# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2006 data_global _journal_coden_Cambridge 182 _publ_requested_journal Chem.Commun. _publ_contact_author_name 'Roberto Pattacini' _publ_contact_author_address ; LCC, Uni. L. Pasteur, Inst. Le Bel, 4 Rue B. Pascal F-67000 Strasbourg France ; _publ_contact_author_email rpattacini@virgilio.it _publ_contact_author_phone '+33 39024313' _publ_contact_author_fax '+33 390241322' loop_ _publ_author_name _publ_author_address 'Braunstein, Pierre' 'LCC, Uni. L. Pasteur, Inst. Le Bel, 4 Rue B. Pascal F-67000 Strasbourg ' 'Messaoudi, Abdelatif' 'LCC, Uni. L. Pasteur, Inst. Le Bel, 4 Rue B. Pascal F-67000 Strasbourg ' 'Belletti, Daniele' 'Dip. Chimica GIAF, Univ. Parma, P. Area delle Scienze 17/A, I-43100, PR, Italy' 'Tiripicchio, Antonio' 'Dip. Chimica GIAF, Univ. Parma, P. Area delle Scienze 17/A, I-43100, PR, Italy' 'Predieri, Giovanni' 'Dip. Chimica GIAF, Univ. Parma, P. Area delle Scienze 17/A, I-43100, PR, Italy' _publ_section_title ; Trapping a pseudo-Hofmann rearrangement on a ruthenium cluster ; data_Compound2 _database_code_depnum_ccdc_archive 'CCDC 617271' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C47.40 H39 Cl0.60 N2.40 O9.40 P2 Ru3 Si' _chemical_formula_weight 1207.12 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_int_tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.6159(7) _cell_length_b 13.3036(7) _cell_length_c 17.1405(10) _cell_angle_alpha 98.4730(10) _cell_angle_beta 90.4370(10) _cell_angle_gamma 104.3700(10) _cell_volume 2535.2(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 999 _cell_measurement_theta_min 3 _cell_measurement_theta_max 27 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.581 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1203 _exptl_absorpt_coefficient_mu 1.055 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.860 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART1000' _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22509 _diffrn_reflns_av_R_equivalents 0.0491 _diffrn_reflns_av_sigmaI/netI 0.0798 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.60 _diffrn_reflns_theta_max 24.02 _reflns_number_total 7973 _reflns_number_gt 4879 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELX-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics Ortep3 _computing_publication_material Platon _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0100P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7973 _refine_ls_number_parameters 613 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0799 _refine_ls_R_factor_gt 0.0380 _refine_ls_wR_factor_ref 0.0584 _refine_ls_wR_factor_gt 0.0536 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.026 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.29651(4) 0.79769(3) 0.28839(3) 0.04199(13) Uani 1 1 d . . . Ru2 Ru 0.33636(4) 0.60177(3) 0.16690(3) 0.04534(14) Uani 1 1 d . . . Ru3 Ru 0.11395(4) 0.58427(4) 0.24330(3) 0.04878(14) Uani 1 1 d . . . Si1 Si 0.16732(15) 0.75154(13) 0.10149(9) 0.0596(5) Uani 1 1 d . . . Cl1 Cl 0.0855(6) 0.7474(5) 0.3375(5) 0.0676(19) Uani 0.60 1 d P . . P1 P 0.65047(14) 0.95861(11) 0.20604(9) 0.0530(4) Uani 1 1 d . . . P2 P 0.35676(13) 0.58720(10) 0.35956(8) 0.0441(4) Uani 1 1 d . . . N1 N 0.118(3) 0.738(3) 0.323(2) 0.126(17) Uani 0.40 1 d P . . N2 N 0.5206(4) 0.9234(3) 0.2421(2) 0.0562(12) Uani 1 1 d . . . N3 N 0.2991(3) 0.6336(3) 0.2912(2) 0.0404(11) Uani 1 1 d . . . O1 O 0.4220(4) 0.9138(3) 0.4397(2) 0.0910(15) Uani 1 1 d . . . O2 O 0.2783(4) 1.0128(3) 0.2672(3) 0.0866(15) Uani 1 1 d . . . O3 O 0.4955(4) 0.4583(4) 0.1607(2) 0.0999(16) Uani 1 1 d . . . O4 O 0.3644(4) 0.5669(4) -0.0081(2) 0.1086(18) Uani 1 1 d . . . O5 O 0.1417(4) 0.4039(3) 0.1271(2) 0.0734(12) Uani 1 1 d . . . O6 O -0.1224(4) 0.5428(4) 0.1576(3) 0.0929(15) Uani 1 1 d . . . O7 O -0.0091(4) 0.4162(4) 0.3334(3) 0.1129(18) Uani 1 1 d . . . O8 O 0.0071(10) 0.7916(9) 0.4326(6) 0.094(4) Uani 0.40 1 d P . . O9 O 0.4750(3) 0.7510(3) 0.1894(2) 0.0548(10) Uani 1 1 d . . . O10 O 0.2158(3) 0.7050(2) 0.17857(17) 0.0420(9) Uani 1 1 d . . . C1 C 0.3725(5) 0.8661(4) 0.3824(3) 0.0571(16) Uani 1 1 d . . . C2 C 0.2829(5) 0.9288(4) 0.2734(3) 0.0543(16) Uani 1 1 d . . . C3 C 0.4333(5) 0.5141(4) 0.1658(3) 0.0613(17) Uani 1 1 d . . . C4 C 0.3518(5) 0.5827(4) 0.0592(4) 0.0644(18) Uani 1 1 d . . . C5 C 0.1819(5) 0.4887(4) 0.1622(3) 0.0515(16) Uani 1 1 d . . . C6 C -0.0316(5) 0.5582(4) 0.1914(3) 0.0629(17) Uani 1 1 d . . . C7 C 0.0419(5) 0.4817(5) 0.2993(4) 0.0705(19) Uani 1 1 d . . . C8 C 0.0579(19) 0.7662(17) 0.3780(11) 0.046(6) Uani 0.40 1 d P . . C9 C 0.4502(5) 0.8250(4) 0.2349(3) 0.0483(15) Uani 1 1 d . . . C10 C 0.7641(5) 0.9671(4) 0.2809(4) 0.0553(15) Uani 1 1 d . . . C11 C 0.7368(6) 0.9850(4) 0.3601(4) 0.0732(19) Uani 1 1 d . . . H11 H 0.6603 0.9885 0.3736 0.088 Uiso 1 1 calc R . . C12 C 0.8229(8) 0.9972(6) 0.4172(4) 0.115(3) Uani 1 1 d . . . H12 H 0.8061 1.0094 0.4702 0.138 Uiso 1 1 calc R . . C13 C 0.9333(8) 0.9916(7) 0.3964(5) 0.123(3) Uani 1 1 d . . . H13 H 0.9917 0.9997 0.4359 0.148 Uiso 1 1 calc R . . C14 C 0.9617(6) 0.9747(6) 0.3213(5) 0.100(3) Uani 1 1 d . . . H14 H 1.0385 0.9709 0.3092 0.121 Uiso 1 1 calc R . . C15 C 0.8778(6) 0.9631(4) 0.2620(4) 0.0741(19) Uani 1 1 d . . . H15 H 0.8975 0.9525 0.2095 0.089 Uiso 1 1 calc R . . C16 C 0.6657(5) 1.0910(4) 0.1875(3) 0.0482(14) Uani 1 1 d . . . C17 C 0.5688(6) 1.1296(5) 0.1821(4) 0.080(2) Uani 1 1 d . . . H17 H 0.4935 1.0868 0.1870 0.095 Uiso 1 1 calc R . . C18 C 0.5804(7) 1.2323(5) 0.1694(4) 0.093(2) Uani 