# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 1999 # CCDC Number: 186/1678 #============================================================================ # 1. TITLE AND AUTHOR LIST data_first_block _publ_section_title ; A Comparative Study of the Synthesis, Stereochemical Characterization and reactivity of New Chiral Ruthenium(II) Complexes with (Aminoferrocenyl) phosphine Ligands. X-ray Crystal Structure of RuHCl(cod)(PTFA) and Ru(\M^3^-C~8~H~13~)Cl(PPFA), (PTFA =1-diphenylphosphino-2.3-endo-(a-dimethyl amino)-tetramethylene ferrocene and PPFA = 2-(1-dimethylaminoethyl)-1-diphenyl phosphino ferrocene) ; # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. loop_ _publ_author_name _publ_author_address 'Jalon, F.A.' ; Departamento de Qumica Inorgnica Facultad de Ciencias Qumicas Universidad de Castilla-La Mancha Campus Universitario 13071, Ciudad Real Spain ; 'Lopez-Agenjo, A.' ; Departamento de Qumica Inorgnica Facultad de Ciencias Qumicas Universidad de Castilla-La Mancha Campus Universitario 13071, Ciudad Real Spain ; 'Manzano, B.R.' ; Departamento de Qumica Inorgnica Facultad de Ciencias Qumicas Universidad de Castilla-La Mancha Campus Universitario 13071, Ciudad Real Spain ; 'Moreno-Lara, M.' ; Departamento de Qumica Inorgnica Facultad de Ciencias Qumicas Universidad de Castilla-La Mancha Campus Universitario 13071, Ciudad Real Spain ; 'Rodriguez, A.M.' ; Departamento de Qumica Inorgnica Facultad de Ciencias Qumicas Universidad de Castilla-La Mancha Campus Universitario 13071, Ciudad Real Spain ; 'Sturm, T' ; Institut fr Organische Chemie Universitt Wien Whringer Strabe 38 A-1090 Wien Austria ; 'Weissensteiner, W' ; Institut fr Organische Chemie Universitt Wien Whringer Strabe 38 A-1090 Wien Austria ; #============================================================================ # 2. PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ? _journal_techeditor_code ? _journal_techeditor_notes ? _journal_coden_ASTM ? _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #============================================================================ data_1 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C36 H43 Cl Fe N P Ru' _chemical_formula_weight 713.05 _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' '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' 'Ru' 'Ru' -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.2600(10) _cell_length_b 22.998(8) _cell_length_c 12.0024(9) _cell_angle_alpha 90.00 _cell_angle_beta 91.369(7) _cell_angle_gamma 90.00 _cell_volume 3107.2(11) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 8 _cell_measurement_theta_max 20 _exptl_crystal_description prismatic _exptl_crystal_colour ? _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.524 _exptl_crystal_density_method ? _exptl_crystal_F_000 1472 _exptl_absorpt_coefficient_mu 1.117 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.998 _exptl_absorpt_correction_T_max 1.000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'four circle diffracctometer Nonius_Mach3' _diffrn_measurement_method '\w/2\2q scans' _diffrn_standards_number 2 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 90 _diffrn_standards_decay_% ? _diffrn_reflns_number 14767 _diffrn_reflns_av_R_equivalents 0.0196 _diffrn_reflns_av_sigmaI/netI 0.0310 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.01 _diffrn_reflns_theta_max 27.99 _reflns_number_total 7474 _reflns_number_observed 5747 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Nonius (control program)' _computing_cell_refinement 'Nonius (control program)' _computing_data_reduction 'XRAY80 (Stewart, 1976)' _computing_structure_solution 'SIR92 (Altomare, 1994)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0351P)^2^+2.2406P] 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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7474 _refine_ls_number_parameters 374 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0425 _refine_ls_R_factor_obs 0.0260 _refine_ls_wR_factor_all 0.0807 _refine_ls_wR_factor_obs 0.0608 _refine_ls_goodness_of_fit_all 1.011 _refine_ls_goodness_of_fit_obs 0.874 _refine_ls_restrained_S_all 1.011 _refine_ls_restrained_S_obs 0.874 _refine_ls_shift/esd_max -0.044 _refine_ls_shift/esd_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Ru1 Ru 0.25738(2) 0.182490(8) 0.84737(2) 0.02609(6) Uani 1 d . . H1 H 0.2399(22) 0.1330(11) 0.9287(21) 0.027(7) Uiso 1 d . . Fe2 Fe 0.57032(3) 0.03838(2) 0.72097(3) 0.03182(9) Uani 1 d . . Cl3 Cl 0.33470(6) 0.25570(3) 0.70971(7) 0.0442(2) Uani 1 d . . P4 P 0.28496(6) 0.10630(3) 0.72504(5) 0.02562(13) Uani 1 d . . N5 N 0.4584(2) 0.17559(9) 0.9075(2) 0.0289(4) Uani 1 d . . C6 C 0.4861(3) 0.22828(14) 0.9762(3) 0.0445(7) Uani 1 d . . H6A H 0.4782 0.2624 0.9306 0.067 Uiso 1 calc . . H6B H 0.5659 0.2257 1.0056 0.067 Uiso 1 calc . . H6C H 0.4319 0.2306 1.0366 0.067 Uiso 1 calc . . C7 C 0.4718(3) 0.12428(13) 0.9807(2) 0.0386(6) Uani 1 d . . H7A H 0.4545 0.0897 0.9386 0.058 Uiso 1 calc . . H7B H 0.4177 0.1273 1.0411 0.058 Uiso 1 calc . . H7C H 0.5518 0.1225 1.0100 0.058 Uiso 1 calc . . C8 C 0.5488(2) 0.17476(11) 0.8162(2) 0.0293(5) Uani 1 d . . H8 H 0.5358 0.2112 0.7753 0.035 Uiso 1 calc . . C9 C 0.6801(2) 0.17732(14) 0.8566(2) 0.0414(6) Uani 1 d . . H9A H 0.6903 0.2077 0.9120 0.050 Uiso 1 calc . . H9B H 0.7028 0.1406 0.8906 0.050 Uiso 1 calc . . C10 C 0.7585(3) 0.18970(14) 0.7571(3) 0.0465(7) Uani 1 d . . H10A H 0.7289 0.2238 0.7180 0.056 Uiso 1 calc . . H10B H 0.8388 0.1979 0.7837 0.056 Uiso 1 calc . . C11 C 0.7603(2) 0.1387(2) 0.6775(3) 0.0463(7) Uani 1 d . . H11A H 0.7915 0.1512 0.6067 0.056 Uiso 1 calc . . H11B H 0.8121 0.1086 0.7077 0.056 Uiso 1 calc . . C12 C 0.6375(2) 0.11479(12) 0.6597(2) 0.0338(6) Uani 1 d . . C13 C 0.5379(2) 0.12764(11) 0.7286(2) 0.0285(5) Uani 1 d . . C14 C 0.4367(2) 0.09741(10) 0.6824(2) 0.0266(5) Uani 1 d . . C15 C 0.4753(2) 0.06662(12) 0.5856(2) 0.0330(5) Uani 1 d . . H15 H 0.4281 0.0431 0.5397 0.040 Uiso 1 calc . . C16 C 0.5971(3) 0.07825(13) 0.5722(2) 0.0379(6) Uani 1 d . . H16 H 0.6433 0.0641 0.5150 0.045 Uiso 1 calc . . C17 C 0.6192(3) 0.00513(15) 0.8735(2) 0.0509(8) Uani 1 d . . H17 H 0.6246 0.0260 0.9398 0.061 Uiso 1 calc . . C18 C 0.5178(3) -0.02363(15) 0.8309(3) 0.0538(8) Uani 1 d . . H18 H 0.4440 -0.0251 0.8639 0.065 Uiso 1 calc . . C19 C 0.5478(4) -0.04979(14) 0.7298(3) 0.0602(10) Uani 1 d . . H19 H 0.4975 -0.0722 0.6847 0.072 Uiso 1 calc . . C20 C 0.6671(4) -0.0363(2) 0.7083(3) 0.0594(10) Uani 1 d . . H20 H 0.7090 -0.0474 0.6459 0.071 Uiso 1 calc . . C21 C 0.7112(3) -0.0032(2) 0.7977(3) 0.0549(9) Uani 1 d . . H21 H 0.7883 0.0109 0.8059 0.066 Uiso 1 calc . . C22 C 0.2377(2) 0.03241(11) 0.7671(2) 0.0321(5) Uani 1 d . . C23 C 0.1945(3) 0.02058(13) 0.8720(2) 0.0443(7) Uani 1 d . . H23 H 0.1861 0.0507 0.9230 0.053 Uiso 1 calc . . C24 C 0.1637(4) -0.03599(15) 0.9017(3) 0.0593(9) Uani 1 d . . H24 H 0.1347 -0.0432 0.9723 0.071 Uiso 1 calc . . C25 C 0.1756(3) -0.08077(14) 0.8284(3) 0.0568(9) Uani 1 d . . H25 H 0.1561 -0.1185 0.8488 0.068 Uiso 1 calc . . C26 C 0.2169(3) -0.06920(12) 0.7236(3) 0.0501(8) Uani 1 d . . H26 H 0.2252 -0.0994 0.6729 0.060 Uiso 1 calc . . C27 C 0.2459(3) -0.01359(12) 0.6932(3) 0.0429(7) Uani 1 d . . H27 H 0.2716 -0.0066 0.6214 0.052 Uiso 1 calc . . C28 C 0.2069(2) 0.11287(11) 0.5894(2) 0.0329(5) Uani 1 d . . C29 C 0.0984(3) 0.0869(2) 0.5677(3) 0.0508(8) Uani 1 d . . H29 H 0.0643 0.0637 0.6218 0.061 Uiso 1 calc . . C30 C 0.0397(3) 0.0949(2) 0.4661(3) 0.0646(10) Uani 1 d . . H30 H -0.0327 0.0765 0.4522 0.078 Uiso 1 calc . . C31 C 0.0868(4) 0.1298(2) 0.3858(3) 0.0656(11) Uani 1 d . . H31 H 0.0470 0.1349 0.3178 0.079 Uiso 1 calc . . C32 C 0.1926(4) 0.1568(2) 0.4066(3) 0.0575(9) Uani 1 d . . H32 H 0.2247 0.1807 0.3525 0.069 Uiso 1 calc . . C33 C 0.2535(3) 0.14910(13) 0.5085(2) 0.0419(7) Uani 1 d . . H33 H 0.3252 0.1682 0.5222 0.050 Uiso 1 calc . . C34 C 0.2113(3) 0.26071(13) 0.9506(3) 0.0458(7) Uani 1 d . . H34 H 0.2786 0.2864 0.9686 0.055 Uiso 1 calc . . C35 