Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2005 data_global #============================================================================== # 0. AUDIT DETAILS _audit_creation_date ' 2004' _audit_creation_method SHELX-97 _audit_update_record ; ? ; #============================================================================== # 1. SUBMISSION DETAILS _journal_coden_Cambridge 222 _publ_contact_author_name 'Prof. F. Gordon A. Stone' _publ_contact_author_address ; Department of Chemistry and Biochemistry Baylor University One Bear Place # 97348 Waco TX, 76798-7348 USA ; _publ_contact_author_email Gordon_Stone@baylor.edu _publ_contact_author_fax '+1 254 710 2403' _publ_contact_author_phone '+1 254 710 4427' _publ_requested_journal ; Dalton Transactions ; _publ_requested_category ? _publ_requested_coeditor_name ? _publ_section_title ; Substitution, Cage Functionalization, and Oxidation of the Charge- Compensated Triruthenamonocarbollide Cluster Complex [1-SMe~2~-2,2-(CO)~2~-7,11-(\m-H)~2~-2,7,11-{Ru~2~(CO)~6~}- closo-2,1-RuCB~10~H~8~] ; loop_ _publ_author_name _publ_author_address 'McGrath, Thomas D.' ; Department of Chemistry and Biochemistry Baylor University Waco TX, 76798-7348 USA ; 'Stone, F. Gordon A.' ; Department of Chemistry and Biochemistry Baylor University Waco TX, 76798-7348 USA ; ' Sukcharoenphon, Kengkaj ' ; Department of Chemistry and Biochemistry Baylor University Waco TX, 76798-7348 USA ; #============================================================================== _publ_section_exptl_refinement ; X-ray intensity data were collected at 110(2) K on a Bruker-Nonius X8 APEX CCD area-detector diffractometer using Mo-K\a X-radiation. Several sets of narrow data 'frames' were collected at different values of \q, for various initial values of \f and \w, using 0.5\% increments of \f or \w. The data frames were integrated using SAINT (Bruker, 2003); the substantial redundancy in data allowed an empirical absorption correction (SADABS; Bruker, 2003) to be applied, based on multiple measurements of equivalent reflections. All structures were solved using conventional direct methods (Bruker, 2000; Bruker, 2003) and refined by full-matrix least-squares on all F^2^ data using SHELXTL version 6.12 (Bruker, 2003) with anisotropic thermal parameters assigned to all non-H atoms. The locations of the cage-carbon atoms were verified by examination of the appropriate internuclear distances and the magnitudes of their isotropic thermal displacement parameters. Hydrogen atoms in organic functions and those in terminal BH units were set riding in calculated positions with fixed isotropic thermal parameters defined as U~iso~(H) = 1.2 x U~iso~(parent), or U~iso~(H) = 1.5 x U~iso~(parent) for methyl groups. The hydrogen atoms involved in B-H-Ru agostic-type interactions, that in the C-H...Ru agostic bond in 13, and those in Ru-H-Ru bridges were located in difference maps and allowed positional refinement with fixed isotropic thermal parameters as above. However, exceptions to this were that in 6 the agostic-type and metal-bridging H atoms had to be added from initial calculated positions, and the location of the Ru-H-Ru hydrogens were restrained towards a mean (refining) Ru-H distance (1.77(5) \%A) using the DFIX card in SHELXL-97 (Bruker, 2003). The PMe~3~ unit in the crystals of compound 4 suffered from rotational disorder with two components related by rotation about the Ru-P bond. Both disordered components were included in the model and treated as above; they were assigned refining complementary occupancies, which were in the approximate ratio of 77:23 at convergence. Compound 6 crystallized with two crystallographically independent molecules, plus two molecules of CH~2~Cl~2~ as solvate, per asymmetric unit. One of the Cy rings in one of the independent molecules of 6 was slightly disordered, such that there were two positions for two of the ring CH~2~ units. With the alternate positions paired such that the chair conformation was maintained, the two components were assigned refining complementary occupancies, around 84:16 at convergence, and otherwise treated as above. One of the solvate molecules was ordered, whilst the other was disordered over two proximal positions. These two fractional molecules were assigned refining complementary occupancies that converged close to 76 and 24%. All C-Cl bonding distances were restrained towards 1.76(2) \%A using the DFIX card, but the solvates were otherwise treated as described. In the crystals obtained for compound 10, four (partial) molecules of THF were found to crystallize along with one of compound 10 in the asymmetric fraction of the unit cell. Whilst the ruthenacarborane molecule was straightforward and refined as above, the solvate was at first problematic. Ultimately it was established that two of the THF molecules had unit occupancy, whilst the occupancies of the other two were allowed to refine, achieving values of approximately 53.4 and 63.3 %. The solvate molecules were otherwise well behaved and treated as above; some slight disorder was apparent but accommodated by the relatively large thermal parameters of some of the atoms therein. The structure determinations for compounds 12-14 were all relatively free of difficulty and were refined as described above, with the following specific features. In 12 there was some slight disorder in two of the Me groups in the Ru-(\m-SBu^t^)-Ru unit. Each component was assigned a refining complementary occupancy, which converged to the approximate ratio 63:37. Crystals of 13 contained one-quarter molecule of CH~2~Cl~2~ as solvate, located close to a C~2~ axis (Wyckoff position e), of which the C-Cl distances were restrained as for 6 above. One molecule of CH~2~Cl~2~ also co-crystallized with each molecule of 14 and was treated without restraint as described above. ; _publ_section_references ; Bruker (2000). SHELXTL-PC. Version 6.10. Bruker Analytical X-ray Solutions, Madison, Wisconsin, USA. Bruker (2003). APEX 2. Version 1.0-5. Bruker Analytical X-ray Solutions, Madison, Wisconsin, USA. Wilson, A.J.C. (1992) Ed. International Tables for Crystallography, Volume C, Kluwer Academic Publishers, Dordrecht, The Netherlands. ; _publ_section_figure_captions ; ? ; _publ_section_acknowledgements ; ? ; #============================================================================== data_4 _database_code_depnum_ccdc_archive 'CCDC 268993' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C13 H25 B10 O7 P Ru3 S' _chemical_formula_weight 767.67 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P2(1)/n ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.7732(6) _cell_length_b 11.7293(6) _cell_length_c 21.4925(11) _cell_angle_alpha 90.00 _cell_angle_beta 97.692(2) _cell_angle_gamma 90.00 _cell_volume 2691.4(2) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 7034 _cell_measurement_theta_min 2.25 _cell_measurement_theta_max 34.72 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.895 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1488 _exptl_absorpt_coefficient_mu 1.831 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6815 _exptl_absorpt_correction_T_max 0.8396 _exptl_absorpt_process_details 'SADABS (Bruker, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(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 'Bruker-Nonius X8 Apex CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 123745 _diffrn_reflns_av_R_equivalents 0.0491 _diffrn_reflns_av_sigmaI/netI 0.0389 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -38 _diffrn_reflns_limit_l_max 39 _diffrn_reflns_theta_min 1.91 _diffrn_reflns_theta_max 40.66 _reflns_number_total 17217 _reflns_number_gt 13106 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2 (Bruker, 2003)' _computing_cell_refinement 'Bruker APEX2 (Bruker, 2003)' _computing_data_reduction 'Bruker APEX2 (Bruker, 2003)' _computing_structure_solution 'Bruker SHELXTL (Bruker, 2000)' _computing_structure_refinement 'Bruker SHELXTL (Bruker, 2000)' _computing_molecular_graphics 'Bruker SHELXTL (Bruker, 2000)' _computing_publication_material 'Bruker SHELXTL (Bruker, 2000)' _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^)+(0.0267P)^2^+0.2023P] 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 17217 _refine_ls_number_parameters 358 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0453 _refine_ls_R_factor_gt 0.0275 _refine_ls_wR_factor_ref 0.0626 _refine_ls_wR_factor_gt 0.0589 _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_restrained_S_all 1.059 _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 0.246624(8) 0.266317(8) 0.111449(4) 0.01488(2) Uani 1 1 d . A . Ru2 Ru 0.387091(9) 0.081169(8) 0.163527(4) 0.01562(2) Uani 1 1 d . . . Ru3 Ru 0.133495(8) 0.057611(8) 0.114370(5) 0.01566(2) Uani 1 1 d . A . C1 C 0.26402(11) 0.37937(10) 0.02895(6) 0.01682(19) Uani 1 1 d . . . B3 B 0.40752(12) 0.32103(11) 0.06198(7) 0.0180(2) Uani 1 1 d . A . H3 H 0.4789 0.3653 0.0963 0.022 Uiso 1 1 calc R . . B4 B 0.37884(13) 0.36686(12) -0.01832(7) 0.0193(2) Uani 1 1 d . A . H4 H 0.4308 0.4412 -0.0349 0.023 Uiso 1 1 calc R . . B5 B 0.21917(13) 0.34110(12) -0.04798(7) 0.0193(2) Uani 1 1 d . A . H5 H 0.1661 0.3981 -0.0840 0.023 Uiso 1 1 calc R . . B6 B 0.14409(12) 0.27877(11) 0.01373(7) 0.0175(2) Uani 1 1 d . A . H6 H 0.0426 0.2953 0.0166 0.021 Uiso 1 1 calc R . . B7 B 0.38045(12) 0.16701(11) 0.06088(6) 0.0169(2) Uani 1 1 d . A . H7 H 0.4441(16) 0.0916(15) 0.0838(8) 0.020 Uiso 1 1 d . A . B8 B 0.45353(13) 0.23388(12) 0.00086(7) 0.0190(2) Uani 1 1 d . . . H8 H 0.5551 0.2199 -0.0028 0.023 Uiso 1 1 calc R A . B9 B 0.33756(14) 0.24719(12) -0.06693(7) 0.0204(2) Uani 1 1 d . A . H9 H 0.3630 0.2414 -0.1157 0.024 Uiso 1 1 calc R . . B10 B 0.19243(13) 0.19225(12) -0.04746(7) 0.0187(2) Uani 1 1 d . . . H10 H 0.1213 0.1506 -0.0831 0.022 Uiso 1 1 calc R A . B11 B 0.22108(12) 0.14236(11) 0.03133(6) 0.0168(2) Uani 1 1 d . A . H11 H 0.1788(16) 0.0497(14) 0.0381(9) 0.020 Uiso 1 1 d . . . B12 B 0.33819(13) 0.12532(12) -0.01854(7) 0.0184(2) Uani 1 1 d . A . H12 H 0.3637 0.0395 -0.0358 0.022 Uiso 1 1 calc R . . C11 C 0.33898(14) 0.31148(11) 0.18916(7) 0.0257(3) Uani 1 1 d . . . O11 O 0.39179(14) 0.35011(10) 0.23428(6) 0.0429(3) Uani 1 1 d . A . C12 C 0.09646(13) 0.31381(11) 0.14188(6) 0.0217(2) Uani 1 1 d . . . O12 O 0.00506(10) 0.34540(9) 0.15807(6) 0.0310(2) Uani 1 1 d . A . C13 C 0.34987(12) 0.07344(11) 0.24547(6) 0.0212(2) Uani 1 1 d . A . O13 O 0.33516(11) 0.07004(10) 0.29746(5) 0.0311(2) Uani 1 1 d . . . C14 C 0.41184(12) -0.07659(11) 0.16443(7) 0.0222(2) Uani 1 1 d . A . O14 O 0.42482(11) -0.17307(9) 0.16681(6) 0.0326(2) Uani 1 1 d . . . C15 C 0.13393(11) -0.10478(11) 0.11639(7) 0.0217(2) Uani 1 1 d . . . O15 O 0.13523(10) -0.20218(9) 0.11567(6) 0.0326(2) Uani 1 1 d . A . C16 C 0.08883(12) 0.07744(11) 0.19600(7) 0.0212(2) Uani 1 1 d . . . O16 O 0.05429(11) 0.09443(10) 0.24316(5) 0.0301(2) Uani 1 1 d . A . C17 C -0.03679(12) 0.08975(10) 0.07663(6) 0.0208(2) Uani 1 1 d . . . O17 O -0.13678(10) 0.11113(9) 0.05596(6) 0.0301(2) Uani 1 1 d . A . S S 0.21253(3) 0.51962(3) 0.048330(16) 0.01903(5) Uani 1 1 d . A . C21 C 0.33837(12) 0.57648(11) 0.10244(7) 0.0216(2) Uani 1 1 d . . . H21A H 0.3535 0.5268 0.1393 0.032 Uiso 1 1 calc R A . H21B H 0.3160 0.6530 0.1155 0.032 Uiso 1 1 calc R . . H21C H 0.4143 0.5807 0.0821 0.032 Uiso 1 1 calc R . . C22 C 0.22422(14) 0.61278(11) -0.01725(7) 0.0256(3) Uani 1 1 d . . . H22A H 0.2114 0.6918 -0.0048 0.038 Uiso 1 1 calc R A . H22B H 0.1602 0.5921 -0.0522 0.038 Uiso 1 1 calc R . . H22C H 0.3074 0.6051 -0.0304 0.038 Uiso 1 1 calc R . . P1 P 0.59891(3) 0.12508(3) 0.201756(16) 0.02182(6) Uani 0.771(11) 1 d P A 1 C311 C 0.6794(4) 0.2384(2) 0.16570(19) 0.0342(8) Uani 0.771(11) 1 d PU A 1 H31A H 0.6413 0.3119 0.1738 0.051 Uiso 0.771(11) 1 calc PR A 1 H31B H 0.6722 0.2255 0.1203 0.051 Uiso 0.771(11) 1 calc PR A 1 H31C H 0.7680 0.2390 0.1836 0.051 Uiso 0.771(11) 1 calc PR A 1 C321 C 0.7055(2) 0.0044(2) 0.19376(14) 0.0330(6) Uani 0.771(11) 1 d P A 1 H32A H 0.7915 0.0267 0.2098 0.049 Uiso 0.771(11) 1 calc PR A 1 H32B H 0.7007 -0.0169 0.1494 0.049 Uiso 0.771(11) 1 calc PR A 1 H32C H 0.6808 -0.0608 0.2179 0.049 Uiso 0.771(11) 1 calc PR A 1 C331 C 0.6316(3) 0.1565(4) 0.28405(13) 0.0442(8) Uani 0.771(11) 1 d P A 1 H33A H 0.7209 0.1735 0.2949 0.066 Uiso 0.771(11) 1 calc PR A 1 H33B H 0.6096 0.0905 0.3083 0.066 Uiso 0.771(11) 1 calc PR A 1 H33C H 0.5820 0.2226 0.2938 0.066 Uiso 0.771(11) 1 calc PR A 1 P1A P 0.59891(3) 0.12508(3) 0.201756(16) 0.02182(6) Uani 0.229(11) 1 d P A 2 C312 C 0.6846(14) 0.199(3) 0.1503(7) 0.089(8) Uani 0.229(11) 1 d PU A 2 H31D H 0.6515 0.2762 0.1439 0.133 Uiso 0.229(11) 1 calc PR A 2 H31E H 0.6770 0.1587 0.1100 0.133 Uiso 0.229(11) 1 calc PR A 2 H31F H 0.7729 0.2021 0.1685 0.133 Uiso 0.229(11) 1 calc PR A 2 C322 C 0.6788(14) 0.0068(14) 0.235(2) 0.151(17) Uani 0.229(11) 1 d P A 2 H32D H 0.7589 0.0311 0.2585 0.227 Uiso 0.229(11) 1 calc PR A 2 H32E H 0.6942 -0.0467 0.2021 0.227 Uiso 0.229(11) 1 calc PR A 2 H32F H 0.6284 -0.0306 0.2640 0.227 Uiso 0.229(11) 1 calc PR A 2 C332 C 0.6196(11) 0.228(3) 0.2712(8) 0.082(7) Uani 0.229(11) 1 d P A 2 H33D H 0.5820 0.3022 0.2581 0.123 Uiso 0.229(11) 1 calc PR A 2 H33E H 0.7091 0.2389 0.2857 0.123 Uiso 0.229(11) 1 calc PR A 2 H33F H 0.5784 0.1974 0.3055 0.123 Uiso 0.229(11) 1 calc PR A 2 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 0.01906(4) 0.01095(4) 0.01504(4) -0.00056(3) 0.00373(3) -0.00147(3) Ru2 0.01802(4) 0.01297(4) 0.01569(4) 0.00024(3) 0.00157(3) -0.00096(3) Ru3 0.01733(4) 0.01185(4) 0.01798(4) 0.00007(3) 0.00300(3) -0.00223(3) C1 0.0182(5) 0.0137(4) 0.0192(5) 0.0004(4) 0.0049(4) -0.0013(4) B3 0.0180(5) 0.0155(5) 0.0205(6) 0.0000(4) 0.0029(4) -0.0018(4) B4 0.0194(5) 0.0189(6) 0.0207(6) 0.0023(5) 0.0069(5) -0.0007(4) B5 0.0221(6) 0.0194(6) 0.0170(6) 0.0015(4) 0.0043(5) -0.0008(4) B6 0.0178(5) 0.0168(5) 0.0183(6) 0.0006(4) 0.0039(4) -0.0010(4) B7 0.0178(5) 0.0152(5) 0.0177(5) -0.0008(4) 0.0025(4) -0.0010(4) B8 0.0190(5) 0.0178(5) 0.0207(6) -0.0005(5) 0.0045(4) -0.0005(4) B9 0.0223(6) 0.0214(6) 0.0183(6) 0.0002(5) 0.0060(5) 0.0013(5) B10 0.0198(5) 0.0186(6) 0.0176(6) -0.0006(4) 0.0028(4) -0.0005(4) B11 0.0188(5) 0.0152(5) 0.0167(5) -0.0010(4) 0.0037(4) -0.0015(4) B12 0.0201(5) 0.0160(5) 0.0194(6) -0.0021(4) 0.0041(4) -0.0008(4) C11 0.0377(7) 0.0159(5) 0.0223(6) -0.0009(4) 0.0002(5) -0.0016(5) O11 0.0712(9) 0.0236(5) 0.0283(6) -0.0063(4) -0.0141(6) -0.0005(6) C12 0.0281(6) 0.0154(5) 0.0228(6) -0.0003(4) 0.0081(5) -0.0013(4) O12 0.0313(5) 0.0264(5) 0.0386(6) -0.0013(4) 0.0167(4) 0.0026(4) C13 0.0233(5) 0.0184(5) 0.0225(6) 0.0023(4) 0.0051(4) 0.0001(4) O13 0.0377(6) 0.0344(6) 0.0228(5) 0.0036(4) 0.0099(4) 0.0010(4) C14 0.0221(5) 0.0183(5) 0.0261(6) -0.0009(4) 0.0032(4) -0.0009(4) O14 0.0328(5) 0.0175(4) 0.0472(7) -0.0012(4) 0.0047(5) 0.0025(4) C15 0.0191(5) 0.0180(5) 0.0277(6) 0.0014(4) 0.0021(4) -0.0007(4) O15 0.0300(5) 0.0157(4) 0.0507(7) 0.0001(4) 0.0005(5) -0.0003(4) C16 0.0228(5) 0.0179(5) 0.0230(6) 0.0034(4) 0.0041(4) -0.0004(4) O16 0.0371(5) 0.0297(5) 0.0254(5) 0.0024(4) 0.0110(4) 0.0024(4) C17 0.0241(5) 0.0142(5) 0.0242(6) -0.0019(4) 0.0032(4) -0.0026(4) O17 0.0248(5) 0.0226(5) 0.0407(6) -0.0014(4) -0.0035(4) 0.0004(4) S 0.02014(12) 0.01348(12) 0.02459(14) 0.00177(10) 0.00713(11) 0.00037(9) C21 0.0252(6) 0.0155(5) 0.0253(6) -0.0034(4) 0.0076(5) -0.0010(4) C22 0.0312(6) 0.0171(5) 0.0289(7) 0.0070(5) 0.0058(5) 0.0015(5) P1 0.02137(14) 0.02392(16) 0.01909(14) 0.00058(12) -0.00121(11) -0.00407(11) C311 0.0242(10) 0.0316(12) 0.045(2) 0.0104(10) -0.0013(12) -0.0080(8) C321 0.0214(9) 0.0281(11) 0.0473(15) -0.0026(9) -0.0033(8) 0.0015(7) C331 0.0342(12) 0.077(2) 0.0195(10) -0.0145(12) -0.0018(8) -0.0076(14) P1A 0.02137(14) 0.02392(16) 0.01909(14) 0.00058(12) -0.00121(11) -0.00407(11) C312 0.027(5) 0.21(2) 0.030(6) 0.025(10) -0.001(4) -0.046(10) C322 0.035(6) 0.063(9) 0.33(5) 0.095(17) -0.058(14) -0.005(6) C332 0.034(5) 0.16(2) 0.052(8) -0.048(10) -0.012(5) -0.025(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 C11 1.9014(14) . ? Ru1 C12 1.9075(13) . ? Ru1 C1 2.2419(12) . ? Ru1 B11 2.2422(13) . ? Ru1 B6 2.2431(14) . ? Ru1 B7 2.2442(13) . ? Ru1 B3 2.2450(13) . ? Ru1 Ru3 2.73905(17) . ? Ru1 Ru2 2.79383(16) . ? Ru2 C13 1.8600(13) . ? Ru2 C14 1.8693(13) . ? Ru2 H7 1.901(18) . ? Ru2 P1 2.3761(4) . ? Ru2 B7 2.4174(14) . ? Ru2 Ru3 2.8078(2) . ? Ru3 H11 1.773(18) . ? Ru3 C16 1.8946(14) . ? Ru3 C15 1.9052(13) . ? Ru3 C17 1.9409(13) . ? Ru3 B11 2.3483(13) . ? C1 B4 1.7089(17) . ? C1 B5 1.7190(19) . ? C1 B6 1.7480(17) . ? C1 B3 1.7516(18) . ? C1 S 1.8026(12) . ? B3 B8 1.786(2) . ? B3 B4 1.795(2) . ? B3 B7 1.8296(19) . ? B4 B9 1.771(2) . ? B4 B8 1.778(2) . ? B4 B5 1.779(2) . ? B5 B10 1.770(2) . ? B5 B9 1.773(2) . ? B5 B6 1.7986(19) . ? B6 B10 1.7928(19) . ? B6 B11 1.8186(19) . ? B7 H7 1.185(17) . ? B7 B11 1.7727(19) . ? B7 B12 1.775(2) . ? B7 B8 1.7806(19) . ? B8 B12 1.7890(19) . ? B8 B9 1.795(2) . ? B9 B12 1.767(2) . ? B9 B10 1.7916(19) . ? B10 B11 1.779(2) . ? B10 B12 1.791(2) . ? B11 H11 1.195(17) . ? B11 B12 1.7728(18) . ? C11 O11 1.1496(18) . ? C12 O12 1.1487(16) . ? C13 O13 1.1501(17) . ? C14 O14 1.1405(16) . ? C15 O15 1.1427(16) . ? C16 O16 1.1430(17) . ? C17 O17 1.1369(17) . ? S C21 1.7925(14) . ? S C22 1.8011(14) . ? P1 C331 1.795(3) . ? P1 C311 1.816(3) . ? P1 C321 1.845(2) . ? 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 C11 Ru1 C12 89.17(6) . . ? C11 Ru1 C1 116.14(5) . . ? C12 Ru1 C1 105.25(5) . . ? C11 Ru1 B11 148.35(6) . . ? C12 Ru1 B11 115.48(5) . . ? C1 Ru1 B11 77.93(5) . . ? C11 Ru1 B6 159.81(5) . . ? C12 Ru1 B6 88.17(5) . . ? C1 Ru1 B6 45.88(4) . . ? B11 Ru1 B6 47.84(5) . . ? C11 Ru1 B7 105.99(6) . . ? C12 Ru1 B7 161.26(5) . . ? C1 Ru1 B7 78.28(5) . . ? B11 Ru1 B7 46.55(5) . . ? B6 Ru1 B7 81.26(5) . . ? C11 Ru1 B3 89.43(6) . . ? C12 Ru1 B3 145.38(5) . . ? C1 Ru1 B3 45.96(5) . . ? B11 Ru1 B3 81.07(5) . . ? B6 Ru1 B3 81.52(5) . . ? B7 Ru1 B3 48.10(5) . . ? C11 Ru1 Ru3 114.27(4) . . ? C12 Ru1 Ru3 81.53(4) . . ? C1 Ru1 Ru3 129.14(3) . . ? B11 Ru1 Ru3 55.17(3) . . ? B6 Ru1 Ru3 85.11(3) . . ? B7 Ru1 Ru3 82.18(3) . . ? B3 Ru1 Ru3 129.82(3) . . ? C11 Ru1 Ru2 70.91(4) . . ? C12 Ru1 Ru2 121.90(4) . . ? C1 Ru1 Ru2 132.72(3) . . ? B11 Ru1 Ru2 78.92(4) . . ? B6 Ru1 Ru2 126.74(3) . . ? B7 Ru1 Ru2 56.08(4) . . ? B3 Ru1 Ru2 90.05(4) . . ? Ru3 Ru1 Ru2 60.983(5) . . ? C13 Ru2 C14 89.46(6) . . ? C13 Ru2 H7 173.6(5) . . ? C14 Ru2 H7 90.6(5) . . ? C13 Ru2 P1 90.11(4) . . ? C14 Ru2 P1 94.70(4) . . ? H7 Ru2 P1 83.5(5) . . ? C13 Ru2 B7 154.24(5) . . ? C14 Ru2 B7 114.11(5) . . ? H7 Ru2 B7 28.8(5) . . ? P1 Ru2 B7 97.76(3) . . ? C13 Ru2 Ru1 104.08(4) . . ? C14 Ru2 Ru1 147.40(4) . . ? H7 Ru2 Ru1 79.2(5) . . ? P1 Ru2 Ru1 114.436(10) . . ? B7 Ru2 Ru1 50.38(3) . . ? C13 Ru2 Ru3 91.68(4) . . ? C14 Ru2 Ru3 92.10(4) . . ? H7 Ru2 Ru3 94.7(5) . . ? P1 Ru2 Ru3 172.980(10) . . ? B7 Ru2 Ru3 77.83(3) . . ? Ru1 Ru2 Ru3 58.545(4) . . ? H11 Ru3 C16 175.8(6) . . ? H11 Ru3 C15 88.2(5) . . ? C16 Ru3 C15 95.85(6) . . ? H11 Ru3 C17 89.2(6) . . ? C16 Ru3 C17 91.15(6) . . ? C15 Ru3 C17 101.71(5) . . ? H11 Ru3 B11 29.7(5) . . ? C16 Ru3 B11 146.04(5) . . ? C15 Ru3 B11 116.13(5) . . ? C17 Ru3 B11 93.08(5) . . ? H11 Ru3 Ru1 81.2(6) . . ? C16 Ru3 Ru1 94.61(4) . . ? C15 Ru3 Ru1 153.41(4) . . ? C17 Ru3 Ru1 102.44(4) . . ? B11 Ru3 Ru1 51.61(3) . . ? H11 Ru3 Ru2 88.8(6) . . ? C16 Ru3 Ru2 89.68(4) . . ? C15 Ru3 Ru2 95.19(4) . . ? C17 Ru3 Ru2 162.90(4) . . ? B11 Ru3 Ru2 76.97(3) . . ? Ru1 Ru3 Ru2 60.472(4) . . ? B4 C1 B5 62.51(8) . . ? B4 C1 B6 113.98(9) . . ? B5 C1 B6 62.49(8) . . ? B4 C1 B3 62.46(8) . . ? B5 C1 B3 114.02(9) . . ? B6 C1 B3 113.72(9) . . ? B4 C1 S 119.04(8) . . ? B5 C1 S 113.89(8) . . ? B6 C1 S 114.62(8) . . ? B3 C1 S 123.03(8) . . ? B4 C1 Ru1 124.28(8) . . ? B5 C1 Ru1 124.32(8) . . ? B6 C1 Ru1 67.10(6) . . ? B3 C1 Ru1 67.11(6) . . ? S C1 Ru1 107.23(6) . . ? C1 B3 B8 104.02(10) . . ? C1 B3 B4 57.60(7) . . ? B8 B3 B4 59.55(8) . . ? C1 B3 B7 104.48(9) . . ? B8 B3 B7 58.99(7) . . ? B4 B3 B7 106.06(9) . . ? C1 B3 Ru1 66.93(6) . . ? B8 B3 Ru1 119.51(8) . . ? B4 B3 Ru1 119.78(8) . . ? B7 B3 Ru1 65.92(6) . . ? C1 B4 B9 105.92(9) . . ? C1 B4 B8 106.17(9) . . ? B9 B4 B8 60.76(8) . . ? C1 B4 B5 59.03(7) . . ? B9 B4 B5 59.96(8) . . ? B8 B4 B5 108.67(10) . . ? C1 B4 B3 59.94(7) . . ? B9 B4 B3 109.10(10) . . ? B8 B4 B3 59.99(8) . . ? B5 B4 B3 109.12(9) . . ? C1 B5 B10 106.05(9) . . ? C1 B5 B9 105.36(10) . . ? B10 B5 B9 60.75(8) . . ? C1 B5 B4 58.47(7) . . ? B10 B5 B4 108.40(10) . . ? B9 B5 B4 59.80(8) . . ? C1 B5 B6 59.54(7) . . ? B10 B5 B6 60.31(8) . . ? B9 B5 B6 108.97(10) . . ? B4 B5 B6 108.27(10) . . ? C1 B6 B10 103.85(9) . . ? C1 B6 B5 57.97(7) . . ? B10 B6 B5 59.05(8) . . ? C1 B6 B11 104.47(9) . . ? B10 B6 B11 59.03(7) . . ? B5 B6 B11 105.87(9) . . ? C1 B6 Ru1 67.03(6) . . ? B10 B6 Ru1 119.67(8) . . ? B5 B6 Ru1 120.21(8) . . ? B11 B6 Ru1 66.06(6) . . ? H7 B7 B11 120.4(8) . . ? H7 B7 B12 104.7(9) . . ? B11 B7 B12 59.95(7) . . ? H7 B7 B8 110.0(9) . . ? B11 B7 B8 108.26(10) . . ? B12 B7 B8 60.41(8) . . ? H7 B7 B3 130.5(8) . . ? B11 B7 B3 108.10(9) . . ? B12 B7 B3 107.71(9) . . ? B8 B7 B3 59.28(7) . . ? H7 B7 Ru1 124.1(9) . . ? B11 B7 Ru1 66.67(6) . . ? B12 B7 Ru1 120.66(8) . . ? B8 B7 Ru1 119.81(8) . . ? B3 B7 Ru1 65.97(6) . . ? H7 B7 Ru2 50.6(9) . . ? B11 B7 Ru2 99.67(7) . . ? B12 B7 Ru2 137.33(8) . . ? B8 B7 Ru2 151.96(8) . . ? B3 B7 Ru2 114.47(8) . . ? Ru1 B7 Ru2 73.54(4) . . ? B4 B8 B7 108.92(9) . . ? B4 B8 B3 60.46(8) . . ? B7 B8 B3 61.72(8) . . ? B4 B8 B12 106.96(10) . . ? B7 B8 B12 59.65(8) . . ? B3 B8 B12 109.05(9) . . ? B4 B8 B9 59.41(8) . . ? B7 B8 B9 107.41(9) . . ? B3 B8 B9 108.40(10) . . ? B12 B8 B9 59.09(8) . . ? B12 B9 B4 108.25(10) . . ? B12 B9 B5 108.27(10) . . ? B4 B9 B5 60.24(8) . . ? B12 B9 B10 60.42(8) . . ? B4 B9 B10 107.79(9) . . ? B5 B9 B10 59.53(8) . . ? B12 B9 B8 60.29(8) . . ? B4 B9 B8 59.82(8) . . ? B5 B9 B8 108.15(10) . . ? B10 B9 B8 108.27(10) . . ? B5 B10 B11 108.83(10) . . ? B5 B10 B12 107.38(9) . . ? B11 B10 B12 59.55(8) . . ? B5 B10 B9 59.72(8) . . ? B11 B10 B9 107.15(10) . . ? B12 B10 B9 59.11(8) . . ? B5 B10 B6 60.64(8) . . ? B11 B10 B6 61.21(8) . . ? B12 B10 B6 108.72(10) . . ? B9 B10 B6 108.42(10) . . ? H11 B11 B7 118.1(9) . . ? H11 B11 B12 106.6(9) . . ? B7 B11 B12 60.10(8) . . ? H11 B11 B10 113.3(9) . . ? B7 B11 B10 108.88(9) . . ? B12 B11 B10 60.55(8) . . ? H11 B11 B6 130.9(8) . . ? B7 B11 B6 108.90(9) . . ? B12 B11 B6 108.37(9) . . ? B10 B11 B6 59.76(8) . . ? H11 B11 Ru1 120.3(9) . . ? B7 B11 Ru1 66.78(6) . . ? B12 B11 Ru1 120.89(8) . . ? B10 B11 Ru1 120.37(8) . . ? B6 B11 Ru1 66.11(6) . . ? H11 B11 Ru3 47.4(9) . . ? B7 B11 Ru3 105.38(8) . . ? B12 B11 Ru3 143.39(9) . . ? B10 B11 Ru3 145.73(8) . . ? B6 B11 Ru3 108.18(7) . . ? Ru1 B11 Ru3 73.22(4) . . ? B9 B12 B11 108.52(10) . . ? B9 B12 B7 108.86(10) . . ? B11 B12 B7 59.95(7) . . ? B9 B12 B8 60.62(8) . . ? B11 B12 B8 107.88(9) . . ? B7 B12 B8 59.94(8) . . ? B9 B12 B10 60.46(8) . . ? B11 B12 B10 59.90(8) . . ? B7 B12 B10 108.24(9) . . ? B8 B12 B10 108.56(10) . . ? O11 C11 Ru1 172.95(13) . . ? O12 C12 Ru1 177.13(13) . . ? O13 C13 Ru2 175.44(12) . . ? O14 C14 Ru2 177.58(13) . . ? O15 C15 Ru3 177.78(13) . . ? O16 C16 Ru3 174.70(12) . . ? O17 C17 Ru3 177.82(12) . . ? C21 S C22 98.97(7) . . ? C21 S C1 105.07(6) . . ? C22 S C1 108.48(6) . . ? C331 P1 C311 103.21(16) . . ? C331 P1 C321 101.94(16) . . ? C311 P1 C321 100.58(14) . . ? C331 P1 Ru2 115.96(10) . . ? C311 P1 Ru2 120.14(12) . . ? C321 P1 Ru2 112.47(8) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 37.