# 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 ? _publ_contact_author_email fuyi.wang@iccas.ac.cn _publ_contact_author_name 'Fuyi Wang' loop_ _publ_author_name 'Yumiao Han' 'Qun Luo' 'Xiang Hao' 'Xianchan Li' 'Fuyi Wang' 'Wenbing Hu' 'Kui Wu' 'Shuang Lv' 'Peter J. Sadler' data_sa76 _database_code_depnum_ccdc_archive 'CCDC 821489' #TrackingRef '5003_web_deposit_cif_file_0_FuyiWang_1302593773.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C13 H11 N O S' _chemical_formula_sum 'C13 H11 N O S' _chemical_formula_weight 229.29 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 9.6385(19) _cell_length_b 11.635(2) _cell_length_c 20.051(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2248.5(8) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 456 _cell_measurement_theta_min 2.17 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.37 _exptl_crystal_size_mid 0.29 _exptl_crystal_size_min 0.26 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.355 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 960 _exptl_absorpt_coefficient_mu 0.263 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.9088 _exptl_absorpt_correction_T_max 0.9347 _exptl_absorpt_process_details 'CrystalClear (Rigaku Inc., 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Saturn724+ CCD' _diffrn_measurement_method '\w scans at fixed \c = 45\%' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18364 _diffrn_reflns_av_R_equivalents 0.0350 _diffrn_reflns_av_sigmaI/netI 0.0299 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.74 _diffrn_reflns_theta_max 27.49 _reflns_number_total 5149 _reflns_number_gt 4983 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2008)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2008)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP in Siemens SHELXTL (Sheldrick, 1994)' _computing_publication_material 'SHELX97 (Sheldrick, 1997)' _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^)+(0.0414P)^2^+0.2948P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.02(5) _refine_ls_number_reflns 5149 _refine_ls_number_parameters 289 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0370 _refine_ls_R_factor_gt 0.0355 _refine_ls_wR_factor_ref 0.0859 _refine_ls_wR_factor_gt 0.0849 _refine_ls_goodness_of_fit_ref 1.077 _refine_ls_restrained_S_all 1.077 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group S1 S 0.49341(4) 0.58676(4) 0.15311(2) 0.03407(11) Uani 1 1 d . . . H1 H 0.4069 0.6589 0.1574 0.041 Uiso 1 1 d R . . S2 S 1.03395(5) 0.39306(4) -0.11182(2) 0.03814(12) Uani 1 1 d . . . H2 H 1.1158 0.3202 -0.1106 0.046 Uiso 1 1 d R . . O1 O 0.73353(14) 0.43879(10) 0.13847(6) 0.0354(3) Uani 1 1 d . . . O2 O 0.77897(15) 0.52860(11) -0.10749(6) 0.0403(3) Uani 1 1 d . . . N1 N 0.79392(16) 0.41919(12) 0.02978(7) 0.0314(3) Uani 1 1 d . . . H1A H 0.7971 0.4537 -0.0092 0.038 Uiso 1 1 calc R . . N2 N 0.72677(15) 0.58213(12) -0.21367(7) 0.0319(3) Uani 1 1 d . . . H2A H 0.7224 0.5572 -0.2551 0.038 Uiso 1 1 calc R . . C1 C 0.5894(2) 0.77919(16) 0.08816(9) 0.0330(4) Uani 1 1 d . . . H1B H 0.5141 0.8185 0.1085 0.040 Uiso 1 1 calc R . . C2 C 0.6787(2) 0.83837(16) 0.04682(9) 0.0369(4) Uani 1 1 d . . . H2B H 0.6650 0.9183 0.0396 0.044 Uiso 1 1 calc R . . C3 C 0.7883(2) 0.78273(16) 0.01570(9) 0.0354(4) Uani 1 1 d . . . H3A H 0.8492 0.8239 -0.0129 0.042 Uiso 1 1 calc R . . C4 C 0.80776(19) 0.66660(16) 0.02675(8) 0.0315(4) Uani 1 1 d . . . H4A H 0.8823 0.6280 0.0053 0.038 Uiso 1 1 calc R . . C5 C 0.71932(17) 0.60493(14) 0.06907(8) 0.0272(3) Uani 1 1 d . . . C6 C 0.60870(17) 0.66196(15) 0.10045(8) 0.0284(3) Uani 1 1 d . . . C7 C 0.74845(18) 0.48082(15) 0.08242(8) 0.0288(3) Uani 1 1 d . . . C8 C 0.83718(18) 0.30227(15) 0.03289(9) 0.0298(4) Uani 1 1 d . . . C9 C 0.7971(2) 0.22815(16) -0.01778(9) 0.0365(4) Uani 1 1 d . . . H9A H 0.7374 0.2543 -0.0523 0.044 Uiso 1 1 calc R . . C10 C 0.8448(2) 0.11560(17) -0.01785(10) 0.0439(5) Uani 1 1 d . . . H10A H 0.8183 0.0650 -0.0528 0.053 Uiso 1 1 calc R . . C11 C 0.9302(2) 0.07681(17) 0.03234(11) 0.0438(5) Uani 1 1 d . . . H11A H 0.9627 -0.0003 0.0320 0.053 Uiso 1 1 calc R . . C12 C 0.9684(2) 0.15020(17) 0.08309(10) 0.0418(4) Uani 1 1 d . . . H12A H 1.0261 0.1229 0.1181 0.050 Uiso 1 1 calc R . . C13 C 0.92345(19) 0.26348(16) 0.08363(9) 0.0346(4) Uani 1 1 d . . . H13A H 0.9514 0.3140 0.1183 0.042 Uiso 1 1 calc R . . C14 C 0.9421(2) 0.21599(16) -0.19169(9) 0.0353(4) Uani 1 1 d . . . H14A H 1.0198 0.1743 -0.1756 0.042 Uiso 1 1 calc R . . C15 C 0.8540(2) 0.16571(16) -0.23766(10) 0.0375(4) Uani 1 1 d . . . H15A H 0.8723 0.0901 -0.2532 0.045 Uiso 1 1 calc R . . C16 C 0.7394(2) 0.22490(16) -0.26120(10) 0.0367(4) Uani 1 1 d . . . H16A H 0.6784 0.1897 -0.2923 0.044 Uiso 1 1 calc R . . C17 C 0.71443(19) 0.33567(17) -0.23919(9) 0.0341(4) Uani 1 1 d . . . H17A H 0.6367 0.3768 -0.2559 0.041 Uiso 1 1 calc R . . C18 C 0.80234(17) 0.38788(15) -0.19261(8) 0.0288(3) Uani 1 1 d . . . C19 C 0.91779(18) 0.32739(15) -0.16876(8) 0.0302(4) Uani 1 1 d . . . C20 C 0.76912(18) 0.50542(15) -0.16708(8) 0.0307(4) Uani 1 1 d . . . C21 C 0.68876(18) 0.69832(15) -0.20272(9) 0.0310(4) Uani 1 1 d . . . C22 C 0.70272(19) 0.77408(16) -0.25580(9) 0.0330(4) Uani 1 1 d . . . H22A H 0.7357 0.7466 -0.2975 0.040 Uiso 1 1 calc R . . C23 C 0.66904(19) 0.88952(16) -0.24869(9) 0.0357(4) Uani 1 1 d . . . H23A H 0.6793 0.9405 -0.2854 0.043 Uiso 1 1 calc R . . C24 C 0.62061(19) 0.93035(16) -0.18829(10) 0.0365(4) Uani 1 1 d . . . H24A H 0.5990 1.0095 -0.1830 0.044 Uiso 1 1 calc R . . C25 C 0.6039(2) 0.85438(17) -0.13550(10) 0.0394(4) Uani 1 1 d . . . H25A H 0.5687 0.8820 -0.0943 0.047 Uiso 1 1 calc R . . C26 C 0.63747(19) 0.73913(16) -0.14174(9) 0.0358(4) Uani 1 1 d . . . H26A H 0.6259 0.6883 -0.1051 0.043 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 S1 0.0319(2) 0.0351(2) 0.0352(2) -0.00079(18) 0.00760(17) -0.00055(19) S2 0.0347(2) 0.0448(3) 0.0350(2) -0.0029(2) -0.00678(19) -0.0007(2) O1 0.0472(7) 0.0351(6) 0.0240(6) 0.0035(5) 0.0065(5) 0.0072(6) O2 0.0563(9) 0.0408(7) 0.0239(6) -0.0011(6) -0.0029(6) 0.0085(6) N1 0.0406(8) 0.0306(7) 0.0229(7) 0.0017(6) 0.0034(6) 0.0051(7) N2 0.0392(8) 0.0328(7) 0.0237(7) -0.0025(6) -0.0001(6) 0.0020(7) C1 0.0353(9) 0.0320(9) 0.0317(9) -0.0029(7) 0.0003(7) 0.0034(7) C2 0.0460(11) 0.0306(9) 0.0342(9) 0.0023(8) 0.0015(8) 0.0028(8) C3 0.0405(10) 0.0332(9) 0.0325(9) 0.0031(7) 0.0044(8) -0.0034(8) C4 0.0337(9) 0.0350(9) 0.0259(8) -0.0018(7) 0.0017(7) 0.0015(8) C5 0.0307(8) 0.0293(8) 0.0216(7) 0.0007(6) -0.0012(6) 0.0008(7) C6 0.0299(8) 0.0319(8) 0.0235(8) -0.0019(7) -0.0008(6) -0.0002(7) C7 0.0269(8) 0.0326(9) 0.0268(8) 0.0000(7) 0.0023(7) 0.0019(7) C8 0.0302(9) 0.0304(8) 0.0288(9) 0.0004(7) 0.0075(7) 0.0032(7) C9 0.0400(10) 0.0368(10) 0.0326(9) -0.0031(8) 0.0006(8) 0.0011(8) C10 0.0520(12) 0.0347(10) 0.0451(11) -0.0105(9) 0.0077(9) -0.0030(9) C11 0.0441(11) 0.0308(9) 0.0566(13) 0.0004(10) 0.0087(9) 0.0069(9) C12 0.0394(10) 0.0397(10) 0.0462(11) 0.0066(9) -0.0001(9) 0.0088(9) C13 0.0353(9) 0.0357(9) 0.0328(9) -0.0019(8) 0.0010(7) 0.0046(8) C14 0.0342(9) 0.0336(9) 0.0382(10) 0.0050(8) 0.0003(8) -0.0003(8) C15 0.0442(11) 0.0292(9) 0.0391(10) 0.0002(8) 0.0020(8) -0.0048(8) C16 0.0391(10) 0.0359(10) 0.0353(10) -0.0024(8) -0.0049(8) -0.0082(8) C17 0.0305(9) 0.0397(10) 0.0321(9) 0.0026(8) -0.0024(7) -0.0023(8) C18 0.0306(8) 0.0331(9) 0.0228(7) 0.0015(7) 0.0025(6) -0.0027(7) C19 0.0304(8) 0.0342(9) 0.0261(8) 0.0026(7) 0.0020(7) -0.0034(7) C20 0.0294(9) 0.0358(9) 0.0271(8) 0.0018(7) 0.0007(7) -0.0007(7) C21 0.0284(8) 0.0350(9) 0.0295(9) -0.0010(7) -0.0014(7) 0.0010(7) C22 0.0333(9) 0.0376(10) 0.0281(9) -0.0004(7) 0.0002(7) 0.0023(8) C23 0.0358(10) 0.0361(10) 0.0351(10) 0.0041(8) -0.0033(7) -0.0010(8) C24 0.0321(9) 0.0334(9) 0.0439(10) -0.0030(8) -0.0018(8) 0.0033(8) C25 0.0378(10) 0.0455(11) 0.0349(10) -0.0063(9) 0.0040(8) 0.0070(9) C26 0.0361(9) 0.0412(10) 0.0300(9) 0.0018(8) 0.0037(7) 0.0014(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 S1 C6 1.7650(17) . ? S1 H1 1.1864 . ? S2 C19 1.7723(18) . ? S2 H2 1.1586 . ? O1 C7 1.234(2) . ? O2 C20 1.229(2) . ? N1 C7 1.349(2) . ? N1 C8 1.424(2) . ? N1 H1A 0.8800 . ? N2 C20 1.355(2) . ? N2 C21 1.418(2) . ? N2 H2A 0.8800 . ? C1 C2 1.379(3) . ? C1 C6 1.398(2) . ? C1 H1B 0.9500 . ? C2 C3 1.387(3) . ? C2 H2B 0.9500 . ? C3 C4 1.382(3) . ? C3 H3A 0.9500 . ? C4 C5 1.401(2) . ? C4 H4A 0.9500 . ? C5 C6 1.405(2) . ? C5 C7 1.495(2) . ? C8 C9 1.387(2) . ? C8 C13 1.389(2) . ? C9 C10 1.388(3) . ? C9 H9A 0.9500 . ? C10 C11 1.376(3) . ? C10 H10A 0.9500 . ? C11 C12 1.379(3) . ? C11 H11A 0.9500 . ? C12 C13 1.387(3) . ? C12 H12A 0.9500 . ? C13 H13A 0.9500 . ? C14 C15 1.383(3) . ? C14 C19 1.395(3) . ? C14 H14A 0.9500 . ? C15 C16 1.384(3) . ? C15 H15A 0.9500 . ? C16 C17 1.383(3) . ? C16 H16A 0.9500 . ? C17 C18 1.400(2) . ? C17 H17A 0.9500 . ? C18 C19 1.401(2) . ? C18 C20 1.495(2) . ? C21 C22 1.388(2) . ? C21 C26 1.402(2) . ? C22 C23 1.389(3) . ? C22 H22A 0.9500 . ? C23 C24 1.382(3) . ? C23 H23A 0.9500 . ? C24 C25 1.388(3) . ? C24 H24A 0.9500 . ? C25 C26 1.385(3) . ? C25 H25A 0.9500 . ? C26 H26A 0.9500 . ? 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 C6 S1 H1 97.8 . . ? C19 S2 H2 97.3 . . ? C7 N1 C8 124.65(15) . . ? C7 N1 H1A 117.7 . . ? C8 N1 H1A 117.7 . . ? C20 N2 C21 126.81(15) . . ? C20 N2 H2A 116.6 . . ? C21 N2 H2A 116.6 . . ? C2 C1 C6 120.67(17) . . ? C2 C1 H1B 119.7 . . ? C6 C1 H1B 119.7 . . ? C1 C2 C3 120.84(17) . . ? C1 C2 H2B 119.6 . . ? C3 C2 H2B 119.6 . . ? C4 C3 C2 119.17(18) . . ? C4 C3 H3A 120.4 . . ? C2 C3 H3A 120.4 . . ? C3 C4 C5 121.03(17) . . ? C3 C4 H4A 119.5 . . ? C5 C4 H4A 119.5 . . ? C4 C5 C6 119.43(15) . . ? C4 C5 C7 119.27(15) . . ? C6 C5 C7 121.23(15) . . ? C1 C6 C5 118.85(16) . . ? C1 C6 S1 120.35(13) . . ? C5 C6 S1 120.78(13) . . ? O1 C7 N1 122.66(16) . . ? O1 C7 C5 121.60(15) . . ? N1 C7 C5 115.73(14) . . ? C9 C8 C13 120.05(17) . . ? C9 C8 N1 118.70(16) . . ? C13 C8 N1 121.17(16) . . ? C8 C9 C10 119.68(18) . . ? C8 C9 H9A 120.2 . . ? C10 C9 H9A 120.2 . . ? C11 C10 C9 120.45(19) . . ? C11 C10 H10A 119.8 . . ? C9 C10 H10A 119.8 . . ? C10 C11 C12 119.76(19) . . ? C10 C11 H11A 120.1 . . ? C12 C11 H11A 120.1 . . ? C11 C12 C13 120.72(19) . . ? C11 C12 H12A 119.6 . . ? C13 C12 H12A 119.6 . . ? C12 C13 C8 119.33(18) . . ? C12 C13 H13A 120.3 . . ? C8 C13 H13A 120.3 . . ? C15 C14 C19 120.65(17) . . ? C15 C14 H14A 119.7 . . ? C19 C14 H14A 119.7 . . ? C14 C15 C16 120.43(17) . . ? C14 C15 H15A 119.8 . . ? C16 C15 H15A 119.8 . . ? C17 C16 C15 119.57(18) . . ? C17 C16 H16A 120.2 . . ? C15 C16 H16A 120.2 . . ? C16 C17 C18 120.78(18) . . ? C16 C17 H17A 119.6 . . ? C18 C17 H17A 119.6 . . ? C17 C18 C19 119.38(16) . . ? C17 C18 C20 119.72(16) . . ? C19 C18 C20 120.86(15) . . ? C14 C19 C18 119.18(16) . . ? C14 C19 S2 120.46(14) . . ? C18 C19 S2 120.34(13) . . ? O2 C20 N2 123.31(16) . . ? O2 C20 C18 121.15(16) . . ? N2 C20 C18 115.53(14) . . ? C22 C21 C26 119.20(17) . . ? C22 C21 N2 117.49(15) . . ? C26 C21 N2 123.31(16) . . ? C21 C22 C23 120.83(17) . . ? C21 C22 H22A 119.6 . . ? C23 C22 H22A 119.6 . . ? C24 C23 C22 120.08(18) . . ? C24 C23 H23A 120.0 . . ? C22 C23 H23A 120.0 . . ? C23 C24 C25 119.23(18) . . ? C23 C24 H24A 120.4 . . ? C25 C24 H24A 120.4 . . ? C26 C25 C24 121.36(18) . . ? C26 C25 H25A 119.3 . . ? C24 C25 H25A 119.3 . . ? C25 C26 C21 119.28(18) . . ? C25 C26 H26A 120.4 . . ? C21 C26 H26A 120.4 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 C3 1.0(3) . . . . ? C1 C2 C3 C4 -0.3(3) . . . . ? C2 C3 C4 C5 -0.4(3) . . . . ? C3 C4 C5 C6 0.4(3) . . . . ? C3 C4 C5 C7 -176.84(16) . . . . ? C2 C1 C6 C5 -1.1(3) . . . . ? C2 C1 C6 S1 -179.70(14) . . . . ? C4 C5 C6 C1 0.4(2) . . . . ? C7 C5 C6 C1 177.53(16) . . . . ? C4 C5 C6 S1 179.02(13) . . . . ? C7 C5 C6 S1 -3.8(2) . . . . ? C8 N1 C7 O1 -3.7(3) . . . . ? C8 N1 C7 C5 175.16(15) . . . . ? C4 C5 C7 O1 140.04(18) . . . . ? C6 C5 C7 O1 -37.1(3) . . . . ? C4 C5 C7 N1 -38.9(2) . . . . ? C6 C5 C7 N1 143.98(16) . . . . ? C7 N1 C8 C9 138.43(19) . . . . ? C7 N1 C8 C13 -44.7(3) . . . . ? C13 C8 C9 C10 -0.6(3) . . . . ? N1 C8 C9 C10 176.23(17) . . . . ? C8 C9 C10 C11 0.7(3) . . . . ? C9 C10 C11 C12 0.1(3) . . . . ? C10 C11 C12 C13 -1.0(3) . . . . ? C11 C12 C13 C8 1.1(3) . . . . ? C9 C8 C13 C12 -0.2(3) . . . . ? N1 C8 C13 C12 -177.02(17) . . . . ? C19 C14 C15 C16 -0.6(3) . . . . ? C14 C15 C16 C17 1.0(3) . . . . ? C15 C16 C17 C18 -1.0(3) . . . . ? C16 C17 C18 C19 0.8(3) . . . . ? C16 C17 C18 C20 -176.96(17) . . . . ? C15 C14 C19 C18 0.3(3) . . . . ? C15 C14 C19 S2 -178.03(14) . . . . ? C17 C18 C19 C14 -0.4(2) . . . . ? C20 C18 C19 C14 177.29(16) . . . . ? C17 C18 C19 S2 177.96(13) . . . . ? C20 C18 C19 S2 -4.3(2) . . . . ? C21 N2 C20 O2 0.5(3) . . . . ? C21 N2 C20 C18 179.76(15) . . . . ? C17 C18 C20 O2 135.98(19) . . . . ? C19 C18 C20 O2 -41.7(3) . . . . ? C17 C18 C20 N2 -43.3(2) . . . . ? C19 C18 C20 N2 138.99(17) . . . . ? C20 N2 C21 C22 154.48(18) . . . . ? C20 N2 C21 C26 -26.0(3) . . . . ? C26 C21 C22 C23 1.2(3) . . . . ? N2 C21 C22 C23 -179.28(17) . . . . ? C21 C22 C23 C24 -0.2(3) . . . . ? C22 C23 C24 C25 -1.1(3) . . . . ? C23 C24 C25 C26 1.4(3) . . . . ? C24 C25 C26 C21 -0.3(3) . . . . ? C22 C21 C26 C25 -1.0(3) . . . . ? N2 C21 C26 C25 179.54(17) . . . . ? 