# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_test1 _database_code_depnum_ccdc_archive 'CCDC 903652' #TrackingRef 'compound 2.cif' _audit_creation_date 2012-12-11T14:19:09-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.4 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common compound2 _chemical_formula_sum 'C21 H18 O12 Ru4 Si2' _chemical_formula_weight 922.81 _chemical_absolute_configuration unk #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M P3121 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z+1/3' '-x+y, -x, z+2/3' 'x-y, -y, -z+2/3' '-x, -x+y, -z+1/3' 'y, x, -z' _cell_length_a 9.7557(14) _cell_length_b 9.7557(14) _cell_length_c 27.274(6) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_volume 2248.0(6) _cell_formula_units_Z 3 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 600 _cell_measurement_theta_min 1 _cell_measurement_theta_max 14 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour purple _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.03 _exptl_crystal_density_diffrn 2.045 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1332 _exptl_special_details ; Diffractometer operator Marco Background measurement : Moving crystal and moving counter at the beginning and end of scan, each for 25% of total scan area. Crystal mounted on a micromount. ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 2.112 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.6203 _exptl_absorpt_correction_T_max 0.9394 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 3 _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 -0.110527 _diffrn_orient_matrix_ub_12 -0.194331E-1 _diffrn_orient_matrix_ub_13 -0.27953E-2 _diffrn_orient_matrix_ub_21 0.41137E-2 _diffrn_orient_matrix_ub_22 0.328818E-1 _diffrn_orient_matrix_ub_23 0.349449E-1 _diffrn_orient_matrix_ub_31 0.421458E-1 _diffrn_orient_matrix_ub_32 0.11203 _diffrn_orient_matrix_ub_33 -0.107416E-1 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type 'Enraf-Nonius CCD' _diffrn_measurement_method \w _diffrn_standards_number 100 _diffrn_reflns_av_R_equivalents 0.0487 _diffrn_reflns_av_unetI/netI 0.072 _diffrn_reflns_number 7063 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 1.49 _diffrn_reflns_theta_max 27.69 _diffrn_reflns_theta_full 25 _diffrn_measured_fraction_theta_full 0.906 _diffrn_measured_fraction_theta_max 0.857 _reflns_number_total 2636 _reflns_number_gt 2077 _reflns_threshold_expression >2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'hkl2000 software (Enraf-Nonius, 2000)' _computing_cell_refinement 'hkl2000 software (Enraf-Nonius, 2000)' _computing_data_reduction 'WinGx (Ferrugia Louis, 2000)' _computing_structure_solution 'SHELXS-97(Sheldrick 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick 1997)' _computing_molecular_graphics 'WinGx (Ferrugia Louis, 2000)' _computing_publication_material 'SHELXL-97 (Sheldrick 1997)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Twin relation is 0.521(1) 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^)+(0.0075P)^2^+2.8735P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 2636 _refine_ls_number_parameters 181 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0666 _refine_ls_R_factor_gt 0.041 _refine_ls_wR_factor_ref 0.0639 _refine_ls_wR_factor_gt 0.0581 _refine_ls_goodness_of_fit_ref 1.05 _refine_ls_restrained_S_all 1.05 _refine_ls_shift/su_max 0.007 _refine_ls_shift/su_mean 0 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.33(11) _refine_diff_density_max 0.833 _refine_diff_density_min -0.609 _refine_diff_density_rms 0.147 #----------------------------------------------------------------------------# # 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' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 0.4173(10) 0.4430(10) 0.5475(3) 0.037(2) Uani 1 1 d . . . C2 C 0.4467(12) 0.4467(12) 0.5 0.041(3) Uani 1 2 d S . . C3 C 0.2329(10) 0.4548(12) 0.6374(4) 0.068(4) Uani 1 1 d . . . H3A H 0.2944 0.4327 0.6613 0.102 Uiso 1 1 calc R . . H3B H 0.126 0.4169 0.6502 0.102 Uiso 1 1 calc R . . H3C H 0.2847 0.5691 0.6316 0.102 Uiso 1 1 calc R . . C4 C 0.0756(10) 0.3619(12) 0.5375(4) 0.076(4) Uani 1 1 d . . . H4A H 0.108 0.4728 0.531 0.115 Uiso 1 1 calc R . . H4B H -0.0292 0.3092 0.5529 0.115 Uiso 1 1 calc R . . H4C H 0.0711 0.3086 0.5066 0.115 Uiso 1 1 calc R . . C5 C 0.1586(13) 0.1458(12) 0.5915(5) 0.083(4) Uani 1 1 d . . . H5A H 0.135 0.0874 0.5605 0.125 Uiso 1 1 calc R . . H5B H 0.0637 0.0993 0.6122 0.125 Uiso 1 1 calc R . . H5C H 0.2438 0.1396 0.6086 0.125 Uiso 1 1 calc R . . C11 C 0.8610(13) 0.5894(13) 0.5928(5) 0.065(3) Uani 1 1 d . . . C12 C 0.6194(13) 0.2942(15) 0.5683(5) 0.068(3) Uani 1 1 d . . . C13 C 0.5808(11) 0.4654(13) 0.6407(4) 0.058(3) Uani 1 1 d . . . C21 C 0.7203(14) 0.8984(13) 0.5034(5) 0.074(4) Uani 1 1 d . . . C22 C 0.4095(12) 0.7562(11) 0.5395(4) 0.052(3) Uani 1 1 d . . . C23 C 0.6649(11) 0.7652(12) 0.5909(4) 0.056(3) Uani 1 1 d . . . O11 O 0.9835(8) 0.6426(12) 0.6069(4) 0.109(4) Uani 1 1 d . . . O12 O 0.6034(10) 0.1706(9) 0.5656(4) 0.099(3) Uani 1 1 d . . . O13 O 0.5544(10) 0.4500(12) 0.6803(3) 0.102(3) Uani 1 1 d . . . O21 O 0.8169(10) 1.0208(10) 0.4910(4) 0.097(4) Uani 1 1 d . . . O22 O 0.3207(8) 0.7953(7) 0.5460(3) 0.073(2) Uani 1 1 d . . . O23 O 0.7214(11) 0.8355(10) 0.6258(4) 0.110(4) Uani 1 1 d . . . Si1 Si 0.2208(3) 0.3524(3) 0.57908(11) 0.0492(7) Uani 1 1 d . . . Ru1 Ru 0.63905(9) 0.49308(9) 0.57359(3) 0.0454(2) Uani 1 1 d . . . Ru2 Ru 0.56832(8) 0.70123(9) 0.52847(3) 0.03849(18) 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 C1 0.041(5) 0.032(5) 0.033(5) -0.008(4) -0.002(5) 0.014(4) C2 0.031(5) 0.031(5) 0.049(8) -0.003(4) 0.003(4) 0.006(6) C3 0.037(5) 0.083(9) 0.060(8) -0.002(7) 0.018(6) 0.013(5) C4 0.035(6) 0.096(8) 0.084(9) -0.011(7) -0.019(6) 0.021(5) C5 0.079(8) 0.052(7) 0.093(11) 0.000(8) 0.022(8) 0.013(6) C11 0.059(6) 0.075(8) 0.069(8) -0.001(7) -0.008(7) 0.040(6) C12 0.076(8) 0.075(8) 0.053(8) 0.001(7) -0.012(7) 0.037(7) C13 0.065(6) 0.070(7) 0.043(6) -0.004(6) 0.000(6) 0.037(6) C21 0.090(9) 0.048(7) 0.072(9) -0.014(7) 0.021(8) 0.026(7) C22 0.054(7) 0.036(6) 0.064(8) 0.002(5) 0.009(6) 0.021(5) C23 0.063(6) 0.052(6) 0.054(7) -0.013(6) -0.012(6) 0.029(5) O11 0.055(5) 0.146(8) 0.127(10) -0.011(7) -0.026(6) 0.051(5) O12 0.131(7) 0.053(5) 0.113(9) 0.014(6) -0.007(6) 0.047(5) O13 0.113(6) 0.171(9) 0.043(5) 0.024(6) 0.003(5) 0.088(7) O21 0.082(6) 0.038(5) 0.126(11) 0.006(5) 0.022(6) -0.003(4) O22 0.063(5) 0.077(5) 0.092(7) 0.000(4) 0.006(4) 0.046(4) O23 0.141(7) 0.106(7) 0.103(9) -0.062(6) -0.075(7) 0.076(6) Si1 0.0332(14) 0.0524(17) 0.0434(16) 0.0012(15) 0.0051(14) 0.0075(12) Ru1 0.0422(4) 0.0539(5) 0.0397(4) 0.0025(4) -0.0020(4) 0.0237(4) Ru2 0.0355(4) 0.0344(4) 0.0414(4) -0.0048(4) 0.0009(4) 0.0144(3) #----------------------------------------------------------------------------# # 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 1.325(9) . ? C1 Si1 1.871(9) . ? C1 Ru1 2.090(9) . ? C1 Ru2 2.253(9) . ? C2 C1 1.325(9) 6_556 ? C2 Ru2 2.287(10) . ? C2 Ru2 2.287(10) 6_556 ? C3 Si1 1.851(11) . ? C3 H3A 0.98 . ? C3 H3B 0.98 . ? C3 H3C 0.98 . ? C4 Si1 1.853(10) . ? C4 H4A 0.98 . ? C4 H4B 0.98 . ? C4 H4C 0.98 . ? C5 Si1 1.823(11) . ? C5 H5A 0.98 . ? C5 H5B 0.98 . ? C5 H5C 0.98 . ? C11 O11 1.107(11) . ? C11 Ru1 1.952(11) . ? C12 O12 1.139(13) . ? C12 Ru1 1.857(13) . ? C13 O13 1.103(14) . ? C13 Ru1 1.895(11) . ? C21 O21 1.142(13) . ? C21 Ru2 1.874(12) . ? C22 O22 1.122(11) . ? C22 Ru2 1.899(11) . ? C23 O23 1.139(13) . ? C23 Ru2 1.895(11) . ? C23 Ru1 2.582(11) . ? Ru1 Ru2 2.7414(12) . ? Ru1 Ru2 2.8652(13) 6_556 ? Ru2 Ru2 2.7304(16) 6_556 ? Ru2 Ru1 2.8652(13) 6_556 ? 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 Si1 128.3(8) . . ? C2 C1 Ru1 98.1(6) . . ? Si1 C1 Ru1 130.6(5) . . ? C2 C1 Ru2 74.4(7) . . ? Si1 C1 Ru2 125.2(5) . . ? Ru1 C1 Ru2 78.2(3) . . ? C1 C2 C1 166.0(14) . 6_556 ? C1 C2 Ru2 71.7(5) . . ? C1 C2 Ru2 120.7(7) 6_556 . ? C1 C2 Ru2 120.7(7) . 6_556 ? C1 C2 Ru2 71.7(5) 6_556 6_556 ? Ru2 C2 Ru2 73.3(4) . 6_556 ? Si1 C3 H3A 109.5 . . ? Si1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? Si1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? Si1 C4 H4A 109.5 . . ? Si1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? Si1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? Si1 C5 H5A 109.5 . . ? Si1 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? Si1 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? O11 C11 Ru1 175.1(13) . . ? O12 C12 Ru1 178.2(12) . . ? O13 C13 Ru1 176.2(10) . . ? O21 C21 Ru2 175.8(12) . . ? O22 C22 Ru2 177.0(9) . . ? O23 C23 Ru2 163.6(11) . . ? O23 C23 Ru1 122.7(9) . . ? Ru2 C23 Ru1 73.7(3) . . ? C5 Si1 C3 109.5(6) . . ? C5 Si1 C4 109.2(5) . . ? C3 Si1 C4 110.1(5) . . ? C5 Si1 C1 107.7(5) . . ? C3 Si1 C1 111.5(4) . . ? C4 Si1 C1 108.9(5) . . ? C12 Ru1 C13 93.4(5) . . ? C12 Ru1 C11 91.9(4) . . ? C13 Ru1 C11 89.5(5) . . ? C12 Ru1 C1 100.1(4) . . ? C13 Ru1 C1 95.3(4) . . ? C11 Ru1 C1 166.7(4) . . ? C12 Ru1 C23 173.9(5) . . ? C13 Ru1 C23 80.6(4) . . ? C11 Ru1 C23 86.6(4) . . ? C1 Ru1 C23 82.0(3) . . ? C12 Ru1 Ru2 143.7(4) . . ? C13 Ru1 Ru2 111.7(3) . . ? C11 Ru1 Ru2 113.1(3) . . ? C1 Ru1 Ru2 53.6(2) . . ? C23 Ru1 Ru2 41.6(2) . . ? C12 Ru1 Ru2 95.2(4) . 6_556 ? C13 Ru1 Ru2 169.9(3) . 6_556 ? C11 Ru1 Ru2 95.4(4) . 6_556 ? C1 Ru1 Ru2 78.0(3) . 6_556 ? C23 Ru1 Ru2 90.9(3) . 6_556 ? Ru2 Ru1 Ru2 58.24(3) . 6_556 ? C21 Ru2 C23 89.0(5) . . ? C21 Ru2 C22 96.1(4) . . ? C23 Ru2 C22 96.1(5) . . ? C21 Ru2 C1 166.2(4) . . ? C23 Ru2 C1 95.8(4) . . ? C22 Ru2 C1 96.3(3) . . ? C21 Ru2 C2 134.8(4) . . ? C23 Ru2 C2 124.4(3) . . ? C22 Ru2 C2 107.9(3) . . ? C1 Ru2 C2 33.9(3) . . ? C21 Ru2 Ru2 87.7(3) . 6_556 ? C23 Ru2 Ru2 113.1(3) . 6_556 ? C22 Ru2 Ru2 150.7(3) . 6_556 ? C1 Ru2 Ru2 78.5(2) . 6_556 ? C2 Ru2 Ru2 53.35(18) . 6_556 ? C21 Ru2 Ru1 124.1(4) . . ? C23 Ru2 Ru1 64.7(3) . . ? C22 Ru2 Ru1 132.9(3) . . ? C1 Ru2 Ru1 48.3(2) . . ? C2 Ru2 Ru1 62.24(5) . . ? Ru2 Ru2 Ru1 63.15(4) 6_556 . ? C21 Ru2 Ru1 81.4(4) . 6_556 ? C23 Ru2 Ru1 167.3(3) . 6_556 ? C22 Ru2 Ru1 93.2(3) . 6_556 ? C1 Ru2 Ru1 91.9(2) . 6_556 ? C2 Ru2 Ru1 60.09(6) . 6_556 ? Ru2 Ru2 Ru1 58.61(3) 6_556 6_556 ? Ru1 Ru2 Ru1 114.33(3) . 6_556 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Si1 C1 C2 C1 -30.3(7) . . . 6_556 ? Ru1 C1 C2 C1 131.6(3) . . . 6_556 ? Ru2 C1 C2 C1 -153.19(18) . . . 6_556 ? Si1 C1 C2 Ru2 122.9(8) . . . . ? Ru1 C1 C2 Ru2 -75.2(3) . . . . ? Si1 C1 C2 Ru2 179.6(5) . . . 6_556 ? Ru1 C1 C2 Ru2 -18.6(7) . . . 6_556 ? Ru2 C1 C2 Ru2 56.7(5) . . . 6_556 ? C2 C1 Si1 C5 87.9(10) . . . . ? Ru1 C1 Si1 C5 -68.2(8) . . . . ? Ru2 C1 Si1 C5 -174.1(6) . . . . ? C2 C1 Si1 C3 -152.1(8) . . . . ? Ru1 C1 Si1 C3 51.9(7) . . . . ? Ru2 C1 Si1 C3 -54.0(7) . . . . ? C2 C1 Si1 C4 -30.4(10) . . . . ? Ru1 C1 Si1 C4 173.5(6) . . . . ? Ru2 C1 Si1 C4 67.6(7) . . . . ? O12 C12 Ru1 C13 5E1(4) . . . . ? O12 C12 Ru1 C11 14E1(4) . . . . ? O12 C12 Ru1 C1 -4E1(4) . . . . ? O12 C12 Ru1 C23 7E1(4) . . . . ? O12 C12 Ru1 Ru2 -8E1(4) . . . . ? O12 C12 Ru1 Ru2 -12E1(4) . . . 6_556 ? O13 C13 Ru1 C12 71(18) . . . . ? O13 C13 Ru1 C11 -21(18) . . . . ? O13 C13 Ru1 C1 172(18) . . . . ? O13 C13 Ru1 C23 -107(18) . . . . ? O13 C13 Ru1 Ru2 -135(18) . . . . ? O13 C13 Ru1 Ru2 -140(17) . . . 6_556 ? O11 C11 Ru1 C12 -94(13) . . . . ? O11 C11 Ru1 C13 -1(13) . . . . ? O11 C11 Ru1 C1 111(13) . . . . ? O11 C11 Ru1 C23 80(13) . . . . ? O11 C11 Ru1 Ru2 113(13) . . . . ? O11 C11 Ru1 Ru2 171(13) . . . 6_556 ? C2 C1 Ru1 C12 -80.3(8) . . . . ? Si1 C1 Ru1 C12 80.9(7) . . . . ? Ru2 C1 Ru1 C12 -152.4(4) . . . . ? C2 C1 Ru1 C13 -174.7(7) . . . . ? Si1 C1 Ru1 C13 -13.5(7) . . . . ? Ru2 C1 Ru1 C13 113.1(4) . . . . ? C2 C1 Ru1 C11 74(2) . . . . ? Si1 C1 Ru1 C11 -124.6(18) . . . . ? Ru2 C1 Ru1 C11 2(2) . . . . ? C2 C1 Ru1 C23 105.5(7) . . . . ? Si1 C1 Ru1 C23 -93.3(6) . . . . ? Ru2 C1 Ru1 C23 33.4(3) . . . . ? C2 C1 Ru1 Ru2 72.1(6) . . . . ? Si1 C1 Ru1 Ru2 -126.7(7) . . . . ? C2 C1 Ru1 Ru2 12.9(6) . . . 6_556 ? Si1 C1 Ru1 Ru2 174.1(6) . . . 6_556 ? Ru2 C1 Ru1 Ru2 -59.23(17) . . . 6_556 ? O23 C23 Ru1 C12 29(4) . . . . ? Ru2 C23 Ru1 C12 -152(4) . . . . ? O23 C23 Ru1 C13 42.6(11) . . . . ? Ru2 C23 Ru1 C13 -138.7(4) . . . . ? O23 C23 Ru1 C11 -47.5(12) . . . . ? Ru2 C23 Ru1 C11 131.3(5) . . . . ? O23 C23 Ru1 C1 139.4(12) . . . . ? Ru2 C23 Ru1 C1 -41.9(3) . . . . ? O23 C23 Ru1 Ru2 -178.7(13) . . . . ? O23 C23 Ru1 Ru2 -142.9(11) . . . 6_556 ? Ru2 C23 Ru1 Ru2 35.8(3) . . . 6_556 ? O21 C21 Ru2 C23 1(15) . . . . ? O21 C21 Ru2 C22 97(15) . . . . ? O21 C21 Ru2 C1 -109(14) . . . . ? O21 C21 Ru2 C2 -140(15) . . . . ? O21 C21 Ru2 Ru2 -112(15) . . . 6_556 ? O21 C21 Ru2 Ru1 -57(15) . . . . ? O21 C21 Ru2 Ru1 -171(15) . . . 6_556 ? O23 C23 Ru2 C21 47(4) . . . . ? Ru1 C23 Ru2 C21 -129.0(4) . . . . ? O23 C23 Ru2 C22 -49(4) . . . . ? Ru1 C23 Ru2 C22 135.0(3) . . . . ? O23 C23 Ru2 C1 -146(4) . . . . ? Ru1 C23 Ru2 C1 38.0(3) . . . . ? O23 C23 Ru2 C2 -165(4) . . . . ? Ru1 C23 Ru2 C2 18.4(4) . . . . ? O23 C23 Ru2 Ru2 134(4) . . . 6_556 ? Ru1 C23 Ru2 Ru2 -41.9(3) . . . 6_556 ? O23 C23 Ru2 Ru1 176(4) . . . . ? O23 C23 Ru2 Ru1 88(4) . . . 6_556 ? Ru1 C23 Ru2 Ru1 -88.6(15) . . . 6_556 ? O22 C22 Ru2 C21 -20(19) . . . . ? O22 C22 Ru2 C23 70(19) . . . . ? O22 C22 Ru2 C1 166(19) . . . . ? O22 C22 Ru2 C2 -161(19) . . . . ? O22 C22 Ru2 Ru2 -116(19) . . . 6_556 ? O22 C22 Ru2 Ru1 131(19) . . . . ? O22 C22 Ru2 Ru1 -102(19) . . . 6_556 ? C2 C1 Ru2 C21 -41(2) . . . . ? Si1 C1 Ru2 C21 -167.0(17) . . . . ? Ru1 C1 Ru2 C21 61.2(19) . . . . ? C2 C1 Ru2 C23 -150.3(5) . . . . ? Si1 C1 Ru2 C23 83.5(6) . . . . ? Ru1 C1 Ru2 C23 -48.3(4) . . . . ? C2 C1 Ru2 C22 112.9(6) . . . . ? Si1 C1 Ru2 C22 -13.3(6) . . . . ? Ru1 C1 Ru2 C22 -145.1(4) . . . . ? Si1 C1 Ru2 C2 -126.2(8) . . . . ? Ru1 C1 Ru2 C2 102.0(5) . . . . ? C2 C1 Ru2 Ru2 -37.9(4) . . . 6_556 ? Si1 C1 Ru2 Ru2 -164.1(6) . . . 6_556 ? Ru1 C1 Ru2 Ru2 64.14(19) . . . 6_556 ? C2 C1 Ru2 Ru1 -102.0(5) . . . . ? Si1 C1 Ru2 Ru1 131.7(7) . . . . ? C2 C1 Ru2 Ru1 19.5(4) . . . 6_556 ? Si1 C1 Ru2 Ru1 -106.7(5) . . . 6_556 ? Ru1 C1 Ru2 Ru1 121.6(2) . . . 6_556 ? C1 C2 Ru2 C21 167.3(7) . . . . ? C1 C2 Ru2 C21 -20.0(9) 6_556 . . . ? Ru2 C2 Ru2 C21 35.9(6) 6_556 . . . ? C1 C2 Ru2 C23 36.7(7) . . . . ? C1 C2 Ru2 C23 -150.6(7) 6_556 . . . ? Ru2 C2 Ru2 C23 -94.7(4) 6_556 . . . ? C1 C2 Ru2 C22 -74.1(6) . . . . ? C1 C2 Ru2 C22 98.6(7) 6_556 . . . ? Ru2 C2 Ru2 C22 154.5(3) 6_556 . . . ? C1 C2 Ru2 C1 172.7(8) 6_556 . . . ? Ru2 C2 Ru2 C1 -131.4(5) 6_556 . . . ? C1 C2 Ru2 Ru2 131.4(5) . . . 6_556 ? C1 C2 Ru2 Ru2 -55.9(6) 6_556 . . 6_556 ? C1 C2 Ru2 Ru1 55.6(4) . . . . ? C1 C2 Ru2 Ru1 -131.8(7) 6_556 . . . ? Ru2 C2 Ru2 Ru1 -75.85(10) 6_556 . . . ? C1 C2 Ru2 Ru1 -157.3(5) . . . 6_556 ? C1 C2 Ru2 Ru1 15.4(6) 6_556 . . 6_556 ? Ru2 C2 Ru2 Ru1 71.28(10) 6_556 . . 6_556 ? C12 Ru1 Ru2 C21 -115.0(7) . . . . ? C13 Ru1 Ru2 C21 114.4(5) . . . . ? C11 Ru1 Ru2 C21 15.1(6) . . . . ? C1 Ru1 Ru2 C21 -165.4(5) . . . . ? C23 Ru1 Ru2 C21 69.8(5) . . . . ? Ru2 Ru1 Ru2 C21 -66.6(4) 6_556 . . . ? C12 Ru1 Ru2 C23 175.1(7) . . . . ? C13 Ru1 Ru2 C23 44.5(5) . . . . ? C11 Ru1 Ru2 C23 -54.7(5) . . . . ? C1 Ru1 Ru2 C23 124.8(4) . . . . ? Ru2 Ru1 Ru2 C23 -136.5(3) 6_556 . . . ? C12 Ru1 Ru2 C22 101.4(8) . . . . ? C13 Ru1 Ru2 C22 -29.2(5) . . . . ? C11 Ru1 Ru2 C22 -128.5(6) . . . . ? C1 Ru1 Ru2 C22 51.0(5) . . . . ? C23 Ru1 Ru2 C22 -73.8(6) . . . . ? Ru2 Ru1 Ru2 C22 149.8(4) 6_556 . . . ? C12 Ru1 Ru2 C1 50.4(7) . . . . ? C13 Ru1 Ru2 C1 -80.2(4) . . . . ? C11 Ru1 Ru2 C1 -179.5(5) . . . . ? C23 Ru1 Ru2 C1 -124.8(4) . . . . ? Ru2 Ru1 Ru2 C1 98.8(3) 6_556 . . . ? C12 Ru1 Ru2 C2 12.3(6) . . . . ? C13 Ru1 Ru2 C2 -118.3(4) . . . . ? C11 Ru1 Ru2 C2 142.4(5) . . . . ? C1 Ru1 Ru2 C2 -38.1(4) . . . . ? C23 Ru1 Ru2 C2 -162.8(4) . . . . ? Ru2 Ru1 Ru2 C2 60.7(2) 6_556 . . . ? C12 Ru1 Ru2 Ru2 -48.4(6) . . . 6_556 ? C13 Ru1 Ru2 Ru2 -179.0(3) . . . 6_556 ? C11 Ru1 Ru2 Ru2 81.8(4) . . . 6_556 ? C1 Ru1 Ru2 Ru2 -98.8(3) . . . 6_556 ? C23 Ru1 Ru2 Ru2 136.5(3) . . . 6_556 ? C12 Ru1 Ru2 Ru1 -18.8(6) . . . 6_556 ? C13 Ru1 Ru2 Ru1 -149.4(3) . . . 6_556 ? C11 Ru1 Ru2 Ru1 111.4(4) . . . 6_556 ? C1 Ru1 Ru2 Ru1 -69.2(3) . . . 6_556 ? C23 Ru1 Ru2 Ru1 166.1(3) . . . 6_556 ? Ru2 Ru1 Ru2 Ru1 29.60(4) 6_556 . . 6_556 ? data_mrvian14a _database_code_depnum_ccdc_archive 'CCDC 903653' #TrackingRef 'compound 3.cif' _audit_creation_date 2012-12-11T12:55:18-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.4 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common compound3 _chemical_formula_moiety 'C36 H40 O12 Ru5 Si4' _chemical_formula_sum 'C33 H45 O12 Ru5 Si4' _chemical_formula_weight 1251.4 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c _symmetry_space_group_name_Hall '-C 2yc' _symmetry_Int_Tables_number 15 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 34.9630(4) _cell_length_b 14.3422(2) _cell_length_c 21.6132(3) _cell_angle_alpha 90 _cell_angle_beta 117.9340(10) _cell_angle_gamma 90 _cell_volume 9575.1(2) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 600 _cell_measurement_theta_min 1 _cell_measurement_theta_max 14 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 1.736 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4920 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.691 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.7014 _exptl_absorpt_correction_T_max 0.7709 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 9 _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 0.117411E-1 _diffrn_orient_matrix_ub_12 -0.636351E-1 _diffrn_orient_matrix_ub_13 0.176152E-1 _diffrn_orient_matrix_ub_21 0.280475E-1 _diffrn_orient_matrix_ub_22 0.178301E-1 _diffrn_orient_matrix_ub_23 0.14072E-2 _diffrn_orient_matrix_ub_31 0.111141E-1 _diffrn_orient_matrix_ub_32 0.222293E-1 _diffrn_orient_matrix_ub_33 0.492979E-1 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.0716 _diffrn_reflns_av_unetI/netI 0.0846 _diffrn_reflns_number 47689 _diffrn_reflns_limit_h_min -43 _diffrn_reflns_limit_h_max 44 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.06 _diffrn_reflns_theta_max 28.49 _diffrn_reflns_theta_full 25 _diffrn_measured_fraction_theta_full 0.966 _diffrn_measured_fraction_theta_max 0.845 _reflns_number_total 10245 _reflns_number_gt 6543 _reflns_threshold_expression >2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _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^)+(0.0548P)^2^+35.6028P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 10245 _refine_ls_number_parameters 500 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.1243 _refine_ls_R_factor_gt 0.0647 _refine_ls_wR_factor_ref 0.1402 _refine_ls_wR_factor_gt 0.1087 _refine_ls_goodness_of_fit_ref 1.074 _refine_ls_restrained_S_all 1.074 _refine_ls_shift/su_max 0.019 _refine_ls_shift/su_mean 0.001 _refine_diff_density_max 0.961 _refine_diff_density_min -1.334 _refine_diff_density_rms 0.161 #----------------------------------------------------------------------------# # 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' O O 0.0106 0.006 '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' Si Si 0.0817 0.0704 '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 0.39912(11) 0.5975(3) 0.5125(2) 0.0499(11) Uani 1 1 d . . . C2 C 0.38990(12) 0.6790(3) 0.4853(2) 0.0541(12) Uani 1 1 d . . . C3 C 0.30899(11) 0.4986(3) 0.4118(2) 0.0474(11) Uani 1 1 d . . . C4 C 0.28886(12) 0.5680(3) 0.3719(2) 0.0517(12) Uani 1 1 d . . . C5 C 0.39154(12) 0.3860(3) 0.5001(2) 0.0563(13) Uani 1 1 d . . . C6 C 0.39141(12) 0.3459(3) 0.5542(3) 0.0577(13) Uani 1 1 d . . . C7 C 0.4152(2) 0.7210(7) 0.3690(4) 0.175(4) Uani 1 1 d . . . H7A H 0.3886 0.705 0.3285 0.262 Uiso 1 1 calc R . . H7B H 0.4322 0.6657 0.3879 0.262 Uiso 1 1 calc R . . H7C H 0.431 0.7644 0.3559 0.262 Uiso 1 1 calc R . . C8 C 0.45358(19) 0.8368(6) 0.5006(4) 0.140(3) Uani 1 1 d . . . H8A H 0.4583 0.8904 0.4784 0.21 Uiso 1 1 calc R . . H8B H 0.4777 0.795 0.5151 0.21 Uiso 1 1 calc R . . H8C H 0.4508 0.8563 0.5407 0.21 Uiso 1 1 calc R . . C9 C 0.3586(2) 0.8642(6) 0.3988(5) 0.184(4) Uani 1 1 d . . . H9A H 0.3684 0.917 0.3828 0.276 Uiso 1 1 calc R . . H9B H 0.3508 0.8839 0.4338 0.276 Uiso 1 1 calc R . . H9C H 0.3339 0.837 0.3601 0.276 Uiso 1 1 calc R . . C15 C 0.3029(2) 0.6240(7) 0.2496(4) 0.196(4) Uani 1 1 d . . . H15A H 0.3113 0.5615 0.2454 0.294 Uiso 1 1 calc R . . H15C H 0.328 0.6585 0.2815 0.294 Uiso 1 1 calc R . . H15B H 0.2902 0.6536 0.2045 0.294 Uiso 1 1 calc R . . C16 C 0.2439(2) 0.7413(5) 0.2822(4) 0.144(3) Uani 1 1 d . . . H16C H 0.2659 0.7768 0.3195 0.216 Uiso 1 1 calc R . . H16A H 0.2186 0.7383 0.2887 0.216 Uiso 1 1 calc R . . H16B H 0.2367 0.7708 0.2382 0.216 Uiso 1 1 calc R . . C11 C 0.38800(15) 0.8172(3) 0.5872(3) 0.0751(17) Uani 1 1 d . . . C14 C 0.2174(3) 0.5463(6) 0.2261(4) 0.182(4) Uani 1 1 d . . . H14C H 0.2049 0.5679 0.1786 0.272 Uiso 1 1 calc R . . H14A H 0.196 0.5494 0.2422 0.272 Uiso 1 1 calc R . . H14B H 0.2269 0.4831 0.2285 0.272 Uiso 1 1 calc R . . C12 C 0.46281(15) 0.7036(4) 0.6443(3) 0.0744(17) Uani 1 1 d . . . C24 C 0.46928(19) 0.3762(8) 0.4776(4) 0.181(4) Uani 1 1 d . . . H24B H 0.4799 0.3819 0.4441 0.271 Uiso 1 1 calc R . . H24A H 0.48 0.3195 0.5037 0.271 Uiso 1 1 calc R . . H24C H 0.479 0.4284 0.509 0.271 Uiso 1 1 calc R . . C13 C 0.39937(14) 0.6772(4) 0.6821(3) 0.0719(16) Uani 1 1 d . . . C25 C 0.3899(2) 0.4670(5) 0.3683(4) 0.188(3) Uani 1 1 d . . . H25B H 0.3932 0.5253 0.3922 0.282 Uiso 1 1 calc R . . H25C H 0.3598 0.4571 0.3363 0.282 Uiso 1 1 calc R . . H25A H 0.4062 0.4685 0.343 0.282 Uiso 1 1 calc R . . C23 C 0.3927(3) 0.2573(6) 0.3928(4) 0.191(3) Uani 1 1 d . . . H23C H 0.3633 0.2593 0.3565 0.287 Uiso 1 1 calc R . . H23A H 0.3952 0.2141 0.4285 0.287 Uiso 1 1 calc R . . H23B H 0.4111 0.2375 0.3734 0.287 Uiso 1 1 calc R . . C17 C 0.4079(2) 0.2378(5) 0.6902(4) 0.149(3) Uani 1 1 d . . . H17B H 0.3795 0.2578 0.6806 0.224 Uiso 1 1 calc R . . H17A H 0.4291 0.28 0.7229 0.224 Uiso 1 1 calc R . . H17C H 0.4132 0.1762 0.7099 0.224 Uiso 1 1 calc R . . C19 C 0.46952(18) 0.2279(5) 0.6312(4) 0.147(3) Uani 1 1 d . . . H19A H 0.4794 0.1655 0.6464 0.22 Uiso 1 1 calc R . . H19C H 0.4858 0.2708 0.6685 0.22 Uiso 1 1 calc R . . H19B H 0.4735 0.2428 0.5913 0.22 Uiso 1 1 calc R . . C18 C 0.3805(3) 0.1389(5) 0.5515(5) 0.200(6) Uani 1 1 d . . . H18C H 0.3912 0.1232 0.5193 0.3 Uiso 1 1 calc R . . H18A H 0.3506 0.1566 0.5258 0.3 Uiso 1 1 calc R . . H18B H 0.3831 0.0858 0.5803 0.3 Uiso 1 1 calc R . . C21 C 0.31741(12) 0.5997(3) 0.5661(3) 0.0583(13) Uani 1 1 d . . . C22 C 0.30136(13) 0.7324(3) 0.4661(3) 0.0612(14) Uani 1 1 d . . . C31 C 0.46680(15) 0.4871(4) 0.6260(3) 0.0773(18) Uani 1 1 d . . . C32 C 0.40101(15) 0.4684(4) 0.6609(3) 0.0689(16) Uani 1 1 d . . . C41 C 0.23690(14) 0.4864(4) 0.5018(3) 0.0714(16) Uani 1 1 d . . . C42 C 0.21523(14) 0.4302(4) 0.3667(3) 0.0744(17) Uani 1 1 d . . . C43 C 0.21251(13) 0.6204(4) 0.3942(3) 0.0676(15) Uani 1 1 d . . . C51 C 0.31365(13) 0.3552(4) 0.5579(3) 0.0706(15) Uani 1 1 d . . . C52 C 0.30061(14) 0.2992(3) 0.4294(3) 0.0650(15) Uani 1 1 d . . . O11 O 0.37941(14) 0.8945(3) 0.5813(3) 0.1139(17) Uani 1 1 d . . . O12 O 0.49972(11) 0.7117(3) 0.6731(2) 0.1078(17) Uani 1 1 d . . . O13 O 0.39761(12) 0.6725(3) 0.7332(2) 0.1030(15) Uani 1 1 d . . . O21 O 0.30933(9) 0.5951(3) 0.61142(18) 0.0771(11) Uani 1 1 d . . . O22 O 0.28424(11) 0.8027(2) 0.4561(2) 0.0892(14) Uani 1 1 d . . . O31 O 0.50366(12) 0.4816(3) 0.6545(3) 0.127(2) Uani 1 1 d . . . O32 O 0.39641(14) 0.4575(3) 0.7091(2) 0.1096(15) Uani 1 1 d . . . O41 O 0.22544(11) 0.4680(3) 0.5409(2) 0.0989(13) Uani 1 1 d . . . O42 O 0.19291(13) 0.3765(3) 0.3276(3) 0.1170(19) Uani 1 1 d . . . O43 O 0.18805(11) 0.6777(3) 0.3732(2) 0.1030(15) Uani 1 1 d . . . O51 O 0.30407(12) 0.3271(3) 0.5974(2) 0.1119(14) Uani 1 1 d . . . O52 O 0.28526(13) 0.2353(3) 0.3955(2) 0.1003(15) Uani 1 1 d . . . Ru1 Ru 0.402402(10) 0.68728(3) 0.59655(2) 0.05306(10) Uani 1 1 d . . . Ru2 Ru 0.329533(9) 0.61539(2) 0.490006(18) 0.04388(9) Uani 1 1 d . . . H1AA H 0.3459 0.7098 0.5604 0.08 Uiso 1 1 d R . . Ru3 Ru 0.406768(10) 0.49590(2) 0.578596(19) 0.04931(10) Uani 1 1 d . . . Ru4 Ru 0.253532(10) 0.51882(3) 0.43084(2) 0.05166(10) Uani 1 1 d . . . Ru5 Ru 0.326031(9) 0.40302(2) 0.485974(18) 0.04592(9) Uani 1 1 d . . . H2AA H 0.2715 0.6261 0.4761 0.08 Uiso 1 1 d R . . Si1 Si 0.40294(5) 0.77604(13) 0.43734(10) 0.0908(6) Uani 1 1 d . . . Si2 Si 0.26420(5) 0.62111(11) 0.28240(8) 0.0735(5) Uani 1 1 d . . . Si3 Si 0.41206(5) 0.23663(10) 0.60715(9) 0.0785(5) Uani 1 1 d . . . Si4 Si 0.40929(4) 0.37374(11) 0.43122(8) 0.0768(4) Uani 1 1 d . . . C100 C 0.5209(3) 0.9648(9) 0.7560(5) 0.488(17) Uani 1 1 d D . . H10A H 0.5346 0.9173 0.7915 0.586 Uiso 1 1 calc R . . H10B H 0.5323 1.0236 0.7795 0.586 Uiso 1 1 calc R . . C101 C 0.5413(2) 0.9534(11) 0.7093(6) 0.427(18) Uani 1 1 d D . . H10C H 0.5346 0.889 0.6942 0.513 Uiso 1 1 calc R . . H10D H 0.5224 0.99 0.6686 0.513 Uiso 1 1 calc R . . C102 C 0.5844(3) 0.9664(11) 0.7117(9) 0.415(15) Uani 1 1 d D . . H10E H 0.5804 0.9925 0.6682 0.622 Uiso 1 1 calc R . . H10F H 0.5987 0.9072 0.7191 0.622 Uiso 1 1 calc R . . H10G H 0.6017 1.0078 0.7494 0.622 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 C1 0.0414(16) 0.063(2) 0.049(2) 0.000(2) 0.0243(15) -0.0012(17) C2 0.0534(18) 0.064(3) 0.049(2) 0.006(2) 0.0274(16) -0.0002(19) C3 0.0496(17) 0.062(2) 0.035(2) -0.0104(18) 0.0236(14) -0.0088(17) C4 0.0549(19) 0.059(2) 0.041(2) 0.002(2) 0.0227(16) -0.0009(19) C5 0.0550(19) 0.048(2) 0.069(3) 0.000(2) 0.0314(18) 0.0037(17) C6 0.0512(19) 0.052(2) 0.068(3) 0.011(2) 0.0260(18) 0.0036(18) C7 0.199(5) 0.240(10) 0.142(6) -0.013(6) 0.127(4) -0.058(7) C8 0.111(4) 0.163(7) 0.146(6) 0.008(5) 0.060(4) -0.049(4) C9 0.138(5) 0.182(7) 0.243(8) 0.134(6) 0.099(5) 0.048(5) C15 0.166(5) 0.337(11) 0.133(5) 0.137(6) 0.109(4) 0.113(6) C16 0.212(7) 0.130(5) 0.067(5) 0.044(4) 0.047(4) 0.070(5) C11 0.074(3) 0.062(3) 0.084(4) -0.010(3) 0.032(2) -0.017(2) C14 0.209(8) 0.192(8) 0.057(5) 0.005(5) -0.011(5) -0.101(6) C12 0.066(2) 0.080(3) 0.069(3) -0.012(3) 0.025(2) -0.013(2) C24 0.123(3) 0.302(12) 0.173(6) 0.043(7) 0.116(3) 0.043(6) C13 0.065(2) 0.087(3) 0.057(3) -0.010(3) 0.024(2) -0.014(2) C25 0.339(5) 0.183(6) 0.148(4) 0.112(4) 0.202(3) 0.165(5) C23 0.328(7) 0.129(6) 0.222(6) -0.090(5) 0.217(5) -0.077(6) C17 0.193(5) 0.152(6) 0.135(5) 0.096(4) 0.103(4) 0.060(5) C19 0.094(4) 0.150(5) 0.196(7) 0.098(5) 0.067(4) 0.062(4) C18 0.228(9) 0.063(4) 0.180(10) 0.014(5) -0.013(8) -0.018(5) C21 0.0472(18) 0.067(3) 0.061(3) -0.007(2) 0.0254(18) -0.0010(19) C22 0.060(2) 0.061(3) 0.057(3) -0.008(2) 0.022(2) -0.002(2) C31 0.054(2) 0.076(3) 0.085(4) 0.011(3) 0.018(2) -0.001(2) C32 0.075(3) 0.076(3) 0.049(3) 0.006(2) 0.023(2) -0.009(2) C41 0.051(2) 0.082(3) 0.084(3) 0.004(3) 0.034(2) -0.004(2) C42 0.061(2) 0.078(3) 0.071(4) 0.008(3) 0.020(2) -0.008(2) C43 0.054(2) 0.080(3) 0.069(3) -0.004(3) 0.0295(19) 0.003(2) C51 0.059(2) 0.078(3) 0.079(3) 0.010(3) 0.036(2) 0.003(2) C52 0.068(2) 0.062(3) 0.059(3) 0.004(2) 0.026(2) -0.002(2) O11 0.135(3) 0.064(2) 0.141(4) -0.008(2) 0.064(3) -0.006(2) O12 0.0580(19) 0.133(3) 0.108(3) -0.012(3) 0.018(2) -0.019(2) O13 0.116(2) 0.143(4) 0.059(2) -0.015(2) 0.0487(18) -0.025(2) O21 0.0726(14) 0.114(3) 0.0640(19) -0.0042(19) 0.0481(13) -0.0044(17) O22 0.091(2) 0.065(2) 0.095(3) -0.001(2) 0.0302(19) 0.0227(18) O31 0.053(2) 0.148(4) 0.147(4) 0.017(3) 0.019(2) 0.013(2) O32 0.160(3) 0.127(3) 0.058(2) 0.016(2) 0.065(2) -0.009(3) O41 0.0900(17) 0.122(3) 0.113(3) 0.014(2) 0.0716(17) -0.010(2) O42 0.099(3) 0.100(3) 0.113(4) -0.024(3) 0.018(3) -0.040(2) O43 0.0807(19) 0.104(3) 0.122(3) 0.021(2) 0.045(2) 0.041(2) O51 0.116(2) 0.145(4) 0.106(3) 0.048(2) 0.0783(18) 0.015(2) O52 0.122(3) 0.074(2) 0.088(3) -0.026(2) 0.035(2) -0.029(2) Ru1 0.05027(15) 0.0595(2) 0.0469(2) -0.00546(17) 0.02065(13) -0.00776(15) Ru2 0.04218(13) 0.05082(17) 0.03973(18) 0.00139(14) 0.02010(12) 0.00150(13) Ru3 0.04302(14) 0.05743(19) 0.04533(19) 0.00568(16) 0.01889(12) 0.00147(14) Ru4 0.04164(14) 0.0615(2) 0.0490(2) 0.00180(17) 0.01885(13) -0.00203(14) Ru5 0.04810(14) 0.04980(18) 0.04142(18) 0.00366(15) 0.02227(12) -0.00093(13) Si1 0.0826(8) 0.1001(11) 0.0916(11) 0.0302(9) 0.0425(7) -0.0030(8) Si2 0.0876(8) 0.0782(9) 0.0456(8) 0.0110(7) 0.0237(6) 0.0047(7) Si3 0.0754(8) 0.0672(8) 0.0857(11) 0.0310(8) 0.0318(7) 0.0132(7) Si4 0.0972(7) 0.0714(8) 0.0923(9) 0.0046(7) 0.0697(6) 0.0150(7) C100 0.36(2) 0.180(10) 0.43(2) -0.107(13) -0.223(19) 0.115(10) C101 0.325(18) 0.198(13) 0.61(4) -0.074(19) 0.10(2) -0.126(13) C102 0.303(17) 0.225(16) 0.69(4) -0.133(19) 0.21(2) -0.044(15) #----------------------------------------------------------------------------# # 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 1.281(6) . ? C1 Ru3 1.969(4) . ? C1 Ru1 2.185(5) . ? C1 Ru2 2.261(4) . ? C2 Si1 1.913(5) . ? C2 Ru1 2.236(5) . ? C2 Ru2 2.345(4) . ? C3 C4 1.290(6) . ? C3 Ru5 1.977(4) . ? C3 Ru4 2.181(4) . ? C3 Ru2 2.244(4) . ? C4 Si2 1.871(5) . ? C4 Ru4 2.264(5) . ? C4 Ru2 2.367(4) . ? C5 C6 1.305(7) . ? C5 Si4 1.870(5) . ? C5 Ru5 2.178(4) . ? C5 Ru3 2.192(5) . ? C6 Si3 1.875(5) . ? C6 Ru5 2.216(4) . ? C6 Ru3 2.220(4) . ? C7 Si1 1.893(9) . ? C7 H7A 0.96 . ? C7 H7B 0.96 . ? C7 H7C 0.96 . ? C8 Si1 1.870(6) . ? C8 H8A 0.96 . ? C8 H8B 0.96 . ? C8 H8C 0.96 . ? C9 Si1 1.866(8) . ? C9 H9A 0.96 . ? C9 H9B 0.96 . ? C9 H9C 0.96 . ? C15 Si2 1.799(8) . ? C15 H15A 0.96 . ? C15 H15C 0.96 . ? C15 H15B 0.96 . ? C16 Si2 1.864(7) . ? C16 H16C 0.96 . ? C16 H16A 0.96 . ? C16 H16B 0.96 . ? C11 O11 1.140(6) . ? C11 Ru1 1.916(5) . ? C14 Si2 1.856(7) . ? C14 H14C 0.96 . ? C14 H14A 0.96 . ? C14 H14B 0.96 . ? C12 O12 1.146(5) . ? C12 Ru1 1.881(5) . ? C24 Si4 1.853(6) . ? C24 H24B 0.96 . ? C24 H24A 0.96 . ? C24 H24C 0.96 . ? C13 O13 1.137(7) . ? C13 Ru1 1.907(6) . ? C25 Si4 1.798(7) . ? C25 H25B 0.96 . ? C25 H25C 0.96 . ? C25 H25A 0.96 . ? C23 Si4 1.834(8) . ? C23 H23C 0.96 . ? C23 H23A 0.96 . ? C23 H23B 0.96 . ? C17 Si3 1.867(8) . ? C17 H17B 0.96 . ? C17 H17A 0.96 . ? C17 H17C 0.96 . ? C19 Si3 1.829(6) . ? C19 H19A 0.96 . ? C19 H19C 0.96 . ? C19 H19B 0.96 . ? C18 Si3 1.841(7) . ? C18 H18C 0.96 . ? C18 H18A 0.96 . ? C18 H18B 0.96 . ? C21 O21 1.141(6) . ? C21 Ru2 1.895(5) . ? C22 O22 1.141(5) . ? C22 Ru2 1.891(5) . ? C31 O31 1.142(6) . ? C31 Ru3 1.859(5) . ? C32 O32 1.136(7) . ? C32 Ru3 1.923(6) . ? C41 O41 1.123(7) . ? C41 Ru4 1.935(6) . ? C42 O42 1.140(6) . ? C42 Ru4 1.894(5) . ? C43 O43 1.117(6) . ? C43 Ru4 1.935(5) . ? C51 O51 1.128(7) . ? C51 Ru5 1.924(6) . ? C52 O52 1.140(6) . ? C52 Ru5 1.866(5) . ? Ru1 Ru2 2.7130(4) . ? Ru1 Ru3 2.7863(5) . ? Ru1 H1AA 1.7813 . ? Ru2 Ru4 2.7260(4) . ? Ru2 Ru3 3.0084(4) . ? Ru2 Ru5 3.0479(5) . ? Ru2 H1AA 1.9134 . ? Ru2 H2AA 1.9124 . ? Ru3 Ru5 2.9079(4) . ? Ru4 Ru5 2.7881(4) . ? Ru4 H2AA 1.7727 . ? C100 C100 1.357(18) 2_656 ? C100 C101 1.495(9) . ? C100 H10A 0.97 . ? C100 H10B 0.97 . ? C101 C102 1.492(9) . ? C101 H10C 0.97 . ? C101 H10D 0.97 . ? C102 H10E 0.96 . ? C102 H10F 0.96 . ? C102 H10G 0.96 . ? 