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.582 _refine_diff_density_min -0.581 _refine_diff_density_rms 0.126 #============================================================================== data_5 _database_code_depnum_ccdc_archive 'CCDC 268994' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H49 B10 O7 P Ru3 S C H2 Cl2' _chemical_formula_sum 'C29 H51 B10 Cl2 O7 P Ru3 S' _chemical_formula_weight 1056.94 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P-1 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.878(4) _cell_length_b 19.443(8) _cell_length_c 19.706(7) _cell_angle_alpha 107.28(2) _cell_angle_beta 100.15(2) _cell_angle_gamma 94.40(2) _cell_volume 4237(3) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 4368 _cell_measurement_theta_min 2.63 _cell_measurement_theta_max 31.48 _exptl_crystal_description block _exptl_crystal_colour yellow-orange _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.657 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2112 _exptl_absorpt_coefficient_mu 1.310 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.682 _exptl_absorpt_correction_T_max 0.875 _exptl_absorpt_process_details 'SADABS (Bruker, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(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 'Bruker-Nonius X8 Apex CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 62894 _diffrn_reflns_av_R_equivalents 0.0670 _diffrn_reflns_av_sigmaI/netI 0.1029 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.29 _diffrn_reflns_theta_max 31.82 _reflns_number_total 27629 _reflns_number_gt 17069 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2 (Bruker, 2003)' _computing_cell_refinement 'Bruker APEX2 (Bruker, 2003)' _computing_data_reduction 'Bruker APEX2 (Bruker, 2003)' _computing_structure_solution 'Bruker SHELXTL (Bruker, 2000)' _computing_structure_refinement 'Bruker SHELXTL (Bruker, 2000)' _computing_molecular_graphics 'Bruker SHELXTL (Bruker, 2000)' _computing_publication_material 'Bruker SHELXTL (Bruker, 2000)' _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^)+(0.0312P)^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 27629 _refine_ls_number_parameters 1019 _refine_ls_number_restraints 40 _refine_ls_R_factor_all 0.0759 _refine_ls_R_factor_gt 0.0435 _refine_ls_wR_factor_ref 0.1044 _refine_ls_wR_factor_gt 0.0950 _refine_ls_goodness_of_fit_ref 0.878 _refine_ls_restrained_S_all 0.878 _refine_ls_shift/su_max 0.013 _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 0.21373(2) 0.857292(13) 0.163712(14) 0.01175(5) Uani 1 1 d . . . Ru2 Ru 0.07660(2) 0.969491(14) 0.160644(14) 0.01449(5) Uani 1 1 d D . . Ru3 Ru 0.22654(2) 0.963347(13) 0.296907(14) 0.01186(5) Uani 1 1 d D A . C1 C 0.3491(3) 0.82984(18) 0.09460(18) 0.0152(6) Uani 1 1 d . . . B3 B 0.2431(3) 0.8727(2) 0.0586(2) 0.0153(7) Uani 1 1 d . . . H3 H 0.1668 0.8434 0.0143 0.018 Uiso 1 1 calc R . . B4 B 0.3848(4) 0.8777(2) 0.0383(2) 0.0200(7) Uani 1 1 d . . . H4 H 0.3989 0.8520 -0.0179 0.024 Uiso 1 1 calc R . . B5 B 0.4855(3) 0.8770(2) 0.1156(2) 0.0202(7) Uani 1 1 d . . . H5 H 0.5655 0.8507 0.1102 0.024 Uiso 1 1 calc R . . B6 B 0.4089(3) 0.8728(2) 0.1866(2) 0.0161(7) Uani 1 1 d . . . H6 H 0.4412 0.8441 0.2262 0.019 Uiso 1 1 calc R . . B7 B 0.2414(3) 0.9572(2) 0.1318(2) 0.0159(7) Uani 1 1 d . . . H99 H 0.139(3) 1.018(2) 0.2539(18) 0.019 Uiso 1 1 d D . . B8 B 0.3176(4) 0.9575(2) 0.0612(2) 0.0198(7) Uani 1 1 d . . . H8 H 0.2863 0.9843 0.0197 0.024 Uiso 1 1 calc R . . B9 B 0.4682(4) 0.9606(2) 0.0961(2) 0.0215(8) Uani 1 1 d . . . H9 H 0.5365 0.9900 0.0784 0.026 Uiso 1 1 calc R . . B10 B 0.4846(3) 0.9578(2) 0.1883(2) 0.0192(7) Uani 1 1 d . . . H10 H 0.5642 0.9849 0.2308 0.023 Uiso 1 1 calc R . . B11 B 0.3449(3) 0.9562(2) 0.2096(2) 0.0154(7) Uani 1 1 d . . . H11 H 0.351(4) 1.002(2) 0.272(2) 0.019 Uiso 1 1 d . . . B12 B 0.3800(4) 1.0083(2) 0.1538(2) 0.0191(7) Uani 1 1 d . . . H12 H 0.3911 1.0692 0.1736 0.023 Uiso 1 1 calc R . . C11 C 0.2119(3) 0.79770(18) 0.22473(19) 0.0171(6) Uani 1 1 d . . . O11 O 0.2130(3) 0.76218(14) 0.26209(15) 0.0258(6) Uani 1 1 d . . . C12 C 0.0619(3) 0.80963(18) 0.11626(19) 0.0175(6) Uani 1 1 d . . . O12 O -0.0264(2) 0.77657(16) 0.08572(17) 0.0302(6) Uani 1 1 d . . . C13 C 0.0122(3) 0.93731(19) 0.0594(2) 0.0206(7) Uani 1 1 d . . . O13 O -0.0263(3) 0.91922(16) -0.00083(15) 0.0303(6) Uani 1 1 d . . . C14 C -0.0747(3) 0.9495(2) 0.1878(2) 0.0265(8) Uani 1 1 d . . . O14 O -0.1659(3) 0.9379(2) 0.1962(2) 0.0500(10) Uani 1 1 d . . . C15 C 0.0870(4) 1.0665(2) 0.1615(2) 0.0267(8) Uani 1 1 d . . . O15 O 0.0986(4) 1.12555(17) 0.16279(19) 0.0471(10) Uani 1 1 d . . . C16 C 0.0921(3) 0.92042(19) 0.3156(2) 0.0190(7) Uani 1 1 d . . . O16 O 0.0112(2) 0.89203(16) 0.32546(17) 0.0287(6) Uani 1 1 d . . . C17 C 0.3259(3) 0.91949(18) 0.35316(19) 0.0185(6) Uani 1 1 d . . . O17 O 0.3874(3) 0.89386(16) 0.38620(16) 0.0304(7) Uani 1 1 d . . . S1 S 0.36254(8) 0.73535(5) 0.04837(5) 0.01785(16) Uani 1 1 d . . . C21 C 0.3966(4) 0.6955(2) 0.1184(2) 0.0284(8) Uani 1 1 d . . . H21A H 0.3357 0.7003 0.1465 0.043 Uiso 1 1 calc R . . H21B H 0.4704 0.7204 0.1505 0.043 Uiso 1 1 calc R . . H21C H 0.4025 0.6439 0.0968 0.043 Uiso 1 1 calc R . . C22 C 0.2193(4) 0.6900(2) 0.0077(3) 0.0349(10) Uani 1 1 d . . . H22A H 0.2210 0.6376 -0.0115 0.052 Uiso 1 1 calc R . . H22B H 0.1869 0.7080 -0.0321 0.052 Uiso 1 1 calc R . . H22C H 0.1713 0.6996 0.0442 0.052 Uiso 1 1 calc R . . P1 P 0.24806(7) 1.07402(4) 0.39335(4) 0.01246(15) Uani 1 1 d . . . C31A C 0.2272(4) 1.0707(2) 0.4849(2) 0.0233(7) Uani 0.842(7) 1 d P A 1 H31A H 0.1459 1.0805 0.4860 0.028 Uiso 0.842(7) 1 calc PR A 1 C32A C 0.2305(4) 0.9972(2) 0.4969(2) 0.0226(10) Uani 0.842(7) 1 d P A 1 H32A H 0.3100 0.9846 0.4995 0.027 Uiso 0.842(7) 1 calc PR A 1 H32B H 0.1789 0.9594 0.4554 0.027 Uiso 0.842(7) 1 calc PR A 1 C33A C 0.1914(5) 0.9991(3) 0.5681(3) 0.0357(10) Uani 0.842(7) 1 d P A 1 H33A H 0.1092 1.0066 0.5630 0.043 Uiso 0.842(7) 1 calc PR A 1 H33B H 0.1978 0.9516 0.5762 0.043 Uiso 0.842(7) 1 calc PR A 1 C34A C 0.2614(5) 1.0579(3) 0.6327(3) 0.0391(11) Uani 0.842(7) 1 d P A 1 H34A H 0.2290 1.0590 0.6759 0.047 Uiso 0.842(7) 1 calc PR A 1 H34B H 0.3415 1.0467 0.6420 0.047 Uiso 0.842(7) 1 calc PR A 1 C35A C 0.2638(5) 1.1313(3) 0.6227(2) 0.0277(11) Uani 0.842(7) 1 d P A 1 H35A H 0.3184 1.1671 0.6642 0.033 Uiso 0.842(7) 1 calc PR A 1 H35B H 0.1861 1.1465 0.6222 0.033 Uiso 0.842(7) 1 calc PR A 1 C36A C 0.3007(4) 1.1309(2) 0.5509(2) 0.0287(8) Uani 0.842(7) 1 d P A 1 H36A H 0.2932 1.1786 0.5436 0.034 Uiso 0.842(7) 1 calc PR A 1 H36B H 0.3829 1.1236 0.5548 0.034 Uiso 0.842(7) 1 calc PR A 1 C31B C 0.2272(4) 1.0707(2) 0.4849(2) 0.0233(7) Uani 0.158(7) 1 d PU A 2 H31B H 0.2820 1.0345 0.4873 0.028 Uiso 0.158(7) 1 calc PR A 2 C32B C 0.149(2) 1.0353(15) 0.4994(13) 0.026(5) Uani 0.158(7) 1 d PU A 2 H32C H 0.1111 0.9951 0.4549 0.031 Uiso 0.158(7) 1 calc PR A 2 H32D H 0.0898 1.0673 0.5130 0.031 Uiso 0.158(7) 1 calc PR A 2 C33B C 0.1914(5) 0.9991(3) 0.5681(3) 0.0357(10) Uani 0.158(7) 1 d PU A 2 H33C H 0.1228 0.9783 0.5812 0.043 Uiso 0.158(7) 1 calc PR A 2 H33D H 0.2381 0.9597 0.5517 0.043 Uiso 0.158(7) 1 calc PR A 2 C34B C 0.2614(5) 1.0579(3) 0.6327(3) 0.0391(11) Uani 0.158(7) 1 d PU A 2 H34C H 0.2078 1.0873 0.6581 0.047 Uiso 0.158(7) 1 calc PR A 2 H34D H 0.3024 1.0348 0.6665 0.047 Uiso 0.158(7) 1 calc PR A 2 C35B C 0.341(2) 1.1042(15) 0.6192(14) 0.028(5) Uani 0.158(7) 1 d PU A 2 H35C H 0.4102 1.0796 0.6122 0.033 Uiso 0.158(7) 1 calc PR A 2 H35D H 0.3651 1.1476 0.6629 0.033 Uiso 0.158(7) 1 calc PR A 2 C36B C 0.3007(4) 1.1309(2) 0.5509(2) 0.0287(8) Uani 0.158(7) 1 d PU A 2 H36C H 0.2555 1.1715 0.5652 0.034 Uiso 0.158(7) 1 calc PR A 2 H36D H 0.3699 1.1496 0.5368 0.034 Uiso 0.158(7) 1 calc PR A 2 C41 C 0.1421(3) 1.13439(18) 0.37277(18) 0.0147(6) Uani 1 1 d . A . H41 H 0.1494 1.1391 0.3245 0.018 Uiso 1 1 calc R . . C42 C 0.1605(3) 1.21212(19) 0.4259(2) 0.0206(7) Uani 1 1 d . . . H42A H 0.1486 1.2106 0.4739 0.025 Uiso 1 1 calc R A . H42B H 0.2409 1.2346 0.4321 0.025 Uiso 1 1 calc R . . C43 C 0.0766(4) 1.2586(2) 0.3980(2) 0.0288(9) Uani 1 1 d . A . H43A H 0.0883 1.3079 0.4339 0.035 Uiso 1 1 calc R . . H43B H 0.0926 1.2634 0.3519 0.035 Uiso 1 1 calc R . . C44 C -0.0475(4) 1.2243(2) 0.3857(2) 0.0306(9) Uani 1 1 d . . . H44A H -0.0999 1.2532 0.3644 0.037 Uiso 1 1 calc R A . H44B H -0.0662 1.2250 0.4329 0.037 Uiso 1 1 calc R . . C45 C -0.0672(3) 1.1461(2) 0.3348(2) 0.0274(8) Uani 1 1 d . A . H45A H -0.0566 1.1459 0.2861 0.033 Uiso 1 1 calc R . . H45B H -0.1475 1.1243 0.3300 0.033 Uiso 1 1 calc R . . C46 C 0.0168(3) 1.1001(2) 0.3636(2) 0.0206(7) Uani 1 1 d . . . H46A H 0.0037 1.0500 0.3291 0.025 Uiso 1 1 calc R A . H46B H 0.0031 1.0975 0.4109 0.025 Uiso 1 1 calc R . . C51 C 0.3890(3) 1.12999(18) 0.40839(19) 0.0169(6) Uani 1 1 d . A . H51 H 0.3930 1.1738 0.4515 0.020 Uiso 1 1 calc R . . C52 C 0.4004(3) 1.1576(2) 0.3438(2) 0.0211(7) Uani 1 1 d . . . H52A H 0.3966 1.1156 0.2999 0.025 Uiso 1 1 calc R A . H52B H 0.3353 1.1845 0.3340 0.025 Uiso 1 1 calc R . . C53 C 0.5140(3) 1.2073(2) 0.3599(3) 0.0304(9) Uani 1 1 d . A . H53A H 0.5144 1.2518 0.4007 0.037 Uiso 1 1 calc R . . H53B H 0.5213 1.2220 0.3167 0.037 Uiso 1 1 calc R . . C54 C 0.6171(4) 1.1686(2) 0.3797(3) 0.0415(12) Uani 1 1 d . . . H54A H 0.6210 1.1264 0.3375 0.050 Uiso 1 1 calc R A . H54B H 0.6898 1.2025 0.3923 0.050 Uiso 1 1 calc R . . C55 C 0.6033(3) 1.1431(2) 0.4440(3) 0.0380(11) Uani 1 1 d . A . H55A H 0.6024 1.1857 0.4865 0.046 Uiso 1 1 calc R . . H55B H 0.6700 1.1186 0.4569 0.046 Uiso 1 1 calc R . . C56 C 0.4918(3) 1.0907(2) 0.4266(2) 0.0255(8) Uani 1 1 d . . . H56A H 0.4850 1.0743 0.4688 0.031 Uiso 1 1 calc R A . H56B H 0.4926 1.0475 0.3847 0.031 Uiso 1 1 calc R . . Ru11 Ru 0.24802(2) 0.353573(13) 0.163230(13) 0.01145(5) Uani 1 1 d . . . Ru12 Ru 0.10907(2) 0.464396(14) 0.155213(14) 0.01281(5) Uani 1 1 d D . . Ru13 Ru 0.24939(2) 0.460014(13) 0.293795(13) 0.01075(5) Uani 1 1 d D . . C101 C 0.3867(3) 0.32633(18) 0.09690(18) 0.0167(6) Uani 1 1 d . . . B103 B 0.2839(3) 0.3682(2) 0.0588(2) 0.0170(7) Uani 1 1 d . . . H103 H 0.2099 0.3381 0.0131 0.020 Uiso 1 1 calc R . . B104 B 0.4272(4) 0.3751(2) 0.0422(2) 0.0205(7) Uani 1 1 d . . . H104 H 0.4451 0.3498 -0.0131 0.025 Uiso 1 1 calc R . . B105 B 0.5238(3) 0.3755(2) 0.1209(2) 0.0196(7) Uani 1 1 d . . . H105 H 0.6049 0.3499 0.1173 0.023 Uiso 1 1 calc R . . B106 B 0.4432(3) 0.3709(2) 0.1902(2) 0.0163(7) Uani 1 1 d . . . H106 H 0.4741 0.3429 0.2308 0.020 Uiso 1 1 calc R . . B107 B 0.2774(3) 0.4528(2) 0.1314(2) 0.0136(6) Uani 1 1 d . . . H199 H 0.196(3) 0.512(2) 0.2450(18) 0.016 Uiso 1 1 d D . . B108 B 0.3577(4) 0.4532(2) 0.0623(2) 0.0197(7) Uani 1 1 d . . . H108 H 0.3279 0.4794 0.0199 0.024 Uiso 1 1 calc R . . B109 B 0.5068(4) 0.4572(2) 0.1009(2) 0.0215(8) Uani 1 1 d . . . H109 H 0.5768 0.4868 0.0847 0.026 Uiso 1 1 calc R . . B110 B 0.5186(3) 0.4555(2) 0.1926(2) 0.0184(7) Uani 1 1 d . . . H110 H 0.5962 0.4831 0.2366 0.022 Uiso 1 1 calc R . . B111 B 0.3766(3) 0.45362(19) 0.2110(2) 0.0135(6) Uani 1 1 d . . . H111 H 0.369(4) 0.494(2) 0.266(2) 0.016 Uiso 1 1 d . . . B112 B 0.4160(3) 0.5052(2) 0.1553(2) 0.0179(7) Uani 1 1 d . . . H112 H 0.4266 0.5661 0.1742 0.021 Uiso 1 1 calc R . . C111 C 0.2477(3) 0.29514(19) 0.22579(19) 0.0177(6) Uani 1 1 d . . . O111 O 0.2511(3) 0.25939(15) 0.26281(16) 0.0273(6) Uani 1 1 d . . . C112 C 0.0973(3) 0.30315(18) 0.11543(19) 0.0173(6) Uani 1 1 d . . . O112 O 0.0105(2) 0.26871(15) 0.08534(16) 0.0275(6) Uani 1 1 d . . . C113 C 0.0472(3) 0.43090(18) 0.0536(2) 0.0195(7) Uani 1 1 d . . . O113 O 0.0099(3) 0.41336(16) -0.00745(16) 0.0311(6) Uani 1 1 d . . . C114 C -0.0451(3) 0.4487(2) 0.1816(2) 0.0215(7) Uani 1 1 d . . . O114 O -0.1350(3) 0.4431(2) 0.19192(19) 0.0387(8) Uani 1 1 d . . . C115 C 0.1292(3) 0.5598(2) 0.1525(2) 0.0243(8) Uani 1 1 d . . . O115 O 0.1483(3) 0.61789(16) 0.15097(19) 0.0403(8) Uani 1 1 d . . . C116 C 0.1129(3) 0.41252(18) 0.30525(19) 0.0166(6) Uani 1 1 d . . . O116 O 0.0324(2) 0.38026(15) 0.30997(16) 0.0244(6) Uani 1 1 d . . . C117 C 0.3435(3) 0.42151(18) 0.35721(18) 0.0167(6) Uani 1 1 d . . . O117 O 0.4006(3) 0.40006(17) 0.39662(16) 0.0295(6) Uani 1 1 d . . . S11 S 0.40344(8) 0.23249(5) 0.05243(5) 0.02000(17) Uani 1 1 d . . . C121 C 0.4358(5) 0.1928(2) 0.1233(3) 0.0431(13) Uani 1 1 d . . . H12A H 0.3706 0.1934 0.1477 0.065 Uiso 1 1 calc R . . H12B H 0.5050 0.2208 0.1585 0.065 Uiso 1 1 calc R . . H12C H 0.4494 0.1425 0.1025 0.065 Uiso 1 1 calc R . . C122 C 0.2621(4) 0.1876(3) 0.0079(4) 0.0601(19) Uani 1 1 d . . . H12D H 0.2653 0.1359 -0.0155 0.090 Uiso 1 1 calc R . . H12E H 0.2302 0.2094 -0.0289 0.090 Uiso 1 1 calc R . . H12F H 0.2128 0.1926 0.0436 0.090 Uiso 1 1 calc R . . P11 P 0.25594(7) 0.57122(4) 0.38741(4) 0.01150(14) Uani 1 1 d . . . C131 C 0.2669(3) 0.56253(18) 0.47974(17) 0.0152(6) Uani 1 1 d . . . H131 H 0.3468 0.5510 0.4929 0.018 Uiso 1 1 calc R . . C132 C 0.1873(3) 0.49851(19) 0.48459(19) 0.0188(6) Uani 1 1 d . . . H13A H 0.1059 0.5076 0.4758 0.023 Uiso 1 1 calc R . . H13B H 0.1945 0.4532 0.4469 0.023 Uiso 1 1 calc R . . C133 C 0.2207(3) 0.4899(2) 0.5598(2) 0.0223(7) Uani 1 1 d . . . H13C H 0.3000 0.4770 0.5665 0.027 Uiso 1 1 calc R . . H13D H 0.1680 0.4494 0.5627 0.027 Uiso 1 1 calc R . . C134 C 0.2157(4) 0.5593(2) 0.6218(2) 0.0282(8) Uani 1 1 d . . . H13E H 0.1350 0.5697 0.6188 0.034 Uiso 1 1 calc R . . H13F H 0.2429 0.5520 0.6693 0.034 Uiso 1 1 calc R . . C135 C 0.2912(4) 0.6234(2) 0.6161(2) 0.0253(8) Uani 1 1 d . . . H13G H 0.3732 0.6158 0.6259 0.030 Uiso 1 1 calc R . . H13H H 0.2820 0.6684 0.6535 0.030 Uiso 1 1 calc R . . C136 C 0.2601(3) 0.63267(19) 0.54125(19) 0.0205(7) Uani 1 1 d . . . H13I H 0.3136 0.6732 0.5390 0.025 Uiso 1 1 calc R . . H13J H 0.1809 0.6456 0.5337 0.025 Uiso 1 1 calc R . . C141 C 0.1346(3) 0.62202(17) 0.36760(17) 0.0134(6) Uani 1 1 d . . . H141 H 0.1297 0.6207 0.3160 0.016 Uiso 1 1 calc R . . C142 C 0.0173(3) 0.58277(19) 0.36852(19) 0.0172(6) Uani 1 1 d . . . H14A H 0.0099 0.5307 0.3400 0.021 Uiso 1 1 calc R . . H14B H 0.0131 0.5862 0.4191 0.021 Uiso 1 1 calc R . . C143 C -0.0817(3) 0.6172(2) 0.3360(2) 0.0213(7) Uani 1 1 d . . . H14C H -0.1564 0.5920 0.3374 0.026 Uiso 1 1 calc R . . H14D H -0.0798 0.6113 0.2846 0.026 Uiso 1 1 calc R . . C144 C -0.0716(3) 0.6984(2) 0.3784(2) 0.0251(8) Uani 1 1 d . . . H14E H -0.1341 0.7200 0.3552 0.030 Uiso 1 1 calc R . . H14F H -0.0809 0.7041 0.4287 0.030 Uiso 1 1 calc R . . C145 C 0.0452(3) 0.7384(2) 0.3804(2) 0.0248(8) Uani 1 1 d . . . H14G H 0.0513 0.7899 0.4104 0.030 Uiso 1 1 calc R . . H14H H 0.0505 0.7372 0.3305 0.030 Uiso 1 1 calc R . . C146 C 0.1463(3) 0.70404(19) 0.4120(2) 0.0206(7) Uani 1 1 d . . . H14I H 0.1460 0.7094 0.4635 0.025 Uiso 1 1 calc R . . H14J H 0.2205 0.7295 0.4099 0.025 Uiso 1 1 calc R . . C151 C 0.3847(3) 0.63621(18) 0.39729(18) 0.0148(6) Uani 1 1 d . . . H151 H 0.3827 0.6814 0.4376 0.018 Uiso 1 1 calc R . . C152 C 0.4988(3) 0.60707(18) 0.41695(19) 0.0172(6) Uani 1 1 d . . . H15A H 0.5044 0.5988 0.4646 0.021 Uiso 1 1 calc R . . H15B H 0.5002 0.5600 0.3800 0.021 Uiso 1 1 calc R . . C153 C 0.6020(3) 0.6615(2) 0.4205(2) 0.0221(7) Uani 1 1 d . . . H15C H 0.6031 0.7075 0.4597 0.027 Uiso 1 1 calc R . . H15D H 0.6745 0.6416 0.4324 0.027 Uiso 1 1 calc R . . C154 C 0.5964(3) 0.6773(2) 0.3487(2) 0.0241(7) Uani 1 1 d . . . H15E H 0.5977 0.6319 0.3094 0.029 Uiso 1 1 calc R . . H15F H 0.6641 0.7123 0.3525 0.029 Uiso 1 1 calc R . . C155 C 0.4852(3) 0.70908(19) 0.3309(2) 0.0216(7) Uani 1 1 d . . . H15G H 0.4866 0.7561 0.3688 0.026 Uiso 1 1 calc R . . H15H H 0.4801 0.7183 0.2838 0.026 Uiso 1 1 calc R . . C156 C 0.3796(3) 0.65678(19) 0.32707(19) 0.0176(6) Uani 1 1 d . . . H15I H 0.3739 0.6120 0.2856 0.021 Uiso 1 1 calc R . . H15J H 0.3092 0.6796 0.3181 0.021 Uiso 1 1 calc R . . C100 C 0.8113(5) 0.1742(3) 0.1527(3) 0.0515(14) Uani 1 1 d D . . H10A H 0.8090 0.1585 0.0998 0.062 Uiso 1 1 calc R . . H10B H 0.8907 0.1734 0.1780 0.062 Uiso 1 1 calc R . . Cl1 Cl 0.77662(16) 0.26365(9) 0.18034(12) 0.0709(5) Uani 1 1 d D . . Cl2 Cl 0.71502(16) 0.11345(10) 0.17195(11) 0.0757(6) Uani 1 1 d D . . C201 C -0.2768(9) 0.6394(5) 0.1543(5) 0.055(3) Uani 0.763(4) 1 d PD B 3 H20A H -0.2989 0.6159 0.1892 0.066 Uiso 0.763(4) 1 calc PR B 3 H20B H -0.3327 0.6178 0.1075 0.066 Uiso 0.763(4) 1 calc PR B 3 Cl3 Cl -0.1378(2) 0.62215(17) 0.14189(13) 0.0823(11) Uani 0.763(4) 1 d PD B 3 Cl4 Cl -0.2837(2) 0.73333(14) 0.18727(14) 0.0639(7) Uani 0.763(4) 1 d PD B 3 C202 C -0.186(2) 0.6876(9) 0.1598(12) 0.068(10) Uani 0.237(4) 1 d PD B 4 H20C H -0.1724 0.6716 0.1098 0.082 Uiso 0.237(4) 1 calc PR B 4 H20D H -0.1119 0.6949 0.1944 0.082 Uiso 0.237(4) 1 calc PR B 4 Cl5 Cl -0.2483(8) 0.7702(4) 0.1757(5) 0.073(3) Uani 0.237(4) 1 d PD B 4 Cl6 Cl -0.2836(11) 0.6222(6) 0.1716(6) 0.076(3) Uani 0.237(4) 1 d PD B 4 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 0.01297(11) 0.01163(11) 0.01210(11) 0.00501(9) 0.00394(9) 0.00224(8) Ru2 0.01591(12) 0.01471(12) 0.01339(12) 0.00552(9) 0.00143(9) 0.00481(9) Ru3 0.01328(11) 0.01194(11) 0.01163(11) 0.00504(9) 0.00298(9) 0.00330(9) C1 0.0160(15) 0.0157(15) 0.0158(15) 0.0061(11) 0.0054(12) 0.0038(11) B3 0.0155(16) 0.0187(17) 0.0147(16) 0.0084(13) 0.0048(13) 0.0032(13) B4 0.0199(18) 0.0210(19) 0.0209(18) 0.0089(15) 0.0067(15) -0.0011(14) B5 0.0147(17) 0.028(2) 0.0189(18) 0.0077(15) 0.0052(14) 0.0008(14) B6 0.0160(16) 0.0205(18) 0.0131(16) 0.0057(13) 0.0041(13) 0.0052(13) B7 0.0199(17) 0.0130(16) 0.0151(16) 0.0058(13) 0.0013(13) 0.0037(13) B8 0.0241(19) 0.0213(18) 0.0185(18) 0.0104(14) 0.0092(15) 0.0023(15) B9 0.0225(19) 0.025(2) 0.0198(18) 0.0104(15) 0.0087(15) -0.0016(15) B10 0.0170(17) 0.0207(18) 0.0204(18) 0.0071(14) 0.0053(14) -0.0001(14) B11 0.0154(16) 0.0143(16) 0.0170(17) 0.0055(13) 0.0039(13) 0.0013(12) B12 0.0240(19) 0.0180(18) 0.0180(18) 0.0087(14) 0.0081(15) -0.0010(14) C11 0.0214(16) 0.0145(15) 0.0182(15) 0.0061(12) 0.0086(13) 0.0049(12) O11 0.0374(16) 0.0199(13) 0.0257(14) 0.0127(11) 0.0109(12) 0.0068(11) C12 0.0200(16) 0.0164(15) 0.0160(15) 0.0054(12) 0.0033(12) 0.0014(12) O12 0.0237(14) 0.0255(14) 0.0362(16) 0.0071(12) 0.0003(12) -0.0031(11) C13 0.0212(16) 0.0157(15) 0.0243(17) 0.0073(13) 0.0008(14) 0.0039(12) O13 0.0378(16) 0.0314(15) 0.0186(13) 0.0092(11) -0.0035(12) 0.0030(12) C14 0.0210(18) 0.037(2) 0.0221(18) 0.0077(16) 0.0058(14) 0.0084(15) O14 0.0223(16) 0.088(3) 0.043(2) 0.024(2) 0.0114(15) 0.0076(17) C15 0.041(2) 0.0198(17) 0.0154(16) 0.0044(13) -0.0025(15) 0.0078(15) O15 0.083(3) 0.0173(14) 0.0322(17) 0.0088(13) -0.0120(18) 0.0045(15) C16 0.0211(16) 0.0175(16) 0.0217(17) 0.0095(13) 0.0057(13) 0.0053(13) O16 0.0246(14) 0.0285(15) 0.0382(17) 0.0178(13) 0.0095(12) 0.0001(11) C17 0.0219(16) 0.0165(15) 0.0170(15) 0.0036(12) 0.0056(13) 0.0066(12) O17 0.0351(16) 0.0318(15) 0.0263(14) 0.0121(12) 0.0007(12) 0.0185(13) S1 0.0199(4) 0.0180(4) 0.0177(4) 0.0056(3) 0.0076(3) 0.0063(3) C21 0.043(2) 0.0240(19) 0.0260(19) 0.0138(15) 0.0130(18) 0.0139(17) C22 0.0245(19) 0.0204(19) 0.045(3) -0.0056(17) -0.0030(18) 0.0053(15) P1 0.0135(4) 0.0127(4) 0.0126(4) 0.0057(3) 0.0025(3) 0.0035(3) C31A 0.035(2) 0.0188(17) 0.0157(16) 0.0065(13) 0.0030(14) 0.0012(14) C32A 0.035(2) 0.018(2) 0.021(2) 0.0099(16) 0.0130(18) 0.0060(17) C33A 0.050(3) 0.035(2) 0.032(2) 0.0195(19) 0.019(2) 0.005(2) C34A 0.050(3) 0.052(3) 0.026(2) 0.023(2) 0.016(2) 0.009(2) C35A 0.042(3) 0.025(2) 0.016(2) 0.0067(17) 0.0078(19) 0.001(2) C36A 0.040(2) 0.0260(19) 0.0189(17) 0.0073(15) 0.0060(16) -0.0050(16) C31B 0.035(2) 0.0188(17) 0.0157(16) 0.0065(13) 0.0030(14) 0.0012(14) C32B 0.024(11) 0.037(13) 0.018(10) 0.014(9) 0.004(8) -0.010(9) C33B 0.050(3) 0.035(2) 0.032(2) 0.0195(19) 0.019(2) 0.005(2) C34B 0.050(3) 0.052(3) 0.026(2) 0.023(2) 0.016(2) 0.009(2) C35B 0.032(12) 0.038(13) 0.023(11) 0.014(9) 0.021(9) 0.010(10) C36B 0.040(2) 0.0260(19) 0.0189(17) 0.0073(15) 0.0060(16) -0.0050(16) C41 0.0155(14) 0.0169(14) 0.0150(14) 0.0077(11) 0.0051(11) 0.0064(11) C42 0.0190(16) 0.0201(16) 0.0232(17) 0.0052(13) 0.0062(13) 0.0078(13) C43 0.035(2) 0.0240(19) 0.035(2) 0.0138(16) 0.0139(18) 0.0180(16) C44 0.028(2) 0.037(2) 0.034(2) 0.0147(18) 0.0115(17) 0.0217(18) C45 0.0170(16) 0.044(2) 0.0255(18) 0.0132(17) 0.0060(14) 0.0183(16) C46 0.0108(14) 0.0237(17) 0.0268(18) 0.0057(14) 0.0058(13) 0.0052(12) C51 0.0120(14) 0.0159(15) 0.0207(16) 0.0038(12) 0.0015(12) 0.0018(11) C52 0.0151(15) 0.0224(17) 0.0285(18) 0.0108(14) 0.0077(13) 0.0012(13) C53 0.0191(18) 0.0249(19) 0.048(3) 0.0092(17) 0.0147(17) -0.0023(14) C54 