# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Jin, Guo-Xin' _publ_contact_author_email gxjin@fudan.edu.cn _publ_section_title ; Synthesis and Structural Characterization of Binuclear Half-Sandwich Iridium, Rhodium and Ruthenium Complexes Containing 4,4'-Dipyridyldisulfide (4DPDS) Ligands ; _publ_author_name 'Guo-Xin Jin' # Attachment '- Complex 2a.cif' data_Complex_2a _database_code_depnum_ccdc_archive 'CCDC 767811' #TrackingRef '- Complex 2a.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H48 Cl4 Ir2 N2 O S2' _chemical_formula_weight 1091.06 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' S S 0.1246 0.1234 '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' Ir Ir -1.4442 7.9887 '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 Tetragonal _symmetry_space_group_name_H-M P4(2)2(1)2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-y+1/2, x+1/2, z+1/2' 'y+1/2, -x+1/2, z+1/2' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z+1/2' 'y, x, -z' '-y, -x, -z' _cell_length_a 14.994(5) _cell_length_b 14.994(5) _cell_length_c 18.752(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4216(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 871 _cell_measurement_theta_min 2.900 _cell_measurement_theta_max 21.355 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.719 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2112 _exptl_absorpt_coefficient_mu 6.686 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5009 _exptl_absorpt_correction_T_max 0.6168 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 5.35 _diffrn_reflns_number 20444 _diffrn_reflns_av_R_equivalents 0.0600 _diffrn_reflns_av_sigmaI/netI 0.0805 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.92 _diffrn_reflns_theta_max 27.09 _reflns_number_total 4611 _reflns_number_gt 2751 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0273P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.009(10) _refine_ls_number_reflns 4611 _refine_ls_number_parameters 204 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0607 _refine_ls_R_factor_gt 0.0302 _refine_ls_wR_factor_ref 0.0654 _refine_ls_wR_factor_gt 0.0619 _refine_ls_goodness_of_fit_ref 0.804 _refine_ls_restrained_S_all 0.807 _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 Ir1 Ir 0.625785(17) 0.710185(16) 0.24784(2) 0.05273(10) Uani 1 1 d . . . Cl1 Cl 0.50502(13) 0.64544(15) 0.18153(11) 0.0665(6) Uani 1 1 d . . . Cl2 Cl 0.51944(14) 0.77005(14) 0.33195(12) 0.0727(6) Uani 1 1 d . . . N1 N 0.6243(4) 0.5937(4) 0.3150(3) 0.0459(14) Uani 1 1 d . . . S1 S 0.62220(14) 0.34196(13) 0.44933(10) 0.0573(5) Uani 1 1 d . . . C1 C 0.6372(5) 0.5997(5) 0.3841(4) 0.055(2) Uani 1 1 d . . . H1 H 0.6457 0.6561 0.4037 0.066 Uiso 1 1 calc R . . C2 C 0.6389(5) 0.5290(5) 0.4282(4) 0.058(2) Uani 1 1 d . . . H2 H 0.6496 0.5368 0.4767 0.070 Uiso 1 1 calc R . . C3 C 0.6243(4) 0.4430(5) 0.4003(3) 0.0435(17) Uani 1 1 d . . . C4 C 0.6101(4) 0.4366(4) 0.3281(4) 0.0437(17) Uani 1 1 d . . . H4 H 0.6000 0.3815 0.3069 0.052 Uiso 1 1 calc R . . C5 C 0.6111(4) 0.5112(5) 0.2887(4) 0.0464(18) Uani 1 1 d . . . H5 H 0.6021 0.5055 0.2398 0.056 Uiso 1 1 calc R . . C6 C 0.6745(6) 0.8358(5) 0.2090(5) 0.068(2) Uani 1 1 d . . . C7 C 0.7284(5) 0.8081(5) 0.2656(5) 0.068(3) Uani 1 1 d . . . C8 C 0.7700(5) 0.7254(5) 0.2464(6) 0.0607(18) Uani 1 1 d . . . C9 C 0.7399(6) 0.7018(6) 0.1779(5) 0.064(2) Uani 1 1 d . . . C10 C 0.6817(6) 0.7718(6) 0.1551(4) 0.066(2) Uani 1 1 d . . . C11 C 0.6204(7) 0.9219(5) 0.2076(5) 0.112(4) Uani 1 1 d . . . H11A H 0.5836 0.9249 0.2494 0.168 Uiso 1 1 calc R . . H11B H 0.5834 0.9228 0.1658 0.168 Uiso 1 1 calc R . . H11C H 0.6601 0.9720 0.2067 0.168 Uiso 1 1 calc R . . C12 C 0.7443(7) 0.8568(7) 0.3380(6) 0.122(4) Uani 1 1 d . . . H12A H 0.7972 0.8927 0.3347 0.184 Uiso 1 1 calc R . . H12B H 0.7515 0.8135 0.3753 0.184 Uiso 1 1 calc R . . H12C H 0.6941 0.8943 0.3486 0.184 Uiso 1 1 calc R . . C13 C 0.8335(7) 0.6717(7) 0.2912(5) 0.107(4) Uani 1 1 d . . . H13A H 0.8848 0.6561 0.2633 0.161 Uiso 1 1 calc R . . H13B H 0.8043 0.6183 0.3073 0.161 Uiso 1 1 calc R . . H13C H 0.8518 0.7063 0.3317 0.161 Uiso 1 1 calc R . . C14 C 0.7725(7) 0.6272(6) 0.1366(5) 0.108(4) Uani 1 1 d . . . H14A H 0.7233 0.5903 0.1225 0.162 Uiso 1 1 calc R . . H14B H 0.8132 0.5929 0.1651 0.162 Uiso 1 1 calc R . . H14C H 0.8028 0.6489 0.0950 0.162 Uiso 1 1 calc R . . C15 C 0.6366(7) 0.7786(7) 0.0831(5) 0.123(4) Uani 1 1 d . . . H15A H 0.6014 0.7262 0.0749 0.184 Uiso 1 1 calc R . . H15B H 0.6811 0.7837 0.0465 0.184 Uiso 1 1 calc R . . H15C H 0.5988 0.8303 0.0823 0.184 Uiso 1 1 calc R . . O1 O 0.5000 0.0000 0.0115(9) 0.283(10) Uani 1 2 d SD . . C16 C 0.606(2) 0.1190(17) 0.0185(14) 0.404(19) Uiso 1 1 d D . . H16A H 0.6596 0.1406 -0.0033 0.606 Uiso 1 1 calc R . . H16B H 0.6172 0.1058 0.0678 0.606 Uiso 1 1 calc R . . H16C H 0.5603 0.1637 0.0151 0.606 Uiso 1 1 calc R . . C17 C 0.5751(13) 0.0341(14) -0.0198(11) 0.44(2) Uani 1 1 d D . . H17A H 0.5628 0.0477 -0.0694 0.532 Uiso 1 1 calc R . . H17B H 0.6223 -0.0101 -0.0183 0.532 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 Ir1 0.05722(17) 0.04091(14) 0.06006(17) 0.0048(3) 0.0084(3) -0.00784(12) Cl1 0.0653(13) 0.0687(15) 0.0656(13) 0.0124(11) -0.0044(11) -0.0147(10) Cl2 0.0736(16) 0.0616(15) 0.0829(15) -0.0094(12) 0.0209(12) -0.0011(11) N1 0.052(4) 0.040(3) 0.045(4) 0.001(3) 0.006(3) -0.009(3) S1 0.0775(15) 0.0492(11) 0.0451(11) 0.0024(9) 0.0063(11) 0.0124(11) C1 0.073(6) 0.049(5) 0.041(5) -0.003(4) 0.000(4) -0.014(4) C2 0.088(6) 0.055(5) 0.032(4) -0.003(4) -0.003(4) -0.004(5) C3 0.040(4) 0.056(5) 0.034(4) -0.001(3) 0.006(3) 0.003(4) C4 0.048(5) 0.031(4) 0.051(5) 0.000(3) 0.002(4) 0.001(3) C5 0.039(4) 0.058(5) 0.042(4) -0.003(4) 0.000(3) -0.008(4) C6 0.069(6) 0.037(5) 0.099(7) 0.017(5) 0.013(5) -0.008(5) C7 0.062(6) 0.055(6) 0.086(8) 0.000(5) 0.016(5) -0.021(4) C8 0.058(5) 0.053(5) 0.071(5) 0.017(8) 0.002(7) -0.016(3) C9 0.070(6) 0.051(6) 0.070(6) 0.012(5) 0.025(5) -0.013(5) C10 0.072(6) 0.064(6) 0.062(6) 0.024(5) 0.022(5) -0.023(5) C11 