# Electronic Supplementary Material (ESI) for RSC Advances # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name _publ_author_address C.Lopez ; Departament de Qu\'imica Inorg\`anica Universitat de Barcelona Mart\'i i Franqu\`es 1 E-08028-Barcelona Spain ; A.Gonzalez ; Laboratori de Qu\'imica Org\`anica Facultat de Farm\`acia Universitat de Barcelona Pl. Pius XII s/n E-08028-Barcelona Spain ; R.Bosque ; Departament de Qu\'imica Inorg\`anica Universitat de Barcelona Mart\'i i Franqu\`es 1 E-08028-Barcelona Spain ; 'Pradipta Kumar Basu' ; Laboratori de Qu mica Organica, Facultat de Farmacia, Universitat de Barcelona, Pl. Pius XII s/n. E-08028-Barcelona Spain. ; M.Font-Bardia ; Departament de Cristal.lografia Universitat de Barcelona Mart\'i i Franqu\`es, sn E-08028 Barcelona Spain ; T.Calvet ; Departament de Cristal.lografia Universitat de Barcelona Mart\'i i Franqu\`es, sn E-08028 Barcelona Spain ; #TrackingRef 'TOT.CIF' # 3. TITLE AND AUTHOR LIST _publ_section_title ; 'Platinum(II) and Palladium(II) Complexes derived from 1-Ferrocenylmethyl-3,5-diphenylpyrazole. Coordination, Cyclometallation or Transannulation?' ; _publ_contact_author_email mercef@sct.ub.es _publ_contact_author_name 'Merce Font-Bardia' data_chnm14a _database_code_depnum_ccdc_archive 'CCDC 826854' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H22 Fe N2' _chemical_formula_sum 'C26 H22 Fe N2' _chemical_formula_weight 418.31 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' Fe Fe 0.3463 0.8444 '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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.345(7) _cell_length_b 10.589(6) _cell_length_c 11.221(4) _cell_angle_alpha 67.47(4) _cell_angle_beta 67.79(4) _cell_angle_gamma 82.84(5) _cell_volume 1050.8(10) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1237 _cell_measurement_theta_min 3 _cell_measurement_theta_max 31 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.322 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 436 _exptl_absorpt_coefficient_mu 0.731 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.92 _exptl_absorpt_correction_T_max 0.94 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'MAR345 with image plate detector' _diffrn_measurement_method 'phi scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10793 _diffrn_reflns_av_R_equivalents 0.0606 _diffrn_reflns_av_sigmaI/netI 0.0573 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.66 _diffrn_reflns_theta_max 32.98 _reflns_number_total 5687 _reflns_number_gt 4029 _reflns_threshold_expression >2sigma(I) _computing_data_collection MARXDS _computing_cell_refinement AUTOMAR _computing_data_reduction MARSCALE _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP (Brueggermann and Smith, 1990)' _computing_publication_material 'PLATON (Spek, 1990)' _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^)+(0.0863P)^2^+0.3321P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.029(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 5687 _refine_ls_number_parameters 263 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0827 _refine_ls_R_factor_gt 0.0568 _refine_ls_wR_factor_ref 0.1949 _refine_ls_wR_factor_gt 0.1841 _refine_ls_goodness_of_fit_ref 1.130 _refine_ls_restrained_S_all 1.130 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe Fe 0.61784(4) -0.00088(4) 0.21519(5) 0.05372(18) Uani 1 1 d U . . N1 N 0.5306(3) 0.3722(3) 0.1464(3) 0.0504(5) Uani 1 1 d . . . N2 N 0.3981(3) 0.3176(3) 0.2059(3) 0.0534(6) Uani 1 1 d . . . C1 C 0.4184(4) -0.0285(4) 0.3594(4) 0.0666(9) Uani 1 1 d . . . H1 H 0.3751 0.0287 0.4080 0.080 Uiso 1 1 calc R . . C2 C 0.4170(4) -0.0095(4) 0.2287(4) 0.0633(8) Uani 1 1 d U . . H2 H 0.3751 0.0603 0.1758 0.076 Uiso 1 1 calc R . . C3 C 0.4930(4) -0.1195(4) 0.1952(5) 0.0743(10) Uani 1 1 d U . . H3 H 0.5085 -0.1353 0.1149 0.089 Uiso 1 1 calc R . . C4 C 0.5420(4) -0.2021(4) 0.3024(5) 0.0764(10) Uani 1 1 d . . . H4 H 0.5959 -0.2794 0.3030 0.092 Uiso 1 1 calc R . . C5 C 0.4953(4) -0.1475(4) 0.4086(4) 0.0715(9) Uani 1 1 d . . . H5 H 0.5109 -0.1811 0.4916 0.086 Uiso 1 1 calc R . . C6 C 0.7603(4) 0.1124(4) 0.0207(4) 0.0683(8) Uani 1 1 d U . . H6 H 0.7589 0.1217 -0.0647 0.082 Uiso 1 1 calc R . . C7 C 0.8265(4) 0.0021(4) 0.1042(5) 0.0791(9) Uani 1 1 d U . . H7 H 0.8740 -0.0699 0.0796 0.095 Uiso 1 1 calc R . . C8 C 0.8072(4) 0.0218(4) 0.2280(5) 0.0751(8) Uani 1 1 d U . . H8 H 0.8389 -0.0328 0.2985 0.090 Uiso 1 1 calc R . . C9 C 0.7294(4) 0.1426(4) 0.2212(4) 0.0589(7) Uani 1 1 d U . . H9 H 0.7006 0.1804 0.2893 0.071 Uiso 1 1 calc R . . C10 C 0.6997(3) 0.2010(3) 0.0917(3) 0.0529(7) Uani 1 1 d . . . C11 C 0.6320(3) 0.3345(3) 0.0355(3) 0.0538(7) Uani 1 1 d . . . H1A H 0.7034 0.4061 -0.0217 0.065 Uiso 1 1 calc R . . H1B H 0.5862 0.3255 -0.0221 0.065 Uiso 1 1 calc R . . C12 C 0.5537(3) 0.4451(3) 0.2115(3) 0.0493(6) Uani 1 1 d . . . C13 C 0.4255(3) 0.4388(3) 0.3172(3) 0.0570(7) Uani 1 1 d . . . H13 H 0.4046 0.4818 0.3805 0.068 Uiso 1 1 calc R . . C14 C 0.3344(3) 0.3571(3) 0.3116(3) 0.0508(6) Uani 1 1 d . . . C15 C 0.1855(3) 0.3110(3) 0.4061(3) 0.0547(7) Uani 1 1 d . . . C16 C 0.1199(4) 0.3447(4) 0.5189(4) 0.0723(10) Uani 1 1 d . . . H16 H 0.1670 0.3986 0.5390 0.087 Uiso 1 1 calc R . . C17 C -0.0167(4) 0.3006(5) 0.6056(5) 0.0832(12) Uani 1 1 d . . . H17 H -0.0576 0.3244 0.6832 0.100 Uiso 1 1 calc R . . C18 C -0.0929(4) 0.2233(5) 0.5803(5) 0.0769(10) Uani 1 1 d . . . H18 H -0.1855 0.1980 0.6365 0.092 Uiso 1 1 calc R . . C19 C -0.0267(4) 0.1851(5) 0.4690(5) 0.0780(11) Uani 1 1 d . . . H19 H -0.0744 0.1303 0.4504 0.094 Uiso 1 1 calc R . . C20 C 0.1128(4) 0.2271(4) 0.3814(4) 0.0706(9) Uani 1 1 d . . . H20 H 0.1563 0.1987 0.3070 0.085 Uiso 1 1 calc R . . C21 C 0.6903(3) 0.5107(3) 0.1695(3) 0.0527(7) Uani 1 1 d . . . C22 C 0.7597(3) 0.4649(4) 0.2646(4) 0.0588(7) Uani 1 1 d . . . H22 H 0.7192 0.3967 0.3506 0.071 Uiso 1 1 calc R . . C23 C 0.8896(4) 0.5225(4) 0.2287(5) 0.0726(9) Uani 1 1 d . . . H23 H 0.9377 0.4911 0.2895 0.087 Uiso 1 1 calc R . . C24 C 0.9476(4) 0.6295(4) 0.0982(4) 0.0726(10) Uani 1 1 d . . . H24 H 1.0332 0.6685 0.0768 0.087 Uiso 1 1 calc R . . C25 C 0.8830(4) 0.6789(5) 0.0011(4) 0.0774(11) Uani 1 1 d . . . H25 H 0.9242 0.7482 -0.0839 0.093 Uiso 1 1 calc R . . C26 C 0.7535(4) 0.6199(4) 0.0368(4) 0.0661(8) Uani 1 1 d . . . H26 H 0.7070 0.6510 -0.0254 0.079 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 Fe 0.0483(3) 0.0503(3) 0.0588(3) -0.0207(2) -0.01381(19) -0.00146(17) N1 0.0452(12) 0.0478(13) 0.0568(13) -0.0189(11) -0.0164(10) -0.0012(9) N2 0.0468(12) 0.0523(14) 0.0595(14) -0.0206(11) -0.0163(11) -0.0022(10) C1 0.0563(18) 0.063(2) 0.070(2) -0.0247(17) -0.0097(15) -0.0028(14) C2 0.0525(17) 0.065(2) 0.070(2) -0.0199(15) -0.0202(15) -0.0104(13) C3 0.068(2) 0.075(2) 0.079(2) -0.035(2) -0.0151(18) -0.0126(16) C4 0.070(2) 0.059(2) 0.092(3) -0.029(2) -0.018(2) -0.0038(17) C5 0.069(2) 0.067(2) 0.067(2) -0.0167(17) -0.0174(17) -0.0082(17) C6 0.0591(18) 0.068(2) 0.0677(17) -0.0287(15) -0.0042(14) -0.0118(14) C7 0.059(2) 0.070(2) 0.100(2) -0.0386(17) -0.0125(18) 0.0038(15) C8 0.0608(17) 0.0660(19) 0.103(2) -0.0285(18) -0.0368(19) 0.0030(14) C9 0.0566(17) 0.0579(17) 0.0638(18) -0.0204(13) -0.0237(14) -0.0039(11) C10 0.0465(14) 0.0523(17) 0.0549(15) -0.0195(13) -0.0108(12) -0.0067(12) C11 0.0513(15) 0.0568(17) 0.0519(15) -0.0206(13) -0.0138(12) -0.0067(12) C12 0.0475(14) 0.0469(16) 0.0531(15) -0.0176(12) -0.0182(12) -0.0002(11) C13 0.0537(16) 0.0557(18) 0.0600(17) -0.0214(14) -0.0181(14) -0.0007(13) C14 0.0495(15) 0.0479(16) 0.0535(15) -0.0174(12) -0.0185(12) 0.0024(11) C15 0.0485(15) 0.0518(17) 0.0599(17) -0.0172(13) -0.0181(13) -0.0006(12) C16 0.061(2) 0.079(3) 0.077(2) -0.036(2) -0.0153(17) -0.0044(17) C17 0.069(2) 0.089(3) 0.085(3) -0.037(2) -0.012(2) -0.005(2) C18 0.059(2) 0.078(3) 0.084(3) -0.025(2) -0.0169(19) -0.0068(18) C19 0.065(2) 0.080(3) 0.088(3) -0.032(2) -0.022(2) -0.0078(18) C20 0.0597(19) 0.075(2) 0.078(2) -0.0321(19) -0.0190(17) -0.0054(16) C21 0.0472(14) 0.0525(17) 0.0589(16) -0.0224(13) -0.0173(13) 0.0006(12) C22 0.0569(17) 0.0576(19) 0.0638(18) -0.0223(15) -0.0233(14) 0.0002(13) C23 0.065(2) 0.073(2) 0.087(2) -0.034(2) -0.0307(19) 0.0014(17) C24 0.059(2) 0.077(3) 0.086(2) -0.037(2) -0.0200(18) -0.0087(17) C25 0.072(2) 0.080(3) 0.073(2) -0.0231(19) -0.0173(19) -0.0185(19) C26 0.065(2) 0.066(2) 0.0670(19) -0.0236(16) -0.0219(16) -0.0068(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe C3 2.034(4) . ? Fe C2 2.037(4) . ? Fe C7 2.041(4) . ? Fe C9 2.054(4) . ? Fe C1 2.055(4) . ? Fe C8 2.067(4) . ? Fe C4 2.086(4) . ? Fe C6 2.092(4) . ? Fe C10 2.121(3) . ? Fe C5 2.134(4) . ? N1 C12 1.340(4) . ? N1 N2 1.367(4) . ? N1 C11 1.449(4) . ? N2 C14 1.318(4) . ? C1 C2 1.407(5) . ? C1 C5 1.441(6) . ? C1 H1 0.9300 . ? C2 C3 1.414(6) . ? C2 H2 0.9300 . ? C3 C4 1.420(6) . ? C3 H3 0.9300 . ? C4 C5 1.417(6) . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? C6 C10 1.399(5) . ? C6 C7 1.469(6) . ? C6 H6 0.9300 . ? C7 C8 1.420(6) . ? C7 H7 0.9300 . ? C8 C9 1.416(5) . ? C8 H8 0.9300 . ? C9 C10 1.480(5) . ? C9 H9 0.9300 . ? C10 C11 1.513(5) . ? C11 H1A 0.9700 . ? C11 H1B 0.9700 . ? C12 C13 1.393(4) . ? C12 C21 1.480(4) . ? C13 C14 1.390(5) . ? C13 H13 0.9300 . ? C14 C15 1.514(4) . ? C15 C16 1.351(5) . ? C15 C20 1.394(5) . ? C16 C17 1.392(6) . ? C16 H16 0.9300 . ? C17 C18 1.372(6) . ? C17 H17 0.9300 . ? C18 C19 1.365(6) . ? C18 H18 0.9300 . ? C19 C20 1.415(5) . ? C19 H19 0.9300 . ? C20 H20 0.9300 . ? C21 C22 1.409(5) . ? C21 C26 1.454(5) . ? C22 C23 1.395(5) . ? C22 H22 0.9300 . ? C23 C24 1.422(6) . ? C23 H23 0.9300 . ? C24 C25 1.391(6) . ? C24 H24 0.9300 . ? C25 C26 1.399(5) . ? C25 H25 0.9300 . ? C26 H26 0.9300 . ? 