Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Jun-Fang Gong' _publ_contact_author_address ; Department of Chemistry Zhengzhou University Daxue Road 75, Department of Chemis Zhengzhou 450052 CHINA ; _publ_contact_author_email GONGJF@ZZU.EDU.CN _publ_section_title ; Tricyclohexylphosphine adducts of cyclopalladated ferrocenylimines: Synthesis, crystal structures and application in Suzuki and Heck reactions ; loop_ _publ_author_name 'Jun-Fang Gong' 'Yang-Jie Wu' 'Chen Xu' 'Su-Fang Yue' 'Yu Zhu' # Attachment 'Complex 2c .cif' data_p21n_2c _database_code_depnum_ccdc_archive 'CCDC 284580' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C35 H53 Cl Fe N P Pd' _chemical_formula_weight 716.45 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.668(2) _cell_length_b 14.320(3) _cell_length_c 22.676(5) _cell_angle_alpha 90.00 _cell_angle_beta 102.72(3) _cell_angle_gamma 90.00 _cell_volume 3379.1(12) _cell_formula_units_Z 4 _cell_measurement_temperature 291(2) _cell_measurement_reflns_used 378 _cell_measurement_theta_min 2 _cell_measurement_theta_max 25.1 _exptl_crystal_description prismatic _exptl_crystal_colour red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.408 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1496 _exptl_absorpt_coefficient_mu 1.112 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8082 _exptl_absorpt_correction_T_max 0.8335 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 291(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type R-AXIS-IV _diffrn_measurement_method 'Oscillation frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 9523 _diffrn_reflns_av_R_equivalents 0.0260 _diffrn_reflns_av_sigmaI/netI 0.0413 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.69 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5461 _reflns_number_gt 4527 _reflns_threshold_expression >2sigma(I) _computing_data_collection raxis _computing_cell_refinement raxis _computing_data_reduction raxis _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics texsan _computing_publication_material texsan _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0345P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5461 _refine_ls_number_parameters 361 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0503 _refine_ls_R_factor_gt 0.0317 _refine_ls_wR_factor_ref 0.0696 _refine_ls_wR_factor_gt 0.0663 _refine_ls_goodness_of_fit_ref 1.067 _refine_ls_restrained_S_all 1.067 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.38785(2) 0.292891(15) 0.162872(10) 0.03498(8) Uani 1 1 d . . . Fe1 Fe 0.30173(4) 0.19362(3) 0.29134(2) 0.04299(12) Uani 1 1 d . . . P1 P 0.25745(7) 0.24470(5) 0.07520(3) 0.03339(18) Uani 1 1 d . . . Cl1 Cl 0.41282(10) 0.44601(6) 0.12550(4) 0.0676(3) Uani 1 1 d . . . N1 N 0.5473(2) 0.31370(16) 0.23818(11) 0.0393(6) Uani 1 1 d . . . C1 C 0.1901(7) 0.3090(4) 0.2892(2) 0.0985(18) Uani 1 1 d . . . H1A H 0.1597 0.3487 0.2538 0.118 Uiso 1 1 calc R . . C2 C 0.1284(5) 0.2347(4) 0.3040(3) 0.1015(17) Uani 1 1 d . . . H2A H 0.0451 0.2115 0.2815 0.122 Uiso 1 1 calc R . . C3 C 0.1990(7) 0.1972(3) 0.3560(3) 0.0997(19) Uani 1 1 d . . . H3A H 0.1747 0.1429 0.3774 0.120 Uiso 1 1 calc R . . C4 C 0.3076(6) 0.2494(5) 0.3741(2) 0.1080(19) Uani 1 1 d . . . H4A H 0.3751 0.2402 0.4106 0.130 Uiso 1 1 calc R . . C5 C 0.3019(7) 0.3210(4) 0.3308(4) 0.116(3) Uani 1 1 d . . . H5A H 0.3649 0.3710 0.3314 0.140 Uiso 1 1 calc R . . C6 C 0.3661(3) 0.18011(19) 0.21149(13) 0.0367(7) Uani 1 1 d . . . C7 C 0.2767(3) 0.1078(2) 0.21752(14) 0.0444(8) Uani 1 1 d . . . H7A H 0.1947 0.0962 0.1891 0.053 Uiso 1 1 calc R . . C8 C 0.3241(3) 0.0570(2) 0.27163(15) 0.0506(9) Uani 1 1 d . . . H8A H 0.2811 0.0041 0.2862 0.061 Uiso 1 1 calc R . . C9 C 0.4421(3) 0.0963(2) 0.30130(15) 0.0510(9) Uani 1 1 d . . . H9A H 0.4966 0.0751 0.3395 0.061 Uiso 1 1 calc R . . C10 C 0.4680(3) 0.1729(2) 0.26482(14) 0.0417(7) Uani 1 1 d . . . C11 C 0.5611(3) 0.2472(2) 0.27639(14) 0.0447(8) Uani 1 1 d . . . H11A H 0.6285 0.2466 0.3103 0.054 Uiso 1 1 calc R . . C12 C 0.6335(3) 0.3956(2) 0.24700(14) 0.0458(8) Uani 1 1 d . . . H12A H 0.6349 0.4192 0.2066 0.055 Uiso 1 1 calc R . . C13 C 0.5769(3) 0.4724(2) 0.27882(17) 0.0617(10) Uani 1 1 d . . . H13A H 0.5748 0.4524 0.3195 0.074 Uiso 1 1 calc R . . H13B H 0.4894 0.4848 0.2573 0.074 Uiso 1 1 calc R . . C14 C 0.6570(4) 0.5619(3) 0.2818(2) 0.0786(12) Uani 1 1 d . . . H14A H 0.6505 0.5858 0.2412 0.094 Uiso 1 1 calc R . . H14B H 0.6228 0.6088 0.3048 0.094 Uiso 1 1 calc R . . C15 C 0.7963(4) 0.5441(3) 0.31087(19) 0.0785(13) Uani 1 1 d . . . H15A H 0.8456 0.6006 0.3090 0.094 Uiso 1 1 calc R . . H15B H 0.8040 0.5283 0.3531 0.094 Uiso 1 1 calc R . . C16 C 0.8504(4) 0.4659(3) 0.2797(2) 0.0759(12) Uani 1 1 d . . . H16A H 0.9384 0.4539 0.3007 0.091 Uiso 1 1 calc R . . H16B H 0.8512 0.4846 0.2386 0.091 Uiso 1 1 calc R . . C17 C 0.7719(3) 0.3767(3) 0.27815(18) 0.0668(11) Uani 1 1 d . . . H17A H 0.8071 0.3284 0.2566 0.080 Uiso 1 1 calc R . . H17B H 0.7760 0.3550 0.3191 0.080 Uiso 1 1 calc R . . C18 C 0.0871(3) 0.27926(19) 0.06424(13) 0.0365(7) Uani 1 1 d . . . H18A H 0.0435 0.2611 0.0232 0.044 Uiso 1 1 calc R . . C19 C 0.0180(3) 0.2311(2) 0.10827(15) 0.0486(8) Uani 1 1 d . . . H19A H 0.0617 0.2456 0.1495 0.058 Uiso 1 1 calc R . . H19B H 0.0208 0.1640 0.1029 0.058 Uiso 1 1 calc R . . C20 C -0.1223(3) 0.2632(2) 0.09766(18) 0.0629(11) Uani 1 1 d . . . H20A H -0.1679 0.2427 0.0579 0.075 Uiso 1 1 calc R . . H20B H -0.1626 0.2339 0.1274 0.075 Uiso 1 1 calc R . . C21 C -0.1341(4) 0.3681(2) 0.10195(18) 0.0645(10) Uani 1 1 d . . . H21A H -0.0967 0.3884 0.1429 0.077 Uiso 1 1 calc R . . H21B H -0.2241 0.3857 0.0926 0.077 Uiso 1 1 calc R . . C22 C -0.0657(3) 0.4157(2) 0.05809(16) 0.0558(9) Uani 1 1 d . . . H22A H -0.0705 0.4829 0.0626 0.067 Uiso 1 1 calc R . . H22B H -0.1084 0.3998 0.0170 0.067 Uiso 1 1 calc R . . C23 C 0.0749(3) 0.3861(2) 0.06934(15) 0.0482(8) Uani 1 1 d . . . H23A H 0.1192 0.4061 0.1094 0.058 Uiso 1 1 calc R . . H23B H 0.1155 0.4162 0.0401 0.058 Uiso 1 1 calc R . . C24 C 0.2554(3) 0.11622(19) 0.06251(13) 0.0367(7) Uani 1 1 d . . . H24A H 0.2077 0.0898 0.0909 0.044 Uiso 1 1 calc R . . C25 C 0.1843(3) 0.0835(2) -0.00025(14) 0.0490(8) Uani 1 1 d . . . H25A H 0.2299 0.1048 -0.0303 0.059 Uiso 1 1 calc R . . H25B H 0.0988 0.1104 -0.0098 0.059 Uiso 1 1 calc R . . C26 C 0.1744(3) -0.0232(2) -0.00221(18) 0.0654(11) Uani 1 1 d . . . H26A H 0.1227 -0.0440 0.0255 0.078 Uiso 1 1 calc R . . H26B H 0.1319 -0.0429 -0.0426 0.078 Uiso 1 1 calc R . . C27 C 0.3068(4) -0.0683(2) 0.01492(18) 0.0673(11) Uani 1 1 d . . . H27A H 0.2973 -0.1356 0.0161 0.081 Uiso 1 1 calc R . . H27B H 0.3547 -0.0537 -0.0157 0.081 Uiso 1 1 calc R . . C28 C 0.3806(3) -0.0346(2) 0.07539(17) 0.0563(9) Uani 1 1 d . . . H28A H 0.4668 -0.0603 0.0831 0.068 Uiso 1 1 calc R . . H28B H 0.3393 -0.0574 0.1067 0.068 Uiso 1 1 calc R . . C29 C 0.3888(3) 0.0715(2) 0.07885(15) 0.0437(8) Uani 1 1 d . . . H29A H 0.4400 0.0939 0.0513 0.052 Uiso 1 1 calc R . . H29B H 0.4313 0.0901 0.1195 0.052 Uiso 1 1 calc R . . C30 C 0.3125(3) 0.3038(2) 0.01252(12) 0.0372(7) Uani 1 1 d . . . H30A H 0.3211 0.3694 0.0249 0.045 Uiso 1 1 calc R . . C31 C 0.2244(3) 0.3066(2) -0.05096(13) 0.0455(8) Uani 1 1 d . . . H31A H 0.2182 0.2449 -0.0690 0.055 Uiso 1 1 calc R . . H31B H 0.1388 0.3265 -0.0484 0.055 Uiso 1 1 calc R . . C32 C 0.2809(3) 0.3751(2) -0.08971(14) 0.0489(8) Uani 1 1 d . . . H32A H 0.2265 0.3769 -0.1300 0.059 Uiso 1 1 calc R . . H32B H 0.2822 0.4372 -0.0725 0.059 Uiso 1 1 calc R . . C33 C 0.4151(3) 0.3484(2) -0.09382(15) 0.0543(9) Uani 1 1 d . . . H33A H 0.4484 0.3943 -0.1178 0.065 Uiso 1 1 calc R . . H33B H 0.4134 0.2883 -0.1138 0.065 Uiso 1 1 calc R . . C34 C 0.5031(3) 0.3428(3) -0.03075(16) 0.0563(9) Uani 1 1 d . . . H34A H 0.5879 0.3222 -0.0341 0.068 Uiso 1 1 calc R . . H34B H 0.5116 0.4043 -0.0124 0.068 Uiso 1 1 calc R . . C35 C 0.4492(3) 0.2750(2) 0.00940(15) 0.0501(8) Uani 1 1 d . . . H35A H 0.5037 0.2749 0.0497 0.060 Uiso 1 1 calc R . . H35B H 0.4482 0.2122 -0.0068 0.060 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.04023(14) 0.03308(13) 0.03094(13) 0.00052(10) 0.00631(10) -0.00629(11) Fe1 0.0505(3) 0.0431(3) 0.0401(3) 0.0027(2) 0.0202(2) -0.0014(2) P1 0.0347(4) 0.0337(4) 0.0317(4) -0.0021(3) 0.0072(3) -0.0021(3) Cl1 0.0998(8) 0.0400(4) 0.0507(5) 0.0077(4) -0.0101(5) -0.0254(5) N1 0.0361(14) 0.0438(15) 0.0366(14) 0.0014(12) 0.0050(12) -0.0022(11) C1 0.151(5) 0.068(3) 0.094(4) 0.009(3) 0.066(4) 0.046(3) C2 0.063(3) 0.108(4) 0.144(6) -0.046(4) 0.043(4) 0.006(3) C3 0.143(5) 0.079(3) 0.110(4) 0.020(3) 0.098(4) 0.017(4) C4 0.097(4) 0.170(6) 0.056(3) -0.039(4) 0.014(3) 0.030(4) C5 0.130(5) 0.080(4) 0.178(6) -0.076(4) 0.118(5) -0.048(4) C6 0.0392(17) 0.0347(16) 0.0388(17) -0.0028(13) 0.0145(15) -0.0029(13) C7 0.051(2) 0.0397(17) 0.0443(19) 0.0003(15) 0.0146(16) -0.0071(15) C8 0.066(2) 0.0346(17) 0.057(2) 0.0104(16) 0.025(2) -0.0019(16) C9 0.056(2) 0.0478(19) 0.049(2) 0.0155(16) 0.0110(18) 0.0065(17) C10 0.0443(19) 0.0401(17) 0.0409(18) 0.0031(14) 0.0097(15) 0.0032(14) C11 0.0355(18) 0.054(2) 0.0414(19) 0.0024(16) 0.0022(15) 0.0027(15) C12 0.0448(19) 0.0480(19) 0.0421(19) 0.0006(15) 0.0044(16) -0.0151(15) C13 0.047(2) 0.067(2) 0.070(3) -0.018(2) 0.0110(19) -0.0115(18) C14 0.080(3) 0.062(3) 0.091(3) -0.023(2) 0.013(3) -0.023(2) C15 0.068(3) 0.091(3) 0.070(3) -0.011(2) 0.002(2) -0.041(2) C16 0.046(2) 0.093(3) 0.087(3) -0.004(3) 0.011(2) -0.026(2) C17 0.046(2) 0.074(3) 0.078(3) 0.001(2) 0.009(2) -0.0113(19) C18 0.0348(16) 0.0389(16) 0.0357(16) -0.0027(13) 0.0079(13) 0.0005(13) C19 0.0443(19) 0.0462(19) 0.060(2) 0.0052(16) 0.0216(17) 0.0037(15) C20 0.044(2) 0.059(2) 0.093(3) 0.014(2) 0.031(2) 0.0043(17) C21 0.056(2) 0.063(2) 0.081(3) 0.006(2) 0.029(2) 0.0183(18) C22 0.059(2) 0.0451(19) 0.066(2) 0.0038(17) 0.020(2) 0.0161(17) C23 0.051(2) 0.0412(17) 0.056(2) 0.0026(15) 0.0187(17) 0.0048(15) C24 0.0368(17) 0.0380(16) 0.0365(17) -0.0021(13) 0.0104(14) -0.0042(13) C25 0.045(2) 0.0452(18) 0.052(2) -0.0131(16) 0.0008(17) -0.0014(15) C26 0.058(2) 0.049(2) 0.083(3) -0.0209(19) 0.001(2) -0.0057(18) C27 0.069(3) 0.0404(19) 0.090(3) -0.017(2) 0.014(2) 0.0025(18) C28 0.053(2) 0.0408(18) 0.075(3) 0.0035(18) 0.015(2) 0.0041(16) C29 0.0399(18) 0.0394(17) 0.051(2) -0.0013(15) 0.0077(16) 0.0027(14) C30 0.0386(17) 0.0406(17) 0.0323(16) -0.0017(13) 0.0081(13) -0.0029(14) C31 0.0415(18) 0.058(2) 0.0370(17) 0.0002(15) 0.0089(15) -0.0067(15) C32 0.054(2) 0.053(2) 0.0386(18) 0.0067(15) 0.0074(16) -0.0066(16) C33 0.063(2) 0.054(2) 0.053(2) 0.0084(17) 0.0289(19) -0.0054(18) C34 0.043(2) 0.064(2) 0.067(2) 0.0147(19) 0.0231(19) 0.0001(17) C35 0.0425(19) 0.059(2) 0.051(2) 0.0100(17) 0.0147(16) 0.0012(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 C6 1.998(3) . ? Pd1 N1 2.150(3) . ? Pd1 P1 2.2685(10) . ? Pd1 Cl1 2.3868(9) . ? Fe1 C3 2.015(4) . ? Fe1 C10 2.016(3) . ? Fe1 C2 2.020(4) . ? Fe1 C9 2.021(3) . ? Fe1 C4 2.027(4) . ? Fe1 C5 2.031(4) . ? Fe1 C1 2.031(4) . ? Fe1 C8 2.033(3) . ? Fe1 C7 2.046(3) . ? Fe1 C6 2.082(3) . ? P1 C18 1.847(3) . ? P1 C30 1.857(3) . ? P1 C24 1.862(3) . ? N1 C11 1.274(4) . ? N1 C12 1.476(4) . ? C1 C2 1.332(7) . ? C1 C5 1.359(7) . ? C1 H1A 0.9800 . ? C2 C3 1.362(7) . ? C2 H2A 0.9800 . ? C3 C4 1.364(7) . ? C3 H3A 0.9800 . ? C4 C5 1.411(8) . ? C4 H4A 0.9800 . ? C5 H5A 0.9800 . ? C6 C7 1.434(4) . ? C6 C10 1.440(4) . ? C7 C8 1.421(4) . ? C7 H7A 0.9800 . ? C8 C9 1.408(5) . ? C8 H8A 0.9800 . ? C9 C10 1.436(4) . ? C9 H9A 0.9800 . ? C10 C11 1.440(4) . ? C11 H11A 0.9300 . ? C12 C13 1.513(4) . ? C12 C17 1.513(5) . ? C12 H12A 0.9800 . ? C13 C14 1.533(5) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 C15 1.509(5) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 C16 1.506(6) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 C17 1.524(5) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 C19 1.530(4) . ? C18 C23 1.541(4) . ? C18 H18A 0.9800 . ? C19 C20 1.533(4) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 C21 1.513(5) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 C22 1.519(4) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 C23 1.525(4) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 C29 1.530(4) . ? C24 C25 1.531(4) . ? C24 H24A 0.9800 . ? C25 C26 1.532(4) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 C27 1.524(5) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C27 C28 1.502(5) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 C29 1.523(4) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C30 C35 1.531(4) . ? C30 C31 1.537(4) . ? C30 H30A 0.9800 . ? C31 C32 1.527(4) . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C32 C33 1.504(4) . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C33 C34 1.531(5) . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C34 C35 1.528(4) . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? 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 C6 Pd1 N1 80.87(11) . . ? C6 Pd1 P1 96.58(9) . . ? N1 Pd1 P1 164.54(7) . . ? C6 Pd1 Cl1 167.00(8) . . ? N1 Pd1 Cl1 91.38(7) . . ? P1 Pd1 Cl1 93.62(3) . . ? C3 Fe1 C10 151.1(2) . . ? C3 Fe1 C2 39.5(2) . . ? C10 Fe1 C2 168.0(2) . . ? C3 Fe1 C9 116.37(19) . . ? C10 Fe1 C9 41.68(12) . . ? C2 Fe1 C9 149.7(2) . . ? C3 Fe1 C4 39.4(2) . . ? C10 Fe1 C4 119.0(2) . . ? C2 Fe1 C4 66.2(2) . . ? C9 Fe1 C4 107.27(19) . . ? C3 Fe1 C5 66.73(19) . . ? C10 Fe1 C5 110.37(16) . . ? C2 Fe1 C5 65.7(2) . . ? C9 Fe1 C5 129.9(3) . . ? C4 Fe1 C5 40.7(2) . . ? C3 Fe1 C1 65.57(19) . . ? C10 Fe1 C1 131.5(2) . . ? C2 Fe1 C1 38.4(2) . . ? C9 Fe1 C1 168.4(3) . . ? C4 Fe1 C1 66.4(2) . . ? C5 Fe1 C1 39.1(2) . . ? C3 Fe1 C8 107.04(17) . . ? C10 Fe1 C8 68.84(13) . . ? C2 Fe1 C8 117.8(2) . . ? C9 Fe1 C8 40.63(13) . . ? C4 Fe1 C8 127.0(2) . . ? C5 Fe1 C8 166.5(3) . . ? C1 Fe1 C8 151.0(3) . . ? C3 Fe1 C7 128.1(2) . . ? C10 Fe1 C7 68.42(13) . . ? C2 Fe1 C7 109.39(18) . . ? C9 Fe1 C7 68.74(14) . . ? C4 Fe1 C7 164.9(3) . . ? C5 Fe1 C7 152.5(3) . . ? C1 Fe1 C7 119.9(2) . . ? C8 Fe1 C7 40.77(12) . . ? C3 Fe1 C6 166.3(2) . . ? C10 Fe1 C6 41.12(12) . . ? C2 Fe1 C6 129.6(2) . . ? C9 Fe1 C6 69.82(12) . . ? C4 Fe1 C6 153.2(3) . . ? C5 Fe1 C6 119.86(19) . . ? C1 Fe1 C6 111.05(16) . . ? C8 Fe1 C6 69.04(11) . . ? C7 Fe1 C6 40.64(11) . . ? C18 P1 C30 104.05(13) . . ? C18 P1 C24 105.45(13) . . ? C30 P1 C24 109.07(13) . . ? C18 P1 Pd1 115.58(10) . . ? C30 P1 Pd1 107.21(10) . . ? C24 P1 Pd1 114.85(10) . . ? C11 N1 C12 121.8(3) . . ? C11 N1 Pd1 112.9(2) . . ? C12 N1 Pd1 125.33(19) . . ? C2 C1 C5 109.5(5) . . ? C2 C1 Fe1 70.3(3) . . ? C5 C1 Fe1 70.5(3) . . ? C2 C1 H1A 125.3 . . ? C5 C1 H1A 125.3 . . ? Fe1 C1 H1A 125.3 . . ? C1 C2 C3 108.8(5) . . ? C1 C2 Fe1 71.3(3) . . ? C3 C2 Fe1 70.1(3) . . ? C1 C2 H2A 125.6 . . ? C3 C2 H2A 125.6 . . ? Fe1 C2 H2A 125.6 . . ? C2 C3 C4 108.4(5) . . ? C2 C3 Fe1 70.5(3) . . ? C4 C3 Fe1 70.8(3) . . ? C2 C3 H3A 125.8 . . ? C4 C3 H3A 125.8 . . ? Fe1 C3 H3A 125.8 . . ? C3 C4 C5 106.6(5) . . ? C3 C4 Fe1 69.8(3) . . ? C5 C4 Fe1 69.8(3) . . ? C3 C4 H4A 126.7 . . ? C5 C4 H4A 126.7 . . ? Fe1 C4 H4A 126.7 . . ? C1 C5 C4 106.7(5) . . ? C1 C5 Fe1 70.5(3) . . ? C4 C5 Fe1 69.5(3) . . ? C1 C5 H5A 126.6 . . ? C4 C5 H5A 126.6 . . ? Fe1 C5 H5A 126.6 . . ? C7 C6 C10 105.2(3) . . ? C7 C6 Pd1 142.8(2) . . ? C10 C6 Pd1 111.3(2) . . ? C7 C6 Fe1 68.32(16) . . ? C10 C6 Fe1 66.97(16) . . ? Pd1 C6 Fe1 120.35(13) . . ? C8 C7 C6 109.6(3) . . ? C8 C7 Fe1 69.13(18) . . ? C6 C7 Fe1 71.04(17) . . ? C8 C7 H7A 125.2 . . ? C6 C7 H7A 125.2 . . ? Fe1 C7 H7A 125.2 . . ? C9 C8 C7 108.5(3) . . ? C9 C8 Fe1 69.23(18) . . ? C7 C8 Fe1 70.10(17) . . ? C9 C8 H8A 125.7 . . ? C7 C8 H8A 125.7 . . ? Fe1 C8 H8A 125.7 . . ? C8 C9 C10 107.2(3) . . ? C8 C9 Fe1 70.14(19) . . ? C10 C9 Fe1 68.97(17) . . ? C8 C9 H9A 126.4 . . ? C10 C9 H9A 126.4 . . ? Fe1 C9 H9A 126.4 . . ? C9 C10 C11 132.2(3) . . ? C9 C10 C6 109.5(3) . . ? C11 C10 C6 117.5(3) . . ? C9 C10 Fe1 69.35(18) . . ? C11 C10 Fe1 117.0(2) . . ? C6 C10 Fe1 71.91(16) . . ? N1 C11 C10 117.2(3) . . ? N1 C11 H11A 121.4 . . ? C10 C11 H11A 121.4 . . ? N1 C12 C13 109.9(2) . . ? N1 C12 C17 115.8(3) . . ? C13 C12 C17 111.0(3) . . ? N1 C12 H12A 106.5 . . ? C13 C12 H12A 106.5 . . ? C17 C12 H12A 106.5 . . ? C12 C13 C14 110.6(3) . . ? C12 C13 H13A 109.5 . . ? C14 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? C14 C13 H13B 109.5 . . ? H13A C13 H13B 108.1 . . ? C15 C14 C13 111.4(3) . . ? C15 C14 H14A 109.4 . . ? C13 C14 H14A 109.4 . . ? C15 C14 H14B 109.4 . . ? C13 C14 H14B 109.4 . . ? H14A C14 H14B 108.0 . . ? C16 C15 C14 111.2(3) . . ? C16 C15 H15A 109.4 . . ? C14 C15 H15A 109.4 . . ? C16 C15 H15B 109.4 . . ? C14 C15 H15B 109.4 . . ? H15A C15 H15B 108.0 . . ? C15 C16 C17 111.6(3) . . ? C15 C16 H16A 109.3 . . ? C17 C16 H16A 109.3 . . ? C15 C16 H16B 109.3 . . ? C17 C16 H16B 109.3 . . ? H16A C16 H16B 108.0 . . ? C12 C17 C16 109.6(3) . . ? C12 C17 H17A 109.7 . . ? C16 C17 H17A 109.7 . . ? C12 C17 H17B 109.7 . . ? C16 C17 H17B 109.7 . . ? H17A C17 H17B 108.2 . . ? C19 C18 C23 109.7(2) . . ? C19 C18 P1 113.1(2) . . ? C23 C18 P1 110.7(2) . . ? C19 C18 H18A 107.7 . . ? C23 C18 H18A 107.7 . . ? P1 C18 H18A 107.7 . . ? C18 C19 C20 110.9(3) . . ? C18 C19 H19A 109.5 . . ? C20 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? C20 C19 H19B 109.5 . . ? H19A C19 H19B 108.0 . . ? C21 C20 C19 112.3(3) . . ? C21 C20 H20A 109.1 . . ? C19 C20 H20A 109.1 . . ? C21 C20 H20B 109.1 . . ? C19 C20 H20B 109.1 . . ? H20A C20 H20B 107.9 . . ? C20 C21 C22 110.2(3) . . ? C20 C21 H21A 109.6 . . ? C22 C21 H21A 109.6 . . ? C20 C21 H21B 109.6 . . ? C22 C21 H21B 109.6 . . ? H21A C21 H21B 108.1 . . ? C21 C22 C23 111.2(3) . . ? C21 C22 H22A 109.4 . . ? C23 C22 H22A 109.4 . . ? C21 C22 H22B 109.4 . . ? C23 C22 H22B 109.4 . . ? H22A C22 H22B 108.0 . . ? C22 C23 C18 111.1(3) . . ? C22 C23 H23A 109.4 . . ? C18 C23 H23A 109.4 . . ? C22 C23 H23B 109.4 . . ? C18 C23 H23B 109.4 . . ? H23A C23 H23B 108.0 . . ? C29 C24 C25 110.0(2) . . ? C29 C24 P1 113.4(2) . . ? C25 C24 P1 115.6(2) . . ? C29 C24 H24A 105.6 . . ? C25 C24 H24A 105.6 . . ? P1 C24 H24A 105.6 . . ? C24 C25 C26 110.4(3) . . ? C24 C25 H25A 109.6 . . ? C26 C25 H25A 109.6 . . ? C24 C25 H25B 109.6 . . ? C26 C25 H25B 109.6 . . ? H25A C25 H25B 108.1 . . ? C27 C26 C25 111.2(3) . . ? C27 C26 H26A 109.4 . . ? C25 C26 H26A 109.4 . . ? C27 C26 H26B 109.4 . . ? C25 C26 H26B 109.4 . . ? H26A C26 H26B 108.0 . . ? C28 C27 C26 111.5(3) . . ? C28 C27 H27A 109.3 . . ? C26 C27 H27A 109.3 . . ? C28 C27 H27B 109.3 . . ? C26 C27 H27B 109.3 . . ? H27A C27 H27B 108.0 . . ? C27 C28 C29 112.3(3) . . ? C27 C28 H28A 109.1 . . ? C29 C28 H28A 109.1 . . ? C27 C28 H28B 109.1 . . ? C29 C28 H28B 109.1 . . ? H28A C28 H28B 107.9 . . ? C28 C29 C24 111.4(3) . . ? C28 C29 H29A 109.3 . . ? C24 C29 H29A 109.3 . . ? C28 