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 N1 H1A O2 0.88 2.16 3.036(2) 172.6 . N2 H2A O1 0.88 2.18 2.9991(19) 155.3 2_664 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.209 _refine_diff_density_min -0.185 _refine_diff_density_rms 0.041 # Attachment '5004_web_deposit_cif_file_1_FuyiWang_1302593773.cif' data_sa174 _database_code_depnum_ccdc_archive 'CCDC 821490' #TrackingRef '5004_web_deposit_cif_file_1_FuyiWang_1302593773.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C13 H9 N O S' _chemical_formula_weight 227.27 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 5.8793(12) _cell_length_b 14.397(3) _cell_length_c 12.316(3) _cell_angle_alpha 90.00 _cell_angle_beta 98.23(3) _cell_angle_gamma 90.00 _cell_volume 1031.8(4) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 3215 _cell_measurement_theta_min 3.29 _cell_measurement_theta_max 27.49 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.463 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 472 _exptl_absorpt_coefficient_mu 0.287 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8747 _exptl_absorpt_correction_T_max 0.9529 _exptl_absorpt_process_details 'CrystalClear (Rigaku Inc., 2008)' _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 'Saturn724+ CCD' _diffrn_measurement_method '\w scans at fixed \c = 45\%' _diffrn_detector_area_resol_mean 28.5714 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7080 _diffrn_reflns_av_R_equivalents 0.0313 _diffrn_reflns_av_sigmaI/netI 0.0293 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.29 _diffrn_reflns_theta_max 27.49 _reflns_number_total 2341 _reflns_number_gt 2105 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2008)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2008)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2008)' _computing_structure_solution 'SHELX-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELX-97 (Sheldrick, 1997)' _computing_molecular_graphics ; Mercury: visualization and analysis of crystal structures, C. F. Macrae, P. R. Edgington, P. McCabe, E. Pidcock, G. P. Shields, R. Taylor, M. Towler and J. van de Streek, J. Appl. Cryst., 39, 453-457, 2006. ; _computing_publication_material 'SHELX-97 (Sheldrick, 1997)' _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^)+(0.0505P)^2^+0.5327P] 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 2341 _refine_ls_number_parameters 145 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0518 _refine_ls_R_factor_gt 0.0457 _refine_ls_wR_factor_ref 0.1173 _refine_ls_wR_factor_gt 0.1097 _refine_ls_goodness_of_fit_ref 1.120 _refine_ls_restrained_S_all 1.120 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group S1 S 0.37418(8) 0.50697(3) 0.84567(4) 0.03197(17) Uani 1 1 d . . . O1 O -0.1578(2) 0.66029(10) 0.82056(11) 0.0326(3) Uani 1 1 d . . . N1 N 0.1930(3) 0.59304(11) 0.87821(13) 0.0282(4) Uani 1 1 d . . . C1 C -0.0145(3) 0.60058(12) 0.81047(15) 0.0262(4) Uani 1 1 d . . . C2 C -0.0255(3) 0.52746(13) 0.72686(15) 0.0274(4) Uani 1 1 d . . . C3 C -0.2107(4) 0.50862(14) 0.64608(16) 0.0324(4) Uani 1 1 d . . . H3 H -0.3458 0.5456 0.6398 0.039 Uiso 1 1 calc R . . C4 C -0.1950(4) 0.43554(15) 0.57540(17) 0.0373(5) Uani 1 1 d . . . H4 H -0.3205 0.4216 0.5202 0.045 Uiso 1 1 calc R . . C5 C 0.0043(4) 0.38181(15) 0.58441(17) 0.0387(5) Uani 1 1 d . . . H5 H 0.0122 0.3318 0.5348 0.046 Uiso 1 1 calc R . . C6 C 0.1903(4) 0.39947(14) 0.66347(17) 0.0351(5) Uani 1 1 d . . . H6 H 0.3258 0.3628 0.6687 0.042 Uiso 1 1 calc R . . C7 C 0.1724(3) 0.47304(13) 0.73556(16) 0.0287(4) Uani 1 1 d . . . C8 C 0.2579(3) 0.64741(12) 0.97480(14) 0.0257(4) Uani 1 1 d . . . C9 C 0.4658(3) 0.69487(13) 0.98898(15) 0.0286(4) Uani 1 1 d . . . H9 H 0.5646 0.6923 0.9344 0.034 Uiso 1 1 calc R . . C10 C 0.5268(3) 0.74598(14) 1.08382(16) 0.0323(4) Uani 1 1 d . . . H10 H 0.6700 0.7777 1.0949 0.039 Uiso 1 1 calc R . . C11 C 0.3824(3) 0.75156(14) 1.16258(16) 0.0342(4) Uani 1 1 d . . . H11 H 0.4245 0.7882 1.2265 0.041 Uiso 1 1 calc R . . C12 C 0.1754(3) 0.70350(15) 1.14823(16) 0.0340(4) Uani 1 1 d . . . H12 H 0.0761 0.7068 1.2026 0.041 Uiso 1 1 calc R . . C13 C 0.1137(3) 0.65067(14) 1.05451(16) 0.0302(4) Uani 1 1 d . . . H13 H -0.0266 0.6169 1.0450 0.036 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 S1 0.0283(3) 0.0299(3) 0.0361(3) -0.00425(19) -0.0011(2) 0.00577(18) O1 0.0286(7) 0.0327(7) 0.0350(7) -0.0028(6) -0.0005(6) 0.0058(6) N1 0.0267(8) 0.0275(8) 0.0288(8) -0.0040(6) -0.0012(6) 0.0033(6) C1 0.0266(9) 0.0244(8) 0.0269(9) 0.0021(7) 0.0017(7) -0.0011(7) C2 0.0295(9) 0.0251(9) 0.0271(9) 0.0014(7) 0.0027(8) -0.0027(7) C3 0.0332(10) 0.0329(10) 0.0298(10) 0.0015(8) 0.0002(8) -0.0028(8) C4 0.0434(12) 0.0361(11) 0.0308(10) -0.0023(8) -0.0005(9) -0.0093(9) C5 0.0537(13) 0.0294(10) 0.0339(11) -0.0062(8) 0.0089(10) -0.0085(9) C6 0.0413(11) 0.0277(10) 0.0374(11) -0.0018(8) 0.0090(9) 0.0015(8) C7 0.0308(9) 0.0246(9) 0.0303(9) 0.0015(7) 0.0031(8) -0.0026(7) C8 0.0283(9) 0.0226(8) 0.0245(8) 0.0009(7) -0.0023(7) 0.0009(7) C9 0.0268(9) 0.0290(9) 0.0299(9) 0.0005(7) 0.0043(7) 0.0004(7) C10 0.0272(9) 0.0317(10) 0.0361(10) -0.0005(8) -0.0017(8) -0.0033(8) C11 0.0361(11) 0.0365(11) 0.0275(9) -0.0044(8) -0.0035(8) 0.0026(8) C12 0.0332(10) 0.0429(11) 0.0261(9) 0.0001(8) 0.0048(8) 0.0019(9) C13 0.0266(9) 0.0332(10) 0.0304(10) 0.0022(8) 0.0027(8) -0.0033(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag S1 N1 1.7186(16) . ? S1 C7 1.739(2) . ? O1 C1 1.222(2) . ? N1 C1 1.380(2) . ? N1 C8 1.430(2) . ? C1 C2 1.467(3) . ? C2 C3 1.393(3) . ? C2 C7 1.394(3) . ? C3 C4 1.377(3) . ? C3 H3 0.9500 . ? C4 C5 1.395(3) . ? C4 H4 0.9500 . ? C5 C6 1.379(3) . ? C5 H5 0.9500 . ? C6 C7 1.396(3) . ? C6 H6 0.9500 . ? C8 C13 1.387(3) . ? C8 C9 1.390(3) . ? C9 C10 1.384(3) . ? C9 H9 0.9500 . ? C10 C11 1.380(3) . ? C10 H10 0.9500 . ? C11 C12 1.389(3) . ? C11 H11 0.9500 . ? C12 C13 1.387(3) . ? C12 H12 0.9500 . ? C13 H13 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 S1 C7 90.45(8) . . ? C1 N1 C8 124.58(15) . . ? C1 N1 S1 116.08(13) . . ? C8 N1 S1 119.23(12) . . ? O1 C1 N1 123.79(17) . . ? O1 C1 C2 127.89(17) . . ? N1 C1 C2 108.30(16) . . ? C3 C2 C7 120.27(18) . . ? C3 C2 C1 126.33(18) . . ? C7 C2 C1 113.38(16) . . ? C4 C3 C2 118.95(19) . . ? C4 C3 H3 120.5 . . ? C2 C3 H3 120.5 . . ? C3 C4 C5 120.34(19) . . ? C3 C4 H4 119.8 . . ? C5 C4 H4 119.8 . . ? C6 C5 C4 121.71(19) . . ? C6 C5 H5 119.1 . . ? C4 C5 H5 119.1 . . ? C5 C6 C7 117.69(19) . . ? C5 C6 H6 121.2 . . ? C7 C6 H6 121.2 . . ? C2 C7 C6 121.04(18) . . ? C2 C7 S1 111.76(14) . . ? C6 C7 S1 127.17(16) . . ? C13 C8 C9 120.70(17) . . ? C13 C8 N1 119.34(16) . . ? C9 C8 N1 119.95(17) . . ? C10 C9 C8 118.99(18) . . ? C10 C9 H9 120.5 . . ? C8 C9 H9 120.5 . . ? C11 C10 C9 120.88(18) . . ? C11 C10 H10 119.6 . . ? C9 C10 H10 119.6 . . ? C10 C11 C12 119.85(18) . . ? C10 C11 H11 120.1 . . ? C12 C11 H11 120.1 . . ? C13 C12 C11 119.93(18) . . ? C13 C12 H12 120.0 . . ? C11 C12 H12 120.0 . . ? C12 C13 C8 119.62(18) . . ? C12 C13 H13 120.2 . . ? C8 C13 H13 120.2 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C7 S1 N1 C1 -0.89(15) . . . . ? C7 S1 N1 C8 175.47(15) . . . . ? C8 N1 C1 O1 6.6(3) . . . . ? S1 N1 C1 O1 -177.29(15) . . . . ? C8 N1 C1 C2 -174.56(16) . . . . ? S1 N1 C1 C2 1.6(2) . . . . ? O1 C1 C2 C3 -4.3(3) . . . . ? N1 C1 C2 C3 176.85(18) . . . . ? O1 C1 C2 C7 177.15(18) . . . . ? N1 C1 C2 C7 -1.7(2) . . . . ? C7 C2 C3 C4 0.1(3) . . . . ? C1 C2 C3 C4 -178.33(19) . . . . ? C2 C3 C4 C5 -0.4(3) . . . . ? C3 C4 C5 C6 0.1(3) . . . . ? C4 C5 C6 C7 0.5(3) . . . . ? C3 C2 C7 C6 0.6(3) . . . . ? C1 C2 C7 C6 179.17(17) . . . . ? C3 C2 C7 S1 -177.54(15) . . . . ? C1 C2 C7 S1 1.1(2) . . . . ? C5 C6 C7 C2 -0.8(3) . . . . ? C5 C6 C7 S1 176.96(16) . . . . ? N1 S1 C7 C2 -0.14(15) . . . . ? N1 S1 C7 C6 -178.11(19) . . . . ? C1 N1 C8 C13 53.2(3) . . . . ? S1 N1 C8 C13 -122.83(17) . . . . ? C1 N1 C8 C9 -128.04(19) . . . . ? S1 N1 C8 C9 55.9(2) . . . . ? C13 C8 C9 C10 -0.3(3) . . . . ? N1 C8 C9 C10 -179.06(17) . . . . ? C8 C9 C10 C11 -1.2(3) . . . . ? C9 C10 C11 C12 1.6(3) . . . . ? C10 C11 C12 C13 -0.5(3) . . . . ? C11 C12 C13 C8 -1.0(3) . . . . ? C9 C8 C13 C12 1.4(3) . . . . ? N1 C8 C13 C12 -179.81(17) . . . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.284 _refine_diff_density_min -0.248 _refine_diff_density_rms 0.055 # Attachment '5005_web_deposit_cif_file_2_FuyiWang_1302593773.cif' data_mx123 _database_code_depnum_ccdc_archive 'CCDC 821491' #TrackingRef '5005_web_deposit_cif_file_2_FuyiWang_1302593773.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H34 Cl2 F6 N3 O P Ru S' _chemical_formula_weight 753.56 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.811(2) _cell_length_b 12.467(3) _cell_length_c 12.891(3) _cell_angle_alpha 100.77(3) _cell_angle_beta 109.54(3) _cell_angle_gamma 98.87(3) _cell_volume 1564.0(5) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 5484 _cell_measurement_theta_min 1.71 _cell_measurement_theta_max 27.46 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.600 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 764 _exptl_absorpt_coefficient_mu 0.851 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.8688 _exptl_absorpt_correction_T_max 0.9197 _exptl_absorpt_process_details 'CrystalClear (Rigaku Inc., 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Rotating Anode' _diffrn_radiation_monochromator Confocal _diffrn_measurement_device_type 'MM007HF + CCD (Saturn724+)' _diffrn_measurement_method '\w scans at fixed \c = 45\%' _diffrn_detector_area_resol_mean 28.5714 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19247 _diffrn_reflns_av_R_equivalents 0.0455 _diffrn_reflns_av_sigmaI/netI 0.0435 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.71 _diffrn_reflns_theta_max 27.46 _reflns_number_total 7124 _reflns_number_gt 6774 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2008)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2008)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP in Siemens SHELXTL (Sheldrick, 1994)' _computing_publication_material 'SHELX97 (Sheldrick, 1997)' _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^)+(0.0376P)^2^+1.1045P] 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 7124 _refine_ls_number_parameters 467 _refine_ls_number_restraints 830 _refine_ls_R_factor_all 0.0407 _refine_ls_R_factor_gt 0.0384 _refine_ls_wR_factor_ref 0.0958 _refine_ls_wR_factor_gt 0.0939 _refine_ls_goodness_of_fit_ref 1.084 _refine_ls_restrained_S_all 1.110 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.738167(18) 0.096626(16) 0.360599(15) 0.02594(7) Uani 1 1 d U . . Cl1 Cl 0.17377(13) -0.05463(9) 0.07420(10) 0.0757(3) Uani 1 1 d U . . Cl2 Cl 0.02243(10) -0.27199(9) 0.06636(8) 0.0651(3) Uani 1 1 d U . . S1 S 0.97820(6) 0.11358(5) 0.42739(5) 0.02804(13) Uani 1 1 d U . . P1 P 0.44745(8) -0.32336(6) 0.32870(7) 0.03690(17) Uani 1 1 d DU . . F1A F 0.5121(5) -0.3987(4) 0.4116(5) 0.0701(15) Uani 0.622(8) 1 d PDU A 1 F2A F 0.4788(4) -0.2205(4) 0.4369(5) 