Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 _publ_author_name 'Werner, H.' 'Brandt, Carsten D.' 'Ilg, Kerstin' 'Jung, S.' 'Wolf, Justin' _publ_contact_author_name 'Prof H Werner' _publ_contact_author_address ; Institut fur Anorganische Chemie Universitat Wurzburg Am Hubland Wurzburg D-97074 GERMANY ; _publ_contact_author_phone '049 931 888 5261' _publ_contact_author_fax '049 931 888 4605' _publ_contact_author_email helmut.werner@mail.uni-wuerzburg.de _publ_requested_journal 'J. Chem. Soc., Dalton Trans.' _publ_requested_coeditor_name ? _publ_contact_letter ; Please consider this CIF submission for publication in "J. Chem. Soc., Dalton Trans." ; _publ_section_title ; A series of ruthenium(II) complexes containing the bulky, functionalized trialkylphosphines tBu2PCH2XC6H5 as ligands ; _publ_section_abstract ; The monomeric ruthenium(II) complexes [(h6-C6H5XCH2PtBu2-k-P)RuCl2] 3, 4 were prepared either on a reductive route from RuCl3·3H2O and tBu2PCH2XPh (X = CH2 1, OCH2 2) or by ligand replacement reactions from [(p-cym)RuCl2]2 and the phosphine via the p-cymene compounds [(p-cym)(C6H5XCH2PtBu2-k-P)RuCl2] 6, 7 as intermediates. Abstraction of one chloro ligand from 3 with AgPF6 led to the formation of the dinuclear complex [{(h6-C6H5CH2CH2PtBu2-k-P)RuCl}2](PF6)2 8, which reacts with acetone, CH3CN and PMe3 by bridge cleavage to afford the mononuclear compounds [(h6-C6H5CH2CH2PtBu2-k-P)RuCl(L)]PF6 9, 10, 12. Both 10 and 11 (the latter containing 2 as chelating ligand) were also obtained from 3, 4 and AgPF6 in the presence of acetonitrile. Hydridoruthenium(II) complexes [(h6-C6H5XCH2PtBu2-k-P)RuHCl] 13, 14, [RuHCl(H2)(L)2] 15 (L = 1), 16 (L = 2) and [RuHCl(CO)(2)2] 17 could be prepared from RuCl3·3H2O and 1 or 2 in the presence of NEt3 under reductive conditions. Insertion, substitution and addition reactions of compound 17 led to the formation of [Ru(CH=CH2)Cl(CO)(2)2] 18, [RuHF(CO)(2)2] 19, and [RuHCl(CO)2(2)2] 20, respectively. The cationic allenylidene complexes [(h6-C6H5XCH2PtBu2-k-P)RuCl(=C=C=CPh2)]A 22a,b (X = CH2; A = BF4, PF6) and 23 (X = OCH2; A = PF6) were prepared either from 3, 4 or 13, HCºCC(OH)Ph2 and one equiv of AgPF6 or equivalent amounts of HBF4 in diethyl ether. Treatment of 15 and 16 with acetylene afforded the five-coordinate vinylideneruthenium(II) compounds [RuHCl(=C=CH2)(L)2] 24, 25 which in the presence of HBF4 are highly efficient catalysts for the Ring Opening Metathesis Polymerization (ROMP) of cyclooctene. The molecular structures of 10 and 17 were determined crystallographically. ; _publ_section_exptl_prep ; "Crystals were grown from dichloromethane at room temperature." ; _publ_section_exptl_refinement ; The PF6 was found disordered (F3 - F6) and refined anisotropically without restraints. ; _exptl_absorpt_process_details ; no absorption correction; due to the measurement on an area detecting system no standars are reported. ; data_sj4ki _database_code_CSD 175267 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H30 Cl F6 N P2 Ru' _chemical_formula_weight 572.89 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' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 '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 P21/c _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.204(2) _cell_length_b 12.920(3) _cell_length_c 15.626(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.24(3) _cell_angle_gamma 90.00 _cell_volume 2261.9(8) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 5000 _cell_measurement_theta_min 2.41 _cell_measurement_theta_max 25.04 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.682 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1160 _exptl_absorpt_coefficient_mu 1.007 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'IPDS (STOE)' _diffrn_measurement_method phi-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 23880 _diffrn_reflns_av_R_equivalents 0.0401 _diffrn_reflns_av_sigmaI/netI 0.0250 _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 -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.41 _diffrn_reflns_theta_max 25.04 _reflns_number_total 4006 _reflns_number_gt 3518 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'IPDS (Stoe)' _computing_cell_refinement 'IPDS (Stoe)' _computing_data_reduction 'IPDS (Stoe)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ZORTEP (Zsolnai)' _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^)+(0.0507P)^2^+0.0128P] 