# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name 'Caiping Tan' 'Shouhai Wu' 'Sensen Lai' 'Minxu Wang' 'Yu Chen' ; Lingjun Zhou ; 'Yiping Zhu' 'Wu Lian' 'Wenlie Peng' 'Liangnian Ji' 'Anlong Xu' _publ_contact_author_name 'Xu, Anlong' _publ_contact_author_email lssxal@mail.sysu.edu.cn data_763615 _database_code_depnum_ccdc_archive 'CCDC 763615' #TrackingRef '763615.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C58 H48 F6 N8 O6 Ru S2' _chemical_formula_weight 1232.23 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 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 20.372(2) _cell_length_b 18.564(2) _cell_length_c 16.544(2) _cell_angle_alpha 90.00 _cell_angle_beta 119.485(2) _cell_angle_gamma 90.00 _cell_volume 5446.3(11) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.41 _exptl_crystal_size_mid 0.34 _exptl_crystal_size_min 0.29 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.503 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2520 _exptl_absorpt_coefficient_mu 0.445 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8385 _exptl_absorpt_correction_T_max 0.8817 _exptl_absorpt_process_details ? _exptl_special_details ? _diffrn_ambient_temperature 173(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12793 _diffrn_reflns_av_R_equivalents 0.0346 _diffrn_reflns_av_sigmaI/netI 0.0506 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.59 _diffrn_reflns_theta_max 26.00 _reflns_number_total 5295 _reflns_number_gt 3900 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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. disorder: The anion SO3CF3- is disordered and and refined with restrains on bond lengths and bond angles. ; _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^)+(0.0600P)^2^+6.8017P] 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 5295 _refine_ls_number_parameters 394 _refine_ls_number_restraints 54 _refine_ls_R_factor_all 0.0677 _refine_ls_R_factor_gt 0.0436 _refine_ls_wR_factor_ref 0.1191 _refine_ls_wR_factor_gt 0.1055 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.200 _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 0.5000 0.88634(2) 0.7500 0.02100(14) Uani 1 2 d S . . N1 N 0.47735(16) 0.80719(15) 0.64830(19) 0.0207(6) Uani 1 1 d . . . N2 N 0.39323(17) 0.89522(15) 0.7345(2) 0.0235(7) Uani 1 1 d . . . N3 N 0.51589(16) 0.96697(15) 0.8425(2) 0.0230(7) Uani 1 1 d . . . N4 N 0.55157(18) 0.64264(17) 0.5978(2) 0.0299(7) Uani 1 1 d . . . H4B H 0.5879 0.6225 0.6482 0.036 Uiso 1 1 calc R . . C1 C 0.5218(2) 0.74921(19) 0.6659(3) 0.0248(8) Uani 1 1 d . . . H1A H 0.5598 0.7393 0.7278 0.030 Uiso 1 1 calc R . . C2 C 0.5128(2) 0.70380(19) 0.5952(2) 0.0243(8) Uani 1 1 d . . . C3 C 0.4575(2) 0.71771(19) 0.5023(2) 0.0243(8) Uani 1 1 d . . . C4 C 0.4104(2) 0.7767(2) 0.4860(3) 0.0273(8) Uani 1 1 d . . . H4A H 0.3710 0.7872 0.4250 0.033 Uiso 1 1 calc R . . C5 C 0.4218(2) 0.81893(19) 0.5592(2) 0.0247(8) Uani 1 1 d . . . H5A H 0.3891 0.8589 0.5474 0.030 Uiso 1 1 calc R . . C6 C 0.4651(2) 0.6633(2) 0.4461(2) 0.0265(8) Uani 1 1 d . . . C7 C 0.5240(2) 0.6178(2) 0.5079(3) 0.0276(8) Uani 1 1 d . . . C8 C 0.5460(2) 0.5584(2) 0.4760(3) 0.0345(9) Uani 1 1 d . . . H8A H 0.5860 0.5281 0.5175 0.041 Uiso 1 1 calc R . . C9 C 0.5078(3) 0.5450(2) 0.3823(3) 0.0412(11) Uani 1 1 d . . . H9A H 0.5209 0.5040 0.3590 0.049 Uiso 1 1 calc R . . C10 C 0.4502(3) 0.5899(2) 0.3205(3) 0.0397(11) Uani 1 1 d . . . H10A H 0.4257 0.5793 0.2559 0.048 Uiso 1 1 calc R . . C11 C 0.4281(2) 0.6497(2) 0.3510(3) 0.0327(9) Uani 1 1 d . . . H11A H 0.3889 0.6804 0.3086 0.039 Uiso 1 1 calc R . . C12 C 0.3835(2) 0.9508(2) 0.7807(3) 0.0255(8) Uani 1 1 d . . . C13 C 0.3149(2) 0.9662(2) 0.7724(3) 0.0387(10) Uani 1 1 d . . . H13A H 0.3099 1.0059 0.8051 0.046 Uiso 1 1 calc R . . C14 C 0.2532(2) 0.9243(2) 0.7168(3) 0.0428(11) Uani 1 1 d . . . H14A H 0.2050 0.9352 0.7095 0.051 Uiso 1 1 calc R . . C15 C 0.2630(2) 0.8663(2) 0.6720(3) 0.0370(10) Uani 1 1 d . . . H15A H 0.2218 0.8355 0.6346 0.044 Uiso 1 1 calc R . . C16 C 0.3330(2) 0.8534(2) 0.6820(3) 0.0265(8) Uani 1 1 d . . . H16A H 0.3392 0.8133 0.6507 0.032 Uiso 1 1 calc R . . C17 C 0.4527(2) 0.99181(19) 0.8409(3) 0.0258(8) Uani 1 1 d . . . C18 C 0.4548(2) 1.0513(2) 0.8938(3) 0.0346(10) Uani 1 1 d . . . H18A H 0.4098 1.0682 0.8915 0.041 Uiso 1 1 calc R . . C19 C 0.5224(2) 1.0852(2) 0.9494(3) 0.0391(10) Uani 1 1 d . . . H19A H 