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 C3 Fe C2 40.66(16) . . ? C3 Fe C7 116.78(18) . . ? C2 Fe C7 148.99(18) . . ? C3 Fe C9 171.66(16) . . ? C2 Fe C9 132.64(15) . . ? C7 Fe C9 66.74(17) . . ? C3 Fe C1 66.44(17) . . ? C2 Fe C1 40.23(16) . . ? C7 Fe C1 168.72(18) . . ? C9 Fe C1 111.70(16) . . ? C3 Fe C8 147.27(18) . . ? C2 Fe C8 170.09(16) . . ? C7 Fe C8 40.44(18) . . ? C9 Fe C8 40.19(15) . . ? C1 Fe C8 131.10(18) . . ? C3 Fe C4 40.30(18) . . ? C2 Fe C4 68.43(17) . . ? C7 Fe C4 108.62(18) . . ? C9 Fe C4 147.39(17) . . ? C1 Fe C4 66.23(17) . . ? C8 Fe C4 114.62(18) . . ? C3 Fe C6 110.00(17) . . ? C2 Fe C6 116.26(17) . . ? C7 Fe C6 41.62(18) . . ? C9 Fe C6 67.09(15) . . ? C1 Fe C6 149.20(17) . . ? C8 Fe C6 69.33(18) . . ? C4 Fe C6 132.22(17) . . ? C3 Fe C10 131.46(16) . . ? C2 Fe C10 109.17(15) . . ? C7 Fe C10 67.84(16) . . ? C9 Fe C10 41.47(13) . . ? C1 Fe C10 119.02(15) . . ? C8 Fe C10 69.57(16) . . ? C4 Fe C10 169.56(15) . . ? C6 Fe C10 38.79(14) . . ? C3 Fe C5 67.14(17) . . ? C2 Fe C5 68.71(17) . . ? C7 Fe C5 129.58(18) . . ? C9 Fe C5 117.17(16) . . ? C1 Fe C5 40.17(16) . . ? C8 Fe C5 107.25(18) . . ? C4 Fe C5 39.21(17) . . ? C6 Fe C5 169.51(16) . . ? C10 Fe C5 150.49(15) . . ? C12 N1 N2 113.1(2) . . ? C12 N1 C11 127.4(3) . . ? N2 N1 C11 119.0(2) . . ? C14 N2 N1 105.8(2) . . ? C2 C1 C5 111.6(4) . . ? C2 C1 Fe 69.2(2) . . ? C5 C1 Fe 72.9(2) . . ? C2 C1 H1 124.2 . . ? C5 C1 H1 124.2 . . ? Fe C1 H1 125.3 . . ? C1 C2 C3 105.1(4) . . ? C1 C2 Fe 70.6(2) . . ? C3 C2 Fe 69.6(2) . . ? C1 C2 H2 127.4 . . ? C3 C2 H2 127.4 . . ? Fe C2 H2 124.1 . . ? C2 C3 C4 109.8(4) . . ? C2 C3 Fe 69.8(2) . . ? C4 C3 Fe 71.8(2) . . ? C2 C3 H3 125.1 . . ? C4 C3 H3 125.1 . . ? Fe C3 H3 124.9 . . ? C5 C4 C3 108.8(4) . . ? C5 C4 Fe 72.2(2) . . ? C3 C4 Fe 67.9(2) . . ? C5 C4 H4 125.6 . . ? C3 C4 H4 125.6 . . ? Fe C4 H4 125.8 . . ? C4 C5 C1 104.7(4) . . ? C4 C5 Fe 68.6(2) . . ? C1 C5 Fe 67.0(2) . . ? C4 C5 H5 127.6 . . ? C1 C5 H5 127.6 . . ? Fe C5 H5 128.3 . . ? C10 C6 C7 108.2(4) . . ? C10 C6 Fe 71.7(2) . . ? C7 C6 Fe 67.3(2) . . ? C10 C6 H6 125.9 . . ? C7 C6 H6 125.9 . . ? Fe C6 H6 126.6 . . ? C8 C7 C6 109.9(3) . . ? C8 C7 Fe 70.8(2) . . ? C6 C7 Fe 71.1(2) . . ? C8 C7 H7 125.0 . . ? C6 C7 H7 125.0 . . ? Fe C7 H7 124.7 . . ? C9 C8 C7 105.2(4) . . ? C9 C8 Fe 69.4(2) . . ? C7 C8 Fe 68.8(2) . . ? C9 C8 H8 127.4 . . ? C7 C8 H8 127.4 . . ? Fe C8 H8 126.0 . . ? C8 C9 C10 111.3(3) . . ? C8 C9 Fe 70.4(2) . . ? C10 C9 Fe 71.71(18) . . ? C8 C9 H9 124.4 . . ? C10 C9 H9 124.4 . . ? Fe C9 H9 125.1 . . ? C6 C10 C9 105.4(3) . . ? C6 C10 C11 125.0(3) . . ? C9 C10 C11 129.3(3) . . ? C6 C10 Fe 69.5(2) . . ? C9 C10 Fe 66.82(18) . . ? C11 C10 Fe 132.4(2) . . ? N1 C11 C10 111.2(3) . . ? N1 C11 H1A 109.4 . . ? C10 C11 H1A 109.4 . . ? N1 C11 H1B 109.4 . . ? C10 C11 H1B 109.4 . . ? H1A C11 H1B 108.0 . . ? N1 C12 C13 103.7(3) . . ? N1 C12 C21 123.3(3) . . ? C13 C12 C21 133.0(3) . . ? C14 C13 C12 108.1(3) . . ? C14 C13 H13 126.0 . . ? C12 C13 H13 126.0 . . ? N2 C14 C13 109.2(3) . . ? N2 C14 C15 120.8(3) . . ? C13 C14 C15 129.9(3) . . ? C16 C15 C20 117.6(3) . . ? C16 C15 C14 122.0(3) . . ? C20 C15 C14 120.3(3) . . ? C15 C16 C17 121.4(4) . . ? C15 C16 H16 119.3 . . ? C17 C16 H16 119.3 . . ? C18 C17 C16 122.2(4) . . ? C18 C17 H17 118.9 . . ? C16 C17 H17 118.9 . . ? C19 C18 C17 117.0(4) . . ? C19 C18 H18 121.5 . . ? C17 C18 H18 121.5 . . ? C18 C19 C20 121.4(4) . . ? C18 C19 H19 119.3 . . ? C20 C19 H19 119.3 . . ? C15 C20 C19 120.2(4) . . ? C15 C20 H20 119.9 . . ? C19 C20 H20 119.9 . . ? C22 C21 C26 119.4(3) . . ? C22 C21 C12 117.6(3) . . ? C26 C21 C12 123.0(3) . . ? C23 C22 C21 119.6(3) . . ? C23 C22 H22 120.2 . . ? C21 C22 H22 120.2 . . ? C22 C23 C24 119.3(4) . . ? C22 C23 H23 120.4 . . ? C24 C23 H23 120.4 . . ? C25 C24 C23 123.3(4) . . ? C25 C24 H24 118.3 . . ? C23 C24 H24 118.3 . . ? C24 C25 C26 117.2(4) . . ? C24 C25 H25 121.4 . . ? C26 C25 H25 121.4 . . ? C25 C26 C21 121.1(4) . . ? C25 C26 H26 119.4 . . ? C21 C26 H26 119.4 . . ? _diffrn_measured_fraction_theta_max 0.719 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.930 _refine_diff_density_max 0.377 _refine_diff_density_min -0.333 _refine_diff_density_rms 0.074 #==END data_chmm114a1 _database_code_depnum_ccdc_archive 'CCDC 826855' #TrackingRef 'TOT.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H28 Cl2 Fe N2 O Pt S' _chemical_formula_sum 'C28 H28 Cl2 Fe N2 O Pt S' _chemical_formula_weight 762.42 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' Fe Fe 0.3463 0.8444 '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' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 15.865(4) _cell_length_b 13.213(6) _cell_length_c 26.348(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5523(4) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 1203 _cell_measurement_theta_min 3 _cell_measurement_theta_max 31 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.834 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2976 _exptl_absorpt_coefficient_mu 5.879 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.49 _exptl_absorpt_correction_T_max 0.55 _exptl_absorpt_process_details SADABS _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_type 'MAR345 with image plate detector' _diffrn_measurement_method 'phi scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 38751 _diffrn_reflns_av_R_equivalents 0.0833 _diffrn_reflns_av_sigmaI/netI 0.0417 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -39 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 2.57 _diffrn_reflns_theta_max 32.53 _reflns_number_total 7641 _reflns_number_gt 6900 _reflns_threshold_expression >2sigma(I) _computing_data_collection MARXDS _computing_cell_refinement AUTOMAR _computing_data_reduction MARSCALE _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP (Brueggermann and Smith, 1990)' _computing_publication_material 'PLATON (Spek, 1990)' _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^)+(0.0746P)^2^+1.9662P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7641 _refine_ls_number_parameters 327 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0440 _refine_ls_R_factor_gt 0.0414 _refine_ls_wR_factor_ref 0.1174 _refine_ls_wR_factor_gt 0.1148 _refine_ls_goodness_of_fit_ref 1.083 _refine_ls_restrained_S_all 1.083 _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 Pt Pt -0.042018(8) 0.519844(9) 0.214425(4) 0.03849(7) Uani 1 1 d . . . Fe Fe 0.14129(3) 0.23089(4) 0.10042(2) 0.04494(12) Uani 1 1 d . . . Cl1 Cl 0.01263(9) 0.55926(12) 0.29204(3) 0.0691(3) Uani 1 1 d . . . Cl2 Cl -0.15446(6) 0.43781(7) 0.25257(3) 0.0531(2) Uani 1 1 d . . . S1 S 0.05836(6) 0.60872(7) 0.17754(3) 0.04798(18) Uani 1 1 d . . . O1 O 0.0636(2) 0.6056(2) 0.12208(10) 0.0554(6) Uani 1 1 d . . . N1 N -0.09036(18) 0.48227(18) 0.14601(9) 0.0364(5) Uani 1 1 d . . . N2 N -0.08319(17) 0.38814(19) 0.12536(9) 0.0375(5) Uani 1 1 d . . . C1 C 0.1858(3) 0.1572(3) 0.03754(14) 0.0536(8) Uani 1 1 d . . . H1 H 0.2160 0.1860 0.0110 0.064 Uiso 1 1 d R . . C2 C 0.2204(3) 0.1142(3) 0.08191(14) 0.0522(8) Uani 1 1 d . . . H2 H 0.2775 0.1099 0.0895 0.063 Uiso 1 1 d R . . C3 C 0.1539(3) 0.0791(3) 0.11290(13) 0.0503(8) Uani 1 1 d . . . H3 H 0.1593 0.0477 0.1443 0.060 Uiso 1 1 d R . . C4 C 0.0772(2) 0.1006(3) 0.08713(14) 0.0481(7) Uani 1 1 d . . . H4 H 0.0234 0.0857 0.0990 0.058 Uiso 1 1 d R . . C5 C 0.0964(3) 0.1486(3) 0.04062(14) 0.0542(8) Uani 1 1 d . . . H5 H 0.0578 0.1704 0.0164 0.065 Uiso 1 1 d R . . C6 C 0.0952(3) 0.3741(3) 0.09359(19) 0.0592(10) Uani 1 1 d . . . H6 H 0.0638 0.3990 0.0665 0.071 Uiso 1 1 d R . . C7 C 0.1843(3) 0.3761(3) 0.0976(3) 0.0840(18) Uani 1 1 d . . . H7 H 0.2215 0.4024 0.0738 0.101 Uiso 1 1 d R . . C8 C 0.2060(3) 0.3317(5) 0.1435(3) 0.0845(18) Uani 1 1 d . . . H8 H 0.2607 0.3236 0.1556 0.101 Uiso 1 1 d R . . C9 C 0.1306(3) 0.3003(4) 0.1693(2) 0.0701(13) Uani 1 1 d . . . H9 H 0.1274 0.2682 0.2006 0.084 Uiso 1 1 d R . . C10 C 0.0624(3) 0.3280(3) 0.13763(15) 0.0506(8) Uani 1 1 d . . . C11 C -0.0303(2) 0.3115(2) 0.14858(11) 0.0409(6) Uani 1 1 d . . . H11A H -0.0469 0.2455 0.1360 0.049 Uiso 1 1 calc R . . H11B H -0.0391 0.3122 0.1850 0.049 Uiso 1 1 calc R . . C12 C -0.1160(2) 0.3895(2) 0.07755(11) 0.0395(6) Uani 1 1 d . . . C13 C -0.1177(2) 0.2981(3) 0.04454(13) 0.0443(7) Uani 1 1 d . . . C14 C -0.1483(2) 0.2067(3) 0.06272(14) 0.0496(7) Uani 1 1 d . . . H14 H -0.1682 0.2024 0.0958 0.060 Uiso 1 1 calc R . . C15 C -0.1493(3) 0.1212(3) 0.03173(18) 0.0614(10) Uani 1 1 d . . . H15 H -0.1672 0.0592 0.0445 0.074 Uiso 1 1 calc R . . C16 C -0.1235(3) 0.1297(3) -0.01817(18) 0.0619(11) Uani 1 1 d . . . H16 H -0.1247 0.0733 -0.0393 0.074 Uiso 1 1 calc R . . C17 C -0.0960(3) 0.2210(3) -0.03675(14) 0.0582(10) Uani 1 1 d . . . H17 H -0.0790 0.2259 -0.0705 0.070 Uiso 1 1 calc R . . C18 C -0.0931(2) 0.3064(3) -0.00580(12) 0.0481(7) Uani 1 1 d . . . H18 H -0.0750 0.3681 -0.0187 0.058 Uiso 1 1 calc R . . C19 C -0.1444(2) 0.4852(2) 0.06764(13) 0.0429(7) Uani 1 1 d . . . H19 H -0.1688 0.5084 0.0377 0.051 Uiso 1 1 calc R . . C20 C -0.1291(2) 0.5414(3) 0.11215(12) 0.0418(6) Uani 1 1 d . . . C21 C -0.1496(2) 0.6466(3) 0.12403(13) 0.0470(7) Uani 1 1 d . . . C22 C -0.1284(3) 0.7238(3) 0.09010(15) 0.0585(10) Uani 1 1 d . . . H22 H -0.1022 0.7077 0.0595 0.070 Uiso 1 1 calc R . . C23 C -0.1458(4) 0.8232(4) 0.1014(2) 0.0800(15) Uani 1 1 d . . . H23 H -0.1310 0.8742 0.0788 0.096 Uiso 1 1 calc R . . C24 C -0.1853(5) 0.8470(4) 0.1467(2) 0.0883(18) Uani 1 1 d . . . H24 H -0.1958 0.9142 0.1550 0.106 Uiso 1 1 calc R . . C25 C -0.2086(4) 0.7719(4) 0.17876(19) 0.0759(14) Uani 1 1 d . . . H25 H -0.2378 0.7882 0.2083 0.091 Uiso 1 1 calc R . . C26 C -0.1901(3) 0.6724(3) 0.16877(15) 0.0596(10) Uani 1 1 d . . . H26 H -0.2047 0.6224 0.1920 0.072 Uiso 1 1 calc R . . C27 C 0.0449(3) 0.7364(4) 0.1953(2) 0.0677(12) Uani 1 1 d . . . H27A H -0.0096 0.7594 0.1845 0.102 Uiso 1 1 calc R . . H27B H 0.0878 0.7769 0.1796 0.102 Uiso 1 1 calc R . . H27C H 0.0492 0.7422 0.2316 0.102 Uiso 1 1 calc R . . C28 C 0.1602(3) 0.5796(4) 0.20276(18) 0.0643(11) Uani 1 1 d . . . H28A H 0.1717 0.5089 0.1980 0.097 Uiso 1 1 calc R . . H28B H 0.1613 0.5952 0.2383 0.097 Uiso 1 1 calc R . . H28C H 0.2021 0.6190 0.1855 0.097 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 Pt 0.04213(11) 0.04225(11) 0.03110(9) -0.00410(3) 0.00125(3) 0.00164(4) Fe 0.0401(2) 0.0383(2) 0.0564(3) -0.00591(18) -0.00295(18) 0.00356(18) Cl1 0.0726(7) 0.0967(9) 0.0379(4) -0.0137(5) -0.0032(4) -0.0129(7) Cl2 0.0545(5) 0.0566(5) 0.0481(4) 0.0026(3) 