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 Ru3 158.2(4) . . ? C2 C1 Ru1 75.4(3) . . ? Ru3 C1 Ru1 84.08(17) . . ? C2 C1 Ru2 77.5(2) . . ? Ru3 C1 Ru2 90.40(16) . . ? Ru1 C1 Ru2 75.18(14) . . ? C1 C2 Si1 147.2(4) . . ? C1 C2 Ru1 71.0(3) . . ? Si1 C2 Ru1 124.6(2) . . ? C1 C2 Ru2 70.3(3) . . ? Si1 C2 Ru2 139.0(2) . . ? Ru1 C2 Ru2 72.58(14) . . ? C4 C3 Ru5 160.3(4) . . ? C4 C3 Ru4 76.7(3) . . ? Ru5 C3 Ru4 84.06(17) . . ? C4 C3 Ru2 79.1(3) . . ? Ru5 C3 Ru2 92.23(16) . . ? Ru4 C3 Ru2 76.02(14) . . ? C3 C4 Si2 148.1(4) . . ? C3 C4 Ru4 69.7(3) . . ? Si2 C4 Ru4 126.86(19) . . ? C3 C4 Ru2 68.6(2) . . ? Si2 C4 Ru2 138.7(2) . . ? Ru4 C4 Ru2 72.09(14) . . ? C6 C5 Si4 144.5(4) . . ? C6 C5 Ru5 74.3(3) . . ? Si4 C5 Ru5 128.2(2) . . ? C6 C5 Ru3 74.0(3) . . ? Si4 C5 Ru3 129.3(2) . . ? Ru5 C5 Ru3 83.43(16) . . ? C5 C6 Si3 138.8(4) . . ? C5 C6 Ru5 71.1(2) . . ? Si3 C6 Ru5 134.2(2) . . ? C5 C6 Ru3 71.6(3) . . ? Si3 C6 Ru3 133.2(2) . . ? Ru5 C6 Ru3 81.92(14) . . ? Si1 C7 H7A 109.5 . . ? Si1 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? Si1 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? Si1 C8 H8A 109.5 . . ? Si1 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? Si1 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? Si1 C9 H9A 109.5 . . ? Si1 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? Si1 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? Si2 C15 H15A 109.5 . . ? Si2 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? Si2 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? H15C C15 H15B 109.5 . . ? Si2 C16 H16C 109.5 . . ? Si2 C16 H16A 109.5 . . ? H16C C16 H16A 109.5 . . ? Si2 C16 H16B 109.5 . . ? H16C C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? O11 C11 Ru1 179.7(6) . . ? Si2 C14 H14C 109.5 . . ? Si2 C14 H14A 109.5 . . ? H14C C14 H14A 109.5 . . ? Si2 C14 H14B 109.5 . . ? H14C C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? O12 C12 Ru1 178.5(5) . . ? Si4 C24 H24B 109.5 . . ? Si4 C24 H24A 109.5 . . ? H24B C24 H24A 109.5 . . ? Si4 C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? O13 C13 Ru1 179.1(5) . . ? Si4 C25 H25B 109.5 . . ? Si4 C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? Si4 C25 H25A 109.5 . . ? H25B C25 H25A 109.5 . . ? H25C C25 H25A 109.5 . . ? Si4 C23 H23C 109.5 . . ? Si4 C23 H23A 109.5 . . ? H23C C23 H23A 109.5 . . ? Si4 C23 H23B 109.5 . . ? H23C C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? Si3 C17 H17B 109.5 . . ? Si3 C17 H17A 109.5 . . ? H17B C17 H17A 109.5 . . ? Si3 C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? Si3 C19 H19A 109.5 . . ? Si3 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? Si3 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? H19C C19 H19B 109.5 . . ? Si3 C18 H18C 109.5 . . ? Si3 C18 H18A 109.5 . . ? H18C C18 H18A 109.5 . . ? Si3 C18 H18B 109.5 . . ? H18C C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? O21 C21 Ru2 176.3(4) . . ? O22 C22 Ru2 175.1(5) . . ? O31 C31 Ru3 179.3(7) . . ? O32 C32 Ru3 175.7(5) . . ? O41 C41 Ru4 177.0(4) . . ? O42 C42 Ru4 178.3(6) . . ? O43 C43 Ru4 178.2(5) . . ? O51 C51 Ru5 176.2(4) . . ? O52 C52 Ru5 179.2(5) . . ? C12 Ru1 C13 92.0(2) . . ? C12 Ru1 C11 96.2(2) . . ? C13 Ru1 C11 92.6(2) . . ? C12 Ru1 C1 97.9(2) . . ? C13 Ru1 C1 139.1(2) . . ? C11 Ru1 C1 125.2(2) . . ? C12 Ru1 C2 101.6(2) . . ? C13 Ru1 C2 165.26(17) . . ? C11 Ru1 C2 91.6(2) . . ? C1 Ru1 C2 33.65(15) . . ? C12 Ru1 Ru2 151.62(18) . . ? C13 Ru1 Ru2 109.74(13) . . ? C11 Ru1 Ru2 100.61(14) . . ? C1 Ru1 Ru2 53.68(9) . . ? C2 Ru1 Ru2 55.56(10) . . ? C12 Ru1 Ru3 94.50(16) . . ? C13 Ru1 Ru3 95.29(16) . . ? C11 Ru1 Ru3 166.45(15) . . ? C1 Ru1 Ru3 44.65(11) . . ? C2 Ru1 Ru3 78.12(11) . . ? Ru2 Ru1 Ru3 66.315(12) . . ? C12 Ru1 H1AA 161.4 . . ? C13 Ru1 H1AA 83.4 . . ? C11 Ru1 H1AA 66.1 . . ? C1 Ru1 H1AA 97.3 . . ? C2 Ru1 H1AA 85.4 . . ? Ru2 Ru1 H1AA 44.7 . . ? Ru3 Ru1 H1AA 103.9 . . ? C22 Ru2 C21 92.5(2) . . ? C22 Ru2 C3 120.95(17) . . ? C21 Ru2 C3 116.21(18) . . ? C22 Ru2 C1 122.00(18) . . ? C21 Ru2 C1 117.09(16) . . ? C3 Ru2 C1 90.57(15) . . ? C22 Ru2 C2 90.40(18) . . ? C21 Ru2 C2 130.98(16) . . ? C3 Ru2 C2 103.60(16) . . ? C1 Ru2 C2 32.23(14) . . ? C22 Ru2 C4 89.26(17) . . ? C21 Ru2 C4 129.56(16) . . ? C3 Ru2 C4 32.34(14) . . ? C1 Ru2 C4 103.98(15) . . ? C2 Ru2 C4 99.39(16) . . ? C22 Ru2 Ru1 93.25(13) . . ? C21 Ru2 Ru1 79.13(12) . . ? C3 Ru2 Ru1 139.87(9) . . ? C1 Ru2 Ru1 51.14(11) . . ? C2 Ru2 Ru1 51.86(11) . . ? C4 Ru2 Ru1 151.11(11) . . ? C22 Ru2 Ru4 93.10(13) . . ? C21 Ru2 Ru4 77.38(12) . . ? C3 Ru2 Ru4 50.94(10) . . ? C1 Ru2 Ru4 139.23(11) . . ? C2 Ru2 Ru4 151.26(11) . . ? C4 Ru2 Ru4 52.20(11) . . ? Ru1 Ru2 Ru4 155.88(2) . . ? C22 Ru2 Ru3 151.25(13) . . ? C21 Ru2 Ru3 83.03(12) . . ? C3 Ru2 Ru3 85.95(9) . . ? C1 Ru2 Ru3 40.87(11) . . ? C2 Ru2 Ru3 72.03(10) . . ? C4 Ru2 Ru3 115.44(10) . . ? Ru1 Ru2 Ru3 58.011(11) . . ? Ru4 Ru2 Ru3 113.343(15) . . ? C22 Ru2 Ru5 150.46(13) . . ? C21 Ru2 Ru5 83.31(14) . . ? C3 Ru2 Ru5 40.39(11) . . ? C1 Ru2 Ru5 85.26(11) . . ? C2 Ru2 Ru5 114.38(11) . . ? C4 Ru2 Ru5 71.73(10) . . ? Ru1 Ru2 Ru5 114.410(14) . . ? Ru4 Ru2 Ru5 57.423(11) . . ? Ru3 Ru2 Ru5 57.386(10) . . ? C22 Ru2 H1AA 60.8 . . ? C21 Ru2 H1AA 59.9 . . ? C3 Ru2 H1AA 176.1 . . ? C1 Ru2 H1AA 91.1 . . ? C2 Ru2 H1AA 79.6 . . ? C4 Ru2 H1AA 150 . . ? Ru1 Ru2 H1AA 40.9 . . ? Ru4 Ru2 H1AA 126.5 . . ? Ru3 Ru2 H1AA 93 . . ? Ru5 Ru2 H1AA 136.3 . . ? C22 Ru2 H2AA 60.5 . . ? C21 Ru2 H2AA 59.6 . . ? C3 Ru2 H2AA 90 . . ? C1 Ru2 H2AA 176.4 . . ? C2 Ru2 H2AA 150.7 . . ? C4 Ru2 H2AA 78.3 . . ? Ru1 Ru2 H2AA 127.5 . . ? Ru4 Ru2 H2AA 40.4 . . ? Ru3 Ru2 H2AA 135.7 . . ? Ru5 Ru2 H2AA 92.9 . . ? H1AA Ru2 H2AA 88.2 . . ? C31 Ru3 C32 93.2(2) . . ? C31 Ru3 C1 100.6(2) . . ? C32 Ru3 C1 141.8(2) . . ? C31 Ru3 C5 100.4(2) . . ? C32 Ru3 C5 118.4(2) . . ? C1 Ru3 C5 93.99(18) . . ? C31 Ru3 C6 98.65(19) . . ? C32 Ru3 C6 84.4(2) . . ? C1 Ru3 C6 127.54(18) . . ? C5 Ru3 C6 34.42(18) . . ? C31 Ru3 Ru1 96.39(16) . . ? C32 Ru3 Ru1 92.10(16) . . ? C1 Ru3 Ru1 51.27(13) . . ? C5 Ru3 Ru1 143.84(12) . . ? C6 Ru3 Ru1 164.73(10) . . ? C31 Ru3 Ru5 146.06(17) . . ? C32 Ru3 Ru5 93.13(14) . . ? C1 Ru3 Ru5 94.67(10) . . ? C5 Ru3 Ru5 48.09(11) . . ? C6 Ru3 Ru5 48.99(10) . . ? Ru1 Ru3 Ru5 116.636(14) . . ? C31 Ru3 Ru2 146.56(17) . . ? C32 Ru3 Ru2 104.70(15) . . ? C1 Ru3 Ru2 48.73(11) . . ? C5 Ru3 Ru2 95.57(10) . . ? C6 Ru3 Ru2 110.84(10) . . ? Ru1 Ru3 Ru2 55.674(11) . . ? Ru5 Ru3 Ru2 61.989(11) . . ? C42 Ru4 C41 92.7(2) . . ? C42 Ru4 C43 94.1(2) . . ? C41 Ru4 C43 93.7(2) . . ? C42 Ru4 C3 99.2(2) . . ? C41 Ru4 C3 137.82(17) . . ? C43 Ru4 C3 125.2(2) . . ? C42 Ru4 C4 100.5(2) . . ? C41 Ru4 C4 165.33(16) . . ? C43 Ru4 C4 91.7(2) . . ? C3 Ru4 C4 33.66(14) . . ? C42 Ru4 Ru2 152.08(18) . . ? C41 Ru4 Ru2 109.83(14) . . ? C43 Ru4 Ru2 100.50(14) . . ? C3 Ru4 Ru2 53.04(10) . . ? C4 Ru4 Ru2 55.71(10) . . ? C42 Ru4 Ru5 95.90(15) . . ? C41 Ru4 Ru5 93.93(14) . . ? C43 Ru4 Ru5 167.11(14) . . ? C3 Ru4 Ru5 44.84(11) . . ? C4 Ru4 Ru5 78.44(10) . . ? Ru2 Ru4 Ru5 67.100(12) . . ? C42 Ru4 H2AA 158.8 . . ? C41 Ru4 H2AA 86.1 . . ? C43 Ru4 H2AA 64.9 . . ? C3 Ru4 H2AA 95.9 . . ? C4 Ru4 H2AA 83.9 . . ? Ru2 Ru4 H2AA 44.3 . . ? Ru5 Ru4 H2AA 105.3 . . ? C52 Ru5 C51 91.5(2) . . ? C52 Ru5 C3 98.73(19) . . ? C51 Ru5 C3 143.65(19) . . ? C52 Ru5 C5 98.56(19) . . ? C51 Ru5 C5 117.81(18) . . ? C3 Ru5 C5 95.13(17) . . ? C52 Ru5 C6 99.65(18) . . ? C51 Ru5 C6 83.28(19) . . ? C3 Ru5 C6 128.39(17) . . ? C5 Ru5 C6 34.55(18) . . ? C52 Ru5 Ru4 97.84(14) . . ? C51 Ru5 Ru4 93.10(14) . . ? C3 Ru5 Ru4 51.09(12) . . ? C5 Ru5 Ru4 144.35(12) . . ? C6 Ru5 Ru4 162.21(12) . . ? C52 Ru5 Ru3 145.82(14) . . ? C51 Ru5 Ru3 96.92(13) . . ? C3 Ru5 Ru3 93.85(10) . . ? C5 Ru5 Ru3 48.48(12) . . ? C6 Ru5 Ru3 49.09(11) . . ? Ru4 Ru5 Ru3 114.604(15) . . ? C52 Ru5 Ru2 144.70(14) . . ? C51 Ru5 Ru2 110.76(16) . . ? C3 Ru5 Ru2 47.38(12) . . ? C5 Ru5 Ru2 94.75(11) . . ? C6 Ru5 Ru2 109.57(11) . . ? Ru4 Ru5 Ru2 55.477(10) . . ? Ru3 Ru5 Ru2 60.625(10) . . ? C9 Si1 C8 108.3(4) . . ? C9 Si1 C7 112.2(4) . . ? C8 Si1 C7 106.4(4) . . ? C9 Si1 C2 112.1(3) . . ? C8 Si1 C2 109.1(3) . . ? C7 Si1 C2 108.6(3) . . ? C15 Si2 C14 110.6(4) . . ? C15 Si2 C16 109.5(4) . . ? C14 Si2 C16 108.3(4) . . ? C15 Si2 C4 110.4(3) . . ? C14 Si2 C4 106.3(3) . . ? C16 Si2 C4 111.7(3) . . ? C19 Si3 C18 112.1(4) . . ? C19 Si3 C17 107.3(3) . . ? C18 Si3 C17 110.0(4) . . ? C19 Si3 C6 106.8(3) . . ? C18 Si3 C6 107.2(3) . . ? C17 Si3 C6 113.5(3) . . ? C25 Si4 C23 114.1(4) . . ? C25 Si4 C24 109.0(4) . . ? C23 Si4 C24 107.4(4) . . ? C25 Si4 C5 112.5(3) . . ? C23 Si4 C5 107.1(3) . . ? C24 Si4 C5 106.3(3) . . ? C100 C100 C101 133.2(10) 2_656 . ? C100 C100 H10A 103.9 2_656 . ? C101 C100 H10A 103.9 . . ? C100 C100 H10B 103.9 2_656 . ? C101 C100 H10B 103.9 . . ? H10A C100 H10B 105.4 . . ? C102 C101 C100 139.1(11) . . ? C102 C101 H10C 102.3 . . ? C100 C101 H10C 102.3 . . ? C102 C101 H10D 102.3 . . ? C100 C101 H10D 102.3 . . ? H10C C101 H10D 104.9 . . ? C101 C102 H10E 109.5 . . ? C101 C102 H10F 109.5 . . ? H10E C102 H10F 109.5 . . ? C101 C102 H10G 109.5 . . ? H10E C102 H10G 109.5 . . ? H10F C102 H10G 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Ru3 C1 C2 Si1 145.1(6) . . . . ? Ru1 C1 C2 Si1 125.0(6) . . . . ? Ru2 C1 C2 Si1 -157.3(6) . . . . ? Ru3 C1 C2 Ru1 20.0(8) . . . . ? Ru2 C1 C2 Ru1 77.71(11) . . . . ? Ru3 C1 C2 Ru2 -57.7(8) . . . . ? Ru1 C1 C2 Ru2 -77.71(11) . . . . ? Ru5 C3 C4 Si2 -141.0(8) . . . . ? Ru4 C3 C4 Si2 -128.0(6) . . . . ? Ru2 C3 C4 Si2 153.9(6) . . . . ? Ru5 C3 C4 Ru4 -13.0(9) . . . . ? Ru2 C3 C4 Ru4 -78.05(11) . . . . ? Ru5 C3 C4 Ru2 65.1(9) . . . . ? Ru4 C3 C4 Ru2 78.05(11) . . . . ? Si4 C5 C6 Si3 1.3(9) . . . . ? Ru5 C5 C6 Si3 136.8(5) . . . . ? Ru3 C5 C6 Si3 -135.7(4) . . . . ? Si4 C5 C6 Ru5 -135.5(5) . . . . ? Ru3 C5 C6 Ru5 87.54(12) . . . . ? Si4 C5 C6 Ru3 137.0(5) . . . . ? Ru5 C5 C6 Ru3 -87.54(12) . . . . ? O12 C12 Ru1 C13 11E1(2) . . . . ? O12 C12 Ru1 C11 -16E1(2) . . . . ? O12 C12 Ru1 C1 -3E1(2) . . . . ? O12 C12 Ru1 C2 -7E1(2) . . . . ? O12 C12 Ru1 Ru2 -4E1(2) . . . . ? O12 C12 Ru1 Ru3 1E1(2) . . . . ? O13 C13 Ru1 C12 8E1(2) . . . . ? O13 C13 Ru1 C11 -2E1(2) . . . . ? O13 C13 Ru1 C1 -18E1(10) . . . . ? O13 C13 Ru1 C2 -12E1(2) . . . . ? O13 C13 Ru1 Ru2 -12E1(2) . . . . ? O13 C13 Ru1 Ru3 17E1(10) . . . . ? O11 C11 Ru1 C12 10E1(10) . . . . ? O11 C11 Ru1 C13 -17E1(10) . . . . ? O11 C11 Ru1 C1 -0E1(10) . . . . ? O11 C11 Ru1 C2 -0E1(10) . . . . ? O11 C11 Ru1 Ru2 -6E1(10) . . . . ? O11 C11 Ru1 Ru3 -4E1(10) . . . . ? C2 C1 Ru1 C12 -99.0(3) . . . . ? Ru3 C1 Ru1 C12 88.4(2) . . . . ? Ru2 C1 Ru1 C12 -179.64(19) . . . . ? C2 C1 Ru1 C13 158.6(3) . . . . ? Ru3 C1 Ru1 C13 -14.1(3) . . . . ? Ru2 C1 Ru1 C13 77.9(2) . . . . ? C2 C1 Ru1 C11 4.5(3) . . . . ? Ru3 C1 Ru1 C11 -168.17(18) . . . . ? Ru2 C1 Ru1 C11 -76.2(2) . . . . ? Ru3 C1 Ru1 C2 -172.6(3) . . . . ? Ru2 C1 Ru1 C2 -80.7(2) . . . . ? C2 C1 Ru1 Ru2 80.7(2) . . . . ? Ru3 C1 Ru1 Ru2 -91.99(13) . . . . ? C2 C1 Ru1 Ru3 172.6(3) . . . . ? Ru2 C1 Ru1 Ru3 91.99(13) . . . . ? C1 C2 Ru1 C12 86.9(3) . . . . ? Si1 C2 Ru1 C12 -60.4(3) . . . . ? Ru2 C2 Ru1 C12 161.52(18) . . . . ? C1 C2 Ru1 C13 -69.8(8) . . . . ? Si1 C2 Ru1 C13 142.8(7) . . . . ? Ru2 C2 Ru1 C13 4.8(8) . . . . ? C1 C2 Ru1 C11 -176.3(3) . . . . ? Si1 C2 Ru1 C11 36.3(3) . . . . ? Ru2 C2 Ru1 C11 -101.76(16) . . . . ? Si1 C2 Ru1 C1 -147.4(4) . . . . ? Ru2 C2 Ru1 C1 74.6(2) . . . . ? C1 C2 Ru1 Ru2 -74.6(2) . . . . ? Si1 C2 Ru1 Ru2 138.1(3) . . . . ? C1 C2 Ru1 Ru3 -5.3(2) . . . . ? Si1 C2 Ru1 Ru3 -152.6(2) . . . . ? Ru2 C2 Ru1 Ru3 69.30(7) . . . . ? O22 C22 Ru2 C21 11(5) . . . . ? O22 C22 Ru2 C3 133(5) . . . . ? O22 C22 Ru2 C1 -114(5) . . . . ? O22 C22 Ru2 C2 -121(5) . . . . ? O22 C22 Ru2 C4 140(5) . . . . ? O22 C22 Ru2 Ru1 -69(5) . . . . ? O22 C22 Ru2 Ru4 88(5) . . . . ? O22 C22 Ru2 Ru3 -69(5) . . . . ? O22 C22 Ru2 Ru5 91(5) . . . . ? O21 C21 Ru2 C22 -9(5) . . . . ? O21 C21 Ru2 C3 -135(5) . . . . ? O21 C21 Ru2 C1 120(5) . . . . ? O21 C21 Ru2 C2 84(5) . . . . ? O21 C21 Ru2 C4 -100(5) . . . . ? O21 C21 Ru2 Ru1 84(5) . . . . ? O21 C21 Ru2 Ru4 -101(5) . . . . ? O21 C21 Ru2 Ru3 143(5) . . . . ? O21 C21 Ru2 Ru5 -159(5) . . . . ? C4 C3 Ru2 C22 12.7(4) . . . . ? Ru5 C3 Ru2 C22 -149.4(2) . . . . ? Ru4 C3 Ru2 C22 -66.1(2) . . . . ? C4 C3 Ru2 C21 123.3(3) . . . . ? Ru5 C3 Ru2 C21 -38.8(2) . . . . ? Ru4 C3 Ru2 C21 44.50(18) . . . . ? C4 C3 Ru2 C1 -115.9(3) . . . . ? Ru5 C3 Ru2 C1 82.00(16) . . . . ? Ru4 C3 Ru2 C1 165.32(14) . . . . ? C4 C3 Ru2 C2 -86.1(3) . . . . ? Ru5 C3 Ru2 C2 111.77(15) . . . . ? Ru4 C3 Ru2 C2 -164.91(12) . . . . ? Ru5 C3 Ru2 C4 -162.1(3) . . . . ? Ru4 C3 Ru2 C4 -78.8(3) . . . . ? C4 C3 Ru2 Ru1 -131.7(2) . . . . ? Ru5 C3 Ru2 Ru1 66.1(2) . . . . ? Ru4 C3 Ru2 Ru1 149.44(8) . . . . ? C4 C3 Ru2 Ru4 78.8(3) . . . . ? Ru5 C3 Ru2 Ru4 -83.32(15) . . . . ? C4 C3 Ru2 Ru3 -156.5(3) . . . . ? Ru5 C3 Ru2 Ru3 41.36(11) . . . . ? Ru4 C3 Ru2 Ru3 124.68(9) . . . . ? C4 C3 Ru2 Ru5 162.1(3) . . . . ? Ru4 C3 Ru2 Ru5 83.32(15) . . . . ? C2 C1 Ru2 C22 -12.6(4) . . . . ? Ru3 C1 Ru2 C22 149.1(2) . . . . ? Ru1 C1 Ru2 C22 65.3(2) . . . . ? C2 C1 Ru2 C21 -124.8(3) . . . . ? Ru3 C1 Ru2 C21 36.9(2) . . . . ? Ru1 C1 Ru2 C21 -46.8(2) . . . . ? C2 C1 Ru2 C3 115.2(3) . . . . ? Ru3 C1 Ru2 C3 -83.14(17) . . . . ? Ru1 C1 Ru2 C3 -166.91(14) . . . . ? Ru3 C1 Ru2 C2 161.7(4) . . . . ? Ru1 C1 Ru2 C2 77.9(3) . . . . ? C2 C1 Ru2 C4 85.4(3) . . . . ? Ru3 C1 Ru2 C4 -112.88(16) . . . . ? Ru1 C1 Ru2 C4 163.35(13) . . . . ? C2 C1 Ru2 Ru1 -77.9(3) . . . . ? Ru3 C1 Ru2 Ru1 83.77(15) . . . . ? C2 C1 Ru2 Ru4 132.7(2) . . . . ? Ru3 C1 Ru2 Ru4 -65.6(2) . . . . ? Ru1 C1 Ru2 Ru4 -149.37(8) . . . . ? C2 C1 Ru2 Ru3 -161.7(4) . . . . ? Ru1 C1 Ru2 Ru3 -83.77(15) . . . . ? C2 C1 Ru2 Ru5 155.3(3) . . . . ? Ru3 C1 Ru2 Ru5 -43.05(12) . . . . ? Ru1 C1 Ru2 Ru5 -126.82(10) . . . . ? C1 C2 Ru2 C22 169.3(3) . . . . ? Si1 C2 Ru2 C22 -29.3(4) . . . . ? Ru1 C2 Ru2 C22 93.81(17) . . . . ? C1 C2 Ru2 C21 75.7(4) . . . . ? Si1 C2 Ru2 C21 -122.9(4) . . . . ? Ru1 C2 Ru2 C21 0.2(2) . . . . ? C1 C2 Ru2 C3 -68.6(3) . . . . ? Si1 C2 Ru2 C3 92.8(4) . . . . ? Ru1 C2 Ru2 C3 -144.12(12) . . . . ? Si1 C2 Ru2 C1 161.4(6) . . . . ? Ru1 C2 Ru2 C1 -75.5(3) . . . . ? C1 C2 Ru2 C4 -101.4(3) . . . . ? Si1 C2 Ru2 C4 60.0(4) . . . . ? Ru1 C2 Ru2 C4 -176.87(12) . . . . ? C1 C2 Ru2 Ru1 75.5(3) . . . . ? Si1 C2 Ru2 Ru1 -123.1(4) . . . . ? C1 C2 Ru2 Ru4 -93.5(3) . . . . ? Si1 C2 Ru2 Ru4 67.9(5) . . . . ? Ru1 C2 Ru2 Ru4 -169.00(11) . . . . ? C1 C2 Ru2 Ru3 12.5(3) . . . . ? Si1 C2 Ru2 Ru3 173.9(4) . . . . ? Ru1 C2 Ru2 Ru3 -63.03(7) . . . . ? C1 C2 Ru2 Ru5 -27.3(3) . . . . ? Si1 C2 Ru2 Ru5 134.1(3) . . . . ? Ru1 C2 Ru2 Ru5 -102.77(9) . . . . ? C3 C4 Ru2 C22 -169.1(3) . . . . ? Si2 C4 Ru2 C22 31.5(4) . . . . ? Ru4 C4 Ru2 C22 -94.50(17) . . . . ? C3 C4 Ru2 C21 -76.5(3) . . . . ? Si2 C4 Ru2 C21 124.1(3) . . . . ? Ru4 C4 Ru2 C21 -1.9(2) . . . . ? Si2 C4 Ru2 C3 -159.4(5) . . . . ? Ru4 C4 Ru2 C3 74.6(3) . . . . ? C3 C4 Ru2 C1 68.0(3) . . . . ? Si2 C4 Ru2 C1 -91.4(3) . . . . ? Ru4 C4 Ru2 C1 142.62(13) . . . . ? C3 C4 Ru2 C2 100.6(3) . . . . ? Si2 C4 Ru2 C2 -58.8(4) . . . . ? Ru4 C4 Ru2 C2 175.22(12) . . . . ? C3 C4 Ru2 Ru1 95.5(3) . . . . ? Si2 C4 Ru2 Ru1 -63.9(4) . . . . ? Ru4 C4 Ru2 Ru1 170.12(11) . . . . ? C3 C4 Ru2 Ru4 -74.6(3) . . . . ? Si2 C4 Ru2 Ru4 126.0(4) . . . . ? C3 C4 Ru2 Ru3 26.1(3) . . . . ? Si2 C4 Ru2 Ru3 -133.3(3) . . . . ? Ru4 C4 Ru2 Ru3 100.74(9) . . . . ? C3 C4 Ru2 Ru5 -12.1(2) . . . . ? Si2 C4 Ru2 Ru5 -171.5(4) . . . . ? Ru4 C4 Ru2 Ru5 62.52(7) . . . . ? C12 Ru1 Ru2 C22 -128.7(4) . . . . ? C13 Ru1 Ru2 C22 93.3(2) . . . . ? C11 Ru1 Ru2 C22 -3.3(3) . . . . ? C1 Ru1 Ru2 C22 -129.5(2) . . . . ? C2 Ru1 Ru2 C22 -88.0(2) . . . . ? Ru3 Ru1 Ru2 C22 -179.57(17) . . . . ? C12 Ru1 Ru2 C21 139.4(4) . . . . ? C13 Ru1 Ru2 C21 1.4(2) . . . . ? C11 Ru1 Ru2 C21 -95.2(2) . . . . ? C1 Ru1 Ru2 C21 138.6(2) . . . . ? C2 Ru1 Ru2 C21 -179.86(19) . . . . ? Ru3 Ru1 Ru2 C21 88.53(14) . . . . ? C12 Ru1 Ru2 C3 21.3(4) . . . . ? C13 Ru1 Ru2 C3 -116.6(2) . . . . ? C11 Ru1 Ru2 C3 146.7(3) . . . . ? C1 Ru1 Ru2 C3 20.6(2) . . . . ? C2 Ru1 Ru2 C3 62.1(2) . . . . ? Ru3 Ru1 Ru2 C3 -29.50(18) . . . . ? C12 Ru1 Ru2 C1 0.8(4) . . . . ? C13 Ru1 Ru2 C1 -137.2(2) . . . . ? C11 Ru1 Ru2 C1 126.2(2) . . . . ? C2 Ru1 Ru2 C1 41.53(19) . . . . ? Ru3 Ru1 Ru2 C1 -50.08(14) . . . . ? C12 Ru1 Ru2 C2 -40.8(4) . . . . ? C13 Ru1 Ru2 C2 -178.7(2) . . . . ? C11 Ru1 Ru2 C2 84.6(2) . . . . ? C1 Ru1 Ru2 C2 -41.53(19) . . . . ? Ru3 Ru1 Ru2 C2 -91.61(13) . . . . ? C12 Ru1 Ru2 C4 -34.4(4) . . . . ? C13 Ru1 Ru2 C4 -172.3(3) . . . . ? C11 Ru1 Ru2 C4 91.0(3) . . . . ? C1 Ru1 Ru2 C4 -35.1(3) . . . . ? C2 Ru1 Ru2 C4 6.4(2) . . . . ? Ru3 Ru1 Ru2 C4 -85.2(2) . . . . ? C12 Ru1 Ru2 Ru4 126.2(4) . . . . ? C13 Ru1 Ru2 Ru4 -11.69(18) . . . . ? C11 Ru1 Ru2 Ru4 -108.3(2) . . . . ? C1 Ru1 Ru2 Ru4 125.49(15) . . . . ? C2 Ru1 Ru2 Ru4 167.02(14) . . . . ? Ru3 Ru1 Ru2 Ru4 75.41(4) . . . . ? C12 Ru1 Ru2 Ru3 50.8(4) . . . . ? C13 Ru1 Ru2 Ru3 -87.10(17) . . . . ? C11 Ru1 Ru2 Ru3 176.25(19) . . . . ? C1 Ru1 Ru2 Ru3 50.08(14) . . . . ? C2 Ru1 Ru2 Ru3 91.61(13) . . . . ? C12 Ru1 Ru2 Ru5 61.9(4) . . . . ? C13 Ru1 Ru2 Ru5 -76.01(17) . . . . ? C11 Ru1 Ru2 Ru5 -172.66(19) . . . . ? C1 Ru1 Ru2 Ru5 61.17(14) . . . . ? C2 Ru1 Ru2 Ru5 102.70(13) . . . . ? Ru3 Ru1 Ru2 Ru5 11.093(17) . . . . ? O31 C31 Ru3 C32 16E1(10) . . . . ? O31 C31 Ru3 C1 -6E1(4) . . . . ? O31 C31 Ru3 C5 4E1(4) . . . . ? O31 C31 Ru3 C6 7E1(4) . . . . ? O31 C31 Ru3 Ru1 -11E1(4) . . . . ? O31 C31 Ru3 Ru5 6E1(4) . . . . ? O31 C31 Ru3 Ru2 -8E1(4) . . . . ? O32 C32 Ru3 C31 120(6) . . . . ? O32 C32 Ru3 C1 8(6) . . . . ? O32 C32 Ru3 C5 -137(6) . . . . ? O32 C32 Ru3 C6 -142(6) . . . . ? O32 C32 Ru3 Ru1 23(6) . . . . ? O32 C32 Ru3 Ru5 -94(6) . . . . ? O32 C32 Ru3 Ru2 -32(6) . . . . ? C2 C1 Ru3 C31 -109.2(8) . . . . ? Ru1 C1 Ru3 C31 -89.7(2) . . . . ? Ru2 C1 Ru3 C31 -164.7(2) . . . . ? C2 C1 Ru3 C32 0.2(9) . . . . ? Ru1 C1 Ru3 C32 19.7(3) . . . . ? Ru2 C1 Ru3 C32 -55.4(3) . . . . ? C2 C1 Ru3 C5 149.5(8) . . . . ? Ru1 C1 Ru3 C5 168.96(12) . . . . ? Ru2 C1 Ru3 C5 93.91(15) . . . . ? C2 C1 Ru3 C6 141.1(8) . . . . ? Ru1 C1 Ru3 C6 160.60(14) . . . . ? Ru2 C1 Ru3 C6 85.6(2) . . . . ? C2 C1 Ru3 Ru1 -19.5(7) . . . . ? Ru2 C1 Ru3 Ru1 -75.05(13) . . . . ? C2 C1 Ru3 Ru5 101.3(8) . . . . ? Ru1 C1 Ru3 Ru5 120.73(8) . . . . ? Ru2 C1 Ru3 Ru5 45.68(12) . . . . ? C2 C1 Ru3 Ru2 55.6(8) . . . . ? Ru1 C1 Ru3 Ru2 75.05(13) . . . . ? C6 C5 Ru3 C31 90.2(3) . . . . ? Si4 C5 Ru3 C31 -59.1(3) . . . . ? Ru5 C5 Ru3 C31 165.7(2) . . . . ? C6 C5 Ru3 C32 -9.3(3) . . . . ? Si4 C5 Ru3 C32 -158.5(3) . . . . ? Ru5 C5 Ru3 C32 66.2(2) . . . . ? C6 C5 Ru3 C1 -168.2(2) . . . . ? Si4 C5 Ru3 C1 42.5(3) . . . . ? Ru5 C5 Ru3 C1 -92.70(15) . . . . ? Si4 C5 Ru3 C6 -149.2(4) . . . . ? Ru5 C5 Ru3 C6 75.5(3) . . . . ? C6 C5 Ru3 Ru1 -153.6(2) . . . . ? Si4 C5 Ru3 Ru1 57.2(3) . . . . ? Ru5 C5 Ru3 Ru1 -78.0(2) . . . . ? C6 C5 Ru3 Ru5 -75.5(3) . . . . ? Si4 C5 Ru3 Ru5 135.2(3) . . . . ? C6 C5 Ru3 Ru2 -119.3(2) . . . . ? Si4 C5 Ru3 Ru2 91.4(2) . . . . ? Ru5 C5 Ru3 Ru2 -43.81(12) . . . . ? C5 C6 Ru3 C31 -95.8(3) . . . . ? Si3 C6 Ru3 C31 45.1(4) . . . . ? Ru5 C6 Ru3 C31 -168.5(2) . . . . ? C5 C6 Ru3 C32 171.8(3) . . . . ? Si3 C6 Ru3 C32 -47.3(4) . . . . ? Ru5 C6 Ru3 C32 99.08(19) . . . . ? C5 C6 Ru3 C1 14.9(3) . . . . ? Si3 C6 Ru3 C1 155.8(3) . . . . ? Ru5 C6 Ru3 C1 -57.8(2) . . . . ? Si3 C6 Ru3 C5 140.9(5) . . . . ? Ru5 C6 Ru3 C5 -72.7(2) . . . . ? C5 C6 Ru3 Ru1 94.5(6) . . . . ? Si3 C6 Ru3 Ru1 -124.7(3) . . . . ? Ru5 C6 Ru3 Ru1 21.7(6) . . . . ? C5 C6 Ru3 Ru5 72.7(2) . . . . ? Si3 C6 Ru3 Ru5 -146.4(4) . . . . ? C5 C6 Ru3 Ru2 68.2(3) . . . . ? Si3 C6 Ru3 Ru2 -150.9(3) . . . . ? Ru5 C6 Ru3 Ru2 -4.55(17) . . . . ? C12 Ru1 Ru3 C31 1.8(3) . . . . ? C13 Ru1 Ru3 C31 -90.7(2) . . . . ? C11 Ru1 Ru3 C31 144.2(8) . . . . ? C1 Ru1 Ru3 C31 98.5(2) . . . . ? C2 Ru1 Ru3 C31 102.7(2) . . . . ? Ru2 Ru1 Ru3 C31 160.1(2) . . . . ? C12 Ru1 Ru3 C32 95.3(2) . . . . ? C13 Ru1 Ru3 C32 2.85(19) . . . . ? C11 Ru1 Ru3 C32 -122.3(8) . . . . ? C1 Ru1 Ru3 C32 -167.97(19) . . . . ? C2 Ru1 Ru3 C32 -163.81(17) . . . . ? Ru2 Ru1 Ru3 C32 -106.41(14) . . . . ? C12 Ru1 Ru3 C1 -96.7(2) . . . . ? C13 Ru1 Ru3 C1 170.82(18) . . . . ? C11 Ru1 Ru3 C1 45.6(8) . . . . ? C2 Ru1 Ru3 C1 4.16(16) . . . . ? Ru2 Ru1 Ru3 C1 61.56(13) . . . . ? C12 Ru1 Ru3 C5 -115.6(3) . . . . ? C13 Ru1 Ru3 C5 151.9(2) . . . . ? C11 Ru1 Ru3 C5 26.8(8) . . . . ? C1 Ru1 Ru3 C5 -18.9(2) . . . . ? C2 Ru1 Ru3 C5 -14.7(2) . . . . ? Ru2 Ru1 Ru3 C5 42.68(19) . . . . ? C12 Ru1 Ru3 C6 171.6(6) . . . . ? C13 Ru1 Ru3 C6 79.2(5) . . . . ? C11 Ru1 Ru3 C6 -46.0(9) . . . . ? C1 Ru1 Ru3 C6 -91.6(5) . . . . ? C2 Ru1 Ru3 C6 -87.5(5) . . . . ? Ru2 Ru1 Ru3 C6 -30.1(5) . . . . ? C12 Ru1 Ru3 Ru5 -170.16(19) . . . . ? C13 Ru1 Ru3 Ru5 97.40(13) . . . . ? C11 Ru1 Ru3 Ru5 -27.8(8) . . . . ? C1 Ru1 Ru3 Ru5 -73.42(13) . . . . ? C2 Ru1 Ru3 Ru5 -69.26(10) . . . . ? Ru2 Ru1 Ru3 Ru5 -11.855(19) . . . . ? C12 Ru1 Ru3 Ru2 -158.30(19) . . . . ? C13 Ru1 Ru3 Ru2 109.26(13) . . . . ? C11 Ru1 Ru3 Ru2 -15.9(8) . . . . ? C1 Ru1 Ru3 Ru2 -61.56(13) . . . . ? C2 Ru1 Ru3 Ru2 -57.40(10) . . . . ? C22 Ru2 Ru3 C31 -37.0(5) . . . . ? C21 Ru2 Ru3 C31 -119.4(4) . . . . ? C3 Ru2 Ru3 C31 123.6(4) . . . . ? C1 Ru2 Ru3 C31 28.0(4) . . . . ? C2 Ru2 Ru3 C31 17.9(4) . . . . ? C4 Ru2 Ru3 C31 109.9(4) . . . . ? Ru1 Ru2 Ru3 C31 -37.9(4) . . . . ? Ru4 Ru2 Ru3 C31 167.6(4) . . . . ? Ru5 Ru2 Ru3 C31 154.1(4) . . . . ? C22 Ru2 Ru3 C32 83.2(4) . . . . ? C21 Ru2 Ru3 C32 0.8(2) . . . . ? C3 Ru2 Ru3 C32 -116.22(19) . . . . ? C1 Ru2 Ru3 C32 148.2(2) . . . . ? C2 Ru2 Ru3 C32 138.07(19) . . . . ? C4 Ru2 Ru3 C32 -129.9(2) . . . . ? Ru1 Ru2 Ru3 C32 82.34(15) . . . . ? Ru4 Ru2 Ru3 C32 -72.15(15) . . . . ? Ru5 Ru2 Ru3 C32 -85.66(15) . . . . ? C22 Ru2 Ru3 C1 -65.0(4) . . . . ? C21 Ru2 Ru3 C1 -147.4(2) . . . . ? C3 Ru2 Ru3 C1 95.6(2) . . . . ? C2 Ru2 Ru3 C1 -10.1(2) . . . . ? C4 Ru2 Ru3 C1 81.9(2) . . . . ? Ru1 Ru2 Ru3 C1 -65.88(17) . . . . ? Ru4 Ru2 Ru3 C1 139.63(17) . . . . ? Ru5 Ru2 Ru3 C1 126.13(17) . . . . ? C22 Ru2 Ru3 C5 -155.4(4) . . . . ? C21 Ru2 Ru3 C5 122.19(18) . . . . ? C3 Ru2 Ru3 C5 5.14(17) . . . . ? C1 Ru2 Ru3 C5 -90.4(2) . . . . ? C2 Ru2 Ru3 C5 -100.57(18) . . . . ? C4 Ru2 Ru3 C5 -8.52(18) . . . . ? Ru1 Ru2 Ru3 C5 -156.30(13) . . . . ? Ru4 Ru2 Ru3 C5 49.20(13) . . . . ? Ru5 Ru2 Ru3 C5 35.70(13) . . . . ? C22 Ru2 Ru3 C6 172.8(4) . . . . ? C21 Ru2 Ru3 C6 90.4(2) . . . . ? C3 Ru2 Ru3 C6 -26.67(19) . . . . ? C1 Ru2 Ru3 C6 -122.2(2) . . . . ? C2 Ru2 Ru3 C6 -132.38(19) . . . . ? C4 Ru2 Ru3 C6 -40.34(19) . . . . ? Ru1 Ru2 Ru3 C6 171.88(15) . . . . ? Ru4 Ru2 Ru3 C6 17.39(15) . . . . ? Ru5 Ru2 Ru3 C6 3.88(15) . . . . ? C22 Ru2 Ru3 Ru1 0.9(3) . . . . ? C21 Ru2 Ru3 Ru1 -81.50(13) . . . . ? C3 Ru2 Ru3 Ru1 161.45(11) . . . . ? C1 Ru2 Ru3 Ru1 65.88(17) . . . . ? C2 Ru2 Ru3 Ru1 55.74(12) . . . . ? C4 Ru2 Ru3 Ru1 147.78(12) . . . . ? Ru4 Ru2 Ru3 Ru1 -154.49(2) . . . . ? Ru5 Ru2 Ru3 Ru1 -167.995(19) . . . . ? C22 Ru2 Ru3 Ru5 168.9(3) . . . . ? C21 Ru2 Ru3 Ru5 86.49(13) . . . . ? C3 Ru2 Ru3 Ru5 -30.56(11) . . . . ? C1 Ru2 Ru3 Ru5 -126.13(17) . . . . ? C2 Ru2 Ru3 Ru5 -136.27(12) . . . . ? C4 Ru2 Ru3 Ru5 -44.23(12) . . . . ? Ru1 Ru2 Ru3 Ru5 167.995(19) . . . . ? Ru4 Ru2 Ru3 Ru5 13.504(18) . . . . ? O42 C42 Ru4 C41 -144(18) . . . . ? O42 C42 Ru4 C43 122(18) . . . . ? O42 C42 Ru4 C3 -5(18) . . . . ? O42 C42 Ru4 C4 30(18) . . . . ? O42 C42 Ru4 Ru2 0(19) . . . . ? O42 C42 Ru4 Ru5 -50(18) . . . . ? O41 C41 Ru4 C42 -51(9) . . . . ? O41 C41 Ru4 C43 43(9) . . . . ? O41 C41 Ru4 C3 -158(9) . . . . ? O41 C41 Ru4 C4 155(9) . . . . ? O41 C41 Ru4 Ru2 146(9) . . . . ? O41 C41 Ru4 Ru5 -147(9) . . . . ? O43 C43 Ru4 C42 52(17) . . . . ? O43 C43 Ru4 C41 -41(17) . . . . ? O43 C43 Ru4 C3 156(17) . . . . ? O43 C43 Ru4 C4 152(17) . . . . ? O43 C43 Ru4 Ru2 -152(17) . . . . ? O43 C43 Ru4 Ru5 -17E1(10) . . . . ? C4 C3 Ru4 C42 95.2(3) . . . . ? Ru5 C3 Ru4 C42 -89.16(19) . . . . ? Ru2 C3 Ru4 C42 177.05(17) . . . . ? C4 C3 Ru4 C41 -160.4(3) . . . . ? Ru5 C3 Ru4 C41 15.2(3) . . . . ? Ru2 C3 Ru4 C41 -78.6(3) . . . . ? C4 C3 Ru4 C43 -6.4(3) . . . . ? Ru5 C3 Ru4 C43 169.17(18) . . . . ? Ru2 C3 Ru4 C43 75.4(2) . . . . ? Ru5 C3 Ru4 C4 175.6(3) . . . . ? Ru2 C3 Ru4 C4 81.8(2) . . . . ? C4 C3 Ru4 Ru2 -81.8(2) . . . . ? Ru5 C3 Ru4 Ru2 93.79(13) . . . . ? C4 C3 Ru4 Ru5 -175.6(3) . . . . ? Ru2 C3 Ru4 Ru5 -93.79(13) . . . . ? C3 C4 Ru4 C42 -90.8(3) . . . . ? Si2 C4 Ru4 C42 57.9(3) . . . . ? Ru2 C4 Ru4 C42 -163.99(16) . . . . ? C3 C4 Ru4 C41 62.8(8) . . . . ? Si2 C4 Ru4 C41 -148.5(6) . . . . ? Ru2 C4 Ru4 C41 -10.4(8) . . . . ? C3 C4 Ru4 C43 174.7(3) . . . . ? Si2 C4 Ru4 C43 -36.6(3) . . . . ? Ru2 C4 Ru4 C43 101.54(16) . . . . ? Si2 C4 Ru4 C3 148.7(4) . . . . ? Ru2 C4 Ru4 C3 -73.2(2) . . . . ? C3 C4 Ru4 Ru2 73.2(2) . . . . ? Si2 C4 Ru4 Ru2 -138.1(3) . . . . ? C3 C4 Ru4 Ru5 3.1(2) . . . . ? Si2 C4 Ru4 Ru5 151.8(3) . . . . ? Ru2 C4 Ru4 Ru5 -70.05(7) . . . . ? C22 Ru2 Ru4 C42 122.1(4) . . . . ? C21 Ru2 Ru4 C42 -146.1(4) . . . . ? C3 Ru2 Ru4 C42 -6.2(4) . . . . ? C1 Ru2 Ru4 C42 -29.1(4) . . . . ? C2 Ru2 Ru4 C42 25.5(4) . . . . ? C4 Ru2 Ru4 C42 35.4(4) . . . . ? Ru1 Ru2 Ru4 C42 -132.9(3) . . . . ? Ru3 Ru2 Ru4 C42 -69.5(3) . . . . ? Ru5 Ru2 Ru4 C42 -56.0(3) . . . . ? C22 Ru2 Ru4 C41 -96.1(2) . . . . ? C21 Ru2 Ru4 C41 -4.3(2) . . . . ? C3 Ru2 Ru4 C41 135.6(2) . . . . ? C1 Ru2 Ru4 C41 112.8(2) . . . . ? C2 Ru2 Ru4 C41 167.4(3) . . . . ? C4 Ru2 Ru4 C41 177.2(2) . . . . ? Ru1 Ru2 Ru4 C41 8.93(16) . . . . ? Ru3 Ru2 Ru4 C41 72.30(16) . . . . ? Ru5 Ru2 Ru4 C41 85.80(16) . . . . ? C22 Ru2 Ru4 C43 1.8(2) . . . . ? C21 Ru2 Ru4 C43 93.6(2) . . . . ? C3 Ru2 Ru4 C43 -126.5(2) . . . . ? C1 Ru2 Ru4 C43 -149.3(2) . . . . ? C2 Ru2 Ru4 C43 -94.7(3) . . . . ? C4 Ru2 Ru4 C43 -84.9(2) . . . . ? Ru1 Ru2 Ru4 C43 106.82(18) . . . . ? Ru3 Ru2 Ru4 C43 170.19(17) . . . . ? Ru5 Ru2 Ru4 C43 -176.31(17) . . . . ? C22 Ru2 Ru4 C3 128.3(2) . . . . ? C21 Ru2 Ru4 C3 -139.88(19) . . . . ? C1 Ru2 Ru4 C3 -22.8(2) . . . . ? C2 Ru2 Ru4 C3 31.8(3) . . . . ? C4 Ru2 Ru4 C3 41.62(18) . . . . ? Ru1 Ru2 Ru4 C3 -126.68(14) . . . . ? Ru3 Ru2 Ru4 C3 -63.30(14) . . . . ? Ru5 Ru2 Ru4 C3 -49.80(14) . . . . ? C22 Ru2 Ru4 C4 86.7(2) . . . . ? C21 Ru2 Ru4 C4 178.50(19) . . . . ? C3 Ru2 Ru4 C4 -41.62(18) . . . . ? C1 Ru2 Ru4 C4 -64.4(2) . . . . ? C2 Ru2 Ru4 C4 -9.9(2) . . . . ? Ru1 Ru2 Ru4 C4 -168.29(13) . . . . ? Ru3 Ru2 Ru4 C4 -104.92(13) . . . . ? Ru5 Ru2 Ru4 C4 -91.42(13) . . . . ? C22 Ru2 Ru4 Ru5 178.08(17) . . . . ? C21 Ru2 Ru4 Ru5 -90.08(14) . . . . ? C3 Ru2 Ru4 Ru5 49.80(13) . . . . ? C1 Ru2 Ru4 Ru5 26.97(18) . . . . ? C2 Ru2 Ru4 Ru5 81.6(2) . . . . ? C4 Ru2 Ru4 Ru5 91.42(13) . . . . ? Ru1 Ru2 Ru4 Ru5 -76.88(4) . . . . ? Ru3 Ru2 Ru4 Ru5 -13.498(17) . . . . ? O52 C52 Ru5 C51 -4E1(4) . . . . ? O52 C52 Ru5 C3 18E1(10) . . . . ? O52 C52 Ru5 C5 8E1(4) . . . . ? O52 C52 Ru5 C6 5E1(4) . . . . ? O52 C52 Ru5 Ru4 -13E1(4) . . . . ? O52 C52 Ru5 Ru3 7E1(4) . . . . ? O52 C52 Ru5 Ru2 -17E1(10) . . . . ? O51 C51 Ru5 C52 -58(8) . . . . ? O51 C51 Ru5 C3 49(8) . . . . ? O51 C51 Ru5 C5 -159(8) . . . . ? O51 C51 Ru5 C6 -158(8) . . . . ? O51 C51 Ru5 Ru4 39(8) . . . . ? O51 C51 Ru5 Ru3 155(8) . . . . ? O51 C51 Ru5 Ru2 94(8) . . . . ? C4 C3 Ru5 C52 105.8(10) . . . . ? Ru4 C3 Ru5 C52 93.06(19) . . . . ? Ru2 C3 Ru5 C52 168.76(18) . . . . ? C4 C3 Ru5 C51 1.1(11) . . . . ? Ru4 C3 Ru5 C51 -11.7(3) . . . . ? Ru2 C3 Ru5 C51 64.0(3) . . . . ? C4 C3 Ru5 C5 -154.7(9) . . . . ? Ru4 C3 Ru5 C5 -167.44(14) . . . . ? Ru2 C3 Ru5 C5 -91.74(16) . . . . ? C4 C3 Ru5 C6 -144.5(9) . . . . ? Ru4 C3 Ru5 C6 -157.18(16) . . . . ? Ru2 C3 Ru5 C6 -81.5(2) . . . . ? C4 C3 Ru5 Ru4 12.7(9) . . . . ? Ru2 C3 Ru5 Ru4 75.70(13) . . . . ? C4 C3 Ru5 Ru3 -106.1(9) . . . . ? Ru4 C3 Ru5 Ru3 -118.82(9) . . . . ? Ru2 C3 Ru5 Ru3 -43.12(11) . . . . ? C4 C3 Ru5 Ru2 -63.0(9) . . . . ? Ru4 C3 Ru5 Ru2 -75.70(13) . . . . ? C6 C5 Ru5 C52 -94.6(3) . . . . ? Si4 C5 Ru5 C52 54.2(3) . . . . ? Ru3 C5 Ru5 C52 -169.75(18) . . . . ? C6 C5 Ru5 C51 1.7(4) . . . . ? Si4 C5 Ru5 C51 150.5(3) . . . . ? Ru3 C5 Ru5 C51 -73.4(2) . . . . ? C6 C5 Ru5 C3 165.7(3) . . . . ? Si4 C5 Ru5 C3 -45.5(3) . . . . ? Ru3 C5 Ru5 C3 90.60(16) . . . . ? Si4 C5 Ru5 C6 148.8(4) . . . . ? Ru3 C5 Ru5 C6 -75.1(3) . . . . ? C6 C5 Ru5 Ru4 148.9(2) . . . . ? Si4 C5 Ru5 Ru4 -62.3(4) . . . . ? Ru3 C5 Ru5 Ru4 73.7(2) . . . . ? C6 C5 Ru5 Ru3 75.1(3) . . . . ? Si4 C5 Ru5 Ru3 -136.1(3) . . . . ? C6 C5 Ru5 Ru2 118.2(3) . . . . ? Si4 C5 Ru5 Ru2 -93.0(3) . . . . ? Ru3 C5 Ru5 Ru2 43.04(12) . . . . ? C5 C6 Ru5 C52 91.1(3) . . . . ? Si3 C6 Ru5 C52 -49.9(4) . . . . ? Ru3 C6 Ru5 C52 164.4(2) . . . . ? C5 C6 Ru5 C51 -178.5(3) . . . . ? Si3 C6 Ru5 C51 40.5(4) . . . . ? Ru3 C6 Ru5 C51 -105.2(2) . . . . ? C5 C6 Ru5 C3 -18.2(4) . . . . ? Si3 C6 Ru5 C3 -159.3(3) . . . . ? Ru3 C6 Ru5 C3 55.0(3) . . . . ? Si3 C6 Ru5 C5 -141.0(5) . . . . ? Ru3 C6 Ru5 C5 73.3(3) . . . . ? C5 C6 Ru5 Ru4 -99.4(5) . . . . ? Si3 C6 Ru5 Ru4 119.6(3) . . . . ? Ru3 C6 Ru5 Ru4 -26.2(5) . . . . ? C5 C6 Ru5 Ru3 -73.3(3) . . . . ? Si3 C6 Ru5 Ru3 145.7(5) . . . . ? C5 C6 Ru5 Ru2 -68.8(3) . . . . ? Si3 C6 Ru5 Ru2 150.2(3) . . . . ? Ru3 C6 Ru5 Ru2 4.45(17) . . . . ? C42 Ru4 Ru5 C52 2.2(3) . . . . ? C41 Ru4 Ru5 C52 95.3(2) . . . . ? C43 Ru4 Ru5 C52 -138.4(8) . . . . ? C3 Ru4 Ru5 C52 -94.9(2) . . . . ? C4 Ru4 Ru5 C52 -97.4(2) . . . . ? Ru2 Ru4 Ru5 C52 -154.85(18) . . . . ? C42 Ru4 Ru5 C51 -89.8(2) . . . . ? C41 Ru4 Ru5 C51 3.3(2) . . . . ? C43 Ru4 Ru5 C51 129.7(8) . . . . ? C3 Ru4 Ru5 C51 173.1(2) . . . . ? C4 Ru4 Ru5 C51 170.64(18) . . . . ? Ru2 Ru4 Ru5 C51 113.18(15) . . . . ? C42 Ru4 Ru5 C3 97.1(2) . . . . ? C41 Ru4 Ru5 C3 -169.8(2) . . . . ? C43 Ru4 Ru5 C3 -43.4(8) . . . . ? C4 Ru4 Ru5 C3 -2.48(18) . . . . ? Ru2 Ru4 Ru5 C3 -59.94(14) . . . . ? C42 Ru4 Ru5 C5 118.9(3) . . . . ? C41 Ru4 Ru5 C5 -148.0(3) . . . . ? C43 Ru4 Ru5 C5 -21.6(8) . . . . ? C3 Ru4 Ru5 C5 21.8(3) . . . . ? C4 Ru4 Ru5 C5 19.3(2) . . . . ? Ru2 Ru4 Ru5 C5 -38.1(2) . . . . ? C42 Ru4 Ru5 C6 -167.4(5) . . . . ? C41 Ru4 Ru5 C6 -74.3(5) . . . . ? C43 Ru4 Ru5 C6 52.1(9) . . . . ? C3 Ru4 Ru5 C6 95.5(5) . . . . ? C4 Ru4 Ru5 C6 93.1(4) . . . . ? Ru2 Ru4 Ru5 C6 35.6(4) . . . . ? C42 Ru4 Ru5 Ru3 171.14(19) . . . . ? C41 Ru4 Ru5 Ru3 -95.77(15) . . . . ? C43 Ru4 Ru5 Ru3 30.6(7) . . . . ? C3 Ru4 Ru5 Ru3 74.05(14) . . . . ? C4 Ru4 Ru5 Ru3 71.57(11) . . . . ? Ru2 Ru4 Ru5 Ru3 14.114(18) . . . . ? C42 Ru4 Ru5 Ru2 157.02(19) . . . . ? C41 Ru4 Ru5 Ru2 -109.88(15) . . . . ? C43 Ru4 Ru5 Ru2 16.5(7) . . . . ? C3 Ru4 Ru5 Ru2 59.94(14) . . . . ? C4 Ru4 Ru5 Ru2 57.46(11) . . . . ? C31 Ru3 Ru5 C52 -7.5(5) . . . . ? C32 Ru3 Ru5 C52 -108.1(3) . . . . ? C1 Ru3 Ru5 C52 109.4(3) . . . . ? C5 Ru3 Ru5 C52 18.3(3) . . . . ? C6 Ru3 Ru5 C52 -28.2(3) . . . . ? Ru1 Ru3 Ru5 C52 158.0(3) . . . . ? Ru2 Ru3 Ru5 C52 146.9(3) . . . . ? C31 Ru3 Ru5 C51 95.6(4) . . . . ? C32 Ru3 Ru5 C51 -5.0(2) . . . . ? C1 Ru3 Ru5 C51 -147.5(2) . . . . ? C5 Ru3 Ru5 C51 121.3(2) . . . . ? C6 Ru3 Ru5 C51 74.9(2) . . . . ? Ru1 Ru3 Ru5 C51 -98.88(15) . . . . ? Ru2 Ru3 Ru5 C51 -109.96(15) . . . . ? C31 Ru3 Ru5 C3 -119.2(4) . . . . ? C32 Ru3 Ru5 C3 140.3(2) . . . . ? C1 Ru3 Ru5 C3 -2.27(18) . . . . ? C5 Ru3 Ru5 C3 -93.4(2) . . . . ? C6 Ru3 Ru5 C3 -139.9(2) . . . . ? Ru1 Ru3 Ru5 C3 46.33(13) . . . . ? Ru2 Ru3 Ru5 C3 35.25(13) . . . . ? C31 Ru3 Ru5 C5 -25.8(4) . . . . ? C32 Ru3 Ru5 C5 -126.3(2) . . . . ? C1 Ru3 Ru5 C5 91.2(2) . . . . ? C6 Ru3 Ru5 C5 -46.5(2) . . . . ? Ru1 Ru3 Ru5 C5 139.78(17) . . . . ? Ru2 Ru3 Ru5 C5 128.70(17) . . . . ? C31 Ru3 Ru5 C6 20.7(4) . . . . ? C32 Ru3 Ru5 C6 -79.8(2) . . . . ? C1 Ru3 Ru5 C6 137.7(2) . . . . ? C5 Ru3 Ru5 C6 46.5(2) . . . . ? Ru1 Ru3 Ru5 C6 -173.73(19) . . . . ? Ru2 Ru3 Ru5 C6 175.19(19) . . . . ? C31 Ru3 Ru5 Ru4 -167.8(4) . . . . ? C32 Ru3 Ru5 Ru4 91.67(16) . . . . ? C1 Ru3 Ru5 Ru4 -50.86(13) . . . . ? C5 Ru3 Ru5 Ru4 -142.03(17) . . . . ? C6 Ru3 Ru5 Ru4 171.48(19) . . . . ? Ru1 Ru3 Ru5 Ru4 -2.25(3) . . . . ? Ru2 Ru3 Ru5 Ru4 -13.330(17) . . . . ? C31 Ru3 Ru5 Ru2 -154.5(4) . . . . ? C32 Ru3 Ru5 Ru2 105.00(16) . . . . ? C1 Ru3 Ru5 Ru2 -37.53(13) . . . . ? C5 Ru3 Ru5 Ru2 -128.70(17) . . . . ? C6 Ru3 Ru5 Ru2 -175.19(19) . . . . ? Ru1 Ru3 Ru5 Ru2 11.079(18) . . . . ? C22 Ru2 Ru5 C52 42.9(4) . . . . ? C21 Ru2 Ru5 C52 126.0(3) . . . . ? C3 Ru2 Ru5 C52 -19.5(3) . . . . ? C1 Ru2 Ru5 C52 -115.9(3) . . . . ? C2 Ru2 Ru5 C52 -101.8(3) . . . . ? C4 Ru2 Ru5 C52 -9.5(3) . . . . ? Ru1 Ru2 Ru5 C52 -159.1(3) . . . . ? Ru4 Ru2 Ru5 C52 46.8(3) . . . . ? Ru3 Ru2 Ru5 C52 -148.0(3) . . . . ? C22 Ru2 Ru5 C51 -82.9(4) . . . . ? C21 Ru2 Ru5 C51 0.26(17) . . . . ? C3 Ru2 Ru5 C51 -145.2(2) . . . . ? C1 Ru2 Ru5 C51 118.28(17) . . . . ? C2 Ru2 Ru5 C51 132.46(18) . . . . ? C4 Ru2 Ru5 C51 -135.30(17) . . . . ? Ru1 Ru2 Ru5 C51 75.08(13) . . . . ? Ru4 Ru2 Ru5 C51 -79.01(13) . . . . ? Ru3 Ru2 Ru5 C51 86.25(13) . . . . ? C22 Ru2 Ru5 C3 62.3(4) . . . . ? C21 Ru2 Ru5 C3 145.51(19) . . . . ? C1 Ru2 Ru5 C3 -96.47(19) . . . . ? C2 Ru2 Ru5 C3 -82.29(19) . . . . ? C4 Ru2 Ru5 C3 9.95(19) . . . . ? Ru1 Ru2 Ru5 C3 -139.67(16) . . . . ? Ru4 Ru2 Ru5 C3 66.24(15) . . . . ? Ru3 Ru2 Ru5 C3 -128.50(15) . . . . ? C22 Ru2 Ru5 C5 154.9(4) . . . . ? C21 Ru2 Ru5 C5 -121.89(17) . . . . ? C3 Ru2 Ru5 C5 92.6(2) . . . . ? C1 Ru2 Ru5 C5 -3.87(17) . . . . ? C2 Ru2 Ru5 C5 10.31(17) . . . . ? C4 Ru2 Ru5 C5 102.55(17) . . . . ? Ru1 Ru2 Ru5 C5 -47.07(13) . . . . ? Ru4 Ru2 Ru5 C5 158.84(13) . . . . ? Ru3 Ru2 Ru5 C5 -35.90(13) . . . . ? C22 Ru2 Ru5 C6 -173.0(4) . . . . ? C21 Ru2 Ru5 C6 -89.85(19) . . . . ? C3 Ru2 Ru5 C6 124.6(2) . . . . ? C1 Ru2 Ru5 C6 28.17(19) . . . . ? C2 Ru2 Ru5 C6 42.36(19) . . . . ? C4 Ru2 Ru5 C6 134.59(19) . . . . ? Ru1 Ru2 Ru5 C6 -15.03(15) . . . . ? Ru4 Ru2 Ru5 C6 -169.12(15) . . . . ? Ru3 Ru2 Ru5 C6 -3.86(15) . . . . ? C22 Ru2 Ru5 Ru4 -3.9(3) . . . . ? C21 Ru2 Ru5 Ru4 79.27(11) . . . . ? C3 Ru2 Ru5 Ru4 -66.24(15) . . . . ? C1 Ru2 Ru5 Ru4 -162.71(11) . . . . ? C2 Ru2 Ru5 Ru4 -148.52(12) . . . . ? C4 Ru2 Ru5 Ru4 -56.29(11) . . . . ? Ru1 Ru2 Ru5 Ru4 154.09(2) . . . . ? Ru3 Ru2 Ru5 Ru4 165.260(19) . . . . ? C22 Ru2 Ru5 Ru3 -169.2(3) . . . . ? C21 Ru2 Ru5 Ru3 -85.99(11) . . . . ? C3 Ru2 Ru5 Ru3 128.50(15) . . . . ? C1 Ru2 Ru5 Ru3 32.03(11) . . . . ? C2 Ru2 Ru5 Ru3 46.21(12) . . . . ? C4 Ru2 Ru5 Ru3 138.45(11) . . . . ? Ru1 Ru2 Ru5 Ru3 -11.170(18) . . . . ? Ru4 Ru2 Ru5 Ru3 -165.260(19) . . . . ? C1 C2 Si1 C9 165.1(7) . . . . ? Ru1 C2 Si1 C9 -85.0(4) . . . . ? Ru2 C2 Si1 C9 18.8(5) . . . . ? C1 C2 Si1 C8 -74.9(7) . . . . ? Ru1 C2 Si1 C8 34.9(4) . . . . ? Ru2 C2 Si1 C8 138.7(4) . . . . ? C1 C2 Si1 C7 40.6(7) . . . . ? Ru1 C2 Si1 C7 150.4(3) . . . . ? Ru2 C2 Si1 C7 -105.7(4) . . . . ? C3 C4 Si2 C15 -54.2(8) . . . . ? Ru4 C4 Si2 C15 -166.7(4) . . . . ? Ru2 C4 Si2 C15 87.5(5) . . . . ? C3 C4 Si2 C14 65.8(7) . . . . ? Ru4 C4 Si2 C14 -46.8(5) . . . . ? Ru2 C4 Si2 C14 -152.5(4) . . . . ? C3 C4 Si2 C16 -176.3(7) . . . . ? Ru4 C4 Si2 C16 71.2(4) . . . . ? Ru2 C4 Si2 C16 -34.6(5) . . . . ? C5 C6 Si3 C19 50.9(6) . . . . ? Ru5 C6 Si3 C19 166.2(4) . . . . ? Ru3 C6 Si3 C19 -63.6(5) . . . . ? C5 C6 Si3 C18 -69.4(6) . . . . ? Ru5 C6 Si3 C18 45.9(6) . . . . ? Ru3 C6 Si3 C18 176.0(5) . . . . ? C5 C6 Si3 C17 168.9(5) . . . . ? Ru5 C6 Si3 C17 -75.8(4) . . . . ? Ru3 C6 Si3 C17 54.3(4) . . . . ? C6 C5 Si4 C25 174.8(6) . . . . ? Ru5 C5 Si4 C25 54.0(4) . . . . ? Ru3 C5 Si4 C25 -63.1(4) . . . . ? C6 C5 Si4 C23 48.6(6) . . . . ? Ru5 C5 Si4 C23 -72.1(4) . . . . ? Ru3 C5 Si4 C23 170.8(3) . . . . ? C6 C5 Si4 C24 -65.9(7) . . . . ? Ru5 C5 Si4 C24 173.3(4) . . . . ? Ru3 C5 Si4 C24 56.2(4) . . . . ? C100 C100 C101 C102 167.3(14) 2_656 . . . ? data_mrvian28 _database_code_depnum_ccdc_archive 'CCDC 903654' #TrackingRef 'compound 3a.cif' _audit_creation_date 2012-12-11T15:58:08-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.4 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common compound3a _chemical_formula_moiety 'C25 H15 O9 Ru3 Si1' _chemical_formula_sum 'C22 H30 O8 Ru3 Si3' _chemical_formula_weight 809.94 _chemical_compound_source 'synthesis as described' _chemical_absolute_configuration unk #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _space_group_crystal_system orthorhombic _space_group_name_H-M_alt 'P 21 21 21' _space_group_name_Hall 'P 2ac 2ab' _space_group_IT_number 19 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M P212121 _symmetry_space_group_name_Hall 'P 2ac 2ab' _symmetry_Int_Tables_number 19 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 9.2297(6) _cell_length_b 18.2204(13) _cell_length_c 18.5059(13) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 3112.1(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 600 _cell_measurement_theta_min 1 _cell_measurement_theta_max 14 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 1.729 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1600 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.591 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.7151 _exptl_absorpt_correction_T_max 0.782 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 9 _diffrn_orient_matrix_type 'by Bruker AXS Collect from scalepack cell' _diffrn_orient_matrix_ub_11 -0.208712E-1 _diffrn_orient_matrix_ub_12 -0.375E-4 _diffrn_orient_matrix_ub_13 -0.530247E-1 _diffrn_orient_matrix_ub_21 -0.106317 _diffrn_orient_matrix_ub_22 0.31E-5 _diffrn_orient_matrix_ub_23 0.104094E-1 _diffrn_orient_matrix_ub_31 -0.83E-5 _diffrn_orient_matrix_ub_32 0.548835E-1 _diffrn_orient_matrix_ub_33 -0.368E-4 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.1791 _diffrn_reflns_number 21413 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.138 _diffrn_reflns_theta_max 27.653 _diffrn_reflns_theta_full 25 _diffrn_measured_fraction_theta_full 0.983 _diffrn_measured_fraction_theta_max 0.873 _diffrn_reflns_Laue_measured_fraction_full 0.983 _diffrn_reflns_Laue_measured_fraction_max 0.873 _diffrn_reflns_point_group_measured_fraction_ful 0.965 _diffrn_reflns_point_group_measured_fraction_max 0.85 _reflns_number_total 6152 _reflns_number_gt 3624 _reflns_threshold_expression 'I > 2\s(I)' _diffrn_reflns_reduction_process ; Scaled and merged with Sortav R.H. Blessing, (1987) Cryst. Rev. 1, 3-58 R.H. Blessing, (1989) J. Appl. Cryst. 