C 0.1003(3) 0.29178(15) 0.9083(3) 0.0607(10) Uani 1 d . . H35A H 0.0373 0.2860 0.9609 0.073 Uiso 1 calc . . H35B H 0.1162 0.3332 0.9043 0.073 Uiso 1 calc . . C36 C 0.0592(3) 0.27038(14) 0.7948(3) 0.0505(8) Uani 1 d . . H36A H -0.0263 0.2751 0.7881 0.061 Uiso 1 calc . . H36B H 0.0947 0.2946 0.7384 0.061 Uiso 1 calc . . C37 C 0.0892(2) 0.20807(13) 0.7715(2) 0.0369(6) Uani 1 d . . H37 H 0.0814 0.1976 0.6925 0.044 Uiso 1 calc . . C38 C 0.0695(2) 0.16107(12) 0.8441(2) 0.0363(6) Uani 1 d . . H38 H 0.0508 0.1245 0.8055 0.044 Uiso 1 calc . . C39 C 0.0093(3) 0.1673(2) 0.9556(3) 0.0529(8) Uani 1 d . . H39A H -0.0510 0.1973 0.9489 0.063 Uiso 1 calc . . H39B H -0.0306 0.1311 0.9723 0.063 Uiso 1 calc . . C40 C 0.0918(3) 0.1823(2) 1.0518(3) 0.0608(10) Uani 1 d . . H40A H 0.1117 0.1470 1.0924 0.073 Uiso 1 calc . . H40B H 0.0508 0.2080 1.1022 0.073 Uiso 1 calc . . C41 C 0.2057(3) 0.21144(15) 1.0160(2) 0.0461(7) Uani 1 d . . H41 H 0.2704 0.2087 1.0718 0.055 Uiso 1 calc . . 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 Ru1 0.02537(10) 0.02587(10) 0.02712(10) -0.00267(8) 0.00205(7) -0.00250(8) Fe2 0.0347(2) 0.0338(2) 0.0269(2) 0.00225(15) -0.00114(15) 0.0088(2) Cl3 0.0370(4) 0.0410(4) 0.0548(4) 0.0167(3) 0.0054(3) 0.0001(3) P4 0.0262(3) 0.0266(3) 0.0240(3) -0.0012(2) -0.0015(2) -0.0010(2) N5 0.0296(11) 0.0315(11) 0.0255(10) -0.0007(8) -0.0020(8) -0.0029(8) C6 0.039(2) 0.047(2) 0.048(2) -0.0192(14) -0.0014(13) -0.0090(13) C7 0.041(2) 0.046(2) 0.0286(13) 0.0084(12) -0.0010(11) 0.0013(12) C8 0.0272(12) 0.0315(13) 0.0291(12) 0.0028(10) -0.0020(10) -0.0033(10) C9 0.0289(13) 0.054(2) 0.040(2) 0.0006(13) -0.0058(11) -0.0051(12) C10 0.0274(14) 0.058(2) 0.054(2) 0.008(2) -0.0022(12) -0.0077(13) C11 0.0276(14) 0.063(2) 0.049(2) 0.0095(15) 0.0062(12) -0.0006(13) C12 0.0312(13) 0.0390(14) 0.0313(13) 0.0059(11) 0.0047(10) 0.0036(11) C13 0.0274(12) 0.0347(13) 0.0234(11) 0.0049(10) 0.0010(9) 0.0014(10) C14 0.0284(12) 0.0288(12) 0.0223(11) 0.0022(9) -0.0017(9) 0.0052(9) C15 0.0370(14) 0.0387(14) 0.0233(12) -0.0004(10) -0.0021(10) 0.0065(11) C16 0.043(2) 0.044(2) 0.0268(13) 0.0013(11) 0.0077(11) 0.0076(12) C17 0.068(2) 0.054(2) 0.0306(15) 0.0067(13) -0.0105(14) 0.020(2) C18 0.061(2) 0.047(2) 0.053(2) 0.026(2) 0.000(2) 0.008(2) C19 0.082(3) 0.036(2) 0.061(2) 0.005(2) -0.024(2) 0.009(2) C20 0.074(2) 0.052(2) 0.052(2) -0.002(2) -0.006(2) 0.036(2) C21 0.047(2) 0.060(2) 0.058(2) 0.009(2) -0.013(2) 0.019(2) C22 0.0319(13) 0.0284(12) 0.0357(14) -0.0024(10) -0.0032(11) -0.0035(10) C23 0.058(2) 0.040(2) 0.0351(15) -0.0016(12) -0.0001(13) -0.0137(14) C24 0.082(3) 0.048(2) 0.047(2) 0.006(2) 0.005(2) -0.023(2) C25 0.067(2) 0.035(2) 0.067(2) 0.005(2) -0.007(2) -0.017(2) C26 0.057(2) 0.0263(14) 0.067(2) -0.0134(14) -0.002(2) -0.0060(13) C27 0.053(2) 0.0316(14) 0.045(2) -0.0101(12) 0.0064(14) -0.0048(12) C28 0.0353(14) 0.0323(13) 0.0307(13) -0.0059(10) -0.0072(10) 0.0080(10) C29 0.039(2) 0.068(2) 0.044(2) -0.005(2) -0.0124(14) -0.0033(15) C30 0.054(2) 0.076(3) 0.063(2) -0.012(2) -0.032(2) 0.005(2) C31 0.073(3) 0.078(3) 0.045(2) -0.008(2) -0.030(2) 0.028(2) C32 0.079(3) 0.059(2) 0.035(2) 0.0055(15) -0.009(2) 0.030(2) C33 0.051(2) 0.040(2) 0.0348(15) 0.0058(12) -0.0043(13) 0.0108(13) C34 0.043(2) 0.040(2) 0.054(2) -0.0231(14) -0.0009(14) 0.0022(13) C35 0.059(2) 0.043(2) 0.080(3) -0.020(2) 0.001(2) 0.011(2) C36 0.042(2) 0.043(2) 0.066(2) -0.003(2) -0.003(2) 0.0134(13) C37 0.0265(13) 0.0436(15) 0.0405(15) -0.0043(12) -0.0030(11) 0.0042(11) C38 0.0234(12) 0.0422(14) 0.043(2) -0.0059(12) 0.0009(11) -0.0041(11) C39 0.038(2) 0.067(2) 0.054(2) 0.001(2) 0.0150(15) -0.0106(15) C40 0.050(2) 0.088(3) 0.045(2) -0.011(2) 0.019(2) -0.010(2) C41 0.043(2) 0.060(2) 0.036(2) -0.0203(14) 0.0063(13) -0.0035(14) _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 Ru1 C37 2.163(3) . ? Ru1 C38 2.171(3) . ? Ru1 C41 2.221(3) . ? Ru1 C34 2.252(3) . ? Ru1 P4 2.3118(8) . ? Ru1 N5 2.365(2) . ? Ru1 Cl3 2.5281(8) . ? Fe2 C15 2.031(3) . ? Fe2 C16 2.036(3) . ? Fe2 C20 2.042(3) . ? Fe2 