0.0617(16) Uani 0.622(8) 1 d PDU A 1 F3A F 0.3853(4) -0.2508(5) 0.2467(6) 0.0706(16) Uani 0.622(8) 1 d PDU A 1 F4A F 0.4165(4) -0.4273(4) 0.2238(4) 0.0499(12) Uani 0.622(8) 1 d PDU A 1 F1B F 0.4173(12) -0.3692(15) 0.1979(6) 0.064(3) Uani 0.214(6) 1 d PDU A 2 F2B F 0.4192(13) -0.2034(8) 0.3126(13) 0.045(2) Uani 0.214(6) 1 d PDU A 2 F3B F 0.4907(14) -0.2692(12) 0.4627(5) 0.058(3) Uani 0.214(6) 1 d PDU A 2 F4B F 0.4987(14) -0.4314(8) 0.3548(14) 0.062(3) Uani 0.214(6) 1 d PDU A 2 F1C F 0.4646(19) -0.3441(16) 0.4479(8) 0.080(4) Uani 0.170(5) 1 d PDU A 3 F2C F 0.4455(14) -0.1935(6) 0.3707(15) 0.045(3) Uani 0.170(5) 1 d PDU A 3 F3C F 0.4217(15) -0.2980(14) 0.2051(8) 0.058(3) Uani 0.170(5) 1 d PDU A 3 F4C F 0.4512(15) -0.4471(6) 0.2764(15) 0.051(3) Uani 0.170(5) 1 d PDU A 3 F5A F 0.3036(5) -0.3692(3) 0.3321(9) 0.0564(16) Uani 0.80(2) 1 d PDU A 1 F6A F 0.5958(4) -0.2763(7) 0.3309(7) 0.0481(13) Uani 0.80(2) 1 d PDU A 1 F5B F 0.2861(7) -0.3560(16) 0.282(3) 0.060(4) Uani 0.20(2) 1 d PDU A 2 F6B F 0.6057(9) -0.277(3) 0.362(2) 0.046(4) Uani 0.20(2) 1 d PDU A 2 O1 O 0.95896(19) 0.37856(16) 0.50695(17) 0.0371(4) Uani 1 1 d U . . N1 N 1.1789(2) 0.40204(19) 0.62180(18) 0.0338(5) Uani 1 1 d U . . H1N1 H 1.2578 0.3858 0.6236 0.041 Uiso 1 1 d R . . N2 N 0.7409(2) -0.03106(19) 0.45188(19) 0.0325(5) Uani 1 1 d U . . H1N2 H 0.6813 -0.0962 0.4096 0.039 Uiso 1 1 d R . . H2N2 H 0.8237 -0.0446 0.4671 0.039 Uiso 1 1 d R . . N3 N 0.7808(2) 0.19461(19) 0.52778(18) 0.0333(5) Uani 1 1 d U . . H1N3 H 0.8426 0.2580 0.5411 0.040 Uiso 1 1 d R . . H2N3 H 0.7059 0.2187 0.5259 0.040 Uiso 1 1 d R . . C1 C 1.0573(2) 0.2052(2) 0.3658(2) 0.0285(5) Uani 1 1 d U . . C2 C 1.1087(2) 0.3199(2) 0.4203(2) 0.0300(5) Uani 1 1 d U . . C3 C 1.1877(3) 0.3878(2) 0.3813(3) 0.0381(6) Uani 1 1 d U . . H3A H 1.2245 0.4648 0.4206 0.046 Uiso 1 1 calc R . . C4 C 1.2134(3) 0.3441(3) 0.2854(3) 0.0424(6) Uani 1 1 d U . . H4A H 1.2671 0.3910 0.2587 0.051 Uiso 1 1 calc R . . C5 C 1.1602(3) 0.2317(3) 0.2291(2) 0.0398(6) Uani 1 1 d U . . H5A H 1.1760 0.2016 0.1627 0.048 Uiso 1 1 calc R . . C6 C 1.0836(3) 0.1627(2) 0.2693(2) 0.0323(5) Uani 1 1 d U . . H6A H 1.0487 0.0855 0.2305 0.039 Uiso 1 1 calc R . . C7 C 1.0739(3) 0.3693(2) 0.5199(2) 0.0317(5) Uani 1 1 d U . . C8 C 1.1784(3) 0.4462(2) 0.7314(2) 0.0338(5) Uani 1 1 d U . . C9 C 1.0677(3) 0.4765(3) 0.7486(3) 0.0480(7) Uani 1 1 d U . . H9A H 0.9872 0.4691 0.6854 0.058 Uiso 1 1 calc R . . C10 C 1.0750(4) 0.5178(3) 0.8587(3) 0.0574(9) Uani 1 1 d U . . H10A H 0.9989 0.5388 0.8703 0.069 Uiso 1 1 calc R . . C11 C 1.1909(4) 0.5289(3) 0.9517(3) 0.0517(8) Uani 1 1 d U . . H11A H 1.1942 0.5556 1.0268 0.062 Uiso 1 1 calc R . . C12 C 1.3016(3) 0.5005(3) 0.9338(3) 0.0519(8) Uani 1 1 d U . . H12A H 1.3826 0.5093 0.9969 0.062 Uiso 1 1 calc R . . C13 C 1.2955(3) 0.4594(3) 0.8243(3) 0.0457(7) Uani 1 1 d U . . H13A H 1.3724 0.4401 0.8128 0.055 Uiso 1 1 calc R . . C14 C 0.7268(3) 0.0134(3) 0.5619(2) 0.0395(6) Uani 1 1 d U . . H14A H 0.7534 -0.0359 0.6134 0.047 Uiso 1 1 calc R . . H14B H 0.6320 0.0166 0.5487 0.047 Uiso 1 1 calc R . . C15 C 0.8175(3) 0.1289(3) 0.6136(2) 0.0390(6) Uani 1 1 d U . . H15A H 0.8050 0.1648 0.6835 0.047 Uiso 1 1 calc R . . H15B H 0.9131 0.1248 0.6340 0.047 Uiso 1 1 calc R . . C16 C 0.6245(3) 0.2122(2) 0.2829(2) 0.0337(5) Uani 1 1 d U . . C17 C 0.5306(3) 0.1161(2) 0.2797(2) 0.0351(6) Uani 1 1 d U . . H17A H 0.4739 0.1256 0.3266 0.042 Uiso 1 1 calc R . . C18 C 0.5397(3) 0.0080(2) 0.2339(2) 0.0349(6) Uani 1 1 d U . . H18A H 0.4884 -0.0571 0.2493 0.042 Uiso 1 1 calc R . . C19 C 0.6386(3) -0.0112(2) 0.1858(2) 0.0342(5) Uani 1 1 d U . . C20 C 0.7286(3) 0.0843(2) 0.1879(2) 0.0329(5) Uani 1 1 d U . . H20A H 0.8102 0.0740 0.1706 0.039 Uiso 1 1 calc R . . C21 C 0.7224(3) 0.1954(2) 0.2361(2) 0.0325(5) Uani 1 1 d U . . H21A H 0.7989 0.2599 0.2508 0.039 Uiso 1 1 calc R . . C22 C 0.6204(3) 0.3286(2) 0.3376(3) 0.0456(7) Uani 1 1 d U . . H22A H 0.5663 0.3609 0.2793 0.068 Uiso 1 1 calc R . . H22B H 0.7124 0.3758 0.3744 0.068 Uiso 1 1 calc R . . H22C H 0.5798 0.3250 0.3947 0.068 Uiso 1 1 calc R . . C23 C 0.6442(3) -0.1303(2) 0.1389(2) 0.0402(6) Uani 1 1 d DU . . H23A H 0.6100 -0.1785 0.1820 0.048 Uiso 1 1 calc R . . C24 C 0.7852(4) -0.1443(3) 0.1524(4) 0.0659(10) Uani 1 1 d DU . . H24A H 0.7825 -0.2241 0.1271 0.099 Uiso 1 1 calc R . . H24B H 0.8453 -0.1152 0.2326 0.099 Uiso 1 1 calc R . . H24C H 0.8189 -0.1027 0.1061 0.099 Uiso 1 1 calc R . . C25 C 0.5483(4) -0.1716(3) 0.0143(3) 0.0655(11) Uani 1 1 d DU . . H25A H 0.5483 -0.2500 -0.0154 0.098 Uiso 1 1 calc R . . H25B H 0.5783 -0.1251 -0.0302 0.098 Uiso 1 1 calc R . . H25C H 0.4569 -0.1663 0.0085 0.098 Uiso 1 1 calc R . . C26 C 0.1483(4) -0.2003(3) 0.0310(3) 0.0583(9) Uani 1 1 d U . . H26A H 0.1231 -0.2235 -0.0526 0.070 Uiso 1 1 calc R . . H26B H 0.2339 -0.2218 0.0671 0.070 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 0.02385(11) 0.02950(12) 0.02439(11) 0.00845(8) 0.00773(8) 0.00704(8) Cl1 0.0905(8) 0.0604(6) 0.0765(7) 0.0094(5) 0.0362(6) 0.0175(5) Cl2 0.0676(6) 0.0768(6) 0.0546(5) 0.0086(4) 0.0346(5) 0.0113(5) S1 0.0251(3) 0.0299(3) 0.0314(3) 0.0119(2) 0.0105(2) 0.0083(2) P1 0.0366(4) 0.0343(4) 0.0458(4) 0.0082(3) 0.0232(3) 0.0098(3) F1A 0.080(3) 0.071(3) 0.060(3) 0.036(2) 0.015(2) 0.021(2) F2A 0.057(2) 0.052(2) 0.069(3) -0.019(2) 0.040(2) -0.003(2) F3A 0.054(2) 0.067(3) 0.091(3) 0.046(3) 0.013(2) 0.017(2) F4A 0.048(2) 0.053(2) 0.045(2) -0.0038(17) 0.0229(17) 0.0051(17) F1B 0.061(5) 0.073(6) 0.049(4) 0.000(4) 0.016(4) 0.022(5) F2B 0.040(4) 0.047(4) 0.061(6) 0.027(4) 0.023(4) 0.021(3) F3B 0.074(5) 0.064(6) 0.047(4) 0.020(4) 0.035(4) 0.015(5) F4B 0.066(5) 0.044(4) 0.075(6) 0.020(4) 0.023(5) 0.015(4) F1C 0.094(6) 0.081(7) 0.067(5) 0.025(5) 0.036(5) 0.002(6) F2C 0.041(5) 0.043(5) 0.055(6) -0.003(5) 0.028(5) 0.011(4) F3C 0.054(5) 0.057(6) 0.055(5) 0.017(5) 0.011(4) 0.011(5) F4C 0.051(5) 0.035(4) 0.069(6) 0.014(4) 0.023(5) 0.019(4) F5A 0.0495(16) 0.0428(15) 0.085(4) 0.0046(17) 0.045(2) 0.0023(12) F6A 0.0387(15) 0.0490(16) 0.063(3) 0.011(2) 0.0296(15) 0.0109(15) F5B 0.043(4) 0.055(5) 0.078(8) 0.006(6) 0.029(4) -0.002(4) F6B 0.032(4) 0.053(5) 0.055(7) 0.011(7) 0.016(4) 0.018(4) O1 0.0288(9) 0.0350(10) 0.0434(11) 0.0045(8) 0.0109(8) 0.0085(8) N1 0.0288(11) 0.0373(12) 0.0322(11) 0.0030(9) 0.0100(9) 0.0094(9) N2 0.0282(11) 0.0365(11) 0.0358(11) 0.0162(9) 0.0117(9) 0.0085(9) N3 0.0320(11) 0.0396(12) 0.0292(10) 0.0057(9) 0.0131(9) 0.0107(9) C1 0.0251(11) 0.0314(12) 0.0295(12) 0.0102(10) 0.0085(10) 0.0094(10) C2 0.0263(12) 0.0315(12) 0.0302(12) 0.0085(10) 0.0076(10) 0.0071(10) C3 0.0367(14) 0.0309(13) 0.0465(15) 0.0100(11) 0.0164(12) 0.0047(11) C4 0.0434(16) 0.0422(15) 0.0467(16) 0.0185(13) 0.0216(13) 0.0047(12) C5 0.0397(15) 0.0465(16) 0.0366(14) 0.0116(12) 0.0178(12) 0.0103(12) C6 0.0308(13) 0.0324(13) 0.0339(13) 0.0077(10) 0.0132(10) 0.0061(10) C7 0.0332(13) 0.0246(11) 0.0367(13) 0.0082(10) 0.0122(11) 0.0063(10) C8 0.0336(13) 0.0327(13) 0.0341(13) 0.0050(10) 0.0130(11) 0.0089(11) C9 0.0404(16) 0.0568(18) 0.0410(15) -0.0002(14) 0.0106(13) 0.0207(14) C10 0.0464(17) 0.077(2) 0.0484(18) -0.0006(16) 0.0217(15) 0.0241(17) C11 0.0558(19) 0.0599(19) 0.0398(16) 0.0021(14) 0.0222(14) 0.0176(16) C12 0.0459(17) 0.066(2) 0.0378(15) 0.0038(14) 0.0109(13) 0.0200(16) C13 0.0355(15) 0.0614(19) 0.0365(14) 0.0025(13) 0.0114(12) 0.0179(14) C14 0.0350(14) 0.0572(17) 0.0371(14) 0.0244(13) 0.0183(12) 0.0161(13) C15 0.0349(14) 0.0604(17) 0.0255(12) 0.0124(12) 0.0120(11) 0.0187(13) C16 0.0312(13) 0.0371(13) 0.0301(12) 0.0136(10) 0.0034(10) 0.0126(10) C17 0.0235(12) 0.0466(15) 0.0347(13) 0.0156(11) 0.0061(10) 0.0111(11) C18 0.0275(12) 0.0390(13) 0.0298(12) 0.0122(11) 0.0013(10) 0.0013(10) C19 0.0360(13) 0.0372(13) 0.0225(11) 0.0088(10) 0.0020(10) 0.0081(11) C20 0.0356(13) 0.0407(14) 0.0213(11) 0.0111(10) 0.0069(10) 0.0109(11) C21 0.0316(13) 0.0377(13) 0.0269(12) 0.0146(10) 0.0065(10) 0.0062(10) C22 0.0495(17) 0.0399(15) 0.0495(17) 0.0133(13) 0.0165(14) 0.0188(14) C23 0.0480(16) 0.0365(14) 0.0295(13) 0.0059(11) 0.0094(12) 0.0066(12) C24 0.062(2) 0.0453(19) 0.079(3) -0.0048(18) 0.019(2) 0.0213(17) C25 0.089(3) 0.0482(19) 0.0352(17) -0.0022(14) 0.0023(17) 0.0102(19) C26 0.061(2) 0.062(2) 0.061(2) 0.0136(18) 0.0327(18) 0.0195(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 N3 2.128(2) . ? Ru1 N2 2.147(2) . ? Ru1 C20 2.169(3) . ? Ru1 C21 2.177(3) . ? Ru1 C18 2.178(3) . ? Ru1 C19 2.201(3) . ? Ru1 C16 2.202(3) . ? Ru1 C17 2.209(3) . ? Ru1 S1 2.4059(9) . ? Cl1 C26 1.747(4) . ? Cl2 C26 1.747(4) . ? S1 C1 1.777(3) . ? P1 F1C 1.560(6) . ? P1 F3A 1.568(3) . ? P1 F4C 1.576(6) . ? P1 F1B 1.578(6) . ? P1 F4B 1.584(6) . ? P1 F4A 1.591(3) . ? P1 F5A 1.591(3) . ? P1 F6B 1.599(7) . ? P1 F5B 1.600(7) . ? P1 F2A 1.608(3) . ? P1 F3B 1.608(6) . ? P1 F2B 1.609(6) . ? O1 C7 1.224(3) . ? N1 C7 1.357(3) . ? N1 C8 1.419(3) . ? N1 H1N1 0.9000 . ? N2 C14 1.489(3) . ? N2 H1N2 0.9000 . ? N2 H2N2 0.9000 . ? N3 C15 1.483(4) . ? N3 H1N3 0.9000 . ? N3 H2N3 0.9000 . ? C1 C6 1.395(3) . ? C1 C2 1.403(4) . ? C2 C3 1.386(4) . ? C2 C7 1.505(4) . ? C3 C4 1.389(4) . ? C3 H3A 0.9500 . ? C4 C5 1.383(4) . ? C4 H4A 0.9500 . ? C5 C6 1.388(4) . ? C5 H5A 0.9500 . ? C6 H6A 0.9500 . ? C8 C9 1.381(4) . ? C8 C13 1.383(4) . ? C9 C10 1.388(4) . ? C9 H9A 0.9500 . ? C10 C11 1.380(5) . ? C10 H10A 0.9500 . ? C11 C12 1.377(4) . ? C11 H11A 0.9500 . ? C12 C13 1.385(4) . ? C12 H12A 0.9500 . ? C13 H13A 0.9500 . ? C14 C15 1.499(4) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C21 1.406(4) . ? C16 C17 1.430(4) . ? C16 C22 1.505(4) . ? C17 C18 1.400(4) . ? C17 H17A 1.0000 . ? C18 C19 1.433(4) . ? C18 H18A 1.0000 . ? C19 C20 1.406(4) . ? C19 C23 1.514(4) . ? C20 C21 1.430(4) . ? C20 H20A 1.0000 . ? C21 H21A 1.0000 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 C24 1.517(4) . ? C23 C25 1.527(4) . ? C23 H23A 1.0000 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? 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 N2 78.87(9) . . ? N3 Ru1 C20 150.46(10) . . ? N2 Ru1 C20 129.60(10) . . ? N3 Ru1 C21 113.50(10) . . ? N2 Ru1 C21 167.60(10) . . ? C20 Ru1 C21 38.41(10) . . ? N3 Ru1 C18 126.56(10) . . ? N2 Ru1 C18 91.58(10) . . ? C20 Ru1 C18 67.63(11) . . ? C21 Ru1 C18 80.25(10) . . ? N3 Ru1 C19 164.76(10) . . ? N2 Ru1 C19 98.90(10) . . ? C20 Ru1 C19 37.54(10) . . ? C21 Ru1 C19 68.92(10) . . ? C18 Ru1 C19 38.20(11) . . ? N3 Ru1 C16 91.79(10) . . ? N2 Ru1 C16 146.35(10) . . ? C20 Ru1 C16 68.52(10) . . ? C21 Ru1 C16 37.45(10) . . ? C18 Ru1 C16 68.09(11) . . ? C19 Ru1 C16 81.75(10) . . ? N3 Ru1 C17 98.08(10) . . ? N2 Ru1 C17 111.03(10) . . ? C20 Ru1 C17 80.02(11) . . ? C21 Ru1 C17 67.55(10) . . ? C18 Ru1 C17 37.21(10) . . ? C19 Ru1 C17 68.44(11) . . ? C16 Ru1 C17 37.82(10) . . ? N3 Ru1 S1 84.16(7) . . ? N2 Ru1 S1 83.68(7) . . ? C20 Ru1 S1 90.85(8) . . ? C21 Ru1 S1 98.16(8) . . ? C18 Ru1 S1 147.48(8) . . ? C19 Ru1 S1 110.72(8) . . ? C16 Ru1 S1 127.86(8) . . ? C17 Ru1 S1 165.28(8) . . ? C1 S1 Ru1 111.74(9) . . ? F1C P1 F3A 142.3(8) . . ? F1C P1 F4C 93.5(7) . . ? F3A P1 F4C 119.2(6) . . ? F1C P1 F1B 150.6(9) . . ? F3A P1 F1B 62.3(5) . . ? F4C P1 F1B 57.9(7) . . ? F1C P1 F4B 62.9(8) . . ? F3A P1 F4B 153.1(5) . . ? F4C P1 F4B 34.3(7) . . ? F1B P1 F4B 90.8(6) . . ? F1C P1 F4A 119.4(7) . . ? F3A P1 F4A 91.3(3) . . ? F4C P1 F4A 27.9(6) . . ? F1B P1 F4A 31.2(6) . . ? F4B P1 F4A 62.2(6) . . ? F1C P1 F5A 70.1(8) . . ? F3A P1 F5A 90.5(4) . . ? F4C P1 F5A 89.7(5) . . ? F1B P1 F5A 100.4(6) . . ? F4B P1 F5A 93.1(6) . . ? F4A P1 F5A 89.3(3) . . ? F1C P1 F6B 93.9(13) . . ? F3A P1 F6B 102.0(13) . . ? F4C P1 F6B 92.8(14) . . ? F1B P1 F6B 94.3(11) . . ? F4B P1 F6B 80.3(14) . . ? F4A P1 F6B 100.2(12) . . ? F5A P1 F6B 163.9(9) . . ? F1C P1 F5B 94.3(16) . . ? F3A P1 F5B 68.6(13) . . ? F4C P1 F5B 91.3(8) . . ? F1B P1 F5B 80.7(13) . . ? F4B P1 F5B 107.6(11) . . ? F4A P1 F5B 79.7(7) . . ? F5A P1 F5B 24.4(11) . . ? F6B P1 F5B 170.6(14) . . ? F1C P1 F2A 59.1(7) . . ? F3A P1 F2A 90.1(3) . . ? F4C P1 F2A 150.7(6) . . ? F1B P1 F2A 150.3(6) . . ? F4B P1 F2A 116.5(5) . . ? F4A P1 F2A 178.5(3) . . ? F5A P1 F2A 90.0(3) . . ? F6B P1 F2A 80.1(12) . . ? F5B P1 F2A 100.3(8) . . ? F1C P1 F3B 