Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 186 # 1. SUBMISSION DETAILS _publ_contact_letter ; Please consider this CIF submission for publication in the Dalton Transactions ; _publ_contact_author 'Dr Esther Delgado' _publ_contact_author_address ; Departamento de Quimica Inorganica (C-8) Facultad de Ciencias Universidad Autonoma de Madrid 28049 Madrid, Spain ; _publ_contact_author_fax ' (34) 913974833 ' _publ_contact_author_email ' esther.delgado@uam.es ' _publ_requested_journal 'Dalton Transactions.' #=========================================================================== # 2. TITLE AND AUTHOR LIST _publ_section_title ; Syntheses of new ruthenium clusters containing sulfur, ynyl and diynyl ligands. Crystal structures of [Ru3(CO)9(m-SCēCSiMe3)(m3,h2-CēCSiMe3)], [Ru4(CO)12(m4-S)(m2,h2-CēCSiMe3)2] and [Ru4(CO)9(m-CO)2(m4-S)(m4,h2-C(SiMe3)C(CēCSiMe3)], ref. B103202J ; loop_ _publ_author_name _publ_author_address ' M. I. Alcade' ; Departamento de Quimica Inorganica (C-8) Facultad de Ciencias Universidad Autonoma de Madrid 28049 Madrid, Spain ; 'E. Delgado' ; Departamento de Quimica Inorganica (C-8) Facultad de Ciencias Universidad Autonoma de Madrid 28049 Madrid, Spain ; 'E. Hernandez' ; Departamento de Quimica Inorganica (C-8) Facultad de Ciencias Universidad Autonoma de Madrid 28049 Madrid, Spain ; 'J. Sanchez-Nieves' ; Departamento de Quimica Inorganica (C-8) Facultad de Ciencias Universidad Autonoma de Madrid 28049 Madrid, Spain ; 'K.Dallmann' ; ? ; 'A. J. Carty ' ; Insitute for Molecular Sciences, National Research Council of Canada, 100 Sussex Drive, Ottawa, Ontario K1 OR6, Canada ' ; 'Y. Chi' ; Department of Chemistry, National Tsing Hua University, Hsinchu 30043, Taiwan ; 'B. Donnadieu' ; Laboratoire de Chimie de Coordination UPR-CNRS 8241 205, route de Narbonne 31077 Toulouse cedex, France ; #=========================================================================== _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo, G., Guagliardi, A., Burla, M.C., Polidori, G. and Camalli, M. (1994)., SIR92 program for automatic solution of crystal structures by direct methods. J. Appl. Cryst. 27, 435. Farrugia, L. J., ORTEP3 for Windows, J. Appl. Crystallogr. 1997, 30, 565. Flack H D (1983), Acta Cryst. A39, 876-881 Sheldrick, G. M. (1997). SHELXL97. Program for the refinement of Crystal Structures. University of Göttingen, Germany. Stoe, IPDS Manual. Version 2.75. Stoe & Cie, Darmstadt,1996, Germany. Stoe, X-RED, Data Reduction for STADI4 and IPDS, Revision 1.08. Stoe & Cie, Darmstadt, 1996, Germany. Stoe, FACEIT: Numerical Absorption Correction, Manual. Version 2.75. Stoe & Cie, Darmstadt, 1996, Germany. X-SHAPE (revision 1.01) July 1996. A Crystal Optimisation For numerical Correction STOE and Cie. Zsolnai, L (1997) ZORTEP Molecular Graphics, University of Heidelberg, Germany. ; #**************************************************************************** data_(1) _database_code_CSD 162095 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C19 H18 O9 Ru3 S Si2' _chemical_formula_weight 781.78 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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Si' 'Si' 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ru' 'Ru' -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'Orthorhombic ' _symmetry_space_group_name_H-M 'P 21 21 21 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x+1/2, -y, z+1/2' _cell_length_a 9.5045(12) _cell_length_b 16.499(2) _cell_length_c 18.014(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2824.8(6) _cell_formula_units_Z 4 _cell_measurement_temperature 160(2) _cell_measurement_reflns_used 5000 _cell_measurement_theta_min 2.15 _cell_measurement_theta_max 26.0 _exptl_crystal_description parallelepiped _exptl_crystal_colour 'light yellow ' _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.838 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1520 _exptl_absorpt_coefficient_mu 1.783 _exptl_absorpt_correction_type 'numerical' _exptl_absorpt_correction_T_min 0.601 _exptl_absorpt_correction_T_max 0.801 _exptl_special_details ; The data were collected on a Stoe Imaging Plate Diffraction System (IPDS). The crystal-to-detector distance was 70 mm. 313 frames (2 min per frame) were obtained with 0 < \f < 250.4\% and with the crystals rotated through 0.8\% in \f. Coverage of the unique set was over 98.2% complete to at least 25.93\%. Crystal decay was monitored by measuring 200 reflexions per frame. ; _diffrn_ambient_temperature 160(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Stoe IPDS' _diffrn_measurement_method \f _diffrn_standards_number 200 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 'every frame' _diffrn_standards_decay_% <0.1 _diffrn_reflns_number 27385 _diffrn_reflns_av_R_equivalents 0.0310 _diffrn_reflns_av_sigmaI/netI 0.0159 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.42 _diffrn_reflns_theta_max 25.93 _reflns_number_total 5417 _reflns_number_gt 5364 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Stoe IPDS software (Stoe, 1996)' _computing_data_reduction 'XRED (Stoe, 1.08, 1996)' _computing_cell_refinement 'Stoe IPDS software (Stoe, 1996)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP3 for Windows (Farrugia, 1997)' _computing_structure_solution 'SIR92 (Giacovazzo et al, 1992)' _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^)+(0.0282P)^2^+0.6692P] where P==(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.021(19) _refine_ls_number_reflns 5417 _refine_ls_number_parameters 313 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0169 _refine_ls_R_factor_gt 0.0166 _refine_ls_wR_factor_ref 0.0426 _refine_ls_wR_factor_gt 0.0424 _refine_ls_goodness_of_fit_ref 1.080 _refine_ls_restrained_S_all 1.080 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.642449(17) 0.104267(11) 0.743385(9) 0.02278(5) Uani 1 1 d . . . Ru2 Ru 0.622144(18) 0.167921(12) 0.889458(10) 0.02517(5) Uani 1 1 d . . . Ru3 Ru 0.909532(17) 0.167196(11) 0.850325(9) 0.02027(5) Uani 1 1 d . . . S1 S 0.81372(6) 0.21348(3) 0.73249(3) 0.02327(11) Uani 1 1 d . . . Si1A Si 0.92889(8) -0.05128(4) 0.79192(4) 0.03544(16) Uani 1 1 d . . . Si1B Si 1.11481(9) 0.14411(6) 0.53265(4) 0.0447(2) Uani 1 1 d . . . O11 O 0.4335(2) 0.22637(15) 0.68263(13) 0.0529(6) Uani 1 1 d . . . O12 O 0.4152(2) -0.01942(14) 0.77734(13) 0.0503(5) Uani 1 1 d . . . O13 O 0.7177(3) 0.02479(16) 0.59361(13) 0.0600(7) Uani 1 1 d . . . O21 O 0.33255(19) 0.10032(15) 0.92747(12) 0.0479(5) Uani 1 1 d . . . O22 O 0.5277(3) 0.33824(15) 0.84273(14) 0.0628(7) Uani 1 1 d . . . O23 O 0.7121(2) 0.20453(16) 1.04798(11) 0.0534(6) Uani 1 1 d . . . O31 O 0.9062(3) 0.33836(12) 0.91278(12) 0.0476(5) Uani 1 1 d . . . O32 O 1.0065(2) 0.10029(14) 0.99892(11) 0.0450(5) Uani 1 1 d . . . O33 O 1.20711(18) 0.15767(14) 0.78493(12) 