data_7557 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H30 Br2 N4 Pd2 S2' _chemical_formula_weight 907.34 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' 'S' 'S' 0.1246 0.1234 '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 Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) 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 9.6224(3) _cell_length_b 15.5833(5) _cell_length_c 21.3048(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3194.63(18) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 6448 _cell_measurement_theta_min 2.32 _cell_measurement_theta_max 24.31 _exptl_crystal_description BLOCK _exptl_crystal_colour YELLOW _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.887 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1776 _exptl_absorpt_coefficient_mu 3.787 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.3126 _exptl_absorpt_correction_T_max 0.7032 _exptl_absorpt_process_details 'Sadabs, (Sheldrick 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22411 _diffrn_reflns_av_R_equivalents 0.0377 _diffrn_reflns_av_sigmaI/netI 0.0528 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.62 _diffrn_reflns_theta_max 27.50 _reflns_number_total 7216 _reflns_number_gt 6513 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0200P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.018(7) _refine_ls_number_reflns 7216 _refine_ls_number_parameters 404 _refine_ls_number_restraints 72 _refine_ls_R_factor_all 0.0376 _refine_ls_R_factor_gt 0.0322 _refine_ls_wR_factor_ref 0.0636 _refine_ls_wR_factor_gt 0.0621 _refine_ls_goodness_of_fit_ref 1.000 _refine_ls_restrained_S_all 0.999 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.72698(3) 0.67921(2) 0.421622(13) 0.02239(7) Uani 1 1 d . . . Pd2 Pd 0.70400(3) 0.81229(2) 0.315393(13) 0.02241(7) Uani 1 1 d . . . Br1 Br 0.57599(5) 0.55362(3) 0.42687(2) 0.03714(11) Uani 1 1 d . . . Br2 Br 0.60381(5) 0.95607(3) 0.33220(2) 0.03428(11) Uani 1 1 d . . . S1 S 0.83710(10) 0.80873(7) 0.40908(5) 0.0263(2) Uani 1 1 d . . . S2 S 0.77735(10) 0.67226(6) 0.31283(5) 0.0261(2) Uani 1 1 d . . . N1 N 0.7415(3) 0.6474(2) 0.56259(14) 0.0266(8) Uani 1 1 d . . . N2 N 0.6660(4) 0.7741(2) 0.53776(15) 0.0262(8) Uani 1 1 d . . . N3 N 0.5211(3) 0.7293(2) 0.22364(14) 0.0239(7) Uani 1 1 d . . . N4 N 0.6035(3) 0.8447(2) 0.18151(15) 0.0266(8) Uani 1 1 d . A . C1 C 0.7086(4) 0.6987(3) 0.51294(18) 0.0248(9) Uani 1 1 d . . . C2 C 0.7217(4) 0.6923(3) 0.61878(18) 0.0291(9) Uani 1 1 d . . . C3 C 0.7373(4) 0.6669(3) 0.68123(19) 0.0371(11) Uani 1 1 d . . . H3 H 0.7700 0.6121 0.6923 0.044 Uiso 1 1 calc R . . C4 C 0.7013(5) 0.7279(3) 0.7262(2) 0.0421(12) Uani 1 1 d . . . H4 H 0.7115 0.7143 0.7689 0.050 Uiso 1 1 calc R . . C5 C 0.6510(5) 0.8080(3) 0.7097(2) 0.0413(12) Uani 1 1 d . . . H5 H 0.6256 0.8463 0.7417 0.050 Uiso 1 1 calc R . . C6 C 0.6365(4) 0.8339(3) 0.6480(2) 0.0340(11) Uani 1 1 d . . . H6 H 0.6049 0.8890 0.6370 0.041 Uiso 1 1 calc R . . C7 C 0.6723(4) 0.7723(3) 0.60300(19) 0.0275(9) Uani 1 1 d . . . C8 C 0.7989(4) 0.5608(3) 0.55801(18) 0.0294(9) Uani 1 1 d . . . H8A H 0.8892 0.5599 0.5793 0.035 Uiso 1 1 calc R . . H8B H 0.8153 0.5477 0.5136 0.035 Uiso 1 1 calc R . . C9 C 0.7087(4) 0.4911(3) 0.58560(17) 0.0262(9) Uani 1 1 d . . . C10 C 0.7673(5) 0.4117(3) 0.59722(18) 0.0310(10) Uani 1 1 d . . . H10 H 0.8623 0.4030 0.5890 0.037 Uiso 1 1 calc R . . C11 C 0.6892(5) 0.3450(3) 0.6207(2) 0.0350(11) Uani 1 1 d . . . H11 H 0.7305 0.2912 0.6275 0.042 Uiso 1 1 calc R . . C12 C 0.5506(5) 0.3570(3) 0.6341(2) 0.0408(12) Uani 1 1 d . . . H12 H 0.4968 0.3117 0.6502 0.049 Uiso 1 1 calc R . . C13 C 0.4921(5) 0.4359(3) 0.6237(2) 0.0504(14) Uani 1 1 d . . . H13 H 0.3976 0.4446 0.6328 0.060 Uiso 1 1 calc R . . C14 C 0.5704(5) 0.5028(3) 0.6001(2) 0.0426(12) Uani 1 1 d . . . H14 H 0.5290 0.5567 0.5939 0.051 Uiso 1 1 calc R . . C15 C 0.6350(4) 0.8490(3) 0.4991(2) 0.0321(10) Uani 1 1 d . . . H15A H 0.5955 0.8945 0.5255 0.038 Uiso 1 1 calc R . . H15B H 0.5658 0.8337 0.4673 0.038 Uiso 1 1 calc R . . C16 C 0.7657(5) 0.8819(3) 0.46714(18) 0.0323(10) Uani 1 1 d . . . H16A H 0.8365 0.8929 0.4992 0.039 Uiso 1 1 calc R . . H16B H 0.7445 0.9367 0.4466 0.039 Uiso 1 1 calc R . . C17 C 0.6031(4) 0.7967(3) 0.23430(17) 0.0247(9) Uani 1 1 d . . . C18 C 0.4635(4) 0.7335(3) 0.16314(19) 0.0272(9) Uani 1 1 d . . . C19 C 0.3688(4) 0.6819(3) 0.13258(19) 0.0334(9) Uani 1 1 d . . . H19 H 0.3319 0.6324 0.1515 0.040 Uiso 1 1 calc R . . C20 C 0.3308(5) 0.7066(3) 0.0726(2) 0.0419(12) Uani 1 1 d U . . H20 H 0.2648 0.6740 0.0505 0.050 Uiso 1 1 calc R . . C21 C 0.3886(5) 0.7790(3) 0.0442(2) 0.0439(13) Uani 1 1 d . . . H21 H 0.3633 0.7928 0.0029 0.053 Uiso 1 1 calc R . . C22 C 0.4825(5) 0.8309(3) 0.0758(2) 0.0355(10) Uani 1 1 d . . . H22 H 0.5210 0.8799 0.0568 0.043 Uiso 1 1 calc R . . C23 C 0.5172(4) 0.8074(3) 0.13658(18) 0.0257(9) Uani 1 1 d . . . C24 C 0.6758(5) 0.9266(3) 0.1727(2) 0.0318(10) Uani 1 1 d . . . H24A H 0.6696 0.9593 0.2118 0.038 Uiso 0.667(13) 1 calc PR A 1 H24B H 0.6266 0.9593 0.1403 0.038 Uiso 0.667(13) 1 calc PR A 1 H24C H 0.6919 0.9525 0.2134 0.038 Uiso 0.333(13) 1 d PR A 2 H24D H 0.6154 0.9647 0.1492 0.038 Uiso 0.333(13) 1 d PR A 2 C31 C 0.5061(4) 0.6571(3) 0.26696(19) 0.0268(9) Uani 1 1 d . . . H31A H 0.4347 0.6177 0.2512 0.032 Uiso 1 1 calc R . . H31B H 0.4762 0.6782 0.3081 0.032 Uiso 1 1 calc R . . C32 C 0.6428(4) 0.6095(3) 0.27366(18) 0.0269(9) Uani 1 1 d . . . H32A H 0.6760 0.5931 0.2318 0.032 Uiso 1 1 calc R . . H32B H 0.6269 0.5567 0.2975 0.032 Uiso 1 1 calc R . . C25 C 0.8263(4) 0.9204(3) 0.1542(3) 0.032(2) Uani 0.667(13) 1 d PGU A 1 C26 C 0.9294(6) 0.9425(5) 0.1969(3) 0.056(3) Uani 0.667(13) 1 d PGU A 1 H26A H 0.9053 0.9581 0.2381 0.068 Uiso 0.667(13) 1 calc PR A 1 C27 C 1.0681(5) 0.9414(5) 0.1788(4) 0.068(3) Uani 0.667(13) 1 d PGU A 1 H27A H 1.1379 0.9563 0.2077 0.082 Uiso 0.667(13) 1 calc PR A 1 C28 C 1.1038(4) 0.9182(4) 0.1178(5) 0.083(4) Uani 0.667(13) 1 d PGU A 1 H28A H 1.1976 0.9175 0.1056 0.100 Uiso 0.667(13) 1 calc PR A 1 C29 C 1.0007(7) 0.8961(4) 0.0751(4) 0.088(4) Uani 0.667(13) 1 d PGU A 1 H29A H 1.0248 0.8805 0.0339 0.105 Uiso 0.667(13) 1 calc PR A 1 C30 C 0.8619(6) 0.8972(4) 0.0933(4) 0.058(3) Uani 0.667(13) 1 d PG A 1 H30A H 0.7922 0.8823 0.0643 0.070 Uiso 0.667(13) 1 calc PR A 1 C25A C 0.8150(4) 0.9196(3) 0.1381(3) 0.034(5) Uani 0.333(13) 1 d PGU A 2 C26A C 0.8245(7) 0.9295(5) 0.0734(3) 0.049(5) Uani 0.333(13) 1 d PGU A 2 H26B H 0.7435 0.9368 0.0493 0.059 Uiso 0.333(13) 1 calc PR A 2 C27A C 0.9537(9) 0.9286(6) 0.0443(3) 0.060(6) Uani 0.333(13) 1 d PGU A 2 H27B H 0.9601 0.9353 0.0005 0.071 Uiso 0.333(13) 1 calc PR A 2 C28A C 1.0735(6) 0.9178(4) 0.0799(5) 0.061(6) Uani 0.333(13) 1 d PGU A 2 H28B H 1.1610 0.9172 0.0602 0.073 Uiso 0.333(13) 1 calc PR A 2 C29A C 1.0641(4) 0.9079(3) 0.1446(5) 0.089(9) Uani 0.333(13) 1 d PGU A 2 H29B H 1.1451 0.9007 0.1686 0.107 Uiso 0.333(13) 1 calc PR A 2 C30A C 0.9348(4) 0.9088(3) 0.1737(4) 0.079(7) Uani 0.333(13) 1 d PGU A 2 H30B H 0.9284 0.9022 0.2174 0.094 Uiso 0.333(13) 1 calc PR A 2 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 0.02311(14) 0.02028(16) 0.02377(15) 0.00132(12) -0.00311(12) -0.00167(13) Pd2 0.02401(14) 0.01967(16) 0.02356(15) 0.00150(12) -0.00141(12) -0.00172(13) Br1 0.0435(3) 0.0321(3) 0.0357(2) -0.0004(2) 0.0007(2) -0.0146(2) Br2 0.0418(2) 0.0262(2) 0.0349(2) 0.00001(18) 0.0028(2) 0.0044(2) S1 0.0242(4) 0.0251(6) 0.0298(5) 0.0025(4) -0.0037(4) -0.0054(4) S2 0.0271(5) 0.0239(5) 0.0274(5) 0.0013(4) -0.0006(4) 0.0012(4) N1 0.0260(18) 0.027(2) 0.0263(18) 