data_global _journal_name_full Org.Biomol.Chem. _journal_coden_cambridge 0177 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email guy.clarkson@warwick.ac.uk _publ_contact_author_name 'Guy J. Clarkson' loop_ _publ_author_name 'Rina Soni' 'Fung Kei Cheung' 'Guy J. Clarkson' 'Jose E. D.Martins' 'Mark A. Graham' ; M.Wills ; data_rs3 _database_code_depnum_ccdc_archive 'CCDC 793888' #TrackingRef '2482_web_deposit_cif_file_0_GuyClarkson_1284659941.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C31 H33 Cl N2 O2 Ru S' _chemical_formula_weight 634.17 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru 0.0552 3.2960 '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 8.39707(8) _cell_length_b 9.14896(9) _cell_length_c 35.0858(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2695.44(4) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 7176 _cell_measurement_theta_min 3.7710 _cell_measurement_theta_max 61.7737 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.2108 _exptl_crystal_size_mid 0.1391 _exptl_crystal_size_min 0.0319 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist _exptl_oxdiff_crystal_face_indexfrac_h _exptl_oxdiff_crystal_face_indexfrac_k _exptl_oxdiff_crystal_face_indexfrac_l _exptl_oxdiff_crystal_face_x _exptl_oxdiff_crystal_face_y _exptl_oxdiff_crystal_face_z -5 0 -2 0.0150 -5.0015 0.0014 -1.9695 -0.6534 0.0966 0.6429 5 0 2 0.0169 5.0015 -0.0014 1.9695 0.6534 -0.0966 -0.6429 1 -6 1 0.0980 1.0046 -5.9992 0.9895 0.6949 0.6791 0.3356 1 6 -5 0.0910 0.9943 5.9979 -4.9997 -0.3599 -0.8694 -0.4664 -1 0 -23 0.0626 -1.0082 -0.0031 -22.9847 0.2161 -0.6946 0.7238 1 0 23 0.0626 1.0082 0.0031 22.9847 -0.2161 0.6946 -0.7238 -2 4 14 0.1048 -1.9982 4.0021 14.0089 -0.8708 0.0532 -0.4526 _exptl_absorpt_coefficient_mu 6.436 _exptl_absorpt_correction_T_min 0.319 _exptl_absorpt_correction_T_max 0.818 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET) (compiled Nov 6 2009,16:24:50) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.563 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1304 _exptl_special_details ; Very weakly diffracting poor quality crystals. Mounted with inert oil. The temperature of the crystal was controlled using the Oxford Cryosystem Cryostream Cobra. The data collection nominally covered over a hemisphere of Reciprocal space, by a combination of four sets of exposures with different \f angles for the crystal; each 150 s exposure covered 0.75\% in \w. The crystal-to-detector distance was 5.5 cm. Crystal decay was found to be negligible by by repeating the initial frames at the end of data collection and analyzing the duplicate reflections. Hydrogen atoms were added at calculated positions and refined using a riding model. Anisotropic displacement parameters were used for all non-H atoms; H-atoms were given isotropic displacement parameter equal to 1.2 (or 1.5 for methyl H-atoms) times the equivalent isotropic displacement parameter of the atom to which they are attached. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Gemini R' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean 10.2833 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% nil _diffrn_reflns_number 8126 _diffrn_reflns_av_R_equivalents 0.0204 _diffrn_reflns_av_sigmaI/netI 0.0198 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -38 _diffrn_reflns_limit_l_max 39 _diffrn_reflns_theta_min 5.00 _diffrn_reflns_theta_max 61.84 _reflns_number_total 4144 _reflns_number_gt 4038 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1997)' _computing_publication_material 'SHELXTL (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^)+(0.0594P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881, 1717 Friedel pairs' _refine_ls_abs_structure_Flack 0.005(7) _chemical_absolute_configuration rmad _refine_ls_number_reflns 4144 _refine_ls_number_parameters 345 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0299 _refine_ls_R_factor_gt 0.0292 _refine_ls_wR_factor_ref 0.0745 _refine_ls_wR_factor_gt 0.0742 _refine_ls_goodness_of_fit_ref 1.096 _refine_ls_restrained_S_all 1.096 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.50483(3) 0.47841(2) 0.157026(6) 0.01663(10) Uani 1 1 d . . . Cl1 Cl 0.78812(9) 0.51674(9) 0.16767(2) 0.01953(18) Uani 1 1 d . . . C1 C 1.1405(4) -0.0670(4) 0.23007(10) 0.0250(8) Uani 1 1 d . . . H1A H 1.1713 -0.1660 0.2224 0.037 Uiso 1 1 calc R . . H1B H 1.1349 -0.0616 0.2579 0.037 Uiso 1 1 calc R . . H1C H 1.2198 0.0030 0.2207 0.037 Uiso 1 1 calc R . . C2 C 0.9805(4) -0.0307(3) 0.21343(9) 0.0210(7) Uani 1 1 d . . . C3 C 0.9017(4) -0.1247(4) 0.18857(9) 0.0216(7) Uani 1 1 d . . . H3A H 0.9462 -0.2181 0.1834 0.026 Uiso 1 1 calc R . . C4 C 0.7602(4) -0.0853(4) 0.17122(9) 0.0209(7) Uani 1 1 d . . . H4A H 0.7090 -0.1507 0.1541 0.025 Uiso 1 1 calc R . . C5 C 0.6935(4) 0.0500(4) 0.17892(9) 0.0191(7) Uani 1 1 d . . . C6 C 0.7670(4) 0.1448(4) 0.20486(9) 0.0219(7) Uani 1 1 d . . . H6A H 0.7196 0.2360 0.2110 0.026 Uiso 1 1 calc R . . C7 C 0.9088(4) 0.1038(4) 0.22127(9) 0.0220(7) Uani 1 1 d . . . H7A H 0.9597 0.1690 0.2385 0.026 Uiso 1 1 calc R . . O8B O 0.4830(3) 0.0023(2) 0.12614(6) 0.0216(5) Uani 1 1 d . . . O8A O 0.4012(3) 0.1309(2) 0.18436(6) 0.0225(5) Uani 1 1 d . . . S8 S 0.51954(9) 0.11078(8) 0.15501(2) 0.01759(18) Uani 1 1 d . . . N9 N 0.5612(3) 0.2650(3) 0.13607(7) 0.0175(6) Uani 1 1 d . . . C10 C 0.6393(4) 0.2526(4) 0.09783(8) 0.0180(7) Uani 1 1 d . . . H10A H 0.5599 0.2119 0.0794 0.022 Uiso 1 1 calc R . . C11 C 0.7869(4) 0.1574(3) 0.09672(9) 0.0191(7) Uani 1 1 d . . . C12 C 0.7912(4) 0.0328(4) 0.07382(9) 0.0213(7) Uani 1 1 d . . . H12A H 0.7027 0.0107 0.0580 0.026 Uiso 1 1 calc R . . C13 C 0.9215(4) -0.0586(4) 0.07374(10) 0.0247(8) Uani 1 1 d . . . H13A H 0.9229 -0.1420 0.0576 0.030 Uiso 1 1 calc R . . C14 C 1.0497(4) -0.0292(4) 0.09698(10) 0.0246(8) Uani 1 1 d . . . H14A H 1.1381 -0.0941 0.0975 0.029 Uiso 1 1 calc R . . C15 C 1.0501(4) 0.0953(4) 0.11978(9) 0.0195(7) Uani 1 1 d . . . H15A H 1.1393 0.1163 0.1355 0.023 Uiso 1 1 calc R . . C16 C 0.9212(4) 0.1876(4) 0.11952(9) 0.0194(7) Uani 1 1 d . . . H16A H 0.9225 0.2731 0.1349 0.023 Uiso 1 1 calc R . . C17 C 0.6824(4) 0.4069(3) 0.08509(9) 0.0182(7) Uani 1 1 d . . . H17A H 0.7781 0.4353 0.1003 0.022 Uiso 1 1 calc R . . C18 C 0.7332(4) 0.4151(3) 0.04346(9) 