# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' #TrackingRef '- publiLSL213LV.cif' _journal_coden_Cambridge 0222 # 1. SUBMISSION DETAILS _publ_contact_letter ; Please consider this CIF submission for publication in Dalton Transactions ; _publ_contact_author ; Sylviane Sabo-Etienne ; _publ_contact_author_address ; Laboratoire de Chimie de Coordination 205 Route de Narbonne 31077 Toulouse Cedex 04 ; _publ_contact_author_email sylviane.sabo@lcc-toulouse.fr #============================================================================= # 2. TITLE AND AUTHOR LIST _publ_section_title ;Silyl and ?-silane ruthenium complexes: Chlorine substituent effects on the catalysed silylation of ethylene ; loop_ _publ_author_name _publ_author_address "S\'ebastien Lachaize" ; CNRS, LCC (Laboratoire de Chimie de Coordination) 205 Route de Narbonne F-31077 Toulouse, France Universit\'e de Toulouse, UPS, INPT, F-31077 Toulouse, France ; 'Laure Vendier' ; CNRS, LCC (Laboratoire de Chimie de Coordination) 205 Route de Narbonne F-31077 Toulouse, France Universit\'e de Toulouse, UPS, INPT, F-31077 Toulouse, France ; S.Sabo-Etienne ; CNRS, LCC (Laboratoire de Chimie de Coordination) 205 Route de Narbonne F-31077 Toulouse, France Universit\'e de Toulouse, UPS, INPT, F-31077 Toulouse, France ; #============================================================================== _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo, G., Guagliardi, A., Burla, M.C., Polidori, G. and Camalli, M. (1994)., SIR92 program for automatic solution of crystal structures by direct methods. J. Appl. Cryst. 27, 435. Sheldrick, G. M. (1997). SHELXL97. Program for the refinement of Crystal Structures. University of Gottingen, Germany. MULTI SCAN - c.f. r.h. blessing, acta cryst. (1995), a51, 33-38 WINGX - 1.63 Integrated System of Windows Programs for the Solution, Refinement and Analysis of Single Crystal X-Ray Diffraction Data. Farrugia, L. J. Appl. Crystallogr., 1999, 32, 837. ORTEP3 for Windows, Farrugia, L. J. J. Appl. Crystallogr. 1997, 30, 565.; ; _publ_contact_author_name 'Sylviane Sabo-Etienne' #------------------ SECTION 2. COMPOUND(S) DETAILS -------------------------# data_lsl213lv _database_code_depnum_ccdc_archive 'CCDC 765257' #TrackingRef '- publiLSL213LV.cif' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C38 H72 Cl4 P2 Ru1 Si2' _chemical_formula_sum 'C38 H72 Cl4 P2 Ru Si2' _chemical_formula_weight 889.95 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 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 9.7901(8) _cell_length_b 44.9570(7) _cell_length_c 10.1672(9) _cell_angle_alpha 90 _cell_angle_beta 105.977(3) _cell_angle_gamma 90 _cell_volume 4302.1(5) _cell_formula_units_Z 4 _cell_measurement_temperature 160(2) _cell_measurement_reflns_used 5400 _cell_measurement_theta_min 2.2 _cell_measurement_theta_max 30 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.05 _exptl_crystal_density_diffrn 1.374 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1880 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.769 _exptl_absorpt_correction_type refdelf _exptl_absorpt_process_details ; (See: Walker, N. & Stuart, D. (1983) Acta Cryst. A39, 158-166) ; _exptl_absorpt_correction_T_min 0.569 _exptl_absorpt_correction_T_max 0.869 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 160(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford-Diffraction XCALIBUR' _diffrn_measurement_method \w-\f _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_av_R_equivalents 0.1095 _diffrn_reflns_av_unetI/netI 0.1294 _diffrn_reflns_number 28188 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -54 _diffrn_reflns_limit_k_max 54 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 3.13 _diffrn_reflns_theta_max 25.35 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _reflns_number_total 7865 _reflns_number_gt 5254 _reflns_threshold_expression >2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd.' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd.' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd.' _computing_structure_solution 'SIR92 (Giacovazzo et al, 1993)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^ > 2\s(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^)+(0.0394P)^2^+7.2472P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 7865 _refine_ls_number_parameters 414 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.133 _refine_ls_R_factor_gt 0.0867 _refine_ls_wR_factor_ref 0.1532 _refine_ls_wR_factor_gt 0.1396 _refine_ls_goodness_of_fit_ref 1.137 _refine_ls_restrained_S_all 1.137 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.82 _refine_diff_density_min -0.815 _refine_diff_density_rms 0.12 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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' 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 C111 C 0.7374(9) 0.12504(19) 1.6793(7) 0.032(2) Uani 1 1 d . . . H11A H 0.6713 0.1272 1.7369 0.038 Uiso 1 1 calc R . . H11B H 0.8224 0.1142 1.7331 0.038 Uiso 1 1 calc R . . C112 C 0.6582(9) 0.17282(18) 1.5516(8) 0.032(2) Uani 1 1 d . . . H11C H 0.6931 0.1921 1.5263 0.038 Uiso 1 1 calc R . . H11D H 0.5862 0.177 1.6011 0.038 Uiso 1 1 calc R . . C113 C 0.7812(10) 0.15540(19) 1.6435(8) 0.039(2) Uani 1 1 d . . . H11E H 0.8569 0.1532 1.5967 0.047 Uiso 1 1 calc R . . H11F H 0.8211 0.1668 1.7288 0.047 Uiso 1 1 calc R . . C114 C 0.5911(8) 0.15478(16) 1.4226(7) 0.0210(17) Uani 1 1 d . . . H114 H 0.6699 0.1506 1.3802 0.025 Uiso 1 1 calc R . . C115 C 0.6659(8) 0.10719(18) 1.5529(8) 0.028(2) Uani 1 1 d . . . H11G H 0.6311 0.0882 1.5807 0.033 Uiso 1 1 calc R . . H11H H 0.7361 0.1025 1.502 0.033 Uiso 1 1 calc R . . C116 C 0.5415(8) 0.12416(17) 1.4596(7) 0.0242(18) Uani 1 1 d . . . H11I H 0.4661 0.1269 1.5065 0.029 Uiso 1 1 calc R . . H11J H 0.5012 0.1126 1.375 0.029 Uiso 1 1 calc R . . C121 C 0.6919(8) 0.19364(16) 1.2129(8) 0.0235(18) Uani 1 1 d . . . H12A