0.0443(5) Uani 1 1 d . . . C1 C 0.7341(2) 0.07644(14) 0.85532(13) 0.0233(4) Uani 1 1 d . . . C2 C 0.8215(2) 0.04021(13) 0.81176(13) 0.0248(4) Uani 1 1 d . . . C3 C 0.9271(2) 0.18542(14) 0.66412(13) 0.0261(5) Uani 1 1 d . . . C4 C 1.0031(3) 0.16937(17) 0.61291(14) 0.0326(5) Uani 1 1 d . . . C1A C 1.0311(5) -0.0751(2) 0.8771(2) 0.0746(13) Uani 1 1 d . . . H1A1 H 0.9662 -0.0839 0.9187 0.112 Uiso 1 1 calc R . . H1A2 H 1.0940 -0.0298 0.8887 0.112 Uiso 1 1 calc R . . H1A3 H 1.0868 -0.1243 0.8689 0.112 Uiso 1 1 calc R . . C2A C 1.0523(4) -0.0285(2) 0.7146(3) 0.0672(11) Uani 1 1 d . . . H2A1 H 1.1188 -0.0735 0.7089 0.101 Uiso 1 1 calc R . . H2A2 H 1.1042 0.0214 0.7258 0.101 Uiso 1 1 calc R . . H2A3 H 0.9991 -0.0214 0.6685 0.101 Uiso 1 1 calc R . . C3A C 0.8078(4) -0.13436(19) 0.7668(3) 0.0651(10) Uani 1 1 d . . . H3A1 H 0.7310 -0.1370 0.8030 0.098 Uiso 1 1 calc R . . H3A2 H 0.8591 -0.1859 0.7667 0.098 Uiso 1 1 calc R . . H3A3 H 0.7690 -0.1243 0.7172 0.098 Uiso 1 1 calc R . . C1B C 1.1853(7) 0.2413(3) 0.4966(3) 0.107(2) Uani 1 1 d . . . H1B1 H 1.2408 0.2310 0.4517 0.160 Uiso 1 1 calc R . . H1B2 H 1.2453 0.2665 0.5343 0.160 Uiso 1 1 calc R . . H1B3 H 1.1072 0.2777 0.4847 0.160 Uiso 1 1 calc R . . C2B C 1.2571(4) 0.0742(3) 0.5638(2) 0.0742(12) Uani 1 1 d . . . H2B1 H 1.3262 0.0677 0.5239 0.111 Uiso 1 1 calc R . . H2B2 H 1.2164 0.0213 0.5762 0.111 Uiso 1 1 calc R . . H2B3 H 1.3035 0.0969 0.6077 0.111 Uiso 1 1 calc R . . C3B C 1.0032(5) 0.0939(3) 0.4618(2) 0.0778(13) Uani 1 1 d . . . H3B1 H 1.0604 0.0808 0.4182 0.117 Uiso 1 1 calc R . . H3B2 H 0.9267 0.1305 0.4474 0.117 Uiso 1 1 calc R . . H3B3 H 0.9635 0.0440 0.4826 0.117 Uiso 1 1 calc R . . C11 C 0.5078(3) 0.17971(18) 0.70653(14) 0.0342(6) Uani 1 1 d . . . C12 C 0.5011(3) 0.02598(16) 0.76449(14) 0.0333(5) Uani 1 1 d . . . C13 C 0.6924(3) 0.05438(18) 0.64892(15) 0.0364(6) Uani 1 1 d . . . C21 C 0.4387(3) 0.12669(18) 0.91245(14) 0.0355(6) Uani 1 1 d . . . C22 C 0.5604(3) 0.27644(19) 0.86248(14) 0.0399(6) Uani 1 1 d . . . C23 C 0.6747(3) 0.19114(18) 0.98939(15) 0.0370(6) Uani 1 1 d . . . C31 C 0.9077(3) 0.27466(16) 0.88829(13) 0.0325(5) Uani 1 1 d . . . C32 C 0.9697(3) 0.12582(15) 0.94338(14) 0.0286(5) Uani 1 1 d . . . C33 C 1.0975(2) 0.15929(15) 0.80899(14) 0.0285(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.01935(8) 0.02904(9) 0.01997(9) -0.00222(7) -0.00133(7) 0.00008(6) Ru2 0.02277(9) 0.03303(10) 0.01971(9) -0.00202(7) 0.00252(6) 0.00419(7) Ru3 0.02069(8) 0.02114(8) 0.01900(8) -0.00158(7) -0.00137(6) -0.00042(7) S1 0.0250(2) 0.0243(3) 0.0205(2) 0.0003(2) 0.0004(2) 0.0025(2) Si1A 0.0374(4) 0.0230(3) 0.0459(4) -0.0081(3) -0.0091(3) 0.0063(3) Si1B 0.0459(4) 0.0590(5) 0.0291(4) -0.0090(3) 0.0148(3) -0.0052(4) O11 0.0381(11) 0.0673(15) 0.0533(13) 0.0179(12) -0.0039(10) 0.0202(10) O12 0.0431(11) 0.0583(13) 0.0496(12) 0.0001(10) 0.0014(10) -0.0253(10) O13 0.0666(15) 0.0758(17) 0.0377(12) -0.0287(12) 0.0087(11) -0.0118(13) O21 0.0238(9) 0.0752(15) 0.0447(11) 0.0032(11) 0.0053(8) -0.0040(10) O22 0.0927(18) 0.0465(13) 0.0494(13) 0.0034(11) 0.0016(13) 0.0303(14) O23 0.0454(11) 0.0869(17) 0.0280(10) -0.0150(11) -0.0035(9) 0.0031(11) O31 0.0763(14) 0.0264(10) 0.0402(10) -0.0090(8) -0.0159(10) 0.0030(11) O32 0.0514(12) 0.0555(12) 0.0282(9) 0.0051(9) -0.0101(9) 0.0074(10) O33 0.0235(9) 0.0598(13) 0.0497(12) 0.0132(11) 0.0059(8) 0.0006(9) C1 0.0213(10) 0.0261(11) 0.0225(10) 0.0019(9) -0.0025(8) -0.0053(8) C2 0.0250(11) 0.0224(10) 0.0269(11) 0.0006(9) -0.0032(9) -0.0006(8) C3 0.0273(11) 0.0283(12) 0.0228(11) 0.0024(9) -0.0022(9) -0.0023(9) C4 0.0323(12) 0.0399(13) 0.0257(12) -0.0038(11) 0.0036(10) -0.0049(11) C1A 0.095(3) 0.0461(19) 0.083(3) -0.0098(19) -0.047(2) 0.0311(19) C2A 0.058(2) 0.054(2) 0.089(3) -0.029(2) 0.028(2) 0.0067(16) C3A 0.067(2) 0.0301(15) 0.098(3) -0.0120(17) -0.016(2) -0.0077(14) C1B 0.133(5) 0.088(3) 0.099(3) 0.004(3) 0.086(3) -0.023(3) C2B 0.053(2) 0.113(4) 0.057(2) -0.014(2) 0.0192(17) 0.017(2) C3B 0.083(3) 0.106(4) 0.0446(19) -0.035(2) 0.0009(19) 0.011(3) C11 0.0239(11) 0.0496(16) 0.0293(12) 0.0030(12) 0.0022(10) -0.0004(11) C12 0.0294(12) 0.0424(14) 0.0280(12) -0.0051(11) -0.0044(10) -0.0007(11) C13 0.0311(12) 0.0438(15) 0.0342(14) -0.0068(12) -0.0020(11) -0.0062(11) C21 0.0328(14) 0.0488(16) 0.0249(12) -0.0006(11) 0.0001(10) 0.0090(11) C22 0.0448(15) 0.0478(17) 0.0270(12) -0.0058(12) 0.0049(11) 0.0127(13) C23 0.0288(12) 0.0501(16) 0.0320(14) -0.0047(12) 0.0037(10) 0.0060(11) C31 0.0423(13) 0.0318(13) 0.0234(11) 0.0022(10) -0.0068(10) -0.0007(11) C32 0.0265(11) 0.0304(12) 0.0288(12) -0.0049(10) 0.0012(9) -0.0018(9) C33 0.0263(11) 0.0311(12) 0.0280(11) 0.0042(10) -0.0039(9) -0.0005(10) _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 C12 1.901(3) . ? Ru1 C11 1.906(3) . ? Ru1 C13 1.949(3) . ? Ru1 C1 2.245(2) . ? Ru1 C2 2.353(2) . ? Ru1 S1 2.4353(7) . ? Ru1 Ru2 2.8397(5) . ? Ru2 C23 1.908(3) . ? Ru2 C21 1.916(3) . ? Ru2 C22 1.946(3) . ? Ru2 C1 1.947(2) . ? Ru2 Ru3 2.8204(5) . ? Ru3 C32 1.899(3) . ? Ru3 C31 1.900(3) . ? Ru3 C33 1.939(2) . ? Ru3 C1 2.242(2) . ? Ru3 C2 2.360(2) . ? Ru3 S1 2.4337(7) . ? S1 C3 1.700(2) . ? Si1A C3A 1.846(3) . ? Si1A C2 1.857(2) . ? Si1A C2A 1.858(4) . ? Si1A C1A 1.860(4) . ? Si1B C4 1.841(3) . ? Si1B C1B 1.854(5) . ? Si1B C3B 1.855(4) . ? Si1B C2B 1.865(4) . ? O11 C11 1.130(3) . ? O12 C12 1.132(3) . ? O13 C13 1.135(3) . ? O21 C21 1.131(3) . ? O22 C22 1.124(4) . ? O23 C23 1.136(3) . ? O31 C31 1.140(3) . ? O32 C32 1.141(3) . ? O33 C33 1.129(3) . ? C1 C2 1.289(3) . ? C3 C4 1.201(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C12 Ru1 C11 92.22(12) . . ? C12 Ru1 C13 93.40(11) . . ? C11 Ru1 C13 97.76(12) . . ? C12 Ru1 C1 87.48(9) . . ? C11 Ru1 C1 135.08(10) . . ? C13 Ru1 C1 127.12(10) . . ? C12 Ru1 C2 95.82(10) . . ? C11 Ru1 C2 164.26(10) . . ? C13 Ru1 C2 95.25(10) . . ? C1 Ru1 C2 32.46(8) . . ? C12 Ru1 S1 172.02(8) . . ? C11 Ru1 S1 86.42(8) . . ? C13 Ru1 S1 94.58(8) . . ? C1 Ru1 S1 87.93(6) . . ? C2 Ru1 S1 83.74(6) . . ? C12 Ru1 Ru2 91.05(8) . . ? C11 Ru1 Ru2 92.06(8) . . ? C13 Ru1 Ru2 169.05(8) . . ? C1 Ru1 Ru2 43.07(6) . . ? C2 Ru1 Ru2 74.33(6) . . ? S1 Ru1 Ru2 81.14(2) . . ? C23 Ru2 C21 96.09(12) . . ? C23 Ru2 C22 97.48(12) . . ? C21 Ru2 C22 96.07(13) . . ? C23 Ru2 C1 108.07(11) . . ? C21 Ru2 C1 106.89(11) . . ? C22 Ru2 C1 143.10(11) . . ? C23 Ru2 Ru3 88.99(8) . . ? C21 Ru2 Ru3 158.94(9) . . ? C22 Ru2 Ru3 103.54(9) . . ? C1 Ru2 Ru3 52.28(6) . . ? C23 Ru2 Ru1 158.61(8) . . ? C21 Ru2 Ru1 97.49(8) . . ? C22 Ru2 Ru1 97.42(8) . . ? C1 Ru2 Ru1 51.95(7) . . ? Ru3 Ru2 Ru1 72.637(16) . . ? C32 Ru3 C31 91.18(11) . . ? C32 Ru3 C33 92.11(10) . . ? C31 Ru3 C33 102.11(12) . . ? C32 Ru3 C1 87.07(10) . . ? C31 Ru3 C1 126.98(11) . . ? C33 Ru3 C1 130.91(10) . . ? C32 Ru3 C2 92.73(9) . . ? C31 Ru3 C2 158.55(10) . . ? C33 Ru3 C2 98.82(9) . . ? C1 Ru3 C2 32.41(8) . . ? C32 Ru3 S1 175.01(8) . . ? C31 Ru3 