32.8(7) . . ? F3A P1 F3B 116.7(5) . . ? F4C P1 F3B 123.9(8) . . ? F1B P1 F3B 174.7(7) . . ? F4B P1 F3B 90.2(5) . . ? F4A P1 F3B 151.4(5) . . ? F5A P1 F3B 84.7(6) . . ? F6B P1 F3B 80.8(11) . . ? F5B P1 F3B 103.9(12) . . ? F2A P1 F3B 27.1(4) . . ? F1C P1 F2B 115.7(8) . . ? F3A P1 F2B 31.5(4) . . ? F4C P1 F2B 150.1(7) . . ? F1B P1 F2B 92.3(5) . . ? F4B P1 F2B 171.2(6) . . ? F4A P1 F2B 122.4(5) . . ? F5A P1 F2B 94.4(5) . . ? F6B P1 F2B 91.3(14) . . ? F5B P1 F2B 81.0(10) . . ? F2A P1 F2B 59.0(5) . . ? F3B P1 F2B 85.9(5) . . ? C7 N1 C8 128.6(2) . . ? C7 N1 H1N1 117.4 . . ? C8 N1 H1N1 113.4 . . ? C14 N2 Ru1 109.91(17) . . ? C14 N2 H1N2 113.8 . . ? Ru1 N2 H1N2 112.9 . . ? C14 N2 H2N2 108.4 . . ? Ru1 N2 H2N2 104.6 . . ? H1N2 N2 H2N2 106.7 . . ? C15 N3 Ru1 111.78(17) . . ? C15 N3 H1N3 115.0 . . ? Ru1 N3 H1N3 108.1 . . ? C15 N3 H2N3 111.0 . . ? Ru1 N3 H2N3 106.5 . . ? H1N3 N3 H2N3 103.9 . . ? C6 C1 C2 118.2(2) . . ? C6 C1 S1 120.7(2) . . ? C2 C1 S1 120.69(19) . . ? C3 C2 C1 120.5(2) . . ? C3 C2 C7 120.3(2) . . ? C1 C2 C7 119.2(2) . . ? C2 C3 C4 120.6(3) . . ? C2 C3 H3A 119.7 . . ? C4 C3 H3A 119.7 . . ? C5 C4 C3 119.4(3) . . ? C5 C4 H4A 120.3 . . ? C3 C4 H4A 120.3 . . ? C4 C5 C6 120.3(3) . . ? C4 C5 H5A 119.8 . . ? C6 C5 H5A 119.8 . . ? C5 C6 C1 121.0(3) . . ? C5 C6 H6A 119.5 . . ? C1 C6 H6A 119.5 . . ? O1 C7 N1 124.1(2) . . ? O1 C7 C2 121.1(2) . . ? N1 C7 C2 114.8(2) . . ? C9 C8 C13 119.4(3) . . ? C9 C8 N1 123.2(3) . . ? C13 C8 N1 117.5(2) . . ? C8 C9 C10 119.6(3) . . ? C8 C9 H9A 120.2 . . ? C10 C9 H9A 120.2 . . ? C11 C10 C9 121.2(3) . . ? C11 C10 H10A 119.4 . . ? C9 C10 H10A 119.4 . . ? C12 C11 C10 118.9(3) . . ? C12 C11 H11A 120.5 . . ? C10 C11 H11A 120.5 . . ? C11 C12 C13 120.4(3) . . ? C11 C12 H12A 119.8 . . ? C13 C12 H12A 119.8 . . ? C8 C13 C12 120.6(3) . . ? C8 C13 H13A 119.7 . . ? C12 C13 H13A 119.7 . . ? N2 C14 C15 107.3(2) . . ? N2 C14 H14A 110.3 . . ? C15 C14 H14A 110.3 . . ? N2 C14 H14B 110.3 . . ? C15 C14 H14B 110.3 . . ? H14A C14 H14B 108.5 . . ? N3 C15 C14 107.4(2) . . ? N3 C15 H15A 110.2 . . ? C14 C15 H15A 110.2 . . ? N3 C15 H15B 110.2 . . ? C14 C15 H15B 110.2 . . ? H15A C15 H15B 108.5 . . ? C21 C16 C17 118.6(3) . . ? C21 C16 C22 120.8(3) . . ? C17 C16 C22 120.6(3) . . ? C21 C16 Ru1 70.30(15) . . ? C17 C16 Ru1 71.33(15) . . ? C22 C16 Ru1 128.92(19) . . ? C18 C17 C16 120.2(3) . . ? C18 C17 Ru1 70.18(15) . . ? C16 C17 Ru1 70.85(14) . . ? C18 C17 H17A 119.1 . . ? C16 C17 H17A 119.1 . . ? Ru1 C17 H17A 119.1 . . ? C17 C18 C19 122.2(3) . . ? C17 C18 Ru1 72.61(15) . . ? C19 C18 Ru1 71.77(15) . . ? C17 C18 H18A 118.3 . . ? C19 C18 H18A 118.3 . . ? Ru1 C18 H18A 118.3 . . ? C20 C19 C18 116.9(2) . . ? C20 C19 C23 123.5(3) . . ? C18 C19 C23 119.6(3) . . ? C20 C19 Ru1 69.99(15) . . ? C18 C19 Ru1 70.03(15) . . ? C23 C19 Ru1 129.31(18) . . ? C19 C20 C21 121.7(3) . . ? C19 C20 Ru1 72.47(15) . . ? C21 C20 Ru1 71.11(15) . . ? C19 C20 H20A 118.5 . . ? C21 C20 H20A 118.5 . . ? Ru1 C20 H20A 118.5 . . ? C16 C21 C20 120.4(2) . . ? C16 C21 Ru1 72.26(15) . . ? C20 C21 Ru1 70.47(14) . . ? C16 C21 H21A 119.2 . . ? C20 C21 H21A 119.2 . . ? Ru1 C21 H21A 119.2 . . ? C16 C22 H22A 109.5 . . ? C16 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C16 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C19 C23 C24 113.9(2) . . ? C19 C23 C25 109.2(3) . . ? C24 C23 C25 111.1(3) . . ? C19 C23 H23A 107.5 . . ? C24 C23 H23A 107.5 . . ? C25 C23 H23A 107.5 . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C23 C25 H25A 109.5 . . ? C23 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C23 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? Cl2 C26 Cl1 112.6(2) . . ? Cl2 C26 H26A 109.1 . . ? Cl1 C26 H26A 109.1 . . ? Cl2 C26 H26B 109.1 . . ? Cl1 C26 H26B 109.1 . . ? H26A C26 H26B 107.8 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N3 Ru1 S1 C1 -108.00(11) . . . . ? N2 Ru1 S1 C1 172.60(11) . . . . ? C20 Ru1 S1 C1 42.83(12) . . . . ? C21 Ru1 S1 C1 4.97(12) . . . . ? C18 Ru1 S1 C1 89.61(16) . . . . ? C19 Ru1 S1 C1 75.45(12) . . . . ? C16 Ru1 S1 C1 -20.28(13) . . . . ? C17 Ru1 S1 C1 -8.4(3) . . . . ? N3 Ru1 N2 C14 17.50(17) . . . . ? C20 Ru1 N2 C14 -171.38(16) . . . . ? C21 Ru1 N2 C14 -157.9(4) . . . . ? C18 Ru1 N2 C14 -109.50(18) . . . . ? C19 Ru1 N2 C14 -147.18(18) . . . . ? C16 Ru1 N2 C14 -58.7(3) . . . . ? C17 Ru1 N2 C14 -76.96(19) . . . . ? S1 Ru1 N2 C14 102.76(17) . . . . ? N2 Ru1 N3 C15 12.38(17) . . . . ? C20 Ru1 N3 C15 -153.7(2) . . . . ? C21 Ru1 N3 C15 -168.69(17) . . . . ? C18 Ru1 N3 C15 96.01(19) . . . . ? C19 Ru1 N3 C15 95.4(4) . . . . ? C16 Ru1 N3 C15 159.80(18) . . . . ? C17 Ru1 N3 C15 122.35(18) . . . . ? S1 Ru1 N3 C15 -72.31(17) . . . . ? Ru1 S1 C1 C6 -95.5(2) . . . . ? Ru1 S1 C1 C2 92.0(2) . . . . ? C6 C1 C2 C3 -2.4(4) . . . . ? S1 C1 C2 C3 170.3(2) . . . . ? C6 C1 C2 C7 175.9(2) . . . . ? S1 C1 C2 C7 -11.3(3) . . . . ? C1 C2 C3 C4 2.2(4) . . . . ? C7 C2 C3 C4 -176.1(3) . . . . ? C2 C3 C4 C5 -0.4(5) . . . . ? C3 C4 C5 C6 -1.1(5) . . . . ? C4 C5 C6 C1 0.9(4) . . . . ? C2 C1 C6 C5 0.9(4) . . . . ? S1 C1 C6 C5 -171.9(2) . . . . ? C8 N1 C7 O1 3.7(4) . . . . ? C8 N1 C7 C2 -176.7(2) . . . . ? C3 C2 C7 O1 109.3(3) . . . . ? C1 C2 C7 O1 -69.1(3) . . . . ? C3 C2 C7 N1 -70.3(3) . . . . ? C1 C2 C7 N1 111.3(3) . . . . ? C7 N1 C8 C9 -8.8(5) . . . . ? C7 N1 C8 C13 171.6(3) . . . . ? C13 C8 C9 C10 -1.1(5) . . . . ? N1 C8 C9 C10 179.2(3) . . . . ? C8 C9 C10 C11 -0.2(6) . . . . ? C9 C10 C11 C12 1.5(6) . . . . ? C10 C11 C12 C13 -1.4(6) . . . . ? C9 C8 C13 C12 1.2(5) . . . . ? N1 C8 C13 C12 -179.1(3) . . . . ? C11 C12 C13 C8 0.0(6) . . . . ? Ru1 N2 C14 C15 -44.0(2) . . . . ? Ru1 N3 C15 C14 -39.7(2) . . . . ? N2 C14 C15 N3 54.5(3) . . . . ? N3 Ru1 C16 C21 127.97(16) . . . . ? N2 Ru1 C16 C21 -159.59(17) . . . . ? C20 Ru1 C16 C21 -29.41(16) . . . . ? C18 Ru1 C16 C21 -102.99(18) . . . . ? C19 Ru1 C16 C21 -65.89(17) . . . . ? C17 Ru1 C16 C21 -131.1(2) . . . . ? S1 Ru1 C16 C21 43.99(18) . . . . ? N3 Ru1 C16 C17 -100.90(17) . . . . ? N2 Ru1 C16 C17 -28.5(3) . . . . ? C20 Ru1 C16 C17 101.72(18) . . . . ? C21 Ru1 C16 C17 131.1(2) . . . . ? C18 Ru1 C16 C17 28.13(16) . . . . ? C19 Ru1 C16 C17 65.23(17) . . . . ? S1 Ru1 C16 C17 175.11(13) . . . . ? N3 Ru1 C16 C22 13.8(3) . . . . ? N2 Ru1 C16 C22 86.3(3) . . . . ? C20 Ru1 C16 C22 -143.5(3) . . . . ? C21 Ru1 C16 C22 -114.1(3) . . . . ? C18 Ru1 C16 C22 142.9(3) . . . . ? C19 Ru1 C16 C22 180.0(3) . . . . ? C17 Ru1 C16 C22 114.7(3) . . . . ? S1 Ru1 C16 C22 -70.1(3) . . . . ? C21 C16 C17 C18 2.0(4) . . . . ? C22 C16 C17 C18 -176.7(2) . . . . ? Ru1 C16 C17 C18 -51.9(2) . . . . ? C21 C16 C17 Ru1 53.9(2) . . . . ? C22 C16 C17 Ru1 -124.8(2) . . . . ? N3 Ru1 C17 C18 -143.89(16) . . . . ? N2 Ru1 C17 C18 -62.77(18) . . . . ? C20 Ru1 C17 C18 65.97(17) . . . . ? C21 Ru1 C17 C18 103.96(18) . . . . ? C19 Ru1 C17 C18 28.74(16) . . . . ? C16 Ru1 C17 C18 133.7(2) . . . . ? S1 Ru1 C17 C18 118.3(3) . . . . ? N3 Ru1 C17 C16 82.45(17) . . . . ? N2 Ru1 C17 C16 163.57(15) . . . . ? C20 Ru1 C17 C16 -67.69(17) . . . . ? C21 Ru1 C17 C16 -29.71(16) . . . . ? C18 Ru1 C17 C16 -133.7(2) . . . . ? C19 Ru1 C17 C16 -104.93(18) . . . . ? S1 Ru1 C17 C16 -15.3(4) . . . . ? C16 C17 C18 C19 -2.0(4) . . . . ? Ru1 C17 C18 C19 -54.2(2) . . . . ? C16 C17 C18 Ru1 52.2(2) . . . . ? N3 Ru1 C18 C17 46.6(2) . . . . ? N2 Ru1 C18 C17 123.87(17) . . . . ? C20 Ru1 C18 C17 -103.42(18) . . . . ? C21 Ru1 C18 C17 -65.51(17) . . . . ? C19 Ru1 C18 C17 -133.7(2) . . . . ? C16 Ru1 C18 C17 -28.56(16) . . . . ? S1 Ru1 C18 C17 -155.42(13) . . . . ? N3 Ru1 C18 C19 -179.72(14) . . . . ? N2 Ru1 C18 C19 -102.44(16) . . . . ? C20 Ru1 C18 C19 30.27(15) . . . . ? C21 Ru1 C18 C19 68.18(16) . . . . ? C16 Ru1 C18 C19 105.13(17) . . . . ? C17 Ru1 C18 C19 133.7(2) . . . . ? S1 Ru1 C18 C19 -21.7(2) . . . . ? C17 C18 C19 C20 0.9(4) . . . . ? Ru1 C18 C19 C20 -53.7(2) . . . . ? C17 C18 C19 C23 179.3(2) . . . . ? Ru1 C18 C19 C23 124.7(2) . . . . ? C17 C18 C19 Ru1 54.6(2) . . . . ? N3 Ru1 C19 C20 130.9(3) . . . . ? N2 Ru1 C19 C20 -148.78(15) . . . . ? C21 Ru1 C19 C20 28.76(16) . . . . ? C18 Ru1 C19 C20 130.1(2) . . . . ? C16 Ru1 C19 C20 65.26(16) . . . . ? C17 Ru1 C19 C20 102.04(17) . . . . ? S1 Ru1 C19 C20 -62.21(16) . . . . ? N3 Ru1 C19 C18 0.8(4) . . . . ? N2 Ru1 C19 C18 81.14(16) . . . . ? C20 Ru1 C19 C18 -130.1(2) . . . . ? C21 Ru1 C19 C18 -101.32(17) . . . . ? C16 Ru1 C19 C18 -64.82(16) . . . . ? C17 Ru1 C19 C18 -28.05(15) . . . . ? S1 Ru1 C19 C18 167.71(13) . . . . ? N3 Ru1 C19 C23 -111.6(4) . . . . ? N2 Ru1 C19 C23 -31.3(3) . . . . ? C20 Ru1 C19 C23 117.5(3) . . . . ? C21 Ru1 C19 C23 146.3(3) . . . . ? C18 Ru1 C19 C23 -112.4(3) . . . . ? C16 Ru1 C19 C23 -177.2(3) . . . . ? C17 Ru1 C19 C23 -140.5(3) . . . . ? S1 Ru1 C19 C23 55.3(3) . . . . ? C18 C19 C20 C21 0.2(4) . . . . ? C23 C19 C20 C21 -178.1(2) . . . . ? Ru1 C19 C20 C21 -53.5(2) . . . . ? C18 C19 C20 Ru1 53.7(2) . . . . ? C23 C19 C20 Ru1 -124.6(2) . . . . ? N3 Ru1 C20 C19 -156.24(18) . . . . ? N2 Ru1 C20 C19 41.7(2) . . . . ? C21 Ru1 C20 C19 -133.7(2) . . . . ? C18 Ru1 C20 C19 -30.77(16) . . . . ? C16 Ru1 C20 C19 -105.01(18) . . . . ? C17 Ru1 C20 C19 -67.45(17) . . . . ? S1 Ru1 C20 C19 124.16(15) . . . . ? N3 Ru1 C20 C21 -22.5(3) . . . . ? N2 Ru1 C20 C21 175.39(14) . . . . ? C18 Ru1 C20 C21 102.96(18) . . . . ? C19 Ru1 C20 C21 133.7(2) . . . . ? C16 Ru1 C20 C21 28.72(15) . . . . ? C17 Ru1 C20 C21 66.28(17) . . . . ? S1 Ru1 C20 C21 -102.11(15) . . . . ? C17 C16 C21 C20 -0.9(4) . . . . ? C22 C16 C21 C20 177.8(2) . . . . ? Ru1 C16 C21 C20 53.5(2) . . . . ? C17 C16 C21 Ru1 -54.4(2) . . . . ? C22 C16 C21 Ru1 124.3(2) . . . . ? C19 C20 C21 C16 -0.2(4) . . . . ? Ru1 C20 C21 C16 -54.3(2) . . . . ? C19 C20 C21 Ru1 54.1(2) . . . . ? N3 Ru1 C21 C16 -59.22(18) . . . . ? N2 Ru1 C21 C16 115.9(4) . . . . ? C20 Ru1 C21 C16 132.7(2) . . . . ? C18 Ru1 C21 C16 66.53(17) . . . . ? C19 Ru1 C21 C16 104.50(18) . . . . ? C17 Ru1 C21 C16 29.99(16) . . . . ? S1 Ru1 C21 C16 -146.37(15) . . . . ? N3 Ru1 C21 C20 168.12(15) . . . . ? N2 Ru1 C21 C20 -16.8(5) . . . . ? C18 Ru1 C21 C20 -66.12(17) . . . . ? C19 Ru1 C21 C20 -28.15(16) . . . . ? C16 Ru1 C21 C20 -132.7(2) . . . . ? C17 Ru1 C21 C20 -102.67(18) . . . . ? S1 Ru1 C21 C20 80.98(15) . . . . ? C20 C19 C23 C24 30.8(4) . . . . ? C18 C19 C23 C24 -147.4(3) . . . . ? Ru1 C19 C23 C24 -59.9(4) . . . . ? C20 C19 C23 C25 -94.0(3) . . . . ? C18 C19 C23 C25 87.8(3) . . . . ? Ru1 C19 C23 C25 175.3(2) . . . . ? 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 N1 H1N1 F6B 0.90 2.14 2.96(3) 152.7 2_756 N1 H1N1 F6A 0.90 2.25 3.050(8) 148.1 2_756 N1 H1N1 F4B 0.90 2.51 3.352(14) 155.0 2_756 N1 H1N1 F1A 0.90 2.66 3.513(6) 158.3 2_756 N2 H1N2 F6B 0.90 2.17 3.01(3) 154.4 . N2 H1N2 F6A 0.90 2.19 3.056(8) 160.8 . N2 H1N2 F2C 0.90 2.49 3.220(13) 138.9 . N2 H2N2 S1 0.90 2.50 3.332(2) 154.6 2_756 N3 H1N3 O1 0.90 2.02 2.873(3) 158.3 . N3 H2N3 F2A 0.90 2.21 3.044(5) 154.5 2_656 N3 H2N3 F3B 0.90 2.35 3.246(14) 173.0 2_656 N3 H2N3 F2C 0.90 2.45 3.137(13) 133.0 2_656 N3 H2N3 F5A 0.90 2.41 3.013(4) 125.0 2_656 _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.681 _refine_diff_density_min -0.688 _refine_diff_density_rms 0.076 # Attachment '5006_web_deposit_cif_file_3_FuyiWang_1302593773.cif' data_sx2609 _database_code_depnum_ccdc_archive 'CCDC 821492' #TrackingRef '5006_web_deposit_cif_file_3_FuyiWang_1302593773.