H 0.7538 0.1916 1.3075 0.028 Uiso 1 1 calc R . . H12B H 0.6888 0.1741 1.1668 0.028 Uiso 1 1 calc R . . C122 C 0.5405(8) 0.20231(16) 1.2171(7) 0.0215(18) Uani 1 1 d . . . H122 H 0.4846 0.2052 1.1197 0.026 Uiso 1 1 calc R . . C123 C 0.6111(9) 0.25630(17) 1.2071(8) 0.030(2) Uani 1 1 d . . . H12C H 0.5473 0.2586 1.1134 0.036 Uiso 1 1 calc R . . H12D H 0.6169 0.2757 1.2541 0.036 Uiso 1 1 calc R . . C124 C 0.7540(9) 0.21684(18) 1.1371(9) 0.036(2) Uani 1 1 d . . . H12E H 0.8518 0.2109 1.1386 0.043 Uiso 1 1 calc R . . H12F H 0.6965 0.2175 1.0404 0.043 Uiso 1 1 calc R . . C125 C 0.5492(9) 0.23314(16) 1.2845(8) 0.0246(18) Uani 1 1 d . . . H12G H 0.453 0.2394 1.2866 0.03 Uiso 1 1 calc R . . H12H H 0.6095 0.2319 1.3801 0.03 Uiso 1 1 calc R . . C126 C 0.7573(9) 0.24730(18) 1.1992(9) 0.034(2) Uani 1 1 d . . . H12I H 0.792 0.2619 1.1431 0.041 Uiso 1 1 calc R . . H12J H 0.8239 0.2473 1.2922 0.041 Uiso 1 1 calc R . . C131 C 0.3377(8) 0.19346(16) 1.3756(7) 0.0212(17) Uani 1 1 d . . . H131 H 0.4025 0.2087 1.4316 0.025 Uiso 1 1 calc R . . C132 C 0.1494(10) 0.23282(19) 1.3554(9) 0.036(2) Uani 1 1 d . . . H13A H 0.2205 0.2479 1.401 0.043 Uiso 1 1 calc R . . H13B H 0.0701 0.2432 1.2899 0.043 Uiso 1 1 calc R . . C133 C 0.2087(10) 0.19839(19) 1.5562(8) 0.035(2) Uani 1 1 d . . . H13C H 0.1684 0.1872 1.6205 0.043 Uiso 1 1 calc R . . H13D H 0.2835 0.2118 1.6105 0.043 Uiso 1 1 calc R . . C134 C 0.0936(10) 0.2166(2) 1.4621(9) 0.042(2) Uani 1 1 d . . . H13E H 0.0571 0.2314 1.5163 0.05 Uiso 1 1 calc R . . H13F H 0.0139 0.2035 1.4153 0.05 Uiso 1 1 calc R . . C135 C 0.2178(8) 0.21067(17) 1.2780(8) 0.0254(19) Uani 1 1 d . . . H13G H 0.1448 0.1965 1.2269 0.03 Uiso 1 1 calc R . . H13H H 0.2557 0.2216 1.211 0.03 Uiso 1 1 calc R . . C136 C 0.2750(9) 0.17646(19) 1.4748(8) 0.034(2) Uani 1 1 d . . . H13I H 0.3505 0.1648 1.5386 0.041 Uiso 1 1 calc R . . H13J H 0.2014 0.1625 1.4234 0.041 Uiso 1 1 calc R . . C211 C 0.6231(9) 0.00105(18) 1.3172(9) 0.038(2) Uani 1 1 d . . . H21A H 0.605 -0.0013 1.4078 0.046 Uiso 1 1 calc R . . H21B H 0.7017 -0.0125 1.3135 0.046 Uiso 1 1 calc R . . C212 C 0.3693(8) 0.01444(16) 1.2003(8) 0.0278(19) Uani 1 1 d . . . H21C H 0.3423 0.0135 1.2871 0.033 Uiso 1 1 calc R . . H21D H 0.2856 0.0087 1.1249 0.033 Uiso 1 1 calc R . . C213 C 0.6657(9) 0.03247(19) 1.3005(10) 0.042(2) Uani 1 1 d . . . H21E H 0.696 0.034 1.2155 0.051 Uiso 1 1 calc R . . H21F H 0.7482 0.0377 1.3782 0.051 Uiso 1 1 calc R . . C214 C 0.4142(8) 0.04657(16) 1.1768(7) 0.0211(18) Uani 1 1 d . . . H214 H 0.4454 0.0462 1.0911 0.025 Uiso 1 1 calc R . . C215 C 0.5462(8) 0.05476(18) 1.2940(8) 0.029(2) Uani 1 1 d . . . H21G H 0.5787 0.075 1.2788 0.035 Uiso 1 1 calc R . . H21H H 0.5214 0.0547 1.382 0.035 Uiso 1 1 calc R . . C216 C 0.4910(9) -0.00728(18) 1.2062(9) 0.038(2) Uani 1 1 d . . . H21I H 0.4611 -0.0276 1.2235 0.045 Uiso 1 1 calc R . . H21J H 0.5129 -0.0074 1.1167 0.045 Uiso 1 1 calc R . . C221 C -0.1410(9) 0.05427(18) 0.9059(8) 0.029(2) Uani 1 1 d . . . H22A H -0.156 0.0373 0.9625 0.035 Uiso 1 1 calc R . . H22B H -0.2295 0.0662 0.8804 0.035 Uiso 1 1 calc R . . C222 C 0.0351(9) 0.02673(18) 0.8108(8) 0.0273(19) Uani 1 1 d . . . H22C H 0.0296 0.0084 0.8631 0.033 Uiso 1 1 calc R . . H22D H 0.0558 0.0208 0.7245 0.033 Uiso 1 1 calc R . . C223 C -0.1087(9) 0.04264(18) 0.7770(7) 0.028(2) Uani 1 1 d . . . H22E H -0.1078 0.0595 0.7144 0.033 Uiso 1 1 calc R . . H22F H -0.1844 0.0287 0.7296 0.033 Uiso 1 1 calc R . . C224 C 0.1236(8) 0.05682(17) 1.0251(7) 0.0212(17) Uani 1 1 d . . . H224 H 0.106 0.0383 1.0721 0.025 Uiso 1 1 calc R . . C225 C -0.0190(8) 0.07348(16) 0.9888(7) 0.0214(17) Uani 1 1 d . . . H22G H -0.0402 0.0799 1.0741 0.026 Uiso 1 1 calc R . . H22H H -0.0111 0.0915 0.9354 0.026 Uiso 1 1 calc R . . C226 C 0.1552(8) 0.04602(18) 0.8933(7) 0.0245(18) Uani 1 1 d . . . H22I H 0.1676 0.0634 0.8378 0.029 Uiso 1 1 calc R . . H22J H 0.2448 0.0345 0.9166 0.029 Uiso 1 1 calc R . . C231 C 0.0833(9) 0.05299(19) 1.4701(8) 0.032(2) Uani 1 1 d . . . H23A H 0.018 0.037 1.4812 0.038 Uiso 1 1 calc R . . H23B H 0.1731 0.0509 1.5437 0.038 Uiso 1 1 calc R . . C232 C 0.1128(9) 0.10841(18) 1.4635(8) 0.030(2) Uani 1 1 d . . . H23C H 0.2019 0.1082 1.5388 0.035 Uiso 1 1 calc R . . H23D H 0.0645 0.1276 1.4665 0.035 Uiso 1 1 calc R . . C233 C 0.2118(8) 0.07488(16) 1.3107(7) 0.0194(17) Uani 1 1 d . . . H233 H 0.3 0.0732 1.3884 0.023 Uiso 1 1 calc R . . C234 C 0.1132(8) 0.04998(16) 1.3308(8) 0.0251(19) Uani 1 1 d . . . H23E H 0.1579 0.0305 1.3249 0.03 Uiso 1 1 calc R . . H23F H 0.0227 0.0509 1.2574 0.03 Uiso 1 1 calc R . . C235 C 0.0173(10) 0.08300(19) 1.4820(8) 0.036(2) Uani 1 1 d . . . H23G H -0.0005 0.0847 1.5729 0.043 Uiso 1 1 calc R . . H23H H -0.0753 0.0845 1.4117 0.043 Uiso 1 1 calc R . . C236 C 0.1472(9) 0.10520(16) 1.3256(7) 0.0214(16) Uani 1 1 d . . . H23I H 0.0591 0.1079 1.2505 0.026 Uiso 1 1 calc R . . H23J H 0.2147 0.121 1.3174 0.026 Uiso 1 1 calc R . . Ru1 Ru 0.34977(6) 0.126924(13) 1.17164(6) 0.01560(16) Uani 1 1 d . A . P1 P 0.4475(2) 0.17183(4) 1.28549(18) 0.0173(4) Uani 1 1 d . . . P2 P 0.2712(2) 0.07558(4) 1.15070(19) 0.0170(4) Uani 1 1 d . . . Cl1 Cl -0.0087(3) 0.15200(5) 1.0349(2) 0.0447(6) Uani 1 1 d . A . Cl4 Cl 0.7074(2) 0.11357(5) 1.1516(2) 0.0366(5) Uani 1 1 d . A . Si1 Si 0.1882(2) 0.14821(5) 0.9942(2) 0.0216(5) Uani 1 1 d . . . C2A C 0.2203(4) 0.19114(7) 0.9414(3) 0.0192(4) Uani 0.57 1 d P A 1 H2A H 0.2463 0.2035 1.0238 0.023 Uiso 0.57 1 calc PR A 1 H2B H 0.1328 0.1988 0.8784 0.023 Uiso 0.57 1 calc PR A 1 H2C H 0.2971 0.1916 0.8967 0.023 Uiso 0.57 1 calc PR A 1 Cl3A Cl 0.1363(3) 0.12852(6) 0.8026(2) 0.0192(4) Uani 0.57 1 d P A 1 Cl3B Cl 0.2203(4) 0.19114(7) 0.9414(3) 0.0192(4) Uani 0.43 1 d P A 2 C2B C 0.1363(3) 0.12852(6) 0.8026(2) 0.0192(4) Uani 0.43 1 d P A 2 H2B1 H 0.0771 0.1422 0.7354 0.029 Uiso 0.43 1 calc PR A 2 H2B2 H 0.0837 0.1101 0.805 0.029 Uiso 0.43 1 calc PR A 2 H2B3 H 0.2234 0.124 0.7769 0.029 Uiso 0.43 1 calc PR A 2 Si2 Si 0.4958(2) 0.12394(5) 1.0331(2) 