# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_coden_Cambridge 222 _journal_volume ? _journal_page_first ? _journal_year ? loop_ _publ_author_name 'Marcus Cole' 'M Bruce' 'Craig M Forsyth' 'Ricky S C Fung' 'Matthias Hilder' 'Peter Junk' 'Kristina Konstas' _publ_contact_author_name 'Marcus Cole' _publ_contact_author_email M.COLE@UNSW.EDU.AU _publ_section_title ; The Reactivity of N-Heterocyclic Carbenes and their Precursors with [Ru3(CO)12] ; _publ_contact_author_address ; School of Chemistry University of New South Wales Sydney NSW 2052 Australia ; _publ_contact_author_fax '+61 (0)2 9385 6141' _publ_contact_author_phone '+61 (0)2 9385 4678' # Attachment 'Compound 1.cif' data_Compound_1.cif _database_code_depnum_ccdc_archive 'CCDC 682713' loop_ _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common '[Ru(CO)4(IMes)]' _chemical_melting_point '460 (dec.)' _chemical_formula_moiety 'C12.50 H12 N O2 Ru0.50' _chemical_formula_sum 'C12.50 H12 N O2 Ru0.50' _chemical_formula_weight 258.77 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P n m a' _symmetry_int_tables_number 62 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-x, y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z-1/2' 'x, -y-1/2, z' _cell_length_a 15.8629(3) _cell_length_b 19.4171(4) _cell_length_c 7.6391(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2352.93(11) _cell_formula_units_Z 8 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour pink-orange _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.461 _exptl_crystal_density_method none _exptl_crystal_F_000 1056 _exptl_absorpt_coefficient_mu 0.699 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6791 _exptl_absorpt_correction_T_max 0.8177 _exptl_absorpt_process_details 'performed as part of the DENZO-SMN package' _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method 'psi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23689 _diffrn_reflns_av_R_equivalents 0.1188 _diffrn_reflns_av_sigmaI/netI 0.0787 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 3.70 _diffrn_reflns_theta_max 28.34 _reflns_number_total 2998 _reflns_number_gt 2231 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius Collect' _computing_cell_refinement DENZO-SMN _computing_data_reduction X-Seed _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed / POV-Ray' _computing_publication_material 'Microsoft Office 2000' _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^)+(0.0553P)^2^+4.6972P] 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 2998 _refine_ls_number_parameters 157 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0979 _refine_ls_R_factor_gt 0.0597 _refine_ls_wR_factor_ref 0.1226 _refine_ls_wR_factor_gt 0.1104 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.036 _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 Ru1 Ru 0.04639(3) 0.7500 0.10908(6) 0.01361(14) Uani 1 2 d S . . O1 O 0.11051(19) 0.61199(14) 0.2578(4) 0.0308(7) Uani 1 1 d . . . O2 O -0.1152(3) 0.7500 -0.1142(6) 0.0294(10) Uani 1 2 d S . . O3 O -0.0633(3) 0.7500 0.4378(6) 0.0326(11) Uani 1 2 d S . . N1 N 0.13695(19) 0.69488(14) -0.2308(4) 0.0142(7) Uani 1 1 d . . . C1 C 0.1155(3) 0.7500 -0.1289(7) 0.0125(11) Uani 1 2 d S . . C2 C 0.1696(2) 0.71534(19) -0.3908(5) 0.0182(8) Uani 1 1 d . . . H2 H 0.1883 0.6861 -0.4827 0.022 Uiso 1 1 calc R . . C3 C 0.1397(2) 0.62282(18) -0.1788(5) 0.0152(8) Uani 1 1 d . . . C4 C 0.0745(2) 0.57902(19) -0.2269(5) 0.0184(8) Uani 1 1 d . . . C5 C 0.0831(3) 0.50932(19) -0.1816(5) 0.0202(8) Uani 1 1 d . . . H5 H 0.0389 0.4783 -0.2099 0.024 Uiso 1 1 calc R . . C6 C 0.1534(3) 0.4846(2) -0.0979(5) 0.0222(9) Uani 1 1 d . . . C7 C 0.2176(2) 0.5305(2) -0.0540(5) 0.0206(9) Uani 1 1 d . . . H7 H 0.2664 0.5136 0.0043 0.025 Uiso 1 1 calc R . . C8 C 0.2123(2) 0.5999(2) -0.0931(5) 0.0173(8) Uani 1 1 d . . . C9 C -0.0018(2) 0.6032(2) -0.3257(6) 0.0232(9) Uani 1 1 d . . . H9A H -0.0184 0.6489 -0.2830 0.035 Uiso 1 1 calc R . . H9B H -0.0482 0.5707 -0.3077 0.035 Uiso 1 1 calc R . . H9C H 0.0115 0.6060 -0.4508 0.035 Uiso 1 1 calc R . . C10 C 0.1621(3) 0.4091(2) -0.0541(6) 0.0307(11) Uani 1 1 d . . . H10A H 0.1066 0.3870 -0.0598 0.046 Uiso 1 1 calc R . . H10B H 0.1851 0.4041 0.0643 0.046 Uiso 1 1 calc R . . H10C H 0.2001 0.3871 -0.1383 0.046 Uiso 1 1 calc R . . C11 C 0.2814(2) 0.6491(2) -0.0421(6) 0.0218(9) Uani 1 1 d . . . H11A H 0.3285 0.6233 0.0089 0.033 Uiso 1 1 calc R . . H11B H 0.2598 0.6820 0.0441 0.033 Uiso 1 1 calc R . . H11C H 0.3009 0.6740 -0.1461 0.033 Uiso 1 1 calc R . . C12 C 0.0924(2) 0.6624(2) 0.1910(5) 0.0213(9) Uani 1 1 d . . . C13 C -0.0531(4) 0.7500 -0.0359(8) 0.0191(12) Uani 1 2 d S . . C14 C -0.0224(3) 0.7500 0.3159(8) 0.0190(12) Uani 1 2 d S . . 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 0.0154(2) 0.0109(2) 0.0146(2) 0.000 0.0018(2) 0.000 O1 0.0482(19) 0.0180(15) 0.0263(16) 0.0093(13) 0.0068(14) 0.0118(15) O2 0.024(2) 0.024(2) 0.040(3) 0.000 -0.012(2) 0.000 O3 0.033(2) 0.027(2) 0.038(3) 0.000 0.020(2) 0.000 N1 0.0179(16) 0.0079(15) 0.0167(16) 0.0004(13) 0.0027(13) 0.0000(13) C1 0.009(2) 0.012(2) 0.016(3) 0.000 -0.002(2) 0.000 C2 0.0214(19) 0.0153(18) 0.0177(18) -0.0014(17) 0.0039(17) 0.0035(16) C3 0.022(2) 0.0075(17) 0.0164(18) 0.0019(15) 0.0051(16) 0.0017(16) C4 0.0201(19) 0.0165(19) 0.018(2) -0.0024(16) 0.0040(16) 0.0013(17) C5 0.026(2) 0.0116(18) 0.023(2) -0.0016(16) 0.0010(18) -0.0031(17) C6 0.027(2) 0.0145(19) 0.025(2) 0.0013(18) 0.0033(19) 0.0014(17) C7 0.020(2) 0.021(2) 0.020(2) 0.0000(17) -0.0021(16) 0.0066(18) C8 0.0173(19) 0.0168(19) 0.018(2) -0.0009(17) 0.0037(16) 0.0023(16) C9 0.023(2) 0.017(2) 0.029(2) -0.0021(18) -0.0062(19) -0.0040(17) C10 0.041(3) 0.017(2) 0.035(3) 0.0047(19) -0.004(2) 0.004(2) C11 0.0186(19) 0.022(2) 0.025(2) 0.0009(18) 0.0007(17) -0.0003(18) C12 0.023(2) 0.022(2) 0.019(2) -0.0025(18) 0.0043(17) 0.0028(18) C13 0.020(3) 0.011(3) 0.026(3) 0.000 0.007(3) 0.000 C14 0.021(3) 0.014(3) 0.022(3) 0.000 0.002(2) 0.000 _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 C14 1.920(6) . ? Ru1 C13 1.928(6) . ? Ru1 C12 1.954(4) 8_575 ? Ru1 C12 1.954(4) . ? Ru1 C1 2.123(5) . ? O1 C12 1.140(5) . ? O2 C13 1.153(7) . ? O3 C14 1.135(7) . ? N1 C1 1.367(4) . ? N1 C2 1.385(5) . ? N1 C3 1.455(4) . ? C1 N1 1.367(4) 8_575 ? C2 C2 1.346(7) 8_575 ? C3 C4 1.388(5) . ? C3 C8 1.398(5) . ? C4 C5 1.404(5) . ? C4 C9 1.502(6) . ? C5 C6 1.372(6) . ? C6 C7 1.395(6) . ? C6 C10 1.510(5) . ? C7 C8 1.383(5) . ? C8 C11 1.505(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 C14 Ru1 C13 90.4(2) . . ? C14 Ru1 C12 87.06(14) . 8_575 ? C13 Ru1 C12 119.33(12) . 8_575 ? C14 Ru1 C12 87.06(14) . . ? C13 Ru1 C12 119.33(12) . . ? C12 Ru1 C12 121.0(2) 8_575 . ? C14 Ru1 C1 176.5(2) . . ? C13 Ru1 C1 86.0(2) . . ? C12 Ru1 C1 94.67(13) 8_575 . ? C12 Ru1 C1 94.67(13) . . ? C1 N1 C2 111.8(3) . . ? C1 N1 C3 127.2(3) . . ? C2 N1 C3 120.4(3) . . ? N1 C1 N1 103.1(4) . 8_575 ? N1 C1 Ru1 128.1(2) . . ? N1 C1 Ru1 128.1(2) 8_575 . ? C2 C2 N1 106.7(2) 8_575 . ? C4 C3 C8 122.9(3) . . ? C4 C3 N1 119.6(3) . . ? C8 C3 N1 117.3(3) . . ? C3 C4 C5 116.9(4) . . ? C3 C4 C9 122.8(3) . . ? C5 C4 C9 120.3(4) . . ? C6 C5 C4 122.2(4) . . ? C5 C6 C7 118.8(4) . . ? C5 C6 C10 121.2(4) . . ? C7 C6 C10 120.0(4) . . ? C8 C7 C6 121.7(4) . . ? C7 C8 C3 117.5(4) . . ? C7 C8 C11 121.2(4) . . ? C3 C8 C11 121.3(3) . . ? O1 C12 Ru1 169.9(4) . . ? O2 C13 Ru1 176.3(5) . . ? O3 C14 Ru1 179.8(5) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 28.34 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.272 _refine_diff_density_min -1.082 _refine_diff_density_rms 0.139 _chemical_compound_source Hexane # Attachment 'Compound 2.cif' data_Compound_2.cif _database_code_depnum_ccdc_archive 'CCDC 682714' loop_ _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common '[Ru(CO)4(IPr)].toluene' _chemical_melting_point '413 (dec.)' _chemical_formula_moiety 'C38 H44 N2 O4 Ru' _chemical_formula_sum 'C38 H44 N2 O4 Ru' _chemical_formula_weight 693.82 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' Ru Ru -1.2594 0.8363 '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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P n a 21' _symmetry_int_tables_number 33 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x+1/2, y+1/2, z+1/2' 'x+1/2, -y+1/2, z' _cell_length_a 18.9137(5) _cell_length_b 9.3589(3) _cell_length_c 19.9644(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3533.93(18) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour 'light red' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.304 _exptl_crystal_density_method none _exptl_crystal_F_000 1448 _exptl_absorpt_coefficient_mu 0.484 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.9095 _exptl_absorpt_correction_T_max 0.9532 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method 'psi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 40131 _diffrn_reflns_av_R_equivalents 0.0803 _diffrn_reflns_av_sigmaI/netI 0.0823 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.04 _diffrn_reflns_theta_max 28.18 _reflns_number_total 8570 _reflns_number_gt 5722 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius Collect' _computing_cell_refinement DENZO-SMN _computing_data_reduction X-Seed _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed / POV-Ray' _computing_publication_material 'Microsoft Office 2000' _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^)+(0.0214P)^2^+1.6876P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.05(4) _refine_ls_number_reflns 8570 _refine_ls_number_parameters 415 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1073 _refine_ls_R_factor_gt 0.0533 _refine_ls_wR_factor_ref 0.0792 _refine_ls_wR_factor_gt 0.0699 _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_restrained_S_all 1.057 _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 Ru1 Ru 0.251318(13) 0.49410(3) 0.08363(4) 0.01788(6) Uani 1 1 d . . . O1 O 0.12221(13) 0.3307(3) 0.13776(16) 0.0392(8) Uani 1 1 d . . . O2 O 0.29201(13) 0.4113(3) -0.06045(14) 0.0318(7) Uani 1 1 d . . . O3 O 0.29935(14) 0.7621(3) 0.16123(15) 0.0389(7) Uani 1 1 d . . . O4 O 0.14502(14) 0.6815(3) 0.01004(16) 0.0375(8) Uani 1 1 d . . . N1 N 0.33456(12) 0.2184(3) 0.13125(15) 0.0164(6) Uani 1 1 d . . . N2 N 0.40570(13) 0.3959(3) 0.12365(15) 0.0148(6) Uani 1 1 d . . . C1 C 0.33545(16) 0.3616(3) 0.11958(18) 0.0152(8) Uani 1 1 d . . . C2 C 0.40245(17) 0.1650(4) 0.14086(18) 0.0214(9) Uani 1 1 d . . . H2 H 0.4151 0.0683 0.1491 0.026 Uiso 1 1 calc R . . C3 C 0.44640(17) 0.2763(3) 0.13632(18) 0.0193(8) Uani 1 1 d . . . H3 H 0.4964 0.2737 0.1409 0.023 Uiso 1 1 calc R . . C4 C 0.27245(17) 0.1308(4) 0.1408(2) 0.0186(9) Uani 1 1 d . . . C5 C 0.24091(15) 0.0668(3) 0.0848(3) 0.0206(7) Uani 1 1 d . . . C6 C 0.17954(17) -0.0127(3) 0.0962(2) 