# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_coden_Cambridge 222 _journal_volume ? _journal_page_first ? _journal_year ? loop_ _publ_author_name 'M. Wills' 'Fung Kei Cheung.' 'Adam J. Clarke' 'Guy J. Clarkson' 'Adriana Lorente Criville' 'David J. Fox' 'Mark A. Graham' 'Changxue Lin.' _publ_contact_author_name 'M. Wills' _publ_contact_author_email M.WILLS@WARWICK.AC.UK _publ_section_title ; Kinetic and structural studies on 'tethered' Ru(II) arene ketone reduction catalysts ; # Attachment 'Cl1new compound rr-3.cif' data_cl1 _database_code_depnum_ccdc_archive 'CCDC 741012' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C31.50 H35 Cl N2 O2.50 Ru S' _chemical_formula_weight 650.20 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 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 7.0703(3) _cell_length_b 11.9645(6) _cell_length_c 34.9758(18) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2958.7(2) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 25686 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description rod _exptl_crystal_colour orange _exptl_crystal_size_max 0.80 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.460 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1340 _exptl_absorpt_coefficient_mu 0.724 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5849 _exptl_absorpt_correction_T_max 0.9182 _exptl_absorpt_process_details 'SADABS 2007/2 (Sheldrick, G.M., 2007)' _exptl_special_details ; We are grateful for the EPSRC Crystallographic Service for recording the data for Cl1. The data collection nominally covered over a hemisphere of Reciprocal space, by a combination of three sets of exposures with different \f angles for the crystal; each 10 s exposure covered 0.3\% in \w. The crystal-to-detector distance was 5.0 cm. Coverage of the unique Set is over 97% complete to at least 26\% in \q. 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 amine hydrogen which was located in a difference map. This was allowed to refine freely but given thermal paramaters equal to 1.5 times the nitrogen to which it was attached. 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 and NH H-atoms) times the equivalent isotropic displacement parameter of the atom to which they are attached. ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-Nonius Roper CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% nil _diffrn_reflns_number 21250 _diffrn_reflns_av_R_equivalents 0.0594 _diffrn_reflns_av_sigmaI/netI 0.0659 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -45 _diffrn_reflns_limit_l_max 45 _diffrn_reflns_theta_min 2.94 _diffrn_reflns_theta_max 27.48 _reflns_number_total 6734 _reflns_number_gt 5765 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' #Although determined using DirAx, the cell is refined in the HKL #package during data reduction _computing_data_reduction 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' _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^)+(0.0265P)^2^+3.2074P] 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, 2879 Friedel pairs' _refine_ls_abs_structure_Flack 0.01(3) _chemical_absolute_configuration rmad _refine_ls_number_reflns 6734 _refine_ls_number_parameters 366 _refine_ls_number_restraints 13 _refine_ls_R_factor_all 0.0535 _refine_ls_R_factor_gt 0.0392 _refine_ls_wR_factor_ref 0.0876 _refine_ls_wR_factor_gt 0.0826 _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_restrained_S_all 1.072 _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 Cl1 Cl -0.65420(13) 0.07721(9) 0.28327(3) 0.0278(2) Uani 1 1 d . . . Ru1 Ru -0.38600(4) 0.15281(3) 0.317567(9) 0.01960(8) Uani 1 1 d . . . C1 C -0.6059(10) 0.1087(5) 0.55770(14) 0.0601(16) Uani 1 1 d U . . H1A H -0.6473 0.0362 0.5677 0.090 Uiso 1 1 calc R . . H1B H -0.6797 0.1684 0.5698 0.090 Uiso 1 1 calc R . . H1C H -0.4714 0.1194 0.5634 0.090 Uiso 1 1 calc R . . C2 C -0.6361(7) 0.1119(4) 0.51453(13) 0.0404(12) Uani 1 1 d . . . C3 C -0.7535(7) 0.0349(4) 0.49703(13) 0.0355(11) Uani 1 1 d . . . H3A H -0.8180 -0.0188 0.5122 0.043 Uiso 1 1 calc R . . C4 C -0.7788(6) 0.0347(4) 0.45761(13) 0.0305(10) Uani 1 1 d . . . H4A H -0.8608 -0.0181 0.4459 0.037 Uiso 1 1 calc R . . C5 C -0.6821(6) 0.1134(4) 0.43528(12) 0.0251(9) Uani 1 1 d . . . C6 C -0.5669(6) 0.1913(4) 0.45299(13) 0.0332(11) Uani 1 1 d . . . H6A H -0.5025 0.2455 0.4380 0.040 Uiso 1 1 calc R . . C7 C -0.5448(7) 0.1911(4) 0.49215(13) 0.0372(12) Uani 1 1 d . . . H7A H -0.4664 0.2456 0.5039 0.045 Uiso 1 1 calc R . . S8 S -0.70162(14) 0.11121(9) 0.38445(3) 0.0234(2) Uani 1 1 d . . . O9 O -0.7388(4) 0.2251(3) 0.37347(8) 0.0285(7) Uani 1 1 d D . . O10 O -0.8485(4) 0.0301(3) 0.37587(8) 0.0293(7) Uani 1 1 d . . . N11 N -0.4973(5) 0.0764(3) 0.36853(10) 0.0207(7) Uani 1 1 d . . . C12 C -0.4607(6) -0.0455(4) 0.36955(12) 0.0231(9) Uani 1 1 d . . . H12A H -0.5645 -0.0849 0.3556 0.028 Uiso 1 1 calc R . . C13 C -0.2719(6) -0.0673(3) 0.34879(12) 0.0218(9) Uani 1 1 d . . . H13A H -0.1696 -0.0278 0.3632 0.026 Uiso 1 1 calc R . . N14 N -0.2872(5) -0.0149(3) 0.30985(10) 0.0212(8) Uani 1 1 d . . . H14 H -0.374(8) -0.050(4) 0.2962(12) 0.032 Uiso 1 1 d . . . C15 C -0.1076(6) -0.0341(4) 0.28754(11) 0.0256(9) Uani 1 1 d . . . H15A H -0.0574 -0.1090 0.2939 0.031 Uiso 1 1 calc R . . H15B H -0.0123 0.0218 0.2956 0.031 Uiso 1 1 calc R . . C16 C -0.1337(7) -0.0263(4) 0.24428(12) 0.0323(10) Uani 1 1 d . . . H16A H -0.0078 -0.0367 0.2324 0.039 Uiso 1 1 calc R . . H16B H -0.2126 -0.0906 0.2363 0.039 Uiso 1 1 calc R . . C17 C -0.2208(6) 0.0783(4) 0.22683(12) 0.0312(10) Uani 1 1 d . . . H17A H -0.3558 0.0815 0.2343 0.037 Uiso 1 1 calc R . . H17B H -0.2156 0.0715 0.1986 0.037 Uiso 1 1 calc R . . C18 C -0.1262(7) 0.1894(4) 0.23839(11) 0.0297(9) Uani 1 1 d . . . H18A H 0.0118 0.1773 0.2407 0.036 Uiso 1 1 calc R . . H18B H -0.1468 0.2448 0.2178 0.036 Uiso 1 1 calc R . . C19 C -0.2001(6) 0.2373(4) 0.27576(13) 0.0276(10) Uani 1 1 d . . . C20 C -0.1021(6) 0.2253(3) 0.31128(11) 0.0246(9) Uani 1 1 d . . . H20A H 0.0196 0.1917 0.3114 0.030 Uiso 1 1 calc R . . C21 C -0.1802(6) 0.2617(3) 0.34604(13) 0.0256(9) Uani 1 1 d . . . H21A