22, 396-397 ; #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-1997 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-2012 (Sheldrick, 2012)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; ? ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; w=1/[\s^2^(Fo^2^)+3.4053P] where P=(Fo^2^+2Fc^2^)/3 ; _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 6152 _refine_ls_number_parameters 342 _refine_ls_number_restraints 64 _refine_ls_R_factor_all 0.1421 _refine_ls_R_factor_gt 0.0697 _refine_ls_wR_factor_ref 0.1147 _refine_ls_wR_factor_gt 0.0948 _refine_ls_goodness_of_fit_ref 1.115 _refine_ls_restrained_S_all 1.114 _refine_ls_shift/su_max 0.013 _refine_ls_shift/su_mean 0 _refine_ls_abs_structure_details ; Flack x determined using 1052 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons and Flack (2004), Acta Cryst. A60, s61). ; _refine_ls_abs_structure_Flack 0.04(7) _refine_diff_density_max 0.491 _refine_diff_density_min -0.646 _refine_diff_density_rms 0.117 #----------------------------------------------------------------------------# # 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' O O 0.0106 0.006 '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' Si Si 0.0817 0.0704 '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_calc_flag _atom_site_disorder_assembly _atom_site_disorder_group C4 C 0.5223(16) 0.3998(8) 0.1774(7) 0.047(4) Uani 1 d . . C3 C 0.6164(15) 0.3409(8) 0.2052(7) 0.046(3) Uani 1 d . . C2 C 0.6075(19) 0.3299(9) 0.2855(7) 0.064(4) Uani 1 d . . C1 C 0.5128(14) 0.3809(8) 0.3228(7) 0.043(4) Uani 1 d . . C7 C 0.688(2) 0.2670(12) 0.3214(9) 0.106(8) Uani 1 d . . H7C H 0.6737 0.2228 0.2941 0.159 Uiso 1 calc . . H7B H 0.6522 0.2602 0.3696 0.159 Uiso 1 calc . . H7A H 0.7898 0.2782 0.3232 0.159 Uiso 1 calc . . C15 C 0.2778(17) 0.4318(11) 0.0688(9) 0.082(5) Uani 1 d . . H15A H 0.2325 0.3991 0.1026 0.123 Uiso 1 calc . . H15C H 0.2556 0.4164 0.0204 0.123 Uiso 1 calc . . H15B H 0.2423 0.4807 0.0762 0.123 Uiso 1 calc . . C16 C 0.552(2) 0.5240(9) 0.0697(9) 0.087(5) Uani 1 d . . H16C H 0.5345 0.5524 0.1125 0.13 Uiso 1 calc . . H16B H 0.5047 0.5469 0.0293 0.13 Uiso 1 calc . . H16A H 0.6539 0.521 0.0608 0.13 Uiso 1 calc . . C17 C 0.536(2) 0.3747(11) 0.0021(8) 0.104(6) Uani 1 d . . H17A H 0.4892 0.3276 0.0036 0.155 Uiso 1 calc . . H17B H 0.6387 0.3684 0.0032 0.155 Uiso 1 calc . . H17C H 0.5084 0.3998 -0.0414 0.155 Uiso 1 calc . . C9 C 0.6429(16) 0.2168(9) 0.0922(9) 0.083(5) Uani 1 d . . H9A H 0.6071 0.1798 0.1246 0.124 Uiso 1 calc . . H9B H 0.7036 0.1943 0.0564 0.124 Uiso 1 calc . . H9C H 0.5628 0.2407 0.069 0.124 Uiso 1 calc . . C10 C 0.8555(15) 0.3478(9) 0.0885(8) 0.073(5) Uani 1 d . . H10A H 0.924 0.3732 0.1185 0.11 Uiso 1 calc . . H10B H 0.7923 0.3827 0.0658 0.11 Uiso 1 calc . . H10C H 0.9064 0.3206 0.052 0.11 Uiso 1 calc . . C11 C 0.8902(17) 0.2310(10) 0.1939(9) 0.086(5) Uani 1 d . . H11A H 0.9324 0.2611 0.2308 0.13 Uiso 1 calc . . H11B H 0.9643 0.2155 0.1608 0.13 Uiso 1 calc . . H11C H 0.846 0.1887 0.2156 0.13 Uiso 1 calc . . C12 C 0.5648(17) 0.5408(9) 0.2769(9) 0.069(5) Uani 1 d . . C13 C 0.8160(18) 0.4587(15) 0.3312(9) 0.101(7) Uani 1 d . . C14 C 0.818(2) 0.4943(11) 0.1995(9) 0.075(5) Uani 1 d . . C8 C 0.541(2) 0.4793(12) 0.4587(9) 0.109(8) Uani 1 d . . H8A H 0.546 0.4785 0.5105 0.163 Uiso 1 calc . . H8C H 0.4699 0.5146 0.4436 0.163 Uiso 1 calc . . H8B H 0.6339 0.4926 0.4393 0.163 Uiso 1 calc . . C5A C 0.627(10) 0.332(5) 0.477(2) 0.11(2) Uani 0.50(15) d A 1 H5A1 H 0.722 0.3469 0.4619 0.163 Uiso 0.50(15) calc A 1 H5A2 H 0.6147 0.2805 0.4684 0.163 Uiso 0.50(15) calc A 1 H5A3 H 0.6148 0.3421 0.5275 0.163 Uiso 0.50(15) calc A 1 C5B C 0.569(12) 0.312(4) 0.484(3) 0.15(3) Uani 0.50(15) d A 2 H5B1 H 0.6722 0.314 0.4804 0.226 Uiso 0.50(15) calc A 2 H5B2 H 0.535 0.2647 0.4687 0.226 Uiso 0.50(15) calc A 2 H5B3 H 0.5397 0.3207 0.533 0.226 Uiso 0.50(15) calc A 2 C6 C 0.295(2) 0.3643(11) 0.4462(10) 0.104(6) Uani 1 d . . H6A H 0.2771 0.3127 0.4408 0.156 Uiso 1 calc . . H6B H 0.2328 0.3912 0.414 0.156 Uiso 1 calc . . H6C H 0.2751 0.3787 0.4951 0.156 Uiso 1 calc . . C21 C 0.3054(18) 0.5330(10) 0.2011(9) 0.064(5) Uani 1 d . . C22 C 0.2852(16) 0.5078(9) 0.3370(8) 0.056(4) Uani 1 d . . C23 C 0.2133(16) 0.3868(7) 0.2491(10) 0.062(4) Uani 1 d . . C31 C 0.3002(17) 0.2675(9) 0.1610(9) 0.059(4) Uani 1 d . . C32 C 0.301(2) 0.2393(11) 0.2967(10) 0.089(6) Uani 1 d . . O12 O 0.5752(13) 0.6018(8) 0.2902(7) 0.097(4) Uani 1 d . . O13A O 0.903(3) 0.483(3) 0.3730(16) 0.097(4) Uani 0.54(5) d B 1 O13B O 0.900(3) 0.445(3) 0.3792(16) 0.097(4) Uani 0.46(5) d B 2 O14 O 0.9015(14) 0.5244(8) 0.1650(7) 0.105(5) Uani 1 d . . O21 O 0.2514(15) 0.5812(8) 0.1703(8) 0.111(5) Uani 1 d . . O22 O 0.2152(12) 0.5368(8) 0.3767(7) 0.089(4) Uani 1 d . . O23 O 0.0885(10) 0.3916(6) 0.2510(8) 0.090(4) Uani 1 d . . O31 O 0.2542(14) 0.2350(8) 0.1117(8) 0.104(5) Uani 1 d . . O32 O 0.256(2) 0.1951(9) 0.3307(9) 0.142(7) Uani 1 d . . Ru1 Ru 0.68051(11) 0.44860(7) 0.25978(7) 0.0563(4) Uani 1 d . . Ru2 Ru 0.39274(11) 0.46276(6) 0.26055(6) 0.0480(3) Uani 1 d . . Ru3 Ru 0.37983(11) 0.31775(6) 0.23801(7) 0.0528(3) Uani 1 d . . Si3 Si 0.4774(5) 0.4302(3) 0.0823(2) 0.0612(13) Uani 1 d . . Si2 Si 0.7491(4) 0.2851(3) 0.1437(3) 0.0572(12) Uani 1 d . . Si1 Si 0.4879(6) 0.3845(4) 0.4242(3) 0.0851(18) Uani 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 C4 0.047(10) 0.057(10) 0.037(8) -0.011(7) -0.004(6) 0.006(8) C3 0.033(8) 0.038(8) 0.067(9) -0.007(7) 0.001(7) -0.011(8) C2 0.078(11) 0.064(11) 0.050(9) 0.007(8) 0.004(8) 0.007(11) C1 0.033(10) 0.049(10) 0.047(8) 0.004(7) 0.002(6) 0.004(7) C7 0.132(17) 0.13(2) 0.051(11) 0.018(12) 0.003(10) 0.052(17) C15 0.081(10) 0.102(14) 0.062(10) 0.008(11) -0.011(7) 0.002(10) C16 0.089(12) 0.096(12) 0.076(11) 0.013(10) 0.007(9) -0.002(10) C17 0.115(13) 0.134(16) 0.061(10) -0.007(11) -0.004(9) 0.038(12) C9 0.069(11) 0.071(11) 0.108(13) -0.033(10) 0.019(8) 0.002(9) C10 0.059(10) 0.074(10) 0.086(10) -0.014(8) 0.023(8) 0.005(8) C11 0.062(9) 0.083(12) 0.115(12) -0.005(10) 0.031(8) 0.019(10) C12 0.066(11) 0.057(10) 0.085(11) -0.036(10) 0.021(8) -0.032(9) C13 0.047(10) 0.17(2) 0.082(12) -0.047(13) -0.004(8) 0.000(13) C14 0.051(10) 0.106(15) 0.067(11) -0.012(10) 0.008(8) -0.010(11) C8 0.066(12) 0.18(2) 0.080(12) -0.041(14) -0.012(10) 0.001(15) C5A 0.12(3) 0.17(5) 0.03(2) -0.03(2) 0.022(17) 0.04(3) C5B 0.12(3) 0.19(5) 0.15(5) 0.09(5) 0.04(2) 0.02(3) C6 0.117(13) 0.114(17) 0.081(12) 0.006(13) 0.041(10) -0.009(13) C21 0.053(10) 0.062(12) 0.079(11) -0.004(10) 0.004(8) 0.013(10) C22 0.041(9) 0.059(11) 0.069(11) -0.027(9) 0.015(8) -0.006(8) C23 0.060(9) 0.052(9) 0.074(11) -0.014(10) 0.002(10) -0.002(7) C31 0.054(10) 0.049(10) 0.073(11) -0.002(9) 0.011(8) -0.017(9) C32 0.133(17) 0.057(13) 0.078(13) -0.022(11) 0.034(12) -0.025(13) O12 0.070(6) 0.093(9) 0.127(8) -0.031(8) 0.011(5) -0.023(7) O13A 0.070(6) 0.093(9) 0.127(8) -0.031(8) 0.011(5) -0.023(7) O13B 0.070(6) 0.093(9) 0.127(8) -0.031(8) 0.011(5) -0.023(7) O14 0.077(9) 0.117(12) 0.122(10) -0.011(9) 0.035(7) -0.029(9) O21 0.118(12) 0.088(11) 0.128(13) 0.022(10) -0.002(8) 0.055(10) O22 0.059(7) 0.112(11) 0.096(9) -0.033(9) 0.025(6) 0.004(8) O23 0.046(6) 0.095(8) 0.129(10) -0.024(9) 0.004(9) 0.002(6) O31 0.102(10) 0.109(11) 0.101(11) -0.047(10) -0.004(7) -0.028(9) O32 0.195(18) 0.089(11) 0.142(14) 0.033(11) 0.066(12) -0.045(12) Ru1 0.0410(6) 0.0688(8) 0.0592(7) -0.0167(8) 0.0014(6) -0.0025(6) Ru2 0.0422(6) 0.0474(7) 0.0543(7) -0.0078(6) 0.0030(6) 0.0031(5) Ru3 0.0521(6) 0.0464(7) 0.0599(7) -0.0050(6) 0.0053(7) -0.0012(6) Si3 0.061(3) 0.074(4) 0.049(2) -0.001(2) -0.001(2) 0.006(3) Si2 0.049(3) 0.057(3) 0.065(3) -0.013(3) 0.0053(19) 0.007(2) Si1 0.090(4) 0.113(5) 0.052(3) -0.001(3) 0.005(2) 0.026(4) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 C4 C3 1.473(19) . ? C4 Si3 1.890(14) . ? C4 Ru2 2.261(14) . ? C4 Ru3 2.286(15) . ? C4 Ru1 2.291(14) . ? C3 C2 1.502(17) . ? C3 Si2 1.957(14) . ? C3 Ru1 2.285(14) . ? C3 Ru3 2.305(14) . ? C2 C1 1.452(19) . ? C2 C7 1.52(2) . ? C2 Ru3 2.288(17) . ? C2 Ru1 2.316(16) . ? C1 Si1 1.890(14) . ? C1 Ru2 2.186(14) . ? C1 Ru1 2.298(13) . ? C1 Ru3 2.301(14) . ? C7 H7C 0.96 . ? C7 H7B 0.96 . ? C7 H7A 0.96 . ? C15 Si3 1.860(16) . ? C15 H15A 0.96 . ? C15 H15C 0.96 . ? C15 H15B 0.96 . ? C16 Si3 1.855(18) . ? C16 H16C 0.96 . ? C16 H16B 0.96 . ? C16 H16A 0.96 . ? C17 Si3 1.874(16) . ? C17 H17A 0.96 . ? C17 H17B 0.96 . ? C17 H17C 0.96 . ? C9 Si2 1.848(16) . ? C9 H9A 0.96 . ? C9 H9B 0.96 . ? C9 H9C 0.96 . ? C10 Si2 1.821(15) . ? C10 H10A 0.96 . ? C10 H10B 0.96 . ? C10 H10C 0.96 . ? C11 Si2 1.879(17) . ? C11 H11A 0.96 . ? C11 H11B 0.96 . ? C11 H11C 0.96 . ? C12 O12 1.142(17) . ? C12 Ru1 2.017(17) . ? C12 Ru2 2.153(15) . ? C13 O13A 1.200(13) . ? C13 O13B 1.203(13) . ? C13 Ru1 1.830(15) . ? C14 O14 1.143(19) . ? C14 Ru1 1.881(19) . ? C8 Si1 1.91(2) . ? C8 H8A 0.96 . ? C8 H8C 0.96 . ? C8 H8B 0.96 . ? C5A Si1 1.872(13) . ? C5A H5A1 0.96 . ? C5A H5A2 0.96 . ? C5A H5A3 0.96 . ? C5B Si1 1.873(13) . ? C5B H5B1 0.96 . ? C5B H5B2 0.96 . ? C5B H5B3 0.96 . ? C6 Si1 1.864(19) . ? C6 H6A 0.96 . ? C6 H6B 0.96 . ? C6 H6C 0.96 . ? C21 O21 1.160(18) . ? C21 Ru2 1.870(18) . ? C22 O22 1.112(16) . ? C22 Ru2 1.913(15) . ? C23 O23 1.155(14) . ? C23 Ru3 1.997(14) . ? C23 Ru2 2.169(14) . ? C31 O31 1.167(18) . ? C31 Ru3 1.847(17) . ? C32 O32 1.10(2) . ? C32 Ru3 1.94(2) . ? Ru1 Ru2 2.6686(14) . ? Ru2 Ru3 2.6776(15) . ? 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 C3 C4 Si3 131.9(10) . . ? C3 C4 Ru2 116.3(9) . . ? Si3 C4 Ru2 111.7(7) . . ? C3 C4 Ru3 72.0(8) . . ? Si3 C4 Ru3 121.5(7) . . ? Ru2 C4 Ru3 72.1(4) . . ? C3 C4 Ru1 71.0(7) . . ? Si3 C4 Ru1 130.2(8) . . ? Ru2 C4 Ru1 71.8(4) . . ? Ru3 C4 Ru1 107.1(5) . . ? C4 C3 C2 114.3(13) . . ? C4 C3 Si2 123.0(10) . . ? C2 C3 Si2 122.7(13) . . ? C4 C3 Ru1 71.4(8) . . ? C2 C3 Ru1 72.0(9) . . ? Si2 C3 Ru1 122.8(7) . . ? C4 C3 Ru3 70.6(8) . . ? C2 C3 Ru3 70.3(10) . . ? Si2 C3 Ru3 130.6(7) . . ? Ru1 C3 Ru3 106.6(6) . . ? C1 C2 C3 114.7(14) . . ? C1 C2 C7 124.8(12) . . ? C3 C2 C7 120.5(15) . . ? C1 C2 Ru3 72.1(9) . . ? C3 C2 Ru3 71.5(9) . . ? C7 C2 Ru3 123.1(12) . . ? C1 C2 Ru1 71.0(8) . . ? C3 C2 Ru1 69.8(8) . . ? C7 C2 Ru1 130.6(13) . . ? Ru3 C2 Ru1 106.2(6) . . ? C2 C1 Si1 124.6(10) . . ? C2 C1 Ru2 119.4(9) . . ? Si1 C1 Ru2 116.0(7) . . ? C2 C1 Ru1 72.3(8) . . ? Si1 C1 Ru1 124.6(7) . . ? Ru2 C1 Ru1 73.0(4) . . ? C2 C1 Ru3 71.1(9) . . ? Si1 C1 Ru3 129.0(7) . . ? Ru2 C1 Ru3 73.2(4) . . ? Ru1 C1 Ru3 106.3(5) . . ? C2 C7 H7C 109.5 . . ? C2 C7 H7B 109.5 . . ? H7C C7 H7B 109.5 . . ? C2 C7 H7A 109.5 . . ? H7C C7 H7A 109.5 . . ? H7B C7 H7A 109.5 . . ? Si3 C15 H15A 109.5 . . ? Si3 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? Si3 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? H15C C15 H15B 109.5 . . ? Si3 C16 H16C 109.5 . . ? Si3 C16 H16B 109.5 . . ? H16C C16 H16B 109.5 . . ? Si3 C16 H16A 109.5 . . ? H16C C16 H16A 109.5 . . ? H16B C16 H16A 109.5 . . ? Si3 C17 H17A 109.5 . . ? Si3 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? Si3 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? Si2 C9 H9A 109.5 . . ? Si2 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? Si2 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? Si2 C10 H10A 109.5 . . ? Si2 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? Si2 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? Si2 C11 H11A 109.5 . . ? Si2 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? Si2 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? O12 C12 Ru1 143.1(14) . . ? O12 C12 Ru2 137.4(14) . . ? Ru1 C12 Ru2 79.5(6) . . ? O13A C13 Ru1 164(3) . . ? O13B C13 Ru1 162(3) . . ? O14 C14 Ru1 177.1(17) . . ? Si1 C8 H8A 109.5 . . ? Si1 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? Si1 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? H8C C8 H8B 109.5 . . ? Si1 C5A H5A1 109.5 . . ? Si1 C5A H5A2 109.5 . . ? H5A1 C5A H5A2 109.5 . . ? Si1 C5A H5A3 109.5 . . ? H5A1 C5A H5A3 109.5 . . ? H5A2 C5A H5A3 109.5 . . ? Si1 C5B H5B1 109.5 . . ? Si1 C5B H5B2 109.5 . . ? H5B1 C5B H5B2 109.5 . . ? Si1 C5B H5B3 109.5 . . ? H5B1 C5B H5B3 109.5 . . ? H5B2 C5B H5B3 109.5 . . ? Si1 C6 H6A 109.5 . . ? Si1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? Si1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? O21 C21 Ru2 173.0(16) . . ? O22 C22 Ru2 173.7(16) . . ? O23 C23 Ru3 144.9(12) . . ? O23 C23 Ru2 135.2(12) . . ? Ru3 C23 Ru2 79.9(5) . . ? O31 C31 Ru3 177.9(15) . . ? O32 C32 Ru3 179.2(17) . . ? C13 Ru1 C14 85.6(8) . . ? C13 Ru1 C12 99.4(9) . . ? C14 Ru1 C12 94.6(7) . . ? C13 Ru1 C3 125.7(9) . . ? C14 Ru1 C3 107.0(7) . . ? C12 Ru1 C3 130.4(6) . . ? C13 Ru1 C1 98.5(8) . . ? C14 Ru1 C1 172.7(7) . . ? C12 Ru1 C1 90.6(6) . . ? C3 Ru1 C1 65.8(5) . . ? C13 Ru1 C4 163.0(9) . . ? C14 Ru1 C4 101.9(7) . . ? C12 Ru1 C4 95.2(6) . . ? C3 Ru1 C4 37.6(5) . . ? C1 Ru1 C4 72.6(4) . . ? C13 Ru1 C2 98.3(9) . . ? C14 Ru1 C2 137.0(7) . . ? C12 Ru1 C2 126.3(6) . . ? C3 Ru1 C2 38.1(4) . . ? C1 Ru1 C2 36.7(5) . . ? C4 Ru1 C2 65.7(5) . . ? C13 Ru1 Ru2 131.8(6) . . ? C14 Ru1 Ru2 129.0(6) . . ? C12 Ru1 Ru2 52.5(4) . . ? C3 Ru1 Ru2 80.1(4) . . ? C1 Ru1 Ru2 51.6(3) . . ? C4 Ru1 Ru2 53.6(4) . . ? C2 Ru1 Ru2 78.4(4) . . ? C21 Ru2 C22 85.3(7) . . ? C21 Ru2 C23 92.8(7) . . ? C22 Ru2 C23 87.1(6) . . ? C21 Ru2 C12 87.1(8) . . ? C22 Ru2 C12 89.7(6) . . ? C23 Ru2 C12 176.8(6) . . ? C21 Ru2 C1 174.4(6) . . ? C22 Ru2 C1 99.5(6) . . ? C23 Ru2 C1 90.2(6) . . ? C12 Ru2 C1 90.1(6) . . ? C21 Ru2 C4 100.0(6) . . ? C22 Ru2 C4 174.4(6) . . ? C23 Ru2 C4 90.8(6) . . ? C12 Ru2 C4 92.3(6) . . ? C1 Ru2 C4 75.2(5) . . ? C21 Ru2 Ru1 119.5(5) . . ? C22 Ru2 Ru1 124.2(5) . . ? C23 Ru2 Ru1 134.3(4) . . ? C12 Ru2 Ru1 48.0(5) . . ? C1 Ru2 Ru1 55.4(3) . . ? C4 Ru2 Ru1 54.6(4) . . ? C21 Ru2 Ru3 124.3(5) . . ? C22 Ru2 Ru3 121.0(5) . . ? C23 Ru2 Ru3 47.2(4) . . ? C12 Ru2 Ru3 135.0(5) . . ? C1 Ru2 Ru3 55.4(4) . . ? C4 Ru2 Ru3 54.4(4) . . ? Ru1 Ru2 Ru3 87.02(5) . . ? C31 Ru3 C32 85.3(7) . . ? C31 Ru3 C23 94.9(7) . . ? C32 Ru3 C23 96.8(8) . . ? C31 Ru3 C4 100.0(5) . . ? C32 Ru3 C4 166.9(8) . . ? C23 Ru3 C4 94.7(6) . . ? C31 Ru3 C2 135.2(6) . . ? C32 Ru3 C2 101.5(8) . . ? C23 Ru3 C2 127.4(6) . . ? C4 Ru3 C2 66.2(5) . . ? C31 Ru3 C1 170.7(6) . . ? C32 Ru3 C1 100.8(7) . . ? C23 Ru3 C1 91.5(6) . . ? C4 Ru3 C1 72.6(4) . . ? C2 Ru3 C1 36.9(5) . . ? C31 Ru3 C3 105.3(6) . . ? C32 Ru3 C3 129.7(8) . . ? C23 Ru3 C3 129.9(5) . . ? C4 Ru3 C3 37.4(5) . . ? C2 Ru3 C3 38.2(4) . . ? C1 Ru3 C3 65.4(5) . . ? C31 Ru3 Ru2 128.8(5) . . ? C32 Ru3 Ru2 131.1(5) . . ? C23 Ru3 Ru2 52.9(4) . . ? C4 Ru3 Ru2 53.5(4) . . ? C2 Ru3 Ru2 78.7(4) . . ? C1 Ru3 Ru2 51.4(4) . . ? C3 Ru3 Ru2 79.5(4) . . ? C16 Si3 C15 109.5(9) . . ? C16 Si3 C17 107.0(8) . . ? C15 Si3 C17 100.7(8) . . ? C16 Si3 C4 107.8(7) . . ? C15 Si3 C4 110.3(7) . . ? C17 Si3 C4 121.1(8) . . ? C10 Si2 C9 114.8(8) . . ? C10 Si2 C11 103.4(7) . . ? C9 Si2 C11 105.6(8) . . ? C10 Si2 C3 109.7(7) . . ? C9 Si2 C3 108.5(6) . . ? C11 Si2 C3 114.8(7) . . ? C6 Si1 C5B 96(4) . . ? C6 Si1 C5A 116(4) . . ? C6 Si1 C1 109.0(8) . . ? C5B Si1 C1 121(2) . . ? C5A Si1 C1 114.6(17) . . ? C6 Si1 C8 110.6(9) . . ? C5B Si1 C8 110(3) . . ? C5A Si1 C8 96(3) . . ? C1 Si1 C8 109.4(8) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Si3 C4 C3 C2 -173.1(13) . . . . ? Ru2 C4 C3 C2 2.1(17) . . . . ? Ru3 C4 C3 C2 -56.6(12) . . . . ? Ru1 C4 C3 C2 59.4(12) . . . . ? Si3 C4 C3 Si2 9.9(19) . . . . ? Ru2 C4 C3 Si2 -174.9(7) . . . . ? Ru3 C4 C3 Si2 126.4(10) . . . . ? Ru1 C4 C3 Si2 -117.6(10) . . . . ? Si3 C4 C3 Ru1 127.5(13) . . . . ? Ru2 C4 C3 Ru1 -57.4(7) . . . . ? Ru3 C4 C3 Ru1 -116.0(4) . . . . ? Si3 C4 C3 Ru3 -116.5(13) . . . . ? Ru2 C4 C3 Ru3 58.6(7) . . . . ? Ru1 C4 C3 Ru3 116.0(4) . . . . ? C4 C3 C2 C1 -3(2) . . . . ? Si2 C3 C2 C1 174.5(9) . . . . ? Ru1 C3 C2 C1 56.6(12) . . . . ? Ru3 C3 C2 C1 -59.2(12) . . . . ? C4 C3 C2 C7 174.8(15) . . . . ? Si2 C3 C2 C7 -8(2) . . . . ? Ru1 C3 C2 C7 -126.1(16) . . . . ? Ru3 C3 C2 C7 118.1(17) . . . . ? C4 C3 C2 Ru3 56.7(11) . . . . ? Si2 C3 C2 Ru3 -126.3(11) . . . . ? Ru1 C3 C2 Ru3 115.8(4) . . . . ? C4 C3 C2 Ru1 -59.1(11) . . . . ? Si2 C3 C2 Ru1 117.9(10) . . . . ? Ru3 C3 C2 Ru1 -115.8(4) . . . . ? C3 C2 C1 Si1 -176.2(12) . . . . ? C7 C2 C1 Si1 7(2) . . . . ? Ru3 C2 C1 Si1 124.8(11) . . . . ? Ru1 C2 C1 Si1 -120.3(11) . . . . ? C3 C2 C1 Ru2 1.9(19) . . . . ? C7 C2 C1 Ru2 -175.3(14) . . . . ? Ru3 C2 C1 Ru2 -57.0(8) . . . . ? Ru1 C2 C1 Ru2 57.9(8) . . . . ? C3 C2 C1 Ru1 -56.0(13) . . . . ? C7 C2 C1 Ru1 126.8(17) . . . . ? Ru3 C2 C1 Ru1 -114.9(4) . . . . ? C3 C2 C1 Ru3 59.0(13) . . . . ? C7 C2 C1 Ru3 -118.3(17) . . . . ? Ru1 C2 C1 Ru3 114.9(4) . . . . ? O13A C13 Ru1 C14 55(8) . . . . ? O13B C13 Ru1 C14 -123(7) . . . . ? O13A C13 Ru1 C12 -39(8) . . . . ? O13B C13 Ru1 C12 143(7) . . . . ? O13A C13 Ru1 C3 162(7) . . . . ? O13B C13 Ru1 C3 -16(8) . . . . ? O13A C13 Ru1 C1 -131(8) . . . . ? O13B C13 Ru1 C1 51(7) . . . . ? O13A C13 Ru1 C4 172(7) . . . . ? O13B C13 Ru1 C4 -6(9) . . . . ? O13A C13 Ru1 C2 -168(8) . . . . ? O13B C13 Ru1 C2 14(7) . . . . ? O13A C13 Ru1 Ru2 -87(8) . . . . ? O13B C13 Ru1 Ru2 95(7) . . . . ? C3 C4 Si3 C16 -114.4(15) . . . . ? Ru2 C4 Si3 C16 70.2(10) . . . . ? Ru3 C4 Si3 C16 152.0(9) . . . . ? Ru1 C4 Si3 C16 -13.7(13) . . . . ? C3 C4 Si3 C15 126.0(15) . . . . ? Ru2 C4 Si3 C15 -49.3(10) . . . . ? Ru3 C4 Si3 C15 32.4(11) . . . . ? Ru1 C4 Si3 C15 -133.3(10) . . . . ? C3 C4 Si3 C17 9.0(18) . . . . ? Ru2 C4 Si3 C17 -166.3(8) . . . . ? Ru3 C4 Si3 C17 -84.6(11) . . . . ? Ru1 C4 Si3 C17 109.7(11) . . . . ? C2 C1 Si1 C6 -118.2(14) . . . . ? Ru2 C1 Si1 C6 63.6(10) . . . . ? Ru1 C1 Si1 C6 150.2(9) . . . . ? Ru3 C1 Si1 C6 -25.3(12) . . . . ? C2 C1 Si1 C5B -8(5) . . . . ? Ru2 C1 Si1 C5B 174(4) . . . . ? Ru1 C1 Si1 C5B -100(4) . . . . ? Ru3 C1 Si1 C5B 85(5) . . . . ? C2 C1 Si1 C5A 14(4) . . . . ? Ru2 C1 Si1 C5A -164(4) . . . . ? Ru1 C1 Si1 C5A -78(4) . . . . ? Ru3 C1 Si1 C5A 107(4) . . . . ? C2 C1 Si1 C8 120.8(14) . . . . ? Ru2 C1 Si1 C8 -57.4(10) . . . . ? Ru1 C1 Si1 C8 29.2(11) . . . . ? Ru3 C1 Si1 C8 -146.3(9) . . . . ? data_mrvian23 _database_code_depnum_ccdc_archive 'CCDC 903655' #TrackingRef 'compound 3b.cif' _audit_creation_date 2012-12-13T12:30:12-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.4 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common 'Compound 3b' _chemical_formula_moiety 'C19 H22 O8 Ru3 Si2' _chemical_formula_sum 'C19 H22 O8 Ru3 Si2' _chemical_formula_weight 737.76 _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 9.0636(2) _cell_length_b 10.3594(3) _cell_length_c 14.9040(4) _cell_angle_alpha 96.689(2) _cell_angle_beta 102.959(2) _cell_angle_gamma 100.3910(10) _cell_volume 1323.28(6) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 600 _cell_measurement_theta_min 1 _cell_measurement_theta_max 14 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.05 _exptl_crystal_density_diffrn 1.852 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 720 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.819 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.6 _exptl_absorpt_correction_T_max 0.6652 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 9 _diffrn_orient_matrix_type 'by Bruker AXS Collect from scalepack cell' _diffrn_orient_matrix_ub_11 -0.55608E-2 _diffrn_orient_matrix_ub_12 -0.928642E-1 _diffrn_orient_matrix_ub_13 0.134328E-1 _diffrn_orient_matrix_ub_21 0.880711E-1 _diffrn_orient_matrix_ub_22 -0.76569E-2 _diffrn_orient_matrix_ub_23 -0.290065E-1 _diffrn_orient_matrix_ub_31 0.751089E-1 _diffrn_orient_matrix_ub_32 0.348479E-1 _diffrn_orient_matrix_ub_33 0.620402E-1 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.0657 _diffrn_reflns_av_unetI/netI 0.064 _diffrn_reflns_number 23465 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.99 _diffrn_reflns_theta_max 27.46 _diffrn_reflns_theta_full 25 _diffrn_measured_fraction_theta_full 0.995 _diffrn_measured_fraction_theta_max 0.988 _reflns_number_total 5974 _reflns_number_gt 4373 _reflns_threshold_expression >2\s(I) _diffrn_reflns_reduction_process ; Scaled and merged with Sortav R.H. Blessing, (1987) Cryst. Rev. 1, 3-58 R.H. Blessing, (1989) J. Appl. Cryst. 22, 396-397 ; #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _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^)+(0.0441P)^2^+0.1463P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 5974 _refine_ls_number_parameters 346 _refine_ls_number_restraints 90 _refine_ls_R_factor_all 0.0691 _refine_ls_R_factor_gt 0.0413 _refine_ls_wR_factor_ref 0.0957 _refine_ls_wR_factor_gt 0.0859 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.028 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.848 _refine_diff_density_min -0.84 _refine_diff_density_rms 0.114 #----------------------------------------------------------------------------# # 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' O O 0.0106 0.006 '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' Si Si 0.0817 0.0704 '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 C4 C 0.8996(5) 0.1701(4) 0.3498(3) 0.0439(9) Uani 1 1 d . . . C3 C 0.7451(5) 0.0953(4) 0.2995(3) 0.0426(9) Uani 1 1 d . A . C2 C 0.6887(5) 0.1465(4) 0.2136(3) 0.0410(9) Uani 1 1 d . . . C1 C 0.7909(5) 0.2606(4) 0.1968(3) 0.0394(9) Uani 1 1 d . A . C5 C 0.8822(13) 0.3221(9) 0.0182(5) 0.147(4) Uani 1 1 d . A . H5A H 0.8348 0.2437 -0.0275 0.221 Uiso 1 1 calc R . . H5B H 0.9783 0.3104 0.0556 0.221 Uiso 1 1 calc R . . H5C H 0.9015 0.3973 -0.0129 0.221 Uiso 1 1 calc R . . C6 C 0.7836(8) 0.5328(5) 0.1353(4) 0.0811(17) Uani 1 1 d . A . H6A H 0.7548 0.5769 0.0829 0.122 Uiso 1 1 calc R . . H6B H 0.8913 0.5664 0.1657 0.122 Uiso 1 1 calc R . . H6C H 0.7223 0.5491 0.1786 0.122 Uiso 1 1 calc R . . C7 C 0.5319(6) 0.0802(5) 0.1488(3) 0.0575(12) Uani 1 1 d . A . H7A H 0.4573 0.1324 0.1574 0.086 Uiso 1 1 calc R . . H7B H 0.4998 -0.0071 0.1628 0.086 Uiso 1 1 calc R . . H7C H 0.5395 0.0732 0.0853 0.086 Uiso 1 1 calc R . . C8 C 0.5468(11) 0.3038(8) 0.0197(6) 0.144(4) Uani 1 1 d . A . H8A H 0.4754 0.3085 0.0582 0.217 Uiso 1 1 calc R . . H8B H 0.5283 0.2146 -0.013 0.217 Uiso 1 1 calc R . . H8C H 0.5327 0.3637 -0.0244 0.217 Uiso 1 1 calc R . . C9 C 0.5989(12) -0.2066(6) 0.2574(6) 0.139(4) Uani 1 1 d . A . H9A H 0.5414 -0.2785 0.279 0.209 Uiso 1 1 calc R . . H9B H 0.6955 -0.227 0.2509 0.209 Uiso 1 1 calc R . . H9C H 0.54 -0.1945 0.198 0.209 Uiso 1 1 calc R . . C10 C 0.7662(9) -0.0647(7) 0.4565(5) 0.112(3) Uani 1 1 d . A . H10A H 0.8003 0.0211 0.4952 0.167 Uiso 1 1 calc R . . H10B H 0.8544 -0.0969 0.4453 0.167 Uiso 1 1 calc R . . H10C H 0.7102 -0.1256 0.4872 0.167 Uiso 1 1 calc R . . C11 C 0.4528(7) -0.0142(6) 0.3616(5) 0.0891(19) Uani 1 1 d . A . H11A H 0.3877 -0.0057 0.3031 0.134 Uiso 1 1 calc R . . H11B H 0.4738 0.0675 0.4045 0.134 Uiso 1 1 calc R . . H11C H 0.4012 -0.0853 0.3868 0.134 Uiso 1 1 calc R . . C12 C 0.9200(5) 0.4772(4) 0.3742(3) 0.0447(9) Uani 1 1 d . . . C13 C 0.7023(6) 0.3183(4) 0.4582(3) 0.0524(11) Uani 1 1 d . . . C14 C 0.5834(6) 0.4104(4) 0.3107(3) 0.0551(11) Uani 1 1 d . . . C21 C 1.1187(6) 0.4802(5) 0.2517(3) 0.0551(11) Uani 1 1 d . . . C22 C 1.1990(6) 0.3635(4) 0.4011(3) 0.0506(10) Uani 1 1 d . . . C23 C 1.1218(6) 0.2080(5) 0.2170(4) 0.0618(13) Uani 1 1 d . . . O12 O 0.9565(4) 0.5881(3) 0.4101(2) 0.0631(9) Uani 1 1 d . A . O13 O 0.6761(5) 0.3161(4) 0.5297(2) 0.0779(11) Uani 1 1 d . A . O14 O 0.4877(5) 0.4678(4) 0.2947(3) 0.0859(12) Uani 1 1 d . A . O21 O 1.1818(5) 0.5664(4) 0.2247(3) 0.0868(12) Uani 1 1 d . A . O22 O 1.3054(5) 0.3744(4) 0.4615(3) 0.0751(10) Uani 1 1 d . A . O23 O 1.2366(5) 0.2147(4) 0.1947(3) 0.0997(16) Uani 1 1 d . A . Ru3A Ru 0.9179(5) 0.0846(3) 0.2116(4) 0.0444(8) Uani 0.63(5) 1 d PDU A 1 C31A C 0.996(4) -0.064(2) 0.247(2) 0.071(5) Uani 0.63(5) 1 d PDU A 1 C32A C 0.859(3) 0.012(3) 0.0845(11) 0.070(5) Uani 0.63(5) 1 d PDU A 1 O31A O 1.0448(19) -0.1496(13) 0.2739(19) 0.099(5) Uani 0.63(5) 1 d PDU A 1 O32A O 0.836(3) -0.068(2) 0.0123(15) 0.104(6) Uani 0.63(5) 1 d PDU A 1 Ru3B Ru 0.9178(8) 0.0886(7) 0.2025(11) 0.0597(18) Uani 0.37(5) 1 d PDU A 2 C31B C 1.015(6) -0.055(4) 0.224(4) 0.083(12) Uani 0.37(5) 1 d PDU A 2 C32B C 0.885(6) -0.013(6) 0.0844(17) 0.070(8) Uani 0.37(5) 1 d PDU A 2 O31B O 1.064(4) -0.148(3) 0.226(3) 0.114(9) Uani 0.37(5) 1 d PDU A 2 O32B O 0.827(5) -0.014(4) 0.0011(17) 0.096(7) Uani 0.37(5) 1 d PDU A 2 Ru1 Ru 0.74388(4) 0.31647(3) 0.34010(2) 0.03808(11) Uani 1 1 d . A . Ru2 Ru 1.02049(4) 0.33500(3) 0.30076(2) 0.03928(11) Uani 1 1 d . A . Si1 Si 0.74935(19) 0.35141(14) 0.09453(9) 0.0619(4) Uani 1 1 d . . . Si2 Si 0.63718(18) -0.05076(13) 0.34318(11) 0.0641(4) Uani 1 1 d . . . H4 H 0.947(5) 0.152(4) 0.407(3) 0.039(11) Uiso 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 C4 0.038(2) 0.042(2) 0.046(2) 0.0043(18) 0.000(2) 0.0113(18) C3 0.032(2) 0.037(2) 0.054(2) -0.0013(17) 0.0049(19) 0.0063(17) C2 0.033(2) 0.042(2) 0.047(2) -0.0019(17) 0.0099(18) 0.0110(17) C1 0.031(2) 0.044(2) 0.040(2) 0.0021(16) 0.0045(17) 0.0078(17) C5 0.242(13) 0.168(8) 0.093(5) 0.061(5) 0.106(7) 0.092(8) C6 0.080(4) 0.067(3) 0.089(4) 0.029(3) -0.003(3) 0.017(3) C7 0.036(3) 0.069(3) 0.056(3) -0.003(2) -0.003(2) 0.007(2) C8 0.130(8) 0.117(6) 0.126(6) 0.054(5) -0.078(6) -0.008(5) C9 0.177(10) 0.048(3) 0.184(9) -0.008(4) 0.073(8) -0.017(4) C10 0.091(6) 0.123(6) 0.133(6) 0.086(5) 0.019(5) 0.020(4) C11 0.062(4) 0.097(4) 0.105(5) 0.034(4) 0.023(4) -0.007(3) C12 0.035(2) 0.048(2) 0.047(2) 0.0014(19) 0.0065(19) 0.0052(18) C13 0.051(3) 0.050(2) 0.051(3) -0.003(2) 0.016(2) 0.001(2) C14 0.045(3) 0.043(2) 0.074(3) 0.004(2) 0.017(2) 0.003(2) C21 0.041(3) 0.059(3) 0.068(3) 0.017(2) 0.018(2) 0.009(2) C22 0.042(3) 0.042(2) 0.060(3) 0.005(2) 0.006(2) 0.0027(19) C23 0.037(3) 0.061(3) 0.079(3) -0.016(2) 0.013(3) 0.007(2) O12 0.057(2) 0.0421(17) 0.081(2) -0.0138(16) 0.0188(18) 0.0001(15) O13 0.085(3) 0.091(3) 0.058(2) 0.0061(18) 0.031(2) 0.007(2) O14 0.048(2) 0.069(2) 0.144(4) 0.018(2) 0.018(2) 0.029(2) O21 0.060(3) 0.092(3) 0.115(3) 0.053(2) 0.024(2) 0.007(2) O22 0.049(2) 0.083(2) 0.077(2) 0.0096(19) -0.013(2) 0.0078(19) O23 0.044(2) 0.098(3) 0.140(4) -0.048(3) 0.040(3) -0.005(2) Ru3A 0.0369(12) 0.0353(14) 0.0576(10) -0.0050(10) 0.0101(8) 0.0097(7) C31A 0.052(11) 0.047(6) 0.113(12) 0.001(6) 0.023(7) 0.011(5) C32A 0.027(8) 0.080(13) 0.094(8) -0.041(6) 0.014(5) 0.021(6) O31A 0.082(6) 0.055(5) 0.159(13) 0.008(6) 0.013(8) 0.036(4) O32A 0.093(8) 0.099(12) 0.098(8) -0.052(8) 0.028(6) 0.001(10) Ru3B 0.0266(19) 0.068(3) 0.072(3) -0.022(2) 0.0039(15) 0.0090(17) C31B 0.026(11) 0.059(13) 0.14(3) -0.033(14) 0.006(17) 0.011(11) C32B 0.044(18) 0.076(18) 0.092(11) -0.032(10) 0.029(9) 0.030(11) O31B 0.099(14) 0.077(9) 0.16(2) -0.019(12) 0.009(15) 0.049(9) O32B 0.081(11) 0.098(19) 0.086(9) -0.050(11) 0.018(8) 0.008(15) Ru1 0.03165(19) 0.03770(18) 0.04201(19) 0.00026(13) 0.00738(14) 0.00634(13) Ru2 0.02864(19) 0.03977(18) 0.04533(19) 0.00138(14) 0.00544(14) 0.00517(13) Si1 0.0696(10) 0.0667(8) 0.0440(7) 0.0121(6) 0.0035(7) 0.0118(7) Si2 0.0557(9) 0.0478(7) 0.0855(10) 0.0211(7) 0.0134(8) 0.0014(6) #----------------------------------------------------------------------------# # 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 C4 C3 1.458(6) . ? C4 Ru2 2.151(4) . ? C4 Ru3A 2.200(7) . ? C4 Ru1 2.246(4) . ? C4 Ru3B 2.311(15) . ? C4 H4 0.93(4) . ? C3 C2 1.465(6) . ? C3 Si2 1.911(4) . ? C3 Ru3A 2.266(6) . ? C3 Ru1 2.303(4) . ? C3 Ru3B 2.361(13) . ? C2 C1 1.448(6) . ? C2 C7 1.517(6) . ? C2 Ru3A 2.288(6) . ? C2 Ru3B 2.298(8) . ? C2 Ru1 2.322(4) . ? C1 Si1 1.885(4) . ? C1 Ru2 2.241(4) . ? C1 Ru3B 2.288(8) . ? C1 Ru1 2.300(4) . ? C1 Ru3A 2.331(5) . ? C5 Si1 1.872(7) . ? C5 H5A 0.96 . ? C5 H5B 0.96 . ? C5 H5C 0.96 . ? C6 Si1 1.854(6) . ? C6 H6A 0.96 . ? C6 H6B 0.96 . ? C6 H6C 0.96 . ? C7 H7A 0.96 . ? C7 H7B 0.96 . ? C7 H7C 0.96 . ? C8 Si1 1.866(8) . ? C8 H8A 0.96 . ? C8 H8B 0.96 . ? C8 H8C 0.96 . ? C9 Si2 1.865(6) . ? C9 H9A 0.96 . ? C9 H9B 0.96 . ? C9 H9C 0.96 . ? C10 Si2 1.863(7) . ? C10 H10A 0.96 . ? C10 H10B 0.96 . ? C10 H10C 0.96 . ? C11 Si2 1.850(7) . ? C11 H11A 0.96 . ? C11 H11B 0.96 . ? C11 H11C 0.96 . ? C12 O12 1.164(5) . ? C12 Ru1 2.015(4) . ? C12 Ru2 2.180(4) . ? C13 O13 1.146(5) . ? C13 Ru1 1.879(4) . ? C14 O14 1.135(6) . ? C14 Ru1 1.892(5) . ? C21 O21 1.135(5) . ? C21 Ru2 1.912(5) . ? C22 O22 1.140(6) . ? C22 Ru2 1.893(5) . ? C23 O23 1.153(6) . ? C23 Ru3B 1.982(9) . ? C23 Ru3A 2.028(6) . ? C23 Ru2 2.169(4) . ? Ru3A C32A 1.873(11) . ? Ru3A C31A 1.891(10) . ? Ru3A Ru2 2.670(3) . ? C31A O31A 1.132(11) . ? C32A O32A 1.229(17) . ? Ru3B C32B 1.875(14) . ? Ru3B C31B 1.885(13) . ? Ru3B Ru2 2.681(7) . ? C31B O31B 1.135(16) . ? C32B O32B 1.23(2) . ? Ru1 Ru2 2.6792(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C3 C4 Ru2 122.5(3) . . ? C3 C4 Ru3A 73.4(3) . . ? Ru2 C4 Ru3A 75.70(18) . . ? C3 C4 Ru1 73.5(2) . . ? Ru2 C4 Ru1 75.05(13) . . ? Ru3A C4 Ru1 112.0(2) . . ? C3 C4 Ru3B 73.7(3) . . ? Ru2 C4 Ru3B 73.7(3) . . ? Ru3A C4 Ru3B 2.4(3) . . ? Ru1 C4 Ru3B 109.9(3) . . ? C3 C4 H4 120(3) . . ? Ru2 C4 H4 117(3) . . ? Ru3A C4 H4 128(2) . . ? Ru1 C4 H4 121(2) . . ? Ru3B C4 H4 130(2) . . ? C4 C3 C2 111.2(4) . . ? C4 C3 Si2 122.6(3) . . ? C2 C3 Si2 126.2(3) . . ? C4 C3 Ru3A 68.5(3) . . ? C2 C3 Ru3A 72.0(2) . . ? Si2 C3 Ru3A 126.1(2) . . ? C4 C3 Ru1 69.2(2) . . ? C2 C3 Ru1 72.2(2) . . ? Si2 C3 Ru1 126.12(19) . . ? Ru3A C3 Ru1 107.51(18) . . ? C4 C3 Ru3B 70.0(3) . . ? C2 C3 Ru3B 69.3(4) . . ? Si2 C3 Ru3B 127.5(3) . . ? Ru3A C3 Ru3B 2.7(3) . . ? Ru1 C3 Ru3B 106.3(2) . . ? C1 C2 C3 115.8(4) . . ? C1 C2 C7 124.3(4) . . ? C3 C2 C7 120.0(4) . . ? C1 C2 Ru3A 73.4(2) . . ? C3 C2 Ru3A 70.4(3) . . ? C7 C2 Ru3A 125.7(3) . . ? C1 C2 Ru3B 71.2(3) . . ? C3 C2 Ru3B 74.0(5) . . ? C7 C2 Ru3B 124.2(4) . . ? Ru3A C2 Ru3B 3.6(4) . . ? C1 C2 Ru1 70.9(2) . . ? C3 C2 Ru1 70.8(2) . . ? C7 C2 Ru1 128.0(3) . . ? Ru3A C2 Ru1 106.1(2) . . ? Ru3B C2 Ru1 107.7(3) . . ? C2 C1 Si1 125.9(3) . . ? C2 C1 Ru2 117.2(3) . . ? Si1 C1 Ru2 116.9(2) . . ? C2 C1 Ru3B 72.0(3) . . ? Si1 C1 Ru3B 125.1(4) . . ? Ru2 C1 Ru3B 72.6(3) . . ? C2 C1 Ru1 72.6(2) . . ? Si1 C1 Ru1 125.78(19) . . ? Ru2 C1 Ru1 72.31(11) . . ? Ru3B C1 Ru1 108.9(4) . . ? C2 C1 Ru3A 70.1(2) . . ? Si1 C1 Ru3A 128.6(2) . . ? Ru2 C1 Ru3A 71.45(16) . . ? Ru3B C1 Ru3A 3.4(4) . . ? Ru1 C1 Ru3A 105.5(2) . . ? Si1 C5 H5A 109.5 . . ? Si1 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? Si1 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? Si1 C6 H6A 109.5 . . ? Si1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? Si1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C2 C7 H7A 109.5 . . ? C2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? Si1 C8 H8A 109.5 . . ? Si1 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? Si1 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? Si2 C9 H9A 109.5 . . ? Si2 