# Copyright The Royal Society of Chemistry, 1998 data_zgf125 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common (+)-(Rp,S)-4 _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C17 H21 Br Fe N2 O Pd' _chemical_formula_weight 511.52 _chemical_melting_point ? _chemical_compound_source synthesized 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' 'Fe' 'Fe' 0.3463 0.8444 '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 8.296(2) _cell_length_b 13.865(3) _cell_length_c 15.585(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1792.6(7) _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 block _exptl_crystal_colour red _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.895 _exptl_crystal_density_method ? _exptl_crystal_F_000 1008 _exptl_absorpt_coefficient_mu 4.045 _exptl_absorpt_correction_type 'ABSCOR' _exptl_absorpt_correction_T_min 0.807 _exptl_absorpt_correction_T_max 1.165 _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 'IP Rigaku' _diffrn_measurement_method 'IP' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6054 _diffrn_reflns_av_R_equivalents 0.0465 _diffrn_reflns_av_sigmaI/netI 0.0630 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.61 _diffrn_reflns_theta_max 25.56 _reflns_number_total 3291 _reflns_number_observed 3183 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'RAXIS Rigaku' _computing_cell_refinement 'BIOTEX Rigaku' _computing_data_reduction 'BIOTEX Rigaku' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'XP Siemens' _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^)+(0.0357P)^2^+0.3172P] 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 SHELXL _refine_ls_extinction_coef 0.0071(2) _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 0.440(8) _refine_ls_number_reflns 3291 _refine_ls_number_parameters 210 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0393 _refine_ls_R_factor_obs 0.0377 _refine_ls_wR_factor_all 0.0911 _refine_ls_wR_factor_obs 0.0899 _refine_ls_goodness_of_fit_all 1.037 _refine_ls_goodness_of_fit_obs 1.042 _refine_ls_restrained_S_all 1.037 _refine_ls_restrained_S_obs 1.042 _refine_ls_shift/esd_max 0.055 _refine_ls_shift/esd_mean 0.002 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Pd1 Pd 0.24069(2) 0.189824(11) 0.145031(11) 0.05680(5) Uani 1 d . . Fe1 Fe 0.47136(4) 0.28150(2) 0.31071(2) 0.05125(8) Uani 1 d . . Br1 Br -0.01563(3) 0.21277(3) 0.21584(3) 0.10319(13) Uani 1 d . . O1 O 0.1712(2) 0.05513(13) 0.07643(14) 0.0813(6) Uani 1 d . . N1 N 0.4693(2) 0.18164(12) 0.09483(11) 0.0519(5) Uani 1 d . . N2 N 0.5134(2) 0.10287(12) 0.04525(13) 0.0599(5) Uani 1 d . . C1 C 0.3347(3) 0.29983(15) 0.2030(2) 0.0557(6) Uani 1 d . . C2 C 0.5057(3) 0.3106(2) 0.18396(14) 0.0545(6) Uani 1 d . . C3 C 0.5681(3) 0.3870(2) 0.2353(2) 0.0674(7) Uani 1 d . . H3 H 0.6745(3) 0.4083(2) 0.2360(2) 0.081 Uiso 1 calc R . C4 C 0.4413(4) 0.4247(2) 0.2846(2) 0.0743(8) Uani 1 d . . H4 H 0.4489(4) 0.4752(2) 0.3236(2) 0.089 Uiso 1 calc R . C5 C 0.2983(3) 0.3716(2) 0.2643(2) 0.0696(8) Uani 1 d . . H5 H 0.1970(3) 0.3826(2) 0.2879(2) 0.084 Uiso 1 calc R . C6 C 0.6426(4) 0.2309(2) 0.3958(2) 0.0798(9) Uani 1 d . . H6 H 0.7466(4) 0.2547(2) 0.4027(2) 0.096 Uiso 1 calc R . C7 C 0.5023(4) 0.2614(2) 0.4404(2) 0.0766(8) Uani 1 d . . H7 H 0.4981(4) 0.3081(2) 0.4832(2) 0.092 Uiso 1 calc R . C8 C 0.3701(4) 0.2078(2) 0.4082(2) 0.0812(9) Uani 1 d . . H8 H 0.2631(4) 0.2144(2) 0.4251(2) 0.097 Uiso 1 calc R . C9 C 0.4293(4) 0.1424(2) 0.3457(2) 0.0769(9) Uani 1 d . . H9 H 0.3682(4) 0.0978(2) 0.3152(2) 0.092 Uiso 1 calc R . C10 C 0.5929(4) 0.1565(2) 0.3381(2) 0.0750(9) Uani 1 d . . H10 H 0.6606(4) 0.1229(2) 0.3011(2) 0.090 Uiso 1 calc R . C11 C 0.5729(3) 0.2407(2) 0.12687(14) 0.0528(6) Uani 1 d . . H11 H 0.6823(3) 0.2381(2) 0.11395(14) 0.063 Uiso 1 calc R . C12 C 0.3969(4) 0.0784(2) -0.0209(2) 0.0754(9) Uani 1 d . . H12 H 0.3458(4) 0.1373(2) -0.0426(2) 0.091 Uiso 1 calc R . C13 C 0.4959(5) 0.0314(2) -0.0922(2) 0.1018(13) Uani 1 d . . H13A H 0.4514(5) -0.0310(2) -0.1075(2) 0.122 Uiso 1 calc R . H13B H 0.4982(5) 0.0719(2) -0.1429(2) 0.122 Uiso 1 calc R . C14 C 0.6635(5) 0.0204(2) -0.0546(2) 0.1082(12) Uani 1 d . . H14A H 0.7451(5) 0.0255(2) -0.0989(2) 0.130 Uiso 1 calc R . H14B H 0.6750(5) -0.0412(2) -0.0258(2) 0.130 Uiso 1 calc R . C15 C 0.6771(4) 0.1034(2) 0.0090(2) 0.0778(9) Uani 1 d . . H15A H 0.7581(4) 0.0908(2) 0.0525(2) 0.093 Uiso 1 calc R . H15B H 0.7012(4) 0.1639(2) -0.0195(2) 0.093 Uiso 1 calc R . C16 C 0.2685(5) 0.0101(2) 0.0134(2) 0.0892(10) Uani 1 d . . H16A H 0.2010(5) -0.0116(2) -0.0336(2) 0.107 Uiso 1 calc R . H16B H 0.3203(5) -0.0461(2) 0.0382(2) 0.107 Uiso 1 calc R . C17 C 0.0582(4) -0.0126(2) 0.1133(3) 0.1052(14) Uani 1 d . . H17A H -0.0063(4) 0.0195(2) 0.1557(3) 0.158 Uiso 1 calc R . H17B H 0.1162(4) -0.0647(2) 0.1396(3) 0.158 Uiso 1 calc R . H17C H -0.0104(4) -0.0377(2) 0.0689(3) 0.158 Uiso 1 calc R . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.04515(7) 0.05938(9) 0.06585(11) -0.00422(7) -0.00748(8) 0.00170(8) Fe1 0.05740(15) 0.04565(13) 0.0507(2) -0.00037(12) -0.00102(14) -0.00134(13) Br1 0.04597(11) 0.1291(3) 0.1345(3) -0.0221(2) 0.0092(2) 0.0011(2) O1 0.0749(10) 0.0659(9) 0.1032(14) -0.0109(10) -0.0149(10) -0.0159(9) N1 0.0626(10) 0.0468(8) 0.0463(9) 0.0022(7) -0.0004(8) 0.0042(9) N2 0.0695(11) 0.0522(9) 0.0580(11) -0.0001(8) 0.0060(10) 0.0101(9) C1 0.0578(11) 0.0508(11) 0.0584(13) 0.0011(10) -0.0033(10) 0.0088(10) C2 0.0595(10) 0.0498(9) 0.0543(11) 0.0039(10) -0.0034(10) -0.0061(10) C3 0.0788(14) 0.0505(11) 0.073(2) 0.0097(11) -0.0132(13) -0.0190(12) C4 0.103(2) 0.0499(11) 0.070(2) -0.0055(11) -0.0118(15) 0.0044(14) C5 0.076(2) 0.0613(12) 0.072(2) -0.0053(12) -0.0051(13) 0.0148(12) C6 0.087(2) 0.085(2) 0.067(2) 0.0147(14) -0.0189(14) 0.000(2) C7 0.109(2) 0.0676(13) 0.0527(13) -0.0029(12) -0.0069(15) -0.003(2) C8 0.092(2) 0.074(2) 0.078(2) 0.0079(15) 0.015(2) -0.012(2) C9 0.114(2) 0.0500(11) 0.066(2) 0.0041(12) 0.005(2) -0.0150(14) C10 0.100(2) 0.0630(13) 0.062(2) 0.0123(12) -0.0029(14) 0.0152(14) C11 0.0504(10) 0.0534(10) 0.0547(13) 0.0045(10) 0.0051(9) -0.0020(10) C12 0.106(2) 0.0604(13) 0.060(2) -0.0049(11) -0.0097(15) 0.0053(15) C13 0.158(3) 0.084(2) 0.063(2) -0.0132(14) 0.016(2) -0.004(3) C14 0.162(3) 0.067(2) 0.095(2) -0.006(2) 0.049(2) 0.017(2) C15 0.086(2) 0.0749(15) 0.073(2) -0.0006(14) 0.0245(13) 0.0153(14) C16 0.102(2) 0.0642(13) 0.101(2) -0.0246(13) -0.021(2) -0.003(2) C17 0.072(2) 0.079(2) 0.165(4) 0.008(2) -0.011(2) -0.015(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 1.937(2) . ? Pd1 N1 2.055(2) . ? Pd1 O1 2.228(2) . ? Pd1 Br1 2.4167(6) . ? Fe1 C8 2.015(3) . ? Fe1 C9 2.035(2) . ? Fe1 C5 2.035(3) . ? Fe1 C2 2.036(2) . ? Fe1 C3 2.041(2) . ? Fe1 C4 2.041(2) . ? Fe1 C1 2.041(2) . ? Fe1 C10 2.050(3) . ? Fe1 C7 2.057(3) . ? Fe1 C6 2.066(3) . ? O1 C16 1.417(4) . ? O1 C17 1.446(4) . ? N1 C11 1.288(3) . ? N1 N2 1.387(2) . ? N2 C12 1.453(4) . ? N2 C15 1.471(4) . ? C1 C5 1.412(3) . ? C1 C2 1.457(3) . ? C2 C3 1.425(3) . ? C2 C11 1.429(3) . ? C3 C4 1.403(4) . ? C4 C5 1.432(4) . ? C6 C7 1.420(4) . ? C6 C10 1.430(4) . ? C7 C8 1.416(4) . ? C8 C9 1.419(4) . ? C9 C10 1.376(4) . ? C12 C16 1.523(4) . ? C12 C13 1.527(5) . ? C13 C14 1.516(6) . ? C14 C15 1.522(4) . ? 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 81.34(8) . . ? C1 Pd1 O1 171.21(8) . . ? N1 Pd1 O1 90.56(7) . . ? C1 Pd1 Br1 92.16(7) . . ? N1 Pd1 Br1 173.35(5) . . ? O1 Pd1 Br1 95.84(5) . . ? C8 Fe1 C9 41.04(11) . . ? C8 Fe1 C5 106.53(12) . . ? C9 Fe1 C5 123.77(12) . . ? C8 Fe1 C2 152.95(11) . . ? C9 Fe1 C2 118.16(10) . . ? C5 Fe1 C2 68.45(10) . . ? C8 Fe1 C3 164.09(11) . . ? C9 Fe1 C3 154.34(11) . . ? C5 Fe1 C3 68.48(11) . . ? C2 Fe1 C3 40.92(9) . . ? C8 Fe1 C4 126.32(12) . . ? C9 Fe1 C4 162.60(13) . . ? C5 Fe1 C4 41.12(11) . . ? C2 Fe1 C4 68.35(10) . . ? C3 Fe1 C4 40.20(11) . . ? C8 Fe1 C1 116.86(11) . . ? C9 Fe1 C1 104.07(10) . . ? C5 Fe1 C1 40.54(9) . . ? C2 Fe1 C1 41.87(9) . . ? C3 Fe1 C1 69.87(10) . . ? C4 Fe1 C1 69.35(10) . . ? C8 Fe1 C10 67.65(12) . . ? C9 Fe1 C10 39.39(12) . . ? C5 Fe1 C10 159.96(11) . . ? C2 Fe1 C10 107.48(10) . . ? C3 Fe1 C10 122.16(11) . . ? C4 Fe1 C10 157.45(12) . . ? C1 Fe1 C10 123.32(10) . . ? C8 Fe1 C7 40.69(12) . . ? C9 Fe1 C7 68.24(11) . . ? C5 Fe1 C7 121.35(11) . . ? C2 Fe1 C7 164.35(11) . . ? C3 Fe1 C7 127.89(11) . . ? C4 Fe1 C7 110.07(11) . . ? C1 Fe1 C7 153.43(11) . . ? C10 Fe1 C7 67.64(11) . . ? C8 Fe1 C6 68.32(13) . . ? C9 Fe1 C6 67.91(12) . . ? C5 Fe1 C6 157.10(11) . . ? C2 Fe1 C6 126.42(11) . . ? C3 Fe1 C6 110.03(12) . . ? C4 Fe1 C6 122.82(12) . . ? C1 Fe1 C6 162.14(11) . . ? C10 Fe1 C6 40.65(12) . . ? C7 Fe1 C6 40.30(12) . . ? C16 O1 C17 111.0(2) . . ? C16 O1 Pd1 123.7(2) . . ? C17 O1 Pd1 121.5(2) . . ? C11 N1 N2 122.8(2) . . ? C11 N1 Pd1 115.67(14) . . ? N2 N1 Pd1 119.92(14) . . ? N1 N2 C12 113.8(2) . . ? N1 N2 C15 117.0(2) . . ? C12 N2 C15 110.0(2) . . ? C5 C1 C2 105.9(2) . . ? C5 C1 Pd1 141.7(2) . . ? C2 C1 Pd1 112.2(2) . . ? C5 C1 Fe1 69.50(14) . . ? C2 C1 Fe1 68.87(12) . . ? Pd1 C1 Fe1 120.61(11) . . ? C3 C2 C11 135.4(2) . . ? C3 C2 C1 108.4(2) . . ? C11 C2 C1 115.9(2) . . ? C3 C2 Fe1 69.73(14) . . ? C11 C2 Fe1 121.6(2) . . ? C1 C2 Fe1 69.26(13) . . ? C4 C3 C2 108.1(2) . . ? C4 C3 Fe1 69.91(15) . . ? C2 C3 Fe1 69.35(13) . . ? C3 C4 C5 108.0(2) . . ? C3 C4 Fe1 69.89(14) . . ? C5 C4 Fe1 69.22(14) . . ? C1 C5 C4 109.5(2) . . ? C1 C5 Fe1 69.96(14) . . ? C4 C5 Fe1 69.66(15) . . ? C7 C6 C10 106.7(3) . . ? C7 C6 Fe1 69.5(2) . . ? C10 C6 Fe1 69.1(2) . . ? C8 C7 C6 107.8(2) . . ? C8 C7 Fe1 68.1(2) . . ? C6 C7 Fe1 70.2(2) . . ? C7 C8 C9 108.1(3) . . ? C7 C8 Fe1 71.3(2) . . ? C9 C8 Fe1 70.2(2) . . ? C10 C9 C8 108.1(3) . . ? C10 C9 Fe1 70.9(2) . . ? C8 C9 Fe1 68.73(15) . . ? C9 C10 C6 109.4(3) . . ? C9 C10 Fe1 69.7(2) . . ? C6 C10 Fe1 70.3(2) . . ? N1 C11 C2 114.4(2) . . ? N2 C12 C16 111.1(2) . . ? N2 C12 C13 105.0(3) . . ? C16 C12 C13 111.5(2) . . ? C14 C13 C12 104.8(3) . . ? C13 C14 C15 