0.0191(7) Uani 1 1 d . . . C19 C 0.6575(4) 0.3382(3) 0.01418(9) 0.0214(7) Uani 1 1 d . . . H19A H 0.5719 0.2741 0.0200 0.026 Uiso 1 1 calc R . . C20 C 0.7066(4) 0.3549(4) -0.02335(9) 0.0258(8) Uani 1 1 d . . . H20A H 0.6534 0.3029 -0.0430 0.031 Uiso 1 1 calc R . . C21 C 0.8318(4) 0.4463(4) -0.03244(10) 0.0286(8) Uani 1 1 d . . . H21A H 0.8638 0.4580 -0.0582 0.034 Uiso 1 1 calc R . . C22 C 0.9098(4) 0.5203(4) -0.00375(10) 0.0275(8) Uani 1 1 d . . . H22A H 0.9969 0.5826 -0.0097 0.033 Uiso 1 1 calc R . . C23 C 0.8611(4) 0.5040(3) 0.03398(9) 0.0234(7) Uani 1 1 d . . . H23A H 0.9164 0.5546 0.0536 0.028 Uiso 1 1 calc R . . N24 N 0.5516(3) 0.5158(3) 0.09592(7) 0.0182(6) Uani 1 1 d . . . C25 C 0.6145(4) 0.6663(3) 0.08880(9) 0.0205(7) Uani 1 1 d . . . H25A H 0.6305 0.6804 0.0614 0.031 Uiso 1 1 calc R . . H25B H 0.7163 0.6785 0.1021 0.031 Uiso 1 1 calc R . . H25C H 0.5380 0.7386 0.0983 0.031 Uiso 1 1 calc R . . C26 C 0.4056(4) 0.4904(4) 0.07236(8) 0.0202(7) Uani 1 1 d . . . H26A H 0.3693 0.3888 0.0767 0.024 Uiso 1 1 calc R . . H26B H 0.4354 0.4987 0.0452 0.024 Uiso 1 1 calc R . . C27 C 0.2657(4) 0.5930(4) 0.07987(9) 0.0223(7) Uani 1 1 d . . . H27A H 0.1952 0.5923 0.0573 0.027 Uiso 1 1 calc R . . H27B H 0.3074 0.6936 0.0828 0.027 Uiso 1 1 calc R . . C28 C 0.1655(4) 0.5551(4) 0.11530(9) 0.0232(7) Uani 1 1 d . . . H28A H 0.0789 0.6280 0.1178 0.028 Uiso 1 1 calc R . . H28B H 0.1155 0.4583 0.1114 0.028 Uiso 1 1 calc R . . C29 C 0.2591(4) 0.5519(4) 0.15169(9) 0.0201(7) Uani 1 1 d . . . C30 C 0.3565(4) 0.6753(4) 0.16228(10) 0.0214(7) Uani 1 1 d . . . H30A H 0.3714 0.7569 0.1437 0.026 Uiso 1 1 calc R . . C31 C 0.4570(4) 0.6671(4) 0.19436(9) 0.0227(8) Uani 1 1 d . . . H31A H 0.5416 0.7428 0.1978 0.027 Uiso 1 1 calc R . . C32 C 0.4610(4) 0.5388(4) 0.21736(9) 0.0244(8) Uani 1 1 d . . . H32A H 0.5476 0.5260 0.2367 0.029 Uiso 1 1 calc R . . C33 C 0.3613(4) 0.4199(4) 0.20818(9) 0.0232(7) Uani 1 1 d . . . H33A H 0.3791 0.3235 0.2209 0.028 Uiso 1 1 calc R . . C34 C 0.2618(4) 0.4274(4) 0.17494(9) 0.0213(7) Uani 1 1 d . . . H34A H 0.2110 0.3356 0.1654 0.026 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 0.01948(15) 0.01561(15) 0.01480(14) -0.00090(8) 0.00187(10) -0.00039(12) Cl1 0.0220(4) 0.0207(4) 0.0159(3) -0.0023(3) -0.0006(3) -0.0020(3) C1 0.0253(19) 0.0250(18) 0.0247(18) 0.0052(15) -0.0001(14) -0.0025(15) C2 0.0246(17) 0.0215(16) 0.0169(15) 0.0047(12) 0.0026(13) -0.0009(17) C3 0.0307(19) 0.0158(16) 0.0182(16) 0.0039(13) 0.0032(14) 0.0014(15) C4 0.0283(19) 0.0165(16) 0.0178(16) 0.0008(13) -0.0007(14) -0.0036(15) C5 0.0237(17) 0.0200(17) 0.0134(15) 0.0038(13) -0.0005(13) -0.0035(14) C6 0.034(2) 0.0165(15) 0.0156(16) -0.0007(13) 0.0002(14) 0.0001(15) C7 0.0250(18) 0.0219(18) 0.0191(17) -0.0021(13) -0.0035(15) -0.0030(15) O8B 0.0257(12) 0.0175(10) 0.0216(11) -0.0015(8) -0.0046(9) -0.0029(11) O8A 0.0261(13) 0.0209(12) 0.0206(12) 0.0025(10) 0.0050(10) -0.0012(10) S8 0.0195(4) 0.0156(4) 0.0177(4) 0.0013(3) 0.0003(4) -0.0016(3) N9 0.0197(13) 0.0176(14) 0.0153(12) 0.0013(11) 0.0024(10) 0.0000(11) C10 0.0229(17) 0.0199(16) 0.0112(15) -0.0017(13) 0.0023(12) -0.0017(14) C11 0.0224(16) 0.0166(16) 0.0182(16) 0.0046(13) 0.0024(13) -0.0013(14) C12 0.0258(17) 0.0208(16) 0.0174(16) 0.0003(13) 0.0022(13) -0.0034(15) C13 0.035(2) 0.0183(17) 0.0206(18) -0.0009(14) 0.0067(15) 0.0009(16) C14 0.0275(17) 0.0171(16) 0.0291(18) 0.0083(15) 0.0069(14) 0.0073(14) C15 0.0192(17) 0.0206(17) 0.0188(16) 0.0051(13) 0.0008(13) -0.0017(13) C16 0.0244(17) 0.0182(16) 0.0157(15) 0.0029(13) 0.0025(13) -0.0061(15) C17 0.0201(18) 0.0180(16) 0.0165(16) -0.0014(13) -0.0015(13) -0.0007(14) C18 0.0237(17) 0.0181(15) 0.0154(15) 0.0004(13) -0.0013(13) 0.0063(14) C19 0.0303(19) 0.0177(16) 0.0160(16) -0.0006(13) -0.0021(14) 0.0032(14) C20 0.0293(19) 0.0306(18) 0.0173(17) -0.0022(15) -0.0015(14) 0.0096(16) C21 0.0310(19) 0.038(2) 0.0172(17) 0.0016(16) 0.0038(15) 0.0117(17) C22 0.0236(17) 0.033(2) 0.0263(18) 0.0068(16) 0.0068(14) 0.0024(17) C23 0.0258(18) 0.0221(18) 0.0222(16) 0.0005(15) 0.0026(14) 0.0052(16) N24 0.0192(13) 0.0171(13) 0.0183(13) -0.0021(11) -0.0003(10) 0.0009(11) C25 0.0275(18) 0.0154(16) 0.0187(17) 0.0010(12) 0.0031(14) -0.0013(14) C26 0.0223(16) 0.0223(17) 0.0159(15) -0.0027(14) -0.0015(13) -0.0024(15) C27 0.0194(18) 0.0250(17) 0.0226(17) 0.0038(14) 0.0009(14) 0.0031(14) C28 0.0216(17) 0.0248(18) 0.0231(18) -0.0006(14) 0.0018(14) 0.0011(15) C29 0.0173(16) 0.0208(17) 0.0223(16) 0.0004(14) 0.0082(13) 0.0059(14) C30 0.0222(17) 0.0165(16) 0.0254(18) -0.0016(13) 0.0098(14) 0.0049(14) C31 0.0227(19) 0.0227(17) 0.0227(17) -0.0049(13) 0.0086(13) -0.0009(13) C32 0.0261(18) 0.0282(19) 0.0190(16) -0.0047(14) 0.0052(13) -0.0011(15) C33 0.0240(19) 0.0269(18) 0.0188(17) -0.0010(14) 0.0069(14) 0.0017(15) C34 0.0159(16) 0.0251(17) 0.0229(17) -0.0032(14) 0.0085(14) -0.0026(14) _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 N9 2.139(3) . ? Ru1 C29 2.178(3) . ? Ru1 C34 2.186(3) . ? Ru1 C30 2.197(3) . ? Ru1 C31 2.204(3) . ? Ru1 N24 2.206(3) . ? Ru1 C32 2.218(3) . ? Ru1 C33 2.227(3) . ? Ru1 Cl1 2.4333(8) . ? C1 C2 1.502(5) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C3 1.392(5) . ? C2 C7 1.398(5) . ? C3 C4 1.383(5) . ? C3 H3A 0.9500 . ? C4 C5 1.385(5) . ? C4 H4A 0.9500 . ? C5 C6 1.401(4) . ? C5 S8 1.774(3) . ? C6 C7 1.375(5) . ? C6 H6A 0.9500 . ? C7 H7A 0.9500 . ? O8B S8 1.451(2) . ? O8A S8 1.443(2) . ? S8 N9 1.598(3) . ? N9 C10 1.498(4) . ? C10 C11 1.515(5) . ? C10 C17 1.524(4) . ? C10 H10A 1.0000 . ? C11 C12 1.395(5) . ? C11 C16 1.410(5) . ? C12 C13 1.377(5) . ? C12 H12A 0.9500 . ? C13 C14 1.377(5) . ? C13 H13A 0.9500 . ? C14 C15 1.392(5) . ? C14 H14A 0.9500 . ? C15 C16 1.373(5) . ? C15 H15A 0.9500 . ? C16 H16A 0.9500 . ? C17 C18 1.524(4) . ? C17 N24 1.531(4) . ? C17 H17A 1.0000 . ? C18 C23 1.388(5) . ? C18 C19 1.398(5) . ? C19 C20 1.388(5) . ? C19 H19A 0.9500 . ? C20 C21 1.380(5) . ? C20 H20A 0.9500 . ? C21 C22 1.379(5) . ? C21 H21A 0.9500 . ? C22 C23 1.394(5) . ? C22 H22A 0.9500 . ? C23 H23A 0.9500 . ? N24 C25 1.495(4) . ? N24 C26 1.496(4) . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 C27 1.527(4) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 C28 1.541(4) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 C29 1.500(5) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 C34 1.401(5) . ? C29 C30 1.443(5) . ? C30 C31 1.409(5) . ? C30 H30A 1.0000 . ? C31 C32 1.425(5) . ? C31 H31A 1.0000 . ? C32 C33 1.409(5) . ? C32 H32A 1.0000 . ? C33 C34 1.436(5) . ? C33 H33A 1.0000 . ? C34 H34A 1.0000 . ? 