# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Georgii Nikonov' _publ_contact_author_email GNIKONOV@BROCKU.CA _publ_section_title ; Unexpected effect of the ring on the extent of Si...H interligand interactions in half-sandwich silyl hydrides of ruthenium ; loop_ _publ_author_name 'Georgii Nikonov' 'Dmitry V Gutsulyak' 'Judith A K Howard' 'Lyudmila G Kuzmina' 'Alexander L Osipov' # Attachment 'all_cifs_revised.cif' data_3c _database_code_depnum_ccdc_archive 'CCDC 685290' _audit_creation_method SHELXL-97 _chemical_name_systematic ;(cyclopentadienyl)(triphenylphosphine)(dimethylchlorosilyl) ruthenium dihydride ; _chemical_name_common ;(cyclopentadienyl)(triphenylphosphine)(dimethylchlorosilyl) ruthenium dihydride ; _chemical_melting_point ? _chemical_formula_moiety 'C25 H28 Cl P Ru Si' _chemical_formula_sum 'C25 H28 Cl P Ru Si' _chemical_formula_weight 524.05 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.7357(2) _cell_length_b 11.5961(2) _cell_length_c 11.9794(2) _cell_angle_alpha 73.7570(10) _cell_angle_beta 86.0050(10) _cell_angle_gamma 82.2760(10) _cell_volume 1153.85(4) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 5340 _cell_measurement_theta_min 2.811 _cell_measurement_theta_max 30.506 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.46 _exptl_crystal_size_mid 0.42 _exptl_crystal_size_min 0.38 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.508 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 536 _exptl_absorpt_coefficient_mu 0.926 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6753 _exptl_absorpt_correction_T_max 0.7198 _exptl_absorpt_process_details 'SADABS (Bruker, 2004)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART-6K' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 11526 _diffrn_reflns_av_R_equivalents 0.0131 _diffrn_reflns_av_sigmaI/netI 0.0187 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.77 _diffrn_reflns_theta_max 29.00 _reflns_number_total 6037 _reflns_number_gt 5783 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0263P)^2^+0.5628P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0046(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 6037 _refine_ls_number_parameters 271 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0203 _refine_ls_R_factor_gt 0.0194 _refine_ls_wR_factor_ref 0.0529 _refine_ls_wR_factor_gt 0.0525 _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_restrained_S_all 1.063 _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 0.320714(11) 0.833635(8) 0.297149(8) 0.01443(4) Uani 1 1 d . . . P1 P 0.40831(4) 0.71435(3) 0.17855(3) 0.01331(7) Uani 1 1 d . . . Si1 Si 0.11340(4) 0.74350(3) 0.40846(3) 0.01578(7) Uani 1 1 d . . . Cl1 Cl -0.08207(4) 0.87939(3) 0.40171(3) 0.02653(8) Uani 1 1 d . . . C1 C 0.2787(2) 0.98291(14) 0.38430(14) 0.0285(3) Uani 1 1 d . . . H1A H 0.1943 0.9924 0.4430 0.034 Uiso 1 1 calc R . . C2 C 0.4308(2) 0.92401(14) 0.40870(14) 0.0290(3) Uani 1 1 d . . . H2A H 0.4713 0.8836 0.4880 0.035 Uiso 1 1 calc R . . C3 C 0.51794(18) 0.93807(13) 0.30274(15) 0.0266(3) Uani 1 1 d . . . H3A H 0.6304 0.9100 0.2941 0.032 Uiso 1 1 calc R . . C4 C 0.41949(19) 1.00893(13) 0.21117(14) 0.0251(3) Uani 1 1 d . . . H4A H 0.4509 1.0383 0.1271 0.030 Uiso 1 1 calc R . . C5 C 0.27322(19) 1.03626(13) 0.26181(14) 0.0257(3) Uani 1 1 d . . . H5A H 0.1830 1.0885 0.2195 0.031 Uiso 1 1 calc R . . C6 C 0.02066(18) 0.62567(13) 0.36833(13) 0.0235(3) Uani 1 1 d . . . H6A H -0.0628 0.5997 0.4251 0.035 Uiso 1 1 calc R . . H6B H 0.0979 0.5561 0.3681 0.035 Uiso 1 1 calc R . . H6C H -0.0218 0.6593 0.2907 0.035 Uiso 1 1 calc R . . C7 C 0.14472(17) 0.68974(14) 0.57154(12) 0.0230(3) Uani 1 1 d . . . H7A H 0.0539 0.6535 0.6116 0.034 Uiso 1 1 calc R . . H7B H 0.1602 0.7587 0.5999 0.034 Uiso 1 1 calc R . . H7C H 0.2361 0.6293 0.5870 0.034 Uiso 1 1 calc R . . C8 C 0.33627(15) 0.76372(11) 0.02967(11) 0.0149(2) Uani 1 1 d . . . C9 C 0.22876(15) 0.86655(12) -0.00369(12) 0.0170(2) Uani 1 1 d . . . H9A H 0.1906 0.9092 0.0516 0.020 Uiso 1 1 calc R . . C10 C 0.17673(16) 0.90742(12) -0.11714(12) 0.0197(3) Uani 1 1 d . . . H10A H 0.1041 0.9779 -0.1390 0.024 Uiso 1 1 calc R . . C11 C 0.23125(18) 0.84507(12) -0.19803(12) 0.0215(3) Uani 1 1 d . . . H11A H 0.1941 0.8716 -0.2748 0.026 Uiso 1 1 calc R . . C12 C 0.34049(18) 0.74342(13) -0.16659(12) 0.0220(3) Uani 1 1 d . . . H12A H 0.3786 0.7012 -0.2222 0.026 Uiso 1 1 calc R . . C13 C 0.39378(16) 0.70370(12) -0.05393(12) 0.0190(2) Uani 1 1 d . . . H13A H 0.4698 0.6353 -0.0334 0.023 Uiso 1 1 calc R . . C14 C 0.61612(15) 0.69654(11) 0.13953(11) 0.0157(2) Uani 1 1 d . . . C15 C 0.68733(16) 0.80141(12) 0.09058(13) 0.0206(3) Uani 1 1 d . . . H15A H 0.6321 0.8783 0.0885 0.025 Uiso 1 1 calc R . . C16 C 0.83759(16) 0.79412(13) 0.04508(13) 0.0229(3) Uani 1 1 d . . . H16A H 0.8840 0.8660 0.0115 0.027 Uiso 1 1 calc R . . C17 C 0.92064(16) 0.68250(13) 0.04819(13) 0.0223(3) Uani 1 1 d . . . H17A H 1.0227 0.6779 0.0153 0.027 Uiso 1 1 calc R . . C18 C 0.85315(16) 0.57762(13) 0.09987(14) 0.0230(3) Uani 1 1 d . . . H18A H 0.9104 0.5008 0.1046 0.028 Uiso 1 1 calc R . . C19 C 0.70172(16) 0.58477(12) 0.14476(13) 0.0207(3) Uani 1 1 d . . . H19A H 0.6563 0.5126 0.1794 0.025 Uiso 1 1 calc R . . C20 C 0.36911(15) 0.55632(11) 0.23434(11) 0.0154(2) Uani 1 1 d . . . C21 C 0.42148(16) 0.49194(12) 0.34529(12) 0.0195(3) Uani 1 1 d . . . H21A H 0.4815 0.5290 0.3855 0.023 Uiso 1 1 calc R . . C22 C 0.38696(18) 0.37498(12) 0.39714(13) 0.0230(3) Uani 1 1 d . . . H22A H 0.4223 0.3330 0.4726 0.028 Uiso 1 1 calc R . . C23 C 0.30057(18) 0.31928(12) 0.33843(13) 0.0240(3) Uani 1 1 d . . . H23A H 0.2752 0.2398 0.3742 0.029 Uiso 1 1 calc R . . C24 C 0.25195(17) 0.38058(12) 0.22757(13) 0.0222(3) Uani 1 1 d . . . H24A H 0.1950 0.3421 0.1866 0.027 Uiso 1 1 calc R . . C25 C 0.28592(16) 0.49858(12) 0.17540(12) 0.0180(2) Uani 1 1 d . . . H25A H 0.2521 0.5396 0.0993 0.022 Uiso 1 1 calc