0.0085(3) -0.0045(4) S1 0.0508(4) 0.0497(4) 0.0434(4) -0.0079(3) 0.0033(3) -0.0056(4) O1 0.0691(16) 0.0535(14) 0.0434(12) -0.0012(10) 0.0121(12) -0.0063(13) N1 0.0383(13) 0.0385(13) 0.0324(11) 0.0002(8) 0.0015(9) 0.0028(10) N2 0.0434(13) 0.0369(11) 0.0323(10) -0.0027(8) 0.0023(9) 0.0041(10) C1 0.051(2) 0.056(2) 0.0539(18) -0.0029(15) 0.0047(15) 0.0072(17) C2 0.0512(19) 0.0534(19) 0.0521(18) -0.0059(14) 0.0003(14) 0.0118(16) C3 0.060(2) 0.0465(16) 0.0449(16) 0.0014(13) -0.0015(14) 0.0055(16) C4 0.0461(18) 0.0381(15) 0.0602(19) -0.0108(13) 0.0069(14) 0.0037(14) C5 0.053(2) 0.059(2) 0.0498(18) -0.0027(15) -0.0055(14) 0.0056(18) C6 0.050(2) 0.0393(16) 0.088(3) 0.0053(16) 0.0161(19) 0.0020(16) C7 0.052(2) 0.047(2) 0.153(6) -0.022(3) 0.021(3) -0.004(2) C8 0.047(2) 0.079(3) 0.128(5) -0.048(3) -0.012(3) 0.002(2) C9 0.070(3) 0.062(2) 0.078(3) -0.032(2) -0.023(2) 0.022(2) C10 0.0516(18) 0.0427(16) 0.0575(19) -0.0160(14) -0.0050(15) 0.0084(16) C11 0.0496(17) 0.0384(14) 0.0348(13) -0.0003(10) 0.0009(11) 0.0104(13) C12 0.0348(13) 0.0440(15) 0.0397(13) -0.0063(11) -0.0036(10) 0.0036(12) C13 0.0365(15) 0.0451(16) 0.0511(16) -0.0106(13) -0.0062(12) 0.0002(13) C14 0.0474(18) 0.0523(18) 0.0493(17) -0.0092(14) 0.0005(13) -0.0032(15) C15 0.061(2) 0.0466(19) 0.077(3) -0.0122(17) -0.0030(19) -0.0054(18) C16 0.054(2) 0.059(2) 0.073(2) -0.0294(19) -0.0150(18) 0.0002(18) C17 0.060(2) 0.070(2) 0.0441(17) -0.0204(16) -0.0074(15) 0.013(2) C18 0.0548(19) 0.0509(17) 0.0387(14) -0.0041(12) -0.0070(13) 0.0035(15) C19 0.0442(17) 0.0454(17) 0.0390(15) -0.0021(11) -0.0055(12) 0.0045(13) C20 0.0404(16) 0.0414(14) 0.0437(15) -0.0058(12) -0.0041(11) 0.0041(13) C21 0.057(2) 0.0398(15) 0.0439(15) -0.0064(12) -0.0077(13) 0.0104(15) C22 0.084(3) 0.0421(17) 0.0498(18) 0.0010(14) -0.0023(17) 0.0117(18) C23 0.103(4) 0.051(2) 0.086(3) 0.009(2) -0.015(3) 0.009(3) C24 0.127(5) 0.053(2) 0.084(3) -0.020(2) -0.023(3) 0.037(3) C25 0.088(3) 0.074(3) 0.066(2) -0.018(2) -0.002(2) 0.035(3) C26 0.071(3) 0.0543(19) 0.0532(19) -0.0025(15) -0.0064(17) 0.0211(19) C27 0.079(3) 0.051(2) 0.073(3) -0.015(2) 0.014(2) -0.015(2) C28 0.041(2) 0.090(3) 0.062(2) -0.004(2) -0.0036(17) 0.000(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt N1 2.021(3) . ? Pt S1 2.2044(10) . ? Pt Cl1 2.2814(12) . ? Pt Cl2 2.3166(10) . ? Fe C4 2.029(4) . ? Fe C8 2.029(5) . ? Fe C6 2.036(4) . ? Fe C7 2.037(5) . ? Fe C9 2.040(4) . ? Fe C3 2.042(4) . ? Fe C10 2.042(4) . ? Fe C5 2.043(4) . ? Fe C2 2.047(4) . ? Fe C1 2.047(4) . ? S1 O1 1.464(3) . ? S1 C27 1.763(5) . ? S1 C28 1.788(4) . ? N1 C20 1.336(4) . ? N1 N2 1.362(3) . ? N2 C12 1.363(4) . ? N2 C11 1.450(4) . ? C1 C2 1.411(5) . ? C1 C5 1.424(6) . ? C1 H1 0.9299 . ? C2 C3 1.412(5) . ? C2 H2 0.9299 . ? C3 C4 1.422(5) . ? C3 H3 0.9299 . ? C4 C5 1.413(5) . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? C6 C10 1.410(6) . ? C6 C7 1.417(7) . ? C6 H6 0.9300 . ? C7 C8 1.387(8) . ? C7 H7 0.9300 . ? C8 C9 1.437(8) . ? C8 H8 0.9300 . ? C9 C10 1.414(6) . ? C9 H9 0.9300 . ? C10 C11 1.515(5) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 C19 1.367(5) . ? C12 C13 1.489(4) . ? C13 C14 1.386(5) . ? C13 C18 1.387(5) . ? C14 C15 1.394(5) . ? C14 H14 0.9300 . ? C15 C16 1.382(7) . ? C15 H15 0.9300 . ? C16 C17 1.373(7) . ? C16 H16 0.9300 . ? C17 C18 1.393(5) . ? C17 H17 0.9300 . ? C18 H18 0.9300 . ? C19 C20 1.409(4) . ? C19 H19 0.9300 . ? C20 C21 1.462(5) . ? C21 C26 1.385(5) . ? C21 C22 1.397(5) . ? C22 C23 1.375(6) . ? C22 H22 0.9300 . ? C23 C24 1.382(8) . ? C23 H23 0.9300 . ? C24 C25 1.355(8) . ? C24 H24 0.9300 . ? C25 C26 1.372(6) . ? C25 H25 0.9300 . ? C26 H26 0.9300 . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 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 N1 Pt S1 90.68(8) . . ? N1 Pt Cl1 178.97(8) . . ? S1 Pt Cl1 89.94(5) . . ? N1 Pt Cl2 88.84(8) . . ? S1 Pt Cl2 175.37(4) . . ? Cl1 Pt Cl2 90.61(5) . . ? C4 Fe C8 155.1(2) . . ? C4 Fe C6 126.39(17) . . ? C8 Fe C6 67.7(2) . . ? C4 Fe C7 163.8(2) . . ? C8 Fe C7 39.9(2) . . ? C6 Fe C7 40.72(19) . . ? C4 Fe C9 119.6(2) . . ? C8 Fe C9 41.4(2) . . ? C6 Fe C9 68.4(2) . . ? C7 Fe C9 68.7(2) . . ? C4 Fe C3 40.89(15) . . ? C8 Fe C3 120.3(2) . . ? C6 Fe C3 164.16(16) . . ? C7 Fe C3 153.8(2) . . ? C9 Fe C3 107.85(19) . . ? C4 Fe C10 107.99(16) . . ? C8 Fe C10 68.25(18) . . ? C6 Fe C10 40.45(17) . . ? C7 Fe C10 68.35(19) . . ? C9 Fe C10 40.54(16) . . ? C3 Fe C10 126.85(17) . . ? C4 Fe C5 40.60(16) . . ? C8 Fe C5 163.2(2) . . ? C6 Fe C5 107.56(19) . . ? C7 Fe C5 126.2(2) . . ? C9 Fe C5 153.72(19) . . ? C3 Fe C5 68.62(15) . . ? C10 Fe C5 119.43(16) . . ? C4 Fe C2 68.10(16) . . ? C8 Fe C2 108.50(19) . . ? C6 Fe C2 154.00(16) . . ? C7 Fe C2 119.69(18) . . ? C9 Fe C2 126.97(17) . . ? C3 Fe C2 40.40(15) . . ? C10 Fe C2 164.36(16) . . ? C5 Fe C2 68.20(16) . . ? C4 Fe C1 68.27(15) . . ? C8 Fe C1 126.2(2) . . ? C6 Fe C1 119.60(17) . . ? C7 Fe C1 107.6(2) . . ? C9 Fe C1 164.18(17) . . ? C3 Fe C1 68.25(15) . . ? C10 Fe C1 153.93(16) . . ? C5 Fe C1 40.76(16) . . ? C2 Fe C1 40.32(15) . . ? O1 S1 C27 107.4(2) . . ? O1 S1 C28 108.3(2) . . ? C27 S1 C28 102.5(3) . . ? O1 S1 Pt 117.75(13) . . ? C27 S1 Pt 107.76(16) . . ? C28 S1 Pt 111.97(18) . . ? C20 N1 N2 107.8(2) . . ? C20 N1 Pt 128.8(2) . . ? N2 N1 Pt 123.28(19) . . ? N1 N2 C12 108.9(2) . . ? N1 N2 C11 121.1(2) . . ? C12 N2 C11 128.3(2) . . ? C2 C1 C5 107.9(3) . . ? C2 C1 Fe 69.8(2) . . ? C5 C1 Fe 69.5(2) . . ? C2 C1 H1 126.0 . . ? C5 C1 H1 126.1 . . ? Fe C1 H1 126.4 . . ? C1 C2 C3 108.7(3) . . ? C1 C2 Fe 69.9(2) . . ? C3 C2 Fe 69.6(2) . . ? C1 C2 H2 125.6 . . ? C3 C2 H2 125.6 . . ? Fe C2 H2 126.4 . . ? C2 C3 C4 107.3(3) . . ? C2 C3 Fe 70.0(2) . . ? C4 C3 Fe 69.1(2) . . ? C2 C3 H3 126.4 . . ? C4 C3 H3 126.4 . . ? Fe C3 H3 126.2 . . ? C5 C4 C3 108.6(3) . . ? C5 C4 Fe 70.2(2) . . ? C3 C4 Fe 70.0(2) . . ? C5 C4 H4 125.7 . . ? C3 C4 H4 125.7 . . ? Fe C4 H4 125.6 . . ? C4 C5 C1 107.5(3) . . ? C4 C5 Fe 69.2(2) . . ? C1 C5 Fe 69.8(2) . . ? C4 C5 H5 126.3 . . ? C1 C5 H5 126.3 . . ? Fe C5 H5 126.3 . . ? C10 C6 C7 108.3(5) . . ? C10 C6 Fe 70.0(2) . . ? C7 C6 Fe 69.7(3) . . ? C10 C6 H6 125.9 . . ? C7 C6 H6 125.8 . . ? Fe C6 H6 126.0 . . ? C8 C7 C6 107.8(5) . . ? C8 C7 Fe 69.8(3) . . ? C6 C7 Fe 69.6(2) . . ? C8 C7 H7 126.1 . . ? C6 C7 H7 126.1 . . ? Fe C7 H7 126.1 . . ? C7 C8 C9 109.1(4) . . ? C7 C8 Fe 70.4(3) . . ? C9 C8 Fe 69.7(3) . . ? C7 C8 H8 125.4 . . ? C9 C8 H8 125.5 . . ? Fe C8 H8 126.0 . . ? C10 C9 C8 106.5(5) . . ? C10 C9 Fe 69.8(2) . . ? C8 C9 Fe 68.9(3) . . ? C10 C9 H9 126.8 . . ? C8 C9 H9 126.7 . . ? Fe C9 H9 126.1 . . ? C6 C10 C9 108.3(4) . . ? C6 C10 C11 125.2(4) . . ? C9 C10 C11 126.4(4) . . ? C6 C10 Fe 69.5(2) . . ? C9 C10 Fe 69.6(2) . . ? C11 C10 Fe 126.6(2) . . ? N2 C11 C10 112.4(3) . . ? N2 C11 H11A 109.1 . . ? C10 C11 H11A 109.1 . . ? N2 C11 H11B 109.1 . . ? C10 C11 H11B 109.1 . . ? H11A C11 H11B 107.9 . . ? N2 C12 C19 108.4(3) . . ? N2 C12 C13 122.4(3) . . ? C19 C12 C13 129.3(3) . . ? C14 C13 C18 119.8(3) . . ? C14 C13 C12 120.7(3) . . ? C18 C13 C12 119.3(3) . . ? C13 C14 C15 120.5(4) . . ? C13 C14 H14 119.8 . . ? C15 C14 H14 119.8 . . ? C16 C15 C14 119.2(4) . . ? C16 C15 H15 120.4 . . ? C14 C15 H15 120.4 . . ? C17 C16 C15 120.3(4) . . ? C17 C16 H16 119.8 . . ? C15 C16 H16 119.8 . . ? C16 C17 C18 120.9(4) . . ? C16 C17 H17 119.6 . . ? C18 C17 H17 119.6 . . ? C13 C18 C17 119.1(4) . . ? C13 C18 H18 120.4 . . ? C17 C18 H18 120.4 . . ? C12 C19 C20 105.8(3) . . ? C12 C19 H19 127.1 . . ? C20 C19 H19 127.1 . . ? N1 C20 C19 109.1(3) . . ? N1 C20 C21 121.1(3) . . ? C19 C20 C21 129.9(3) . . ? C26 C21 C22 118.5(3) . . ? C26 C21 C20 121.3(3) . . ? C22 C21 C20 120.2(3) . . ? C23 C22 C21 120.6(4) . . ? C23 C22 H22 119.7 . . ? C21 C22 H22 119.7 . . ? C22 C23 C24 119.7(5) . . ? C22 C23 H23 120.2 . . ? C24 C23 H23 120.2 . . ? C25 C24 C23 119.7(4) . . ? C25 C24 H24 120.2 . . ? C23 C24 H24 120.2 . . ? C24 C25 C26 121.5(5) . . ? C24 C25 H25 119.2 . . ? C26 C25 H25 119.2 . . ? C25 C26 C21 119.9(4) . . ? C25 C26 H26 120.1 . . ? C21 C26 H26 120.1 . . ? S1 C27 H27A 109.5 . . ? S1 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? S1 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? S1 C28 H28A 109.5 . . ? S1 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? S1 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.763 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.963 _refine_diff_density_max 3.868 _refine_diff_density_min -1.880 _refine_diff_density_rms 0.209 #==END data_chnm35b _database_code_depnum_ccdc_archive 'CCDC 826856' #TrackingRef 'TOT.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H28 Cl2 Fe N2 O Pd S' _chemical_formula_sum 'C28 H28 Cl2 Fe N2 O Pd S' _chemical_formula_weight 673.73 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' Fe Fe 0.3463 0.8444 '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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 15.938(5) _cell_length_b 13.226(5) _cell_length_c 26.424(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5570(3) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 7287 _cell_measurement_theta_min 3 _cell_measurement_theta_max 31 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.607 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2720 _exptl_absorpt_coefficient_mu 1.458 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.83 _exptl_absorpt_correction_T_max 0.86 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'MAR345 with image plate detector' _diffrn_measurement_method 'phi scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 40442 _diffrn_reflns_av_R_equivalents 0.0542 _diffrn_reflns_av_sigmaI/netI 0.0507 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 39 _diffrn_reflns_theta_min 2.98 _diffrn_reflns_theta_max 32.39 _reflns_number_total 7038 _reflns_number_gt 5917 _reflns_threshold_expression >2sigma(I) _computing_data_collection MARXDS _computing_cell_refinement AUTOMAR _computing_data_reduction MARSCALE _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP (Brueggermann and Smith, 1990)' _computing_publication_material 'PLATON (Spek, 