998(4) -0.6858(2) 0.071(2) Uani 1 d . . H66 H 0.0681(4) 0.3209(4) -0.7190(2) 0.086 Uiso 1 calc R . C67 C 0.0892(5) 0.2153(4) -0.6793(4) 0.103(3) Uani 1 d . . H67 H 0.0816(5) 0.1805(4) -0.7080(4) 0.124 Uiso 1 calc R . C68 C 0.1071(4) 0.1860(5) -0.6320(3) 0.087(2) Uani 1 d . . H68 H 0.1090(4) 0.1298(5) -0.6276(3) 0.105 Uiso 1 calc R . C69 C 0.1227(5) 0.2329(5) -0.5906(3) 0.097(3) Uani 1 d . . H69 H 0.1400(5) 0.2099(5) -0.5588(3) 0.117 Uiso 1 calc R . C70 C 0.1132(4) 0.3160(4) -0.5948(3) 0.084(2) Uani 1 d . . H70 H 0.1199(4) 0.3479(4) -0.5647(3) 0.101 Uiso 1 calc R . Pd1' Pd -0.68284(3) 0.38489(3) 0.02377(2) 0.06729(13) Uani 1 d . . Pd2' Pd -0.32134(3) 0.50160(3) -0.20528(2) 0.08009(15) Uani 1 d . . Fe1' Fe -0.53137(5) 0.49128(6) -0.09869(3) 0.0672(2) Uani 1 d . . Br1' Br -0.61197(5) 0.27278(5) -0.02722(3) 0.0898(2) Uani 1 d . . Br2' Br -0.37119(6) 0.38072(6) -0.25892(3) 0.1106(3) Uani 1 d . . P1' P -0.72340(10) 0.45086(10) -0.05143(6) 0.0635(4) Uani 1 d . . P2' P -0.33367(10) 0.43139(12) -0.12823(7) 0.0768(5) Uani 1 d . . N1' N -0.6352(4) 0.3467(3) 0.0973(2) 0.080(2) Uani 1 d . . N2' N -0.3085(3) 0.5768(4) -0.2743(2) 0.093(2) Uani 1 d . . O1' O -0.9405(4) 0.5659(4) 0.0879(3) 0.143(2) Uani 1 d . . O2' O -0.1825(4) 0.7150(4) -0.0554(2) 0.119(2) Uani 1 d . . C1' C -0.6505(4) 0.4679(4) -0.1023(2) 0.067(2) Uani 1 d . . C2' C -0.6068(4) 0.4077(5) -0.1324(2) 0.081(2) Uani 1 d . . H2' H -0.6061(4) 0.3517(5) -0.1268(2) 0.097 Uiso 1 calc R . C3' C -0.5633(4) 0.4533(5) -0.1742(3) 0.091(2) Uani 1 d . . H3' H -0.5306(4) 0.4304(5) -0.1997(3) 0.109 Uiso 1 calc R . C4' C -0.5795(4) 0.5341(5) -0.1687(3) 0.090(2) Uani 1 d . . H4' H -0.5580(4) 0.5750(5) -0.1897(3) 0.108 Uiso 1 calc R . C5' C -0.6342(3) 0.5476(4) -0.1261(2) 0.067(2) Uani 1 d . . H5' H -0.6552(3) 0.5975(4) -0.1157(2) 0.080 Uiso 1 calc R . C6' C -0.4118(4) 0.4724(4) -0.0863(2) 0.071(2) Uani 1 d . . C7' C -0.4291(4) 0.5569(4) -0.0833(3) 0.071(2) Uani 1 d . . H7' H -0.4081(4) 0.5976(4) -0.1046(3) 0.085 Uiso 1 calc R . C8' C -0.4843(4) 0.5675(4) -0.0418(2) 0.071(2) Uani 1 d . . H8' H -0.5060(4) 0.6172(4) -0.0317(2) 0.086 Uiso 1 calc R . C9' C -0.5010(4) 0.4938(4) -0.0189(2) 0.070(2) Uani 1 d . . H9' H -0.5349(4) 0.4842(4) 0.0093(2) 0.084 Uiso 1 calc R . C10' C -0.4558(4) 0.4352(5) -0.0471(3) 0.079(2) Uani 1 d . . H10' H -0.4558(4) 0.3796(5) -0.0402(3) 0.095 Uiso 1 calc R . C11' C -0.7262(5) 0.4361(5) 0.1273(2) 0.085(2) Uani 1 d . . C12' C -0.7518(4) 0.4464(4) 0.0723(2) 0.074(2) Uani 1 d . . C13' C -0.8244(5) 0.4889(5) 0.0626(3) 0.088(2) Uani 1 d . . H13' H -0.8430(5) 0.4923(5) 0.0278(3) 0.105 Uiso 1 calc R . C14' C -0.8715(5) 0.5277(5) 0.1038(3) 0.104(2) Uani 1 d . . C15' C -0.8421(5) 0.5147(5) 0.1565(3) 0.112(2) Uani 1 d . . H15' H -0.8720(5) 0.5338(5) 0.1847(3) 0.134 Uiso 1 calc R . C16' C -0.7730(5) 0.4762(6) 0.1669(3) 0.106(3) Uani 1 d . . H16' H -0.7543(5) 0.4754(6) 0.2017(3) 0.127 Uiso 1 calc R . C17' C -0.6687(4) 0.3826(5) 0.1346(3) 0.084(2) Uani 1 d . . H17' H -0.6522(4) 0.3709(5) 0.1691(3) 0.101 Uiso 1 calc R . C18' C -0.5696(4) 0.2896(4) 0.1053(3) 0.087(2) Uani 1 d . . H18C H -0.5784(4) 0.2419(4) 0.0833(3) 0.104 Uiso 1 calc R . H18D H -0.5685(4) 0.2719(4) 0.1420(3) 0.104 Uiso 1 calc R . C19' C -0.4897(5) 0.3275(6) 0.0919(3) 0.101(3) Uani 1 d . . H19' H -0.4940(5) 0.3430(6) 0.0545(3) 0.121 Uiso 1 calc R . C20' C -0.4213(6) 0.2660(7) 0.0950(5) 0.162(5) Uani 1 d . . H20C H -0.4116(6) 0.2468(7) 0.0594(5) 0.195 Uiso 1 calc R . H20D H -0.4399(6) 0.2196(7) 0.1153(5) 0.195 Uiso 1 calc R . C21' C -0.3394(7) 0.2932(9) 0.1194(6) 0.279(5) Uani 1 d . . H21C H -0.2989(7) 0.2928(9) 0.0922(6) 0.335 Uiso 1 calc R . H21D H -0.3232(7) 0.2554(9) 0.1470(6) 0.335 Uiso 1 calc R . C22' C -0.3474(5) 0.3832(7) 0.1436(3) 0.120(3) Uani 1 d . . H22' H -0.2993(5) 0.4064(7) 0.1602(3) 0.144 Uiso 1 calc R . C23' C -0.3878(5) 0.4328(7) 0.1034(4) 0.130(3) Uani 1 d . . H23C H -0.3751(5) 0.4170(7) 0.0674(4) 0.156 Uiso 1 calc R . H23D H -0.3800(5) 0.4908(7) 0.1084(4) 0.156 Uiso 1 calc R . C24' C -0.4668(4) 0.4037(5) 0.1206(3) 0.093(3) Uani 1 d . . H24' H -0.5086(4) 0.4453(5) 0.1229(3) 0.112 Uiso 1 calc R . C25' C -0.4197(7) 0.3847(10) 0.1742(4) 0.161(5) Uani 1 d . . C26' C -0.4515(12) 0.3218(16) 0.2077(6) 0.379(12) Uani 1 d . . H26D H -0.5005(12) 0.3404(16) 0.2230(6) 0.569 Uiso 1 calc R . H26E H -0.4136(12) 0.3095(16) 0.2354(6) 0.569 Uiso 1 calc R . H26F H -0.4617(12) 0.2738(16) 0.1870(6) 0.569 Uiso 1 calc R . C27' C -0.4186(8) 0.4724(10) 0.2070(5) 0.283(5) Uani 1 d . . H27D H -0.3975(8) 0.5144(10) 0.1848(5) 0.424 Uiso 1 calc R . H27E H -0.3857(8) 0.4671(10) 0.2382(5) 0.424 Uiso 1 calc R . H27F H -0.4721(8) 