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 N9 Ru1 C29 117.49(11) . . ? N9 Ru1 C34 96.35(11) . . ? C29 Ru1 C34 37.45(13) . . ? N9 Ru1 C30 154.44(11) . . ? C29 Ru1 C30 38.50(12) . . ? C34 Ru1 C30 67.77(12) . . ? N9 Ru1 C31 163.62(11) . . ? C29 Ru1 C31 68.70(12) . . ? C34 Ru1 C31 79.98(12) . . ? C30 Ru1 C31 37.34(13) . . ? N9 Ru1 N24 76.60(10) . . ? C29 Ru1 N24 92.12(11) . . ? C34 Ru1 N24 118.60(11) . . ? C30 Ru1 N24 93.16(11) . . ? C31 Ru1 N24 119.25(11) . . ? N9 Ru1 C32 126.28(11) . . ? C29 Ru1 C32 81.27(12) . . ? C34 Ru1 C32 67.91(12) . . ? C30 Ru1 C32 67.80(13) . . ? C31 Ru1 C32 37.59(13) . . ? N24 Ru1 C32 156.66(12) . . ? N9 Ru1 C33 100.22(11) . . ? C29 Ru1 C33 68.33(13) . . ? C34 Ru1 C33 37.98(13) . . ? C30 Ru1 C33 79.78(13) . . ? C31 Ru1 C33 67.07(12) . . ? N24 Ru1 C33 156.44(11) . . ? C32 Ru1 C33 36.97(12) . . ? N9 Ru1 Cl1 88.17(7) . . ? C29 Ru1 Cl1 153.48(9) . . ? C34 Ru1 Cl1 154.08(9) . . ? C30 Ru1 Cl1 115.03(9) . . ? C31 Ru1 Cl1 88.52(9) . . ? N24 Ru1 Cl1 87.30(7) . . ? C32 Ru1 Cl1 88.84(9) . . ? C33 Ru1 Cl1 116.10(9) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C3 C2 C7 117.6(3) . . ? C3 C2 C1 122.2(3) . . ? C7 C2 C1 120.2(3) . . ? C4 C3 C2 121.5(3) . . ? C4 C3 H3A 119.2 . . ? C2 C3 H3A 119.2 . . ? C3 C4 C5 119.6(3) . . ? C3 C4 H4A 120.2 . . ? C5 C4 H4A 120.2 . . ? C4 C5 C6 120.1(3) . . ? C4 C5 S8 121.4(2) . . ? C6 C5 S8 118.4(3) . . ? C7 C6 C5 119.0(3) . . ? C7 C6 H6A 120.5 . . ? C5 C6 H6A 120.5 . . ? C6 C7 C2 122.1(3) . . ? C6 C7 H7A 119.0 . . ? C2 C7 H7A 119.0 . . ? O8A S8 O8B 116.10(13) . . ? O8A S8 N9 109.54(13) . . ? O8B S8 N9 111.09(13) . . ? O8A S8 C5 105.64(14) . . ? O8B S8 C5 106.85(14) . . ? N9 S8 C5 107.06(14) . . ? C10 N9 S8 113.7(2) . . ? C10 N9 Ru1 118.3(2) . . ? S8 N9 Ru1 127.91(14) . . ? N9 C10 C11 115.1(2) . . ? N9 C10 C17 107.2(3) . . ? C11 C10 C17 109.3(3) . . ? N9 C10 H10A 108.3 . . ? C11 C10 H10A 108.3 . . ? C17 C10 H10A 108.3 . . ? C12 C11 C16 117.8(3) . . ? C12 C11 C10 120.4(3) . . ? C16 C11 C10 121.8(3) . . ? C13 C12 C11 121.2(3) . . ? C13 C12 H12A 119.4 . . ? C11 C12 H12A 119.4 . . ? C12 C13 C14 120.1(3) . . ? C12 C13 H13A 119.9 . . ? C14 C13 H13A 119.9 . . ? C13 C14 C15 120.1(3) . . ? C13 C14 H14A 120.0 . . ? C15 C14 H14A 120.0 . . ? C16 C15 C14 119.9(3) . . ? C16 C15 H15A 120.1 . . ? C14 C15 H15A 120.1 . . ? C15 C16 C11 120.9(3) . . ? C15 C16 H16A 119.6 . . ? C11 C16 H16A 119.6 . . ? C18 C17 C10 113.2(3) . . ? C18 C17 N24 114.0(3) . . ? C10 C17 N24 111.1(3) . . ? C18 C17 H17A 105.9 . . ? C10 C17 H17A 105.9 . . ? N24 C17 H17A 105.9 . . ? C23 C18 C19 118.1(3) . . ? C23 C18 C17 118.4(3) . . ? C19 C18 C17 123.5(3) . . ? C20 C19 C18 120.5(3) . . ? C20 C19 H19A 119.8 . . ? C18 C19 H19A 119.8 . . ? C21 C20 C19 120.8(3) . . ? C21 C20 H20A 119.6 . . ? C19 C20 H20A 119.6 . . ? C22 C21 C20 119.4(3) . . ? C22 C21 H21A 120.3 . . ? C20 C21 H21A 120.3 . . ? C21 C22 C23 120.1(3) . . ? C21 C22 H22A 120.0 . . ? C23 C22 H22A 120.0 . . ? C18 C23 C22 121.2(3) . . ? C18 C23 H23A 119.4 . . ? C22 C23 H23A 119.4 . . ? C25 N24 C26 109.9(2) . . ? C25 N24 C17 107.7(2) . . ? C26 N24 C17 110.4(2) . . ? C25 N24 Ru1 111.59(19) . . ? C26 N24 Ru1 111.53(19) . . ? C17 N24 Ru1 105.53(18) . . ? N24 C25 H25A 109.5 . . ? N24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? N24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? N24 C26 C27 116.0(3) . . ? N24 C26 H26A 108.3 . . ? C27 C26 H26A 108.3 . . ? N24 C26 H26B 108.3 . . ? C27 C26 H26B 108.3 . . ? H26A C26 H26B 107.4 . . ? C26 C27 C28 114.9(3) . . ? C26 C27 H27A 108.5 . . ? C28 C27 H27A 108.5 . . ? C26 C27 H27B 108.5 . . ? C28 C27 H27B 108.5 . . ? H27A C27 H27B 107.5 . . ? C29 C28 C27 113.9(3) . . ? C29 C28 H28A 108.8 . . ? C27 C28 H28A 108.8 . . ? C29 C28 H28B 108.8 . . ? C27 C28 H28B 108.8 . . ? H28A C28 H28B 107.7 . . ? C34 C29 C30 118.5(3) . . ? C34 C29 C28 121.3(3) . . ? C30 C29 C28 120.1(3) . . ? C34 C29 Ru1 71.57(18) . . ? C30 C29 Ru1 71.46(18) . . ? C28 C29 Ru1 125.2(2) . . ? C31 C30 C29 120.2(3) . . ? C31 C30 Ru1 71.58(19) . . ? C29 C30 Ru1 70.04(18) . . ? C31 C30 H30A 119.1 . . ? C29 C30 H30A 119.1 . . ? Ru1 C30 H30A 119.1 . . ? C30 C31 C32 120.7(3) . . ? C30 C31 Ru1 71.08(18) . . ? C32 C31 Ru1 71.76(19) . . ? C30 C31 H31A 119.0 . . ? C32 C31 H31A 119.0 . . ? Ru1 C31 H31A 119.0 . . ? C33 C32 C31 119.5(3) . . ? C33 C32 Ru1 71.85(18) . . ? C31 C32 Ru1 70.65(18) . . ? C33 C32 H32A 119.8 . . ? C31 C32 H32A 119.8 . . ? Ru1 C32 H32A 119.8 . . ? C32 C33 C34 119.6(3) . . ? C32 C33 Ru1 71.18(19) . . ? C34 C33 Ru1 69.47(18) . . ? C32 C33 H33A 119.4 . . ? C34 C33 H33A 119.4 . . ? Ru1 C33 H33A 119.4 . . ? C29 C34 C33 121.4(3) . . ? C29 C34 Ru1 70.98(18) . . ? C33 C34 Ru1 72.55(19) . . ? C29 C34 H34A 118.7 . . ? C33 C34 H34A 118.7 . . ? Ru1 C34 H34A 118.7 . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 61.84 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 1.312 _refine_diff_density_min -0.411 _refine_diff_density_rms 0.116 # Attachment '2483_web_deposit_cif_file_1_GuyClarkson_1284659941.cif' data_rs4 _database_code_depnum_ccdc_archive 'CCDC 793889' #TrackingRef '2483_web_deposit_cif_file_1_GuyClarkson_1284659941.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C31 H37 Cl N2 O3 Ru S' _chemical_formula_weight 654.21 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' 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 P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' _cell_length_a 10.3603(2) _cell_length_b 11.0519(3) _cell_length_c 14.0747(3) _cell_angle_alpha 90.6376(19) _cell_angle_beta 103.5283(17) _cell_angle_gamma 107.614(2) _cell_volume 1487.56(6) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 22067 _cell_measurement_theta_min 3.20 _cell_measurement_theta_max 29.28 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.461 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 676 _exptl_absorpt_coefficient_mu 0.721 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.93 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details 'ABSPACK(CrysAlis, Oxford Diffraction)' _exptl_special_details ; The temperature of the crystal was controlled using the Oxford Cryosystem Cryostream Cobra. The data collection nominally covered over a hemisphere of Reciprocal space, by a combination of four sets of exposures with different \f angles for the crystal; each 30 s exposure covered 1\% in \w. The crystal-to-detector distance was 5.5 cm. Crystal decay was found to be negligible by by repeating the initial frames at the end of data collection and analyzing the duplicate reflections. Hydrogen atoms were added at calculated positions and refined using a riding model except the hydrogens on the ethanols which were located in a difference map. Anisotropic displacement parameters were used for all non-H atoms; H-atoms were given isotropic displacement parameter equal to 1.2 (or 1.5 for methyl or OH H-atoms) times the equivalent isotropic displacement parameter of the atom to which they are attached. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Gemini R' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean 10.2833 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% nil _diffrn_reflns_number 26930 _diffrn_reflns_av_R_equivalents 0.0230 _diffrn_reflns_av_sigmaI/netI 0.0326 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.21 _diffrn_reflns_theta_max 29.34 _reflns_number_total 13849 _reflns_number_gt 13324 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1997)' _computing_publication_material 'SHELXTL (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^)+(0.0337P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881, 6538 Friedel pairs' _refine_ls_abs_structure_Flack 0.009(11) _chemical_absolute_configuration rmad _refine_ls_number_reflns 13849 _refine_ls_number_parameters 717 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0247 _refine_ls_R_factor_gt 0.0233 _refine_ls_wR_factor_ref 0.0553 _refine_ls_wR_factor_gt 0.0548 _refine_ls_goodness_of_fit_ref 1.004 _refine_ls_restrained_S_all 1.004 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.052360(13) 0.187633(12) 0.256855(10) 0.01401(4) Uani 1 1 d . . . Cl1 Cl 0.04297(5) 0.16975(5) 0.42658(4) 0.01727(10) Uani 1 1 d . . . Ru2 Ru 0.660853(13) 0.450284(12) 0.895958(10) 0.01350(4) Uani 1 1 d . . . Cl2 Cl 0.57796(5) 0.38881(5) 0.72084(4) 0.01763(10) Uani 1 1 d . . . C101 C -0.3017(3) -0.4255(3) 0.50651(17) 0.0302(6) Uani 1 1 d . . . H10A H -0.3174 -0.5169 0.4943 0.045 Uiso 1 1 calc R . . H10B H -0.3912 -0.4109 0.5038 0.045 Uiso 1 1 calc R . . H10C H -0.2386 -0.3946 0.5715 0.045 Uiso 1 1 calc R . . C102 C -0.2372(2) -0.3549(2) 0.42962(16) 0.0216(5) Uani 1 1 d . . . C103 C -0.1725(2) -0.4101(2) 0.37319(16) 0.0230(5) Uani 1 1 d . . . H10D H -0.1716 -0.4950 0.3818 0.028 Uiso 1 1 calc R . . C104 C -0.1085(2) -0.3424(2) 0.30377(16) 0.0203(4) Uani 1 1 d . . . H10E H -0.0650 -0.3810 0.2654 0.024 Uiso 1 1 calc R . . C105 C -0.1099(2) -0.2192(2) 0.29224(15) 0.0168(4) Uani 1 1 d . . . C106 C -0.1747(2) -0.1626(2) 0.34761(16) 0.0218(5) Uani 1 1 d . . . H10F H -0.1751 -0.0776 0.3391 0.026 Uiso 1 1 calc R . . C107 C -0.2383(2) -0.2302(2) 0.41478(16) 0.0224(5) Uani 1 1 d . . . H10G H -0.2835 -0.1916 0.4517 0.027 Uiso 1 1 calc R . . S108 S -0.03409(6) -0.12774(5) 0.20407(4) 0.01726(12) Uani 1 1 d . . . O18A O 0.03288(17) -0.20619(15) 0.16260(11) 0.0224(3) Uani 1 1 d . . . O18B O -0.14906(17) -0.10075(16) 0.13788(11) 0.0233(3) Uani 1 1 d . . . N109 N 0.0761(2) 0.00204(18) 0.25857(13) 0.0160(4) Uani 1 1 d . . . C110 C 0.2170(2) -0.0071(2) 0.30754(15) 0.0149(4) Uani 1 1 d . . . H11A H 0.2641 -0.0194 0.2554 0.018 Uiso 1 1 calc R . . C111 C 0.2159(2) -0.1142(2) 0.37415(17) 0.0170(5) Uani 1 1 d . . . C112 C 0.2664(3) -0.2128(2) 0.3516(2) 0.0263(6) Uani 1 1 d . . . H11B H 0.2994 -0.2131 0.2940 0.032 Uiso 1 1 calc R . . C113 C 0.2683(3) -0.3104(3) 0.4135(2) 0.0367(7) Uani 1 1 d . . . H11D H 0.3023 -0.3771 0.3982 0.044 Uiso 1 1 calc R . . C114 C 0.2205(3) -0.3096(3) 0.4970(2) 0.0381(8) Uani 1 1 d . . . H11E H 0.2223 -0.3759 0.5392 0.046 Uiso 1 1 calc R . . C115 C 0.1705(3) -0.2146(3) 0.51966(19) 0.0311(6) Uani 1 1 d . . . H11F H 0.1372 -0.2156 0.5771 0.037 Uiso 1 1 calc R . . C116 C 0.1684(2) -0.1172(2) 0.45924(16) 0.0214(5) Uani 1 1 d . . . H11G H 0.1341 -0.0514 0.4759 0.026 Uiso 1 1 calc R . . C117 C 0.3016(2) 0.12001(19) 0.36674(14) 0.0135(4) Uani 1 1 d . . . H11H H 0.2600 0.1235 0.4237 0.016 Uiso 1 1 calc R . . C118 C 0.4542(2) 0.1323(2) 0.41027(16) 0.0136(4) Uani 1 1 d . . . C119 C 0.5334(3) 0.0817(2) 0.36278(18) 0.0197(5) Uani 1 1 d . . . H11I H 0.4916 0.0370 0.2996 0.024 Uiso 1 1 calc R . . C120 C 0.6727(3) 0.0965(2) 0.40715(19) 0.0229(5) Uani 1 1 d . . . H12A H 0.7251 0.0614 0.3742 0.027 Uiso 1 1 calc R . . C121 C 0.7357(3) 0.1618(2) 0.49921(18) 0.0216(5) Uani 1 1 d . . . H12B H 0.8315 0.1733 0.5286 0.026 Uiso 1 1 calc R . . C122 C 0.6581(2) 0.2100(2) 0.54783(17) 0.0196(5) Uani 1 1 d . . . H12C H 0.7001 0.2539 0.6112 0.024 Uiso 1 1 calc R . . C123 C 0.5184(2) 0.1941(2) 0.50386(16) 0.0155(4) Uani 1 1 d . . . H12D H 0.4654 0.2262 0.5385 0.019 Uiso 1 1 calc R . . N124 N 0.27948(19) 0.22806(17) 0.30721(13) 0.0149(3) Uani 1 1 d . . . C125 C 0.3444(2) 0.3507(2) 0.36939(16) 0.0198(4) Uani 1 1 d . . . H12E H 0.3049 0.3462 0.4265 0.030 Uiso 1 1 calc R . . H12F H 0.3257 0.4199 0.3313 0.030 Uiso 1 1 calc R . . H12G H 0.4457 0.3670 0.3914 0.030 Uiso 1 1 calc R . . C126 C 0.3438(3) 0.2383(2) 0.22233(17) 0.0209(5) Uani 1 1 d . . . H12H H 0.3348 0.3138 0.1890 0.031 Uiso 1 1 calc R . . H12I H 0.2961 0.1619 0.1764 0.031 Uiso 1 1 calc R . . H12J H 0.4430 0.2460 0.2457 0.031 Uiso 1 1 calc R . . C127 C -0.1631(3) 0.1537(3) 0.16866(19) 0.0244(6) Uani 1 1 d . . . H12K H -0.2369 0.0713 0.1701 0.029 Uiso 1 1 calc R . . C128 C -0.1302(3) 0.2527(3) 0.2415(2) 0.0274(6) Uani 1 1 d . . . H12L H -0.1810 0.2388 0.2947 0.033 Uiso 1 1 calc R . . C129 C -0.0096(3) 0.3601(3) 0.2533(2) 0.0240(6) Uani 1 1 d . . . H12M H 0.0220 0.4213 0.3132 0.029 Uiso 1 1 calc R . . C130 C 0.0773(3) 0.3676(3) 0.1896(2) 0.0276(6) Uani 1 1 d . . . H13A H 0.1715 0.4339 0.2055 0.033 Uiso 1 1 calc R . . C131 C 0.0459(3) 0.2688(3) 0.11442(18) 0.0256(6) Uani 1 1 d . . . H13B H 0.1183 0.2668 0.0788 0.031 Uiso 1 1 calc R . . C132 C -0.0717(3) 0.1615(3) 0.10492(18) 0.0282(6) Uani 1 1 d . . . H13C H -0.0827 0.0844 0.0621 0.034 Uiso 1 1 calc R . . C201 C -0.0727(2) -0.0431(2) 0.63806(17) 