Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2003 data_global _journal_coden_Cambridge 186 loop_ _publ_author_name 'Masanobu Watanabe' 'Masahiro Kai' 'Masaru Sato' _publ_contact_author_name 'Dr Masanobu Watanabe' _publ_contact_author_address ; Tokyo Metroplitan Koishikawa High School Bunko-ku Honkomagome 2-29-29 Tokyo 113-0021 JAPAN ; _publ_contact_author_email 'WATA@SE.CATV.NE.JP' _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Synthesis of the first non-carbonyl cisoid fulvalene complexes with a Ru Ru bond Bridged by thiolate ligands ; _publ_section_references ; Mackay, S., Gilmore, C. J.,Edwards, C., Stewart, N. & Shankland, K. (1999). maXus Computer Program for the Solution and Refinement of Crystal Structures. Nonius, The Netherlands, MacScience, Japan & The University of Glasgow. Johnson, C. K. (1976). ORTEP-II. A Fortran Thermal-Ellipsoid Plot Program. Report ORNL-5138. Oak Ridge National Laboratory, Oak Ridge, Tennessee, USA. Otwinowski, Z. and Minor, W, (1997). In Methods in Enzymology, 276, edited by C.W. Carter, Jr. & R.M. Sweet pp. 307-326, New York:Academic Press. Beurskens, P.T., Admiraal, G., Beurskens, G., Bosman, W.P.,Garci', A,A, ia-Granda, S., Gould, R.O., Smits, J.M.M. &', Smykalla, C. (1992). The DIRDIF92 program system, Technical Report of the Crystallography Laboratory, University of Nijmegen, The Netherlands. Waasmaier, D. & Kirfel, A. (1995). Acta Cryst. A51, 416-431. ; data_compond_2b _database_code_CSD 191659 _chemical_compound_source 'Local laboratory' _exptl_crystal_description Needle _exptl_crystal_colour Orange _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.04 _cell_measurement_temperature 298 _refine_ls_hydrogen_treatment refxyz _diffrn_measurement_device KappaCCD _computing_data_collection KappaCCD _computing_data_reduction 'Denzo and Scalepak (Otwinowski & Minor, 1997)' _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 21 loop_ _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_wavelength_id all _diffrn_orient_matrix_type X=UH _diffrn_orient_matrix_UB_11 0.01663 _diffrn_orient_matrix_UB_12 0.10117 _diffrn_orient_matrix_UB_13 -0.00516 _diffrn_orient_matrix_UB_21 0.10473 _diffrn_orient_matrix_UB_22 0.00649 _diffrn_orient_matrix_UB_23 -0.01137 _diffrn_orient_matrix_UB_31 -0.04735 _diffrn_orient_matrix_UB_32 -0.01445 _diffrn_orient_matrix_UB_33 -0.06421 _cell_formula_units_Z 1 _exptl_crystal_density_diffrn 1.563 _exptl_crystal_density_method 'not measured' _exptl_special_details ; ? ; _chemical_formula_weight 1309.034 _diffrn_radiation_type ' MoK¥a' loop_ _symmetry_equiv_pos_as_xyz +X,+Y,+Z -X,-Y,-Z _symmetry_space_group_name_H-M 'P -1 ' _symmetry_cell_setting Triclinic _chemical_formula_moiety 'C54 H50 F12 N4 P4 Ru2 ' _chemical_formula_sum 'C54 H50 F12 N4 P4 Ru2 ' _chemical_name_systematic ; ? ; _cell_length_a 9.1510(8) _cell_length_b 10.180(2) _cell_length_c 15.852(2) _cell_angle_alpha 83.319(6) _cell_angle_beta 103.008(7) _cell_angle_gamma 104.474(8) _cell_volume 1390.3(3) _diffrn_reflns_number 6567 _diffrn_reflns_theta_max 32.17 _diffrn_reflns_theta_min 2.07 _diffrn_reflns_theta_full 32.17 _computing_structure_solution 'DIRDIF (Buerskens et al., 1992)' _atom_sites_solution_primary vecmap _atom_sites_solution_secondary difmap _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 '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' _exptl_absorpt_coefficient_mu 0.739 _reflns_number_total 6024 _reflns_number_gt 5731 _reflns_threshold_expression >2sigma(I) _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even largeR . ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[¥s^2^(Fo^2^)+(0.0180P)^2^+13.6800P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6024 _refine_ls_number_parameters 343 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0950 _refine_ls_R_factor_gt 0.0892 _refine_ls_wR_factor_ref 0.1876 _refine_ls_wR_factor_gt 0.1845 _refine_ls_goodness_of_fit_ref 1.200 _refine_ls_restrained_S_all 1.200 _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 Ru1 Ru 0.17609(7) 0.93038(6) 0.14353(4) 0.03467(17) Uani 1 1 d . . . P1 P 0.2824(2) 0.95547(18) 0.29113(11) 0.0348(4) Uani 1 1 d . . . N1 N -0.0473(8) 0.8359(7) 0.1534(4) 0.0453(16) Uani 1 1 d . . . N2 N 0.2185(8) 0.7403(6) 0.1426(4) 0.0448(15) Uani 1 1 d . . . C1 C 0.0806(9) 1.0226(7) 0.0241(4) 0.0413(18) Uani 1 1 d . . . C2 C 0.2044(10) 0.9713(8) 0.0099(5) 0.048(2) Uani 1 1 d . . . C3 C 0.3434(10) 1.0381(9) 0.0725(5) 0.049(2) Uani 1 1 d . . . C4 C 0.3026(10) 1.1337(8) 0.1220(5) 0.052(2) Uani 1 1 d . . . C5 C 0.1403(9) 1.1211(7) 0.0949(5) 0.0441(18) Uani 1 1 d . . . C6 C -0.1755(10) 0.7907(9) 0.1420(6) 0.054(2) Uani 1 1 d . . . C7 C -0.3441(12) 0.7310(12) 0.1243(8) 0.084(4) Uani 1 1 d . . . C8 C 0.2370(11) 0.6378(9) 0.1350(6) 0.055(2) Uani 1 1 d . . . C9 C 0.2598(15) 0.5020(10) 0.1240(9) 0.086(4) Uani 1 1 d . . . C10 C 0.1795(9) 0.8500(7) 0.3645(4) 0.0399(16) Uani 1 1 d . . . C11 C 0.1877(11) 0.8948(10) 0.4487(5) 0.055(2) Uani 1 1 d . . . C12 C 0.1141(12) 0.8091(10) 0.5030(6) 0.064(3) Uani 1 1 d . . . C13 C 0.0289(12) 0.6814(10) 0.4740(6) 0.065(3) Uani 1 1 d . . . C14 C 0.0194(11) 0.6350(8) 0.3914(6) 0.054(2) Uani 1 1 d . . . C15 C 0.0925(10) 0.7189(8) 0.3356(5) 0.0445(18) Uani 1 1 d . . . C16 C 0.3164(9) 1.1294(7) 0.3351(4) 0.0412(17) Uani 1 1 d . . . C17 C 0.4595(11) 1.2051(9) 0.3798(6) 0.057(2) Uani 1 1 d . . . C18 C 0.4802(15) 1.3404(11) 0.4039(8) 0.080(3) Uani 1 1 d . . . C19 C 0.3547(17) 1.3958(11) 0.3880(7) 0.082(4) Uani 1 1 d . . . C20 C 0.2110(15) 1.3205(11) 0.3454(7) 0.075(3) Uani 1 1 d . . . C21 C 0.1921(11) 1.1876(9) 0.3192(6) 0.055(2) Uani 1 1 d . . . C22 C 0.4729(9) 0.9204(7) 0.3186(4) 0.0385(16) Uani 1 1 d . . . C23 C 0.5098(11) 0.8229(10) 0.3746(6) 0.060(2) Uani 1 1 d . . . C24 C 0.6549(13) 0.7980(11) 0.3895(7) 0.076(3) Uani 1 1 d . . . C25 C 0.7654(12) 0.8710(11) 0.3497(7) 0.070(3) Uani 1 1 d . . . C26 C 0.7314(11) 0.9697(10) 0.2938(6) 0.061(2) Uani 1 1 d . . . C27 C 0.5852(10) 0.9946(9) 0.2786(5) 0.052(2) Uani 1 1 d . . . P2 P 0.7744(4) 0.3600(3) 0.1495(3) 0.0815(9) Uani 1 1 d . . . F1 F 0.6920(14) 0.2092(10) 0.1302(10) 0.190(6) Uani 1 1 d . . . F2 F 0.8717(15) 0.4957(11) 0.1857(9) 0.198(6) Uani 1 1 d . . . F3 F 0.866(3) 0.316(2) 0.2282(17) 0.395(18) Uani 1 1 d . . . F4 F 0.8913(17) 0.3375(15) 0.1006(15) 0.252(9) Uani 1 1 d . . . F5 F 0.699(3) 0.402(3) 0.0724(9) 0.367(14) Uani 1 1 d . . . F6 F 0.6494(17) 0.3740(15) 0.1894(12) 0.244(8) Uani 1 1 d . . . H2 H 0.1954 0.8981 -0.0256 0.058 Uiso 1 1 d R . . H3 H 0.4681 1.0349 0.0622 0.058 Uiso 1 1 d R . . H4 H 0.3805 1.1913 0.1640 0.062 Uiso 1 1 d R . . H5 H 0.1070 1.1784 0.1137 0.053 Uiso 1 1 d R . . H7A H -0.3926 0.7578 0.1652 0.101 Uiso 1 1 d R . . H7B H -0.3596 0.6339 0.1286 0.101 Uiso 1 1 d R . . H7C H -0.3885 0.7606 0.0666 0.101 Uiso 1 1 d R . . H9A H 0.2639 0.4905 0.0654 0.104 Uiso 1 1 d R . . H9B H 0.1768 0.4336 0.1413 0.104 Uiso 1 1 d R . . H9C H 0.3554 0.4934 0.1617 0.104 Uiso 1 1 d R . . H11 H 0.2524 0.9755 0.4665 0.066 Uiso 1 1 d R . . H12 H 0.1161 0.8518 0.5615 0.077 Uiso 1 1 d R . . H13 H -0.0234 0.6341 0.5105 0.078 Uiso 1 1 d R . . H14 H -0.0238 0.5642 0.3693 0.065 Uiso 1 1 d R . . H15 H 0.0840 0.6855 0.2790 0.053 Uiso 1 1 d R . . H17 H 0.5384 1.1786 0.3785 0.069 Uiso 1 1 d R . . H18 H 0.5952 1.4024 0.4403 0.096 Uiso 1 1 d R . . H19 H 0.3540 1.4685 0.4034 0.098 Uiso 1 1 d R . . H20 H 0.1231 1.3600 0.3339 0.090 Uiso 1 1 d R . . H21 H 0.1022 1.1408 0.2913 0.066 Uiso 1 1 d R . . H23 H 0.4169 0.7612 0.4001 0.072 Uiso 1 1 d R . . H24 H 0.6830 0.7248 0.4335 0.092 Uiso 1 1 d R . . H25 H 0.8648 0.8500 0.3604 0.084 Uiso 1 1 d R . . H26 H 0.8075 1.0245 0.2635 0.073 Uiso 1 1 d R . . H27 H 0.5625 1.0685 0.2385 0.062 Uiso 1 1 d 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 0.0355(3) 0.0325(3) 0.0321(2) 0.00470(18) 0.0022(2) 0.0079(2) P1 0.0329(11) 0.0351(9) 0.0337(8) 0.0044(6) 0.0028(7) 0.0091(7) N1 0.041(4) 0.046(4) 0.043(3) 0.009(3) 0.000(3) 0.013(3) N2 0.053(4) 0.035(3) 0.050(4) 0.005(3) 0.013(3) 0.017(3) C1 0.044(5) 0.039(4) 0.036(3) 0.005(3) 0.001(3) 0.010(3) C2 0.054(5) 0.053(5) 0.033(3) 0.011(3) 0.008(3) 0.012(4) C3 0.036(5) 0.056(5) 0.048(4) 0.017(3) 0.013(3) 0.006(3) C4 0.053(5) 0.040(4) 0.044(4) 0.014(3) -0.003(3) -0.006(3) C5 0.052(5) 0.029(3) 0.047(4) 0.007(3) 0.004(3) 0.013(3) C6 0.038(5) 0.051(5) 0.063(5) 0.010(4) 0.001(4) 0.005(4) C7 0.043(7) 0.084(8) 0.115(10) 0.008(7) 0.015(6) 0.001(5) C8 0.063(6) 0.049(5) 0.059(5) 0.012(4) 0.029(4) 0.015(4) C9 0.096(10) 0.048(6) 0.127(11) 0.010(6) 0.043(8) 0.028(6) C10 0.037(4) 0.042(4) 0.038(3) 0.008(3) 0.003(3) 0.015(3) C11 0.055(6) 0.064(5) 0.039(4) 0.006(4) 0.012(4) 0.005(4) C12 0.082(8) 0.065(6) 0.041(4) 0.007(4) 0.016(4) 0.013(5) C13 0.083(8) 0.064(6) 0.051(5) 0.025(4) 0.026(5) 0.027(5) C14 0.065(6) 0.042(4) 0.055(5) 0.011(3) 0.020(4) 0.012(4) C15 0.047(5) 0.045(4) 0.043(4) 0.006(3) 0.016(3) 0.010(3) C16 0.049(5) 0.040(4) 0.035(3) -0.003(3) 0.007(3) 0.012(3) C17 0.048(6) 0.060(5) 0.062(5) -0.008(4) 0.004(4) 0.013(4) C18 0.083(9) 0.060(6) 0.091(8) -0.022(6) 0.015(6) 0.000(6) C19 0.139(12) 0.048(6) 0.066(6) -0.011(5) 0.030(7) 0.025(7) C20 0.108(10) 0.069(7) 0.061(6) -0.002(5) 0.015(6) 0.047(6) C21 0.053(6) 0.057(5) 0.061(5) -0.007(4) 0.010(4) 0.023(4) C22 0.037(4) 0.042(4) 0.036(3) 0.005(3) 0.008(3) 0.012(3) C23 0.046(6) 0.065(6) 0.070(6) 0.020(4) 0.015(4) 0.024(4) C24 0.066(7) 0.084(7) 0.084(7) 0.036(6) 0.013(6) 0.046(6) C25 0.044(6) 0.084(7) 0.086(7) 0.012(6) 0.013(5) 0.030(5) C26 0.047(6) 0.076(6) 0.062(5) 0.011(5) 0.017(4) 0.022(5) C27 0.044(5) 0.058(5) 0.052(4) 0.014(4) 0.010(4) 0.018(4) P2 0.062(2) 0.0587(17) 0.121(3) -0.0082(17) 0.0260(19) 0.0020(14) F1 0.182(11) 0.095(7) 0.301(16) -0.044(9) 0.121(11) -0.030(7) F2 0.209(12) 0.109(8) 0.249(14) -0.067(9) 0.063(11) -0.057(8) F3 0.37(3) 0.26(2) 0.40(3) 0.07(2) -0.21(3) 0.08(2) F4 0.147(12) 0.195(13) 0.46(3) -0.141(16) 0.163(16) -0.031(10) F5 0.49(3) 0.52(4) 0.118(10) 0.144(16) 0.028(16) 0.26(3) F6 0.177(13) 0.232(15) 0.38(2) -0.101(15) 0.187(15) -0.009(11) _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 N1 2.063(7) . ? Ru1 N2 2.069(6) . ? Ru1 C5 2.080(7) . ? Ru1 C3 2.113(8) . ? Ru1 C1 2.117(6) . ? Ru1 C4 2.135(7) . ? Ru1 C2 2.171(7) . ? Ru1 P1 2.3402(18) . ? P1 C10 1.757(8) . ? P1 C22 1.813(8) . ? P1 C16 1.906(8) . ? N1 C6 1.129(10) . ? N2 C8 1.122(10) . ? C1 C2 1.429(12) . ? C1 C1 1.486(14) 2_575 ? C1 C5 1.509(10) . ? C2 C3 1.491(11) . ? C3 C4 1.481(13) . ? C4 C5 1.427(11) . ? C6 C7 1.485(13) . ? C8 C9 1.484(13) . ? C10 C15 1.439(11) . ? C10 C11 1.441(11) . ? C11 C12 1.322(12) . ? C12 C13 1.407(14) . ? C13 C14 1.420(13) . ? C14 C15 1.328(11) . ? C16 C21 1.372(11) . ? C16 C17 1.420(11) . ? C17 C18 1.427(14) . ? C18 C19 1.364(16) . ? C19 C20 1.410(16) . ? C20 C21 1.419(13) . ? C22 C23 1.311(10) . ? C22 C27 1.350(11) . ? C23 C24 1.377(13) . ? C24 C25 1.333(15) . ? C25 C26 1.310(13) . ? C26 C27 1.386(12) . ? P2 F5 1.339(13) . ? P2 F3 1.431(15) . ? P2 F6 1.468(11) . ? P2 F4 1.528(13) . ? P2 F2 1.540(9) . ? P2 F1 1.563(10) . ? C2 H2 0.9617 . ? C3 H3 1.1973 . ? C4 H4 0.9816 . ? C5 H5 0.8319 . ? C7 H7A 0.9601 . ? C7 H7B 0.9599 . ? C7 H7C 0.9601 . ? C9 H9A 0.9600 . ? C9 H9B 0.9599 . ? C9 H9C 0.9600 . ? C11 H11 0.9168 . ? C12 H12 1.0637 . ? C13 H13 0.8604 . ? C14 H14 0.8077 . ? C15 H15 0.9765 . ? C17 H17 0.8366 . ? C18 H18 1.1482 . ? C19 H19 0.8082 . ? C20 H20 0.9595 . ? C21 H21 0.8880 . ? C23 H23 1.0529 . ? C24 H24 1.0010 . ? C25 H25 0.9598 . ? C26 H26 0.9597 . ? C27 H27 0.9595 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ru1 N2 88.4(3) . . ? N1 Ru1 C5 98.4(3) . . ? N2 Ru1 C5 157.7(3) . . ? N1 Ru1 C3 152.3(3) . . ? N2 Ru1 C3 96.9(3) . . ? C5 Ru1 C3 67.6(3) . . ? N1 Ru1 C1 86.8(3) . . ? N2 Ru1 C1 118.0(3) . . ? C5 Ru1 C1 42.1(3) . . ? C3 Ru1 C1 66.7(3) . . ? N1 Ru1 C4 136.5(3) . . ? N2 Ru1 C4 134.3(3) . . ? C5 Ru1 C4 39.6(3) . . ? C3 Ru1 C4 40.8(3) . . ? C1 Ru1 C4 68.0(3) . . ? N1 Ru1 C2 112.7(3) . . ? N2 Ru1 C2 89.1(3) . . ? C5 Ru1 C2 68.7(3) . . ? C3 Ru1 C2 40.7(3) . . ? C1 Ru1 C2 38.9(3) . . ? C4 Ru1 C2 68.8(3) . . ? N1 Ru1 P1 98.57(18) . . ? N2 Ru1 P1 95.16(19) . . ? C5 Ru1 P1 104.6(2) . . ? C3 Ru1 P1 108.0(2) . . ? C1 Ru1 P1 146.7(2) . . ? C4 Ru1 P1 86.6(2) . . ? C2 Ru1 P1 148.6(2) . . ? C10 P1 C22 105.2(3) . . ? C10 P1 C16 101.4(4) . . ? C22 P1 C16 102.9(3) . . ? C10 P1 Ru1 116.5(3) . . ? C22 P1 Ru1 110.7(2) . . ? C16 P1 Ru1 118.4(2) . . ? C6 N1 Ru1 166.6(7) . . ? C8 N2 Ru1 174.4(7) . . ? C2 C1 C1 122.6(9) . 