104.1(3) . . ? N2 C15 C14 100.2(3) . . ? O1 C16 C12 111.6(2) . . ? _refine_diff_density_max 0.433 _refine_diff_density_min -0.492 _refine_diff_density_rms 0.077 #=END data_zgf65 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common syn-(-)-(Sp,R,R,Sp)-5 _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C36 H46 Br2 Fe2 N4 O2 Pd2' _chemical_formula_weight 1051.09 _chemical_melting_point ? _chemical_compound_source synthesized 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' 'Fe' 'Fe' 0.3463 0.8444 '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 monoclinic _symmetry_space_group_name_H-M P2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 12.8720(10) _cell_length_b 11.2960(10) _cell_length_c 13.3370(10) _cell_angle_alpha 90.00 _cell_angle_beta 96.370(10) _cell_angle_gamma 90.00 _cell_volume 1927.3(3) _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 plate _exptl_crystal_colour red _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.811 _exptl_crystal_density_method ? _exptl_crystal_F_000 1040 _exptl_absorpt_coefficient_mu 3.766 _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 'RIGAKU RXAIS II' _diffrn_measurement_method 'IP' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6579 _diffrn_reflns_av_R_equivalents 0.0609 _diffrn_reflns_av_sigmaI/netI 0.0645 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.33 _diffrn_reflns_theta_max 25.54 _reflns_number_total 6458 _reflns_number_observed 6337 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'R-AXIS' _computing_cell_refinement 'BIOTEX' _computing_data_reduction 'BIOTEX' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'SIEMENS SHELXL PC' _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 1 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^)+(0.1178P)^2^+0.4703P] 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 refxyz _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0256(5) _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 0.641(6) _refine_ls_number_reflns 6457 _refine_ls_number_parameters 435 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0560 _refine_ls_R_factor_obs 0.0551 _refine_ls_wR_factor_all 0.1586 _refine_ls_wR_factor_obs 0.1555 _refine_ls_goodness_of_fit_all 1.004 _refine_ls_goodness_of_fit_obs 1.006 _refine_ls_restrained_S_all 1.016 _refine_ls_restrained_S_obs 1.006 _refine_ls_shift/esd_max 1.566 _refine_ls_shift/esd_mean 0.020 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 0.37106(2) 0.22825(2) 0.61664(2) 0.05872(6) Uani 1 d . . Pd2 Pd 0.36209(2) 0.30461(2) 0.85808(2) 0.05761(6) Uani 1 d . . Fe1 Fe 0.12951(4) 0.13241(5) 0.48939(4) 0.0752(2) Uani 1 d . . Fe2 Fe 0.33900(4) 0.05352(4) 1.01075(4) 0.06622(13) Uani 1 d . . Br1 Br 0.50764(3) 0.23081(4) 0.77374(3) 0.07624(10) Uani 1 d . . Br2 Br 0.30600(3) 0.41160(3) 0.68801(3) 0.07288(9) Uani 1 d . . O1 O 0.3325(3) -0.1590(3) 0.6388(3) 0.1118(12) Uani 1 d . . O2 O -0.0571(2) 0.3152(5) 0.7859(3) 0.1203(13) Uani 1 d . . N1 N 0.4111(2) 0.0747(3) 0.5403(2) 0.0663(7) Uani 1 d . . N2 N 0.4979(2) -0.0001(3) 0.5681(2) 0.0758(9) Uani 1 d . . N3 N 0.2484(2) 0.3557(3) 0.9511(2) 0.0623(7) Uani 1 d . . N4 N 0.1678(2) 0.4413(3) 0.9329(2) 0.0666(8) Uani 1 d . . C1 C 0.2631(3) 0.2300(3) 0.5014(2) 0.0648(8) Uani 1 d . . C2 C 0.2688(3) 0.1340(3) 0.4334(3) 0.0680(9) Uani 1 d . . C3 C 0.1849(3) 0.1423(5) 0.3526(3) 0.0854(13) Uani 1 d . . H3 H 0.1699(3) 0.0894(5) 0.2995(3) 0.102 Uiso 1 calc R . C4 C 0.1292(3) 0.2485(5) 0.3708(3) 0.0882(13) Uani 1 d . . H4 H 0.0722(3) 0.2783(5) 0.3294(3) 0.106 Uiso 1 calc R . C5 C 0.1739(3) 0.3001(4) 0.4604(3) 0.0761(10) Uani 1 d . . H5 H 0.1502(3) 0.3685(4) 0.4893(3) 0.091 Uiso 1 calc R . C6 C -0.0108(8) 0.0502(13) 0.4914(7) 0.425(4) Uani 1 d . . H6 H -0.0599(8) 0.0433(13) 0.4350(7) 0.510 Uiso 1 calc R . C7 C 0.0723(6) -0.0303(7) 0.5196(6) 0.201(3) Uani 1 d . . H7 H 0.0890(6) -0.0996(7) 0.4873(6) 0.242 Uiso 1 calc R . C8 C 0.1211(4) 0.0183(5) 0.6048(4) 0.111(2) Uani 1 d . . H8 H 0.1792(4) -0.0126(5) 0.6436(4) 0.133 Uiso 1 calc R . C9 C 0.0739(6) 0.1135(7) 0.6227(5) 0.183(2) Uani 1 d . . H9 H 0.0913(6) 0.1659(7) 0.6756(5) 0.219 Uiso 1 calc R . C10 C -0.0072(4) 0.1230(7) 0.5483(6) 0.330(2) Uani 1 d . . H10 H -0.0553(4) 0.1847(7) 0.5452(6) 0.396 Uiso 1 calc R . C11 C 0.3516(3) 0.0483(3) 0.4589(2) 0.0686(9) Uani 1 d . . C12 C 0.3690(4) -0.0567(4) 0.3945(3) 0.0958(14) Uani 1 d . . H12A H 0.4274(4) -0.1015(4) 0.4252(3) 0.144 Uiso 1 calc R . H12B H 0.3832(4) -0.0303(4) 0.3289(3) 0.144 Uiso 1 calc R . H12C H 0.3076(4) -0.1055(4) 0.3879(3) 0.144 Uiso 1 calc R . C13 C 0.4964(4) -0.0594(4) 0.6648(3) 0.0861(12) Uani 1 d . . H13 H 0.4644(4) -0.0066(4) 0.7109(3) 0.103 Uiso 1 calc R . C14 C 0.6090(4) -0.0785(6) 0.7045(4) 0.119(2) Uani 1 d . . H14A H 0.6188(4) -0.0709(6) 0.7774(4) 0.142 Uiso 1 calc R . H14B H 0.6322(4) -0.1566(6) 0.6863(4) 0.142 Uiso 1 calc R . C15 C 0.6675(4) 0.0152(7) 0.6563(5) 0.127(2) Uani 1 d . . H15A H 0.7305(4) -0.0175(7) 0.6335(5) 0.152 Uiso 1 calc R . H15B H 0.6873(4) 0.0781(7) 0.7042(5) 0.152 Uiso 1 calc R . C16 C 0.5966(3) 0.0628(4) 0.5679(3) 0.0861(12) Uani 1 d . . H16A H 0.5862(3) 0.1472(4) 0.5752(3) 0.103 Uiso 1 calc R . H16B H 0.6264(3) 0.0486(4) 0.5053(3) 0.103 Uiso 1 calc R . C17 C 0.4377(4) -0.1774(4) 0.6587(4) 0.0946(14) Uani 1 d . . H17A H 0.4618(4) -0.2259(4) 0.6058(4) 0.114 Uiso 1 calc R . H17B H 0.4522(4) -0.2195(4) 0.7221(4) 0.114 Uiso 1 calc R . C18 C 0.2734(5) -0.2616(5) 0.6540(6) 0.152(3) Uani 1 d . . H18A H 0.2003(5) -0.2442(5) 0.6390(6) 0.228 Uiso 1 calc R . H18B H 0.2872(5) -0.2866(5) 0.7229(6) 0.228 Uiso 1 calc R . H18C H 0.2925(5) -0.3236(5) 0.6103(6) 0.228 Uiso 1 calc R . C19 C 0.4075(2) 0.2115(3) 0.9772(2) 0.0656(9) Uani 1 d . . C20 C 0.3392(3) 0.2227(4) 1.0563(2) 0.0670(9) Uani 1 d . . C21 C 0.3771(3) 0.1486(4) 1.1392(3) 0.0736(10) Uani 1 d . . H21 H 0.3480(3) 0.1414(4) 1.1997(3) 0.088 Uiso 1 calc R . C22 C 0.4653(3) 0.0889(4) 1.1135(3) 0.0783(11) Uani 1 d . . H22 H 0.5050(3) 0.0346(4) 1.1538(3) 0.094 Uiso 1 calc R . C23 C 0.4842(3) 0.1261(3) 1.0129(3) 0.0691(10) Uani 1 d . . H23 H 0.5377(3) 0.0987(3) 0.9775(3) 0.083 Uiso 1 calc R . C24 C 0.3173(4) -0.1269(4) 1.0131(4) 0.102(2) Uani 1 d . . H24 H 0.3557(4) -0.1806(4) 1.0551(4) 0.122 Uiso 1 calc R . C25 C 0.2260(5) -0.0653(5) 1.0351(5) 0.123(2) Uani 1 d . . H25 H 0.1925(5) -0.0677(5) 1.0934(5) 0.148 Uiso 1 calc R . C26 C 0.1973(4) 0.0057(5) 0.9387(6) 0.159(3) Uani 1 d . . H26 H 0.1401(4) 0.0556(5) 0.9242(6) 0.191 Uiso 1 calc R . C27 C 0.2714(5) -0.0188(6) 0.8797(5) 0.138(2) Uani 1 d . . H27 H 0.2743(5) 0.0146(6) 0.8163(5) 0.166 Uiso 1 calc R . C28 C 0.3383(5) -0.0935(6) 0.9198(5) 0.134(2) Uani 1 d . . H28 H 0.3946(5) -0.1214(6) 0.8887(5) 0.160 Uiso 1 calc R . C29 C 0.2511(3) 0.3007(3) 1.0375(2) 0.0677(9) Uani 1 d . . C30 C 0.1748(3) 0.3220(4) 1.1103(3) 0.0824(12) Uani 1 d . . H30A H 0.1227(3) 0.3770(4) 1.0820(3) 0.124 Uiso 1 calc R . H30B H 0.2102(3) 0.3542(4) 1.1714(3) 0.124 Uiso 1 calc R . H30C H 0.1418(3) 0.2487(4) 1.1249(3) 0.124 Uiso 1 calc R . C31 C 0.0944(3) 0.4199(4) 0.8435(3) 0.0782(11) Uani 1 d . . H31 H 0.1318(3) 0.3963(4) 0.7865(3) 0.094 Uiso 1 calc R . C32 C 0.0437(4) 0.5418(5) 0.8241(4) 0.118(2) Uani 1 d . . H32A H 0.0325(4) 0.5577(5) 0.7522(4) 0.141 Uiso 1 calc R . H32B H -0.0233(4) 0.5446(5) 0.8508(4) 0.141 Uiso 1 calc R . C33 C 0.1172(4) 0.6322(5) 0.8761(5) 0.114(2) Uani 1 d . . H33A H 0.0857(4) 0.6706(5) 0.9304(5) 0.136 Uiso 1 calc R . H33B H 0.1349(4) 0.6921(5) 0.8288(5) 0.136 Uiso 1 calc R . C34 C 0.2144(3) 0.5621(4) 0.9176(3) 0.0857(12) Uani 1 d . . H34A H 0.2657(3) 0.5592(4) 0.8695(3) 0.103 Uiso 1 calc R . H34B H 0.2465(3) 0.5951(4) 0.9807(3) 0.103 Uiso 1 calc R . C35 C 0.0173(3) 0.3252(5) 0.8658(4) 0.097(2) Uani 1 d . . H35A H 0.0532(3) 0.2502(5) 0.8780(4) 0.117 Uiso 1 calc R . H35B H -0.0149(3) 0.3462(5) 0.9258(4) 0.117 Uiso 1 calc R . C36 C -0.1146(5) 0.2056(7) 0.8004(6) 0.225(3) Uani 1 d . . H36A H -0.1683(5) 0.1952(7) 0.7452(6) 0.337 Uiso 1 calc R . H36B H -0.1457(5) 0.2103(7) 0.8624(6) 0.337 Uiso 1 calc R . H36C H -0.0673(5) 0.1397(7) 0.8032(6) 0.337 Uiso 1 calc R . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.06802(11) 0.04599(10) 0.06363(11) -0.00179(9) 0.01386(9) -0.00018(9) Pd2 0.06372(10) 0.04666(10) 0.06339(11) 0.00086(8) 0.01125(8) -0.00129(9) Fe1 0.0772(3) 0.0737(3) 0.0745(3) 0.0090(2) 0.0085(2) -0.0078(2) Fe2 0.0681(2) 0.0579(2) 0.0715(2) 0.0083(2) 0.0030(2) -0.0014(2) Br1 0.0735(2) 0.0763(2) 0.0802(2) -0.0118(2) 0.01384(14) 0.0019(2) Br2 0.1013(2) 0.04983(14) 0.0698(2) 0.00224(12) 0.01974(14) 0.00991(14) O1 0.118(2) 0.0595(15) 0.160(3) 0.027(2) 0.022(2) -0.007(2) O2 0.086(2) 0.147(3) 0.126(2) -0.030(2) 0.005(2) -0.019(2) N1 0.0778(14) 0.0576(13) 0.0652(13) -0.0017(11) 0.0154(11) 0.0110(12) N2 0.084(2) 0.0600(15) 0.084(2) 0.0017(13) 0.0158(13) 0.0137(13) N3 0.0629(12) 0.0637(13) 0.0604(12) 0.0061(11) 0.0070(10) 0.0033(12) N4 0.0693(13) 0.0648(14) 0.0653(14) 0.0080(12) 0.0063(11) 0.0076(12) C1 0.083(2) 0.0519(14) 0.0613(14) -0.0002(13) 0.0153(12) -0.0072(15) C2 0.081(2) 0.063(2) 0.059(2) 0.0060(13) 0.0063(13) -0.007(2) C3 0.082(2) 0.102(3) 0.071(2) -0.008(2) 0.004(2) -0.007(2) C4 0.088(2) 0.100(3) 0.076(2) 0.015(2) 0.008(2) 0.009(2) C5 0.080(2) 0.066(2) 0.084(2) 0.009(2) 0.0142(15) 0.006(2) C6 0.318(6) 0.712(10) 0.204(5) 0.289(5) -0.158(4) -0.367(6) C7 0.335(6) 0.116(4) 0.178(4) -0.007(3) 0.142(4) -0.101(4) C8 0.133(3) 0.115(3) 0.084(2) 0.029(2) 0.011(2) -0.034(3) C9 0.280(4) 0.133(5) 0.164(3) -0.040(3) 0.157(2) -0.070(4) C10 0.122(2) 0.357(4) 0.547(5) 0.382(3) 0.201(2) 0.135(3) C11 0.088(2) 0.059(2) 0.0613(14) -0.0008(13) 0.0191(13) 0.002(2) C12 0.120(3) 0.085(2) 0.080(2) -0.022(2) 0.002(2) 0.015(2) C13 0.108(2) 0.066(2) 0.084(2) 0.005(2) 0.008(2) 0.020(2) C14 0.120(3) 0.125(4) 0.108(3) 0.015(3) 0.002(3) 0.038(3) C15 0.087(3) 0.147(5) 0.146(5) -0.007(4) 0.009(3) 0.024(3) C16 0.080(2) 0.080(2) 0.103(2) 0.000(2) 0.028(2) 0.015(2) C17 0.125(3) 0.055(2) 0.106(3) 