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 4006 _refine_ls_number_parameters 305 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0430 _refine_ls_R_factor_gt 0.0353 _refine_ls_wR_factor_ref 0.0968 _refine_ls_wR_factor_gt 0.0871 _refine_ls_goodness_of_fit_ref 0.883 _refine_ls_restrained_S_all 0.883 _refine_ls_shift/su_max 0.018 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru Ru 0.66592(3) 0.74110(3) 0.13420(2) 0.0518(6) Uani 1 1 d . . . P1 P 0.77267(11) 0.89483(9) 0.17360(7) 0.0514(6) Uani 1 1 d . . . P2 P 0.18988(12) 0.68993(11) -0.00230(8) 0.0610(6) Uani 1 1 d . . . F1 F 0.1390(5) 0.7136(4) 0.0897(3) 0.1103(15) Uani 1 1 d . A . F2 F 0.2377(5) 0.6640(4) -0.0949(3) 0.1188(17) Uani 1 1 d . A . F3 F 0.2784(14) 0.6035(12) 0.0333(12) 0.074(3) Uani 0.69(6) 1 d P A 1 F4 F 0.0973(15) 0.7720(19) -0.0367(17) 0.103(5) Uani 0.69(6) 1 d P A 1 F5 F 0.2843(19) 0.786(2) 0.0064(12) 0.092(5) Uani 0.69(6) 1 d P A 1 F6 F 0.0998(16) 0.5978(12) -0.0152(12) 0.096(4) Uani 0.69(6) 1 d P A 1 F3^ F 0.289(4) 0.631(5) 0.052(4) 0.109(13) Uani 0.31(6) 1 d P A 2 F4^ F 0.098(4) 0.764(4) -0.053(3) 0.099(11) Uani 0.31(6) 1 d P A 2 F5^ F 0.285(4) 0.767(5) 0.005(3) 0.098(12) Uani 0.31(6) 1 d P A 2 F6^ F 0.087(3) 0.608(3) 0.003(4) 0.111(11) Uani 0.31(6) 1 d P A 2 Cl Cl 0.67318(12) 0.66856(9) 0.27693(8) 0.0635(6) Uani 1 1 d . . . N N 0.5028(4) 0.7983(3) 0.1696(3) 0.0575(10) Uani 1 1 d . . . C1 C 0.7434(5) 0.7763(4) 0.0110(3) 0.0638(13) Uani 1 1 d . . . C2 C 0.8172(5) 0.6993(4) 0.0522(3) 0.0643(13) Uani 1 1 d . . . H2 H 0.9005 0.7110 0.0585 0.077 Uiso 1 1 calc R . . C3 C 0.7670(5) 0.6084(4) 0.0825(4) 0.0662(14) Uani 1 1 d . . . H3 H 0.8153 0.5607 0.1133 0.079 Uiso 1 1 calc R . . C4 C 0.6446(5) 0.5856(4) 0.0683(4) 0.0690(14) Uani 1 1 d . . . H4 H 0.6121 0.5218 0.0876 0.083 Uiso 1 1 calc R . . C5 C 0.5725(5) 0.6568(5) 0.0260(3) 0.0668(14) Uani 1 1 d . . . H5 H 0.4909 0.6412 0.0153 0.080 Uiso 1 1 calc R . . C6 C 0.6209(5) 0.7531(4) -0.0015(3) 0.0633(13) Uani 1 1 d . . . H6 H 0.5704 0.8025 -0.0285 0.076 Uiso 1 1 calc R . . C7 C 0.7936(6) 0.8824(5) -0.0073(3) 0.0723(15) Uani 1 1 d . . . H7A H 0.7286 0.9292 -0.0261 0.087 Uiso 1 1 calc R . . H7B H 0.8527 0.8777 -0.0541 0.087 Uiso 1 1 calc R . . C8 C 0.8539(5) 0.9265(4) 0.0737(3) 0.0661(13) Uani 1 1 d . . . H8A H 0.8597 1.0027 0.0682 0.079 Uiso 1 1 calc R . . H8B H 0.9361 0.8988 0.0779 0.079 Uiso 1 1 calc R . . C10 C 0.4100(5) 0.8305(4) 0.1848(3) 0.0582(12) Uani 1 1 d . . . C11 C 0.2961(5) 0.8774(4) 0.2045(4) 0.0680(14) Uani 1 1 d . . . H11A H 0.2688 0.8530 0.2605 0.102 Uiso 1 1 calc R . . H11B H 0.2376 0.8581 0.1605 0.102 Uiso 1 1 calc R . . H11C H 0.3049 0.9529 0.2057 0.102 Uiso 1 1 calc R . . C20 C 0.8962(4) 0.8841(4) 0.2561(3) 0.0578(12) Uani 1 1 d . . . C21 C 0.6762(5) 1.0098(4) 0.1964(3) 0.0606(12) Uani 1 1 d . . . C22 C 0.9585(5) 0.7790(4) 0.2437(4) 0.0661(14) Uani 1 1 d . . . H22A H 1.0221 0.7712 0.2865 0.099 Uiso 1 1 calc R . . H22B H 0.9929 0.7758 0.1862 0.099 Uiso 1 1 calc R . . H22C H 0.9002 0.7231 0.2505 0.099 Uiso 1 1 calc R . . C23 C 0.8464(5) 0.8894(4) 0.3472(3) 0.0622(12) Uani 1 1 d . . . H23A H 0.7782 0.8423 0.3522 0.093 Uiso 1 1 calc R . . H23B H 0.8206 0.9603 0.3595 0.093 Uiso 1 1 calc R . . H23C H 0.9086 0.8689 0.3881 0.093 Uiso 1 1 calc R . . C24 C 0.9918(5) 0.9699(5) 0.2462(4) 0.0724(15) Uani 1 1 d . . . H24A H 0.9555 1.0376 0.2571 0.109 Uiso 1 1 calc R . . H24B H 1.0238 0.9683 0.1880 0.109 Uiso 1 1 calc R . . H24C H 1.0566 0.9580 0.2874 0.109 Uiso 1 1 calc R . . C25 C 0.5977(5) 0.9906(4) 0.2761(3) 0.0648(13) Uani 1 1 d . . . H25A H 0.5234 1.0300 0.2708 0.097 Uiso 1 1 calc R . . H25B H 0.6409 1.0129 0.3276 0.097 Uiso 1 1 calc R . . H25C H 0.5792 0.9166 0.2805 0.097 Uiso 1 1 calc R . . C26 C 0.7466(5) 1.1105(3) 0.2118(3) 0.0749(15) Uani 1 1 d . . . H26A H 0.8014 1.1221 0.1640 0.112 Uiso 1 1 calc R . . H26B H 0.7923 1.1046 0.2652 0.112 Uiso 1 1 calc R . . H26C H 0.6909 1.1687 0.2160 0.112 Uiso 1 1 calc R . . C27 C 0.5972(5) 1.0274(3) 0.1155(3) 0.0695(14) Uani 1 1 d R . . H27A H 0.5416 1.0845 0.1260 0.104 Uiso 1 1 calc R . . H27B H 0.5521 0.9642 0.1029 0.104 Uiso 1 1 calc R . . H27C H 0.6483 1.0445 0.0667 0.104 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 Ru 0.0480(6) 0.0532(6) 0.0541(6) -0.00327(15) -0.00082(15) 0.00208(15) P1 0.0518(8) 0.0501(8) 0.0525(8) -0.0003(5) 0.0003(5) -0.0003(5) P2 0.0589(9) 0.0652(9) 0.0588(9) -0.0002(5) -0.0006(6) 0.0038(6) F1 0.126(4) 0.124(3) 0.081(2) -0.016(2) 0.035(2) -0.009(3) F2 0.177(5) 0.109(3) 0.071(2) -0.002(2) 0.026(3) 