0.0240(10) Uani 1 1 d . . . H6 H 0.1565 -0.0575 0.0595 0.029 Uiso 1 1 calc R . . C7 C 0.15176(19) -0.0271(4) 0.1599(2) 0.0295(10) Uani 1 1 d . . . H7 H 0.1096 -0.0805 0.1665 0.035 Uiso 1 1 calc R . . C8 C 0.1850(2) 0.0358(4) 0.2140(2) 0.0283(10) Uani 1 1 d . . . H8 H 0.1657 0.0235 0.2575 0.034 Uiso 1 1 calc R . . C9 C 0.2463(2) 0.1167(4) 0.2061(2) 0.0259(10) Uani 1 1 d . . . C10 C 0.27402(19) 0.0733(4) 0.0163(2) 0.0230(9) Uani 1 1 d . . . H10 H 0.3062 0.1580 0.0156 0.028 Uiso 1 1 calc R . . C11 C 0.2205(2) 0.0928(5) -0.0399(2) 0.0335(11) Uani 1 1 d . . . H11A H 0.1900 0.0084 -0.0425 0.050 Uiso 1 1 calc R . . H11B H 0.2455 0.1052 -0.0825 0.050 Uiso 1 1 calc R . . H11C H 0.1916 0.1775 -0.0309 0.050 Uiso 1 1 calc R . . C12 C 0.3196(2) -0.0601(4) 0.0026(2) 0.0328(10) Uani 1 1 d . . . H12A H 0.3559 -0.0688 0.0373 0.049 Uiso 1 1 calc R . . H12B H 0.3423 -0.0510 -0.0413 0.049 Uiso 1 1 calc R . . H12C H 0.2895 -0.1453 0.0030 0.049 Uiso 1 1 calc R . . C13 C 0.2838(2) 0.1773(4) 0.26682(19) 0.0291(10) Uani 1 1 d . . . H13 H 0.3235 0.2385 0.2505 0.035 Uiso 1 1 calc R . . C14 C 0.2359(2) 0.2698(6) 0.3097(3) 0.0675(17) Uani 1 1 d . . . H14A H 0.2184 0.3502 0.2830 0.101 Uiso 1 1 calc R . . H14B H 0.2626 0.3062 0.3482 0.101 Uiso 1 1 calc R . . H14C H 0.1958 0.2127 0.3256 0.101 Uiso 1 1 calc R . . C15 C 0.3154(3) 0.0581(5) 0.3093(3) 0.0580(14) Uani 1 1 d . . . H15A H 0.2780 -0.0088 0.3225 0.087 Uiso 1 1 calc R . . H15B H 0.3372 0.0991 0.3495 0.087 Uiso 1 1 calc R . . H15C H 0.3514 0.0072 0.2833 0.087 Uiso 1 1 calc R . . C16 C 0.43572(16) 0.5392(3) 0.1265(2) 0.0160(7) Uani 1 1 d . . . C17 C 0.45862(16) 0.6051(4) 0.06721(17) 0.0178(9) Uani 1 1 d . . . C18 C 0.48950(16) 0.7391(4) 0.0733(2) 0.0220(10) Uani 1 1 d . . . H18 H 0.5051 0.7876 0.0342 0.026 Uiso 1 1 calc R . . C19 C 0.49803(16) 0.8031(4) 0.1350(2) 0.0267(9) Uani 1 1 d . . . H19 H 0.5198 0.8943 0.1379 0.032 Uiso 1 1 calc R . . C20 C 0.47519(18) 0.7358(4) 0.1926(2) 0.0220(9) Uani 1 1 d . . . H20 H 0.4813 0.7813 0.2347 0.026 Uiso 1 1 calc R . . C21 C 0.44327(17) 0.6017(4) 0.18950(19) 0.0178(8) Uani 1 1 d . . . C22 C 0.45400(18) 0.5323(4) -0.00018(19) 0.0205(9) Uani 1 1 d . . . H22 H 0.4225 0.4471 0.0047 0.025 Uiso 1 1 calc R . . C23 C 0.42194(19) 0.6296(4) -0.05403(19) 0.0288(10) Uani 1 1 d . . . H23A H 0.3756 0.6636 -0.0391 0.043 Uiso 1 1 calc R . . H23B H 0.4165 0.5757 -0.0958 0.043 Uiso 1 1 calc R . . H23C H 0.4532 0.7114 -0.0616 0.043 Uiso 1 1 calc R . . C24 C 0.52747(17) 0.4791(4) -0.02185(19) 0.0270(9) Uani 1 1 d . . . H24A H 0.5587 0.5611 -0.0294 0.041 Uiso 1 1 calc R . . H24B H 0.5232 0.4239 -0.0634 0.041 Uiso 1 1 calc R . . H24C H 0.5474 0.4183 0.0134 0.041 Uiso 1 1 calc R . . C25 C 0.41994(19) 0.5274(4) 0.25378(19) 0.0270(9) Uani 1 1 d . . . H25 H 0.3859 0.4502 0.2412 0.032 Uiso 1 1 calc R . . C26 C 0.3826(2) 0.6276(5) 0.3026(2) 0.0394(11) Uani 1 1 d . . . H26A H 0.3667 0.5733 0.3418 0.059 Uiso 1 1 calc R . . H26B H 0.3417 0.6713 0.2805 0.059 Uiso 1 1 calc R . . H26C H 0.4155 0.7025 0.3170 0.059 Uiso 1 1 calc R . . C27 C 0.4833(2) 0.4572(5) 0.2872(2) 0.0380(11) Uani 1 1 d . . . H27A H 0.5058 0.3911 0.2557 0.057 Uiso 1 1 calc R . . H27B H 0.4675 0.4043 0.3269 0.057 Uiso 1 1 calc R . . H27C H 0.5173 0.5308 0.3006 0.057 Uiso 1 1 calc R . . C28 C 0.1746(2) 0.3828(4) 0.1219(2) 0.0273(10) Uani 1 1 d . . . C29 C 0.28012(19) 0.4391(4) -0.0062(2) 0.0220(9) Uani 1 1 d . . . C30 C 0.28492(18) 0.6590(4) 0.1340(2) 0.0238(9) Uani 1 1 d . . . C31 C 0.1840(2) 0.6128(4) 0.0401(2) 0.0233(10) Uani 1 1 d . . . C32 C 0.5210(3) 0.0796(6) -0.0533(3) 0.0713(16) Uani 1 1 d . . . H32A H 0.5550 0.1584 -0.0566 0.107 Uiso 1 1 calc R . . H32B H 0.5465 -0.0116 -0.0526 0.107 Uiso 1 1 calc R . . H32C H 0.4934 0.0896 -0.0120 0.107 Uiso 1 1 calc R . . C33 C 0.4738(2) 0.0831(5) -0.1106(3) 0.0467(13) Uani 1 1 d . . . C34 C 0.4796(3) -0.0235(5) -0.1615(3) 0.0479(13) Uani 1 1 d . . . H34 H 0.5146 -0.0959 -0.1584 0.057 Uiso 1 1 calc R . . C35 C 0.4346(3) -0.0199(5) -0.2140(3) 0.0491(13) Uani 1 1 d . . . H35 H 0.4385 -0.0921 -0.2472 0.059 Uiso 1 1 calc R . . C36 C 0.3823(3) 0.0859(6) -0.2217(3) 0.0590(15) Uani 1 1 d . . . H36 H 0.3520 0.0867 -0.2597 0.071 Uiso 1 1 calc R . . C37 C 0.3764(3) 0.1850(5) -0.1738(3) 0.0532(13) Uani 1 1 d . . . H37 H 0.3413 0.2571 -0.1777 0.064 Uiso 1 1 calc R . . C38 C 0.4217(2) 0.1843(4) -0.1176(2) 0.0371(11) Uani 1 1 d . . . H38 H 0.4161 0.2552 -0.0839 0.044 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 Ru1 0.01145(9) 0.01863(11) 0.02357(11) -0.00082(17) -0.00170(16) 0.00136(13) O1 0.0178(13) 0.0370(16) 0.063(2) 0.0072(16) 0.0072(16) -0.0015(13) O2 0.0324(16) 0.0399(17) 0.0230(18) -0.0053(14) -0.0032(14) 0.0075(13) O3 0.0361(16) 0.0278(16) 0.053(2) -0.0110(14) -0.0172(15) 0.0119(14) O4 0.0275(15) 0.0315(17) 0.053(2) -0.0048(15) -0.0130(15) 0.0088(13) N1 0.0128(13) 0.0154(14) 0.0212(18) -0.0026(14) -0.0001(14) -0.0012(12) N2 0.0136(14) 0.0158(14) 0.0149(16) 0.0016(13) -0.0002(13) 0.0010(12) C1 0.0136(17) 0.0185(18) 0.013(2) -0.0050(16) 0.0004(15) -0.0002(14) C2 0.0190(18) 0.0213(19) 0.024(2) -0.0021(17) -0.0002(17) 0.0059(16) C3 0.0143(16) 0.026(2) 0.018(2) -0.0085(17) -0.0002(16) -0.0014(16) C4 0.0146(17) 0.0123(18) 0.029(3) -0.0023(16) 0.0028(17) -0.0002(15) C5 0.0160(16) 0.0164(13) 0.0295(18) -0.001(3) -0.002(2) 0.0021(13) C6 0.0184(15) 0.0202(18) 0.033(3) -0.0015(19) -0.0051(17) -0.0015(15) C7 0.0184(19) 0.024(2) 0.046(3) 0.0026(19) 0.0011(19) -0.0058(17) C8 0.023(2) 0.028(2) 0.034(3) 0.0017(18) 0.0088(18) -0.0011(17) C9 0.023(2) 0.0184(19) 0.036(3) 0.0025(17) -0.001(2) 0.0067(18) C10 0.0166(18) 0.023(2) 0.029(3) -0.0028(18) -0.0033(17) -0.0032(17) C11 0.034(2) 0.044(3) 0.022(3) -0.003(2) -0.003(2) -0.009(2) C12 0.031(2) 0.025(2) 0.042(3) -0.005(2) 0.009(2) 0.0012(19) C13 0.031(2) 0.033(2) 0.023(3) 0.0021(18) 0.0046(19) -0.0081(19) C14 0.057(3) 0.085(4) 0.060(4) -0.045(3) -0.017(3) 0.013(3) C15 0.056(3) 0.070(3) 0.048(3) 0.014(3) -0.018(3) -0.007(3) C16 0.0098(16) 0.0181(17) 0.020(2) -0.0026(16) 0.0004(16) 0.0029(13) C17 0.0113(16) 0.0244(19) 0.018(3) 0.0001(15) 0.0018(14) 0.0009(14) C18 0.0178(19) 0.0277(19) 0.020(3) 0.007(2) 0.0011(18) -0.0024(16) C19 0.0158(18) 0.0266(19) 0.038(3) 0.003(2) -0.003(2) -0.0015(16) C20 0.0163(17) 0.025(2) 0.024(2) -0.0112(18) -0.0033(16) 0.0022(16) C21 0.0097(17) 0.028(2) 0.016(2) 0.0005(17) -0.0037(16) 0.0021(16) C22 0.0174(18) 0.026(2) 0.019(2) 0.0020(17) 0.0006(17) -0.0021(15) C23 0.025(2) 0.036(2) 0.025(3) 0.0013(19) 0.0000(19) 0.0003(18) C24 0.0187(18) 0.041(2) 0.021(2) -0.0038(19) 0.0024(16) 0.0041(18) C25 0.025(2) 0.036(2) 0.020(2) -0.0056(19) -0.0017(17) -0.0102(18) C26 0.030(2) 0.069(3) 0.020(3) 0.003(2) -0.002(2) 0.008(2) C27 0.048(3) 0.043(3) 0.023(3) -0.001(2) -0.004(2) 0.005(2) C28 0.020(2) 0.026(2) 0.036(3) 0.001(2) 0.0006(19) 0.0038(17) C29 0.0172(18) 0.0185(19) 0.030(3) 0.0002(18) -0.0046(19) 0.0063(16) C30 0.0207(19) 0.022(2) 0.029(2) -0.0038(19) -0.0098(19) 0.0058(17) C31 0.016(2) 0.020(2) 0.034(3) -0.0033(19) 0.0027(18) -0.0008(18) C32 0.084(4) 0.057(3) 0.072(5) 0.017(3) -0.005(4) 0.002(3) C33 0.033(3) 0.045(3) 0.062(4) 0.020(3) 0.002(2) -0.010(2) C34 0.053(3) 0.031(3) 0.059(4) 0.000(2) 0.018(3) -0.014(2) C35 0.051(3) 0.038(3) 0.058(4) 0.000(2) 0.019(3) 0.002(2) C36 0.057(3) 0.071(4) 0.049(4) 0.004(3) 0.004(3) -0.030(3) C37 0.055(3) 0.050(3) 0.054(4) 0.002(3) 0.018(3) -0.014(3) C38 0.040(3) 0.037(2) 0.035(3) -0.004(2) 0.007(2) -0.002(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 C31 1.900(4) . ? Ru1 C28 1.942(4) . ? Ru1 C29 1.943(4) . ? Ru1 C30 1.949(4) . ? Ru1 C1 2.141(3) . ? O1 C28 1.150(4) . ? O2 C29 1.137(4) . ? O3 C30 1.141(4) . ? O4 C31 1.148(4) . ? N1 C1 1.361(4) . ? N1 C2 1.391(4) . ? N1 C4 1.445(4) . ? N2 C1 1.369(4) . ? N2 C3 1.382(4) . ? N2 C16 1.457(4) . ? C2 C3 1.336(4) . ? C4 C9 1.400(5) . ? C4 C5 1.403(6) . ? C5 C6 1.397(4) . ? C5 C10 1.505(6) . ? C6 C7 1.383(5) . ? C7 C8 1.381(6) . ? C8 C9 1.393(5) . ? C9 C13 1.515(5) . ? C10 C11 1.522(5) . ? C10 C12 1.541(5) . ? C13 C14 1.517(6) . ? C13 C15 1.524(6) . ? C16 C21 1.395(5) . ? C16 C17 1.403(5) . ? C17 C18 1.389(4) . ? C17 C22 1.510(5) . ? C18 C19 1.379(6) . ? C19 C20 1.380(5) . ? C20 C21 1.394(5) . ? C21 C25 1.525(5) . ? C22 C23 1.533(5) . ? C22 C24 1.538(5) . ? C25 C27 1.520(5) . ? C25 C26 1.526(5) . ? C32 C33 1.450(7) . ? C33 C38 1.373(6) . ? C33 C34 1.428(7) . ? C34 C35 1.350(7) . ? C35 C36 1.409(7) . ? C36 C37 1.336(7) . ? C37 C38 1.413(6) . ? 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 C31 Ru1 C28 89.59(14) . . ? C31 Ru1 C29 85.47(16) . . ? C28 Ru1 C29 115.47(17) . . ? C31 Ru1 C30 89.53(16) . . ? C28 Ru1 C30 117.72(17) . . ? C29 Ru1 C30 126.50(16) . . ? C31 Ru1 C1 171.84(16) . . ? C28 Ru1 C1 96.47(14) . . ? C29 Ru1 C1 86.99(14) . . ? C30 Ru1 C1 92.47(13) . . ? C1 N1 C2 111.5(3) . . ? C1 N1 C4 126.2(3) . . ? C2 N1 C4 121.9(3) . . ? C1 N2 C3 111.2(3) . . ? C1 N2 C16 126.6(3) . . ? C3 N2 C16 121.4(2) . . ? N1 C1 N2 103.5(3) . . ? N1 C1 Ru1 128.2(2) . . ? N2 C1 Ru1 127.2(2) . . ? C3 C2 N1 106.5(3) . . ? C2 C3 N2 107.3(3) . . ? C9 C4 C5 123.5(3) . . ? C9 C4 N1 117.7(3) . . ? C5 C4 N1 118.9(3) . . ? C6 C5 C4 116.8(4) . . ? C6 C5 C10 121.0(4) . . ? C4 C5 C10 122.0(3) . . ? C7 C6 C5 121.2(4) . . ? C8 C7 C6 120.3(3) . . ? C7 C8 C9 121.5(4) . . ? C8 C9 C4 116.8(4) . . ? C8 C9 C13 120.2(4) . . ? C4 C9 C13 123.0(3) . . ? C5 C10 C11 113.5(3) . . ? C5 C10 C12 111.2(3) . . ? C11 C10 C12 109.7(3) . . ? C9 C13 C14 112.7(3) . . ? C9 C13 C15 110.8(3) . . ? C14 C13 C15 109.8(4) . . ? C21 C16 C17 123.0(3) . . ? C21 C16 N2 117.4(3) . . ? C17 C16 N2 119.5(3) . . ? C18 C17 C16 116.9(3) . . ? C18 C17 C22 120.7(3) . . ? C16 C17 C22 122.4(3) . . ? C19 C18 C17 121.4(4) . . ? C18 C19 C20 120.6(3) . . ? C19 C20 C21 120.6(4) . . ? C20 C21 C16 117.5(3) . . ? C20 C21 C25 119.9(3) . . ? C16 C21 C25 122.6(3) . . ? C17 C22 C23 112.3(3) . . ? C17 C22 C24 110.1(3) . . ? C23 C22 C24 110.6(3) . . ? C27 C25 C21 109.8(3) . . ? C27 C25 C26 110.5(3) . . ? C21 C25 C26 113.0(3) . . ? O1 C28 Ru1 168.6(3) . . ? O2 C29 Ru1 174.5(3) . . ? O3 C30 Ru1 173.7(3) . . ? O4 C31 Ru1 175.7(4) . . ? C38 C33 C34 117.6(5) . . ? C38 C33 C32 122.5(5) . . ? C34 C33 C32 119.9(5) . . ? C35 C34 C33 119.2(5) . . ? C34 C35 C36 123.0(5) . . ? C37 C36 C35 117.9(5) . . ? C36 C37 C38 121.0(5) . . ? C33 C38 C37 121.3(5) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 28.18 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.564 _refine_diff_density_min -0.522 _refine_diff_density_rms 0.074 _chemical_compound_source Toluene # Attachment 'Compound 3.cif' data_Compound_3.cif _database_code_depnum_ccdc_archive 'CCDC 682715' loop_ _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common '[Ru4(mu4-S)2(CO)9(IMes)2]2THF' _chemical_melting_point '571 dec.' _chemical_formula_moiety 