# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Mark Stradiotto' _publ_contact_author_email MARK.STRADIOTTO@DAL.CA _publ_section_title ; Exploring the Reactivity of a Coordinatively Unsaturated Cp*Ru(kappa2-P,O) Complex with Small Molecule Substrates: Application in E-H Bond Activation (E = H, B, and Si). ; loop_ _publ_author_name 'Mark Stradiotto' 'Kevin D. Hesp' 'Robert McDonald' 'Matthew A. Rankin' 'Gabriele Schatte' # Attachment 'Dalton_combinedcif_passed.cif' data_damsmr0705 _database_code_depnum_ccdc_archive 'CCDC 654073' # CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C25 H36 Cl O P Ru, 0.5(C6 H6)' _chemical_formula_sum 'C28 H39 Cl O P Ru' _chemical_formula_weight 559.08 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' 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' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' # Crystal Data _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/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 20.2188(2) _cell_length_b 8.5282(3) _cell_length_c 16.0143(3) _cell_angle_alpha 90.00 _cell_angle_beta 105.8122(10) _cell_angle_gamma 90.00 _cell_volume 2656.86(11) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 11672 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.88 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.398 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1164 _exptl_absorpt_coefficient_mu 0.769 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8614 _exptl_absorpt_correction_T_max 0.9271 _exptl_absorpt_process_details 'HKL Scalepack (Otwinowski & Minor 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Nonius FR590D, fine-focus sealed tube' _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type 'KappaCCD (BruKer AXS-Nonius, FR540C)' _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 'no decay' _diffrn_reflns_number 21126 _diffrn_reflns_av_R_equivalents 0.0417 _diffrn_reflns_av_sigmaI/netI 0.0358 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.56 _diffrn_reflns_theta_max 27.94 _reflns_number_total 6346 _reflns_number_gt 5293 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT, Bruker AXS/Nonius' _computing_cell_refinement 'HKL DENZO and SCALEPACK, Bruker AXS/Nonius' _computing_data_reduction 'HKL DENZO and SCALEPACK, Bruker AXS/Nonius' _computing_structure_solution ; SIR-97 (A. Altomare, G. Cascarano, C. Giacovazzo et al., 1999) ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; Cameron (WinGX v1.70-01), Ortep (SHELXTL-NT v6.14, Bruker AXS) ; _computing_publication_material 'WinGX v1.70.01 (L. J. Farrugia)' # REFINEMENT DATA _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^)+(0.0327P)^2^+2.0873P] 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 0.0026(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 6346 _refine_ls_number_parameters 303 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0439 _refine_ls_R_factor_gt 0.0324 _refine_ls_wR_factor_ref 0.0783 _refine_ls_wR_factor_gt 0.0725 _refine_ls_goodness_of_fit_ref 1.076 _refine_ls_restrained_S_all 1.076 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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 0.320149(9) 0.15489(2) 0.027482(11) 0.01663(7) Uani 1 1 d . . . Cl1 Cl 0.22329(3) 0.31102(7) -0.05744(4) 0.02727(14) Uani 1 1 d . . . P1 P 0.24508(3) -0.04977(7) 0.03624(4) 0.01876(13) Uani 1 1 d . . . O1 O 0.28119(8) 0.23639(19) 0.13696(10) 0.0213(3) Uani 1 1 d . . . C1 C 0.18334(12) 0.0684(3) 0.07896(15) 0.0207(5) Uani 1 1 d . . . H1 H 0.1635(15) 0.127(4) 0.031(2) 0.036(8) Uiso 1 1 d . . . C2 C 0.22596(12) 0.1838(3) 0.14233(14) 0.0203(5) Uani 1 1 d . . . C3 C 0.19287(12) 0.2175(3) 0.21422(15) 0.0255(5) Uani 1 1 d . . . H3A H 0.2260 0.2034 0.2719 0.031 Uiso 1 1 calc R . . H3B H 0.1743 0.3256 0.2098 0.031 Uiso 1 1 calc R . . C3A C 0.13598(12) 0.0981(3) 0.19915(15) 0.0246(5) Uani 1 1 d . . . C4 C 0.09073(13) 0.0705(4) 0.24918(16) 0.0342(6) Uani 1 1 d . . . H4 H 0.0944 0.1279 0.3011 0.041 Uiso 1 1 calc . . . C5 C 0.04013(14) -0.0423(4) 0.22182(19) 0.0422(7) Uani 1 1 d . . . H5 H 0.0090 -0.0626 0.2556 0.051 Uiso 1 1 calc . . . C6 C 0.03428(15) -0.1257(4) 0.1461(2) 0.0449(8) Uani 1 1 d . . . H6 H -0.0008 -0.2026 0.1284 0.054 Uiso 1 1 calc . . . C7 C 0.07899(14) -0.0983(4) 0.09571(18) 0.0343(6) Uani 1 1 d . . . H7 H 0.0744 -0.1547 0.0433 0.041 Uiso 1 1 calc . . . C7A C 0.13057(12) 0.0126(3) 0.12303(15) 0.0248(5) Uani 1 1 d . . . C10 C 0.38789(12) 0.1128(3) -0.05215(15) 0.0245(5) Uani 1 1 d . . . C11 C 0.41277(12) 0.0300(3) 0.02912(17) 0.0256(5) Uani 1 1 d . . . C12 C 0.42694(11) 0.1433(3) 0.09723(15) 0.0233(5) Uani 1 1 d . . . C13 C 0.41340(12) 0.2965(3) 0.05826(15) 0.0233(5) Uani 1 1 d . . . C14 C 0.39107(12) 0.2779(3) -0.03257(15) 0.0246(5) Uani 1 1 d . . . C15 C 0.37489(15) 0.0442(4) -0.14158(18) 0.0427(7) Uani 1 1 d . . . H15A H 0.3366 0.0998 -0.1813 0.051 Uiso 1 1 