0.120(9) 0.039(5) 0.177(10) 0.017(6) 0.023(7) 0.004(6) C12 0.126(10) 0.113(10) 0.129(10) -0.034(8) 0.033(7) -0.065(8) C13 0.076(7) 0.108(8) 0.138(9) 0.045(7) 0.006(6) -0.027(7) C14 0.124(9) 0.085(8) 0.116(8) -0.005(7) 0.056(7) 0.006(7) C15 0.114(10) 0.145(11) 0.109(9) 0.055(8) -0.006(7) -0.045(8) O1 0.202(19) 0.51(4) 0.140(14) 0.000 0.000 -0.03(2) C17 0.51(5) 0.43(5) 0.39(3) 0.22(4) 0.38(3) 0.17(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ir1 C10 2.140(7) . ? Ir1 C6 2.148(8) . ? Ir1 C7 2.153(8) . ? Ir1 N1 2.153(5) . ? Ir1 C9 2.160(8) . ? Ir1 C8 2.175(7) . ? Ir1 Cl1 2.401(2) . ? Ir1 Cl2 2.416(2) . ? N1 C1 1.314(7) . ? N1 C5 1.346(8) . ? S1 C3 1.773(7) . ? S1 S1 2.047(4) 8_666 ? C1 C2 1.346(9) . ? C2 C3 1.408(9) . ? C3 C4 1.374(8) . ? C4 C5 1.340(9) . ? C6 C10 1.397(10) . ? C6 C7 1.398(11) . ? C6 C11 1.524(11) . ? C7 C8 1.435(10) . ? C7 C12 1.560(12) . ? C8 C9 1.408(12) . ? C8 C13 1.503(11) . ? C9 C10 1.429(11) . ? C9 C14 1.445(11) . ? C10 C15 1.513(12) . ? O1 C17 1.369(9) 2_655 ? O1 C17 1.369(9) . ? C16 C17 1.533(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 C10 Ir1 C6 38.0(3) . . ? C10 Ir1 C7 63.4(3) . . ? C6 Ir1 C7 37.9(3) . . ? C10 Ir1 N1 146.0(3) . . ? C6 Ir1 N1 156.0(3) . . ? C7 Ir1 N1 118.0(3) . . ? C10 Ir1 C9 38.8(3) . . ? C6 Ir1 C9 64.9(3) . . ? C7 Ir1 C9 64.4(3) . . ? N1 Ir1 C9 108.4(3) . . ? C10 Ir1 C8 63.6(4) . . ? C6 Ir1 C8 64.3(3) . . ? C7 Ir1 C8 38.7(3) . . ? N1 Ir1 C8 95.9(3) . . ? C9 Ir1 C8 37.9(3) . . ? C10 Ir1 Cl1 92.8(2) . . ? C6 Ir1 Cl1 115.8(3) . . ? C7 Ir1 Cl1 153.5(3) . . ? N1 Ir1 Cl1 88.11(16) . . ? C9 Ir1 Cl1 105.0(3) . . ? C8 Ir1 Cl1 141.8(3) . . ? C10 Ir1 Cl2 129.0(3) . . ? C6 Ir1 Cl2 96.9(2) . . ? C7 Ir1 Cl2 96.7(2) . . ? N1 Ir1 Cl2 85.01(16) . . ? C9 Ir1 Cl2 160.2(2) . . ? C8 Ir1 Cl2 128.7(3) . . ? Cl1 Ir1 Cl2 89.46(8) . . ? C1 N1 C5 116.5(6) . . ? C1 N1 Ir1 121.3(5) . . ? C5 N1 Ir1 122.2(4) . . ? C3 S1 S1 104.6(2) . 8_666 ? N1 C1 C2 123.7(7) . . ? C1 C2 C3 119.3(6) . . ? C4 C3 C2 117.0(6) . . ? C4 C3 S1 116.7(5) . . ? C2 C3 S1 126.3(5) . . ? C5 C4 C3 118.9(6) . . ? C4 C5 N1 124.5(6) . . ? C10 C6 C7 107.5(7) . . ? C10 C6 C11 127.7(9) . . ? C7 C6 C11 124.8(9) . . ? C10 C6 Ir1 70.7(4) . . ? C7 C6 Ir1 71.2(5) . . ? C11 C6 Ir1 124.5(6) . . ? C6 C7 C8 108.5(9) . . ? C6 C7 C12 127.7(9) . . ? C8 C7 C12 123.8(10) . . ? C6 C7 Ir1 70.8(5) . . ? C8 C7 Ir1 71.5(4) . . ? C12 C7 Ir1 124.3(5) . . ? C9 C8 C7 107.8(8) . . ? C9 C8 C13 125.4(8) . . ? C7 C8 C13 126.7(10) . . ? C9 C8 Ir1 70.5(5) . . ? C7 C8 Ir1 69.8(4) . . ? C13 C8 Ir1 124.5(6) . . ? C8 C9 C10 106.5(8) . . ? C8 C9 C14 125.0(9) . . ? C10 C9 C14 128.0(9) . . ? C8 C9 Ir1 71.6(4) . . ? C10 C9 Ir1 69.8(4) . . ? C14 C9 Ir1 129.7(6) . . ? C6 C10 C9 109.6(8) . . ? C6 C10 C15 124.3(9) . . ? C9 C10 C15 126.1(9) . . ? C6 C10 Ir1 71.3(4) . . ? C9 C10 Ir1 71.3(4) . . ? C15 C10 Ir1 125.4(6) . . ? C17 O1 C17 129(3) 2_655 . ? O1 C17 C16 110.9(17) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.09 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.795 _refine_diff_density_min -0.341 _refine_diff_density_rms 0.132 # Attachment '- Complex 2c.cif' data_Complex_2c _database_code_depnum_ccdc_archive 'CCDC 767812' #TrackingRef '- Complex 2c.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H40 Cl8 N2 Ru2 S2' _chemical_formula_weight 1002.52 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' S S 0.1246 0.1234 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 40.54(3) _cell_length_b 10.141(7) _cell_length_c 26.817(19) _cell_angle_alpha 90.00 _cell_angle_beta 128.862(7) _cell_angle_gamma 90.00 _cell_volume 8584(11) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1013 _cell_measurement_theta_min 2.790 _cell_measurement_theta_max 26.445 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.552 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4016 _exptl_absorpt_coefficient_mu 1.323 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7777 _exptl_absorpt_correction_T_max 0.8790 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 8.03 _diffrn_reflns_number 19975 _diffrn_reflns_av_R_equivalents 0.0403 _diffrn_reflns_av_sigmaI/netI 0.0419 _diffrn_reflns_limit_h_min -51 _diffrn_reflns_limit_h_max 44 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 1.29 _diffrn_reflns_theta_max 27.10 _reflns_number_total 9126 _reflns_number_gt 6637 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0652P)^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 9126 _refine_ls_number_parameters 421 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0582 _refine_ls_R_factor_gt 0.0404 _refine_ls_wR_factor_ref 0.1124 _refine_ls_wR_factor_gt 0.1054 _refine_ls_goodness_of_fit_ref 0.977 _refine_ls_restrained_S_all 0.982 _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 0.197031(8) -0.04887(3) -0.015433(12) 0.04039(9) Uani 1 1 d . . . Ru2 Ru 0.419651(8) 0.46928(3) 0.378640(13) 0.04772(10) Uani 1 1 d . . . N1 N 0.19425(9) 0.1010(3) 0.03776(13) 0.0417(6) Uani 1 1 d . . . N2 N 0.35286(9) 0.5046(3) 0.31141(13) 0.0471(7) Uani 1 1 d . . . S1 S 0.18014(3) 0.41083(11) 0.14652(4) 0.0517(2) Uani 1 1 d . . . S2 S 0.21166(3) 0.57446(10) 0.15315(4) 0.0512(2) Uani 1 1 d . . . Cl1 Cl 0.26505(3) 0.04148(9) 0.02664(4) 0.0486(2) Uani 1 1 d . . . Cl2 Cl 0.23211(3) -0.17996(10) 0.08038(4) 0.0566(2) Uani 1 1 d . . . Cl3 Cl 0.42566(3) 0.70194(12) 0.40206(5) 0.0679(3) Uani 1 1 d . . . Cl4 Cl 0.40842(3) 0.43443(12) 0.45541(4) 0.0652(3) Uani 1 1 d . . . C1 C 0.20602(11) 0.2264(4) 0.03965(16) 0.0459(8) Uani 1 1 d . . . H1 H 0.2169 0.2468 0.0188 0.055 Uiso 1 1 calc R . . C2 C 0.20256(11) 0.3253(4) 0.07110(17) 0.0489(8) Uani 1 1 d . . . H2 H 0.2111 0.4107 0.0715 0.059 Uiso 1 1 calc R . . C3 C 0.18622(10) 0.2966(4) 0.10221(16) 0.0449(8) Uani 1 1 d . . . C4 C 0.17293(11) 0.1702(4) 0.09884(17) 0.0513(9) Uani 1 1 d . . . H4 H 0.1608 0.1489 0.1179 0.062 Uiso 1 1 calc R . . C5 C 0.17756(12) 0.0756(4) 0.06719(18) 0.0514(9) Uani 1 1 d . . . H5 H 0.1688 -0.0100 0.0660 0.062 Uiso 1 1 calc R . . C6 C 0.33730(11) 0.6092(4) 