# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/2209 data_global # SUBMISSION DETAILS _publ_contact_author_name 'Dr Concepci\'on L\'opez' _publ_contact_author_address ; Qu\'imica Inorg\`anica Universitat de Barcelona Mart\'i i Franqu\`es 1-11 E-08028 Barcelona Spain ; _publ_contact_author_email clopez@kripto.qui.ub.es _publ_contact_letter ; Please consider this CIF as the structural information of a manuscript , which was sent by post-mail ; # TITLE AND AUTHOR LIST _publ_section_title ; A Comparative Study of the Reactivity of the \s(Pd-Csp2,ferrocene) and s(Pd-Csp2,biphenyl) Bonds in Cyclopalladated Complexes derived from ... ; loop_ _publ_author_name _publ_author_footnote _publ_author_address 'M. Benito' . ; Qu\'imica Inorg\`anica Universitat de Barcelona Mart\'i i Franqu\`es 1-11 E-08028 Barcelona Spain ; 'C. L\'opez' . ; Qu\'imica Inorg\`anica Universitat de Barcelona Mart\'i i Franqu\`es 1-11 E-08028 Barcelona Spain ; 'X. Morvan' . ; Qu\'imica Inorg\`anica Universitat de Barcelona Mart\'i i Franqu\`es 1-11 E-08028 Barcelona Spain ; 'X. Solans' . ; Departament de Cristal.lografia, Mineralogia i Dip\`osits Minerals Universitat de Barcelona Marti i Franqu\'es s/n E-08028 Barcelona Spain ; 'M. Font-Bardia' . ; Departament de Cristal.lografia, Mineralogia i Dip\`osits Minerals Universitat de Barcelona Marti i Franqu\'es s/n E-08028 Barcelona Spain ; data_chbc6 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C35 H38 Cl Fe N Pd' _chemical_formula_weight 670.36 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pd' 'Pd' -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-y+3/4, x+1/4, z+1/4' 'y+3/4, -x+3/4, z+3/4' 'x+1/2, y+1/2, z+1/2' '-x+1, -y+1/2, z+1' '-y+5/4, x+3/4, z+3/4' 'y+5/4, -x+5/4, z+5/4' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'y-3/4, -x-1/4, -z-1/4' '-y-3/4, x-3/4, -z-3/4' '-x+1/2, -y+1/2, -z+1/2' 'x, y+1/2, -z' 'y-1/4, -x+1/4, -z+1/4' '-y-1/4, x-1/4, -z-1/4' _cell_length_a 34.337(5) _cell_length_b 34.337(5) _cell_length_c 11.335(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 13364.3(36) _cell_formula_units_Z 16 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.333 _exptl_crystal_density_method ? _exptl_crystal_F_000 5504 _exptl_absorpt_coefficient_mu 1.074 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device ? _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9299 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.1210 _diffrn_reflns_limit_h_min -33 _diffrn_reflns_limit_h_max 34 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 48 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.23 _diffrn_reflns_theta_max 30.02 _reflns_number_total 9299 _reflns_number_observed 4770 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 54 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0332P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00002(2) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 9245 _refine_ls_number_parameters 458 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1134 _refine_ls_R_factor_obs 0.0365 _refine_ls_wR_factor_all 0.1397 _refine_ls_wR_factor_obs 0.0780 _refine_ls_goodness_of_fit_all 0.958 _refine_ls_goodness_of_fit_obs 1.044 _refine_ls_restrained_S_all 1.326 _refine_ls_restrained_S_obs 1.044 _refine_ls_shift/esd_max 0.067 _refine_ls_shift/esd_mean 0.004 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Pd Pd 0.004544(7) 0.587892(7) 0.08871(2) 0.03940(9) Uani 1 d . . Fe Fe -0.12041(2) 0.52891(2) -0.22696(5) 0.0614(2) Uani 1 d . . Cl Cl 0.05630(3) 0.55741(3) -0.00474(8) 0.0550(2) Uani 1 d . . N N -0.03029(7) 0.58055(8) -0.0669(2) 0.0421(6) Uani 1 d . . C1 C -0.1411(2) 0.5008(3) -0.0840(7) 0.131(3) Uani 1 d . . C2 C -0.1445(2) 0.5429(2) -0.0662(5) 0.111(2) Uani 1 d . . C3 C -0.1675(2) 0.5570(2) -0.1550(6) 0.108(2) Uani 1 d . . C4 C -0.17994(15) 0.5261(2) -0.2314(6) 0.105(2) Uani 1 d . . C5 C -0.1646(2) 0.4913(2) -0.1906(8) 0.115(2) Uani 1 d . . C6 C -0.06794(12) 0.50578(11) -0.2719(3) 0.0582(9) Uani 1 d . . C7 C -0.09221(13) 0.50928(12) -0.3754(3) 0.0687(11) Uani 1 d . . C8 C -0.10132(14) 0.54802(13) -0.3882(4) 0.0712(12) Uani 1 d . . C9 C -0.08448(12) 0.57006(11) -0.2946(3) 0.0599(10) Uani 1 d . . C10 C -0.06331(10) 0.54328(10) -0.2231(3) 0.0475(8) Uani 1 d . . C11 C -0.04324(10) 0.54932(10) -0.1123(3) 0.0439(8) Uani 1 d . . C12 C 0.03244(10) 0.59562(9) 0.2422(3) 0.0458(8) Uani 1 d . . C13 C 0.07489(13) 0.5989(2) 0.2637(4) 0.0571(10) Uani 1 d . . C14 C 0.09233(13) 0.63453(14) 0.2098(4) 0.0841(14) Uani 1 d . . H14 H 0.11974(13) 0.63521(14) 0.2263(4) 0.163(9) Uiso 1 calc R . H14A H 0.08012(13) 0.65726(14) 0.2424(4) 0.163(9) Uiso 1 calc R . H14B H 0.08834(13) 0.63404(14) 0.1260(4) 0.163(9) Uiso 1 calc R . C15 C 0.00245(10) 0.59549(9) 0.3152(3) 0.0448(8) Uani 1 d . . C16 C 0.0025(2) 0.59656(14) 0.4493(3) 0.0591(12) Uani 1 d . . C17 C 0.00762(15) 0.55902(13) 0.5094(3) 0.0775(12) Uani 1 d . . H17 H 0.00718(15) 0.56297(13) 0.5932(3) 0.163(9) Uiso 1 calc R . H17A H 0.03214(15) 0.54785(13) 0.4869(3) 0.163(9) Uiso 1 calc R . H17B H -0.01310(15) 0.54171(13) 0.4874(3) 0.163(9) Uiso 1 calc R . C18 C -0.03350(9) 0.59452(9) 0.2413(3) 0.0419(7) Uani 1 d . . C19 C -0.06026(13) 