# Supplementary Material (ESI) for ChemComm # This journal is © The Royal Society of Chemistry 2001 # CCDC Number: 182/1872 data_3a _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C38.50 H33.50 Cl2.50 Fe N2 O4 P2 Pd' _chemical_formula_weight 900.99 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 39.920(8) _cell_length_b 11.851(2) _cell_length_c 16.940(3) _cell_angle_alpha 90.00 _cell_angle_beta 105.60(3) _cell_angle_gamma 90.00 _cell_volume 7719.0(24) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.551 _exptl_crystal_density_method ? _exptl_crystal_F_000 3640 _exptl_absorpt_coefficient_mu 1.140 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Stoe IPDS' _diffrn_measurement_method 'image plate' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24525 _diffrn_reflns_av_R_equivalents 0.0867 _diffrn_reflns_av_sigmaI/netI 0.1144 _diffrn_reflns_limit_h_min -52 _diffrn_reflns_limit_h_max 52 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.27 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6796 _reflns_number_observed 3374 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0500P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment 'riding model' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6796 _refine_ls_number_parameters 448 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1209 _refine_ls_R_factor_obs 0.0574 _refine_ls_wR_factor_all 0.1372 _refine_ls_wR_factor_obs 0.1241 _refine_ls_goodness_of_fit_all 1.042 _refine_ls_goodness_of_fit_obs 1.384 _refine_ls_restrained_S_all 1.042 _refine_ls_restrained_S_obs 1.384 _refine_ls_shift/esd_max 0.111 _refine_ls_shift/esd_mean 0.007 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Pd Pd 0.324365(13) 0.18733(5) 0.47574(3) 0.0343(2) Uani 1 d . . Fe Fe 0.36112(3) 0.32047(10) 0.39684(6) 0.0450(3) Uani 1 d . . Cl1 Cl 0.26823(5) 0.2342(2) 0.38733(10) 0.0399(4) Uani 1 d . . P1 P 0.41230(5) 0.2749(2) 0.48816(12) 0.0421(5) Uani 1 d . . P2 P 0.37364(5) 0.1422(2) 0.57415(11) 0.0373(5) Uani 1 d . . N1 N 0.27633(13) 0.0723(5) 0.5534(3) 0.0316(13) Uani 1 d . . N2 N 0.40898(13) 0.1892(5) 0.5583(3) 0.0419(15) Uani 1 d . . H2 H 0.42855(13) 0.1652(5) 0.5917(3) 0.050 Uiso 1 calc R . O1 O 0.3994(2) 0.4573(6) 0.3056(4) 0.096(2) Uani 1 d . . O2 O 0.34826(14) 0.4561(5) 0.5314(3) 0.061(2) Uani 1 d . . O3 O 0.35829(15) 0.0827(6) 0.3432(3) 0.065(2) Uani 1 d . . O4 O 0.2985(2) 0.3959(6) 0.2703(4) 0.081(2) Uani 1 d . . C1 C 0.3845(2) 0.4023(8) 0.3433(5) 0.061(2) Uani 1 d . . C2 C 0.3525(2) 0.3999(7) 0.4788(5) 0.048(2) Uani 1 d . . C3 C 0.3585(2) 0.1748(9) 0.3667(4) 0.051(2) Uani 1 d . . C4 C 0.3220(2) 0.3631(8) 0.3212(5) 0.058(2) Uani 1 d . . C5 C 0.2992(2) 0.0610(6) 0.5102(4) 0.035(2) Uani 1 d . . C6 C 0.3025(2) -0.0515(6) 0.4735(4) 0.043(2) Uani 1 d . . H6A H 0.3267(3) -0.0639(16) 0.4734(24) 0.064 Uiso 1 calc R . H6B H 0.2876(9) -0.0538(14) 0.4172(10) 0.064 Uiso 1 calc R . H6C H 0.2952(11) -0.1106(7) 0.5059(16) 0.064 Uiso 1 calc R . C7 C 0.2539(2) -0.0152(6) 0.5719(4) 0.035(2) Uani 1 d . . C8 C 0.2282(2) -0.0680(6) 0.5099(4) 0.038(2) Uani 1 d . . C9 C 0.2203(2) -0.0350(7) 0.4196(4) 0.047(2) Uani 1 d . . H9A H 0.2325(10) -0.0865(24) 0.3914(7) 0.070 Uiso 1 calc R . H9B H 0.2282(11) 0.0424(15) 0.4151(4) 0.070 Uiso 1 calc R . H9C H 0.1952(2) -0.0399(38) 0.3944(8) 0.070 Uiso 1 calc R . C10 C 0.2088(2) -0.1538(6) 0.5333(5) 0.045(2) Uani 1 d . . H10 H 0.1914(2) -0.1920(6) 0.4928(5) 0.054 Uiso 1 calc R . C11 C 0.2147(2) -0.1829(7) 0.6136(5) 0.051(2) Uani 1 d . . H11 H 0.2016(2) -0.2425(7) 0.6283(5) 0.062 Uiso 1 calc R . C12 C 0.2394(2) -0.1274(7) 0.6741(5) 0.049(2) Uani 1 d . . H12 H 0.2428(2) -0.1488(7) 0.7297(5) 0.059 Uiso 1 calc R . C13 C 0.2593(2) -0.0414(6) 0.6554(4) 0.037(2) Uani 1 d . . C14 C 0.2842(2) 0.0245(7) 0.7220(4) 0.049(2) Uani 1 d . . H14A H 0.2879(9) -0.0157(20) 0.7742(7) 0.073 Uiso 1 calc R . H14B H 0.2744(6) 0.0992(15) 0.7267(19) 0.073 Uiso 1 calc R . H14C H 0.3064(4) 0.0329(34) 0.7084(14) 0.073 Uiso 1 calc R . C15 C 0.4349(2) 0.3979(6) 0.5414(5) 0.043(2) Uani 1 d . . C16 C 0.4522(2) 0.4746(7) 0.5037(6) 0.060(2) Uani 1 d . . H16 H 0.4529(2) 0.4624(7) 0.4488(6) 0.072 Uiso 1 calc R . C17 C 0.4683(2) 0.5686(8) 0.5460(7) 0.077(3) Uani 1 d . . H17 H 0.4802(2) 0.6199(8) 0.5198(7) 0.092 Uiso 1 calc R . C18 C 0.4674(2) 0.5885(8) 0.6251(7) 0.077(3) Uani 1 d . . H18 H 0.4787(2) 0.6530(8) 0.6537(7) 0.093 Uiso 1 calc R . C19 C 0.4503(2) 0.5150(9) 0.6623(6) 0.078(3) Uani 1 d . . H19 H 0.4498(2) 0.5282(9) 0.7173(6) 0.094 Uiso 1 calc R . C20 C 0.4338(2) 0.4218(8) 0.6209(5) 0.065(3) Uani 1 d . . H20 H 0.4215(2) 0.3727(8) 0.6474(5) 0.078 Uiso 1 calc R . C21 C 0.4452(2) 0.2142(7) 0.4423(5) 0.048(2) Uani 1 d . . C22 C 