1 1 d . . . H18 H 0.5135 1.2575 0.1637 0.112 Uiso 1 1 calc R . . C19 C 0.6916(8) 1.2953(5) 0.1655(4) 0.081(2) Uani 1 1 d . . . H19 H 0.7001 1.3650 0.1593 0.098 Uiso 1 1 calc R . . C20 C 0.7890(6) 1.2594(5) 0.1703(3) 0.0745(19) Uani 1 1 d . . . H20 H 0.8640 1.3033 0.1663 0.089 Uiso 1 1 calc R . . C21 C 0.7769(6) 1.1560(5) 0.1814(3) 0.0671(17) Uani 1 1 d . . . H21 H 0.8442 1.1305 0.1846 0.081 Uiso 1 1 calc R . . C22 C 0.6854(5) 0.8864(4) 0.1188(4) 0.0590(16) Uani 1 1 d . . . C23 C 0.7112(5) 0.7887(5) 0.1160(4) 0.0763(19) Uani 1 1 d . . . H23 H 0.7134 0.7605 0.1624 0.092 Uiso 1 1 calc R . . C24 C 0.7337(6) 0.7329(6) 0.0450(5) 0.099(3) Uani 1 1 d . . . H24 H 0.7511 0.6683 0.0448 0.119 Uiso 1 1 calc R . . C25 C 0.7308(9) 0.7712(8) -0.0240(5) 0.142(4) Uani 1 1 d . . . H25 H 0.7490 0.7345 -0.0707 0.170 Uiso 1 1 calc R . . C26 C 0.7013(9) 0.8630(7) -0.0241(5) 0.158(4) Uani 1 1 d . . . H26 H 0.6955 0.8880 -0.0715 0.190 Uiso 1 1 calc R . . C27 C 0.6790(7) 0.9211(5) 0.0470(4) 0.111(3) Uani 1 1 d . . . H27 H 0.6595 0.9846 0.0457 0.133 Uiso 1 1 calc R . . C28 C 0.2982(5) 0.8399(4) 0.0627(3) 0.078(2) Uani 1 1 d . . . H28A H 0.3548 0.8006 0.0452 0.117 Uiso 1 1 calc R . . H28B H 0.3347 0.8964 0.1038 0.117 Uiso 1 1 calc R . . H28C H 0.2724 0.8679 0.0191 0.117 Uiso 1 1 calc R . . C29 C 0.0579(5) 0.8261(4) 0.1358(3) 0.090(2) Uani 1 1 d . . . H29A H 0.0948 0.8833 0.1763 0.134 Uiso 1 1 calc R . . H29B H -0.0082 0.7806 0.1567 0.134 Uiso 1 1 calc R . . H29C H 0.0303 0.8532 0.0923 0.134 Uiso 1 1 calc R . . C30 C 0.0940(5) 0.6404(4) 0.0238(3) 0.081(2) Uani 1 1 d . . . H30A H 0.1503 0.6014 0.0053 0.122 Uiso 1 1 calc R . . H30B H 0.0654 0.6673 -0.0195 0.122 Uiso 1 1 calc R . . H30C H 0.0284 0.5952 0.0454 0.122 Uiso 1 1 calc R . . C31 C 0.5115(5) 0.5938(4) 0.3487(3) 0.0467(14) Uani 1 1 d . . . C32 C 0.5590(5) 0.5076(4) 0.3525(3) 0.0602(16) Uani 1 1 d . . . H32 H 0.5089 0.4437 0.3600 0.072 Uiso 1 1 calc R . . C33 C 0.6805(6) 0.5163(5) 0.3452(3) 0.0728(19) Uani 1 1 d . . . H33 H 0.7096 0.4573 0.3454 0.087 Uiso 1 1 calc R . . C34 C 0.7574(6) 0.6101(6) 0.3377(3) 0.077(2) Uani 1 1 d . . . H34 H 0.8386 0.6161 0.3345 0.092 Uiso 1 1 calc R . . C35 C 0.7113(6) 0.6955(5) 0.3349(3) 0.0733(19) Uani 1 1 d . . . H35 H 0.7621 0.7598 0.3291 0.088 Uiso 1 1 calc R . . C36 C 0.5909(5) 0.6875(5) 0.3406(3) 0.0614(16) Uani 1 1 d . . . H36 H 0.5626 0.7468 0.3390 0.074 Uiso 1 1 calc R . . C37 C 0.3455(5) 0.6562(4) 0.4561(3) 0.0483(15) Uani 1 1 d . . . C38 C 0.2375(6) 0.6697(4) 0.4798(3) 0.0676(18) Uani 1 1 d . . . H38 H 0.1714 0.6436 0.4450 0.081 Uiso 1 1 calc R . . C39 C 0.2237(8) 0.7207(6) 0.5534(4) 0.098(3) Uani 1 1 d . . . H39 H 0.1493 0.7289 0.5680 0.117 Uiso 1 1 calc R . . C40 C 0.3181(9) 0.7587(6) 0.6042(4) 0.104(3) Uani 1 1 d . . . H40 H 0.3080 0.7914 0.6546 0.125 Uiso 1 1 calc R . . C41 C 0.4303(8) 0.7500(5) 0.5829(4) 0.093(3) Uani 1 1 d . . . H41 H 0.4958 0.7787 0.6179 0.112 Uiso 1 1 calc R . . C42 C 0.4431(6) 0.6980(4) 0.5086(3) 0.0699(18) Uani 1 1 d . . . H42 H 0.5178 0.6909 0.4937 0.084 Uiso 1 1 calc R . . C43 C 0.2885(5) 0.4505(4) 0.3655(3) 0.0500(15) Uani 1 1 d . . . C44 C 0.2557(5) 0.4198(5) 0.4369(3) 0.077(2) Uani 1 1 d . . . H44 H 0.2664 0.4696 0.4822 0.092 Uiso 1 1 calc R . . C45 C 0.2060(7) 0.3134(5) 0.4416(4) 0.112(3) Uani 1 1 d . . . H45 H 0.1820 0.2929 0.4897 0.134 Uiso 1 1 calc R . . C46 C 0.1931(7) 0.2410(5) 0.3758(5) 0.120(3) Uani 1 1 d . . . H46 H 0.1621 0.1704 0.3794 0.144 Uiso 1 1 calc R . . C47 C 0.2248(7) 0.2697(5) 0.3045(4) 0.104(3) Uani 1 1 d . . . H47 H 0.2137 0.2194 0.2594 0.124 Uiso 1 1 calc R . . C48 C 0.2736(5) 0.3743(4) 0.3000(3) 0.0701(18) Uani 1 1 d . . . H48 H 0.2971 0.3937 0.2515 0.084 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.0453(3) 0.0323(3) 0.0463(3) 0.0020(2) 0.0031(2) 0.0082(2) Ru2 0.0593(3) 0.0374(3) 0.0397(3) 0.0020(2) 0.0044(2) 0.0152(3) Ru3 0.0480(3) 0.0421(3) 0.0508(3) 0.0044(2) 0.0033(2) 0.0027(2) Si1 0.0640(12) 0.0583(11) 0.0574(11) 0.0129(9) -0.0085(9) 0.0150(10) Cl1 0.056(3) 0.056(3) 0.088(6) 0.012(3) 0.010(3) 0.007(3) P1 0.0536(11) 0.0392(9) 0.0646(11) 0.0060(8) 0.0025(9) 0.0098(8) P2 0.0555(10) 0.0343(8) 0.0402(9) 0.0051(7) 0.0011(7) 0.0076(8) N1 0.22(4) 0.15(2) 0.054(15) 0.030(13) 0.024(19) 0.11(2) N2 0.050(3) 0.048(3) 0.069(3) 0.004(3) 0.011(3) 0.013(3) N3 0.049(3) 0.031(2) 0.041(3) 0.003(2) 0.003(2) 0.011(2) O1 0.131(4) 0.060(3) 0.063(3) -0.012(2) -0.020(3) 0.002(3) O2 0.080(3) 0.045(3) 0.141(4) 0.019(3) 0.004(3) 0.025(3) O3 0.145(5) 0.113(4) 0.072(3) 0.012(3) 0.017(3) 0.089(4) O4 0.165(5) 0.133(4) 0.048(3) 0.017(3) 0.027(3) 0.072(4) O5 0.082(3) 0.059(3) 0.070(3) -0.005(2) -0.004(2) 0.008(3) O6 0.061(3) 0.107(4) 0.099(4) 0.013(3) -0.011(3) 0.002(3) O7 0.091(4) 0.114(4) 0.123(4) 0.062(3) 0.013(3) -0.021(3) O8 0.095(9) 0.114(10) 0.080(9) 0.010(7) 0.035(7) 0.044(8) O9 0.059(3) 0.048(2) 0.063(3) 0.012(2) 0.012(2) 0.022(2) O10 0.043(2) 0.0339(19) 0.046(2) 0.0057(17) -0.0014(17) 0.0056(17) C1 0.070(5) 0.034(4) 0.065(4) 0.004(3) 0.006(3) 0.009(3) C2 0.052(4) 0.043(4) 0.064(4) -0.001(3) 0.003(3) 0.009(3) C3 0.088(5) 0.056(4) 0.048(4) 0.005(3) 0.012(3) 0.036(4) C4 0.076(5) 0.058(4) 0.068(5) 0.011(4) 0.014(4) 0.032(4) C5 0.066(4) 0.035(3) 0.044(4) 0.001(3) -0.016(3) -0.003(3) C6 0.051(4) 0.059(4) 0.070(5) 0.008(3) 0.004(4) -0.001(4) C7 0.056(5) 0.082(5) 0.068(5) 0.011(4) 0.004(3) 0.005(4) C8 0.040(12) 0.065(12) 0.047(15) 0.004(11) 0.019(10) 0.042(9) C9 0.061(4) 0.023(3) 0.057(4) 0.004(3) -0.024(3) 0.007(3) C10 0.052(4) 0.042(4) 0.071(5) 0.012(3) -0.004(3) 0.008(3) C11 0.068(5) 0.078(5) 