# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Guo-Xin Jin' _publ_contact_author_email GXJIN@FUDAN.EDU.CN _publ_section_title ; Synthesis and Characterization of Molecular Rectangles of Half-Sandwich p-Cymene Ruthenium Complexes Bearing Oxamide Ligands ; loop_ _publ_author_name 'Guo-Xin Jin' 'Ying-Feng Han' 'Yue-Jian Lin' 'Wan-Zheng Zhang' # Attachment 'binuclear.cif' data_f80629c _database_code_depnum_ccdc_archive 'CCDC 731558' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H42 Cl6 N2 O2 Ru2' _chemical_formula_weight 949.56 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' 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.142(14) _cell_length_b 9.416(14) _cell_length_c 12.623(19) _cell_angle_alpha 103.083(19) _cell_angle_beta 97.87(2) _cell_angle_gamma 106.425(18) _cell_volume 991(3) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 717 _cell_measurement_theta_min 2.484 _cell_measurement_theta_max 25.560 _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 1.591 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 478 _exptl_absorpt_coefficient_mu 1.200 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8694 _exptl_absorpt_correction_T_max 0.9101 _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_% 9.40 _diffrn_reflns_number 4081 _diffrn_reflns_av_R_equivalents 0.0821 _diffrn_reflns_av_sigmaI/netI 0.0719 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.70 _diffrn_reflns_theta_max 25.01 _reflns_number_total 3401 _reflns_number_gt 2626 _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^)+(0.2000P)^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 3401 _refine_ls_number_parameters 220 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1189 _refine_ls_R_factor_gt 0.1030 _refine_ls_wR_factor_ref 0.2921 _refine_ls_wR_factor_gt 0.2720 _refine_ls_goodness_of_fit_ref 1.178 _refine_ls_restrained_S_all 1.178 _refine_ls_shift/su_max 0.003 _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 0.24521(9) 0.38768(9) 0.09031(6) 0.0383(4) Uani 1 1 d . . . Cl1 Cl 0.1814(4) 0.2041(4) -0.0896(2) 0.0607(8) Uani 1 1 d . . . N1 N 0.4743(9) 0.3861(10) 0.0908(7) 0.0384(18) Uani 1 1 d . . . O1 O 0.3277(8) 0.5472(8) 0.0031(6) 0.0420(16) Uani 1 1 d . . . C1 C 0.4570(11) 0.5456(10) -0.0252(8) 0.036(2) Uani 1 1 d . . . C2 C 0.5491(11) 0.3004(12) 0.1491(8) 0.042(2) Uani 1 1 d . . . C3 C 0.6855(13) 0.3762(15) 0.2296(9) 0.053(3) Uani 1 1 d . . . H3 H 0.7304 0.4826 0.2467 0.063 Uiso 1 1 calc R . . C4 C 0.7550(16) 0.2913(19) 0.2851(10) 0.066(3) Uani 1 1 d . . . H4 H 0.8469 0.3414 0.3390 0.079 Uiso 1 1 calc R . . C5 C 0.689(2) 0.135(2) 0.2605(13) 0.081(5) Uani 1 1 d . . . H5 H 0.7367 0.0788 0.2966 0.097 Uiso 1 1 calc R . . C6 C 0.549(2) 0.0595(16) 0.1809(13) 0.077(4) Uani 1 1 d . . . H6 H 0.5012 -0.0466 0.1643 0.092 Uiso 1 1 calc R . . C7 C 0.4825(15) 0.1465(15) 0.1278(11) 0.060(3) Uani 1 1 d . . . H7 H 0.3889 0.0975 0.0755 0.072 Uiso 1 1 calc R . . C8 C 0.0048(12) 0.2977(14) 0.1103(10) 0.049(3) Uani 1 1 d . . . C9 C 0.0428(11) 0.4539(13) 0.1318(9) 0.044(2) Uani 1 1 d . . . H9 H -0.0230 0.4970 0.0970 0.053 Uiso 1 1 calc R . . C10 C 0.1834(12) 0.5491(12) 0.2076(8) 0.043(2) Uani 1 1 d . . . H10 H 0.2091 0.6549 0.2182 0.052 Uiso 1 1 calc R . . C11 C 0.2860(13) 0.4975(12) 0.2675(8) 0.042(2) Uani 1 1 d . . . C12 C 0.2346(13) 0.3237(11) 0.2436(9) 0.046(3) Uani 1 1 d . . . H12 H 0.2937 0.2774 0.2812 0.055 Uiso 1 1 calc R . . C13 C 0.1013(12) 0.2354(10) 0.1666(10) 0.047(3) Uani 1 1 d . . . H13 H 0.0735 0.1287 0.1511 0.057 Uiso 1 1 calc R . . C14 C -0.1392(14) 0.1948(15) 0.0205(11) 0.065(3) Uani 1 1 d . . . H14A H -0.1291 0.0949 -0.0065 0.097 Uiso 1 1 calc R . . H14B H -0.1483 0.2401 -0.0400 0.097 Uiso 1 1 calc R . . H14C H -0.2307 0.1846 0.0514 0.097 Uiso 1 1 calc R . . C15 C 0.4332(13) 0.5955(10) 0.3522(10) 0.056(3) Uani 1 1 d . . . H15 H 0.5012 0.5319 0.3549 0.067 Uiso 1 1 calc R . . C16 C 0.3950(19) 0.634(2) 0.4669(10) 0.085(5) Uani 1 1 d . . . H16A H 0.4901 0.6866 0.5221 0.128 Uiso 1 1 calc R . . H16B H 0.3403 0.5402 0.4825 0.128 Uiso 1 1 calc R . . H16C H 0.3306 0.6987 0.4683 0.128 Uiso 1 1 calc R . . C17 C 0.5203(17) 0.7333(19) 0.3195(11) 0.080(4) Uani 1 1 d . . . H17A H 0.5491 0.7001 0.2500 0.120 Uiso 1 1 calc R . . H17B H 0.6128 0.7924 0.3760 0.120 Uiso 1 1 calc R . . H17C H 0.4551 0.7959 0.3116 0.120 Uiso 1 1 calc R . . C18 C 0.009(3) 0.863(4) 0.358(2) 0.195(17) Uani 1 1 d . . . H18A H -0.0361 0.8001 0.2818 0.234 Uiso 1 1 calc R . . H18B H -0.0499 0.9340 0.3749 0.234 Uiso 1 1 calc R . . Cl2 Cl -0.0164(11) 0.7445(11) 0.4457(7) 0.182(3) Uani 1 1 d . . . Cl3 Cl 0.1980(11) 0.9691(9) 0.3657(9) 0.187(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 0.0360(6) 0.0528(6) 0.0380(6) 0.0192(4) 0.0134(3) 0.0251(4) Cl1 0.0524(17) 0.0829(19) 0.0441(15) 0.0078(13) 0.0112(12) 0.0254(14) N1 0.031(4) 0.057(5) 0.040(4) 0.022(4) 0.012(3) 0.025(3) O1 0.042(4) 0.045(4) 0.062(4) 0.034(3) 0.024(3) 0.027(3) C1 0.041(5) 0.038(5) 0.036(5) 0.009(4) 0.011(4) 0.025(4) C2 0.038(5) 0.059(6) 0.041(5) 0.026(4) 0.012(4) 0.024(4) C3 0.052(7) 0.075(7) 0.042(6) 0.019(5) 0.013(5) 0.035(5) C4 0.071(9) 0.103(11) 0.048(7) 0.031(7) 0.019(6) 0.057(8) C5 0.103(12) 0.132(15) 0.083(10) 0.084(11) 0.050(9) 0.097(12) C6 0.104(12) 0.056(7) 0.099(11) 0.045(7) 0.028(9) 0.048(8) C7 0.054(7) 0.066(7) 0.074(8) 0.035(6) 0.017(6) 0.027(5) C8 0.034(5) 0.065(7) 0.065(7) 0.031(6) 0.022(5) 0.025(5) C9 0.032(5) 0.064(7) 0.050(6) 0.023(5) 0.016(4) 0.028(4) C10 0.045(6) 0.044(5) 0.042(6) 0.006(4) 0.015(4) 0.019(4) C11 0.053(6) 0.045(5) 0.033(5) 0.005(4) 0.019(4) 0.026(5) C12 0.057(6) 0.033(5) 0.063(7) 0.028(4) 0.025(5) 0.020(4) C13 0.047(6) 0.018(4) 0.079(8) 0.018(4) 0.030(5) 0.000(4) C14 0.046(7) 0.071(8) 0.076(9) 0.015(6) 0.019(6) 0.020(6) C15 0.053(6) 0.015(4) 0.076(8) 0.007(4) -0.005(6) -0.009(4) C16 0.096(11) 0.124(13) 0.036(7) 0.009(7) 0.006(7) 0.047(10) C17 0.068(9) 0.110(12) 0.053(8) 0.015(7) 0.003(6) 0.028(8) C18 0.16(2) 0.33(5) 0.081(15) -0.04(2) -0.033(15) 0.16(3) Cl2 0.202(8) 0.200(8) 0.137(6) 0.034(5) -0.022(5) 0.089(6) Cl3 0.172(7) 0.138(6) 0.227(10) 0.015(6) -0.006(6) 0.068(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 O1 2.091(6) . ? Ru1 N1 2.098(9) . ? Ru1 C10 2.126(10) . ? Ru1 C13 2.150(9) . ? Ru1 C12 2.159(10) . ? Ru1 C11 2.172(10) . ? Ru1 C8 2.192(11) . ? Ru1 C9 2.204(11) . ? Ru1 Cl1 2.403(4) . ? N1 C1 1.283(13) 2_665 ? N1 C2 1.450(13) . ? O1 C1 1.284(12) . ? C1 N1 1.283(13) 2_665 ? C1 C1 1.501(19) 2_665 ? C2 C7 1.350(15) . ? C2 C3 1.385(15) . ? C3 C4 1.397(18) . ? C4 C5 1.37(2) . ? C5 C6 1.40(2) . ? C6 