calc R . . H15B H 0.3633 -0.0671 -0.1400 0.051 Uiso 1 1 calc R . . H15C H 0.4163 0.0552 -0.1617 0.051 Uiso 1 1 calc R . . C16 C 0.42828(14) -0.1411(3) 0.0376(2) 0.0377(7) Uani 1 1 d . . . H16A H 0.4718 -0.1616 0.0238 0.045 Uiso 1 1 calc R . . H16B H 0.3913 -0.1995 -0.0026 0.045 Uiso 1 1 calc R . . H16C H 0.4319 -0.1747 0.0972 0.045 Uiso 1 1 calc R . . C17 C 0.45854(14) 0.1159(4) 0.19255(17) 0.0370(6) Uani 1 1 d . . . H17A H 0.4563 0.0040 0.2054 0.044 Uiso 1 1 calc R . . H17B H 0.4332 0.1759 0.2260 0.044 Uiso 1 1 calc R . . H17C H 0.5066 0.1501 0.2083 0.044 Uiso 1 1 calc R . . C18 C 0.42180(15) 0.4489(3) 0.1066(2) 0.0392(7) Uani 1 1 d . . . H18A H 0.4700 0.4821 0.1205 0.047 Uiso 1 1 calc R . . H18B H 0.4083 0.4353 0.1605 0.047 Uiso 1 1 calc R . . H18C H 0.3927 0.5288 0.0706 0.047 Uiso 1 1 calc R . . C19 C 0.37386(15) 0.4071(4) -0.09806(19) 0.0379(7) Uani 1 1 d . . . H19A H 0.3467 0.4873 -0.0785 0.046 Uiso 1 1 calc R . . H19B H 0.3472 0.3646 -0.1540 0.046 Uiso 1 1 calc R . . H19C H 0.4164 0.4541 -0.1046 0.046 Uiso 1 1 calc R . . C21 C 0.27854(13) -0.2074(3) 0.11698(17) 0.0274(5) Uani 1 1 d . . . H21 H 0.3184 -0.2551 0.1006 0.033 Uiso 1 1 calc R . . C22 C 0.30784(15) -0.1353(3) 0.20685(17) 0.0359(6) Uani 1 1 d . . . H22A H 0.2701 -0.0993 0.2295 0.043 Uiso 1 1 calc R . . H22B H 0.3373 -0.0461 0.2026 0.043 Uiso 1 1 calc R . . H22C H 0.3349 -0.2142 0.2461 0.043 Uiso 1 1 calc R . . C23 C 0.22992(16) -0.3432(3) 0.1215(2) 0.0393(7) Uani 1 1 d . . . H23A H 0.2540 -0.4194 0.1650 0.047 Uiso 1 1 calc R . . H23B H 0.2149 -0.3943 0.0646 0.047 Uiso 1 1 calc R . . H23C H 0.1898 -0.3026 0.1377 0.047 Uiso 1 1 calc R . . C24 C 0.19006(13) -0.1565(3) -0.05773(16) 0.0263(5) Uani 1 1 d . . . H24 H 0.1588 -0.2266 -0.0357 0.032 Uiso 1 1 calc R . . C25 C 0.23509(16) -0.2606(4) -0.0977(2) 0.0430(7) Uani 1 1 d . . . H25A H 0.2058 -0.3236 -0.1445 0.052 Uiso 1 1 calc R . . H25B H 0.2629 -0.3301 -0.0530 0.052 Uiso 1 1 calc R . . H25C H 0.2655 -0.1946 -0.1211 0.052 Uiso 1 1 calc R . . C26 C 0.14544(18) -0.0497(4) -0.1263(2) 0.0537(9) Uani 1 1 d . . . H26A H 0.1747 0.0246 -0.1465 0.064 Uiso 1 1 calc R . . H26B H 0.1136 0.0082 -0.1012 0.064 Uiso 1 1 calc R . . H26C H 0.1193 -0.1129 -0.1753 0.064 Uiso 1 1 calc R . . C31 C 0.04720(16) 0.9658(4) 0.4547(2) 0.0445(8) Uani 1 1 d . . . H31 H 0.0796 0.9426 0.4233 0.053 Uiso 1 1 calc . . . C32 C -0.01528(19) 0.8897(4) 0.4347(2) 0.0496(8) Uani 1 1 d . . . H32 H -0.0259 0.8132 0.3900 0.059 Uiso 1 1 calc . . . C33 C 0.06249(15) 1.0745(4) 0.5197(2) 0.0472(8) Uani 1 1 d . . . H33 H 0.1058 1.1259 0.5338 0.057 Uiso 1 1 calc . . . 