0.0239(5) Uani 1 1 d . . . Cl5A Cl 0.4668(3) 0.08878(6) 0.8948(2) 0.0322(6) Uani 0.77 1 d P A 1 C6A C 0.5238(5) 0.15745(11) 0.9130(5) 0.0322(6) Uani 0.77 1 d P A 1 H6A H 0.5392 0.176 0.9657 0.039 Uiso 0.77 1 calc PR A 1 H6B H 0.4392 0.1594 0.8351 0.039 Uiso 0.77 1 calc PR A 1 H6C H 0.6067 0.1533 0.8796 0.039 Uiso 0.77 1 calc PR A 1 Cl5B Cl 0.5238(5) 0.15745(11) 0.9130(5) 0.0322(6) Uani 0.23 1 d P A 2 C6B C 0.4668(3) 0.08878(6) 0.8948(2) 0.0322(6) Uani 0.23 1 d P A 2 H6B1 H 0.4182 0.0724 0.927 0.048 Uiso 0.23 1 calc PR A 2 H6B2 H 0.5594 0.0819 0.8875 0.048 Uiso 0.23 1 calc PR A 2 H6B3 H 0.4091 0.0955 0.8049 0.048 Uiso 0.23 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 C111 0.035(5) 0.033(5) 0.025(4) 0.001(4) 0.003(4) 0.001(4) C112 0.041(6) 0.026(5) 0.025(4) -0.008(4) 0.001(4) -0.002(4) C113 0.042(6) 0.040(6) 0.028(5) -0.006(4) -0.003(4) 0.002(5) C114 0.017(4) 0.024(4) 0.020(4) 0.000(3) 0.002(3) -0.003(3) C115 0.018(4) 0.033(5) 0.028(4) 0.006(4) -0.002(4) 0.013(4) C116 0.016(4) 0.031(5) 0.023(4) -0.004(4) 0.000(3) -0.002(4) C121 0.022(5) 0.018(4) 0.030(4) 0.007(3) 0.006(4) 0.001(3) C122 0.021(4) 0.024(4) 0.014(4) 0.001(3) -0.003(3) -0.004(4) C123 0.032(5) 0.019(4) 0.038(5) 0.007(4) 0.007(4) -0.003(4) C124 0.025(5) 0.038(5) 0.049(5) 0.011(5) 0.015(4) -0.004(4) C125 0.025(5) 0.022(4) 0.026(4) 0.003(4) 0.004(4) 0.001(4) C126 0.032(5) 0.028(5) 0.047(5) 0.010(4) 0.019(4) 0.000(4) C131 0.018(4) 0.021(4) 0.023(4) 0.000(3) 0.003(3) 0.008(3) C132 0.033(5) 0.032(5) 0.042(5) -0.002(4) 0.012(4) 0.013(4) C133 0.043(6) 0.037(5) 0.033(5) -0.001(4) 0.020(5) 0.008(4) C134 0.039(6) 0.040(6) 0.054(6) -0.014(5) 0.026(5) 0.010(5) C135 0.022(5) 0.027(5) 0.025(4) -0.002(4) 0.004(4) 0.001(4) C136 0.042(6) 0.033(5) 0.035(5) 0.007(4) 0.021(4) 0.016(4) C211 0.028(5) 0.032(5) 0.051(6) 0.007(5) 0.003(5) 0.015(4) C212 0.025(5) 0.016(4) 0.037(5) -0.003(4) 0.000(4) 0.001(4) C213 0.022(5) 0.039(6) 0.061(6) 0.002(5) 0.004(5) 0.000(4) C214 0.020(4) 0.019(4) 0.023(4) 0.005(3) 0.003(4) 0.012(3) C215 0.020(5) 0.025(5) 0.037(5) 0.003(4) -0.002(4) -0.001(4) C216 0.041(6) 0.020(5) 0.049(6) 0.000(4) 0.008(5) 0.012(4) C221 0.023(5) 0.033(5) 0.028(4) -0.002(4) 0.000(4) -0.006(4) C222 0.035(5) 0.028(5) 0.020(4) -0.006(4) 0.009(4) -0.005(4) C223 0.029(5) 0.034(5) 0.018(4) 0.002(4) 0.003(4) -0.009(4) C224 0.021(4) 0.020(4) 0.020(4) 0.001(3) 0.003(3) 0.000(3) C225 0.024(5) 0.015(4) 0.024(4) -0.005(3) 0.005(4) 0.002(3) C226 0.016(4) 0.031(5) 0.025(4) -0.001(4) 0.004(4) -0.002(4) C231 0.028(5) 0.042(6) 0.027(4) 0.013(4) 0.010(4) -0.007(4) C232 0.029(5) 0.033(5) 0.031(4) -0.012(4) 0.016(4) -0.007(4) C233 0.021(4) 0.020(4) 0.019(4) 0.004(3) 0.009(3) 0.004(3) C234 0.028(5) 0.015(4) 0.037(5) 0.004(4) 0.017(4) -0.001(3) C235 0.047(6) 0.041(6) 0.025(4) -0.001(4) 0.018(4) -0.001(5) C236 0.022(4) 0.023(4) 0.021(4) -0.001(4) 0.009(3) -0.003(4) Ru1 0.0158(3) 0.0144(3) 0.0162(3) 0.0004(3) 0.0038(2) 0.0009(3) P1 0.0177(11) 0.0155(10) 0.0175(10) 0.0017(8) 0.0027(8) 0.0015(8) P2 0.0162(11) 0.0155(10) 0.0199(10) -0.0005(8) 0.0061(9) 0.0018(8) Cl1 0.0398(14) 0.0444(15) 0.0474(14) 0.0009(12) 0.0078(11) 0.0046(12) Cl4 0.0256(12) 0.0364(12) 0.0502(13) -0.0004(11) 0.0146(11) 0.0046(10) Si1 0.0232(12) 0.0210(12) 0.0185(10) 0.0011(9) 0.0020(9) 0.0018(10) C2A 0.0272(12) 0.0185(11) 0.0091(9) 0.0015(9) 0.0005(8) 0.0016(10) Cl3A 0.0272(12) 0.0185(11) 0.0091(9) 0.0015(9) 0.0005(8) 0.0016(10) Cl3B 0.0272(12) 0.0185(11) 0.0091(9) 0.0015(9) 0.0005(8) 0.0016(10) C2B 0.0272(12) 0.0185(11) 0.0091(9) 0.0015(9) 0.0005(8) 0.0016(10) Si2 0.0258(12) 0.0239(12) 0.0257(11) -0.0002(10) 0.0133(10) 0.0034(11) Cl5A 0.0349(14) 0.0316(13) 0.0369(12) -0.0094(11) 0.0215(11) -0.0036(10) C6A 0.0349(14) 0.0316(13) 0.0369(12) -0.0094(11) 0.0215(11) -0.0036(10) Cl5B 0.0349(14) 0.0316(13) 0.0369(12) -0.0094(11) 0.0215(11) -0.0036(10) C6B 0.0349(14) 0.0316(13) 0.0369(12) -0.0094(11) 0.0215(11) -0.0036(10) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 C111 C113 1.505(11) . ? C111 C115 1.513(10) . ? C111 H11A 0.99 . ? C111 H11B 0.99 . ? C112 C113 1.522(11) . ? C112 C114 1.528(10) . ? C112 H11C 0.99 . ? C112 H11D 0.99 . ? C113 H11E 0.99 . ? C113 H11F 0.99 . ? C114 C116 1.540(10) . ? C114 P1 1.851(7) . ? C114 H114 1 . ? C115 C116 1.526(10) . ? C115 H11G 0.99 . ? C115 H11H 0.99 . ? C116 Ru1 3.014(7) . ? C116 H11I 0.99 . ? C116 H11J 0.99 . ? C121 C124 1.520(10) . ? C121 C122 1.545(10) . ? C121 H12A 0.99 . ? C121 H12B 0.99 . ? C122 C125 1.538(10) . ? C122 P1 1.880(7) . ? C122 H122 1 . ? C123 C126 1.511(11) . ? C123 C125 1.527(10) . ? C123 H12C 0.99 . ? C123 H12D 0.99 . ? C124 C126 1.505(11) . ? C124 H12E 0.99 . ? C124 H12F 0.99 . ? C125 H12G 0.99 . ? C125 H12H 0.99 . ? C126 H12I 0.99 . ? C126 H12J 0.99 . ? C131 C136 1.522(10) . ? C131 C135 1.523(10) . ? C131 P1 1.866(7) . ? C131 H131 1 . ? C132 C134 1.526(12) . ? C132 C135 1.532(10) . ? C132 H13A 0.99 . ? C132 H13B 0.99 . ? C133 C134 1.505(12) . ? C133 C136 1.541(10) . ? C133 H13C 0.99 . ? C133 H13D 0.99 . ? C134 H13E 0.99 . ? C134 H13F 0.99 . ? C135 H13G 0.99 . ? C135 H13H 0.99 . ? C136 H13I 0.99 . ? C136 H13J 0.99 . ? C211 C213 1.496(11) . ? C211 C216 1.511(11) . ? C211 H21A 0.99 . ? C211 H21B 0.99 . ? C212 C216 1.529(11) . ? C212 C214 1.547(10) . ? C212 H21C 0.99 . ? C212 H21D 0.99 . ? C213 C215 1.528(11) . ? C213 H21E 0.99 . ? C213 H21F 0.99 . ? C214 C215 1.542(10) . ? C214 P2 1.878(7) . ? C214 H214 1 . ? C215 H21G 0.99 . ? C215 H21H 0.99 . ? C216 H21I 0.99 . ? C216 H21J 0.99 . ? C221 C223 1.523(10) . ? C221 C225 1.526(10) . ? C221 H22A 0.99 . ? C221 H22B 0.99 . ? C222 C226 1.515(10) . ? C222 C223 1.531(11) . ? C222 H22C 0.99 . ? C222 H22D 0.99 . ? C223 H22E 0.99 . ? C223 H22F 0.99 . ? C224 C226 1.535(10) . ? C224 C225 1.537(10) . ? C224 P2 1.847(7) . ? C224 H224 1 . ? C225 H22G 0.99 . ? C225 H22H 0.99 . ? C226 H22I 0.99 . ? C226 H22J 0.99 . ? C231 C235 1.515(11) . ? C231 C234 1.529(10) . ? C231 H23A 0.99 . ? C231 H23B 0.99 . ? C232 C235 1.520(11) . ? C232 C236 1.536(10) . ? C232 H23C 0.99 . ? C232 H23D 0.99 . ? C233 C236 1.527(10) . ? C233 C234 1.528(10) . ? C233 P2 1.873(7) . ? C233 H233 1 . ? C234 H23E 0.99 . ? C234 H23F 0.99 . ? C235 H23G 0.99 . ? C235 H23H 0.99 . ? C236 Ru1 3.008(7) . ? C236 H23I 0.99 . ? C236 H23J 0.99 . ? Ru1 H23J 2.2569 . ? Ru1 Si1 2.259(2) . ? Ru1 Si2 2.270(2) . ? Ru1 H11J 2.2813 . ? Ru1 P1 2.392(2) . ? Ru1 P2 2.424(2) . ? Cl1 Si1 2.087(3) . ? Cl4 Si2 2.142(3) . ? Si1 C2A 2.050(4) . ? Si1 Cl3A 2.071(3) . ? C2A H2A 0.98 . ? C2A H2B 0.98 . ? C2A H2C 0.98 . ? Si2 C6A 2.005(5) . ? Si2 Cl5A 2.082(3) . ? C6A H6A 0.98 . ? C6A H6B 0.98 . ? C6A H6C 0.98 . ? 