0.076(5) 0.011(4) 0.004(4) 0.022(4) C12 0.097(7) 0.175(8) 0.070(6) 0.010(5) -0.009(5) 0.032(7) C13 0.094(7) 0.182(9) 0.100(7) 0.031(7) -0.025(6) 0.039(7) C14 0.071(6) 0.125(7) 0.106(6) 0.002(6) -0.007(6) 0.034(5) C15 0.054(5) 0.081(5) 0.084(5) 0.012(4) -0.007(4) 0.013(4) C16 0.053(4) 0.036(3) 0.054(4) 0.007(3) 0.007(3) 0.007(3) C17 0.060(5) 0.051(4) 0.127(6) 0.027(4) -0.006(4) 0.006(4) C18 0.093(6) 0.061(5) 0.138(7) 0.032(5) 0.000(5) 0.033(5) C19 0.113(7) 0.049(5) 0.081(5) 0.022(4) 0.001(5) 0.012(5) C20 0.084(6) 0.052(5) 0.081(5) 0.014(4) 0.013(4) 0.001(4) C21 0.077(5) 0.054(4) 0.071(4) 0.015(4) 0.010(4) 0.016(4) C22 0.060(4) 0.044(4) 0.072(5) 0.012(3) 0.003(3) 0.010(3) C23 0.069(5) 0.062(5) 0.096(6) 0.002(4) 0.005(4) 0.018(4) C24 0.092(6) 0.071(5) 0.128(7) -0.033(6) 0.006(6) 0.035(4) C25 0.217(11) 0.124(9) 0.083(7) -0.033(6) -0.005(7) 0.068(8) C26 0.284(13) 0.118(8) 0.081(7) -0.012(6) 0.018(7) 0.081(9) C27 0.198(9) 0.074(5) 0.069(5) 0.002(4) 0.026(5) 0.056(6) C28 0.094(5) 0.066(4) 0.072(4) 0.033(4) -0.003(4) 0.003(4) C29 0.075(5) 0.099(5) 0.101(5) 0.011(4) -0.016(4) 0.037(4) C30 0.087(5) 0.089(5) 0.056(4) 0.008(4) -0.013(3) 0.005(4) C31 0.065(4) 0.037(3) 0.040(3) 0.006(3) -0.002(3) 0.015(3) C32 0.064(5) 0.051(4) 0.064(4) 0.007(3) 0.002(3) 0.013(4) C33 0.069(5) 0.078(5) 0.081(5) 0.001(4) -0.006(4) 0.042(4) C34 0.067(5) 0.087(5) 0.082(5) 0.020(4) 0.000(4) 0.027(5) C35 0.065(5) 0.069(5) 0.088(5) 0.030(4) -0.010(4) 0.011(4) C36 0.055(4) 0.062(4) 0.072(4) 0.026(3) -0.007(3) 0.015(4) C37 0.064(4) 0.038(3) 0.046(4) 0.011(3) 0.004(3) 0.016(3) C38 0.097(6) 0.071(5) 0.042(4) 0.014(3) 0.016(4) 0.030(4) C39 0.150(8) 0.097(6) 0.064(6) 0.019(5) 0.019(5) 0.060(6) C40 0.201(11) 0.084(6) 0.044(5) 0.003(4) 0.029(6) 0.070(7) C41 0.164(9) 0.067(5) 0.041(5) -0.008(4) -0.020(5) 0.025(5) C42 0.103(6) 0.055(4) 0.048(4) 0.001(3) -0.004(4) 0.019(4) C43 0.061(4) 0.046(4) 0.043(4) 0.014(3) -0.002(3) 0.010(3) C44 0.106(6) 0.053(4) 0.057(4) 0.012(4) -0.003(4) -0.008(4) C45 0.171(8) 0.060(5) 0.089(6) 0.034(5) 0.008(5) -0.014(5) C46 0.182(9) 0.044(5) 0.107(7) 0.015(5) -0.014(6) -0.022(5) C47 0.174(8) 0.045(5) 0.085(6) 0.011(4) -0.014(5) 0.016(5) C48 0.106(5) 0.044(4) 0.058(4) 0.015(3) -0.004(4) 0.010(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 C1 1.831(6) . ? Ru1 C2 1.844(6) . ? Ru1 C9 1.990(6) . ? Ru1 O10 2.158(3) . ? Ru1 N1 2.15(3) . ? Ru1 N3 2.199(3) . ? Ru1 Cl1 2.558(7) . ? Ru1 Ru3 3.0815(6) . ? Ru2 C3 1.809(6) . ? Ru2 C4 1.841(6) . ? Ru2 C5 2.028(5) . ? Ru2 N3 2.178(3) . ? Ru2 O10 2.182(3) . ? Ru2 O9 2.205(3) . ? Ru2 Ru3 2.8787(7) . ? Ru3 C7 1.821(7) . ? Ru3 C6 1.834(6) . ? Ru3 C5 2.041(6) . ? Ru3 O10 2.194(3) . ? Ru3 N3 2.201(4) . ? Ru3 N1 2.27(4) . ? Ru3 Cl1 2.600(8) . ? Si1 O10 1.688(3) . ? Si1 C29 1.846(5) . ? Si1 C30 1.861(5) . ? Si1 C28 1.869(5) . ? Cl1 C8 0.800(16) . ? Cl1 O8 1.960(13) . ? P1 N2 1.620(4) . ? P1 C22 1.761(6) . ? P1 C16 1.801(5) . ? P1 C10 1.805(6) . ? P2 N3 1.615(4) . ? P2 C31 1.790(5) . ? P2 C37 1.792(5) . ? P2 C43 1.812(5) . ? N1 C8 1.25(4) . ? N2 C9 1.348(6) . ? O1 C1 1.151(5) . ? O2 C2 1.153(5) . ? O3 C3 1.153(5) . ? O4 C4 1.160(6) . ? O5 C5 1.178(5) . ? O6 C6 1.157(6) . ? O7 C7 1.162(6) . ? O8 C8 1.163(16) . ? O9 C9 1.257(5) . ? C10 C15 1.375(7) . ? C10 C11 1.396(7) . ? C11 C12 1.358(8) . ? C11 H11 0.9300 . ? C12 C13 1.351(9) . ? C12 H12 0.9300 . ? C13 C14 1.332(9) . ? C13 H13 0.9300 . ? C14 C15 1.366(8) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C16 C17 1.357(7) . ? C16 C21 1.379(7) . ? C17 C18 1.388(7) . ? C17 H17 0.9300 . ? C18 C19 1.363(8) . ? C18 H18 0.9300 . ? C19 C20 1.339(7) . ? C19 H19 0.9300 . ? C20 C21 1.388(7) . ? C20 H20 0.9300 . ? C21 H21 0.9300 . ? C22 C27 1.386(7) . ? C22 C23 1.399(7) . ? C23 C24 1.391(8) . ? C23 H23 0.9300 . ? C24 C25 1.358(9) . ? C24 H24 0.9300 . ? C25 C26 1.348(9) . ? C25 H25 0.9300 . ? C26 C27 1.405(8) . ? C26 H26 0.9300 . ? C27 H27 0.9300 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C31 C36 1.381(6) . ? C31 C32 1.400(6) . ? C32 C33 1.395(7) . ? C32 H32 0.9300 . ? C33 C34 1.366(7) . ? C33 H33 0.9300 . ? C34 C35 1.378(7) . ? C34 H34 0.9300 . ? C35 C36 1.381(7) . ? C35 H35 0.9300 . ? C36 H36 0.9300 . ? C37 C38 1.368(7) . ? C37 C42 1.389(7) . ? C38 C39 1.372(7) . ? C38 H38 0.9300 . ? C39 C40 1.339(9) . ? C39 H39 0.9300 . ? C40 C41 1.384(9) . ? C40 H40 0.9300 . ? C41 C42 1.385(7) . ? C41 H41 0.9300 . ? C42 H42 0.9300 . ? C43 C44 1.374(6) . ? C43 C48 1.376(6) . ? C44 C45 1.405(7) . ? C44 H44 0.9300 . ? C45 C46 1.351(8) . ? C45 H45 0.9300 . ? C46 C47 1.360(8) . ? C46 H46 0.9300 . ? C47 C48 1.380(7) . ? C47 H47 0.9300 . ? C48 H48 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Ru1 C2 84.7(2) . . ? C1 Ru1 C9 90.5(2) . . ? C2 Ru1 C9 88.7(2) . . ? C1 Ru1 O10 174.30(18) . . ? C2 Ru1 O10 100.55(18) . . ? C9 Ru1 O10 87.49(16) . . ? C1 Ru1 N1 102.1(10) . . ? C2 Ru1 N1 97.8(10) . . ? C9 Ru1 N1 166.3(10) . . ? O10 Ru1 N1 79.5(10) . . ? C1 Ru1 N3 102.91(18) . . ? C2 Ru1 N3 172.36(19) . . ? C9 Ru1 N3 91.53(17) . . ? O10 Ru1 N3 71.84(12) . . ? N1 Ru1 N3 80.4(10) . . ? C1 Ru1 Cl1 97.9(3) . . ? C2 Ru1 Cl1 92.5(2) . . ? C9 Ru1 Cl1 171.6(2) . . ? O10 Ru1 Cl1 84.1(2) . . ? N1 Ru1 Cl1 6.5(11) . . ? N3 Ru1 Cl1 86.13(19) . . ? C1 Ru1 Ru3 132.23(17) . . ? C2 Ru1 Ru3 128.35(17) . . ? C9 Ru1 Ru3 119.37(15) . . ? O10 Ru1 Ru3 45.39(8) . . ? N1 Ru1 Ru3 47.5(10) . . ? N3 Ru1 Ru3 45.58(9) . . ? Cl1 Ru1 Ru3 53.93(16) . . ? C3 Ru2 C4 83.9(2) . . ? C3 Ru2 C5 95.9(2) . . ? C4 Ru2 C5 94.2(2) . . ? C3 Ru2 N3 103.43(19) . . ? C4 Ru2 N3 172.47(19) . . ? C5 Ru2 N3 