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 0.01816(10) 0.01565(10) 0.01703(10) -0.00021(7) 0.00640(7) 0.00055(7) Cl1 0.0265(3) 0.0314(3) 0.0246(3) 0.0081(2) 0.0080(2) 0.0077(2) P1 0.0208(3) 0.0165(3) 0.0205(3) -0.0024(2) 0.0084(2) -0.0008(2) O1 0.0253(8) 0.0211(8) 0.0194(8) -0.0027(6) 0.0091(6) -0.0017(7) C1 0.0222(11) 0.0200(12) 0.0211(11) -0.0018(9) 0.0082(9) 0.0010(9) C2 0.0236(11) 0.0193(12) 0.0193(10) 0.0002(9) 0.0079(9) 0.0035(9) C3 0.0273(12) 0.0308(13) 0.0203(11) -0.0054(10) 0.0100(9) -0.0004(10) C3A 0.0216(11) 0.0308(13) 0.0222(11) 0.0008(10) 0.0073(9) 0.0016(10) C4 0.0286(13) 0.0532(18) 0.0229(12) -0.0028(12) 0.0104(10) -0.0033(12) C5 0.0305(14) 0.066(2) 0.0357(15) 0.0017(14) 0.0182(12) -0.0080(14) C6 0.0319(15) 0.057(2) 0.0513(18) -0.0095(15) 0.0207(14) -0.0169(14) C7 0.0294(13) 0.0412(16) 0.0355(14) -0.0115(12) 0.0145(11) -0.0093(12) C7A 0.0210(11) 0.0302(13) 0.0252(11) 0.0005(10) 0.0096(9) 0.0020(10) C10 0.0204(11) 0.0325(13) 0.0250(12) -0.0058(10) 0.0137(9) -0.0020(10) C11 0.0194(11) 0.0212(12) 0.0393(14) -0.0003(10) 0.0131(10) 0.0034(9) C12 0.0160(10) 0.0282(13) 0.0255(11) 0.0026(10) 0.0053(9) 0.0008(9) C13 0.0195(11) 0.0230(12) 0.0285(12) -0.0007(10) 0.0082(9) -0.0029(9) C14 0.0201(11) 0.0288(13) 0.0286(12) 0.0062(10) 0.0130(10) -0.0009(10) C15 0.0384(15) 0.061(2) 0.0341(15) -0.0176(14) 0.0182(12) -0.0075(14) C16 0.0287(13) 0.0213(13) 0.068(2) 0.0016(13) 0.0214(14) 0.0061(10) C17 0.0281(13) 0.0523(18) 0.0279(13) 0.0089(12) 0.0027(11) 0.0004(12) C18 0.0386(15) 0.0278(15) 0.0508(17) -0.0114(13) 0.0118(13) -0.0076(12) C19 0.0357(14) 0.0420(17) 0.0397(15) 0.0172(13) 0.0163(12) 0.0028(13) C21 0.0287(12) 0.0193(12) 0.0365(13) 0.0048(10) 0.0127(11) 0.0020(10) C22 0.0413(15) 0.0338(15) 0.0290(13) 0.0131(11) 0.0035(11) -0.0004(12) C23 0.0482(17) 0.0251(14) 0.0467(17) 0.0073(12) 0.0163(14) -0.0059(12) C24 0.0273(12) 0.0260(13) 0.0275(12) -0.0085(10) 0.0108(10) -0.0045(10) C25 0.0484(17) 0.0429(18) 0.0421(16) -0.0209(14) 0.0201(14) -0.0058(14) C26 0.056(2) 0.054(2) 0.0369(16) -0.0166(15) -0.0125(14) 0.0048(17) C31 0.0434(16) 0.052(2) 0.0408(16) 0.0204(15) 0.0167(13) 0.0123(15) C32 0.065(2) 0.0360(17) 0.0419(17) 0.0009(14) 0.0047(16) -0.0020(16) C33 0.0356(15) 0.049(2) 0.0511(18) 0.0159(16) 