H -0.1123 0.2519 0.3692 0.031 Uiso 1 1 calc R . . C22 C -0.3598(7) 0.3129(3) 0.34639(12) 0.0285(10) Uani 1 1 d . . . H22A H -0.4131 0.3370 0.3699 0.034 Uiso 1 1 calc R . . C23 C -0.4609(6) 0.3286(3) 0.31209(13) 0.0296(10) Uani 1 1 d . . . H23A H -0.5807 0.3645 0.3123 0.036 Uiso 1 1 calc R . . C24 C -0.3817(7) 0.2901(3) 0.27713(12) 0.0286(9) Uani 1 1 d . . . H24A H -0.4511 0.2997 0.2541 0.034 Uiso 1 1 calc R . . C25 C -0.2248(6) -0.1901(3) 0.34803(12) 0.0224(9) Uani 1 1 d . . . C26 C -0.3347(6) -0.2690(4) 0.32877(12) 0.0300(10) Uani 1 1 d . . . H26A H -0.4439 -0.2446 0.3153 0.036 Uiso 1 1 calc R . . C27 C -0.2901(7) -0.3811(4) 0.32863(13) 0.0337(11) Uani 1 1 d . . . H27A H -0.3664 -0.4326 0.3149 0.040 Uiso 1 1 calc R . . C28 C -0.1325(7) -0.4182(4) 0.34875(13) 0.0339(10) Uani 1 1 d . . . H28A H -0.1018 -0.4955 0.3493 0.041 Uiso 1 1 calc R . . C29 C -0.0208(6) -0.3416(4) 0.36790(13) 0.0333(10) Uani 1 1 d . . . H29A H 0.0878 -0.3667 0.3814 0.040 Uiso 1 1 calc R . . C30 C -0.0652(6) -0.2286(4) 0.36766(13) 0.0274(10) Uani 1 1 d . . . H30A H 0.0133 -0.1771 0.3809 0.033 Uiso 1 1 calc R . . C31 C -0.4437(6) -0.0951(4) 0.40973(12) 0.0289(10) Uani 1 1 d . . . C32 C -0.5396(7) -0.1924(4) 0.41915(15) 0.0374(12) Uani 1 1 d . . . H32A H -0.6209 -0.2264 0.4009 0.045 Uiso 1 1 calc R . . C33 C -0.5180(9) -0.2405(5) 0.45498(18) 0.0572(17) Uani 1 1 d . . . H33A H -0.5827 -0.3077 0.4611 0.069 Uiso 1 1 calc R . . C34 C -0.4019(9) -0.1904(5) 0.48185(16) 0.0581(16) Uani 1 1 d U . . H34A H -0.3889 -0.2222 0.5066 0.070 Uiso 1 1 calc R . . C35 C -0.3062(7) -0.0950(5) 0.47266(14) 0.0484(14) Uani 1 1 d . . . H35A H -0.2258 -0.0610 0.4911 0.058 Uiso 1 1 calc R . . C36 C -0.3252(6) -0.0467(4) 0.43641(13) 0.0327(11) Uani 1 1 d . . . H36A H -0.2567 0.0191 0.4302 0.039 Uiso 1 1 calc R . . O01 O -0.7262(10) 0.4574(5) 0.37990(19) 0.0362(16) Uani 0.50 1 d PD . . C01 C -0.6367(15) 0.4924(8) 0.4133(3) 0.042(2) Uani 0.50 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cl1 0.0139(5) 0.0443(6) 0.0253(5) -0.0011(4) -0.0039(4) -0.0045(4) Ru1 0.01384(13) 0.02435(15) 0.02063(14) 0.00296(14) -0.00283(13) -0.00298(14) C1 0.059(3) 0.091(4) 0.030(2) -0.001(3) 0.002(3) 0.004(3) C2 0.031(3) 0.061(3) 0.029(2) -0.003(2) 0.002(2) 0.007(2) C3 0.031(3) 0.045(3) 0.030(2) 0.007(2) 0.009(2) 0.001(2) C4 0.021(2) 0.041(3) 0.029(2) 0.000(2) 0.0044(19) -0.0025(19) C5 0.0180(19) 0.033(2) 0.024(2) 0.0000(18) 0.0023(17) -0.0013(17) C6 0.026(2) 0.045(3) 0.028(2) 0.002(2) -0.0001(19) -0.0116(19) C7 0.034(3) 0.052(3) 0.026(2) -0.008(2) -0.002(2) -0.005(2) S8 0.0149(5) 0.0332(6) 0.0220(5) 0.0004(4) -0.0011(4) -0.0032(4) O9 0.0230(16) 0.0353(18) 0.0272(16) 0.0023(14) -0.0007(13) 0.0027(13) O10 0.0158(15) 0.0422(18) 0.0299(16) -0.0028(13) -0.0019(12) -0.0072(13) N11 0.0138(16) 0.0252(19) 0.0232(18) 0.0045(14) 0.0003(14) -0.0024(14) C12 0.0135(18) 0.028(2) 0.028(2) 0.0049(18) -0.0009(16) -0.0028(16) C13 0.017(2) 0.025(2) 0.023(2) 0.0022(17) -0.0023(17) -0.0045(17) N14 0.0143(16) 0.0263(19) 0.023(2) 0.0010(14) 0.0001(14) -0.0051(14) C15 0.0166(19) 0.031(2) 0.029(2) 0.0007(17) 0.0036(19) -0.002(2) C16 0.029(2) 0.039(3) 0.029(2) -0.0028(19) 0.004(2) -0.005(2) C17 0.021(2) 0.050(3) 0.023(2) 0.002(2) 0.0036(18) -0.004(2) C18 0.024(2) 0.039(2) 0.026(2) 0.0092(17) 0.005(2) -0.005(2) C19 0.022(2) 0.029(2) 0.032(2) 0.0091(19) 0.0055(19) -0.0087(18) C20 0.0156(18) 0.024(2) 0.035(2) 0.0054(16) 0.0009(19) -0.0093(17) C21 0.023(2) 0.024(2) 0.030(2) -0.0001(18) -0.0091(18) -0.0117(17) C22 0.033(3) 0.024(2) 0.029(2) -0.0021(16) -0.001(2) -0.0008(19) C23 0.028(2) 0.023(2) 0.038(3) 0.009(2) -0.0018(19) 0.0000(17) C24 0.028(2) 0.034(2) 0.024(2) 0.0101(18) -0.004(2) -0.001(2) C25 0.019(2) 0.025(2) 0.024(2) 0.0002(17) 0.0010(17) -0.0026(16) C26 0.029(2) 0.029(2) 0.032(2) 0.0016(18) -0.0076(18) -0.0033(18) C27 0.036(3) 0.030(3) 0.034(3) -0.0005(19) -0.006(2) -0.012(2) C28 0.034(3) 0.026(2) 0.042(3) 0.0017(19) 0.006(2) -0.001(2) C29 0.027(2) 0.035(3) 0.038(2) 0.002(2) 0.0007(19) 0.005(2) C30 0.022(2) 0.029(2) 0.031(2) -0.0011(19) -0.0051(18) 0.0005(18) C31 0.020(2) 0.041(3) 0.026(2) 0.008(2) 0.0030(17) 0.0036(19) C32 0.026(2) 0.041(3) 0.045(3) 0.015(2) 0.005(2) -0.002(2) C33 0.050(3) 0.062(4) 0.060(4) 0.034(3) 0.013(3) 0.001(3) C34 0.052(3) 0.077(4) 0.045(3) 0.031(3) 0.007(3) 0.009(3) C35 0.035(3) 0.079(4) 0.031(3) 0.016(3) -0.003(2) 0.007(3) C36 0.021(2) 0.049(3) 0.028(2) 0.006(2) -0.0005(18) 0.006(2) O01 0.036(4) 0.029(3) 0.044(4) -0.001(3) 0.004(3) 0.013(3) C01 0.035(6) 0.038(5) 0.053(6) -0.014(5) -0.013(5) 0.003(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cl1 Ru1 2.4193(10) . ? Ru1 N14 2.141(3) . ? Ru1 N11 2.152(3) . ? Ru1 C24 2.168(4) . ? Ru1 C22 2.172(4) . ? Ru1 C23 2.177(4) . ? Ru1 C21 2.192(4) . ? Ru1 C20 2.198(4) . ? Ru1 C19 2.211(4) . ? C1 C2 1.525(6) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C3 1.383(7) . ? C2 C7 1.388(7) . ? C3 C4 1.390(6) . ? C3 H3A 0.9500 . ? C4 C5 1.401(6) . ? C4 H4A 0.9500 . ? C5 C6 1.384(6) . ? C5 S8 1.783(4) . ? C6 C7 1.379(6) . ? C6 H6A 0.9500 . ? C7 H7A 0.9500 . ? S8 O9 1.440(3) . ? S8 O10 1.453(3) . ? S8 N11 1.604(3) . ? N11 C12 1.482(5) . ? C12 C31 1.530(6) . ? C12 C13 1.542(5) . ? C12 H12A 1.0000 . ? C13 N14 1.504(5) . ? C13 C25 1.507(6) . ? C13 H13A 1.0000 . ? N14 C15 1.508(5) . ? N14 H14 0.88(5) . ? C15 C16 1.527(6) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.523(6) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.542(6) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C19 1.520(6) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.429(6) . ? C19 C24 1.432(6) . ? C20 C21 1.405(6) . ? C20 H20A 0.9500 . ? C21 C22 1.409(6) . ? C21 H21A 0.9500 . ? C22 C23 1.409(6) . ? C22 H22A 0.9500 . ? C23 C24 1.421(6) . ? C23 H23A 0.9500 . ? C24 H24A 0.9500 . ? C25 C26 1.396(6) . ? C25 C30 1.399(6) . ? C26 C27 1.377(6) . ? C26 H26A 0.9500 . ? C27 C28 1.391(7) . ? C27 H27A 0.9500 . ? C28 C29 1.383(7) . ? C28 H28A 0.9500 . ? C29 C30 1.388(7) . ? C29 H29A 0.9500 . ? C30 H30A 0.9500 . ? C31 C36 1.382(6) . ? C31 C32 1.387(6) . ? C32 C33 1.387(7) . ? C32 H32A 0.9500 . ? C33 C34 1.384(9) . ? C33 H33A 0.9500 . ? C34 C35 1.365(8) . ? C34 H34A 0.9500 . ? C35 C36 1.399(6) . ? C35 H35A 0.9500 . ? C36 H36A 0.9500 . ? O01 C01 1.393(11) . ? 