2_575 ? C2 C1 C5 109.6(6) . . ? C1 C1 C5 127.8(9) 2_575 . ? C2 C1 Ru1 72.6(4) . . ? C1 C1 Ru1 124.7(7) 2_575 . ? C5 C1 Ru1 67.6(3) . . ? C1 C2 C3 105.5(7) . . ? C1 C2 Ru1 68.5(4) . . ? C3 C2 Ru1 67.6(4) . . ? C4 C3 C2 109.9(7) . . ? C4 C3 Ru1 70.4(5) . . ? C2 C3 Ru1 71.7(4) . . ? C5 C4 C3 106.8(7) . . ? C5 C4 Ru1 68.2(4) . . ? C3 C4 Ru1 68.8(4) . . ? C4 C5 C1 108.1(7) . . ? C4 C5 Ru1 72.3(4) . . ? C1 C5 Ru1 70.2(4) . . ? N1 C6 C7 178.4(11) . . ? N2 C8 C9 179.2(12) . . ? C15 C10 C11 123.6(7) . . ? C15 C10 P1 116.0(6) . . ? C11 C10 P1 120.3(6) . . ? C12 C11 C10 117.9(9) . . ? C11 C12 C13 118.0(9) . . ? C12 C13 C14 125.1(8) . . ? C15 C14 C13 118.2(9) . . ? C14 C15 C10 117.2(8) . . ? C21 C16 C17 117.6(8) . . ? C21 C16 P1 116.6(6) . . ? C17 C16 P1 125.7(6) . . ? C16 C17 C18 122.8(9) . . ? C19 C18 C17 118.4(10) . . ? C18 C19 C20 119.3(10) . . ? C19 C20 C21 122.0(10) . . ? C16 C21 C20 119.7(9) . . ? C23 C22 C27 116.1(8) . . ? C23 C22 P1 123.9(7) . . ? C27 C22 P1 120.0(5) . . ? C22 C23 C24 120.9(9) . . ? C25 C24 C23 122.9(9) . . ? C26 C25 C24 117.4(9) . . ? C25 C26 C27 119.8(9) . . ? C22 C27 C26 123.0(8) . . ? F5 P2 F3 174.8(18) . . ? F5 P2 F6 89.6(12) . . ? F3 P2 F6 95.6(16) . . ? F5 P2 F4 86.3(13) . . ? F3 P2 F4 88.5(14) . . ? F6 P2 F4 174.0(10) . . ? F5 P2 F2 101.8(13) . . ? F3 P2 F2 77.8(10) . . ? F6 P2 F2 89.1(8) . . ? F4 P2 F2 96.1(7) . . ? F5 P2 F1 89.8(13) . . ? F3 P2 F1 90.7(10) . . ? F6 P2 F1 91.3(7) . . ? F4 P2 F1 84.3(7) . . ? F2 P2 F1 168.4(9) . . ? C1 C2 H2 126.4 . . ? C3 C2 H2 127.4 . . ? Ru1 C2 H2 120.7 . . ? C4 C3 H3 128.5 . . ? C2 C3 H3 118.8 . . ? Ru1 C3 H3 139.5 . . ? C5 C4 H4 131.4 . . ? C3 C4 H4 121.8 . . ? Ru1 C4 H4 128.0 . . ? C4 C5 H5 114.6 . . ? C1 C5 H5 135.9 . . ? Ru1 C5 H5 133.1 . . ? C6 C7 H7A 111.3 . . ? C6 C7 H7B 108.0 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.1 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C8 C9 H9A 112.6 . . ? C8 C9 H9B 108.7 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 107.0 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C12 C11 H11 121.0 . . ? C10 C11 H11 120.6 . . ? C11 C12 H12 113.9 . . ? C13 C12 H12 127.6 . . ? C12 C13 H13 113.0 . . ? C14 C13 H13 121.8 . . ? C15 C14 H14 109.2 . . ? C13 C14 H14 132.6 . . ? C14 C15 H15 117.1 . . ? C10 C15 H15 125.8 . . ? C16 C17 H17 117.0 . . ? C18 C17 H17 117.7 . . ? C19 C18 H18 118.1 . . ? C17 C18 H18 123.4 . . ? C18 C19 H19 125.1 . . ? C20 C19 H19 115.5 . . ? C19 C20 H20 119.2 . . ? C21 C20 H20 118.9 . . ? C16 C21 H21 118.1 . . ? C20 C21 H21 122.1 . . ? C22 C23 H23 114.1 . . ? C24 C23 H23 124.7 . . ? C25 C24 H24 116.8 . . ? C23 C24 H24 120.3 . . ? C26 C25 H25 121.6 . . ? C24 C25 H25 121.0 . . ? C25 C26 H26 120.0 . . ? C27 C26 H26 120.2 . . ? C22 C27 H27 118.0 . . ? C26 C27 H27 119.0 . . ? _diffrn_measured_fraction_theta_max 0.615 _diffrn_measured_fraction_theta_full 0.615 _refine_diff_density_max 1.051 _refine_diff_density_min -0.962 _refine_diff_density_rms 0.155 #=============== data_compound_3a _database_code_CSD 191660 _chemical_compound_source 'Local laboratory' _exptl_crystal_description Plate _exptl_crystal_colour Red _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.03 _cell_measurement_temperature 298 _refine_ls_hydrogen_treatment refxyz _diffrn_measurement_device KappaCCD _computing_data_collection KappaCCD _computing_data_reduction 'Denzo and Scalepak (Otwinowski & Minor, 1997)' _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 35 loop_ _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_wavelength_id all _diffrn_orient_matrix_type X=UH _diffrn_orient_matrix_UB_11 0.03288 _diffrn_orient_matrix_UB_12 -0.03965 _diffrn_orient_matrix_UB_13 0.01563 _diffrn_orient_matrix_UB_21 -0.07007 _diffrn_orient_matrix_UB_22 -0.00197 _diffrn_orient_matrix_UB_23 0.02073 _diffrn_orient_matrix_UB_31 -0.05344 _diffrn_orient_matrix_UB_32 -0.02181 _diffrn_orient_matrix_UB_33 -0.03029 _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.575 _exptl_crystal_density_method 'not measured' _exptl_special_details ; ? ; _chemical_formula_weight 1441.889 _diffrn_radiation_type ' MoK¥a' loop_ _symmetry_equiv_pos_as_xyz +X,+Y,+Z -X,-Y,-Z '-X,+Y+ 1/2,-Z+ 1/2' '+X,-Y+ 1/2,+Z+ 1/2' _symmetry_space_group_name_H-M 'P 21/c ' _symmetry_cell_setting Monoclinic _chemical_formula_moiety 'C65 H56 B2 Cl2 F8 O2 P2 Ru2 S2 ' _chemical_formula_sum 'C65 H56 B2 Cl2 F8 O2 P2 Ru2 S2 ' _chemical_name_systematic ; ? ; _cell_length_a 10.8350(14) _cell_length_b 22.267(4) _cell_length_c 25.606(4) _cell_angle_alpha 90.00 _cell_angle_beta 100.057(7) _cell_angle_gamma 90.00 _cell_volume 6083.(2) _diffrn_reflns_number 14871 _diffrn_reflns_theta_max 30.32 _diffrn_reflns_theta_min 1.62 _diffrn_reflns_theta_full 30.32 _computing_structure_solution 'DIRDIF (Buerskens et al., 1992)' _atom_sites_solution_primary vecmap _atom_sites_solution_secondary difmap _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_coefficient_mu 0.78 _exptl_crystal_F_000 2911 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 'Waasmaier & Kirfel, 1995' 'H ' 'H ' 0.0000 0.0000 'Waasmaier & Kirfel, 1995' 'B ' 'B ' 0.0013 0.0007 'Waasmaier & Kirfel, 1995' Cl Cl 0.1484 0.1585 'Waasmaier & Kirfel, 1995' 'F ' 'F ' 0.0171 0.0103 'Waasmaier & Kirfel, 1995' 'O ' 'O ' 0.0106 0.0060 'Waasmaier & Kirfel, 1995' 'P ' 'P ' 0.1023 0.0942 'Waasmaier & Kirfel, 1995' Ru Ru -1.2594 0.8363 'Waasmaier & Kirfel, 1995' 'S ' 'S ' 0.1246 0.1234 'Waasmaier & Kirfel, 1995' # Refinement statistics _reflns_d_resolution_low 2.51 _reflns_d_resolution_high 0.59 _reflns_limit_h_max 14 _reflns_limit_h_min 0 _reflns_limit_k_max 31 _reflns_limit_k_min 0 _reflns_limit_l_max 35 _reflns_limit_l_min -36 _refine_ls_matrix_type full _refine_ls_shift/su_max 0.018 _refine_ls_shift/su_mean 0.012 _reflns_number_total 17358 _refine_ls_R_factor_all 0.240 _refine_ls_wR_factor_all 0.277 _refine_ls_goodness_of_fit_all 1.297 _reflns_number_gt 4446 _reflns_threshold_expression 'I> 3.00 sigma(I)' _refine_ls_R_factor_gt 0.065 _refine_ls_wR_factor_gt 0.098 _refine_ls_goodness_of_fit_gt 1.137 _refine_ls_number_reflns 4446 _refine_ls_number_parameters 735 _refine_ls_number_restraints 0 _refine_ls_number_constraints 47 _refine_ls_wR_factor_ref 0.098 _refine_ls_goodness_of_fit_ref 1.137 _refine_ls_structure_factor_coef F^2^ _refine_special_details ; Refinement on F^2^. ; _refine_ls_weighting_scheme sigma _refine_ls_weighting_details ; w = exp ( 3.00 sin(¥q)/¥l^2^ )/ s^2^(Fo^2^) + 0.00200 * Fo^2^ ; _refine_ls_extinction_method none _refine_ls_extinction_coef ? _computing_structure_refinement 'maXus(Mackay et al., 1999)' _computing_molecular_graphics 'Ortep (Johnson, 1976)' _computing_publication_material 'maXus(Mackay et al., 1999)' _atom_sites_solution_hydrogens geom _refine_diff_density_max 0.72 _refine_diff_density_min -1.12 _refine_diff_density_rms 0.37 #================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_adp_type Ru1 0.62749(12) 0.09354(6) 0.39204(5) 0.0389(8) 1.00 Uij Ru2 0.63508(13) 0.21454(7) 0.40347(5) 0.0413(9) 1.00 Uij Cl1 0.1218(13) 0.3490(11) 0.4247(5) 0.360(19) 1.00 Uij Cl2 -0.0363(13) 0.4446(7) 0.4296(6) 0.319(14) 1.00 Uij S1 0.6768(3) 0.1616(2) 0.32843(14) 0.042(3) 1.00 Uij S2 0.4513(3) 0.1577(2) 0.37353(14) 0.042(3) 1.00 Uij P1 0.5617(4) 0.0241(2) 0.32209(16) 0.041(3) 1.00 Uij P2 0.5782(4) 0.2970(2) 0.34580(16) 0.044(3) 1.00 Uij F1 0.323(2) 0.1964(7) 0.0930(7) 0.199(17) 1.00 Uij F2 0.3125(18) 0.1155(9) 0.0551(7) 0.175(16) 1.00 Uij F3 0.4254(16) 0.1913(7) 0.0305(6) 0.178(15) 1.00 Uij F4 0.4852(16) 0.1355(13) 0.0971(11) 0.28(2) 1.00 Uij F5 -0.0001(16) 0.4729(7) 0.0837(5) 0.261(19) 1.00 Uij F6 0.0181(14) 0.3987(15) 0.1412(12) 0.201(15) 1.00 Uij F7 -0.109(3) 0.3930(12) 0.0712(6) 0.30(3) 1.00 Uij F8 -0.1636(18) 0.4468(12) 0.1101(14) 0.40(3) 1.00 Uij O1 -0.054(3) 0.7820(13) 0.4063(16) 0.23(3) 1.00 Uij O2 0.271(2) 0.6023(13) 0.4142(15) 0.22(3) 1.00 Uij C1 0.7284(16) 0.1119(9) 0.4722(7) 0.045(12) 1.00 Uij C2 0.6221(17) 0.0772(8) 0.4757(6) 0.049(11) 1.00 Uij C3 0.6325(16) 0.0238(8) 0.4530(6) 0.048(11) 1.00 Uij C4 0.7512(19) 0.0206(10) 0.4349(6) 0.055(14) 1.00 Uij C5 0.8097(14) 0.0758(8) 0.4457(6) 0.049(10) 1.00 Uij C6 0.7318(16) 0.1749(9) 0.4772(6) 0.053(11) 1.00 Uij C7 0.6348(17) 0.2130(9) 0.4890(6) 0.052(13) 1.00 Uij C8 0.6511(16) 0.2706(7) 0.4766(6) 0.051(10) 1.00 Uij C9 0.7668(18) 0.2756(9) 0.4576(6) 0.058(12) 1.00 Uij C10 0.8189(14) 0.2174(9) 0.4586(6) 0.056(11) 1.00 Uij C11 0.5452(14) -0.0509(7) 0.3492(6) 0.045(10) 1.00 Uij C12 0.4455(15) -0.0649(9) 0.3747(6) 0.050(11) 1.00 Uij C13 0.4385(18) -0.1202(9) 0.3976(6) 0.057(12) 1.00 Uij C14 0.531(2) -0.1616(9) 0.3971(6) 0.064(14) 1.00 Uij C15 0.6319(17) -0.1481(9) 0.3736(7) 0.070(13) 1.00 Uij C16 0.6381(17) -0.0942(9) 0.3496(7) 0.055(14) 1.00 Uij C17 0.4170(14) 0.0370(8) 0.2758(6) 0.043(10) 1.00 Uij C18 0.404(2) 0.0878(10) 0.2442(8) 0.085(16) 1.00 Uij C19 0.302(2) 0.0942(11) 0.2027(9) 0.086(17) 1.00 Uij C20 0.208(2) 0.0540(13) 0.1957(8) 0.075(17) 1.00 Uij C21 0.2159(19) 0.0052(13) 0.2275(9) 0.085(17) 1.00 Uij C22 0.3203(17) -0.0039(9) 0.2667(7) 0.070(13) 1.00 Uij C23 0.6758(14) 0.0158(7) 0.2787(6) 0.040(9) 1.00 Uij C24 0.8024(16) 0.0185(8) 0.2972(6) 0.055(12) 1.00 Uij C25 0.8896(17) 0.0105(8) 0.2662(10) 0.067(14) 1.00 Uij C26 0.854(2) 0.0016(11) 0.2130(9) 0.085(17) 1.00 Uij C27 0.728(2) -0.0001(9) 0.1933(7) 0.090(15) 1.00 Uij C28 0.6380(16) 0.0059(8) 0.2247(7) 0.068(11) 1.00 Uij C29 0.5680(16) 0.3668(7) 0.3809(6) 0.048(10) 1.00 Uij C30 0.6350(17) 0.4183(7) 0.3731(6) 0.063(11) 1.00 Uij C31 0.623(2) 0.4699(10) 0.3988(8) 0.085(17) 1.00 Uij C32 0.537(2) 0.4750(9) 0.4320(7) 0.073(14) 1.00 Uij C33 0.470(2) 0.4251(13) 0.4403(8) 0.069(17) 1.00 Uij C34 0.4794(18) 0.3727(9) 0.4147(7) 0.059(13) 1.00 Uij C35 0.6956(17) 0.3117(7) 0.3045(7) 0.044(11) 1.00 Uij C36 0.8185(19) 0.3084(9) 0.3267(7) 0.067(13) 1.00 Uij C37 0.9145(16) 0.3225(9) 0.2969(8) 0.064(13) 1.00 Uij C38 0.8821(16) 0.3365(10) 0.2439(8) 0.075(14) 1.00 Uij C39 0.7584(17) 0.3394(9) 0.2221(7) 0.084(14) 1.00 Uij C40 0.6678(17) 0.3270(8) 0.2526(8) 0.067(13) 1.00 Uij C41 0.4312(17) 0.2951(9) 0.2996(7) 0.049(12) 1.00 Uij C42 0.409(2) 0.2499(10) 0.2616(8) 0.072(15) 1.00 Uij C43 0.301(3) 0.2501(10) 0.2213(8) 0.078(16) 1.00 Uij C44 0.2143(18) 0.2922(13) 0.2229(9) 0.078(17) 1.00 Uij C45 0.231(2) 0.3349(13) 0.2595(9) 0.075(19) 1.00 Uij C46 0.3395(17) 0.3365(10) 0.2978(7) 0.065(14) 1.00 Uij C47 0.8287(16) 0.1627(9) 0.3111(7) 0.045(14) 1.00 Uij C48 0.8296(14) 0.1682(8) 0.2579(6) 0.060(11) 1.00 Uij C49 0.9432(19) 0.1690(9) 0.2397(7) 0.073(14) 1.00 Uij C50 1.0508(18) 0.1653(10) 0.2747(10) 0.079(16) 1.00 Uij C51 1.0526(16) 0.1587(11) 0.3273(9) 0.092(17) 1.00 Uij C52 0.9389(16) 0.1570(9) 0.3453(7) 0.074(14) 1.00 Uij C53 0.3523(12) 0.1495(9) 0.4217(6) 0.037(10) 1.00 Uij C54 0.2980(15) 0.0939(8) 0.4266(6) 0.058(12) 1.00 Uij C55 0.2066(17) 0.0858(10) 0.4592(8) 0.068(14) 1.00 Uij C56 0.1779(17) 0.1344(11) 0.4867(8) 0.073(14) 1.00 Uij C57 0.2306(19) 0.1893(12) 0.4828(7) 0.079(16) 1.00 Uij C58 0.3172(16) 0.1975(9) 0.4485(7) 0.061(12) 1.00 Uij C59 0.106(3) 0.428(2) 0.4512(18) 0.48(5) 1.00 Uij C60 0.2362(14) 0.7037(11) 0.3958(7) 0.16(2) 1.00 Uij C61 0.1501(18) 0.7464(8) 0.3954(6) 0.11(2) 1.00 Uij C62 0.0284(18) 0.7241(10) 0.4074(9) 0.18(4) 1.00 Uij C63 -0.0097(14) 0.6682(10) 0.4220(6) 0.36(8) 1.00 Uij C64 0.0696(18) 0.6304(8) 0.4223(6) 0.17(4) 1.00 Uij C65 0.1925(19) 0.6453(10) 0.4098(9) 0.20(4) 1.00 Uij B1 0.393(5) 0.1596(16) 0.0711(19) 0.15(3) 1.00 Uij B2 -0.0410(11) 0.4322(7) 0.1059(5) 0.124(9) 1.00 Uiso H2 0.5(4) 0.09(7) 0.48(11) 0.052093 1.00 Uiso H3 0.587(8) -0.002(5) 0.456(4) 0.053540 1.00 Uiso H4 0.771(5) -0.008(4) 0.409(3) 0.073253 1.00 Uiso H5 0.877(5) 0.091(4) 0.429(3) 0.048157 1.00 Uiso H7 0.556(5) 0.197(4) 0.494(3) 0.061631 1.00 Uiso H8 0.595(12) 0.306(6) 0.480(5) 0.044982 1.00 Uiso H9 0.790672 0.308633 0.437420 0.058334 1.00 Uiso H10 0.883333 0.205772 0.439228 0.051826 1.00 Uiso H12 0.379488 -0.036502 0.376004 0.059176 1.00 Uiso H13 0.367955 -0.128816 0.414376 0.059250 1.00 Uiso H14 0.524102 -0.200039 0.413363 0.070596 1.00 Uiso H15 0.698048 -0.176807 0.373426 0.069664 1.00 Uiso H16 0.707762 -0.084593 0.332530 0.067998 1.00 Uiso H18 0.467387 0.118573 0.250712 0.087837 1.00 Uiso H19 0.298060 0.127713 0.178798 0.089679 1.00 Uiso H20 0.135339 0.061216 0.168924 0.081009 1.00 Uiso H21 0.150849 -0.024565 0.222936 0.098390 1.00 Uiso H22 0.325765 -0.039606 0.288084 0.063183 1.00 Uiso H24 0.832117 0.025854 0.334216 0.068693 1.00 Uiso H25 0.977248 0.012196 0.281109 0.079154 1.00 Uiso H26 0.911774 -0.004335 0.188850 0.100482 1.00 Uiso H27 0.701427 -0.004851 0.155700 0.081107 1.00 Uiso H28 0.550424 0.003178 0.209988 0.059253 1.00 Uiso H30 0.694706 0.417172 0.349459 0.056399 1.00 Uiso H31 0.675608 0.503458 0.394339 0.090171 1.00 Uiso H32 0.523468 0.512392 0.448789 0.072794 1.00 Uiso H33 0.409379 0.428513 0.463543 0.095877 1.00 Uiso H34 0.425593 0.340139 0.420806 0.068248 1.00 Uiso H36 0.844405 0.296229 0.362923 0.074650 1.00 Uiso H37 1.001719 0.323973 0.312401 0.074855 1.00 Uiso H39 0.733810 0.351575 0.185826 0.077684 1.00 Uiso H40 0.580668 0.327706 0.236873 0.076880 1.00 Uiso H42 0.490041 0.237332 0.254930 0.076476 1.00 Uiso H43 0.289620 0.220294 0.193741 0.083702 1.00 Uiso H44 0.138886 0.291855 0.196814 0.085565 1.00 Uiso H45 0.165904 0.364165 0.258919 0.098712 1.00 Uiso H46 0.347767 0.367409 0.324318 0.066722 1.00 Uiso H48 0.768871 0.169226 0.231712 0.060364 1.00 Uiso H49 0.947315 0.173519 0.202759 0.076276 1.00 Uiso H50 1.125936 0.166608 0.259647 0.089917 1.00 Uiso H51 1.130940 0.155786 0.351399 0.095499 1.00 Uiso H52 0.939714 0.152529 0.382628 0.071478 1.00 Uiso H54 0.323021 0.060032 0.407719 0.065370 1.00 Uiso H55 0.163881 0.048907 0.463650 0.075915 1.00 Uiso H56 0.118764 0.129465 0.510230 0.073659 1.00 Uiso H57 0.207685 0.222912 0.502596 0.100309 1.00 Uiso H58 0.352686 0.236374 0.444334 0.061746 1.00 Uiso loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ru1 0.0447(8) 0.0370(10) 0.0329(8) 0.0027(8) 0.0017(6) 0.0038(7) Ru2 0.0498(9) 0.0396(10) 0.0325(8) -.0024(8) 0.0026(7) 0.0009(7) Cl1 0.218(15) 0.55(3) 0.285(15) 0.128(18) -.066(11) -.165(18) Cl2 0.211(12) 0.337(19) 0.376(18) 0.022(11) -.080(11) 0.010(13) S1 0.051(2) 0.039(3) 0.034(2) -.002(2) 0.001(2) 0.003(2) S2 0.047(2) 0.041(3) 0.036(2) 0.003(2) 0.006(2) 0.001(2) P1 0.044(3) 0.037(3) 0.039(3) 0.004(2) 0.004(2) 0.000(2) P2 0.052(3) 0.037(3) 0.039(3) -.006(2) 0.005(2) 0.000(2) F1 0.33(3) 0.092(12) 0.181(16) -.009(14) 0.142(17) -.019(11) F2 0.19(2) 0.131(16) 0.195(17) -.019(14) 0.001(14) -.008(13) F3 0.246(17) 0.148(17) 0.148(14) 0.005(13) 0.120(13) 0.038(12) F4 0.108(14) 0.35(3) 0.37(4) 0.000(16) -.015(17) 0.20(3) F5 0.110(13) 0.33(2) 0.34(3) -.036(14) 0.037(15) 0.22(2) F6 0.259(18) 0.187(19) 0.135(12) 0.003(15) -.051(11) 0.026(12) F7 0.37(4) 0.32(3) 0.16(2) -.06(3) -.13(2) -.02(2) F8 0.22(2) 0.30(4) 0.71(7) 0.03(2) 0.32(4) 0.07(4) O1 0.16(2) 0.36(4) 0.15(3) 0.04(2) 0.008(19) 0.01(3) O2 0.22(3) 0.24(4) 0.18(3) -.01(3) 0.02(2) -.06(3) C1 0.060(13) 0.028(15) 0.043(12) -.008(11) -.002(10) 0.017(10) C2 0.095(14) 0.022(13) 0.026(10) 0.014(10) -.010(9) -.002(8) C3 0.059(12) 0.045(13) 0.038(11) -.009(10) 0.008(10) 0.016(9) C4 0.089(15) 0.04(2) 0.034(10) 0.006(13) -.004(11) 0.002(11) C5 0.042(10) 0.051(14) 0.050(10) 0.013(9) -.004(9) 0.012(9) C6 0.068(11) 0.056(17) 0.031(10) -.002(10) -.007(9) -.005(10) C7 0.085(15) 0.036(16) 0.030(9) -.021(13) -.008(9) -.003(10) C8 0.081(13) 0.031(13) 0.035(10) 0.001(9) -.006(9) -.008(8) C9 0.073(14) 0.069(18) 0.026(9) -.036(12) -.013(9) 0.002(9) C10 0.059(11) 0.050(14) 0.053(11) -.013(10) -.013(9) 0.002(10) C11 0.061(10) 0.031(12) 0.041(10) 0.002(9) 0.008(8) 0.003(9) C12 0.059(11) 0.045(16) 0.045(10) -.003(10) 0.009(9) -.002(10) C13 0.082(15) 0.043(14) 0.044(10) -.007(11) 0.013(10) 0.001(9) C14 0.124(16) 0.024(15) 0.043(11) -.013(13) 0.018(12) 0.007(10) C15 0.099(13) 0.056(15) 0.055(12) 0.025(12) 0.031(11) 0.005(11) C16 0.064(14) 0.046(14) 0.056(12) 0.006(12) 0.029(11) 0.011(12) C17 0.053(11) 0.030(12) 0.043(11) 0.009(9) 0.003(9) -.004(8) C18 0.118(19) 0.034(17) 0.089(15) -.009(15) -.042(14) 0.000(13) C19 0.11(2) 0.065(17) 0.068(18) 0.005(15) -.034(15) -.007(14) C20 0.062(15) 0.10(2) 0.063(14) 0.017(15) -.005(12) 0.001(15) C21 0.067(14) 0.11(3) 0.070(16) -.011(15) 0.002(12) -.002(17) C22 0.064(12) 0.081(16) 0.060(13) -.003(11) -.009(10) 0.015(11) C23 0.036(10) 0.040(11) 0.046(10) 0.006(7) 