C18 2.040(3) . ? Fe2 C17 2.047(3) . ? Fe2 C19 2.047(3) . ? Fe2 C21 2.052(3) . ? Fe2 C12 2.056(3) . ? Fe2 C14 2.071(2) . ? Fe2 C13 2.087(3) . ? P4 C14 1.806(2) . ? P4 C28 1.838(3) . ? P4 C22 1.854(3) . ? N5 C7 1.477(3) . ? N5 C6 1.494(3) . ? N5 C8 1.515(3) . ? C8 C13 1.513(3) . ? C8 C9 1.545(4) . ? C9 C10 1.528(4) . ? C10 C11 1.513(5) . ? C11 C12 1.499(4) . ? C12 C16 1.411(4) . ? C12 C13 1.440(3) . ? C13 C14 1.436(3) . ? C14 C15 1.437(3) . ? C15 C16 1.410(4) . ? C17 C18 1.405(5) . ? C17 C21 1.407(5) . ? C18 C19 1.403(5) . ? C19 C20 1.409(6) . ? C20 C21 1.397(5) . ? C22 C27 1.385(4) . ? C22 C23 1.388(4) . ? C23 C24 1.395(4) . ? C24 C25 1.364(5) . ? C25 C26 1.377(5) . ? C26 C27 1.371(4) . ? C28 C29 1.380(4) . ? C28 C33 1.391(4) . ? C29 C30 1.385(4) . ? C30 C31 1.369(6) . ? C31 C32 1.361(6) . ? C32 C33 1.399(4) . ? C34 C41 1.380(5) . ? C34 C35 1.517(5) . ? C35 C36 1.511(5) . ? C36 C37 1.500(4) . ? C37 C38 1.409(4) . ? C38 C39 1.522(4) . ? C39 C40 1.504(5) . ? C40 C41 1.519(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 C37 Ru1 C38 37.93(11) . . ? C37 Ru1 C41 93.21(11) . . ? C38 Ru1 C41 78.95(11) . . ? C37 Ru1 C34 78.67(11) . . ? C38 Ru1 C34 87.38(11) . . ? C41 Ru1 C34 35.94(12) . . ? C37 Ru1 P4 93.93(8) . . ? C38 Ru1 P4 87.83(8) . . ? C41 Ru1 P4 147.99(9) . . ? C34 Ru1 P4 172.38(9) . . ? C37 Ru1 N5 165.65(9) . . ? C38 Ru1 N5 156.25(9) . . ? C41 Ru1 N5 90.66(10) . . ? C34 Ru1 N5 96.70(9) . . ? P4 Ru1 N5 90.06(5) . . ? C37 Ru1 Cl3 81.70(8) . . ? C38 Ru1 Cl3 119.32(8) . . ? C41 Ru1 Cl3 119.84(9) . . ? C34 Ru1 Cl3 85.13(9) . . ? P4 Ru1 Cl3 92.07(3) . . ? N5 Ru1 Cl3 84.39(5) . . ? C15 Fe2 C16 40.58(11) . . ? C15 Fe2 C20 118.79(13) . . ? C16 Fe2 C20 102.89(13) . . ? C15 Fe2 C18 125.86(13) . . ? C16 Fe2 C18 158.96(14) . . ? C20 Fe2 C18 67.9(2) . . ? C15 Fe2 C17 163.80(13) . . ? C16 Fe2 C17 155.52(14) . . ? C20 Fe2 C17 67.64(13) . . ? C18 Fe2 C17 40.21(14) . . ? C15 Fe2 C19 107.15(13) . . ? C16 Fe2 C19 120.85(14) . . ? C20 Fe2 C19 40.3(2) . . ? C18 Fe2 C19 40.15(15) . . ? C17 Fe2 C19 67.33(14) . . ? C15 Fe2 C21 153.55(13) . . ? C16 Fe2 C21 118.34(13) . . ? C20 Fe2 C21 39.90(14) . . ? C18 Fe2 C21 67.45(15) . . ? C17 Fe2 C21 40.16(14) . . ? C19 Fe2 C21 67.06(15) . . ? C15 Fe2 C12 68.38(11) . . ? C16 Fe2 C12 40.35(11) . . ? C20 Fe2 C12 119.38(14) . . ? C18 Fe2 C12 160.67(14) . . ? C17 Fe2 C12 123.08(13) . . ? C19 Fe2 C12 155.84(14) . . ? C21 Fe2 C12 105.79(13) . . ? C15 Fe2 C14 40.99(9) . . ? C16 Fe2 C14 68.33(10) . . ? C20 Fe2 C14 157.09(13) . . ? C18 Fe2 C14 112.49(12) . . ? C17 Fe2 C14 128.56(11) . . ? C19 Fe2 C14 124.80(13) . . ? C21 Fe2 C14 162.92(13) . . ? C12 Fe2 C14 68.37(10) . . ? C15 Fe2 C13 68.35(10) . . ? C16 Fe2 C13 67.99(10) . . ? C20 Fe2 C13 157.62(14) . . ? C18 Fe2 C13 127.26(13) . . ? C17 Fe2 C13 111.83(12) . . ? C19 Fe2 C13 161.82(14) . . ? C21 Fe2 C13 124.96(13) . . ? C12 Fe2 C13 40.66(10) . . ? C14 Fe2 C13 40.39(9) . . ? C14 P4 C28 101.14(12) . . ? C14 P4 C22 104.66(11) . . ? C28 P4 C22 100.49(12) . . ? C14 P4 Ru1 114.09(8) . . ? C28 P4 Ru1 115.58(8) . . ? C22 P4 Ru1 118.56(9) . . ? C7 N5 C6 107.6(2) . . ? C7 N5 C8 111.1(2) . . ? C6 N5 C8 105.9(2) . . ? C7 N5 Ru1 108.6(2) . . ? C6 N5 Ru1 107.4(2) . . ? C8 N5 Ru1 115.80(14) . . ? C13 C8 N5 117.9(2) . . ? C13 C8 C9 107.9(2) . . ? N5 C8 C9 115.3(2) . . ? C10 C9 C8 109.1(2) . . ? C11 C10 C9 111.5(3) . . ? C12 C11 C10 110.4(2) . . ? C16 C12 C13 107.9(2) . . ? C16 C12 C11 127.2(2) . . ? C13 C12 C11 124.8(3) . . ? C16 C12 Fe2 69.1(2) . . ? C13 C12 Fe2 70.83(15) . . ? C11 C12 Fe2 127.5(2) . . ? C14 C13 C12 107.5(2) . . ? C14 C13 C8 131.8(2) . . ? C12 C13 C8 119.6(2) . . ? C14 C13 Fe2 69.20(14) . . ? C12 C13 Fe2 68.52(15) . . ? C8 C13 Fe2 136.3(2) . . ? C15 C14 C13 107.3(2) . . ? C15 C14 P4 126.3(2) . . ? C13 C14 P4 125.7(2) . . ? C15 C14 Fe2 68.00(14) . . ? C13 C14 Fe2 70.42(14) . . ? P4 C14 Fe2 134.25(13) . . ? C16 C15 C14 108.2(2) . . ? C16 C15 Fe2 69.9(2) . . ? C14 C15 Fe2 71.01(14) . . ? C15 C16 C12 109.0(2) . . ? C15 C16 Fe2 69.51(15) . . ? C12 