0.4864(10) 0.2170(5) 0.424 Uiso 1 calc R . C28' C -0.9951(10) 0.6051(18) 0.1165(7) 0.296(14) Uani 1 d . . H28D H -1.0365(10) 0.6255(18) 0.0934(7) 0.445 Uiso 1 calc R . H28E H -0.9702(10) 0.6497(18) 0.1349(7) 0.445 Uiso 1 calc R . H28F H -1.0179(10) 0.5682(18) 0.1416(7) 0.445 Uiso 1 calc R . C29' C -0.2556(4) 0.6639(5) -0.2115(3) 0.090(2) Uani 1 d . . C30' C -0.2738(4) 0.6012(4) -0.1716(3) 0.076(2) Uani 1 d . . C31' C -0.2478(4) 0.6194(5) -0.1198(3) 0.088(2) Uani 1 d . . H31' H -0.2571(4) 0.5822(5) -0.0928(3) 0.105 Uiso 1 calc R . C32' C -0.2078(5) 0.6935(4) -0.1079(3) 0.092(2) Uani 1 d . . C33' C -0.1897(4) 0.7513(5) -0.1465(4) 0.100(3) Uani 1 d . . H33' H -0.1622(4) 0.7989(5) -0.1379(4) 0.120 Uiso 1 calc R . C34' C -0.2141(4) 0.7353(6) -0.1983(3) 0.100(3) Uani 1 d . . H34' H -0.2027(4) 0.7728(6) -0.2247(3) 0.120 Uiso 1 calc R . C35' C -0.2796(4) 0.6466(5) -0.2646(3) 0.086(2) Uani 1 d . . H35' H -0.2742(4) 0.6853(5) -0.2912(3) 0.103 Uiso 1 calc R . C36' C -0.3382(5) 0.5596(6) -0.3267(3) 0.102(3) Uani 1 d . . H36C H -0.3255(5) 0.5036(6) -0.3355(3) 0.122 Uiso 1 calc R . H36D H -0.3109(5) 0.5945(6) -0.3516(3) 0.122 Uiso 1 calc R . C37' C -0.4293(4) 0.5724(5) -0.3331(3) 0.085(2) Uani 1 d . . H37' H -0.4520(4) 0.5390(5) -0.3049(3) 0.102 Uiso 1 calc R . C38' C -0.4611(5) 0.5336(6) -0.3831(4) 0.123(4) Uani 1 d . . H38C H -0.4810(5) 0.4799(6) -0.3742(4) 0.147 Uiso 1 calc R . H38D H -0.4167(5) 0.5261(6) -0.4070(4) 0.147 Uiso 1 calc R . C39' C -0.5282(7) 0.5795(8) -0.4135(5) 0.156(5) Uani 1 d . . H39C H -0.5117(7) 0.5890(8) -0.4497(5) 0.187 Uiso 1 calc R . H39D H -0.5762(7) 0.5463(8) -0.4145(5) 0.187 Uiso 1 calc R . C40' C -0.5463(6) 0.6617(6) -0.3866(4) 0.114(3) Uani 1 d . . H40' H -0.5880(6) 0.6954(6) -0.4031(4) 0.137 Uiso 1 calc R . C41' C -0.5555(5) 0.6427(8) -0.3253(4) 0.134(4) Uani 1 d . . H41C H -0.5748(5) 0.5884(8) -0.3174(4) 0.160 Uiso 1 calc R . H41D H -0.5844(5) 0.6839(8) -0.3057(4) 0.160 Uiso 1 calc R . C42' C -0.4603(5) 0.6523(6) -0.3230(4) 0.106(3) Uani 1 d . . H42' H -0.4385(5) 0.6798(6) -0.2915(4) 0.127 Uiso 1 calc R . C43' C -0.4659(5) 0.7041(5) -0.3734(4) 0.106(3) Uani 1 d . . C44' C -0.4816(10) 0.7937(7) -0.3627(7) 0.203(7) Uani 1 d . . H44D H -0.5207(10) 0.7989(7) -0.3354(7) 0.304 Uiso 1 calc R . H44E H -0.5013(10) 0.8193(7) -0.3945(7) 0.304 Uiso 1 calc R . H44F H -0.4328(10) 0.8197(7) -0.3516(7) 0.304 Uiso 1 calc R . C45' C -0.4055(7) 0.7010(7) -0.4153(5) 0.164(5) Uani 1 d . . H45D H -0.3934(7) 0.6453(7) -0.4233(5) 0.246 Uiso 1 calc R . H45E H -0.3578(7) 0.7283(7) -0.4034(5) 0.246 Uiso 1 calc R . H45F H -0.4260(7) 0.7276(7) -0.4465(5) 0.246 Uiso 1 calc R . C46' C -0.1990(7) 0.6559(6) -0.0134(3) 0.131(4) Uani 1 d . . H46D H -0.1795(7) 0.6767(6) 0.0199(3) 0.197 Uiso 1 calc R . H46E H -0.1728(7) 0.6054(6) -0.0212(3) 0.197 Uiso 1 calc R . H46F H -0.2556(7) 0.6470(6) -0.0114(3) 0.197 Uiso 1 calc R . C47' C -0.7599(4) 0.5534(4) -0.0427(2) 0.076(2) Uani 1 d . . C48' C -0.8338(5) 0.5780(5) -0.0649(3) 0.097(3) Uani 1 d . . H48' H -0.8630(5) 0.5414(5) -0.0855(3) 0.116 Uiso 1 calc R . C49' C -0.8639(7) 0.6565(7) -0.0566(4) 0.192(4) Uani 1 d . . H49' H -0.9126(7) 0.6721(7) -0.0716(4) 0.230 Uiso 1 calc R . C50' C -0.8221(8) 0.7079(6) -0.0272(4) 0.155(5) Uani 1 d . . H50' H -0.8414(8) 0.7603(6) -0.0219(4) 0.186 Uiso 1 calc R . C51' C -0.7486(8) 0.6850(6) -0.0034(3) 0.141(4) Uani 1 d . . H51' H -0.7210(8) 0.7215(6) 0.0182(3) 0.170 Uiso 1 calc R . C52' C -0.7179(5) 0.6081(4) -0.0124(3) 0.094(2) Uani 1 d . . H52' H -0.6686(5) 0.5935(4) 0.0022(3) 0.112 Uiso 1 calc R . C53' C -0.8054(4) 0.3962(4) -0.0852(2) 0.074(2) Uani 1 d . . C54' C -0.8198(5) 0.4015(5) -0.1411(2) 0.093(2) Uani 1 d . . H54' H -0.7862(5) 0.4312(5) -0.1630(2) 0.112 Uiso 1 calc R . C55' C -0.8834(4) 0.3620(5) -0.1605(3) 0.091(2) Uani 1 d . . H55' H -0.8934(4) 0.3662(5) -0.1967(3) 0.109 Uiso 1 calc R . C56' C -0.9325(5) 0.3182(6) -0.1330(3) 0.101(3) Uani 1 d . . H56' H -0.9758(5) 0.2920(6) -0.1490(3) 0.121 Uiso 1 calc R . C57' C -0.9182(4) 0.3119(5) -0.0791(3) 0.087(2) Uani 1 d . . H57' H -0.9529(4) 0.2812(5) -0.0586(3) 0.104 Uiso 1 calc R . C58' C -0.8536(4) 0.3501(4) -0.0546(2) 0.067(2) Uani 1 d . . H58' H -0.8438(4) 0.3442(4) -0.0185(2) 0.080 Uiso 1 calc R . C59' C -0.3517(4) 0.3221(4) -0.1311(3) 0.085(2) Uani 1 d . . C60' C -0.4275(6) 0.2899(6) -0.1337(5) 0.131(4) Uani 1 d . . H60' H -0.4711(6) 0.3251(6) -0.1332(5) 0.158 Uiso 1 calc R . C61' C -0.4413(7) 0.2060(6) -0.1371(5) 0.156(4) Uani 1 d . . H61' H -0.4936(7) 0.1874(6) -0.1400(5) 0.188 Uiso 1 calc R . C62' C -0.3820(7) 0.1521(6) -0.1364(4) 0.143(4) Uani 1 d . . H62' H -0.3917(7) 0.0963(6) -0.1383(4) 0.171 Uiso 