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? Si2 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? Si2 C10 H10A 109.5 . . ? Si2 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? Si2 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? Si2 C11 H11A 109.5 . . ? Si2 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? Si2 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? O12 C12 Ru1 143.3(3) . . ? O12 C12 Ru2 137.4(3) . . ? Ru1 C12 Ru2 79.28(14) . . ? O13 C13 Ru1 178.3(4) . . ? O14 C14 Ru1 178.8(5) . . ? O21 C21 Ru2 177.5(5) . . ? O22 C22 Ru2 176.9(4) . . ? O23 C23 Ru3B 142.6(5) . . ? O23 C23 Ru3A 143.9(4) . . ? Ru3B C23 Ru3A 3.9(5) . . ? O23 C23 Ru2 137.1(4) . . ? Ru3B C23 Ru2 80.3(3) . . ? Ru3A C23 Ru2 79.0(2) . . ? C32A Ru3A C31A 93.0(15) . . ? C32A Ru3A C23 99.7(11) . . ? C31A Ru3A C23 98.4(10) . . ? C32A Ru3A C4 159.8(8) . . ? C31A Ru3A C4 97.7(9) . . ? C23 Ru3A C4 95.6(2) . . ? C32A Ru3A C3 122.9(9) . . ? C31A Ru3A C3 101.3(9) . . ? C23 Ru3A C3 131.3(3) . . ? C4 Ru3A C3 38.07(18) . . ? C32A Ru3A C2 95.3(8) . . ? C31A Ru3A C2 132.2(9) . . ? C23 Ru3A C2 126.2(2) . . ? C4 Ru3A C2 65.0(2) . . ? C3 Ru3A C2 37.53(16) . . ? C32A Ru3A C1 96.0(10) . . ? C31A Ru3A C1 166.2(9) . . ? C23 Ru3A C1 90.4(2) . . ? C4 Ru3A C1 70.64(19) . . ? C3 Ru3A C1 64.91(17) . . ? C2 Ru3A C1 36.53(15) . . ? C32A Ru3A Ru2 132.0(13) . . ? C31A Ru3A Ru2 125.9(11) . . ? C23 Ru3A Ru2 52.86(15) . . ? C4 Ru3A Ru2 51.32(14) . . ? C3 Ru3A Ru2 79.83(16) . . ? C2 Ru3A Ru2 79.25(14) . . ? C1 Ru3A Ru2 52.71(12) . . ? O31A C31A Ru3A 175(3) . . ? O32A C32A Ru3A 160(4) . . ? C32B Ru3B C31B 75(2) . . ? C32B Ru3B C23 102(2) . . ? C31B Ru3B C23 90.4(17) . . ? C32B Ru3B C1 112.0(16) . . ? C31B Ru3B C1 171.7(17) . . ? C23 Ru3B C1 92.8(4) . . ? C32B Ru3B C2 108.0(15) . . ? C31B Ru3B C2 137.7(16) . . ? C23 Ru3B C2 128.1(4) . . ? C1 Ru3B C2 36.81(18) . . ? C32B Ru3B C4 164(2) . . ? C31B Ru3B C4 102.7(17) . . ? C23 Ru3B C4 93.4(4) . . ? C1 Ru3B C4 69.5(3) . . ? C2 Ru3B C4 63.1(3) . . ? C32B Ru3B C3 128.9(19) . . ? C31B Ru3B C3 108.1(16) . . ? C23 Ru3B C3 128.4(5) . . ? C1 Ru3B C3 64.1(3) . . ? C2 Ru3B C3 36.6(2) . . ? C4 Ru3B C3 36.3(3) . . ? C32B Ru3B Ru2 144(2) . . ? C31B Ru3B Ru2 124.5(17) . . ? C23 Ru3B Ru2 52.9(2) . . ? C1 Ru3B Ru2 52.90(17) . . ? C2 Ru3B Ru2 78.9(2) . . ? C4 Ru3B Ru2 50.4(2) . . ? C3 Ru3B Ru2 78.0(3) . . ? O31B C31B Ru3B 172(5) . . ? O32B C32B Ru3B 142(4) . . ? C13 Ru1 C14 86.7(2) . . ? C13 Ru1 C12 97.55(18) . . ? C14 Ru1 C12 96.27(18) . . ? C13 Ru1 C4 98.84(19) . . ? C14 Ru1 C4 167.36(18) . . ? C12 Ru1 C4 94.27(17) . . ? C13 Ru1 C1 166.20(16) . . ? C14 Ru1 C1 102.17(18) . . ? C12 Ru1 C1 92.04(15) . . ? C4 Ru1 C1 70.45(15) . . ? C13 Ru1 C3 101.37(17) . . ? C14 Ru1 C3 130.49(17) . . ? C12 Ru1 C3 129.96(16) . . ? C4 Ru1 C3 37.36(15) . . ? C1 Ru1 C3 64.83(14) . . ? C13 Ru1 C2 131.27(16) . . ? C14 Ru1 C2 104.15(18) . . ? C12 Ru1 C2 127.22(15) . . ? C4 Ru1 C2 63.69(15) . . ? C1 Ru1 C2 36.51(14) . . ? C3 Ru1 C2 36.93(15) . . ? C13 Ru1 Ru2 127.22(16) . . ? C14 Ru1 Ru2 133.07(14) . . ? C12 Ru1 Ru2 53.09(12) . . ? C4 Ru1 Ru2 50.88(11) . . ? C1 Ru1 Ru2 52.83(10) . . ? C3 Ru1 Ru2 79.00(10) . . ? C2 Ru1 Ru2 78.48(10) . . ? C22 Ru2 C21 89.5(2) . . ? C22 Ru2 C4 93.53(18) . . ? C21 Ru2 C4 177.0(2) . . ? C22 Ru2 C23 90.2(2) . . ? C21 Ru2 C23 86.9(2) . . ? C4 Ru2 C23 92.99(18) . . ? C22 Ru2 C12 92.36(18) . . ? C21 Ru2 C12 87.51(18) . . ? C4 Ru2 C12 92.40(15) . . ? C23 Ru2 C12 173.85(19) . . ? C22 Ru2 C1 166.75(16) . . ? C21 Ru2 C1 103.71(18) . . ? C4 Ru2 C1 73.27(16) . . ? C23 Ru2 C1 89.31(17) . . ? C12 Ru2 C1 89.42(15) . . ? C22 Ru2 Ru3A 115.29(16) . . ? C21 Ru2 Ru3A 125.46(19) . . ? C4 Ru2 Ru3A 52.98(16) . . ? C23 Ru2 Ru3A 48.19(17) . . ? C12 Ru2 Ru3A 134.67(15) . . ? C1 Ru2 Ru3A 55.84(13) . . ? C22 Ru2 Ru1 118.31(14) . . ? C21 Ru2 Ru1 124.29(14) . . ? C4 Ru2 Ru1 54.07(11) . . ? C23 Ru2 Ru1 134.98(13) . . ? C12 Ru2 Ru1 47.63(11) . . ? C1 Ru2 Ru1 54.86(10) . . ? Ru3A Ru2 Ru1 87.07(10) . . ? C22 Ru2 Ru3B 117.2(3) . . ? C21 Ru2 Ru3B 122.5(4) . . ? C4 Ru2 Ru3B 55.9(4) . . ? C23 Ru2 Ru3B 46.8(2) . . ? C12 Ru2 Ru3B 135.7(2) . . ? C1 Ru2 Ru3B 54.5(2) . . ? Ru3A Ru2 Ru3B 3.1(4) . . ? Ru1 Ru2 Ru3B 88.2(2) . . ? C6 Si1 C8 105.4(3) . . ? C6 Si1 C5 108.4(4) . . ? C8 Si1 C5 107.6(5) . . ? C6 Si1 C1 110.5(2) . . ? C8 Si1 C1 115.5(3) . . ? C5 Si1 C1 109.1(3) . . ? C11 Si2 C10 110.0(3) . . ? C11 Si2 C9 110.3(4) . . ? C10 Si2 C9 110.9(4) . . ? C11 Si2 C3 109.4(2) . . ? C10 Si2 C3 105.9(3) . . ? C9 Si2 C3 110.3(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Ru2 C4 C3 C2 0.8(5) . . . . ? Ru3A C4 C3 C2 -59.5(3) . . . . ? Ru1 C4 C3 C2 60.2(3) . . . . ? Ru3B C4 C3 C2 -57.0(4) . . . . ? Ru2 C4 C3 Si2 -179.77(19) . . . . ? Ru3A C4 C3 Si2 120.0(3) . . . . ? Ru1 C4 C3 Si2 -120.4(3) . . . . ? Ru3B C4 C3 Si2 122.4(4) . . . . ? Ru2 C4 C3 Ru3A 60.3(3) . . . . ? Ru1 C4 C3 Ru3A 119.70(18) . . . . ? Ru3B C4 C3 Ru3A 2.5(3) . . . . ? Ru2 C4 C3 Ru1 -59.4(2) . . . . ? Ru3A C4 C3 Ru1 -119.70(18) . . . . ? Ru3B C4 C3 Ru1 -117.2(3) . . . . ? Ru2 C4 C3 Ru3B 57.8(4) . . . . ? Ru3A C4 C3 Ru3B -2.5(3) . . . . ? Ru1 C4 C3 Ru3B 117.2(3) . . . . ? C4 C3 C2 C1 -1.9(5) . . . . ? Si2 C3 C2 C1 178.6(3) . . . . ? Ru3A C3 C2 C1 -59.4(3) . . . . ? Ru1 C3 C2 C1 56.4(3) . . . . ? Ru3B C3 C2 C1 -59.3(3) . . . . ? C4 C3 C2 C7 178.1(3) . . . . ? Si2 C3 C2 C7 -1.4(5) . . . . ? Ru3A C3 C2 C7 120.6(4) . . . . ? Ru1 C3 C2 C7 -123.5(3) . . . . ? Ru3B C3 C2 C7 120.7(4) . . . . ? C4 C3 C2 Ru3A 57.4(3) . . . . ? Si2 C3 C2 Ru3A -122.0(3) . . . . ? Ru1 C3 C2 Ru3A 115.83(15) . . . . ? Ru3B C3 C2 Ru3A 0.0(3) . . . . ? C4 C3 C2 Ru3B 57.4(3) . . . . ? Si2 C3 C2 Ru3B -122.0(3) . . . . ? Ru3A C3 C2 Ru3B 0.0(3) . . . . ? Ru1 C3 C2 Ru3B 115.8(2) . . . . ? C4 C3 C2 Ru1 -58.4(3) . . . . ? Si2 C3 C2 Ru1 122.2(3) . . . . ? Ru3A C3 C2 Ru1 -115.83(15) . . . . ? Ru3B C3 C2 Ru1 -115.8(2) . . . . ? C3 C2 C1 Si1 -178.4(3) . . . . ? C7 C2 C1 Si1 1.6(5) . . . . ? Ru3A C2 C1 Si1 123.8(3) . . . . ? Ru3B C2 C1 Si1 120.7(5) . . . . ? Ru1 C2 C1 Si1 -122.0(3) . . . . ? C3 C2 C1 Ru2 2.3(4) . . . . ? C7 C2 C1 Ru2 -177.7(3) . . . . ? Ru3A C2 C1 Ru2 -55.5(2) . . . . ? Ru3B C2 C1 Ru2 -58.6(4) . . . . ? Ru1 C2 C1 Ru2 58.72(19) . . . . ? C3 C2 C1 Ru3B 60.9(5) . . . . ? C7 C2 C1 Ru3B -119.1(5) . . . . ? Ru3A C2 C1 Ru3B 3.1(4) . . . . ? Ru1 C2 C1 Ru3B 117.3(4) . . . . ? C3 C2 C1 Ru1 -56.4(3) . . . . ? C7 C2 C1 Ru1 123.6(4) . . . . ? Ru3A C2 C1 Ru1 -114.22(19) . . . . ? Ru3B C2 C1 Ru1 -117.3(4) . . . . ? C3 C2 C1 Ru3A 57.8(3) . . . . ? C7 C2 C1 Ru3A -122.2(4) . . . . ? Ru3B C2 C1 Ru3A -3.1(4) . . . . ? Ru1 C2 C1 Ru3A 114.22(19) . . . . ? O23 C23 Ru3A C32A -47.1(14) . . . . ? Ru3B C23 Ru3A C32A 27(4) . . . . ? Ru2 C23 Ru3A C32A 136.3(10) . . . . ? O23 C23 Ru3A C31A 47.4(13) . . . . ? Ru3B C23 Ru3A C31A 121(4) . . . . ? Ru2 C23 Ru3A C31A -129.2(10) . . . . ? O23 C23 Ru3A C4 146.1(9) . . . . ? Ru3B C23 Ru3A C4 -140(4) . . . . ? Ru2 C23 Ru3A C4 -30.5(2) . . . . ? O23 C23 Ru3A C3 160.7(8) . . . . ? Ru3B C23 Ru3A C3 -126(4) . . . . ? Ru2 C23 Ru3A C3 -15.9(4) . . . . ? O23 C23 Ru3A C2 -151.0(8) . . . . ? Ru3B C23 Ru3A C2 -77(4) . . . . ? Ru2 C23 Ru3A C2 32.4(4) . . . . ? O23 C23 Ru3A C1 -143.3(9) . . . . ? Ru3B C23 Ru3A C1 -70(4) . . . . ? Ru2 C23 Ru3A C1 40.08(19) . . . . ? O23 C23 Ru3A Ru2 176.6(10) . . . . ? Ru3B C23 Ru3A Ru2 -110(4) . . . . ? C3 C4 Ru3A C32A 23(4) . . . . ? Ru2 C4 Ru3A C32A -108(4) . . . . ? Ru1 C4 Ru3A C32A -41(4) . . . . ? Ru3B C4 Ru3A C32A -74(8) . . . . ? C3 C4 Ru3A C31A -98.6(11) . . . . ? Ru2 C4 Ru3A C31A 130.5(11) . . . . ? Ru1 C4 Ru3A C31A -162.5(11) . . . . ? Ru3B C4 Ru3A C31A 165(7) . . . . ? C3 C4 Ru3A C23 162.2(3) . . . . ? Ru2 C4 Ru3A C23 31.2(2) . . . . ? Ru1 C4 Ru3A C23 98.3(3) . . . . ? Ru3B C4 Ru3A C23 66(7) . . . . ? Ru2 C4 Ru3A C3 -130.9(3) . . . . ? Ru1 C4 Ru3A C3 -63.9(2) . . . . ? Ru3B C4 Ru3A C3 -97(7) . . . . ? C3 C4 Ru3A C2 34.6(2) . . . . ? Ru2 C4 Ru3A C2 -96.33(17) . . . . ? Ru1 C4 Ru3A C2 -29.27(19) . . . . ? Ru3B C4 Ru3A C2 -62(7) . . . . ? C3 C4 Ru3A C1 73.7(3) . . . . ? Ru2 C4 Ru3A C1 -57.22(14) . . . . ? Ru1 C4 Ru3A C1 9.84(19) . . . . ? Ru3B C4 Ru3A C1 -23(7) . . . . ? C3 C4 Ru3A Ru2 130.9(3) . . . . ? Ru1 C4 Ru3A Ru2 67.06(16) . . . . ? Ru3B C4 Ru3A Ru2 34(7) . . . . ? C4 C3 Ru3A C32A -170.8(14) . . . . ? C2 C3 Ru3A C32A -48.4(14) . . . . ? Si2 C3 Ru3A C32A 73.7(14) . . . . ? Ru1 C3 Ru3A C32A -112.4(14) . . . . ? Ru3B C3 Ru3A C32A -49(5) . . . . ? C4 C3 Ru3A C31A 88.0(11) . . . . ? C2 C3 Ru3A C31A -149.6(11) . . . . ? Si2 C3 Ru3A C31A -27.5(12) . . . . ? Ru1 C3 Ru3A C31A 146.4(11) . . . . ? Ru3B C3 Ru3A C31A -150(6) . . . . ? C4 C3 Ru3A C23 -24.0(4) . . . . ? C2 C3 Ru3A C23 98.4(4) . . . . ? Si2 C3 Ru3A C23 -139.5(4) . . . . ? Ru1 C3 Ru3A C23 34.4(4) . . . . ? Ru3B C3 Ru3A C23 98(5) . . . . ? C2 C3 Ru3A C4 122.4(3) . . . . ? Si2 C3 Ru3A C4 -115.5(4) . . . . ? Ru1 C3 Ru3A C4 58.4(2) . . . . ? Ru3B C3 Ru3A C4 122(5) . . . . ? C4 C3 Ru3A C2 -122.4(3) . . . . ? Si2 C3 Ru3A C2 122.1(4) . . . . ? Ru1 C3 Ru3A C2 -64.0(2) . . . . ? Ru3B C3 Ru3A C2 -1(5) . . . . ? C4 C3 Ru3A C1 -90.3(3) . . . . ? C2 C3 Ru3A C1 32.1(2) . . . . ? Si2 C3 Ru3A C1 154.3(3) . . . . ? Ru1 C3 Ru3A C1 -31.89(19) . . . . ? Ru3B C3 Ru3A C1 31(5) . . . . ? C4 C3 Ru3A Ru2 -36.8(2) . . . . ? C2 C3 Ru3A Ru2 85.6(2) . . . . ? Si2 C3 Ru3A Ru2 -152.3(3) . . . . ? Ru1 C3 Ru3A Ru2 21.55(18) . . . . ? Ru3B C3 Ru3A Ru2 85(5) . . . . ? C1 C2 Ru3A C32A -93.1(13) . . . . ? C3 C2 Ru3A C32A 140.9(13) . . . . ? C7 C2 Ru3A C32A 27.5(13) . . . . ? Ru3B C2 Ru3A C32A -40(4) . . . . ? Ru1 C2 Ru3A C32A -156.8(12) . . . . ? C1 C2 Ru3A C31A 168.0(14) . . . . ? C3 C2 Ru3A C31A 42.0(14) . . . . ? C7 C2 Ru3A C31A -71.4(15) . . . . ? Ru3B C2 Ru3A C31A -139(4) . . . . ? Ru1 C2 Ru3A C31A 104.3(14) . . . . ? C1 C2 Ru3A C23 13.0(4) . . . . ? C3 C2 Ru3A C23 -113.0(4) . . . . ? C7 C2 Ru3A C23 133.6(4) . . . . ? Ru3B C2 Ru3A C23 66(4) . . . . ? Ru1 C2 Ru3A C23 -50.8(4) . . . . ? C1 C2 Ru3A C4 90.9(2) . . . . ? C3 C2 Ru3A C4 -35.1(2) . . . . ? C7 C2 Ru3A C4 -148.5(4) . . . . ? Ru3B C2 Ru3A C4 144(4) . . . . ? Ru1 C2 Ru3A C4 27.16(18) . . . . ? C1 C2 Ru3A C3 126.0(3) . . . . ? C7 C2 Ru3A C3 -113.4(4) . . . . ? Ru3B C2 Ru3A C3 179(4) . . . . ? Ru1 C2 Ru3A C3 62.2(2) . . . . ? C3 C2 Ru3A C1 -126.0(3) . . . . ? C7 C2 Ru3A C1 120.6(5) . . . . ? Ru3B C2 Ru3A C1 53(4) . . . . ? Ru1 C2 Ru3A C1 -63.8(2) . . . . ? C1 C2 Ru3A Ru2 38.8(2) . . . . ? C3 C2 Ru3A Ru2 -87.2(2) . . . . ? C7 C2 Ru3A Ru2 159.3(4) . . . . ? Ru3B C2 Ru3A Ru2 92(4) . . . . ? Ru1 C2 Ru3A Ru2 -25.01(17) . . . . ? C2 C1 Ru3A C32A 90.7(11) . . . . ? Si1 C1 Ru3A C32A -29.9(12) . . . . ? Ru2 C1 Ru3A C32A -140.0(11) . . . . ? Ru3B C1 Ru3A C32A -31(5) . . . . ? Ru1 C1 Ru3A C32A 155.2(11) . . . . ? C2 C1 Ru3A C31A -40(5) . . . . ? Si1 C1 Ru3A C31A -161(5) . . . . ? Ru2 C1 Ru3A C31A 89(5) . . . . ? Ru3B C1 Ru3A C31A -162(7) . . . . ? Ru1 C1 Ru3A C31A 25(5) . . . . ? C2 C1 Ru3A C23 -169.5(3) . . . . ? Si1 C1 Ru3A C23 69.9(3) . . . . ? Ru2 C1 Ru3A C23 -40.2(2) . . . . ? Ru3B C1 Ru3A C23 68(4) . . . . ? Ru1 C1 Ru3A C23 -105.0(3) . . . . ? C2 C1 Ru3A C4 -73.8(3) . . . . ? Si1 C1 Ru3A C4 165.7(3) . . . . ? Ru2 C1 Ru3A C4 55.59(15) . . . . ? Ru3B C1 Ru3A C4 164(5) . . . . ? Ru1 C1 Ru3A C4 -9.24(18) . . . . ? C2 C1 Ru3A C3 -33.0(2) . . . . ? Si1 C1 Ru3A C3 -153.5(3) . . . . ? Ru2 C1 Ru3A C3 96.40(17) . . . . ? Ru3B C1 Ru3A C3 -155(5) . . . . ? Ru1 C1 Ru3A C3 31.57(18) . . . . ? Si1 C1 Ru3A C2 -120.6(4) . . . . ? Ru2 C1 Ru3A C2 129.4(3) . . . . ? Ru3B C1 Ru3A C2 -122(5) . . . . ? Ru1 C1 Ru3A C2 64.5(2) . . . . ? C2 C1 Ru3A Ru2 -129.4(3) . . . . ? Si1 C1 Ru3A Ru2 110.1(3) . . . . ? Ru3B C1 Ru3A Ru2 109(5) . . . . ? Ru1 C1 Ru3A Ru2 -64.83(13) . . . . ? C32A Ru3A C31A O31A -18E1(3) . . . . ? C23 Ru3A C31A O31A 9E1(3) . . . . ? C4 Ru3A C31A O31A -1E1(3) . . . . ? C3 Ru3A C31A O31A -5E1(3) . . . . ? C2 Ru3A C31A O31A -8E1(3) . . . . ? C1 Ru3A C31A O31A -4E1(4) . . . . ? Ru2 Ru3A C31A O31A 4E1(3) . . . . ? C31A Ru3A C32A O32A 4(9) . . . . ? C23 Ru3A C32A O32A 103(9) . . . . ? C4 Ru3A C32A O32A -118(7) . . . . ? C3 Ru3A C32A O32A -101(8) . . . . ? C2 Ru3A C32A O32A -128(8) . . . . ? C1 Ru3A C32A O32A -165(8) . . . . ? Ru2 Ru3A C32A O32A 151(8) . . . . ? O23 C23 Ru3B C32B -28(2) . . . . ? Ru3A C23 Ru3B C32B -140(5) . . . . ? Ru2 C23 Ru3B C32B 150.7(16) . . . . ? O23 C23 Ru3B C31B 46.0(19) . . . . ? Ru3A C23 Ru3B C31B -65(4) . . . . ? Ru2 C23 Ru3B C31B -134.9(17) . . . . ? O23 C23 Ru3B C1 -141.7(9) . . . . ? Ru3A C23 Ru3B C1 107(4) . . . . ? Ru2 C23 Ru3B C1 37.4(4) . . . . ? O23 C23 Ru3B C2 -153.2(9) . . . . ? Ru3A C23 Ru3B C2 96(4) . . . . ? Ru2 C23 Ru3B C2 25.9(8) . . . . ? O23 C23 Ru3B C4 148.7(9) . . . . ? Ru3A C23 Ru3B C4 37(4) . . . . ? Ru2 C23 Ru3B C4 -32.2(3) . . . . ? O23 C23 Ru3B C3 159.6(8) . . . . ? Ru3A C23 Ru3B C3 48(4) . . . . ? Ru2 C23 Ru3B C3 -21.3(7) . . . . ? O23 C23 Ru3B Ru2 -179.1(11) . . . . ? Ru3A C23 Ru3B Ru2 70(4) . . . . ? C2 C1 Ru3B C32B 91(2) . . . . ? Si1 C1 Ru3B C32B -31(2) . . . . ? Ru2 C1 Ru3B C32B -142(2) . . . . ? Ru1 C1 Ru3B C32B 155(2) . . . . ? Ru3A C1 Ru3B C32B 148(5) . . . . ? C2 C1 Ru3B C31B -52(12) . . . . ? Si1 C1 Ru3B C31B -174(12) . . . . ? Ru2 C1 Ru3B C31B 75(12) . . . . ? Ru1 C1 Ru3B C31B 11(12) . . . . ? Ru3A C1 Ru3B C31B 5(12) . . . . ? C2 C1 Ru3B C23 -164.7(6) . . . . ? Si1 C1 Ru3B C23 73.6(6) . . . . ? Ru2 C1 Ru3B C23 -37.4(4) . . . . ? Ru1 C1 Ru3B C23 -101.1(5) . . . . ? Ru3A C1 Ru3B C23 -108(5) . . . . ? Si1 C1 Ru3B C2 -121.6(4) . . . . ? Ru2 C1 Ru3B C2 127.3(3) . . . . ? Ru1 C1 Ru3B C2 63.7(3) . . . . ? Ru3A C1 Ru3B C2 57(5) . . . . ? C2 C1 Ru3B C4 -72.1(3) . . . . ? Si1 C1 Ru3B C4 166.3(3) . . . . ? Ru2 C1 Ru3B C4 55.20(17) . . . . ? Ru1 C1 Ru3B C4 -8.5(2) . . . . ? Ru3A C1 Ru3B C4 -15(4) . . . . ? C2 C1 Ru3B C3 -32.9(2) . . . . ? Si1 C1 Ru3B C3 -154.5(3) . . . . ? Ru2 C1 Ru3B C3 94.4(3) . . . . ? Ru1 C1 Ru3B C3 30.8(2) . . . . ? Ru3A C1 Ru3B C3 24(4) . . . . ? C2 C1 Ru3B Ru2 -127.3(3) . . . . ? Si1 C1 Ru3B Ru2 111.1(3) . . . . ? Ru1 C1 Ru3B Ru2 -63.7(2) . . . . ? Ru3A C1 Ru3B Ru2 -70(5) . . . . ? C1 C2 Ru3B C32B -103(2) . . . . ? C3 C2 Ru3B C32B 132(2) . . . . ? C7 C2 Ru3B C32B 16(2) . . . . ? Ru3A C2 Ru3B C32B 131(5) . . . . ? Ru1 C2 Ru3B C32B -165(2) . . . . ? C1 C2 Ru3B C31B 170(3) . . . . ? C3 C2 Ru3B C31B 45(3) . . . . ? C7 C2 Ru3B C31B -71(3) . . . . ? Ru3A C2 Ru3B C31B 45(4) . . . . ? Ru1 C2 Ru3B C31B 108(3) . . . . ? C1 C2 Ru3B C23 19.5(9) . . . . ? C3 C2 Ru3B C23 -105.6(10) . . . . ? C7 C2 Ru3B C23 138.7(8) . . . . ? Ru3A C2 Ru3B C23 -106(4) . . . . ? Ru1 C2 Ru3B C23 -42.3(11) . . . . ? C3 C2 Ru3B C1 -125.1(4) . . . . ? C7 C2 Ru3B C1 119.2(5) . . . . ? Ru3A C2 Ru3B C1 -126(4) . . . . ? Ru1 C2 Ru3B C1 -61.8(3) . . . . ? C1 C2 Ru3B C4 91.3(3) . . . . ? C3 C2 Ru3B C4 -33.8(3) . . . . ? C7 C2 Ru3B C4 -149.5(4) . . . . ? Ru3A C2 Ru3B C4 -34(4) . . . . ? Ru1 C2 Ru3B C4 29.5(3) . . . . ? C1 C2 Ru3B C3 125.1(4) . . . . ? C7 C2 Ru3B C3 -115.7(5) . . . . ? Ru3A C2 Ru3B C3 -1(4) . . . . ? Ru1 C2 Ru3B C3 63.2(2) . . . . ? C1 C2 Ru3B Ru2 40.3(3) . . . . ? C3 C2 Ru3B Ru2 -84.8(3) . . . . ? C7 C2 Ru3B Ru2 159.5(4) . . . . ? Ru3A C2 Ru3B Ru2 -85(4) . . . . ? Ru1 C2 Ru3B Ru2 -21.6(4) . . . . ? C3 C4 Ru3B C32B -25(6) . . . . ? Ru2 C4 Ru3B C32B -157(6) . . . . ? Ru3A C4 Ru3B C32B 58(8) . . . . ? Ru1 C4 Ru3B C32B -90(6) . . . . ? C3 C4 Ru3B C31B -103.4(17) . . . . ? Ru2 C4 Ru3B C31B 124.6(17) . . . . ? Ru3A C4 Ru3B C31B -21(7) . . . . ? Ru1 C4 Ru3B C31B -168.4(17) . . . . ? C3 C4 Ru3B C23 165.5(5) . . . . ? Ru2 C4 Ru3B C23 33.5(3) . . . . ? Ru3A C4 Ru3B C23 -112(7) . . . . ? Ru1 C4 Ru3B C23 100.4(4) . . . . ? C3 C4 Ru3B C1 73.8(3) . . . . ? Ru2 C4 Ru3B C1 -58.23(19) . . . . ? Ru3A C4 Ru3B C1 156(7) . . . . ? Ru1 C4 Ru3B C1 8.7(3) . . . . ? C3 C4 Ru3B C2 34.0(2) . . . . ? Ru2 C4 Ru3B C2 -98.0(3) . . . . ? Ru3A C4 Ru3B C2 117(7) . . . . ? Ru1 C4 Ru3B C2 -31.0(3) . . . . ? Ru2 C4 Ru3B C3 -132.0(3) . . . . ? Ru3A C4 Ru3B C3 83(7) . . . . ? Ru1 C4 Ru3B C3 -65.1(3) . . . . ? C3 C4 Ru3B Ru2 132.0(3) . . . . ? Ru3A C4 Ru3B Ru2 -145(7) . . . . ? Ru1 C4 Ru3B Ru2 66.94(17) . . . . ? C4 C3 Ru3B C32B 172(2) . . . . ? C2 C3 Ru3B C32B -65(2) . . . . ? Si2 C3 Ru3B C32B 55(2) . . . . ? Ru3A C3 Ru3B C32B 114(6) . . . . ? Ru1 C3 Ru3B C32B -129(2) . . . . ? C4 C3 Ru3B C31B 86.9(18) . . . . ? C2 C3 Ru3B C31B -149.9(18) . . . . ? Si2 C3 Ru3B C31B -29.5(19) . . . . ? Ru3A C3 Ru3B C31B 29(5) . . . . ? Ru1 C3 Ru3B C31B 146.8(18) . . . . ? C4 C3 Ru3B C23 -18.6(7) . . . . ? C2 C3 Ru3B C23 104.7(8) . . . . ? Si2 C3 Ru3B C23 -134.9(6) . . . . ? Ru3A C3 Ru3B C23 -76(5) . . . . ? Ru1 C3 Ru3B C23 41.4(8) . . . . ? C4 C3 Ru3B C1 -90.2(3) . . . . ? C2 C3 Ru3B C1 33.0(2) . . . . ? Si2 C3 Ru3B C1 153.4(3) . . . . ? Ru3A C3 Ru3B C1 -148(5) . . . . ? Ru1 C3 Ru3B C1 -30.3(3) . . . . ? C4 C3 Ru3B C2 -123.3(3) . . . . ? Si2 C3 Ru3B C2 120.4(4) . . . . ? Ru3A C3 Ru3B C2 18E1(10) . . . . ? Ru1 C3 Ru3B C2 -63.3(2) . . . . ? C2 C3 Ru3B C4 123.3(3) . . . . ? Si2 C3 Ru3B C4 -116.3(4) . . . . ? Ru3A C3 Ru3B C4 -58(5) . . . . ? Ru1 C3 Ru3B C4 60.0(3) . . . . ? C4 C3 Ru3B Ru2 -35.8(3) . . . . ? C2 C3 Ru3B Ru2 87.4(3) . . . . ? Si2 C3 Ru3B Ru2 -152.2(3) . . . . ? Ru3A C3 Ru3B Ru2 -93(5) . . . . ? Ru1 C3 Ru3B Ru2 24.1(3) . . . . ? C32B Ru3B C31B O31B -1E1(3) . . . . ? C23 Ru3B C31B O31B -12E1(3) . . . . ? C1 Ru3B C31B O31B 13E1(3) . . . . ? C2 Ru3B C31B O31B 9E1(3) . . . . ? C4 Ru3B C31B O31B 15E1(3) . . . . ? C3 Ru3B C31B O31B 11E1(3) . . . . ? Ru2 Ru3B C31B O31B -16E1(3) . . . . ? C31B Ru3B C32B O32B -178(9) . . . . ? C23 Ru3B C32B O32B -91(8) . . . . ? C1 Ru3B C32B O32B 8(9) . . . . ? C2 Ru3B C32B O32B 47(9) . . . . ? C4 Ru3B C32B O32B 100(11) . . . . ? C3 Ru3B C32B O32B 81(9) . . . . ? Ru2 Ru3B C32B O32B -49(9) . . . . ? O13 C13 Ru1 C14 119(16) . . . . ? O13 C13 Ru1 C12 -145(16) . . . . ? O13 C13 Ru1 C4 -49(16) . . . . ? O13 C13 Ru1 C1 -11(16) . . . . ? O13 C13 Ru1 C3 -12(16) . . . . ? O13 C13 Ru1 C2 13(16) . . . . ? O13 C13 Ru1 Ru2 -96(16) . . . . ? O14 C14 Ru1 C13 3E1(2) . . . . ? O14 C14 Ru1 C12 -7E1(2) . . . . ? O14 C14 Ru1 C4 15E1(2) . . . . ? O14 C14 Ru1 C1 -16E1(2) . . . . ? O14 C14 Ru1 C3 13E1(2) . . . . ? O14 C14 Ru1 C2 16E1(2) . . . . ? O14 C14 Ru1 Ru2 -11E1(2) . . . . ? O12 C12 Ru1 C13 -50.4(6) . . . . ? Ru2 C12 Ru1 C13 131.58(18) . . . . ? O12 C12 Ru1 C14 37.1(6) . . . . ? Ru2 C12 Ru1 C14 -140.96(17) . . . . ? O12 C12 Ru1 C4 -149.9(6) . . . . ? Ru2 C12 Ru1 C4 32.06(15) . . . . ? O12 C12 Ru1 C1 139.6(6) . . . . ? Ru2 C12 Ru1 C1 -38.48(14) . . . . ? O12 C12 Ru1 C3 -162.1(5) . . . . ? Ru2 C12 Ru1 C3 19.8(2) . . . . ? O12 C12 Ru1 C2 150.2(5) . . . . ? Ru2 C12 Ru1 C2 -27.9(2) . . . . ? O12 C12 Ru1 Ru2 178.1(7) . . . . ? C3 C4 Ru1 C13 97.2(3) . . . . ? Ru2 C4 Ru1 C13 -131.50(16) . . . . ? Ru3A C4 Ru1 C13 161.0(2) . . . . ? Ru3B C4 Ru1 C13 162.4(3) . . . . ? C3 C4 Ru1 C14 -18.0(9) . . . . ? Ru2 C4 Ru1 C14 113.3(8) . . . . ? Ru3A C4 Ru1 C14 45.8(9) . . . . ? Ru3B C4 Ru1 C14 47.2(9) . . . . ? C3 C4 Ru1 C12 -164.5(3) . . . . ? Ru2 C4 Ru1 C12 -33.17(15) . . . . ? Ru3A C4 Ru1 C12 -100.6(2) . . . . ? Ru3B C4 Ru1 C12 -99.3(3) . . . . ? C3 C4 Ru1 C1 -73.8(2) . . . . ? Ru2 C4 Ru1 C1 57.48(13) . . . . ? Ru3A C4 Ru1 C1 -9.99(19) . . . . ? Ru3B C4 Ru1 C1 -8.6(3) . . . . ? Ru2 C4 Ru1 C3 131.3(3) . . . . ? Ru3A C4 Ru1 C3 63.8(3) . . . . ? Ru3B C4 Ru1 C3 65.2(3) . . . . ? C3 C4 Ru1 C2 -34.7(2) . . . . ? Ru2 C4 Ru1 C2 96.60(15) . . . . ? Ru3A C4 Ru1 C2 29.1(2) . . . . ? Ru3B C4 Ru1 C2 30.5(3) . . . . ? C3 C4 Ru1 Ru2 -131.3(3) . . . . ? Ru3A C4 Ru1 Ru2 -67.5(2) . . . . ? Ru3B C4 Ru1 Ru2 -66.1(3) . . . . ? C2 C1 Ru1 C13 31.6(9) . . . . ? Si1 C1 Ru1 C13 153.7(7) . . . . ? Ru2 C1 Ru1 C13 -95.5(8) . . . . ? Ru3B C1 Ru1 C13 -31.7(9) . . . . ? Ru3A C1 Ru1 C13 -31.3(8) . . . . ? C2 C1 Ru1 C14 -97.4(3) . . . . ? Si1 C1 Ru1 C14 24.7(3) . . . . ? Ru2 C1 Ru1 C14 135.50(15) . . . . ? Ru3B C1 Ru1 C14 -160.7(3) . . . . ? Ru3A C1 Ru1 C14 -160.3(2) . . . . ? C2 C1 Ru1 C12 165.7(3) . . . . ? Si1 C1 Ru1 C12 -72.2(3) . . . . ? Ru2 C1 Ru1 C12 38.63(15) . . . . ? Ru3B C1 Ru1 C12 102.5(3) . . . . ? Ru3A C1 Ru1 C12 102.9(2) . . . . ? C2 C1 Ru1 C4 71.9(2) . . . . ? Si1 C1 Ru1 C4 -166.0(3) . . . . ? Ru2 C1 Ru1 C4 -55.18(13) . . . . ? Ru3B C1 Ru1 C4 8.6(2) . . . . ? Ru3A C1 Ru1 C4 9.06(18) . . . . ? C2 C1 Ru1 C3 31.8(2) . . . . ? Si1 C1 Ru1 C3 153.9(3) . . . . ? Ru2 C1 Ru1 C3 -95.26(15) . . . . ? Ru3B C1 Ru1 C3 -31.4(2) . . . . ? Ru3A C1 Ru1 C3 -31.02(18) . . . . ? Si1 C1 Ru1 C2 122.1(4) . . . . ? Ru2 C1 Ru1 C2 -127.1(3) . . . . ? Ru3B C1 Ru1 C2 -63.3(3) . . . . ? Ru3A C1 Ru1 C2 -62.8(2) . . . . ? C2 C1 Ru1 Ru2 127.1(3) . . . . ? Si1 C1 Ru1 Ru2 -110.8(3) . . . . ? Ru3B C1 Ru1 Ru2 63.8(2) . . . . ? Ru3A C1 Ru1 Ru2 64.24(16) . . . . ? C4 C3 Ru1 C13 -89.7(3) . . . . ? C2 C3 Ru1 C13 148.5(3) . . . . ? Si2 C3 Ru1 C13 26.2(3) . . . . ? Ru3A C3 Ru1 C13 -147.7(2) . . . . ? Ru3B C3 Ru1 C13 -150.2(4) . . . . ? C4 C3 Ru1 C14 174.9(3) . . . . ? C2 C3 Ru1 C14 53.1(3) . . . . ? Si2 C3 Ru1 C14 -69.2(3) . . . . ? Ru3A C3 Ru1 C14 116.9(3) . . . . ? Ru3B C3 Ru1 C14 114.4(4) . . . . ? C4 C3 Ru1 C12 20.4(3) . . . . ? C2 C3 Ru1 C12 -101.5(3) . . . . ? Si2 C3 Ru1 C12 136.3(2) . . . . ? Ru3A C3 Ru1 C12 -37.6(3) . . . . ? Ru3B C3 Ru1 C12 -40.1(4) . . . . ? C2 C3 Ru1 C4 -121.8(3) . . . . ? Si2 C3 Ru1 C4 115.9(4) . . . . ? Ru3A C3 Ru1 C4 -58.0(3) . . . . ? Ru3B C3 Ru1 C4 -60.5(4) . . . . ? C4 C3 Ru1 C1 90.4(3) . . . . ? C2 C3 Ru1 C1 -31.5(2) . . . . ? Si2 C3 Ru1 C1 -153.7(3) . . . . ? Ru3A C3 Ru1 C1 32.4(2) . . . . ? Ru3B C3 Ru1 C1 29.9(3) . . . . ? C4 C3 Ru1 C2 121.8(3) . . . . ? Si2 C3 Ru1 C2 -122.3(4) . . . . ? Ru3A C3 Ru1 C2 63.9(3) . . . . ? Ru3B C3 Ru1 C2 61.4(4) . . . . ? C4 C3 Ru1 Ru2 36.4(2) . . . . ? C2 C3 Ru1 Ru2 -85.4(2) . . . . ? Si2 C3 Ru1 Ru2 152.3(3) . . . . ? Ru3A C3 Ru1 Ru2 -21.54(19) . . . . ? Ru3B C3 Ru1 Ru2 -24.1(3) . . . . ? C1 C2 Ru1 C13 -170.4(3) . . . . ? C3 C2 Ru1 C13 -43.0(3) . . . . ? C7 C2 Ru1 C13 70.5(5) . . . . ? Ru3A C2 Ru1 C13 -105.0(3) . . . . ? Ru3B C2 Ru1 C13 -108.4(5) . . . . ? C1 C2 Ru1 C14 91.4(3) . . . . ? C3 C2 Ru1 C14 -141.2(3) . . . . ? C7 C2 Ru1 C14 -27.6(4) . . . . ? Ru3A C2 Ru1 C14 156.9(2) . . . . ? Ru3B C2 Ru1 C14 153.5(4) . . . . ? C1 C2 Ru1 C12 -18.0(3) . . . . ? C3 C2 Ru1 C12 109.4(3) . . . . ? C7 C2 Ru1 C12 -137.1(4) . . . . ? Ru3A C2 Ru1 C12 47.4(3) . . . . ? Ru3B C2 Ru1 C12 44.0(5) . . . . ? C1 C2 Ru1 C4 -92.3(3) . . . . ? C3 C2 Ru1 C4 35.1(2) . . . . ? C7 C2 Ru1 C4 148.7(4) . . . . ? Ru3A C2 Ru1 C4 -26.9(2) . . . . ? Ru3B C2 Ru1 C4 -30.3(4) . . . . ? C3 C2 Ru1 C1 127.4(3) . . . . ? C7 C2 Ru1 C1 -119.0(5) . . . . ? Ru3A C2 Ru1 C1 65.4(3) . . . . ? Ru3B C2 Ru1 C1 62.1(4) . . . . ? C1 C2 Ru1 C3 -127.4(3) . . . . ? C7 C2 Ru1 C3 113.5(5) . . . . ? Ru3A C2 Ru1 C3 -62.0(3) . . . . ? Ru3B C2 Ru1 C3 -65.4(4) . . . . ? C1 C2 Ru1 Ru2 -40.5(2) . . . . ? C3 C2 Ru1 Ru2 87.0(2) . . . . ? C7 C2 Ru1 Ru2 -159.5(4) . . . . ? Ru3A C2 Ru1 Ru2 24.99(17) . . . . ? Ru3B C2 Ru1 Ru2 21.6(4) . . . . ? O22 C22 Ru2 C21 -144(8) . . . . ? O22 C22 Ru2 C4 36(8) . . . . ? O22 C22 Ru2 C23 -57(8) . . . . ? O22 C22 Ru2 C12 128(8) . . . . ? O22 C22 Ru2 C1 31(8) . . . . ? O22 C22 Ru2 Ru3A -15(8) . . . . ? O22 C22 Ru2 Ru1 86(8) . . . . ? O22 C22 Ru2 Ru3B -18(8) . . . . ? O21 C21 Ru2 C22 11(11) . . . . ? O21 C21 Ru2 C4 -168(9) . . . . ? O21 C21 Ru2 C23 -79(11) . . . . ? O21 C21 Ru2 C12 104(11) . . . . ? O21 C21 Ru2 C1 -167(11) . . . . ? O21 C21 Ru2 Ru3A -110(11) . . . . ? O21 C21 Ru2 Ru1 136(11) . . . . ? O21 C21 Ru2 Ru3B -111(11) . . . . ? C3 C4 Ru2 C22 -178.5(3) . . . . ? Ru3A C4 Ru2 C22 -119.3(2) . . . . ? Ru1 C4 Ru2 C22 122.82(16) . . . . ? Ru3B C4 Ru2 C22 -120.7(3) . . . . ? C3 C4 Ru2 C21 1(3) . . . . ? Ru3A C4 Ru2 C21 60(3) . . . . ? Ru1 C4 Ru2 C21 -58(3) . . . . ? Ru3B C4 Ru2 C21 58(3) . . . . ? C3 C4 Ru2 C23 -88.1(4) . . . . ? Ru3A C4 Ru2 C23 -28.9(2) . . . . ? Ru1 C4 Ru2 C23 -146.74(16) . . . . ? Ru3B C4 Ru2 C23 -30.3(3) . . . . ? C3 C4 Ru2 C12 89.0(3) . . . . ? Ru3A C4 Ru2 C12 148.17(18) . . . . ? Ru1 C4 Ru2 C12 30.30(15) . . . . ? Ru3B C4 Ru2 C12 146.8(3) . . . . ? C3 C4 Ru2 C1 0.3(3) . . . . ? Ru3A C4 Ru2 C1 59.49(17) . . . . ? Ru1 C4 Ru2 C1 -58.37(12) . . . . ? Ru3B C4 Ru2 C1 58.1(3) . . . . ? C3 C4 Ru2 Ru3A -59.2(3) . . . . ? Ru1 C4 Ru2 Ru3A -117.86(19) . . . . ? Ru3B C4 Ru2 Ru3A -1.4(3) . . . . ? C3 C4 Ru2 Ru1 58.7(3) . . . . ? Ru3A C4 Ru2 Ru1 117.86(19) . . . . ? Ru3B C4 Ru2 Ru1 116.5(3) . . . . ? C3 C4 Ru2 Ru3B -57.8(4) . . . . ? Ru3A C4 Ru2 Ru3B 1.4(3) . . . . ? Ru1 C4 Ru2 Ru3B -116.5(3) . . . . ? O23 C23 Ru2 C22 -52.4(8) . . . . ? Ru3B C23 Ru2 C22 128.5(5) . . . . ? Ru3A C23 Ru2 C22 124.7(2) . . . . ? O23 C23 Ru2 C21 37.1(8) . . . . ? Ru3B C23 Ru2 C21 -142.1(5) . . . . ? Ru3A C23 Ru2 C21 -145.8(3) . . . . ? O23 C23 Ru2 C4 -145.9(7) . . . . ? Ru3B C23 Ru2 C4 34.9(5) . . . . ? Ru3A C23 Ru2 C4 31.2(2) . . . . ? O23 C23 Ru2 C12 63(2) . . . . ? Ru3B C23 Ru2 C12 -116.4(16) . . . . ? Ru3A C23 Ru2 C12 -120.1(16) . . . . ? O23 C23 Ru2 C1 140.9(8) . . . . ? Ru3B C23 Ru2 C1 -38.3(5) . . . . ? Ru3A C23 Ru2 C1 -42.0(2) . . . . ? O23 C23 Ru2 Ru3A -177.1(9) . . . . ? Ru3B C23 Ru2 Ru3A 3.8(5) . . . . ? O23 C23 Ru2 Ru1 175.2(6) . . . . ? Ru3B C23 Ru2 Ru1 -4.0(5) . . . . ? Ru3A C23 Ru2 Ru1 -7.7(3) . . . . ? O23 C23 Ru2 Ru3B 179.2(10) . . . . ? Ru3A C23 Ru2 Ru3B -3.8(5) . . . . ? O12 C12 Ru2 C22 54.5(5) . . . . ? Ru1 C12 Ru2 C22 -127.21(17) . . . . ? O12 C12 Ru2 C21 -34.9(5) . . . . ? Ru1 C12 Ru2 C21 143.40(19) . . . . ? O12 C12 Ru2 C4 148.1(5) . . . . ? Ru1 C12 Ru2 C4 -33.58(17) . . . . ? O12 C12 Ru2 C23 -60.6(18) . . . . ? Ru1 C12 Ru2 C23 117.7(16) . . . . ? O12 C12 Ru2 C1 -138.6(5) . . . . ? Ru1 C12 Ru2 C1 39.65(14) . . . . ? O12 C12 Ru2 Ru3A -175.6(5) . . . . ? Ru1 C12 Ru2 Ru3A 2.7(3) . . . . ? O12 C12 Ru2 Ru1 -178.3(6) . . . . ? O12 C12 Ru2 Ru3B -171.4(6) . . . . ? Ru1 C12 Ru2 Ru3B 6.9(5) . . . . ? C2 C1 Ru2 C22 3.8(9) . . . . ? Si1 C1 Ru2 C22 -175.6(6) . . . . ? Ru3B C1 Ru2 C22 -54.4(8) . . . . ? Ru1 C1 Ru2 C22 62.7(7) . . . . ? Ru3A C1 Ru2 C22 -51.0(7) . . . . ? C2 C1 Ru2 C21 178.6(3) . . . . ? Si1 C1 Ru2 C21 -0.7(2) . . . . ? Ru3B C1 Ru2 C21 120.4(4) . . . . ? Ru1 C1 Ru2 C21 -122.50(15) . . . . ? Ru3A C1 Ru2 C21 123.8(2) . . . . ? C2 C1 Ru2 C4 -1.4(3) . . . . ? Si1 C1 Ru2 C4 179.2(2) . . . . ? Ru3B C1 Ru2 C4 -59.6(4) . . . . ? Ru1 C1 Ru2 C4 57.48(13) . . . . ? Ru3A C1 Ru2 C4 -56.23(19) . . . . ? C2 C1 Ru2 C23 91.9(3) . . . . ? Si1 C1 Ru2 C23 -87.4(2) . . . . ? Ru3B C1 Ru2 C23 33.7(4) . . . . ? Ru1 C1 Ru2 C23 150.81(17) . . . . ? Ru3A C1 Ru2 C23 37.1(2) . . . . ? C2 C1 Ru2 C12 -94.1(3) . . . . ? Si1 C1 Ru2 C12 86.6(2) . . . . ? Ru3B C1 Ru2 C12 -152.3(4) . . . . ? Ru1 C1 Ru2 C12 -35.21(13) . . . . ? Ru3A C1 Ru2 C12 -148.91(19) . . . . ? C2 C1 Ru2 Ru3A 54.8(3) . . . . ? Si1 C1 Ru2 Ru3A -124.5(3) . . . . ? Ru3B C1 Ru2 Ru3A -3.4(4) . . . . ? Ru1 C1 Ru2 Ru3A 113.71(18) . . . . ? C2 C1 Ru2 Ru1 -58.9(2) . . . . ? Si1 C1 Ru2 Ru1 121.8(2) . . . . ? Ru3B C1 Ru2 Ru1 -117.1(4) . . . . ? Ru3A C1 Ru2 Ru1 -113.71(18) . . . . ? C2 C1 Ru2 Ru3B 58.2(5) . . . . ? Si1 C1 Ru2 Ru3B -121.1(5) . . . . ? Ru1 C1 Ru2 Ru3B 117.1(4) . . . . ? Ru3A C1 Ru2 Ru3B 3.4(4) . . . . ? C32A Ru3A Ru2 C22 -131.9(11) . . . . ? C31A Ru3A Ru2 C22 5.8(11) . . . . ? C23 Ru3A Ru2 C22 -65.4(3) . . . . ? C4 Ru3A Ru2 C22 74.3(2) . . . . ? C3 Ru3A Ru2 C22 102.5(2) . . . . ? C2 Ru3A Ru2 C22 140.7(2) . . . . ? C1 Ru3A Ru2 C22 168.63(19) . . . . ? C32A Ru3A Ru2 C21 -23.0(11) . . . . ? C31A Ru3A Ru2 C21 114.7(11) . . . . ? C23 Ru3A Ru2 C21 43.5(3) . . . . ? C4 Ru3A Ru2 C21 -176.8(2) . . . . ? C3 Ru3A Ru2 C21 -148.6(2) . . . . ? C2 Ru3A Ru2 C21 -110.4(2) . . . . ? C1 Ru3A Ru2 C21 -82.4(2) . . . . ? C32A Ru3A Ru2 C4 153.8(11) . . . . ? C31A Ru3A Ru2 C4 -68.5(11) . . . . ? C23 Ru3A Ru2 C4 -139.7(3) . . . . ? C3 Ru3A Ru2 C4 28.2(2) . . . . ? C2 Ru3A Ru2 C4 66.4(2) . . . . ? C1 Ru3A Ru2 C4 94.4(2) . . . . ? C32A Ru3A Ru2 C23 -66.5(11) . . . . ? C31A Ru3A Ru2 C23 71.2(11) . . . . ? C4 Ru3A Ru2 C23 139.7(3) . . . . ? C3 Ru3A Ru2 C23 167.9(3) . . . . ? C2 Ru3A Ru2 C23 -153.9(3) . . . . ? C1 Ru3A Ru2 C23 -126.0(3) . . . . ? C32A Ru3A Ru2 C12 106.0(11) . . . . ? C31A Ru3A Ru2 C12 -116.3(11) . . . . ? C23 Ru3A Ru2 C12 172.5(3) . . . . ? C4 Ru3A Ru2 C12 -47.8(3) . . . . ? C3 Ru3A Ru2 C12 -19.6(3) . . . . ? C2 Ru3A Ru2 C12 18.6(3) . . . . ? C1 Ru3A Ru2 C12 46.5(3) . . . . ? C32A Ru3A Ru2 C1 59.5(11) . . . . ? C31A Ru3A Ru2 C1 -162.8(11) . . . . ? C23 Ru3A Ru2 C1 126.0(3) . . . . ? C4 Ru3A Ru2 C1 -94.4(2) . . . . ? C3 Ru3A Ru2 C1 -66.11(18) . . . . ? C2 Ru3A Ru2 C1 -27.93(16) . . . . ? C32A Ru3A Ru2 Ru1 108.0(11) . . . . ? C31A Ru3A Ru2 Ru1 -114.3(11) . . . . ? C23 Ru3A Ru2 Ru1 174.5(2) . . . . ? C4 Ru3A Ru2 Ru1 -45.79(16) . . . . ? C3 Ru3A Ru2 Ru1 -17.55(15) . . . . ? C2 Ru3A Ru2 Ru1 20.64(15) . . . . ? C1 Ru3A Ru2 Ru1 48.57(14) . . . . ? C32A Ru3A Ru2 Ru3B -4(4) . . . . ? C31A Ru3A Ru2 Ru3B 133(5) . . . . ? C23 Ru3A Ru2 Ru3B 62(4) . . . . ? C4 Ru3A Ru2 Ru3B -158(4) . . . . ? C3 Ru3A Ru2 Ru3B -130(4) . . . . ? C2 Ru3A Ru2 Ru3B -92(4) . . . . ? C1 Ru3A Ru2 Ru3B -64(4) . . . . ? C13 Ru1 Ru2 C22 -4.0(2) . . . . ? C14 Ru1 Ru2 C22 123.7(2) . . . . ? C12 Ru1 Ru2 C22 64.7(2) . . . . ? C4 Ru1 Ru2 C22 -72.3(2) . . . . ? C1 Ru1 Ru2 C22 -166.62(19) . . . . ? C3 Ru1 Ru2 C22 -99.97(18) . . . . ? C2 Ru1 Ru2 C22 -137.65(18) . . . . ? C13 Ru1 Ru2 C21 -114.8(2) . . . . ? C14 Ru1 Ru2 C21 12.9(3) . . . . ? C12 Ru1 Ru2 C21 -46.1(2) . . . . ? C4 Ru1 Ru2 C21 176.9(2) . . . . ? C1 Ru1 Ru2 C21 82.6(2) . . . . ? C3 Ru1 Ru2 C21 149.2(2) . . . . ? C2 Ru1 Ru2 C21 111.6(2) . . . . ? C13 Ru1 Ru2 C4 68.3(2) . . . . ? C14 Ru1 Ru2 C4 -164.0(2) . . . . ? C12 Ru1 Ru2 C4 137.0(2) . . . . ? C1 Ru1 Ru2 C4 -94.32(19) . . . . ? C3 Ru1 Ru2 C4 -27.67(18) . . . . ? C2 Ru1 Ru2 C4 -65.34(17) . . . . ? C13 Ru1 Ru2 C23 119.1(3) . . . . ? C14 Ru1 Ru2 C23 -113.3(3) . . . . ? C12 Ru1 Ru2 C23 -172.3(3) . . . . ? C4 Ru1 Ru2 C23 50.7(3) . . . . ? C1 Ru1 Ru2 C23 -43.6(3) . . . . ? C3 Ru1 Ru2 C23 23.1(2) . . . . ? C2 Ru1 Ru2 C23 -14.6(2) . . . . ? C13 Ru1 Ru2 C12 -68.6(2) . . . . ? C14 Ru1 Ru2 C12 59.0(2) . . . . ? C4 Ru1 Ru2 C12 -137.0(2) . . . . ? C1 Ru1 Ru2 C12 128.7(2) . . . . ? C3 Ru1 Ru2 C12 -164.64(19) . . . . ? C2 Ru1 Ru2 C12 157.68(19) . . . . ? C13 Ru1 Ru2 C1 162.7(2) . . . . ? C14 Ru1 Ru2 C1 -69.7(2) . . . . ? C12 Ru1 Ru2 C1 -128.7(2) . . . . ? C4 Ru1 Ru2 C1 94.32(19) . . . . ? C3 Ru1 Ru2 C1 66.65(16) . . . . ? C2 Ru1 Ru2 C1 28.97(16) . . . . ? C13 Ru1 Ru2 Ru3A 113.3(2) . . . . ? C14 Ru1 Ru2 Ru3A -119.1(2) . . . . ? C12 Ru1 Ru2 Ru3A -178.06(19) . . . . ? C4 Ru1 Ru2 Ru3A 44.97(18) . . . . ? C1 Ru1 Ru2 Ru3A -49.35(17) . . . . ? C3 Ru1 Ru2 Ru3A 17.30(16) . . . . ? C2 Ru1 Ru2 Ru3A -20.37(15) . . . . ? C13 Ru1 Ru2 Ru3B 116.2(4) . . . . ? C14 Ru1 Ru2 Ru3B -116.2(4) . . . . ? C12 Ru1 Ru2 Ru3B -175.2(4) . . . . ? C4 Ru1 Ru2 Ru3B 47.8(4) . . . . ? C1 Ru1 Ru2 Ru3B -46.5(3) . . . . ? C3 Ru1 Ru2 Ru3B 20.2(3) . . . . ? C2 Ru1 Ru2 Ru3B -17.5(3) . . . . ? C32B Ru3B Ru2 C22 -116(2) . . . . ? C31B Ru3B Ru2 C22 -2(2) . . . . ? C23 Ru3B Ru2 C22 -61.6(5) . . . . ? C1 Ru3B Ru2 C22 167.9(2) . . . . ? C2 Ru3B Ru2 C22 138.8(3) . . . . ? C4 Ru3B Ru2 C22 74.7(3) . . . . ? C3 Ru3B Ru2 C22 101.4(3) . . . . ? C32B Ru3B Ru2 C21 -7(2) . . . . ? C31B Ru3B Ru2 C21 106(2) . . . . ? C23 Ru3B Ru2 C21 46.7(5) . . . . ? C1 Ru3B Ru2 C21 -83.7(3) . . . . ? C2 Ru3B Ru2 C21 -112.8(4) . . . . ? C4 Ru3B Ru2 C21 -176.9(2) . . . . ? C3 Ru3B Ru2 C21 -150.2(3) . . . . ? C32B Ru3B Ru2 C4 169(2) . . . . ? C31B Ru3B Ru2 C4 -77(2) . . . . ? C23 Ru3B Ru2 C4 -136.3(5) . . . . ? C1 Ru3B Ru2 C4 93.2(3) . . . . ? C2 Ru3B Ru2 C4 64.2(3) . . . . ? C3 Ru3B Ru2 C4 26.8(2) . . . . ? C32B Ru3B Ru2 C23 -54(2) . . . . ? C31B Ru3B Ru2 C23 59(2) . . . . ? C1 Ru3B Ru2 C23 -130.5(6) . . . . ? C2 Ru3B Ru2 C23 -159.5(7) . . . . ? C4 Ru3B Ru2 C23 136.3(5) . . . . ? C3 Ru3B Ru2 C23 163.1(6) . . . . ? C32B Ru3B Ru2 C12 118(2) . . . . ? C31B Ru3B Ru2 C12 -129(2) . . . . ? C23 Ru3B Ru2 C12 172.1(3) . . . . ? C1 Ru3B Ru2 C12 41.6(6) . . . . ? C2 Ru3B Ru2 C12 12.6(7) . . . . ? C4 Ru3B Ru2 C12 -51.6(5) . . . . ? C3 Ru3B Ru2 C12 -24.8(6) . . . . ? C32B Ru3B Ru2 C1 76(2) . . . . ? C31B Ru3B Ru2 C1 -170(2) . . . . ? C23 Ru3B Ru2 C1 130.5(6) . . . . ? C2 Ru3B Ru2 C1 -29.1(2) . . . . ? C4 Ru3B Ru2 C1 -93.2(3) . . . . ? C3 Ru3B Ru2 C1 -66.5(2) . . . . ? C32B Ru3B Ru2 Ru3A -169(5) . . . . ? C31B Ru3B Ru2 Ru3A -56(5) . . . . ? C23 Ru3B Ru2 Ru3A -115(4) . . . . ? C1 Ru3B Ru2 Ru3A 114(4) . . . . ? C2 Ru3B Ru2 Ru3A 85(4) . . . . ? C4 Ru3B Ru2 Ru3A 21(4) . . . . ? C3 Ru3B Ru2 Ru3A 48(4) . . . . ? C32B Ru3B Ru2 Ru1 123(2) . . . . ? C31B Ru3B Ru2 Ru1 -124(2) . . . . ? C23 Ru3B Ru2 Ru1 177.2(4) . . . . ? C1 Ru3B Ru2 Ru1 46.7(3) . . . . ? C2 Ru3B Ru2 Ru1 17.7(4) . . . . ? C4 Ru3B Ru2 Ru1 -46.49(19) . . . . ? C3 Ru3B Ru2 Ru1 -19.7(3) . . . . ? C2 C1 Si1 C6 129.2(4) . . . . ? Ru2 C1 Si1 C6 -51.5(3) . . . . ? Ru3B C1 Si1 C6 -138.4(4) . . . . ? Ru1 C1 Si1 C6 35.4(4) . . . . ? Ru3A C1 Si1 C6 -138.5(3) . . . . ? C2 C1 Si1 C8 9.7(5) . . . . ? Ru2 C1 Si1 C8 -171.0(4) . . . . ? Ru3B C1 Si1 C8 102.1(5) . . . . ? Ru1 C1 Si1 C8 -84.1(4) . . . . ? Ru3A C1 Si1 C8 102.0(4) . . . . ? C2 C1 Si1 C5 -111.7(5) . . . . ? Ru2 C1 Si1 C5 67.6(4) . . . . ? Ru3B C1 Si1 C5 -19.3(5) . . . . ? Ru1 C1 Si1 C5 154.5(4) . . . . ? Ru3A C1 Si1 C5 -19.4(5) . . . . ? C4 C3 Si2 C11 120.3(4) . . . . ? C2 C3 Si2 C11 -60.3(4) . . . . ? Ru3A C3 Si2 C11 -153.8(3) . . . . ? Ru1 C3 Si2 C11 33.5(4) . . . . ? Ru3B C3 Si2 C11 -150.9(5) . . . . ? C4 C3 Si2 C10 1.8(5) . . . . ? C2 C3 Si2 C10 -178.8(4) . . . . ? Ru3A C3 Si2 C10 87.8(4) . . . . ? Ru1 C3 Si2 C10 -85.0(4) . . . . ? Ru3B C3 Si2 C10 90.6(5) . . . . ? C4 C3 Si2 C9 -118.2(5) . . . . ? C2 C3 Si2 C9 61.2(5) . . . . ? Ru3A C3 Si2 C9 -32.3(5) . . . . ? Ru1 C3 Si2 C9 155.0(4) . . . . ? Ru3B C3 Si2 C9 -29.4(6) . . . . ? data_mrvian33a _database_code_depnum_ccdc_archive 'CCDC 903656' #TrackingRef 'compound 3c.cif' _audit_creation_date 2012-12-13T13:42:57-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.4 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common 'compound 3c' _chemical_formula_moiety 'C14 H10 O9 Ru3 Si1' _chemical_formula_sum 'C23 H28 O8 Ru3 Si3' _chemical_formula_weight 819.93 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _space_group_crystal_system monoclinic _space_group_name_H-M_alt P21/m _space_group_name_Hall '-P 2yb' _space_group_IT_number 11 _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/m _symmetry_space_group_name_Hall '-P 2yb' _symmetry_Int_Tables_number 11 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' '-x, -y, -z' 'x, -y-1/2, z' _cell_length_a 11.6029(4) _cell_length_b 12.1947(5) _cell_length_c 12.0513(5) _cell_angle_alpha 90 _cell_angle_beta 103.988(2) _cell_angle_gamma 90 _cell_volume 1654.62(11) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 600 _cell_measurement_theta_min 1 _cell_measurement_theta_max 14 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.15 _exptl_crystal_density_diffrn 1.646 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 808 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.498 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.6794 _exptl_absorpt_correction_T_max 0.7253 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 9 _diffrn_orient_matrix_type 'by Bruker AXS Collect from scalepack cell' _diffrn_orient_matrix_ub_11 0.691877E-1 _diffrn_orient_matrix_ub_12 0.426063E-1 _diffrn_orient_matrix_ub_13 0.45232E-1 _diffrn_orient_matrix_ub_21 -0.297921E-1 _diffrn_orient_matrix_ub_22 0.67102E-1 _diffrn_orient_matrix_ub_23 -0.456668E-1 _diffrn_orient_matrix_ub_31 -0.470565E-1 _diffrn_orient_matrix_ub_32 0.201614E-1 _diffrn_orient_matrix_ub_33 0.56403E-1 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.0788 _diffrn_reflns_number 17656 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.259 _diffrn_reflns_theta_max 27.487 _diffrn_reflns_theta_full 25.5 _diffrn_measured_fraction_theta_full 0.994 _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_Laue_measured_fraction_full 0.994 _diffrn_reflns_Laue_measured_fraction_max 0.987 _diffrn_reflns_point_group_measured_fraction_ful 0.994 _diffrn_reflns_point_group_measured_fraction_max 0.987 _reflns_number_total 3916 _reflns_number_gt 2100 _reflns_threshold_expression 'I > 2\s(I)' _diffrn_reflns_reduction_process ; Scaled and merged with Sortav R.H. Blessing, (1987) Cryst. Rev. 1, 3-58 R.H. Blessing, (1989) J. Appl. Cryst. 