C7 1.379(19) . ? C8 C9 1.364(16) . ? C8 C13 1.392(17) . ? C8 C14 1.526(16) . ? C9 C10 1.413(14) . ? C10 C11 1.385(16) . ? C11 C15 1.504(13) . ? C11 C12 1.514(14) . ? C12 C13 1.363(16) . ? C15 C17 1.495(18) . ? C15 C16 1.524(18) . ? C18 Cl3 1.71(3) . ? C18 Cl2 1.74(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Ru1 N1 77.2(3) . . ? O1 Ru1 C10 92.8(4) . . ? N1 Ru1 C10 124.4(4) . . ? O1 Ru1 C13 164.2(4) . . ? N1 Ru1 C13 118.5(4) . . ? C10 Ru1 C13 79.7(4) . . ? O1 Ru1 C12 151.3(4) . . ? N1 Ru1 C12 94.7(4) . . ? C10 Ru1 C12 68.9(4) . . ? C13 Ru1 C12 36.9(4) . . ? O1 Ru1 C11 111.8(4) . . ? N1 Ru1 C11 95.9(4) . . ? C10 Ru1 C11 37.6(4) . . ? C13 Ru1 C11 70.3(4) . . ? C12 Ru1 C11 40.9(4) . . ? O1 Ru1 C8 126.8(4) . . ? N1 Ru1 C8 154.9(4) . . ? C10 Ru1 C8 67.3(4) . . ? C13 Ru1 C8 37.4(4) . . ? C12 Ru1 C8 67.6(4) . . ? C11 Ru1 C8 82.4(4) . . ? O1 Ru1 C9 99.2(3) . . ? N1 Ru1 C9 162.4(4) . . ? C10 Ru1 C9 38.0(4) . . ? C13 Ru1 C9 66.4(4) . . ? C12 Ru1 C9 80.1(4) . . ? C11 Ru1 C9 69.2(4) . . ? C8 Ru1 C9 36.2(4) . . ? O1 Ru1 Cl1 83.5(3) . . ? N1 Ru1 Cl1 84.8(2) . . ? C10 Ru1 Cl1 149.1(3) . . ? C13 Ru1 Cl1 95.7(3) . . ? C12 Ru1 Cl1 123.6(3) . . ? C11 Ru1 Cl1 164.5(3) . . ? C8 Ru1 Cl1 90.4(3) . . ? C9 Ru1 Cl1 112.1(3) . . ? C1 N1 C2 119.8(8) 2_665 . ? C1 N1 Ru1 115.4(7) 2_665 . ? C2 N1 Ru1 124.5(6) . . ? C1 O1 Ru1 114.1(6) . . ? N1 C1 O1 128.7(9) 2_665 . ? N1 C1 C1 114.4(11) 2_665 2_665 ? O1 C1 C1 116.9(10) . 2_665 ? C7 C2 C3 119.7(10) . . ? C7 C2 N1 119.8(9) . . ? C3 C2 N1 120.5(10) . . ? C2 C3 C4 119.4(13) . . ? C5 C4 C3 120.4(13) . . ? C4 C5 C6 119.9(11) . . ? C7 C6 C5 118.3(13) . . ? C2 C7 C6 122.2(13) . . ? C9 C8 C13 119.7(10) . . ? C9 C8 C14 118.9(11) . . ? C13 C8 C14 121.3(11) . . ? C9 C8 Ru1 72.4(6) . . ? C13 C8 Ru1 69.6(6) . . ? C14 C8 Ru1 127.8(8) . . ? C8 C9 C10 119.0(10) . . ? C8 C9 Ru1 71.5(6) . . ? C10 C9 Ru1 68.0(6) . . ? C11 C10 C9 125.2(10) . . ? C11 C10 Ru1 73.0(6) . . ? C9 C10 Ru1 74.0(6) . . ? C10 C11 C15 126.7(10) . . ? C10 C11 C12 113.3(9) . . ? C15 C11 C12 120.0(10) . . ? C10 C11 Ru1 69.4(6) . . ? C15 C11 Ru1 131.7(8) . . ? C12 C11 Ru1 69.1(5) . . ? C13 C12 C11 119.7(10) . . ? C13 C12 Ru1 71.2(6) . . ? C11 C12 Ru1 70.0(5) . . ? C12 C13 C8 122.9(9) . . ? C12 C13 Ru1 71.9(5) . . ? C8 C13 Ru1 73.0(6) . . ? C17 C15 C11 112.5(10) . . ? C17 C15 C16 114.1(10) . . ? C11 C15 C16 109.3(10) . . ? Cl3 C18 Cl2 115.3(16) . . ? _diffrn_measured_fraction_theta_max 0.973 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.973 _refine_diff_density_max 2.845 _refine_diff_density_min -3.458 _refine_diff_density_rms 0.250 # Attachment 'bpe.cif' data_f81023d _database_code_depnum_ccdc_archive 'CCDC 731559' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C100 H106 F12 N8 O17 Ru4 S4' _chemical_formula_weight 2452.45 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' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pccn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-x, y+1/2, -z+1/2' 'x+1/2, -y, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'x, -y-1/2, z-1/2' '-x-1/2, y, z-1/2' _cell_length_a 16.560(5) _cell_length_b 41.448(13) _cell_length_c 15.582(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 10695(6) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 984 _cell_measurement_theta_min 2.956 _cell_measurement_theta_max 22.094 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.523 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4984 _exptl_absorpt_coefficient_mu 0.719 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9187 _exptl_absorpt_correction_T_max 0.9315 _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_% 99.01 _diffrn_reflns_number 49321 _diffrn_reflns_av_R_equivalents 0.0881 _diffrn_reflns_av_sigmaI/netI 0.1167 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -46 _diffrn_reflns_limit_k_max 51 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.32 _diffrn_reflns_theta_max 27.11 _reflns_number_total 11652 _reflns_number_gt 5426 _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^)+(0.1058P)^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 11652 _refine_ls_number_parameters 661 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1540 _refine_ls_R_factor_gt 0.0747 _refine_ls_wR_factor_ref 0.2097 _refine_ls_wR_factor_gt 0.1841 _refine_ls_goodness_of_fit_ref 0.955 _refine_ls_restrained_S_all 0.955 _refine_ls_shift/su_max 0.006 _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 0.42599(3) 0.102968(14) 1.05817(4) 0.04659(19) Uani 1 1 d . . . Ru2 Ru 0.49810(4) 0.118450(15) 0.71206(4) 0.04874(19) Uani 1 1 d . . . N1 N 0.3782(3) 0.09347(13) 0.9348(3) 0.0432(13) Uani 1 1 d . . . N2 N 0.5371(3) 0.13278(13) 0.8343(4) 0.0449(14) Uani 1 1 d . . . N3 N 0.3787(4) 0.15028(14) 1.0438(4) 0.0553(16) Uani 1 1 d . . . N4 N 0.4244(4) 0.16084(14) 0.7159(4) 0.0528(15) Uani 1 1 d . . . O1 O 0.5166(2) 0.12116(11) 0.9764(3) 0.0456(12) Uani 1 1 d . . . O2 O 0.4094(3) 0.09886(11) 0.7920(3) 0.0499(12) Uani 1 1 d . . . O3 O 0.7254(13) 0.0128(3) 0.8661(10) 0.341(12) Uani 1 1 d . . . O4 O 0.6452(6) 0.0228(2) 0.9854(7) 0.171(4) Uani 1 1 d . . . O5 O 0.6561(10) 0.0614(3) 0.8783(9) 0.298(10) Uani 1 1 d . . . O6 O 0.5089(7) 0.1524(2) 0.3670(6) 0.188(5) Uani 1 1 d . . . O7 O 0.4225(10) 0.1843(5) 0.4620(10) 0.340(13) Uani 1 1 d . . . O8 O 0.3880(9) 0.1782(3) 0.3151(13) 0.293(10) Uani 1 1 d . . . S1 S 0.6918(3) 0.03627(8) 0.9167(3) 0.1442(15) Uani 1 1 d . . . S2 S 0.4420(2) 0.17790(9) 0.3738(3) 0.1249(12) Uani 1 1 d D . . F1 F 0.8292(8) 0.0663(4) 0.9096(9) 0.279(8) Uani 1 1 d . . . F2 F 0.8188(7) 0.0363(3) 1.0118(10) 0.276(7) Uani 1 1 d . . . F3 F 0.7651(5) 0.0784(3) 1.0117(7) 0.214(5) Uani 1 1 d . . . F4 F 0.4461(8) 0.2372(2) 0.3690(7) 0.234(5) Uani 1 1 d . . . F5 F 0.5554(8) 0.2139(3) 0.4027(14) 0.336(11) Uani 1 1 d . . . F6 F 0.5172(15) 0.2071(6) 0.2806(11) 0.427(18) Uani 1 1 d . . . C1 C 0.4989(4) 0.11955(16) 0.8997(4) 0.0388(15) Uani 1 1 d . . . C2 C 0.4246(4) 0.10207(15) 0.8732(4) 0.0347(14) Uani 1 1 d . . . C3 C 0.3019(5) 0.07857(18) 0.9142(5) 0.0516(19) Uani 1 1 d . . . C4 C 0.2331(4) 0.0969(2) 0.9029(5) 0.058(2) Uani 1 1 d . . . H4 H 0.2370 0.1192 0.9066 0.070 Uiso 1 1 calc R . . C5 C 0.1587(5) 0.0832(3) 0.8864(5) 0.087(3) Uani 1 1 d . . . H5 H 0.1116 0.0954 0.8837 0.104 Uiso 1 1 calc R . . C6 C 0.1585(8) 0.0492(4) 0.8738(7) 0.112(4) Uani 1 1 d . . . H6 H 0.1105 0.0391 0.8585 0.135 Uiso 1 1 calc R . . C7 C 0.2231(8) 0.0318(3) 0.8827(8) 0.120(5) Uani 1 1 d . . . H7 H 0.2200 0.0096 0.8754 0.144 Uiso 1 1 calc R . . C8 C 0.2975(6) 0.0460(2) 0.9033(6) 0.088(3) Uani 