0.023(3) F3 0.056(6) 0.073(5) 0.093(6) 0.014(4) 0.000(5) 0.005(4) F4 0.077(7) 0.085(7) 0.145(12) 0.018(8) 0.002(7) 0.020(6) F5 0.092(8) 0.087(11) 0.096(7) 0.005(5) 0.005(6) -0.031(6) F6 0.103(10) 0.073(5) 0.112(7) -0.021(6) -0.026(6) -0.009(5) F3^ 0.076(11) 0.13(3) 0.12(2) 0.07(2) -0.034(13) -0.027(16) F4^ 0.12(2) 0.083(15) 0.090(13) 0.013(9) -0.065(16) 0.009(13) F5^ 0.076(15) 0.061(13) 0.16(3) 0.015(10) -0.033(15) -0.008(10) F6^ 0.043(10) 0.12(2) 0.17(3) 0.066(18) 0.006(13) -0.011(10) Cl 0.0688(9) 0.0590(8) 0.0627(8) 0.0066(5) -0.0029(6) -0.0077(5) N 0.054(2) 0.059(2) 0.059(2) -0.0026(17) -0.0016(18) 0.0001(18) C1 0.067(3) 0.074(3) 0.051(2) -0.010(2) 0.000(2) 0.006(2) C2 0.057(3) 0.076(3) 0.060(3) -0.013(2) 0.000(2) 0.007(2) C3 0.064(3) 0.064(3) 0.071(3) -0.011(2) -0.004(2) 0.013(2) C4 0.073(3) 0.058(3) 0.076(3) -0.018(2) -0.001(3) -0.003(2) C5 0.057(3) 0.078(3) 0.066(3) -0.016(2) -0.002(2) -0.003(2) C6 0.062(3) 0.074(3) 0.054(3) -0.008(2) -0.005(2) 0.009(2) C7 0.085(4) 0.078(3) 0.055(3) 0.000(2) 0.013(2) -0.008(3) C8 0.070(3) 0.069(3) 0.059(3) 0.001(2) 0.004(2) -0.009(2) C10 0.058(3) 0.058(3) 0.059(3) -0.003(2) -0.002(2) 0.002(2) C11 0.055(3) 0.064(3) 0.085(3) -0.010(3) 0.007(2) 0.005(2) C20 0.051(3) 0.058(3) 0.065(3) -0.003(2) -0.002(2) -0.001(2) C21 0.065(3) 0.051(2) 0.066(3) -0.0015(19) -0.004(2) 0.006(2) C22 0.052(3) 0.073(3) 0.074(3) -0.006(2) -0.006(2) 0.008(2) C23 0.061(3) 0.070(3) 0.056(3) -0.002(2) -0.005(2) 0.003(2) C24 0.059(3) 0.080(4) 0.078(3) -0.004(3) -0.005(2) -0.012(3) C25 0.061(3) 0.066(3) 0.068(3) -0.011(2) -0.001(2) 0.007(2) C26 0.089(4) 0.053(3) 0.083(4) -0.003(2) -0.004(3) -0.001(3) C27 0.075(3) 0.064(3) 0.069(3) 0.008(2) -0.008(3) 0.010(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru N 2.050(4) . ? Ru C1 2.163(5) . ? Ru C6 2.183(5) . ? Ru C2 2.196(5) . ? Ru C3 2.209(5) . ? Ru C5 2.265(5) . ? Ru C4 2.270(5) . ? Ru P1 2.3976(13) . ? Ru Cl 2.4201(13) . ? P1 C8 1.856(5) . ? P1 C21 1.872(5) . ? P1 C20 1.893(5) . ? P2 F5^ 1.46(5) . ? P2 F6^ 1.57(3) . ? P2 F6 1.574(14) . ? P2 F4 1.576(18) . ? P2 F1 1.578(4) . ? P2 F2 1.580(4) . ? P2 F3^ 1.59(4) . ? P2 F3 1.591(16) . ? P2 F4^ 1.61(4) . ? P2 F5 1.63(3) . ? N C10 1.146(6) . ? C1 C6 1.417(8) . ? C1 C2 1.443(8) . ? C1 C7 1.509(8) . ? C2 C3 1.386(8) . ? C3 C4 1.420(8) . ? C4 C5 1.390(8) . ? C5 C6 1.425(8) . ? C7 C8 1.542(8) . ? C10 C11 1.446(7) . ? C20 C23 1.531(7) . ? C20 C22 1.540(7) . ? C20 C24 1.550(7) . ? C21 C26 1.539(6) . ? C21 C25 1.548(7) . ? C21 C27 1.556(6) . ? 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 N Ru C1 121.73(19) . . ? N Ru C6 91.95(18) . . ? C1 Ru C6 38.1(2) . . ? N Ru C2 159.60(18) . . ? C1 Ru C2 38.7(2) . . ? C6 Ru C2 68.1(2) . . ? N Ru C3 146.89(19) . . ? C1 Ru C3 68.3(2) . . ? C6 Ru C3 79.5(2) . . ? C2 Ru C3 36.7(2) . . ? N Ru C5 88.01(18) . . ? C1 Ru C5 67.8(2) . . ? C6 Ru C5 37.3(2) . . ? C2 Ru C5 78.5(2) . . ? C3 Ru C5 65.8(2) . . ? N Ru C4 110.46(19) . . ? C1 Ru C4 79.9(2) . . ? C6 Ru C4 66.4(2) . . ? C2 Ru C4 66.3(2) . . ? C3 Ru C4 36.9(2) . . ? C5 Ru C4 35.7(2) . . ? N Ru P1 94.38(12) . . ? C1 Ru P1 81.53(15) . . ? C6 Ru P1 107.66(15) . . ? C2 Ru P1 88.16(15) . . ? C3 Ru P1 118.72(15) . . ? C5 Ru P1 144.98(16) . . ? C4 Ru P1 154.31(15) . . ? N Ru Cl 85.26(12) . . ? C1 Ru Cl 152.80(15) . . ? C6 Ru Cl 158.34(15) . . ? C2 Ru Cl 114.80(15) . . ? C3 Ru Cl 91.20(16) . . ? C5 Ru Cl 121.03(16) . . ? C4 Ru Cl 94.49(16) . . ? P1 Ru Cl 93.98(5) . . ? C8 P1 C21 105.7(2) . . ? C8 P1 C20 103.3(2) . . ? C21 P1 C20 110.5(2) . . ? C8 P1 Ru 102.28(17) . . ? C21 P1 Ru 114.72(17) . . ? C20 P1 Ru 118.47(16) . . ? F5^ P2 F6^ 173(3) . . ? F5^ P2 F6 173(2) . . ? F6^ P2 F6 13(2) . . ? F5^ P2 F4 93(2) . . ? F6^ P2 F4 89.3(17) . . ? F6 P2 F4 92.5(12) . . ? F5^ P2 F1 94(2) . . ? F6^ P2 F1 79(2) . . ? F6 P2 F1 91.7(7) . . ? F4 P2 F1 86.6(10) . . ? F5^ P2 F2 88(2) . . ? F6^ P2 F2 99(2) . . ? F6 P2 F2 86.7(7) . . ? F4 P2 F2 93.2(10) . . ? F1 P2 F2 178.4(3) . . ? F5^ P2 F3^ 77(3) . . ? F6^ P2 F3^ 99(2) . . ? F6 P2 F3^ 99(2) . . ? F4 P2 F3^ 164(2) . . ? F1 P2 F3^ 82(2) . . ? F2 P2 F3^ 98(2) . . ? F5^ P2 F3 90(2) . . ? F6^ P2 F3 88.1(16) . . ? F6 P2 F3 85.0(10) . . ? F4 P2 F3 177.4(10) . . ? F1 P2 F3 92.6(6) . . ? F2 P2 F3 87.6(6) . . ? F3^ P2 F3 17(3) . . ? F5^ P2 F4^ 96(2) . . ? F6^ P2 F4^ 87(2) . . ? F6 P2 F4^ 88.6(19) . . ? F4 P2 F4^ 10(2) . . ? F1 P2 F4^ 95.8(17) . . ? F2 P2 F4^ 83.9(17) . . ? F3^ P2 F4^ 173(3) . . ? F3 P2 F4^ 169.6(17) . . ? F5^ P2 F5 6(3) . . ? F6^ P2 F5 170(2) . . ? F6 P2 F5 