0.0251(5) Uani 1 1 d . . . H20A H -0.0598 -0.0218 0.5728 0.038 Uiso 1 1 calc R . . H20B H -0.1685 -0.0503 0.6402 0.038 Uiso 1 1 calc R . . H20C H -0.0556 -0.1245 0.6518 0.038 Uiso 1 1 calc R . . C202 C 0.0284(2) 0.0598(2) 0.71374(15) 0.0193(4) Uani 1 1 d . . . C203 C -0.0167(2) 0.1268(2) 0.77673(16) 0.0223(5) Uani 1 1 d . . . H20D H -0.1139 0.1068 0.7722 0.027 Uiso 1 1 calc R . . C204 C 0.0783(2) 0.2224(2) 0.84627(16) 0.0195(4) Uani 1 1 d . . . H20E H 0.0459 0.2678 0.8883 0.023 Uiso 1 1 calc R . . C205 C 0.2195(2) 0.25079(19) 0.85367(14) 0.0144(4) Uani 1 1 d . . . C206 C 0.2672(2) 0.1853(2) 0.79117(15) 0.0175(4) Uani 1 1 d . . . H20F H 0.3644 0.2055 0.7958 0.021 Uiso 1 1 calc R . . C207 C 0.1717(2) 0.0909(2) 0.72266(16) 0.0187(4) Uani 1 1 d . . . H20G H 0.2045 0.0460 0.6805 0.022 Uiso 1 1 calc R . . S208 S 0.34453(6) 0.36901(5) 0.94441(4) 0.01524(11) Uani 1 1 d . . . O28A O 0.40975(16) 0.29904(15) 1.01578(10) 0.0203(3) Uani 1 1 d . . . O28B O 0.26410(16) 0.43964(15) 0.97983(11) 0.0201(3) Uani 1 1 d . . . N209 N 0.45682(18) 0.45841(17) 0.89460(12) 0.0139(3) Uani 1 1 d . . . C210 C 0.4169(2) 0.56917(19) 0.85168(14) 0.0132(4) Uani 1 1 d . . . H21A H 0.4169 0.6276 0.9064 0.016 Uiso 1 1 calc R . . C211 C 0.2747(2) 0.5342(2) 0.77817(16) 0.0148(4) Uani 1 1 d . . . C212 C 0.2418(2) 0.4481(2) 0.69639(15) 0.0158(4) Uani 1 1 d . . . H21B H 0.3096 0.4113 0.6856 0.019 Uiso 1 1 calc R . . C213 C 0.1118(3) 0.4153(2) 0.63063(16) 0.0207(5) Uani 1 1 d . . . H21C H 0.0905 0.3556 0.5757 0.025 Uiso 1 1 calc R . . C214 C 0.0125(3) 0.4697(3) 0.64488(19) 0.0248(6) Uani 1 1 d . . . H21D H -0.0768 0.4473 0.5999 0.030 Uiso 1 1 calc R . . C215 C 0.0448(3) 0.5570(3) 0.72545(19) 0.0250(6) Uani 1 1 d . . . H21E H -0.0220 0.5959 0.7348 0.030 Uiso 1 1 calc R . . C216 C 0.1742(3) 0.5876(2) 0.79230(17) 0.0199(5) Uani 1 1 d . . . H21F H 0.1944 0.6455 0.8482 0.024 Uiso 1 1 calc R . . C217 C 0.5282(2) 0.64079(19) 0.79996(14) 0.0131(4) Uani 1 1 d . . . H21H H 0.5112 0.5879 0.7375 0.016 Uiso 1 1 calc R . . C218 C 0.5162(2) 0.7689(2) 0.77111(16) 0.0138(4) Uani 1 1 d . . . C219 C 0.4882(2) 0.8532(2) 0.83269(16) 0.0179(5) Uani 1 1 d . . . H21I H 0.4769 0.8307 0.8959 0.021 Uiso 1 1 calc R . . C220 C 0.4767(3) 0.9690(2) 0.80208(18) 0.0217(5) Uani 1 1 d . . . H22A H 0.4574 1.0250 0.8445 0.026 Uiso 1 1 calc R . . C221 C 0.4931(2) 1.0043(2) 0.71022(17) 0.0221(5) Uani 1 1 d . . . H22C H 0.4867 1.0845 0.6902 0.027 Uiso 1 1 calc R . . C222 C 0.5189(3) 0.9209(2) 0.64800(18) 0.0213(5) Uani 1 1 d . . . H22D H 0.5295 0.9436 0.5847 0.026 Uiso 1 1 calc R . . C223 C 0.5291(2) 0.8048(2) 0.67839(16) 0.0164(4) Uani 1 1 d . . . H22E H 0.5454 0.7480 0.6348 0.020 Uiso 1 1 calc R . . N224 N 0.67269(19) 0.64539(17) 0.86079(12) 0.0135(4) Uani 1 1 d . . . C225 C 0.7169(2) 0.7319(2) 0.95232(16) 0.0179(5) Uani 1 1 d . . . H22F H 0.6545 0.6978 0.9950 0.027 Uiso 1 1 calc R . . H22G H 0.7123 0.8167 0.9358 0.027 Uiso 1 1 calc R . . H22H H 0.8130 0.7383 0.9864 0.027 Uiso 1 1 calc R . . C226 C 0.7764(2) 0.6964(2) 0.80241(16) 0.0187(4) Uani 1 1 d . . . H22I H 0.7517 0.6406 0.7420 0.028 Uiso 1 1 calc R . . H22J H 0.8697 0.7000 0.8409 0.028 Uiso 1 1 calc R . . H22K H 0.7763 0.7822 0.7858 0.028 Uiso 1 1 calc R . . C227 C 0.7081(3) 0.3939(2) 1.04619(18) 0.0223(5) Uani 1 1 d . . . H22B H 0.6484 0.4020 1.0909 0.027 Uiso 1 1 calc R . . C228 C 0.8189(3) 0.4999(3) 1.03764(18) 0.0269(6) Uani 1 1 d . . . H22L H 0.8363 0.5825 1.0760 0.032 Uiso 1 1 calc R . . C229 C 0.8867(3) 0.4987(3) 0.9606(2) 0.0271(6) Uani 1 1 d . . . H22M H 0.9512 0.5801 0.9464 0.033 Uiso 1 1 calc R . . C230 C 0.8437(3) 0.3908(3) 0.8939(2) 0.0228(5) Uani 1 1 d . . . H23A H 0.8786 0.3957 0.8331 0.027 Uiso 1 1 calc R . . C231 C 0.7323(3) 0.2828(2) 0.9039(2) 0.0227(6) Uani 1 1 d . . . H23B H 0.6895 0.2134 0.8491 0.027 Uiso 1 1 calc R . . C232 C 0.6646(3) 0.2830(2) 0.97937(17) 0.0202(5) Uani 1 1 d . . . H23C H 0.5752 0.2142 0.9777 0.024 Uiso 1 1 calc R . . O300 O 0.0997(2) 0.7797(2) 0.97982(14) 0.0420(5) Uani 1 1 d . . . H300 H 0.097(4) 0.780(4) 1.043(3) 0.063 Uiso 1 1 d . . . C301 C 0.1499(4) 0.9088(3) 0.9569(3) 0.0552(9) Uani 1 1 d . . . H30D H 0.0875 0.9555 0.9708 0.066 Uiso 1 1 calc R . . H30E H 0.1458 0.9094 0.8859 0.066 Uiso 1 1 calc R . . C302 C 0.2937(3) 0.9754(3) 1.0128(2) 0.0416(7) Uani 1 1 d . . . H30A H 0.3210 1.0641 0.9965 0.062 Uiso 1 1 calc R . . H30B H 0.3571 0.9332 0.9959 0.062 Uiso 1 1 calc R . . H30C H 0.2991 0.9735 1.0832 0.062 Uiso 1 1 calc R . . O400 O 0.3617(2) 0.55739(18) 0.17113(13) 0.0351(4) Uani 1 1 d . . . H400 H 0.319(4) 0.529(3) 0.113(3) 0.053 Uiso 1 1 d . . . C401 C 0.4998(3) 0.6387(3) 0.1776(2) 0.0416(7) Uani 1 1 d . . . H40D H 0.5448 0.5980 0.1377 0.050 Uiso 1 1 calc R . . H40E H 0.5550 0.6503 0.2466 0.050 Uiso 1 1 calc R . . C402 C 0.5007(3) 0.7669(3) 0.1423(2) 0.0376(6) Uani 1 1 d . . . H40A H 0.5976 0.8217 0.1512 0.056 Uiso 1 1 calc R . . H40B H 0.4533 0.8062 0.1801 0.056 Uiso 1 1 calc R . . H40C H 0.4520 0.7563 0.0726 0.056 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.01518(9) 0.01342(9) 0.01425(8) 0.00496(6) 0.00350(6) 0.00566(7) Cl1 0.0172(2) 0.0216(3) 0.0162(2) 0.0020(2) 0.00629(19) 0.0091(2) Ru2 0.01577(9) 0.01171(8) 0.01370(8) 0.00268(6) 0.00204(6) 0.00645(7) Cl2 0.0218(3) 0.0171(2) 0.0158(2) -0.00093(19) 0.00454(19) 0.0088(2) C101 0.0298(13) 0.0333(15) 0.0234(12) 0.0069(11) 0.0062(10) 0.0043(11) C102 0.0181(11) 0.0236(12) 0.0164(10) 0.0003(9) -0.0017(8) 0.0014(9) C103 0.0252(12) 0.0183(11) 0.0224(11) 0.0040(9) 0.0027(9) 0.0048(9) C104 0.0211(11) 0.0181(11) 0.0211(10) -0.0002(9) 0.0034(8) 0.0069(9) C105 0.0161(10) 0.0150(10) 0.0157(10) -0.0001(8) 0.0015(8) 0.0017(8) C106 0.0252(11) 0.0135(10) 0.0266(11) 0.0003(9) 0.0068(9) 0.0056(9) C107 0.0223(11) 0.0200(12) 0.0223(11) -0.0044(9) 0.0059(9) 0.0030(9) S108 0.0220(3) 0.0133(3) 0.0138(2) -0.0009(2) 0.0028(2) 0.0030(2) O18A 0.0298(9) 0.0178(8) 0.0190(7) -0.0010(6) 0.0074(6) 0.0056(7) O18B 0.0247(8) 0.0207(8) 0.0181(7) 0.0014(6) -0.0025(6) 0.0038(7) N109 0.0195(9) 0.0126(9) 0.0150(9) 0.0012(7) 0.0020(7) 0.0054(7) C110 0.0179(10) 0.0131(10) 0.0159(10) 0.0030(8) 0.0061(8) 0.0068(9) C111 0.0135(11) 0.0159(11) 0.0191(11) 0.0033(9) 0.0032(9) 0.0016(9) C112 0.0218(13) 0.0187(12) 0.0390(15) 0.0040(11) 0.0077(11) 0.0070(10) C113 0.0270(14) 0.0185(13) 0.0629(19) 0.0094(13) 0.0008(13) 