0.4763(2) 0.1812(7) 0.4951(6) 0.062(2) Uani 1 d . . H22 H 0.4804(2) 0.1926(7) 0.5524(6) 0.075 Uiso 1 calc R . C23 C 0.5021(2) 0.1301(8) 0.4638(7) 0.073(3) Uani 1 d . . H23 H 0.5235(2) 0.1073(8) 0.5003(7) 0.087 Uiso 1 calc R . C24 C 0.4965(3) 0.1138(8) 0.3831(8) 0.086(4) Uani 1 d . . H24 H 0.5141(3) 0.0796(8) 0.3627(8) 0.103 Uiso 1 calc R . C25 C 0.4655(3) 0.1463(9) 0.3296(7) 0.086(3) Uani 1 d . . H25 H 0.4617(3) 0.1339(9) 0.2725(7) 0.104 Uiso 1 calc R . C26 C 0.4397(2) 0.1972(8) 0.3588(6) 0.069(3) Uani 1 d . . H26 H 0.4184(2) 0.2201(8) 0.3216(6) 0.083 Uiso 1 calc R . C27 C 0.3697(2) 0.1961(6) 0.6714(4) 0.040(2) Uani 1 d . . C28 C 0.3431(2) 0.2683(7) 0.6763(4) 0.047(2) Uani 1 d . . H28 H 0.3257(2) 0.2881(7) 0.6280(4) 0.056 Uiso 1 calc R . C29 C 0.3417(2) 0.3122(8) 0.7521(5) 0.061(2) Uani 1 d . . H29 H 0.3237(2) 0.3631(8) 0.7553(5) 0.073 Uiso 1 calc R . C30 C 0.3667(3) 0.2808(9) 0.8224(5) 0.076(3) Uani 1 d . . H30 H 0.3655(3) 0.3095(9) 0.8739(5) 0.091 Uiso 1 calc R . C31 C 0.3933(3) 0.2092(9) 0.8191(5) 0.089(3) Uani 1 d . . H31 H 0.4105(3) 0.1891(9) 0.8678(5) 0.107 Uiso 1 calc R . C32 C 0.3948(2) 0.1666(8) 0.7442(5) 0.068(3) Uani 1 d . . H32 H 0.4130(2) 0.1164(8) 0.7418(5) 0.081 Uiso 1 calc R . C33 C 0.3808(2) -0.0075(6) 0.5929(4) 0.040(2) Uani 1 d . . C34 C 0.4004(2) -0.0666(7) 0.5487(4) 0.048(2) Uani 1 d . . H34 H 0.4114(2) -0.0267(7) 0.5140(4) 0.058 Uiso 1 calc R . C35 C 0.4036(2) -0.1822(8) 0.5553(5) 0.055(2) Uani 1 d . . H35 H 0.4170(2) -0.2212(8) 0.5253(5) 0.066 Uiso 1 calc R . C36 C 0.3876(2) -0.2424(8) 0.6053(5) 0.059(2) Uani 1 d . . H36 H 0.3897(2) -0.3222(8) 0.6093(5) 0.071 Uiso 1 calc R . C37 C 0.3684(2) -0.1841(7) 0.6495(5) 0.055(2) Uani 1 d . . H37 H 0.3574(2) -0.2249(7) 0.6839(5) 0.066 Uiso 1 calc R . C38 C 0.36507(13) -0.0712(4) 0.6446(3) 0.046(2) Uani 1 d . . H38 H 0.35206(13) -0.0335(4) 0.6761(3) 0.055 Uiso 1 calc R . Cl2 Cl 0.49999(13) 0.1317(4) 0.7501(3) 0.175(2) Uiso 1 d SR . Cl3 Cl 0.52654(13) 0.3118(4) 0.6713(3) 0.255(3) Uiso 1 d R . C39 C 0.49999(13) 0.2497(4) 0.7501(3) 0.239(14) Uiso 1 d SR . 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 Pd 0.0355(3) 0.0377(3) 0.0333(3) 0.0034(3) 0.0157(2) 0.0031(3) Fe 0.0441(6) 0.0544(8) 0.0424(6) 0.0104(6) 0.0216(5) 0.0018(6) Cl1 0.0439(10) 0.0413(11) 0.0350(10) 0.0027(8) 0.0115(8) 0.0060(8) P1 0.0388(11) 0.0446(13) 0.0504(12) 0.0039(9) 0.0249(10) -0.0010(9) P2 0.0341(10) 0.0427(13) 0.0388(11) 0.0038(9) 0.0165(9) 0.0035(9) N1 0.035(3) 0.037(4) 0.026(3) 0.003(3) 0.013(3) -0.005(3) N2 0.021(3) 0.057(4) 0.049(3) 0.019(3) 0.010(2) 0.002(3) O1 0.091(5) 0.109(6) 0.108(5) 0.048(5) 0.060(4) 0.000(4) O2 0.064(4) 0.057(4) 0.068(4) 0.002(3) 0.029(3) 0.013(3) O3 0.068(4) 0.074(5) 0.066(4) -0.023(3) 0.038(3) -0.013(4) O4 0.069(4) 0.115(6) 0.059(4) 0.044(4) 0.020(3) 0.012(4) C1 0.056(5) 0.072(7) 0.063(6) 0.022(5) 0.031(5) 0.006(5) C2 0.041(5) 0.052(6) 0.053(5) 0.009(4) 0.015(4) 0.010(4) C3 0.046(5) 0.074(7) 0.036(4) 0.000(5) 0.018(3) -0.004(5) C4 0.067(6) 0.068(6) 0.049(5) 0.027(4) 0.035(5) -0.003(5) C5 0.035(4) 0.039(5) 0.030(4) 0.001(3) 0.005(3) 0.010(3) C6 0.042(4) 0.040(5) 0.050(5) -0.005(4) 0.017(4) 0.001(4) C7 0.042(4) 0.032(4) 0.037(4) 0.005(3) 0.019(3) 0.001(3) C8 0.042(4) 0.034(5) 0.039(4) 0.002(3) 0.013(4) 0.004(4) C9 0.044(5) 0.056(5) 0.040(4) -0.002(4) 0.009(4) -0.004(4) C10 0.044(5) 0.041(5) 0.052(5) -0.004(4) 0.016(4) -0.006(4) C11 0.066(5) 0.037(5) 0.057(5) 0.005(4) 0.027(4) -0.010(5) C12 0.063(5) 0.048(5) 0.044(5) 0.012(4) 0.026(4) 0.006(4) C13 0.040(4) 0.038(5) 0.037(4) 0.005(3) 0.016(3) 0.003(4) C14 0.048(5) 0.068(6) 0.035(4) 0.003(4) 0.019(4) 0.002(4) C15 0.036(4) 0.042(5) 0.054(5) -0.006(4) 0.016(4) 0.000(4) C16 0.055(5) 0.047(6) 0.090(7) 0.003(5) 0.039(5) -0.009(5) C17 0.063(6) 0.051(7) 0.128(9) -0.003(6) 0.044(6) -0.005(5) C18 0.056(6) 0.053(7) 0.126(9) -0.025(6) 0.031(6) -0.001(5) C19 0.067(6) 0.081(8) 0.092(8) -0.026(6) 0.030(6) -0.012(6) C20 0.052(5) 0.076(7) 0.071(6) -0.014(5) 0.023(5) -0.016(5) C21 0.037(4) 0.049(6) 0.066(5) -0.001(4) 0.027(4) -0.004(4) C22 0.052(5) 0.052(6) 0.098(7) 0.006(5) 0.045(5) 0.003(5) C23 0.057(6) 0.057(6) 0.120(9) 0.015(6) 0.053(6) 0.005(5) C24 0.082(8) 0.060(7) 0.149(11) 0.007(7) 0.086(8) 0.005(6) C25 0.090(8) 0.097(9) 0.100(8) -0.033(6) 0.072(7) -0.008(7) C26 0.066(6) 0.079(7) 0.076(6) -0.002(5) 0.045(5) 0.006(5) C27 0.041(4) 0.043(5) 0.038(4) -0.007(4) 0.014(3) 0.003(4) C28 0.050(5) 0.056(5) 0.036(4) -0.007(4) 0.015(4) 0.002(4) C29 0.061(5) 0.064(6) 0.063(6) -0.011(5) 0.024(4) 0.006(5) C30 0.096(7) 0.087(8) 0.042(5) -0.015(5) 0.011(5) 0.014(6) C31 0.104(8) 0.106(9) 0.046(5) -0.015(6) 0.001(5) 0.040(7) C32 0.074(6) 0.076(7) 0.052(5) -0.015(5) 0.015(5) 0.013(5) C33 