0.002(2) 0.022(2) 0.018(2) C18 0.161(5) 0.066(2) 0.237(6) 0.041(3) 0.058(4) -0.016(3) C19 0.067(2) 0.063(2) 0.066(2) -0.0017(13) 0.0067(13) -0.0074(14) C20 0.068(2) 0.067(2) 0.064(2) 0.0014(15) -0.0008(12) 0.002(2) C21 0.083(2) 0.078(2) 0.0588(15) 0.0133(15) 0.0035(14) 0.001(2) C22 0.078(2) 0.072(2) 0.079(2) 0.010(2) -0.018(2) 0.007(2) C23 0.0601(14) 0.057(2) 0.089(2) 0.0056(15) 0.0051(14) 0.0022(14) C24 0.107(3) 0.062(2) 0.130(4) 0.004(2) -0.010(3) -0.004(2) C25 0.138(3) 0.093(3) 0.142(4) -0.002(3) 0.035(3) -0.051(3) C26 0.078(2) 0.080(3) 0.298(7) -0.002(4) -0.076(3) -0.004(2) C27 0.178(4) 0.115(4) 0.107(3) 0.025(3) -0.050(3) -0.032(4) C28 0.148(4) 0.130(4) 0.125(4) -0.045(3) 0.028(3) -0.053(3) C29 0.081(2) 0.062(2) 0.061(2) 0.0023(14) 0.0088(13) 0.004(2) C30 0.087(2) 0.096(3) 0.066(2) 0.003(2) 0.013(2) 0.005(2) C31 0.074(2) 0.091(2) 0.067(2) -0.002(2) -0.0004(15) 0.010(2) C32 0.116(3) 0.096(3) 0.132(4) 0.022(3) -0.027(3) 0.025(3) C33 0.117(3) 0.077(3) 0.146(4) 0.011(3) 0.011(3) 0.025(2) C34 0.096(2) 0.071(2) 0.089(2) 0.002(2) 0.005(2) 0.017(2) C35 0.067(2) 0.115(4) 0.113(3) -0.012(3) 0.021(2) -0.004(2) C36 0.190(4) 0.236(5) 0.273(5) -0.173(4) 0.135(4) -0.135(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 C1 1.955(3) . ? Pd1 N1 2.104(3) . ? Pd1 Br2 2.4646(4) . ? Pd1 Br1 2.5815(5) . ? Pd2 C19 1.941(3) . ? Pd2 N3 2.102(3) . ? Pd2 Br1 2.4368(5) . ? Pd2 Br2 2.6006(4) . ? Fe1 C9 2.000(6) . ? Fe1 C10 2.008(6) . ? Fe1 C2 2.018(4) . ? Fe1 C8 2.019(5) . ? Fe1 C5 2.027(4) . ? Fe1 C3 2.034(4) . ? Fe1 C1 2.034(3) . ? Fe1 C6 2.034(11) . ? Fe1 C7 2.037(7) . ? Fe1 C4 2.054(5) . ? Fe2 C20 2.005(4) . ? Fe2 C25 2.032(6) . ? Fe2 C21 2.035(4) . ? Fe2 C27 2.035(6) . ? Fe2 C26 2.038(5) . ? Fe2 C23 2.038(4) . ? Fe2 C22 2.046(4) . ? Fe2 C28 2.055(7) . ? Fe2 C24 2.058(5) . ? Fe2 C19 2.062(4) . ? O1 C17 1.367(6) . ? O1 C18 1.413(7) . ? O2 C35 1.356(6) . ? O2 C36 1.466(9) . ? N1 C11 1.293(4) . ? N1 N2 1.417(4) . ? N2 C16 1.455(5) . ? N2 C13 1.455(5) . ? N3 C29 1.306(4) . ? N3 N4 1.419(4) . ? N4 C31 1.457(4) . ? N4 C34 1.514(5) . ? C1 C2 1.421(5) . ? C1 C5 1.451(5) . ? C2 C3 1.442(5) . ? C2 C11 1.452(5) . ? C3 C4 1.432(7) . ? C4 C5 1.396(6) . ? C6 C10 1.117(15) . ? C6 C7 1.422(15) . ? C7 C8 1.352(9) . ? C8 C9 1.270(10) . ? C9 C10 1.362(9) . ? C11 C12 1.496(6) . ? C13 C14 1.502(7) . ? C13 C17 1.530(6) . ? C14 C15 1.486(10) . ? C15 C16 1.508(8) . ? C19 C23 1.423(5) . ? C19 C20 1.452(5) . ? C20 C21 1.429(5) . ? C20 C29 1.436(5) . ? C21 C22 1.396(6) . ? C22 C23 1.453(6) . ? C24 C28 1.355(9) . ? C24 C25 1.425(8) . ? C25 C26 1.526(10) . ? C26 C27 1.332(10) . ? C27 C28 1.279(9) . ? C29 C30 1.475(5) . ? C31 C35 1.511(7) . ? C31 C32 1.534(7) . ? C32 C33 1.508(8) . ? C33 C34 1.532(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 N1 79.58(12) . . ? C1 Pd1 Br2 93.02(10) . . ? N1 Pd1 Br2 172.60(7) . . ? C1 Pd1 Br1 177.33(10) . . ? N1 Pd1 Br1 102.73(7) . . ? Br2 Pd1 Br1 84.671(14) . . ? C19 Pd2 N3 80.30(12) . . ? C19 Pd2 Br1 90.88(10) . . ? N3 Pd2 Br1 171.04(7) . . ? C19 Pd2 Br2 174.38(11) . . ? N3 Pd2 Br2 104.09(7) . . ? Br1 Pd2 Br2 84.82(2) . . ? C9 Fe1 C10 39.7(3) . . ? C9 Fe1 C2 138.6(2) . . ? C10 Fe1 C2 177.1(2) . . ? C9 Fe1 C8 36.8(3) . . ? C10 Fe1 C8 62.9(3) . . ? C2 Fe1 C8 114.4(2) . . ? C9 Fe1 C5 113.9(3) . . ? C10 Fe1 C5 113.7(2) . . ? C2 Fe1 C5 68.93(15) . . ? C8 Fe1 C5 141.4(2) . . ? C9 Fe1 C3 177.0(3) . . ? C10 Fe1 C3 139.8(2) . . ? C2 Fe1 C3 41.69(14) . . ? C8 Fe1 C3 140.6(2) . . ? C5 Fe1 C3 69.1(2) . . ? C9 Fe1 C1 111.7(2) . . ? C10 Fe1 C1 140.2(2) . . ? C2 Fe1 C1 41.06(14) . . ? C8 Fe1 C1 113.7(2) . . ? C5 Fe1 C1 41.86(14) . . ? C3 Fe1 C1 70.35(15) . . ? C9 Fe1 C6 62.2(3) . . ? C10 Fe1 C6 32.1(4) . . ? C2 Fe1 C6 146.7(4) . . ? C8 Fe1 C6 64.9(3) . . ? C5 Fe1 C6 134.3(4) . . ? C3 Fe1 C6 115.9(3) . . ? C1 Fe1 C6 172.2(4) . . ? C9 Fe1 C7 63.6(3) . . ? C10 Fe1 C7 61.5(3) . . ? C2 Fe1 C7 115.9(3) . . ? C8 Fe1 C7 38.9(3) . . ? C5 Fe1 C7 175.0(3) . . ? C3 Fe1 C7 113.4(3) . . ? C1 Fe1 C7 142.6(2) . . ? C6 Fe1 C7 40.9(4) . . ? C9 Fe1 C4 141.5(3) . . ? C10 Fe1 C4 114.1(2) . . ? C2 Fe1 C4 68.6(2) . . ? C8 Fe1 C4 176.8(2) . . ? C5 Fe1 C4 40.0(2) . . ? C3 Fe1 C4 41.0(2) . . ? C1 Fe1 C4 69.17(15) . . ? C6 Fe1 C4 112.1(3) . . ? C7 Fe1 C4 139.3(3) . . ? C20 Fe2 C25 123.9(2) . . ? C20 Fe2 C21 41.41(15) . . ? C25 Fe2 C21 108.9(2) . . ? C20 Fe2 C27 129.0(2) . . ? C25 Fe2 C27 68.1(3) . . ? C21 Fe2 C27 167.1(2) . . ? C20 Fe2 C26 111.5(2) . . ? C25 Fe2 C26 44.0(3) . . ? C21 Fe2 C26 131.0(2) . . ? C27 Fe2 C26 38.2(3) . . ? C20 Fe2 C23 69.02(14) . . ? C25 Fe2 C23 159.3(2) . . ? C21 Fe2 C23 69.0(2) . . ? C27 Fe2 C23 118.5(2) . . ? C26 Fe2 C23 152.2(3) . . ? C20 Fe2 C22 68.72(14) . . ? C25 Fe2 C22 123.5(2) . . ? C21 Fe2 C22 40.0(2) . . ? C27 Fe2 C22 152.4(2) . . ? C26 Fe2 C22 166.1(3) . . ? C23 Fe2 C22 41.7(2) . . ? C20 Fe2 C28 161.5(2) . . ? C25 Fe2 C28 66.7(3) . . ? C21 Fe2 C28 155.2(2) . . ? C27 Fe2 C28 36.4(3) . . ? C26 Fe2 C28 64.1(3) . . ? C23 Fe2 C28 106.1(2) . . ? C22 Fe2 C28 120.3(2) . . ? C20 Fe2 C24 159.2(2) . . ? C25 Fe2 C24 40.8(2) . . ? C21 Fe2 C24 122.0(2) . . ? C27 Fe2 C24 64.5(2) . . ? C26 Fe2 C24 68.2(2) . . ? C23 Fe2 C24 121.6(2) . . ? C22 Fe2 C24 106.4(2) . . ? C28 Fe2 C24 38.5(2) . . ? C20 Fe2 C19 41.79(14) . . ? C25 Fe2 C19 159.7(2) . . ? C21 Fe2 C19 69.93(15) . . ? C27 Fe2 C19 108.3(2) . . ? C26 Fe2 C19 120.6(2) . . ? C23 Fe2 C19 40.62(13) . . ? C22 Fe2 C19 69.46(14) . . ? C28 Fe2 C19 123.1(2) . . ? C24 Fe2 C19 157.3(2) . . ? Pd2 Br1 Pd1 83.642(14) . . ? Pd1 Br2 Pd2 82.703(13) . . ? C17 O1 C18 112.6(4) . . ? C35 O2 C36 106.8(5) . . ? C11 N1 N2 117.3(3) . . ? C11 N1 Pd1 116.2(2) . . ? N2 N1 Pd1 126.4(2) . . ? N1 N2 C16 111.8(3) . . ? N1 N2 C13 114.7(3) . . ? C16 N2 C13 108.9(3) . . ? C29 N3 N4 115.0(3) . . ? C29 N3 Pd2 116.0(2) . . ? N4 N3 Pd2 129.0(2) . . ? N3 N4 C31 115.0(3) . . ? N3 N4 C34 110.1(3) . . ? C31 N4 C34 105.7(3) . . ? C2 C1 C5 105.7(3) . . ? C2 C1 Pd1 114.3(2) . . ? C5 C1 Pd1 140.0(3) . . ? C2 C1 Fe1 68.9(2) . . ? C5 C1 Fe1 68.8(2) . . ? Pd1 C1 Fe1 125.3(2) . . ? C1 C2 C3 109.9(3) . . ? C1 C2 C11 116.6(3) . . ? C3 C2 C11 133.5(4) . . ? C1 C2 Fe1 70.1(2) . . ? C3 C2 Fe1 69.8(2) . . ? C11 C2 Fe1 124.5(3) . . ? C4 C3 C2 106.0(4) . . ? C4 C3 Fe1 70.3(2) . . ? C2 C3 Fe1 68.6(2) . . ? C5 C4 C3 109.1(4) . . ? C5 C4 Fe1 69.0(2) . . ? C3 C4 Fe1 68.7(3) . . ? C4 C5 C1 109.2(4) . . ? C4 C5 Fe1 71.1(3) . . ? C1 C5 Fe1 69.3(2) . . ? C10 C6 C7 108.5(8) . . ? C10 C6 Fe1 72.7(6) . . ? C7 C6 Fe1 69.7(5) . . ? C8 C7 C6 103.2(7) . . ? C8 C7 Fe1 69.8(4) . . ? C6 C7 Fe1 69.4(6) . . ? C9 C8 C7 108.4(6) . . ? C9 C8 Fe1 70.7(4) . . ? C7 C8 Fe1 71.3(4) . . ? C8 C9 C10 105.9(6) . . ? C8 C9 Fe1 72.4(4) . . ? C10 C9 Fe1 70.5(4) . . ? C6 C10 C9 114.0(8) . . ? C6 C10 Fe1 75.2(6) . . ? C9 C10 Fe1 69.8(4) . . ? N1 C11 C2 113.2(3) . . ? N1 C11 C12 123.5(3) . . ? C2 C11 C12 123.1(3) . . ? N2 C13 C14 105.8(4) . . ? N2 C13 C17 114.1(4) . . ? C14 C13 C17 110.2(4) . . ? C15 C14 C13 105.1(5) . . ? C14 C15 C16 107.5(4) . . ? N2 C16 C15 106.1(4) . . ? O1 C17 C13 110.5(3) . . ? C23 C19 C20 105.7(3) . . ? C23 C19 Pd2 140.9(3) . . ? C20 C19 Pd2 113.3(2) . . ? C23 C19 Fe2 68.8(2) . . ? C20 C19 Fe2 67.0(2) . . ? Pd2 C19 Fe2 123.3(2) . . ? C21 C20 C29 133.6(3) . . ? C21 C20 C19 109.2(3) . . ? C29 C20 C19 117.2(3) . . ? C21 C20 Fe2 70.4(2) . . ? C29 C20 Fe2 123.9(2) . . ? C19 C20 Fe2 71.2(2) . . ? C22 C21 C20 108.1(3) . . ? C22 C21 Fe2 70.4(2) . . ? C20 C21 Fe2 68.2(2) . . ? C21 C22 C23 108.1(3) . . ? C21 C22 Fe2 69.6(2) . . ? C23 C22 Fe2 68.9(2) . . ? C19 C23 C22 108.9(3) . . ? C19 C23 Fe2 70.6(2) . . ? C22 C23 Fe2 69.4(2) . . ? C28 C24 C25 107.8(5) . . ? C28 C24 Fe2 70.6(4) . . ? C25 C24 Fe2 68.6(3) . . ? C24 C25 C26 102.2(5) . . ? C24 C25 Fe2 70.6(3) . . ? C26 C25 Fe2 68.2(3) . . ? C27 C26 C25 105.5(5) . . ? C27 C26 Fe2 70.8(3) . . ? C25 C26 Fe2 67.8(3) . . ? C28 C27 C26 112.5(6) . . ? C28 C27 Fe2 72.6(4) . . ? C26 C27 Fe2 71.0(4) . . ? C27 C28 C24 112.0(6) . . ? C27 C28 Fe2 70.9(4) . . ? C24 C28 Fe2 70.9(3) . . ? N3 C29 C20 112.9(3) . . ? N3 C29 C30 123.3(3) . . ? C20 C29 C30 123.8(3) . . ? N4 C31 C35 109.7(3) . . ? N4 C31 C32 102.4(4) . . ? C35 C31 C32 113.1(4) . . ? C33 C32 C31 107.3(4) . . ? C32 C33 C34 105.2(4) . . ? N4 C34 C33 101.2(4) . . ? O2 C35 C31 109.0(4) . . ? _refine_diff_density_max 0.982 _refine_diff_density_min -1.108 _refine_diff_density_rms 0.130 #=END data_zgf64 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common syn-(-)-(Sp,S,S,Sp)-5 _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C48 H58 Br2 Fe2 N4 O2 Pd2' _chemical_formula_weight 1207.30 _chemical_melting_point ? _chemical_compound_source synthesized 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' 'Fe' 'Fe' 0.3463 0.8444 '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 10.651(2) _cell_length_b 13.215(3) _cell_length_c 34.580(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4867.2(17) _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 plate _exptl_crystal_colour red _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.648 _exptl_crystal_density_method ? _exptl_crystal_F_000 2416 _exptl_absorpt_coefficient_mu 2.994 _exptl_absorpt_correction_type 'ABSCOR' _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 'RIGAKU RXAIS II' _diffrn_measurement_method 'IP' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10974 _diffrn_reflns_av_R_equivalents 0.1174 _diffrn_reflns_av_sigmaI/netI 0.1259 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -41 _diffrn_reflns_limit_l_max 41 _diffrn_reflns_theta_min 1.18 _diffrn_reflns_theta_max 23.00 _reflns_number_total 6296 _reflns_number_observed 5618 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'R-AXIS' _computing_cell_refinement 'BIOTEX' _computing_data_reduction 'BIOTEX' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'SIEMENS SHELXL PC' _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 4 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^)+(0.1812P)^2^+0.9059P] 