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 N14 Ru1 N11 79.95(13) . . ? N14 Ru1 C24 128.55(15) . . ? N11 Ru1 C24 150.15(15) . . ? N14 Ru1 C22 148.95(15) . . ? N11 Ru1 C22 91.24(15) . . ? C24 Ru1 C22 68.49(16) . . ? N14 Ru1 C23 166.71(15) . . ? N11 Ru1 C23 113.23(15) . . ? C24 Ru1 C23 38.19(16) . . ? C22 Ru1 C23 37.80(16) . . ? N14 Ru1 C21 113.43(15) . . ? N11 Ru1 C21 96.83(15) . . ? C24 Ru1 C21 80.60(17) . . ? C22 Ru1 C21 37.68(17) . . ? C23 Ru1 C21 68.11(16) . . ? N14 Ru1 C20 93.40(14) . . ? N11 Ru1 C20 125.77(14) . . ? C24 Ru1 C20 67.84(17) . . ? C22 Ru1 C20 67.69(16) . . ? C23 Ru1 C20 80.33(16) . . ? C21 Ru1 C20 37.32(15) . . ? N14 Ru1 C19 98.70(15) . . ? N11 Ru1 C19 163.61(14) . . ? C24 Ru1 C19 38.16(17) . . ? C22 Ru1 C19 81.54(17) . . ? C23 Ru1 C19 69.18(17) . . ? C21 Ru1 C19 68.53(17) . . ? C20 Ru1 C19 37.84(15) . . ? N14 Ru1 Cl1 80.96(10) . . ? N11 Ru1 Cl1 88.01(9) . . ? C24 Ru1 Cl1 88.32(13) . . ? C22 Ru1 Cl1 128.80(13) . . ? C23 Ru1 Cl1 97.29(12) . . ? C21 Ru1 Cl1 165.37(12) . . ? C20 Ru1 Cl1 144.47(11) . . ? C19 Ru1 Cl1 108.01(12) . . ? 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 118.9(4) . . ? C3 C2 C1 120.4(5) . . ? C7 C2 C1 120.7(5) . . ? C2 C3 C4 121.2(5) . . ? C2 C3 H3A 119.4 . . ? C4 C3 H3A 119.4 . . ? C3 C4 C5 119.3(4) . . ? C3 C4 H4A 120.4 . . ? C5 C4 H4A 120.4 . . ? C6 C5 C4 119.4(4) . . ? C6 C5 S8 120.1(3) . . ? C4 C5 S8 120.5(3) . . ? C7 C6 C5 120.6(4) . . ? C7 C6 H6A 119.7 . . ? C5 C6 H6A 119.7 . . ? C6 C7 C2 120.6(5) . . ? C6 C7 H7A 119.7 . . ? C2 C7 H7A 119.7 . . ? O9 S8 O10 116.55(18) . . ? O9 S8 N11 108.53(19) . . ? O10 S8 N11 113.48(18) . . ? O9 S8 C5 105.43(19) . . ? O10 S8 C5 105.74(19) . . ? N11 S8 C5 106.26(18) . . ? C12 N11 S8 113.9(3) . . ? C12 N11 Ru1 112.0(3) . . ? S8 N11 Ru1 120.43(19) . . ? N11 C12 C31 114.7(4) . . ? N11 C12 C13 107.8(3) . . ? C31 C12 C13 107.4(3) . . ? N11 C12 H12A 108.9 . . ? C31 C12 H12A 108.9 . . ? C13 C12 H12A 108.9 . . ? N14 C13 C25 114.0(3) . . ? N14 C13 C12 107.1(3) . . ? C25 C13 C12 111.4(3) . . ? N14 C13 H13A 108.1 . . ? C25 C13 H13A 108.1 . . ? C12 C13 H13A 108.1 . . ? C13 N14 C15 110.2(3) . . ? C13 N14 Ru1 107.5(2) . . ? C15 N14 Ru1 118.9(2) . . ? C13 N14 H14 110(3) . . ? C15 N14 H14 103(3) . . ? Ru1 N14 H14 107(3) . . ? N14 C15 C16 113.7(4) . . ? N14 C15 H15A 108.8 . . ? C16 C15 H15A 108.8 . . ? N14 C15 H15B 108.8 . . ? C16 C15 H15B 108.8 . . ? H15A C15 H15B 107.7 . . ? C17 C16 C15 119.7(4) . . ? C17 C16 H16A 107.4 . . ? C15 C16 H16A 107.4 . . ? C17 C16 H16B 107.4 . . ? C15 C16 H16B 107.4 . . ? H16A C16 H16B 106.9 . . ? C16 C17 C18 115.4(4) . . ? C16 C17 H17A 108.4 . . ? C18 C17 H17A 108.4 . . ? C16 C17 H17B 108.4 . . ? C18 C17 H17B 108.4 . . ? H17A C17 H17B 107.5 . . ? C19 C18 C17 113.7(3) . . ? C19 C18 H18A 108.8 . . ? C17 C18 H18A 108.8 . . ? C19 C18 H18B 108.8 . . ? C17 C18 H18B 108.8 . . ? H18A C18 H18B 107.7 . . ? C20 C19 C24 116.7(4) . . ? C20 C19 C18 122.9(4) . . ? C24 C19 C18 120.2(4) . . ? C20 C19 Ru1 70.6(2) . . ? C24 C19 Ru1 69.3(2) . . ? C18 C19 Ru1 126.9(3) . . ? C21 C20 C19 122.0(4) . . ? C21 C20 Ru1 71.1(2) . . ? C19 C20 Ru1 71.6(2) . . ? C21 C20 H20A 119.0 . . ? C19 C20 H20A 119.0 . . ? Ru1 C20 H20A 131.3 . . ? C20 C21 C22 119.7(4) . . ? C20 C21 Ru1 71.5(2) . . ? C22 C21 Ru1 70.4(2) . . ? C20 C21 H21A 120.1 . . ? C22 C21 H21A 120.1 . . ? Ru1 C21 H21A 130.5 . . ? C23 C22 C21 120.5(4) . . ? C23 C22 Ru1 71.3(2) . . ? C21 C22 Ru1 71.9(2) . . ? C23 C22 H22A 119.7 . . ? C21 C22 H22A 119.7 . . ? Ru1 C22 H22A 129.5 . . ? C22 C23 C24 119.3(4) . . ? C22 C23 Ru1 70.9(2) . . ? C24 C23 Ru1 70.6(2) . . ? C22 C23 H23A 120.4 . . ? C24 C23 H23A 120.4 . . ? Ru1 C23 H23A 130.8 . . ? C23 C24 C19 121.6(4) . . ? C23 C24 Ru1 71.3(2) . . ? C19 C24 Ru1 72.5(2) . . ? C23 C24 H24A 119.2 . . ? C19 C24 H24A 119.2 . . ? Ru1 C24 H24A 129.6 . . ? C26 C25 C30 117.6(4) . . ? C26 C25 C13 123.0(4) . . ? C30 C25 C13 119.4(4) . . ? C27 C26 C25 122.2(4) . . ? C27 C26 H26A 118.9 . . ? C25 C26 H26A 118.9 . . ? C26 C27 C28 119.5(4) . . ? C26 C27 H27A 120.2 . . ? C28 C27 H27A 120.2 . . ? C29 C28 C27 119.4(4) . . ? C29 C28 H28A 120.3 . . ? C27 C28 H28A 120.3 . . ? C28 C29 C30 120.9(4) . . ? C28 C29 H29A 119.6 . . ? C30 C29 H29A 119.6 . . ? C29 C30 C25 120.4(4) . . ? C29 C30 H30A 119.8 . . ? C25 C30 H30A 119.8 . . ? C36 C31 C32 119.2(4) . . ? C36 C31 C12 120.4(4) . . ? C32 C31 C12 120.4(4) . . ? C31 C32 C33 120.6(5) . . ? C31 C32 H32A 119.7 . . ? C33 C32 H32A 119.7 . . ? C34 C33 C32 120.0(5) . . ? C34 C33 H33A 120.0 . . ? C32 C33 H33A 120.0 . . ? C35 C34 C33 119.7(5) . . ? C35 C34 H34A 120.1 . . ? C33 C34 H34A 120.1 . . ? C34 C35 C36 120.7(5) . . ? C34 C35 H35A 119.7 . . ? C36 C35 H35A 119.7 . . ? C31 C36 C35 119.8(5) . . ? C31 C36 H36A 120.1 . . ? C35 C36 H36A 120.1 . . ? 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 N14 H14 Cl1 0.88(5) 2.54(5) 2.968(4) 111(3) . _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.599 _refine_diff_density_min -0.883 _refine_diff_density_rms 0.084 # Attachment 'kc1new compound RR-5.cif' data_kc1 _database_code_depnum_ccdc_archive 'CCDC 741013' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C31.50 H34 Cl2 N2 O2 Ru S' _chemical_formula_weight 676.64 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 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 13.2206(17) _cell_length_b 17.179(2) _cell_length_c 25.789(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5857.2(13) _cell_formula_units_Z 8 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 2776 _cell_measurement_theta_min 2.20 _cell_measurement_theta_max 27.71 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.535 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2776 _exptl_absorpt_coefficient_mu 0.822 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7346 _exptl_absorpt_correction_T_max 0.8662 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; The temperature of the crystal was controlled using the Oxford Cryosystem Cryostream Cooler (Cosier & Glazer, 1986). The data collection nominally covered over a hemisphere of Reciprocal space, by a combination of three sets of exposures with different \f angles for the crystal; each 10 s exposure covered 0.3\% in \w. The crystal-to-detector distance was 5.0 cm. Coverage of the unique Set is over 97% complete to at least 26\% in \q. 