1 calc R . C63' C -0.3079(8) 0.1818(5) -0.1327(3) 0.145(4) Uani 1 d . . H63' H -0.2649(8) 0.1458(5) -0.1314(3) 0.174 Uiso 1 calc R . C64' C -0.2926(6) 0.2685(6) -0.1306(3) 0.112(3) Uani 1 d . . H64' H -0.2401(6) 0.2870(6) -0.1289(3) 0.135 Uiso 1 calc R . C65' C -0.2448(4) 0.4339(5) -0.0875(3) 0.094(2) Uani 1 d . . C66' C -0.1677(5) 0.4413(6) -0.1080(4) 0.121(3) Uani 1 d . . H66' H -0.1633(5) 0.4501(6) -0.1443(4) 0.146 Uiso 1 calc R . C67' C -0.1019(5) 0.4367(6) -0.0803(5) 0.140(4) Uani 1 d . . H67' H -0.0531(5) 0.4330(6) -0.0974(5) 0.168 Uiso 1 calc R . C68' C -0.1039(6) 0.4375(7) -0.0234(5) 0.140(4) Uani 1 d . . H68' H -0.0573(6) 0.4406(7) -0.0029(5) 0.168 Uiso 1 calc R . C69' C -0.1787(6) 0.4334(6) -0.0006(4) 0.113(3) Uani 1 d . . H69' H -0.1825(6) 0.4321(6) 0.0361(4) 0.135 Uiso 1 calc R . C70' C -0.2477(5) 0.4311(5) -0.0311(3) 0.091(2) Uani 1 d . . H70' H -0.2970(5) 0.4277(5) -0.0146(3) 0.109 Uiso 1 calc R . C71 C 0.2555(9) 0.1849(8) 0.8648(5) 0.188(5) Uani 1 d . . Cl1 Cl 0.2080(3) 0.0898(3) 0.8774(2) 0.184(2) Uani 1 d . . Cl2 Cl 0.3136(3) 0.1828(3) 0.8127(2) 0.219(2) Uani 1 d . . C72 C -0.2307(14) 0.7221(18) -0.5858(12) 0.508(13) Uani 1 d . . Cl3 Cl -0.2972(5) 0.7329(5) -0.5328(3) 0.333(4) Uani 1 d . . Cl4 Cl -0.1800(5) 0.6323(4) -0.5828(4) 0.403(4) 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 Pd1 0.0747(2) 0.0706(2) 0.0514(2) 0.0036(2) 0.0050(2) -0.0076(2) Pd2 0.0676(2) 0.0606(2) 0.0493(2) 0.0039(2) 0.0070(2) 0.0036(2) Fe1 0.0759(4) 0.0678(4) 0.0500(4) 0.0007(4) 0.0118(3) -0.0022(4) Br1 0.1086(5) 0.0786(4) 0.0805(4) -0.0115(4) 0.0081(4) -0.0108(4) Br2 0.0764(3) 0.0687(3) 0.0825(4) 0.0024(3) 0.0084(3) 0.0075(3) P1 0.0695(8) 0.0637(8) 0.0505(7) 0.0022(7) 0.0043(6) -0.0016(7) P2 0.0650(8) 0.0670(8) 0.0505(7) -0.0011(6) 0.0041(6) -0.0021(7) O1 0.138(4) 0.133(4) 0.059(2) -0.021(3) 0.022(3) -0.025(4) O2 0.116(4) 0.101(4) 0.104(4) 0.012(3) 0.006(3) 0.020(3) N1 0.100(4) 0.089(4) 0.060(3) 0.024(3) 0.002(3) -0.011(3) N2 0.071(3) 0.098(4) 0.045(2) 0.009(2) 0.012(2) 0.003(3) C1 0.086(4) 0.072(3) 0.056(3) -0.016(3) 0.014(3) -0.022(3) C2 0.079(4) 0.116(5) 0.053(3) -0.003(3) 0.015(3) -0.020(4) C3 0.088(4) 0.110(5) 0.049(3) 0.006(3) 0.008(3) -0.032(4) C4 0.065(3) 0.126(6) 0.061(3) -0.009(4) 0.014(3) -0.018(4) C5 0.068(3) 0.098(5) 0.072(3) -0.006(4) 0.004(3) -0.001(4) C6 0.088(4) 0.067(3) 0.054(3) 0.007(3) 0.009(3) -0.003(3) C7 0.106(4) 0.056(3) 0.056(3) -0.009(3) 0.001(3) -0.002(3) C8 0.078(4) 0.074(4) 0.078(4) -0.006(3) 0.014(3) 0.007(3) C9 0.081(4) 0.083(4) 0.070(3) 0.010(3) 0.023(3) 0.006(3) C10 0.050(3) 0.101(5) 0.075(4) -0.004(4) 0.002(3) -0.006(3) C11 0.072(3) 0.080(4) 0.059(3) 0.003(3) 0.002(3) 0.007(3) C12 0.067(3) 0.076(4) 0.050(3) 0.016(3) 0.003(2) 0.008(3) C13 0.091(4) 0.072(4) 0.044(3) 0.003(3) 0.010(3) 0.001(3) C14 0.113(5) 0.075(4) 0.051(3) -0.005(3) 0.009(3) -0.008(4) C15 0.109(5) 0.079(4) 0.059(3) 0.002(3) 0.028(3) 0.000(4) C16 0.087(4) 0.117(5) 0.078(3) 0.033(4) 0.035(3) 0.029(4) C17 0.078(3) 0.082(4) 0.067(3) 0.030(3) -0.018(3) -0.012(3) C18 0.075(4) 0.079(4) 0.094(4) 0.013(4) 0.014(3) -0.018(3) C19 0.067(3) 0.106(5) 0.051(3) -0.003(3) -0.006(3) -0.008(3) C20 0.115(5) 0.076(4) 0.078(4) -0.006(3) 0.021(4) -0.015(4) C21 0.121(6) 0.088(5) 0.134(7) 0.005(5) -0.026(5) -0.002(5) C22 0.124(6) 0.147(7) 0.100(5) 0.043(5) -0.034(4) 0.005(6) C23 0.128(6) 0.163(9) 0.068(4) -0.009(5) 0.013(4) -0.001(7) C24 0.093(5) 0.105(5) 0.078(4) -0.013(4) 0.003(4) 0.004(4) C25 0.103(5) 0.090(4) 0.068(4) -0.023(3) -0.006(4) -0.006(4) C26 0.108(5) 0.088(5) 0.116(6) -0.003(5) 0.009(5) -0.028(4) C27 0.122(7) 0.154(8) 0.172(8) -0.072(7) -0.023(6) 0.002(7) C28 0.146(7) 0.199(9) 0.075(4) -0.031(6) 0.021(5) -0.074(6) C29 0.106(4) 0.094(4) 0.041(3) -0.013(3) 0.009(3) -0.019(4) C30 0.069(3) 0.084(4) 0.050(3) -0.003(3) 0.023(2) -0.003(3) C31 0.103(4) 0.068(4) 0.059(3) 0.005(3) 0.006(3) 0.002(4) C32 0.087(4) 0.083(4) 0.059(3) 0.009(3) 0.007(3) 0.016(3) C33 0.140(6) 0.062(3) 0.058(3) 0.003(3) -0.009(4) 0.008(4) C34 0.111(5) 0.055(3) 0.082(4) 0.009(3) -0.002(4) 0.010(3) C35 0.070(3) 0.080(4) 0.066(3) -0.007(3) 0.014(3) -0.011(3) C36 0.067(3) 0.083(4) 0.069(3) 0.000(3) 0.023(3) -0.002(3) C37 0.069(3) 0.088(4) 0.074(4) 0.016(3) 0.007(3) -0.001(3) C38 0.096(5) 0.096(5) 0.085(4) -0.023(4) -0.002(4) -0.001(4) C39 0.122(6) 0.242(10) 0.116(6) -0.067(6) -0.004(5) 0.080(6) C40 0.089(5) 0.144(7) 0.100(5) -0.023(5) -0.008(4) -0.031(5) C41 0.073(4) 0.178(9) 0.094(5) -0.013(6) -0.001(4) 0.019(6) C42 0.089(4) 0.094(4) 0.069(3) 0.004(4) 0.000(3) 0.007(4) C43 0.091(5) 0.161(9) 0.106(6) -0.015(6) 0.000(5) 0.011(6) C44 0.084(5) 0.253(13) 0.157(8) -0.073(9) -0.024(5) 