22, 396-397 ; #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-2012 (Sheldrick, 2012)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_hydrogens mixed #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; ? ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; w=1/[\s^2^(Fo^2^)+(0.0849P)^2^+1.2398P] where P=(Fo^2^+2Fc^2^)/3 ; _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 3916 _refine_ls_number_parameters 204 _refine_ls_number_restraints 31 _refine_ls_R_factor_all 0.1368 _refine_ls_R_factor_gt 0.0542 _refine_ls_wR_factor_ref 0.158 _refine_ls_wR_factor_gt 0.1227 _refine_ls_goodness_of_fit_ref 0.91 _refine_ls_restrained_S_all 0.921 _refine_ls_shift/su_max 0.031 _refine_ls_shift/su_mean 0.001 _refine_diff_density_max 0.638 _refine_diff_density_min -0.523 _refine_diff_density_rms 0.088 #----------------------------------------------------------------------------# # 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' O O 0.0106 0.006 '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' Si Si 0.0817 0.0704 '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_calc_flag _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.9333(5) 0.25 0.6868(5) 0.0647(17) Uani 1 d . . C2 C 1.0411(5) 0.25 0.6504(5) 0.0643(17) Uani 1 d . . C3 C 1.1510(5) 0.25 0.7417(5) 0.0697(18) Uani 1 d . . C4 C 1.1272(5) 0.25 0.8532(5) 0.0674(18) Uani 1 d . . C5 C 1.2285(4) 0.27873(11) 0.95836(12) 0.076(3) Uani 0.5276(8) d . . C6 C 1.2698(4) 0.20628(11) 1.03847(12) 0.074(3) Uani 0.4726(8) d . . C7 C 1.3782(12) 0.3634(11) 1.2600(10) 0.298(7) Uani 1 d . . H7A H 1.3024 0.3578 1.2786 0.446 Uiso 1 calc . . H7B H 1.3831 0.4321 1.2226 0.446 Uiso 1 calc . . H7C H 1.4403 0.3593 1.3288 0.446 Uiso 1 calc . . C8 C 1.5318(14) 0.25 1.1249(13) 0.296(11) Uani 1 d . . H8A H 1.5955 0.2436 1.1923 0.444 Uiso 0.5 calc . . H8B H 1.5401 0.3172 1.0861 0.444 Uiso 0.5 calc . . H8C H 1.5343 0.1891 1.075 0.444 Uiso 0.5 calc . . C9 C 1.3919(6) 0.3682(7) 0.7718(8) 0.190(4) Uani 1 d . . H9A H 1.3515 0.4344 0.7419 0.284 Uiso 1 calc . . H9B H 1.4685 0.3663 0.7547 0.284 Uiso 1 calc . . H9C H 1.4016 0.3659 0.8532 0.284 Uiso 1 calc . . C10 C 1.2870(9) 0.25 0.5581(10) 0.211(6) Uani 1 d . . H10A H 1.3635 0.2476 0.5409 0.317 Uiso 1 calc . . H10B H 1.246 0.3155 0.5263 0.317 Uiso 0.5 calc . . H10C H 1.2415 0.187 0.5257 0.317 Uiso 0.5 calc . . C15 C 0.8132(9) 0.25 0.4312(7) 0.166(5) Uani 1 d . . H15C H 0.7389 0.25 0.3749 0.248 Uiso 1 calc . . H15A H 0.8577 0.1857 0.4217 0.248 Uiso 0.5 calc . . H15B H 0.8577 0.3143 0.4217 0.248 Uiso 0.5 calc . . C16 C 0.6949(6) 0.3714(7) 0.5976(7) 0.146(3) Uani 1 d . . H16B H 0.6199 0.3697 0.5423 0.219 Uiso 1 calc . . H16C H 0.7366 0.4374 0.588 0.219 Uiso 1 calc . . H16A H 0.6817 0.3697 0.6732 0.219 Uiso 1 calc . . C12 C 0.9757(6) 0.5099(5) 0.6553(5) 0.1127(19) Uani 1 d . . C13 C 0.9291(4) 0.4272(4) 0.8654(4) 0.0766(14) Uani 1 d . . C14 C 1.1490(5) 0.5102(5) 0.8314(5) 0.0979(17) Uani 1 d . . C21 C 0.7794(5) 0.25 0.8760(6) 0.081(2) Uani 1 d . . C22 C 0.9845(6) 0.25 1.0335(5) 0.0721(19) Uani 1 d . . O12 O 0.9405(5) 0.5781(4) 0.5909(4) 0.159(2) Uani 1 d . . O13 O 0.8807(3) 0.4928(3) 0.9040(3) 0.0995(11) Uani 1 d . . O14 O 1.2129(4) 0.5781(3) 0.8721(4) 0.1316(15) Uani 1 d . . O21 O 0.6842(4) 0.25 0.8791(5) 0.125(2) Uani 1 d . . O22 O 1.0110(5) 0.25 1.1320(4) 0.0994(17) Uani 1 d . . Ru1 Ru 1.03947(3) 0.40236(3) 0.76154(3) 0.07070(11) Uani 1 d . . Ru2 Ru 0.94363(4) 0.25 0.87174(4) 0.05989(14) Uani 1 d . . Si1 Si 0.78505(19) 0.25 0.57675(19) 0.0944(7) Uani 1 d . . Si2 Si 1.30482(16) 0.25 0.70658(19) 0.0921(7) Uani 1 d . . Si3 Si 1.39468(19) 0.25 1.1640(2) 0.0981(8) Uani 1 d . . H2 H 1.052(4) 0.25 0.567(4) 0.042(12) Uiso 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 C1 0.057(3) 0.067(4) 0.075(3) 0 0.025(3) 0 C2 0.074(3) 0.061(4) 0.064(3) 0 0.028(3) 0 C3 0.061(3) 0.072(4) 0.083(4) 0 0.031(3) 0 C4 0.054(3) 0.081(4) 0.070(3) 0 0.021(3) 0 C5 0.076(4) 0.066(9) 0.094(5) -0.009(4) 0.037(3) -0.004(4) C6 0.064(5) 0.083(7) 0.077(5) 0.022(4) 0.023(4) -0.011(4) C7 0.263(13) 0.331(16) 0.242(11) -0.066(11) -0.049(10) 0.069(11) C8 0.169(12) 0.52(3) 0.172(12) 0 -0.008(10) 0 C9 0.106(4) 0.187(8) 0.305(8) -0.030(7) 0.108(4) -0.044(5) C10 0.109(6) 0.359(18) 0.196(8) 0 0.094(5) 0 C15 0.117(7) 0.290(14) 0.074(5) 0 -0.008(5) 0 C16 0.088(4) 0.184(7) 0.155(6) 0.006(5) 0.008(4) 0.035(4) C12 0.148(4) 0.083(4) 0.126(4) 0.015(3) 0.071(3) 0.006(4) C13 0.072(2) 0.069(3) 0.097(3) -0.003(3) 0.037(2) 0.003(2) C14 0.104(3) 0.083(3) 0.123(3) -0.020(3) 0.060(2) -0.027(3) C21 0.057(3) 0.095(5) 0.099(4) 0 0.034(3) 0 C22 0.074(3) 0.071(4) 0.079(4) 0 0.034(3) 0 O12 0.230(5) 0.109(3) 0.158(3) 0.060(3) 0.083(3) 0.031(3) O13 0.115(2) 0.073(2) 0.130(2) -0.0063(19) 0.0669(17) 0.0124(19) O14 0.135(3) 0.099(3) 0.181(4) -0.039(3) 0.078(2) -0.051(2) O21 0.060(3) 0.179(6) 0.145(4) 0 0.044(3) 0 O22 0.110(3) 0.120(4) 0.079(3) 0 0.043(2) 0 Ru1 0.0747(2) 0.0614(2) 0.0862(2) 0.00016(18) 0.03926(16) -0.00471(17) Ru2 0.0516(2) 0.0623(3) 0.0720(3) 0 0.02717(19) 0 Si1 0.0667(11) 0.1283(19) 0.0854(13) 0 0.0131(10) 0 Si2 0.0630(9) 0.1197(17) 0.1069(12) 0 0.0468(8) 0 Si3 0.0673(12) 0.1285(19) 0.0920(14) 0 0.0068(11) 0 #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 C1 C2 1.422(9) . ? C1 Si1 1.901(6) . ? C1 Ru2 2.203(6) . ? C1 Ru1 2.290(3) . ? C1 Ru1 2.290(3) 4_565 ? C2 C3 1.469(8) . ? C2 Ru1 2.293(4) . ? C2 Ru1 2.293(4) 4_565 ? C2 H2 1.04(4) . ? C3 C4 1.436(9) . ? C3 Si2 1.932(6) . ? C3 Ru1 2.309(4) . ? C3 Ru1 2.309(4) 4_565 ? C4 C5 1.546(6) . ? C4 C5 1.546(6) 4_565 ? C4 Ru2 2.194(6) . ? C4 Ru1 2.273(3) . ? C4 Ru1 2.273(3) 4_565 ? C5 C5 0.701(3) 4_565 ? C5 C6 0.9857(18) 4_565 ? C5 C6 1.3110(9) . ? C6 C5 0.9857(18) 4_565 ? C6 C6 1.066(3) 4_565 ? C6 Si3 1.901(3) . ? C7 Si3 1.842(13) . ? C7 H7A 0.96 . ? C7 H7B 0.96 . ? C7 H7C 0.96 . ? C8 Si3 1.765(18) . ? C8 H8A 0.96 . ? C8 H8B 0.96 . ? C8 H8C 0.96 . ? C9 Si2 1.825(8) . ? C9 H9A 0.96 . ? C9 H9B 0.96 . ? C9 H9C 0.96 . ? C10 Si2 1.751(12) . ? C10 H10A 0.96 . ? C10 H10B 0.96 . ? C10 H10C 0.96 . ? C15 Si1 1.861(10) . ? C15 H15C 0.96 . ? C15 H15A 0.96 . ? C15 H15B 0.96 . ? C16 Si1 1.865(8) . ? C16 H16B 0.96 . ? C16 H16C 0.96 . ? C16 H16A 0.96 . ? C12 O12 1.143(7) . ? C12 Ru1 1.857(6) . ? C13 O13 1.139(6) . ? C13 Ru1 2.018(5) . ? C13 Ru2 2.167(5) . ? C14 O14 1.139(6) . ? C14 Ru1 1.881(5) . ? C21 O21 1.114(8) . ? C21 Ru2 1.919(6) . ? C22 O22 1.152(7) . ? C22 Ru2 1.892(6) . ? Ru1 Ru2 2.6769(5) . ? Ru2 C13 2.167(5) 4_565 ? Ru2 Ru1 2.6769(5) 4_565 ? Si1 C16 1.865(8) 4_565 ? Si2 C9 1.825(8) 4_565 ? Si3 C7 1.842(13) 4_565 ? Si3 C6 1.901(3) 4_565 ? 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 Si1 120.0(4) . . ? C2 C1 Ru2 118.4(4) . . ? Si1 C1 Ru2 121.6(3) . . ? C2 C1 Ru1 72.0(2) . . ? Si1 C1 Ru1 125.76(12) . . ? Ru2 C1 Ru1 73.10(15) . . ? C2 C1 Ru1 72.0(2) . 4_565 ? Si1 C1 Ru1 125.76(12) . 4_565 ? Ru2 C1 Ru1 73.10(15) . 4_565 ? Ru1 C1 Ru1 108.4(2) . 4_565 ? C1 C2 C3 116.0(5) . . ? C1 C2 Ru1 71.8(2) . . ? C3 C2 Ru1 72.0(2) . . ? C1 C2 Ru1 71.8(2) . 4_565 ? C3 C2 Ru1 72.0(2) . 4_565 ? Ru1 C2 Ru1 108.2(2) . 4_565 ? C1 C2 H2 128(2) . . ? C3 C2 H2 116(2) . . ? Ru1 C2 H2 125.7(2) . . ? Ru1 C2 H2 125.7(2) 4_565 . ? C4 C3 C2 111.9(5) . . ? C4 C3 Si2 127.0(4) . . ? C2 C3 Si2 121.1(5) . . ? C4 C3 Ru1 70.4(2) . . ? C2 C3 Ru1 70.8(2) . . ? Si2 C3 Ru1 126.39(12) . . ? C4 C3 Ru1 70.4(2) . 4_565 ? C2 C3 Ru1 70.8(2) . 4_565 ? Si2 C3 Ru1 126.39(12) . 4_565 ? Ru1 C3 Ru1 107.1(2) . 4_565 ? C3 C4 C5 119.1(5) . . ? C3 C4 C5 119.1(5) . 4_565 ? C5 C4 C5 26.19(13) . 4_565 ? C3 C4 Ru2 120.4(4) . . ? C5 C4 Ru2 118.8(4) . . ? C5 C4 Ru2 118.8(4) 4_565 . ? C3 C4 Ru1 73.1(2) . . ? C5 C4 Ru1 112.07(8) . . ? C5 C4 Ru1 138.26(16) 4_565 . ? Ru2 C4 Ru1 73.61(14) . . ? C3 C4 Ru1 73.1(2) . 4_565 ? C5 C4 Ru1 138.26(16) . 4_565 ? C5 C4 Ru1 112.07(8) 4_565 4_565 ? Ru2 C4 Ru1 73.61(14) . 4_565 ? Ru1 C4 Ru1 109.7(2) . 4_565 ? C5 C5 C6 100.69(12) 4_565 4_565 ? C5 C5 C6 47.63(10) 4_565 . ? C6 C5 C6 53.06(17) 4_565 . ? C5 C5 C4 76.90(7) 4_565 . ? C6 C5 C4 159.7(5) 4_565 . ? C6 C5 C4 121.4(2) . . ? C5 C6 C6 79.31(12) 4_565 4_565 ? C5 C6 C5 31.68(15) 4_565 . ? C6 C6 C5 47.63(10) 4_565 . ? C5 C6 Si3 145.5(3) 4_565 . ? C6 C6 Si3 73.71(5) 4_565 . ? C5 C6 Si3 118.03(19) . . ? Si3 C7 H7A 109.5 . . ? Si3 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? Si3 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? Si3 C8 H8A 109.5 . . ? Si3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? Si3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? Si2 C9 H9A 109.5 . . ? Si2 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? Si2 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? Si2 C10 H10A 109.5 . . ? Si2 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? Si2 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? Si1 C15 H15C 109.5 . . ? Si1 C15 H15A 109.5 . . ? H15C C15 H15A 109.5 . . ? Si1 C15 H15B 109.5 . . ? H15C C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? Si1 C16 H16B 109.5 . . ? Si1 C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? Si1 C16 H16A 109.5 . . ? H16B C16 H16A 109.5 . . ? H16C C16 H16A 109.5 . . ? O12 C12 Ru1 177.4(6) . . ? O13 C13 Ru1 143.9(4) . . ? O13 C13 Ru2 136.7(4) . . ? Ru1 C13 Ru2 79.43(18) . . ? O14 C14 Ru1 177.8(5) . . ? O21 C21 Ru2 179.6(6) . . ? O22 C22 Ru2 179.1(6) . . ? C12 Ru1 C14 85.9(3) . . ? C12 Ru1 C13 96.6(2) . . ? C14 Ru1 C13 94.5(2) . . ? C12 Ru1 C4 165.8(2) . . ? C14 Ru1 C4 100.3(2) . . ? C13 Ru1 C4 95.6(2) . . ? C12 Ru1 C1 102.4(2) . . ? C14 Ru1 C1 169.9(2) . . ? C13 Ru1 C1 90.2(2) . . ? C4 Ru1 C1 70.32(16) . . ? C12 Ru1 C2 103.1(2) . . ? C14 Ru1 C2 136.7(2) . . ? C13 Ru1 C2 125.4(2) . . ? C4 Ru1 C2 63.62(18) . . ? C1 Ru1 C2 36.1(2) . . ? C12 Ru1 C3 129.5(3) . . ? C14 Ru1 C3 105.9(2) . . ? C13 Ru1 C3 129.8(2) . . ? C4 Ru1 C3 36.5(2) . . ? C1 Ru1 C3 64.41(18) . . ? C2 Ru1 C3 37.23(19) . . ? C12 Ru1 Ru2 133.5(2) . . ? C14 Ru1 Ru2 125.47(17) . . ? C13 Ru1 Ru2 52.74(15) . . ? C4 Ru1 Ru2 51.86(15) . . ? C1 Ru1 Ru2 51.95(15) . . ? C2 Ru1 Ru2 77.90(13) . . ? C3 Ru1 Ru2 78.66(13) . . ? C22 Ru2 C21 88.6(3) . . ? C22 Ru2 C13 91.96(13) . 4_565 ? C21 Ru2 C13 86.09(13) . 4_565 ? C22 Ru2 C13 91.96(13) . . ? C21 Ru2 C13 86.09(12) . . ? C13 Ru2 C13 171.2(2) 4_565 . ? C22 Ru2 C4 95.6(2) . . ? C21 Ru2 C4 175.8(3) . . ? C13 Ru2 C4 93.75(13) 4_565 . ? C13 Ru2 C4 93.75(13) . . ? C22 Ru2 C1 168.9(2) . . ? C21 Ru2 C1 102.5(3) . . ? C13 Ru2 C1 88.83(13) 4_565 . ? C13 Ru2 C1 88.84(13) . . ? C4 Ru2 C1 73.4(2) . . ? C22 Ru2 Ru1 118.72(12) . . ? C21 Ru2 Ru1 123.21(12) . . ? C13 Ru2 Ru1 135.45(13) 4_565 . ? C13 Ru2 Ru1 47.82(13) . . ? C4 Ru2 Ru1 54.54(8) . . ? C1 Ru2 Ru1 54.95(8) . . ? C22 Ru2 Ru1 118.72(12) . 4_565 ? C21 Ru2 Ru1 123.21(12) . 4_565 ? C13 Ru2 Ru1 47.82(13) 4_565 4_565 ? C13 Ru2 Ru1 135.45(13) . 4_565 ? C4 Ru2 Ru1 54.54(8) . 4_565 ? C1 Ru2 Ru1 54.94(8) . 4_565 ? Ru1 Ru2 Ru1 87.91(2) . 4_565 ? C15 Si1 C16 111.1(3) . 4_565 ? C15 Si1 C16 111.1(3) . . ? C16 Si1 C16 105.1(5) 4_565 . ? C15 Si1 C1 108.8(4) . . ? C16 Si1 C1 110.4(2) 4_565 . ? C16 Si1 C1 110.4(2) . . ? C10 Si2 C9 110.9(4) . . ? C10 Si2 C9 110.9(4) . 4_565 ? C9 Si2 C9 104.3(5) . 4_565 ? C10 Si2 C3 109.7(4) . . ? C9 Si2 C3 110.5(3) . . ? C9 Si2 C3 110.5(3) 4_565 . ? C8 Si3 C7 113.9(5) . 4_565 ? C8 Si3 C7 113.9(5) . . ? C7 Si3 C7 97.3(9) 4_565 . ? C8 Si3 C6 110.5(5) . . ? C7 Si3 C6 96.6(4) 4_565 . ? C7 Si3 C6 122.4(4) . . ? C8 Si3 C6 110.5(5) . 4_565 ? C7 Si3 C6 122.4(4) 4_565 4_565 ? C7 Si3 C6 96.6(4) . 4_565 ? C6 Si3 C6 32.58(9) . 4_565 ? data_mrvian35 _database_code_depnum_ccdc_archive 'CCDC 903657' #TrackingRef 'compound 7.cif' _audit_creation_date 2012-02-07T13:21:19-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.4 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common 'compound 7' _chemical_formula_moiety 'C38 H43 O10 Ru3 Si3' _chemical_formula_sum 'C63 H48 O3 Ru Si3' _chemical_formula_weight 1038.35 _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 11.2271(3) _cell_length_b 13.7405(4) _cell_length_c 19.1205(3) _cell_angle_alpha 83.763(2) _cell_angle_beta 77.420(2) _cell_angle_gamma 67.1720(10) _cell_volume 2652.39(11) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 600 _cell_measurement_theta_min 1 _cell_measurement_theta_max 14 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.03 _exptl_crystal_density_diffrn 1.3 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1072 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.409 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.9239 _exptl_absorpt_correction_T_max 0.9851 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 9 _diffrn_orient_matrix_type 'by Bruker AXS Collect from scalepack cell' _diffrn_orient_matrix_ub_11 -0.45141E-1 _diffrn_orient_matrix_ub_12 0.698755E-1 _diffrn_orient_matrix_ub_13 0.236436E-1 _diffrn_orient_matrix_ub_21 0.827318E-1 _diffrn_orient_matrix_ub_22 -0.94492E-2 _diffrn_orient_matrix_ub_23 0.162758E-1 _diffrn_orient_matrix_ub_31 0.285195E-1 _diffrn_orient_matrix_ub_32 0.356048E-1 _diffrn_orient_matrix_ub_33 -0.45273E-1 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.063 _diffrn_reflns_av_unetI/netI 0.0838 _diffrn_reflns_number 37351 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.11 _diffrn_reflns_theta_max 27.58 _diffrn_reflns_theta_full 27.58 _diffrn_measured_fraction_theta_full 0.976 _diffrn_measured_fraction_theta_max 0.976 _reflns_number_total 11980 _reflns_number_gt 7310 _reflns_threshold_expression >2\s(I) _diffrn_reflns_reduction_process ; Scaled and merged with Sortav R.H. Blessing, (1987) Cryst. Rev. 1, 3-58 R.H. Blessing, (1989) J. Appl. Cryst. 22, 396-397 ; #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _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^)+(0.0472P)^2^+0.3408P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 11980 _refine_ls_number_parameters 632 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1065 _refine_ls_R_factor_gt 0.0473 _refine_ls_wR_factor_ref 0.114 _refine_ls_wR_factor_gt 0.0958 _refine_ls_goodness_of_fit_ref 1.017 _refine_ls_restrained_S_all 1.017 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.504 _refine_diff_density_min -0.392 _refine_diff_density_rms 0.059 #----------------------------------------------------------------------------# # 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' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 0.3454(3) -0.0168(2) 0.23280(14) 0.0415(6) Uani 1 1 d . . . C2 C 0.3844(3) -0.0693(2) 0.16523(14) 0.0422(7) Uani 1 1 d . . . H2 H 0.4252 -0.1459 0.1593 0.051 Uiso 1 1 calc R . . C3 C 0.3645(3) 0.0062(2) 0.10942(14) 0.0434(7) Uani 1 1 d . . . H3 H 0.3895 -0.0095 0.0583 0.052 Uiso 1 1 calc R . . C4 C 0.3130(3) 0.1111(2) 0.13821(14) 0.0415(6) Uani 1 1 d . . . C5 C 0.3082(3) 0.0930(2) 0.21323(14) 0.0431(7) Uani 1 1 d . . . C6 C 0.0084(3) 0.1249(2) 0.23869(15) 0.0513(7) Uani 1 1 d . . . C7 C -0.0907(3) 0.1900(3) 0.27220(17) 0.0574(8) Uani 1 1 d . . . C11 C 0.1231(3) -0.0891(3) 0.20274(19) 0.0652(9) Uani 1 1 d . . . C12 C 0.0762(3) 0.0630(3) 0.10282(18) 0.0611(9) Uani 1 1 d . . . C111 C 0.5588(3) -0.1159(3) 0.31728(14) 0.0544(8) Uani 1 1 d . . . C112 C 0.6111(4) -0.0388(4) 0.29651(18) 0.0768(11) Uani 1 1 d . . . H112 H 0.5564 0.0291 0.2851 0.092 Uiso 1 1 calc R . . C113 C 0.7456(5) -0.0617(5) 0.2924(2) 0.1007(16) Uani 1 1 d . . . H113 H 0.7798 -0.0093 0.2782 0.121 Uiso 1 1 calc R . . C114 C 0.8259(5) -0.1611(6) 0.3093(2) 0.112(2) Uani 1 1 d . . . H114 H 0.915 -0.1764 0.3067 0.134 Uiso 1 1 calc R . . C115 C 0.7771(5) -0.2374(5) 0.3298(3) 0.1045(17) Uani 1 1 d . . . H115 H 0.8326 -0.3049 0.3414 0.125 Uiso 1 1 calc R . . C116 C 0.6456(4) -0.2159(3) 0.33382(19) 0.0775(11) Uani 1 1 d . . . H116 H 0.6138 -0.2696 0.3479 0.093 Uiso 1 1 calc R . . C121 C 0.3478(3) -0.2093(2) 0.33201(16) 0.0538(8) Uani 1 1 d . . . C122 C 0.4164(4) -0.2932(3) 0.28598(18) 0.0666(9) Uani 1 1 d . . . H122 H 0.4793 -0.2866 0.2471 0.08 Uiso 1 1 calc R . . C123 C 0.3937(4) -0.3855(3) 0.2965(2) 0.0820(12) Uani 1 1 d . . . H123 H 0.442 -0.441 0.2654 0.098 Uiso 1 1 calc R . . C124 C 0.3004(5) -0.3957(3) 0.3526(3) 0.1056(16) Uani 1 1 d . . . H124 H 0.2836 -0.4576 0.3592 0.127 Uiso 1 1 calc R . . C125 C 0.2325(5) -0.3160(3) 0.3983(3) 0.1178(19) Uani 1 1 d . . . H125 H 0.17 -0.3236 0.4371 0.141 Uiso 1 1 calc R . . C126 C 0.2550(4) -0.2234(3) 0.3880(2) 0.0886(13) Uani 1 1 d . . . H126 H 0.2062 -0.1689 0.4198 0.106 Uiso 1 1 calc R . . C131 C 0.2769(3) 0.0038(2) 0.39697(14) 0.0488(7) Uani 1 1 d . . . C132 C 0.1437(4) 0.0579(3) 0.40148(17) 0.0664(10) Uani 1 1 d . . . H132 H 0.105 0.0561 0.3636 0.08 Uiso 1 1 calc R . . C133 C 0.0658(4) 0.1153(3) 0.46170(18) 0.0789(12) Uani 1 1 d . . . H133 H -0.0242 0.1515 0.4642 0.095 Uiso 1 1 calc R . . C134 C 0.1237(5) 0.1173(3) 0.51686(19) 0.0878(13) Uani 1 1 d . . . H134 H 0.0722 0.1549 0.5575 0.105 Uiso 1 1 calc R . . C135 C 0.2545(4) 0.0658(4) 0.51369(19) 0.0904(13) Uani 1 1 d . . . H135 H 0.2922 0.0685 0.5519 0.108 Uiso 1 1 calc R . . C136 C 0.3322(4) 0.0093(3) 0.45394(16) 0.0694(10) Uani 1 1 d . . . H136 H 0.4224 -0.0254 0.4518 0.083 Uiso 1 1 calc R . . C211 C 0.4874(3) 0.2031(2) 0.04124(15) 0.0466(7) Uani 1 1 d . . . C212 C 0.5863(3) 0.1384(3) 0.07704(18) 0.0602(8) Uani 1 1 d . . . H212 H 0.5642 0.1045 0.1198 0.072 Uiso 1 1 calc R . . C213 C 0.7171(3) 0.1230(3) 0.0505(2) 0.0720(10) Uani 1 1 d . . . H213 H 0.7816 0.0784 0.0752 0.086 Uiso 1 1 calc R . . C214 C 0.7517(3) 0.1728(3) -0.0115(2) 0.0663(9) Uani 1 1 d . . . H214 H 0.8396 0.1629 -0.0289 0.08 Uiso 1 1 calc R . . C215 C 0.6573(3) 0.2371(3) -0.04799(18) 0.0626(9) Uani 1 1 d . . . H215 H 0.6808 0.2714 -0.0902 0.075 Uiso 1 1 calc R . . C216 C 0.5269(3) 0.2517(2) -0.02275(16) 0.0530(8) Uani 1 1 d . . . H216 H 0.4638 0.2948 -0.0488 0.064 Uiso 1 1 calc R . . C221 C 0.2188(3) 0.2426(2) 0.00626(14) 0.0441(7) Uani 1 1 d . . . C222 C 0.2760(3) 0.1719(3) -0.04971(15) 0.0574(8) Uani 1 1 d . . . H222 H 0.3592 0.1198 -0.0498 0.069 Uiso 1 1 calc R . . C223 C 0.2123(4) 0.1773(3) -0.10494(17) 0.0674(10) Uani 1 1 d . . . H223 H 0.2525 0.1291 -0.1416 0.081 Uiso 1 1 calc R . . C224 C 0.0895(4) 0.2537(3) -0.10571(19) 0.0745(11) Uani 1 1 d . . . H224 H 0.0458 0.2571 -0.1426 0.089 Uiso 1 1 calc R . . C225 C 0.0318(4) 0.3248(3) -0.05187(19) 0.0767(11) Uani 1 1 d . . . H225 H -0.0508 0.3773 -0.0525 0.092 Uiso 1 1 calc R . . C226 C 0.0957(3) 0.3189(3) 0.00344(17) 0.0612(9) Uani 1 1 d . . . H226 H 0.0548 0.3676 0.0398 0.073 Uiso 1 1 calc R . . C231 C 0.2404(3) 0.3542(2) 0.13341(15) 0.0476(7) Uani 1 1 d . . . C232 C 0.3138(4) 0.4160(3) 0.12943(17) 0.0625(9) Uani 1 1 d . . . H232 H 0.3972 0.3956 0.1005 0.075 Uiso 1 1 calc R . . C233 C 0.2655(5) 0.5081(3) 0.1677(2) 0.0818(12) Uani 1 1 d . . . H233 H 0.3167 0.5485 0.1645 0.098 Uiso 1 1 calc R . . C234 C 0.1432(5) 0.5394(3) 0.2101(2) 0.0825(13) Uani 1 1 d . . . H234 H 0.1113 0.6008 0.2361 0.099 Uiso 1 1 calc R . . C235 C 0.0674(4) 0.4805(3) 0.2144(2) 0.0773(11) Uani 1 1 d . . . H235 H -0.0165 0.5023 0.2428 0.093 Uiso 1 1 calc R . . C236 C 0.1158(3) 0.3884(3) 0.17633(17) 0.0628(9) Uani 1 1 d . . . H236 H 0.0638 0.3487 0.1796 0.075 Uiso 1 1 calc R . . C311 C -0.2063(4) 0.3841(3) 0.36356(16) 0.0594(8) Uani 1 1 d . . . C312 C -0.3118(5) 0.4622(3) 0.4038(2) 0.0838(12) Uani 1 1 d . . . H312 H -0.3973 0.4733 0.3999 0.101 Uiso 1 1 calc R . . C313 C -0.2917(6) 0.5240(4) 0.4497(2) 0.1069(17) Uani 1 1 d . . . H313 H -0.3629 0.5766 0.4757 0.128 Uiso 1 1 calc R . . C314 C -0.1672(8) 0.5068(5) 0.4561(3) 0.119(2) Uani 1 1 d . . . H314 H -0.1537 0.5471 0.4875 0.143 Uiso 1 1 calc R . . C315 C -0.0626(6) 0.4324(5) 0.4178(3) 0.1131(17) Uani 1 1 d . . . H315 H 0.0223 0.4226 0.422 0.136 Uiso 1 1 calc R . . C316 C -0.0822(4) 0.3709(3) 0.3723(2) 0.0819(11) Uani 1 1 d . . . H316 H -0.0095 0.3189 0.3467 0.098 Uiso 1 1 calc R . . C321 C -0.3885(3) 0.2837(2) 0.33531(16) 0.0550(8) Uani 1 1 d . . . C322 C -0.4064(4) 0.2351(3) 0.4017(2) 0.0860(12) Uani 1 1 d . . . H322 H -0.338 0.2097 0.4271 0.103 Uiso 1 1 calc R . . C323 C -0.5248(5) 0.2234(4) 0.4312(2) 0.1012(15) Uani 1 1 d . . . H323 H -0.5345 0.1905 0.4761 0.121 Uiso 1 1 calc R . . C324 C -0.6263(4) 0.2593(3) 0.3955(3) 0.0888(12) Uani 1 1 d . . . H324 H -0.7049 0.2508 0.4157 0.107 Uiso 1 1 calc R . . C325 C -0.6127(4) 0.3074(3) 0.3308(3) 0.0794(11) Uani 1 1 d . . . H325 H -0.6822 0.3327 0.3062 0.095 Uiso 1 1 calc R . . C326 C -0.4955(4) 0.3191(3) 0.3011(2) 0.0656(9) Uani 1 1 d . . . H326 H -0.4878 0.3522 0.2562 0.079 Uiso 1 1 calc R . . C331 C -0.2564(3) 0.3901(2) 0.21200(16) 0.0542(8) Uani 1 1 d . . . C332 C -0.2598(4) 0.3453(3) 0.15150(18) 0.0770(11) Uani 1 1 d . . . H332 H -0.2544 0.2758 0.1543 0.092 Uiso 1 1 calc R . . C333 C -0.2710(5) 0.4005(3) 0.0873(2) 0.0898(13) Uani 1 1 d . . . H333 H -0.2759 0.3686 0.0481 0.108 Uiso 1 1 calc R . . C334 C -0.2749(4) 0.5012(3) 0.0806(2) 0.0856(13) Uani 1 1 d . . . H334 H -0.2796 0.5376 0.0368 0.103 Uiso 1 1 calc R . . C335 C -0.2718(4) 0.5480(3) 0.1391(2) 0.0792(11) Uani 1 1 d . . . H335 H -0.275 0.617 0.1351 0.095 Uiso 1 1 calc R . . C336 C -0.2639(3) 0.4935(3) 0.20483(18) 0.0622(9) Uani 1 1 d . . . H336 H -0.2636 0.5271 0.2445 0.075 Uiso 1 1 calc R . . O6 O 0.2741(2) 0.17089(15) 0.25931(10) 0.0587(6) Uani 1 1 d . . . H6 H 0.2605 0.1481 0.3005 0.088 Uiso 1 1 calc R . . O11 O 0.1016(3) -0.1654(2) 0.21569(18) 0.1061(10) Uani 1 1 d . . . O12 O 0.0196(3) 0.0857(2) 0.05691(15) 0.0917(9) Uani 1 1 d . . . Si1 Si 0.38053(8) -0.08476(6) 0.32073(4) 0.0463(2) Uani 1 1 d . . . Si2 Si 0.30893(8) 0.23117(6) 0.08022(4) 0.04300(19) Uani 1 1 d . . . Si3 Si -0.23413(9) 0.30907(7) 0.29718(4) 0.0521(2) Uani 1 1 d . . . Ru1 Ru 0.17216(2) 0.025717(19) 0.176735(12) 0.04409(9) 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 C1 0.0417(17) 0.0430(16) 0.0388(14) -0.0039(12) -0.0062(12) -0.0150(13) C2 0.0370(16) 0.0399(16) 0.0448(15) -0.0060(12) -0.0060(12) -0.0087(13) C3 0.0374(16) 0.0514(17) 0.0394(15) -0.0063(13) -0.0034(12) -0.0153(14) C4 0.0381(16) 0.0471(17) 0.0408(15) -0.0025(12) -0.0113(12) -0.0154(13) C5 0.0444(17) 0.0446(17) 0.0425(15) -0.0071(12) -0.0088(13) -0.0174(14) C6 0.0446(19) 0.0519(18) 0.0529(17) -0.0004(14) -0.0106(14) -0.0131(16) C7 0.048(2) 0.056(2) 0.0585(19) -0.0024(15) -0.0114(16) -0.0092(17) C11 0.048(2) 0.063(2) 0.084(2) -0.0075(18) 0.0004(17) -0.0260(18) C12 0.047(2) 0.076(2) 0.066(2) -0.0060(17) -0.0161(17) -0.0247(18) C111 0.052(2) 0.072(2) 0.0357(15) -0.0071(14) -0.0062(13) -0.0192(18) C112 0.073(3) 0.107(3) 0.055(2) -0.001(2) -0.0138(18) -0.039(2) C113 0.091(4) 0.180(5) 0.053(2) -0.005(3) -0.005(2) -0.079(4) C114 0.060(3) 0.209(7) 0.058(3) -0.023(3) -0.005(2) -0.040(4) C115 0.057(3) 0.139(5) 0.088(3) -0.020(3) -0.020(2) 0.003(3) C116 0.056(2) 0.086(3) 0.074(2) -0.012(2) -0.0206(19) -0.002(2) C121 0.056(2) 0.0444(18) 0.0534(18) 0.0008(14) -0.0109(15) -0.0115(15) C122 0.078(3) 0.051(2) 0.062(2) -0.0047(16) -0.0122(18) -0.0156(18) C123 0.091(3) 0.050(2) 0.099(3) -0.014(2) -0.022(2) -0.015(2) C124 0.098(4) 0.053(3) 0.164(5) -0.007(3) -0.002(3) -0.037(3) C125 0.108(4) 0.063(3) 0.154(4) -0.004(3) 0.043(3) -0.037(3) C126 0.090(3) 0.054(2) 0.098(3) -0.003(2) 0.026(2) -0.024(2) C131 0.057(2) 0.0465(17) 0.0399(15) 0.0004(12) -0.0065(14) -0.0178(16) C132 0.064(2) 0.074(2) 0.0483(18) -0.0069(16) -0.0136(16) -0.0089(19) C133 0.061(2) 0.086(3) 0.059(2) -0.0101(19) -0.0009(18) 0.001(2) C134 0.093(3) 0.100(3) 0.048(2) -0.0232(19) 0.005(2) -0.016(3) C135 0.081(3) 0.123(4) 0.056(2) -0.031(2) -0.007(2) -0.022(3) C136 0.066(2) 0.086(3) 0.0509(19) -0.0112(17) -0.0111(17) -0.020(2) C211 0.0444(17) 0.0462(17) 0.0520(17) -0.0046(13) -0.0131(14) -0.0171(14) C212 0.052(2) 0.071(2) 0.066(2) 0.0083(17) -0.0208(16) -0.0289(18) C213 0.045(2) 0.080(3) 0.094(3) 0.005(2) -0.0271(19) -0.0213(19) C214 0.047(2) 0.073(2) 0.086(3) -0.012(2) -0.0049(18) -0.0317(19) C215 0.062(2) 0.067(2) 0.061(2) -0.0059(17) 0.0036(17) -0.0331(19) C216 0.050(2) 0.0533(19) 0.0544(18) -0.0008(14) -0.0079(15) -0.0199(16) C221 0.0414(17) 0.0448(17) 0.0451(16) 0.0046(13) -0.0123(13) -0.0146(14) C222 0.059(2) 0.062(2) 0.0482(18) -0.0016(15) -0.0163(15) -0.0163(17) C223 0.084(3) 0.069(2) 0.0520(19) -0.0083(16) -0.0215(18) -0.025(2) C224 0.080(3) 0.089(3) 0.060(2) 0.003(2) -0.032(2) -0.029(2) C225 0.057(2) 0.090(3) 0.071(2) 0.001(2) -0.0289(19) -0.007(2) C226 0.055(2) 0.068(2) 0.0534(18) -0.0058(16) -0.0143(15) -0.0124(18) C231 0.056(2) 0.0432(17) 0.0448(16) 0.0044(13) -0.0182(14) -0.0162(15) C232 0.073(2) 0.062(2) 0.060(2) -0.0035(16) -0.0136(17) -0.0321(19) C233 0.118(4) 0.064(2) 0.082(3) -0.004(2) -0.030(3) -0.048(3) C234 0.113(4) 0.054(2) 0.072(2) -0.0171(18) -0.033(2) -0.009(2) C235 0.074(3) 0.064(2) 0.077(2) -0.0173(19) -0.014(2) -0.004(2) C236 0.058(2) 0.057(2) 0.069(2) -0.0076(17) -0.0132(17) -0.0142(17) C311 0.065(2) 0.055(2) 0.0515(18) -0.0020(15) -0.0116(16) -0.0148(17) C312 0.097(3) 0.077(3) 0.074(2) -0.017(2) -0.021(2) -0.023(2) C313 0.151(5) 0.081(3) 0.083(3) -0.025(2) -0.025(3) -0.029(3) C314 0.190(7) 0.115(4) 0.091(4) -0.014(3) -0.050(4) -0.082(5) C315 0.136(5) 0.141(5) 0.102(4) 0.001(3) -0.054(3) -0.079(4) C316 0.082(3) 0.091(3) 0.076(3) -0.003(2) -0.024(2) -0.032(2) C321 0.055(2) 0.0423(17) 0.0578(19) -0.0052(14) -0.0069(15) -0.0085(15) C322 0.076(3) 0.100(3) 0.078(3) 0.019(2) -0.019(2) -0.032(2) C323 0.097(4) 0.116(4) 0.081(3) 0.021(3) 0.003(3) -0.048(3) C324 0.065(3) 0.074(3) 0.123(4) -0.009(3) -0.004(3) -0.027(2) C325 0.066(3) 0.059(2) 0.118(3) -0.004(2) -0.024(2) -0.025(2) C326 0.062(2) 0.055(2) 0.080(2) -0.0004(17) -0.0176(19) -0.0194(18) C331 0.0489(19) 0.0475(19) 0.0554(18) -0.0083(14) -0.0043(14) -0.0077(15) C332 0.110(3) 0.055(2) 0.061(2) -0.0049(17) -0.019(2) -0.024(2) C333 0.125(4) 0.080(3) 0.058(2) -0.009(2) -0.025(2) -0.025(3) C334 0.101(3) 0.071(3) 0.062(2) 0.006(2) -0.015(2) -0.010(2) C335 0.089(3) 0.056(2) 0.085(3) 0.009(2) -0.014(2) -0.023(2) C336 0.061(2) 0.056(2) 0.067(2) -0.0033(16) -0.0160(17) -0.0174(17) O6 0.0891(17) 0.0496(13) 0.0426(11) -0.0066(9) -0.0171(11) -0.0279(12) O11 0.095(2) 0.090(2) 0.146(3) 0.0051(19) -0.0019(19) -0.0621(19) O12 0.0697(18) 0.128(2) 0.0905(19) 0.0019(17) -0.0423(15) -0.0380(17) Si1 0.0494(5) 0.0450(5) 0.0387(4) -0.0022(3) -0.0075(4) -0.0117(4) Si2 0.0417(5) 0.0436(5) 0.0436(4) 0.0006(3) -0.0109(3) -0.0149(4) Si3 0.0478(5) 0.0467(5) 0.0518(5) -0.0057(4) -0.0067(4) -0.0075(4) Ru1 0.03772(14) 0.04592(15) 0.04733(15) -0.00636(10) -0.00629(10) -0.01398(11) #----------------------------------------------------------------------------# # 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 C5 1.431(4) . ? C1 C2 1.447(4) . ? C1 Si1 1.875(3) . ? C1 Ru1 2.272(3) . ? C2 C3 1.396(4) . ? C2 Ru1 2.203(3) . ? C2 H2 0.98 . ? C3 C4 1.451(4) . ? C3 Ru1 2.192(3) . ? C3 H3 0.98 . ? C4 C5 1.422(4) . ? C4 Si2 1.875(3) . ? C4 Ru1 2.273(3) . ? C5 O6 1.344(3) . ? C5 Ru1 2.319(3) . ? C6 C7 1.221(4) . ? C6 Ru1 2.024(3) . ? C7 Si3 1.814(3) . ? C11 O11 1.154(4) . ? C11 Ru1 1.851(4) . ? C12 O12 1.140(4) . ? C12 Ru1 1.871(3) . ? C111 C112 1.383(5) . ? C111 C116 1.392(5) . ? C111 Si1 1.865(3) . ? C112 C113 1.404(6) . ? C112 H112 0.93 . ? C113 C114 1.363(7) . ? C113 H113 0.93 . ? C114 C115 1.347(7) . ? C114 H114 0.93 . ? C115 C116 1.374(6) . ? C115 H115 0.93 . ? C116 H116 0.93 . ? C121 C126 1.377(5) . ? C121 C122 1.390(4) . ? C121 Si1 1.866(3) . ? C122 C123 1.374(5) . ? C122 H122 0.93 . ? C123 C124 1.363(6) . ? C123 H123 0.93 . ? C124 C125 1.348(6) . ? C124 H124 0.93 . ? C125 C126 1.377(5) . ? C125 H125 0.93 . ? C126 H126 0.93 . ? C131 C132 1.375(5) . ? C131 C136 1.388(4) . ? C131 Si1 1.873(3) . ? C132 C133 1.391(4) . ? C132 H132 0.93 . ? C133 C134 1.362(5) . ? C133 H133 0.93 . ? C134 C135 1.351(6) . ? C134 H134 0.93 . ? C135 C136 1.379(5) . ? C135 H135 0.93 . ? C136 H136 0.93 . ? C211 C212 1.388(4) . ? C211 C216 1.398(4) . ? C211 Si2 1.879(3) . ? C212 C213 1.384(5) . ? C212 H212 0.93 . ? C213 C214 1.363(5) . ? C213 H213 0.93 . ? C214 C215 1.361(5) . ? C214 H214 0.93 . ? C215 C216 1.379(4) . ? C215 H215 0.93 . ? C216 H216 0.93 . ? C221 C226 1.381(4) . ? C221 C222 1.394(4) . ? C221 Si2 1.871(3) . ? C222 C223 1.380(4) . ? C222 H222 0.93 . ? C223 C224 1.374(5) . ? C223 H223 0.93 . ? C224 C225 1.368(5) . ? C224 H224 0.93 . ? C225 C226 1.381(5) . ? C225 H225 0.93 . ? C226 H226 0.93 . ? C231 C232 1.382(4) . ? C231 C236 1.387(4) . ? C231 Si2 1.873(3) . ? C232 C233 1.389(5) . ? C232 H232 0.93 . ? C233 C234 1.363(6) . ? C233 H233 0.93 . ? C234 C235 1.371(6) . ? C234 H234 0.93 . ? C235 C236 1.386(5) . ? C235 H235 0.93 . ? C236 H236 0.93 . ? C311 C316 1.379(5) . ? C311 C312 1.393(5) . ? C311 Si3 1.865(3) . ? C312 C313 1.392(6) . ? C312 H312 0.93 . ? C313 C314 1.355(7) . ? C313 H313 0.93 . ? C314 C315 1.348(7) . ? C314 H314 0.93 . ? C315 C316 1.381(6) . ? C315 H315 0.93 . ? C316 H316 0.93 . ? C321 C322 1.381(5) . ? C321 C326 1.388(5) . ? C321 Si3 1.876(3) . ? C322 C323 1.389(6) . ? C322 H322 0.93 . ? C323 C324 1.355(6) . ? C323 H323 0.93 . ? C324 C325 1.345(6) . ? C324 H324 0.93 . ? C325 C326 1.378(5) . ? C325 H325 0.93 . ? C326 H326 0.93 . ? C331 C332 1.383(4) . ? C331 C336 1.383(4) . ? C331 Si3 1.877(3) . ? C332 C333 1.373(5) . ? C332 H332 0.93 . ? C333 C334 1.361(5) . ? C333 H333 0.93 . ? C334 C335 1.362(5) . ? C334 H334 0.93 . ? C335 C336 1.393(5) . ? C335 H335 0.93 . ? C336 H336 0.93 . ? O6 H6 0.82 . ? 