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 amine hydrogens which were located in a difference map. These were allowed to refine freely but given thermal paramaters equal to 1.5 times the nitrogen to which they were attached. 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 and NH H-atoms) times the equivalent isotropic displacement parameter of the atom to which they are attached. ; _diffrn_ambient_temperature 180(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 'Siemens SMART diffractometer' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 8.192 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% nil _diffrn_reflns_number 58808 _diffrn_reflns_av_R_equivalents 0.0570 _diffrn_reflns_av_sigmaI/netI 0.0571 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 1.42 _diffrn_reflns_theta_max 29.20 _reflns_number_total 14480 _reflns_number_gt 11570 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Siemens, 1994)' _computing_cell_refinement 'SAINT (Siemens, 1995)' _computing_data_reduction 'SAINT (Siemens, 1995)' _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^)+(0.0668P)^2^+2.5821P] 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, 8164 Friedel Pairs' _refine_ls_abs_structure_Flack 0.02(3) _chemical_absolute_configuration rmad _refine_ls_number_reflns 14480 _refine_ls_number_parameters 722 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0714 _refine_ls_R_factor_gt 0.0513 _refine_ls_wR_factor_ref 0.1231 _refine_ls_wR_factor_gt 0.1150 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.043 _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 0.01140(3) 0.83631(2) 0.985170(13) 0.02643(9) Uani 1 1 d . . . Cl1 Cl 0.18497(9) 0.87633(8) 1.00359(5) 0.0409(3) Uani 1 1 d . . . C101 C -0.1723(5) 0.5018(3) 1.2213(2) 0.0535(16) Uani 1 1 d . . . H10A H -0.2436 0.5167 1.2241 0.080 Uiso 1 1 calc R . . H10B H -0.1412 0.5025 1.2558 0.080 Uiso 1 1 calc R . . H10C H -0.1673 0.4494 1.2066 0.080 Uiso 1 1 calc R . . C102 C -0.1177(5) 0.5589(3) 1.1864(2) 0.0416(13) Uani 1 1 d . . . C103 C -0.0185(5) 0.5823(3) 1.1998(2) 0.0538(16) Uani 1 1 d . . . H10D H 0.0121 0.5623 1.2303 0.065 Uiso 1 1 calc R . . C104 C 0.0342(5) 0.6338(3) 1.1690(2) 0.0503(15) Uani 1 1 d . . . H10E H 0.0999 0.6505 1.1789 0.060 Uiso 1 1 calc R . . C105 C -0.0091(4) 0.6614(3) 1.12334(17) 0.0356(10) Uani 1 1 d . . . C106 C -0.1053(4) 0.6399(3) 1.1102(2) 0.0378(12) Uani 1 1 d . . . H10F H -0.1353 0.6597 1.0795 0.045 Uiso 1 1 calc R . . C107 C -0.1595(4) 0.5891(3) 1.1419(2) 0.0396(12) Uani 1 1 d . . . H10G H -0.2266 0.5751 1.1326 0.048 Uiso 1 1 calc R . . S108 S 0.06759(10) 0.71937(7) 1.08083(5) 0.0345(3) Uani 1 1 d . . . O18A O 0.1568(3) 0.7395(2) 1.11007(14) 0.0413(8) Uani 1 1 d . . . O18B O 0.0817(3) 0.6695(2) 1.03629(13) 0.0465(9) Uani 1 1 d . . . N109 N 0.0034(3) 0.7948(2) 1.06345(14) 0.0291(8) Uani 1 1 d . . . C110 C 0.0087(4) 0.8598(2) 1.10199(16) 0.0274(9) Uani 1 1 d . . . H11A H 0.0799 0.8793 1.1034 0.033 Uiso 1 1 calc R . . C111 C -0.0587(3) 0.9243(2) 1.08008(17) 0.0259(9) Uani 1 1 d . . . H11B H -0.1290 0.9032 1.0781 0.031 Uiso 1 1 calc R . . N112 N -0.0254(3) 0.9414(2) 1.02625(14) 0.0260(8) Uani 1 1 d D . . H112 H 0.032(2) 0.963(3) 1.026(2) 0.039 Uiso 1 1 d D . . C113 C -0.0922(4) 0.9978(3) 1.00044(18) 0.0321(10) Uani 1 1 d . . . H11C H -0.0569 1.0187 0.9696 0.038 Uiso 1 1 calc R . . H11D H -0.1046 1.0418 1.0244 0.038 Uiso 1 1 calc R . . C114 C -0.1939(4) 0.9645(3) 0.9834(2) 0.0380(11) Uani 1 1 d . . . H11E H -0.2181 0.9278 1.0103 0.046 Uiso 1 1 calc R . . H11F H -0.2436 1.0074 0.9811 0.046 Uiso 1 1 calc R . . C115 C -0.1904(4) 0.9226(3) 0.9320(2) 0.0419(12) Uani 1 1 d . . . H11G H -0.1767 0.9610 0.9043 0.050 Uiso 1 1 calc R . . H11H H -0.2576 0.8994 0.9251 0.050 Uiso 1 1 calc R . . C116 C -0.1104(4) 0.8586(3) 0.92963(19) 0.0337(11) Uani 1 1 d . . . C117 C -0.0159(4) 0.8745(3) 0.90566(18) 0.0388(12) Uani 1 1 d . . . H11I H -0.0048 0.9232 0.8891 0.047 Uiso 1 1 calc R . . C118 C 0.0600(4) 0.8191(3) 0.90642(19) 0.0424(13) Uani 1 1 d . . . H11J H 0.1240 0.8319 0.8919 0.051 Uiso 1 1 calc R . . C119 C 0.0463(4) 0.7433(3) 0.92810(19) 0.0388(12) Uani 1 1 d . . . C120 C -0.0473(4) 0.7282(3) 0.95110(18) 0.0361(11) Uani 1 1 d . . . H12I H -0.0589 0.6785 0.9661 0.043 Uiso 1 1 calc R . . C121 C -0.1264(4) 0.7851(3) 0.95285(18) 0.0325(10) Uani 1 1 d . . . H12J H -0.1888 0.7735 0.9694 0.039 Uiso 1 1 calc R . . C122 C 0.1325(5) 0.6861(4) 0.9263(2) 0.0520(16) Uani 1 1 d . . . H12A H 0.1443 0.6700 0.8904 0.078 Uiso 1 1 calc R . . H12B H 0.1155 0.6403 0.9473 0.078 Uiso 1 1 calc R . . H12C H 0.1937 0.7106 0.9401 0.078 Uiso 1 1 calc R . . C123 C -0.0619(4) 0.9963(3) 1.11457(17) 0.0280(10) Uani 1 1 d . . . C124 C 0.0196(4) 1.0482(3) 1.11555(19) 0.0385(11) Uani 1 1 d . . . H12D H 0.0789 1.0370 1.0961 0.046 Uiso 1 1 calc R . . C125 C 0.0143(5) 1.1163(3) 1.1450(2) 0.0446(13) Uani 1 1 d . . . H12E H 0.0692 1.1521 1.1449 0.054 Uiso 1 1 calc R . . C126 C -0.0698(5) 1.1314(3) 1.1739(2) 0.0509(15) Uani 1 1 d . . . H12F H -0.0729 1.1773 1.1944 0.061 Uiso 1 1 calc R . . C127 C -0.1510(5) 1.0800(4) 1.1736(2) 0.0511(15) Uani 1 1 d . . . H12G H -0.2094 1.0905 1.1939 0.061 Uiso 1 1 calc R . . C128 C -0.1458(4) 1.0130(3) 1.1434(2) 0.0406(12) Uani 1 1 d . . . H12H H -0.2017 0.9783 1.1427 0.049 Uiso 1 1 calc R . . C129 C -0.0244(4) 0.8384(3) 1.15644(16) 0.0309(9) Uani 1 1 d . . . C130 C 0.0417(4) 0.8465(3) 1.19794(19) 0.0408(12) Uani 1 1 d . . . H13A H 0.1086 0.8645 1.1922 0.049 Uiso 1 1 calc R . . C131 C 0.0099(5) 0.8280(3) 1.24846(19) 0.0509(14) Uani 1 1 d . . . H13B H 0.0561 0.8331 1.2765 0.061 Uiso 1 1 calc R . . C132 C -0.0849(5) 0.8032(3) 1.2576(2) 0.0527(16) Uani 1 1 d . . . H13C H -0.1053 0.7901 1.2918 0.063 Uiso 1 1 calc R . . C133 C -0.1531(5) 0.7968(3) 1.2166(2) 0.0506(15) Uani 1 1 d . . . H13D