0.052(7) C45 0.128(6) 0.102(6) 0.118(6) 0.006(5) 0.021(5) -0.025(5) C46 0.119(6) 0.114(6) 0.144(8) 0.029(6) 0.006(6) 0.046(5) C47 0.085(3) 0.047(3) 0.056(3) -0.002(3) 0.000(3) 0.003(3) C48 0.066(4) 0.094(5) 0.111(5) 0.024(4) -0.001(4) 0.000(4) C49 0.101(5) 0.095(5) 0.117(6) 0.010(5) -0.014(5) -0.003(5) C50 0.122(5) 0.068(4) 0.113(6) 0.002(4) -0.024(5) 0.032(4) C51 0.155(6) 0.119(5) 0.061(4) 0.007(4) -0.003(4) 0.070(4) C52 0.096(4) 0.092(5) 0.083(4) -0.012(4) -0.003(4) 0.017(4) C53 0.077(3) 0.061(3) 0.051(3) 0.006(3) 0.010(3) 0.005(3) C54 0.075(4) 0.071(4) 0.087(4) -0.008(3) 0.016(3) -0.007(3) C55 0.074(4) 0.112(6) 0.106(5) -0.030(5) 0.005(4) -0.010(4) C56 0.117(5) 0.071(4) 0.098(4) -0.033(4) 0.016(4) 0.007(4) C57 0.110(5) 0.049(3) 0.118(5) 0.005(4) 0.022(4) 0.004(3) C58 0.075(4) 0.101(5) 0.057(3) 0.000(3) 0.008(3) 0.010(4) C59 0.076(3) 0.078(4) 0.054(3) 0.010(3) 0.002(3) -0.005(3) C60 0.070(4) 0.073(4) 0.097(5) -0.001(4) 0.001(3) 0.004(3) C61 0.066(4) 0.086(5) 0.133(6) 0.020(5) -0.012(4) 0.001(3) C62 0.125(6) 0.117(7) 0.128(6) 0.016(6) -0.049(5) 0.011(6) C63 0.126(6) 0.173(10) 0.104(6) 0.010(7) -0.042(5) 0.006(7) C64 0.099(5) 0.118(6) 0.081(4) 0.001(4) -0.003(4) 0.002(5) C65 0.068(3) 0.087(4) 0.058(3) -0.002(3) 0.006(3) 0.001(3) C66 0.097(4) 0.063(3) 0.054(3) -0.013(3) 0.000(3) -0.003(3) C67 0.108(5) 0.064(4) 0.139(6) -0.037(4) -0.002(5) 0.016(4) C68 0.085(4) 0.074(4) 0.103(5) 0.004(4) 0.007(4) -0.005(4) C69 0.145(7) 0.067(4) 0.080(4) 0.008(4) -0.011(5) 0.000(4) C70 0.108(5) 0.052(3) 0.092(4) 0.002(3) -0.029(4) -0.002(3) Pd1' 0.0787(3) 0.0686(2) 0.0547(2) 0.0014(2) 0.0058(2) -0.0036(2) Pd2' 0.0854(3) 0.0839(3) 0.0716(2) 0.0198(2) 0.0265(2) 0.0235(2) Fe1' 0.0804(5) 0.0641(4) 0.0574(4) 0.0020(4) 0.0170(4) 0.0015(4) Br1' 0.1063(5) 0.0736(4) 0.0898(4) -0.0054(4) 0.0167(4) 0.0026(4) Br2' 0.1575(7) 0.0912(5) 0.0832(4) 0.0002(4) 0.0112(5) 0.0238(5) P1' 0.0759(8) 0.0638(8) 0.0510(7) -0.0054(7) 0.0096(6) -0.0013(7) P2' 0.0850(9) 0.0752(9) 0.0707(8) 0.0203(8) 0.0259(7) 0.0184(8) N1' 0.094(3) 0.068(3) 0.079(3) 0.008(3) 0.005(3) -0.007(3) N2' 0.078(3) 0.121(5) 0.079(3) 0.013(3) 0.029(3) 0.036(3) O1' 0.141(4) 0.125(4) 0.166(5) -0.023(4) 0.075(3) 0.039(4) O2' 0.170(5) 0.075(3) 0.112(4) 0.022(3) 0.012(4) 0.004(4) C1' 0.081(3) 0.062(3) 0.060(3) 0.002(3) 0.029(3) -0.008(3) C2' 0.095(4) 0.078(4) 0.070(3) -0.004(3) 0.002(3) 0.009(4) C3' 0.106(4) 0.094(5) 0.074(3) -0.024(3) 0.041(3) -0.014(4) C4' 0.102(5) 0.102(5) 0.066(3) 0.032(3) 0.011(3) 0.002(4) C5' 0.066(3) 0.083(4) 0.051(3) 0.008(3) -0.003(3) 0.006(3) C6' 0.078(3) 0.069(3) 0.066(3) 0.014(3) 0.019(3) 0.012(3) C7' 0.075(4) 0.063(3) 0.075(4) 0.011(3) 0.003(3) 0.002(3) C8' 0.067(3) 0.075(4) 0.072(3) 0.006(3) 0.013(3) 0.022(3) C9' 0.072(3) 0.078(4) 0.059(3) 0.012(3) 0.009(3) 0.008(3) C10' 0.081(4) 0.074(4) 0.081(4) 0.005(4) 0.008(3) -0.013(3) C11' 0.114(5) 0.083(4) 0.059(3) 0.000(3) 0.004(3) -0.024(4) C12' 0.103(4) 0.077(4) 0.043(2) 0.007(3) 0.009(3) -0.010(4) C13' 0.116(5) 0.079(4) 0.069(3) 0.011(3) 0.026(3) -0.003(4) C14' 0.132(5) 0.084(4) 0.099(4) -0.020(4) 0.061(4) -0.029(4) C15' 0.148(5) 0.101(5) 0.089(3) -0.040(4) 0.071(3) -0.038(5) C16' 0.116(5) 0.135(7) 0.066(3) -0.029(4) 0.033(4) -0.034(5) C17' 0.092(4) 0.085(4) 0.077(4) 0.025(4) 0.000(3) -0.003(4) C18' 0.109(5) 0.058(3) 0.094(5) 0.013(3) -0.006(4) -0.020(3) C19' 0.103(5) 0.112(6) 0.087(4) -0.023(4) -0.016(4) 0.025(5) C20' 0.117(7) 0.141(7) 0.228(11) -0.086(7) -0.027(7) 0.035(6) C21' 0.226(8) 0.198(9) 0.407(12) -0.191(8) -0.216(8) 0.093(8) C22' 0.092(5) 0.159(8) 0.108(5) -0.029(6) -0.029(4) -0.002(6) C23' 0.126(6) 0.145(7) 0.120(6) 0.029(6) 0.012(5) -0.055(6) C24' 0.084(4) 0.091(5) 0.106(5) -0.007(4) 0.016(4) 0.014(4) C25' 0.151(8) 0.236(13) 0.096(6) -0.033(8) 0.015(6) -0.063(9) C26' 0.406(18) 0.602(32) 0.127(10) 0.074(16) -0.074(12) -0.330(18) C27' 0.174(9) 0.408(12) 0.268(8) -0.272(7) 0.073(8) -0.116(9) C28' 0.218(15) 0.453(36) 0.219(17) -0.064(22) 0.025(14) 0.091(21) C29' 0.071(3) 0.105(5) 0.094(4) 0.031(4) 0.036(3) 0.009(4) C30' 0.068(3) 0.071(3) 0.090(4) 0.012(3) 0.032(3) 0.024(3) C31' 0.105(5) 0.083(4) 0.076(4) 0.018(3) 0.030(3) 0.018(4) C32' 0.104(5) 0.051(3) 0.122(6) 0.009(4) 0.019(4) 0.007(3) C33' 0.080(4) 0.076(4) 0.144(7) -0.006(5) 0.024(4) 0.004(4) C34' 0.086(4) 0.116(6) 0.100(5) 0.014(5) 0.027(4) 0.007(4) C35' 0.100(4) 0.085(4) 0.073(4) 0.023(3) 0.018(3) 0.002(4) C36' 0.113(5) 0.128(6) 0.065(3) 0.033(4) 0.028(3) 0.040(4) C37' 0.097(5) 0.081(4) 0.078(4) 0.022(3) 0.009(4) 0.004(4) C38' 0.115(6) 0.095(6) 0.157(8) 0.016(6) -0.023(6) -0.006(5) C39' 0.166(10) 0.135(9) 0.166(10) 0.012(9) -0.029(8) -0.003(8) C40' 0.113(6) 