C16 Fe2 70.6(2) . . ? C18 C17 C21 107.8(3) . . ? C18 C17 Fe2 69.6(2) . . ? C21 C17 Fe2 70.1(2) . . ? C17 C18 C19 107.8(3) . . ? C17 C18 Fe2 70.2(2) . . ? C19 C18 Fe2 70.2(2) . . ? C18 C19 C20 108.3(3) . . ? C18 C19 Fe2 69.7(2) . . ? C20 C19 Fe2 69.7(2) . . ? C21 C20 C19 107.6(3) . . ? C21 C20 Fe2 70.5(2) . . ? C19 C20 Fe2 70.0(2) . . ? C20 C21 C17 108.5(3) . . ? C20 C21 Fe2 69.6(2) . . ? C17 C21 Fe2 69.7(2) . . ? C27 C22 C23 117.5(3) . . ? C27 C22 P4 120.1(2) . . ? C23 C22 P4 122.4(2) . . ? C22 C23 C24 120.6(3) . . ? C25 C24 C23 120.7(3) . . ? C24 C25 C26 119.0(3) . . ? C27 C26 C25 120.7(3) . . ? C26 C27 C22 121.5(3) . . ? C29 C28 C33 118.3(3) . . ? C29 C28 P4 122.3(2) . . ? C33 C28 P4 119.2(2) . . ? C28 C29 C30 120.7(3) . . ? C31 C30 C29 120.8(3) . . ? C32 C31 C30 119.4(3) . . ? C31 C32 C33 120.7(3) . . ? C28 C33 C32 120.0(3) . . ? C41 C34 C35 121.9(3) . . ? C41 C34 Ru1 70.8(2) . . ? C35 C34 Ru1 113.0(2) . . ? C36 C35 C34 112.4(3) . . ? C37 C36 C35 114.4(3) . . ? C38 C37 C36 125.4(3) . . ? C38 C37 Ru1 71.4(2) . . ? C36 C37 Ru1 112.4(2) . . ? C37 C38 C39 123.5(3) . . ? C37 C38 Ru1 70.71(15) . . ? C39 C38 Ru1 114.6(2) . . ? C40 C39 C38 114.7(3) . . ? C39 C40 C41 113.2(3) . . ? C34 C41 C40 125.0(3) . . ? C34 C41 Ru1 73.2(2) . . ? C40 C41 Ru1 111.6(2) . . ? _refine_diff_density_max 0.441 _refine_diff_density_min -0.420 _refine_diff_density_rms 0.075 #======END data_4 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C34 H41 Cl Fe N P Ru' _chemical_formula_weight 687.02 _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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' 0.3463 0.8444 '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' 'Ru' 'Ru' -1.2594 0.8363 '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, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.477(5) _cell_length_b 16.1020(10) _cell_length_c 20.281(3) _cell_angle_alpha 90.00 _cell_angle_beta 103.57(2) _cell_angle_gamma 90.00 _cell_volume 3008.5(17) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 8 _cell_measurement_theta_max 20 _exptl_crystal_description prismatic _exptl_crystal_colour ? _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.517 _exptl_crystal_density_method ? _exptl_crystal_F_000 1416 _exptl_absorpt_coefficient_mu 1.151 _exptl_absorpt_correction_type 'psi scan ' _exptl_absorpt_correction_T_min 0.830 _exptl_absorpt_correction_T_max 1.000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'fine focus sealed tube' _diffrn_measurement_method '\w/2\2q scans' _diffrn_standards_number 2 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 90 _diffrn_standards_decay_% ? _diffrn_reflns_number 7239 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0363 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.07 _diffrn_reflns_theta_max 27.98 _reflns_number_total 7239 _reflns_number_observed 5421 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Nonius (control program)' _computing_cell_refinement 'Nonius (control program)' _computing_data_reduction 'XRAY80 (Stewart, 1976)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0612P)^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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7239 _refine_ls_number_parameters 404 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0432 _refine_ls_R_factor_obs 0.0248 _refine_ls_wR_factor_all 0.0835 _refine_ls_wR_factor_obs 0.0615 _refine_ls_goodness_of_fit_all 0.800 _refine_ls_goodness_of_fit_obs 0.687 _refine_ls_restrained_S_all 0.800 _refine_ls_restrained_S_obs 0.687 _refine_ls_shift/esd_max 0.028 _refine_ls_shift/esd_mean 0.002 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Ru1 Ru 0.76637(2) 0.196409(12) 0.864130(10) 0.03236(6) Uani 1 d . . Fe2 Fe 0.43350(3) 0.41589(2) 0.87774(2) 0.03282(9) Uani 1 d . . Cl3 Cl 0.52546(8) 0.15686(5) 0.79575(4) 0.0527(2) Uani 1 d . . P4 P 0.71588(6) 0.27356(4) 0.94308(3) 0.02827(12) Uani 1 d . . N5 N 0.7615(2) 0.30552(13) 0.79086(10) 0.0361(4) Uani 1 d . . C1 C 0.9961(3) 