C29 H29B 109.3 . . ? C24 C29 H29B 109.3 . . ? H29A C29 H29B 108.0 . . ? C35 C30 C31 110.9(2) . . ? C35 C30 P1 112.2(2) . . ? C31 C30 P1 119.8(2) . . ? C35 C30 H30A 104.0 . . ? C31 C30 H30A 104.0 . . ? P1 C30 H30A 104.0 . . ? C32 C31 C30 108.6(2) . . ? C32 C31 H31A 110.0 . . ? C30 C31 H31A 110.0 . . ? C32 C31 H31B 110.0 . . ? C30 C31 H31B 110.0 . . ? H31A C31 H31B 108.4 . . ? C33 C32 C31 112.0(3) . . ? C33 C32 H32A 109.2 . . ? C31 C32 H32A 109.2 . . ? C33 C32 H32B 109.2 . . ? C31 C32 H32B 109.2 . . ? H32A C32 H32B 107.9 . . ? C32 C33 C34 110.6(3) . . ? C32 C33 H33A 109.5 . . ? C34 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? C34 C33 H33B 109.5 . . ? H33A C33 H33B 108.1 . . ? C35 C34 C33 110.8(3) . . ? C35 C34 H34A 109.5 . . ? C33 C34 H34A 109.5 . . ? C35 C34 H34B 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 108.1 . . ? C34 C35 C30 110.1(3) . . ? C34 C35 H35A 109.6 . . ? C30 C35 H35A 109.6 . . ? C34 C35 H35B 109.6 . . ? C30 C35 H35B 109.6 . . ? H35A C35 H35B 108.2 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 Pd1 P1 C18 90.72(13) . . . . ? N1 Pd1 P1 C18 170.2(3) . . . . ? Cl1 Pd1 P1 C18 -81.20(10) . . . . ? C6 Pd1 P1 C30 -153.81(13) . . . . ? N1 Pd1 P1 C30 -74.3(3) . . . . ? Cl1 Pd1 P1 C30 34.28(10) . . . . ? C6 Pd1 P1 C24 -32.45(13) . . . . ? N1 Pd1 P1 C24 47.0(3) . . . . ? Cl1 Pd1 P1 C24 155.64(10) . . . . ? C6 Pd1 N1 C11 3.3(2) . . . . ? P1 Pd1 N1 C11 -78.3(3) . . . . ? Cl1 Pd1 N1 C11 172.8(2) . . . . ? C6 Pd1 N1 C12 -176.0(2) . . . . ? P1 Pd1 N1 C12 102.4(3) . . . . ? Cl1 Pd1 N1 C12 -6.5(2) . . . . ? C3 Fe1 C1 C2 -37.6(4) . . . . ? C10 Fe1 C1 C2 170.4(3) . . . . ? C9 Fe1 C1 C2 -140.0(8) . . . . ? C4 Fe1 C1 C2 -81.0(4) . . . . ? C5 Fe1 C1 C2 -120.2(5) . . . . ? C8 Fe1 C1 C2 43.5(6) . . . . ? C7 Fe1 C1 C2 83.7(4) . . . . ? C6 Fe1 C1 C2 127.9(4) . . . . ? C3 Fe1 C1 C5 82.6(4) . . . . ? C10 Fe1 C1 C5 -69.4(4) . . . . ? C2 Fe1 C1 C5 120.2(5) . . . . ? C9 Fe1 C1 C5 -19.8(10) . . . . ? C4 Fe1 C1 C5 39.2(3) . . . . ? C8 Fe1 C1 C5 163.7(4) . . . . ? C7 Fe1 C1 C5 -156.1(3) . . . . ? C6 Fe1 C1 C5 -111.9(3) . . . . ? C5 C1 C2 C3 0.5(5) . . . . ? Fe1 C1 C2 C3 60.3(3) . . . . ? C5 C1 C2 Fe1 -59.8(3) . . . . ? C3 Fe1 C2 C1 119.0(5) . . . . ? C10 Fe1 C2 C1 -36.7(10) . . . . ? C9 Fe1 C2 C1 165.1(4) . . . . ? C4 Fe1 C2 C1 81.5(4) . . . . ? C5 Fe1 C2 C1 36.7(3) . . . . ? C8 Fe1 C2 C1 -157.8(4) . . . . ? C7 Fe1 C2 C1 -114.0(4) . . . . ? C6 Fe1 C2 C1 -72.9(4) . . . . ? C10 Fe1 C2 C3 -155.7(7) . . . . ? C9 Fe1 C2 C3 46.1(5) . . . . ? C4 Fe1 C2 C3 -37.6(3) . . . . ? C5 Fe1 C2 C3 -82.3(4) . . . . ? C1 Fe1 C2 C3 -119.0(5) . . . . ? C8 Fe1 C2 C3 83.1(4) . . . . ? C7 Fe1 C2 C3 126.9(3) . . . . ? C6 Fe1 C2 C3 168.1(3) . . . . ? C1 C2 C3 C4 -0.2(5) . . . . ? Fe1 C2 C3 C4 60.9(3) . . . . ? C1 C2 C3 Fe1 -61.0(3) . . . . ? C10 Fe1 C3 C2 169.8(3) . . . . ? C9 Fe1 C3 C2 -156.1(3) . . . . ? C4 Fe1 C3 C2 118.6(5) . . . . ? C5 Fe1 C3 C2 79.5(4) . . . . ? C1 Fe1 C3 C2 36.6(3) . . . . ? C8 Fe1 C3 C2 -113.3(4) . . . . ? C7 Fe1 C3 C2 -73.3(4) . . . . ? C6 Fe1 C3 C2 -42.1(8) . . . . ? C10 Fe1 C3 C4 51.2(5) . . . . ? C2 Fe1 C3 C4 -118.6(5) . . . . ? C9 Fe1 C3 C4 85.3(4) . . . . ? C5 Fe1 C3 C4 -39.1(4) . . . . ? C1 Fe1 C3 C4 -82.0(4) . . . . ? C8 Fe1 C3 C4 128.1(4) . . . . ? C7 Fe1 C3 C4 168.1(3) . . . . ? C6 Fe1 C3 C4 -160.6(6) . . . . ? C2 C3 C4 C5 -0.2(5) . . . . ? Fe1 C3 C4 C5 60.4(3) . . . . ? C2 C3 C4 Fe1 -60.7(3) . . . . ? C10 Fe1 C4 C3 -154.6(3) . . . . ? C2 Fe1 C4 C3 37.6(3) . . . . ? C9 Fe1 C4 C3 -110.8(4) . . . . ? C5 Fe1 C4 C3 117.3(5) . . . . ? C1 Fe1 C4 C3 79.7(4) . . . . ? C8 Fe1 C4 C3 -70.3(4) . . . . ? C7 Fe1 C4 C3 -38.6(9) . . . . ? C6 Fe1 C4 C3 170.0(3) . . . . ? C3 Fe1 C4 C5 -117.3(5) . . . . ? C10 Fe1 C4 C5 88.1(4) . . . . ? C2 Fe1 C4 C5 -79.8(4) . . . . ? C9 Fe1 C4 C5 131.9(4) . . . . ? C1 Fe1 C4 C5 -37.7(3) . . . . ? C8 Fe1 C4 C5 172.4(3) . . . . ? C7 Fe1 C4 C5 -155.9(6) . . . . ? C6 Fe1 C4 C5 52.6(6) . . . . ? C2 C1 C5 C4 -0.7(5) . . . . ? Fe1 C1 C5 C4 -60.4(3) . . . . ? C2 C1 C5 Fe1 59.7(3) . . . . ? C3 C4 C5 C1 0.6(5) . . . . ? Fe1 C4 C5 C1 61.0(3) . . . . ? C3 C4 C5 Fe1 -60.4(3) . . . . ? C3 Fe1 C5 C1 -79.4(3) . . . . ? C10 Fe1 C5 C1 131.6(3) . . . . ? C2 Fe1 C5 C1 -36.1(3) . . . . ? C9 Fe1 C5 C1 174.9(3) . . . . ? C4 Fe1 C5 C1 -117.3(4) . . . . ? C8 Fe1 C5 C1 -144.3(7) . . . . ? C7 Fe1 C5 C1 49.5(5) . . . . ? C6 Fe1 C5 C1 87.1(3) . . . . ? C3 Fe1 C5 C4 37.9(3) . . . . ? C10 Fe1 C5 C4 -111.1(4) . . . . ? C2 Fe1 C5 C4 81.2(3) . . . . ? C9 Fe1 C5 C4 -67.8(4) . . . . ? C1 Fe1 C5 C4 117.3(4) . . . . ? C8 Fe1 C5 C4 -27.0(9) . . . . ? C7 Fe1 C5 C4 166.7(3) . . . . ? C6 Fe1 C5 C4 -155.6(3) . . . . ? N1 Pd1 C6 C7 165.3(4) . . . . ? P1 Pd1 C6 C7 -30.1(3) . . . . ? Cl1 Pd1 C6 C7 111.3(5) . . . . ? N1 Pd1 C6 C10 -3.43(19) . . . . ? P1 Pd1 C6 C10 161.18(18) . . . . ? Cl1 Pd1 C6 C10 -57.4(5) . . . . ? N1 Pd1 C6 Fe1 71.63(16) . . . . ? P1 Pd1 C6 Fe1 -123.77(14) . . . . ? Cl1 Pd1 C6 Fe1 17.6(5) . . . . ? C3 Fe1 C6 C7 -38.8(7) . . . . ? C10 Fe1 C6 C7 118.4(2) . . . . ? C2 Fe1 C6 C7 -72.4(3) . . . . ? C9 Fe1 C6 C7 80.5(2) . . . . ? C4 Fe1 C6 C7 169.0(4) . . . . ? C5 Fe1 C6 C7 -154.3(3) . . . . ? C1 Fe1 C6 C7 -111.9(3) . . . . ? C8 Fe1 C6 C7 36.98(19) . . . . ? C3 Fe1 C6 C10 -157.2(7) . . . . ? C2 Fe1 C6 C10 169.2(3) . . . . ? C9 Fe1 C6 C10 -37.91(18) . . . . ? C4 Fe1 C6 C10 50.6(5) . . . . ? C5 Fe1 C6 C10 87.3(3) . . . . ? C1 Fe1 C6 C10 129.7(3) . . . . ? C8 Fe1 C6 C10 -81.44(19) . . . . ? C7 Fe1 C6 C10 -118.4(2) . . . . ? C3 Fe1 C6 Pd1 100.7(7) . . . . ? C10 Fe1 C6 Pd1 -102.1(2) . . . . ? C2 Fe1 C6 Pd1 67.1(3) . . . . ? C9 Fe1 C6 Pd1 -140.0(2) . . . . ? C4 Fe1 C6 Pd1 -51.5(5) . . . . ? C5 Fe1 C6 Pd1 -14.8(3) . . . . ? C1 Fe1 C6 Pd1 27.6(3) . . . . ? C8 Fe1 C6 Pd1 176.5(2) . . . . ? C7 Fe1 C6 Pd1 139.5(3) . . . . ? C10 C6 C7 C8 -1.5(3) . . . . ? Pd1 C6 C7 C8 -170.6(3) . . . . ? Fe1 C6 C7 C8 -58.5(2) . . . . ? C10 C6 C7 Fe1 57.02(19) . . . . ? Pd1 C6 C7 Fe1 -112.1(3) . . . . ? C3 Fe1 C7 C8 -70.2(3) . . . . ? C10 Fe1 C7 C8 82.2(2) . . . . ? C2 Fe1 C7 C8 -110.4(3) . . . . ? C9 Fe1 C7 C8 37.27(19) . . . . ? C4 Fe1 C7 C8 -40.0(7) . . . . ? C5 Fe1 C7 C8 175.1(4) . . . . ? C1 Fe1 C7 C8 -151.3(3) . . . . ? C6 Fe1 C7 C8 120.7(3) . . . . ? C3 Fe1 C7 C6 169.1(3) . . . . ? C10 Fe1 C7 C6 -38.45(17) . . . . ? C2 Fe1 C7 C6 128.9(3) . . . . ? C9 Fe1 C7 C6 -83.39(19) . . . . ? C4 Fe1 C7 C6 -160.7(7) . . . . ? C5 Fe1 C7 C6 54.5(4) . . . . ? C1 Fe1 C7 C6 88.0(3) . . . . ? C8 Fe1 C7 C6 -120.7(3) . . . . ? C6 C7 C8 C9 1.0(4) . . . . ? Fe1 C7 C8 C9 -58.7(2) . . . . ? C6 C7 C8 Fe1 59.7(2) . . . . ? C3 Fe1 C8 C9 -110.9(3) . . . . ? C10 Fe1 C8 C9 38.86(19) . . . . ? C2 Fe1 C8 C9 -152.2(3) . . . . ? C4 Fe1 C8 C9 -72.1(3) . . . . ? C5 Fe1 C8 C9 -50.4(7) . . . . ? C1 Fe1 C8 C9 178.9(3) . . . . ? C7 Fe1 C8 C9 119.9(3) . . . . ? C6 Fe1 C8 C9 83.1(2) . . . . ? C3 Fe1 C8 C7 129.2(3) . . . . ? C10 Fe1 C8 C7 -81.1(2) . . . . ? C2 Fe1 C8 C7 87.9(3) . . . . ? C9 Fe1 C8 C7 -119.9(3) . . . . ? C4 Fe1 C8 C7 167.9(3) . . . . ? C5 Fe1 C8 C7 -170.3(6) . . . . ? C1 Fe1 C8 C7 59.0(4) . . . . ? C6 Fe1 C8 C7 -36.87(18) . . . . ? C7 C8 C9 C10 0.0(4) . . . . ? Fe1 C8 C9 C10 -59.3(2) . . . . ? C7 C8 C9 Fe1 59.3(2) . . . . ? C3 Fe1 C9 C8 85.7(3) . . . . ? C10 Fe1 C9 C8 -118.4(3) . . . . ? C2 Fe1 C9 C8 54.9(4) . . . . ? C4 Fe1 C9 C8 127.2(3) . . . . ? C5 Fe1 C9 C8 166.4(3) . . . . ? C1 Fe1 C9 C8 -177.4(8) . . . . ? C7 Fe1 C9 C8 -37.39(18) . . . . ? C6 Fe1 C9 C8 -81.0(2) . . . . ? C3 Fe1 C9 C10 -155.9(3) . . . . ? C2 Fe1 C9 C10 173.3(4) . . . . ? C4 Fe1 C9 C10 -114.4(3) . . . . ? C5 Fe1 C9 C10 -75.2(3) . . . . ? C1 Fe1 C9 C10 -59.1(9) . . . . ? C8 Fe1 C9 C10 118.4(3) . . . . ? C7 Fe1 C9 C10 80.99(19) . . . . ? C6 Fe1 C9 C10 37.42(18) . . . . ? C8 C9 C10 C11 168.2(3) . . . . ? Fe1 C9 C10 C11 108.2(3) . . . . ? C8 C9 C10 C6 -1.0(3) . . . . ? Fe1 C9 C10 C6 -61.0(2) . . . . ? C8 C9 C10 Fe1 60.0(2) . . . . ? C7 C6 C10 C9 1.5(3) . . . . ? Pd1 C6 C10 C9 174.5(2) . . . . ? Fe1 C6 C10 C9 59.4(2) . . . . ? C7 C6 C10 C11 -169.5(3) . . . . ? Pd1 C6 C10 C11 3.5(3) . . . . ? Fe1 C6 C10 C11 -111.6(3) . . . . ? C7 C6 C10 Fe1 -57.88(19) . . . . ? Pd1 C6 C10 Fe1 115.05(15) . . . . ? C3 Fe1 C10 C9 49.2(4) . . . . ? C2 Fe1 C10 C9 -163.6(8) . . . . ? C4 Fe1 C10 C9 83.6(3) . . . . ? C5 Fe1 C10 C9 127.7(3) . . . . ? C1 Fe1 C10 C9 166.7(3) . . . . ? C8 Fe1 C10 C9 -37.9(2) . . . . ? C7 Fe1 C10 C9 -81.8(2) . . . . ? C6 Fe1 C10 C9 -119.9(3) . . . . ? C3 Fe1 C10 C11 -78.7(4) . . . . ? C2 Fe1 C10 C11 68.5(9) . . . . ? C9 Fe1 C10 C11 -127.8(3) . . . . ? C4 Fe1 C10 C11 -44.2(4) . . . . ? C5 Fe1 C10 C11 -0.2(4) . . . . ? C1 Fe1 C10 C11 38.8(4) . . . . ? C8 Fe1 C10 C11 -165.7(3) . . . . ? C7 Fe1 C10 C11 150.3(3) . . . . ? C6 Fe1 C10 C11 112.3(3) . . . . ? C3 Fe1 C10 C6 169.0(3) . . . . ? C2 Fe1 C10 C6 -43.8(9) . . . . ? C9 Fe1 C10 C6 119.9(3) . . . . ? C4 Fe1 C10 C6 -156.5(3) . . . . ? C5 Fe1 C10 C6 -112.5(3) . . . . ? C1 Fe1 C10 C6 -73.5(3) . . . . ? C8 Fe1 C10 C6 81.95(18) . . . . ? C7 Fe1 C10 C6 38.03(16) . . . . ? C12 N1 C11 C10 177.1(3) . . . . ? Pd1 N1 C11 C10 -2.3(3) . . . . ? C9 C10 C11 N1 -169.2(3) . . . . ? C6 C10 C11 N1 -0.6(4) . . . . ? Fe1 C10 C11 N1 -83.3(3) . . . . ? C11 N1 C12 C13 -92.8(4) . . . . ? Pd1 N1 C12 C13 86.5(3) . . . . ? C11 N1 C12 C17 33.9(4) . . . . ? Pd1 N1 C12 C17 -146.7(2) . . . . ? N1 C12 C13 C14 -173.4(3) . . . . ? C17 C12 C13 C14 57.2(4) . . . . ? C12 C13 C14 C15 -55.0(5) . . . . ? C13 C14 C15 C16 54.3(5) . . . . ? C14 C15 C16 C17 -55.9(5) . . . . ? N1 C12 C17 C16 175.8(3) . . . . ? C13 C12 C17 C16 -58.0(4) . . . . ? C15 C16 C17 C12 57.4(5) . . . . ? C30 P1 C18 C19 175.0(2) . . . . ? C24 P1 C18 C19 60.2(2) . . . . ? Pd1 P1 C18 C19 -67.8(2) . . . . ? C30 P1 C18 C23 -61.4(2) . . . . ? C24 P1 C18 C23 -176.2(2) . . . . ? Pd1 P1 C18 C23 55.8(2) . . . . ? C23 C18 C19 C20 55.2(4) . . . . ? P1 C18 C19 C20 179.3(2) . . . . ? C18 C19 C20 C21 -56.1(4) . . . . ? C19 C20 C21 C22 55.9(4) . . . . ? C20 C21 C22 C23 -56.4(4) . . . . ? C21 C22 C23 C18 57.6(4) . . . . ? C19 C18 C23 C22 -56.5(4) . . . . ? P1 C18 C23 C22 177.9(2) . . . . ? C18 P1 C24 C29 -171.3(2) . . . . ? C30 P1 C24 C29 77.5(2) . . . . ? Pd1 P1 C24 C29 -42.9(2) . . . . ? C18 P1 C24 C25 60.4(2) . . . . ? C30 P1 C24 C25 -50.9(3) . . . . ? Pd1 P1 C24 C25 -171.21(19) . . . . ? C29 C24 C25 C26 57.4(3) . . . . ? P1 C24 C25 C26 -172.6(2) . . . . ? C24 C25 C26 C27 -57.0(4) . . . . ? C25 C26 C27 C28 55.0(4) . . . . ? C26 C27 C28 C29 -53.7(4) . . . . ? C27 C28 C29 C24 54.7(4) . . . . ? C25 C24 C29 C28 -56.0(3) . . . . ? P1 C24 C29 C28 172.7(2) . . . . ? C18 P1 C30 C35 -173.6(2) . . . . ? C24 P1 C30 C35 -61.5(2) . . . . ? Pd1 P1 C30 C35 63.4(2) . . . . ? C18 P1 C30 C31 -41.0(3) . . . . ? C24 P1 C30 C31 71.1(3) . . . . ? Pd1 P1 C30 C31 -163.9(2) . . . . ? C35 C30 C31 C32 -58.1(3) . . . . ? P1 C30 C31 C32 168.7(2) . . . . ? C30 C31 C32 C33 58.3(3) . . . . ? C31 C32 C33 C34 -57.7(4) . . . . ? C32 C33 C34 C35 56.0(4) . . . . ? C33 C34 C35 C30 -56.2(4) . . . . ? C31 C30 C35 C34 58.0(3) . . . . ? P1 C30 C35 C34 -165.0(2) . . . . ? _diffrn_measured_fraction_theta_max 0.918 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.918 _refine_diff_density_max 0.699 _refine_diff_density_min -0.592 _refine_diff_density_rms 0.055 # Attachment 'Complex 2e .CIF' data_p-1_2e _database_code_depnum_ccdc_archive 'CCDC 600773' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C37 H50 Br Cl3 Fe N P Pd' _chemical_formula_weight 888.26 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.118(2) _cell_length_b 11.126(2) _cell_length_c 18.050(4) _cell_angle_alpha 102.98(3) _cell_angle_beta 93.17(3) _cell_angle_gamma 105.25(3) _cell_volume 1896.0(7) _cell_formula_units_Z 2 _cell_measurement_temperature 291(2) _cell_measurement_reflns_used 356 _cell_measurement_theta_min 2 _cell_measurement_theta_max 25.1 _exptl_crystal_description PRISMATIC _exptl_crystal_colour Red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.556 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 904 _exptl_absorpt_coefficient_mu 2.191 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6684 _exptl_absorpt_correction_T_max 0.7071 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 291(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type R-AXIS-IV _diffrn_measurement_method 'Oscillation frames' _diffrn_detector_area_resol_mean 0 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% ? _diffrn_reflns_number 5862 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0516 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.96 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5862 _reflns_number_gt 4746 _reflns_threshold_expression >2sigma(I) _computing_data_collection raxis _computing_cell_refinement raxis _computing_data_reduction raxis _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics texsan _computing_publication_material texsan _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0755P)^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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0045(6) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 5862 _refine_ls_number_parameters 407 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0579 _refine_ls_R_factor_gt 0.0428 _refine_ls_wR_factor_ref 0.1192 _refine_ls_wR_factor_gt 0.1125 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.035 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 1.24694(4) 0.51335(4) 0.30606(2) 0.02666(14) Uani 1 1 d . . . Br1 Br 0.87446(6) 0.87470(6) 0.59989(4) 0.04905(19) Uani 1 1 d . . . Fe1 Fe 1.58788(7) 0.73560(7) 0.36026(4) 0.0357(2) Uani 1 1 d . . . P1 P 1.23908(13) 0.38232(12) 0.18772(7) 0.0272(3) Uani 1 1 d . . . Cl1 Cl 1.00493(13) 0.49406(13) 0.29276(8) 0.0394(3) Uani 1 1 d . . . Cl2 Cl 1.8339(3) 0.6853(4) 0.12620(19) 0.1394(12) Uani 1 1 d . . . Cl3 Cl 2.0820(4) 0.8510(3) 0.22100(19) 0.1341(11) Uani 1 1 d . . . N1 N 1.2686(4) 0.6198(4) 0.4256(2) 0.0330(10) Uani 1 1 d . . . C1 C 1.6603(7) 0.9284(6) 0.4167(4) 0.0617(19) Uani 1 1 d . . . H1A H 1.7077 0.9636 0.4690 0.074 Uiso 1 1 calc R . . C2 C 1.7236(6) 0.9042(6) 0.3492(4) 0.0573(18) Uani 1 1 d . . . H2A H 1.8231 0.9186 0.3473 0.069 Uiso 1 1 calc R . . C3 C 1.6209(7) 0.8528(6) 0.2848(4) 0.0580(18) Uani 1 1 d . . . H3A H 1.6365 0.8276 0.2311 0.070 Uiso 1 1 calc R . . C4 C 1.4911(7) 0.8461(6) 0.3128(4) 0.0554(17) Uani 1 1 d . . . H4A H 1.4011 0.8148 0.2814 0.066 Uiso 1 1 calc R . . C5 C 1.5136(6) 0.8928(6) 0.3947(4) 0.0531(17) Uani 1 1 d . . . H5A H 1.4428 0.9000 0.4290 0.064 Uiso 1 1 calc R . . C6 C 1.4524(5) 0.5520(5) 0.3323(3) 0.0326(12) Uani 1 1 d . . . C7 C 1.5784(5) 0.5505(5) 0.3005(3) 0.0358(12) Uani 1 1 d . . . H7A H 1.5871 0.5237 0.2458 0.043 Uiso 1 1 calc R . . C8 C 1.6910(5) 0.5976(5) 0.3617(3) 0.0387(13) Uani 1 1 d . . . H8A H 1.7888 0.6079 0.3557 0.046 Uiso 1 1 calc R . . C9 C 1.6374(6) 0.6310(5) 0.4310(3) 0.0424(14) Uani 1 1 d . . . H9A H 1.6910 0.6661 0.4818 0.051 Uiso 1 1 calc R . . C10 C 1.4901(5) 0.6030(5) 0.4150(3) 0.0321(12) Uani 1 1 d . . . C11 C 1.3898(6) 0.6430(5) 0.4609(3) 0.0370(13) Uani 1 1 d . . . C12 C 1.4391(6) 0.7161(6) 0.5428(3) 0.0507(16) Uani 1 1 d . . . H12A H 1.3632 0.7372 0.5671 0.076 Uiso 1 1 calc R . . H12B H 1.5098 0.7938 0.5443 0.076 Uiso 1 1 calc R . . H12C H 1.4758 0.6640 0.5694 0.076 Uiso 1 1 calc R . . C13 C 1.1679(5) 0.6702(5) 0.4633(3) 0.0326(12) Uani 1 1 d . . . C14 C 1.1177(5) 0.7596(5) 0.4352(3) 0.0355(12) Uani 1 1 d . . . H14A H 1.1443 0.7798 0.3899 0.043 Uiso 1 1 calc R . . C15 C 1.0285(6) 0.8175(5) 0.4749(3) 0.0387(13) Uani 1 1 d . . . H15A H 0.9960 0.8776 0.4568 0.046 Uiso 1 1 calc R . . C16 C 0.9877(5) 0.7855(5) 0.5418(3) 0.0369(13) Uani 1 1 d . . . C17 C 1.0324(6) 0.6949(6) 0.5696(3) 0.0435(14) Uani 1 1 d . . . H17A H 1.0046 0.6745 0.6146 0.052 Uiso 1 1 calc R . . C18 C 1.1192(6) 0.6356(5) 0.5289(3) 0.0404(13) Uani 1 1 d . . . H18A H 1.1459 0.5712 0.5455 0.048 Uiso 1 1 calc R . . C19 C 1.3626(5) 0.2859(5) 0.1826(3) 0.0288(11) Uani 1 1 d . . . H19A H 1.4535 0.3478 0.1870 0.035 Uiso 1 1 calc R . . C20 C 1.3694(6) 0.2255(5) 0.2521(3) 0.0385(13) Uani 1 1 d . . . H20A H 1.3813 0.2913 0.2994 0.046 Uiso 1 1 calc R . . H20B H 1.2835 0.1598 0.2501 0.046 Uiso 1 1 calc R . . C21 C 1.4892(6) 0.1662(6) 0.2509(3) 0.0458(15) Uani 1 1 d . . . H21A H 1.5755 0.2335 0.2579 0.055 Uiso 1 1 calc R . . H21B H 1.4895 0.1257 0.2932 0.055 Uiso 1 1 calc R . . C22 C 1.4795(6) 0.0676(6) 0.1767(4) 0.0488(15) Uani 1 1 d . . . H22A H 1.3974 -0.0037 0.1719 0.059 Uiso 1 1 calc R . . H22B H 1.5591 0.0345 0.1772 0.059 Uiso 1 1 calc R . . C23 C 1.4734(6) 0.1261(6) 0.1084(3) 0.0482(15) Uani 1 1 d . . . H23A H 1.4627 0.0600 0.0613 0.058 Uiso 1 1 calc R . . H23B H 1.5593 0.1920 0.1107 0.058 Uiso 1 1 calc R . . C24 C 1.3520(6) 0.1856(6) 0.1079(3) 0.0424(14) Uani 1 1 d . . . H24A H 1.3524 0.2255 0.0653 0.051 Uiso 1 1 calc R . . H24B H 1.2656 0.1184 0.1011 0.051 Uiso 1 1 calc R . . C25 C 1.2737(5) 0.4715(5) 0.1127(3) 0.0310(11) Uani 1 1 d . . . H25A H 1.2570 0.4083 0.0631 0.037 Uiso 1 1 calc R . . C26 C 1.4231(6) 0.5572(5) 0.1218(3) 0.0415(13) Uani 1 1 d . . . H26A H 1.4452 0.6148 0.1727 0.050 Uiso 1 1 calc R . . H26B H 1.4853 0.5036 0.1169 0.050 Uiso 1 1 calc R . . C27 C 1.4453(6) 0.6362(6) 0.0624(4) 0.0520(16) Uani 1 1 d . . . H27A H 1.4354 0.5791 0.0119 0.062 Uiso 1 1 calc R . . H27B H 1.5383 0.6938 0.0728 0.062 Uiso 1 1 calc R . . C28 C 1.3413(7) 0.7153(6) 0.0635(4) 0.0564(17) Uani 1 1 d . . . H28A H 1.3570 0.7782 0.1123 0.068 Uiso 1 1 calc R . . H28B H 1.3551 0.7613 0.0235 0.068 Uiso 1 1 calc R . . C29 C 1.1944(7) 0.6296(6) 0.0512(4) 0.0578(17) Uani 1 1 d . . . H29A H 1.1760 0.5716 0.0005 0.069 Uiso 1 1 calc R . . H29B H 1.1309 0.6819 0.0544 0.069 Uiso 1 1 calc R . . C30 C 1.1713(6) 0.5517(6) 0.1113(4) 0.0444(14) Uani 1 1 d . . . H30A H 1.0780 0.4947 0.1009 0.053 Uiso 1 1 calc R . . H30B H 1.1805 0.6099 0.1614 0.053 Uiso 1 1 calc R . . C31 C 1.0625(5) 0.2727(5) 0.1539(3) 0.0314(11) Uani 1 1 d . . . H31A H 1.0008 0.3275 0.1643 0.038 Uiso 1 1 calc R . . C32 C 1.0271(5) 0.2053(5) 0.0677(3) 0.0399(13) Uani 1 1 d . . . H32A H 1.0508 0.2687 0.0378 0.048 Uiso 1 1 calc R . . H32B H 1.0805 0.1446 0.0540 0.048 Uiso 1 1 calc R . . C33 C 0.8741(5) 0.1350(6) 0.0497(3) 0.0442(14) Uani 1 1 d . . . H33A H 0.8538 0.0897 -0.0041 0.053 Uiso 1 1 calc R . . H33B H 0.8214 0.1971 0.0588 0.053 Uiso 1 1 calc R . . C34 C 0.8301(6) 0.0392(6) 0.0984(4) 0.0553(17) Uani 1 1 d . . . H34A H 0.7313 -0.0004 0.0873 0.066 Uiso 1 1 calc R . . H34B H 0.8754 -0.0281 0.0852 0.066 Uiso 1 1 calc R . . C35 C 0.8663(6) 0.1037(6) 0.1829(4) 0.0517(16) Uani 1 1 d . . . H35A H 0.8420 0.0396 0.2122 0.062 Uiso 1 1 calc R . . H35B H 0.8135 0.1648 0.1974 0.062 Uiso 1 1 calc R . . C36 C 1.0202(5) 0.1736(5) 0.2018(3) 0.0426(14) Uani 1 1 d . . . H36A H 1.0729 0.1117 