R . . H1 H 0.355(2) 0.7106(18) 0.3826(17) 0.032(5) Uiso 1 1 d . . . H2 H 0.172(2) 0.8252(18) 0.2392(18) 0.034(5) 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 Ru1 0.01597(6) 0.01253(6) 0.01600(6) -0.00571(4) 0.00069(4) -0.00263(4) P1 0.01343(14) 0.01172(14) 0.01515(14) -0.00438(11) 0.00049(11) -0.00174(11) Si1 0.01678(17) 0.01655(16) 0.01431(16) -0.00493(12) 0.00083(12) -0.00228(13) Cl1 0.02276(16) 0.02545(17) 0.02824(17) -0.00668(13) 0.00415(13) 0.00410(13) C1 0.0387(9) 0.0212(7) 0.0321(8) -0.0177(6) 0.0051(6) -0.0070(6) C2 0.0422(9) 0.0215(7) 0.0290(8) -0.0125(6) -0.0080(7) -0.0088(6) C3 0.0239(7) 0.0210(6) 0.0391(8) -0.0123(6) -0.0031(6) -0.0084(5) C4 0.0305(8) 0.0160(6) 0.0298(7) -0.0061(5) 0.0025(6) -0.0091(5) C5 0.0292(7) 0.0148(6) 0.0347(8) -0.0100(5) -0.0008(6) -0.0019(5) C6 0.0239(7) 0.0249(7) 0.0246(7) -0.0096(5) 0.0043(5) -0.0096(5) C7 0.0231(7) 0.0294(7) 0.0142(6) -0.0014(5) 0.0000(5) -0.0051(5) C8 0.0141(5) 0.0145(5) 0.0163(6) -0.0038(4) 0.0008(4) -0.0038(4) C9 0.0162(6) 0.0155(5) 0.0194(6) -0.0052(5) 0.0014(5) -0.0020(4) C10 0.0194(6) 0.0175(6) 0.0209(6) -0.0029(5) -0.0022(5) -0.0017(5) C11 0.0275(7) 0.0193(6) 0.0177(6) -0.0028(5) -0.0035(5) -0.0055(5) C12 0.0302(7) 0.0192(6) 0.0178(6) -0.0072(5) 0.0009(5) -0.0041(5) C13 0.0211(6) 0.0161(6) 0.0195(6) -0.0054(5) 0.0004(5) -0.0007(5) C14 0.0133(5) 0.0166(6) 0.0178(6) -0.0059(4) -0.0004(4) -0.0017(4) C15 0.0179(6) 0.0158(6) 0.0269(7) -0.0052(5) 0.0024(5) -0.0012(5) C16 0.0175(6) 0.0212(6) 0.0293(7) -0.0056(5) 0.0029(5) -0.0048(5) C17 0.0145(6) 0.0264(7) 0.0271(7) -0.0100(6) 0.0007(5) -0.0014(5) C18 0.0179(6) 0.0196(6) 0.0320(7) -0.0101(5) -0.0003(5) 0.0020(5) C19 0.0179(6) 0.0165(6) 0.0281(7) -0.0074(5) 0.0006(5) -0.0017(5) C20 0.0156(6) 0.0131(5) 0.0177(6) -0.0051(4) 0.0019(4) -0.0017(4) C21 0.0231(6) 0.0159(6) 0.0196(6) -0.0053(5) -0.0021(5) -0.0013(5) C22 0.0300(7) 0.0164(6) 0.0204(6) -0.0020(5) -0.0014(5) -0.0010(5) C23 0.0290(7) 0.0136(6) 0.0280(7) -0.0033(5) 0.0034(6) -0.0054(5) C24 0.0233(7) 0.0171(6) 0.0284(7) -0.0079(5) -0.0003(5) -0.0063(5) C25 0.0181(6) 0.0161(6) 0.0203(6) -0.0056(5) 0.0000(5) -0.0024(5) _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 2.2378(14) . ? Ru1 C2 2.2454(14) . ? Ru1 C3 2.2499(14) . ? Ru1 C5 2.2535(14) . ? Ru1 C4 2.2614(14) . ? Ru1 P1 2.2762(3) . ? Ru1 Si1 2.3544(4) . ? Ru1 H1 1.51(2) . ? Ru1 H2 1.54(2) . ? P1 C20 1.8368(13) . ? P1 C14 1.8416(13) . ? P1 C8 1.8420(13) . ? Si1 C6 1.8638(14) . ? Si1 C7 1.9046(14) . ? Si1 Cl1 2.1518(5) . ? C1 C2 1.419(2) . ? C1 C5 1.426(2) . ? C1 H1A 1.0000 . ? C2 C3 1.414(2) . ? C2 H2A 1.0000 . ? C3 C4 1.434(2) . ? C3 H3A 1.0000 . ? C4 C5 1.411(2) . ? C4 H4A 1.0000 . ? C5 H5A 1.0000 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 C9 1.3958(18) . ? C8 C13 1.4020(18) . ? C9 C10 1.3951(19) . ? C9 H9A 0.9500 . ? C10 C11 1.387(2) . ? C10 H10A 0.9500 . ? C11 C12 1.393(2) . ? C11 H11A 0.9500 . ? C12 C13 1.3900(19) . ? C12 H12A 0.9500 . ? C13 H13A 0.9500 . ? C14 C19 1.3942(18) . ? C14 C15 1.4012(18) . ? C15 C16 1.3869(19) . ? C15 H15A 0.9500 . ? C16 C17 1.388(2) . ? C16 H16A 0.9500 . ? C17 C18 1.389(2) . ? C17 H17A 0.9500 . ? C18 C19 1.394(2) . ? C18 H18A 0.9500 . ? C19 H19A 0.9500 . ? C20 C25 1.3935(17) . ? C20 C21 1.4040(18) . ? C21 C22 1.3888(19) . ? C21 H21A 0.9500 . ? C22 C23 1.393(2) . ? C22 H22A 0.9500 . ? C23 C24 1.385(2) . ? C23 H23A 0.9500 . ? C24 C25 1.3985(18) . ? C24 H24A 0.9500 . ? C25 H25A 0.9500 . ? 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 36.92(6) . . ? C1 Ru1 C3 61.72(6) . . ? C2 Ru1 C3 36.68(6) . . ? C1 Ru1 C5 37.01(6) . . ? C2 Ru1 C5 61.30(6) . . ? C3 Ru1 C5 61.40(6) . . ? C1 Ru1 C4 61.54(6) . . ? C2 Ru1 C4 61.32(6) . . ? C3 Ru1 C4 37.06(6) . . ? C5 Ru1 C4 36.43(6) . . ? C1 Ru1 P1 164.66(4) . . ? C2 Ru1 P1 135.43(5) . . ? C3 Ru1 P1 104.96(4) . . ? C5 Ru1 P1 131.50(4) . . ? C4 Ru1 P1 103.36(4) . . ? C1 Ru1 Si1 89.43(4) . . ? C2 Ru1 Si1 106.75(5) . . ? C3 Ru1 Si1 143.35(4) . . ? C5 Ru1 Si1 109.46(4) . . ? C4 Ru1 Si1 145.87(4) . . ? P1 Ru1 Si1 105.760(12) . . ? C1 Ru1 H1 112.5(8) . . ? C2 Ru1 H1 91.9(8) . . ? C3 Ru1 H1 106.6(8) . . ? C5 Ru1 H1 149.4(8) . . ? C4 Ru1 H1 143.3(8) . . ? P1 Ru1 H1 77.5(8) . . ? Si1 Ru1 H1 61.9(8) . . ? C1 Ru1 H2 109.6(8) . . ? C2 Ru1 H2 146.4(8) . . ? C3 Ru1 H2 148.7(8) . . ? C5 Ru1 H2 93.1(8) . . ? C4 Ru1 H2 111.7(8) . . ? P1 Ru1 H2 77.5(8) . . ? Si1 Ru1 H2 59.0(8) . . ? H1 Ru1 H2 104.4(11) . . ? C20 P1 C14 101.89(6) . . ? C20 P1 C8 104.77(6) . . ? C14 P1 C8 97.57(6) . . ? C20 P1 Ru1 114.56(4) . . ? C14 P1 Ru1 119.10(4) . . ? C8 P1 Ru1 116.42(4) . . ? C6 Si1 C7 107.60(7) . . ? C6 Si1 Cl1 100.17(5) . . ? C7 Si1 Cl1 100.76(5) . . ? C6 Si1 Ru1 121.87(5) . . ? C7 Si1 Ru1 114.36(5) . . ? Cl1 Si1 Ru1 109.091(18) . . ? C2 C1 C5 107.43(14) . . ? C2 C1 Ru1 71.83(8) . . ? C5 C1 Ru1 72.09(8) . . ? C2 C1 H1A 126.1 . . ? C5 C1 H1A 126.1 . . ? Ru1 C1 H1A 126.1 . . ? C3 C2 C1 108.65(14) . . ? C3 C2 Ru1 71.83(8) . . ? C1 C2 Ru1 71.25(8) . . ? C3 C2 H2A 125.6 . . ? C1 C2 H2A 125.6 . . ? Ru1 C2 H2A 125.6 . . ? C2 C3 C4 107.59(14) . . ? C2 C3 Ru1 71.49(8) . . ? C4 C3 Ru1 71.91(8) . . ? C2 C3 H3A 126.1 . . ? C4 C3 H3A 126.1 . . ? Ru1 C3 H3A 126.1 . . ? C5 C4 C3 107.83(14) . . ? C5 C4 Ru1 71.48(8) . . ? C3 C4 Ru1 71.04(8) . . ? C5 C4 H4A 126.0 . . ? C3 C4 H4A 126.0 . . ? Ru1 C4 H4A 126.0 . . ? C4 C5 C1 108.47(14) . . ? C4 C5 Ru1 72.09(8) . . ? C1 C5 Ru1 70.90(8) . . ? C4 C5 H5A 125.7 . . ? C1 C5 H5A 125.7 . . ? Ru1 C5 H5A 125.7 . . ? 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 . . ? 