'C59 H64 N4 O11 Ru4 S2' _chemical_formula_sum 'C29.50 H32 N2 O5.50 Ru2 S' _chemical_formula_weight 736.77 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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 orthorhombic _symmetry_space_group_name_H-M 'P c c n' _symmetry_int_tables_number 56 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' 'x+1/2, -y, -z+1/2' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' '-x-1/2, y, z-1/2' 'x, -y-1/2, z-1/2' _cell_length_a 10.73890(10) _cell_length_b 22.2879(3) _cell_length_c 24.3237(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5821.82(12) _cell_formula_units_Z 8 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour 'red orange' _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.681 _exptl_crystal_density_method none _exptl_crystal_F_000 2968 _exptl_absorpt_coefficient_mu 1.153 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7236 _exptl_absorpt_correction_T_max 0.8646 _exptl_absorpt_process_details 'performed as part of the DENZO-SMN package' _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method 'psi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 45226 _diffrn_reflns_av_R_equivalents 0.0840 _diffrn_reflns_av_sigmaI/netI 0.0501 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 1.91 _diffrn_reflns_theta_max 30.33 _reflns_number_total 8324 _reflns_number_gt 5840 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius Collect' _computing_cell_refinement DENZO-SMN _computing_data_reduction X-Seed _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed / POV-Ray' _computing_publication_material 'Microsoft Office 2000' _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^)+(0.0699P)^2^+0.8871P] 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 8324 _refine_ls_number_parameters 368 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0738 _refine_ls_R_factor_gt 0.0452 _refine_ls_wR_factor_ref 0.1271 _refine_ls_wR_factor_gt 0.1112 _refine_ls_goodness_of_fit_ref 1.062 _refine_ls_restrained_S_all 1.062 _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 Ru1 Ru 0.81805(2) 0.698660(10) 0.023200(10) 0.01278(8) Uani 1 1 d . . . Ru2 Ru 0.81314(2) 0.696110(10) 0.135950(10) 0.01515(8) Uani 1 1 d . . . S1 S 0.87442(7) 0.78280(3) 0.08399(3) 0.01588(16) Uani 1 1 d . . . O1 O 0.7500 0.7500 -0.08858(12) 0.0262(8) Uani 1 2 d S . . O2 O 1.0801(2) 0.71220(10) -0.01660(9) 0.0261(5) Uani 1 1 d . . . O3 O 0.9382(2) 0.59256(10) 0.08367(8) 0.0243(5) Uani 1 1 d . . . O4 O 0.6770(2) 0.60910(12) 0.20817(10) 0.0358(6) Uani 1 1 d . . . O5 O 1.0305(3) 0.70578(13) 0.21498(11) 0.0432(7) Uani 1 1 d . . . O6 O 0.8891(4) 0.51572(14) 0.28939(12) 0.0612(9) Uani 1 1 d . . . N1 N 0.6720(2) 0.58628(12) -0.01200(11) 0.0207(6) Uani 1 1 d . . . N2 N 0.8342(2) 0.59481(13) -0.06251(12) 0.0226(6) Uani 1 1 d . . . C1 C 0.7703(3) 0.62344(14) -0.02141(12) 0.0184(6) Uani 1 1 d . . . C2 C 0.6754(3) 0.53731(16) -0.04525(15) 0.0302(8) Uani 1 1 d . . . H2 H 0.6167 0.5054 -0.0460 0.036 Uiso 1 1 calc R . . C3 C 0.7771(4) 0.54256(17) -0.07666(14) 0.0319(9) Uani 1 1 d . . . H3 H 0.8044 0.5149 -0.1038 0.038 Uiso 1 1 calc R . . C4 C 0.5628(3) 0.59871(14) 0.02115(13) 0.0215(7) Uani 1 1 d . . . C5 C 0.4690(3) 0.63292(14) -0.00215(13) 0.0229(7) Uani 1 1 d . . . C6 C 0.3651(3) 0.64513(15) 0.03024(14) 0.0267(7) Uani 1 1 d . . . H6 H 0.2995 0.6684 0.0150 0.032 Uiso 1 1 calc R . . C7 C 0.3537(3) 0.62473(17) 0.08355(14) 0.0273(8) Uani 1 1 d . . . C8 C 0.4453(3) 0.58757(15) 0.10373(14) 0.0260(7) Uani 1 1 d . . . H8 H 0.4359 0.5714 0.1396 0.031 Uiso 1 1 calc R . . C9 C 0.5517(3) 0.57271(14) 0.07341(12) 0.0218(7) Uani 1 1 d . . . C10 C 0.4789(3) 0.65581(17) -0.06016(14) 0.0290(8) Uani 1 1 d . . . H10A H 0.5530 0.6812 -0.0636 0.043 Uiso 1 1 calc R . . H10B H 0.4046 0.6793 -0.0692 0.043 Uiso 1 1 calc R . . H10C H 0.4857 0.6218 -0.0855 0.043 Uiso 1 1 calc R . . C11 C 0.2432(4) 0.6409(2) 0.11816(17) 0.0459(11) Uani 1 1 d . . . H11A H 0.1726 0.6152 0.1082 0.069 Uiso 1 1 calc R . . H11B H 0.2212 0.6830 0.1119 0.069 Uiso 1 1 calc R . . H11C H 0.2636 0.6350 0.1571 0.069 Uiso 1 1 calc R . . C12 C 0.6446(3) 0.52888(16) 0.09373(15) 0.0286(8) Uani 1 1 d . . . H12A H 0.6336 0.5231 0.1334 0.043 Uiso 1 1 calc R . . H12B H 0.7287 0.5440 0.0865 0.043 Uiso 1 1 calc R . . H12C H 0.6330 0.4905 0.0748 0.043 Uiso 1 1 calc R . . C13 C 0.9368(3) 0.61613(15) -0.09530(13) 0.0225(7) Uani 1 1 d . . . C14 C 0.9098(3) 0.64544(15) -0.14447(13) 0.0270(8) Uani 1 1 d . . . C15 C 1.0090(4) 0.66393(17) -0.17678(14) 0.0324(8) Uani 1 1 d . . . H15 H 0.9923 0.6858 -0.2095 0.039 Uiso 1 1 calc R . . C16 C 1.1313(4) 0.65170(16) -0.16312(15) 0.0316(8) Uani 1 1 d . . . C17 C 1.1544(3) 0.61894(16) -0.11574(15) 0.0293(8) Uani 1 1 d . . . H17 H 1.2379 0.6090 -0.1066 0.035 Uiso 1 1 calc R . . C18 C 1.0588(3) 0.60016(15) -0.08108(13) 0.0238(7) Uani 1 1 d . . . C19 C 0.7777(4) 0.6516(2) -0.16517(14) 0.0358(9) Uani 1 1 d . . . H19A H 0.7555 0.6161 -0.1867 0.054 Uiso 1 1 calc R . . H19B H 0.7712 0.6874 -0.1884 0.054 Uiso 1 1 calc R . . H19C H 0.7209 0.6554 -0.1338 0.054 Uiso 1 1 calc R . . C20 C 1.2386(4) 0.67036(18) -0.19934(19) 0.0470(11) Uani 1 1 d . . . H20A H 1.2808 0.6346 -0.2135 0.070 Uiso 1 1 calc R . . H20B H 1.2976 0.6944 -0.1779 0.070 Uiso 1 1 calc R . . H20C H 1.2071 0.6943 -0.2302 0.070 Uiso 1 1 calc R . . C21 C 1.0875(3) 0.56357(16) -0.03147(14) 0.0289(8) Uani 1 1 d . . . H21A H 1.0318 0.5752 -0.0014 0.043 Uiso 1 1 calc R . . H21B H 1.1741 0.5704 -0.0204 0.043 Uiso 1 1 calc R . . H21C H 1.0756 0.5210 -0.0399 0.043 Uiso 1 1 calc R . . C22 C 0.7500 0.7500 -0.04104(18) 0.0189(9) Uani 1 2 d S . . C23 C 0.9775(3) 0.70315(13) -0.00533(13) 0.0185(6) Uani 1 1 d . . . C24 C 0.8857(3) 0.63701(15) 0.08334(11) 0.0186(6) Uani 1 1 d . . . C25 C 0.7310(3) 0.64172(15) 0.18097(13) 0.0235(7) Uani 1 1 d . . . C26 C 0.9497(3) 0.70060(15) 0.18430(13) 0.0239(7) Uani 1 1 d . . . C27 C 0.8851(5) 0.4781(2) 0.24342(18) 0.0593(14) Uani 1 1 d . . . H27A H 0.8045 0.4827 0.2241 0.071 Uiso 1 1 calc R . . H27B H 0.8940 0.4357 0.2549 0.071 Uiso 1 1 calc R . . C28 C 0.9905(6) 0.4954(2) 0.2059(2) 0.0782(18) Uani 1 1 d . . . H28A H 1.0578 0.4651 0.2075 0.094 Uiso 1 1 calc R . . H28B H 0.9610 0.4986 0.1675 0.094 Uiso 1 1 calc R . . C29 C 1.0330(6) 0.5502(3) 0.2245(2) 0.084(2) Uani 1 1 d . . . H29A H 1.0017 0.5828 0.2005 0.101 Uiso 1 1 calc R . . H29B H 1.1252 0.5512 0.2240 0.101 Uiso 1 1 calc R . . C30 C 0.9867(4) 0.55832(19) 0.28115(16) 0.0465(11) Uani 1 1 d . . . H30A H 1.0547 0.5514 0.3079 0.056 Uiso 1 1 calc R . . H30B H 0.9548 0.5996 0.2862 0.056 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.01311(13) 0.01376(13) 0.01146(13) -0.00094(8) 0.00027(9) -0.00054(9) Ru2 0.01853(14) 0.01498(13) 0.01193(13) 0.00093(8) -0.00157(10) 0.00025(9) S1 0.0158(4) 0.0163(3) 0.0156(4) -0.0006(3) -0.0003(3) -0.0015(3) O1 0.038(2) 0.0269(18) 0.0137(16) 0.000 0.000 0.0035(15) O2 0.0190(12) 0.0252(12) 0.0341(13) -0.0077(10) 0.0048(10) -0.0025(9) O3 0.0296(13) 0.0185(11) 0.0249(12) -0.0004(9) 0.0029(10) 0.0055(10) O4 0.0486(17) 0.0352(15) 0.0235(13) 0.0070(11) 0.0036(11) -0.0113(12) O5 0.0448(17) 0.0469(17) 0.0379(16) 0.0006(12) -0.0220(14) -0.0005(13) O6 0.097(3) 0.0434(18) 0.0431(17) -0.0059(14) 0.0231(19) -0.0106(18) N1 0.0168(13) 0.0202(13) 0.0250(14) -0.0084(11) 0.0026(11) -0.0030(10) N2 0.0205(14) 0.0232(14) 0.0242(14) -0.0095(11) 0.0064(11) -0.0064(11) C1 0.0174(15) 0.0223(16) 0.0154(15) -0.0051(12) -0.0004(12) -0.0013(12) C2 0.0266(19) 0.0251(18) 0.039(2) -0.0190(16) 0.0063(16) -0.0097(14) C3 0.0297(19) 0.0280(19) 0.038(2) -0.0210(15) 0.0094(17) -0.0092(15) C4 0.0177(15) 0.0206(15) 0.0263(17) -0.0104(12) 0.0026(14) -0.0082(12) C5 0.0196(16) 0.0220(16) 0.0269(17) -0.0076(13) -0.0027(14) -0.0054(13) C6 0.0174(16) 0.0274(18) 0.0353(19) -0.0097(14) 0.0003(15) -0.0015(14) C7 0.0202(17) 0.0307(19) 0.0310(19) -0.0120(14) 0.0073(15) -0.0049(15) C8 0.0235(18) 0.0264(17) 0.0281(17) -0.0060(14) 0.0093(15) -0.0088(14) C9 0.0231(17) 0.0169(15) 0.0254(17) -0.0059(12) 0.0046(14) -0.0084(13) C10 0.0255(19) 0.033(2) 0.0284(18) -0.0053(15) -0.0036(15) -0.0028(15) C11 0.034(2) 0.058(3) 0.046(2) -0.013(2) 0.018(2) -0.003(2) C12 0.0321(19) 0.0208(17) 0.0329(19) 0.0002(14) 0.0019(16) -0.0038(15) C13 0.0207(17) 0.0219(16) 0.0250(16) -0.0079(13) 0.0090(14) -0.0028(13) C14 0.033(2) 0.0276(18) 0.0209(16) -0.0093(13) 0.0043(15) 0.0023(15) C15 0.041(2) 0.0304(19) 0.0255(18) -0.0065(15) 0.0103(17) 0.0014(16) C16 0.037(2) 0.0230(17) 0.034(2) -0.0062(15) 0.0175(17) -0.0037(15) C17 0.0235(18) 0.0239(17) 0.040(2) -0.0069(15) 0.0119(16) -0.0030(14) C18 0.0258(18) 0.0191(16) 0.0266(17) -0.0098(12) 0.0069(14) -0.0031(13) C19 0.038(2) 0.046(2) 0.0227(18) -0.0103(16) 0.0026(17) 0.0049(18) C20 0.052(3) 0.029(2) 0.061(3) 0.0011(19) 0.034(2) -0.0028(19) C21 0.0252(18) 0.0259(18) 0.0355(19) -0.0001(15) 0.0057(16) 0.0013(14) C22 0.019(2) 0.017(2) 0.020(2) 0.000 0.000 -0.0018(17) C23 0.0209(16) 0.0164(14) 0.0184(15) 0.0001(11) 0.0018(13) 0.0011(12) C24 0.0181(16) 0.0238(16) 0.0139(14) -0.0004(12) -0.0022(12) -0.0030(13) C25 0.0304(18) 0.0234(17) 0.0166(15) -0.0009(13) -0.0036(15) -0.0009(14) C26 0.0273(18) 0.0265(17) 0.0180(15) 0.0030(12) -0.0047(15) 0.0009(14) C27 0.085(4) 0.049(3) 0.043(3) -0.006(2) 0.016(3) -0.022(3) C28 0.135(5) 0.053(3) 0.047(3) -0.017(2) 0.027(3) -0.035(3) C29 0.078(4) 0.097(5) 0.077(4) -0.041(3) 0.027(3) -0.034(3) C30 0.065(3) 0.035(2) 0.040(2) -0.0059(18) -0.007(2) 0.004(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 C23 1.850(3) . ? Ru1 C1 2.062(3) . ? Ru1 C22 2.070(3) . ? Ru1 C24 2.135(3) . ? Ru1 S1 2.4637(8) . ? Ru1 S1 2.5747(8) 2_665 ? Ru1 Ru1 2.7154(5) 2_665 ? Ru1 Ru2 2.7436(3) . ? Ru2 C25 1.857(3) . ? Ru2 C26 1.882(3) . ? Ru2 C24 1.995(3) . ? Ru2 S1 2.4007(8) . ? Ru2 S1 2.4239(8) 2_665 ? Ru2 Ru2 2.7585(5) 2_665 ? S1 Ru2 2.4239(8) 2_665 ? S1 Ru1 2.5747(8) 2_665 ? O1 C22 1.156(5) . ? O2 C23 1.154(4) . ? O3 C24 1.139(4) . ? O4 C25 1.141(4) . ? O5 C26 1.151(4) . ? O6 C27 1.398(5) . ? O6 C30 1.429(5) . ? N1 C2 1.359(4) . ? N1 C1 1.361(4) . ? N1 C4 1.450(4) . ? N2 C3 1.360(4) . ? N2 C1 1.370(4) . ? N2 C13 1.441(4) . ? C2 C3 1.338(5) . ? C4 C5 1.385(5) . ? C4 C9 1.402(4) . ? C5 C6 1.393(5) . ? C5 C10 1.504(5) . ? C6 C7 1.379(5) . ? C7 C8 1.376(5) . ? C7 C11 1.499(5) . ? C8 C9 1.400(5) . ? C9 C12 1.481(5) . ? C13 C14 1.393(5) . ? C13 C18 1.401(5) . ? C14 C15 1.386(5) . ? C14 C19 1.512(5) . ? C15 C16 1.382(5) . ? C16 C17 1.387(5) . ? C16 C20 1.509(5) . ? C17 C18 1.393(5) . ? C18 C21 1.489(5) . ? C22 Ru1 2.070(3) 2_665 ? C27 C28 1.504(7) . ? C28 C29 1.381(7) . ? C29 C30 1.477(7) . ? 