S1 91.01(8) . . ? C33 Ru3 S1 91.81(7) . . ? C1 Ru3 S1 88.04(6) . . ? C2 Ru3 S1 83.62(6) . . ? C32 Ru3 Ru2 94.20(7) . . ? C31 Ru3 Ru2 84.08(9) . . ? C33 Ru3 Ru2 171.08(7) . . ? C1 Ru3 Ru2 43.38(6) . . ? C2 Ru3 Ru2 74.60(6) . . ? S1 Ru3 Ru2 81.57(2) . . ? C3 S1 Ru3 107.97(8) . . ? C3 S1 Ru1 106.26(8) . . ? Ru3 S1 Ru1 87.02(2) . . ? C3A Si1A C2 107.94(14) . . ? C3A Si1A C2A 111.1(2) . . ? C2 Si1A C2A 109.06(15) . . ? C3A Si1A C1A 111.8(2) . . ? C2 Si1A C1A 107.50(15) . . ? C2A Si1A C1A 109.4(2) . . ? C4 Si1B C1B 106.69(18) . . ? C4 Si1B C3B 108.14(16) . . ? C1B Si1B C3B 110.6(3) . . ? C4 Si1B C2B 108.78(15) . . ? C1B Si1B C2B 112.2(3) . . ? C3B Si1B C2B 110.3(2) . . ? C2 C1 Ru2 154.67(19) . . ? C2 C1 Ru3 78.84(14) . . ? Ru2 C1 Ru3 84.33(9) . . ? C2 C1 Ru1 78.39(15) . . ? Ru2 C1 Ru1 84.98(9) . . ? Ru3 C1 Ru1 96.69(9) . . ? C1 C2 Si1A 147.99(19) . . ? C1 C2 Ru1 69.14(14) . . ? Si1A C2 Ru1 131.48(12) . . ? C1 C2 Ru3 68.75(13) . . ? Si1A C2 Ru3 125.70(11) . . ? Ru1 C2 Ru3 90.68(8) . . ? C4 C3 S1 175.7(2) . . ? C3 C4 Si1B 178.3(2) . . ? O11 C11 Ru1 176.4(2) . . ? O12 C12 Ru1 178.7(3) . . ? O13 C13 Ru1 178.1(3) . . ? O21 C21 Ru2 177.6(3) . . ? O22 C22 Ru2 175.9(2) . . ? O23 C23 Ru2 176.9(2) . . ? O31 C31 Ru3 178.3(2) . . ? O32 C32 Ru3 179.3(2) . . ? O33 C33 Ru3 177.5(2) . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 25.93 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 0.409 _refine_diff_density_min -0.346 _refine_diff_density_rms 0.065 #========END #=========================================================================== data_(5) _database_code_CSD 162096 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H18 O11 Ru4 S Si2' _chemical_formula_weight 938.87 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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Si' 'Si' 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ru' 'Ru' -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'Monoclinic ' _symmetry_space_group_name_H-M 'P 2/c ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' _cell_length_a 17.1122(19) _cell_length_b 9.9572(9) _cell_length_c 17.7322(18) _cell_angle_alpha 90.00 _cell_angle_beta 101.522(12) _cell_angle_gamma 90.00 _cell_volume 2960.5(5) _cell_formula_units_Z 4 _cell_measurement_temperature 160(2) _cell_measurement_reflns_used 5000 _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 26.0 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.106 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1808 _exptl_absorpt_coefficient_mu 2.205 _exptl_absorpt_correction_type 'numerical' _exptl_absorpt_correction_T_min 0.546 _exptl_absorpt_correction_T_max 0.859 _exptl_special_details ; The data were collected on a Stoe Imaging Plate Diffraction System (IPDS). The crystal-to-detector distance was 70 mm. 286 frames (5 min per frame) were obtained with 0 < \f < 250.5\% and with the crystals rotated through 1.5\% in \f. Coverage of the unique set was over 96.7% complete to at least 25.96\%. Crystal decay was monitored by measuring 200 reflexions per frame. ; _diffrn_ambient_temperature 160(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Stoe IPDS' _diffrn_measurement_method \f _diffrn_detector_area_resol_mean ? _diffrn_standards_number 200 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 'every frame' _diffrn_standards_decay_% <0.1 _diffrn_reflns_number 22878 _diffrn_reflns_av_R_equivalents 0.0317 _diffrn_reflns_av_sigmaI/netI 0.0216 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.05 _diffrn_reflns_theta_max 25.96 _reflns_number_total 5608 _reflns_number_gt 4974 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Stoe IPDS software (Stoe, 1996)' _computing_data_reduction 'XRED (Stoe, 1.08, 1996)' _computing_cell_refinement 'Stoe IPDS software (Stoe, 1996)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP3 for Windows (Farrugia, 1997)' _computing_structure_solution 'SIR92 (Giacovazzo et al, 1992)' _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^)+(0.0350P)^2^+0.0000P] where P==(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5608 _refine_ls_number_parameters 358 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0246 _refine_ls_R_factor_gt 0.0198 _refine_ls_wR_factor_ref 0.0502 _refine_ls_wR_factor_gt 0.0472 _refine_ls_goodness_of_fit_ref 1.015 _refine_ls_restrained_S_all 1.015 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.850434(11) 0.348302(17) 0.017517(11) 0.01347(5) Uani 1 1 d . . . Ru2 Ru 0.836612(11) 0.079685(17) 0.050757(11) 0.01470(6) Uani 1 1 d . . . Ru3 Ru 0.875804(11) 0.311811(17) -0.130945(11) 0.01436(6) Uani 1 1 d . . . Ru4 Ru 0.805326(11) 0.069696(17) -0.113387(11) 0.01436(6) Uani 1 1 d . . . S1 S 0.92691(3) 0.16206(5) -0.02534(3) 0.01506(12) Uani 1 1 d . . . Si1 Si 0.67703(4) 0.37936(7) -0.15492(4) 0.02005(14) Uani 1 1 d . . . Si2 Si 0.53430(5) 0.19947(9) 0.07851(5) 0.03195(19) Uani 1 1 d . . . O11 O 0.73015(13) 0.5170(2) 0.08012(13) 0.0365(5) Uani 1 1 d . . . O12 O 0.97074(13) 0.3559(2) 0.16834(12) 0.0334(5) Uani 1 1 d . . . O13 O 0.92554(12) 0.60147(18) -0.03377(12) 0.0288(4) Uani 1 1 d . . . O21 O 0.98560(12) -0.0103(2) 0.16571(12) 0.0318(5) Uani 1 1 d . . . O22 O 0.74682(15) 0.1210(3) 0.18008(13) 0.0488(7) Uani 1 1 d . . . O23 O 0.77884(18) -0.2055(2) 0.02042(15) 0.0525(7) Uani 1 1 d . . . O31 O 1.04497(12) 0.3312(2) -0.15801(13) 0.0331(5) Uani 1 1 d . . . O32 O 0.83708(13) 0.5248(2) -0.25399(12) 0.0343(5) Uani 1 1 d . . . O34 O 0.84172(12) 0.13179(18) -0.27061(11) 0.0265(4) Uani 1 1 d . . . O41 O 0.64922(13) -0.0440(2) -0.19715(15) 0.0436(6) Uani 1 1 d . . . O42 O 0.87671(14) -0.19429(19) -0.15004(14) 0.0394(5) Uani 1 1 d . . . C1 C 0.76094(14) 0.2812(2) -0.09068(14) 0.0142(5) Uani 1 1 d . . . C2 C 0.74902(14) 0.1998(2) -0.02794(14) 0.0152(5) Uani 1 1 d . . . C3 C 0.67351(15) 0.1928(2) -0.00422(14) 0.0181(5) Uani 1 1 d . . . C4 C 0.61557(16) 0.1893(3) 0.02454(16) 0.0233(6) Uani 1 1 d . . . C1A C 0.57437(18) 0.3550(4) -0.1366(2) 0.0410(8) Uani 1 1 d . . . H1A1 H 0.5607 0.2593 -0.1407 0.061 Uiso 1 1 calc R . . H1A2 H 0.5363 0.4057 -0.1746 0.061 Uiso 1 1 calc R . . H1A3 H 0.5723 0.3870 -0.0848 0.061 Uiso 1 1 calc R . . C1B C 0.69818(19) 0.5631(3) -0.14026(18) 0.0307(6) Uani 1 1 d . . . H1B1 H 0.7504 0.5836 -0.1521 0.046 Uiso 1 1 calc R . . H1B2 H 0.6983 0.5869 -0.0866 0.046 Uiso 1 1 calc R . . H1B3 H 0.6569 0.6149 -0.1744 0.046 Uiso 1 1 calc R . . C1C C 0.66840(18) 0.3262(3) -0.25736(17) 0.0290(6) Uani 1 1 d . . . H1C1 H 0.7198 0.3387 -0.2727 0.043 Uiso 1 1 calc R . . H1C2 H 0.6277 0.3807 -0.2904 0.043 Uiso 1 1 calc R . . H1C3 H 0.6531 0.2312 -0.2626 0.043 Uiso 1 1 calc R . . C2A C 0.5231(2) 0.0329(4) 0.1223(2) 0.0550(10) Uani 1 1 d . . . H2A1 H 0.5759 -0.0034 0.1445 0.083 Uiso 1 1 calc R . . H2A2 H 0.4954 -0.0286 0.0826 0.083 Uiso 1 1 calc R . . H2A3 H 0.4921 0.0427 0.1628 0.083 Uiso 1 1 calc