83.48(17) . . ? C3 Ru2 O10 175.05(18) . . ? C4 Ru2 O10 100.84(18) . . ? C5 Ru2 O10 82.46(17) . . ? N3 Ru2 O10 71.77(12) . . ? C3 Ru2 O9 97.7(2) . . ? C4 Ru2 O9 94.8(2) . . ? C5 Ru2 O9 164.42(18) . . ? N3 Ru2 O9 85.98(13) . . ? O10 Ru2 O9 83.37(11) . . ? C3 Ru2 Ru3 126.95(18) . . ? C4 Ru2 Ru3 124.79(18) . . ? C5 Ru2 Ru3 45.15(16) . . ? N3 Ru2 Ru3 49.25(10) . . ? O10 Ru2 Ru3 49.04(8) . . ? O9 Ru2 Ru3 119.54(9) . . ? C7 Ru3 C6 85.4(3) . . ? C7 Ru3 C5 95.7(2) . . ? C6 Ru3 C5 95.7(2) . . ? C7 Ru3 O10 174.9(2) . . ? C6 Ru3 O10 99.2(2) . . ? C5 Ru3 O10 81.87(16) . . ? C7 Ru3 N3 104.2(2) . . ? C6 Ru3 N3 170.3(2) . . ? C5 Ru3 N3 82.60(17) . . ? O10 Ru3 N3 71.12(12) . . ? C7 Ru3 N1 105.1(9) . . ? C6 Ru3 N1 100.9(9) . . ? C5 Ru3 N1 154.2(9) . . ? O10 Ru3 N1 76.1(9) . . ? N3 Ru3 N1 77.7(9) . . ? C7 Ru3 Cl1 99.3(3) . . ? C6 Ru3 Cl1 94.4(2) . . ? C5 Ru3 Cl1 162.5(2) . . ? O10 Ru3 Cl1 82.41(18) . . ? N3 Ru3 Cl1 85.07(17) . . ? N1 Ru3 Cl1 8.5(9) . . ? C7 Ru3 Ru2 126.78(19) . . ? C6 Ru3 Ru2 124.58(18) . . ? C5 Ru3 Ru2 44.78(15) . . ? O10 Ru3 Ru2 48.70(8) . . ? N3 Ru3 Ru2 48.57(9) . . ? N1 Ru3 Ru2 109.5(9) . . ? Cl1 Ru3 Ru2 117.94(14) . . ? C7 Ru3 Ru1 133.41(19) . . ? C6 Ru3 Ru1 127.58(18) . . ? C5 Ru3 Ru1 110.03(15) . . ? O10 Ru3 Ru1 44.46(7) . . ? N3 Ru3 Ru1 45.51(9) . . ? N1 Ru3 Ru1 44.2(9) . . ? Cl1 Ru3 Ru1 52.70(13) . . ? Ru2 Ru3 Ru1 65.265(15) . . ? O10 Si1 C29 109.0(2) . . ? O10 Si1 C30 109.9(2) . . ? C29 Si1 C30 108.9(3) . . ? O10 Si1 C28 108.1(2) . . ? C29 Si1 C28 110.0(3) . . ? C30 Si1 C28 110.9(3) . . ? C8 Cl1 O8 4.0(17) . . ? C8 Cl1 Ru1 131.5(18) . . ? O8 Cl1 Ru1 135.0(5) . . ? C8 Cl1 Ru3 144.3(18) . . ? O8 Cl1 Ru3 143.6(5) . . ? Ru1 Cl1 Ru3 73.4(2) . . ? N2 P1 C22 120.1(2) . . ? N2 P1 C16 105.8(3) . . ? C22 P1 C16 107.2(3) . . ? N2 P1 C10 109.3(3) . . ? C22 P1 C10 107.8(3) . . ? C16 P1 C10 105.7(3) . . ? N3 P2 C31 113.3(2) . . ? N3 P2 C37 112.2(2) . . ? C31 P2 C37 106.1(3) . . ? N3 P2 C43 114.6(2) . . ? C31 P2 C43 104.8(2) . . ? C37 P2 C43 104.9(3) . . ? C8 N1 Ru1 134(3) . . ? C8 N1 Ru3 136(3) . . ? Ru1 N1 Ru3 88.3(13) . . ? C9 N2 P1 126.5(4) . . ? P2 N3 Ru2 123.1(2) . . ? P2 N3 Ru1 127.72(19) . . ? Ru2 N3 Ru1 94.67(14) . . ? P2 N3 Ru3 127.3(2) . . ? Ru2 N3 Ru3 82.18(12) . . ? Ru1 N3 Ru3 88.91(13) . . ? C8 O8 Cl1 2.8(12) . . ? C9 O9 Ru2 116.8(3) . . ? Si1 O10 Ru1 125.91(16) . . ? Si1 O10 Ru2 123.22(16) . . ? Ru1 O10 Ru2 95.72(11) . . ? Si1 O10 Ru3 127.55(17) . . ? Ru1 O10 Ru3 90.15(11) . . ? Ru2 O10 Ru3 82.27(10) . . ? O1 C1 Ru1 176.4(5) . . ? O2 C2 Ru1 176.6(5) . . ? O3 C3 Ru2 176.2(5) . . ? O4 C4 Ru2 176.6(5) . . ? O5 C5 Ru2 137.2(5) . . ? O5 C5 Ru3 132.7(5) . . ? Ru2 C5 Ru3 90.1(2) . . ? O6 C6 Ru3 178.8(6) . . ? O7 C7 Ru3 176.8(6) . . ? Cl1 C8 O8 173(3) . . ? Cl1 C8 N1 11(2) . . ? O8 C8 N1 176(3) . . ? O9 C9 N2 120.9(5) . . ? O9 C9 Ru1 118.7(4) . . ? N2 C9 Ru1 120.0(4) . . ? C15 C10 C11 119.5(6) . . ? C15 C10 P1 121.8(5) . . ? C11 C10 P1 118.5(5) . . ? C12 C11 C10 119.3(6) . . ? C12 C11 H11 120.3 . . ? C10 C11 H11 120.3 . . ? C13 C12 C11 119.4(8) . . ? C13 C12 H12 120.3 . . ? C11 C12 H12 120.3 . . ? C14 C13 C12 122.4(8) . . ? C14 C13 H13 118.8 . . ? C12 C13 H13 118.8 . . ? C13 C14 C15 120.0(8) . . ? C13 C14 H14 120.0 . . ? C15 C14 H14 120.0 . . ? C14 C15 C10 119.3(7) . . ? C14 C15 H15 120.3 . . ? C10 C15 H15 120.3 . . ? C17 C16 C21 118.8(5) . . ? C17 C16 P1 120.8(5) . . ? C21 C16 P1 120.3(5) . . ? C16 C17 C18 120.9(6) . . ? C16 C17 H17 119.5 . . ? C18 C17 H17 119.5 . . ? C19 C18 C17 118.8(6) . . ? C19 C18 H18 120.6 . . ? C17 C18 H18 120.6 . . ? C20 C19 C18 121.6(7) . . ? C20 C19 H19 119.2 . . ? C18 C19 H19 119.2 . . ? C19 C20 C21 119.4(7) . . ? C19 C20 H20 120.3 . . ? C21 C20 H20 120.3 . . ? C16 C21 C20 120.3(6) . . ? C16 C21 H21 119.8 . . ? C20 C21 H21 119.8 . . ? C27 C22 C23 116.1(6) . . ? C27 C22 P1 120.4(5) . . ? C23 C22 P1 123.4(5) . . ? C24 C23 C22 121.1(7) . . ? C24 C23 H23 119.4 . . ? C22 C23 H23 119.4 . . ? C25 C24 C23 121.1(8) . . ? C25 C24 H24 119.4 . . ? C23 C24 H24 119.4 . . ? C26 C25 C24 119.4(9) . . ? C26 C25 H25 120.3 . . ? C24 C25 H25 120.3 . . ? C25 C26 C27 120.5(9) . . ? C25 C26 H26 119.8 . . ? C27 C26 H26 119.8 . . ? C22 C27 C26 121.7(7) . . ? C22 C27 H27 119.1 . . ? C26 C27 H27 119.1 . . ? Si1 C28 H28A 109.5 . . ? Si1 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? Si1 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? Si1 C29 H29A 109.5 . . ? Si1 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? Si1 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? Si1 C30 H30A 109.5 . . ? Si1 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? Si1 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C36 C31 C32 116.9(5) . . ? C36 C31 P2 120.5(4) . . ? C32 C31 P2 122.5(4) . . ? C33 C32 C31 120.8(6) . . ? C33 C32 H32 119.6 . . ? C31 C32 H32 119.6 . . ? C34 C33 C32 121.2(6) . . ? C34 C33 H33 119.4 . . ? C32 C33 H33 119.4 . . ? C33 C34 C35 118.2(6) . . ? C33 C34 H34 120.9 . . ? C35 C34 H34 120.9 . . ? C34 C35 C36 121.2(6) . . ? C34 C35 H35 119.4 . . ? C36 C35 H35 119.4 . . ? C35 C36 C31 121.7(6) . . ? C35 C36 H36 119.2 . . ? C31 C36 H36 119.2 . . ? C38 C37 C42 117.8(5) . . ? C38 C37 P2 119.6(5) . . ? C42 C37 P2 122.6(5) . . ? C37 C38 C39 121.9(7) . . ? C37 C38 H38 119.0 . . ? C39 C38 H38 119.0 . . ? C40 C39 C38 119.7(8) . . ? C40 C39 H39 120.1 . . ? C38 C39 H39 120.1 . . ? C39 C40 C41 121.1(8) . . ? C39 C40 H40 119.5 . . ? C41 C40 H40 119.5 . . ? C40 C41 C42 118.7(7) . . ? C40 C41 H41 120.6 . . ? C42 C41 H41 120.6 . . ? C41 C42 C37 120.7(6) . . ? C41 C42 H42 119.6 . . ? C37 C42 H42 119.6 . . ? C44 C43 C48 118.2(5) . . ? C44 C43 P2 120.4(4) . . ? C48 C43 P2 121.4(4) . . ? C43 C44 C45 120.2(6) . . ? C43 C44 H44 119.9 . . ? C45 C44 H44 119.9 . . ? C46 C45 C44 119.6(7) . . ? C46 C45 H45 120.2 . . ? C44 C45 H45 120.2 . . ? C45 C46 C47 121.1(7) . . ? C45 C46 H46 119.4 . . ? C47 C46 H46 119.4 . . ? C46 C47 C48 119.1(7) . . ? C46 C47 H47 120.5 . . ? C48 C47 H47 120.5 . . ? C43 C48 C47 121.7(6) . . ? C43 C48 H48 119.1 . . ? C47 C48 H48 119.1 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 24.02 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.640 _refine_diff_density_min -0.545 _refine_diff_density_rms 0.073 # Attachment 'compound3_cif.cif' data_Compound3 _database_code_depnum_ccdc_archive 'CCDC 617272' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C47 H41 Cl N2 O9 P2 Ru3 Si, C0.5 H2 O0.5' _chemical_formula_sum 'C47.50 H43 Cl N2 O9.50 P2 Ru3 Si' _chemical_formula_weight 1220.51 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 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' P P 0.1023 0.0942 '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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_int_tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.608(3) _cell_length_b 13.277(3) _cell_length_c 17.196(3) _cell_angle_alpha 81.920(3) _cell_angle_beta 89.945(3) _cell_angle_gamma 76.225(3) _cell_volume 2547.1(10) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 999 _cell_measurement_theta_min 3 _cell_measurement_theta_max 27 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.591 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1218 _exptl_absorpt_coefficient_mu 1.072 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.671 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART1000' _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27031 _diffrn_reflns_av_R_equivalents 0.0341 _diffrn_reflns_av_sigmaI/netI 0.0441 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.60 _diffrn_reflns_theta_max 26.50 _reflns_number_total 10474 _reflns_number_gt 7729 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELX-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics Ortep3 _computing_publication_material Platon _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0400P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10474 _refine_ls_number_parameters 604 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0539 _refine_ls_R_factor_gt 0.0350 _refine_ls_wR_factor_ref 0.0883 _refine_ls_wR_factor_gt 0.0843 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.053 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.21855(2) 0.29192(2) 0.209934(16) 0.03601(8) Uani 1 1 d . . . Ru2 Ru 0.16893(3) 0.09878(2) 0.331251(16) 0.03781(8) Uani 1 1 d . . . Ru3 Ru 0.39391(3) 0.07422(2) 0.258503(17) 0.04245(9) Uani 1 1 d . . . Cl1 Cl 0.43158(9) 0.23534(8) 0.16209(6) 0.0562(3) Uani 1 1 d . . . P2 P 0.15348(9) 0.08169(7) 0.13926(5) 0.0395(2) Uani 1 1 d . . . P1 P -0.13543(8) 0.45583(7) 0.28818(6) 0.0403(2) Uani 1 1 d . . . Si1 Si 0.34250(10) 0.24750(8) 0.39625(6) 0.0479(3) Uani 1 1 d . . . O1 O 0.0989(3) 0.4118(2) 0.05964(17) 0.0745(9) Uani 1 1 d . . . O2 O 0.2421(3) 0.5069(2) 0.2311(2) 0.0777(10) Uani 1 1 d . . . O3 O 0.0053(3) -0.0437(2) 0.33642(18) 0.0795(10) Uani 1 1 d . . . O4 O 0.1336(4) 0.0680(3) 0.50538(18) 0.0958(12) Uani 1 1 d . . . O7 O 0.5169(3) -0.0979(3) 0.1715(2) 0.1027(13) Uani 1 1 d . . . O6 O 0.6282(3) 0.0293(3) 0.3462(2) 0.0819(10) Uani 1 1 d . . . O5 O 0.3533(2) -0.10398(19) 0.37423(16) 0.0593(7) Uani 1 1 d . . . O8 O 0.0341(2) 0.25025(17) 0.30740(14) 0.0431(6) Uani 1 1 d . . . O9 O 0.29454(19) 0.19981(16) 0.32054(13) 0.0373(5) Uani 1 1 d . . . N2 N 0.2114(2) 0.12781(19) 0.20743(15) 0.0352(6) Uani 1 1 d . . . N1 N -0.0056(3) 0.4226(2) 0.25273(17) 0.0434(7) Uani 1 1 d . . . C1 C 0.1457(4) 0.3623(3) 0.1154(2) 0.0490(9) Uani 1 1 d . . . C2 C 0.2359(3) 0.4236(3) 0.2248(2) 0.0505(10) Uani 1 1 d . . . C3 C 0.0675(4) 0.0112(3) 0.3320(2) 0.0492(9) Uani 1 1 d . . . C4 C 0.1492(4) 0.0820(3) 0.4397(2) 0.0553(10) Uani 1 1 d . . . C7 C 0.4660(4) -0.0323(3) 0.2041(3) 0.0622(11) Uani 1 1 d . . . C6 C 0.5383(4) 0.0460(3) 0.3135(2) 0.0543(10) Uani 1 1 d . . . C5 C 0.3196(3) -0.0180(3) 0.3393(2) 0.0472(9) Uani 1 1 d . . . C8 C 0.0608(3) 0.3244(3) 0.26314(19) 0.0387(8) Uani 1 1 d . . . C9 C 0.4069(4) 0.1390(3) 0.4763(2) 0.0696(13) Uani 1 1 d . . . H9A H 0.4729 0.0916 0.4571 0.104 Uiso 1 1 calc R . . H9B H 0.3476 0.1021 0.4937 0.104 Uiso 1 1 calc R . . H9C H 0.4334 0.1674 0.5195 0.104 Uiso 1 1 calc R . . C10 C 0.4592(4) 0.3147(4) 0.3622(3) 0.0745(14) Uani 1 1 d . . . H10A H 0.5241 0.2656 0.3434 0.112 Uiso 1 1 calc R . . H10B H 0.4869 0.3430 0.4050 0.112 Uiso 1 1 calc R . . H10C H 0.4274 0.3705 0.3204 0.112 Uiso 1 1 calc R . . C11 C 0.2159(4) 0.3391(3) 0.4329(3) 0.0684(12) Uani 1 1 d . . . H11A H 0.1831 0.3951 0.3915 0.103 Uiso 1 1 calc R . . H11B H 0.2424 0.3673 0.4761 0.103 Uiso 1 1 calc R . . H11C H 0.1563 0.3025 0.4502 0.103 Uiso 1 1 calc R . . C12 C 0.2225(3) -0.0545(3) 0.1310(2) 0.0492(9) Uani 1 1 d . . . C13 C 0.2608(5) -0.0833(3) 0.0592(3) 0.0771(15) Uani 1 1 d . . . H13 H 0.2527 -0.0327 0.0150 0.092 Uiso 1 1 calc R . . C14 C 0.3118(6) -0.1886(4) 0.0532(3) 0.114(2) Uani 1 1 d . . . H14 H 0.3397 -0.2074 0.0052 0.136 Uiso 1 1 calc R . . C15 C 0.3209(6) -0.2635(4) 0.1171(4) 0.114(2) Uani 1 1 d . . . H15 H 0.3535 -0.3335 0.1126 0.137 Uiso 1 1 calc R . . C16 C 0.2811(5) -0.2351(3) 0.1891(3) 0.0928(18) Uani 1 1 d . . . H16 H 0.2869 -0.2863 0.2327 0.111 Uiso 1 1 calc