# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _publ_contact_author_name 'Petr Stepnicka' _publ_contact_author_email stepnic@natur.cuni.cz loop_ _publ_author_name J.Tauchman I.Cisarova 'Petr Stepnicka' data_ps758 _database_code_depnum_ccdc_archive 'CCDC 823874' #TrackingRef 'deposit' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C8 H13 N2 Pd, Cl O4' _chemical_formula_sum 'C8 H13 Cl N2 O4 Pd' _chemical_formula_weight 343.05 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' Cl Cl 0.1484 0.1585 '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' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' '-x, -y, -z' 'x, -y-1/2, z' _cell_length_a 7.3756(2) _cell_length_b 10.4597(3) _cell_length_c 8.3592(2) _cell_angle_alpha 90.00 _cell_angle_beta 95.8421(17) _cell_angle_gamma 90.00 _cell_volume 641.53(3) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 1517 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.776 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 340 _exptl_absorpt_coefficient_mu 1.655 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.654 _exptl_absorpt_correction_T_max 0.750 _exptl_absorpt_process_details SORTAV _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'horizontally mounted graphite crystal' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method '\w and \p scans to fill the Ewald sphere' _diffrn_detector_area_resol_mean 9.091 _diffrn_reflns_number 8315 _diffrn_reflns_av_R_equivalents 0.0278 _diffrn_reflns_av_sigmaI/netI 0.0181 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 3.39 _diffrn_reflns_theta_max 27.50 _reflns_number_total 1543 _reflns_number_gt 1505 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor, 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR97 (Altomare et al., 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 2001)' _computing_publication_material 'PLATON (Spek, 2001)' _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^)+(0.0190P)^2^+0.3098P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.027(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 1543 _refine_ls_number_parameters 84 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0180 _refine_ls_R_factor_gt 0.0176 _refine_ls_wR_factor_ref 0.0445 _refine_ls_wR_factor_gt 0.0442 _refine_ls_goodness_of_fit_ref 1.126 _refine_ls_restrained_S_all 1.126 _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 Pd Pd 0.03923(2) 0.2500 0.662659(18) 0.02245(9) Uani 1 2 d S . . Cl Cl 0.73400(7) 0.2500 0.19146(6) 0.02212(12) Uani 1 2 d S . . O1 O 0.6218(2) 0.2500 0.0402(2) 0.0314(4) Uani 1 2 d S . . O2 O 0.6952(2) 0.13873(15) 0.28120(19) 0.0556(4) Uani 1 1 d . . . O3 O 0.9221(3) 0.2500 0.1637(2) 0.0561(6) Uani 1 2 d S . . C1 C 0.1811(3) 0.13710(17) 0.50852(19) 0.0321(4) Uani 1 1 d . . . H1A H 0.0989 0.1381 0.4240 0.039 Uiso 1 1 d R . . H1B H 0.2456 0.0505 0.5408 0.039 Uiso 1 1 d R . . C2 C 0.2809(3) 0.2500 0.5401(3) 0.0312(5) Uani 1 2 d S . . C3 C 0.4647(4) 0.2500 0.6355(4) 0.0596(10) Uani 1 2 d S . . H3A H 0.4843 0.3196 0.7181 0.089 Uiso 1 1 d R . . H3B H 0.5591 0.2500 0.5655 0.089 Uiso 1 2 d SR . . N N -0.0929(2) 0.10767(13) 0.77993(17) 0.0285(3) Uani 1 1 d . . . C4 C -0.1712(2) 0.03424(15) 0.84451(19) 0.0264(3) Uani 1 1 d . . . C5 C -0.2716(3) -0.06086(17) 0.9267(2) 0.0375(4) Uani 1 1 d . . . H5A H -0.3857 -0.0781 0.8645 0.056 Uiso 1 1 calc R . . H5B H -0.2940 -0.0291 1.0306 0.056 Uiso 1 1 calc R . . H5C H -0.2015 -0.1382 0.9392 0.056 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 Pd 0.02400(13) 0.02006(12) 0.02300(12) 0.000 0.00106(6) 0.000 Cl 0.0214(2) 0.0214(2) 0.0232(2) 0.000 0.00055(18) 0.000 O1 0.0268(9) 0.0385(10) 0.0273(8) 0.000 -0.0048(6) 0.000 O2 0.0707(11) 0.0427(8) 0.0507(8) 0.0233(7) -0.0073(7) -0.0131(8) O3 0.0210(9) 0.106(2) 0.0410(11) 0.000 0.0021(8) 0.000 C1 0.0389(9) 0.0323(9) 0.0254(7) -0.0012(7) 0.0047(6) 0.0093(7) C2 0.0286(12) 0.0464(14) 0.0191(10) 0.000 0.0046(8) 0.000 C3 0.0260(14) 0.117(3) 0.0354(14) 0.000 0.0009(11) 0.000 N 0.0302(7) 0.0231(7) 0.0326(7) -0.0015(6) 0.0053(6) 0.0002(6) C4 0.0243(8) 0.0220(7) 0.0328(7) -0.0053(6) 0.0026(6) 0.0017(6) C5 0.0320(9) 0.0267(8) 0.0553(11) 0.0016(8) 0.0109(8) -0.0055(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 Pd N 2.0786(14) 4_565 ? Pd N 2.0786(14) . ? Pd C1 2.1033(16) . ? Pd C1 2.1033(16) 4_565 ? Pd C2 2.144(2) . ? Cl O2 1.4292(14) 4_565 ? Cl O2 1.4292(14) . ? Cl O3 1.430(2) . ? Cl O1 1.4389(17) . ? C1 C2 1.402(2) . ? C1 H1A 0.8828 . ? C1 H1B 1.0460 . ? C2 C1 1.402(2) 4_565 ? C2 C3 1.502(4) . ? C3 H3A 1.0033 . ? C3 H3B 0.9541 . ? N C4 1.131(2) . ? C4 C5 1.454(2) . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? 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 N Pd N 91.48(8) 4_565 . ? N Pd C1 167.76(6) 4_565 . ? N Pd C1 99.97(6) . . ? N Pd C1 99.97(6) 4_565 4_565 ? N Pd C1 167.76(6) . 4_565 ? C1 Pd C1 68.31(10) . 