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 . . ? C9 C8 C13 118.64(12) . . ? C9 C8 P1 120.08(10) . . ? C13 C8 P1 121.19(10) . . ? C10 C9 C8 120.82(12) . . ? C10 C9 H9A 119.6 . . ? C8 C9 H9A 119.6 . . ? C11 C10 C9 119.89(13) . . ? C11 C10 H10A 120.1 . . ? C9 C10 H10A 120.1 . . ? C10 C11 C12 119.96(13) . . ? C10 C11 H11A 120.0 . . ? C12 C11 H11A 120.0 . . ? C13 C12 C11 120.09(13) . . ? C13 C12 H12A 120.0 . . ? C11 C12 H12A 120.0 . . ? C12 C13 C8 120.56(13) . . ? C12 C13 H13A 119.7 . . ? C8 C13 H13A 119.7 . . ? C19 C14 C15 118.36(12) . . ? C19 C14 P1 123.26(10) . . ? C15 C14 P1 118.02(10) . . ? C16 C15 C14 120.69(13) . . ? C16 C15 H15A 119.7 . . ? C14 C15 H15A 119.7 . . ? C15 C16 C17 120.50(13) . . ? C15 C16 H16A 119.7 . . ? C17 C16 H16A 119.7 . . ? C16 C17 C18 119.38(13) . . ? C16 C17 H17A 120.3 . . ? C18 C17 H17A 120.3 . . ? C17 C18 C19 120.20(13) . . ? C17 C18 H18A 119.9 . . ? C19 C18 H18A 119.9 . . ? C18 C19 C14 120.82(12) . . ? C18 C19 H19A 119.6 . . ? C14 C19 H19A 119.6 . . ? C25 C20 C21 118.40(12) . . ? C25 C20 P1 124.06(10) . . ? C21 C20 P1 117.48(9) . . ? C22 C21 C20 121.02(13) . . ? C22 C21 H21A 119.5 . . ? C20 C21 H21A 119.5 . . ? C21 C22 C23 120.00(13) . . ? C21 C22 H22A 120.0 . . ? C23 C22 H22A 120.0 . . ? C24 C23 C22 119.52(13) . . ? C24 C23 H23A 120.2 . . ? C22 C23 H23A 120.2 . . ? C23 C24 C25 120.58(13) . . ? C23 C24 H24A 119.7 . . ? C25 C24 H24A 119.7 . . ? C20 C25 C24 120.43(13) . . ? C20 C25 H25A 119.8 . . ? C24 C25 H25A 119.8 . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 29.00 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.422 _refine_diff_density_min -0.463 _refine_diff_density_rms 0.061 #==end data_3e _database_code_depnum_ccdc_archive 'CCDC 685291' _audit_creation_method SHELXL-97 _chemical_name_systematic ; (cyclopentadienyl)(diisopropylphenylphosphine)(dimethylchlorosilyl) ruthenium dihydride ; _chemical_name_common ; (cyclopentadienyl)(diisopropylphenylphosphine)(dimethylchloros ilyl) ruthenium dihydride ; _chemical_melting_point ? _chemical_formula_moiety 'C19 H32 Cl P Ru Si' _chemical_formula_sum 'C19 H32 Cl P Ru Si' _chemical_formula_weight 456.03 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.7462(1) _cell_length_b 16.4554(3) _cell_length_c 29.3627(5) _cell_angle_alpha 90.00 _cell_angle_beta 92.351(1) _cell_angle_gamma 90.00 _cell_volume 4222.39(12) _cell_formula_units_Z 8 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 9570 _cell_measurement_theta_min 2.331 _cell_measurement_theta_max 59.985 _exptl_crystal_description yellow _exptl_crystal_colour block _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.435 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1888 _exptl_absorpt_coefficient_mu 1.000 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7148 _exptl_absorpt_correction_T_max 0.9243 _exptl_absorpt_process_details 'SADABS (Bruker, 2004)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 37465 _diffrn_reflns_av_R_equivalents 0.0490 _diffrn_reflns_av_sigmaI/netI 0.0505 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -37 _diffrn_reflns_limit_l_max 39 _diffrn_reflns_theta_min 1.39 _diffrn_reflns_theta_max 28.50 _reflns_number_total 10680 _reflns_number_gt 7708 _reflns_threshold_expression I>2\s(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0325P)^2^+3.1047P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10680 _refine_ls_number_parameters 431 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0653 _refine_ls_R_factor_gt 0.0383 _refine_ls_wR_factor_ref 0.0857 _refine_ls_wR_factor_gt 0.0795 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.022 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.21832(2) 0.699756(15) 0.151303(7) 0.01453(6) Uani 1 1 d . . . Ru2 Ru -0.58221(2) 1.201788(16) 0.145658(9) 0.02155(7) Uani 1 1 d . . . P1 P 0.06265(8) 0.60362(5) 0.11699(2) 0.01520(14) Uani 1 1 d . . . P2 P -0.43458(8) 1.09685(5) 0.12087(3) 0.01651(15) Uani 1 1 d . . . Si1 Si 0.05880(9) 0.80840(5) 0.16745(3) 0.01991(17) Uani 1 1 d . . . Si2 Si -0.43017(9) 1.31785(5) 0.14353(3) 0.02154(18) Uani 1 1 d . . . Cl1 Cl 0.09102(10) 0.91192(5) 0.12342(4) 0.0378(2) Uani 1 1 d . . . Cl2 Cl -0.49160(11) 1.40164(6) 0.08913(3) 0.0388(2) Uani 1 1 d . . . C1 C 0.4317(3) 0.7699(2) 0.16806(12) 0.0266(7) Uani 1 1 d . . . H1A H 0.4395 0.8304 0.1707 0.032 Uiso 1 1 calc R . . C2 C 0.4601(3) 0.7233(2) 0.12857(11) 0.0253(7) Uani 1 1 d . . . H2A H 0.4884 0.7453 0.0983 0.030 Uiso 1 1 calc R . . C3 C 0.4518(3) 0.6405(2) 0.14060(12) 0.0274(7) Uani 1 1 d . . . H3A H 0.4712 0.5934 0.1201 0.033 Uiso 1 1 calc R . . C4 C 0.4171(3) 0.6355(2) 0.18698(12) 0.0272(7) Uani 1 1 d . . . H4A H 0.4111 0.5845 0.2053 0.033 Uiso 1 1 calc R . . C5 C 0.4055(3) 0.7157(2) 0.20405(11) 0.0267(7) Uani 1 1 d . . . H5A H 0.3924 0.7310 0.2366 0.032 Uiso 1 1 calc R . . C14 C -0.1029(3) 0.63395(19) 0.08004(10) 0.0183(6) Uani 1 1 d . . . C19 C -0.1006(3) 0.7067(2) 0.05571(11) 0.0272(7) Uani 1 1 d . . . H19A H -0.0165 0.7426 0.0604 0.033 Uiso 1 1 calc R . . C18 C -0.2187(4) 0.7278(2) 0.02473(12) 0.0332(8) Uani 1 1 d . . . H18A H -0.2151 0.7779 0.0087 0.040 Uiso 1 1 calc R . . C17 C -0.3422(4) 0.6754(2) 0.01736(12) 0.0325(8) Uani 1 1 d . . . H17A H -0.4229 0.6892 -0.0039 0.039 Uiso 1 1 calc R . . C16 C -0.3463(3) 0.6036(2) 0.04094(11) 0.0258(7) Uani 1 1 d . . . H16A H -0.4302 0.5676 0.0359 0.031 Uiso 1 1 calc R . . C15 C -0.2288(3) 0.5829(2) 0.07217(11) 0.0230(6) Uani 1 1 d . . . H15A H -0.2343 0.5332 0.0884 0.028 Uiso 1 1 calc R . . C11 C -0.0207(3) 0.52913(18) 0.15620(10) 0.0203(6) Uani 1 1 d . . . H11A H -0.0774 0.4876 0.1373 0.024 Uiso 1 1 calc R . . C13 C -0.1339(4) 0.5676(2) 0.18834(11) 0.0278(7) Uani 1 1 d . . . H13A H -0.1743 0.5256 0.2082 0.042 Uiso 1 1 calc R . . H13B H -0.2185 0.5925 0.1704 0.042 Uiso 1 1 calc R . . H13C H -0.0815 0.6093 0.2070 0.042 Uiso 1 1 calc R . . C12 C 0.1072(4) 0.4855(2) 0.18359(12) 0.0290(7) Uani 1 1 d . . . H12A H 0.0624 0.4461 0.2043 0.043 Uiso 1 1 calc R . . H12C H 0.1678 0.5253 0.2014 0.043 Uiso 1 1 calc R . . H12D H 0.1734 0.4570 0.1627 0.043 Uiso 1 1 calc R . . C8 C 0.1681(3) 0.53782(19) 0.07722(10) 0.0201(6) Uani 1 1 d . . . H8A H 0.2616 0.5177 0.0944 0.024 Uiso 1 1 calc R . . C10 C 0.2234(3) 0.5885(2) 0.03709(10) 0.0252(7) Uani 1 1 d . . . H10A H 0.2787 0.5533 