R . . C17 C 0.2332(4) -0.1314(3) 0.1959(2) 0.0624(12) Uani 1 1 d . . . H17 H 0.2078 -0.1129 0.2444 0.075 Uiso 1 1 calc R . . C18 C 0.1634(4) 0.1539(3) 0.0434(2) 0.0486(9) Uani 1 1 d . . . C19 C 0.0647(4) 0.1967(3) -0.0068(2) 0.0630(12) Uani 1 1 d . . . H19 H -0.0095 0.1874 0.0084 0.076 Uiso 1 1 calc R . . C20 C 0.0763(6) 0.2534(4) -0.0796(3) 0.0868(17) Uani 1 1 d . . . H20 H 0.0102 0.2823 -0.1130 0.104 Uiso 1 1 calc R . . C21 C 0.1859(7) 0.2666(4) -0.1018(3) 0.0935(19) Uani 1 1 d . . . H21 H 0.1936 0.3047 -0.1504 0.112 Uiso 1 1 calc R . . C22 C 0.2839(6) 0.2243(4) -0.0533(3) 0.0852(16) Uani 1 1 d . . . H22 H 0.3578 0.2332 -0.0693 0.102 Uiso 1 1 calc R . . C23 C 0.2735(4) 0.1683(3) 0.0198(2) 0.0629(11) Uani 1 1 d . . . H23 H 0.3402 0.1404 0.0529 0.075 Uiso 1 1 calc R . . C24 C -0.0021(3) 0.0853(3) 0.1501(2) 0.0434(9) Uani 1 1 d . . . C25 C -0.0815(4) 0.1765(3) 0.1631(2) 0.0560(10) Uani 1 1 d . . . H25 H -0.0537 0.2355 0.1679 0.067 Uiso 1 1 calc R . . C26 C -0.2008(4) 0.1818(4) 0.1692(3) 0.0655(12) Uani 1 1 d . . . H26 H -0.2526 0.2442 0.1776 0.079 Uiso 1 1 calc R . . C27 C -0.2442(4) 0.0948(4) 0.1629(3) 0.0676(12) Uani 1 1 d . . . H27 H -0.3249 0.0985 0.1671 0.081 Uiso 1 1 calc R . . C28 C -0.1692(4) 0.0050(4) 0.1508(3) 0.0691(13) Uani 1 1 d . . . H28 H -0.1981 -0.0539 0.1473 0.083 Uiso 1 1 calc R . . C29 C -0.0478(4) -0.0009(3) 0.1432(2) 0.0587(11) Uani 1 1 d . . . H29 H 0.0029 -0.0632 0.1334 0.070 Uiso 1 1 calc R . . C30 C -0.2459(3) 0.4568(3) 0.2145(2) 0.0464(9) Uani 1 1 d . . . C31 C -0.3610(4) 0.4538(3) 0.2334(3) 0.0618(11) Uani 1 1 d . . . H31 H -0.3842 0.4509 0.2853 0.074 Uiso 1 1 calc R . . C32 C -0.4417(5) 0.4551(4) 0.1725(4) 0.0920(17) Uani 1 1 d . . . H32 H -0.5189 0.4517 0.1846 0.110 Uiso 1 1 calc R . . C33 C -0.4103(6) 0.4612(5) 0.0975(4) 0.111(2) Uani 1 1 d . . . H33 H -0.4654 0.4616 0.0582 0.133 Uiso 1 1 calc R . . C34 C -0.2984(6) 0.4666(5) 0.0787(3) 0.103(2) Uani 1 1 d . . . H34 H -0.2772 0.4718 0.0264 0.124 Uiso 1 1 calc R . . C35 C -0.2161(4) 0.4644(3) 0.1365(3) 0.0655(12) Uani 1 1 d . . . H35 H -0.1395 0.4681 0.1231 0.079 Uiso 1 1 calc R . . C36 C -0.1678(3) 0.3836(3) 0.3783(2) 0.0488(9) Uani 1 1 d . . . C37 C -0.2008(4) 0.2897(3) 0.3810(3) 0.0595(11) Uani 1 1 d . . . H37 H -0.2122 0.2655 0.3340 0.071 Uiso 1 1 calc R . . C38 C -0.2172(4) 0.2315(4) 0.4500(4) 0.0844(16) Uani 1 1 d . . . H38 H -0.2420 0.1699 0.4501 0.101 Uiso 1 1 calc R . . C39 C -0.1963(6) 0.2653(5) 0.5201(4) 0.117(2) Uani 1 1 d . . . H39 H -0.2061 0.2255 0.5675 0.140 Uiso 1 1 calc R . . C40 C -0.1613(7) 0.3571(5) 0.5201(3) 0.127(3) Uani 1 1 d . . . H40 H -0.1476 0.3799 0.5673 0.153 Uiso 1 1 calc R . . C41 C -0.1464(5) 0.4160(4) 0.4480(3) 0.0824(15) Uani 1 1 d . . . H41 H -0.1217 0.4777 0.4475 0.099 Uiso 1 1 calc R . . C42 C -0.1533(3) 0.5900(3) 0.3050(2) 0.0434(9) Uani 1 1 d . . . C43 C -0.2627(4) 0.6508(3) 0.3176(2) 0.0604(11) Uani 1 1 d . . . H43 H -0.3290 0.6229 0.3177 0.072 Uiso 1 1 calc R . . C44 C -0.2756(4) 0.7539(3) 0.3302(3) 0.0679(13) Uani 1 1 d . . . H44 H -0.3501 0.7944 0.3394 0.081 Uiso 1 1 calc R . . C45 C -0.1803(5) 0.7954(3) 0.3291(3) 0.0731(13) Uani 1 1 d . . . H45 H -0.1886 0.8642 0.3382 0.088 Uiso 1 1 calc R . . C46 C -0.0708(5) 0.7354(3) 0.3145(3) 0.0847(16) Uani 1 1 d . . . H46 H -0.0054 0.7646 0.3123 0.102 Uiso 1 1 calc R . . C47 C -0.0567(4) 0.6332(3) 0.3032(3) 0.0650(12) Uani 1 1 d . . . H47 H 0.0181 0.5931 0.2942 0.078 Uiso 1 1 calc R . . O1S O 0.4770(11) 0.4562(12) 0.5369(7) 0.199(8) Uani 0.50 1 d P . . C1S C 0.5534(13) 0.3986(11) 0.6022(13) 0.165(9) Uani 0.50 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.03615(16) 0.02876(14) 0.04220(16) -0.00255(12) 0.00387(12) -0.00751(12) Ru2 0.04534(18) 0.03051(15) 0.03722(16) -0.00223(12) 0.00360(13) -0.00996(13) Ru3 0.03992(18) 0.03720(16) 0.04554(18) -0.00529(13) 0.00238(13) -0.00049(13) Cl1 0.0437(6) 0.0559(6) 0.0684(6) -0.0087(5) 0.0126(5) -0.0111(5) P2 0.0491(6) 0.0303(5) 0.0377(5) -0.0053(4) 0.0010(4) -0.0067(4) P1 0.0410(5) 0.0298(5) 0.0482(5) -0.0042(4) 0.0027(4) -0.0055(4) Si1 0.0484(6) 0.0462(6) 0.0496(6) -0.0114(5) -0.0060(5) -0.0098(5) O1 0.102(3) 0.0533(18) 0.0522(18) 0.0115(15) -0.0096(17) 0.0020(17) O2 0.073(2) 0.0402(16) 0.129(3) -0.0204(17) 0.0044(19) -0.0259(15) O3 0.107(3) 0.082(2) 0.071(2) -0.0101(17) 0.0159(18) -0.065(2) O4 0.137(3) 0.116(3) 0.0455(19) -0.0095(19) 0.020(2) -0.053(3) O7 0.079(3) 0.106(3) 0.117(3) -0.066(3) 0.007(2) 0.017(2) O6 0.0474(19) 0.095(2) 0.091(2) -0.0138(19) -0.0131(17) 0.0061(18) O5 0.0664(19) 0.0374(15) 0.0623(17) 0.0064(13) -0.0045(14) 0.0029(13) O8 0.0403(14) 0.0331(13) 0.0556(15) -0.0049(11) 0.0116(12) -0.0090(11) O9 0.0367(13) 0.0332(12) 0.0396(13) -0.0032(10) -0.0020(10) -0.0052(10) N2 0.0401(16) 0.0280(14) 0.0360(15) -0.0022(12) 0.0008(12) -0.0067(12) N1 0.0401(17) 0.0345(16) 0.0524(18) -0.0032(13) 0.0067(14) -0.0048(13) C1 0.057(3) 0.035(2) 0.053(2) -0.0033(18) 0.011(2) -0.0079(18) C2 0.040(2) 0.041(2) 0.069(3) -0.0045(19) 0.0005(19) -0.0095(18) C3 0.063(3) 0.044(2) 0.043(2) -0.0026(17) 0.0039(19) -0.019(2) C4 0.069(3) 0.049(2) 0.049(2) -0.0054(19) 0.009(2) -0.018(2) C7 0.056(3) 0.061(3) 0.063(3) -0.016(2) 0.004(2) 0.004(2) C6 0.047(2) 0.048(2) 0.059(3) -0.0061(19) 0.003(2) 0.0042(19) C5 0.058(3) 0.036(2) 0.047(2) -0.0080(17) -0.0069(18) -0.0078(18) C8 0.047(2) 0.0305(18) 0.0385(19) -0.0073(15) -0.0067(16) -0.0081(16) C9 0.078(3) 0.070(3) 0.053(3) -0.007(2) -0.016(2) -0.003(2) C10 0.060(3) 0.083(3) 0.089(3) -0.015(3) -0.015(3) -0.032(3) C11 0.070(3) 0.061(3) 0.074(3) -0.027(2) -0.001(2) -0.003(2) C12 