0.0019(14) -0.0020(15) -0.0008(15) N2 0.0275(18) 0.025(2) 0.0261(19) -0.0021(15) -0.0016(15) -0.0020(15) N3 0.0269(18) 0.0243(19) 0.0204(18) 0.0023(14) -0.0019(15) -0.0011(15) N4 0.0332(18) 0.0208(19) 0.0260(18) 0.0011(14) 0.0016(16) 0.0033(15) C1 0.0201(18) 0.026(2) 0.029(2) 0.0039(16) -0.0006(17) -0.0047(18) C2 0.0256(19) 0.034(3) 0.027(2) -0.0005(18) -0.0047(17) -0.008(2) C3 0.034(2) 0.045(3) 0.032(2) 0.004(2) -0.003(2) -0.006(2) C4 0.042(3) 0.059(3) 0.026(2) -0.001(2) -0.001(2) -0.012(3) C5 0.038(2) 0.056(3) 0.029(2) -0.016(2) 0.0095(19) -0.006(3) C6 0.028(2) 0.034(3) 0.039(3) -0.0063(19) 0.0037(19) -0.009(2) C7 0.022(2) 0.034(3) 0.027(2) -0.0040(18) 0.0012(18) -0.0054(18) C8 0.028(2) 0.033(3) 0.028(2) 0.0053(17) -0.0020(18) 0.0039(19) C9 0.028(2) 0.029(2) 0.021(2) -0.0006(16) -0.0048(19) -0.0004(18) C10 0.031(2) 0.030(2) 0.032(2) 0.0008(17) -0.0031(19) 0.003(2) C11 0.045(3) 0.027(2) 0.033(2) 0.0052(18) -0.007(2) 0.004(2) C12 0.048(3) 0.037(3) 0.037(3) 0.005(2) 0.005(2) -0.009(2) C13 0.035(3) 0.045(3) 0.072(4) 0.007(3) 0.016(3) -0.003(2) C14 0.035(3) 0.023(3) 0.070(3) 0.009(2) 0.004(2) 0.004(2) C15 0.038(3) 0.026(2) 0.032(2) -0.0023(18) -0.005(2) 0.0032(19) C16 0.044(3) 0.023(2) 0.030(2) -0.0003(17) -0.008(2) -0.006(2) C17 0.0248(19) 0.026(2) 0.023(2) -0.0008(16) 0.0027(17) 0.0041(17) C18 0.028(2) 0.026(2) 0.027(2) 0.0008(18) -0.0002(19) 0.0080(18) C19 0.030(2) 0.034(2) 0.037(2) -0.002(2) -0.0055(18) -0.001(2) C20 0.050(3) 0.042(3) 0.034(2) -0.002(2) -0.013(2) 0.003(2) C21 0.059(3) 0.045(3) 0.028(2) 0.001(2) -0.015(2) 0.006(3) C22 0.051(3) 0.029(3) 0.027(2) 0.0051(19) -0.002(2) 0.005(2) C23 0.025(2) 0.025(2) 0.027(2) -0.0021(18) -0.0034(16) 0.0040(19) C24 0.047(3) 0.019(2) 0.029(2) 0.0034(17) -0.001(2) -0.0009(19) C31 0.027(2) 0.027(2) 0.026(2) 0.0028(17) -0.0006(18) -0.0077(17) C32 0.038(2) 0.023(2) 0.019(2) -0.0021(16) -0.0022(18) 0.0000(19) C25 0.036(5) 0.021(5) 0.040(4) 0.011(3) -0.002(4) -0.004(4) C26 0.053(5) 0.045(6) 0.071(6) 0.011(5) -0.015(5) -0.003(4) C27 0.051(5) 0.044(6) 0.110(8) 0.020(6) -0.022(6) -0.008(4) C28 0.062(7) 0.079(8) 0.110(10) 0.020(7) 0.040(7) 0.002(6) C29 0.072(8) 0.083(9) 0.107(9) -0.013(8) 0.027(7) -0.017(7) C30 0.063(6) 0.063(7) 0.048(6) -0.013(5) 0.011(5) -0.028(5) C25A 0.036(10) 0.029(10) 0.037(9) 0.008(7) -0.009(7) -0.004(8) C26A 0.058(10) 0.041(9) 0.048(9) 0.007(7) 0.016(8) -0.013(8) C27A 0.056(10) 0.043(10) 0.079(12) 0.010(8) 0.022(9) -0.002(8) C28A 0.043(10) 0.048(11) 0.090(14) 0.018(10) 0.013(10) 0.019(8) C29A 0.053(12) 0.116(17) 0.099(16) 0.071(13) 0.011(11) -0.002(11) C30A 0.077(13) 0.081(14) 0.078(13) 0.050(11) 0.010(11) -0.007(11) _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 1.977(4) . ? Pd1 S1 2.2952(11) . ? Pd1 S2 2.3705(10) . ? Pd1 Br1 2.4401(5) . ? Pd1 Pd2 3.0776(4) . ? Pd2 C17 1.997(4) . ? Pd2 S2 2.2941(10) . ? Pd2 S1 2.3721(10) . ? Pd2 Br2 2.4652(5) . ? S1 C16 1.818(4) . ? S2 C32 1.825(4) . ? N1 C1 1.364(5) . ? N1 C2 1.400(5) . ? N1 C8 1.460(5) . ? N2 C1 1.351(5) . ? N2 C7 1.392(5) . ? N2 C15 1.460(5) . ? N3 C17 1.333(5) . ? N3 C18 1.405(5) . ? N3 C31 1.463(5) . ? N4 C17 1.351(5) . ? N4 C23 1.394(5) . ? N4 C24 1.465(5) . ? C2 C7 1.375(6) . ? C2 C3 1.396(5) . ? C3 C4 1.393(6) . ? C4 C5 1.384(7) . ? C5 C6 1.382(6) . ? C6 C7 1.400(6) . ? C8 C9 1.510(6) . ? C9 C14 1.378(6) . ? C9 C10 1.382(6) . ? C10 C11 1.376(6) . ? C11 C12 1.377(6) . ? C12 C13 1.370(7) . ? C13 C14 1.381(6) . ? C15 C16 1.520(6) . ? C18 C19 1.378(6) . ? C18 C23 1.383(6) . ? C19 C20 1.384(6) . ? C20 C21 1.395(7) . ? C21 C22 1.387(6) . ? C22 C23 1.387(6) . ? C24 C25 1.504(5) . ? C24 C25A 1.533(5) . ? C31 C32 1.517(6) . ? C25 C26 1.3900 . ? C25 C30 1.3900 . ? C26 C27 1.3900 . ? C27 C28 1.3900 . ? C28 C29 1.3900 . ? C29 C30 1.3900 . ? C25A C26A 1.3900 . ? C25A C30A 1.3900 . ? C26A C27A 1.3900 . ? C27A C28A 1.3900 . ? C28A C29A 1.3900 . ? C29A C30A 1.3900 . ? 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 S1 91.17(11) . . ? C1 Pd1 S2 170.93(11) . . ? S1 Pd1 S2 80.32(4) . . ? C1 Pd1 Br1 91.44(11) . . ? S1 Pd1 Br1 170.26(3) . . ? S2 Pd1 Br1 97.46(3) . . ? C1 Pd1 Pd2 127.84(11) . . ? S1 Pd1 Pd2 49.83(2) . . ? S2 Pd1 Pd2 47.66(3) . . ? Br1 Pd1 Pd2 122.101(16) . . ? C17 Pd2 S2 90.75(12) . . ? C17 Pd2 S1 171.01(12) . . ? S2 Pd2 S1 80.31(4) . . ? C17 Pd2 Br2 92.65(11) . . ? S2 Pd2 Br2 171.21(3) . . ? S1 Pd2 Br2 96.33(3) . . ? C17 Pd2 Pd1 126.10(12) . . ? S2 Pd2 Pd1 49.79(3) . . ? S1 Pd2 Pd1 47.68(3) . . ? Br2 Pd2 Pd1 122.254(15) . . ? C16 S1 Pd1 107.35(14) . . ? C16 S1 Pd2 110.72(14) . . ? Pd1 S1 Pd2 82.49(3) . . ? C32 S2 Pd2 107.61(13) . . ? C32 S2 Pd1 109.06(13) . . ? Pd2 S2 Pd1 82.55(3) . . ? C1 N1 C2 109.7(3) . . ? C1 N1 C8 125.3(3) . . ? C2 N1 C8 124.8(3) . . ? C1 N2 C7 111.1(3) . . ? C1 N2 C15 122.4(3) . . ? C7 N2 C15 126.0(4) . . ? C17 N3 C18 110.7(3) . . ? C17 N3 C31 123.9(3) . . ? C18 N3 C31 125.1(3) . . ? C17 N4 C23 109.8(3) . . ? C17 N4 C24 126.2(3) . . ? C23 N4 C24 123.9(3) . . ? N2 C1 N1 106.1(3) . . ? N2 C1 Pd1 123.1(3) . . ? N1 C1 Pd1 130.7(3) . . ? C7 C2 C3 121.8(4) . . ? C7 C2 N1 106.9(3) . . ? C3 C2 N1 131.2(4) . . ? C4 C3 C2 115.7(4) . . ? C5 C4 C3 121.9(4) . . ? C6 C5 C4 122.7(4) . . ? C5 C6 C7 115.2(4) . . ? C2 C7 N2 106.1(3) . . ? C2 C7 C6 122.6(4) . . ? N2 C7 C6 131.2(4) . . ? N1 C8 C9 114.9(3) . . ? C14 C9 C10 118.2(4) . . ? C14 C9 C8 123.2(4) . . ? C10 C9 C8 118.7(4) . . ? C11 C10 C9 121.2(4) . . ? C10 C11 C12 120.1(4) . . ? C13 C12 C11 119.1(4) . . ? C12 C13 C14 120.8(5) . . ? C9 C14 C13 120.6(4) . . ? N2 C15 C16 110.7(3) . . ? C15 C16 S1 114.0(3) . . ? N3 C17 N4 107.2(3) . . ? N3 C17 Pd2 122.1(3) . . ? N4 C17 Pd2 130.7(3) . . ? C19 C18 C23 122.7(4) . . ? C19 C18 N3 131.9(4) . . ? C23 C18 N3 105.4(3) . . ? C18 C19 C20 116.6(4) . . ? C19 C20 C21 121.3(4) . . ? C22 C21 C20 121.4(4) . . ? C23 C22 C21 117.1(4) . . ? C18 C23 C22 120.8(4) . . ? C18 C23 N4 106.8(3) . . ? C22 C23 N4 132.4(4) . . ? N4 C24 C25 115.8(4) . . ? N4 C24 C25A 114.6(4) . . ? C25 C24 C25A 13.6 . . ? N3 C31 C32 110.5(3) . . ? C31 C32 S2 113.3(3) . . ? C26 C25 C30 120.0 . . ? C26 C25 C24 120.0(4) . . ? C30 C25 C24 119.9(4) . . ? C27 C26 C25 120.0 . . ? C26 C27 C28 120.0 . . ? C29 C28 C27 120.0 . . ? C28 C29 C30 120.0 . . ? C29 C30 C25 120.0 . . ? C26A C25A C30A 120.0 . . ? C26A C25A C24 121.8(4) . . ? C30A C25A C24 118.1(4) . . ? C25A C26A C27A 120.0 . . ? C28A C27A C26A 120.0 . . ? C29A C28A C27A 120.0 . . ? C30A C29A C28A 120.0 . . ? C29A C30A C25A 120.0 . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.060 _refine_diff_density_min -0.389 _refine_diff_density_rms 0.101 #===END data_8697 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C37 H32 Cl2 F6 N4 O4 Pd2 S2' _chemical_formula_weight 1058.49 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' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 '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 Orthorhombic _symmetry_space_group_name_H-M Pbca 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' '-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 20.9496(7) _cell_length_b 21.0979(7) _cell_length_c 36.6305(13) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 16190.4(10) _cell_formula_units_Z 16 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 7624 _cell_measurement_theta_min 2.16 _cell_measurement_theta_max 26.63 _exptl_crystal_description Block _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas 'Not Measured' _exptl_crystal_density_diffrn 1.737 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 8416 _exptl_absorpt_coefficient_mu 1.196 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.6727 _exptl_absorpt_correction_T_max 0.9317 _exptl_absorpt_process_details 'Sadabs, (Sheldrick 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 124955 _diffrn_reflns_av_R_equivalents 0.0661 _diffrn_reflns_av_sigmaI/netI 0.0426 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -47 _diffrn_reflns_limit_l_max 47 _diffrn_reflns_theta_min 1.11 _diffrn_reflns_theta_max 27.50 _reflns_number_total 18607 _reflns_number_gt 14727 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0445P)^2^+43.7712P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 18607 _refine_ls_number_parameters 1055 _refine_ls_number_restraints 69 _refine_ls_R_factor_all 0.0665 _refine_ls_R_factor_gt 0.0488 _refine_ls_wR_factor_ref 0.1157 _refine_ls_wR_factor_gt 0.1088 _refine_ls_goodness_of_fit_ref 1.081 _refine_ls_restrained_S_all 1.090 _refine_ls_shift/su_max 0.008 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group F4 F 0.0696(3) 0.7220(3) 0.7398(2) 0.068(3) Uani 0.584(14) 1 d PDU A 1 F5 F 0.0716(5) 0.6291(5) 0.7610(2) 0.136(5) Uani 0.584(14) 1 d PDU A 1 F6 F 0.0990(3) 0.6465(4) 0.70643(14) 0.062(2) Uani 0.584(14) 1 d PDU A 1 F4A F 0.0616(4) 0.7013(5) 0.7593(3) 0.075(4) Uani 0.416(14) 1 d PDU A 2 F5A F 0.0980(5) 0.6092(3) 0.7533(2) 0.056(3) Uani 0.416(14) 1 d PDU A 2 F6A F 0.0882(6) 0.6677(5) 0.70681(16) 0.057(3) Uani 0.416(14) 1 d PDU A 2 Pd1 Pd 0.363578(15) 0.814643(15) 0.730415(9) 0.02043(8) Uani 1 1 d . . . Pd2 Pd 0.308325(15) 0.684599(15) 0.743860(9) 0.02039(8) Uani 1 1 d . . . Pd3 Pd 0.696176(16) 0.670590(15) 0.478486(9) 0.02211(8) Uani 1 1 d . . . Pd4 Pd 0.647567(15) 0.536980(15) 0.465822(9) 0.02235(8) Uani 1 1 d . . . S1 S 0.32054(5) 0.74515(5) 0.68979(3) 0.0230(2) Uani 1 1 d . . . S2 S 0.40921(5) 0.72024(5) 0.75315(3) 0.0257(2) Uani 1 1 d . . . S4 S 0.68372(5) 0.60975(5) 0.42473(3) 0.0238(2) Uani 1 1 d . . . S3 S 0.59848(5) 0.62917(5) 0.48970(3) 0.0297(2) Uani 1 1 d . . . O1 O 0.40152(14) 0.87150(14) 0.77142(8) 0.0252(6) Uani 1 1 d . . . O2 O 0.30447(15) 0.88885(16) 0.79594(9) 0.0341(8) Uani 1 1 d . . . O3 O 0.21422(14) 0.65910(15) 0.73331(8) 0.0260(6) Uani 1 1 d . . . O4 O 0.1779(2) 0.7346(2) 0.76994(11) 0.0534(10) Uani 1 1 d . . . O5 O 0.78817(14) 0.69999(14) 0.46513(8) 0.0241(6) Uani 1 1 d . . . O6 O 0.8310(2) 0.6385(2) 0.50826(12) 0.0689(14) Uani 1 1 d . . . O7 O 0.60450(14) 0.47776(14) 0.50368(8) 0.0282(7) Uani 1 1 d . . . O8 O 0.68931(16) 0.46378(17) 0.54059(10) 0.0374(8) Uani 1 1 d . . . N1 N 0.25476(16) 0.88408(16) 0.69923(9) 0.0192(7) Uani 1 1 d . . . N2 N 0.33665(17) 0.94622(17) 0.70021(10) 0.0241(8) Uani 1 1 d . . . N3 N 0.32868(17) 0.66940(17) 0.82311(10) 0.0240(8) Uani 1 1 d . . . N4 N 0.29411(17) 0.58062(17) 0.80009(9) 0.0235(8) Uani 1 1 d . . . N5 N 0.68307(19) 0.68336(17) 0.55837(10) 0.0288(8) Uani 1 1 d . . . N6 N 0.71768(18) 0.77193(17) 0.53552(10) 0.0253(8) Uani 1 1 d . . . N7 N 0.76169(17) 0.47793(16) 0.43292(9) 0.0224(7) Uani 1 1 d . . . N8 N 0.68751(17) 0.40646(16) 0.43656(9) 0.0226(7) Uani 1 1 d . . . F1 F 0.4060(2) 0.99611(17) 0.80403(11) 0.0758(12) Uani 1 1 d . . . F2 F 0.44901(18) 0.9212(2) 0.83262(11) 0.0865(15) Uani 1 1 d . . . F3 F 0.35790(16) 0.95612(18) 0.84882(9) 0.0592(10) Uani 1 1 d . . . F7 F 0.92672(17) 0.73847(17) 0.48699(12) 0.0670(11) Uani 1 1 d . . . F8 F 0.89869(15) 0.70980(17) 0.43341(9) 0.0533(9) Uani 1 1 d . . . F9 F 0.93794(15) 0.64194(15) 0.47028(9) 0.0494(8) Uani 1 1 d . . . F10 F 0.53954(17) 0.43305(17) 0.56346(11) 0.0689(11) Uani 1 1 d . . . F11 F 0.62148(18) 0.3836(2) 0.58087(10) 0.0748(13) Uani 1 1 d . . . F12 F 0.5759(2) 0.35894(16) 0.53128(9) 0.0752(13) Uani 1 1 d . . . C1 C 0.3169(2) 0.8867(2) 0.70788(11) 0.0217(8) Uani 1 1 d . . . C2 C 0.23332(19) 0.94210(19) 0.68558(10) 0.0195(8) Uani 1 1 d . . . C3 C 0.1741(2) 0.9623(2) 0.67353(11) 0.0250(9) Uani 1 1 d . . . H3 H 0.1382 0.9348 0.6730 0.030 Uiso 1 1 calc R . . C4 C 0.1698(2) 1.0253(2) 0.66227(12) 0.0287(10) Uani 1 1 d . . . H4 H 0.1303 1.0410 0.6533 0.034 Uiso 1 1 calc R . . C5 C 0.2230(2) 1.0659(2) 0.66394(12) 0.0305(10) Uani 1 1 d . . . H5 H 0.2181 1.1089 0.6568 0.037 Uiso 1 1 calc R . . C6 C 0.2817(2) 1.0452(2) 0.67562(11) 0.0271(9) Uani 1 1 d . . . H6 H 0.3176 1.0727 0.6764 0.033 Uiso 1 1 calc R . . C7 C 0.2859(2) 0.9825(2) 0.68621(11) 0.0230(9) Uani 1 1 d . . . C8 C 0.4023(2) 0.9693(2) 0.70413(12) 0.0268(9) Uani 1 1 d . . . H8A H 0.4273 0.9374 0.7179 0.032 Uiso 1 1 calc R . . H8B H 0.4018 1.0088 0.7187 0.032 Uiso 1 1 calc R . . C9 C 0.4357(2) 0.9822(2) 0.66812(12) 0.0259(9) Uani 1 1 d . . . C10 C 0.4259(2) 0.9450(2) 0.63749(13) 0.0336(11) Uani 1 1 d . . . H10 H 0.3946 0.9125 0.6380 0.040 Uiso 1 1 calc R . . C11 C 0.4616(2) 0.9547(3) 0.60604(14) 0.0437(13) Uani 1 1 d . . . H11 H 0.4549 0.9286 0.5853 0.052 Uiso 1 1 calc R . . C12 C 0.5067(2) 1.0023(3) 0.60497(14) 0.0483(15) Uani 1 1 d . . . H12 H 0.5313 1.0090 0.5835 0.058 Uiso 1 1 calc R . . C13 C 0.5158(2) 1.0401(3) 0.63504(15) 0.0455(14) Uani 1 1 d . . . H13 H 0.5465 1.0731 0.6342 0.055 Uiso 1 1 calc R . . C14 C 0.4806(2) 1.0305(2) 0.66652(13) 0.0332(11) Uani 1 1 d . . . H14 H 0.4873 1.0571 0.6871 0.040 Uiso 1 1 calc R . . C15 C 0.21672(19) 0.82601(19) 0.70288(11) 0.0217(8) Uani 1 1 d . . . H15A H 0.1716 0.8352 0.6969 0.026 Uiso 1 1 calc R . . H15B H 0.2187 0.8108 0.7284 0.026 Uiso 1 1 calc R . . C16 C 0.2418(2) 0.77506(19) 0.67748(11) 0.0227(9) Uani 1 1 d . . . H16A H 0.2437 0.7924 0.6524 0.027 Uiso 1 1 calc R . . H16B H 0.2113 0.7392 0.6773 0.027 Uiso 1 1 calc R . . C17 C 0.3618(2) 0.8951(2) 0.79371(12) 0.0240(9) Uani 1 1 d . . . C18 C 0.3944(2) 0.9405(3) 0.82085(14) 0.0381(12) Uani 1 1 d . . . C19 C 0.3103(2) 0.6411(2) 0.79175(12) 0.0228(9) Uani 1 1 d . . . C20 C 0.3233(2) 0.6271(2) 0.85209(12) 0.0245(9) Uani 1 1 d . . . C21 C 0.3340(2) 0.6336(2) 0.88960(12) 0.0301(10) Uani 1 1 d . . . H21 H 0.3482 0.6725 0.8999 0.036 Uiso 1 1 calc R . . C22 C 0.3226(3) 0.5807(3) 0.91111(13) 0.0370(12) Uani 1 1 d . . . H22 H 0.3289 0.5834 0.9367 0.044 Uiso 1 1 calc R . . C23 C 0.3023(3) 0.5235(3) 0.89591(14) 0.0412(12) Uani 1 1 d . . . H23 H 0.2959 0.4879 0.9114 0.049 Uiso 1 1 calc R . . C24 C 0.2912(2) 0.5172(2) 0.85890(13) 0.0334(11) Uani 1 1 d . . . H24 H 0.2772 0.4783 0.8486 0.040 Uiso 1 1 calc R . . C25 C 0.3017(2) 0.5707(2) 0.83748(12) 0.0257(9) Uani 1 1 d . . . C26 C 0.2813(2) 0.5305(2) 0.77348(11) 0.0234(9) Uani 1 1 d . . . H26A H 0.2658 0.5497 0.7505 0.028 Uiso 1 1 calc R . . H26B H 0.2473 0.5024 0.7830 0.028 Uiso 1 1 calc R . . C27 C 0.3406(2) 0.4914(2) 0.76567(11) 0.0222(9) Uani 1 1 d . . . C28 C 0.3948(2) 0.5199(2) 0.75110(12) 0.0270(9) Uani 1 1 d . . . H28 H 0.3953 0.5643 0.7468 0.032 Uiso 1 1 calc R . . C29 C 0.4479(2) 0.4835(3) 0.74279(13) 0.0346(11) Uani 1 1 d . . . H29 H 0.4849 0.5032 0.7330 0.042 Uiso 1 1 calc R . . C30 C 0.4474(2) 0.4190(2) 0.74859(13) 0.0349(11) Uani 1 1 d . . . H30 H 0.4838 0.3942 0.7426 0.042 Uiso 1 1 calc R . . C31 C 0.3939(2) 0.3905(2) 0.76315(13) 0.0313(10) Uani 1 1 d . . . H31 H 0.3937 0.3461 0.7672 0.038 Uiso 1 1 calc R . . C32 C 0.3404(2) 0.4264(2) 0.77195(11) 0.0243(9) Uani 1 1 d . . . H32 H 0.3039 0.4066 0.7822 0.029 Uiso 1 1 calc R . . C33 C 0.3576(2) 0.7322(2) 0.82368(12) 0.0272(9) Uani 1 1 d . . . H33A H 0.3662 0.7449 0.8492 0.033 Uiso 1 1 calc R . . H33B H 0.3278 0.7634 0.8129 0.033 Uiso 1 1 calc R . . C34 C 0.4195(2) 0.7318(2) 0.80223(12) 0.0293(10) Uani 1 1 d . . . H34A H 0.4472 0.6975 0.8118 0.035 Uiso 1 1 calc R . . H34B H 0.4419 0.7725 0.8063 0.035 Uiso 1 1 calc R . . C35 C 0.1722(3) 0.6866(3) 0.75028(14) 0.0389(12) Uani 1 1 d . A . C36 C 0.1036(2) 0.66818(19) 