0.5245 1.1263 0.9848 0.047 Uiso 1 1 calc R . . C20 C 0.5869(2) 1.0589(2) 0.9530(3) 0.0368(10) Uani 1 1 d . . . H20A H 0.6344 1.0807 0.9922 0.044 Uiso 1 1 calc R . . C21 C 0.5815(2) 1.0008(2) 0.8989(3) 0.0304(9) Uani 1 1 d . . . H21A H 0.6263 0.9834 0.9012 0.037 Uiso 1 1 calc R . . C22 C 0.2609(3) 0.7405(3) 0.1309(3) 0.0580(14) Uani 1 1 d . . . C23 C 0.2993(4) 0.8038(3) 0.1719(4) 0.0745(18) Uani 1 1 d . . . H23A H 0.2771 0.8390 0.1926 0.089 Uiso 1 1 calc R . . C24 C 0.3716(5) 0.8156(4) 0.1825(5) 0.090(2) Uani 1 1 d . . . H24A H 0.3980 0.8587 0.2109 0.108 Uiso 1 1 calc R . . C25 C 0.4038(4) 0.7661(5) 0.1528(5) 0.087(2) Uani 1 1 d . . . H25A H 0.4522 0.7746 0.1594 0.104 Uiso 1 1 calc R . . C26 C 0.3665(4) 0.7052(4) 0.1141(4) 0.0713(17) Uani 1 1 d . . . H26A H 0.3893 0.6703 0.0937 0.086 Uiso 1 1 calc R . . C27 C 0.2956(3) 0.6913(3) 0.1027(3) 0.0617(15) Uani 1 1 d . . . H27A H 0.2708 0.6473 0.0752 0.074 Uiso 1 1 calc R . . C28 C 0.1821(3) 0.7272(4) 0.1163(4) 0.086(2) Uani 1 1 d . . . H28A H 0.1734 0.6753 0.1156 0.129 Uiso 1 1 calc R . . H28B H 0.1448 0.7483 0.0569 0.129 Uiso 1 1 calc R . . H28C H 0.1775 0.7496 0.1669 0.129 Uiso 1 1 calc R . . S1 S 0.28465(5) 0.61531(5) 0.66183(7) 0.0324(2) Uani 1 1 d D . . O1 O 0.2956(2) 0.69046(19) 0.6706(3) 0.0860(14) Uani 1 1 d . A . O2 O 0.3196(2) 0.5781(2) 0.7478(2) 0.0712(12) Uani 1 1 d . A . O3 O 0.21001(16) 0.59022(17) 0.5979(2) 0.0495(9) Uani 1 1 d . A . C29 C 0.3398(3) 0.5876(4) 0.6125(4) 0.092(2) Uani 0.50 1 d PD A 1 F1 F 0.3266(6) 0.5963(6) 0.5336(5) 0.104(3) Uani 0.50 1 d PDU A 1 F2 F 0.3372(4) 0.5069(3) 0.6153(5) 0.066(2) Uani 0.50 1 d PDU A 1 F3 F 0.4144(3) 0.5940(6) 0.6778(7) 0.078(3) Uani 0.50 1 d PDU A 1 C29' C 0.3398(3) 0.5876(4) 0.6125(4) 0.092(2) Uani 0.50 1 d PD A 2 F1' F 0.3138(6) 0.6439(6) 0.5356(6) 0.135(4) Uani 0.50 1 d PDU A 2 F2' F 0.3258(6) 0.5331(6) 0.5654(8) 0.145(5) Uani 0.50 1 d PDU A 2 F3' F 0.4100(4) 0.6112(8) 0.6554(9) 0.128(6) Uani 0.50 1 d PDU A 2 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 0.0206(2) 0.0192(2) 0.0223(2) 0.000 0.00989(17) 0.000 N1 0.0195(15) 0.0209(15) 0.0215(15) -0.0001(12) 0.0099(12) -0.0010(13) N2 0.0244(16) 0.0211(16) 0.0244(15) 0.0035(13) 0.0116(13) -0.0004(13) N3 0.0261(17) 0.0199(16) 0.0245(16) -0.0002(13) 0.0136(13) -0.0008(13) N4 0.0304(18) 0.0280(17) 0.0249(17) -0.0013(14) 0.0089(14) 0.0045(15) C1 0.0221(19) 0.025(2) 0.0234(18) 0.0004(15) 0.0078(15) -0.0017(16) C2 0.0228(19) 0.0209(19) 0.028(2) -0.0007(15) 0.0120(16) -0.0017(15) C3 0.0235(19) 0.0235(19) 0.0262(19) 0.0000(15) 0.0125(16) -0.0043(16) C4 0.028(2) 0.029(2) 0.0223(19) -0.0004(16) 0.0100(16) -0.0032(17) C5 0.0240(19) 0.0229(19) 0.0250(19) 0.0033(15) 0.0104(16) 0.0019(16) C6 0.027(2) 0.029(2) 0.0266(19) -0.0010(16) 0.0157(16) -0.0030(17) C7 0.029(2) 0.030(2) 0.029(2) -0.0033(17) 0.0182(17) -0.0057(18) C8 0.036(2) 0.029(2) 0.042(2) -0.0009(18) 0.023(2) 0.0014(18) C9 0.051(3) 0.037(2) 0.049(3) -0.013(2) 0.034(2) -0.006(2) C10 0.046(3) 0.046(3) 0.031(2) -0.011(2) 0.023(2) -0.010(2) C11 0.032(2) 0.039(2) 0.031(2) -0.0042(18) 0.0184(18) -0.0067(19) C12 0.0244(19) 0.0235(19) 0.032(2) 0.0042(16) 0.0164(16) 0.0025(16) C13 0.035(2) 0.034(2) 0.051(3) -0.006(2) 0.024(2) 0.0008(19) C14 0.025(2) 0.042(3) 0.063(3) -0.004(2) 0.023(2) 0.003(2) C15 0.029(2) 0.036(2) 0.044(3) -0.0028(19) 0.0170(19) -0.0074(19) C16 0.024(2) 0.024(2) 0.029(2) 0.0024(16) 0.0120(16) -0.0017(16) C17 0.029(2) 0.0223(19) 0.029(2) 0.0018(16) 0.0154(16) 0.0028(16) C18 0.038(2) 0.028(2) 0.042(2) -0.0011(18) 0.023(2) 0.0061(19) C19 0.047(3) 0.029(2) 0.045(3) -0.013(2) 0.026(2) -0.006(2) C20 0.035(2) 0.035(2) 0.037(2) -0.0131(19) 0.0154(19) -0.0065(19) C21 0.027(2) 0.030(2) 0.035(2) -0.0027(17) 0.0159(17) -0.0009(17) C22 0.063(3) 0.069(4) 0.042(3) 0.013(3) 0.026(3) 0.018(3) C23 0.114(6) 0.068(4) 0.064(4) 0.004(3) 0.061(4) 0.017(4) C24 0.128(7) 0.072(5) 0.079(5) -0.002(4) 0.057(5) -0.030(5) C25 0.095(5) 0.111(6) 0.072(4) 0.005(4) 0.054(4) -0.006(5) C26 0.076(4) 0.092(5) 0.051(3) 0.019(3) 0.035(3) 0.027(4) C27 0.069(4) 0.072(4) 0.045(3) 0.007(3) 0.029(3) 0.021(3) C28 0.069(4) 0.124(6) 0.065(4) 0.009(4) 0.033(3) 0.017(4) S1 0.0260(5) 0.0282(5) 0.0401(6) 0.0003(5) 0.0141(4) -0.0027(4) O1 0.065(3) 0.0287(19) 0.145(4) -0.009(2) 0.037(3) -0.0054(18) O2 0.061(2) 0.083(3) 0.0381(19) 0.0131(19) -0.0008(17) -0.035(2) O3 0.0256(16) 0.0481(19) 0.056(2) 0.0166(16) 0.0057(14) -0.0023(14) C29 