0.0159(18) 0.028(2) 0.073(4) 0.003(2) 0.013(2) -0.0018(15) C55 0.0127(17) 0.031(2) 0.062(3) 0.007(2) -0.0028(18) 0.0054(15) C56 0.0128(15) 0.0257(18) 0.036(2) 0.0092(16) -0.0010(14) 0.0064(13) Ru11 0.01130(11) 0.01247(11) 0.01205(11) 0.00524(9) 0.00333(8) 0.00294(8) Ru12 0.01210(11) 0.01379(12) 0.01353(11) 0.00629(9) 0.00118(9) 0.00334(9) Ru13 0.00964(11) 0.01318(11) 0.01131(11) 0.00580(9) 0.00306(8) 0.00312(8) C101 0.0180(15) 0.0175(15) 0.0160(15) 0.0061(12) 0.0045(12) 0.0049(12) B103 0.0177(17) 0.0202(18) 0.0168(17) 0.0098(14) 0.0061(14) 0.0037(14) B104 0.0220(19) 0.0232(19) 0.0208(18) 0.0096(15) 0.0097(15) 0.0067(15) B105 0.0177(18) 0.0242(19) 0.0211(18) 0.0105(15) 0.0088(14) 0.0043(14) B106 0.0149(16) 0.0173(17) 0.0178(17) 0.0061(13) 0.0050(13) 0.0037(13) B107 0.0163(16) 0.0156(16) 0.0136(15) 0.0092(13) 0.0073(13) 0.0018(13) B108 0.0239(19) 0.0235(19) 0.0175(17) 0.0122(15) 0.0088(15) 0.0049(15) B109 0.0179(18) 0.030(2) 0.0229(19) 0.0120(16) 0.0120(15) 0.0052(15) B110 0.0173(17) 0.0217(18) 0.0200(18) 0.0099(14) 0.0080(14) 0.0021(14) B111 0.0128(15) 0.0126(15) 0.0153(16) 0.0050(12) 0.0020(12) 0.0023(12) B112 0.0195(18) 0.0188(18) 0.0189(18) 0.0091(14) 0.0080(14) 0.0029(14) C111 0.0159(15) 0.0200(16) 0.0198(16) 0.0087(13) 0.0060(12) 0.0035(12) O111 0.0359(16) 0.0256(14) 0.0289(15) 0.0196(12) 0.0084(12) 0.0068(12) C112 0.0159(15) 0.0178(15) 0.0186(16) 0.0067(12) 0.0023(12) 0.0032(12) O112 0.0198(13) 0.0258(14) 0.0327(15) 0.0078(12) -0.0005(11) -0.0022(10) C113 0.0197(16) 0.0162(15) 0.0224(17) 0.0083(13) -0.0001(13) 0.0033(12) O113 0.0346(16) 0.0340(16) 0.0208(14) 0.0089(12) -0.0045(12) 0.0037(12) C114 0.0194(17) 0.0244(18) 0.0185(16) 0.0048(13) 0.0006(13) 0.0056(13) O114 0.0175(14) 0.056(2) 0.0428(19) 0.0142(16) 0.0092(13) 0.0054(13) C115 0.0295(19) 0.0195(17) 0.0204(17) 0.0061(13) -0.0041(14) 0.0042(14) O115 0.057(2) 0.0190(14) 0.0378(18) 0.0134(13) -0.0118(16) -0.0035(13) C116 0.0148(15) 0.0148(15) 0.0212(16) 0.0059(12) 0.0041(12) 0.0068(12) O116 0.0182(12) 0.0243(13) 0.0360(16) 0.0156(12) 0.0097(11) 0.0014(10) C117 0.0151(14) 0.0206(16) 0.0162(15) 0.0063(12) 0.0051(12) 0.0065(12) O117 0.0300(15) 0.0381(17) 0.0280(15) 0.0188(13) 0.0057(12) 0.0169(13) S11 0.0219(4) 0.0194(4) 0.0209(4) 0.0057(3) 0.0090(3) 0.0078(3) C121 0.079(4) 0.026(2) 0.040(3) 0.021(2) 0.029(3) 0.025(2) C122 0.024(2) 0.031(3) 0.088(4) -0.024(3) -0.008(3) 0.0063(18) P11 0.0098(3) 0.0139(4) 0.0128(4) 0.0059(3) 0.0037(3) 0.0038(3) C131 0.0168(15) 0.0172(15) 0.0139(14) 0.0066(11) 0.0053(11) 0.0039(12) C132 0.0178(16) 0.0208(16) 0.0204(16) 0.0088(13) 0.0072(13) 0.0007(12) C133 0.0224(17) 0.0266(18) 0.0264(18) 0.0173(15) 0.0104(14) 0.0056(14) C134 0.028(2) 0.044(2) 0.0207(18) 0.0171(17) 0.0122(15) 0.0100(17) C135 0.0277(19) 0.034(2) 0.0132(16) 0.0074(14) 0.0038(14) 0.0015(15) C136 0.0245(17) 0.0187(16) 0.0170(16) 0.0031(12) 0.0056(13) 0.0037(13) C141 0.0105(13) 0.0168(14) 0.0148(14) 0.0060(11) 0.0050(11) 0.0045(11) C142 0.0094(13) 0.0224(16) 0.0227(16) 0.0101(13) 0.0051(12) 0.0042(12) C143 0.0116(14) 0.0310(19) 0.0247(17) 0.0126(14) 0.0037(13) 0.0088(13) C144 0.0160(16) 0.033(2) 0.033(2) 0.0150(16) 0.0110(15) 0.0149(15) C145 0.0234(18) 0.0249(18) 0.032(2) 0.0143(16) 0.0090(15) 0.0118(15) C146 0.0174(16) 0.0194(16) 0.0266(18) 0.0072(13) 0.0071(13) 0.0065(12) C151 0.0115(14) 0.0172(15) 0.0155(14) 0.0047(11) 0.0029(11) 0.0017(11) C152 0.0103(14) 0.0187(15) 0.0212(16) 0.0055(12) 0.0008(12) 0.0030(11) C153 0.0112(14) 0.0255(18) 0.0282(18) 0.0077(14) 0.0014(13) 0.0037(12) C154 0.0114(15) 0.0263(18) 0.034(2) 0.0078(15) 0.0075(14) 0.0016(13) C155 0.0208(16) 0.0205(16) 0.0260(18) 0.0102(14) 0.0074(14) 0.0000(13) C156 0.0132(14) 0.0207(16) 0.0210(16) 0.0099(13) 0.0046(12) -0.0003(12) C100 0.056(3) 0.073(4) 0.035(3) 0.029(3) 0.008(2) 0.021(3) Cl1 0.0641(10) 0.0531(9) 0.0895(13) 0.0128(9) 0.0207(10) 0.0006(7) Cl2 0.0668(10) 0.0699(11) 0.0788(12) 0.0412(10) -0.0326(9) -0.0203(8) C201 0.054(6) 0.073(7) 0.033(4) 0.006(4) 0.002(4) 0.040(6) Cl3 0.0717(15) 0.162(3) 0.0613(13) 0.0738(16) 0.0428(12) 0.0801(18) Cl4 0.0532(12) 0.0539(14) 0.0672(14) -0.0048(11) 0.0105(10) 0.0049(10) C202 0.14(3) 0.041(13) 0.031(11) 0.005(9) 0.049(15) -0.027(15) Cl5 0.085(6) 0.039(4) 0.096(6) 0.012(4) 0.043(5) 0.004(4) Cl6 0.078(6) 0.075(6) 0.067(6) 0.040(5) -0.025(4) -0.019(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 C12 1.902(4) . ? Ru1 C11 1.903(3) . ? Ru1 B11 2.225(4) . ? Ru1 B7 2.232(4) . ? Ru1 B3 2.260(4) . ? Ru1 B6 2.261(4) . ? Ru1 C1 2.280(3) . ? Ru1 Ru3 2.7857(11) . ? Ru1 Ru2 2.8294(10) . ? Ru2 H99 1.79(3) . ? Ru2 C15 1.875(4) . ? Ru2 C13 1.899(4) . ? Ru2 C14 2.005(4) . ? Ru2 B7 2.144(4) . ? Ru2 Ru3 2.9889(11) . ? Ru3 H11 1.81(4) . ? Ru3 H99 1.82(3) . ? Ru3 C16 1.889(4) . ? Ru3 C17 1.898(3) . ? Ru3 P1 2.3711(12) . ? Ru3 B11 2.387(4) . ? C1 B5 1.717(5) . ? C1 B3 1.726(5) . ? C1 B4 1.731(5) . ? C1 B6 1.745(5) . ? C1 S1 1.826(3) . ? B3 B8 1.793(6) . ? B3 B4 1.800(5) . ? B3 B7 1.841(5) . ? B4 B5 1.768(6) . ? B4 B9 1.773(6) . ? B4 B8 1.775(6) . ? B5 B10 1.786(6) . ? B5 B9 1.795(6) . ? B5 B6 1.815(6) . ? B6 B10 1.808(6) . ? B6 B11 1.813(5) . ? B7 B12 1.768(6) . ? B7 B8 1.789(6) . ? B7 B11 1.794(5) . ? B8 B12 1.787(6) . ? B8 B9 1.790(6) . ? B9 B12 1.787(6) . ? B9 B10 1.810(6) . ? B10 B11 1.782(5) . ? B10 B12 1.806(6) . ? B11 H11 1.27(4) . ? B11 B12 1.781(5) . ? C11 O11 1.149(4) . ? C12 O12 1.149(5) . ? C13 O13 1.130(5) . ? C14 O14 1.140(5) . ? C15 O15 1.138(5) . ? C16 O16 1.146(5) . ? C17 O17 1.135(4) . ? S1 C21 1.776(4) . ? S1 C22 1.784(4) . ? P1 C51 1.852(4) . ? P1 C41 1.859(3) . ? P1 C31A 1.884(4) . ? C31A C32A 1.518(5) . ? C31A C36A 1.537(6) . ? C32A C33A 1.546(6) . ? C33A C34A 1.496(7) . ? C34A C35A 1.495(6) . ? C35A C36A 1.551(6) . ? C41 C42 1.535(5) . ? C41 C46 1.541(5) . ? C42 C43 1.533(5) . ? C43 C44 1.517(6) . ? C44 C45 1.526(6) . ? C45 C46 1.535(5) . ? C51 C56 1.534(4) . ? C51 C52 1.543(5) . ? C52 C53 1.523(5) . ? C53 C54 1.538(6) . ? C54 C55 1.521(7) . ? C55 C56 1.527(5) . ? Ru11 C112 1.908(4) . ? Ru11 C111 1.909(3) . ? Ru11 B107 2.220(4) . ? Ru11 B111 2.225(4) . ? Ru11 B106 2.261(4) . ? Ru11 B103 2.266(4) . ? Ru11 C101 2.277(3) . ? Ru11 Ru13 2.7785(11) . ? Ru11 Ru12 2.8370(10) . ? Ru12 H199 1.81(3) . ? Ru12 C115 1.869(4) . ? Ru12 C113 1.899(4) . ? Ru12 C114 2.015(4) . ? Ru12 B107 2.146(4) . ? Ru12 Ru13 2.9661(11) . ? Ru13 H199 1.67(3) . ? Ru13 H111 1.75(4) . ? Ru13 C116 1.886(4) . ? Ru13 C117 1.888(3) . ? Ru13 P11 2.3745(12) . ? Ru13 B111 2.396(4) . ? C101 B103 1.707(5) . ? C101 B104 1.734(5) . ? C101 B105 1.735(5) . ? C101 B106 1.764(5) . ? C101 S11 1.818(3) . ? B103 B108 1.787(6) . ? B103 B104 1.791(6) . ? B103 B107 1.847(5) . ? B104 B109 1.751(6) . ? B104 B105 1.756(6) . ? B104 B108 1.760(6) . ? B105 B109 1.764(6) . ? B105 B110 1.779(6) . ? B105 B106 1.820(6) . ? B106 B110 1.795(6) . ? B106 B111 1.816(5) . ? B107 B112 1.777(5) . ? B107 B111 1.784(5) . ? B107 B108 1.797(5) . ? B108 B109 1.786(6) . ? B108 B112 1.790(6) . ? B109 B112 1.775(5) . ? B109 B110 1.799(6) . ? B110 B111 1.786(5) . ? B110 B112 1.803(5) . ? B111 H111 1.16(4) . ? B111 B112 1.788(5) . ? C111 O111 1.145(4) . ? C112 O112 1.143(4) . ? C113 O113 1.142(5) . ? C114 O114 1.126(5) . ? C115 O115 1.146(5) . ? C116 O116 1.136(4) . ? C117 O117 1.135(4) . ? S11 C122 1.775(5) . ? S11 C121 1.786(4) . ? P11 C151 1.851(3) . ? P11 C141 1.859(3) . ? P11 C131 1.860(3) . ? C131 C132 1.541(5) . ? C131 C136 1.551(5) . ? C132 C133 1.528(5) . ? C133 C134 1.541(6) . ? C134 C135 1.522(6) . ? C135 C136 1.524(5) . ? C141 C142 1.541(4) . ? C141 C146 1.556(5) . ? C142 C143 1.534(4) . ? C143 C144 1.534(5) . ? C144 C145 1.526(5) . ? C145 C146 1.543(5) . ? C151 C152 1.540(4) . ? C151 C156 1.543(5) . ? C152 C153 1.535(5) . ? C153 C154 1.525(5) . ? C154 C155 1.529(5) . ? C155 C156 1.529(5) . ? C100 Cl2 1.749(6) . ? C100 Cl1 1.765(6) . ? C201 Cl3 1.754(9) . ? C201 Cl4 1.761(9) . ? C202 Cl6 1.746(15) . ? C202 Cl5 1.785(17) . ? 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 86.62(15) . . ? C12 Ru1 B11 151.85(14) . . ? C11 Ru1 B11 114.18(15) . . ? C12 Ru1 B7 107.72(14) . . ? C11 Ru1 B7 159.01(14) . . ? B11 Ru1 B7 47.48(14) . . ? C12 Ru1 B3 89.89(15) . . ? C11 Ru1 B3 149.72(13) . . ? B11 Ru1 B3 81.13(14) . . ? B7 Ru1 B3 48.38(13) . . ? C12 Ru1 B6 156.38(14) . . ? C11 Ru1 B6 91.22(15) . . ? B11 Ru1 B6 47.67(14) . . ? B7 Ru1 B6 81.60(14) . . ? B3 Ru1 B6 80.22(14) . . ? C12 Ru1 C1 114.25(14) . . ? C11 Ru1 C1 110.72(13) . . ? B11 Ru1 C1 77.32(13) . . ? B7 Ru1 C1 77.90(13) . . ? B3 Ru1 C1 44.68(12) . . ? B6 Ru1 C1 45.18(13) . . ? C12 Ru1 Ru3 114.40(11) . . ? C11 Ru1 Ru3 79.95(11) . . ? B11 Ru1 Ru3 55.55(10) . . ? B7 Ru1 Ru3 80.14(10) . . ? B3 Ru1 Ru3 128.23(10) . . ? B6 Ru1 Ru3 88.27(10) . . ? C1 Ru1 Ru3 130.64(9) . . ? C12 Ru1 Ru2 74.27(10) . . ? C11 Ru1 Ru2 125.96(10) . . ? B11 Ru1 Ru2 78.03(10) . . ? B7 Ru1 Ru2 48.38(10) . . ? B3 Ru1 Ru2 81.51(9) . . ? B6 Ru1 Ru2 124.58(10) . . ? C1 Ru1 Ru2 123.27(8) . . ? Ru3 Ru1 Ru2 64.32(3) . . ? H99 Ru2 C15 78.1(12) . . ? H99 Ru2 C13 168.4(12) . . ? C15 Ru2 C13 90.39(15) . . ? H99 Ru2 C14 89.7(13) . . ? C15 Ru2 C14 105.20(18) . . ? C13 Ru2 C14 93.76(17) . . ? H99 Ru2 B7 93.3(13) . . ? C15 Ru2 B7 92.47(17) . . ? C13 Ru2 B7 86.75(15) . . ? C14 Ru2 B7 162.32(15) . . ? H99 Ru2 Ru1 90.9(11) . . ? C15 Ru2 Ru1 141.58(14) . . ? C13 Ru2 Ru1 98.06(10) . . ? C14 Ru2 Ru1 111.50(12) . . ? B7 Ru2 Ru1 51.08(10) . . ? H99 Ru2 Ru3 34.3(11) . . ? C15 Ru2 Ru3 108.57(12) . . ? C13 Ru2 Ru3 155.18(10) . . ? C14 Ru2 Ru3 96.40(12) . . ? B7 Ru2 Ru3 76.83(10) . . ? Ru1 Ru2 Ru3 57.13(2) . . ? H11 Ru3 H99 88.7(18) . . ? H11 Ru3 C16 175.8(14) . . ? H99 Ru3 C16 89.3(13) . . ? H11 Ru3 C17 89.5(13) . . ? H99 Ru3 C17 171.7(12) . . ? C16 Ru3 C17 93.03(15) . . ? H11 Ru3 P1 87.2(13) . . ? H99 Ru3 P1 78.3(12) . . ? C16 Ru3 P1 96.02(12) . . ? C17 Ru3 P1 93.53(11) . . ? H11 Ru3 B11 31.6(14) . . ? H99 Ru3 B11 88.5(13) . . ? C16 Ru3 B11 144.62(15) . . ? C17 Ru3 B11 94.20(14) . . ? P1 Ru3 B11 117.99(10) . . ? H11 Ru3 Ru1 81.8(14) . . ? H99 Ru3 Ru1 91.7(12) . . ? C16 Ru3 Ru1 94.57(12) . . ? C17 Ru3 Ru1 96.12(11) . . ? P1 Ru3 Ru1 165.25(2) . . ? B11 Ru3 Ru1 50.23(9) . . ? H11 Ru3 Ru2 89.7(14) . . ? H99 Ru3 Ru2 33.6(12) . . ? C16 Ru3 Ru2 86.57(11) . . ? C17 Ru3 Ru2 154.48(10) . . ? P1 Ru3 Ru2 111.89(4) . . ? B11 Ru3 Ru2 72.51(10) . . ? Ru1 Ru3 Ru2 58.55(3) . . ? B5 C1 B3 113.9(3) . . ? B5 C1 B4 61.7(2) . . ? B3 C1 B4 62.7(2) . . ? B5 C1 B6 63.2(2) . . ? B3 C1 B6 114.2(2) . . ? B4 C1 B6 114.1(3) . . ? B5 C1 S1 106.0(2) . . ? B3 C1 S1 120.9(2) . . ? B4 C1 S1 105.3(2) . . ? B6 C1 S1 122.3(2) . . ? B5 C1 Ru1 124.4(2) . . ? B3 C1 Ru1 67.07(16) . . ? B4 C1 Ru1 124.2(2) . . ? B6 C1 Ru1 66.86(17) . . ? S1 C1 Ru1 120.64(17) . . ? C1 B3 B8 104.7(3) . . ? C1 B3 B4 58.8(2) . . ? B8 B3 B4 59.2(2) . . ? C1 B3 B7 105.3(2) . . ? B8 B3 B7 59.0(2) . . ? B4 B3 B7 106.5(3) . . ? C1 B3 Ru1 68.25(16) . . ? B8 B3 Ru1 119.0(2) . . ? B4 B3 Ru1 121.7(2) . . ? B7 B3 Ru1 65.00(17) . . ? C1 B4 B5 58.8(2) . . ? C1 B4 B9 106.2(3) . . ? B5 B4 B9 60.9(2) . . ? C1 B4 B8 105.2(3) . . ? B5 B4 B8 108.8(3) . . ? B9 B4 B8 60.6(2) . . ? C1 B4 B3 58.5(2) . . ? B5 B4 B3 108.0(3) . . ? B9 B4 B3 109.1(3) . . ? B8 B4 B3 60.2(2) . . ? C1 B5 B4 59.5(2) . . ? C1 B5 B10 105.7(3) . . ? B4 B5 B10 108.5(3) . . ? C1 B5 B9 105.8(3) . . ? B4 B5 B9 59.7(2) . . ? B10 B5 B9 60.7(2) . . ? C1 B5 B6 59.1(2) . . ? B4 B5 B6 109.0(3) . . ? B10 B5 B6 60.3(2) . . ? B9 B5 B6 109.1(3) . . ? C1 B6 B10 103.6(3) . . ? C1 B6 B11 104.5(2) . . ? B10 B6 B11 59.0(2) . . ? C1 B6 B5 57.7(2) . . ? B10 B6 B5 59.1(2) . . ? B11 B6 B5 105.8(3) . . ? C1 B6 Ru1 67.96(17) . . ? B10 B6 Ru1 118.8(2) . . ? B11 B6 Ru1 65.11(17) . . ? B5 B6 Ru1 120.5(2) . . ? B12 B7 B8 60.3(2) . . ? B12 B7 B11 60.0(2) . . ? B8 B7 B11 107.7(3) . . ? B12 B7 B3 107.3(3) . . ? B8 B7 B3 59.2(2) . . ? B11 B7 B3 106.7(2) . . ? B12 B7 Ru2 138.4(2) . . ? B8 B7 Ru2 142.7(2) . . ? B11 B7 Ru2 109.2(2) . . ? B3 B7 Ru2 114.2(2) . . ? B12 B7 Ru1 120.8(2) . . ? B8 B7 Ru1 120.6(2) . . ? B11 B7 Ru1 66.05(17) . . ? B3 B7 Ru1 66.62(16) . . ? Ru2 B7 Ru1 80.54(14) . . ? B4 B8 B12 107.7(3) . . ? B4 B8 B7 109.8(3) . . ? B12 B8 B7 59.3(2) . . ? B4 B8 B9 59.6(2) . . ? B12 B8 B9 59.9(2) . . ? B7 B8 B9 108.4(3) . . ? B4 B8 B3 60.6(2) . . ? B12 B8 B3 108.5(3) . . ? B7 B8 B3 61.8(2) . . ? B9 B8 B3 108.6(3) . . ? B4 B9 B12 107.8(3) . . ? B4 B9 B8 59.8(2) . . ? B12 B9 B8 60.0(2) . . ? B4 B9 B5 59.4(2) . . ? B12 B9 B5 107.4(3) . . ? B8 B9 B5 107.0(3) . . ? B4 B9 B10 107.2(3) . . ? B12 B9 B10 60.3(2) . . ? B8 B9 B10 107.7(3) . . ? B5 B9 B10 59.4(2) . . ? B11 B10 B5 108.4(3) . . ? B11 B10 B12 59.5(2) . . ? B5 B10 B12 107.0(3) . . ? B11 B10 B6 60.7(2) . . ? B5 B10 B6 60.7(2) . . ? B12 B10 B6 108.1(3) . . ? B11 B10 B9 107.5(3) . . ? B5 B10 B9 59.9(2) . . ? B12 B10 B9 59.2(2) . . ? B6 B10 B9 108.8(3) . . ? H11 B11 B12 105.9(18) . . ? H11 B11 B10 109(2) . . ? B12 B11 B10 60.9(2) . . ? H11 B11 B7 121.4(19) . . ? B12 B11 B7 59.3(2) . . ? B10 B11 B7 108.6(3) . . ? H11 B11 B6 128.4(18) . . ? B12 B11 B6 109.0(3) . . ? B10 B11 B6 60.4(2) . . ? B7 B11 B6 108.9(3) . . ? H11 B11 Ru1 122.4(19) . . ? B12 B11 Ru1 120.6(2) . . ? B10 B11 Ru1 122.0(2) . . ? B7 B11 Ru1 66.46(18) . . ? B6 B11 Ru1 67.22(17) . . ? H11 B11 Ru3 48.3(19) . . ? B12 B11 Ru3 136.9(2) . . ? B10 B11 Ru3 149.6(2) . . ? B7 B11 Ru3 101.4(2) . . ? B6 B11 Ru3 113.9(2) . . ? Ru1 B11 Ru3 74.23(12) . . ? B7 B12 B11 60.7(2) . . ? B7 B12 B9 109.4(3) . . ? B11 B12 B9 108.6(3) . . ? B7 B12 B8 60.4(2) . . ? B11 B12 B8 108.3(3) . . ? B9 B12 B8 60.1(2) . . ? B7 B12 B10 108.8(3) . . ? B11 B12 B10 59.6(2) . . ? B9 B12 B10 60.5(2) . . ? B8 B12 B10 108.0(3) . . ? O11 C11 Ru1 178.7(4) . . ? O12 C12 Ru1 175.3(3) . . ? O13 C13 Ru2 179.0(3) . . ? O14 C14 Ru2 172.9(4) . . ? O15 C15 Ru2 176.9(4) . . ? O16 C16 Ru3 177.6(3) . . ? O17 C17 Ru3 178.3(4) . . ? C21 S1 C22 99.8(2) . . ? C21 S1 C1 105.51(17) . . ? C22 S1 C1 106.43(17) . . ? C51 P1 C41 103.13(15) . . ? C51 P1 C31A 107.00(17) . . ? C41 P1 C31A 102.10(16) . . ? C51 P1 Ru3 112.18(11) . . ? C41 P1 Ru3 112.05(11) . . ? C31A P1 Ru3 118.83(12) . . ? C32A C31A C36A 110.4(3) . . ? C32A C31A P1 115.9(3) . . ? C36A C31A P1 115.8(3) . . ? C31A C32A C33A 110.2(3) . . ? C34A C33A C32A 112.6(4) . . ? C35A C34A C33A 112.6(4) . . ? C34A C35A C36A 111.6(4) . . ? C31A C36A C35A 112.0(3) . . ? C42 C41 C46 108.9(3) . . ? C42 C41 P1 116.3(2) . . ? C46 C41 P1 111.9(2) . . ? C43 C42 C41 111.0(3) . . ? C44 C43 C42 110.7(3) . . ? C43 C44 C45 111.2(3) . . ? C44 C45 C46 111.3(3) . . ? C45 C46 C41 109.7(3) . . ? C56 C51 C52 110.3(3) . . ? C56 C51 P1 112.7(2) . . ? C52 C51 P1 112.4(2) . . ? C53 C52 C51 111.0(3) . . ? C52 C53 C54 110.9(3) . . ? C55 C54 C53 109.5(4) . . ? C54 C55 C56 111.3(4) . . ? C55 C56 C51 108.8(3) . . ? C112 Ru11 C111 86.34(15) . . ? C112 Ru11 B107 109.53(14) . . ? C111 Ru11 B107 158.02(15) . . ? C112 Ru11 B111 152.82(13) . . ? C111 Ru11 B111 112.82(14) . . ? B107 Ru11 B111 47.31(13) . . ? C112 Ru11 B106 156.62(14) . . ? C111 Ru11 B106 89.75(14) . . ? B107 Ru11 B106 81.36(14) . . ? B111 Ru11 B106 47.74(13) . . ? C112 Ru11 B103 91.73(15) . . ? C111 Ru11 B103 149.26(14) . . ? B107 Ru11 B103 48.63(14) . . ? B111 Ru11 B103 81.29(14) . . ? B106 Ru11 B103 80.01(14) . . ? C112 Ru11 C101 114.69(14) . . ? C111 Ru11 C101 109.89(13) . . ? B107 Ru11 C101 77.94(13) . . ? B111 Ru11 C101 78.00(13) . . ? B106 Ru11 C101 45.76(13) . . ? B103 Ru11 C101 44.13(12) . . ? C112 Ru11 Ru13 112.79(11) . . ? C111 Ru11 Ru13 79.89(11) . . ? B107 Ru11 Ru13 79.92(10) . . ? B111 Ru11 Ru13 55.90(10) . . ? B106 Ru11 Ru13 89.10(10) . . ? B103 Ru11 Ru13 128.33(10) . . ? C101 Ru11 Ru13 131.95(9) . . ? C112 Ru11 Ru12 75.06(10) . . ? C111 Ru11 Ru12 127.06(10) . . ? B107 Ru11 Ru12 48.35(10) . . ? B111 Ru11 Ru12 77.93(9) . . ? B106 Ru11 Ru12 124.47(10) . . ? B103 Ru11 Ru12 81.54(10) . . ? C101 Ru11 Ru12 122.98(8) . . ? Ru13 Ru11 Ru12 63.76(3) . . ? H199 Ru12 C115 78.5(11) . . ? H199 Ru12 C113 164.2(12) . . ? C115 Ru12 C113 89.84(15) . . ? H199 Ru12 C114 99.6(13) . . ? C115 Ru12 C114 106.91(16) . . ? C113 Ru12 C114 93.97(15) . . ? H199 Ru12 B107 80.9(13) . . ? C115 Ru12 B107 88.60(16) . . ? C113 Ru12 B107 88.25(15) . . ? C114 Ru12 B107 164.32(14) . . ? H199 Ru12 Ru11 83.4(11) . . ? C115 Ru12 Ru11 137.60(13) . . ? C113 Ru12 Ru11 98.68(10) . . ? C114 Ru12 Ru11 113.74(11) . . ? B107 Ru12 Ru11 50.61(9) . . ? H199 Ru12 Ru13 30.4(11) . . ? C115 Ru12 Ru13 108.35(12) . . ? C113 Ru12 Ru13 155.84(10) . . ? C114 Ru12 Ru13 95.67(11) . . ? B107 Ru12 Ru13 76.76(10) . . ? Ru11 Ru12 Ru13 57.16(2) . . ? H199 Ru13 H111 75.2(19) . . ? H199 Ru13 C116 101.4(14) . . ? H111 Ru13 C116 169.4(14) . . ? H199 Ru13 C117 164.6(13) . . ? H111 Ru13 C117 92.4(13) . . ? C116 Ru13 C117 92.38(15) . . ? H199 Ru13 P11 79.3(13) . . ? H111 Ru13 P11 92.3(13) . . ? C116 Ru13 P11 97.00(11) . . ? C117 Ru13 P11 92.31(11) . . ? H199 Ru13 B111 77.1(14) . . ? H111 Ru13 B111 27.4(14) . . ? C116 Ru13 B111 142.38(14) . . ? C117 Ru13 B111 96.17(13) . . ? P11 Ru13 B111 119.08(9) . . ? H199 Ru13 Ru11 87.7(13) . . ? H111 Ru13 Ru11 77.7(14) . . ? C116 Ru13 Ru11 92.24(11) . . ? C117 Ru13 Ru11 98.78(11) . . ? P11 Ru13 Ru11 165.26(2) . . ? B111 Ru13 Ru11 50.28(9) . . ? H199 Ru13 Ru12 33.2(13) . . ? H111 Ru13 Ru12 86.4(14) . . ? C116 Ru13 Ru12 85.58(11) . . ? C117 Ru13 Ru12 157.59(10) . . ? P11 Ru13 Ru12 110.10(3) . . ? B111 Ru13 Ru12 72.91(9) . . ? Ru11 Ru13 Ru12 59.08(3) . . ? B103 C101 B104 62.7(2) . . ? B103 C101 B105 113.1(3) . . ? B104 C101 B105 60.8(2) . . ? B103 C101 B106 113.9(3) . . ? B104 C101 B106 112.8(3) . . ? B105 C101 B106 62.7(2) . . ? B103 C101 S11 121.3(2) . . ? B104 C101 S11 105.9(2) . . ? B105 C101 S11 106.2(2) . . ? B106 C101 S11 122.4(2) . . ? B103 C101 Ru11 67.59(17) . . ? B104 C101 Ru11 124.2(2) . . ? B105 C101 Ru11 123.6(2) . . ? B106 C101 Ru11 66.62(17) . . ? S11 C101 Ru11 121.01(18) . . ? C101 B103 B108 105.3(3) . . ? C101 B103 B104 59.4(2) . . ? B108 B103 B104 58.9(2) . . ? C101 B103 B107 105.4(3) . . ? B108 B103 B107 59.2(2) . . ? B104 B103 B107 106.2(3) . . ? C101 B103 Ru11 68.27(17) . . ? B108 B103 Ru11 118.8(2) . . ? B104 B103 Ru11 121.9(2) . . ? B107 B103 Ru11 64.37(16) . . ? C101 B104 B109 106.5(3) . . ? C101 B104 B105 59.6(2) . . ? B109 B104 B105 60.4(2) . . ? C101 B104 B108 105.4(3) . . ? B109 B104 B108 61.1(2) . . ? B105 B104 B108 109.1(3) . . ? C101 B104 B103 57.9(2) . . ? B109 B104 B103 109.4(3) . . ? B105 B104 B103 108.1(3) . . ? B108 B104 B103 60.4(2) . . ? C101 B105 B104 59.6(2) . . ? C101 B105 B109 105.9(3) . . ? B104 B105 B109 59.7(2) . . ? C101 B105 B110 105.9(3) . . ? B104 B105 B110 108.8(3) . . ? B109 B105 B110 61.0(2) . . ? C101 B105 B106 59.4(2) . . ? B104 B105 B106 109.1(3) . . ? B109 B105 B106 108.9(3) . . ? B110 B105 B106 59.8(2) . . ? C101 B106 B110 103.9(3) . . ? C101 B106 B111 104.6(2) . . ? B110 B106 B111 59.3(2) . . ? C101 B106 B105 57.9(2) . . ? B110 B106 B105 58.9(2) . . ? B111 B106 B105 105.9(3) . . ? C101 B106 Ru11 67.61(17) . . ? B110 B106 Ru11 119.1(2) . . ? B111 B106 Ru11 65.11(16) . . ? B105 B106 Ru11 120.3(2) . . ? B112 B107 B111 60.3(2) . . ? B112 B107 B108 60.1(2) . . ? B111 B107 B108 108.0(3) . . ? B112 B107 B103 106.8(3) . . ? B111 B107 B103 107.4(2) . . ? B108 B107 B103 58.7(2) . . ? B112 B107 Ru12 138.5(2) . . ? B111 B107 Ru12 109.6(2) . . ? B108 B107 Ru12 141.7(2) . . ? B103 B107 Ru12 114.4(2) . . ? B112 B107 Ru11 121.3(2) . . ? B111 B107 Ru11 66.51(16) . . ? B108 B107 Ru11 120.7(2) . . ? B103 B107 Ru11 67.00(16) . . ? Ru12 B107 Ru11 81.04(12) . . ? B104 B108 B109 59.2(2) . . ? B104 B108 B103 60.6(2) . . ? B109 B108 B103 108.0(3) . . ? B104 B108 B112 107.4(3) . . ? B109 B108 B112 59.5(2) . . ? B103 B108 B112 108.9(3) . . ? B104 B108 B107 109.8(3) . . ? B109 B108 B107 107.6(3) . . ? B103 B108 B107 62.0(2) . . ? B112 B108 B107 59.4(2) . . ? B104 B109 B105 59.9(2) . . ? B104 B109 B112 108.5(3) . . ? B105 B109 B112 108.5(3) . . ? B104 B109 B108 59.7(2) . . ? B105 B109 B108 107.6(3) . . ? B112 B109 B108 60.4(2) . . ? B104 B109 B110 108.1(3) . . ? B105 B109 B110 59.9(2) . . ? B112 B109 B110 60.6(2) . . ? B108 B109 B110 108.3(3) . . ? B105 B110 B111 109.0(3) . . ? B105 B110 B106 61.2(2) . . ? B111 B110 B106 60.9(2) . . ? B105 B110 B109 59.1(2) . . ? B111 B110 B109 107.5(3) . . ? B106 B110 B109 108.5(3) . . ? B105 B110 B112 106.6(3) . . ? B111 B110 B112 59.8(2) . . ? B106 B110 B112 108.4(3) . . ? B109 B110 B112 59.0(2) . . ? H111 B111 B107 118(2) . . ? H111 B111 B110 115(2) . . ? B107 B111 B110 108.5(3) . . ? H111 B111 B112 108(2) . . ? B107 B111 B112 59.7(2) . . ? B110 B111 B112 60.6(2) . . ? H111 B111 B106 131(2) . . ? B107 B111 B106 108.5(3) . . ? B110 B111 B106 59.8(2) . . ? B112 B111 B106 108.2(3) . . ? H111 B111 Ru11 118(2) . . ? B107 B111 Ru11 66.18(17) . . ? B110 B111 Ru11 121.3(2) . . ? B112 B111 Ru11 120.5(2) . . ? B106 B111 Ru11 67.15(17) . . ? H111 B111 Ru13 44(2) . . ? B107 B111 Ru13 100.6(2) . . ? B110 B111 Ru13 150.7(2) . . ? B112 B111 Ru13 137.1(2) . . ? B106 B111 Ru13 114.4(2) . . ? Ru11 B111 Ru13 73.82(11) . . ? B109 B112 B107 109.0(3) . . ? B109 B112 B111 108.5(3) . . ? B107 B112 B111 60.0(2) . . ? B109 B112 B108 60.1(2) . . ? B107 B112 B108 60.5(2) . . ? B111 B112 B108 108.2(3) . . ? B109 B112 B110 60.4(2) . . ? B107 B112 B110 108.0(3) . . ? B111 B112 B110 59.7(2) . . ? B108 B112 B110 108.0(3) . . ? O111 C111 Ru11 177.6(3) . . ? O112 C112 Ru11 175.3(3) . . ? O113 C113 Ru12 177.5(3) . . ? O114 C114 Ru12 173.7(4) . . ? O115 C115 Ru12 176.0(4) . . ? O116 C116 Ru13 176.1(3) . . ? O117 C117 Ru13 178.3(3) . . ? C122 S11 C121 101.6(3) . . ? C122 S11 C101 105.75(19) . . ? C121 S11 C101 105.95(19) . . ? C151 P11 C141 102.85(15) . . ? C151 P11 C131 103.81(16) . . ? C141 P11 C131 109.86(15) . . ? C151 P11 Ru13 111.78(11) . . ? C141 P11 Ru13 112.94(11) . . ? C131 P11 Ru13 114.59(11) . . ? C132 C131 C136 109.6(3) . . ? C132 C131 P11 115.6(2) . . ? C136 C131 P11 116.2(2) . . ? C133 C132 C131 109.7(3) . . ? C132 C133 C134 112.9(3) . . ? C135 C134 C133 110.0(3) . . ? C134 C135 C136 111.8(3) . . ? C135 C136 C131 111.9(3) . . ? C142 C141 C146 109.8(3) . . ? C142 C141 P11 