0.093(5) 0.135(7) 0.027(5) -0.012(5) 0.014(5) C41' 0.086(5) 0.194(10) 0.120(6) -0.003(7) -0.028(5) 0.047(6) C42' 0.084(4) 0.132(7) 0.102(5) 0.014(5) 0.012(4) 0.024(5) C43' 0.099(5) 0.086(5) 0.134(6) 0.022(5) 0.026(5) 0.015(4) C44' 0.291(17) 0.071(6) 0.244(15) -0.015(9) -0.053(13) 0.023(9) C45' 0.176(10) 0.126(7) 0.188(9) 0.070(7) -0.037(8) 0.001(8) C46' 0.209(10) 0.108(6) 0.076(5) 0.013(5) -0.017(6) -0.009(7) C47' 0.125(5) 0.058(3) 0.046(3) -0.007(2) 0.020(3) 0.011(3) C48' 0.141(6) 0.076(4) 0.073(4) -0.012(4) 0.001(4) 0.020(4) C49' 0.291(9) 0.186(6) 0.099(6) -0.032(5) -0.028(7) 0.176(5) C50' 0.276(13) 0.090(6) 0.097(6) -0.013(5) -0.025(8) 0.048(7) C51' 0.269(12) 0.074(5) 0.082(5) -0.007(4) 0.036(7) -0.013(7) C52' 0.138(5) 0.060(3) 0.084(4) 0.012(3) 0.042(4) 0.012(4) C53' 0.081(3) 0.078(4) 0.062(3) -0.004(3) 0.024(3) 0.008(3) C54' 0.144(6) 0.085(4) 0.050(3) -0.001(3) 0.007(4) -0.023(4) C55' 0.101(5) 0.110(5) 0.061(3) -0.019(4) -0.003(3) -0.014(4) C56' 0.104(5) 0.099(5) 0.099(5) 0.009(5) -0.019(4) 0.004(5) C57' 0.088(4) 0.096(5) 0.076(4) 0.010(4) 0.001(3) 0.014(4) C58' 0.076(4) 0.067(3) 0.056(3) 0.011(3) 0.000(3) 0.006(3) C59' 0.115(4) 0.066(3) 0.074(3) 0.014(3) 0.029(3) 0.048(3) C60' 0.128(7) 0.073(5) 0.194(10) 0.003(6) 0.041(7) -0.008(5) C61' 0.207(9) 0.060(4) 0.205(9) -0.021(5) 0.096(7) -0.004(5) C62' 0.227(10) 0.088(5) 0.111(6) 0.000(5) -0.045(7) 0.051(6) C63' 0.258(10) 0.091(5) 0.085(5) -0.034(4) -0.036(6) 0.076(6) C64' 0.134(6) 0.134(7) 0.068(4) -0.017(5) 0.021(4) 0.022(6) C65' 0.096(4) 0.094(4) 0.092(4) 0.042(4) 0.032(3) 0.007(4) C66' 0.098(5) 0.109(6) 0.158(7) 0.042(6) 0.048(5) 0.035(4) C67' 0.093(5) 0.114(5) 0.213(9) 0.084(6) 0.026(6) 0.028(5) C68' 0.112(6) 0.126(7) 0.183(9) 0.066(7) -0.010(6) -0.002(6) C69' 0.153(7) 0.092(5) 0.093(5) 0.010(5) -0.010(5) 0.002(6) C70' 0.101(5) 0.086(4) 0.086(4) 0.028(4) 0.007(4) 0.012(4) C71 0.229(11) 0.137(7) 0.199(9) -0.091(6) 0.085(8) -0.016(9) Cl1 0.204(3) 0.158(3) 0.191(3) -0.047(2) 0.032(3) -0.027(3) Cl2 0.306(4) 0.182(3) 0.172(3) 0.019(3) 0.102(3) 0.055(3) C72 0.568(18) 0.388(23) 0.577(30) 0.117(23) 0.381(17) 0.319(16) Cl3 0.410(7) 0.266(6) 0.326(7) -0.093(6) 0.113(6) -0.143(5) Cl4 0.541(9) 0.157(4) 0.517(9) 0.062(5) 0.293(7) 0.015(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 C12 2.044(6) . ? Pd1 N1 2.082(6) . ? Pd1 P1 2.269(2) . ? Pd1 Br1 2.5287(10) . ? Pd2 C30 2.050(7) . ? Pd2 N2 2.114(5) . ? Pd2 P2 2.266(2) . ? Pd2 Br2 2.5402(9) . ? Fe1 C2 1.996(7) . ? Fe1 C1 2.027(6) . ? Fe1 C5 2.029(7) . ? Fe1 C4 2.032(7) . ? Fe1 C10 2.032(6) . ? Fe1 C6 2.035(6) . ? Fe1 C3 2.042(7) . ? Fe1 C7 2.051(6) . ? Fe1 C9 2.062(7) . ? Fe1 C8 2.085(7) . ? P1 C53 1.801(6) . ? P1 C1 1.815(6) . ? P1 C47 1.834(6) . ? P2 C65 1.798(7) . ? P2 C6 1.799(6) . ? P2 C59 1.831(6) . ? O1 C14 1.376(9) . ? O1 C28 1.390(11) . ? O2 C32 1.386(9) . ? O2 C46 1.425(11) . ? N1 C17 1.329(8) . ? N1 C18 1.466(9) . ? N2 C35 1.286(9) . ? N2 C36 1.459(8) . ? C1 C5 1.420(10) . ? C1 C2 1.429(10) . ? C2 C3 1.431(9) . ? C3 C4 1.367(11) . ? C4 C5 1.423(9) . ? C6 C10 1.433(9) . ? C6 C7 1.448(9) . ? C7 C8 1.407(9) . ? C8 C9 1.371(10) . ? C9 C10 1.410(10) . ? C11 C12 1.365(8) . ? C11 C16 1.417(9) . ? C11 C17 1.429(9) . ? C12 C13 1.413(8) . ? C13 C14 1.402(8) . ? C14 C15 1.361(10) . ? C15 C16 1.443(10) . ? C18 C19 1.580(9) . ? C19 C24 1.491(10) . ? C19 C20 1.542(11) . ? C20 C21 1.530(12) . ? C21 C22 1.578(14) . ? C22 C23 1.461(13) . ? C22 C25 1.508(13) . ? C23 C24 1.583(12) . ? C24 C25 1.593(11) . ? C25 C27 1.498(14) . ? C25 C26 1.531(11) . ? C29 C35 1.362(10) . ? C29 C30 1.419(9) . ? C29 C34 1.423(10) . ? C30 C31 1.408(9) . ? C31 C32 1.398(10) . ? C32 C33 1.333(10) . ? C33 C34 1.341(11) . ? C36 C37 1.544(9) . ? C37 C38 1.503(11) . ? C37 C42 1.524(10) . ? C38 C39 1.525(12) . ? C39 C40 1.580(15) . ? C40 C41 1.42(2) . ? C40 C43 1.532(13) . ? C41 C42 1.571(10) . ? C42 C43 1.606(13) . ? C43 C45 1.527(14) . ? C43 C44 1.558(15) . ? C47 C48 1.328(9) . ? C47 C52 1.398(9) . ? C48 C49 1.387(11) . ? C49 C50 1.373(12) . ? C50 C51 1.308(12) . ? C51 C52 1.365(11) . ? C53 C58 1.421(9) . ? C53 C54 1.424(9) . ? C54 C55 1.427(11) . ? C55 C56 1.342(11) . ? C56 C57 1.352(11) . ? C57 C58 1.393(10) . ? C59 C64 1.384(10) . ? C59 C60 1.389(9) . ? C60 C61 1.440(10) . ? C61 C62 1.309(13) . ? C62 C63 1.469(14) . ? C63 C64 1.410(12) . ? C65 C70 1.383(9) . ? C65 C66 1.423(9) . ? C66 C67 1.402(10) . ? C67 C68 1.319(12) . ? C68 C69 1.322(11) . ? C69 C70 1.378(10) . ? Pd1' C12' 1.972(6) . ? Pd1' N1' 2.106(6) . ? Pd1' P1' 2.282(2) . ? Pd1' Br1' 2.5470(10) . ? Pd2' C30' 2.003(7) . ? Pd2' N2' 2.148(6) . ? Pd2' P2' 2.273(2) . ? Pd2' Br2' 2.5375(12) . ? Fe1' C10' 