0.070(5) 0.132(7) 0.086(5) -0.047(5) 0.048(4) -0.024(4) F1 0.149(7) 0.127(7) 0.070(5) 0.000(5) 0.080(5) 0.018(6) F2 0.068(4) 0.058(4) 0.063(4) -0.022(3) 0.025(4) 0.009(3) F3 0.035(5) 0.103(6) 0.103(6) -0.043(5) 0.039(4) -0.009(4) C29' 0.070(5) 0.132(7) 0.086(5) -0.047(5) 0.048(4) -0.024(4) F1' 0.158(8) 0.204(10) 0.083(6) -0.015(6) 0.089(6) -0.048(7) F2' 0.127(8) 0.182(10) 0.132(8) -0.089(7) 0.069(7) -0.001(7) F3' 0.076(8) 0.167(11) 0.178(11) -0.030(7) 0.092(7) -0.029(6) _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 N3 2.049(3) . ? Ru1 N3 2.049(3) 2_656 ? Ru1 N2 2.067(3) . ? Ru1 N2 2.067(3) 2_656 ? Ru1 N1 2.107(3) . ? Ru1 N1 2.107(3) 2_656 ? N1 C1 1.342(4) . ? N1 C5 1.364(4) . ? N2 C16 1.346(5) . ? N2 C12 1.355(5) . ? N3 C21 1.351(5) . ? N3 C17 1.354(5) . ? N4 C2 1.371(5) . ? N4 C7 1.384(5) . ? N4 H4B 0.8800 . ? C1 C2 1.380(5) . ? C1 H1A 0.9500 . ? C2 C3 1.412(5) . ? C3 C4 1.391(5) . ? C3 C6 1.432(5) . ? C4 C5 1.363(5) . ? C4 H4A 0.9500 . ? C5 H5A 0.9500 . ? C6 C11 1.392(5) . ? C6 C7 1.412(5) . ? C7 C8 1.389(5) . ? C8 C9 1.372(6) . ? C8 H8A 0.9500 . ? C9 C10 1.391(6) . ? C9 H9A 0.9500 . ? C10 C11 1.385(6) . ? C10 H10A 0.9500 . ? C11 H11A 0.9500 . ? C12 C13 1.365(5) . ? C12 C17 1.476(5) . ? C13 C14 1.377(6) . ? C13 H13A 0.9500 . ? C14 C15 1.377(6) . ? C14 H14A 0.9500 . ? C15 C16 1.374(6) . ? C15 H15A 0.9500 . ? C16 H16A 0.9500 . ? C17 C18 1.398(5) . ? C18 C19 1.375(6) . ? C18 H18A 0.9500 . ? C19 C20 1.376(6) . ? C19 H19A 0.9500 . ? C20 C21 1.371(5) . ? C20 H20A 0.9500 . ? C21 H21A 0.9500 . ? C22 C27 1.368(7) . ? C22 C23 1.390(8) . ? C22 C28 1.520(8) . ? C23 C24 1.411(9) . ? C23 H23A 0.9500 . ? C24 C25 1.353(10) . ? C24 H24A 0.9500 . ? C25 C26 1.338(9) . ? C25 H25A 0.9500 . ? C26 C27 1.387(8) . ? C26 H26A 0.9500 . ? C27 H27A 0.9500 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? S1 O1 1.409(4) . ? S1 O2 1.419(3) . ? S1 O3 1.437(3) . ? S1 C29 1.758(6) . ? C29 F1 1.208(7) . ? C29 F3 1.369(8) . ? C29 F2 1.499(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 N3 Ru1 N3 86.18(16) . 2_656 ? N3 Ru1 N2 78.72(12) . . ? N3 Ru1 N2 94.54(11) 2_656 . ? N3 Ru1 N2 94.54(11) . 2_656 ? N3 Ru1 N2 78.72(12) 2_656 2_656 ? N2 Ru1 N2 170.85(16) . 2_656 ? N3 Ru1 N1 176.21(11) . . ? N3 Ru1 N1 91.20(11) 2_656 . ? N2 Ru1 N1 98.79(11) . . ? N2 Ru1 N1 87.62(11) 2_656 . ? N3 Ru1 N1 91.20(11) . 2_656 ? N3 Ru1 N1 176.21(12) 2_656 2_656 ? N2 Ru1 N1 87.62(11) . 2_656 ? N2 Ru1 N1 98.79(11) 2_656 2_656 ? N1 Ru1 N1 91.55(16) . 2_656 ? C1 N1 C5 118.3(3) . . ? C1 N1 Ru1 121.8(2) . . ? C5 N1 Ru1 119.4(2) . . ? C16 N2 C12 117.5(3) . . ? C16 N2 Ru1 127.1(3) . . ? C12 N2 Ru1 115.3(2) . . ? C21 N3 C17 117.6(3) . . ? C21 N3 Ru1 126.4(3) . . ? C17 N3 Ru1 115.7(2) . . ? C2 N4 C7 108.6(3) . . ? C2 N4 H4B 125.7 . . ? C7 N4 H4B 125.7 . . ? N1 C1 C2 120.8(3) . . ? N1 C1 H1A 119.6 . . ? C2 C1 H1A 119.6 . . ? N4 C2 C1 130.2(3) . . ? N4 C2 C3 108.9(3) . . ? C1 C2 C3 120.8(3) . . ? C4 C3 C2 117.4(3) . . ? C4 C3 C6 135.5(3) . . ? C2 C3 C6 107.1(3) . . ? C5 C4 C3 118.7(3) . . ? C5 C4 H4A 120.6 . . ? C3 C4 H4A 120.6 . . ? C4 C5 N1 123.8(3) . . ? C4 C5 H5A 118.1 . . ? N1 C5 H5A 118.1 . . ? C11 C6 C7 120.3(4) . . ? C11 C6 C3 133.6(4) . . ? C7 C6 C3 106.1(3) . . ? N4 C7 C8 129.6(4) . . ? N4 C7 C6 109.3(3) . . ? C8 C7 C6 121.2(4) . . ? C9 C8 C7 117.6(4) . . ? C9 C8 H8A 121.2 . . ? C7 C8 H8A 121.2 . . ? C8 C9 C10 121.8(4) . . ? C8 C9 H9A 119.1 . . ? C10 C9 H9A 119.1 . . ? C11 C10 C9 121.4(4) . . ? C11 C10 H10A 119.3 . . ? C9 C10 H10A 119.3 . . ? C10 C11 C6 117.7(4) . . ? C10 C11 H11A 121.1 . . ? C6 C11 H11A 121.1 . . ? N2 C12 C13 122.0(4) . . ? N2 C12 C17 114.6(3) . . ? C13 C12 C17 123.4(4) . . ? C12 C13 C14 120.2(4) . . ? C12 C13 H13A 119.9 . . ? C14 C13 H13A 119.9 . . ? C13 C14 C15 118.3(4) . . ? C13 C14 H14A 120.8 . . ? C15 C14 H14A 120.8 . . ? C16 C15 C14 119.3(4) . . ? C16 C15 H15A 120.4 . . ? C14 C15 H15A 120.4 . . ? N2 C16 C15 122.7(4) . . ? N2 C16 H16A 118.7 . . ? C15 C16 H16A 118.7 . . ? N3 C17 C18 121.4(3) . . ? N3 C17 C12 114.9(3) . . ? C18 C17 C12 123.7(3) . . ? C19 C18 C17 119.4(4) . . ? C19 C18 H18A 120.3 . . ? C17 C18 H18A 120.3 . . ? C18 C19 C20 119.3(4) . . ? C18 C19 H19A 120.4 . . ? C20 C19 H19A 120.4 . . ? C21 C20 C19 118.9(4) . . ? C21 C20 H20A 120.6 . . ? C19 C20 H20A 120.6 . . ? N3 C21 C20 123.4(4) . . ? N3 C21 H21A 118.3 . . ? C20 C21 H21A 118.3 . . ? C27 C22 C23 117.9(6) . . ? C27 C22 C28 