0.0125(11) C114 0.0290(15) 0.0237(15) 0.0541(19) 0.0281(14) -0.0006(13) 0.0049(12) C115 0.0240(12) 0.0299(14) 0.0298(13) 0.0168(11) -0.0006(10) -0.0005(11) C116 0.0169(11) 0.0187(12) 0.0229(11) 0.0058(9) 0.0010(9) 0.0000(9) C117 0.0169(10) 0.0132(10) 0.0132(9) 0.0043(8) 0.0057(8) 0.0070(8) C118 0.0138(10) 0.0115(10) 0.0188(11) 0.0049(8) 0.0070(8) 0.0063(8) C119 0.0199(12) 0.0177(12) 0.0226(11) 0.0018(9) 0.0080(9) 0.0054(9) C120 0.0223(12) 0.0204(12) 0.0330(13) 0.0052(10) 0.0138(10) 0.0114(10) C121 0.0162(11) 0.0207(12) 0.0311(13) 0.0100(10) 0.0079(10) 0.0085(10) C122 0.0178(11) 0.0182(11) 0.0235(11) 0.0067(9) 0.0064(9) 0.0055(9) C123 0.0169(11) 0.0130(10) 0.0191(10) 0.0049(8) 0.0071(9) 0.0062(9) N124 0.0162(8) 0.0117(9) 0.0170(8) 0.0042(7) 0.0049(7) 0.0042(7) C125 0.0210(11) 0.0123(10) 0.0241(11) 0.0009(9) 0.0031(9) 0.0044(9) C126 0.0232(12) 0.0236(12) 0.0205(11) 0.0076(9) 0.0103(9) 0.0101(10) C127 0.0184(12) 0.0223(13) 0.0309(13) 0.0131(11) 0.0008(10) 0.0076(10) C128 0.0237(13) 0.0328(15) 0.0337(14) 0.0160(12) 0.0085(11) 0.0189(12) C129 0.0250(14) 0.0198(13) 0.0289(14) 0.0086(11) 0.0017(11) 0.0130(11) C130 0.0234(13) 0.0225(13) 0.0330(14) 0.0189(11) -0.0015(10) 0.0072(11) C131 0.0239(13) 0.0338(14) 0.0208(11) 0.0172(11) 0.0043(10) 0.0121(11) C132 0.0355(15) 0.0322(15) 0.0158(11) 0.0089(10) -0.0024(10) 0.0155(13) C201 0.0220(11) 0.0266(13) 0.0239(11) 0.0010(10) 0.0042(9) 0.0051(10) C202 0.0220(11) 0.0171(11) 0.0180(10) 0.0077(8) 0.0045(9) 0.0051(9) C203 0.0154(10) 0.0283(12) 0.0234(11) 0.0057(9) 0.0047(9) 0.0073(9) C204 0.0212(11) 0.0220(11) 0.0185(10) 0.0027(9) 0.0071(9) 0.0099(9) C205 0.0182(10) 0.0105(9) 0.0151(9) 0.0063(8) 0.0047(8) 0.0050(8) C206 0.0171(10) 0.0151(10) 0.0213(10) 0.0047(8) 0.0061(8) 0.0052(8) C207 0.0232(11) 0.0147(10) 0.0215(10) 0.0027(8) 0.0096(9) 0.0076(9) S208 0.0195(3) 0.0138(3) 0.0136(2) 0.0036(2) 0.0064(2) 0.0051(2) O28A 0.0247(8) 0.0201(8) 0.0166(7) 0.0092(6) 0.0054(6) 0.0071(7) O28B 0.0250(8) 0.0190(8) 0.0196(7) 0.0028(6) 0.0124(6) 0.0066(7) N209 0.0153(8) 0.0124(9) 0.0149(8) 0.0046(7) 0.0050(7) 0.0044(7) C210 0.0182(10) 0.0086(9) 0.0146(9) 0.0015(8) 0.0048(8) 0.0062(8) C211 0.0169(10) 0.0109(10) 0.0179(10) 0.0070(8) 0.0056(8) 0.0052(8) C212 0.0170(10) 0.0139(10) 0.0170(10) 0.0057(9) 0.0049(8) 0.0052(8) C213 0.0238(12) 0.0173(11) 0.0178(11) 0.0027(9) 0.0038(9) 0.0027(10) C214 0.0143(11) 0.0307(14) 0.0268(12) 0.0106(11) 0.0016(10) 0.0056(10) C215 0.0169(12) 0.0310(14) 0.0339(13) 0.0103(11) 0.0117(10) 0.0131(11) C216 0.0207(12) 0.0218(12) 0.0209(11) 0.0025(9) 0.0095(9) 0.0088(10) C217 0.0155(10) 0.0131(10) 0.0116(9) 0.0030(8) 0.0038(8) 0.0054(8) C218 0.0137(10) 0.0097(10) 0.0181(10) 0.0052(8) 0.0020(8) 0.0052(8) C219 0.0236(12) 0.0159(11) 0.0173(10) 0.0049(9) 0.0074(9) 0.0088(9) C220 0.0280(12) 0.0171(11) 0.0246(11) 0.0050(9) 0.0106(10) 0.0107(10) C221 0.0230(12) 0.0181(12) 0.0274(12) 0.0092(10) 0.0069(10) 0.0088(10) C222 0.0227(12) 0.0238(13) 0.0190(11) 0.0093(10) 0.0068(9) 0.0081(10) C223 0.0179(10) 0.0163(11) 0.0166(10) 0.0015(9) 0.0053(8) 0.0070(9) N224 0.0146(9) 0.0139(9) 0.0125(8) 0.0031(7) 0.0016(7) 0.0066(7) C225 0.0223(12) 0.0155(11) 0.0156(10) 0.0003(9) 0.0017(9) 0.0079(9) C226 0.0177(10) 0.0208(11) 0.0198(10) 0.0086(9) 0.0066(8) 0.0077(9) C227 0.0265(13) 0.0248(13) 0.0163(11) 0.0068(9) -0.0011(9) 0.0138(11) C228 0.0303(14) 0.0220(13) 0.0232(12) 0.0038(10) -0.0099(10) 0.0131(11) C229 0.0174(12) 0.0237(13) 0.0362(14) 0.0138(11) -0.0029(10) 0.0076(10) C230 0.0185(12) 0.0263(14) 0.0292(13) 0.0101(11) 0.0063(10) 0.0144(11) C231 0.0273(14) 0.0177(13) 0.0281(13) 0.0047(11) 0.0019(11) 0.0179(12) C232 0.0224(12) 0.0176(12) 0.0227(12) 0.0098(10) 0.0017(10) 0.0118(10) O300 0.0477(12) 0.0403(12) 0.0270(9) 0.0037(9) 0.0125(9) -0.0046(10) C301 0.051(2) 0.054(2) 0.060(2) 0.0399(17) 0.0131(16) 0.0153(17) C302 0.062(2) 0.0231(14) 0.0424(16) 0.0065(12) 0.0265(15) 0.0073(14) O400 0.0389(11) 0.0316(10) 0.0224(8) 0.0026(8) 0.0069(8) -0.0065(8) C401 0.0295(14) 0.0356(16) 0.0463(16) 0.0133(13) -0.0042(12) 0.0007(12) C402 0.0395(15) 0.0300(15) 0.0434(16) 0.0057(12) 0.0178(13) 0.0055(12) _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 N109 2.1382(18) . ? Ru1 C130 2.182(3) . ? Ru1 C129 2.185(3) . ? Ru1 C128 2.186(3) . ? Ru1 C132 2.187(2) . ? Ru1 N124 2.1944(18) . ? Ru1 C131 2.200(2) . ? Ru1 C127 2.202(3) . ? Ru1 Cl1 2.4213(5) . ? Ru2 N209 2.1384(17) . ? Ru2 C231 2.187(2) . ? Ru2 N224 2.1912(18) . ? Ru2 C230 2.192(2) . ? Ru2 C229 2.196(3) . ? Ru2 C227 2.197(2) . ? Ru2 C228 2.205(2) . ? Ru2 C232 2.206(2) . ? Ru2 Cl2 2.4276(5) . ? C101 C102 1.506(3) . ? C101 H10A 0.9800 . ? C101 H10B 0.9800 . ? C101 H10C 0.9800 . ? C102 C103 1.392(3) . ? C102 C107 1.399(3) . ? C103 C104 1.405(3) . ? C103 H10D 0.9500 . ? C104 C105 1.377(3) . ? C104 H10E 0.9500 . ? C105 C106 1.392(3) . ? C105 S108 1.784(2) . ? C106 C107 1.376(3) . ? C106 H10F 0.9500 . ? C107 H10G 0.9500 . ? S108 O18B 1.4414(17) . ? S108 O18A 1.4547(16) . ? S108 N109 1.5886(19) . ? N109 C110 1.495(3) . ? C110 C111 1.517(3) . ? C110 C117 1.524(3) . ? C110 H11A 1.0000 . ? C111 C116 1.394(3) . ? C111 C112 1.407(3) . ? C112 C113 1.396(4) . ? C112 H11B 0.9500 . ? C113 C114 1.379(5) . ? C113 H11D 0.9500 . ? C114 C115 1.368(4) . ? C114 H11E 0.9500 . ? C115 C116 1.382(3) . ? C115 H11F 0.9500 . ? C116 H11G 0.9500 . ? C117 N124 1.510(3) . ? C117 C118 1.519(3) . ? C117 H11H 1.0000 . ? C118 C123 1.393(3) . ? C118 C119 1.399(3) . ? C119 C120 1.390(4) . ? C119 H11I 0.9500 . ? C120 C121 1.387(4) . ? C120 H12A 0.9500 . ? C121 C122 1.380(3) . ? C121 H12B 0.9500 . ? C122 C123 1.391(3) . ? C122 H12C 0.9500 . ? C123 H12D 0.9500 . ? N124 C125 1.484(3) . ? N124 C126 1.488(3) . ? C125 H12E 0.9800 . ? C125 H12F 0.9800 . ? C125 H12G 0.9800 . ? C126 H12H 0.9800 . ? C126 H12I 0.9800 . ? C126 H12J 0.9800 . ? C127 C128 1.397(4) . ? C127 C132 1.434(4) . ? C127 H12K 1.0000 . ? C128 C129 1.413(4) . ? C128 H12L 1.0000 . ? C129 C130 1.399(4) . ? C129 H12M 1.0000 . ? C130 C131 1.420(4) . ? C130 H13A 1.0000 . ? C131 C132 1.398(4) . ? C131 H13B 1.0000 . ? C132 H13C 1.0000 . ? C201 C202 1.502(3) . ? C201 H20A 0.9800 . ? C201 H20B 0.9800 . ? C201 H20C 0.9800 . ? C202 C207 1.393(3) . ? C202 C203 1.393(3) . ? C203 C204 1.393(3) . ? C203 H20D 0.9500 . ? C204 C205 1.379(3) . ? C204 H20E 0.9500 . ? C205 C206 1.396(3) . ? C205 S208 