R . . C2B C 0.5672(2) 0.3264(4) 0.1552(2) 0.0517(10) Uani 1 1 d . . . H2B1 H 0.6164 0.2958 0.1890 0.078 Uiso 1 1 calc R . . H2B2 H 0.5255 0.3381 0.1854 0.078 Uiso 1 1 calc R . . H2B3 H 0.5770 0.4122 0.1317 0.078 Uiso 1 1 calc R . . C2C C 0.4409(2) 0.2536(6) 0.0144(3) 0.0759(15) Uani 1 1 d . . . H2C1 H 0.3971 0.2509 0.0426 0.114 Uiso 1 1 calc R . . H2C2 H 0.4288 0.1931 -0.0300 0.114 Uiso 1 1 calc R . . H2C3 H 0.4471 0.3454 -0.0034 0.114 Uiso 1 1 calc R . . C11 C 0.77622(16) 0.4568(2) 0.05732(15) 0.0215(5) Uani 1 1 d . . . C12 C 0.92416(16) 0.3536(2) 0.11318(16) 0.0206(5) Uani 1 1 d . . . C13 C 0.89734(16) 0.4998(3) -0.02711(17) 0.0237(6) Uani 1 1 d . . . C21 C 0.92911(16) 0.0207(2) 0.12446(15) 0.0209(5) Uani 1 1 d . . . C22 C 0.77859(17) 0.1020(3) 0.13151(16) 0.0276(6) Uani 1 1 d . . . C23 C 0.80077(19) -0.0985(3) 0.02826(18) 0.0318(7) Uani 1 1 d . . . C31 C 0.98081(16) 0.3262(2) -0.14963(16) 0.0213(5) Uani 1 1 d . . . C32 C 0.84793(16) 0.4457(3) -0.20700(16) 0.0230(6) Uani 1 1 d . . . C34 C 0.84140(15) 0.1576(2) -0.20700(15) 0.0177(5) Uani 1 1 d . . . C41 C 0.70799(16) 0.0005(3) -0.16629(16) 0.0237(6) Uani 1 1 d . . . C42 C 0.85076(16) -0.0958(2) -0.13357(16) 0.0225(6) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.01521(10) 0.01412(9) 0.01125(11) -0.00062(7) 0.00305(8) 0.00025(7) Ru2 0.01525(10) 0.01574(10) 0.01374(11) 0.00337(7) 0.00445(8) 0.00154(7) Ru3 0.01648(10) 0.01454(9) 0.01287(11) 0.00055(7) 0.00487(8) -0.00117(7) Ru4 0.01543(10) 0.01363(9) 0.01468(11) -0.00109(7) 0.00462(8) -0.00082(7) S1 0.0140(3) 0.0168(3) 0.0152(3) 0.0009(2) 0.0046(2) 0.0011(2) Si1 0.0184(3) 0.0222(3) 0.0186(4) 0.0039(3) 0.0014(3) 0.0042(3) Si2 0.0184(4) 0.0515(5) 0.0288(5) -0.0118(4) 0.0117(4) -0.0027(3) O11 0.0405(12) 0.0349(11) 0.0378(13) -0.0056(9) 0.0167(11) 0.0140(9) O12 0.0337(11) 0.0431(12) 0.0194(12) -0.0025(8) -0.0043(11) 0.0054(9) O13 0.0339(11) 0.0210(9) 0.0310(12) 0.0020(8) 0.0051(10) -0.0090(8) O21 0.0232(10) 0.0442(12) 0.0263(12) 0.0098(8) 0.0007(10) 0.0072(8) O22 0.0471(14) 0.0773(16) 0.0284(13) 0.0221(11) 0.0228(12) 0.0335(12) O23 0.0797(19) 0.0263(11) 0.0491(16) 0.0005(10) 0.0073(14) -0.0223(11) O31 0.0247(11) 0.0349(11) 0.0444(14) -0.0026(9) 0.0180(10) -0.0045(8) O32 0.0417(12) 0.0345(10) 0.0273(12) 0.0150(9) 0.0086(10) 0.0016(9) O34 0.0383(11) 0.0262(9) 0.0176(10) -0.0048(7) 0.0113(9) -0.0058(8) O41 0.0234(11) 0.0609(14) 0.0460(15) -0.0206(11) 0.0060(11) -0.0137(10) O42 0.0502(14) 0.0213(10) 0.0486(14) -0.0048(9) 0.0144(12) 0.0108(9) C1 0.0144(11) 0.0153(10) 0.0127(12) -0.0029(9) 0.0022(10) 0.0014(8) C2 0.0158(11) 0.0131(10) 0.0166(13) -0.0014(8) 0.0032(10) -0.0004(8) C3 0.0181(12) 0.0209(12) 0.0141(13) 0.0005(9) 0.0008(11) 0.0010(9) C4 0.0196(13) 0.0301(13) 0.0202(15) -0.0006(10) 0.0042(12) 0.0006(10) C1A 0.0230(15) 0.058(2) 0.040(2) 0.0231(15) 0.0017(15) 0.0126(14) C1B 0.0352(16) 0.0257(13) 0.0292(17) 0.0042(11) 0.0015(14) 0.0114(11) C1C 0.0267(14) 0.0334(14) 0.0241(16) 0.0017(11) -0.0017(13) 0.0015(11) C2A 0.055(2) 0.067(2) 0.051(2) -0.0124(18) 0.031(2) -0.0294(19) C2B 0.051(2) 0.060(2) 0.049(2) -0.0261(17) 0.020(2) 0.0007(17) C2C 0.0286(19) 0.140(4) 0.058(3) -0.029(3) 0.005(2) 0.030(2) C11 0.0256(13) 0.0193(11) 0.0193(14) -0.0007(10) 0.0036(12) -0.0015(10) C12 0.0239(13) 0.0206(12) 0.0182(15) -0.0016(9) 0.0067(13) 0.0011(10) C13 0.0202(13) 0.0235(13) 0.0263(15) 0.0023(10) 0.0022(12) 0.0008(10) C21 0.0229(14) 0.0232(12) 0.0186(14) 0.0058(10) 0.0090(12) -0.0001(10) C22 0.0274(14) 0.0338(14) 0.0223(16) 0.0115(11) 0.0064(13) 0.0130(11) C23 0.0357(16) 0.0294(15) 0.0290(17) 0.0050(12) 0.0031(14) -0.0035(12) C31 0.0252(14) 0.0190(11) 0.0199(14) -0.0011(9) 0.0052(12) -0.0014(10) C32 0.0225(13) 0.0234(12) 0.0244(15) -0.0027(11) 0.0076(12) -0.0018(10) C34 0.0184(12) 0.0160(11) 0.0190(14) -0.0004(9) 0.0046(11) -0.0021(9) C41 0.0233(14) 0.0268(13) 0.0236(15) -0.0050(10) 0.0105(12) -0.0017(10) C42 0.0246(14) 0.0222(13) 0.0211(15) 0.0034(10) 0.0050(12) -0.0009(10) _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 C12 1.902(3) . ? Ru1 C11 1.907(3) . ? Ru1 C13 1.949(3) . ? Ru1 C2 2.300(2) . ? Ru1 C1 2.302(2) . ? Ru1 S1 2.4752(6) . ? Ru1 Ru2 2.7591(3) . ? Ru1 Ru3 2.7762(4) . ? Ru2 C23 1.893(3) . ? Ru2 C22 1.911(3) . ? Ru2 C21 1.932(3) . ? Ru2 C2 2.188(2) . ? Ru2 S1 2.3904(6) . ? Ru2 Ru4 2.8541(4) . ? Ru3 C32 1.888(3) . ? Ru3 C31 1.897(3) . ? Ru3 C34 2.051(2) . ? Ru3 C1 2.242(2) . ? Ru3 S1 2.4167(6) . ? Ru3 C13 2.600(3) . ? Ru3 Ru4 2.7410(3) . ? Ru4 C41 1.872(3) . ? Ru4 C42 1.886(3) . ? Ru4 C34 2.077(2) . ? Ru4 C1 2.301(2) . ? Ru4 C2 2.342(2) . ? Ru4 S1 2.5128(7) . ? Si1 C1A 1.865(3) . ? Si1 C1C 1.869(3) . ? Si1 C1B 1.873(3) . ? Si1 C1 1.914(2) . ? Si2 C4 1.842(3) . ? Si2 C2C 1.848(4) . ? Si2 C2A 1.857(4) . ? Si2 C2B 1.860(4) . ? O11 C11 1.127(3) . ? O12 C12 1.132(3) . ? O13 C13 1.137(3) . ? O21 C21 1.132(3) . ? O22 C22 1.123(3) . ? O23 C23 1.129(4) . ? O31 C31 1.138(3) . ? O32 C32 1.135(3) . ? O34 C34 1.158(3) . ? O41 C41 1.135(3) . ? O42 C42 1.139(3) . ? C1 C2 1.424(3) . ? C2 C3 1.438(3) . ? C3 C4 1.203(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C12 Ru1 C11 91.51(11) . . ? C12 Ru1 C13 94.99(11) . . ? C11 Ru1 C13 94.03(11) . . ? C12 Ru1 C2 130.55(10) . . ? C11 Ru1 C2 89.00(10) . . ? C13 Ru1 C2 134.30(10) . . ? C12 Ru1 C1 164.53(9) . . ? C11 Ru1 C1 95.26(10) . . ? C13 Ru1 C1 98.38(10) . . ? C2 Ru1 C1 36.04(8) . . ? C12 Ru1 S1 89.85(7) . . ? C11 Ru1 S1 165.98(8) . . ? C13 Ru1 S1 99.75(8) . . ? C2 Ru1 S1 79.56(6) . . ? C1 Ru1 S1 80.28(6) . . ? C12 Ru1 Ru2 84.62(7) . . ? C11 Ru1 Ru2 112.24(7) . . ? C13 Ru1 Ru2 153.73(8) . . ? C2 Ru1 Ru2 50.26(6) . . ? C1 Ru1 Ru2 79.95(6) . . ? S1 Ru1 Ru2 54.016(15) . . ? C12 Ru1 Ru3 130.38(8) . . ? C11 Ru1 Ru3 131.83(8) . . ? C13 Ru1 Ru3 63.98(8) . . ? C2 Ru1 Ru3 80.41(6) . . ? C1 Ru1 Ru3 51.37(6) . . ? S1 Ru1 Ru3 54.435(16) . . ? Ru2 Ru1 Ru3 96.431(8) . . ? C23 Ru2 C22 94.12(13) . . ? C23 Ru2 C21 92.56(12) . . ? C22 Ru2 C21 90.38(11) . . ? C23 Ru2 C2 103.05(11) . . ? C22 Ru2 C2 91.27(10) . . ? C21 Ru2 C2 164.14(9) . . ? C23 Ru2 S1 114.91(10) . . ? C22 Ru2 S1 150.94(9) . . ? C21 Ru2 S1 87.22(7) . . ? C2 Ru2 S1 83.69(6) . . ? C23 Ru2 Ru1 154.32(10) . . ? C22 Ru2 Ru1 97.29(8) . . ? C21 Ru2 Ru1 110.23(7) . . ? C2 Ru2 Ru1 53.92(6) . . ? S1 Ru2 Ru1 56.917(14) . . ? C23 Ru2 Ru4 76.44(9) . . ? C22 Ru2 Ru4 138.45(9) . . ? C21 Ru2 Ru4 129.85(7) . . ? C2 Ru2 Ru4 53.39(6) . . ? S1 Ru2 Ru4 56.427(18) . . ? Ru1 Ru2 Ru4 79.779(7) . . ? C32 Ru3 C31 86.27(11) . . ? C32 Ru3 C34 93.47(11) . . ? C31 Ru3 C34 95.69(10) . . ? C32 Ru3 C1 102.18(10) . . ? C31 Ru3 C1 170.88(10) . . ? C34 Ru3 C1 87.30(9) . . ? C32 Ru3 S1 171.71(8) . . ? C31 Ru3 S1 88.46(8) . . ? C34 Ru3 S1 93.41(7) . . ? C1 Ru3 S1 82.76(6) . . ? C32 Ru3 C13 88.70(10) . . ? C31 Ru3 C13 93.67(10) . . ? C34 Ru3 C13 170.50(9) . . ? C1 Ru3 C13 83.21(8) . . ? S1 Ru3 C13 85.26(6) . . ? C32 Ru3 Ru4 