0.0009(14) -0.0143(14) _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. ; # MOLECULAR GEOMETRY 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 C10 2.141(2) . ? Ru1 C12 2.146(2) . ? Ru1 C11 2.148(2) . ? Ru1 C13 2.180(2) . ? Ru1 C14 2.198(2) . ? Ru1 O1 2.2204(15) . ? Ru1 P1 2.3422(6) . ? Ru1 Cl1 2.4508(6) . ? P1 C24 1.849(2) . ? P1 C21 1.860(3) . ? P1 C1 1.873(2) . ? O1 C2 1.228(3) . ? C1 C2 1.505(3) . ? C1 C7A 1.508(3) . ? C1 H1 0.91(3) . ? C2 C3 1.508(3) . ? C3 C3A 1.506(3) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C3A C4 1.391(3) . ? C3A C7A 1.399(3) . ? C4 C5 1.386(4) . ? C4 H4 0.9500 . ? C5 C6 1.383(4) . ? C5 H5 0.9500 . ? C6 C7 1.386(4) . ? C6 H6 0.9500 . ? C7 C7A 1.388(4) . ? C7 H7 0.9500 . ? C10 C14 1.440(4) . ? C10 C11 1.446(3) . ? C10 C15 1.502(3) . ? C11 C12 1.427(3) . ? C11 C16 1.491(3) . ? C12 C13 1.442(3) . ? C12 C17 1.504(3) . ? C13 C14 1.410(3) . ? C13 C18 1.498(4) . ? C14 C19 1.495(4) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C21 C22 1.528(4) . ? C21 C23 1.534(4) . ? C21 H21 1.0000 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 C26 1.520(4) . ? C24 C25 1.531(4) . ? C24 H24 1.0000 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C31 C33 1.364(5) . ? C31 C32 1.378(5) . ? C31 H31 0.9500 . ? C32 C33 1.384(5) 3_576 ? C32 H32 0.9500 . ? C33 C32 1.384(5) 3_576 ? C33 H33 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 C10 Ru1 C12 65.54(9) . . ? C10 Ru1 C11 39.39(9) . . ? C12 Ru1 C11 38.81(9) . . ? C10 Ru1 C13 64.73(9) . . ? C12 Ru1 C13 38.94(9) . . ? C11 Ru1 C13 64.83(9) . . ? C10 Ru1 C14 38.73(9) . . ? C12 Ru1 C14 64.27(9) . . ? C11 Ru1 C14 64.64(9) . . ? C13 Ru1 C14 37.56(9) . . ? C10 Ru1 O1 160.92(8) . . ? C12 Ru1 O1 97.27(8) . . ? C11 Ru1 O1 129.88(8) . . ? C13 Ru1 O1 96.84(7) . . ? C14 Ru1 O1 127.60(8) . . ? C10 Ru1 P1 116.17(7) . . ? C12 Ru1 P1 120.73(7) . . ? C11 Ru1 P1 101.93(7) . . ? C13 Ru1 P1 159.11(7) . . ? C14 Ru1 P1 153.17(7) . . ? O1 Ru1 P1 79.10(4) . . ? C10 Ru1 Cl1 107.74(7) . . ? C12 Ru1 Cl1 148.48(7) . . ? C11 Ru1 Cl1 146.95(7) . . ? C13 Ru1 Cl1 109.60(7) . . ? C14 Ru1 Cl1 90.91(6) . . ? O1 Ru1 Cl1 82.32(4) . . ? P1 Ru1 Cl1 90.30(2) . . ? C24 P1 C21 103.54(12) . . ? C24 P1 C1 104.43(11) . . ? C21 P1 C1 106.70(11) . . ? C24 P1 Ru1 125.04(8) . . ? C21 P1 Ru1 117.47(8) . . ? C1 P1 Ru1 97.36(8) . . ? C2 O1 Ru1 117.77(14) . . ? C2 C1 C7A 103.82(18) . . ? C2 C1 P1 106.39(15) . . ? C7A C1 P1 128.92(18) . . ? C2 C1 H1 104.3(19) . . ? C7A C1 H1 111.2(19) . . ? P1 