4_565 ? N Pd C2 132.66(4) 4_565 . ? N Pd C2 132.66(4) . . ? C1 Pd C2 38.53(6) . . ? C1 Pd C2 38.53(6) 4_565 . ? O2 Cl O2 109.04(15) 4_565 . ? O2 Cl O3 109.54(9) 4_565 . ? O2 Cl O3 109.54(9) . . ? O2 Cl O1 109.46(8) 4_565 . ? O2 Cl O1 109.46(8) . . ? O3 Cl O1 109.78(11) . . ? C2 C1 Pd 72.32(11) . . ? C2 C1 H1A 116.4 . . ? Pd C1 H1A 98.0 . . ? C2 C1 H1B 117.7 . . ? Pd C1 H1B 124.7 . . ? H1A C1 H1B 118.3 . . ? C1 C2 C1 114.7(2) . 4_565 ? C1 C2 C3 121.88(11) . . ? C1 C2 C3 121.88(11) 4_565 . ? C1 C2 Pd 69.15(11) . . ? C1 C2 Pd 69.15(11) 4_565 . ? C3 C2 Pd 119.71(17) . . ? C2 C3 H3A 115.1 . . ? C2 C3 H3B 110.5 . . ? H3A C3 H3B 111.1 . . ? C4 N Pd 176.74(13) . . ? N C4 C5 179.58(18) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.409 _refine_diff_density_min -0.457 _refine_diff_density_rms 0.057 #===END data_jt168 _database_code_depnum_ccdc_archive 'CCDC 823875' #TrackingRef 'deposit' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H31 Cl Fe N O3 P Pd, H2 O' _chemical_formula_sum 'C30 H33 Cl Fe N O4 P Pd' _chemical_formula_weight 700.24 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 monoclinic _symmetry_space_group_name_H-M P21/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 10.0468(7) _cell_length_b 30.550(2) _cell_length_c 9.7502(7) _cell_angle_alpha 90.00 _cell_angle_beta 105.252(4) _cell_angle_gamma 90.00 _cell_volume 2887.2(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9882 _cell_measurement_theta_min 2.54 _cell_measurement_theta_max 34.05 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.43 _exptl_crystal_size_mid 0.34 _exptl_crystal_size_min 0.28 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.611 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1424 _exptl_absorpt_coefficient_mu 1.310 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6028 _exptl_absorpt_correction_T_max 0.7106 _exptl_absorpt_process_details SADABS _diffrn_ambient_temperature 150(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 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_standards_number 0 _diffrn_reflns_number 28502 _diffrn_reflns_av_R_equivalents 0.0265 _diffrn_reflns_av_sigmaI/netI 0.0240 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -39 _diffrn_reflns_limit_k_max 39 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.33 _diffrn_reflns_theta_max 27.50 _reflns_number_total 6639 _reflns_number_gt 5960 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 2003)' _computing_publication_material 'PLATON (Spek, 2003)' _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^)+(0.0272P)^2^+3.4204P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6639 _refine_ls_number_parameters 364 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0377 _refine_ls_R_factor_gt 0.0322 _refine_ls_wR_factor_ref 0.0747 _refine_ls_wR_factor_gt 0.0724 _refine_ls_goodness_of_fit_ref 1.106 _refine_ls_restrained_S_all 1.106 _refine_ls_shift/su_max 0.004 _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 Pd Pd 0.84112(3) 0.822555(18) 0.37935(4) 0.02370(13) Uani 0.961(2) 1 d P . . PdA Pd 0.8138(8) 0.8032(4) 0.4106(8) 0.025(2) Uani 0.039(2) 1 d P . . Fe Fe 0.65113(3) 0.960481(11) 0.32592(4) 0.01945(8) Uani 1 1 d . . . Cl Cl 1.00188(6) 0.85502(2) 0.57572(7) 0.03122(14) Uani 1 1 d . . . P P 0.62622(6) 0.848631(19) 0.38527(6) 0.02000(13) Uani 1 1 d . . . O1 O 0.96501(19) 0.99188(6) 0.2061(2) 0.0330(4) Uani 1 1 d . . . O2 O 0.94108(19) 0.88515(7) 0.0917(2) 0.0380(5) Uani 1 1 d . . . O3 O 1.1387(2) 0.90690(7) 0.0479(2) 0.0367(5) Uani 1 1 d . . . N N 1.0204(2) 0.93349(7) 0.3501(2) 0.0270(5) Uani 1 1 d . . . H1N H 1.0073 0.9185 0.4226 0.032 Uiso 1 1 calc R . . C1 C 0.5811(2) 0.89780(7) 0.2834(2) 0.0192(4) Uani 1 1 d . . . C2 C 0.4697(2) 0.92692(8) 0.2848(3) 0.0217(5) Uani 1 1 d . . . H2 H 0.4107 0.9249 0.3464 0.026 Uiso 1 1 calc R . . C3 C 0.4623(3) 0.95926(8) 0.1792(3) 0.0270(5) Uani 1 1 d . . . H3 H 0.3971 0.9824 0.1569 0.032 Uiso 1 1 calc R . . C4 C 0.5699(3) 0.95093(9) 0.1125(3) 0.0270(5) Uani 1 1 d . . . H4 H 0.5892 0.9678 0.0381 0.032 Uiso 1 1 calc R . . C5 C 0.6433(2) 0.91319(8) 0.1759(2) 0.0228(5) Uani 1 1 d . . . H5 H 0.7202 0.9004 0.1514 0.027 Uiso 1 1 calc R . . C6 C 0.8474(2) 0.98332(8) 0.3848(3) 0.0240(5) Uani 1 1 d . . . C7 C 0.8150(2) 0.96216(8) 0.5026(3) 0.0247(5) Uani 1 1 d . . . H7 H 0.8612 0.9376 0.5531 0.030 Uiso 1 1 calc R . . C8 C 0.7014(3) 0.98459(9) 0.5304(3) 0.0286(6) Uani 1 1 d . . . H8 H 0.6580 0.9776 0.6032 0.034 Uiso 1 1 calc R . . C9 C 0.6633(3) 1.01929(8) 0.4312(3) 0.0321(6) Uani 1 1 d . . . H9 H 0.5902 1.0395 0.4262 0.039 Uiso 1 1 calc R . . C10 C 0.7529(3) 1.01869(8) 0.3412(3) 0.0294(6) Uani 1 1 d . . . H10 H 0.7506 1.0383 0.2651 0.035 Uiso 1 1 calc R . . C11 C 0.9482(2) 0.97011(8) 0.3069(3) 0.0248(5) Uani 1 1 d . . . C12 C 0.5779(2) 0.86059(7) 0.5497(2) 0.0205(5) Uani 1 1 d . . . C13 C 0.4406(3) 0.85702(8) 0.5560(3) 0.0242(5) Uani 1 1 d . . . H13 H 0.3725 0.8462 0.4763 0.029 Uiso 1 1 calc R . . C14 C 0.4035(3) 0.86915(8) 