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C62 H70 F6 N3 O6 P Ru2 S3' _chemical_formula_weight 1396.50 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.0581(3) _cell_length_b 15.6374(4) _cell_length_c 17.9756(5) _cell_angle_alpha 84.0760(10) _cell_angle_beta 80.4740(10) _cell_angle_gamma 88.8860(10) _cell_volume 3049.10(14) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 25422 _cell_measurement_theta_min 2.03 _cell_measurement_theta_max 27.46 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.53 _exptl_crystal_size_mid 0.46 _exptl_crystal_size_min 0.36 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.521 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1432 _exptl_absorpt_coefficient_mu 0.696 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7094 _exptl_absorpt_correction_T_max 0.7878 _exptl_absorpt_process_details 'ABSCOR by T.Higashi 8 March, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku raxis Rapid IP Area Detector' _diffrn_measurement_method '\w scans at fixed \c = 45\%' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25422 _diffrn_reflns_av_R_equivalents 0.0277 _diffrn_reflns_av_sigmaI/netI 0.0360 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.03 _diffrn_reflns_theta_max 27.46 _reflns_number_total 13920 _reflns_number_gt 13153 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Rapid Auto(Rigaku 2001)' _computing_cell_refinement 'Rapid Auto(Rigaku 2001)' _computing_data_reduction 'Rapid Auto(Rigaku 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP in Siemens SHELXTL (Sheldrick, 1994)' _computing_publication_material 'SHELX97 (Sheldrick, 1997)' _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^)+(0.0255P)^2^+3.7576P] 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 13920 _refine_ls_number_parameters 849 _refine_ls_number_restraints 218 _refine_ls_R_factor_all 0.0547 _refine_ls_R_factor_gt 0.0478 _refine_ls_wR_factor_ref 0.0922 _refine_ls_wR_factor_gt 0.0900 _refine_ls_goodness_of_fit_ref 1.289 _refine_ls_restrained_S_all 1.309 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 1.053906(19) 0.333907(14) -0.191694(12) 0.01486(6) Uani 1 1 d . . . Ru2 Ru 1.353848(19) 0.313068(14) -0.259161(12) 0.01524(6) Uani 1 1 d . . . S1 S 1.17222(6) 0.24197(4) -0.27603(4) 0.01681(13) Uani 1 1 d . . . S2 S 1.23145(6) 0.29972(5) -0.13407(4) 0.01748(13) Uani 1 1 d . . . S3 S 1.20594(6) 0.42696(4) -0.26866(4) 0.01517(13) Uani 1 1 d . . . P1 P 0.98646(8) 0.30271(6) 0.17762(5) 0.03219(19) Uani 1 1 d D . . F1 F 1.1150(7) 0.3457(7) 0.1796(7) 0.068(3) Uani 0.515(16) 1 d PDU A 1 F2 F 1.0086(15) 0.2298(5) 0.2397(4) 0.087(3) Uani 0.515(16) 1 d PDU A 1 F3 F 0.9692(10) 0.3751(5) 0.1119(5) 0.067(2) Uani 0.515(16) 1 d PDU A 1 F4 F 0.8624(7) 0.2614(7) 0.1680(8) 0.074(3) Uani 0.515(16) 1 d PDU A 1 F1' F 1.1018(9) 0.3233(9) 0.2116(8) 0.082(3) Uani 0.485(16) 1 d PDU A 2 F2' F 0.9354(14) 0.2356(5) 0.2468(4) 0.076(3) Uani 0.485(16) 1 d PDU A 2 F3' F 1.0239(13) 0.3699(6) 0.1064(5) 0.079(3) Uani 0.485(16) 1 d PDU A 2 F4' F 0.8666(7) 0.2822(8) 0.1436(5) 0.048(2) Uani 0.485(16) 1 d PDU A 2 F5 F 0.9150(3) 0.37100(19) 0.22831(19) 0.0739(9) Uani 1 1 d . A . F6 F 1.0556(2) 0.23688(19) 0.12242(17) 0.0644(8) Uani 1 1 d . A . O1 O 0.8787(2) 0.14041(17) -0.29046(14) 0.0358(6) Uani 1 1 d . . . O2 O 1.4811(3) 0.2487(2) -0.03873(18) 0.0619(10) Uani 1 1 d . . . O3 O 1.4558(3) 0.5788(2) -0.44978(15) 0.0486(7) Uani 1 1 d . . . O4 O 1.2444(2) 0.02171(17) -0.43970(17) 0.0414(6) Uani 1 1 d . . . H1O4 H 1.2788 0.0417 -0.4830 0.050 Uiso 1 1 d R . . O5 O 1.3291(3) 0.0649(2) -0.58847(18) 0.0583(8) Uani 1 1 d . . . H1O5 H 1.4051 0.0580 -0.6004 0.070 Uiso 1 1 d R . . O6 O 1.4280(3) -0.0520(2) -0.3616(2) 0.0684(10) Uani 1 1 d . . . H1O6 H 1.3639 -0.0383 -0.3793 0.082 Uiso 1 1 d R . . N1 N 1.0365(2) 0.13890(17) -0.38903(15) 0.0270(6) Uani 1 1 d . . . H1 H 1.1104 0.1173 -0.4013 0.032 Uiso 1 1 calc R . . N2 N 1.3125(3) 0.21746(19) 0.04831(17) 0.0335(6) Uani 1 1 d D . . H2 H 1.2427 0.2375 0.0712 0.040 Uiso 1 1 calc R B 1 N3 N 1.3533(2) 0.58732(17) -0.33148(15) 0.0240(5) Uani 1 1 d . . . H3 H 1.2806 0.5789 -0.3034 0.029 Uiso 1 1 calc R . . C1 C 0.9124(3) 0.2796(2) -0.09465(16) 0.0219(6) Uani 1 1 d . . . C2 C 0.8810(2) 0.2598(2) -0.16396(16) 0.0213(6) Uani 1 1 d . . . H2A H 0.8815 0.1984 -0.1749 0.026 Uiso 1 1 calc R . . C3 C 0.8693(2) 0.3257(2) -0.22303(17) 0.0225(6) Uani 1 1 d . . . H3A H 0.8622 0.3091 -0.2744 0.027 Uiso 1 1 calc R . . C4 C 0.8907(3) 0.4126(2) -0.21483(18) 0.0242(6) Uani 1 1 d . . . C5 C 0.9256(3) 0.4334(2) -0.14631(18) 0.0252(6) Uani 1 1 d . . . H5A H 0.9570 0.4923 -0.1434 0.030 Uiso 1 1 calc R . . C6 C 0.9378(3) 0.3676(2) -0.08782(17) 0.0236(6) Uani 1 1 d . . . H6A H 0.9777 0.3814 -0.0445 0.028 Uiso 1 1 calc R . . C7 C 0.9127(3) 0.2131(2) -0.02745(18) 0.0293(7) Uani 1 1 d . . . H7A H 0.9564 0.2383 0.0096 0.035 Uiso 1 1 calc R . . C8 C 0.7786(3) 0.1989(3) 0.0100(2) 0.0448(10) Uani 1 1 d . . . H8A H 0.7393 0.2546 0.0183 0.067 Uiso 1 1 calc R . . H8B H 0.7755 0.1639 0.0587 0.067 Uiso 1 1 calc R . . H8C H 0.7354 0.1692 -0.0232 0.067 Uiso 1 1 calc R . . C9 C 0.9765(5) 0.1294(3) -0.0463(2) 0.0572(13) Uani 1 1 d . . . H9A H 1.0612 0.1413 -0.0709 0.086 Uiso 1 1 calc R . . H9B H 0.9330 0.1018 -0.0806 0.086 Uiso 1 1 calc R . . H9C H 0.9764 0.0911 0.0004 0.086 Uiso 1 1 calc R . . C10 C 0.8758(3) 0.4829(2) -0.2764(2) 0.0363(8) Uani 1 1 d . . . H10A H 0.8044 0.5183 -0.2595 0.054 Uiso 1 1 calc R . . H10B H 0.8636 0.4573 -0.3222 0.054 Uiso 1 1 calc R . . H10C H 0.9495 0.5188 -0.2878 0.054 Uiso 1 1 calc R . . C11 C 1.4736(3) 0.25091(19) -0.34940(18) 0.0230(6) Uani 1 1 d . . . C12 C 1.4978(3) 0.2138(2) -0.27640(19) 0.0263(6) Uani 1 1 d . . . H12A H 1.4759 0.1522 -0.2597 0.032 Uiso 1 1 calc R . . C13 C 1.5252(3) 0.2660(2) -0.22293(18) 0.0247(6) Uani 1 1 d . . . H13A H 1.5226 0.2403 -0.1694 0.030 Uiso 1 1 calc R . . C14 C 1.5346(2) 0.3579(2) -0.23910(17) 0.0227(6) Uani 1 1 d . . . C15 C 1.5144(2) 0.39253(19) -0.31132(17) 0.0209(6) Uani 1 1 d . . . H15A H 1.5024 0.4561 -0.3201 0.025 Uiso 1 1 calc R . . C16 C 1.4845(3) 0.34052(19) -0.36648(16) 0.0211(6) Uani 1 1 d . . . H16A H 1.4539 0.3687 -0.4123 0.025 Uiso 1 1 calc R . . C17 C 1.4362(3) 0.1919(2) -0.40384(19) 0.0287(7) Uani 1 1 d . . . H17A H 1.3798 0.1474 -0.3733 0.034 Uiso 1 1 calc R . . C18 C 1.3686(4) 0.2378(2) -0.4634(2) 0.0382(8) Uani 1 1 d . . . H18A H 1.2951 0.2657 -0.4383 0.057 Uiso 1 1 calc R . . H18B H 1.3449 0.1961 -0.4954 0.057 Uiso 1 1 calc R . . H18C H 1.4223 0.2813 -0.4948 0.057 Uiso 1 1 calc R . . C19 C 1.5502(4) 0.1453(3) -0.4408(3) 0.0517(11) Uani 1 1 d . . . H19A H 1.5253 0.1013 -0.4703 0.078 Uiso 1 1 calc R . . H19B H 1.5938 0.1181 -0.4014 0.078 Uiso 1 1 calc R . . H19C H 1.6043 0.1868 -0.4745 0.078 Uiso 1 1 calc R . . C20 C 1.5608(3) 0.4142(2) -0.18113(19) 0.0297(7) Uani 1 1 d . . . H20A H 1.6496 0.4217 -0.1857 0.045 Uiso 1 1 calc R . . H20B H 1.5281 0.3874 -0.1302 0.045 Uiso 1 1 calc R . . H20C H 1.5219 0.4705 -0.1895 0.045 Uiso 1 1 calc R . . C21 C 1.1590(3) 0.13111(19) -0.23969(17) 0.0215(6) Uani 1 1 d . . . C22 C 1.0694(3) 0.08288(19) -0.26410(17) 0.0241(6) Uani 1 1 d . . . C23 C 1.0540(3) -0.0033(2) -0.2365(2) 0.0346(8) Uani 1 1 d . . . H23A H 0.9929 -0.0360 -0.2520 0.041 Uiso 1 1 calc R . . C24 C 1.1261(4) -0.0419(2) -0.1868(2) 0.0418(9) Uani 1 1 d . . . H24A H 1.1148 -0.1009 -0.1686 0.050 Uiso 1 1 calc R . . C25 C 1.2151(4) 0.0057(2) -0.1635(2) 0.0382(8) Uani 1 1 d . . . H25A H 1.2647 -0.0208 -0.1293 0.046 Uiso 1 1 calc R . . C26 C 1.2317(3) 0.0919(2) -0.19003(19) 0.0274(7) Uani 1 1 d . . . H26A H 1.2931 0.1241 -0.1742 0.033 Uiso 1 1 calc R . . C27 C 0.9849(3) 0.12415(19) -0.31538(18) 0.0250(6) Uani 1 1 d . . . C28 C 0.9862(3) 0.1851(2) -0.44922(18) 0.0272(7) Uani 1 1 d . . . C29 C 0.8731(3) 0.2271(2) -0.4391(2) 0.0305(7) Uani 1 1 d . . . H29A H 0.8236 0.2245 -0.3904 0.037 Uiso 1 1 calc R . . C30 C 0.8338(3) 0.2728(2) -0.5014(2) 0.0366(8) Uani 1 1 d . . . H30A H 0.7573 0.3022 -0.4945 0.044 Uiso 1 1 calc R . . C31 C 0.9029(4) 0.2765(3) -0.5728(2) 0.0417(9) Uani 1 1 d . . . H31A H 0.8744 0.3076 -0.6148 0.050 Uiso 1 1 calc R . . C32 C 1.0147(4) 0.2343(3) -0.5824(2) 0.0388(8) Uani 1 1 d . . . H32A H 1.0629 0.2360 -0.6315 0.047 Uiso 1 1 calc R . . C33 C 1.0570(3) 0.1894(2) -0.5210(2) 0.0330(7) Uani 1 1 d . . . H33A H 1.1346 0.1617 -0.5281 0.040 Uiso 1 1 calc R . . C34 C 1.2650(2) 0.38201(19) -0.07843(15) 0.0189(5) Uani 1 1 d . C . C35 C 1.3315(3) 0.3588(2) -0.01917(16) 0.0242(6) Uani 1 1 d . . . C36 C 1.3586(3) 0.4215(3) 0.02521(19) 0.0343(8) Uani 1 1 d . C . H36A H 1.4025 0.4059 0.0658 0.041 Uiso 1 1 calc R . . C37 C 1.3230(3) 0.5056(2) 0.01144(19) 0.0339(8) Uani 1 1 d . . . H37A H 1.3440 0.5478 0.0416 0.041 Uiso 1 1 calc R C . C38 C 1.2567(3) 0.5286(2) -0.04639(18) 0.0285(7) Uani 1 1 d . C . H38A H 1.2317 0.5867 -0.0559 0.034 Uiso 1 1 calc R . . C39 C 1.2266(3) 0.4672(2) -0.09058(16) 0.0229(6) Uani 1 1 d . . . H39A H 1.1794 0.4831 -0.1295 0.028 Uiso 1 1 calc R C . C40 C 1.3819(3) 0.2693(2) -0.00510(18) 0.0295(7) Uani 1 1 d . C . C41 C 1.3468(7) 0.1301(4) 0.0702(7) 0.032(3) Uani 0.561(9) 1 d PDU C 1 C42 C 1.2592(8) 0.0845(5) 0.1229(5) 0.041(2) Uani 0.561(9) 1 d PDU C 1 H42A H 1.1838 0.1116 0.1407 0.049 Uiso 0.561(9) 1 calc PR C 1 C43 C 1.2797(9) 0.0003(5) 0.1499(5) 0.048(3) Uani 0.561(9) 1 d PDU C 1 H43A H 1.2194 -0.0293 0.1868 0.057 Uiso 0.561(9) 1 calc PR C 1 C44 C 1.3880(8) -0.0409(5) 0.1234(6) 0.057(3) Uani 0.561(9) 1 d PDU C 1 H44A H 1.4010 -0.0995 0.1401 0.069 Uiso 0.561(9) 1 calc PR C 1 C45 C 1.4764(7) 0.0047(5) 0.0723(7) 0.076(3) Uani 0.561(9) 1 d PDU C 1 H45A H 1.5517 -0.0225 0.0547 0.091 Uiso 0.561(9) 1 calc PR C 1 C46 C 1.4571(7) 0.0899(5) 0.0461(6) 0.061(2) Uani 0.561(9) 1 d PDU C 1 H46A H 1.5197 0.1206 0.0117 0.073 Uiso 0.561(9) 1 calc PR C 1 C41' C 1.3275(9) 0.1342(6) 0.0845(10) 0.030(3) Uani 0.439(9) 1 d PDU C 2 C42' C 1.2310(8) 0.0779(7) 0.1026(7) 0.037(2) Uani 0.439(9) 1 d PDU C 2 H42B H 1.1520 0.0957 0.0929 0.044 Uiso 0.439(9) 1 calc PR C 2 C43' C 1.2483(10) -0.0046(7) 0.1348(9) 0.047(3) Uani 0.439(9) 1 d PDU C 2 H43B H 1.1828 -0.0448 0.1441 0.057 Uiso 0.439(9) 1 calc PR C 2 C44' C 1.3616(10) -0.0282(6) 0.1533(7) 0.045(3) Uani 0.439(9) 1 d PDU C 2 H44B H 1.3727 -0.0826 0.1801 0.054 Uiso 0.439(9) 1 calc PR C 2 C45' C 1.4580(9) 0.0282(7) 0.1323(9) 0.071(3) Uani 0.439(9) 1 d PDU C 2 H45B H 1.5375 0.0102 0.1409 0.085 Uiso 0.439(9) 1 calc PR C 2 C46' C 1.4423(8) 0.1110(6) 0.0987(8) 0.055(3) Uani 0.439(9) 1 d PDU C 2 H46B H 1.5089 0.1501 0.0860 0.066 Uiso 0.439(9) 1 calc PR C 2 C47 C 1.1899(3) 0.44527(18) -0.36699(15) 0.0179(5) Uani 1 1 d . . . C48 C 1.2691(3) 0.50220(19) -0.41828(16) 0.0211(6) Uani 1 1 d . . . C49 C 1.2615(3) 0.5053(2) -0.49544(17) 0.0276(7) Uani 1 1 d . . . H49A H 1.3165 0.5413 -0.5308 0.033 Uiso 1 1 calc R . . C50 C 1.1771(3) 0.4582(2) -0.52172(18) 0.0307(7) Uani 1 1 d . . . H50A H 1.1749 0.4610 -0.5745 0.037 Uiso 1 1 calc R . . C51 C 1.0950(3) 0.4064(2) -0.47073(18) 0.0272(7) Uani 1 1 d . . . H51A H 1.0335 0.3757 -0.4881 0.033 Uiso 1 1 calc R . . C52 C 1.1029(3) 0.39952(19) -0.39444(17) 0.0220(6) Uani 1 1 d . . . H52A H 1.0478 0.3627 -0.3599 0.026 Uiso 1 1 calc R . . C53 C 1.3678(3) 0.5590(2) -0.40092(17) 0.0245(6) Uani 1 1 d . . . C54 C 1.4405(3) 0.62885(19) -0.29843(18) 0.0238(6) Uani 1 1 d . . . C55 C 1.4017(3) 0.6548(2) -0.2268(2) 0.0324(7) Uani 1 1 d . . . H55A H 1.3186 0.6465 -0.2035 0.039 Uiso 1 1 calc R . . C56 C 1.4828(4) 0.6926(3) -0.1889(2) 0.0436(9) Uani 1 1 d . . . H56A H 1.4551 0.7103 -0.1399 0.052 Uiso 1 1 calc R . . C57 C 1.6040(4) 0.7045(3) -0.2225(2) 0.0455(10) Uani 1 1 d . . . H57A H 1.6600 0.7303 -0.1967 0.055 Uiso 1 1 calc R . . C58 C 1.6428(3) 0.6788(3) -0.2934(2) 0.0420(9) Uani 1 1 d . . . H58A H 1.7263 0.6867 -0.3160 0.050 Uiso 1 1 calc R . . C59 C 1.5635(3) 0.6415(2) -0.3331(2) 0.0317(7) Uani 1 1 d . . . H59A H 1.5916 0.6249 -0.3824 0.038 Uiso 1 1 calc R . . C60 C 1.1601(4) -0.0464(3) -0.4395(3) 0.0608(13) Uani 1 1 d . . . H60A H 1.1339 -0.0721 -0.3874 0.091 Uiso 1 1 calc R . . H60B H 1.2001 -0.0903 -0.4704 0.091 Uiso 1 1 calc R . . H60C H 1.0884 -0.0235 -0.4607 0.091 Uiso 1 1 calc R . . C61 C 1.2658(6) 0.0493(4) -0.6485(3) 0.0836(19) Uani 1 1 d . . . H61A H 1.1773 0.0487 -0.6302 0.125 Uiso 1 1 calc R . . H61B H 1.2914 -0.0064 -0.6665 0.125 Uiso 1 1 calc R . . H61C H 1.2853 0.0949 -0.6903 0.125 Uiso 1 1 calc R . . C62 C 1.3857(6) -0.1336(4) -0.3235(4) 0.098(2) Uani 1 1 d . . . H62A H 1.3876 -0.1754 -0.3608 0.147 Uiso 1 1 calc R . . H62B H 1.3016 -0.1277 -0.2970 0.147 Uiso 1 1 calc R . . H62C H 1.4391 -0.1535 -0.2868 0.147 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 0.01353(10) 0.01551(11) 0.01472(11) 0.00093(8) -0.00139(8) -0.00077(8) Ru2 0.01378(10) 0.01435(11) 0.01664(11) 0.00074(8) -0.00113(8) -0.00012(8) S1 0.0174(3) 0.0141(3) 0.0184(3) -0.0004(2) -0.0021(2) -0.0011(2) S2 0.0169(3) 0.0191(3) 0.0159(3) 0.0018(2) -0.0035(2) -0.0003(2) S3 