0.1912 0.051 Uiso 1 1 calc R . . H36C H 1.0408 0.2169 0.2558 0.051 Uiso 1 1 calc R . . C37 C 1.9274(10) 0.7264(10) 0.2150(6) 0.104(3) Uani 1 1 d . . . H37C H 1.9499 0.6515 0.2249 0.125 Uiso 1 1 calc R . . H37A H 1.8721 0.7548 0.2538 0.125 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.0306(2) 0.0244(2) 0.0228(2) 0.00167(16) 0.00245(15) 0.00786(15) Br1 0.0522(4) 0.0564(4) 0.0390(4) 0.0031(3) 0.0137(3) 0.0218(3) Fe1 0.0359(4) 0.0282(4) 0.0378(5) 0.0025(3) -0.0010(3) 0.0059(3) P1 0.0348(7) 0.0230(7) 0.0226(7) 0.0033(5) 0.0016(5) 0.0086(5) Cl1 0.0363(7) 0.0436(8) 0.0381(8) 0.0031(6) 0.0036(6) 0.0168(6) Cl2 0.130(2) 0.179(3) 0.118(3) 0.037(2) 0.0112(19) 0.058(2) Cl3 0.195(3) 0.0682(16) 0.136(3) 0.0084(16) 0.012(2) 0.0469(18) N1 0.033(2) 0.034(3) 0.026(2) 0.0016(19) -0.0007(18) 0.0059(18) C1 0.074(5) 0.027(3) 0.066(5) -0.005(3) -0.009(4) 0.001(3) C2 0.043(3) 0.036(4) 0.084(5) 0.016(3) 0.001(3) -0.002(3) C3 0.067(4) 0.035(4) 0.068(5) 0.014(3) 0.004(4) 0.006(3) C4 0.061(4) 0.034(3) 0.071(5) 0.017(3) -0.005(3) 0.013(3) C5 0.054(4) 0.033(3) 0.074(5) 0.011(3) 0.018(3) 0.016(3) C6 0.045(3) 0.023(3) 0.027(3) 0.002(2) 0.006(2) 0.009(2) C7 0.042(3) 0.030(3) 0.033(3) 0.000(2) 0.003(2) 0.013(2) C8 0.027(3) 0.034(3) 0.049(4) 0.005(3) 0.001(2) 0.006(2) C9 0.044(3) 0.035(3) 0.045(4) 0.004(3) -0.004(3) 0.012(2) C10 0.031(3) 0.028(3) 0.034(3) 0.005(2) -0.003(2) 0.007(2) C11 0.053(3) 0.029(3) 0.025(3) 0.003(2) -0.004(2) 0.011(2) C12 0.057(4) 0.059(4) 0.024(3) -0.001(3) -0.003(3) 0.009(3) C13 0.037(3) 0.026(3) 0.029(3) -0.001(2) 0.005(2) 0.005(2) C14 0.043(3) 0.040(3) 0.025(3) 0.010(2) 0.011(2) 0.013(2) C15 0.053(3) 0.034(3) 0.029(3) 0.008(2) 0.005(2) 0.012(2) C16 0.042(3) 0.034(3) 0.032(3) 0.002(2) 0.005(2) 0.010(2) C17 0.059(4) 0.044(3) 0.031(3) 0.012(3) 0.018(3) 0.015(3) C18 0.054(3) 0.039(3) 0.036(3) 0.018(3) 0.012(3) 0.017(3) C19 0.038(3) 0.026(3) 0.023(3) 0.007(2) 0.005(2) 0.009(2) C20 0.054(3) 0.039(3) 0.029(3) 0.010(3) 0.010(2) 0.021(3) C21 0.052(3) 0.040(3) 0.048(4) 0.008(3) -0.005(3) 0.021(3) C22 0.047(3) 0.045(4) 0.060(4) 0.010(3) 0.005(3) 0.024(3) C23 0.059(4) 0.050(4) 0.040(4) 0.002(3) 0.013(3) 0.029(3) C24 0.045(3) 0.047(4) 0.035(3) -0.002(3) -0.002(2) 0.024(3) C25 0.040(3) 0.032(3) 0.023(3) 0.009(2) 0.005(2) 0.011(2) C26 0.054(3) 0.038(3) 0.038(3) 0.020(3) 0.010(3) 0.012(3) C27 0.056(4) 0.061(4) 0.053(4) 0.035(3) 0.019(3) 0.018(3) C28 0.071(4) 0.049(4) 0.057(4) 0.031(3) 0.011(3) 0.016(3) C29 0.079(5) 0.051(4) 0.061(4) 0.030(3) 0.009(3) 0.035(4) C30 0.053(3) 0.044(3) 0.048(4) 0.018(3) 0.012(3) 0.026(3) C31 0.035(3) 0.031(3) 0.029(3) 0.005(2) 0.001(2) 0.011(2) C32 0.050(3) 0.034(3) 0.030(3) 0.002(2) 0.000(2) 0.008(2) C33 0.040(3) 0.046(4) 0.039(3) 0.004(3) -0.009(2) 0.008(3) C34 0.053(4) 0.042(4) 0.059(4) 0.006(3) -0.004(3) 0.001(3) C35 0.044(3) 0.054(4) 0.052(4) 0.018(3) 0.007(3) 0.002(3) C36 0.051(3) 0.037(3) 0.037(3) 0.012(3) -0.001(3) 0.005(3) C37 0.124(8) 0.133(9) 0.106(8) 0.063(7) 0.059(6) 0.084(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 C6 2.015(5) . ? Pd1 N1 2.183(4) . ? Pd1 P1 2.2838(15) . ? Pd1 Cl1 2.3948(13) . ? Br1 C16 1.913(5) . ? Fe1 C10 2.031(5) . ? Fe1 C9 2.035(6) . ? Fe1 C4 2.053(6) . ? Fe1 C5 2.065(6) . ? Fe1 C3 2.070(7) . ? Fe1 C1 2.070(6) . ? Fe1 C2 2.071(6) . ? Fe1 C6 2.072(5) . ? Fe1 C7 2.074(5) . ? Fe1 C8 2.075(5) . ? P1 C19 1.843(5) . ? P1 C25 1.849(5) . ? P1 C31 1.858(5) . ? Cl2 C37 1.717(10) . ? Cl3 C37 1.775(10) . ? N1 C11 1.284(6) . ? N1 C13 1.422(6) . ? C1 C2 1.413(10) . ? C1 C5 1.439(9) . ? C1 H1A 0.9800 . ? C2 C3 1.419(9) . ? C2 H2A 0.9800 . ? C3 C4 1.423(9) . ? C3 H3A 0.9800 . ? C4 C5 1.436(9) . ? C4 H4A 0.9800 . ? C5 H5A 0.9800 . ? C6 C7 1.430(7) . ? C6 C10 1.461(7) . ? C7 C8 1.442(7) . ? C7 H7A 0.9800 . ? C8 C9 1.404(8) . ? C8 H8A 0.9800 . ? C9 C10 1.439(7) . ? C9 H9A 0.9800 . ? C10 C11 1.442(8) . ? C11 C12 1.505(7) . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 C18 1.402(7) . ? C13 C14 1.404(7) . ? C14 C15 1.383(7) . ? C14 H14A 0.9300 . ? C15 C16 1.388(8) . ? C15 H15A 0.9300 . ? C16 C17 1.383(8) . ? C17 C18 1.379(8) . ? C17 H17A 0.9300 . ? C18 H18A 0.9300 . ? C19 C24 1.522(7) . ? C19 C20 1.557(7) . ? C19 H19A 0.9800 . ? C20 C21 1.524(7) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 C22 1.508(8) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 C23 1.524(8) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 C24 1.542(7) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 C26 1.537(7) . ? C25 C30 1.537(7) . ? C25 H25A 0.9800 . ? C26 C27 1.522(7) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C27 C28 1.537(8) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 C29 1.513(9) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C29 C30 1.524(8) . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C31 C36 1.538(7) . ? C31 C32 1.545(7) . ? C31 H31A 0.9800 . ? C32 C33 1.519(7) . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C33 C34 1.524(8) . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C34 C35 1.512(9) . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C35 C36 1.527(7) . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C36 H36A 0.9700 . ? C36 H36C 0.9700 . ? C37 H37C 0.9700 . ? C37 H37A 0.9700 . ? 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 C6 Pd1 N1 80.49(18) . . ? C6 Pd1 P1 94.86(15) . . ? N1 Pd1 P1 171.59(12) . . ? C6 Pd1 Cl1 170.86(15) . . ? N1 Pd1 Cl1 90.78(11) . . ? P1 Pd1 Cl1 94.14(6) . . ? C10 Fe1 C9 41.4(2) . . ? C10 Fe1 C4 123.5(2) . . ? C9 Fe1 C4 161.4(3) . . ? C10 Fe1 C5 106.2(2) . . ? C9 Fe1 C5 124.5(3) . . ? C4 Fe1 C5 40.8(3) . . ? C10 Fe1 C3 160.5(2) . . ? C9 Fe1 C3 156.9(3) . . ? C4 Fe1 C3 40.4(3) . . ? C5 Fe1 C3 68.4(3) . . ? C10 Fe1 C1 121.0(3) . . ? C9 Fe1 C1 108.2(3) . . ? C4 Fe1 C1 68.1(3) . . ? C5 Fe1 C1 40.7(2) . . ? C3 Fe1 C1 67.9(3) . . ? C10 Fe1 C2 157.0(3) . . ? C9 Fe1 C2 122.4(3) . . ? C4 Fe1 C2 67.3(3) . . ? C5 Fe1 C2 67.7(3) . . ? C3 Fe1 C2 40.1(3) . . ? C1 Fe1 C2 39.9(3) . . ? C10 Fe1 C6 41.7(2) . . ? C9 Fe1 C6 69.7(2) . . ? C4 Fe1 C6 105.9(2) . . ? C5 Fe1 C6 119.7(2) . . ? C3 Fe1 C6 123.3(2) . . ? C1 Fe1 C6 156.2(3) . . ? C2 Fe1 C6 160.9(3) . . ? C10 Fe1 C7 68.6(2) . . ? C9 Fe1 C7 68.3(2) . . ? C4 Fe1 C7 120.7(2) . . ? C5 Fe1 C7 155.4(2) . . ? C3 Fe1 C7 108.1(3) . . ? C1 Fe1 C7 162.6(3) . . ? C2 Fe1 C7 126.3(3) . . ? C6 Fe1 C7 40.4(2) . . ? C10 Fe1 C8 68.3(2) . . ? C9 Fe1 C8 39.9(2) . . ? C4 Fe1 C8 156.8(3) . . ? C5 Fe1 C8 161.7(3) . . ? C3 Fe1 C8 122.5(3) . . ? C1 Fe1 C8 125.9(2) . . ? C2 Fe1 C8 110.2(2) . . ? C6 Fe1 C8 68.6(2) . . ? C7 Fe1 C8 40.7(2) . . ? C19 P1 C25 106.0(2) . . ? C19 P1 C31 108.9(2) . . ? C25 P1 C31 103.3(2) . . ? C19 P1 Pd1 114.13(16) . . ? C25 P1 Pd1 112.90(17) . . ? C31 P1 Pd1 110.91(18) . . ? C11 N1 C13 119.9(4) . . ? C11 N1 Pd1 113.2(4) . . ? C13 N1 Pd1 126.7(3) . . ? C2 C1 C5 107.7(6) . . ? C2 C1 Fe1 70.1(4) . . ? C5 C1 Fe1 69.4(3) . . ? C2 C1 H1A 126.1 . . ? C5 C1 H1A 126.1 . . ? Fe1 C1 H1A 126.1 . . ? C1 C2 C3 109.5(6) . . ? C1 C2 Fe1 70.0(4) . . ? C3 C2 Fe1 69.9(3) . . ? C1 C2 H2A 125.2 . . ? C3 C2 H2A 125.2 . . ? Fe1 C2 H2A 125.2 . . ? C2 C3 C4 107.1(6) . . ? C2 C3 Fe1 70.0(4) . . ? C4 C3 Fe1 69.2(4) . . ? C2 C3 H3A 126.5 . . ? C4 C3 H3A 126.5 . . ? Fe1 C3 H3A 126.5 . . ? C3 C4 C5 108.8(6) . . ? C3 C4 Fe1 70.4(4) . . ? C5 C4 Fe1 70.0(3) . . ? C3 C4 H4A 125.6 . . ? C5 C4 H4A 125.6 . . ? Fe1 C4 H4A 125.6 . . ? C4 C5 C1 106.9(6) . . ? C4 C5 Fe1 69.2(4) . . ? C1 C5 Fe1 69.8(3) . . ? C4 C5 H5A 126.6 . . ? C1 C5 H5A 126.6 . . ? Fe1 C5 H5A 126.6 . . ? C7 C6 C10 106.2(4) . . ? C7 C6 Pd1 143.8(4) . . ? C10 C6 Pd1 109.9(4) . . ? C7 C6 Fe1 69.9(3) . . ? C10 C6 Fe1 67.6(3) . . ? Pd1 C6 Fe1 124.0(2) . . ? C6 C7 C8 108.9(5) . . ? C6 C7 Fe1 69.8(3) . . ? C8 C7 Fe1 69.7(3) . . ? C6 C7 H7A 125.6 . . ? C8 C7 H7A 125.6 . . ? Fe1 C7 H7A 125.6 . . ? C9 C8 C7 108.4(4) . . ? C9 C8 Fe1 68.5(3) . . ? C7 C8 Fe1 69.6(3) . . ? C9 C8 H8A 125.8 . . ? C7 C8 H8A 125.8 . . ? Fe1 C8 H8A 125.8 . . ? C8 C9 C10 108.4(5) . . ? C8 C9 Fe1 71.6(3) . . ? C10 C9 Fe1 69.1(3) . . ? C8 C9 H9A 125.8 . . ? C10 C9 H9A 125.8 . . ? Fe1 C9 H9A 125.8 . . ? C9 C10 C11 131.1(5) . . ? C9 C10 C6 108.1(5) . . ? C11 C10 C6 118.9(4) . . ? C9 C10 Fe1 69.4(3) . . ? C11 C10 Fe1 113.4(4) . . ? C6 C10 Fe1 70.7(3) . . ? N1 C11 C10 115.9(5) . . ? N1 C11 C12 126.5(5) . . ? C10 C11 C12 117.5(5) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C18 C13 C14 118.7(5) . . ? C18 C13 N1 122.1(5) . . ? C14 C13 N1 119.2(5) . . ? C15 C14 C13 119.8(5) . . ? C15 C14 H14A 120.1 . . ? C13 C14 H14A 120.1 . . ? C14 C15 C16 119.8(5) . . ? C14 C15 H15A 120.1 . . ? C16 C15 H15A 120.1 . . ? C17 C16 C15 121.5(5) . . ? C17 C16 Br1 119.0(4) . . ? C15 C16 Br1 119.4(4) . . ? C18 C17 C16 118.4(5) . . ? C18 C17 H17A 120.8 . . ? C16 C17 H17A 120.8 . . ? C17 C18 C13 121.5(5) . . ? C17 C18 H18A 119.3 . . ? C13 C18 H18A 119.3 . . ? C24 C19 C20 110.4(4) . . ? C24 C19 P1 116.9(3) . . ? C20 C19 P1 113.3(3) . . ? C24 C19 H19A 105.0 . . ? C20 C19 H19A 105.0 . . ? P1 C19 H19A 105.0 . . ? C21 C20 C19 110.3(5) . . ? C21 C20 H20A 109.6 . . ? C19 C20 H20A 109.6 . . ? C21 C20 H20B 109.6 . . ? C19 C20 H20B 109.6 . . ? H20A C20 H20B 108.1 . . ? C22 C21 C20 111.8(4) . . ? C22 C21 H21A 109.3 . . ? C20 C21 H21A 109.3 . . ? C22 C21 H21B 109.3 . . ? C20 C21 H21B 109.3 . . ? H21A C21 H21B 107.9 . . ? C21 C22 C23 111.0(5) . . ? C21 C22 H22A 109.4 . . ? C23 C22 H22A 109.4 . . ? C21 C22 H22B 109.4 . . ? C23 C22 H22B 109.4 . . ? H22A C22 H22B 108.0 . . ? C22 C23 C24 110.9(5) . . ? C22 C23 H23A 109.5 . . ? C24 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? C24 C23 H23B 109.5 . . ? H23A C23 H23B 108.0 . . ? C19 C24 C23 110.7(4) . . ? C19 C24 H24A 109.5 . . ? C23 C24 H24A 109.5 . . ? C19 C24 H24B 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 108.1 . . ? C26 C25 C30 110.6(4) . . ? C26 C25 P1 113.5(3) . . ? C30 C25 P1 109.4(4) . . ? C26 C25 H25A 107.7 . . ? C30 C25 H25A 107.7 . . ? P1 C25 H25A 107.7 . . ? C27 C26 C25 112.1(4) . . ? C27 C26 H26A 109.2 . . ? C25 C26 H26A 109.2 . . ? C27 C26 H26B 109.2 . . ? C25 C26 H26B 109.2 . . ? H26A C26 H26B 107.9 . . ? C26 C27 C28 111.4(5) . . ? C26 C27 H27A 109.4 . . ? C28 C27 H27A 109.4 . . ? C26 C27 H27B 109.4 . . ? C28 C27 H27B 109.4 . . ? H27A C27 H27B 108.0 . . ? C29 C28 C27 111.1(5) . . ? C29 C28 H28A 109.4 . . ? C27 C28 H28A 109.4 . . ? C29 C28 H28B 109.4 . . ? C27 C28 H28B 109.4 . . ? H28A C28 H28B 108.0 . . ? C28 C29 C30 110.6(5) . . ? C28 C29 H29A 109.5 . . ? C30 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? C30 C29 H29B 109.5 . . ? H29A C29 H29B 108.1 . . ? C29 C30 C25 112.5(5) . . ? C29 C30 H30A 109.1 . . ? C25 C30 H30A 109.1 . . ? C29 C30 H30B 109.1 . . ? C25 C30 H30B 109.1 . . ? H30A C30 H30B 107.8 . . ? C36 C31 C32 110.0(4) . . ? C36 C31 P1 112.3(3) . . ? C32 C31 P1 117.9(4) . . ? C36 C31 H31A 105.2 . . ? C32 C31 H31A 105.2 . . ? P1 C31 H31A 105.2 . . ? C33 C32 C31 109.9(5) . . ? C33 C32 H32A 109.7 . . ? C31 C32 H32A 109.7 . . ? C33 C32 H32B 109.7 . . ? C31 C32 H32B 109.7 . . ? H32A C32 H32B 108.2 . . ? C32 C33 C34 111.7(5) . . ? C32 C33 H33A 109.3 . . ? C34 C33 H33A 109.3 . . ? C32 C33 H33B 109.3 . . ? C34 C33 H33B 109.3 . . ? H33A C33 H33B 107.9 . . ? C35 C34 C33 111.5(5) . . ? C35 C34 H34A 109.3 . . ? C33 C34 H34A 109.3 . . ? C35 C34 H34B 109.3 . . ? C33 C34 H34B 109.3 . . ? H34A C34 H34B 108.0 . . ? C34 C35 C36 110.8(5) . . ? C34 C35 H35A 109.5 . . ? C36 C35 H35A 109.5 . . ? C34 C35 H35B 109.5 . . ? C36 C35 H35B 109.5 . . ? H35A C35 H35B 108.1 . . ? C35 C36 C31 110.5(4) . . ? C35 C36 H36A 109.5 . . ? C31 C36 H36A 109.5 . . ? C35 C36 H36C 109.5 . . ? C31 C36 H36C 109.5 . . ? H36A C36 H36C 108.1 . . ? Cl2 C37 Cl3 111.2(5) . . ? Cl2 C37 H37C 109.4 . . ? Cl3 C37 H37C 109.4 . . ? Cl2 C37 H37A 109.4 . . ? Cl3 C37 H37A 109.4 . . ? H37C C37 H37A 108.0 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 Pd1 P1 C19 34.9(2) . . . . ? N1 Pd1 P1 C19 -21.0(8) . . . . ? Cl1 Pd1 P1 C19 -146.68(18) . . . . ? C6 Pd1 P1 C25 -86.2(2) . . . . ? N1 Pd1 P1 C25 -142.2(8) . . . . ? Cl1 Pd1 P1 C25 92.17(17) . . . . ? C6 Pd1 P1 C31 158.4(2) . . . . ? N1 Pd1 P1 C31 102.4(8) . . . . ? Cl1 Pd1 P1 C31 -23.21(18) . . . . ? C6 Pd1 N1 C11 -8.6(4) . . . . ? P1 Pd1 N1 C11 48.2(10) . . . . ? Cl1 Pd1 N1 C11 174.1(4) . . . . ? C6 Pd1 N1 C13 166.7(4) . . . . ? P1 Pd1 N1 C13 -136.4(7) . . . . ? Cl1 Pd1 N1 C13 -10.6(4) . . . . ? C10 Fe1 C1 C2 162.8(4) . . . . ? C9 Fe1 C1 C2 119.1(4) . . . . ? C4 Fe1 C1 C2 -80.3(4) . . . . ? C5 Fe1 C1 C2 -118.8(6) . . . . ? C3 Fe1 C1 C2 -36.6(4) . . . . ? C6 Fe1 C1 C2 -160.0(5) . . . . ? C7 Fe1 C1 C2 43.5(10) . . . . ? C8 Fe1 C1 C2 78.4(5) . . . . ? C10 Fe1 C1 C5 -78.4(5) . . . . ? C9 Fe1 C1 C5 -122.2(4) . . . . ? C4 Fe1 C1 C5 38.4(4) . . . . ? C3 Fe1 C1 C5 82.1(4) . . . . ? C2 Fe1 C1 C5 118.8(6) . . . . ? C6 Fe1 C1 C5 -41.2(8) . . . . ? C7 Fe1 C1 C5 162.2(8) . . . . ? C8 Fe1 C1 C5 -162.9(4) . . . . ? C5 C1 C2 C3 -0.6(7) . . . . ? Fe1 C1 C2 C3 58.9(4) . . . . ? C5 C1 C2 Fe1 -59.5(4) . . . . ? C10 Fe1 C2 C1 -40.4(8) . . . . ? C9 Fe1 C2 C1 -79.5(5) . . . . ? C4 Fe1 C2 C1 82.5(4) . . . . ? C5 Fe1 C2 C1 38.2(4) . . . . ? C3 Fe1 C2 C1 120.8(6) . . . . ? C6 Fe1 C2 C1 155.1(6) . . . . ? C7 Fe1 C2 C1 -165.2(4) . . . . ? C8 Fe1 C2 C1 -122.3(4) . . . . ? C10 Fe1 C2 C3 -161.2(5) . . . . ? C9 Fe1 C2 C3 159.7(4) . . . . ? C4 Fe1 C2 C3 -38.2(4) . . . . ? C5 Fe1 C2 C3 -82.6(4) . . . . ? C1 Fe1 C2 C3 -120.8(6) . . . . ? C6 Fe1 C2 C3 34.3(9) . . . . ? C7 Fe1 C2 C3 74.0(5) . . . . ? C8 Fe1 C2 C3 117.0(4) . . . . ? C1 C2 C3 C4 0.6(7) . . . . ? Fe1 C2 C3 C4 59.5(4) . . . . ? C1 C2 C3 Fe1 -58.9(5) . . . . ? C10 Fe1 C3 C2 157.8(7) . . . . ? C9 Fe1 C3 C2 -48.3(8) . . . . ? C4 Fe1 C3 C2 118.2(6) . . . . ? C5 Fe1 C3 C2 80.5(4) . . . . ? C1 Fe1 C3 C2 36.5(4) . . . . ? C6 Fe1 C3 C2 -167.3(4) . . . . ? C7 Fe1 C3 C2 -125.4(4) . . . . ? C8 Fe1 C3 C2 -82.9(5) . . . . ? C10 Fe1 C3 C4 39.6(9) . . . . ? C9 Fe1 C3 C4 -166.5(6) . . . . ? C5 Fe1 C3 C4 -37.7(4) . . . . ? C1 Fe1 C3 C4 -81.7(4) . . . . ? C2 Fe1 C3 C4 -118.2(6) . . . . ? C6 Fe1 C3 C4 74.5(4) . . . . ? C7 Fe1 C3 C4 116.4(4) . . . . ? C8 Fe1 C3 C4 158.9(4) . . . . ? C2 C3 C4 C5 -0.3(7) . . . . ? Fe1 C3 C4 C5 59.7(4) . . . . ? C2 C3 C4 Fe1 -60.0(4) . . . . ? C10 Fe1 C4 C3 -165.2(4) . . . . ? C9 Fe1 C4 C3 163.3(7) . . . . ? C5 Fe1 C4 C3 119.6(5) . . . . ? C1 Fe1 C4 C3 81.2(4) . . . . ? C2 Fe1 C4 C3 37.9(4) . . . . ? C6 Fe1 C4 C3 -123.1(4) . . . . ? C7 Fe1 C4 C3 -81.9(4) . . . . ? C8 Fe1 C4 C3 -50.5(7) . . . . ? C10 Fe1 C4 C5 75.2(4) . . . . ? C9 Fe1 C4 C5 43.8(9) . . . . ? C3 Fe1 C4 C5 -119.6(5) . . . . ? C1 Fe1 C4 C5 -38.4(4) . . . . ? C2 Fe1 C4 C5 -81.6(4) . . . . ? C6 Fe1 C4 C5 117.3(4) . . . . ? C7 Fe1 C4 C5 158.5(3) . . . . ? C8 Fe1 C4 C5 -170.1(5) . . . . ? C3 C4 C5 C1 0.0(7) . . . . ? Fe1 C4 C5 C1 59.9(4) . . . . ? C3 C4 C5 Fe1 -60.0(4) . . . . ? C2 C1 C5 C4 0.4(7) . . . . ? Fe1 C1 C5 C4 -59.5(4) . . . . ? C2 C1 C5 Fe1 59.9(4) . . . . ? C10 Fe1 C5 C4 -122.9(4) . . . . ? C9 Fe1 C5 C4 -164.5(4) . . . . ? C3 Fe1 C5 C4 37.3(4) . . . . ? C1 Fe1 C5 C4 118.1(6) . . . . ? C2 Fe1 C5 C4 80.6(4) . . . . ? C6 Fe1 C5 C4 -79.8(4) . . . . ? C7 Fe1 C5 C4 -49.2(8) . . . . ? C8 Fe1 C5 C4 167.5(7) . . . . ? C10 Fe1 C5 C1 119.0(4) . . . . ? C9 Fe1 C5 C1 77.5(5) . . . . ? C4 Fe1 C5 C1 -118.1(6) . . . . ? C3 Fe1 C5 C1 -80.8(4) . . . . ? C2 Fe1 C5 C1 -37.4(4) . . . . ? C6 Fe1 C5 C1 162.2(4) . . . . ? C7 Fe1 C5 C1 -167.3(6) . . . . ? C8 Fe1 C5 C1 49.5(9) . . . . ? N1 Pd1 C6 C7 -167.9(7) . . . . ? P1 Pd1 C6 C7 19.2(7) . . . . ? Cl1 Pd1 C6 C7 -150.7(7) . . . . ? N1 Pd1 C6 C10 10.7(3) . . . . ? P1 Pd1 C6 C10 -162.3(3) . . . . ? Cl1 Pd1 C6 C10 27.9(12) . . . . ? N1 Pd1 C6 Fe1 -65.2(3) . . . . ? P1 Pd1 C6 Fe1 121.8(3) . . . . ? Cl1 Pd1 C6 Fe1 -48.0(11) . . . . ? C10 Fe1 C6 C7 -118.2(4) . . . . ? C9 Fe1 C6 C7 -80.1(3) . . . . ? C4 Fe1 C6 C7 119.0(4) . . . . ? C5 Fe1 C6 C7 160.9(3) . . . . ? C3 Fe1 C6 C7 78.5(4) . . . . ? C1 Fe1 C6 C7 -169.4(6) . . . . ? C2 Fe1 C6 C7 52.8(8) . . . . ? C8 Fe1 C6 C7 -37.2(3) . . . . ? C9 Fe1 C6 C10 38.1(3) . . . . ? C4 Fe1 C6 C10 -122.8(3) . . . . ? C5 Fe1 C6 C10 -80.9(4) . . . . ? C3 Fe1 C6 C10 -163.3(3) . . . . ? C1 Fe1 C6 C10 -51.2(7) . . . . ? C2 Fe1 C6 C10 171.0(7) . . . . ? C7 Fe1 C6 C10 118.2(4) . . . . ? C8 Fe1 C6 C10 81.0(3) . . . . ? C10 Fe1 C6 Pd1 99.6(4) . . . . ? C9 Fe1 C6 Pd1 137.8(4) . . . . ? C4 Fe1 C6 Pd1 -23.2(4) . . . . ? C5 Fe1 C6 Pd1 18.8(4) . . . . ? C3 Fe1 C6 Pd1 -63.7(4) . . . . ? C1 Fe1 C6 Pd1 48.5(7) . . . . ? C2 Fe1 C6 Pd1 -89.4(8) . . . . ? C7 Fe1 C6 Pd1 -142.1(5) . . . . ? C8 Fe1 C6 Pd1 -179.4(4) . . . . ? C10 C6 C7 C8 0.8(6) . . . . ? Pd1 C6 C7 C8 179.4(5) . . . . ? Fe1 C6 C7 C8 58.9(4) . . . . ? C10 C6 C7 Fe1 -58.1(3) . . . . ? Pd1 C6 C7 Fe1 120.5(6) . . . . ? C10 Fe1 C7 C6 39.0(3) . . . . ? C9 Fe1 C7 C6 83.7(3) . . . . ? C4 Fe1 C7 C6 -78.1(4) . . . . ? C5 Fe1 C7 C6 -43.0(7) . . . . ? C3 Fe1 C7 C6 -120.5(3) . . . . ? C1 Fe1 C7 C6 165.6(8) . . . . ? C2 Fe1 C7 C6 -161.2(3) . . . . ? C8 Fe1 C7 C6 120.3(5) . . . . ? C10 Fe1 C7 C8 -81.2(3) . . . . ? C9 Fe1 C7 C8 -36.5(3) . . . . ? C4 Fe1 C7 C8 161.6(3) . . . . ? C5 Fe1 C7 C8 -163.2(6) . . . . ? C3 Fe1 C7 C8 119.2(3) . . . . ? C1 Fe1 C7 C8 45.4(10) . . . . ? C2 Fe1 C7 C8 78.6(4) . . . . ? C6 Fe1 C7 C8 -120.3(5) . . . . ? C6 C7 C8 C9 -1.2(6) . . . . ? Fe1 C7 C8 C9 57.7(4) . . . . ? C6 C7 C8 Fe1 -58.9(4) . . . . ? C10 Fe1 C8 C9 -38.6(3) . . . . ? C4 Fe1 C8 C9 -164.0(6) . . . . ? C5 Fe1 C8 C9 37.0(9) . . . . ? C3 Fe1 C8 C9 159.7(3) . . . . ? C1 Fe1 C8 C9 74.8(4) . . . . ? C2 Fe1 C8 C9 116.8(4) . . . . ? C6 Fe1 C8 C9 -83.6(3) . . . . ? C7 Fe1 C8 C9 -120.5(4) . . . . ? C10 Fe1 C8 C7 81.9(3) . . . . ? C9 Fe1 C8 C7 120.5(4) . . . . ? C4 Fe1 C8 C7 -43.5(7) . . . . ? C5 Fe1 C8 C7 157.5(7) . . . . ? C3 Fe1 C8 C7 -79.8(4) . . . . ? C1 Fe1 C8 C7 -164.7(4) . . . . ? C2 Fe1 C8 C7 -122.7(4) . . . . ? C6 Fe1 C8 C7 36.9(3) . . . . ? C7 C8 C9 C10 1.2(6) . . . . ? Fe1 C8 C9 C10 59.5(4) . . . . ? C7 C8 C9 Fe1 -58.3(4) . . . . ? C10 Fe1 C9 C8 118.9(4) . . . . ? C4 Fe1 C9 C8 160.0(7) . . . . ? C5 Fe1 C9 C8 -166.7(3) . . . . ? C3 Fe1 C9 C8 -48.2(8) . . . . ? C1 Fe1 C9 C8 -124.6(4) . . . . ? C2 Fe1 C9 C8 -83.0(4) . . . . ? C6 Fe1 C9 C8 80.5(3) . . . . ? C7 Fe1 C9 C8 37.2(3) . . . . ? C4 Fe1 C9 C10 41.1(9) . . . . ? C5 Fe1 C9 C10 74.4(4) . . . . ? C3 Fe1 C9 C10 -167.1(6) . . . . ? C1 Fe1 C9 C10 116.5(4) . . . . ? C2 Fe1 C9 C10 158.1(3) . . . . ? C6 Fe1 C9 C10 -38.4(3) . . . . ? C7 Fe1 C9 C10 -81.7(3) . . . . ? C8 Fe1 C9 C10 -118.9(4) . . . . ? C8 C9 C10 C11 -164.7(6) . . . . ? Fe1 C9 C10 C11 -103.6(6) . . . . ? C8 C9 C10 C6 -0.7(6) . . . . ? Fe1 C9 C10 C6 60.3(4) . . . . ? C8 C9 C10 Fe1 -61.1(4) . . . . ? C7 C6 C10 C9 0.0(6) . . . . ? Pd1 C6 C10 C9 -179.1(3) . . . . ? Fe1 C6 C10 C9 -59.6(4) . . . . ? C7 C6 C10 C11 166.2(5) . . . . ? Pd1 C6 C10 