112.2(2) . . ? C146 C141 P11 118.0(2) . . ? C143 C142 C141 110.2(3) . . ? C142 C143 C144 110.9(3) . . ? C145 C144 C143 110.8(3) . . ? C144 C145 C146 111.8(3) . . ? C145 C146 C141 109.8(3) . . ? C152 C151 C156 110.5(3) . . ? C152 C151 P11 112.8(2) . . ? C156 C151 P11 109.9(2) . . ? C153 C152 C151 110.3(3) . . ? C154 C153 C152 111.7(3) . . ? C153 C154 C155 109.2(3) . . ? C156 C155 C154 110.7(3) . . ? C155 C156 C151 112.6(3) . . ? Cl2 C100 Cl1 111.4(3) . . ? Cl3 C201 Cl4 111.5(6) . . ? Cl6 C202 Cl5 107.8(12) . . ? _diffrn_measured_fraction_theta_max 0.953 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.972 _refine_diff_density_max 1.860 _refine_diff_density_min -1.733 _refine_diff_density_rms 0.160 #============================================================================== data_7 _database_code_depnum_ccdc_archive 'CCDC 268995' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C55.80 H69.60 B10 Fe O9.20 P2 Ru3 S' _chemical_formula_weight 1448.67 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 '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 12.0673(8) _cell_length_b 12.1253(9) _cell_length_c 23.2231(16) _cell_angle_alpha 98.947(3) _cell_angle_beta 91.021(4) _cell_angle_gamma 109.356(3) _cell_volume 3158.1(4) _cell_formula_units_Z 2 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 6375 _cell_measurement_theta_min 2.61 _cell_measurement_theta_max 29.86 _exptl_crystal_description irregular _exptl_crystal_colour red-orange _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.523 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1464 _exptl_absorpt_coefficient_mu 1.065 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8652 _exptl_absorpt_correction_T_max 0.8901 _exptl_absorpt_process_details 'SADABS (Bruker, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(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 'Bruker-Nonius X8 APEX CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 56504 _diffrn_reflns_av_R_equivalents 0.0558 _diffrn_reflns_av_sigmaI/netI 0.0702 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 2.31 _diffrn_reflns_theta_max 29.88 _reflns_number_total 17833 _reflns_number_gt 12978 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2 (Bruker, 2003)' _computing_cell_refinement 'Bruker APEX2 (Bruker, 2003)' _computing_data_reduction 'Bruker APEX2 (Bruker, 2003)' _computing_structure_solution 'Bruker SHELXTL (Bruker, 2000)' _computing_structure_refinement 'Bruker SHELXTL (Bruker, 2000)' _computing_molecular_graphics 'Bruker SHELXTL (Bruker, 2000)' _computing_publication_material 'Bruker SHELXTL (Bruker, 2000)' _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^+6.6190P] 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 17833 _refine_ls_number_parameters 802 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0812 _refine_ls_R_factor_gt 0.0489 _refine_ls_wR_factor_ref 0.1059 _refine_ls_wR_factor_gt 0.0899 _refine_ls_goodness_of_fit_ref 1.067 _refine_ls_restrained_S_all 1.067 _refine_ls_shift/su_max 0.003 _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 0.11884(2) 0.66533(3) 0.283165(13) 0.01524(7) Uani 1 1 d . . . Ru2 Ru 0.23610(2) 0.59878(3) 0.191085(12) 0.01570(7) Uani 1 1 d . . . Ru3 Ru 0.33932(3) 0.83466(3) 0.269275(13) 0.01598(7) Uani 1 1 d . . . C1 C 0.0702(3) 0.5918(3) 0.36564(16) 0.0180(7) Uani 1 1 d . . . B3 B 0.0950(4) 0.4896(4) 0.30922(18) 0.0176(8) Uani 1 1 d . . . H3 H 0.017(3) 0.418(3) 0.2849(17) 0.021 Uiso 1 1 d . . . B4 B 0.1105(4) 0.4794(4) 0.38518(19) 0.0193(8) Uani 1 1 d . . . H4 H 0.043(4) 0.406(4) 0.3998(18) 0.023 Uiso 1 1 d . . . B5 B 0.1639(4) 0.6247(4) 0.42686(19) 0.0197(8) Uani 1 1 d . . . H5 H 0.129(4) 0.644(3) 0.4688(18) 0.024 Uiso 1 1 d . . . B6 B 0.1818(4) 0.7293(4) 0.37776(18) 0.0194(8) Uani 1 1 d . . . H6 H 0.160(3) 0.806(4) 0.3952(18) 0.023 Uiso 1 1 d . . . B7 B 0.2396(4) 0.5624(4) 0.28874(19) 0.0190(8) Uani 1 1 d . . . H7 H 0.284(3) 0.532(3) 0.2426(18) 0.023 Uiso 1 1 d . . . H99 H 0.365(3) 0.723(3) 0.2162(17) 0.023 Uiso 1 1 d . . . B8 B 0.2181(4) 0.4596(4) 0.33787(19) 0.0208(9) Uani 1 1 d . . . H8 H 0.231(4) 0.369(4) 0.3254(18) 0.025 Uiso 1 1 d . . . B9 B 0.2610(4) 0.5452(4) 0.40974(19) 0.0208(9) Uani 1 1 d . . . H9 H 0.298(4) 0.510(4) 0.4450(18) 0.025 Uiso 1 1 d . . . B10 B 0.3060(4) 0.6993(4) 0.40460(18) 0.0193(8) Uani 1 1 d . . . H10 H 0.372(4) 0.767(4) 0.4368(18) 0.023 Uiso 1 1 d . . . B12 B 0.3405(4) 0.5967(4) 0.35011(19) 0.0197(8) Uani 1 1 d . . . H12 H 0.432(4) 0.601(3) 0.3443(18) 0.024 Uiso 1 1 d . . . B11 B 0.2972(3) 0.7119(4) 0.32939(19) 0.0186(8) Uani 1 1 d . . . C11 C -0.0209(3) 0.5873(3) 0.23311(17) 0.0209(8) Uiso 1 1 d . . . O11 O -0.1079(2) 0.5360(2) 0.20549(13) 0.0279(6) Uani 1 1 d . . . C12 C 0.0956(3) 0.8106(3) 0.27674(16) 0.0212(8) Uani 1 1 d . . . O12 O 0.0698(3) 0.8934(3) 0.27394(14) 0.0312(7) Uani 1 1 d . . . C13 C 0.1091(3) 0.4559(4) 0.16510(17) 0.0249(8) Uani 1 1 d . . . O13 O 0.0322(3) 0.3701(3) 0.15034(14) 0.0379(8) Uani 1 1 d . . . C14 C 0.1788(3) 0.6810(3) 0.14272(17) 0.0221(8) Uani 1 1 d . . . O14 O 0.1387(3) 0.7282(3) 0.11328(13) 0.0344(7) Uani 1 1 d . . . C15 C 0.3206(3) 0.9235(3) 0.20890(18) 0.0221(8) Uani 1 1 d . . . O15 O 0.3035(3) 0.9803(3) 0.17674(15) 0.0410(8) Uani 1 1 d . . . C16 C 0.3342(3) 0.9555(3) 0.32858(18) 0.0226(8) Uani 1 1 d . . . O16 O 0.3290(3) 1.0315(3) 0.36372(13) 0.0313(7) Uani 1 1 d . . . S1 S -0.08420(8) 0.56655(9) 0.37380(4) 0.02115(19) Uani 1 1 d . . . C21 C -0.1157(4) 0.5354(4) 0.44602(19) 0.0347(11) Uani 1 1 d . . . H21A H -0.1088 0.4583 0.4493 0.052 Uiso 1 1 calc R . . H21B H -0.1960 0.5335 0.4534 0.052 Uiso 1 1 calc R . . H21C H -0.0596 0.5973 0.4748 0.052 Uiso 1 1 calc R . . C22 C -0.1033(4) 0.7079(4) 0.38148(19) 0.0288(9) Uani 1 1 d . . . H22A H -0.1864 0.6980 0.3860 0.043 Uiso 1 1 calc R . . H22B H -0.0784 0.7433 0.3466 0.043 Uiso 1 1 calc R . . H22C H -0.0554 0.7600 0.4160 0.043 Uiso 1 1 calc R . . Fe1 Fe 0.62464(5) 0.73838(5) 0.16948(2) 0.01871(12) Uani 1 1 d . . . P1 P 0.35009(8) 0.54763(8) 0.11849(4) 0.01683(19) Uani 1 1 d . . . C111 C 0.4871(3) 0.6592(3) 0.10885(15) 0.0195(7) Uani 1 1 d . . . C112 C 0.5923(3) 0.6416(4) 0.08727(16) 0.0237(8) Uani 1 1 d . . . H112 H 0.6029 0.5674 0.0754 0.028 Uiso 1 1 calc R . . C113 C 0.6775(4) 0.7555(4) 0.08688(17) 0.0280(9) Uani 1 1 d . . . H113 H 0.7551 0.7703 0.0747 0.034 Uiso 1 1 calc R . . C114 C 0.6275(4) 0.8431(4) 0.10761(17) 0.0276(9) Uani 1 1 d . . . H114 H 0.6658 0.9265 0.1119 0.033 Uiso 1 1 calc R . . C115 C 0.5100(3) 0.7853(3) 0.12099(16) 0.0223(8) Uani 1 1 d . . . H115 H 0.4562 0.8231 0.1354 0.027 Uiso 1 1 calc R . . C121 C 0.2713(3) 0.5152(3) 0.04630(16) 0.0208(8) Uani 1 1 d . . . C122 C 0.1786(4) 0.4085(4) 0.02947(18) 0.0307(10) Uani 1 1 d . . . H122 H 0.1611 0.3503 0.0542 0.037 Uiso 1 1 calc R . . C123 C 0.1119(4) 0.3866(5) -0.0228(2) 0.0409(12) Uani 1 1 d . . . H123 H 0.0482 0.3142 -0.0336 0.049 Uiso 1 1 calc R . . C124 C 0.1385(4) 0.4705(5) -0.0592(2) 0.0441(13) Uani 1 1 d . . . H124 H 0.0926 0.4562 -0.0950 0.053 Uiso 1 1 calc R . . C125 C 0.2317(5) 0.5749(5) -0.0434(2) 0.0433(12) Uani 1 1 d . . . H125 H 0.2513 0.6314 -0.0690 0.052 Uiso 1 1 calc R . . C126 C 0.2969(4) 0.5978(4) 0.00933(18) 0.0326(10) Uani 1 1 d . . . H126 H 0.3597 0.6709 0.0202 0.039 Uiso 1 1 calc R . . C131 C 0.3897(3) 0.4148(3) 0.11975(17) 0.0197(7) Uani 1 1 d . . . C132 C 0.3946(4) 0.3710(4) 0.17111(18) 0.0265(9) Uani 1 1 d . . . H132 H 0.3768 0.4100 0.2066 0.032 Uiso 1 1 calc R . . C133 C 0.4253(4) 0.2707(4) 0.1708(2) 0.0373(11) Uani 1 1 d . . . H133 H 0.4285 0.2414 0.2062 0.045 Uiso 1 1 calc R . . C134 C 0.4515(4) 0.2125(4) 0.1195(2) 0.0338(10) Uani 1 1 d . . . H134 H 0.4727 0.1437 0.1196 0.041 Uiso 1 1 calc R . . C135 C 0.4465(4) 0.2556(4) 0.0682(2) 0.0308(10) Uani 1 1 d . . . H135 H 0.4637 0.2160 0.0327 0.037 Uiso 1 1 calc R . . C136 C 0.4165(4) 0.3561(4) 0.06832(17) 0.0254(9) Uani 1 1 d . . . H136 H 0.4141 0.3856 0.0329 0.030 Uiso 1 1 calc R . . P2 P 0.53936(8) 0.89112(8) 0.29114(4) 0.01784(19) Uani 1 1 d . . . C211 C 0.6181(3) 0.7992(3) 0.25604(16) 0.0193(7) Uani 1 1 d . . . C212 C 0.5796(3) 0.6722(3) 0.24421(16) 0.0187(7) Uani 1 1 d . . . H212 H 0.5042 0.6203 0.2508 0.022 Uiso 1 1 calc R . . C213 C 0.6732(3) 0.6371(4) 0.22103(17) 0.0243(8) Uani 1 1 d . . . H213 H 0.6712 0.5577 0.2096 0.029 Uiso 1 1 calc R . . C214 C 0.7691(3) 0.7398(4) 0.21795(17) 0.0251(8) Uani 1 1 d . . . H214 H 0.8430 0.7416 0.2039 0.030 Uiso 1 1 calc R . . C215 C 0.7375(3) 0.8404(4) 0.23915(17) 0.0226(8) Uani 1 1 d . . . H215 H 0.7863 0.9209 0.2418 0.027 Uiso 1 1 calc R . . C221 C 0.5863(3) 0.9027(3) 0.36790(16) 0.0206(8) Uani 1 1 d . . . C222 C 0.6249(3) 0.8171(4) 0.38678(16) 0.0224(8) Uani 1 1 d . . . H222 H 0.6282 0.7515 0.3594 0.027 Uiso 1 1 calc R . . C223 C 0.6585(4) 0.8273(4) 0.44540(18) 0.0321(10) Uani 1 1 d . . . H223 H 0.6840 0.7682 0.4580 0.038 Uiso 1 1 calc R . . C224 C 0.6551(4) 0.9224(5) 0.48522(19) 0.0371(11) Uani 1 1 d . . . H224 H 0.6784 0.9290 0.5253 0.044 Uiso 1 1 calc R . . C225 C 0.6178(4) 1.0090(4) 0.46707(19) 0.0366(11) Uani 1 1 d . . . H225 H 0.6172 1.0756 0.4945 0.044 Uiso 1 1 calc R . . C226 C 0.5816(4) 0.9985(4) 0.40921(18) 0.0286(9) Uani 1 1 d . . . H226 H 0.5533 1.0564 0.3972 0.034 Uiso 1 1 calc R . . C231 C 0.6309(3) 1.0356(3) 0.27507(17) 0.0214(8) Uani 1 1 d . . . C232 C 0.7320(4) 1.1068(4) 0.3108(2) 0.0360(11) Uani 1 1 d . . . H232 H 0.7515 1.0822 0.3454 0.043 Uiso 1 1 calc R . . C233 C 0.8035(4) 1.2126(4) 0.2963(2) 0.0477(14) Uani 1 1 d . . . H233 H 0.8712 1.2604 0.3212 0.057 Uiso 1 1 calc R . . C234 C 0.7772(4) 1.2489(4) 0.2461(2) 0.0442(13) Uani 1 1 d . . . H234 H 0.8267 1.3215 0.2362 0.053 Uiso 1 1 calc R . . C235 C 0.6792(4) 1.1799(4) 0.2102(2) 0.0376(11) Uani 1 1 d . . . H235 H 0.6612 1.2041 0.1753 0.045 Uiso 1 1 calc R . . C236 C 0.6063(4) 1.0740(4) 0.2252(2) 0.0290(9) Uani 1 1 d . . . H236 H 0.5380 1.0274 0.2004 0.035 Uiso 1 1 calc R . . O100 O 0.6352(3) 0.5106(3) 0.38093(14) 0.0368(7) Uani 1 1 d . . . C100 C 0.5592(4) 0.4777(5) 0.4265(2) 0.0421(12) Uani 1 1 d . . . H10A H 0.4988 0.5167 0.4277 0.051 Uiso 1 1 calc R . . H10B H 0.6050 0.5015 0.4649 0.051 Uiso 1 1 calc R . . C101 C 0.5021(8) 0.3456(6) 0.4128(3) 0.095(3) Uani 1 1 d . . . H10C H 0.5357 0.3072 0.4398 0.114 Uiso 1 1 calc R . . H10D H 0.4162 0.3228 0.4167 0.114 Uiso 1 1 calc R . . C102 C 0.5260(7) 0.3092(6) 0.3523(3) 0.083(2) Uani 1 1 d . . . H10E H 0.4516 0.2640 0.3282 0.100 Uiso 1 1 calc R . . H10F H 0.5762 0.2589 0.3510 0.100 Uiso 1 1 calc R . . C103 C 0.5880(5) 0.4216(4) 0.3306(2) 0.0428(12) Uani 1 1 d . . . H10G H 0.6520 0.4124 0.3063 0.051 Uiso 1 1 calc R . . H10H H 0.5323 0.4433 0.3067 0.051 Uiso 1 1 calc R . . O200 O 0.0506(4) 0.1978(4) 0.47590(16) 0.0677(13) Uani 1 1 d . . . C200 C 0.1338(5) 0.2016(5) 0.4337(2) 0.0447(13) Uani 1 1 d . . . H20A H 0.1929 0.1679 0.4461 0.054 Uiso 1 1 calc R . . H20B H 0.1752 0.2845 0.4287 0.054 Uiso 1 1 calc R . . C201 C 0.0678(6) 0.1301(6) 0.3779(3) 0.076(2) Uani 1 1 d . . . H20C H 0.1174 0.0950 0.3529 0.091 Uiso 1 1 calc R . . H20D H 0.0357 0.1776 0.3558 0.091 Uiso 1 1 calc R . . C202 C -0.0284(8) 0.0367(6) 0.4013(4) 0.105(3) Uani 1 1 d . . . H20E H -0.0966 -0.0018 0.3721 0.127 Uiso 1 1 calc R . . H20F H 0.0005 -0.0246 0.4130 0.127 Uiso 1 1 calc R . . C203 C -0.0595(6) 0.1079(8) 0.4532(3) 0.097(3) Uani 1 1 d . . . H20G H -0.1170 0.1441 0.4414 0.117 Uiso 1 1 calc R . . H20H H -0.0933 0.0577 0.4827 0.117 Uiso 1 1 calc R . . O300 O 0.6807(6) 1.1233(6) 0.0648(3) 0.050(2) Uani 0.534(6) 1 d P . . C300 C 0.6540(11) 1.0700(9) 0.0062(5) 0.054(3) Uani 0.534(6) 1 d P . . H30A H 0.6293 1.1215 -0.0166 0.065 Uiso 0.534(6) 1 calc PR . . H30B H 0.5896 0.9926 0.0023 0.065 Uiso 0.534(6) 1 calc PR . . C301 C 0.7640(12) 1.0535(11) -0.0147(6) 0.075(4) Uani 0.534(6) 1 d P . . H30C H 0.7653 0.9737 -0.0111 0.090 Uiso 0.534(6) 1 calc PR . . H30D H 0.7723 1.0641 -0.0560 0.090 Uiso 0.534(6) 1 calc PR . . C302 C 0.8555(11) 1.1444(14) 0.0231(6) 0.084(5) Uani 0.534(6) 1 d P . . H30E H 0.9263 1.1210 0.0265 0.100 Uiso 0.534(6) 1 calc PR . . H30F H 0.8777 1.2202 0.0080 0.100 Uiso 0.534(6) 1 calc PR . . C303 C 0.8075(9) 1.1550(10) 0.0767(5) 0.063(4) Uani 0.534(6) 1 d P . . H30G H 0.8414 1.2375 0.0981 0.075 Uiso 0.534(6) 1 calc PR . . H30H H 0.8245 1.1013 0.1008 0.075 Uiso 0.534(6) 1 calc PR . . O400 O -0.0524(9) 0.9954(9) 0.1578(5) 0.121(4) Uani 0.633(7) 1 d P . . C400 C 0.0259(10) 0.9961(12) 0.1178(6) 0.095(5) Uani 0.633(7) 1 d P . . H40A H -0.0127 0.9782 0.0778 0.114 Uiso 0.633(7) 1 calc PR . . H40B H 0.0640 0.9366 0.1218 0.114 Uiso 0.633(7) 1 calc PR . . C401 C 0.1118(9) 1.1151(9) 0.1291(5) 0.066(3) Uani 0.633(7) 1 d P . . H40C H 0.0861 1.1700 0.1092 0.079 Uiso 0.633(7) 1 calc PR . . H40D H 0.1899 1.1157 0.1165 0.079 Uiso 0.633(7) 1 calc PR . . C402 C 0.1146(9) 1.1482(9) 0.1968(5) 0.062(3) Uani 0.633(7) 1 d P . . H40E H 0.1659 1.1148 0.2169 0.074 Uiso 0.633(7) 1 calc PR . . H40F H 0.1411 1.2351 0.2098 0.074 Uiso 0.633(7) 1 calc PR . . C403 C -0.0049(9) 1.0939(10) 0.2061(5) 0.076(3) Uani 0.633(7) 1 d P . . H40G H -0.0475 1.1511 0.2066 0.091 Uiso 0.633(7) 1 calc PR . . H40H H -0.0124 1.0648 0.2439 0.091 Uiso 0.633(7) 1 calc PR . . 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 0.01425(13) 0.01630(14) 0.01474(14) 0.00277(10) 0.00116(10) 0.00457(11) Ru2 0.01538(13) 0.01687(15) 0.01293(14) 0.00018(10) -0.00016(10) 0.00405(11) Ru3 0.01628(13) 0.01456(14) 0.01464(14) 0.00058(10) 0.00118(10) 0.00285(11) C1 0.0154(16) 0.0215(19) 0.0183(18) 0.0049(14) 0.0033(14) 0.0069(14) B3 0.0181(19) 0.016(2) 0.0157(19) 0.0004(15) 0.0000(15) 0.0028(16) B4 0.0188(19) 0.022(2) 0.019(2) 0.0052(16) 0.0011(16) 0.0081(17) B5 0.021(2) 0.021(2) 0.018(2) 0.0044(16) 0.0017(16) 0.0083(17) B6 0.0189(19) 0.022(2) 0.016(2) 0.0004(16) 0.0029(15) 0.0060(17) B7 0.020(2) 0.019(2) 0.019(2) 0.0011(16) -0.0004(16) 0.0078(17) B8 0.022(2) 0.023(2) 0.021(2) 0.0084(17) 0.0051(17) 0.0105(18) B9 0.021(2) 0.026(2) 0.017(2) 0.0045(17) -0.0009(16) 0.0088(18) B10 0.021(2) 0.022(2) 0.015(2) 0.0016(16) 0.0003(16) 0.0084(17) B12 0.020(2) 0.022(2) 0.017(2) 0.0043(16) 0.0028(16) 0.0064(17) B11 0.0136(18) 0.019(2) 0.019(2) -0.0020(16) -0.0006(15) 0.0027(16) O11 0.0246(14) 0.0288(16) 0.0285(16) 0.0019(12) -0.0045(12) 0.0082(12) C12 0.0184(17) 0.025(2) 0.0181(19) 0.0014(15) -0.0014(14) 0.0058(16) O12 0.0300(16) 0.0236(15) 0.0408(19) 0.0053(13) -0.0012(13) 0.0106(13) C13 0.0235(19) 0.027(2) 0.022(2) 0.0011(16) 0.0011(16) 0.0066(17) O13 0.0318(17) 0.0297(17) 0.0369(19) -0.0069(14) 0.0011(14) -0.0041(14) C14 0.0210(18) 0.023(2) 0.0192(19) -0.0023(15) -0.0024(15) 0.0055(16) O14 0.0402(18) 0.0322(17) 0.0310(17) 0.0036(13) -0.0119(14) 0.0142(14) C15 0.0180(17) 0.0203(19) 0.026(2) 0.0049(16) 0.0015(15) 0.0030(15) O15 0.046(2) 0.0352(19) 0.043(2) 0.0180(15) -0.0050(16) 0.0113(16) C16 0.0171(17) 0.023(2) 0.029(2) 0.0074(16) -0.0004(15) 0.0060(15) O16 0.0344(16) 0.0268(16) 0.0291(16) -0.0062(13) 0.0029(13) 0.0106(13) S1 0.0166(4) 0.0265(5) 0.0218(5) 0.0076(4) 0.0039(3) 0.0076(4) C21 0.027(2) 0.051(3) 0.032(2) 0.022(2) 0.0163(18) 0.014(2) C22 0.026(2) 0.035(2) 0.031(2) 0.0096(18) 0.0104(17) 0.0173(19) Fe1 0.0188(3) 0.0196(3) 0.0149(3) 0.0005(2) 0.0030(2) 0.0038(2) P1 0.0180(4) 0.0187(5) 0.0126(4) 0.0011(3) 0.0003(3) 0.0053(4) C111 0.0222(18) 0.0239(19) 0.0101(16) 0.0019(14) 0.0021(13) 0.0053(15) C112 0.0249(19) 0.027(2) 0.0154(18) -0.0013(15) 0.0044(15) 0.0059(17) C113 0.026(2) 0.034(2) 0.0175(19) 0.0040(16) 0.0084(16) 0.0010(18) C114 0.034(2) 0.024(2) 0.018(2) 0.0066(16) 0.0061(17) 0.0008(18) C115 0.028(2) 0.024(2) 0.0155(18) 0.0038(15) 0.0010(15) 0.0085(16) C121 0.0223(18) 0.027(2) 0.0138(17) -0.0008(14) -0.0008(14) 0.0112(16) C122 0.032(2) 0.039(3) 0.0160(19) -0.0009(17) -0.0045(16) 0.0082(19) C123 0.035(2) 0.051(3) 0.026(2) 0.000(2) -0.0092(19) 0.005(2) C124 0.039(3) 0.069(4) 0.020(2) 0.000(2) -0.0150(19) 0.016(3) C125 0.050(3) 0.059(3) 0.023(2) 0.015(2) -0.005(2) 0.018(3) C126 0.038(2) 0.037(3) 0.021(2) 0.0062(18) -0.0047(18) 0.009(2) C131 0.0178(17) 0.0195(19) 0.0210(19) 0.0020(14) 0.0013(14) 0.0057(15) C132 0.036(2) 0.026(2) 0.019(2) 0.0021(16) 0.0006(17) 0.0143(18) C133 0.058(3) 0.033(2) 0.029(2) 0.0093(19) 0.001(2) 0.023(2) C134 0.042(3) 0.027(2) 0.038(3) 0.0038(19) 0.002(2) 0.019(2) C135 0.036(2) 0.028(2) 0.031(2) -0.0004(18) 0.0061(19) 0.0155(19) C136 0.031(2) 0.026(2) 0.0190(19) 0.0018(15) 0.0070(16) 0.0102(17) P2 0.0185(4) 0.0165(5) 0.0162(5) -0.0006(4) -0.0017(4) 0.0045(4) C211 0.0223(18) 0.0222(19) 0.0131(17) 0.0020(14) 0.0003(14) 0.0077(15) C212 0.0185(17) 0.0219(19) 0.0159(17) 0.0035(14) -0.0005(14) 0.0072(15) C213 0.0236(19) 0.025(2) 0.025(2) 0.0035(16) 0.0027(16) 0.0096(16) C214 0.0173(17) 0.032(2) 0.024(2) -0.0012(16) -0.0018(15) 0.0086(16) C215 0.0222(18) 0.023(2) 0.0198(19) 0.0022(15) 0.0009(15) 0.0042(16) C221 0.0171(17) 0.025(2) 0.0162(18) -0.0017(14) -0.0028(14) 0.0050(15) C222 0.0228(19) 0.030(2) 0.0156(18) 0.0017(15) -0.0011(14) 0.0119(17) C223 0.035(2) 0.047(3) 0.020(2) 0.0054(19) 0.0006(17) 0.020(2) C224 0.038(2) 0.060(3) 0.017(2) -0.001(2) -0.0015(18) 0.025(2) C225 0.034(2) 0.048(3) 0.023(2) -0.015(2) -0.0039(18) 0.019(2) C226 0.027(2) 0.031(2) 0.027(2) -0.0066(17) -0.0047(17) 0.0145(18) C231 0.0176(17) 0.0141(18) 0.028(2) 0.0024(15) -0.0031(15) -0.0003(14) C232 0.031(2) 0.027(2) 0.044(3) 0.011(2) -0.011(2) 0.0003(19) C233 0.036(3) 0.030(3) 0.063(4) 0.014(2) -0.022(2) -0.008(2) C234 0.033(2) 0.032(3) 0.060(3) 0.022(2) -0.011(2) -0.005(2) C235 0.029(2) 0.032(3) 0.045(3) 0.017(2) -0.006(2) -0.0013(19) C236 0.0219(19) 0.026(2) 0.035(2) 0.0058(18) 0.0020(17) 0.0022(17) O100 0.0318(17) 0.0436(19) 0.0313(18) 0.0071(14) 0.0043(13) 0.0075(15) C100 0.031(2) 0.072(4) 0.032(3) 0.020(2) 0.007(2) 0.024(3) C101 0.121(7) 0.070(5) 0.072(5) 0.030(4) 0.035(5) -0.006(5) C102 0.107(6) 0.046(4) 0.095(6) 0.023(4) 0.041(5) 0.016(4) C103 0.053(3) 0.035(3) 0.038(3) 0.006(2) 0.010(2) 0.011(2) O200 0.070(3) 0.068(3) 0.032(2) -0.0022(19) 0.0016(19) -0.016(2) C200 0.052(3) 0.041(3) 0.045(3) 0.003(2) -0.012(2) 0.022(2) C201 0.081(5) 0.078(5) 0.067(5) -0.033(4) -0.023(4) 0.046(4) C202 0.148(8) 0.027(3) 0.120(7) -0.013(4) -0.085(6) 0.018(4) C203 0.064(4) 0.127(7) 0.056(4) 0.036(5) -0.011(3) -0.034(4) O300 0.051(4) 0.043(4) 0.050(5) 0.002(3) -0.002(3) 0.011(3) C300 0.079(8) 0.034(5) 0.050(7) -0.002(5) -0.009(6) 0.024(5) C301 0.093(10) 0.055(8) 0.063(8) 0.010(6) 0.026(7) 0.006(7) C302 0.048(7) 0.114(12) 0.085(10) 0.029(9) 0.026(7) 0.017(8) C303 0.048(6) 0.042(6) 0.079(9) 0.018(6) -0.026(6) -0.013(5) O400 0.113(8) 0.105(8) 0.111(8) 0.018(6) -0.034(7) -0.007(6) C400 0.055(7) 0.111(10) 0.102(10) -0.049(8) -0.008(7) 0.039(7) C401 0.066(7) 0.053(6) 0.079(8) -0.005(5) 0.012(6) 0.026(5) C402 0.060(6) 0.050(6) 0.080(8) 0.013(5) 0.011(5) 0.024(5) C403 0.058(7) 0.075(8) 0.090(9) 0.020(7) -0.007(6) 0.015(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 C12 1.900(4) . ? Ru1 C11 1.903(4) . ? Ru1 B7 2.224(4) . ? Ru1 B3 2.234(4) . ? Ru1 B6 2.242(4) . ? Ru1 B11 2.242(4) . ? Ru1 C1 2.243(4) . ? Ru1 Ru2 2.7485(4) . ? Ru1 Ru3 2.8309(4) . ? Ru2 H7 1.73(4) . ? Ru2 H99 1.78(4) . ? Ru2 C14 1.874(4) . ? Ru2 C13 1.896(4) . ? Ru2 P1 2.3328(10) . ? Ru2 B7 2.379(4) . ? Ru2 Ru3 2.9953(4) . ? Ru3 H99 1.79(4) . ? Ru3 C16 1.866(4) . ? Ru3 C15 1.948(4) . ? Ru3 B11 2.143(4) . ? Ru3 P2 2.3036(10) . ? C1 B5 1.710(6) . ? C1 B4 1.711(6) . ? C1 B6 1.739(6) . ? C1 B3 1.760(5) . ? C1 S1 1.804(4) . ? B3 B8 1.783(6) . ? B3 B7 1.786(6) . ? B3 B4 1.798(6) . ? B4 B9 1.767(6) . ? B4 B8 1.768(6) . ? B4 B5 1.775(6) . ? B5 B9 1.763(6) . ? B5 B10 1.782(6) . ? B5 B6 1.798(6) . ? B6 B10 1.779(6) . ? B6 B11 1.850(6) . ? B7 H7 1.27(4) . ? B7 B12 1.762(6) . ? B7 B8 1.778(6) . ? B7 B11 1.808(6) . ? B8 B9 1.790(6) . ? B8 B12 1.799(6) . ? B9 B12 1.775(6) . ? B9 B10 1.790(6) . ? B10 B11 1.781(6) . ? B10 B12 1.788(6) . ? B12 B11 1.772(6) . ? C11 O11 1.148(4) . ? C12 O12 1.156(5) . ? C13 O13 1.140(5) . ? C14 O14 1.150(5) . ? C15 O15 1.151(5) . ? C16 O16 1.151(5) . ? S1 C22 1.786(4) . ? S1 C21 1.796(4) . ? Fe1 C111 2.024(4) . ? Fe1 C212 2.032(4) . ? Fe1 C112 2.037(4) . ? Fe1 C115 2.042(4) . ? Fe1 C211 2.043(4) . ? Fe1 C215 2.046(4) . ? Fe1 C213 2.048(4) . ? Fe1 C214 2.051(4) . ? Fe1 C113 2.052(4) . ? Fe1 C114 2.054(4) . ? P1 C111 1.800(4) . ? P1 C131 1.829(4) . ? P1 C121 1.833(4) . ? C111 C115 1.440(5) . ? C111 C112 1.441(5) . ? C112 C113 1.424(5) . ? C113 C114 1.414(6) . ? C114 C115 1.422(5) . ? C121 C126 1.381(6) . ? C121 C122 1.394(6) . ? C122 C123 1.383(6) . ? C123 C124 1.383(7) . ? C124 C125 1.378(7) . ? C125 C126 1.382(6) . ? C131 C132 1.387(5) . ? C131 C136 1.392(5) . ? C132 C133 1.383(6) . ? C133 C134 1.385(6) . ? C134 C135 1.382(6) . ? C135 C136 1.382(6) . ? P2 C211 1.805(4) . ? P2 C221 1.831(4) . ? P2 C231 1.833(4) . ? C211 C212 1.432(5) . ? C211 C215 1.443(5) . ? C212 C213 1.420(5) . ? C213 C214 1.404(5) . ? C214 C215 1.415(5) . ? C221 C222 1.394(5) . ? C221 C226 1.404(5) . ? C222 C223 1.388(5) . ? C223 C224 1.375(6) . ? C224 C225 1.388(7) . ? C225 C226 1.379(6) . ? C231 C236 1.376(6) . ? C231 C232 1.403(5) . ? C232 C233 1.384(6) . ? C233 C234 1.377(7) . ? C234 C235 1.373(6) . ? C235 C236 1.395(6) . ? O100 C103 1.424(6) . ? O100 C100 1.430(5) . ? C100 C101 1.498(8) . ? C101 C102 1.469(9) . ? C102 C103 1.490(7) . ? O200 C200 1.410(6) . ? O200 C203 1.438(7) . ? C200 C201 1.491(7) . ? C201 C202 1.505(11) . ? C202 C203 1.500(11) . ? O300 C300 1.395(12) . ? O300 C303 1.459(12) . ? C300 C301 1.485(16) . ? C301 C302 1.436(17) . ? C302 C303 1.389(16) . ? O400 C400 1.336(14) . ? O400 C403 1.456(14) . ? C400 C401 1.452(15) . ? C401 C402 1.558(14) . ? C402 C403 1.409(13) . ? 