121.2(6) . . ? C23 C22 C28 120.8(6) . . ? C22 C23 C24 119.6(6) . . ? C22 C23 H23A 120.2 . . ? C24 C23 H23A 120.2 . . ? C25 C24 C23 120.9(7) . . ? C25 C24 H24A 119.6 . . ? C23 C24 H24A 119.6 . . ? C26 C25 C24 119.0(7) . . ? C26 C25 H25A 120.5 . . ? C24 C25 H25A 120.5 . . ? C25 C26 C27 122.0(6) . . ? C25 C26 H26A 119.0 . . ? C27 C26 H26A 119.0 . . ? C22 C27 C26 120.6(6) . . ? C22 C27 H27A 119.7 . . ? C26 C27 H27A 119.7 . . ? C22 C28 H28A 109.5 . . ? C22 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C22 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? O1 S1 O2 113.8(3) . . ? O1 S1 O3 116.9(2) . . ? O2 S1 O3 114.0(2) . . ? O1 S1 C29 103.5(3) . . ? O2 S1 C29 101.7(3) . . ? O3 S1 C29 104.4(2) . . ? F1 C29 F3 114.2(8) . . ? F1 C29 F2 100.0(6) . . ? F3 C29 F2 96.0(6) . . ? F1 C29 S1 127.6(6) . . ? F3 C29 S1 108.9(5) . . ? F2 C29 S1 103.8(5) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N4 H4B O2 0.88 2.00 2.872(4) 170.6 2_656 N4 H4B S1 0.88 2.93 3.761(3) 157.3 2_656 _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.675 _refine_diff_density_min -0.381 _refine_diff_density_rms 0.084 # Attachment '772641.cif' data_772641 _database_code_depnum_ccdc_archive 'CCDC 772641' #TrackingRef '772641.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H38 F6 N8 O9 Ru S2' _chemical_formula_weight 1150.05 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 Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.7259(16) _cell_length_b 21.933(2) _cell_length_c 17.942(2) _cell_angle_alpha 90.00 _cell_angle_beta 109.690(2) _cell_angle_gamma 90.00 _cell_volume 5085.6(10) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.502 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2336 _exptl_absorpt_coefficient_mu 0.475 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8667 _exptl_absorpt_correction_T_max 0.9068 _exptl_absorpt_process_details ? _exptl_special_details ? _diffrn_ambient_temperature 173(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28214 _diffrn_reflns_av_R_equivalents 0.0428 _diffrn_reflns_av_sigmaI/netI 0.0570 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.52 _diffrn_reflns_theta_max 26.00 _reflns_number_total 9957 _reflns_number_gt 6252 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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. disorder: One of the Norharman moiety is disordered and refined with restrains on bond lengths and bond angles. ; _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 9957 _refine_ls_number_parameters 694 _refine_ls_number_restraints 111 _refine_ls_R_factor_all 0.1508 _refine_ls_R_factor_gt 0.1039 _refine_ls_wR_factor_ref 0.3449 _refine_ls_wR_factor_gt 0.2933 _refine_ls_goodness_of_fit_ref 1.293 _refine_ls_restrained_S_all 1.307 _refine_ls_shift/su_max 0.006 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_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 0.73170(5) 0.53438(3) 0.75499(3) 0.0331(3) Uani 1 1 d . . . N1 N 0.6103(5) 0.5989(3) 0.7256(4) 0.0426(16) Uani 1 1 d . . . N2 N 0.5244(7) 0.7433(4) 0.6255(5) 0.069(2) Uani 1 1 d . . . H2A H 0.5723 0.7610 0.6107 0.083 Uiso 1 1 calc R . . N3 N 0.8429(5) 0.6050(3) 0.7852(3) 0.0414(15) Uani 1 1 d D . . N5 N 0.7124(5) 0.5288(2) 0.6356(3) 0.0315(13) Uani 1 1 d . . . N6 N 0.6261(5) 0.4640(3) 0.7210(4) 0.0367(14) Uani 1 1 d . . . N7 N 0.8477(5) 0.4705(3) 0.7880(4) 0.0415(16) Uani 1 1 d . . . N8 N 0.7542(6) 0.5267(3) 0.8751(4) 0.0497(19) Uani 1 1 d . . . C1 C 0.6173(7) 0.6499(3) 0.6877(5) 0.0450(19) Uani 1 1 d . . . H1A H 0.6786 0.6581 0.6760 0.054 Uiso 1 1 calc R . . C2 C 0.5365(8) 0.6911(4) 0.6649(5) 0.059(3) Uani 1 1 d . . . C3 C 0.4421(8) 0.6759(6) 0.6782(6) 0.078(4) Uani 1 1 d . . . C4 C 0.4343(9) 0.6222(5) 0.7160(6) 0.071(3) Uani 1 1 d . . . H4A H 0.3725 0.6107 0.7250 0.086 Uiso 1 1 calc R . . C5 C 0.5222(7) 0.5865(5) 0.7397(5) 0.058(2) Uani 1 1 d . . . H5A H 0.5203 0.5503 0.7682 0.069 Uiso 1 1 calc R . . C6 C 0.3711(8) 0.7247(4) 0.6441(6) 0.064(3) Uani 1 1 d . . . C7 C 0.4251(10) 0.7659(5) 0.6110(8) 0.085(4) Uani 1 1 d . . . C8 C 0.3795(10) 0.8165(6) 0.5715(10) 0.117(6) Uani 1 1 d . . . H8A H 0.4165 0.8431 0.5489 0.140 Uiso 1 1 calc R . . C9 C 0.2782(14) 0.8288(7) 0.5645(10) 0.117(6) Uani 1 1 d . . . H9A H 0.2480 0.8656 0.5394 0.141 Uiso 1 1 calc R . . C10 C 0.2172(12) 0.7892(7) 0.5929(11) 0.126(6) Uani 1 1 d . . . H10A H 0.1468 0.7989 0.5844 0.151 Uiso 1 1 calc