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 C113 C111 C115 111.8(6) . . ? C113 C111 H11A 109.3 . . ? C115 C111 H11A 109.3 . . ? C113 C111 H11B 109.3 . . ? C115 C111 H11B 109.3 . . ? H11A C111 H11B 107.9 . . ? C113 C112 C114 109.5(7) . . ? C113 C112 H11C 109.8 . . ? C114 C112 H11C 109.8 . . ? C113 C112 H11D 109.8 . . ? C114 C112 H11D 109.8 . . ? H11C C112 H11D 108.2 . . ? C111 C113 C112 112.7(8) . . ? C111 C113 H11E 109.1 . . ? C112 C113 H11E 109.1 . . ? C111 C113 H11F 109.1 . . ? C112 C113 H11F 109.1 . . ? H11E C113 H11F 107.8 . . ? C112 C114 C116 110.8(6) . . ? C112 C114 P1 119.0(6) . . ? C116 C114 P1 109.2(5) . . ? C112 C114 H114 105.6 . . ? C116 C114 H114 105.6 . . ? P1 C114 H114 105.6 . . ? C111 C115 C116 111.5(7) . . ? C111 C115 H11G 109.3 . . ? C116 C115 H11G 109.3 . . ? C111 C115 H11H 109.3 . . ? C116 C115 H11H 109.3 . . ? H11G C115 H11H 108 . . ? C115 C116 C114 110.3(6) . . ? C115 C116 Ru1 143.3(5) . . ? C114 C116 Ru1 83.1(4) . . ? C115 C116 H11I 109.6 . . ? C114 C116 H11I 109.6 . . ? Ru1 C116 H11I 96.6 . . ? C115 C116 H11J 109.6 . . ? C114 C116 H11J 109.6 . . ? Ru1 C116 H11J 35.5 . . ? H11I C116 H11J 108.1 . . ? C124 C121 C122 111.2(6) . . ? C124 C121 H12A 109.4 . . ? C122 C121 H12A 109.4 . . ? C124 C121 H12B 109.4 . . ? C122 C121 H12B 109.4 . . ? H12A C121 H12B 108 . . ? C125 C122 C121 107.7(6) . . ? C125 C122 P1 117.7(5) . . ? C121 C122 P1 113.1(5) . . ? C125 C122 H122 105.8 . . ? C121 C122 H122 105.8 . . ? P1 C122 H122 105.8 . . ? C126 C123 C125 111.1(7) . . ? C126 C123 H12C 109.4 . . ? C125 C123 H12C 109.4 . . ? C126 C123 H12D 109.4 . . ? C125 C123 H12D 109.4 . . ? H12C C123 H12D 108 . . ? C126 C124 C121 112.2(7) . . ? C126 C124 H12E 109.2 . . ? C121 C124 H12E 109.2 . . ? C126 C124 H12F 109.2 . . ? C121 C124 H12F 109.2 . . ? H12E C124 H12F 107.9 . . ? C123 C125 C122 111.5(6) . . ? C123 C125 H12G 109.3 . . ? C122 C125 H12G 109.3 . . ? C123 C125 H12H 109.3 . . ? C122 C125 H12H 109.3 . . ? H12G C125 H12H 108 . . ? C124 C126 C123 110.8(7) . . ? C124 C126 H12I 109.5 . . ? C123 C126 H12I 109.5 . . ? C124 C126 H12J 109.5 . . ? C123 C126 H12J 109.5 . . ? H12I C126 H12J 108.1 . . ? C136 C131 C135 107.9(7) . . ? C136 C131 P1 117.1(5) . . ? C135 C131 P1 112.9(5) . . ? C136 C131 H131 106 . . ? C135 C131 H131 106 . . ? P1 C131 H131 106 . . ? C134 C132 C135 110.4(7) . . ? C134 C132 H13A 109.6 . . ? C135 C132 H13A 109.6 . . ? C134 C132 H13B 109.6 . . ? C135 C132 H13B 109.6 . . ? H13A C132 H13B 108.1 . . ? C134 C133 C136 111.1(7) . . ? C134 C133 H13C 109.4 . . ? C136 C133 H13C 109.4 . . ? C134 C133 H13D 109.4 . . ? C136 C133 H13D 109.4 . . ? H13C C133 H13D 108 . . ? C133 C134 C132 111.1(7) . . ? C133 C134 H13E 109.4 . . ? C132 C134 H13E 109.4 . . ? C133 C134 H13F 109.4 . . ? C132 C134 H13F 109.4 . . ? H13E C134 H13F 108 . . ? C131 C135 C132 111.3(6) . . ? C131 C135 H13G 109.4 . . ? C132 C135 H13G 109.4 . . ? C131 C135 H13H 109.4 . . ? C132 C135 H13H 109.4 . . ? H13G C135 H13H 108 . . ? C131 C136 C133 109.9(7) . . ? C131 C136 H13I 109.7 . . ? C133 C136 H13I 109.7 . . ? C131 C136 H13J 109.7 . . ? C133 C136 H13J 109.7 . . ? H13I C136 H13J 108.2 . . ? C213 C211 C216 110.9(7) . . ? C213 C211 H21A 109.5 . . ? C216 C211 H21A 109.5 . . ? C213 C211 H21B 109.5 . . ? C216 C211 H21B 109.5 . . ? H21A C211 H21B 108 . . ? C216 C212 C214 110.6(7) . . ? C216 C212 H21C 109.5 . . ? C214 C212 H21C 109.5 . . ? C216 C212 H21D 109.5 . . ? C214 C212 H21D 109.5 . . ? H21C C212 H21D 108.1 . . ? C211 C213 C215 113.0(7) . . ? C211 C213 H21E 109 . . ? C215 C213 H21E 109 . . ? C211 C213 H21F 109 . . ? C215 C213 H21F 109 . . ? H21E C213 H21F 107.8 . . ? C215 C214 C212 108.5(6) . . ? C215 C214 P2 112.2(5) . . ? C212 C214 P2 116.0(5) . . ? C215 C214 H214 106.5 . . ? C212 C214 H214 106.5 . . ? P2 C214 H214 106.5 . . ? C213 C215 C214 110.3(7) . . ? C213 C215 H21G 109.6 . . ? C214 C215 H21G 109.6 . . ? C213 C215 H21H 109.6 . . ? C214 C215 H21H 109.6 . . ? H21G C215 H21H 108.1 . . ? C211 C216 C212 111.6(7) . . ? C211 C216 H21I 109.3 . . ? C212 C216 H21I 109.3 . . ? C211 C216 H21J 109.3 . . ? C212 C216 H21J 109.3 . . ? H21I C216 H21J 108 . . ? C223 C221 C225 110.6(7) . . ? C223 C221 H22A 109.5 . . ? C225 C221 H22A 109.5 . . ? C223 C221 H22B 109.5 . . ? C225 C221 H22B 109.5 . . ? H22A C221 H22B 108.1 . . ? C226 C222 C223 112.5(7) . . ? C226 C222 H22C 109.1 . . ? C223 C222 H22C 109.1 . . ? C226 C222 H22D 109.1 . . ? C223 C222 H22D 109.1 . . ? H22C C222 H22D 107.8 . . ? C221 C223 C222 111.3(6) . . ? C221 C223 H22E 109.4 . . ? C222 C223 H22E 109.4 . . ? C221 C223 H22F 109.4 . . ? C222 C223 H22F 109.4 . . ? H22E C223 H22F 108 . . ? C226 C224 C225 109.4(6) . . ? C226 C224 P2 116.2(5) . . ? C225 C224 P2 115.4(5) . . ? C226 C224 H224 104.8 . . ? C225 C224 H224 104.8 . . ? P2 C224 H224 104.8 . . ? C221 C225 C224 112.2(6) . . ? C221 C225 H22G 109.2 . . ? C224 C225 H22G 109.2 . . ? C221 C225 H22H 109.2 . . ? C224 C225 H22H 109.2 . . ? H22G C225 H22H 107.9 . . ? C222 C226 C224 110.6(6) . . ? C222 C226 H22I 109.5 . . ? C224 C226 H22I 109.5 . . ? C222 C226 H22J 109.5 . . ? C224 C226 H22J 109.5 . . ? H22I C226 H22J 108.1 . . ? C235 C231 C234 110.3(6) . . ? C235 C231 H23A 109.6 . . ? C234 C231 H23A 109.6 . . ? C235 C231 H23B 109.6 . . ? C234 C231 H23B 109.6 . . ? H23A C231 H23B 108.1 . . ? C235 C232 C236 109.8(6) . . ? C235 