130.38(8) . . ? C31 Ru3 Ru4 122.68(7) . . ? C34 Ru3 Ru4 48.79(7) . . ? C1 Ru3 Ru4 53.89(5) . . ? S1 Ru3 Ru4 57.904(16) . . ? C13 Ru3 Ru4 123.79(6) . . ? C32 Ru3 Ru1 121.31(8) . . ? C31 Ru3 Ru1 119.26(8) . . ? C34 Ru3 Ru1 130.01(7) . . ? C1 Ru3 Ru1 53.33(6) . . ? S1 Ru3 Ru1 56.423(15) . . ? C13 Ru3 Ru1 42.36(6) . . ? Ru4 Ru3 Ru1 81.472(9) . . ? C41 Ru4 C42 86.72(11) . . ? C41 Ru4 C34 97.54(11) . . ? C42 Ru4 C34 90.97(10) . . ? C41 Ru4 C1 97.62(10) . . ? C42 Ru4 C1 174.51(10) . . ? C34 Ru4 C1 85.14(9) . . ? C41 Ru4 C2 95.04(10) . . ? C42 Ru4 C2 147.59(10) . . ? C34 Ru4 C2 120.69(9) . . ? C1 Ru4 C2 35.70(8) . . ? C41 Ru4 S1 171.64(8) . . ? C42 Ru4 S1 96.67(9) . . ? C34 Ru4 S1 90.05(7) . . ? C1 Ru4 S1 79.49(6) . . ? C2 Ru4 S1 78.01(6) . . ? C41 Ru4 Ru3 129.36(8) . . ? C42 Ru4 Ru3 122.63(8) . . ? C34 Ru4 Ru3 47.98(7) . . ? C1 Ru4 Ru3 51.91(6) . . ? C2 Ru4 Ru3 80.46(5) . . ? S1 Ru4 Ru3 54.564(14) . . ? C41 Ru4 Ru2 119.39(8) . . ? C42 Ru4 Ru2 102.91(8) . . ? C34 Ru4 Ru2 140.84(7) . . ? C1 Ru4 Ru2 77.93(6) . . ? C2 Ru4 Ru2 48.59(6) . . ? S1 Ru4 Ru2 52.429(16) . . ? Ru3 Ru4 Ru2 95.050(9) . . ? Ru2 S1 Ru3 118.32(3) . . ? Ru2 S1 Ru1 69.067(17) . . ? Ru3 S1 Ru1 69.142(17) . . ? Ru2 S1 Ru4 71.144(18) . . ? Ru3 S1 Ru4 67.532(19) . . ? Ru1 S1 Ru4 92.41(2) . . ? C1A Si1 C1C 103.77(15) . . ? C1A Si1 C1B 105.41(15) . . ? C1C Si1 C1B 112.78(13) . . ? C1A Si1 C1 116.78(12) . . ? C1C Si1 C1 109.75(12) . . ? C1B Si1 C1 108.37(12) . . ? C4 Si2 C2C 110.27(17) . . ? C4 Si2 C2A 108.63(15) . . ? C2C Si2 C2A 111.6(2) . . ? C4 Si2 C2B 105.53(15) . . ? C2C Si2 C2B 110.5(2) . . ? C2A Si2 C2B 110.06(19) . . ? C2 C1 Si1 123.26(17) . . ? C2 C1 Ru3 126.71(17) . . ? Si1 C1 Ru3 110.02(11) . . ? C2 C1 Ru4 73.71(13) . . ? Si1 C1 Ru4 126.72(12) . . ? Ru3 C1 Ru4 74.20(7) . . ? C2 C1 Ru1 71.90(14) . . ? Si1 C1 Ru1 130.02(11) . . ? Ru3 C1 Ru1 75.31(7) . . ? Ru4 C1 Ru1 102.92(9) . . ? C1 C2 C3 122.2(2) . . ? C1 C2 Ru2 128.51(17) . . ? C3 C2 Ru2 109.14(16) . . ? C1 C2 Ru1 72.06(13) . . ? C3 C2 Ru1 126.00(16) . . ? Ru2 C2 Ru1 75.82(8) . . ? C1 C2 Ru4 70.59(13) . . ? C3 C2 Ru4 132.23(17) . . ? Ru2 C2 Ru4 78.02(7) . . ? Ru1 C2 Ru4 101.73(9) . . ? C4 C3 C2 172.0(3) . . ? C3 C4 Si2 172.2(2) . . ? O11 C11 Ru1 177.2(2) . . ? O12 C12 Ru1 176.9(2) . . ? O13 C13 Ru1 161.5(2) . . ? O13 C13 Ru3 124.8(2) . . ? Ru1 C13 Ru3 73.66(8) . . ? O21 C21 Ru2 176.6(2) . . ? O22 C22 Ru2 176.3(3) . . ? O23 C23 Ru2 174.8(3) . . ? O31 C31 Ru3 176.9(2) . . ? O32 C32 Ru3 174.5(2) . . ? O34 C34 Ru3 138.61(19) . . ? O34 C34 Ru4 138.16(19) . . ? Ru3 C34 Ru4 83.22(9) . . ? O41 C41 Ru4 178.3(3) . . ? O42 C42 Ru4 176.2(2) . . ? _diffrn_measured_fraction_theta_max 0.967 _diffrn_reflns_theta_full 25.96 _diffrn_measured_fraction_theta_full 0.967 _refine_diff_density_max 0.517 _refine_diff_density_min -0.550 _refine_diff_density_rms 0.096 #========END #=========================================================================== data_(4) _database_code_CSD 162097 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H18 O12 Ru4 S Si2' _chemical_formula_weight 966.88 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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Si' 'Si' 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ru' 'Ru' -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'Triclinic ' _symmetry_space_group_name_H-M 'P -1 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.8445(9) _cell_length_b 12.8209(12) _cell_length_c 27.638(3) _cell_angle_alpha 99.767(12) _cell_angle_beta 95.019(11) _cell_angle_gamma 97.193(11) _cell_volume 3389.6(6) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 5000 _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 26.0 _exptl_crystal_description rod _exptl_crystal_colour 'yellow green' _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.895 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1864 _exptl_absorpt_coefficient_mu 1.931 _exptl_absorpt_correction_type 'numerical' _exptl_absorpt_correction_T_min 0.5460 _exptl_absorpt_correction_T_max 0.8590 _exptl_absorpt_process_details ? _exptl_special_details ; The data were collected on a Stoe Imaging Plate Diffraction System (IPDS). The crystal-to-detector distance was 70 mm. 227 frames (5 min per frame) were obtained with 0 < \f < 249.7\% and with the crystals rotated through 1.1\% in \f. Coverage of the unique set was over 94.8% complete to at least 26.0\%. Crystal decay was monitored by measuring 200 reflexions per frame. ; _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Stoe IPDS' _diffrn_measurement_method \f _diffrn_detector_area_resol_mean ? _diffrn_standards_number 200 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 'every frame' _diffrn_standards_decay_% <0.1 _diffrn_reflns_number 25238 _diffrn_reflns_av_R_equivalents 0.0318 _diffrn_reflns_av_sigmaI/netI 0.0289 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 2.10 _diffrn_reflns_theta_max 23.26 _reflns_number_total 9214 _reflns_number_gt 7856 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Stoe IPDS software (Stoe, 1996)' _computing_data_reduction 'XRED (Stoe, 1.08, 1996)' _computing_cell_refinement 'Stoe IPDS software (Stoe, 1996)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP3 for Windows (Farrugia, 1997)' _computing_structure_solution 'SIR92 (Giacovazzo et al, 1992)' _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^)+(0.0803P)^2^+0.0000P] where P==(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9214 _refine_ls_number_parameters 751 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0464 _refine_ls_R_factor_gt 0.0395 _refine_ls_wR_factor_ref 0.1021 _refine_ls_wR_factor_gt 0.0968 _refine_ls_goodness_of_fit_ref 1.009 _refine_ls_restrained_S_all 1.009 _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 Ru1A Ru 0.37412(4) 0.87108(3) 0.424883(15) 0.02220(12) Uani 1 1 d . . . Ru2A Ru 0.45907(5) 0.92663(3) 0.340753(15) 0.02351(12) Uani 1 1 d . . . Ru3A Ru 0.63278(4) 0.64161(3) 0.365797(15) 0.02164(12) Uani 1 1 d . . . Ru4A Ru 0.36886(5) 0.57669(3) 0.323813(15) 0.02236(12) Uani 1 1 d . . . S1A S 0.46084(14) 0.75521(9) 0.36219(4) 0.0213(3) Uani 1 1 d . . . Si1A Si 0.82766(17) 1.06491(13) 0.39459(6) 0.0329(4) Uani 1 1 d . . . Si2A Si 0.23021(18) 0.46927(13) 0.43784(6) 0.0351(4) Uani 1 1 d . . . O11A O 0.2699(5) 1.0759(4) 0.46934(18) 0.0514(12) Uani 1 1 d . . . O12A O 0.4365(6) 0.7771(4) 0.51750(17) 0.0554(13) Uani 1 1 d . . . O13A O 0.0814(5) 0.7551(4) 0.3924(2) 0.0539(13) Uani 1 1 d . . . O21A O 0.6197(6) 0.9195(4) 0.25013(18) 0.0595(14) Uani 1 1 d . . . O22A O 0.1799(6) 0.8408(4) 0.2845(2) 0.0621(14) Uani 1 1 d . . . O23A O 0.4134(6) 1.1600(4) 0.3526(2) 0.0655(15) Uani 1 1 d . . . O31A O 0.8336(5) 0.7611(4) 0.45406(18) 0.0555(13) Uani 1 1 d . . . O32A O 0.7793(6) 0.7256(4) 0.28384(19) 0.0616(15) Uani 1 1 d . . . O33A O 0.7510(6) 0.4330(4) 0.3475(2) 0.0605(14) Uani 