177.4(9) . . ? F4 P2 F5 86.8(13) . . ? F1 P2 F5 90.8(7) . . ? F2 P2 F5 90.8(7) . . ? F3^ P2 F5 83(3) . . ? F3 P2 F5 95.7(12) . . ? F4^ P2 F5 90.4(19) . . ? C10 N Ru 176.3(4) . . ? C6 C1 C2 117.9(5) . . ? C6 C1 C7 121.8(5) . . ? C2 C1 C7 119.8(5) . . ? C6 C1 Ru 71.7(3) . . ? C2 C1 Ru 71.9(3) . . ? C7 C1 Ru 120.8(3) . . ? C3 C2 C1 120.3(5) . . ? C3 C2 Ru 72.2(3) . . ? C1 C2 Ru 69.4(3) . . ? C2 C3 C4 121.0(5) . . ? C2 C3 Ru 71.2(3) . . ? C4 C3 Ru 73.9(3) . . ? C5 C4 C3 119.8(5) . . ? C5 C4 Ru 71.9(3) . . ? C3 C4 Ru 69.2(3) . . ? C4 C5 C6 120.0(5) . . ? C4 C5 Ru 72.4(3) . . ? C6 C5 Ru 68.2(3) . . ? C1 C6 C5 120.9(5) . . ? C1 C6 Ru 70.2(3) . . ? C5 C6 Ru 74.5(3) . . ? C1 C7 C8 110.0(4) . . ? C7 C8 P1 113.2(4) . . ? N C10 C11 176.5(5) . . ? C23 C20 C22 108.9(4) . . ? C23 C20 C24 108.4(4) . . ? C22 C20 C24 107.7(4) . . ? C23 C20 P1 111.2(3) . . ? C22 C20 P1 108.0(3) . . ? C24 C20 P1 112.5(4) . . ? C26 C21 C25 107.6(4) . . ? C26 C21 C27 107.0(4) . . ? C25 C21 C27 110.8(4) . . ? C26 C21 P1 113.8(4) . . ? C25 C21 P1 110.9(3) . . ? C27 C21 P1 106.7(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N Ru P1 C8 -126.0(2) . . . . ? C1 Ru P1 C8 -4.5(2) . . . . ? C6 Ru P1 C8 -32.5(2) . . . . ? C2 Ru P1 C8 33.7(2) . . . . ? C3 Ru P1 C8 54.9(3) . . . . ? C5 Ru P1 C8 -33.2(3) . . . . ? C4 Ru P1 C8 39.5(4) . . . . ? Cl Ru P1 C8 148.5(2) . . . . ? N Ru P1 C21 -12.1(2) . . . . ? C1 Ru P1 C21 109.4(2) . . . . ? C6 Ru P1 C21 81.4(2) . . . . ? C2 Ru P1 C21 147.6(2) . . . . ? C3 Ru P1 C21 168.8(2) . . . . ? C5 Ru P1 C21 80.7(3) . . . . ? C4 Ru P1 C21 153.4(4) . . . . ? Cl Ru P1 C21 -97.62(18) . . . . ? N Ru P1 C20 121.4(2) . . . . ? C1 Ru P1 C20 -117.2(2) . . . . ? C6 Ru P1 C20 -145.2(2) . . . . ? C2 Ru P1 C20 -78.9(2) . . . . ? C3 Ru P1 C20 -57.7(3) . . . . ? C5 Ru P1 C20 -145.9(3) . . . . ? C4 Ru P1 C20 -73.2(4) . . . . ? Cl Ru P1 C20 35.82(19) . . . . ? C1 Ru N C10 27(6) . . . . ? C6 Ru N C10 2(6) . . . . ? C2 Ru N C10 13(7) . . . . ? C3 Ru N C10 -72(6) . . . . ? C5 Ru N C10 -35(6) . . . . ? C4 Ru N C10 -63(6) . . . . ? P1 Ru N C10 110(6) . . . . ? Cl Ru N C10 -156(6) . . . . ? N Ru C1 C6 -43.5(4) . . . . ? C2 Ru C1 C6 128.8(5) . . . . ? C3 Ru C1 C6 100.9(3) . . . . ? C5 Ru C1 C6 29.2(3) . . . . ? C4 Ru C1 C6 64.4(3) . . . . ? P1 Ru C1 C6 -133.5(3) . . . . ? Cl Ru C1 C6 144.4(3) . . . . ? N Ru C1 C2 -172.4(3) . . . . ? C6 Ru C1 C2 -128.8(5) . . . . ? C3 Ru C1 C2 -27.9(3) . . . . ? C5 Ru C1 C2 -99.6(3) . . . . ? C4 Ru C1 C2 -64.5(3) . . . . ? P1 Ru C1 C2 97.7(3) . . . . ? Cl Ru C1 C2 15.5(5) . . . . ? N Ru C1 C7 73.2(5) . . . . ? C6 Ru C1 C7 116.7(6) . . . . ? C2 Ru C1 C7 -114.4(6) . . . . ? C3 Ru C1 C7 -142.3(5) . . . . ? C5 Ru C1 C7 146.0(5) . . . . ? C4 Ru C1 C7 -178.9(5) . . . . ? P1 Ru C1 C7 -16.7(4) . . . . ? Cl Ru C1 C7 -98.9(5) . . . . ? C6 C1 C2 C3 -3.6(7) . . . . ? C7 C1 C2 C3 168.9(5) . . . . ? Ru C1 C2 C3 53.3(4) . . . . ? C6 C1 C2 Ru -56.9(4) . . . . ? C7 C1 C2 Ru 115.7(4) . . . . ? N Ru C2 C3 -114.4(5) . . . . ? C1 Ru C2 C3 -133.3(5) . . . . ? C6 Ru C2 C3 -102.1(4) . . . . ? C5 Ru C2 C3 -64.6(3) . . . . ? C4 Ru C2 C3 -29.3(3) . . . . ? P1 Ru C2 C3 148.0(3) . . . . ? Cl Ru C2 C3 54.4(3) . . . . ? N Ru C2 C1 18.9(7) . . . . ? C6 Ru C2 C1 31.2(3) . . . . ? C3 Ru C2 C1 133.3(5) . . . . ? C5 Ru C2 C1 68.7(3) . . . . ? C4 Ru C2 C1 104.0(4) . . . . ? P1 Ru C2 C1 -78.7(3) . . . . ? Cl Ru C2 C1 -172.2(3) . . . . ? C1 C2 C3 C4 4.7(8) . . . . ? Ru C2 C3 C4 56.8(4) . . . . ? C1 C2 C3 Ru -52.0(4) . . . . ? N Ru C3 C2 144.5(3) . . . . ? C1 Ru C3 C2 29.3(3) . . . . ? C6 Ru C3 C2 67.3(3) . . . . ? C5 Ru C3 C2 103.8(4) . . . . ? C4 Ru C3 C2 131.7(5) . . . . ? P1 Ru C3 C2 -37.2(4) . . . . ? Cl Ru C3 C2 -132.4(3) . . . . ? N Ru C3 C4 12.7(5) . . . . ? C1 Ru C3 C4 -102.4(4) . . . . ? C6 Ru C3 C4 -64.5(4) . . . . ? C2 Ru C3 C4 -131.7(5) . . . . ? C5 Ru C3 C4 -27.9(3) . . . . ? P1 Ru C3 C4 -168.9(3) . . . . ? Cl Ru C3 C4 95.9(3) . . . . ? C2 C3 C4 C5 -2.3(8) . . . . ? Ru C3 C4 C5 53.2(5) . . . . ? C2 C3 C4 Ru -55.5(4) . . . . ? N Ru C4 C5 54.4(4) . . . . ? C1 Ru C4 C5 -65.9(4) . . . . ? C6 Ru C4 C5 -28.5(3) . . . . ? C2 Ru C4 C5 -103.9(4) . . . . ? C3 Ru C4 C5 -133.0(5) . . . . ? P1 Ru C4 C5 -110.1(4) . . . . ? Cl Ru C4 C5 141.0(3) . . . . ? N Ru C4 C3 -172.6(3) . . . . ? C1 Ru C4 C3 67.1(4) . . . . ? C6 Ru C4 C3 104.5(4) . . . . ? C2 Ru C4 C3 29.1(3) . . . . ? C5 Ru C4 C3 133.0(5) . . . . ? P1 Ru C4 C3 22.9(6) . . . . ? Cl Ru C4 C3 -86.0(3) . . . . ? C3 C4 C5 C6 -1.2(8) . . . . ? Ru C4 C5 C6 50.7(4) . . . . ? C3 C4 C5 