C232 H23C 109.7 . . ? C236 C232 H23C 109.7 . . ? C235 C232 H23D 109.7 . . ? C236 C232 H23D 109.7 . . ? H23C C232 H23D 108.2 . . ? C236 C233 C234 110.3(6) . . ? C236 C233 P2 107.9(5) . . ? C234 C233 P2 119.1(5) . . ? C236 C233 H233 106.2 . . ? C234 C233 H233 106.2 . . ? P2 C233 H233 106.2 . . ? C233 C234 C231 110.4(6) . . ? C233 C234 H23E 109.6 . . ? C231 C234 H23E 109.6 . . ? C233 C234 H23F 109.6 . . ? C231 C234 H23F 109.6 . . ? H23E C234 H23F 108.1 . . ? C231 C235 C232 111.6(7) . . ? C231 C235 H23G 109.3 . . ? C232 C235 H23G 109.3 . . ? C231 C235 H23H 109.3 . . ? C232 C235 H23H 109.3 . . ? H23G C235 H23H 108 . . ? C233 C236 C232 112.0(6) . . ? C233 C236 Ru1 83.6(4) . . ? C232 C236 Ru1 141.8(5) . . ? C233 C236 H23I 109.2 . . ? C232 C236 H23I 109.2 . . ? Ru1 C236 H23I 96.8 . . ? C233 C236 H23J 109.2 . . ? C232 C236 H23J 109.2 . . ? Ru1 C236 H23J 34.1 . . ? H23I C236 H23J 107.9 . . ? H23J Ru1 Si1 99.6 . . ? H23J Ru1 Si2 169.5 . . ? Si1 Ru1 Si2 87.21(8) . . ? H23J Ru1 H11J 74 . . ? Si1 Ru1 H11J 169 . . ? Si2 Ru1 H11J 100.5 . . ? H23J Ru1 P1 90.6 . . ? Si1 Ru1 P1 97.35(7) . . ? Si2 Ru1 P1 96.52(8) . . ? H11J Ru1 P1 74.1 . . ? H23J Ru1 P2 73.5 . . ? Si1 Ru1 P2 101.40(8) . . ? Si2 Ru1 P2 97.37(8) . . ? H11J Ru1 P2 85.5 . . ? P1 Ru1 P2 157.12(7) . . ? H23J Ru1 C236 14.2 . . ? Si1 Ru1 C236 97.83(16) . . ? Si2 Ru1 C236 157.18(15) . . ? H11J Ru1 C236 78.1 . . ? P1 Ru1 C236 104.81(14) . . ? P2 Ru1 C236 59.84(14) . . ? H23J Ru1 C116 71.2 . . ? Si1 Ru1 C116 154.86(16) . . ? Si2 Ru1 C116 105.68(15) . . ? H11J Ru1 C116 14.6 . . ? P1 Ru1 C116 60.36(15) . . ? P2 Ru1 C116 98.27(15) . . ? C236 Ru1 C116 78.7(2) . . ? C114 P1 C131 105.4(3) . . ? C114 P1 C122 103.6(3) . . ? C131 P1 C122 101.8(3) . . ? C114 P1 Ru1 97.7(2) . . ? C131 P1 Ru1 118.0(3) . . ? C122 P1 Ru1 127.3(2) . . ? C224 P2 C233 102.9(3) . . ? C224 P2 C214 101.0(3) . . ? C233 P2 C214 105.3(3) . . ? C224 P2 Ru1 131.6(3) . . ? C233 P2 Ru1 96.1(2) . . ? C214 P2 Ru1 116.3(3) . . ? C2A Si1 Cl3A 99.90(14) . . ? C2A Si1 Cl1 101.06(15) . . ? Cl3A Si1 Cl1 102.74(13) . . ? C2A Si1 Ru1 118.93(13) . . ? Cl3A Si1 Ru1 120.43(12) . . ? Cl1 Si1 Ru1 110.97(11) . . ? Si1 C2A H2A 109.5 . . ? Si1 C2A H2B 109.5 . . ? H2A C2A H2B 109.5 . . ? Si1 C2A H2C 109.5 . . ? H2A C2A H2C 109.5 . . ? H2B C2A H2C 109.5 . . ? C6A Si2 Cl5A 100.11(17) . . ? C6A Si2 Cl4 103.47(18) . . ? Cl5A Si2 Cl4 98.37(13) . . ? C6A Si2 Ru1 123.27(17) . . ? Cl5A Si2 Ru1 118.13(12) . . ? Cl4 Si2 Ru1 109.89(10) . . ? Si2 C6A H6A 109.5 . . ? Si2 C6A H6B 109.5 . . ? H6A C6A H6B 109.5 . . ? Si2 C6A H6C 109.5 . . ? H6A C6A H6C 109.5 . . ? H6B C6A H6C 109.5 . . ? # END of CIF # Attachment '- publiLSL221LV.cif' # CCDC deposition number: 765258 data_lsl221lv _database_code_depnum_ccdc_archive 'CCDC 765258' #TrackingRef '- publiLSL221LV.cif' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C27 H47 Cl4 P Ru Si2, 0.5(C7 H8 )' _chemical_formula_sum 'C30.50 H51 Cl4 P Ru Si2' _chemical_formula_weight 747.73 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.1180(8) _cell_length_b 11.3620(10) _cell_length_c 14.9910(9) _cell_angle_alpha 94.278(5) _cell_angle_beta 94.911(3) _cell_angle_gamma 92.777(6) _cell_volume 1709.7(2) _cell_formula_units_Z 2 _cell_measurement_temperature 160(2) _cell_measurement_reflns_used 5600 _cell_measurement_theta_min 2.1 _cell_measurement_theta_max 32.5 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.07 _exptl_crystal_density_diffrn 1.453 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 778 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.908 _exptl_absorpt_correction_type refdelf _exptl_absorpt_process_details ; (See: Walker, N. & Stuart, D. (1983) Acta Cryst. A39, 158-166) ; _exptl_absorpt_correction_T_min 0.533 _exptl_absorpt_correction_T_max 0.855 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 160(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford-Diffraction XCALIBUR' _diffrn_measurement_method \w-\f _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_av_R_equivalents 0.0311 _diffrn_reflns_av_unetI/netI 0.0187 _diffrn_reflns_number 23632 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.25 _diffrn_reflns_theta_max 25.02 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.936 _diffrn_measured_fraction_theta_max 0.936 _reflns_number_total 5653 _reflns_number_gt 5326 _reflns_threshold_expression >2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd.' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd.' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd.' _computing_structure_solution 'SIR92 (Giacovazzo et al, 1993)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^ > 2\s(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^)+(0.0463P)^2^+5.2083P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 5653 _refine_ls_number_parameters 371 _refine_ls_number_restraints 31 _refine_ls_R_factor_all 0.0409 _refine_ls_R_factor_gt 0.0391 _refine_ls_wR_factor_ref 0.0971 _refine_ls_wR_factor_gt 0.0954 _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_restrained_S_all 1.053 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.956 _refine_diff_density_min -3.062 _refine_diff_density_rms 0.094 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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' 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 C1 C 0.0474(3) 0.0429(3) 0.3629(2) 0.0250(8) Uani 1 1 d . . . C2 C 0.0418(3) 0.1654(3) 0.3620(2) 0.0255(8) Uani 1 1 d . . . H2 H -0.0334 0.1975 0.3323 0.031 Uiso 1 1 calc R . . C3 C 0.1462(4) 0.2428(3) 0.4046(2) 0.0256(8) Uani 1 1 d . . . H3 H 0.1403 0.3257 0.4026 0.031 Uiso 1 1 calc R . . C4 C 0.2585(4) 0.1984(3) 0.4497(2) 0.0238(8) Uani 1 1 d . . . H4 H 0.3263 0.2503 0.4809 0.029 Uiso 1 1 calc R . . C5 C 0.2679(4) 0.0741(3) 0.4475(2) 0.0244(8) Uani 1 1 d . . . H5 H 0.3447 0.0423 0.4753 0.029 Uiso 1 1 calc R . . C6 C 0.1649(4) -0.0023(3) 0.4045(2) 0.0248(8) Uani 1 1 d . . . H6 H 0.1732 -0.0854 0.4031 0.03 