0.74089(11) 0.0451(14) Uani 1 1 d D . . C37 C 0.6976(2) 0.7126(2) 0.52674(11) 0.0239(9) Uani 1 1 d . . . C38 C 0.6945(2) 0.7233(2) 0.58790(12) 0.0289(10) Uani 1 1 d . . . C39 C 0.6887(2) 0.7151(2) 0.62549(13) 0.0362(11) Uani 1 1 d . . . H39 H 0.6733 0.6768 0.6358 0.043 Uiso 1 1 calc R . . C40 C 0.7067(2) 0.7659(3) 0.64686(13) 0.0411(13) Uani 1 1 d . . . H40 H 0.7035 0.7621 0.6726 0.049 Uiso 1 1 calc R . . C41 C 0.7293(2) 0.8227(3) 0.63224(14) 0.0388(12) Uani 1 1 d . . . H41 H 0.7415 0.8561 0.6482 0.047 Uiso 1 1 calc R . . C42 C 0.7342(2) 0.8311(2) 0.59504(13) 0.0348(11) Uani 1 1 d . . . H42 H 0.7488 0.8699 0.5848 0.042 Uiso 1 1 calc R . . C43 C 0.7168(2) 0.7801(2) 0.57316(12) 0.0271(9) Uani 1 1 d . . . C44 C 0.7283(2) 0.8231(2) 0.50908(12) 0.0264(9) Uani 1 1 d . . . H44A H 0.7426 0.8046 0.4856 0.032 Uiso 1 1 calc R . . H44B H 0.7626 0.8512 0.5182 0.032 Uiso 1 1 calc R . . C45 C 0.6684(2) 0.8619(2) 0.50267(11) 0.0246(9) Uani 1 1 d . . . C46 C 0.6674(2) 0.9268(2) 0.51018(12) 0.0281(10) Uani 1 1 d . . . H46 H 0.7040 0.9468 0.5202 0.034 Uiso 1 1 calc R . . C47 C 0.6129(2) 0.9619(2) 0.50292(12) 0.0323(11) Uani 1 1 d . . . H47 H 0.6124 1.0062 0.5078 0.039 Uiso 1 1 calc R . . C48 C 0.5593(2) 0.9331(2) 0.48875(13) 0.0342(11) Uani 1 1 d . . . H48 H 0.5222 0.9574 0.4837 0.041 Uiso 1 1 calc R . . C49 C 0.5596(2) 0.8689(2) 0.48183(13) 0.0335(11) Uani 1 1 d . . . H49 H 0.5226 0.8490 0.4722 0.040 Uiso 1 1 calc R . . C50 C 0.6137(2) 0.8333(2) 0.48890(12) 0.0289(10) Uani 1 1 d . . . H50 H 0.6135 0.7890 0.4843 0.035 Uiso 1 1 calc R . . C51 C 0.6545(2) 0.6197(2) 0.55971(13) 0.0329(11) Uani 1 1 d . . . H51A H 0.6470 0.6075 0.5855 0.040 Uiso 1 1 calc R . . H51B H 0.6844 0.5886 0.5488 0.040 Uiso 1 1 calc R . . C52 C 0.5918(2) 0.6183(2) 0.53903(13) 0.0348(11) Uani 1 1 d . . . H52A H 0.5637 0.6519 0.5489 0.042 Uiso 1 1 calc R . . H52B H 0.5706 0.5771 0.5437 0.042 Uiso 1 1 calc R . . C53 C 0.8331(2) 0.6754(2) 0.48293(13) 0.0305(10) Uani 1 1 d . . . C54 C 0.8996(2) 0.6917(2) 0.46829(14) 0.0336(11) Uani 1 1 d . . . C55 C 0.7006(2) 0.46853(19) 0.44324(11) 0.0220(8) Uani 1 1 d . . . C56 C 0.7886(2) 0.4222(2) 0.41944(11) 0.0239(9) Uani 1 1 d . . . C57 C 0.8488(2) 0.4094(2) 0.40554(12) 0.0273(9) Uani 1 1 d . . . H57 H 0.8806 0.4413 0.4032 0.033 Uiso 1 1 calc R . . C58 C 0.8599(2) 0.3467(2) 0.39517(12) 0.0299(10) Uani 1 1 d . . . H58 H 0.9004 0.3354 0.3856 0.036 Uiso 1 1 calc R . . C59 C 0.8130(2) 0.3006(2) 0.39843(12) 0.0301(10) Uani 1 1 d . . . H59 H 0.8229 0.2584 0.3914 0.036 Uiso 1 1 calc R . . C60 C 0.7526(2) 0.3137(2) 0.41144(11) 0.0265(9) Uani 1 1 d . . . H60 H 0.7206 0.2819 0.4132 0.032 Uiso 1 1 calc R . . C61 C 0.7411(2) 0.3766(2) 0.42190(11) 0.0225(9) Uani 1 1 d . . . C62 C 0.6252(2) 0.3757(2) 0.44139(11) 0.0269(9) Uani 1 1 d . . . H62A H 0.6044 0.3930 0.4636 0.032 Uiso 1 1 calc R . . H62B H 0.6317 0.3297 0.4452 0.032 Uiso 1 1 calc R . . C63 C 0.5812(2) 0.3852(2) 0.40911(11) 0.0229(9) Uani 1 1 d . . . C64 C 0.5794(2) 0.3429(2) 0.38037(12) 0.0299(10) Uani 1 1 d . . . H64 H 0.6061 0.3065 0.3809 0.036 Uiso 1 1 calc R . . C65 C 0.5392(2) 0.3524(2) 0.35086(13) 0.0338(11) Uani 1 1 d . . . H65 H 0.5390 0.3233 0.3311 0.041 Uiso 1 1 calc R . . C66 C 0.4993(2) 0.4044(2) 0.35038(14) 0.0357(11) Uani 1 1 d . . . H66 H 0.4715 0.4109 0.3303 0.043 Uiso 1 1 calc R . . C67 C 0.4996(2) 0.4471(2) 0.37902(14) 0.0347(11) Uani 1 1 d . . . H67 H 0.4719 0.4827 0.3787 0.042 Uiso 1 1 calc R . . C68 C 0.5408(2) 0.4375(2) 0.40824(13) 0.0298(10) Uani 1 1 d . . . H68 H 0.5413 0.4670 0.4278 0.036 Uiso 1 1 calc R . . C69 C 0.7943(2) 0.53910(19) 0.43553(11) 0.0229(9) Uani 1 1 d . . . H69A H 0.8398 0.5338 0.4289 0.028 Uiso 1 1 calc R . . H69B H 0.7923 0.5546 0.4610 0.028 Uiso 1 1 calc R . . C70 C 0.7635(2) 0.5874(2) 0.41029(11) 0.0231(9) Uani 1 1 d . . . H70A H 0.7613 0.5695 0.3853 0.028 Uiso 1 1 calc R . . H70B H 0.7906 0.6257 0.4093 0.028 Uiso 1 1 calc R . . C71 C 0.6347(2) 0.4548(2) 0.53059(12) 0.0244(9) Uani 1 1 d . . . C72 C 0.5933(2) 0.4073(2) 0.55186(12) 0.0297(10) Uani 1 1 d . . . C1S C 0.4677(3) 0.3072(3) 0.60534(18) 0.0586(18) Uani 1 1 d . . . H1S1 H 0.4325 0.3066 0.5873 0.070 Uiso 1 1 calc R . . H1S2 H 0.4904 0.3481 0.6028 0.070 Uiso 1 1 calc R . . C2S C 0.5566(3) 0.8410(4) 0.64793(18) 0.0628(18) Uani 1 1 d . . . H2S1 H 0.5561 0.8879 0.6482 0.075 Uiso 1 1 calc R . . H2S2 H 0.5978 0.8269 0.6584 0.075 Uiso 1 1 calc R . . Cl1 Cl 0.49334(7) 0.81226(7) 0.67532(5) 0.0614(4) Uani 1 1 d . . . Cl2 Cl 0.55090(9) 0.81427(12) 0.60282(6) 0.0906(7) Uani 1 1 d . . . Cl3 Cl 0.52066(7) 0.24501(7) 0.59582(4) 0.0498(3) Uani 1 1 d . . . Cl4 Cl 0.43548(6) 0.30150(7) 0.64971(4) 0.0443(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 F4 0.063(3) 0.063(3) 0.077(4) -0.002(2) 0.001(2) 0.013(2) F5 0.095(8) 0.192(13) 0.121(8) 0.073(8) 0.026(6) -0.073(8) F6 0.027(3) 0.064(5) 0.094(5) -0.047(4) -0.036(3) 0.025(3) F4A 0.065(4) 0.076(5) 0.083(5) -0.012(3) 0.007(3) 0.001(3) F5A 0.049(4) 0.057(4) 0.062(4) -0.006(3) 0.009(3) -0.019(3) F6A 0.053(4) 0.060(4) 0.057(4) 0.009(3) -0.015(3) 0.004(3) Pd1 0.01722(15) 0.01953(16) 0.02453(16) 0.00047(12) -0.00265(12) -0.00030(12) Pd2 0.01853(15) 0.01725(15) 0.02539(16) -0.00016(12) -0.00358(12) 0.00217(12) Pd3 0.02491(17) 0.01618(15) 0.02523(16) -0.00048(12) 0.00219(13) 0.00314(13) Pd4 0.02271(16) 0.01711(16) 0.02725(16) 0.00029(12) -0.00135(13) 0.00142(13) S1 0.0241(5) 0.0209(5) 0.0240(5) -0.0025(4) -0.0005(4) 0.0020(4) S2 0.0182(5) 0.0247(5) 0.0343(6) 0.0017(4) -0.0031(4) 0.0028(4) S4 0.0261(5) 0.0191(5) 0.0262(5) 0.0011(4) -0.0041(4) 0.0034(4) S3 0.0242(6) 0.0220(5) 0.0430(6) -0.0007(5) 0.0041(5) 0.0035(4) O1 0.0196(15) 0.0281(16) 0.0279(15) -0.0030(13) -0.0032(12) -0.0028(13) O2 0.0217(17) 0.039(2) 0.0419(19) -0.0032(15) 0.0003(14) -0.0033(14) O3 0.0188(15) 0.0270(16) 0.0321(16) -0.0001(13) -0.0036(12) 0.0023(13) O4 0.051(2) 0.051(3) 0.058(3) -0.013(2) 0.001(2) 0.001(2) O5 0.0266(16) 0.0212(15) 0.0246(15) -0.0009(12) 0.0001(12) 0.0038(12) O6 0.052(3) 0.094(4) 0.061(3) 0.049(3) -0.009(2) -0.003(2) O7 0.0254(16) 0.0258(16) 0.0334(17) 0.0023(13) 0.0018(13) -0.0014(13) O8 0.0273(18) 0.039(2) 0.046(2) 0.0096(16) -0.0060(15) -0.0045(15) N1 0.0192(17) 0.0173(17) 0.0211(16) -0.0027(13) -0.0016(13) 0.0003(14) N2 0.0248(19) 0.0191(18) 0.0284(18) 0.0011(14) -0.0013(15) -0.0058(15) N3 0.0209(18) 0.0213(18) 0.0296(19) -0.0007(15) -0.0033(15) 0.0061(15) N4 0.0245(19) 0.0223(18) 0.0236(17) -0.0040(14) 0.0008(14) -0.0009(15) N5 0.035(2) 0.0215(19) 0.0298(19) 0.0018(15) 0.0056(16) 0.0079(16) N6 0.028(2) 0.0189(18) 0.0290(19) -0.0026(15) 0.0017(15) 0.0048(15) N7 0.0273(19) 0.0159(17) 0.0241(17) -0.0010(14) -0.0043(14) 0.0019(14) N8 0.0270(19) 0.0167(17) 0.0241(17) 0.0004(14) -0.0053(14) 0.0002(15) F1 0.098(3) 0.045(2) 0.085(3) -0.0169(19) 0.009(2) -0.037(2) F2 0.053(2) 0.118(4) 0.088(3) -0.068(3) -0.042(2) 0.034(2) F3 0.052(2) 0.079(3) 0.0464(19) -0.0259(18) 0.0077(15) -0.0064(19) F7 0.054(2) 0.043(2) 0.104(3) -0.023(2) -0.001(2) -0.0170(17) F8 0.0372(17) 0.068(2) 0.055(2) 0.0232(17) 0.0134(15) 0.0118(16) F9 0.0481(19) 0.0437(18) 0.0565(19) -0.0018(15) -0.0082(15) 0.0209(15) F10 0.051(2) 0.051(2) 0.105(3) 0.020(2) 0.045(2) 0.0121(17) F11 0.059(2) 0.100(3) 0.065(2) 0.053(2) -0.0144(19) -0.026(2) F12 0.139(4) 0.0360(19) 0.051(2) -0.0125(16) 0.034(2) -0.041(2) C1 0.022(2) 0.021(2) 0.022(2) -0.0022(16) -0.0013(16) -0.0006(17) C2 0.024(2) 0.020(2) 0.0151(18) -0.0033(15) 0.0016(15) 0.0040(16) C3 0.025(2) 0.026(2) 0.024(2) 0.0015(17) 0.0031(17) 0.0042(18) C4 0.030(2) 0.034(3) 0.022(2) 0.0022(18) 0.0016(18) 0.012(2) C5 0.047(3) 