0.036(4) 0.048(5) 0.038(4) 0.009(4) 0.012(3) 0.013(4) C34 0.047(5) 0.053(6) 0.047(5) 0.008(4) 0.017(4) 0.015(4) C35 0.060(5) 0.051(6) 0.060(5) 0.005(5) 0.028(4) 0.016(5) C36 0.066(6) 0.047(6) 0.065(6) 0.004(4) 0.017(5) 0.012(5) C37 0.066(5) 0.047(5) 0.054(5) 0.015(4) 0.021(4) 0.002(5) C38 0.056(5) 0.049(6) 0.038(4) 0.008(4) 0.023(4) 0.008(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd C5 1.978(7) . ? Pd P2 2.274(2) . ? Pd Cl1 2.402(2) . ? Pd C3 2.578(7) . ? Pd Fe 2.7356(12) . ? Fe C1 1.758(8) . ? Fe C2 1.785(9) . ? Fe C3 1.795(10) . ? Fe C4 1.806(10) . ? Fe P1 2.271(2) . ? P1 N2 1.595(6) . ? P1 C15 1.820(8) . ? P1 C21 1.843(7) . ? P2 N2 1.605(5) . ? P2 C33 1.811(8) . ? P2 C27 1.814(7) . ? N1 C5 1.319(8) . ? N1 C7 1.457(8) . ? O1 C1 1.179(9) . ? O2 C2 1.162(9) . ? O3 C3 1.162(9) . ? O4 C4 1.158(9) . ? C5 C6 1.491(9) . ? C7 C8 1.403(9) . ? C7 C13 1.407(9) . ? C8 C10 1.399(9) . ? C8 C9 1.527(9) . ? C10 C11 1.361(10) . ? C11 C12 1.384(10) . ? C12 C13 1.380(10) . ? C13 C14 1.505(10) . ? C15 C20 1.388(10) . ? C15 C16 1.395(10) . ? C16 C17 1.386(12) . ? C17 C18 1.370(13) . ? C18 C19 1.362(13) . ? C19 C20 1.378(12) . ? C21 C22 1.377(11) . ? C21 C26 1.386(11) . ? C22 C23 1.415(11) . ? C23 C24 1.339(13) . ? C24 C25 1.378(14) . ? C25 C26 1.396(11) . ? C27 C28 1.383(9) . ? C27 C32 1.407(10) . ? C28 C29 1.400(10) . ? C29 C30 1.384(11) . ? C30 C31 1.372(12) . ? C31 C32 1.381(11) . ? C33 C34 1.406(9) . ? C33 C38 1.423(8) . ? C34 C35 1.378(11) . ? C35 C36 1.388(11) . ? C36 C37 1.389(11) . ? C37 C38 1.346(9) . ? Cl2 C39 1.40 . ? Cl3 C39 2.05 . ? C39 Cl3 2.048(9) 2_656 ? 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 C5 Pd P2 90.8(2) . . ? C5 Pd Cl1 84.0(2) . . ? P2 Pd Cl1 171.75(6) . . ? C5 Pd C3 125.2(3) . . ? P2 Pd C3 89.6(2) . . ? Cl1 Pd C3 98.7(2) . . ? C5 Pd Fe 164.4(2) . . ? P2 Pd Fe 91.27(5) . . ? Cl1 Pd Fe 95.46(5) . . ? C3 Pd Fe 39.4(2) . . ? C1 Fe C2 110.5(4) . . ? C1 Fe C3 112.5(4) . . ? C2 Fe C3 136.0(3) . . ? C1 Fe C4 87.6(4) . . ? C2 Fe C4 95.4(4) . . ? C3 Fe C4 95.4(4) . . ? C1 Fe P1 88.7(3) . . ? C2 Fe P1 85.5(2) . . ? C3 Fe P1 86.5(3) . . ? C4 Fe P1 176.3(2) . . ? C1 Fe Pd 177.9(3) . . ? C2 Fe Pd 71.6(3) . . ? C3 Fe Pd 65.6(2) . . ? C4 Fe Pd 91.9(2) . . ? P1 Fe Pd 91.86(6) . . ? N2 P1 C15 105.7(3) . . ? N2 P1 C21 106.1(3) . . ? C15 P1 C21 101.9(3) . . ? N2 P1 Fe 114.8(2) . . ? C15 P1 Fe 112.5(3) . . ? C21 P1 Fe 114.7(3) . . ? N2 P2 C33 105.4(3) . . ? N2 P2 C27 109.0(3) . . ? C33 P2 C27 103.5(3) . . ? N2 P2 Pd 114.9(2) . . ? C33 P2 Pd 115.0(2) . . ? C27 P2 Pd 108.3(2) . . ? C5 N1 C7 127.0(6) . . ? P1 N2 P2 126.8(3) . . ? O1 C1 Fe 178.1(8) . . ? O2 C2 Fe 176.1(7) . . ? O3 C3 Fe 174.8(6) . . ? O3 C3 Pd 110.1(6) . . ? Fe C3 Pd 75.1(3) . . ? O4 C4 Fe 174.7(7) . . ? N1 C5 C6 118.3(6) . . ? N1 C5 Pd 124.6(5) . . ? C6 C5 Pd 116.4(5) . . ? C8 C7 C13 122.5(6) . . ? C8 C7 N1 121.6(6) . . ? C13 C7 N1 115.9(6) . . ? C10 C8 C7 117.5(6) . . ? C10 C8 C9 119.2(6) . . ? C7 C8 C9 123.3(6) . . ? C11 C10 C8 120.5(7) . . ? C10 C11 C12 121.1(7) . . ? C13 C12 C11 121.4(7) . . ? C12 C13 C7 116.9(7) . . ? C12 C13 C14 121.0(6) . . ? C7 C13 C14 122.0(6) . . ? C20 C15 C16 117.3(8) . . ? C20 C15 P1 120.2(6) . . ? C16 C15 P1 122.4(6) . . ? C17 C16 C15 120.4(9) . . ? C18 C17 C16 120.8(9) . . ? C19 C18 C17 119.4(9) . . ? C18 C19 C20 120.5(10) . . ? C19 C20 C15 121.5(9) . . ? C22 C21 C26 119.4(7) . . ? C22 C21 P1 117.1(6) . . ? C26 C21 P1 123.4(6) . . ? C21 C22 C23 119.8(9) . . ? C24 C23 C22 120.6(10) . . ? C23 C24 C25 120.2(9) . . ? C24 C25 C26 120.5(10) . . ? C21 C26 C25 119.6(9) . . ? C28 C27 C32 118.6(7) . . ? C28 C27 P2 121.9(5) . . ? C32 C27 P2 119.5(5) . . ? C27 C28 C29 120.4(7) . . ? C30 C29 C28 119.4(8) . . ? C29 C30 C31 121.3(8) . . ? C32 C31 C30 119.2(9) . . ? C31 C32 C27 121.2(8) . . ? C34 C33 C38 117.6(6) . . ? C34 C33 P2 118.6(5) . . ? C38 C33 P2 123.5(5) . . ? C35 C34 C33 120.4(7) . . ? C34 C35 C36 120.8(7) . . ? C35 C36 C37 119.0(8) . . ? C38 C37 C36 121.4(7) . . ? C37 C38 C33 120.8(6) . . ? Cl2 C39 Cl3 111.07(10) . 