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 refxyz _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00079(13) _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 0.490(12) _refine_ls_number_reflns 6292 _refine_ls_number_parameters 543 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1049 _refine_ls_R_factor_obs 0.0958 _refine_ls_wR_factor_all 0.2590 _refine_ls_wR_factor_obs 0.2468 _refine_ls_goodness_of_fit_all 1.067 _refine_ls_goodness_of_fit_obs 1.082 _refine_ls_restrained_S_all 1.074 _refine_ls_restrained_S_obs 1.082 _refine_ls_shift/esd_max -0.614 _refine_ls_shift/esd_mean 0.033 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 0.59929(4) 0.16294(4) 0.863852(14) 0.06046(13) Uani 1 d . . Pd2 Pd 0.78691(4) 0.28651(4) 0.789639(15) 0.06004(13) Uani 1 d . . Fe1 Fe 0.32211(9) 0.18683(8) 0.92142(3) 0.0678(3) Uani 1 d . . Fe2 Fe 1.08665(8) 0.39273(7) 0.78299(3) 0.0611(3) Uani 1 d . . Br1 Br 0.55998(6) 0.30171(7) 0.81788(2) 0.0858(2) Uani 1 d . . Br2 Br 0.83420(7) 0.18909(7) 0.84813(2) 0.0863(2) Uani 1 d . . O1 O 0.8669(5) -0.1882(4) 0.8671(2) 0.099(2) Uani 1 d . . O2 O 0.4827(8) 0.2353(10) 0.6716(4) 0.264(5) Uani 1 d . . N1 N 0.6047(4) 0.0443(4) 0.90393(13) 0.0549(14) Uani 1 d . . N2 N 0.7104(5) 0.0087(5) 0.9250(2) 0.071(2) Uani 1 d . . N3 N 0.7790(5) 0.3705(4) 0.7392(2) 0.061(2) Uani 1 d . . N4 N 0.6751(6) 0.4215(5) 0.7216(2) 0.088(2) Uani 1 d . . C1 C 0.4208(6) 0.1413(5) 0.8737(2) 0.067(2) Uani 1 d . . C2 C 0.3914(6) 0.0593(5) 0.8964(2) 0.066(2) Uani 1 d . . C3 C 0.2564(6) 0.0530(6) 0.9007(2) 0.076(2) Uani 1 d . . H3 H 0.2131(6) 0.0047(6) 0.9151(2) 0.092 Uiso 1 calc R . C4 C 0.2040(6) 0.1300(7) 0.8802(2) 0.083(3) Uani 1 d . . H4 H 0.1188(6) 0.1444(7) 0.8782(2) 0.100 Uiso 1 calc R . C5 C 0.3045(5) 0.1848(5) 0.8623(2) 0.064(2) Uani 1 d . . H5 H 0.2952(5) 0.2399(5) 0.8459(2) 0.077 Uiso 1 calc R . C6 C 0.2622(10) 0.2023(10) 0.9764(3) 0.123(4) Uani 1 d . . H6 H 0.2131(10) 0.1544(10) 0.9891(3) 0.147 Uiso 1 calc R . C7 C 0.2195(12) 0.2830(10) 0.9551(3) 0.157(5) Uani 1 d . . H7 H 0.1361(12) 0.3023(10) 0.9521(3) 0.188 Uiso 1 calc R . C8 C 0.3281(13) 0.3331(7) 0.9381(3) 0.132(4) Uani 1 d . . H8 H 0.3289(13) 0.3887(7) 0.9216(3) 0.159 Uiso 1 calc R . C9 C 0.4328(11) 0.2777(7) 0.9523(3) 0.115(4) Uani 1 d . . H9 H 0.5159(11) 0.2912(7) 0.9459(3) 0.138 Uiso 1 calc R . C10 C 0.3970(9) 0.2058(9) 0.9754(2) 0.120(4) Uani 1 d . . H10 H 0.4502(9) 0.1632(9) 0.9892(2) 0.144 Uiso 1 calc R . C11 C 0.4949(6) 0.0100(6) 0.9156(2) 0.067(2) Uani 1 d . . C12 C 0.4797(7) -0.0771(6) 0.9447(2) 0.086(2) Uani 1 d . . H12A H 0.5610(7) -0.0979(6) 0.9537(2) 0.129 Uiso 1 calc R . H12B H 0.4387(7) -0.1331(6) 0.9324(2) 0.129 Uiso 1 calc R . H12C H 0.4301(7) -0.0546(6) 0.9662(2) 0.129 Uiso 1 calc R . C13 C 0.8054(6) -0.0386(5) 0.9007(2) 0.071(2) Uani 1 d . . H13 H 0.8130(6) 0.0003(5) 0.8767(2) 0.085 Uiso 1 calc R . C14 C 0.9274(7) -0.0272(6) 0.9239(3) 0.100(3) Uani 1 d . . H14A H 0.9445(7) -0.0876(6) 0.9390(3) 0.121 Uiso 1 calc R . H14B H 0.9981(7) -0.0141(6) 0.9070(3) 0.121 Uiso 1 calc R . C15 C 0.9028(8) 0.0604(9) 0.9494(3) 0.109(3) Uani 1 d . . H15A H 0.9247(8) 0.0431(9) 0.9758(3) 0.130 Uiso 1 calc R . H15B H 0.9547(8) 0.1171(9) 0.9415(3) 0.130 Uiso 1 calc R . C16 C 0.7693(9) 0.0894(8) 0.9475(2) 0.095(3) Uani 1 d . . H16A H 0.7331(9) 0.0935(8) 0.9732(2) 0.114 Uiso 1 calc R . H16B H 0.7593(9) 0.1543(8) 0.9347(2) 0.114 Uiso 1 calc R . C17 C 0.7720(7) -0.1452(6) 0.8909(2) 0.071(2) Uani 1 d . . H17A H 0.7636(7) -0.1846(6) 0.9144(2) 0.086 Uiso 1 calc R . H17B H 0.6922(7) -0.1467(6) 0.8774(2) 0.086 Uiso 1 calc R . C18 C 0.8548(10) -0.2869(7) 0.8569(3) 0.115(4) Uani 1 d . . H18A H 0.9245(10) -0.3064(7) 0.8410(3) 0.173 Uiso 1 calc R . H18B H 0.7780(10) -0.2960(7) 0.8428(3) 0.173 Uiso 1 calc R . H18C H 0.8533(10) -0.3281(7) 0.8798(3) 0.173 Uiso 1 calc R . C19 C 0.9635(6) 0.2763(5) 0.7722(2) 0.062(2) Uani 1 d . . C20 C 0.9894(6) 0.3333(5) 0.7382(2) 0.063(2) Uani 1 d . . C21 C 1.1193(6) 0.3284(6) 0.7297(2) 0.069(2) Uani 1 d . . H21 H 1.1603(6) 0.3568(6) 0.7085(2) 0.083 Uiso 1 calc R . C22 C 1.1749(6) 0.2705(5) 0.7605(2) 0.066(2) Uani 1 d . . H22 H 1.2603(6) 0.2570(5) 0.7628(2) 0.080 Uiso 1 calc R . C23 C 1.0800(6) 0.2358(4) 0.7876(2) 0.066(2) Uani 1 d . . H23 H 1.0912(6) 0.1967(4) 0.8098(2) 0.079 Uiso 1 calc R . C24 C 0.9967(10) 0.4856(5) 0.8232(3) 0.093(3) Uani 1 d . . H24 H 0.9168(10) 0.4790(5) 0.8337(3) 0.112 Uiso 1 calc R . C25 C 1.0327(8) 0.5413(6) 0.7877(3) 0.092(3) Uani 1 d . . H25 H 0.9794(8) 0.5757(6) 0.7709(3) 0.111 Uiso 1 calc R . C26 C 1.1730(8) 0.5310(7) 0.7842(4) 0.109(4) Uani 1 d . . H26 H 1.2221(8) 0.5597(7) 0.7648(4) 0.131 Uiso 1 calc R . C27 C 1.2162(8) 0.4739(7) 0.8133(3) 0.107(3) Uani 1 d . . H27 H 1.3002(8) 0.4570(7) 0.8168(3) 0.129 Uiso 1 calc R . C28 C 1.1166(9) 0.4424(6) 0.8383(3) 0.096(3) Uani 1 d . . H28 H 1.1250(9) 0.4020(6) 0.8602(3) 0.115 Uiso 1 calc R . C29 C 0.8840(6) 0.3847(5) 0.7204(2) 0.060(2) Uani 1 d . . C30 C 0.9017(9) 0.4482(8) 0.6848(2) 0.100(3) Uani 1 d . . H30A H 0.8224(9) 0.4763(8) 0.6771(2) 0.150 Uiso 1 calc R . H30B H 0.9344(9) 0.4070(8) 0.6643(2) 0.150 Uiso 1 calc R . H30C H 0.9596(9) 0.5020(8) 0.6903(2) 0.150 Uiso 1 calc R . C31 C 0.5620(7) 0.3533(7) 0.7143(3) 0.092(3) Uani 1 d . . H31 H 0.5476(7) 0.3073(7) 0.7361(3) 0.111 Uiso 1 calc R . C32 C 0.4640(8) 0.4409(8) 0.7139(5) 0.148(5) Uani 1 d . . H32A H 0.4490(8) 0.4610(8) 0.6873(5) 0.177 Uiso 1 calc R . H32B H 0.3853(8) 0.4160(8) 0.7243(5) 0.177 Uiso 1 calc R . C33 C 0.5011(10) 0.5260(9) 0.7350(4) 0.149(5) Uani 1 d . . H33A H 0.4487(10) 0.5351(9) 0.7577(4) 0.178 Uiso 1 calc R . H33B H 0.4973(10) 0.5867(9) 0.7193(4) 0.178 Uiso 1 calc R . C34 C 0.6275(10) 0.5031(7) 0.7457(4) 0.134(4) Uani 1 d . . H34A H 0.6305(10) 0.4831(7) 0.7727(4) 0.161 Uiso 1 calc R . H34B H 0.6796(10) 0.5627(7) 0.7425(4) 0.161 Uiso 1 calc R . C35 C 0.5902(13) 0.2968(14) 0.6785(4) 0.206(7) Uani 1 d . . H35A H 0.6041(13) 0.3429(14) 0.6571(4) 0.247 Uiso 1 calc R . H35B H 0.6645(13) 0.2552(14) 0.6818(4) 0.247 Uiso 1 calc R . C36 C 0.4901(15) 0.1466(16) 0.6698(9) 0.338(15) Uani 1 d . . H36A H 0.4084(15) 0.1186(16) 0.6650(9) 0.507 Uiso 1 calc R . H36B H 0.5222(15) 0.1207(16) 0.6937(9) 0.507 Uiso 1 calc R . H36C H 0.5457(15) 0.1282(16) 0.6491(9) 0.507 Uiso 1 calc R . C37 C 0.7384(17) 0.4263(11) 0.9131(5) 0.176(7) Uani 1 d . . H37 H 0.7120(17) 0.3746(11) 0.8967(5) 0.211 Uiso 1 calc R . C38 C 0.6514(16) 0.4916(12) 0.9277(4) 0.171(6) Uani 1 d . . H38 H 0.5669(16) 0.4840(12) 0.9215(4) 0.205 Uiso 1 calc R . C39 C 0.6895(17) 0.5693(18) 0.9519(5) 0.223(11) Uani 1 d . . H39 H 0.6316(17) 0.6150(18) 0.9619(5) 0.268 Uiso 1 calc R . C40 C 0.8126(24) 0.5774(13) 0.9606(4) 0.220(10) Uani 1 d . . H40 H 0.8389(24) 0.6290(13) 0.9770(4) 0.264 Uiso 1 calc R . C41 C 0.8967(13) 0.5139(15) 0.9464(5) 0.184(7) Uani 1 d . . H41 H 0.9808(13) 0.5217(15) 0.9529(5) 0.221 Uiso 1 calc R . C42 C 0.8606(14) 0.4343(14) 0.9215(4) 0.187(7) Uani 1 d . . H42 H 0.9193(14) 0.3894(14) 0.9114(4) 0.225 Uiso 1 calc R . C43 C 1.2990(22) 0.6156(16) 0.9577(7) 0.257(10) Uani 1 d . . H43 H 1.3555(22) 0.5731(16) 0.9701(7) 0.309 Uiso 1 calc R . C44 C 1.2826(27) 0.6074(14) 0.9192(6) 0.290(13) Uani 1 d . . H44 H 1.3289(27) 0.5599(14) 0.9054(6) 0.348 Uiso 1 calc R . C45 C 1.1978(14) 0.6685(9) 0.8998(4) 0.143(5) Uani 1 d . . H45 H 1.1814(14) 0.6596(9) 0.8737(4) 0.171 Uiso 1 calc R . C46 C 1.1379(16) 0.7440(11) 0.9212(4) 0.191(6) Uani 1 d . . H46 H 1.0865(16) 0.7897(11) 0.9082(4) 0.230 Uiso 1 calc R . C47 C 1.1515(11) 0.7534(12) 0.9596(5) 0.183(6) Uani 1 d . . H47 H 1.1082(11) 0.8029(12) 0.9733(5) 0.220 Uiso 1 calc R . C48 C 1.2337(17) 0.6857(12) 0.9787(4) 0.169(7) Uani 1 d . . H48 H 1.2434(17) 0.6888(12) 1.0054(4) 0.203 Uiso 1 calc R . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.0516(2) 0.0700(3) 0.0597(2) 0.0069(2) 0.0048(2) 0.0011(2) Pd2 0.0515(2) 0.0610(2) 0.0677(3) 0.0112(2) 0.0011(2) -0.0002(2) Fe1 0.0588(5) 0.0820(6) 0.0627(5) -0.0084(5) 0.0021(4) 0.0028(4) Fe2 0.0557(4) 0.0600(5) 0.0676(5) 0.0015(4) 0.0023(4) 0.0023(4) Br1 0.0603(4) 0.1018(5) 0.0955(4) 0.0346(4) 0.0093(3) 0.0103(3) Br2 0.0585(3) 0.1038(5) 0.0967(4) 0.0417(4) 0.0041(3) 0.0019(4) O1 0.090(3) 0.079(3) 0.126(4) -0.019(3) 0.025(3) 0.004(3) O2 0.149(5) 0.278(11) 0.367(11) -0.135(10) -0.152(6) 0.086(6) N1 0.044(2) 0.071(3) 0.049(2) 0.006(2) 0.004(2) 0.005(2) N2 0.064(3) 0.082(4) 0.067(3) 0.000(3) 0.006(3) 0.009(3) N3 0.042(2) 0.072(3) 0.069(3) 0.010(3) -0.001(2) -0.004(2) N4 0.058(3) 0.101(4) 0.104(4) 0.031(4) -0.014(3) -0.001(3) C1 0.050(3) 0.081(4) 0.069(4) 0.002(3) 0.011(3) 0.005(3) C2 0.046(3) 0.076(4) 0.075(4) -0.004(3) 0.008(3) -0.007(3) C3 0.055(4) 0.094(5) 0.080(4) 0.009(4) -0.002(3) -0.009(3) C4 0.039(3) 0.135(7) 0.075(4) 0.023(4) -0.005(3) -0.002(4) C5 0.044(3) 0.072(4) 0.076(4) -0.004(3) 0.000(3) -0.003(3) C6 0.114(7) 0.163(10) 0.091(6) 0.005(6) 0.024(5) -0.034(7) C7 0.140(8) 0.198(10) 0.132(7) -0.078(7) -0.001(7) 0.057(8) C8 0.181(10) 0.074(5) 0.142(8) -0.044(6) 0.011(8) 0.021(6) C9 0.139(8) 0.099(6) 0.107(5) -0.045(5) 0.001(6) -0.006(6) C10 0.111(6) 0.166(9) 0.082(4) -0.048(5) -0.047(4) 0.028(6) C11 0.068(4) 0.075(4) 0.057(3) 0.008(3) 0.008(3) 0.011(3) C12 0.067(4) 0.080(4) 0.110(5) 0.035(4) 0.023(4) 0.001(3) C13 0.064(4) 0.059(4) 0.090(4) 0.003(4) 0.008(3) -0.004(3) C14 0.052(4) 0.071(4) 0.178(8) -0.026(5) -0.004(5) -0.009(3) C15 0.068(4) 0.145(8) 0.113(6) -0.007(6) -0.028(5) 0.000(5) C16 0.100(5) 0.127(7) 0.058(4) 0.005(4) -0.011(4) 0.020(5) C17 0.059(3) 0.083(4) 0.073(4) -0.016(4) -0.003(3) -0.004(3) C18 0.146(8) 0.069(5) 0.131(7) -0.014(5) 0.002(6) 0.006(6) C19 0.058(3) 0.058(3) 0.070(3) -0.008(3) -0.007(3) 0.001(3) C20 0.067(3) 0.074(4) 0.047(3) 0.011(3) 0.003(3) -0.009(3) C21 0.072(4) 0.079(4) 0.056(3) -0.006(3) 0.005(3) 0.020(3) C22 0.050(3) 0.072(4) 0.077(4) 0.001(3) -0.010(3) 0.006(3) C23 0.054(3) 0.050(3) 0.094(4) -0.014(3) 0.008(3) 0.004(2) C24 0.126(6) 0.048(3) 0.107(5) -0.029(4) -0.003(5) -0.011(4) C25 