0.0164 0.038 Uiso 1 1 calc R . . H10C H 0.2918 0.6316 0.0487 0.038 Uiso 1 1 calc R . . H10D H 0.1351 0.6128 0.0206 0.038 Uiso 1 1 calc R . . C9 C 0.0809(3) 0.4626(2) 0.05945(11) 0.0256(7) Uani 1 1 d . . . H9A H 0.1452 0.4320 0.0389 0.038 Uiso 1 1 calc R . . H9B H -0.0132 0.4796 0.0429 0.038 Uiso 1 1 calc R . . H9C H 0.0550 0.4280 0.0852 0.038 Uiso 1 1 calc R . . C7 C -0.1548(3) 0.7982(2) 0.16356(13) 0.0348(8) Uani 1 1 d . . . H7A H -0.2017 0.8501 0.1716 0.052 Uiso 1 1 calc R . . H7B H -0.1866 0.7560 0.1847 0.052 Uiso 1 1 calc R . . H7C H -0.1877 0.7832 0.1324 0.052 Uiso 1 1 calc R . . C6 C 0.1038(5) 0.8579(3) 0.22364(14) 0.0494(12) Uani 1 1 d . . . H6A H 0.0324 0.9028 0.2281 0.074 Uiso 1 1 calc R . . H6B H 0.2088 0.8789 0.2242 0.074 Uiso 1 1 calc R . . H6C H 0.0940 0.8180 0.2481 0.074 Uiso 1 1 calc R . . C1A C -0.7512(5) 1.2452(4) 0.19409(18) 0.0634(16) Uani 1 1 d . . . H1AA H -0.7294 1.2827 0.2203 0.076 Uiso 1 1 calc R . . C2A C -0.8021(4) 1.2678(3) 0.15138(18) 0.0523(12) Uani 1 1 d . . . H2AA H -0.8238 1.3246 0.1409 0.063 Uiso 1 1 calc R . . C3A C -0.8340(4) 1.1977(4) 0.1268(2) 0.0739(19) Uani 1 1 d . . . H3AA H -0.8793 1.1959 0.0950 0.089 Uiso 1 1 calc R . . C4A C -0.8032(6) 1.1326(3) 0.1533(4) 0.108(3) Uani 1 1 d . . . H4AA H -0.8219 1.0746 0.1445 0.129 Uiso 1 1 calc R . . C5A C -0.7506(6) 1.1604(5) 0.1961(3) 0.099(3) Uani 1 1 d . . . H5AA H -0.7280 1.1263 0.2238 0.118 Uiso 1 1 calc R . . C14A C -0.2932(3) 1.11487(18) 0.07731(10) 0.0179(6) Uani 1 1 d . . . C19A C -0.3237(4) 1.1707(2) 0.04238(11) 0.0258(7) Uani 1 1 d . . . H19B H -0.4116 1.2045 0.0433 0.031 Uiso 1 1 calc R . . C18A C -0.2265(4) 1.1775(2) 0.00602(12) 0.0327(8) Uani 1 1 d . . . H18B H -0.2491 1.2153 -0.0177 0.039 Uiso 1 1 calc R . . C17A C -0.0976(4) 1.1292(2) 0.00455(12) 0.0299(8) Uani 1 1 d . . . H17B H -0.0320 1.1333 -0.0204 0.036 Uiso 1 1 calc R . . C16A C -0.0647(3) 1.0754(2) 0.03910(11) 0.0271(7) Uani 1 1 d . . . H16B H 0.0251 1.0431 0.0383 0.032 Uiso 1 1 calc R . . C15A C -0.1610(3) 1.06761(19) 0.07531(11) 0.0214(6) Uani 1 1 d . . . H15B H -0.1367 1.0297 0.0989 0.026 Uiso 1 1 calc R . . C11A C -0.3235(4) 1.0407(2) 0.16597(10) 0.0233(6) Uani 1 1 d . . . H11B H -0.2721 0.9941 0.1510 0.028 Uiso 1 1 calc R . . C13A C -0.1984(3) 1.0926(2) 0.18960(11) 0.0282(7) Uani 1 1 d . . . H13D H -0.1436 1.0601 0.2130 0.042 Uiso 1 1 calc R . . H13E H -0.2450 1.1398 0.2039 0.042 Uiso 1 1 calc R . . H13F H -0.1264 1.1110 0.1671 0.042 Uiso 1 1 calc R . . C12A C -0.4298(4) 1.0055(2) 0.20090(12) 0.0345(8) Uani 1 1 d . . . H12B H -0.3692 0.9761 0.2244 0.052 Uiso 1 1 calc R . . H12E H -0.5025 0.9681 0.1857 0.052 Uiso 1 1 calc R . . H12F H -0.4860 1.0497 0.2151 0.052 Uiso 1 1 calc R . . C8A C -0.5503(3) 1.01479(19) 0.09230(11) 0.0225(6) Uani 1 1 d . . . H8AA H -0.6323 0.9997 0.1135 0.027 Uiso 1 1 calc R . . C10A C -0.6305(4) 1.0466(2) 0.04887(12) 0.0311(8) Uani 1 1 d . . . H10B H -0.6906 1.0028 0.0343 0.047 Uiso 1 1 calc R . . H10E H -0.5539 1.0659 0.0280 0.047 Uiso 1 1 calc R . . H10F H -0.6985 1.0916 0.0564 0.047 Uiso 1 1 calc R . . C9A C -0.4625(4) 0.9363(2) 0.08210(12) 0.0284(7) Uani 1 1 d . . . H9AA H -0.5324 0.8970 0.0672 0.043 Uiso 1 1 calc R . . H9AB H -0.4202 0.9131 0.1107 0.043 Uiso 1 1 calc R . . H9AC H -0.3790 0.9486 0.0619 0.043 Uiso 1 1 calc R . . C7A C -0.2194(3) 1.3089(2) 0.13664(13) 0.0319(8) Uani 1 1 d . . . H7AA H -0.1737 1.3632 0.1365 0.048 Uiso 1 1 calc R . . H7AB H -0.2004 1.2813 0.1078 0.048 Uiso 1 1 calc R . . H7AC H -0.1737 1.2773 0.1620 0.048 Uiso 1 1 calc R . . C6A C -0.4580(4) 1.3888(2) 0.19359(12) 0.0296(7) Uani 1 1 d . . . H6AA H -0.3915 1.4363 0.1909 0.044 Uiso 1 1 calc R . . H6AB H -0.4318 1.3602 0.2221 0.044 Uiso 1 1 calc R . . H6AC H -0.5650 1.4064 0.1935 0.044 Uiso 1 1 calc R . . H2 H 0.150(4) 0.740(2) 0.1102(12) 0.040(11) Uiso 1 1 d . . . H1 H 0.099(5) 0.688(3) 0.1884(15) 0.062(14) Uiso 1 1 d . . . H3 H -0.448(4) 1.204(3) 0.1816(14) 0.051(12) Uiso 1 1 d . . . H4 H -0.546(4) 1.226(2) 0.0983(12) 0.038(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 Ru1 0.01219(10) 0.01441(11) 0.01701(11) -0.00030(9) 0.00100(7) -0.00017(9) Ru2 0.01344(11) 0.01932(13) 0.03225(15) -0.00449(11) 0.00529(9) -0.00036(9) P1 0.0129(3) 0.0156(4) 0.0171(4) 0.0007(3) 0.0006(2) -0.0005(3) P2 0.0147(3) 0.0152(4) 0.0198(4) 0.0003(3) 0.0030(3) -0.0016(3) Si1 0.0179(4) 0.0174(4) 0.0244(4) -0.0034(3) 0.0010(3) 0.0027(3) Si2 0.0175(4) 0.0156(4) 0.0313(5) -0.0030(3) -0.0020(3) 0.0008(3) Cl1 0.0342(4) 0.0192(4) 0.0608(6) 0.0104(4) 0.0098(4) 0.0038(3) Cl2 0.0459(5) 0.0257(4) 0.0440(5) 0.0066(4) -0.0092(4) -0.0007(4) C1 0.0156(13) 0.0233(17) 0.041(2) -0.0055(15) -0.0004(12) -0.0049(12) C2 0.0124(13) 0.0336(19) 0.0301(18) -0.0004(14) 0.0045(11) -0.0048(12) C3 0.0118(13) 0.0315(19) 0.039(2) -0.0091(15) -0.0010(12) -0.0007(12) C4 0.0163(14) 0.0315(19) 0.0330(19) 0.0084(15) -0.0065(12) 0.0037(13) C5 0.0147(13) 0.042(2) 0.0227(16) -0.0061(14) -0.0021(11) -0.0018(13) C14 0.0128(12) 0.0220(16) 0.0203(15) -0.0010(12) 0.0014(10) 0.0013(11) C19 0.0222(14) 0.0287(18) 0.0301(18) 0.0061(15) -0.0043(12) -0.0027(13) C18 0.0310(17) 0.034(2) 0.033(2) 0.0094(16) -0.0090(14) 0.0045(15) C17 0.0227(15) 0.046(2) 0.0283(18) -0.0025(16) -0.0082(13) 0.0094(15) C16 0.0125(12) 0.0356(19) 0.0292(17) -0.0075(15) -0.0019(11) 0.0009(13) C15 0.0173(13) 0.0270(17) 0.0249(16) -0.0038(13) 0.0035(11) 0.0000(12) C11 0.0208(14) 0.0167(15) 0.0235(16) 0.0027(12) 0.0012(11) -0.0035(11) C13 0.0262(16) 0.0304(19) 0.0273(18) 0.0032(14) 0.0093(13) -0.0064(14) C12 0.0320(17) 0.0228(17) 0.0319(19) 0.0107(14) -0.0002(13) 0.0015(14) C8 0.0158(13) 0.0200(15) 0.0242(16) -0.0057(12) -0.0016(11) 0.0020(11) C10 0.0193(14) 0.0334(19) 0.0230(16) -0.0053(14) 0.0028(11) -0.0026(13) C9 0.0259(15) 0.0226(17) 0.0282(18) -0.0092(13) 0.0009(12) 0.0008(13) C7 0.0216(15) 0.0293(19) 0.054(2) -0.0001(18) 0.0099(14) 0.0044(15) C6 0.051(2) 0.057(3) 0.040(2) -0.028(2) -0.0102(18) 