1 1 d . . . O41A O 0.4321(6) 0.6313(4) 0.22538(17) 0.0595(14) Uani 1 1 d . . . O42A O 0.3743(6) 0.3390(3) 0.28878(18) 0.0521(12) Uani 1 1 d . . . O43A O 0.0576(5) 0.5769(4) 0.3012(2) 0.0539(12) Uani 1 1 d . . . C1A C 0.5585(6) 0.9534(4) 0.42023(18) 0.0252(12) Uani 1 1 d . . . C2A C 0.6583(6) 0.9921(4) 0.4003(2) 0.0297(13) Uani 1 1 d . . . C3A C 0.3625(6) 0.5372(4) 0.4059(2) 0.0296(13) Uani 1 1 d . . . C4A C 0.4820(6) 0.5722(4) 0.3991(2) 0.0257(12) Uani 1 1 d . . . C5A C 0.9100(9) 1.1159(8) 0.4589(3) 0.070(2) Uani 1 1 d . . . H5A1 H 0.8575 1.1686 0.4755 0.106 Uiso 1 1 calc R . . H5A2 H 1.0046 1.1495 0.4581 0.106 Uiso 1 1 calc R . . H5A3 H 0.9112 1.0563 0.4769 0.106 Uiso 1 1 calc R . . C6A C 0.7994(8) 1.1773(5) 0.3622(3) 0.0507(18) Uani 1 1 d . . . H6A1 H 0.7443 1.2245 0.3812 0.076 Uiso 1 1 calc R . . H6A2 H 0.7505 1.1489 0.3292 0.076 Uiso 1 1 calc R . . H6A3 H 0.8885 1.2177 0.3591 0.076 Uiso 1 1 calc R . . C7A C 0.9309(8) 0.9729(6) 0.3610(3) 0.056(2) Uani 1 1 d . . . H7A1 H 1.0208 1.0119 0.3577 0.084 Uiso 1 1 calc R . . H7A2 H 0.8829 0.9425 0.3281 0.084 Uiso 1 1 calc R . . H7A3 H 0.9441 0.9151 0.3793 0.084 Uiso 1 1 calc R . . C8A C 0.2202(15) 0.3245(7) 0.4159(6) 0.135(6) Uani 1 1 d . . . H8A1 H 0.3086 0.3016 0.4253 0.202 Uiso 1 1 calc R . . H8A2 H 0.1993 0.3085 0.3799 0.202 Uiso 1 1 calc R . . H8A3 H 0.1473 0.2864 0.4310 0.202 Uiso 1 1 calc R . . C9A C 0.0628(10) 0.5124(13) 0.4265(5) 0.134(6) Uani 1 1 d . . . H9A1 H -0.0076 0.4657 0.4387 0.201 Uiso 1 1 calc R . . H9A2 H 0.0401 0.5085 0.3909 0.201 Uiso 1 1 calc R . . H9A3 H 0.0657 0.5863 0.4436 0.201 Uiso 1 1 calc R . . C10A C 0.2915(12) 0.4988(11) 0.5048(3) 0.110(5) Uani 1 1 d . . . H10A H 0.3833 0.4779 0.5100 0.165 Uiso 1 1 calc R . . H10B H 0.2275 0.4586 0.5225 0.165 Uiso 1 1 calc R . . H10C H 0.2961 0.5756 0.5173 0.165 Uiso 1 1 calc R . . C11A C 0.3095(6) 0.9973(5) 0.4535(2) 0.0332(13) Uani 1 1 d . . . C12A C 0.4102(7) 0.8117(4) 0.4832(2) 0.0338(14) Uani 1 1 d . . . C13A C 0.1899(7) 0.7965(5) 0.4059(2) 0.0339(14) Uani 1 1 d . . . C21A C 0.5641(7) 0.9242(4) 0.2845(2) 0.0359(14) Uani 1 1 d . . . C22A C 0.2871(8) 0.8754(5) 0.3050(2) 0.0373(15) Uani 1 1 d . . . C23A C 0.4300(7) 1.0723(5) 0.3471(2) 0.0404(15) Uani 1 1 d . . . C31A C 0.7609(7) 0.7175(5) 0.4212(2) 0.0349(14) Uani 1 1 d . . . C32A C 0.7279(7) 0.6960(4) 0.3151(2) 0.0345(14) Uani 1 1 d . . . C33A C 0.7084(7) 0.5116(5) 0.3541(2) 0.0363(14) Uani 1 1 d . . . C41A C 0.4060(7) 0.6096(4) 0.2622(2) 0.0370(15) Uani 1 1 d . . . C42A C 0.3706(6) 0.4289(5) 0.3014(2) 0.0327(13) Uani 1 1 d . . . C43A C 0.1717(7) 0.5766(4) 0.3116(2) 0.0340(14) Uani 1 1 d . . . Ru1B Ru 1.23505(5) 0.86220(3) 0.824191(16) 0.02507(13) Uani 1 1 d . . . Ru2B Ru 1.12745(5) 0.65464(3) 0.814774(16) 0.02720(13) Uani 1 1 d . . . Ru3B Ru 0.96317(5) 0.83197(3) 0.937698(15) 0.02314(12) Uani 1 1 d . . . Ru4B Ru 0.81434(5) 0.86651(3) 0.856324(16) 0.02535(13) Uani 1 1 d . . . S1B S 1.03026(14) 0.80081(10) 0.85676(5) 0.0241(3) Uani 1 1 d . . . Si1B Si 1.3546(2) 0.58780(14) 0.92546(7) 0.0410(4) Uani 1 1 d . . . Si2B Si 0.9347(2) 1.17070(13) 0.86914(6) 0.0387(4) Uani 1 1 d . . . O11B O 1.4688(5) 0.8363(4) 0.7616(2) 0.0595(14) Uani 1 1 d . . . O12B O 1.0618(5) 0.9339(4) 0.74226(16) 0.0465(11) Uani 1 1 d . . . O13B O 1.3428(6) 1.0851(4) 0.88458(19) 0.0560(13) Uani 1 1 d . . . O21B O 0.9525(7) 0.4530(4) 0.8332(2) 0.0682(16) Uani 1 1 d . . . O22B O 0.9577(6) 0.6714(4) 0.72098(18) 0.0545(13) Uani 1 1 d . . . O23B O 1.3423(7) 0.5429(5) 0.7625(2) 0.0700(16) Uani 1 1 d . . . O31B O 1.2393(6) 0.8669(4) 1.00275(19) 0.0537(12) Uani 1 1 d . . . O32B O 0.8817(6) 0.5922(3) 0.93374(19) 0.0547(13) Uani 1 1 d . . . O33B O 0.7682(5) 0.8861(4) 1.01433(17) 0.0490(12) Uani 1 1 d . . . O41B O 0.6679(6) 0.6399(4) 0.82695(19) 0.0594(14) Uani 1 1 d . . . O42B O 0.7573(5) 0.9324(4) 0.75542(18) 0.0575(14) Uani 1 1 d . . . O43B O 0.5787(5) 0.9466(4) 0.9086(2) 0.0618(14) Uani 1 1 d . . . C1B C 1.3003(6) 0.7613(4) 0.8665(2) 0.0299(13) Uani 1 1 d . . . C2B C 1.2965(7) 0.6790(5) 0.8851(2) 0.0356(14) Uani 1 1 d . . . C3B C 0.9401(6) 1.0427(4) 0.8908(2) 0.0314(13) Uani 1 1 d . . . C4B C 0.9603(6) 0.9755(4) 0.9174(2) 0.0260(12) Uani 1 1 d . . . C5B C 1.5215(9) 0.6557(9) 0.9601(4) 0.082(3) Uani 1 1 d . . . H5B1 H 1.5537 0.6121 0.9834 0.123 Uiso 1 1 calc R . . H5B2 H 1.5090 0.7258 0.9782 0.123 Uiso 1 1 calc R . . H5B3 H 1.5898 0.6651 0.9368 0.123 Uiso 1 1 calc R . . C6B C 1.3740(13) 0.4598(7) 0.8864(4) 0.089(3) Uani 1 1 d . . . H6B1 H 1.3989 0.4093 0.9075 0.133 Uiso 1 1 calc R . . H6B2 H 1.4465 0.4719 0.8650 0.133 Uiso 1 1 calc R . . H6B3 H 1.2868 0.4302 0.8660 0.133 Uiso 1 1 calc R . . C7B C 1.2265(9) 0.5630(6) 0.9685(3) 0.058(2) Uani 1 1 d . . . H7B1 H 1.2523 0.5079 0.9867 0.086 Uiso 1 1 calc R . . H7B2 H 1.1355 0.5386 0.9498 0.086 Uiso 1 1 calc R . . H7B3 H 1.2236 0.6292 0.9918 0.086 Uiso 1 1 calc R . . C8B C 1.0368(8) 1.1758(5) 0.8164(3) 0.0503(18) Uani 1 1 d . . . H8B1 H 1.1336 1.1726 0.8271 0.075 Uiso 1 1 calc R . . H8B2 H 1.0296 1.2426 0.8042 0.075 Uiso 1 1 calc R . . H8B3 H 1.0015 1.1149 0.7899 0.075 Uiso 1 1 calc R . . C9B C 0.7552(9) 1.1862(7) 0.8522(4) 0.070(2) Uani 1 1 d . . . H9B1 H 0.7524 1.2521 0.8389 0.105 Uiso 1 1 calc R . . H9B2 H 0.7056 1.1898 0.8815 0.105 Uiso 1 1 calc R . . H9B3 H 0.7117 1.1249 0.8271 0.105 Uiso 1 1 calc R . . C10B C 1.0122(11) 1.2775(5) 0.9216(3) 0.070(3) Uani 1 1 d . . . H10D H 1.1037 1.2634 0.9333 0.104 Uiso 1 1 calc R . . H10E H 0.9533 1.2790 0.9485 0.104 Uiso 1 1 calc R . . H10F H 1.0204 1.3467 0.9108 0.104 Uiso 1 1 calc R . . C11B C 1.3831(7) 0.8484(5) 0.7858(2) 0.0353(14) Uani 1 1 d . . . C12B C 1.1276(6) 0.9113(4) 0.7728(2) 0.0327(14) Uani 1 1 d . . . C13B C 1.3005(6) 1.0019(5) 0.8624(2) 0.0350(14) Uani 1 1 d . . . C21B C 1.0193(8) 0.5277(5) 0.8284(2) 0.0441(16) Uani 1 1 d . . . C22B C 1.0219(7) 0.6638(4) 0.7562(2) 0.0345(14) Uani 1 1 d . . . C23B C 1.2594(8) 0.5832(5) 0.7806(2) 0.0432(16) Uani 1 1 d . . . C31B C 1.1361(7) 0.8526(4) 0.9791(2) 0.0326(14) Uani 1 1 d . . . C32B C 0.9162(6) 0.6813(5) 0.9366(2) 0.0338(14) Uani 1 1 d . . . C33B C 0.8442(6) 0.8663(4) 0.9867(2) 0.0322(13) Uani 1 1 d . . . C41B C 0.7222(7) 0.7273(5) 0.8382(2) 0.0395(15) Uani 1 1 d . . . C42B C 0.7800(7) 0.9091(5) 0.7928(2) 0.0393(15) Uani 1 1 d . . . C43B C 0.6626(7) 0.9152(5) 0.8870(2) 0.0393(15) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1A 0.0228(3) 0.0217(2) 0.0219(2) 0.00152(17) 0.00437(19) 0.00441(18) Ru2A 0.0281(3) 0.0210(2) 0.0219(2) 0.00511(17) 0.0004(2) 0.00494(18) Ru3A 0.0207(3) 0.0216(2) 0.0233(2) 0.00423(17) 0.00482(19) 0.00407(17) Ru4A 0.0253(3) 0.0192(2) 0.0211(2) 0.00078(17) 0.00069(19) 0.00277(18) S1A 0.0244(7) 0.0193(6) 0.0207(6) 0.0031(5) 0.0037(6) 0.0048(5) Si1A 0.0296(10) 0.0353(8) 0.0338(9) 0.0100(7) 0.0044(7) -0.0017(7) Si2A 0.0287(10) 0.0398(9) 0.0407(9) 0.0176(7) 0.0093(8) 0.0021(7) O11A 0.055(3) 