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 C23 Ru1 C1 94.41(13) . . ? C23 Ru1 C22 90.78(11) . . ? C1 Ru1 C22 87.96(10) . . ? C23 Ru1 C24 88.66(13) . . ? C1 Ru1 C24 85.53(12) . . ? C22 Ru1 C24 173.40(11) . . ? C23 Ru1 S1 87.51(10) . . ? C1 Ru1 S1 174.82(9) . . ? C22 Ru1 S1 96.84(7) . . ? C24 Ru1 S1 89.71(8) . . ? C23 Ru1 S1 161.74(10) . 2_665 ? C1 Ru1 S1 103.47(9) . 2_665 ? C22 Ru1 S1 93.52(7) . 2_665 ? C24 Ru1 S1 89.04(9) . 2_665 ? S1 Ru1 S1 74.36(3) . 2_665 ? C23 Ru1 Ru1 116.90(9) . 2_665 ? C1 Ru1 Ru1 123.46(9) . 2_665 ? C22 Ru1 Ru1 49.01(8) . 2_665 ? C24 Ru1 Ru1 136.54(8) . 2_665 ? S1 Ru1 Ru1 59.385(19) . 2_665 ? S1 Ru1 Ru1 55.435(18) 2_665 2_665 ? C23 Ru1 Ru2 113.19(10) . . ? C1 Ru1 Ru2 120.29(8) . . ? C22 Ru1 Ru2 139.40(8) . . ? C24 Ru1 Ru2 46.23(8) . . ? S1 Ru1 Ru2 54.588(18) . . ? S1 Ru1 Ru2 54.115(17) 2_665 . ? Ru1 Ru1 Ru2 90.408(6) 2_665 . ? C25 Ru2 C26 92.08(14) . . ? C25 Ru2 C24 97.64(14) . . ? C26 Ru2 C24 97.55(14) . . ? C25 Ru2 S1 165.07(11) . . ? C26 Ru2 S1 94.17(10) . . ? C24 Ru2 S1 94.97(9) . . ? C25 Ru2 S1 92.26(10) . 2_665 ? C26 Ru2 S1 164.32(10) . 2_665 ? C24 Ru2 S1 96.80(9) . 2_665 ? S1 Ru2 S1 78.30(3) . 2_665 ? C25 Ru2 Ru1 127.75(10) . . ? C26 Ru2 Ru1 127.48(10) . . ? C24 Ru2 Ru1 50.58(9) . . ? S1 Ru2 Ru1 56.758(18) . . ? S1 Ru2 Ru1 59.386(18) 2_665 . ? C25 Ru2 Ru2 109.57(11) . 2_665 ? C26 Ru2 Ru2 109.67(10) . 2_665 ? C24 Ru2 Ru2 140.09(9) . 2_665 ? S1 Ru2 Ru2 55.52(2) . 2_665 ? S1 Ru2 Ru2 54.733(19) 2_665 2_665 ? Ru1 Ru2 Ru2 89.508(6) . 2_665 ? Ru2 S1 Ru2 69.74(2) . 2_665 ? Ru2 S1 Ru1 68.65(2) . . ? Ru2 S1 Ru1 104.86(3) 2_665 . ? Ru2 S1 Ru1 102.21(3) . 2_665 ? Ru2 S1 Ru1 66.50(2) 2_665 2_665 ? Ru1 S1 Ru1 65.18(2) . 2_665 ? C27 O6 C30 108.0(3) . . ? C2 N1 C1 111.6(3) . . ? C2 N1 C4 120.4(3) . . ? C1 N1 C4 127.2(3) . . ? C3 N2 C1 110.9(3) . . ? C3 N2 C13 119.1(3) . . ? C1 N2 C13 129.3(3) . . ? N1 C1 N2 103.2(3) . . ? N1 C1 Ru1 126.8(2) . . ? N2 C1 Ru1 129.6(2) . . ? C3 C2 N1 106.9(3) . . ? C2 C3 N2 107.4(3) . . ? C5 C4 C9 122.4(3) . . ? C5 C4 N1 117.8(3) . . ? C9 C4 N1 119.6(3) . . ? C4 C5 C6 117.3(3) . . ? C4 C5 C10 121.3(3) . . ? C6 C5 C10 121.4(3) . . ? C7 C6 C5 122.5(3) . . ? C8 C7 C6 118.1(3) . . ? C8 C7 C11 120.7(3) . . ? C6 C7 C11 121.2(4) . . ? C7 C8 C9 122.5(3) . . ? C8 C9 C4 116.7(3) . . ? C8 C9 C12 122.0(3) . . ? C4 C9 C12 121.2(3) . . ? C14 C13 C18 121.7(3) . . ? C14 C13 N2 118.1(3) . . ? C18 C13 N2 119.6(3) . . ? C15 C14 C13 117.8(3) . . ? C15 C14 C19 120.3(3) . . ? C13 C14 C19 121.6(3) . . ? C16 C15 C14 122.4(3) . . ? C15 C16 C17 118.3(3) . . ? C15 C16 C20 122.1(4) . . ? C17 C16 C20 119.6(4) . . ? C16 C17 C18 122.0(3) . . ? C17 C18 C13 117.6(3) . . ? C17 C18 C21 120.2(3) . . ? C13 C18 C21 122.2(3) . . ? O1 C22 Ru1 139.01(8) . 2_665 ? O1 C22 Ru1 139.01(8) . . ? Ru1 C22 Ru1 81.98(16) 2_665 . ? O2 C23 Ru1 169.4(3) . . ? O3 C24 Ru2 139.7(2) . . ? O3 C24 Ru1 137.1(2) . . ? Ru2 C24 Ru1 83.19(12) . . ? O4 C25 Ru2 177.8(3) . . ? O5 C26 Ru2 176.7(3) . . ? O6 C27 C28 108.0(4) . . ? C29 C28 C27 106.1(4) . . ? C28 C29 C30 107.6(5) . . ? O6 C30 C29 107.3(4) . . ? _diffrn_measured_fraction_theta_max 0.951 _diffrn_reflns_theta_full 30.33 _diffrn_measured_fraction_theta_full 0.951 _refine_diff_density_max 2.744 _refine_diff_density_min -1.203 _refine_diff_density_rms 0.160 _chemical_compound_source THF-Hexane # Attachment 'Compound 4.cif' data_Compound_4.cif _database_code_depnum_ccdc_archive 'CCDC 682716' loop_ _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common '[Ru4(mu4-S)(CO)10(IMes)2]half hexane' _chemical_melting_point '526 dec.' _chemical_formula_moiety 'C55 H55 N4 O10 Ru4 S' _chemical_formula_sum 'C55 H55 N4 O10 Ru4 S' _chemical_formula_weight 1368.37 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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 'P 21/c' _symmetry_int_tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.49940(10) _cell_length_b 11.17230(10) _cell_length_c 47.2989(8) _cell_angle_alpha 90.00 _cell_angle_beta 95.4700(10) _cell_angle_gamma 90.00 _cell_volume 5523.01(12) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.646 _exptl_crystal_density_method none _exptl_crystal_F_000 2740 _exptl_absorpt_coefficient_mu 1.171 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7585 _exptl_absorpt_correction_T_max 0.9122 _exptl_absorpt_process_details 'performed as part of the DENZO-SMN package' _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method 'psi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 48289 _diffrn_reflns_av_R_equivalents 0.0766 _diffrn_reflns_av_sigmaI/netI 0.0656 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -55 _diffrn_reflns_limit_l_max 62 _diffrn_reflns_theta_min 2.24 _diffrn_reflns_theta_max 27.88 _reflns_number_total 12691 _reflns_number_gt 9473 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius Collect' _computing_cell_refinement DENZO-SMN _computing_data_reduction X-Seed _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed / POV-Ray' _computing_publication_material 'Microsoft Office 2000' _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^)+(0.0518P)^2^+2.2337P] 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 12691 _refine_ls_number_parameters 680 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0713 _refine_ls_R_factor_gt 0.0438 _refine_ls_wR_factor_ref 0.1062 _refine_ls_wR_factor_gt 0.0952 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.039 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.61287(3) 0.62814(3) 0.121429(6) 0.01815(8) Uani 1 1 d . . . Ru2 Ru 0.73032(3) 0.83442(3) 0.139664(6) 0.01753(8) Uani 1 1 d . . . Ru3 Ru 0.77619(3) 0.74020(3) 0.086160(6) 0.01689(8) Uani 1 1 d . . . Ru4 Ru 0.74267(3) 0.64033(3) 0.176807(6) 0.01682(8) Uani 1 1 d . . . S1 S 0.83837(8) 0.65014(8) 0.13212(2) 0.0179(2) Uani 1 1 d . . . O1 O 0.5639(3) 0.4216(3) 0.07955(7) 0.0464(9) Uani 1 1 d . . . O2 O 0.3979(3) 0.7872(3) 0.09506(7) 0.0391(8) Uani 1 1 d . . . O3 O 0.4512(2) 0.5014(2) 0.16223(6) 0.0276(6) Uani 1 1 d . . . O4 O 0.6955(3) 1.0295(2) 0.09522(6) 0.0343(7) Uani 1 1 d . . . O5 O 0.8937(3) 0.9979(3) 0.17987(6) 0.0336(7) Uani 1 1 d . . . O6 O 0.4867(3) 0.9216(3) 0.16276(7) 0.0436(8) Uani 1 1 d . . . O7 O 0.8121(3) 0.5190(3) 0.05181(7) 0.0395(8) Uani 1 1 d . . . O8 O 0.5643(3) 0.8281(3) 0.04440(6) 0.0337(7) Uani 1 1 d . . . O9 O 0.5604(3) 0.7450(2) 0.21488(6) 0.0304(7) Uani 1 1 d . . . O10 O 0.9518(3) 0.7562(3) 0.21485(7) 0.0354(7) Uani 1 1 d . . . N1 N 1.0467(3) 0.8585(3) 0.08418(7) 0.0196(7) Uani 1 1 d . . . N2 N 0.9383(3) 0.8815(3) 0.04429(7) 0.0214(7) Uani 1 1 d . . . N3 N 0.8004(3) 0.3646(3) 0.18270(7) 0.0230(7) Uani 1 1 d . . . N4 N 0.7328(3) 0.4307(3) 0.22093(7) 0.0240(7) Uani 1 1 d . . . C1 C 0.9296(3) 0.8339(3) 0.07062(8) 0.0189(8) Uani 1 1 d . . . C2 C 1.1247(4) 0.9192(4) 0.06696(9) 0.0258(9) Uani 1 1 d . . . H2 H 1.2100 0.9451 0.0720 0.031 Uiso 1 1 calc R . . C3 C 1.0564(4) 0.9343(4) 0.04185(9) 0.0289(10) Uani 1 1 d . . . H3 H 1.0834 0.9733 0.0256 0.035 Uiso 1 1 calc R . . C4 C 1.0949(3) 0.8236(3) 0.11271(8) 0.0202(8) Uani 1 1 d . . . C5 C 1.1404(3) 0.7073(4) 0.11725(8) 0.0225(9) Uani 1 1 d . . . C6 C 1.1924(3) 0.6786(4) 0.14462(8) 0.0244(9) Uani 1 1 d . . . H6 H 1.2229 0.5996 0.1484 0.029 Uiso 1 1 calc R . . C7 C 1.2009(3) 0.7609(4) 0.16646(8) 0.0245(9) Uani 1 1 d . . . C8 C 1.1583(4) 0.8771(4) 0.16069(9) 0.0277(9) Uani 1 1 d . . . H8 H 1.1648 0.9347 0.1755 0.033 Uiso 1 1 calc R . . C9 C 1.1063(4) 0.9110(4) 0.13374(9) 0.0249(9) Uani 1 1 d . . . C10 C 1.1378(4) 0.6174(4) 0.09350(9) 0.0275(9) Uani 1 1 d . . . H10A H 1.0564 0.5739 0.0921 0.041 Uiso 1 1 calc R . . H10B H 1.2086 0.5607 0.0973 0.041 Uiso 1 1 calc R . . H10C H 1.1468 0.6590 0.0756 0.041 Uiso 1 1 calc R . . C11 C 1.2546(4) 0.7278(4) 0.19619(9) 0.0362(11) Uani 1 1 d . . . H11A H 1.1843 0.7078 0.2076 0.054 Uiso 1 1 calc R . . H11B H 1.3030 0.7956 0.2049 0.054 Uiso 1 1 calc R . . H11C H 1.3114 0.6585 0.1954 0.054 Uiso 1 1 calc R . . C12 C 1.0680(4) 1.0388(4) 0.12766(9) 0.0335(10) Uani 1 1 d . . . H12A H 1.1299 1.0764 0.1162 0.050 Uiso 1 1 calc R . . H12B H 1.0662 1.0824 0.1456 0.050 Uiso 1 1 calc R . . H12C H 0.9828 1.0408 0.1172 0.050 Uiso 1 1 calc R . . C13 C 0.8446(3) 0.8759(4) 0.01966(8) 0.0222(9) Uani 1 1 d . . . C14 C 0.8457(4) 0.7780(4) 0.00142(8) 0.0281(9) Uani 1 1 d . . . C15 C 0.7582(4) 0.7782(4) -0.02265(9) 0.0333(10) Uani 1 1 d . . . H15 H 0.7574 0.7124 -0.0354 0.040 Uiso 1 1 calc R . . C16 C 0.6718(4) 0.8714(4) -0.02871(10) 0.0357(11) Uani 1 1 d . . . C17 C 0.6762(4) 0.9680(4) -0.01057(9) 0.0311(10) Uani 1 1 d . . . H17 H 0.6185 1.0325 -0.0147 0.037 Uiso 1 1 calc R . . C18 C 0.7627(4) 0.9743(4) 0.01380(9) 0.0265(9) Uani 1 1 d . . . C19 C 0.9436(4) 0.6799(4) 0.00548(10) 0.0375(11) Uani 1 1 d . . . H19A H 1.0112 0.6937 -0.0071 0.056 Uiso 1 1 calc R . . H19B H 0.9025 0.6026 0.0009 0.056 Uiso 1 1 calc R . . H19C H 0.9808 0.6792 0.0253 0.056 Uiso 1 1 calc R . . C20 C 0.5795(5) 0.8673(6) -0.05515(11) 0.0581(16) Uani 1 1 d . . . H20A H 0.5162 0.8041 -0.0532 0.087 Uiso 1 1 calc R . . H20B H 0.6265 0.8506 -0.0716 0.087 Uiso 1 1 calc R . . H20C H 0.5358 0.9446 -0.0577 0.087 Uiso 1 1 calc R . . C21 C 0.7714(4) 1.0833(4) 0.03206(10) 0.0387(11) Uani 1 1 d . . . H21A H 0.8480 1.1290 0.0285 0.058 Uiso 1 1 calc R . . H21B H 0.7767 1.0595 0.0521 0.058 Uiso 1 1 calc R . . H21C H 0.6953 1.1330 0.0276 0.058 Uiso 1 1 calc R . . C22 C 0.7606(3) 0.4678(3) 0.19459(8) 0.0198(8) Uani 1 1 d . . . C23 C 0.7967(4) 0.2685(4) 0.20093(9) 0.0316(10) Uani 1 1 d . . . H23 H 0.8199 0.1883 0.1972 0.038 Uiso 1 1 calc R . . C24 C 0.7545(4) 0.3091(4) 0.22476(9) 0.0342(11) Uani 1 1 d . . . H24 H 0.7418 0.2636 0.2412 0.041 Uiso 1 1 calc R . . C25 C 0.8565(4) 0.3527(3) 0.15597(8) 0.0222(9) Uani 1 1 d . . . C26 C 0.9855(4) 0.3823(3) 0.15553(9) 0.0262(9) Uani 1 1 d . . . C27 C 1.0392(4) 0.3637(3) 0.13010(9) 0.0298(10) Uani 1 1 d . . . H27 H 1.1270 0.3824 0.1292 0.036 Uiso 1 1 calc R . . C28 C 0.9694(4) 0.3191(3) 0.10617(9) 0.0293(10) Uani 1 1 d . . . C29 C 0.8420(4) 0.2874(4) 0.10797(9) 0.0294(10) Uani 1 1 d . . . H29 H 0.7936 0.2561 0.0916 0.035 Uiso 1 1 calc R . . C30 C 0.7841(4) 0.3001(3) 0.13287(9) 0.0258(9) Uani 1 1 d . . . C31 C 1.0625(4) 0.4308(4) 0.18112(9) 0.0319(10) Uani 1 1 d . . . H31A H 1.1537 0.4256 0.1784 0.048 Uiso 1 1 calc R . . H31B H 1.0450 0.3841 0.1979 0.048 Uiso 1 1 calc R . . H31C H 1.0393 0.5147 0.1839 0.048 Uiso 1 1 calc R . . C32 C 1.0307(5) 0.3009(4) 0.07876(10) 0.0407(12) Uani 1 1 d . . . H32A H 1.1222 0.3194 0.0819 0.061 Uiso 1 1 calc R . . H32B H 0.9901 0.3539 0.0641 0.061 Uiso 1 1 calc R . . H32C H 1.0196 0.2174 0.0726 0.061 Uiso 1 1 calc R . . C33 C 0.6490(4) 0.2568(4) 0.13542(10) 0.0326(10) Uani 1 1 d . . . H33A H 0.6078 0.2373 0.1165 0.049 Uiso 1 1 calc R . . H33B H 0.6002 0.3197 0.1440 0.049 Uiso 1 1 calc R . . H33C H 0.6515 0.1851 0.1474 0.049 Uiso 1 1 calc R . . C34 C 0.7053(4) 0.5051(3) 0.24494(8) 0.0265(9) Uani 1 1 d . . . C35 C 0.8068(4) 