1990)' _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^)+(0.0920P)^2^+21.1887P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0031(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 7038 _refine_ls_number_parameters 326 _refine_ls_number_restraints 17 _refine_ls_R_factor_all 0.0761 _refine_ls_R_factor_gt 0.0675 _refine_ls_wR_factor_ref 0.2097 _refine_ls_wR_factor_gt 0.2041 _refine_ls_goodness_of_fit_ref 1.082 _refine_ls_restrained_S_all 1.095 _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 0.54164(2) 0.47985(3) 0.214371(13) 0.02961(16) Uani 1 1 d U . . Fe Fe 0.35859(5) 0.76825(7) 0.10100(3) 0.0401(2) Uani 1 1 d U . . Cl1 Cl 0.65330(11) 0.56281(14) 0.25199(6) 0.0502(4) Uani 1 1 d U . . Cl2 Cl 0.48819(13) 0.44054(16) 0.29124(6) 0.0530(4) Uani 1 1 d U . . S S 0.44120(11) 0.39278(15) 0.17775(6) 0.0491(4) Uani 1 1 d U . . O1 O 0.4351(4) 0.3905(4) 0.12125(19) 0.0589(13) Uani 1 1 d . . . N1 N 0.5897(4) 0.5177(5) 0.14665(19) 0.0529(15) Uani 1 1 d U . . N2 N 0.5806(4) 0.6119(5) 0.1272(2) 0.0558(14) Uani 1 1 d . . . C1 C 0.4217(6) 0.8978(7) 0.0885(3) 0.0627(19) Uani 1 1 d . . . H1 H 0.4753 0.9117 0.1006 0.075 Uiso 1 1 calc R . . C2 C 0.3466(6) 0.9200(7) 0.1132(3) 0.064(2) Uani 1 1 d . . . H2 H 0.3410 0.9506 0.1447 0.077 Uiso 1 1 calc R . . C3 C 0.2814(6) 0.8876(7) 0.0817(3) 0.065(2) Uani 1 1 d . . . H3 H 0.2245 0.8939 0.0889 0.078 Uiso 1 1 calc R . . C4 C 0.3150(6) 0.8440(7) 0.0375(3) 0.068(2) Uani 1 1 d U . . H4 H 0.2847 0.8163 0.0108 0.082 Uiso 1 1 calc R . . C5 C 0.4025(6) 0.8502(7) 0.0413(3) 0.066(2) Uani 1 1 d U . . H5 H 0.4411 0.8274 0.0175 0.079 Uiso 1 1 calc R . . C6 C 0.3654(6) 0.7000(8) 0.1668(3) 0.071(2) Uani 1 1 d U . . H6 H 0.3667 0.7341 0.1975 0.085 Uiso 1 1 calc R . . C7 C 0.2936(6) 0.6685(7) 0.1419(3) 0.071(2) Uani 1 1 d U . . H7 H 0.2389 0.6774 0.1534 0.085 Uiso 1 1 calc R . . C8 C 0.3181(6) 0.6192(7) 0.0948(4) 0.072(2) Uani 1 1 d . . . H8 H 0.2824 0.5920 0.0705 0.086 Uiso 1 1 calc R . . C9 C 0.4052(6) 0.6205(7) 0.0932(3) 0.068(2) Uani 1 1 d . . . H9 H 0.4384 0.5929 0.0678 0.081 Uiso 1 1 calc R . . C10 C 0.4358(6) 0.6723(7) 0.1381(3) 0.065(2) Uani 1 1 d U . . C11 C 0.5258(5) 0.6887(7) 0.1474(3) 0.063(2) Uani 1 1 d . . . H11A H 0.5415 0.7534 0.1329 0.076 Uiso 1 1 calc R . . H11B H 0.5347 0.6930 0.1836 0.076 Uiso 1 1 calc R . . C12 C 0.6123(6) 0.6075(6) 0.0785(3) 0.0643(18) Uani 1 1 d DU . . C13 C 0.6436(6) 0.5116(6) 0.0663(3) 0.072(2) Uani 1 1 d DU . . H13 H 0.6662 0.4884 0.0360 0.087 Uiso 1 1 calc R . . C14 C 0.6318(6) 0.4599(6) 0.1124(3) 0.067(2) Uani 1 1 d D . . C15 C 0.6196(5) 0.6996(7) 0.0421(3) 0.0620(18) Uani 1 1 d U . . C16 C 0.6469(5) 0.7903(7) 0.0631(3) 0.068(2) Uani 1 1 d . . . H16 H 0.6630 0.7924 0.0969 0.081 Uiso 1 1 calc R . . C17 C 0.6501(6) 0.8769(7) 0.0341(3) 0.069(2) Uani 1 1 d . . . H17 H 0.6683 0.9376 0.0482 0.083 Uiso 1 1 calc R . . C18 C 0.6256(6) 0.8724(7) -0.0166(3) 0.069(2) Uani 1 1 d . . . H18 H 0.6272 0.9306 -0.0364 0.083 Uiso 1 1 calc R . . C19 C 0.5990(6) 0.7823(7) -0.0377(3) 0.070(2) Uani 1 1 d . . . H19 H 0.5837 0.7792 -0.0717 0.085 Uiso 1 1 calc R . . C20 C 0.5954(6) 0.6966(7) -0.0075(3) 0.067(2) Uani 1 1 d . . . H20 H 0.5762 0.6361 -0.0212 0.080 Uiso 1 1 calc R . . C21 C 0.6490(6) 0.3517(7) 0.1256(3) 0.064(2) Uani 1 1 d . . . C22 C 0.6911(6) 0.3278(8) 0.1696(3) 0.074(2) Uani 1 1 d . . . H22 H 0.7043 0.3784 0.1927 0.088 Uiso 1 1 calc R . . C23 C 0.7138(6) 0.2282(7) 0.1797(3) 0.073(2) Uani 1 1 d . . . H23 H 0.7429 0.2124 0.2092 0.088 Uiso 1 1 calc R . . C24 C 0.6931(6) 0.1527(8) 0.1457(3) 0.073(2) Uani 1 1 d . . . H24 H 0.7074 0.0861 0.1529 0.087 Uiso 1 1 calc R . . C25 C 0.6503(6) 0.1753(8) 0.1000(4) 0.076(2) Uani 1 1 d U . . H25 H 0.6368 0.1251 0.0768 0.092 Uiso 1 1 calc R . . C26 C 0.6293(6) 0.2762(7) 0.0914(3) 0.069(2) Uani 1 1 d U . . H26 H 0.6012 0.2932 0.0618 0.082 Uiso 1 1 calc R . . C27 C 0.4582(3) 0.2513(5) 0.19404(17) 0.0333(9) Uani 1 1 d U . . H27A H 0.5124 0.2303 0.1822 0.050 Uiso 1 1 calc R . . H27B H 0.4155 0.2114 0.1780 0.050 Uiso 1 1 calc R . . H27C H 0.4551 0.2423 0.2300 0.050 Uiso 1 1 calc R . . C28 C 0.3414(6) 0.4321(8) 0.1986(4) 0.073(2) Uani 1 1 d U . . H28A H 0.3335 0.5022 0.1904 0.110 Uiso 1 1 calc R . . H28B H 0.3373 0.4230 0.2345 0.110 Uiso 1 1 calc R . . H28C H 0.2990 0.3925 0.1821 0.110 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 0.0300(3) 0.0301(3) 0.0287(2) 0.00129(12) -0.00045(11) 0.00064(14) Fe 0.0372(5) 0.0413(5) 0.0419(4) 0.0004(3) 0.0001(3) 0.0006(3) Cl1 0.0489(9) 0.0525(11) 0.0492(7) -0.0009(7) -0.0021(6) -0.0012(7) Cl2 0.0536(10) 0.0600(12) 0.0453(7) 0.0024(7) 0.0003(6) -0.0021(8) S 0.0489(9) 0.0499(10) 0.0486(8) 0.0022(7) -0.0009(6) -0.0018(7) O1 0.062(3) 0.060(3) 0.054(3) -0.001(2) -0.005(2) -0.003(3) N1 0.059(4) 0.064(4) 0.035(2) 0.008(2) 0.007(2) -0.003(3) N2 0.055(4) 0.055(4) 0.058(3) 0.002(3) -0.003(3) 0.004(3) C1 0.063(5) 0.057(5) 0.068(4) 0.002(4) 0.004(4) -0.001(4) C2 0.065(5) 0.059(5) 0.068(4) -0.003(4) -0.001(4) 0.005(4) C3 0.062(5) 0.061(5) 0.071(5) 0.004(4) 0.001(4) 0.005(4) C4 0.071(5) 0.080(6) 0.053(4) 0.012(3) -0.010(3) 0.011(4) C5 0.067(5) 0.075(6) 0.056(4) 0.014(3) 0.010(3) -0.009(4) C6 0.078(6) 0.075(6) 0.059(3) 0.023(3) 0.003(4) 0.007(5) C7 0.062(5) 0.070(6) 0.080(5) 0.020(4) 0.008(4) -0.014(4) C8 0.061(5) 0.060(6) 0.094(6) 0.001(5) -0.005(4) -0.006(4) C9 0.069(5) 0.060(5) 0.074(5) -0.005(4) 0.002(4) 0.006(4) C10 0.067(5) 0.059(5) 0.069(5) 0.009(4) -0.007(4) 0.018(4) C11 0.068(5) 0.057(5) 0.065(4) -0.007(4) -0.001(4) 0.000(4) C12 0.064(5) 0.069(4) 0.060(4) 0.005(3) -0.001(3) 0.001(4) C13 0.073(6) 0.077(5) 0.066(5) -0.011(4) 0.004(4) 0.002(4) C14 0.069(6) 0.068(6) 0.064(4) -0.007(4) 0.005(4) -0.004(4) C15 0.061(5) 0.060(5) 0.066(4) 0.001(3) 0.002(3) -0.003(4) C16 0.064(5) 0.078(6) 0.062(4) 0.003(4) -0.001(3) -0.004(4) C17 0.071(6) 0.057(6) 0.079(5) 0.001(4) 0.002(4) -0.001(4) C18 0.075(6) 0.063(6) 0.071(5) 0.004(4) 0.002(4) 0.000(4) C19 0.068(5) 0.072(6) 0.071(5) 0.000(4) -0.003(4) 0.004(5) C20 0.066(5) 0.068(6) 0.066(4) 0.000(4) 0.002(4) -0.003(4) C21 0.064(5) 0.064(6) 0.065(4) -0.001(4) 0.000(3) 0.003(4) C22 0.075(6) 0.073(6) 0.073(5) -0.003(4) -0.001(4) 0.008(5) C23 0.078(6) 0.072(6) 0.070(5) 0.012(4) 0.004(4) 0.013(5) C24 0.079(6) 0.072(6) 0.067(5) 0.001(4) 0.000(4) 0.009(5) C25 0.075(6) 0.068(4) 0.086(6) -0.005(5) 0.001(5) 0.004(5) C26 0.071(5) 0.070(4) 0.065(4) 0.002(4) -0.001(4) 0.001(4) C27 0.027(2) 0.0477(17) 0.0254(19) -0.0016(18) -0.0006(14) -0.0041(19) C28 0.053(3) 0.085(7) 0.082(5) -0.011(5) 0.005(4) 0.004(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 N1 2.010(5) . ? Pd S 2.1965(19) . ? Pd Cl2 2.2630(17) . ? Pd Cl1 2.3150(18) . ? Fe C6 1.961(8) . ? Fe C7 1.996(8) . ? Fe C1 2.015(9) . ? Fe C10 2.022(8) . ? Fe C5 2.037(7) . ? Fe C2 2.041(9) . ? Fe C3 2.065(9) . ? Fe C4 2.074(7) . ? Fe C8 2.081(9) . ? Fe C9 2.101(9) . ? S O1 1.497(5) . ? S C28 1.762(9) . ? S C27 1.939(7) . ? N1 N2 1.355(9) . ? N1 C14 1.362(10) . ? N2 C12 1.382(10) . ? N2 C11 1.444(11) . ? C1 C2 1.394(12) . ? C1 C5 1.429(12) . ? C1 H1 0.9300 . ? C2 C3 1.398(12) . ? C2 H2 0.9300 . ? C3 C4 1.408(12) . ? C3 H3 0.9300 . ? C4 C5 1.401(12) . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? C6 C7 1.383(13) . ? C6 C10 1.403(12) . ? C6 H6 0.9300 . ? C7 C8 1.460(13) . ? C7 H7 0.9300 . ? C8 C9 1.389(13) . ? C8 H8 0.9300 . ? C9 C10 1.454(12) . ? C9 H9 0.9300 . ? C10 C11 1.471(12) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 C13 1.400(8) . ? C12 C15 1.558(11) . ? C13 C14 1.409(8) . ? C13 H13 0.9300 . ? C14 C21 1.498(12) . ? C15 C20 1.365(11) . ? C15 C16 1.390(12) . ? C16 C17 1.379(12) . ? C16 H16 0.9300 . ? C17 C18 1.397(12) . ? C17 H17 0.9300 . ? C18 C19 1.382(13) . ? C18 H18 0.9300 . ? C19 C20 1.389(12) . ? C19 H19 0.9300 . ? C20 H20 0.9300 . ? C21 C22 1.379(12) . ? C21 C26 1.383(12) . ? C22 C23 1.392(13) . ? C22 H22 0.9300 . ? C23 C24 1.382(13) . ? C23 H23 0.9300 . ? C24 C25 1.419(13) . ? C24 H24 0.9300 . ? C25 C26 1.393(14) . ? C25 H25 0.9300 . ? C26 H26 0.9300 . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 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 N1 Pd S 90.92(19) . . ? N1 Pd Cl2 178.8(2) . . ? S Pd Cl2 90.04(7) . . ? N1 Pd Cl1 88.35(19) . . ? S Pd Cl1 176.26(7) . . ? Cl2 Pd Cl1 90.74(7) . . ? C6 Fe C7 40.9(4) . . ? C6 Fe C1 120.6(4) . . ? C7 Fe C1 155.6(4) . . ? C6 Fe C10 41.2(4) . . ? C7 Fe C10 68.8(4) . . ? C1 Fe C10 108.0(4) . . ? C6 Fe C5 155.7(4) . . ? C7 Fe C5 161.7(4) . . ? C1 Fe C5 41.3(3) . . ? C10 Fe C5 120.0(4) . . ? C6 Fe C2 108.6(4) . . ? C7 Fe C2 121.1(4) . . ? C1 Fe C2 40.2(3) . . ? C10 Fe C2 126.7(4) . . ? C5 Fe C2 68.3(4) . . ? C6 Fe C3 127.1(4) . . ? C7 Fe C3 109.2(4) . . ? C1 Fe C3 66.9(4) . . ? C10 Fe C3 164.2(4) . . ? C5 Fe C3 66.9(4) . . ? C2 Fe C3 39.8(3) . . ? C6 Fe C4 163.2(4) . . ? C7 Fe C4 125.7(4) . . ? C1 Fe C4 67.9(4) . . ? C10 Fe C4 154.1(4) . . ? C5 Fe C4 39.8(3) . . ? C2 Fe C4 67.7(4) . . ? C3 Fe C4 39.8(3) . . ? C6 Fe C8 69.6(4) . . ? C7 Fe C8 41.9(4) . . ? C1 Fe C8 161.4(4) . . ? C10 Fe C8 68.4(4) . . ? C5 Fe C8 123.3(4) . . ? C2 Fe C8 156.2(4) . . ? C3 Fe C8 121.4(4) . . ? C4 Fe C8 106.9(4) . . ? C6 Fe C9 68.8(4) . . ? C7 Fe C9 67.8(4) . . ? C1 Fe C9 126.8(4) . . ? C10 Fe C9 41.2(3) . . ? C5 Fe C9 107.3(4) . . ? C2 Fe C9 164.3(4) . . ? C3 Fe C9 153.9(3) . . ? C4 Fe C9 119.3(4) . . ? C8 Fe C9 38.8(4) . . ? O1 S C28 105.0(4) . . ? O1 S C27 102.2(3) . . ? C28 S C27 110.0(4) . . ? O1 S Pd 119.8(2) . . ? C28 S Pd 111.5(3) . . ? C27 S Pd 107.83(16) . . ? N2 N1 C14 108.4(5) . . ? N2 N1 Pd 121.8(5) . . ? C14 N1 Pd 129.8(5) . . ? N1 N2 C12 106.0(6) . . ? N1 N2 C11 124.8(6) . . ? C12 N2 C11 126.5(7) . . ? C2 C1 C5 108.4(8) . . ? C2 C1 Fe 70.9(5) . . ? C5 C1 Fe 70.2(5) . . ? C2 C1 H1 125.8 . . ? C5 C1 H1 125.8 . . ? Fe C1 H1 124.7 . . ? C1 C2 C3 107.2(8) . . ? C1 C2 Fe 68.9(5) . . ? C3 C2 Fe 71.0(5) . . ? C1 C2 H2 126.4 . . ? C3 C2 H2 126.4 . . ? Fe C2 H2 125.3 . . ? C2 C3 C4 109.6(8) . . ? C2 C3 Fe 69.2(5) . . ? C4 C3 Fe 70.4(5) . . ? C2 C3 H3 125.2 . . ? C4 C3 H3 125.2 . . ? Fe C3 H3 126.8 . . ? C5 C4 C3 107.2(8) . . ? C5 C4 Fe 68.7(4) . . ? C3 C4 Fe 69.8(5) . . ? C5 C4 H4 126.4 . . ? C3 C4 H4 126.4 . . ? Fe C4 H4 126.7 . . ? C4 