0.6775(3) 0.0285(5) Uani 1 1 d . . . H14 H 0.3099 0.8672 0.6805 0.034 Uiso 1 1 calc R . . C15 C 0.5029(3) 0.88407(9) 0.7945(3) 0.0311(6) Uani 1 1 d . . . H15 H 0.4774 0.8923 0.8781 0.037 Uiso 1 1 calc R . . C16 C 0.6391(3) 0.88716(9) 0.7908(3) 0.0323(6) Uani 1 1 d . . . H16 H 0.7070 0.8974 0.8718 0.039 Uiso 1 1 calc R . . C17 C 0.6769(3) 0.87535(8) 0.6688(3) 0.0262(5) Uani 1 1 d . . . H17 H 0.7707 0.8774 0.6666 0.031 Uiso 1 1 calc R . . C18 C 0.4894(3) 0.81032(8) 0.2990(3) 0.0237(5) Uani 1 1 d . . . C19 C 0.4922(4) 0.76890(9) 0.3572(3) 0.0431(7) Uani 1 1 d . . . H19 H 0.5639 0.7613 0.4386 0.052 Uiso 1 1 calc R . . C20 C 0.3916(4) 0.73846(10) 0.2981(4) 0.0506(9) Uani 1 1 d . . . H20 H 0.3942 0.7103 0.3400 0.061 Uiso 1 1 calc R . . C21 C 0.2883(4) 0.74850(10) 0.1796(4) 0.0453(8) Uani 1 1 d . . . H21 H 0.2195 0.7275 0.1393 0.054 Uiso 1 1 calc R . . C22 C 0.2851(3) 0.78951(10) 0.1194(3) 0.0410(7) Uani 1 1 d . . . H22 H 0.2142 0.7966 0.0368 0.049 Uiso 1 1 calc R . . C23 C 0.3853(3) 0.82049(9) 0.1791(3) 0.0305(6) Uani 1 1 d . . . H23 H 0.3822 0.8487 0.1374 0.037 Uiso 1 1 calc R . . C24 C 1.1194(2) 0.91874(10) 0.2772(3) 0.0308(6) Uani 1 1 d . . . H24A H 1.1760 0.8951 0.3334 0.037 Uiso 1 1 calc R . . H24B H 1.1819 0.9433 0.2708 0.037 Uiso 1 1 calc R . . C25 C 1.0525(3) 0.90193(8) 0.1292(3) 0.0264(5) Uani 1 1 d . . . C26 C 1.0875(3) 0.89284(11) -0.0980(3) 0.0432(7) Uani 1 1 d . . . H26A H 1.0507 0.8631 -0.1003 0.065 Uiso 1 1 calc R . . H26B H 1.1630 0.8932 -0.1444 0.065 Uiso 1 1 calc R . . H26C H 1.0142 0.9127 -0.1481 0.065 Uiso 1 1 calc R . . C30 C 1.0027(3) 0.79036(11) 0.3013(4) 0.0437(7) Uani 1 1 d . . . H30A H 1.0036 0.8205 0.2772 0.052 Uiso 1 1 d R . . H30S H 1.0851 0.7765 0.3537 0.052 Uiso 1 1 d R . . C31 C 0.8807(3) 0.76634(10) 0.2594(3) 0.0416(7) Uani 1 1 d . . . C32 C 0.7646(3) 0.79089(12) 0.1820(3) 0.0486(8) Uani 1 1 d . . . H32A H 0.7748 0.8210 0.1626 0.058 Uiso 1 1 d R . . H32S H 0.6771 0.7772 0.1494 0.058 Uiso 1 1 d R . . C33 C 0.8670(5) 0.72206(11) 0.3170(5) 0.0689(12) Uani 1 1 d . . . H33A H 0.8905 0.6999 0.2545 0.103 Uiso 1 1 calc R . . H33B H 0.7718 0.7176 0.3220 0.103 Uiso 1 1 calc R . . H33C H 0.9297 0.7194 0.4124 0.103 Uiso 1 1 calc R . . O1W O 0.8183(2) 0.97819(7) 0.9113(2) 0.0439(5) Uani 1 1 d . . . H1W H 0.8815 0.9909 0.8620 0.053 Uiso 1 1 d R . . H2W H 0.8610 0.9837 1.0160 0.053 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd 0.02200(12) 0.0267(2) 0.02166(13) -0.00334(13) 0.00452(9) 0.00671(12) PdA 0.022(3) 0.026(5) 0.025(3) 0.005(3) 0.005(2) 0.001(3) Fe 0.01833(16) 0.02187(17) 0.01981(17) -0.00205(13) 0.00795(13) -0.00124(12) Cl 0.0245(3) 0.0424(4) 0.0251(3) -0.0001(3) 0.0036(2) 0.0015(3) P 0.0199(3) 0.0224(3) 0.0167(3) -0.0031(2) 0.0030(2) 0.0026(2) O1 0.0283(9) 0.0454(11) 0.0284(10) 0.0044(8) 0.0128(8) -0.0043(8) O2 0.0267(10) 0.0558(13) 0.0326(11) -0.0084(9) 0.0100(8) -0.0095(9) O3 0.0324(10) 0.0519(12) 0.0303(11) -0.0099(9) 0.0164(9) -0.0088(9) N 0.0227(10) 0.0383(12) 0.0219(11) -0.0009(9) 0.0092(9) -0.0008(9) C1 0.0166(10) 0.0230(11) 0.0173(11) -0.0038(9) 0.0034(9) -0.0014(8) C2 0.0147(10) 0.0259(12) 0.0253(12) -0.0008(10) 0.0069(9) -0.0017(9) C3 0.0222(12) 0.0306(13) 0.0263(13) 0.0051(10) 0.0033(10) 0.0029(10) C4 0.0275(12) 0.0341(13) 0.0190(12) 0.0036(10) 0.0056(10) -0.0019(10) C5 0.0221(11) 0.0305(12) 0.0166(11) -0.0068(9) 0.0062(9) -0.0026(9) C6 0.0196(11) 0.0273(12) 0.0260(13) -0.0072(10) 0.0078(10) -0.0079(9) C7 0.0234(12) 0.0317(13) 0.0192(12) -0.0076(10) 0.0058(10) -0.0064(10) C8 0.0290(13) 0.0347(14) 0.0259(13) -0.0129(11) 0.0137(11) -0.0087(11) C9 0.0318(14) 0.0265(13) 0.0421(16) -0.0122(12) 0.0169(12) -0.0028(10) C10 0.0309(13) 0.0228(12) 0.0370(15) -0.0033(11) 0.0134(12) -0.0056(10) C11 0.0180(11) 0.0346(13) 0.0215(12) -0.0050(10) 0.0044(9) -0.0072(9) C12 0.0261(12) 0.0186(10) 0.0170(11) -0.0002(9) 0.0059(9) 0.0017(9) C13 0.0250(12) 0.0238(12) 0.0229(12) -0.0014(9) 0.0048(10) 0.0001(9) C14 0.0292(13) 0.0313(13) 0.0281(14) 0.0006(11) 0.0128(11) 0.0005(10) C15 0.0406(15) 0.0338(14) 0.0225(13) -0.0041(11) 0.0150(12) -0.0026(11) C16 0.0375(15) 0.0394(15) 0.0192(12) -0.0051(11) 0.0061(11) -0.0079(12) C17 0.0239(12) 0.0329(13) 0.0216(12) -0.0005(10) 0.0057(10) -0.0019(10) C18 0.0271(12) 0.0219(11) 0.0221(12) -0.0048(9) 0.0063(10) -0.0005(9) C19 0.065(2) 0.0275(14) 0.0307(15) -0.0012(12) 0.0017(14) -0.0035(13) C20 0.084(3) 0.0256(14) 0.0425(19) -0.0055(13) 0.0167(18) -0.0159(15) C21 0.0523(19) 0.0373(16) 0.0503(19) -0.0200(14) 0.0206(16) -0.0201(14) C22 0.0294(14) 0.0448(17) 0.0428(17) -0.0094(14) -0.0010(13) -0.0077(12) C23 0.0278(13) 0.0281(13) 0.0334(15) -0.0020(11) 0.0043(11) -0.0022(10) C24 0.0183(12) 0.0457(15) 0.0288(14) -0.0070(12) 0.0070(10) -0.0001(11) C25 0.0229(12) 0.0323(13) 0.0259(13) 0.0011(10) 0.0098(10) 0.0040(10) C26 0.0527(19) 0.0532(19) 0.0289(15) -0.0092(13) 0.0197(14) -0.0052(15) C30 0.0385(16) 0.0465(17) 0.0499(19) -0.0064(14) 0.0183(15) 