1.783(2) . ? C206 C207 1.380(3) . ? C206 H20F 0.9500 . ? C207 H20G 0.9500 . ? S208 O28A 1.4421(16) . ? S208 O28B 1.4600(15) . ? S208 N209 1.5883(18) . ? N209 C210 1.497(3) . ? C210 C211 1.524(3) . ? C210 C217 1.530(3) . ? C210 H21A 1.0000 . ? C211 C216 1.392(3) . ? C211 C212 1.394(3) . ? C212 C213 1.385(3) . ? C212 H21B 0.9500 . ? C213 C214 1.388(3) . ? C213 H21C 0.9500 . ? C214 C215 1.390(4) . ? C214 H21D 0.9500 . ? C215 C216 1.388(4) . ? C215 H21E 0.9500 . ? C216 H21F 0.9500 . ? C217 C218 1.510(3) . ? C217 N224 1.526(3) . ? C217 H21H 1.0000 . ? C218 C223 1.393(3) . ? C218 C219 1.403(3) . ? C219 C220 1.385(3) . ? C219 H21I 0.9500 . ? C220 C221 1.388(3) . ? C220 H22A 0.9500 . ? C221 C222 1.389(3) . ? C221 H22C 0.9500 . ? C222 C223 1.384(3) . ? C222 H22D 0.9500 . ? C223 H22E 0.9500 . ? N224 C226 1.485(3) . ? N224 C225 1.489(3) . ? C225 H22F 0.9800 . ? C225 H22G 0.9800 . ? C225 H22H 0.9800 . ? C226 H22I 0.9800 . ? C226 H22J 0.9800 . ? C226 H22K 0.9800 . ? C227 C228 1.399(4) . ? C227 C232 1.426(4) . ? C227 H22B 1.0000 . ? C228 C229 1.425(4) . ? C228 H22L 1.0000 . ? C229 C230 1.400(4) . ? C229 H22M 1.0000 . ? C230 C231 1.422(4) . ? C230 H23A 1.0000 . ? C231 C232 1.404(4) . ? C231 H23B 1.0000 . ? C232 H23C 1.0000 . ? O300 C301 1.431(4) . ? O300 H300 0.89(4) . ? C301 C302 1.468(5) . ? C301 H30D 0.9900 . ? C301 H30E 0.9900 . ? C302 H30A 0.9800 . ? C302 H30B 0.9800 . ? C302 H30C 0.9800 . ? O400 C401 1.422(3) . ? O400 H400 0.84(3) . ? C401 C402 1.504(4) . ? C401 H40D 0.9900 . ? C401 H40E 0.9900 . ? C402 H40A 0.9800 . ? C402 H40B 0.9800 . ? C402 H40C 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 N109 Ru1 C130 148.89(9) . . ? N109 Ru1 C129 170.18(9) . . ? C130 Ru1 C129 37.36(11) . . ? N109 Ru1 C128 132.47(9) . . ? C130 Ru1 C128 67.37(11) . . ? C129 Ru1 C128 37.72(11) . . ? N109 Ru1 C132 95.78(9) . . ? C130 Ru1 C132 67.81(11) . . ? C129 Ru1 C132 80.66(11) . . ? C128 Ru1 C132 67.80(11) . . ? N109 Ru1 N124 76.84(7) . . ? C130 Ru1 N124 91.88(9) . . ? C129 Ru1 N124 112.64(9) . . ? C128 Ru1 N124 148.99(9) . . ? C132 Ru1 N124 126.98(9) . . ? N109 Ru1 C131 114.40(9) . . ? C130 Ru1 C131 37.81(11) . . ? C129 Ru1 C131 67.94(11) . . ? C128 Ru1 C131 79.69(10) . . ? C132 Ru1 C131 37.16(10) . . ? N124 Ru1 C131 98.21(8) . . ? N109 Ru1 C127 103.64(8) . . ? C130 Ru1 C127 80.08(10) . . ? C129 Ru1 C127 67.94(10) . . ? C128 Ru1 C127 37.13(10) . . ? C132 Ru1 C127 38.14(10) . . ? N124 Ru1 C127 165.00(8) . . ? C131 Ru1 C127 67.72(10) . . ? N109 Ru1 Cl1 86.55(5) . . ? C130 Ru1 Cl1 122.33(8) . . ? C129 Ru1 Cl1 91.17(7) . . ? C128 Ru1 Cl1 84.95(7) . . ? C132 Ru1 Cl1 145.01(8) . . ? N124 Ru1 Cl1 87.62(5) . . ? C131 Ru1 Cl1 159.00(8) . . ? C127 Ru1 Cl1 107.38(7) . . ? N209 Ru2 C231 128.01(9) . . ? N209 Ru2 N224 76.72(7) . . ? C231 Ru2 N224 153.82(9) . . ? N209 Ru2 C230 165.73(8) . . ? C231 Ru2 C230 37.90(10) . . ? N224 Ru2 C230 116.82(9) . . ? N209 Ru2 C229 152.78(9) . . ? C231 Ru2 C229 67.55(10) . . ? N224 Ru2 C229 93.94(9) . . ? C230 Ru2 C229 37.22(10) . . ? N209 Ru2 C227 96.07(8) . . ? C231 Ru2 C227 67.61(10) . . ? N224 Ru2 C227 123.87(8) . . ? C230 Ru2 C227 80.29(10) . . ? C229 Ru2 C227 67.71(10) . . ? N209 Ru2 C228 117.15(9) . . ? C231 Ru2 C228 79.66(10) . . ? N224 Ru2 C228 97.18(8) . . ? C230 Ru2 C228 67.66(10) . . ? C229 Ru2 C228 37.77(11) . . ? C227 Ru2 C228 37.07(10) . . ? N209 Ru2 C232 100.69(8) . . ? C231 Ru2 C232 37.26(10) . . ? N224 Ru2 C232 161.58(7) . . ? C230 Ru2 C232 67.99(10) . . ? C229 Ru2 C232 80.08(10) . . ? C227 Ru2 C232 37.78(9) . . ? C228 Ru2 C232 67.45(9) . . ? N209 Ru2 Cl2 88.12(5) . . ? C231 Ru2 Cl2 85.50(7) . . ? N224 Ru2 Cl2 87.18(5) . . ? C230 Ru2 Cl2 88.09(7) . . ? C229 Ru2 Cl2 117.27(8) . . ? C227 Ru2 Cl2 148.84(7) . . ? C228 Ru2 Cl2 154.71(8) . . ? C232 Ru2 Cl2 111.09(6) . . ? C102 C101 H10A 109.5 . . ? C102 C101 H10B 109.5 . . ? H10A C101 H10B 109.5 . . ? C102 C101 H10C 109.5 . . ? H10A C101 H10C 109.5 . . ? H10B C101 H10C 109.5 . . ? C103 C102 C107 118.2(2) . . ? C103 C102 C101 121.3(2) . . ? C107 C102 C101 120.4(2) . . ? C102 C103 C104 121.1(2) . . ? C102 C103 H10D 119.4 . . ? C104 C103 H10D 119.4 . . ? C105 C104 C103 119.0(2) . . ? C105 C104 H10E 120.5 . . ? C103 C104 H10E 120.5 . . ? C104 C105 C106 120.8(2) . . ? C104 C105 S108 121.76(17) . . ? C106 C105 S108 117.45(17) . . ? C107 C106 C105 119.8(2) . . ? C107 C106 H10F 120.1 . . ? C105 C106 H10F 120.1 . . ? C106 C107 C102 121.1(2) . . ? C106 C107 H10G 119.5 . . ? C102 C107 H10G 119.5 . . ? O18B S108 O18A 116.48(10) . . ? O18B S108 N109 109.32(10) . . ? O18A S108 N109 111.66(10) . . ? O18B S108 C105 104.76(10) . . ? O18A S108 C105 105.43(10) . . ? N109 S108 C105 108.65(10) . . ? C110 N109 S108 114.78(14) . . ? C110 N109 Ru1 117.24(13) . . ? S108 N109 Ru1 127.64(11) . . ? N109 C110 C111 115.13(18) . . ? N109 C110 C117 107.46(16) . . ? C111 C110 C117 109.34(17) . . ? N109 C110 H11A 108.2 . . ? C111 C110 H11A 108.2 . . ? C117 C110 H11A 108.2 . . ? C116 C111 C112 118.2(2) . . ? C116 C111 C110 121.9(2) . . ? C112 C111 C110 119.8(2) . . ? C113 C112 C111 120.2(3) . . ? C113 C112 H11B 119.9 . . ? C111 C112 H11B 119.9 . . ? C114 C113 C112 119.7(2) . . ? C114 C113 H11D 120.2 . . ? C112 C113 H11D 120.2 . . ? C115 C114 C113 120.8(3) . . ? C115 C114 H11E 119.6 . . ? C113 C114 H11E 119.6 . . ? C114 C115 C116 120.2(3) . . ? C114 C115 H11F 119.9 . . ? C116 C115 H11F 119.9 . . ? C115 C116 C111 120.9(2) . . ? C115 C116 H11G 119.5 . . ? C111 C116 H11G 119.5 . . ? N124 C117 C118 114.20(17) . . ? N124 C117 C110 109.74(16) . . ? C118 C117 C110 113.82(17) . . ? N124 C117 H11H 106.1 . . ? C118 C117 H11H 106.1 . . ? C110 C117 H11H 106.1 . . ? C123 C118 C119 117.8(2) . . ? C123 C118 C117 118.43(18) . . ? C119 C118 C117 123.7(2) . . ? C120 C119 C118 120.6(2) . . ? C120 C119 H11I 119.7 . . ? C118 C119 H11I 119.7 . . ? C121 C120 C119 120.6(2) . . ? C121 C120 H12A 119.7 . . ? C119 C120 H12A 119.7 . . ? C122 C121 C120 119.5(2) . . ? C122 C121 H12B 120.3 . . ? C120 C121 H12B 120.3 . . ? C121 C122 C123 119.9(2) . . ? C121 C122 H12C 120.0 . . ? C123 C122 H12C 120.0 . . ? C122 C123 C118 121.5(2) . . ? C122 C123 H12D 119.2 . . ? C118 C123 H12D 119.2 . . ? C125 N124 C126 107.70(17) . . ? C125 N124 C117 109.88(16) . . ? C126 N124 C117 111.78(17) . . ? C125 N124 Ru1 110.59(13) . . ? C126 N124 Ru1 110.70(14) . . ? C117 N124 Ru1 