2_656 ? Cl2 C39 Cl3 111.0 . . ? Cl3 C39 Cl3 137.90(10) 2_656 . ? _refine_diff_density_max 1.318 _refine_diff_density_min -1.307 _refine_diff_density_rms 0.125 data_5a _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C33 H31 B Cl2 F4 Fe N O5 P2 Pd' _chemical_formula_weight 903.49 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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 12.468(2) _cell_length_b 14.540(3) _cell_length_c 20.969(4) _cell_angle_alpha 90.00 _cell_angle_beta 103.40(3) _cell_angle_gamma 90.00 _cell_volume 3697.9(12) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.623 _exptl_crystal_density_method ? _exptl_crystal_F_000 1812 _exptl_absorpt_coefficient_mu 1.170 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Stoe IPDS ' _diffrn_measurement_method 'image plate' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29287 _diffrn_reflns_av_R_equivalents 0.0607 _diffrn_reflns_av_sigmaI/netI 0.0632 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.24 _diffrn_reflns_theta_max 26.00 _reflns_number_total 7202 _reflns_number_observed 4531 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 1 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0899P)^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 'geom, riding model' _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0033(4) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 7201 _refine_ls_number_parameters 457 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0881 _refine_ls_R_factor_obs 0.0573 _refine_ls_wR_factor_all 0.1518 _refine_ls_wR_factor_obs 0.1404 _refine_ls_goodness_of_fit_all 1.001 _refine_ls_goodness_of_fit_obs 1.187 _refine_ls_restrained_S_all 1.002 _refine_ls_restrained_S_obs 1.187 _refine_ls_shift/esd_max -0.050 _refine_ls_shift/esd_mean 0.002 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Pd Pd 0.88617(4) 0.12415(3) 0.18868(2) 0.0415(2) Uani 1 d . . Fe Fe 1.08639(6) 0.20077(5) 0.19176(4) 0.0407(2) Uani 1 d . . P1 P 1.07718(11) 0.28445(9) 0.28003(7) 0.0394(3) Uani 1 d . . P2 P 0.87108(11) 0.18054(8) 0.28285(7) 0.0372(3) Uani 1 d . . N N 0.9823(4) 0.2433(3) 0.3173(3) 0.0417(11) Uani 1 d . . H1 H 0.9871(46) 0.2634(37) 0.3447(26) 0.027(17) Uiso 1 d . . O1 O 0.8968(3) 0.3005(2) 0.1096(2) 0.0518(10) Uani 1 d . . O2 O 1.2939(4) 0.2926(3) 0.1871(2) 0.0675(12) Uani 1 d . . O3 O 1.1001(5) 0.0927(4) 0.0754(3) 0.082(2) Uani 1 d . . O4 O 1.1372(4) 0.0344(3) 0.2741(2) 0.0617(11) Uani 1 d . . O5 O 0.8646(4) 0.0640(3) 0.0939(2) 0.0607(11) Uani 1 d . . C1 C 0.9660(5) 0.2586(3) 0.1446(3) 0.0457(13) Uani 1 d . . C2 C 1.2129(5) 0.2580(4) 0.1901(3) 0.0529(15) Uani 1 d . . C3 C 1.0940(5) 0.1336(4) 0.1216(3) 0.056(2) Uani 1 d . . C4 C 1.1148(5) 0.0998(4) 0.2431(3) 0.0475(14) Uani 1 d . . C5 C 0.7456(5) 0.0500(4) 0.1877(3) 0.0467(13) Uani 1 d . . H5A H 0.7640(5) -0.0096(4) 0.2104(3) 0.056 Uiso 1 calc R . H5B H 0.6960(5) 0.0846(4) 0.2097(3) 0.056 Uiso 1 calc R . C6 C 0.6905(5) 0.0348(4) 0.1150(3) 0.0501(14) Uani 1 d . . H6A H 0.6507(5) -0.0246(4) 0.1104(3) 0.060 Uiso 1 calc R . H6B H 0.6354(5) 0.0840(4) 0.1004(3) 0.060 Uiso 1 calc R . C7 C 0.7685(6) 0.0343(4) 0.0721(3) 0.059(2) Uani 1 d . . C8 C 0.7311(7) 0.0022(5) 0.0026(4) 0.086(2) Uani 1 d . . H8A H 0.6710(32) 0.0417(24) -0.0208(8) 0.129 Uiso 1 calc R . H8B H 0.7049(44) -0.0614(14) 0.0020(4) 0.129 Uiso 1 calc R . H8C H 0.7928(14) 0.0054(37) -0.0190(9) 0.129 Uiso 1 calc R . C9 C 1.0555(4) 0.4079(3) 0.2655(3) 0.0411(12) Uani 1 d . . C10 C 1.0413(5) 0.4640(4) 0.3176(3) 0.0514(14) Uani 1 d . . H10 H 1.0346(5) 0.4372(4) 0.3578(3) 0.062 Uiso 1 calc R . C11 C 1.0373(5) 0.5596(4) 0.3098(4) 0.063(2) Uani 1 d . . H11 H 1.0265(5) 0.5977(4) 0.3445(4) 0.075 Uiso 1 calc R . C12 C 1.0488(5) 0.5986(4) 0.2518(4) 0.061(2) Uani 1 d . . H12 H 1.0474(5) 0.6636(4) 0.2472(4) 0.073 Uiso 1 calc R . C13 C 1.0625(5) 0.5441(4) 0.2006(3) 0.056(2) Uani 1 d . . H13 H 1.0697(5) 0.5714(4) 0.1607(3) 0.067 Uiso 1 calc R . C14 C 1.0655(5) 0.4487(4) 0.2075(3) 0.0485(13) Uani 1 d . . H14 H 1.0746(5) 0.4113(4) 0.1719(3) 0.058 Uiso 1 calc R . C15 C 1.2014(5) 0.2848(4) 0.3448(3) 0.0464(13) Uani 1 d . . C16 C 1.2835(5) 0.3522(4) 0.3456(3) 0.056(2) Uani 1 d . . H16 H 1.2741(5) 0.3970(4) 0.3118(3) 0.067 Uiso 1 calc R . C17 C 1.3774(5) 0.3525(5) 0.3958(4) 0.069(2) Uani 1 d . . H17 H 1.4331(5) 0.3971(5) 0.3959(4) 0.083 Uiso 1 calc R . C18 C 1.3914(6) 0.2897(6) 0.4453(4) 0.078(2) Uani 1 d . . H18 H 1.4552(6) 0.2924(6) 0.4802(4) 0.094 Uiso 1 calc R . C19 C 1.3137(6) 0.2226(6) 0.4449(4) 0.086(2) Uani 1 d . . H19 H 1.3252(6) 0.1777(6) 0.4787(4) 0.104 Uiso 1 calc R . C20 C 1.2181(6) 0.2206(5) 0.3949(3) 0.069(2) Uani 1 d . . H20 H 1.1639(6) 0.1747(5) 0.3951(3) 0.083 Uiso 1 calc R . C21 C 0.7514(4) 0.2521(3) 0.2797(3) 0.0374(11) Uani 1 d . . C22 C 0.7258(5) 0.2806(3) 0.3377(3) 0.0472(13) Uani 1 d . . H22 H 0.7737(5) 0.2661(3) 0.3788(3) 0.057 Uiso 1 calc R . C23 C 0.6304(5) 0.3300(4) 0.3355(3) 0.055(2) Uani 1 d . . H23 H 0.6131(5) 0.3493(4) 0.3752(3) 0.066 Uiso 1 calc R . C24 C 0.5602(5) 0.3516(4) 0.2767(3) 0.054(2) Uani 1 d . . H24 H 0.4945(5) 0.3850(4) 0.2759(3) 0.065 Uiso 1 calc R . C25 C 0.5851(5) 0.3249(4) 0.2194(3) 0.054(2) Uani 1 d . . H25 H 0.5367(5) 0.3405(4) 0.1788(3) 0.065 Uiso 1 calc R . C26 C 0.6806(5) 0.2750(4) 0.2199(3) 0.0481(13) Uani 1 d . . H26 H 0.6976(5) 0.2567(4) 0.1798(3) 0.058 Uiso 1 calc R . C27 C 0.8596(4) 0.0921(3) 