C1 H1 100.0(18) . . ? O1 C2 C1 123.79(19) . . ? O1 C2 C3 125.8(2) . . ? C1 C2 C3 110.36(19) . . ? C3A C3 C2 103.12(19) . . ? C3A C3 H3A 111.1 . . ? C2 C3 H3A 111.1 . . ? C3A C3 H3B 111.1 . . ? C2 C3 H3B 111.1 . . ? H3A C3 H3B 109.1 . . ? C4 C3A C7A 120.4(2) . . ? C4 C3A C3 128.0(2) . . ? C7A C3A C3 111.5(2) . . ? C5 C4 C3A 118.7(2) . . ? C5 C4 H4 120.6 . . ? C3A C4 H4 120.6 . . ? C6 C5 C4 120.9(2) . . ? C6 C5 H5 119.5 . . ? C4 C5 H5 119.5 . . ? C5 C6 C7 120.7(3) . . ? C5 C6 H6 119.7 . . ? C7 C6 H6 119.7 . . ? C6 C7 C7A 119.0(2) . . ? C6 C7 H7 120.5 . . ? C7A C7 H7 120.5 . . ? C7 C7A C3A 120.2(2) . . ? C7 C7A C1 129.4(2) . . ? C3A C7A C1 110.3(2) . . ? C14 C10 C11 107.3(2) . . ? C14 C10 C15 125.1(2) . . ? C11 C10 C15 126.5(2) . . ? C14 C10 Ru1 72.80(12) . . ? C11 C10 Ru1 70.59(12) . . ? C15 C10 Ru1 131.22(18) . . ? C12 C11 C10 107.8(2) . . ? C12 C11 C16 126.8(2) . . ? C10 C11 C16 125.0(2) . . ? C12 C11 Ru1 70.50(13) . . ? C10 C11 Ru1 70.02(13) . . ? C16 C11 Ru1 130.35(17) . . ? C11 C12 C13 108.0(2) . . ? C11 C12 C17 127.8(2) . . ? C13 C12 C17 123.9(2) . . ? C11 C12 Ru1 70.69(13) . . ? C13 C12 Ru1 71.79(13) . . ? C17 C12 Ru1 128.64(17) . . ? C14 C13 C12 108.3(2) . . ? C14 C13 C18 126.2(2) . . ? C12 C13 C18 125.5(2) . . ? C14 C13 Ru1 71.94(13) . . ? C12 C13 Ru1 69.27(13) . . ? C18 C13 Ru1 124.52(17) . . ? C13 C14 C10 108.5(2) . . ? C13 C14 C19 126.0(3) . . ? C10 C14 C19 125.4(2) . . ? C13 C14 Ru1 70.50(13) . . ? C10 C14 Ru1 68.47(12) . . ? C19 C14 Ru1 127.12(17) . . ? C10 C15 H15A 109.5 . . ? C10 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C10 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C11 C16 H16A 109.5 . . ? C11 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C11 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C12 C17 H17A 109.5 . . ? C12 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C12 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C13 C18 H18A 109.5 . . ? C13 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C13 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C14 C19 H19A 109.5 . . ? C14 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C14 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C22 C21 C23 110.4(2) . . ? C22 C21 P1 109.77(17) . . ? C23 C21 P1 117.52(19) . . ? C22 C21 H21 106.1 . . ? C23 C21 H21 106.1 . . ? P1 C21 H21 106.1 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C26 C24 C25 110.4(2) . . ? C26 C24 P1 113.56(19) . . ? C25 C24 P1 109.34(18) . . ? C26 C24 H24 107.8 . . ? C25 C24 H24 107.8 . . ? P1 C24 H24 107.8 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C33 C31 C32 120.0(3) . . ? C33 C31 H31 120.0 . . ? C32 C31 H31 120.0 . . ? C31 C32 C33 119.6(3) . 