1 1 d . . . H8 H 0.3434 0.0333 0.9093 0.106 Uiso 1 1 calc R . . C9 C 0.6074(4) 0.15190(19) 0.8523(5) 0.0532(19) Uani 1 1 d . . . C10 C 0.6826(5) 0.1391(2) 0.8636(6) 0.074(2) Uani 1 1 d . . . H10 H 0.6896 0.1168 0.8630 0.089 Uiso 1 1 calc R . . C11 C 0.7482(6) 0.1590(3) 0.8760(7) 0.103(4) Uani 1 1 d . . . H11 H 0.7989 0.1497 0.8829 0.123 Uiso 1 1 calc R . . C12 C 0.7417(8) 0.1910(4) 0.8783(8) 0.121(4) Uani 1 1 d . . . H12 H 0.7868 0.2038 0.8887 0.145 Uiso 1 1 calc R . . C13 C 0.6657(9) 0.2051(3) 0.8648(9) 0.133(5) Uani 1 1 d . . . H13 H 0.6606 0.2275 0.8642 0.160 Uiso 1 1 calc R . . C14 C 0.5986(6) 0.1861(2) 0.8523(7) 0.086(3) Uani 1 1 d . . . H14 H 0.5481 0.1954 0.8441 0.103 Uiso 1 1 calc R . . C15 C 0.3003(5) 0.15622(19) 1.0446(5) 0.061(2) Uani 1 1 d . . . H15 H 0.2654 0.1391 1.0550 0.073 Uiso 1 1 calc R . . C16 C 0.2677(5) 0.1858(2) 1.0313(6) 0.074(3) Uani 1 1 d . . . H16 H 0.2119 0.1881 1.0287 0.088 Uiso 1 1 calc R . . C17 C 0.3170(6) 0.2123(2) 1.0215(5) 0.069(2) Uani 1 1 d . . . C18 C 0.3991(6) 0.2068(2) 1.0225(6) 0.080(3) Uani 1 1 d . . . H18 H 0.4350 0.2238 1.0156 0.096 Uiso 1 1 calc R . . C19 C 0.4282(5) 0.1755(2) 1.0337(6) 0.077(3) Uani 1 1 d . . . H19 H 0.4837 0.1721 1.0341 0.092 Uiso 1 1 calc R . . C20 C 0.2874(5) 0.2455(2) 1.0147(5) 0.077(3) Uani 1 1 d . . . H20 H 0.3260 0.2617 1.0098 0.092 Uiso 1 1 calc R . . C21 C 0.3486(5) 0.16078(19) 0.7423(5) 0.058(2) Uani 1 1 d . . . H21 H 0.3249 0.1410 0.7547 0.070 Uiso 1 1 calc R . . C22 C 0.3019(5) 0.1886(2) 0.7529(5) 0.067(2) Uani 1 1 d . . . H22 H 0.2495 0.1872 0.7741 0.080 Uiso 1 1 calc R . . C23 C 0.3338(5) 0.2175(2) 0.7320(5) 0.061(2) Uani 1 1 d . . . C24 C 0.4118(6) 0.2179(2) 0.7045(7) 0.089(3) Uani 1 1 d . . . H24 H 0.4359 0.2374 0.6901 0.107 Uiso 1 1 calc R . . C25 C 0.4557(5) 0.1895(2) 0.6976(6) 0.077(3) Uani 1 1 d . . . H25 H 0.5091 0.1907 0.6795 0.092 Uiso 1 1 calc R . . C26 C 0.2884(5) 0.2489(2) 0.7374(5) 0.074(3) Uani 1 1 d . . . H26 H 0.3182 0.2679 0.7410 0.088 Uiso 1 1 calc R . . C27 C 0.5197(5) 0.0862(3) 1.1459(5) 0.070(3) Uani 1 1 d . . . C28 C 0.4678(6) 0.1066(2) 1.1917(5) 0.073(2) Uani 1 1 d . . . H28 H 0.4888 0.1235 1.2237 0.087 Uiso 1 1 calc R . . C29 C 0.3824(6) 0.1013(2) 1.1894(5) 0.069(2) Uani 1 1 d . . . H29 H 0.3485 0.1155 1.2181 0.083 Uiso 1 1 calc R . . C30 C 0.3486(5) 0.0753(2) 1.1451(5) 0.061(2) Uani 1 1 d . . . C31 C 0.4020(5) 0.0539(2) 1.1038(5) 0.068(2) Uani 1 1 d . . . H31 H 0.3806 0.0359 1.0764 0.082 Uiso 1 1 calc R . . C32 C 0.4853(5) 0.0584(2) 1.1020(5) 0.064(2) Uani 1 1 d . . . H32 H 0.5185 0.0438 1.0733 0.077 Uiso 1 1 calc R . . C33 C 0.6099(6) 0.0912(3) 1.1397(7) 0.099(4) Uani 1 1 d . . . H33 H 0.6273 0.0851 1.0819 0.119 Uiso 1 1 calc R . . C34 C 0.6331(7) 0.1266(3) 1.1545(9) 0.157(6) Uani 1 1 d . . . H34A H 0.6145 0.1334 1.2101 0.236 Uiso 1 1 calc R . . H34B H 0.6085 0.1398 1.1111 0.236 Uiso 1 1 calc R . . H34C H 0.6907 0.1288 1.1517 0.236 Uiso 1 1 calc R . . C35 C 0.6504(7) 0.0688(4) 1.2036(11) 0.212(9) Uani 1 1 d . . . H35A H 0.6587 0.0801 1.2568 0.318 Uiso 1 1 calc R . . H35B H 0.7015 0.0619 1.1811 0.318 Uiso 1 1 calc R . . H35C H 0.6166 0.0504 1.2133 0.318 Uiso 1 1 calc R . . C36 C 0.2586(5) 0.0687(2) 1.1466(6) 0.091(3) Uani 1 1 d . . . H36A H 0.2300 0.0886 1.1546 0.136 Uiso 1 1 calc R . . H36B H 0.2463 0.0543 1.1929 0.136 Uiso 1 1 calc R . . H36C H 0.2426 0.0591 1.0932 0.136 Uiso 1 1 calc R . . C37 C 0.5074(5) 0.0710(2) 0.6509(6) 0.066(2) Uani 1 1 d . . . C38 C 0.4724(6) 0.0912(3) 0.5954(6) 0.089(3) Uani 1 1 d . . . H38 H 0.4225 0.0860 0.5719 0.107 Uiso 1 1 calc R . . C39 C 0.5098(7) 0.1203(3) 0.5720(5) 0.090(4) Uani 1 1 d . . . H39 H 0.4858 0.1335 0.5310 0.108 Uiso 1 1 calc R . . C40 C 0.5863(6) 0.1302(2) 0.6114(6) 0.080(3) Uani 1 1 d . . . C41 C 0.6198(5) 0.1076(2) 0.6702(6) 0.071(2) Uani 1 1 d . . . H41 H 0.6687 0.1123 0.6970 0.085 Uiso 1 1 calc R . . C42 C 0.5802(5) 0.0784(2) 0.6884(5) 0.064(2) Uani 1 1 d . . . H42 H 0.6037 0.0639 0.7264 0.077 Uiso 1 1 calc R . . C43 C 0.4609(6) 0.0389(3) 0.6798(8) 0.095(3) Uani 1 1 d . . . H43 H 0.4039 0.0443 0.6886 0.115 Uiso 1 1 calc R . . C44 C 0.4914(9) 0.0219(3) 0.7597(9) 0.143(5) Uani 1 1 d . . . H44A H 0.5453 0.0142 0.7499 0.214 Uiso 1 1 calc R . . H44B H 0.4567 0.0040 0.7727 0.214 Uiso 1 1 calc R . . H44C H 0.4915 0.0367 0.8070 0.214 Uiso 1 1 calc R . . C45 C 0.4667(10) 0.0168(4) 0.6032(11) 0.203(8) Uani 1 1 d . . . H45A H 0.5221 0.0111 0.5935 0.304 Uiso 1 1 calc R . . H45B H 0.4458 0.0276 0.5534 0.304 Uiso 1 1 calc R . . H45C H 0.4357 -0.0024 0.6137 0.304 Uiso 1 1 calc R . . C46 C 0.6328(8) 0.1603(3) 0.5938(10) 0.166(7) Uani 1 1 d . . . H46A H 0.6343 0.1734 0.6447 0.249 Uiso 1 1 calc R . . H46B H 0.6070 0.1721 0.5484 0.249 Uiso 1 1 calc R . . H46C H 0.6868 0.1549 0.5770 0.249 Uiso 1 1 calc R . . C47 C 0.7795(11) 0.0551(4) 0.9658(10) 0.130(5) Uani 1 1 d . . . C48 C 0.5005(10) 0.2146(3) 0.3688(19) 0.240(16) Uani 1 1 d D . . O9 O 0.7500 0.2500 0.6180(16) 0.293(13) Uani 1 2 d S . . C49 C 0.6878(17) 0.2680(12) 0.662(3) 0.47(3) Uani 1 1 d . . . H49A H 0.6780 0.2589 0.7181 0.564 Uiso 1 1 calc R . . H49B H 0.7042 0.2903 0.6686 0.564 Uiso 1 1 calc R . . C50 C 0.6193(13) 0.2663(7) 0.6129(18) 0.298(16) Uani 1 1 d . . . H50A H 0.6298 0.2535 0.5626 0.447 Uiso 1 1 calc R . . H50B H 0.6032 0.2876 0.5960 0.447 Uiso 1 1 calc R . . H50C H 0.5769 0.2564 0.6457 0.447 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 0.0468(3) 0.0549(4) 0.0381(3) 0.0033(3) -0.0008(3) -0.0001(3) Ru2 0.0505(4) 0.0581(4) 0.0376(3) 0.0016(3) 0.0032(3) 0.0152(3) N1 0.046(3) 0.048(3) 0.036(3) 0.003(3) 0.000(3) 0.006(3) N2 0.042(3) 0.047(3) 0.045(4) 0.005(3) 0.007(3) 0.004(3) N3 0.054(4) 0.052(4) 0.060(4) -0.006(3) -0.007(3) -0.005(3) N4 0.050(4) 0.049(4) 0.060(4) 0.010(3) 0.008(3) 0.011(3) O1 0.039(3) 0.056(3) 0.041(3) 0.002(2) 0.002(2) 0.002(2) O2 0.057(3) 0.062(3) 0.031(3) -0.013(2) -0.006(2) 0.002(2) O3 0.54(3) 0.148(11) 0.34(2) -0.124(12) 0.21(2) -0.113(14) O4 0.196(10) 0.160(9) 0.158(9) 0.032(8) 0.032(8) 0.034(7) O5 0.44(2) 0.127(8) 0.330(18) 0.126(10) -0.284(17) -0.097(11) O6 0.295(13) 0.131(8) 0.140(8) -0.018(6) -0.037(8) 0.111(8) O7 0.32(2) 0.45(3) 0.251(16) 0.200(16) 0.183(15) 0.277(19) O8 0.234(14) 0.181(12) 0.46(3) 0.039(13) -0.238(18) 0.025(10) S1 0.254(5) 0.071(2) 0.107(3) 0.008(2) -0.022(3) -0.010(3) S2 0.111(3) 0.121(3) 0.142(3) 0.010(2) -0.022(2) -0.005(2) F1 0.305(16) 0.341(18) 0.191(11) 0.011(11) 0.103(11) -0.101(13) F2 0.193(10) 0.239(12) 0.396(19) 0.165(13) -0.047(11) 0.033(9) F3 0.124(7) 0.321(14) 0.198(10) -0.111(10) -0.045(6) -0.001(8) F4 0.345(14) 0.142(8) 