0.019(9) -.001(8) C24 0.068(12) 0.047(17) 0.049(11) -.002(10) 0.021(11) -.005(10) C25 0.060(13) 0.065(14) 0.076(19) 0.004(10) 0.019(15) -.001(12) C26 0.069(18) 0.12(2) 0.072(16) -.018(15) 0.042(15) -.019(14) C27 0.116(17) 0.111(19) 0.041(13) -.025(13) 0.021(13) -.022(11) C28 0.067(12) 0.089(14) 0.047(11) -.015(10) 0.018(11) -.016(9) C29 0.073(13) 0.027(12) 0.044(11) -.006(9) 0.017(10) -.001(8) C30 0.087(14) 0.036(11) 0.062(11) -.013(10) 0.013(10) -.005(8) C31 0.121(18) 0.052(19) 0.082(15) -.022(16) 0.039(14) -.021(13) C32 0.120(18) 0.038(14) 0.056(13) 0.010(12) 0.013(13) -.021(10) C33 0.123(17) 0.02(3) 0.062(14) -.004(16) 0.037(12) -.002(15) C34 0.071(15) 0.047(14) 0.059(13) -.007(11) 0.025(12) -.011(10) C35 0.066(13) 0.024(12) 0.041(11) -.004(9) 0.005(10) -.009(8) C36 0.070(14) 0.090(19) 0.040(12) -.008(12) 0.008(12) 0.013(11) C37 0.045(12) 0.079(18) 0.064(14) -.008(10) -.002(12) 0.005(12) C38 0.058(12) 0.091(19) 0.073(15) 0.004(12) 0.012(11) 0.017(13) C39 0.094(13) 0.114(15) 0.045(13) 0.044(12) 0.034(12) 0.047(11) C40 0.055(13) 0.085(18) 0.059(14) 0.016(11) 0.021(12) 0.010(11) C41 0.077(13) 0.016(14) 0.052(13) 0.003(11) 0.012(11) 0.011(10) C42 0.079(18) 0.044(16) 0.088(16) 0.008(13) -.007(14) 0.010(12) C43 0.10(2) 0.044(17) 0.076(14) -.002(15) -.025(14) -.009(12) C44 0.069(13) 0.08(2) 0.080(19) -.002(14) 0.017(13) 0.004(17) C45 0.042(16) 0.10(3) 0.079(15) 0.001(18) 0.016(13) 0.007(16) C46 0.066(11) 0.075(17) 0.052(13) 0.015(13) 0.013(11) -.014(12) C47 0.030(12) 0.058(15) 0.048(14) 0.000(12) 0.013(12) 0.006(11) C48 0.058(10) 0.075(17) 0.044(10) -.009(10) 0.008(9) 0.003(10) C49 0.073(15) 0.10(2) 0.048(11) 0.005(13) 0.024(12) 0.007(11) C50 0.050(13) 0.11(2) 0.080(16) 0.003(13) 0.028(14) 0.024(15) C51 0.040(11) 0.15(2) 0.085(18) 0.004(14) -.010(13) 0.032(17) C52 0.059(11) 0.103(16) 0.058(12) -.013(13) 0.014(10) 0.023(12) C53 0.031(8) 0.045(14) 0.037(10) 0.005(9) 0.010(8) 0.008(10) C54 0.057(11) 0.037(14) 0.081(13) 0.007(10) 0.030(11) 0.001(11) C55 0.068(13) 0.051(18) 0.082(14) 0.005(12) 0.009(11) 0.023(13) C56 0.054(12) 0.10(2) 0.065(14) -.018(12) 0.006(10) 0.019(13) C57 0.072(15) 0.11(3) 0.052(14) 0.010(15) 0.012(13) -.024(14) C58 0.066(12) 0.055(16) 0.061(12) -.008(10) 0.020(10) -.008(10) C59 0.19(3) 0.73(8) 0.49(7) 0.20(4) -.07(3) -.15(5) C60 0.22(3) 0.17(3) 0.070(16) 0.13(3) -.063(16) -.063(19) C61 0.08(2) 0.17(3) 0.061(16) 0.00(2) 0.008(15) -.007(16) C62 0.13(3) 0.34(9) 0.073(16) 0.14(4) -.026(16) 0.00(3) C63 0.25(9) 0.79(12) 0.03(3) 0.28(9) -.04(4) -.07(5) C64 0.12(5) 0.25(6) 0.14(4) -.09(4) 0.01(3) -.02(3) C65 0.27(5) 0.21(4) 0.096(18) 0.20(4) -.06(2) -.06(2) B1 0.15(4) 0.072(19) 0.23(4) 0.07(3) 0.13(4) 0.04(3) _geom_special_details ; All standard uncertainties (except dihedral angles between l.s. planes) are estimated using the full covariance matrix. The standard uncertainties in cell dimensions are are used in calculating the standard uncertainties of bond distances, angles and torsion angles. Angles between l.s. planes have standard uncertainties calculated from atomic positional standard uncertainties; the errors in cell dimensions are not used in this case. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 Ru2 2.7097(10) . . ? Ru1 S1 2.353(2) . . ? Ru1 S2 2.365(2) . . ? Ru1 P1 2.380(2) . . ? Ru1 C1 2.189(9) . . ? Ru1 C2 2.184(8) . . ? Ru1 C3 2.196(8) . . ? Ru1 C4 2.265(10) . . ? Ru1 C5 2.234(8) . . ? Ru2 S1 2.364(2) . . ? Ru2 S2 2.371(2) . . ? Ru2 P2 2.370(3) . . ? Ru2 C6 2.179(9) . . ? Ru2 C7 2.191(8) . . ? Ru2 C8 2.233(8) . . ? Ru2 C9 2.261(8) . . ? Ru2 C10 2.233(8) . . ? Cl1 C59 1.91(2) . . ? Cl2 C59 1.59(2) . . ? S1 C47 1.777(8) . . ? S2 C53 1.780(7) . . ? P1 C11 1.828(9) . . ? P1 C17 1.816(9) . . ? P1 C23 1.810(7) . . ? P2 C29 1.807(8) . . ? P2 C35 1.820(8) . . ? P2 C41 1.812(11) . . ? F1 B1 1.304(13) . . ? F2 B1 1.33(3) . . ? F3 B1 1.35(2) . . ? F4 B1 1.22(2) . . ? F5 B2 1.1960 . . ? F6 B2 1.2569 . . ? F7 B2 1.3673 . . ? F8 B2 1.3899 . . ? O1 C62 1.5643 . . ? O2 C65 1.2761 . . ? C1 C2 1.403(12) . . ? C1 C5 1.447(11) . . ? C1 C6 1.409(12) . . ? C2 C3 1.339(11) . . ? C3 C4 1.443(11) . . ? C4 C5 1.390(13) . . ? C6 C7 1.423(12) . . ? C6 C10 1.472(11) . . ? C7 C8 1.341(11) . . ? C8 C9 1.428(11) . . ? C9 C10 1.412(12) . . ? C11 C12 1.393(10) . . ? C11 C16 1.392(11) . . ? C12 C13 1.372(12) . . ? C13 C14 1.361(13) . . ? C14 C15 1.371(12) . . ? C15 C16 1.356(12) . . ? C17 C18 1.383(13) . . ? C17 C22 1.377(11) . . ? C18 C19 1.405(15) . . ? C19 C20 1.347(15) . . ? C20 C21 1.35(2) . . ? C21 C22 1.390(13) . . ? C23 C24 1.372(11) . . ? C23 C28 1.390(10) . . ? C24 C25 1.349(11) . . ? C25 C26 1.364(14) . . ? C26 C27 1.376(14) . . ? C27 C28 1.372(12) . . ? C29 C30 1.390(11) . . ? C29 C34 1.407(11) . . ? C30 C31 1.343(12) . . ? C31 C32 1.371(12) . . ? C32 C33 1.363(14) . . ? C33 C34 1.352(14) . . ? C35 C36 1.355(12) . . ? C35 C40 1.353(11) . . ? C36 C37 1.428(11) . . ? C37 C38 1.377(12) . . ? C38 C39 1.359(12) . . ? C39 C40 1.385(11) . . ? C41 C42 1.392(13) . . ? C41 C46 1.350(12) . . ? C42 C43 1.415(14) . . ? C43 C44 1.335(14) . . ? C44 C45 1.32(2) . . ? C45 C46 1.394(13) . . ? C47 C48 1.370(11) . . ? C47 C52 1.357(12) . . ? C48 C49 1.391(11) . . ? C49 C50 1.343(13) . . ? C50 C51 1.352(13) . . ? C51 C52 1.388(12) . . ? C53 C54 1.386(12) . . ? C53 C58 1.360(12) . . ? C54 C55 1.414(11) . . ? C55 C56 1.355(14) . . ? C56 C57 1.360(14) . . ? C57 C58 1.406(11) . . ? C60 C61 1.3308 . . ? C60 C65 1.4499 . . ? C61 C62 1.4904 . . ? C62 C63 1.3825 . . ? C63 C64 1.2019 . . ? C64 C65 1.4617 . . ? 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Ru2 Ru1 S1 55.14(6) . . . ? Ru2 Ru1 S2 55.20(6) . . . ? Ru2 Ru1 P1 136.64(7) . . . ? Ru2 Ru1 C1 73.3(3) . . . ? Ru2 Ru1 C2 93.7(3) . . . ? Ru2 Ru1 C3 129.1(3) . . . ? Ru2 Ru1 C4 131.1(3) . . . ? Ru2 Ru1 C5 95.9(3) . . . ? S1 Ru1 S2 75.23(7) . . . ? S1 Ru1 P1 88.39(8) . . . ? S1 Ru1 C1 113.1(3) . . . ? S1 Ru1 C2 146.5(3) . . . ? S1 Ru1 C3 165.2(3) . . . ? S1 Ru1 C4 127.6(3) . . . ? S1 Ru1 C5 104.8(2) . . . ? S2 Ru1 P1 96.70(8) . . . ? S2 Ru1 C1 109.2(3) . . . ? S2 Ru1 C2 97.9(2) . . . ? S2 Ru1 C3 119.3(3) . . . ? S2 Ru1 C4 156.8(2) . . . ? S2 Ru1 C5 145.6(2) . . . ? P1 Ru1 C1 149.6(3) . . . ? P1 Ru1 C2 125.1(3) . . . ? P1 Ru1 C3 92.4(3) . . . ? P1 Ru1 C4 88.4(3) . . . ? P1 Ru1 C5 117.7(2) . . . ? C1 Ru1 C2 37.4(3) . . . ? C1 Ru1 C3 61.3(4) . . . ? C1 Ru1 C4 61.5(4) . . . ? C1 Ru1 C5 38.2(3) . . . ? C2 Ru1 C3 35.6(3) . . . ? C2 Ru1 C4 61.3(3) . . . ? C2 Ru1 C5 62.6(3) . . . ? C3 Ru1 C4 37.7(3) . . . ? C3 Ru1 C5 61.9(3) . . . ? C4 Ru1 C5 36.0(3) . . . ? Ru1 Ru2 S1 54.75(6) . . . ? Ru1 Ru2 S2 55.00(6) . . . ? Ru1 Ru2 P2 134.72(7) . . . ? Ru1 Ru2 C6 72.1(3) . . . ? Ru1 Ru2 C7 95.0(3) . . . ? Ru1 Ru2 C8 130.0(2) . . . ? Ru1 Ru2 C9 131.9(3) . . . ? Ru1 Ru2 C10 95.9(3) . . . ? S1 Ru2 S2 74.92(7) . . . ? S1 Ru2 P2 86.91(8) . . . ? S1 Ru2 C6 111.8(3) . . . ? S1 Ru2 C7 147.0(3) . . . ? S1 Ru2 C8 164.4(3) . . . ? S1 Ru2 C9 127.4(3) . . . ? S1 Ru2 C10 104.6(2) . . . ? S2 Ru2 P2 95.73(9) . . . ? S2 Ru2 C6 108.3(3) . . . ? S2 Ru2 C7 99.6(3) . . . ? S2 Ru2 C8 120.5(3) . . . ? S2 Ru2 C9 157.5(2) . . . ? S2 Ru2 C10 145.7(3) . . . ? P2 Ru2 C6 152.5(3) . . . ? P2 Ru2 C7 126.1(3) . . . ? P2 Ru2 C8 93.6(2) . . . ? P2 Ru2 C9 89.1(3) . . . ? P2 Ru2 C10 118.6(3) . . . ? C6 Ru2 C7 38.0(3) . . . ? C6 Ru2 C8 62.9(3) . . . ? C6 Ru2 C9 63.6(4) . . . ? C6 Ru2 C10 38.9(3) . . . ? C7 Ru2 C8 35.3(3) . . . ? C7 Ru2 C9 60.5(3) . . . ? C7 Ru2 C10 61.6(3) . . . ? C8 Ru2 C9 37.0(3) . . . ? C8 Ru2 C10 61.5(3) . . . ? C9 Ru2 C10 36.6(3) . . . ? Ru1 S1 Ru2 70.11(6) . . . ? Ru1 S1 C47 120.9(4) . . . ? Ru2 S1 C47 120.8(4) . . . ? Ru1 S2 Ru2 69.81(6) . . . ? Ru1 S2 C53 111.2(3) . . . ? Ru1 P1 C11 110.1(3) . . . ? Ru1 P1 C17 119.9(3) . . . ? Ru1 P1 C23 112.4(3) . . . ? C11 P1 C17 105.2(4) . . . ? C11 P1 C23 105.2(4) . . . ? C17 P1 C23 102.7(4) . . . ? Ru2 P2 C29 112.9(3) . . . ? Ru2 P2 C35 111.6(3) . . . ? Ru2 P2 C41 119.5(3) . . . ? C29 P2 C35 104.2(4) . . . ? C29 P2 C41 102.8(5) . . . ? C35 P2 C41 104.4(4) . . . ? Ru1 C1 C2 71.1(5) . . . ? Ru1 C1 C5 72.6(5) . . . ? Ru1 C1 C6 105.8(7) . . . ? C2 C1 C5 107.3(9) . . . ? C2 C1 C6 123.5(9) . . . ? C5 C1 C6 126.0(9) . . . ? Ru1 C2 C1 71.5(5) . . . ? Ru1 C2 C3 72.7(5) . . . ? C1 C2 C3 109.2(8) . . . ? Ru1 C3 C2 71.7(5) . . . ? Ru1 C3 C4 73.7(5) . . . ? C2 C3 C4 109.3(9) . . . ? Ru1 C4 C3 68.6(5) . . . ? Ru1 C4 C5 70.8(6) . . . ? C3 C4 C5 107.1(9) . . . ? Ru1 C5 C1 69.2(5) . . . ? Ru1 C5 C4 73.2(6) . . . ? C1 C5 C4 106.9(8) . . . ? Ru2 C6 C1 108.9(7) . . . ? Ru2 C6 C7 71.4(5) . . . ? Ru2 C6 C10 72.5(5) . . . ? C1 C6 C7 127.1(9) . . . ? C1 C6 C10 128.2(9) . . . ? C7 C6 C10 103.0(9) . . . ? Ru2 C7 C6 70.6(5) . . . ? Ru2 C7 C8 74.1(5) . . . ? C6 C7 C8 112.8(8) . . . ? Ru2 C8 C7 70.7(5) . . . ? Ru2 C8 C9 72.6(5) . . . ? C7 C8 C9 108.3(9) . . . ? Ru2 C9 C8 70.4(5) . . . ? Ru2 C9 C10 70.6(5) . . . ? C8 C9 C10 107.1(8) . . . ? Ru2 C10 C6 68.5(5) . . . ? Ru2 C10 C9 72.8(5) . . . ? C6 C10 C9 108.6(8) . . . ? P1 C11 C12 121.2(7) . . . ? P1 C11 C16 121.1(7) . . . ? C12 C11 C16 117.4(9) . . . ? C11 C12 C13 120.5(9) . . . ? C12 C13 C14 120.6(9) . . . ? C13 C14 C15 120.0(10) . . . ? C14 C15 C16 119.9(9) . . . ? C11 C16 C15 121.6(8) . . . ? P1 C17 C18 119.8(8) . . . ? P1 C17 C22 123.3(8) . . . ? C18 C17 C22 116.7(9) . . . ? C17 C18 C19 120.6(11) . . . ? C18 C19 C20 121.0(12) . . . ? C19 C20 C21 119.0(12) . . . ? C20 C21 C22 120.9(12) . . . ? C17 C22 C21 121.6(10) . . . ? P1 C23 C24 122.1(6) . . . ? P1 C23 C28 120.9(6) . . . ? C24 C23 C28 117.0(7) . . . ? C23 C24 C25 123.5(9) . . . ? C24 C25 C26 120.3(10) . . . ? C25 C26 C27 117.3(9) . . . ? C26 C27 C28 123.0(9) . . . ? C23 C28 C27 118.9(9) . . . ? P2 C29 C30 124.0(7) . . . ? P2 C29 C34 119.5(7) . . . ? C30 C29 C34 116.2(8) . . . ? C29 C30 C31 122.5(8) . . . ? C30 C31 C32 120.6(10) . . . ? C31 C32 C33 118.0(10) . . . ? C32 C33 C34 122.6(9) . . . ? C29 C34 C33 119.9(9) . . . ? C36 C35 C40 117.3(9) . . . ? P2 C35 C36 118.8(7) . . . ? P2 C35 C40 123.9(8) . . . ? C35 C36 C37 121.2(9) . . . ? C36 C37 C38 119.5(9) . . . ? C37 C38 C39 118.5(8) . . . ? C38 C39 C40 120.3(9) . . . ? C35 C40 C39 123.1(10) . . . ? P2 C41 C42 120.0(8) . . . ? P2 C41 C46 124.3(9) . . . ? C42 C41 C46 115.7(10) . . . ? C41 C42 C43 121.9(11) . . . ? C42 C43 C44 118.4(11) . . . ? C43 C44 C45 121.0(12) . . . ? C44 C45 C46 120.8(11) . . . ? C41 C46 C45 122.1(11) . . . ? S1 C47 C48 114.6(8) . . . ? S1 C47 C52 126.0(7) . . . ? C48 C47 C52 119.4(7) . . . ? C47 C48 C49 119.7(8) . . . ? C48 C49 C50 119.4(8) . . . ? C49 C50 C51 122.1(8) . . . ? C50 C51 C52 118.3(9) . . . ? C47 C52 C51 121.1(8) . . . ? S2 C53 C54 118.1(7) . . . ? S2 C53 C58 121.7(8) . . . ? C54 C53 C58 119.7(7) . . . ? C53 C54 C55 121.3(9) . . . ? C54 C55 C56 116.9(10) . . . ? C55 C56 C57 122.9(10) . . . ? C56 C57 C58 119.8(11) . . . ? C53 C58 C57 119.3(10) . . . ? Cl1 C59 Cl2 103.3(13) . . . ? C61 C60 C65 112.5873 . . . ? C60 C61 C62 113.8157 . . . ? O1 C62 C61 104.0329 . . . ? O1 C62 C63 123.3742 . . . ? C61 C62 C63 132.2916 . . . ? C62 C63 C64 112.6637 . . . ? C63 C64 C65 121.1090 . . . ? O2 C65 C60 116.8696 . . . ? O2 C65 C64 115.6439 . . . ? C60 C65 C64 127.4021 . . . ? F1 B1 F2 101.(2) . . . ? F1 B1 F3 104.5(12) . . . ? F1 B1 F4 121.(3) . . . ? F2 B1 F3 113.(2) . . . ? F2 B1 F4 106.(2) . . . ? F3 B1 F4 111.(2) . . . ? F5 B2 F6 127.3994 . . . ? F5 B2 F7 112.1532 . . . ? F5 B2 F8 107.4014 . . . ? F6 B2 F7 103.7399 . . . ? F6 B2 F8 117.2070 . . . ? F7 B2 F8 77.4584 . . . ? #============================================================= data_compound_4a _database_code_CSD 191661 _chemical_compound_source 'Local laboratory' _exptl_crystal_description Needle _exptl_crystal_colour Red _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.02 _cell_measurement_temperature 298 _refine_ls_hydrogen_treatment refxyz _diffrn_measurement_device KappaCCD _computing_data_collection KappaCCD _computing_data_reduction 'Denzo and Scalepak (Otwinowski & Minor, 1997)' _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 16 loop_ _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_wavelength_id all _cell_formula_units_Z 2 _exptl_crystal_density_diffrn 1.632 _exptl_crystal_density_method 'not measured' _exptl_special_details ; ? ; _chemical_formula_weight 851.927 _diffrn_radiation_type ' MoK¥a' loop_ _symmetry_equiv_pos_as_xyz +X,+Y,+Z '-X,+Y+ 1/2,-Z' _symmetry_space_group_name_H-M 'P 21 ' _symmetry_cell_setting Monoclinic _chemical_formula_moiety 'C35 H30 Cl2 Ru2 S4 ' _chemical_formula_sum 'C35 H30 Cl2 Ru2 S4 ' _chemical_name_systematic ; ? ; _cell_length_a 10.3140(5) _cell_length_b 13.4390(8) _cell_length_c 12.8140(9) _cell_angle_alpha 90.00 _cell_angle_beta 102.500(2) _cell_angle_gamma 90.00 _cell_volume 1734.0(2) _diffrn_reflns_number 6525 _diffrn_reflns_theta_max 27.06 _diffrn_reflns_theta_min 0.00 _diffrn_reflns_theta_full 27.06 _diffrn_reflns_av_R_equivalents 0.034 _computing_structure_solution 'DIRDIF (Buerskens et al., 1992)' _atom_sites_solution_primary vecmap _atom_sites_solution_secondary difmap _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? 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' 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _exptl_absorpt_coefficient_mu 1.290 _reflns_number_total 6517 _reflns_number_gt 5763 _reflns_threshold_expression >2sigma(I) _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even largeR . ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[¥s^2^(Fo^2^)+(0.0800P)^2^+0.5800P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.91(5) _refine_ls_number_reflns 6517 _refine_ls_number_parameters 397 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0563 _refine_ls_R_factor_gt 0.0495 _refine_ls_wR_factor_ref 0.1432 _refine_ls_wR_factor_gt 0.1381 _refine_ls_goodness_of_fit_ref 1.080 _refine_ls_restrained_S_all 1.080 _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 0.41136(5) 0.30301(4) 0.19461(4) 0.04473(15) Uani 1 1 d . . . Ru2 Ru 0.41589(5) 0.24909(3) -0.00490(4) 0.04345(15) Uani 1 1 d . . . Cl1 Cl 0.7461(8) 0.1653(8) 0.5396(7) 0.176(4) Uani 0.67 1 d p . . Cl2 Cl 0.785(2) 0.1742(7) 0.7551(9) 0.304(10) Uani 0.67 1 d p . . Cl3 Cl 0.9663(8) 0.0954(17) 0.6733(11) 0.327(12) Uani 0.67 1 d p . . S1 S 0.59392(16) 0.32619(13) 0.11414(14) 0.0454(4) Uani 1 1 d . . . S2 S 0.31567(17) 0.39529(13) 0.04033(14) 0.0449(4) Uani 1 1 d . . . S3 S 0.4990(2) 0.32973(17) -0.14432(15) 0.0597(5) Uani 1 1 d . . . S4 S 0.4419(2) 0.45908(17) 0.28628(17) 0.0585(5) Uani 1 1 d . . . C1 C 0.3414(9) 0.1484(7) 0.1772(7) 0.063(2) Uani 1 1 d . . . C2 C 0.2407(9) 0.2084(7) 0.2064(7) 0.065(2) Uani 1 1 d . . . C3 C 0.2920(9) 0.2512(8) 0.3085(7) 0.0644(19) Uani 1 1 d . . . C4 C 0.4224(10) 0.2169(8) 0.3437(7) 0.073(3) Uani 1 1 d . . . C5 C 0.4569(9) 0.1525(7) 0.2669(7) 0.063(2) Uani 1 1 d . . . C6 C 0.3453(8) 0.1189(6) 0.0695(7) 0.0534(18) Uani 1 1 d . . . C7 C 0.2464(9) 0.1457(6) -0.0238(7) 0.063(2) Uani 1 1 d . . . C8 C 0.3025(10) 0.1353(6) -0.1146(7) 0.061(2) Uani 1 1 d . . . C9 C 0.4321(10) 0.1007(6) -0.0795(8) 0.067(2) Uani 1 1 d . . . C10 C 0.4598(9) 0.0875(6) 0.0306(8) 0.061(2) Uani 1 1 d . . . C11 C 0.7241(6) 0.2382(5) 0.1575(6) 0.0488(15) Uani 1 1 d . . . C12 C 0.7851(9) 0.2297(6) 0.2641(7) 0.065(2) Uani 1 1 d . . . C13 C 0.8957(10) 0.1674(8) 0.2949(9) 0.078(3) Uani 1 1 d . . . C14 C 0.9450(10) 0.1154(7) 0.2244(11) 0.084(3) Uani 1 1 d . . . C15 C 0.8834(9) 0.1257(7) 0.1152(10) 0.073(3) Uani 1 1 d . . . C16 C 0.7749(9) 0.1869(7) 0.0830(8) 0.066(2) Uani 1 1 d . . . C17 C 0.1400(7) 0.3885(5) 0.0154(6) 0.0495(16) Uani 1 1 d . . . C18 C 0.0769(8) 0.4188(7) 0.0974(8) 0.064(2) Uani 1 1 d . . . C19 C -0.0645(10) 0.4258(8) 0.0744(10) 0.079(3) Uani 1 1 d . . . C20 C -0.1345(10) 0.4055(9) -0.0232(11) 0.086(3) Uani 1 1 d . . . C21 C -0.0749(10) 0.3752(9) -0.1025(10) 0.083(3) Uani 1 1 d . . . C22 C 0.0656(9) 0.3674(6) -0.0847(7) 0.062(2) Uani 1 1 d . . . C23 C 0.3702(9) 0.3238(7) -0.2601(6) 0.059(2) Uani 1 1 d . . . C24 C 0.3676(10) 0.2454(8) -0.3324(7) 0.073(2) Uani 1 1 d . . . C25 C 0.2572(14) 0.2426(10) -0.4252(7) 0.097(4) Uani 1 1 d . . . C26 C 0.1659(12) 0.3186(12) -0.4420(8) 0.096(4) Uani 1 1 d . . . C27 C 0.1766(13) 0.3929(13) -0.3735(10) 0.102(4) Uani 1 1 d . . . C28 C 0.2731(11) 0.3983(10) -0.2821(7) 0.081(3) Uani 1 1 d . . . C29 C 0.5700(9) 0.4478(6) 0.4048(7) 0.062(2) Uani 1 1 d . . . C30 C 0.5416(12) 0.4354(8) 0.5045(8) 0.076(3) Uani 1 1 d . . . C31 C 0.638(2) 0.4363(10) 0.5941(9) 0.115(5) Uani 1 1 d . . . C32 C 0.7713(16) 0.4444(12) 0.5900(11) 0.117(6) Uani 1 1 d . . . C33 C 0.7971(13) 0.4583(14) 0.4977(16) 0.130(6) Uani 1 1 d . . . C34 C 0.6988(12) 0.4601(9) 0.3973(10) 0.093(3) Uani 1 1 d . . . C35 C 0.8076(17) 0.1066(11) 0.6532(11) 0.109(4) Uani 1 1 d . . . H2 H 0.1624 0.2342 0.1596 0.078 Uiso 1 1 d R . . H3 H 0.2551 0.2997 0.3414 0.077 Uiso 1 1 d R . . H4 H 0.4782 0.2516 0.4048 0.088 Uiso 1 1 d R . . H5 H 0.5454 0.1344 0.2620 0.076 Uiso 1 1 d R . . H7 H 0.1692 0.1826 -0.0184 0.076 Uiso 1 1 d R . . H8 H 0.2700 0.1620 -0.1850 0.074 Uiso 1 1 d R . . H9 H 0.5076 0.1029 -0.1134 0.080 Uiso 1 1 d R . . H10 H 0.5523 0.0852 0.0837 0.073 Uiso 1 1 d R . . H12 H 0.7458 0.2666 0.3134 0.078 Uiso 1 1 d R . . H13 H 0.9431 0.1574 0.3768 0.093 Uiso 1 1 d R . . H14 H 1.0261 0.0762 0.2402 0.101 Uiso 1 1 d R . . H15 H 0.9107 0.0915 0.0578 0.087 Uiso 1 1 d R . . H16 H 0.7405 0.1990 0.0065 0.079 Uiso 1 1 d R . . H18 H 0.1245 0.4363 0.1683 0.076 Uiso 1 1 d R . . H19 H -0.0924 0.4588 0.1231 0.095 Uiso 1 1 d R . . H20 H -0.2483 0.4049 -0.0279 0.103 Uiso 1 1 d R . . H21 H -0.1237 0.3671 -0.1748 0.099 Uiso 1 1 d R . . H22 H 0.1022 0.3443 -0.1431 0.075 Uiso 1 1 d R . . H24 H 0.4399 0.1953 -0.3132 0.087 Uiso 1 1 d R . . H25 H 0.2565 0.1990 -0.4558 0.116 Uiso 1 1 d R . . H26 H 0.1089 0.2864 -0.5150 0.115 Uiso 1 1 d R . . H28 H 0.3186 0.4726 -0.2314 0.097 Uiso 1 1 d R . . H30 H 0.4613 0.4220 0.5033 0.091 Uiso 1 1 d R . . H31 H 0.6224 0.4266 0.6646 0.138 Uiso 1 1 d R . . H34 H 0.7262 0.4797 0.3460 0.111 Uiso 1 1 d 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 0.0340(3) 0.0535(3) 0.0458(3) 0.0049(2) 0.00679(19) -0.0018(2) Ru2 0.0356(3) 0.0453(3) 0.0481(3) 0.0006(2) 0.0062(2) -0.0018(2) Cl1 0.143(6) 0.226(10) 0.147(6) 0.103(7) 0.002(5) 0.018(6) Cl2 0.64(3) 0.133(6) 0.198(9) -0.093(7) 0.224(14) -0.157(11) Cl3 0.062(4) 0.61(3) 0.302(13) 0.257(18) 0.031(6) 0.030(9) S1 0.0310(7) 0.0516(9) 0.0526(8) 0.0042(7) 0.0068(6) -0.0014(7) S2 0.0338(8) 0.0477(9) 0.0505(9) 0.0023(7) 0.0031(6) -0.0012(7) S3 0.0466(10) 0.0762(14) 0.0562(10) 0.0031(9) 0.0111(8) -0.0091(9) S4 0.0534(12) 0.0651(12) 0.0536(11) -0.0058(9) 0.0041(8) 0.0079(9) C1 0.060(5) 0.063(5) 0.060(5) 0.021(4) 0.002(4) -0.019(4) C2 0.050(4) 0.075(5) 0.072(5) 0.022(4) 0.018(4) -0.011(4) C3 0.064(5) 0.066(4) 0.069(5) 0.003(4) 0.026(4) -0.007(5) C4 0.078(6) 0.082(6) 0.060(5) 0.025(4) 0.012(4) -0.014(5) C5 0.057(5) 0.066(5) 0.065(5) 0.024(4) 0.011(4) -0.010(4) C6 0.046(4) 0.047(4) 0.068(5) 0.005(3) 0.013(3) -0.013(3) C7 0.059(5) 0.049(4) 0.073(5) 0.005(4) -0.003(4) -0.017(4) C8 0.068(6) 0.054(4) 0.056(4) -0.005(3) -0.001(4) -0.004(4) C9 0.063(6) 0.048(4) 0.090(6) -0.011(4) 0.016(5) -0.004(4) C10 0.054(5) 0.043(4) 0.085(6) -0.001(4) 0.016(4) -0.003(3) C11 0.032(3) 0.043(4) 0.069(4) 0.003(3) 0.008(3) -0.001(3) C12 0.054(5) 0.062(5) 0.074(5) 0.015(4) 0.000(4) 0.004(4) C13 0.048(5) 0.082(7) 0.093(7) 0.020(5) -0.007(5) 0.000(5) C14 0.041(5) 0.063(6) 0.146(10) 0.019(6) 0.014(6) 0.005(4) C15 0.041(5) 0.058(5) 0.119(8) -0.005(5) 0.017(5) 0.002(4) C16 0.048(5) 0.060(5) 0.090(6) -0.005(4) 0.016(4) 0.001(4) C17 0.035(3) 0.044(3) 0.068(4) 0.002(3) 0.006(3) 0.000(3) C18 0.041(4) 0.068(5) 0.084(6) -0.005(4) 0.018(4) 0.008(4) C19 0.050(5) 0.069(6) 0.127(9) 0.002(6) 0.039(6) 0.007(4) C20 0.043(5) 0.081(6) 0.121(9) 0.032(6) -0.012(6) -0.006(5) C21 0.054(6) 0.085(7) 0.094(7) 0.015(6) -0.019(5) -0.004(5) C22 0.055(5) 0.064(5) 0.062(5) 0.003(4) -0.001(4) -0.003(4) C23 0.057(5) 0.074(5) 0.047(4) -0.004(3) 0.013(3) -0.011(4) C24 0.084(6) 0.072(5) 0.063(5) 0.000(5) 0.019(4) -0.004(5) C25 0.151(11) 0.090(7) 0.050(4) -0.016(5) 0.022(6) -0.049(8) C26 0.093(8) 0.120(10) 0.064(6) 0.000(7) -0.007(5) -0.005(8) C27 0.077(8) 0.134(11) 0.086(7) -0.004(8) -0.004(6) 0.019(8) C28 0.076(7) 0.103(8) 0.058(5) 0.003(5) 0.002(4) 0.011(6) C29 0.058(5) 0.058(4) 0.068(5) -0.006(4) 0.006(4) -0.004(4) C30 0.086(7) 0.078(6) 0.059(5) -0.008(4) 0.005(5) -0.009(6) C31 0.194(18) 0.086(8) 0.057(6) 0.003(5) 0.009(8) -0.017(10) C32 0.115(12) 0.124(11) 0.084(8) 0.024(8) -0.039(8) -0.052(9) C33 0.059(7) 0.141(13) 0.165(15) 0.047(11) -0.031(8) -0.019(8) C34 0.075(7) 0.088(7) 0.101(8) 0.015(6) -0.011(6) -0.016(6) C35 0.124(11) 0.104(9) 0.103(9) 0.001(7) 0.031(8) -0.049(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 C1 2.195(9) . ? Ru1 C2 2.203(8) . ? Ru1 C3 2.216(8) . ? Ru1 C4 2.216(8) . ? Ru1 C5 2.232(9) . ? Ru1 S1 2.3550(18) . ? Ru1 S2 2.3614(18) . ? Ru1 S4 2.391(2) . ? Ru1 Ru2 2.6674(8) . ? Ru2 C6 2.191(7) . ? Ru2 C7 2.205(8) . ? Ru2 C8 2.230(8) . ? Ru2 C9 2.233(8) . ? Ru2 C10 2.245(8) . ? Ru2 S2 2.3503(19) . ? Ru2 S1 2.3579(17) . ? Ru2 S3 2.401(2) . ? Cl1 C35 1.657(16) . ? Cl2 C35 1.647(17) . ? Cl3 C35 1.607(18) . ? S1 C11 1.785(7) . ? S2 C17 1.773(7) . ? S3 C23 1.766(8) . ? S4 C29 1.790(9) . ? C1 C2 1.428(14) . ? C1 C6 1.445(13) . ? C1 C5 1.467(13) . ? C2 C3 1.422(13) . ? C3 C4 1.401(14) . ? C4 C5 1.412(15) . ? C6 C7 1.439(12) . ? C6 C10 1.441(12) . ? C7 C8 1.413(14) . ? C8 C9 1.395(13) . ? C9 C10 1.388(13) . ? C11 C16 1.370(12) . ? C11 C12 1.380(11) . ? C12 C13 1.401(13) . ? C13 C14 1.326(16) . ? C14 C15 1.413(17) . ? C15 C16 1.378(13) . ? C17 C22 1.374(11) . ? C17 C18 1.411(12) . ? C18 C19 1.427(13) . ? C19 C20 1.330(17) . ? C20 C21 1.360(18) . ? C21 C22 1.421(14) . ? C23 C24 1.399(13) . ? C23 C28 1.402(15) . ? C24 C25 1.458(14) . ? C25 C26 1.374(19) . ? C26 C27 1.32(2) . ? C27 C28 1.365(15) . ? C29 C34 1.363(15) . ? C29 C30 1.382(13) . ? C30 C31 1.347(17) . ? C31 C32 1.39(2) . ? C32 C33 1.28(2) . ? C33 C34 1.456(18) . ? 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 C1 Ru1 C2 37.9(4) . . ? C1 Ru1 C3 63.4(4) . . ? C2 Ru1 C3 37.5(3) . . ? C1 Ru1 C4 63.1(3) . . ? C2 Ru1 C4 62.1(3) . . ? C3 Ru1 C4 36.9(4) . . ? C1 Ru1 C5 38.7(3) . . ? C2 Ru1 C5 63.1(3) . . ? C3 Ru1 C5 62.5(4) . . ? C4 Ru1 C5 37.0(4) . . ? C1 Ru1 S1 110.9(3) . . ? C2 Ru1 S1 146.4(3) . . ? C3 Ru1 S1 160.2(2) . . ? C4 Ru1 S1 123.4(3) . . ? C5 Ru1 S1 100.7(3) . . ? C1 Ru1 S2 110.1(2) . . ? C2 Ru1 S2 99.5(2) . . ? C3 Ru1 S2 121.7(2) . . ? C4 Ru1 S2 158.5(3) . . ? C5 Ru1 S2 146.7(3) . . ? S1 Ru1 S2 78.04(6) . . ? C1 Ru1 S4 152.4(3) . . ? C2 Ru1 S4 119.7(3) . . ? C3 Ru1 S4 89.2(3) . . ? C4 Ru1 S4 93.3(3) . . ? C5 Ru1 S4 126.7(3) . . ? S1 Ru1 S4 93.79(7) . . ? S2 Ru1 S4 86.41(7) . . ? C1 Ru1 Ru2 73.7(2) . . ? C2 Ru1 Ru2 95.1(2) . . ? C3 Ru1 Ru2 132.3(2) . . ? C4 Ru1 Ru2 132.6(3) . . ? C5 Ru1 Ru2 96.1(3) . . ? S1 Ru1 Ru2 55.58(4) . . ? S2 Ru1 Ru2 55.32(5) . . ? S4 Ru1 Ru2 132.94(6) . . ? C6 Ru2 C7 38.2(3) . . ? C6 Ru2 C8 63.1(3) . . ? C7 Ru2 C8 37.2(4) . . ? C6 Ru2 C9 62.3(3) . . ? C7 Ru2 C9 61.4(4) . . ? C8 Ru2 C9 36.4(3) . . ? C6 Ru2 C10 37.9(3) . . ? C7 Ru2 C10 62.1(3) . . ? C8 Ru2 C10 61.2(3) . . ? C9 Ru2 C10 36.1(3) . . ? C6 Ru2 S2 110.8(2) . . ? C7 Ru2 S2 100.0(3) . . ? C8 Ru2 S2 122.0(2) . . ? C9 Ru2 S2 158.4(2) . . ? C10 Ru2 S2 147.0(2) . . ? C6 Ru2 S1 110.8(2) . . ? C7 Ru2 S1 146.7(2) . . ? C8 Ru2 S1 159.7(2) . . ? C9 Ru2 S1 123.3(3) . . ? C10 Ru2 S1 101.5(2) . . ? S2 Ru2 S1 78.21(6) . . ? C6 Ru2 S3 152.9(2) . . ? C7 Ru2 S3 127.2(2) . . ? C8 Ru2 S3 93.7(2) . . ? C9 Ru2 S3 90.7(3) . . ? C10 Ru2 S3 119.9(2) . . ? S2 Ru2 S3 93.05(7) . . ? S1 Ru2 S3 85.96(7) . . ? C6 Ru2 Ru1 74.0(2) . . ? C7 Ru2 Ru1 95.7(2) . . ? C8 Ru2 Ru1 132.4(3) . . ? C9 Ru2 Ru1 132.2(3) . . ? C10 Ru2 Ru1 96.5(2) . . ? S2 Ru2 Ru1 55.72(4) . . ? S1 Ru2 Ru1 55.48(4) . . ? S3 Ru2 Ru1 132.36(6) . . ? C11 S1 Ru1 113.3(2) . . ? C11 S1 Ru2 109.8(2) . . ? Ru1 S1 Ru2 68.94(5) . . ? C17 S2 Ru2 113.6(2) . . ? C17 S2 Ru1 110.5(3) . . ? Ru2 S2 Ru1 68.96(5) . . ? C23 S3 Ru2 106.3(3) . . ? C29 S4 Ru1 109.7(3) . . ? C2 C1 C6 125.3(8) . . ? C2 C1 C5 106.7(8) . . ? C6 C1 C5 125.0(9) . . ? C2 C1 Ru1 71.4(5) . . ? C6 C1 Ru1 106.3(5) . . ? C5 C1 Ru1 72.0(5) . . ? C1 C2 C3 108.8(8) . . ? C1 C2 Ru1 70.7(5) . . ? C3 C2 Ru1 71.7(5) . . ? C4 C3 C2 107.7(9) . . ? C4 C3 Ru1 71.6(5) . . ? C2 C3 Ru1 70.8(4) . . ? C5 C4 C3 110.2(9) . . ? C5 C4 Ru1 72.1(5) . . ? C3 C4 Ru1 71.6(5) . . ? C4 C5 C1 106.6(9) . . ? C4 C5 Ru1 70.9(5) . . ? C1 C5 Ru1 69.3(5) . . ? C7 C6 C10 105.8(8) . . ? C7 C6 C1 124.3(8) . . ? C10 C6 C1 127.3(8) . . ? C7 C6 Ru2 71.4(4) . . ? C10 C6 Ru2 73.1(4) . . ? C1 C6 Ru2 106.1(5) . . ? C8 C7 C6 108.4(8) . . ? C8 C7 Ru2 72.4(5) . . ? C6 C7 Ru2 70.4(4) . . ? C9 C8 C7 107.6(8) . . ? C9 C8 Ru2 71.9(5) . . ? C7 C8 Ru2 70.5(4) . . ? C8 C9 C10 110.0(8) . . ? C8 C9 Ru2 71.6(5) . . ? C10 C9 Ru2 72.4(5) . . ? C9 C10 C6 108.1(8) . . ? C9 C10 Ru2 71.5(5) . . ? C6 C10 Ru2 69.0(4) . . ? C12 C11 C16 119.1(8) . . ? C12 C11 S1 120.9(6) . . ? C16 C11 S1 119.5(6) . . ? C11 C12 C13 119.8(10) . . ? C14 C13 C12 122.1(10) . . ? C13 C14 C15 117.8(9) . . ? C16 C15 C14 121.1(10) . . ? C15 C16 C11 120.0(10) . . ? C22 C17 C18 120.0(8) . . ? C22 C17 S2 121.4(6) . . ? C18 C17 S2 118.0(6) . . ? C17 C18 C19 118.7(9) . . ? C20 C19 C18 120.2(10) . . ? C21 C20 C19 121.5(10) . . ? C20 C21 C22 120.8(9) . . ? C17 C22 C21 118.6(9) . . ? C28 C23 C24 119.6(8) . . ? C28 C23 S3 120.8(7) . . ? C24 C23 S3 119.6(8) . . ? C23 C24 C25 117.3(10) . . ? C26 C25 C24 119.8(10) . . ? C27 C26 C25 120.2(10) . . ? C26 C27 C28 123.5(13) . . ? C27 C28 C23 119.4(11) . . ? C34 C29 C30 119.0(10) . . ? C34 C29 S4 118.8(8) . . ? C30 C29 S4 122.0(8) . . ? C31 C30 C29 121.5(12) . . ? C30 C31 C32 121.4(12) . . ? C33 C32 C31 116.8(11) . . ? C32 C33 C34 125.1(14) . . ? C29 C34 C33 116.1(13) . . ? Cl3 C35 Cl1 111.6(9) . . ? Cl3 C35 Cl2 103.7(13) . . ? Cl1 C35 Cl2 110.0(12) . . ? _diffrn_measured_fraction_theta_max 0.941 _diffrn_measured_fraction_theta_full 0.941 _refine_diff_density_max 0.741 _refine_diff_density_min -0.917 _refine_diff_density_rms 0.103 #========= data_compound_4c _database_code_CSD 191662 _exptl_crystal_description Needle _exptl_crystal_colour Red _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.04 _cell_measurement_temperature 298 _refine_ls_hydrogen_treatment refxyz _diffrn_measurement_device KappaCCD _computing_data_collection KappaCCD _computing_data_reduction 'Denzo and Scalepak (Otwinowski & Minor, 1997)' _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 26 loop_ _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_wavelength_id all _diffrn_orient_matrix_type X=UH _diffrn_orient_matrix_UB_11 0.05419 _diffrn_orient_matrix_UB_12 0.05688 _diffrn_orient_matrix_UB_13 0.04821 _diffrn_orient_matrix_UB_21 -0.13368 _diffrn_orient_matrix_UB_22 0.00842 _diffrn_orient_matrix_UB_23 0.00903 _diffrn_orient_matrix_UB_31 -0.00775 _diffrn_orient_matrix_UB_32 -0.05714 _diffrn_orient_matrix_UB_33 0.02527 _cell_formula_units_Z 2 _exptl_crystal_density_diffrn 1.772 _exptl_crystal_density_method 'not measured' _exptl_special_details ; ? ; _chemical_formula_weight 904.75 _diffrn_radiation_type ' MoK¥a' loop_ _symmetry_equiv_pos_as_xyz +X,+Y,+Z -X,-Y,-Z _symmetry_space_group_name_H-M 'P -1 ' _symmetry_cell_setting Triclinic _chemical_formula_moiety 'C34 H24 Cl4 Ru2 S4 ' _chemical_formula_sum 'C34 H24 Cl4 Ru2 S4 ' _chemical_name_systematic ; ? ; _cell_length_a 7.1130(4) _cell_length_b 13.2430(10) _cell_length_c 19.248(2) _cell_angle_alpha 106.481(4) _cell_angle_beta 95.341(6) _cell_angle_gamma 99.585(4) _cell_volume 1695.4(3) _diffrn_reflns_number 8318 _diffrn_reflns_theta_max 30.33 _computing_structure_solution 'DIRDIF (Buerskens et al., 1992)' _atom_sites_solution_primary vecmap _atom_sites_solution_secondary difmap _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? 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' Ru Ru -1.2594 0.8363 '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' _exptl_absorpt_coefficient_mu 1.478 _reflns_number_total 7631 _reflns_number_gt 7176 _reflns_threshold_expression >2sigma(I) _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even largeR . ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[¥s^2^(Fo^2^)+(0.0177P)^2^+7.7758P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7631 _refine_ls_number_parameters 397 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0615 _refine_ls_R_factor_gt 0.0570 _refine_ls_wR_factor_ref 0.1181 _refine_ls_wR_factor_gt 0.1158 _refine_ls_goodness_of_fit_ref 1.199 _refine_ls_restrained_S_all 1.199 _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 0.82429(6) 0.33888(3) 0.24899(2) 0.04035(11) Uani 1 1 d . . . Ru2 Ru 0.74492(6) 0.14243(3) 0.15264(2) 0.03721(11) Uani 1 1 d . . . Cl1 Cl 0.8411(6) 0.2542(2) 0.61244(14) 0.1416(13) Uani 1 1 d . . . Cl2 Cl 0.1555(4) 0.0383(3) 0.45175(17) 0.1267(12) Uani 1 1 d . . . Cl3 Cl 0.1614(4) 0.4173(2) -0.06957(14) 0.1072(9) Uani 1 1 d . . . Cl4 Cl 0.6046(5) -0.3437(2) 0.29480(15) 0.1085(9) Uani 1 1 d . . . S1 S 0.6746(3) 0.42791(14) 0.34672(9) 0.0577(4) Uani 1 1 d . . . S2 S 0.80236(18) 0.17908(10) 0.27999(6) 0.0370(3) Uani 1 1 d . . . S3 S 0.52614(19) 0.25682(11) 0.17640(7) 0.0403(3) Uani 1 1 d . . . S4 S 0.4866(2) -0.00386(12) 0.13322(8) 0.0508(4) Uani 1 1 d . . . C1 C 1.0544(8) 0.3322(5) 0.1800(3) 0.0478(13) Uani 1 1 d . . . C2 C 0.9543(10) 0.4176(5) 0.1733(4) 0.0593(17) Uani 1 1 d . . . C3 C 0.9819(10) 0.4939(6) 0.2416(5) 0.0666(19) Uani 1 1 d . . . C4 C 1.1009(10) 0.4618(5) 0.2929(4) 0.0649(18) Uani 1 1 d . . . C5 C 1.1442(8) 0.3635(5) 0.2547(4) 0.0526(14) Uani 1 1 d . . . C6 C 1.0126(8) 0.2259(5) 0.1281(3) 0.0504(14) Uani 1 1 d . . . C7 C 0.8713(9) 0.1911(6) 0.0630(3) 0.0545(15) Uani 1 1 d . . . C8 C 0.8224(9) 0.0792(6) 0.0408(3) 0.0568(16) Uani 1 1 d . . . C9 C 0.9321(9) 0.0408(5) 0.0906(3) 0.0545(15) Uani 1 1 d . . . C10 C 1.0491(9) 0.1308(5) 0.1437(3) 0.0495(13) Uani 1 1 d . . . C11 C 0.7373(10) 0.3872(5) 0.4237(3) 0.0541(15) Uani 1 1 d . . . C12 C 0.5964(13) 0.3745(6) 0.4681(4) 0.073(2) Uani 1 1 d . . . C13 C 0.6324(16) 0.3359(7) 0.5275(4) 0.088(3) Uani 1 1 d . . . C14 C 0.8062(17) 0.3106(6) 0.5415(4) 0.088(3) Uani 1 1 d . . . C15 C 0.9526(14) 0.3270(6) 0.5016(4) 0.081(2) Uani 1 1 d . . . C16 C 0.9165(11) 0.3656(5) 0.4428(4) 0.0660(18) Uani 1 1 d . . . C17 C 0.6076(8) 0.1381(4) 0.3238(3) 0.0386(11) Uani 1 1 d . . . C18 C 0.4241(8) 0.1575(5) 0.3135(3) 0.0508(14) Uani 1 1 d . . . C19 C 0.2839(9) 0.1256(6) 0.3516(4) 0.0599(17) Uani 1 1 d . . . C20 C 0.3296(10) 0.0733(6) 0.4006(4) 0.0658(19) Uani 1 1 d . . . C21 C 0.5073(11) 0.0496(7) 0.4107(4) 0.077(2) Uani 1 1 d . . . C22 C 0.6492(10) 0.0823(6) 0.3723(3) 0.0570(16) Uani 1 1 d . . . C23 C 0.4627(7) 0.3090(5) 0.1037(3) 0.0420(12) Uani 1 1 d . . . C24 C 0.4092(9) 0.2414(5) 0.0325(3) 0.0527(14) Uani 1 1 d . . . C25 C 0.3203(10) 0.2761(6) -0.0212(4) 0.0621(17) Uani 1 1 d . . . C26 C 0.2860(10) 0.3773(6) -0.0031(4) 0.0638(18) Uani 1 1 d . . . C27 C 0.3447(10) 0.4480(6) 0.0663(4) 0.0632(18) Uani 1 1 d . . . C28 C 0.4342(9) 0.4131(5) 0.1198(3) 0.0524(14) Uani 1 1 d . . . C29 C 0.5357(10) -0.0947(5) 0.1803(3) 0.0518(14) Uani 1 1 d . . . C30 C 0.7158(10) -0.0968(5) 0.2134(3) 0.0565(15) Uani 1 1 d . . . C31 C 0.7384(12) -0.1735(6) 0.2491(4) 0.0665(19) Uani 1 1 d . . . C32 C 0.5789(14) -0.2478(6) 0.2503(4) 0.076(2) Uani 1 1 d . . . C33 C 0.4005(14) -0.2473(7) 0.2178(5) 0.089(3) Uani 1 1 d . . . C34 C 0.3778(12) -0.1721(6) 0.1825(5) 0.075(2) Uani 1 1 d . . . H2 H 0.8562 0.4105 0.1331 0.071 Uiso 1 1 d R . . H3 H 0.9405 0.5756 0.2574 0.080 Uiso 1 1 d R . . H4 H 1.1103 0.4875 0.3453 0.078 Uiso 1 1 d R . . H5 H 1.1895 0.3147 0.2775 0.063 Uiso 1 1 d R . . H7 H 0.7956 0.2363 0.0469 0.065 Uiso 1 1 d R . . H8 H 0.7083 0.0379 0.0077 0.068 Uiso 1 1 d R . . H9 H 0.9334 -0.0352 0.0868 0.065 Uiso 1 1 d R . . H10 H 1.1115 0.1305 0.1900 0.059 Uiso 1 1 d R . . H12 H 0.4731 0.3922 0.4574 0.087 Uiso 1 1 d R . . H13 H 0.5390 0.3261 0.5592 0.105 Uiso 1 1 d R . . H15 H 1.0748 0.3113 0.5155 0.097 Uiso 1 1 d R . . H16 H 1.0165 0.3780 0.4144 0.079 Uiso 1 1 d R . . H18 H 0.3941 0.1952 0.2794 0.061 Uiso 1 1 d R . . H19 H 0.1554 0.1384 0.3454 0.072 Uiso 1 1 d R . . H21 H 0.5359 0.0119 0.4451 0.092 Uiso 1 1 d R . . H22 H 0.7761 0.0669 0.3783 0.068 Uiso 1 1 d R . . H24 H 0.4398 0.1709 0.0214 0.063 Uiso 1 1 d R . . H25 H 0.2791 0.2276 -0.0700 0.075 Uiso 1 1 d R . . H27 H 0.3150 0.5182 0.0727 0.076 Uiso 1 1 d R . . H28 H 0.4729 0.4578 0.1696 0.063 Uiso 1 1 d R . . H30 H 0.8266 -0.0453 0.2118 0.068 Uiso 1 1 d R . . H31 H 0.8620 -0.1766 0.2729 0.080 Uiso 1 1 d R . . H33 H 0.2923 -0.2995 0.2194 0.107 Uiso 1 1 d R . . H34 H 0.2531 -0.1722 0.1592 0.090 Uiso 1 1 d 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 0.0307(2) 0.0459(2) 0.0499(2) 0.02194(18) 0.00784(17) 0.00877(17) Ru2 0.0285(2) 0.0528(2) 0.03600(19) 0.02000(17) 0.00760(15) 0.01092(17) Cl1 0.242(4) 0.113(2) 0.0758(15) 0.0391(15) -0.0089(19) 0.053(2) Cl2 0.0813(17) 0.218(3) 0.166(2) 0.154(3) 0.0754(17) 0.0651(19) Cl3 0.1008(18) 0.146(2) 0.1112(17) 0.0921(17) -0.0003(14) 0.0399(15) Cl4 0.148(2) 0.0875(15) 0.125(2) 0.0671(15) 0.0406(17) 0.0486(15) S1 0.0611(11) 0.0620(9) 0.0579(9) 0.0204(7) 0.0138(7) 0.0275(8) S2 0.0310(7) 0.0469(6) 0.0373(6) 0.0187(5) 0.0045(5) 0.0097(5) S3 0.0286(7) 0.0571(7) 0.0453(6) 0.0279(6) 0.0102(5) 0.0124(5) S4 0.0424(8) 0.0576(8) 0.0509(7) 0.0218(6) -0.0032(6) 0.0026(6) C1 0.021(3) 0.063(3) 0.071(4) 0.034(3) 0.020(2) 0.010(2) C2 0.045(4) 0.065(4) 0.082(5) 0.043(4) 0.019(3) 0.007(3) C3 0.047(4) 0.058(4) 0.106(6) 0.044(4) 0.022(4) 0.003(3) C4 0.046(4) 0.060(4) 0.084(5) 0.023(3) 0.008(3) -0.003(3) C5 0.024(3) 0.062(4) 0.074(4) 0.027(3) 0.011(3) 0.005(2) C6 0.028(3) 0.080(4) 0.058(3) 0.037(3) 0.022(2) 0.014(3) C7 0.035(3) 0.093(5) 0.051(3) 0.039(3) 0.016(2) 0.021(3) C8 0.038(4) 0.092(5) 0.042(3) 0.017(3) 0.015(2) 0.017(3) C9 0.049(4) 0.068(4) 0.051(3) 0.016(3) 0.021(3) 0.021(3) C10 0.035(3) 0.071(4) 0.050(3) 0.023(3) 0.016(2) 0.018(3) C11 0.059(4) 0.053(3) 0.047(3) 0.008(2) 0.004(3) 0.017(3) C12 0.093(6) 0.069(4) 0.056(4) 0.012(3) 0.013(4) 0.027(4) C13 0.129(9) 0.084(6) 0.052(4) 0.020(4) 0.024(5) 0.026(5) C14 0.144(9) 0.067(5) 0.047(4) 0.009(3) -0.009(5) 0.030(5) C15 0.094(7) 0.076(5) 0.062(4) 0.008(4) -0.015(4) 0.024(4) C16 0.073(5) 0.059(4) 0.058(4) 0.011(3) -0.007(3) 0.012(3) C17 0.034(3) 0.051(3) 0.035(2) 0.020(2) 0.0076(19) 0.009(2) C18 0.038(3) 0.076(4) 0.051(3) 0.037(3) 0.008(2) 0.015(3) C19 0.036(4) 0.096(5) 0.068(4) 0.050(4) 0.016(3) 0.020(3) C20 0.048(4) 0.101(5) 0.073(4) 0.057(4) 0.026(3) 0.020(4) C21 0.065(5) 0.124(7) 0.088(5) 0.082(5) 0.036(4) 0.044(5) C22 0.047(4) 0.085(4) 0.063(4) 0.046(3) 0.019(3) 0.030(3) C23 0.028(3) 0.059(3) 0.049(3) 0.030(2) 0.011(2) 0.011(2) C24 0.048(4) 0.065(4) 0.052(3) 0.024(3) 0.006(3) 0.019(3) C25 0.060(4) 0.083(5) 0.051(3) 0.031(3) 0.002(3) 0.019(3) C26 0.056(4) 0.088(5) 0.066(4) 0.051(4) 0.009(3) 0.018(3) C27 0.057(4) 0.065(4) 0.088(5) 0.048(4) 0.017(4) 0.020(3) C28 0.046(4) 0.058(3) 0.059(3) 0.027(3) 0.010(3) 0.012(3) C29 0.059(4) 0.051(3) 0.043(3) 0.012(2) 0.007(3) 0.009(3) C30 0.064(4) 0.052(3) 0.054(3) 0.019(3) 0.004(3) 0.011(3) C31 0.084(6) 0.063(4) 0.056(4) 0.019(3) 0.007(3) 0.027(4) C32 0.103(7) 0.069(5) 0.075(5) 0.038(4) 0.028(4) 0.036(4) C33 0.085(7) 0.078(5) 0.123(7) 0.057(5) 0.025(5) 0.012(4) C34 0.061(5) 0.074(5) 0.099(6) 0.043(4) 0.013(4) 0.006(4) _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 C1 2.199(6) . ? Ru1 C2 2.204(6) . ? Ru1 C3 2.219(6) . ? Ru1 C5 2.232(6) . ? Ru1 C4 2.254(6) . ? Ru1 S3 2.3345(14) . ? Ru1 S2 2.3415(13) . ? Ru1 S1 2.3653(17) . ? Ru1 Ru2 2.6655(7) . ? Ru2 C6 2.198(5) . ? Ru2 C10 2.213(6) . ? Ru2 C7 2.219(5) . ? Ru2 C9 2.234(6) . ? Ru2 C8 2.234(6) . ? Ru2 S3 2.3346(15) . ? Ru2 S2 2.3418(12) . ? Ru2 S4 2.3548(15) . ? Cl1 C14 1.749(8) . ? Cl2 C20 1.736(6) . ? Cl3 C26 1.741(6) . ? Cl4 C32 1.745(7) . ? S1 C11 1.760(6) . ? S2 C17 1.775(5) . ? S3 C23 1.782(5) . ? S4 C29 1.758(6) . ? C1 C5 1.432(8) . ? C1 C6 1.440(9) . ? C1 C2 1.462(9) . ? C2 C3 1.386(10) . ? C3 C4 1.441(10) . ? C4 C5 1.401(9) . ? C6 C10 1.432(8) . ? C6 C7 1.442(8) . ? C7 C8 1.393(9) . ? C8 C9 1.433(9) . ? C9 C10 1.407(9) . ? C11 C16 1.392(9) . ? C11 C12 1.395(10) . ? C12 C13 1.398(10) . ? C13 C14 1.357(13) . ? C14 C15 1.376(13) . ? C15 C16 1.387(10) . ? C17 C18 1.378(8) . ? C17 C22 1.384(7) . ? C18 C19 1.372(8) . ? C19 C20 1.365(8) . ? C20 C21 1.362(10) . ? C21 C22 1.389(9) . ? C23 C28 1.378(8) . ? C23 C24 1.385(8) . ? C24 C25 1.388(8) . ? C25 C26 1.355(10) . ? C26 C27 1.375(10) . ? C27 C28 1.388(8) . ? C29 C30 1.385(9) . ? C29 C34 1.402(9) . ? C30 C31 1.401(9) . ? C31 C32 1.379(11) . ? C32 C33 1.364(12) . ? C33 C34 1.377(10) . ? C2 H2 0.9647 . ? C3 H3 1.1335 . ? C4 H4 0.9607 . ? C5 H5 0.9584 . ? C7 H7 0.9630 . ? C8 H8 0.9604 . ? C9 H9 0.9903 . ? C10 H10 0.9596 . ? C12 H12 0.9638 . ? C13 H13 0.9611 . ? C15 H15 0.9585 . ? C16 H16 0.9568 . ? C18 H18 0.9604 . ? C19 H19 0.9597 . ? C21 H21 0.9609 . ? C22 H22 0.9621 . ? C24 H24 0.9629 . ? C25 H25 0.9604 . ? C27 H27 0.9641 . ? C28 H28 0.9594 . ? C30 H30 0.9621 . ? C31 H31 0.9656 . ? C33 H33 0.9541 . ? C34 H34 0.9555 . ? 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 C1 Ru1 C2 38.8(2) . . ? C1 Ru1 C3 62.8(3) . . ? C2 Ru1 C3 36.5(3) . . ? C1 Ru1 C5 37.7(2) . . ? C2 Ru1 C5 62.9(2) . . ? C3 Ru1 C5 61.9(3) . . ? C1 Ru1 C4 62.5(3) . . ? C2 Ru1 C4 62.3(3) . . ? C3 Ru1 C4 37.6(3) . . ? C5 Ru1 C4 36.4(2) . . ? C1 Ru1 S3 109.90(17) . . ? C2 Ru1 S3 98.11(19) . . ? C3 Ru1 S3 120.1(2) . . ? C5 Ru1 S3 146.12(17) . . ? C4 Ru1 S3 157.57(19) . . ? C1 Ru1 S2 103.22(16) . . ? C2 Ru1 S2 140.64(19) . . ? C3 Ru1 S2 153.62(19) . . ? C5 Ru1 S2 93.11(17) . . ? C4 Ru1 S2 116.77(19) . . ? S3 Ru1 S2 85.13(4) . . ? C1 Ru1 S1 152.38(17) . . ? C2 Ru1 S1 123.40(19) . . ? C3 Ru1 S1 91.7(2) . . ? C5 Ru1 S1 122.27(18) . . ? C4 Ru1 S1 91.0(2) . . ? S3 Ru1 S1 91.54(6) . . ? S2 Ru1 S1 95.54(5) . . ? C1 Ru1 Ru2 73.58(16) . . ? C2 Ru1 Ru2 94.6(2) . . ? C3 Ru1 Ru2 130.9(2) . . ? C5 Ru1 Ru2 96.46(17) . . ? C4 Ru1 Ru2 132.3(2) . . ? S3 Ru1 Ru2 55.19(4) . . ? S2 Ru1 Ru2 55.31(3) . . ? S1 Ru1 Ru2 134.03(5) . . ? C6 Ru2 C10 37.9(2) . . ? C6 Ru2 C7 38.1(2) . . ? C10 Ru2 C7 62.7(2) . . ? C6 Ru2 C9 62.6(2) . . ? C10 Ru2 C9 36.9(2) . . ? C7 Ru2 C9 62.1(2) . . ? C6 Ru2 C8 62.5(2) . . ? C10 Ru2 C8 62.1(2) . . ? C7 Ru2 C8 36.5(2) . . ? C9 Ru2 C8 37.4(2) . . ? C6 Ru2 S3 110.40(18) . . ? C10 Ru2 S3 146.06(17) . . ? C7 Ru2 S3 100.03(18) . . ? C9 Ru2 S3 159.42(16) . . ? C8 Ru2 S3 122.06(18) . . ? C6 Ru2 S2 103.37(16) . . ? C10 Ru2 S2 91.47(15) . . ? C7 Ru2 S2 140.59(17) . . ? C9 Ru2 S2 115.02(16) . . ? C8 Ru2 S2 151.81(17) . . ? S3 Ru2 S2 85.12(5) . . ? C6 Ru2 S4 154.40(18) . . ? C10 Ru2 S4 125.51(17) . . ? C7 Ru2 S4 123.85(18) . . ? C9 Ru2 S4 93.63(18) . . ? C8 Ru2 S4 93.10(19) . . ? S3 Ru2 S4 88.42(5) . . ? S2 Ru2 S4 95.15(5) . . ? C6 Ru2 Ru1 74.05(18) . . ? C10 Ru2 Ru1 95.61(16) . . ? C7 Ru2 Ru1 95.78(19) . . ? C9 Ru2 Ru1 132.10(17) . . ? C8 Ru2 Ru1 131.85(19) . . ? S3 Ru2 Ru1 55.19(4) . . ? S2 Ru2 Ru1 55.30(3) . . ? S4 Ru2 Ru1 131.52(5) . . ? C11 S1 Ru1 109.0(2) . . ? C17 S2 Ru1 119.59(18) . . ? C17 S2 Ru2 117.69(17) . . ? Ru1 S2 Ru2 69.38(3) . . ? C23 S3 Ru1 116.11(18) . . ? C23 S3 Ru2 114.6(2) . . ? Ru1 S3 Ru2 69.62(4) . . ? C29 S4 Ru2 113.2(2) . . ? C5 C1 C6 127.2(5) . . ? C5 C1 C2 106.3(6) . . ? C6 C1 C2 123.6(6) . . ? C5 C1 Ru1 72.4(3) . . ? C6 C1 Ru1 106.6(3) . . ? C2 C1 Ru1 70.8(3) . . ? C3 C2 C1 107.8(6) . . ? C3 C2 Ru1 72.3(4) . . ? C1 C2 Ru1 70.4(3) . . ? C2 C3 C4 109.3(7) . . ? C2 C3 Ru1 71.2(4) . . ? C4 C3 Ru1 72.5(3) . . ? C5 C4 C3 107.3(7) . . ? C5 C4 Ru1 71.0(3) . . ? C3 C4 Ru1 69.9(4) . . ? C4 C5 C1 109.3(6) . . ? C4 C5 Ru1 72.6(4) . . ? C1 C5 Ru1 69.9(3) . . ? C10 C6 C1 125.3(5) . . ? C10 C6 C7 106.8(6) . . ? C1 C6 C7 124.7(6) . . ? C10 C6 Ru2 71.6(3) . . ? C1 C6 Ru2 105.8(4) . . ? C7 C6 Ru2 71.7(3) . . ? C8 C7 C6 108.3(5) . . ? C8 C7 Ru2 72.3(3) . . ? C6 C7 Ru2 70.2(3) . . ? C7 C8 C9 108.6(6) . . ? C7 C8 Ru2 71.2(3) . . ? C9 C8 Ru2 71.3(3) . . ? C10 C9 C8 107.8(6) . . ? C10 C9 Ru2 70.8(3) . . ? C8 C9 Ru2 71.3(4) . . ? C9 C10 C6 108.5(5) . . ? C9 C10 Ru2 72.4(4) . . ? C6 C10 Ru2 70.5(3) . . ? C16 C11 C12 117.9(6) . . ? C16 C11 S1 124.5(6) . . ? C12 C11 S1 117.6(5) . . ? C13 C12 C11 120.6(8) . . ? C14 C13 C12 119.2(9) . . ? C13 C14 C15 122.1(8) . . ? C13 C14 Cl1 118.1(8) . . ? C15 C14 Cl1 119.8(8) . . ? C14 C15 C16 118.4(8) . . ? C15 C16 C11 121.6(8) . . ? C18 C17 C22 119.0(5) . . ? C18 C17 S2 125.7(4) . . ? C22 C17 S2 115.3(4) . . ? C19 C18 C17 121.7(5) . . ? C20 C19 C18 118.3(6) . . ? C21 C20 C19 121.9(6) . . ? C21 C20 Cl2 119.8(5) . . ? C19 C20 Cl2 118.3(5) . . ? C20 C21 C22 119.6(5) . . ? C17 C22 C21 119.5(6) . . ? C28 C23 C24 119.0(5) . . ? C28 C23 S3 119.5(4) . . ? C24 C23 S3 120.5(4) . . ? C23 C24 C25 120.6(6) . . ? C26 C25 C24 119.1(6) . . ? C25 C26 C27 121.7(6) . . ? C25 C26 Cl3 118.7(6) . . ? C27 C26 Cl3 119.6(6) . . ? C26 C27 C28 119.0(6) . . ? C23 C28 C27 120.4(6) . . ? C30 C29 C34 118.4(6) . . ? C30 C29 S4 125.5(5) . . ? C34 C29 S4 116.1(5) . . ? C29 C30 C31 120.6(6) . . ? C32 C31 C30 119.1(7) . . ? C33 C32 C31 121.2(7) . . ? C33 C32 Cl4 119.2(7) . . ? C31 C32 Cl4 119.6(7) . . ? C32 C33 C34 119.9(8) . . ? C33 C34 C29 120.9(8) . . ? C3 C2 H2 125.2 . . ? C1 C2 H2 124.4 . . ? Ru1 C2 H2 108.7 . . ? C2 C3 H3 129.0 . . ? C4 C3 H3 121.2 . . ? Ru1 C3 H3 128.8 . . ? C5 C4 H4 123.8 . . ? C3 C4 H4 125.6 . . ? Ru1 C4 H4 108.0 . . ? C4 C5 H5 124.3 . . ? C1 C5 H5 123.6 . . ? Ru1 C5 H5 108.6 . . ? C8 C7 H7 124.3 . . ? C6 C7 H7 124.9 . . ? Ru2 C7 H7 109.0 . . ? C7 C8 H8 123.9 . . ? C9 C8 H8 125.0 . . ? Ru2 C8 H8 109.2 . . ? C10 C9 H9 125.4 . . ? C8 C9 H9 126.7 . . ? Ru2 C9 H9 126.6 . . ? C9 C10 H10 125.1 . . ? C6 C10 H10 123.9 . . ? Ru2 C10 H10 108.9 . . ? C13 C12 H12 119.9 . . ? C11 C12 H12 119.5 . . ? C14 C13 H13 117.9 . . ? C12 C13 H13 122.9 . . ? C14 C15 H15 118.7 . . ? C16 C15 H15 122.9 . . ? C15 C16 H16 119.8 . . ? C11 C16 H16 118.6 . . ? C19 C18 H18 119.1 . . ? C17 C18 H18 119.2 . . ? C20 C19 H19 118.6 . . ? C18 C19 H19 123.0 . . ? C20 C21 H21 120.5 . . ? C22 C21 H21 119.9 . . ? C17 C22 H22 119.0 . . ? C21 C22 H22 121.5 . . ? C23 C24 H24 117.8 . . ? C25 C24 H24 121.5 . . ? C26 C25 H25 121.0 . . ? C24 C25 H25 119.9 . . ? C26 C27 H27 114.6 . . ? C28 C27 H27 126.4 . . ? C23 C28 H28 116.9 . . ? C27 C28 H28 122.6 . . ? C29 C30 H30 119.8 . . ? C31 C30 H30 119.6 . . ? C32 C31 H31 118.5 . . ? C30 C31 H31 122.4 . . ? C32 C33 H33 119.7 . . ? C34 C33 H33 120.4 . . ? C33 C34 H34 120.0 . . ? C29 C34 H34 119.2 . . ? _diffrn_measured_fraction_theta_max 0.750 _diffrn_reflns_theta_full 30.33 _diffrn_measured_fraction_theta_full 0.750 _refine_diff_density_max 0.583 _refine_diff_density_min -0.903 _refine_diff_density_rms 0.107 #=========END data_compound_5a _database_code_CSD 191663 _chemical_compound_source 'Local laboratory' _exptl_crystal_description Plate _exptl_crystal_colour Red _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.03 _cell_measurement_temperature 298 _refine_ls_hydrogen_treatment refxyz _diffrn_measurement_device 'Mac Science MXC18' _diffrn_measurement_method '¥q ¥w scans' _computing_cell_refinement 'MXC(MAC Science)' _computing_data_collection 'MXC(MAC Science)' _computing_data_reduction 'maXus (Mackay et al., 1999)' _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 25 loop_ _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_wavelength_id all _cell_formula_units_Z 2 _exptl_crystal_density_diffrn 1.504 _exptl_crystal_density_method 'not measured' _exptl_special_details ; ? ; _chemical_formula_weight 1278.842 _diffrn_radiation_type ' MoK¥a' loop_ _symmetry_equiv_pos_as_xyz +X,+Y,+Z -X,-Y,-Z _symmetry_space_group_name_H-M 'P -1 ' _symmetry_cell_setting Triclinic _chemical_formula_moiety 'C58 H48 B2 F8 O2 P2 Ru2 S2 ' _chemical_formula_sum 'C58 H48 B2 F8 O2 P2 Ru2 S2 ' _chemical_name_systematic ; ? ; _cell_length_a 10.5000(5) _cell_length_b 14.0460(7) _cell_length_c 20.3850(10) _cell_angle_alpha 94.024(2) _cell_angle_beta 97.434(2) _cell_angle_gamma 107.514(2) _cell_volume 2824.0(3) _diffrn_reflns_number 10295 _diffrn_reflns_theta_max 27.03 _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? 