3_576 ? C31 C32 H32 120.2 . . ? C33 C32 H32 120.2 3_576 . ? C31 C33 C32 120.4(3) . 3_576 ? C31 C33 H33 119.8 . . ? C32 C33 H33 119.8 3_576 . ? 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 C10 Ru1 P1 C24 -49.22(13) . . . . ? C12 Ru1 P1 C24 -125.07(12) . . . . ? C11 Ru1 P1 C24 -88.30(12) . . . . ? C13 Ru1 P1 C24 -136.6(2) . . . . ? C14 Ru1 P1 C24 -31.83(18) . . . . ? O1 Ru1 P1 C24 142.90(11) . . . . ? Cl1 Ru1 P1 C24 60.78(10) . . . . ? C10 Ru1 P1 C21 84.17(12) . . . . ? C12 Ru1 P1 C21 8.32(12) . . . . ? C11 Ru1 P1 C21 45.09(12) . . . . ? C13 Ru1 P1 C21 -3.2(2) . . . . ? C14 Ru1 P1 C21 101.56(17) . . . . ? O1 Ru1 P1 C21 -83.72(10) . . . . ? Cl1 Ru1 P1 C21 -165.84(9) . . . . ? C10 Ru1 P1 C1 -162.65(11) . . . . ? C12 Ru1 P1 C1 121.50(11) . . . . ? C11 Ru1 P1 C1 158.28(10) . . . . ? C13 Ru1 P1 C1 110.00(19) . . . . ? C14 Ru1 P1 C1 -145.25(16) . . . . ? O1 Ru1 P1 C1 29.47(9) . . . . ? Cl1 Ru1 P1 C1 -52.65(8) . . . . ? C10 Ru1 O1 C2 -166.9(2) . . . . ? C12 Ru1 O1 C2 -142.14(17) . . . . ? C11 Ru1 O1 C2 -118.64(18) . . . . ? C13 Ru1 O1 C2 178.61(17) . . . . ? C14 Ru1 O1 C2 154.86(16) . . . . ? P1 Ru1 O1 C2 -22.13(16) . . . . ? Cl1 Ru1 O1 C2 69.66(16) . . . . ? C24 P1 C1 C2 -167.66(16) . . . . ? C21 P1 C1 C2 83.10(17) . . . . ? Ru1 P1 C1 C2 -38.53(16) . . . . ? C24 P1 C1 C7A 68.5(2) . . . . ? C21 P1 C1 C7A -40.8(2) . . . . ? Ru1 P1 C1 C7A -162.4(2) . . . . ? Ru1 O1 C2 C1 -0.3(3) . . . . ? Ru1 O1 C2 C3 176.44(18) . . . . ? C7A C1 C2 O1 167.6(2) . . . . ? P1 C1 C2 O1 29.3(3) . . . . ? C7A C1 C2 C3 -9.6(3) . . . . ? P1 C1 C2 C3 -147.86(17) . . . . ? O1 C2 C3 C3A -167.9(2) . . . . ? C1 C2 C3 C3A 9.2(3) . . . . ? C2 C3 C3A C4 176.6(3) . . . . ? C2 C3 C3A C7A -5.2(3) . . . . ? C7A C3A C4 C5 -0.4(4) . . . . ? C3 C3A C4 C5 177.7(3) . . . . ? C3A C4 C5 C6 -0.3(5) . . . . ? C4 C5 C6 C7 0.0(5) . . . . ? C5 C6 C7 C7A 1.0(5) . . . . ? C6 C7 C7A C3A -1.7(4) . . . . ? C6 C7 C7A C1 -177.3(3) . . . . ? C4 C3A C7A C7 1.4(4) . . . . ? C3 C3A C7A C7 -177.0(2) . . . . ? C4 C3A C7A C1 177.8(2) . . . . ? C3 C3A C7A C1 -0.6(3) . . . . ? C2 C1 C7A C7 -177.8(3) . . . . ? P1 C1 C7A C7 -53.0(4) . . . . ? C2 C1 C7A C3A 6.2(3) . . . . ? P1 C1 C7A C3A 