0.56042(13) 0.2557(4) 0.0591(10) Uani 1 d . . C20 C -0.0412(2) 0.52043(14) 0.2476(5) 0.0701(12) Uani 1 d . . C21 C -0.04080(10) 0.62666(10) 0.1668(3) 0.0451(8) Uani 1 d . . H21 H -0.02652(10) 0.61739(10) 0.0975(3) 0.163(9) Uiso 1 calc R . C22 C -0.02088(12) 0.66585(10) 0.1793(3) 0.0525(9) Uani 1 d . . C23 C -0.0382(2) 0.6914(2) 0.2763(5) 0.0760(14) Uani 1 d . . C24 C -0.08059(10) 0.63106(10) 0.1092(3) 0.0470(8) Uani 1 d . . C25 C -0.11269(11) 0.63011(12) 0.1840(3) 0.0574(9) Uani 1 d . . C26 C -0.14994(12) 0.63778(14) 0.1437(4) 0.0672(11) Uani 1 d . . C27 C -0.1550(2) 0.6482(2) 0.0290(5) 0.070(2) Uani 1 d . . C28 C -0.12510(12) 0.64949(12) -0.0477(4) 0.0547(9) Uani 1 d . . C29 C -0.08674(10) 0.64144(9) -0.0100(3) 0.0455(8) Uani 1 d . . C30 C -0.05560(10) 0.64618(10) -0.1005(3) 0.0474(8) Uani 1 d . . C31 C -0.05330(12) 0.68100(11) -0.1651(3) 0.0603(10) Uani 1 d . . H31 H -0.07020(12) 0.70135(11) -0.1475(3) 0.163(9) Uiso 1 calc R . C32 C -0.02611(14) 0.68548(14) -0.2550(3) 0.0667(11) Uani 1 d . . C33 C -0.00120(13) 0.65568(13) -0.2807(4) 0.0613(10) Uani 1 d . . C34 C -0.00277(10) 0.62116(12) -0.2205(3) 0.0501(8) Uani 1 d . . C35 C -0.03002(9) 0.61603(9) -0.1299(3) 0.0412(7) Uani 1 d . . H3 H -0.1826(16) 0.5866(16) -0.1388(46) 0.121(18) Uiso 1 d . . H6 H -0.0520(11) 0.4807(11) -0.2412(34) 0.068(11) Uiso 1 d . . H8 H -0.1190(12) 0.5570(12) -0.4476(41) 0.085(14) Uiso 1 d . . H9 H -0.0820(11) 0.6058(12) -0.3008(35) 0.075(12) Uiso 1 d . . H11 H -0.0429(9) 0.5273(9) -0.0570(29) 0.044(9) Uiso 1 d . . H13 H 0.0840(11) 0.5815(10) 0.2497(36) 0.042(13) Uiso 1 d . . H13A H 0.0750(14) 0.6029(14) 0.3566(51) 0.108(16) Uiso 1 d . . H16 H -0.0127(11) 0.6072(12) 0.4635(37) 0.046(14) Uiso 1 d . . H16A H 0.0276(13) 0.6119(12) 0.4711(40) 0.080(14) Uiso 1 d . . H19 H -0.0767(10) 0.5637(10) 0.2019(34) 0.046(10) Uiso 1 d . . H19A H -0.0715(13) 0.5637(14) 0.3305(47) 0.098(16) Uiso 1 d . . H20 H -0.0273(8) 0.5176(8) 0.1632(29) 0.036(8) Uiso 1 d . . H20A H -0.0543(12) 0.5003(12) 0.2613(38) 0.073(14) Uiso 1 d . . H20B H -0.0182(13) 0.5206(12) 0.2790(40) 0.072(14) Uiso 1 d . . H22 H 0.0091(10) 0.6635(8) 0.2004(28) 0.041(8) Uiso 1 d . . H22A H -0.0268(13) 0.6791(13) 0.1002(44) 0.096(15) Uiso 1 d . . H23 H -0.0693(12) 0.7000(11) 0.2640(35) 0.070(12) Uiso 1 d . . H23B H -0.0285(17) 0.6831(17) 0.3249(49) 0.099(22) Uiso 1 d . . H23A H -0.0282(16) 0.7264(18) 0.2711(51) 0.141(20) Uiso 1 d . . H25 H -0.1097(9) 0.6257(9) 0.2667(32) 0.048(9) Uiso 1 d . . H26 H -0.1735(11) 0.6360(11) 0.1888(33) 0.064(11) Uiso 1 d . . H27 H -0.1685(12) 0.6502(15) 0.0115(44) 0.051(18) Uiso 1 d . . H28 H -0.1239(12) 0.6627(12) -0.1083(38) 0.070(14) Uiso 1 d . . H32 H -0.0260(12) 0.7142(14) -0.2898(39) 0.091(14) Uiso 1 d . . H33 H 0.0154(13) 0.6586(13) -0.3381(42) 0.089(15) Uiso 1 d . . H34 H 0.0170(13) 0.5950(13) -0.2275(41) 0.090(14) Uiso 1 d . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd 0.0465(2) 0.0449(2) 0.02679(11) -0.00311(10) -0.00194(10) 0.00171(12) Fe 0.0578(3) 0.0645(3) 0.0619(3) 0.0033(3) -0.0125(3) -0.0017(3) Cl 0.0596(5) 0.0642(5) 0.0414(4) -0.0017(4) 0.0046(4) 0.0125(4) N 0.045(2) 0.047(2) 0.0346(13) -0.0084(12) -0.0046(12) 0.0055(13) C1 0.064(3) 0.191(7) 0.138(6) 0.105(6) 0.029(4) 0.018(4) C2 0.088(4) 0.164(6) 0.081(4) 0.015(4) 0.015(3) 0.011(4) C3 0.075(3) 0.133(5) 0.115(5) -0.017(4) -0.003(4) 0.016(4) C4 0.062(3) 0.119(5) 0.134(5) 0.008(4) -0.006(3) -0.005(3) C5 0.068(3) 0.098(4) 0.177(7) 0.011(4) 0.021(4) -0.011(3) C6 0.070(3) 0.048(2) 0.057(2) -0.008(2) -0.010(2) 0.000(2) C7 0.090(3) 0.062(2) 0.054(2) -0.008(2) -0.008(2) -0.007(2) C8 0.093(3) 0.073(3) 0.047(2) 0.005(2) -0.025(2) -0.016(2) C9 0.077(3) 0.058(2) 0.045(2) 0.004(2) -0.018(2) -0.007(2) C10 0.056(2) 0.046(2) 0.040(2) -0.0033(15) -0.006(2) 0.001(2) C11 0.050(2) 0.042(2) 0.040(2) -0.0012(15) -0.0057(15) 0.007(2) C12 0.058(2) 0.046(2) 0.034(2) 0.0009(14) -0.007(2) -0.003(2) C13 0.054(2) 0.069(3) 0.049(2) -0.002(2) -0.009(2) -0.009(2) C14 0.068(3) 0.100(3) 0.085(3) 0.018(3) -0.012(2) -0.031(3) C15 0.062(2) 0.042(2) 0.0304(14) -0.0050(13) -0.0023(15) 0.002(2) C16 0.081(3) 0.068(3) 0.029(2) -0.008(2) 0.004(2) 0.008(3) C17 0.118(4) 0.083(3) 0.031(2) 0.003(2) -0.004(2) 0.008(3) C18 0.047(2) 0.047(2) 0.0323(15) -0.0077(14) 0.0081(14) -0.0037(15) C19 0.061(3) 0.068(3) 0.048(2) 0.003(2) -0.002(2) -0.012(2) C20 0.081(3) 0.059(3) 0.070(3) 0.003(2) -0.006(3) -0.017(3) C21 0.052(2) 0.054(2) 0.0288(14) -0.0098(15) 0.0010(14) 0.001(2) C22 0.067(3) 0.043(2) 0.047(2) -0.004(2) -0.003(2) 0.003(2) C23 0.100(4) 0.068(3) 0.059(3) -0.025(2) -0.010(3) 0.011(3) C24 0.051(2) 0.052(2) 0.038(2) -0.0106(15) 0.0024(15) 0.003(2) C25 0.058(2) 0.073(3) 0.041(2) -0.009(2) 0.007(2) 0.005(2) C26 0.050(2) 0.087(3) 0.064(3) -0.015(2) 0.008(2) 0.004(2) C27 0.054(3) 0.088(4) 0.068(3) -0.007(2) -0.004(3) 0.016(3) C28 0.057(2) 0.058(2) 0.048(2) -0.003(2) -0.001(2) 0.009(2) C29 0.046(2) 0.047(2) 0.044(2) -0.005(2) 0.001(2) 0.008(2) C30 0.054(2) 0.054(2) 0.034(2) -0.005(2) -0.0053(15) 0.008(2) C31 0.081(3) 0.052(2) 0.048(2) -0.001(2) -0.008(2) 0.015(2) C32 0.089(3) 0.069(3) 0.042(2) 0.010(2) 0.002(2) -0.010(2) C33 0.064(3) 0.075(3) 0.045(2) -0.007(2) 0.001(2) -0.013(2) C34 0.055(2) 0.063(2) 