0.116(6) 0.055(4) 0.106(5) -0.007(4) 0.030(5) 0.017(4) C26 0.071(5) 0.089(5) 0.167(9) -0.001(6) 0.000(6) -0.012(4) C27 0.069(4) 0.096(5) 0.156(7) -0.042(5) -0.025(5) 0.000(4) C28 0.092(5) 0.061(4) 0.135(7) -0.020(5) 0.002(5) 0.004(4) C29 0.060(3) 0.059(3) 0.062(3) 0.020(3) -0.002(3) -0.012(3) C30 0.090(5) 0.139(7) 0.071(4) 0.038(4) 0.027(4) -0.005(5) C31 0.057(4) 0.127(7) 0.093(5) 0.021(5) -0.008(4) -0.004(4) C32 0.059(4) 0.113(7) 0.271(14) 0.056(8) -0.035(6) 0.011(4) C33 0.106(6) 0.142(8) 0.197(11) 0.030(8) 0.045(7) 0.073(5) C34 0.121(8) 0.087(6) 0.195(10) 0.054(6) 0.038(7) 0.011(5) C35 0.164(10) 0.314(16) 0.139(8) -0.088(9) -0.043(8) -0.066(11) C36 0.115(11) 0.279(18) 0.620(41) 0.219(23) 0.053(20) 0.061(12) C37 0.217(15) 0.119(10) 0.192(14) -0.013(10) 0.007(13) -0.040(10) C38 0.181(11) 0.140(11) 0.191(12) 0.042(9) -0.066(10) -0.032(9) C39 0.169(14) 0.324(28) 0.178(13) -0.002(17) -0.043(12) 0.049(17) C40 0.433(29) 0.142(11) 0.085(6) 0.013(7) -0.053(12) 0.032(16) C41 0.118(8) 0.268(18) 0.167(11) 0.031(12) -0.041(8) -0.063(11) C42 0.121(9) 0.276(17) 0.165(10) 0.091(11) 0.002(8) -0.031(11) C43 0.271(20) 0.256(19) 0.245(19) 0.078(16) 0.033(18) 0.130(14) C44 0.503(35) 0.187(14) 0.179(14) 0.060(12) 0.083(20) 0.158(17) C45 0.194(11) 0.111(7) 0.122(8) 0.011(7) -0.001(8) -0.046(8) C46 0.251(14) 0.172(10) 0.152(8) -0.083(7) -0.093(8) 0.080(10) C47 0.096(7) 0.194(12) 0.259(14) -0.086(11) -0.061(8) 0.037(8) C48 0.214(15) 0.160(13) 0.133(10) -0.007(10) 0.028(10) 0.015(12) _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 1.952(6) . ? Pd1 N1 2.094(5) . ? Pd1 Br1 2.4630(10) . ? Pd1 Br2 2.5837(10) . ? Pd2 C19 1.980(6) . ? Pd2 N3 2.071(5) . ? Pd2 Br2 2.4498(10) . ? Pd2 Br1 2.6145(9) . ? Fe1 C9 1.993(11) . ? Fe1 C6 2.016(10) . ? Fe1 C8 2.018(10) . ? Fe1 C3 2.032(8) . ? Fe1 C2 2.034(7) . ? Fe1 C7 2.042(12) . ? Fe1 C4 2.044(8) . ? Fe1 C10 2.047(8) . ? Fe1 C1 2.046(7) . ? Fe1 C5 2.053(7) . ? Fe2 C20 2.022(6) . ? Fe2 C22 2.024(7) . ? Fe2 C27 2.039(9) . ? Fe2 C26 2.046(9) . ? Fe2 C28 2.048(10) . ? Fe2 C25 2.052(8) . ? Fe2 C19 2.056(6) . ? Fe2 C21 2.060(7) . ? Fe2 C23 2.082(6) . ? Fe2 C24 2.086(9) . ? O1 C18 1.357(11) . ? O1 C17 1.422(9) . ? O2 C36 1.18(2) . ? O2 C35 1.42(2) . ? N1 C11 1.317(9) . ? N1 N2 1.422(7) . ? N2 C13 1.457(9) . ? N2 C16 1.461(11) . ? N3 C29 1.306(8) . ? N3 N4 1.431(8) . ? N4 C34 1.453(13) . ? N4 C31 1.525(11) . ? C1 C2 1.373(10) . ? C1 C5 1.421(9) . ? C2 C11 1.443(10) . ? C2 C3 1.449(9) . ? C3 C4 1.360(11) . ? C4 C5 1.433(10) . ? C6 C7 1.37(2) . ? C6 C10 1.436(15) . ? C7 C8 1.46(2) . ? C8 C9 1.42(2) . ? C9 C10 1.299(15) . ? C11 C12 1.537(11) . ? C13 C17 1.493(10) . ? C13 C14 1.535(11) . ? C14 C15 1.478(14) . ? C15 C16 1.475(13) . ? C19 C20 1.423(9) . ? C19 C23 1.453(9) . ? C20 C21 1.416(9) . ? C20 C29 1.449(9) . ? C21 C22 1.440(10) . ? C22 C23 1.454(9) . ? C24 C25 1.481(12) . ? C24 C28 1.494(13) . ? C25 C26 1.506(13) . ? C26 C27 1.340(15) . ? C27 C28 1.432(14) . ? C29 C30 1.501(10) . ? C31 C35 1.48(2) . ? C31 C32 1.559(13) . ? C32 C33 1.40(2) . ? C33 C34 1.43(2) . ? C37 C38 1.36(2) . ? C37 C42 1.34(2) . ? C38 C39 1.38(3) . ? C39 C40 1.35(3) . ? C40 C41 1.32(3) . ? C41 C42 1.41(2) . ? C43 C44 1.35(3) . ? C43 C48 1.37(3) . ? C44 C45 1.38(3) . ? C45 C46 1.39(2) . ? C46 C47 1.34(2) . ? C47 C48 1.41(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 C1 Pd1 N1 78.5(2) . . ? C1 Pd1 Br1 93.2(2) . . ? N1 Pd1 Br1 171.76(13) . . ? C1 Pd1 Br2 177.8(2) . . ? N1 Pd1 Br2 102.30(13) . . ? Br1 Pd1 Br2 85.94(3) . . ? C19 Pd2 N3 79.5(2) . . ? C19 Pd2 Br2 91.2(2) . . ? N3 Pd2 Br2 170.46(14) . . ? C19 Pd2 Br1 175.8(2) . . ? N3 Pd2 Br1 103.66(14) . . ? Br2 Pd2 Br1 85.53(3) . . ? C9 Fe1 C6 67.7(5) . . ? C9 Fe1 C8 41.5(5) . . ? C6 Fe1 C8 69.1(5) . . ? C9 Fe1 C3 156.5(4) . . ? C6 Fe1 C3 108.1(4) . . ? C8 Fe1 C3 160.9(4) . . ? C9 Fe1 C2 120.9(4) . . ? C6 Fe1 C2 126.9(4) . . ? C8 Fe1 C2 154.7(4) . . ? C3 Fe1 C2 41.7(3) . . ? C9 Fe1 C7 68.6(5) . . ? C6 Fe1 C7 39.6(5) . . ? C8 Fe1 C7 42.1(5) . . ? C3 Fe1 C7 123.9(4) . . ? C2 Fe1 C7 162.5(4) . . ? C9 Fe1 C4 163.6(4) . . ? C6 Fe1 C4 120.0(4) . . ? C8 Fe1 C4 124.8(4) . . ? C3 Fe1 C4 39.0(3) . . ? C2 Fe1 C4 67.8(3) . . ? C7 Fe1 C4 107.3(4) . . ? C9 Fe1 C10 37.5(4) . . ? C6 Fe1 C10 41.4(4) . . ? C8 Fe1 C10 67.0(5) . . ? C3 Fe1 C10 124.2(4) . . ? C2 Fe1 C10 110.4(4) . . ? C7 Fe1 C10 67.1(5) . . ? C4 Fe1 C10 157.1(4) . . ? C9 Fe1 C1 107.8(4) . . ? C6 Fe1 C1 162.3(4) . . ? C8 Fe1 C1 119.7(4) . . ? C3 Fe1 C1 68.7(3) . . ? C2 Fe1 C1 39.3(3) . . ? C7 Fe1 C1 156.6(4) . . ? C4 Fe1 C1 69.3(3) . . ? C10 Fe1 C1 124.9(3) . . ? C9 Fe1 C5 126.6(4) . . ? C6 Fe1 C5 155.7(4) . . ? C8 Fe1 C5 107.4(4) . . ? C3 Fe1 C5 66.8(3) . . ? C2 Fe1 C5 66.3(3) . . ? C7 Fe1 C5 121.8(4) . . ? C4 Fe1 C5 41.0(3) . . ? C10 Fe1 C5 161.1(3) . . ? C1 Fe1 C5 40.6(2) . . ? C20 Fe2 C22 68.5(3) . . ? C20 Fe2 C27 160.9(3) . . ? C22 Fe2 C27 107.6(3) . . ? C20 Fe2 C26 126.3(4) . . ? C22 Fe2 C26 120.8(3) . . ? C27 Fe2 C26 38.3(4) . . ? C20 Fe2 C28 156.9(3) . . ? C22 Fe2 C28 122.8(3) . . ? C27 Fe2 C28 41.0(4) . . ? C26 Fe2 C28 68.0(4) . . ? C20 Fe2 C25 106.8(3) . . ? C22 Fe2 C25 157.5(3) . . ? C27 Fe2 C25 69.2(4) . . ? C26 Fe2 C25 43.1(4) . . ? C28 Fe2 C25 70.3(3) . . ? C20 Fe2 C19 40.8(3) . . ? C22 Fe2 C19 68.2(3) . . ? C27 Fe2 C19 156.8(3) . . ? C26 Fe2 C19 163.5(3) . . ? C28 Fe2 C19 120.6(3) . . ? C25 Fe2 C19 123.5(3) . . ? C20 Fe2 C21 40.6(3) . . ? C22 Fe2 C21 41.3(3) . . ? C27 Fe2 C21 124.3(3) . . ? C26 Fe2 C21 108.1(4) . . ? C28 Fe2 C21 160.4(3) . . ? C25 Fe2 C21 120.8(3) . . ? C19 Fe2 C21 68.7(3) . . ? C20 Fe2 C23 69.8(3) . . ? C22 Fe2 C23 41.4(3) . . ? C27 Fe2 C23 120.5(3) . . ? C26 Fe2 C23 154.6(3) . . ? C28 Fe2 C23 104.6(3) . . ? C25 Fe2 C23 159.7(3) . . ? C19 Fe2 C23 41.1(3) . . ? C21 Fe2 C23 70.4(3) . . ? C20 Fe2 C24 120.2(3) . . ? C22 Fe2 C24 159.8(3) . . ? C27 Fe2 C24 70.0(4) . . ? C26 Fe2 C24 70.6(4) . . ? C28 Fe2 C24 42.3(4) . . ? C25 Fe2 C24 41.9(3) . . ? C19 Fe2 C24 105.6(3) . . ? C21 Fe2 C24 156.4(3) . . ? C23 Fe2 C24 121.3(3) . . ? Pd1 Br1 Pd2 91.53(3) . . ? Pd2 Br2 Pd1 92.58(3) . . ? C18 O1 C17 117.8(7) . . ? C36 O2 C35 121.6(13) . . ? C11 N1 N2 115.6(5) . . ? C11 N1 Pd1 115.8(4) . . ? N2 N1 Pd1 127.5(4) . . ? N1 N2 C13 113.3(5) . . ? N1 N2 C16 111.8(6) . . ? C13 N2 C16 108.8(6) . . ? C29 N3 N4 112.6(5) . . ? C29 N3 Pd2 117.4(4) . . ? N4 N3 Pd2 129.9(4) . . ? N3 N4 C34 112.1(7) . . ? N3 N4 C31 113.8(6) . . ? C34 N4 C31 105.0(7) . . ? C2 C1 C5 106.2(6) . . ? C2 C1 Pd1 115.9(5) . . ? C5 C1 Pd1 137.8(5) . . ? C2 C1 Fe1 69.8(4) . . ? C5 C1 Fe1 70.0(4) . . ? Pd1 C1 Fe1 126.7(3) . . ? C1 C2 C11 116.4(6) . . ? C1 C2 C3 109.3(6) . . ? C11 C2 C3 133.2(7) . . ? C1 C2 Fe1 70.8(4) . . ? C11 C2 Fe1 117.1(5) . . ? C3 C2 Fe1 69.1(4) . . ? C4 C3 C2 108.1(7) . . ? C4 C3 Fe1 71.0(5) . . ? C2 C3 Fe1 69.2(4) . . ? C3 C4 C5 107.3(6) . . ? C3 C4 Fe1 70.1(4) . . ? C5 C4 Fe1 69.9(4) . . ? C1 C5 C4 109.1(6) . . ? C1 C5 Fe1 69.5(4) . . ? C4 C5 Fe1 69.2(4) . . ? C7 C6 C10 107.0(11) . . ? C7 C6 Fe1 71.2(6) . . ? C10 C6 Fe1 70.4(5) . . ? C6 C7 C8 107.8(11) . . ? C6 C7 Fe1 69.2(7) . . ? C8 C7 Fe1 68.1(6) . . ? C9 C8 C7 104.4(10) . . ? C9 C8 Fe1 68.3(6) . . ? C7 C8 Fe1 69.8(7) . . ? C10 C9 C8 111.1(11) . . ? C10 C9 Fe1 73.5(6) . . ? C8 C9 Fe1 70.2(6) . . ? C9 C10 C6 109.4(10) . . ? C9 C10 Fe1 69.0(6) . . ? C6 C10 Fe1 68.2(5) . . ? N1 C11 C2 112.4(6) . . ? N1 C11 C12 123.4(6) . . ? C2 C11 C12 124.1(6) . . ? N2 C13 C17 111.8(6) . . ? N2 C13 C14 104.1(6) . . ? C17 C13 C14 114.5(6) . . ? C15 C14 C13 103.8(6) . . ? C16 C15 C14 110.3(8) . . ? N2 C16 C15 104.4(8) . . ? O1 C17 C13 109.9(6) . . ? C20 C19 C23 109.5(6) . . ? C20 C19 Pd2 113.6(5) . . ? C23 C19 Pd2 136.4(5) . . ? C20 C19 Fe2 68.3(4) . . ? C23 C19 Fe2 70.4(3) . . ? Pd2 C19 Fe2 120.0(3) . . ? C21 C20 C19 109.7(6) . . ? C21 C20 C29 133.6(6) . . ? C19 C20 C29 116.7(6) . . ? C21 C20 Fe2 71.1(4) . . ? C19 C20 Fe2 70.8(4) . . ? C29 C20 Fe2 122.7(5) . . ? C20 C21 C22 105.8(6) . . ? C20 C21 Fe2 68.3(4) . . ? C22 C21 Fe2 68.0(4) . . ? C21 C22 C23 111.1(6) . . ? C21 C22 Fe2 70.7(4) . . ? C23 C22 Fe2 71.4(4) . . ? C19 C23 C22 103.9(6) . . ? C19 C23 Fe2 68.5(3) . . ? C22 C23 Fe2 67.2(4) . . ? C25 C24 C28 105.1(8) . . ? C25 C24 Fe2 67.8(5) . . ? C28 C24 Fe2 67.5(5) . . ? C24 C25 C26 106.1(8) . . ? C24 C25 Fe2 70.3(4) . . ? C26 C25 Fe2 68.2(5) . . ? C27 C26 C25 109.4(9) . . ? C27 C26 Fe2 70.6(6) . . ? C25 C26 Fe2 68.7(4) . . ? C26 C27 C28 111.3(8) . . ? C26 C27 Fe2 71.1(6) . . ? C28 C27 Fe2 69.8(5) . . ? C27 C28 C24 108.1(8) . . ? C27 C28 Fe2 69.1(6) . . ? C24 C28 Fe2 70.2(5) . . ? N3 C29 C20 112.7(5) . . ? N3 C29 C30 126.5(6) . . ? C20 C29 C30 120.8(6) . . ? C35 C31 N4 106.1(8) . . ? C35 C31 C32 120.3(10) . . ? N4 C31 C32 95.2(7) . . ? C33 C32 C31 113.7(9) . . ? C32 C33 C34 103.4(9) . . ? C33 C34 N4 109.7(10) . . ? O2 C35 C31 105.4(11) . . ? C38 C37 C42 122.0(16) . . ? C37 C38 C39 119.6(16) . . ? C38 C39 C40 118.6(18) . . ? C41 C40 C39 121.7(17) . . ? C40 C41 C42 121.0(15) . . ? C37 C42 C41 117.2(15) . . ? C44 C43 C48 120.9(20) . . ? C43 C44 C45 121.0(20) . . ? C46 C45 C44 117.3(14) . . ? C47 C46 C45 122.7(14) . . ? C46 C47 C48 118.0(15) . . ? C43 C48 C47 119.8(16) . . ? _refine_diff_density_max 1.354 _refine_diff_density_min -0.851 _refine_diff_density_rms 0.140 #=END data_zgf120 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common (-)-(Sp,R)-4 _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C17 H21 Br Fe N2 O Pd' _chemical_formula_weight 511.52 _chemical_melting_point ? _chemical_compound_source synthesized 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' 'Fe' 'Fe' 0.3463 0.8444 '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 8.2940(10) _cell_length_b 13.8520(10) _cell_length_c 15.567(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1788.5(3) _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 plate _exptl_crystal_colour red _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas 'not measued' _exptl_crystal_density_diffrn 1.900 _exptl_crystal_density_method ? _exptl_crystal_F_000 1008 _exptl_absorpt_coefficient_mu 4.055 _exptl_absorpt_correction_type 'ABSCOR' _exptl_absorpt_correction_T_min 0.915 _exptl_absorpt_correction_T_max 1.017 _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 'IP Rigaku' _diffrn_measurement_method 'IP' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5608 _diffrn_reflns_av_R_equivalents 0.0520 _diffrn_reflns_av_sigmaI/netI 0.0742 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.97 _diffrn_reflns_theta_max 25.58 _reflns_number_total 3165 _reflns_number_observed 2871 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'RAXIS Rigaku' _computing_cell_refinement 'BIOTEX Rigaku' _computing_data_reduction 'BIOTEX Rigaku' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'XP Siemens' _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^)+(0.0475P)^2^+0.0942P] 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 SHELXL _refine_ls_extinction_coef 0.0067(3) _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 0.409(12) _refine_ls_number_reflns 3165 _refine_ls_number_parameters 210 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0584 _refine_ls_R_factor_obs 0.0498 _refine_ls_wR_factor_all 0.1162 _refine_ls_wR_factor_obs 0.1117 _refine_ls_goodness_of_fit_all 1.071 _refine_ls_goodness_of_fit_obs 1.083 _refine_ls_restrained_S_all 1.071 _refine_ls_restrained_S_obs 1.083 _refine_ls_shift/esd_max -0.064 _refine_ls_shift/esd_mean 0.003 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 0.74062(3) 0.18977(2) 0.85494(2) 0.05673(7) Uani 1 d . . Fe1 Fe 0.97140(6) 0.28152(3) 0.68929(3) 0.05106(12) Uani 1 d . . Br1 Br 0.48445(5) 0.21266(4) 0.78433(4) 0.1023(2) Uani 1 d . . O1 O 0.6719(3) 0.0547(2) 0.9238(2) 0.0843(10) Uani 1 d . . N1 N 0.9690(3) 0.1813(2) 0.9048(2) 0.0510(7) Uani 1 d . . N2 N 1.0135(4) 0.1022(2) 0.9543(2) 0.0612(9) Uani 1 d . . C1 C 0.8358(4) 0.2997(2) 0.7976(2) 0.0555(10) Uani 1 d . . C2 C 1.0055(4) 0.3100(2) 0.8152(2) 0.0567(9) Uani 1 d . . C3 C 1.0692(5) 0.3864(3) 0.7656(2) 0.0696(12) Uani 1 d . . H3 H 1.1755(5) 0.4076(3) 0.7656(2) 0.084 Uiso 1 calc R . C4 C 0.9427(5) 0.4244(3) 0.7162(3) 0.0703(12) Uani 1 d . . H4 H 0.9518(5) 0.4753(3) 0.6776(3) 0.084 Uiso 1 calc R . C5 C 0.7971(5) 0.3723(3) 0.7346(2) 0.0658(12) Uani 1 d . . H5 H 0.6963(5) 0.3834(3) 0.7104(2) 0.079 Uiso 1 calc R . C6 C 0.8692(6) 0.2075(3) 0.5913(3) 0.0820(15) Uani 1 d . . H6 H 0.7622(6) 0.2140(3) 0.5744(3) 0.098 Uiso 1 calc R . C7 C 1.0021(6) 0.2606(3) 0.5598(2) 0.0796(14) Uani 1 d . . H7 H 0.9989(6) 0.3071(3) 0.5168(2) 0.096 Uiso 1 calc R . C8 C 1.1418(6) 0.2303(3) 0.6054(3) 0.0768(13) Uani 1 d . . H8 H 1.2452(6) 0.2552(3) 0.5990(3) 0.092 Uiso 1 calc R . C9 C 1.0958(6) 0.1560(3) 0.6621(3) 0.0795(15) Uani 1 d . . H9 H 1.1639(6) 0.1221(3) 0.6987(3) 0.095 Uiso 1 calc R . C10 C 0.9301(5) 0.1423(3) 0.6536(3) 0.0738(13) Uani 1 d . . H10 H 0.8691(5) 0.0975(3) 0.6840(3) 0.089 Uiso 1 calc R . C11 C 1.0718(4) 0.2407(3) 0.8730(2) 0.0572(10) Uani 1 d . . H11 H 1.1809(4) 0.2386(3) 0.8866(2) 0.069 Uiso 1 calc R . C12 C 0.8968(5) 0.0773(3) 1.0209(3) 0.0744(14) Uani 1 d . . H12 H 0.8453(5) 0.1362(3) 1.0424(3) 0.089 Uiso 1 calc R . C13 C 0.9940(7) 0.0301(4) 1.0931(3) 0.099(2) Uani 1 d . . H13A H 0.9500(7) -0.0327(4) 1.1079(3) 0.119 Uiso 1 calc R . H13B H 0.9951(7) 0.0704(4) 1.1441(3) 0.119 Uiso 1 calc R . C14 C 1.1637(7) 0.0204(3) 1.0549(3) 0.101(2) Uani 1 d . . H14A H 1.2451(7) 0.0265(3) 1.0993(3) 0.121 Uiso 1 calc R . H14B H 1.1766(7) -0.0416(3) 1.0267(3) 0.121 Uiso 1 calc R . C15 C 1.1772(5) 0.1029(3) 0.9900(3) 0.0770(13) Uani 1 d . . H15A H 1.2019(5) 0.1638(3) 1.0178(3) 0.092 Uiso 1 calc R . H15B H 1.2576(5) 0.0895(3) 0.9463(3) 0.092 Uiso 1 calc R . C16 C 0.7691(6) 0.0094(3) 0.9858(3) 0.0835(14) Uani 1 d . . H16A H 0.8213(6) -0.0463(3) 0.9602(3) 0.100 Uiso 1 calc R . H16B H 0.7019(6) -0.0132(3) 1.0326(3) 0.100 Uiso 1 calc R . C17 C 0.5568(6) -0.0117(3) 0.8888(4) 0.109(2) Uani 1 d . . H17A H 0.4917(6) 0.0207(3) 0.8467(4) 0.163 Uiso 1 calc R . H17B H 0.4891(6) -0.0358(3) 0.9340(4) 0.163 Uiso 1 calc R . H17C H 0.6125(6) -0.0646(3) 0.8622(4) 0.163 Uiso 1 calc R . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.04765(11) 0.05643(13) 0.06611(14) 0.00454(13) 0.00730(13) 0.00174(13) Fe1 0.0605(2) 0.0419(2) 0.0508(2) 0.0009(2) 0.0010(2) -0.0021(2) Br1 0.0484(2) 0.1240(4) 0.1344(4) 0.0229(4) -0.0092(2) 0.0008(3) O1 0.082(2) 0.065(2) 0.106(2) 0.016(2) 0.017(2) -0.0123(15) N1 0.0634(15) 0.0438(13) 0.0458(13) 0.0028(12) 0.0006(12) 0.0016(14) N2 0.071(2) 0.054(2) 0.058(2) 0.0011(14) -0.003(2) 0.0103(15) C1 0.062(2) 0.048(2) 0.057(2) 0.006(2) 0.002(2) 0.007(2) C2 0.066(2) 0.045(2) 0.060(2) -0.002(2) 0.009(2) -0.007(2) C3 0.085(2) 0.054(2) 0.069(2) 0.000(2) 0.008(2) -0.018(2) C4 0.097(3) 0.048(2) 0.066(2) 0.009(2) 0.011(2) 0.007(2) C5 0.079(2) 0.061(2) 0.057(2) 0.010(2) -0.002(2) 0.021(2) C6 0.101(3) 0.077(3) 0.068(2) -0.010(2) -0.014(2) -0.016(3) C7 0.133(3) 0.055(2) 0.051(2) -0.001(2) 0.000(2) 0.008(3) C8 0.093(3) 0.072(3) 0.066(2) -0.010(2) 0.014(2) 0.005(2) C9 0.115(3) 0.060(2) 0.064(3) -0.010(2) -0.002(2) 0.023(2) C10 0.113(3) 0.049(2) 0.059(2) 0.004(2) -0.002(2) -0.011(2) C11 0.056(2) 0.055(2) 0.060(2) -0.004(2) -0.002(2) -0.002(2) C12 0.109(3) 0.057(2) 0.057(2) 0.009(2) 0.009(2) 0.007(2) C13 0.153(5) 0.076(3) 0.068(3) 0.015(2) -0.019(3) -0.006(4) C14 0.152(4) 0.072(3) 0.080(3) 0.005(3) -0.046(3) 0.016(3) C15 0.091(2) 0.074(3) 0.066(2) 0.003(2) -0.027(2) 0.010(2) C16 0.101(3) 0.060(2) 0.089(3) 0.019(2) 0.013(3) -0.011(3) C17 0.071(3) 0.078(3) 0.177(6) -0.018(3) 0.021(3) -0.016(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 1.934(3) . ? Pd1 N1 2.051(3) . ? Pd1 O1 2.230(3) . ? Pd1 Br1 2.4131(6) . ? Fe1 C2 2.020(3) . ? Fe1 C6 2.025(4) . ? Fe1 C10 2.036(4) . ? Fe1 C4 2.037(4) . ? Fe1 C1 2.042(3) . ? Fe1 C5 2.042(4) . ? Fe1 C3 2.044(4) . ? Fe1 C8 2.051(4) . ? Fe1 C7 2.053(4) . ? Fe1 C9 2.066(4) . ? O1 C16 1.405(5) . ? O1 C17 1.434(6) . ? N1 C11 1.283(4) . ? N1 N2 1.390(4) . ? N2 C12 1.459(5) . ? N2 C15 1.467(5) . ? C1 C5 1.440(5) . ? C1 C2 1.441(5) . ? C2 C3 1.413(5) . ? C2 C11 1.426(5) . ? C3 C4 1.402(6) . ? C4 C5 1.436(6) . ? C6 C7 1.413(6) . ? C6 C10 1.419(6) . ? C7 C8 1.422(6) . ? C8 C9 1.408(6) . ? C9 C10 1.393(6) . ? C12 C16 1.518(6) . ? C12 C13 1.531(6) . ? C13 C14 1.534(8) . ? C14 C15 1.529(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Pd1 N1 80.95(13) . . ? C1 Pd1 O1 170.71(13) . . ? N1 Pd1 O1 90.36(11) . . ? C1 Pd1 Br1 92.60(10) . . ? N1 Pd1 Br1 173.37(8) . . ? O1 Pd1 Br1 95.98(8) . . ? C2 Fe1 C6 152.8(2) . . ? C2 Fe1 C10 118.26(15) . . ? C6 Fe1 C10 40.9(2) . . ? C2 Fe1 C4 68.07(15) . . ? C6 Fe1 C4 126.8(2) . . ? C10 Fe1 C4 163.1(2) . . ? C2 Fe1 C1 41.56(14) . . ? C6 Fe1 C1 117.0(2) . . ? C10 Fe1 C1 104.4(2) . . ? C4 Fe1 C1 69.24(15) . . ? C2 Fe1 C5 69.10(14) . . ? C6 Fe1 C5 106.0(2) . . ? C10 Fe1 C5 123.9(2) . . ? C4 Fe1 C5 41.2(2) . . ? C1 Fe1 C5 41.28(14) . . ? C2 Fe1 C3 40.69(14) . . ? C6 Fe1 C3 164.6(2) . . ? C10 Fe1 C3 154.0(2) . . ? C4 Fe1 C3 40.2(2) . . ? C1 Fe1 C3 69.59(15) . . ? C5 Fe1 C3 69.1(2) . . ? C2 Fe1 C8 126.1(2) . . ? C6 Fe1 C8 68.5(2) . . ? C10 Fe1 C8 67.3(2) . . ? C4 Fe1 C8 123.2(2) . . ? C1 Fe1 C8 161.4(2) . . ? C5 Fe1 C8 157.1(2) . . ? C3 Fe1 C8 110.0(2) . . ? C2 Fe1 C7 164.5(2) . . ? C6 Fe1 C7 40.6(2) . . ? C10 Fe1 C7 67.6(2) . . ? C4 Fe1 C7 110.7(2) . . ? C1 Fe1 C7 153.7(2) . . ? C5 Fe1 C7 121.0(2) . . ? C3 Fe1 C7 128.4(2) . . ? C8 Fe1 C7 40.6(2) . . ? C2 Fe1 C9 107.1(2) . . ? C6 Fe1 C9 68.2(2) . . ? C10 Fe1 C9 39.7(2) . . ? C4 Fe1 C9 156.7(2) . . ? C1 Fe1 C9 123.2(2) . . ? C5 Fe1 C9 160.5(2) . . ? C3 Fe1 C9 121.3(2) . . ? C8 Fe1 C9 40.0(2) . . ? C7 Fe1 C9 67.5(2) . . ? C16 O1 C17 110.9(3) . . ? C16 O1 Pd1 123.9(2) . . ? C17 O1 Pd1 121.7(3) . . ? C11 N1 N2 122.9(3) . . ? C11 N1 Pd1 115.5(2) . . ? N2 N1 Pd1 120.0(2) . . ? N1 N2 C12 113.9(3) . . ? N1 N2 C15 116.8(3) . . ? C12 N2 C15 110.3(3) . . ? C5 C1 C2 106.2(3) . . ? C5 C1 Pd1 140.6(3) . . ? C2 C1 Pd1 112.8(2) . . ? C5 C1 Fe1 69.4(2) . . ? C2 C1 Fe1 68.4(2) . . ? Pd1 C1 Fe1 120.6(2) . . ? C3 C2 C11 134.9(3) . . ? C3 C2 C1 109.6(3) . . ? C11 C2 C1 115.5(3) . . ? C3 C2 Fe1 70.6(2) . . ? C11 C2 Fe1 122.3(3) . . ? C1 C2 Fe1 70.0(2) . . ? C4 C3 C2 107.5(3) . . ? C4 C3 Fe1 69.6(2) . . ? C2 C3 Fe1 68.7(2) . . ? C3 C4 C5 109.4(3) . . ? C3 C4 Fe1 70.2(2) . . ? C5 C4 Fe1 69.6(2) . . ? C4 C5 C1 107.4(3) . . ? C4 C5 Fe1 69.2(2) . . ? C1 C5 Fe1 69.4(2) . . ? C7 C6 C10 106.9(4) . . ? C7 C6 Fe1 70.8(2) . . ? C10 C6 Fe1 70.0(2) . . ? C6 C7 C8 108.0(4) . . ? C6 C7 Fe1 68.7(2) . . ? C8 C7 Fe1 69.6(2) . . ? C9 C8 C7 107.9(4) . . ? C9 C8 Fe1 70.6(2) . . ? C7 C8 Fe1 69.8(2) . . ? C10 C9 C8 107.9(4) . . ? C10 C9 Fe1 69.0(2) . . ? C8 C9 Fe1 69.4(3) . . ? C9 C10 C6 109.2(4) . . ? C9 C10 Fe1 71.3(2) . . ? C6 C10 Fe1 69.1(2) . . ? N1 C11 C2 114.8(3) . . ? N2 C12 C16 110.7(3) . . ? N2 C12 C13 105.9(4) . . ? C16 C12 C13 111.5(4) . . ? C12 C13 C14 103.6(4) . . ? C15 C14 C13 105.0(4) . . ? N2 C15 C14 100.2(4) . . ? O1 C16 C12 111.8(3) . . ? _refine_diff_density_max 0.464 _refine_diff_density_min -0.652 _refine_diff_density_rms 0.093 #=END data_zgf66 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common syn-(+)-(Rp,R,R,Rp)-5 _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C48 H58 Br2 Fe2 N4 O2 Pd2' _chemical_formula_weight 1207.30 _chemical_melting_point ? _chemical_compound_source synthesized 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' 'Fe' 'Fe' 0.3463 0.8444 '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 10.654(2) _cell_length_b 13.156(3) _cell_length_c 34.577(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4846.5(17) _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 plate _exptl_crystal_colour red _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.655 _exptl_crystal_density_method ? _exptl_crystal_F_000 2416 _exptl_absorpt_coefficient_mu 3.007 _exptl_absorpt_correction_type 