0.0162(13) C31 0.0465(17) 0.0402(16) 0.0427(17) -0.0157(14) 0.0198(15) 0.0098(13) C32 0.0444(18) 0.061(2) 0.0388(18) -0.0282(16) 0.0078(14) 0.0084(15) C33 0.092(3) 0.0374(18) 0.091(3) -0.0175(19) 0.049(3) 0.0047(19) O1W 0.0346(11) 0.0510(13) 0.0456(13) 0.0070(10) 0.0099(10) -0.0061(9) _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 PdA 0.750(15) . ? Pd C32 2.110(3) . ? Pd C31 2.172(3) . ? Pd C30 2.198(3) . ? Pd P 2.3162(6) . ? Pd Cl 2.3730(7) . ? Pd H30A 2.1249 . ? Pd H32A 2.0427 . ? PdA C31 2.100(6) . ? PdA C32 2.185(7) . ? PdA P 2.301(6) . ? PdA C30 2.441(9) . ? PdA Cl 2.659(9) . ? Fe C6 2.027(2) . ? Fe C2 2.037(2) . ? Fe C10 2.037(2) . ? Fe C5 2.043(2) . ? Fe C1 2.045(2) . ? Fe C7 2.047(2) . ? Fe C4 2.047(3) . ? Fe C3 2.054(3) . ? Fe C9 2.057(3) . ? Fe C8 2.060(3) . ? P C1 1.792(2) . ? P C12 1.830(2) . ? P C18 1.833(2) . ? O1 C11 1.235(3) . ? O2 C25 1.197(3) . ? O3 C25 1.327(3) . ? O3 C26 1.445(3) . ? N C11 1.339(3) . ? N C24 1.438(3) . ? N H1N 0.8800 . ? C1 C2 1.432(3) . ? C1 C5 1.434(3) . ? C2 C3 1.415(3) . ? C2 H2 0.9500 . ? C3 C4 1.424(4) . ? C3 H3 0.9500 . ? C4 C5 1.420(4) . ? C4 H4 0.9500 . ? C5 H5 0.9500 . ? C6 C10 1.427(4) . ? C6 C7 1.428(3) . ? C6 C11 1.474(3) . ? C7 C8 1.417(3) . ? C7 H7 0.9500 . ? C8 C9 1.418(4) . ? C8 H8 0.9500 . ? C9 C10 1.414(4) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C12 C17 1.390(3) . ? C12 C13 1.401(3) . ? C13 C14 1.383(4) . ? C13 H13 0.9500 . ? C14 C15 1.381(4) . ? C14 H14 0.9500 . ? C15 C16 1.382(4) . ? C15 H15 0.9500 . ? C16 C17 1.388(4) . ? C16 H16 0.9500 . ? C17 H17 0.9500 . ? C18 C23 1.383(4) . ? C18 C19 1.384(4) . ? C19 C20 1.383(4) . ? C19 H19 0.9500 . ? C20 C21 1.369(5) . ? C20 H20 0.9500 . ? C21 C22 1.380(5) . ? C21 H21 0.9500 . ? C22 C23 1.393(4) . ? C22 H22 0.9500 . ? C23 H23 0.9500 . ? C24 C25 1.513(4) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C30 C31 1.394(5) . ? C30 H30A 0.9500 . ? C30 H30S 0.9500 . ? C31 C32 1.425(5) . ? C31 C33 1.485(5) . ? C32 H32A 0.9500 . ? C32 H32S 0.9500 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? O1W H1W 0.9723 . ? O1W H2W 1.0115 . ? 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 PdA Pd C32 85.7(4) . . ? PdA Pd C31 74.5(4) . . ? C32 Pd C31 38.84(12) . . ? PdA Pd C30 99.8(4) . . ? C32 Pd C30 66.68(12) . . ? C31 Pd C30 37.20(12) . . ? PdA Pd P 79.5(4) . . ? C32 Pd P 93.55(9) . . ? C31 Pd P 126.09(9) . . ? C30 Pd P 160.15(9) . . ? PdA Pd Cl 104.3(4) . . ? C32 Pd Cl 159.21(9) . . ? C31 Pd Cl 125.63(9) . . ? C30 Pd Cl 93.36(9) . . ? P Pd Cl 106.09(2) . . ? PdA Pd H30A 125.1 . . ? C32 Pd H30A 72.5 . . ? C31 Pd H30A 56.8 . . ? C30 Pd H30A 25.3 . . ? P Pd H30A 149.1 . . ? Cl Pd H30A 87.0 . . ? PdA Pd H32A 110.3 . . ? C32 Pd H32A 26.4 . . ? C31 Pd H32A 58.7 . . ? C30 Pd H32A 72.6 . . ? P Pd H32A 88.9 . . ? Cl Pd H32A 144.3 . . ? H30A Pd H32A 66.2 . . ? Pd PdA C31 85.3(6) . . ? Pd PdA C32 74.3(6) . . ? C31 PdA C32 38.78(16) . . ? Pd PdA P 81.8(6) . . ? C31 PdA P 130.7(3) . . ? C32 PdA P 92.0(3) . . ? Pd PdA C30 62.6(5) . . ? C31 PdA C30 34.75(17) . . ? C32 PdA C30 61.3(2) . . ? P PdA C30 139.4(6) . . ? Pd PdA Cl 59.9(5) . . ? C31 PdA Cl 115.9(4) . . ? C32 PdA Cl 130.8(7) . . ? P PdA Cl 97.9(3) . . ? C30 PdA Cl 81.3(3) . . ? C6 Fe C2 169.21(10) . . ? C6 Fe C10 41.12(10) . . ? C2 Fe C10 149.28(10) . . ? C6 Fe C5 107.31(10) . . ? C2 Fe C5 68.87(9) . . ? C10 Fe C5 126.41(10) . . ? C6 Fe C1 129.58(9) . . ? C2 Fe C1 41.08(9) . . ? C10 Fe C1 166.34(10) . . ? C5 Fe C1 41.08(9) . . ? C6 Fe C7 41.04(10) . . ? C2 Fe C7 131.16(10) . . ? C10 Fe C7 68.87(11) . . ? C5 Fe C7 119.43(10) . . ? C1 Fe C7 110.61(10) . . ? C6 Fe C4 115.80(10) . . ? C2 Fe C4 68.37(10) . . ? C10 Fe C4 104.89(11) . . ? C5 Fe C4 40.63(10) . . ? C1 Fe C4 68.67(10) . . ? C7 Fe C4 151.26(10) . . ? C6 Fe C3 148.76(10) . . ? C2 Fe C3 40.47(10) . . ? C10 Fe C3 114.87(11) . . ? C5 Fe C3 68.54(10) . . ? C1 Fe C3 68.66(10) . . ? C7 Fe C3 167.89(10) . . ? C4 Fe C3 40.62(10) . . ? C6 Fe C9 68.43(10) . . ? C2 Fe C9 118.05(10) . . ? C10 Fe C9 40.39(10) . . ? C5 Fe C9 163.99(11) . . ? C1 Fe C9 153.04(10) . . ? C7 Fe C9 68.22(11) . . ? C4 Fe C9 125.98(11) . . ? C3 Fe C9 106.62(11) . . ? C6 Fe C8 68.31(10) . . ? C2 Fe C8 110.43(10) . . ? C10 Fe C8 68.08(11) . . ? C5 Fe C8 154.10(11) . . ? C1 Fe C8 120.99(10) . . ? C7 Fe C8 40.39(10) . . ? C4 Fe C8 164.98(11) . . ? C3 Fe C8 128.81(10) . . ? C9 Fe C8 40.29(11) . . ? C1 P C12 103.38(10) . . ? C1 P C18 103.35(11) . . ? C12 P C18 100.93(11) . . ? C1 P PdA 130.2(4) . . ? C12 P PdA 115.2(2) . . ? C18 P PdA 99.1(3) . . ? C1 P Pd 112.10(8) . . ? C12 P Pd 123.67(8) . . ? C18 P Pd 111.13(8) . . ? C25 O3 C26 115.7(2) . . ? C11 N C24 119.6(2) . . ? C11 N H1N 120.2 . . ? C24 N H1N 120.2 . . ? C2 C1 C5 107.2(2) . . ? C2 C1 P 126.84(18) . . ? C5 C1 P 125.77(17) . . ? C2 C1 Fe 69.17(13) . . ? C5 C1 Fe 69.39(13) . . ? P C1 Fe 130.47(12) . . ? C3 C2 C1 108.6(2) . . ? C3 C2 Fe 70.41(14) . . ? C1 C2 Fe 69.75(13) . . ? C3 C2 H2 