0.1787(2) 0.8956(2) 0.0431(6) Uani 1 d . . C2 C 0.9232(3) 0.1347(2) 0.93797(14) 0.0442(6) Uani 1 d . . C3 C 0.8090(3) 0.0772(2) 0.9127(2) 0.0459(6) Uani 1 d . . C4 C 0.8124(4) 0.0128(2) 0.8585(2) 0.0530(8) Uani 1 d . . C5 C 0.9464(4) -0.0447(2) 0.8732(2) 0.0660(10) Uani 1 d . . C6 C 1.0932(4) -0.0027(2) 0.8933(2) 0.0597(8) Uani 1 d . . C7 C 1.1301(4) 0.0616(2) 0.8460(2) 0.0661(9) Uani 1 d . . C8 C 1.0335(4) 0.1412(2) 0.8340(2) 0.0528(7) Uani 1 d . . C9 C 0.6236(2) 0.3559(2) 0.77966(12) 0.0345(5) Uani 1 d . . H9 H 0.5427 0.3164 0.7717 0.041 Uiso 1 calc . . C11 C 0.5871(2) 0.2331(2) 0.99081(13) 0.0367(5) Uani 1 d . . C12 C 0.5621(3) 0.2749(2) 1.04739(14) 0.0438(6) Uani 1 d . . H12 H 0.6173 0.3214 1.0638 0.053 Uiso 1 calc . . C13 C 0.4565(3) 0.2479(2) 1.0793(2) 0.0587(8) Uani 1 d . . H13 H 0.4392 0.2769 1.1162 0.070 Uiso 1 calc . . C14 C 0.3773(4) 0.1782(3) 1.0560(2) 0.0752(12) Uani 1 d . . H14 H 0.3053 0.1604 1.0770 0.090 Uiso 1 calc . . C15 C 0.4034(4) 0.1347(3) 1.0023(2) 0.0754(11) Uani 1 d . . H15 H 0.3513 0.0865 0.9879 0.091 Uiso 1 calc . . C16 C 0.5076(3) 0.1623(2) 0.9690(2) 0.0553(8) Uani 1 d . . H16 H 0.5237 0.1329 0.9320 0.066 Uiso 1 calc . . C21 C 0.8683(2) 0.30582(14) 1.01333(12) 0.0307(5) Uani 1 d . . C22 C 0.9075(3) 0.2608(2) 1.07321(13) 0.0378(5) Uani 1 d . . H22 H 0.8529 0.2147 1.0793 0.045 Uiso 1 calc . . C23 C 1.0264(3) 0.2832(2) 1.12399(14) 0.0489(7) Uani 1 d . . H23 H 1.0510 0.2521 1.1637 0.059 Uiso 1 calc . . C24 C 1.1085(3) 0.3516(2) 1.1159(2) 0.0522(7) Uani 1 d . . H24 H 1.1877 0.3671 1.1502 0.063 Uiso 1 calc . . C25 C 1.0721(3) 0.3966(2) 1.0567(2) 0.0543(8) Uani 1 d . . H25 H 1.1276 0.4425 1.0508 0.065 Uiso 1 calc . . C26 C 0.9539(3) 0.3741(2) 1.00589(14) 0.0429(6) Uani 1 d . . H26 H 0.9309 0.4050 0.9661 0.052 Uiso 1 calc . . C31 C 0.6411(2) 0.37374(14) 0.91142(11) 0.0293(5) Uani 1 d . . C32 C 0.6131(2) 0.4411(2) 0.95266(13) 0.0349(5) Uani 1 d . . H32 H 0.6190 0.4388 0.9990 0.042 Uiso 1 calc . . C33 C 0.5750(3) 0.5118(2) 0.91093(14) 0.0399(6) Uani 1 d . . H33 H 0.5519 0.5638 0.9252 0.048 Uiso 1 calc . . C34 C 0.5778(3) 0.4899(2) 0.84405(13) 0.0363(5) Uani 1 d . . H34 H 0.5570 0.5253 0.8068 0.044 Uiso 1 calc . . C35 C 0.6181(2) 0.40409(15) 0.84272(12) 0.0314(5) Uani 1 d . . C41 C 0.2971(3) 0.3171(2) 0.8575(2) 0.0661(10) Uani 1 d . . H41 H 0.3258 0.2620 0.8570 0.079 Uiso 1 calc . . C42 C 0.2732(3) 0.3603(3) 0.9139(2) 0.0638(10) Uani 1 d . . H42 H 0.2833 0.3390 0.9573 0.077 Uiso 1 calc . . C43 C 0.2317(3) 0.4410(2) 0.8931(2) 0.0586(9) Uani 1 d . . H43 H 0.2092 0.4831 0.9203 0.070 Uiso 1 calc . . C44 C 0.2297(3) 0.4474(2) 0.8244(2) 0.0583(8) Uani 1 d . . H44 H 0.2054 0.4945 0.7976 0.070 Uiso 1 calc . . C45 C 0.2705(3) 0.3708(3) 0.8028(2) 0.0629(10) Uani 1 d . . H45 H 0.2784 0.3579 0.7591 0.075 Uiso 1 calc . . C50 C 0.5975(3) 0.4142(2) 0.71816(14) 0.0518(7) Uani 1 d . . H50A H 0.6007 0.3829 0.6782 0.078 Uiso 1 calc . . H50B H 0.6714 0.4562 0.7255 0.078 Uiso 1 calc . . H50C H 0.5040 0.4400 0.7123 0.078 Uiso 1 calc . . C51 C 0.8906(3) 0.3599(2) 0.80985(15) 0.0478(7) Uani 1 d . . H51A H 0.8899 0.3882 0.8514 0.072 Uiso 1 calc . . H51B H 0.8887 0.3999 0.7746 0.072 Uiso 1 calc . . H51C H 0.9770 0.3268 0.8159 0.072 Uiso 1 calc . . C52 C 0.7669(4) 0.2626(2) 0.72652(15) 0.0568(8) Uani 1 d . . H52A H 0.6839 0.2270 0.7130 0.085 Uiso 1 calc . . H52B H 0.8539 0.2300 0.7333 0.085 Uiso 1 calc . . H52C H 0.7663 0.3031 0.6917 0.085 Uiso 1 calc . . H1 H 1.0514(35) 0.2178(21) 0.9147(17) 0.067(11) Uiso 1 d . . H2 H 0.9364(30) 0.1494(19) 0.9838(15) 0.052(9) Uiso 1 d . . H3 H 0.7517(34) 0.0627(20) 0.9450(17) 0.063(10) Uiso 1 d . . H4A H 0.8059(32) 0.0373(19) 0.8132(16) 0.056(9) Uiso 1 d . . H4B H 0.7222(38) -0.0220(23) 0.8556(17) 0.073(11) Uiso 1 d . . H5A H 0.9407(41) -0.0758(25) 0.8347(21) 0.087(13) Uiso 1 d . . H5B H 0.9336(41) -0.0844(25) 0.9107(20) 0.091(13) Uiso 1 d . . H6A H 1.0983(31) 0.0242(19) 0.9386(16) 0.055(9) Uiso 1 d . . H6B H 1.1685(35) -0.0500(21) 0.8980(16) 0.068(10) Uiso 1 d . . H7A H 1.2287(45) 