0.027(2) C1A 0.033(2) 0.102(5) 0.057(3) -0.037(3) 0.024(2) -0.006(3) C2A 0.0190(17) 0.049(3) 0.090(4) -0.011(2) 0.0146(19) 0.0093(17) C3A 0.0103(16) 0.121(5) 0.091(4) -0.063(4) 0.0065(19) -0.009(2) C4A 0.039(3) 0.030(3) 0.261(10) -0.045(4) 0.080(5) -0.018(2) C5A 0.037(3) 0.131(7) 0.132(6) 0.082(5) 0.056(3) 0.027(4) C14A 0.0153(12) 0.0179(15) 0.0204(15) 0.0004(12) 0.0008(10) -0.0029(11) C19A 0.0268(15) 0.0229(16) 0.0279(18) 0.0066(13) 0.0035(13) 0.0039(13) C18A 0.0415(19) 0.0294(19) 0.0277(19) 0.0081(14) 0.0085(14) -0.0035(15) C17A 0.0298(16) 0.0298(19) 0.0311(19) -0.0047(15) 0.0133(13) -0.0107(14) C16A 0.0171(14) 0.0323(19) 0.0322(19) -0.0076(15) 0.0055(12) -0.0004(13) C15A 0.0183(13) 0.0228(16) 0.0230(16) -0.0003(12) 0.0007(11) 0.0021(12) C11A 0.0321(16) 0.0207(16) 0.0174(15) 0.0039(12) 0.0025(12) 0.0046(13) C13A 0.0262(15) 0.0324(19) 0.0255(17) 0.0017(14) -0.0046(12) 0.0057(14) C12A 0.053(2) 0.030(2) 0.0217(17) 0.0034(15) 0.0054(15) -0.0070(17) C8A 0.0186(13) 0.0229(16) 0.0264(17) -0.0035(13) 0.0049(11) -0.0060(12) C10A 0.0215(15) 0.036(2) 0.035(2) -0.0097(16) -0.0053(13) -0.0001(14) C9A 0.0380(18) 0.0186(16) 0.0288(18) -0.0030(13) 0.0027(14) -0.0045(14) C7A 0.0215(15) 0.0227(18) 0.052(2) -0.0035(16) 0.0021(14) -0.0045(13) C6A 0.0257(15) 0.0233(17) 0.039(2) -0.0122(15) -0.0066(13) 0.0045(13) _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 C5 2.223(3) . ? Ru1 C1 2.232(3) . ? Ru1 C4 2.256(3) . ? Ru1 C2 2.276(3) . ? Ru1 P1 2.2933(8) . ? Ru1 C3 2.296(3) . ? Ru1 Si1 2.3286(8) . ? Ru1 H2 1.48(4) . ? Ru1 H1 1.56(4) . ? Ru2 C1A 2.211(4) . ? Ru2 C2A 2.221(4) . ? Ru2 C5A 2.238(4) . ? Ru2 C3A 2.250(4) . ? Ru2 C4A 2.262(4) . ? Ru2 P2 2.2926(8) . ? Ru2 Si2 2.3296(9) . ? Ru2 H3 1.54(4) . ? Ru2 H4 1.49(4) . ? P1 C14 1.842(3) . ? P1 C11 1.851(3) . ? P1 C8 1.864(3) . ? P2 C14A 1.839(3) . ? P2 C11A 1.856(3) . ? P2 C8A 1.866(3) . ? Si1 C6 1.868(4) . ? Si1 C7 1.874(3) . ? Si1 H1 2.11(4) . ? Si1 Cl1 2.1638(12) . ? Si1 H2 2.20(4) . ? Si2 C7A 1.868(3) . ? Si2 C6A 1.901(3) . ? Si2 Cl2 2.1610(12) . ? Si2 H3 2.19(4) . ? Si2 H4 2.23(4) . ? C1 C5 1.408(5) . ? C1 C2 1.420(5) . ? C1 H1A 1.0000 . ? C2 C3 1.410(5) . ? C2 H2A 1.0000 . ? C3 C4 1.410(5) . ? C3 H3A 1.0000 . ? C4 C5 1.417(5) . ? C4 H4A 1.0000 . ? C5 H5A 1.0000 . ? C14 C19 1.394(4) . ? C14 C15 1.396(4) . ? C19 C18 1.392(4) . ? C19 H19A 0.9500 . ? C18 C17 1.392(5) . ? C18 H18A 0.9500 . ? C17 C16 1.370(5) . ? C17 H17A 0.9500 . ? C16 C15 1.391(4) . ? C16 H16A 0.9500 . ? C15 H15A 0.9500 . ? C11 C12 1.530(4) . ? C11 C13 1.533(4) . ? C11 H11A 1.0000 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12C 0.9800 . ? C12 H12D 0.9800 . ? C8 C9 1.534(4) . ? C8 C10 1.537(4) . ? C8 H8A 1.0000 . ? C10 H10A 0.9800 . ? C10 H10C 0.9800 . ? C10 H10D 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C1A C2A 1.366(7) . ? C1A C5A 1.396(9) . ? C1A H1AA 1.0000 . ? C2A C3A 1.382(7) . ? C2A H2AA 1.0000 . ? C3A C4A 1.343(9) . ? C3A H3AA 1.0000 . ? C4A C5A 1.399(10) . ? C4A H4AA 1.0000 . ? C5A H5AA 1.0000 . ? C14A C19A 1.395(4) . ? C14A C15A 1.396(4) . ? C19A C18A 1.396(4) . ? C19A H19B 0.9500 . ? C18A C17A 1.382(5) . ? C18A H18B 0.9500 . ? C17A C16A 1.368(5) . ? C17A H17B 0.9500 . ? C16A C15A 1.389(4) . ? C16A H16B 0.9500 . ? C15A H15B 0.9500 . ? C11A C12A 1.527(4) . ? C11A C13A 1.531(4) . ? C11A H11B 1.0000 . ? C13A H13D 0.9800 . ? C13A H13E 0.9800 . ? C13A H13F 0.9800 . ? C12A H12B 0.9800 . ? C12A H12E 0.9800 . ? C12A H12F 0.9800 . ? C8A C10A 1.523(5) . ? C8A C9A 1.539(4) . ? C8A H8AA 1.0000 . ? C10A H10B 0.9800 . ? C10A H10E 0.9800 . ? C10A H10F 0.9800 . ? C9A H9AA 0.9800 . ? C9A H9AB 0.9800 . ? C9A H9AC 0.9800 . ? C7A H7AA 0.9800 . ? C7A H7AB 0.9800 . ? C7A H7AC 0.9800 . ? C6A H6AA 0.9800 . ? C6A H6AB 0.9800 . ? C6A H6AC 0.9800 . ? 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 Ru1 C1 36.87(12) . . ? C5 Ru1 C4 36.87(12) . . ? C1 Ru1 C4 61.21(12) . . ? C5 Ru1 C2 61.16(12) . . ? C1 Ru1 C2 36.71(12) . . ? C4 Ru1 C2 60.55(12) . . ? C5 Ru1 P1 142.63(10) . . ? C1 Ru1 P1 158.37(9) . . ? C4 Ru1 P1 108.25(9) . . ? C2 Ru1 P1 122.04(9) . . ? C5 Ru1 C3 60.77(12) . . ? C1 Ru1 C3 60.63(12) . . ? C4 Ru1 C3 36.07(12) . . ? C2 Ru1 C3 35.93(12) . . ? P1 Ru1 C3 99.33(8) . . ? C5 Ru1 Si1 101.41(9) . . ? C1 Ru1 Si1 93.47(9) . . ? C4 Ru1 Si1 136.23(9) . . ? C2 Ru1 Si1 120.03(9) . . ? P1 Ru1 Si1 105.62(3) . . ? C3 Ru1 Si1 153.85(9) . . ? C5 Ru1 H2 140.9(15) . . ? C1 Ru1 H2 104.7(14) . . ? C4 Ru1 H2 150.0(14) . . ? C2 Ru1 H2 91.9(14) . . ? P1 Ru1 H2 74.8(15) . . ? C3 Ru1 H2 114.2(14) . . ? Si1 Ru1 H2 66.2(15) . . ? C5 Ru1 H1 91.4(16) . . ? C1 Ru1 H1 119.6(16) . . ? C4 Ru1 H1 98.2(16) . . ? C2 Ru1 H1 152.6(16) . . ? P1 Ru1 H1 79.3(16) . . ? C3 Ru1 H1 132.0(16) . . ? Si1 Ru1 H1 62.0(17) . . ? H2 Ru1 H1 112(2) . . ? C1A Ru2 C2A 35.89(18) . . ? C1A Ru2 C5A 36.6(2) . . ? C2A Ru2 C5A 60.2(2) . . ? C1A Ru2 C3A 59.61(17) . . ? C2A Ru2 C3A 36.01(17) . . ? C5A Ru2 C3A 59.3(2) . . ? C1A Ru2 C4A 60.2(2) . . ? C2A Ru2 C4A 59.50(18) . . ? C5A Ru2 C4A 36.2(2) . . ? C3A Ru2 C4A 34.6(2) . . ? C1A Ru2 P2 147.93(18) . . ? C2A Ru2 P2 153.27(12) . . ? C5A Ru2 P2 112.1(2) . . ? C3A Ru2 P2 117.27(14) . . ? C4A Ru2 P2 98.47(12) . . ? C1A Ru2 Si2 98.63(15) . . ? C2A Ru2 Si2 95.62(12) . . ? C5A Ru2 Si2 131.2(3) . . ? C3A Ru2 Si2 124.88(19) . . ? C4A Ru2 Si2 154.97(13) . . ? P2 Ru2 Si2 106.23(3) . . ? C1A Ru2 H3 93.6(15) . . ? C2A Ru2 H3 124.9(15) . . ? C5A Ru2 H3 93.3(15) . . ? C3A Ru2 H3 151.2(15) . . ? C4A Ru2 H3 124.9(15) . . ? P2 Ru2 H3 79.2(15) . . ? Si2 Ru2 H3 65.2(16) . . ? C1A Ru2 H4 133.4(14) . . ? C2A Ru2 H4 99.1(14) . . ? C5A Ru2 H4 150.3(14) . . ? C3A Ru2 H4 91.3(14) . . ? C4A Ru2 H4 116.1(14) . . ? P2 Ru2 H4 76.2(14) . . ? Si2 Ru2 H4 67.3(14) . . ? H3 Ru2 H4 116(2) . . ? C14 P1 C11 103.04(13) . . ? C14 P1 C8 100.69(13) . . ? C11 P1 C8 102.86(14) . . ? C14 P1 Ru1 120.66(10) . . ? C11 P1 Ru1 115.16(10) . . ? C8 P1 Ru1 112.08(9) . . ? C14A P2 C11A 