C11 -12.9(6) . . . . ? Fe1 C6 C10 C11 106.7(5) . . . . ? C7 C6 C10 Fe1 59.5(4) . . . . ? Pd1 C6 C10 Fe1 -119.6(3) . . . . ? C4 Fe1 C10 C9 -165.5(3) . . . . ? C5 Fe1 C10 C9 -124.3(3) . . . . ? C3 Fe1 C10 C9 164.9(7) . . . . ? C1 Fe1 C10 C9 -82.6(4) . . . . ? C2 Fe1 C10 C9 -53.5(7) . . . . ? C6 Fe1 C10 C9 118.9(4) . . . . ? C7 Fe1 C10 C9 81.1(3) . . . . ? C8 Fe1 C10 C9 37.2(3) . . . . ? C9 Fe1 C10 C11 127.1(5) . . . . ? C4 Fe1 C10 C11 -38.4(5) . . . . ? C5 Fe1 C10 C11 2.8(4) . . . . ? C3 Fe1 C10 C11 -68.1(9) . . . . ? C1 Fe1 C10 C11 44.5(5) . . . . ? C2 Fe1 C10 C11 73.5(7) . . . . ? C6 Fe1 C10 C11 -114.0(5) . . . . ? C7 Fe1 C10 C11 -151.8(4) . . . . ? C8 Fe1 C10 C11 164.3(4) . . . . ? C9 Fe1 C10 C6 -118.9(4) . . . . ? C4 Fe1 C10 C6 75.6(4) . . . . ? C5 Fe1 C10 C6 116.8(3) . . . . ? C3 Fe1 C10 C6 45.9(8) . . . . ? C1 Fe1 C10 C6 158.5(3) . . . . ? C2 Fe1 C10 C6 -172.5(6) . . . . ? C7 Fe1 C10 C6 -37.8(3) . . . . ? C8 Fe1 C10 C6 -81.7(3) . . . . ? C13 N1 C11 C10 -171.9(5) . . . . ? Pd1 N1 C11 C10 3.8(6) . . . . ? C13 N1 C11 C12 3.1(8) . . . . ? Pd1 N1 C11 C12 178.8(5) . . . . ? C9 C10 C11 N1 168.5(5) . . . . ? C6 C10 C11 N1 5.9(7) . . . . ? Fe1 C10 C11 N1 86.0(5) . . . . ? C9 C10 C11 C12 -7.0(9) . . . . ? C6 C10 C11 C12 -169.5(5) . . . . ? Fe1 C10 C11 C12 -89.5(5) . . . . ? C11 N1 C13 C18 -62.6(7) . . . . ? Pd1 N1 C13 C18 122.3(5) . . . . ? C11 N1 C13 C14 116.0(6) . . . . ? Pd1 N1 C13 C14 -59.1(6) . . . . ? C18 C13 C14 C15 4.0(8) . . . . ? N1 C13 C14 C15 -174.6(4) . . . . ? C13 C14 C15 C16 -0.9(8) . . . . ? C14 C15 C16 C17 -1.1(8) . . . . ? C14 C15 C16 Br1 175.8(4) . . . . ? C15 C16 C17 C18 -0.2(9) . . . . ? Br1 C16 C17 C18 -177.1(4) . . . . ? C16 C17 C18 C13 3.5(9) . . . . ? C14 C13 C18 C17 -5.4(8) . . . . ? N1 C13 C18 C17 173.2(5) . . . . ? C25 P1 C19 C24 -61.8(4) . . . . ? C31 P1 C19 C24 48.8(5) . . . . ? Pd1 P1 C19 C24 173.3(3) . . . . ? C25 P1 C19 C20 168.3(4) . . . . ? C31 P1 C19 C20 -81.2(4) . . . . ? Pd1 P1 C19 C20 43.4(4) . . . . ? C24 C19 C20 C21 56.1(6) . . . . ? P1 C19 C20 C21 -170.7(4) . . . . ? C19 C20 C21 C22 -56.4(6) . . . . ? C20 C21 C22 C23 56.8(7) . . . . ? C21 C22 C23 C24 -56.4(7) . . . . ? C20 C19 C24 C23 -56.3(6) . . . . ? P1 C19 C24 C23 172.3(4) . . . . ? C22 C23 C24 C19 56.7(7) . . . . ? C19 P1 C25 C26 -57.8(4) . . . . ? C31 P1 C25 C26 -172.3(4) . . . . ? Pd1 P1 C25 C26 67.9(4) . . . . ? C19 P1 C25 C30 178.2(4) . . . . ? C31 P1 C25 C30 63.7(4) . . . . ? Pd1 P1 C25 C30 -56.1(4) . . . . ? C30 C25 C26 C27 -52.7(6) . . . . ? P1 C25 C26 C27 -176.0(4) . . . . ? C25 C26 C27 C28 54.4(7) . . . . ? C26 C27 C28 C29 -56.4(7) . . . . ? C27 C28 C29 C30 56.7(7) . . . . ? C28 C29 C30 C25 -56.1(7) . . . . ? C26 C25 C30 C29 53.7(7) . . . . ? P1 C25 C30 C29 179.4(4) . . . . ? C19 P1 C31 C36 58.9(4) . . . . ? C25 P1 C31 C36 171.3(4) . . . . ? Pd1 P1 C31 C36 -67.5(4) . . . . ? C19 P1 C31 C32 -70.6(4) . . . . ? C25 P1 C31 C32 41.8(5) . . . . ? Pd1 P1 C31 C32 163.0(3) . . . . ? C36 C31 C32 C33 57.2(6) . . . . ? P1 C31 C32 C33 -172.3(4) . . . . ? C31 C32 C33 C34 -56.3(7) . . . . ? C32 C33 C34 C35 56.0(7) . . . . ? C33 C34 C35 C36 -55.8(7) . . . . ? C34 C35 C36 C31 57.2(7) . . . . ? C32 C31 C36 C35 -57.9(6) . . . . ? P1 C31 C36 C35 168.7(4) . . . . ? _diffrn_measured_fraction_theta_max 0.879 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.879 _refine_diff_density_max 0.538 _refine_diff_density_min -0.711 _refine_diff_density_rms 0.126 # Attachment 'Complex 2d .cif' data_p-1_2d _database_code_depnum_ccdc_archive 'CCDC 600775' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C39 H55 Cl3 Fe N O P Pd' _chemical_formula_weight 853.41 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.927(2) _cell_length_b 12.477(3) _cell_length_c 16.594(3) _cell_angle_alpha 103.00(3) _cell_angle_beta 90.52(3) _cell_angle_gamma 94.15(3) _cell_volume 1996.7(7) _cell_formula_units_Z 2 _cell_measurement_temperature 291(2) _cell_measurement_reflns_used 356 _cell_measurement_theta_min 2 _cell_measurement_theta_max 25.1 _exptl_crystal_description PRISMATIC _exptl_crystal_colour Red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.419 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 884 _exptl_absorpt_coefficient_mu 1.085 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8123 _exptl_absorpt_correction_T_max 0.8287 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 291(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type R-AXIS-IV _diffrn_measurement_method 'Oscillation frames' _diffrn_detector_area_resol_mean 0 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% ? _diffrn_reflns_number 6145 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0440 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.26 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6145 _reflns_number_gt 4786 _reflns_threshold_expression >2sigma(I) _computing_data_collection raxis _computing_cell_refinement raxis _computing_data_reduction raxis _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics texsan _computing_publication_material texsan _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0780P)^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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0022(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 6145 _refine_ls_number_parameters 425 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0614 _refine_ls_R_factor_gt 0.0447 _refine_ls_wR_factor_ref 0.1241 _refine_ls_wR_factor_gt 0.1181 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.037 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.40645(6) 0.48179(5) 0.71087(4) 0.0462(2) Uani 1 1 d . . . Pd1 Pd 0.74328(3) 0.59300(3) 0.71427(2) 0.04422(15) Uani 1 1 d . . . P1 P 0.75448(12) 0.76799(9) 0.79242(7) 0.0416(3) Uani 1 1 d . . . Cl1 Cl 0.95741(15) 0.55373(12) 0.76241(13) 0.1017(7) Uani 1 1 d . . . Cl2 Cl 0.9472(4) 1.2232(2) 0.87538(19) 0.1964(16) Uani 1 1 d . . . Cl3 Cl 0.8172(5) 1.4054(4) 0.9658(4) 0.277(3) Uani 1 1 d . . . N1 N 0.7311(4) 0.4393(3) 0.6234(2) 0.0478(9) Uani 1 1 d . . . O1 O 1.1308(4) 0.1382(3) 0.5546(2) 0.0672(10) Uani 1 1 d . . . C1 C 0.4696(8) 0.4436(6) 0.8169(4) 0.094(3) Uani 1 1 d . . . H1A H 0.5504 0.4763 0.8503 0.113 Uiso 1 1 calc R . . C2 C 0.3387(13) 0.4830(6) 0.8255(5) 0.120(3) Uani 1 1 d . . . H2A H 0.3115 0.5470 0.8663 0.144 Uiso 1 1 calc R . . C3 C 0.2556(7) 0.4092(7) 0.7682(6) 0.100(3) Uani 1 1 d . . . H3A H 0.1585 0.4139 0.7598 0.120 Uiso 1 1 calc R . . C4 C 0.3309(8) 0.3304(6) 0.7245(5) 0.0853(19) Uani 1 1 d . . . H4A H 0.2969 0.2689 0.6795 0.102 Uiso 1 1 calc R . . C5 C 0.4622(6) 0.3506(5) 0.7540(4) 0.0788(18) Uani 1 1 d . . . H5A H 0.5373 0.3057 0.7341 0.095 Uiso 1 1 calc R . . C6 C 0.5514(4) 0.5901(3) 0.6756(3) 0.0404(10) Uani 1 1 d . . . C7 C 0.4278(4) 0.6405(4) 0.6946(3) 0.0430(10) Uani 1 1 d . . . H7A H 0.4177 0.7068 0.7382 0.052 Uiso 1 1 calc R . . C8 C 0.3202(5) 0.5788(4) 0.6437(3) 0.0514(12) Uani 1 1 d . . . H8A H 0.2255 0.5964 0.6453 0.062 Uiso 1 1 calc R . . C9 C 0.3734(5) 0.4855(4) 0.5910(3) 0.0535(13) Uani 1 1 d . . . H9A H 0.3232 0.4287 0.5489 0.064 Uiso 1 1 calc R . . C10 C 0.5152(5) 0.4925(4) 0.6105(3) 0.0456(11) Uani 1 1 d . . . C11 C 0.6143(5) 0.4128(4) 0.5871(3) 0.0459(11) Uani 1 1 d . . . C12 C 0.5763(6) 0.3063(4) 0.5263(3) 0.0608(14) Uani 1 1 d . . . H12A H 0.6531 0.2629 0.5173 0.091 Uiso 1 1 calc R . . H12B H 0.5473 0.3212 0.4748 0.091 Uiso 1 1 calc R . . H12C H 0.5041 0.2663 0.5478 0.091 Uiso 1 1 calc R . . C13 C 0.8359(5) 0.3643(4) 0.6071(3) 0.0487(12) Uani 1 1 d . . . C14 C 0.8541(5) 0.2927(4) 0.6585(3) 0.0562(13) Uani 1 1 d . . . H14A H 0.7993 0.2951 0.7039 0.067 Uiso 1 1 calc R . . C15 C 0.9516(5) 0.2180(4) 0.6436(3) 0.0573(13) Uani 1 1 d . . . H15A H 0.9624 0.1707 0.6789 0.069 Uiso 1 1 calc R . . C16 C 1.0336(5) 0.2135(4) 0.5757(3) 0.0550(13) Uani 1 1 d . . . C17 C 1.0187(5) 0.2873(4) 0.5261(3) 0.0598(13) Uani 1 1 d . . . H17A H 1.0758 0.2869 0.4819 0.072 Uiso 1 1 calc R . . C18 C 0.9206(5) 0.3615(4) 0.5408(3) 0.0581(13) Uani 1 1 d . . . H18A H 0.9111 0.4099 0.5063 0.070 Uiso 1 1 calc R . . C19 C 1.1305(6) 0.0500(5) 0.5956(4) 0.0712(16) Uani 1 1 d . . . H19A H 1.0414 0.0115 0.5908 0.085 Uiso 1 1 calc R . . H19B H 1.1527 0.0787 0.6539 0.085 Uiso 1 1 calc R . . C20 C 1.2303(7) -0.0267(5) 0.5583(4) 0.090(2) Uani 1 1 d . . . H20A H 1.2305 -0.0862 0.5862 0.134 Uiso 1 1 calc R . . H20B H 1.3184 0.0117 0.5634 0.134 Uiso 1 1 calc R . . H20C H 1.2072 -0.0556 0.5008 0.134 Uiso 1 1 calc R . . C21 C 0.6807(6) 0.7837(5) 0.8962(3) 0.0682(15) Uani 1 1 d . . . H21A H 0.7189 0.8567 0.9257 0.082 Uiso 1 1 calc R . . C22 C 0.5390(8) 0.7916(8) 0.9054(4) 0.121(3) Uani 1 1 d . . . H22A H 0.4924 0.7231 0.8752 0.145 Uiso 1 1 calc R . . H22B H 0.5121 0.8501 0.8803 0.145 Uiso 1 1 calc R . . C23 C 0.4926(8) 0.8144(6) 0.9951(4) 0.099(2) Uani 1 1 d . . . H23A H 0.5232 0.8893 1.0229 0.119 Uiso 1 1 calc R . . H23B H 0.3947 0.8078 0.9956 0.119 Uiso 1 1 calc R . . C24 C 0.5473(9) 0.7352(8) 1.0411(5) 0.120(3) Uani 1 1 d . . . H24A H 0.5305 0.7609 1.0995 0.144 Uiso 1 1 calc R . . H24B H 0.4978 0.6638 1.0223 0.144 Uiso 1 1 calc R . . C25 C 0.6858(9) 0.7215(9) 1.0317(5) 0.130(3) Uani 1 1 d . . . H25A H 0.7060 0.6578 1.0528 0.157 Uiso 1 1 calc R . . H25B H 0.7353 0.7853 1.0665 0.157 Uiso 1 1 calc R . . C26 C 0.7403(6) 0.7064(5) 0.9444(3) 0.0710(16) Uani 1 1 d . . . H26A H 0.7192 0.6306 0.9146 0.085 Uiso 1 1 calc R . . H26B H 0.8378 0.7202 0.9478 0.085 Uiso 1 1 calc R . . C27 C 0.9334(5) 0.8205(4) 0.8138(3) 0.0512(12) Uani 1 1 d . . . H27A H 0.9722 0.7612 0.8341 0.061 Uiso 1 1 calc R . . C28 C 1.0123(5) 0.8235(5) 0.7374(3) 0.0625(14) Uani 1 1 d . . . H28A H 0.9866 0.8846 0.7148 0.075 Uiso 1 1 calc R . . H28B H 0.9903 0.7558 0.6961 0.075 Uiso 1 1 calc R . . C29 C 1.1648(6) 0.8366(6) 0.7563(4) 0.090(2) Uani 1 1 d . . . H29A H 1.1920 0.7703 0.7712 0.107 Uiso 1 1 calc R . . H29B H 1.2119 0.8442 0.7067 0.107 Uiso 1 1 calc R . . C30 C 1.2052(7) 0.9308(7) 0.8225(5) 0.112(3) Uani 1 1 d . . . H30A H 1.1915 0.9979 0.8043 0.134 Uiso 1 1 calc R . . H30B H 1.3007 0.9305 0.8351 0.134 Uiso 1 1 calc R . . C31 C 1.1262(7) 0.9306(6) 0.9003(4) 0.106(3) Uani 1 1 d . . . H31A H 1.1503 0.9984 0.9411 0.128 Uiso 1 1 calc R . . H31B H 1.1500 0.8694 0.9233 0.128 Uiso 1 1 calc R . . C32 C 0.9713(6) 0.9203(5) 0.8816(4) 0.094(2) Uani 1 1 d . . . H32A H 0.9232 0.9142 0.9312 0.113 Uiso 1 1 calc R . . H32B H 0.9455 0.9859 0.8651 0.113 Uiso 1 1 calc R . . C33 C 0.6668(5) 0.8658(3) 0.7451(3) 0.0445(11) Uani 1 1 d . . . H33A H 0.5702 0.8477 0.7509 0.053 Uiso 1 1 calc R . . C34 C 0.6869(5) 0.8500(4) 0.6515(3) 0.0551(12) Uani 1 1 d . . . H34A H 0.7793 0.8738 0.6415 0.066 Uiso 1 1 calc R . . H34B H 0.6710 0.7725 0.6248 0.066 Uiso 1 1 calc R . . C35 C 0.5900(6) 0.9167(4) 0.6151(3) 0.0666(15) Uani 1 1 d . . . H35A H 0.4978 0.8888 0.6214 0.080 Uiso 1 1 calc R . . H35B H 0.6057 0.9078 0.5565 0.080 Uiso 1 1 calc R . . C36 C 0.6079(7) 1.0396(4) 0.6577(4) 0.0760(17) Uani 1 1 d . . . H36A H 0.5403 1.0788 0.6360 0.091 Uiso 1 1 calc R . . H36B H 0.6963 1.0699 0.6457 0.091 Uiso 1 1 calc R . . C37 C 0.5938(7) 1.0568(4) 0.7523(4) 0.0764(17) Uani 1 1 d . . . H37A H 0.6131 1.1343 0.7784 0.092 Uiso 1 1 calc R . . H37B H 0.5019 1.0353 0.7647 0.092 Uiso 1 1 calc R . . C38 C 0.6915(6) 0.9880(4) 0.7869(3) 0.0636(14) Uani 1 1 d . . . H38A H 0.7837 1.0133 0.7781 0.076 Uiso 1 1 calc R . . H38B H 0.6798 0.9979 0.8460 0.076 Uiso 1 1 calc R . . C39 C 0.9415(10) 1.3624(7) 0.9037(6) 0.138(3) Uani 1 1 d . . . H39A H 1.0267 1.3940 0.9311 0.166 Uiso 1 1 calc R . . H39B H 0.9330 1.3905 0.8541 0.166 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0382(4) 0.0436(4) 0.0610(4) 0.0214(3) -0.0002(3) 0.0015(3) Pd1 0.0367(2) 0.0305(2) 0.0645(3) 0.00783(16) -0.00105(16) 0.00536(13) P1 0.0433(7) 0.0338(6) 0.0482(7) 0.0098(5) 0.0069(5) 0.0043(5) Cl1 0.0608(9) 0.0505(8) 0.1791(18) -0.0073(10) -0.0478(11) 0.0179(7) Cl2 0.323(5) 0.0883(17) 0.164(2) 0.0092(16) -0.044(3) -0.010(2) Cl3 0.240(5) 0.202(4) 0.404(6) 0.092(4) 0.168(5) 0.025(3) N1 0.044(2) 0.037(2) 0.061(2) 0.0082(18) 0.0087(19) 0.0079(17) O1 0.062(2) 0.062(2) 0.082(2) 0.0177(19) 0.0164(19) 0.0289(18) C1 0.127(7) 0.088(5) 0.074(4) 0.052(4) -0.041(4) -0.046(5) C2 0.218(11) 0.065(5) 0.092(5) 0.039(4) 0.077(7) 0.030(6) C3 0.056(4) 0.116(7) 0.158(7) 0.088(6) 0.027(5) 0.008(4) C4 0.089(5) 0.069(4) 0.107(5) 0.046(4) -0.001(4) -0.015(4) C5 0.063(4) 0.079(4) 0.114(5) 0.061(4) 0.013(4) 0.017(3) C6 0.042(2) 0.034(2) 0.046(2) 0.0120(19) 0.002(2) 0.0038(19) C7 0.039(2) 0.039(2) 0.053(3) 0.013(2) 0.000(2) 0.0079(19) C8 0.043(3) 0.055(3) 0.063(3) 0.025(2) -0.003(2) 0.010(2) C9 0.050(3) 0.047(3) 0.062(3) 0.012(2) -0.018(2) -0.001(2) C10 0.051(3) 0.039(2) 0.048(3) 0.013(2) 0.000(2) 0.008(2) C11 0.052(3) 0.038(2) 0.049(3) 0.014(2) 0.004(2) 0.005(2) C12 0.073(4) 0.047(3) 0.057(3) 0.000(2) -0.002(3) 0.010(3) C13 0.046(3) 0.032(2) 0.067(3) 0.006(2) 0.004(2) 0.006(2) C14 0.059(3) 0.048(3) 0.066(3) 0.016(2) 0.017(3) 0.015(2) C15 0.061(3) 0.044(3) 0.072(3) 0.021(2) 0.011(3) 0.017(2) C16 0.047(3) 0.045(3) 0.072(3) 0.009(2) 0.003(3) 0.014(2) C17 0.055(3) 0.060(3) 0.068(3) 0.018(3) 0.021(3) 0.014(3) C18 0.063(3) 0.050(3) 0.066(3) 0.021(2) 0.010(3) 0.009(3) C19 0.078(4) 0.059(3) 0.080(4) 0.018(3) 0.003(3) 0.026(3) C20 0.086(5) 0.081(4) 0.105(5) 0.020(4) 0.009(4) 0.035(4) C21 0.068(4) 0.083(4) 0.067(3) 0.040(3) 0.022(3) 0.024(3) C22 0.110(6) 0.186(9) 0.101(5) 0.087(6) 0.049(5) 0.070(6) C23 0.108(6) 0.127(6) 0.083(4) 0.051(4) 0.054(4) 0.045(5) C24 0.151(8) 0.145(8) 0.085(5) 0.058(5) 0.054(5) 0.045(6) C25 0.125(7) 0.206(10) 0.101(5) 0.110(6) 0.029(5) 0.044(7) C26 0.075(4) 0.083(4) 0.068(3) 0.039(3) 0.010(3) 0.020(3) C27 0.049(3) 0.049(3) 0.053(3) 0.009(2) 0.003(2) -0.001(2) C28 0.049(3) 0.075(4) 0.064(3) 0.018(3) 0.010(3) -0.003(3) C29 0.052(4) 0.123(6) 0.099(5) 0.037(4) 0.015(3) 0.001(4) C30 0.066(4) 0.120(6) 0.136(7) 0.015(5) -0.005(5) -0.034(4) C31 0.077(5) 0.114(6) 0.103(5) -0.019(4) -0.020(4) -0.027(4) C32 0.073(4) 0.082(4) 0.102(5) -0.023(4) 0.006(4) -0.016(4) C33 0.049(3) 0.032(2) 0.053(3) 0.010(2) 0.008(2) 0.005(2) C34 0.068(3) 0.047(3) 0.055(3) 0.020(2) 0.003(3) 0.005(2) C35 0.084(4) 0.050(3) 0.069(3) 0.022(3) -0.017(3) -0.004(3) C36 0.085(4) 0.047(3) 0.102(5) 0.033(3) -0.014(4) -0.002(3) C37 0.093(5) 0.042(3) 0.099(4) 0.020(3) 0.008(4) 0.019(3) C38 0.087(4) 0.040(3) 0.063(3) 0.010(2) 0.001(3) 0.009(3) C39 0.143(8) 0.115(7) 0.153(8) 0.030(6) 0.011(7) -0.019(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 C10 2.017(5) . ? Fe1 C2 2.020(7) . ? Fe1 C9 2.024(5) . ? Fe1 C1 2.028(6) . ? Fe1 C5 2.036(6) . ? Fe1 C4 2.042(6) . ? Fe1 C8 2.045(5) . ? Fe1 C3 2.046(6) . ? Fe1 C7 2.055(4) . ? Fe1 C6 2.080(4) . ? Pd1 C6 1.999(4) . ? Pd1 N1 2.151(4) . ? Pd1 P1 2.2692(14) . ? Pd1 Cl1 2.3859(15) . ? P1 C27 1.851(5) . ? P1 C21 1.853(5) . ? P1 C33 1.854(5) . ? Cl2 C39 1.700(9) . ? Cl3 C39 1.656(10) . ? N1 C11 1.288(6) . ? N1 C13 1.437(6) . ? O1 C16 1.387(6) . ? O1 C19 1.418(7) . ? C1 C5 1.371(9) . ? C1 C2 1.419(11) . ? C1 H1A 0.9800 . ? C2 C3 1.383(11) . ? C2 H2A 0.9800 . ? C3 C4 1.359(9) . ? C3 H3A 0.9800 . ? C4 C5 1.374(8) . ? C4 H4A 0.9800 . ? C5 H5A 0.9800 . ? C6 C7 1.425(6) . ? C6 C10 1.455(6) . ? C7 C8 1.421(6) . ? C7 H7A 0.9800 . ? C8 C9 1.427(7) . ? C8 H8A 0.9800 . ? C9 C10 1.433(6) . ? C9 H9A 0.9800 . ? C10 C11 1.443(6) . ? C11 C12 1.498(6) . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 C14 1.385(7) . ? C13 C18 1.386(7) . ? C14 C15 1.378(7) . ? C14 H14A 0.9300 . ? C15 C16 1.390(7) . ? C15 H15A 0.9300 . ? C16 C17 1.381(7) . ? C17 C18 1.378(7) . ? C17 H17A 0.9300 . ? C18 H18A 0.9300 . ? C19 C20 1.470(7) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 C22 1.424(9) . ? C21 C26 1.529(7) . ? C21 H21A 0.9800 . ? C22 C23 1.533(8) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 C24 1.505(10) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 C25 1.403(11) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 C26 1.528(8) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C27 C32 1.501(7) . ? C27 C28 1.503(7) . ? C27 H27A 0.9800 . ? C28 C29 1.533(7) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C29 C30 1.446(9) . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C30 C31 1.517(10) . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C31 C32 1.556(8) . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C33 C38 1.528(6) . ? C33 C34 1.537(6) . ? C33 H33A 0.9800 . ? C34 C35 1.521(7) . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C35 C36 1.534(7) . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C36 C37 1.545(8) . ? C36 H36A 0.9700 . ? C36 H36B 0.9700 . ? C37 C38 1.529(7) . ? C37 H37A 0.9700 . ? C37 H37B 0.9700 . ? C38 H38A 0.9700 . ? C38 H38B 0.9700 . ? C39 H39A 0.9700 . ? C39 H39B 0.9700 . ? 