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 C5 C1 C2 104.4(2) . . ? C5 C1 Si1 129.1(2) . . ? C2 C1 Si1 124.7(2) . . ? C5 C1 Ru1 73.61(16) . . ? C2 C1 Ru1 68.56(15) . . ? Si1 C1 Ru1 133.08(14) . . ? C3 C2 C1 109.4(2) . . ? C3 C2 Ru1 71.08(16) . . ? C1 C2 Ru1 73.76(16) . . ? C3 C2 H2 125.2 . . ? C1 C2 H2 125.2 . . ? Ru1 C2 H2 125.2 . . ? C2 C3 C4 109.7(2) . . ? C2 C3 Ru1 71.89(16) . . ? C4 C3 Ru1 74.09(15) . . ? C2 C3 H3 125 . . ? C4 C3 H3 125 . . ? Ru1 C3 H3 125 . . ? C5 C4 C3 104.3(2) . . ? C5 C4 Si2 130.8(2) . . ? C3 C4 Si2 122.41(19) . . ? C5 C4 Ru1 73.71(16) . . ? C3 C4 Ru1 68.05(15) . . ? Si2 C4 Ru1 135.16(14) . . ? O6 C5 C4 123.2(2) . . ? O6 C5 C1 124.8(2) . . ? C4 C5 C1 112.0(2) . . ? O6 C5 Ru1 128.0(2) . . ? C4 C5 Ru1 70.23(16) . . ? C1 C5 Ru1 70.08(16) . . ? C7 C6 Ru1 175.4(3) . . ? C6 C7 Si3 162.9(3) . . ? O11 C11 Ru1 174.7(3) . . ? O12 C12 Ru1 178.8(3) . . ? C112 C111 C116 116.8(4) . . ? C112 C111 Si1 120.3(3) . . ? C116 C111 Si1 122.8(3) . . ? C111 C112 C113 120.9(4) . . ? C111 C112 H112 119.6 . . ? C113 C112 H112 119.6 . . ? C114 C113 C112 119.6(5) . . ? C114 C113 H113 120.2 . . ? C112 C113 H113 120.2 . . ? C115 C114 C113 120.5(5) . . ? C115 C114 H114 119.7 . . ? C113 C114 H114 119.7 . . ? C114 C115 C116 120.3(5) . . ? C114 C115 H115 119.9 . . ? C116 C115 H115 119.9 . . ? C115 C116 C111 121.8(5) . . ? C115 C116 H116 119.1 . . ? C111 C116 H116 119.1 . . ? C126 C121 C122 116.3(3) . . ? C126 C121 Si1 121.1(3) . . ? C122 C121 Si1 122.5(3) . . ? C123 C122 C121 121.7(4) . . ? C123 C122 H122 119.2 . . ? C121 C122 H122 119.2 . . ? C124 C123 C122 119.8(4) . . ? C124 C123 H123 120.1 . . ? C122 C123 H123 120.1 . . ? C125 C124 C123 120.0(4) . . ? C125 C124 H124 120 . . ? C123 C124 H124 120 . . ? C124 C125 C126 120.4(4) . . ? C124 C125 H125 119.8 . . ? C126 C125 H125 119.8 . . ? C125 C126 C121 121.8(4) . . ? C125 C126 H126 119.1 . . ? C121 C126 H126 119.1 . . ? C132 C131 C136 118.1(3) . . ? C132 C131 Si1 121.9(2) . . ? C136 C131 Si1 119.8(3) . . ? C131 C132 C133 121.2(3) . . ? C131 C132 H132 119.4 . . ? C133 C132 H132 119.4 . . ? C134 C133 C132 118.8(4) . . ? C134 C133 H133 120.6 . . ? C132 C133 H133 120.6 . . ? C135 C134 C133 121.3(3) . . ? C135 C134 H134 119.3 . . ? C133 C134 H134 119.3 . . ? C134 C135 C136 120.1(4) . . ? C134 C135 H135 120 . . ? C136 C135 H135 120 . . ? C135 C136 C131 120.5(4) . . ? C135 C136 H136 119.8 . . ? C131 C136 H136 119.8 . . ? C212 C211 C216 116.5(3) . . ? C212 C211 Si2 121.5(2) . . ? C216 C211 Si2 121.9(2) . . ? C213 C212 C211 121.5(3) . . ? C213 C212 H212 119.2 . . ? C211 C212 H212 119.2 . . ? C214 C213 C212 120.3(3) . . ? C214 C213 H213 119.8 . . ? C212 C213 H213 119.8 . . ? C215 C214 C213 119.8(3) . . ? C215 C214 H214 120.1 . . ? C213 C214 H214 120.1 . . ? C214 C215 C216 120.5(3) . . ? C214 C215 H215 119.8 . . ? C216 C215 H215 119.8 . . ? C215 C216 C211 121.4(3) . . ? C215 C216 H216 119.3 . . ? C211 C216 H216 119.3 . . ? C226 C221 C222 116.8(3) . . ? C226 C221 Si2 123.3(2) . . ? C222 C221 Si2 119.9(2) . . ? C223 C222 C221 121.6(3) . . ? C223 C222 H222 119.2 . . ? C221 C222 H222 119.2 . . ? C224 C223 C222 120.0(3) . . ? C224 C223 H223 120 . . ? C222 C223 H223 120 . . ? C225 C224 C223 119.5(3) . . ? C225 C224 H224 120.2 . . ? C223 C224 H224 120.2 . . ? C224 C225 C226 120.3(3) . . ? C224 C225 H225 119.9 . . ? C226 C225 H225 119.9 . . ? C225 C226 C221 121.7(3) . . ? C225 C226 H226 119.1 . . ? C221 C226 H226 119.1 . . ? C232 C231 C236 117.5(3) . . ? C232 C231 Si2 119.8(2) . . ? C236 C231 Si2 122.7(2) . . ? C231 C232 C233 121.3(4) . . ? C231 C232 H232 119.4 . . ? C233 C232 H232 119.4 . . ? C234 C233 C232 120.0(4) . . ? C234 C233 H233 120 . . ? C232 C233 H233 120 . . ? C233 C234 C235 120.0(3) . . ? C233 C234 H234 120 . . ? C235 C234 H234 120 . . ? C234 C235 C236 119.9(4) . . ? C234 C235 H235 120.1 . . ? C236 C235 H235 120.1 . . ? C235 C236 C231 121.3(4) . . ? C235 C236 H236 119.4 . . ? C231 C236 H236 119.4 . . ? C316 C311 C312 116.5(4) . . ? C316 C311 Si3 122.6(3) . . ? C312 C311 Si3 120.8(3) . . ? C313 C312 C311 121.3(5) . . ? C313 C312 H312 119.4 . . ? C311 C312 H312 119.4 . . ? C314 C313 C312 119.3(5) . . ? C314 C313 H313 120.3 . . ? C312 C313 H313 120.3 . . ? C315 C314 C313 121.1(5) . . ? C315 C314 H314 119.4 . . ? C313 C314 H314 119.4 . . ? C314 C315 C316 119.7(5) . . ? C314 C315 H315 120.2 . . ? C316 C315 H315 120.2 . . ? C311 C316 C315 122.0(4) . . ? C311 C316 H316 119 . . ? C315 C316 H316 119 . . ? C322 C321 C326 115.6(3) . . ? C322 C321 Si3 121.9(3) . . ? C326 C321 Si3 122.3(3) . . ? C321 C322 C323 121.1(4) . . ? C321 C322 H322 119.4 . . ? C323 C322 H322 119.4 . . ? C324 C323 C322 120.9(4) . . ? C324 C323 H323 119.6 . . ? C322 C323 H323 119.6 . . ? C325 C324 C323 119.7(4) . . ? C325 C324 H324 120.2 . . ? C323 C324 H324 120.2 . . ? C324 C325 C326 119.8(4) . . ? C324 C325 H325 120.1 . . ? C326 C325 H325 120.1 . . ? C325 C326 C321 122.9(4) . . ? C325 C326 H326 118.6 . . ? C321 C326 H326 118.6 . . ? C332 C331 C336 116.8(3) . . ? C332 C331 Si3 120.0(2) . . ? C336 C331 Si3 123.2(2) . . ? C333 C332 C331 121.9(3) . . ? C333 C332 H332 119 . . ? C331 C332 H332 119 . . ? C334 C333 C332 120.6(4) . . ? C334 C333 H333 119.7 . . ? C332 C333 H333 119.7 . . ? C333 C334 C335 119.1(4) . . ? C333 C334 H334 120.5 . . ? C335 C334 H334 120.5 . . ? C334 C335 C336 120.6(4) . . ? C334 C335 H335 119.7 . . ? C336 C335 H335 119.7 . . ? C331 C336 C335 121.0(3) . . ? C331 C336 H336 119.5 . . ? C335 C336 H336 119.5 . . ? C5 O6 H6 109.5 . . ? C111 Si1 C121 109.91(15) . . ? C111 Si1 C131 110.64(14) . . ? C121 Si1 C131 109.30(14) . . ? C111 Si1 C1 105.65(13) . . ? C121 Si1 C1 110.69(13) . . ? C131 Si1 C1 110.61(12) . . ? C221 Si2 C231 112.38(13) . . ? C221 Si2 C4 110.14(12) . . ? C231 Si2 C4 112.21(12) . . ? C221 Si2 C211 109.39(13) . . ? C231 Si2 C211 108.79(14) . . ? C4 Si2 C211 103.52(13) . . ? C7 Si3 C311 110.98(16) . . ? C7 Si3 C321 113.60(15) . . ? C311 Si3 C321 108.43(15) . . ? C7 Si3 C331 105.44(14) . . ? C311 Si3 C331 109.52(14) . . ? C321 Si3 C331 108.77(15) . . ? C11 Ru1 C12 90.71(16) . . ? C11 Ru1 C6 92.81(14) . . ? C12 Ru1 C6 86.75(13) . . ? C11 Ru1 C3 120.79(13) . . ? C12 Ru1 C3 96.97(12) . . ? C6 Ru1 C3 146.02(12) . . ? C11 Ru1 C2 94.09(13) . . ? C12 Ru1 C2 125.63(12) . . ? C6 Ru1 C2 146.71(11) . . ? C3 Ru1 C2 37.04(10) . . ? C11 Ru1 C1 101.20(14) . . ? C12 Ru1 C1 159.47(12) . . ? C6 Ru1 C1 109.04(11) . . ? C3 Ru1 C1 62.58(10) . . ? C2 Ru1 C1 37.68(9) . . ? C11 Ru1 C4 156.56(13) . . ? C12 Ru1 C4 100.50(12) . . ? C6 Ru1 C4 108.20(11) . . ? C3 Ru1 C4 37.86(10) . . ? C2 Ru1 C4 62.65(10) . . ? C1 Ru1 C4 62.70(10) . . ? C11 Ru1 C5 135.78(14) . . ? C12 Ru1 C5 133.39(13) . . ? C6 Ru1 C5 92.89(11) . . ? C3 Ru1 C5 60.31(10) . . ? C2 Ru1 C5 60.34(10) . . ? C1 Ru1 C5 36.31(10) . . ? C4 Ru1 C5 36.06(9) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C5 C1 C2 C3 -3.0(3) . . . . ? Si1 C1 C2 C3 -169.1(2) . . . . ? Ru1 C1 C2 C3 62.6(2) . . . . ? C5 C1 C2 Ru1 -65.5(2) . . . . ? Si1 C1 C2 Ru1 128.4(2) . . . . ? C1 C2 C3 C4 0.7(3) . . . . ? Ru1 C2 C3 C4 64.9(2) . . . . ? C1 C2 C3 Ru1 -64.3(2) . . . . ? C2 C3 C4 C5 1.9(3) . . . . ? Ru1 C3 C4 C5 65.48(19) . . . . ? C2 C3 C4 Si2 165.9(2) . . . . ? Ru1 C3 C4 Si2 -130.5(2) . . . . ? C2 C3 C4 Ru1 -63.5(2) . . . . ? C3 C4 C5 O6 175.3(3) . . . . ? Si2 C4 C5 O6 13.2(4) . . . . ? Ru1 C4 C5 O6 -123.2(3) . . . . ? C3 C4 C5 C1 -3.9(3) . . . . ? Si2 C4 C5 C1 -166.0(2) . . . . ? Ru1 C4 C5 C1 57.6(2) . . . . ? C3 C4 C5 Ru1 -61.54(18) . . . . ? Si2 C4 C5 Ru1 136.4(3) . . . . ? C2 C1 C5 O6 -174.9(3) . . . . ? Si1 C1 C5 O6 -9.6(5) . . . . ? Ru1 C1 C5 O6 123.1(3) . . . . ? C2 C1 C5 C4 4.3(3) . . . . ? Si1 C1 C5 C4 169.6(2) . . . . ? Ru1 C1 C5 C4 -57.7(2) . . . . ? C2 C1 C5 Ru1 62.02(19) . . . . ? Si1 C1 C5 Ru1 -132.7(2) . . . . ? Ru1 C6 C7 Si3 5(5) . . . . ? C116 C111 C112 C113 0.2(5) . . . . ? Si1 C111 C112 C113 -178.8(3) . . . . ? C111 C112 C113 C114 -0.2(6) . . . . ? C112 C113 C114 C115 0.1(7) . . . . ? C113 C114 C115 C116 0.1(7) . . . . ? C114 C115 C116 C111 -0.2(6) . . . . ? C112 C111 C116 C115 0.0(5) . . . . ? Si1 C111 C116 C115 179.0(3) . . . . ? C126 C121 C122 C123 -0.7(6) . . . . ? Si1 C121 C122 C123 177.9(3) . . . . ? C121 C122 C123 C124 1.1(6) . . . . ? C122 C123 C124 C125 -1.3(8) . . . . ? C123 C124 C125 C126 1.2(9) . . . . ? C124 C125 C126 C121 -0.9(8) . . . . ? C122 C121 C126 C125 0.7(7) . . . . ? Si1 C121 C126 C125 -178.0(4) . . . . ? C136 C131 C132 C133 -0.9(5) . . . . ? Si1 C131 C132 C133 173.7(3) . . . . ? C131 C132 C133 C134 0.0(6) . . . . ? C132 C133 C134 C135 0.6(7) . . . . ? C133 C134 C135 C136 -0.3(7) . . . . ? C134 C135 C136 C131 -0.7(7) . . . . ? C132 C131 C136 C135 1.3(5) . . . . ? Si1 C131 C136 C135 -173.5(3) . . . . ? C216 C211 C212 C213 0.0(5) . . . . ? Si2 C211 C212 C213 -175.9(3) . . . . ? C211 C212 C213 C214 0.9(6) . . . . ? C212 C213 C214 C215 -0.7(6) . . . . ? C213 C214 C215 C216 -0.3(5) . . . . ? C214 C215 C216 C211 1.3(5) . . . . ? C212 C211 C216 C215 -1.1(4) . . . . ? Si2 C211 C216 C215 174.8(2) . . . . ? C226 C221 C222 C223 -0.6(5) . . . . ? Si2 C221 C222 C223 179.6(3) . . . . ? C221 C222 C223 C224 0.1(5) . . . . ? C222 C223 C224 C225 0.7(6) . . . . ? C223 C224 C225 C226 -0.9(6) . . . . ? C224 C225 C226 C221 0.4(6) . . . . ? C222 C221 C226 C225 0.4(5) . . . . ? Si2 C221 C226 C225 -179.8(3) . . . . ? C236 C231 C232 C233 0.9(5) . . . . ? Si2 C231 C232 C233 179.5(3) . . . . ? C231 C232 C233 C234 -0.3(6) . . . . ? C232 C233 C234 C235 -0.6(6) . . . . ? C233 C234 C235 C236 0.8(6) . . . . ? C234 C235 C236 C231 -0.2(5) . . . . ? C232 C231 C236 C235 -0.6(5) . . . . ? Si2 C231 C236 C235 -179.3(3) . . . . ? C316 C311 C312 C313 0.7(6) . . . . ? Si3 C311 C312 C313 -175.3(3) . . . . ? C311 C312 C313 C314 -1.0(7) . . . . ? C312 C313 C314 C315 1.3(8) . . . . ? C313 C314 C315 C316 -1.4(9) . . . . ? C312 C311 C316 C315 -0.8(6) . . . . ? Si3 C311 C316 C315 175.1(3) . . . . ? C314 C315 C316 C311 1.1(7) . . . . ? C326 C321 C322 C323 0.0(6) . . . . ? Si3 C321 C322 C323 175.6(4) . . . . ? C321 C322 C323 C324 0.1(7) . . . . ? C322 C323 C324 C325 -0.3(7) . . . . ? C323 C324 C325 C326 0.5(6) . . . . ? C324 C325 C326 C321 -0.4(6) . . . . ? C322 C321 C326 C325 0.2(5) . . . . ? Si3 C321 C326 C325 -175.4(3) . . . . ? C336 C331 C332 C333 -0.4(6) . . . . ? Si3 C331 C332 C333 -177.5(3) . . . . ? C331 C332 C333 C334 2.1(7) . . . . ? C332 C333 C334 C335 -2.1(7) . . . . ? C333 C334 C335 C336 0.4(7) . . . . ? C332 C331 C336 C335 -1.3(5) . . . . ? Si3 C331 C336 C335 175.8(3) . . . . ? C334 C335 C336 C331 1.3(6) . . . . ? C112 C111 Si1 C121 168.4(2) . . . . ? C116 C111 Si1 C121 -10.5(3) . . . . ? C112 C111 Si1 C131 -70.8(3) . . . . ? C116 C111 Si1 C131 110.4(3) . . . . ? C112 C111 Si1 C1 49.0(3) . . . . ? C116 C111 Si1 C1 -129.9(3) . . . . ? C126 C121 Si1 C111 124.3(3) . . . . ? C122 C121 Si1 C111 -54.3(3) . . . . ? C126 C121 Si1 C131 2.7(4) . . . . ? C122 C121 Si1 C131 -175.9(3) . . . . ? C126 C121 Si1 C1 -119.4(3) . . . . ? C122 C121 Si1 C1 62.0(3) . . . . ? C132 C131 Si1 C111 164.5(3) . . . . ? C136 C131 Si1 C111 -20.9(3) . . . . ? C132 C131 Si1 C121 -74.3(3) . . . . ? C136 C131 Si1 C121 100.3(3) . . . . ? C132 C131 Si1 C1 47.8(3) . . . . ? C136 C131 Si1 C1 -137.6(3) . . . . ? C5 C1 Si1 C111 -87.4(3) . . . . ? C2 C1 Si1 C111 75.1(3) . . . . ? Ru1 C1 Si1 C111 167.36(18) . . . . ? C5 C1 Si1 C121 153.6(3) . . . . ? C2 C1 Si1 C121 -43.8(3) . . . . ? Ru1 C1 Si1 C121 48.4(2) . . . . ? C5 C1 Si1 C131 32.3(3) . . . . ? C2 C1 Si1 C131 -165.1(2) . . . . ? Ru1 C1 Si1 C131 -72.9(2) . . . . ? C226 C221 Si2 C231 -17.0(3) . . . . ? C222 C221 Si2 C231 162.9(2) . . . . ? C226 C221 Si2 C4 108.9(3) . . . . ? C222 C221 Si2 C4 -71.2(3) . . . . ? C226 C221 Si2 C211 -137.9(3) . . . . ? C222 C221 Si2 C211 41.9(3) . . . . ? C232 C231 Si2 C221 -111.4(3) . . . . ? C236 C231 Si2 C221 67.2(3) . . . . ? C232 C231 Si2 C4 123.8(2) . . . . ? C236 C231 Si2 C4 -57.6(3) . . . . ? C232 C231 Si2 C211 9.9(3) . . . . ? C236 C231 Si2 C211 -171.6(2) . . . . ? C5 C4 Si2 C221 -145.4(3) . . . . ? C3 C4 Si2 C221 55.3(3) . . . . ? Ru1 C4 Si2 C221 -35.3(2) . . . . ? C5 C4 Si2 C231 -19.4(3) . . . . ? C3 C4 Si2 C231 -178.7(2) . . . . ? Ru1 C4 Si2 C231 90.7(2) . . . . ? C5 C4 Si2 C211 97.7(3) . . . . ? C3 C4 Si2 C211 -61.6(2) . . . . ? Ru1 C4 Si2 C211 -152.21(18) . . . . ? C212 C211 Si2 C221 -144.9(3) . . . . ? C216 C211 Si2 C221 39.4(3) . . . . ? C212 C211 Si2 C231 92.0(3) . . . . ? C216 C211 Si2 C231 -83.7(3) . . . . ? C212 C211 Si2 C4 -27.5(3) . . . . ? C216 C211 Si2 C4 156.8(2) . . . . ? C6 C7 Si3 C311 -109.1(10) . . . . ? C6 C7 Si3 C321 128.4(10) . . . . ? C6 C7 Si3 C331 9.4(11) . . . . ? C316 C311 Si3 C7 20.8(3) . . . . ? C312 C311 Si3 C7 -163.5(3) . . . . ? C316 C311 Si3 C321 146.2(3) . . . . ? C312 C311 Si3 C321 -38.1(3) . . . . ? C316 C311 Si3 C331 -95.3(3) . . . . ? C312 C311 Si3 C331 80.5(3) . . . . ? C322 C321 Si3 C7 69.6(3) . . . . ? C326 C321 Si3 C7 -115.1(3) . . . . ? C322 C321 Si3 C311 -54.3(3) . . . . ? C326 C321 Si3 C311 121.0(3) . . . . ? C322 C321 Si3 C331 -173.3(3) . . . . ? C326 C321 Si3 C331 2.0(3) . . . . ? C332 C331 Si3 C7 51.4(3) . . . . ? C336 C331 Si3 C7 -125.5(3) . . . . ? C332 C331 Si3 C311 170.9(3) . . . . ? C336 C331 Si3 C311 -6.1(3) . . . . ? C332 C331 Si3 C321 -70.8(3) . . . . ? C336 C331 Si3 C321 112.3(3) . . . . ? O11 C11 Ru1 C12 95(4) . . . . ? O11 C11 Ru1 C6 -18E1(10) . . . . ? O11 C11 Ru1 C3 -3(4) . . . . ? O11 C11 Ru1 C2 -30(4) . . . . ? O11 C11 Ru1 C1 -68(4) . . . . ? O11 C11 Ru1 C4 -24(4) . . . . ? O11 C11 Ru1 C5 -81(4) . . . . ? O12 C12 Ru1 C11 -126(16) . . . . ? O12 C12 Ru1 C6 141(16) . . . . ? O12 C12 Ru1 C3 -5(16) . . . . ? O12 C12 Ru1 C2 -31(16) . . . . ? O12 C12 Ru1 C1 0(16) . . . . ? O12 C12 Ru1 C4 33(16) . . . . ? O12 C12 Ru1 C5 50(16) . . . . ? C7 C6 Ru1 C11 -140(4) . . . . ? C7 C6 Ru1 C12 -50(4) . . . . ? C7 C6 Ru1 C3 48(4) . . . . ? C7 C6 Ru1 C2 118(4) . . . . ? C7 C6 Ru1 C1 117(4) . . . . ? C7 C6 Ru1 C4 50(4) . . . . ? C7 C6 Ru1 C5 84(4) . . . . ? C2 C3 Ru1 C11 -49.3(2) . . . . ? C4 C3 Ru1 C11 -166.83(18) . . . . ? C2 C3 Ru1 C12 -144.33(19) . . . . ? C4 C3 Ru1 C12 98.15(18) . . . . ? C2 C3 Ru1 C6 121.1(2) . . . . ? C4 C3 Ru1 C6 3.6(3) . . . . ? C4 C3 Ru1 C2 -117.5(2) . . . . ? C2 C3 Ru1 C1 37.56(16) . . . . ? C4 C3 Ru1 C1 -79.95(16) . . . . ? C2 C3 Ru1 C4 117.5(2) . . . . ? C2 C3 Ru1 C5 79.04(17) . . . . ? C4 C3 Ru1 C5 -38.48(15) . . . . ? C3 C2 Ru1 C11 139.22(19) . . . . ? C1 C2 Ru1 C11 -103.06(19) . . . . ? C3 C2 Ru1 C12 45.4(2) . . . . ? C1 C2 Ru1 C12 163.12(18) . . . . ? C3 C2 Ru1 C6 -119.3(2) . . . . ? C1 C2 Ru1 C6 -1.6(3) . . . . ? C1 C2 Ru1 C3 117.7(2) . . . . ? C3 C2 Ru1 C1 -117.7(2) . . . . ? C3 C2 Ru1 C4 -37.79(16) . . . . ? C1 C2 Ru1 C4 79.92(17) . . . . ? C3 C2 Ru1 C5 -78.95(17) . . . . ? C1 C2 Ru1 C5 38.76(15) . . . . ? C5 C1 Ru1 C11 -164.66(18) . . . . ? C2 C1 Ru1 C11 82.10(18) . . . . ? Si1 C1 Ru1 C11 -36.0(2) . . . . ? C5 C1 Ru1 C12 71.0(4) . . . . ? C2 C1 Ru1 C12 -42.3(4) . . . . ? Si1 C1 Ru1 C12 -160.4(3) . . . . ? C5 C1 Ru1 C6 -67.69(18) . . . . ? C2 C1 Ru1 C6 179.06(16) . . . . ? Si1 C1 Ru1 C6 61.0(2) . . . . ? C5 C1 Ru1 C3 76.32(17) . . . . ? C2 C1 Ru1 C3 -36.92(16) . . . . ? Si1 C1 Ru1 C3 -155.0(2) . . . . ? C5 C1 Ru1 C2 113.2(2) . . . . ? Si1 C1 Ru1 C2 -118.1(3) . . . . ? C5 C1 Ru1 C4 33.48(15) . . . . ? C2 C1 Ru1 C4 -79.76(17) . . . . ? Si1 C1 Ru1 C4 162.2(2) . . . . ? C2 C1 Ru1 C5 -113.2(2) . . . . ? Si1 C1 Ru1 C5 128.7(3) . . . . ? C5 C4 Ru1 C11 -83.8(4) . . . . ? C3 C4 Ru1 C11 29.5(4) . . . . ? Si2 C4 Ru1 C11 143.9(3) . . . . ? C5 C4 Ru1 C12 158.83(18) . . . . ? C3 C4 Ru1 C12 -87.86(18) . . . . ? Si2 C4 Ru1 C12 26.6(2) . . . . ? C5 C4 Ru1 C6 68.81(18) . . . . ? C3 C4 Ru1 C6 -177.88(16) . . . . ? Si2 C4 Ru1 C6 -63.4(2) . . . . ? C5 C4 Ru1 C3 -113.3(2) . . . . ? Si2 C4 Ru1 C3 114.5(3) . . . . ? C5 C4 Ru1 C2 -76.34(17) . . . . ? C3 C4 Ru1 C2 36.97(15) . . . . ? Si2 C4 Ru1 C2 151.4(2) . . . . ? C5 C4 Ru1 C1 -33.71(15) . . . . ? C3 C4 Ru1 C1 79.61(16) . . . . ? Si2 C4 Ru1 C1 -165.9(2) . . . . ? C3 C4 Ru1 C5 113.3(2) . . . . ? Si2 C4 Ru1 C5 -132.2(3) . . . . ? O6 C5 Ru1 C11 -97.4(3) . . . . ? C4 C5 Ru1 C11 145.5(2) . . . . ? C1 C5 Ru1 C11 21.8(2) . . . . ? O6 C5 Ru1 C12 87.9(3) . . . . ? C4 C5 Ru1 C12 -29.3(2) . . . . ? C1 C5 Ru1 C12 -152.86(18) . . . . ? O6 C5 Ru1 C6 -0.3(2) . . . . ? C4 C5 Ru1 C6 -117.52(17) . . . . ? C1 C5 Ru1 C6 118.88(16) . . . . ? O6 C5 Ru1 C3 157.6(3) . . . . ? C4 C5 Ru1 C3 40.45(16) . . . . ? C1 C5 Ru1 C3 -83.16(17) . . . . ? O6 C5 Ru1 C2 -159.5(3) . . . . ? C4 C5 Ru1 C2 83.33(17) . . . . ? C1 C5 Ru1 C2 -40.27(15) . . . . ? O6 C5 Ru1 C1 -119.2(3) . . . . ? C4 C5 Ru1 C1 123.6(2) . . . . ? O6 C5 Ru1 C4 117.2(3) . . . . ? C1 C5 Ru1 C4 -123.6(2) . . . . ? data_mrvian30 _database_code_depnum_ccdc_archive 'CCDC 903658' #TrackingRef 'compound 8.cif' _audit_creation_date 2012-12-13T15:56:27-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.4 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common 'compound 8' _chemical_formula_moiety 'C54 H25 O12 Ru3 Si2' _chemical_formula_sum 'C50 H44 Cl2 O4 Ru2 Si3' _chemical_formula_weight 1066.16 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _space_group_crystal_system monoclinic _space_group_name_H-M_alt 'P 21/c' _space_group_name_Hall '-P 2ybc' _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/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' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 _cell_length_a 21.1550(4) _cell_length_b 10.5856(2) _cell_length_c 21.6389(5) _cell_angle_alpha 90 _cell_angle_beta 95.8720(10) _cell_angle_gamma 90 _cell_volume 4820.35(17) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 600 _cell_measurement_theta_min 1 _cell_measurement_theta_max 14 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.33 _exptl_crystal_size_min 0.21 _exptl_crystal_density_diffrn 1.469 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2160 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.855 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.7219 _exptl_absorpt_correction_T_max 0.7822 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 9 _diffrn_orient_matrix_type 'by Bruker AXS Collect from scalepack cell' _diffrn_orient_matrix_ub_11 0.18262E-1 _diffrn_orient_matrix_ub_12 -0.0803 _diffrn_orient_matrix_ub_13 -0.148211E-1 _diffrn_orient_matrix_ub_21 -0.284551E-1 _diffrn_orient_matrix_ub_22 -0.497369E-1 _diffrn_orient_matrix_ub_23 0.250443E-1 _diffrn_orient_matrix_ub_31 -0.333902E-1 _diffrn_orient_matrix_ub_32 -0.15324E-2 _diffrn_orient_matrix_ub_33 -0.362126E-1 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.0581 _diffrn_reflns_number 27726 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.312 _diffrn_reflns_theta_max 27.502 _diffrn_reflns_theta_full 25 _diffrn_measured_fraction_theta_full 0.935 _diffrn_measured_fraction_theta_max 0.926 _diffrn_reflns_Laue_measured_fraction_full 0.935 _diffrn_reflns_Laue_measured_fraction_max 0.926 _diffrn_reflns_point_group_measured_fraction_ful 0.935 _diffrn_reflns_point_group_measured_fraction_max 0.926 _reflns_number_total 10264 _reflns_number_gt 6504 _reflns_threshold_expression 'I > 2\s(I)' _diffrn_reflns_reduction_process ; Scaled and merged with Sortav R.H. Blessing, (1987) Cryst. Rev. 1, 3-58 R.H. Blessing, (1989) J. Appl. Cryst. 22, 396-397 ; #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXL-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-2012 (Sheldrick, 2012)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_hydrogens mixed #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; ? ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; w=1/[\s^2^(Fo^2^)+(0.0690P)^2^+5.2521P] where P=(Fo^2^+2Fc^2^)/3 ; _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_coef 0.00045(18) _refine_ls_number_reflns 10264 _refine_ls_number_parameters 560 _refine_ls_number_restraints 26 _refine_ls_R_factor_all 0.1238 _refine_ls_R_factor_gt 0.0673 _refine_ls_wR_factor_ref 0.1595 _refine_ls_wR_factor_gt 0.1296 _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_restrained_S_all 1.059 _refine_ls_shift/su_max 0.046 _refine_ls_shift/su_mean 0.001 _refine_diff_density_max 0.886 _refine_diff_density_min -0.965 _refine_diff_density_rms 0.123 #----------------------------------------------------------------------------# # 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' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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_calc_flag _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.14016(17) 0.4891(3) 0.49758(16) 0.0398(9) Uani 1 d . . H1 H 0.1206 0.5316 0.5311 0.048 Uiso 1 calc . . C2 C 0.19002(17) 0.4021(3) 0.51101(15) 0.0359(8) Uani 1 d . . C3 C 0.19530(16) 0.3032(3) 0.46270(15) 0.0371(8) Uani 1 d . . C4 C 0.16754(16) 0.3385(3) 0.39796(15) 0.0385(9) Uani 1 d . . C5 C 0.19736(16) 0.4538(3) 0.38310(15) 0.0380(9) Uani 1 d . . C6 C 0.21547(18) 0.4737(3) 0.31941(16) 0.0431(9) Uani 1 d . . C7 C 0.26775(18) 0.5272(4) 0.30241(16) 0.0433(9) Uani 1 d . . C8 C 0.1015(3) 0.0802(4) 0.3901(3) 0.0842(17) Uani 1 d . . H6A H 0.0925 0.0059 0.3653 0.126 Uiso 1 calc . . H6B H 0.0623 0.1174 0.3998 0.126 Uiso 1 calc . . H6C H 0.1267 0.0576 0.4279 0.126 Uiso 1 calc . . C9 C 0.2200(3) 0.1243(5) 0.3240(2) 0.0859(16) Uani 1 d . . H5A H 0.2447 0.0934 0.3605 0.129 Uiso 1 calc . . H5B H 0.2441 0.1865 0.3041 0.129 Uiso 1 calc . . H5C H 0.2096 0.0555 0.2959 0.129 Uiso 1 calc . . C10 C 0.0919(2) 0.2379(5) 0.2745(2) 0.0779(16) Uani 1 d . . H7A H 0.0771 0.1618 0.2536 0.117 Uiso 1 calc . . H7B H 0.1147 0.2878 0.2471 0.117 Uiso 1 calc . . H7C H 0.0563 0.2851 0.2862 0.117 Uiso 1 calc . . C11 C 0.0303(2) 0.3953(4) 0.4212(2) 0.0604(12) Uani 1 d . . C12 C 0.0666(2) 0.6605(4) 0.4272(2) 0.0652(13) Uani 1 d . . C13 C 0.0738(2) 0.5376(4) 0.3183(2) 0.0601(12) Uani 1 d . . C14 C 0.31819(19) 0.6212(3) 0.48273(17) 0.0468(10) Uani 1 d . . H14 H 0.3527 0.567 0.4902 0.056 Uiso 1 calc . . C15 C 0.2840(2) 0.6581(4) 0.53284(17) 0.0559(11) Uani 1 d . . H15 H 0.2962 0.6273 0.5725 0.067 Uiso 1 calc . . C16 C 0.2323(2) 0.7402(4) 0.5231(2) 0.0611(12) Uani 1 d . . H16 H 0.2112 0.7675 0.5563 0.073 Uiso 1 calc . . C17 C 0.2127(2) 0.7808(4) 0.4629(2) 0.0602(12) Uani 1 d . . H17 H 0.1771 0.8324 0.4557 0.072 Uiso 1 calc . . C18 C 0.2467(2) 0.7440(3) 0.41254(19) 0.0528(11) Uani 1 d . . H18 H 0.2331 0.7724 0.3727 0.063 Uiso 1 calc . . C19 C 0.30080(18) 0.6652(3) 0.42153(17) 0.0435(9) Uani 1 d . . C111 C 0.19343(18) 0.4828(3) 0.64802(15) 0.0406(9) Uani 1 d . . C112 C 0.2387(2) 0.5653(3) 0.67743(16) 0.0468(10) Uani 1 d . . H112 H 0.2813 0.5552 0.6714 0.056 Uiso 1 calc . . C113 C 0.2211(2) 0.6616(4) 0.71529(18) 0.0599(13) Uani 1 d . . H113 H 0.2518 0.7158 0.7342 0.072 Uiso 1 calc . . C114 C 0.1589(3) 0.6773(4) 0.7249(2) 0.0699(14) Uani 1 d . . H114 H 0.1474 0.7424 0.7504 0.084 Uiso 1 calc . . C115 C 0.1133(2) 0.5978(4) 0.6974(2) 0.0673(13) Uani 1 d . . H115 H 0.071 0.6084 0.7045 0.081 Uiso 1 calc . . C116 C 0.1304(2) 0.5008(4) 0.65868(18) 0.0524(11) Uani 1 d . . H116 H 0.0992 0.4475 0.6398 0.063 Uiso 1 calc . . C121 C 0.17163(18) 0.2033(3) 0.60614(16) 0.0429(9) Uani 1 d . . C122 C 0.1108(2) 0.1848(4) 0.5792(2) 0.0651(13) Uani 1 d . . H122 H 0.0904 0.2501 0.5563 0.078 Uiso 1 calc . . C123 C 0.0787(2) 0.0725(4) 0.5849(3) 0.0811(17) Uani 1 d . . H123 H 0.0373 0.0635 0.5662 0.097 Uiso 1 calc . . C124 C 0.1075(2) -0.0256(4) 0.6178(2) 0.0724(14) Uani 1 d . . H124 H 0.0862 -0.1015 0.6217 0.087 Uiso 1 calc . . C125 C 0.1683(2) -0.0101(4) 0.6451(2) 0.0678(14) Uani 1 d . . H125 H 0.1886 -0.0762 0.6674 0.081 Uiso 1 calc . . C126 C 0.1996(2) 0.1022(4) 0.63958(18) 0.0553(12) Uani 1 d . . H126 H 0.2407 0.111 0.6588 0.066 Uiso 1 calc . . C131 C 0.30383(17) 0.3255(3) 0.61063(16) 0.0408(9) Uani 1 d . . C132 C 0.32974(19) 0.2966(4) 0.67106(18) 0.0517(11) Uani 1 d . . H132 H 0.3033 0.2984 0.7029 0.062 Uiso 1 calc . . C133 C 0.3929(2) 0.2656(4) 0.6853(2) 0.0650(13) Uani 1 d . . H133 H 0.4085 0.2464 0.726 0.078 Uiso 1 calc . . C134 C 0.4326(2) 0.2635(5) 0.6385(2) 0.0704(14) Uani 1 d . . H134 H 0.4751 0.2416 0.6472 0.084 Uiso 1 calc . . C135 C 0.4087(2) 0.2941(4) 0.5786(2) 0.0638(13) Uani 1 d . . H135 H 0.4357 0.2954 0.5472 0.077 Uiso 1 calc . . C136 C 0.34534(18) 0.3228(3) 0.56491(17) 0.0466(10) Uani 1 d . . H136 H 0.33 0.3409 0.5241 0.056 Uiso 1 calc . . C311 C 0.3908(2) 0.4622(4) 0.38103(18) 0.0505(10) Uani 1 d . . C312 C 0.3694(3) 0.3390(4) 0.3821(2) 0.0757(16) Uani 1 d . . H312 H 0.3271 0.3207 0.3696 0.091 Uiso 1 calc . . C313 C 0.4110(3) 0.2428(6) 0.4019(3) 0.1074(15) Uani 1 d . . H313 H 0.3961 0.1602 0.4024 0.129 Uiso 1 calc . . C314 C 0.4728(3) 0.2664(6) 0.4205(3) 0.1074(15) Uani 1 d . . H314 H 0.5001 0.2004 0.4333 0.129 Uiso 1 calc . . C315 C 0.4945(3) 0.3855(7) 0.4205(3) 0.110(2) Uani 1 d . . H315 H 0.5369 0.4023 0.4338 0.131 Uiso 1 calc . . C316 C 0.4538(3) 0.4837(5) 0.4006(2) 0.0784(16) Uani 1 d . . H316 H 0.4695 0.5658 0.4005 0.094 Uiso 1 calc . . C321 C 0.37786(18) 0.7135(4) 0.31056(17) 0.0481(10) Uani 1 d . . C322 C 0.4111(2) 0.6772(5) 0.26195(19) 0.0674(13) Uani 1 d . . H322 H 0.4138 0.5918 0.2525 0.081 Uiso 1 calc . . C323 C 0.4406(2) 0.7652(6) 0.2267(2) 0.0841(17) Uani 1 d . . H323 H 0.4628 0.7385 0.1942 0.101 Uiso 1 calc . . C324 C 0.4368(3) 0.8913(5) 0.2400(2) 0.0879(17) Uani 1 d . . H324 H 0.4559 0.9507 0.2163 0.105 Uiso 1 calc . . C325 C 0.4052(3) 0.9283(5) 0.2877(3) 0.098(2) Uani 1 d . . H325 H 0.4033 1.0138 0.2972 0.118 Uiso 1 calc . . C326 C 0.3755(2) 0.8419(4) 0.3231(2) 0.0741(14) Uani 1 d . . H326 H 0.3537 0.8702 0.3557 0.089 Uiso 1 calc . . O3 O 0.22237(14) 0.2029(2) 0.47334(12) 0.0541(8) Uani 1 d . . O11 O -0.00977(16) 0.3316(4) 0.43265(18) 0.0956(12) Uani 1 d . . O12 O 0.04889(18) 0.7563(3) 0.4431(2) 0.1031(13) Uani 1 d . . O13 O 0.05633(18) 0.5641(4) 0.26952(15) 0.0914(12) Uani 1 d . . Si1 Si 0.21663(5) 0.35409(9) 0.59351(4) 0.0369(2) Uani 1 d . . Si2 Si 0.14607(6) 0.19654(11) 0.34594(5) 0.0538(3) Uani 1 d . . Si3 Si 0.33517(5) 0.59229(10) 0.35380(5) 0.0430(3) Uani 1 d . . Ru1 Ru 0.09987(2) 0.50121(3) 0.40620(2) 0.04367(8) Uani 1 d . . Ru2 Ru 0.21734(2) 0.57261(2) 0.45749(2) 0.03647(7) Uani 1 d . . H6 H 0.1884(11) 0.442(3) 0.2853(9) 0.040(9) Uiso 1 d . . H7 H 0.2723(17) 0.522(3) 0.2584(7) 0.054(11) Uiso 1 d . . C50A C 0.3270(5) -0.0092(8) 0.5546(4) 0.116(4) Uani 0.603(3) d A 1 H50A H 0.3323 0.0802 0.5637 0.139 Uiso 0.603(3) calc A 1 H50B H 0.2825 -0.0234 0.5406 0.139 Uiso 0.603(3) calc A 1 Cl1A Cl 0.34553(19) -0.0909(3) 0.62030(16) 0.1288(7) Uani 0.603(3) d A 1 Cl2A Cl 0.37287(18) -0.0481(3) 0.49340(16) 0.1288(7) Uani 0.603(3) d A 1 C50B C 0.3463(6) 0.0065(12) 0.5405(5) 0.116(4) Uani 0.397(3) d A 2 H50C H 0.3487 0.0975 0.5455 0.139 Uiso 0.397(3) calc A 2 H50D H 0.3049 -0.0151 0.5196 0.139 Uiso 0.397(3) calc A 2 Cl1B Cl 0.3580(3) -0.0671(5) 0.6114(2) 0.1288(7) Uani 0.397(3) d A 2 Cl2B Cl 0.4074(3) -0.0483(5) 0.4978(2) 0.1288(7) Uani 0.397(3) d 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 C1 0.0412(19) 0.0450(18) 0.0349(17) 0.0066(14) 0.0115(14) -0.0035(15) C2 0.0399(19) 0.0362(17) 0.0324(16) -0.0004(13) 0.0068(14) -0.0015(14) C3 0.0374(18) 0.0374(17) 0.0363(16) 0.0025(14) 0.0031(14) -0.0079(14) C4 0.0374(19) 0.0442(18) 0.0346(16) -0.0060(14) 0.0066(14) -0.0066(14) C5 0.0310(18) 0.0494(18) 0.0334(16) -0.0003(15) 0.0024(14) 0.0010(15) C6 0.042(2) 0.0508(19) 0.0361(18) -0.0012(16) 0.0016(16) -0.0008(16) C7 0.043(2) 0.055(2) 0.0331(17) 0.0044(16) 0.0081(15) -0.0071(16) C8 0.102(4) 0.063(3) 0.088(3) -0.006(2) 0.013(3) -0.036(2) C9 0.095(4) 0.083(3) 0.082(3) -0.042(2) 0.023(3) -0.004(3) C10 0.081(3) 0.092(3) 0.056(3) -0.015(2) -0.014(2) -0.021(3) C11 0.041(2) 0.083(3) 0.057(2) 0.013(2) 0.0058(19) 0.000(2) C12 0.043(2) 0.077(3) 0.075(3) 0.022(2) 0.005(2) 0.016(2) C13 0.043(2) 0.084(3) 0.053(2) 0.020(2) 0.0027(19) 0.001(2) C14 0.051(2) 0.0458(19) 0.0430(19) 0.0019(16) 0.0030(17) -0.0150(17) C15 0.077(3) 0.053(2) 0.0387(19) -0.0072(17) 0.0088(19) -0.0238(19) C16 0.081(3) 0.047(2) 0.060(2) -0.0095(19) 0.026(2) -0.013(2) C17 0.070(3) 0.0344(18) 0.079(3) -0.0034(19) 0.023(2) 0.0026(18) C18 0.069(3) 0.0375(18) 0.052(2) 0.0118(17) 0.008(2) -0.0008(18) C19 0.047(2) 0.0383(17) 0.0465(19) 0.0055(15) 0.0101(16) -0.0105(15) C111 0.051(2) 0.0420(18) 0.0293(16) 0.0041(14) 0.0062(15) 0.0009(15) C112 0.060(2) 0.0439(19) 0.0370(18) 0.0033(16) 0.0087(17) -0.0030(17) C113 0.091(3) 0.042(2) 0.046(2) -0.0023(17) 0.005(2) 0.000(2) C114 0.108(4) 0.049(2) 0.053(2) -0.0075(19) 0.010(2) 0.020(2) C115 0.072(3) 0.076(3) 0.057(2) 0.001(2) 0.019(2) 0.028(2) C116 0.058(2) 0.058(2) 0.0420(19) 0.0007(17) 0.0107(18) 0.0099(18) C121 0.054(2) 0.0426(18) 0.0340(17) 0.0036(15) 0.0113(16) -0.0001(16) C122 0.051(3) 0.056(2) 0.084(3) 0.020(2) -0.012(2) -0.0044(19) C123 0.060(3) 0.064(3) 0.118(4) 0.014(3) -0.004(3) -0.013(2) C124 0.077(3) 0.051(2) 0.089(3) 0.015(2) 0.007(3) -0.021(2) C125 0.081(3) 0.048(2) 0.070(3) 0.022(2) -0.012(3) -0.009(2) C126 0.068(3) 0.050(2) 0.047(2) 0.0101(17) -0.003(2) -0.0022(19) C131 0.040(2) 0.0396(17) 0.0422(18) 0.0014(15) 0.0008(16) -0.0007(15) C132 0.043(2) 0.062(2) 0.048(2) 0.0019(18) -0.0048(18) -0.0020(18) C133 0.055(3) 0.074(3) 0.062(3) 0.003(2) -0.010(2) 0.002(2) C134 0.047(3) 0.079(3) 0.084(3) -0.002(3) -0.002(2) -0.002(2) C135 0.047(2) 0.079(3) 0.067(3) -0.003(2) 0.017(2) -0.010(2) C136 0.042(2) 0.052(2) 0.0451(19) -0.0008(17) 0.0042(17) -0.0058(16) C311 0.050(2) 0.059(2) 0.044(2) 0.0032(18) 0.0106(17) 0.0020(18) C312 0.081(4) 0.063(3) 0.080(3) 0.004(2) -0.007(3) 0.004(2) C313 0.138(3) 0.100(2) 0.088(3) 0.025(2) 0.032(3) 0.063(3) C314 0.138(3) 0.100(2) 0.088(3) 0.025(2) 0.032(3) 0.063(3) C315 0.055(3) 0.186(6) 0.086(4) 0.028(4) -0.001(3) 0.038(4) C316 0.060(3) 0.096(3) 0.078(3) 0.017(3) 0.004(3) 0.005(3) C321 0.042(2) 0.063(2) 0.0391(18) 0.0134(17) 0.0036(16) -0.0104(17) C322 0.072(3) 0.081(3) 0.052(2) 0.007(2) 0.024(2) -0.011(2) C323 0.076(3) 0.125(4) 0.054(3) 0.016(3) 0.022(2) -0.021(3) C324 0.097(4) 0.098(3) 0.071(3) 0.031(3) 0.020(3) -0.033(3) C325 0.135(5) 0.063(3) 0.100(4) 0.015(3) 0.028(4) -0.032(3) C326 0.090(3) 0.069(3) 0.067(3) 0.015(2) 0.027(2) -0.021(2) O3 0.0711(18) 0.0419(13) 0.0489(14) -0.0004(11) 0.0041(14) 0.0093(13) O11 0.0502(19) 0.128(3) 0.108(3) 0.027(2) 0.0093(19) -0.0265(19) O12 0.093(2) 0.078(2) 0.143(3) 0.015(2) 0.034(2) 0.0402(18) O13 0.082(3) 0.139(3) 0.0502(17) 0.0326(18) -0.0054(17) 0.015(2) Si1 0.0420(5) 0.0375(5) 0.0315(4) 0.0020(4) 0.0051(4) 0.0009(4) Si2 0.0595(7) 0.0542(6) 0.0476(6) -0.0133(5) 0.0049(5) -0.0163(5) Si3 0.0426(6) 0.0495(5) 0.0377(5) 0.0063(4) 0.0075(4) -0.0072(4) Ru1 0.03558(16) 0.05572(17) 0.03989(15) 0.00916(13) 0.00476(12) 0.00318(13) Ru2 0.04135(15) 0.03477(13) 0.03397(13) 0.00098(11) 0.00710(11) -0.00158(11) C50A 0.111(8) 0.056(4) 0.179(8) -0.018(4) 0.015(6) -0.022(4) Cl1A 0.1405(17) 0.1093(10) 0.1286(11) 0.0025(9) -0.0253(12) -0.0147(11) Cl2A 0.1405(17) 0.1093(10) 0.1286(11) 0.0025(9) -0.0253(12) -0.0147(11) C50B 0.111(8) 0.056(4) 0.179(8) -0.018(4) 0.015(6) -0.022(4) Cl1B 0.1405(17) 0.1093(10) 0.1286(11) 0.0025(9) -0.0253(12) -0.0147(11) Cl2B 0.1405(17) 0.1093(10) 0.1286(11) 0.0025(9) -0.0253(12) -0.0147(11) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 C1 C2 1.408(5) . ? C1 Ru1 2.076(3) . ? C1 Ru2 2.119(3) . ? C1 H1 0.98 . ? C2 C3 1.492(5) . ? C2 Si1 1.886(3) . ? C2 Ru2 2.252(3) . ? C3 O3 1.218(4) . ? C3 C4 1.509(5) . ? C4 C5 1.427(5) . ? C4 Si2 1.904(3) . ? C4 Ru1 2.259(3) . ? C5 C6 1.483(5) . ? C5 Ru2 2.052(3) . ? C5 Ru1 2.228(4) . ? C6 C7 1.327(5) . ? C6 H6 0.947(15) . ? C7 Si3 1.850(4) . ? C7 H7 0.968(14) . ? C8 Si2 1.873(5) . ? C8 H6A 0.96 . ? C8 H6B 0.96 . ? C8 H6C 0.96 . ? C9 Si2 1.846(5) . ? C9 H5A 0.96 . ? C9 H5B 0.96 . ? C9 H5C 0.96 . ? C10 Si2 1.880(5) . ? C10 H7A 0.96 . ? C10 H7B 0.96 . ? C10 H7C 0.96 . ? C11 O11 1.131(5) . ? C11 Ru1 1.904(4) . ? C12 O12 1.146(6) . ? C12 Ru1 1.900(5) . ? C13 O13 1.118(5) . ? C13 Ru1 1.964(4) . ? C14 C19 1.416(5) . ? C14 C15 1.418(5) . ? C14 Ru2 2.208(4) . ? C14 H14 0.93 . ? C15 C16 1.396(6) . ? C15 Ru2 2.235(4) . ? C15 H15 0.93 . ? C16 C17 1.394(6) . ? C16 Ru2 2.274(4) . ? C16 H16 0.93 . ? C17 C18 1.420(6) . ? C17 Ru2 2.210(4) . ? C17 H17 0.93 . ? C18 C19 1.413(5) . ? C18 Ru2 2.179(4) . ? C18 H18 0.93 . ? C19 Si3 1.869(4) . ? C19 Ru2 2.228(4) . ? C111 C116 1.389(6) . ? C111 C112 1.400(5) . ? C111 Si1 1.899(4) . ? C112 C113 1.382(5) . ? C112 H112 0.93 . ? C113 C114 1.364(7) . ? C113 H113 0.93 . ? C114 C115 1.371(7) . ? C114 H114 0.93 . ? C115 C116 1.397(6) . ? C115 H115 0.93 . ? C116 H116 0.93 . ? C121 C122 1.372(6) . ? C121 C126 1.390(5) . ? C121 Si1 1.892(4) . ? C122 C123 1.381(6) . ? C122 H122 0.93 . ? C123 C124 1.367(7) . ? C123 H123 0.93 . ? C124 C125 1.369(7) . ? C124 H124 0.93 . ? C125 C126 1.371(6) . ? C125 H125 0.93 . ? C126 H126 0.93 . ? C131 C136 1.389(5) . ? C131 C132 1.399(5) . ? C131 Si1 1.869(4) . ? C132 C133 1.380(6) . ? C132 H132 0.93 . ? C133 C134 1.380(7) . ? C133 H133 0.93 . ? C134 C135 1.381(6) . ? C134 H134 0.93 . ? C135 C136 1.377(6) . ? C135 H135 0.93 . ? C136 H136 0.93 . ? C311 C316 1.375(7) . ? C311 C312 1.381(6) . ? C311 Si3 1.867(4) . ? C312 C313 1.385(7) . ? C312 H312 0.93 . ? C313 C314 1.351(9) . ? C313 H313 0.93 . ? C314 C315 1.342(9) . ? C314 H314 0.93 . ? C315 C316 1.390(8) . ? C315 H315 0.93 . ? C316 H316 0.93 . ? C321 C322 1.378(6) . ? C321 C326 1.388(6) . ? C321 Si3 1.874(4) . ? C322 C323 1.392(7) . ? C322 H322 0.93 . ? C323 C324 1.370(8) . ? C323 H323 0.93 . ? C324 C325 1.345(8) . ? C324 H324 0.93 . ? C325 C326 1.384(7) . ? C325 H325 0.93 . ? C326 H326 0.93 . ? Ru1 Ru2 2.7229(4) . ? C50A Cl1A 1.677(9) . ? C50A Cl2A 1.769(10) . ? C50A H50A 0.97 . ? C50A H50B 0.97 . ? C50B Cl1B 1.715(12) . ? C50B Cl2B 1.762(13) . ? C50B H50C 0.97 . ? C50B H50D 0.97 . ? 