0.0161(3) 0.0146(3) 0.0141(3) 0.0016(2) -0.0020(2) -0.0013(2) P1 0.0327(4) 0.0276(5) 0.0364(5) -0.0073(4) -0.0038(4) 0.0048(3) F1 0.044(3) 0.071(5) 0.100(6) -0.035(4) -0.026(4) 0.005(3) F2 0.159(8) 0.060(4) 0.037(3) 0.006(3) -0.017(4) 0.026(5) F3 0.090(5) 0.043(3) 0.075(5) 0.004(3) -0.044(4) 0.019(4) F4 0.048(4) 0.050(5) 0.122(8) -0.037(5) 0.018(4) -0.017(3) F1' 0.051(4) 0.107(7) 0.109(7) -0.054(5) -0.047(4) 0.013(4) F2' 0.129(7) 0.047(4) 0.047(4) -0.002(3) 0.003(4) -0.022(4) F3' 0.114(7) 0.045(4) 0.065(4) -0.004(3) 0.025(5) -0.029(5) F4' 0.038(3) 0.069(6) 0.046(4) -0.028(3) -0.017(3) 0.008(3) F5 0.0648(18) 0.0675(19) 0.091(2) -0.0517(17) 0.0108(16) -0.0001(14) F6 0.0477(14) 0.0707(19) 0.084(2) -0.0456(16) -0.0166(14) 0.0231(13) O1 0.0300(13) 0.0411(15) 0.0360(13) -0.0051(11) -0.0042(10) 0.0010(10) O2 0.0458(17) 0.072(2) 0.0538(18) 0.0229(16) 0.0125(14) 0.0323(16) O3 0.0460(16) 0.067(2) 0.0287(13) -0.0089(13) 0.0106(11) -0.0318(14) O4 0.0335(13) 0.0350(15) 0.0567(17) -0.0123(12) -0.0049(12) -0.0045(11) O5 0.0502(18) 0.072(2) 0.0579(19) -0.0259(17) -0.0119(15) 0.0039(15) O6 0.0511(19) 0.065(2) 0.082(3) 0.0168(19) -0.0062(17) 0.0043(16) N1 0.0271(13) 0.0277(15) 0.0279(14) -0.0061(11) -0.0079(11) 0.0017(11) N2 0.0308(15) 0.0311(16) 0.0378(16) 0.0014(12) -0.0070(12) 0.0006(12) N3 0.0223(12) 0.0232(13) 0.0246(13) -0.0015(10) 0.0016(10) -0.0048(10) C1 0.0157(13) 0.0283(16) 0.0197(14) 0.0014(12) 0.0004(10) -0.0011(11) C2 0.0149(13) 0.0243(15) 0.0231(14) -0.0001(12) 0.0008(11) -0.0050(11) C3 0.0129(12) 0.0329(17) 0.0205(14) 0.0003(12) -0.0014(10) 0.0008(11) C4 0.0144(13) 0.0254(16) 0.0299(16) 0.0029(12) 0.0013(11) 0.0028(11) C5 0.0193(14) 0.0214(15) 0.0329(16) -0.0034(12) 0.0017(12) 0.0016(11) C6 0.0194(14) 0.0294(17) 0.0204(14) -0.0059(12) 0.0031(11) 0.0008(12) C7 0.0302(16) 0.0349(19) 0.0197(15) 0.0064(13) -0.0002(12) -0.0030(13) C8 0.036(2) 0.053(3) 0.037(2) 0.0165(18) 0.0075(16) -0.0092(17) C9 0.077(3) 0.043(3) 0.038(2) 0.0178(18) 0.011(2) 0.022(2) C10 0.0302(17) 0.036(2) 0.0383(19) 0.0106(15) -0.0024(14) 0.0104(14) C11 0.0199(14) 0.0177(15) 0.0291(16) -0.0034(12) 0.0031(12) 0.0007(11) C12 0.0209(14) 0.0198(15) 0.0347(17) 0.0029(12) 0.0014(12) 0.0065(11) C13 0.0182(14) 0.0305(17) 0.0241(15) 0.0034(12) -0.0044(11) 0.0032(12) C14 0.0123(12) 0.0274(16) 0.0276(15) -0.0019(12) -0.0015(11) 0.0003(11) C15 0.0160(13) 0.0209(15) 0.0238(14) 0.0019(11) 0.0003(11) 0.0004(11) C16 0.0165(13) 0.0243(15) 0.0199(14) -0.0004(11) 0.0036(10) -0.0004(11) C17 0.0279(16) 0.0240(17) 0.0325(17) -0.0110(13) 0.0056(13) -0.0036(12) C18 0.049(2) 0.037(2) 0.0305(18) -0.0098(15) -0.0046(16) -0.0076(16) C19 0.038(2) 0.050(3) 0.068(3) -0.037(2) 0.0079(19) 0.0018(18) C20 0.0208(14) 0.041(2) 0.0285(16) -0.0063(14) -0.0043(12) -0.0057(13) C21 0.0246(14) 0.0149(14) 0.0236(14) 0.0005(11) -0.0011(11) -0.0017(11) C22 0.0286(15) 0.0174(15) 0.0257(15) -0.0012(12) -0.0028(12) -0.0027(12) C23 0.0402(19) 0.0191(17) 0.045(2) -0.0017(14) -0.0083(16) -0.0091(14) C24 0.056(2) 0.0150(17) 0.054(2) 0.0087(15) -0.0134(19) -0.0070(15) C25 0.044(2) 0.0243(18) 0.047(2) 0.0097(15) -0.0174(17) 0.0002(15) C26 0.0265(15) 0.0216(16) 0.0340(17) 0.0023(13) -0.0084(13) -0.0001(12) C27 0.0275(15) 0.0179(15) 0.0321(16) -0.0070(12) -0.0089(13) -0.0045(12) C28 0.0318(16) 0.0234(16) 0.0292(16) -0.0046(13) -0.0121(13) -0.0041(12) C29 0.0309(17) 0.0263(17) 0.0368(18) -0.0066(14) -0.0106(14) -0.0022(13) C30 0.0357(19) 0.0279(18) 0.050(2) -0.0039(16) -0.0185(16) -0.0003(14) C31 0.049(2) 0.038(2) 0.043(2) 0.0024(17) -0.0258(18) -0.0042(17) C32 0.047(2) 0.043(2) 0.0284(18) -0.0014(15) -0.0128(16) -0.0107(17) C33 0.0308(17) 0.038(2) 0.0320(17) -0.0079(15) -0.0087(14) -0.0020(14) C34 0.0170(13) 0.0250(15) 0.0145(12) -0.0013(11) -0.0016(10) -0.0027(11) C35 0.0202(14) 0.0344(18) 0.0163(13) 0.0022(12) -0.0014(11) 0.0003(12) C36 0.0309(17) 0.053(2) 0.0231(16) -0.0090(15) -0.0126(13) 0.0026(15) C37 0.0333(17) 0.045(2) 0.0264(16) -0.0157(15) -0.0069(14) -0.0011(15) C38 0.0297(16) 0.0311(18) 0.0243(15) -0.0054(13) -0.0020(13) -0.0012(13) C39 0.0246(14) 0.0266(16) 0.0176(13) -0.0016(11) -0.0038(11) -0.0004(12) C40 0.0256(15) 0.042(2) 0.0209(15) 0.0031(13) -0.0080(12) 0.0057(14) C41 0.028(4) 0.034(4) 0.034(5) 0.000(3) -0.007(4) -0.004(3) C42 0.040(4) 0.033(4) 0.049(5) -0.004(3) -0.007(3) 0.003(3) C43 0.057(5) 0.032(4) 0.055(5) 0.003(3) -0.014(4) -0.004(4) C44 0.066(5) 0.034(4) 0.073(6) 0.003(4) -0.021(5) 0.008(4) C45 0.052(4) 0.055(5) 0.115(7) 0.005(5) -0.009(5) 0.025(4) C46 0.041(4) 0.047(4) 0.090(6) 0.004(4) -0.004(4) 0.012(3) C41' 0.026(4) 0.034(4) 0.029(5) -0.003(4) 0.001(4) 0.005(3) C42' 0.027(4) 0.030(4) 0.056(6) -0.004(4) -0.015(4) -0.003(3) C43' 0.049(5) 0.036(5) 0.058(6) -0.002(4) -0.013(5) -0.008(4) C44' 0.051(5) 0.038(5) 0.042(5) 0.005(4) -0.007(4) 0.006(4) C45' 0.046(5) 0.063(6) 0.100(7) 0.029(5) -0.025(5) 0.009(4) C46' 0.035(4) 0.051(5) 0.079(6) 0.018(5) -0.021(4) -0.002(4) C47 0.0222(13) 0.0159(14) 0.0147(12) 0.0005(10) -0.0023(10) 0.0028(10) C48 0.0244(14) 0.0176(14) 0.0196(14) 0.0028(11) -0.0018(11) 0.0003(11) C49 0.0329(17) 0.0290(17) 0.0181(14) 0.0042(12) -0.0002(12) -0.0004(13) C50 0.0417(19) 0.0343(19) 0.0167(14) 0.0011(13) -0.0091(13) 0.0030(14) C51 0.0307(16) 0.0277(17) 0.0261(16) -0.0043(13) -0.0122(13) 0.0028(13) C52 0.0233(14) 0.0185(15) 0.0241(15) 0.0014(11) -0.0058(11) 0.0006(11) C53 0.0262(15) 0.0220(16) 0.0230(15) 0.0041(12) -0.0010(12) -0.0026(12) C54 0.0256(15) 0.0174(15) 0.0279(15) 0.0027(12) -0.0065(12) -0.0019(11) C55 0.0298(17) 0.037(2) 0.0299(17) -0.0026(14) -0.0046(13) -0.0011(14) C56 0.046(2) 0.053(3) 0.036(2) -0.0102(18) -0.0146(17) 0.0017(18) C57 0.041(2) 0.054(3) 0.049(2) -0.0101(19) -0.0225(18) -0.0063(18) C58 0.0293(18) 0.044(2) 0.053(2) 0.0000(18) -0.0102(16) -0.0066(16) C59 0.0307(17) 0.0295(18) 0.0330(18) 0.0011(14) -0.0016(14) -0.0052(13) C60 0.046(2) 0.046(3) 0.093(4) -0.034(3) -0.002(2) -0.011(2) C61 0.077(4) 0.114(5) 0.074(4) -0.048(4) -0.032(3) 0.023(4) C62 0.083(4) 0.068(4) 0.119(6) 0.038(4) 0.019(4) 0.026(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 C6 2.190(3) . ? Ru1 C5 2.211(3) . ? Ru1 C2 2.213(3) . ? Ru1 C3 2.215(3) . ? Ru1 C4 2.236(3) . ? Ru1 C1 2.248(3) . ? Ru1 S2 2.3940(7) . ? Ru1 S3 2.4015(7) . ? Ru1 S1 2.4077(7) . ? Ru2 C13 2.194(3) . ? Ru2 C15 2.207(3) . ? Ru2 C12 2.210(3) . ? Ru2 C11 2.212(3) . ? Ru2 C16 2.219(3) . ? Ru2 C14 2.227(3) . ? Ru2 S1 2.3916(7) . ? Ru2 S3 2.4068(7) . ? Ru2 S2 2.4163(7) . ? S1 C21 1.788(3) . ? S2 C34 1.789(3) . ? S3 C47 1.799(3) . ? P1 F1' 1.555(5) . ? P1 F2 1.557(5) . ? P1 F4 1.571(6) . ? P1 F3' 1.574(6) . ? P1 F2' 1.577(5) . ? P1 F3 1.582(5) . ? P1 F5 1.589(3) . ? P1 F1 1.591(5) . ? P1 F4' 1.599(5) . ? P1 F6 1.599(2) . ? O1 C27 1.217(4) . ? O2 C40 1.217(4) . ? O3 C53 1.220(4) . ? O4 C60 1.429(5) . ? O4 H1O4 0.8401 . ? O5 C61 1.423(6) . ? O5 H1O5 0.8400 . ? O6 C62 1.431(6) . ? O6 H1O6 0.8399 . ? N1 C27 1.351(4) . ? N1 C28 1.423(4) . ? N1 H1 0.8800 . ? N2 C40 1.337(4) . ? N2 C41' 1.413(7) . ? N2 C41 1.443(6) . ? N2 H2 0.8800 . ? N3 C53 1.351(4) . ? N3 C54 1.414(4) . ? N3 H3 0.8800 . ? C1 C2 1.413(4) . ? C1 C6 1.430(4) . ? C1 C7 1.512(4) . ? C2 C3 1.421(4) . ? C2 H2A 1.0000 . ? C3 C4 1.411(4) . ? C3 H3A 1.0000 . ? C4 C5 1.419(5) . ? C4 C10 1.504(4) . ? C5 C6 1.414(4) . ? C5 H5A 1.0000 . ? C6 H6A 1.0000 . ? C7 C9 1.516(5) . ? C7 C8 1.534(5) . ? C7 H7A 1.0000 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C16 1.406(4) . ? C11 C12 1.444(4) . ? C11 C17 1.521(4) . ? C12 C13 1.397(5) . ? C12 H12A 1.0000 . ? C13 C14 1.438(4) . ? C13 H13A 1.0000 . ? C14 C15 1.405(4) . ? C14 C20 1.499(4) . ? C15 C16 1.428(4) . ? C15 H15A 1.0000 . ? C16 H16A 1.0000 . ? C17 C18 1.518(5) . ? C17 C19 1.532(5) . ? C17 H17A 1.0000 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C26 1.388(4) . ? C21 C22 1.408(4) . ? C22 C23 1.391(4) . ? C22 C27 1.510(4) . ? C23 C24 1.379(5) . ? C23 H23A 0.9500 . ? C24 C25 1.388(5) . ? C24 H24A 0.9500 . ? C25 C26 1.388(5) . ? C25 H25A 0.9500 . ? C26 H26A 0.9500 . ? C28 C33 1.390(5) . ? C28 C29 1.395(5) . ? C29 C30 1.392(5) . ? C29 H29A 0.9500 . ? C30 C31 1.378(6) . ? C30 H30A 0.9500 . ? C31 C32 1.383(6) . ? C31 H31A 0.9500 . ? C32 C33 1.389(5) . ? C32 H32A 0.9500 . ? C33 H33A 0.9500 . ? C34 C39 1.396(4) . ? C34 C35 1.406(4) . ? C35 C36 1.393(5) . ? C35 C40 1.508(5) . ? C36 C37 1.375(5) . ? C36 H36A 0.9500 . ? C37 C38 1.383(5) . ? C37 H37A 0.9500 . ? C38 C39 1.387(4) . ? C38 H38A 0.9500 . ? C39 H39A 0.9500 . ? C41 C46 1.386(7) . ? C41 C42 1.389(7) . ? C42 C43 1.383(6) . ? C42 H42A 0.9500 . ? C43 C44 1.386(7) . ? C43 H43A 0.9500 . ? C44 C45 1.380(7) . ? C44 H44A 0.9500 . ? C45 C46 1.390(7) . ? C45 H45A 0.9500 . ? C46 H46A 0.9500 . ? C41' C46' 1.370(9) . ? C41' C42' 1.372(9) . ? C42' C43' 1.381(9) . ? C42' H42B 0.9500 . ? C43' C44' 1.383(10) . ? C43' H43B 0.9500 . ? C44' C45' 1.377(10) . ? C44' H44B 0.9500 . ? C45' C46' 1.391(9) . ? C45' H45B 0.9500 . ? C46' H46B 0.9500 . ? C47 C52 1.392(4) . ? C47 C48 1.415(4) . ? C48 C49 1.399(4) . ? C48 C53 1.511(4) . ? C49 C50 1.372(5) . ? C49 H49A 0.9500 . ? C50 C51 1.386(5) . ? C50 H50A 0.9500 . ? C51 C52 1.382(4) . ? C51 H51A 0.9500 . ? C52 H52A 0.9500 . ? C54 C55 1.387(5) . ? C54 C59 1.408(4) . ? C55 C56 1.387(5) . ? C55 H55A 0.9500 . ? C56 C57 1.384(6) . ? C56 H56A 0.9500 . ? C57 C58 1.375(6) . ? C57 H57A 0.9500 . ? C58 C59 1.389(5) . ? C58 H58A 0.9500 . ? C59 H59A 0.9500 . ? C60 H60A 0.9800 . ? C60 H60B 0.9800 . ? C60 H60C 0.9800 . ? C61 H61A 0.9800 . ? C61 H61B 0.9800 . ? C61 H61C 0.9800 . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C62 H62C 0.9800 . ? 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 C6 Ru1 C5 37.49(12) . . ? C6 Ru1 C2 67.01(11) . . ? C5 Ru1 C2 79.40(11) . . ? C6 Ru1 C3 79.09(11) . . ? C5 Ru1 C3 66.73(12) . . ? C2 Ru1 C3 37.44(11) . . ? C6 Ru1 C4 67.36(12) . . ? C5 Ru1 C4 37.22(12) . . ? C2 Ru1 C4 67.33(11) . . ? C3 Ru1 C4 36.96(12) . . ? C6 Ru1 C1 37.57(11) . . ? C5 Ru1 C1 67.69(11) . . ? C2 Ru1 C1 36.91(11) . . ? C3 Ru1 C1 67.06(11) . . ? C4 Ru1 C1 79.80(11) . . ? C6 Ru1 S2 95.42(8) . . ? C5 Ru1 S2 118.85(9) . . ? C2 Ru1 S2 123.97(8) . . ? C3 Ru1 S2 161.27(8) . . ? C4 Ru1 S2 155.09(9) . . ? C1 Ru1 S2 97.65(8) . . ? C6 Ru1 S3 124.47(8) . . ? C5 Ru1 S3 98.54(8) . . ? C2 Ru1 S3 156.25(8) . . ? C3 Ru1 S3 119.96(8) . . ? C4 Ru1 S3 96.61(8) . . ? C1 Ru1 S3 161.63(8) . . ? S2 Ru1 S3 77.97(2) . . ? C6 Ru1 S1 156.94(9) . . ? C5 Ru1 S1 162.62(9) . . ? C2 Ru1 S1 99.44(8) . . ? C3 Ru1 S1 101.74(8) . . ? C4 Ru1 S1 126.29(9) . . ? C1 Ru1 S1 121.22(8) . . ? S2 Ru1 S1 76.35(2) . . ? S3 Ru1 S1 75.46(2) . . ? C13 Ru2 C15 66.73(11) . . ? C13 Ru2 C12 36.99(12) . . ? C15 Ru2 C12 78.82(11) . . ? C13 Ru2 C11 68.17(12) . . ? C15 Ru2 C11 67.52(11) . . ? C12 Ru2 C11 38.12(12) . . ? C13 Ru2 C16 79.50(11) . . ? C15 Ru2 C16 37.65(11) . . ? C12 Ru2 C16 67.02(11) . . ? C11 Ru2 C16 37.01(11) . . ? C13 Ru2 C14 37.96(12) . . ? C15 Ru2 C14 36.94(11) . . ? C12 Ru2 C14 67.85(12) . . ? C11 Ru2 C14 81.26(11) . . ? C16 Ru2 C14 67.97(11) . . ? C13 Ru2 S1 132.75(9) . . ? C15 Ru2 S1 147.65(8) . . ? C12 Ru2 S1 103.61(9) . . ? C11 Ru2 S1 94.20(8) . . ? C16 Ru2 S1 112.90(8) . . ? C14 Ru2 S1 170.69(8) . . ? C13 Ru2 S3 149.08(9) . . ? C15 Ru2 S3 95.40(8) . . ? C12 Ru2 S3 168.07(9) . . ? C11 Ru2 S3 130.00(8) . . ? C16 Ru2 S3 102.04(8) . . ? C14 Ru2 S3 113.47(8) . . ? S1 Ru2 S3 75.66(2) . . ? C13 Ru2 S2 96.07(8) . . ? C15 Ru2 S2 132.92(8) . . ? C12 Ru2 S2 114.16(9) . . ? C11 Ru2 S2 148.37(8) . . ? C16 Ru2 S2 170.56(8) . . ? C14 Ru2 S2 103.42(8) . . ? S1 Ru2 S2 76.24(2) . . ? S3 Ru2 S2 77.44(2) . . ? C21 S1 Ru2 115.84(10) . . ? C21 S1 Ru1 112.14(10) . . ? Ru2 S1 Ru1 88.85(2) . . ? C34 S2 Ru1 111.82(10) . . ? C34 S2 Ru2 112.22(9) . . ? Ru1 S2 Ru2 88.60(2) . . ? C47 S3 Ru1 114.80(10) . . ? C47 S3 Ru2 106.64(9) . . ? Ru1 S3 Ru2 88.64(2) . . ? F1' P1 F2 70.1(6) . . ? F1' P1 F4 161.1(6) . . ? F2 P1 F4 91.8(5) . . ? F1' P1 F3' 92.1(5) . . ? F2 P1 F3' 155.7(5) . . ? F4 P1 F3' 106.8(5) . . ? F1' P1 F2' 93.4(5) . . ? F2 P1 F2' 29.7(4) . . ? F4 P1 F2' 67.6(5) . . ? F3' P1 F2' 174.2(5) . . ? F1' P1 F3 109.2(6) . . ? F2 P1 F3 177.3(5) . . ? F4 P1 F3 89.1(5) . . ? F3' P1 