R . . C11 C 0.2636(12) 0.7317(8) 0.6364(10) 0.128(6) Uani 1 1 d . . . H11A H 0.2263 0.7034 0.6566 0.153 Uiso 1 1 calc R . . N4 N 0.9241(10) 0.7483(6) 0.8877(7) 0.111(4) Uani 1 1 d U . . H4B H 0.8831 0.7650 0.9106 0.133 Uiso 1 1 calc R . . C12 C 0.8285(7) 0.6544(3) 0.8273(4) 0.063(3) Uani 1 1 d DU . . H12A H 0.7674 0.6580 0.8406 0.076 Uiso 1 1 calc R . . C13 C 0.9050(10) 0.6995(4) 0.8503(6) 0.094(5) Uani 1 1 d DU . . C14 C 0.9956(9) 0.6947(5) 0.8294(7) 0.113(6) Uani 1 1 d DU . . C15 C 1.0075(7) 0.6460(5) 0.7880(6) 0.101(5) Uani 1 1 d DU . . H15A H 1.0675 0.6428 0.7730 0.121 Uiso 1 1 calc R . . C16 C 0.9321(6) 0.5997(4) 0.7665(5) 0.060(2) Uani 1 1 d DU . . H16A H 0.9427 0.5647 0.7390 0.072 Uiso 1 1 calc R . . C17 C 1.0757(10) 0.7387(5) 0.8526(6) 0.093(5) Uani 1 1 d DU . . C18 C 1.0203(11) 0.7744(7) 0.8892(10) 0.139(7) Uani 1 1 d DU . . C19 C 1.0635(12) 0.8251(6) 0.9305(10) 0.158(8) Uani 1 1 d DU . . H19A H 1.0258 0.8484 0.9564 0.189 Uiso 1 1 calc R . . C20 C 1.1621(11) 0.8432(6) 0.9352(9) 0.114(5) Uani 1 1 d DU . . H20A H 1.1934 0.8774 0.9668 0.137 Uiso 1 1 calc R . . C21 C 1.2149(10) 0.8120(6) 0.8944(9) 0.125(6) Uani 1 1 d DU . . H21A H 1.2805 0.8268 0.8956 0.150 Uiso 1 1 calc R . . C22 C 1.1760(12) 0.7600(6) 0.8518(8) 0.144(7) Uani 1 1 d DU . . H22A H 1.2127 0.7390 0.8232 0.173 Uiso 1 1 calc R . . C23 C 0.6491(5) 0.4829(3) 0.5972(4) 0.0316(15) Uani 1 1 d . . . C24 C 0.6269(6) 0.4701(3) 0.5160(4) 0.0358(17) Uani 1 1 d . . . C25 C 0.6738(6) 0.5053(4) 0.4751(4) 0.0421(19) Uani 1 1 d . . . H25A H 0.6632 0.4969 0.4210 0.050 Uiso 1 1 calc R . . C26 C 0.7365(7) 0.5531(4) 0.5123(5) 0.0447(19) Uani 1 1 d . . . H26A H 0.7674 0.5786 0.4838 0.054 Uiso 1 1 calc R . . C27 C 0.7541(6) 0.5634(4) 0.5926(4) 0.0397(17) Uani 1 1 d . . . H27A H 0.7975 0.5964 0.6179 0.048 Uiso 1 1 calc R . . C28 C 0.5577(6) 0.4202(4) 0.4828(4) 0.046(2) Uani 1 1 d . . . H28A H 0.5439 0.4096 0.4289 0.055 Uiso 1 1 calc R . . C29 C 0.5117(6) 0.3880(4) 0.5259(5) 0.045(2) Uani 1 1 d . . . H29A H 0.4649 0.3563 0.5011 0.054 Uiso 1 1 calc R . . C30 C 0.5319(6) 0.4006(3) 0.6078(4) 0.0385(17) Uani 1 1 d . . . C31 C 0.6012(6) 0.4483(3) 0.6424(4) 0.0320(15) Uani 1 1 d . . . C32 C 0.4841(7) 0.3701(4) 0.6544(5) 0.055(2) Uani 1 1 d . . . H32A H 0.4335 0.3396 0.6319 0.067 Uiso 1 1 calc R . . C33 C 0.5115(8) 0.3851(5) 0.7344(6) 0.068(3) Uani 1 1 d . . . H33A H 0.4821 0.3635 0.7675 0.081 Uiso 1 1 calc R . . C34 C 0.5829(7) 0.4322(4) 0.7655(5) 0.052(2) Uani 1 1 d . . . H34A H 0.6012 0.4419 0.8201 0.063 Uiso 1 1 calc R . . C35 C 0.8810(7) 0.4556(4) 0.8657(5) 0.050(2) Uani 1 1 d . . . C36 C 0.9642(8) 0.4122(4) 0.9001(6) 0.065(3) Uani 1 1 d . . . C37 C 1.0066(8) 0.3854(5) 0.8488(9) 0.080(4) Uani 1 1 d . . . H37A H 1.0614 0.3569 0.8683 0.096 Uiso 1 1 calc R . . C38 C 0.9718(8) 0.3992(5) 0.7720(7) 0.073(3) Uani 1 1 d . . . H38A H 1.0014 0.3798 0.7374 0.087 Uiso 1 1 calc R . . C39 C 0.8930(7) 0.4413(4) 0.7417(6) 0.051(2) Uani 1 1 d . . . H39A H 0.8701 0.4499 0.6866 0.062 Uiso 1 1 calc R . . C40 C 0.8291(8) 0.4866(4) 0.9122(5) 0.058(3) Uani 1 1 d . . . C41 C 0.8624(10) 0.4730(5) 0.9937(6) 0.065(3) Uani 1 1 d . . . C42 C 0.9399(13) 0.4308(7) 1.0275(6) 0.098(6) Uani 1 1 d . . . H42A H 0.9593 0.4218 1.0824 0.118 Uiso 1 1 calc R . . C43 C 0.9886(12) 0.4021(7) 0.9823(9) 0.128(8) Uani 1 1 d . . . H43A H 1.0419 0.3738 1.0075 0.154 Uiso 1 1 calc R . . C44 C 0.8142(12) 0.5019(6) 1.0358(6) 0.089(5) Uani 1 1 d . . . H44A H 0.8339 0.4933 1.0908 0.107 Uiso 1 1 calc R . . C45 C 0.7337(13) 0.5455(6) 1.0021(7) 0.097(5) Uani 1 1 d . . . H45A H 0.6999 0.5663 1.0330 0.117 Uiso 1 1 calc R . . C46 C 0.7071(9) 0.5558(5) 0.9178(5) 0.067(3) Uani 1 1 d . . . H46A H 0.6542 0.5843 0.8924 0.081 Uiso 1 1 calc R . . C47 C 0.0886(14) 0.5102(8) 0.6191(10) 0.110(5) Uani 1 1 d . . . S1 S 0.1835(3) 0.5265(2) 0.7111(2) 0.1026(13) Uani 1 1 d . . . O1 O 0.1370(9) 0.5043(7) 0.7650(6) 0.152(5) Uani 1 1 d . . . O2 O 0.1900(10) 0.5937(6) 0.7138(9) 0.158(5) Uani 1 1 d . . . O3 O 0.2755(8) 0.4956(5) 0.7041(6) 0.113(3) Uani 1 1 d . . . F1 F 0.0772(11) 0.4527(6) 0.6028(7) 0.173(5) Uani 1 1 d . . . F2 F 0.1107(9) 0.5311(5) 0.5566(6) 0.152(4) Uani 1 1 d . . . F3 F -0.0024(8) 0.5320(5) 0.6158(6) 0.151(4) Uani 1 1 d . . . C48 C 0.9020(13) 0.7226(6) 0.5832(10) 0.101(4) Uani 1 1 d . . . S2 S 0.7645(3) 0.74023(16) 0.5183(2) 0.0978(11) Uani 1 1 d . . . O4 O 0.7592(9) 0.7055(4) 0.4516(6) 0.118(3) Uani 