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 C10 Fe1 C2 166.7(4) . . ? C10 Fe1 C9 41.54(19) . . ? C2 Fe1 C9 151.0(4) . . ? C10 Fe1 C1 128.1(3) . . ? C2 Fe1 C1 41.0(3) . . ? C9 Fe1 C1 164.4(3) . . ? C10 Fe1 C5 108.8(2) . . ? C2 Fe1 C5 67.5(3) . . ? C9 Fe1 C5 126.5(3) . . ? C1 Fe1 C5 39.4(3) . . ? C10 Fe1 C4 119.3(3) . . ? C2 Fe1 C4 66.6(3) . . ? C9 Fe1 C4 106.8(2) . . ? C1 Fe1 C4 66.2(3) . . ? C5 Fe1 C4 39.4(2) . . ? C10 Fe1 C8 68.76(19) . . ? C2 Fe1 C8 118.5(3) . . ? C9 Fe1 C8 41.06(19) . . ? C1 Fe1 C8 154.3(3) . . ? C5 Fe1 C8 163.7(2) . . ? C4 Fe1 C8 126.6(2) . . ? C10 Fe1 C3 151.8(3) . . ? C2 Fe1 C3 39.8(3) . . ? C9 Fe1 C3 117.3(3) . . ? C1 Fe1 C3 66.8(3) . . ? C5 Fe1 C3 66.0(3) . . ? C4 Fe1 C3 38.8(3) . . ? C8 Fe1 C3 108.0(2) . . ? C10 Fe1 C7 68.12(18) . . ? C2 Fe1 C7 109.4(2) . . ? C9 Fe1 C7 68.87(18) . . ? C1 Fe1 C7 121.6(2) . . ? C5 Fe1 C7 154.9(2) . . ? C4 Fe1 C7 164.4(3) . . ? C8 Fe1 C7 40.56(17) . . ? C3 Fe1 C7 128.6(3) . . ? C10 Fe1 C6 41.55(17) . . ? C2 Fe1 C6 128.2(3) . . ? C9 Fe1 C6 70.35(18) . . ? C1 Fe1 C6 109.4(2) . . ? C5 Fe1 C6 120.6(2) . . ? C4 Fe1 C6 154.0(3) . . ? C8 Fe1 C6 69.05(18) . . ? C3 Fe1 C6 165.6(3) . . ? C7 Fe1 C6 40.32(17) . . ? C6 Pd1 N1 80.81(16) . . ? C6 Pd1 P1 95.99(13) . . ? N1 Pd1 P1 170.75(11) . . ? C6 Pd1 Cl1 166.73(13) . . ? N1 Pd1 Cl1 90.26(11) . . ? P1 Pd1 Cl1 94.29(6) . . ? C27 P1 C21 104.3(2) . . ? C27 P1 C33 108.8(2) . . ? C21 P1 C33 104.0(2) . . ? C27 P1 Pd1 109.69(16) . . ? C21 P1 Pd1 115.3(2) . . ? C33 P1 Pd1 114.09(14) . . ? C11 N1 C13 120.2(4) . . ? C11 N1 Pd1 114.1(3) . . ? C13 N1 Pd1 125.5(3) . . ? C16 O1 C19 117.9(4) . . ? C5 C1 C2 107.7(6) . . ? C5 C1 Fe1 70.6(3) . . ? C2 C1 Fe1 69.2(4) . . ? C5 C1 H1A 126.2 . . ? C2 C1 H1A 126.2 . . ? Fe1 C1 H1A 126.2 . . ? C3 C2 C1 106.3(7) . . ? C3 C2 Fe1 71.1(4) . . ? C1 C2 Fe1 69.8(4) . . ? C3 C2 H2A 126.8 . . ? C1 C2 H2A 126.8 . . ? Fe1 C2 H2A 126.8 . . ? C4 C3 C2 108.9(7) . . ? C4 C3 Fe1 70.4(4) . . ? C2 C3 Fe1 69.1(4) . . ? C4 C3 H3A 125.5 . . ? C2 C3 H3A 125.5 . . ? Fe1 C3 H3A 125.5 . . ? C3 C4 C5 108.9(7) . . ? C3 C4 Fe1 70.7(4) . . ? C5 C4 Fe1 70.1(3) . . ? C3 C4 H4A 125.5 . . ? C5 C4 H4A 125.5 . . ? Fe1 C4 H4A 125.5 . . ? C1 C5 C4 108.2(6) . . ? C1 C5 Fe1 70.0(4) . . ? C4 C5 Fe1 70.6(3) . . ? C1 C5 H5A 125.9 . . ? C4 C5 H5A 125.9 . . ? Fe1 C5 H5A 125.9 . . ? C7 C6 C10 104.7(4) . . ? C7 C6 Pd1 143.4(3) . . ? C10 C6 Pd1 111.1(3) . . ? C7 C6 Fe1 68.9(3) . . ? C10 C6 Fe1 66.9(2) . . ? Pd1 C6 Fe1 119.3(2) . . ? C8 C7 C6 110.5(4) . . ? C8 C7 Fe1 69.3(3) . . ? C6 C7 Fe1 70.8(2) . . ? C8 C7 H7A 124.7 . . ? C6 C7 H7A 124.7 . . ? Fe1 C7 H7A 124.7 . . ? C7 C8 C9 108.2(4) . . ? C7 C8 Fe1 70.1(3) . . ? C9 C8 Fe1 68.7(3) . . ? C7 C8 H8A 125.9 . . ? C9 C8 H8A 125.9 . . ? Fe1 C8 H8A 125.9 . . ? C8 C9 C10 106.6(4) . . ? C8 C9 Fe1 70.2(3) . . ? C10 C9 Fe1 69.0(3) . . ? C8 C9 H9A 126.7 . . ? C10 C9 H9A 126.7 . . ? Fe1 C9 H9A 126.7 . . ? C9 C10 C11 130.7(4) . . ? C9 C10 C6 110.0(4) . . ? C11 C10 C6 118.4(4) . . ? C9 C10 Fe1 69.5(3) . . ? C11 C10 Fe1 116.6(3) . . ? C6 C10 Fe1 71.6(3) . . ? N1 C11 C10 115.5(4) . . ? N1 C11 C12 124.6(4) . . ? C10 C11 C12 119.9(4) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C14 C13 C18 118.6(4) . . ? C14 C13 N1 119.9(4) . . ? C18 C13 N1 121.5(4) . . ? C15 C14 C13 121.4(5) . . ? C15 C14 H14A 119.3 . . ? C13 C14 H14A 119.3 . . ? C14 C15 C16 119.7(5) . . ? C14 C15 H15A 120.2 . . ? C16 C15 H15A 120.2 . . ? C17 C16 O1 117.6(5) . . ? C17 C16 C15 119.0(5) . . ? O1 C16 C15 123.4(5) . . ? C18 C17 C16 121.1(5) . . ? C18 C17 H17A 119.4 . . ? C16 C17 H17A 119.4 . . ? C17 C18 C13 120.1(5) . . ? C17 C18 H18A 119.9 . . ? C13 C18 H18A 119.9 . . ? O1 C19 C20 109.5(5) . . ? O1 C19 H19A 109.8 . . ? C20 C19 H19A 109.8 . . ? O1 C19 H19B 109.8 . . ? C20 C19 H19B 109.8 . . ? H19A C19 H19B 108.2 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C22 C21 C26 113.9(5) . . ? C22 C21 P1 119.9(5) . . ? C26 C21 P1 111.3(4) . . ? C22 C21 H21A 103.0 . . ? C26 C21 H21A 103.0 . . ? P1 C21 H21A 103.0 . . ? C21 C22 C23 114.7(6) . . ? C21 C22 H22A 108.6 . . ? C23 C22 H22A 108.6 . . ? C21 C22 H22B 108.6 . . ? C23 C22 H22B 108.6 . . ? H22A C22 H22B 107.6 . . ? C24 C23 C22 111.3(6) . . ? C24 C23 H23A 109.4 . . ? C22 C23 H23A 109.4 . . ? C24 C23 H23B 109.4 . . ? C22 C23 H23B 109.4 . . ? H23A C23 H23B 108.0 . . ? C25 C24 C23 114.9(7) . . ? C25 C24 H24A 108.5 . . ? C23 C24 H24A 108.5 . . ? C25 C24 H24B 108.5 . . ? C23 C24 H24B 108.5 . . ? H24A C24 H24B 107.5 . . ? C24 C25 C26 117.3(7) . . ? C24 C25 H25A 108.0 . . ? C26 C25 H25A 108.0 . . ? C24 C25 H25B 108.0 . . ? C26 C25 H25B 108.0 . . ? H25A C25 H25B 107.2 . . ? C25 C26 C21 112.4(5) . . ? C25 C26 H26A 109.1 . . ? C21 C26 H26A 109.1 . . ? C25 C26 H26B 109.1 . . ? C21 C26 H26B 109.1 . . ? H26A C26 H26B 107.9 . . ? C32 C27 C28 111.2(5) . . ? C32 C27 P1 120.8(4) . . ? C28 C27 P1 113.9(3) . . ? C32 C27 H27A 102.7 . . ? C28 C27 H27A 102.7 . . ? P1 C27 H27A 102.7 . . ? C27 C28 C29 111.4(5) . . ? C27 C28 H28A 109.4 . . ? C29 C28 H28A 109.4 . . ? C27 C28 H28B 109.4 . . ? C29 C28 H28B 109.4 . . ? H28A C28 H28B 108.0 . . ? C30 C29 C28 113.1(6) . . ? C30 C29 H29A 109.0 . . ? C28 C29 H29A 109.0 . . ? C30 C29 H29B 109.0 . . ? C28 C29 H29B 109.0 . . ? H29A C29 H29B 107.8 . . ? C29 C30 C31 112.2(6) . . ? C29 C30 H30A 109.2 . . ? C31 C30 H30A 109.2 . . ? C29 C30 H30B 109.2 . . ? C31 C30 H30B 109.2 . . ? H30A C30 H30B 107.9 . . ? C30 C31 C32 111.2(6) . . ? C30 C31 H31A 109.4 . . ? C32 C31 H31A 109.4 . . ? C30 C31 H31B 109.4 . . ? C32 C31 H31B 109.4 . . ? H31A C31 H31B 108.0 . . ? C27 C32 C31 110.3(5) . . ? C27 C32 H32A 109.6 . . ? C31 C32 H32A 109.6 . . ? C27 C32 H32B 109.6 . . ? C31 C32 H32B 109.6 . . ? H32A C32 H32B 108.1 . . ? C38 C33 C34 109.5(4) . . ? C38 C33 P1 116.4(3) . . ? C34 C33 P1 113.9(3) . . ? C38 C33 H33A 105.3 . . ? C34 C33 H33A 105.3 . . ? P1 C33 H33A 105.3 . . ? C35 C34 C33 110.2(4) . . ? C35 C34 H34A 109.6 . . ? C33 C34 H34A 109.6 . . ? C35 C34 H34B 109.6 . . ? C33 C34 H34B 109.6 . . ? H34A C34 H34B 108.1 . . ? C34 C35 C36 111.6(4) . . ? C34 C35 H35A 109.3 . . ? C36 C35 H35A 109.3 . . ? C34 C35 H35B 109.3 . . ? C36 C35 H35B 109.3 . . ? H35A C35 H35B 108.0 . . ? C35 C36 C37 111.0(4) . . ? C35 C36 H36A 109.4 . . ? C37 C36 H36A 109.4 . . ? C35 C36 H36B 109.4 . . ? C37 C36 H36B 109.4 . . ? H36A C36 H36B 108.0 . . ? C38 C37 C36 110.3(5) . . ? C38 C37 H37A 109.6 . . ? C36 C37 H37A 109.6 . . ? C38 C37 H37B 109.6 . . ? C36 C37 H37B 109.6 . . ? H37A C37 H37B 108.1 . . ? C33 C38 C37 110.9(4) . . ? C33 C38 H38A 109.5 . . ? C37 C38 H38A 109.5 . . ? C33 C38 H38B 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 108.0 . . ? Cl3 C39 Cl2 115.0(6) . . ? Cl3 C39 H39A 108.5 . . ? Cl2 C39 H39A 108.5 . . ? Cl3 C39 H39B 108.5 . . ? Cl2 C39 H39B 108.5 . . ? H39A C39 H39B 107.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 Pd1 P1 C27 -162.0(2) . . . . ? N1 Pd1 P1 C27 -92.8(7) . . . . ? Cl1 Pd1 P1 C27 26.41(18) . . . . ? C6 Pd1 P1 C21 80.6(2) . . . . ? N1 Pd1 P1 C21 149.8(7) . . . . ? Cl1 Pd1 P1 C21 -90.9(2) . . . . ? C6 Pd1 P1 C33 -39.6(2) . . . . ? N1 Pd1 P1 C33 29.6(7) . . . . ? Cl1 Pd1 P1 C33 148.79(18) . . . . ? C6 Pd1 N1 C11 -0.9(3) . . . . ? P1 Pd1 N1 C11 -71.3(8) . . . . ? Cl1 Pd1 N1 C11 169.2(3) . . . . ? C6 Pd1 N1 C13 -175.4(4) . . . . ? P1 Pd1 N1 C13 114.3(6) . . . . ? Cl1 Pd1 N1 C13 -5.3(4) . . . . ? C10 Fe1 C1 C5 -72.0(4) . . . . ? C2 Fe1 C1 C5 118.6(6) . . . . ? C9 Fe1 C1 C5 -28.7(11) . . . . ? C4 Fe1 C1 C5 37.4(4) . . . . ? C8 Fe1 C1 C5 163.3(5) . . . . ? C3 Fe1 C1 C5 79.9(4) . . . . ? C7 Fe1 C1 C5 -157.8(3) . . . . ? C6 Fe1 C1 C5 -114.9(4) . . . . ? C10 Fe1 C1 C2 169.4(4) . . . . ? C9 Fe1 C1 C2 -147.3(9) . . . . ? C5 Fe1 C1 C2 -118.6(6) . . . . ? C4 Fe1 C1 C2 -81.2(5) . . . . ? C8 Fe1 C1 C2 44.7(8) . . . . ? C3 Fe1 C1 C2 -38.6(4) . . . . ? C7 Fe1 C1 C2 83.6(5) . . . . ? C6 Fe1 C1 C2 126.5(5) . . . . ? C5 C1 C2 C3 1.8(7) . . . . ? Fe1 C1 C2 C3 62.2(5) . . . . ? C5 C1 C2 Fe1 -60.4(4) . . . . ? C10 Fe1 C2 C3 -155.4(9) . . . . ? C9 Fe1 C2 C3 46.3(8) . . . . ? C1 Fe1 C2 C3 -116.2(6) . . . . ? C5 Fe1 C2 C3 -79.1(5) . . . . ? C4 Fe1 C2 C3 -36.2(4) . . . . ? C8 Fe1 C2 C3 84.1(5) . . . . ? C7 Fe1 C2 C3 127.6(5) . . . . ? C6 Fe1 C2 C3 168.9(4) . . . . ? C10 Fe1 C2 C1 -39.2(13) . . . . ? C9 Fe1 C2 C1 162.5(5) . . . . ? C5 Fe1 C2 C1 37.1(4) . . . . ? C4 Fe1 C2 C1 80.0(4) . . . . ? C8 Fe1 C2 C1 -159.7(4) . . . . ? C3 Fe1 C2 C1 116.2(6) . . . . ? C7 Fe1 C2 C1 -116.2(4) . . . . ? C6 Fe1 C2 C1 -74.9(5) . . . . ? C1 C2 C3 C4 -1.9(8) . . . . ? Fe1 C2 C3 C4 59.4(5) . . . . ? C1 C2 C3 Fe1 -61.3(5) . . . . ? C10 Fe1 C3 C4 48.1(7) . . . . ? C2 Fe1 C3 C4 -120.2(7) . . . . ? C9 Fe1 C3 C4 83.0(5) . . . . ? C1 Fe1 C3 C4 -80.4(5) . . . . ? C5 Fe1 C3 C4 -37.2(4) . . . . ? C8 Fe1 C3 C4 126.6(4) . . . . ? C7 Fe1 C3 C4 166.8(4) . . . . ? C6 Fe1 C3 C4 -157.7(8) . . . . ? C10 Fe1 C3 C2 168.3(5) . . . . ? C9 Fe1 C3 C2 -156.8(5) . . . . ? C1 Fe1 C3 C2 39.9(5) . . . . ? C5 Fe1 C3 C2 83.1(5) . . . . ? C4 Fe1 C3 C2 120.2(7) . . . . ? C8 Fe1 C3 C2 -113.2(5) . . . . ? C7 Fe1 C3 C2 -72.9(6) . . . . ? C6 Fe1 C3 C2 -37.5(12) . . . . ? C2 C3 C4 C5 1.3(8) . . . . ? Fe1 C3 C4 C5 59.9(4) . . . . ? C2 C3 C4 Fe1 -58.6(5) . . . . ? C10 Fe1 C4 C3 -156.2(4) . . . . ? C2 Fe1 C4 C3 37.0(5) . . . . ? C9 Fe1 C4 C3 -112.9(5) . . . . ? C1 Fe1 C4 C3 82.0(5) . . . . ? C5 Fe1 C4 C3 119.5(6) . . . . ? C8 Fe1 C4 C3 -72.0(5) . . . . ? C7 Fe1 C4 C3 -41.4(11) . . . . ? C6 Fe1 C4 C3 167.6(5) . . . . ? C10 Fe1 C4 C5 84.3(5) . . . . ? C2 Fe1 C4 C5 -82.5(5) . . . . ? C9 Fe1 C4 C5 127.6(4) . . . . ? C1 Fe1 C4 C5 -37.5(4) . . . . ? C8 Fe1 C4 C5 168.4(4) . . . . ? C3 Fe1 C4 C5 -119.5(6) . . . . ? C7 Fe1 C4 C5 -161.0(8) . . . . ? C6 Fe1 C4 C5 48.1(7) . . . . ? C2 C1 C5 C4 -1.0(7) . . . . ? Fe1 C1 C5 C4 -60.5(4) . . . . ? C2 C1 C5 Fe1 59.5(4) . . . . ? C3 C4 C5 C1 -0.2(7) . . . . ? Fe1 C4 C5 C1 60.1(4) . . . . ? C3 C4 C5 Fe1 -60.3(5) . . . . ? C10 Fe1 C5 C1 127.8(4) . . . . ? C2 Fe1 C5 C1 -38.6(5) . . . . ? C9 Fe1 C5 C1 170.8(4) . . . . ? C4 Fe1 C5 C1 -118.7(6) . . . . ? C8 Fe1 C5 C1 -153.7(8) . . . . ? C3 Fe1 C5 C1 -82.1(5) . . . . ? C7 Fe1 C5 C1 49.3(7) . . . . ? C6 Fe1 C5 C1 83.6(5) . . . . ? C10 Fe1 C5 C4 -113.5(4) . . . . ? C2 Fe1 C5 C4 80.1(5) . . . . ? C9 Fe1 C5 C4 -70.5(5) . . . . ? C1 Fe1 C5 C4 118.7(6) . . . . ? C8 Fe1 C5 C4 -34.9(10) . . . . ? C3 Fe1 C5 C4 36.7(4) . . . . ? C7 Fe1 C5 C4 168.1(5) . . . . ? C6 Fe1 C5 C4 -157.7(4) . . . . ? N1 Pd1 C6 C7 167.1(6) . . . . ? P1 Pd1 C6 C7 -21.7(6) . . . . ? Cl1 Pd1 C6 C7 118.9(6) . . . . ? N1 Pd1 C6 C10 -1.1(3) . . . . ? P1 Pd1 C6 C10 170.1(3) . . . . ? Cl1 Pd1 C6 C10 -49.4(7) . . . . ? N1 Pd1 C6 Fe1 73.5(2) . . . . ? P1 Pd1 C6 Fe1 -115.3(2) . . . . ? Cl1 Pd1 C6 Fe1 25.2(7) . . . . ? C10 Fe1 C6 C7 117.5(3) . . . . ? C2 Fe1 C6 C7 -74.2(5) . . . . ? C9 Fe1 C6 C7 80.2(3) . . . . ? C1 Fe1 C6 C7 -116.4(4) . . . . ? C5 Fe1 C6 C7 -158.4(3) . . . . ? C4 Fe1 C6 C7 168.4(5) . . . . ? C8 Fe1 C6 C7 36.3(3) . . . . ? C3 Fe1 C6 C7 -44.5(10) . . . . ? C2 Fe1 C6 C10 168.4(4) . . . . ? C9 Fe1 C6 C10 -37.3(3) . . . . ? C1 Fe1 C6 C10 126.1(4) . . . . ? C5 Fe1 C6 C10 84.1(3) . . . . ? C4 Fe1 C6 C10 50.9(6) . . . . ? C8 Fe1 C6 C10 -81.2(3) . . . . ? C3 Fe1 C6 C10 -161.9(9) . . . . ? C7 Fe1 C6 C10 -117.5(3) . . . . ? C10 Fe1 C6 Pd1 -102.1(3) . . . . ? C2 Fe1 C6 Pd1 66.2(5) . . . . ? C9 Fe1 C6 Pd1 -139.4(3) . . . . ? C1 Fe1 C6 Pd1 24.0(4) . . . . ? C5 Fe1 C6 Pd1 -18.0(4) . . . . ? C4 Fe1 C6 Pd1 -51.2(6) . . . . ? C8 Fe1 C6 Pd1 176.7(3) . . . . ? C3 Fe1 C6 Pd1 95.9(10) . . . . ? C7 Fe1 C6 Pd1 140.4(4) . . . . ? C10 C6 C7 C8 -0.5(5) . . . . ? Pd1 C6 C7 C8 -169.2(4) . . . . ? Fe1 C6 C7 C8 -58.1(3) . . . . ? C10 C6 C7 Fe1 57.5(3) . . . . ? Pd1 C6 C7 Fe1 -111.1(5) . . . . ? C10 Fe1 C7 C8 82.5(3) . . . . ? C2 Fe1 C7 C8 -111.5(5) . . . . ? C9 Fe1 C7 C8 37.7(3) . . . . ? C1 Fe1 C7 C8 -155.3(4) . . . . ? C5 Fe1 C7 C8 170.3(5) . . . . ? C4 Fe1 C7 C8 -39.0(10) . . . . ? C3 Fe1 C7 C8 -71.0(4) . . . . ? C6 Fe1 C7 C8 121.8(4) . . . . ? C10 Fe1 C7 C6 -39.4(2) . . . . ? C2 Fe1 C7 C6 126.7(4) . . . . ? C9 Fe1 C7 C6 -84.2(3) . . . . ? C1 Fe1 C7 C6 82.9(4) . . . . ? C5 Fe1 C7 C6 48.5(6) . . . . ? C4 Fe1 C7 C6 -160.8(9) . . . . ? C8 Fe1 C7 C6 -121.8(4) . . . . ? C3 Fe1 C7 C6 167.1(4) . . . . ? C6 C7 C8 C9 0.6(5) . . . . ? Fe1 C7 C8 C9 -58.3(3) . . . . ? C6 C7 C8 Fe1 58.9(3) . . . . ? C10 Fe1 C8 C7 -80.8(3) . . . . ? C2 Fe1 C8 C7 87.0(5) . . . . ? C9 Fe1 C8 C7 -119.8(4) . . . . ? C1 Fe1 C8 C7 55.3(7) . . . . ? C5 Fe1 C8 C7 -165.3(8) . . . . ? C4 Fe1 C8 C7 167.9(4) . . . . ? C3 Fe1 C8 C7 129.0(4) . . . . ? C6 Fe1 C8 C7 -36.1(3) . . . . ? C10 Fe1 C8 C9 39.1(3) . . . . ? C2 Fe1 C8 C9 -153.2(4) . . . . ? C1 Fe1 C8 C9 175.1(5) . . . . ? C5 Fe1 C8 C9 -45.4(9) . . . . ? C4 Fe1 C8 C9 -72.3(4) . . . . ? C3 Fe1 C8 C9 -111.2(4) . . . . ? C7 Fe1 C8 C9 119.8(4) . . . . ? C6 Fe1 C8 C9 83.8(3) . . . . ? C7 C8 C9 C10 -0.5(5) . . . . ? Fe1 C8 C9 C10 -59.6(3) . . . . ? C7 C8 C9 Fe1 59.2(3) . . . . ? C10 Fe1 C9 C8 -117.6(4) . . . . ? C2 Fe1 C9 C8 55.0(6) . . . . ? C1 Fe1 C9 C8 -172.1(8) . . . . ? C5 Fe1 C9 C8 165.6(3) . . . . ? C4 Fe1 C9 C8 126.9(4) . . . . ? C3 Fe1 C9 C8 86.4(4) . . . . ? C7 Fe1 C9 C8 -37.2(3) . . . . ? C6 Fe1 C9 C8 -80.3(3) . . . . ? C2 Fe1 C9 C10 172.7(5) . . . . ? C1 Fe1 C9 C10 -54.5(9) . . . . ? C5 Fe1 C9 C10 -76.8(4) . . . . ? C4 Fe1 C9 C10 -115.4(3) . . . . ? C8 Fe1 C9 C10 117.6(4) . . . . ? C3 Fe1 C9 C10 -156.0(4) . . . . ? C7 Fe1 C9 C10 80.4(3) . . . . ? C6 Fe1 C9 C10 37.3(3) . . . . ? C8 C9 C10 C11 168.4(5) . . . . ? Fe1 C9 C10 C11 108.0(5) . . . . ? C8 C9 C10 C6 0.1(5) . . . . ? Fe1 C9 C10 C6 -60.3(3) . . . . ? C8 C9 C10 Fe1 60.5(3) . . . . ? C7 C6 C10 C9 0.2(5) . . . . ? Pd1 C6 C10 C9 173.0(3) . . . . ? Fe1 C6 C10 C9 59.1(3) . . . . ? C7 C6 C10 C11 -169.7(4) . . . . ? Pd1 C6 C10 C11 3.1(5) . . . . ? Fe1 C6 C10 C11 -110.9(4) . . . . ? C7 C6 C10 Fe1 -58.8(3) . . . . ? Pd1 C6 C10 Fe1 113.9(2) . . . . ? C2 Fe1 C10 C9 -164.3(10) . . . . ? C1 Fe1 C10 C9 163.8(3) . . . . ? C5 Fe1 C10 C9 124.2(3) . . . . ? C4 Fe1 C10 C9 82.4(4) . . . . ? C8 Fe1 C10 C9 -38.6(3) . . . . ? C3 Fe1 C10 C9 50.0(6) . . . . ? C7 Fe1 C10 C9 -82.4(3) . . . . ? C6 Fe1 C10 C9 -120.6(4) . . . . ? C2 Fe1 C10 C11 69.4(12) . . . . ? C9 Fe1 C10 C11 -126.3(5) . . . . ? C1 Fe1 C10 C11 37.6(5) . . . . ? C5 Fe1 C10 C11 -2.1(4) . . . . ? C4 Fe1 C10 C11 -43.9(4) . . . . ? C8 Fe1 C10 C11 -164.9(4) . . . . ? C3 Fe1 C10 C11 -76.2(6) . . . . ? C7 Fe1 C10 C11 151.4(4) . . . . ? C6 Fe1 C10 C11 113.1(4) . . . . ? C2 Fe1 C10 C6 -43.7(12) . . . . ? C9 Fe1 C10 C6 120.6(4) . . . . ? C1 Fe1 C10 C6 -75.6(4) . . . . ? C5 Fe1 C10 C6 -115.2(3) . . . . ? C4 Fe1 C10 C6 -157.0(3) . . . . ? C8 Fe1 C10 C6 82.0(3) . . . . ? C3 Fe1 C10 C6 170.6(5) . . . . ? C7 Fe1 C10 C6 38.2(2) . . . . ? C13 N1 C11 C10 177.6(4) . . . . ? Pd1 N1 C11 C10 2.8(5) . . . . ? C13 N1 C11 C12 -0.3(7) . . . . ? Pd1 N1 C11 C12 -175.1(4) . . . . ? C9 C10 C11 N1 -171.5(5) . . . . ? C6 C10 C11 N1 -4.0(6) . . . . ? Fe1 C10 C11 N1 -86.5(5) . . . . ? C9 C10 C11 C12 6.5(8) . . . . ? C6 C10 C11 C12 174.0(4) . . . . ? Fe1 C10 C11 C12 91.6(5) . . . . ? C11 N1 C13 C14 -94.2(6) . . . . ? Pd1 N1 C13 C14 79.9(5) . . . . ? C11 N1 C13 C18 85.9(6) . . . . ? Pd1 N1 C13 C18 -100.0(5) . . . . ? C18 C13 C14 C15 -1.6(7) . . . . ? N1 C13 C14 C15 178.5(4) . . . . ? C13 C14 C15 C16 -0.2(8) . . . . ? C19 O1 C16 C17 -168.8(5) . . . . ? C19 O1 C16 C15 11.1(7) . . . . ? C14 C15 C16 C17 2.3(8) . . . . ? C14 C15 C16 O1 -177.6(4) . . . . ? O1 C16 C17 C18 177.2(4) . . . . ? C15 C16 C17 C18 -2.7(8) . . . . ? C16 C17 C18 C13 0.9(8) . . . . ? C14 C13 C18 C17 1.2(7) . . . . ? N1 C13 C18 C17 -178.9(4) . . . . ? C16 O1 C19 C20 173.8(5) . . . . ? C27 P1 C21 C22 156.4(6) . . . . ? C33 P1 C21 C22 42.4(7) . . . . ? Pd1 P1 C21 C22 -83.3(6) . . . . ? C27 P1 C21 C26 -67.0(5) . . . . ? C33 P1 C21 C26 179.0(4) . . . . ? Pd1 P1 C21 C26 53.3(5) . . . . ? C26 C21 C22 C23 49.6(10) . . . . ? P1 C21 C22 C23 -174.9(5) . . . . ? C21 C22 C23 C24 -50.7(11) . . . . ? C22 C23 C24 C25 47.5(12) . . . . ? C23 C24 C25 C26 -45.0(12) . . . . ? C24 C25 C26 C21 41.6(11) . . . . ? C22 C21 C26 C25 -43.3(9) . . . . ? P1 C21 C26 C25 177.4(5) . . . . ? C21 P1 C27 C32 -39.4(5) . . . . ? C33 P1 C27 C32 71.1(5) . . . . ? Pd1 P1 C27 C32 -163.5(5) . . . . ? C21 P1 C27 C28 -175.8(4) . . . . ? C33 P1 C27 C28 -65.3(4) . . . . ? Pd1 P1 C27 C28 60.2(4) . . . . ? C32 C27 C28 C29 55.1(7) . . . . ? P1 C27 C28 C29 -164.4(4) . . . . ? C27 C28 C29 C30 -54.1(8) . . . . ? C28 C29 C30 C31 53.4(9) . . . . ? C29 C30 C31 C32 -53.7(9) . . . . ? C28 C27 C32 C31 -55.9(7) . . . . ? P1 C27 C32 C31 166.8(5) . . . . ? C30 C31 C32 C27 54.6(9) . . . . ? C27 P1 C33 C38 -46.7(4) . . . . ? C21 P1 C33 C38 64.1(4) . . . . ? Pd1 P1 C33 C38 -169.5(3) . . . . ? C27 P1 C33 C34 82.2(4) . . . . ? C21 P1 C33 C34 -167.1(4) . . . . ? Pd1 P1 C33 C34 -40.6(4) . . . . ? C38 C33 C34 C35 -59.1(5) . . . . ? P1 C33 C34 C35 168.5(3) . . . . ? C33 C34 C35 C36 57.3(6) . . . . ? C34 C35 C36 C37 -54.9(7) . . . . ? C35 C36 C37 C38 54.4(7) . . . . ? C34 C33 C38 C37 59.7(6) . . . . ? P1 C33 C38 C37 -169.2(4) . . . . ? C36 C37 C38 C33 -57.4(6) . . . . ? _diffrn_measured_fraction_theta_max 0.875 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.875 _refine_diff_density_max 0.944 _refine_diff_density_min -0.763 _refine_diff_density_rms 0.075 # Attachment 'Complex 2g.cif' data_p-1_2g _database_code_depnum_ccdc_archive 'CCDC 602221' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C37 H50 Cl4 Fe N P Pd' _chemical_formula_weight 843.80 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.319(2) _cell_length_b 11.270(2) _cell_length_c 18.101(4) _cell_angle_alpha 78.72(3) _cell_angle_beta 74.37(3) _cell_angle_gamma 68.02(3) _cell_volume 1869.2(7) _cell_formula_units_Z 2 _cell_measurement_temperature 291(2) _cell_measurement_reflns_used 368 _cell_measurement_theta_min 2 _cell_measurement_theta_max 25.1 _exptl_crystal_description PRISMATIC _exptl_crystal_colour RED _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.499 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 868 _exptl_absorpt_coefficient_mu 1.225 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7917 _exptl_absorpt_correction_T_max 0.8188 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 291(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type R-AXIS-IV _diffrn_measurement_method 'Oscillation frames' _diffrn_detector_area_resol_mean 0 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% ? _diffrn_reflns_number 5754 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0644 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.17 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5754 _reflns_number_gt 4546 _reflns_threshold_expression >2sigma(I) _computing_data_collection raxis _computing_cell_refinement raxis _computing_data_reduction raxis _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics texsan _computing_publication_material texsan _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0656P)^2^+3.8250P] 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 fxed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0009(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 5754 _refine_ls_number_parameters 407 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0798 _refine_ls_R_factor_gt 0.0579 _refine_ls_wR_factor_ref 0.1383 _refine_ls_wR_factor_gt 0.1297 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.036 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.63989(5) 0.87804(4) 0.68314(3) 0.03126(17) Uani 1 1 d . . . Fe1 Fe 1.02423(10) 0.69752(9) 0.63727(6) 0.0450(3) Uani 1 1 d . . . N1 N 0.7016(6) 0.8165(5) 0.5690(3) 0.0405(13) Uani 1 1 d . . . P1 P 0.58633(18) 0.95701(15) 0.79853(9) 0.0337(4) Uani 1 1 d . . . Cl1 Cl 0.39815(18) 0.89435(17) 0.68963(10) 0.0476(4) Uani 1 1 d . . . Cl2 Cl 0.6298(3) 0.5755(2) 0.64487(12) 0.0695(6) Uani 1 1 d . . . Cl3 Cl 1.3235(4) 0.5130(3) 0.84421(19) 0.1139(10) Uani 1 1 d . . . Cl4 Cl 1.1550(3) 0.7678(3) 0.8889(2) 0.1203(11) Uani 1 1 d . . . C1 C 0.9532(9) 0.5474(7) 0.6912(5) 0.056(2) Uani 1 1 d . . . H1A H 0.8554 0.5555 0.7195 0.067 Uiso 1 1 calc R . . C2 C 1.0648(8) 0.5461(7) 0.7232(5) 0.056(2) Uani 1 1 d . . . H2A H 1.0585 0.5526 0.7774 0.067 Uiso 1 1 calc R . . C3 C 1.1888(8) 0.5335(7) 0.6616(5) 0.061(2) Uani 1 1 d . . . H3A H 1.2822 0.5305 0.6666 0.073 Uiso 1 1 calc R . . C4 C 1.1549(9) 0.5250(7) 0.5931(5) 0.060(2) Uani 1 1 d . . . H4A H 1.2199 0.5150 0.5422 0.073 Uiso 1 1 calc R . . C5 C 1.0069(9) 0.5359(7) 0.6108(5) 0.061(2) Uani 1 1 d . . . H5A H 0.9531 0.5336 0.5743 0.073 Uiso 1 1 calc R . . C6 C 0.8465(7) 0.8630(6) 0.6557(4) 0.0395(15) Uani 1 1 d . . . C7 C 0.9614(7) 0.8669(6) 0.6852(4) 0.0430(16) Uani 1 1 d . . . H7A H 0.9563 0.8736 0.7391 0.052 Uiso 1 1 calc