0.032(2) -0.009(2) 0.003(2) -0.009(2) C35 0.044(2) 0.048(2) 0.0313(14) -0.0060(14) -0.0069(13) 0.0042(15) _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 C12 2.004(3) . ? Pd N 2.146(2) . ? Pd C18 2.180(3) . ? Pd C21 2.232(3) . ? Pd Cl 2.3186(9) . ? Pd C15 2.581(3) . ? Fe C1 2.015(5) . ? Fe C10 2.022(4) . ? Fe C9 2.026(4) . ? Fe C6 2.034(4) . ? Fe C5 2.035(5) . ? Fe C4 2.047(5) . ? Fe C8 2.050(4) . ? Fe C3 2.052(6) . ? Fe C7 2.055(4) . ? Fe C2 2.058(6) . ? N C11 1.270(4) . ? N C35 1.412(4) . ? C1 C2 1.465(10) . ? C1 C5 1.488(10) . ? C2 C3 1.367(8) . ? C3 C4 1.435(8) . ? C3 H3 1.16(5) . ? C4 C5 1.386(8) . ? C6 C10 1.411(5) . ? C6 C7 1.444(5) . ? C6 H6 1.08(4) . ? C7 C8 1.374(6) . ? C8 C9 1.426(5) . ? C8 H8 0.96(4) . ? C9 C10 1.425(5) . ? C9 H9 1.23(4) . ? C10 C11 1.447(4) . ? C11 H11 0.98(3) . ? C12 C15 1.321(5) . ? C12 C13 1.482(5) . ? C13 C14 1.493(6) . ? C13 H13 0.69(3) . ? C13 H13A 1.06(6) . ? C14 H14 0.96 . ? C14 H14A 0.96 . ? C14 H14B 0.96 . ? C15 C18 1.492(5) . ? C15 C16 1.520(5) . ? C16 C17 1.469(6) . ? C16 H16 0.66(4) . ? C16 H16A 1.04(5) . ? C17 H17 0.96 . ? C17 H17A 0.96 . ? C17 H17B 0.96 . ? C18 C21 1.412(5) . ? C18 C19 1.497(5) . ? C19 C20 1.524(6) . ? C19 H19 0.84(4) . ? C19 H19A 0.94(5) . ? C20 H20 1.07(3) . ? C20 H20A 0.84(4) . ? C20 H20B 0.86(4) . ? C21 C22 1.516(5) . ? C21 C24 1.522(5) . ? C21 H21 0.98 . ? C22 C23 1.527(6) . ? C22 H22 1.06(3) . ? C22 H22A 1.03(5) . ? C23 H23 1.12(4) . ? C23 H23B 0.70(5) . ? C23 H23A 1.25(6) . ? C24 C25 1.391(5) . ? C24 C29 1.414(4) . ? C25 C26 1.383(6) . ? C25 H25 0.95(3) . ? C26 C27 1.359(7) . ? C26 H26 0.96(4) . ? C27 C28 1.345(7) . ? C27 H27 0.51(4) . ? C28 C29 1.412(5) . ? C28 H28 0.82(4) . ? C29 C30 1.490(5) . ? C30 C35 1.398(4) . ? C30 C31 1.404(5) . ? C31 C32 1.391(6) . ? C31 H31 0.93 . ? C32 C33 1.365(6) . ? C32 H32 1.06(5) . ? C33 C34 1.369(6) . ? C33 H33 0.87(5) . ? C34 C35 1.400(4) . ? C34 H34 1.13(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C12 Pd N 174.67(12) . . ? C12 Pd C18 65.39(13) . . ? N Pd C18 109.30(11) . . ? C12 Pd C21 84.84(13) . . ? N Pd C21 90.42(10) . . ? C18 Pd C21 37.31(12) . . ? C12 Pd Cl 95.16(10) . . ? N Pd Cl 89.93(7) . . ? C18 Pd Cl 150.35(9) . . ? C21 Pd Cl 170.17(9) . . ? C12 Pd C15 30.28(12) . . ? N Pd C15 144.46(11) . . ? C18 Pd C15 35.26(11) . . ? C21 Pd C15 61.68(11) . . ? Cl Pd C15 121.42(8) . . ? C1 Fe C10 116.2(2) . . ? C1 Fe C9 148.5(3) . . ? C10 Fe C9 41.22(14) . . ? C1 Fe C6 109.1(2) . . ? C10 Fe C6 40.71(13) . . ? C9 Fe C6 68.8(2) . . ? C1 Fe C5 43.1(3) . . ? C10 Fe C5 150.8(2) . . ? C9 Fe C5 166.7(3) . . ? C6 Fe C5 