0.5560(4) 0.26143(9) 0.0292(10) Uani 1 1 d . . . C36 C 0.7784(5) 0.6226(4) 0.28493(9) 0.0347(11) Uani 1 1 d . . . H36 H 0.8458 0.6620 0.2961 0.042 Uiso 1 1 calc R . . C37 C 0.6546(5) 0.6329(4) 0.29239(10) 0.0360(11) Uani 1 1 d . . . C38 C 0.5568(5) 0.5783(4) 0.27588(9) 0.0345(11) Uani 1 1 d . . . H38 H 0.4720 0.5847 0.2811 0.041 Uiso 1 1 calc R . . C39 C 0.5785(4) 0.5138(4) 0.25173(9) 0.0295(10) Uani 1 1 d . . . C40 C 0.9442(4) 0.5339(4) 0.25623(9) 0.0366(11) Uani 1 1 d . . . H40A H 0.9748 0.4610 0.2662 0.055 Uiso 1 1 calc R . . H40B H 0.9967 0.6021 0.2633 0.055 Uiso 1 1 calc R . . H40C H 0.9504 0.5244 0.2358 0.055 Uiso 1 1 calc R . . C41 C 0.6280(6) 0.7014(4) 0.31924(10) 0.0505(14) Uani 1 1 d . . . H41A H 0.5441 0.7402 0.3162 0.076 Uiso 1 1 calc R . . H41B H 0.6943 0.7623 0.3235 0.076 Uiso 1 1 calc R . . H41C H 0.6286 0.6455 0.3352 0.076 Uiso 1 1 calc R . . C42 C 0.4711(4) 0.4518(4) 0.23418(10) 0.0379(11) Uani 1 1 d . . . H42A H 0.3891 0.4769 0.2405 0.057 Uiso 1 1 calc R . . H42B H 0.4806 0.3649 0.2364 0.057 Uiso 1 1 calc R . . H42C H 0.4737 0.4731 0.2141 0.057 Uiso 1 1 calc R . . C43 C 0.5868(4) 0.4965(4) 0.09571(9) 0.0294(10) Uani 1 1 d . . . C44 C 0.4774(4) 0.7264(4) 0.10532(9) 0.0271(9) Uani 1 1 d . . . C45 C 0.5240(4) 0.5537(3) 0.15009(8) 0.0219(8) Uani 1 1 d . . . C46 C 0.7157(4) 0.9437(4) 0.10874(9) 0.0245(9) Uani 1 1 d . . . C47 C 0.8396(4) 0.9330(3) 0.16427(8) 0.0222(8) Uani 1 1 d . . . C48 C 0.5787(4) 0.8869(4) 0.15421(9) 0.0290(10) Uani 1 1 d . . . C49 C 0.7996(4) 0.6046(4) 0.06452(9) 0.0266(9) Uani 1 1 d . . . C50 C 0.6486(4) 0.7966(3) 0.05954(9) 0.0228(9) Uani 1 1 d . . . C51 C 0.6285(4) 0.6988(3) 0.20081(8) 0.0221(8) Uani 1 1 d . . . C52 C 0.8736(4) 0.7077(3) 0.20054(8) 0.0221(8) Uani 1 1 d . . . C53 C 0.4570(9) 0.4926(14) 0.0077(3) 0.205(7) Uani 1 1 d . . . H53A H 0.4892 0.4798 0.0278 0.246 Uiso 1 1 calc R . . H53B H 0.3978 0.4274 0.0010 0.246 Uiso 1 1 calc R . . C54 C 0.3884(7) 0.6397(6) 0.00124(15) 0.082(2) Uani 1 1 d . . . H54A H 0.4553 0.7025 0.0025 0.098 Uiso 1 1 calc R . . H54B H 0.3388 0.6442 -0.0176 0.098 Uiso 1 1 calc R . . C55 C 0.3066(7) 0.6508(8) 0.02383(18) 0.102(3) Uani 1 1 d . . . H55A H 0.2898 0.5713 0.0314 0.154 Uiso 1 1 calc R . . H55B H 0.2256 0.6880 0.0165 0.154 Uiso 1 1 calc R . . H55C H 0.3487 0.7007 0.0390 0.154 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 Ru1 0.01915(15) 0.01967(17) 0.01532(17) 0.00163(13) 0.00002(12) -0.00321(12) Ru2 0.02180(16) 0.01531(16) 0.01520(17) 0.00109(12) 0.00039(12) 0.00058(12) Ru3 0.01948(16) 0.01777(16) 0.01313(17) 0.00153(12) 0.00001(12) -0.00209(12) Ru4 0.02071(15) 0.01628(16) 0.01324(17) 0.00119(12) 0.00048(12) 0.00124(12) S1 0.0197(4) 0.0183(5) 0.0157(5) 0.0011(4) 0.0011(4) 0.0011(4) O1 0.070(2) 0.0350(19) 0.033(2) -0.0086(16) -0.0012(17) -0.0162(17) O2 0.0228(15) 0.055(2) 0.039(2) 0.0222(17) -0.0029(13) 0.0043(15) O3 0.0268(14) 0.0289(16) 0.0277(17) 0.0085(13) 0.0059(12) -0.0046(12) O4 0.062(2) 0.0186(15) 0.0223(17) 0.0055(13) 0.0038(14) 0.0054(14) O5 0.0388(17) 0.0263(16) 0.0327(18) -0.0091(14) -0.0116(14) 0.0003(14) O6 0.0405(18) 0.041(2) 0.051(2) -0.0005(16) 0.0158(16) 0.0139(15) O7 0.058(2) 0.0281(17) 0.0335(19) -0.0135(15) 0.0086(15) -0.0052(15) O8 0.0247(15) 0.0477(19) 0.0268(18) 0.0148(15) -0.0073(13) -0.0035(14) O9 0.0334(16) 0.0316(17) 0.0276(17) 0.0031(13) 0.0101(13) 0.0122(13) O10 0.0361(17) 0.0332(18) 0.0338(19) 0.0007(14) -0.0124(14) -0.0043(14) N1 0.0177(15) 0.0222(17) 0.0186(18) 0.0035(14) 0.0010(13) -0.0027(13) N2 0.0202(16) 0.0296(19) 0.0143(18) 0.0056(14) 0.0018(13) -0.0010(14) N3 0.0350(19) 0.0158(17) 0.0188(19) -0.0019(14) 0.0059(14) 0.0018(14) N4 0.0398(19) 0.0172(17) 0.0155(18) 0.0012(14) 0.0051(14) 0.0060(15) C1 0.0219(19) 0.020(2) 0.014(2) 0.0010(16) -0.0030(15) 0.0032(15) C2 0.0192(19) 0.032(2) 0.026(2) 0.0079(19) 0.0031(16) -0.0050(17) C3 0.024(2) 0.040(3) 0.023(2) 0.010(2) 0.0007(17) -0.0043(19) C4 0.0168(18) 0.028(2) 0.015(2) 0.0036(17) -0.0017(14) -0.0029(16) C5 0.0184(19) 0.027(2) 0.022(2) 0.0010(18) 0.0024(16) -0.0020(16) C6 0.0175(19) 0.028(2) 0.028(2) 0.0096(19) 0.0003(16) 0.0009(16) C7 0.0189(19) 0.035(2) 0.019(2) 0.0005(18) -0.0018(16) -0.0021(17) C8 0.024(2) 0.035(2) 0.024(2) -0.0077(19) 0.0001(17) -0.0039(18) C9 0.024(2) 0.024(2) 0.027(2) 0.0012(18) 0.0021(17) -0.0027(17) C10 0.028(2) 0.029(2) 0.026(2) 0.0015(18) 0.0009(17) 0.0035(18) C11 0.032(2) 0.054(3) 0.021(2) 0.001(2) -0.0045(18) 0.003(2) C12 0.037(2) 0.028(2) 0.034(3) -0.005(2) -0.001(2) -0.0048(19) C13 0.0209(19) 0.031(2) 0.015(2) 0.0074(17) 0.0043(15) -0.0029(16) C14 0.031(2) 0.037(2) 0.016(2) 0.0062(19) 0.0042(17) -0.0003(19) C15 0.039(2) 0.041(3) 0.020(2) 0.001(2) 0.0012(19) -0.007(2) C16 0.027(2) 0.056(3) 0.023(3) 0.016(2) -0.0041(18) -0.009(2) C17 0.020(2) 0.047(3) 0.027(2) 0.022(2) 0.0049(17) 0.0056(19) C18 0.024(2) 0.035(2) 0.022(2) 0.0123(19) 0.0088(16) 0.0009(18) C19 0.047(3) 0.042(3) 0.024(3) 0.002(2) 0.008(2) 0.006(2) C20 0.042(3) 0.088(4) 0.041(3) 0.016(3) -0.014(2) -0.015(3) C21 0.047(3) 0.039(3) 0.032(3) 0.010(2) 0.011(2) 0.017(2) C22 0.0221(19) 0.022(2) 0.014(2) -0.0030(16) -0.0025(15) 0.0023(16) C23 0.054(3) 0.013(2) 0.029(3) 0.0036(18) 0.007(2) 0.0043(19) C24 0.064(3) 0.020(2) 0.020(2) 0.0034(18) 0.008(2) 0.006(2) C25 0.033(2) 0.0147(19) 0.019(2) -0.0003(16) 0.0054(17) 0.0078(16) C26 0.040(2) 0.014(2) 0.026(2) 0.0006(17) 0.0052(18) 0.0092(17) C27 0.034(2) 0.020(2) 0.036(3) 0.0049(19) 0.011(2) 0.0091(18) C28 0.046(3) 0.016(2) 0.028(3) -0.0015(18) 0.013(2) 0.0029(18) C29 0.046(3) 0.021(2) 0.021(2) -0.0026(18) 0.0050(19) 0.0013(19) C30 0.040(2) 0.015(2) 0.023(2) 0.0019(17) 0.0077(18) 0.0053(17) C31 0.036(2) 0.028(2) 0.031(3) 0.000(2) 0.0028(19) 0.0084(19) C32 0.059(3) 0.031(3) 0.036(3) -0.001(2) 0.026(2) 0.001(2) C33 0.044(3) 0.023(2) 0.032(3) -0.0059(19) 0.009(2) -0.0032(19) C34 0.050(3) 0.016(2) 0.014(2) 0.0025(16) 0.0050(18) 0.0039(18) C35 0.050(3) 0.020(2) 0.018(2) 0.0062(18) 0.0035(19) 0.0057(19) C36 0.060(3) 0.024(2) 0.020(2) 0.0001(19) 0.003(2) -0.001(2) C37 0.067(3) 0.020(2) 0.023(3) 0.0025(19) 0.017(2) 0.004(2) C38 0.053(3) 0.027(2) 0.027(3) 0.003(2) 0.017(2) 0.007(2) C39 0.046(3) 0.023(2) 0.020(2) 0.0063(18) 0.0052(19) 0.0020(19) C40 0.048(3) 0.033(3) 0.027(3) 0.003(2) -0.006(2) 0.006(2) C41 0.084(4) 0.037(3) 0.034(3) -0.006(2) 0.024(3) 0.004(3) C42 0.045(3) 0.040(3) 0.029(3) 0.005(2) 0.008(2) -0.004(2) C43 0.034(2) 0.030(2) 0.024(2) 0.004(2) 0.0021(18) -0.0061(19) C44 0.021(2) 0.035(2) 0.026(2) 0.0042(19) 0.0050(17) -0.0098(18) C45 0.027(2) 0.020(2) 0.019(2) -0.0015(17) -0.0021(16) 0.0013(17) C46 0.029(2) 0.022(2) 0.021(2) -0.0023(18) -0.0023(17) -0.0029(17) C47 0.031(2) 0.018(2) 0.017(2) 0.0027(17) -0.0002(16) 0.0024(17) C48 0.037(2) 0.025(2) 0.026(2) 0.0006(19) 0.0076(19) -0.0002(19) C49 0.028(2) 0.031(2) 0.020(2) 0.0053(19) -0.0004(17) -0.0070(18) C50 0.023(2) 0.023(2) 0.023(2) 0.0057(18) 0.0035(17) -0.0048(17) C51 0.028(2) 0.0162(19) 0.021(2) 0.0034(17) -0.0024(17) 0.0021(17) C52 0.028(2) 0.019(2) 0.019(2) 0.0009(17) 0.0000(17) 0.0010(17) C53 0.115(10) 0.309(16) 0.173(13) 0.160(11) -0.074(9) -0.093(11) C54 0.091(5) 0.073(5) 0.073(5) -0.015(4) -0.030(4) 0.015(4) C55 0.079(5) 0.133(7) 0.096(7) -0.005(5) 0.007(5) -0.030(5) _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 C44 1.898(4) . ? Ru1 C45 1.908(4) . ? Ru1 C43 1.912(5) . ? Ru1 S1 2.3862(9) . ? Ru1 Ru2 2.7153(4) . ? Ru1 Ru3 2.7993(4) . ? Ru1 Ru4 2.8383(4) . ? Ru2 C48 1.887(4) . ? Ru2 C46 1.900(4) . ? Ru2 C47 1.905(4) . ? Ru2 S1 2.3938(9) . ? Ru2 Ru4 2.7860(4) . ? Ru2 Ru3 2.8243(4) . ? Ru3 C49 1.858(5) . ? Ru3 C50 1.859(4) . ? Ru3 C1 2.111(4) . ? Ru3 S1 2.4279(10) . ? Ru4 C51 1.847(4) . ? Ru4 C52 1.850(4) . ? Ru4 C22 2.105(4) . ? Ru4 S1 2.4276(10) . ? O1 C43 1.143(5) . ? O2 C44 1.147(5) . ? O3 C45 1.157(4) . ? O4 C46 1.160(5) . ? O5 C47 1.146(4) . ? O6 C48 1.149(5) . ? O7 C49 1.144(5) . ? O8 C50 1.140(5) . ? O9 C51 1.145(4) . ? O10 C52 1.149(5) . ? N1 C1 1.360(5) . ? N1 C2 1.385(5) . ? N1 C4 1.449(5) . ? N2 C1 1.365(5) . ? N2 C3 1.388(5) . ? N2 C13 1.453(5) . ? N3 C22 1.365(5) . ? N3 C23 1.380(5) . ? N3 C25 1.451(5) . ? N4 C22 1.370(5) . ? N4 C24 1.388(5) . ? N4 C34 1.458(5) . ? C2 C3 1.338(5) . ? C4 C9 1.391(6) . ? C4 C5 1.393(5) . ? C5 C6 1.393(5) . ? C5 C10 1.505(6) . ? C6 C7 1.380(6) . ? C7 C8 1.391(6) . ? C7 C11 1.510(5) . ? C8 C9 1.390(6) . ? C9 C12 1.504(6) . ? C13 C14 1.394(6) . ? C13 C18 1.407(5) . ? C14 C15 1.393(6) . ? C14 C19 1.502(6) . ? C15 C16 1.393(6) . ? C16 C17 1.377(7) . ? C16 C20 1.508(6) . ? C17 C18 1.400(6) . ? C18 C21 1.490(6) . ? C23 C24 1.329(6) . ? C25 C26 1.396(6) . ? C25 C30 1.400(6) . ? C26 C27 1.392(6) . ? C26 C31 1.492(6) . ? C27 C28 1.382(6) . ? C28 C29 1.394(6) . ? C28 C32 1.515(5) . ? C29 C30 1.383(5) . ? C30 C33 1.514(6) . ? C34 C35 1.381(6) . ? C34 C39 1.402(6) . ? C35 C36 1.393(6) . ? C35 C40 1.506(6) . ? C36 C37 1.384(6) . ? C37 C38 1.373(7) . ? C37 C41 1.531(6) . ? C38 C39 1.387(6) . ? C39 C42 1.504(6) . ? C53 C53 1.22(2) 3_665 ? C53 C54 1.808(16) . ? C54 C55 1.439(10) . ? 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 C44 Ru1 C45 97.98(16) . . ? C44 Ru1 C43 97.66(18) . . ? C45 Ru1 C43 93.83(16) . . ? C44 Ru1 S1 135.73(12) . . ? C45 Ru1 S1 115.90(12) . . ? C43 Ru1 S1 107.04(13) . . ? C44 Ru1 Ru2 86.38(12) . . ? C45 Ru1 Ru2 112.48(12) . . ? C43 Ru1 Ru2 152.65(12) . . ? S1 Ru1 Ru2 55.52(2) . . ? C44 Ru1 Ru3 88.87(11) . . ? C45 Ru1 Ru3 170.79(12) . . ? C43 Ru1 Ru3 91.34(12) . . ? S1 Ru1 Ru3 55.14(2) . . ? Ru2 Ru1 Ru3 61.592(11) . . ? C44 Ru1 Ru4 128.19(13) . . ? C45 Ru1 Ru4 65.78(12) . . ? C43 Ru1 Ru4 130.63(13) . . ? S1 Ru1 Ru4 54.55(2) . . ? Ru2 Ru1 Ru4 60.169(11) . . ? Ru3 Ru1 Ru4 105.126(13) . . ? C48 Ru2 C46 94.11(17) . . ? C48 Ru2 C47 94.46(17) . . ? C46 Ru2 C47 95.64(16) . . ? C48 Ru2 S1 138.59(13) . . ? C46 Ru2 S1 116.28(12) . . ? C47 Ru2 S1 108.77(12) . . ? C48 Ru2 Ru1 90.36(13) . . ? C46 Ru2 Ru1 107.45(12) . . ? C47 Ru2 Ru1 156.01(11) . . ? S1 Ru2 Ru1 55.25(2) . . ? C48 Ru2 Ru4 90.13(13) . . ? C46 Ru2 Ru4 168.81(12) . . ? C47 Ru2 Ru4 94.35(11) . . ? S1 Ru2 Ru4 55.27(2) . . ? Ru1 Ru2 Ru4 62.105(11) . . ? C48 Ru2 Ru3 131.63(14) . . ? C46 Ru2 Ru3 63.77(12) . . ? C47 Ru2 Ru3 128.20(11) . . ? S1 Ru2 Ru3 54.71(2) . . ? Ru1 Ru2 Ru3 60.667(11) . . ? Ru4 Ru2 Ru3 105.859(13) . . ? C49 Ru3 C50 91.59(18) . . ? C49 Ru3 C1 93.84(15) . . ? C50 Ru3 C1 96.94(15) . . ? C49 Ru3 S1 96.73(13) . . ? C50 Ru3 S1 149.53(11) . . ? C1 Ru3 S1 111.60(10) . . ? C49 Ru3 Ru1 94.85(12) . . ? C50 Ru3 Ru1 96.45(11) . . ? C1 Ru3 Ru1 163.81(10) . . ? S1 Ru3 Ru1 53.75(2) . . ? C49 Ru3 Ru2 147.20(12) . . ? C50 Ru3 Ru2 107.88(12) . . ? C1 Ru3 Ru2 109.16(10) . . ? S1 Ru3 Ru2 53.59(2) . . ? Ru1 Ru3 Ru2 57.741(10) . . ? C51 Ru4 C52 88.36(17) . . ? C51 Ru4 C22 96.74(15) . . ? C52 Ru4 C22 95.57(15) . . ? C51 Ru4 S1 