103.25(13) . . ? C14A P2 C8A 99.90(13) . . ? C11A P2 C8A 102.65(15) . . ? C14A P2 Ru2 120.19(10) . . ? C11A P2 Ru2 115.68(10) . . ? C8A P2 Ru2 112.68(10) . . ? C6 Si1 C7 105.45(18) . . ? C6 Si1 H1 97.3(12) . . ? C7 Si1 H1 94.9(11) . . ? C6 Si1 Cl1 98.99(17) . . ? C7 Si1 Cl1 100.83(13) . . ? H1 Si1 Cl1 153.4(12) . . ? C6 Si1 H2 145.9(10) . . ? C7 Si1 H2 107.4(10) . . ? H1 Si1 H2 71.3(15) . . ? Cl1 Si1 H2 83.5(10) . . ? C6 Si1 Ru1 114.11(12) . . ? C7 Si1 Ru1 121.53(12) . . ? H1 Si1 Ru1 40.7(12) . . ? Cl1 Si1 Ru1 112.89(4) . . ? H2 Si1 Ru1 38.0(10) . . ? C7A Si2 C6A 106.90(15) . . ? C7A Si2 Cl2 100.78(12) . . ? C6A Si2 Cl2 98.27(12) . . ? C7A Si2 H3 94.5(10) . . ? C6A Si2 H3 96.7(11) . . ? Cl2 Si2 H3 154.4(10) . . ? C7A Si2 H4 107.9(9) . . ? C6A Si2 H4 143.9(9) . . ? Cl2 Si2 H4 84.2(10) . . ? H3 Si2 H4 71.5(14) . . ? C7A Si2 Ru2 120.31(11) . . ? C6A Si2 Ru2 113.04(12) . . ? Cl2 Si2 Ru2 114.71(4) . . ? H3 Si2 Ru2 39.8(10) . . ? H4 Si2 Ru2 38.1(9) . . ? C5 C1 C2 108.1(3) . . ? C5 C1 Ru1 71.22(17) . . ? C2 C1 Ru1 73.36(17) . . ? C5 C1 H1A 125.8 . . ? C2 C1 H1A 125.8 . . ? Ru1 C1 H1A 125.8 . . ? C3 C2 C1 107.7(3) . . ? C3 C2 Ru1 72.78(17) . . ? C1 C2 Ru1 69.93(16) . . ? C3 C2 H2A 126.1 . . ? C1 C2 H2A 126.1 . . ? Ru1 C2 H2A 126.1 . . ? C4 C3 C2 108.3(3) . . ? C4 C3 Ru1 70.43(17) . . ? C2 C3 Ru1 71.29(17) . . ? C4 C3 H3A 125.8 . . ? C2 C3 H3A 125.8 . . ? Ru1 C3 H3A 125.8 . . ? C3 C4 C5 108.0(3) . . ? C3 C4 Ru1 73.50(17) . . ? C5 C4 Ru1 70.29(17) . . ? C3 C4 H4A 125.9 . . ? C5 C4 H4A 125.9 . . ? Ru1 C4 H4A 125.9 . . ? C1 C5 C4 107.9(3) . . ? C1 C5 Ru1 71.91(17) . . ? C4 C5 Ru1 72.84(17) . . ? C1 C5 H5A 125.9 . . ? C4 C5 H5A 125.9 . . ? Ru1 C5 H5A 125.9 . . ? C19 C14 C15 117.3(3) . . ? C19 C14 P1 120.4(2) . . ? C15 C14 P1 122.0(2) . . ? C18 C19 C14 121.6(3) . . ? C18 C19 H19A 119.2 . . ? C14 C19 H19A 119.2 . . ? C19 C18 C17 119.8(3) . . ? C19 C18 H18A 120.1 . . ? C17 C18 H18A 120.1 . . ? C16 C17 C18 119.5(3) . . ? C16 C17 H17A 120.3 . . ? C18 C17 H17A 120.3 . . ? C17 C16 C15 120.7(3) . . ? C17 C16 H16A 119.7 . . ? C15 C16 H16A 119.7 . . ? C16 C15 C14 121.2(3) . . ? C16 C15 H15A 119.4 . . ? C14 C15 H15A 119.4 . . ? C12 C11 C13 110.3(3) . . ? C12 C11 P1 109.9(2) . . ? C13 C11 P1 113.0(2) . . ? C12 C11 H11A 107.8 . . ? C13 C11 H11A 107.8 . . ? P1 C11 H11A 107.8 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? C11 C12 H12D 109.5 . . ? H12A C12 H12D 109.5 . . ? H12C C12 H12D 109.5 . . ? C9 C8 C10 110.2(3) . . ? C9 C8 P1 115.5(2) . . ? C10 C8 P1 110.2(2) . . ? C9 C8 H8A 106.9 . . ? C10 C8 H8A 106.9 . . ? P1 C8 H8A 106.9 . . ? C8 C10 H10A 109.5 . . ? C8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? C8 C10 H10D 109.5 . . ? H10A C10 H10D 109.5 . . ? H10C C10 H10D 109.5 . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? 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 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 . . ? C2A C1A C5A 108.2(5) . . ? C2A C1A Ru2 72.5(2) . . ? C5A C1A Ru2 72.8(3) . . ? C2A C1A H1AA 125.7 . . ? C5A C1A H1AA 125.7 . . ? Ru2 C1A H1AA 125.7 . . ? C1A C2A C3A 107.6(5) . . ? C1A C2A Ru2 71.6(2) . . ? C3A C2A Ru2 73.1(2) . . ? C1A C2A H2AA 126.0 . . ? C3A C2A H2AA 126.0 . . ? Ru2 C2A H2AA 126.0 . . ? C4A C3A C2A 109.4(5) . . ? C4A C3A Ru2 73.2(3) . . ? C2A C3A Ru2 70.9(2) . . ? C4A C3A H3AA 125.2 . . ? C2A C3A H3AA 125.2 . . ? Ru2 C3A H3AA 125.2 . . ? C3A C4A C5A 108.1(5) . . ? C3A C4A Ru2 72.2(3) . . ? C5A C4A Ru2 71.0(3) . . ? C3A C4A H4AA 125.9 . . ? C5A C4A H4AA 125.9 . . ? Ru2 C4A H4AA 125.9 . . ? C1A C5A C4A 106.7(5) . . ? C1A C5A Ru2 70.7(3) . . ? C4A C5A Ru2 72.8(3) . . ? C1A C5A H5AA 126.5 . . ? C4A C5A H5AA 126.5 . . ? Ru2 C5A H5AA 126.5 . . ? C19A C14A C15A 118.0(3) . . ? C19A C14A P2 120.2(2) . . ? C15A C14A P2 121.4(2) . . ? C14A C19A C18A 120.7(3) . . ? C14A C19A H19B 119.7 . . ? C18A C19A H19B 119.7 . . ? C17A C18A C19A 120.1(3) . . ? C17A C18A H18B 119.9 . . ? C19A C18A H18B 119.9 . . ? C16A C17A C18A 119.7(3) . . ? C16A C17A H17B 120.1 . . ? C18A C17A H17B 120.1 . . ? C17A C16A C15A 120.8(3) . . ? C17A C16A H16B 119.6 . . ? C15A C16A H16B 119.6 . . ? C16A C15A C14A 120.6(3) . . ? C16A C15A H15B 119.7 . . ? C14A C15A H15B 119.7 . . ? C12A C11A C13A 110.5(3) . . ? C12A C11A P2 110.7(2) . . ? C13A C11A P2 112.9(2) . . ? C12A C11A H11B 107.5 . . ? C13A C11A H11B 107.5 . . ? P2 C11A H11B 107.5 . . ? C11A C13A H13D 109.5 . . ? C11A C13A H13E 109.5 . . ? H13D C13A H13E 109.5 . . ? C11A C13A H13F 109.5 . . ? H13D C13A H13F 109.5 . . ? H13E C13A H13F 109.5 . . ? C11A C12A H12B 109.5 . . ? C11A C12A H12E 109.5 . . ? H12B C12A H12E 109.5 . . ? C11A C12A H12F 109.5 . . ? H12B C12A H12F 109.5 . . ? H12E C12A H12F 109.5 . . ? C10A C8A C9A 110.0(3) . . ? C10A C8A P2 110.5(2) . . ? C9A C8A P2 115.4(2) . . ? C10A C8A H8AA 106.8 . . ? C9A C8A H8AA 106.8 . . ? P2 C8A H8AA 106.8 . . ? C8A C10A H10B 109.5 . . ? C8A C10A H10E 109.5 . . ? H10B C10A H10E 109.5 . . ? C8A C10A H10F 109.5 . . ? H10B C10A H10F 109.5 . . ? H10E C10A H10F 109.5 . . ? C8A C9A H9AA 109.5 . . ? C8A C9A H9AB 109.5 . . ? H9AA C9A H9AB 109.5 . . ? C8A C9A H9AC 109.5 . . ? H9AA C9A H9AC 109.5 . . ? H9AB C9A H9AC 109.5 . . ? Si2 C7A H7AA 109.5 . . ? Si2 C7A H7AB 109.5 . . ? H7AA C7A H7AB 109.5 . . ? Si2 C7A H7AC 109.5 . . ? H7AA C7A H7AC 109.5 . . ? H7AB C7A H7AC 109.5 . . ? Si2 C6A H6AA 109.5 . . ? Si2 C6A H6AB 109.5 . . ? H6AA C6A H6AB 109.5 . . ? Si2 C6A H6AC 109.5 . . ? H6AA C6A H6AC 109.5 . . ? H6AB C6A H6AC 109.5 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 28.