0.037(2) 0.059(3) -0.009(2) 0.008(3) 0.017(2) O12A 0.082(4) 0.049(3) 0.038(3) 0.020(2) 0.001(3) 0.007(3) O13A 0.023(3) 0.049(3) 0.080(4) -0.009(2) 0.007(3) 0.000(2) O21A 0.081(4) 0.059(3) 0.043(3) 0.017(2) 0.032(3) 0.002(3) O22A 0.044(4) 0.074(3) 0.061(3) 0.022(3) -0.029(3) -0.007(3) O23A 0.095(5) 0.032(3) 0.073(4) 0.012(2) 0.002(3) 0.026(3) O31A 0.041(3) 0.069(3) 0.040(3) -0.018(2) -0.009(3) -0.003(2) O32A 0.077(4) 0.063(3) 0.055(3) 0.024(3) 0.038(3) 0.010(3) O33A 0.072(4) 0.043(3) 0.071(3) 0.003(2) 0.006(3) 0.036(3) O41A 0.089(4) 0.067(3) 0.028(3) 0.018(2) 0.013(3) 0.013(3) O42A 0.073(4) 0.027(2) 0.054(3) -0.005(2) 0.011(3) 0.012(2) O43A 0.034(3) 0.052(3) 0.070(3) -0.003(2) -0.009(3) 0.012(2) C1A 0.027(3) 0.027(3) 0.019(3) 0.002(2) -0.001(2) 0.005(2) C2A 0.034(4) 0.031(3) 0.025(3) 0.008(2) 0.002(3) 0.005(3) C3A 0.037(4) 0.027(3) 0.025(3) 0.004(2) -0.001(3) 0.009(3) C4A 0.028(4) 0.025(3) 0.026(3) 0.007(2) 0.004(3) 0.004(2) C5A 0.054(6) 0.096(6) 0.051(5) 0.011(4) 0.003(4) -0.023(5) C6A 0.049(5) 0.038(3) 0.071(5) 0.022(3) 0.018(4) 0.005(3) C7A 0.044(4) 0.052(4) 0.085(6) 0.034(4) 0.026(4) 0.014(3) C8A 0.177(13) 0.045(5) 0.188(13) 0.016(6) 0.122(12) -0.023(6) C9A 0.049(6) 0.245(16) 0.165(12) 0.156(13) 0.049(7) 0.052(8) C10A 0.095(8) 0.179(11) 0.041(5) 0.028(6) 0.015(5) -0.057(8) C11A 0.029(4) 0.038(3) 0.029(3) -0.001(3) 0.001(3) 0.002(3) C12A 0.035(4) 0.024(3) 0.041(4) 0.002(3) 0.005(3) -0.001(2) C13A 0.031(4) 0.029(3) 0.040(3) -0.004(3) 0.011(3) 0.008(3) C21A 0.047(4) 0.028(3) 0.033(3) 0.013(2) 0.000(3) 0.000(3) C22A 0.046(5) 0.035(3) 0.031(3) 0.011(3) -0.004(3) 0.007(3) C23A 0.047(4) 0.042(4) 0.035(3) 0.012(3) 0.001(3) 0.015(3) C31A 0.033(4) 0.038(3) 0.039(4) 0.012(3) 0.014(3) 0.012(3) C32A 0.038(4) 0.028(3) 0.037(3) -0.002(3) 0.012(3) 0.007(3) C33A 0.034(4) 0.038(3) 0.039(3) 0.011(3) 0.003(3) 0.007(3) C41A 0.040(4) 0.028(3) 0.040(4) -0.001(3) -0.004(3) 0.009(3) C42A 0.030(4) 0.033(3) 0.031(3) 0.001(3) -0.001(3) -0.001(3) C43A 0.044(5) 0.024(3) 0.033(3) 0.001(2) 0.003(3) 0.007(3) Ru1B 0.0259(3) 0.0256(2) 0.0238(2) 0.00634(18) 0.0038(2) 0.00123(19) Ru2B 0.0342(3) 0.0227(2) 0.0233(2) 0.00151(18) 0.0034(2) 0.00260(19) Ru3B 0.0259(3) 0.0237(2) 0.0195(2) 0.00497(17) 0.00136(19) 0.00213(18) Ru4B 0.0242(3) 0.0268(2) 0.0236(2) 0.00543(18) -0.0024(2) 0.00037(19) S1B 0.0271(8) 0.0241(6) 0.0205(6) 0.0044(5) 0.0032(6) 0.0006(5) Si1B 0.0432(11) 0.0414(9) 0.0444(10) 0.0189(8) 0.0044(9) 0.0137(8) Si2B 0.0529(12) 0.0278(8) 0.0363(9) 0.0103(7) -0.0002(8) 0.0066(8) O11B 0.042(3) 0.084(4) 0.057(3) 0.017(3) 0.022(3) 0.011(3) O12B 0.048(3) 0.063(3) 0.032(2) 0.022(2) 0.000(2) 0.007(2) O13B 0.059(4) 0.037(3) 0.065(3) -0.002(2) 0.000(3) -0.002(2) O21B 0.092(5) 0.030(3) 0.081(4) 0.015(2) 0.019(3) -0.010(3) O22B 0.063(4) 0.046(3) 0.046(3) 0.009(2) -0.020(3) -0.007(2) O23B 0.079(4) 0.086(4) 0.047(3) -0.010(3) 0.022(3) 0.040(3) O31B 0.040(3) 0.062(3) 0.053(3) 0.003(2) -0.017(3) 0.011(2) O32B 0.072(4) 0.025(2) 0.069(3) 0.014(2) 0.013(3) 0.000(2) O33B 0.046(3) 0.057(3) 0.039(3) -0.002(2) 0.017(3) -0.003(2) O41B 0.066(4) 0.045(3) 0.056(3) 0.006(2) -0.007(3) -0.021(3) O42B 0.046(3) 0.085(4) 0.043(3) 0.036(3) -0.014(2) -0.005(3) O43B 0.034(3) 0.076(4) 0.071(4) -0.005(3) 0.004(3) 0.016(3) C1B 0.033(4) 0.034(3) 0.022(3) 0.003(2) 0.005(3) 0.006(3) C2B 0.042(4) 0.031(3) 0.033(3) 0.005(3) 0.003(3) 0.005(3) C3B 0.032(4) 0.028(3) 0.031(3) 0.002(2) -0.002(3) 0.000(2) C4B 0.023(3) 0.025(3) 0.028(3) 0.001(2) 0.001(2) 0.000(2) C5B 0.049(5) 0.115(8) 0.094(7) 0.060(6) -0.005(5) 0.014(5) C6B 0.140(10) 0.069(6) 0.078(6) 0.029(5) 0.036(6) 0.059(6) C7B 0.067(5) 0.055(4) 0.060(5) 0.022(4) 0.017(4) 0.019(4) C8B 0.064(5) 0.044(4) 0.045(4) 0.019(3) 0.001(4) 0.003(3) C9B 0.066(6) 0.059(5) 0.096(7) 0.039(5) 0.008(5) 0.025(4) C10B 0.137(9) 0.027(3) 0.042(4) 0.009(3) 0.002(5) -0.001(4) C11B 0.032(4) 0.036(3) 0.037(3) 0.010(3) 0.003(3) 0.002(3) C12B 0.035(4) 0.034(3) 0.034(3) 0.013(3) 0.017(3) 0.004(3) C13B 0.032(4) 0.033(3) 0.043(3) 0.011(3) 0.006(3) 0.007(3) C21B 0.060(5) 0.035(4) 0.037(3) 0.005(3) 0.009(3) 0.006(3) C22B 0.044(4) 0.026(3) 0.029(3) -0.003(2) 0.002(3) -0.001(3) C23B 0.048(4) 0.049(4) 0.032(3) 0.006(3) 0.005(3) 0.008(3) C31B 0.041(4) 0.028(3) 0.031(3) 0.007(2) 0.003(3) 0.008(3) C32B 0.034(4) 0.044(4) 0.024(3) 0.011(3) 0.000(3) 0.005(3) C33B 0.033(4) 0.033(3) 0.029(3) 0.006(2) 0.000(3) -0.003(3) C41B 0.038(4) 0.041(4) 0.037(3) 0.009(3) 0.000(3) -0.004(3) C42B 0.027(4) 0.041(3) 0.046(4) 0.008(3) -0.005(3) -0.002(3) C43B 0.029(4) 0.046(4) 0.037(3) -0.001(3) -0.007(3) 0.001(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1A C11A 1.888(6) . ? Ru1A C12A 1.921(6) . ? Ru1A C13A 1.925(7) . ? Ru1A C1A 2.008(6) . ? Ru1A S1A 2.3750(13) . ? Ru1A Ru2A 2.7140(6) . ? Ru2A C22A 1.866(8) . ? Ru2A C23A 1.906(6) . ? Ru2A C21A 1.939(6) . ? Ru2A C1A 2.277(5) . ? Ru2A S1A 2.3730(12) . ? Ru2A C2A 2.411(6) . ? Ru3A C33A 1.900(6) . ? Ru3A C32A 1.930(6) . ? Ru3A C31A 1.931(7) . ? Ru3A C4A 2.008(5) . ? Ru3A S1A 2.3735(13) . ? Ru3A Ru4A 2.7190(7) . ? Ru4A C41A 1.879(7) . ? Ru4A C42A 1.894(6) . ? Ru4A C43A 1.940(7) . ? Ru4A C4A 2.287(5) . ? Ru4A S1A 2.3818(14) . ? Ru4A C3A 2.411(5) . ? Si1A C7A 1.839(7) . ? Si1A C2A 1.839(6) . ? Si1A C6A 1.858(6) . ? Si1A C5A 1.861(8) . ? Si2A C9A 1.822(9) . ? Si2A C8A 1.839(10) . ? Si2A C3A 1.847(6) . ? Si2A C10A 1.856(9) . ? O11A C11A 1.156(7) . ? O12A C12A 1.135(7) . ? O13A C13A 1.133(8) . ? O21A C21A 1.134(7) . ? O22A C22A 1.151(8) . ? O23A C23A 1.143(8) . ? O31A C31A 1.125(8) . ? O32A C32A 1.134(7) . ? O33A C33A 1.131(7) . ? O41A C41A 1.140(7) . ? O42A C42A 1.153(7) . ? O43A C43A 1.135(8) . ? C1A C2A 1.257(8) . ? C3A C4A 1.247(8) . ? Ru1B C11B 1.885(6) . ? Ru1B C13B 1.920(7) . ? Ru1B C12B 1.933(6) . ? Ru1B C1B 2.012(5) . ? Ru1B S1B 2.3780(14) . ? Ru1B Ru2B 2.6986(7) . ? Ru2B C22B 1.874(6) . ? Ru2B C23B 1.908(7) . ? Ru2B C21B 1.941(7) . ? Ru2B C1B 2.267(6) . ? Ru2B S1B 2.3832(14) . ? Ru2B C2B 2.397(6) . ? Ru3B C33B 1.899(6) . ? Ru3B C32B 1.923(6) . ? Ru3B C31B 1.929(7) . ? Ru3B C4B 2.016(5) . ? Ru3B S1B 2.3710(13) . ? Ru3B Ru4B 2.7064(6) . ? Ru4B C41B 1.863(7) . ? Ru4B C43B 1.901(7) . ? Ru4B C42B 1.940(6) . ? Ru4B C4B 2.268(6) . ? Ru4B S1B 2.3822(15) . ? Ru4B C3B 2.430(6) . ? Si1B C7B 1.843(7) . ? Si1B C6B 1.846(9) . ? Si1B C2B 1.854(6) . ? Si1B C5B 1.859(10) . ? Si2B C9B 1.832(9) . ? Si2B C3B 1.845(5) . ? Si2B C8B 1.847(7) . ? Si2B C10B 1.852(8) . ? O11B C11B 1.131(8) . ? O12B C12B 1.120(7) . ? O13B C13B 1.145(8) . ? O21B C21B 1.126(8) . ? O22B C22B 1.139(7) . ? O23B C23B 1.126(8) . ? O31B C31B 1.135(8) . ? O32B C32B 1.138(7) . ? O33B C33B 1.135(7) . ? O41B C41B 1.157(8) . ? O42B C42B 1.135(7) . ? O43B C43B 1.135(8) . ? C1B C2B 1.247(8) . ? C3B C4B 1.248(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C11A Ru1A C12A 99.3(2) . . ? C11A Ru1A C13A 92.3(2) . . ? C12A Ru1A C13A 96.6(3) . . ? C11A Ru1A C1A 