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 Ru1 117.6(2) . . ? C2 C1 Ru2 76.4(2) . . ? Ru1 C1 Ru2 80.95(12) . . ? C2 C1 H1 120.8 . . ? Ru1 C1 H1 120.8 . . ? Ru2 C1 H1 120.8 . . ? C1 C2 C3 115.0(3) . . ? C1 C2 Si1 121.1(3) . . ? C3 C2 Si1 116.0(2) . . ? C1 C2 Ru2 66.16(18) . . ? C3 C2 Ru2 99.2(2) . . ? Si1 C2 Ru2 129.45(17) . . ? O3 C3 C2 123.2(3) . . ? O3 C3 C4 121.5(3) . . ? C2 C3 C4 115.3(3) . . ? C5 C4 C3 106.4(3) . . ? C5 C4 Si2 128.8(3) . . ? C3 C4 Si2 113.6(2) . . ? C5 C4 Ru1 70.3(2) . . ? C3 C4 Ru1 107.7(2) . . ? Si2 C4 Ru1 122.26(17) . . ? C4 C5 C6 119.5(3) . . ? C4 C5 Ru2 114.1(2) . . ? C6 C5 Ru2 126.2(3) . . ? C4 C5 Ru1 72.6(2) . . ? C6 C5 Ru1 120.7(2) . . ? Ru2 C5 Ru1 78.89(12) . . ? C7 C6 C5 128.3(3) . . ? C7 C6 H6 112.8(16) . . ? C5 C6 H6 118.8(16) . . ? C6 C7 Si3 127.3(3) . . ? C6 C7 H7 115(2) . . ? Si3 C7 H7 118(2) . . ? Si2 C8 H6A 109.5 . . ? Si2 C8 H6B 109.5 . . ? H6A C8 H6B 109.5 . . ? Si2 C8 H6C 109.5 . . ? H6A C8 H6C 109.5 . . ? H6B C8 H6C 109.5 . . ? Si2 C9 H5A 109.5 . . ? Si2 C9 H5B 109.5 . . ? H5A C9 H5B 109.5 . . ? Si2 C9 H5C 109.5 . . ? H5A C9 H5C 109.5 . . ? H5B C9 H5C 109.5 . . ? Si2 C10 H7A 109.5 . . ? Si2 C10 H7B 109.5 . . ? H7A C10 H7B 109.5 . . ? Si2 C10 H7C 109.5 . . ? H7A C10 H7C 109.5 . . ? H7B C10 H7C 109.5 . . ? O11 C11 Ru1 177.0(4) . . ? O12 C12 Ru1 175.9(4) . . ? O13 C13 Ru1 175.4(4) . . ? C19 C14 C15 121.3(4) . . ? C19 C14 Ru2 72.2(2) . . ? C15 C14 Ru2 72.4(2) . . ? C19 C14 H14 119.3 . . ? C15 C14 H14 119.3 . . ? Ru2 C14 H14 128.4 . . ? C16 C15 C14 120.6(4) . . ? C16 C15 Ru2 73.5(2) . . ? C14 C15 Ru2 70.4(2) . . ? C16 C15 H15 119.7 . . ? C14 C15 H15 119.7 . . ? Ru2 C15 H15 128.7 . . ? C17 C16 C15 119.1(4) . . ? C17 C16 Ru2 69.4(2) . . ? C15 C16 Ru2 70.4(2) . . ? C17 C16 H16 120.4 . . ? C15 C16 H16 120.4 . . ? Ru2 C16 H16 132.7 . . ? C16 C17 C18 120.5(4) . . ? C16 C17 Ru2 74.4(2) . . ? C18 C17 Ru2 69.9(2) . . ? C16 C17 H17 119.8 . . ? C18 C17 H17 119.8 . . ? Ru2 C17 H17 128 . . ? C19 C18 C17 121.5(4) . . ? C19 C18 Ru2 73.2(2) . . ? C17 C18 Ru2 72.3(2) . . ? C19 C18 H18 119.2 . . ? C17 C18 H18 119.2 . . ? Ru2 C18 H18 127.4 . . ? C18 C19 C14 116.9(3) . . ? C18 C19 Si3 120.7(3) . . ? C14 C19 Si3 120.8(3) . . ? C18 C19 Ru2 69.4(2) . . ? C14 C19 Ru2 70.6(2) . . ? Si3 C19 Ru2 118.54(17) . . ? C116 C111 C112 117.5(3) . . ? C116 C111 Si1 121.0(3) . . ? C112 C111 Si1 121.4(3) . . ? C113 C112 C111 121.1(4) . . ? C113 C112 H112 119.5 . . ? C111 C112 H112 119.5 . . ? C114 C113 C112 120.2(4) . . ? C114 C113 H113 119.9 . . ? C112 C113 H113 119.9 . . ? C113 C114 C115 120.4(4) . . ? C113 C114 H114 119.8 . . ? C115 C114 H114 119.8 . . ? C114 C115 C116 119.9(4) . . ? C114 C115 H115 120.1 . . ? C116 C115 H115 120.1 . . ? C111 C116 C115 120.9(4) . . ? C111 C116 H116 119.6 . . ? C115 C116 H116 119.6 . . ? C122 C121 C126 116.2(4) . . ? C122 C121 Si1 121.6(3) . . ? C126 C121 Si1 122.1(3) . . ? C121 C122 C123 122.3(4) . . ? C121 C122 H122 118.9 . . ? C123 C122 H122 118.9 . . ? C124 C123 C122 120.2(5) . . ? C124 C123 H123 119.9 . . ? C122 C123 H123 119.9 . . ? C123 C124 C125 118.9(4) . . ? C123 C124 H124 120.5 . . ? C125 C124 H124 120.5 . . ? C124 C125 C126 120.4(4) . . ? C124 C125 H125 119.8 . . ? C126 C125 H125 119.8 . . ? C125 C126 C121 122.0(4) . . ? C125 C126 H126 119 . . ? C121 C126 H126 119 . . ? C136 C131 C132 116.5(3) . . ? C136 C131 Si1 123.0(3) . . ? C132 C131 Si1 120.3(3) . . ? C133 C132 C131 122.6(4) . . ? C133 C132 H132 118.7 . . ? C131 C132 H132 118.7 . . ? C132 C133 C134 119.1(4) . . ? C132 C133 H133 120.4 . . ? C134 C133 H133 120.4 . . ? C135 C134 C133 119.6(4) . . ? C135 C134 H134 120.2 . . ? C133 C134 H134 120.2 . . ? C136 C135 C134 120.5(4) . . ? C136 C135 H135 119.7 . . ? C134 C135 H135 119.7 . . ? C135 C136 C131 121.6(4) . . ? C135 C136 H136 119.2 . . ? C131 C136 H136 119.2 . . ? C316 C311 C312 117.4(4) . . ? C316 C311 Si3 122.3(3) . . ? C312 C311 Si3 120.3(3) . . ? C311 C312 C313 120.1(5) . . ? C311 C312 H312 120 . . ? C313 C312 H312 120 . . ? C314 C313 C312 121.4(6) . . ? C314 C313 H313 119.3 . . ? C312 C313 H313 119.3 . . ? C315 C314 C313 119.6(5) . . ? C315 C314 H314 120.2 . . ? C313 C314 H314 120.2 . . ? C314 C315 C316 120.1(6) . . ? C314 C315 H315 119.9 . . ? C316 C315 H315 119.9 . . ? C311 C316 C315 121.4(5) . . ? C311 C316 H316 119.3 . . ? C315 C316 H316 119.3 . . ? C322 C321 C326 117.0(4) . . ? C322 C321 Si3 120.0(3) . . ? C326 C321 Si3 123.0(3) . . ? C321 C322 C323 121.6(5) . . ? C321 C322 H322 119.2 . . ? C323 C322 H322 119.2 . . ? C324 C323 C322 119.9(5) . . ? C324 C323 H323 120.1 . . ? C322 C323 H323 120.1 . . ? C325 C324 C323 119.3(5) . . ? C325 C324 H324 120.3 . . ? C323 C324 H324 120.3 . . ? C324 C325 C326 121.5(5) . . ? C324 C325 H325 119.3 . . ? C326 C325 H325 119.3 . . ? C325 C326 C321 120.7(5) . . ? C325 C326 H326 119.6 . . ? C321 C326 H326 119.6 . . ? C131 Si1 C2 115.11(16) . . ? C131 Si1 C121 109.62(16) . . ? C2 Si1 C121 104.95(15) . . ? C131 Si1 C111 107.80(16) . . ? C2 Si1 C111 108.88(15) . . ? C121 Si1 C111 110.46(16) . . ? C9 Si2 C8 110.1(2) . . ? C9 Si2 C10 110.2(2) . . ? C8 Si2 C10 106.1(2) . . ? C9 Si2 C4 108.8(2) . . ? C8 Si2 C4 108.6(2) . . ? C10 Si2 C4 113.0(2) . . ? C7 Si3 C311 109.71(18) . . ? C7 Si3 C19 106.72(17) . . ? C311 Si3 C19 109.91(17) . . ? C7 Si3 C321 109.66(16) . . ? C311 Si3 C321 110.01(18) . . ? C19 Si3 C321 110.78(17) . . ? C12 Ru1 C11 99.8(2) . . ? C12 Ru1 C13 89.1(2) . . ? C11 Ru1 C13 97.79(18) . . ? C12 Ru1 C1 87.31(17) . . ? C11 Ru1 C1 92.89(16) . . ? C13 Ru1 C1 169.17(16) . . ? C12 Ru1 C5 128.88(16) . . ? C11 Ru1 C5 130.90(16) . . ? C13 Ru1 C5 90.07(16) . . ? C1 Ru1 C5 84.29(13) . . ? C12 Ru1 C4 161.64(16) . . ? C11 Ru1 C4 94.08(16) . . ? C13 Ru1 C4 100.98(16) . . ? C1 Ru1 C4 79.99(13) . . ? C5 Ru1 C4 37.07(12) . . ? C12 Ru1 Ru2 90.08(14) . . ? C11 Ru1 Ru2 141.52(13) . . ? C13 Ru1 Ru2 119.63(13) . . ? C1 Ru1 Ru2 50.21(10) . . ? C5 Ru1 Ru2 47.69(9) . . ? C4 Ru1 Ru2 71.61(8) . . ? C5 Ru2 C1 87.71(14) . . ? C5 Ru2 C18 101.84(14) . . ? C1 Ru2 C18 142.85(14) . . ? C5 Ru2 C14 116.93(14) . . ? C1 Ru2 C14 139.59(13) . . ? C18 Ru2 C14 66.67(14) . . ? C5 Ru2 C17 130.23(15) . . ? C1 Ru2 C17 110.76(15) . . ? C18 Ru2 C17 37.75(15) . . ? C14 Ru2 C17 78.55(15) . . ? C5 Ru2 C19 95.89(14) . . ? C1 Ru2 C19 176.22(13) . . ? C18 Ru2 C19 37.38(14) . . ? C14 Ru2 C19 37.23(13) . . ? C17 Ru2 C19 67.70(15) . . ? C5 Ru2 C15 152.14(15) . . ? C1 Ru2 C15 109.00(14) . . ? C18 Ru2 C15 78.53(15) . . ? C14 Ru2 C15 37.22(14) . . ? C17 Ru2 C15 65.53(16) . . ? C19 Ru2 C15 67.24(14) . . ? C5 Ru2 C2 82.49(13) . . ? C1 Ru2 C2 37.43(13) . . ? C18 Ru2 C2 175.57(13) . . ? C14 Ru2 C2 110.60(13) . . ? C17 Ru2 C2 139.22(14) . . ? C19 Ru2 C2 141.86(13) . . ? C15 Ru2 C2 97.20(13) . . ? C5 Ru2 C16 166.41(15) . . ? C1 Ru2 C16 97.70(15) . . ? C18 Ru2 C16 66.50(15) . . ? C14 Ru2 C16 66.08(15) . . ? C17 Ru2 C16 36.19(15) . . ? C19 Ru2 C16 79.04(15) . . ? C15 Ru2 C16 36.06(15) . . ? C2 Ru2 C16 109.33(13) . . ? C5 Ru2 Ru1 53.42(10) . . ? C1 Ru2 Ru1 48.83(9) . . ? C18 Ru2 Ru1 109.83(11) . . ? C14 Ru2 Ru1 169.68(10) . . ? C17 Ru2 Ru1 104.77(12) . . ? C19 Ru2 Ru1 134.63(9) . . ? C15 Ru2 Ru1 153.03(11) . . ? C2 Ru2 Ru1 73.48(9) . . ? C16 Ru2 Ru1 122.28(12) . . ? Cl1A C50A Cl2A 114.6(6) . . ? Cl1A C50A H50A 108.6 . . ? Cl2A C50A H50A 108.6 . . ? Cl1A C50A H50B 108.6 . . ? Cl2A C50A H50B 108.6 . . ? H50A C50A H50B 107.6 . . ? Cl1B C50B Cl2B 105.8(7) . . ? Cl1B C50B H50C 110.6 . . ? Cl2B C50B H50C 110.6 . . ? Cl1B C50B H50D 110.6 . . ? Cl2B C50B H50D 110.6 . . ? H50C C50B H50D 108.7 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Ru1 C1 C2 C3 -17.3(4) . . . . ? Ru2 C1 C2 C3 -89.3(3) . . . . ? Ru1 C1 C2 Si1 -164.98(17) . . . . ? Ru2 C1 C2 Si1 123.0(2) . . . . ? Ru1 C1 C2 Ru2 72.01(19) . . . . ? C1 C2 C3 O3 -158.6(3) . . . . ? Si1 C2 C3 O3 -9.2(5) . . . . ? Ru2 C2 C3 O3 133.5(3) . . . . ? C1 C2 C3 C4 24.5(4) . . . . ? Si1 C2 C3 C4 173.9(2) . . . . ? Ru2 C2 C3 C4 -43.4(3) . . . . ? O3 C3 C4 C5 -121.9(4) . . . . ? C2 C3 C4 C5 55.1(4) . . . . ? O3 C3 C4 Si2 25.3(4) . . . . ? C2 C3 C4 Si2 -157.7(2) . . . . ? O3 C3 C4 Ru1 164.0(3) . . . . ? C2 C3 C4 Ru1 -19.0(3) . . . . ? C3 C4 C5 C6 140.7(3) . . . . ? Si2 C4 C5 C6 0.2(5) . . . . ? Ru1 C4 C5 C6 -115.9(3) . . . . ? C3 C4 C5 Ru2 -34.6(3) . . . . ? Si2 C4 C5 Ru2 -175.1(2) . . . . ? Ru1 C4 C5 Ru2 68.83(18) . . . . ? C3 C4 C5 Ru1 -103.4(2) . . . . ? Si2 C4 C5 Ru1 116.1(3) . . . . ? C4 C5 C6 C7 -139.9(4) . . . . ? Ru2 C5 C6 C7 34.8(6) . . . . ? Ru1 C5 C6 C7 133.7(4) . . . . ? C5 C6 C7 Si3 0.8(6) . . . . ? C19 C14 C15 C16 -0.6(6) . . . . ? Ru2 C14 C15 C16 -55.8(3) . . . . ? C19 C14 C15 Ru2 55.3(3) . . . . ? C14 C15 C16 C17 3.1(6) . . . . ? Ru2 C15 C16 C17 -51.3(3) . . . . ? C14 C15 C16 Ru2 54.4(3) . . . . ? C15 C16 C17 C18 -3.0(6) . . . . ? Ru2 C16 C17 C18 -54.8(3) . . . . ? C15 C16 C17 Ru2 51.8(3) . . . . ? C16 C17 C18 C19 0.3(6) . . . . ? Ru2 C17 C18 C19 -56.5(3) . . . . ? C16 C17 C18 Ru2 56.9(4) . . . . ? C17 C18 C19 C14 2.1(5) . . . . ? Ru2 C18 C19 C14 -54.0(3) . . . . ? C17 C18 C19 Si3 167.9(3) . . . . ? Ru2 C18 C19 Si3 111.8(2) . . . . ? C17 C18 C19 Ru2 56.1(3) . . . . ? C15 C14 C19 C18 -2.0(5) . . . . ? Ru2 C14 C19 C18 53.4(3) . . . . ? C15 C14 C19 Si3 -167.7(3) . . . . ? Ru2 C14 C19 Si3 -112.3(2) . . . . ? C15 C14 C19 Ru2 -55.4(3) . . . . ? C116 C111 C112 C113 -0.5(5) . . . . ? Si1 C111 C112 C113 177.7(3) . . . . ? C111 C112 C113 C114 0.4(6) . . . . ? C112 C113 C114 C115 0.2(6) . . . . ? C113 C114 C115 C116 -0.6(7) . . . . ? C112 C111 C116 C115 0.0(5) . . . . ? Si1 C111 C116 C115 -178.2(3) . . . . ? C114 C115 C116 C111 0.6(6) . . . . ? C126 C121 C122 C123 0.1(7) . . . . ? Si1 C121 C122 C123 176.0(4) . . . . ? C121 C122 C123 C124 -0.4(8) . . . . ? C122 C123 C124 C125 0.2(9) . . . . ? C123 C124 C125 C126 0.4(8) . . . . ? C124 C125 C126 C121 -0.7(7) . . . . ? C122 C121 C126 C125 0.5(6) . . . . ? Si1 C121 C126 C125 -175.4(4) . . . . ? C136 C131 C132 C133 -0.7(6) . . . . ? Si1 C131 C132 C133 175.1(3) . . . . ? C131 C132 C133 C134 0.4(7) . . . . ? C132 C133 C134 C135 1.0(7) . . . . ? C133 C134 C135 C136 -2.0(7) . . . . ? C134 C135 C136 C131 1.8(6) . . . . ? C132 C131 C136 C135 -0.4(5) . . . . ? Si1 C131 C136 C135 -176.1(3) . . . . ? C316 C311 C312 C313 -0.5(7) . . . . ? Si3 C311 C312 C313 179.5(4) . . . . ? C311 C312 C313 C314 0.1(9) . . . . ? C312 C313 C314 C315 0.7(9) . . . . ? C313 C314 C315 C316 -0.9(9) . . . . ? C312 C311 C316 C315 0.2(8) . . . . ? Si3 C311 C316 C315 -179.8(4) . . . . ? C314 C315 C316 C311 0.5(9) . . . . ? C326 C321 C322 C323 -0.4(6) . . . . ? Si3 C321 C322 C323 176.6(4) . . . . ? C321 C322 C323 C324 -0.1(7) . . . . ? C322 C323 C324 C325 0.9(8) . . . . ? C323 C324 C325 C326 -1.1(9) . . . . ? C324 C325 C326 C321 0.5(9) . . . . ? C322 C321 C326 C325 0.3(7) . . . . ? Si3 C321 C326 C325 -176.7(4) . . . . ? C136 C131 Si1 C2 -8.2(4) . . . . ? C132 C131 Si1 C2 176.2(3) . . . . ? C136 C131 Si1 C121 109.8(3) . . . . ? C132 C131 Si1 C121 -65.8(3) . . . . ? C136 C131 Si1 C111 -130.0(3) . . . . ? C132 C131 Si1 C111 54.5(3) . . . . ? C1 C2 Si1 C131 -144.5(3) . . . . ? C3 C2 Si1 C131 68.1(3) . . . . ? Ru2 C2 Si1 C131 -61.1(3) . . . . ? C1 C2 Si1 C121 94.9(3) . . . . ? C3 C2 Si1 C121 -52.5(3) . . . . ? Ru2 C2 Si1 C121 178.3(2) . . . . ? C1 C2 Si1 C111 -23.4(3) . . . . ? C3 C2 Si1 C111 -170.8(3) . . . . ? Ru2 C2 Si1 C111 60.0(3) . . . . ? C122 C121 Si1 C131 -159.1(3) . . . . ? C126 C121 Si1 C131 16.5(4) . . . . ? C122 C121 Si1 C2 -34.9(4) . . . . ? C126 C121 Si1 C2 140.7(3) . . . . ? C122 C121 Si1 C111 82.3(4) . . . . ? C126 C121 Si1 C111 -102.1(3) . . . . ? C116 C111 Si1 C131 -162.1(3) . . . . ? C112 C111 Si1 C131 19.9(3) . . . . ? C116 C111 Si1 C2 72.4(3) . . . . ? C112 C111 Si1 C2 -105.6(3) . . . . ? C116 C111 Si1 C121 -42.3(3) . . . . ? C112 C111 Si1 C121 139.6(3) . . . . ? C6 C7 Si3 C311 83.1(4) . . . . ? C6 C7 Si3 C19 -35.9(4) . . . . ? C6 C7 Si3 C321 -156.0(4) . . . . ? C316 C311 Si3 C7 156.5(4) . . . . ? C312 C311 Si3 C7 -23.5(4) . . . . ? C316 C311 Si3 C19 -86.4(4) . . . . ? C312 C311 Si3 C19 93.6(4) . . . . ? C316 C311 Si3 C321 35.8(4) . . . . ? C312 C311 Si3 C321 -144.2(4) . . . . ? C18 C19 Si3 C7 -45.9(3) . . . . ? C14 C19 Si3 C7 119.3(3) . . . . ? Ru2 C19 Si3 C7 35.9(2) . . . . ? C18 C19 Si3 C311 -164.8(3) . . . . ? C14 C19 Si3 C311 0.4(4) . . . . ? Ru2 C19 Si3 C311 -83.0(2) . . . . ? C18 C19 Si3 C321 73.4(3) . . . . ? C14 C19 Si3 C321 -121.4(3) . . . . ? Ru2 C19 Si3 C321 155.24(18) . . . . ? C322 C321 Si3 C7 -67.8(4) . . . . ? C326 C321 Si3 C7 109.1(4) . . . . ? C322 C321 Si3 C311 53.0(4) . . . . ? C326 C321 Si3 C311 -130.1(4) . . . . ? C322 C321 Si3 C19 174.7(3) . . . . ? C326 C321 Si3 C19 -8.4(4) . . . . ? data_mrvian27 _database_code_depnum_ccdc_archive 'CCDC 903659' #TrackingRef 'compound 9.cif' _audit_creation_date 2012-12-14T12:16:10-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.4 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common 'compound 9' _chemical_formula_moiety 'C16 H12 O9 Ru3 Si1' _chemical_formula_sum 'C52 H46 Cl4 O5 Ru3 Si3' _chemical_formula_weight 1280.17 _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 9.9128(2) _cell_length_b 15.4684(4) _cell_length_c 17.7928(4) _cell_angle_alpha 72.928(2) _cell_angle_beta 84.8990(10) _cell_angle_gamma 86.6140(10) _cell_volume 2596.16(10) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 600 _cell_measurement_theta_min 1 _cell_measurement_theta_max 14 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 1.638 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1280 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.183 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.7916 _exptl_absorpt_correction_T_max 0.8208 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 9 _diffrn_orient_matrix_type 'by Bruker AXS Collect from scalepack cell' _diffrn_orient_matrix_ub_11 -0.885726E-1 _diffrn_orient_matrix_ub_12 -0.267926E-1 _diffrn_orient_matrix_ub_13 -0.18663E-2 _diffrn_orient_matrix_ub_21 0.435197E-1 _diffrn_orient_matrix_ub_22 -0.316786E-1 _diffrn_orient_matrix_ub_23 -0.379616E-1 _diffrn_orient_matrix_ub_31 0.230439E-1 _diffrn_orient_matrix_ub_32 -0.53457E-1 _diffrn_orient_matrix_ub_33 0.450736E-1 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.0804 _diffrn_reflns_av_unetI/netI 0.0987 _diffrn_reflns_number 42836 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.07 _diffrn_reflns_theta_max 27.54 _diffrn_reflns_theta_full 25 _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.989 _reflns_number_total 11821 _reflns_number_gt 7814 _reflns_threshold_expression >2\s(I) _diffrn_reflns_reduction_process ; Scaled and merged with Sortav R.H. Blessing, (1987) Cryst. Rev. 1, 3-58 R.H. Blessing, (1989) J. Appl. Cryst. 22, 396-397 ; #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _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^)+(0.0935P)^2^+0.9867P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 11821 _refine_ls_number_parameters 610 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.1086 _refine_ls_R_factor_gt 0.0606 _refine_ls_wR_factor_ref 0.1784 _refine_ls_wR_factor_gt 0.1512 _refine_ls_goodness_of_fit_ref 1.078 _refine_ls_restrained_S_all 1.082 _refine_ls_shift/su_max 0.026 _refine_ls_shift/su_mean 0 _refine_diff_density_max 2.007 _refine_diff_density_min -1.079 _refine_diff_density_rms 0.215 #----------------------------------------------------------------------------# # 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' O O 0.0106 0.006 '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' Si Si 0.0817 0.0704 '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' 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 C15 C 0.7608(9) 0.7110(5) 0.9443(5) 0.062(2) Uani 1 1 d . . . H15B H 0.7687 0.702 0.8929 0.094 Uiso 1 1 calc R . . H15C H 0.6996 0.6683 0.9787 0.094 Uiso 1 1 calc R . . H15A H 0.8482 0.7023 0.9652 0.094 Uiso 1 1 calc R . . C16 C 0.5160(6) 0.8397(5) 0.9098(4) 0.0420(17) Uani 1 1 d . . . H16C H 0.4881 0.9025 0.8947 0.063 Uiso 1 1 calc R . . H16B H 0.4587 0.8073 0.9543 0.063 Uiso 1 1 calc R . . H16A H 0.5092 0.8153 0.8666 0.063 Uiso 1 1 calc R . . C17 C 0.7026(7) 0.8521(5) 1.0323(4) 0.0428(18) Uani 1 1 d . . . H17C H 0.7952 0.8479 1.0452 0.064 Uiso 1 1 calc R . . H17A H 0.6507 0.8089 1.0728 0.064 Uiso 1 1 calc R . . H17B H 0.666 0.912 1.0283 0.064 Uiso 1 1 calc R . . C4 C 1.1822(6) 0.8644(4) 0.8226(3) 0.0269(13) Uani 1 1 d . . . C5 C 1.2311(5) 0.9533(4) 0.8073(3) 0.0276(14) Uani 1 1 d . . . H5 H 1.279 0.9805 0.7596 0.033 Uiso 1 1 calc R . . C6 C 1.2067(6) 0.9994(5) 0.8645(3) 0.0289(14) Uani 1 1 d . . . C7 C 1.1378(6) 0.9587(5) 0.9385(4) 0.0312(15) Uani 1 1 d . . . C8 C 1.0966(6) 0.8705(5) 0.9564(3) 0.0279(14) Uani 1 1 d . . . C9 C 1.1173(6) 0.8250(5) 0.8983(3) 0.0295(14) Uani 1 1 d . . . H9 H 1.087 0.7664 0.9101 0.035 Uiso 1 1 calc R . . C19 C 1.1223(7) 1.0384(5) 0.6356(3) 0.0314(14) Uani 1 1 d . . . C18 C 0.8797(6) 1.0073(5) 0.5836(4) 0.0340(15) Uani 1 1 d . . . C11 C 1.0156(6) 0.8416(4) 0.6938(3) 0.0284(14) Uani 1 1 d . . . H11 H 1.0136 0.8249 0.6448 0.034 Uiso 1 1 calc R . . C12 C 0.8898(6) 1.1172(4) 0.6849(3) 0.0268(13) Uani 1 1 d . . . H14 H 0.8391 1.1536 0.6409 0.032 Uiso 1 1 calc R . . C1 C 0.8689(5) 0.8924(4) 0.7914(3) 0.0243(13) Uani 1 1 d . . . C10 C 0.8877(6) 0.8472(4) 0.7320(3) 0.0285(14) Uani 1 1 d . . . H10 H 0.8087 0.8273 0.713 0.034 Uiso 1 1 calc R . . C2 C 0.7953(6) 0.9084(4) 0.8547(3) 0.0248(13) Uani 1 1 d . . . C14 C 0.9617(6) 1.0997(4) 0.8182(3) 0.0243(13) Uani 1 1 d . . . C31 C 0.6050(7) 1.0650(4) 0.7417(4) 0.0313(14) Uani 1 1 d . . . C32 C 0.6752(6) 1.0731(5) 0.8796(4) 0.0343(15) Uani 1 1 d . . . C13 C 0.9139(6) 1.1586(4) 0.7422(3) 0.0254(13) Uani 1 1 d . . . C20B C 1.0673(6) 1.3269(5) 0.7204(4) 0.0349(15) Uani 1 1 d . . . C21B C 1.1794(7) 1.2720(5) 0.7067(5) 0.0480(19) Uani 1 1 d . . . H21B H 1.1668 1.214 0.704 0.058 Uiso 1 1 calc R . . C22B C 1.3087(8) 1.3047(6) 0.6973(6) 0.068(3) Uani 1 1 d . . . H22B H 1.3827 1.2681 0.6886 0.081 Uiso 1 1 calc R . . C23B C 1.3291(8) 1.3897(6) 0.7006(5) 0.057(2) Uani 1 1 d . . . H23B H 1.4165 1.4111 0.6929 0.069 Uiso 1 1 calc R . . C24B C 1.2224(7) 1.4435(5) 0.7151(4) 0.0481(19) Uani 1 1 d . . . H24B H 1.2364 1.5011 0.7185 0.058 Uiso 1 1 calc R . . C25B C 1.0937(7) 1.4115(5) 0.7244(4) 0.0395(16) Uani 1 1 d . . . H25B H 1.0213 1.4489 0.7339 0.047 Uiso 1 1 calc R . . C20D C 0.7910(6) 1.3132(4) 0.8160(4) 0.0311(14) Uani 1 1 d . . . C21D C 0.8532(7) 1.3299(5) 0.8780(4) 0.0386(16) Uani 1 1 d . . . H21D H 0.9468 1.3223 0.8797 0.046 Uiso 1 1 calc R . . C22D C 0.7769(8) 1.3575(5) 0.9369(4) 0.0454(18) Uani 1 1 d . . . H22D H 0.8207 1.3697 0.9766 0.055 Uiso 1 1 calc R . . C23D C 0.6420(8) 1.3668(5) 0.9375(4) 0.051(2) Uani 1 1 d . . . H23D H 0.5927 1.3858 0.9771 0.062 Uiso 1 1 calc R . . C24D C 0.5751(8) 1.3481(5) 0.8786(5) 0.054(2) Uani 1 1 d . . . H24D H 0.4811 1.3533 0.8793 0.065 Uiso 1 1 calc R . . C25D C 0.6492(7) 1.3218(5) 0.8195(4) 0.0427(17) Uani 1 1 d . . . H25D H 0.6038 1.3094 0.7806 0.051 Uiso 1 1 calc R . . C20C C 0.8046(6) 1.3400(4) 0.6389(4) 0.0337(15) Uani 1 1 d . . . C21C C 0.8539(9) 1.4173(6) 0.5853(5) 0.066(3) Uani 1 1 d . . . H21C H 0.9319 1.4419 0.5946 0.079 Uiso 1 1 calc R . . C22C C 0.7874(11) 1.4591(7) 0.5167(6) 0.088(4) Uani 1 1 d . . . H22C H 0.8248 1.5092 0.4795 0.105 Uiso 1 1 calc R . . C23C C 0.6709(9) 1.4278(7) 0.5043(5) 0.068(3) Uani 1 1 d . . . H23C H 0.626 1.4579 0.4597 0.082 Uiso 1 1 calc R . . C24C C 0.6185(8) 1.3533(6) 0.5558(4) 0.0481(19) Uani 1 1 d . . . H24C H 0.5378 1.3317 0.5467 0.058 Uiso 1 1 calc R . . C25C C 0.6847(7) 1.3086(5) 0.6228(4) 0.0418(17) Uani 1 1 d . . . H25C H 0.6482 1.2565 0.6576 0.05 Uiso 1 1 calc R . . C20A C 1.3261(6) 0.8328(4) 0.6701(4) 0.0320(15) Uani 1 1 d . . . C21A C 1.4424(7) 0.8717(5) 0.6821(4) 0.0403(17) Uani 1 1 d . . . H21A H 1.4494 0.8821 0.7305 0.048 Uiso 1 1 calc R . . C22A C 1.5475(7) 0.8951(6) 0.6248(5) 0.051(2) Uani 1 1 d . . . H22A H 1.6241 0.9203 0.635 0.061 Uiso 1 1 calc R . . C23A C 1.5395(8) 0.8814(6) 0.5539(4) 0.054(2) Uani 1 1 d . . . H23A H 1.61 0.8986 0.5151 0.065 Uiso 1 1 calc R . . C24A C 1.4292(8) 0.8427(6) 0.5384(4) 0.056(2) Uani 1 1 d . . . H24A H 1.4253 0.8324 0.4898 0.067 Uiso 1 1 calc R . . C25A C 1.3214(8) 0.8185(5) 0.5966(4) 0.0474(19) Uani 1 1 d . . . H25A H 1.2457 0.7926 0.5858 0.057 Uiso 1 1 calc R . . C20 C 1.1727(7) 0.6829(5) 0.7992(4) 0.0355(16) Uani 1 1 d . . . C21 C 1.2885(9) 0.6356(5) 0.8305(5) 0.053(2) Uani 1 1 d . . . H21 H 1.3706 0.6645 0.8184 0.064 Uiso 1 1 calc R . . C22 C 1.2864(13) 0.5478(6) 0.8788(6) 0.076(3) Uani 1 1 d . . . H22 H 1.3655 0.5183 0.8992 0.091 Uiso 1 1 calc R . . C23 C 1.1649(14) 0.5043(6) 0.8962(5) 0.083(3) Uani 1 1 d . . . H23 H 1.1622 0.445 0.9288 0.099 Uiso 1 1 calc R . . C24 C 1.0474(12) 0.5477(6) 0.8660(5) 0.071(3) Uani 1 1 d . . . H24 H 0.9649 0.5191 0.8779 0.085 Uiso 1 1 calc R . . C25 C 1.0570(8) 0.6358(5) 0.8171(4) 0.0466(19) Uani 1 1 d . . . H25 H 0.9788 0.6646 0.7949 0.056 Uiso 1 1 calc R . . O19 O 1.2221(5) 1.0695(4) 0.6105(3) 0.0452(12) Uani 1 1 d . . . O18 O 0.8392(5) 1.0195(4) 0.5231(3) 0.0516(14) Uani 1 1 d . . . O14 O 0.9898(4) 1.1325(3) 0.8700(2) 0.0298(10) Uani 1 1 d . . . O31 O 0.5050(5) 1.0782(4) 0.7125(3) 0.0537(14) Uani 1 1 d . . . O32 O 0.6217(5) 1.0931(4) 0.9309(3) 0.0513(14) Uani 1 1 d . . . Ru1 Ru 0.95208(4) 0.98823(3) 0.68149(3) 0.02289(12) Uani 1 1 d . . . Ru2 Ru 1.00462(4) 0.95368(3) 0.83885(2) 0.02135(12) Uani 1 1 d . . . Ru3 Ru 0.76833(4) 1.04342(3) 0.79226(3) 0.02253(12) Uani 1 1 d . . . Si3 Si 0.89171(17) 1.28303(12) 0.73201(9) 0.0259(4) Uani 1 1 d . . . Si2 Si 1.17640(17) 0.80649(12) 0.74302(9) 0.0276(4) Uani 1 1 d . . . Si1 Si 0.69447(17) 0.82797(12) 0.93676(10) 0.0279(4) Uani 1 1 d . . . H8 H 1.060(5) 0.839(4) 1.006(3) 0.014(14) Uiso 1 1 d . . . H6 H 1.226(6) 1.055(4) 0.857(3) 0.019(16) Uiso 1 1 d . . . H7 H 1.120(7) 0.988(5) 0.971(4) 0.032(19) Uiso 1 1 d . . . C51A C 0.653(3) 0.5507(18) 0.7174(16) 0.167(15) Uiso 0.5 1 d PD A 1 H51A H 0.738 0.5452 0.6873 0.08 Uiso 0.5 1 d PR A 1 H51B H 0.6209 0.4906 0.7445 0.08 Uiso 0.5 1 d PR A 1 Cl1A Cl 0.6754(9) 0.6145(6) 0.7841(5) 0.126(3) Uiso 0.5 1 d PD A 1 Cl2A Cl 0.5379(11) 0.6160(8) 0.6556(6) 0.168(4) Uiso 0.5 1 d PD A 1 C51B C 0.714(6) 0.641(4) 0.6424(18) 0.59(10) Uiso 0.5 1 d PD . 2 H51C H 0.8086 0.6242 0.6321 0.08 Uiso 0.5 1 d PR . 2 H51D H 0.698 0.7042 0.6149 0.08 Uiso 0.5 1 d PR . 2 Cl1B Cl 0.681(3) 0.6000(19) 0.7488(15) 0.357(14) Uiso 0.5 1 d PD . 2 Cl2B Cl 0.615(5) 0.562(3) 0.615(2) 0.67 Uiso 0.5 1 d PD . 2 C50A C 0.021(2) 0.7236(18) 0.5221(13) 0.135(11) Uiso 0.5 1 d PD B 1 H50A H 0.0877 0.7688 0.518 0.08 Uiso 0.5 1 d PR B 1 H50B H 0.0392 0.6977 0.4786 0.08 Uiso 0.5 1 d PR B 1 Cl3A Cl 0.0205(9) 0.6385(6) 0.6183(5) 0.137(3) Uiso 0.5 1 d PD B 1 Cl4A Cl -0.1403(17) 0.7703(11) 0.5268(10) 0.272(8) Uiso 0.5 1 d PD B 1 C50B C -0.071(3) 0.664(3) 0.5577(19) 0.190(17) Uiso 0.5 1 d PD . 2 H50C H -0.0409 0.6028 0.5585 0.08 Uiso 0.5 1 d PR . 2 H50D H 0.0053 0.6966 0.5638 0.08 Uiso 0.5 1 d PR . 2 Cl3B Cl -0.196(5) 0.662(4) 0.6355(19) 0.711 Uiso 0.5 1 d PD . 2 Cl4B Cl -0.157(5) 0.717(4) 0.4711(18) 0.67 Uiso 0.5 1 d PD . 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 C15 0.064(5) 0.033(4) 0.076(6) -0.001(4) 0.024(5) -0.011(4) C16 0.024(3) 0.050(5) 0.050(4) -0.009(3) -0.005(3) -0.010(3) C17 0.035(4) 0.058(5) 0.034(4) -0.011(3) 0.004(3) -0.013(3) C4 0.019(3) 0.035(4) 0.024(3) -0.005(3) -0.002(2) 0.005(3) C5 0.014(3) 0.041(4) 0.025(3) -0.007(3) -0.001(2) 0.000(3) C6 0.024(3) 0.035(4) 0.030(3) -0.012(3) -0.003(2) -0.004(3) C7 0.020(3) 0.051(4) 0.025(3) -0.016(3) 0.002(2) 0.000(3) C8 0.018(3) 0.041(4) 0.022(3) -0.007(3) -0.004(2) 0.003(3) C9 0.025(3) 0.037(4) 0.024(3) -0.005(3) -0.004(2) 0.004(3) C19 0.033(3) 0.039(4) 0.027(3) -0.015(3) -0.002(3) -0.006(3) C18 0.031(3) 0.045(4) 0.028(3) -0.016(3) 0.006(3) -0.002(3) C11 0.030(3) 0.029(3) 0.025(3) -0.004(2) -0.005(2) 0.000(3) C12 0.027(3) 0.032(3) 0.020(3) -0.005(2) -0.003(2) -0.007(3) C1 0.017(3) 0.031(3) 0.022(3) -0.002(2) -0.002(2) -0.005(2) C10 0.026(3) 0.037(4) 0.027(3) -0.015(3) -0.007(2) 0.002(3) C2 0.017(3) 0.033(3) 0.025(3) -0.008(2) -0.002(2) -0.004(2) C14 0.020(3) 0.029(3) 0.024(3) -0.009(2) 0.001(2) -0.005(2) C31 0.033(3) 0.025(3) 0.039(3) -0.012(3) -0.006(3) -0.001(3) C32 0.023(3) 0.038(4) 0.039(4) -0.007(3) 0.000(3) 0.000(3) C13 0.022(3) 0.028(3) 0.026(3) -0.008(2) 0.005(2) -0.006(2) C20B 0.029(3) 0.039(4) 0.033(3) -0.006(3) 0.000(3) -0.004(3) C21B 0.037(4) 0.036(4) 0.066(5) -0.009(4) 0.008(4) -0.008(3) C22B 0.032(4) 0.052(6) 0.109(7) -0.008(5) -0.007(4) 0.001(4) C23B 0.033(4) 0.059(6) 0.077(6) -0.011(4) -0.009(4) -0.021(4) C24B 0.036(4) 0.047(5) 0.058(5) -0.007(4) -0.006(3) -0.016(3) C25B 0.036(4) 0.038(4) 0.048(4) -0.017(3) 0.000(3) -0.011(3) C20D 0.029(3) 0.028(3) 0.034(3) -0.005(3) -0.002(3) 0.004(3) C21D 0.039(4) 0.036(4) 0.036(4) -0.004(3) -0.003(3) 0.001(3) C22D 0.065(5) 0.035(4) 0.034(4) -0.008(3) 0.000(3) -0.002(4) C23D 0.056(5) 0.050(5) 0.045(4) -0.016(4) 0.016(4) 0.006(4) C24D 0.045(4) 0.050(5) 0.069(5) -0.027(4) 0.015(4) -0.001(4) C25D 0.036(4) 0.046(4) 0.048(4) -0.018(3) 0.003(3) 0.001(3) C20C 0.031(3) 0.033(4) 0.033(3) -0.007(3) 0.001(3) 0.002(3) C21C 0.058(5) 0.060(6) 0.064(5) 0.015(4) -0.025(4) -0.024(4) C22C 0.084(7) 0.074(7) 0.074(6) 0.038(5) -0.031(5) -0.029(6) C23C 0.062(6) 0.082(7) 0.049(5) 0.005(5) -0.021(4) -0.008(5) C24C 0.042(4) 0.057(5) 0.044(4) -0.008(4) -0.013(3) -0.006(4) C25C 0.037(4) 0.039(4) 0.044(4) -0.002(3) -0.008(3) -0.004(3) C20A 0.029(3) 0.034(4) 0.035(3) -0.013(3) 0.002(3) 0.003(3) C21A 0.030(3) 0.052(5) 0.039(4) -0.016(3) 0.001(3) 0.007(3) C22A 0.026(4) 0.066(5) 0.060(5) -0.020(4) 0.011(3) -0.011(3) C23A 0.047(5) 0.061(5) 0.041(4) -0.001(4) 0.016(4) 0.005(4) C24A 0.050(5) 0.087(6) 0.031(4) -0.020(4) 0.007(3) -0.005(4) C25A 0.038(4) 0.058(5) 0.047(4) -0.020(4) 0.004(3) -0.004(4) C20 0.043(4) 0.036(4) 0.030(3) -0.015(3) -0.007(3) 0.007(3) C21 0.060(5) 0.043(5) 0.062(5) -0.022(4) -0.023(4) 0.012(4) C22 0.118(9) 0.037(5) 0.074(6) -0.012(4) -0.047(6) 0.025(6) C23 0.150(11) 0.036(5) 0.057(6) -0.004(4) -0.018(6) 0.005(6) C24 0.102(8) 0.038(5) 0.066(6) -0.009(4) 0.011(5) -0.014(5) C25 0.054(5) 0.032(4) 0.052(4) -0.013(3) 0.009(4) -0.008(3) O19 0.027(2) 0.070(4) 0.038(3) -0.017(2) 0.013(2) -0.019(2) O18 0.041(3) 0.085(4) 0.032(3) -0.021(3) -0.007(2) 0.000(3) O14 0.030(2) 0.035(2) 0.029(2) -0.0164(19) -0.0052(18) 0.0014(19) O31 0.035(3) 0.055(3) 0.070(3) -0.011(3) -0.022(3) -0.005(2) O32 0.049(3) 0.063(4) 0.045(3) -0.027(3) 0.014(2) 0.005(3) Ru1 0.0194(2) 0.0306(3) 0.0198(2) -0.00937(19) 0.00071(17) -0.00164(19) Ru2 0.0169(2) 0.0270(3) 0.0201(2) -0.00734(18) 0.00072(17) -0.00087(18) Ru3 0.0169(2) 0.0271(3) 0.0230(2) -0.00708(19) 0.00116(17) -0.00096(19) Si3 0.0237(8) 0.0271(9) 0.0265(8) -0.0076(7) 0.0008(6) -0.0032(7) Si2 0.0250(8) 0.0314(10) 0.0264(8) -0.0099(7) 0.0012(7) 0.0031(7) Si1 0.0232(8) 0.0315(10) 0.0262(8) -0.0046(7) 0.0024(7) -0.0040(7) #----------------------------------------------------------------------------# # 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 C15 Si1 1.859(8) . ? C15 H15B 0.96 . ? C15 H15C 0.96 . ? C15 H15A 0.96 . ? C16 Si1 1.858(7) . ? C16 H16C 0.96 . ? C16 H16B 0.96 . ? C16 H16A 0.96 . ? C17 Si1 1.853(7) . ? C17 H17C 0.96 . ? C17 H17A 0.96 . ? C17 H17B 0.96 . ? C4 C9 1.418(8) . ? C4 C5 1.427(9) . ? C4 Si2 1.891(6) . ? C4 Ru2 2.224(6) . ? C5 C6 1.401(9) . ? C5 Ru2 2.265(5) . ? C5 H5 0.93 . ? C6 C7 1.414(9) . ? C6 Ru2 2.290(6) . ? C6 H6 0.87(6) . ? C7 C8 1.385(10) . ? C7 Ru2 2.324(6) . ? C7 H7 0.83(7) . ? C8 C9 1.406(9) . ? C8 Ru2 2.342(6) . ? C8 H8 0.92(5) . ? C9 Ru2 2.245(6) . ? C9 H9 0.93 . ? C19 O19 1.123(7) . ? C19 Ru1 1.911(6) . ? C18 O18 1.142(8) . ? C18 Ru1 1.880(7) . ? C11 C10 1.395(8) . ? C11 Si2 1.863(6) . ? C11 Ru1 2.271(6) . ? C11 H11 0.98 . ? C12 C13 1.397(8) . ? C12 Ru1 2.069(6) . ? C12 Ru3 2.208(6) . ? C12 H14 0.98 . ? C1 C2 1.364(8) . ? C1 C10 1.423(8) . ? C1 Ru2 2.060(6) . ? C1 Ru1 2.203(5) . ? C1 Ru3 2.488(6) . ? C10 Ru1 2.211(6) . ? C10 H10 0.98 . ? C2 Si1 1.870(6) . ? C2 Ru3 2.072(6) . ? C2 Ru2 2.197(6) . ? C14 O14 1.233(7) . ? C14 C13 1.491(8) . ? C14 Ru2 2.202(6) . ? C14 Ru3 2.289(6) . ? C31 O31 1.140(8) . ? C31 Ru3 1.887(7) . ? C32 O32 1.127(7) . ? C32 Ru3 1.895(7) . ? C13 Si3 1.881(6) . ? C13 Ru3 2.279(6) . ? C20B C25B 1.373(10) . ? C20B C21B 1.406(10) . ? C20B Si3 1.877(7) . ? C21B C22B 1.384(11) . ? C21B H21B 0.93 . ? C22B C23B 1.360(12) . ? C22B H22B 0.93 . ? C23B C24B 1.360(11) . ? C23B H23B 0.93 . ? C24B C25B 1.374(10) . ? C24B H24B 0.93 . ? C25B H25B 0.93 . ? C20D C25D 1.401(9) . ? C20D C21D 1.403(9) . ? C20D Si3 1.881(6) . ? C21D C22D 1.393(10) . ? C21D H21D 0.93 . ? C22D C23D 1.336(11) . ? C22D H22D 0.93 . ? C23D C24D 1.395(12) . ? C23D H23D 0.93 . ? C24D C25D 1.373(10) . ? C24D H24D 0.93 . ? C25D H25D 0.93 . ? C20C C21C 1.376(10) . ? C20C C25C 1.393(10) . ? C20C Si3 1.891(7) . ? C21C C22C 1.405(12) . ? C21C H21C 0.93 . ? C22C C23C 1.338(13) . ? C22C H22C 0.93 . ? C23C C24C 1.344(11) . ? C23C H23C 0.93 . ? C24C C25C 1.389(10) . ? C24C H24C 0.93 . ? C25C H25C 0.93 . ? C20A C21A 1.392(10) . ? C20A C25A 1.395(10) . ? C20A Si2 1.863(6) . ? C21A C22A 1.377(9) . ? C21A H21A 0.93 . ? C22A C23A 1.349(11) . ? C22A H22A 0.93 . ? C23A C24A 1.362(12) . ? C23A H23A 0.93 . ? C24A C25A 1.406(10) . ? C24A H24A 0.93 . ? C25A H25A 0.93 . ? C20 C25 1.358(10) . ? C20 C21 1.393(10) . ? C20 Si2 1.880(7) . ? C21 C22 1.378(12) . ? C21 H21 0.93 . ? C22 C23 1.381(16) . ? C22 H22 0.93 . ? C23 C24 1.380(15) . ? C23 H23 0.93 . ? C24 C25 1.389(11) . ? C24 H24 0.93 . ? C25 H25 0.93 . ? Ru1 Ru2 2.7828(6) . ? Ru1 Ru3 2.8454(6) . ? Ru2 Ru3 2.7178(6) . ? C51A Cl2A 1.723(18) . ? C51A Cl1A 1.786(18) . ? C51A H51A 0.97 . ? C51A H51B 0.97 . ? C51B Cl3B 0.95(8) 1_655 ? C51B Cl2B 1.81(2) . ? C51B Cl1B 1.817(19) . ? C51B H51A 1.4763 . ? C51B H51C 0.97 . ? C51B H51D 0.97 . ? Cl1B Cl3B 2.24(4) 1_655 ? Cl1B H51A 1.6159 . ? Cl2B H51A 1.8069 . ? C50A Cl4A 1.723(17) . ? C50A Cl3A 1.827(17) . ? C50A H50A 0.97 . ? C50A H50B 0.97 . ? C50A H50D 0.7457 . ? Cl3A H50C 1.519 . ? Cl3A H50D 1.1262 . ? C50B Cl3B 1.765(19) . ? C50B Cl4B 1.780(19) . ? C50B H50C 0.97 . ? C50B H50D 0.97 . ? Cl3B C51B 0.95(8) 1_455 ? Cl3B Cl1B 2.24(4) 1_455 ? 