H -0.2211 0.7815 1.2230 0.061 Uiso 1 1 calc R . . C134 C -0.1216(4) 0.8128(3) 1.1668(2) 0.0385(12) Uani 1 1 d . . . H13E H -0.1677 0.8062 1.1389 0.046 Uiso 1 1 calc R . . Ru2 Ru 0.31460(2) 1.16874(2) 0.978950(13) 0.02548(9) Uani 1 1 d . . . Cl2 Cl 0.14296(8) 1.12622(7) 0.99957(5) 0.0349(3) Uani 1 1 d . . . C201 C 0.5458(6) 1.4831(4) 1.2031(3) 0.071(2) Uani 1 1 d . . . H20A H 0.5085 1.5234 1.2220 0.107 Uiso 1 1 calc R . . H20B H 0.5945 1.5076 1.1796 0.107 Uiso 1 1 calc R . . H20C H 0.5819 1.4498 1.2279 0.107 Uiso 1 1 calc R . . C202 C 0.4737(5) 1.4350(3) 1.1726(2) 0.0470(15) Uani 1 1 d . . . C203 C 0.3780(5) 1.4151(4) 1.1919(2) 0.0495(15) Uani 1 1 d . . . H20D H 0.3572 1.4342 1.2248 0.059 Uiso 1 1 calc R . . C204 C 0.3132(5) 1.3677(3) 1.1635(2) 0.0429(12) Uani 1 1 d . . . H20E H 0.2485 1.3543 1.1769 0.052 Uiso 1 1 calc R . . C205 C 0.3438(4) 1.3399(3) 1.11538(17) 0.0325(10) Uani 1 1 d . . . C206 C 0.4379(4) 1.3589(3) 1.09612(19) 0.0349(11) Uani 1 1 d . . . H20F H 0.4584 1.3392 1.0633 0.042 Uiso 1 1 calc R . . C207 C 0.5031(4) 1.4066(3) 1.1243(2) 0.0407(12) Uani 1 1 d . . . H20G H 0.5675 1.4197 1.1105 0.049 Uiso 1 1 calc R . . S208 S 0.25896(9) 1.28183(7) 1.07768(4) 0.0290(2) Uani 1 1 d . . . O28A O 0.1774(3) 1.26052(18) 1.11220(13) 0.0365(8) Uani 1 1 d . . . O28B O 0.2337(3) 1.3300(2) 1.03395(13) 0.0406(8) Uani 1 1 d . . . N209 N 0.3227(3) 1.2081(2) 1.05768(14) 0.0290(8) Uani 1 1 d . . . C210 C 0.3257(4) 1.1421(2) 1.09511(17) 0.0289(10) Uani 1 1 d . . . H21A H 0.2561 1.1198 1.0981 0.035 Uiso 1 1 calc R . . C211 C 0.3947(3) 1.0809(3) 1.07059(17) 0.0287(10) Uani 1 1 d . . . H21B H 0.4626 1.1055 1.0658 0.034 Uiso 1 1 calc R . . N212 N 0.3551(3) 1.0628(2) 1.01834(16) 0.0276(8) Uani 1 1 d D . . H212 H 0.297(2) 1.044(3) 1.021(2) 0.041 Uiso 1 1 d D . . C213 C 0.4189(4) 1.0046(3) 0.98950(19) 0.0325(10) Uani 1 1 d . . . H21C H 0.3799 0.9848 0.9595 0.039 Uiso 1 1 calc R . . H21D H 0.4331 0.9600 1.0127 0.039 Uiso 1 1 calc R . . C214 C 0.5188(4) 1.0373(3) 0.97005(19) 0.0363(11) Uani 1 1 d . . . H21E H 0.5670 0.9939 0.9651 0.044 Uiso 1 1 calc R . . H21F H 0.5472 1.0723 0.9969 0.044 Uiso 1 1 calc R . . C215 C 0.5097(4) 1.0823(3) 0.9193(2) 0.0415(12) Uani 1 1 d . . . H21G H 0.5765 1.1047 0.9106 0.050 Uiso 1 1 calc R . . H21H H 0.4913 1.0454 0.8913 0.050 Uiso 1 1 calc R . . C216 C 0.4330(4) 1.1467(3) 0.92038(18) 0.0333(11) Uani 1 1 d . . . C217 C 0.3363(4) 1.1354(3) 0.89765(18) 0.0372(12) Uani 1 1 d . . . H21I H 0.3217 1.0880 0.8801 0.045 Uiso 1 1 calc R . . C218 C 0.2624(4) 1.1934(3) 0.90086(19) 0.0361(12) Uani 1 1 d . . . H21J H 0.1973 1.1836 0.8866 0.043 Uiso 1 1 calc R . . C219 C 0.2816(4) 1.2671(3) 0.92497(19) 0.0351(11) Uani 1 1 d . . . C220 C 0.3762(4) 1.2773(3) 0.94789(19) 0.0343(11) Uani 1 1 d . . . H22I H 0.3902 1.3247 0.9655 0.041 Uiso 1 1 calc R . . C221 C 0.4530(4) 1.2187(3) 0.94582(19) 0.0326(10) Uani 1 1 d . . . H22J H 0.5171 1.2278 0.9614 0.039 Uiso 1 1 calc R . . C222 C 0.1996(4) 1.3284(3) 0.9247(2) 0.0435(12) Uani 1 1 d . . . H22A H 0.1808 1.3405 0.8889 0.065 Uiso 1 1 calc R . . H22B H 0.2245 1.3756 0.9418 0.065 Uiso 1 1 calc R . . H22C H 0.1402 1.3087 0.9434 0.065 Uiso 1 1 calc R . . C223 C 0.4095(4) 1.0101(3) 1.10486(18) 0.0307(10) Uani 1 1 d . . . C224 C 0.3321(4) 0.9566(3) 1.1121(2) 0.0409(12) Uani 1 1 d . . . H22D H 0.2697 0.9626 1.0943 0.049 Uiso 1 1 calc R . . C225 C 0.3465(5) 0.8942(3) 1.1457(2) 0.0544(16) Uani 1 1 d . . . H22E H 0.2928 0.8583 1.1512 0.065 Uiso 1 1 calc R . . C226 C 0.4358(6) 0.8837(4) 1.1705(2) 0.0555(17) Uani 1 1 d . . . H22F H 0.4450 0.8401 1.1927 0.067 Uiso 1 1 calc R . . C227 C 0.5121(6) 0.9356(4) 1.1635(2) 0.0556(17) Uani 1 1 d . . . H22G H 0.5744 0.9285 1.1812 0.067 Uiso 1 1 calc R . . C228 C 0.4997(4) 0.9992(3) 1.13080(19) 0.0417(12) Uani 1 1 d . . . H22H H 0.5534 1.0353 1.1263 0.050 Uiso 1 1 calc R . . C229 C 0.3626(4) 1.1632(3) 1.14922(17) 0.0341(10) Uani 1 1 d . . . C230 C 0.3031(4) 1.1459(3) 1.19230(19) 0.0406(12) Uani 1 1 d . . . H23A H 0.2383 1.1229 1.1877 0.049 Uiso 1 1 calc R . . C231 C 0.3378(5) 1.1621(3) 1.2417(2) 0.0511(15) Uani 1 1 d . . . H23B H 0.2979 1.1487 1.2710 0.061 Uiso 1 1 calc R . . C232 C 0.4287(6) 1.1970(3) 1.2484(2) 0.0552(16) Uani 1 1 d . . . H23C H 0.4509 1.2102 1.2823 0.066 Uiso 1 1 calc R . . C233 C 0.4899(5) 1.2138(3) 1.2058(2) 0.0515(15) Uani 1 1 d . . . H23D H 0.5542 1.2374 1.2108 0.062 Uiso 1 1 calc R . . C234 C 0.4572(4) 1.1963(3) 1.1568(2) 0.0385(12) Uani 1 1 d . . . H23E H 0.4995 1.2069 1.1279 0.046 Uiso 1 1 calc R . . C01 C 0.3084(6) 0.7006(4) 1.1982(3) 0.088(3) Uani 1 1 d D . . H01B H 0.2672 0.7113 1.1669 0.105 Uiso 1 1 calc R . . H01A H 0.3778 0.7197 1.1913 0.105 Uiso 1 1 calc R . . Cl3 Cl 0.25728(17) 0.75268(15) 1.25122(10) 0.0994(8) Uani 1 1 d D . . Cl4 Cl 0.3125(2) 0.60149(16) 1.20832(9) 0.1022(7) Uani 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.02920(17) 0.02417(17) 0.02593(17) -0.00277(16) 0.00086(14) -0.00275(15) Cl1 0.0301(6) 0.0487(7) 0.0440(7) -0.0114(5) 0.0012(5) -0.0043(5) C101 0.076(5) 0.035(3) 0.049(3) 0.003(2) 0.011(3) 0.002(3) C102 0.063(4) 0.021(2) 0.041(3) 0.000(2) 0.006(3) 0.001(2) C103 0.080(4) 0.040(3) 0.042(3) 0.010(2) -0.013(3) -0.005(3) C104 0.061(4) 0.042(3) 0.047(3) 0.013(2) -0.018(3) -0.010(3) C105 0.054(3) 0.017(2) 0.036(2) -0.0023(19) 0.001(2) 0.003(2) C106 0.053(3) 0.024(2) 0.037(3) -0.003(2) -0.008(2) 0.008(2) C107 0.050(3) 0.025(2) 0.044(3) -0.002(2) -0.001(2) 0.001(2) S108 0.0438(7) 0.0248(6) 0.0350(6) -0.0012(5) -0.0007(5) 0.0078(5) O18A 0.040(2) 0.0328(19) 0.051(2) 0.0031(16) 0.0002(17) 0.0103(16) O18B 0.066(2) 0.0312(18) 0.0427(19) -0.0036(17) 0.0004(17) 0.014(2) N109 0.037(2) 0.0216(19) 0.0282(19) -0.0036(14) -0.0009(17) 0.0076(17) C110 0.032(2) 0.019(2) 0.031(2) -0.0018(16) 0.0029(19) -0.0036(18) C111 0.027(2) 0.020(2) 0.031(2) -0.0011(17) 0.0011(19) 0.0003(17) N112 0.0312(19) 0.0208(18) 0.0261(18) -0.0014(14) 0.0000(16) -0.0034(15) C113 0.044(3) 0.026(2) 0.027(2) 0.0022(18) -0.0033(19) 0.000(2) C114 0.039(3) 0.032(2) 0.043(3) 0.007(2) 0.001(2) 0.006(2) C115 0.044(3) 0.034(3) 0.048(3) 0.005(2) -0.015(3) 0.000(2) C116 0.042(3) 0.028(2) 