0.3419(3) 0.0375(11) Uani 1 d . . H27 H 0.8662(4) 0.1424(3) 0.3141(3) 0.045 Uiso 1 calc R . C28 C 0.7559(5) 0.0619(3) 0.3476(3) 0.0438(12) Uani 1 d . . H28 H 0.6912(5) 0.0919(3) 0.3239(3) 0.053 Uiso 1 calc R . C29 C 0.7477(5) -0.0118(4) 0.3880(3) 0.0518(14) Uani 1 d . . H29 H 0.6769(5) -0.0319(4) 0.3917(3) 0.062 Uiso 1 calc R . C30 C 0.8397(6) -0.0562(4) 0.4226(3) 0.0523(15) Uani 1 d . . H30 H 0.8329(6) -0.1071(4) 0.4498(3) 0.063 Uiso 1 calc R . C31 C 0.9418(5) -0.0265(4) 0.4175(3) 0.0506(14) Uani 1 d . . H31 H 1.0058(5) -0.0569(4) 0.4418(3) 0.061 Uiso 1 calc R . C32 C 0.9537(5) 0.0469(4) 0.3777(3) 0.0450(13) Uani 1 d . . H32 H 1.0250(5) 0.0664(4) 0.3747(3) 0.054 Uiso 1 calc R . C33 C -0.2592(8) 0.6296(5) -0.0278(4) 0.091(3) Uani 1 d . . H33A H -0.3102(8) 0.6714(5) -0.0577(4) 0.109 Uiso 1 calc R . H33B H -0.2956(8) 0.6111(5) 0.0075(4) 0.109 Uiso 1 calc R . F1 F 0.9694(5) 0.2066(4) 0.4731(3) 0.126(2) Uani 1 d . . F2 F 0.9889(4) 0.3474(4) 0.4475(3) 0.113(2) Uani 1 d . . F3 F 1.1105(6) 0.2802(4) 0.5302(3) 0.141(2) Uani 1 d . . F4 F 0.9479(7) 0.3161(4) 0.5432(3) 0.148(3) Uani 1 d . . B B 0.9999(8) 0.2884(5) 0.4994(4) 0.064(2) Uani 1 d . . Cl1 Cl -0.2401(3) 0.5324(2) -0.07132(13) 0.1156(9) Uani 1 d . . Cl2 Cl -0.1442(4) 0.6883(3) 0.0060(2) 0.196(2) Uani 1 d . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd 0.0380(3) 0.0377(2) 0.0517(3) -0.0032(2) 0.0161(2) -0.0009(2) Fe 0.0347(5) 0.0358(4) 0.0548(5) 0.0027(3) 0.0167(4) 0.0066(3) P1 0.0310(8) 0.0350(6) 0.0533(8) 0.0016(6) 0.0120(6) 0.0019(5) P2 0.0314(8) 0.0335(6) 0.0476(8) 0.0032(6) 0.0114(6) 0.0012(5) N 0.041(3) 0.042(3) 0.044(3) -0.010(2) 0.013(2) -0.005(2) O1 0.053(3) 0.043(2) 0.056(2) 0.003(2) 0.005(2) 0.010(2) O2 0.044(3) 0.078(3) 0.086(3) 0.012(2) 0.026(2) -0.007(2) O3 0.087(4) 0.085(3) 0.089(4) -0.024(3) 0.048(3) 0.014(3) O4 0.062(3) 0.041(2) 0.086(3) 0.012(2) 0.023(2) 0.009(2) O5 0.058(3) 0.060(2) 0.074(3) -0.015(2) 0.034(2) -0.012(2) C1 0.052(4) 0.035(3) 0.056(3) -0.009(2) 0.024(3) 0.000(2) C2 0.048(4) 0.048(3) 0.065(4) 0.012(3) 0.018(3) 0.012(3) C3 0.046(4) 0.052(3) 0.076(4) 0.001(3) 0.029(3) 0.004(3) C4 0.040(3) 0.045(3) 0.063(4) -0.008(3) 0.021(3) 0.002(2) C5 0.048(4) 0.041(3) 0.053(3) -0.004(2) 0.016(3) -0.001(2) C6 0.046(4) 0.047(3) 0.057(3) -0.009(3) 0.011(3) -0.006(3) C7 0.067(5) 0.048(3) 0.067(4) -0.014(3) 0.025(3) -0.003(3) C8 0.096(6) 0.094(5) 0.080(5) -0.041(4) 0.044(5) -0.024(4) C9 0.029(3) 0.036(3) 0.058(3) -0.005(2) 0.009(2) -0.006(2) C10 0.044(4) 0.045(3) 0.069(4) -0.007(3) 0.020(3) 0.003(3) C11 0.043(4) 0.044(3) 0.104(5) -0.018(3) 0.022(4) 0.002(3) C12 0.036(4) 0.038(3) 0.107(6) 0.002(3) 0.013(3) 0.000(2) C13 0.051(4) 0.038(3) 0.076(4) 0.009(3) 0.010(3) 0.000(3) C14 0.040(3) 0.040(3) 0.064(4) 0.002(3) 0.008(3) -0.002(2) C15 0.032(3) 0.047(3) 0.062(4) -0.007(3) 0.014(3) 0.002(2) C16 0.029(3) 0.057(3) 0.084(4) -0.003(3) 0.016(3) -0.004(3) C17 0.033(4) 0.082(5) 0.091(5) -0.019(4) 0.015(3) -0.003(3) C18 0.044(5) 0.109(6) 0.071(5) -0.018(5) -0.006(3) 0.009(4) C19 0.051(5) 0.117(6) 0.076(5) 0.024(5) -0.013(4) -0.008(4) C20 0.053(5) 0.071(4) 0.074(5) 0.010(4) -0.003(3) -0.004(3) C21 0.031(3) 0.031(2) 0.050(3) 0.006(2) 0.008(2) -0.001(2) C22 0.043(4) 0.041(3) 0.061(4) -0.002(2) 0.019(3) 0.003(2) C23 0.048(4) 0.047(3) 0.077(4) -0.004(3) 0.027(3) 0.010(3) C24 0.041(4) 0.037(3) 0.087(5) 0.006(3) 0.020(3) 0.011(2) C25 0.039(4) 0.046(3) 0.075(4) 0.024(3) 0.009(3) 0.006(2) C26 0.042(4) 0.043(3) 0.059(3) 0.013(3) 0.011(3) 0.000(2) C27 0.039(3) 0.030(2) 0.045(3) 0.003(2) 0.011(2) 0.003(2) C28 0.041(3) 0.038(3) 0.053(3) 0.005(2) 0.012(3) -0.002(2) C29 0.055(4) 0.040(3) 0.062(4) 0.002(3) 0.016(3) -0.009(3) C30 0.072(5) 0.037(3) 0.051(3) 0.007(2) 0.020(3) 0.003(3) C31 0.062(4) 0.037(3) 0.051(3) 0.008(2) 0.009(3) 0.012(3) C32 0.040(3) 0.045(3) 0.048(3) 0.002(2) 0.005(2) 0.003(2) C33 0.111(7) 0.083(5) 0.080(5) -0.009(4) 0.022(5) -0.038(5) F1 0.165(6) 0.093(4) 0.107(4) -0.042(3) 0.006(4) 0.004(3) F2 0.114(4) 0.112(4) 0.118(4) 0.063(3) 0.034(3) 0.024(3) F3 0.143(6) 0.098(4) 0.147(5) -0.005(3) -0.038(4) 0.032(4) F4 0.224(8) 0.141(5) 0.106(4) -0.032(4) 0.093(5) -0.002(5) B 0.086(7) 0.043(4) 0.061(5) 0.007(3) 0.011(4) 0.005(4) Cl1 0.141(2) 0.109(2) 0.108(2) -0.0280(14) 0.053(2) -0.034(2) Cl2 0.205(4) 0.247(4) 0.149(3) -0.079(3) 0.064(3) -0.168(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd C5 2.054(6) . ? Pd O5 2.130(4) . ? Pd P2 2.1861(14) . ? Pd C1 2.468(5) . ? Pd Fe 2.7208(9) . ? Fe C3 1.786(6) . ? Fe C2 1.791(7) . ? Fe C1 1.802(6) . ? Fe C4 1.806(6) . ? Fe P1 2.240(2) . ? P1 N 1.673(5) . ? P1 C15 1.807(6) . ? P1 C9 1.830(5) . ? P2 N 1.677(5) . ? P2 C21 1.808(5) . ? P2 C27 1.813(5) . ? O1 C1 1.167(7) . ? O2 