0.0812(27) 0.8604(20) 0.100(15) Uiso 1 d . . H7B H 1.1126(40) 0.0390(24) 0.7971(20) 0.090(13) Uiso 1 d . . H8A H 1.0804(30) 0.1821(18) 0.8131(14) 0.044(8) Uiso 1 d . . H8B H 0.9508(32) 0.1248(18) 0.8002(15) 0.049(8) 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 Ru1 0.03582(11) 0.03048(10) 0.03049(10) -0.00367(8) 0.00722(7) -0.00082(8) Fe2 0.0250(2) 0.0374(2) 0.0372(2) 0.00192(15) 0.00954(14) -0.00130(13) Cl3 0.0486(4) 0.0472(4) 0.0559(4) -0.0084(3) -0.0010(3) -0.0090(3) P4 0.0279(3) 0.0296(3) 0.0281(3) -0.0002(2) 0.0084(2) -0.0037(2) N5 0.0344(10) 0.0454(12) 0.0307(10) -0.0003(9) 0.0123(8) 0.0030(9) C1 0.0386(13) 0.0373(14) 0.051(2) -0.0083(12) 0.0051(12) -0.0002(11) C2 0.051(2) 0.0381(14) 0.0387(14) -0.0056(12) 0.0016(12) 0.0119(12) C3 0.055(2) 0.0351(14) 0.048(2) 0.0042(12) 0.0121(13) 0.0038(12) C4 0.058(2) 0.0327(14) 0.062(2) -0.0069(14) 0.002(2) -0.0005(13) C5 0.073(2) 0.037(2) 0.078(3) -0.009(2) -0.003(2) 0.0101(15) C6 0.058(2) 0.048(2) 0.067(2) -0.003(2) 0.002(2) 0.0185(15) C7 0.067(2) 0.057(2) 0.076(3) -0.008(2) 0.019(2) 0.016(2) C8 0.054(2) 0.049(2) 0.060(2) -0.002(2) 0.022(2) 0.0062(14) C9 0.0317(11) 0.0402(13) 0.0322(12) 0.0041(10) 0.0086(9) 0.0010(10) C11 0.0301(11) 0.0417(14) 0.0389(13) 0.0104(11) 0.0091(10) -0.0046(10) C12 0.0413(13) 0.051(2) 0.0431(15) 0.0086(13) 0.0183(12) 0.0031(12) C13 0.051(2) 0.080(2) 0.053(2) 0.020(2) 0.0275(14) 0.010(2) C14 0.051(2) 0.113(3) 0.068(2) 0.033(2) 0.026(2) -0.016(2) C15 0.063(2) 0.092(3) 0.069(2) 0.016(2) 0.011(2) -0.041(2) C16 0.049(2) 0.067(2) 0.050(2) 0.008(2) 0.0105(13) -0.0236(15) C21 0.0292(10) 0.0336(11) 0.0308(11) -0.0051(10) 0.0099(9) -0.0004(9) C22 0.0401(13) 0.0420(14) 0.0317(12) -0.0006(11) 0.0092(10) -0.0025(11) C23 0.0465(15) 0.061(2) 0.0358(14) -0.0021(13) 0.0033(12) 0.0030(13) C24 0.0361(13) 0.065(2) 0.051(2) -0.0125(15) 0.0007(12) -0.0061(13) C25 0.0408(15) 0.053(2) 0.065(2) -0.006(2) 0.0051(14) -0.0173(13) C26 0.0394(13) 0.0465(15) 0.0422(14) 0.0024(12) 0.0082(11) -0.0073(11) C31 0.0251(10) 0.0336(12) 0.0301(11) -0.0008(9) 0.0081(9) -0.0020(9) C32 0.0308(11) 0.0363(12) 0.0388(13) -0.0041(11) 0.0108(10) -0.0034(9) C33 0.0358(12) 0.0329(12) 0.053(2) -0.0046(12) 0.0150(11) -0.0017(10) C34 0.0334(12) 0.0328(12) 0.0445(14) 0.0082(11) 0.0127(11) -0.0006(10) C35 0.0276(10) 0.0358(12) 0.0323(12) 0.0033(10) 0.0097(9) -0.0030(9) C41 0.0300(13) 0.050(2) 0.114(3) -0.008(2) 0.006(2) -0.0096(12) C42 0.0289(13) 0.103(3) 0.058(2) 0.028(2) 0.0070(13) -0.018(2) C43 0.0303(13) 0.083(2) 0.066(2) -0.027(2) 0.0181(13) -0.0030(14) C44 0.0321(13) 0.067(2) 0.070(2) 0.021(2) 0.0009(14) 0.0033(13) C45 0.0331(14) 0.107(3) 0.048(2) -0.019(2) 0.0088(13) -0.013(2) C50 0.060(2) 0.059(2) 0.0373(14) 0.0082(13) 0.0122(13) 0.0099(15) C51 0.0365(13) 0.056(2) 0.054(2) 0.0120(14) 0.0178(12) -0.0025(12) C52 0.066(2) 0.074(2) 0.0351(15) 0.0005(14) 0.0219(14) 0.020(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 Ru1 C2 2.096(3) . ? Ru1 C3 2.152(3) . ? Ru1 C1 2.140(3) . ? Ru1 P4 2.1669(7) . ? Ru1 N5 2.295(2) . ? Ru1 Cl3 2.4608(13) . ? Fe2 C45 2.030(3) . ? Fe2 C41 2.030(3) . ? Fe2 C31 2.041(2) . ? Fe2 C32 2.039(3) . ? Fe2 C35 2.045(2) . ? Fe2 C42 2.042(3) . ? Fe2 C34 2.049(2) . ? Fe2 C44 2.044(3) . ? Fe2 C33 2.052(3) . ? Fe2 C43 2.049(3) . ? P4 C31 1.818(2) . ? P4 C11 1.846(2) . ? P4 C21 1.850(2) . ? N5 C51 1.480(3) . ? N5 C52 1.488(3) . ? N5 C9 1.510(3) . ? C1 C2 1.413(4) . ? C1 C8 1.503(4) . ? C2 C3 1.426(4) . ? C3 C4 1.517(4) . ? C4 C5 1.543(5) . ? C5 C6 1.514(5) . ? C6 C7 1.507(5) . ? C7 C8 1.560(5) . ? C9 C35 1.507(3) . ? C9 C50 1.534(4) . ? C11 C16 1.382(4) . ? C11 C12 1.397(4) . ? C12 C13 1.383(4) . ? C13 C14 1.370(5) . ? C14 C15 1.366(6) . ? C15 C16 1.393(4) . ? C21 C22 1.388(3) . ? C21 C26 1.396(3) . ? C22 C23 1.384(4) . ? C23 C24 1.380(4) . ? C24 C25 1.376(4) . ? C25 C26 1.381(4) . ? C31 C32 1.432(3) . ? C31 C35 1.444(3) . ? C32 C33 1.413(4) . ? C33 C34 1.408(4) . ? C34 C35 1.436(3) . ? C41 C45 1.382(5) . ? C41 C42 1.400(5) . ? C42 C43 1.394(5) . ? C43 C44 1.392(5) . ? C44 C45 1.393(5) . ? 