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 87.44(16) . . ? C12 Ru1 B7 149.79(16) . . ? C11 Ru1 B7 115.77(16) . . ? C12 Ru1 B3 160.68(15) . . ? C11 Ru1 B3 86.85(16) . . ? B7 Ru1 B3 47.24(15) . . ? C12 Ru1 B6 91.57(16) . . ? C11 Ru1 B6 141.78(16) . . ? B7 Ru1 B6 81.76(16) . . ? B3 Ru1 B6 81.66(16) . . ? C12 Ru1 B11 106.95(16) . . ? C11 Ru1 B11 163.20(15) . . ? B7 Ru1 B11 47.76(15) . . ? B3 Ru1 B11 82.14(16) . . ? B6 Ru1 B11 48.74(15) . . ? C12 Ru1 C1 117.51(15) . . ? C11 Ru1 C1 102.30(15) . . ? B7 Ru1 C1 78.04(14) . . ? B3 Ru1 C1 46.29(14) . . ? B6 Ru1 C1 45.62(14) . . ? B11 Ru1 C1 79.07(14) . . ? C12 Ru1 Ru2 110.62(11) . . ? C11 Ru1 Ru2 86.05(11) . . ? B7 Ru1 Ru2 55.97(11) . . ? B3 Ru1 Ru2 87.37(10) . . ? B6 Ru1 Ru2 129.30(11) . . ? B11 Ru1 Ru2 80.83(11) . . ? C1 Ru1 Ru2 131.34(9) . . ? C12 Ru1 Ru3 71.60(11) . . ? C11 Ru1 Ru3 133.45(12) . . ? B7 Ru1 Ru3 78.26(11) . . ? B3 Ru1 Ru3 124.61(11) . . ? B6 Ru1 Ru3 81.47(11) . . ? B11 Ru1 Ru3 48.27(11) . . ? C1 Ru1 Ru3 124.25(9) . . ? Ru2 Ru1 Ru3 64.919(11) . . ? H7 Ru2 H99 85.3(18) . . ? H7 Ru2 C14 173.3(13) . . ? H99 Ru2 C14 93.1(13) . . ? H7 Ru2 C13 90.0(13) . . ? H99 Ru2 C13 173.9(13) . . ? C14 Ru2 C13 92.08(17) . . ? H7 Ru2 P1 94.8(13) . . ? H99 Ru2 P1 85.4(13) . . ? C14 Ru2 P1 91.47(12) . . ? C13 Ru2 P1 91.09(12) . . ? H7 Ru2 B7 31.1(13) . . ? H99 Ru2 B7 85.0(13) . . ? C14 Ru2 B7 142.38(15) . . ? C13 Ru2 B7 93.01(16) . . ? P1 Ru2 B7 125.64(10) . . ? H7 Ru2 Ru1 81.8(13) . . ? H99 Ru2 Ru1 90.7(13) . . ? C14 Ru2 Ru1 91.77(12) . . ? C13 Ru2 Ru1 92.52(12) . . ? P1 Ru2 Ru1 175.06(3) . . ? B7 Ru2 Ru1 50.78(10) . . ? H7 Ru2 Ru3 89.8(13) . . ? H99 Ru2 Ru3 33.1(13) . . ? C14 Ru2 Ru3 85.29(11) . . ? C13 Ru2 Ru3 151.08(12) . . ? P1 Ru2 Ru3 117.74(3) . . ? B7 Ru2 Ru3 72.72(10) . . ? Ru1 Ru2 Ru3 58.870(10) . . ? H99 Ru3 C16 172.1(13) . . ? H99 Ru3 C15 91.5(13) . . ? C16 Ru3 C15 91.81(17) . . ? H99 Ru3 B11 89.3(13) . . ? C16 Ru3 B11 89.94(16) . . ? C15 Ru3 B11 160.70(15) . . ? H99 Ru3 P2 83.2(13) . . ? C16 Ru3 P2 89.03(12) . . ? C15 Ru3 P2 105.55(11) . . ? B11 Ru3 P2 93.69(11) . . ? H99 Ru3 Ru1 87.9(13) . . ? C16 Ru3 Ru1 97.80(12) . . ? C15 Ru3 Ru1 109.42(11) . . ? B11 Ru3 Ru1 51.34(11) . . ? P2 Ru3 Ru1 144.06(3) . . ? H99 Ru3 Ru2 32.9(13) . . ? C16 Ru3 Ru2 153.74(12) . . ? C15 Ru3 Ru2 93.74(11) . . ? B11 Ru3 Ru2 76.73(11) . . ? P2 Ru3 Ru2 114.00(3) . . ? Ru1 Ru3 Ru2 56.211(10) . . ? B5 C1 B4 62.5(2) . . ? B5 C1 B6 62.8(2) . . ? B4 C1 B6 114.3(3) . . ? B5 C1 B3 113.9(3) . . ? B4 C1 B3 62.4(2) . . ? B6 C1 B3 113.5(3) . . ? B5 C1 S1 119.0(2) . . ? B4 C1 S1 111.2(2) . . ? B6 C1 S1 125.7(3) . . ? B3 C1 S1 112.8(2) . . ? B5 C1 Ru1 124.5(2) . . ? B4 C1 Ru1 123.8(2) . . ? B6 C1 Ru1 67.15(18) . . ? B3 C1 Ru1 66.58(18) . . ? S1 C1 Ru1 108.78(18) . . ? C1 B3 B8 103.9(3) . . ? C1 B3 B7 104.9(3) . . ? B8 B3 B7 59.7(2) . . ? C1 B3 B4 57.5(2) . . ? B8 B3 B4 59.2(2) . . ? B7 B3 B4 106.5(3) . . ? C1 B3 Ru1 67.13(18) . . ? B8 B3 Ru1 120.2(2) . . ? B7 B3 Ru1 66.09(19) . . ? B4 B3 Ru1 119.9(2) . . ? C1 B4 B9 105.2(3) . . ? C1 B4 B8 106.6(3) . . ? B9 B4 B8 60.8(2) . . ? C1 B4 B5 58.7(2) . . ? B9 B4 B5 59.7(2) . . ? B8 B4 B5 109.1(3) . . ? C1 B4 B3 60.1(2) . . ? B9 B4 B3 108.4(3) . . ? B8 B4 B3 60.0(2) . . ? B5 B4 B3 109.0(3) . . ? C1 B5 B9 105.3(3) . . ? C1 B5 B4 58.7(2) . . ? B9 B5 B4 59.9(2) . . ? C1 B5 B10 105.2(3) . . ? B9 B5 B10 60.6(2) . . ? B4 B5 B10 108.2(3) . . ? C1 B5 B6 59.4(2) . . ? B9 B5 B6 108.5(3) . . ? B4 B5 B6 108.3(3) . . ? B10 B5 B6 59.6(2) . . ? C1 B6 B10 104.1(3) . . ? C1 B6 B5 57.8(2) . . ? B10 B6 B5 59.8(2) . . ? C1 B6 B11 105.4(3) . . ? B10 B6 B11 58.7(2) . . ? B5 B6 B11 106.8(3) . . ? C1 B6 Ru1 67.23(18) . . ? B10 B6 Ru1 118.7(2) . . ? B5 B6 Ru1 120.1(3) . . ? B11 B6 Ru1 65.64(18) . . ? H7 B7 B12 110.8(18) . . ? H7 B7 B8 112.8(18) . . ? B12 B7 B8 61.1(2) . . ? H7 B7 B3 126.2(18) . . ? B12 B7 B3 108.9(3) . . ? B8 B7 B3 60.0(2) . . ? H7 B7 B11 121.1(18) . . ? B12 B7 B11 59.5(2) . . ? B8 B7 B11 109.4(3) . . ? B3 B7 B11 109.8(3) . . ? H7 B7 Ru1 118.2(18) . . ? B12 B7 Ru1 120.2(3) . . ? B8 B7 Ru1 121.0(3) . . ? B3 B7 Ru1 66.67(19) . . ? B11 B7 Ru1 66.64(19) . . ? H7 B7 Ru2 45.1(18) . . ? B12 B7 Ru2 139.2(3) . . ? B8 B7 Ru2 149.2(3) . . ? B3 B7 Ru2 111.6(2) . . ? B11 B7 Ru2 101.3(2) . . ? Ru1 B7 Ru2 73.25(13) . . ? B4 B8 B7 108.1(3) . . ? B4 B8 B3 60.8(2) . . ? B7 B8 B3 60.2(2) . . ? B4 B8 B9 59.5(2) . . ? B7 B8 B9 106.8(3) . . ? B3 B8 B9 108.1(3) . . ? B4 B8 B12 107.0(3) . . ? B7 B8 B12 59.0(2) . . ? B3 B8 B12 107.4(3) . . ? B9 B8 B12 59.3(2) . . ? B5 B9 B4 60.4(2) . . ? B5 B9 B12 108.7(3) . . ? B4 B9 B12 108.1(3) . . ? B5 B9 B10 60.2(2) . . ? B4 B9 B10 108.2(3) . . ? B12 B9 B10 60.2(2) . . ? B5 B9 B8 108.7(3) . . ? B4 B9 B8 59.6(2) . . ? B12 B9 B8 60.6(2) . . ? B10 B9 B8 108.8(3) . . ? B6 B10 B11 62.6(2) . . ? B6 B10 B5 60.6(2) . . ? B11 B10 B5 110.5(3) . . ? B6 B10 B12 109.0(3) . . ? B11 B10 B12 59.5(2) . . ? B5 B10 B12 107.3(3) . . ? B6 B10 B9 108.2(3) . . ? B11 B10 B9 108.3(3) . . ? B5 B10 B9 59.1(2) . . ? B12 B10 B9 59.5(2) . . ? B7 B12 B11 61.5(2) . . ? B7 B12 B9 108.1(3) . . ? B11 B12 B9 109.4(3) . . ? B7 B12 B10 108.4(3) . . ? B11 B12 B10 60.1(2) . . ? B9 B12 B10 60.3(2) . . ? B7 B12 B8 59.9(2) . . ? B11 B12 B8 110.1(3) . . ? B9 B12 B8 60.1(2) . . ? B10 B12 B8 108.5(3) . . ? B12 B11 B10 60.4(2) . . ? B12 B11 B7 59.0(2) . . ? B10 B11 B7 106.7(3) . . ? B12 B11 B6 106.5(3) . . ? B10 B11 B6 58.6(2) . . ? B7 B11 B6 106.0(3) . . ? B12 B11 Ru3 140.1(3) . . ? B10 B11 Ru3 144.0(3) . . ? B7 B11 Ru3 109.1(2) . . ? B6 B11 Ru3 113.3(3) . . ? B12 B11 Ru1 118.8(2) . . ? B10 B11 Ru1 118.6(2) . . ? B7 B11 Ru1 65.59(18) . . ? B6 B11 Ru1 65.62(18) . . ? Ru3 B11 Ru1 80.39(15) . . ? O11 C11 Ru1 175.8(4) . . ? O12 C12 Ru1 173.0(3) . . ? O13 C13 Ru2 178.9(4) . . ? O14 C14 Ru2 176.9(4) . . ? O15 C15 Ru3 173.7(4) . . ? O16 C16 Ru3 177.6(4) . . ? C22 S1 C21 99.0(2) . . ? C22 S1 C1 106.90(18) . . ? C21 S1 C1 108.32(19) . . ? C111 Fe1 C212 107.90(15) . . ? C111 Fe1 C112 41.58(15) . . ? C212 Fe1 C112 125.50(16) . . ? C111 Fe1 C115 41.48(15) . . ? C212 Fe1 C115 121.79(15) . . ? C112 Fe1 C115 69.35(16) . . ? C111 Fe1 C211 127.34(15) . . ? C212 Fe1 C211 41.15(14) . . ? C112 Fe1 C211 164.57(15) . . ? C115 Fe1 C211 109.38(15) . . ? C111 Fe1 C215 165.94(15) . . ? C212 Fe1 C215 68.83(15) . . ? C112 Fe1 C215 151.53(15) . . ? C115 Fe1 C215 127.64(16) . . ? C211 Fe1 C215 41.33(14) . . ? C111 Fe1 C213 118.97(16) . . ? C212 Fe1 C213 40.73(14) . . ? C112 Fe1 C213 105.60(17) . . ? C115 Fe1 C213 155.65(16) . . ? C211 Fe1 C213 68.88(15) . . ? C215 Fe1 C213 68.11(16) . . ? C111 Fe1 C214 152.43(16) . . ? C212 Fe1 C214 68.16(16) . . ? C112 Fe1 C214 116.92(16) . . ? C115 Fe1 C214 163.79(16) . . ? C211 Fe1 C214 68.76(15) . . ? C215 Fe1 C214 40.41(15) . . ? C213 Fe1 C214 40.06(16) . . ? C111 Fe1 C113 69.14(15) . . ? C212 Fe1 C113 162.21(16) . . ? C112 Fe1 C113 40.76(15) . . ? C115 Fe1 C113 68.38(17) . . ? C211 Fe1 C113 154.21(16) . . ? C215 Fe1 C113 118.28(16) . . ? C213 Fe1 C113 124.14(17) . . ? C214 Fe1 C113 105.89(17) . . ? C111 Fe1 C114 69.16(16) . . ? C212 Fe1 C114 156.58(16) . . ? C112 Fe1 C114 68.64(16) . . ? C115 Fe1 C114 40.62(16) . . ? C211 Fe1 C114 121.07(16) . . ? C215 Fe1 C114 108.08(16) . . ? C213 Fe1 C114 161.51(16) . . ? C214 Fe1 C114 125.45(17) . . ? C113 Fe1 C114 40.30(17) . . ? C111 P1 C131 103.86(17) . . ? C111 P1 C121 102.29(17) . . ? C131 P1 C121 102.39(17) . . ? C111 P1 Ru2 117.27(12) . . ? C131 P1 Ru2 118.45(12) . . ? C121 P1 Ru2 110.43(12) . . ? C115 C111 C112 107.3(3) . . ? C115 C111 P1 125.0(3) . . ? C112 C111 P1 127.7(3) . . ? C115 C111 Fe1 69.9(2) . . ? C112 C111 Fe1 69.7(2) . . ? P1 C111 Fe1 126.34(19) . . ? C113 C112 C111 107.6(4) . . ? C113 C112 Fe1 70.2(2) . . ? C111 C112 Fe1 68.8(2) . . ? C114 C113 C112 108.7(4) . . ? C114 C113 Fe1 70.0(2) . . ? C112 C113 Fe1 69.1(2) . . ? C113 C114 C115 108.4(4) . . ? C113 C114 Fe1 69.8(2) . . ? C115 C114 Fe1 69.2(2) . . ? C114 C115 C111 108.0(3) . . ? C114 C115 Fe1 70.2(2) . . ? C111 C115 Fe1 68.6(2) . . ? C126 C121 C122 118.8(4) . . ? C126 C121 P1 121.2(3) . . ? C122 C121 P1 119.9(3) . . ? C123 C122 C121 120.7(4) . . ? C124 C123 C122 119.7(4) . . ? C125 C124 C123 119.9(4) . . ? C124 C125 C126 120.4(5) . . ? C121 C126 C125 120.5(4) . . ? C132 C131 C136 118.8(4) . . ? C132 C131 P1 121.5(3) . . ? C136 C131 P1 119.8(3) . . ? C133 C132 C131 120.2(4) . . ? C132 C133 C134 120.8(4) . . ? C135 C134 C133 119.2(4) . . ? C136 C135 C134 120.2(4) . . ? C135 C136 C131 120.8(4) . . ? C211 P2 C221 100.49(17) . . ? C211 P2 C231 99.80(18) . . ? C221 P2 C231 101.73(18) . . ? C211 P2 Ru3 118.67(13) . . ? C221 P2 Ru3 115.93(12) . . ? C231 P2 Ru3 117.20(13) . . ? C212 C211 C215 106.6(3) . . ? C212 C211 P2 127.3(3) . . ? C215 C211 P2 125.9(3) . . ? C212 C211 Fe1 69.0(2) . . ? C215 C211 Fe1 69.4(2) . . ? P2 C211 Fe1 130.4(2) . . ? C213 C212 C211 108.4(3) . . ? C213 C212 Fe1 70.2(2) . . ? C211 C212 Fe1 69.8(2) . . ? C214 C213 C212 108.2(3) . . ? C214 C213 Fe1 70.1(2) . . ? C212 C213 Fe1 69.0(2) . . ? C213 C214 C215 108.8(3) . . ? C213 C214 Fe1 69.8(2) . . ? C215 C214 Fe1 69.6(2) . . ? C214 C215 C211 108.0(3) . . ? C214 C215 Fe1 70.0(2) . . ? C211 C215 Fe1 69.2(2) . . ? C222 C221 C226 118.8(4) . . ? C222 C221 P2 121.5(3) . . ? C226 C221 P2 119.7(3) . . ? C223 C222 C221 120.3(4) . . ? C224 C223 C222 120.3(4) . . ? C223 C224 C225 120.1(4) . . ? C226 C225 C224 120.1(4) . . ? C225 C226 C221 120.3(4) . . ? C236 C231 C232 117.8(4) . . ? C236 C231 P2 120.6(3) . . ? C232 C231 P2 121.4(3) . . ? C233 C232 C231 120.6(4) . . ? C234 C233 C232 120.5(4) . . ? C235 C234 C233 119.8(4) . . ? C234 C235 C236 119.8(5) . . ? C231 C236 C235 121.5(4) . . ? C103 O100 C100 106.8(4) . . ? O100 C100 C101 106.5(4) . . ? C102 C101 C100 106.4(5) . . ? C101 C102 C103 105.5(5) . . ? O100 C103 C102 106.7(5) . . ? C200 O200 C203 109.0(5) . . ? O200 C200 C201 107.1(5) . . ? C200 C201 C202 100.2(6) . . ? C203 C202 C201 102.1(5) . . ? O200 C203 C202 104.3(6) . . ? C300 O300 C303 107.2(9) . . ? O300 C300 C301 105.8(10) . . ? C302 C301 C300 103.8(10) . . ? C303 C302 C301 104.9(10) . . ? C302 C303 O300 107.1(10) . . ? C400 O400 C403 111.2(10) . . ? O400 C400 C401 105.4(9) . . ? C400 C401 C402 102.1(9) . . ? C403 C402 C401 100.9(9) . . ? C402 C403 O400 106.2(10) . . ? _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.762 _refine_diff_density_min -0.977 _refine_diff_density_rms 0.136 #============================================================================== data_8 _database_code_depnum_ccdc_archive 'CCDC 268996' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C35 H46 B20 Cl2 O6 P2 Ru3 S' _chemical_formula_weight 1247.03 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P2(1)/c ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.861(2) _cell_length_b 38.045(8) _cell_length_c 12.413(3) _cell_angle_alpha 90.00 _cell_angle_beta 94.27(3) _cell_angle_gamma 90.00 _cell_volume 5585.9(19) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 3712 _cell_measurement_theta_min 2.30 _cell_measurement_theta_max 22.48 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_min 0.035 _exptl_crystal_size_mid 0.108 _exptl_crystal_size_max 0.136 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.483 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2464 _exptl_absorpt_coefficient_mu 1.030 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.49 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_process_details 'TWINABS (Bruker, 2003)' _exptl_special_details ; Crystals of compound 11 were badly twinned and although the unresolved data could be solved and partially refined in various monoclinic space groups, the refinement was not stable and anisotropic refinement could not be achieved. However, use of CELL_NOW (Bruker, 2003) resolved two main domains and allowed their separate integration and data reduction (Bruker, 2003). From the resulting (somewhat approximate) intensity data, the structure could be solved and refined without great difficulty. However, the poor quality of the data so obtained (R~int~ is over 20%) still prevented a very accurate determination. Despite this, there is no question as to the connectivity pattern and in particular that the dppc ligand is bonded to only a single ruthenium atom. ; _diffrn_ambient_temperature 110(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 'Bruker-Nonius X8 Apex CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 38079 _diffrn_reflns_av_R_equivalents 0.2105 _diffrn_reflns_av_sigmaI/netI 0.4347 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -40 _diffrn_reflns_limit_k_max 50 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.03 _diffrn_reflns_theta_max 28.37 _reflns_number_total 11675 _reflns_number_gt 4896 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2 (Bruker, 2003)' _computing_cell_refinement 'Bruker APEX2 (Bruker, 2003)' _computing_data_reduction 'Bruker APEX2 (Bruker, 2003)' _computing_structure_solution 'Bruker SHELXTL (Bruker, 2000)' _computing_structure_refinement 'Bruker SHELXTL (Bruker, 2000)' _computing_molecular_graphics 'Bruker SHELXTL (Bruker, 2000)' _computing_publication_material 'Bruker SHELXTL (Bruker, 2000)' _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^)+(0.1096P)^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 SHELXL _refine_ls_extinction_coef 0.0090(6) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 11675 _refine_ls_number_parameters 639 _refine_ls_number_restraints 291 _refine_ls_R_factor_all 0.2217 _refine_ls_R_factor_gt 0.1059 _refine_ls_wR_factor_ref 0.2549 _refine_ls_wR_factor_gt 0.2250 _refine_ls_goodness_of_fit_ref 0.982 _refine_ls_restrained_S_all 0.970 _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 0.90830(9) 0.13146(2) -0.11342(7) 0.0189(3) Uani 1 1 d . . . Ru2 Ru 0.92870(9) 0.10482(2) 0.09660(7) 0.0178(3) Uani 1 1 d . . . Ru3 Ru 1.13191(9) 0.12096(2) -0.02672(8) 0.0217(3) Uani 1 1 d . . . C1 C 0.8425(11) 0.1835(3) -0.1767(9) 0.023(2) Uani 1 1 d U . . B3 B 0.7856(14) 0.1708(3) -0.0520(11) 0.024(3) Uani 1 1 d U . . H3 H 0.7036 0.1582 -0.0418 0.028 Uiso 1 1 calc R . . B4 B 0.7987(15) 0.2164(3) -0.0981(12) 0.029(3) Uani 1 1 d U . . H4 H 0.7219 0.2319 -0.1185 0.034 Uiso 1 1 calc R . . B5 B 0.9163(15) 0.2216(3) -0.1722(11) 0.028(3) Uani 1 1 d U . . H5 H 0.9160 0.2403 -0.2399 0.034 Uiso 1 1 calc R . . B6 B 0.9880(13) 0.1800(3) -0.1788(11) 0.024(3) Uani 1 1 d U . . H6 H 1.0335 0.1725 -0.2494 0.029 Uiso 1 1 calc R . . B7 B 0.9115(14) 0.1639(3) 0.0356(10) 0.022(3) Uani 1 1 d U . . H7 H 0.922(10) 0.149(3) 0.133(9) 0.026 Uiso 1 1 d . . . B8 B 0.8412(14) 0.2053(4) 0.0359(12) 0.027(3) Uani 1 1 d U . . H8 H 0.7932 0.2136 0.1040 0.033 Uiso 1 1 calc R . . B9 B 0.9206(15) 0.2357(4) -0.0359(11) 0.031(3) Uani 1 1 d U . . H9 H 0.9242 0.2636 -0.0128 0.037 Uiso 1 1 calc R . . B10 B 1.0390(15) 0.2145(4) -0.0872(11) 0.029(3) Uani 1 1 d U . . H10 H 1.1182 0.2284 -0.0996 0.035 Uiso 1 1 calc R . . B11 B 1.0372(14) 0.1700(4) -0.0385(11) 0.026(3) Uani 1 1 d U . . B12 B 0.9941(14) 0.2041(4) 0.0448(11) 0.026(3) Uani 1 1 d U . . H12 H 1.0455 0.2112 0.1190 0.031 Uiso 1 1 calc R . . H100 H 1.095(11) 0.110(3) 0.095(9) 0.031 Uiso 1 1 d . . . C11 C 0.7857(11) 0.1006(3) -0.1521(9) 0.021(3) Uani 1 1 d U . . O11 O 0.7103(8) 0.0837(2) -0.1896(6) 0.027(2) Uani 1 1 d U . . C12 C 0.9917(13) 0.1034(3) -0.2070(9) 0.031(3) Uani 1 1 d U . . O12 O 1.0290(8) 0.0852(2) -0.2724(7) 0.037(2) Uani 1 1 d U . . C13 C 0.9316(12) 0.0608(3) 0.0307(10) 0.023(3) Uani 1 1 d U . . O13 O 0.9358(8) 0.0345(2) -0.0190(6) 0.028(2) Uani 1 1 d U . . C14 C 1.1818(11) 0.0708(3) -0.0382(11) 0.024(3) Uani 1 1 d U . . O14 O 1.2107(9) 0.0423(3) -0.0444(8) 0.040(3) Uani 1 1 d U . . C15 C 1.2392(13) 0.1401(4) 0.0742(10) 0.037(3) Uani 1 1 d U . . O15 O 1.3021(10) 0.1515(3) 0.1378(9) 0.064(3) Uani 1 1 d U . . C16 C 1.2149(13) 0.1382(3) -0.1409(10) 0.032(3) Uani 1 1 d U . . O16 O 1.2676(9) 0.1499(3) -0.2070(7) 0.043(3) Uani 1 1 d U . . S1 S 0.7457(3) 0.17445(8) -0.2925(3) 0.0297(8) Uani 1 1 d . . . C21 C 0.8302(14) 0.1590(3) -0.3962(10) 0.040(4) Uani 1 1 d . . . H21A H 0.7824 0.1537 -0.4599 0.060 Uiso 1 1 calc R . . H21B H 0.8702 0.1382 -0.3718 0.060 Uiso 1 1 calc R . . H21C H 0.8835 0.1769 -0.4126 0.060 Uiso 1 1 calc R . . C22 C 0.6950(13) 0.2155(3) -0.3504(11) 0.040(4) Uani 1 1 d . . . H22A H 0.6472 0.2269 -0.3018 0.060 Uiso 1 1 calc R . . H22B H 0.6527 0.2111 -0.4180 0.060 Uiso 1 1 calc R . . H22C H 0.7581 0.2305 -0.3622 0.060 Uiso 1 1 calc R . . P1 P 0.7487(3) 0.09812(8) 0.1560(2) 0.0193(7) Uani 1 1 d . . . C31 C 0.6414(11) 0.0807(3) 0.0586(9) 0.021(3) Uani 1 1 d U . . C32 C 0.6464(11) 0.0464(3) 0.0206(9) 0.022(3) Uani 1 1 d U . . H32 H 0.7045 0.0318 0.0482 0.026 Uiso 1 1 calc R . . C33 C 0.5672(11) 0.0332(3) -0.0574(9) 0.025(3) Uani 1 1 d U . . H33 H 0.5706 0.0098 -0.0793 0.031 Uiso 1 1 calc R . . C34 C 0.4808(12) 0.0559(3) -0.1035(10) 0.031(3) Uani 1 1 d U . . H34 H 0.4275 0.0474 -0.1559 0.038 Uiso 1 1 calc R . . C35 C 0.4769(12) 0.0896(3) -0.0705(10) 0.029(3) Uani 1 1 d U . . H35 H 0.4202 0.1043 -0.1000 0.035 Uiso 1 1 calc R . . C36 C 0.5590(12) 0.1028(3) 0.0093(9) 0.028(3) Uani 1 1 d U . . H36 H 0.5575 0.1264 0.0286 0.033 Uiso 1 1 calc R . . C41 C 0.6802(12) 0.1356(3) 0.2228(9) 0.025(3) Uani 1 1 d . . . C42 C 0.5680(12) 0.1359(3) 0.2389(10) 0.029(3) Uani 1 1 d . . . H42 H 0.5223 0.1177 0.2115 0.035 Uiso 1 1 calc R . . C43 C 0.5197(15) 0.1632(4) 0.2959(11) 0.047(4) Uani 1 1 d . . . H43 H 0.4430 0.1633 0.3069 0.056 Uiso 1 1 calc R . . C44 C 0.5933(13) 0.1910(3) 0.3366(10) 0.036(4) Uani 1 1 d . . . H44 H 0.5633 0.2099 0.3726 0.043 Uiso 1 1 calc R . . C45 C 0.7014(13) 0.1901(3) 0.3238(10) 0.031(3) Uani 1 1 d . . . H45 H 0.7476 0.2080 0.3526 0.037 Uiso 1 1 calc R . . C46 C 0.7489(12) 0.1627(3) 0.2676(9) 0.023(3) Uani 1 1 d . . . H46 H 0.8263 0.1623 0.2599 0.028 Uiso 1 1 calc R . . P2 P 1.0004(3) 0.08564(8) 0.2623(2) 0.0189(7) Uani 1 1 d . . . C51 C 1.1268(11) 0.0572(3) 0.2630(10) 0.022(3) Uani 1 1 d . . . C52 C 1.2318(12) 0.0691(3) 0.3054(11) 0.032(3) Uani 1 1 d . . . H52 H 1.2382 0.0917 0.3337 0.038 Uiso 1 1 calc R . . C53 C 1.3247(12) 0.0484(4) 0.3062(11) 0.033(3) Uani 1 1 d . . . H53 H 1.3942 0.0569 0.3344 0.039 Uiso 1 1 calc R . . C54 C 1.3166(13) 0.0147(4) 0.2656(11) 0.039(4) Uani 1 1 d . . . H54 H 1.3800 0.0002 0.2709 0.046 Uiso 1 1 calc R . . C55 C 1.2166(13) 0.0022(3) 0.2173(9) 0.031(3) Uani 1 1 d . . . H55 H 1.2122 -0.0202 0.1870 0.037 Uiso 1 1 calc R . . C56 C 1.1230(12) 0.0237(3) 0.2152(9) 0.028(3) Uani 1 1 d . . . H56 H 1.0553 0.0159 0.1809 0.034 Uiso 1 1 calc R . . C61 C 1.0479(12) 0.1196(3) 0.3630(10) 0.030(3) Uani 1 1 d . . . C62 C 1.0887(13) 0.1112(4) 0.4644(10) 0.038(4) Uani 1 1 d . . . H62 H 1.0858 0.0879 0.4866 0.046 Uiso 1 1 calc R . . C63 C 1.1360(15) 0.1370(5) 0.5386(13) 0.053(5) Uani 1 1 d . . . H63 H 1.1669 0.1309 0.6071 0.063 Uiso 1 1 calc R . . C64 C 1.1337(16) 0.1708(5) 0.5042(16) 0.068(6) Uani 1 1 d . . . H64 H 1.1567 0.1884 0.5530 0.082 Uiso 1 1 calc R . . C65 C 1.0982(15) 0.1801(4) 0.3992(14) 0.052(5) Uani 1 1 d . . . H65 H 1.1047 0.2032 0.3758 0.062 Uiso 1 1 calc R . . C66 C 1.0525(12) 0.1542(3) 0.3291(12) 0.034(4) Uani 1 1 d . . . H66 H 1.0250 0.1602 0.2594 0.041 Uiso 1 1 calc R . . C101 C 0.7553(11) 0.0652(3) 0.2737(9) 0.020(2) Uani 1 1 d U . . C102 C 0.8898(10) 0.0587(3) 0.3293(8) 0.0163(19) Uani 1 1 d U . . B103 B 0.7949(13) 0.0822(4) 0.4007(10) 0.020(2) Uani 1 1 d U . . H103 H 0.8045 0.1104 0.4183 0.024 Uiso 1 1 calc R . . B104 B 0.6598(14) 0.0626(4) 0.3707(11) 0.028(2) Uani 1 1 d U . . H104 H 0.5818 0.0783 0.3692 0.033 Uiso 1 1 calc R . . B105 B 0.6752(13) 0.0272(4) 0.2794(11) 0.025(2) Uani 1 1 d U . . H105 H 0.6066 0.0199 0.2190 0.030 Uiso 1 1 calc R . . B106 B 0.8214(12) 0.0257(3) 0.2501(11) 0.020(2) Uani 1 1 d U . . H106 H 0.8490 0.0177 0.1710 0.024 Uiso 1 1 calc R . . B107 B 0.8856(13) 0.0488(3) 0.4648(11) 0.023(2) Uani 1 1 d U . . H107 H 0.9549 0.0554 0.5253 0.028 Uiso 1 1 calc R . . B108 B 0.7418(14) 0.0518(4) 0.4935(11) 0.027(3) Uani 1 1 d U . . H108 H 0.7174 0.0606 0.5729 0.033 Uiso 1 1 calc R . . B109 B 0.6661(14) 0.0182(4) 0.4174(12) 0.033(3) Uani 1 1 d U . . H109 H 0.5922 0.0051 0.4478 0.039 Uiso 1 1 calc R . . B110 B 0.7643(14) -0.0044(4) 0.3406(11) 0.028(3) Uani 1 1 d U . . H110 H 0.7541 -0.0324 0.3190 0.033 Uiso 1 1 calc R . . B111 B 0.9029(13) 0.0150(3) 0.3763(11) 0.024(2) Uani 1 1 d U . . H111 H 0.9822 -0.0001 0.3795 0.028 Uiso 1 1 calc R . . B112 B 0.8044(14) 0.0100(4) 0.4743(12) 0.029(3) Uani 1 1 d U . . H112 H 0.8189 -0.0089 0.5409 0.035 Uiso 1 1 calc R . . C100 C 0.506(4) -0.1165(9) 0.351(2) 0.077(18) Uani 0.358(10) 1 d PDU . . H10A H 0.4352 -0.1083 0.3160 0.092 Uiso 0.358(10) 1 calc PR . . H10B H 0.5449 -0.1303 0.2991 0.092 Uiso 0.358(10) 1 calc PR . . Cl1 Cl 0.5908(13) -0.0803(3) 0.3952(11) 0.088(7) Uani 0.358(10) 1 d PD . . Cl2 Cl 0.4816(11) -0.1422(3) 0.4639(9) 0.058(4) Uani 0.358(10) 1 d PD . . 