0.022(2) 0.023(2) 0.0041(17) 0.007(2) 0.006(2) C6 0.040(3) 0.021(2) 0.019(2) 0.0001(16) 0.0004(18) 0.0006(19) C7 0.030(2) 0.022(2) 0.0172(19) -0.0027(16) 0.0007(16) 0.0022(18) C8 0.026(2) 0.026(2) 0.028(2) -0.0001(18) -0.0044(18) -0.0083(19) C9 0.022(2) 0.028(2) 0.029(2) 0.0023(18) -0.0020(17) 0.0033(18) C10 0.029(2) 0.032(3) 0.040(3) -0.004(2) -0.004(2) 0.002(2) C11 0.030(3) 0.063(4) 0.038(3) -0.015(3) 0.000(2) 0.008(3) C12 0.025(3) 0.086(5) 0.034(3) 0.005(3) 0.007(2) 0.007(3) C13 0.028(3) 0.065(4) 0.044(3) 0.007(3) 0.003(2) -0.015(3) C14 0.029(2) 0.038(3) 0.032(2) -0.001(2) -0.0017(19) -0.005(2) C15 0.019(2) 0.020(2) 0.026(2) -0.0003(16) -0.0033(16) -0.0018(16) C16 0.025(2) 0.017(2) 0.026(2) -0.0032(16) -0.0062(17) -0.0004(17) C17 0.026(2) 0.018(2) 0.029(2) 0.0064(17) -0.0027(18) -0.0009(17) C18 0.032(3) 0.043(3) 0.040(3) -0.013(2) 0.003(2) -0.004(2) C19 0.019(2) 0.020(2) 0.029(2) -0.0006(17) -0.0010(17) 0.0035(17) C20 0.023(2) 0.021(2) 0.030(2) -0.0021(17) 0.0000(17) 0.0040(17) C21 0.030(2) 0.031(3) 0.030(2) -0.0069(19) -0.0001(19) 0.006(2) C22 0.045(3) 0.043(3) 0.024(2) 0.001(2) 0.003(2) 0.004(2) C23 0.054(3) 0.036(3) 0.033(3) 0.006(2) 0.006(2) -0.003(3) C24 0.044(3) 0.028(2) 0.029(2) -0.0017(19) 0.005(2) -0.006(2) C25 0.024(2) 0.029(2) 0.025(2) -0.0011(18) 0.0021(17) 0.0021(18) C26 0.026(2) 0.022(2) 0.022(2) 0.0014(16) -0.0017(17) -0.0012(18) C27 0.019(2) 0.026(2) 0.021(2) -0.0023(17) -0.0080(16) -0.0030(17) C28 0.027(2) 0.027(2) 0.027(2) -0.0051(18) -0.0028(18) -0.0017(19) C29 0.024(2) 0.046(3) 0.034(3) -0.009(2) 0.0025(19) -0.007(2) C30 0.023(2) 0.043(3) 0.039(3) -0.013(2) -0.007(2) 0.006(2) C31 0.034(3) 0.024(2) 0.036(2) -0.0052(19) -0.009(2) 0.003(2) C32 0.024(2) 0.021(2) 0.027(2) -0.0017(17) -0.0035(17) -0.0022(17) C33 0.030(2) 0.021(2) 0.031(2) -0.0022(18) -0.0081(19) 0.0020(18) C34 0.027(2) 0.025(2) 0.035(2) 0.0032(19) -0.0096(19) -0.0018(19) C35 0.035(3) 0.045(3) 0.037(3) -0.015(2) -0.008(2) 0.003(2) C36 0.026(3) 0.039(3) 0.071(4) -0.019(3) 0.001(3) 0.002(2) C37 0.029(2) 0.023(2) 0.020(2) 0.0005(16) 0.0023(17) 0.0036(18) C38 0.031(2) 0.028(2) 0.028(2) -0.0029(18) 0.0019(19) 0.012(2) C39 0.040(3) 0.034(3) 0.034(3) 0.003(2) 0.007(2) 0.015(2) C40 0.041(3) 0.059(4) 0.023(2) 0.000(2) -0.004(2) 0.025(3) C41 0.040(3) 0.041(3) 0.036(3) -0.010(2) -0.008(2) 0.013(2) C42 0.033(3) 0.033(3) 0.038(3) -0.008(2) -0.006(2) 0.008(2) C43 0.029(2) 0.026(2) 0.026(2) -0.0043(18) -0.0034(18) 0.0092(19) C44 0.030(2) 0.018(2) 0.031(2) -0.0021(17) 0.0037(18) -0.0018(18) C45 0.030(2) 0.022(2) 0.022(2) 0.0020(16) 0.0074(17) 0.0036(18) C46 0.034(2) 0.024(2) 0.026(2) -0.0043(18) 0.0071(19) -0.0041(19) C47 0.047(3) 0.021(2) 0.029(2) -0.0025(18) 0.011(2) 0.008(2) C48 0.035(3) 0.037(3) 0.031(2) -0.002(2) 0.007(2) 0.013(2) C49 0.033(3) 0.033(3) 0.034(2) -0.005(2) 0.004(2) -0.001(2) C50 0.033(2) 0.022(2) 0.031(2) -0.0054(18) 0.0045(19) -0.0027(19) C51 0.043(3) 0.021(2) 0.035(2) 0.0021(19) 0.013(2) 0.001(2) C52 0.042(3) 0.026(2) 0.037(3) -0.003(2) 0.016(2) 0.000(2) C53 0.033(3) 0.025(2) 0.034(2) 0.0090(19) -0.004(2) 0.000(2) C54 0.031(3) 0.029(3) 0.041(3) 0.000(2) -0.001(2) 0.007(2) C55 0.025(2) 0.018(2) 0.023(2) 0.0004(16) -0.0028(16) 0.0000(17) C56 0.032(2) 0.018(2) 0.021(2) 0.0009(16) -0.0091(17) 0.0027(18) C57 0.028(2) 0.024(2) 0.029(2) -0.0014(18) -0.0092(18) 0.0033(19) C58 0.028(2) 0.028(2) 0.034(2) -0.0046(19) -0.0100(19) 0.011(2) C59 0.042(3) 0.019(2) 0.029(2) -0.0047(18) -0.015(2) 0.009(2) C60 0.036(2) 0.020(2) 0.024(2) -0.0011(17) -0.0111(18) 0.0005(19) C61 0.029(2) 0.019(2) 0.0193(19) 0.0018(16) -0.0075(17) 0.0028(17) C62 0.036(3) 0.021(2) 0.023(2) 0.0031(17) -0.0033(18) -0.0069(19) C63 0.025(2) 0.018(2) 0.026(2) 0.0041(16) -0.0007(17) -0.0057(17) C64 0.038(3) 0.022(2) 0.029(2) -0.0009(18) -0.0036(19) -0.001(2) C65 0.045(3) 0.027(2) 0.029(2) 0.0003(19) -0.008(2) -0.004(2) C66 0.036(3) 0.034(3) 0.037(3) 0.007(2) -0.011(2) -0.005(2) C67 0.028(2) 0.034(3) 0.043(3) -0.001(2) -0.004(2) 0.008(2) C68 0.027(2) 0.029(2) 0.033(2) -0.0031(19) 0.0023(19) -0.0019(19) C69 0.025(2) 0.018(2) 0.027(2) -0.0020(16) -0.0014(17) -0.0022(17) C70 0.026(2) 0.021(2) 0.022(2) -0.0024(16) 0.0014(16) 0.0016(17) C71 0.026(2) 0.017(2) 0.030(2) -0.0058(17) 0.0065(18) 0.0054(17) C72 0.036(3) 0.029(2) 0.025(2) -0.0002(18) 0.0070(19) 0.000(2) C1S 0.049(4) 0.061(4) 0.065(4) 0.037(3) 0.019(3) 0.010(3) C2S 0.029(3) 0.084(5) 0.076(4) -0.019(4) -0.003(3) 0.011(3) Cl1 0.0425(8) 0.0353(8) 0.1063(13) -0.0082(8) 0.0030(8) -0.0012(6) Cl2 0.0545(10) 0.1349(19) 0.0824(13) -0.0443(13) -0.0159(9) 0.0448(12) Cl3 0.0364(7) 0.0568(9) 0.0563(8) -0.0040(7) 0.0033(6) -0.0024(7) Cl4 0.0331(7) 0.0500(8) 0.0499(7) 0.0008(6) -0.0010(6) 0.0013(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 F4 C36 1.342(4) . ? F5 C36 1.292(4) . ? F6 C36 1.346(4) . ? F4A C36 1.310(4) . ? F5A C36 1.329(5) . ? F6A C36 1.289(5) . ? Pd1 C1 1.988(4) . ? Pd1 O1 2.080(3) . ? Pd1 S1 2.2754(11) . ? Pd1 S2 2.3611(11) . ? Pd2 C19 1.980(4) . ? Pd2 O3 2.080(3) . ? Pd2 S2 2.2689(11) . ? Pd2 S1 2.3709(11) . ? Pd3 C37 1.978(4) . ? Pd3 O5 2.083(3) . ? Pd3 S3 2.2630(12) . ? Pd3 S4 2.3651(11) . ? Pd4 C55 2.002(4) . ? Pd4 O7 2.073(3) . ? Pd4 S4 2.2796(11) . ? Pd4 S3 2.3676(11) . ? S1 C16 1.823(4) . ? S2 C34 1.827(5) . ? S4 C70 1.815(4) . ? S3 C52 1.827(5) . ? O1 C17 1.267(5) . ? O2 C17 1.212(5) . ? O3 C35 1.224(6) . ? O4 C35 1.248(6) . ? O5 C53 1.257(5) . ? O6 C53 1.212(6) . ? O7 C71 1.268(5) . ? O8 C71 1.215(5) . ? N1 C1 1.341(5) . ? N1 C2 1.397(5) . ? N1 C15 1.468(5) . ? N2 C1 1.351(5) . ? N2 C7 1.406(6) . ? N2 C8 1.466(5) . ? N3 C19 1.350(5) . ? N3 C20 1.391(6) . ? N3 C33 1.457(6) . ? N4 C19 1.356(5) . ? N4 C25 1.394(5) . ? N4 C26 1.464(5) . ? N5 C37 1.348(5) . ? N5 C38 1.392(6) . ? N5 C51 1.471(6) . ? N6 C37 1.359(6) . ? N6 C43 1.389(5) . ? N6 C44 1.467(6) . ? N7 C55 1.348(5) . ? N7 C56 1.394(5) . ? N7 C69 1.463(5) . ? N8 C55 1.360(5) . ? N8 C61 1.395(5) . ? N8 C62 1.469(6) . ? F1 C18 1.347(7) . ? F2 C18 1.289(6) . ? F3 C18 1.320(6) . ? F7 C54 1.329(6) . ? F8 C54 1.334(6) . ? F9 C54 1.323(5) . ? F10 C72 1.321(5) . ? F11 C72 1.314(6) . ? F12 C72 1.319(6) . ? C2 C3 1.385(6) . ? C2 C7 1.393(6) . ? C3 C4 1.394(6) . ? C4 C5 1.407(7) . ? C5 C6 1.374(7) . ? C6 C7 1.383(6) . ? C8 C9 1.518(6) . ? C9 C10 1.385(6) . ? C9 C14 1.388(6) . ? C10 C11 1.388(7) . ? C11 C12 1.379(8) . ? C12 C13 1.373(8) . ? C13 C14 1.383(7) . ? C15 C16 1.516(6) . ? C17 C18 1.540(6) . ? C20 C25 1.381(6) . ? C20 C21 1.398(6) . ? C21 C22 1.388(7) . ? C22 C23 1.395(7) . ? C23 C24 1.382(7) . ? C24 C25 1.393(6) . ? C26 C27 1.519(6) . ? C27 C28 1.389(6) . ? C27 C32 1.392(6) . ? C28 C29 1.386(7) . ? C29 C30 1.378(7) . ? C30 C31 1.378(7) . ? C31 C32 1.390(6) . ? C33 C34 1.517(6) . ? C35 C36 1.528(7) . ? C38 C39 1.393(6) . ? C38 C43 1.395(7) . ? C39 C40 1.379(8) . ? C40 C41 1.396(8) . ? C41 C42 1.378(7) . ? C42 C43 1.391(6) . ? C44 C45 1.515(6) . ? C45 C50 1.389(6) . ? C45 C46 1.397(6) . ? C46 C47 1.388(7) . ? C47 C48 1.378(7) . ? C48 C49 1.378(7) . ? C49 C50 1.383(7) . ? C51 C52 1.517(7) . ? C53 C54 1.533(7) . ? C56 C61 1.387(6) . ? C56 C57 1.388(6) . ? C57 C58 1.394(6) . ? C58 C59 1.387(7) . ? C59 C60 1.380(7) . ? C60 C61 1.402(6) . ? C62 C63 1.512(6) . ? C63 C64 1.382(6) . ? C63 C68 1.391(6) . ? C64 C65 1.385(6) . ? C65 C66 1.378(7) . ? C66 C67 1.382(7) . ? C67 C68 1.389(7) . ? C69 C70 1.519(6) . ? C71 C72 1.539(6) . ? C1S Cl3 1.754(6) . ? C1S Cl4 1.764(6) . ? C2S Cl2 1.750(7) . ? C2S Cl1 1.769(7) . ? 