0.27210(16) 0.0515(9) Uani 1 1 d . . . H6 H 0.3563 0.6701 0.2769 0.062 Uiso 1 1 calc R . . C7 C 0.29471(11) 0.6309(4) 0.22507(16) 0.0492(8) Uani 1 1 d . . . H7 H 0.2853 0.7053 0.1992 0.059 Uiso 1 1 calc R . . C8 C 0.26592(11) 0.5406(4) 0.21664(15) 0.0437(8) Uani 1 1 d . . . C9 C 0.28162(11) 0.4329(4) 0.25740(18) 0.0527(9) Uani 1 1 d . . . H9 H 0.2633 0.3709 0.2536 0.063 Uiso 1 1 calc R . . C10 C 0.32467(11) 0.4191(4) 0.30347(18) 0.0542(9) Uani 1 1 d . . . H10 H 0.3348 0.3465 0.3306 0.065 Uiso 1 1 calc R . . C11 C 0.15157(11) -0.2121(4) -0.06873(17) 0.0501(9) Uani 1 1 d . . . C12 C 0.18214(12) -0.2123(4) -0.07944(17) 0.0530(9) Uani 1 1 d . . . H12 H 0.1972 -0.2890 -0.0722 0.064 Uiso 1 1 calc R . . C13 C 0.18943(13) -0.0996(4) -0.10052(17) 0.0590(10) Uani 1 1 d . . . H13 H 0.2093 -0.1024 -0.1072 0.071 Uiso 1 1 calc R . . C14 C 0.16723(12) 0.0208(5) -0.11229(17) 0.0608(11) Uani 1 1 d . . . C15 C 0.13812(12) 0.0203(4) -0.10059(18) 0.0587(10) Uani 1 1 d . . . H15 H 0.1235 0.0976 -0.1070 0.070 Uiso 1 1 calc R . . C16 C 0.13007(11) -0.0943(4) -0.07919(18) 0.0558(9) Uani 1 1 d . . . H16 H 0.1104 -0.0910 -0.0721 0.067 Uiso 1 1 calc R . . C17 C 0.14515(14) -0.3384(4) -0.0457(2) 0.0648(11) Uani 1 1 d . . . H17 H 0.1731 -0.3789 -0.0146 0.078 Uiso 1 1 calc R . . C18 C 0.12603(15) -0.3194(5) -0.0130(2) 0.0800(14) Uani 1 1 d . . . H18A H 0.1429 -0.2580 0.0216 0.120 Uiso 1 1 calc R . . H18B H 0.1252 -0.4024 0.0034 0.120 Uiso 1 1 calc R . . H18C H 0.0978 -0.2857 -0.0432 0.120 Uiso 1 1 calc R . . C19 C 0.1187(2) -0.4327(5) -0.1032(3) 0.106(2) Uani 1 1 d . . . H19A H 0.1182 -0.5185 -0.0886 0.159 Uiso 1 1 calc R . . H19B H 0.1311 -0.4388 -0.1241 0.159 Uiso 1 1 calc R . . H19C H 0.0903 -0.3996 -0.1330 0.159 Uiso 1 1 calc R . . C20 C 0.17737(16) 0.1433(5) -0.1323(2) 0.0836(15) Uani 1 1 d . . . H20A H 0.1620 0.2168 -0.1333 0.125 Uiso 1 1 calc R . . H20B H 0.1693 0.1304 -0.1741 0.125 Uiso 1 1 calc R . . H20C H 0.2072 0.1608 -0.1021 0.125 Uiso 1 1 calc R . . C21 C 0.46020(12) 0.4931(5) 0.35086(19) 0.0639(11) Uani 1 1 d . . . C22 C 0.48527(12) 0.4502(5) 0.4165(2) 0.0684(13) Uani 1 1 d . . . H22 H 0.5093 0.4977 0.4482 0.082 Uiso 1 1 calc R . . C23 C 0.47416(13) 0.3390(5) 0.4333(2) 0.0686(12) Uani 1 1 d . . . H23 H 0.4907 0.3143 0.4761 0.082 Uiso 1 1 calc R . . C24 C 0.43805(14) 0.2621(5) 0.3865(2) 0.0694(12) Uani 1 1 d . . . C25 C 0.41371(13) 0.3034(5) 0.3227(2) 0.0640(11) Uani 1 1 d . . . H25 H 0.3898 0.2553 0.2911 0.077 Uiso 1 1 calc R . . C26 C 0.42470(13) 0.4164(5) 0.30537(19) 0.0642(12) Uani 1 1 d . . . H26 H 0.4079 0.4407 0.2625 0.077 Uiso 1 1 calc R . . C27 C 0.47296(16) 0.6150(6) 0.3349(3) 0.0872(16) Uani 1 1 d . . . H27 H 0.4804 0.6825 0.3666 0.105 Uiso 1 1 calc R . . C28 C 0.4397(2) 0.6713(8) 0.2703(4) 0.133(3) Uani 1 1 d . . . H28A H 0.4393 0.6240 0.2389 0.199 Uiso 1 1 calc R . . H28B H 0.4457 0.7626 0.2698 0.199 Uiso 1 1 calc R . . H28C H 0.4126 0.6637 0.2605 0.199 Uiso 1 1 calc R . . C29 C 0.5134(2) 0.5848(9) 0.3424(4) 0.150(3) Uani 1 1 d . . . H29A H 0.5067 0.5227 0.3102 0.225 Uiso 1 1 calc R . . H29B H 0.5347 0.5482 0.3841 0.225 Uiso 1 1 calc R . . H29C H 0.5238 0.6648 0.3376 0.225 Uiso 1 1 calc R . . C30 C 0.4250(2) 0.1441(6) 0.4050(3) 0.1054(18) Uani 1 1 d . . . H30A H 0.3959 0.1229 0.3706 0.158 Uiso 1 1 calc R . . H30B H 0.4282 0.1644 0.4428 0.158 Uiso 1 1 calc R . . H30C H 0.4426 0.0701 0.4133 0.158 Uiso 1 1 calc R . . C31 C 0.0683(2) 0.3346(11) 0.9726(4) 0.198(6) Uani 1 1 d D . . H31A H 0.0633 0.2745 0.9954 0.238 Uiso 1 1 calc R . . H31B H 0.0949 0.3793 1.0040 0.238 Uiso 1 1 calc R . . Cl5 Cl 0.07232(11) 0.2469(4) 0.92319(16) 0.2125(13) Uani 1 1 d D . . Cl6 Cl 0.02913(11) 0.4472(4) 0.9341(2) 0.2179(15) Uani 1 1 d . . . C32 C 0.1828(2) 0.5194(6) 0.3115(3) 0.125(3) Uani 1 1 d D . . H32A H 0.2035 0.4499 0.3360 0.151 Uiso 1 1 calc R . . H32B H 0.1812 0.5694 0.3407 0.151 Uiso 1 1 calc R . . Cl7 Cl 0.19981(6) 0.6206(2) 0.28146(8) 0.1252(6) Uani 1 1 d . . . Cl8 Cl 0.13501(9) 0.4499(3) 0.25488(14) 0.1823(11) Uani 1 1 d 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 0.03644(16) 0.04283(17) 0.03592(15) 0.00126(12) 0.01981(13) -0.00428(12) Ru2 0.03134(16) 0.0692(2) 0.03246(15) -0.00475(13) 0.01509(13) 0.00329(13) N1 0.0395(15) 0.0470(17) 0.0375(14) 0.0034(12) 0.0236(13) -0.0038(13) N2 0.0357(15) 0.0566(19) 0.0374(15) 0.0002(14) 0.0174(13) 0.0033(14) S1 0.0412(5) 0.0639(6) 0.0508(5) -0.0075(4) 0.0292(4) -0.0036(4) S2 0.0364(5) 0.0512(6) 0.0457(5) 0.0004(4) 0.0160(4) 0.0041(4) Cl1 0.0417(5) 0.0522(5) 0.0503(5) 0.0012(4) 0.0281(4) -0.0064(4) Cl2 0.0521(5) 0.0562(6) 0.0472(5) 0.0117(4) 0.0243(4) -0.0036(4) Cl3 0.0535(6) 0.0733(7) 0.0550(6) -0.0131(5) 0.0236(5) -0.0032(5) Cl4 0.0452(5) 0.1040(9) 0.0447(5) 0.0083(5) 0.0273(4) 0.0130(5) C1 0.046(2) 0.048(2) 0.048(2) 0.0029(16) 0.0323(18) -0.0036(16) C2 0.053(2) 0.042(2) 0.057(2) -0.0002(16) 0.0372(19) -0.0052(16) C3 0.0322(17) 0.057(2) 0.0372(17) -0.0004(16) 0.0178(15) 0.0003(16) C4 0.053(2) 0.061(2) 0.051(2) -0.0009(18) 0.0383(19) -0.0077(18) C5 0.056(2) 0.051(2) 0.055(2) 0.0001(17) 0.038(2) -0.0110(18) C6 0.0409(19) 0.064(3) 0.0421(19) 0.0027(18) 0.0225(17) -0.0062(18) C7 0.0406(19) 0.060(2) 0.0351(17) 0.0075(16) 0.0178(16) 0.0041(17) C8 0.0399(18) 0.050(2) 0.0343(17) -0.0032(15) 0.0198(15) 0.0028(16) C9 0.0380(19) 0.051(2) 0.054(2) 0.0016(18) 0.0212(17) -0.0020(16) C10 0.043(2) 0.052(2) 0.047(2) 0.0088(17) 0.0183(17) 0.0038(17) C11 0.0399(19) 0.052(2) 0.0417(19) -0.0084(16) 0.0175(16) -0.0110(17) C12 0.049(2) 0.054(2) 0.047(2) -0.0076(17) 0.0259(18) -0.0070(18) C13 0.064(3) 0.068(3) 0.041(2) -0.0073(19) 0.031(2) -0.017(2) C14 0.050(2) 0.074(3) 0.0332(19) 0.0031(18) 0.0138(18) -0.014(2) C15 0.044(2) 0.051(2) 0.043(2) 0.0033(17) 0.0086(18) 0.0008(18) C16 0.0356(19) 0.061(2) 0.052(2) -0.0031(19) 0.0180(17) -0.0047(18) C17 0.058(2) 0.054(2) 0.075(3) -0.005(2) 0.038(2) -0.015(2) C18 0.073(3) 0.082(3) 0.081(3) 0.008(3) 0.046(3) -0.016(3) C19 0.130(5) 0.074(4) 0.114(5) -0.041(3) 0.076(4) -0.058(4) C20 0.088(3) 0.072(3) 0.049(2) 0.018(2) 