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 0.0253(6) 0.0124(7) 0.0186(5) 0.0012(4) -0.0012(4) 0.0013(4) Ru2 0.0221(6) 0.0123(7) 0.0186(5) 0.0006(3) -0.0017(4) 0.0008(4) Ru3 0.0225(6) 0.0188(7) 0.0237(6) 0.0023(4) -0.0002(5) 0.0001(4) C1 0.035(6) 0.014(6) 0.022(5) 0.000(4) 0.002(5) 0.000(4) B3 0.037(6) 0.008(6) 0.026(7) 0.010(4) -0.001(5) 0.003(5) B4 0.048(6) 0.003(6) 0.034(7) 0.005(4) -0.002(5) 0.007(5) B5 0.053(8) 0.005(6) 0.025(5) 0.004(4) 0.000(5) -0.004(5) B6 0.033(6) 0.015(7) 0.024(5) 0.003(4) -0.002(5) -0.003(5) B7 0.037(8) 0.017(6) 0.011(6) 0.000(4) -0.004(4) -0.006(4) B8 0.036(6) 0.022(7) 0.023(5) -0.001(4) 0.000(5) 0.002(5) B9 0.054(8) 0.010(6) 0.027(6) 0.000(4) -0.002(5) 0.000(4) B10 0.045(6) 0.013(7) 0.029(7) 0.004(4) 0.002(5) -0.009(5) B11 0.037(6) 0.017(6) 0.025(6) 0.004(4) 0.000(5) 0.000(5) B12 0.037(6) 0.015(7) 0.026(5) 0.002(4) 0.003(5) -0.002(5) C11 0.032(8) 0.018(8) 0.015(6) 0.003(4) 0.006(5) 0.005(5) O11 0.028(6) 0.026(6) 0.026(5) -0.004(3) 0.001(4) -0.004(4) C12 0.048(10) 0.029(9) 0.014(7) -0.010(5) -0.014(6) 0.000(6) O12 0.042(7) 0.039(7) 0.031(6) -0.011(4) 0.002(5) 0.005(4) C13 0.036(8) 0.011(8) 0.022(7) 0.011(4) -0.005(6) 0.007(5) O13 0.039(6) 0.021(6) 0.024(5) -0.002(3) 0.003(4) 0.005(4) C14 0.011(7) 0.016(8) 0.048(8) 0.006(6) 0.013(6) -0.004(5) O14 0.030(7) 0.039(7) 0.054(7) 0.010(5) 0.020(5) 0.003(5) C15 0.034(10) 0.057(11) 0.020(8) -0.003(6) 0.012(6) -0.005(7) O15 0.025(7) 0.111(10) 0.052(8) -0.006(6) -0.013(6) -0.017(6) C16 0.040(9) 0.037(10) 0.020(7) 0.009(5) 0.003(6) -0.005(6) O16 0.034(7) 0.068(8) 0.030(6) 0.020(4) 0.016(5) 0.002(5) S1 0.035(2) 0.026(2) 0.0279(19) 0.0057(12) -0.0017(16) 0.0030(14) C21 0.059(12) 0.033(10) 0.026(8) -0.002(5) -0.004(7) 0.011(7) C22 0.043(10) 0.043(10) 0.034(9) 0.002(6) -0.007(7) 0.005(7) P1 0.0208(19) 0.018(2) 0.0193(17) -0.0014(11) 0.0007(14) 0.0019(12) C31 0.022(7) 0.010(7) 0.031(7) 0.004(4) -0.002(5) -0.007(5) C32 0.027(7) 0.019(6) 0.020(6) 0.003(4) 0.012(5) 0.000(5) C33 0.031(8) 0.027(8) 0.020(6) -0.006(4) 0.011(5) -0.004(5) C34 0.029(8) 0.041(8) 0.024(7) -0.005(5) -0.001(6) -0.010(5) C35 0.018(7) 0.034(7) 0.036(8) -0.001(5) 0.002(6) 0.007(5) C36 0.034(8) 0.024(7) 0.024(7) -0.008(5) 0.000(5) 0.018(5) C41 0.049(10) 0.003(8) 0.022(7) -0.001(4) -0.006(6) 0.006(5) C42 0.026(9) 0.029(9) 0.031(8) -0.014(5) -0.002(6) 0.008(6) C43 0.052(12) 0.063(12) 0.024(8) -0.008(6) -0.006(8) 0.015(8) C44 0.048(11) 0.030(10) 0.027(8) -0.019(6) -0.010(7) 0.020(7) C45 0.038(10) 0.018(9) 0.036(8) -0.005(5) -0.003(7) 0.011(6) C46 0.032(9) 0.018(8) 0.020(7) -0.002(5) 0.006(6) 0.002(5) P2 0.0219(19) 0.018(2) 0.0159(16) -0.0001(11) -0.0025(14) -0.0006(13) C51 0.019(7) 0.019(9) 0.028(7) 0.011(5) -0.002(6) 0.005(5) C52 0.027(9) 0.024(9) 0.045(9) -0.002(6) 0.003(7) -0.004(6) C53 0.015(8) 0.034(10) 0.050(10) 0.007(6) 0.003(7) 0.007(6) C54 0.027(10) 0.065(12) 0.024(8) 0.012(6) 0.007(7) 0.027(7) C55 0.049(11) 0.027(9) 0.017(7) -0.001(5) 0.007(7) 0.016(6) C56 0.036(9) 0.034(10) 0.014(7) -0.002(5) -0.005(6) 0.007(6) C61 0.039(9) 0.035(10) 0.014(7) -0.010(5) -0.009(6) -0.013(6) C62 0.044(10) 0.056(11) 0.016(7) -0.003(5) 0.008(7) -0.031(7) C63 0.049(12) 0.073(14) 0.038(10) 0.009(8) 0.011(8) -0.042(9) C64 0.047(13) 0.086(16) 0.076(15) -0.053(11) 0.029(11) -0.034(10) C65 0.058(13) 0.029(11) 0.067(12) -0.019(7) 0.002(10) -0.013(7) C66 0.035(9) 0.012(9) 0.052(10) -0.005(6) -0.020(7) 0.004(6) C101 0.025(6) 0.016(5) 0.018(4) -0.001(4) -0.002(4) 0.002(4) C102 0.024(5) 0.010(5) 0.015(5) 0.002(3) 0.001(4) 0.004(4) B103 0.023(7) 0.024(6) 0.014(5) 0.001(3) 0.008(5) 0.003(4) B104 0.026(5) 0.033(6) 0.024(7) -0.002(4) 0.000(4) 0.000(5) B105 0.025(5) 0.024(7) 0.027(5) 0.002(4) 0.004(5) -0.004(4) B106 0.024(6) 0.011(6) 0.025(5) 0.002(4) -0.001(4) -0.002(4) B107 0.028(6) 0.024(7) 0.017(5) 0.004(4) -0.001(5) 0.001(4) B108 0.034(7) 0.032(7) 0.017(5) 0.004(4) 0.010(4) -0.001(5) B109 0.031(5) 0.038(7) 0.030(6) 0.007(5) 0.005(5) -0.006(5) B110 0.037(8) 0.019(6) 0.026(6) 0.007(4) 0.001(5) -0.007(4) B111 0.032(5) 0.014(6) 0.025(6) 0.007(4) 0.002(4) 0.001(4) B112 0.033(7) 0.026(6) 0.028(5) 0.006(5) 0.005(5) -0.005(5) C100 0.05(3) 0.10(4) 0.07(4) 0.02(3) -0.05(3) -0.03(3) Cl1 0.102(13) 0.056(10) 0.096(11) 0.031(7) -0.054(9) -0.053(8) Cl2 0.075(10) 0.053(9) 0.044(7) 0.010(5) 0.000(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 C11 1.902(13) . ? Ru1 C12 1.907(14) . ? Ru1 B7 2.222(13) . ? Ru1 C1 2.249(11) . ? Ru1 B6 2.254(14) . ? Ru1 B3 2.260(15) . ? Ru1 B11 2.268(15) . ? Ru1 Ru2 2.7907(14) . ? Ru1 Ru3 2.8155(16) . ? Ru2 H7 1.75(10) . ? Ru2 C13 1.864(13) . ? Ru2 H100 1.98(13) . ? Ru2 P2 2.286(3) . ? Ru2 P1 2.324(4) . ? Ru2 B7 2.375(13) . ? Ru2 Ru3 3.0131(17) . ? Ru3 H100 1.66(11) . ? Ru3 C15 1.865(14) . ? Ru3 C16 1.902(14) . ? Ru3 C14 2.006(14) . ? Ru3 B11 2.178(14) . ? C1 B4 1.691(19) . ? C1 B5 1.691(19) . ? C1 B6 1.73(2) . ? C1 B3 1.800(19) . ? C1 S1 1.805(12) . ? B3 B8 1.800(19) . ? B3 B7 1.80(2) . ? B3 B4 1.836(18) . ? B4 B5 1.74(2) . ? B4 B9 1.75(2) . ? B4 B8 1.753(19) . ? B5 B10 1.75(2) . ? B5 B9 1.77(2) . ? B5 B6 1.80(2) . ? B6 B10 1.810(19) . ? B6 B11 1.835(19) . ? B7 H7 1.33(11) . ? B7 B8 1.78(2) . ? B7 B12 1.81(2) . ? B7 B11 1.82(2) . ? B8 B9 1.77(2) . ? B8 B12 1.81(2) . ? B9 B12 1.76(2) . ? B9 B10 1.78(2) . ? B10 B11 1.796(19) . ? B10 B12 1.80(2) . ? B11 B12 1.76(2) . ? C11 O11 1.170(14) . ? C12 O12 1.178(14) . ? C13 O13 1.179(13) . ? C14 O14 1.143(13) . ? C15 O15 1.132(16) . ? C16 O16 1.157(15) . ? S1 C21 1.789(14) . ? S1 C22 1.805(13) . ? P1 C31 1.814(12) . ? P1 C41 1.867(12) . ? P1 C101 1.923(11) . ? C31 C36 1.394(16) . ? C31 C32 1.393(15) . ? C32 C33 1.391(17) . ? C33 C34 1.426(18) . ? C34 C35 1.348(16) . ? C35 C36 1.428(17) . ? C41 C42 1.361(19) . ? C41 C46 1.400(17) . ? C42 C43 1.401(18) . ? C43 C44 1.44(2) . ? C44 C45 1.304(19) . ? C45 C46 1.398(17) . ? P2 C51 1.849(13) . ? P2 C61 1.856(12) . ? P2 C102 1.903(12) . ? C51 C52 1.391(18) . ? C51 C56 1.404(17) . ? C52 C53 1.355(19) . ? C53 C54 1.377(18) . ? C54 C55 1.37(2) . ? C55 C56 1.379(19) . ? C61 C62 1.352(18) . ? C61 C66 1.383(17) . ? C62 C63 1.43(2) . ? C63 C64 1.35(2) . ? C64 C65 1.39(2) . ? C65 C66 1.399(19) . ? C101 C102 1.708(17) . ? C101 B104 1.72(2) . ? C101 B106 1.730(18) . ? C101 B105 1.732(18) . ? C101 B103 1.736(17) . ? C102 B107 1.729(17) . ? C102 B103 1.731(18) . ? C102 B106 1.757(16) . ? C102 B111 1.767(16) . ? B103 B108 1.779(19) . ? B103 B104 1.78(2) . ? B103 B107 1.810(19) . ? B104 B105 1.78(2) . ? B104 B109 1.78(2) . ? B104 B108 1.79(2) . ? B105 B110 1.74(2) . ? B105 B109 1.76(2) . ? B105 B106 1.80(2) . ? B106 B110 1.77(2) . ? B106 B111 1.824(19) . ? B107 B111 1.713(19) . ? B107 B112 1.77(2) . ? B107 B108 1.77(2) . ? B108 B112 1.78(2) . ? B108 B109 1.79(2) . ? B109 B112 1.77(2) . ? B109 B110 1.78(2) . ? B110 B112 1.78(2) . ? B110 B111 1.83(2) . ? B111 B112 1.76(2) . ? C100 Cl2 1.753(19) . ? C100 Cl1 1.766(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 C11 Ru1 C12 85.6(5) . . ? C11 Ru1 B7 121.2(5) . . ? C12 Ru1 B7 147.2(6) . . ? C11 Ru1 C1 102.5(5) . . ? C12 Ru1 C1 117.5(5) . . ? B7 Ru1 C1 77.6(4) . . ? C11 Ru1 B6 138.4(5) . . ? C12 Ru1 B6 89.4(6) . . ? B7 Ru1 B6 82.1(5) . . ? C1 Ru1 B6 45.3(5) . . ? C11 Ru1 B3 89.7(5) . . ? C12 Ru1 B3 162.3(5) . . ? B7 Ru1 B3 47.4(5) . . ? C1 Ru1 B3 47.1(5) . . ? B6 Ru1 B3 82.9(6) . . ? C11 Ru1 B11 169.1(5) . . ? C12 Ru1 B11 104.3(6) . . ? B7 Ru1 B11 47.9(6) . . ? C1 Ru1 B11 77.3(5) . . ? B6 Ru1 B11 47.9(5) . . ? B3 Ru1 B11 82.2(5) . . ? C11 Ru1 Ru2 91.3(3) . . ? C12 Ru1 Ru2 110.7(4) . . ? B7 Ru1 Ru2 55.2(3) . . ? C1 Ru1 Ru2 130.5(3) . . ? B6 Ru1 Ru2 128.7(3) . . ? B3 Ru1 Ru2 86.5(3) . . ? B11 Ru1 Ru2 81.0(3) . . ? C11 Ru1 Ru3 133.6(4) . . ? C12 Ru1 Ru3 68.7(4) . . ? B7 Ru1 Ru3 78.6(4) . . ? C1 Ru1 Ru3 123.4(3) . . ? B6 Ru1 Ru3 81.1(4) . . ? B3 Ru1 Ru3 125.2(4) . . ? B11 Ru1 Ru3 49.3(4) . . ? Ru2 Ru1 Ru3 65.02(4) . . ? H7 Ru2 C13 169(4) . . ? H7 Ru2 H100 88(5) . . ? C13 Ru2 H100 92(3) . . ? H7 Ru2 P2 95(4) . . ? C13 Ru2 P2 95.2(3) . . ? H100 Ru2 P2 75(3) . . ? H7 Ru2 P1 88(4) . . ? C13 Ru2 P1 95.0(4) . . ? H100 Ru2 P1 162(3) . . ? P2 Ru2 P1 88.20(12) . . ? H7 Ru2 B7 34(4) . . ? C13 Ru2 B7 135.5(5) . . ? H100 Ru2 B7 88(3) . . ? P2 Ru2 B7 127.3(3) . . ? P1 Ru2 B7 98.4(4) . . ? H7 Ru2 Ru1 84(4) . . ? C13 Ru2 Ru1 85.4(3) . . ? H100 Ru2 Ru1 88(3) . . ? P2 Ru2 Ru1 163.13(10) . . ? P1 Ru2 Ru1 108.57(9) . . ? B7 Ru2 Ru1 50.2(3) . . ? H7 Ru2 Ru3 89(4) . . ? C13 Ru2 Ru3 85.3(4) . . ? H100 Ru2 Ru3 31(3) . . ? P2 Ru2 Ru3 105.31(9) . . ? P1 Ru2 Ru3 166.42(8) . . ? B7 Ru2 Ru3 72.4(4) . . ? Ru1 Ru2 Ru3 57.89(4) . . ? H100 Ru3 C15 72(4) . . ? H100 Ru3 C16 162(4) . . ? C15 Ru3 C16 90.0(6) . . ? H100 Ru3 C14 86(4) . . ? C15 Ru3 C14 103.2(6) . . ? C16 Ru3 C14 95.9(5) . . ? H100 Ru3 B11 96(4) . . ? C15 Ru3 B11 91.9(6) . . ? C16 Ru3 B11 87.0(6) . . ? C14 Ru3 B11 164.6(5) . . ? H100 Ru3 Ru1 94(4) . . ? C15 Ru3 Ru1 141.0(4) . . ? C16 Ru3 Ru1 101.0(4) . . ? C14 Ru3 Ru1 112.5(4) . . ? B11 Ru3 Ru1 52.1(4) . . ? H100 Ru3 Ru2 38(4) . . ? C15 Ru3 Ru2 105.7(4) . . ? C16 Ru3 Ru2 158.0(4) . . ? C14 Ru3 Ru2 95.4(4) . . ? B11 Ru3 Ru2 77.3(4) . . ? Ru1 Ru3 Ru2 57.09(4) . . ? B4 C1 B5 61.9(8) . . ? B4 C1 B6 114.5(10) . . ? B5 C1 B6 63.4(9) . . ? B4 C1 B3 63.4(8) . . ? B5 C1 B3 115.4(9) . . ? B6 C1 B3 115.5(9) . . ? B4 C1 S1 113.4(9) . . ? B5 C1 S1 119.1(8) . . ? B6 C1 S1 123.2(8) . . ? B3 C1 S1 112.1(9) . . ? B4 C1 Ru1 124.3(8) . . ? B5 C1 Ru1 125.3(9) . . ? B6 C1 Ru1 67.5(6) . . ? B3 C1 Ru1 66.8(6) . . ? S1 C1 Ru1 107.1(5) . . ? B8 B3 C1 100.4(10) . . ? B8 B3 B7 59.3(8) . . ? C1 B3 B7 102.2(10) . . ? B8 B3 B4 57.6(7) . . ? C1 B3 B4 55.4(7) . . ? B7 B3 B4 103.9(10) . . ? B8 B3 Ru1 118.1(9) . . ? C1 B3 Ru1 66.2(6) . . ? B7 B3 Ru1 65.2(7) . . ? B4 B3 Ru1 116.7(9) . . ? C1 B4 B5 59.1(8) . . ? C1 B4 B9 106.6(12) . . ? B5 B4 B9 61.1(9) . . ? C1 B4 B8 106.9(10) . . ? B5 B4 B8 110.1(11) . . ? B9 B4 B8 60.8(8) . . ? C1 B4 B3 61.2(7) . . ? B5 B4 B3 111.3(11) . . ? B9 B4 B3 110.2(10) . . ? B8 B4 B3 60.1(8) . . ? C1 B5 B4 59.0(8) . . ? C1 B5 B10 107.0(9) . . ? B4 B5 B10 109.0(10) . . ? C1 B5 B9 105.6(10) . . ? B4 B5 B9 59.8(9) . . ? B10 B5 B9 60.6(9) . . ? C1 B5 B6 59.4(8) . . ? B4 B5 B6 108.9(10) . . ? B10 B5 B6 61.2(8) . . ? B9 B5 B6 109.3(10) . . ? C1 B6 B5 57.2(8) . . ? C1 B6 B10 102.8(10) . . ? B5 B6 B10 58.1(8) . . ? C1 B6 B11 104.4(10) . . ? B5 B6 B11 104.9(9) . . ? B10 B6 B11 59.0(7) . . ? C1 B6 Ru1 67.2(6) . . ? B5 B6 Ru1 119.5(10) . . ? B10 B6 Ru1 119.8(9) . . ? B11 B6 Ru1 66.5(6) . . ? H7 B7 B8 112(5) . . ? H7 B7 B3 129(5) . . ? B8 B7 B3 60.3(8) . . ? H7 B7 B12 106(5) . . ? B8 B7 B12 60.4(8) . . ? B3 B7 B12 109.6(9) . . ? H7 B7 B11 119(5) . . ? B8 B7 B11 106.7(10) . . ? B3 B7 B11 110.4(9) . . ? B12 B7 B11 57.8(8) . . ? H7 B7 Ru1 121(5) . . ? B8 B7 Ru1 120.9(8) . . ? B3 B7 Ru1 67.4(6) . . ? B12 B7 Ru1 119.7(9) . . ? B11 B7 Ru1 67.4(6) . . ? H7 B7 Ru2 47(4) . . ? B8 B7 Ru2 149.8(10) . . ? B3 B7 Ru2 112.2(8) . . ? B12 B7 Ru2 138.1(9) . . ? B11 B7 Ru2 103.2(8) . . ? Ru1 B7 Ru2 74.7(4) . . ? B4 B8 B9 59.5(8) . . ? B4 B8 B7 108.2(10) . . ? B9 B8 B7 108.1(12) . . ? B4 B8 B3 62.2(7) . . ? B9 B8 B3 110.9(10) . . ? B7 B8 B3 60.3(7) . . ? B4 B8 B12 106.3(11) . . ? B9 B8 B12 58.7(9) . . ? B7 B8 B12 60.7(9) . . ? B3 B8 B12 109.8(11) . . ? B4 B9 B12 108.8(10) . . ? B4 B9 B5 59.2(9) . . ? B12 B9 B5 108.3(11) . . ? B4 B9 B8 59.7(8) . . ? B12 B9 B8 61.6(8) . . ? B5 B9 B8 107.6(10) . . ? B4 B9 B10 107.4(10) . . ? B12 B9 B10 61.4(9) . . ? B5 B9 B10 59.2(9) . . ? B8 B9 B10 110.2(10) . . ? B5 B10 B9 60.2(9) . . ? B5 B10 B11 108.5(10) . . ? B9 B10 B11 106.2(11) . . ? B5 B10 B12 107.0(12) . . ? B9 B10 B12 58.7(8) . . ? B11 B10 B12 58.4(8) . . ? B5 B10 B6 60.6(8) . . ? B9 B10 B6 108.6(11) . . ? B11 B10 B6 61.2(8) . . ? B12 B10 B6 107.7(10) . . ? B12 B11 B10 61.0(8) . . ? B12 B11 B7 60.8(8) . . ? B10 B11 B7 108.7(10) . . ? B12 B11 B6 108.7(10) . . ? B10 B11 B6 59.8(7) . . ? B7 B11 B6 106.9(10) . . ? B12 B11 Ru3 139.8(9) . . ? B10 B11 Ru3 144.2(11) . . ? B7 B11 Ru3 107.0(8) . . ? B6 B11 Ru3 111.6(8) . . ? B12 B11 Ru1 120.1(10) . . ? B10 B11 Ru1 119.7(9) . . ? B7 B11 Ru1 64.7(6) . . ? B6 B11 Ru1 65.7(6) . . ? Ru3 B11 Ru1 78.6(5) . . ? B9 B12 B11 108.9(10) . . ? B9 B12 B10 59.9(9) . . ? B11 B12 B10 60.6(8) . . ? B9 B12 B8 59.6(9) . . ? B11 B12 B8 108.5(10) . . ? B10 B12 B8 107.5(10) . . ? B9 B12 B7 107.4(11) . . ? B11 B12 B7 61.4(8) . . ? B10 B12 B7 108.8(9) . . ? B8 B12 B7 59.0(8) . . ? O11 C11 Ru1 170.8(10) . . ? O12 C12 Ru1 170.8(11) . . ? O13 C13 Ru2 174.1(11) . . ? O14 C14 Ru3 179.7(13) . . ? O15 C15 Ru3 177.9(13) . . ? O16 C16 Ru3 176.6(12) . . ? C21 S1 C1 106.2(6) . . ? C21 S1 C22 100.7(6) . . ? C1 S1 C22 109.0(6) . . ? C31 P1 C41 105.5(6) . . ? C31 P1 C101 104.8(5) . . ? C41 P1 C101 99.0(5) . . ? C31 P1 Ru2 116.3(4) . . ? C41 P1 Ru2 119.8(5) . . ? C101 P1 Ru2 109.0(4) . . ? C36 C31 C32 117.5(11) . . ? C36 C31 P1 120.5(9) . . ? C32 C31 P1 121.5(9) . . ? C33 C32 C31 122.1(11) . . ? C32 C33 C34 119.2(11) . . ? C35 C34 C33 119.6(12) . . ? C34 C35 C36 120.5(11) . . ? C31 C36 C35 120.9(11) . . ? C42 C41 C46 118.8(11) . . ? C42 C41 P1 122.3(9) . . ? C46 C41 P1 118.5(11) . . ? C41 C42 C43 121.4(13) . . ? C42 C43 C44 117.5(15) . . ? C45 C44 C43 120.9(12) . . ? C44 C45 C46 121.2(13) . . ? C45 C46 C41 120.1(13) . . ? C51 P2 C61 101.4(6) . . ? C51 P2 C102 105.5(5) . . ? C61 P2 C102 105.3(6) . . ? C51 P2 Ru2 116.0(4) . . ? C61 P2 Ru2 117.3(4) . . ? C102 P2 Ru2 110.0(3) . . ? C52 C51 C56 117.1(11) . . ? C52 C51 P2 120.9(10) . . ? C56 C51 P2 121.9(10) . . ? C53 C52 C51 121.1(12) . . ? C52 C53 C54 120.3(13) . . ? C55 C54 C53 121.1(12) . . ? C54 C55 C56 118.0(12) . . ? C55 C56 C51 122.0(13) . . ? C62 C61 C66 119.3(11) . . ? C62 C61 P2 122.1(10) . . ? C66 C61 P2 118.3(9) . . ? C61 C62 C63 122.2(14) . . ? C64 C63 C62 116.7(15) . . ? C63 C64 C65 122.5(14) . . ? C64 C65 C66 118.7(15) . . ? C61 C66 C65 120.3(14) . . ? C102 C101 B104 110.8(9) . . ? C102 C101 B106 61.5(7) . . ? B104 C101 B106 113.6(9) . . ? C102 C101 B105 111.3(8) . . ? B104 C101 B105 62.0(8) . . ? B106 C101 B105 62.7(8) . . ? C102 C101 B103 60.3(7) . . ? B104 C101 B103 62.2(8) . . ? B106 C101 B103 112.5(9) . . ? B105 C101 B103 112.7(9) . . ? C102 C101 P1 112.6(8) . . ? B104 C101 P1 125.4(8) . . ? B106 C101 P1 115.5(8) . . ? B105 C101 P1 125.7(8) . . ? B103 C101 P1 116.1(7) . . ? C101 C102 B107 109.3(9) . . ? C101 C102 B103 60.6(7) . . ? B107 C102 B103 63.1(7) . . ? C101 C102 B106 59.9(7) . . ? B107 C102 B106 110.0(9) . . ? B103 C102 B106 111.4(10) . . ? C101 C102 B111 108.9(9) . . ? B107 C102 B111 58.7(7) . . ? B103 C102 B111 111.2(9) . . ? B106 C102 B111 62.4(7) . . ? C101 C102 P2 113.6(7) . . ? B107 C102 P2 127.9(8) . . ? B103 C102 P2 116.2(7) . . ? B106 C102 P2 116.4(8) . . ? B111 C102 P2 127.2(8) . . ? C102 B103 C101 59.0(7) . . ? C102 B103 B108 105.8(9) . . ? C101 B103 B108 105.1(10) . . ? C102 B103 B104 106.6(9) . . ? C101 B103 B104 58.4(8) . . ? B108 B103 B104 60.5(8) . . ? C102 B103 B107 58.4(7) . . ? C101 B103 B107 104.4(9) . . ? B108 B103 B107 59.2(8) . . ? B104 B103 B107 107.1(10) . . ? C101 B104 B105 59.4(8) . . ? C101 B104 B103 59.5(8) . . ? B105 B104 B103 108.4(11) . . ? C101 B104 B109 105.5(10) . . ? B105 B104 B109 59.1(8) . . ? B103 B104 B109 108.2(11) . . ? C101 B104 B108 105.3(11) . . ? B105 B104 B108 107.1(10) . . ? B103 B104 B108 59.7(8) . . ? B109 B104 B108 60.1(8) . . ? C101 B105 B110 106.1(11) . . ? C101 B105 B109 106.0(10) . . ? B110 B105 B109 61.2(9) . . ? C101 B105 B104 58.5(8) . . ? B110 B105 B104 109.5(10) . . ? B109 B105 B104 60.7(8) . . ? C101 B105 B106 58.6(8) . . ? B110 B105 B106 60.2(8) . . ? B109 B105 B106 108.7(11) . . ? B104 B105 B106 107.5(10) . . ? C101 B106 C102 58.7(7) . . ? C101 B106 B110 104.7(11) . . ? C102 B106 B110 106.8(9) . . ? C101 B106 B105 58.7(8) . . ? C102 B106 B105 106.0(10) . . ? B110 B106 B105 58.2(8) . . ? C101 B106 B111 105.4(9) . . ? C102 B106 B111 59.1(7) . . ? B110 B106 B111 61.0(8) . . ? B105 B106 B111 106.9(10) . . ? B111 B107 C102 61.8(7) . . ? B111 B107 B112 60.6(8) . . ? C102 B107 B112 107.6(9) . . ? B111 B107 B108 109.9(11) . . ? C102 B107 B108 106.2(10) . . ? B112 B107 B108 60.3(9) . . ? B111 B107 B103 109.9(10) . . ? C102 B107 B103 58.5(7) . . ? B112 B107 B103 107.8(11) . . ? B108 B107 B103 59.5(8) . . ? B107 B108 B103 61.3(8) . . ? B107 B108 B112 59.8(9) . . ? B103 B108 B112 108.8(11) . . ? B107 B108 B109 107.4(11) . . ? B103 B108 B109 108.1(10) . . ? B112 B108 B109 59.2(8) . . ? B107 B108 B104 108.3(10) . . ? B103 B108 B104 59.9(8) . . ? B112 B108 B104 107.2(10) . . ? B109 B108 B104 59.7(8) . . ? B105 B109 B112 107.6(12) . . ? B105 B109 B110 58.9(8) . . ? B112 B109 B110 60.2(9) . . ? B105 B109 B104 60.2(8) . . ? B112 B109 B104 108.2(11) . . ? B110 B109 B104 107.3(11) . . ? B105 B109 B108 108.0(10) . . ? B112 B109 B108 60.1(9) . . ? B110 B109 B108 107.8(11) . . ? B104 B109 B108 60.2(8) . . ? B105 B110 B106 61.6(8) . . ? B105 B110 B112 107.8(11) . . ? B106 B110 B112 107.6(10) . . ? B105 B110 B109 59.9(9) . . ? B106 B110 B109 108.8(10) . . ? B112 B110 B109 59.5(9) . . ? B105 B110 B111 109.4(10) . . ? B106 B110 B111 60.8(8) . . ? B112 B110 B111 58.4(8) . . ? B109 B110 B111 106.7(10) . . ? B107 B111 B112 61.3(8) . . ? B107 B111 C102 59.5(7) . . ? B112 B111 C102 106.5(10) . . ? B107 B111 B106 107.6(9) . . ? B112 B111 B106 106.4(11) . . ? C102 B111 B106 58.6(7) . . ? B107 B111 B110 108.1(11) . . ? B112 B111 B110 59.5(8) . . ? C102 B111 B110 104.2(9) . . ? B106 B111 B110 58.2(7) . . ? B111 B112 B109 110.4(10) . . ? B111 B112 B107 58.1(8) . . ? B109 B112 B107 108.7(10) . . ? B111 B112 B110 62.2(8) . . ? B109 B112 B110 60.3(9) . . ? B107 B112 B110 107.7(10) . . ? B111 B112 B108 107.5(10) . . ? B109 B112 B108 60.7(9) . . ? B107 B112 B108 59.9(8) . . ? B110 B112 B108 108.4(10) . . ? Cl2 C100 Cl1 108.0(14) . . ? _diffrn_measured_fraction_theta_max 0.834 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.923 _refine_diff_density_max 3.419 _refine_diff_density_min -1.697 _refine_diff_density_rms 0.268 #============================================================================== data_9 _database_code_depnum_ccdc_archive 'CCDC 268997' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C17 H34 B10 O6 Ru3 S3' _chemical_formula_weight 841.93 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' 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' 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 'P2(1)/c ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 16.336(3) _cell_length_b 13.428(2) _cell_length_c 16.324(3) _cell_angle_alpha 90.00 _cell_angle_beta 118.522(6) _cell_angle_gamma 90.00 _cell_volume 3146.2(9) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 7507 _cell_measurement_theta_min 2.84 _cell_measurement_theta_max 29.38 _exptl_crystal_description block _exptl_crystal_colour 'dark orange' _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.777 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1656 _exptl_absorpt_coefficient_mu 1.652 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.808 _exptl_absorpt_correction_T_max 0.902 _exptl_absorpt_process_details 'SADABS (Bruker, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(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 'Bruker-Nonius X8 Apex CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 41854 _diffrn_reflns_av_R_equivalents 0.0391 _diffrn_reflns_av_sigmaI/netI 0.0338 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.08 _diffrn_reflns_theta_max 29.42 _reflns_number_total 8656 _reflns_number_gt 7260 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2 (Bruker, 2003)' _computing_cell_refinement 'Bruker APEX2 (Bruker, 2003)' _computing_data_reduction 'Bruker APEX2 (Bruker, 2003)' _computing_structure_solution 'Bruker SHELXTL (Bruker, 2000)' _computing_structure_refinement 'Bruker SHELXTL (Bruker, 2000)' _computing_molecular_graphics 'Bruker SHELXTL (Bruker, 2000)' _computing_publication_material 'Bruker SHELXTL (Bruker, 2000)' _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^)+(0.0276P)^2^+0.5920P] 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 8656 _refine_ls_number_parameters 378 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0314 _refine_ls_R_factor_gt 0.0232 _refine_ls_wR_factor_ref 0.0580 _refine_ls_wR_factor_gt 0.0559 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.050 _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 0.255947(11) 0.925930(11) 0.453910(10) 0.01273(4) Uani 1 1 d . . . Ru2 Ru 0.324410(11) 0.752820(11) 0.577673(11) 0.01444(4) Uani 1 1 d . . . Ru3 Ru 0.136510(11) 0.801688(11) 0.487382(11) 0.01470(4) Uani 1 1 d . . . H23 H 0.2312(16) 0.7840(18) 0.5985(17) 0.031(7) Uiso 1 1 d . . . C1 C 0.23972(14) 1.09465(14) 0.43058(13) 0.0151(4) Uani 1 1 d . . . B3 B 0.33951(17) 1.06214(16) 0.53256(15) 0.0165(4) Uani 1 1 d . . . H3 H 0.4106 1.0563 0.5387 0.020 Uiso 1 1 calc R . . B4 B 0.28430(18) 1.18183(17) 0.51794(16) 0.0193(5) Uani 1 1 d . . . H4 H 0.3198 1.2520 0.5148 0.023 Uiso 1 1 calc R . . B5 B 0.16161(17) 1.16578(17) 0.44822(16) 0.0196(5) Uani 1 1 d . . . H5 H 0.1165 1.2254 0.3997 0.023 Uiso 1 1 calc R . . B6 B 0.13913(16) 1.03562(16) 0.41764(16) 0.0164(4) Uani 1 1 d . . . H6 H 0.0792 1.0135 0.3490 0.020 Uiso 1 1 calc R . . B7 B 0.30200(16) 0.98544(16) 0.59997(15) 0.0152(4) Uani 1 1 d . . . B8 B 0.32139(17) 1.11526(16) 0.62313(16) 0.0177(5) Uani 1 1 d . . . H8 H 0.3814 1.1423 0.6896 0.021 Uiso 1 1 calc R . . B9 B 0.21121(18) 1.17737(17) 0.57090(16) 0.0208(5) Uani 1 1 d . . . H9 H 0.1983 1.2446 0.6037 0.025 Uiso 1 1 calc R . . B10 B 0.12224(18) 1.08691(17) 0.50970(17) 0.0202(5) Uani 1 1 d . . . H10 H 0.0504 1.0946 0.5015 0.024 Uiso 1 1 calc R . . B11 B 0.17543(16) 0.96796(16) 0.52658(16) 0.0165(4) Uani 1 1 d . . . H11 H 0.1245(15) 0.9092(16) 0.5378(15) 0.020 Uiso 1 1 d . . . B12 B 0.22052(17) 1.05638(17) 0.61977(16) 0.0180(5) Uani 1 1 d . . . H12 H 0.2135 1.0443 0.6840 0.022 Uiso 1 1 calc R . . C21 C 0.18626(15) 0.87001(15) 0.33145(14) 0.0209(4) Uani 1 1 d . . . O21 O 0.14554(12) 0.84281(13) 0.25649(11) 0.0334(4) Uani 1 1 d . . . C22 C 0.36758(15) 0.88367(15) 0.45337(14) 0.0186(4) Uani 1 1 d . . . O22 O 0.43444(11) 0.86950(12) 0.44866(11) 0.0268(3) Uani 1 1 d . . . C23 C 0.43433(16) 0.71806(15) 0.57200(14) 0.0208(4) Uani 1 1 d . . . O23 O 0.50245(11) 0.69591(12) 0.57353(12) 0.0309(4) Uani 1 1 d . . . C24 C 0.35627(16) 0.65477(16) 0.66930(15) 0.0224(4) Uani 1 1 d . . . O24 O 0.37880(13) 0.59473(12) 0.72610(12) 0.0356(4) Uani 1 1 d . . . C25 C 0.06172(15) 0.73248(15) 0.52808(15) 0.0200(4) Uani 1 1 d . . . O25 O 0.01372(11) 0.69450(12) 0.55184(12) 0.0294(4) Uani 1 1 d . . . C26 C 0.02864(15) 0.82453(16) 0.37094(15) 0.0233(5) Uani 1 1 d . . . O26 O -0.03743(12) 0.83583(14) 0.30130(12) 0.0393(4) Uani 1 1 d . . . S1 S 0.23899(4) 1.12623(4) 0.32287(3) 0.02356(12) Uani 1 1 d . . . C11 C 0.25044(17) 1.25966(16) 0.31868(16) 0.0268(5) Uani 1 1 d . . . H11A H 0.1932 1.2919 0.3106 0.040 Uiso 1 1 calc R . . H11B H 0.2610 1.2770 0.2662 0.040 Uiso 1 1 calc R . . H11C H 0.3033 1.2825 0.3770 0.040 Uiso 1 1 calc R . . C12 C 0.35151(19) 1.09339(18) 0.33672(18) 0.0339(6) Uani 1 1 d . . . H12A H 0.3541 1.1094 0.2794 0.051 Uiso 1 1 calc R . . H12B H 0.3621 1.0219 0.3494 0.051 Uiso 1 1 calc R . . H12C H 0.3998 1.1309 0.3889 0.051 Uiso 1 1 calc R . . S3 S 0.20555(4) 0.67159(4) 0.44539(3) 0.01807(10) Uani 1 1 d . A . C31 C 0.17474(18) 0.54079(16) 0.45972(17) 0.0285(5) Uani 1 1 d . . . C32A C 0.0990(12) 0.5081(10) 0.3667(10) 0.036(3) Uani 0.37(3) 1 d P A 1 H32A H 0.1144 0.5283 0.3180 0.054 Uiso 0.37(3) 1 calc PR A 1 H32B H 0.0400 0.5390 0.3550 0.054 Uiso 0.37(3) 1 calc PR A 1 H32C H 0.0928 0.4354 0.3662 0.054 Uiso 0.37(3) 