1 1 d . . . O5 O 0.7090(8) 0.7136(4) 0.5640(7) 0.128(4) Uani 1 1 d . . . O6 O 0.7763(10) 0.8018(4) 0.5177(7) 0.139(4) Uani 1 1 d . . . F4 F 0.9686(7) 0.7480(4) 0.5556(7) 0.138(3) Uani 1 1 d . . . F5 F 0.9248(11) 0.7447(5) 0.6546(6) 0.190(6) Uani 1 1 d . . . F6 F 0.9230(8) 0.6632(4) 0.5907(8) 0.164(4) Uani 1 1 d . . . O1W O 0.661(2) 0.8479(7) 0.6394(18) 0.146(10) Uani 0.50 1 d P . . O1W' O 0.751(2) 0.8499(19) 0.719(3) 0.236(19) Uani 0.50 1 d P . . O2W O 0.428(2) 0.4668(19) 0.858(2) 0.174(15) Uani 0.50 1 d P . . O2W' O 0.476(3) 0.446(2) 0.907(3) 0.208(17) Uani 0.50 1 d P . . O3W O 0.562(3) 0.6624(9) 0.957(3) 0.24(2) Uani 0.50 1 d P . . O3W' O 0.511(2) 0.7232(18) 0.907(2) 0.24(2) Uani 0.50 1 d P . . 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 0.0339(4) 0.0392(4) 0.0204(4) -0.0005(2) 0.0017(3) -0.0026(3) N1 0.047(4) 0.047(4) 0.031(3) -0.014(3) 0.008(3) 0.002(3) N2 0.055(5) 0.071(5) 0.080(6) 0.007(5) 0.020(5) 0.012(4) N3 0.047(4) 0.038(3) 0.028(3) 0.001(3) -0.002(3) -0.003(3) N5 0.025(3) 0.040(3) 0.027(3) 0.001(2) 0.004(2) 0.002(2) N6 0.038(4) 0.039(3) 0.028(3) 0.004(3) 0.004(3) 0.001(3) N7 0.032(4) 0.039(3) 0.038(4) 0.013(3) -0.007(3) -0.009(3) N8 0.062(5) 0.056(4) 0.026(3) 0.000(3) 0.009(3) -0.021(4) C1 0.042(5) 0.041(4) 0.042(4) -0.004(3) 0.002(4) 0.006(4) C2 0.076(7) 0.051(5) 0.040(5) -0.014(4) 0.006(5) 0.007(5) C3 0.046(6) 0.124(10) 0.065(7) -0.051(7) 0.021(5) 0.009(6) C4 0.081(8) 0.080(7) 0.064(6) -0.002(5) 0.037(6) 0.011(6) C5 0.054(6) 0.074(6) 0.049(5) -0.017(5) 0.023(5) 0.000(5) C6 0.058(6) 0.061(6) 0.071(7) -0.011(5) 0.016(5) 0.025(5) C7 0.079(8) 0.056(6) 0.107(10) -0.008(6) 0.012(7) 0.007(6) C8 0.063(8) 0.084(9) 0.170(15) -0.035(9) -0.005(8) 0.037(7) C9 0.113(13) 0.079(9) 0.139(14) -0.014(9) 0.014(11) 0.030(9) C10 0.088(11) 0.083(9) 0.172(16) -0.025(10) -0.002(10) 0.057(9) C11 0.081(10) 0.155(15) 0.146(14) -0.064(12) 0.037(10) -0.016(10) N4 0.098(8) 0.126(8) 0.101(8) -0.008(7) 0.022(7) -0.011(7) C12 0.089(7) 0.045(5) 0.030(4) 0.008(4) -0.014(4) 0.000(5) C13 0.152(11) 0.033(5) 0.044(5) -0.002(4) -0.039(7) -0.010(6) C14 0.128(11) 0.082(8) 0.074(8) 0.037(7) -0.041(8) -0.059(8) C15 0.090(8) 0.108(9) 0.063(7) 0.045(6) -0.030(6) -0.049(7) C16 0.045(5) 0.080(6) 0.043(5) 0.017(4) 0.001(4) -0.013(5) C17 0.106(9) 0.070(7) 0.059(6) 0.025(5) -0.029(6) -0.058(7) C18 0.132(13) 0.111(11) 0.140(13) 0.057(10) -0.001(10) -0.027(10) C19 0.146(14) 0.128(11) 0.162(14) 0.056(10) 0.002(11) -0.050(11) C20 0.110(11) 0.090(9) 0.130(12) 0.011(8) 0.025(9) -0.044(8) C21 0.126(11) 0.082(8) 0.125(11) 0.012(8) -0.013(9) -0.070(8) C22 0.162(14) 0.138(12) 0.100(10) 0.023(9) 0.001(10) -0.054(11) C23 0.025(4) 0.035(3) 0.030(4) -0.004(3) 0.004(3) 0.004(3) C24 0.037(4) 0.036(4) 0.031(4) -0.005(3) 0.007(3) 0.013(3) C25 0.039(5) 0.064(5) 0.019(3) -0.005(3) 0.005(3) 0.010(4) C26 0.042(5) 0.059(5) 0.037(4) 0.007(4) 0.019(4) 0.004(4) C27 0.033(4) 0.048(4) 0.034(4) 0.001(3) 0.007(3) -0.001(3) C28 0.046(5) 0.049(4) 0.028(4) -0.013(3) -0.005(4) 0.009(4) C29 0.041(5) 0.042(4) 0.039(4) -0.005(3) -0.003(4) 0.007(4) C30 0.031(4) 0.037(4) 0.038(4) 0.004(3) -0.001(3) 0.005(3) C31 0.029(4) 0.036(4) 0.027(4) -0.002(3) 0.004(3) 0.004(3) C32 0.057(6) 0.054(5) 0.046(5) -0.003(4) 0.004(4) -0.023(4) C33 0.056(6) 0.079(7) 0.061(6) 0.012(5) 0.010(5) -0.029(5) C34 0.060(6) 0.063(5) 0.032(4) 0.001(4) 0.012(4) -0.019(5) C35 0.041(5) 0.046(5) 0.046(5) 0.004(4) -0.006(4) -0.018(4) C36 0.049(6) 0.055(5) 0.059(6) 0.030(5) -0.024(5) -0.031(5) C37 0.043(6) 0.063(6) 0.120(11) 0.015(7) 0.010(7) 0.003(5) C38 0.049(6) 0.067(6) 0.088(8) 0.013(6) 0.005(5) 0.006(5) C39 0.038(5) 0.047(5) 0.064(6) 0.007(4) 0.011(4) 0.007(4) C40 0.066(6) 0.049(5) 0.032(4) 0.016(4) -0.019(4) -0.040(5) C41 0.091(8) 0.064(6) 0.026(5) -0.002(4) 0.001(5) -0.038(6) C42 0.120(12) 0.100(10) 0.034(6) 0.026(6) -0.030(7) -0.068(9) C43 0.089(11) 0.099(11) 0.119(12) 0.077(10) -0.068(9) -0.055(9) C44 0.121(11) 0.083(8) 0.040(6) 0.019(6) -0.005(7) -0.052(8) C45 0.143(13) 0.110(10) 0.056(7) -0.046(7) 0.056(8) -0.071(10) C46 0.096(9) 0.082(6) 0.028(4) -0.015(4) 0.027(5) -0.018(6) C47 0.114(13) 0.111(11) 0.119(13) -0.017(10) 0.058(11) 0.011(10) S1 0.099(3) 0.139(3) 0.088(3) -0.004(2) 0.055(2) -0.036(2) O1 0.131(10) 0.243(13) 0.090(7) 0.020(8) 0.047(7) -0.079(10) O2 0.130(10) 0.146(10) 0.240(14) -0.062(10) 0.117(10) -0.058(8) O3 0.102(8) 0.122(8) 0.105(7) 0.020(6) 0.022(6) 