125.7 . . ? C1 C2 H2 125.7 . . ? Fe C2 H2 125.7 . . ? C2 C3 C4 107.9(2) . . ? C2 C3 Fe 69.13(14) . . ? C4 C3 Fe 69.43(14) . . ? C2 C3 H3 126.1 . . ? C4 C3 H3 126.1 . . ? Fe C3 H3 127.0 . . ? C5 C4 C3 108.4(2) . . ? C5 C4 Fe 69.54(14) . . ? C3 C4 Fe 69.95(15) . . ? C5 C4 H4 125.8 . . ? C3 C4 H4 125.8 . . ? Fe C4 H4 126.3 . . ? C4 C5 C1 107.9(2) . . ? C4 C5 Fe 69.83(14) . . ? C1 C5 Fe 69.53(13) . . ? C4 C5 H5 126.0 . . ? C1 C5 H5 126.0 . . ? Fe C5 H5 126.2 . . ? C10 C6 C7 107.9(2) . . ? C10 C6 C11 123.2(2) . . ? C7 C6 C11 128.6(2) . . ? C10 C6 Fe 69.82(14) . . ? C7 C6 Fe 70.22(13) . . ? C11 C6 Fe 120.62(17) . . ? C8 C7 C6 107.5(2) . . ? C8 C7 Fe 70.30(15) . . ? C6 C7 Fe 68.74(14) . . ? C8 C7 H7 126.3 . . ? C6 C7 H7 126.3 . . ? Fe C7 H7 126.3 . . ? C7 C8 C9 108.5(2) . . ? C7 C8 Fe 69.31(14) . . ? C9 C8 Fe 69.75(15) . . ? C7 C8 H8 125.7 . . ? C9 C8 H8 125.7 . . ? Fe C8 H8 126.8 . . ? C10 C9 C8 108.2(2) . . ? C10 C9 Fe 69.04(14) . . ? C8 C9 Fe 69.95(14) . . ? C10 C9 H9 125.9 . . ? C8 C9 H9 125.9 . . ? Fe C9 H9 126.7 . . ? C9 C10 C6 107.9(2) . . ? C9 C10 Fe 70.56(15) . . ? C6 C10 Fe 69.06(13) . . ? C9 C10 H10 126.1 . . ? C6 C10 H10 126.1 . . ? Fe C10 H10 125.9 . . ? O1 C11 N 121.6(2) . . ? O1 C11 C6 121.3(2) . . ? N C11 C6 117.1(2) . . ? C17 C12 C13 119.0(2) . . ? C17 C12 P 119.98(18) . . ? C13 C12 P 120.94(18) . . ? C14 C13 C12 120.5(2) . . ? C14 C13 H13 119.8 . . ? C12 C13 H13 119.8 . . ? C15 C14 C13 119.8(2) . . ? C15 C14 H14 120.1 . . ? C13 C14 H14 120.1 . . ? C14 C15 C16 120.5(2) . . ? C14 C15 H15 119.8 . . ? C16 C15 H15 119.8 . . ? C15 C16 C17 120.0(2) . . ? C15 C16 H16 120.0 . . ? C17 C16 H16 120.0 . . ? C16 C17 C12 120.2(2) . . ? C16 C17 H17 119.9 . . ? C12 C17 H17 119.9 . . ? C23 C18 C19 118.8(2) . . ? C23 C18 P 123.59(19) . . ? C19 C18 P 117.6(2) . . ? C20 C19 C18 120.7(3) . . ? C20 C19 H19 119.7 . . ? C18 C19 H19 119.7 . . ? C21 C20 C19 120.6(3) . . ? C21 C20 H20 119.7 . . ? C19 C20 H20 119.7 . . ? C20 C21 C22 119.4(3) . . ? C20 C21 H21 120.3 . . ? C22 C21 H21 120.3 . . ? C21 C22 C23 120.3(3) . . ? C21 C22 H22 119.8 . . ? C23 C22 H22 119.8 . . ? C18 C23 C22 120.2(3) . . ? C18 C23 H23 119.9 . . ? C22 C23 H23 119.9 . . ? N C24 C25 112.7(2) . . ? N C24 H24A 109.1 . . ? C25 C24 H24A 109.1 . . ? N C24 H24B 109.1 . . ? C25 C24 H24B 109.1 . . ? H24A C24 H24B 107.8 . . ? O2 C25 O3 124.9(2) . . ? O2 C25 C24 125.6(2) . . ? O3 C25 C24 109.5(2) . . ? O3 C26 H26A 109.5 . . ? O3 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? O3 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C31 C30 Pd 70.39(16) . . ? C31 C30 PdA 59.2(3) . . ? C31 C30 H30A 120.1 . . ? Pd C30 H30A 73.0 . . ? PdA C30 H30A 90.7 . . ? C31 C30 H30S 119.9 . . ? Pd C30 H30S 129.1 . . ? PdA C30 H30S 120.3 . . ? H30A C30 H30S 120.0 . . ? C30 C31 C32 114.3(3) . . ? C30 C31 C33 122.1(3) . . ? C32 C31 C33 122.4(3) . . ? C30 C31 PdA 86.1(4) . . ? C32 C31 PdA 73.8(3) . . ? C33 C31 PdA 98.3(5) . . ? C30 C31 Pd 72.41(17) . . ? C32 C31 Pd 68.23(16) . . ? C33 C31 Pd 118.0(2) . . ? C31 C32 Pd 72.94(17) . . ? C31 C32 PdA 67.4(2) . . ? C31 C32 H32A 119.9 . . ? Pd C32 H32A 72.8 . . ? PdA C32 H32A 91.7 . . ? C31 C32 H32S 120.1 . . ? Pd C32 H32S 126.2 . . ? PdA C32 H32S 111.0 . . ? H32A C32 H32S 120.0 . . ? C31 C33 H33A 109.5 . . ? C31 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C31 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? H1W O1W H2W 105.9 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.543 _refine_diff_density_min -0.464 _refine_diff_density_rms 0.072 #===END data_jt158 _database_code_depnum_ccdc_archive 'CCDC 823876' #TrackingRef 'deposit' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H31 Fe N O3 P Pd, Cl O4' _chemical_formula_sum 'C30 H31 Cl Fe N O7 P Pd' _chemical_formula_weight 746.23 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 monoclinic _symmetry_space_group_name_H-M P21/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 14.4397(6) _cell_length_b 15.1067(6) _cell_length_c 15.0910(7) _cell_angle_alpha 90.00 _cell_angle_beta 112.4940(10) _cell_angle_gamma 90.00 _cell_volume 3041.4(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9064 _cell_measurement_theta_min 2.70 _cell_measurement_theta_max 27.09 _exptl_crystal_description bar _exptl_crystal_colour orange _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.630 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1512 _exptl_absorpt_coefficient_mu 1.256 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.6409 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_process_details ; numerical absorption correction using SADABS ; _diffrn_ambient_temperature 150(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 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_reflns_number 26854 _diffrn_reflns_av_R_equivalents 0.0396 _diffrn_reflns_av_sigmaI/netI 0.0464 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.53 _diffrn_reflns_theta_max 27.52 _reflns_number_total 6962 _reflns_number_gt 4760 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'PLATON (Spekm 2003)' _computing_publication_material 'PLATON (Spekm 2003)' _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^)+(0.0349P)^2^+7.0568P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6962 _refine_ls_number_parameters 381 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0769 _refine_ls_R_factor_gt 0.0386 _refine_ls_wR_factor_ref 0.1025 _refine_ls_wR_factor_gt 0.0834 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.047 _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 Pd Pd 0.68246(2) 0.579705(19) 0.28580(2) 0.02405(9) Uani 1 1 d . . . Fe Fe 0.73741(4) 0.58454(4) 0.04387(4) 0.02417(13) Uani 1 1 d . . . P P 0.82147(7) 0.64753(7) 0.27530(7) 0.0249(2) Uani 1 1 d . . . O1 O 0.67849(19) 0.45688(17) 0.21355(18) 0.0261(6) Uani 1 1 d . . . O2 O 0.8485(2) 0.3093(2) 0.2242(2) 0.0452(8) Uani 1 1 d . . . O3 O 0.7910(3) 0.1970(2) 0.2856(2) 0.0486(9) Uani 1 1 d . . . N N 0.6518(2) 0.3527(2) 0.1016(2) 0.0302(8) Uani 1 1 d . . . H1N H 0.6324 0.3381 0.0452 0.036 Uiso 1 1 d R . . C1 C 0.8475(3) 0.6205(3) 0.1706(3) 0.0262(8) Uani 1 1 d . . . C2 C 0.8454(3) 0.6801(3) 0.0955(3) 0.0313(9) Uani 1 1 d . . . H2 H 0.8343 0.7421 0.0941 0.038 Uiso 1 1 calc R . . C3 C 0.8626(3) 0.6304(3) 0.0242(3) 0.0362(10) Uani 1 1 d . . . H3 H 0.8658 0.6535 -0.0331 0.043 Uiso 1 1 calc R . . C4 C 0.8742(3) 0.5403(3) 0.0523(3) 0.0354(10) Uani 1 1 d . . . H4 H 0.8862 0.4927 0.0170 0.042 Uiso 1 1 calc R . . C5 C 0.8649(3) 0.5335(3) 0.1422(3) 0.0279(9) Uani 1 1 d . . . H5 H 0.8694 0.4805 0.1776 0.033 Uiso 1 1 calc R . . C6 C 0.6293(3) 0.5037(3) 0.0503(3) 0.0252(8) Uani 1 1 d . . . C7 C 0.6035(3) 0.5936(3) 0.0591(3) 0.0265(8) Uani 1 1 d . . . H7 H 0.5929 0.6183 0.1123 0.032 Uiso 1 1 calc R . . C8 C 0.5963(3) 0.6394(3) -0.0247(3) 0.0323(9) Uani 1 1 d . . . H8 H 0.5802 0.7002 -0.0375 0.039 Uiso 1 1 calc R . . C9 C 0.6171(3) 0.5794(3) -0.0859(3) 0.0337(9) Uani 1 1 d . . . H9 H 0.6173 0.5930 -0.1473 0.040 Uiso 1 1 calc R . . C10 C 0.6377(3) 0.4956(3) -0.0411(3) 0.0306(9) Uani 1 1 d . . . H10 H 0.6541 0.4433 -0.0669 0.037 Uiso 1 1 calc R . . C11 C 0.6546(3) 0.4369(2) 0.1273(3) 0.0243(8) Uani 1 1 d . . . C12 C 0.8154(3) 0.7682(3) 0.2669(3) 0.0276(8) Uani 1 1 d . . . C13 C 0.9014(3) 0.8204(3) 0.2950(3) 0.0389(11) Uani 1 1 d . . . H13 H 0.9657 0.7935 0.3220 0.047 Uiso 1 1 calc R . . C14 C 0.8936(4) 0.9111(3) 0.2837(4) 0.0490(13) Uani 1 1 d . . . H14 H 0.9526 0.9461 0.3024 0.059 Uiso 1 1 calc R . . C15 C 0.8006(4) 0.9514(3) 0.2454(3) 0.0453(12) Uani 1 1 d . . . H15 H 0.7958 1.0139 0.2385 0.054 Uiso 1 1 calc R . . C16 C 0.7153(3) 0.9007(3) 0.2173(3) 0.0367(10) Uani 1 1 d . . . H16 H 0.6513 0.9282 0.1914 0.044 Uiso 1 1 calc R . . C17 C 0.7226(3) 0.8090(3) 0.2269(3) 0.0314(9) Uani 1 1 d . . . H17 H 0.6634 0.7741 0.2057 0.038 Uiso 1 1 calc R . . C18 C 0.9379(3) 0.6265(3) 0.3767(3) 0.0295(9) Uani 1 1 d . . . C19 C 0.9345(3) 0.6201(3) 0.4670(3) 0.0336(9) Uani 1 1 d . . . H19 H 0.8718 0.6238 0.4737 0.040 Uiso 1 1 calc R . . C20 C 1.0217(3) 0.6082(3) 0.5480(3) 0.0393(11) Uani 1 1 d . . . H20 H 1.0187 0.6050 0.6097 0.047 Uiso 1 1 calc R . . C21 C 1.1122(3) 0.6010(3) 0.5386(3) 0.0427(12) Uani 1 1 d . . . H21 H 1.1719 0.5931 0.5938 0.051 Uiso 1 1 calc R . . C22 C 1.1169(3) 0.6054(3) 0.4484(3) 0.0447(12) Uani 1 1 d . . . H22 H 1.1796 0.5999 0.4421 0.054 Uiso 1 1 calc R . . C23 C 1.0296(3) 0.6178(3) 0.3674(3) 0.0387(10) Uani 1 1 d . . . H23 H 1.0327 0.6203 0.3057 0.046 Uiso 1 1 calc R . . C24 C 0.6706(3) 0.2818(3) 0.1699(3) 0.0336(10) Uani 1 1 d . . . H24A H 0.6412 0.2266 0.1352 0.040 Uiso 1 1 calc R . . H24B H 0.6364 0.2952 0.2140 0.040 Uiso 1 1 calc R . . C25 C 0.7809(3) 0.2667(3) 0.2283(3) 0.0338(10) Uani 1 1 d . . . C26 C 0.8898(4) 0.1778(3) 0.3547(4) 0.0573(15) Uani 1 1 d . . . H26A H 0.9399 0.2039 0.3334 0.075 Uiso 1 1 calc R . . H26B H 0.8994 0.1136 0.3608 0.075 Uiso 1 1 calc R . . H26C H 0.8973 0.2029 0.4170 0.075 Uiso 1 1 calc R . . C30 C 0.5391(3) 0.5558(3) 0.3027(3) 0.0329(9) Uani 1 1 d . . . H30S H 0.5203 0.4957 0.3117 0.039 Uiso 1 1 d R . . H30A H 0.4861 0.5951 0.2401 0.039 Uiso 1 1 d R . . C31 C 0.6057(3) 0.5986(3) 0.3833(3) 0.0294(9) Uani 1 1 d . . . C32 C 0.6471(3) 0.6787(3) 0.3641(3) 0.0354(10) Uani 1 1 d . . . H32S H 0.7075 0.6966 0.4238 0.042 Uiso 1 1 d R . . H32A H 0.5974 0.7195 0.3133 0.042 Uiso 1 1 d R . . C33 C 0.6460(4) 0.5557(3) 0.4801(3) 0.0467(12) Uani 1 1 d . . . H33A H 0.6109 0.5791 0.5192 0.061 Uiso 1 1 calc R . . H33B H 0.7179 0.5683 0.5115 0.061 Uiso 1 1 calc R . . H33C H 0.6358 0.4916 0.4728 0.061 Uiso 1 1 calc R . . Cl Cl 0.42874(8) 0.70482(7) 0.60586(8) 0.0338(2) Uani 1 1 d . . . O4 O 0.4322(3) 0.7990(2) 0.6069(3) 0.0604(10) Uani 1 1 d . . . O5 O 0.4847(3) 0.6731(2) 0.7008(3) 0.0550(9) Uani 1 1 d . . . O6 O 0.3301(3) 0.6760(3) 0.5754(4) 0.0975(17) Uani 1 1 d . . . O7 O 0.4750(4) 0.6743(3) 0.5442(3) 