Uiso 1 1 calc R . . C13 C -0.0705(4) -0.0386(4) 0.3273(3) 0.0391(10) Uani 1 1 d . . . H13A H -0.1232 -0.057 0.3769 0.059 Uiso 1 1 calc R . . H13B H -0.0394 -0.1118 0.2996 0.059 Uiso 1 1 calc R . . H13C H -0.1256 0.0001 0.2824 0.059 Uiso 1 1 calc R . . C111 C 0.3301(3) 0.2521(3) 0.0929(2) 0.0163(7) Uani 1 1 d . . . H111 H 0.4047 0.1983 0.1013 0.02 Uiso 1 1 calc R . . C112 C 0.3902(4) 0.3632(3) 0.0542(2) 0.0223(7) Uani 1 1 d . . . H11D H 0.319 0.4174 0.0397 0.027 Uiso 1 1 calc R . . H11E H 0.4559 0.4054 0.0997 0.027 Uiso 1 1 calc R . . C113 C 0.4580(4) 0.3284(3) -0.0308(2) 0.0268(8) Uani 1 1 d . . . H11F H 0.4939 0.4007 -0.0553 0.032 Uiso 1 1 calc R . . H11G H 0.5336 0.2795 -0.015 0.032 Uiso 1 1 calc R . . C114 C 0.3634(4) 0.2599(3) -0.1025(2) 0.0264(8) Uani 1 1 d . . . H11H H 0.4123 0.2344 -0.1544 0.032 Uiso 1 1 calc R . . H11I H 0.2929 0.3113 -0.1237 0.032 Uiso 1 1 calc R . . C115 C 0.3008(3) 0.1519(3) -0.0643(2) 0.0238(8) Uani 1 1 d . . . H11J H 0.3707 0.097 -0.0485 0.029 Uiso 1 1 calc R . . H11K H 0.2358 0.1099 -0.1104 0.029 Uiso 1 1 calc R . . C116 C 0.2307(3) 0.1881(3) 0.0195(2) 0.0190(7) Uani 1 1 d . . . H11L H 0.19 0.1169 0.0428 0.023 Uiso 1 1 calc R . . H11M H 0.159 0.241 0.0034 0.023 Uiso 1 1 calc R . . C121 C 0.0957(3) 0.3416(3) 0.1877(2) 0.0187(7) Uani 1 1 d . . . H121 H 0.0717 0.367 0.2493 0.022 Uiso 1 1 calc R . . C122 C 0.0936(3) 0.4545(3) 0.1366(2) 0.0227(7) Uani 1 1 d . . . H12A H 0.165 0.512 0.164 0.027 Uiso 1 1 calc R . . H12B H 0.1108 0.4346 0.0733 0.027 Uiso 1 1 calc R . . C123 C -0.0410(4) 0.5104(3) 0.1395(3) 0.0298(8) Uani 1 1 d . . . H12C H -0.0537 0.5377 0.2023 0.036 Uiso 1 1 calc R . . H12D H -0.0417 0.5802 0.1037 0.036 Uiso 1 1 calc R . . C124 C -0.1556(4) 0.4229(4) 0.1025(3) 0.0315(9) Uani 1 1 d . . . H12E H -0.241 0.4598 0.1098 0.038 Uiso 1 1 calc R . . H12F H -0.1494 0.4036 0.0376 0.038 Uiso 1 1 calc R . . C125 C -0.1525(3) 0.3097(3) 0.1509(3) 0.0269(8) Uani 1 1 d . . . H12G H -0.2235 0.2525 0.1226 0.032 Uiso 1 1 calc R . . H12H H -0.17 0.3275 0.2144 0.032 Uiso 1 1 calc R . . C126 C -0.0180(3) 0.2543(3) 0.1475(2) 0.0196(7) Uani 1 1 d . . . H12I H -0.0039 0.23 0.0843 0.024 Uiso 1 1 calc R . . H12J H -0.0178 0.1827 0.1813 0.024 Uiso 1 1 calc R . . C131 C 0.3680(3) 0.4069(3) 0.2550(2) 0.0159(6) Uani 1 1 d . . . H131 H 0.3587 0.4667 0.2095 0.019 Uiso 1 1 calc R . . C132 C 0.5166(3) 0.3850(3) 0.2665(2) 0.0196(7) Uani 1 1 d . . . H13D H 0.5348 0.3354 0.3172 0.023 Uiso 1 1 calc R . . H13E H 0.5429 0.3422 0.2113 0.023 Uiso 1 1 calc R . . C133 C 0.5975(3) 0.5025(3) 0.2845(2) 0.0239(7) Uani 1 1 d . . . H13F H 0.6933 0.4877 0.291 0.029 Uiso 1 1 calc R . . H13G H 0.5813 0.5509 0.2328 0.029 Uiso 1 1 calc R . . C134 C 0.5601(4) 0.5700(3) 0.3694(2) 0.0284(8) Uani 1 1 d . . . H13H H 0.6085 0.6484 0.3772 0.034 Uiso 1 1 calc R . . H13I H 0.5868 0.5262 0.4221 0.034 Uiso 1 1 calc R . . C135 C 0.4110(4) 0.5860(3) 0.3646(3) 0.0304(9) Uani 1 1 d . . . H13J H 0.3874 0.6405 0.3179 0.036 Uiso 1 1 calc R . . H13K H 0.3884 0.6229 0.4229 0.036 Uiso 1 1 calc R . . C136 C 0.3281(4) 0.4685(3) 0.3427(2) 0.0251(8) Uani 1 1 d . . . H13L H 0.3434 0.4166 0.3924 0.03 Uiso 1 1 calc R . . H13M H 0.2324 0.4838 0.3362 0.03 Uiso 1 1 calc R . . C101 C -0.0329(7) 0.4334(8) 0.5222(5) 0.0257(17) Uani 0.5 1 d PD A -1 C102 C -0.091(3) 0.475(2) 0.4447(18) 0.040(5) Uani 0.5 1 d PD A -1 H102 H -0.165 0.4315 0.413 0.048 Uiso 0.5 1 calc PR A -1 C103 C -0.0425(11) 0.5770(10) 0.4124(6) 0.047(3) Uani 0.5 1 d PD A -1 H103 H -0.0869 0.6067 0.361 0.057 Uiso 0.5 1 calc PR A -1 C104 C 0.0702(14) 0.6360(12) 0.4548(9) 0.053(5) Uani 0.5 1 d PD A -1 H104 H 0.1063 0.7045 0.431 0.064 Uiso 0.5 1 calc PR A -1 C105 C 0.1308(9) 0.5960(10) 0.5319(7) 0.046(3) Uani 0.5 1 d PD A -1 H105 H 0.2059 0.6387 0.5631 0.056 Uiso 0.5 1 calc PR A -1 C106 C 0.081(2) 0.493(2) 0.5632(18) 0.031(4) Uani 0.5 1 d PD A -1 H106 H 0.1257 0.4621 0.6139 0.037 Uiso 0.5 1 calc PR A -1 C107 C -0.0869(14) 0.3214(13) 0.5560(9) 0.040(3) Uani 0.5 1 d PD A -1 H10A H -0.0193 0.2625 0.5552 0.06 Uiso 0.5 1 calc PR A -1 H10B H -0.166 0.291 0.5173 0.06 Uiso 0.5 1 calc PR A -1 H10C H -0.1106 0.3375 0.6176 0.06 Uiso 0.5 1 calc PR A -1 Ru1 Ru 0.24427(2) 0.11633(2) 0.303612(16) 0.01396(10) Uani 1 1 d . B . P1 P 0.26193(8) 0.27406(7) 0.20593(5) 0.01354(18) Uani 1 1 d . . . Cl1 Cl 0.58607(8) 0.16052(8) 0.42239(6) 0.0257(2) Uani 1 1 d . B . Cl5 Cl 0.19449(10) -0.20943(8) 0.24026(7) 0.0336(2) Uani 1 1 d . B . Si1 Si 0.46694(8) 0.06740(8) 0.30994(6) 0.01634(19) Uani 1 1 d . . . Cl2A Cl 0.59285(9) 0.09443(8) 0.20886(6) 0.0250(2) Uani 0.9 1 d P B 1 C98A C 0.5053(3) -0.0936(2) 0.33715(19) 0.0250(2) Uani 0.9 1 d P B 1 H98A H 0.473 -0.1488 0.2857 0.037 Uiso 0.9 1 calc PR B 1 H98B H 0.4608 -0.1139 0.3899 0.037 Uiso 0.9 1 calc PR B 1 H98C H 0.6015 -0.0989 0.3495 0.037 Uiso 0.9 1 calc PR B 1 Cl2B Cl 0.5053(3) -0.0936(2) 0.33715(19) 0.0250(2) Uani 0.1 1 d P B 2 C98B C 0.59285(9) 0.09443(8) 0.20886(6) 0.0250(2) Uani 0.1 1 d P B 2 H98D H 0.6774 0.0585 0.2235 0.037 Uiso 0.1 1 d P C 2 H98E H 0.609 0.1794 0.2045 0.037 Uiso 0.1 1 d P D 2 H98F H 0.551 0.0579 0.1514 0.037 Uiso 0.1 1 d P E 2 Si2 Si 0.21496(9) -0.03900(8) 0.18844(6) 0.0178(2) Uani 1 1 d . . . Cl3A Cl 0.03119(9) -0.04684(9) 0.11129(6) 0.0236(2) Uani 0.8 1 d P B 1 C99A C 0.3344(2) -0.07597(19) 0.09814(14) 0.0236(2) Uani 0.8 1 d P B 1 H99A H 0.2921 -0.1372 0.054 0.035 Uiso 0.8 1 d P F 1 H99B H 0.4163 -0.105 0.1266 0.035 Uiso 0.8 1 d P G 1 H99C H 0.356 -0.0048 0.0681 0.035 Uiso 0.8 1 d P H 1 Cl3B Cl 0.3344(2) -0.07597(19) 0.09814(14) 0.0236(2) Uani 0.2 1 d P B 2 C99B C 0.03119(9) -0.04684(9) 0.11129(6) 0.0236(2) Uani 0.2 1 d P B 2 H99D H 0.0261 0.0222 0.076 0.035 Uiso 0.2 1 d P I 2 H99E H -0.0407 -0.0473 0.1511 0.035 Uiso 0.2 1 d P J 2 H99F H 0.0225 -0.1191 0.0707 0.035 Uiso 0.2 1 d P K 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 C1 0.0208(17) 0.034(2) 0.0216(17) 0.0065(15) 0.0083(14) -0.0004(15) C2 0.0222(17) 0.037(2) 0.0196(17) 0.0079(16) 