149.97(12) . . ? C52 Ru4 S1 99.47(12) . . ? C22 Ru4 S1 111.13(10) . . ? C51 Ru4 Ru2 96.79(12) . . ? C52 Ru4 Ru2 93.05(12) . . ? C22 Ru4 Ru2 164.14(10) . . ? S1 Ru4 Ru2 54.14(2) . . ? C51 Ru4 Ru1 107.55(12) . . ? C52 Ru4 Ru1 147.48(12) . . ? C22 Ru4 Ru1 109.97(10) . . ? S1 Ru4 Ru1 53.20(2) . . ? Ru2 Ru4 Ru1 57.726(10) . . ? Ru1 S1 Ru2 69.23(3) . . ? Ru1 S1 Ru3 71.10(3) . . ? Ru2 S1 Ru3 71.71(3) . . ? Ru1 S1 Ru4 72.26(3) . . ? Ru2 S1 Ru4 70.59(3) . . ? Ru3 S1 Ru4 134.43(4) . . ? C1 N1 C2 112.3(3) . . ? C1 N1 C4 127.2(3) . . ? C2 N1 C4 120.4(3) . . ? C1 N2 C3 112.2(3) . . ? C1 N2 C13 128.0(3) . . ? C3 N2 C13 119.6(3) . . ? C22 N3 C23 111.8(3) . . ? C22 N3 C25 127.0(3) . . ? C23 N3 C25 120.8(3) . . ? C22 N4 C24 111.6(3) . . ? C22 N4 C34 127.7(3) . . ? C24 N4 C34 119.9(3) . . ? N1 C1 N2 102.5(3) . . ? N1 C1 Ru3 128.5(3) . . ? N2 C1 Ru3 129.0(3) . . ? C3 C2 N1 106.7(3) . . ? C2 C3 N2 106.3(3) . . ? C9 C4 C5 122.6(4) . . ? C9 C4 N1 118.4(3) . . ? C5 C4 N1 118.6(3) . . ? C6 C5 C4 117.1(4) . . ? C6 C5 C10 121.1(4) . . ? C4 C5 C10 121.7(4) . . ? C7 C6 C5 122.3(4) . . ? C6 C7 C8 118.6(4) . . ? C6 C7 C11 121.7(4) . . ? C8 C7 C11 119.7(4) . . ? C9 C8 C7 121.6(4) . . ? C8 C9 C4 117.6(4) . . ? C8 C9 C12 120.6(4) . . ? C4 C9 C12 121.8(4) . . ? C14 C13 C18 122.2(4) . . ? C14 C13 N2 119.0(3) . . ? C18 C13 N2 118.6(4) . . ? C15 C14 C13 117.4(4) . . ? C15 C14 C19 119.7(4) . . ? C13 C14 C19 122.6(4) . . ? C16 C15 C14 122.4(4) . . ? C17 C16 C15 118.4(4) . . ? C17 C16 C20 121.4(5) . . ? C15 C16 C20 120.2(5) . . ? C16 C17 C18 122.2(4) . . ? C17 C18 C13 117.3(4) . . ? C17 C18 C21 121.2(4) . . ? C13 C18 C21 121.4(4) . . ? N3 C22 N4 102.7(3) . . ? N3 C22 Ru4 128.9(3) . . ? N4 C22 Ru4 128.4(3) . . ? C24 C23 N3 107.2(4) . . ? C23 C24 N4 106.7(4) . . ? C26 C25 C30 122.9(4) . . ? C26 C25 N3 117.8(4) . . ? C30 C25 N3 118.9(3) . . ? C27 C26 C25 116.8(4) . . ? C27 C26 C31 121.5(4) . . ? C25 C26 C31 121.7(4) . . ? C28 C27 C26 122.3(4) . . ? C27 C28 C29 118.6(4) . . ? C27 C28 C32 120.9(4) . . ? C29 C28 C32 120.5(4) . . ? C30 C29 C28 121.9(4) . . ? C29 C30 C25 117.2(4) . . ? C29 C30 C33 121.7(4) . . ? C25 C30 C33 121.0(4) . . ? C35 C34 C39 122.7(4) . . ? C35 C34 N4 118.4(4) . . ? C39 C34 N4 118.7(4) . . ? C34 C35 C36 117.3(4) . . ? C34 C35 C40 122.7(4) . . ? C36 C35 C40 119.9(4) . . ? C37 C36 C35 121.7(4) . . ? C38 C37 C36 119.2(4) . . ? C38 C37 C41 120.6(4) . . ? C36 C37 C41 120.2(5) . . ? C37 C38 C39 121.8(4) . . ? C38 C39 C34 117.3(4) . . ? C38 C39 C42 121.3(4) . . ? C34 C39 C42 121.3(4) . . ? O1 C43 Ru1 175.4(4) . . ? O2 C44 Ru1 178.0(3) . . ? O3 C45 Ru1 164.5(3) . . ? O4 C46 Ru2 162.2(3) . . ? O5 C47 Ru2 172.7(3) . . ? O6 C48 Ru2 178.3(4) . . ? O7 C49 Ru3 177.8(4) . . ? O8 C50 Ru3 175.3(3) . . ? O9 C51 Ru4 173.9(3) . . ? O10 C52 Ru4 175.9(4) . . ? C53 C53 C54 94.7(13) 3_665 . ? C55 C54 C53 102.1(7) . . ? _diffrn_measured_fraction_theta_max 0.963 _diffrn_reflns_theta_full 27.88 _diffrn_measured_fraction_theta_full 0.963 _refine_diff_density_max 1.490 _refine_diff_density_min -0.801 _refine_diff_density_rms 0.137 _chemical_compound_source Hexane # Attachment 'Compound 6.cif' data_Compound_6.cif _database_code_depnum_ccdc_archive 'CCDC 682717' loop_ _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common '[Ru3S2(CO)7(IMeMe)2]' _chemical_melting_point 578-583 _chemical_formula_moiety 'C21 H24 N4 O7 Ru3 S2' _chemical_formula_sum 'C21 H24 N4 O7 Ru3 S2' _chemical_formula_weight 811.77 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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 triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_int_tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.8571(3) _cell_length_b 12.0289(4) _cell_length_c 13.4641(6) _cell_angle_alpha 64.0540(10) _cell_angle_beta 69.5140(10) _cell_angle_gamma 63.2560(10) _cell_volume 1386.12(9) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow-orange _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.945 _exptl_crystal_density_method none _exptl_crystal_F_000 796 _exptl_absorpt_coefficient_mu 1.810 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.5313 _exptl_absorpt_correction_T_max 0.6127 _exptl_absorpt_process_details 'performed as part of the DENZO-SMN package' _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method 'psi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21697 _diffrn_reflns_av_R_equivalents 0.0395 _diffrn_reflns_av_sigmaI/netI 0.0526 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.71 _diffrn_reflns_theta_max 27.50 _reflns_number_total 6345 _reflns_number_gt 5082 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius Collect' _computing_cell_refinement DENZO-SMN _computing_data_reduction X-Seed _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed / POV-Ray' _computing_publication_material 'Microsoft Office 2000' _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^)+(0.0960P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6345 _refine_ls_number_parameters 342 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0764 _refine_ls_R_factor_gt 0.0475 _refine_ls_wR_factor_ref 0.1646 _refine_ls_wR_factor_gt 0.1177 _refine_ls_goodness_of_fit_ref 1.209 _refine_ls_restrained_S_all 1.209 _refine_ls_shift/su_max 0.002 _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 Ru1 Ru 0.73492(5) 0.72927(5) 0.72456(4) 0.01952(16) Uani 1 1 d . . . Ru2 Ru 0.88434(5) 0.46123(5) 0.82671(4) 0.01714(15) Uani 1 1 d . . . Ru3 Ru 0.60617(5) 0.61860(5) 0.66434(4) 0.01762(15) Uani 1 1 d . . . S1 S 0.85343(16) 0.56064(14) 0.63651(13) 0.0176(3) Uani 1 1 d . . . S2 S 0.63317(16) 0.56334(15) 0.85235(13) 0.0188(3) Uani 1 1 d . . . O1 O 0.9173(6) 0.8789(5) 0.5379(5) 0.0471(15) Uani 1 1 d . . . O2 O 0.7823(7) 0.7616(6) 0.9196(5) 0.0464(15) Uani 1 1 d . . . O3 O 0.4475(6) 0.9475(5) 0.6950(5) 0.0507(16) Uani 1 1 d . . . O4 O 1.1983(5) 0.3968(5) 0.7699(4) 0.0368(13) Uani 1 1 d . . . O5 O 0.8943(6) 0.4194(5) 1.0633(4) 0.0383(13) Uani 1 1 d . . . O6 O 0.6121(5) 0.7558(5) 0.4134(4) 0.0337(12) Uani 1 1 d . . . O7 O 0.2876(5) 0.7383(6) 0.7118(4) 0.0441(14) Uani 1 1 d . . . N1 N 0.8241(5) 0.2006(5) 0.9467(4) 0.0184(11) Uani 1 1 d . . . N2 N 0.9607(6) 0.2007(5) 0.7867(4) 0.0214(12) Uani 1 1 d . . . N3 N 0.5450(6) 0.3583(5) 0.7659(4) 0.0211(11) Uani 1 1 d . . . N4 N 0.6815(5) 0.3722(5) 0.6038(4) 0.0196(11) Uani 1 1 d . . . C1 C 0.8918(7) 0.2747(6) 0.8559(5) 0.0211(13) Uani 1 1 d . . . C2 C 0.8486(7) 0.0824(6) 0.9350(6) 0.0236(14) Uani 1 1 d . . . C3 C 0.9331(8) 0.0834(6) 0.8353(6) 0.0265(15) Uani 1 1 d . . . C4 C 0.7363(8) 0.2366(7) 1.0448(6) 0.0321(17) Uani 1 1 d . . . H4A H 0.7956 0.2169 1.0953 0.048 Uiso 1 1 calc R . . H4B H 0.6731 0.1861 1.0841 0.048 Uiso 1 1 calc R . . H4C H 0.6808 0.3313 1.0214 0.048 Uiso 1 1 calc R . . C5 C 0.7912(8) -0.0189(6) 1.0224(6) 0.0315(17) Uani 1 1 d . . . H5A H 0.8248 -0.0950 0.9978 0.047 Uiso 1 1 calc R . . H5B H 0.6883 0.0182 1.0351 0.047 Uiso 1 1 calc R . . H5C H 0.8223 -0.0473 1.0926 0.047 Uiso 1 1 calc R . . C6 C 0.9946(9) -0.0148(7) 0.7752(7) 0.039(2) Uani 1 1 d . . . H6A H 0.9718 -0.0943 0.8246 0.059 Uiso 1 1 calc R . . H6B H 1.0969 -0.0382 0.7545 0.059 Uiso 1 1 calc R . . H6C H 0.9554 0.0239 0.7070 0.059 Uiso 1 1 calc R . . C7 C 1.0527(8) 0.2332(7) 0.6792(6) 0.0301(16) Uani 1 1 d . . . H7A H 1.0075 0.2526 0.6190 0.045 Uiso 1 1 calc R . . H7B H 1.1413 0.1582 0.6779 0.045 Uiso 1 1 calc R . . H7C H 1.0715 0.3107 0.6677 0.045 Uiso 1 1 calc R . . C8 C 0.6093(7) 0.4387(6) 0.6782(5) 0.0193(13) Uani 1 1 d . . . C9 C 0.5749(7) 0.2449(6) 0.7453(6) 0.0249(15) Uani 1 1 d . . . C10 C 0.6615(7) 0.2532(6) 0.6433(6) 0.0225(14) Uani 1 1 d . . . C11 C 0.4529(8) 0.3846(7) 0.8668(6) 0.0311(16) Uani 1 1 d . . . H11A H 0.4916 0.3148 0.9328 0.047 Uiso 1 1 calc R . . H11B H 0.3598 0.3867 0.8716 0.047 Uiso 1 1 calc R . . H11C H 0.4450 0.4700 0.8646 0.047 Uiso 1 1 calc R . . C12 C 0.5180(8) 0.1401(7) 0.8255(6) 0.0326(17) Uani 1 1 d . . . H12A H 0.5497 0.0704 0.7934 0.049 Uiso 1 1 calc R . . H12B H 0.4152 0.1776 0.8400 0.049 Uiso 1 1 calc R . . H12C H 0.5515 0.1027 0.8961 0.049 Uiso 1 1 calc R . . C13 C 0.7231(7) 0.1614(7) 0.5778(6) 0.0301(16) Uani 1 1 d . . . H13A H 0.8258 0.1297 0.5656 0.045 Uiso 1 1 calc R . . H13B H 0.6931 0.2081 0.5049 0.045 Uiso 1 1 calc R . . H13C H 0.6909 0.0861 0.6196 0.045 Uiso 1 1 calc R . . C14 C 0.7644(7) 0.4204(7) 0.4918(5) 0.0285(15) Uani 1 1 d . . . H14A H 0.7025 0.4737 0.4366 0.043 Uiso 1 1 calc R . . H14B H 0.8375 0.3449 0.4701 0.043 Uiso 1 1 calc R . . H14C H 0.8082 0.4745 0.4942 0.043 Uiso 1 1 calc R . . C15 C 0.8470(8) 0.8250(6) 0.6089(6) 0.0302(16) Uani 1 1 d . . . C16 C 0.7702(8) 0.7457(7) 0.8467(6) 0.0324(17) Uani 1 1 d . . . C17 C 0.5557(8) 0.8639(7) 0.6998(6) 0.0323(17) Uani 1 1 d . . . C18 C 1.0806(7) 0.4207(6) 0.7898(5) 0.0230(14) Uani 1 1 d . . . C19 C 0.8899(7) 0.4319(6) 0.9755(6) 0.0255(15) Uani 1 1 d . . . C20 C 0.6089(7) 0.7007(6) 0.5077(6) 0.0240(14) Uani 1 1 d . . . C21 C 0.4072(8) 0.6927(7) 0.6947(6) 0.0283(16) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.0231(3) 0.0141(3) 0.0229(3) -0.0089(2) 0.0014(2) -0.0096(2) Ru2 0.0187(3) 0.0163(3) 0.0177(3) -0.0067(2) -0.0005(2) -0.0085(2) Ru3 0.0179(3) 0.0164(3) 0.0189(3) -0.0077(2) -0.0004(2) -0.0069(2) S1 0.0198(8) 0.0155(7) 0.0173(7) -0.0066(6) 0.0008(6) -0.0084(6) S2 0.0197(8) 0.0190(8) 0.0187(8) -0.0094(6) 0.0029(6) -0.0097(6) O1 0.054(4) 0.032(3) 0.050(3) -0.022(3) 0.024(3) -0.029(3) O2 0.068(4) 0.058(4) 0.037(3) -0.030(3) 0.002(3) -0.038(3) O3 0.038(3) 0.023(3) 0.080(5) -0.018(3) -0.011(3) -0.001(3) O4 0.019(3) 0.057(3) 0.032(3) -0.016(3) 0.000(2) -0.014(2) O5 0.039(3) 0.061(4) 0.027(3) -0.020(3) -0.001(2) -0.028(3) O6 0.036(3) 0.032(3) 0.023(3) 0.001(2) -0.006(2) -0.013(2) O7 0.019(3) 0.061(4) 0.038(3) -0.024(3) -0.002(2) 0.002(3) N1 0.021(3) 0.019(3) 0.016(3) -0.003(2) -0.004(2) -0.011(2) N2 0.025(3) 0.015(3) 0.023(3) -0.005(2) -0.009(2) -0.003(2) N3 0.027(3) 0.023(3) 0.020(3) -0.008(2) -0.003(2) -0.014(2) N4 0.020(3) 0.018(3) 0.022(3) -0.008(2) -0.002(2) -0.007(2) C1 0.021(3) 0.021(3) 0.020(3) -0.005(3) -0.005(3) -0.007(3) C2 0.025(4) 0.022(3) 0.026(4) -0.004(3) -0.012(3) -0.009(3) C3 0.036(4) 0.013(3) 0.032(4) -0.005(3) -0.019(3) -0.003(3) C4 0.036(4) 0.026(4) 0.026(4) -0.007(3) 0.004(3) -0.015(3) C5 0.043(4) 0.017(3) 0.039(4) 0.003(3) -0.018(4) -0.018(3) C6 0.062(6) 0.016(4) 0.039(4) -0.009(3) -0.021(4) -0.005(3) C7 0.032(4) 0.026(4) 0.025(4) -0.011(3) 0.002(3) -0.007(3) C8 0.022(3) 0.019(3) 0.018(3) -0.006(3) -0.004(3) -0.008(3) C9 0.027(4) 0.023(3) 0.032(4) -0.003(3) -0.013(3) -0.015(3) C10 0.021(3) 0.019(3) 0.033(4) -0.012(3) -0.009(3) -0.005(3) C11 0.045(5) 0.038(4) 0.022(4) -0.010(3) 0.000(3) -0.030(4) C12 0.041(4) 0.026(4) 0.033(4) 0.000(3) -0.009(3) -0.022(3) C13 0.029(4) 0.023(4) 