C2 1.143(7) . ? O3 C3 1.155(7) . ? O4 C4 1.149(6) . ? O5 C7 1.256(8) . ? C5 C6 1.534(8) . ? C6 C7 1.472(8) . ? C7 C8 1.498(9) . ? C9 C14 1.387(8) . ? C9 C10 1.406(7) . ? C10 C11 1.399(8) . ? C11 C12 1.378(9) . ? C12 C13 1.377(9) . ? C13 C14 1.394(7) . ? C15 C20 1.384(8) . ? C15 C16 1.414(8) . ? C16 C17 1.382(10) . ? C17 C18 1.361(10) . ? C18 C19 1.374(11) . ? C19 C20 1.394(9) . ? C21 C22 1.390(7) . ? C21 C26 1.397(7) . ? C22 C23 1.380(8) . ? C23 C24 1.372(9) . ? C24 C25 1.365(9) . ? C25 C26 1.393(8) . ? C27 C28 1.396(7) . ? C27 C32 1.402(7) . ? C28 C29 1.384(7) . ? C29 C30 1.369(8) . ? C30 C31 1.373(9) . ? C31 C32 1.382(7) . ? C33 Cl2 1.679(8) . ? C33 Cl1 1.727(9) . ? F1 B 1.329(9) . ? F2 B 1.368(8) . ? F3 B 1.385(10) . ? F4 B 1.304(9) . ? 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 C5 Pd O5 81.5(2) . . ? C5 Pd P2 87.4(2) . . ? O5 Pd P2 167.93(12) . . ? C5 Pd C1 146.0(2) . . ? O5 Pd C1 87.2(2) . . ? P2 Pd C1 99.65(13) . . ? C5 Pd Fe 172.5(2) . . ? O5 Pd Fe 96.13(12) . . ? P2 Pd Fe 95.48(5) . . ? C1 Pd Fe 40.28(15) . . ? C3 Fe C2 91.3(3) . . ? C3 Fe C1 90.0(3) . . ? C2 Fe C1 113.4(3) . . ? C3 Fe C4 90.3(3) . . ? C2 Fe C4 109.7(3) . . ? C1 Fe C4 136.8(3) . . ? C3 Fe P1 179.7(2) . . ? C2 Fe P1 88.8(2) . . ? C1 Fe P1 90.2(2) . . ? C4 Fe P1 89.4(2) . . ? C3 Fe Pd 88.9(2) . . ? C2 Fe Pd 175.7(2) . . ? C1 Fe Pd 62.3(2) . . ? C4 Fe Pd 74.5(2) . . ? P1 Fe Pd 91.12(5) . . ? N P1 C15 103.0(3) . . ? N P1 C9 109.6(2) . . ? C15 P1 C9 101.0(2) . . ? N P1 Fe 111.7(2) . . ? C15 P1 Fe 115.0(2) . . ? C9 P1 Fe 115.4(2) . . ? N P2 C21 107.2(2) . . ? N P2 C27 106.2(3) . . ? C21 P2 C27 103.7(2) . . ? N P2 Pd 111.0(2) . . ? C21 P2 Pd 115.2(2) . . ? C27 P2 Pd 112.8(2) . . ? P1 N P2 126.6(3) . . ? C7 O5 Pd 112.7(4) . . ? O1 C1 Fe 171.5(5) . . ? O1 C1 Pd 110.2(4) . . ? Fe C1 Pd 77.4(2) . . ? O2 C2 Fe 177.6(6) . . ? O3 C3 Fe 177.7(5) . . ? O4 C4 Fe 176.5(5) . . ? C6 C5 Pd 105.7(4) . . ? C7 C6 C5 113.7(5) . . ? O5 C7 C6 119.0(5) . . ? O5 C7 C8 121.2(6) . . ? C6 C7 C8 119.7(6) . . ? C14 C9 C10 119.1(5) . . ? C14 C9 P1 121.7(4) . . ? C10 C9 P1 118.7(4) . . ? C11 C10 C9 119.6(6) . . ? C12 C11 C10 120.2(6) . . ? C13 C12 C11 120.5(5) . . ? C12 C13 C14 119.9(6) . . ? C9 C14 C13 120.7(6) . . ? C20 C15 C16 118.4(6) . . ? C20 C15 P1 121.3(4) . . ? C16 C15 P1 120.2(5) . . ? C17 C16 C15 119.7(6) . . ? C18 C17 C16 121.0(7) . . ? C17 C18 C19 120.4(7) . . ? C18 C19 C20 119.9(7) . . ? C15 C20 C19 120.6(7) . . ? C22 C21 C26 119.3(5) . . ? C22 C21 P2 119.7(4) . . ? C26 C21 P2 120.9(4) . . ? C23 C22 C21 119.7(6) . . ? C24 C23 C22 121.0(6) . . ? C25 C24 C23 119.9(5) . . ? C24 C25 C26 120.7(6) . . ? C25 C26 C21 119.4(6) . . ? C28 C27 C32 118.9(5) . . ? C28 C27 P2 120.2(4) . . ? C32 C27 P2 120.7(4) . . ? C29 C28 C27 119.8(5) . . ? C30 C29 C28 121.2(6) . . ? C29 C30 C31 119.2(5) . . ? C30 C31 C32 121.4(5) . . ? C31 C32 C27 119.5(5) . . ? Cl2 C33 Cl1 115.5(6) . . ? F4 B F1 115.3(8) . . ? F4 B F2 113.1(7) . . ? F1 B F2 105.3(7) . . ? F4 B F3 107.6(8) . . ? F1 B F3 106.0(6) . . ? F2 B F3 109.2(7) . . ? _refine_diff_density_max 0.862 _refine_diff_density_min -0.910 _refine_diff_density_rms 0.111 data_1b _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C30 H25 Cl Fe O4 P2 Pd' _chemical_formula_weight 709.14 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.931(2) _cell_length_b 12.0774(15) _cell_length_c 22.688(3) _cell_angle_alpha 90.00 _cell_angle_beta 98.48(2) _cell_angle_gamma 90.00 _cell_volume 2962.5(7) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.590 _exptl_crystal_density_method ? _exptl_crystal_F_000 1424 _exptl_absorpt_coefficient_mu 1.328 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Stoe IPDS ' _diffrn_measurement_method 'image plate' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24209 _diffrn_reflns_av_R_equivalents 0.0549 _diffrn_reflns_av_sigmaI/netI 0.0394 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.42 _diffrn_reflns_theta_max 26.00 _reflns_number_total 5811 _reflns_number_observed 4643 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 1 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0991P)^2^+8.3220P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment 'riding model' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5810 _refine_ls_number_parameters 353 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0723 _refine_ls_R_factor_obs 0.0599 _refine_ls_wR_factor_all 0.1760 _refine_ls_wR_factor_obs 0.1677 _refine_ls_goodness_of_fit_all 1.110 _refine_ls_goodness_of_fit_obs 1.191 _refine_ls_restrained_S_all 1.110 _refine_ls_restrained_S_obs 1.191 _refine_ls_shift/esd_max 0.004 _refine_ls_shift/esd_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Pd