Ru -51.9(4) . . . . ? N Ru C5 C4 -130.4(4) . . . . ? C1 Ru C5 C4 104.0(4) . . . . ? C6 Ru C5 C4 133.8(5) . . . . ? C2 Ru C5 C4 65.1(4) . . . . ? C3 Ru C5 C4 28.8(3) . . . . ? P1 Ru C5 C4 134.8(3) . . . . ? Cl Ru C5 C4 -47.1(4) . . . . ? N Ru C5 C6 95.8(3) . . . . ? C1 Ru C5 C6 -29.8(3) . . . . ? C2 Ru C5 C6 -68.7(3) . . . . ? C3 Ru C5 C6 -105.0(4) . . . . ? C4 Ru C5 C6 -133.8(5) . . . . ? P1 Ru C5 C6 1.0(4) . . . . ? Cl Ru C5 C6 179.1(3) . . . . ? C2 C1 C6 C5 0.1(7) . . . . ? C7 C1 C6 C5 -172.3(5) . . . . ? Ru C1 C6 C5 -56.9(4) . . . . ? C2 C1 C6 Ru 57.0(4) . . . . ? C7 C1 C6 Ru -115.4(5) . . . . ? C4 C5 C6 C1 2.3(8) . . . . ? Ru C5 C6 C1 54.9(4) . . . . ? C4 C5 C6 Ru -52.6(5) . . . . ? N Ru C6 C1 144.1(3) . . . . ? C2 Ru C6 C1 -31.6(3) . . . . ? C3 Ru C6 C1 -68.1(3) . . . . ? C5 Ru C6 C1 -131.7(5) . . . . ? C4 Ru C6 C1 -104.4(4) . . . . ? P1 Ru C6 C1 48.9(3) . . . . ? Cl Ru C6 C1 -133.8(4) . . . . ? N Ru C6 C5 -84.1(3) . . . . ? C1 Ru C6 C5 131.7(5) . . . . ? C2 Ru C6 C5 100.1(3) . . . . ? C3 Ru C6 C5 63.6(3) . . . . ? C4 Ru C6 C5 27.4(3) . . . . ? P1 Ru C6 C5 -179.4(3) . . . . ? Cl Ru C6 C5 -2.1(6) . . . . ? C6 C1 C7 C8 122.7(6) . . . . ? C2 C1 C7 C8 -49.5(7) . . . . ? Ru C1 C7 C8 36.2(6) . . . . ? C1 C7 C8 P1 -38.1(6) . . . . ? C21 P1 C8 C7 -95.9(4) . . . . ? C20 P1 C8 C7 148.0(4) . . . . ? Ru P1 C8 C7 24.5(4) . . . . ? Ru N C10 C11 -98(10) . . . . ? C8 P1 C20 C23 163.5(4) . . . . ? C21 P1 C20 C23 50.9(4) . . . . ? Ru P1 C20 C23 -84.4(4) . . . . ? C8 P1 C20 C22 -77.1(4) . . . . ? C21 P1 C20 C22 170.3(3) . . . . ? Ru P1 C20 C22 35.0(4) . . . . ? C8 P1 C20 C24 41.7(4) . . . . ? C21 P1 C20 C24 -71.0(4) . . . . ? Ru P1 C20 C24 153.8(3) . . . . ? C8 P1 C21 C26 -61.7(4) . . . . ? C20 P1 C21 C26 49.3(4) . . . . ? Ru P1 C21 C26 -173.6(3) . . . . ? C8 P1 C21 C25 176.8(4) . . . . ? C20 P1 C21 C25 -72.1(4) . . . . ? Ru P1 C21 C25 64.9(4) . . . . ? C8 P1 C21 C27 56.1(4) . . . . ? C20 P1 C21 C27 167.2(3) . . . . ? Ru P1 C21 C27 -55.8(4) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.04 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.030 _refine_diff_density_min -0.029 _refine_diff_density_rms 0.003 #===END data_sj1cb _database_code_CSD 175268 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C33 H55 Cl O3 P2 Ru' _chemical_formula_weight 698.23 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' '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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 11.676(2) _cell_length_b 12.255(3) _cell_length_c 13.537(3) _cell_angle_alpha 79.57(3) _cell_angle_beta 68.26(3) _cell_angle_gamma 82.44(3) _cell_volume 1765.1(6) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 5000 _cell_measurement_theta_min 2.23 _cell_measurement_theta_max 25.0 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.314 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 736 _exptl_absorpt_coefficient_mu 0.640 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; The hydride could not be located, but was verified by NMR-spectroscopy. ; _diffrn_ambient_temperature 173(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 'IPDS (STOE)' _diffrn_measurement_method 'IPDS (STOE)' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 16057 _diffrn_reflns_av_R_equivalents 0.0533 _diffrn_reflns_av_sigmaI/netI 0.0581 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.18 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5845 _reflns_number_gt 4320 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'IPDS (STOE)' _computing_cell_refinement 'IPDS (STOE)' _computing_data_reduction 'IPDS (STOE)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _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^)+(0.1062P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0000(8) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 5845 _refine_ls_number_parameters 374 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0699 _refine_ls_R_factor_gt 0.0509 _refine_ls_wR_factor_ref 0.1464 _refine_ls_wR_factor_gt 0.1398 _refine_ls_goodness_of_fit_ref 0.947 _refine_ls_restrained_S_all 0.947 _refine_ls_shift/su_max 2.207 _refine_ls_shift/su_mean 0.006 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru Ru 0.63777(3) 0.78384(3) 0.25788(3) 0.02171(16) Uani 1 1 d . . . P1 P 0.41639(10) 0.79784(10) 0.32204(10) 0.0228(3) Uani 1 1 d . . . P2 P 0.85964(10) 0.76552(9) 0.18469(10) 0.0218(3) Uani 1 1 d . . . Cl Cl 0.63705(15) 0.7416(2) 0.43970(14) 0.0720(6) Uani 1 1 d . . . O1 O 0.3640(4) 