0.031(2) -0.0066(19) -0.011(2) -0.008(2) C117 0.048(3) 0.042(3) 0.026(2) 0.001(2) -0.003(2) -0.011(3) C118 0.041(3) 0.056(4) 0.030(3) -0.008(2) 0.005(2) -0.007(3) C119 0.051(3) 0.034(3) 0.031(3) -0.008(2) 0.002(2) 0.000(2) C120 0.049(3) 0.031(3) 0.029(2) -0.008(2) -0.009(2) -0.005(2) C121 0.038(3) 0.026(2) 0.034(3) 0.000(2) -0.009(2) -0.004(2) C122 0.053(3) 0.054(4) 0.049(3) -0.025(3) 0.002(3) 0.013(3) C123 0.035(2) 0.022(2) 0.027(2) 0.0011(18) 0.0012(19) 0.0033(19) C124 0.046(3) 0.032(3) 0.037(3) -0.005(2) 0.002(2) -0.001(2) C125 0.057(3) 0.031(3) 0.045(3) -0.002(2) -0.013(3) -0.004(3) C126 0.093(5) 0.021(3) 0.038(3) -0.009(2) -0.009(3) 0.010(3) C127 0.064(4) 0.046(3) 0.044(3) -0.013(3) 0.007(3) 0.020(3) C128 0.048(3) 0.035(3) 0.038(3) -0.002(2) 0.010(2) 0.002(2) C129 0.044(3) 0.017(2) 0.032(2) -0.0045(19) 0.0035(19) 0.003(2) C130 0.055(3) 0.032(3) 0.036(3) -0.001(2) 0.005(2) 0.002(2) C131 0.078(4) 0.044(3) 0.031(2) 0.004(2) -0.002(3) 0.007(3) C132 0.081(5) 0.038(3) 0.039(3) 0.009(2) 0.024(3) 0.010(3) C133 0.061(4) 0.031(3) 0.060(4) 0.008(3) 0.025(3) -0.003(3) C134 0.048(3) 0.027(3) 0.041(3) 0.002(2) 0.009(2) -0.003(2) Ru2 0.02816(17) 0.02155(16) 0.02673(17) -0.00060(16) -0.00003(14) -0.00278(15) Cl2 0.0286(5) 0.0390(6) 0.0371(6) 0.0043(5) -0.0004(5) -0.0046(5) C201 0.089(5) 0.077(5) 0.048(4) 0.006(3) -0.019(3) -0.037(4) C202 0.071(4) 0.031(3) 0.039(3) 0.007(2) -0.015(3) -0.015(3) C203 0.069(4) 0.046(3) 0.034(3) -0.007(2) 0.002(3) -0.007(3) C204 0.055(3) 0.035(3) 0.039(3) -0.006(2) 0.007(3) -0.012(3) C205 0.047(3) 0.016(2) 0.035(2) 0.0003(19) -0.002(2) 0.000(2) C206 0.045(3) 0.025(2) 0.035(3) 0.0039(19) -0.003(2) 0.003(2) C207 0.042(3) 0.030(3) 0.050(3) 0.014(2) -0.005(3) -0.004(2) S208 0.0356(6) 0.0204(5) 0.0310(6) -0.0024(4) -0.0017(5) 0.0044(5) O28A 0.0379(19) 0.0276(17) 0.0441(19) -0.0054(14) 0.0019(16) 0.0037(15) O28B 0.056(2) 0.0314(18) 0.0342(17) 0.0030(16) -0.0013(15) 0.0113(18) N209 0.035(2) 0.0226(19) 0.0290(19) 0.0000(15) 0.0007(17) 0.0064(17) C210 0.035(3) 0.019(2) 0.032(2) 0.0020(16) 0.003(2) 0.0017(18) C211 0.030(2) 0.025(2) 0.031(2) -0.0030(19) -0.0006(19) -0.0012(18) N212 0.0315(19) 0.0196(17) 0.0318(19) -0.0046(16) 0.0023(18) -0.0011(15) C213 0.043(3) 0.021(2) 0.034(3) -0.0053(18) 0.003(2) 0.0008(19) C214 0.037(3) 0.032(3) 0.040(3) -0.008(2) 0.000(2) 0.006(2) C215 0.040(3) 0.040(3) 0.045(3) -0.014(2) 0.012(3) -0.005(2) C216 0.038(3) 0.031(3) 0.031(2) -0.0050(19) 0.005(2) -0.009(2) C217 0.046(3) 0.038(3) 0.028(2) -0.002(2) 0.001(2) -0.013(2) C218 0.039(3) 0.041(3) 0.029(3) 0.004(2) -0.002(2) -0.011(2) C219 0.039(3) 0.032(3) 0.034(3) 0.007(2) 0.004(2) -0.002(2) C220 0.042(3) 0.026(2) 0.035(3) 0.003(2) 0.006(2) -0.004(2) C221 0.036(3) 0.026(2) 0.036(3) 0.000(2) 0.001(2) -0.005(2) C222 0.049(3) 0.039(3) 0.042(3) 0.010(3) -0.002(2) 0.011(3) C223 0.039(3) 0.019(2) 0.034(3) 0.0007(18) 0.002(2) 0.0033(19) C224 0.047(3) 0.028(3) 0.047(3) 0.003(2) 0.003(3) 0.006(2) C225 0.077(4) 0.032(3) 0.055(4) 0.010(3) 0.016(3) 0.004(3) C226 0.090(5) 0.037(3) 0.039(3) 0.011(3) -0.001(3) 0.017(3) C227 0.081(5) 0.050(4) 0.036(3) 0.001(3) -0.009(3) 0.027(3) C228 0.048(3) 0.040(3) 0.036(3) -0.007(2) -0.004(2) 0.011(3) C229 0.048(3) 0.020(2) 0.034(2) -0.002(2) -0.004(2) 0.009(2) C230 0.057(3) 0.027(3) 0.037(3) 0.005(2) 0.003(2) 0.011(2) C231 0.082(4) 0.036(3) 0.035(3) 0.005(3) 0.006(3) 0.014(3) C232 0.088(5) 0.043(3) 0.034(3) 0.004(2) -0.013(3) 0.008(3) C233 0.075(4) 0.031(3) 0.049(3) -0.001(2) -0.024(3) -0.007(3) C234 0.048(3) 0.030(3) 0.038(3) 0.003(2) -0.009(2) 0.003(2) C01 0.067(5) 0.129(8) 0.067(5) 0.001(5) -0.004(4) -0.022(5) Cl3 0.0709(13) 0.1001(16) 0.127(2) 0.0345(15) 0.0081(13) 0.0149(12) Cl4 0.1128(18) 0.1086(19) 0.0854(15) 0.0133(13) 0.0145(14) 0.0025(15) _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 2.144(4) . ? Ru1 N112 2.149(4) . ? Ru1 C118 2.151(5) . ? Ru1 C117 2.183(5) . ? Ru1 C121 2.188(5) . ? Ru1 C116 2.189(5) . ? Ru1 C120 2.196(5) . ? Ru1 C119 2.221(5) . ? Ru1 Cl1 2.4420(13) . ? C101 C102 1.515(8) . ? C101 H10A 0.9800 . ? C101 H10B 0.9800 . ? C101 H10C 0.9800 . ? C102 C107 1.375(7) . ? C102 C103 1.414(9) . ? C103 C104 1.378(8) . ? C103 H10D 0.9500 . ? C104 C105 1.392(7) . ? C104 H10E 0.9500 . ? C105 C106 1.366(7) . ? C105 S108 1.795(5) . ? C106 C107 1.394(7) . ? C106 H10F 0.9500 . ? C107 H10G 0.9500 . ? S108 O18A 1.442(4) . ? S108 O18B 1.446(4) . ? S108 N109 1.613(4) . ? N109 C110 1.496(5) . ? C110 C129 1.516(6) . ? C110 C111 1.530(6) . ? C110 H11A 1.0000 . ? C111 N112 1.485(6) . ? C111 C123 1.524(6) . ? C111 H11B 1.0000 . ? N112 C113 1.470(6) . ? N112 H112 0.844(19) . ? C113 C114 1.526(7) . ? C113 H11C 0.9900 . ? C113 H11D 0.9900 . ? C114 C115 1.509(7) . ? C114 H11E 0.9900 . ? C114 H11F 0.9900 . ? C115 C116 1.528(7) . ? C115 H11G 0.9900 . ? C115 H11H 0.9900 . ? C116 C121 1.414(7) . ? C116 C117 1.420(7) . ? C117 C118 1.384(8) . ? C117 H11I 0.9500 . ? C118 C119 1.428(8) . ? C118 H11J 0.9500 . ? C119 C120 1.396(7) . ? C119 C122 1.506(8) . ? C120 C121 1.431(7) . ? C120 H12I 0.9500 . ? C121 H12J 0.9500 . ? C122 H12A 0.9800 . ? C122 H12B 0.9800 . ? C122 H12C 0.9800 . ? C123 C128 1.366(7) . ? C123 C124 1.399(7) . ? C124 C125 1.398(7) . ? C124 H12D 0.9500 . ? C125 C126 1.363(8) . ? C125 H12E 0.9500 . ? C126 C127 1.390(9) . ? C126 H12F 0.9500 . ? C127 C128 1.392(7) . ? C127 H12G 0.9500 . ? C128 H12H 0.9500 . ? C129 C134 1.384(7) . ? C129 C130 1.389(7) . ? C130 C131 1.405(7) . ? C130 H13A 0.9500 . ? C131 C132 1.345(9) . ? C131 H13B 0.9500 . ? C132 C133 1.393(9) . ? C132 H13C 0.9500 . ? C133 C134 1.378(7) . ? C133 H13D 0.9500 . ? C134 H13E 0.9500 . ? Ru2 N209 2.142(4) . ? Ru2 N212 2.152(4) . ? Ru2 C218 2.171(5) . ? Ru2 C220 2.187(5) . ? Ru2 C217 2.192(5) . ? Ru2 C221 2.194(5) . ? Ru2 C216 2.208(5) . ? Ru2 C219 2.233(5) . ? Ru2 Cl2 2.4424(12) . ? C201 C202 1.487(8) . ? C201 H20A 0.9800 . ? C201 H20B 0.9800 . ? C201 H20C 0.9800 . ? C202 C207 1.394(8) . ? C202 C203 1.402(9) . ? C203 C204 1.391(8) . ? C203 H20D 0.9500 . ? C204 C205 1.389(7) . ? C204 H20E 0.9500 . ? C205 C206 1.378(7) . ? C205 S208 1.789(5) . ? C206 C207 1.394(7) . ? C206 H20F 0.9500 . ? C207 H20G 0.9500 . ? S208 O28B 