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.759 _refine_diff_density_min -1.080 _refine_diff_density_rms 0.099 #==end data_3f _database_code_depnum_ccdc_archive 'CCDC 685292' _audit_creation_method SHELXL-97 _chemical_name_systematic ;(cyclopentadienyl)(triisopropylphosphine)(dimethylchlorosilyl) ruthenium dihydride ; _chemical_name_common ; (cyclopentadienyl)(triisopropylphosphine)(dimethylchlorosilyl) ruthenium dihydride ; _chemical_melting_point ? _chemical_formula_moiety 'C16 H34 Cl P Ru Si' _chemical_formula_sum 'C16 H34 Cl P Ru Si' _chemical_formula_weight 422.01 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 2(1)/n 1' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.4433(2) _cell_length_b 15.4953(4) _cell_length_c 13.8057(4) _cell_angle_alpha 90.00 _cell_angle_beta 94.1670(10) _cell_angle_gamma 90.00 _cell_volume 2014.80(9) _cell_formula_units_Z 4 _cell_measurement_reflns_used 7705 _cell_measurement_theta_min 2.520 _cell_measurement_theta_max 30.011 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.391 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 880 _exptl_absorpt_coefficient_mu 1.041 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8348 _exptl_absorpt_correction_T_max 0.9595 _exptl_absorpt_process_details 'SADABS (Bruker, 2004)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART-1K' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 14596 _diffrn_reflns_av_R_equivalents 0.0343 _diffrn_reflns_av_sigmaI/netI 0.0392 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.53 _diffrn_reflns_theta_max 28.00 _reflns_number_total 4851 _reflns_number_gt 3970 _reflns_threshold_expression I>2\s(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0273P)^2^+1.0962P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4851 _refine_ls_number_parameters 208 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0458 _refine_ls_R_factor_gt 0.0311 _refine_ls_wR_factor_ref 0.0653 _refine_ls_wR_factor_gt 0.0624 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.032 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.52274(2) 0.010498(11) 0.268349(14) 0.01440(6) Uani 1 1 d . A . P1 P 0.40686(7) 0.13021(4) 0.20269(5) 0.01601(13) Uani 1 1 d . . . Si1 Si 0.75859(7) 0.04966(4) 0.30924(5) 0.01930(15) Uani 1 1 d . . . Cl1 Cl 0.9090(2) -0.02346(13) 0.23273(17) 0.0309(4) Uani 0.838(4) 1 d P A 1 C6 C 0.8250(13) 0.0257(8) 0.4388(8) 0.031(2) Uani 0.838(4) 1 d P A 1 H6A H 0.9242 0.0441 0.4494 0.047 Uiso 0.838(4) 1 calc PR A 1 H6B H 0.8183 -0.0364 0.4508 0.047 Uiso 0.838(4) 1 calc PR A 1 H6C H 0.7670 0.0570 0.4832 0.047 Uiso 0.838(4) 1 calc PR A 1 Cl1A Cl 0.8065(17) 0.0124(12) 0.4576(13) 0.034(3) Uani 0.162(4) 1 d P A 2 C6A C 0.878(4) -0.032(3) 0.248(4) 0.034(11) Uani 0.162(4) 1 d P A 2 H6AA H 0.9780 -0.0171 0.2639 0.051 Uiso 0.162(4) 1 calc PR A 2 H6AB H 0.8574 -0.0298 0.1775 0.051 Uiso 0.162(4) 1 calc PR A 2 H6AC H 0.8595 -0.0901 0.2716 0.051 Uiso 0.162(4) 1 calc PR A 2 C1 C 0.3748(3) -0.09700(16) 0.2166(2) 0.0282(6) Uani 1 1 d . . . H1A H 0.3109 -0.0971 0.1556 0.034 Uiso 1 1 calc R A . C2 C 0.5155(3) -0.13030(15) 0.2276(2) 0.0283(6) Uani 1 1 d . A . H2A H 0.5679 -0.1577 0.1752 0.034 Uiso 1 1 calc R . . C3 C 0.5650(3) -0.12351(16) 0.3270(2) 0.0291(6) Uani 1 1 d . . . H3A H 0.6578 -0.1454 0.3567 0.035 Uiso 1 1 calc R A . C4 C 0.4540(3) -0.08642(16) 0.3783(2) 0.0285(6) Uani 1 1 d . A . H4A H 0.4557 -0.0775 0.4501 0.034 Uiso 1 1 calc R . . C5 C 0.3375(3) -0.06967(15) 0.3101(2) 0.0267(6) Uani 1 1 d . A . H5A H 0.2428 -0.0469 0.3258 0.032 Uiso 1 1 calc R . . C7 C 0.8226(3) 0.16316(17) 0.2915(2) 0.0319(7) Uani 1 1 d . A . H7A H 0.9237 0.1670 0.3127 0.048 Uiso 1 1 calc R . . H7B H 0.7687 0.2030 0.3299 0.048 Uiso 1 1 calc R . . H7C H 0.8087 0.1786 0.2226 0.048 Uiso 1 1 calc R . . C8 C 0.5149(3) 0.20783(16) 0.1355(2) 0.0245(6) Uani 1 1 d . . . H8A H 0.5857 0.2322 0.1856 0.029 Uiso 1 1 calc R . . C9 C 0.6041(3) 0.16773(18) 0.0579(2) 0.0345(7) Uani 1 1 d . . . H9A H 0.6566 0.2133 0.0268 0.052 Uiso 1 1 calc R . . H9B H 0.5412 0.1383 0.0089 0.052 Uiso 1 1 calc R . . H9C H 0.6713 0.1260 0.0887 0.052 Uiso 1 1 calc R . . C10 C 0.4339(3) 0.28640(18) 0.0916(2) 0.0374(7) Uani 1 1 d . . . H10A H 0.4991 0.3231 0.0580 0.056 Uiso 1 1 calc R . . H10B H 0.3939 0.3195 0.1436 0.056 Uiso 1 1 calc R . . H10C H 0.3570 0.2667 0.0454 0.056 Uiso 1 1 calc R . . C11 C 0.3297(3) 0.20240(15) 0.29334(18) 0.0209(5) Uani 1 1 d . . . H11A H 0.2670 0.2450 0.2567 0.025 Uiso 1 1 calc R . . C12 C 0.4417(3) 0.25355(16) 0.3563(2) 0.0273(6) Uani 1 1 d . . . H12A H 0.3943 0.2899 0.4022 0.041 Uiso 1 1 calc R . . H12B H 0.4962 0.2900 0.3145 0.041 Uiso 1 1 calc R . . H12C H 0.5060 0.2133 0.3923 0.041 Uiso 1 1 calc R . . C13 C 0.2371(3) 0.15026(17) 0.35823(19) 0.0271(6) Uani 1 1 d . . . H13A H 0.1973 0.1887 0.4056 0.041 Uiso 1 1 calc R . . H13B H 0.2949 0.1057 0.3925 0.041 Uiso 1 1 calc R . . H13C H 0.1598 0.1229 0.3182 0.041 Uiso 1 1 calc R . . C14 C 0.2455(3) 0.09826(17) 0.12382(19) 0.0245(6) Uani 1 1 d . . . H14A H 0.2009 0.0502 0.1591 0.029 Uiso 1 1 calc R . . C15 C 0.2854(3) 0.0589(2) 0.0268(2) 0.0394(7) Uani 1 1 d . . . H15A H 0.1987 0.0431 -0.0126 0.059 Uiso 1 1 calc R . . H15B H 0.3437 0.0073 0.0398 0.059 Uiso 1 1 calc R . . H15C H 0.3391 0.1013 -0.0084 0.059 Uiso 1 1 calc R . . C16 C 0.1273(3) 0.1656(2) 0.1039(2) 0.0349(7) Uani 1 1 d . . . H16A H 0.0502 0.1403 0.0617 0.052 Uiso 1 1 calc R . . H16C H 0.1657 0.2160 0.0718 0.052 Uiso 1 1 calc R . . H16D H 0.0906 0.1834 0.1654 0.052 Uiso 1 1 calc R . . H1 H 0.560(3) 0.077(2) 0.346(2) 0.048(10) Uiso 1 1 d . A . H2 H 0.617(4) 0.029(2) 0.188(3) 0.056(11) Uiso 1 1 d . A . 