0.7814(3) 0.0451(3) 0.0371(9) Uani 1 1 d . . . O2 O 0.9109(4) 0.7693(4) -0.1311(3) 0.0450(10) Uani 1 1 d . . . O3 O 0.6357(5) 0.9271(5) 0.0570(6) 0.0866(19) Uani 1 1 d . . . C1 C 0.6368(5) 0.8705(5) 0.1334(6) 0.0383(13) Uani 1 1 d . . . C2 C 0.3569(4) 0.8169(4) 0.2109(4) 0.0280(11) Uani 1 1 d . . . H2A H 0.2655 0.8222 0.2427 0.034 Uiso 1 1 calc R . . H2B H 0.3820 0.8894 0.1667 0.034 Uiso 1 1 calc R . . C3 C 0.3958(5) 0.7292(4) 0.1359(4) 0.0304(11) Uani 1 1 d . . . H3A H 0.4857 0.7088 0.1144 0.036 Uiso 1 1 calc R . . H3B H 0.3507 0.6614 0.1708 0.036 Uiso 1 1 calc R . . C4 C 0.9205(5) 0.7877(4) 0.0357(4) 0.0308(11) Uani 1 1 d . . . H4A H 0.9079 0.8680 0.0111 0.037 Uiso 1 1 calc R . . H4B H 1.0108 0.7686 0.0111 0.037 Uiso 1 1 calc R . . C5 C 0.8663(5) 0.7240(4) -0.0196(4) 0.0354(12) Uani 1 1 d . . . H5A H 0.8928 0.6439 -0.0099 0.042 Uiso 1 1 calc R . . H5B H 0.7749 0.7326 0.0104 0.042 Uiso 1 1 calc R . . C10 C 0.3694(5) 0.7188(4) -0.0310(4) 0.0282(11) Uani 1 1 d . . . C11 C 0.3531(6) 0.7803(5) -0.1219(5) 0.0460(15) Uani 1 1 d . . . H11 H 0.3424 0.8591 -0.1278 0.055 Uiso 1 1 calc R . . C12 C 0.3521(7) 0.7284(5) -0.2043(6) 0.0584(18) Uani 1 1 d . . . H12 H 0.3419 0.7712 -0.2668 0.070 Uiso 1 1 calc R . . C13 C 0.3659(6) 0.6140(5) -0.1947(5) 0.0457(15) Uani 1 1 d . . . H13 H 0.3653 0.5774 -0.2507 0.055 Uiso 1 1 calc R . . C14 C 0.3805(5) 0.5539(5) -0.1052(5) 0.0398(13) Uani 1 1 d . . . H14 H 0.3892 0.4751 -0.0991 0.048 Uiso 1 1 calc R . . C15 C 0.3830(5) 0.6048(4) -0.0219(4) 0.0336(12) Uani 1 1 d . . . H15 H 0.3940 0.5613 0.0401 0.040 Uiso 1 1 calc R . . C20 C 0.8625(5) 0.7342(5) -0.1972(4) 0.0346(12) Uani 1 1 d . . . C21 C 0.9299(6) 0.7556(6) -0.3063(5) 0.0500(16) Uani 1 1 d . . . H21 H 1.0057 0.7901 -0.3304 0.060 Uiso 1 1 calc R . . C22 C 0.8872(6) 0.7270(7) -0.3803(5) 0.0583(19) Uani 1 1 d . . . H22 H 0.9336 0.7420 -0.4549 0.070 Uiso 1 1 calc R . . C23 C 0.7778(6) 0.6768(5) -0.3455(5) 0.0487(16) Uani 1 1 d . . . H23 H 0.7486 0.6570 -0.3962 0.058 Uiso 1 1 calc R . . C24 C 0.7112(6) 0.6556(5) -0.2385(5) 0.0494(16) Uani 1 1 d . . . H24 H 0.6352 0.6216 -0.2150 0.059 Uiso 1 1 calc R . . C25 C 0.7530(6) 0.6830(5) -0.1637(5) 0.0446(14) Uani 1 1 d . . . H25 H 0.7065 0.6666 -0.0892 0.053 Uiso 1 1 calc R . . C30 C 0.3435(5) 0.9295(4) 0.3840(5) 0.0361(13) Uani 1 1 d . . . C31 C 0.2025(6) 0.9424(6) 0.4204(6) 0.0589(19) Uani 1 1 d . . . H31A H 0.1675 0.8814 0.4775 0.088 Uiso 1 1 calc R . . H31B H 0.1772 0.9403 0.3594 0.088 Uiso 1 1 calc R . . H31C H 0.1725 1.0136 0.4475 0.088 Uiso 1 1 calc R . . C32 C 0.3818(9) 0.9363(7) 0.4766(8) 0.083(3) Uani 1 1 d . . . H32A H 0.3537 1.0093 0.5004 0.124 Uiso 1 1 calc R . . H32B H 0.4721 0.9262 0.4541 0.124 Uiso 1 1 calc R . . H32C H 0.3448 0.8780 0.5360 0.124 Uiso 1 1 calc R . . C33 C 0.3952(9) 1.0273(5) 0.2972(7) 0.090(3) Uani 1 1 d . . . H33A H 0.3733 1.0963 0.3291 0.135 Uiso 1 1 calc R . . H33B H 0.3602 1.0328 0.2408 0.135 Uiso 1 1 calc R . . H33C H 0.4854 1.0155 0.2660 0.135 Uiso 1 1 calc R . . C40 C 0.3405(5) 0.6707(4) 0.4136(4) 0.0310(11) Uani 1 1 d . . . C41 C 0.4259(5) 0.5687(4) 0.3744(5) 0.0408(14) Uani 1 1 d . . . H41A H 0.5061 0.5727 0.3807 0.061 Uiso 1 1 calc R . . H41B H 0.4375 0.5673 0.2992 0.061 Uiso 1 1 calc R . . H41C H 0.3884 0.5008 0.4185 0.061 Uiso 1 1 calc R . . C42 C 0.3269(6) 0.6702(6) 0.5314(5) 0.0482(15) Uani 1 1 d . . . H42A H 0.2597 0.7243 0.5636 0.072 Uiso 1 1 calc R . . H42B H 0.4043 0.6901 0.5338 0.072 Uiso 1 1 calc R . . H42C H 0.3081 0.5958 0.5716 0.072 Uiso 1 1 calc R . . C43 C 0.2118(5) 0.6585(5) 0.4126(5) 0.0465(15) Uani 1 1 d . . . H43A H 0.1772 0.5923 0.4621 0.070 Uiso 1 1 calc R . . H43B H 0.2185 0.6511 0.3398 0.070 Uiso 1 1 calc R . . H43C H 0.1575 0.7245 0.4353 0.070 Uiso 1 1 calc R . . C50 C 0.9283(4) 0.8837(4) 0.2125(4) 0.0276(10) Uani 1 1 d . . . C51 C 1.0599(5) 0.9047(5) 0.1355(5) 0.0442(14) Uani 1 1 d . . . H51A H 1.0895 0.9659 0.1551 0.066 Uiso 1 1 calc R . . H51B H 1.0605 0.9243 0.0619 0.066 Uiso 1 1 calc R . . H51C H 1.1141 0.8372 0.1402 0.066 Uiso 1 1 calc R . . C52 C 0.9263(6) 0.8678(5) 0.3271(5) 0.0474(15) Uani 1 1 d . . . H52A H 0.9850 0.8057 0.3369 0.071 Uiso 1 1 calc R . . H52B H 0.8430 0.8515 0.3773 0.071 Uiso 1 1 calc R . . H52C H 0.9496 0.9359 0.3410 0.071 Uiso 1 1 calc R . . C53 C 0.8452(5) 0.9891(4) 0.1969(5) 0.0408(13) Uani 1 1 d . . . H53A H 0.7607 0.9796 0.2479 0.061 Uiso 1 1 calc R . . H53B H 0.8451 1.0012 0.1233 0.061 Uiso 1 1 calc R . . H53C H 0.8769 1.0534 0.2095 0.061 Uiso 1 1 calc R . . C60 C 