2.025(7) . ? Fe1' C1' 2.030(6) . ? Fe1' C2' 2.043(7) . ? Fe1' C6' 2.045(6) . ? Fe1' C8' 2.054(7) . ? Fe1' C7' 2.055(6) . ? Fe1' C4' 2.057(7) . ? Fe1' C5' 2.065(6) . ? Fe1' C3' 2.070(7) . ? Fe1' C9' 2.072(6) . ? P1' C1' 1.804(6) . ? P1' C47' 1.806(7) . ? P1' C53' 1.840(7) . ? P2' C65' 1.798(7) . ? P2' C59' 1.821(7) . ? P2' C6' 1.822(6) . ? N1' C17' 1.250(9) . ? N1' C18' 1.457(9) . ? N2' C35' 1.267(10) . ? N2' C36' 1.436(9) . ? O1' C28' 1.34(2) . ? O1' C14' 1.369(10) . ? O2' C32' 1.431(11) . ? O2' C46' 1.466(11) . ? C1' C2' 1.451(9) . ? C1' C5' 1.467(9) . ? C2' C3' 1.491(10) . ? C3' C4' 1.360(11) . ? C4' C5' 1.438(9) . ? C6' C10' 1.383(9) . ? C6' C7' 1.418(9) . ? C7' C8' 1.415(9) . ? C8' C9' 1.372(9) . ? C9' C10' 1.420(9) . ? C11' C17' 1.314(11) . ? C11' C16' 1.438(10) . ? C11' C12' 1.457(8) . ? C12' C13' 1.419(10) . ? C13' C14' 1.459(10) . ? C14' C15' 1.429(10) . ? C15' C16' 1.340(12) . ? C18' C19' 1.517(11) . ? C19' C24' 1.493(12) . ? C19' C20' 1.527(13) . ? C20' C21' 1.56(2) . ? C21' C22' 1.60(2) . ? C22' C25' 1.444(14) . ? C22' C23' 1.461(14) . ? C23' C24' 1.477(11) . ? C24' C25' 1.589(13) . ? C25' C26' 1.44(3) . ? C25' C27' 1.66(2) . ? C29' C34' 1.400(12) . ? C29' C35' 1.422(10) . ? C29' C30' 1.475(10) . ? C30' C31' 1.405(10) . ? C31' C32' 1.418(11) . ? C32' C33' 1.397(12) . ? C33' C34' 1.390(12) . ? C36' C37' 1.545(11) . ? C37' C42' 1.434(12) . ? C37' C38' 1.504(12) . ? C38' C39' 1.55(2) . ? C39' C40' 1.54(2) . ? C40' C43' 1.548(13) . ? C40' C41' 1.588(14) . ? C41' C42' 1.601(11) . ? C42' C43' 1.533(13) . ? C43' C45' 1.473(15) . ? C43' C44' 1.519(14) . ? C47' C52' 1.368(10) . ? C47' C48' 1.409(11) . ? C48' C49' 1.400(13) . ? C49' C50' 1.32(2) . ? C50' C51' 1.41(2) . ? C51' C52' 1.383(12) . ? C53' C58' 1.355(9) . ? C53' C54' 1.432(9) . ? C54' C55' 1.334(11) . ? C55' C56' 1.299(11) . ? C56' C57' 1.384(11) . ? C57' C58' 1.387(10) . ? C59' C64' 1.323(12) . ? C59' C60' 1.374(12) . ? C60' C61' 1.399(13) . ? C61' C62' 1.33(2) . ? C62' C63' 1.33(2) . ? C63' C64' 1.447(14) . ? C65' C66' 1.402(11) . ? C65' C70' 1.425(10) . ? C66' C67' 1.300(13) . ? C67' C68' 1.44(2) . ? C68' C69' 1.385(14) . ? C69' C70' 1.382(12) . ? C71 Cl2 1.646(14) . ? C71 Cl1 1.783(14) . ? C72 Cl4 1.70(3) . ? C72 Cl3 1.76(3) . ? 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 C12 Pd1 N1 80.1(2) . . ? C12 Pd1 P1 96.9(2) . . ? N1 Pd1 P1 171.4(2) . . ? C12 Pd1 Br1 163.3(2) . . ? N1 Pd1 Br1 91.5(2) . . ? P1 Pd1 Br1 93.33(5) . . ? C30 Pd2 N2 79.5(2) . . ? C30 Pd2 P2 96.8(2) . . ? N2 Pd2 P2 171.36(15) . . ? C30 Pd2 Br2 167.8(2) . . ? N2 Pd2 Br2 92.8(2) . . ? P2 Pd2 Br2 92.08(5) . . ? C2 Fe1 C1 41.6(3) . . ? C2 Fe1 C5 69.1(3) . . ? C1 Fe1 C5 41.0(3) . . ? C2 Fe1 C4 68.5(3) . . ? C1 Fe1 C4 69.1(2) . . ? C5 Fe1 C4 41.0(3) . . ? C2 Fe1 C10 157.9(3) . . ? C1 Fe1 C10 123.9(3) . . ? C5 Fe1 C10 111.3(3) . . ? C4 Fe1 C10 127.3(3) . . ? C2 Fe1 C6 156.9(3) . . ? C1 Fe1 C6 160.8(3) . . ? C5 Fe1 C6 125.0(3) . . ? C4 Fe1 C6 108.9(3) . . ? C10 Fe1 C6 41.3(2) . . ? C2 Fe1 C3 41.5(2) . . ? C1 Fe1 C3 69.4(2) . . ? C5 Fe1 C3 67.9(3) . . ? C4 Fe1 C3 39.2(3) . . ? C10 Fe1 C3 160.5(3) . . ? C6 Fe1 C3 121.9(2) . . ? C2 Fe1 C7 119.2(3) . . ? C1 Fe1 C7 155.8(3) . . ? C5 Fe1 C7 161.0(3) . . ? C4 Fe1 C7 123.1(3) . . ? C10 Fe1 C7 68.0(3) . . ? C6 Fe1 C7 41.5(3) . . ? C3 Fe1 C7 106.0(3) . . ? C2 Fe1 C9 120.3(3) . . ? C1 Fe1 C9 107.1(3) . . ? C5 Fe1 C9 125.5(3) . . ? C4 Fe1 C9 163.2(3) . . ? C10 Fe1 C9 40.3(3) . . ? C6 Fe1 C9 69.0(3) . . ? C3 Fe1 C9 156.3(3) . . ? C7 Fe1 C9 67.1(3) . . ? C2 Fe1 C8 105.0(3) . . ? C1 Fe1 C8 121.2(3) . . ? C5 Fe1 C8 158.8(3) . . ? C4 Fe1 C8 157.5(3) . . ? C10 Fe1 C8 66.2(3) . . ? C6 Fe1 C8 68.2(3) . . ? C3 Fe1 C8 121.9(3) . . ? C7 Fe1 C8 39.8(3) . . ? C9 Fe1 C8 38.6(3) . . ? C53 P1 C1 99.2(3) . . ? C53 P1 C47 104.9(3) . . ? C1 P1 C47 103.2(3) . . ? C53 P1 Pd1 114.3(2) . . ? C1 P1 Pd1 120.1(2) . . ? C47 P1 Pd1 113.1(2) . . ? C65 P2 C6 106.8(3) . . ? C65 P2 C59 102.0(3) . . ? C6 P2 C59 104.7(3) . . ? C65 P2 Pd2 115.4(2) . . ? C6 P2 Pd2 110.7(2) . . ? C59 P2 Pd2 116.2(2) . . ? C14 O1 C28 117.1(6) . . ? C32 O2 C46 118.5(6) . . ? C17 N1 C18 116.2(6) . . ? C17 N1 Pd1 113.1(4) . . ? C18 N1 Pd1 129.9(4) . . ? C35 N2 C36 119.7(6) . . ? C35 N2 Pd2 113.0(4) . . ? C36 N2 Pd2 127.1(4) . . ? C5 C1 C2 106.4(5) . . ? C5 C1 P1 128.6(5) . . ? C2 C1 P1 124.7(5) . . ? C5 C1 Fe1 69.6(4) . . ? C2 C1 Fe1 68.0(3) . . ? P1 C1 Fe1 131.9(3) . . ? C3 C2 C1 108.1(7) . . ? C3 C2 Fe1 71.0(4) . . ? C1 C2 Fe1 70.4(4) . . ? C4 C3 C2 108.1(6) . . ? C4 C3 Fe1 70.0(4) . . ? C2 C3 Fe1 67.5(4) . . ? C3 C4 C5 109.2(6) . . ? C3 C4 Fe1 70.8(4) . . ? C5 C4 Fe1 69.4(4) . . ? C1 C5 C4 108.1(7) . . ? C1 C5 