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' B B 0.0013 0.0007 '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' F F 0.0171 0.0103 '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' Ru Ru -1.2594 0.8363 '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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _exptl_absorpt_coefficient_mu 0.73 _reflns_number_total 10295 _reflns_number_gt 7168 _reflns_threshold_expression >2sigma(I) _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even largeR. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[¥s^2^(Fo^2^)+(0.1856P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10295 _refine_ls_number_parameters 685 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1086 _refine_ls_R_factor_gt 0.0811 _refine_ls_wR_factor_ref 0.2700 _refine_ls_wR_factor_gt 0.2508 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.051 _refine_ls_shift/su_max 0.059 _refine_ls_shift/su_mean 0.010 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 0.77745(6) -0.13542(4) 0.35417(3) 0.0366(2) Uani 1 1 d . . . Ru2 Ru 0.70712(6) 0.00259(4) 0.28147(3) 0.0371(2) Uani 1 1 d . . . S1 S 0.81129(19) -0.11429(14) 0.24375(9) 0.0406(4) Uani 1 1 d . . . S2 S 0.55790(18) -0.15150(14) 0.29986(10) 0.0415(4) Uani 1 1 d . . . P1 P 0.7461(2) -0.31239(15) 0.34712(11) 0.0422(5) Uani 1 1 d . . . P2 P 0.58606(19) 0.00743(15) 0.17447(10) 0.0394(4) Uani 1 1 d . . . F1 F 1.079(2) 0.3291(14) 0.1636(10) 0.270(11) Uani 1 1 d . . . F2 F 1.2117(10) 0.2597(17) 0.1582(9) 0.288(12) Uani 1 1 d . . . F3 F 1.0225(13) 0.1963(17) 0.1978(6) 0.224(9) Uani 1 1 d . . . F4 F 1.0168(8) 0.1968(7) 0.0902(4) 0.111(3) Uani 1 1 d . . . F5 F 0.4213(8) -0.0861(7) 0.4227(5) 0.125(3) Uani 1 1 d . . . F6 F 0.2118(9) -0.1458(8) 0.3705(4) 0.126(3) Uani 1 1 d . . . F7 F 0.3074(11) -0.2428(6) 0.4239(6) 0.133(4) Uani 1 1 d . . . F8 F 0.2461(8) -0.1299(7) 0.4788(4) 0.105(3) Uani 1 1 d . . . O1 O 0.6278(13) 0.3362(8) 0.4660(7) 0.144(5) Uani 1 1 d . . . O2 O 0.1748(9) 0.1075(7) 0.2924(5) 0.100(3) Uani 1 1 d . . . C1 C 0.8596(9) 0.0118(6) 0.4141(4) 0.0479(19) Uani 1 1 d . . . C2 C 0.9667(8) -0.0264(6) 0.4055(4) 0.050(2) Uani 1 1 d . . . C3 C 0.9475(9) -0.1144(7) 0.4366(4) 0.056(2) Uani 1 1 d . . . C4 C 0.8266(10) -0.1325(6) 0.4636(4) 0.054(2) Uani 1 1 d . . . C5 C 0.7706(9) -0.0574(6) 0.4517(4) 0.0484(19) Uani 1 1 d . . . C6 C 0.8189(9) 0.0840(6) 0.3768(4) 0.0466(19) Uani 1 1 d . . . C7 C 0.8877(9) 0.1306(6) 0.3258(5) 0.054(2) Uani 1 1 d . . . C8 C 0.7996(9) 0.1688(6) 0.2864(5) 0.054(2) Uani 1 1 d . . . C9 C 0.6739(10) 0.1471(6) 0.3147(4) 0.052(2) Uani 1 1 d . . . C10 C 0.6873(10) 0.0951(6) 0.3692(5) 0.054(2) Uani 1 1 d . . . C11 C 0.6693(9) -0.2133(6) 0.1997(4) 0.0464(18) Uani 1 1 d . . . C12 C 0.6736(12) -0.2744(7) 0.1448(5) 0.065(3) Uani 1 1 d . . . C13 C 0.5537(13) -0.3451(7) 0.1123(5) 0.068(3) Uani 1 1 d . . . C14 C 0.4386(14) -0.3499(8) 0.1321(6) 0.082(4) Uani 1 1 d . . . C15 C 0.4281(10) -0.2913(6) 0.1914(5) 0.059(2) Uani 1 1 d . . . C16 C 0.5478(8) -0.2243(6) 0.2241(4) 0.0450(18) Uani 1 1 d . . . C17 C 0.8433(9) -0.3661(7) 0.2952(5) 0.054(2) Uani 1 1 d . . . C18 C 0.8309(10) -0.4683(7) 0.2955(6) 0.065(2) Uani 1 1 d . . . C19 C 0.8997(12) -0.5126(9) 0.2606(7) 0.079(3) Uani 1 1 d . . . C20 C 0.9878(13) -0.4563(10) 0.2212(6) 0.080(3) Uani 1 1 d . . . C21 C 1.0082(12) -0.3533(10) 0.2241(7) 0.081(3) Uani 1 1 d . . . C22 C 0.9367(10) -0.3072(8) 0.2604(5) 0.063(2) Uani 1 1 d . . . C23 C 0.7952(10) -0.3534(7) 0.4261(5) 0.055(2) Uani 1 1 d . . . C24 C 0.7018(11) -0.3882(8) 0.4694(6) 0.066(3) Uani 1 1 d . . . C25 C 0.7471(16) -0.4120(11) 0.5334(6) 0.096(4) Uani 1 1 d . . . C26 C 0.8808(16) -0.4067(11) 0.5508(7) 0.102(5) Uani 1 1 d . . . C27 C 0.9698(14) -0.3708(11) 0.5088(6) 0.089(4) Uani 1 1 d . . . C28 C 0.9278(10) -0.3463(8) 0.4454(5) 0.062(2) Uani 1 1 d . . . C29 C 0.5699(8) -0.3880(6) 0.3192(4) 0.0462(18) Uani 1 1 d . . . C30 C 0.4720(9) -0.3683(6) 0.3539(5) 0.052(2) Uani 1 1 d . . . C31 C 0.3377(9) -0.4238(7) 0.3335(6) 0.061(2) Uani 1 1 d . . . C32 C 0.2998(9) -0.4983(7) 0.2810(6) 0.060(2) Uani 1 1 d . . . C33 C 0.3946(9) -0.5173(7) 0.2454(6) 0.061(3) Uani 1 1 d . . . C34 C 0.5295(9) -0.4605(6) 0.2648(5) 0.051(2) Uani 1 1 d . . . C35 C 0.6038(8) 0.1344(6) 0.1526(4) 0.0440(17) Uani 1 1 d . . . C36 C 0.5173(10) 0.1848(7) 0.1741(5) 0.054(2) Uani 1 1 d . . . C37 C 0.5336(12) 0.2826(8) 0.1630(5) 0.066(3) Uani 1 1 d . . . C38 C 0.6380(12) 0.3353(7) 0.1328(6) 0.073(3) Uani 1 1 d . . . C39 C 0.7197(11) 0.2857(8) 0.1106(6) 0.066(3) Uani 1 1 d . . . C40 C 0.7042(9) 0.1881(7) 0.1211(5) 0.055(2) Uani 1 1 d . . . C41 C 0.6438(8) -0.0485(6) 0.1073(4) 0.0416(17) Uani 1 1 d . . . C42 C 0.7840(10) -0.0149(7) 0.1054(4) 0.054(2) Uani 1 1 d . . . C43 C 0.8337(13) -0.0540(10) 0.0526(5) 0.076(3) Uani 1 1 d . . . C44 C 0.7476(15) -0.1247(10) 0.0043(5) 0.082(4) Uani 1 1 d . . . C45 C 0.6143(15) -0.1600(9) 0.0065(5) 0.079(3) Uani 1 1 d . . . C46 C 0.5586(10) -0.1215(7) 0.0582(4) 0.054(2) Uani 1 1 d . . . C47 C 0.4034(8) -0.0430(6) 0.1645(4) 0.0476(18) Uani 1 1 d . . . C48 C 0.3358(9) -0.0627(7) 0.2193(5) 0.055(2) Uani 1 1 d . . . C49 C 0.1978(9) -0.0929(8) 0.2118(6) 0.064(3) Uani 1 1 d . . . C50 C 0.1237(11) -0.1038(10) 0.1505(7) 0.084(4) Uani 1 1 d . . . C51 C 0.1870(10) -0.0814(10) 0.0948(7) 0.080(3) Uani 1 1 d . . . C52 C 0.3262(9) -0.0505(7) 0.1019(5) 0.058(2) Uani 1 1 d . . . C53 C 0.2942(13) 0.1679(9) 0.3345(7) 0.082(3) Uani 1 1 d . . . C54 C 0.3442(12) 0.1271(9) 0.3901(7) 0.075(3) Uani 1 1 d . . . C55 C 0.4529(13) 0.1810(9) 0.4327(7) 0.075(3) Uani 1 1 d . . . C56 C 0.5223(14) 0.2798(10) 0.4239(8) 0.086(4) Uani 1 1 d . . . C57 C 0.4749(17) 0.3200(10) 0.3709(9) 0.102(5) Uani 1 1 d . . . C58 C 0.3635(17) 0.2631(11) 0.3259(8) 0.097(5) Uani 1 1 d . . . B1 B 1.0904(13) 0.2403(12) 0.1504(8) 0.075(4) Uani 1 1 d . . . B2 B 0.2989(13) -0.1506(10) 0.4235(6) 0.068(3) Uani 1 1 d . . . H2 H 1.0470 0.0285 0.4044 0.060 Uiso 1 1 d R . . H3 H 0.9943 -0.1643 0.4279 0.067 Uiso 1 1 d R . . H4 H 0.7815 -0.1963 0.4759 0.065 Uiso 1 1 d R . . H5 H 0.6809 -0.0609 0.4544 0.058 Uiso 1 1 d R . . H7 H 0.9648 0.1186 0.3118 0.065 Uiso 1 1 d R . . H8 H 0.8054 0.1854 0.2419 0.064 Uiso 1 1 d R . . H9 H 0.5879 0.1480 0.2908 0.063 Uiso 1 1 d R . . H10 H 0.6142 0.0568 0.3897 0.065 Uiso 1 1 d R . . H12 H 0.7609 -0.2695 0.1281 0.078 Uiso 1 1 d R . . H13 H 0.5646 -0.3888 0.0750 0.082 Uiso 1 1 d R . . H14 H 0.3635 -0.3960 0.1070 0.098 Uiso 1 1 d R . . H15 H 0.3469 -0.2996 0.2052 0.070 Uiso 1 1 d R . . H18 H 0.7828 -0.5084 0.3233 0.078 Uiso 1 1 d R . . H19 H 0.8969 -0.5834 0.2586 0.095 Uiso 1 1 d R . . H20 H 1.0465 -0.4863 0.1951 0.096 Uiso 1 1 d R . . H21 H 1.0699 -0.3137 0.1960 0.097 Uiso 1 1 d R . . H22 H 0.9627 -0.2353 0.2649 0.076 Uiso 1 1 d R . . H24 H 0.6148 -0.3953 0.4583 0.079 Uiso 1 1 d R . . H25 H 0.6909 -0.4341 0.5629 0.115 Uiso 1 1 d R . . H26 H 0.9175 -0.4239 0.5938 0.122 Uiso 1 1 d R . . H27 H 1.0698 -0.3661 0.5221 0.106 Uiso 1 1 d R . . H28 H 0.9957 -0.3242 0.4146 0.075 Uiso 1 1 d R . . H30 H 0.5035 -0.3157 0.3903 0.062 Uiso 1 1 d R . . H31 H 0.2770 -0.4112 0.3569 0.073 Uiso 1 1 d R . . H32 H 0.2156 -0.5380 0.2684 0.072 Uiso 1 1 d R . . H33 H 0.3775 -0.5696 0.2087 0.073 Uiso 1 1 d R . . H34 H 0.6044 -0.4733 0.2406 0.061 Uiso 1 1 d R . . H36 H 0.4450 0.1512 0.1980 0.064 Uiso 1 1 d R . . H37 H 0.4660 0.3154 0.1749 0.079 Uiso 1 1 d R . . H38 H 0.6448 0.4051 0.1290 0.088 Uiso 1 1 d R . . H39 H 0.7829 0.3222 0.0864 0.079 Uiso 1 1 d R . . H40 H 0.7651 0.1569 0.1068 0.066 Uiso 1 1 d R . . H42 H 0.8403 0.0349 0.1404 0.065 Uiso 1 1 d R . . H43 H 0.9297 -0.0336 0.0511 0.091 Uiso 1 1 d R . . H44 H 0.7825 -0.1483 -0.0335 0.098 Uiso 1 1 d R . . H45 H 0.5630 -0.2107 -0.0284 0.095 Uiso 1 1 d R . . H46 H 0.4657 -0.1496 0.0581 0.065 Uiso 1 1 d R . . H48 H 0.3900 -0.0595 0.2640 0.066 Uiso 1 1 d R . . H49 H 0.1610 -0.1072 0.2515 0.077 Uiso 1 1 d R . . H50 H 0.0290 -0.1272 0.1437 0.101 Uiso 1 1 d R . . H51 H 0.1365 -0.0880 0.0514 0.096 Uiso 1 1 d R . . H52 H 0.3719 -0.0318 0.0645 0.070 Uiso 1 1 d R . . H54 H 0.2967 0.0594 0.3967 0.090 Uiso 1 1 d R . . H55 H 0.4898 0.1556 0.4704 0.090 Uiso 1 1 d R . . H57 H 0.5170 0.3873 0.3633 0.123 Uiso 1 1 d R . . H58 H 0.3259 0.2926 0.2892 0.116 Uiso 1 1 d 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 0.0378(4) 0.0375(3) 0.0317(3) 0.0014(2) 0.0042(2) 0.0089(2) Ru2 0.0405(4) 0.0349(3) 0.0346(3) 0.0021(2) 0.0073(2) 0.0096(2) S1 0.0443(11) 0.0432(10) 0.0342(9) 0.0025(8) 0.0074(7) 0.0133(8) S2 0.0378(10) 0.0413(10) 0.0442(10) 0.0081(8) 0.0081(7) 0.0094(7) P1 0.0445(11) 0.0384(10) 0.0427(11) 0.0046(8) 0.0068(8) 0.0117(8) P2 0.0389(11) 0.0410(10) 0.0386(10) 0.0066(8) 0.0083(8) 0.0118(8) F1 0.37(3) 0.186(15) 0.224(19) -0.106(14) -0.073(17) 0.118(16) F2 0.054(6) 0.46(3) 0.279(19) -0.185(19) 0.004(8) 0.028(10) F3 0.142(9) 0.41(3) 0.087(7) 0.052(12) 0.020(7) 0.028(12) F4 0.095(5) 0.127(7) 0.073(5) 0.001(5) 0.002(4) -0.011(5) F5 0.076(5) 0.136(7) 0.142(8) 0.032(6) 0.015(5) -0.003(5) F6 0.114(6) 0.168(9) 0.076(5) 0.020(6) -0.011(4) 0.024(6) F7 0.164(9) 0.081(5) 0.160(10) -0.016(6) 0.011(7) 0.060(5) F8 0.103(5) 0.150(7) 0.078(5) -0.019(5) 0.019(4) 0.066(5) O1 0.161(11) 0.083(7) 0.153(12) 0.029(7) -0.011(9) -0.002(7) O2 0.084(6) 0.101(7) 0.115(8) 0.023(6) 0.011(5) 0.027(5) C1 0.053(5) 0.046(4) 0.036(4) -0.007(3) 0.002(3) 0.008(3) C2 0.041(5) 0.049(5) 0.045(5) -0.002(4) -0.010(3) 0.000(3) C3 0.061(6) 0.056(5) 0.043(5) -0.005(4) -0.009(4) 0.018(4) C4 0.076(6) 0.033(4) 0.041(4) 0.001(3) 0.004(4) 0.003(4) C5 0.059(5) 0.049(5) 0.036(4) 0.003(3) 0.008(3) 0.015(4) C6 0.060(5) 0.034(4) 0.038(4) -0.003(3) 0.002(3) 0.007(3) C7 0.060(5) 0.041(4) 0.050(5) -0.004(4) 0.001(4) 0.004(4) C8 0.071(6) 0.033(4) 0.048(5) 0.005(3) 0.001(4) 0.007(4) C9 0.073(6) 0.044(5) 0.041(4) 0.000(4) 0.008(4) 0.022(4) C10 0.068(6) 0.037(4) 0.054(5) -0.009(4) 0.012(4) 0.015(4) C11 0.062(5) 0.038(4) 0.034(4) -0.004(3) 0.000(3) 0.014(3) C12 0.095(8) 0.057(6) 0.042(5) -0.002(4) 0.007(5) 0.024(5) C13 0.092(8) 0.049(5) 0.050(6) -0.003(4) -0.002(5) 0.011(5) C14 0.104(9) 0.042(5) 0.071(7) -0.003(5) -0.028(7) 0.000(5) C15 0.055(5) 0.042(5) 0.065(6) 0.005(4) -0.009(4) 0.002(4) C16 0.051(5) 0.034(4) 0.042(4) 0.006(3) -0.002(3) 0.006(3) C17 0.046(5) 0.051(5) 0.062(6) 0.000(4) 0.001(4) 0.015(4) C18 0.061(6) 0.052(5) 0.080(7) 0.003(5) 0.011(5) 0.016(4) C19 0.084(8) 0.059(6) 0.089(9) -0.012(6) -0.009(6) 0.029(5) C20 0.083(8) 0.097(9) 0.079(8) -0.006(7) 0.008(6) 0.059(7) C21 0.073(8) 0.093(9) 0.092(9) 0.027(7) 0.030(6) 0.041(6) C22 0.063(6) 0.070(6) 0.070(6) 0.011(5) 0.024(5) 0.036(5) C23 0.070(6) 0.045(5) 0.051(5) 0.009(4) 0.009(4) 0.017(4) C24 0.065(6) 0.065(6) 0.067(6) 0.016(5) 0.007(5) 0.019(5) C25 0.119(11) 0.102(10) 0.057(7) 0.038(7) 0.015(7) 0.014(8) C26 0.112(11) 0.114(11) 0.075(9) 0.047(8) -0.003(7) 0.029(8) C27 0.090(9) 0.110(10) 0.066(7) 0.026(7) -0.008(6) 0.036(7) C28 0.061(6) 0.074(6) 0.052(5) 0.012(5) 0.000(4) 0.023(5) C29 0.048(5) 0.038(4) 0.050(5) 0.010(3) 0.006(3) 0.010(3) C30 0.054(5) 0.044(4) 0.057(5) 0.010(4) 0.018(4) 0.011(3) C31 0.052(5) 0.044(5) 0.087(7) 0.018(5) 0.018(5) 0.010(4) C32 0.041(5) 0.053(5) 0.082(7) 0.017(5) 0.006(4) 0.012(4) C33 0.045(5) 0.042(5) 0.088(7) 0.004(4) -0.014(4) 0.012(3) C34 0.050(5) 0.042(4) 0.060(5) 0.005(4) 0.000(4) 0.017(3) C35 0.042(4) 0.047(4) 0.043(4) 0.004(3) 0.002(3) 0.017(3) C36 0.061(6) 0.048(5) 0.058(5) 0.008(4) 0.017(4) 0.022(4) C37 0.093(8) 0.058(6) 0.052(6) -0.004(5) 0.000(5) 0.038(5) C38 0.086(8) 0.036(5) 0.099(9) 0.018(5) 0.011(6) 0.019(5) C39 0.069(6) 0.057(6) 0.069(7) 0.018(5) 0.016(5) 0.013(5) C40 0.047(5) 0.054(5) 0.064(6) 0.011(4) 0.013(4) 0.016(4) C41 0.040(4) 0.046(4) 0.045(4) 0.010(3) 0.016(3) 0.017(3) C42 0.072(6) 0.058(5) 0.038(4) 0.013(4) 0.010(4) 0.027(4) C43 0.091(8) 0.114(10) 0.053(6) 0.039(6) 0.036(6) 0.062(7) C44 0.122(11) 0.106(10) 0.042(6) 0.013(6) 0.029(6) 0.065(8) C45 0.134(11) 0.069(7) 0.038(5) 0.009(5) -0.001(6) 0.042(7) C46 0.062(5) 0.058(5) 0.040(4) -0.003(4) 0.001(4) 0.019(4) C47 0.045(5) 0.046(4) 0.053(5) 0.012(4) 0.010(4) 0.015(3) C48 0.057(5) 0.060(5) 0.058(5) 0.028(4) 0.019(4) 0.024(4) C49 0.040(5) 0.089(7) 0.071(6) 0.036(6) 0.018(4) 0.021(4) C50 0.048(6) 0.097(9) 0.109(10) 0.040(8) 0.020(6) 0.017(5) C51 0.049(6) 0.108(9) 0.083(8) 0.040(7) 0.004(5) 0.019(5) C52 0.040(5) 0.071(6) 0.062(6) 0.028(5) 0.006(4) 0.012(4) C53 0.093(9) 0.072(7) 0.102(10) 0.034(7) 0.042(7) 0.043(6) C54 0.074(8) 0.077(7) 0.089(8) 0.037(7) 0.040(6) 0.029(6) C55 0.082(8) 0.075(7) 0.081(8) 0.025(6) 0.032(6) 0.031(6) C56 0.097(9) 0.069(8) 0.096(10) 0.024(7) 0.024(7) 0.024(6) C57 0.116(12) 0.063(8) 0.130(13) 0.033(9) 0.036(10) 0.020(7) C58 0.135(12) 0.092(10) 0.101(10) 0.061(9) 0.068(10) 0.060(9) B1 0.056(8) 0.081(9) 0.080(9) 0.001(7) 0.013(6) 0.009(6) B2 0.074(8) 0.067(8) 0.058(7) -0.004(6) 0.009(6) 0.018(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 C2 2.190(7) . ? Ru1 C1 2.194(8) . ? Ru1 C4 2.219(9) . ? Ru1 C3 2.221(8) . ? Ru1 C5 2.223(8) . ? Ru1 S1 2.349(2) . ? Ru1 S2 2.363(2) . ? Ru1 P1 2.398(2) . ? Ru1 Ru2 2.7351(8) . ? Ru2 C6 2.180(8) . ? Ru2 C10 2.206(8) . ? Ru2 C7 2.218(8) . ? Ru2 C8 2.231(8) . ? Ru2 C9 2.234(8) . ? Ru2 S2 2.3463(19) . ? Ru2 S1 2.367(2) . ? Ru2 P2 2.394(2) . ? S1 C11 1.787(8) . ? S2 C16 1.764(9) . ? P1 C23 1.812(10) . ? P1 C29 1.826(8) . ? P1 C17 1.834(9) . ? P2 C41 1.791(8) . ? P2 C47 1.812(8) . ? P2 C35 1.829(8) . ? F1 B1 1.30(2) . ? F2 B1 1.206(16) . ? F3 B1 1.348(18) . ? F4 B1 1.357(16) . ? F5 B2 1.335(14) . ? F6 B2 1.342(15) . ? F7 B2 1.326(15) . ? F8 B2 