117.6(2) . . ? C1 Fe C4 69.2(2) . . ? C10 Fe C4 168.6(2) . . ? C9 Fe C4 129.2(2) . . ? C6 Fe C4 149.3(2) . . ? C5 Fe C4 39.7(2) . . ? C1 Fe C8 169.4(3) . . ? C10 Fe C8 68.4(2) . . ? C9 Fe C8 40.96(15) . . ? C6 Fe C8 67.6(2) . . ? C5 Fe C8 128.5(3) . . ? C4 Fe C8 108.2(2) . . ? C1 Fe C3 68.1(3) . . ? C10 Fe C3 129.8(2) . . ? C9 Fe C3 107.6(2) . . ? C6 Fe C3 168.9(2) . . ? C5 Fe C3 68.3(3) . . ? C4 Fe C3 41.0(2) . . ? C8 Fe C3 117.1(3) . . ? C1 Fe C7 131.9(3) . . ? C10 Fe C7 68.96(15) . . ? C9 Fe C7 68.4(2) . . ? C6 Fe C7 41.3(2) . . ? C5 Fe C7 108.0(2) . . ? C4 Fe C7 115.8(2) . . ? C8 Fe C7 39.1(2) . . ? C3 Fe C7 148.3(2) . . ? C1 Fe C2 42.1(3) . . ? C10 Fe C2 108.3(2) . . ? C9 Fe C2 114.6(2) . . ? C6 Fe C2 132.0(2) . . ? C5 Fe C2 70.7(3) . . ? C4 Fe C2 68.4(3) . . ? C8 Fe C2 147.5(3) . . ? C3 Fe C2 38.9(2) . . ? C7 Fe C2 172.3(2) . . ? C11 N C35 121.7(3) . . ? C11 N Pd 128.9(2) . . ? C35 N Pd 108.1(2) . . ? C2 C1 C5 106.6(5) . . ? C2 C1 Fe 70.5(3) . . ? C5 C1 Fe 69.1(3) . . ? C3 C2 C1 107.1(6) . . ? C3 C2 Fe 70.3(4) . . ? C1 C2 Fe 67.4(3) . . ? C2 C3 C4 110.8(6) . . ? C2 C3 Fe 70.8(3) . . ? C4 C3 Fe 69.3(3) . . ? C2 C3 H3 117.0(28) . . ? C4 C3 H3 127.7(27) . . ? Fe C3 H3 146.2(27) . . ? C5 C4 C3 108.9(6) . . ? C5 C4 Fe 69.7(3) . . ? C3 C4 Fe 69.7(3) . . ? C4 C5 C1 106.7(6) . . ? C4 C5 Fe 70.6(3) . . ? C1 C5 Fe 67.7(3) . . ? C10 C6 C7 107.9(3) . . ? C10 C6 Fe 69.2(2) . . ? C7 C6 Fe 70.1(2) . . ? C10 C6 H6 123.0(20) . . ? C7 C6 H6 128.5(20) . . ? Fe C6 H6 132.8(20) . . ? C8 C7 C6 107.3(3) . . ? C8 C7 Fe 70.2(3) . . ? C6 C7 Fe 68.5(2) . . ? C7 C8 C9 110.0(4) . . ? C7 C8 Fe 70.7(3) . . ? C9 C8 Fe 68.6(2) . . ? C7 C8 H8 122.0(26) . . ? C9 C8 H8 127.5(27) . . ? Fe C8 H8 121.8(26) . . ? C10 C9 C8 106.7(3) . . ? C10 C9 Fe 69.2(2) . . ? C8 C9 Fe 70.4(2) . . ? C10 C9 H9 129.8(18) . . ? C8 C9 H9 121.0(19) . . ? Fe C9 H9 139.3(18) . . ? C6 C10 C9 107.9(3) . . ? C6 C10 C11 121.7(3) . . ? C9 C10 C11 130.1(3) . . ? C6 C10 Fe 70.1(2) . . ? C9 C10 Fe 69.5(2) . . ? C11 C10 Fe 121.0(2) . . ? N C11 C10 129.7(3) . . ? N C11 H11 112.8(18) . . ? C10 C11 H11 116.7(18) . . ? C15 C12 C13 131.6(3) . . ? C15 C12 Pd 99.8(2) . . ? C13 C12 Pd 128.5(3) . . ? C12 C13 C14 112.9(4) . . ? C12 C13 H13 109.9(34) . . ? C14 C13 H13 115.6(34) . . ? C12 C13 H13A 100.1(27) . . ? C14 C13 H13A 107.4(27) . . ? H13 C13 H13A 109.6(44) . . ? C13 C14 H14 109.5(2) . . ? C13 C14 H14A 109.5(3) . . ? H14 C14 H14A 109.5 . . ? C13 C14 H14B 109.5(2) . . ? H14 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C15 C18 107.1(3) . . ? C12 C15 C16 128.8(4) . . ? C18 C15 C16 124.2(4) . . ? C12 C15 Pd 