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 O1 92.67(14) . . ? C1 Pd1 S1 91.52(12) . . ? O1 Pd1 S1 174.44(9) . . ? C1 Pd1 S2 172.39(12) . . ? O1 Pd1 S2 94.42(9) . . ? S1 Pd1 S2 81.23(4) . . ? C19 Pd2 O3 93.72(15) . . ? C19 Pd2 S2 90.06(13) . . ? O3 Pd2 S2 175.26(9) . . ? C19 Pd2 S1 170.95(13) . . ? O3 Pd2 S1 94.96(9) . . ? S2 Pd2 S1 81.15(4) . . ? C37 Pd3 O5 93.60(15) . . ? C37 Pd3 S3 91.38(13) . . ? O5 Pd3 S3 173.97(9) . . ? C37 Pd3 S4 171.53(13) . . ? O5 Pd3 S4 93.91(8) . . ? S3 Pd3 S4 80.90(4) . . ? C55 Pd4 O7 94.79(15) . . ? C55 Pd4 S4 91.63(12) . . ? O7 Pd4 S4 172.82(9) . . ? C55 Pd4 S3 170.64(13) . . ? O7 Pd4 S3 93.37(9) . . ? S4 Pd4 S3 80.51(4) . . ? C16 S1 Pd1 107.29(13) . . ? C16 S1 Pd2 107.19(14) . . ? Pd1 S1 Pd2 81.00(3) . . ? C34 S2 Pd2 107.58(15) . . ? C34 S2 Pd1 106.42(15) . . ? Pd2 S2 Pd1 81.34(4) . . ? C70 S4 Pd4 108.85(14) . . ? C70 S4 Pd3 106.40(14) . . ? Pd4 S4 Pd3 81.51(4) . . ? C52 S3 Pd3 107.33(17) . . ? C52 S3 Pd4 107.19(16) . . ? Pd3 S3 Pd4 81.80(4) . . ? C17 O1 Pd1 116.2(3) . . ? C35 O3 Pd2 117.6(3) . . ? C53 O5 Pd3 116.6(3) . . ? C71 O7 Pd4 122.2(3) . . ? C1 N1 C2 111.1(3) . . ? C1 N1 C15 122.7(3) . . ? C2 N1 C15 126.1(3) . . ? C1 N2 C7 110.5(4) . . ? C1 N2 C8 125.1(4) . . ? C7 N2 C8 124.4(4) . . ? C19 N3 C20 110.1(4) . . ? C19 N3 C33 122.2(4) . . ? C20 N3 C33 127.3(4) . . ? C19 N4 C25 109.5(4) . . ? C19 N4 C26 125.2(4) . . ? C25 N4 C26 124.6(4) . . ? C37 N5 C38 110.6(4) . . ? C37 N5 C51 122.6(4) . . ? C38 N5 C51 126.6(4) . . ? C37 N6 C43 110.2(4) . . ? C37 N6 C44 124.6(4) . . ? C43 N6 C44 124.4(4) . . ? C55 N7 C56 111.0(4) . . ? C55 N7 C69 123.7(3) . . ? C56 N7 C69 125.3(4) . . ? C55 N8 C61 109.9(4) . . ? C55 N8 C62 125.7(4) . . ? C61 N8 C62 124.2(4) . . ? N1 C1 N2 106.7(4) . . ? N1 C1 Pd1 122.9(3) . . ? N2 C1 Pd1 130.3(3) . . ? C3 C2 C7 121.7(4) . . ? C3 C2 N1 132.3(4) . . ? C7 C2 N1 106.0(3) . . ? C2 C3 C4 116.5(4) . . ? C3 C4 C5 121.1(4) . . ? C6 C5 C4 122.0(4) . . ? C5 C6 C7 116.6(4) . . ? C6 C7 C2 122.0(4) . . ? C6 C7 N2 132.2(4) . . ? C2 C7 N2 105.7(4) . . ? N2 C8 C9 114.0(3) . . ? C10 C9 C14 118.8(4) . . ? C10 C9 C8 122.3(4) . . ? C14 C9 C8 118.8(4) . . ? C9 C10 C11 120.6(5) . . ? C12 C11 C10 120.0(5) . . ? C13 C12 C11 119.6(5) . . ? C12 C13 C14 120.7(5) . . ? C13 C14 C9 120.2(5) . . ? N1 C15 C16 110.4(3) . . ? C15 C16 S1 114.1(3) . . ? O2 C17 O1 130.7(4) . . ? O2 C17 C18 117.6(4) . . ? O1 C17 C18 111.7(4) . . ? F2 C18 F3 109.5(5) . . ? F2 C18 F1 105.5(5) . . ? F3 C18 F1 104.0(4) . . ? F2 C18 C17 114.4(4) . . ? F3 C18 C17 113.6(4) . . ? F1 C18 C17 109.1(4) . . ? N3 C19 N4 107.2(4) . . ? N3 C19 Pd2 123.7(3) . . ? N4 C19 Pd2 129.1(3) . . ? C25 C20 N3 106.4(4) . . ? C25 C20 C21 121.2(4) . . ? N3 C20 C21 132.4(4) . . ? C22 C21 C20 116.8(4) . . ? C21 C22 C23 121.5(4) . . ? C24 C23 C22 121.7(5) . . ? C23 C24 C25 116.7(5) . . ? C20 C25 C24 122.1(4) . . ? C20 C25 N4 106.8(4) . . ? C24 C25 N4 131.0(4) . . ? N4 C26 C27 111.5(3) . . ? C28 C27 C32 119.5(4) . . ? C28 C27 C26 120.4(4) . . ? C32 C27 C26 120.1(4) . . ? C29 C28 C27 120.0(4) . . ? C30 C29 C28 120.5(5) . . ? C31 C30 C29 119.7(5) . . ? C30 C31 C32 120.5(4) . . ? C31 C32 C27 119.7(4) . . ? N3 C33 C34 110.1(4) . . ? C33 C34 S2 114.2(3) . . ? O3 C35 O4 127.5(5) . . ? O3 C35 C36 116.1(4) . . ? O4 C35 C36 115.3(4) . . ? F6A C36 F5 114.6(9) . . ? F6A C36 F4A 109.5(5) . . ? F5 C36 F4A 72.5(5) . . ? F6A C36 F5A 107.5(4) . . ? F5 C36 F5A 33.2(5) . . ? F4A C36 F5A 105.4(4) . . ? F6A C36 F4 81.0(5) . . ? F5 C36 F4 106.4(4) . . ? F4A C36 F4 37.5(4) . . ? F5A C36 F4 139.1(5) . . ? F6A C36 F6 21.8(5) . . ? F5 C36 F6 106.3(4) . . ? F4A C36 F6 127.9(6) . . ? F5A C36 F6 89.8(6) . . ? F4 C36 F6 102.7(4) . . ? F6A C36 C35 117.0(7) . . ? F5 C36 C35 121.5(6) . . ? F4A C36 C35 112.3(6) . . ? F5A C36 C35 104.2(6) . . ? F4 C36 C35 106.9(5) . . ? F6 C36 C35 111.4(4) . . ? N5 C37 N6 106.7(4) . . ? N5 C37 Pd3 124.0(3) . . ? N6 C37 Pd3 129.0(3) . . ? N5 C38 C39 132.7(5) . . ? N5 C38 C43 106.1(4) . . ? C39 C38 C43 121.2(4) . . ? C40 C39 C38 116.2(5) . . ? C39 C40 C41 122.8(5) . . ? C42 C41 C40 121.0(5) . . ? C41 C42 C43 116.8(5) . . ? N6 C43 C42 131.7(5) . . ? N6 C43 C38 106.4(4) . . ? C42 C43 C38 122.0(4) . . ? N6 C44 C45 112.0(4) . . ? C50 C45 C46 118.9(4) . . ? C50 C45 C44 120.3(4) . . ? C46 C45 C44 120.7(4) . . ? C47 C46 C45 119.9(4) . . ? C48 C47 C46 120.4(4) . . ? C49 C48 C47 120.0(5) . . ? C48 C49 C50 120.1(5) . . ? C49 C50 C45 120.6(4) . . ? N5 C51 C52 110.7(4) . . ? C51 C52 S3 115.1(3) . . ? O6 C53 O5 129.5(5) . . ? O6 C53 C54 116.3(4) . . ? O5 C53 C54 114.0(4) . . ? F9 C54 F7 107.5(4) . . ? F9 C54 F8 106.8(4) . . ? F7 C54 F8 106.6(4) . . ? F9 C54 C53 110.8(4) . . ? F7 C54 C53 112.0(4) . . ? F8 C54 C53 112.7(4) . . ? N7 C55 N8 106.4(4) . . ? N7 C55 Pd4 122.5(3) . . ? N8 C55 Pd4 131.0(3) . . ? C61 C56 C57 122.8(4) . . ? C61 C56 N7 105.8(4) . . ? C57 C56 N7 131.4(4) . . ? C56 C57 C58 115.8(4) . . ? C59 C58 C57 121.6(4) . . ? C60 C59 C58 122.6(4) . . ? C59 C60 C61 116.1(4) . . ? C56 C61 N8 106.8(4) . . ? C56 C61 C60 121.1(4) . . ? N8 C61 C60 132.1(4) . . ? N8 C62 C63 112.9(3) . . ? C64 C63 C68 118.6(4) . . ? C64 C63 C62 121.8(4) . . ? C68 C63 C62 119.6(4) . . ? C63 C64 C65 121.2(4) . . ? C66 C65 C64 119.6(5) . . ? C65 C66 C67 120.4(4) . . ? C66 C67 C68 119.6(5) . . ? C67 C68 C63 120.7(4) . . ? N7 C69 C70 110.7(3) . . ? C69 C70 S4 112.8(3) . . ? O8 C71 O7 130.2(4) . . ? O8 C71 C72 118.6(4) . . ? O7 C71 C72 111.2(4) . . ? F11 C72 F12 107.0(4) . . ? F11 C72 F10 106.2(4) . . ? F12 C72 F10 105.4(4) . . ? F11 C72 C71 113.9(4) . . ? F12 C72 C71 111.8(4) . . ? F10 C72 C71 112.0(4) . . ? Cl3 C1S Cl4 112.0(3) . . ? Cl2 C2S Cl1 112.0(4) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.540 _refine_diff_density_min -0.733 _refine_diff_density_rms 0.121 #===END data_8664 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C70 H74 B2 Br2 F8 N10 O3 Pd4 S4' _chemical_formula_weight 1990.67 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' 'B' 'B' 0.0013 0.0007 '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' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 '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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.922(3) _cell_length_b 13.527(3) _cell_length_c 23.326(5) _cell_angle_alpha 90.00 _cell_angle_beta 91.314(5) _cell_angle_gamma 90.00 _cell_volume 4076.4(14) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 1177 _cell_measurement_theta_min 2.18 _cell_measurement_theta_max 17.26 _exptl_crystal_description Needle _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas 'Not Measured' _exptl_crystal_density_diffrn 1.622 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1976 _exptl_absorpt_coefficient_mu 2.018 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.3772 _exptl_absorpt_correction_T_max 0.8885 _exptl_absorpt_process_details 'Sadabs, (Sheldrick 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23534 _diffrn_reflns_av_R_equivalents 0.1199 _diffrn_reflns_av_sigmaI/netI 0.1288 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.74 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7177 _reflns_number_gt 4128 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1216P)^2^+2.6890P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7177 _refine_ls_number_parameters 389 _refine_ls_number_restraints 48 _refine_ls_R_factor_all 0.1525 _refine_ls_R_factor_gt 0.0869 _refine_ls_wR_factor_ref 0.2448 _refine_ls_wR_factor_gt 0.2116 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.025 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.63734(7) 0.38166(7) 0.51047(4) 0.0440(3) Uani 1 1 d . . . Pd2 Pd 0.49000(7) 0.46955(8) 0.60243(4) 