0.0086(14) 0.0094(16) C3 0.035(2) 0.0243(18) 0.0186(17) -0.0017(14) 0.0118(15) 0.0038(16) C4 0.0290(18) 0.0286(19) 0.0138(16) -0.0008(14) 0.0045(14) -0.0001(15) C5 0.0278(18) 0.033(2) 0.0135(16) 0.0085(15) 0.0032(13) 0.0035(16) C6 0.0316(19) 0.0240(18) 0.0212(17) 0.0114(15) 0.0084(14) 0.0003(15) C13 0.026(2) 0.047(3) 0.045(2) 0.008(2) 0.0073(17) -0.0074(18) C111 0.0164(15) 0.0168(16) 0.0162(15) 0.0019(13) 0.0035(12) 0.0001(13) C112 0.0297(18) 0.0191(17) 0.0183(16) 0.0019(14) 0.0053(14) -0.0025(14) C113 0.0321(19) 0.0262(19) 0.0240(18) 0.0045(15) 0.0128(15) -0.0026(16) C114 0.0317(19) 0.032(2) 0.0175(17) 0.0031(15) 0.0093(14) 0.0063(16) C115 0.0236(17) 0.0282(19) 0.0185(17) -0.0047(14) 0.0035(14) -0.0016(15) C116 0.0159(15) 0.0236(17) 0.0173(16) -0.0005(13) 0.0024(13) -0.0007(13) C121 0.0198(16) 0.0189(16) 0.0181(16) 0.0035(13) 0.0015(13) 0.0046(13) C122 0.0209(17) 0.0195(17) 0.0284(18) 0.0086(15) -0.0001(14) 0.0032(14) C123 0.0299(19) 0.0274(19) 0.035(2) 0.0109(17) 0.0018(16) 0.0142(16) C124 0.0204(17) 0.037(2) 0.039(2) 0.0137(18) 0.0028(16) 0.0103(16) C125 0.0155(16) 0.035(2) 0.032(2) 0.0112(17) 0.0057(14) 0.0044(15) C126 0.0165(15) 0.0210(17) 0.0214(17) 0.0053(14) -0.0004(13) 0.0011(13) C131 0.0182(15) 0.0125(15) 0.0165(15) -0.0004(13) 0.0012(12) -0.0001(12) C132 0.0188(16) 0.0186(16) 0.0207(16) 0.0008(13) -0.0019(13) 0.0023(13) C133 0.0202(17) 0.0243(18) 0.0258(18) -0.0004(15) -0.0023(14) -0.0019(14) C134 0.0309(19) 0.0244(19) 0.0270(19) -0.0054(15) -0.0040(15) -0.0053(15) C135 0.033(2) 0.0202(18) 0.036(2) -0.0126(16) 0.0010(16) -0.0003(15) C136 0.0265(18) 0.0236(18) 0.0239(18) -0.0074(15) 0.0025(14) 0.0028(15) C101 0.020(4) 0.028(5) 0.029(5) -0.003(4) 0.007(4) 0.005(4) C102 0.040(10) 0.037(15) 0.039(10) -0.010(8) -0.016(8) 0.018(7) C103 0.073(8) 0.045(6) 0.029(5) 0.012(5) 0.012(5) 0.025(6) C104 0.070(11) 0.026(9) 0.075(10) 0.015(7) 0.056(9) 0.006(7) C105 0.031(5) 0.034(6) 0.074(8) -0.010(5) 0.020(5) -0.003(4) C106 0.032(7) 0.032(13) 0.028(7) -0.003(6) -0.004(6) 0.013(7) C107 0.034(5) 0.037(9) 0.051(7) 0.004(6) 0.024(5) -0.008(5) Ru1 0.01471(14) 0.01449(15) 0.01277(15) 0.00224(10) 0.00037(10) 0.00136(10) P1 0.0143(4) 0.0132(4) 0.0130(4) 0.0011(3) 0.0004(3) 0.0013(3) Cl1 0.0273(4) 0.0248(4) 0.0226(4) 0.0027(3) -0.0097(3) -0.0034(3) Cl5 0.0398(5) 0.0182(4) 0.0411(5) 0.0059(4) -0.0066(4) -0.0021(4) Si1 0.0162(4) 0.0157(4) 0.0165(4) 0.0012(3) -0.0018(3) 0.0016(3) Cl2A 0.0212(4) 0.0251(4) 0.0293(5) 0.0035(4) 0.0045(3) 0.0031(3) C98A 0.0212(4) 0.0251(4) 0.0293(5) 0.0035(4) 0.0045(3) 0.0031(3) Cl2B 0.0212(4) 0.0251(4) 0.0293(5) 0.0035(4) 0.0045(3) 0.0031(3) C98B 0.0212(4) 0.0251(4) 0.0293(5) 0.0035(4) 0.0045(3) 0.0031(3) Si2 0.0178(4) 0.0155(4) 0.0192(4) -0.0001(4) -0.0026(3) -0.0001(3) Cl3A 0.0198(4) 0.0260(5) 0.0230(4) 0.0003(4) -0.0068(3) -0.0027(4) C99A 0.0198(4) 0.0260(5) 0.0230(4) 0.0003(4) -0.0068(3) -0.0027(4) Cl3B 0.0198(4) 0.0260(5) 0.0230(4) 0.0003(4) -0.0068(3) -0.0027(4) C99B 0.0198(4) 0.0260(5) 0.0230(4) 0.0003(4) -0.0068(3) -0.0027(4) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 C1 C2 1.397(5) . ? C1 C6 1.431(5) . ? C1 C13 1.508(5) . ? C1 Ru1 2.389(3) . ? C2 C3 1.416(5) . ? C2 Ru1 2.371(3) . ? C2 H2 0.95 . ? C3 C4 1.407(5) . ? C3 Ru1 2.326(3) . ? C3 H3 0.95 . ? C4 C5 1.418(5) . ? C4 Ru1 2.306(3) . ? C4 H4 0.95 . ? C5 C6 1.404(5) . ? C5 Ru1 2.240(3) . ? C5 H5 0.95 . ? C6 Ru1 2.271(3) . ? C6 H6 0.95 . ? C13 H13A 0.98 . ? C13 H13B 0.98 . ? C13 H13C 0.98 . ? C111 C116 1.539(4) . ? C111 C112 1.547(4) . ? C111 P1 1.888(3) . ? C111 H111 1 . ? C112 C113 1.534(4) . ? C112 H11D 0.99 . ? C112 H11E 0.99 . ? C113 C114 1.518(5) . ? C113 H11F 0.99 . ? C113 H11G 0.99 . ? C114 C115 1.525(5) . ? C114 H11H 0.99 . ? C114 H11I 0.99 . ? C115 C116 1.534(4) . ? C115 H11J 0.99 . ? C115 H11K 0.99 . ? C116 H11L 0.99 . ? C116 H11M 0.99 . ? C121 C126 1.534(4) . ? C121 C122 1.543(5) . ? C121 P1 1.889(3) . ? C121 H121 1 . ? C122 C123 1.534(5) . ? C122 H12A 0.99 . ? C122 H12B 0.99 . ? C123 C124 1.528(5) . ? C123 H12C 0.99 . ? C123 H12D 0.99 . ? C124 C125 1.524(5) . ? C124 H12E 0.99 . ? C124 H12F 0.99 . ? C125 C126 1.531(5) . ? C125 H12G 0.99 . ? C125 H12H 0.99 . ? C126 H12I 0.99 . ? C126 H12J 0.99 . ? C131 C132 1.534(4) . ? C131 C136 1.536(4) . ? C131 P1 1.874(3) . ? C131 H131 1 . ? C132 C133 1.526(4) . ? C132 H13D 0.99 . ? C132 H13E 0.99 . ? C133 C134 1.522(5) . ? C133 H13F 0.99 . ? C133 H13G 0.99 . ? C134 C135 1.525(5) . ? C134 H13H 0.99 . ? C134 H13I 0.99 . ? C135 C136 1.541(5) . ? C135 H13J 0.99 . ? C135 H13K 0.99 . ? C136 H13L 0.99 . ? C136 H13M 0.99 . ? C101 C106 1.376(11) . ? C101 C102 1.379(11) . ? C101 C107 1.500(13) . ? C102 C103 1.376(12) . ? C102 H102 0.95 . ? C103 C104 1.376(12) . ? C103 H103 0.95 . ? C104 C105 1.379(12) . ? C104 H104 0.95 . ? C105 C106 1.387(12) . ? C105 H105 0.95 . ? C106 H106 0.95 . ? C107 H10A 0.98 . ? C107 H10B 0.98 . ? C107 H10C 0.98 . ? Ru1 Si1 2.3423(9) . ? Ru1 Si2 2.3645(9) . ? Ru1 P1 2.4069(9) . ? Cl1 Si1 2.1625(12) . ? Cl5 Si2 2.1469(13) . ? Si1 C98A 1.954(3) . ? Si1 Cl2A 2.0918(12) . ? Cl2A H98D 0.9799 . ? Cl2A H98E 0.9793 . ? Cl2A H98F 0.9795 . ? C98A H98A 0.98 . ? C98A H98B 0.98 . ? C98A H98C 0.98 . ? Si2 C99A 1.927(2) . ? Si2 Cl3A 2.0984(13) . ? Cl3A H99D 0.9799 . ? Cl3A H99E 0.9795 . ? Cl3A H99F 0.9801 . ? C99A H99A 0.9796 . ? C99A H99B 0.9814 . ? C99A H99C 0.979 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 C6 117.8(3) . . ? C2 C1 C13 121.0(3) . . ? C6 C1 C13 121.0(3) . . ? C2 C1 Ru1 72.22(19) . . ? C6 C1 Ru1 67.69(18) . . ? C13 C1 Ru1 135.4(3) . . ? C1 C2 C3 121.2(3) . . ? C1 C2 Ru1 73.65(19) . . ? C3 C2 Ru1 70.73(19) . . ? C1 C2 H2 119.4 . . ? C3 C2 H2 119.4 . . ? Ru1 C2 H2 128.5 . . ? C4 C3 C2 120.9(3) . . ? C4 C3 Ru1 71.54(19) . . ? C2 C3 Ru1 74.18(19) . . ? C4 C3 H3 119.5 . . ? C2 C3 H3 119.5 . . ? Ru1 C3 H3 126.7 . . ? C3 C4 C5 118.3(3) . . ? C3 C4 Ru1 73.10(19) . . ? C5 C4 Ru1 69.32(19) . . ? C3 C4 H4 120.9 . . ? C5 C4 H4 120.9 . . ? Ru1 C4 H4 128.9 . . ? C6 C5 