1.368(14) . ? O1 C56 1.312(17) . ? O2 C53 1.417(17) . ? C1 C2 1.409(13) . ? C1 C6 1.440(12) . ? C1 C5 1.467(12) . ? C2 C3 1.401(12) . ? C3 C4 1.409(14) . ? C4 C5 1.375(13) . ? C6 C7 1.427(12) . ? C6 C10 1.427(13) . ? C7 C8 1.398(13) . ? C8 C9 1.465(13) . ? C9 C10 1.386(13) . ? C11 C12 1.375(12) . ? C11 C16 1.399(12) . ? C12 C13 1.396(15) . ? C13 C14 1.308(17) . ? C14 C15 1.450(17) . ? C15 C16 1.375(11) . ? C17 C22 1.387(13) . ? C17 C18 1.402(13) . ? C18 C19 1.326(16) . ? C19 C20 1.403(18) . ? C20 C21 1.393(17) . ? C21 C22 1.378(15) . ? C23 C28 1.368(14) . ? C23 C24 1.405(14) . ? C24 C25 1.427(16) . ? C25 C26 1.381(19) . ? C26 C27 1.358(19) . ? C27 C28 1.411(15) . ? C29 C34 1.381(12) . ? C29 C30 1.403(12) . ? C30 C31 1.381(12) . ? C31 C32 1.372(15) . ? C32 C33 1.382(15) . ? C33 C34 1.389(12) . ? C35 C40 1.362(12) . ? C35 C36 1.402(12) . ? C36 C37 1.372(13) . ? C37 C38 1.371(16) . ? C38 C39 1.357(16) . ? C39 C40 1.367(13) . ? C41 C46 1.388(12) . ? C41 C42 1.411(12) . ? C42 C43 1.402(14) . ? C43 C44 1.366(18) . ? C44 C45 1.345(17) . ? C45 C46 1.419(15) . ? C47 C52 1.399(13) . ? C47 C48 1.400(12) . ? C48 C49 1.367(13) . ? C49 C50 1.357(17) . ? C50 C51 1.396(17) . ? C51 C52 1.379(13) . ? C53 C58 1.353(17) . ? C53 C54 1.415(17) . ? C54 C55 1.327(18) . ? C55 C56 1.397(16) . ? C56 C57 1.36(2) . ? C57 C58 1.38(2) . ? C2 H2 0.9598 . ? C3 H3 0.9883 . ? C4 H4 0.9475 . ? C5 H5 0.9376 . ? C7 H7 0.9495 . ? C8 H8 0.9569 . ? C9 H9 0.9739 . ? C10 H10 0.9585 . ? C12 H12 1.0038 . ? C13 H13 0.9844 . ? C14 H14 0.9197 . ? C15 H15 0.9087 . ? C18 H18 0.9157 . ? C19 H19 0.9835 . ? C20 H20 1.0250 . ? C21 H21 0.9907 . ? C22 H22 0.9569 . ? C24 H24 0.8857 . ? C25 H25 0.9029 . ? C26 H26 0.9866 . ? C27 H27 1.0310 . ? C28 H28 1.0038 . ? C30 H30 0.9588 . ? C31 H31 0.8948 . ? C32 H32 0.8849 . ? C33 H33 0.9690 . ? C34 H34 1.0324 . ? C36 H36 0.9728 . ? C37 H37 1.0003 . ? C38 H38 0.9715 . ? C39 H39 0.9284 . ? C40 H40 0.9409 . ? C42 H42 0.9594 . ? C43 H43 0.9663 . ? C44 H44 0.9733 . ? C45 H45 0.9513 . ? C46 H46 0.9357 . ? C48 H48 1.0011 . ? C49 H49 0.9486 . ? C50 H50 0.9365 . ? C51 H51 0.9532 . ? C52 H52 0.9637 . ? C54 H54 0.9598 . ? C55 H55 0.9549 . ? C57 H57 0.9487 . ? C58 H58 0.9766 . ? 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 C2 Ru1 C1 37.5(3) . . ? C2 Ru1 C4 62.1(3) . . ? C1 Ru1 C4 62.3(3) . . ? C2 Ru1 C3 37.0(3) . . ? C1 Ru1 C3 62.1(3) . . ? C4 Ru1 C3 37.0(4) . . ? C2 Ru1 C5 63.2(3) . . ? C1 Ru1 C5 38.8(3) . . ? C4 Ru1 C5 36.1(3) . . ? C3 Ru1 C5 61.7(3) . . ? C2 Ru1 S1 98.8(2) . . ? C1 Ru1 S1 108.4(2) . . ? C4 Ru1 S1 159.1(3) . . ? C3 Ru1 S1 122.4(3) . . ? C5 Ru1 S1 144.9(2) . . ? C2 Ru1 S2 143.4(2) . . ? C1 Ru1 S2 108.5(2) . . ? C4 Ru1 S2 122.7(3) . . ? C3 Ru1 S2 159.3(3) . . ? C5 Ru1 S2 99.1(2) . . ? S1 Ru1 S2 77.48(7) . . ? C2 Ru1 P1 120.9(2) . . ? C1 Ru1 P1 147.7(2) . . ? C4 Ru1 P1 86.8(2) . . ? C3 Ru1 P1 87.8(2) . . ? C5 Ru1 P1 117.8(2) . . ? S1 Ru1 P1 97.29(7) . . ? S2 Ru1 P1 95.59(7) . . ? C2 Ru1 Ru2 93.5(2) . . ? C1 Ru1 Ru2 72.0(2) . . ? C4 Ru1 Ru2 129.9(2) . . ? C3 Ru1 Ru2 130.0(2) . . ? C5 Ru1 Ru2 94.4(2) . . ? S1 Ru1 Ru2 54.87(5) . . ? S2 Ru1 Ru2 54.21(5) . . ? P1 Ru1 Ru2 140.18(6) . . ? C6 Ru2 C10 38.0(3) . . ? C6 Ru2 C7 37.9(3) . . ? C10 Ru2 C7 63.2(4) . . ? C6 Ru2 C8 62.3(3) . . ? C10 Ru2 C8 62.8(4) . . ? C7 Ru2 C8 36.6(3) . . ? C6 Ru2 C9 62.0(3) . . ? C10 Ru2 C9 36.4(3) . . ? C7 Ru2 C9 62.5(4) . . ? C8 Ru2 C9 38.3(3) . . ? C6 Ru2 S2 109.2(2) . . ? C10 Ru2 S2 98.1(2) . . ? C7 Ru2 S2 144.9(2) . . ? C8 Ru2 S2 158.6(3) . . ? C9 Ru2 S2 120.5(3) . . ? C6 Ru2 S1 109.9(2) . . ? C10 Ru2 S1 144.8(3) . . ? C7 Ru2 S1 100.6(3) . . ? C8 Ru2 S1 123.5(3) . . ? C9 Ru2 S1 161.5(3) . . ? S2 Ru2 S1 77.45(7) . . ? C6 Ru2 P2 147.9(2) . . ? C10 Ru2 P2 119.8(3) . . ? C7 Ru2 P2 120.0(2) . . ? C8 Ru2 P2 87.6(2) . . ? C9 Ru2 P2 87.8(2) . . ? S2 Ru2 P2 94.93(7) . . ? S1 Ru2 P2 95.47(7) . . ? C6 Ru2 Ru1 73.5(2) . . ? C10 Ru2 Ru1 94.3(3) . . ? C7 Ru2 Ru1 95.2(2) . . ? C8 Ru2 Ru1 131.4(2) . . ? C9 Ru2 Ru1 130.4(2) . . ? S2 Ru2 Ru1 54.77(5) . . ? S1 Ru2 Ru1 54.24(5) . . ? P2 Ru2 Ru1 138.58(5) . . ? C11 S1 Ru1 100.6(3) . . ? C11 S1 Ru2 101.8(3) . . ? Ru1 S1 Ru2 70.89(6) . . ? C16 S2 Ru2 100.2(3) . . ? C16 S2 Ru1 102.3(3) . . ? Ru2 S2 Ru1 71.02(5) . . ? C23 P1 C29 105.7(4) . . ? C23 P1 C17 99.5(4) . . ? C29 P1 C17 105.0(4) . . ? C23 P1 Ru1 113.2(3) . . ? C29 P1 Ru1 112.5(3) . . ? C17 P1 Ru1 119.5(3) . . ? C41 P2 C47 109.0(4) . . ? C41 P2 C35 103.1(4) . . ? C47 P2 C35 99.8(4) . . ? C41 P2 Ru2 113.1(3) . . ? C47 P2 Ru2 116.3(3) . . ? C35 P2 Ru2 114.1(3) . . ? C2 C1 C6 126.9(8) . . ? C2 C1 C5 106.9(8) . . ? C6 C1 C5 123.5(8) . . ? C2 C1 Ru1 71.1(5) . . ? C6 C1 Ru1 108.0(5) . . ? C5 C1 Ru1 71.7(5) . . ? C3 C2 C1 108.4(8) . . ? C3 C2 Ru1 72.7(5) . . ? C1 C2 Ru1 71.4(4) . . ? C2 C3 C4 108.0(8) . . ? C2 C3 Ru1 70.3(5) . . ? C4 C3 Ru1 71.4(5) . . ? C5 C4 C3 109.9(8) . . ? C5 C4 Ru1 72.1(5) . . ? C3 C4 Ru1 71.6(5) . . ? C4 C5 C1 106.8(8) . . ? C4 C5 Ru1 71.8(5) . . ? C1 C5 Ru1 69.5(4) . . ? C7 C6 C10 108.6(8) . . ? C7 C6 C1 123.4(8) . . ? C10 C6 C1 125.2(8) . . ? C7 C6 Ru2 72.5(5) . . ? C10 C6 Ru2 72.0(5) . . ? C1 C6 Ru2 106.4(5) . . ? C8 C7 C6 107.8(8) . . ? C8 C7 Ru2 72.2(5) . . ? C6 C7 Ru2 69.6(4) . . ? C7 C8 C9 107.4(8) . . ? C7 C8 Ru2 71.2(5) . . ? C9 C8 Ru2 71.0(4) . . ? C10 C9 C8 108.2(8) . . ? C10 C9 Ru2 70.7(5) . . ? C8 C9 Ru2 70.7(5) . . ? C9 C10 C6 107.9(8) . . ? C9 C10 Ru2 72.9(5) . . ? C6 C10 Ru2 70.0(5) . . ? C12 C11 C16 120.6(8) . . ? C12 C11 S1 124.5(8) . . ? C16 C11 S1 114.9(6) . . ? C11 C12 C13 118.9(10) . . ? C14 C13 C12 120.3(10) . . ? C13 C14 C15 123.3(10) . . ? C16 C15 C14 115.4(10) . . ? C15 C16 C11 121.1(8) . . ? C15 C16 S2 122.3(7) . . ? C11 C16 S2 116.6(6) . . ? C22 C17 C18 119.3(9) . . ? C22 C17 P1 121.9(7) . . ? C18 C17 P1 118.6(8) . . ? C19 C18 C17 122.4(11) . . ? C18 C19 C20 119.4(11) . . ? C21 C20 C19 118.6(10) . . ? C22 C21 C20 121.9(11) . . ? C21 C22 C17 118.1(10) . . ? C28 C23 C24 119.1(9) . . ? C28 C23 P1 119.1(7) . . ? C24 C23 P1 121.7(8) . . ? C23 C24 C25 119.8(11) . . ? C26 C25 C24 119.8(12) . . ? C27 C26 C25 119.3(12) . . ? C26 C27 C28 121.9(12) . . ? C23 C28 C27 119.9(11) . . ? C34 C29 C30 119.3(8) . . ? C34 C29 P1 123.1(7) . . ? C30 C29 P1 117.6(7) . . ? C31 C30 C29 118.9(9) . . ? C32 C31 C30 121.1(9) . . ? C31 C32 C33 120.7(8) . . ? C32 C33 C34 118.5(9) . . ? C29 C34 C33 121.5(9) . . ? C40 C35 C36 116.4(8) . . ? C40 C35 P2 124.2(6) . . ? C36 C35 P2 119.1(6) . . ? C37 C36 C35 121.0(9) . . ? C38 C37 C36 121.0(10) . . ? C39 C38 C37 117.9(9) . . ? C38 C39 C40 121.5(10) . . ? C35 C40 C39 122.1(9) . . ? C46 C41 C42 119.5(8) . . ? C46 C41 P2 123.6(6) . . ? C42 C41 P2 116.9(6) . . ? C43 C42 C41 119.1(10) . . ? C44 C43 C42 120.3(11) . . ? C45 C44 C43 121.3(10) . . ? C44 C45 C46 120.5(11) . . ? C41 C46 C45 119.2(10) . . ? C52 C47 C48 118.3(8) . . ? C52 C47 P2 119.6(7) . . ? C48 C47 P2 121.6(7) . . ? C49 C48 C47 121.2(9) . . ? C50 C49 C48 120.0(10) . . ? C49 C50 C51 120.7(10) . . ? C52 C51 C50 119.6(11) . . ? C51 C52 C47 120.1(10) . . ? C58 C53 C54 117.3(14) . . ? C58 C53 O2 124.3(13) . . ? C54 C53 O2 118.4(11) . . ? C55 C54 C53 121.3(11) . . ? C54 C55 C56 120.9(12) . . ? O1 C56 C57 119.0(13) . . ? O1 C56 C55 122.6(13) . . ? C57 C56 C55 118.4(14) . . ? C56 C57 C58 120.5(12) . . ? C53 C58 C57 121.5(14) . . ? F2 B1 F1 101.0(17) . . ? F2 B1 F3 118.8(18) . . ? F1 B1 F3 97.0(17) . . ? F2 B1 F4 119.2(14) . . ? F1 B1 F4 110.1(15) . . ? F3 B1 F4 107.8(11) . . ? F7 B2 F5 109.3(12) . . ? F7 B2 F6 110.4(11) . . ? F5 B2 F6 110.4(12) . . ? F7 B2 F8 107.7(11) . . ? F5 B2 F8 112.2(11) . . ? F6 B2 F8 106.7(11) . . ? C3 C2 H2 131.0 . . ? C1 C2 H2 109.1 . . ? Ru1 C2 H2 150.1 . . ? C2 C3 H3 123.6 . . ? C4 C3 H3 125.7 . . ? Ru1 C3 H3 109.3 . . ? C5 C4 H4 126.0 . . ? C3 C4 H4 121.9 . . ? Ru1 C4 H4 109.0 . . ? C4 C5 H5 125.6 . . ? C1 C5 H5 124.9 . . ? Ru1 C5 H5 109.0 . . ? C8 C7 H7 123.7 . . ? C6 C7 H7 125.4 . . ? Ru2 C7 H7 108.1 . . ? C7 C8 H8 126.6 . . ? C9 C8 H8 123.1 . . ? Ru2 C8 H8 108.1 . . ? C10 C9 H9 124.5 . . ? C8 C9 H9 124.1 . . ? Ru2 C9 H9 108.5 . . ? C9 C10 H10 125.3 . . ? C6 C10 H10 124.5 . . ? Ru2 C10 H10 109.1 . . ? C11 C12 H12 121.4 . . ? C13 C12 H12 119.7 . . ? C14 C13 H13 125.0 . . ? C12 C13 H13 114.8 . . ? C13 C14 H14 115.4 . . ? C15 C14 H14 121.2 . . ? C16 C15 H15 123.7 . . ? C14 C15 H15 120.9 . . ? C19 C18 H18 113.9 . . ? C17 C18 H18 123.3 . . ? C18 C19 H19 127.1 . . ? C20 C19 H19 113.5 . . ? C21 C20 H20 118.7 . . ? C19 C20 H20 122.2 . . ? C22 C21 H21 119.5 . . ? C20 C21 H21 118.4 . . ? C21 C22 H22 117.9 . . ? C17 C22 H22 123.4 . . ? C23 C24 H24 121.8 . . ? C25 C24 H24 118.4 . . ? C26 C25 H25 117.3 . . ? C24 C25 H25 122.9 . . ? C27 C26 H26 117.1 . . ? C25 C26 H26 123.5 . . ? C26 C27 H27 119.2 . . ? C28 C27 H27 118.8 . . ? C23 C28 H28 120.6 . . ? C27 C28 H28 119.5 . . ? C31 C30 H30 124.2 . . ? C29 C30 H30 116.9 . . ? C32 C31 H31 121.2 . . ? C30 C31 H31 117.6 . . ? C31 C32 H32 123.4 . . ? C33 C32 H32 115.8 . . ? C32 C33 H33 126.3 . . ? C34 C33 H33 115.1 . . ? C29 C34 H34 117.2 . . ? C33 C34 H34 121.3 . . ? C37 C36 H36 118.5 . . ? C35 C36 H36 120.5 . . ? C38 C37 H37 119.0 . . ? C36 C37 H37 119.9 . . ? C39 C38 H38 126.5 . . ? C37 C38 H38 115.6 . . ? C38 C39 H39 114.8 . . ? C40 C39 H39 123.6 . . ? C35 C40 H40 118.5 . . ? C39 C40 H40 119.4 . . ? C43 C42 H42 123.5 . . ? C41 C42 H42 117.4 . . ? C44 C43 H43 119.2 . . ? C42 C43 H43 120.4 . . ? C45 C44 H44 119.0 . . ? C43 C44 H44 119.6 . . ? C44 C45 H45 115.3 . . ? C46 C45 H45 124.2 . . ? C41 C46 H46 123.6 . . ? C45 C46 H46 117.2 . . ? C49 C48 H48 119.8 . . ? C47 C48 H48 118.8 . . ? C50 C49 H49 124.8 . . ? C48 C49 H49 115.2 . . ? C49 C50 H50 121.8 . . ? C51 C50 H50 117.5 . . ? C52 C51 H51 118.6 . . ? C50 C51 H51 121.8 . . ? C51 C52 H52 120.9 . . ? C47 C52 H52 119.0 . . ? C55 C54 H54 120.3 . . ? C53 C54 H54 118.4 . . ? C54 C55 H55 123.4 . . ? C56 C55 H55 115.6 . . ? C56 C57 H57 121.7 . . ? C58 C57 H57 117.8 . . ? C53 C58 H58 117.2 . . ? C57 C58 H58 120.9 . . ? _diffrn_measured_fraction_theta_max 0.832 _diffrn_reflns_theta_full 27.03 _diffrn_measured_fraction_theta_full 0.832 _refine_diff_density_max 3.526 _refine_diff_density_min -0.831 _refine_diff_density_rms 0.188 #=========END data_compound_6b _database_code_CSD 191664 _chemical_compound_source 'Local laboratory' _exptl_crystal_description Plate _exptl_crystal_colour Red _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.05 _cell_measurement_temperature 298 _refine_ls_hydrogen_treatment refxyz _diffrn_measurement_device 'DIP Image plate' _computing_data_collection 'DIP Image plate' _computing_data_reduction 'maXus (Mackay et al., 1999)' _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 loop_ _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_wavelength_id all _cell_formula_units_Z 2 _exptl_crystal_density_diffrn 1.531 _exptl_crystal_density_method 'not measured' _exptl_special_details ; ? ; _chemical_formula_weight 1005.108 _diffrn_radiation_type ' MoK¥a' loop_ _symmetry_equiv_pos_as_xyz +X,+Y,+Z -X,-Y,-Z _symmetry_space_group_name_H-M 'P -1 ' _symmetry_cell_setting Triclinic _chemical_formula_moiety 'C40 H50 F6 P2 Ru2 S3 ' _chemical_formula_sum 'C40 H50 F6 P2 Ru2 S3 ' _chemical_name_systematic ; ? ; _cell_length_a 10.8940(9) _cell_length_b 12.4920(10) _cell_length_c 17.162(2) _cell_angle_alpha 77.769(3) _cell_angle_beta 87.894(4) _cell_angle_gamma 72.83(4) _cell_volume 2180.0(4) _diffrn_reflns_number 11238 _diffrn_reflns_theta_max 27.09 _diffrn_reflns_theta_min 1.21 _diffrn_reflns_theta_full 27.09 _diffrn_reflns_av_R_equivalents 0.077 _computing_structure_solution 'DIRDIF (Buerskens et al., 1992)' _atom_sites_solution_primary vecmap _atom_sites_solution_secondary difmap _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_coefficient_mu 0.96 _exptl_crystal_F_000 1020 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 'Waasmaier & Kirfel, 1995' 'H ' 'H ' 0.0000 0.0000 'Waasmaier & Kirfel, 1995' 'F ' 'F ' 0.0171 0.0103 'Waasmaier & Kirfel, 1995' 'P ' 'P ' 0.1023 0.0942 'Waasmaier & Kirfel, 1995' Ru Ru -1.2594 0.8363 'Waasmaier & Kirfel, 1995' 'S ' 'S ' 0.1246 0.1234 'Waasmaier & Kirfel, 1995' # Refinement statistics _reflns_d_resolution_low 2.90 _reflns_d_resolution_high 0.62 _reflns_limit_h_max 13 _reflns_limit_h_min 0 _reflns_limit_k_max 15 _reflns_limit_k_min -14 _reflns_limit_l_max 21 _reflns_limit_l_min -21 _refine_ls_matrix_type full _refine_ls_shift/su_max 0.014 _refine_ls_shift/su_mean 0.006 _reflns_number_total 8775 _refine_ls_R_factor_all 0.142 _refine_ls_wR_factor_all 0.152 _refine_ls_goodness_of_fit_all 1.568 _reflns_number_gt 4105 _reflns_threshold_expression 'I> 3.00 sigma(I)' _refine_ls_R_factor_gt 0.081 _refine_ls_wR_factor_gt 0.135 _refine_ls_goodness_of_fit_gt 1.294 _refine_ls_number_reflns 4076 _refine_ls_number_parameters 478 _refine_ls_number_restraints 0 _refine_ls_number_constraints 50 _refine_ls_wR_factor_ref 0.135 _refine_ls_goodness_of_fit_ref 1.236 _refine_ls_structure_factor_coef F^2^ _refine_special_details ; Refinement on F^2^. ; _refine_ls_weighting_scheme sigma _refine_ls_weighting_details ; w = exp ( 5.00 sin(¥q)/¥l^2^ )/ s^2^(Fo^2^) + 0.00100 * Fo^2^ ; _refine_ls_extinction_method none _refine_ls_extinction_coef ? _computing_structure_refinement 'maXus(Mackay et al., 1999)' _computing_molecular_graphics 'Ortep (Johnson, 1976)' _computing_publication_material 'maXus(Mackay et al., 1999)' _atom_sites_solution_hydrogens geom _refine_diff_density_max 0.72 _refine_diff_density_min -1.08 _refine_diff_density_rms 0.22 #================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_adp_type Ru1 0.17130(13) 0.26168(8) 0.17344(7) 0.0524(6) 1.00 Uij Ru2 0.35038(14) 0.05831(10) 0.18818(8) 0.0669(7) 1.00 Uij S1 0.3399(4) 0.1844(3) 0.2725(2) 0.067(2) 1.00 Uij S2 0.1480(4) 0.0850(3) 0.2449(2) 0.0597(18) 1.00 Uij S3 0.5724(13) -0.1439(11) 0.2937(6) 0.218(10) 1.00 Uij P1 0.0410(4) 0.3678(3) 0.2601(2) 0.0538(18) 1.00 Uij P2 0.2839(6) 0.7025(4) 0.0348(3) 0.089(3) 1.00 Uij F1 0.3320(16) 0.5724(11) 0.0698(11) 0.146(10) 1.00 Uij F2 0.322(2) 0.7265(15) 0.1128(9) 0.168(14) 1.00 Uij F3 0.2410(18) 0.8328(11) 0.0019(10) 0.157(11) 1.00 Uij F4 0.237(2) 0.6803(16) -0.0396(11) 0.194(16) 1.00 Uij F5 0.4215(17) 0.6954(15) 0.0039(11) 0.158(13) 1.00 Uij F6 0.1491(18) 0.7042(18) 0.0696(15) 0.197(17) 1.00 Uij C1 0.2550(19) 0.2405(13) 0.0558(8) 0.069(9) 1.00 Uij C2 0.2669(18) 0.3442(11) 0.0719(8) 0.065(8) 1.00 Uij C3 0.1434(18) 0.4165(10) 0.0785(8) 0.062(7) 