Pd 0.34848(4) 0.95639(4) 0.29976(2) 0.0304(2) Uani 1 d . . Fe Fe 0.42255(6) 1.09972(6) 0.39781(3) 0.0242(2) Uani 1 d . . P1 P 0.26383(13) 1.21675(11) 0.36958(6) 0.0267(3) Uani 1 d . . P2 P 0.18381(12) 1.05671(11) 0.26621(6) 0.0252(3) Uani 1 d . . Cl Cl 0.51842(15) 0.83566(14) 0.32383(8) 0.0476(4) Uani 1 d . . O1 O 0.4907(7) 1.2399(5) 0.5007(3) 0.084(2) Uani 1 d . . O2 O 0.6493(6) 0.9831(6) 0.4392(2) 0.0611(14) Uani 1 d . . O3 O 0.5273(4) 1.1538(5) 0.2882(2) 0.0545(13) Uani 1 d . . O4 O 0.2713(4) 0.9038(4) 0.4275(2) 0.0433(10) Uani 1 d . . C1 C 0.4634(7) 1.1867(6) 0.4599(3) 0.049(2) Uani 1 d . . C2 C 0.5692(8) 1.0187(6) 0.4239(3) 0.046(2) Uani 1 d . . C3 C 0.4801(6) 1.1287(6) 0.3291(3) 0.050(2) Uani 1 d . . C4 C 0.3252(6) 0.9785(6) 0.4126(3) 0.0437(15) Uani 1 d . . C5 C 0.2812(6) 0.8462(5) 0.2331(3) 0.047(2) Uani 1 d . . H5A H 0.2978(42) 0.7703(5) 0.2473(8) 0.070 Uiso 1 calc R . H5B H 0.3220(35) 0.8593(28) 0.1981(9) 0.070 Uiso 1 calc R . H5C H 0.1918(10) 0.8567(29) 0.2223(16) 0.070 Uiso 1 calc R . C6 C 0.3077(5) 1.3637(5) 0.3758(2) 0.0333(12) Uani 1 d . . C7 C 0.3620(8) 1.4162(6) 0.3318(3) 0.056(2) Uani 1 d . . H7 H 0.3742(8) 1.3769(6) 0.2968(3) 0.068 Uiso 1 calc R . C9 C 0.3846(8) 1.5828(6) 0.3902(3) 0.059(2) Uani 1 d . . H9 H 0.4089(8) 1.6582(6) 0.3945(3) 0.071 Uiso 1 calc R . C8 C 0.3984(10) 1.5263(7) 0.3389(3) 0.072(3) Uani 1 d . . H8 H 0.4331(10) 1.5627(7) 0.3082(3) 0.087 Uiso 1 calc R . C10 C 0.3360(8) 1.5307(7) 0.4346(4) 0.061(2) Uani 1 d . . H10 H 0.3288(8) 1.5688(7) 0.4705(4) 0.073 Uiso 1 calc R . C11 C 0.2970(7) 1.4217(6) 0.4272(3) 0.048(2) Uani 1 d . . H11 H 0.2621(7) 1.3862(6) 0.4581(3) 0.058 Uiso 1 calc R . C12 C 0.1298(5) 1.2097(5) 0.4091(2) 0.0308(11) Uani 1 d . . C13 C 0.1323(6) 1.1466(5) 0.4606(3) 0.0396(14) Uani 1 d . . H13 H 0.2049(6) 1.1064(5) 0.4757(3) 0.047 Uiso 1 calc R . C14 C 0.0297(7) 1.1417(6) 0.4901(3) 0.048(2) Uani 1 d . . H14 H 0.0319(7) 1.0984(6) 0.5252(3) 0.058 Uiso 1 calc R . C15 C -0.0752(7) 1.2003(6) 0.4680(3) 0.052(2) Uani 1 d . . H15 H -0.1461(7) 1.1958(6) 0.4876(3) 0.062 Uiso 1 calc R . C16 C -0.0786(7) 1.2651(7) 0.4179(3) 0.055(2) Uani 1 d . . H16 H -0.1507(7) 1.3066(7) 0.4036(3) 0.066 Uiso 1 calc R . C17 C 0.0237(6) 1.2695(6) 0.3884(3) 0.0440(15) Uani 1 d . . H17 H 0.0212(6) 1.3140(6) 0.3537(3) 0.053 Uiso 1 calc R . C18 C 0.2013(5) 1.2014(4) 0.2902(2) 0.0266(11) Uani 1 d . . H18A H 0.1197(5) 1.2383(4) 0.2824(2) 0.032 Uiso 1 calc R . H18B H 0.2571(5) 1.2394(4) 0.2661(2) 0.032 Uiso 1 calc R . C19 C 0.0419(5) 1.0083(5) 0.2902(2) 0.0297(11) Uani 1 d . . C20 C -0.0649(6) 1.0715(6) 0.2837(3) 0.045(2) Uani 1 d . . H20 H -0.0667(6) 1.1417(6) 0.2647(3) 0.054 Uiso 1 calc R . C21 C -0.1692(6) 1.0323(7) 0.3050(4) 0.061(2) Uani 1 d . . H21 H -0.2420(6) 1.0762(7) 0.3007(4) 0.074 Uiso 1 calc R . C22 C -0.1683(7) 0.9308(7) 0.3322(4) 0.057(2) Uani 1 d . . H22 H -0.2404(7) 0.9046(7) 0.3465(4) 0.068 Uiso 1 calc R . C23 C -0.0636(6) 0.8670(6) 0.3387(3) 0.045(2) Uani 1 d . . H23 H -0.0630(6) 0.7968(6) 0.3577(3) 0.054 Uiso 1 calc R . C24 C 0.0419(6) 0.9049(5) 0.3177(3) 0.0363(13) Uani 1 d . . H24 H 0.1143(6) 0.8604(5) 0.3220(3) 0.044 Uiso 1 calc R . C25 C 0.1523(5) 1.0736(5) 0.1854(3) 0.0310(12) Uani 1 d . . C26 C 0.0376(6) 1.0539(5) 0.1522(3) 0.0394(14) Uani 1 d . . H26 H -0.0293(6) 1.0295(5) 0.1712(3) 0.047 Uiso 1 calc R . C27 C 0.0205(7) 1.0701(6) 0.0905(3) 0.049(2) Uani 1 d . . H27 H -0.0582(7) 1.0565(6) 0.0676(3) 0.059 Uiso 1 calc R . C28 C 0.1169(7) 1.1054(6) 0.0627(3) 0.048(2) Uani 1 d . . H28 H 0.1043(7) 1.1161(6) 0.0207(3) 0.058 Uiso 1 calc R . C29 C 0.2305(7) 1.1255(6) 0.0947(3) 0.047(2) Uani 1 d . . H29 H 0.2969(7) 1.1496(6) 0.0752(3) 0.057 Uiso 1 calc R . C30 C 0.2482(6) 1.1102(5) 0.1567(3) 0.0375(13) Uani 1 d . . H30 H 0.3268(6) 1.1250(5) 0.1792(3) 0.045 Uiso 1 calc R . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd 0.0272(3) 0.0288(3) 0.0351(3) -0.0015(2) 0.0041(2) 0.0008(2) Fe 0.0219(4) 0.0311(4) 0.0193(4) 0.0017(3) 0.0022(3) 0.0041(3) P1 0.0296(7) 0.0276(7) 0.0230(6) 0.0010(5) 0.0048(5) 0.0014(5) P2 0.0226(6) 0.0249(7) 0.0280(7) 0.0007(5) 0.0030(5) 0.0012(5) Cl 0.0380(8) 0.0451(9) 0.0573(10) -0.0062(7) -0.0011(7) 0.0047(7) O1 0.110(5) 0.061(4) 0.070(4) -0.028(3) -0.024(4) 0.006(4) O2 0.060(3) 0.083(4) 0.037(3) -0.008(3) -0.002(3) -0.001(3) O3 0.043(3) 0.073(3) 0.051(3) 0.017(3) 0.019(2) -0.014(2) O4 0.054(3) 0.038(2) 0.039(2) 0.010(2) 0.012(2) -0.007(2) C1 0.054(4) 0.050(4) 0.042(4) 0.004(3) -0.001(3) 0.012(3) C2 0.069(5) 0.045(4) 0.028(3) -0.012(3) 0.021(3) -0.005(4) C3 0.042(4) 0.054(4) 0.053(4) -0.001(3) 0.002(3) 0.001(3) C4 0.043(3) 0.045(4) 0.042(3) 0.001(3) 0.004(3) 0.010(3) C5 0.046(4) 0.038(3) 0.053(4) -0.008(3) -0.001(3) 