0.0443(3) Uani 1 1 d . . . Br3 Br 0.44151(9) 0.37064(10) 0.51394(6) 0.0510(4) Uani 1 1 d . . . S1 S 0.6273(3) 0.3595(2) 0.60887(15) 0.0518(9) Uani 1 1 d . . . S2 S 0.6403(2) 0.4112(3) 0.41194(15) 0.0512(9) Uani 1 1 d . . . N1 N 0.8642(7) 0.3327(8) 0.4892(5) 0.054(3) Uani 1 1 d . C . N2 N 0.8403(7) 0.4396(8) 0.5557(5) 0.049(3) Uani 1 1 d . . . N3 N 0.5190(9) 0.4861(9) 0.7300(4) 0.061(3) Uani 1 1 d . C . N4 N 0.5298(9) 0.6260(9) 0.6874(5) 0.066(3) Uani 1 1 d . . . C1 C 0.7885(9) 0.3864(9) 0.5167(5) 0.046(3) Uani 1 1 d . . . C2 C 0.9636(11) 0.3527(11) 0.5128(7) 0.061(4) Uani 1 1 d . . . C3 C 1.0588(11) 0.3177(11) 0.4983(8) 0.079(6) Uani 1 1 d . . . H3 H 1.0664 0.2711 0.4682 0.095 Uiso 1 1 calc R . . C4 C 1.1412(14) 0.3519(14) 0.5283(9) 0.086(6) Uani 1 1 d . . . H4 H 1.2086 0.3285 0.5202 0.104 Uiso 1 1 calc R . . C5 C 1.1276(10) 0.4218(12) 0.5712(8) 0.073(5) Uani 1 1 d . . . H5 H 1.1873 0.4446 0.5918 0.087 Uiso 1 1 calc R . . C6 C 1.0313(11) 0.4607(10) 0.5860(7) 0.065(4) Uani 1 1 d . . . H6 H 1.0234 0.5092 0.6150 0.078 Uiso 1 1 calc R . . C7 C 0.9495(9) 0.4224(10) 0.5548(6) 0.051(4) Uani 1 1 d . . . C8 C 0.8466(11) 0.2566(10) 0.4458(6) 0.061(4) Uani 1 1 d . . . H8A H 0.9113 0.2516 0.4241 0.074 Uiso 1 1 calc R A 1 H8B H 0.7931 0.2829 0.4188 0.074 Uiso 1 1 calc R A 1 C9 C 0.7876(11) 0.4968(10) 0.5992(7) 0.064(4) Uani 1 1 d . . . H9A H 0.7348 0.5400 0.5806 0.077 Uiso 1 1 calc R . . H9B H 0.8381 0.5394 0.6201 0.077 Uiso 1 1 calc R . . C10 C 0.7360(9) 0.4274(11) 0.6411(6) 0.058(4) Uani 1 1 d . . . H10A H 0.7112 0.4662 0.6740 0.069 Uiso 1 1 calc R . . H10B H 0.7880 0.3795 0.6559 0.069 Uiso 1 1 calc R . . C11 C 0.5205(10) 0.5296(11) 0.6787(6) 0.054(3) Uani 1 1 d . . . C12 C 0.5366(13) 0.6472(15) 0.7455(8) 0.082(5) Uani 1 1 d . . . C13 C 0.5419(14) 0.7335(15) 0.7766(9) 0.103(6) Uani 1 1 d . . . H13 H 0.5477 0.7944 0.7566 0.123 Uiso 1 1 calc R . . C14 C 0.5395(17) 0.735(2) 0.8323(9) 0.122(9) Uani 1 1 d . . . H14 H 0.5417 0.7964 0.8524 0.146 Uiso 1 1 calc R . . C15 C 0.5334(18) 0.644(3) 0.8629(9) 0.141(11) Uani 1 1 d . . . H15 H 0.5331 0.6438 0.9037 0.169 Uiso 1 1 calc R . . C16 C 0.5280(13) 0.5568(16) 0.8339(6) 0.087(6) Uani 1 1 d . . . H16 H 0.5236 0.4957 0.8539 0.105 Uiso 1 1 calc R . . C17 C 0.5289(12) 0.5591(15) 0.7729(7) 0.078(5) Uani 1 1 d . . . C18 C 0.5034(12) 0.3796(12) 0.7413(6) 0.070(4) Uani 1 1 d . . . H18A H 0.5270 0.3700 0.7816 0.084 Uiso 1 1 calc R B 1 H18B H 0.5549 0.3455 0.7176 0.084 Uiso 1 1 calc R B 1 C19 C 0.5216(11) 0.6993(11) 0.6401(6) 0.066(4) Uani 1 1 d . . . H19A H 0.5671 0.6791 0.6086 0.079 Uiso 1 1 calc R . . H19B H 0.5453 0.7647 0.6543 0.079 Uiso 1 1 calc R . . C20 C 0.4120(11) 0.7074(10) 0.6176(6) 0.059(4) Uani 1 1 d . . . H20A H 0.4089 0.7583 0.5872 0.071 Uiso 1 1 calc R . . H20B H 0.3674 0.7297 0.6491 0.071 Uiso 1 1 calc R . . C21 C 0.8153(8) 0.1542(6) 0.4594(4) 0.036(6) Uiso 0.50 1 d PG C 1 C22 C 0.7999(6) 0.1312(5) 0.5166(3) 0.056(7) Uiso 0.50 1 d PG C 1 H22 H 0.8018 0.1820 0.5448 0.067 Uiso 0.50 1 calc PR C 1 C23 C 0.7819(7) 0.0339(5) 0.5327(3) 0.068(10) Uiso 0.50 1 d PG C 1 H23 H 0.7714 0.0182 0.5719 0.082 Uiso 0.50 1 calc PR C 1 C24 C 0.7792(8) -0.0404(5) 0.4916(4) 0.063(8) Uiso 0.50 1 d PG C 1 H24 H 0.7668 -0.1069 0.5026 0.075 Uiso 0.50 1 calc PR C 1 C25 C 0.7946(8) -0.0175(7) 0.4343(4) 0.064(8) Uiso 0.50 1 d PG C 1 H25 H 0.7928 -0.0683 0.4062 0.077 Uiso 0.50 1 calc PR C 1 C26 C 0.8127(8) 0.0798(7) 0.4182(3) 0.071(9) Uiso 0.50 1 d PG C 1 H26 H 0.8232 0.0955 0.3791 0.086 Uiso 0.50 1 calc PR C 1 C41 C 0.8512(7) 0.1555(5) 0.4758(4) 0.044(6) Uiso 0.50 1 d PG C -2 C42 C 0.7620(6) 0.1267(5) 0.5035(3) 0.060(8) Uiso 0.50 1 d PG C -2 H42 H 0.7070 0.1725 0.5081 0.071 Uiso 0.50 1 calc PR C -2 C43 C 0.7533(7) 0.0310(5) 0.5246(3) 0.071(10) Uiso 0.50 1 d PG C -2 H43 H 0.6923 0.0114 0.5435 0.085 Uiso 0.50 1 calc PR C -2 C44 C 0.8338(8) -0.0359(6) 0.5180(4) 0.068(8) Uiso 0.50 1 d PG C -2 H44 H 0.8278 -0.1013 0.5324 0.082 Uiso 0.50 1 calc PR C -2 C45 C 0.9230(7) -0.0071(7) 0.4903(4) 0.072(9) Uiso 0.50 1 d PG C -2 H45 H 0.9780 -0.0528 0.4857 0.086 Uiso 0.50 1 calc PR C -2 C46 C 0.9317(7) 0.0886(7) 0.4692(4) 0.064(8) Uiso 0.50 1 d PG C -2 H46 H 0.9926 0.1083 0.4502 0.077 Uiso 0.50 1 calc PR C -2 C31 C 0.4022(6) 0.3160(6) 0.7347(3) 0.040(6) Uiso 0.50 1 d PG C 1 C32 C 0.3246(6) 0.3315(7) 0.6934(4) 0.120(14) Uiso 0.50 1 d PG C 1 H32 H 0.3297 0.3850 0.6673 0.144 Uiso 0.50 1 calc PR C 1 C33 C 0.2395(6) 0.2688(9) 0.6904(5) 0.108(13) Uiso 0.50 1 d PG C 1 H33 H 0.1864 0.2793 0.6622 0.129 Uiso 0.50 1 calc PR C 1 C34 C 0.2319(8) 0.1905(8) 0.7287(6) 0.094(11) Uiso 0.50 1 d PG C 1 H34 H 0.1738 0.1476 0.7267 0.113 Uiso 0.50 1 calc PR C 1 C35 C 0.3095(10) 0.1750(7) 0.7700(5) 0.141(17) Uiso 0.50 1 d PG C 1 H35 H 0.3044 0.1215 0.7962 0.169 Uiso 0.50 1 calc PR C 1 C36 C 0.3947(9) 0.2377(7) 0.7730(4) 0.147(18) Uiso 0.50 1 d PG C 1 H36 H 0.4477 0.2271 0.8012 0.176 Uiso 0.50 1 calc PR C 1 C51 C 0.3795(7) 0.3933(7) 0.7598(4) 0.062(8) Uiso 0.50 1 d PG C -2 C52 C 0.3028(7) 0.4069(7) 0.7179(4) 0.050(7) Uiso 0.50 1 d PG C -2 H52 H 0.3203 0.4078 0.6785 0.060 Uiso 0.50 1 calc PR C -2 C53 C 0.2004(8) 0.4194(9) 0.7334(4) 0.072(9) Uiso 0.50 1 d PG C -2 H53 H 0.1479 0.4287 0.7047 0.087 Uiso 0.50 1 calc PR C -2 C54 C 0.1748(8) 0.4181(8) 0.7910(5) 0.073(9) Uiso 0.50 1 d PG C -2 H54 H 0.1048 0.4265 0.8016 0.087 Uiso 0.50 1 calc PR C -2 C55 C 0.2515(8) 0.4044(8) 0.8330(4) 0.077(9) Uiso 0.50 1 d PG C -2 H55 H 0.2340 0.4035 0.8723 0.092 Uiso 0.50 1 calc PR C -2 C56 C 0.3539(8) 0.3920(9) 0.8174(4) 0.082(10) Uiso 0.50 1 d PG C -2 H56 H 0.4063 0.3826 0.8461 0.098 Uiso 0.50 1 calc PR C -2 C1S C 0.916(2) 0.541(2) 0.7429(12) 0.058(7) Uiso 0.50 1 d P D 3 H1S H 0.9416 0.6022 0.7291 0.070 Uiso 0.50 1 calc PR D 3 C2S C 0.817(2) 0.630(2) 0.8120(13) 0.068(8) Uiso 0.50 1 d P D 3 H2S1 H 0.8619 0.6553 0.8428 0.102 Uiso 0.50 1 calc PR D 3 H2S2 H 0.7501 0.6099 0.8278 0.102 Uiso 0.50 1 calc PR D 3 H2S3 H 0.8050 0.6811 0.7830 0.102 Uiso 0.50 1 calc PR D 3 C3S C 0.814(3) 0.471(2) 0.8027(14) 0.077(9) Uiso 0.50 1 d P D 3 H3S1 H 0.8547 0.4384 0.8330 0.115 Uiso 0.50 1 calc PR D 3 H3S2 H 0.8094 0.4285 0.7688 0.115 Uiso 0.50 1 calc PR D 3 H3S3 H 0.7442 0.4850 0.8163 0.115 Uiso 0.50 1 calc PR D 3 N1S N 0.8591(16) 0.5550(15) 0.7890(9) 0.047(5) Uiso 0.50 1 d P D 3 O1S O 0.9435(12) 0.4784(11) 0.7156(7) 0.045(4) Uiso 0.50 1 d P D 3 B1 B 0.6624(10) 0.2587(10) 0.8663(6) 0.064(9) Uiso 0.50 1 d PD E 3 F1 F 0.7315(9) 0.2381(10) 0.9101(7) 0.070(5) Uani 0.50 1 d PD E 3 F2 F 0.5804(8) 0.1953(10) 0.8693(6) 0.062(4) Uani 0.50 1 d PD E 3 F3 F 0.6266(11) 0.3528(9) 0.8715(6) 0.072(5) Uani 0.50 1 d PD E 3 F4 F 0.7084(14) 0.2474(14) 0.8147(6) 0.124(10) Uani 0.50 1 d PD E 3 F5 F 0.6003(14) 0.269(2) 0.8637(11) 0.143(6) Uiso 0.50 1 d PD F 4 F6 F 0.7246(18) 0.3535(15) 0.8214(10) 0.143(6) Uiso 0.50 1 d PD F 4 F7 F 0.734(2) 0.1910(15) 0.8252(11) 0.143(6) Uiso 0.50 1 d PD F 4 F8 F 0.756(2) 0.2799(19) 0.9052(9) 0.143(6) Uiso 0.50 1 d PD F 4 B2 B 0.7036(15) 0.2729(14) 0.8539(8) 0.086(13) Uiso 0.50 1 d PD F 4 O1W O 0.518(3) 0.079(3) 0.4137(15) 0.150(12) Uiso 0.50 1 d P G 5 C6X C 0.506(7) 0.045(4) 0.395(2) 0.29(2) Uiso 0.50 1 d PD H -6 H6X1 H 0.5617 0.0176 0.3721 0.442 Uiso 0.50 1 calc PR H -6 H6X2 H 0.5100 0.1173 0.3947 0.442 Uiso 0.50 1 calc PR H -6 H6X3 H 0.4387 0.0245 0.3780 0.442 Uiso 0.50 1 calc PR H -6 C4X C 0.552(5) -0.086(3) 0.461(2) 0.29(2) Uiso 0.50 1 d PD H -6 H4X H 0.5597 -0.1135 0.4980 0.353 Uiso 0.50 1 calc PR H -6 N2X N 0.515(3) 0.010(3) 0.4514(17) 0.29(2) Uiso 0.50 1 d PD H -6 O2X O 0.574(4) -0.135(3) 0.415(2) 0.29(2) Uiso 0.50 1 d PD H -6 C5X C 