0.9379(5) 0.6255(4) 0.2202(4) 0.0308(11) Uani 1 1 d . . . C61 C 0.9237(10) 0.6007(6) 0.3372(6) 0.080(3) Uani 1 1 d . . . H61A H 0.9567 0.5245 0.3529 0.120 Uiso 1 1 calc R . . H61B H 0.8360 0.6088 0.3818 0.120 Uiso 1 1 calc R . . H61C H 0.9692 0.6529 0.3531 0.120 Uiso 1 1 calc R . . C62 C 0.8727(9) 0.5373(5) 0.2000(8) 0.080(3) Uani 1 1 d . . . H62A H 0.9058 0.4633 0.2228 0.121 Uiso 1 1 calc R . . H62B H 0.8863 0.5456 0.1232 0.121 Uiso 1 1 calc R . . H62C H 0.7839 0.5459 0.2410 0.121 Uiso 1 1 calc R . . C63 C 1.0740(7) 0.6146(7) 0.1543(10) 0.114(5) Uani 1 1 d . . . H63A H 1.1178 0.6644 0.1748 0.171 Uiso 1 1 calc R . . H63B H 1.0861 0.6347 0.0779 0.171 Uiso 1 1 calc R . . H63C H 1.1064 0.5376 0.1676 0.171 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 Ru 0.0193(2) 0.0280(2) 0.0197(2) -0.00311(14) -0.00917(15) -0.00146(13) P1 0.0190(6) 0.0290(6) 0.0227(7) -0.0080(5) -0.0090(5) 0.0006(5) P2 0.0175(6) 0.0285(6) 0.0198(6) -0.0017(5) -0.0073(5) -0.0036(5) Cl 0.0327(8) 0.1454(19) 0.0351(9) -0.0004(10) -0.0148(7) -0.0064(9) O1 0.056(2) 0.0334(18) 0.031(2) -0.0078(16) -0.0267(19) 0.0055(16) O2 0.046(2) 0.073(3) 0.021(2) -0.0039(18) -0.0116(18) -0.025(2) O3 0.046(3) 0.081(4) 0.121(6) -0.023(4) -0.011(3) -0.009(3) C1 0.019(3) 0.043(3) 0.055(4) -0.017(3) -0.011(3) -0.004(2) C2 0.025(2) 0.036(3) 0.026(3) -0.008(2) -0.013(2) 0.003(2) C3 0.033(3) 0.037(3) 0.025(3) -0.002(2) -0.016(2) 0.002(2) C4 0.025(3) 0.041(3) 0.025(3) -0.003(2) -0.007(2) -0.005(2) C5 0.045(3) 0.039(3) 0.019(3) -0.004(2) -0.007(2) -0.004(2) C10 0.030(3) 0.038(3) 0.020(3) -0.009(2) -0.012(2) 0.001(2) C11 0.070(4) 0.036(3) 0.041(3) -0.005(3) -0.032(3) 0.005(3) C12 0.072(5) 0.042(3) 0.067(5) 0.000(3) -0.038(4) 0.005(3) C13 0.046(3) 0.047(3) 0.051(4) -0.022(3) -0.020(3) 0.004(3) C14 0.046(3) 0.035(3) 0.039(3) -0.011(2) -0.015(3) 0.002(2) C15 0.039(3) 0.035(3) 0.026(3) -0.004(2) -0.014(2) 0.005(2) C20 0.034(3) 0.047(3) 0.020(3) -0.007(2) -0.008(2) 0.001(2) C21 0.042(3) 0.085(5) 0.023(3) -0.007(3) -0.010(3) -0.009(3) C22 0.047(4) 0.101(6) 0.022(3) -0.012(3) -0.010(3) 0.006(4) C23 0.058(4) 0.064(4) 0.036(3) -0.020(3) -0.030(3) 0.011(3) C24 0.051(4) 0.060(4) 0.043(4) -0.001(3) -0.024(3) -0.015(3) C25 0.050(4) 0.063(4) 0.025(3) -0.006(3) -0.015(3) -0.016(3) C30 0.032(3) 0.037(3) 0.041(3) -0.020(2) -0.010(2) 0.006(2) C31 0.040(4) 0.070(4) 0.074(5) -0.042(4) -0.022(3) 0.020(3) C32 0.110(7) 0.077(5) 0.108(7) -0.068(5) -0.080(6) 0.035(5) C33 0.098(7) 0.035(3) 0.093(6) -0.026(4) 0.024(5) -0.003(4) C40 0.027(3) 0.041(3) 0.026(3) -0.003(2) -0.010(2) -0.008(2) C41 0.044(3) 0.034(3) 0.040(3) 0.005(2) -0.014(3) -0.006(2) C42 0.048(4) 0.069(4) 0.026(3) 0.003(3) -0.011(3) -0.017(3) C43 0.036(3) 0.066(4) 0.041(4) 0.001(3) -0.017(3) -0.020(3) C50 0.028(3) 0.033(2) 0.025(3) -0.002(2) -0.013(2) -0.007(2) C51 0.031(3) 0.052(3) 0.050(4) -0.010(3) -0.011(3) -0.012(2) C52 0.064(4) 0.053(3) 0.037(3) -0.003(3) -0.028(3) -0.021(3) C53 0.044(3) 0.037(3) 0.051(4) -0.009(3) -0.026(3) -0.004(2) C60 0.026(3) 0.032(3) 0.035(3) -0.004(2) -0.011(2) 0.000(2) C61 0.137(8) 0.056(4) 0.058(5) -0.007(4) -0.062(5) 0.032(5) C62 0.126(8) 0.029(3) 0.123(8) -0.002(4) -0.094(7) 0.004(4) C63 0.033(4) 0.058(5) 0.179(11) 0.039(6) 0.013(5) 0.019(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru C1 1.825(7) . ? Ru P1 2.3959(14) . ? Ru P2 2.4021(14) . ? Ru Cl 2.4187(18) . ? P1 C2 1.845(5) . ? P1 C40 1.897(5) . ? P1 C30 1.906(5) . ? P2 C4 1.854(5) . ? P2 C50 1.900(5) . ? P2 C60 1.904(5) . ? O1 C10 1.370(6) . ? O1 C3 1.431(6) . ? O2 C20 1.372(7) . ? O2 C5 1.431(6) . ? O3 C1 1.140(9) . ? C2 C3 1.522(7) . ? C4 C5 1.505(8) . ? C10 C15 1.373(7) . ? C10 C11 1.386(8) . ? C11 C12 1.385(10) . ? C12 C13 1.377(9) . ? C13 C14 1.355(9) . ? C14 C15 1.395(8) . ? C20 C25 1.383(8) . ? C20 C21 1.387(8) . ? C21 C22 1.384(10) . ? C22 C23 1.375(10) . ? C23 C24 1.361(9) . ? C24 C25 1.381(9) . ? C30 C32 1.498(10) . ? C30 C31 1.528(8) . ? C30 C33 1.529(9) . ? C40 C43 1.535(7) . ? C40 C41 1.537(8) . ? C40 C42 1.541(8) . ? C50 C52 1.520(8) . ? C50 C51 1.527(7) . ? C50 C53 1.542(7) . ? C60 C63 1.508(8) . ? C60 C61 1.508(9) . ? C60 C62 1.517(9) . ? 