0.044(4) -0.018(3) -0.007(3) -0.007(3) C14 0.034(4) 0.028(4) 0.023(3) -0.012(3) 0.002(3) -0.013(3) C15 0.038(4) 0.018(3) 0.035(4) -0.017(3) 0.006(3) -0.013(3) C16 0.041(5) 0.025(4) 0.032(4) -0.010(3) 0.005(3) -0.022(3) C17 0.039(5) 0.017(4) 0.037(4) -0.006(3) -0.003(3) -0.014(3) C18 0.032(4) 0.025(3) 0.013(3) -0.003(3) -0.003(3) -0.015(3) C19 0.022(4) 0.026(4) 0.031(4) -0.010(3) -0.002(3) -0.013(3) C20 0.020(3) 0.020(3) 0.035(4) -0.012(3) -0.004(3) -0.007(3) C21 0.034(4) 0.026(4) 0.024(4) -0.008(3) -0.005(3) -0.010(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 C15 1.897(7) . ? Ru1 C17 1.915(8) . ? Ru1 C16 1.918(8) . ? Ru1 S2 2.4111(16) . ? Ru1 S1 2.4213(16) . ? Ru1 Ru3 2.7920(7) . ? Ru1 Ru2 2.8094(7) . ? Ru2 C18 1.887(7) . ? Ru2 C19 1.894(7) . ? Ru2 C1 2.069(6) . ? Ru2 S1 2.3793(16) . ? Ru2 S2 2.4004(17) . ? Ru3 C20 1.893(7) . ? Ru3 C21 1.897(8) . ? Ru3 C8 2.075(6) . ? Ru3 S1 2.3818(16) . ? Ru3 S2 2.4098(16) . ? O1 C15 1.144(8) . ? O2 C16 1.139(9) . ? O3 C17 1.152(9) . ? O4 C18 1.134(8) . ? O5 C19 1.140(8) . ? O6 C20 1.144(8) . ? O7 C21 1.140(9) . ? N1 C1 1.355(8) . ? N1 C2 1.393(8) . ? N1 C4 1.445(8) . ? N2 C1 1.364(8) . ? N2 C3 1.395(9) . ? N2 C7 1.445(9) . ? N3 C8 1.359(8) . ? N3 C9 1.383(8) . ? N3 C11 1.445(8) . ? N4 C8 1.358(8) . ? N4 C10 1.383(8) . ? N4 C14 1.475(8) . ? C2 C3 1.334(10) . ? C2 C5 1.475(9) . ? C3 C6 1.497(9) . ? C9 C10 1.357(10) . ? C9 C12 1.476(9) . ? C10 C13 1.489(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C15 Ru1 C17 97.3(3) . . ? C15 Ru1 C16 95.9(3) . . ? C17 Ru1 C16 104.1(3) . . ? C15 Ru1 S2 165.4(2) . . ? C17 Ru1 S2 93.0(2) . . ? C16 Ru1 S2 91.5(2) . . ? C15 Ru1 S1 87.4(2) . . ? C17 Ru1 S1 123.6(2) . . ? C16 Ru1 S1 131.4(2) . . ? S2 Ru1 S1 78.33(5) . . ? C15 Ru1 Ru3 118.3(2) . . ? C17 Ru1 Ru3 75.8(2) . . ? C16 Ru1 Ru3 145.7(2) . . ? S2 Ru1 Ru3 54.59(4) . . ? S1 Ru1 Ru3 53.80(4) . . ? C15 Ru1 Ru2 114.5(2) . . ? C17 Ru1 Ru2 147.0(2) . . ? C16 Ru1 Ru2 82.0(2) . . ? S2 Ru1 Ru2 54.10(4) . . ? S1 Ru1 Ru2 53.49(4) . . ? Ru3 Ru1 Ru2 81.384(19) . . ? C18 Ru2 C19 88.6(3) . . ? C18 Ru2 C1 96.1(3) . . ? C19 Ru2 C1 96.6(3) . . ? C18 Ru2 S1 94.73(19) . . ? C19 Ru2 S1 164.0(2) . . ? C1 Ru2 S1 98.56(18) . . ? C18 Ru2 S2 167.0(2) . . ? C19 Ru2 S2 94.1(2) . . ? C1 Ru2 S2 96.18(18) . . ? S1 Ru2 S2 79.36(5) . . ? C18 Ru2 Ru1 112.74(19) . . ? C19 Ru2 Ru1 109.5(2) . . ? C1 Ru2 Ru1 140.83(17) . . ? S1 Ru2 Ru1 54.88(4) . . ? S2 Ru2 Ru1 54.45(4) . . ? C20 Ru3 C21 90.6(3) . . ? C20 Ru3 C8 97.1(3) . . ? C21 Ru3 C8 93.7(3) . . ? C20 Ru3 S1 91.8(2) . . ? C21 Ru3 S1 168.3(2) . . ? C8 Ru3 S1 97.29(18) . . ? C20 Ru3 S2 162.4(2) . . ? C21 Ru3 S2 95.4(2) . . ? C8 Ru3 S2 98.95(17) . . ? S1 Ru3 S2 79.12(5) . . ? C20 Ru3 Ru1 107.8(2) . . ? C21 Ru3 Ru1 113.3(2) . . ? C8 Ru3 Ru1 142.28(17) . . ? S1 Ru3 Ru1 55.12(4) . . ? S2 Ru3 Ru1 54.63(4) . . ? Ru2 S1 Ru3 100.18(6) . . ? Ru2 S1 Ru1 71.63(5) . . ? Ru3 S1 Ru1 71.08(4) . . ? Ru2 S2 Ru3 98.79(6) . . ? Ru2 S2 Ru1 71.45(5) . . ? Ru3 S2 Ru1 70.78(5) . . ? C1 N1 C2 111.7(5) . . ? C1 N1 C4 125.4(5) . . ? C2 N1 C4 122.8(5) . . ? C1 N2 C3 110.2(6) . . ? C1 N2 C7 126.8(6) . . ? C3 N2 C7 123.0(6) . . ? C8 N3 C9 110.8(5) . . ? C8 N3 C11 126.8(5) . . ? C9 N3 C11 122.4(5) . . ? C8 N4 C10 111.2(5) . . ? C8 N4 C14 126.0(5) . . ? C10 N4 C14 122.7(5) . . ? N1 C1 N2 104.2(5) . . ? N1 C1 Ru2 127.6(5) . . ? N2 C1 Ru2 128.1(5) . . ? C3 C2 N1 106.0(6) . . ? C3 C2 C5 130.6(7) . . ? N1 C2 C5 123.4(6) . . ? C2 C3 N2 107.8(6) . . ? C2 C3 C6 131.3(7) . . ? N2 C3 C6 120.9(7) . . ? N4 C8 N3 104.7(5) . . ? N4 C8 Ru3 127.6(5) . . ? N3 C8 Ru3 127.7(4) . . ? C10 C9 N3 107.0(6) . . ? C10 C9 C12 130.2(6) . . ? N3 C9 C12 122.9(6) . . ? C9 C10 N4 106.4(6) . . ? C9 C10 C13 130.3(6) . . ? N4 C10 C13 123.3(6) . . ? O1 C15 Ru1 177.6(6) . . ? O2 C16 Ru1 175.4(7) . . ? O3 C17 Ru1 172.6(7) . . ? O4 C18 Ru2 178.4(6) . . ? O5 C19 Ru2 177.0(6) . . ? O6 C20 Ru3 176.1(6) . . ? O7 C21 Ru3 179.3(7) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.359 _refine_diff_density_min -2.355 _refine_diff_density_rms 0.547 _chemical_compound_source THF-Hexane # Attachment 'Compound 7.cif' data_Compound_7.cif _database_code_depnum_ccdc_archive 'CCDC 682718' loop_ _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common '[{Ru(mu-Cl)(CO)2(IMes)}2]' _chemical_melting_point '566 (dec. 573)' _chemical_formula_moiety 'C46 H48 Cl2 N4 O4 Ru2' _chemical_formula_sum 'C46 H48 Cl2 N4 O4 Ru2' _chemical_formula_weight 993.92 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_int_tables_number 14 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 15.5442(5) _cell_length_b 14.3837(4) _cell_length_c 20.5832(6) _cell_angle_alpha 90.00 _cell_angle_beta 101.2570(10) _cell_angle_gamma 90.00 _cell_volume 4513.5(2) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.463 _exptl_crystal_density_method none _exptl_crystal_F_000 2024 _exptl_absorpt_coefficient_mu 0.833 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7881 _exptl_absorpt_correction_T_max 0.8994 _exptl_absorpt_process_details 'Bruker Scalepack' _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker X8 Apex' _diffrn_measurement_method 'psi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 59697 _diffrn_reflns_av_R_equivalents 0.0319 _diffrn_reflns_av_sigmaI/netI 0.0344 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 2.02 _diffrn_reflns_theta_max 30.08 _reflns_number_total 13205 _reflns_number_gt 11911 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker AXS Collect Software' _computing_cell_refinement 'Bruker Scalepack' _computing_data_reduction X-Seed _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed / POV-Ray' _computing_publication_material 'Microsoft Office 2000' _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^)+(0.0183P)^2^+3.3751P] 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 13205 _refine_ls_number_parameters 535 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0370 _refine_ls_R_factor_gt 0.0315 _refine_ls_wR_factor_ref 0.0666 _refine_ls_wR_factor_gt 0.0632 _refine_ls_goodness_of_fit_ref 1.114 _refine_ls_restrained_S_all 1.114 _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 Ru1 Ru 0.183047(9) 0.089913(10) 0.276309(7) 0.01373(4) Uani 1 1 d . . . Ru2 Ru 0.285834(9) 0.231111(10) 0.317935(7) 0.01371(4) Uani 1 1 d . . . Cl1 Cl 0.21507(3) 0.21267(3) 0.20100(2) 0.02044(9) Uani 1 1 d . . . Cl2 Cl 0.34505(3) 0.07689(3) 0.29253(2) 0.01916(9) Uani 1 1 d . . . O1 O 0.00014(10) 0.15700(12) 0.27083(9) 0.0408(4) Uani 1 1 d . . . O2 O 0.17643(11) 0.02280(11) 0.41284(7) 0.0330(4) Uani 1 1 d . . . O3 O 0.15156(10) 0.36976(11) 0.33998(8) 0.0352(4) Uani 1 1 d . . . O4 O 0.31365(10) 0.18843(11) 0.46243(7) 0.0282(3) Uani 1 1 d . . . N1 N 0.13997(10) -0.11893(10) 0.23334(7) 0.0175(3) Uani 1 1 d . . . N2 N 0.12480(10) -0.03362(10) 0.14724(7) 0.0178(3) Uani 1 1 d . . . N3 N 0.39791(11) 0.39479(11) 0.27184(8) 0.0219(3) Uani 1 1 d . . . N4 N 0.47713(10) 0.31818(11) 0.35035(8) 0.0202(3) Uani 1 1 d . . . C1 C 0.14760(11) -0.02883(12) 0.21445(8) 0.0152(3) Uani 1 1 d . . . C2 C 0.11272(14) -0.17685(14) 0.17956(10) 0.0254(4) Uani 1 1 d . . . H2 H 0.1028 -0.2419 0.1808 0.030 Uiso 1 1 calc R . . C3 C 0.10301(14) -0.12308(14) 0.12542(10) 0.0250(4) Uani 1 1 d . . . H3 H 0.0847 -0.1426 0.0808 0.030 Uiso 1 1 calc R . . C4 C 0.15766(13) -0.15390(12) 0.30021(9) 0.0184(4) Uani 1 1 d . . . C5 C 0.09097(13) -0.15232(13) 0.33676(10) 0.0206(4) Uani 1 1 d . . . C6 C 0.11195(14) -0.18522(14) 0.40171(10) 0.0252(4) Uani 1 1 d . . . H6 H 0.0690 -0.1819 0.4287 0.030 Uiso 1 1 calc R . . C7 C 0.19334(14) -0.22255(15) 0.42813(10) 0.0277(4) Uani 1 1 d . . . C8 C 0.25606(14) -0.22633(14) 0.38862(11) 0.0263(4) Uani 1 1 d . . . H8 H 0.3114 -0.2538 0.4058 0.032 Uiso 1 1 calc R . . C9 C 0.24018(13) -0.19103(13) 0.32469(10) 0.0224(4) Uani 1 1 d . . . C10 C 0.00131(13) -0.11486(16) 0.30887(11) 0.0285(4) Uani 1 1 d . . . H10A H 0.0019 -0.0470 0.3129 0.043 Uiso 1 1 calc R . . H10B H -0.0411 -0.1410 0.3334 0.043 Uiso 1 1 calc R . . H10C H -0.0154 -0.1322 0.2621 0.043 Uiso 1 1 calc R . . C11 C 0.21508(17) -0.2581(2) 0.49870(12) 0.0427(6) Uani 1 1 d . . . H11A H 0.2089 -0.3260 0.4987 0.064 Uiso 1 1 calc R . . H11B H 0.1749 -0.2303 0.5244 0.064 Uiso 1 1 calc R . . H11C H 0.2755 -0.2412 0.5186 0.064 Uiso 1 1 calc R . . C12 C 0.31065(15) -0.19092(16) 0.28386(12) 0.0324(5) Uani 1 1 d . . . H12A H 0.3628 -0.2228 0.3082 0.049 Uiso 1 1 calc R . . H12B H 0.3258 -0.1267 0.2749 0.049 Uiso 1 1 calc R . . H12C H 0.2893 -0.2232 0.2419 0.049 Uiso 1 1 calc R . . C13 C 0.11593(12) 0.04343(12) 0.10150(8) 0.0168(3) Uani 1 1 d . . . C14 C 0.18854(12) 0.07157(13) 0.07590(9) 0.0188(4) Uani 1 1 d . . . C15 C 0.17756(13) 0.14513(14) 0.03104(9) 0.0213(4) Uani 1 1 d . . . H15 H 0.2262 0.1654 0.0131 0.026 Uiso 1 1 calc R . . C16 C 0.09730(13) 0.18950(13) 0.01192(9) 0.0198(4) Uani 1 1 d . . . C17 C 0.02681(12) 0.15770(13) 0.03800(9) 0.0188(4) Uani 1 1 d . . . H17 H -0.0284 0.1874 0.0248 0.023 Uiso 1 1 calc R . . C18 C 0.03372(12) 0.08420(13) 0.08260(9) 0.0183(4) Uani 1 1 d . . . C19 C 0.27655(13) 0.02573(15) 0.09786(10) 0.0254(4) Uani 1 1 d . . . H19A H 0.2992 0.0401 0.1446 0.038 Uiso 1 1 calc R . . H19B H 0.3175 0.0490 0.0710 0.038 Uiso 1 1 calc R . . H19C H 0.2702 -0.0417 0.0923 0.038 Uiso 1 1 calc R . . C20 C 0.08633(15) 0.27025(15) -0.03576(11) 0.0288(5) Uani 1 1 d . . . H20A H 0.1412 0.3056 -0.0298 0.043 Uiso 1 1 calc R . . H20B H 0.0391 0.3107 -0.0271 0.043 Uiso 1 1 calc R . . H20C H 0.0716 0.2469 -0.0813 0.043 Uiso 1 1 calc R . . C21 C -0.04543(13) 0.05050(15) 0.10782(11) 0.0266(4) Uani 1 1 d . . . H21A H -0.0730 -0.0007 0.0799 0.040 Uiso 1 1 calc R . . H21B H -0.0874 0.1016 0.1064 0.040 Uiso 1 1 calc R . . H21C H -0.0273 0.0286 0.1535 0.040 Uiso 1 1 calc R . . C22 C 0.07076(13) 0.13141(14) 0.27257(10) 0.0244(4) Uani 1 1 d . . . C23 C 0.17939(13) 0.04353(13) 0.35925(9) 0.0204(4) Uani 1 1 d . . . C24 C 0.39455(12) 0.32089(12) 0.31240(9) 0.0175(3) Uani 1 1 d . . . C25 C 0.48080(14) 0.43575(16) 0.28358(12) 0.0341(5) Uani 1 1 d . . . H25 H 0.4988 0.4877 0.2610 0.041 Uiso 1 1 calc R . . C26 C 0.52999(14) 0.38757(15) 0.33280(12) 0.0316(5) Uani 1 1 d . . . H26 H 0.5898 0.3988 0.3520 0.038 Uiso 1 1 calc R . . C27 C 0.32587(13) 0.42897(14) 0.22273(10) 0.0222(4) Uani 1 1 d . . . C28 C 0.27063(14) 0.49597(14) 0.24090(11) 0.0261(4) Uani 1 1 d . . . C29 C 0.20192(15) 0.52754(15) 0.19154(12) 0.0324(5) Uani 1 1 d . . . H29 H 0.1622 0.5723 0.2027 0.039 Uiso 1 1 calc R . . C30 C 0.18991(15) 0.49568(17) 0.12691(12) 0.0346(5) Uani 1 1 d . . . C31 C 0.24835(14) 0.43095(16) 0.11081(11) 0.0314(5) Uani 1 1 d . . . H31 H 0.2411 0.4098 0.0664 0.038 Uiso 1 1 calc R . . C32 C 0.31698(13) 0.39624(14) 0.15773(10) 0.0250(4) Uani 1 1 d . . . C33 C 0.28563(18) 0.53582(16) 0.30968(12) 0.0385(6) Uani 1 1 d . . . H33A H 