1.438(4) . ? S208 O28A 1.446(4) . ? S208 N209 1.607(4) . ? N209 C210 1.489(5) . ? C210 C229 1.522(6) . ? C210 C211 1.529(6) . ? C210 H21A 1.0000 . ? C211 N212 1.479(6) . ? C211 C223 1.516(6) . ? C211 H21B 1.0000 . ? N212 C213 1.505(6) . ? N212 H212 0.830(19) . ? C213 C214 1.520(7) . ? C213 H21C 0.9900 . ? C213 H21D 0.9900 . ? C214 C215 1.525(7) . ? C214 H21E 0.9900 . ? C214 H21F 0.9900 . ? C215 C216 1.500(7) . ? C215 H21G 0.9900 . ? C215 H21H 0.9900 . ? C216 C217 1.420(7) . ? C216 C221 1.425(6) . ? C217 C218 1.398(8) . ? C217 H21I 0.9500 . ? C218 C219 1.434(7) . ? C218 H21J 0.9500 . ? C219 C220 1.395(7) . ? C219 C222 1.511(7) . ? C220 C221 1.430(7) . ? C220 H22I 0.9500 . ? C221 H22J 0.9500 . ? C222 H22A 0.9800 . ? C222 H22B 0.9800 . ? C222 H22C 0.9800 . ? C223 C228 1.380(7) . ? C223 C224 1.387(7) . ? C224 C225 1.390(7) . ? C224 H22D 0.9500 . ? C225 C226 1.356(9) . ? C225 H22E 0.9500 . ? C226 C227 1.359(10) . ? C226 H22F 0.9500 . ? C227 C228 1.390(8) . ? C227 H22G 0.9500 . ? C228 H22H 0.9500 . ? C229 C234 1.387(7) . ? C229 C230 1.393(7) . ? C230 C231 1.382(8) . ? C230 H23A 0.9500 . ? C231 C232 1.354(9) . ? C231 H23B 0.9500 . ? C232 C233 1.394(9) . ? C232 H23C 0.9500 . ? C233 C234 1.369(7) . ? C233 H23D 0.9500 . ? C234 H23E 0.9500 . ? C01 Cl4 1.724(7) . ? C01 Cl3 1.769(6) . ? C01 H01B 0.9900 . ? C01 H01A 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 N109 Ru1 N112 78.69(14) . . ? N109 Ru1 C118 149.12(19) . . ? N112 Ru1 C118 130.47(19) . . ? N109 Ru1 C117 167.53(18) . . ? N112 Ru1 C117 99.97(18) . . ? C118 Ru1 C117 37.2(2) . . ? N109 Ru1 C121 100.59(17) . . ? N112 Ru1 C121 109.70(17) . . ? C118 Ru1 C121 80.4(2) . . ? C117 Ru1 C121 68.00(19) . . ? N109 Ru1 C116 129.65(18) . . ? N112 Ru1 C116 90.52(16) . . ? C118 Ru1 C116 68.0(2) . . ? C117 Ru1 C116 37.91(19) . . ? C121 Ru1 C116 37.69(17) . . ? N109 Ru1 C120 94.48(17) . . ? N112 Ru1 C120 145.84(18) . . ? C118 Ru1 C120 67.1(2) . . ? C117 Ru1 C120 79.63(19) . . ? C121 Ru1 C120 38.11(18) . . ? C116 Ru1 C120 68.05(18) . . ? N109 Ru1 C119 113.27(17) . . ? N112 Ru1 C119 168.01(17) . . ? C118 Ru1 C119 38.1(2) . . ? C117 Ru1 C119 68.2(2) . . ? C121 Ru1 C119 68.33(19) . . ? C116 Ru1 C119 81.07(19) . . ? C120 Ru1 C119 36.84(19) . . ? N109 Ru1 Cl1 87.53(12) . . ? N112 Ru1 Cl1 83.14(10) . . ? C118 Ru1 Cl1 86.65(15) . . ? C117 Ru1 Cl1 104.68(14) . . ? C121 Ru1 Cl1 165.83(13) . . ? C116 Ru1 Cl1 140.29(14) . . ? C120 Ru1 Cl1 130.38(14) . . ? C119 Ru1 Cl1 97.84(15) . . ? 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 . . ? C107 C102 C103 118.0(5) . . ? C107 C102 C101 123.3(6) . . ? C103 C102 C101 118.7(5) . . ? C104 C103 C102 120.7(5) . . ? C104 C103 H10D 119.6 . . ? C102 C103 H10D 119.6 . . ? C103 C104 C105 119.9(6) . . ? C103 C104 H10E 120.1 . . ? C105 C104 H10E 120.1 . . ? C106 C105 C104 120.0(5) . . ? C106 C105 S108 121.6(4) . . ? C104 C105 S108 118.2(4) . . ? C105 C106 C107 120.2(5) . . ? C105 C106 H10F 119.9 . . ? C107 C106 H10F 119.9 . . ? C102 C107 C106 121.2(5) . . ? C102 C107 H10G 119.4 . . ? C106 C107 H10G 119.4 . . ? O18A S108 O18B 116.9(2) . . ? O18A S108 N109 112.5(2) . . ? O18B S108 N109 108.9(2) . . ? O18A S108 C105 106.0(2) . . ? O18B S108 C105 103.3(2) . . ? N109 S108 C105 108.6(2) . . ? C110 N109 S108 113.0(3) . . ? C110 N109 Ru1 112.0(3) . . ? S108 N109 Ru1 120.2(2) . . ? N109 C110 C129 114.9(4) . . ? N109 C110 C111 105.5(3) . . ? C129 C110 C111 110.5(4) . . ? N109 C110 H11A 108.6 . . ? C129 C110 H11A 108.6 . . ? C111 C110 H11A 108.6 . . ? N112 C111 C123 113.2(4) . . ? N112 C111 C110 108.4(4) . . ? C123 C111 C110 112.9(4) . . ? N112 C111 H11B 107.3 . . ? C123 C111 H11B 107.3 . . ? C110 C111 H11B 107.3 . . ? C113 N112 C111 112.1(4) . . ? C113 N112 Ru1 117.8(3) . . ? C111 N112 Ru1 111.2(3) . . ? C113 N112 H112 105(4) . . ? C111 N112 H112 110(4) . . ? Ru1 N112 H112 99(4) . . ? N112 C113 C114 114.3(4) . . ? N112 C113 H11C 108.7 . . ? C114 C113 H11C 108.7 . . ? N112 C113 H11D 108.7 . . ? C114 C113 H11D 108.7 . . ? H11C C113 H11D 107.6 . . ? C115 C114 C113 113.9(4) . . ? C115 C114 H11E 108.8 . . ? C113 C114 H11E 108.8 . . ? C115 C114 H11F 108.8 . . ? C113 C114 H11F 108.8 . . ? H11E C114 H11F 107.7 . . ? C114 C115 C116 113.5(4) . . ? C114 C115 H11G 108.9 . . ? C116 C115 H11G 108.9 . . ? C114 C115 H11H 108.9 . . ? C116 C115 H11H 108.9 . . ? H11G C115 H11H 107.7 . . ? C121 C116 C117 119.2(5) . . ? C121 C116 C115 121.5(5) . . ? C117 C116 C115 119.2(5) . . ? C121 C116 Ru1 71.1(3) . . ? C117 C116 Ru1 70.8(3) . . ? C115 C116 Ru1 127.5(3) . . ? C118 C117 C116 119.9(5) . . ? C118 C117 Ru1 70.1(3) . . ? C116 C117 Ru1 71.3(3) . . ? C118 C117 H11I 120.0 . . ? C116 C117 H11I 120.0 . . ? Ru1 C117 H11I 131.4 . . ? C117 C118 C119 122.7(5) . . ? C117 C118 Ru1 72.6(3) . . ? C119 C118 Ru1 73.6(3) . . ? C117 C118 H11J 118.6 . . ? C119 C118 H11J 118.6 . . ? Ru1 C118 H11J 127.2 . . ? C120 C119 C118 116.6(5) . . ? C120 C119 C122 124.2(5) . . ? C118 C119 C122 119.1(5) . . ? C120 C119 Ru1 70.6(3) . . ? C118 C119 Ru1 68.3(3) . . ? C122 C119 Ru1 130.3(4) . . ? C119 C120 C121 122.3(5) . . ? C119 C120 Ru1 72.5(3) . . ? C121 C120 Ru1 70.6(3) . . ? C119 C120 H12I 118.9 . . ? C121 C120 H12I 118.9 . . ? Ru1 C120 H12I 130.8 . . ? C116 C121 C120 119.1(5) . . ? C116 C121 Ru1 71.2(3) . . ? C120 C121 Ru1 71.2(3) . . ? C116 C121 H12J 120.4 . . ? C120 C121 H12J 120.4 . . ? Ru1 C121 H12J 129.5 . . ? C119 C122 H12A 109.5 . . ? C119 C122 H12B 109.5 . . ? H12A C122 H12B 109.5 . . ? C119 C122 H12C 109.5 . . ? H12A C122 H12C 109.5 . . ? H12B C122 H12C 109.5 . . ? C128 C123 C124 118.8(4) . . ? C128 C123 C111 120.8(4) . . ? C124 C123 C111 120.4(4) . . ? C125 C124 C123 120.3(5) . . ? C125 C124 H12D 119.8 . . ? C123 C124 H12D 119.8 . . ? C126 C125 C124 119.8(5) . . ? C126 C125 H12E 120.1 . . ? C124 C125 H12E 120.1 . . ? C125 C126 C127 120.4(5) . . ? C125 C126 H12F 119.8 . . ? C127 C126 H12F 119.8 . . ? C126 C127 C128 119.3(5) . . ? C126 C127 H12G 120.3 . . ? C128 C127 H12G 120.3 . . ? C123 C128 C127 121.3(5) . . ? C123 C128 H12H 119.4 . . ? C127 C128 H12H 119.4 . . ? C134 C129 C130 117.8(4) . . ? C134 C129 C110 121.6(4) . . ? C130 C129 C110 120.5(4) . . ? C129 C130 