C5 C1 107.6(8) . . ? C4 C5 Fe 71.5(5) . . ? C1 C5 Fe 68.5(4) . . ? C4 C5 H5 126.2 . . ? C1 C5 H5 126.2 . . ? Fe C5 H5 125.3 . . ? C7 C6 C10 109.1(9) . . ? C7 C6 Fe 70.9(5) . . ? C10 C6 Fe 71.7(5) . . ? C7 C6 H6 125.4 . . ? C10 C6 H6 125.4 . . ? Fe C6 H6 123.5 . . ? C6 C7 C8 108.5(8) . . ? C6 C7 Fe 68.2(5) . . ? C8 C7 Fe 72.2(5) . . ? C6 C7 H7 125.7 . . ? C8 C7 H7 125.7 . . ? Fe C7 H7 125.4 . . ? C9 C8 C7 106.7(8) . . ? C9 C8 Fe 71.4(5) . . ? C7 C8 Fe 65.9(5) . . ? C9 C8 H8 126.6 . . ? C7 C8 H8 126.6 . . ? Fe C8 H8 127.6 . . ? C8 C9 C10 108.5(8) . . ? C8 C9 Fe 69.8(5) . . ? C10 C9 Fe 66.5(5) . . ? C8 C9 H9 125.8 . . ? C10 C9 H9 125.8 . . ? Fe C9 H9 129.5 . . ? C6 C10 C9 107.2(8) . . ? C6 C10 C11 130.7(9) . . ? C9 C10 C11 122.2(8) . . ? C6 C10 Fe 67.1(5) . . ? C9 C10 Fe 72.3(5) . . ? C11 C10 Fe 125.5(7) . . ? N2 C11 C10 115.1(7) . . ? N2 C11 H11A 108.5 . . ? C10 C11 H11A 108.5 . . ? N2 C11 H11B 108.5 . . ? C10 C11 H11B 108.5 . . ? H11A C11 H11B 107.5 . . ? N2 C12 C13 112.5(6) . . ? N2 C12 C15 124.7(7) . . ? C13 C12 C15 122.6(7) . . ? C12 C13 C14 101.2(6) . . ? C12 C13 H13 129.4 . . ? C14 C13 H13 129.4 . . ? N1 C14 C13 111.5(6) . . ? N1 C14 C21 118.1(7) . . ? C13 C14 C21 129.9(8) . . ? C20 C15 C16 119.8(9) . . ? C20 C15 C12 123.3(8) . . ? C16 C15 C12 116.8(7) . . ? C17 C16 C15 120.4(8) . . ? C17 C16 H16 119.8 . . ? C15 C16 H16 119.8 . . ? C16 C17 C18 119.1(9) . . ? C16 C17 H17 120.5 . . ? C18 C17 H17 120.5 . . ? C19 C18 C17 120.7(9) . . ? C19 C18 H18 119.7 . . ? C17 C18 H18 119.7 . . ? C18 C19 C20 119.0(8) . . ? C18 C19 H19 120.5 . . ? C20 C19 H19 120.5 . . ? C15 C20 C19 121.1(9) . . ? C15 C20 H20 119.5 . . ? C19 C20 H20 119.5 . . ? C22 C21 C26 119.7(9) . . ? C22 C21 C14 120.3(8) . . ? C26 C21 C14 119.7(8) . . ? C21 C22 C23 120.3(9) . . ? C21 C22 H22 119.9 . . ? C23 C22 H22 119.9 . . ? C24 C23 C22 119.9(9) . . ? C24 C23 H23 120.1 . . ? C22 C23 H23 120.1 . . ? C23 C24 C25 121.0(9) . . ? C23 C24 H24 119.5 . . ? C25 C24 H24 119.5 . . ? C26 C25 C24 117.1(9) . . ? C26 C25 H25 121.4 . . ? C24 C25 H25 121.4 . . ? C21 C26 C25 122.0(9) . . ? C21 C26 H26 119.0 . . ? C25 C26 H26 119.0 . . ? S C27 H27A 109.5 . . ? S C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? S C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? S C28 H28A 109.5 . . ? S C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? S C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.704 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.902 _refine_diff_density_max 3.151 _refine_diff_density_min -1.371 _refine_diff_density_rms 0.150 #==END data_chnm92a _database_code_depnum_ccdc_archive 'CCDC 826857' #TrackingRef 'TOT.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C44 H36 Cl Fe N2 P Pd, C H2 Cl2' _chemical_formula_sum 'C45 H38 Cl3 Fe N2 P Pd' _chemical_formula_weight 906.34 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.817(6) _cell_length_b 11.219(5) _cell_length_c 19.794(9) _cell_angle_alpha 76.47(3) _cell_angle_beta 82.46(3) _cell_angle_gamma 69.94(3) _cell_volume 1987.9(18) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 217 _cell_measurement_theta_min 3 _cell_measurement_theta_max 31 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.514 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 920 _exptl_absorpt_coefficient_mu 1.094 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.88 _exptl_absorpt_correction_T_max 0.89 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'MAR345 with image plate detector' _diffrn_measurement_method 'phi scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18781 _diffrn_reflns_av_R_equivalents 0.0481 _diffrn_reflns_av_sigmaI/netI 0.0473 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.59 _diffrn_reflns_theta_max 32.58 _reflns_number_total 10074 _reflns_number_gt 8148 _reflns_threshold_expression >2sigma(I) _computing_data_collection MARXDS _computing_cell_refinement AUTOMAR _computing_data_reduction MARSCALE _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP (Brueggermann and Smith, 1990)' _computing_publication_material 'PLATON (Spek, 1990)' _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^)+(0.0496P)^2^+0.4172P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10074 _refine_ls_number_parameters 478 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0502 _refine_ls_R_factor_gt 0.0401 _refine_ls_wR_factor_ref 0.1034 _refine_ls_wR_factor_gt 0.0995 _refine_ls_goodness_of_fit_ref 1.078 _refine_ls_restrained_S_all 1.078 _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 0.076966(18) 0.531057(18) 0.230657(9) 0.04027(6) Uani 1 1 d . . . Fe Fe -0.10331(5) 0.98159(4) 0.31700(2) 0.05271(10) Uani 1 1 d . . . P1 P 0.25125(6) 0.52549(6) 0.14436(3) 0.03804(12) Uani 1 1 d . . . Cl1 Cl -0.08833(7) 0.71803(7) 0.16263(3) 0.05530(17) Uani 1 1 d . . . N1 N -0.0553(2) 0.5274(2) 0.32444(10) 0.0429(4) Uani 1 1 d . . . N2 N -0.1747(2) 0.6058(2) 0.35478(10) 0.0433(4) Uani 1 1 d . . . C1 C -0.0639(5) 1.0292(4) 0.21289(18) 0.0891(12) Uani 1 1 d U . . H1 H -0.0068 0.9720 0.1851 0.107 Uiso 1 1 calc R . . C2 C -0.0150(4) 1.1043(4) 0.2477(2) 0.0889(13) Uani 1 1 d . . . H2 H 0.0795 1.1055 0.2465 0.107 Uiso 1 1 calc R . . C3 C -0.1337(4) 1.1745(3) 0.2833(2) 0.0792(10) Uani 1 1 d . . . H3 H -0.1330 1.2307 0.3110 0.095 Uiso 1 1 calc R . . C4 C -0.2552(4) 1.1473(3) 0.2710(2) 0.0709(8) Uani 1 1 d U . . H4 H -0.3493 1.1835 0.2887 0.085 Uiso 1 1 calc R . . C5 C -0.2140(4) 1.0578(3) 0.22841(17) 0.0711(7) Uani 1 1 d U . . H5 H -0.2745 1.0230 0.2129 0.085 Uiso 1 1 calc R . . C6 C -0.1933(5) 0.8966(3) 0.40618(16) 0.0782(11) Uani 1 1 d . . . H6 H -0.2892 0.9251 0.4234 0.094 Uiso 1 1 calc R . . C7 C -0.0737(7) 0.9326(5) 0.42066(18) 0.1070(19) Uani 1 1 d . . . H7 H -0.0796 0.9887 0.4496 0.128 Uiso 1 1 calc R . . C8 C 0.0518(6) 0.8697(4) 0.3842(3) 0.0996(16) Uani 1 1 d . . . H8 H 0.1430 0.8777 0.3844 0.119 Uiso 1 1 calc R . . C9 C 0.0171(4) 0.7915(3) 0.3467(2) 0.0726(10) Uani 1 1 d . . . H9 H 0.0812 0.7387 0.3186 0.087 Uiso 1 1 calc R . . C10 C -0.1346(3) 0.8086(3) 0.36012(14) 0.0528(6) Uani 1 1 d . . . C11 C -0.2181(3) 0.7474(2) 0.32866(13) 0.0464(5) Uani 1 1 d . . . H11A H -0.3211 0.7857 0.3395 0.056 Uiso 1 1 calc R . . H11B H -0.2017 0.7653 0.2784 0.056 Uiso 1 1 calc R . . C12 C -0.2074(3) 0.5429(3) 0.41919(12) 0.0445(5) Uani 1 1 d . . . C13 C -0.3325(3) 0.6060(3) 0.46339(13) 0.0469(5) Uani 1 1 d . . . C14 C -0.4721(3) 0.6525(3) 0.44098(14) 0.0577(7) Uani 1 1 d . . . H14 H -0.4885 0.6430 0.3976 0.069 Uiso 1 1 calc R . . C15 C -0.5883(3) 0.7133(4) 0.48274(17) 0.0693(9) Uani 1 1 d . . . H15 H -0.6816 0.7455 0.4668 0.083 Uiso 1 1 calc R . . C16 C -0.5662(4) 0.7260(4) 0.54704(17) 0.0725(9) Uani 1 1 d . . . H16 H -0.6445 0.7664 0.5748 0.087 Uiso 1 1 calc R . . C17 C -0.4285(4) 0.6791(4) 0.57074(17) 0.0725(9) Uani 1 1 d . . . H17 H -0.4136 0.6885 0.6144 0.087 Uiso 1 1 calc R . . C18 C -0.3108(3) 0.6173(3) 0.52951(15) 0.0597(7) Uani 1 1 d . . . H18 H -0.2180 0.5838 0.5461 0.072 Uiso 1 1 calc R . . C19 C -0.1068(3) 0.4201(3) 0.43059(13) 0.0496(6) Uani 1 1 d . . . H19 H -0.1018 0.3547 0.4699 0.060 Uiso 1 1 calc R . . C20 C -0.0131(3) 0.4143(3) 0.37029(12) 0.0443(5) Uani 1 1 d . . . C21 C 0.1146(3) 0.3149(2) 0.34855(12) 0.0431(5) Uani 1 1 d . . . C22 C 0.1653(3) 0.1921(3) 0.39007(15) 0.0568(7) Uani 1 1 d . . . H22 H 0.1166 0.1716 0.4325 0.068 Uiso 1 1 calc R . . C23 C 0.2888(3) 0.0995(3) 0.36836(16) 0.0595(7) Uani 1 1 d . . . H23 H 0.3239 0.0176 0.3964 0.071 Uiso 1 1 calc R . . C24 C 0.3584(3) 0.1306(3) 0.30490(15) 0.0564(6) Uani 1 1 d . . . H24 H 0.4402 0.0692 0.2897 0.068 Uiso 1 1 calc R . . C25 C 0.3065(3) 0.2536(2) 0.26369(13) 0.0474(5) Uani 1 1 d . . . H25 H 0.3546 0.2720 0.2208 0.057 Uiso 1 1 calc R . . C26 C 0.1861(3) 0.3502(2) 0.28362(12) 0.0429(5) Uani 1 1 d . . . C27 C 0.2690(3) 0.4039(2) 0.09342(12) 0.0423(5) Uani 1 1 d . . . C28 C 0.1404(3) 0.3944(4) 0.07648(19) 0.0684(9) Uani 1 1 d . . . H28 H 0.0518 0.4431 0.0944 0.082 Uiso 1 1 calc R . . C29 C 0.1436(4) 0.3123(4) 0.0327(2) 0.0816(11) Uani 1 1 d . . . H29 H 0.0572 0.3068 0.0215 0.098 Uiso 1 1 calc R . . C30 C 0.2730(4) 0.2402(3) 0.00638(17) 0.0647(8) Uani 1 1 d . . . H30 H 0.2744 0.1865 -0.0233 0.078 Uiso 1 1 calc R . . C31 C 0.3996(4) 0.2464(3) 0.02324(16) 0.0605(7) Uani 1 1 d . . . H31 H 0.4873 0.1956 0.0057 0.073 Uiso 1 1 calc R . . C32 C 0.3996(3) 0.3278(3) 0.06633(14) 0.0492(6) Uani 1 1 d . . . H32 H 0.4871 0.3316 0.0772 0.059 Uiso 1 1 calc R . . C33 C 0.4301(2) 0.5042(2) 0.17307(12) 0.0399(5) Uani 1 1 d . . . C34 C 0.5447(3) 0.5124(3) 0.12391(13) 0.0475(5) Uani 1 1 d . . . H34 H 0.5311 0.5247 0.0768 0.057 Uiso 1 1 calc R . . C35 C 0.6778(3) 0.5024(3) 0.14484(16) 0.0567(7) Uani 1 1 d . . . H35 H 0.7540 0.5062 0.1120 0.068 Uiso 1 1 calc R . . C36 C 0.6969(3) 0.4868(3) 0.21411(17) 0.0574(7) Uani 1 1 d . . . H36 H 0.7865 0.4797 0.2283 0.069 Uiso 1 1 calc R . . C37 C 0.5840(3) 0.4817(3) 0.26296(15) 0.0541(6) Uani 1 1 d . . . H37 H 0.5972 0.4727 0.3098 0.065 Uiso 1 1 calc R . . C38 C 0.4507(3) 0.4900(2) 0.24228(13) 0.0445(5) Uani 1 1 d . . . H38 H 0.3750 0.4860 0.2754 0.053 Uiso 1 1 calc R . . C39 C 0.2242(2) 0.6760(2) 0.07857(12) 0.0424(5) Uani 1 1 d . . . C40 C 0.2199(3) 0.6804(3) 0.00865(13) 0.0512(6) Uani 1 1 d . . . H40 H 0.2301 0.6053 -0.0065 0.061 Uiso 1 1 calc R . . C41 C 0.2004(3) 0.7970(3) -0.03942(15) 0.0644(8) Uani 1 1 d . . . H41 H 0.1967 0.7993 -0.0864 0.077 Uiso 1 1 calc R . . C42 C 0.1865(3) 0.9085(3) -0.01749(18) 0.0670(9) Uani 1 1 d . . . H42 H 0.1729 0.9863 -0.0495 0.080 Uiso 1 1 calc R . . C43 C 0.1930(3) 0.9041(3) 0.05260(18) 0.0622(7) Uani 1 1 d . . . H43 H 0.1848 0.9792 0.0675 0.075 Uiso 1 1 calc R . . C44 C 0.2118(3) 0.7884(3) 0.10086(14) 0.0507(6) Uani 1 1 d . . . H44 H 0.2161 0.7861 0.1478 0.061 Uiso 1 1 calc R . . Cl2 Cl 0.38872(15) 0.82523(11) 0.25688(6) 0.0995(3) Uani 1 1 d . . . Cl3 Cl 0.49224(16) 0.97197(12) 0.13355(7) 0.1125(4) Uani 1 1 d . . . C45 C 0.5105(4) 0.8189(3) 0.1828(2) 0.0768(10) Uani 1 1 d . . . H45A H 0.6093 0.7781 0.1975 0.092 Uiso 1 1 calc R . . H45B H 0.4924 0.7666 0.1546 0.092 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 