0.0811(14) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd 0.02403(15) 0.02184(15) 0.02694(16) -0.00385(13) 0.01048(12) -0.00263(13) Fe 0.0186(3) 0.0290(3) 0.0212(3) 0.0000(2) 0.0035(2) -0.0017(2) P 0.0207(5) 0.0260(5) 0.0261(5) -0.0029(4) 0.0070(4) -0.0019(4) O1 0.0290(14) 0.0211(13) 0.0275(15) -0.0016(11) 0.0103(12) 0.0002(11) O2 0.0360(18) 0.047(2) 0.045(2) 0.0007(16) 0.0073(15) 0.0020(16) O3 0.055(2) 0.0284(17) 0.046(2) 0.0079(15) 0.0016(16) 0.0088(15) N 0.0327(19) 0.0236(17) 0.0289(18) -0.0042(14) 0.0055(15) 0.0002(15) C1 0.0135(17) 0.034(2) 0.027(2) -0.0033(17) 0.0041(15) -0.0059(16) C2 0.024(2) 0.033(2) 0.033(2) 0.0017(18) 0.0077(17) -0.0069(17) C3 0.028(2) 0.053(3) 0.030(2) 0.004(2) 0.0126(18) -0.005(2) C4 0.023(2) 0.050(3) 0.031(2) -0.006(2) 0.0090(17) 0.0023(19) C5 0.0192(19) 0.034(2) 0.026(2) -0.0003(17) 0.0027(15) 0.0040(16) C6 0.0197(18) 0.025(2) 0.027(2) -0.0029(16) 0.0038(15) -0.0053(15) C7 0.0184(18) 0.029(2) 0.030(2) 0.0017(17) 0.0060(15) -0.0016(16) C8 0.0193(19) 0.034(2) 0.035(2) 0.0090(19) 0.0007(17) -0.0003(17) C9 0.024(2) 0.046(3) 0.0216(19) 0.0035(19) -0.0016(16) -0.0078(19) C10 0.026(2) 0.034(2) 0.026(2) -0.0054(18) 0.0038(16) -0.0078(17) C11 0.0167(18) 0.026(2) 0.027(2) -0.0034(16) 0.0042(15) -0.0010(15) C12 0.028(2) 0.028(2) 0.027(2) -0.0037(16) 0.0100(16) -0.0071(17) C13 0.026(2) 0.040(3) 0.047(3) -0.004(2) 0.0100(19) -0.0104(19) C14 0.044(3) 0.041(3) 0.057(3) -0.004(2) 0.013(2) -0.022(2) C15 0.055(3) 0.031(2) 0.046(3) -0.001(2) 0.015(2) -0.011(2) C16 0.038(2) 0.032(2) 0.042(3) 0.0034(19) 0.017(2) 0.0026(19) C17 0.029(2) 0.028(2) 0.036(2) 0.0006(18) 0.0116(18) -0.0046(17) C18 0.026(2) 0.029(2) 0.028(2) -0.0022(17) 0.0052(16) 0.0004(17) C19 0.034(2) 0.032(2) 0.032(2) -0.0083(18) 0.0095(18) -0.0051(19) C20 0.045(3) 0.039(3) 0.025(2) -0.0030(19) 0.0031(19) -0.006(2) C21 0.036(3) 0.036(3) 0.037(3) -0.001(2) -0.007(2) -0.002(2) C22 0.029(2) 0.055(3) 0.039(3) 0.001(2) 0.0009(19) 0.000(2) C23 0.028(2) 0.050(3) 0.033(2) -0.002(2) 0.0047(18) -0.002(2) C24 0.037(2) 0.019(2) 0.041(2) -0.0024(18) 0.0112(19) 0.0015(18) C25 0.044(3) 0.021(2) 0.029(2) -0.0056(17) 0.0061(19) 0.0077(19) C26 0.067(4) 0.039(3) 0.042(3) 0.003(2) -0.005(3) 0.019(3) C30 0.026(2) 0.038(2) 0.039(2) -0.0003(19) 0.0159(18) -0.0023(18) C31 0.028(2) 0.033(2) 0.031(2) -0.0048(17) 0.0161(17) 0.0050(17) C32 0.039(2) 0.031(2) 0.039(2) -0.0107(19) 0.019(2) 0.0015(19) C33 0.054(3) 0.056(3) 0.032(2) 0.000(2) 0.018(2) 0.001(2) Cl 0.0317(5) 0.0267(5) 0.0372(6) 0.0064(4) 0.0069(4) -0.0026(4) O4 0.093(3) 0.0272(18) 0.050(2) 0.0083(16) 0.015(2) -0.0069(18) O5 0.050(2) 0.054(2) 0.053(2) 0.0271(18) 0.0096(17) 0.0047(17) O6 0.038(2) 0.097(4) 0.127(4) -0.002(3) -0.003(2) -0.027(2) O7 0.113(4) 0.080(3) 0.060(3) 0.006(2) 0.044(3) 0.034(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 C32 2.087(4) . ? Pd O1 2.142(3) . ? Pd C31 2.174(4) . ? Pd C30 2.210(4) . ? Pd P 2.3125(10) . ? Fe C6 2.013(4) . ? Fe C5 2.024(4) . ? Fe C10 2.027(4) . ? Fe C7 2.038(4) . ? Fe C1 2.038(4) . ? Fe C4 2.043(4) . ? Fe C2 2.047(4) . ? Fe C3 2.060(4) . ? Fe C9 2.063(4) . ? Fe C8 2.072(4) . ? P C1 1.805(4) . ? P C18 1.816(4) . ? P C12 1.827(4) . ? O1 C11 1.249(4) . ? O2 C25 1.191(5) . ? O3 C25 1.334(5) . ? O3 C26 1.438(5) . ? N C11 1.325(5) . ? N C24 1.439(5) . ? N H1N 0.8181 . ? C1 C5 1.433(6) . ? C1 C2 1.439(6) . ? C2 C3 1.409(6) . ? C2 H2 0.9500 . ? C3 C4 1.416(6) . ? C3 H3 0.9500 . ? C4 C5 1.418(6) . ? C4 H4 0.9500 . ? C5 H5 0.9500 . ? C6 C7 1.427(5) . ? C6 C10 1.436(5) . ? C6 C11 1.476(5) . ? C7 C8 1.410(6) . ? C7 H7 0.9500 . ? C8 C9 1.407(6) . ? C8 H8 0.9500 . ? C9 C10 1.412(6) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C12 C17 1.386(6) . ? C12 C13 1.394(5) . ? C13 C14 1.379(6) . ? C13 H13 0.9500 . ? C14 C15 1.384(7) . ? C14 H14 0.9500 . ? C15 C16 1.373(6) . ? C15 H15 0.9500 . ? C16 C17 1.392(6) . ? C16 H16 0.9500 . ? C17 H17 0.9500 . ? C18 C19 1.387(6) . ? C18 C23 1.391(6) . ? C19 C20 1.391(6) . ? C19 H19 0.9500 . ? C20 C21 1.372(7) . ? C20 H20 0.9500 . ? C21 C22 1.389(7) . ? C21 H21 0.9500 . ? C22 C23 1.393(6) . ? C22 H22 0.9500 . ? C23 H23 0.9500 . ? C24 C25 1.514(6) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C30 C31 1.389(6) . ? C30 H30S 0.9716 . ? C30 H30A 1.1302 . ? C31 C32 1.427(6) . ? C31 C33 1.497(6) . ? C32 H32S 1.0223 . ? C32 H32A 1.0301 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? Cl O6 1.389(4) . ? Cl O7 1.413(4) . ? Cl O4 1.423(3) . ? Cl O5 1.432(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C32 Pd O1 160.79(14) . . ? C32 Pd C31 39.07(16) . . ? O1 Pd C31 122.51(13) . . ? C32 Pd C30 66.96(16) . . ? O1 Pd C30 94.21(13) . . ? C31 Pd C30 36.92(15) . . ? C32 Pd P 97.37(12) . . ? O1 Pd P 101.76(7) . . ? C31 Pd P 131.98(11) . . ? C30 Pd P 162.98(12) . . ? C6 Fe C5 103.79(16) . . ? C6 Fe C10 41.62(15) . . ? C5 Fe C10 116.00(17) . . ? C6 Fe C7 41.25(15) . . ? C5 Fe C7 125.39(16) . . ? C10 Fe C7 68.94(16) . . ? C6 Fe