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 Ru P1 88.55(17) . . ? C1 Ru P2 89.62(17) . . ? P1 Ru P2 176.66(5) . . ? C1 Ru Cl 157.26(19) . . ? P1 Ru Cl 91.16(6) . . ? P2 Ru Cl 91.61(6) . . ? C2 P1 C40 104.0(2) . . ? C2 P1 C30 100.0(2) . . ? C40 P1 C30 110.6(2) . . ? C2 P1 Ru 111.80(16) . . ? C40 P1 Ru 115.16(16) . . ? C30 P1 Ru 113.78(18) . . ? C4 P2 C50 100.5(2) . . ? C4 P2 C60 103.4(2) . . ? C50 P2 C60 111.0(2) . . ? C4 P2 Ru 112.28(17) . . ? C50 P2 Ru 111.08(16) . . ? C60 P2 Ru 117.04(16) . . ? C10 O1 C3 119.3(4) . . ? C20 O2 C5 117.8(4) . . ? O3 C1 Ru 178.1(6) . . ? C3 C2 P1 118.3(3) . . ? O1 C3 C2 104.3(4) . . ? C5 C4 P2 117.2(4) . . ? O2 C5 C4 106.6(4) . . ? O1 C10 C15 126.2(4) . . ? O1 C10 C11 114.2(5) . . ? C15 C10 C11 119.5(5) . . ? C12 C11 C10 120.8(5) . . ? C13 C12 C11 119.3(6) . . ? C14 C13 C12 119.7(6) . . ? C13 C14 C15 121.8(5) . . ? C10 C15 C14 118.8(5) . . ? O2 C20 C25 125.5(5) . . ? O2 C20 C21 115.5(5) . . ? C25 C20 C21 118.9(6) . . ? C22 C21 C20 120.3(6) . . ? C23 C22 C21 119.9(6) . . ? C24 C23 C22 120.0(7) . . ? C23 C24 C25 120.7(6) . . ? C24 C25 C20 120.1(6) . . ? C32 C30 C31 109.3(6) . . ? C32 C30 C33 107.4(7) . . ? C31 C30 C33 108.2(6) . . ? C32 C30 P1 110.8(4) . . ? C31 C30 P1 114.4(4) . . ? C33 C30 P1 106.4(4) . . ? C43 C40 C41 109.0(5) . . ? C43 C40 C42 107.4(5) . . ? C41 C40 C42 107.4(5) . . ? C43 C40 P1 113.4(4) . . ? C41 C40 P1 106.9(3) . . ? C42 C40 P1 112.4(4) . . ? C52 C50 C51 108.7(5) . . ? C52 C50 C53 107.9(5) . . ? C51 C50 C53 107.5(4) . . ? C52 C50 P2 112.6(4) . . ? C51 C50 P2 114.0(4) . . ? C53 C50 P2 105.8(3) . . ? C63 C60 C61 107.9(7) . . ? C63 C60 C62 109.5(7) . . ? C61 C60 C62 106.5(6) . . ? C63 C60 P2 113.1(4) . . ? C61 C60 P2 112.9(4) . . ? C62 C60 P2 106.8(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 Ru P1 C2 28.7(3) . . . . ? P2 Ru P1 C2 -27.9(8) . . . . ? Cl Ru P1 C2 -174.01(18) . . . . ? C1 Ru P1 C40 147.1(3) . . . . ? P2 Ru P1 C40 90.5(8) . . . . ? Cl Ru P1 C40 -55.6(2) . . . . ? C1 Ru P1 C30 -83.7(3) . . . . ? P2 Ru P1 C30 -140.3(8) . . . . ? Cl Ru P1 C30 73.6(2) . . . . ? C1 Ru P2 C4 -23.8(3) . . . . ? P1 Ru P2 C4 32.8(8) . . . . ? Cl Ru P2 C4 178.86(19) . . . . ? C1 Ru P2 C50 87.8(2) . . . . ? P1 Ru P2 C50 144.4(8) . . . . ? Cl Ru P2 C50 -69.49(18) . . . . ? C1 Ru P2 C60 -143.2(3) . . . . ? P1 Ru P2 C60 -86.6(8) . . . . ? Cl Ru P2 C60 59.5(2) . . . . ? P1 Ru C1 O3 82(16) . . . . ? P2 Ru C1 O3 -100(16) . . . . ? Cl Ru C1 O3 -7(17) . . . . ? C40 P1 C2 C3 -67.1(4) . . . . ? C30 P1 C2 C3 178.6(4) . . . . ? Ru P1 C2 C3 57.8(4) . . . . ? C10 O1 C3 C2 -170.0(4) . . . . ? P1 C2 C3 O1 -164.8(3) . . . . ? C50 P2 C4 C5 -168.1(4) . . . . ? C60 P2 C4 C5 77.1(4) . . . . ? Ru P2 C4 C5 -50.0(4) . . . . ? C20 O2 C5 C4 -172.3(4) . . . . ? P2 C4 C5 O2 169.9(3) . . . . ? C3 O1 C10 C15 11.6(8) . . . . ? C3 O1 C10 C11 -171.7(5) . . . . ? O1 C10 C11 C12 -177.9(6) . . . . ? C15 C10 C11 C12 -0.9(9) . . . . ? C10 C11 C12 C13 0.9(11) . . . . ? C11 C12 C13 C14 -0.1(10) . . . . ? C12 C13 C14 C15 -0.6(10) . . . . ? O1 C10 C15 C14 176.8(5) . . . . ? C11 C10 C15 C14 0.3(8) . . . . ? C13 C14 C15 C10 0.5(9) . . . . ? C5 O2 C20 C25 18.5(8) . . . . ? C5 O2 C20 C21 -163.2(5) . . . . ? O2 C20 C21 C22 -177.8(6) . . . . ? C25 C20 C21 C22 0.6(9) . . . . ? C20 C21 C22 C23 -0.2(10) . . . . ? C21 C22 C23 C24 0.2(10) . . . . ? C22 C23 C24 C25 -0.6(10) . . . . ? C23 C24 C25 C20 1.1(10) . . . . ? O2 C20 C25 C24 177.2(5) . . . . ? C21 C20 C25 C24 -1.1(9) . . . . ? C2 P1 C30 C32 -178.1(6) . . . . ? C40 P1 C30 C32 72.7(6) . . . . ? Ru P1 C30 C32 -58.8(6) . . . . ? C2 P1 C30 C31 57.8(5) . . . . ? C40 P1 C30 C31 -51.4(5) . . . . ? Ru P1 C30 C31 177.2(4) . . . . ? C2 P1 C30 C33 -61.6(6) . . . . ? C40 P1 C30 C33 -170.8(5) . . . . ? Ru P1 C30 C33 57.7(6) . . . . ? C2 P1 C40 C43 -31.5(5) . . . . ? C30 P1 C40 C43 75.1(5) . . . . ? Ru P1 C40 C43 -154.1(4) . . . . ? C2 P1 C40 C41 88.8(4) . . . . ? C30 P1 C40 C41 -164.6(4) . . . . ? Ru P1 C40 C41 -33.9(4) . . . . ? C2 P1 C40 C42 -153.6(4) . . . . ? C30 P1 C40 C42 -47.0(5) . . . . ? Ru P1 C40 C42 83.8(4) . . . . ? C4 P2 C50 C52 -163.1(4) . . . . ? C60 P2 C50 C52 -54.1(5) . . . . ? Ru P2 C50 C52 78.0(4) . . . . ? C4 P2 C50 C51 -38.7(4) . . . . ? C60 P2 C50 C51 70.2(4) . . . . ? Ru P2 C50 C51 -157.7(3) . . . . ? C4 P2 C50 C53 79.3(4) . . . . ? C60 P2 C50 C53 -171.8(3) . . . . ? Ru P2 C50 C53 -39.7(4) . . . . ? C4 P2 C60 C63 44.9(7) . . . . ? C50 P2 C60 C63 -62.1(7) . . . . ? Ru P2 C60 C63 168.9(6) . . . . ? C4 P2 C60 C61 167.7(5) . . . . ? C50 P2 C60 C61 60.7(6) . . . . ? Ru P2 C60 C61 -68.2(6) . . . . ? C4 P2 C60 C62 -75.6(5) . . . . ? C50 P2 C60 C62 177.4(5) . . . . ? Ru P2 C60 C62 48.5(5) . . . . ? _diffrn_measured_fraction_theta_max 0.941 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.941 _refine_diff_density_max 1.924 _refine_diff_density_min -0.567 _refine_diff_density_rms 0.145