0.024(6) F1 0.187(12) 0.159(10) 0.147(10) -0.061(8) 0.021(9) -0.008(8) F2 0.148(9) 0.215(11) 0.126(8) 0.057(6) 0.091(7) 0.063(7) F3 0.091(7) 0.249(12) 0.129(8) -0.034(7) 0.059(6) 0.015(6) C48 0.125(13) 0.077(9) 0.111(11) 0.021(8) 0.050(10) -0.013(8) S2 0.117(3) 0.085(2) 0.107(3) -0.0112(19) 0.058(2) -0.047(2) O4 0.143(9) 0.098(6) 0.103(7) -0.020(5) 0.029(7) -0.038(6) O5 0.119(8) 0.088(6) 0.204(11) 0.047(6) 0.092(8) 0.005(5) O6 0.162(11) 0.056(5) 0.187(11) 0.029(6) 0.043(9) -0.011(6) F4 0.104(7) 0.122(6) 0.205(10) 0.005(6) 0.074(7) -0.029(5) F5 0.281(17) 0.184(10) 0.079(6) -0.003(6) 0.028(8) -0.017(10) F6 0.147(9) 0.082(6) 0.273(13) 0.036(7) 0.083(9) -0.006(5) O1W 0.19(2) 0.067(10) 0.25(3) -0.026(14) 0.17(2) -0.033(13) O1W' 0.10(2) 0.28(4) 0.33(4) -0.15(4) 0.07(2) -0.03(2) O2W 0.12(2) 0.28(4) 0.14(2) 0.04(2) 0.068(19) 0.11(2) O2W' 0.14(3) 0.20(3) 0.28(5) 0.01(3) 0.07(3) 0.06(3) O3W 0.35(5) 0.057(12) 0.47(6) 0.033(19) 0.32(4) 0.041(18) O3W' 0.19(3) 0.34(5) 0.22(3) 0.18(3) 0.12(3) 0.15(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 N7 2.053(7) . ? Ru1 N6 2.064(6) . ? Ru1 N5 2.072(6) . ? Ru1 N8 2.078(7) . ? Ru1 N3 2.113(6) . ? Ru1 N1 2.113(7) . ? N1 C1 1.329(10) . ? N1 C5 1.345(11) . ? N2 C2 1.325(12) . ? N2 C7 1.389(15) . ? N2 H2A 0.8800 . ? N3 C12 1.373(9) . ? N3 C16 1.379(10) . ? N5 C27 1.340(10) . ? N5 C23 1.357(9) . ? N6 C34 1.340(10) . ? N6 C31 1.377(9) . ? N7 C35 1.353(11) . ? N7 C39 1.356(12) . ? N8 C46 1.321(12) . ? N8 C40 1.347(12) . ? C1 C2 1.382(12) . ? C1 H1A 0.9500 . ? C2 C3 1.433(15) . ? C3 C4 1.380(16) . ? C3 C6 1.438(15) . ? C4 C5 1.380(14) . ? C4 H4A 0.9500 . ? C5 H5A 0.9500 . ? C6 C7 1.420(16) . ? C6 C11 1.444(18) . ? C7 C8 1.352(17) . ? C8 C9 1.38(2) . ? C8 H8A 0.9500 . ? C9 C10 1.41(2) . ? C9 H9A 0.9500 . ? C10 C11 1.51(2) . ? C10 H10A 0.9500 . ? C11 H11A 0.9500 . ? N4 C13 1.244(14) . ? N4 C18 1.431(16) . ? N4 H4B 0.8800 . ? C12 C13 1.400(11) . ? C12 H12A 0.9500 . ? C13 C14 1.418(14) . ? C14 C15 1.342(13) . ? C14 C17 1.417(10) . ? C15 C16 1.408(11) . ? C15 H15A 0.9500 . ? C16 H16A 0.9500 . ? C17 C18 1.398(15) . ? C17 C22 1.458(14) . ? C18 C19 1.358(14) . ? C19 C20 1.386(13) . ? C19 H19A 0.9500 . ? C20 C21 1.374(13) . ? C20 H20A 0.9500 . ? C21 C22 1.377(12) . ? C21 H21A 0.9500 . ? C22 H22A 0.9500 . ? C23 C24 1.412(10) . ? C23 C31 1.423(11) . ? C24 C25 1.367(11) . ? C24 C28 1.441(11) . ? C25 C26 1.377(12) . ? C25 H25A 0.9500 . ? C26 C27 1.397(11) . ? C26 H26A 0.9500 . ? C27 H27A 0.9500 . ? C28 C29 1.349(12) . ? C28 H28A 0.9500 . ? C29 C30 1.428(11) . ? C29 H29A 0.9500 . ? C30 C32 1.395(12) . ? C30 C31 1.410(10) . ? C32 C33 1.394(13) . ? C32 H32A 0.9500 . ? C33 C34 1.405(12) . ? C33 H33A 0.9500 . ? C34 H34A 0.9500 . ? C35 C40 1.436(15) . ? C35 C36 1.455(13) . ? C36 C37 1.376(16) . ? C36 C43 1.416(18) . ? C37 C38 1.331(16) . ? C37 H37A 0.9500 . ? C38 C39 1.386(13) . ? C38 H38A 0.9500 . ? C39 H39A 0.9500 . ? C40 C41 1.409(12) . ? C41 C44 1.321(18) . ? C41 C42 1.387(19) . ? C42 C43 1.37(2) . ? C42 H42A 0.9500 . ? C43 H43A 0.9500 . ? C44 C45 1.43(2) . ? C44 H44A 0.9500 . ? C45 C46 1.450(14) . ? C45 H45A 0.9500 . ? C46 H46A 0.9500 . ? C47 F1 1.292(18) . ? C47 F3 1.321(18) . ? C47 F2 1.337(18) . ? C47 S1 1.760(18) . ? S1 O1 1.414(10) . ? S1 O2 1.476(12) . ? S1 O3 1.474(11) . ? C48 F4 1.301(15) . ? C48 F5 1.304(16) . ? C48 F6 1.332(15) . ? C48 S2 1.894(17) . ? S2 O6 1.360(8) . ? S2 O4 1.400(10) . ? S2 O5 1.420(9) . ? O1W O1W' 1.54(4) . ? O2W O2W' 1.00(4) . ? O3W O3W' 1.62(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 N7 Ru1 N6 88.5(3) . . ? N7 Ru1 N5 94.3(3) . . ? N6 Ru1 N5 79.5(2) . . ? N7 Ru1 N8 79.4(3) . . ? N6 Ru1 N8 95.2(3) . . ? N5 Ru1 N8 171.9(3) . . ? N7 Ru1 N3 90.2(2) . . ? N6 Ru1 N3 177.0(2) . . ? N5 Ru1 N3 97.9(2) . . ? N8 Ru1 N3 87.2(2) . . ? N7 Ru1 N1 177.3(3) . . ? N6 Ru1 N1 90.7(3) . . ? N5 Ru1 N1 88.0(2) . . ? N8 Ru1 N1 98.2(3) . . ? N3 Ru1 N1 90.8(3) . . ? C1 N1 C5 119.5(8) . . ? C1 N1 Ru1 120.3(6) . . ? C5 N1 Ru1 120.0(6) . . ? C2 N2 C7 110.3(10) . . ? C2 N2 H2A 124.8 . . ? C7 N2 H2A 124.8 . . ? C12 N3 C16 120.3(6) . . ? C12 N3 Ru1 119.6(5) . . ? C16 N3 Ru1 120.0(5) . . ? C27 N5 C23 116.9(6) . . ? C27 N5 Ru1 129.2(5) . . ? C23 N5 Ru1 114.0(5) . . ? C34 N6 C31 118.3(6) . . ? C34 N6 Ru1 128.3(5) . . ? C31 N6 Ru1 113.4(5) . . ? C35 N7 C39 116.9(7) . . ? C35 N7 Ru1 115.0(6) . . ? C39 N7 Ru1 128.1(6) . . ? C46 N8 C40 118.1(8) . . ? C46 N8 Ru1 