1.00 Uij C4 0.0544(18) 0.3643(11) 0.0655(9) 0.068(8) 1.00 Uij C5 0.120(2) 0.2553(13) 0.0516(9) 0.073(9) 1.00 Uij C6 0.353(2) 0.1329(13) 0.0627(10) 0.082(11) 1.00 Uij C7 0.477(2) 0.1110(16) 0.0933(13) 0.089(12) 1.00 Uij C8 0.525(2) -0.0072(18) 0.1211(13) 0.099(14) 1.00 Uij C9 0.434(2) -0.0621(14) 0.1075(12) 0.092(12) 1.00 Uij C10 0.327(2) 0.0231(17) 0.0684(12) 0.095(13) 1.00 Uij C11 -0.1009(16) 0.4762(11) 0.2086(9) 0.060(8) 1.00 Uij C12 -0.1926(19) 0.4394(14) 0.1793(10) 0.075(10) 1.00 Uij C13 -0.3011(18) 0.5189(16) 0.1379(11) 0.082(11) 1.00 Uij C14 -0.317(2) 0.6330(19) 0.1278(11) 0.099(13) 1.00 Uij C15 -0.225(3) 0.6715(15) 0.1557(12) 0.101(13) 1.00 Uij C16 -0.114(2) 0.5913(14) 0.1957(12) 0.088(11) 1.00 Uij C17 -0.0205(16) 0.2922(11) 0.3469(9) 0.059(8) 1.00 Uij C18 0.0657(19) 0.2061(12) 0.4001(10) 0.074(9) 1.00 Uij C19 0.023(2) 0.1522(15) 0.4690(10) 0.092(12) 1.00 Uij C20 -0.104(3) 0.1814(19) 0.4868(11) 0.101(15) 1.00 Uij C21 -0.190(2) 0.263(2) 0.4346(13) 0.106(15) 1.00 Uij C22 -0.1500(18) 0.3194(14) 0.3664(9) 0.074(10) 1.00 Uij C23 0.1159(16) 0.4550(10) 0.3044(8) 0.060(7) 1.00 Uij C24 0.093(2) 0.4721(14) 0.3813(11) 0.082(10) 1.00 Uij C25 0.139(3) 0.5447(18) 0.4104(13) 0.108(15) 1.00 Uij C26 0.209(3) 0.6011(16) 0.3672(12) 0.103(14) 1.00 Uij C27 0.239(3) 0.5896(19) 0.2900(15) 0.121(17) 1.00 Uij C28 0.186(2) 0.5170(14) 0.2593(10) 0.084(11) 1.00 Uij C29 0.478(2) 0.236(2) 0.2806(16) 0.113(16) 1.00 Uij C30 0.593(3) 0.138(3) 0.295(3) 0.20(3) 1.00 Uij C31 0.497(3) 0.326(3) 0.214(2) 0.16(3) 1.00 Uij C32 0.453(2) 0.291(2) 0.3544(17) 0.126(18) 1.00 Uij C33 0.028(2) 0.0178(14) 0.2149(12) 0.083(11) 1.00 Uij C34 -0.089(3) 0.082(6) 0.234(6) 0.52(8) 1.00 Uij C35 0.070(8) -0.095(5) 0.263(4) 0.43(8) 1.00 Uij C36 0.022(5) 0.007(5) 0.139(2) 0.27(5) 1.00 Uij C37 0.590(4) -0.279(3) 0.3772(18) 0.18(3) 1.00 Uij C38 0.749(5) -0.293(5) 0.390(3) 0.27(5) 1.00 Uij C39 0.519(9) -0.263(8) 0.443(2) 0.57(11) 1.00 Uij C40 0.586(6) -0.393(7) 0.351(5) 0.39(8) 1.00 Uij H2 0.350(6) 0.351(4) 0.091(3) 0.068700 1.00 Uiso H3 0.136514 0.484445 0.072831 0.062853 1.00 Uiso H4 -0.027864 0.392010 0.078908 0.067204 1.00 Uiso H5 0.081112 0.196445 0.056036 0.073105 1.00 Uiso H7 0.512431 0.165572 0.110880 0.091025 1.00 Uiso H8 0.594816 -0.042971 0.159312 0.098984 1.00 Uiso H9 0.435081 -0.138517 0.134271 0.093283 1.00 Uiso H10 0.244616 0.012898 0.064444 0.098108 1.00 Uiso H12 -0.177873 0.359212 0.186286 0.075113 1.00 Uiso H13 -0.357886 0.494494 0.116182 0.080474 1.00 Uiso H14 -0.375102 0.678831 0.107353 0.092592 1.00 Uiso H15 -0.204494 0.767627 0.145292 0.098074 1.00 Uiso H16 -0.039401 0.620615 0.213005 0.087767 1.00 Uiso H18 0.161282 0.180206 0.393572 0.074852 1.00 Uiso H19 0.084191 0.091873 0.506635 0.090253 1.00 Uiso H20 -0.132111 0.143773 0.533915 0.103728 1.00 Uiso H21 -0.273435 0.284813 0.445934 0.107072 1.00 Uiso H22 -0.204590 0.379775 0.331345 0.074885 1.00 Uiso H24 0.049626 0.431028 0.414380 0.083537 1.00 Uiso H25 0.128267 0.557321 0.463146 0.111683 1.00 Uiso H26 0.260543 0.646936 0.389954 0.107284 1.00 Uiso H27 0.299695 0.634463 0.259911 0.123146 1.00 Uiso H28 0.210055 0.507241 0.205417 0.088076 1.00 Uiso H30A 0.614655 0.105213 0.248778 0.194402 1.00 Uiso H30B 0.579375 0.083253 0.339018 0.194402 1.00 Uiso H30C 0.669475 0.160753 0.308508 0.194402 1.00 Uiso H31A 0.519578 0.292581 0.167440 0.169020 1.00 Uiso H31B 0.576418 0.348361 0.226200 0.169020 1.00 Uiso H31C 0.429878 0.392081 0.203260 0.169020 1.00 Uiso H32A 0.385993 0.356856 0.344319 0.127155 1.00 Uiso H32B 0.532242 0.312196 0.367559 0.127155 1.00 Uiso H32C 0.442043 0.234696 0.398139 0.127155 1.00 Uiso H38A 0.784302 -0.360482 0.430847 0.250814 1.00 Uiso H38B 0.763303 -0.228092 0.405037 0.250814 1.00 Uiso H38C 0.79(7) -0.30(6) 0.34(4) 0.250814 1.00 Uiso H40A 0.60(12) -0.45(9) 0.40(7) 0.386303 1.00 Uiso H40B 0.652299 -0.418550 0.314591 0.386303 1.00 Uiso H40C 0.50(10) -0.38(9) 0.33(6) 0.386303 1.00 Uiso H34A -0.154574 0.051593 0.219939 0.544464 1.00 Uiso H34B -0.107922 0.161220 0.207272 0.544464 1.00 Uiso H34C -0.09(7) 0.08(6) 0.29(4) 0.544464 1.00 Uiso H36A -0.043189 -0.027833 0.132071 0.281780 1.00 Uiso H36B 0.104844 -0.042794 0.129838 0.281780 1.00 Uiso H36C 0.006597 0.079074 0.102196 0.281780 1.00 Uiso H35A 0.015753 -0.138539 0.252000 0.429119 1.00 Uiso H35B 0.071085 -0.096184 0.318889 0.429119 1.00 Uiso H35C 0.155606 -0.127466 0.246394 0.429119 1.00 Uiso H39A 0.537612 -0.336196 0.479520 0.309209 1.00 Uiso H39B 0.430956 -0.239080 0.425265 0.309209 1.00 Uiso H39C 0.535481 -0.207880 0.468894 0.309209 1.00 Uiso loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ru1 0.0627(9) 0.0435(5) 0.0433(6) -.0148(5) 0.0031(5) -.0093(4) Ru2 0.0662(10) 0.0502(7) 0.0734(9) -.0094(6) 0.0143(7) -.0159(5) S1 0.060(3) 0.066(2) 0.065(2) -.0100(18) -.0030(19) -.0187(16) S2 0.062(3) 0.0476(16) 0.060(2) -.0144(15) 0.0121(18) -.0080(13) S3 0.210(12) 0.226(11) 0.134(8) 0.075(9) 0.007(7) 0.002(7) P1 0.059(3) 0.0454(17) 0.0486(19) -.0101(15) 0.0005(17) -.0108(13) P2 0.089(4) 0.080(3) 0.090(4) -.040(3) -.011(3) -.017(2) F1 0.133(14) 0.090(8) 0.193(16) -.042(8) 0.001(11) -.001(8) F2 0.206(19) 0.188(15) 0.094(10) -.079(13) -.016(11) -.040(9) F3 0.191(17) 0.087(8) 0.169(15) -.030(9) -.039(12) -.020(8) F4 0.22(2) 0.182(15) 0.159(15) -.033(14) -.065(14) -.101(13) F5 0.125(14) 0.176(14) 0.151(14) -.066(11) 0.042(11) -.009(11) F6 0.116(15) 0.201(18) 0.25(3) -.056(13) 0.013(15) -.058(17) C1 0.079(14) 0.083(10) 0.035(7) -.032(9) 0.022(8) -.014(6) C2 0.096(14) 0.048(7) 0.047(7) -.031(7) 0.036(8) -.019(5) C3 0.095(13) 0.039(6) 0.039(7) -.015(7) 0.000(7) 0.000(5) C4 0.088(14) 0.048(7) 0.051(8) -.008(7) 0.001(8) 0.001(5) C5 0.095(15) 0.066(9) 0.044(8) -.027(9) 0.003(8) 0.002(6) C6 0.111(18) 0.065(9) 0.062(10) -.033(10) 0.045(10) -.028(7) C7 0.074(15) 0.081(12) 0.102(15) -.017(10) 0.028(12) -.037(10) C8 0.083(17) 0.096(14) 0.103(15) -.018(12) 0.050(12) -.033(11) C9 0.105(18) 0.053(9) 0.106(15) -.020(10) 0.053(12) -.032(9) C10 0.094(17) 0.089(12) 0.098(14) -.046(11) 0.050(12) -.044(10) C11 0.062(10) 0.051(7) 0.055(8) 0.004(7) -.016(7) -.015(6) C12 0.080(13) 0.072(9) 0.059(9) -.008(9) 0.009(9) -.018(7) C13 0.067(13) 0.094(12) 0.066(11) -.003(10) -.020(9) -.010(8) C14 0.101(18) 0.101(14) 0.061(11) 0.031(13) -.006(11) -.015(9) C15 0.13(2) 0.059(9) 0.088(14) 0.014(11) -.028(14) -.020(9) C16 0.088(15) 0.063(9) 0.098(14) -.001(9) -.015(11) -.025(8) C17 0.060(11) 0.051(7) 0.060(9) -.022(7) -.001(8) -.011(5) C18 0.094(14) 0.053(8) 0.062(9) -.013(8) 0.016(9) -.010(6) C19 0.13(2) 0.075(11) 0.055(10) -.013(11) 0.013(11) -.008(7) C20 0.13(2) 0.117(15) 0.047(10) -.059(15) 0.026(12) -.024(9) C21 0.075(15) 0.16(2) 0.077(14) -.042(14) 0.008(12) -.032(13) C22 0.076(14) 0.084(10) 0.049(9) -.022(9) -.008(8) -.011(7) C23 0.082(12) 0.049(7) 0.041(7) -.019(7) -.003(7) -.011(5) C24 0.092(15) 0.076(10) 0.069(11) -.023(9) 0.012(10) -.027(8) C25 0.14(2) 0.091(13) 0.089(14) -.050(14) 0.015(14) -.046(11) C26 0.15(2) 0.083(12) 0.076(13) -.052(13) 0.007(13) -.037(9) C27 0.15(3) 0.102(15) 0.103(17) -.074(15) 0.004(16) -.010(12) C28 0.115(17) 0.074(10) 0.060(10) -.048(10) -.012(10) -.019(7) C29 0.081(17) 0.118(17) 0.13(2) -.027(14) 0.015(14) -.052(15) C30 0.060(17) 0.20(3) 0.32(5) -.014(19) -.03(2) -.14(3) C31 0.11(2) 0.23(3) 0.15(3) -.12(2) 0.03(2) -.07(2) C32 0.095(18) 0.130(19) 0.14(2) -.024(15) -.013(16) -.067(16) C33 0.085(15) 0.072(10) 0.087(13) -.037(9) 0.014(11) -.022(8) C34 0.09(2) 0.48(8) 1.04(17) -.09(4) 0.14(5) -.66(11) C35 0.55(11) 0.27(5) 0.43(9) -.34(7) -.29(8) 0.17(6) C36 0.31(6) 0.40(6) 0.13(3) -.29(5) 0.01(3) -.05(3) C37 0.17(3) 0.19(3) 0.09(2) 0.09(3) 0.006(19) 0.009(19) C38 0.21(5) 0.34(7) 0.18(5) 0.00(5) 0.00(4) 0.04(4) C39 0.70(15) 0.63(13) 0.07(2) 0.44(12) 0.00(5) -.01(4) C40 0.20(6) 0.43(10) 0.48(12) 0.07(6) 0.03(6) -.24(10) _geom_special_details ; All standard uncertainties (except dihedral angles between l.s. planes) are estimated using the full covariance matrix. The standard uncertainties in cell dimensions are are used in calculating the standard uncertainties of bond distances, angles and torsion angles. Angles between l.s. planes have standard uncertainties calculated from atomic positional standard uncertainties; the errors in cell dimensions are not used in this case. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 Ru2 2.6762(10) . . ? Ru1 S1 2.384(3) . . ? Ru1 S2 2.367(2) . . ? Ru1 P1 2.357(2) . . ? Ru1 C1 2.219(9) . . ? Ru1 C2 2.220(9) . . ? Ru1 C3 2.201(8) . . ? Ru1 C4 2.213(10) . . ? Ru1 C5 2.209(11) . . ? Ru2 S1 2.332(3) . . ? Ru2 S2 2.338(3) . . ? Ru2 C6 2.161(11) . . ? Ru2 C7 2.213(14) . . ? Ru2 C8 2.220(12) . . ? Ru2 C9 2.234(11) . . ? Ru2 C10 2.228(14) . . ? S1 C29 1.83(2) . . ? S2 C33 1.883(13) . . ? S3 C37 1.94(2) . . ? P1 C11 1.834(9) . . ? P1 C17 1.806(11) . . ? P1 C23 1.831(10) . . ? P2 F1 1.545(9) . . ? P2 F2 1.528(10) . . ? P2 F3 1.538(9) . . ? P2 F4 1.501(10) . . ? P2 F5 1.555(12) . . ? P2 F6 1.562(14) . . ? C1 C2 1.423(14) . . ? C1 C5 1.43(2) . . ? C1 C6 1.44(2) . . ? C2 C3 1.40(2) . . ? C3 C4 1.37(2) . . ? C4 C5 1.404(14) . . ? C6 C7 1.39(2) . . ? C6 C10 1.46(2) . . ? C7 C8 1.39(2) . . ? C8 C9 1.41(2) . . ? C9 C10 1.40(2) . . ? C11 C12 1.37(2) . . ? C11 C16 1.373(15) . . ? C12 C13 1.40(2) . . ? C13 C14 1.36(2) . . ? C14 C15 1.36(2) . . ? C15 C16 1.42(2) . . ? C17 C18 1.387(14) . . ? C17 C22 1.40(2) . . ? C18 C19 1.37(2) . . ? C19 C20 1.36(2) . . ? C20 C21 1.35(2) . . ? C21 C22 1.36(2) . . ? C23 C24 1.383(14) . . ? C23 C28 1.35(2) . . ? C24 C25 1.35(2) . . ? C25 C26 1.30(2) . . ? C26 C27 1.38(2) . . ? C27 C28 1.40(2) . . ? C29 C30 1.45(2) . . ? C29 C31 1.48(3) . . ? C29 C32 1.54(2) . . ? C33 C34 1.36(2) . . ? C33 C35 1.42(3) . . ? C33 C36 1.34(3) . . ? C37 C38 1.71(5) . . ? C37 C39 1.36(4) . . ? C37 C40 1.60(6) . . ? 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Ru2 Ru1 S1 54.50(7) . . . ? Ru2 Ru1 S2 54.82(7) . . . ? Ru2 Ru1 P1 136.40(7) . . . ? Ru2 Ru1 C1 69.9(3) . . . ? Ru2 Ru1 C2 93.2(3) . . . ? Ru2 Ru1 C3 129.1(3) . . . ? Ru2 Ru1 C4 127.4(3) . . . ? Ru2 Ru1 C5 90.8(3) . . . ? S1 Ru1 S2 73.04(10) . . . ? S1 Ru1 P1 90.49(9) . . . ? S1 Ru1 C1 108.4(3) . . . ? S1 Ru1 C2 102.1(3) . . . ? S1 Ru1 C3 127.1(3) . . . ? S1 Ru1 C4 162.5(3) . . . ? S1 Ru1 C5 142.4(3) . . . ? S2 Ru1 P1 93.55(9) . . . ? S2 Ru1 C1 109.6(3) . . . ? S2 Ru1 C2 144.7(2) . . . ? S2 Ru1 C3 159.3(3) . . . ? S2 Ru1 C4 123.4(3) . . . ? S2 Ru1 C5 100.1(3) . . . ? P1 Ru1 C1 153.4(3) . . . ? P1 Ru1 C2 121.7(2) . . . ? P1 Ru1 C3 91.5(3) . . . ? P1 Ru1 C4 94.1(3) . . . ? P1 Ru1 C5 127.1(3) . . . ? C1 Ru1 C2 37.4(4) . . . ? C1 Ru1 C3 62.2(4) . . . ? C1 Ru1 C4 62.5(4) . . . ? C1 Ru1 C5 37.8(4) . . . ? C2 Ru1 C3 36.9(4) . . . ? C2 Ru1 C4 61.3(5) . . . ? C2 Ru1 C5 61.9(4) . . . ? C3 Ru1 C4 36.0(4) . . . ? C3 Ru1 C5 61.3(4) . . . ? C4 Ru1 C5 37.0(4) . . . ? Ru1 Ru2 S1 56.36(7) . . . ? Ru1 Ru2 S2 55.84(6) . . . ? Ru1 Ru2 C6 77.2(3) . . . ? Ru1 Ru2 C7 97.3(3) . . . ? Ru1 Ru2 C8 133.8(4) . . . ? Ru1 Ru2 C9 135.6(4) . . . ? Ru1 Ru2 C10 99.4(4) . . . ? S1 Ru2 S2 74.53(10) . . . ? S1 Ru2 C6 114.5(3) . . . ? S1 Ru2 C7 102.6(3) . . . ? S1 Ru2 C8 122.6(5) . . . ? S1 Ru2 C9 159.3(5) . . . ? S1 Ru2 C10 151.5(4) . . . ? S2 Ru2 C6 116.4(4) . . . ? S2 Ru2 C7 150.2(4) . . . ? S2 Ru2 C8 162.6(5) . . . ? S2 Ru2 C9 125.8(4) . . . ? S2 Ru2 C10 105.7(4) . . . ? C6 Ru2 C7 37.0(5) . . . ? C6 Ru2 C8 61.5(5) . . . ? C6 Ru2 C9 63.1(4) . . . ? C6 Ru2 C10 38.9(5) . . . ? C7 Ru2 C8 36.7(5) . . . ? C7 Ru2 C9 62.4(5) . . . ? C7 Ru2 C10 62.7(5) . . . ? C8 Ru2 C9 36.9(5) . . . ? C8 Ru2 C10 61.0(6) . . . ? C9 Ru2 C10 36.5(5) . . . ? Ru1 S1 Ru2 69.14(8) . . . ? Ru1 S1 C29 126.8(6) . . . ? Ru2 S1 C29 118.7(5) . . . ? Ru1 S2 Ru2 69.34(8) . . . ? Ru1 S2 C33 123.1(4) . . . ? Ru2 S2 C33 121.5(4) . . . ? Ru1 P1 C11 112.3(3) . . . ? Ru1 P1 C17 118.9(3) . . . ? Ru1 P1 C23 115.2(4) . . . ? F1 P2 F2 90.1(7) . . . ? F1 P2 F3 177.4(7) . . . ? F1 P2 F4 90.3(7) . . . ? F1 P2 F5 88.2(6) . . . ? F1 P2 F6 89.1(7) . . . ? F2 P2 F3 87.8(6) . . . ? F2 P2 F4 175.7(9) . . . ? F2 P2 F5 89.7(7) . . . ? F2 P2 F6 88.7(8) . . . ? F3 P2 F4 91.9(7) . . . ? F3 P2 F5 90.2(7) . . . ? F3 P2 F6 92.4(7) . . . ? F4 P2 F5 94.6(8) . . . ? F4 P2 F6 87.0(8) . . . ? F5 P2 F6 176.8(8) . . . ? Ru1 C1 C2 71.3(5) . . . ? Ru1 C1 C5 70.7(6) . . . ? Ru1 C1 C6 111.0(7) . . . ? C2 C1 C5 105.7(10) . . . ? C2 C1 C6 127.6(13) . . . ? C5 C1 C6 124.9(11) . . . ? Ru1 C2 C1 71.3(5) . . . ? Ru1 C2 C3 70.8(6) . . . ? C1 C2 C3 108.1(11) . . . ? Ru1 C3 C2 72.3(5) . . . ? Ru1 C3 C4 72.5(5) . . . ? C2 C3 C4 109.6(8) . . . ? Ru1 C4 C3 71.5(6) . . . ? Ru1 C4 C5 71.3(6) . . . ? C3 C4 C5 108.4(11) . . . ? Ru1 C5 C1 71.5(6) . . . ? Ru1 C5 C4 71.7(6) . . . ? C1 C5 C4 108.2(10) . . . ? Ru2 C6 C1 101.9(6) . . . ? Ru2 C6 C7 73.5(8) . . . ? Ru2 C6 C10 73.0(7) . . . ? C1 C6 C7 124.2(11) . . . ? C1 C6 C10 123.9(15) . . . ? C7 C6 C10 108.2(12) . . . ? Ru2 C7 C6 69.5(8) . . . ? Ru2 C7 C8 71.9(8) . . . ? C6 C7 C8 107.2(13) . . . ? Ru2 C8 C7 71.4(7) . . . ? Ru2 C8 C9 72.1(7) . . . ? C7 C8 C9 110.5(14) . . . ? Ru2 C9 C8 71.0(7) . . . ? Ru2 C9 C10 71.5(6) . . . ? C8 C9 C10 107.0(11) . . . ? Ru2 C10 C6 68.1(7) . . . ? Ru2 C10 C9 71.9(8) . . . ? C6 C10 C9 106.9(14) . . . ? P1 C11 C12 118.1(7) . . . ? P1 C11 C16 121.8(9) . . . ? C12 C11 C16 120.0(9) . . . ? C11 C12 C13 120.1(11) . . . ? C12 C13 C14 120.1(13) . . . ? C13 C14 C15 120.7(11) . . . ? C14 C15 C16 119.4(12) . . . ? C11 C16 C15 119.6(13) . . . ? P1 C17 C18 118.7(9) . . . ? P1 C17 C22 123.9(8) . . . ? C18 C17 C22 117.3(10) . . . ? C17 C18 C19 120.1(12) . . . ? C18 C19 C20 121.2(12) . . . ? C19 C20 C21 119.6(13) . . . ? C20 C21 C22 120.4(14) . . . ? C17 C22 C21 121.2(11) . . . ? P1 C23 C24 122.8(9) . . . ? P1 C23 C28 120.3(7) . . . ? C24 C23 C28 116.5(10) . . . ? C23 C24 C25 122.0(13) . . . ? C24 C25 C26 120.9(13) . . . ? C25 C26 C27 121.6(13) . . . ? C26 C27 C28 117.0(14) . . . ? C23 C28 C27 121.9(12) . . . ? S1 C29 C30 108.7(14) . . . ? S1 C29 C31 117.1(14) . . . ? S1 C29 C32 104.6(12) . . . ? C30 C29 C31 110.(2) . . . ? C30 C29 C32 110.(2) . . . ? C31 C29 C32 106.2(15) . . . ? S2 C33 C34 105.8(12) . . . ? S2 C33 C35 102.0(14) . . . ? S2 C33 C36 119.6(14) . . . ? C34 C33 C35 114.(4) . . . ? C34 C33 C36 109.(3) . . . ? C35 C33 C36 107.(3) . . . ? S3 C37 C38 90.(2) . . . ? S3 C37 C39 116.(3) . . . ? S3 C37 C40 117.(3) . . . ? C38 C37 C39 114.(4) . . . ? C38 C37 C40 106.(2) . . . ? C39 C37 C40 111.(5) . . . ? #===================================================