0.024(2) -0.015(3) C21 0.044(2) 0.096(3) 0.050(2) -0.014(2) 0.029(2) -0.003(2) C22 0.0305(19) 0.110(4) 0.049(2) -0.024(2) 0.0174(18) -0.001(2) C23 0.049(2) 0.099(4) 0.048(2) 0.004(2) 0.025(2) 0.025(2) C24 0.065(3) 0.074(3) 0.064(3) 0.000(2) 0.038(2) 0.018(2) C25 0.054(2) 0.077(3) 0.055(2) -0.019(2) 0.032(2) -0.003(2) C26 0.048(2) 0.099(4) 0.042(2) -0.010(2) 0.0266(19) 0.003(2) C27 0.072(3) 0.114(4) 0.085(3) -0.018(3) 0.054(3) -0.023(3) C28 0.103(5) 0.155(7) 0.149(6) 0.041(5) 0.083(5) 0.001(5) C29 0.081(4) 0.232(10) 0.155(7) 0.021(6) 0.082(5) -0.013(5) C30 0.123(5) 0.073(4) 0.116(5) 0.016(3) 0.073(4) 0.014(3) C31 0.080(5) 0.368(17) 0.116(6) 0.035(9) 0.047(5) -0.065(8) Cl5 0.235(3) 0.239(3) 0.185(3) 0.060(2) 0.142(3) 0.037(3) Cl6 0.189(3) 0.243(4) 0.272(4) -0.092(3) 0.169(3) -0.099(3) C32 0.171(7) 0.101(5) 0.071(4) 0.024(3) 0.060(4) 0.034(5) Cl7 0.1106(12) 0.1553(17) 0.0980(11) 0.0092(11) 0.0598(10) -0.0056(12) Cl8 0.150(2) 0.169(2) 0.167(2) 0.0418(17) 0.0693(17) -0.0302(17) _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 N1 2.135(3) . ? Ru1 C15 2.137(4) . ? Ru1 C16 2.163(4) . ? Ru1 C13 2.164(4) . ? Ru1 C12 2.181(4) . ? Ru1 C14 2.183(4) . ? Ru1 C11 2.207(4) . ? Ru1 Cl2 2.4096(17) . ? Ru1 Cl1 2.4106(19) . ? Ru2 N2 2.141(3) . ? Ru2 C25 2.164(4) . ? Ru2 C26 2.167(4) . ? Ru2 C23 2.171(4) . ? Ru2 C22 2.180(4) . ? Ru2 C24 2.195(5) . ? Ru2 C21 2.203(4) . ? Ru2 Cl4 2.3974(17) . ? Ru2 Cl3 2.414(2) . ? N1 C1 1.348(4) . ? N1 C5 1.348(4) . ? N2 C6 1.341(5) . ? N2 C10 1.342(5) . ? S1 C3 1.784(4) . ? S1 S2 2.0327(18) . ? S2 C8 1.776(4) . ? C1 C2 1.374(5) . ? C2 C3 1.383(5) . ? C3 C4 1.371(5) . ? C4 C5 1.370(5) . ? C6 C7 1.374(5) . ? C7 C8 1.386(5) . ? C8 C9 1.386(5) . ? C9 C10 1.373(5) . ? C11 C16 1.399(5) . ? C11 C12 1.437(5) . ? C11 C17 1.514(6) . ? C12 C13 1.387(5) . ? C13 C14 1.429(6) . ? C14 C15 1.398(6) . ? C14 C20 1.509(6) . ? C15 C16 1.422(6) . ? C17 C18 1.503(6) . ? C17 C19 1.539(6) . ? C21 C26 1.400(6) . ? C21 C22 1.441(6) . ? C21 C27 1.502(7) . ? C22 C23 1.390(7) . ? C23 C24 1.421(6) . ? C24 C25 1.399(6) . ? C24 C30 1.511(7) . ? C25 C26 1.410(6) . ? C27 C28 1.488(8) . ? C27 C29 1.552(8) . ? C31 Cl6 1.682(10) . ? C31 Cl5 1.686(8) . ? C32 Cl8 1.693(6) . ? C32 Cl7 1.695(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 N1 Ru1 C15 89.33(15) . . ? N1 Ru1 C16 96.52(14) . . ? C15 Ru1 C16 38.62(15) . . ? N1 Ru1 C13 147.28(14) . . ? C15 Ru1 C13 68.09(18) . . ? C16 Ru1 C13 80.69(16) . . ? N1 Ru1 C12 164.17(12) . . ? C15 Ru1 C12 80.60(16) . . ? C16 Ru1 C12 68.02(15) . . ? C13 Ru1 C12 37.22(14) . . ? N1 Ru1 C14 110.05(15) . . ? C15 Ru1 C14 37.75(16) . . ? C16 Ru1 C14 69.23(15) . . ? C13 Ru1 C14 38.38(17) . . ? C12 Ru1 C14 68.67(17) . . ? N1 Ru1 C11 126.41(13) . . ? C15 Ru1 C11 68.59(15) . . ? C16 Ru1 C11 37.32(14) . . ? C13 Ru1 C11 68.30(14) . . ? C12 Ru1 C11 38.22(13) . . ? C14 Ru1 C11 81.84(15) . . ? N1 Ru1 Cl2 85.61(10) . . ? C15 Ru1 Cl2 146.81(12) . . ? C16 Ru1 Cl2 109.48(11) . . ? C13 Ru1 Cl2 126.26(13) . . ? C12 Ru1 Cl2 96.12(12) . . ? C14 Ru1 Cl2 164.32(13) . . ? C11 Ru1 Cl2 88.35(11) . . ? N1 Ru1 Cl1 86.63(8) . . ? C15 Ru1 Cl1 123.95(12) . . ? C16 Ru1 Cl1 161.88(11) . . ? C13 Ru1 Cl1 87.03(11) . . ? C12 Ru1 Cl1 109.12(10) . . ? C14 Ru1 Cl1 92.89(11) . . ? C11 Ru1 Cl1 146.41(10) . . ? Cl2 Ru1 Cl1 88.52(4) . . ? N2 Ru2 C25 90.84(14) . . ? N2 Ru2 C26 93.84(14) . . ? C25 Ru2 C26 38.01(17) . . ? N2 Ru2 C23 152.14(17) . . ? C25 Ru2 C23 67.56(17) . . ? C26 Ru2 C23 80.01(16) . . ? N2 Ru2 C22 159.34(15) . . ? C25 Ru2 C22 80.01(16) . . ? C26 Ru2 C22 67.59(15) . . ? C23 Ru2 C22 37.25(17) . . ? N2 Ru2 C24 114.53(16) . . ? C25 Ru2 C24 37.41(16) . . ? C26 Ru2 C24 68.30(18) . . ? C23 Ru2 C24 37.99(17) . . ? C22 Ru2 C24 68.18(18) . . ? N2 Ru2 C21 120.97(15) . . ? C25 Ru2 C21 68.47(17) . . ? C26 Ru2 C21 37.37(16) . . ? C23 Ru2 C21 68.64(19) . . ? C22 Ru2 C21 38.40(17) . . ? C24 Ru2 C21 81.75(18) . . ? N2 Ru2 Cl4 85.80(10) . . ? C25 Ru2 Cl4 118.81(13) . . ? C26 Ru2 Cl4 156.81(14) . . ? C23 Ru2 Cl4 89.52(13) . . ? C22 Ru2 Cl4 114.85(13) . . ? C24 Ru2 Cl4 90.73(13) . . ? C21 Ru2 Cl4 152.97(11) . . ? N2 Ru2 Cl3 85.60(9) . . ? C25 Ru2 Cl3 152.77(13) . . ? C26 Ru2 Cl3 115.23(14) . . ? C23 Ru2 Cl3 121.70(14) . . ? C22 Ru2 Cl3 94.09(13) . . ? C24 Ru2 Cl3 159.68(13) . . ? C21 Ru2 Cl3 90.35(13) . . ? Cl4 Ru2 Cl3 87.88(5) . . ? C1 N1 C5 117.0(3) . . ? C1 N1 Ru1 122.1(2) . . ? C5 N1 Ru1 120.8(2) . . ? C6 N2 C10 116.9(3) . . ? C6 N2 Ru2 121.1(2) . . ? C10 N2 Ru2 121.8(3) . . ? C3 S1 S2 104.27(13) . . ? C8 S2 S1 104.99(13) . . ? N1 C1 C2 122.8(3) . . ? C1 C2 C3 119.2(3) . . ? C4 C3 C2 118.3(3) . . ? C4 C3 S1 116.0(3) . . ? C2 C3 S1 125.7(3) . . ? C5 C4 C3 119.7(3) . . ? N1 C5 C4 122.9(3) . . ? N2 C6 C7 123.3(3) . . ? C6 C7 C8 119.3(3) . . ? C7 C8 C9 118.0(3) . . ? C7 C8 S2 116.0(3) . . ? C9 C8 S2 126.0(3) . . ? C10 C9 C8 119.1(4) . . ? N2 C10 C9 123.5(4) . . ? C16 C11 C12 118.0(4) . . ? C16 C11 C17 124.0(3) . . ? C12 C11 C17 118.1(4) . . ? C16 C11 Ru1 69.6(2) . . ? C12 C11 Ru1 69.9(2) . . ? C17 C11 Ru1 131.1(3) . . ? C13 C12 C11 120.7(4) . . ? C13 C12 Ru1 70.7(2) . . ? C11 C12 Ru1 71.9(2) . . ? C12 C13 C14 121.9(4) . . ? C12 C13 Ru1 72.1(2) . . ? C14 C13 Ru1 71.5(2) . . ? C15 C14 C13 116.8(4) . . ? C15 C14 C20 122.6(4) . . ? C13 C14 C20 120.5(4) . . ? C15 C14 Ru1 69.3(2) . . ? C13 C14 Ru1 70.1(2) . . ? C20 C14 Ru1 128.2(3) . . ? C14 C15 C16 122.2(4) . . ? C14 C15 Ru1 72.9(2) . . ? C16 C15 Ru1 71.7(2) . . ? C11 C16 C15 120.4(4) . . ? C11 C16 Ru1 73.0(2) . . ? C15 C16 Ru1 69.7(2) . . ? C18 C17 C11 114.4(4) . . ? C18 C17 C19 112.0(4) . . ? C11 C17 C19 107.9(4) . . ? C26 C21 C22 116.6(4) . . ? C26 C21 C27 124.0(4) . . ? C22 C21 C27 119.4(4) . . ? C26 C21 Ru2 69.9(2) . . ? C22 C21 Ru2 70.0(2) . . ? C27 C21 Ru2 130.5(3) . . ? C23 C22 C21 121.1(4) . . ? C23 C22 Ru2 71.0(2) . . ? C21 C22 Ru2 71.6(2) . . ? C22 C23 C24 121.5(4) . . ? C22 C23 Ru2 71.7(3) . . ? C24 C23 Ru2 71.9(2) . . ? C25 C24 C23 117.5(5) . . ? C25 C24 C30 120.9(5) . . ? C23 C24 C30 121.5(5) . . ? C25 C24 Ru2 70.1(3) . . ? C23 C24 Ru2 