0.056(2) 0.036(2) 0.055(2) -0.0151(18) -0.0020(19) -0.0039(18) C13 0.112(4) 0.053(3) 0.056(3) -0.018(2) -0.007(3) 0.006(3) C14 0.183(7) 0.058(3) 0.078(4) -0.033(3) -0.011(4) 0.027(4) C15 0.169(7) 0.045(3) 0.107(5) -0.020(3) -0.017(4) 0.023(3) C16 0.138(5) 0.037(3) 0.094(4) -0.006(3) -0.015(4) -0.005(3) C17 0.085(3) 0.040(2) 0.057(3) -0.0057(19) -0.006(2) -0.006(2) C18 0.069(3) 0.039(2) 0.037(2) -0.0098(16) 0.0025(19) -0.0085(19) C19 0.087(3) 0.049(2) 0.049(2) -0.004(2) -0.008(2) -0.010(2) C20 0.131(5) 0.072(3) 0.046(3) 0.005(2) -0.014(3) -0.012(3) C21 0.168(7) 0.068(3) 0.049(3) 0.001(2) 0.014(4) -0.042(4) C22 0.124(5) 0.089(4) 0.057(3) -0.018(3) 0.030(3) -0.050(4) C23 0.080(3) 0.065(3) 0.049(2) -0.012(2) 0.013(2) -0.024(2) C24 0.052(2) 0.041(2) 0.039(2) -0.0079(16) -0.0003(17) -0.0131(18) C25 0.056(3) 0.052(2) 0.067(3) -0.024(2) -0.004(2) -0.017(2) C26 0.056(3) 0.070(3) 0.072(3) -0.027(2) 0.000(2) -0.007(2) C27 0.055(3) 0.087(4) 0.068(3) -0.021(3) 0.009(2) -0.026(3) C28 0.072(3) 0.070(3) 0.075(3) -0.007(2) -0.001(3) -0.038(3) C29 0.068(3) 0.047(2) 0.062(3) -0.010(2) -0.004(2) -0.015(2) C30 0.044(2) 0.038(2) 0.056(2) -0.0053(17) -0.0020(18) -0.0096(17) C31 0.053(3) 0.062(3) 0.070(3) -0.001(2) -0.004(2) -0.018(2) C32 0.064(3) 0.091(4) 0.118(5) 0.011(4) -0.022(3) -0.028(3) C33 0.112(5) 0.146(6) 0.079(4) 0.022(4) -0.045(4) -0.062(5) C34 0.107(5) 0.148(6) 0.061(3) 0.012(3) -0.018(3) -0.060(4) C35 0.066(3) 0.072(3) 0.062(3) -0.005(2) 0.004(2) -0.027(2) C36 0.047(2) 0.040(2) 0.054(2) -0.0026(18) 0.0056(18) -0.0029(18) C37 0.054(3) 0.044(2) 0.077(3) 0.003(2) 0.012(2) -0.013(2) C38 0.076(4) 0.058(3) 0.110(4) 0.023(3) 0.006(3) -0.020(3) C39 0.154(7) 0.092(5) 0.086(5) 0.038(4) 0.006(4) -0.025(4) C40 0.213(8) 0.114(5) 0.056(3) 0.015(3) -0.016(4) -0.057(5) C41 0.117(5) 0.061(3) 0.064(3) 0.003(2) 0.001(3) -0.018(3) C42 0.050(2) 0.0301(18) 0.046(2) -0.0063(16) 0.0007(17) -0.0016(17) C43 0.063(3) 0.046(2) 0.073(3) -0.012(2) 0.018(2) -0.012(2) C44 0.074(3) 0.043(2) 0.078(3) -0.016(2) 0.015(3) 0.007(2) C45 0.093(4) 0.042(2) 0.086(3) -0.019(2) -0.003(3) -0.014(3) C46 0.071(3) 0.051(3) 0.140(5) -0.031(3) -0.011(3) -0.020(3) C47 0.050(3) 0.043(2) 0.102(4) -0.019(2) -0.012(2) -0.007(2) O1S 0.154(11) 0.37(2) 0.187(12) -0.228(14) 0.099(8) -0.168(12) C1S 0.091(11) 0.097(10) 0.30(3) -0.043(13) 0.129(13) -0.003(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 C1 1.852(4) . ? Ru1 C2 1.859(4) . ? Ru1 C8 2.027(4) . ? Ru1 O9 2.174(2) . ? Ru1 N2 2.207(3) . ? Ru1 Cl1 2.5772(11) . ? Ru1 Ru3 3.1175(7) . ? Ru2 C3 1.840(4) . ? Ru2 C4 1.868(4) . ? Ru2 C5 2.032(4) . ? Ru2 N2 2.187(3) . ? Ru2 O9 2.196(2) . ? Ru2 O8 2.221(2) . ? Ru2 Ru3 2.8627(7) . ? Ru3 C7 1.840(4) . ? Ru3 C6 1.857(4) . ? Ru3 C5 2.048(4) . ? Ru3 O9 2.198(2) . ? Ru3 N2 2.208(3) . ? Ru3 Cl1 2.6389(11) . ? P2 N2 1.613(3) . ? P2 C18 1.804(4) . ? P2 C24 1.805(4) . ? P2 C12 1.821(4) . ? P1 N1 1.611(3) . ? P1 C36 1.793(4) . ? P1 C30 1.800(4) . ? P1 C42 1.808(3) . ? Si1 O9 1.675(2) . ? Si1 C11 1.843(4) . ? Si1 C10 1.844(4) . ? Si1 C9 1.860(4) . ? O1 C1 1.140(4) . ? O2 C2 1.145(4) . ? O3 C3 1.138(4) . ? O4 C4 1.139(4) . ? O7 C7 1.146(5) . ? O6 C6 1.145(4) . ? O5 C5 1.189(4) . ? O8 C8 1.256(4) . ? N1 C8 1.335(4) . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 C13 1.385(5) . ? C12 C17 1.387(5) . ? C13 C14 1.401(6) . ? C13 H13 0.9300 . ? C14 C15 1.361(7) . ? C14 H14 0.9300 . ? C15 C16 1.391(7) . ? C15 H15 0.9300 . ? C16 C17 1.378(6) . ? C16 H16 0.9300 . ? C17 H17 0.9300 . ? C18 C23 1.389(6) . ? C18 C19 1.392(5) . ? C19 C20 1.392(6) . ? C19 H19 0.9300 . ? C20 C21 1.370(8) . ? C20 H20 0.9300 . ? C21 C22 1.368(7) . ? C21 H21 0.9300 . ? C22 C23 1.388(6) . ? C22 H22 0.9300 . ? C23 H23 0.9300 . ? C24 C25 1.382(5) . ? C24 C29 1.391(5) . ? C25 C26 1.374(6) . ? C25 H25 0.9300 . ? C26 C27 1.383(6) . ? C26 H26 0.9300 . ? C27 C28 1.341(6) . ? C27 H27 0.9300 . ? C28 C29 1.400(6) . ? C28 H28 0.9300 . ? C29 H29 0.9300 . ? C30 C35 1.380(5) . ? C30 C31 1.383(5) . ? C31 C32 1.400(6) . ? C31 H31 0.9300 . ? C32 C33 1.337(8) . ? C32 H32 0.9300 . ? C33 C34 1.355(8) . ? C33 H33 0.9300 . ? C34 C35 1.371(6) . ? C34 H34 0.9300 . ? C35 H35 0.9300 . ? C36 C41 1.372(6) . ? C36 C37 1.384(5) . ? C37 C38 1.362(6) . ? C37 H37 0.9300 . ? C38 C39 1.384(8) . ? C38 H38 0.9300 . ? C39 C40 1.374(8) . ? C39 H39 0.9300 . ? C40 C41 1.403(7) . ? C40 H40 0.9300 . ? C41 H41 0.9300 . ? C42 C43 1.368(5) . ? C42 C47 1.374(5) . ? C43 C44 1.389(5) . ? C43 H43 0.9300 . ? C44 C45 1.347(6) . ? C44 H44 0.9300 . ? C45 C46 1.374(6) . ? C45 H45 0.9300 . ? C46 C47 1.370(5) . ? C46 H46 0.9300 . ? C47 H47 0.9300 . ? O1S C1S 1.44(2) . ? O1S O1S 1.77(3) 2_666 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Ru1 C2 83.76(16) . . ? C1 Ru1 C8 90.09(15) . . ? C2 Ru1 C8 88.22(15) . . ? C1 Ru1 O9 175.07(13) . . ? C2 Ru1 O9 100.56(13) . . ? C8 Ru1 O9 87.70(11) . . ? C1 Ru1 N2 103.93(13) . . ? C2 Ru1 N2 172.30(14) . . ? C8 Ru1 N2 92.15(11) . . ? O9 Ru1 N2 71.77(9) . . ? C1 Ru1 Cl1 98.37(12) . . ? C2 Ru1 Cl1 93.11(12) . . ? C8 Ru1 Cl1 171.53(10) . . ? O9 Ru1 Cl1 83.83(6) . . ? N2 Ru1 Cl1 85.41(7) . . ? C1 Ru1 Ru3 133.58(11) . . ? C2 Ru1 Ru3 128.63(12) . . ? C8 Ru1 Ru3 118.97(9) . . ? O9 Ru1 Ru3 44.82(6) . . ? N2 Ru1 Ru3 45.10(7) . . ? Cl1 Ru1 Ru3 54.21(2) . . ? C3 Ru2 C4 83.76(17) . . ? C3 Ru2 C5 95.06(16) . . ? C4 Ru2 C5 93.23(17) . . ? C3 Ru2 N2 103.66(13) . . ? C4 Ru2 N2 172.41(14) . . ? C5 Ru2 N2 84.60(13) . . ? C3 Ru2 O9 175.17(13) . . ? C4 Ru2 O9 100.80(14) . . ? C5 Ru2 O9 83.15(12) . . ? N2 Ru2 O9 71.74(9) . . ? C3 Ru2 