0.017(3) C6 0.038(3) 0.031(3) 0.030(3) 0.001(2) 0.001(2) -0.003(2) C7 0.092(6) 0.048(4) 0.032(3) -0.004(3) 0.015(3) -0.034(4) C9 0.081(5) 0.032(3) 0.060(5) -0.003(3) -0.007(4) -0.018(4) C8 0.116(8) 0.057(5) 0.043(4) 0.009(4) 0.006(4) -0.045(5) C10 0.070(5) 0.051(4) 0.065(5) -0.024(4) 0.021(4) -0.016(4) C11 0.060(4) 0.044(4) 0.044(4) -0.011(3) 0.021(3) -0.010(3) C12 0.039(3) 0.028(3) 0.025(3) -0.002(2) 0.005(2) -0.004(2) C13 0.055(4) 0.034(3) 0.032(3) 0.003(2) 0.013(3) 0.007(3) C14 0.070(5) 0.045(4) 0.035(3) 0.000(3) 0.025(3) -0.007(3) C15 0.048(4) 0.059(4) 0.054(4) -0.014(3) 0.024(3) -0.010(3) C16 0.042(4) 0.078(5) 0.047(4) -0.003(4) 0.012(3) 0.010(4) C17 0.041(3) 0.057(4) 0.036(3) 0.003(3) 0.012(3) 0.013(3) C18 0.032(3) 0.026(3) 0.022(2) 0.001(2) 0.002(2) 0.003(2) C19 0.028(3) 0.032(3) 0.028(3) 0.002(2) 0.002(2) -0.002(2) C20 0.032(3) 0.042(3) 0.063(4) 0.006(3) 0.013(3) 0.005(3) C21 0.028(3) 0.067(5) 0.091(6) -0.007(4) 0.015(4) 0.002(3) C22 0.045(4) 0.065(5) 0.065(5) -0.018(4) 0.023(4) -0.021(4) C23 0.052(4) 0.046(4) 0.040(3) -0.007(3) 0.015(3) -0.021(3) C24 0.040(3) 0.036(3) 0.033(3) -0.003(2) 0.006(2) -0.003(3) C25 0.037(3) 0.024(2) 0.032(3) -0.003(2) 0.004(2) 0.002(2) C26 0.039(3) 0.040(3) 0.038(3) -0.003(3) 0.002(3) -0.012(3) C27 0.056(4) 0.048(4) 0.038(3) -0.003(3) -0.008(3) -0.011(3) C28 0.063(4) 0.053(4) 0.027(3) -0.004(3) 0.001(3) 0.000(3) C29 0.051(4) 0.062(4) 0.032(3) 0.003(3) 0.018(3) -0.002(3) C30 0.035(3) 0.051(4) 0.027(3) -0.001(3) 0.004(2) -0.002(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd C5 2.066(6) . ? Pd P2 2.2098(14) . ? Pd Cl 2.361(2) . ? Pd C3 2.562(8) . ? Pd C4 2.623(7) . ? Pd Fe 2.8408(9) . ? Fe C1 1.761(7) . ? Fe C3 1.799(8) . ? Fe C4 1.869(8) . ? Fe C2 1.897(9) . ? Fe P1 2.256(2) . ? P1 C12 1.829(6) . ? P1 C6 1.838(6) . ? P1 C18 1.839(5) . ? P2 C19 1.815(6) . ? P2 C25 1.826(6) . ? P2 C18 1.831(5) . ? O1 C1 1.131(9) . ? O2 C2 0.991(9) . ? O3 C3 1.166(9) . ? O4 C4 1.155(8) . ? C6 C11 1.380(9) . ? C6 C7 1.388(9) . ? C7 C8 1.391(10) . ? C9 C10 1.361(11) . ? C9 C8 1.376(12) . ? C10 C11 1.386(10) . ? C12 C17 1.389(9) . ? C12 C13 1.391(8) . ? C13 C14 1.390(9) . ? C14 C15 1.378(11) . ? C15 C16 1.377(11) . ? C16 C17 1.385(9) . ? C19 C20 1.384(8) . ? C19 C24 1.395(8) . ? C20 C21 1.385(10) . ? C21 C22 1.372(12) . ? C22 C23 1.369(11) . ? C23 C24 1.389(9) . ? C25 C30 1.386(9) . ? C25 C26 1.385(8) . ? C26 C27 1.398(9) . ? C27 C28 1.373(11) . ? C28 C29 1.364(10) . ? C29 C30 1.404(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C5 Pd P2 85.2(2) . . ? C5 Pd Cl 87.4(2) . . ? P2 Pd Cl 172.42(6) . . ? C5 Pd C3 147.0(3) . . ? P2 Pd C3 92.4(2) . . ? Cl Pd C3 92.8(2) . . ? C5 Pd C4 134.8(3) . . ? P2 Pd C4 95.11(15) . . ? Cl Pd C4 91.34(15) . . ? C3 Pd C4 78.2(2) . . ? C5 Pd Fe 174.3(2) . . ? P2 Pd Fe 93.40(4) . . ? Cl Pd Fe 94.10(5) . . ? C3 Pd Fe 38.5(2) . . ? C4 Pd Fe 39.7(2) . . ? C1 Fe C3 119.8(4) . . ? C1 Fe C4 114.1(3) . . ? C3 Fe C4 126.1(3) . . ? C1 Fe C2 87.4(3) . . ? C3 Fe C2 89.0(3) . . ? C4 Fe C2 91.0(3) . . ? C1 Fe P1 87.0(2) . . ? C3 Fe P1 89.1(2) . . ? C4 Fe P1 96.2(2) . . ? C2 Fe P1 172.3(2) . . ? C1 Fe Pd 177.7(3) . . ? C3 Fe Pd 62.3(2) . . ? C4 Fe Pd 63.8(2) . . ? C2 Fe Pd 93.5(2) . . ? P1 Fe Pd 92.35(4) . . ? C12 P1 C6 103.1(3) . . ? C12 P1 C18 105.5(2) . . ? C6 P1 C18 103.2(2) . . ? C12 P1 Fe 118.0(2) . . ? C6 P1 Fe 113.7(2) . . ? C18 P1 Fe 111.9(2) . . ? C19 P2 C25 107.1(3) . . ? C19 P2 C18 105.9(3) . . ? C25 P2 C18 100.8(2) . . ? C19 P2 Pd 114.1(2) . . ? C25 P2 Pd 115.5(2) . . ? C18 P2 Pd 112.1(2) . . ? O1 C1 Fe 178.0(6) . . ? O2 C2 Fe 174.5(7) . . ? O3 C3 Fe 172.7(6) . . ? O3 C3 Pd 107.6(5) . . ? Fe C3 Pd 79.2(3) . . ? O4 C4 Fe 173.1(6) . . ? O4 C4 Pd 109.5(5) . . ? Fe C4 Pd 76.4(2) . . ? C11 C6 C7 118.3(6) . . ? C11 C6 P1 120.1(5) . . ? C7 C6 P1 121.3(5) . . ? C6 C7 C8 119.8(7) . . ? C10 C9 C8 120.0(7) . . ? C9 C8 C7 120.6(7) . . ? C9 C10 C11 119.7(7) . . ? C6 C11 C10 121.5(7) . . ? C17 C12 C13 118.7(6) . . ? C17 C12 P1 120.0(4) . . ? C13 C12 P1 121.3(5) . . ? C14 C13 C12 120.7(6) . . ? C15 C14 C13 119.3(6) . . ? C16 C15 C14 120.8(6) . . ? C15 C16 C17 119.7(7) . . ? C16 C17 C12 120.7(6) . . ? P2 C18 P1 113.3(3) . . ? C20 C19 C24 119.0(5) . . ? C20 C19 P2 122.3(5) . . ? C24 C19 P2 118.6(4) . . ? C19 C20 C21 119.9(7) . . ? C22 C21 C20 120.7(7) . . ? C23 C22 C21 120.1(7) . . ? C22 C23 C24 120.0(7) . . ? C23 C24 C19 120.2(6) . . ? C30 C25 C26 119.1(5) . . ? C30 C25 P2 117.6(4) . . ? C26 C25 P2 123.3(5) . . ? C25 C26 C27 119.8(6) . . ? C28 C27 C26 120.3(6) . . ? C29 C28 C27 120.7(6) . . ? C28 C29 C30 119.4(6) . . ? C25 C30 C29 120.7(6) . . ? _refine_diff_density_max 1.321 _refine_diff_density_min -1.502 _refine_diff_density_rms 0.141