70.1(3) . . ? C30 C24 Ru2 128.4(3) . . ? C24 C25 C26 121.3(4) . . ? C24 C25 Ru2 72.5(3) . . ? C26 C25 Ru2 71.1(2) . . ? C21 C26 C25 121.9(4) . . ? C21 C26 Ru2 72.7(2) . . ? C25 C26 Ru2 70.9(2) . . ? C28 C27 C21 115.1(5) . . ? C28 C27 C29 109.8(5) . . ? C21 C27 C29 109.0(5) . . ? Cl6 C31 Cl5 113.3(5) . . ? Cl8 C32 Cl7 113.8(3) . . ? _diffrn_measured_fraction_theta_max 0.964 _diffrn_reflns_theta_full 27.10 _diffrn_measured_fraction_theta_full 0.964 _refine_diff_density_max 1.030 _refine_diff_density_min -0.661 _refine_diff_density_rms 0.094 # Attachment '- Complex 3c-CH2Cl2.cif' data_Complex_3c_CH2Cl2 _database_code_depnum_ccdc_archive 'CCDC 767813' #TrackingRef '- Complex 3c-CH2Cl2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44 H48 Cl6 F6 N4 O6 Ru2 S6' _chemical_formula_weight 1450.06 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' F F 0.0171 0.0103 '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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.808(4) _cell_length_b 14.203(4) _cell_length_c 15.707(4) _cell_angle_alpha 90.00 _cell_angle_beta 102.793(4) _cell_angle_gamma 90.00 _cell_volume 2786.5(14) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1020 _cell_measurement_theta_min 2.350 _cell_measurement_theta_max 26.677 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.728 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1456 _exptl_absorpt_coefficient_mu 1.124 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8769 _exptl_absorpt_correction_T_max 0.9155 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 4.40 _diffrn_reflns_number 13213 _diffrn_reflns_av_R_equivalents 0.0519 _diffrn_reflns_av_sigmaI/netI 0.0898 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.86 _diffrn_reflns_theta_max 27.12 _reflns_number_total 5980 _reflns_number_gt 3428 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0602P)^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 5980 _refine_ls_number_parameters 337 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0961 _refine_ls_R_factor_gt 0.0497 _refine_ls_wR_factor_ref 0.1220 _refine_ls_wR_factor_gt 0.1101 _refine_ls_goodness_of_fit_ref 0.877 _refine_ls_restrained_S_all 0.877 _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 0.73608(3) 0.26170(3) 0.55603(3) 0.03597(14) Uani 1 1 d . . . Cl1 Cl 0.79517(11) 0.26449(9) 0.71223(8) 0.0500(3) Uani 1 1 d . . . N1 N 0.9021(3) 0.2647(3) 0.5485(3) 0.0387(9) Uani 1 1 d . . . N2 N 1.2502(3) -0.1115(3) 0.4347(3) 0.0384(10) Uani 1 1 d . . . S1 S 1.25566(10) 0.25918(9) 0.54124(9) 0.0494(3) Uani 1 1 d . . . S2 S 1.26619(11) 0.20877(9) 0.42242(9) 0.0485(4) Uani 1 1 d . . . C1 C 0.9332(4) 0.2342(3) 0.4777(3) 0.0436(12) Uani 1 1 d . . . H1 H 0.8806 0.2145 0.4302 0.052 Uiso 1 1 calc R . . C2 C 1.0369(4) 0.2302(3) 0.4704(3) 0.0425(12) Uani 1 1 d . . . H2 H 1.0538 0.2057 0.4203 0.051 Uiso 1 1 calc R . . C3 C 1.1172(4) 0.2628(3) 0.5380(3) 0.0376(11) Uani 1 1 d . . . C4 C 1.0865(4) 0.2986(4) 0.6101(3) 0.0495(14) Uani 1 1 d . . . H4 H 1.1374 0.3233 0.6563 0.059 Uiso 1 1 calc R . . C5 C 0.9809(4) 0.2978(4) 0.6135(3) 0.0514(14) Uani 1 1 d . . . H5 H 0.9622 0.3213 0.6633 0.062 Uiso 1 1 calc R . . C6 C 1.2589(4) 0.0850(3) 0.4323(3) 0.0387(11) Uani 1 1 d . . . C7 C 1.2303(4) 0.0379(3) 0.4993(3) 0.0467(13) Uani 1 1 d . . . H7 H 1.2126 0.0712 0.5451 0.056 Uiso 1 1 calc R . . C8 C 1.2276(4) -0.0586(3) 0.4991(3) 0.0457(13) Uani 1 1 d . . . H8 H 1.2092 -0.0891 0.5460 0.055 Uiso 1 1 calc R . . C9 C 1.2782(4) -0.0650(4) 0.3700(3) 0.0479(13) Uani 1 1 d . . . H9 H 1.2950 -0.0998 0.3247 0.057 Uiso 1 1 calc R . . C10 C 1.2839(4) 0.0324(4) 0.3660(3) 0.0484(14) Uani 1 1 d . . . H10 H 1.3042 0.0617 0.3192 0.058 Uiso 1 1 calc R . . C11 C 0.6622(4) 0.4026(3) 0.5575(3) 0.0444(13) Uani 1 1 d . . . C12 C 0.5909(4) 0.3307(4) 0.5728(4) 0.0470(13) Uani 1 1 d . . . H12 H 0.5631 0.3339 0.6226 0.056 Uiso 1 1 calc R . . C13 C 0.5617(4) 0.2558(4) 0.5150(4) 0.0494(13) Uani 1 1 d . . . H13 H 0.5143 0.2105 0.5266 0.059 Uiso 1 1 calc R . . C14 C 0.6033(4) 0.2476(4) 0.4386(4) 0.0526(14) Uani 1 1 d . . . C15 C 0.6746(4) 0.3168(4) 0.4242(3) 0.0567(16) Uani 1 1 d . . . H15 H 0.7035 0.3132 0.3750 0.068 Uiso 1 1 calc R . . C16 C 0.7037(4) 0.3928(4) 0.4834(4) 0.0542(15) Uani 1 1 d . . . H16 H 0.7521 0.4375 0.4722 0.065 Uiso 1 1 calc R . . C17 C 0.6874(4) 0.4834(4) 0.6200(4) 0.0578(15) Uani 1 1 d . . . H17 H 0.6853 0.4597 0.6782 0.069 Uiso 1 1 calc R . . C18 C 0.7973(5) 0.5246(5) 0.6253(5) 0.087(2) Uani 1 1 d . . . H18A H 0.8507 0.4807 0.6537 0.131 Uiso 1 1 calc R . . H18B H 0.8041 0.5823 0.6579 0.131 Uiso 1 1 calc R . . H18C H 0.8069 0.5371 0.5674 0.131 Uiso 1 1 calc R . . C19 C 0.6014(5) 0.5570(4) 0.5963(4) 0.0708(18) Uani 1 1 d . . . H19A H 0.6013 0.5816 0.5394 0.106 Uiso 1 1 calc R . . H19B H 0.6149 0.6070 0.6384 0.106 Uiso 1 1 calc R . . H19C H 0.5330 0.5292 0.5961 0.106 Uiso 1 1 calc R . . C20 C 0.5695(5) 0.1667(5) 0.3763(4) 0.083(2) Uani 1 1 d . . . H20A H 0.5091 0.1854 0.3315 0.125 Uiso 1 1 calc R . . H20B H 0.5501 0.1138 0.4075 0.125 Uiso 1 1 calc R . . H20C H 0.6278 0.1495 0.3501 0.125 Uiso 1 1 calc R . . S3 S 0.38695(15) 0.41393(12) 0.74827(10) 0.0693(5) Uani 1 1 d . . . O1 O 0.4850(4) 0.3596(4) 0.7607(3) 0.1120(18) Uani 1 1 d . . . O2 O 0.3113(4) 0.3772(4) 0.7921(3) 0.0928(15) Uani 1 1 d . . . O3 O 0.3458(4) 0.4457(3) 0.6623(3) 0.0944(16) Uani 1 1 d . . . C21 C 0.4342(6) 0.5170(6) 0.8073(5) 0.081(2) Uani 1 1 d . . . F1 F 0.4708(4) 0.5019(4) 0.8901(3) 0.1179(16) Uani 1 1 d . . . F2 F 0.5091(4) 0.5608(4) 0.7775(3) 0.138(2) Uani 1 1 d . . . F3 F 0.3548(4) 0.5800(3) 0.8026(3) 0.1313(18) Uani 1 1 d . . . C22 C 0.0815(8) 0.6344(6) 0.7378(6) 0.131(3) Uani 1 1 d . . . H22A H 0.0374 0.6875 0.7132 0.157 Uiso 1 1 calc R . . H22B H 0.1530 0.6582 0.7616 0.157 Uiso 1 1 calc R . . Cl2 Cl 0.0316(2) 0.5889(2) 0.82166(19) 0.1460(10) Uani 1 1 d . . . Cl3 Cl 0.0879(2) 0.55775(19) 0.6554(2) 0.1606(12) 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 0.0365(2) 0.0357(2) 0.0348(2) 0.00162(18) 0.00581(16) 