0.03708(9) 0.04817(11) 0.03504(9) -0.00541(7) 0.00169(6) -0.01650(8) Fe 0.0598(2) 0.0479(2) 0.0487(2) -0.00061(16) -0.00809(17) -0.01958(19) P1 0.0354(3) 0.0459(3) 0.0328(3) -0.0060(2) 0.0006(2) -0.0153(2) Cl1 0.0421(3) 0.0673(4) 0.0422(3) 0.0029(3) -0.0005(2) -0.0098(3) N1 0.0460(10) 0.0506(11) 0.0321(9) -0.0059(8) 0.0056(7) -0.0203(9) N2 0.0420(10) 0.0496(11) 0.0366(10) -0.0070(8) 0.0046(7) -0.0167(9) C1 0.102(2) 0.095(3) 0.0463(17) 0.0033(17) 0.0129(16) -0.020(2) C2 0.061(2) 0.089(3) 0.102(3) 0.033(2) -0.0148(19) -0.038(2) C3 0.085(3) 0.0496(18) 0.100(3) 0.0046(17) -0.025(2) -0.0243(18) C4 0.0622(17) 0.0531(17) 0.087(2) -0.0026(13) -0.0164(14) -0.0091(14) C5 0.0927(18) 0.0636(18) 0.0557(17) 0.0085(12) -0.0239(15) -0.0303(17) C6 0.137(3) 0.071(2) 0.0416(15) -0.0100(14) 0.0082(18) -0.058(2) C7 0.214(6) 0.099(3) 0.0402(17) 0.0097(18) -0.033(3) -0.097(4) C8 0.116(3) 0.088(3) 0.107(3) 0.025(2) -0.070(3) -0.055(3) C9 0.0605(18) 0.0474(16) 0.099(3) 0.0125(16) -0.0307(17) -0.0126(14) C10 0.0662(17) 0.0434(13) 0.0469(14) -0.0002(10) -0.0067(12) -0.0201(12) C11 0.0488(13) 0.0465(13) 0.0381(11) -0.0002(9) 0.0015(9) -0.0150(11) C12 0.0410(11) 0.0580(15) 0.0358(11) -0.0079(10) 0.0019(8) -0.0203(11) C13 0.0475(12) 0.0574(15) 0.0387(12) -0.0083(10) 0.0073(9) -0.0254(12) C14 0.0498(14) 0.077(2) 0.0415(13) -0.0087(13) 0.0013(10) -0.0185(14) C15 0.0466(14) 0.083(2) 0.0600(18) -0.0026(16) 0.0043(12) -0.0092(15) C16 0.0632(18) 0.082(2) 0.0604(19) -0.0170(17) 0.0165(14) -0.0136(18) C17 0.071(2) 0.104(3) 0.0502(17) -0.0325(17) 0.0095(14) -0.031(2) C18 0.0500(14) 0.086(2) 0.0465(14) -0.0193(14) 0.0021(11) -0.0246(15) C19 0.0515(13) 0.0569(15) 0.0393(12) -0.0040(10) 0.0077(10) -0.0236(12) C20 0.0423(11) 0.0571(14) 0.0367(11) -0.0081(10) 0.0031(9) -0.0229(11) C21 0.0502(13) 0.0442(13) 0.0375(11) -0.0049(9) -0.0007(9) -0.0214(11) C22 0.0652(17) 0.0552(16) 0.0483(14) -0.0032(12) 0.0038(12) -0.0249(14) C23 0.0654(17) 0.0459(15) 0.0597(17) -0.0021(12) -0.0015(13) -0.0150(13) C24 0.0596(16) 0.0495(15) 0.0585(16) -0.0133(12) 0.0017(12) -0.0158(13) C25 0.0490(13) 0.0468(13) 0.0446(12) -0.0100(10) 0.0045(10) -0.0155(11) C26 0.0456(12) 0.0450(13) 0.0418(12) -0.0062(9) -0.0008(9) -0.0215(11) C27 0.0411(11) 0.0483(13) 0.0390(11) -0.0073(9) -0.0030(9) -0.0171(10) C28 0.0459(14) 0.088(2) 0.086(2) -0.0391(19) -0.0029(14) -0.0262(16) C29 0.0595(19) 0.098(3) 0.106(3) -0.049(2) -0.0199(19) -0.025(2) C30 0.084(2) 0.0602(18) 0.0584(17) -0.0186(14) -0.0084(15) -0.0286(17) C31 0.0653(18) 0.0634(18) 0.0588(17) -0.0258(14) 0.0068(13) -0.0234(15) C32 0.0438(12) 0.0574(15) 0.0483(13) -0.0130(11) 0.0042(10) -0.0198(12) C33 0.0388(11) 0.0426(12) 0.0403(11) -0.0069(9) -0.0064(8) -0.0154(10) C34 0.0444(12) 0.0576(15) 0.0417(12) -0.0092(11) -0.0007(9) -0.0192(12) C35 0.0408(12) 0.0634(17) 0.0655(17) -0.0067(13) -0.0007(11) -0.0215(13) C36 0.0483(14) 0.0547(16) 0.0746(19) -0.0032(13) -0.0189(13) -0.0245(13) C37 0.0622(16) 0.0538(15) 0.0491(14) -0.0013(11) -0.0245(12) -0.0207(13) C38 0.0449(12) 0.0476(13) 0.0411(12) -0.0079(10) -0.0047(9) -0.0148(11) C39 0.0357(10) 0.0528(13) 0.0353(11) -0.0005(9) 0.0016(8) -0.0168(10) C40 0.0469(13) 0.0637(16) 0.0391(12) -0.0053(11) 0.0010(9) -0.0178(12) C41 0.0560(16) 0.081(2) 0.0434(14) 0.0091(14) -0.0054(11) -0.0190(16) C42 0.0554(16) 0.0620(19) 0.0669(19) 0.0167(15) -0.0015(14) -0.0183(15) C43 0.0527(15) 0.0469(15) 0.080(2) -0.0048(14) -0.0013(14) -0.0142(13) C44 0.0525(14) 0.0518(15) 0.0471(13) -0.0049(11) -0.0020(11) -0.0195(12) Cl2 0.1281(10) 0.0884(7) 0.0891(7) -0.0274(6) 0.0027(6) -0.0410(7) Cl3 0.1363(11) 0.0836(7) 0.1088(9) 0.0005(6) -0.0128(8) -0.0358(7) C45 0.072(2) 0.0576(19) 0.095(3) -0.0215(18) -0.0215(19) -0.0028(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd C26 2.043(3) . ? Pd N1 2.122(2) . ? Pd P1 2.2492(12) . ? Pd Cl1 2.4007(14) . ? Fe C1 2.024(4) . ? Fe C8 2.026(4) . ? Fe C7 2.029(3) . ? Fe C5 2.036(3) . ? Fe C3 2.037(3) . ? Fe C2 2.037(3) . ? Fe C10 2.039(3) . ? Fe C9 2.039(3) . ? Fe C4 2.042(3) . ? Fe C6 2.046(3) . ? P1 C27 1.828(3) . ? P1 C39 1.836(3) . ? P1 C33 1.837(3) . ? N1 C20 1.343(3) . ? N1 N2 1.365(3) . ? N2 C12 1.362(3) . ? N2 C11 1.477(3) . ? C1 C5 1.403(6) . ? C1 C2 1.433(6) . ? C1 H1 0.9300 . ? C2 C3 1.374(6) . ? C2 H2 0.9300 . ? C3 C4 1.391(5) . ? C3 H3 0.9300 . ? C4 C5 1.382(5) . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? C6 C10 1.425(5) . ? C6 C7 1.447(6) . ? C6 H6 0.9300 . ? C7 C8 1.395(7) . ? C7 H7 0.9300 . ? C8 C9 1.418(6) . ? C8 H8 0.9300 . ? C9 C10 1.432(5) . ? C9 H9 0.9300 . ? C10 C11 1.500(4) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 C19 1.380(4) . ? C12 C13 1.479(4) . ? C13 C14 1.381(4) . ? C13 C18 1.394(4) . ? C14 C15 1.390(4) . ? C14 H14 0.9300 . ? C15 C16 1.366(5) . ? C15 H15 0.9300 . ? C16 C17 1.374(5) . ? C16 H16 0.9300 . ? C17 C18 1.396(4) . ? C17 H17 0.9300 . ? C18 H18 0.9300 . ? C19 C20 1.408(3) . ? C19 H19 0.9300 . ? C20 C21 1.458(4) . ? C21 C22 1.389(4) . ? C21 C26 1.420(3) . ? C22 C23 1.394(4) . ? C22 H22 0.9300 . ? C23 C24 1.378(4) . ? C23 H23 0.9300 . ? C24 C25 1.389(4) . ? C24 H24 0.9300 . ? C25 C26 1.388(4) . ? C25 H25 0.9300 . ? C27 C28 1.392(4) . ? C27 C32 1.394(4) . ? C28 C29 1.395(5) . ? C28 H28 0.9300 . ? C29 C30 1.364(5) . ? C29 H29 0.9300 . ? C30 C31 1.357(4) . ? C30 H30 0.9300 . ? C31 C32 1.387(4) . ? C31 H31 0.9300 . ? C32 H32 0.9300 . ? C33 C38 1.375(3) . ? C33 C34 1.401(3) . ? C34 C35 1.382(4) . ? C34 H34 0.9300 . ? C35 C36 1.371(4) . ? C35 H35 0.9300 . ? C36 C37 1.379(4) . ? C36 H36 0.9300 . ? C37 C38 1.389(3) . ? C37 H37 0.9300 . ? C38 H38 0.9300 . ? C39 C40 1.379(3) . ? C39 C44 1.394(4) . ? C40 C41 1.395(4) . ? C40 H40 0.9300 . ? C41 C42 1.377(5) . ? C41 H41 0.9300 . ? C42 C43 1.386(5) . ? C42 H42 0.9300 . ? C43 C44 1.391(4) . ? C43 H43 0.9300 . ? C44 H44 0.9300 . ? Cl2 C45 1.764(4) . ? Cl3 C45 1.727(4) . ? C45 H45A 0.9700 . ? C45 H45B 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C26 Pd N1 80.46(10) . . ? C26 Pd P1 93.18(8) . . ? N1 Pd P1 169.28(6) . . ? C26 Pd Cl1 166.34(7) . . ? N1 Pd Cl1 97.13(7) . . ? P1 Pd Cl1 91.05(5) . . ? C1 Fe C8 123.8(2) . . ? C1 Fe C7 161.0(2) . . ? C8 Fe C7 40.2(2) . . ? C1 Fe C5 40.43(16) . . ? C8 Fe C5 161.2(2) . . ? C7 Fe C5 157.5(2) . . ? C1 Fe C3 67.70(19) . . ? C8 Fe C3 120.84(17) . . ? C7 Fe C3 109.11(18) . . ? C5 Fe C3 67.43(15) . . ? C1 Fe C2 41.32(18) . . ? C8 Fe C2 106.59(18) . . ? C7 Fe C2 124.25(19) . . ? C5 Fe C2 68.23(16) . . ? C3 Fe C2 39.43(17) . . ? C1 Fe C10 119.92(17) . . ? C8 Fe C10 68.93(15) . . ? C7 Fe C10 68.71(14) . . ? C5 Fe C10 107.86(13) . . ? C3 Fe C10 163.32(15) . . ? C2 Fe C10 155.59(18) . . ? C1 Fe C9 106.16(18) . . ? C8 Fe C9 40.84(17) . . ? C7 Fe C9 68.3(2) . . ? C5 Fe C9 124.67(16) . . ? C3 Fe C9 154.86(15) . . ? C2 Fe C9 119.85(17) . . ? C10 Fe C9 41.11(13) . . ? C1 Fe C4 67.07(17) . . ? C8 Fe C4 156.66(18) . . ? C7 Fe C4 123.4(2) . . ? C5 Fe C4 39.62(15) . . ? C3 Fe C4 39.88(14) . . ? C2 Fe C4 66.81(16) . . ? C10 Fe C4 126.48(14) . . ? C9 Fe C4 162.19(15) . . ? C1 Fe C6 155.42(18) . . ? C8 Fe C6 69.3(2) . . ? C7 Fe C6 41.58(18) . . ? C5 Fe C6 121.20(17) . . ? C3 Fe C6 126.57(17) . . ? C2 Fe C6 162.05(18) . . ? C10 Fe C6 40.83(13) . . ? C9 Fe C6 69.20(17) . . ? C4 Fe C6 109.65(18) . . ? C27 P1 C39 103.59(12) . . ? C27 P1 C33 109.52(11) . . ? C39 P1 C33 100.14(11) . . ? C27 P1 Pd 112.83(9) . . ? C39 P1 Pd 115.41(9) . . ? C33 P1 Pd 114.17(9) . . ? C20 N1 N2 106.47(19) . . ? C20 N1 Pd 113.67(16) . . ? N2 N1 Pd 139.86(16) . . ? C12 N2 N1 110.5(2) . . ? C12 N2 C11 126.9(2) . . ? N1 N2 C11 119.12(19) . . ? C5 C1 C2 107.3(4) . . ? C5 C1 Fe 70.24(19) . . ? C2 C1 Fe 69.8(2) . . ? C5 C1 H1 126.3 . . ? C2 C1 H1 126.3 . . ? Fe C1 H1 125.2 . . ? C3 C2 C1 107.4(3) . . ? C3 C2 Fe 70.3(2) . . ? C1 C2 Fe 68.9(2) . . ? C3 C2 H2 126.3 . . ? C1 C2 H2 126.3 . . ? Fe C2 H2 126.1 . . ? C2 C3 C4 108.6(4) . . ? C2 C3 Fe 70.3(2) . . ? C4 C3 Fe 70.26(19) . . ? C2 C3 H3 125.7 . . ? C4 C3 H3 125.7 . . ? Fe C3 H3 125.3 . . ? C5 C4 C3 109.2(4) . . ? C5 C4 Fe 69.97(19) . . ? C3 C4 Fe 69.86(19) . . ? C5 C4 H4 125.4 . . ? C3 C4 H4 125.4 . . ? Fe C4 H4 126.4 . . ? C4 C5 C1 107.5(3) . . ? C4 C5 Fe 70.41(19) . . ? C1 C5 Fe 69.3(2) . . ? C4 C5 H5 126.3 . . ? C1 C5 H5 126.3 . . ? Fe C5 H5 125.6 . . ? C10 C6 C7 106.1(4) . . ? C10 C6 Fe 69.29(17) . . ? C7 C6 Fe 68.6(2) . . ? C10 C6 H6 126.9 . . ? C7 C6 H6 126.9 . . ? Fe C6 H6 126.8 . . ? C8 C7 C6 109.1(4) . . ? C8 C7 Fe 69.8(2) . . ? C6 C7 Fe 69.86(19) . . ? C8 C7 H7 125.4 . . ? C6 C7 H7 125.4 . . ? Fe C7 H7 126.5 . . ? C7 C8 C9 108.5(4) . . ? C7 C8 Fe 70.0(2) . . ? C9 C8 Fe 70.07(18) . . ? C7 C8 H8 125.7 . . ? C9 C8 H8 125.7 . . ? Fe C8 H8 125.8 . . ? C8 C9 C10 107.6(4) . . ? C8 C9 Fe 69.1(2) . . ? C10 C9 Fe 69.44(17) . . ? C8 C9 H9 126.2 . . ? C10 C9 H9 126.2 . . ? Fe C9 H9 126.8 . . ? C6 C10 C9 108.6(3) . . ? C6 C10 C11 126.0(3) . . ? C9 C10 C11 125.4(3) . . ? C6 C10 Fe 69.88(17) . . ? C9 C10 Fe 69.45(16) . . ? C11 C10 Fe 124.89(18) . . ? N2 C11 C10 111.8(2) . . ? N2 C11 H11A 109.3 . . ? C10 C11 H11A 109.3 . . ? N2 C11 H11B 109.3 . . ? C10 C11 H11B 109.3 . . ? H11A C11 H11B 107.9 . . ? N2 C12 C19 107.4(2) . . ? N2 C12 C13 121.5(2) . . ? C19 C12 C13 131.0(2) . . ? C14 C13 C18 118.9(3) . . ? C14 C13 C12 121.2(2) . . ? C18 C13 C12 119.9(2) . . ? C13 C14 C15 120.5(3) . . ? C13 C14 H14 119.7 . . ? C15 C14 H14 119.7 . . ? C16 C15 C14 120.4(3) . . ? C16 C15 H15 119.8 . . ? C14 C15 H15 119.8 . . ? C15 C16 C17 120.1(3) . . ? C15 C16 H16 120.0 . . ? C17 C16 H16 120.0 . . ? C16 C17 C18 120.2(3) . . ? C16 C17 H17 119.9 . . ? C18 C17 H17 119.9 . . ? C13 C18 C17 119.9(3) . . ? C13 C18 H18 120.0 . . ? C17 C18 H18 120.0 . . ? C12 C19 C20 105.7(2) . . ? C12 C19 H19 127.2 . . ? C20 C19 H19 127.2 . . ? N1 C20 C19 109.9(2) . . ? N1 C20 C21 116.0(2) . . ? C19 C20 C21 134.1(2) . . ? C22 C21 C26 121.7(3) . . ? C22 C21 C20 121.4(2) . . ? C26 C21 C20 116.9(2) . . ? C21 C22 C23 120.1(3) . . ? C21 C22 H22 119.9 . . ? C23 C22 H22 119.9 . . ? C24 C23 C22 119.3(3) . . ? C24 C23 H23 120.4 . . ? C22 C23 H23 120.4 . . ? C23 C24 C25 120.1(3) . . ? C23 C24 H24 120.0 . . ? C25 C24 H24 120.0 . . ? C26 