C131 120.3(5) . . ? C129 C130 H13A 119.9 . . ? C131 C130 H13A 119.9 . . ? C132 C131 C130 120.8(6) . . ? C132 C131 H13B 119.6 . . ? C130 C131 H13B 119.6 . . ? C131 C132 C133 119.7(5) . . ? C131 C132 H13C 120.1 . . ? C133 C132 H13C 120.1 . . ? C134 C133 C132 119.7(6) . . ? C134 C133 H13D 120.2 . . ? C132 C133 H13D 120.2 . . ? C133 C134 C129 121.7(5) . . ? C133 C134 H13E 119.2 . . ? C129 C134 H13E 119.2 . . ? N209 Ru2 N212 78.87(14) . . ? N209 Ru2 C218 146.48(18) . . ? N212 Ru2 C218 132.99(17) . . ? N209 Ru2 C220 93.42(17) . . ? N212 Ru2 C220 143.26(17) . . ? C218 Ru2 C220 67.21(19) . . ? N209 Ru2 C217 169.18(18) . . ? N212 Ru2 C217 101.41(18) . . ? C218 Ru2 C217 37.4(2) . . ? C220 Ru2 C217 79.86(19) . . ? N209 Ru2 C221 101.78(17) . . ? N212 Ru2 C221 107.90(16) . . ? C218 Ru2 C221 80.09(19) . . ? C220 Ru2 C221 38.10(18) . . ? C217 Ru2 C221 67.73(18) . . ? N209 Ru2 C216 131.84(17) . . ? N212 Ru2 C216 90.09(17) . . ? C218 Ru2 C216 67.9(2) . . ? C220 Ru2 C216 68.38(18) . . ? C217 Ru2 C216 37.66(18) . . ? C221 Ru2 C216 37.77(17) . . ? N209 Ru2 C219 111.22(17) . . ? N212 Ru2 C219 169.47(17) . . ? C218 Ru2 C219 37.99(19) . . ? C220 Ru2 C219 36.77(18) . . ? C217 Ru2 C219 68.11(19) . . ? C221 Ru2 C219 67.91(18) . . ? C216 Ru2 C219 80.90(19) . . ? N209 Ru2 Cl2 86.23(11) . . ? N212 Ru2 Cl2 82.84(10) . . ? C218 Ru2 Cl2 87.97(14) . . ? C220 Ru2 Cl2 132.91(14) . . ? C217 Ru2 Cl2 104.56(14) . . ? C221 Ru2 Cl2 167.55(13) . . ? C216 Ru2 Cl2 139.14(13) . . ? C219 Ru2 Cl2 100.41(13) . . ? 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 118.9(5) . . ? C207 C202 C201 119.3(6) . . ? C203 C202 C201 121.7(6) . . ? C204 C203 C202 120.7(5) . . ? C204 C203 H20D 119.6 . . ? C202 C203 H20D 119.6 . . ? C205 C204 C203 119.5(5) . . ? C205 C204 H20E 120.2 . . ? C203 C204 H20E 120.2 . . ? C206 C205 C204 120.3(5) . . ? C206 C205 S208 120.1(4) . . ? C204 C205 S208 119.6(4) . . ? C205 C206 C207 120.6(5) . . ? C205 C206 H20F 119.7 . . ? C207 C206 H20F 119.7 . . ? C206 C207 C202 120.0(5) . . ? C206 C207 H20G 120.0 . . ? C202 C207 H20G 120.0 . . ? O28B S208 O28A 117.1(2) . . ? O28B S208 N209 108.9(2) . . ? O28A S208 N209 112.9(2) . . ? O28B S208 C205 104.5(2) . . ? O28A S208 C205 105.9(2) . . ? N209 S208 C205 106.6(2) . . ? C210 N209 S208 114.0(3) . . ? C210 N209 Ru2 112.1(3) . . ? S208 N209 Ru2 121.8(2) . . ? N209 C210 C229 115.0(4) . . ? N209 C210 C211 105.7(3) . . ? C229 C210 C211 110.6(4) . . ? N209 C210 H21A 108.5 . . ? C229 C210 H21A 108.5 . . ? C211 C210 H21A 108.5 . . ? N212 C211 C223 114.1(4) . . ? N212 C211 C210 108.1(4) . . ? C223 C211 C210 112.8(4) . . ? N212 C211 H21B 107.2 . . ? C223 C211 H21B 107.2 . . ? C210 C211 H21B 107.2 . . ? C211 N212 C213 113.0(4) . . ? C211 N212 Ru2 109.9(3) . . ? C213 N212 Ru2 117.9(3) . . ? C211 N212 H212 110(4) . . ? C213 N212 H212 107(4) . . ? Ru2 N212 H212 97(4) . . ? N212 C213 C214 113.9(4) . . ? N212 C213 H21C 108.8 . . ? C214 C213 H21C 108.8 . . ? N212 C213 H21D 108.8 . . ? C214 C213 H21D 108.8 . . ? H21C C213 H21D 107.7 . . ? C213 C214 C215 113.7(4) . . ? C213 C214 H21E 108.8 . . ? C215 C214 H21E 108.8 . . ? C213 C214 H21F 108.8 . . ? C215 C214 H21F 108.8 . . ? H21E C214 H21F 107.7 . . ? C216 C215 C214 114.2(4) . . ? C216 C215 H21G 108.7 . . ? C214 C215 H21G 108.7 . . ? C216 C215 H21H 108.7 . . ? C214 C215 H21H 108.7 . . ? H21G C215 H21H 107.6 . . ? C217 C216 C221 118.4(5) . . ? C217 C216 C215 120.0(4) . . ? C221 C216 C215 121.6(4) . . ? C217 C216 Ru2 70.6(3) . . ? C221 C216 Ru2 70.6(3) . . ? C215 C216 Ru2 128.2(3) . . ? C218 C217 C216 120.5(5) . . ? C218 C217 Ru2 70.5(3) . . ? C216 C217 Ru2 71.8(3) . . ? C218 C217 H21I 119.8 . . ? C216 C217 H21I 119.8 . . ? Ru2 C217 H21I 130.7 . . ? C217 C218 C219 122.1(5) . . ? C217 C218 Ru2 72.2(3) . . ? C219 C218 Ru2 73.4(3) . . ? C217 C218 H21J 119.0 . . ? C219 C218 H21J 119.0 . . ? Ru2 C218 H21J 127.7 . . ? C220 C219 C218 117.0(5) . . ? C220 C219 C222 123.9(5) . . ? C218 C219 C222 119.1(5) . . ? C220 C219 Ru2 69.8(3) . . ? C218 C219 Ru2 68.7(3) . . ? C222 C219 Ru2 132.0(4) . . ? C219 C220 C221 122.2(5) . . ? C219 C220 Ru2 73.4(3) . . ? C221 C220 Ru2 71.2(3) . . ? C219 C220 H22I 118.9 . . ? C221 C220 H22I 118.9 . . ? Ru2 C220 H22I 128.9 . . ? C216 C221 C220 119.8(5) . . ? C216 C221 Ru2 71.6(3) . . ? C220 C221 Ru2 70.7(3) . . ? C216 C221 H22J 120.1 . . ? C220 C221 H22J 120.1 . . ? Ru2 C221 H22J 130.1 . . ? C219 C222 H22A 109.5 . . ? C219 C222 H22B 109.5 . . ? H22A C222 H22B 109.5 . . ? C219 C222 H22C 109.5 . . ? H22A C222 H22C 109.5 . . ? H22B C222 H22C 109.5 . . ? C228 C223 C224 118.8(5) . . ? C228 C223 C211 120.1(4) . . ? C224 C223 C211 121.0(4) . . ? C223 C224 C225 119.6(5) . . ? C223 C224 H22D 120.2 . . ? C225 C224 H22D 120.2 . . ? C226 C225 C224 121.0(6) . . ? C226 C225 H22E 119.5 . . ? C224 C225 H22E 119.5 . . ? C225 C226 C227 119.7(6) . . ? C225 C226 H22F 120.1 . . ? C227 C226 H22F 120.1 . . ? C226 C227 C228 120.6(6) . . ? C226 C227 H22G 119.7 . . ? C228 C227 H22G 119.7 . . ? C223 C228 C227 120.1(6) . . ? C223 C228 H22H 119.9 . . ? C227 C228 H22H 119.9 . . ? C234 C229 C230 118.9(5) . . ? C234 C229 C210 121.1(5) . . ? C230 C229 C210 119.9(5) . . ? C231 C230 C229 120.3(6) . . ? C231 C230 H23A 119.9 . . ? C229 C230 H23A 119.9 . . ? C232 C231 C230 120.1(6) . . ? C232 C231 H23B 120.0 . . ? C230 C231 H23B 120.0 . . ? C231 C232 C233 120.4(5) . . ? C231 C232 H23C 119.8 . . ? C233 C232 H23C 119.8 . . ? C234 C233 C232 119.8(6) . . ? C234 C233 H23D 120.1 . . ? C232 C233 H23D 120.1 . . ? C233 C234 C229 120.4(6) . . ? C233 C234 H23E 119.8 . . ? C229 C234 H23E 119.8 . . ? Cl4 C01 Cl3 113.2(5) . . ? Cl4 C01 H01B 108.9 . . ? Cl3 C01 H01B 108.9 . . ? Cl4 C01 H01A 108.9 . . ? Cl3 C01 H01A 108.9 . . ? H01B C01 H01A 107.8 . . ? 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 N112 H112 Cl2 0.844(19) 3.24(4) 3.939(4) 142(5) . N112 H112 Cl1 0.844(19) 2.58(5) 3.054(4) 117(4) . N212 H212 Cl1 0.830(19) 3.27(4) 3.932(4) 138(5) . N212 H212 Cl2 0.830(19) 2.54(5) 3.047(4) 121(5) . _diffrn_measured_fraction_theta_max 0.942 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.078 _refine_diff_density_min -1.007 _refine_diff_density_rms 0.102