0.00829(19) Cl1 0.0599(8) 0.0519(8) 0.0368(7) -0.0010(6) 0.0076(6) 0.0096(7) N1 0.038(2) 0.039(2) 0.036(2) -0.0031(18) 0.0033(19) 0.0037(19) N2 0.041(2) 0.036(2) 0.040(2) 0.0011(19) 0.012(2) 0.0055(19) S1 0.0405(7) 0.0481(8) 0.0591(9) -0.0122(7) 0.0101(7) -0.0027(6) S2 0.0527(8) 0.0375(7) 0.0604(9) -0.0003(6) 0.0232(7) -0.0011(6) C1 0.041(3) 0.048(3) 0.040(3) -0.002(2) 0.004(2) 0.002(2) C2 0.044(3) 0.047(3) 0.036(3) -0.006(2) 0.010(2) 0.002(2) C3 0.039(3) 0.030(2) 0.043(3) -0.001(2) 0.008(2) 0.004(2) C4 0.038(3) 0.058(3) 0.047(3) -0.017(3) -0.001(3) 0.002(3) C5 0.048(3) 0.063(4) 0.043(3) -0.012(3) 0.008(3) 0.007(3) C6 0.036(3) 0.039(3) 0.042(3) 0.000(2) 0.011(2) 0.001(2) C7 0.050(3) 0.042(3) 0.052(3) -0.010(2) 0.021(3) 0.003(3) C8 0.056(3) 0.046(3) 0.038(3) 0.005(2) 0.017(3) 0.008(3) C9 0.058(4) 0.047(3) 0.042(3) -0.004(2) 0.019(3) 0.005(3) C10 0.063(4) 0.045(3) 0.040(3) 0.005(2) 0.017(3) 0.001(3) C11 0.044(3) 0.035(3) 0.051(3) 0.004(2) 0.004(3) 0.012(2) C12 0.039(3) 0.051(3) 0.052(3) 0.007(3) 0.014(3) 0.019(3) C13 0.035(3) 0.044(3) 0.066(4) 0.007(3) 0.003(3) 0.005(2) C14 0.043(3) 0.062(4) 0.045(3) -0.001(3) -0.008(3) 0.020(3) C15 0.052(4) 0.078(4) 0.037(3) 0.017(3) 0.002(3) 0.026(3) C16 0.052(4) 0.050(3) 0.056(4) 0.024(3) 0.003(3) 0.015(3) C17 0.056(4) 0.043(3) 0.068(4) -0.004(3) 0.002(3) 0.008(3) C18 0.063(4) 0.061(4) 0.125(7) -0.007(4) -0.009(4) -0.001(4) C19 0.072(4) 0.045(3) 0.094(5) -0.010(3) 0.014(4) 0.012(3) C20 0.064(4) 0.092(5) 0.080(5) -0.031(4) -0.014(4) 0.009(4) S3 0.0890(13) 0.0657(10) 0.0497(10) 0.0044(8) 0.0078(9) -0.0075(10) O1 0.119(4) 0.113(4) 0.104(4) 0.008(3) 0.025(3) 0.058(4) O2 0.088(3) 0.112(4) 0.078(3) 0.012(3) 0.016(3) -0.037(3) O3 0.144(5) 0.082(3) 0.044(3) 0.007(2) -0.006(3) -0.012(3) C21 0.077(5) 0.105(6) 0.060(5) -0.011(4) 0.013(4) 0.001(5) F1 0.113(4) 0.163(4) 0.065(3) -0.025(3) -0.007(3) -0.019(3) F2 0.147(4) 0.151(4) 0.134(4) -0.039(3) 0.071(4) -0.084(4) F3 0.161(5) 0.096(3) 0.131(4) -0.026(3) 0.021(4) 0.029(3) C22 0.189(10) 0.083(6) 0.132(8) -0.014(5) 0.059(8) -0.034(6) Cl2 0.127(2) 0.169(3) 0.142(2) 0.017(2) 0.0289(18) -0.0288(19) Cl3 0.153(2) 0.122(2) 0.237(3) 0.003(2) 0.107(2) 0.0019(18) _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 N2 2.143(4) 3_756 ? Ru1 N1 2.156(4) . ? Ru1 C12 2.169(5) . ? Ru1 C16 2.175(5) . ? Ru1 C13 2.185(5) . ? Ru1 C15 2.190(5) . ? Ru1 C11 2.216(5) . ? Ru1 C14 2.224(5) . ? Ru1 Cl1 2.4023(15) . ? N1 C1 1.334(6) . ? N1 C5 1.351(6) . ? N2 C9 1.326(6) . ? N2 C8 1.341(6) . ? N2 Ru1 2.143(4) 3_756 ? S1 C3 1.763(5) . ? S1 S2 2.031(2) . ? S2 C6 1.769(5) . ? C1 C2 1.359(7) . ? C2 C3 1.384(7) . ? C3 C4 1.376(7) . ? C4 C5 1.365(7) . ? C6 C7 1.365(6) . ? C6 C10 1.375(7) . ? C7 C8 1.371(6) . ? C9 C10 1.388(7) . ? C11 C16 1.389(7) . ? C11 C12 1.425(7) . ? C11 C17 1.500(7) . ? C12 C13 1.395(7) . ? C13 C14 1.421(8) . ? C14 C15 1.394(8) . ? C14 C20 1.509(8) . ? C15 C16 1.420(8) . ? C17 C19 1.503(7) . ? C17 C18 1.510(8) . ? S3 O2 1.408(5) . ? S3 O3 1.411(4) . ? S3 O1 1.450(5) . ? S3 C21 1.766(8) . ? C21 F1 1.300(7) . ? C21 F2 1.314(8) . ? C21 F3 1.345(8) . ? C22 Cl3 1.706(8) . ? C22 Cl2 1.714(8) . ? 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 N2 Ru1 N1 87.49(14) 3_756 . ? N2 Ru1 C12 120.08(18) 3_756 . ? N1 Ru1 C12 151.68(17) . . ? N2 Ru1 C16 153.00(19) 3_756 . ? N1 Ru1 C16 91.73(18) . . ? C12 Ru1 C16 66.9(2) . . ? N2 Ru1 C13 92.55(17) 3_756 . ? N1 Ru1 C13 160.18(18) . . ? C12 Ru1 C13 37.38(19) . . ? C16 Ru1 C13 79.3(2) . . ? N2 Ru1 C15 115.3(2) 3_756 . ? N1 Ru1 C15 95.39(18) . . ? C12 Ru1 C15 79.3(2) . . ? C16 Ru1 C15 37.9(2) . . ? C13 Ru1 C15 66.7(2) . . ? N2 Ru1 C11 158.00(17) 3_756 . ? N1 Ru1 C11 114.30(17) . . ? C12 Ru1 C11 37.92(18) . . ? C16 Ru1 C11 36.86(19) . . ? C13 Ru1 C11 68.10(19) . . ? C15 Ru1 C11 67.8(2) . . ? N2 Ru1 C14 90.12(18) 3_756 . ? N1 Ru1 C14 122.60(19) . . ? C12 Ru1 C14 67.8(2) . . ? C16 Ru1 C14 67.7(2) . . ? C13 Ru1 C14 37.6(2) . . ? C15 Ru1 C14 36.8(2) . . ? C11 Ru1 C14 80.80(19) . . ? N2 Ru1 Cl1 86.84(11) 3_756 . ? N1 Ru1 Cl1 87.95(11) . . ? C12 Ru1 Cl1 87.33(14) . . ? C16 Ru1 Cl1 120.12(16) . . ? C13 Ru1 Cl1 111.85(16) . . ? C15 Ru1 Cl1 157.74(17) . . ? C11 Ru1 Cl1 90.77(14) . . ? C14 Ru1 Cl1 149.15(17) . . ? C1 N1 C5 115.6(4) . . ? C1 N1 Ru1 121.3(3) . . ? C5 N1 Ru1 123.1(3) . . ? C9 N2 C8 116.1(4) . . ? C9 N2 Ru1 121.0(3) . 3_756 ? C8 N2 Ru1 122.3(3) . 3_756 ? C3 S1 S2 104.75(17) . . ? C6 S2 S1 104.74(18) . . ? N1 C1 C2 124.1(5) . . ? C1 C2 C3 119.8(5) . . ? C4 C3 C2 117.1(5) . . ? C4 C3 S1 117.1(4) . . ? C2 C3 S1 125.8(4) . . ? C5 C4 C3 119.7(5) . . ? N1 C5 C4 123.7(5) . . ? C7 C6 C10 117.7(4) . . ? C7 C6 S2 125.7(4) . . ? C10 C6 S2 116.6(4) . . ? C6 C7 C8 119.9(5) . . ? N2 C8 C7 123.5(5) . . ? N2 C9 C10 123.8(5) . . ? C6 C10 C9 118.9(5) . . ? C16 C11 C12 116.6(5) . . ? C16 C11 C17 124.0(5) . . ? C12 C11 C17 119.4(5) . . ? C16 C11 Ru1 70.0(3) . . ? C12 C11 Ru1 69.3(3) . . ? C17 C11 Ru1 131.9(4) . . ? C13 C12 C11 121.7(5) . . ? C13 C12 Ru1 71.9(3) . . ? C11 C12 Ru1 72.8(3) . . ? C12 C13 C14 121.0(5) . . ? C12 C13 Ru1 70.7(3) . . ? C14 C13 Ru1 72.7(3) . . ? C15 C14 C13 117.4(5) . . ? C15 C14 C20 122.4(6) . . ? C13 C14 C20 120.2(6) . . ? C15 C14 Ru1 70.3(3) . . ? C13 C14 Ru1 69.7(3) . . ? C20 C14 Ru1 131.6(4) . . ? C14 C15 C16 121.1(5) . . ? C14 C15 Ru1 72.9(3) . . ? C16 C15 Ru1 70.4(3) . . ? C11 C16 C15 122.0(5) . . ? C11 C16 Ru1 73.1(3) . . ? C15 C16 Ru1 71.6(3) . . ? C11 C17 C19 109.3(5) . . ? C11 C17 C18 113.3(5) . . ? C19 C17 C18 111.6(5) . . ? O2 S3 O3 115.8(3) . . ? O2 S3 O1 114.0(3) . . ? O3 S3 O1 115.4(3) . . ? O2 S3 C21 104.1(3) . . ? O3 S3 C21 104.4(3) . . ? O1 S3 C21 100.6(4) . . ? F1 C21 F2 107.8(6) . . ? F1 C21 F3 105.4(6) . . ? F2 C21 F3 105.6(7) . . ? F1 C21 S3 113.2(6) . . ? F2 C21 S3 113.5(5) . . ? F3 C21 S3 110.8(5) . . ? Cl3 C22 Cl2 115.6(5) . . ? _diffrn_measured_fraction_theta_max 0.970 _diffrn_reflns_theta_full 27.12 _diffrn_measured_fraction_theta_full 0.970 _refine_diff_density_max 0.944 _refine_diff_density_min -0.672 _refine_diff_density_rms 0.104 # Attachment '- Complex 3c-CHCl3.cif' data_Complex_3c_CHCl3 _database_code_depnum_ccdc_archive 'CCDC 767814' #TrackingRef '- Complex 3c-CHCl3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C46 H48 Cl14 F6 N4 O6 Ru2 S6' _chemical_formula_weight 1757.68 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' F F 0.0171 0.0103 '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' 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 18.679(7) _cell_length_b 11.237(4) _cell_length_c 32.559(12) _cell_angle_alpha 90.00 _cell_angle_beta 94.083(5) _cell_angle_gamma 90.00 _cell_volume 6816(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 891 _cell_measurement_theta_min 2.420 _cell_measurement_theta_max 21.434 _exptl_crystal_description prism _exptl_crystal_colour ? _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.713 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3504 _exptl_absorpt_coefficient_mu 1.238 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8656 _exptl_absorpt_correction_T_max 0.9074 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 4.15 _diffrn_reflns_number 13708 _diffrn_reflns_av_R_equivalents 0.0498 _diffrn_reflns_av_sigmaI/netI 0.0824 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -38 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 2.12 _diffrn_reflns_theta_max 25.01 _reflns_number_total 5971 _reflns_number_gt 3778 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.1390P)^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 5971 _refine_ls_number_parameters 362 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.1113 _refine_ls_R_factor_gt 0.0755 _refine_ls_wR_factor_ref 0.2211 _refine_ls_wR_factor_gt 0.2044 _refine_ls_goodness_of_fit_ref 0.980 _refine_ls_restrained_S_all 0.993 _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 0.26289(3) 0.45195(6) 0.627167(18) 0.0378(2) Uani 1 1 d . . . Cl1 Cl 0.33395(13) 0.2971(2) 0.59933(7) 0.0586(6) Uani 1 1 d . . . S1 S 0.48413(12) 0.8612(2) 0.55613(7) 0.0561(6) Uani 1 1 d . . . S2 S 0.43205(13) 1.0199(2) 0.55379(7) 0.0538(6) Uani 1 1 d . . . N1 N 0.3319(3) 0.5825(6) 0.60184(18) 0.0381(15) Uani 1 1 d . . . N2 N 0.2990(3) 1.0394(5) 0.43109(19) 0.0372(15) Uani 1 1 d . . . C1 C 0.4002(4) 0.5600(7) 0.5951(2) 0.045(2) Uani 1 1 d . . . H1 H 0.4172 0.4829 0.5995 0.054 Uiso 1 1 calc R . . C2 C 0.4463(5) 0.6441(8) 0.5822(3) 0.051(2) Uani 1 1 d . . . H2 H 0.4939 0.6253 0.5784 0.062 Uiso 1 1 calc R . . C3 C 0.4204(4) 0.7578(7) 0.5751(2) 0.0406(19) Uani 1 1 d . . . C4 C 0.3533(4) 0.7828(7) 0.5819(2) 0.043(2) Uani 1 1 d . . . H4 H 0.3358 0.8594 0.5773 0.052 Uiso 1 1 calc R . . C5 C 0.3095(4) 0.6966(7) 0.5958(2) 0.044(2) Uani 1 1 d . . . H5 H 0.2628 0.7167 0.6013 0.053 Uiso 1 1 calc R . . C6 C 0.3817(4) 1.0205(7) 0.5055(2) 0.0400(19) Uani 1 1 d . . . C7 C 0.3807(5) 0.9314(7) 0.4762(3) 0.044(2) Uani 1 1 d . . . H7 H 0.4080 0.8630 0.4812 0.053 Uiso 1 1 calc R . . C8 C 0.3400(4) 0.9431(7) 0.4402(3) 0.0422(19) Uani 1 1 d . . . H8 H 0.3404 0.8819 0.4210 0.051 Uiso 1 1 calc R . . C9 C 0.3011(5) 1.1264(7) 0.4595(3) 0.046(2) Uani 1 1 d . . . H9 H 0.2746 1.1951 0.4537 0.056 Uiso 1 1 calc R . . C10 C 0.3401(5) 1.1192(7) 0.4964(3) 0.047(2) Uani 1 1 d . . . H10 H 0.3386 1.1809 0.5154 0.057 Uiso 1 1 calc R . . C11 C 0.2844(6) 0.5363(9) 0.6886(2) 0.059(3) Uani 1 1 d . . . C12 C 0.3001(6) 0.4149(8) 0.6913(2) 0.055(2) Uani 1 1 d . . . H12 H 0.3448 0.3895 0.7023 0.066 Uiso 1 1 calc R . . C13 C 0.2483(5) 0.3320(9) 0.6774(3) 0.057(2) Uani 1 1 d . . . H13 H 0.2599 0.2517 0.6794 0.068 Uiso 1 1 calc R . . C14 C 0.1804(5) 0.3625(8) 0.6607(3) 0.052(2) Uani 1 1 d . . . C15 C 0.1676(5) 0.4838(8) 0.6582(3) 0.051(2) Uani 1 1 d . . . H15 H 0.1231 0.5087 0.6468 0.062 Uiso 1 1 calc R . . C16 C 0.2160(5) 0.5694(9) 0.6714(2) 0.054(2) Uani 1 1 d . . . H16 H 0.2037 0.6495 0.6690 0.065 Uiso 1 1 calc R . . C17 C 0.3392(7) 0.6312(10) 0.7027(3) 0.074(3) Uani 1 1 d . . . H17 H 0.3358 0.6943 0.6819 0.089 Uiso 1 1 calc R . . C18 C 0.3120(8) 0.6858(13) 0.7433(4) 0.111(5) Uani 1 1 d . . . H18A H 0.3089 0.6243 0.7635 0.166 Uiso 1 1 calc R . . H18B H 0.2654 0.7206 0.7374 0.166 Uiso 1 1 calc R . . H18C H 0.3450 0.7460 0.7537 0.166 Uiso 1 1 calc R . . C19 C 0.4132(8) 0.5970(13) 0.7077(4) 0.109(5) Uani 1 1 d . . . H19A H 0.4207 0.5470 0.7315 0.163 Uiso 1 1 calc R . . H19B H 0.4426 0.6668 0.7112 0.163 Uiso 1 1 calc R . . H19C H 0.4258 0.5542 0.6838 0.163 Uiso 1 1 calc R . . C20 C 0.1247(6) 0.2740(11) 0.6471(3) 0.082(3) Uani 1 1 d . . . H20A H 0.0969 0.3038 0.6234 0.124 Uiso 1 1 calc R . . H20B H 0.0938 0.2601 0.6690 0.124 Uiso 1 1 calc R . . H20C H 0.1474 0.2007 0.6402 0.124 Uiso 1 1 calc R . . S3 S 0.4264(3) 0.6955(4) 0.37336(15) 0.1366(19) Uani 1 1 d D . . C21 C 0.4305(14) 0.638(3) 0.3255(11) 0.32(2) Uiso 1 1 d D . . F1 F 0.3909(10) 0.6922(17) 0.2952(6) 0.267(7) Uiso 1 1 d D . . F2 F 0.4998(11) 0.6485(17) 0.3156(6) 0.267(7) Uiso 1 1 d D . . F3 F 0.4021(13) 0.527(2) 0.3251(8) 0.332(11) Uiso 1 1 d D . . O1 O 0.3543(4) 0.7025(8) 0.3793(3) 0.117(3) Uani 1 1 d D . . O2 O 0.4620(7) 0.6088(16) 0.3953(5) 0.264(12) Uani 1 1 d D . . O3 O 0.4593(8) 0.8021(10) 0.3656(5) 0.186(6) Uani 1 1 d D . . C22 C 0.1513(7) 0.9767(10) 0.5401(4) 0.083(3) Uani 1 1 d . . . H22 H 0.1194 0.9364 0.5582 0.100 Uiso 1 1 calc R . . Cl2 Cl 0.2139(2) 1.0589(3) 0.57040(11) 0.1032(11) Uani 1 1 d . . . Cl3 Cl 0.19198(18) 0.8713(3) 0.51167(9) 0.0884(9) Uani 1 1 d . . . Cl4 Cl 0.0997(2) 1.0750(3) 0.50775(14) 0.1171(13) Uani 1 1 d . . . C23 C 0.1049(8) 0.4512(12) 0.3251(5) 0.107(4) Uani 1 1 d . . . H23 H 0.0970 0.3924 0.3465 0.129 Uiso 1 1 calc R . . Cl5 Cl 0.1905(3) 0.5104(5) 0.33257(17) 0.1458(17) Uani 1 1 d . . . Cl6 Cl 0.0992(3) 0.3812(5) 0.27534(16) 0.167(2) Uani 1 1 d . . . Cl7 Cl 0.0431(3) 0.5641(4) 0.3264(2) 0.163(2) 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 0.0428(4) 0.0348(4) 0.0364(4) 0.0071(3) 0.0070(3) 0.0109(3) Cl1 0.0633(15) 0.0468(14) 0.0663(14) 0.0000(11) 0.0092(12) 0.0166(11) S1 0.0363(13) 0.0699(16) 0.0617(14) 0.0248(12) 0.0009(10) -0.0040(11) S2 