Fe1 69.4(4) . . ? C4 C5 Fe1 69.6(4) . . ? C10 C6 C7 104.8(5) . . ? C10 C6 P2 132.6(5) . . ? C7 C6 P2 122.0(4) . . ? C10 C6 Fe1 69.3(3) . . ? C7 C6 Fe1 69.8(3) . . ? P2 C6 Fe1 131.4(4) . . ? C8 C7 C6 107.9(6) . . ? C8 C7 Fe1 71.4(4) . . ? C6 C7 Fe1 68.6(3) . . ? C9 C8 C7 109.9(6) . . ? C9 C8 Fe1 69.8(4) . . ? C7 C8 Fe1 68.8(4) . . ? C8 C9 C10 107.8(6) . . ? C8 C9 Fe1 71.6(4) . . ? C10 C9 Fe1 68.7(3) . . ? C9 C10 C6 109.5(6) . . ? C9 C10 Fe1 71.0(4) . . ? C6 C10 Fe1 69.5(3) . . ? C12 C11 C16 123.4(6) . . ? C12 C11 C17 117.6(6) . . ? C16 C11 C17 118.9(6) . . ? C11 C12 C13 116.5(5) . . ? C11 C12 Pd1 112.5(4) . . ? C13 C12 Pd1 130.5(4) . . ? C14 C13 C12 122.0(6) . . ? C15 C14 O1 114.6(6) . . ? C15 C14 C13 121.2(6) . . ? O1 C14 C13 124.1(7) . . ? C14 C15 C16 118.5(6) . . ? C11 C16 C15 118.3(6) . . ? N1 C17 C11 116.5(6) . . ? N1 C18 C19 111.2(6) . . ? C24 C19 C20 114.5(6) . . ? C24 C19 C18 111.1(6) . . ? C20 C19 C18 110.9(5) . . ? C21 C20 C19 115.8(6) . . ? C20 C21 C22 111.3(7) . . ? C23 C22 C25 91.0(8) . . ? C23 C22 C21 108.6(8) . . ? C25 C22 C21 108.7(7) . . ? C22 C23 C24 88.5(6) . . ? C19 C24 C23 103.1(7) . . ? C19 C24 C25 113.3(6) . . ? C23 C24 C25 83.6(6) . . ? C27 C25 C22 112.2(7) . . ? C27 C25 C26 108.0(7) . . ? C22 C25 C26 123.5(7) . . ? C27 C25 C24 108.0(7) . . ? C22 C25 C24 86.5(6) . . ? C26 C25 C24 116.6(6) . . ? C35 C29 C30 119.0(7) . . ? C35 C29 C34 123.4(7) . . ? C30 C29 C34 117.6(6) . . ? C31 C30 C29 119.6(6) . . ? C31 C30 Pd2 130.6(5) . . ? C29 C30 Pd2 109.8(4) . . ? C32 C31 C30 118.4(6) . . ? C33 C32 O2 116.7(7) . . ? C33 C32 C31 121.4(7) . . ? O2 C32 C31 121.9(6) . . ? C32 C33 C34 122.2(7) . . ? C33 C34 C29 120.6(7) . . ? N2 C35 C29 118.4(6) . . ? N2 C36 C37 109.7(5) . . ? C38 C37 C42 110.4(6) . . ? C38 C37 C36 112.4(6) . . ? C42 C37 C36 113.5(5) . . ? C37 C38 C39 118.0(8) . . ? C38 C39 C40 110.6(9) . . ? C41 C40 C43 91.5(8) . . ? C41 C40 C39 112.0(8) . . ? C43 C40 C39 108.3(8) . . ? C40 C41 C42 87.7(7) . . ? C37 C42 C41 108.2(6) . . ? C37 C42 C43 115.5(7) . . ? C41 C42 C43 83.6(6) . . ? C45 C43 C40 125.6(10) . . ? C45 C43 C44 110.5(8) . . ? C40 C43 C44 111.0(8) . . ? C45 C43 C42 116.9(7) . . ? C40 C43 C42 82.9(6) . . ? C44 C43 C42 105.9(9) . . ? C48 C47 C52 117.4(6) . . ? C48 C47 P1 124.1(5) . . ? C52 C47 P1 118.5(5) . . ? C47 C48 C49 122.4(7) . . ? C50 C49 C48 117.4(8) . . ? C51 C50 C49 121.1(8) . . ? C50 C51 C52 120.9(7) . . ? C51 C52 C47 120.0(7) . . ? C58 C53 C54 118.8(6) . . ? C58 C53 P1 117.7(5) . . ? C54 C53 P1 123.4(5) . . ? C53 C54 C55 119.1(6) . . ? C56 C55 C54 119.0(7) . . ? C55 C56 C57 123.4(7) . . ? C56 C57 C58 120.7(7) . . ? C57 C58 C53 118.9(6) . . ? C64 C59 C60 118.9(6) . . ? C64 C59 P2 119.6(5) . . ? C60 C59 P2 121.5(5) . . ? C59 C60 C61 121.8(7) . . ? C62 C61 C60 118.6(7) . . ? C61 C62 C63 122.1(8) . . ? C64 C63 C62 117.2(8) . . ? C59 C64 C63 120.9(8) . . ? C70 C65 C66 115.0(6) . . ? C70 C65 P2 125.6(5) . . ? C66 C65 P2 119.4(5) . . ? C67 C66 C65 120.7(6) . . ? C68 C67 C66 119.2(8) . . ? C67 C68 C69 122.9(8) . . ? C68 C69 C70 119.6(8) . . ? C69 C70 C65 122.3(7) . . ? C12' Pd1' N1' 79.8(2) . . ? C12' Pd1' P1' 96.0(2) . . ? N1' Pd1' P1' 168.5(2) . . ? C12' Pd1' Br1' 164.5(2) . . ? N1' Pd1' Br1' 93.3(2) . . ? P1' Pd1' Br1' 93.32(5) . . ? C30' Pd2' N2' 80.3(3) . . ? C30' Pd2' P2' 95.2(2) . . ? N2' Pd2' P2' 175.3(2) . . ? C30' Pd2' Br2' 172.3(2) . . ? N2' Pd2' Br2' 93.0(2) . . ? P2' Pd2' Br2' 91.59(6) . . ? C10' Fe1' C1' 123.2(3) . . ? C10' Fe1' C2' 109.9(3) . . ? C1' Fe1' C2' 41.7(3) . . ? C10' Fe1' C6' 39.7(2) . . ? C1' Fe1' C6' 159.4(3) . . ? C2' Fe1' C6' 124.1(3) . . ? C10' Fe1' C8' 66.2(3) . . ? C1' Fe1' C8' 120.9(2) . . ? C2' Fe1' C8' 158.4(3) . . ? C6' Fe1' C8' 67.6(2) . . ? C10' Fe1' C7' 66.7(3) . . ? C1' Fe1' C7' 157.2(3) . . ? C2' Fe1' C7' 160.0(3) . . ? C6' Fe1' C7' 40.5(3) . . ? C8' Fe1' C7' 40.3(2) . . ? C10' Fe1' C4' 160.5(3) . . ? C1' Fe1' C4' 69.7(3) . . ? C2' Fe1' C4' 68.8(3) . . ? C6' Fe1' C4' 123.7(3) . . ? C8' Fe1' C4' 122.4(3) . . ? C7' Fe1' C4' 107.5(3) . . ? C10' Fe1' C5' 158.4(2) . . ? C1' Fe1' C5' 42.0(2) . . ? C2' Fe1' C5' 69.7(3) . . ? C6' Fe1' C5' 158.2(3) . . ? C8' Fe1' C5' 105.8(3) . . ? C7' Fe1' C5' 121.1(3) . . ? C4' Fe1' C5' 40.8(3) . . ? C10' Fe1' C3' 127.4(3) . . ? C1' Fe1' C3' 70.1(3) . . ? C2' Fe1' C3' 42.5(3) . . ? C6' Fe1' C3' 109.7(3) . . ? C8' Fe1' C3' 156.9(3) . . ? C7' Fe1' C3' 122.5(3) . . ? C4' Fe1' C3' 38.5(3) . . ? C5' Fe1' C3' 67.8(3) . . ? C10' Fe1' C9' 40.5(3) . . ? C1' Fe1' C9' 106.0(2) . . ? C2' Fe1' C9' 124.2(3) . . ? C6' Fe1' C9' 68.0(2) . . ? C8' Fe1' C9' 38.8(3) . . ? C7' Fe1' C9' 67.1(3) . . ? C4' Fe1' C9' 156.6(3) . . ? C5' Fe1' C9' 