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 0.01480(9) 0.01069(9) 0.01777(10) 0.00086(8) 0.00170(6) 0.00025(7) P1 0.0185(3) 0.0149(3) 0.0148(3) 0.0003(2) 0.0016(2) 0.0035(2) Si1 0.0144(3) 0.0201(3) 0.0234(4) 0.0001(3) 0.0011(3) 0.0017(2) Cl1 0.0193(9) 0.0341(6) 0.0399(10) -0.0054(6) 0.0056(6) 0.0074(5) C6 0.024(3) 0.037(4) 0.031(5) -0.005(3) -0.006(3) -0.001(2) Cl1A 0.023(4) 0.052(6) 0.028(5) 0.005(4) -0.004(3) 0.004(4) C6A 0.009(17) 0.06(2) 0.034(16) 0.013(12) 0.017(11) 0.011(12) C1 0.0340(15) 0.0149(12) 0.0346(16) -0.0007(11) -0.0043(12) -0.0082(10) C2 0.0391(16) 0.0123(12) 0.0343(16) -0.0011(11) 0.0076(13) -0.0006(10) C3 0.0335(15) 0.0148(12) 0.0386(17) 0.0081(11) -0.0001(13) 0.0001(10) C4 0.0410(17) 0.0179(12) 0.0274(15) 0.0061(11) 0.0075(12) -0.0058(11) C5 0.0226(13) 0.0172(12) 0.0411(17) 0.0032(11) 0.0076(12) -0.0064(10) C7 0.0183(13) 0.0241(13) 0.053(2) -0.0004(13) 0.0009(13) -0.0039(10) C8 0.0327(15) 0.0177(12) 0.0238(14) 0.0060(10) 0.0067(11) 0.0032(10) C9 0.0459(18) 0.0301(15) 0.0298(16) 0.0094(12) 0.0185(14) 0.0073(13) C10 0.0471(19) 0.0252(14) 0.0408(18) 0.0146(13) 0.0106(14) 0.0085(13) C11 0.0228(13) 0.0181(11) 0.0219(13) -0.0040(10) 0.0030(10) 0.0079(9) C12 0.0337(16) 0.0206(13) 0.0276(15) -0.0077(11) 0.0029(12) 0.0011(10) C13 0.0250(14) 0.0326(14) 0.0245(14) -0.0065(11) 0.0075(11) 0.0034(11) C14 0.0241(14) 0.0282(14) 0.0204(13) -0.0023(11) -0.0044(10) 0.0052(10) C15 0.0425(19) 0.0499(19) 0.0244(16) -0.0120(14) -0.0074(13) 0.0079(14) C16 0.0270(15) 0.0437(17) 0.0325(17) -0.0018(13) -0.0078(12) 0.0118(13) _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 C2 2.253(2) . ? Ru1 C3 2.254(2) . ? Ru1 C5 2.254(2) . ? Ru1 C1 2.257(2) . ? Ru1 C4 2.264(3) . ? Ru1 P1 2.3056(6) . ? Ru1 Si1 2.3377(7) . ? Ru1 H1 1.51(3) . ? Ru1 H2 1.50(3) . ? P1 C11 1.865(2) . ? P1 C8 1.867(3) . ? P1 C14 1.874(3) . ? Si1 C7 1.881(3) . ? Si1 C6 1.888(11) . ? Si1 C6A 1.93(4) . ? Si1 H1 2.02(3) . ? Si1 H2 2.09(4) . ? Si1 Cl1A 2.145(16) . ? Si1 Cl1 2.153(2) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C6A H6AA 0.9800 . ? C6A H6AB 0.9800 . ? C6A H6AC 0.9800 . ? C1 C2 1.423(4) . ? C1 C5 1.427(4) . ? C1 H1A 1.0000 . ? C2 C3 1.422(4) . ? C2 H2A 1.0000 . ? C3 C4 1.427(4) . ? C3 H3A 1.0000 . ? C4 C5 1.419(4) . ? C4 H4A 1.0000 . ? C5 H5A 1.0000 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 C10 1.538(4) . ? C8 C9 1.541(4) . ? C8 H8A 1.0000 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C13 1.528(4) . ? C11 C12 1.539(4) . ? C11 H11A 1.0000 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 C16 1.538(4) . ? C14 C15 1.544(4) . ? C14 H14A 1.0000 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16C 0.9800 . ? C16 H16D 0.9800 . ? 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 Ru1 C3 36.78(10) . . ? C2 Ru1 C5 61.34(10) . . ? C3 Ru1 C5 61.36(10) . . ? C2 Ru1 C1 36.80(10) . . ? C3 Ru1 C1 61.51(10) . . ? C5 Ru1 C1 36.87(10) . . ? C2 Ru1 C4 61.33(10) . . ? C3 Ru1 C4 36.83(10) . . ? C5 Ru1 C4 36.62(10) . . ? C1 Ru1 C4 61.41(10) . . ? C2 Ru1 P1 132.53(8) . . ? C3 Ru1 P1 161.63(8) . . ? C5 Ru1 P1 100.89(7) . . ? C1 Ru1 P1 101.78(7) . . ? C4 Ru1 P1 130.28(7) . . ? C2 Ru1 Si1 108.83(8) . . ? C3 Ru1 Si1 90.67(8) . . ? C5 Ru1 Si1 145.56(8) . . ? C1 Ru1 Si1 145.61(7) . . ? C4 Ru1 Si1 108.95(8) . . ? P1 Ru1 Si1 107.62(2) . . ? C2 Ru1 H1 147.1(12) . . ? C3 Ru1 H1 110.3(12) . . ? C5 Ru1 H1 109.8(12) . . ? C1 Ru1 H1 146.6(12) . . ? C4 Ru1 H1 92.3(12) . . ? P1 Ru1 H1 79.0(12) . . ? Si1 Ru1 H1 58.9(12) . . ? C2 Ru1 H2 90.4(13) . . ? C3 Ru1 H2 110.0(13) . . ? C5 Ru1 H2 143.8(13) . . ? C1 Ru1 H2 107.0(13) . . ? C4 Ru1 H2 146.8(13) . . ? P1 Ru1 H2 81.2(13) . . ? Si1 Ru1 H2 61.6(13) . . ? H1 Ru1 H2 106.1(18) . . ? C11 P1 C8 101.61(11) . . ? C11 P1 C14 101.98(11) . . ? C8 P1 C14 109.40(13) . . ? C11 P1 Ru1 114.58(8) . . ? C8 P1 Ru1 116.91(8) . . ? C14 P1 Ru1 111.02(8) . . ? C7 Si1 C6 102.7(4) . . ? C7 Si1 C6A 110.6(12) . . ? C6 Si1 C6A 97.0(17) . . ? C7 Si1 H1 98.6(9) . . ? C6 Si1 H1 93.0(10) . . ? C6A Si1 H1 146.1(16) . . ? C7 Si1 H2 103.5(9) . . ? C6 Si1 H2 151.3(10) . . ? C6A Si1 H2 84.8(19) . . ? H1 Si1 H2 71.5(14) . . ? C7 Si1 Cl1A 109.2(5) . . ? C6 Si1 Cl1A 8.2(7) . . ? C6A Si1 Cl1A 98.8(17) . . ? H1 Si1 Cl1A 87.2(10) . . ? H2 Si1 Cl1A 143.2(10) . . ? C7 Si1 Cl1 101.44(11) . . ? C6 Si1 Cl1 100.1(4) . . ? C6A Si1 Cl1 9.2(12) . . ? H1 Si1 Cl1 152.9(9) . . ? H2 Si1 Cl1 86.2(9) . . ? Cl1A Si1 Cl1 103.1(5) . . ? C7 Si1 Ru1 121.37(9) . . ? C6 Si1 Ru1 115.0(3) . . ? C6A Si1 Ru1 107.5(15) . . ? H1 Si1 Ru1 39.8(9) . . ? H2 Si1 Ru1 39.0(9) . . ? Cl1A Si1 Ru1 107.0(4) . . ? Cl1 Si1 Ru1 113.32(6) . . ? 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 . . ? Si1 C6A H6AA 109.5 . . ? Si1 C6A H6AB 109.5 . . ? H6AA C6A H6AB 109.5 . . ? Si1 C6A H6AC 109.5 . . ? H6AA C6A H6AC 109.5 . . ? H6AB C6A H6AC 109.5 . . ? C2 C1 C5 107.5(3) . . ? C2 C1 Ru1 71.46(15) . . ? C5 C1 Ru1 71.48(14) . . ? C2 C1 H1A 126.1 . . ? C5 C1 H1A 126.1 . . ? Ru1 C1 H1A 126.1 . . ? C3 C2 C1 108.3(2) . . ? C3 C2 Ru1 71.65(15) . . ? C1 C2 Ru1 71.73(14) . . ? C3 C2 H2A 125.8 . . ? C1 C2 H2A 125.8 . . ? Ru1 C2 H2A 125.8 . . ? C2 C3 C4 107.9(3) . . ? C2 C3 Ru1 71.57(14) . . ? C4 C3 Ru1 71.95(14) . . ? C2 C3 H3A 126.0 . . ? C4 C3 H3A 126.0 . . ? Ru1 C3 H3A 126.0 . . ? C5 C4 C3 107.8(3) . . ? C5 C4 Ru1 71.33(14) . . ? C3 C4 Ru1 71.22(15) . . ? C5 C4 H4A 126.0 . . ? C3 C4 H4A 126.0 . . ? Ru1 C4 H4A 126.0 . . ? C4 C5 C1 108.4(2) . . ? C4 C5 Ru1 72.04(15) . . ? C1 C5 Ru1 71.65(14) . . ? C4 C5 H5A 125.7 . . ? C1 C5 H5A 125.7 . . ? Ru1 C5 H5A 125.7 . . ? 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 . . ? C10 C8 C9 109.1(2) . . ? C10 C8 P1 115.52(19) . . ? C9 C8 P1 115.58(18) . . ? C10 C8 H8A 105.2 . . ? C9 C8 H8A 105.2 . . ? P1 C8 H8A 105.2 . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C8 C10 H10A 109.5 . . ? C8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C13 C11 C12 109.9(2) . . ? C13 C11 P1 110.14(16) . . ? C12 C11 P1 113.70(17) . . ? C13 C11 H11A 107.6 . . ? C12 C11 H11A 107.6 . . ? P1 C11 H11A 107.6 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C16 C14 C15 109.4(2) . . ? C16 C14 P1 118.28(19) . . ? C15 C14 P1 111.66(19) . . ? C16 C14 H14A 105.5 . . ? C15 C14 H14A 105.5 . . ? P1 C14 H14A 105.5 . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C14 C16 H16A 109.5 . . ? C14 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? C14 C16 H16D 109.5 . . ? H16A C16 H16D 109.5 . . ? H16C C16 H16D 109.5 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.546 _refine_diff_density_min -0.391 _refine_diff_density_rms 0.081 #==end