F3 22.0(4) . . ? F2' P1 F3 152.5(5) . . ? F1' P1 F5 87.1(5) . . ? F2 P1 F5 100.8(4) . . ? F4 P1 F5 91.1(5) . . ? F3' P1 F5 94.4(5) . . ? F2' P1 F5 84.2(4) . . ? F3 P1 F5 81.7(4) . . ? F1' P1 F1 23.4(5) . . ? F2 P1 F1 91.6(5) . . ? F4 P1 F1 175.1(5) . . ? F3' P1 F1 68.9(5) . . ? F2' P1 F1 116.7(5) . . ? F3 P1 F1 87.3(4) . . ? F5 P1 F1 91.7(4) . . ? F1' P1 F4' 179.2(7) . . ? F2 P1 F4' 109.9(5) . . ? F4 P1 F4' 18.7(5) . . ? F3' P1 F4' 88.1(5) . . ? F2' P1 F4' 86.3(4) . . ? F3 P1 F4' 70.8(5) . . ? F5 P1 F4' 92.1(4) . . ? F1 P1 F4' 157.0(5) . . ? F1' P1 F6 94.9(5) . . ? F2 P1 F6 82.4(4) . . ? F4 P1 F6 87.9(5) . . ? F3' P1 F6 82.9(5) . . ? F2' P1 F6 98.3(4) . . ? F3 P1 F6 95.1(4) . . ? F5 P1 F6 176.67(19) . . ? F1 P1 F6 89.1(4) . . ? F4' P1 F6 85.9(4) . . ? C60 O4 H1O4 114.5 . . ? C61 O5 H1O5 111.5 . . ? C62 O6 H1O6 96.9 . . ? C27 N1 C28 128.0(3) . . ? C27 N1 H1 116.0 . . ? C28 N1 H1 116.0 . . ? C40 N2 C41' 134.7(6) . . ? C40 N2 C41 123.0(4) . . ? C41' N2 C41 12.7(10) . . ? C40 N2 H2 118.5 . . ? C41' N2 H2 106.5 . . ? C41 N2 H2 118.5 . . ? C53 N3 C54 128.0(3) . . ? C53 N3 H3 116.0 . . ? C54 N3 H3 116.0 . . ? C2 C1 C6 117.5(3) . . ? C2 C1 C7 122.7(3) . . ? C6 C1 C7 119.8(3) . . ? C2 C1 Ru1 70.19(16) . . ? C6 C1 Ru1 69.00(16) . . ? C7 C1 Ru1 135.2(2) . . ? C1 C2 C3 120.9(3) . . ? C1 C2 Ru1 72.90(16) . . ? C3 C2 Ru1 71.37(16) . . ? C1 C2 H2A 119.1 . . ? C3 C2 H2A 119.1 . . ? Ru1 C2 H2A 119.1 . . ? C4 C3 C2 121.1(3) . . ? C4 C3 Ru1 72.33(17) . . ? C2 C3 Ru1 71.20(16) . . ? C4 C3 H3A 118.9 . . ? C2 C3 H3A 118.9 . . ? Ru1 C3 H3A 118.9 . . ? C3 C4 C5 118.7(3) . . ? C3 C4 C10 121.4(3) . . ? C5 C4 C10 120.0(3) . . ? C3 C4 Ru1 70.71(16) . . ? C5 C4 Ru1 70.45(17) . . ? C10 C4 Ru1 131.4(2) . . ? C6 C5 C4 120.1(3) . . ? C6 C5 Ru1 70.43(17) . . ? C4 C5 Ru1 72.34(17) . . ? C6 C5 H5A 119.4 . . ? C4 C5 H5A 119.4 . . ? Ru1 C5 H5A 119.4 . . ? C5 C6 C1 121.7(3) . . ? C5 C6 Ru1 72.09(17) . . ? C1 C6 Ru1 73.43(16) . . ? C5 C6 H6A 118.8 . . ? C1 C6 H6A 118.8 . . ? Ru1 C6 H6A 118.8 . . ? C1 C7 C9 114.6(3) . . ? C1 C7 C8 106.8(3) . . ? C9 C7 C8 112.0(3) . . ? C1 C7 H7A 107.7 . . ? C9 C7 H7A 107.7 . . ? C8 C7 H7A 107.7 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C4 C10 H10A 109.5 . . ? C4 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C4 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C16 C11 C12 118.1(3) . . ? C16 C11 C17 123.1(3) . . ? C12 C11 C17 118.8(3) . . ? C16 C11 Ru2 71.76(16) . . ? C12 C11 Ru2 70.85(17) . . ? C17 C11 Ru2 128.0(2) . . ? C13 C12 C11 120.7(3) . . ? C13 C12 Ru2 70.88(17) . . ? C11 C12 Ru2 71.03(16) . . ? C13 C12 H12A 118.9 . . ? C11 C12 H12A 118.9 . . ? Ru2 C12 H12A 118.9 . . ? C12 C13 C14 121.7(3) . . ? C12 C13 Ru2 72.13(17) . . ? C14 C13 Ru2 72.27(16) . . ? C12 C13 H13A 118.6 . . ? C14 C13 H13A 118.6 . . ? Ru2 C13 H13A 118.6 . . ? C15 C14 C13 116.7(3) . . ? C15 C14 C20 121.5(3) . . ? C13 C14 C20 121.8(3) . . ? C15 C14 Ru2 70.74(16) . . ? C13 C14 Ru2 69.77(16) . . ? C20 C14 Ru2 128.6(2) . . ? C14 C15 C16 122.6(3) . . ? C14 C15 Ru2 72.31(16) . . ? C16 C15 Ru2 71.64(16) . . ? C14 C15 H15A 118.0 . . ? C16 C15 H15A 118.0 . . ? Ru2 C15 H15A 118.0 . . ? C11 C16 C15 120.1(3) . . ? C11 C16 Ru2 71.23(16) . . ? C15 C16 Ru2 70.71(16) . . ? C11 C16 H16A 119.3 . . ? C15 C16 H16A 119.3 . . ? Ru2 C16 H16A 119.3 . . ? C18 C17 C11 113.6(3) . . ? C18 C17 C19 111.0(3) . . ? C11 C17 C19 109.1(3) . . ? C18 C17 H17A 107.6 . . ? C11 C17 H17A 107.6 . . ? C19 C17 H17A 107.6 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C14 C20 H20A 109.5 . . ? C14 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C14 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C26 C21 C22 119.8(3) . . ? C26 C21 S1 123.4(2) . . ? C22 C21 S1 116.7(2) . . ? C23 C22 C21 119.0(3) . . ? C23 C22 C27 119.5(3) . . ? C21 C22 C27 121.4(3) . . ? C24 C23 C22 121.0(3) . . ? C24 C23 H23A 119.5 . . ? C22 C23 H23A 119.5 . . ? C23 C24 C25 119.8(3) . . ? C23 C24 H24A 120.1 . . ? C25 C24 H24A 120.1 . . ? C26 C25 C24 120.2(3) . . ? C26 C25 H25A 119.9 . . ? C24 C25 H25A 119.9 . . ? C21 C26 C25 120.1(3) . . ? C21 C26 H26A 119.9 . . ? C25 C26 H26A 119.9 . . ? O1 C27 N1 124.5(3) . . ? O1 C27 C22 121.0(3) . . ? N1 C27 C22 114.5(3) . . ? C33 C28 C29 119.5(3) . . ? C33 C28 N1 116.9(3) . . ? C29 C28 N1 123.5(3) . . ? C30 C29 C28 119.1(3) . . ? C30 C29 H29A 120.5 . . ? C28 C29 H29A 120.5 . . ? C31 C30 C29 121.6(3) . . ? C31 C30 H30A 119.2 . . ? C29 C30 H30A 119.2 . . ? C30 C31 C32 118.9(3) . . ? C30 C31 H31A 120.5 . . ? C32 C31 H31A 120.5 . . ? C31 C32 C33 120.6(4) . . ? C31 C32 H32A 119.7 . . ? C33 C32 H32A 119.7 . . ? C32 C33 C28 120.2(3) . . ? C32 C33 H33A 119.9 . . ? C28 C33 H33A 119.9 . . ? C39 C34 C35 119.1(3) . . ? C39 C34 S2 123.0(2) . . ? C35 C34 S2 117.9(2) . . ? C36 C35 C34 119.1(3) . . ? C36 C35 C40 118.5(3) . . ? C34 C35 C40 122.2(3) . . ? C37 C36 C35 121.2(3) . . ? C37 C36 H36A 119.4 . . ? C35 C36 H36A 119.4 . . ? C36 C37 C38 119.8(3) . . ? C36 C37 H37A 120.1 . . ? C38 C37 H37A 120.1 . . ? C37 C38 C39 120.1(3) . . ? C37 C38 H38A 119.9 . . ? C39 C38 H38A 119.9 . . ? C38 C39 C34 120.6(3) . . ? C38 C39 H39A 119.7 . . ? C34 C39 H39A 119.7 . . ? O2 C40 N2 123.7(3) . . ? O2 C40 C35 121.0(3) . . ? N2 C40 C35 115.2(3) . . ? C46 C41 C42 118.5(5) . . ? C46 C41 N2 127.0(6) . . ? C42 C41 N2 114.5(6) . . ? C43 C42 C41 121.1(6) . . ? C43 C42 H42A 119.4 . . ? C41 C42 H42A 119.4 . . ? C42 C43 C44 120.3(7) . . ? C42 C43 H43A 119.9 . . ? C44 C43 H43A 119.9 . . ? C45 C44 C43 118.7(6) . . ? C45 C44 H44A 120.6 . . ? C43 C44 H44A 120.6 . . ? C44 C45 C46 121.1(6) . . ? C44 C45 H45A 119.4 . . ? C46 C45 H45A 119.4 . . ? C41 C46 C45 120.2(6) . . ? C41 C46 H46A 119.9 . . ? C45 C46 H46A 119.9 . . ? C46' C41' C42' 121.3(7) . . ? C46' C41' N2 117.7(8) . . ? C42' C41' N2 120.9(8) . . ? C41' C42' C43' 120.3(8) . . ? C41' C42' H42B 119.8 . . ? C43' C42' H42B 119.8 . . ? C42' C43' C44' 119.5(8) . . ? C42' C43' H43B 120.3 . . ? C44' C43' H43B 120.3 . . ? C45' C44' C43' 119.0(8) . . ? C45' C44' H44B 120.5 . . ? C43' C44' H44B 120.5 . . ? C44' C45' C46' 121.8(8) . . ? C44' C45' H45B 119.1 . . ? C46' C45' H45B 119.1 . . ? C41' C46' C45' 117.8(7) . . ? C41' C46' H46B 121.1 . . ? C45' C46' H46B 121.1 . . ? C52 C47 C48 119.0(3) . . ? C52 C47 S3 119.9(2) . . ? C48 C47 S3 121.0(2) . . ? C49 C48 C47 117.9(3) . . ? C49 C48 C53 114.1(3) . . ? C47 C48 C53 127.9(3) . . ? C50 C49 C48 122.2(3) . . ? C50 C49 H49A 118.9 . . ? C48 C49 H49A 118.9 . . ? C49 C50 C51 119.6(3) . . ? C49 C50 H50A 120.2 . . ? C51 C50 H50A 120.2 . . ? C52 C51 C50 119.6(3) . . ? C52 C51 H51A 120.2 . . ? C50 C51 H51A 120.2 . . ? C51 C52 C47 121.5(3) . . ? C51 C52 H52A 119.2 . . ? C47 C52 H52A 119.2 . . ? O3 C53 N3 122.4(3) . . ? O3 C53 C48 119.5(3) . . ? N3 C53 C48 118.1(3) . . ? C55 C54 C59 119.5(3) . . ? C55 C54 N3 117.0(3) . . ? C59 C54 N3 123.4(3) . . ? C54 C55 C56 120.8(3) . . ? C54 C55 H55A 119.6 . . ? C56 C55 H55A 119.6 . . ? C57 C56 C55 119.9(4) . . ? C57 C56 H56A 120.0 . . ? C55 C56 H56A 120.0 . . ? C58 C57 C56 119.4(4) . . ? C58 C57 H57A 120.3 . . ? C56 C57 H57A 120.3 . . ? C57 C58 C59 122.0(4) . . ? C57 C58 H58A 119.0 . . ? C59 C58 H58A 119.0 . . ? C58 C59 C54 118.4(3) . . ? C58 C59 H59A 120.8 . . ? C54 C59 H59A 120.8 . . ? O4 C60 H60A 109.5 . . ? O4 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? O4 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? O5 C61 H61A 109.5 . . ? O5 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? O5 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? O6 C62 H62A 109.5 . . ? O6 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? O6 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C13 Ru2 S1 C21 11.03(16) . . . . ? C15 Ru2 S1 C21 128.03(18) . . . . ? C12 Ru2 S1 C21 37.48(14) . . . . ? C11 Ru2 S1 C21 74.93(14) . . . . ? C16 Ru2 S1 C21 107.99(14) . . . . ? C14 Ru2 S1 C21 14.5(5) . . . . ? S3 Ru2 S1 C21 -154.79(11) . . . . ? S2 Ru2 S1 C21 -74.49(11) . . . . ? C13 Ru2 S1 Ru1 125.18(11) . . . . ? C15 Ru2 S1 Ru1 -117.82(15) . . . . ? C12 Ru2 S1 Ru1 151.63(9) . . . . ? C11 Ru2 S1 Ru1 -170.92(8) . . . . ? C16 Ru2 S1 Ru1 -137.86(9) . . . . ? C14 Ru2 S1 Ru1 128.7(5) . . . . ? S3 Ru2 S1 Ru1 -40.64(2) . . . . ? S2 Ru2 S1 Ru1 39.66(2) . . . . ? C6 Ru1 S1 C21 6.3(2) . . . . ? C5 Ru1 S1 C21 -130.0(3) . . . . ? C2 Ru1 S1 C21 -45.38(13) . . . . ? C3 Ru1 S1 C21 -83.42(13) . . . . ? C4 Ru1 S1 C21 -114.11(14) . . . . ? C1 Ru1 S1 C21 -13.27(14) . . . . ? S2 Ru1 S1 C21 77.47(11) . . . . ? S3 Ru1 S1 C21 158.34(11) . . . . ? C6 Ru1 S1 Ru2 -111.3(2) . . . . ? C5 Ru1 S1 Ru2 112.4(3) . . . . ? C2 Ru1 S1 Ru2 -162.93(8) . . . . ? C3 Ru1 S1 Ru2 159.03(8) . . . . ? C4 Ru1 S1 Ru2 128.34(10) . . . . ? C1 Ru1 S1 Ru2 -130.82(9) . . . . ? S2 Ru1 S1 Ru2 -40.08(2) . . . . ? S3 Ru1 S1 Ru2 40.80(2) . . . . ? C6 Ru1 S2 C34 -48.85(13) . . . . ? C5 Ru1 S2 C34 -17.92(14) . . . . ? C2 Ru1 S2 C34 -114.70(14) . . . . ? C3 Ru1 S2 C34 -120.7(3) . . . . ? C4 Ru1 S2 C34 -4.4(2) . . . . ? C1 Ru1 S2 C34 -86.61(13) . . . . ? S3 Ru1 S2 C34 75.28(10) . . . . ? S1 Ru1 S2 C34 153.02(10) . . . . ? C6 Ru1 S2 Ru2 -162.28(9) . . . . ? C5 Ru1 S2 Ru2 -131.35(9) . . . . ? C2 Ru1 S2 Ru2 131.88(10) . . . . ? C3 Ru1 S2 Ru2 125.9(3) . . . . ? C4 Ru1 S2 Ru2 -117.81(18) . . . . ? C1 Ru1 S2 Ru2 159.96(8) . . . . ? S3 Ru1 S2 Ru2 -38.15(2) . . . . ? S1 Ru1 S2 Ru2 39.59(2) . . . . ? C13 Ru2 S2 C34 74.42(13) . . . . ? C15 Ru2 S2 C34 10.76(15) . . . . ? C12 Ru2 S2 C34 108.05(14) . . . . ? C11 Ru2 S2 C34 131.71(18) . . . . ? C16 Ru2 S2 C34 13.0(5) . . . . ? C14 Ru2 S2 C34 36.58(13) . . . . ? S1 Ru2 S2 C34 -152.99(11) . . . . ? S3 Ru2 S2 C34 -74.91(10) . . . . ? C13 Ru2 S2 Ru1 -172.53(9) . . . . ? C15 Ru2 S2 Ru1 123.81(11) . . . . ? C12 Ru2 S2 Ru1 -138.89(10) . . . . ? C11 Ru2 S2 Ru1 -115.23(16) . . . . ? C16 Ru2 S2 Ru1 126.0(5) . . . . ? C14 Ru2 S2 Ru1 149.63(8) . . . . ? S1 Ru2 S2 Ru1 -39.93(2) . . . . ? S3 Ru2 S2 Ru1 38.14(2) . . . . ? C6 Ru1 S3 C47 -125.62(14) . . . . ? C5 Ru1 S3 C47 -96.11(13) . . . . ? C2 Ru1 S3 C47 -13.0(2) . . . . ? C3 Ru1 S3 C47 -28.10(14) . . . . ? C4 Ru1 S3 C47 -58.60(13) . . . . ? C1 Ru1 S3 C47 -136.1(3) . . . . ? S2 Ru1 S3 C47 146.06(10) . . . . ? S1 Ru1 S3 C47 67.24(10) . . . . ? C6 Ru1 S3 Ru2 126.65(10) . . . . ? C5 Ru1 S3 Ru2 156.16(9) . . . . ? C2 Ru1 S3 Ru2 -120.8(2) . . . . ? C3 Ru1 S3 Ru2 -135.83(10) . . . . ? C4 Ru1 S3 Ru2 -166.33(9) . . . . ? C1 Ru1 S3 Ru2 116.2(2) . . . . ? S2 Ru1 S3 Ru2 38.33(2) . . . . ? S1 Ru1 S3 Ru2 -40.49(2) . . . . ? C13 Ru2 S3 C47 125.74(18) . . . . ? C15 Ru2 S3 C47 73.66(13) . . . . ? C12 Ru2 S3 C47 13.3(4) . . . . ? C11 Ru2 S3 C47 8.61(14) . . . . ? C16 Ru2 S3 C47 36.13(13) . . . . ? C14 Ru2 S3 C47 107.13(13) . . . . ? S1 Ru2 S3 C47 -74.74(10) . . . . ? S2 Ru2 S3 C47 -153.52(10) . . . . ? C13 Ru2 S3 Ru1 -118.74(16) . . . . ? C15 Ru2 S3 Ru1 -170.82(8) . . . . ? C12 Ru2 S3 Ru1 128.8(4) . . . . ? C11 Ru2 S3 Ru1 124.13(10) . . . . ? C16 Ru2 S3 Ru1 151.65(8) . . . . ? C14 Ru2 S3 Ru1 -137.35(9) . . . . ? S1 Ru2 S3 Ru1 40.78(2) . . . . ? S2 Ru2 S3 Ru1 -38.00(2) . . . . ? C6 Ru1 C1 C2 131.6(3) . . . . ? C5 Ru1 C1 C2 102.4(2) . . . . ? C3 Ru1 C1 C2 29.29(18) . . . . ? C4 Ru1 C1 C2 65.64(19) . . . . ? S2 Ru1 C1 C2 -139.45(16) . . . . ? S3 Ru1 C1 C2 145.8(2) . . . . ? S1 Ru1 C1 C2 -60.82(19) . . . . ? C5 Ru1 C1 C6 -29.16(18) . . . . ? C2 Ru1 C1 C6 -131.6(3) . . . . ? C3 Ru1 C1 C6 -102.3(2) . . . . ? C4 Ru1 C1 C6 -65.96(18) . . . . ? S2 Ru1 C1 C6 88.95(17) . . . . ? S3 Ru1 C1 C6 14.2(4) . . . . ? S1 Ru1 C1 C6 167.59(15) . . . . ? C6 Ru1 C1 C7 -111.6(4) . . . . ? C5 Ru1 C1 C7 -140.8(3) . . . . ? C2 Ru1 C1 C7 116.8(4) . . . . ? C3 Ru1 C1 C7 146.1(3) . . . . ? C4 Ru1 C1 C7 -177.5(3) . . . . ? S2 Ru1 C1 C7 -22.6(3) . . . . ? S3 Ru1 C1 C7 -97.4(4) . . . . ? S1 Ru1 C1 C7 56.0(3) . . . . ? C6 C1 C2 C3 -3.0(4) . . . . ? C7 C1 C2 C3 173.4(3) . . . . ? Ru1 C1 C2 C3 -55.0(2) . . . . ? C6 C1 C2 Ru1 51.9(2) . . . . ? C7 C1 C2 Ru1 -131.7(3) . . . . ? C6 Ru1 C2 C1 -29.69(18) . . . . ? C5 Ru1 C2 C1 -66.80(19) . . . . ? C3 Ru1 C2 C1 -132.2(3) . . . . ? C4 Ru1 C2 C1 -103.7(2) . . . . ? S2 Ru1 C2 C1 51.0(2) . . . . ? S3 Ru1 C2 C1 -153.91(17) . . . . ? S1 Ru1 C2 C1 130.81(16) . . . . ? C6 Ru1 C2 C3 