0.2965 0.4852 0.3421 0.058 Uiso 1 1 calc R . . H33B H 0.2336 0.5708 0.3156 0.058 Uiso 1 1 calc R . . H33C H 0.3365 0.5774 0.3161 0.058 Uiso 1 1 calc R . . C34 C 0.11404(18) 0.5305(2) 0.07491(14) 0.0521(7) Uani 1 1 d . . . H34A H 0.0679 0.4831 0.0667 0.078 Uiso 1 1 calc R . . H34B H 0.1346 0.5434 0.0337 0.078 Uiso 1 1 calc R . . H34C H 0.0905 0.5877 0.0906 0.078 Uiso 1 1 calc R . . C35 C 0.37997(15) 0.32593(18) 0.13947(11) 0.0350(5) Uani 1 1 d . . . H35A H 0.3645 0.3130 0.0919 0.053 Uiso 1 1 calc R . . H35B H 0.3766 0.2684 0.1643 0.053 Uiso 1 1 calc R . . H35C H 0.4398 0.3507 0.1503 0.053 Uiso 1 1 calc R . . C36 C 0.50921(12) 0.25173(13) 0.40157(10) 0.0195(4) Uani 1 1 d . . . C37 C 0.49975(13) 0.27027(14) 0.46628(10) 0.0237(4) Uani 1 1 d . . . C38 C 0.52970(14) 0.20351(18) 0.51410(11) 0.0343(5) Uani 1 1 d . . . H38 H 0.5228 0.2142 0.5583 0.041 Uiso 1 1 calc R . . C39 C 0.56901(15) 0.12253(18) 0.49963(13) 0.0401(6) Uani 1 1 d . . . C40 C 0.58086(14) 0.10863(15) 0.43561(14) 0.0381(6) Uani 1 1 d . . . H40 H 0.6101 0.0540 0.4257 0.046 Uiso 1 1 calc R . . C41 C 0.55130(13) 0.17208(14) 0.38500(11) 0.0266(4) Uani 1 1 d . . . C42 C 0.45853(16) 0.35939(17) 0.48353(12) 0.0372(5) Uani 1 1 d . . . H42A H 0.4522 0.3574 0.5300 0.056 Uiso 1 1 calc R . . H42B H 0.4007 0.3668 0.4549 0.056 Uiso 1 1 calc R . . H42C H 0.4959 0.4120 0.4769 0.056 Uiso 1 1 calc R . . C43 C 0.5997(2) 0.0502(2) 0.55275(18) 0.0685(11) Uani 1 1 d . . . H43A H 0.6016 -0.0109 0.5320 0.103 Uiso 1 1 calc R . . H43B H 0.5589 0.0482 0.5835 0.103 Uiso 1 1 calc R . . H43C H 0.6584 0.0666 0.5770 0.103 Uiso 1 1 calc R . . C44 C 0.56497(16) 0.15685(18) 0.31567(13) 0.0422(6) Uani 1 1 d . . . H44A H 0.5079 0.1515 0.2856 0.063 Uiso 1 1 calc R . . H44B H 0.5985 0.0995 0.3139 0.063 Uiso 1 1 calc R . . H44C H 0.5974 0.2095 0.3022 0.063 Uiso 1 1 calc R . . C45 C 0.20490(13) 0.31793(14) 0.33136(10) 0.0225(4) Uani 1 1 d . . . C46 C 0.30616(12) 0.20613(13) 0.40721(9) 0.0191(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.01359(7) 0.01311(7) 0.01420(7) -0.00038(5) 0.00204(5) -0.00112(5) Ru2 0.01360(7) 0.01317(7) 0.01389(7) -0.00051(5) 0.00155(5) -0.00104(5) Cl1 0.0262(2) 0.0181(2) 0.01511(19) 0.00201(16) -0.00078(17) -0.00383(18) Cl2 0.01590(19) 0.0175(2) 0.0236(2) -0.00134(16) 0.00269(16) 0.00106(16) O1 0.0213(8) 0.0372(9) 0.0650(12) -0.0075(8) 0.0108(8) 0.0061(7) O2 0.0509(10) 0.0303(8) 0.0193(7) -0.0016(6) 0.0105(7) -0.0136(7) O3 0.0319(8) 0.0313(8) 0.0434(10) -0.0032(7) 0.0099(7) 0.0112(7) O4 0.0276(8) 0.0392(9) 0.0172(7) 0.0019(6) 0.0030(6) -0.0052(7) N1 0.0215(8) 0.0148(7) 0.0157(7) -0.0009(6) 0.0022(6) -0.0028(6) N2 0.0218(8) 0.0161(7) 0.0144(7) 0.0002(6) 0.0007(6) -0.0013(6) N3 0.0198(8) 0.0207(8) 0.0237(8) 0.0060(6) 0.0006(7) -0.0055(7) N4 0.0180(8) 0.0185(8) 0.0225(8) 0.0014(6) 0.0001(6) -0.0036(6) C1 0.0131(8) 0.0176(8) 0.0145(8) 0.0010(6) 0.0017(6) -0.0009(7) C2 0.0369(12) 0.0156(9) 0.0228(10) -0.0039(7) 0.0037(8) -0.0054(8) C3 0.0376(12) 0.0184(9) 0.0178(9) -0.0047(7) 0.0027(8) -0.0039(8) C4 0.0228(9) 0.0141(8) 0.0175(8) 0.0016(7) 0.0020(7) -0.0029(7) C5 0.0212(9) 0.0168(9) 0.0237(9) 0.0005(7) 0.0037(7) -0.0052(7) C6 0.0283(10) 0.0265(10) 0.0217(9) 0.0033(8) 0.0072(8) -0.0090(9) C7 0.0303(11) 0.0267(10) 0.0235(10) 0.0065(8) -0.0014(8) -0.0130(9) C8 0.0217(10) 0.0231(10) 0.0300(11) 0.0066(8) -0.0052(8) -0.0021(8) C9 0.0221(9) 0.0193(9) 0.0250(10) 0.0025(7) 0.0028(8) -0.0006(8) C10 0.0196(10) 0.0315(11) 0.0347(12) 0.0051(9) 0.0059(9) -0.0018(9) C11 0.0402(14) 0.0567(16) 0.0269(12) 0.0168(11) -0.0043(10) -0.0191(12) C12 0.0266(11) 0.0348(12) 0.0379(12) 0.0029(10) 0.0113(9) 0.0087(9) C13 0.0199(9) 0.0158(8) 0.0136(8) -0.0005(6) 0.0007(7) -0.0008(7) C14 0.0175(8) 0.0225(9) 0.0154(8) -0.0005(7) 0.0008(7) 0.0014(7) C15 0.0204(9) 0.0261(10) 0.0184(9) 0.0014(7) 0.0063(7) -0.0004(8) C16 0.0226(9) 0.0205(9) 0.0158(8) 0.0016(7) 0.0026(7) 0.0029(8) C17 0.0175(8) 0.0209(9) 0.0165(8) -0.0019(7) -0.0005(7) 0.0031(7) C18 0.0174(8) 0.0215(9) 0.0154(8) -0.0027(7) 0.0015(7) -0.0022(7) C19 0.0207(9) 0.0308(11) 0.0247(10) 0.0051(8) 0.0046(8) 0.0062(8) C20 0.0309(11) 0.0290(11) 0.0270(11) 0.0103(9) 0.0066(9) 0.0039(9) C21 0.0188(9) 0.0325(11) 0.0287(11) 0.0042(9) 0.0048(8) -0.0010(8) C22 0.0230(10) 0.0191(9) 0.0315(11) -0.0027(8) 0.0060(8) -0.0012(8) C23 0.0235(9) 0.0165(9) 0.0218(9) -0.0036(7) 0.0057(8) -0.0044(7) C24 0.0183(9) 0.0167(8) 0.0174(8) -0.0015(7) 0.0032(7) 0.0004(7) C25 0.0243(11) 0.0304(11) 0.0443(13) 0.0140(10) -0.0014(10) -0.0133(9) C26 0.0218(10) 0.0289(11) 0.0409(13) 0.0074(9) -0.0019(9) -0.0122(9) C27 0.0206(9) 0.0203(9) 0.0239(10) 0.0090(7) 0.0004(8) -0.0045(8) C28 0.0284(10) 0.0197(9) 0.0307(11) 0.0059(8) 0.0072(9) -0.0041(8) C29 0.0275(11) 0.0234(10) 0.0467(14) 0.0127(10) 0.0084(10) 0.0030(9) C30 0.0276(11) 0.0370(12) 0.0368(12) 0.0192(10) 0.0009(10) -0.0013(10) C31 0.0290(11) 0.0396(12) 0.0240(10) 0.0101(9) 0.0016(9) -0.0041(10) C32 0.0221(10) 0.0280(10) 0.0253(10) 0.0069(8) 0.0055(8) -0.0047(8) C33 0.0490(15) 0.0240(11) 0.0431(14) -0.0023(10) 0.0106(12) -0.0015(10) C34 0.0376(14) 0.0663(19) 0.0472(16) 0.0273(14) -0.0046(12) 0.0079(14) C35 0.0313(12) 0.0466(14) 0.0290(11) 0.0003(10) 0.0103(9) 0.0005(11) C36 0.0138(8) 0.0171(8) 0.0262(10) 0.0018(7) 0.0000(7) -0.0024(7) C37 0.0166(9) 0.0292(10) 0.0238(10) -0.0012(8) -0.0001(8) -0.0038(8) C38 0.0203(10) 0.0513(14) 0.0271(11) 0.0116(10) -0.0057(8) -0.0110(10) C39 0.0209(10) 0.0379(13) 0.0533(16) 0.0209(12) -0.0133(10) -0.0096(10) C40 0.0152(9) 0.0188(10) 0.0750(19) 0.0017(11) -0.0042(11) 0.0003(8) C41 0.0148(9) 0.0222(10) 0.0426(12) -0.0048(9) 0.0050(8) -0.0032(8) C42 0.0345(12) 0.0417(14) 0.0351(12) -0.0167(10) 0.0064(10) -0.0014(11) C43 0.0504(17) 0.0506(17) 0.085(2) 0.0403(17) -0.0340(16) -0.0191(15) C44 0.0320(12) 0.0421(14) 0.0580(16) -0.0256(12) 0.0226(12) -0.0118(11) C45 0.0231(10) 0.0221(9) 0.0215(9) -0.0010(7) 0.0024(8) -0.0022(8) C46 0.0172(8) 0.0189(9) 0.0210(9) -0.0024(7) 0.0030(7) -0.0022(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 C22 1.832(2) . ? Ru1 C23 1.8442(19) . ? Ru1 C1 2.1373(18) . ? Ru1 Cl1 2.4636(5) . ? Ru1 Cl2 2.4819(5) . ? Ru1 Ru2 2.6224(2) . ? Ru2 C45 1.831(2) . ? Ru2 C46 1.8381(19) . ? Ru2 C24 2.1474(18) . ? Ru2 Cl1 2.4576(5) . ? Ru2 Cl2 2.4959(5) . ? O1 C22 1.152(2) . ? O2 C23 1.152(2) . ? O3 C45 1.154(2) . ? O4 C46 1.148(2) . ? N1 C1 1.365(2) . ? N1 C2 1.384(2) . ? N1 C4 1.441(2) . ? N2 C1 1.361(2) . ? N2 C3 1.383(2) . ? N2 C13 1.443(2) . ? N3 C24 1.359(2) . ? N3 C25 1.394(3) . ? N3 C27 1.441(2) . ? N4 C24 1.367(2) . ? N4 C26 1.385(2) . ? N4 C36 1.438(2) . ? C2 C3 1.340(3) . ? C4 C9 1.390(3) . ? C4 C5 1.395(3) . ? C5 C6 1.395(3) . ? C5 C10 1.500(3) . ? C6 C7 1.384(3) . ? C7 C8 1.387(3) . ? C7 C11 1.515(3) . ? C8 C9 1.387(3) . ? C9 C12 1.505(3) . ? C13 C18 1.391(3) . ? C13 C14 1.396(3) . ? C14 C15 1.393(3) . ? C14 C19 1.506(3) . ? C15 C16 1.388(3) . ? C16 C17 1.388(3) . ? C16 C20 1.509(3) . ? C17 C18 1.391(3) . ? C18 C21 1.506(3) . ? C25 C26 1.338(3) . ? C27 C28 1.390(3) . ? C27 C32 1.399(3) . ? C28 C29 1.398(3) . ? C28 C33 1.503(3) . ? C29 C30 1.385(3) . ? C30 C31 1.385(3) . ? C30 C34 1.515(3) . ? C31 C32 1.385(3) . ? C32 C35 1.505(3) . ? C36 C41 1.394(3) . ? C36 C37 1.394(3) . ? C37 C38 1.389(3) . ? C37 C42 1.506(3) . ? C38 C39 1.375(4) . ? C39 C40 1.380(4) . ? C39 C43 1.517(3) . ? C40 C41 1.394(3) . ? C41 C44 1.499(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C22 Ru1 C23 87.45(9) . . ? C22 Ru1 C1 95.89(8) . . ? C23 Ru1 C1 102.21(7) . . ? C22 Ru1 Cl1 92.74(6) . . ? C23 Ru1 Cl1 152.66(6) . . ? C1 Ru1 Cl1 104.96(5) . . ? C22 Ru1 Cl2 164.49(6) . . ? C23 Ru1 Cl2 93.55(6) . . ? C1 Ru1 Cl2 99.01(5) . . ? Cl1 Ru1 Cl2 79.305(16) . . ? C22 Ru1 Ru2 106.03(6) . . ? C23 Ru1 Ru2 96.01(6) . . ? C1 Ru1 Ru2 152.04(4) . . ? Cl1 Ru1 Ru2 57.689(11) . . ? Cl2 Ru1 Ru2 58.469(11) . . ? C45 Ru2 C46 88.37(8) . . ? C45 Ru2 C24 99.72(8) . . ? C46 Ru2 C24 100.78(8) . . ? C45 Ru2 Cl1 91.83(6) . . ? C46 Ru2 Cl1 156.16(6) . . ? C24 Ru2 Cl1 102.67(5) . . ? C45 Ru2 Cl2 158.42(6) . . ? C46 Ru2 Cl2 92.14(6) . . ? C24 Ru2 Cl2 101.37(5) . . ? Cl1 Ru2 Cl2 79.149(16) . . ? C45 Ru2 Ru1 100.64(6) . . ? C46 Ru2 Ru1 98.63(6) . . ? C24 Ru2 Ru1 152.12(5) . . ? Cl1 Ru2 Ru1 57.911(11) . . ? Cl2 Ru2 Ru1 57.950(11) . . ? Ru2 Cl1 Ru1 64.400(12) . . ? Ru1 Cl2 Ru2 63.581(11) . . ? C1 N1 C2 111.94(15) . . ? C1 N1 C4 126.36(15) . . ? C2 N1 C4 121.70(15) . . ? C1 N2 C3 112.07(15) . . ? C1 N2 C13 126.64(15) . . ? C3 N2 C13 121.10(15) . . ? C24 N3 C25 111.66(17) . . ? C24 N3 C27 125.47(16) . . ? C25 N3 C27 122.87(16) . . ? C24 N4 C26 111.67(16) . . ? C24 N4 C36 126.19(15) . . ? C26 N4 C36 122.12(16) . . ? N2 C1 N1 102.81(15) . . ? N2 C1 Ru1 129.17(13) . . ? N1 C1 Ru1 128.00(12) . . ? C3 C2 N1 106.54(17) . . ? C2 C3 N2 106.63(17) . . ? C9 C4 C5 122.76(17) . . ? C9 C4 N1 118.11(16) . . ? C5 C4 N1 119.09(17) . . ? C4 C5 C6 116.86(18) . . ? C4 C5 C10 122.16(17) . . ? C6 C5 C10 120.96(18) . . ? C7 C6 C5 122.19(19) . . ? C6 C7 C8 118.56(19) . . ? C6 C7 C11 121.6(2) . . ? C8 C7 C11 119.9(2) . . ? C9 C8 C7 121.77(19) . . ? C8 C9 C4 117.74(18) . . ? C8 C9 C12 121.06(19) . . ? C4 C9 C12 121.18(18) . . ? C18 C13 C14 122.60(17) . . ? C18 C13 N2 118.15(16) . . ? C14 C13 N2 119.19(16) . . ? C15 C14 C13 117.85(17) . . ? C15 C14 C19 121.20(17) . . ? C13 C14 C19 120.92(17) . . ? C16 C15 C14 121.62(17) . . ? C15 C16 C17 118.19(17) . . ? C15 C16 C20 121.31(17) . . ? C17 C16 C20 120.50(17) . . ? C16 C17 C18 122.72(17) . . ? C17 C18 C13 116.98(17) . . ? C17 C18 C21 120.62(17) . . ? C13 C18 C21 122.40(17) . . ? O1 C22 Ru1 179.3(2) . . ? O2 C23 Ru1 173.77(17) . . ? N3 C24 N4 103.24(15) . . ? N3 C24 Ru2 128.90(14) . . ? N4 C24 Ru2 127.85(13) . . ? C26 C25 N3 106.53(18) . . ? C25 C26 N4 106.88(18) . . ? C28 C27 C32 122.67(19) . . ? C28 C27 N3 118.96(18) . . ? C32 C27 N3 118.31(18) . . ? C27 C28 C29 117.0(2) . . ? C27 C28 C33 121.8(2) . . ? C29 C28 C33 121.1(2) . . ? C30 C29 C28 122.1(2) . . ? C29 C30 C31 118.7(2) . . ? C29 C30 C34 120.6(2) . . ? C31 C30 C34 120.6(2) . . ? C32 C31 C30 121.8(2) . . ? C31 C32 C27 117.7(2) . . ? C31 C32 C35 121.2(2) . . ? C27 C32 C35 121.14(19) . . ? C41 C36 C37 122.21(19) . . ? C41 C36 N4 118.61(18) . . ? C37 C36 N4 119.15(17) . . ? C38 C37 C36 117.5(2) . . ? C38 C37 C42 121.4(2) . . ? C36 C37 C42 121.14(19) . . ? C39 C38 C37 122.3(2) . . ? C38 C39 C40 118.5(2) . . ? C38 C39 C43 121.0(3) . . ? C40 C39 C43 120.5(3) . . ? C39 C40 C41 122.2(2) . . ? C40 C41 C36 117.2(2) . . ? C40 C41 C44 121.9(2) . . ? C36 C41 C44 120.9(2) . . ? O3 C45 Ru2 177.24(18) . . ? O4 C46 Ru2 175.76(17) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 30.08 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.616 _refine_diff_density_min -0.626 _refine_diff_density_rms 0.082 _chemical_compound_source THF-Hexane