0.0589(15) 0.0499(14) 0.0511(13) 0.0088(10) -0.0066(11) -0.0125(11) N1 0.036(4) 0.041(4) 0.038(3) 0.004(3) 0.006(3) 0.008(3) N2 0.044(4) 0.029(3) 0.040(3) 0.009(3) 0.009(3) 0.005(3) C1 0.043(5) 0.039(5) 0.054(5) 0.014(4) 0.003(4) 0.014(4) C2 0.037(5) 0.062(6) 0.057(5) 0.011(5) 0.009(4) 0.010(4) C3 0.040(5) 0.047(5) 0.035(4) 0.009(4) -0.001(3) -0.002(4) C4 0.041(5) 0.041(5) 0.047(5) 0.007(4) 0.001(4) 0.008(4) C5 0.040(5) 0.040(5) 0.052(5) 0.011(4) 0.005(4) 0.009(4) C6 0.036(5) 0.034(5) 0.051(5) 0.007(4) 0.009(4) -0.010(3) C7 0.047(5) 0.029(5) 0.057(5) 0.010(4) 0.000(4) 0.003(3) C8 0.046(5) 0.030(4) 0.051(5) 0.004(4) 0.006(4) 0.006(4) C9 0.057(6) 0.031(5) 0.050(5) 0.005(4) -0.001(4) 0.005(4) C10 0.054(6) 0.032(5) 0.055(5) -0.004(4) 0.000(4) -0.001(4) C11 0.087(8) 0.061(6) 0.030(4) -0.004(4) 0.013(4) 0.008(5) C12 0.072(7) 0.054(6) 0.037(4) 0.016(4) -0.002(4) 0.013(5) C13 0.066(7) 0.055(6) 0.051(5) 0.016(4) 0.007(5) 0.009(5) C14 0.057(6) 0.060(6) 0.043(5) 0.016(4) 0.019(4) 0.005(5) C15 0.044(5) 0.055(6) 0.058(5) 0.011(4) 0.020(4) 0.011(4) C16 0.062(6) 0.062(6) 0.039(5) 0.004(4) 0.011(4) 0.022(5) C17 0.100(9) 0.069(7) 0.054(6) -0.017(5) 0.009(6) -0.003(6) C18 0.132(12) 0.125(12) 0.075(8) -0.044(8) -0.001(8) 0.015(10) C19 0.085(10) 0.133(12) 0.106(10) -0.026(9) -0.010(8) -0.009(9) C20 0.078(8) 0.089(9) 0.080(7) 0.019(6) 0.002(6) -0.031(7) S3 0.130(4) 0.129(4) 0.158(4) 0.071(3) 0.061(3) 0.062(3) O1 0.095(7) 0.124(8) 0.140(8) 0.038(6) 0.053(6) 0.067(6) O2 0.125(10) 0.34(2) 0.34(2) 0.269(19) 0.110(12) 0.150(12) O3 0.197(13) 0.118(10) 0.244(15) 0.062(10) 0.017(11) -0.043(9) C22 0.093(9) 0.073(8) 0.084(8) -0.004(6) 0.015(7) -0.008(6) Cl2 0.130(3) 0.086(2) 0.094(2) -0.0213(18) 0.009(2) -0.012(2) Cl3 0.107(2) 0.0671(19) 0.091(2) -0.0174(15) 0.0092(17) 0.0087(16) Cl4 0.123(3) 0.091(3) 0.138(3) 0.005(2) 0.010(3) 0.018(2) C23 0.103(11) 0.089(10) 0.130(12) -0.016(8) 0.013(9) 0.016(8) Cl5 0.158(4) 0.115(3) 0.160(4) -0.018(3) -0.014(3) 0.022(3) Cl6 0.172(5) 0.191(5) 0.133(4) -0.060(4) -0.018(3) 0.039(4) Cl7 0.145(4) 0.133(4) 0.218(6) -0.030(4) 0.058(4) 0.031(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 2.139(8) . ? Ru1 C13 2.151(9) . ? Ru1 N2 2.152(6) 7_566 ? Ru1 N1 2.156(6) . ? Ru1 C16 2.183(8) . ? Ru1 C12 2.193(8) . ? Ru1 C14 2.195(8) . ? Ru1 C11 2.224(8) . ? Ru1 Cl1 2.405(2) . ? S1 C3 1.804(8) . ? S1 S2 2.031(4) . ? S2 C6 1.773(8) . ? N1 C1 1.332(10) . ? N1 C5 1.359(10) . ? N2 C9 1.345(10) . ? N2 C8 1.347(9) . ? N2 Ru1 2.152(6) 7_566 ? C1 C2 1.365(12) . ? C2 C3 1.381(11) . ? C3 C4 1.318(11) . ? C4 C5 1.366(11) . ? C6 C10 1.375(11) . ? C6 C7 1.381(11) . ? C7 C8 1.356(11) . ? C9 C10 1.362(11) . ? C11 C12 1.396(13) . ? C11 C16 1.409(13) . ? C11 C17 1.526(15) . ? C12 C13 1.395(13) . ? C13 C14 1.386(12) . ? C14 C15 1.385(13) . ? C14 C20 1.484(13) . ? C15 C16 1.368(13) . ? C17 C19 1.432(16) . ? C17 C18 1.573(14) . ? S3 O2 1.353(7) . ? S3 O1 1.375(7) . ? S3 O3 1.379(8) . ? S3 C21 1.70(4) . ? C21 F1 1.337(19) . ? C21 F3 1.349(19) . ? C21 F2 1.362(19) . ? C22 Cl3 1.714(12) . ? C22 Cl2 1.739(12) . ? C22 Cl4 1.766(13) . ? C23 Cl7 1.718(13) . ? C23 Cl5 1.732(15) . ? C23 Cl6 1.797(15) . ? 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 C13 65.8(3) . . ? C15 Ru1 N2 89.8(3) . 7_566 ? C13 Ru1 N2 127.5(3) . 7_566 ? C15 Ru1 N1 127.4(3) . . ? C13 Ru1 N1 146.0(3) . . ? N2 Ru1 N1 86.0(2) 7_566 . ? C15 Ru1 C16 36.9(3) . . ? C13 Ru1 C16 78.4(4) . . ? N2 Ru1 C16 109.8(3) 7_566 . ? N1 Ru1 C16 96.9(3) . . ? C15 Ru1 C12 78.4(4) . . ? C13 Ru1 C12 37.5(3) . . ? N2 Ru1 C12 164.1(3) 7_566 . ? N1 Ru1 C12 109.6(3) . . ? C16 Ru1 C12 66.5(3) . . ? C15 Ru1 C14 37.2(3) . . ? C13 Ru1 C14 37.2(3) . . ? N2 Ru1 C14 96.2(3) 7_566 . ? N1 Ru1 C14 164.2(3) . . ? C16 Ru1 C14 67.6(4) . . ? C12 Ru1 C14 68.0(4) . . ? C15 Ru1 C11 66.8(4) . . ? C13 Ru1 C11 66.9(4) . . ? N2 Ru1 C11 145.6(3) 7_566 . ? N1 Ru1 C11 88.8(3) . . ? C16 Ru1 C11 37.3(3) . . ? C12 Ru1 C11 36.8(3) . . ? C14 Ru1 C11 80.5(4) . . ? C15 Ru1 Cl1 143.1(3) . . ? C13 Ru1 Cl1 86.4(3) . . ? N2 Ru1 Cl1 88.66(17) 7_566 . ? N1 Ru1 Cl1 89.25(18) . . ? C16 Ru1 Cl1 160.8(2) . . ? C12 Ru1 Cl1 94.3(3) . . ? C14 Ru1 Cl1 106.4(3) . . ? C11 Ru1 Cl1 125.3(3) . . ? C3 S1 S2 104.6(3) . . ? C6 S2 S1 105.0(3) . . ? C1 N1 C5 116.4(7) . . ? C1 N1 Ru1 122.6(5) . . ? C5 N1 Ru1 120.7(5) . . ? C9 N2 C8 116.3(7) . . ? C9 N2 Ru1 124.2(5) . 7_566 ? C8 N2 Ru1 119.5(5) . 7_566 ? N1 C1 C2 123.4(8) . . ? C1 C2 C3 118.1(8) . . ? C4 C3 C2 119.7(8) . . ? C4 C3 S1 125.4(7) . . ? C2 C3 S1 114.9(6) . . ? C3 C4 C5 120.3(8) . . ? N1 C5 C4 122.0(8) . . ? C10 C6 C7 117.1(8) . . ? C10 C6 S2 116.7(6) . . ? C7 C6 S2 126.2(6) . . ? C8 C7 C6 120.4(7) . . ? N2 C8 C7 122.9(8) . . ? N2 C9 C10 123.5(8) . . ? C9 C10 C6 119.7(8) . . ? C12 C11 C16 117.6(10) . . ? C12 C11 C17 122.0(10) . . ? C16 C11 C17 120.4(9) . . ? C12 C11 Ru1 70.4(5) . . ? C16 C11 Ru1 69.8(5) . . ? C17 C11 Ru1 130.0(6) . . ? C13 C12 C11 119.6(9) . . ? C13 C12 Ru1 69.7(5) . . ? C11 C12 Ru1 72.8(5) . . ? C14 C13 C12 123.7(9) . . ? C14 C13 Ru1 73.1(5) . . ? C12 C13 Ru1 72.9(5) . . ? C15 C14 C13 114.6(9) . . ? C15 C14 C20 121.9(9) . . ? C13 C14 C20 123.5(9) . . ? C15 C14 Ru1 69.2(5) . . ? C13 C14 Ru1 69.7(5) . . ? C20 C14 Ru1 131.3(7) . . ? C16 C15 C14 124.5(9) . . ? C16 C15 Ru1 73.3(5) . . ? C14 C15 Ru1 73.6(5) . . ? C15 C16 C11 120.0(9) . . ? C15 C16 Ru1 69.8(5) . . ? C11 C16 Ru1 73.0(5) . . ? C19 C17 C11 117.9(10) . . ? C19 C17 C18 112.1(10) . . ? C11 C17 C18 106.0(10) . . ? O2 S3 O1 114.6(7) . . ? O2 S3 O3 120.9(11) . . ? O1 S3 O3 115.5(8) . . ? O2 S3 C21 99.0(14) . . ? O1 S3 C21 105.0(11) . . ? O3 S3 C21 96.5(12) . . ? F1 C21 F3 103(3) . . ? F1 C21 F2 106(2) . . ? F3 C21 F2 117(3) . . ? F1 C21 S3 116(3) . . ? F3 C21 S3 109(2) . . ? F2 C21 S3 107(2) . . ? Cl3 C22 Cl2 111.6(7) . . ? Cl3 C22 Cl4 110.8(7) . . ? Cl2 C22 Cl4 108.8(7) . . ? Cl7 C23 Cl5 109.2(8) . . ? Cl7 C23 Cl6 110.5(9) . . ? Cl5 C23 Cl6 106.9(8) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 2.185 _refine_diff_density_min -1.285 _refine_diff_density_rms 0.139