0.216(12) -0.024(7) -0.085(11) 0.069(9) F5 0.164(11) 0.225(13) 0.62(3) 0.048(17) -0.147(17) -0.070(9) F6 0.51(4) 0.53(4) 0.239(18) 0.127(19) 0.21(2) 0.16(3) C1 0.044(4) 0.056(4) 0.016(3) 0.003(3) -0.004(3) 0.008(3) C2 0.043(4) 0.032(3) 0.029(3) 0.000(3) -0.005(3) 0.005(3) C3 0.059(5) 0.052(5) 0.043(4) 0.012(3) -0.006(4) -0.011(4) C4 0.047(5) 0.073(6) 0.055(5) 0.005(4) -0.009(4) -0.008(4) C5 0.054(6) 0.150(10) 0.057(6) 0.026(6) -0.020(4) -0.002(6) C6 0.105(10) 0.139(12) 0.093(8) 0.039(8) -0.039(7) -0.058(9) C7 0.141(11) 0.077(8) 0.143(11) 0.027(7) -0.074(9) -0.056(8) C8 0.107(8) 0.064(6) 0.095(7) 0.014(5) -0.039(6) -0.007(5) C9 0.047(4) 0.070(5) 0.043(4) 0.003(4) 0.010(3) 0.000(4) C10 0.053(5) 0.083(6) 0.086(7) 0.001(5) -0.014(5) -0.001(5) C11 0.052(6) 0.118(10) 0.138(10) -0.019(8) -0.010(6) -0.009(6) C12 0.088(9) 0.119(11) 0.156(12) -0.013(9) -0.004(8) -0.047(8) C13 0.135(12) 0.067(7) 0.198(15) 0.002(8) -0.026(11) -0.032(8) C14 0.077(6) 0.056(6) 0.125(9) -0.003(5) -0.003(6) -0.005(5) C15 0.055(5) 0.062(5) 0.065(6) -0.004(4) 0.006(4) 0.005(4) C16 0.056(5) 0.082(7) 0.084(7) -0.012(5) 0.002(5) 0.016(5) C17 0.081(7) 0.057(5) 0.069(6) -0.001(4) 0.004(5) 0.007(5) C18 0.071(6) 0.059(6) 0.110(8) -0.015(5) 0.004(5) -0.005(5) C19 0.057(5) 0.055(5) 0.118(8) -0.009(5) -0.001(5) -0.001(4) C20 0.088(7) 0.069(6) 0.073(6) -0.005(5) -0.002(5) 0.008(5) C21 0.051(5) 0.058(5) 0.066(5) 0.000(4) -0.004(4) 0.012(4) C22 0.054(5) 0.069(6) 0.077(6) 0.012(5) 0.007(4) 0.016(5) C23 0.064(5) 0.058(5) 0.062(5) 0.002(4) 0.004(4) 0.021(4) C24 0.078(7) 0.059(6) 0.130(9) 0.006(6) 0.008(6) 0.015(5) C25 0.057(5) 0.070(6) 0.103(8) 0.016(5) 0.023(5) 0.022(5) C26 0.070(6) 0.071(6) 0.080(6) -0.003(5) -0.008(4) 0.027(5) C27 0.052(5) 0.122(8) 0.036(5) 0.026(5) -0.003(4) 0.000(5) C28 0.088(7) 0.091(7) 0.039(5) 0.006(4) 0.000(5) -0.024(6) C29 0.080(6) 0.085(6) 0.041(5) 0.003(4) 0.010(4) 0.007(5) C30 0.062(5) 0.087(6) 0.033(4) 0.012(4) -0.001(4) -0.004(5) C31 0.083(7) 0.064(6) 0.057(5) 0.021(4) -0.005(5) -0.005(5) C32 0.067(6) 0.064(5) 0.060(5) 0.012(4) -0.010(4) 0.010(4) C33 0.059(6) 0.154(10) 0.084(7) 0.036(7) -0.028(5) -0.010(6) C34 0.102(10) 0.191(15) 0.179(14) 0.013(12) -0.062(9) -0.060(10) C35 0.084(9) 0.27(2) 0.28(2) 0.156(17) -0.093(11) -0.021(10) C36 0.059(6) 0.121(8) 0.093(7) 0.026(6) 0.014(5) -0.020(5) C37 0.063(6) 0.069(6) 0.066(6) -0.012(4) -0.004(5) 0.022(5) C38 0.080(7) 0.146(10) 0.041(5) -0.022(6) 0.012(5) 0.008(7) C39 0.100(8) 0.139(10) 0.030(5) 0.014(5) 0.031(5) 0.067(7) C40 0.084(7) 0.096(7) 0.061(6) 0.010(5) 0.037(5) 0.021(6) C41 0.057(5) 0.081(7) 0.074(6) -0.008(5) 0.024(5) 0.024(5) C42 0.072(6) 0.063(5) 0.057(5) -0.006(4) 0.003(5) 0.035(5) C43 0.077(6) 0.083(7) 0.126(10) -0.048(7) -0.004(7) 0.011(6) C44 0.200(15) 0.085(9) 0.143(13) 0.004(8) 0.017(11) 0.003(9) C45 0.199(15) 0.149(13) 0.26(2) -0.121(14) -0.067(15) 0.034(12) C46 0.165(12) 0.110(10) 0.222(16) 0.065(10) 0.143(12) 0.029(9) C47 0.192(16) 0.094(10) 0.103(11) 0.008(8) -0.025(11) 0.027(10) C48 0.173(19) 0.131(15) 0.42(4) -0.07(2) -0.18(3) 0.071(15) O9 0.35(4) 0.32(3) 0.21(2) 0.000 0.000 0.02(3) C49 0.16(3) 0.70(9) 0.55(8) -0.20(6) 0.04(3) -0.04(4) C50 0.16(2) 0.43(4) 0.31(3) 0.06(3) 0.03(2) 0.05(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 O1 2.109(4) . ? Ru1 N1 2.116(5) . ? Ru1 N3 2.124(6) . ? Ru1 C29 2.169(8) . ? Ru1 C27 2.182(7) . ? Ru1 C30 2.190(8) . ? Ru1 C31 2.192(8) . ? Ru1 C28 2.198(8) . ? Ru1 C32 2.203(8) . ? Ru2 O2 2.090(5) . ? Ru2 N2 2.097(6) . ? Ru2 N4 2.140(6) . ? Ru2 C41 2.166(7) . ? Ru2 C42 2.176(7) . ? Ru2 C38 2.181(9) . ? Ru2 C37 2.192(8) . ? Ru2 C39 2.193(8) . ? Ru2 C40 2.197(8) . ? N1 C2 1.281(8) . ? N1 C3 1.443(9) . ? N2 C1 1.318(8) . ? N2 C9 1.436(9) . ? N3 C15 1.322(9) . ? N3 C19 1.339(9) . ? N4 C21 1.321(9) . ? N4 C25 1.328(10) . ? O1 C1 1.232(7) . ? O2 C2 1.295(7) . ? O3 S1 1.371(13) . ? O4 S1 1.432(10) . ? O5 S1 1.340(10) . ? O6 S2 1.533(9) . ? O7 S2 1.436(15) . ? O8 S2 1.279(11) . ? S1 C47 1.819(17) . ? S2 C48 1.806(10) . ? F1 C47 1.288(18) . ? F2 C47 1.244(14) . ? F3 C47 1.223(14) . ? F4 C48 1.299(17) . ? F5 C48 1.053(16) . ? F6 C48 1.44(3) . ? C1 C2 1.487(9) . ? C3 C8 1.362(11) . ? C3 C4 1.381(10) . ? C4 C5 1.381(11) . ? C5 C6 1.423(15) . ? C6 C7 1.297(15) . ? C7 C8 1.403(13) . ? C9 C10 1.366(10) . ? C9 C14 1.424(11) . ? C10 C11 1.377(12) . ? C11 C12 1.334(15) . ? C12 C13 1.404(16) . ? C13 C14 1.376(13) . ? C15 C16 1.354(10) . ? C16 C17 1.378(11) . ? C17 C18 1.381(11) . ? C17 C20 1.465(11) . ? C18 C19 1.391(11) . ? C20 C20 1.291(15) 2 ? C21 C22 1.400(10) . ? C22 C23 1.348(11) . ? C23 C24 1.360(11) . ? C23 C26 1.506(11) . ? C24 C25 1.385(11) . ? C26 C26 1.276(15) 2 ? C27 C28 1.401(12) . ? C27 C32 1.457(12) . ? C27 C33 1.511(12) . ? C28 C29 1.431(12) . ? C29 C30 1.396(11) . ? C30 C31 1.408(11) . ? C30 C36 1.515(11) . ? C31 C32 1.392(11) . ? C33 C35 1.517(14) . ? C33 C34 1.534(15) . ? C37 C38 1.337(13) . ? C37 C42 1.375(11) . ? C37 C43 1.602(14) . ? C38 C39 1.404(14) . ? C39 C40 1.467(14) . ? C40 C41 1.421(12) . ? C40 C46 1.493(14) . ? C41 C42 1.406(11) . ? C43 C45 1.507(15) . ? C43 C44 1.516(16) . ? O9 C49 1.44(3) 2_655 ? O9 C49 1.44(3) . ? C49 C50 1.37(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Ru1 N1 77.53(19) . . ? O1 Ru1 N3 82.4(2) . . ? N1 Ru1 N3 86.4(2) . . ? O1 Ru1 C29 144.9(3) . . ? N1 Ru1 C29 136.5(3) . . ? N3 Ru1 C29 90.4(3) . . ? O1 Ru1 C27 89.2(2) . . ? N1 Ru1 C27 140.9(3) . . ? N3 Ru1 C27 128.5(3) . . ? C29 Ru1 C27 68.6(3) . . ? O1 Ru1 C30 167.9(3) . . ? N1 Ru1 C30 104.2(3) . . ? N3 Ru1 C30 109.5(3) . . ? C29 Ru1 C30 37.4(3) . . ? C27 Ru1 C30 82.0(3) . . ? O1 Ru1 C31 131.1(3) . . ? N1 Ru1 C31 93.1(3) . . ? N3 Ru1 C31 145.6(3) . . ? C29 Ru1 C31 66.7(3) . . ? C27 Ru1 C31 68.3(3) . . ? C30 Ru1 C31 37.5(3) . . ? O1 Ru1 C28 108.9(3) . . ? N1 Ru1 C28 172.1(3) . . ? N3 Ru1 C28 98.8(3) . . ? C29 Ru1 C28 38.2(3) . . ? C27 Ru1 C28 37.3(3) . . ? C30 Ru1 C28 68.5(3) . . ? C31 Ru1 C28 79.2(3) . . ? O1 Ru1 C32 99.8(3) . . ? N1 Ru1 C32 107.0(3) . . ? N3 Ru1 C32 166.5(3) . . ? C29 Ru1 C32 80.1(3) . . ? C27 Ru1 C32 38.8(3) . . ? C30 Ru1 C32 68.2(3) . . ? C31 Ru1 C32 36.9(3) . . ? C28 Ru1 C32 67.8(3) . . ? O2 Ru2 N2 77.57(19) . . ? O2 Ru2 N4 84.4(2) . . ? N2 Ru2 N4 85.3(2) . . ? O2 Ru2 C41 138.9(3) . . ? N2 Ru2 C41 92.6(3) . . ? N4 Ru2 C41 135.2(3) . . ? O2 Ru2 C42 104.1(3) . . ? N2 Ru2 C42 100.2(3) . . ? N4 Ru2 C42 170.7(3) . . ? C41 Ru2 C42 37.8(3) . . ? O2 Ru2 C38 99.1(3) . . ? N2 Ru2 C38 164.5(4) . . ? N4 Ru2 C38 109.7(3) . . ? C41 Ru2 C38 79.8(4) . . ? C42 Ru2 C38 65.6(4) . . ? O2 Ru2 C37 87.7(3) . . ? N2 Ru2 