102.5(2) . . . . ? C5 Ru1 C2 C3 65.38(19) . . . . ? C4 Ru1 C2 C3 28.49(18) . . . . ? C1 Ru1 C2 C3 132.2(3) . . . . ? S2 Ru1 C2 C3 -176.85(14) . . . . ? S3 Ru1 C2 C3 -21.7(3) . . . . ? S1 Ru1 C2 C3 -97.01(17) . . . . ? C1 C2 C3 C4 1.1(4) . . . . ? Ru1 C2 C3 C4 -54.6(2) . . . . ? C1 C2 C3 Ru1 55.7(2) . . . . ? C6 Ru1 C3 C4 66.69(18) . . . . ? C5 Ru1 C3 C4 29.51(18) . . . . ? C2 Ru1 C3 C4 132.9(3) . . . . ? C1 Ru1 C3 C4 104.04(19) . . . . ? S2 Ru1 C3 C4 141.1(2) . . . . ? S3 Ru1 C3 C4 -56.97(19) . . . . ? S1 Ru1 C3 C4 -136.83(16) . . . . ? C6 Ru1 C3 C2 -66.25(18) . . . . ? C5 Ru1 C3 C2 -103.43(19) . . . . ? C4 Ru1 C3 C2 -132.9(3) . . . . ? C1 Ru1 C3 C2 -28.90(17) . . . . ? S2 Ru1 C3 C2 8.1(4) . . . . ? S3 Ru1 C3 C2 170.09(14) . . . . ? S1 Ru1 C3 C2 90.24(17) . . . . ? C2 C3 C4 C5 0.6(4) . . . . ? Ru1 C3 C4 C5 -53.5(2) . . . . ? C2 C3 C4 C10 -178.6(3) . . . . ? Ru1 C3 C4 C10 127.4(3) . . . . ? C2 C3 C4 Ru1 54.0(2) . . . . ? C6 Ru1 C4 C3 -102.31(19) . . . . ? C5 Ru1 C4 C3 -131.6(3) . . . . ? C2 Ru1 C4 C3 -28.83(17) . . . . ? C1 Ru1 C4 C3 -65.20(18) . . . . ? S2 Ru1 C4 C3 -151.38(16) . . . . ? S3 Ru1 C4 C3 133.01(16) . . . . ? S1 Ru1 C4 C3 56.22(19) . . . . ? C6 Ru1 C4 C5 29.26(17) . . . . ? C2 Ru1 C4 C5 102.73(19) . . . . ? C3 Ru1 C4 C5 131.6(3) . . . . ? C1 Ru1 C4 C5 66.37(18) . . . . ? S2 Ru1 C4 C5 -19.8(3) . . . . ? S3 Ru1 C4 C5 -95.42(17) . . . . ? S1 Ru1 C4 C5 -172.22(14) . . . . ? C6 Ru1 C4 C10 142.4(4) . . . . ? C5 Ru1 C4 C10 113.2(4) . . . . ? C2 Ru1 C4 C10 -144.1(4) . . . . ? C3 Ru1 C4 C10 -115.3(4) . . . . ? C1 Ru1 C4 C10 179.5(3) . . . . ? S2 Ru1 C4 C10 93.4(4) . . . . ? S3 Ru1 C4 C10 17.8(3) . . . . ? S1 Ru1 C4 C10 -59.0(3) . . . . ? C3 C4 C5 C6 -0.2(4) . . . . ? C10 C4 C5 C6 179.0(3) . . . . ? Ru1 C4 C5 C6 -53.8(2) . . . . ? C3 C4 C5 Ru1 53.6(2) . . . . ? C10 C4 C5 Ru1 -127.2(3) . . . . ? C2 Ru1 C5 C6 65.85(18) . . . . ? C3 Ru1 C5 C6 102.83(19) . . . . ? C4 Ru1 C5 C6 132.2(3) . . . . ? C1 Ru1 C5 C6 29.22(17) . . . . ? S2 Ru1 C5 C6 -57.23(19) . . . . ? S3 Ru1 C5 C6 -138.14(16) . . . . ? S1 Ru1 C5 C6 153.6(2) . . . . ? C6 Ru1 C5 C4 -132.2(3) . . . . ? C2 Ru1 C5 C4 -66.30(18) . . . . ? C3 Ru1 C5 C4 -29.32(17) . . . . ? C1 Ru1 C5 C4 -102.93(19) . . . . ? S2 Ru1 C5 C4 170.62(14) . . . . ? S3 Ru1 C5 C4 89.71(17) . . . . ? S1 Ru1 C5 C4 21.4(4) . . . . ? C4 C5 C6 C1 -1.8(4) . . . . ? Ru1 C5 C6 C1 -56.5(2) . . . . ? C4 C5 C6 Ru1 54.7(2) . . . . ? C2 C1 C6 C5 3.4(4) . . . . ? C7 C1 C6 C5 -173.1(3) . . . . ? Ru1 C1 C6 C5 55.9(2) . . . . ? C2 C1 C6 Ru1 -52.5(2) . . . . ? C7 C1 C6 Ru1 131.0(3) . . . . ? C2 Ru1 C6 C5 -103.0(2) . . . . ? C3 Ru1 C6 C5 -65.81(19) . . . . ? C4 Ru1 C6 C5 -29.07(18) . . . . ? C1 Ru1 C6 C5 -132.2(3) . . . . ? S2 Ru1 C6 C5 132.29(17) . . . . ? S3 Ru1 C6 C5 53.2(2) . . . . ? S1 Ru1 C6 C5 -160.18(17) . . . . ? C5 Ru1 C6 C1 132.2(3) . . . . ? C2 Ru1 C6 C1 29.20(17) . . . . ? C3 Ru1 C6 C1 66.39(18) . . . . ? C4 Ru1 C6 C1 103.14(19) . . . . ? S2 Ru1 C6 C1 -95.50(16) . . . . ? S3 Ru1 C6 C1 -174.62(13) . . . . ? S1 Ru1 C6 C1 -28.0(3) . . . . ? C2 C1 C7 C9 46.8(4) . . . . ? C6 C1 C7 C9 -136.8(4) . . . . ? Ru1 C1 C7 C9 -47.4(5) . . . . ? C2 C1 C7 C8 -77.8(4) . . . . ? C6 C1 C7 C8 98.5(3) . . . . ? Ru1 C1 C7 C8 -172.1(3) . . . . ? C13 Ru2 C11 C16 -101.8(2) . . . . ? C15 Ru2 C11 C16 -29.00(17) . . . . ? C12 Ru2 C11 C16 -129.8(3) . . . . ? C14 Ru2 C11 C16 -64.76(18) . . . . ? S1 Ru2 C11 C16 123.42(17) . . . . ? S3 Ru2 C11 C16 48.6(2) . . . . ? S2 Ru2 C11 C16 -166.18(14) . . . . ? C13 Ru2 C11 C12 27.96(18) . . . . ? C15 Ru2 C11 C12 100.8(2) . . . . ? C16 Ru2 C11 C12 129.8(3) . . . . ? C14 Ru2 C11 C12 65.04(19) . . . . ? S1 Ru2 C11 C12 -106.78(17) . . . . ? S3 Ru2 C11 C12 178.44(14) . . . . ? S2 Ru2 C11 C12 -36.4(3) . . . . ? C13 Ru2 C11 C17 140.0(3) . . . . ? C15 Ru2 C11 C17 -147.1(3) . . . . ? C12 Ru2 C11 C17 112.1(3) . . . . ? C16 Ru2 C11 C17 -118.1(4) . . . . ? C14 Ru2 C11 C17 177.1(3) . . . . ? S1 Ru2 C11 C17 5.3(3) . . . . ? S3 Ru2 C11 C17 -69.5(3) . . . . ? S2 Ru2 C11 C17 75.7(3) . . . . ? C16 C11 C12 C13 3.2(4) . . . . ? C17 C11 C12 C13 -176.2(3) . . . . ? Ru2 C11 C12 C13 -52.6(3) . . . . ? C16 C11 C12 Ru2 55.8(2) . . . . ? C17 C11 C12 Ru2 -123.5(3) . . . . ? C15 Ru2 C12 C13 65.98(19) . . . . ? C11 Ru2 C12 C13 133.7(3) . . . . ? C16 Ru2 C12 C13 103.5(2) . . . . ? C14 Ru2 C12 C13 29.03(18) . . . . ? S1 Ru2 C12 C13 -147.07(16) . . . . ? S3 Ru2 C12 C13 127.9(4) . . . . ? S2 Ru2 C12 C13 -66.26(19) . . . . ? C13 Ru2 C12 C11 -133.7(3) . . . . ? C15 Ru2 C12 C11 -67.70(18) . . . . ? C16 Ru2 C12 C11 -30.16(17) . . . . ? C14 Ru2 C12 C11 -104.65(19) . . . . ? S1 Ru2 C12 C11 79.25(17) . . . . ? S3 Ru2 C12 C11 -5.8(5) . . . . ? S2 Ru2 C12 C11 160.06(15) . . . . ? C11 C12 C13 C14 -2.2(4) . . . . ? Ru2 C12 C13 C14 -54.9(2) . . . . ? C11 C12 C13 Ru2 52.7(2) . . . . ? C15 Ru2 C13 C12 -102.7(2) . . . . ? C11 Ru2 C13 C12 -28.75(18) . . . . ? C16 Ru2 C13 C12 -65.56(19) . . . . ? C14 Ru2 C13 C12 -133.1(3) . . . . ? S1 Ru2 C13 C12 46.0(2) . . . . ? S3 Ru2 C13 C12 -161.48(15) . . . . ? S2 Ru2 C13 C12 122.87(17) . . . . ? C15 Ru2 C13 C14 30.34(17) . . . . ? C12 Ru2 C13 C14 133.1(3) . . . . ? C11 Ru2 C13 C14 104.32(19) . . . . ? C16 Ru2 C13 C14 67.51(18) . . . . ? S1 Ru2 C13 C14 179.08(13) . . . . ? S3 Ru2 C13 C14 -28.4(3) . . . . ? S2 Ru2 C13 C14 -104.07(16) . . . . ? C12 C13 C14 C15 0.2(4) . . . . ? Ru2 C13 C14 C15 -54.7(2) . . . . ? C12 C13 C14 C20 178.4(3) . . . . ? Ru2 C13 C14 C20 123.6(3) . . . . ? C12 C13 C14 Ru2 54.8(3) . . . . ? C13 Ru2 C14 C15 129.5(3) . . . . ? C12 Ru2 C14 C15 101.1(2) . . . . ? C11 Ru2 C14 C15 63.96(18) . . . . ? C16 Ru2 C14 C15 27.99(17) . . . . ? S1 Ru2 C14 C15 125.3(5) . . . . ? S3 Ru2 C14 C15 -66.00(18) . . . . ? S2 Ru2 C14 C15 -147.95(16) . . . . ? C15 Ru2 C14 C13 -129.5(3) . . . . ? C12 Ru2 C14 C13 -28.33(18) . . . . ? C11 Ru2 C14 C13 -65.51(18) . . . . ? C16 Ru2 C14 C13 -101.48(19) . . . . ? S1 Ru2 C14 C13 -4.2(6) . . . . ? S3 Ru2 C14 C13 164.54(15) . . . . ? S2 Ru2 C14 C13 82.59(17) . . . . ? C13 Ru2 C14 C20 -115.1(4) . . . . ? C15 Ru2 C14 C20 115.5(4) . . . . ? C12 Ru2 C14 C20 -143.4(3) . . . . ? C11 Ru2 C14 C20 179.4(3) . . . . ? C16 Ru2 C14 C20 143.5(3) . . . . ? S1 Ru2 C14 C20 -119.2(5) . . . . ? S3 Ru2 C14 C20 49.5(3) . . . . ? S2 Ru2 C14 C20 -32.5(3) . . . . ? C13 C14 C15 C16 0.8(4) . . . . ? C20 C14 C15 C16 -177.5(3) . . . . ? Ru2 C14 C15 C16 -53.4(2) . . . . ? C13 C14 C15 Ru2 54.2(2) . . . . ? C20 C14 C15 Ru2 -124.1(3) . . . . ? C13 Ru2 C15 C14 -31.13(18) . . . . ? C12 Ru2 C15 C14 -67.87(19) . . . . ? C11 Ru2 C15 C14 -106.0(2) . . . . ? C16 Ru2 C15 C14 -134.6(3) . . . . ? S1 Ru2 C15 C14 -165.72(14) . . . . ? S3 Ru2 C15 C14 122.68(17) . . . . ? S2 Ru2 C15 C14 44.8(2) . . . . ? C13 Ru2 C15 C16 103.46(19) . . . . ? C12 Ru2 C15 C16 66.71(18) . . . . ? C11 Ru2 C15 C16 28.54(17) . . . . ? C14 Ru2 C15 C16 134.6(3) . . . . ? S1 Ru2 C15 C16 -31.1(3) . . . . ? S3 Ru2 C15 C16 -102.73(16) . . . . ? S2 Ru2 C15 C16 179.41(13) . . . . ? C12 C11 C16 C15 -2.3(4) . . . . ? C17 C11 C16 C15 177.1(3) . . . . ? Ru2 C11 C16 C15 53.1(2) . . . . ? C12 C11 C16 Ru2 -55.4(2) . . . . ? C17 C11 C16 Ru2 124.0(3) . . . . ? C14 C15 C16 C11 0.3(4) . . . . ? Ru2 C15 C16 C11 -53.4(2) . . . . ? C14 C15 C16 Ru2 53.7(2) . . . . ? C13 Ru2 C16 C11 67.52(19) . . . . ? C15 Ru2 C16 C11 132.8(3) . . . . ? C12 Ru2 C16 C11 31.01(18) . . . . ? C14 Ru2 C16 C11 105.3(2) . . . . ? S1 Ru2 C16 C11 -64.64(18) . . . . ? S3 Ru2 C16 C11 -143.99(16) . . . . ? S2 Ru2 C16 C11 130.2(4) . . . . ? C13 Ru2 C16 C15 -65.32(18) . . . . ? C12 Ru2 C16 C15 -101.83(19) . . . . ? C11 Ru2 C16 C15 -132.8(3) . . . . ? C14 Ru2 C16 C15 -27.50(17) . . . . ? S1 Ru2 C16 C15 162.53(14) . . . . ? S3 Ru2 C16 C15 83.17(16) . . . . ? S2 Ru2 C16 C15 -2.6(6) . . . . ? C16 C11 C17 C18 -21.0(4) . . . . ? C12 C11 C17 C18 158.3(3) . . . . ? Ru2 C11 C17 C18 70.9(4) . . . . ? C16 C11 C17 C19 103.4(4) . . . . ? C12 C11 C17 C19 -77.2(4) . . . . ? Ru2 C11 C17 C19 -164.6(3) . . . . ? Ru2 S1 C21 C26 14.3(3) . . . . ? Ru1 S1 C21 C26 -85.6(3) . . . . ? Ru2 S1 C21 C22 -165.5(2) . . . . ? Ru1 S1 C21 C22 94.6(2) . . . . ? C26 C21 C22 C23 1.3(5) . . . . ? S1 C21 C22 C23 -178.9(3) . . . . ? C26 C21 C22 C27 177.3(3) . . . . ? S1 C21 C22 C27 -2.9(4) . . . . ? C21 C22 C23 C24 -1.0(5) . . . . ? C27 C22 C23 C24 -177.0(3) . . . . ? C22 C23 C24 C25 0.3(6) . . . . ? C23 C24 C25 C26 0.0(6) . . . . ? C22 C21 C26 C25 -1.0(5) . . . . ? S1 C21 C26 C25 179.2(3) . . . . ? C24 C25 C26 C21 0.4(6) . . . . ? C28 N1 C27 O1 9.0(5) . . . . ? C28 N1 C27 C22 -172.3(3) . . . . ? C23 C22 C27 O1 72.4(4) . . . . ? C21 C22 C27 O1 -103.5(4) . . . . ? C23 C22 C27 N1 -106.3(3) . . . . ? C21 C22 C27 N1 77.7(4) . . . . ? C27 N1 C28 C33 -178.4(3) . . . . ? C27 N1 C28 C29 3.4(5) . . . . ? C33 C28 C29 C30 -0.1(5) . . . . ? N1 C28 C29 C30 178.0(3) . . . . ? C28 C29 C30 C31 0.9(5) . . . . ? C29 C30 C31 C32 -0.6(6) . . . . ? C30 C31 C32 C33 -0.5(6) . . . . ? C31 C32 C33 C28 1.3(5) . . . . ? C29 C28 C33 C32 -0.9(5) . . . . ? N1 C28 C33 C32 -179.2(3) . . . . ? Ru1 S2 C34 C39 -23.7(3) . . . . ? Ru2 S2 C34 C39 74.1(3) . . . . ? Ru1 S2 C34 C35 155.3(2) . . . . ? Ru2 S2 C34 C35 -106.9(2) . . . . ? C39 C34 C35 C36 -0.8(4) . . . . ? S2 C34 C35 C36 -179.8(2) . . . . ? C39 C34 C35 C40 -176.7(3) . . . . ? S2 C34 C35 C40 4.3(4) . . . . ? C34 C35 C36 C37 -0.9(5) . . . . ? C40 C35 C36 C37 175.1(3) . . . . ? C35 C36 C37 C38 1.4(5) . . . . ? C36 C37 C38 C39 -0.3(5) . . . . ? C37 C38 C39 C34 -1.4(5) . . . . ? C35 C34 C39 C38 1.9(4) . . . . ? S2 C34 C39 C38 -179.1(2) . . . . ? C41' N2 C40 O2 4.4(12) . . . . ? C41 N2 C40 O2 -1.9(8) . . . . ? C41' N2 C40 C35 -172.9(11) . . . . ? C41 N2 C40 C35 -179.1(6) . . . . ? C36 C35 C40 O2 -90.3(4) . . . . ? C34 C35 C40 O2 85.6(4) . . . . ? C36 C35 C40 N2 87.0(4) . . . . ? C34 C35 C40 N2 -97.1(4) . . . . ? C40 N2 C41 C46 6.5(14) . . . . ? C41' N2 C41 C46 -153(5) . . . . ? C40 N2 C41 C42 -175.8(5) . . . . ? C41' N2 C41 C42 25(4) . . . . ? C46 C41 C42 C43 -1.3(9) . . . . ? N2 C41 C42 C43 -179.2(9) . . . . ? C41 C42 C43 C44 -1.4(9) . . . . ? C42 C43 C44 C45 2.8(15) . . . . ? C43 C44 C45 C46 -1.5(17) . . . . ? C42 C41 C46 C45 2.6(15) . . . . ? N2 C41 C46 C45 -179.8(10) . . . . ? C44 C45 C46 C41 -1.2(17) . . . . ? C40 N2 C41' C46' 36(2) . . . . ? C41 N2 C41' C46' 60(3) . . . . ? C40 N2 C41' C42' -142.4(11) . . . . ? C41 N2 C41' C42' -118(6) . . . . ? C46' C41' C42' C43' -1(3) . . . . ? N2 C41' C42' C43' 177.0(14) . . . . ? C41' C42' C43' C44' 4(2) . . . . ? C42' C43' C44' C45' -6(2) . . . . ? C43' C44' C45' C46' 6(2) . . . . ? C42' C41' C46' C45' 0(3) . . . . ? N2 C41' C46' C45' -178.2(13) . . . . ? C44' C45' C46' C41' -2(2) . . . . ? Ru1 S3 C47 C52 -6.8(3) . . . . ? Ru2 S3 C47 C52 89.6(2) . . . . ? Ru1 S3 C47 C48 176.7(2) . . . . ? Ru2 S3 C47 C48 -86.9(2) . . . . ? C52 C47 C48 C49 -4.2(4) . . . . ? S3 C47 C48 C49 172.2(2) . . . . ? C52 C47 C48 C53 178.8(3) . . . . ? S3 C47 C48 C53 -4.7(4) . . . . ? C47 C48 C49 C50 2.8(5) . . . . ? C53 C48 C49 C50 -179.8(3) . . . . ? C48 C49 C50 C51 1.0(5) . . . . ? C49 C50 C51 C52 -3.2(5) . . . . ? C50 C51 C52 C47 1.6(5) . . . . ? C48 C47 C52 C51 2.1(4) . . . . ? S3 C47 C52 C51 -174.4(2) . . . . ? C54 N3 C53 O3 -12.3(5) . . . . ? C54 N3 C53 C48 169.0(3) . . . . ? C49 C48 C53 O3 -24.5(4) . . . . ? C47 C48 C53 O3 152.6(3) . . . . ? C49 C48 C53 N3 154.2(3) . . . . ? C47 C48 C53 N3 -28.7(5) . . . . ? C53 N3 C54 C55 177.7(3) . . . . ? C53 N3 C54 C59 -5.0(5) . . . . ? C59 C54 C55 C56 -0.3(5) . . . . ? N3 C54 C55 C56 177.2(3) . . . . ? C54 C55 C56 C57 -0.2(6) . . . . ? C55 C56 C57 C58 0.1(6) . . . . ? C56 C57 C58 C59 0.5(6) . . . . ? C57 C58 C59 C54 -1.0(6) . . . . ? C55 C54 C59 C58 0.9(5) . . . . ? N3 C54 C59 C58 -176.4(3) . . . . ? 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 O4 H1O4 O5 0.84 1.88 2.703(4) 164.6 . O5 H1O5 O6 0.84 1.86 2.698(5) 172.5 2_854 O6 H1O6 O4 0.84 2.01 2.818(4) 162.8 . N1 H1 O4 0.88 2.17 2.993(4) 156.2 . N2 H2 F6 0.88 2.12 2.955(4) 158.0 . N3 H3 S3 0.88 2.51 3.031(3) 118.3 . N3 H3 F5 0.88 2.51 3.319(4) 153.2 2_765 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.733 _refine_diff_density_min -0.800 _refine_diff_density_rms 0.104