O8 97.88(14) . . ? C4 Ru2 O8 94.76(14) . . ? C5 Ru2 O8 165.44(12) . . ? N2 Ru2 O8 85.89(9) . . ? O9 Ru2 O8 83.41(8) . . ? C3 Ru2 Ru3 126.58(12) . . ? C4 Ru2 Ru3 124.42(13) . . ? C5 Ru2 Ru3 45.67(11) . . ? N2 Ru2 Ru3 49.68(7) . . ? O9 Ru2 Ru3 49.37(6) . . ? O8 Ru2 Ru3 120.14(6) . . ? C7 Ru3 C6 85.48(18) . . ? C7 Ru3 C5 95.45(17) . . ? C6 Ru3 C5 94.82(16) . . ? C7 Ru3 O9 175.59(15) . . ? C6 Ru3 O9 98.66(13) . . ? C5 Ru3 O9 82.74(12) . . ? C7 Ru3 N2 104.55(15) . . ? C6 Ru3 N2 169.94(14) . . ? C5 Ru3 N2 83.70(13) . . ? O9 Ru3 N2 71.30(9) . . ? C7 Ru3 Cl1 99.26(14) . . ? C6 Ru3 Cl1 95.30(13) . . ? C5 Ru3 Cl1 162.73(11) . . ? O9 Ru3 Cl1 81.92(6) . . ? N2 Ru3 Cl1 83.90(7) . . ? C7 Ru3 Ru2 126.91(14) . . ? C6 Ru3 Ru2 124.04(13) . . ? C5 Ru3 Ru2 45.22(11) . . ? O9 Ru3 Ru2 49.31(6) . . ? N2 Ru3 Ru2 49.04(7) . . ? Cl1 Ru3 Ru2 117.69(2) . . ? C7 Ru3 Ru1 133.69(13) . . ? C6 Ru3 Ru1 127.51(12) . . ? C5 Ru3 Ru1 110.51(11) . . ? O9 Ru3 Ru1 44.21(6) . . ? N2 Ru3 Ru1 45.06(7) . . ? Cl1 Ru3 Ru1 52.39(3) . . ? Ru2 Ru3 Ru1 65.306(14) . . ? Ru1 Cl1 Ru3 73.40(3) . . ? N2 P2 C18 111.82(16) . . ? N2 P2 C24 114.35(15) . . ? C18 P2 C24 105.36(18) . . ? N2 P2 C12 114.51(16) . . ? C18 P2 C12 105.43(17) . . ? C24 P2 C12 104.48(17) . . ? N1 P1 C36 119.07(16) . . ? N1 P1 C30 109.12(17) . . ? C36 P1 C30 108.60(18) . . ? N1 P1 C42 105.64(16) . . ? C36 P1 C42 106.96(17) . . ? C30 P1 C42 106.77(17) . . ? O9 Si1 C11 108.68(17) . . ? O9 Si1 C10 108.71(17) . . ? C11 Si1 C10 111.0(2) . . ? O9 Si1 C9 110.25(16) . . ? C11 Si1 C9 109.7(2) . . ? C10 Si1 C9 108.6(2) . . ? C8 O8 Ru2 118.2(2) . . ? Si1 O9 Ru1 125.43(12) . . ? Si1 O9 Ru2 123.86(12) . . ? Ru1 O9 Ru2 95.47(8) . . ? Si1 O9 Ru3 127.64(12) . . ? Ru1 O9 Ru3 90.97(8) . . ? Ru2 O9 Ru3 81.32(7) . . ? P2 N2 Ru2 122.90(14) . . ? P2 N2 Ru1 127.46(14) . . ? Ru2 N2 Ru1 94.78(10) . . ? P2 N2 Ru3 127.64(15) . . ? Ru2 N2 Ru3 81.28(9) . . ? Ru1 N2 Ru3 89.84(10) . . ? C8 N1 P1 123.3(3) . . ? O1 C1 Ru1 175.3(3) . . ? O2 C2 Ru1 176.5(4) . . ? O3 C3 Ru2 176.7(3) . . ? O4 C4 Ru2 176.4(4) . . ? O7 C7 Ru3 176.2(4) . . ? O6 C6 Ru3 178.8(4) . . ? O5 C5 Ru2 136.9(3) . . ? O5 C5 Ru3 134.0(3) . . ? Ru2 C5 Ru3 89.11(14) . . ? O8 C8 N1 123.8(3) . . ? O8 C8 Ru1 117.0(2) . . ? N1 C8 Ru1 119.2(2) . . ? 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 . . ? Si1 C10 H10A 109.5 . . ? Si1 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? Si1 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? Si1 C11 H11A 109.5 . . ? Si1 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? Si1 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C13 C12 C17 119.1(4) . . ? C13 C12 P2 120.5(3) . . ? C17 C12 P2 120.3(3) . . ? C12 C13 C14 120.0(4) . . ? C12 C13 H13 120.0 . . ? C14 C13 H13 120.0 . . ? C15 C14 C13 120.3(5) . . ? C15 C14 H14 119.8 . . ? C13 C14 H14 119.8 . . ? C14 C15 C16 119.8(5) . . ? C14 C15 H15 120.1 . . ? C16 C15 H15 120.1 . . ? C17 C16 C15 120.3(5) . . ? C17 C16 H16 119.9 . . ? C15 C16 H16 119.9 . . ? C16 C17 C12 120.4(4) . . ? C16 C17 H17 119.8 . . ? C12 C17 H17 119.8 . . ? C23 C18 C19 119.1(4) . . ? C23 C18 P2 118.5(3) . . ? C19 C18 P2 122.3(3) . . ? C18 C19 C20 120.3(5) . . ? C18 C19 H19 119.9 . . ? C20 C19 H19 119.9 . . ? C21 C20 C19 119.6(5) . . ? C21 C20 H20 120.2 . . ? C19 C20 H20 120.2 . . ? C20 C21 C22 120.8(5) . . ? C20 C21 H21 119.6 . . ? C22 C21 H21 119.6 . . ? C21 C22 C23 120.3(5) . . ? C21 C22 H22 119.9 . . ? C23 C22 H22 119.9 . . ? C22 C23 C18 119.9(5) . . ? C22 C23 H23 120.0 . . ? C18 C23 H23 120.0 . . ? C25 C24 C29 117.2(4) . . ? C25 C24 P2 120.5(3) . . ? C29 C24 P2 122.2(3) . . ? C26 C25 C24 121.5(4) . . ? C26 C25 H25 119.3 . . ? C24 C25 H25 119.3 . . ? C25 C26 C27 120.3(4) . . ? C25 C26 H26 119.9 . . ? C27 C26 H26 119.9 . . ? C28 C27 C26 119.7(4) . . ? C28 C27 H27 120.2 . . ? C26 C27 H27 120.2 . . ? C27 C28 C29 120.6(4) . . ? C27 C28 H28 119.7 . . ? C29 C28 H28 119.7 . . ? C24 C29 C28 120.7(4) . . ? C24 C29 H29 119.6 . . ? C28 C29 H29 119.6 . . ? C35 C30 C31 118.9(4) . . ? C35 C30 P1 119.1(3) . . ? C31 C30 P1 122.0(3) . . ? C30 C31 C32 118.4(4) . . ? C30 C31 H31 120.8 . . ? C32 C31 H31 120.8 . . ? C33 C32 C31 121.5(5) . . ? C33 C32 H32 119.2 . . ? C31 C32 H32 119.2 . . ? C32 C33 C34 120.1(5) . . ? C32 C33 H33 119.9 . . ? C34 C33 H33 119.9 . . ? C33 C34 C35 120.3(5) . . ? C33 C34 H34 119.9 . . ? C35 C34 H34 119.9 . . ? C34 C35 C30 120.7(5) . . ? C34 C35 H35 119.6 . . ? C30 C35 H35 119.6 . . ? C41 C36 C37 118.2(4) . . ? C41 C36 P1 118.9(3) . . ? C37 C36 P1 122.5(3) . . ? C38 C37 C36 122.2(5) . . ? C38 C37 H37 118.9 . . ? C36 C37 H37 118.9 . . ? C37 C38 C39 119.1(5) . . ? C37 C38 H38 120.4 . . ? C39 C38 H38 120.4 . . ? C40 C39 C38 120.6(5) . . ? C40 C39 H39 119.7 . . ? C38 C39 H39 119.7 . . ? C39 C40 C41 119.0(6) . . ? C39 C40 H40 120.5 . . ? C41 C40 H40 120.5 . . ? C36 C41 C40 120.9(5) . . ? C36 C41 H41 119.6 . . ? C40 C41 H41 119.6 . . ? C43 C42 C47 119.0(3) . . ? C43 C42 P1 121.0(3) . . ? C47 C42 P1 120.0(3) . . ? C42 C43 C44 120.6(4) . . ? C42 C43 H43 119.7 . . ? C44 C43 H43 119.7 . . ? C45 C44 C43 120.1(4) . . ? C45 C44 H44 119.9 . . ? C43 C44 H44 119.9 . . ? C44 C45 C46 119.5(4) . . ? C44 C45 H45 120.3 . . ? C46 C45 H45 120.3 . . ? C47 C46 C45 120.9(4) . . ? C47 C46 H46 119.5 . . ? C45 C46 H46 119.5 . . ? C46 C47 C42 119.9(4) . . ? C46 C47 H47 120.0 . . ? C42 C47 H47 120.0 . . ? C1S O1S O1S 122.7(12) . 2_666 ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 26.50 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.880 _refine_diff_density_min -0.458 _refine_diff_density_rms 0.083