C37 128.9(3) . . ? N4 Ru2 C37 142.1(3) . . ? C41 Ru2 C37 67.6(3) . . ? C42 Ru2 C37 36.7(3) . . ? C38 Ru2 C37 35.6(4) . . ? O2 Ru2 C39 132.0(4) . . ? N2 Ru2 C39 150.1(4) . . ? N4 Ru2 C39 92.8(3) . . ? C41 Ru2 C39 68.0(3) . . ? C42 Ru2 C39 78.6(3) . . ? C38 Ru2 C39 37.4(4) . . ? C37 Ru2 C39 66.0(4) . . ? O2 Ru2 C40 168.1(3) . . ? N2 Ru2 C40 112.4(3) . . ? N4 Ru2 C40 102.5(3) . . ? C41 Ru2 C40 38.0(3) . . ? C42 Ru2 C40 68.4(3) . . ? C38 Ru2 C40 69.5(4) . . ? C37 Ru2 C40 80.9(4) . . ? C39 Ru2 C40 39.0(4) . . ? C2 N1 C3 118.5(6) . . ? C2 N1 Ru1 113.9(4) . . ? C3 N1 Ru1 127.6(4) . . ? C1 N2 C9 117.8(6) . . ? C1 N2 Ru2 115.9(4) . . ? C9 N2 Ru2 125.7(4) . . ? C15 N3 C19 117.2(7) . . ? C15 N3 Ru1 122.2(5) . . ? C19 N3 Ru1 120.6(5) . . ? C21 N4 C25 116.1(7) . . ? C21 N4 Ru2 123.3(5) . . ? C25 N4 Ru2 120.5(5) . . ? C1 O1 Ru1 113.4(4) . . ? C2 O2 Ru2 113.9(4) . . ? O5 S1 O3 118.3(12) . . ? O5 S1 O4 113.6(10) . . ? O3 S1 O4 111.9(8) . . ? O5 S1 C47 101.9(7) . . ? O3 S1 C47 102.8(11) . . ? O4 S1 C47 106.4(8) . . ? O8 S2 O7 121.6(12) . . ? O8 S2 O6 117.6(9) . . ? O7 S2 O6 110.9(6) . . ? O8 S2 C48 109.5(10) . . ? O7 S2 C48 90.3(13) . . ? O6 S2 C48 101.0(8) . . ? O1 C1 N2 127.8(6) . . ? O1 C1 C2 119.6(6) . . ? N2 C1 C2 112.6(5) . . ? N1 C2 O2 125.9(6) . . ? N1 C2 C1 115.0(5) . . ? O2 C2 C1 118.8(6) . . ? C8 C3 C4 119.0(8) . . ? C8 C3 N1 119.9(7) . . ? C4 C3 N1 121.0(7) . . ? C3 C4 C5 122.3(8) . . ? C4 C5 C6 115.7(9) . . ? C7 C6 C5 122.4(10) . . ? C6 C7 C8 120.9(11) . . ? C3 C8 C7 119.5(9) . . ? C10 C9 C14 118.7(8) . . ? C10 C9 N2 123.4(7) . . ? C14 C9 N2 117.8(7) . . ? C9 C10 C11 120.3(9) . . ? C12 C11 C10 122.5(10) . . ? C11 C12 C13 118.8(10) . . ? C14 C13 C12 120.5(11) . . ? C13 C14 C9 119.2(9) . . ? N3 C15 C16 123.9(8) . . ? C15 C16 C17 120.3(8) . . ? C16 C17 C18 116.6(8) . . ? C16 C17 C20 124.1(9) . . ? C18 C17 C20 119.2(8) . . ? C17 C18 C19 119.8(8) . . ? N3 C19 C18 122.0(8) . . ? C20 C20 C17 126.2(12) 2 . ? N4 C21 C22 124.1(8) . . ? C23 C22 C21 119.1(8) . . ? C22 C23 C24 117.3(8) . . ? C22 C23 C26 123.9(8) . . ? C24 C23 C26 118.8(8) . . ? C23 C24 C25 120.9(9) . . ? N4 C25 C24 122.5(8) . . ? C26 C26 C23 124.0(12) 2 . ? C28 C27 C32 118.5(8) . . ? C28 C27 C33 123.8(10) . . ? C32 C27 C33 117.7(9) . . ? C28 C27 Ru1 72.0(5) . . ? C32 C27 Ru1 71.4(4) . . ? C33 C27 Ru1 128.2(6) . . ? C27 C28 C29 120.1(9) . . ? C27 C28 Ru1 70.7(5) . . ? C29 C28 Ru1 69.8(5) . . ? C30 C29 C28 121.8(8) . . ? C30 C29 Ru1 72.1(4) . . ? C28 C29 Ru1 72.0(5) . . ? C29 C30 C31 117.4(8) . . ? C29 C30 C36 121.7(8) . . ? C31 C30 C36 120.8(8) . . ? C29 C30 Ru1 70.5(5) . . ? C31 C30 Ru1 71.3(4) . . ? C36 C30 Ru1 132.7(6) . . ? C32 C31 C30 123.2(8) . . ? C32 C31 Ru1 71.9(5) . . ? C30 C31 Ru1 71.2(5) . . ? C31 C32 C27 118.9(8) . . ? C31 C32 Ru1 71.1(5) . . ? C27 C32 Ru1 69.8(5) . . ? C27 C33 C35 108.1(9) . . ? C27 C33 C34 111.7(10) . . ? C35 C33 C34 112.1(11) . . ? C38 C37 C42 120.9(9) . . ? C38 C37 C43 119.7(9) . . ? C42 C37 C43 119.3(8) . . ? C38 C37 Ru2 71.8(5) . . ? C42 C37 Ru2 71.0(5) . . ? C43 C37 Ru2 126.2(6) . . ? C37 C38 C39 121.1(10) . . ? C37 C38 Ru2 72.6(5) . . ? C39 C38 Ru2 71.7(6) . . ? C38 C39 C40 120.8(9) . . ? C38 C39 Ru2 70.8(5) . . ? C40 C39 Ru2 70.7(5) . . ? C41 C40 C39 115.1(9) . . ? C41 C40 C46 117.9(11) . . ? C39 C40 C46 126.9(11) . . ? C41 C40 Ru2 69.8(5) . . ? C39 C40 Ru2 70.3(5) . . ? C46 C40 Ru2 131.2(7) . . ? C42 C41 C40 120.9(9) . . ? C42 C41 Ru2 71.5(4) . . ? C40 C41 Ru2 72.2(5) . . ? C37 C42 C41 121.2(8) . . ? C37 C42 Ru2 72.3(4) . . ? C41 C42 Ru2 70.7(4) . . ? C45 C43 C44 110.4(11) . . ? C45 C43 C37 104.6(11) . . ? C44 C43 C37 117.2(9) . . ? F3 C47 F2 105.1(15) . . ? F3 C47 F1 103.7(15) . . ? F2 C47 F1 106.5(17) . . ? F3 C47 S1 115.4(13) . . ? F2 C47 S1 113.0(12) . . ? F1 C47 S1 112.3(12) . . ? F5 C48 F4 128(2) . . ? F5 C48 F6 108(3) . . ? F4 C48 F6 107(2) . . ? F5 C48 S2 114.5(14) . . ? F4 C48 S2 103.7(11) . . ? F6 C48 S2 87.8(14) . . ? C49 O9 C49 124(5) 2_655 . ? C50 C49 O9 108(4) . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 27.11 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 1.002 _refine_diff_density_min -0.580 _refine_diff_density_rms 0.120 # Attachment 'bpy.cif' data_f81129a _database_code_depnum_ccdc_archive 'CCDC 731560' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C93.30 H94.60 Cl2.60 F12 N8 O16 Ru4 S4' _chemical_formula_weight 2436.66 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 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 25.896(13) _cell_length_b 20.555(10) _cell_length_c 21.037(11) _cell_angle_alpha 90.00 _cell_angle_beta 101.970(8) _cell_angle_gamma 90.00 _cell_volume 10954(9) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 784 _cell_measurement_theta_min 2.276 _cell_measurement_theta_max 24.291 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.475 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4914 _exptl_absorpt_coefficient_mu 0.760 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8629 _exptl_absorpt_correction_T_max 0.9279 _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_% 4.44 _diffrn_reflns_number 24569 _diffrn_reflns_av_R_equivalents 0.0694 _diffrn_reflns_av_sigmaI/netI 0.1419 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.28 _diffrn_reflns_theta_max 26.01 _reflns_number_total 10778 _reflns_number_gt 3964 _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^)+(0.0883P)^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 10778 _refine_ls_number_parameters 614 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.1455 _refine_ls_R_factor_gt 0.0662 _refine_ls_wR_factor_ref 0.1834 _refine_ls_wR_factor_gt 0.1619 _refine_ls_goodness_of_fit_ref 0.790 _refine_ls_restrained_S_all 0.792 _refine_ls_shift/su_max 0.003 _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 0.43735(2) 0.27638(3) 0.12517(3) 0.0597(2) Uani 1 1 d . . . Ru2 Ru 0.39941(4) 0.82029(3) 0.17040(3) 0.1166(4) Uani 1 1 d . . . N1 N 0.5174(2) 0.2777(3) 0.1743(3) 0.0618(14) Uani 1 1 d . . . N2 N 0.4362(4) 0.8226(3) 0.2692(4) 0.112(3) Uani 1 1 d . . . N3 N 0.4387(2) 0.3783(3) 0.1393(2) 0.0610(14) Uani 1 1 d . . . N4 N 0.4174(3) 0.7207(3) 0.1707(3) 0.094(2) Uani 1 1 d . . . O1 O 0.43162(17) 0.2713(2) 0.2228(2) 0.0641(12) Uani 1 1 d . . . O2 O 0.4814(3) 0.8270(2) 0.1654(2) 0.111(2) Uani 1 1 d . . . O3 O 0.7034(6) 0.0926(7) 0.0647(8) 0.150(6) Uani 0.50 1 d P . . O4 O 0.7883(5) 0.1147(6) 0.1142(6) 0.130(4) Uani 0.50 1 d P . . O5 O 0.7590(5) 0.1626(7) 0.0159(7) 0.137(5) Uani 0.50 1 d P . . O6 O 0.5000 -0.0301(4) 0.2500 0.204(6) Uani 1 2 d S . . O7 O 0.5733(3) 