C1 117.20(15) . . ? C5 Fe C1 41.32(16) . . ? C10 Fe C1 151.69(17) . . ? C7 Fe C1 108.04(15) . . ? C6 Fe C4 123.22(18) . . ? C5 Fe C4 40.82(16) . . ? C10 Fe C4 104.97(18) . . ? C7 Fe C4 162.16(17) . . ? C1 Fe C4 68.93(16) . . ? C6 Fe C2 154.28(16) . . ? C5 Fe C2 69.07(17) . . ? C10 Fe C2 163.94(16) . . ? C7 Fe C2 121.85(16) . . ? C1 Fe C2 41.25(15) . . ? C4 Fe C2 68.24(18) . . ? C6 Fe C3 161.79(18) . . ? C5 Fe C3 68.39(17) . . ? C10 Fe C3 125.54(17) . . ? C7 Fe C3 156.44(17) . . ? C1 Fe C3 68.50(16) . . ? C4 Fe C3 40.36(18) . . ? C2 Fe C3 40.14(17) . . ? C6 Fe C9 68.66(16) . . ? C5 Fe C9 151.78(17) . . ? C10 Fe C9 40.36(17) . . ? C7 Fe C9 67.60(16) . . ? C1 Fe C9 166.46(18) . . ? C4 Fe C9 119.29(17) . . ? C2 Fe C9 129.04(17) . . ? C3 Fe C9 110.01(17) . . ? C6 Fe C8 68.53(16) . . ? C5 Fe C8 164.38(17) . . ? C10 Fe C8 67.94(17) . . ? C7 Fe C8 40.11(15) . . ? C1 Fe C8 128.82(17) . . ? C4 Fe C8 154.74(17) . . ? C2 Fe C8 111.61(17) . . ? C3 Fe C8 122.88(17) . . ? C9 Fe C8 39.78(17) . . ? C1 P C18 105.20(18) . . ? C1 P C12 100.70(19) . . ? C18 P C12 103.74(18) . . ? C1 P Pd 115.87(12) . . ? C18 P Pd 114.37(14) . . ? C12 P Pd 115.27(13) . . ? C11 O1 Pd 133.1(2) . . ? C25 O3 C26 117.5(4) . . ? C11 N C24 121.9(3) . . ? C11 N H1N 121.6 . . ? C24 N H1N 116.1 . . ? C5 C1 C2 106.9(3) . . ? C5 C1 P 126.0(3) . . ? C2 C1 P 126.8(3) . . ? C5 C1 Fe 68.8(2) . . ? C2 C1 Fe 69.7(2) . . ? P C1 Fe 122.21(19) . . ? C3 C2 C1 108.1(4) . . ? C3 C2 Fe 70.4(2) . . ? C1 C2 Fe 69.0(2) . . ? C3 C2 H2 125.9 . . ? C1 C2 H2 125.9 . . ? Fe C2 H2 126.2 . . ? C2 C3 C4 108.6(4) . . ? C2 C3 Fe 69.4(2) . . ? C4 C3 Fe 69.2(2) . . ? C2 C3 H3 125.7 . . ? C4 C3 H3 125.7 . . ? Fe C3 H3 127.3 . . ? C3 C4 C5 108.2(4) . . ? C3 C4 Fe 70.5(2) . . ? C5 C4 Fe 68.9(2) . . ? C3 C4 H4 125.9 . . ? C5 C4 H4 125.9 . . ? Fe C4 H4 126.3 . . ? C4 C5 C1 108.1(4) . . ? C4 C5 Fe 70.3(2) . . ? C1 C5 Fe 69.9(2) . . ? C4 C5 H5 125.9 . . ? C1 C5 H5 125.9 . . ? Fe C5 H5 125.5 . . ? C7 C6 C10 107.0(3) . . ? C7 C6 C11 124.9(3) . . ? C10 C6 C11 127.7(4) . . ? C7 C6 Fe 70.3(2) . . ? C10 C6 Fe 69.7(2) . . ? C11 C6 Fe 119.3(3) . . ? C8 C7 C6 108.4(4) . . ? C8 C7 Fe 71.3(2) . . ? C6 C7 Fe 68.5(2) . . ? C8 C7 H7 125.8 . . ? C6 C7 H7 125.8 . . ? Fe C7 H7 126.0 . . ? C9 C8 C7 108.2(4) . . ? C9 C8 Fe 69.8(2) . . ? C7 C8 Fe 68.6(2) . . ? C9 C8 H8 125.9 . . ? C7 C8 H8 125.9 . . ? Fe C8 H8 127.3 . . ? C8 C9 C10 108.8(4) . . ? C8 C9 Fe 70.5(2) . . ? C10 C9 Fe 68.5(2) . . ? C8 C9 H9 125.6 . . ? C10 C9 H9 125.6 . . ? Fe C9 H9 127.0 . . ? C9 C10 C6 107.7(4) . . ? C9 C10 Fe 71.2(2) . . ? C6 C10 Fe 68.7(2) . . ? C9 C10 H10 126.1 . . ? C6 C10 H10 126.1 . . ? Fe C10 H10 125.6 . . ? O1 C11 N 120.1(4) . . ? O1 C11 C6 122.8(3) . . ? N C11 C6 117.1(3) . . ? C17 C12 C13 118.7(4) . . ? C17 C12 P 119.2(3) . . ? C13 C12 P 122.0(3) . . ? C14 C13 C12 120.2(4) . . ? C14 C13 H13 119.9 . . ? C12 C13 H13 119.9 . . ? C13 C14 C15 120.6(4) . . ? C13 C14 H14 119.7 . . ? C15 C14 H14 119.7 . . ? C16 C15 C14 119.7(4) . . ? C16 C15 H15 120.1 . . ? C14 C15 H15 120.1 . . ? C15 C16 C17 120.0(4) . . ? C15 C16 H16 120.0 . . ? C17 C16 H16 120.0 . . ? C12 C17 C16 120.7(4) . . ? C12 C17 H17 119.7 . . ? C16 C17 H17 119.7 . . ? C19 C18 C23 119.1(4) . . ? C19 C18 P 118.1(3) . . ? C23 C18 P 122.8(3) . . ? C18 C19 C20 120.8(4) . . ? C18 C19 H19 119.6 . . ? C20 C19 H19 119.6 . . ? C21 C20 C19 119.8(4) . . ? C21 C20 H20 120.1 . . ? C19 C20 H20 120.1 . . ? C20 C21 C22 120.2(4) . . ? C20 C21 H21 119.9 . . ? C22 C21 H21 119.9 . . ? C21 C22 C23 120.0(5) . . ? C21 C22 H22 120.0 . . ? C23 C22 H22 120.0 . . ? C18 C23 C22 120.0(4) . . ? C18 C23 H23 120.0 . . ? C22 C23 H23 120.0 . . ? N C24 C25 113.4(4) . . ? N C24 H24A 108.9 . . ? C25 C24 H24A 108.9 . . ? N C24 H24B 108.9 . . ? C25 C24 H24B 108.9 . . ? H24A C24 H24B 107.7 . . ? O2 C25 O3 124.8(4) . . ? O2 C25 C24 126.1(4) . . ? O3 C25 C24 109.0(4) . . ? O3 C26 H26A 109.5 . . ? O3 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? O3 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C31 C30 Pd 70.1(2) . . ? C31 C30 H30S 116.7 . . ? Pd C30 H30S 119.5 . . ? C31 C30 H30A 120.5 . . ? Pd C30 H30A 100.5 . . ? H30S C30 H30A 118.2 . . ? C30 C31 C32 114.8(4) . . ? C30 C31 C33 122.2(4) . . ? C32 C31 C33 121.9(4) . . ? C30 C31 Pd 73.0(2) . . ? C32 C31 Pd 67.2(2) . . ? C33 C31 Pd 119.6(3) . . ? C31 C32 Pd 73.8(2) . . ? C31 C32 H32S 109.1 . . ? Pd C32 H32S 112.2 . . ? C31 C32 H32A 115.6 . . ? Pd C32 H32A 105.0 . . ? H32S C32 H32A 127.9 . . ? C31 C33 H33A 109.5 . . ? C31 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C31 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? O6 Cl O7 111.3(3) . . ? O6 Cl O4 110.1(3) . . ? O7 Cl O4 108.1(3) . . ? O6 Cl O5 109.9(3) . . ? O7 Cl O5 108.8(2) . . ? O4 Cl O5 108.7(2) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.52 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 2.020 _refine_diff_density_min -1.145 _refine_diff_density_rms 0.105 #===END