C25 C24 122.9(2) . . ? C26 C25 H25 118.5 . . ? C24 C25 H25 118.5 . . ? C25 C26 C21 115.9(2) . . ? C25 C26 Pd 130.98(19) . . ? C21 C26 Pd 112.71(18) . . ? C28 C27 C32 118.0(3) . . ? C28 C27 P1 116.6(2) . . ? C32 C27 P1 125.2(2) . . ? C27 C28 C29 120.4(3) . . ? C27 C28 H28 119.8 . . ? C29 C28 H28 119.8 . . ? C30 C29 C28 120.2(3) . . ? C30 C29 H29 119.9 . . ? C28 C29 H29 119.9 . . ? C31 C30 C29 120.3(3) . . ? C31 C30 H30 119.9 . . ? C29 C30 H30 119.9 . . ? C30 C31 C32 120.7(3) . . ? C30 C31 H31 119.6 . . ? C32 C31 H31 119.6 . . ? C31 C32 C27 120.3(3) . . ? C31 C32 H32 119.8 . . ? C27 C32 H32 119.8 . . ? C38 C33 C34 119.0(2) . . ? C38 C33 P1 120.75(19) . . ? C34 C33 P1 120.08(18) . . ? C35 C34 C33 120.5(2) . . ? C35 C34 H34 119.7 . . ? C33 C34 H34 119.7 . . ? C36 C35 C34 119.7(3) . . ? C36 C35 H35 120.1 . . ? C34 C35 H35 120.1 . . ? C35 C36 C37 120.4(2) . . ? C35 C36 H36 119.8 . . ? C37 C36 H36 119.8 . . ? C36 C37 C38 120.1(3) . . ? C36 C37 H37 120.0 . . ? C38 C37 H37 120.0 . . ? C33 C38 C37 120.3(2) . . ? C33 C38 H38 119.9 . . ? C37 C38 H38 119.9 . . ? C40 C39 C44 119.5(2) . . ? C40 C39 P1 122.6(2) . . ? C44 C39 P1 117.91(19) . . ? C39 C40 C41 120.4(3) . . ? C39 C40 H40 119.8 . . ? C41 C40 H40 119.8 . . ? C42 C41 C40 120.2(3) . . ? C42 C41 H41 119.9 . . ? C40 C41 H41 119.9 . . ? C41 C42 C43 119.6(3) . . ? C41 C42 H42 120.2 . . ? C43 C42 H42 120.2 . . ? C42 C43 C44 120.5(3) . . ? C42 C43 H43 119.7 . . ? C44 C43 H43 119.7 . . ? C43 C44 C39 119.7(3) . . ? C43 C44 H44 120.1 . . ? C39 C44 H44 120.1 . . ? Cl3 C45 Cl2 111.4(2) . . ? Cl3 C45 H45A 109.3 . . ? Cl2 C45 H45A 109.3 . . ? Cl3 C45 H45B 109.3 . . ? Cl2 C45 H45B 109.3 . . ? H45A C45 H45B 108.0 . . ? _diffrn_measured_fraction_theta_max 0.697 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.925 _refine_diff_density_max 0.536 _refine_diff_density_min -0.761 _refine_diff_density_rms 0.060 #==END data_chnm55a _database_code_depnum_ccdc_archive 'CCDC 826858' #TrackingRef 'TOT.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C44 H36 Cl Fe N2 P Pd' _chemical_formula_sum 'C44 H36 Cl Fe N2 P Pd' _chemical_formula_weight 821.42 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' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.625(6) _cell_length_b 12.789(5) _cell_length_c 14.469(6) _cell_angle_alpha 93.58(2) _cell_angle_beta 105.39(2) _cell_angle_gamma 107.09(2) _cell_volume 1790.7(14) _cell_formula_units_Z 2 _cell_measurement_temperature 233(2) _cell_measurement_reflns_used 257 _cell_measurement_theta_min 3 _cell_measurement_theta_max 31 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.523 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 836 _exptl_absorpt_coefficient_mu 1.062 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.90 _exptl_absorpt_correction_T_max 0.91 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 233(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 'MAR345 with image plate detector' _diffrn_measurement_method 'phi scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16450 _diffrn_reflns_av_R_equivalents 0.0502 _diffrn_reflns_av_sigmaI/netI 0.0864 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.87 _diffrn_reflns_theta_max 32.12 _reflns_number_total 8927 _reflns_number_gt 6689 _reflns_threshold_expression >2sigma(I) _computing_data_collection MARXDS _computing_cell_refinement AUTOMAR _computing_data_reduction MARSCALE _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP (Brueggermann and Smith, 1990)' _computing_publication_material 'PLATON (Spek, 1990)' _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^)+(0.1101P)^2^+0.0973P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.017(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 8927 _refine_ls_number_parameters 452 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0763 _refine_ls_R_factor_gt 0.0624 _refine_ls_wR_factor_ref 0.1978 _refine_ls_wR_factor_gt 0.1884 _refine_ls_goodness_of_fit_ref 1.089 _refine_ls_restrained_S_all 1.091 _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 0.31549(3) 0.73885(2) 0.21419(2) 0.05638(13) Uani 1 1 d U . . Fe Fe 0.18529(7) 0.56475(5) 0.37333(5) 0.06263(18) Uani 1 1 d . . . P P 0.17578(11) 0.83425(9) 0.15291(8) 0.0574(2) Uani 1 1 d . . . Cl Cl 0.39065(12) 0.72670(10) 0.07329(8) 0.0700(3) Uani 1 1 d U . . N1 N 0.4523(4) 0.5617(3) 0.2572(2) 0.0591(7) Uani 1 1 d . . . N2 N 0.4718(3) 0.6699(3) 0.2776(2) 0.0561(7) Uani 1 1 d . . . C1 C 0.2373(4) 0.7164(3) 0.3269(3) 0.0597(8) Uani 1 1 d . . . C2 C 0.0968(5) 0.6797(4) 0.3267(4) 0.0704(10) Uani 1 1 d . . . H2 H 0.0210 0.6685 0.2726 0.085 Uiso 1 1 calc R . . C3 C 0.0902(5) 0.6630(4) 0.4224(4) 0.0714(11) Uani 1 1 d . . . H3 H 0.0104 0.6373 0.4409 0.086 Uiso 1 1 calc R . . C4 C 0.2278(6) 0.6928(4) 0.4838(4) 0.0787(12) Uani 1 1 d . . . H4 H 0.2554 0.6943 0.5507 0.094 Uiso 1 1 calc R . . C5 C 0.3154(5) 0.7199(4) 0.4237(3) 0.0694(10) Uani 1 1 d . . . H5 H 0.4108 0.7376 0.4450 0.083 Uiso 1 1 calc R . . C6 C 0.0911(5) 0.4212(4) 0.2739(4) 0.0713(11) Uani 1 1 d . . . H6 H 0.0256 0.4108 0.2140 0.086 Uiso 1 1 calc R . . C7 C 0.0644(6) 0.4036(5) 0.3636(4) 0.0856(14) Uani 1 1 d . . . H7 H -0.0222 0.3797 0.3730 0.103 Uiso 1 1 calc R . . C8 C 0.1947(6) 0.4288(4) 0.4377(4) 0.0819(13) Uani 1 1 d . . . H8 H 0.2067 0.4236 0.5031 0.098 Uiso 1 1 calc R . . C9 C 0.3024(5) 0.4633(4) 0.3932(4) 0.0674(10) Uani 1 1 d . . . H9 H 0.3965 0.4848 0.4247 0.081 Uiso 1 1 calc R . . C10 C 0.2407(4) 0.4590(3) 0.2933(3) 0.0619(9) Uani 1 1 d . . . C11 C 0.3128(4) 0.4847(4) 0.2156(3) 0.0651(9) Uani 1 1 d . . . H11A H 0.3165 0.4167 0.1847 0.078 Uiso 1 1 calc R . . H11B H 0.2605 0.5166 0.1665 0.078 Uiso 1 1 calc R . . C12 C 0.6118(4) 0.7212(3) 0.3084(3) 0.0598(8) Uani 1 1 d . . . C13 C 0.6751(4) 0.6413(4) 0.3081(3) 0.0632(9) Uani 1 1 d . . . H13 H 0.7695 0.6531 0.3266 0.076 Uiso 1 1 calc R . . C14 C 0.5723(4) 0.5407(3) 0.2752(3) 0.0619(9) Uani 1 1 d . . . C15 C 0.6777(4) 0.8436(4) 0.3361(3) 0.0622(8) Uani 1 1 d U . . C16 C 0.6056(5) 0.9143(4) 0.3497(4) 0.0728(11) Uani 1 1 d U . . H16 H 0.5111 0.8861 0.3403 0.087 Uiso 1 1 calc R . . C17 C 0.6734(5) 1.0273(4) 0.3773(4) 0.0751(11) Uani 1 1 d . . . H17 H 0.6242 1.0745 0.3859 0.090 Uiso 1 1 calc R . . C18 C 0.8133(6) 1.0693(5) 0.3919(4) 0.0843(14) Uani 1 1 d . . . H18 H 0.8588 1.1449 0.4109 0.101 Uiso 1 1 calc R . . C19 C 0.8852(6) 1.0002(5) 0.3784(5) 0.0920(16) Uani 1 1 d . . . H19 H 0.9797 1.0293 0.3882 0.110 Uiso 1 1 calc R . . C20 C 0.8198(5) 0.8869(5) 0.3504(4) 0.0795(12) Uani 1 1 d . . . H20 H 0.8699 0.8406 0.3413 0.095 Uiso 1 1 calc R . . C21 C 0.5878(5) 0.4300(4) 0.2603(3) 0.0658(9) Uani 1 1 d . . . C22 C 0.5065(5) 0.3369(4) 0.2864(4) 0.0774(12) Uani 1 1 d . . . H22 H 0.4410 0.3428 0.3163 0.093 Uiso 1 1 calc R . . C23 C 0.5236(5) 0.2354(4) 0.2676(4) 0.0749(11) Uani 1 1 d . . . H23 H 0.4707 0.1733 0.2864 0.090 Uiso 1 1 calc R . . C24 C 0.6181(6) 0.2253(5) 0.2213(4) 0.0804(13) Uani 1 1 d . . . H24 H 0.6272 0.1563 0.2077 0.097 Uiso 1 1 calc R . . C25 C 0.7001(6) 0.3181(4) 0.1949(4) 0.0774(12) Uani 1 1 d . . . H25 H 0.7651 0.3118 0.1646 0.093 Uiso 1 1 calc R . . C26 C 0.6836(6) 0.4201(5) 0.2143(4) 0.0827(13) Uani 1 1 d . . . H26 H 0.7374 0.4823 0.1963 0.099 Uiso 1 1 calc R . . C27 C -0.0040(5) 0.7489(4) 0.1078(3) 0.0651(9) Uani 1 1 d . . . C28 C -0.0325(5) 0.6384(4) 0.0733(3) 0.0698(10) Uani 1 1 d . . . H28 H 0.0394 0.6105 0.0748 0.084 Uiso 1 1 calc R . . C29 C -0.1678(6) 0.5693(5) 0.0366(4) 0.0820(13) Uani 1 1 d . . . H29 H -0.1859 0.4957 0.0121 0.098 Uiso 1 1 calc R . . C30 C -0.2762(6) 0.6082(5) 0.0359(4) 0.0846(14) Uani 1 1 d . . . H30 H -0.3668 0.5613 0.0121 0.102 Uiso 1 1 calc R . . C31 C -0.2474(6) 0.7192(5) 0.0715(5) 0.0891(15) Uani 1 1 d . . . H31 H -0.3194 0.7467 0.0714 0.107 Uiso 1 1 calc R . . C32 C -0.1123(5) 0.7889(4) 0.1068(4) 0.0772(12) Uani 1 1 d . . . H32 H -0.0941 0.8629 0.1301 0.093 Uiso 1 1 calc R . . C33 C 0.1892(4) 0.9577(3) 0.2308(3) 0.0609(9) Uani 1 1 d . . . C34 C 0.2487(5) 0.9731(4) 0.3325(4) 0.0698(10) Uani 1 1 d . . . H34 H 0.2769 0.9174 0.3610 0.084 Uiso 1 1 calc R . . C35 C 0.2659(6) 1.0700(5) 0.3905(4) 0.0839(13) Uani 1 1 d . . . H35 H 0.3058 1.0792 0.4572 0.101 Uiso 1 1 calc R . . C36 C 0.2236(6) 1.1521(4) 0.3486(4) 0.0785(12) Uani 1 1 d . . . H36 H 0.2330 1.2164 0.3874 0.094 Uiso 1 1 calc R . . C37 C 0.1673(6) 1.1399(4) 0.2496(4) 0.0824(13) Uani 1 1 d . . . H37 H 0.1417 1.1969 0.2217 0.099 Uiso 1 1 calc R . . C38 C 0.1487(5) 1.0424(4) 0.1913(4) 0.0709(10) Uani 1 1 d . . . H38 H 0.1083 1.0343 0.1247 0.085 Uiso 1 1 calc R . . C39 C 0.2151(4) 0.8959(3) 0.0486(3) 0.0612(9) Uani 1 1 d . . . C40 C 0.1346(5) 0.8525(5) -0.0459(4) 0.0755(12) Uani 1 1 d . . . H40 H 0.0577 0.7896 -0.0582 0.091 Uiso 1 1 calc R . . C41 C 0.1684(6) 0.9027(5) -0.1223(4) 0.0777(12) Uani 1 1 d . . . H41 H 0.1134 0.8738 -0.1856 0.093 Uiso 1 1 calc R . . C42 C 0.2832(5) 0.9953(5) -0.1046(4) 0.0777(12) Uani 1 1 d . . . H42 H 0.3057 1.0287 -0.1559 0.093 Uiso 1 1 calc R . . C43 C 0.3655(6) 1.0389(5) -0.0094(4) 0.0828(13) Uani 1 1 d . . . H43 H 0.4429 1.1014 0.0030 0.099 Uiso 1 1 calc R . . C44 C 0.3312(5) 0.9887(4) 0.0656(4) 0.0731(11) Uani 1 1 d . . . H44 H 0.3866 1.0173 0.1289 0.088 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 0.0570(2) 0.05605(19) 0.0570(2) 0.00854(12) 0.01667(12) 0.01971(13) Fe 0.0652(4) 0.0641(4) 0.0609(3) 0.0112(3) 0.0202(3) 0.0226(3) P 0.0572(5) 0.0584(5) 0.0568(5) 0.0087(4) 0.0154(4) 0.0205(4) Cl 0.0746(6) 0.0728(6) 0.0685(6) 0.0131(5) 0.0266(5) 0.0273(5) N1 0.0617(18) 0.0577(17) 0.0581(18) 0.0065(13) 0.0165(13) 0.0215(14) N2 0.0555(17) 0.0531(16) 0.0588(17) 0.0074(13) 0.0126(13) 0.0203(13) C1 0.063(2) 0.058(2) 0.060(2) 0.0112(16) 0.0205(16) 0.0216(16) C2 0.077(3) 0.072(3) 0.068(3) 0.013(2) 0.026(2) 0.029(2) C3 0.080(3) 0.076(3) 0.071(3) 0.018(2) 0.031(2) 0.034(2) C4 0.086(3) 0.082(3) 0.070(3) 0.007(2) 0.026(2) 0.029(2) C5 0.073(3) 0.067(2) 0.068(3) 0.0061(19) 0.0183(19) 0.0252(19) C6 0.068(2) 0.068(3) 0.074(3) 0.004(2) 0.024(2) 0.0152(19) C7 0.088(3) 0.077(3) 0.095(4) 0.014(3) 0.036(3) 0.023(3) C8 0.093(3) 0.073(3) 0.087(3) 0.023(3) 0.035(3) 0.030(2) C9 