0.0571(4) 0.2633(5) 0.190(4) Uani 0.50 1 d P . . O8 O 0.5143(3) 0.0578(3) 0.1677(4) 0.171(3) Uani 0.50 1 d P . . S1 S 0.7560(2) 0.1145(3) 0.0566(3) 0.0997(15) Uani 0.50 1 d PD . . S2 S 0.5222(3) 0.0402(4) 0.2407(4) 0.140(3) Uani 0.50 1 d P . . F1 F 0.7486(7) 0.0439(8) -0.0383(8) 0.222(7) Uani 0.50 1 d PD . . F2 F 0.8256(6) 0.0692(11) 0.0104(10) 0.41(2) Uani 0.50 1 d PD . . F3 F 0.7733(6) -0.0024(6) 0.0491(9) 0.208(7) Uani 0.50 1 d PD . . F4 F 0.4797(8) 0.1383(5) 0.2746(10) 0.229(10) Uani 0.50 1 d P . . F5 F 0.5733(3) 0.0571(4) 0.2633(5) 0.190(4) Uani 0.50 1 d P . . F6 F 0.5143(3) 0.0578(3) 0.1677(4) 0.171(3) Uani 0.50 1 d P . . C1 C 0.4758(2) 0.2741(3) 0.2622(3) 0.0517(15) Uani 1 1 d . . . C2 C 0.5629(3) 0.2773(5) 0.1447(3) 0.071(2) Uani 1 1 d . . . C3 C 0.5877(3) 0.2186(5) 0.1407(4) 0.104(3) Uani 1 1 d . . . H3 H 0.5772 0.1808 0.1586 0.125 Uiso 1 1 calc R . . C4 C 0.6306(5) 0.2188(9) 0.1074(6) 0.157(7) Uani 1 1 d . . . H4 H 0.6475 0.1798 0.1026 0.189 Uiso 1 1 calc R . . C5 C 0.6467(6) 0.2718(13) 0.0836(8) 0.199(12) Uani 1 1 d . . . H5 H 0.6747 0.2700 0.0622 0.238 Uiso 1 1 calc R . . C6 C 0.6227(5) 0.3299(8) 0.0898(6) 0.156(6) Uani 1 1 d . . . H6 H 0.6350 0.3676 0.0734 0.188 Uiso 1 1 calc R . . C7 C 0.5803(4) 0.3334(5) 0.1203(4) 0.106(3) Uani 1 1 d . . . H7 H 0.5639 0.3730 0.1243 0.127 Uiso 1 1 calc R . . C8 C 0.5121(5) 0.8230(4) 0.2201(4) 0.106(4) Uani 1 1 d . . . C9 C 0.4120(5) 0.8364(5) 0.3218(4) 0.107(4) Uani 1 1 d . . . C10 C 0.4152(6) 0.8967(5) 0.3476(5) 0.182(6) Uani 1 1 d . . . H10 H 0.4354 0.9285 0.3330 0.219 Uiso 1 1 calc R . . C11 C 0.3882(8) 0.9105(7) 0.3958(7) 0.219(9) Uani 1 1 d . . . H11 H 0.3918 0.9513 0.4152 0.263 Uiso 1 1 calc R . . C12 C 0.3562(6) 0.8657(9) 0.4157(5) 0.152(5) Uani 1 1 d . . . H12 H 0.3361 0.8755 0.4463 0.183 Uiso 1 1 calc R . . C13 C 0.3554(5) 0.8053(6) 0.3881(7) 0.143(5) Uani 1 1 d . . . H13 H 0.3349 0.7730 0.4016 0.172 Uiso 1 1 calc R . . C14 C 0.3835(5) 0.7905(6) 0.3414(6) 0.119(4) Uani 1 1 d . . . H14 H 0.3824 0.7488 0.3239 0.143 Uiso 1 1 calc R . . C15 C 0.4217(3) 0.4073(4) 0.1880(4) 0.080(2) Uani 1 1 d . . . H15 H 0.4106 0.3809 0.2184 0.096 Uiso 1 1 calc R . . C16 C 0.4197(3) 0.4717(4) 0.1961(4) 0.086(2) Uani 1 1 d . . . H16 H 0.4070 0.4883 0.2310 0.103 Uiso 1 1 calc R . . C17 C 0.4362(3) 0.5135(3) 0.1537(3) 0.070(2) Uani 1 1 d . . . C18 C 0.4558(3) 0.4848(4) 0.1047(4) 0.094(3) Uani 1 1 d . . . H18 H 0.4690 0.5106 0.0753 0.112 Uiso 1 1 calc R . . C19 C 0.4561(3) 0.4179(4) 0.0988(4) 0.086(2) Uani 1 1 d . . . H19 H 0.4691 0.3998 0.0647 0.103 Uiso 1 1 calc R . . C20 C 0.4295(4) 0.6934(4) 0.1200(6) 0.111(3) Uani 1 1 d . . . H20 H 0.4330 0.7206 0.0859 0.133 Uiso 1 1 calc R . . C21 C 0.4375(3) 0.6271(4) 0.1120(4) 0.102(3) Uani 1 1 d . . . H21 H 0.4468 0.6117 0.0744 0.123 Uiso 1 1 calc R . . C22 C 0.4317(3) 0.5858(4) 0.1595(4) 0.082(2) Uani 1 1 d . . . C23 C 0.4195(7) 0.6130(5) 0.2139(5) 0.211(7) Uani 1 1 d . . . H23 H 0.4155 0.5869 0.2486 0.253 Uiso 1 1 calc R . . C24 C 0.4132(6) 0.6793(5) 0.2170(5) 0.191(7) Uani 1 1 d . . . H24 H 0.4054 0.6962 0.2549 0.229 Uiso 1 1 calc R . . C25 C 0.3638(3) 0.2210(5) 0.0974(4) 0.087(2) Uani 1 1 d . . . C26 C 0.3617(3) 0.2745(4) 0.0565(4) 0.085(2) Uani 1 1 d . . . H26 H 0.3332 0.3029 0.0512 0.102 Uiso 1 1 calc R . . C27 C 0.4028(3) 0.2858(4) 0.0229(4) 0.079(2) Uani 1 1 d . . . H27 H 0.4010 0.3226 -0.0032 0.095 Uiso 1 1 calc R . . C28 C 0.4455(3) 0.2444(4) 0.0275(4) 0.071(2) Uani 1 1 d . . . C29 C 0.4467(3) 0.1899(4) 0.0695(4) 0.080(2) Uani 1 1 d . . . H29 H 0.4751 0.1613 0.0742 0.096 Uiso 1 1 calc R . . C30 C 0.4078(4) 0.1778(4) 0.1032(4) 0.087(2) Uani 1 1 d . . . H30 H 0.4101 0.1415 0.1299 0.104 Uiso 1 1 calc R . . C31 C 0.3238(4) 0.2059(6) 0.1353(6) 0.138(4) Uani 1 1 d . . . H31 H 0.3411 0.1789 0.1719 0.166 Uiso 1 1 calc R . . C32 C 0.2997(5) 0.2587(8) 0.1623(7) 0.204(7) Uani 1 1 d . . . H32A H 0.3265 0.2854 0.1880 0.306 Uiso 1 1 calc R . . H32B H 0.2770 0.2419 0.1892 0.306 Uiso 1 1 calc R . . H32C H 0.2792 0.2842 0.1278 0.306 Uiso 1 1 calc R . . C33 C 0.2812(5) 0.1651(7) 0.0957(9) 0.239(8) Uani 1 1 d . . . H33A H 0.2498 0.1685 0.1130 0.358 Uiso 1 1 calc R . . H33B H 0.2925 0.1206 0.0971 0.358 Uiso 1 1 calc R . . H33C H 0.2739 0.1801 0.0515 0.358 Uiso 1 1 calc R . . C34 C 0.4887(3) 0.2550(4) -0.0102(4) 0.104(3) Uani 1 1 d . . . H34A H 0.4851 0.2236 -0.0447 0.156 Uiso 1 1 calc R . . H34B H 0.5226 0.2499 0.0184 0.156 Uiso 1 1 calc R . . H34C H 0.4859 0.2981 -0.0282 0.156 Uiso 1 1 calc R . . C35 C 0.3801(6) 0.9011(6) 0.1009(6) 0.167(6) Uani 1 1 d . . . C36 C 0.3585(6) 0.8415(5) 0.0696(5) 0.145(6) Uani 1 1 d . . . H36 H 0.3651 0.8298 0.0294 0.174 Uiso 1 1 calc R . . C37 C 0.3279(6) 0.8021(7) 0.1005(7) 0.162(6) Uani 1 1 d . . . H37 H 0.3177 0.7623 0.0808 0.195 Uiso 1 1 calc R . . C38 C 0.3095(6) 0.8165(8) 0.1622(6) 0.150(5) Uani 1 1 d . . . C39 C 0.3318(7) 0.8721(8) 0.1880(6) 0.181(7) Uani 1 1 d . . . H39 H 0.3251 0.8827 0.2285 0.217 Uiso 1 1 calc R . . C40 C 0.3635(6) 0.9164(6) 0.1637(6) 0.157(6) Uani 1 1 d . . . H40 H 0.3743 0.9548 0.1859 0.189 Uiso 1 1 calc R . . C41 C 0.4158(7) 0.9436(6) 0.0750(7) 0.182(6) Uani 1 1 d . . . H41 H 0.4436 0.9561 0.1120 0.218 Uiso 1 1 calc R . . C42 C 0.4424(6) 0.9140(6) 0.0269(6) 0.185(6) Uani 1 1 d . . . H42A H 0.4533 0.8706 0.0403 0.278 Uiso 1 1 calc R . . H42B H 0.4728 0.9395 0.0235 0.278 Uiso 1 1 calc R . . H42C H 0.4185 0.9125 -0.0146 0.278 Uiso 1 1 calc R . . C43 C 0.3871(7) 1.0057(6) 0.0499(7) 0.261(9) Uani 1 1 d . . . H43A H 0.4068 1.0283 0.0227 0.392 Uiso 1 1 calc R . . H43B H 0.3838 1.0330 0.0859 0.392 Uiso 1 1 calc R . . H43C H 0.3526 0.9953 0.0251 0.392 Uiso 1 1 calc R . . C44 C 0.2770(4) 0.7686(8) 0.1946(7) 0.197(7) Uani 1 1 d . . . H44A H 0.2569 0.7924 0.2204 0.296 Uiso 1 1 calc R . . H44B H 0.3004 0.7391 0.2219 0.296 Uiso 1 1 calc R . . H44C H 0.2535 0.7445 0.1617 0.296 Uiso 1 1 calc R . . C45 C 0.7813(9) 0.0519(9) 0.0193(10) 0.27(3) Uani 0.50 1 d PD . . C46 C 0.4794(6) 0.0810(9) 0.2753(8) 0.057(5) Uiso 0.50 1 d P . . Cl1 Cl 0.7759(3) -0.0502(6) 0.2304(5) 0.327(5) Uani 0.65 1 d P . . Cl2 Cl 0.7003(4) 0.0452(5) 0.2437(5) 0.312(5) Uani 0.65 1 d P . . C47 C 0.7531(15) 0.037(2) 0.2252(19) 0.34(2) Uiso 0.65 1 d P . . H47A H 0.7791 0.0632 0.2537 0.410 Uiso 0.65 1 calc PR . . H47B H 0.7506 0.0524 0.1811 0.410 Uiso 0.65 1 calc PR . . 