R . . C8 C 1.0864(8) 0.8556(7) 0.6234(4) 0.0509(18) Uani 1 1 d . . . H8A H 1.1793 0.8545 0.6281 0.061 Uiso 1 1 calc R . . C9 C 1.0515(8) 0.8446(7) 0.5550(4) 0.0515(18) Uani 1 1 d . . . H9A H 1.1150 0.8359 0.5037 0.062 Uiso 1 1 calc R . . C10 C 0.9052(7) 0.8490(6) 0.5751(4) 0.0442(16) Uani 1 1 d . . . C11 C 0.8270(8) 0.8180(6) 0.5307(4) 0.0421(16) Uani 1 1 d . . . C12 C 0.8932(9) 0.7879(8) 0.4492(4) 0.061(2) Uani 1 1 d . . . H12A H 0.8268 0.7702 0.4284 0.091 Uiso 1 1 calc R . . H12B H 0.9788 0.7140 0.4480 0.091 Uiso 1 1 calc R . . H12C H 0.9163 0.8602 0.4189 0.091 Uiso 1 1 calc R . . C13 C 0.6125(7) 0.7802(6) 0.5350(4) 0.0426(16) Uani 1 1 d . . . C14 C 0.5693(8) 0.6746(6) 0.5649(4) 0.0471(18) Uani 1 1 d . . . C15 C 0.4807(8) 0.6420(7) 0.5338(5) 0.0530(19) Uani 1 1 d . . . H15A H 0.4544 0.5702 0.5552 0.064 Uiso 1 1 calc R . . C16 C 0.4323(8) 0.7167(7) 0.4711(4) 0.055(2) Uani 1 1 d . . . H16A H 0.3715 0.6961 0.4501 0.067 Uiso 1 1 calc R . . C17 C 0.4726(9) 0.8223(8) 0.4386(4) 0.061(2) Uani 1 1 d . . . H17A H 0.4394 0.8716 0.3956 0.073 Uiso 1 1 calc R . . C18 C 0.5621(8) 0.8560(7) 0.4693(4) 0.0519(19) Uani 1 1 d . . . H18A H 0.5889 0.9274 0.4471 0.062 Uiso 1 1 calc R . . C19 C 0.3905(7) 1.0377(6) 0.8308(3) 0.0394(15) Uani 1 1 d . . . H19A H 0.3477 0.9785 0.8224 0.047 Uiso 1 1 calc R . . C20 C 0.3294(7) 1.1622(6) 0.7802(4) 0.0474(17) Uani 1 1 d . . . H20A H 0.3615 1.2284 0.7883 0.057 Uiso 1 1 calc R . . H20B H 0.3640 1.1472 0.7262 0.057 Uiso 1 1 calc R . . C21 C 0.1669(8) 1.2072(8) 0.8002(5) 0.060(2) Uani 1 1 d . . . H21A H 0.1297 1.2871 0.7687 0.072 Uiso 1 1 calc R . . H21B H 0.1356 1.1436 0.7878 0.072 Uiso 1 1 calc R . . C22 C 0.1061(9) 1.2277(8) 0.8840(5) 0.067(2) Uani 1 1 d . . . H22A H 0.0028 1.2511 0.8945 0.080 Uiso 1 1 calc R . . H22B H 0.1276 1.2982 0.8951 0.080 Uiso 1 1 calc R . . C23 C 0.1673(8) 1.1075(8) 0.9358(4) 0.063(2) Uani 1 1 d . . . H23A H 0.1344 1.0406 0.9297 0.075 Uiso 1 1 calc R . . H23B H 0.1321 1.1260 0.9891 0.075 Uiso 1 1 calc R . . C24 C 0.3306(8) 1.0588(8) 0.9175(4) 0.0554(19) Uani 1 1 d . . . H24A H 0.3656 0.9783 0.9490 0.066 Uiso 1 1 calc R . . H24B H 0.3641 1.1208 0.9298 0.066 Uiso 1 1 calc R . . C25 C 0.6831(7) 1.0641(6) 0.8011(3) 0.0371(15) Uani 1 1 d . . . H25A H 0.7822 1.0072 0.7998 0.045 Uiso 1 1 calc R . . C26 C 0.6921(8) 1.1636(6) 0.7290(4) 0.0455(17) Uani 1 1 d . . . H26A H 0.7237 1.1204 0.6827 0.055 Uiso 1 1 calc R . . H26B H 0.5980 1.2275 0.7285 0.055 Uiso 1 1 calc R . . C27 C 0.7961(8) 1.2296(7) 0.7298(4) 0.0534(19) Uani 1 1 d . . . H27A H 0.8918 1.1666 0.7246 0.064 Uiso 1 1 calc R . . H27B H 0.7962 1.2943 0.6858 0.064 Uiso 1 1 calc R . . C28 C 0.7595(9) 1.2922(7) 0.8020(5) 0.061(2) Uani 1 1 d . . . H28A H 0.6703 1.3640 0.8035 0.073 Uiso 1 1 calc R . . H28B H 0.8338 1.3256 0.8015 0.073 Uiso 1 1 calc R . . C29 C 0.7448(9) 1.1965(8) 0.8745(5) 0.062(2) Uani 1 1 d . . . H29A H 0.8376 1.1314 0.8769 0.075 Uiso 1 1 calc R . . H29B H 0.7120 1.2417 0.9201 0.075 Uiso 1 1 calc R . . C30 C 0.6396(8) 1.1319(7) 0.8735(4) 0.0510(19) Uani 1 1 d . . . H30A H 0.5449 1.1962 0.8759 0.061 Uiso 1 1 calc R . . H30B H 0.6353 1.0697 0.9187 0.061 Uiso 1 1 calc R . . C31 C 0.6317(7) 0.8245(6) 0.8761(4) 0.0383(15) Uani 1 1 d . . . H31A H 0.5914 0.8612 0.9256 0.046 Uiso 1 1 calc R . . C32 C 0.7923(8) 0.7573(6) 0.8698(4) 0.0478(17) Uani 1 1 d . . . H32A H 0.8342 0.8183 0.8752 0.057 Uiso 1 1 calc R . . H32B H 0.8359 0.7275 0.8192 0.057 Uiso 1 1 calc R . . C33 C 0.8251(9) 0.6420(7) 0.9320(4) 0.059(2) Uani 1 1 d . . . H33A H 0.9279 0.5989 0.9241 0.070 Uiso 1 1 calc R . . H33B H 0.7915 0.6732 0.9824 0.070 Uiso 1 1 calc R . . C34 C 0.7551(10) 0.5463(7) 0.9303(5) 0.063(2) Uani 1 1 d . . . H34A H 0.7959 0.5078 0.8820 0.075 Uiso 1 1 calc R . . H34B H 0.7737 0.4782 0.9721 0.075 Uiso 1 1 calc R . . C35 C 0.5955(10) 0.6118(7) 0.9382(5) 0.068(2) Uani 1 1 d . . . H35A H 0.5536 0.6423 0.9887 0.082 Uiso 1 1 calc R . . H35B H 0.5536 0.5500 0.9341 0.082 Uiso 1 1 calc R . . C36 C 0.5601(8) 0.7255(7) 0.8761(4) 0.0520(19) Uani 1 1 d . . . H36A H 0.4572 0.7680 0.8849 0.062 Uiso 1 1 calc R . . H36B H 0.5923 0.6937 0.8259 0.062 Uiso 1 1 calc R . . C37 C 1.2593(11) 0.6774(9) 0.8134(6) 0.084(3) Uani 1 1 d . . . H37A H 1.3397 0.7064 0.7887 0.101 Uiso 1 1 calc R . . H37B H 1.2030 0.6911 0.7754 0.101 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.0382(3) 0.0282(3) 0.0283(3) 0.00022(19) -0.0071(2) -0.0141(2) Fe1 0.0424(6) 0.0336(5) 0.0550(6) -0.0058(5) -0.0029(5) -0.0132(5) N1 0.048(3) 0.033(3) 0.041(3) -0.006(2) -0.003(3) -0.017(3) P1 0.0421(10) 0.0311(8) 0.0280(8) -0.0005(7) -0.0086(7) -0.0131(7) Cl1 0.0458(10) 0.0585(11) 0.0445(9) -0.0108(8) -0.0069(8) -0.0237(9) Cl2 0.0917(16) 0.0558(12) 0.0669(13) 0.0169(10) -0.0322(12) -0.0330(12) Cl3 0.133(3) 0.088(2) 0.116(2) 0.0119(17) -0.051(2) -0.0260(19) Cl4 0.087(2) 0.119(2) 0.155(3) -0.041(2) 0.0001(19) -0.0401(18) C1 0.056(5) 0.038(4) 0.067(5) 0.000(4) -0.009(4) -0.016(4) C2 0.063(5) 0.038(4) 0.056(5) -0.001(4) -0.013(4) -0.008(4) C3 0.044(4) 0.045(4) 0.080(6) -0.019(4) -0.005(4) 0.001(4) C4 0.061(5) 0.040(4) 0.066(5) -0.027(4) 0.006(4) -0.003(4) C5 0.070(6) 0.035(4) 0.078(6) -0.015(4) -0.014(5) -0.015(4) C6 0.047(4) 0.035(3) 0.041(4) 0.004(3) -0.013(3) -0.020(3) C7 0.051(4) 0.031(3) 0.049(4) 0.000(3) -0.014(3) -0.014(3) C8 0.042(4) 0.044(4) 0.069(5) -0.007(4) -0.005(4) -0.022(3) C9 0.046(4) 0.048(4) 0.055(5) -0.002(4) 0.002(4) -0.021(4) C10 0.050(4) 0.035(4) 0.047(4) 0.005(3) -0.012(3) -0.018(3) C11 0.061(5) 0.027(3) 0.033(3) -0.003(3) -0.001(3) -0.016(3) C12 0.070(5) 0.068(5) 0.044(4) -0.010(4) 0.006(4) -0.035(4) C13 0.053(4) 0.039(4) 0.033(3) -0.012(3) 0.002(3) -0.016(3) C14 0.057(5) 0.037(4) 0.043(4) -0.001(3) -0.009(3) -0.014(3) C15 0.050(4) 0.049(4) 0.065(5) -0.013(4) -0.009(4) -0.021(4) C16 0.054(5) 0.056(5) 0.057(5) -0.019(4) -0.009(4) -0.016(4) C17 0.071(5) 0.069(5) 0.038(4) -0.010(4) -0.014(4) -0.016(5) C18 0.059(5) 0.047(4) 0.050(4) -0.016(4) -0.016(4) -0.011(4) C19 0.043(4) 0.043(4) 0.031(3) -0.008(3) -0.006(3) -0.013(3) C20 0.051(4) 0.034(4) 0.053(4) -0.001(3) -0.015(4) -0.009(3) C21 0.045(4) 0.050(5) 0.077(6) -0.004(4) -0.018(4) -0.006(4) C22 0.048(5) 0.065(6) 0.086(6) -0.028(5) -0.008(4) -0.014(4) C23 0.057(5) 0.076(6) 0.052(5) -0.022(4) 0.009(4) -0.026(4) C24 0.053(5) 0.067(5) 0.043(4) -0.013(4) -0.008(4) -0.015(4) C25 0.043(4) 0.034(3) 0.034(3) -0.010(3) -0.005(3) -0.012(3) C26 0.050(4) 0.039(4) 0.049(4) 0.007(3) -0.018(3) -0.017(3) C27 0.064(5) 0.037(4) 0.061(5) 0.004(4) -0.010(4) -0.025(4) C28 0.069(5) 0.043(4) 0.082(6) -0.010(4) -0.015(4) -0.029(4) C29 0.067(5) 0.070(5) 0.064(5) -0.026(4) -0.009(4) -0.032(4) C30 0.067(5) 0.055(4) 0.039(4) -0.012(4) -0.006(4) -0.031(4) C31 0.043(4) 0.034(3) 0.036(3) 0.000(3) -0.011(3) -0.011(3) C32 0.056(5) 0.036(4) 0.048(4) 0.006(3) -0.013(3) -0.016(3) C33 0.071(5) 0.045(4) 0.051(5) 0.009(4) -0.023(4) -0.009(4) C34 0.094(7) 0.034(4) 0.055(5) 0.011(4) -0.023(5) -0.018(4) C35 0.095(7) 0.047(5) 0.067(5) 0.017(4) -0.016(5) -0.041(5) C36 0.059(5) 0.051(4) 0.053(4) 0.006(4) -0.014(4) -0.031(4) C37 0.100(8) 0.089(7) 0.082(7) 0.010(5) -0.030(6) -0.056(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 C6 2.004(7) . ? Pd1 N1 2.162(5) . ? Pd1 P1 2.2797(17) . ? Pd1 Cl1 2.4037(18) . ? Fe1 C10 2.028(7) . ? Fe1 C9 2.050(7) . ? Fe1 C5 2.052(7) . ? Fe1 C3 2.056(8) . ? Fe1 C7 2.057(6) . ? Fe1 C8 2.059(7) . ? Fe1 C1 2.061(7) . ? Fe1 C2 2.071(7) . ? Fe1 C4 2.075(7) . ? Fe1 C6 2.075(7) . ? N1 C11 1.297(8) . ? N1 C13 1.441(8) . ? P1 C25 1.846(6) . ? P1 C31 1.852(6) . ? P1 C19 1.857(6) . ? Cl2 C14 1.751(7) . ? Cl3 C37 1.749(10) . ? Cl4 C37 1.731(10) . ? C1 C2 1.417(11) . ? C1 C5 1.423(11) . ? C1 H1A 0.9800 . ? C2 C3 1.435(10) . ? C2 H2A 0.9800 . ? C3 C4 1.406(11) . ? C3 H3A 0.9800 . ? C4 C5 1.435(11) . ? C4 H4A 0.9800 . ? C5 H5A 0.9800 . ? C6 C10 1.435(9) . ? C6 C7 1.443(9) . ? C7 C8 1.444(9) . ? C7 H7A 0.9800 . ? C8 C9 1.418(10) . ? C8 H8A 0.9800 . ? C9 C10 1.439(10) . ? C9 H9A 0.9800 . ? C10 C11 1.445(10) . ? C11 C12 1.496(9) . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 C14 1.386(9) . ? C13 C18 1.420(10) . ? C14 C15 1.377(10) . ? C15 C16 1.364(10) . ? C15 H15A 0.9300 . ? C16 C17 1.379(11) . ? C16 H16A 0.9300 . ? C17 C18 1.389(10) . ? C17 H17A 0.9300 . ? C18 H18A 0.9300 . ? C19 C20 1.534(9) . ? C19 C24 1.553(9) . ? C19 H19A 0.9800 . ? C20 C21 1.520(10) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 C22 1.505(11) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 C23 1.515(11) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 C24 1.526(10) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 C30 1.524(8) . ? C25 C26 1.552(9) . ? C25 H25A 0.9800 . ? C26 C27 1.521(9) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C27 C28 1.496(10) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 C29 1.540(11) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C29 C30 1.521(10) . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C31 C32 1.525(9) . ? C31 C36 1.552(9) . ? C31 H31A 0.9800 . ? C32 C33 1.540(9) . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C33 C34 1.515(11) . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C34 C35 1.510(12) . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C35 C36 1.531(10) . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C36 H36A 0.9700 . ? C36 H36B 0.9700 . ? C37 H37A 0.9700 . ? C37 H37B 0.9700 . ? 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 C6 Pd1 N1 79.7(2) . . ? C6 Pd1 P1 96.34(19) . . ? N1 Pd1 P1 174.37(15) . . ? C6 Pd1 Cl1 168.80(19) . . ? N1 Pd1 Cl1 89.45(16) . . ? P1 Pd1 Cl1 94.26(7) . . ? C10 Fe1 C9 41.3(3) . . ? C10 Fe1 C5 106.4(3) . . ? C9 Fe1 C5 122.3(3) . . ? C10 Fe1 C3 159.6(3) . . ? C9 Fe1 C3 123.9(3) . . ? C5 Fe1 C3 67.8(3) . . ? C10 Fe1 C7 67.9(3) . . ? C9 Fe1 C7 68.6(3) . . ? C5 Fe1 C7 157.8(3) . . ? C3 Fe1 C7 124.8(3) . . ? C10 Fe1 C8 68.4(3) . . ? C9 Fe1 C8 40.4(3) . . ? C5 Fe1 C8 159.0(3) . . ? C3 Fe1 C8 109.6(3) . . ? C7 Fe1 C8 41.1(3) . . ? C10 Fe1 C1 121.4(3) . . ? C9 Fe1 C1 158.1(3) . . ? C5 Fe1 C1 40.5(3) . . ? C3 Fe1 C1 67.7(3) . . ? C7 Fe1 C1 122.6(3) . . ? C8 Fe1 C1 159.7(3) . . ? C10 Fe1 C2 157.3(3) . . ? C9 Fe1 C2 160.3(3) . . ? C5 Fe1 C2 68.0(3) . . ? C3 Fe1 C2 40.7(3) . . ? C7 Fe1 C2 108.5(3) . . ? C8 Fe1 C2 124.7(3) . . ? C1 Fe1 C2 40.1(3) . . ? C10 Fe1 C4 123.2(3) . . ? C9 Fe1 C4 108.0(3) . . ? C5 Fe1 C4 40.7(3) . . ? C3 Fe1 C4 39.8(3) . . ? C7 Fe1 C4 160.3(3) . . ? C8 Fe1 C4 123.8(3) . . ? C1 Fe1 C4 67.9(3) . . ? C2 Fe1 C4 67.8(3) . . ? C10 Fe1 C6 40.9(3) . . ? C9 Fe1 C6 69.9(3) . . ? C5 Fe1 C6 120.7(3) . . ? C3 Fe1 C6 159.1(3) . . ? C7 Fe1 C6 40.9(3) . . ? C8 Fe1 C6 69.5(3) . . ? C1 Fe1 C6 105.5(3) . . ? C2 Fe1 C6 121.5(3) . . ? C4 Fe1 C6 158.0(3) . . ? C11 N1 C13 121.0(6) . . ? C11 N1 Pd1 114.4(4) . . ? C13 N1 Pd1 124.5(4) . . ? C25 P1 C31 105.5(3) . . ? C25 P1 C19 110.3(3) . . ? C31 P1 C19 103.6(3) . . ? C25 P1 Pd1 114.7(2) . . ? C31 P1 Pd1 110.8(2) . . ? C19 P1 Pd1 111.3(2) . . ? C2 C1 C5 108.5(7) . . ? C2 C1 Fe1 70.3(4) . . ? C5 C1 Fe1 69.4(4) . . ? C2 C1 H1A 125.8 . . ? C5 C1 H1A 125.8 . . ? Fe1 C1 H1A 125.8 . . ? C1 C2 C3 107.2(7) . . ? C1 C2 Fe1 69.6(4) . . ? C3 C2 Fe1 69.1(4) . . ? C1 C2 H2A 126.4 . . ? C3 C2 H2A 126.4 . . ? Fe1 C2 H2A 126.4 . . ? C4 C3 C2 109.0(7) . . ? C4 C3 Fe1 70.8(4) . . ? C2 C3 Fe1 70.2(4) . . ? C4 C3 H3A 125.5 . . ? C2 C3 H3A 125.5 . . ? Fe1 C3 H3A 125.5 . . ? C3 C4 C5 107.5(7) . . ? C3 C4 Fe1 69.4(4) . . ? C5 C4 Fe1 68.8(4) . . ? C3 C4 H4A 126.2 . . ? C5 C4 H4A 126.2 . . ? Fe1 C4 H4A 126.2 . . ? C1 C5 C4 107.9(8) . . ? C1 C5 Fe1 70.1(4) . . ? C4 C5 Fe1 70.5(4) . . ? C1 C5 H5A 126.1 . . ? C4 C5 H5A 126.1 . . ? Fe1 C5 H5A 126.1 . . ? C10 C6 C7 105.0(6) . . ? C10 C6 Pd1 110.8(5) . . ? C7 C6 Pd1 144.1(5) . . ? C10 C6 Fe1 67.8(4) . . ? C7 C6 Fe1 68.9(4) . . ? Pd1 C6 Fe1 127.7(3) . . ? C6 C7 C8 109.5(6) . . ? C6 C7 Fe1 70.2(4) . . ? C8 C7 Fe1 69.5(4) . . ? C6 C7 H7A 125.2 . . ? C8 C7 H7A 125.2 . . ? Fe1 C7 H7A 125.2 . . ? C9 C8 C7 107.9(6) . . ? C9 C8 Fe1 69.4(4) . . ? C7 C8 Fe1 69.4(4) . . ? C9 C8 H8A 126.1 . . ? C7 C8 H8A 126.1 . . ? Fe1 C8 H8A 126.1 . . ? C8 C9 C10 107.0(6) . . ? C8 C9 Fe1 70.2(4) . . ? C10 C9 Fe1 68.5(4) . . ? C8 C9 H9A 126.5 . . ? C10 C9 H9A 126.5 . . ? Fe1 C9 H9A 126.5 . . ? C6 C10 C9 110.6(6) . . ? C6 C10 C11 119.4(6) . . ? C9 C10 C11 128.9(7) . . ? C6 C10 Fe1 71.3(4) . . ? C9 C10 Fe1 70.2(4) . . ? C11 C10 Fe1 115.5(5) . . ? N1 C11 C10 113.6(6) . . ? N1 C11 C12 126.0(7) . . ? C10 C11 C12 120.4(6) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C14 C13 C18 117.4(7) . . ? C14 C13 N1 122.8(6) . . ? C18 C13 N1 119.8(6) . . ? C15 C14 C13 122.8(7) . . ? C15 C14 Cl2 117.5(6) . . ? C13 C14 Cl2 119.7(6) . . ? C16 C15 C14 119.0(7) . . ? C16 C15 H15A 120.5 . . ? C14 C15 H15A 120.5 . . ? C15 C16 C17 120.7(7) . . ? C15 C16 H16A 119.6 . . ? C17 C16 H16A 119.6 . . ? C16 C17 C18 120.8(8) . . ? C16 C17 H17A 119.6 . . ? C18 C17 H17A 119.6 . . ? C17 C18 C13 119.3(7) . . ? C17 C18 H18A 120.4 . . ? C13 C18 H18A 120.4 . . ? C20 C19 C24 110.2(5) . . ? C20 C19 P1 113.5(4) . . ? C24 C19 P1 117.8(5) . . ? C20 C19 H19A 104.6 . . ? C24 C19 H19A 104.6 . . ? P1 C19 H19A 104.6 . . ? C21 C20 C19 110.0(6) . . ? C21 C20 H20A 109.7 . . ? C19 C20 H20A 109.7 . . ? C21 C20 H20B 109.7 . . ? C19 C20 H20B 109.7 . . ? H20A C20 H20B 108.2 . . ? C22 C21 C20 112.5(7) . . ? C22 C21 H21A 109.1 . . ? C20 C21 H21A 109.1 . . ? C22 C21 H21B 109.1 . . ? C20 C21 H21B 109.1 . . ? H21A C21 H21B 107.8 . . ? C21 C22 C23 111.3(6) . . ? C21 C22 H22A 109.4 . . ? C23 C22 H22A 109.4 . . ? C21 C22 H22B 109.4 . . ? C23 C22 H22B 109.4 . . ? H22A C22 H22B 108.0 . . ? C22 C23 C24 112.1(7) . . ? C22 C23 H23A 109.2 . . ? C24 C23 H23A 109.2 . . ? C22 C23 H23B 109.2 . . ? C24 C23 H23B 109.2 . . ? H23A C23 H23B 107.9 . . ? C23 C24 C19 110.5(6) . . ? C23 C24 H24A 109.5 . . ? C19 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? C19 C24 H24B 109.5 . . ? H24A C24 H24B 108.1 . . ? C30 C25 C26 109.1(5) . . ? C30 C25 P1 117.1(5) . . ? C26 C25 P1 114.7(4) . . ? C30 C25 H25A 104.8 . . ? C26 C25 H25A 104.8 . . ? P1 C25 H25A 104.8 . . ? C27 C26 C25 110.5(6) . . ? C27 C26 H26A 109.5 . . ? C25 C26 H26A 109.5 . . ? C27 C26 H26B 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 108.1 . . ? C28 C27 C26 112.9(6) . . ? C28 C27 H27A 109.0 . . ? C26 C27 H27A 109.0 . . ? C28 C27 H27B 109.0 . . ? C26 C27 H27B 109.0 . . ? H27A C27 H27B 107.8 . . ? C27 C28 C29 111.4(6) . . ? C27 C28 H28A 109.3 . . ? C29 C28 H28A 109.3 . . ? C27 C28 H28B 109.3 . . ? C29 C28 H28B 109.3 . . ? H28A C28 H28B 108.0 . . ? C30 C29 C28 111.0(6) . . ? C30 C29 H29A 109.4 . . ? C28 C29 H29A 109.4 . . ? C30 C29 H29B 109.4 . . ? C28 C29 H29B 109.4 . . ? H29A C29 H29B 108.0 . . ? C29 C30 C25 111.5(6) . . ? C29 C30 H30A 109.3 . . ? C25 C30 H30A 109.3 . . ? C29 C30 H30B 109.3 . . ? C25 C30 H30B 109.3 . . ? H30A C30 H30B 108.0 . . ? C32 C31 C36 110.1(6) . . ? C32 C31 P1 113.5(4) . . ? C36 C31 P1 109.3(4) . . ? C32 C31 H31A 107.9 . . ? C36 C31 H31A 107.9 . . ? P1 C31 H31A 107.9 . . ? C31 C32 C33 111.8(6) . . ? C31 C32 H32A 109.3 . . ? C33 C32 H32A 109.3 . . ? C31 C32 H32B 109.3 . . ? C33 C32 H32B 109.3 . . ? H32A C32 H32B 107.9 . . ? C34 C33 C32 112.3(6) . . ? C34 C33 H33A 109.2 . . ? C32 C33 H33A 109.2 . . ? C34 C33 H33B 109.2 . . ? C32 C33 H33B 109.2 . . ? H33A C33 H33B 107.9 . . ? C35 C34 C33 110.6(6) . . ? C35 C34 H34A 109.5 . . ? C33 C34 H34A 109.5 . . ? C35 C34 H34B 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 108.1 . . ? C34 C35 C36 111.7(6) . . ? C34 C35 H35A 109.3 . . ? C36 C35 H35A 109.3 . . ? C34 C35 H35B 109.3 . . ? C36 C35 H35B 109.3 . . ? H35A C35 H35B 107.9 . . ? C35 C36 C31 112.1(6) . . ? C35 C36 H36A 109.2 . . ? C31 C36 H36A 109.2 . . ? C35 C36 H36B 109.2 . . ? C31 C36 H36B 109.2 . . ? H36A C36 H36B 107.9 . . ? Cl4 C37 Cl3 112.1(5) . . ? Cl4 C37 H37A 109.2 . . ? Cl3 C37 H37A 109.2 . . ? Cl4 C37 H37B 109.2 . . ? Cl3 C37 H37B 109.2 . . ? H37A C37 H37B 107.9 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 Pd1 N1 C11 -10.4(5) . . . . ? P1 Pd1 N1 C11 35.4(19) . . . . ? Cl1 Pd1 N1 C11 166.7(4) . . . . ? C6 Pd1 N1 C13 171.6(5) . . . . ? P1 Pd1 N1 C13 -142.5(14) . . . . ? Cl1 Pd1 N1 C13 -11.3(5) . . . . ? C6 Pd1 P1 C25 34.6(3) . . . . ? N1 Pd1 P1 C25 -10.6(17) . . . . ? Cl1 Pd1 P1 C25 -141.7(2) . . . . ? C6 Pd1 P1 C31 -84.7(3) . . . . ? N1 Pd1 P1 C31 -130.0(16) . . . . ? Cl1 Pd1 P1 C31 99.0(2) . . . . ? C6 Pd1 P1 C19 160.7(3) . . . . ? N1 Pd1 P1 C19 115.4(16) . . . . ? Cl1 Pd1 P1 C19 -15.7(2) . . . . ? C10 Fe1 C1 C2 -162.3(4) . . . . ? C9 Fe1 C1 C2 164.7(7) . . . . ? C5 Fe1 C1 C2 119.6(7) . . . . ? C3 Fe1 C1 C2 38.2(4) . . . . ? C7 Fe1 C1 C2 -79.9(5) . . . . ? C8 Fe1 C1 C2 -48.2(10) . . . . ? C4 Fe1 C1 C2 81.3(5) . . . . ? C6 Fe1 C1 C2 -120.9(4) . . . . ? C10 Fe1 C1 C5 78.1(5) . . . . ? C9 Fe1 C1 C5 45.1(10) . . . . ? C3 Fe1 C1 C5 -81.4(5) . . . . ? C7 Fe1 C1 C5 160.5(5) . . . . ? C8 Fe1 C1 C5 -167.8(8) . . . . ? C2 Fe1 C1 C5 -119.6(7) . . . . ? C4 Fe1 C1 C5 -38.3(5) . . . . ? C6 Fe1 C1 C5 119.5(5) . . . . ? C5 C1 C2 C3 0.0(8) . . . . ? Fe1 C1 C2 C3 -59.1(5) . . . . ? C5 C1 C2 Fe1 59.1(5) . . . . ? C10 Fe1 C2 C1 42.2(9) . . . . ? C9 Fe1 C2 C1 -163.0(8) . . . . ? C5 Fe1 C2 C1 -37.5(4) . . . . ? C3 Fe1 C2 C1 -118.6(7) . . . . ? C7 Fe1 C2 C1 119.1(5) . . . . ? C8 Fe1 C2 C1 161.7(4) . . . . ? C4 Fe1 C2 C1 -81.6(5) . . . . ? C6 Fe1 C2 C1 76.0(5) . . . . ? C10 Fe1 C2 C3 160.8(7) . . . . ? C9 Fe1 C2 C3 -44.4(11) . . . . ? C5 Fe1 C2 C3 81.1(5) . . . . ? C7 Fe1 C2 C3 -122.3(5) . . . . ? C8 Fe1 C2 C3 -79.7(5) . . . . ? C1 Fe1 C2 C3 118.6(7) . . . . ? C4 Fe1 C2 C3 37.0(5) . . . . ? C6 Fe1 C2 C3 -165.4(4) . . . . ? C1 C2 C3 C4 -1.0(8) . . . . ? Fe1 C2 C3 C4 -60.4(5) . . . . ? C1 C2 C3 Fe1 59.4(5) . . . . ? C10 Fe1 C3 C4 -39.3(11) . . . . ? C9 Fe1 C3 C4 -77.1(6) . . . . ? C5 Fe1 C3 C4 37.9(5) . . . . ? C7 Fe1 C3 C4 -163.1(5) . . . . ? C8 Fe1 C3 C4 -119.8(5) . . . . ? C1 Fe1 C3 C4 81.8(5) . . . . ? C2 Fe1 C3 C4 119.4(7) . . . . ? C6 Fe1 C3 C4 156.5(7) . . . . ? C10 Fe1 C3 C2 -158.7(8) . . . . ? C9 Fe1 C3 C2 163.5(5) . . . . ? C5 Fe1 C3 C2 -81.5(5) . . . . ? C7 Fe1 C3 C2 77.5(5) . . . . ? C8 Fe1 C3 C2 120.8(5) . . . . ? C1 Fe1 C3 C2 -37.7(5) . . . . ? C4 Fe1 C3 C2 -119.4(7) . . . . ? C6 Fe1 C3 C2 37.1(10) . . . . ? C2 C3 C4 C5 1.6(8) . . . . ? Fe1 C3 C4 C5 -58.4(5) . . . . ? C2 C3 C4 Fe1 60.1(5) . . . . ? C10 Fe1 C4 C3 164.7(5) . . . . ? C9 Fe1 C4 C3 121.7(5) . . . . ? C5 Fe1 C4 C3 -119.4(7) . . . . ? C7 Fe1 C4 C3 45.0(11) . . . . ? C8 Fe1 C4 C3 80.0(6) . . . . ? C1 Fe1 C4 C3 -81.3(5) . . . . ? C2 Fe1 C4 C3 -37.8(5) . . . . ? C6 Fe1 C4 C3 -157.6(7) . . . . ? C10 Fe1 C4 C5 -75.9(6) . . . . ? C9 Fe1 C4 C5 -118.9(5) . . . . ? C3 Fe1 C4 C5 119.4(7) . . . . ? C7 Fe1 C4 C5 164.4(8) . . . . ? C8 Fe1 C4 C5 -160.7(5) . . . . ? C1 Fe1 C4 C5 38.1(5) . . . . ? C2 Fe1 C4 C5 81.5(5) . . . . ? C6 Fe1 C4 C5 -38.2(10) . . . . ? C2 C1 C5 C4 1.0(8) . . . . ? Fe1 C1 C5 C4 60.7(5) . . . . ? C2 C1 C5 Fe1 -59.7(5) . . . . ? C3 C4 C5 C1 -1.6(8) . . . . ? Fe1 C4 C5 C1 -60.4(5) . . . . ? C3 C4 C5 Fe1 58.8(5) . . . . ? C10 Fe1 C5 C1 -119.5(5) . . . . ? C9 Fe1 C5 C1 -161.7(5) . . . . ? C3 Fe1 C5 C1 81.3(5) . . . . ? C7 Fe1 C5 C1 -47.8(10) . . . . ? C8 Fe1 C5 C1 168.2(8) . . . . ? C2 Fe1 C5 C1 37.2(5) . . . . ? C4 Fe1 C5 C1 118.3(7) . . . . ? C6 Fe1 C5 C1 -77.3(5) . . . . ? C10 Fe1 C5 C4 122.2(5) . . . . ? C9 Fe1 C5 C4 80.0(6) . . . . ? C3 Fe1 C5 C4 -37.0(5) . . . . ? C7 Fe1 C5 C4 -166.1(7) . . . . ? C8 Fe1 C5 C4 49.9(11) . . . . ? C1 Fe1 C5 C4 -118.3(7) . . . . ? C2 Fe1 C5 C4 -81.1(5) . . . . ? C6 Fe1 C5 C4 164.4(5) . . . . ? N1 Pd1 C6 C10 12.2(4) . . . . ? P1 Pd1 C6 C10 -163.8(4) . . . . ? Cl1 Pd1 C6 C10 -2.8(13) . . . . ? N1 Pd1 C6 C7 -172.2(8) . . . . ? P1 Pd1 C6 C7 11.8(8) . . . . ? Cl1 Pd1 C6 C7 172.8(5) . . . . ? N1 Pd1 C6 Fe1 -65.3(4) . . . . ? P1 Pd1 C6 Fe1 118.8(4) . . . . ? Cl1 Pd1 C6 Fe1 -80.3(11) . . . . ? C9 Fe1 C6 C10 37.0(4) . . . . ? C5 Fe1 C6 C10 -79.4(5) . . . . ? C3 Fe1 C6 C10 171.7(8) . . . . ? C7 Fe1 C6 C10 117.2(5) . . . . ? C8 Fe1 C6 C10 80.2(4) . . . . ? C1 Fe1 C6 C10 -120.4(4) . . . . ? C2 Fe1 C6 C10 -160.9(4) . . . . ? C4 Fe1 C6 C10 -51.3(9) . . . . ? C10 Fe1 C6 C7 -117.2(5) . . . . ? C9 Fe1 C6 C7 -80.2(4) . . . . ? C5 Fe1 C6 C7 163.4(4) . . . . ? C3 Fe1 C6 C7 54.5(9) . . . . ? C8 Fe1 C6 C7 -37.0(4) . . . . ? C1 Fe1 C6 C7 122.4(4) . . . . ? C2 Fe1 C6 C7 81.9(5) . . . . ? C4 Fe1 C6 C7 -168.5(7) . . . . ? C10 Fe1 C6 Pd1 99.8(5) . . . . ? C9 Fe1 C6 Pd1 136.8(5) . . . . ? C5 Fe1 C6 Pd1 20.4(5) . . . . ? C3 Fe1 C6 Pd1 -88.5(9) . . . . ? C7 Fe1 C6 Pd1 -143.0(6) . . . . ? C8 Fe1 C6 Pd1 180.0(5) . . . . ? C1 Fe1 C6 Pd1 -20.6(5) . . . . ? C2 Fe1 C6 Pd1 -61.1(5) . . . . ? C4 Fe1 C6 Pd1 48.4(10) . . . . ? C10 C6 C7 C8 0.1(7) . . . . ? Pd1 C6 C7 C8 -175.7(6) . . . . ? Fe1 C6 C7 C8 58.5(5) . . . . ? C10 C6 C7 Fe1 -58.5(4) . . . . ? Pd1 C6 C7 Fe1 125.8(8) . . . . ? C10 Fe1 C7 C6 38.9(4) . . . . ? C9 Fe1 C7 C6 83.6(4) . . . . ? C5 Fe1 C7 C6 -40.3(10) . . . . ? C3 Fe1 C7 C6 -159.3(4) . . . . ? C8 Fe1 C7 C6 120.9(6) . . . . ? C1 Fe1 C7 C6 -75.2(5) . . . . ? C2 Fe1 C7 C6 -117.1(4) . . . . ? C4 Fe1 C7 C6 167.3(8) . . . . ? C10 Fe1 C7 C8 -82.0(5) . . . . ? C9 Fe1 C7 C8 -37.3(4) . . . . ? C5 Fe1 C7 C8 -161.2(8) . . . . ? C3 Fe1 C7 C8 79.8(5) . . . . ? C1 Fe1 C7 C8 163.9(4) . . . . ? C2 Fe1 C7 C8 122.0(5) . . . . ? C4 Fe1 C7 C8 46.4(11) . . . . ? C6 Fe1 C7 C8 -120.9(6) . . . . ? C6 C7 C8 C9 0.0(8) . . . . ? Fe1 C7 C8 C9 59.0(5) . . . . ? C6 C7 C8 Fe1 -59.0(5) . . . . ? C10 Fe1 C8 C9 -38.6(4) . . . . ? C5 Fe1 C8 C9 40.7(11) . . . . ? C3 Fe1 C8 C9 119.7(5) . . . . ? C7 Fe1 C8 C9 -119.4(6) . . . . ? C1 Fe1 C8 C9 -161.7(8) . . . . ? C2 Fe1 C8 C9 162.6(4) . . . . ? C4 Fe1 C8 C9 77.7(5) . . . . ? C6 Fe1 C8 C9 -82.6(4) . . . . ? C10 Fe1 C8 C7 80.8(4) . . . . ? C9 Fe1 C8 C7 119.4(6) . . . . ? C5 Fe1 C8 C7 160.2(8) . . . . ? C3 Fe1 C8 C7 -120.9(5) . . . . ? C1 Fe1 C8 C7 -42.3(10) . . . . ? C2 Fe1 C8 C7 -78.0(5) . . . . ? C4 Fe1 C8 C7 -162.9(4) . . . . ? C6 Fe1 C8 C7 36.8(4) . . . . ? C7 C8 C9 C10 -0.1(8) . . . . ? Fe1 C8 C9 C10 58.8(5) . . . . ? C7 C8 C9 Fe1 -58.9(5) . . . . ? C10 Fe1 C9 C8 118.4(6) . . . . ? C5 Fe1 C9 C8 -163.9(4) . . . . ? C3 Fe1 C9 C8 -80.4(5) . . . . ? C7 Fe1 C9 C8 37.9(4) . . . . ? C1 Fe1 C9 C8 163.1(7) . . . . ? C2 Fe1 C9 C8 -47.1(10) . . . . ? C4 Fe1 C9 C8 -121.4(5) . . . . ? C6 Fe1 C9 C8 81.8(4) . . . . ? C5 Fe1 C9 C10 77.7(5) . . . . ? C3 Fe1 C9 C10 161.1(4) . . . . ? C7 Fe1 C9 C10 -80.5(4) . . . . ? C8 Fe1 C9 C10 -118.4(6) . . . . ? C1 Fe1 C9 C10 44.7(10) . . . . ? C2 Fe1 C9 C10 -165.6(8) . . . . ? C4 Fe1 C9 C10 120.1(5) . . . . ? C6 Fe1 C9 C10 -36.7(4) . . . . ? C7 C6 C10 C9 -0.2(7) . . . . ? Pd1 C6 C10 C9 177.2(5) . . . . ? Fe1 C6 C10 C9 -59.4(5) . . . . ? C7 C6 C10 C11 168.6(6) . . . . ? Pd1 C6 C10 C11 -14.1(7) . . . . ? Fe1 C6 C10 C11 109.4(6) . . . . ? C7 C6 C10 Fe1 59.2(4) . . . . ? Pd1 C6 C10 Fe1 -123.4(4) . . . . ? C8 C9 C10 C6 0.2(8) . . . . ? Fe1 C9 C10 C6 60.0(5) . . . . ? C8 C9 C10 C11 -167.2(6) . . . . ? Fe1 C9 C10 C11 -107.3(7) . . . . ? C8 C9 C10 Fe1 -59.9(5) . . . . ? C9 Fe1 C10 C6 -121.1(6) . . . . ? C5 Fe1 C10 C6 118.3(4) . . . . ? C3 Fe1 C10 C6 -171.5(8) . . . . ? C7 Fe1 C10 C6 -38.9(4) . . . . ? C8 Fe1 C10 C6 -83.3(4) . . . . ? C1 Fe1 C10 C6 76.8(5) . . . . ? C2 Fe1 C10 C6 46.4(9) . . . . ? C4 Fe1 C10 C6 159.6(4) . . . . ? C5 Fe1 C10 C9 -120.6(5) . . . . ? C3 Fe1 C10 C9 -50.4(10) . . . . ? C7 Fe1 C10 C9 82.2(4) . . . . ? C8 Fe1 C10 C9 37.8(4) . . . . ? C1 Fe1 C10 C9 -162.1(4) . . . . ? C2 Fe1 C10 C9 167.5(7) . . . . ? C4 Fe1 C10 C9 -79.4(5) . . . . ? C6 Fe1 C10 C9 121.1(6) . . . . ? C9 Fe1 C10 C11 124.6(7) . . . . ? C5 Fe1 C10 C11 4.0(6) . . . . ? C3 Fe1 C10 C11 74.2(11) . . . . ? C7 Fe1 C10 C11 -153.2(6) . . . . ? C8 Fe1 C10 C11 162.4(6) . . . . ? C1 Fe1 C10 C11 -37.5(6) . . . . ? C2 Fe1 C10 C11 -68.0(10) . . . . ? C4 Fe1 C10 C11 45.2(6) . . . . ? C6 Fe1 C10 C11 -114.4(7) . . . . ? C13 N1 C11 C10 -176.4(5) . . . . ? Pd1 N1 C11 C10 5.5(7) . . . . ? C13 N1 C11 C12 1.9(10) . . . . ? Pd1 N1 C11 C12 -176.2(5) . . . . ? C6 C10 C11 N1 5.5(9) . . . . ? C9 C10 C11 N1 171.9(6) . . . . ? Fe1 C10 C11 N1 87.5(6) . . . . ? C6 C10 C11 C12 -172.9(6) . . . . ? C9 C10 C11 C12 -6.5(11) . . . . ? Fe1 C10 C11 C12 -90.9(7) . . . . ? C11 N1 C13 C14 118.3(7) . . . . ? Pd1 N1 C13 C14 -63.9(8) . . . . ? C11 N1 C13 C18 -63.4(9) . . . . ? Pd1 N1 C13 C18 114.4(6) . . . . ? C18 C13 C14 C15 -0.3(10) . . . . ? N1 C13 C14 C15 178.1(7) . . . . ? C18 C13 C14 Cl2 178.9(5) . . . . ? N1 C13 C14 Cl2 -2.7(9) . . . . ? C13 C14 C15 C16 -0.4(11) . . . . ? Cl2 C14 C15 C16 -179.6(6) . . . . ? C14 C15 C16 C17 0.8(11) . . . . ? C15 C16 C17 C18 -0.7(11) . . . . ? C16 C17 C18 C13 0.0(11) . . . . ? C14 C13 C18 C17 0.4(10) . . . . ? N1 C13 C18 C17 -178.0(6) . . . . ? C25 P1 C19 C20 60.6(5) . . . . ? C31 P1 C19 C20 173.1(5) . . . . ? Pd1 P1 C19 C20 -67.8(5) . . . . ? C25 P1 C19 C24 -70.3(6) . . . . ? C31 P1 C19 C24 42.2(6) . . . . ? Pd1 P1 C19 C24 161.3(5) . . . . ? C24 C19 C20 C21 -56.8(8) . . . . ? P1 C19 C20 C21 168.6(5) . . . . ? C19 C20 C21 C22 57.2(8) . . . . ? C20 C21 C22 C23 -55.5(9) . . . . ? C21 C22 C23 C24 54.2(9) . . . . ? C22 C23 C24 C19 -54.7(9) . . . . ? C20 C19 C24 C23 56.0(8) . . . . ? P1 C19 C24 C23 -171.6(5) . . . . ? C31 P1 C25 C30 -64.5(6) . . . . ? C19 P1 C25 C30 46.7(6) . . . . ? Pd1 P1 C25 C30 173.2(5) . . . . ? C31 P1 C25 C26 165.6(5) . . . . ? C19 P1 C25 C26 -83.2(5) . . . . ? Pd1 P1 C25 C26 43.4(5) . . . . ? C30 C25 C26 C27 56.8(8) . . . . ? P1 C25 C26 C27 -169.5(5) . . . . ? C25 C26 C27 C28 -55.8(8) . . . . ? C26 C27 C28 C29 53.8(9) . . . . ? C27 C28 C29 C30 -53.5(9) . . . . ? C28 C29 C30 C25 56.7(9) . . . . ? C26 C25 C30 C29 -58.1(8) . . . . ? P1 C25 C30 C29 169.4(5) . . . . ? C25 P1 C31 C32 -54.1(5) . . . . ? C19 P1 C31 C32 -170.1(5) . . . . ? Pd1 P1 C31 C32 70.6(5) . . . . ? C25 P1 C31 C36 -177.5(5) . . . . ? C19 P1 C31 C36 66.6(5) . . . . ? Pd1 P1 C31 C36 -52.8(5) . . . . ? C36 C31 C32 C33 -53.1(8) . . . . ? P1 C31 C32 C33 -176.0(5) . . . . ? C31 C32 C33 C34 55.4(8) . . . . ? C32 C33 C34 C35 -55.8(9) . . . . ? C33 C34 C35 C36 55.9(9) . . . . ? C34 C35 C36 C31 -55.5(9) . . . . ? C32 C31 C36 C35 53.6(8) . . . . ? P1 C31 C36 C35 179.0(5) . . . . ? _diffrn_measured_fraction_theta_max 0.873 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.873 _refine_diff_density_max 0.884 _refine_diff_density_min -1.098 _refine_diff_density_rms 0.102 # Attachment 'Complex 2f.cif' data_p-1_2f _database_code_depnum_ccdc_archive 'CCDC 602222' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C37 H50 Cl4 Fe N P Pd' _chemical_formula_weight 843.80 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.115(2) _cell_length_b 11.148(2) _cell_length_c 17.938(4) _cell_angle_alpha 102.77(3) _cell_angle_beta 92.87(3) _cell_angle_gamma 105.73(3) _cell_volume 1885.9(6) _cell_formula_units_Z 2 _cell_measurement_temperature 291(2) _cell_measurement_reflns_used 375 _cell_measurement_theta_min 2 _cell_measurement_theta_max 25.1 _exptl_crystal_description Prismatic _exptl_crystal_colour Red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.486 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 868 _exptl_absorpt_coefficient_mu 1.214 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7933 _exptl_absorpt_correction_T_max 0.8202 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 291(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type R-AXIS-IV _diffrn_measurement_method 'Oscillation frames' _diffrn_detector_area_resol_mean 0 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% ? _diffrn_reflns_number 5774 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0663 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.17 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5774 _reflns_number_gt 4545 _reflns_threshold_expression >2sigma(I) _computing_data_collection raxis _computing_cell_refinement raxis _computing_data_reduction raxis _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics texsan _computing_publication_material texsan _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0341P)^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 fixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0008(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 5774 _refine_ls_number_parameters 407 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0625 _refine_ls_R_factor_gt 0.0405 _refine_ls_wR_factor_ref 0.0758 _refine_ls_wR_factor_gt 0.0708 _refine_ls_goodness_of_fit_ref 1.020 _refine_ls_restrained_S_all 1.020 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.75548(3) 0.98737(3) 0.692371(18) 0.02524(11) Uani 1 1 d . . . Fe1 Fe 0.41250(6) 0.76536(6) 0.63829(4) 0.03453(17) Uani 1 1 d . . . P1 P 0.76409(10) 1.11877(10) 0.81082(6) 0.0264(3) Uani 1 1 d . . . N1 N 0.7350(3) 0.8804(3) 0.57338(18) 0.0331(9) Uani 1 1 d . . . Cl1 Cl 0.99807(9) 1.00707(11) 0.70613(6) 0.0388(3) Uani 1 1 d . . . Cl2 Cl 1.12166(12) 0.63076(13) 0.40684(7) 0.0547(3) Uani 1 1 d . . . Cl3 Cl 0.8338(2) 0.1845(2) 0.12573(12) 0.1359(8) Uani 1 1 d . . . Cl4 Cl 1.0744(2) 0.35195(19) 0.22614(14) 0.1326(8) Uani 1 1 d . . . C1 C 0.3796(5) 0.6482(4) 0.7138(3) 0.0500(13) Uani 1 1 d . . . H1A H 0.3654 0.6735 0.7680 0.060 Uiso 1 1 calc R . . C2 C 0.2743(5) 0.5973(4) 0.6498(3) 0.0576(14) Uani 1 1 d . . . H2A H 0.1747 0.5818 0.6520 0.069 Uiso 1 1 calc R . . C3 C 0.3397(5) 0.5727(4) 0.5832(3) 0.0566(14) Uani 1 1 d . . . H3A H 0.2929 0.5376 0.5305 0.068 Uiso 1 1 calc R . . C4 C 0.4842(5) 0.6072(4) 0.6046(3) 0.0551(14) Uani 1 1 d . . . H4A H 0.5548 0.5992 0.5699 0.066 Uiso 1 1 calc R . . C5 C 0.5071(5) 0.6532(4) 0.6849(3) 0.0502(13) Uani 1 1 d . . . H5A H 0.5976 0.6836 0.7160 0.060 Uiso 1 1 calc R . . C6 C 0.5504(4) 0.9495(4) 0.6649(2) 0.0344(10) Uani 1 1 d . . . C7 C 0.4234(4) 0.9498(4) 0.6971(2) 0.0347(10) Uani 1 1 d . . . H7A H 0.4142 0.9774 0.7519 0.042 Uiso 1 1 calc R . . C8 C 0.3123(4) 0.9029(4) 0.6355(3) 0.0385(11) Uani 1 1 d . . . H8A H 0.2144 0.8927 0.6415 0.046 Uiso 1 1 calc R . . C9 C 0.3655(4) 0.8694(4) 0.5655(3) 0.0396(12) Uani 1 1 d . . . H9A H 0.3128 0.8350 0.5142 0.048 Uiso 1 1 calc R . . C10 C 0.5128(4) 0.8977(4) 0.5835(2) 0.0310(10) Uani 1 1 d . . . C11 C 0.6142(4) 0.8558(4) 0.5367(2) 0.0327(10) Uani 1 1 d . . . C12 C 0.5665(5) 0.7831(5) 0.4538(2) 0.0508(13) Uani 1 1 d . . . H12A H 0.6428 0.7615 0.4302 0.076 Uiso 1 1 calc R . . H12B H 0.5322 0.8358 0.4267 0.076 Uiso 1 1 calc R . . H12C H 0.4942 0.7058 0.4520 0.076 Uiso 1 1 calc R . . C13 C 0.8356(4) 0.8284(4) 0.5350(2) 0.0324(10) Uani 1 1 d . . . C14 C 0.8829(4) 0.7395(4) 0.5637(2) 0.0348(11) Uani 1 1 d . . . H14A H 0.8538 0.7195 0.6089 0.042 Uiso 1 1 calc R . . C15 C 0.9728(4) 0.6806(4) 0.5256(2) 0.0374(11) Uani 1 1 d . . . H15A H 1.0041 0.6209 0.5447 0.045 Uiso 1 1 calc R . . C16 C 1.0154(4) 0.7122(4) 0.4587(2) 0.0362(11) Uani 1 1 d . . . C17 C 0.9745(4) 0.8030(4) 0.4313(3) 0.0448(12) Uani 1 1 d . . . H17A H 1.0066 0.8254 0.3871 0.054 Uiso 1 1 calc R . . C18 C 0.8855(4) 0.8606(4) 0.4696(3) 0.0426(11) Uani 1 1 d . . . H18A H 0.8580 0.9228 0.4512 0.051 Uiso 1 1 calc R . . C19 C 0.9426(4) 1.2287(4) 0.8451(2) 0.0294(10) Uani 1 1 d . . . H19A H 1.0040 1.1741 0.8340 0.035 Uiso 1 1 calc R . . C20 C 0.9849(4) 1.3283(4) 0.7977(2) 0.0408(12) Uani 1 1 d . . . H20A H 0.9645 1.2858 0.7433 0.049 Uiso 1 1 calc R . . H20B H 0.9320 1.3895 0.8087 0.049 Uiso 1 1 calc R . . C21 C 1.1391(4) 1.3994(5) 0.8163(3) 0.0542(14) Uani 1 1 d . . . H21A H 1.1922 1.3392 0.8013 0.065 Uiso 1 1 calc R . . H21B H 1.1631 1.4642 0.7870 0.065 Uiso 1 1 calc R . . C22 C 1.1759(4) 1.4631(5) 0.9017(3) 0.0548(14) Uani 1 1 d . . . H22A H 1.2749 1.5032 0.9127 0.066 Uiso 1 1 calc R . . H22B H 1.1303 1.5297 0.9155 0.066 Uiso 1 1 calc R . . C23 C 1.1319(4) 1.3659(4) 0.9491(3) 0.0473(13) Uani 1 1 d . . . H23A H 1.1524 1.4095 1.0033 0.057 Uiso 1 1 calc R . . H23B H 1.1848 1.3045 0.9389 0.057 Uiso 1 1 calc R . . C24 C 0.9784(4) 1.2943(4) 0.9314(2) 0.0409(11) Uani 1 1 d . . . H24A H 0.9246 1.3540 0.9459 0.049 Uiso 1 1 calc R . . H24B H 0.9552 1.2301 0.9611 0.049 Uiso 1 1 calc R . . C25 C 0.6410(4) 1.2153(4) 0.8156(2) 0.0298(10) Uani 1 1 d . . . H25A H 0.5498 1.1530 0.8110 0.036 Uiso 1 1 calc R . . C26 C 0.6345(4) 1.2753(4) 0.7470(2) 0.0367(11) Uani 1 1 d . . . H26A H 0.7215 1.3400 0.7484 0.044 Uiso 1 1 calc R . . H26B H 0.6211 1.2095 0.6995 0.044 Uiso 1 1 calc R . . C27 C 0.5171(4) 1.3367(4) 0.7481(3) 0.0461(12) Uani 1 1 d . . . H27A H 0.5193 1.3785 0.7059 0.055 Uiso 1 1 calc R . . H27B H 0.4293 1.2705 0.7407 0.055 Uiso 1 1 calc R . . C28 C 0.5285(4) 1.4347(4) 0.8236(3) 0.0479(13) Uani 1 1 d . . . H28A H 0.4504 1.4696 0.8234 0.058 Uiso 1 1 calc R . . H28B H 0.6123 1.5050 0.8288 0.058 Uiso 1 1 calc R . . C29 C 0.5311(4) 1.3750(5) 0.8918(3) 0.0509(13) Uani 1 1 d . . . H29A H 0.4441 1.3097 0.8892 0.061 Uiso 1 1 calc R . . H29B H 0.5426 1.4404 0.9393 0.061 Uiso 1 1 calc R . . C30 C 0.6506(4) 1.3143(4) 0.8914(2) 0.0398(11) Uani 1 1 d . . . H30A H 0.7379 1.3812 0.8990 0.048 Uiso 1 1 calc R . . H30B H 0.6484 1.2730 0.9337 0.048 Uiso 1 1 calc R . . C31 C 0.7280(3) 1.0283(4) 0.8859(2) 0.0290(10) Uani 1 1 d . . . H31A H 0.7456 1.0911 0.9358 0.035 Uiso 1 1 calc R . . C32 C 0.8297(4) 0.9473(4) 0.8867(3) 0.0426(12) Uani 1 1 d . . . H32A H 0.8198 0.8893 0.8363 0.051 Uiso 1 1 calc R . . H32B H 0.9237 1.0038 0.8970 0.051 Uiso 1 1 calc R . . C33 C 0.8038(4) 0.8696(5) 0.9473(3) 0.0510(13) Uani 1 1 d . . . H33A H 0.8657 0.8161 0.9441 0.061 Uiso 1 1 calc R . . H33B H 0.8236 0.9277 0.9982 0.061 Uiso 1 1 calc R . . C34 C 0.6561(4) 0.7857(5) 0.9363(3) 0.0560(14) Uani 1 1 d . . . H34A H 0.6421 0.7400 0.9767 0.067 Uiso 1 1 calc R . . H34B H 0.6390 0.7225 0.8874 0.067 Uiso 1 1 calc R . . C35 C 0.5538(4) 0.8643(5) 0.9378(3) 0.0528(14) Uani 1 1 d . . . H35A H 0.4601 0.8071 0.9276 0.063 Uiso 1 1 calc R . . H35B H 0.5642 0.9214 0.9885 0.063 Uiso 1 1 calc R . . C36 C 0.5783(4) 0.9430(4) 0.8776(2) 0.0370(11) Uani 1 1 d . . . H36A H 0.5166 0.9967 0.8822 0.044 Uiso 1 1 calc R . . H36B H 0.5559 0.8851 0.8267 0.044 Uiso 1 1 calc R . . C37 C 0.9257(6) 0.2223(6) 0.2143(4) 0.093(2) Uani 1 1 d . . . H37A H 0.9520 0.1479 0.2217 0.112 Uiso 1 1 calc R . . H37B H 0.8671 0.2429 0.2535 0.112 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.03044(17) 0.0224(2) 0.02099(19) 0.00166(14) 0.00244(12) 0.00748(13) Fe1 0.0346(3) 0.0270(4) 0.0371(4) 0.0029(3) -0.0014(3) 0.0057(3) P1 0.0347(6) 0.0213(6) 0.0218(6) 0.0028(5) 0.0020(4) 0.0080(5) N1 0.039(2) 0.035(2) 0.022(2) 0.0015(17) 0.0008(15) 0.0104(16) Cl1 0.0355(5) 0.0441(7) 0.0359(7) 0.0014(6) 0.0029(5) 0.0169(5) Cl2 0.0552(7) 0.0616(9) 0.0462(8) -0.0007(7) 0.0142(6) 0.0246(6) Cl3 0.1258(16) 0.183(2) 0.1023(17) 0.0274(16) 0.0068(13) 0.0578(16) Cl4 0.180(2) 0.0669(14) 0.145(2) 0.0177(13) 0.0075(16) 0.0352(14) C1 0.058(3) 0.036(3) 0.056(3) 0.017(3) 0.007(3) 0.008(2) C2 0.053(3) 0.030(3) 0.079(4) 0.009(3) 0.006(3) -0.002(2) C3 0.068(3) 0.027(3) 0.057(4) -0.006(3) -0.006(3) 0.000(2) C4 0.060(3) 0.029(3) 0.075(4) 0.005(3) 0.014(3) 0.014(2) C5 0.048(3) 0.035(3) 0.068(4) 0.018(3) -0.004(2) 0.012(2) C6 0.044(2) 0.022(2) 0.033(3) 0.001(2) 0.0079(19) 0.0079(19) C7 0.041(2) 0.024(3) 0.034(3) -0.001(2) 0.0060(19) 0.0060(19) C8 0.027(2) 0.033(3) 0.050(3) 0.003(2) -0.007(2) 0.0059(18) C9 0.032(2) 0.043(3) 0.042(3) 0.008(2) -0.006(2) 0.011(2) C10 0.034(2) 0.033(3) 0.024(2) 0.006(2) -0.0012(17) 0.0087(18) C11 0.042(2) 0.027(3) 0.024(2) 0.004(2) -0.0007(18) 0.0032(19) C12 0.065(3) 0.050(3) 0.025(3) -0.001(2) -0.003(2) 0.007(2) C13 0.042(2) 0.024(3) 0.023(2) -0.002(2) 0.0049(19) 0.0037(19) C14 0.039(2) 0.037(3) 0.027(3) 0.006(2) 0.0080(19) 0.011(2) C15 0.043(2) 0.033(3) 0.037(3) 0.006(2) 0.001(2) 0.013(2) C16 0.028(2) 0.040(3) 0.034(3) -0.002(2) 0.0056(18) 0.0075(19) C17 0.058(3) 0.045(3) 0.033(3) 0.014(2) 0.017(2) 0.013(2) C18 0.059(3) 0.033(3) 0.041(3) 0.015(2) 0.015(2) 0.016(2) C19 0.036(2) 0.023(2) 0.028(2) 0.0041(19) 0.0026(17) 0.0079(18) C20 0.045(3) 0.035(3) 0.036(3) 0.007(2) 0.001(2) 0.001(2) C21 0.046(3) 0.050(3) 0.059(4) 0.020(3) 0.010(2) -0.003(2) C22 0.048(3) 0.045(3) 0.055(4) 0.001(3) -0.005(2) -0.004(2) C23 0.049(3) 0.040(3) 0.043(3) -0.003(3) -0.013(2) 0.011(2) C24 0.046(3) 0.039(3) 0.032(3) 0.003(2) -0.003(2) 0.009(2) C25 0.038(2) 0.023(2) 0.029(3) 0.004(2) 0.0055(18) 0.0116(18) C26 0.048(3) 0.034(3) 0.029(3) 0.006(2) 0.0003(19) 0.017(2) C27 0.057(3) 0.044(3) 0.045(3) 0.012(3) -0.001(2) 0.027(2) C28 0.050(3) 0.038(3) 0.062(4) 0.006(3) 0.001(2) 0.029(2) C29 0.056(3) 0.055(4) 0.046(3) 0.002(3) 0.008(2) 0.033(3) C30 0.053(3) 0.038(3) 0.029(3) -0.001(2) 0.004(2) 0.022(2) C31 0.038(2) 0.027(3) 0.024(2) 0.008(2) 0.0018(17) 0.0115(18) C32 0.048(3) 0.043(3) 0.049(3) 0.024(3) 0.010(2) 0.021(2) C33 0.054(3) 0.055(4) 0.061(4) 0.029(3) 0.007(2) 0.030(3) C34 0.076(3) 0.046(3) 0.058(4) 0.031(3) 0.011(3) 0.022(3) C35 0.050(3) 0.061(4) 0.056(3) 0.035(3) 0.015(2) 0.012(2) C36 0.030(2) 0.040(3) 0.043(3) 0.014(2) 0.0040(19) 0.0102(19) C37 0.121(5) 0.109(6) 0.093(5) 0.055(5) 0.051(4) 0.073(5) _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 C6 2.014(4) . ? Pd1 N1 2.172(3) . ? Pd1 P1 2.2813(14) . ? Pd1 Cl1 2.3987(11) . ? Fe1 C10 2.026(4) . ? Fe1 C9 2.045(4) . ? Fe1 C5 2.052(4) . ? Fe1 C1 2.059(5) . ? Fe1 C8 2.062(4) . ? Fe1 C7 2.064(4) . ? Fe1 C3 2.064(5) . ? Fe1 C4 2.065(5) . ? Fe1 C2 2.070(5) . ? Fe1 C6 2.082(4) . ? P1 C25 1.847(4) . ? P1 C31 1.848(4) . ? P1 C19 1.869(4) . ? N1 C11 1.288(5) . ? N1 C13 1.435(5) . ? Cl2 C16 1.761(4) . ? Cl3 C37 1.706(6) . ? Cl4 C37 1.746(7) . ? C1 C5 1.405(6) . ? C1 C2 1.426(6) . ? C1 H1A 0.9800 . ? C2 C3 1.405(7) . ? C2 H2A 0.9800 . ? C3 C4 1.417(6) . ? C3 H3A 0.9800 . ? C4 C5 1.403(7) . ? C4 H4A 0.9800 . ? C5 H5A 0.9800 . ? C6 C7 1.435(5) . ? C6 C10 1.437(5) . ? C7 C8 1.436(5) . ? C7 H7A 0.9800 . ? C8 C9 1.406(6) . ? C8 H8A 0.9800 . ? C9 C10 1.441(5) . ? C9 H9A 0.9800 . ? C10 C11 1.465(5) . ? C11 C12 1.511(5) . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 C18 1.381(6) . ? C13 C14 1.390(6) . ? C14 C15 1.383(5) . ? C14 H14A 0.9300 . ? C15 C16 1.380(6) . ? C15 H15A 0.9300 . ? C16 C17 1.366(6) . ? C17 C18 1.369(6) . ? C17 H17A 0.9300 . ? C18 H18A 0.9300 . ? C19 C20 1.528(6) . ? C19 C24 1.537(5) . ? C19 H19A 0.9800 . ? C20 C21 1.527(5) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 C22 1.519(6) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 C23 1.510(6) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 C24 1.522(5) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 C30 1.530(5) . ? C25 C26 1.532(5) . ? C25 H25A 0.9800 . ? C26 C27 1.522(5) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C27 C28 1.518(6) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 C29 1.519(6) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C29 C30 1.535(5) . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C31 C36 1.534(5) . ? C31 C32 1.543(5) . ? C31 H31A 0.9800 . ? C32 C33 1.526(6) . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C33 C34 1.508(6) . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C34 C35 1.525(6) . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C35 C36 1.524(6) . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C36 H36A 0.9700 . ? C36 H36B 0.9700 . ? C37 H37A 0.9700 . ? C37 H37B 0.9700 . ? 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 C6 Pd1 N1 80.35(15) . . ? C6 Pd1 P1 95.38(12) . . ? N1 Pd1 P1 172.04(9) . . ? C6 Pd1 Cl1 170.74(12) . . ? N1 Pd1 Cl1 90.63(9) . . ? P1 Pd1 Cl1 93.83(5) . . ? C10 Fe1 C9 41.47(14) . . ? C10 Fe1 C5 123.20(18) . . ? C9 Fe1 C5 160.38(19) . . ? C10 Fe1 C1 159.79(16) . . ? C9 Fe1 C1 157.87(17) . . ? C5 Fe1 C1 39.98(17) . . ? C10 Fe1 C8 67.95(17) . . ? C9 Fe1 C8 40.03(16) . . ? C5 Fe1 C8 158.0(2) . . ? C1 Fe1 C8 123.73(19) . . ? C10 Fe1 C7 68.18(17) . . ? C9 Fe1 C7 68.61(17) . . ? C5 Fe1 C7 121.66(19) . . ? C1 Fe1 C7 108.81(19) . . ? C8 Fe1 C7 40.72(15) . . ? C10 Fe1 C3 121.6(2) . . ? C9 Fe1 C3 108.4(2) . . ? C5 Fe1 C3 66.9(2) . . ? C1 Fe1 C3 67.2(2) . . ? C8 Fe1 C3 126.30(18) . . ? C7 Fe1 C3 162.80(18) . . ? C10 Fe1 C4 106.60(19) . . ? C9 Fe1 C4 124.2(2) . . ? C5 Fe1 C4 39.85(18) . . ? C1 Fe1 C4 67.4(2) . . ? C8 Fe1 C4 161.43(19) . . ? C7 Fe1 C4 155.65(17) . . ? C3 Fe1 C4 40.12(17) . . ? C10 Fe1 C2 157.18(19) . . ? C9 Fe1 C2 122.26(19) . . ? C5 Fe1 C2 67.24(19) . . ? C1 Fe1 C2 40.39(18) . . ? C8 Fe1 C2 110.33(18) . . ? C7 Fe1 C2 126.43(19) . . ? C3 Fe1 C2 39.72(19) . . ? C4 Fe1 C2 67.4(2) . . ? C10 Fe1 C6 40.92(15) . . ? C9 Fe1 C6 69.49(17) . . ? C5 Fe1 C6 106.62(17) . . ? C1 Fe1 C6 123.77(18) . . ? C8 Fe1 C6 68.37(15) . . ? C7 Fe1 C6 40.48(15) . . ? C3 Fe1 C6 155.92(19) . . ? C4 Fe1 C6 119.97(17) . . ? C2 Fe1 C6 161.5(2) . . ? C25 P1 C31 106.40(18) . . ? C25 P1 C19 109.06(19) . . ? C31 P1 C19 103.23(17) . . ? C25 P1 Pd1 114.07(13) . . ? C31 P1 Pd1 112.20(14) . . ? C19 P1 Pd1 111.21(14) . . ? C11 N1 C13 118.5(3) . . ? C11 N1 Pd1 113.9(3) . . ? C13 N1 Pd1 127.4(2) . . ? C5 C1 C2 107.5(5) . . ? C5 C1 Fe1 69.7(3) . . ? C2 C1 Fe1 70.2(3) . . ? C5 C1 H1A 126.3 . . ? C2 C1 H1A 126.3 . . ? Fe1 C1 H1A 126.3 . . ? C3 C2 C1 107.4(4) . . ? C3 C2 Fe1 69.9(3) . . ? C1 C2 Fe1 69.4(3) . . ? C3 C2 H2A 126.3 . . ? C1 C2 H2A 126.3 . . ? Fe1 C2 H2A 126.3 . . ? C2 C3 C4 108.8(5) . . ? C2 C3 Fe1 70.4(3) . . ? C4 C3 Fe1 70.0(3) . . ? C2 C3 H3A 125.6 . . ? C4 C3 H3A 125.6 . . ? Fe1 C3 H3A 125.6 . . ? C5 C4 C3 107.1(4) . . ? C5 C4 Fe1 69.6(3) . . ? C3 C4 Fe1 69.9(3) . . ? C5 C4 H4A 126.4 . . ? C3 C4 H4A 126.4 . . ? Fe1 C4 H4A 126.4 . . ? C4 C5 C1 109.2(4) . . ? C4 C5 Fe1 70.6(3) . . ? C1 C5 Fe1 70.3(3) . . ? C4 C5 H5A 125.4 . . ? C1 C5 H5A 125.4 . . ? Fe1 C5 H5A 125.4 . . ? C7 C6 C10 105.9(3) . . ? C7 C6 Pd1 143.3(3) . . ? C10 C6 Pd1 110.7(3) . . ? C7 C6 Fe1 69.1(2) . . ? C10 C6 Fe1 67.4(2) . . ? Pd1 C6 Fe1 123.7(2) . . ? C6 C7 C8 108.5(4) . . ? C6 C7 Fe1 70.4(2) . . ? C8 C7 Fe1 69.6(2) . . ? C6 C7 H7A 125.8 . . ? C8 C7 H7A 125.8 . . ? Fe1 C7 H7A 125.8 . . ? C9 C8 C7 109.2(3) . . ? C9 C8 Fe1 69.3(2) . . ? C7 C8 Fe1 69.7(2) . . ? C9 C8 H8A 125.4 . . ? C7 C8 H8A 125.4 . . ? Fe1 C8 H8A 125.4 . . ? C8 C9 C10 106.7(4) . . ? C8 C9 Fe1 70.6(3) . . ? C10 C9 Fe1 68.5(2) . . ? C8 C9 H9A 126.6 . . ? C10 C9 H9A 126.6 . . ? Fe1 C9 H9A 126.6 . . ? C6 C10 C9 109.7(4) . . ? C6 C10 C11 119.0(3) . . ? C9 C10 C11 129.7(4) . . ? C6 C10 Fe1 71.7(2) . . ? C9 C10 Fe1 70.0(2) . . ? C11 C10 Fe1 113.0(3) . . ? N1 C11 C10 114.7(4) . . ? N1 C11 C12 127.0(4) . . ? C10 C11 C12 118.2(4) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C18 C13 C14 118.3(4) . . ? C18 C13 N1 122.8(4) . . ? C14 C13 N1 118.8(4) . . ? C15 C14 C13 120.7(4) . . ? C15 C14 H14A 119.6 . . ? C13 C14 H14A 119.6 . . ? C16 C15 C14 118.8(4) . . ? C16 C15 H15A 120.6 . . ? C14 C15 H15A 120.6 . . ? C17 C16 C15 121.4(4) . . ? C17 C16 Cl2 119.6(4) . . ? C15 C16 Cl2 119.0(4) . . ? C16 C17 C18 119.2(4) . . ? C16 C17 H17A 120.4 . . ? C18 C17 H17A 120.4 . . ? C17 C18 C13 121.5(4) . . ? C17 C18 H18A 119.2 . . ? C13 C18 H18A 119.2 . . ? C20 C19 C24 110.0(3) . . ? C20 C19 P1 112.0(3) . . ? C24 C19 P1 118.1(3) . . ? C20 C19 H19A 105.2 . . ? C24 C19 H19A 105.2 . . ? P1 C19 H19A 105.2 . . ? C21 C20 C19 110.8(3) . . ? C21 C20 H20A 109.5 . . ? C19 C20 H20A 109.5 . . ? C21 C20 H20B 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 108.1 . . ? C22 C21 C20 110.9(4) . . ? C22 C21 H21A 109.5 . . ? C20 C21 H21A 109.5 . . ? C22 C21 H21B 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 108.0 . . ? C23 C22 C21 110.8(4) . . ? C23 C22 H22A 109.5 . . ? C21 C22 H22A 109.5 . . ? C23 C22 H22B 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 108.1 . . ? C22 C23 C24 112.2(3) . . ? C22 C23 H23A 109.2 . . ? C24 C23 H23A 109.2 . . ? C22 C23 H23B 109.2 . . ? C24 C23 H23B 109.2 . . ? H23A C23 H23B 107.9 . . ? C23 C24 C19 110.0(4) . . ? C23 C24 H24A 109.7 . . ? C19 C24 H24A 109.7 . . ? C23 C24 H24B 109.7 . . ? C19 C24 H24B 109.7 . . ? H24A C24 H24B 108.2 . . ? C30 C25 C26 110.7(3) . . ? C30 C25 P1 116.7(3) . . ? C26 C25 P1 113.9(3) . . ? C30 C25 H25A 104.7 . . ? C26 C25 H25A 104.7 . . ? P1 C25 H25A 104.7 . . ? C27 C26 C25 111.4(3) . . ? C27 C26 H26A 109.3 . . ? C25 C26 H26A 109.3 . . ? C27 C26 H26B 109.3 . . ? C25 C26 H26B 109.3 . . ? H26A C26 H26B 108.0 . . ? C28 C27 C26 111.3(3) . . ? C28 C27 H27A 109.4 . . ? C26 C27 H27A 109.4 . . ? C28 C27 H27B 109.4 . . ? C26 C27 H27B 109.4 . . ? H27A C27 H27B 108.0 . . ? C27 C28 C29 111.4(4) . . ? C27 C28 H28A 109.4 . . ? C29 C28 H28A 109.4 . . ? C27 C28 H28B 109.4 . . ? C29 C28 H28B 109.4 . . ? H28A C28 H28B 108.0 . . ? C28 C29 C30 110.2(4) . . ? C28 C29 H29A 109.6 . . ? C30 C29 H29A 109.6 . . ? C28 C29 H29B 109.6 . . ? C30 C29 H29B 109.6 . . ? H29A C29 H29B 108.1 . . ? C25 C30 C29 111.5(3) . . ? C25 C30 H30A 109.3 . . ? C29 C30 H30A 109.3 . . ? C25 C30 H30B 109.3 . . ? C29 C30 H30B 109.3 . . ? H30A C30 H30B 108.0 . . ? C36 C31 C32 110.3(3) . . ? C36 C31 P1 114.0(3) . . ? C32 C31 P1 109.4(3) . . ? C36 C31 H31A 107.6 . . ? C32 C31 H31A 107.6 . . ? P1 C31 H31A 107.6 . . ? C33 C32 C31 111.7(3) . . ? C33 C32 H32A 109.3 . . ? C31 C32 H32A 109.3 . . ? C33 C32 H32B 109.3 . . ? C31 C32 H32B 109.3 . . ? H32A C32 H32B 107.9 . . ? C34 C33 C32 111.2(3) . . ? C34 C33 H33A 109.4 . . ? C32 C33 H33A 109.4 . . ? C34 C33 H33B 109.4 . . ? C32 C33 H33B 109.4 . . ? H33A C33 H33B 108.0 . . ? C33 C34 C35 111.7(4) . . ? C33 C34 H34A 109.3 . . ? C35 C34 H34A 109.3 . . ? C33 C34 H34B 109.3 . . ? C35 C34 H34B 109.3 . . ? H34A C34 H34B 107.9 . . ? C36 C35 C34 110.6(4) . . ? C36 C35 H35A 109.5 . . ? C34 C35 H35A 109.5 . . ? C36 C35 H35B 109.5 . . ? C34 C35 H35B 109.5 . . ? H35A C35 H35B 108.1 . . ? C35 C36 C31 112.7(3) . . ? C35 C36 H36A 109.0 . . ? C31 C36 H36A 109.0 . . ? C35 C36 H36B 109.0 . . ? C31 C36 H36B 109.0 . . ? H36A C36 H36B 107.8 . . ? Cl3 C37 Cl4 112.7(4) . . ? Cl3 C37 H37A 109.0 . . ? Cl4 C37 H37A 109.0 . . ? Cl3 C37 H37B 109.0 . . ? Cl4 C37 H37B 109.0 . . ? H37A C37 H37B 107.8 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 Pd1 P1 C25 -34.26(19) . . . . ? N1 Pd1 P1 C25 22.9(7) . . . . ? Cl1 Pd1 P1 C25 146.78(15) . . . . ? C6 Pd1 P1 C31 86.82(17) . . . . ? N1 Pd1 P1 C31 143.9(6) . . . . ? Cl1 Pd1 P1 C31 -92.14(12) . . . . ? C6 Pd1 P1 C19 -158.11(18) . . . . ? N1 Pd1 P1 C19 -101.0(6) . . . . ? Cl1 Pd1 P1 C19 22.93(14) . . . . ? C6 Pd1 N1 C11 8.1(3) . . . . ? P1 Pd1 N1 C11 -49.9(8) . . . . ? Cl1 Pd1 N1 C11 -174.0(3) . . . . ? C6 Pd1 N1 C13 -167.0(4) . . . . ? P1 Pd1 N1 C13 135.0(5) . . . . ? Cl1 Pd1 N1 C13 10.9(3) . . . . ? C10 Fe1 C1 C5 -39.4(7) . . . . ? C9 Fe1 C1 C5 163.5(4) . . . . ? C8 Fe1 C1 C5 -159.9(3) . . . . ? C7 Fe1 C1 C5 -117.2(3) . . . . ? C3 Fe1 C1 C5 80.7(3) . . . . ? C4 Fe1 C1 C5 37.1(3) . . . . ? C2 Fe1 C1 C5 118.2(4) . . . . ? C6 Fe1 C1 C5 -74.8(3) . . . . ? C10 Fe1 C1 C2 -157.6(5) . . . . ? C9 Fe1 C1 C2 45.3(6) . . . . ? C5 Fe1 C1 C2 -118.2(4) . . . . ? C8 Fe1 C1 C2 81.9(3) . . . . ? C7 Fe1 C1 C2 124.6(3) . . . . ? C3 Fe1 C1 C2 -37.5(3) . . . . ? C4 Fe1 C1 C2 -81.1(3) . . . . ? C6 Fe1 C1 C2 167.0(3) . . . . ? C5 C1 C2 C3 -0.3(6) . . . . ? Fe1 C1 C2 C3 59.8(4) . . . . ? C5 C1 C2 Fe1 -60.1(3) . . . . ? C10 Fe1 C2 C3 41.6(6) . . . . ? C9 Fe1 C2 C3 79.9(3) . . . . ? C5 Fe1 C2 C3 -80.7(3) . . . . ? C1 Fe1 C2 C3 -118.6(4) . . . . ? C8 Fe1 C2 C3 122.8(3) . . . . ? C7 Fe1 C2 C3 165.8(3) . . . . ? C4 Fe1 C2 C3 -37.4(3) . . . . ? C6 Fe1 C2 C3 -154.7(5) . . . . ? C10 Fe1 C2 C1 160.2(4) . . . . ? C9 Fe1 C2 C1 -161.5(3) . . . . ? C5 Fe1 C2 C1 37.9(3) . . . . ? C8 Fe1 C2 C1 -118.6(3) . . . . ? C7 Fe1 C2 C1 -75.6(3) . . . . ? C3 Fe1 C2 C1 118.6(4) . . . . ? C4 Fe1 C2 C1 81.2(3) . . . . ? C6 Fe1 C2 C1 -36.1(7) . . . . ? C1 C2 C3 C4 0.2(6) . . . . ? Fe1 C2 C3 C4 59.6(3) . . . . ? C1 C2 C3 Fe1 -59.5(3) . . . . ? C10 Fe1 C3 C2 -162.4(3) . . . . ? C9 Fe1 C3 C2 -118.7(3) . . . . ? C5 Fe1 C3 C2 81.7(3) . . . . ? C1 Fe1 C3 C2 38.1(3) . . . . ? C8 Fe1 C3 C2 -77.9(4) . . . . ? C7 Fe1 C3 C2 -41.8(8) . . . . ? C4 Fe1 C3 C2 119.6(5) . . . . ? C6 Fe1 C3 C2 160.6(4) . . . . ? C10 Fe1 C3 C4 77.9(3) . . . . ? C9 Fe1 C3 C4 121.7(3) . . . . ? C5 Fe1 C3 C4 -37.9(3) . . . . ? C1 Fe1 C3 C4 -81.5(3) . . . . ? C8 Fe1 C3 C4 162.5(3) . . . . ? C7 Fe1 C3 C4 -161.4(6) . . . . ? C2 Fe1 C3 C4 -119.6(5) . . . . ? C6 Fe1 C3 C4 41.0(6) . . . . ? C2 C3 C4 C5 0.0(6) . . . . ? Fe1 C3 C4 C5 59.9(3) . . . . ? C2 C3 C4 Fe1 -59.9(4) . . . . ? C10 Fe1 C4 C5 122.3(3) . . . . ? C9 Fe1 C4 C5 164.3(3) . . . . ? C1 Fe1 C4 C5 -37.2(3) . . . . ? C8 Fe1 C4 C5 -167.7(5) . . . . ? C7 Fe1 C4 C5 48.7(6) . . . . ? C3 Fe1 C4 C5 -118.1(4) . . . . ? C2 Fe1 C4 C5 -81.1(3) . . . . ? C6 Fe1 C4 C5 79.9(3) . . . . ? C10 Fe1 C4 C3 -119.6(3) . . . . ? C9 Fe1 C4 C3 -77.6(4) . . . . ? C5 Fe1 C4 C3 118.1(4) . . . . ? C1 Fe1 C4 C3 80.9(3) . . . . ? C8 Fe1 C4 C3 -49.7(7) . . . . ? C7 Fe1 C4 C3 166.8(4) . . . . ? C2 Fe1 C4 C3 37.0(3) . . . . ? C6 Fe1 C4 C3 -162.0(3) . . . . ? C3 C4 C5 C1 -0.2(5) . . . . ? Fe1 C4 C5 C1 59.9(3) . . . . ? C3 C4 C5 Fe1 -60.1(3) . . . . ? C2 C1 C5 C4 0.3(5) . . . . ? Fe1 C1 C5 C4 -60.1(3) . . . . ? C2 C1 C5 Fe1 60.4(3) . . . . ? C10 Fe1 C5 C4 -75.5(3) . . . . ? C9 Fe1 C5 C4 -41.7(6) . . . . ? C1 Fe1 C5 C4 119.7(4) . . . . ? C8 Fe1 C5 C4 169.6(4) . . . . ? C7 Fe1 C5 C4 -158.7(3) . . . . ? C3 Fe1 C5 C4 38.2(3) . . . . ? C2 Fe1 C5 C4 81.5(3) . . . . ? C6 Fe1 C5 C4 -117.1(3) . . . . ? C10 Fe1 C5 C1 164.8(3) . . . . ? C9 Fe1 C5 C1 -161.4(5) . . . . ? C8 Fe1 C5 C1 49.9(6) . . . . ? C7 Fe1 C5 C1 81.6(3) . . . . ? C3 Fe1 C5 C1 -81.6(3) . . . . ? C4 Fe1 C5 C1 -119.7(4) . . . . ? C2 Fe1 C5 C1 -38.3(3) . . . . ? C6 Fe1 C5 C1 123.1(3) . . . . ? N1 Pd1 C6 C7 166.0(5) . . . . ? P1 Pd1 C6 C7 -20.8(5) . . . . ? Cl1 Pd1 C6 C7 152.8(5) . . . . ? N1 Pd1 C6 C10 -10.3(3) . . . . ? P1 Pd1 C6 C10 163.0(3) . . . . ? Cl1 Pd1 C6 C10 -23.5(10) . . . . ? N1 Pd1 C6 Fe1 65.8(2) . . . . ? P1 Pd1 C6 Fe1 -121.0(2) . . . . ? Cl1 Pd1 C6 Fe1 52.6(9) . . . . ? C10 Fe1 C6 C7 118.5(3) . . . . ? C9 Fe1 C6 C7 80.7(3) . . . . ? C5 Fe1 C6 C7 -119.6(3) . . . . ? C1 Fe1 C6 C7 -79.3(3) . . . . ? C8 Fe1 C6 C7 37.7(2) . . . . ? C3 Fe1 C6 C7 170.0(4) . . . . ? C4 Fe1 C6 C7 -160.8(3) . . . . ? C2 Fe1 C6 C7 -51.9(6) . . . . ? C9 Fe1 C6 C10 -37.8(2) . . . . ? C5 Fe1 C6 C10 121.9(3) . . . . ? C1 Fe1 C6 C10 162.2(2) . . . . ? C8 Fe1 C6 C10 -80.8(3) . . . . ? C7 Fe1 C6 C10 -118.5(3) . . . . ? C3 Fe1 C6 C10 51.5(5) . . . . ? C4 Fe1 C6 C10 80.7(3) . . . . ? C2 Fe1 C6 C10 -170.4(5) . . . . ? C10 Fe1 C6 Pd1 -100.5(3) . . . . ? C9 Fe1 C6 Pd1 -138.3(3) . . . . ? C5 Fe1 C6 Pd1 21.4(3) . . . . ? C1 Fe1 C6 Pd1 61.7(3) . . . . ? C8 Fe1 C6 Pd1 178.6(3) . . . . ? C7 Fe1 C6 Pd1 141.0(4) . . . . ? C3 Fe1 C6 Pd1 -49.0(6) . . . . ? C4 Fe1 C6 Pd1 -19.8(3) . . . . ? C2 Fe1 C6 Pd1 89.0(6) . . . . ? C10 C6 C7 C8 -1.9(5) . . . . ? Pd1 C6 C7 C8 -178.2(4) . . . . ? Fe1 C6 C7 C8 -59.4(3) . . . . ? C10 C6 C7 Fe1 57.5(3) . . . . ? Pd1 C6 C7 Fe1 -118.8(5) . . . . ? C10 Fe1 C7 C6 -38.3(2) . . . . ? C9 Fe1 C7 C6 -83.1(3) . . . . ? C5 Fe1 C7 C6 78.2(3) . . . . ? C1 Fe1 C7 C6 120.4(3) . . . . ? C8 Fe1 C7 C6 -119.4(4) . . . . ? C3 Fe1 C7 C6 -166.2(6) . . . . ? C4 Fe1 C7 C6 43.7(6) . . . . ? C2 Fe1 C7 C6 161.9(3) . . . . ? C10 Fe1 C7 C8 81.1(3) . . . . ? C9 Fe1 C7 C8 36.3(2) . . . . ? C5 Fe1 C7 C8 -162.4(3) . . . . ? C1 Fe1 C7 C8 -120.2(3) . . . . ? C3 Fe1 C7 C8 -46.8(7) . . . . ? C4 Fe1 C7 C8 163.2(4) . . . . ? C2 Fe1 C7 C8 -78.7(3) . . . . ? C6 Fe1 C7 C8 119.4(4) . . . . ? C6 C7 C8 C9 1.7(5) . . . . ? Fe1 C7 C8 C9 -58.2(3) . . . . ? C6 C7 C8 Fe1 59.9(3) . . . . ? C10 Fe1 C8 C9 39.2(2) . . . . ? C5 Fe1 C8 C9 164.3(4) . . . . ? C1 Fe1 C8 C9 -159.5(2) . . . . ? C7 Fe1 C8 C9 120.9(3) . . . . ? C3 Fe1 C8 C9 -74.6(3) . . . . ? C4 Fe1 C8 C9 -37.0(6) . . . . ? C2 Fe1 C8 C9 -116.4(3) . . . . ? C6 Fe1 C8 C9 83.5(3) . . . . ? C10 Fe1 C8 C7 -81.7(3) . . . . ? C9 Fe1 C8 C7 -120.9(3) . . . . ? C5 Fe1 C8 C7 43.3(5) . . . . ? C1 Fe1 C8 C7 79.5(3) . . . . ? C3 Fe1 C8 C7 164.5(3) . . . . ? C4 Fe1 C8 C7 -158.0(5) . . . . ? C2 Fe1 C8 C7 122.7(3) . . . . ? C6 Fe1 C8 C7 -37.5(2) . . . . ? C7 C8 C9 C10 -0.9(5) . . . . ? Fe1 C8 C9 C10 -59.3(3) . . . . ? C7 C8 C9 Fe1 58.4(3) . . . . ? C10 Fe1 C9 C8 -117.8(3) . . . . ? C5 Fe1 C9 C8 -162.4(5) . . . . ? C1 Fe1 C9 C8 50.5(6) . . . . ? C7 Fe1 C9 C8 -36.9(2) . . . . ? C3 Fe1 C9 C8 125.0(3) . . . . ? C4 Fe1 C9 C8 166.6(2) . . . . ? C2 Fe1 C9 C8 83.5(3) . . . . ? C6 Fe1 C9 C8 -80.4(3) . . . . ? C5 Fe1 C9 C10 -44.6(6) . . . . ? C1 Fe1 C9 C10 168.3(4) . . . . ? C8 Fe1 C9 C10 117.8(3) . . . . ? C7 Fe1 C9 C10 80.8(3) . . . . ? C3 Fe1 C9 C10 -117.2(3) . . . . ? C4 Fe1 C9 C10 -75.7(3) . . . . ? C2 Fe1 C9 C10 -158.7(3) . . . . ? C6 Fe1 C9 C10 37.3(2) . . . . ? C7 C6 C10 C9 1.3(5) . . . . ? Pd1 C6 C10 C9 179.0(3) . . . . ? Fe1 C6 C10 C9 59.9(3) . . . . ? C7 C6 C10 C11 -165.3(4) . . . . ? Pd1 C6 C10 C11 12.4(5) . . . . ? Fe1 C6 C10 C11 -106.7(4) . . . . ? C7 C6 C10 Fe1 -58.6(3) . . . . ? Pd1 C6 C10 Fe1 119.1(2) . . . . ? C8 C9 C10 C6 -0.3(5) . . . . ? Fe1 C9 C10 C6 -60.9(3) . . . . ? C8 C9 C10 C11 164.4(4) . . . . ? Fe1 C9 C10 C11 103.8(5) . . . . ? C8 C9 C10 Fe1 60.7(3) . . . . ? C9 Fe1 C10 C6 119.9(3) . . . . ? C5 Fe1 C10 C6 -76.5(3) . . . . ? C1 Fe1 C10 C6 -47.4(6) . . . . ? C8 Fe1 C10 C6 82.0(3) . . . . ? C7 Fe1 C10 C6 37.9(2) . . . . ? C3 Fe1 C10 C6 -158.0(2) . . . . ? C4 Fe1 C10 C6 -116.9(3) . . . . ? C2 Fe1 C10 C6 172.2(4) . . . . ? C5 Fe1 C10 C9 163.6(3) . . . . ? C1 Fe1 C10 C9 -167.2(5) . . . . ? C8 Fe1 C10 C9 -37.9(2) . . . . ? C7 Fe1 C10 C9 -81.9(3) . . . . ? C3 Fe1 C10 C9 82.2(3) . . . . ? C4 Fe1 C10 C9 123.3(3) . . . . ? C2 Fe1 C10 C9 52.3(6) . . . . ? C6 Fe1 C10 C9 -119.9(3) . . . . ? C9 Fe1 C10 C11 -125.7(4) . . . . ? C5 Fe1 C10 C11 37.9(4) . . . . ? C1 Fe1 C10 C11 67.1(6) . . . . ? C8 Fe1 C10 C11 -163.6(3) . . . . ? C7 Fe1 C10 C11 152.3(3) . . . . ? C3 Fe1 C10 C11 -43.6(3) . . . . ? C4 Fe1 C10 C11 -2.4(3) . . . . ? C2 Fe1 C10 C11 -73.4(5) . . . . ? C6 Fe1 C10 C11 114.4(4) . . . . ? C13 N1 C11 C10 172.1(4) . . . . ? Pd1 N1 C11 C10 -3.5(5) . . . . ? C13 N1 C11 C12 -4.2(7) . . . . ? Pd1 N1 C11 C12 -179.7(4) . . . . ? C6 C10 C11 N1 -5.8(6) . . . . ? C9 C10 C11 N1 -169.4(4) . . . . ? Fe1 C10 C11 N1 -86.9(4) . . . . ? C6 C10 C11 C12 170.7(4) . . . . ? C9 C10 C11 C12 7.2(7) . . . . ? Fe1 C10 C11 C12 89.7(4) . . . . ? C11 N1 C13 C18 62.8(5) . . . . ? Pd1 N1 C13 C18 -122.3(4) . . . . ? C11 N1 C13 C14 -115.6(4) . . . . ? Pd1 N1 C13 C14 59.2(5) . . . . ? C18 C13 C14 C15 -2.9(6) . . . . ? N1 C13 C14 C15 175.7(3) . . . . ? C13 C14 C15 C16 0.3(6) . . . . ? C14 C15 C16 C17 2.3(6) . . . . ? C14 C15 C16 Cl2 -176.3(3) . . . . ? C15 C16 C17 C18 -2.3(7) . . . . ? Cl2 C16 C17 C18 176.3(3) . . . . ? C16 C17 C18 C13 -0.4(7) . . . . ? C14 C13 C18 C17 2.9(6) . . . . ? N1 C13 C18 C17 -175.6(4) . . . . ? C25 P1 C19 C20 -58.1(3) . . . . ? C31 P1 C19 C20 -170.9(3) . . . . ? Pd1 P1 C19 C20 68.6(3) . . . . ? C25 P1 C19 C24 71.3(4) . . . . ? C31 P1 C19 C24 -41.5(4) . . . . ? Pd1 P1 C19 C24 -162.1(3) . . . . ? C24 C19 C20 C21 57.5(5) . . . . ? P1 C19 C20 C21 -169.1(3) . . . . ? C19 C20 C21 C22 -57.1(5) . . . . ? C20 C21 C22 C23 55.7(5) . . . . ? C21 C22 C23 C24 -56.1(5) . . . . ? C22 C23 C24 C19 56.7(5) . . . . ? C20 C19 C24 C23 -56.7(4) . . . . ? P1 C19 C24 C23 173.0(3) . . . . ? C31 P1 C25 C30 61.1(3) . . . . ? C19 P1 C25 C30 -49.6(4) . . . . ? Pd1 P1 C25 C30 -174.6(3) . . . . ? C31 P1 C25 C26 -167.9(3) . . . . ? C19 P1 C25 C26 81.3(3) . . . . ? Pd1 P1 C25 C26 -43.7(3) . . . . ? C30 C25 C26 C27 -54.6(4) . . . . ? P1 C25 C26 C27 171.6(3) . . . . ? C25 C26 C27 C28 55.4(5) . . . . ? C26 C27 C28 C29 -56.8(5) . . . . ? C27 C28 C29 C30 56.8(5) . . . . ? C26 C25 C30 C29 55.2(5) . . . . ? P1 C25 C30 C29 -172.4(3) . . . . ? C28 C29 C30 C25 -56.3(5) . . . . ? C25 P1 C31 C36 57.2(3) . . . . ? C19 P1 C31 C36 172.0(3) . . . . ? Pd1 P1 C31 C36 -68.2(3) . . . . ? C25 P1 C31 C32 -178.7(3) . . . . ? C19 P1 C31 C32 -63.9(3) . . . . ? Pd1 P1 C31 C32 55.9(3) . . . . ? C36 C31 C32 C33 -53.3(5) . . . . ? P1 C31 C32 C33 -179.6(3) . . . . ? C31 C32 C33 C34 55.7(5) . . . . ? C32 C33 C34 C35 -56.9(5) . . . . ? C33 C34 C35 C36 55.9(5) . . . . ? C34 C35 C36 C31 -54.6(5) . . . . ? C32 C31 C36 C35 53.3(5) . . . . ? P1 C31 C36 C35 176.9(3) . . . . ? _diffrn_measured_fraction_theta_max 0.871 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.871 _refine_diff_density_max 0.573 _refine_diff_density_min -0.604 _refine_diff_density_rms 0.073