129.1(7) . . ? C40 N8 Ru1 112.8(6) . . ? N1 C1 C2 120.8(9) . . ? N1 C1 H1A 119.6 . . ? C2 C1 H1A 119.6 . . ? N2 C2 C1 131.8(10) . . ? N2 C2 C3 109.4(10) . . ? C1 C2 C3 118.6(10) . . ? C4 C3 C2 120.3(10) . . ? C4 C3 C6 133.6(11) . . ? C2 C3 C6 106.1(11) . . ? C5 C4 C3 115.6(10) . . ? C5 C4 H4A 122.2 . . ? C3 C4 H4A 122.2 . . ? N1 C5 C4 125.1(10) . . ? N1 C5 H5A 117.5 . . ? C4 C5 H5A 117.5 . . ? C7 C6 C3 106.1(10) . . ? C7 C6 C11 123.6(12) . . ? C3 C6 C11 130.1(13) . . ? C8 C7 N2 130.1(13) . . ? C8 C7 C6 121.7(13) . . ? N2 C7 C6 108.2(9) . . ? C7 C8 C9 118.9(17) . . ? C7 C8 H8A 120.5 . . ? C9 C8 H8A 120.5 . . ? C8 C9 C10 123.2(15) . . ? C8 C9 H9A 118.4 . . ? C10 C9 H9A 118.4 . . ? C9 C10 C11 120.1(14) . . ? C9 C10 H10A 119.9 . . ? C11 C10 H10A 119.9 . . ? C6 C11 C10 112.2(15) . . ? C6 C11 H11A 123.9 . . ? C10 C11 H11A 123.9 . . ? C13 N4 C18 112.3(14) . . ? C13 N4 H4B 123.9 . . ? C18 N4 H4B 123.9 . . ? N3 C12 C13 119.2(7) . . ? N3 C12 H12A 120.4 . . ? C13 C12 H12A 120.4 . . ? N4 C13 C14 99.4(12) . . ? N4 C13 C12 140.2(13) . . ? C14 C13 C12 120.4(7) . . ? C15 C14 C17 118.5(12) . . ? C15 C14 C13 119.2(7) . . ? C17 C14 C13 122.3(12) . . ? C14 C15 C16 120.6(8) . . ? C14 C15 H15A 119.7 . . ? C16 C15 H15A 119.7 . . ? N3 C16 C15 120.3(7) . . ? N3 C16 H16A 119.8 . . ? C15 C16 H16A 119.8 . . ? C14 C17 C18 91.6(12) . . ? C14 C17 C22 149.0(13) . . ? C18 C17 C22 119.3(7) . . ? C19 C18 C17 120.6(9) . . ? C19 C18 N4 124.5(15) . . ? C17 C18 N4 114.3(13) . . ? C18 C19 C20 120.3(9) . . ? C18 C19 H19A 119.8 . . ? C20 C19 H19A 119.8 . . ? C21 C20 C19 120.3(8) . . ? C21 C20 H20A 119.8 . . ? C19 C20 H20A 119.8 . . ? C20 C21 C22 122.2(8) . . ? C20 C21 H21A 118.9 . . ? C22 C21 H21A 118.9 . . ? C21 C22 C17 116.8(9) . . ? C21 C22 H22A 121.6 . . ? C17 C22 H22A 121.6 . . ? N5 C23 C24 123.4(7) . . ? N5 C23 C31 116.5(6) . . ? C24 C23 C31 120.1(6) . . ? C25 C24 C23 117.8(7) . . ? C25 C24 C28 124.9(7) . . ? C23 C24 C28 117.3(7) . . ? C24 C25 C26 119.9(7) . . ? C24 C25 H25A 120.0 . . ? C26 C25 H25A 120.0 . . ? C25 C26 C27 119.1(7) . . ? C25 C26 H26A 120.4 . . ? C27 C26 H26A 120.4 . . ? N5 C27 C26 122.9(7) . . ? N5 C27 H27A 118.5 . . ? C26 C27 H27A 118.6 . . ? C29 C28 C24 122.1(7) . . ? C29 C28 H28A 118.9 . . ? C24 C28 H28A 118.9 . . ? C28 C29 C30 121.5(7) . . ? C28 C29 H29A 119.3 . . ? C30 C29 H29A 119.3 . . ? C32 C30 C31 118.4(7) . . ? C32 C30 C29 123.8(7) . . ? C31 C30 C29 117.7(7) . . ? N6 C31 C30 122.3(7) . . ? N6 C31 C23 116.6(6) . . ? C30 C31 C23 121.1(6) . . ? C33 C32 C30 119.0(8) . . ? C33 C32 H32A 120.5 . . ? C30 C32 H32A 120.5 . . ? C32 C33 C34 119.5(8) . . ? C32 C33 H33A 120.2 . . ? C34 C33 H33A 120.2 . . ? N6 C34 C33 122.3(8) . . ? N6 C34 H34A 118.8 . . ? C33 C34 H34A 118.8 . . ? N7 C35 C40 115.0(8) . . ? N7 C35 C36 122.6(10) . . ? C40 C35 C36 122.4(9) . . ? C37 C36 C43 128.7(13) . . ? C37 C36 C35 116.4(9) . . ? C43 C36 C35 114.8(13) . . ? C38 C37 C36 120.6(10) . . ? C38 C37 H37A 119.7 . . ? C36 C37 H37A 119.7 . . ? C37 C38 C39 121.2(12) . . ? C37 C38 H38A 119.4 . . ? C39 C38 H38A 119.4 . . ? N7 C39 C38 122.1(9) . . ? N7 C39 H39A 118.9 . . ? C38 C39 H39A 118.9 . . ? N8 C40 C41 125.3(11) . . ? N8 C40 C35 117.9(7) . . ? C41 C40 C35 116.8(10) . . ? C44 C41 C40 116.3(12) . . ? C44 C41 C42 121.8(11) . . ? C40 C41 C42 121.9(12) . . ? C43 C42 C41 120.3(10) . . ? C43 C42 H42A 119.9 . . ? C41 C42 H42A 119.9 . . ? C42 C43 C36 123.8(13) . . ? C42 C43 H43A 118.1 . . ? C36 C43 H43A 118.1 . . ? C41 C44 C45 122.9(10) . . ? C41 C44 H44A 118.6 . . ? C45 C44 H44A 118.6 . . ? C46 C45 C44 115.5(11) . . ? C46 C45 H45A 122.2 . . ? C44 C45 H45A 122.2 . . ? N8 C46 C45 122.0(11) . . ? N8 C46 H46A 119.0 . . ? C45 C46 H46A 119.0 . . ? F1 C47 F3 107.7(16) . . ? F1 C47 F2 100.9(13) . . ? F3 C47 F2 108.5(14) . . ? F1 C47 S1 114.0(13) . . ? F3 C47 S1 111.0(11) . . ? F2 C47 S1 114.3(13) . . ? O1 S1 O2 111.0(8) . . ? O1 S1 O3 119.8(9) . . ? O2 S1 O3 114.7(6) . . ? O1 S1 C47 102.1(8) . . ? O2 S1 C47 104.5(9) . . ? O3 S1 C47 102.2(7) . . ? F4 C48 F5 104.4(13) . . ? F4 C48 F6 107.6(13) . . ? F5 C48 F6 106.9(13) . . ? F4 C48 S2 111.2(10) . . ? F5 C48 S2 112.8(12) . . ? F6 C48 S2 113.5(11) . . ? O6 S2 O4 120.4(8) . . ? O6 S2 O5 120.1(8) . . ? O4 S2 O5 112.7(7) . . ? O6 S2 C48 96.3(7) . . ? O4 S2 C48 99.7(7) . . ? O5 S2 C48 100.3(7) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 3.307 _refine_diff_density_min -1.054 _refine_diff_density_rms 0.217