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 0.0690(4) 0.0516(3) 0.0557(3) -0.0040(3) 0.0068(3) 0.0002(3) Ru2 0.2083(10) 0.0534(4) 0.0589(4) -0.0101(3) -0.0397(5) 0.0218(5) N1 0.068(4) 0.061(4) 0.057(4) -0.009(3) 0.015(3) 0.001(3) N2 0.194(9) 0.058(4) 0.056(5) -0.005(3) -0.035(6) 0.009(6) N3 0.087(4) 0.054(3) 0.043(3) 0.008(3) 0.015(3) 0.009(3) N4 0.150(6) 0.057(4) 0.056(4) -0.004(4) -0.023(4) 0.001(4) O1 0.060(3) 0.068(3) 0.064(3) 0.010(2) 0.012(2) 0.005(3) O2 0.179(6) 0.068(4) 0.056(3) 0.003(3) -0.043(4) -0.017(4) O3 0.144(11) 0.130(12) 0.217(16) -0.033(10) 0.129(11) -0.011(9) O4 0.155(11) 0.130(11) 0.091(9) 0.002(8) -0.011(9) -0.006(9) O5 0.144(12) 0.141(12) 0.113(11) -0.017(9) -0.004(9) -0.056(10) O6 0.438(19) 0.017(4) 0.138(9) 0.000 0.015(10) 0.000 O7 0.109(5) 0.153(7) 0.290(11) 0.010(6) 0.001(6) -0.009(5) O8 0.205(7) 0.128(6) 0.179(7) 0.043(6) 0.035(6) -0.009(5) S1 0.118(4) 0.092(4) 0.079(4) -0.002(3) -0.002(3) -0.002(3) S2 0.147(9) 0.141(7) 0.125(6) -0.028(5) 0.011(5) -0.001(5) F1 0.276(18) 0.205(16) 0.193(15) -0.071(13) 0.062(14) 0.067(14) F2 0.32(3) 0.49(4) 0.32(3) 0.22(3) -0.15(2) -0.27(3) F3 0.224(15) 0.142(12) 0.29(2) 0.009(12) 0.122(15) 0.031(11) F4 0.32(3) 0.045(6) 0.30(3) -0.038(10) 0.012(15) 0.048(10) F5 0.109(5) 0.153(7) 0.290(11) 0.010(6) 0.001(6) -0.009(5) F6 0.205(7) 0.128(6) 0.179(7) 0.043(6) 0.035(6) -0.009(5) C1 0.052(4) 0.042(4) 0.061(4) 0.009(3) 0.011(3) -0.001(3) C2 0.061(5) 0.106(6) 0.045(4) -0.028(4) 0.009(3) 0.006(5) C3 0.091(6) 0.135(9) 0.083(6) -0.029(6) 0.014(5) 0.029(6) C4 0.086(9) 0.28(2) 0.107(10) -0.088(12) 0.010(7) 0.064(11) C5 0.076(9) 0.42(4) 0.099(11) -0.053(16) 0.027(7) -0.016(15) C6 0.124(11) 0.244(18) 0.122(10) -0.005(10) 0.071(9) -0.047(10) C7 0.106(7) 0.123(9) 0.099(7) -0.017(6) 0.049(6) -0.025(6) C8 0.204(11) 0.040(4) 0.050(5) 0.004(3) -0.030(7) -0.005(7) C9 0.196(11) 0.054(6) 0.050(6) -0.001(5) -0.023(6) 0.003(7) C10 0.40(2) 0.075(7) 0.069(7) -0.015(5) 0.037(10) -0.013(9) C11 0.46(3) 0.115(11) 0.107(11) -0.025(8) 0.107(14) 0.014(14) C12 0.213(14) 0.169(14) 0.063(7) 0.009(9) 0.002(7) 0.030(11) C13 0.164(12) 0.095(9) 0.130(11) 0.005(8) -0.064(9) 0.013(8) C14 0.128(9) 0.095(9) 0.111(9) -0.033(8) -0.031(7) 0.030(7) C15 0.120(6) 0.060(5) 0.068(5) 0.007(4) 0.041(5) 0.012(5) C16 0.149(8) 0.053(5) 0.065(5) -0.003(4) 0.044(5) 0.015(5) C17 0.100(6) 0.054(5) 0.056(5) -0.007(4) 0.016(4) 0.003(4) C18 0.159(8) 0.064(5) 0.066(5) -0.001(4) 0.041(5) -0.024(5) C19 0.132(7) 0.067(5) 0.066(5) -0.010(4) 0.038(5) -0.003(5) C20 0.154(9) 0.051(5) 0.138(9) 0.024(6) 0.055(7) -0.005(5) C21 0.161(8) 0.053(5) 0.115(7) 0.012(5) 0.078(7) 0.004(5) C22 0.120(7) 0.056(5) 0.060(5) -0.008(4) -0.001(4) 0.003(5) C23 0.51(2) 0.066(7) 0.074(7) -0.009(5) 0.088(11) 0.000(10) C24 0.44(2) 0.052(6) 0.070(7) -0.017(5) 0.027(10) 0.041(9) C25 0.069(6) 0.099(7) 0.093(6) -0.010(5) 0.015(5) -0.010(6) C26 0.061(5) 0.094(7) 0.088(6) -0.017(5) -0.012(4) 0.002(5) C27 0.092(6) 0.072(5) 0.063(5) -0.003(4) -0.008(4) -0.007(5) C28 0.083(6) 0.070(5) 0.059(5) -0.017(4) 0.015(4) -0.002(4) C29 0.092(6) 0.052(5) 0.087(6) -0.022(4) 0.000(5) 0.001(4) C30 0.117(7) 0.059(5) 0.078(6) -0.004(4) 0.004(5) -0.021(6) C31 0.089(7) 0.157(11) 0.173(11) -0.053(9) 0.039(8) -0.043(8) C32 0.108(9) 0.30(2) 0.209(16) -0.040(14) 0.045(9) 0.001(11) C33 0.189(13) 0.214(16) 0.35(2) -0.070(14) 0.129(14) -0.124(12) C34 0.119(7) 0.133(8) 0.060(5) -0.022(5) 0.019(5) -0.003(6) C35 0.295(17) 0.072(8) 0.095(9) 0.030(7) -0.050(10) 0.048(9) C36 0.263(15) 0.069(7) 0.066(7) -0.017(5) -0.056(8) 0.069(8) C37 0.219(15) 0.122(11) 0.099(11) -0.001(8) -0.074(10) 0.060(10) C38 0.170(12) 0.147(12) 0.092(10) -0.023(9) -0.068(9) 0.053(10) C39 0.29(2) 0.119(12) 0.095(10) 0.000(9) -0.048(11) 0.105(13) C40 0.296(17) 0.076(8) 0.073(8) -0.015(6) -0.025(9) 0.094(10) C41 0.32(2) 0.087(9) 0.111(10) 0.023(8) -0.016(11) 0.031(11) C42 0.285(17) 0.145(12) 0.126(11) 0.019(9) 0.042(11) 0.032(11) C43 0.48(3) 0.097(9) 0.167(13) 0.047(9) -0.023(14) 0.031(13) C44 0.113(9) 0.290(19) 0.172(13) 0.065(13) -0.011(8) -0.025(11) C45 0.39(6) 0.16(3) 0.16(3) 0.05(2) -0.13(4) -0.18(4) Cl1 0.229(8) 0.439(16) 0.345(12) -0.047(10) 0.135(8) -0.096(9) Cl2 0.254(8) 0.348(12) 0.366(13) 0.033(9) 0.136(9) -0.038(8) _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 O1 2.093(4) . ? Ru1 N1 2.115(5) . ? Ru1 N3 2.115(5) . ? Ru1 C27 2.160(7) . ? Ru1 C29 2.170(7) . ? Ru1 C26 2.180(7) . ? Ru1 C30 2.181(7) . ? Ru1 C25 2.192(8) . ? Ru1 C28 2.209(7) . ? Ru2 N4 2.099(7) . ? Ru2 N2 2.100(7) . ? Ru2 C37 2.145(12) . ? Ru2 C39 2.145(15) . ? Ru2 O2 2.152(7) . ? Ru2 C40 2.174(10) . ? Ru2 C35 2.201(10) . ? Ru2 C36 2.208(9) . ? Ru2 C38 2.300(16) . ? N1 C1 1.313(8) 2_655 ? N1 C2 1.442(8) . ? N2 C8 1.311(12) 2_655 ? N2 C9 1.409(12) . ? N3 C19 1.323(8) . ? N3 C15 1.335(8) . ? N4 C20 1.298(10) . ? N4 C24 1.315(11) . ? O1 C1 1.267(7) . ? O2 C8 1.259(10) . ? O3 S1 1.477(13) . ? O4 S1 1.322(12) . ? O5 S1 1.321(15) . ? O6 S2 1.583(10) 2_655 ? O6 S2 1.583(10) . ? O7 S2 1.353(9) . ? O7 C46 1.517(18) 2_655 ? O8 C46 1.268(17) 2_655 ? O8 S2 1.549(11) . ? S1 C45 1.707(18) . ? S2 C46 0.901(16) 2_655 ? S2 S2 1.292(14) 2_655 ? S2 C46 1.673(15) . ? S2 F4 2.041(12) 2_655 ? F1 C45 1.336(16) . ? F2 C45 1.252(16) . ? F3 C45 1.319(16) . ? F4 C46 1.179(18) . ? F4 F4 1.62(3) 2_655 ? F4 S2 2.041(12) 2_655 ? C1 N1 1.313(8) 2_655 ? C1 C1 1.449(12) 2_655 ? C2 C3 1.377(10) . ? C2 C7 1.378(11) . ? C3 C4 1.429(14) . ? C4 C5 1.30(2) . ? C5 C6 1.37(2) . ? C6 C7 1.384(13) . ? C8 N2 1.311(12) 2_655 ? C8 C8 1.52(2) 2_655 ? C9 C14 1.316(13) . ? C9 C10 1.348(12) . ? C10 C11 1.376(17) . ? C11 C12 1.361(17) . ? C12 C13 1.368(15) . ? C13 C14 1.374(16) . ? C15 C16 1.337(9) . ? C16 C17 1.370(9) . ? C17 C18 1.373(9) . ? C17 C22 1.498(10) . ? C18 C19 1.382(10) . ? C20 C21 1.394(11) . ? C21 C22 1.344(9) . ? C22 C23 1.368(11) . ? C23 C24 1.374(12) . ? C25 C26 1.389(11) . ? C25 C30 1.430(11) . ? C25 C31 1.467(13) . ? C26 C27 1.413(10) . ? C27 C28 1.383(10) . ? C28 C29 1.424(10) . ? C28 C34 1.516(10) . ? C29 C30 1.370(10) . ? C31 C32 1.427(15) . ? C31 C33 1.494(14) . ? C35 C36 1.446(14) . ? C35 C41 1.456(18) . ? C35 C40 1.504(16) . ? C36 C37 1.385(18) . ? C37 C38 1.503(18) . ? C38 C39 1.344(17) . ? C38 C44 1.543(17) . ? C39 C40 1.39(2) . ? C41 C42 1.470(16) . ? C41 C43 1.517(15) . ? C46 S2 0.901(16) 2_655 ? C46 F6 1.268(17) 2_655 ? C46 O8 1.268(17) 2_655 ? C46 O7 1.517(18) 2_655 ? C46 F5 1.517(18) 2_655 ? C46 C46 1.66(3) 2_655 ? Cl1 C47 1.88(4) . ? Cl2 C47 1.51(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Ru1 N1 77.45(19) . . ? O1 Ru1 N3 85.07(18) . . ? N1 Ru1 N3 86.2(2) . . ? O1 Ru1 C27 152.0(3) . . ? N1 Ru1 C27 130.3(3) . . ? N3 Ru1 C27 92.4(2) . . ? O1 Ru1 C29 121.8(3) . . ? N1 Ru1 C29 93.8(3) . . ? N3 Ru1 C29 152.5(3) . . ? C27 Ru1 C29 66.8(3) . . ? O1 Ru1 C26 