120.7(2) . . ? C3' Fe1' C9' 163.6(3) . . ? C1' P1' C47' 100.0(3) . . ? C1' P1' C53' 104.7(3) . . ? C47' P1' C53' 105.1(3) . . ? C1' P1' Pd1' 118.0(2) . . ? C47' P1' Pd1' 116.0(2) . . ? C53' P1' Pd1' 111.5(2) . . ? C65' P2' C59' 100.4(3) . . ? C65' P2' C6' 104.6(3) . . ? C59' P2' C6' 105.5(3) . . ? C65' P2' Pd2' 113.3(2) . . ? C59' P2' Pd2' 118.9(2) . . ? C6' P2' Pd2' 112.6(2) . . ? C17' N1' C18' 122.8(6) . . ? C17' N1' Pd1' 110.9(5) . . ? C18' N1' Pd1' 126.2(5) . . ? C35' N2' C36' 118.9(7) . . ? C35' N2' Pd2' 113.9(5) . . ? C36' N2' Pd2' 126.7(6) . . ? C28' O1' C14' 129.9(10) . . ? C32' O2' C46' 116.8(6) . . ? C2' C1' C5' 107.2(5) . . ? C2' C1' P1' 128.1(5) . . ? C5' C1' P1' 124.2(4) . . ? C2' C1' Fe1' 69.6(4) . . ? C5' C1' Fe1' 70.3(3) . . ? P1' C1' Fe1' 132.0(3) . . ? C1' C2' C3' 106.4(6) . . ? C1' C2' Fe1' 68.6(4) . . ? C3' C2' Fe1' 69.7(4) . . ? C4' C3' C2' 108.6(6) . . ? C4' C3' Fe1' 70.3(4) . . ? C2' C3' Fe1' 67.8(4) . . ? C3' C4' C5' 110.9(6) . . ? C3' C4' Fe1' 71.3(4) . . ? C5' C4' Fe1' 69.9(3) . . ? C4' C5' C1' 107.0(6) . . ? C4' C5' Fe1' 69.3(4) . . ? C1' C5' Fe1' 67.8(3) . . ? C10' C6' C7' 106.4(6) . . ? C10' C6' P2' 130.2(5) . . ? C7' C6' P2' 122.7(5) . . ? C10' C6' Fe1' 69.4(4) . . ? C7' C6' Fe1' 70.1(4) . . ? P2' C6' Fe1' 132.4(3) . . ? C8' C7' C6' 107.2(6) . . ? C8' C7' Fe1' 69.8(4) . . ? C6' C7' Fe1' 69.4(4) . . ? C9' C8' C7' 109.9(6) . . ? C9' C8' Fe1' 71.3(4) . . ? C7' C8' Fe1' 69.9(4) . . ? C8' C9' C10' 105.9(5) . . ? C8' C9' Fe1' 69.9(4) . . ? C10' C9' Fe1' 68.0(4) . . ? C6' C10' C9' 110.5(6) . . ? C6' C10' Fe1' 70.9(4) . . ? C9' C10' Fe1' 71.5(4) . . ? C17' C11' C16' 127.7(7) . . ? C17' C11' C12' 114.7(6) . . ? C16' C11' C12' 117.0(7) . . ? C13' C12' C11' 117.5(6) . . ? C13' C12' Pd1' 130.6(4) . . ? C11' C12' Pd1' 111.4(5) . . ? C12' C13' C14' 124.1(6) . . ? O1' C14' C15' 128.4(7) . . ? O1' C14' C13' 116.8(7) . . ? C15' C14' C13' 114.5(7) . . ? C16' C15' C14' 122.7(7) . . ? C15' C16' C11' 123.7(7) . . ? N1' C17' C11' 122.9(7) . . ? N1' C18' C19' 111.7(6) . . ? C24' C19' C18' 117.2(7) . . ? C24' C19' C20' 110.0(7) . . ? C18' C19' C20' 112.2(8) . . ? C19' C20' C21' 119.0(10) . . ? C20' C21' C22' 109.7(9) . . ? C25' C22' C23' 88.8(8) . . ? C25' C22' C21' 107.1(11) . . ? C23' C22' C21' 106.7(9) . . ? C22' C23' C24' 91.3(7) . . ? C23' C24' C19' 110.6(7) . . ? C23' C24' C25' 83.0(7) . . ? C19' C24' C25' 111.8(8) . . ? C26' C25' C22' 128.3(15) . . ? C26' C25' C24' 117.2(11) . . ? C22' C25' C24' 87.6(7) . . ? C26' C25' C27' 109.3(12) . . ? C22' C25' C27' 106.2(11) . . ? C24' C25' C27' 104.8(11) . . ? C34' C29' C35' 121.7(7) . . ? C34' C29' C30' 121.8(7) . . ? C35' C29' C30' 116.5(7) . . ? C31' C30' C29' 115.0(6) . . ? C31' C30' Pd2' 133.2(5) . . ? C29' C30' Pd2' 111.4(5) . . ? C30' C31' C32' 121.3(7) . . ? C33' C32' C31' 122.8(8) . . ? C33' C32' O2' 114.4(7) . . ? C31' C32' O2' 122.8(7) . . ? C34' C33' C32' 117.6(8) . . ? C33' C34' C29' 121.5(8) . . ? N2' C35' C29' 117.7(7) . . ? N2' C36' C37' 113.6(6) . . ? C42' C37' C38' 114.3(7) . . ? C42' C37' C36' 117.6(7) . . ? C38' C37' C36' 111.7(6) . . ? C37' C38' C39' 117.2(9) . . ? C40' C39' C38' 110.6(9) . . ? C39' C40' C43' 108.3(8) . . ? C39' C40' C41' 106.3(9) . . ? C43' C40' C41' 88.4(7) . . ? C40' C41' C42' 84.7(6) . . ? C37' C42' C43' 112.2(7) . . ? C37' C42' C41' 105.4(8) . . ? C43' C42' C41' 88.5(7) . . ? C45' C43' C44' 106.4(10) . . ? C45' C43' C42' 122.9(8) . . ? C44' C43' C42' 113.6(9) . . ? C45' C43' C40' 115.6(9) . . ? C44' C43' C40' 108.8(9) . . ? C42' C43' C40' 88.5(7) . . ? C52' C47' C48' 118.5(6) . . ? C52' C47' P1' 120.5(6) . . ? C48' C47' P1' 121.0(5) . . ? C49' C48' C47' 121.3(8) . . ? C50' C49' C48' 118.8(10) . . ? C49' C50' C51' 121.5(10) . . ? C52' C51' C50' 119.7(9) . . ? C47' C52' C51' 120.1(8) . . ? C58' C53' C54' 120.1(6) . . ? C58' C53' P1' 117.0(5) . . ? C54' C53' P1' 122.9(5) . . ? C55' C54' C53' 117.2(7) . . ? C56' C55' C54' 125.4(7) . . ? C55' C56' C57' 117.6(8) . . ? C56' C57' C58' 122.0(7) . . ? C53' C58' C57' 117.6(6) . . ? C64' C59' C60' 115.7(8) . . ? C64' C59' P2' 122.1(6) . . ? C60' C59' P2' 122.2(6) . . ? C59' C60' C61' 122.1(9) . . ? C62' C61' C60' 122.2(11) . . ? C61' C62' C63' 116.7(10) . . ? C62' C63' C64' 121.7(10) . . ? C59' C64' C63' 121.5(9) . . ? C66' C65' C70' 114.5(7) . . ? C66' C65' P2' 123.3(6) . . ? C70' C65' P2' 122.2(5) . . ? C67' C66' C65' 124.9(10) . . ? C66' C67' C68' 120.6(9) . . ? C69' C68' C67' 116.5(9) . . ? C70' C69' C68' 121.5(9) . . ? C69' C70' C65' 121.3(7) . . ? Cl2 C71 Cl1 113.1(7) . . ? Cl4 C72 Cl3 111.9(17) . . ? _refine_diff_density_max 0.846 _refine_diff_density_min -0.647 _refine_diff_density_rms 0.096