'ABSCOR' _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 'RIGAKU RXAIS II' _diffrn_measurement_method 'IP' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14539 _diffrn_reflns_av_R_equivalents 0.0870 _diffrn_reflns_av_sigmaI/netI 0.1017 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -42 _diffrn_reflns_limit_l_max 41 _diffrn_reflns_theta_min 1.18 _diffrn_reflns_theta_max 25.59 _reflns_number_total 8380 _reflns_number_observed 7421 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'R-AXIS' _computing_cell_refinement 'BIOTEX' _computing_data_reduction 'BIOTEX' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'SIEMENS SHELXL PC' _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 1 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^)+(0.0664P)^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 refxyz _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00108(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 0.579(8) _refine_ls_number_reflns 8379 _refine_ls_number_parameters 543 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0727 _refine_ls_R_factor_obs 0.0615 _refine_ls_wR_factor_all 0.1467 _refine_ls_wR_factor_obs 0.1387 _refine_ls_goodness_of_fit_all 1.046 _refine_ls_goodness_of_fit_obs 1.066 _refine_ls_restrained_S_all 1.060 _refine_ls_restrained_S_obs 1.066 _refine_ls_shift/esd_max -0.031 _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 0.90202(3) 0.66246(2) 0.863906(9) 0.05635(8) Uani 1 d . . Pd2 Pd 0.71473(3) 0.78581(2) 0.789844(10) 0.05738(8) Uani 1 d . . Fe1 Fe 1.17937(5) 0.68575(5) 0.92159(2) 0.0638(2) Uani 1 d . . Fe2 Fe 0.41468(5) 0.89139(4) 0.78325(2) 0.0579(2) Uani 1 d . . Br1 Br 0.94131(4) 0.80145(4) 0.81809(2) 0.08291(15) Uani 1 d . . Br2 Br 0.66758(4) 0.68854(4) 0.84821(2) 0.0867(2) Uani 1 d . . O1 O 0.6294(3) 0.3126(2) 0.86795(11) 0.0874(11) Uani 1 d . . O2 O 1.0201(5) 0.7331(6) 0.6715(2) 0.248(3) Uani 1 d . . N1 N 0.8963(3) 0.5427(3) 0.90387(10) 0.0598(9) Uani 1 d . . N2 N 0.7910(3) 0.5063(3) 0.92472(10) 0.0617(10) Uani 1 d . . N3 N 0.7222(3) 0.8680(3) 0.73810(10) 0.0674(11) Uani 1 d . . N4 N 0.8270(3) 0.9210(3) 0.72182(12) 0.0789(12) Uani 1 d . . C1 C 1.0812(4) 0.6434(3) 0.87291(11) 0.0580(11) Uani 1 d . . C2 C 1.1089(4) 0.5588(3) 0.89685(11) 0.0574(11) Uani 1 d . . C3 C 1.2430(4) 0.5501(4) 0.90151(13) 0.0645(13) Uani 1 d . . H3 H 1.2861(4) 0.5011(4) 0.91561(13) 0.077 Uiso 1 calc R . C4 C 1.2942(4) 0.6297(4) 0.88067(13) 0.0702(14) Uani 1 d . . H4 H 1.3796(4) 0.6436(4) 0.87893(13) 0.084 Uiso 1 calc R . C5 C 1.1992(4) 0.6868(4) 0.86244(13) 0.0679(13) Uani 1 d . . H5 H 1.2112(4) 0.7428(4) 0.84645(13) 0.081 Uiso 1 calc R . C6 C 1.0668(6) 0.7794(5) 0.9540(2) 0.107(2) Uani 1 d . . H6 H 0.9833(6) 0.7952(5) 0.9491(2) 0.129 Uiso 1 calc R . C7 C 1.1098(6) 0.7034(5) 0.9765(2) 0.110(2) Uani 1 d . . H7 H 1.0587(6) 0.6573(5) 0.9895(2) 0.132 Uiso 1 calc R . C8 C 1.2351(7) 0.7028(6) 0.9779(2) 0.115(2) Uani 1 d . . H8 H 1.2836(7) 0.6572(6) 0.9921(2) 0.138 Uiso 1 calc R . C9 C 1.2812(7) 0.7799(6) 0.9553(2) 0.142(2) Uani 1 d . . H9 H 1.3651(7) 0.7962(6) 0.9513(2) 0.171 Uiso 1 calc R . C10 C 1.1738(11) 0.8305(5) 0.9391(2) 0.152(4) Uani 1 d . . H10 H 1.1743(11) 0.8856(5) 0.9222(2) 0.182 Uiso 1 calc R . C11 C 1.0060(4) 0.5071(3) 0.91553(13) 0.0627(12) Uani 1 d . . C12 C 1.0227(5) 0.4249(4) 0.9446(2) 0.085(2) Uani 1 d . . H12A H 0.9420(5) 0.4014(4) 0.9531(2) 0.127 Uiso 1 calc R . H12B H 1.0689(5) 0.4507(4) 0.9663(2) 0.127 Uiso 1 calc R . H12C H 1.0681(5) 0.3696(4) 0.9331(2) 0.127 Uiso 1 calc R . C13 C 0.6951(4) 0.4613(3) 0.89948(12) 0.0610(12) Uani 1 d . . H13 H 0.6875(4) 0.4999(3) 0.87534(12) 0.073 Uiso 1 calc R . C14 C 0.5782(5) 0.4733(4) 0.9240(2) 0.097(2) Uani 1 d . . H14A H 0.5055(5) 0.4832(4) 0.9076(2) 0.116 Uiso 1 calc R . H14B H 0.5649(5) 0.4127(4) 0.9394(2) 0.116 Uiso 1 calc R . C15 C 0.5957(5) 0.5638(5) 0.9499(2) 0.097(2) Uani 1 d . . H15A H 0.5451(5) 0.6205(5) 0.9411(2) 0.116 Uiso 1 calc R . H15B H 0.5725(5) 0.5475(5) 0.9763(2) 0.116 Uiso 1 calc R . C16 C 0.7323(5) 0.5885(4) 0.94717(14) 0.0755(15) Uani 1 d . . H16A H 0.7444(5) 0.6533(4) 0.93432(14) 0.091 Uiso 1 calc R . H16B H 0.7691(5) 0.5923(4) 0.97278(14) 0.091 Uiso 1 calc R . C17 C 0.7271(4) 0.3513(3) 0.89132(14) 0.0674(13) Uani 1 d . . H17A H 0.8069(4) 0.3466(3) 0.87791(14) 0.081 Uiso 1 calc R . H17B H 0.7328(4) 0.3133(3) 0.91528(14) 0.081 Uiso 1 calc R . C18 C 0.6451(7) 0.2091(4) 0.8570(2) 0.111(2) Uani 1 d . . H18A H 0.5755(7) 0.1882(4) 0.8412(2) 0.166 Uiso 1 calc R . H18B H 0.6489(7) 0.1674(4) 0.8797(2) 0.166 Uiso 1 calc R . H18C H 0.7216(7) 0.2018(4) 0.8425(2) 0.166 Uiso 1 calc R . C19 C 0.5404(4) 0.7770(3) 0.77303(12) 0.0614(12) Uani 1 d . . C20 C 0.5118(4) 0.8321(3) 0.73839(13) 0.0609(12) Uani 1 d . . C21 C 0.3809(4) 0.8254(3) 0.73078(12) 0.0619(11) Uani 1 d . . H21 H 0.3385(4) 0.8542(3) 0.70999(12) 0.074 Uiso 1 calc R . C22 C 0.3271(4) 0.7663(3) 0.76091(14) 0.0675(13) Uani 1 d . . H22 H 0.2425(4) 0.7499(3) 0.76302(14) 0.081 Uiso 1 calc R . C23 C 0.4242(3) 0.7356(3) 0.78788(13) 0.0589(11) Uani 1 d . . H23 H 0.4139(3) 0.6971(3) 0.81020(13) 0.071 Uiso 1 calc R . C24 C 0.4964(6) 0.9845(3) 0.82360(15) 0.082(2) Uani 1 d . . H24 H 0.5760(6) 0.9761(3) 0.83418(15) 0.098 Uiso 1 calc R . C25 C 0.4654(5) 1.0417(3) 0.7894(2) 0.095(2) Uani 1 d . . H25 H 0.5209(5) 1.0781(3) 0.7739(2) 0.114 Uiso 1 calc R . C26 C 0.3332(5) 1.0316(4) 0.7838(2) 0.090(2) Uani 1 d . . H26 H 0.2878(5) 1.0607(4) 0.7637(2) 0.109 Uiso 1 calc R . C27 C 0.2839(5) 0.9733(4) 0.8124(2) 0.093(2) Uani 1 d . . H27 H 0.1999(5) 0.9555(4) 0.8150(2) 0.111 Uiso 1 calc R . C28 C 0.3838(6) 0.9437(4) 0.8380(2) 0.086(2) Uani 1 d . . H28 H 0.3754(6) 0.9045(4) 0.8602(2) 0.104 Uiso 1 calc R . C29 C 0.6159(4) 0.8824(3) 0.72103(12) 0.0623(12) Uani 1 d . . C30 C 0.5989(5) 0.9487(4) 0.68569(14) 0.086(2) Uani 1 d . . H30A H 0.6787(5) 0.9759(4) 0.67800(14) 0.129 Uiso 1 calc R . H30B H 0.5425(5) 1.0034(4) 0.69166(14) 0.129 Uiso 1 calc R . H30C H 0.5647(5) 0.9088(4) 0.66496(14) 0.129 Uiso 1 calc R . C31 C 0.9363(4) 0.8565(4) 0.7142(2) 0.086(2) Uani 1 d . . H31 H 0.9466(4) 0.8092(4) 0.7358(2) 0.104 Uiso 1 calc R . C32 C 1.0457(5) 0.9305(6) 0.7143(3) 0.135(3) Uani 1 d . . H32A H 1.1165(5) 0.9020(6) 0.7282(3) 0.162 Uiso 1 calc R . H32B H 1.0719(5) 0.9456(6) 0.6880(3) 0.162 Uiso 1 calc R . C33 C 0.9994(7) 1.0244(6) 0.7339(2) 0.132(3) Uani 1 d . . H33A H 1.0514(7) 1.0397(6) 0.7562(2) 0.158 Uiso 1 calc R . H33B H 1.0028(7) 1.0817(6) 0.7162(2) 0.158 Uiso 1 calc R . C34 C 0.8670(5) 1.0057(4) 0.7463(2) 0.100(2) Uani 1 d . . H34A H 0.8632(5) 0.9875(4) 0.7735(2) 0.119 Uiso 1 calc R . H34B H 0.8153(5) 1.0653(4) 0.7420(2) 0.119 Uiso 1 calc R . C35 C 0.9168(7) 0.7979(8) 0.6790(2) 0.157(3) Uani 1 d . . H35A H 0.8412(7) 0.7574(8) 0.6816(2) 0.189 Uiso 1 calc R . H35B H 0.9053(7) 0.8438(8) 0.6574(2) 0.189 Uiso 1 calc R . C36 C 1.0161(9) 0.6484(8) 0.6650(5) 0.274(8) Uani 1 d . . H36A H 1.0996(9) 0.6232(8) 0.6608(5) 0.411 Uiso 1 calc R . H36B H 0.9664(9) 0.6372(8) 0.6423(5) 0.411 Uiso 1 calc R . H36C H 0.9790(9) 0.6134(8) 0.6865(5) 0.411 Uiso 1 calc R . C37 C 1.1724(10) 0.4264(6) 1.0435(2) 0.156(4) Uani 1 d . . H37 H 1.1408(10) 0.3733(6) 1.0286(2) 0.187 Uiso 1 calc R . C38 C 1.0956(9) 0.4936(7) 1.0567(3) 0.162(4) Uani 1 d . . H38 H 1.0105(9) 0.4909(7) 1.0508(3) 0.194 Uiso 1 calc R . C39 C 1.1432(10) 0.5694(7) 1.0800(2) 0.154(4) Uani 1 d . . H39 H 1.0879(10) 0.6159(7) 1.0910(2) 0.185 Uiso 1 calc R . C40 C 1.2572(9) 0.5780(7) 1.0869(3) 0.162(4) Uani 1 d . . H40 H 1.2859(9) 0.6335(7) 1.1010(3) 0.195 Uiso 1 calc R . C41 C 1.3395(10) 0.5083(7) 1.0742(3) 0.187(5) Uani 1 d . . H41 H 1.4235(10) 0.5123(7) 1.0813(3) 0.224 Uiso 1 calc R . C42 C 1.2983(10) 0.4302(7) 1.0504(3) 0.175(4) Uani 1 d . . H42 H 1.3535(10) 0.3831(7) 1.0397(3) 0.210 Uiso 1 calc R . C43 C 0.7712(9) 0.3154(7) 1.0197(3) 0.155(4) Uani 1 d . . H43 H 0.7643(9) 0.3107(7) 0.9930(3) 0.186 Uiso 1 calc R . C44 C 0.8467(8) 0.2535(8) 1.0404(3) 0.179(4) Uani 1 d . . H44 H 0.8922(8) 0.2045(8) 1.0270(3) 0.215 Uiso 1 calc R . C45 C 0.8606(8) 0.2575(6) 1.0782(3) 0.156(4) Uani 1 d . . H45 H 0.9098(8) 0.2086(6) 1.0904(3) 0.187 Uiso 1 calc R . C46 C 0.8055(9) 0.3307(6) 1.1000(3) 0.152(4) Uani 1 d . . H46 H 0.8242(9) 0.3443(6) 1.1258(3) 0.182 Uiso 1 calc R . C47 C 0.7156(12) 0.3832(7) 1.0778(3) 0.236(4) Uani 1 d . . H47 H 0.6565(12) 0.4212(7) 1.0913(3) 0.283 Uiso 1 calc R . C48 C 0.7068(12) 0.3841(8) 1.0405(3) 0.204(5) Uani 1 d . . H48 H 0.6563(12) 0.4318(8) 1.0282(3) 0.245 Uiso 1 calc R . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.05555(13) 0.05798(15) 0.05553(15) 0.00649(14) -0.00324(14) -0.00100(14) Pd2 0.05636(13) 0.05227(13) 0.0635(2) 0.01032(15) 0.00046(14) 0.00026(13) Fe1 0.0609(3) 0.0707(4) 0.0599(3) -0.0062(3) -0.0012(3) -0.0035(3) Fe2 0.0606(3) 0.0507(3) 0.0623(3) -0.0010(3) -0.0016(3) -0.0029(3) Br1 0.0685(2) 0.0873(3) 0.0930(3) 0.0336(3) -0.0086(2) -0.0106(2) Br2 0.0672(2) 0.0949(3) 0.0979(3) 0.0428(3) -0.0054(2) -0.0029(2) O1 0.102(2) 0.067(2) 0.093(2) -0.007(2) -0.018(2) -0.010(2) O2 0.150(4) 0.257(6) 0.336(7) -0.153(6) 0.112(5) -0.050(5) N1 0.058(2) 0.059(2) 0.062(2) 0.003(2) 0.000(2) -0.008(2) N2 0.064(2) 0.063(2) 0.058(2) -0.001(2) 0.001(2) -0.006(2) N3 0.068(2) 0.074(2) 0.060(2) 0.015(2) 0.003(2) -0.009(2) N4 0.055(2) 0.097(2) 0.085(2) 0.039(2) 0.007(2) 0.000(2) C1 0.063(2) 0.062(2) 0.049(2) -0.006(2) -0.003(2) -0.011(2) C2 0.050(2) 0.071(2) 0.052(2) -0.008(2) -0.001(2) 0.004(2) C3 0.052(2) 0.078(3) 0.063(2) -0.002(2) -0.002(2) 0.012(2) C4 0.057(2) 0.087(3) 0.066(3) -0.003(2) 0.003(2) -0.004(2) C5 0.058(2) 0.078(3) 0.067(2) 0.008(2) 0.007(2) 0.002(2) C6 0.116(4) 0.107(4) 0.098(4) -0.028(4) 0.018(3) 0.016(4) C7 0.123(4) 0.121(4) 0.085(3) -0.029(4) 0.021(3) -0.020(4) C8 0.136(4) 0.141(5) 0.067(3) -0.027(4) -0.028(3) 0.022(4) C9 0.138(4) 0.180(5) 0.109(4) -0.079(4) 0.009(4) -0.072(4) C10 0.292(11) 0.070(3) 0.094(4) -0.026(3) 0.001(6) 0.000(6) C11 0.065(2) 0.064(2) 0.060(2) 0.004(2) -0.002(2) 0.004(2) C12 0.078(3) 0.085(3) 0.091(3) 0.037(3) -0.008(3) 0.014(3) C13 0.070(2) 0.058(2) 0.055(2) 0.008(2) -0.012(2) -0.006(2) C14 0.065(2) 0.089(3) 0.136(5) -0.031(3) 0.016(3) -0.009(3) C15 0.084(3) 0.109(4) 0.098(4) -0.015(3) 0.007(3) 0.008(3) C16 0.085(3) 0.079(3) 0.063(3) -0.012(2) 0.010(2) -0.004(3) C17 0.071(2) 0.060(2) 0.071(3) -0.004(2) -0.012(2) 0.001(2) C18 0.167(5) 0.065(3) 0.100(4) -0.019(3) -0.008(4) -0.021(4) C19 0.073(2) 0.049(2) 0.062(2) -0.003(2) 0.004(2) -0.008(2) C20 0.058(2) 0.054(2) 0.070(3) 0.004(2) -0.006(2) -0.005(2) C21 0.064(2) 0.069(2) 0.053(2) -0.004(2) -0.014(2) 0.004(2) C22 0.054(2) 0.065(2) 0.084(3) 0.004(2) -0.002(2) -0.008(2) C23 0.056(2) 0.049(2) 0.071(2) -0.002(2) 0.012(2) -0.009(2) C24 0.111(3) 0.056(2) 0.078(3) -0.006(2) -0.015(3) -0.010(3) C25 0.112(4) 0.045(2) 0.126(4) -0.009(3) 0.010(4) -0.015(2) C26 0.086(3) 0.062(2) 0.124(4) 0.006(3) 0.007(3) 0.008(2) C27 0.086(3) 0.081(3) 0.111(4) -0.039(3) 0.023(3) -0.002(3) C28 0.114(4) 0.071(3) 0.073(3) -0.010(3) 0.013(3) -0.009(3) C29 0.056(2) 0.069(2) 0.063(2) 0.004(2) -0.003(2) -0.006(2) C30 0.087(3) 0.097(3) 0.075(3) 0.034(3) -0.018(3) -0.007(3) C31 0.075(2) 0.100(4) 0.084(3) 0.006(3) 0.024(3) 0.001(3) C32 0.067(3) 0.157(5) 0.180(6) 0.063(5) 0.018(4) -0.010(4) C33 0.106(4) 0.144(5) 0.146(6) 0.051(5) -0.007(4) -0.046(4) C34 0.089(3) 0.064(3) 0.146(5) 0.030(3) -0.023(3) -0.006(2) C35 0.108(4) 0.223(8) 0.140(6) -0.048(7) 0.037(5) -0.011(6) C36 0.128(7) 0.201(9) 0.494(21) 0.147(12) 0.009(12) 0.011(8) C37 0.244(10) 0.101(5) 0.122(5) 0.006(5) -0.052(7) -0.006(6) C38 0.158(6) 0.151(6) 0.177(7) 0.057(6) -0.039(7) -0.021(7) C39 0.197(8) 0.128(6) 0.138(6) 0.027(5) 0.009(7) -0.015(6) C40 0.163(6) 0.126(6) 0.198(9) -0.019(6) -0.022(7) -0.041(5) C41 0.175(7) 0.125(6) 0.261(12) 0.045(7) -0.061(8) -0.050(6) C42 0.178(8) 0.131(7) 0.217(10) 0.019(7) 0.017(8) 0.027(7) C43 0.168(7) 0.169(7) 0.127(6) -0.029(6) -0.003(6) 0.018(7) C44 0.142(6) 0.184(7) 0.211(9) -0.083(7) -0.050(6) 0.049(6) C45 0.168(6) 0.107(5) 0.191(8) -0.014(6) -0.015(7) 0.053(4) C46 0.186(7) 0.134(6) 0.135(6) 0.029(6) 0.004(6) 0.018(6) C47 0.319(10) 0.225(7) 0.164(7) 0.094(6) 0.065(8) 0.177(6) C48 0.221(10) 0.182(7) 0.209(9) 0.104(6) -0.014(9) 0.053(7) _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 1.951(4) . ? Pd1 N1 2.097(3) . ? Pd1 Br1 2.4554(7) . ? Pd1 Br2 2.5789(7) . ? Pd2 C19 1.949(4) . ? Pd2 N3 2.092(4) . ? Pd2 Br2 2.4419(7) . ? Pd2 Br1 2.6121(7) . ? Fe1 C10 1.999(6) . ? Fe1 C4 2.011(5) . ? Fe1 C2 2.021(4) . ? Fe1 C9 2.018(7) . ? Fe1 C3 2.031(5) . ? Fe1 C8 2.049(6) . ? Fe1 C6 2.051(6) . ? Fe1 C7 2.052(6) . ? Fe1 C5 2.056(5) . ? Fe1 C1 2.058(4) . ? Fe2 C20 2.021(4) . ? Fe2 C27 2.030(5) . ? Fe2 C22 2.043(4) . ? Fe2 C26 2.039(5) . ? Fe2 C28 2.042(5) . ? Fe2 C19 2.046(4) . ? Fe2 C21 2.043(4) . ? Fe2 C24 2.051(5) . ? Fe2 C23 2.058(4) . ? Fe2 C25 2.061(5) . ? O1 C17 1.413(6) . ? O1 C18 1.424(6) . ? O2 C36 1.137(13) . ? O2 C35 1.416(10) . ? N1 C11 1.322(5) . ? N1 N2 1.417(5) . ? N2 C16 1.470(6) . ? N2 C13 1.469(5) . ? N3 C29 1.291(5) . ? N3 N4 1.432(5) . ? N4 C34 1.463(7) . ? N4 C31 1.466(6) . ? C1 C2 1.417(6) . ? C1 C5 1.427(6) . ? C2 C3 1.442(5) . ? C2 C11 1.443(6) . ? C3 C4 1.383(6) . ? C4 C5 1.409(6) . ? C6 C7 1.348(9) . ? C6 C10 1.420(12) . ? C7 C8 1.336(10) . ? C8 C9 1.372(10) . ? C9 C10 1.437(12) . ? C11 C12 1.486(7) . ? C13 C17 1.513(6) . ? C13 C14 1.515(7) . ? C14 C15 1.500(8) . ? C15 C16 1.494(8) . ? C19 C20 1.433(6) . ? C19 C23 1.447(6) . ? C20 C29 1.424(6) . ? C20 C21 1.422(6) . ? C21 C22 1.420(6) . ? C22 C23 1.450(6) . ? C24 C28 1.405(8) . ? C24 C25 1.440(8) . ? C25 C26 1.428(8) . ? C26 C27 1.357(8) . ? C27 C28 1.437(8) . ? C29 C30 1.512(6) . ? C31 C35 1.454(10) . ? C31 C32 1.519(8) . ? C32 C33 1.494(11) . ? C33 C34 1.494(9) . ? C37 C38 1.290(13) . ? C37 C42 1.363(14) . ? C38 C39 1.378(12) . ? C39 C40 1.242(13) . ? C40 C41 1.343(14) . ? C41 C42 1.387(14) . ? C43 C48 1.343(14) . ? C43 C44 1.350(13) . ? C44 C45 1.316(14) . ? C45 C46 1.356(12) . ? C46 C47 1.409(13) . ? C47 C48 1.292(14) . ? 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 80.02(15) . . ? C1 Pd1 Br1 91.84(12) . . ? N1 Pd1 Br1 171.85(9) . . ? C1 Pd1 Br2 177.02(12) . . ? N1 Pd1 Br2 102.14(9) . . ? Br1 Pd1 Br2 86.00(2) . . ? C19 Pd2 N3 79.2(2) . . ? C19 Pd2 Br2 91.10(12) . . ? N3 Pd2 Br2 170.24(10) . . ? C19 Pd2 Br1 175.24(13) . . ? N3 Pd2 Br1 104.11(10) . . ? Br2 Pd2 Br1 85.55(2) . . ? C10 Fe1 C4 125.5(3) . . ? C10 Fe1 C2 154.7(3) . . ? C4 Fe1 C2 68.0(2) . . ? C10 Fe1 C9 41.9(4) . . ? C4 Fe1 C9 107.8(2) . . ? C2 Fe1 C9 162.1(2) . . ? C10 Fe1 C3 161.8(3) . . ? C4 Fe1 C3 40.0(2) . . ? C2 Fe1 C3 41.7(2) . . ? C9 Fe1 C3 123.9(2) . . ? C10 Fe1 C8 67.4(3) . . ? C4 Fe1 C8 122.2(2) . . ? C2 Fe1 C8 126.9(2) . . ? C9 Fe1 C8 39.4(3) . . ? C3 Fe1 C8 108.9(2) . . ? C10 Fe1 C6 41.0(3) . . ? C4 Fe1 C6 163.8(2) . . ? C2 Fe1 C6 120.7(2) . . ? C9 Fe1 C6 68.3(3) . . ? C3 Fe1 C6 155.4(2) . . ? C8 Fe1 C6 65.5(3) . . ? C10 Fe1 C7 66.5(3) . . ? C4 Fe1 C7 155.9(2) . . ? C2 Fe1 C7 110.6(2) . . ? C9 Fe1 C7 65.8(3) . . ? C3 Fe1 C7 122.4(2) . . ? C8 Fe1 C7 38.0(3) . . ? C6 Fe1 C7 38.3(3) . . ? C10 Fe1 C5 107.3(2) . . ? C4 Fe1 C5 40.5(2) . . ? C2 Fe1 C5 67.8(2) . . ? C9 Fe1 C5 121.0(2) . . ? C3 Fe1 C5 68.4(2) . . ? C8 Fe1 C5 156.2(2) . . ? C6 Fe1 C5 126.8(2) . . ? C7 Fe1 C5 163.1(2) . . ? C10 Fe1 C1 119.4(3) . . ? C4 Fe1 C1 68.5(2) . . ? C2 Fe1 C1 40.7(2) . . ? C9 Fe1 C1 155.8(2) . . ? C3 Fe1 C1 69.6(2) . . ? C8 Fe1 C1 162.6(2) . . ? C6 Fe1 C1 108.2(2) . . ? C7 Fe1 C1 127.2(2) . . ? C5 Fe1 C1 40.6(2) . . ? C20 Fe2 C27 159.7(2) . . ? C20 Fe2 C22 68.4(2) . . ? C27 Fe2 C22 107.6(2) . . ? C20 Fe2 C26 125.1(2) . . ? C27 Fe2 C26 39.0(2) . . ? C22 Fe2 C26 122.6(2) . . ? C20 Fe2 C28 157.6(2) . . ? C27 Fe2 C28 41.3(2) . . ? C22 Fe2 C28 123.3(2) . . ? C26 Fe2 C28 67.5(2) . . ? C20 Fe2 C19 41.2(2) . . ? C27 Fe2 C19 157.8(2) . . ? C22 Fe2 C19 69.0(2) . . ? C26 Fe2 C19 161.1(2) . . ? C28 Fe2 C19 120.9(2) . . ? C20 Fe2 C21 41.0(2) . . ? C27 Fe2 C21 123.1(2) . . ? C22 Fe2 C21 40.7(2) . . ? C26 Fe2 C21 108.6(2) . . ? C28 Fe2 C21 159.8(2) . . ? C19 Fe2 C21 69.5(2) . . ? C20 Fe2 C24 122.4(2) . . ? C27 Fe2 C24 68.6(2) . . ? C22 Fe2 C24 158.8(2) . . ? C26 Fe2 C24 68.5(2) . . ? C28 Fe2 C24 40.2(2) . . ? C19 Fe2 C24 106.2(2) . . ? C21 Fe2 C24 158.9(2) . . ? C20 Fe2 C23 69.5(2) . . ? C27 Fe2 C23 121.6(2) . . ? C22 Fe2 C23 41.4(2) . . ? C26 Fe2 C23 157.1(2) . . ? C28 Fe2 C23 105.8(2) . . ? C19 Fe2 C23 41.3(2) . . ? C21 Fe2 C23 69.8(2) . . ? C24 Fe2 C23 121.4(2) . . ? C20 Fe2 C25 108.4(2) . . ? C27 Fe2 C25 67.6(2) . . ? C22 Fe2 C25 158.7(2) . . ? C26 Fe2 C25 40.8(2) . . ? C28 Fe2 C25 67.8(2) . . ? C19 Fe2 C25 123.5(2) . . ? C21 Fe2 C25 123.1(2) . . ? C24 Fe2 C25 41.0(2) . . ? C23 Fe2 C25 159.1(2) . . ? Pd1 Br1 Pd2 91.43(2) . . ? Pd2 Br2 Pd1 92.54(2) . . ? C17 O1 C18 114.2(4) . . ? C36 O2 C35 126.6(8) . . ? C11 N1 N2 115.2(3) . . ? C11 N1 Pd1 116.2(3) . . ? N2 N1 Pd1 127.8(2) . . ? N1 N2 C16 110.9(3) . . ? N1 N2 C13 112.6(3) . . ? C16 N2 C13 108.3(3) . . ? C29 N3 N4 115.6(3) . . ? C29 N3 Pd2 115.7(3) . . ? N4 N3 Pd2 128.2(3) . . ? N3 N4 C34 111.8(4) . . ? N3 N4 C31 114.1(4) . . ? C34 N4 C31 108.3(4) . . ? C2 C1 C5 106.2(4) . . ? C2 C1 Pd1 113.4(3) . . ? C5 C1 Pd1 140.3(3) . . ? C2 C1 Fe1 68.2(2) . . ? C5 C1 Fe1 69.6(2) . . ? Pd1 C1 Fe1 126.4(2) . . ? C1 C2 C3 109.5(4) . . ? C1 C2 C11 118.2(4) . . ? C3 C2 C11 131.7(4) . . ? C1 C2 Fe1 71.1(2) . . ? C3 C2 Fe1 69.5(2) . . ? C11 C2 Fe1 118.8(3) . . ? C4 C3 C2 105.8(4) . . ? C4 C3 Fe1 69.2(3) . . ? C2 C3 Fe1 68.8(2) . . ? C3 C4 C5 110.7(4) . . ? C3 C4 Fe1 70.8(3) . . ? C5 C4 Fe1 71.5(3) . . ? C4 C5 C1 107.8(4) . . ? C4 C5 Fe1 68.0(3) . . ? C1 C5 Fe1 69.8(2) . . ? C7 C6 C10 106.8(6) . . ? C7 C6 Fe1 70.9(4) . . ? C10 C6 Fe1 67.5(4) . . ? C8 C7 C6 111.4(6) . . ? C8 C7 Fe1 70.9(4) . . ? C6 C7 Fe1 70.8(4) . . ? C7 C8 C9 109.4(6) . . ? C7 C8 Fe1 71.1(4) . . ? C9 C8 Fe1 69.1(4) . . ? C8 C9 C10 106.3(7) . . ? C8 C9 Fe1 71.5(4) . . ? C10 C9 Fe1 68.3(4) . . ? C6 C10 C9 106.1(6) . . ? C6 C10 Fe1 71.5(4) . . ? C9 C10 Fe1 69.7(4) . . ? N1 C11 C2 111.6(4) . . ? N1 C11 C12 124.7(4) . . ? C2 C11 C12 123.6(4) . . ? N2 C13 C17 109.8(3) . . ? N2 C13 C14 101.4(4) . . ? C17 C13 C14 112.9(4) . . ? C15 C14 C13 108.3(4) . . ? C16 C15 C14 104.9(4) . . ? N2 C16 C15 106.7(4) . . ? O1 C17 C13 106.6(3) . . ? C20 C19 C23 107.7(4) . . ? C20 C19 Pd2 115.0(3) . . ? C23 C19 Pd2 137.1(3) . . ? C20 C19 Fe2 68.5(2) . . ? C23 C19 Fe2 69.8(2) . . ? Pd2 C19 Fe2 121.9(2) . . ? C29 C20 C21 135.6(4) . . ? C29 C20 C19 115.0(4) . . ? C21 C20 C19 109.4(4) . . ? C29 C20 Fe2 122.8(3) . . ? C21 C20 Fe2 70.4(2) . . ? C19 C20 Fe2 70.3(2) . . ? C20 C21 C22 107.1(4) . . ? C20 C21 Fe2 68.7(2) . . ? C22 C21 Fe2 69.6(2) . . ? C21 C22 C23 109.7(3) . . ? C21 C22 Fe2 69.7(2) . . ? C23 C22 Fe2 69.9(2) . . ? C22 C23 C19 106.1(4) . . ? C22 C23 Fe2 68.7(2) . . ? C19 C23 Fe2 68.9(2) . . ? C28 C24 C25 107.2(5) . . ? C28 C24 Fe2 69.6(3) . . ? C25 C24 Fe2 69.9(3) . . ? C26 C25 C24 106.7(5) . . ? C26 C25 Fe2 68.8(3) . . ? C24 C25 Fe2 69.1(3) . . ? C27 C26 C25 109.6(5) . . ? C27 C26 Fe2 70.1(3) . . ? C25 C26 Fe2 70.4(3) . . ? C26 C27 C28 108.4(5) . . ? C26 C27 Fe2 70.9(3) . . ? C28 C27 Fe2 69.8(3) . . ? C24 C28 C27 108.1(5) . . ? C24 C28 Fe2 70.3(3) . . ? C27 C28 Fe2 68.9(3) . . ? N3 C29 C20 114.9(4) . . ? N3 C29 C30 124.0(4) . . ? C20 C29 C30 121.0(4) . . ? C35 C31 N4 110.2(5) . . ? C35 C31 C32 116.9(6) . . ? N4 C31 C32 103.8(4) . . ? C33 C32 C31 106.1(5) . . ? C34 C33 C32 107.8(5) . . ? N4 C34 C33 103.5(5) . . ? O2 C35 C31 111.2(6) . . ? C38 C37 C42 122.5(9) . . ? C37 C38 C39 118.1(10) . . ? C40 C39 C38 122.5(10) . . ? C39 C40 C41 120.9(10) . . ? C40 C41 C42 119.6(10) . . ? C37 C42 C41 116.3(9) . . ? C48 C43 C44 115.2(9) . . ? C45 C44 C43 124.7(9) . . ? C44 C45 C46 122.1(9) . . ? C45 C46 C47 109.8(8) . . ? C48 C47 C46 126.7(11) . . ? C47 C48 C43 119.4(10) . . ? _refine_diff_density_max 0.593 _refine_diff_density_min -1.211 _refine_diff_density_rms 0.113