1 calc PR A 1 C33A C 0.2680(10) 0.4840(11) 0.4794(10) 0.027(2) Uani 0.37(3) 1 d P A 1 H33A H 0.3186 0.5045 0.5402 0.041 Uiso 0.37(3) 1 calc PR A 1 H33B H 0.2844 0.5006 0.4306 0.041 Uiso 0.37(3) 1 calc PR A 1 H33C H 0.2584 0.4120 0.4796 0.041 Uiso 0.37(3) 1 calc PR A 1 C32B C 0.0725(9) 0.5300(8) 0.3791(7) 0.052(3) Uani 0.63(3) 1 d P A 2 H32D H 0.0706 0.5445 0.3193 0.078 Uiso 0.63(3) 1 calc PR A 2 H32E H 0.0322 0.5769 0.3890 0.078 Uiso 0.63(3) 1 calc PR A 2 H32F H 0.0507 0.4619 0.3783 0.078 Uiso 0.63(3) 1 calc PR A 2 C33B C 0.2385(13) 0.4742(7) 0.4430(13) 0.057(3) Uani 0.63(3) 1 d P A 2 H33D H 0.2390 0.4945 0.3855 0.086 Uiso 0.63(3) 1 calc PR A 2 H33E H 0.2167 0.4052 0.4368 0.086 Uiso 0.63(3) 1 calc PR A 2 H33F H 0.3017 0.4792 0.4956 0.086 Uiso 0.63(3) 1 calc PR A 2 C34 C 0.1674(2) 0.51840(18) 0.54637(19) 0.0397(7) Uani 1 1 d . A . H34A H 0.1509 0.4482 0.5461 0.060 Uiso 1 1 calc R . . H34B H 0.1191 0.5606 0.5478 0.060 Uiso 1 1 calc R . . H34C H 0.2273 0.5319 0.6015 0.060 Uiso 1 1 calc R . . S7 S 0.39516(3) 0.89437(4) 0.67734(3) 0.01514(10) Uani 1 1 d . . . C71 C 0.40848(15) 0.88322(15) 0.79724(13) 0.0192(4) Uani 1 1 d . . . C72 C 0.32228(15) 0.84024(16) 0.79745(14) 0.0224(4) Uani 1 1 d . . . H72A H 0.3098 0.7736 0.7696 0.034 Uiso 1 1 calc R . . H72B H 0.2687 0.8836 0.7611 0.034 Uiso 1 1 calc R . . H72C H 0.3329 0.8359 0.8617 0.034 Uiso 1 1 calc R . . C73 C 0.42945(17) 0.98726(16) 0.84015(14) 0.0262(5) Uani 1 1 d . . . H73A H 0.4848 1.0139 0.8391 0.039 Uiso 1 1 calc R . . H73B H 0.4409 0.9836 0.9047 0.039 Uiso 1 1 calc R . . H73C H 0.3762 1.0310 0.8041 0.039 Uiso 1 1 calc R . . C74 C 0.49442(15) 0.81695(17) 0.84952(15) 0.0248(5) Uani 1 1 d . . . H74A H 0.4809 0.7499 0.8225 0.037 Uiso 1 1 calc R . . H74B H 0.5104 0.8133 0.9154 0.037 Uiso 1 1 calc R . . H74C H 0.5469 0.8452 0.8441 0.037 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.01414(8) 0.01180(8) 0.01338(7) -0.00034(6) 0.00747(6) -0.00063(6) Ru2 0.01623(9) 0.01184(8) 0.01651(8) 0.00086(6) 0.00883(7) 0.00032(6) Ru3 0.01439(9) 0.01266(8) 0.01773(8) -0.00059(6) 0.00822(7) -0.00167(6) C1 0.0178(10) 0.0135(9) 0.0143(9) 0.0029(7) 0.0079(8) 0.0013(8) B3 0.0205(12) 0.0137(10) 0.0161(10) 0.0004(8) 0.0093(9) -0.0026(9) B4 0.0273(13) 0.0119(10) 0.0187(11) 0.0001(9) 0.0110(10) -0.0020(10) B5 0.0232(13) 0.0153(11) 0.0209(11) 0.0019(9) 0.0111(10) 0.0027(10) B6 0.0165(12) 0.0135(10) 0.0179(10) 0.0015(8) 0.0070(9) 0.0008(9) B7 0.0184(11) 0.0132(10) 0.0143(10) 0.0006(8) 0.0082(9) -0.0009(9) B8 0.0241(13) 0.0140(10) 0.0156(10) -0.0012(9) 0.0100(10) -0.0020(10) B9 0.0295(14) 0.0145(11) 0.0208(11) 0.0002(9) 0.0139(11) 0.0021(10) B10 0.0220(13) 0.0179(11) 0.0243(12) 0.0015(9) 0.0140(11) 0.0032(10) B11 0.0173(12) 0.0141(10) 0.0210(11) 0.0009(9) 0.0113(10) 0.0004(9) B12 0.0238(13) 0.0145(10) 0.0200(11) -0.0023(9) 0.0138(10) -0.0007(10) C21 0.0245(12) 0.0191(10) 0.0206(10) -0.0008(8) 0.0121(9) 0.0006(9) O21 0.0397(10) 0.0347(9) 0.0201(8) -0.0075(7) 0.0097(8) -0.0041(8) C22 0.0237(11) 0.0155(9) 0.0181(9) 0.0022(8) 0.0114(9) 0.0008(9) O22 0.0256(9) 0.0269(8) 0.0358(9) 0.0063(7) 0.0211(8) 0.0057(7) C23 0.0263(12) 0.0172(10) 0.0215(10) 0.0055(8) 0.0135(9) 0.0040(9) O23 0.0275(9) 0.0322(9) 0.0394(10) 0.0112(8) 0.0212(8) 0.0109(8) C24 0.0255(12) 0.0178(10) 0.0243(11) 0.0003(9) 0.0122(10) -0.0005(9) O24 0.0480(12) 0.0237(8) 0.0324(9) 0.0090(7) 0.0170(9) -0.0002(8) C25 0.0183(11) 0.0166(10) 0.0239(10) 0.0012(8) 0.0091(9) 0.0009(9) O25 0.0246(9) 0.0279(9) 0.0400(9) 0.0071(7) 0.0189(8) -0.0015(7) C26 0.0188(11) 0.0230(11) 0.0278(11) -0.0007(9) 0.0110(10) -0.0040(9) O26 0.0241(9) 0.0500(11) 0.0298(9) 0.0031(9) 0.0015(8) -0.0038(9) S1 0.0323(3) 0.0226(3) 0.0160(2) 0.0013(2) 0.0117(2) -0.0056(2) C11 0.0335(14) 0.0211(11) 0.0285(12) 0.0115(9) 0.0171(11) 0.0062(10) C12 0.0548(17) 0.0255(12) 0.0436(14) 0.0092(11) 0.0413(14) 0.0104(12) S3 0.0221(3) 0.0130(2) 0.0207(2) -0.00301(19) 0.0114(2) -0.0023(2) C31 0.0398(15) 0.0130(10) 0.0362(13) -0.0048(9) 0.0210(12) -0.0065(10) C32A 0.045(7) 0.021(4) 0.033(5) -0.013(3) 0.010(4) -0.009(4) C33A 0.035(6) 0.007(4) 0.040(6) -0.004(4) 0.019(5) 0.005(4) C32B 0.067(6) 0.029(4) 0.041(4) -0.008(3) 0.011(3) -0.032(4) C33B 0.093(9) 0.017(3) 0.097(9) -0.007(4) 0.074(8) -0.002(4) C34 0.0619(19) 0.0207(12) 0.0483(16) -0.0030(11) 0.0359(15) -0.0129(13) S7 0.0162(2) 0.0144(2) 0.0150(2) 0.00143(18) 0.0077(2) -0.0009(2) C71 0.0253(11) 0.0178(10) 0.0147(9) 0.0019(8) 0.0097(9) -0.0019(9) C72 0.0277(12) 0.0223(10) 0.0216(10) 0.0040(9) 0.0153(10) 0.0013(9) C73 0.0349(13) 0.0235(11) 0.0165(10) -0.0024(9) 0.0093(10) -0.0052(10) C74 0.0229(12) 0.0287(12) 0.0185(10) 0.0049(9) 0.0064(9) 0.0003(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 C22 1.914(2) . ? Ru1 C21 1.919(2) . ? Ru1 B11 2.224(2) . ? Ru1 B6 2.255(2) . ? Ru1 B7 2.275(2) . ? Ru1 B3 2.277(2) . ? Ru1 C1 2.2916(19) . ? Ru1 Ru3 2.8119(4) . ? Ru1 Ru2 2.9288(4) . ? Ru2 H23 1.76(2) . ? Ru2 C24 1.870(2) . ? Ru2 C23 1.900(2) . ? Ru2 S3 2.3704(6) . ? Ru2 S7 2.4083(6) . ? Ru2 Ru3 2.7757(5) . ? Ru2 B7 3.186(2) . ? Ru3 H11 1.72(2) . ? Ru3 H23 1.75(2) . ? Ru3 C25 1.890(2) . ? Ru3 C26 1.901(2) . ? Ru3 B11 2.326(2) . ? Ru3 S3 2.3520(6) . ? C1 B4 1.715(3) . ? C1 B5 1.725(3) . ? C1 B3 1.740(3) . ? C1 B6 1.744(3) . ? C1 S1 1.8031(19) . ? B3 B8 1.789(3) . ? B3 B4 1.802(3) . ? B3 B7 1.814(3) . ? B4 B8 1.767(3) . ? B4 B9 1.778(3) . ? B4 B5 1.783(4) . ? B5 B9 1.772(3) . ? B5 B10 1.777(3) . ? B5 B6 1.807(3) . ? B6 B10 1.790(3) . ? B6 B11 1.825(3) . ? B7 B8 1.780(3) . ? B7 B12 1.787(3) . ? B7 B11 1.844(3) . ? B7 S7 1.890(2) . ? B8 B9 1.788(4) . ? B8 B12 1.805(3) . ? B9 B12 1.784(3) . ? B9 B10 1.789(4) . ? B10 B11 1.776(3) . ? B10 B12 1.794(4) . ? B11 H11 1.22(2) . ? B11 B12 1.788(3) . ? C21 O21 1.138(3) . ? C22 O22 1.147(2) . ? C23 O23 1.140(3) . ? C24 O24 1.149(3) . ? C25 O25 1.147(2) . ? C26 O26 1.144(3) . ? S1 C12 1.797(3) . ? S1 C11 1.806(2) . ? S3 C31 1.872(2) . ? C31 C33B 1.494(10) . ? C31 C32A 1.495(14) . ? C31 C34 1.506(3) . ? C31 C32B 1.563(10) . ? C31 C33A 1.594(14) . ? S7 C71 1.8691(19) . ? C71 C72 1.523(3) . ? C71 C73 1.527(3) . ? C71 C74 1.532(3) . ? 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 C22 Ru1 C21 88.39(9) . . ? C22 Ru1 B11 152.28(9) . . ? C21 Ru1 B11 116.56(9) . . ? C22 Ru1 B6 151.81(8) . . ? C21 Ru1 B6 88.59(9) . . ? B11 Ru1 B6 48.10(8) . . ? C22 Ru1 B7 105.66(8) . . ? C21 Ru1 B7 164.56(9) . . ? B11 Ru1 B7 48.37(9) . . ? B6 Ru1 B7 81.98(8) . . ? C22 Ru1 B3 85.68(9) . . ? C21 Ru1 B3 143.08(8) . . ? B11 Ru1 B3 80.99(8) . . ? B6 Ru1 B3 80.07(9) . . ? B7 Ru1 B3 46.98(8) . . ? C22 Ru1 C1 109.10(8) . . ? C21 Ru1 C1 104.46(8) . . ? B11 Ru1 C1 77.69(7) . . ? B6 Ru1 C1 45.11(8) . . ? B7 Ru1 C1 77.35(7) . . ? B3 Ru1 C1 44.77(8) . . ? C22 Ru1 Ru3 125.18(6) . . ? C21 Ru1 Ru3 81.30(6) . . ? B11 Ru1 Ru3 53.48(6) . . ? B6 Ru1 Ru3 81.94(6) . . ? B7 Ru1 Ru3 85.28(6) . . ? B3 Ru1 Ru3 130.69(5) . . ? C1 Ru1 Ru3 125.66(5) . . ? C22 Ru1 Ru2 73.56(6) . . ? C21 Ru1 Ru2 104.43(6) . . ? B11 Ru1 Ru2 87.81(6) . . ? B6 Ru1 Ru2 134.12(6) . . ? B7 Ru1 Ru2 74.31(6) . . ? B3 Ru1 Ru2 108.66(6) . . ? C1 Ru1 Ru2 151.05(5) . . ? Ru3 Ru1 Ru2 57.787(11) . . ? H23 Ru2 C24 87.1(8) . . ? H23 Ru2 C23 172.7(8) . . ? C24 Ru2 C23 87.56(9) . . ? H23 Ru2 S3 83.0(8) . . ? C24 Ru2 S3 101.46(7) . . ? C23 Ru2 S3 102.99(7) . . ? H23 Ru2 S7 82.1(8) . . ? C24 Ru2 S7 98.90(7) . . ? C23 Ru2 S7 93.84(7) . . ? S3 Ru2 S7 153.992(19) . . ? H23 Ru2 Ru3 37.6(8) . . ? C24 Ru2 Ru3 113.95(7) . . ? C23 Ru2 Ru3 149.71(6) . . ? S3 Ru2 Ru3 53.695(15) . . ? S7 Ru2 Ru3 102.969(16) . . ? H23 Ru2 Ru1 82.2(8) . . ? C24 Ru2 Ru1 168.28(7) . . ? C23 Ru2 Ru1 102.70(6) . . ? S3 Ru2 Ru1 81.949(17) . . ? S7 Ru2 Ru1 75.026(18) . . ? Ru3 Ru2 Ru1 58.994(6) . . ? H23 Ru2 B7 65.7(8) . . ? C24 Ru2 B7 127.02(7) . . ? C23 Ru2 B7 114.16(8) . . ? S3 Ru2 B7 117.80(4) . . ? S7 Ru2 B7 36.22(4) . . ? Ru3 Ru2 B7 70.77(4) . . ? Ru1 Ru2 B7 43.43(4) . . ? H11 Ru3 H23 82.2(11) . . ? H11 Ru3 C25 90.2(7) . . ? H23 Ru3 C25 88.2(8) . . ? H11 Ru3 C26 94.6(7) . . ? H23 Ru3 C26 175.8(8) . . ? C25 Ru3 C26 89.11(9) . . ? H11 Ru3 B11 30.8(7) . . ? H23 Ru3 B11 81.7(8) . . ? C25 Ru3 B11 120.86(8) . . ? C26 Ru3 B11 96.97(9) . . ? H11 Ru3 S3 160.7(7) . . ? H23 Ru3 S3 83.8(8) . . ? C25 Ru3 S3 102.57(6) . . ? C26 Ru3 S3 99.96(7) . . ? B11 Ru3 S3 133.39(6) . . ? H11 Ru3 Ru2 107.1(7) . . ? H23 Ru3 Ru2 37.9(8) . . ? C25 Ru3 Ru2 115.70(7) . . ? C26 Ru3 Ru2 146.22(6) . . ? B11 Ru3 Ru2 89.61(6) . . ? S3 Ru3 Ru2 54.308(15) . . ? H11 Ru3 Ru1 81.0(7) . . ? H23 Ru3 Ru1 86.0(8) . . ? C25 Ru3 Ru1 170.04(6) . . ? C26 Ru3 Ru1 96.20(6) . . ? B11 Ru3 Ru1 50.21(5) . . ? S3 Ru3 Ru1 84.852(18) . . ? Ru2 Ru3 Ru1 63.219(13) . . ? B4 C1 B5 62.45(13) . . ? B4 C1 B3 62.87(13) . . ? B5 C1 B3 114.14(15) . . ? B4 C1 B6 114.34(15) . . ? B5 C1 B6 62.77(13) . . ? B3 C1 B6 113.58(14) . . ? B4 C1 S1 116.91(13) . . ? B5 C1 S1 111.81(13) . . ? B3 C1 S1 123.98(14) . . ? B6 C1 S1 114.94(13) . . ? B4 C1 Ru1 124.54(12) . . ? B5 C1 Ru1 123.77(12) . . ? B3 C1 Ru1 67.16(10) . . ? B6 C1 Ru1 66.32(10) . . ? S1 C1 Ru1 109.94(9) . . ? C1 B3 B8 103.98(16) . . ? C1 B3 B4 57.90(12) . . ? B8 B3 B4 58.94(12) . . ? C1 B3 B7 106.81(16) . . ? B8 B3 B7 59.20(12) . . ? B4 B3 B7 107.09(16) . . ? C1 B3 Ru1 68.07(10) . . ? B8 B3 Ru1 119.68(13) . . ? B4 B3 Ru1 120.96(15) . . ? B7 B3 Ru1 66.47(10) . . ? C1 B4 B8 105.97(15) . . ? C1 B4 B9 105.31(16) . . ? B8 B4 B9 60.58(13) . . ? C1 B4 B5 59.03(13) . . ? B8 B4 B5 108.57(16) . . ? B9 B4 B5 59.69(14) . . ? C1 B4 B3 59.23(12) . . ? B8 B4 B3 60.16(13) . . ? B9 B4 B3 108.38(16) . . ? B5 B4 B3 108.40(16) . . ? C1 B5 B9 105.18(16) . . ? C1 B5 B10 105.09(16) . . ? B9 B5 B10 60.52(14) . . ? C1 B5 B4 58.52(13) . . ? B9 B5 B4 60.01(13) . . ? B10 B5 B4 108.13(17) . . ? C1 B5 B6 59.14(12) . . ? B9 B5 B6 108.67(16) . . ? B10 B5 B6 59.92(13) . . ? B4 B5 B6 108.15(16) . . ? C1 B6 B10 103.74(15) . . ? C1 B6 B5 58.09(12) . . ? B10 B6 B5 59.23(12) . . ? C1 B6 B11 105.02(15) . . ? B10 B6 B11 58.83(12) . . ? B5 B6 B11 106.49(15) . . ? C1 B6 Ru1 68.57(10) . . ? B10 B6 Ru1 118.77(14) . . ? B5 B6 Ru1 121.64(14) . . ? B11 B6 Ru1 65.07(10) . . ? B8 B7 B12 60.79(13) . . ? B8 B7 B3 59.69(12) . . ? B12 B7 B3 107.67(15) . . ? B8 B7 B11 107.06(16) . . ? B12 B7 B11 58.97(12) . . ? B3 B7 B11 106.08(15) . . ? B8 B7 S7 119.14(15) . . ? B12 B7 S7 130.97(14) . . ? B3 B7 S7 112.04(14) . . ? B11 B7 S7 130.33(14) . . ? B8 B7 Ru1 120.19(12) . . ? B12 B7 Ru1 118.33(14) . . ? B3 B7 Ru1 66.56(10) . . ? B11 B7 Ru1 64.36(9) . . ? S7 B7 Ru1 103.35(10) . . ? B8 B7 Ru2 165.02(14) . . ? B12 B7 Ru2 132.79(13) . . ? B3 B7 Ru2 113.38(11) . . ? B11 B7 Ru2 87.44(10) . . ? S7 B7 Ru2 48.86(5) . . ? Ru1 B7 Ru2 62.25(5) . . ? B4 B8 B7 110.21(15) . . ? B4 B8 B9 60.03(13) . . ? B7 B8 B9 108.60(17) . . ? B4 B8 B3 60.91(12) . . ? B7 B8 B3 61.11(12) . . ? B9 B8 B3 108.55(16) . . ? B4 B8 B12 107.92(17) . . ? B7 B8 B12 59.81(12) . . ? B9 B8 B12 59.55(13) . . ? B3 B8 B12 108.01(16) . . ? B5 B9 B4 60.30(13) . . ? B5 B9 B12 108.70(16) . . ? B4 B9 B12 108.32(16) . . ? B5 B9 B8 108.11(16) . . ? B4 B9 B8 59.39(13) . . ? B12 B9 B8 60.70(13) . . ? B5 B9 B10 59.88(13) . . ? B4 B9 B10 107.85(16) . . ? B12 B9 B10 60.29(14) . . ? B8 B9 B10 108.31(16) . . ? B11 B10 B5 109.96(16) . . ? B11 B10 B9 108.50(17) . . ? B5 B10 B9 59.60(13) . . ? B11 B10 B6 61.58(12) . . ? B5 B10 B6 60.85(13) . . ? B9 B10 B6 108.68(16) . . ? B11 B10 B12 60.10(13) . . ? B5 B10 B12 108.03(17) . . ? B9 B10 B12 59.73(13) . . ? B6 B10 B12 109.26(16) . . ? H11 B11 B10 106.6(10) . . ? H11 B11 B12 109.5(10) . . ? B10 B11 B12 60.46(13) . . ? H11 B11 B6 122.7(10) . . ? B10 B11 B6 59.59(12) . . ? B12 B11 B6 107.97(15) . . ? H11 B11 B7 128.1(10) . . ? B10 B11 B7 107.46(16) . . ? B12 B11 B7 58.94(12) . . ? B6 B11 B7 108.15(15) . . ? H11 B11 Ru1 122.3(10) . . ? B10 B11 Ru1 121.05(13) . . ? B12 B11 Ru1 120.94(14) . . ? B6 B11 Ru1 66.83(10) . . ? B7 B11 Ru1 67.27(10) . . ? H11 B11 Ru3 46.0(10) . . ? B10 B11 Ru3 140.48(15) . . ? B12 B11 Ru3 144.98(14) . . ? B6 B11 Ru3 106.91(13) . . ? B7 B11 Ru3 112.05(12) . . ? Ru1 B11 Ru3 76.31(7) . . ? B9 B12 B7 108.44(15) . . ? B9 B12 B11 108.17(16) . . ? B7 B12 B11 62.09(13) . . ? B9 B12 B10 59.98(14) . . ? B7 B12 B10 109.16(15) . . ? B11 B12 B10 59.44(13) . . ? B9 B12 B8 59.76(13) . . ? B7 B12 B8 59.40(12) . . ? B11 B12 B8 108.42(15) . . ? B10 B12 B8 107.33(16) . . ? O21 C21 Ru1 175.41(19) . . ? O22 C22 Ru1 171.71(17) . . ? O23 C23 Ru2 176.33(18) . . ? O24 C24 Ru2 177.8(2) . . ? O25 C25 Ru3 176.71(18) . . ? O26 C26 Ru3 178.0(2) . . ? C12 S1 C1 106.83(10) . . ? C12 S1 C11 97.47(11) . . ? C1 S1 C11 108.52(10) . . ? C31 S3 Ru3 117.74(8) . . ? C31 S3 Ru2 118.04(8) . . ? Ru3 S3 Ru2 71.997(19) . . ? C33B C31 C32A 87.1(5) . . ? C33B C31 C34 115.3(6) . . ? C32A C31 C34 119.8(7) . . ? C33B C31 C32B 110.4(4) . . ? C32A C31 C32B 23.7(4) . . ? C34 C31 C32B 103.9(5) . . ? C33B C31 C33A 21.1(6) . . ? C32A C31 C33A 108.2(6) . . ? C34 C31 C33A 102.3(6) . . ? C32B C31 C33A 131.3(5) . . ? C33B C31 S3 106.6(4) . . ? C32A C31 S3 106.9(5) . . ? C34 C31 S3 116.83(16) . . ? C32B C31 S3 103.0(3) . . ? C33A C31 S3 100.7(6) . . ? C71 S7 B7 113.93(9) . . ? C71 S7 Ru2 115.00(7) . . ? B7 S7 Ru2 94.91(7) . . ? C72 C71 C73 110.54(18) . . ? C72 C71 C74 112.39(17) . . ? C73 C71 C74 109.32(18) . . ? C72 C71 S7 112.77(14) . . ? C73 C71 S7 107.19(13) . . ? C74 C71 S7 104.32(14) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.544 _refine_diff_density_min -0.513 _refine_diff_density_rms 0.094 #============================================================================== data_10 _database_code_depnum_ccdc_archive 'CCDC 268998' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22.25 H36.50 B10 Cl0.50 O7 Ru3 S' _chemical_formula_weight 877.11 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C2/c ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 42.274(6) _cell_length_b 10.7571(17) _cell_length_c 17.195(3) _cell_angle_alpha 90.00 _cell_angle_beta 113.840(7) _cell_angle_gamma 90.00 _cell_volume 7152.1(19) _cell_formula_units_Z 8 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 6012 _cell_measurement_theta_min 2.37 _cell_measurement_theta_max 26.16 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.629 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3460 _exptl_absorpt_coefficient_mu 1.383 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.807 _exptl_absorpt_correction_T_max 0.916 _exptl_absorpt_process_details 'SADABS (Bruker, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(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 'Bruker-Nonius X8 Apex CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 69779 _diffrn_reflns_av_R_equivalents 0.0674 _diffrn_reflns_av_sigmaI/netI 0.0689 _diffrn_reflns_limit_h_min -60 _diffrn_reflns_limit_h_max 61 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.23 _diffrn_reflns_theta_max 32.48 _reflns_number_total 11335 _reflns_number_gt 7600 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2 (Bruker, 2003)' _computing_cell_refinement 'Bruker APEX2 (Bruker, 2003)' _computing_data_reduction 'Bruker APEX2 (Bruker, 2003)' _computing_structure_solution 'Bruker SHELXTL (Bruker, 2000)' _computing_structure_refinement 'Bruker SHELXTL (Bruker, 2000)' _computing_molecular_graphics 'Bruker SHELXTL (Bruker, 2000)' _computing_publication_material 'Bruker SHELXTL (Bruker, 2000)' _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^)+(0.0425P)^2^+4.0305P] 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 11335 _refine_ls_number_parameters 424 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0814 _refine_ls_R_factor_gt 0.0399 _refine_ls_wR_factor_ref 0.0928 _refine_ls_wR_factor_gt 0.0819 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.023 _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 0.150697(6) 0.88014(2) 0.388960(14) 0.01710(6) Uani 1 1 d . . . Ru2 Ru 0.078002(6) 0.92792(3) 0.287473(16) 0.02278(7) Uani 1 1 d . . . Ru3 Ru 0.110238(6) 0.77842(3) 0.221981(16) 0.02219(7) Uani 1 1 d . . . C1 C 0.19978(7) 0.9937(3) 0.45194(17) 0.0183(6) Uani 1 1 d . . . B3 B 0.16355(8) 1.0825(3) 0.3859(2) 0.0198(7) Uani 1 1 d . . . H3 H 0.1463 1.1384 0.4076 0.024 Uiso 1 1 calc R . . B4 B 0.20772(8) 1.1308(3) 0.4132(2) 0.0196(7) Uani 1 1 d . . . H4 H 0.2183 1.2157 0.4530 0.023 Uiso 1 1 calc R . . B5 B 0.23428(8) 0.9977(3) 0.4235(2) 0.0205(7) Uani 1 1 d . . . H5 H 0.2621 0.9955 0.4693 0.025 Uiso 1 1 calc R . . B6 B 0.20685(8) 0.8630(3) 0.4037(2) 0.0188(7) Uani 1 1 d . . . H6 H 0.2175 0.7734 0.4373 0.023 Uiso 1 1 calc R . . B7 B 0.14850(8) 1.0064(3) 0.2826(2) 0.0168(7) Uani 1 1 d . . . B8 B 0.17652(8) 1.1400(3) 0.3056(2) 0.0199(7) Uani 1 1 d . . . H8 H 0.1667 1.2314 0.2738 0.024 Uiso 1 1 calc R . . B9 B 0.21964(8) 1.0880(4) 0.3287(2) 0.0202(7) Uani 1 1 d . . . H9 H 0.2379 1.1454 0.3112 0.024 Uiso 1 1 calc R . . B10 B 0.21963(8) 0.9218(4) 0.3240(2) 0.0202(7) Uani 1 1 d . . . H10 H 0.2382 0.8696 0.3045 0.024 Uiso 1 1 calc R . . B11 B 0.17620(8) 0.8676(3) 0.2929(2) 0.0191(7) Uani 1 1 d . . . B12 B 0.18378(8) 1.0098(3) 0.2502(2) 0.0182(7) Uani 1 1 d . . . H12 H 0.1785 1.0158 0.1811 0.022 Uiso 1 1 calc R . . C11 C 0.15429(9) 0.7108(4) 0.4232(2) 0.0304(8) Uani 1 1 d . . . O11 O 0.15991(8) 0.6091(3) 0.44642(19) 0.0503(8) Uani 1 1 d . . . C12 C 0.12950(8) 0.9234(3) 0.4643(2) 0.0259(7) Uani 1 1 d . . . O12 O 0.12071(6) 0.9520(3) 0.51719(15) 0.0384(6) Uani 1 1 d . . . C13 C 0.06484(8) 1.0523(4) 0.3526(2) 0.0310(8) Uani 1 1 d . . . O13 O 0.05613(7) 1.1196(3) 0.39022(17) 0.0437(7) Uani 1 1 d . . . C14 C 0.03234(8) 0.9052(3) 0.2053(2) 0.0292(8) Uani 1 1 d . . . O14 O 0.00420(6) 0.8809(3) 0.16107(15) 0.0389(6) Uani 1 1 d . . . C15 C 0.07306(8) 0.7861(4) 0.3473(2) 0.0367(9) Uani 1 1 d . . . O15 O 0.06887(7) 0.7015(3) 0.38403(18) 0.0471(7) Uani 1 1 d . . . C16 C 0.07050(8) 0.7482(3) 0.1218(2) 0.0296(8) Uani 1 1 d . . . O16 O 0.04546(6) 0.7265(3) 0.06349(17) 0.0455(7) Uani 1 1 d . . . C17 C 0.10526(9) 0.6242(4) 0.2563(2) 0.0352(9) Uani 1 1 d . . . O17 O 0.10118(8) 0.5241(3) 0.27843(18) 0.0500(8) Uani 1 1 d . . . C21 C 0.10986(7) 1.0150(3) 0.21527(19) 0.0221(7) Uani 1 1 d . . . H21 H 0.1036(8) 0.971(3) 0.160(2) 0.027 Uiso 1 1 d . . . C22 C 0.08716(7) 1.1082(3) 0.2169(2) 0.0238(7) Uani 1 1 d . . . H22A H 0.1000 1.1732 0.2597 0.029 Uiso 1 1 calc R . . C23 C 0.05847(8) 1.1684(3) 0.1403(2) 0.0300(8) Uani 1 1 d . . . C24 C 0.02942(9) 1.2183(4) 0.1644(3) 0.0425(10) Uani 1 1 d . . . H24A H 0.0113 1.2560 0.1143 0.064 Uiso 1 1 calc R . . H24B H 0.0389 1.2811 0.2093 0.064 Uiso 1 1 calc R . . H24C H 0.0196 1.1497 0.1850 0.064 Uiso 1 1 calc R . . C25 C 0.04324(9) 1.0836(4) 0.0621(2) 0.0347(8) Uani 1 1 d . . . H25A H 0.0251 1.1284 0.0158 0.052 Uiso 1 1 calc R . . H25B H 0.0334 1.0093 0.0767 0.052 Uiso 1 1 calc R . . H25C H 0.0615 1.0590 0.0440 0.052 Uiso 1 1 calc R . . C26 C 0.07640(9) 1.2787(4) 0.1174(2) 0.0391(9) Uani 1 1 d . . . H26A H 0.0596 1.3225 0.0680 0.059 Uiso 1 1 calc R . . H26B H 0.0954 1.2477 0.1038 0.059 Uiso 1 1 calc R . . H26C H 0.0856 1.3358 0.1658 0.059 Uiso 1 1 calc R . . C31 C 0.16527(7) 0.7470(3) 0.2361(2) 0.0204(6) Uani 1 1 d . . . H31 H 0.1722(8) 0.663(3) 0.262(2) 0.024 Uiso 1 1 d . . . C32 C 0.14628(8) 0.7440(3) 0.1490(2) 0.0241(7) Uani 1 1 d . . . H32 H 0.1398(8) 0.819(3) 0.117(2) 0.029 Uiso 1 1 d . . . C33 C 0.14495(9) 0.6332(3) 0.0917(2) 0.0296(8) Uani 1 1 d . . . C34 C 0.14492(16) 0.5075(4) 0.1318(3) 0.0756(18) Uani 1 1 d . . . H34A H 0.1647 0.5023 0.1869 0.113 Uiso 1 1 calc R . . H34B H 0.1466 0.4415 0.0944 0.113 Uiso 1 1 calc R . . H34C H 0.1234 0.4975 0.1399 0.113 Uiso 1 1 calc R . . C35 C 0.11405(10) 0.6452(5) 0.0056(3) 0.0600(14) Uani 1 1 d . . . H35A H 0.1135 0.5733 -0.0300 0.090 Uiso 1 1 calc R . . H35B H 0.1163 0.7215 -0.0227 0.090 Uiso 1 1 calc R . . H35C H 0.0926 0.6483 0.0146 0.090 Uiso 1 1 calc R . . C36 C 0.17788(9) 0.6463(3) 0.0755(2) 0.0328(8) Uani 1 1 d . . . H36A H 0.1982 0.6385 0.1294 0.049 Uiso 1 1 calc R . . H36B H 0.1781 0.7279 0.0503 0.049 Uiso 1 1 calc R . . H36C H 0.1784 0.5809 0.0363 0.049 Uiso 1 1 calc R . . S S 0.208420(18) 1.00277(8) 0.56364(4) 0.02054(16) Uani 1 1 d . . . C41 C 0.25018(9) 1.0731(4) 0.6200(2) 0.0412(10) Uani 1 1 d . . . H41A H 0.2551 1.0778 0.6807 0.062 Uiso 1 1 calc R . . H41B H 0.2502 1.1571 0.5979 0.062 Uiso 1 1 calc R . . H41C H 0.2680 1.0228 0.6120 0.062 Uiso 1 1 calc R . . C42 C 0.21857(9) 0.8477(3) 0.6045(2) 0.0317(8) Uani 1 1 d . . . H42A H 0.1980 0.7953 0.5794 0.048 Uiso 1 1 calc R . . H42B H 0.2263 0.8491 0.6664 0.048 Uiso 1 1 calc R . . H42C H 0.2370 0.8140 0.5900 0.048 Uiso 1 1 calc R . . C100 C -0.0225(4) 1.4729(16) 0.1722(10) 0.046(4) Uani 0.25 1 d PD . . H10A H -0.0152 1.3849 0.1825 0.055 Uiso 0.25 1 calc PR . . H10B H -0.0481 1.4735 0.1426 0.055 Uiso 0.25 1 calc PR . . Cl1 Cl -0.0064(4) 1.5330(11) 0.1051(10) 0.196(5) Uani 0.25 1 d PD . . Cl2 Cl -0.0114(4) 1.5444(14) 0.2717(12) 0.253(9) Uani 0.25 1 d PD . . 