0.072(3) 0.066(2) 0.075(3) 0.017(2) 0.029(2) 0.030(2) C10 0.064(2) 0.057(2) 0.065(2) 0.0087(17) 0.0191(17) 0.0204(17) C11 0.065(2) 0.061(2) 0.064(2) 0.0029(17) 0.0152(17) 0.0177(17) C12 0.060(2) 0.060(2) 0.061(2) 0.0122(16) 0.0170(16) 0.0232(16) C13 0.057(2) 0.066(2) 0.065(2) 0.0098(18) 0.0151(16) 0.0201(17) C14 0.068(2) 0.056(2) 0.061(2) 0.0101(16) 0.0188(17) 0.0202(17) C15 0.064(2) 0.058(2) 0.060(2) 0.0085(16) 0.0134(16) 0.0164(15) C16 0.073(3) 0.069(3) 0.077(3) 0.012(2) 0.019(2) 0.0254(19) C17 0.079(3) 0.065(3) 0.079(3) 0.013(2) 0.020(2) 0.023(2) C18 0.085(3) 0.068(3) 0.092(4) 0.014(2) 0.025(3) 0.015(2) C19 0.079(3) 0.085(4) 0.100(4) 0.010(3) 0.022(3) 0.015(3) C20 0.071(3) 0.080(3) 0.084(3) 0.008(2) 0.023(2) 0.021(2) C21 0.070(2) 0.060(2) 0.071(3) 0.0137(18) 0.0214(19) 0.0241(18) C22 0.078(3) 0.068(3) 0.091(3) 0.014(2) 0.031(2) 0.025(2) C23 0.076(3) 0.064(2) 0.086(3) 0.013(2) 0.022(2) 0.027(2) C24 0.078(3) 0.075(3) 0.092(3) 0.007(2) 0.025(2) 0.031(2) C25 0.077(3) 0.071(3) 0.090(3) 0.015(2) 0.032(2) 0.026(2) C26 0.090(3) 0.078(3) 0.091(4) 0.019(3) 0.036(3) 0.033(3) C27 0.065(2) 0.066(2) 0.064(2) 0.0092(18) 0.0175(17) 0.0225(18) C28 0.071(3) 0.068(2) 0.067(2) 0.0114(19) 0.0181(19) 0.0203(19) C29 0.082(3) 0.079(3) 0.079(3) 0.009(2) 0.021(2) 0.020(2) C30 0.073(3) 0.089(4) 0.082(3) 0.013(3) 0.020(2) 0.015(2) C31 0.070(3) 0.091(4) 0.111(4) 0.022(3) 0.029(3) 0.030(3) C32 0.066(3) 0.072(3) 0.092(3) 0.011(2) 0.020(2) 0.023(2) C33 0.056(2) 0.0526(19) 0.074(2) 0.0077(17) 0.0174(17) 0.0200(15) C34 0.077(3) 0.062(2) 0.071(3) 0.0106(19) 0.023(2) 0.0226(19) C35 0.095(4) 0.083(3) 0.071(3) 0.005(2) 0.027(3) 0.025(3) C36 0.083(3) 0.070(3) 0.087(3) 0.008(2) 0.033(3) 0.027(2) C37 0.090(3) 0.068(3) 0.092(4) 0.012(2) 0.034(3) 0.024(2) C38 0.071(3) 0.064(2) 0.080(3) 0.015(2) 0.025(2) 0.0219(19) C39 0.064(2) 0.061(2) 0.063(2) 0.0130(17) 0.0183(17) 0.0257(17) C40 0.079(3) 0.082(3) 0.068(3) 0.011(2) 0.019(2) 0.033(2) C41 0.081(3) 0.096(4) 0.063(3) 0.016(2) 0.024(2) 0.037(3) C42 0.078(3) 0.082(3) 0.084(3) 0.022(2) 0.033(2) 0.032(2) C43 0.093(4) 0.078(3) 0.083(3) 0.018(3) 0.034(3) 0.028(3) C44 0.071(3) 0.072(3) 0.071(3) 0.010(2) 0.018(2) 0.017(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd C1 2.017(4) . ? Pd N2 2.128(3) . ? Pd P 2.2314(14) . ? Pd Cl 2.3907(14) . ? Fe C5 2.013(5) . ? Fe C2 2.025(5) . ? Fe C9 2.029(5) . ? Fe C3 2.030(5) . ? Fe C10 2.037(4) . ? Fe C8 2.038(5) . ? Fe C7 2.057(6) . ? Fe C1 2.061(4) . ? Fe C6 2.065(5) . ? Fe C4 2.073(5) . ? P C27 1.814(5) . ? P C33 1.828(4) . ? P C39 1.833(4) . ? N1 N2 1.339(4) . ? N1 C14 1.341(5) . ? N1 C11 1.457(5) . ? N2 C12 1.371(5) . ? C1 C5 1.416(6) . ? C1 C2 1.427(6) . ? C2 C3 1.431(6) . ? C2 H2 0.9300 . ? C3 C4 1.419(7) . ? C3 H3 0.9300 . ? C4 C5 1.421(7) . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? C6 C7 1.418(8) . ? C6 C10 1.461(6) . ? C6 H6 0.9300 . ? C7 C8 1.441(8) . ? C7 H7 0.9300 . ? C8 C9 1.431(7) . ? C8 H8 0.9300 . ? C9 C10 1.410(7) . ? C9 H9 0.9300 . ? C10 C11 1.521(6) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 C13 1.380(6) . ? C12 C15 1.493(6) . ? C13 C14 1.376(6) . ? C13 H13 0.9300 . ? C14 C21 1.482(6) . ? C15 C16 1.382(6) . ? C15 C20 1.399(7) . ? C16 C17 1.389(7) . ? C16 H16 0.9300 . ? C17 C18 1.375(8) . ? C17 H17 0.9300 . ? C18 C19 1.364(8) . ? C18 H18 0.9300 . ? C19 C20 1.389(8) . ? C19 H19 0.9300 . ? C20 H20 0.9300 . ? C21 C26 1.385(7) . ? C21 C22 1.391(7) . ? C22 C23 1.383(7) . ? C22 H22 0.9300 . ? C23 C24 1.376(7) . ? C23 H23 0.9300 . ? C24 C25 1.393(8) . ? C24 H24 0.9300 . ? C25 C26 1.387(7) . ? C25 H25 0.9300 . ? C26 H26 0.9300 . ? C27 C28 1.385(6) . ? C27 C32 1.387(6) . ? C28 C29 1.385(7) . ? C28 H28 0.9300 . ? C29 C30 1.381(8) . ? C29 H29 0.9300 . ? C30 C31 1.394(8) . ? C30 H30 0.9300 . ? C31 C32 1.384(7) . ? C31 H31 0.9300 . ? C32 H32 0.9300 . ? C33 C38 1.381(6) . ? C33 C34 1.414(7) . ? C34 C35 1.389(7) . ? C34 H34 0.9300 . ? C35 C36 1.373(8) . ? C35 H35 0.9300 . ? C36 C37 1.377(8) . ? C36 H36 0.9300 . ? C37 C38 1.393(7) . ? C37 H37 0.9300 . ? C38 H38 0.9300 . ? C39 C40 1.384(6) . ? C39 C44 1.390(6) . ? C40 C41 1.388(7) . ? C40 H40 0.9300 . ? C41 C42 1.380(8) . ? C41 H41 0.9300 . ? C42 C43 1.396(8) . ? C42 H42 0.9300 . ? C43 C44 1.372(7) . ? C43 H43 0.9300 . ? C44 H44 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Pd N2 91.53(15) . . ? C1 Pd P 91.08(12) . . ? N2 Pd P 171.82(9) . . ? C1 Pd Cl 168.73(12) . . ? N2 Pd Cl 84.63(10) . . ? P Pd Cl 94.20(5) . . ? C5 Fe C2 68.0(2) . . ? C5 Fe C9 106.6(2) . . ? C2 Fe C9 164.19(19) . . ? C5 Fe C3 68.7(2) . . ? C2 Fe C3 41.33(19) . . ? C9 Fe C3 152.4(2) . . ? C5 Fe C10 119.06(19) . . ? C2 Fe C10 127.73(18) . . ? C9 Fe C10 40.57(18) . . ? C3 Fe C10 165.7(2) . . ? C5 Fe C8 125.5(2) . . ? C2 Fe C8 154.0(2) . . ? C9 Fe C8 41.2(2) . . ? C3 Fe C8 118.0(2) . . ? C10 Fe C8 68.7(2) . . ? C5 Fe C7 163.5(2) . . ? C2 Fe C7 120.0(2) . . ? C9 Fe C7 69.4(2) . . ? C3 Fe C7 107.0(2) . . ? C10 Fe C7 68.9(2) . . ? C8 Fe C7 41.2(2) . . ? C5 Fe C1 40.65(18) . . ? C2 Fe C1 40.87(18) . . ? C9 Fe C1 125.51(18) . . ? C3 Fe C1 69.66(18) . . ? C10 Fe C1 107.71(17) . . ? C8 Fe C1 163.2(2) . . ? C7 Fe C1 154.5(2) . . ? C5 Fe C6 154.81(19) . . ? C2 Fe C6 108.8(2) . . ? C9 Fe C6 69.3(2) . . ? C3 Fe C6 126.5(2) . . ? C10 Fe C6 41.73(17) . . ? C8 Fe C6 68.7(2) . . ? C7 Fe C6 40.2(2) . . ? C1 Fe C6 120.32(19) . . ? C5 Fe C4 40.7(2) . . ? C2 Fe C4 68.1(2) . . ? C9 Fe C4 118.2(2) . . ? C3 Fe C4 40.5(2) . . ? C10 Fe C4 152.94(19) . . ? C8 Fe C4 106.6(2) . . ? C7 Fe C4 126.0(2) . . ? C1 Fe C4 68.7(2) . . ? C6 Fe C4 163.5(2) . . ? C27 P C33 108.7(2) . . ? C27 P C39 105.0(2) . . ? C33 P C39 100.3(2) . . ? C27 P Pd 112.89(15) . . ? C33 P Pd 116.69(15) . . ? C39 P Pd 112.07(14) . . ? N2 N1 C14 111.7(3) . . ? N2 N1 C11 119.6(3) . . ? C14 N1 C11 128.6(4) . . ? N1 N2 C12 106.1(3) . . ? N1 N2 Pd 121.1(2) . . ? C12 N2 Pd 128.0(3) . . ? C5 C1 C2 105.3(4) . . ? C5 C1 Pd 124.9(3) . . ? C2 C1 Pd 129.3(3) . . ? C5 C1 Fe 67.9(3) . . ? C2 C1 Fe 68.2(3) . . ? Pd C1 Fe 121.8(2) . . ? C1 C2 C3 109.7(4) . . ? C1 C2 Fe 70.9(3) . . ? C3 C2 Fe 69.5(3) . . ? C1 C2 H2 125.2 . . ? C3 C2 H2 125.2 . . ? Fe C2 H2 126.0 . . ? C4 C3 C2 107.3(4) . . ? C4 C3 Fe 71.4(3) . . ? C2 C3 Fe 69.2(3) . . ? C4 C3 H3 126.4 . . ? C2 C3 H3 126.4 . . ? Fe C3 H3 124.7 . . ? C3 C4 C5 106.9(5) . . ? C3 C4 Fe 68.1(3) . . ? C5 C4 Fe 67.4(3) . . ? C3 C4 H4 126.6 . . ? C5 C4 H4 126.6 . . ? Fe C4 H4 129.5 . . ? C1 C5 C4 110.7(4) . . ? C1 C5 Fe 71.5(3) . . ? C4 C5 Fe 71.9(3) . . ? C1 C5 H5 124.7 . . ? C4 C5 H5 124.7 . . ? Fe C5 H5 123.5 . . ? C7 C6 C10 107.2(5) . . ? C7 C6 Fe 69.6(3) . . ? C10 C6 Fe 68.1(2) . . ? C7 C6 H6 126.4 . . ? C10 C6 H6 126.4 . . ? Fe C6 H6 127.4 . . ? C6 C7 C8 108.2(5) . . ? C6 C7 Fe 70.2(3) . . ? C8 C7 Fe 68.7(3) . . ? C6 C7 H7 125.9 . . ? C8 C7 H7 125.9 . . ? Fe C7 H7 126.8 . . ? C9 C8 C7 108.1(5) . . ? C9 C8 Fe 69.1(3) . . ? C7 C8 Fe 70.1(3) . . ? C9 C8 H8 125.9 . . ? C7 C8 H8 125.9 . . ? Fe C8 H8 126.5 . . ? C10 C9 C8 108.1(5) . . ? C10 C9 Fe 70.0(3) . . ? C8 C9 Fe 69.7(3) . . ? C10 C9 H9 126.0 . . ? C8 C9 H9 126.0 . . ? Fe C9 H9 125.8 . . ? C9 C10 C6 108.4(4) . . ? C9 C10 C11 127.5(4) . . ? C6 C10 C11 124.0(4) . . ? C9 C10 Fe 69.4(3) . . ? C6 C10 Fe 70.2(3) . . ? C11 C10 Fe 127.7(3) . . ? N1 C11 C10 111.0(3) . . ? N1 C11 H11A 109.4 . . ? C10 C11 H11A 109.4 . . ? N1 C11 H11B 109.4 . . ? C10 C11 H11B 109.4 . . ? H11A C11 H11B 108.0 . . ? N2 C12 C13 108.4(4) . . ? N2 C12 C15 123.4(3) . . ? C13 C12 C15 128.2(4) . . ? C14 C13 C12 107.2(4) . . ? C14 C13 H13 126.4 . . ? C12 C13 H13 126.4 . . ? N1 C14 C13 106.5(4) . . ? N1 C14 C21 125.6(4) . . ? C13 C14 C21 127.8(4) . . ? C16 C15 C20 119.3(4) . . ? C16 C15 C12 123.1(4) . . ? C20 C15 C12 117.6(4) . . ? C15 C16 C17 120.3(4) . . ? C15 C16 H16 119.8 . . ? C17 C16 H16 119.8 . . ? C18 C17 C16 120.1(5) . . ? C18 C17 H17 119.9 . . ? C16 C17 H17 119.9 . . ? C19 C18 C17 119.9(5) . . ? C19 C18 H18 120.0 . . ? C17 C18 H18 120.0 . . ? C18 C19 C20 121.2(5) . . ? C18 C19 H19 119.4 . . ? C20 C19 H19 119.4 . . ? C19 C20 C15 119.2(5) . . ? C19 C20 H20 120.4 . . ? C15 C20 H20 120.4 . . ? C26 C21 C22 119.8(4) . . ? C26 C21 C14 117.5(4) . . ? C22 C21 C14 122.7(4) . . ? C23 C22 C21 119.6(5) . . ? C23 C22 H22 120.2 . . ? C21 C22 H22 120.2 . . ? C24 C23 C22 120.6(5) . . ? C24 C23 H23 119.7 . . ? C22 C23 H23 119.7 . . ? C23 C24 C25 120.2(5) . . ? C23 C24 H24 119.9 . . ? C25 C24 H24 119.9 . . ? C26 C25 C24 119.2(5) . . ? C26 C25 H25 120.4 . . ? C24 C25 H25 120.4 . . ? C21 C26 C25 120.6(5) . . ? C21 C26 H26 119.7 . . ? C25 C26 H26 119.7 . . ? C28 C27 C32 119.2(4) . . ? C28 C27 P 117.5(3) . . ? C32 C27 P 123.3(4) . . ? C29 C28 C27 120.2(5) . . ? C29 C28 H28 119.9 . . ? C27 C28 H28 119.9 . . ? C30 C29 C28 120.9(5) . . ? C30 C29 H29 119.6 . . ? C28 C29 H29 119.6 . . ? C29 C30 C31 118.9(5) . . ? C29 C30 H30 120.6 . . ? C31 C30 H30 120.6 . . ? C32 C31 C30 120.4(5) . . ? C32 C31 H31 119.8 . . ? C30 C31 H31 119.8 . . ? C31 C32 C27 120.4(5) . . ? C31 C32 H32 119.8 . . ? C27 C32 H32 119.8 . . ? C38 C33 C34 117.6(4) . . ? C38 C33 P 120.7(4) . . ? C34 C33 P 121.6(3) . . ? C35 C34 C33 121.2(5) . . ? C35 C34 H34 119.4 . . ? C33 C34 H34 119.4 . . ? C36 C35 C34 119.5(5) . . ? C36 C35 H35 120.3 . . ? C34 C35 H35 120.3 . . ? C35 C36 C37 120.5(5) . . ? C35 C36 H36 119.8 . . ? C37 C36 H36 119.8 . . ? C36 C37 C38 120.2(5) . . ? C36 C37 H37 119.9 . . ? C38 C37 H37 119.9 . . ? C33 C38 C37 121.0(5) . . ? C33 C38 H38 119.5 . . ? C37 C38 H38 119.5 . . ? C40 C39 C44 119.1(4) . . ? C40 C39 P 122.4(4) . . ? C44 C39 P 118.5(3) . . ? C39 C40 C41 120.1(5) . . ? C39 C40 H40 119.9 . . ? C41 C40 H40 119.9 . . ? C42 C41 C40 120.3(5) . . ? C42 C41 H41 119.9 . . ? C40 C41 H41 119.9 . . ? C41 C42 C43 119.8(5) . . ? C41 C42 H42 120.1 . . ? C43 C42 H42 120.1 . . ? C44 C43 C42 119.5(5) . . ? C44 C43 H43 120.3 . . ? C42 C43 H43 120.3 . . ? C43 C44 C39 121.2(5) . . ? C43 C44 H44 119.4 . . ? C39 C44 H44 119.4 . . ? _diffrn_measured_fraction_theta_max 0.712 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.924 _refine_diff_density_max 1.100 _refine_diff_density_min -1.090 _refine_diff_density_rms 0.093 #==END