C4 120.6(3) . . ? C6 C5 Ru1 73.1(2) . . ? C4 C5 Ru1 74.4(2) . . ? C6 C5 H5 119.7 . . ? C4 C5 H5 119.7 . . ? Ru1 C5 H5 124.4 . . ? C5 C6 C1 121.0(3) . . ? C5 C6 Ru1 70.65(19) . . ? C1 C6 Ru1 76.7(2) . . ? C5 C6 H6 119.5 . . ? C1 C6 H6 119.5 . . ? Ru1 C6 H6 124.8 . . ? C1 C13 H13A 109.5 . . ? C1 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C1 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C116 C111 C112 107.9(3) . . ? C116 C111 P1 113.8(2) . . ? C112 C111 P1 116.9(2) . . ? C116 C111 H111 105.8 . . ? C112 C111 H111 105.8 . . ? P1 C111 H111 105.8 . . ? C113 C112 C111 110.5(3) . . ? C113 C112 H11D 109.6 . . ? C111 C112 H11D 109.6 . . ? C113 C112 H11E 109.6 . . ? C111 C112 H11E 109.6 . . ? H11D C112 H11E 108.1 . . ? C114 C113 C112 112.2(3) . . ? C114 C113 H11F 109.2 . . ? C112 C113 H11F 109.2 . . ? C114 C113 H11G 109.2 . . ? C112 C113 H11G 109.2 . . ? H11F C113 H11G 107.9 . . ? C113 C114 C115 109.9(3) . . ? C113 C114 H11H 109.7 . . ? C115 C114 H11H 109.7 . . ? C113 C114 H11I 109.7 . . ? C115 C114 H11I 109.7 . . ? H11H C114 H11I 108.2 . . ? C114 C115 C116 110.9(3) . . ? C114 C115 H11J 109.5 . . ? C116 C115 H11J 109.5 . . ? C114 C115 H11K 109.5 . . ? C116 C115 H11K 109.5 . . ? H11J C115 H11K 108 . . ? C115 C116 C111 110.6(3) . . ? C115 C116 H11L 109.5 . . ? C111 C116 H11L 109.5 . . ? C115 C116 H11M 109.5 . . ? C111 C116 H11M 109.5 . . ? H11L C116 H11M 108.1 . . ? C126 C121 C122 109.5(3) . . ? C126 C121 P1 114.5(2) . . ? C122 C121 P1 116.4(2) . . ? C126 C121 H121 105.1 . . ? C122 C121 H121 105.1 . . ? P1 C121 H121 105.1 . . ? C123 C122 C121 110.8(3) . . ? C123 C122 H12A 109.5 . . ? C121 C122 H12A 109.5 . . ? C123 C122 H12B 109.5 . . ? C121 C122 H12B 109.5 . . ? H12A C122 H12B 108.1 . . ? C124 C123 C122 111.6(3) . . ? C124 C123 H12C 109.3 . . ? C122 C123 H12C 109.3 . . ? C124 C123 H12D 109.3 . . ? C122 C123 H12D 109.3 . . ? H12C C123 H12D 108 . . ? C125 C124 C123 111.3(3) . . ? C125 C124 H12E 109.4 . . ? C123 C124 H12E 109.4 . . ? C125 C124 H12F 109.4 . . ? C123 C124 H12F 109.4 . . ? H12E C124 H12F 108 . . ? C124 C125 C126 111.2(3) . . ? C124 C125 H12G 109.4 . . ? C126 C125 H12G 109.4 . . ? C124 C125 H12H 109.4 . . ? C126 C125 H12H 109.4 . . ? H12G C125 H12H 108 . . ? C125 C126 C121 111.1(3) . . ? C125 C126 H12I 109.4 . . ? C121 C126 H12I 109.4 . . ? C125 C126 H12J 109.4 . . ? C121 C126 H12J 109.4 . . ? H12I C126 H12J 108 . . ? C132 C131 C136 108.8(3) . . ? C132 C131 P1 113.6(2) . . ? C136 C131 P1 116.9(2) . . ? C132 C131 H131 105.5 . . ? C136 C131 H131 105.5 . . ? P1 C131 H131 105.5 . . ? C133 C132 C131 109.9(3) . . ? C133 C132 H13D 109.7 . . ? C131 C132 H13D 109.7 . . ? C133 C132 H13E 109.7 . . ? C131 C132 H13E 109.7 . . ? H13D C132 H13E 108.2 . . ? C134 C133 C132 110.9(3) . . ? C134 C133 H13F 109.5 . . ? C132 C133 H13F 109.5 . . ? C134 C133 H13G 109.5 . . ? C132 C133 H13G 109.5 . . ? H13F C133 H13G 108 . . ? C133 C134 C135 110.9(3) . . ? C133 C134 H13H 109.5 . . ? C135 C134 H13H 109.5 . . ? C133 C134 H13I 109.5 . . ? C135 C134 H13I 109.5 . . ? H13H C134 H13I 108.1 . . ? C134 C135 C136 112.7(3) . . ? C134 C135 H13J 109.1 . . ? C136 C135 H13J 109.1 . . ? C134 C135 H13K 109.1 . . ? C136 C135 H13K 109.1 . . ? H13J C135 H13K 107.8 . . ? C131 C136 C135 109.6(3) . . ? C131 C136 H13L 109.8 . . ? C135 C136 H13L 109.8 . . ? C131 C136 H13M 109.8 . . ? C135 C136 H13M 109.8 . . ? H13L C136 H13M 108.2 . . ? C106 C101 C102 118.1(10) . . ? C106 C101 C107 121.4(9) . . ? C102 C101 C107 120.4(9) . . ? C103 C102 C101 121.4(13) . . ? C103 C102 H102 119.3 . . ? C101 C102 H102 119.3 . . ? C102 C103 C104 119.6(12) . . ? C102 C103 H103 120.2 . . ? C104 C103 H103 120.2 . . ? C103 C104 C105 120.1(10) . . ? C103 C104 H104 119.9 . . ? C105 C104 H104 119.9 . . ? C104 C105 C106 119.2(11) . . ? C104 C105 H105 120.4 . . ? C106 C105 H105 120.4 . . ? C101 C106 C105 121.4(12) . . ? C101 C106 H106 119.3 . . ? C105 C106 H106 119.3 . . ? C5 Ru1 C6 36.25(13) . . ? C5 Ru1 C4 36.31(13) . . ? C6 Ru1 C4 64.75(13) . . ? C5 Ru1 C3 64.12(14) . . ? C6 Ru1 C3 75.04(13) . . ? C4 Ru1 C3 35.36(13) . . ? C5 Ru1 Si1 81.85(10) . . ? C6 Ru1 Si1 100.89(10) . . ? C4 Ru1 Si1 94.50(9) . . ? C3 Ru1 Si1 127.36(10) . . ? C5 Ru1 Si2 119.69(10) . . ? C6 Ru1 Si2 91.46(9) . . ? C4 Ru1 Si2 155.45(10) . . ? C3 Ru1 Si2 147.58(9) . . ? Si1 Ru1 Si2 83.67(3) . . ? C5 Ru1 C2 74.96(13) . . ? C6 Ru1 C2 62.85(13) . . ? C4 Ru1 C2 63.34(12) . . ? C3 Ru1 C2 35.09(13) . . ? Si1 Ru1 C2 156.16(9) . . ? Si2 Ru1 C2 112.54(9) . . ? C5 Ru1 C1 64.32(13) . . ? C6 Ru1 C1 35.65(13) . . ? C4 Ru1 C1 75.12(12) . . ? C3 Ru1 C1 62.63(12) . . ? Si1 Ru1 C1 135.86(10) . . ? Si2 Ru1 C1 89.14(9) . . ? C2 Ru1 C1 34.13(13) . . ? C5 Ru1 P1 143.53(10) . . ? C6 Ru1 P1 160.92(10) . . ? C4 Ru1 P1 108.25(9) . . ? C3 Ru1 P1 89.37(9) . . ? Si1 Ru1 P1 97.30(3) . . ? Si2 Ru1 P1 96.25(3) . . ? C2 Ru1 P1 98.07(9) . . ? C1 Ru1 P1 126.80(10) . . ? C131 P1 C111 99.84(14) . . ? C131 P1 C121 100.48(14) . . ? C111 P1 C121 107.46(15) . . ? C131 P1 Ru1 114.94(11) . . ? C111 P1 Ru1 122.07(11) . . ? C121 P1 Ru1 109.63(10) . . ? C98A Si1 Cl2A 101.12(9) . . ? C98A Si1 Cl1 98.06(9) . . ? Cl2A Si1 Cl1 99.20(5) . . ? C98A Si1 Ru1 117.17(9) . . ? Cl2A Si1 Ru1 124.48(5) . . ? Cl1 Si1 Ru1 112.42(4) . . ? Si1 Cl2A H98D 109.4 . . ? Si1 Cl2A H98E 109.4 . . ? H98D Cl2A H98E 109.5 . . ? Si1 Cl2A H98F 109.4 . . ? H98D Cl2A H98F 109.5 . . ? H98E Cl2A H98F 109.6 . . ? Si1 C98A H98A 109.5 . . ? Si1 C98A H98B 109.5 . . ? Si1 C98A H98C 109.5 . . ? C99A Si2 Cl3A 101.68(8) . . ? C99A Si2 Cl5 99.11(8) . . ? Cl3A Si2 Cl5 97.33(5) . . ? C99A Si2 Ru1 126.79(7) . . ? Cl3A Si2 Ru1 114.75(5) . . ? Cl5 Si2 Ru1 112.40(5) . . ? Si2 Cl3A H99D 109.4 . . ? Si2 Cl3A H99E 109.5 . . ? H99D Cl3A H99E 109.5 . . ? Si2 Cl3A H99F 109.5 . . ? H99D Cl3A H99F 109.5 . . ? H99E Cl3A H99F 109.5 . . ? Si2 C99A H99A 109.5 . . ? Si2 C99A H99B 109.4 . . ? H99A C99A H99B 109.4 . . ? Si2 C99A H99C 109.5 . . ? H99A C99A H99C 109.6 . . ? H99B C99A H99C 109.4 . . ? # END of CIF