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 0.01560(11) 0.02568(14) 0.01383(11) 0.00150(10) 0.00989(9) -0.00031(9) Ru2 0.01430(11) 0.03672(17) 0.01978(13) -0.00288(11) 0.00945(10) -0.00266(10) Ru3 0.02061(12) 0.03007(16) 0.02054(13) -0.00580(11) 0.01313(10) -0.00758(10) C1 0.0164(13) 0.0297(18) 0.0095(13) 0.0008(12) 0.0061(11) 0.0014(12) B3 0.0179(15) 0.0258(19) 0.0179(16) 0.0010(14) 0.0095(13) -0.0010(14) B4 0.0178(15) 0.029(2) 0.0128(15) 0.0002(14) 0.0073(13) -0.0036(14) B5 0.0151(15) 0.030(2) 0.0180(17) -0.0003(15) 0.0084(13) -0.0021(14) B6 0.0165(15) 0.027(2) 0.0157(16) -0.0001(14) 0.0089(13) -0.0002(13) B7 0.0181(15) 0.0222(19) 0.0139(15) 0.0010(13) 0.0105(13) 0.0009(13) B8 0.0183(16) 0.028(2) 0.0144(16) 0.0006(14) 0.0079(13) -0.0015(14) B9 0.0144(15) 0.034(2) 0.0117(15) -0.0022(14) 0.0053(12) -0.0036(14) B10 0.0159(15) 0.031(2) 0.0154(16) 0.0019(14) 0.0080(13) -0.0007(14) B11 0.0186(15) 0.026(2) 0.0141(15) 0.0003(14) 0.0080(13) 0.0000(14) B12 0.0153(15) 0.027(2) 0.0153(16) -0.0008(14) 0.0087(13) -0.0035(13) C11 0.0303(17) 0.042(2) 0.0231(17) 0.0050(16) 0.0155(14) -0.0037(16) O11 0.0608(19) 0.0370(17) 0.0532(19) 0.0180(14) 0.0229(15) -0.0018(14) C12 0.0171(14) 0.043(2) 0.0216(16) -0.0032(15) 0.0114(13) -0.0033(14) O12 0.0244(12) 0.073(2) 0.0247(13) -0.0065(12) 0.0170(10) -0.0003(12) C13 0.0192(15) 0.049(2) 0.0256(18) -0.0009(16) 0.0093(14) 0.0011(15) O13 0.0349(14) 0.065(2) 0.0365(15) -0.0123(14) 0.0196(12) 0.0087(13) C14 0.0246(17) 0.045(2) 0.0232(17) -0.0044(15) 0.0155(14) -0.0036(15) O14 0.0196(12) 0.0671(19) 0.0307(13) -0.0070(13) 0.0109(11) -0.0119(11) C15 0.0202(16) 0.061(3) 0.0311(19) -0.0094(19) 0.0121(15) -0.0039(16) O15 0.0441(16) 0.059(2) 0.0468(17) 0.0120(14) 0.0278(14) -0.0086(14) C16 0.0282(17) 0.039(2) 0.0277(18) -0.0098(15) 0.0175(15) -0.0077(15) O16 0.0286(13) 0.069(2) 0.0360(15) -0.0193(14) 0.0105(12) -0.0079(13) C17 0.0370(19) 0.048(3) 0.0284(19) -0.0091(17) 0.0209(16) -0.0035(17) O17 0.075(2) 0.0388(17) 0.0503(18) -0.0015(14) 0.0397(16) -0.0182(15) C21 0.0165(14) 0.0346(19) 0.0172(15) -0.0019(14) 0.0087(12) -0.0031(13) C22 0.0179(14) 0.0319(19) 0.0230(16) -0.0016(14) 0.0098(13) -0.0047(13) C23 0.0199(15) 0.038(2) 0.0291(18) 0.0030(16) 0.0070(13) 0.0005(14) C24 0.0267(18) 0.055(3) 0.041(2) 0.003(2) 0.0093(16) 0.0093(17) C25 0.0257(17) 0.047(2) 0.0256(18) 0.0023(17) 0.0045(14) -0.0038(16) C26 0.0318(19) 0.040(2) 0.040(2) 0.0056(18) 0.0088(17) 0.0000(17) C31 0.0191(14) 0.0242(18) 0.0226(16) -0.0001(13) 0.0134(12) 0.0000(12) C32 0.0209(15) 0.0301(19) 0.0254(17) -0.0053(14) 0.0136(13) -0.0053(13) C33 0.0337(18) 0.032(2) 0.0303(18) -0.0139(15) 0.0207(15) -0.0123(15) C34 0.156(6) 0.032(3) 0.079(4) -0.025(2) 0.089(4) -0.036(3) C35 0.033(2) 0.094(4) 0.048(3) -0.045(3) 0.0117(19) -0.007(2) C36 0.0339(18) 0.032(2) 0.041(2) -0.0134(16) 0.0248(17) -0.0049(15) S 0.0207(3) 0.0319(5) 0.0116(3) 0.0014(3) 0.0092(3) 0.0023(3) C41 0.036(2) 0.069(3) 0.0138(16) -0.0081(17) 0.0055(14) -0.0195(19) C42 0.042(2) 0.039(2) 0.0181(16) 0.0072(15) 0.0161(15) 0.0136(16) C100 0.043(9) 0.041(10) 0.050(10) -0.004(8) 0.015(8) -0.005(8) Cl1 0.203(13) 0.160(10) 0.286(16) 0.036(11) 0.160(13) 0.026(9) Cl2 0.138(14) 0.266(16) 0.31(2) 0.041(17) 0.038(13) 0.029(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 C11 1.902(4) . ? Ru1 C12 1.906(3) . ? Ru1 B7 2.249(3) . ? Ru1 B3 2.250(4) . ? Ru1 C1 2.270(3) . ? Ru1 B6 2.291(3) . ? Ru1 B11 2.313(3) . ? Ru1 Ru3 2.8977(5) . ? Ru1 Ru2 2.9014(5) . ? Ru2 C14 1.892(3) . ? Ru2 C15 1.898(4) . ? Ru2 C13 1.964(4) . ? Ru2 C21 2.363(3) . ? Ru2 C22 2.401(3) . ? Ru2 Ru3 2.6366(4) . ? Ru3 C17 1.801(4) . ? Ru3 C16 1.886(3) . ? Ru3 C31 2.265(3) . ? Ru3 H21 2.29(3) . ? Ru3 C32 2.362(3) . ? Ru3 C21 2.548(3) . ? C1 B4 1.707(5) . ? C1 B5 1.716(4) . ? C1 B6 1.719(5) . ? C1 B3 1.773(4) . ? C1 S 1.807(3) . ? B3 B8 1.789(5) . ? B3 B4 1.808(5) . ? B3 B7 1.821(5) . ? B4 B9 1.779(5) . ? B4 B5 1.783(5) . ? B4 B8 1.788(5) . ? B5 B10 1.766(5) . ? B5 B9 1.780(5) . ? B5 B6 1.800(5) . ? B6 B10 1.779(5) . ? B6 B11 1.820(5) . ? B7 C21 1.578(4) . ? B7 B12 1.791(4) . ? B7 B8 1.802(5) . ? B7 B11 1.861(5) . ? B8 B12 1.789(5) . ? B8 B9 1.791(5) . ? B9 B12 1.782(5) . ? B9 B10 1.790(5) . ? B10 B11 1.789(5) . ? B10 B12 1.802(5) . ? B11 C31 1.577(5) . ? B11 B12 1.780(5) . ? C11 O11 1.156(4) . ? C12 O12 1.155(4) . ? C13 O13 1.128(4) . ? C14 O14 1.153(4) . ? C15 O15 1.161(5) . ? C16 O16 1.150(4) . ? C17 O17 1.178(4) . ? C21 H21 0.99(3) . ? C21 C22 1.396(4) . ? C22 C23 1.528(4) . ? C23 C25 1.534(5) . ? C23 C26 1.542(5) . ? C23 C24 1.543(5) . ? C31 C32 1.385(4) . ? C32 C33 1.533(4) . ? C33 C34 1.518(5) . ? C33 C35 1.533(5) . ? C33 C36 1.533(4) . ? S C42 1.793(3) . ? S C41 1.802(3) . ? C100 Cl1 1.690(14) . ? C100 Cl2 1.757(16) . ? Cl1 Cl2 1.95(2) 2 ? Cl2 Cl2 1.44(3) 2 ? Cl2 C100 1.57(2) 2 ? Cl2 Cl1 1.95(2) 2 ? 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 C11 Ru1 C12 91.41(15) . . ? C11 Ru1 B7 143.29(13) . . ? C12 Ru1 B7 121.91(13) . . ? C11 Ru1 B3 160.84(14) . . ? C12 Ru1 B3 87.94(14) . . ? B7 Ru1 B3 47.75(12) . . ? C11 Ru1 C1 115.12(13) . . ? C12 Ru1 C1 97.73(12) . . ? B7 Ru1 C1 78.03(11) . . ? B3 Ru1 C1 46.19(11) . . ? C11 Ru1 B6 86.50(13) . . ? C12 Ru1 B6 134.05(12) . . ? B7 Ru1 B6 80.72(12) . . ? B3 Ru1 B6 80.28(13) . . ? C1 Ru1 B6 44.28(11) . . ? C11 Ru1 B11 99.38(13) . . ? C12 Ru1 B11 169.16(14) . . ? B7 Ru1 B11 48.12(12) . . ? B3 Ru1 B11 81.53(12) . . ? C1 Ru1 B11 76.82(11) . . ? B6 Ru1 B11 46.59(12) . . ? C11 Ru1 Ru3 83.45(10) . . ? C12 Ru1 Ru3 120.93(9) . . ? B7 Ru1 Ru3 66.95(9) . . ? B3 Ru1 Ru3 113.17(9) . . ? C1 Ru1 Ru3 137.35(7) . . ? B6 Ru1 Ru3 104.43(8) . . ? B11 Ru1 Ru3 61.91(8) . . ? C11 Ru1 Ru2 106.77(10) . . ? C12 Ru1 Ru2 72.00(9) . . ? B7 Ru1 Ru2 73.64(8) . . ? B3 Ru1 Ru2 91.24(9) . . ? C1 Ru1 Ru2 137.17(8) . . ? B6 Ru1 Ru2 151.53(8) . . ? B11 Ru1 Ru2 105.48(8) . . ? Ru3 Ru1 Ru2 54.086(10) . . ? C14 Ru2 C15 89.92(15) . . ? C14 Ru2 C13 94.32(14) . . ? C15 Ru2 C13 96.91(15) . . ? C14 Ru2 C21 106.54(12) . . ? C15 Ru2 C21 144.52(13) . . ? C13 Ru2 C21 112.47(13) . . ? C14 Ru2 C22 92.92(13) . . ? C15 Ru2 C22 177.15(13) . . ? C13 Ru2 C22 83.01(13) . . ? C21 Ru2 C22 34.06(11) . . ? C14 Ru2 Ru3 98.60(10) . . ? C15 Ru2 Ru3 86.00(11) . . ? C13 Ru2 Ru3 166.77(9) . . ? C21 Ru2 Ru3 60.98(8) . . ? C22 Ru2 Ru3 93.45(8) . . ? C14 Ru2 Ru1 159.95(11) . . ? C15 Ru2 Ru1 81.57(10) . . ? C13 Ru2 Ru1 104.67(9) . . ? C21 Ru2 Ru1 72.32(7) . . ? C22 Ru2 Ru1 95.69(7) . . ? Ru3 Ru2 Ru1 62.885(13) . . ? C17 Ru3 C16 87.79(16) . . ? C17 Ru3 C31 94.48(14) . . ? C16 Ru3 C31 124.69(12) . . ? C17 Ru3 H21 167.2(8) . . ? C16 Ru3 H21 80.6(8) . . ? C31 Ru3 H21 96.5(8) . . ? C17 Ru3 C32 102.44(14) . . ? C16 Ru3 C32 90.86(12) . . ? C31 Ru3 C32 34.75(11) . . ? H21 Ru3 C32 83.1(8) . . ? C17 Ru3 C21 159.32(12) . . ? C16 Ru3 C21 98.28(13) . . ? C31 Ru3 C21 98.14(10) . . ? H21 Ru3 C21 22.9(8) . . ? C32 Ru3 C21 97.24(11) . . ? C17 Ru3 Ru2 105.84(11) . . ? C16 Ru3 Ru2 94.14(10) . . ? C31 Ru3 Ru2 136.99(8) . . ? H21 Ru3 Ru2 70.0(8) . . ? C32 Ru3 Ru2 151.43(9) . . ? C21 Ru3 Ru2 54.21(6) . . ? C17 Ru3 Ru1 97.11(11) . . ? C16 Ru3 Ru1 157.14(10) . . ? C31 Ru3 Ru1 77.34(8) . . ? H21 Ru3 Ru1 91.7(8) . . ? C32 Ru3 Ru1 109.67(8) . . ? C21 Ru3 Ru1 70.00(7) . . ? Ru2 Ru3 Ru1 63.029(13) . . ? B4 C1 B5 62.79(19) . . ? B4 C1 B6 114.7(2) . . ? B5 C1 B6 63.22(19) . . ? B4 C1 B3 62.55(18) . . ? B5 C1 B3 114.7(2) . . ? B6 C1 B3 113.9(2) . . ? B4 C1 S 112.4(2) . . ? B5 C1 S 118.14(19) . . ? B6 C1 S 123.9(2) . . ? B3 C1 S 113.76(19) . . ? B4 C1 Ru1 124.38(18) . . ? B5 C1 Ru1 126.58(19) . . ? B6 C1 Ru1 68.51(15) . . ? B3 C1 Ru1 66.31(15) . . ? S C1 Ru1 106.82(13) . . ? C1 B3 B8 103.1(2) . . ? C1 B3 B4 56.95(18) . . ? B8 B3 B4 59.64(18) . . ? C1 B3 B7 104.7(2) . . ? B8 B3 B7 59.89(18) . . ? B4 B3 B7 107.4(2) . . ? C1 B3 Ru1 67.50(15) . . ? B8 B3 Ru1 120.3(2) . . ? B4 B3 Ru1 120.4(2) . . ? B7 B3 Ru1 66.11(16) . . ? C1 B4 B9 105.1(3) . . ? C1 B4 B5 58.83(18) . . ? B9 B4 B5 59.95(19) . . ? C1 B4 B8 105.8(2) . . ? B9 B4 B8 60.28(18) . . ? B5 B4 B8 108.6(2) . . ? C1 B4 B3 60.50(18) . . ? B9 B4 B3 108.5(2) . . ? B5 B4 B3 109.7(2) . . ? B8 B4 B3 59.65(18) . . ? C1 B5 B10 105.0(2) . . ? C1 B5 B9 104.7(2) . . ? B10 B5 B9 60.6(2) . . ? C1 B5 B4 58.37(18) . . ? B10 B5 B4 108.3(2) . . ? B9 B5 B4 59.89(19) . . ? C1 B5 B6 58.48(18) . . ? B10 B5 B6 59.83(19) . . ? B9 B5 B6 107.9(2) . . ? B4 B5 B6 107.2(2) . . ? C1 B6 B10 104.3(2) . . ? C1 B6 B5 58.31(18) . . ? B10 B6 B5 59.13(19) . . ? C1 B6 B11 107.1(2) . . ? B10 B6 B11 59.61(18) . . ? B5 B6 B11 107.9(2) . . ? C1 B6 Ru1 67.21(14) . . ? B10 B6 Ru1 120.6(2) . . ? B5 B6 Ru1 121.0(2) . . ? B11 B6 Ru1 67.34(14) . . ? C21 B7 B12 121.1(2) . . ? C21 B7 B8 120.5(3) . . ? B12 B7 B8 59.72(18) . . ? C21 B7 B3 122.6(2) . . ? B12 B7 B3 106.7(2) . . ? B8 B7 B3 59.16(18) . . ? C21 B7 B11 122.8(3) . . ? B12 B7 B11 58.32(18) . . ? B8 B7 B11 106.6(2) . . ? B3 B7 B11 108.0(2) . . ? C21 B7 Ru1 108.8(2) . . ? B12 B7 Ru1 119.9(2) . . ? B8 B7 Ru1 119.72(19) . . ? B3 B7 Ru1 66.14(15) . . ? B11 B7 Ru1 67.72(15) . . ? B4 B8 B3 60.72(18) . . ? B4 B8 B12 107.1(2) . . ? B3 B8 B12 108.2(3) . . ? B4 B8 B9 59.59(18) . . ? B3 B8 B9 108.8(2) . . ? B12 B8 B9 59.69(18) . . ? B4 B8 B7 109.1(2) . . ? B3 B8 B7 60.95(19) . . ? B12 B8 B7 59.83(18) . . ? B9 B8 B7 108.6(3) . . ? B4 B9 B5 60.16(19) . . ? B4 B9 B12 107.8(2) . . ? B5 B9 B12 108.1(2) . . ? B4 B9 B10 107.5(2) . . ? B5 B9 B10 59.3(2) . . ? B12 B9 B10 60.61(19) . . ? B4 B9 B8 60.13(18) . . ? B5 B9 B8 108.7(2) . . ? B12 B9 B8 60.09(19) . . ? B10 B9 B8 108.7(2) . . ? B5 B10 B6 61.04(19) . . ? B5 B10 B11 110.9(2) . . ? B6 B10 B11 61.35(18) . . ? B5 B10 B9 60.1(2) . . ? B6 B10 B9 108.4(2) . . ? B11 B10 B9 108.7(2) . . ? B5 B10 B12 107.8(2) . . ? B6 B10 B12 107.4(2) . . ? B11 B10 B12 59.43(19) . . ? B9 B10 B12 59.47(19) . . ? C31 B11 B12 120.5(2) . . ? C31 B11 B10 117.5(2) . . ? B12 B11 B10 60.64(19) . . ? C31 B11 B6 122.1(3) . . ? B12 B11 B6 106.5(2) . . ? B10 B11 B6 59.04(18) . . ? C31 B11 B7 125.9(2) . . ? B12 B11 B7 58.87(18) . . ? B10 B11 B7 107.3(2) . . ? B6 B11 B7 106.0(2) . . ? C31 B11 Ru1 112.7(2) . . ? B12 B11 Ru1 117.2(2) . . ? B10 B11 Ru1 119.0(2) . . ? B6 B11 Ru1 66.08(14) . . ? B7 B11 Ru1 64.16(14) . . ? B11 B12 B9 109.5(2) . . ? B11 B12 B8 110.8(2) . . ? B9 B12 B8 60.22(19) . . ? B11 B12 B7 62.81(19) . . ? B9 B12 B7 109.5(2) . . ? B8 B12 B7 60.45(18) . . ? B11 B12 B10 59.93(19) . . ? B9 B12 B10 59.9(2) . . ? B8 B12 B10 108.2(2) . . ? B7 B12 B10 109.8(2) . . ? O11 C11 Ru1 173.3(3) . . ? O12 C12 Ru1 171.6(3) . . ? O13 C13 Ru2 176.6(3) . . ? O14 C14 Ru2 172.3(3) . . ? O15 C15 Ru2 177.2(3) . . ? O16 C16 Ru3 176.1(3) . . ? O17 C17 Ru3 178.3(3) . . ? H21 C21 C22 116.3(19) . . ? H21 C21 B7 117.9(19) . . ? C22 C21 B7 122.9(3) . . ? H21 C21 Ru2 108.6(19) . . ? C22 C21 Ru2 74.44(17) . . ? B7 C21 Ru2 103.41(19) . . ? H21 C21 Ru3 63.7(19) . . ? C22 C21 Ru3 135.1(2) . . ? B7 C21 Ru3 85.53(19) . . ? Ru2 C21 Ru3 64.82(8) . . ? C21 C22 C23 126.8(3) . . ? C21 C22 Ru2 71.50(19) . . ? C23 C22 Ru2 123.0(2) . . ? C22 C23 C25 114.2(3) . . ? C22 C23 C26 104.2(3) . . ? C25 C23 C26 108.0(3) . . ? C22 C23 C24 110.8(3) . . ? C25 C23 C24 110.2(3) . . ? C26 C23 C24 109.1(3) . . ? C32 C31 B11 125.8(3) . . ? C32 C31 Ru3 76.47(18) . . ? B11 C31 Ru3 88.53(18) . . ? C31 C32 C33 124.6(3) . . ? C31 C32 Ru3 68.78(16) . . ? C33 C32 Ru3 126.8(2) . . ? C34 C33 C35 110.9(3) . . ? C34 C33 C36 109.4(3) . . ? C35 C33 C36 107.4(3) . . ? C34 C33 C32 114.0(3) . . ? C35 C33 C32 110.5(3) . . ? C36 C33 C32 104.2(3) . . ? C42 S C41 98.78(19) . . ? C42 S C1 106.23(15) . . ? C41 S C1 109.12(15) . . ? Cl1 C100 Cl2 118.4(12) . . ? C100 Cl1 Cl2 50.6(7) . 2 ? Cl2 Cl2 C100 71.3(10) 2 2 ? Cl2 Cl2 C100 57.8(12) 2 . ? C100 Cl2 C100 101.6(14) 2 . ? Cl2 Cl2 Cl1 121.2(16) 2 2 ? C100 Cl2 Cl1 56.2(9) 2 2 ? C100 Cl2 Cl1 150.0(12) . 2 ? _diffrn_measured_fraction_theta_max 0.878 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.839 _refine_diff_density_min -1.192 _refine_diff_density_rms 0.136 #============================================================================== data_11 _database_code_depnum_ccdc_archive 'CCDC 268999' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C7 H18 B10 Cl2 O3 Ru S' _chemical_formula_weight 462.34 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' 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' Ru Ru -1.2594 0.8363 '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' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'Pna2(1) ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z+1/2' _cell_length_a 16.812(2) _cell_length_b 10.5893(12) _cell_length_c 10.5479(11) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1877.8(4) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 2580 _cell_measurement_theta_min 2.73 _cell_measurement_theta_max 22.13 _exptl_crystal_description irregular _exptl_crystal_colour orange _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.635 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 912 _exptl_absorpt_coefficient_mu 1.232 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.797 _exptl_absorpt_correction_T_max 0.945 _exptl_absorpt_process_details 'SADABS (Bruker, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(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 'Bruker-Nonius X8 Apex CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21376 _diffrn_reflns_av_R_equivalents 0.1058 _diffrn_reflns_av_sigmaI/netI 0.1059 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.73 _diffrn_reflns_theta_max 28.96 _reflns_number_total 4933 _reflns_number_gt 3285 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2 (Bruker, 2003)' _computing_cell_refinement 'Bruker APEX2 (Bruker, 2003)' _computing_data_reduction 'Bruker APEX2 (Bruker, 2003)' _computing_structure_solution 'Bruker SHELXTL (Bruker, 2000)' _computing_structure_refinement 'Bruker SHELXTL (Bruker, 2000)' _computing_molecular_graphics 'Bruker SHELXTL (Bruker, 2000)' _computing_publication_material 'Bruker SHELXTL (Bruker, 2000)' _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^)+(0.0625P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.09(6) _refine_ls_number_reflns 4933 _refine_ls_number_parameters 217 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1004 _refine_ls_R_factor_gt 0.0531 _refine_ls_wR_factor_ref 0.1242 _refine_ls_wR_factor_gt 0.1078 _refine_ls_goodness_of_fit_ref 0.966 _refine_ls_restrained_S_all 0.966 _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 Ru Ru 0.18680(2) 0.72107(4) 0.64618(5) 0.02024(12) Uani 1 1 d . . . C1 C 0.2058(4) 0.7299(6) 0.4332(7) 0.0210(16) Uani 1 1 d . . . B3 B 0.2499(4) 0.5969(7) 0.5039(7) 0.0219(15) Uani 1 1 d . . . H3 H 0.2224 0.5007 0.5089 0.026 Uiso 1 1 calc R . . B4 B 0.2832(4) 0.6610(8) 0.3537(8) 0.0312(17) Uani 1 1 d . . . H4 H 0.2764 0.6070 0.2630 0.037 Uiso 1 1 calc R . . B5 B 0.2721(4) 0.8306(7) 0.3605(7) 0.0258(15) Uani 1 1 d . . . H5 H 0.2580 0.8882 0.2744 0.031 Uiso 1 1 calc R . . B6 B 0.2313(4) 0.8728(7) 0.5152(7) 0.0216(15) Uani 1 1 d . . . H6 H 0.1918 0.9571 0.5273 0.026 Uiso 1 1 calc R . . B7 B 0.3159(4) 0.6551(6) 0.6255(8) 0.0236(19) Uani 1 1 d . . . H7 H 0.3339 0.5976 0.7099 0.028 Uiso 1 1 calc R . . B8 B 0.3524(4) 0.6168(8) 0.4721(7) 0.0312(18) Uani 1 1 d . . . H8 H 0.3921 0.5330 0.4585 0.037 Uiso 1 1 calc R . . B9 B 0.3653(4) 0.7586(7) 0.3839(8) 0.0284(17) Uani 1 1 d . . . H9 H 0.4140 0.7690 0.3122 0.034 Uiso 1 1 calc R . . B10 B 0.3341(4) 0.8881(7) 0.4813(7) 0.0256(16) Uani 1 1 d . . . H10 H 0.3618 0.9839 0.4733 0.031 Uiso 1 1 calc R . . B11 B 0.3050(4) 0.8285(7) 0.6318(10) 0.0229(16) Uani 1 1 d . . . H11 H 0.3164 0.8850 0.7197 0.027 Uiso 1 1 calc R . . B12 B 0.3852(5) 0.7551(7) 0.5491(8) 0.0305(18) Uani 1 1 d . . . H12 H 0.4474 0.7629 0.5862 0.037 Uiso 1 1 calc R . . C11 C 0.1149(3) 0.5753(6) 0.6594(8) 0.0266(14) Uani 1 1 d . . . O11 O 0.0773(2) 0.4874(4) 0.6603(6) 0.0365(11) Uani 1 1 d . . . C12 C 0.1032(4) 0.8411(6) 0.6835(6) 0.0238(14) Uani 1 1 d . . . O12 O 0.0568(3) 0.9139(5) 0.7092(5) 0.0377(12) Uani 1 1 d . . . C13 C 0.2112(5) 0.7147(7) 0.8236(8) 0.0283(18) Uani 1 1 d . . . O13 O 0.2291(3) 0.7143(5) 0.9261(5) 0.0384(12) Uani 1 1 d . . . S1 S 0.10875(9) 0.70960(14) 0.36130(15) 0.0257(3) Uani 1 1 d . . . C21 C 0.1228(5) 0.6820(7) 0.1940(7) 0.046(2) Uani 1 1 d . . . H21A H 0.1459 0.5981 0.1812 0.069 Uiso 1 1 calc R . . H21B H 0.1587 0.7462 0.1594 0.069 Uiso 1 1 calc R . . H21C H 0.0714 0.6869 0.1506 0.069 Uiso 1 1 calc R . . C22 C 0.0679(3) 0.8635(6) 0.3538(6) 0.0289(15) Uani 1 1 d . . . H22A H 0.0151 0.8597 0.3148 0.043 Uiso 1 1 calc R . . H22B H 0.1027 0.9177 0.3028 0.043 Uiso 1 1 calc R . . H22C H 0.0635 0.8981 0.4396 0.043 Uiso 1 1 calc R . . C100 C 0.0790(4) 0.2681(6) 0.4272(9) 0.0428(19) Uani 1 1 d . . . H10A H 0.0952 0.2291 0.3459 0.051 Uiso 1 1 calc R . . H10B H 0.1265 0.3089 0.4648 0.051 Uiso 1 1 calc R . . Cl1 Cl 0.00661(12) 0.3829(2) 0.3978(2) 0.0526(5) Uani 1 1 d . . . Cl2 Cl 0.04553(17) 0.1526(2) 0.5277(2) 0.0773(8) 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 Ru 0.02010(19) 0.0245(2) 0.01611(18) 0.0012(4) -0.0005(3) -0.00266(19) C1 0.022(3) 0.023(3) 0.018(4) 0.002(3) 0.002(3) 0.003(3) B3 0.026(4) 0.018(4) 0.021(4) 0.000(3) -0.002(3) -0.002(3) B4 0.027(4) 0.035(4) 0.031(4) 0.006(4) 0.011(3) 0.005(4) B5 0.026(4) 0.026(3) 0.026(4) 0.000(3) 0.003(3) -0.005(3) B6 0.021(4) 0.021(4) 0.023(4) -0.001(3) -0.004(3) -0.005(3) B7 0.022(3) 0.022(3) 0.027(6) 0.000(3) -0.003(3) 0.002(3) B8 0.027(4) 0.037(4) 0.029(4) 0.007(4) 0.003(3) 0.005(4) B9 0.018(4) 0.033(4) 0.034(4) 0.007(3) 0.008(3) 0.006(3) B10 0.021(4) 0.029(4) 0.028(4) 0.004(3) -0.005(3) -0.001(3) B11 0.023(3) 0.029(3) 0.017(5) 0.002(4) -0.001(3) -0.005(3) B12 0.021(4) 0.033(4) 0.038(4) 0.001(3) -0.003(3) 0.003(3) C11 0.027(3) 0.030(3) 0.023(4) 0.002(3) -0.007(3) 0.000(2) O11 0.041(2) 0.036(2) 0.032(3) -0.001(3) -0.005(3) -0.015(2) C12 0.023(3) 0.025(3) 0.023(3) 0.004(3) 0.001(2) -0.002(3) O12 0.036(3) 0.043(3) 0.035(3) -0.008(2) 0.005(2) 0.006(2) C13 0.028(4) 0.034(4) 0.023(4) -0.001(3) -0.004(3) -0.016(3) O13 0.039(3) 0.056(3) 0.020(2) 0.000(2) -0.008(2) -0.007(3) S1 0.0279(8) 0.0276(8) 0.0218(8) 0.0005(7) -0.0058(7) -0.0028(7) C21 0.058(5) 0.051(4) 0.030(4) -0.012(3) -0.016(4) 0.017(4) C22 0.023(3) 0.038(4) 0.025(3) -0.001(3) 0.004(3) -0.005(3) C100 0.036(4) 0.043(4) 0.050(5) 0.000(4) 0.005(4) 0.007(3) Cl1 0.0657(13) 0.0500(11) 0.0422(11) -0.0029(9) -0.0142(10) 0.0216(10) Cl2 0.131(2) 0.0435(12) 0.0571(14) 0.0088(11) 0.0497(15) 0.0261(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru C13 1.917(8) . ? Ru C12 1.935(6) . ? Ru C11 1.966(6) . ? Ru B6 2.247(7) . ? Ru B3 2.260(7) . ? Ru C1 2.272(8) . ? Ru B7 2.291(6) . ? Ru B11 2.295(6) . ? C1 B4 1.710(11) . ? C1 B5 1.722(10) . ? C1 B3 1.758(10) . ? C1 B6 1.794(10) . ? C1 S1 1.813(7) . ? B3 B8 1.768(10) . ? B3 B7 1.805(10) . ? B3 B4 1.812(11) . ? B4 B9 1.754(11) . ? B4 B8 1.770(11) . ? B4 B5 1.806(11) . ? B5 B10 1.755(10) . ? B5 B9 1.760(10) . ? B5 B6 1.826(10) . ? B6 B10 1.773(9) . ? B6 B11 1.808(10) . ? B7 B12 1.768(10) . ? B7 B8 1.777(11) . ? B7 B11 1.847(10) . ? B8 B12 1.763(11) . ? B8 B9 1.780(10) . ? B9 B12 1.775(12) . ? B9 B10 1.792(11) . ? B10 B11 1.778(12) . ? B10 B12 1.797(10) . ? B11 B12 1.784(11) . ? C11 O11 1.125(6) . ? C12 O12 1.130(7) . ? C13 O13 1.122(8) . ? S1 C22 1.770(6) . ? S1 C21 1.804(7) . ? C100 Cl2 1.714(8) . ? C100 Cl1 1.748(7) . ? 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 C13 Ru C12 88.8(3) . . ? C13 Ru C11 92.0(3) . . ? C12 Ru C11 93.2(3) . . ? C13 Ru B6 123.7(3) . . ? C12 Ru B6 84.1(3) . . ? C11 Ru B6 144.1(3) . . ? C13 Ru B3 121.8(3) . . ? C12 Ru B3 149.1(2) . . ? C11 Ru B3 83.0(3) . . ? B6 Ru B3 81.5(3) . . ? C13 Ru C1 159.6(2) . . ? C12 Ru C1 106.1(2) . . ? C11 Ru C1 100.9(3) . . ? B6 Ru C1 46.8(2) . . ? B3 Ru C1 45.6(2) . . ? C13 Ru B7 83.1(3) . . ? C12 Ru B7 155.2(2) . . ? C11 Ru B7 110.5(2) . . ? B6 Ru B7 81.0(3) . . ? B3 Ru B7 46.7(3) . . ? C1 Ru B7 77.6(3) . . ? C13 Ru B11 84.1(3) . . ? C12 Ru B11 108.5(3) . . ? C11 Ru B11 157.9(2) . . ? B6 Ru B11 46.9(3) . . ? B3 Ru B11 80.7(3) . . ? C1 Ru B11 78.0(3) . . ? B7 Ru B11 47.5(3) . . ? B4 C1 B5 63.5(5) . . ? B4 C1 B3 63.0(4) . . ? B5 C1 B3 114.4(5) . . ? B4 C1 B6 114.5(5) . . ? B5 C1 B6 62.5(4) . . ? B3 C1 B6 111.7(5) . . ? B4 C1 S1 115.4(5) . . ? B5 C1 S1 118.0(5) . . ? B3 C1 S1 117.5(5) . . ? B6 C1 S1 121.1(4) . . ? B4 C1 Ru 125.0(4) . . ? B5 C1 Ru 123.8(4) . . ? B3 C1 Ru 66.8(3) . . ? B6 C1 Ru 65.9(3) . . ? S1 C1 Ru 106.4(4) . . ? C1 B3 B8 103.6(5) . . ? C1 B3 B7 106.7(5) . . ? B8 B3 B7 59.6(4) . . ? C1 B3 B4 57.2(4) . . ? B8 B3 B4 59.2(4) . . ? B7 B3 B4 107.7(5) . . ? C1 B3 Ru 67.5(3) . . ? B8 B3 Ru 120.9(4) . . ? B7 B3 Ru 67.6(3) . . ? B4 B3 Ru 120.5(4) . . ? C1 B4 B9 105.0(6) . . ? C1 B4 B8 105.5(6) . . ? B9 B4 B8 60.7(4) . . ? C1 B4 B5 58.6(4) . . ? B9 B4 B5 59.2(4) . . ? B8 B4 B5 107.6(5) . . ? C1 B4 B3 59.8(4) . . ? B9 B4 B3 107.8(6) . . ? B8 B4 B3 59.1(4) . . ? B5 B4 B3 107.8(5) . . ? C1 B5 B10 106.0(5) . . ? C1 B5 B9 104.2(5) . . ? B10 B5 B9 61.3(4) . . ? C1 B5 B4 57.9(4) . . ? B10 B5 B4 108.2(5) . . ? B9 B5 B4 58.9(4) . . ? C1 B5 B6 60.7(4) . . ? B10 B5 B6 59.3(4) . . ? B9 B5 B6 108.4(5) . . ? B4 B5 B6 108.5(5) . . ? B10 B6 C1 102.2(5) . . ? B10 B6 B11 59.5(4) . . ? C1 B6 B11 105.8(5) . . ? B10 B6 B5 58.4(4) . . ? C1 B6 B5 56.8(4) . . ? B11 B6 B5 106.7(5) . . ? B10 B6 Ru 120.9(4) . . ? C1 B6 Ru 67.3(3) . . ? B11 B6 Ru 67.9(3) . . ? B5 B6 Ru 120.0(4) . . ? B12 B7 B8 59.6(4) . . ? B12 B7 B3 106.6(5) . . ? B8 B7 B3 59.2(4) . . ? B12 B7 B11 59.1(4) . . ? B8 B7 B11 107.1(6) . . ? B3 B7 B11 107.7(5) . . ? B12 B7 Ru 119.0(4) . . ? B8 B7 Ru 118.9(4) . . ? B3 B7 Ru 65.7(3) . . ? B11 B7 Ru 66.3(3) . . ? B12 B8 B3 108.5(5) . . ? B12 B8 B4 108.1(5) . . ? B3 B8 B4 61.6(4) . . ? B12 B8 B7 59.9(4) . . ? B3 B8 B7 61.2(4) . . ? B4 B8 B7 110.8(5) . . ? B12 B8 B9 60.1(4) . . ? B3 B8 B9 108.6(5) . . ? B4 B8 B9 59.2(4) . . ? B7 B8 B9 109.0(5) . . ? B4 B9 B5 61.9(4) . . ? B4 B9 B12 108.3(5) . . ? B5 B9 B12 108.3(5) . . ? B4 B9 B8 60.1(4) . . ? B5 B9 B8 109.3(5) . . ? B12 B9 B8 59.5(4) . . ? B4 B9 B10 108.9(5) . . ? B5 B9 B10 59.2(4) . . ? B12 B9 B10 60.5(4) . . ? B8 B9 B10 108.1(6) . . ? B5 B10 B6 62.3(4) . . ? B5 B10 B11 111.2(5) . . ? B6 B10 B11 61.2(4) . . ? B5 B10 B9 59.5(4) . . ? B6 B10 B9 109.3(5) . . ? B11 B10 B9 108.7(5) . . ? B5 B10 B12 107.5(5) . . ? B6 B10 B12 108.3(5) . . ? B11 B10 B12 59.9(4) . . ? B9 B10 B12 59.3(4) . . ? B10 B11 B12 60.6(5) . . ? B10 B11 B6 59.3(4) . . ? B12 B11 B6 107.3(6) . . ? B10 B11 B7 107.0(6) . . ? B12 B11 B7 58.3(4) . . ? B6 B11 B7 107.5(5) . . ? B10 B11 Ru 118.3(5) . . ? B12 B11 Ru 118.1(5) . . ? B6 B11 Ru 65.2(3) . . ? B7 B11 Ru 66.2(3) . . ? B8 B12 B7 60.4(4) . . ? B8 B12 B9 60.4(4) . . ? B7 B12 B9 109.7(5) . . ? B8 B12 B11 110.6(5) . . ? B7 B12 B11 62.7(4) . . ? B9 B12 B11 109.2(5) . . ? B8 B12 B10 108.6(5) . . ? B7 B12 B10 109.7(5) . . ? B9 B12 B10 60.2(4) . . ? B11 B12 B10 59.5(4) . . ? O11 C11 Ru 174.7(6) . . ? O12 C12 Ru 176.7(5) . . ? O13 C13 Ru 176.3(7) . . ? C22 S1 C21 99.0(3) . . ? C22 S1 C1 105.0(3) . . ? C21 S1 C1 108.1(4) . . ? Cl2 C100 Cl1 112.2(4) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.758 _refine_diff_density_min -1.320 _refine_diff_density_rms 0.143 #===END