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 C2 Ru1 C3 39.19(11) . . ? C2 Ru1 C1 38.95(11) . . ? C3 Ru1 C1 71.10(11) . . ? C2 Ru1 P4 89.21(8) . . ? C3 Ru1 P4 102.92(8) . . ? C1 Ru1 P4 103.98(8) . . ? C2 Ru1 N5 136.76(10) . . ? C3 Ru1 N5 162.25(10) . . ? C1 Ru1 N5 99.17(10) . . ? P4 Ru1 N5 93.74(5) . . ? C2 Ru1 Cl3 133.52(9) . . ? C3 Ru1 Cl3 94.40(8) . . ? C1 Ru1 Cl3 151.45(8) . . ? P4 Ru1 Cl3 103.19(4) . . ? N5 Ru1 Cl3 87.61(6) . . ? C45 Fe2 C41 39.80(15) . . ? C45 Fe2 C31 129.48(13) . . ? C41 Fe2 C31 108.99(11) . . ? C45 Fe2 C32 169.95(14) . . ? C41 Fe2 C32 133.43(13) . . ? C31 Fe2 C32 41.10(9) . . ? C45 Fe2 C35 105.64(11) . . ? C41 Fe2 C35 114.41(13) . . ? C31 Fe2 C35 41.38(9) . . ? C32 Fe2 C35 69.20(10) . . ? C45 Fe2 C42 67.18(14) . . ? C41 Fe2 C42 40.23(15) . . ? C31 Fe2 C42 118.30(12) . . ? C32 Fe2 C42 112.41(11) . . ? C35 Fe2 C42 148.53(14) . . ? C45 Fe2 C34 114.14(13) . . ? C41 Fe2 C34 146.31(15) . . ? C31 Fe2 C34 68.81(10) . . ? C32 Fe2 C34 68.08(10) . . ? C35 Fe2 C34 41.06(9) . . ? C42 Fe2 C34 170.40(14) . . ? C45 Fe2 C44 40.00(14) . . ? C41 Fe2 C44 67.01(14) . . ? C31 Fe2 C44 167.53(13) . . ? C32 Fe2 C44 149.88(13) . . ? C35 Fe2 C44 128.18(12) . . ? C42 Fe2 C44 66.95(13) . . ? C34 Fe2 C44 107.52(12) . . ? C45 Fe2 C33 147.00(14) . . ? C41 Fe2 C33 172.70(15) . . ? C31 Fe2 C33 68.66(10) . . ? C32 Fe2 C33 40.42(10) . . ? C35 Fe2 C33 68.76(10) . . ? C42 Fe2 C33 134.10(14) . . ? C34 Fe2 C33 40.16(10) . . ? C44 Fe2 C33 116.78(13) . . ? C45 Fe2 C43 67.08(13) . . ? C41 Fe2 C43 67.17(14) . . ? C31 Fe2 C43 151.12(12) . . ? C32 Fe2 C43 119.56(12) . . ? C35 Fe2 C43 167.41(13) . . ? C42 Fe2 C43 39.85(14) . . ? C34 Fe2 C43 130.99(13) . . ? C44 Fe2 C43 39.78(14) . . ? C33 Fe2 C43 111.29(12) . . ? C31 P4 C11 104.32(11) . . ? C31 P4 C21 101.08(11) . . ? C11 P4 C21 100.85(11) . . ? C31 P4 Ru1 112.53(8) . . ? C11 P4 Ru1 118.25(9) . . ? C21 P4 Ru1 117.53(8) . . ? C51 N5 C52 107.9(2) . . ? C51 N5 C9 110.8(2) . . ? C52 N5 C9 108.9(2) . . ? C51 N5 Ru1 113.2(2) . . ? C52 N5 Ru1 102.3(2) . . ? C9 N5 Ru1 113.20(14) . . ? C2 C1 C8 123.2(3) . . ? C2 C1 Ru1 68.9(2) . . ? C8 C1 Ru1 103.2(2) . . ? C1 C2 C3 123.1(3) . . ? C1 C2 Ru1 72.2(2) . . ? C3 C2 Ru1 72.5(2) . . ? C2 C3 C4 124.2(3) . . ? C2 C3 Ru1 68.3(2) . . ? C4 C3 Ru1 108.2(2) . . ? C3 C4 C5 115.2(3) . . ? C6 C5 C4 116.5(3) . . ? C7 C6 C5 118.1(3) . . ? C6 C7 C8 116.6(3) . . ? C1 C8 C7 116.5(3) . . ? C35 C9 N5 110.5(2) . . ? C35 C9 C50 110.1(2) . . ? N5 C9 C50 114.8(2) . . ? C16 C11 C12 118.4(2) . . ? C16 C11 P4 120.1(2) . . ? C12 C11 P4 121.4(2) . . ? C13 C12 C11 120.9(3) . . ? C14 C13 C12 119.6(3) . . ? C13 C14 C15 120.5(3) . . ? C14 C15 C16 120.3(3) . . ? C11 C16 C15 120.2(3) . . ? C22 C21 C26 117.6(2) . . ? C22 C21 P4 121.9(2) . . ? C26 C21 P4 120.5(2) . . ? C23 C22 C21 121.3(2) . . ? C24 C23 C22 120.2(3) . . ? C23 C24 C25 119.4(3) . . ? C26 C25 C24 120.4(3) . . ? C25 C26 C21 121.1(3) . . ? C32 C31 C35 107.5(2) . . ? C32 C31 P4 125.2(2) . . ? C35 C31 P4 126.8(2) . . ? C32 C31 Fe2 69.36(13) . . ? C35 C31 Fe2 69.46(13) . . ? P4 C31 Fe2 132.73(12) . . ? C33 C32 C31 108.4(2) . . ? C33 C32 Fe2 70.28(14) . . ? C31 C32 Fe2 69.54(13) . . ? C34 C33 C32 108.4(2) . . ? C34 C33 Fe2 69.80(15) . . ? C32 C33 Fe2 69.30(14) . . ? C33 C34 C35 108.9(2) . . ? C33 C34 Fe2 70.04(14) . . ? C35 C34 Fe2 69.35(13) . . ? C34 C35 C31 106.8(2) . . ? C34 C35 C9 125.0(2) . . ? C31 C35 C9 128.1(2) . . ? C34 C35 Fe2 69.59(13) . . ? C31 C35 Fe2 69.16(13) . . ? C9 C35 Fe2 123.0(2) . . ? C45 C41 C42 108.1(3) . . ? C45 C41 Fe2 70.1(2) . . ? C42 C41 Fe2 70.3(2) . . ? C41 C42 C43 107.7(3) . . ? C41 C42 Fe2 69.4(2) . . ? C43 C42 Fe2 70.4(2) . . ? C44 C43 C42 107.9(3) . . ? C44 C43 Fe2 69.9(2) . . ? C42 C43 Fe2 69.8(2) . . ? C43 C44 C45 108.0(3) . . ? C43 C44 Fe2 70.3(2) . . ? C45 C44 Fe2 69.5(2) . . ? C41 C45 C44 108.2(3) . . ? C41 C45 Fe2 70.1(2) . . ? C44 C45 Fe2 70.5(2) . . ? _refine_diff_density_max 0.282 _refine_diff_density_min -0.437 _refine_diff_density_rms 0.063