91.1(2) . . ? C12A Ru1A C1A 101.9(2) . . ? C13A Ru1A C1A 160.3(2) . . ? C11A Ru1A S1A 155.88(17) . . ? C12A Ru1A S1A 103.91(18) . . ? C13A Ru1A S1A 91.31(17) . . ? C1A Ru1A S1A 78.00(15) . . ? C11A Ru1A Ru2A 101.01(17) . . ? C12A Ru1A Ru2A 149.39(19) . . ? C13A Ru1A Ru2A 105.11(18) . . ? C1A Ru1A Ru2A 55.25(14) . . ? S1A Ru1A Ru2A 55.10(3) . . ? C22A Ru2A C23A 93.4(3) . . ? C22A Ru2A C21A 96.9(3) . . ? C23A Ru2A C21A 96.7(2) . . ? C22A Ru2A C1A 138.6(2) . . ? C23A Ru2A C1A 91.8(2) . . ? C21A Ru2A C1A 123.2(2) . . ? C22A Ru2A S1A 88.06(17) . . ? C23A Ru2A S1A 158.12(19) . . ? C21A Ru2A S1A 104.83(17) . . ? C1A Ru2A S1A 73.18(13) . . ? C22A Ru2A C2A 169.3(2) . . ? C23A Ru2A C2A 85.9(2) . . ? C21A Ru2A C2A 93.8(2) . . ? C1A Ru2A C2A 30.93(19) . . ? S1A Ru2A C2A 88.73(13) . . ? C22A Ru2A Ru1A 92.53(18) . . ? C23A Ru2A Ru1A 102.94(19) . . ? C21A Ru2A Ru1A 157.66(17) . . ? C1A Ru2A Ru1A 46.43(14) . . ? S1A Ru2A Ru1A 55.17(3) . . ? C2A Ru2A Ru1A 77.28(13) . . ? C33A Ru3A C32A 91.9(2) . . ? C33A Ru3A C31A 99.1(3) . . ? C32A Ru3A C31A 96.7(3) . . ? C33A Ru3A C4A 90.5(2) . . ? C32A Ru3A C4A 160.2(3) . . ? C31A Ru3A C4A 102.4(2) . . ? C33A Ru3A S1A 156.5(2) . . ? C32A Ru3A S1A 93.67(18) . . ? C31A Ru3A S1A 102.85(17) . . ? C4A Ru3A S1A 76.83(15) . . ? C33A Ru3A Ru4A 101.3(2) . . ? C32A Ru3A Ru4A 104.8(2) . . ? C31A Ru3A Ru4A 149.66(17) . . ? C4A Ru3A Ru4A 55.44(16) . . ? S1A Ru3A Ru4A 55.27(3) . . ? C41A Ru4A C42A 92.1(2) . . ? C41A Ru4A C43A 94.5(3) . . ? C42A Ru4A C43A 97.7(2) . . ? C41A Ru4A C4A 139.9(2) . . ? C42A Ru4A C4A 92.3(2) . . ? C43A Ru4A C4A 124.2(2) . . ? C41A Ru4A S1A 89.70(18) . . ? C42A Ru4A S1A 156.62(19) . . ? C43A Ru4A S1A 105.38(17) . . ? C4A Ru4A S1A 71.76(13) . . ? C41A Ru4A C3A 170.4(2) . . ? C42A Ru4A C3A 87.4(2) . . ? C43A Ru4A C3A 95.1(2) . . ? C4A Ru4A C3A 30.6(2) . . ? S1A Ru4A C3A 86.97(14) . . ? C41A Ru4A Ru3A 93.9(2) . . ? C42A Ru4A Ru3A 101.64(19) . . ? C43A Ru4A Ru3A 158.59(17) . . ? C4A Ru4A Ru3A 46.30(14) . . ? S1A Ru4A Ru3A 54.98(3) . . ? C3A Ru4A Ru3A 76.87(15) . . ? Ru2A S1A Ru3A 133.18(6) . . ? Ru2A S1A Ru1A 69.73(4) . . ? Ru3A S1A Ru1A 131.74(6) . . ? Ru2A S1A Ru4A 135.41(6) . . ? Ru3A S1A Ru4A 69.75(4) . . ? Ru1A S1A Ru4A 128.78(6) . . ? C7A Si1A C2A 109.6(3) . . ? C7A Si1A C6A 111.9(3) . . ? C2A Si1A C6A 108.1(3) . . ? C7A Si1A C5A 110.4(4) . . ? C2A Si1A C5A 105.9(3) . . ? C6A Si1A C5A 110.8(4) . . ? C9A Si2A C8A 110.7(8) . . ? C9A Si2A C3A 112.0(3) . . ? C8A Si2A C3A 107.6(4) . . ? C9A Si2A C10A 110.8(7) . . ? C8A Si2A C10A 108.3(7) . . ? C3A Si2A C10A 107.4(3) . . ? C2A C1A Ru1A 158.2(5) . . ? C2A C1A Ru2A 80.4(4) . . ? Ru1A C1A Ru2A 78.32(19) . . ? C1A C2A Si1A 159.4(5) . . ? C1A C2A Ru2A 68.6(4) . . ? Si1A C2A Ru2A 131.5(3) . . ? C4A C3A Si2A 155.3(5) . . ? C4A C3A Ru4A 69.2(3) . . ? Si2A C3A Ru4A 134.3(3) . . ? C3A C4A Ru3A 157.9(5) . . ? C3A C4A Ru4A 80.2(4) . . ? Ru3A C4A Ru4A 78.26(17) . . ? O11A C11A Ru1A 177.3(5) . . ? O12A C12A Ru1A 177.5(6) . . ? O13A C13A Ru1A 176.1(6) . . ? O21A C21A Ru2A 176.3(6) . . ? O22A C22A Ru2A 176.8(5) . . ? O23A C23A Ru2A 177.7(6) . . ? O31A C31A Ru3A 178.6(5) . . ? O32A C32A Ru3A 177.1(6) . . ? O33A C33A Ru3A 178.5(6) . . ? O41A C41A Ru4A 178.0(6) . . ? O42A C42A Ru4A 178.1(6) . . ? O43A C43A Ru4A 175.5(5) . . ? C11B Ru1B C13B 98.4(3) . . ? C11B Ru1B C12B 92.1(2) . . ? C13B Ru1B C12B 95.7(2) . . ? C11B Ru1B C1B 91.7(2) . . ? C13B Ru1B C1B 104.4(2) . . ? C12B Ru1B C1B 158.8(3) . . ? C11B Ru1B S1B 155.28(19) . . ? C13B Ru1B S1B 105.77(18) . . ? C12B Ru1B S1B 90.48(17) . . ? C1B Ru1B S1B 77.66(17) . . ? C11B Ru1B Ru2B 100.03(18) . . ? C13B Ru1B Ru2B 152.67(17) . . ? C12B Ru1B Ru2B 103.56(18) . . ? C1B Ru1B Ru2B 55.24(17) . . ? S1B Ru1B Ru2B 55.56(3) . . ? C22B Ru2B C23B 93.2(3) . . ? C22B Ru2B C21B 97.2(3) . . ? C23B Ru2B C21B 96.8(3) . . ? C22B Ru2B C1B 135.9(2) . . ? C23B Ru2B C1B 90.0(3) . . ? C21B Ru2B C1B 126.0(2) . . ? C22B Ru2B S1B 89.29(18) . . ? C23B Ru2B S1B 157.5(2) . . ? C21B Ru2B S1B 105.0(2) . . ? C1B Ru2B S1B 72.99(15) . . ? C22B Ru2B C2B 166.3(2) . . ? C23B Ru2B C2B 84.4(3) . . ? C21B Ru2B C2B 96.5(3) . . ? C1B Ru2B C2B 30.9(2) . . ? S1B Ru2B C2B 87.88(15) . . ? C22B Ru2B Ru1B 89.79(17) . . ? C23B Ru2B Ru1B 102.3(2) . . ? C21B Ru2B Ru1B 159.26(19) . . ? C1B Ru2B Ru1B 46.81(14) . . ? S1B Ru2B Ru1B 55.38(3) . . ? C2B Ru2B Ru1B 77.55(14) . . ? C33B Ru3B C32B 91.7(2) . . ? C33B Ru3B C31B 99.6(3) . . ? C32B Ru3B C31B 97.4(2) . . ? C33B Ru3B C4B 91.2(2) . . ? C32B Ru3B C4B 159.1(2) . . ? C31B Ru3B C4B 102.5(2) . . ? C33B Ru3B S1B 156.34(18) . . ? C32B Ru3B S1B 91.91(17) . . ? C31B Ru3B S1B 103.06(18) . . ? C4B Ru3B S1B 77.52(15) . . ? C33B Ru3B Ru4B 101.00(18) . . ? C32B Ru3B Ru4B 104.09(18) . . ? C31B Ru3B Ru4B 149.55(16) . . ? C4B Ru3B Ru4B 55.08(16) . . ? S1B Ru3B Ru4B 55.49(4) . . ? C41B Ru4B C43B 92.2(3) . . ? C41B Ru4B C42B 97.0(3) . . ? C43B Ru4B C42B 99.6(3) . . ? C41B Ru4B C4B 142.2(2) . . ? C43B Ru4B C4B 89.4(2) . . ? C42B Ru4B C4B 120.0(2) . . ? C41B Ru4B S1B 90.3(2) . . ? C43B Ru4B S1B 153.42(19) . . ? C42B Ru4B S1B 106.4(2) . . ? C4B Ru4B S1B 72.78(14) . . ? C41B Ru4B C3B 172.5(2) . . ? C43B Ru4B C3B 86.3(2) . . ? C42B Ru4B C3B 90.5(2) . . ? C4B Ru4B C3B 30.56(19) . . ? S1B Ru4B C3B 87.80(15) . . ? C41B Ru4B Ru3B 95.74(19) . . ? C43B Ru4B Ru3B 98.32(19) . . ? C42B Ru4B Ru3B 157.58(19) . . ? C4B Ru4B Ru3B 46.79(13) . . ? S1B Ru4B Ru3B 55.10(3) . . ? C3B Ru4B Ru3B 77.24(13) . . ? Ru3B S1B Ru1B 131.70(6) . . ? Ru3B S1B Ru4B 69.41(4) . . ? Ru1B S1B Ru4B 130.11(5) . . ? Ru3B S1B Ru2B 130.16(5) . . ? Ru1B S1B Ru2B 69.05(4) . . ? Ru4B S1B Ru2B 138.48(6) . . ? C7B Si1B C6B 109.2(4) . . ? C7B Si1B C2B 110.1(3) . . ? C6B Si1B C2B 108.8(3) . . ? C7B Si1B C5B 110.5(4) . . ? C6B Si1B C5B 111.7(5) . . ? C2B Si1B C5B 106.6(3) . . ? C9B Si2B C3B 109.3(3) . . ? C9B Si2B C8B 111.2(4) . . ? C3B Si2B C8B 110.2(3) . . ? C9B Si2B C10B 109.9(5) . . ? C3B Si2B C10B 106.6(3) . . ? C8B Si2B C10B 109.5(4) . . ? C2B C1B Ru1B 157.5(5) . . ? C2B C1B Ru2B 80.3(4) . . ? Ru1B C1B Ru2B 78.0(2) . . ? C1B C2B Si1B 157.4(6) . . ? C1B C2B Ru2B 68.8(4) . . ? Si1B C2B Ru2B 133.2(3) . . ? C4B C3B Si2B 162.0(5) . . ? C4B C3B Ru4B 67.5(3) . . ? Si2B C3B Ru4B 129.8(3) . . ? C3B C4B Ru3B 159.3(5) . . ? C3B C4B Ru4B 81.9(4) . . ? Ru3B C4B Ru4B 78.13(18) . . ? O11B C11B Ru1B 177.0(6) . . ? O12B C12B Ru1B 176.0(6) . . ? O13B C13B Ru1B 178.2(6) . . ? O21B C21B Ru2B 175.4(6) . . ? O22B C22B Ru2B 178.7(5) . . ? O23B C23B Ru2B 176.4(7) . . ? O31B C31B Ru3B 178.0(5) . . ? O32B C32B Ru3B 175.7(6) . . ? O33B C33B Ru3B 176.8(5) . . ? O41B C41B Ru4B 178.4(6) . . ? O42B C42B Ru4B 178.5(6) . . ? O43B C43B Ru4B 174.7(6) . . ? _diffrn_measured_fraction_theta_max 0.948 _diffrn_reflns_theta_full 23.26 _diffrn_measured_fraction_theta_full 0.948 _refine_diff_density_max 0.925 _refine_diff_density_min -0.857 _refine_diff_density_rms 0.151 #========END