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 Si1 C15 H15B 109.5 . . ? Si1 C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? Si1 C15 H15A 109.5 . . ? H15B C15 H15A 109.5 . . ? H15C C15 H15A 109.5 . . ? Si1 C16 H16C 109.5 . . ? Si1 C16 H16B 109.5 . . ? H16C C16 H16B 109.5 . . ? Si1 C16 H16A 109.5 . . ? H16C C16 H16A 109.5 . . ? H16B C16 H16A 109.5 . . ? Si1 C17 H17C 109.5 . . ? Si1 C17 H17A 109.5 . . ? H17C C17 H17A 109.5 . . ? Si1 C17 H17B 109.5 . . ? H17C C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C9 C4 C5 117.0(5) . . ? C9 C4 Si2 119.4(5) . . ? C5 C4 Si2 122.9(4) . . ? C9 C4 Ru2 72.3(3) . . ? C5 C4 Ru2 73.0(3) . . ? Si2 C4 Ru2 116.7(3) . . ? C6 C5 C4 119.7(5) . . ? C6 C5 Ru2 73.0(3) . . ? C4 C5 Ru2 69.9(3) . . ? C6 C5 H5 120.1 . . ? C4 C5 H5 120.1 . . ? Ru2 C5 H5 129.3 . . ? C5 C6 C7 121.4(6) . . ? C5 C6 Ru2 71.1(3) . . ? C7 C6 Ru2 73.5(4) . . ? C5 C6 H6 124(4) . . ? C7 C6 H6 114(4) . . ? Ru2 C6 H6 124(4) . . ? C8 C7 C6 119.8(6) . . ? C8 C7 Ru2 73.4(4) . . ? C6 C7 Ru2 70.8(4) . . ? C8 C7 H7 120(5) . . ? C6 C7 H7 121(5) . . ? Ru2 C7 H7 126(5) . . ? C7 C8 C9 118.8(6) . . ? C7 C8 Ru2 72.0(4) . . ? C9 C8 Ru2 68.4(3) . . ? C7 C8 H8 123(3) . . ? C9 C8 H8 118(3) . . ? Ru2 C8 H8 134(3) . . ? C8 C9 C4 123.0(6) . . ? C8 C9 Ru2 75.9(4) . . ? C4 C9 Ru2 70.7(3) . . ? C8 C9 H9 118.5 . . ? C4 C9 H9 118.5 . . ? Ru2 C9 H9 126.9 . . ? O19 C19 Ru1 177.6(6) . . ? O18 C18 Ru1 178.1(6) . . ? C10 C11 Si2 125.6(4) . . ? C10 C11 Ru1 69.5(4) . . ? Si2 C11 Ru1 113.0(3) . . ? C10 C11 H11 113.6 . . ? Si2 C11 H11 113.6 . . ? Ru1 C11 H11 113.6 . . ? C13 C12 Ru1 127.3(4) . . ? C13 C12 Ru3 74.6(3) . . ? Ru1 C12 Ru3 83.3(2) . . ? C13 C12 H14 116.4 . . ? Ru1 C12 H14 116.4 . . ? Ru3 C12 H14 116.4 . . ? C2 C1 C10 150.4(6) . . ? C2 C1 Ru2 76.9(4) . . ? C10 C1 Ru2 131.2(4) . . ? C2 C1 Ru1 130.1(5) . . ? C10 C1 Ru1 71.5(3) . . ? Ru2 C1 Ru1 81.4(2) . . ? C2 C1 Ru3 56.4(3) . . ? C10 C1 Ru3 132.8(4) . . ? Ru2 C1 Ru3 72.70(19) . . ? Ru1 C1 Ru3 74.40(18) . . ? C11 C10 C1 120.2(6) . . ? C11 C10 Ru1 74.2(4) . . ? C1 C10 Ru1 70.9(3) . . ? C11 C10 H10 119.6 . . ? C1 C10 H10 119.6 . . ? Ru1 C10 H10 119.6 . . ? C1 C2 Si1 129.0(5) . . ? C1 C2 Ru3 90.4(4) . . ? Si1 C2 Ru3 134.0(3) . . ? C1 C2 Ru2 65.9(3) . . ? Si1 C2 Ru2 134.0(3) . . ? Ru3 C2 Ru2 79.0(2) . . ? O14 C14 C13 120.9(5) . . ? O14 C14 Ru2 116.8(4) . . ? C13 C14 Ru2 122.0(4) . . ? O14 C14 Ru3 133.6(4) . . ? C13 C14 Ru3 70.6(3) . . ? Ru2 C14 Ru3 74.47(19) . . ? O31 C31 Ru3 178.6(6) . . ? O32 C32 Ru3 178.0(6) . . ? C12 C13 C14 117.7(5) . . ? C12 C13 Si3 125.7(5) . . ? C14 C13 Si3 116.6(4) . . ? C12 C13 Ru3 69.1(3) . . ? C14 C13 Ru3 71.3(3) . . ? Si3 C13 Ru3 131.0(3) . . ? C25B C20B C21B 116.9(6) . . ? C25B C20B Si3 123.3(5) . . ? C21B C20B Si3 119.8(5) . . ? C22B C21B C20B 119.8(8) . . ? C22B C21B H21B 120.1 . . ? C20B C21B H21B 120.1 . . ? C23B C22B C21B 120.9(8) . . ? C23B C22B H22B 119.5 . . ? C21B C22B H22B 119.5 . . ? C22B C23B C24B 120.4(7) . . ? C22B C23B H23B 119.8 . . ? C24B C23B H23B 119.8 . . ? C23B C24B C25B 119.0(8) . . ? C23B C24B H24B 120.5 . . ? C25B C24B H24B 120.5 . . ? C20B C25B C24B 123.0(7) . . ? C20B C25B H25B 118.5 . . ? C24B C25B H25B 118.5 . . ? C25D C20D C21D 116.2(6) . . ? C25D C20D Si3 121.8(5) . . ? C21D C20D Si3 122.1(5) . . ? C22D C21D C20D 120.9(7) . . ? C22D C21D H21D 119.5 . . ? C20D C21D H21D 119.5 . . ? C23D C22D C21D 121.2(7) . . ? C23D C22D H22D 119.4 . . ? C21D C22D H22D 119.4 . . ? C22D C23D C24D 120.0(7) . . ? C22D C23D H23D 120 . . ? C24D C23D H23D 120 . . ? C25D C24D C23D 119.4(7) . . ? C25D C24D H24D 120.3 . . ? C23D C24D H24D 120.3 . . ? C24D C25D C20D 122.2(7) . . ? C24D C25D H25D 118.9 . . ? C20D C25D H25D 118.9 . . ? C21C C20C C25C 116.7(6) . . ? C21C C20C Si3 121.2(6) . . ? C25C C20C Si3 122.0(5) . . ? C20C C21C C22C 120.5(8) . . ? C20C C21C H21C 119.8 . . ? C22C C21C H21C 119.8 . . ? C23C C22C C21C 120.8(8) . . ? C23C C22C H22C 119.6 . . ? C21C C22C H22C 119.6 . . ? C22C C23C C24C 120.4(8) . . ? C22C C23C H23C 119.8 . . ? C24C C23C H23C 119.8 . . ? C23C C24C C25C 120.1(8) . . ? C23C C24C H24C 120 . . ? C25C C24C H24C 120 . . ? C24C C25C C20C 121.5(7) . . ? C24C C25C H25C 119.3 . . ? C20C C25C H25C 119.3 . . ? C21A C20A C25A 116.4(6) . . ? C21A C20A Si2 124.0(5) . . ? C25A C20A Si2 119.5(5) . . ? C22A C21A C20A 122.2(7) . . ? C22A C21A H21A 118.9 . . ? C20A C21A H21A 118.9 . . ? C23A C22A C21A 120.2(7) . . ? C23A C22A H22A 119.9 . . ? C21A C22A H22A 119.9 . . ? C22A C23A C24A 120.7(7) . . ? C22A C23A H23A 119.6 . . ? C24A C23A H23A 119.6 . . ? C23A C24A C25A 119.6(7) . . ? C23A C24A H24A 120.2 . . ? C25A C24A H24A 120.2 . . ? C20A C25A C24A 120.9(7) . . ? C20A C25A H25A 119.5 . . ? C24A C25A H25A 119.5 . . ? C25 C20 C21 115.6(7) . . ? C25 C20 Si2 123.0(5) . . ? C21 C20 Si2 121.3(6) . . ? C22 C21 C20 122.8(9) . . ? C22 C21 H21 118.6 . . ? C20 C21 H21 118.6 . . ? C21 C22 C23 118.8(9) . . ? C21 C22 H22 120.6 . . ? C23 C22 H22 120.6 . . ? C24 C23 C22 120.8(9) . . ? C24 C23 H23 119.6 . . ? C22 C23 H23 119.6 . . ? C23 C24 C25 117.3(10) . . ? C23 C24 H24 121.3 . . ? C25 C24 H24 121.3 . . ? C20 C25 C24 124.6(8) . . ? C20 C25 H25 117.7 . . ? C24 C25 H25 117.7 . . ? C18 Ru1 C19 93.9(3) . . ? C18 Ru1 C12 91.4(3) . . ? C19 Ru1 C12 86.8(3) . . ? C18 Ru1 C1 123.3(3) . . ? C19 Ru1 C1 138.8(2) . . ? C12 Ru1 C1 107.4(2) . . ? C18 Ru1 C10 96.0(3) . . ? C19 Ru1 C10 132.3(3) . . ? C12 Ru1 C10 139.2(2) . . ? C1 Ru1 C10 37.6(2) . . ? C18 Ru1 C11 94.4(3) . . ? C19 Ru1 C11 96.5(3) . . ? C12 Ru1 C11 173.1(2) . . ? C1 Ru1 C11 66.2(2) . . ? C10 Ru1 C11 36.3(2) . . ? C18 Ru1 Ru2 168.26(19) . . ? C19 Ru1 Ru2 97.57(18) . . ? C12 Ru1 Ru2 86.61(16) . . ? C1 Ru1 Ru2 47.05(15) . . ? C10 Ru1 Ru2 78.25(15) . . ? C11 Ru1 Ru2 87.00(15) . . ? C18 Ru1 Ru3 112.57(19) . . ? C19 Ru1 Ru3 127.96(19) . . ? C12 Ru1 Ru3 50.43(15) . . ? C1 Ru1 Ru3 57.38(16) . . ? C10 Ru1 Ru3 90.19(15) . . ? C11 Ru1 Ru3 123.44(15) . . ? Ru2 Ru1 Ru3 57.735(15) . . ? C1 Ru2 C2 37.2(2) . . ? C1 Ru2 C14 113.3(2) . . ? C2 Ru2 C14 98.8(2) . . ? C1 Ru2 C4 96.0(2) . . ? C2 Ru2 C4 122.5(2) . . ? C14 Ru2 C4 137.0(2) . . ? C1 Ru2 C9 95.3(2) . . ? C2 Ru2 C9 101.4(2) . . ? C14 Ru2 C9 151.0(2) . . ? C4 Ru2 C9 37.0(2) . . ? C1 Ru2 C5 124.0(2) . . ? C2 Ru2 C5 158.5(2) . . ? C14 Ru2 C5 100.2(2) . . ? C4 Ru2 C5 37.1(2) . . ? C9 Ru2 C5 65.1(2) . . ? C1 Ru2 C6 159.8(2) . . ? C2 Ru2 C6 161.2(2) . . ? C14 Ru2 C6 78.9(2) . . ? C4 Ru2 C6 65.6(2) . . ? C9 Ru2 C6 75.2(2) . . ? C5 Ru2 C6 35.8(2) . . ? C1 Ru2 C7 152.6(2) . . ? C2 Ru2 C7 126.1(2) . . ? C14 Ru2 C7 87.8(2) . . ? C4 Ru2 C7 77.5(2) . . ? C9 Ru2 C7 63.4(2) . . ? C5 Ru2 C7 64.7(2) . . ? C6 Ru2 C7 35.7(2) . . ? C1 Ru2 C8 118.5(2) . . ? C2 Ru2 C8 103.3(2) . . ? C14 Ru2 C8 118.9(2) . . ? C4 Ru2 C8 65.8(2) . . ? C9 Ru2 C8 35.6(2) . . ? C5 Ru2 C8 75.9(2) . . ? C6 Ru2 C8 63.0(2) . . ? C7 Ru2 C8 34.5(2) . . ? C1 Ru2 Ru3 60.95(16) . . ? C2 Ru2 Ru3 48.45(15) . . ? C14 Ru2 Ru3 54.23(15) . . ? C4 Ru2 Ru3 151.60(15) . . ? C9 Ru2 Ru3 149.86(17) . . ? C5 Ru2 Ru3 142.63(15) . . ? C6 Ru2 Ru3 133.11(17) . . ? C7 Ru2 Ru3 130.70(16) . . ? C8 Ru2 Ru3 138.15(14) . . ? C1 Ru2 Ru1 51.53(15) . . ? C2 Ru2 Ru1 80.63(14) . . ? C14 Ru2 Ru1 84.53(15) . . ? C4 Ru2 Ru1 90.77(15) . . ? C9 Ru2 Ru1 119.09(15) . . ? C5 Ru2 Ru1 91.35(14) . . ? C6 Ru2 Ru1 117.41(15) . . ? C7 Ru2 Ru1 153.09(15) . . ? C8 Ru2 Ru1 154.65(15) . . ? Ru3 Ru2 Ru1 62.290(16) . . ? C31 Ru3 C32 88.9(3) . . ? C31 Ru3 C2 111.7(2) . . ? C32 Ru3 C2 93.1(3) . . ? C31 Ru3 C12 93.4(2) . . ? C32 Ru3 C12 135.8(3) . . ? C2 Ru3 C12 126.1(2) . . ? C31 Ru3 C13 112.2(2) . . ? C32 Ru3 C13 103.3(2) . . ? C2 Ru3 C13 133.1(2) . . ? C12 Ru3 C13 36.2(2) . . ? C31 Ru3 C14 148.4(2) . . ? C32 Ru3 C14 89.5(2) . . ? C2 Ru3 C14 99.9(2) . . ? C12 Ru3 C14 66.7(2) . . ? C13 Ru3 C14 38.1(2) . . ? C31 Ru3 C1 109.9(2) . . ? C32 Ru3 C1 126.3(2) . . ? C2 Ru3 C1 33.2(2) . . ? C12 Ru3 C1 94.2(2) . . ? C13 Ru3 C1 113.71(19) . . ? C14 Ru3 C1 96.3(2) . . ? C31 Ru3 Ru2 155.92(19) . . ? C32 Ru3 Ru2 108.53(19) . . ? C2 Ru3 Ru2 52.54(15) . . ? C12 Ru3 Ru2 85.60(16) . . ? C13 Ru3 Ru2 80.58(15) . . ? C14 Ru3 Ru2 51.31(15) . . ? C1 Ru3 Ru2 46.36(13) . . ? C31 Ru3 Ru1 102.64(19) . . ? C32 Ru3 Ru1 168.36(19) . . ? C2 Ru3 Ru1 81.18(15) . . ? C12 Ru3 Ru1 46.23(16) . . ? C13 Ru3 Ru1 74.09(14) . . ? C14 Ru3 Ru1 81.56(14) . . ? C1 Ru3 Ru1 48.22(12) . . ? Ru2 Ru3 Ru1 59.975(16) . . ? C20B Si3 C13 106.0(3) . . ? C20B Si3 C20D 109.9(3) . . ? C13 Si3 C20D 115.7(3) . . ? C20B Si3 C20C 108.6(3) . . ? C13 Si3 C20C 108.7(3) . . ? C20D Si3 C20C 107.8(3) . . ? C11 Si2 C20A 111.0(3) . . ? C11 Si2 C20 109.4(3) . . ? C20A Si2 C20 112.1(3) . . ? C11 Si2 C4 108.9(3) . . ? C20A Si2 C4 111.7(3) . . ? C20 Si2 C4 103.6(3) . . ? C17 Si1 C16 109.7(3) . . ? C17 Si1 C15 110.0(4) . . ? C16 Si1 C15 109.4(4) . . ? C17 Si1 C2 112.2(3) . . ? C16 Si1 C2 107.2(3) . . ? C15 Si1 C2 108.4(3) . . ? Cl2A C51A Cl1A 103.6(11) . . ? Cl2A C51A H51A 109.6 . . ? Cl1A C51A H51A 109.9 . . ? Cl2A C51A H51B 112.4 . . ? Cl1A C51A H51B 112.2 . . ? H51A C51A H51B 109 . . ? Cl3B C51B Cl2B 140(8) 1_655 . ? Cl3B C51B Cl1B 104(4) 1_655 . ? Cl2B C51B Cl1B 98.8(14) . . ? Cl3B C51B H51A 100.3 1_655 . ? Cl2B C51B H51A 65.8 . . ? Cl1B C51B H51A 57.7 . . ? Cl3B C51B H51C 36.3 1_655 . ? Cl2B C51B H51C 106.4 . . ? Cl1B C51B H51C 105.5 . . ? H51A C51B H51C 71.8 . . ? Cl3B C51B H51D 80 1_655 . ? Cl2B C51B H51D 115.4 . . ? Cl1B C51B H51D 120.1 . . ? H51A C51B H51D 177.7 . . ? H51C C51B H51D 109.3 . . ? C51B Cl1B Cl3B 24(2) . 1_655 ? C51B Cl1B H51A 50.5 . . ? Cl3B Cl1B H51A 55.9 1_655 . ? C51B Cl2B H51A 48.2 . . ? Cl4A C50A Cl3A 100.7(11) . . ? Cl4A C50A H50A 110.1 . . ? Cl3A C50A H50A 110.5 . . ? Cl4A C50A H50B 113.1 . . ? Cl3A C50A H50B 112.8 . . ? H50A C50A H50B 109.4 . . ? Cl4A C50A H50D 86.1 . . ? Cl3A C50A H50D 15.4 . . ? H50A C50A H50D 111.7 . . ? H50B C50A H50D 124.1 . . ? C50A Cl3A H50C 68.9 . . ? C50A Cl3A H50D 10.1 . . ? H50C Cl3A H50D 71.6 . . ? Cl3B C50B Cl4B 104.1(14) . . ? Cl3B C50B H50C 110.4 . . ? Cl4B C50B H50C 110.5 . . ? Cl3B C50B H50D 108.9 . . ? Cl4B C50B H50D 113.8 . . ? H50C C50B H50D 109 . . ? C51B Cl3B C50B 129(6) 1_455 . ? C51B Cl3B Cl1B 52(2) 1_455 1_455 ? C50B Cl3B Cl1B 156(4) . 1_455 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C9 C4 C5 C6 -3.7(8) . . . . ? Si2 C4 C5 C6 166.7(4) . . . . ? Ru2 C4 C5 C6 55.5(5) . . . . ? C9 C4 C5 Ru2 -59.2(5) . . . . ? Si2 C4 C5 Ru2 111.2(4) . . . . ? C4 C5 C6 C7 1.9(9) . . . . ? Ru2 C5 C6 C7 55.9(5) . . . . ? C4 C5 C6 Ru2 -54.0(5) . . . . ? C5 C6 C7 C8 2.0(9) . . . . ? Ru2 C6 C7 C8 56.8(5) . . . . ? C5 C6 C7 Ru2 -54.8(5) . . . . ? C6 C7 C8 C9 -3.9(9) . . . . ? Ru2 C7 C8 C9 51.7(5) . . . . ? C6 C7 C8 Ru2 -55.6(5) . . . . ? C7 C8 C9 C4 1.9(9) . . . . ? Ru2 C8 C9 C4 55.3(5) . . . . ? C7 C8 C9 Ru2 -53.4(5) . . . . ? C5 C4 C9 C8 1.9(8) . . . . ? Si2 C4 C9 C8 -168.9(4) . . . . ? Ru2 C4 C9 C8 -57.7(5) . . . . ? C5 C4 C9 Ru2 59.6(5) . . . . ? Si2 C4 C9 Ru2 -111.2(4) . . . . ? Si2 C11 C10 C1 48.2(8) . . . . ? Ru1 C11 C10 C1 -56.1(5) . . . . ? Si2 C11 C10 Ru1 104.3(5) . . . . ? C2 C1 C10 C11 -160.6(9) . . . . ? Ru2 C1 C10 C11 -2.2(9) . . . . ? Ru1 C1 C10 C11 57.7(5) . . . . ? Ru3 C1 C10 C11 103.5(6) . . . . ? C2 C1 C10 Ru1 141.7(11) . . . . ? Ru2 C1 C10 Ru1 -59.9(5) . . . . ? Ru3 C1 C10 Ru1 45.9(4) . . . . ? C10 C1 C2 Si1 35.5(14) . . . . ? Ru2 C1 C2 Si1 -128.1(5) . . . . ? Ru1 C1 C2 Si1 165.3(3) . . . . ? Ru3 C1 C2 Si1 154.2(6) . . . . ? C10 C1 C2 Ru3 -118.7(11) . . . . ? Ru2 C1 C2 Ru3 77.77(19) . . . . ? Ru1 C1 C2 Ru3 11.1(5) . . . . ? C10 C1 C2 Ru2 163.5(12) . . . . ? Ru1 C1 C2 Ru2 -66.7(4) . . . . ? Ru3 C1 C2 Ru2 -77.8(2) . . . . ? Ru1 C12 C13 C14 -14.8(8) . . . . ? Ru3 C12 C13 C14 54.1(5) . . . . ? Ru1 C12 C13 Si3 165.0(3) . . . . ? Ru3 C12 C13 Si3 -126.2(4) . . . . ? Ru1 C12 C13 Ru3 -68.9(4) . . . . ? O14 C14 C13 C12 177.2(5) . . . . ? Ru2 C14 C13 C12 3.2(7) . . . . ? Ru3 C14 C13 C12 -53.0(5) . . . . ? O14 C14 C13 Si3 -2.6(7) . . . . ? Ru2 C14 C13 Si3 -176.5(3) . . . . ? Ru3 C14 C13 Si3 127.2(4) . . . . ? O14 C14 C13 Ru3 -129.8(5) . . . . ? Ru2 C14 C13 Ru3 56.2(3) . . . . ? C25B C20B C21B C22B -0.6(11) . . . . ? Si3 C20B C21B C22B 179.3(7) . . . . ? C20B C21B C22B C23B -0.4(14) . . . . ? C21B C22B C23B C24B 1.5(14) . . . . ? C22B C23B C24B C25B -1.5(13) . . . . ? C21B C20B C25B C24B 0.5(11) . . . . ? Si3 C20B C25B C24B -179.3(6) . . . . ? C23B C24B C25B C20B 0.5(12) . . . . ? C25D C20D C21D C22D -2.9(10) . . . . ? Si3 C20D C21D C22D 176.0(5) . . . . ? C20D C21D C22D C23D 1.7(11) . . . . ? C21D C22D C23D C24D 0.5(12) . . . . ? C22D C23D C24D C25D -1.3(12) . . . . ? C23D C24D C25D C20D -0.1(12) . . . . ? C21D C20D C25D C24D 2.1(10) . . . . ? Si3 C20D C25D C24D -176.8(6) . . . . ? C25C C20C C21C C22C -2.3(13) . . . . ? Si3 C20C C21C C22C -179.5(8) . . . . ? C20C C21C C22C C23C 3.9(18) . . . . ? C21C C22C C23C C24C -2.9(18) . . . . ? C22C C23C C24C C25C 0.5(15) . . . . ? C23C C24C C25C C20C 1.0(12) . . . . ? C21C C20C C25C C24C 0.0(11) . . . . ? Si3 C20C C25C C24C 177.2(6) . . . . ? C25A C20A C21A C22A 0.1(10) . . . . ? Si2 C20A C21A C22A -176.0(6) . . . . ? C20A C21A C22A C23A 0.7(12) . . . . ? C21A C22A C23A C24A -1.4(13) . . . . ? C22A C23A C24A C25A 1.4(13) . . . . ? C21A C20A C25A C24A -0.1(11) . . . . ? Si2 C20A C25A C24A 176.1(6) . . . . ? C23A C24A C25A C20A -0.6(13) . . . . ? C25 C20 C21 C22 -2.1(11) . . . . ? Si2 C20 C21 C22 173.1(7) . . . . ? C20 C21 C22 C23 0.7(14) . . . . ? C21 C22 C23 C24 0.1(15) . . . . ? C22 C23 C24 C25 0.7(14) . . . . ? C21 C20 C25 C24 3.0(11) . . . . ? Si2 C20 C25 C24 -172.2(6) . . . . ? C23 C24 C25 C20 -2.4(13) . . . . ? O18 C18 Ru1 C19 9(19) . . . . ? O18 C18 Ru1 C12 96(19) . . . . ? O18 C18 Ru1 C1 -152(19) . . . . ? O18 C18 Ru1 C10 -124(19) . . . . ? O18 C18 Ru1 C11 -88(19) . . . . ? O18 C18 Ru1 Ru2 18E1(10) . . . . ? O18 C18 Ru1 Ru3 143(19) . . . . ? O19 C19 Ru1 C18 133(15) . . . . ? O19 C19 Ru1 C12 42(15) . . . . ? O19 C19 Ru1 C1 -71(15) . . . . ? O19 C19 Ru1 C10 -125(15) . . . . ? O19 C19 Ru1 C11 -132(15) . . . . ? O19 C19 Ru1 Ru2 -44(15) . . . . ? O19 C19 Ru1 Ru3 11(16) . . . . ? C13 C12 Ru1 C18 -176.6(5) . . . . ? Ru3 C12 Ru1 C18 118.6(2) . . . . ? C13 C12 Ru1 C19 -82.8(5) . . . . ? Ru3 C12 Ru1 C19 -147.6(2) . . . . ? C13 C12 Ru1 C1 57.8(6) . . . . ? Ru3 C12 Ru1 C1 -7.1(2) . . . . ? C13 C12 Ru1 C10 82.6(6) . . . . ? Ru3 C12 Ru1 C10 17.7(4) . . . . ? C13 C12 Ru1 C11 37(2) . . . . ? Ru3 C12 Ru1 C11 -28(2) . . . . ? C13 C12 Ru1 Ru2 15.0(5) . . . . ? Ru3 C12 Ru1 Ru2 -49.85(13) . . . . ? C13 C12 Ru1 Ru3 64.9(5) . . . . ? C2 C1 Ru1 C18 -106.7(6) . . . . ? C10 C1 Ru1 C18 49.7(4) . . . . ? Ru2 C1 Ru1 C18 -171.5(2) . . . . ? Ru3 C1 Ru1 C18 -97.2(3) . . . . ? C2 C1 Ru1 C19 102.6(6) . . . . ? C10 C1 Ru1 C19 -101.0(5) . . . . ? Ru2 C1 Ru1 C19 37.9(4) . . . . ? Ru3 C1 Ru1 C19 112.2(3) . . . . ? C2 C1 Ru1 C12 -3.1(6) . . . . ? C10 C1 Ru1 C12 153.3(3) . . . . ? Ru2 C1 Ru1 C12 -67.9(2) . . . . ? Ru3 C1 Ru1 C12 6.5(2) . . . . ? C2 C1 Ru1 C10 -156.4(7) . . . . ? Ru2 C1 Ru1 C10 138.8(4) . . . . ? Ru3 C1 Ru1 C10 -146.8(4) . . . . ? C2 C1 Ru1 C11 174.2(6) . . . . ? C10 C1 Ru1 C11 -29.4(3) . . . . ? Ru2 C1 Ru1 C11 109.4(2) . . . . ? Ru3 C1 Ru1 C11 -176.2(2) . . . . ? C2 C1 Ru1 Ru2 64.8(5) . . . . ? C10 C1 Ru1 Ru2 -138.8(4) . . . . ? Ru3 C1 Ru1 Ru2 74.33(16) . . . . ? C2 C1 Ru1 Ru3 -9.6(5) . . . . ? C10 C1 Ru1 Ru3 146.8(4) . . . . ? Ru2 C1 Ru1 Ru3 -74.33(16) . . . . ? C11 C10 Ru1 C18 89.2(4) . . . . ? C1 C10 Ru1 C18 -140.1(4) . . . . ? C11 C10 Ru1 C19 -11.5(5) . . . . ? C1 C10 Ru1 C19 119.1(4) . . . . ? C11 C10 Ru1 C12 -171.6(4) . . . . ? C1 C10 Ru1 C12 -41.0(5) . . . . ? C11 C10 Ru1 C1 -130.6(5) . . . . ? C1 C10 Ru1 C11 130.6(5) . . . . ? C11 C10 Ru1 Ru2 -101.1(3) . . . . ? C1 C10 Ru1 Ru2 29.5(3) . . . . ? C11 C10 Ru1 Ru3 -158.0(3) . . . . ? C1 C10 Ru1 Ru3 -27.4(3) . . . . ? C10 C11 Ru1 C18 -94.2(4) . . . . ? Si2 C11 Ru1 C18 144.8(3) . . . . ? C10 C11 Ru1 C19 171.4(4) . . . . ? Si2 C11 Ru1 C19 50.4(3) . . . . ? C10 C11 Ru1 C12 53(2) . . . . ? Si2 C11 Ru1 C12 -68.5(19) . . . . ? C10 C11 Ru1 C1 30.4(3) . . . . ? Si2 C11 Ru1 C1 -90.6(3) . . . . ? Si2 C11 Ru1 C10 -121.0(5) . . . . ? C10 C11 Ru1 Ru2 74.1(3) . . . . ? Si2 C11 Ru1 Ru2 -46.9(3) . . . . ? C10 C11 Ru1 Ru3 26.6(4) . . . . ? Si2 C11 Ru1 Ru3 -94.4(3) . . . . ? C10 C1 Ru2 C2 -169.3(8) . . . . ? Ru1 C1 Ru2 C2 134.7(4) . . . . ? Ru3 C1 Ru2 C2 58.5(3) . . . . ? C2 C1 Ru2 C14 -73.1(4) . . . . ? C10 C1 Ru2 C14 117.7(6) . . . . ? Ru1 C1 Ru2 C14 61.6(2) . . . . ? Ru3 C1 Ru2 C14 -14.6(2) . . . . ? C2 C1 Ru2 C4 139.1(4) . . . . ? C10 C1 Ru2 C4 -30.2(6) . . . . ? Ru1 C1 Ru2 C4 -86.2(2) . . . . ? Ru3 C1 Ru2 C4 -162.44(16) . . . . ? C2 C1 Ru2 C9 101.9(4) . . . . ? C10 C1 Ru2 C9 -67.3(6) . . . . ? Ru1 C1 Ru2 C9 -123.37(19) . . . . ? Ru3 C1 Ru2 C9 160.40(16) . . . . ? C2 C1 Ru2 C5 165.3(3) . . . . ? C10 C1 Ru2 C5 -3.9(7) . . . . ? Ru1 C1 Ru2 C5 -60.0(3) . . . . ? Ru3 C1 Ru2 C5 -136.2(2) . . . . ? C2 C1 Ru2 C6 162.6(6) . . . . ? C10 C1 Ru2 C6 -6.7(10) . . . . ? Ru1 C1 Ru2 C6 -62.7(7) . . . . ? Ru3 C1 Ru2 C6 -139.0(6) . . . . ? C2 C1 Ru2 C7 64.9(6) . . . . ? C10 C1 Ru2 C7 -104.4(6) . . . . ? Ru1 C1 Ru2 C7 -160.4(4) . . . . ? Ru3 C1 Ru2 C7 123.3(4) . . . . ? C2 C1 Ru2 C8 73.4(4) . . . . ? C10 C1 Ru2 C8 -95.8(6) . . . . ? Ru1 C1 Ru2 C8 -151.86(18) . . . . ? Ru3 C1 Ru2 C8 131.91(18) . . . . ? C2 C1 Ru2 Ru3 -58.5(3) . . . . ? C10 C1 Ru2 Ru3 132.3(6) . . . . ? Ru1 C1 Ru2 Ru3 76.23(14) . . . . ? C2 C1 Ru2 Ru1 -134.7(4) . . . . ? C10 C1 Ru2 Ru1 56.0(5) . . . . ? Ru3 C1 Ru2 Ru1 -76.23(14) . . . . ? Si1 C2 Ru2 C1 121.8(6) . . . . ? Ru3 C2 Ru2 C1 -95.4(4) . . . . ? C1 C2 Ru2 C14 117.2(4) . . . . ? Si1 C2 Ru2 C14 -120.9(4) . . . . ? Ru3 C2 Ru2 C14 21.8(2) . . . . ? C1 C2 Ru2 C4 -50.6(4) . . . . ? Si1 C2 Ru2 C4 71.3(5) . . . . ? Ru3 C2 Ru2 C4 -145.98(19) . . . . ? C1 C2 Ru2 C9 -83.7(4) . . . . ? Si1 C2 Ru2 C9 38.2(5) . . . . ? Ru3 C2 Ru2 C9 -179.08(18) . . . . ? C1 C2 Ru2 C5 -34.9(7) . . . . ? Si1 C2 Ru2 C5 86.9(7) . . . . ? Ru3 C2 Ru2 C5 -130.4(5) . . . . ? C1 C2 Ru2 C6 -161.3(7) . . . . ? Si1 C2 Ru2 C6 -39.5(10) . . . . ? Ru3 C2 Ru2 C6 103.3(7) . . . . ? C1 C2 Ru2 C7 -149.0(4) . . . . ? Si1 C2 Ru2 C7 -27.2(6) . . . . ? Ru3 C2 Ru2 C7 115.6(3) . . . . ? C1 C2 Ru2 C8 -120.1(4) . . . . ? Si1 C2 Ru2 C8 1.7(5) . . . . ? Ru3 C2 Ru2 C8 144.47(19) . . . . ? C1 C2 Ru2 Ru3 95.4(4) . . . . ? Si1 C2 Ru2 Ru3 -142.8(5) . . . . ? C1 C2 Ru2 Ru1 34.3(3) . . . . ? Si1 C2 Ru2 Ru1 156.2(4) . . . . ? Ru3 C2 Ru2 Ru1 -61.09(12) . . . . ? O14 C14 Ru2 C1 147.1(4) . . . . ? C13 C14 Ru2 C1 -38.7(5) . . . . ? Ru3 C14 Ru2 C1 15.8(2) . . . . ? O14 C14 Ru2 C2 111.3(4) . . . . ? C13 C14 Ru2 C2 -74.5(5) . . . . ? Ru3 C14 Ru2 C2 -20.05(19) . . . . ? O14 C14 Ru2 C4 -83.8(5) . . . . ? C13 C14 Ru2 C4 90.3(5) . . . . ? Ru3 C14 Ru2 C4 144.8(2) . . . . ? O14 C14 Ru2 C9 -22.6(7) . . . . ? C13 C14 Ru2 C9 151.6(4) . . . . ? Ru3 C14 Ru2 C9 -153.9(3) . . . . ? O14 C14 Ru2 C5 -78.7(5) . . . . ? C13 C14 Ru2 C5 95.5(5) . . . . ? Ru3 C14 Ru2 C5 149.94(17) . . . . ? O14 C14 Ru2 C6 -49.7(4) . . . . ? C13 C14 Ru2 C6 124.4(5) . . . . ? Ru3 C14 Ru2 C6 178.90(19) . . . . ? O14 C14 Ru2 C7 -14.9(4) . . . . ? C13 C14 Ru2 C7 159.2(5) . . . . ? Ru3 C14 Ru2 C7 -146.28(18) . . . . ? O14 C14 Ru2 C8 0.8(5) . . . . ? C13 C14 Ru2 C8 174.9(4) . . . . ? Ru3 C14 Ru2 C8 -130.61(19) . . . . ? O14 C14 Ru2 Ru3 131.4(5) . . . . ? C13 C14 Ru2 Ru3 -54.5(4) . . . . ? O14 C14 Ru2 Ru1 -169.1(4) . . . . ? C13 C14 Ru2 Ru1 5.1(4) . . . . ? Ru3 C14 Ru2 Ru1 59.56(10) . . . . ? C9 C4 Ru2 C1 -90.8(4) . . . . ? C5 C4 Ru2 C1 142.6(3) . . . . ? Si2 C4 Ru2 C1 23.8(3) . . . . ? C9 C4 Ru2 C2 -62.8(4) . . . . ? C5 C4 Ru2 C2 170.6(3) . . . . ? Si2 C4 Ru2 C2 51.8(4) . . . . ? C9 C4 Ru2 C14 135.0(4) . . . . ? C5 C4 Ru2 C14 8.4(5) . . . . ? Si2 C4 Ru2 C14 -110.4(4) . . . . ? C5 C4 Ru2 C9 -126.6(5) . . . . ? Si2 C4 Ru2 C9 114.6(5) . . . . ? C9 C4 Ru2 C5 126.6(5) . . . . ? Si2 C4 Ru2 C5 -118.8(5) . . . . ? C9 C4 Ru2 C6 97.8(4) . . . . ? C5 C4 Ru2 C6 -28.7(3) . . . . ? Si2 C4 Ru2 C6 -147.5(4) . . . . ? C9 C4 Ru2 C7 62.2(4) . . . . ? C5 C4 Ru2 C7 -64.4(3) . . . . ? Si2 C4 Ru2 C7 176.8(4) . . . . ? C9 C4 Ru2 C8 27.8(4) . . . . ? C5 C4 Ru2 C8 -98.8(4) . . . . ? Si2 C4 Ru2 C8 142.4(4) . . . . ? C9 C4 Ru2 Ru3 -124.5(4) . . . . ? C5 C4 Ru2 Ru3 108.9(4) . . . . ? Si2 C4 Ru2 Ru3 -9.9(6) . . . . ? C9 C4 Ru2 Ru1 -142.2(4) . . . . ? C5 C4 Ru2 Ru1 91.2(3) . . . . ? Si2 C4 Ru2 Ru1 -27.6(3) . . . . ? C8 C9 Ru2 C1 -134.0(4) . . . . ? C4 C9 Ru2 C1 93.0(4) . . . . ? C8 C9 Ru2 C2 -96.9(4) . . . . ? C4 C9 Ru2 C2 130.1(4) . . . . ? C8 C9 Ru2 C14 36.5(6) . . . . ? C4 C9 Ru2 C14 -96.5(5) . . . . ? C8 C9 Ru2 C4 133.0(6) . . . . ? C8 C9 Ru2 C5 100.8(4) . . . . ? C4 C9 Ru2 C5 -32.3(4) . . . . ? C8 C9 Ru2 C6 64.1(4) . . . . ? C4 C9 Ru2 C6 -68.9(4) . . . . ? C8 C9 Ru2 C7 27.9(3) . . . . ? C4 C9 Ru2 C7 -105.1(4) . . . . ? C4 C9 Ru2 C8 -133.0(6) . . . . ? C8 C9 Ru2 Ru3 -98.3(4) . . . . ? C4 C9 Ru2 Ru3 128.7(3) . . . . ? C8 C9 Ru2 Ru1 177.6(3) . . . . ? C4 C9 Ru2 Ru1 44.5(4) . . . . ? C6 C5 Ru2 C1 -178.4(4) . . . . ? C4 C5 Ru2 C1 -46.8(4) . . . . ? C6 C5 Ru2 C2 -153.7(5) . . . . ? C4 C5 Ru2 C2 -22.1(7) . . . . ? C6 C5 Ru2 C14 54.3(4) . . . . ? C4 C5 Ru2 C14 -174.2(3) . . . . ? C6 C5 Ru2 C4 -131.6(5) . . . . ? C6 C5 Ru2 C9 -99.4(4) . . . . ? C4 C5 Ru2 C9 32.2(3) . . . . ? C4 C5 Ru2 C6 131.6(5) . . . . ? C6 C5 Ru2 C7 -28.4(4) . . . . ? C4 C5 Ru2 C7 103.2(4) . . . . ? C6 C5 Ru2 C8 -63.2(4) . . . . ? C4 C5 Ru2 C8 68.3(3) . . . . ? C6 C5 Ru2 Ru3 96.3(4) . . . . ? C4 C5 Ru2 Ru3 -132.1(3) . . . . ? C6 C5 Ru2 Ru1 138.9(4) . . . . ? C4 C5 Ru2 Ru1 -89.5(3) . . . . ? C5 C6 Ru2 C1 3.9(9) . . . . ? C7 C6 Ru2 C1 -128.6(6) . . . . ? C5 C6 Ru2 C2 149.7(6) . . . . ? C7 C6 Ru2 C2 17.2(9) . . . . ? C5 C6 Ru2 C14 -125.5(4) . . . . ? C7 C6 Ru2 C14 101.9(4) . . . . ? C5 C6 Ru2 C4 29.7(3) . . . . ? C7 C6 Ru2 C4 -102.9(4) . . . . ? C5 C6 Ru2 C9 67.7(4) . . . . ? C7 C6 Ru2 C9 -64.8(4) . . . . ? C7 C6 Ru2 C5 -132.5(6) . . . . ? C5 C6 Ru2 C7 132.5(6) . . . . ? C5 C6 Ru2 C8 103.7(4) . . . . ? C7 C6 Ru2 C8 -28.8(4) . . . . ? C5 C6 Ru2 Ru3 -124.3(3) . . . . ? C7 C6 Ru2 Ru3 103.2(4) . . . . ? C5 C6 Ru2 Ru1 -47.7(4) . . . . ? C7 C6 Ru2 Ru1 179.7(3) . . . . ? C8 C7 Ru2 C1 13.4(7) . . . . ? C6 C7 Ru2 C1 144.1(5) . . . . ? C8 C7 Ru2 C2 56.0(4) . . . . ? C6 C7 Ru2 C2 -173.2(4) . . . . ? C8 C7 Ru2 C14 155.4(4) . . . . ? C6 C7 Ru2 C14 -73.9(4) . . . . ? C8 C7 Ru2 C4 -65.3(4) . . . . ? C6 C7 Ru2 C4 65.5(4) . . . . ? C8 C7 Ru2 C9 -28.8(3) . . . . ? C6 C7 Ru2 C9 102.0(4) . . . . ? C8 C7 Ru2 C5 -102.3(4) . . . . ? C6 C7 Ru2 C5 28.5(4) . . . . ? C8 C7 Ru2 C6 -130.8(6) . . . . ? C6 C7 Ru2 C8 130.8(6) . . . . ? C8 C7 Ru2 Ru3 118.9(3) . . . . ? C6 C7 Ru2 Ru3 -110.3(4) . . . . ? C8 C7 Ru2 Ru1 -131.2(4) . . . . ? C6 C7 Ru2 Ru1 -0.5(7) . . . . ? C7 C8 Ru2 C1 -173.1(3) . . . . ? C9 C8 Ru2 C1 54.6(4) . . . . ? C7 C8 Ru2 C2 -136.5(4) . . . . ? C9 C8 Ru2 C2 91.2(4) . . . . ? C7 C8 Ru2 C14 -28.4(4) . . . . ? C9 C8 Ru2 C14 -160.7(3) . . . . ? C7 C8 Ru2 C4 103.5(4) . . . . ? C9 C8 Ru2 C4 -28.8(4) . . . . ? C7 C8 Ru2 C9 132.3(5) . . . . ? C7 C8 Ru2 C5 65.6(4) . . . . ? C9 C8 Ru2 C5 -66.7(4) . . . . ? C7 C8 Ru2 C6 29.7(4) . . . . ? C9 C8 Ru2 C6 -102.6(4) . . . . ? C9 C8 Ru2 C7 -132.3(5) . . . . ? C7 C8 Ru2 Ru3 -95.8(4) . . . . ? C9 C8 Ru2 Ru3 131.8(3) . . . . ? C7 C8 Ru2 Ru1 127.3(4) . . . . ? C9 C8 Ru2 Ru1 -5.0(6) . . . . ? C18 Ru1 Ru2 C1 37.4(10) . . . . ? C19 Ru1 Ru2 C1 -155.9(3) . . . . ? C12 Ru1 Ru2 C1 117.7(3) . . . . ? C10 Ru1 Ru2 C1 -24.2(3) . . . . ? C11 Ru1 Ru2 C1 -59.7(3) . . . . ? Ru3 Ru1 Ru2 C1 73.5(2) . . . . ? C18 Ru1 Ru2 C2 11.6(10) . . . . ? C19 Ru1 Ru2 C2 178.3(3) . . . . ? C12 Ru1 Ru2 C2 91.9(2) . . . . ? C1 Ru1 Ru2 C2 -25.8(3) . . . . ? C10 Ru1 Ru2 C2 -50.0(2) . . . . ? C11 Ru1 Ru2 C2 -85.6(2) . . . . ? Ru3 Ru1 Ru2 C2 47.73(16) . . . . ? C18 Ru1 Ru2 C14 -88.4(10) . . . . ? C19 Ru1 Ru2 C14 78.3(2) . . . . ? C12 Ru1 Ru2 C14 -8.0(2) . . . . ? C1 Ru1 Ru2 C14 -125.7(3) . . . . ? C10 Ru1 Ru2 C14 -150.0(2) . . . . ? C11 Ru1 Ru2 C14 174.5(2) . . . . ? Ru3 Ru1 Ru2 C14 -52.19(15) . . . . ? C18 Ru1 Ru2 C4 134.4(10) . . . . ? C19 Ru1 Ru2 C4 -58.9(3) . . . . ? C12 Ru1 Ru2 C4 -145.2(2) . . . . ? C1 Ru1 Ru2 C4 97.1(3) . . . . ? C10 Ru1 Ru2 C4 72.8(2) . . . . ? C11 Ru1 Ru2 C4 37.3(2) . . . . ? Ru3 Ru1 Ru2 C4 170.60(17) . . . . ? C18 Ru1 Ru2 C9 109.5(10) . . . . ? C19 Ru1 Ru2 C9 -83.8(3) . . . . ? C12 Ru1 Ru2 C9 -170.2(2) . . . . ? C1 Ru1 Ru2 C9 72.1(3) . . . . ? C10 Ru1 Ru2 C9 47.9(2) . . . . ? C11 Ru1 Ru2 C9 12.4(2) . . . . ? Ru3 Ru1 Ru2 C9 145.65(19) . . . . ? C18 Ru1 Ru2 C5 171.5(10) . . . . ? C19 Ru1 Ru2 C5 -21.8(3) . . . . ? C12 Ru1 Ru2 C5 -108.2(2) . . . . ? C1 Ru1 Ru2 C5 134.1(3) . . . . ? C10 Ru1 Ru2 C5 109.9(2) . . . . ? C11 Ru1 Ru2 C5 74.4(2) . . . . ? Ru3 Ru1 Ru2 C5 -152.33(17) . . . . ? C18 Ru1 Ru2 C6 -162.8(10) . . . . ? C19 Ru1 Ru2 C6 3.9(3) . . . . ? C12 Ru1 Ru2 C6 -82.5(3) . . . . ? C1 Ru1 Ru2 C6 159.8(3) . . . . ? C10 Ru1 Ru2 C6 135.6(2) . . . . ? C11 Ru1 Ru2 C6 100.0(2) . . . . ? Ru3 Ru1 Ru2 C6 -126.67(19) . . . . ? C18 Ru1 Ru2 C7 -162.5(11) . . . . ? C19 Ru1 Ru2 C7 4.2(4) . . . . ? C12 Ru1 Ru2 C7 -82.2(4) . . . . ? C1 Ru1 Ru2 C7 160.1(4) . . . . ? C10 Ru1 Ru2 C7 135.9(4) . . . . ? C11 Ru1 Ru2 C7 100.4(4) . . . . ? Ru3 Ru1 Ru2 C7 -126.3(4) . . . . ? C18 Ru1 Ru2 C8 112.8(11) . . . . ? C19 Ru1 Ru2 C8 -80.5(4) . . . . ? C12 Ru1 Ru2 C8 -166.9(4) . . . . ? C1 Ru1 Ru2 C8 75.4(4) . . . . ? C10 Ru1 Ru2 C8 51.2(4) . . . . ? C11 Ru1 Ru2 C8 15.7(4) . . . . ? Ru3 Ru1 Ru2 C8 149.0(4) . . . . ? C18 Ru1 Ru2 Ru3 -36.2(10) . . . . ? C19 Ru1 Ru2 Ru3 130.5(2) . . . . ? C12 Ru1 Ru2 Ru3 44.17(16) . . . . ? C1 Ru1 Ru2 Ru3 -73.5(2) . . . . ? C10 Ru1 Ru2 Ru3 -97.77(16) . . . . ? C11 Ru1 Ru2 Ru3 -133.29(15) . . . . ? O31 C31 Ru3 C32 -1E1(3) . . . . ? O31 C31 Ru3 C2 8E1(3) . . . . ? O31 C31 Ru3 C12 -15E1(3) . . . . ? O31 C31 Ru3 C13 -12E1(3) . . . . ? O31 C31 Ru3 C14 -10E1(3) . . . . ? O31 C31 Ru3 C1 12E1(3) . . . . ? O31 C31 Ru3 Ru2 13E1(3) . . . . ? O31 C31 Ru3 Ru1 17E1(3) . . . . ? O32 C32 Ru3 C31 -105(17) . . . . ? O32 C32 Ru3 C2 143(17) . . . . ? O32 C32 Ru3 C12 -12(17) . . . . ? O32 C32 Ru3 C13 7(17) . . . . ? O32 C32 Ru3 C14 43(17) . . . . ? O32 C32 Ru3 C1 140(17) . . . . ? O32 C32 Ru3 Ru2 91(17) . . . . ? O32 C32 Ru3 Ru1 83(17) . . . . ? C1 C2 Ru3 C31 93.5(4) . . . . ? Si1 C2 Ru3 C31 -58.4(5) . . . . ? Ru2 C2 Ru3 C31 158.9(2) . . . . ? C1 C2 Ru3 C32 -176.4(4) . . . . ? Si1 C2 Ru3 C32 31.7(5) . . . . ? Ru2 C2 Ru3 C32 -111.1(2) . . . . ? C1 C2 Ru3 C12 -18.1(5) . . . . ? Si1 C2 Ru3 C12 -170.0(3) . . . . ? Ru2 C2 Ru3 C12 47.2(3) . . . . ? C1 C2 Ru3 C13 -64.9(5) . . . . ? Si1 C2 Ru3 C13 143.1(4) . . . . ? Ru2 C2 Ru3 C13 0.4(3) . . . . ? C1 C2 Ru3 C14 -86.4(4) . . . . ? Si1 C2 Ru3 C14 121.7(4) . . . . ? Ru2 C2 Ru3 C14 -21.0(2) . . . . ? Si1 C2 Ru3 C1 -151.9(7) . . . . ? Ru2 C2 Ru3 C1 65.4(3) . . . . ? C1 C2 Ru3 Ru2 -65.4(3) . . . . ? Si1 C2 Ru3 Ru2 142.7(5) . . . . ? C1 C2 Ru3 Ru1 -6.6(3) . . . . ? Si1 C2 Ru3 Ru1 -158.5(4) . . . . ? Ru2 C2 Ru3 Ru1 58.73(11) . . . . ? C13 C12 Ru3 C31 124.1(4) . . . . ? Ru1 C12 Ru3 C31 -104.3(2) . . . . ? C13 C12 Ru3 C32 32.2(5) . . . . ? Ru1 C12 Ru3 C32 163.8(3) . . . . ? C13 C12 Ru3 C2 -115.8(4) . . . . ? Ru1 C12 Ru3 C2 15.8(3) . . . . ? Ru1 C12 Ru3 C13 131.7(4) . . . . ? C13 C12 Ru3 C14 -30.6(3) . . . . ? Ru1 C12 Ru3 C14 101.1(2) . . . . ? C13 C12 Ru3 C1 -125.7(4) . . . . ? Ru1 C12 Ru3 C1 6.0(2) . . . . ? C13 C12 Ru3 Ru2 -80.1(3) . . . . ? Ru1 C12 Ru3 Ru2 51.59(14) . . . . ? C13 C12 Ru3 Ru1 -131.7(4) . . . . ? C12 C13 Ru3 C31 -63.3(4) . . . . ? C14 C13 Ru3 C31 165.9(3) . . . . ? Si3 C13 Ru3 C31 56.4(4) . . . . ? C12 C13 Ru3 C32 -157.6(4) . . . . ? C14 C13 Ru3 C32 71.6(4) . . . . ? Si3 C13 Ru3 C32 -37.8(4) . . . . ? C12 C13 Ru3 C2 95.1(4) . . . . ? C14 C13 Ru3 C2 -35.7(4) . . . . ? Si3 C13 Ru3 C2 -145.2(3) . . . . ? C14 C13 Ru3 C12 -130.8(5) . . . . ? Si3 C13 Ru3 C12 119.7(6) . . . . ? C12 C13 Ru3 C14 130.8(5) . . . . ? Si3 C13 Ru3 C14 -109.5(5) . . . . ? C12 C13 Ru3 C1 62.3(4) . . . . ? C14 C13 Ru3 C1 -68.5(3) . . . . ? Si3 C13 Ru3 C1 -178.0(3) . . . . ? C12 C13 Ru3 Ru2 95.4(3) . . . . ? C14 C13 Ru3 Ru2 -35.4(3) . . . . ? Si3 C13 Ru3 Ru2 -144.8(4) . . . . ? C12 C13 Ru3 Ru1 34.1(3) . . . . ? C14 C13 Ru3 Ru1 -96.7(3) . . . . ? Si3 C13 Ru3 Ru1 153.9(4) . . . . ? O14 C14 Ru3 C31 89.1(7) . . . . ? C13 C14 Ru3 C31 -25.5(6) . . . . ? Ru2 C14 Ru3 C31 -158.5(4) . . . . ? O14 C14 Ru3 C32 2.0(6) . . . . ? C13 C14 Ru3 C32 -112.5(4) . . . . ? Ru2 C14 Ru3 C32 114.5(2) . . . . ? O14 C14 Ru3 C2 -91.0(6) . . . . ? C13 C14 Ru3 C2 154.4(3) . . . . ? Ru2 C14 Ru3 C2 21.4(2) . . . . ? O14 C14 Ru3 C12 143.8(6) . . . . ? C13 C14 Ru3 C12 29.2(3) . . . . ? Ru2 C14 Ru3 C12 -103.8(2) . . . . ? O14 C14 Ru3 C13 114.6(7) . . . . ? Ru2 C14 Ru3 C13 -133.0(4) . . . . ? O14 C14 Ru3 C1 -124.4(6) . . . . ? C13 C14 Ru3 C1 121.0(3) . . . . ? Ru2 C14 Ru3 C1 -12.00(17) . . . . ? O14 C14 Ru3 Ru2 -112.4(6) . . . . ? C13 C14 Ru3 Ru2 133.0(4) . . . . ? O14 C14 Ru3 Ru1 -170.5(6) . . . . ? C13 C14 Ru3 Ru1 74.9(3) . . . . ? Ru2 C14 Ru3 Ru1 -58.05(10) . . . . ? C2 C1 Ru3 C31 -99.5(4) . . . . ? C10 C1 Ru3 C31 44.4(6) . . . . ? Ru2 C1 Ru3 C31 175.0(2) . . . . ? Ru1 C1 Ru3 C31 89.3(2) . . . . ? C2 C1 Ru3 C32 4.5(5) . . . . ? C10 C1 Ru3 C32 148.3(5) . . . . ? Ru2 C1 Ru3 C32 -81.1(3) . . . . ? Ru1 C1 Ru3 C32 -166.8(3) . . . . ? C10 C1 Ru3 C2 143.8(7) . . . . ? Ru2 C1 Ru3 C2 -85.5(4) . . . . ? Ru1 C1 Ru3 C2 -171.2(4) . . . . ? C2 C1 Ru3 C12 165.4(4) . . . . ? C10 C1 Ru3 C12 -50.8(6) . . . . ? Ru2 C1 Ru3 C12 79.89(19) . . . . ? Ru1 C1 Ru3 C12 -5.8(2) . . . . ? C2 C1 Ru3 C13 133.8(4) . . . . ? C10 C1 Ru3 C13 -82.4(6) . . . . ? Ru2 C1 Ru3 C13 48.2(2) . . . . ? Ru1 C1 Ru3 C13 -37.4(2) . . . . ? C2 C1 Ru3 C14 98.5(4) . . . . ? C10 C1 Ru3 C14 -117.7(6) . . . . ? Ru2 C1 Ru3 C14 12.95(19) . . . . ? Ru1 C1 Ru3 C14 -72.74(18) . . . . ? C2 C1 Ru3 Ru2 85.5(4) . . . . ? C10 C1 Ru3 Ru2 -130.6(6) . . . . ? Ru1 C1 Ru3 Ru2 -85.69(16) . . . . ? C2 C1 Ru3 Ru1 171.2(4) . . . . ? C10 C1 Ru3 Ru1 -45.0(5) . . . . ? Ru2 C1 Ru3 Ru1 85.69(16) . . . . ? C1 Ru2 Ru3 C31 -11.6(5) . . . . ? C2 Ru2 Ru3 C31 -55.1(5) . . . . ? C14 Ru2 Ru3 C31 151.9(5) . . . . ? C4 Ru2 Ru3 C31 27.6(6) . . . . ? C9 Ru2 Ru3 C31 -53.3(6) . . . . ? C5 Ru2 Ru3 C31 97.5(5) . . . . ? C6 Ru2 Ru3 C31 150.4(5) . . . . ? C7 Ru2 Ru3 C31 -161.1(5) . . . . ? C8 Ru2 Ru3 C31 -113.0(5) . . . . ? Ru1 Ru2 Ru3 C31 47.6(5) . . . . ? C1 Ru2 Ru3 C32 122.9(3) . . . . ? C2 Ru2 Ru3 C32 79.4(3) . . . . ? C14 Ru2 Ru3 C32 -73.7(3) . . . . ? C4 Ru2 Ru3 C32 162.0(4) . . . . ? C9 Ru2 Ru3 C32 81.2(4) . . . . ? C5 Ru2 Ru3 C32 -128.0(3) . . . . ? C6 Ru2 Ru3 C32 -75.2(3) . . . . ? C7 Ru2 Ru3 C32 -26.7(3) . . . . ? C8 Ru2 Ru3 C32 21.4(3) . . . . ? Ru1 Ru2 Ru3 C32 -177.9(2) . . . . ? C1 Ru2 Ru3 C2 43.5(3) . . . . ? C14 Ru2 Ru3 C2 -153.1(3) . . . . ? C4 Ru2 Ru3 C2 82.6(4) . . . . ? C9 Ru2 Ru3 C2 1.8(4) . . . . ? C5 Ru2 Ru3 C2 152.6(3) . . . . ? C6 Ru2 Ru3 C2 -154.6(3) . . . . ? C7 Ru2 Ru3 C2 -106.0(3) . . . . ? C8 Ru2 Ru3 C2 -58.0(3) . . . . ? Ru1 Ru2 Ru3 C2 102.7(2) . . . . ? C1 Ru2 Ru3 C12 -100.0(2) . . . . ? C2 Ru2 Ru3 C12 -143.5(3) . . . . ? C14 Ru2 Ru3 C12 63.4(2) . . . . ? C4 Ru2 Ru3 C12 -60.9(4) . . . . ? C9 Ru2 Ru3 C12 -141.7(3) . . . . ? C5 Ru2 Ru3 C12 9.1(3) . . . . ? C6 Ru2 Ru3 C12 61.9(3) . . . . ? C7 Ru2 Ru3 C12 110.4(3) . . . . ? C8 Ru2 Ru3 C12 158.5(3) . . . . ? Ru1 Ru2 Ru3 C12 -40.81(16) . . . . ? C1 Ru2 Ru3 C13 -136.2(2) . . . . ? C2 Ru2 Ru3 C13 -179.7(2) . . . . ? C14 Ru2 Ru3 C13 27.2(2) . . . . ? C4 Ru2 Ru3 C13 -97.1(4) . . . . ? C9 Ru2 Ru3 C13 -177.9(3) . . . . ? C5 Ru2 Ru3 C13 -27.1(3) . . . . ? C6 Ru2 Ru3 C13 25.7(2) . . . . ? C7 Ru2 Ru3 C13 74.3(3) . . . . ? C8 Ru2 Ru3 C13 122.3(3) . . . . ? Ru1 Ru2 Ru3 C13 -76.99(14) . . . . ? C1 Ru2 Ru3 C14 -163.4(2) . . . . ? C2 Ru2 Ru3 C14 153.1(3) . . . . ? C4 Ru2 Ru3 C14 -124.3(4) . . . . ? C9 Ru2 Ru3 C14 154.9(3) . . . . ? C5 Ru2 Ru3 C14 -54.3(3) . . . . ? C6 Ru2 Ru3 C14 -1.5(3) . . . . ? C7 Ru2 Ru3 C14 47.0(3) . . . . ? C8 Ru2 Ru3 C14 95.1(3) . . . . ? Ru1 Ru2 Ru3 C14 -104.22(17) . . . . ? C2 Ru2 Ru3 C1 -43.5(3) . . . . ? C14 Ru2 Ru3 C1 163.4(2) . . . . ? C4 Ru2 Ru3 C1 39.1(4) . . . . ? C9 Ru2 Ru3 C1 -41.7(3) . . . . ? C5 Ru2 Ru3 C1 109.1(3) . . . . ? C6 Ru2 Ru3 C1 161.9(3) . . . . ? C7 Ru2 Ru3 C1 -149.6(3) . . . . ? C8 Ru2 Ru3 C1 -101.5(3) . . . . ? Ru1 Ru2 Ru3 C1 59.19(17) . . . . ? C1 Ru2 Ru3 Ru1 -59.19(17) . . . . ? C2 Ru2 Ru3 Ru1 -102.7(2) . . . . ? C14 Ru2 Ru3 Ru1 104.22(17) . . . . ? C4 Ru2 Ru3 Ru1 -20.1(3) . . . . ? C9 Ru2 Ru3 Ru1 -100.9(3) . . . . ? C5 Ru2 Ru3 Ru1 49.9(3) . . . . ? C6 Ru2 Ru3 Ru1 102.7(2) . . . . ? C7 Ru2 Ru3 Ru1 151.3(2) . . . . ? C8 Ru2 Ru3 Ru1 -160.7(2) . . . . ? C18 Ru1 Ru3 C31 10.5(3) . . . . ? C19 Ru1 Ru3 C31 125.1(3) . . . . ? C12 Ru1 Ru3 C31 82.5(3) . . . . ? C1 Ru1 Ru3 C31 -105.6(3) . . . . ? C10 Ru1 Ru3 C31 -86.1(2) . . . . ? C11 Ru1 Ru3 C31 -101.4(3) . . . . ? Ru2 Ru1 Ru3 C31 -162.0(2) . . . . ? C18 Ru1 Ru3 C32 -177.7(10) . . . . ? C19 Ru1 Ru3 C32 -63.1(11) . . . . ? C12 Ru1 Ru3 C32 -105.8(10) . . . . ? C1 Ru1 Ru3 C32 66.2(10) . . . . ? C10 Ru1 Ru3 C32 85.7(10) . . . . ? C11 Ru1 Ru3 C32 70.3(10) . . . . ? Ru2 Ru1 Ru3 C32 9.7(10) . . . . ? C18 Ru1 Ru3 C2 120.9(3) . . . . ? C19 Ru1 Ru3 C2 -124.4(3) . . . . ? C12 Ru1 Ru3 C2 -167.1(3) . . . . ? C1 Ru1 Ru3 C2 4.9(2) . . . . ? C10 Ru1 Ru3 C2 24.4(2) . . . . ? C11 Ru1 Ru3 C2 9.0(2) . . . . ? Ru2 Ru1 Ru3 C2 -51.59(16) . . . . ? C18 Ru1 Ru3 C12 -71.9(3) . . . . ? C19 Ru1 Ru3 C12 42.7(3) . . . . ? C1 Ru1 Ru3 C12 172.0(3) . . . . ? C10 Ru1 Ru3 C12 -168.5(3) . . . . ? C11 Ru1 Ru3 C12 176.1(3) . . . . ? Ru2 Ru1 Ru3 C12 115.5(2) . . . . ? C18 Ru1 Ru3 C13 -99.3(3) . . . . ? C19 Ru1 Ru3 C13 15.3(3) . . . . ? C12 Ru1 Ru3 C13 -27.3(3) . . . . ? C1 Ru1 Ru3 C13 144.6(2) . . . . ? C10 Ru1 Ru3 C13 164.1(2) . . . . ? C11 Ru1 Ru3 C13 148.8(2) . . . . ? Ru2 Ru1 Ru3 C13 88.18(15) . . . . ? C18 Ru1 Ru3 C14 -137.6(3) . . . . ? C19 Ru1 Ru3 C14 -23.0(3) . . . . ? C12 Ru1 Ru3 C14 -65.6(3) . . . . ? C1 Ru1 Ru3 C14 106.3(2) . . . . ? C10 Ru1 Ru3 C14 125.8(2) . . . . ? C11 Ru1 Ru3 C14 110.5(2) . . . . ? Ru2 Ru1 Ru3 C14 49.89(15) . . . . ? C18 Ru1 Ru3 C1 116.1(3) . . . . ? C19 Ru1 Ru3 C1 -129.3(3) . . . . ? C12 Ru1 Ru3 C1 -172.0(3) . . . . ? C10 Ru1 Ru3 C1 19.5(2) . . . . ? C11 Ru1 Ru3 C1 4.1(2) . . . . ? Ru2 Ru1 Ru3 C1 -56.45(18) . . . . ? C18 Ru1 Ru3 Ru2 172.5(2) . . . . ? C19 Ru1 Ru3 Ru2 -72.9(2) . . . . ? C12 Ru1 Ru3 Ru2 -115.5(2) . . . . ? C1 Ru1 Ru3 Ru2 56.45(17) . . . . ? C10 Ru1 Ru3 Ru2 75.95(15) . . . . ? C11 Ru1 Ru3 Ru2 60.59(19) . . . . ? C25B C20B Si3 C13 -168.9(5) . . . . ? C21B C20B Si3 C13 11.3(6) . . . . ? C25B C20B Si3 C20D -43.2(6) . . . . ? C21B C20B Si3 C20D 137.0(6) . . . . ? C25B C20B Si3 C20C 74.5(6) . . . . ? C21B C20B Si3 C20C -105.3(6) . . . . ? C12 C13 Si3 C20B -107.3(5) . . . . ? C14 C13 Si3 C20B 72.4(5) . . . . ? Ru3 C13 Si3 C20B 160.2(4) . . . . ? C12 C13 Si3 C20D 130.6(5) . . . . ? C14 C13 Si3 C20D -49.6(5) . . . . ? Ru3 C13 Si3 C20D 38.1(5) . . . . ? C12 C13 Si3 C20C 9.2(6) . . . . ? C14 C13 Si3 C20C -171.0(4) . . . . ? Ru3 C13 Si3 C20C -83.3(4) . . . . ? C25D C20D Si3 C20B 154.5(5) . . . . ? C21D C20D Si3 C20B -24.3(6) . . . . ? C25D C20D Si3 C13 -85.5(6) . . . . ? C21D C20D Si3 C13 95.6(6) . . . . ? C25D C20D Si3 C20C 36.3(6) . . . . ? C21D C20D Si3 C20C -142.5(5) . . . . ? C21C C20C Si3 C20B -16.4(8) . . . . ? C25C C20C Si3 C20B 166.5(6) . . . . ? C21C C20C Si3 C13 -131.3(7) . . . . ? C25C C20C Si3 C13 51.6(6) . . . . ? C21C C20C Si3 C20D 102.6(7) . . . . ? C25C C20C Si3 C20D -74.5(6) . . . . ? C10 C11 Si2 C20A -167.4(5) . . . . ? Ru1 C11 Si2 C20A -86.8(3) . . . . ? C10 C11 Si2 C20 68.4(6) . . . . ? Ru1 C11 Si2 C20 149.0(3) . . . . ? C10 C11 Si2 C4 -44.2(6) . . . . ? Ru1 C11 Si2 C4 36.4(4) . . . . ? C21A C20A Si2 C11 135.9(6) . . . . ? C25A C20A Si2 C11 -40.1(6) . . . . ? C21A C20A Si2 C20 -101.5(6) . . . . ? C25A C20A Si2 C20 82.5(6) . . . . ? C21A C20A Si2 C4 14.2(7) . . . . ? C25A C20A Si2 C4 -161.7(5) . . . . ? C25 C20 Si2 C11 -15.9(7) . . . . ? C21 C20 Si2 C11 169.1(5) . . . . ? C25 C20 Si2 C20A -139.5(6) . . . . ? C21 C20 Si2 C20A 45.6(6) . . . . ? C25 C20 Si2 C4 100.0(6) . . . . ? C21 C20 Si2 C4 -74.9(6) . . . . ? C9 C4 Si2 C11 84.7(5) . . . . ? C5 C4 Si2 C11 -85.5(5) . . . . ? Ru2 C4 Si2 C11 0.9(4) . . . . ? C9 C4 Si2 C20A -152.4(5) . . . . ? C5 C4 Si2 C20A 37.4(6) . . . . ? Ru2 C4 Si2 C20A 123.7(3) . . . . ? C9 C4 Si2 C20 -31.6(5) . . . . ? C5 C4 Si2 C20 158.2(5) . . . . ? Ru2 C4 Si2 C20 -115.5(3) . . . . ? C1 C2 Si1 C17 144.4(6) . . . . ? Ru3 C2 Si1 C17 -72.9(5) . . . . ? Ru2 C2 Si1 C17 51.4(5) . . . . ? C1 C2 Si1 C16 -95.2(6) . . . . ? Ru3 C2 Si1 C16 47.5(5) . . . . ? Ru2 C2 Si1 C16 171.8(4) . . . . ? C1 C2 Si1 C15 22.8(7) . . . . ? Ru3 C2 Si1 C15 165.5(5) . . . . ? Ru2 C2 Si1 C15 -70.2(5) . . . . ? Cl2B C51B Cl1B Cl3B 147(10) . . . 1_655 ? Cl4B C50B Cl3B C51B 50(10) . . . 1_455 ? Cl4B C50B Cl3B Cl1B 132(8) . . . 1_455 ? # END of CIF