49.9(2) . . ? C18 C15 Pd 57.51(15) . . ? C16 C15 Pd 175.3(3) . . ? C17 C16 C15 116.3(4) . . ? C17 C16 H16 118.1(38) . . ? C15 C16 H16 105.1(39) . . ? C17 C16 H16A 103.5(23) . . ? C15 C16 H16A 104.5(24) . . ? H16 C16 H16A 108.4(45) . . ? C16 C17 H17 109.5(2) . . ? C16 C17 H17A 109.5(3) . . ? H17 C17 H17A 109.5 . . ? C16 C17 H17B 109.5(3) . . ? H17 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C21 C18 C15 117.7(3) . . ? C21 C18 C19 124.6(3) . . ? C15 C18 C19 117.7(3) . . ? C21 C18 Pd 73.3(2) . . ? C15 C18 Pd 87.2(2) . . ? C19 C18 Pd 111.9(2) . . ? C18 C19 C20 115.7(4) . . ? C18 C19 H19 103.4(24) . . ? C20 C19 H19 111.4(24) . . ? C18 C19 H19A 104.9(30) . . ? C20 C19 H19A 109.9(30) . . ? H19 C19 H19A 111.3(37) . . ? C19 C20 H20 109.0(16) . . ? C19 C20 H20A 120.0(29) . . ? H20 C20 H20A 109.2(34) . . ? C19 C20 H20B 111.1(29) . . ? H20 C20 H20B 87.8(32) . . ? H20A C20 H20B 114.7(43) . . ? C18 C21 C22 123.9(3) . . ? C18 C21 C24 119.6(3) . . ? C22 C21 C24 110.9(3) . . ? C18 C21 Pd 69.3(2) . . ? C22 C21 Pd 104.6(2) . . ? C24 C21 Pd 121.0(2) . . ? C18 C21 H21 97.9(2) . . ? C22 C21 H21 97.9(2) . . ? C24 C21 H21 97.9(2) . . ? Pd C21 H21 30.53(8) . . ? C21 C22 C23 113.6(4) . . ? C21 C22 H22 113.1(16) . . ? C23 C22 H22 105.1(17) . . ? C21 C22 H22A 102.9(26) . . ? C23 C22 H22A 107.3(25) . . ? H22 C22 H22A 115.0(31) . . ? C22 C23 H23 115.8(21) . . ? C22 C23 H23B 98.4(48) . . ? H23 C23 H23B 131.2(55) . . ? C22 C23 H23A 114.2(27) . . ? H23 C23 H23A 90.1(31) . . ? H23B C23 H23A 107.1(55) . . ? C25 C24 C29 118.1(3) . . ? C25 C24 C21 116.6(3) . . ? C29 C24 C21 124.7(3) . . ? C26 C25 C24 121.8(4) . . ? C26 C25 H25 116.9(20) . . ? C24 C25 H25 121.2(20) . . ? C27 C26 C25 118.9(4) . . ? C27 C26 H26 114.8(23) . . ? C25 C26 H26 126.3(23) . . ? C28 C27 C26 122.0(5) . . ? C28 C27 H27 116.1(63) . . ? C26 C27 H27 121.4(63) . . ? C27 C28 C29 120.6(4) . . ? C27 C28 H28 126.6(30) . . ? C29 C28 H28 108.3(30) . . ? C28 C29 C24 118.6(3) . . ? C28 C29 C30 116.1(3) . . ? C24 C29 C30 125.3(3) . . ? C35 C30 C31 118.1(3) . . ? C35 C30 C29 122.3(3) . . ? C31 C30 C29 119.5(3) . . ? C32 C31 C30 121.0(4) . . ? C32 C31 H31 119.5(3) . . ? C30 C31 H31 119.5(2) . . ? C33 C32 C31 119.6(4) . . ? C33 C32 H32 128.0(24) . . ? C31 C32 H32 112.1(24) . . ? C32 C33 C34 121.2(4) . . ? C32 C33 H33 119.0(32) . . ? C34 C33 H33 119.8(32) . . ? C33 C34 C35 120.1(4) . . ? C33 C34 H34 129.0(23) . . ? C35 C34 H34 110.7(23) . . ? C30 C35 C34 120.1(3) . . ? C30 C35 N 120.9(3) . . ? C34 C35 N 118.9(3) . . ? _refine_diff_density_max 0.918 _refine_diff_density_min -0.599 _refine_diff_density_rms 0.090