0.491(6) 0.072(5) 0.497(2) 0.29(2) Uiso 0.50 1 d PD H -6 H5X1 H 0.4919 0.1406 0.4846 0.442 Uiso 0.50 1 calc PR H -6 H5X2 H 0.5416 0.0620 0.5284 0.442 Uiso 0.50 1 calc PR H -6 H5X3 H 0.4214 0.0553 0.5108 0.442 Uiso 0.50 1 calc PR H -6 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 0.0266(5) 0.0546(6) 0.0507(6) -0.0103(5) 0.0020(4) -0.0103(4) Pd2 0.0302(5) 0.0600(7) 0.0427(6) -0.0117(5) 0.0015(4) -0.0075(5) Br3 0.0306(7) 0.0664(9) 0.0561(8) -0.0167(7) 0.0033(6) -0.0173(6) S1 0.0426(19) 0.061(2) 0.051(2) -0.0093(17) -0.0019(16) -0.0011(16) S2 0.0324(17) 0.065(2) 0.057(2) -0.0064(18) 0.0027(15) -0.0038(16) N1 0.027(6) 0.058(7) 0.078(8) 0.014(6) 0.010(6) -0.011(5) N2 0.024(5) 0.050(6) 0.073(8) 0.003(6) -0.007(5) -0.004(5) N3 0.061(8) 0.093(9) 0.028(6) -0.013(6) 0.005(5) 0.006(7) N4 0.065(8) 0.078(9) 0.054(8) -0.016(7) -0.002(6) 0.022(7) C1 0.037(7) 0.053(8) 0.048(8) 0.001(7) 0.004(6) -0.013(6) C2 0.044(8) 0.063(9) 0.075(11) 0.022(8) 0.012(8) -0.001(7) C3 0.040(9) 0.066(10) 0.132(16) 0.050(10) 0.028(10) -0.001(8) C4 0.059(12) 0.086(13) 0.115(16) 0.023(12) 0.017(11) -0.003(10) C5 0.022(7) 0.081(11) 0.115(14) 0.051(11) -0.016(8) -0.023(7) C6 0.049(9) 0.050(8) 0.094(12) 0.038(8) -0.018(8) -0.017(7) C7 0.029(7) 0.048(8) 0.075(10) 0.043(8) -0.005(7) -0.010(6) C8 0.052(8) 0.071(9) 0.062(10) -0.006(8) 0.017(7) 0.018(8) C9 0.053(9) 0.047(8) 0.091(12) 0.001(8) -0.029(8) -0.003(7) C10 0.022(6) 0.084(10) 0.067(10) -0.017(8) -0.012(6) 0.001(7) C11 0.043(8) 0.067(10) 0.052(9) -0.014(8) 0.000(6) 0.008(7) C12 0.078(12) 0.102(14) 0.066(12) -0.045(11) -0.010(9) 0.016(11) C13 0.101(15) 0.110(15) 0.096(15) -0.051(13) -0.008(12) 0.020(12) C14 0.109(17) 0.20(3) 0.056(13) -0.064(16) -0.009(12) 0.056(18) C15 0.111(18) 0.26(3) 0.046(12) -0.056(18) -0.009(12) 0.08(2) C16 0.084(12) 0.150(17) 0.028(8) -0.024(10) -0.013(8) 0.037(12) C17 0.060(10) 0.120(15) 0.055(10) -0.027(11) -0.005(8) 0.045(10) C18 0.077(11) 0.094(12) 0.040(8) 0.021(8) 0.003(7) -0.013(9) C19 0.057(9) 0.076(10) 0.064(10) -0.021(9) -0.003(8) -0.017(8) C20 0.066(9) 0.060(9) 0.051(9) -0.026(7) -0.002(7) -0.003(7) F1 0.033(8) 0.060(10) 0.117(15) 0.041(10) -0.004(8) -0.004(7) F2 0.020(7) 0.092(12) 0.074(11) -0.004(9) -0.001(7) 0.008(7) F3 0.077(11) 0.095(12) 0.044(9) 0.001(9) -0.013(8) 0.050(10) F4 0.14(2) 0.133(19) 0.105(18) -0.053(16) 0.090(17) -0.051(16) _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 1.956(12) . ? Pd1 S1 2.321(4) . ? Pd1 S2 2.334(4) . ? Pd1 Br3 2.5382(15) . ? Pd1 Pd2 3.1350(13) . ? Pd2 C11 1.986(13) . ? Pd2 S1 2.318(3) . ? Pd2 S2 2.350(4) 3_666 ? Pd2 Br3 2.5268(16) . ? S1 C10 1.825(12) . ? S2 C20 1.866(13) 3_666 ? S2 Pd2 2.350(4) 3_666 ? N1 C1 1.388(15) . ? N1 C2 1.411(17) . ? N1 C8 1.457(17) . ? N2 C1 1.330(16) . ? N2 C7 1.431(15) . ? N2 C9 1.457(17) . ? N3 C11 1.334(17) . ? N3 C17 1.411(19) . ? N3 C18 1.478(17) . ? N4 C11 1.325(17) . ? N4 C12 1.386(19) . ? N4 C19 1.485(18) . ? C2 C3 1.369(19) . ? C2 C7 1.38(2) . ? C3 C4 1.34(2) . ? C4 C5 1.39(2) . ? C5 C6 1.40(2) . ? C6 C7 1.370(18) . ? C8 C21 1.479(16) . ? C8 C41 1.536(16) . ? C9 C10 1.520(19) . ? C12 C17 1.36(2) . ? C12 C13 1.38(2) . ? C13 C14 1.30(3) . ? C14 C15 1.43(3) . ? C15 C16 1.36(3) . ? C16 C17 1.42(2) . ? C18 C31 1.570(17) . ? C18 C51 1.678(17) . ? C19 C20 1.502(19) . ? C20 S2 1.866(13) 3_666 ? C21 C22 1.3900 . ? C21 C26 1.3900 . ? C22 C23 1.3900 . ? C23 C24 1.3900 . ? C24 C25 1.3900 . ? C25 C26 1.3900 . ? C41 C46 1.3900 . ? C41 C42 1.3900 . ? C42 C43 1.3900 . ? C43 C44 1.3900 . ? C44 C45 1.3900 . ? C45 C46 1.3900 . ? C31 C32 1.3899 . ? C31 C36 1.3900 . ? C32 C33 1.3900 . ? C33 C34 1.3900 . ? C34 C35 1.3900 . ? C35 C36 1.3900 . ? C51 C52 1.3900 . ? C51 C56 1.3900 . ? C52 C53 1.3900 . ? C53 C54 1.3900 . ? C54 C55 1.3900 . ? C55 C56 1.3900 . ? C1S O1S 1.12(3) . ? C1S N1S 1.33(3) . ? C2S N1S 1.27(3) . ? C3S N1S 1.32(3) . ? B1 F3 1.361(10) . ? B1 F4 1.363(10) . ? B1 F2 1.366(10) . ? B1 F1 1.370(10) . ? F5 B2 1.360(10) . ? F6 B2 1.359(10) . ? F7 B2 1.358(10) . ? F8 B2 1.364(10) . ? C6X N2X 1.406(10) . ? C4X O2X 1.289(10) . ? C4X N2X 1.403(10) . ? N2X C5X 1.395(10) . ? 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 S1 90.5(4) . . ? C1 Pd1 S2 91.6(4) . . ? S1 Pd1 S2 176.67(12) . . ? C1 Pd1 Br3 173.8(4) . . ? S1 Pd1 Br3 83.26(9) . . ? S2 Pd1 Br3 94.60(9) . . ? C1 Pd1 Pd2 123.9(4) . . ? S1 Pd1 Pd2 47.45(9) . . ? S2 Pd1 Pd2 129.25(9) . . ? Br3 Pd1 Pd2 51.60(4) . . ? C11 Pd2 S1 93.9(4) . . ? C11 Pd2 S2 88.5(4) . 3_666 ? S1 Pd2 S2 174.09(13) . 3_666 ? C11 Pd2 Br3 171.2(4) . . ? S1 Pd2 Br3 83.58(9) . . ? S2 Pd2 Br3 94.79(10) 3_666 . ? C11 Pd2 Pd1 131.0(4) . . ? S1 Pd2 Pd1 47.53(9) . . ? S2 Pd2 Pd1 127.38(9) 3_666 . ? Br3 Pd2 Pd1 51.92(4) . . ? Pd2 Br3 Pd1 76.48(4) . . ? C10 S1 Pd2 106.6(5) . . ? C10 S1 Pd1 106.4(5) . . ? Pd2 S1 Pd1 85.02(12) . . ? C20 S2 Pd1 101.7(5) 3_666 . ? C20 S2 Pd2 106.6(5) 3_666 3_666 ? Pd1 S2 Pd2 103.31(13) . 3_666 ? C1 N1 C2 111.3(12) . . ? C1 N1 C8 126.1(11) . . ? C2 N1 C8 122.2(12) . . ? C1 N2 C7 112.5(11) . . ? C1 N2 C9 121.9(10) . . ? C7 N2 C9 125.0(11) . . ? C11 N3 C17 109.0(13) . . ? C11 N3 C18 126.5(12) . . ? C17 N3 C18 124.4(13) . . ? C11 N4 C12 111.0(14) . . ? C11 N4 C19 122.6(12) . . ? C12 N4 C19 126.1(14) . . ? N2 C1 N1 104.5(11) . . ? N2 C1 Pd1 123.7(9) . . ? N1 C1 Pd1 131.4(9) . . ? C3 C2 C7 123.2(16) . . ? C3 C2 N1 130.7(17) . . ? C7 C2 N1 106.0(12) . . ? C4 C3 C2 117.3(19) . . ? C3 C4 C5 119.9(17) . . ? C4 C5 C6 124.0(15) . . ? C7 C6 C5 114.0(16) . . ? C6 C7 C2 121.6(14) . . ? C6 C7 N2 132.8(15) . . ? C2 C7 N2 105.6(12) . . ? N1 C8 C21 123.6(11) . . ? N1 C8 C41 108.0(11) . . ? C21 C8 C41 22.7(2) . . ? N2 C9 C10 109.7(10) . . ? C9 C10 S1 113.0(10) . . ? N4 C11 N3 107.4(12) . . ? N4 C11 Pd2 123.8(11) . . ? N3 C11 Pd2 128.0(11) . . ? C17 C12 C13 120.0(18) . . ? C17 C12 N4 106.0(14) . . ? C13 C12 N4 134(2) . . ? C14 C13 C12 123(2) . . ? C13 C14 C15 119(2) . . ? C16 C15 C14 120.2(19) . . ? C15 C16 C17 118(2) . . ? C12 C17 N3 106.6(14) . . ? C12 C17 C16 119.6(17) . . ? N3 C17 C16 133.7(19) . . ? N3 C18 C31 129.3(12) . . ? N3 C18 C51 94.2(10) . . ? C31 C18 C51 44.6(5) . . ? N4 C19 C20 111.0(12) . . ? C19 C20 S2 113.4(10) . 3_666 ? C22 C21 C26 120.0 . . ? C22 C21 C8 117.4(7) . . ? C26 C21 C8 122.2(7) . . ? C23 C22 C21 120.0 . . ? C24 C23 C22 120.0 . . ? C23 C24 C25 120.0 . . ? C24 C25 C26 120.0 . . ? C25 C26 C21 120.0 . . ? C46 C41 C42 120.0 . . ? C46 C41 C8 123.4(6) . . ? C42 C41 C8 115.9(6) . . ? C43 C42 C41 120.0 . . ? C42 C43 C44 120.0 . . ? C45 C44 C43 120.0 . . ? C46 C45 C44 120.0 . . ? C45 C46 C41 120.0 . . ? C32 C31 C36 120.0 . . ? C32 C31 C18 124.8(7) . . ? C36 C31 C18 115.1(7) . . ? C31 C32 C33 120.0 . . ? C34 C33 C32 120.0 . . ? C33 C34 C35 120.0 . . ? C36 C35 C34 120.0 . . ? C35 C36 C31 120.0 . . ? C52 C51 C56 120.0 . . ? C52 C51 C18 120.2(6) . . ? C56 C51 C18 119.8(6) . . ? C51 C52 C53 120.0 . . ? C52 C53 C54 120.0 . . ? C55 C54 C53 120.0 . . ? C54 C55 C56 120.0 . . ? C51 C56 C55 120.0 . . ? O1S C1S N1S 139(3) . . ? C2S N1S C3S 112(2) . . ? C2S N1S C1S 135(2) . . ? C3S N1S C1S 109(2) . . ? F3 B1 F4 109.8(10) . . ? F3 B1 F2 108.5(10) . . ? F4 B1 F2 109.2(10) . . ? F3 B1 F1 110.0(10) . . ? F4 B1 F1 110.2(10) . . ? F2 B1 F1 109.1(10) . . ? F7 B2 F6 108.4(11) . . ? F7 B2 F5 110.5(11) . . ? F6 B2 F5 109.4(11) . . ? F7 B2 F8 110.3(11) . . ? F6 B2 F8 109.4(11) . . ? F5 B2 F8 108.9(11) . . ? O2X C4X N2X 115.9(18) . . ? C5X N2X C4X 121.2(11) . . ? C5X N2X C6X 120.3(11) . . ? C4X N2X C6X 118.5(11) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.089 _refine_diff_density_min -0.711 _refine_diff_density_rms 0.175