106.23(12) . . ? N124 C125 H12E 109.5 . . ? N124 C125 H12F 109.5 . . ? H12E C125 H12F 109.5 . . ? N124 C125 H12G 109.5 . . ? H12E C125 H12G 109.5 . . ? H12F C125 H12G 109.5 . . ? N124 C126 H12H 109.5 . . ? N124 C126 H12I 109.5 . . ? H12H C126 H12I 109.5 . . ? N124 C126 H12J 109.5 . . ? H12H C126 H12J 109.5 . . ? H12I C126 H12J 109.5 . . ? C128 C127 C132 119.0(3) . . ? C128 C127 Ru1 70.79(15) . . ? C132 C127 Ru1 70.38(14) . . ? C128 C127 H12K 119.9 . . ? C132 C127 H12K 119.9 . . ? Ru1 C127 H12K 119.9 . . ? C127 C128 C129 121.5(3) . . ? C127 C128 Ru1 72.07(15) . . ? C129 C128 Ru1 71.11(15) . . ? C127 C128 H12L 118.6 . . ? C129 C128 H12L 118.6 . . ? Ru1 C128 H12L 118.6 . . ? C130 C129 C128 119.0(3) . . ? C130 C129 Ru1 71.21(15) . . ? C128 C129 Ru1 71.16(15) . . ? C130 C129 H12M 120.1 . . ? C128 C129 H12M 120.1 . . ? Ru1 C129 H12M 120.1 . . ? C129 C130 C131 120.8(3) . . ? C129 C130 Ru1 71.43(15) . . ? C131 C130 Ru1 71.79(15) . . ? C129 C130 H13A 119.1 . . ? C131 C130 H13A 119.1 . . ? Ru1 C130 H13A 119.1 . . ? C132 C131 C130 119.8(2) . . ? C132 C131 Ru1 70.92(14) . . ? C130 C131 Ru1 70.40(14) . . ? C132 C131 H13B 119.4 . . ? C130 C131 H13B 119.4 . . ? Ru1 C131 H13B 119.4 . . ? C131 C132 C127 120.0(2) . . ? C131 C132 Ru1 71.92(14) . . ? C127 C132 Ru1 71.49(14) . . ? C131 C132 H13C 119.6 . . ? C127 C132 H13C 119.6 . . ? Ru1 C132 H13C 119.6 . . ? C202 C201 H20A 109.5 . . ? C202 C201 H20B 109.5 . . ? H20A C201 H20B 109.5 . . ? C202 C201 H20C 109.5 . . ? H20A C201 H20C 109.5 . . ? H20B C201 H20C 109.5 . . ? C207 C202 C203 118.0(2) . . ? C207 C202 C201 120.2(2) . . ? C203 C202 C201 121.8(2) . . ? C204 C203 C202 121.1(2) . . ? C204 C203 H20D 119.4 . . ? C202 C203 H20D 119.4 . . ? C205 C204 C203 119.6(2) . . ? C205 C204 H20E 120.2 . . ? C203 C204 H20E 120.2 . . ? C204 C205 C206 120.3(2) . . ? C204 C205 S208 120.88(16) . . ? C206 C205 S208 118.81(16) . . ? C207 C206 C205 119.4(2) . . ? C207 C206 H20F 120.3 . . ? C205 C206 H20F 120.3 . . ? C206 C207 C202 121.6(2) . . ? C206 C207 H20G 119.2 . . ? C202 C207 H20G 119.2 . . ? O28A S208 O28B 115.55(9) . . ? O28A S208 N209 110.22(10) . . ? O28B S208 N209 111.37(10) . . ? O28A S208 C205 105.19(10) . . ? O28B S208 C205 105.15(10) . . ? N209 S208 C205 108.87(10) . . ? C210 N209 S208 113.75(13) . . ? C210 N209 Ru2 117.74(12) . . ? S208 N209 Ru2 128.13(10) . . ? N209 C210 C211 114.94(17) . . ? N209 C210 C217 108.11(16) . . ? C211 C210 C217 108.24(16) . . ? N209 C210 H21A 108.5 . . ? C211 C210 H21A 108.5 . . ? C217 C210 H21A 108.5 . . ? C216 C211 C212 118.6(2) . . ? C216 C211 C210 120.15(19) . . ? C212 C211 C210 121.21(19) . . ? C213 C212 C211 121.0(2) . . ? C213 C212 H21B 119.5 . . ? C211 C212 H21B 119.5 . . ? C212 C213 C214 120.1(2) . . ? C212 C213 H21C 120.0 . . ? C214 C213 H21C 120.0 . . ? C213 C214 C215 119.5(2) . . ? C213 C214 H21D 120.2 . . ? C215 C214 H21D 120.2 . . ? C216 C215 C214 120.3(2) . . ? C216 C215 H21E 119.9 . . ? C214 C215 H21E 119.9 . . ? C215 C216 C211 120.6(2) . . ? C215 C216 H21F 119.7 . . ? C211 C216 H21F 119.7 . . ? C218 C217 N224 114.28(17) . . ? C218 C217 C210 113.24(17) . . ? N224 C217 C210 109.61(16) . . ? C218 C217 H21H 106.4 . . ? N224 C217 H21H 106.4 . . ? C210 C217 H21H 106.4 . . ? C223 C218 C219 117.7(2) . . ? C223 C218 C217 119.30(19) . . ? C219 C218 C217 122.9(2) . . ? C220 C219 C218 120.5(2) . . ? C220 C219 H21I 119.7 . . ? C218 C219 H21I 119.7 . . ? C219 C220 C221 120.9(2) . . ? C219 C220 H22A 119.6 . . ? C221 C220 H22A 119.6 . . ? C220 C221 C222 119.2(2) . . ? C220 C221 H22C 120.4 . . ? C222 C221 H22C 120.4 . . ? C223 C222 C221 119.9(2) . . ? C223 C222 H22D 120.1 . . ? C221 C222 H22D 120.1 . . ? C222 C223 C218 121.8(2) . . ? C222 C223 H22E 119.1 . . ? C218 C223 H22E 119.1 . . ? C226 N224 C225 107.15(17) . . ? C226 N224 C217 108.77(16) . . ? C225 N224 C217 111.81(16) . . ? C226 N224 Ru2 111.69(13) . . ? C225 N224 Ru2 110.41(13) . . ? C217 N224 Ru2 107.05(12) . . ? N224 C225 H22F 109.5 . . ? N224 C225 H22G 109.5 . . ? H22F C225 H22G 109.5 . . ? N224 C225 H22H 109.5 . . ? H22F C225 H22H 109.5 . . ? H22G C225 H22H 109.5 . . ? N224 C226 H22I 109.5 . . ? N224 C226 H22J 109.5 . . ? H22I C226 H22J 109.5 . . ? N224 C226 H22K 109.5 . . ? H22I C226 H22K 109.5 . . ? H22J C226 H22K 109.5 . . ? C228 C227 C232 120.2(2) . . ? C228 C227 Ru2 71.77(14) . . ? C232 C227 Ru2 71.46(14) . . ? C228 C227 H22B 119.4 . . ? C232 C227 H22B 119.4 . . ? Ru2 C227 H22B 119.4 . . ? C227 C228 C229 120.1(2) . . ? C227 C228 Ru2 71.16(14) . . ? C229 C228 Ru2 70.77(14) . . ? C227 C228 H22L 119.3 . . ? C229 C228 H22L 119.3 . . ? Ru2 C228 H22L 119.3 . . ? C230 C229 C228 120.1(2) . . ? C230 C229 Ru2 71.21(15) . . ? C228 C229 Ru2 71.45(15) . . ? C230 C229 H22M 119.4 . . ? C228 C229 H22M 119.4 . . ? Ru2 C229 H22M 119.4 . . ? C229 C230 C231 119.4(2) . . ? C229 C230 Ru2 71.57(15) . . ? C231 C230 Ru2 70.88(14) . . ? C229 C230 H23A 119.8 . . ? C231 C230 H23A 119.8 . . ? Ru2 C230 H23A 119.8 . . ? C232 C231 C230 121.0(2) . . ? C232 C231 Ru2 72.12(14) . . ? C230 C231 Ru2 71.23(14) . . ? C232 C231 H23B 118.9 . . ? C230 C231 H23B 118.9 . . ? Ru2 C231 H23B 118.9 . . ? C231 C232 C227 119.1(2) . . ? C231 C232 Ru2 70.62(14) . . ? C227 C232 Ru2 70.77(14) . . ? C231 C232 H23C 119.8 . . ? C227 C232 H23C 119.8 . . ? Ru2 C232 H23C 119.8 . . ? C301 O300 H300 109(3) . . ? O300 C301 C302 112.9(3) . . ? O300 C301 H30D 109.0 . . ? C302 C301 H30D 109.0 . . ? O300 C301 H30E 109.0 . . ? C302 C301 H30E 109.0 . . ? H30D C301 H30E 107.8 . . ? C301 C302 H30A 109.5 . . ? C301 C302 H30B 109.5 . . ? H30A C302 H30B 109.5 . . ? C301 C302 H30C 109.5 . . ? H30A C302 H30C 109.5 . . ? H30B C302 H30C 109.5 . . ? C401 O400 H400 112(2) . . ? O400 C401 C402 111.9(2) . . ? O400 C401 H40D 109.2 . . ? C402 C401 H40D 109.2 . . ? O400 C401 H40E 109.2 . . ? C402 C401 H40E 109.2 . . ? H40D C401 H40E 107.9 . . ? C401 C402 H40A 109.5 . . ? C401 C402 H40B 109.5 . . ? H40A C402 H40B 109.5 . . ? C401 C402 H40C 109.5 . . ? H40A C402 H40C 109.5 . . ? H40B C402 H40C 109.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O300 H300 O18A 0.89(4) 1.97(4) 2.830(2) 161(3) 1_566 O400 H400 O28B 0.84(3) 1.98(3) 2.796(2) 163(3) 1_554 _diffrn_measured_fraction_theta_max 0.894 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.675 _refine_diff_density_min -0.544 _refine_diff_density_rms 0.058