114.4(3) . . ? N1 Ru1 C26 168.1(3) . . ? N3 Ru1 C26 95.6(3) . . ? C27 Ru1 C26 38.0(3) . . ? C29 Ru1 C26 79.3(3) . . ? O1 Ru1 C30 93.9(3) . . ? N1 Ru1 C30 112.3(3) . . ? N3 Ru1 C30 160.8(3) . . ? C27 Ru1 C30 79.5(3) . . ? C29 Ru1 C30 36.7(3) . . ? C26 Ru1 C30 67.4(3) . . ? O1 Ru1 C25 90.1(3) . . ? N1 Ru1 C25 147.8(3) . . ? N3 Ru1 C25 122.7(3) . . ? C27 Ru1 C25 67.9(3) . . ? C29 Ru1 C25 67.6(3) . . ? C26 Ru1 C25 37.1(3) . . ? C30 Ru1 C25 38.2(3) . . ? O1 Ru1 C28 159.8(3) . . ? N1 Ru1 C28 100.7(3) . . ? N3 Ru1 C28 115.0(3) . . ? C27 Ru1 C28 36.9(3) . . ? C29 Ru1 C28 37.9(3) . . ? C26 Ru1 C28 67.9(3) . . ? C30 Ru1 C28 67.9(3) . . ? C25 Ru1 C28 81.0(3) . . ? N4 Ru2 N2 88.0(3) . . ? N4 Ru2 C37 89.5(4) . . ? N2 Ru2 C37 146.4(6) . . ? N4 Ru2 C39 132.3(6) . . ? N2 Ru2 C39 92.1(4) . . ? C37 Ru2 C39 65.5(6) . . ? N4 Ru2 O2 80.9(3) . . ? N2 Ru2 O2 78.3(3) . . ? C37 Ru2 O2 134.2(5) . . ? C39 Ru2 O2 145.6(6) . . ? N4 Ru2 C40 167.8(5) . . ? N2 Ru2 C40 98.3(4) . . ? C37 Ru2 C40 79.5(5) . . ? C39 Ru2 C40 37.6(5) . . ? O2 Ru2 C40 110.5(5) . . ? N4 Ru2 C35 139.2(4) . . ? N2 Ru2 C35 129.4(4) . . ? C37 Ru2 C35 68.3(5) . . ? C39 Ru2 C35 70.0(6) . . ? O2 Ru2 C35 90.5(5) . . ? C40 Ru2 C35 40.2(4) . . ? N4 Ru2 C36 104.9(3) . . ? N2 Ru2 C36 167.1(3) . . ? C37 Ru2 C36 37.1(5) . . ? C39 Ru2 C36 79.7(5) . . ? O2 Ru2 C36 102.8(5) . . ? C40 Ru2 C36 69.2(4) . . ? C35 Ru2 C36 38.3(4) . . ? N4 Ru2 C38 100.9(5) . . ? N2 Ru2 C38 108.6(5) . . ? C37 Ru2 C38 39.3(5) . . ? C39 Ru2 C38 35.0(5) . . ? O2 Ru2 C38 172.8(4) . . ? C40 Ru2 C38 67.3(5) . . ? C35 Ru2 C38 83.6(6) . . ? C36 Ru2 C38 70.0(5) . . ? C1 N1 C2 119.2(5) 2_655 . ? C1 N1 Ru1 114.1(4) 2_655 . ? C2 N1 Ru1 126.5(4) . . ? C8 N2 C9 118.0(8) 2_655 . ? C8 N2 Ru2 114.0(8) 2_655 . ? C9 N2 Ru2 126.7(7) . . ? C19 N3 C15 115.4(6) . . ? C19 N3 Ru1 121.1(5) . . ? C15 N3 Ru1 123.5(5) . . ? C20 N4 C24 113.5(8) . . ? C20 N4 Ru2 120.7(6) . . ? C24 N4 Ru2 125.5(7) . . ? C1 O1 Ru1 113.6(4) . . ? C8 O2 Ru2 113.1(7) . . ? S2 O6 S2 48.2(6) 2_655 . ? S2 O7 C46 36.0(7) . 2_655 ? C46 O8 S2 35.6(8) 2_655 . ? O5 S1 O4 118.7(9) . . ? O5 S1 O3 118.9(10) . . ? O4 S1 O3 108.5(10) . . ? O5 S1 C45 100.7(10) . . ? O4 S1 C45 101.2(10) . . ? O3 S1 C45 105.9(9) . . ? C46 S2 S2 97.9(13) 2_655 2_655 ? C46 S2 O7 82.0(14) 2_655 . ? S2 S2 O7 139.5(10) 2_655 . ? C46 S2 O8 55.0(12) 2_655 . ? S2 S2 O8 110.9(9) 2_655 . ? O7 S2 O8 102.0(7) . . ? C46 S2 O6 154.9(16) 2_655 . ? S2 S2 O6 65.9(3) 2_655 . ? O7 S2 O6 123.0(7) . . ? O8 S2 O6 111.1(6) . . ? C46 S2 C46 73.3(16) 2_655 . ? S2 S2 C46 32.2(6) 2_655 . ? O7 S2 C46 113.9(7) . . ? O8 S2 C46 110.6(9) . . ? O6 S2 C46 96.4(6) . . ? C46 S2 F4 12.7(13) 2_655 2_655 ? S2 S2 F4 93.0(5) 2_655 2_655 ? O7 S2 F4 78.1(7) . 2_655 ? O8 S2 F4 67.6(7) . 2_655 ? O6 S2 F4 157.5(7) . 2_655 ? C46 S2 F4 65.0(7) . 2_655 ? C46 F4 F4 90.9(11) . 2_655 ? C46 F4 S2 9.6(10) . 2_655 ? F4 F4 S2 84.1(5) 2_655 2_655 ? O1 C1 N1 125.5(6) . 2_655 ? O1 C1 C1 120.0(8) . 2_655 ? N1 C1 C1 114.5(7) 2_655 2_655 ? C3 C2 C7 121.1(8) . . ? C3 C2 N1 117.8(8) . . ? C7 C2 N1 121.1(8) . . ? C2 C3 C4 116.7(11) . . ? C5 C4 C3 122.2(17) . . ? C4 C5 C6 120.4(16) . . ? C5 C6 C7 120.7(15) . . ? C2 C7 C6 118.9(10) . . ? O2 C8 N2 125.8(10) . 2_655 ? O2 C8 C8 117.9(15) . 2_655 ? N2 C8 C8 116.2(11) 2_655 2_655 ? C14 C9 C10 121.7(13) . . ? C14 C9 N2 118.1(10) . . ? C10 C9 N2 120.1(12) . . ? C9 C10 C11 119.2(13) . . ? C12 C11 C10 121.5(13) . . ? C11 C12 C13 116.1(14) . . ? C12 C13 C14 122.8(14) . . ? C9 C14 C13 118.6(12) . . ? N3 C15 C16 124.7(7) . . ? C15 C16 C17 120.8(7) . . ? C16 C17 C18 115.7(7) . . ? C16 C17 C22 121.9(7) . . ? C18 C17 C22 122.4(7) . . ? C17 C18 C19 120.3(7) . . ? N3 C19 C18 123.1(7) . . ? N4 C20 C21 126.1(8) . . ? C22 C21 C20 119.0(8) . . ? C21 C22 C23 116.5(8) . . ? C21 C22 C17 122.9(7) . . ? C23 C22 C17 120.6(8) . . ? C22 C23 C24 119.6(10) . . ? N4 C24 C23 125.3(10) . . ? C26 C25 C30 118.2(8) . . ? C26 C25 C31 124.2(10) . . ? C30 C25 C31 117.6(10) . . ? C26 C25 Ru1 71.0(5) . . ? C30 C25 Ru1 70.5(4) . . ? C31 C25 Ru1 129.6(7) . . ? C25 C26 C27 120.2(8) . . ? C25 C26 Ru1 71.9(5) . . ? C27 C26 Ru1 70.2(4) . . ? C28 C27 C26 122.6(8) . . ? C28 C27 Ru1 73.5(4) . . ? C26 C27 Ru1 71.8(4) . . ? C27 C28 C29 116.2(7) . . ? C27 C28 C34 122.9(8) . . ? C29 C28 C34 120.9(8) . . ? C27 C28 Ru1 69.6(4) . . ? C29 C28 Ru1 69.6(4) . . ? C34 C28 Ru1 131.9(5) . . ? C30 C29 C28 122.7(8) . . ? C30 C29 Ru1 72.1(5) . . ? C28 C29 Ru1 72.5(4) . . ? C29 C30 C25 120.1(8) . . ? C29 C30 Ru1 71.2(4) . . ? C25 C30 Ru1 71.3(4) . . ? C32 C31 C25 118.2(11) . . ? C32 C31 C33 108.4(11) . . ? C25 C31 C33 109.8(10) . . ? C36 C35 C41 123.6(14) . . ? C36 C35 C40 115.0(14) . . ? C41 C35 C40 121.4(13) . . ? C36 C35 Ru2 71.1(6) . . ? C41 C35 Ru2 128.8(10) . . ? C40 C35 Ru2 68.9(6) . . ? C37 C36 C35 119.1(13) . . ? C37 C36 Ru2 69.0(7) . . ? C35 C36 Ru2 70.6(5) . . ? C36 C37 C38 127.2(14) . . ? C36 C37 Ru2 73.9(8) . . ? C38 C37 Ru2 75.9(7) . . ? C39 C38 C37 109.2(16) . . ? C39 C38 C44 126.4(16) . . ? C37 C38 C44 123.8(14) . . ? C39 C38 Ru2 66.2(9) . . ? C37 C38 Ru2 64.7(8) . . ? C44 C38 Ru2 128.6(8) . . ? C38 C39 C40 130.2(16) . . ? C38 C39 Ru2 78.8(9) . . ? C40 C39 Ru2 72.3(10) . . ? C39 C40 C35 118.9(12) . . ? C39 C40 Ru2 70.1(7) . . ? C35 C40 Ru2 70.9(5) . . ? C35 C41 C42 115.7(12) . . ? C35 C41 C43 109.5(14) . . ? C42 C41 C43 111.9(13) . . ? F2 C45 F3 123(2) . . ? F2 C45 F1 109(2) . . ? F3 C45 F1 101.2(17) . . ? F2 C45 S1 107.9(14) . . ? F3 C45 S1 107.8(14) . . ? F1 C45 S1 106.2(13) . . ? S2 C46 F4 158(2) 2_655 . ? S2 C46 F6 89.5(16) 2_655 2_655 ? F4 C46 F6 112.8(18) . 2_655 ? S2 C46 O8 89.5(16) 2_655 2_655 ? F4 C46 O8 112.8(18) . 2_655 ? F6 C46 O8 0.0(10) 2_655 2_655 ? S2 C46 O7 62.0(12) 2_655 2_655 ? F4 C46 O7 109.0(17) . 2_655 ? F6 C46 O7 108.0(12) 2_655 2_655 ? O8 C46 O7 108.0(12) 2_655 2_655 ? S2 C46 F5 62.0(12) 2_655 2_655 ? F4 C46 F5 109.0(17) . 2_655 ? F6 C46 F5 108.0(12) 2_655 2_655 ? O8 C46 F5 108.0(12) 2_655 2_655 ? O7 C46 F5 0.0(10) 2_655 2_655 ? S2 C46 C46 75.3(13) 2_655 2_655 ? F4 C46 C46 89.1(11) . 2_655 ? F6 C46 C46 129.4(16) 2_655 2_655 ? O8 C46 C46 129.4(16) 2_655 2_655 ? O7 C46 C46 106.4(15) 2_655 2_655 ? F5 C46 C46 106.4(15) 2_655 2_655 ? S2 C46 S2 49.9(12) 2_655 . ? F4 C46 S2 119.2(14) . . ? F6 C46 S2 104.9(11) 2_655 . ? O8 C46 S2 104.9(11) 2_655 . ? O7 C46 S2 102.0(11) 2_655 . ? F5 C46 S2 102.0(11) 2_655 . ? C46 C46 S2 31.4(6) 2_655 . ? Cl2 C47 Cl1 113(2) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.01 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.240 _refine_diff_density_min -1.006 _refine_diff_density_rms 0.093