131.1(2) . . . . ? C12 Ru1 C10 C14 -78.75(15) . . . . ? C11 Ru1 C10 C14 -116.1(2) . . . . ? C13 Ru1 C10 C14 -35.66(14) . . . . ? O1 Ru1 C10 C14 -51.5(3) . . . . ? P1 Ru1 C10 C14 167.54(11) . . . . ? Cl1 Ru1 C10 C14 68.15(14) . . . . ? C12 Ru1 C10 C11 37.34(14) . . . . ? C13 Ru1 C10 C11 80.43(15) . . . . ? C14 Ru1 C10 C11 116.1(2) . . . . ? O1 Ru1 C10 C11 64.5(3) . . . . ? P1 Ru1 C10 C11 -76.37(14) . . . . ? Cl1 Ru1 C10 C11 -175.76(12) . . . . ? C12 Ru1 C10 C15 159.4(3) . . . . ? C11 Ru1 C10 C15 122.0(3) . . . . ? C13 Ru1 C10 C15 -157.5(3) . . . . ? C14 Ru1 C10 C15 -121.9(3) . . . . ? O1 Ru1 C10 C15 -173.4(2) . . . . ? P1 Ru1 C10 C15 45.7(3) . . . . ? Cl1 Ru1 C10 C15 -53.7(3) . . . . ? C14 C10 C11 C12 3.3(2) . . . . ? C15 C10 C11 C12 171.8(2) . . . . ? Ru1 C10 C11 C12 -60.69(15) . . . . ? C14 C10 C11 C16 -170.1(2) . . . . ? C15 C10 C11 C16 -1.6(4) . . . . ? Ru1 C10 C11 C16 125.9(2) . . . . ? C14 C10 C11 Ru1 64.00(15) . . . . ? C15 C10 C11 Ru1 -127.5(2) . . . . ? C10 Ru1 C11 C12 118.2(2) . . . . ? C13 Ru1 C11 C12 38.09(14) . . . . ? C14 Ru1 C11 C12 79.80(15) . . . . ? O1 Ru1 C11 C12 -39.13(17) . . . . ? P1 Ru1 C11 C12 -124.81(13) . . . . ? Cl1 Ru1 C11 C12 125.66(14) . . . . ? C12 Ru1 C11 C10 -118.2(2) . . . . ? C13 Ru1 C11 C10 -80.16(15) . . . . ? C14 Ru1 C11 C10 -38.45(14) . . . . ? O1 Ru1 C11 C10 -157.38(12) . . . . ? P1 Ru1 C11 C10 116.95(13) . . . . ? Cl1 Ru1 C11 C10 7.4(2) . . . . ? C10 Ru1 C11 C16 -119.5(3) . . . . ? C12 Ru1 C11 C16 122.3(3) . . . . ? C13 Ru1 C11 C16 160.4(3) . . . . ? C14 Ru1 C11 C16 -157.9(3) . . . . ? O1 Ru1 C11 C16 83.1(3) . . . . ? P1 Ru1 C11 C16 -2.5(3) . . . . ? Cl1 Ru1 C11 C16 -112.1(3) . . . . ? C10 C11 C12 C13 -2.1(2) . . . . ? C16 C11 C12 C13 171.1(2) . . . . ? Ru1 C11 C12 C13 -62.51(15) . . . . ? C10 C11 C12 C17 -175.2(2) . . . . ? C16 C11 C12 C17 -1.9(4) . . . . ? Ru1 C11 C12 C17 124.4(2) . . . . ? C10 C11 C12 Ru1 60.38(15) . . . . ? C16 C11 C12 Ru1 -126.4(2) . . . . ? C10 Ru1 C12 C11 -37.89(14) . . . . ? C13 Ru1 C12 C11 -117.3(2) . . . . ? C14 Ru1 C12 C11 -80.82(15) . . . . ? O1 Ru1 C12 C11 150.77(14) . . . . ? P1 Ru1 C12 C11 69.17(15) . . . . ? Cl1 Ru1 C12 C11 -122.07(15) . . . . ? C10 Ru1 C12 C13 79.44(15) . . . . ? C11 Ru1 C12 C13 117.3(2) . . . . ? C14 Ru1 C12 C13 36.51(13) . . . . ? O1 Ru1 C12 C13 -91.90(13) . . . . ? P1 Ru1 C12 C13 -173.50(11) . . . . ? Cl1 Ru1 C12 C13 -4.7(2) . . . . ? C10 Ru1 C12 C17 -161.3(3) . . . . ? C11 Ru1 C12 C17 -123.4(3) . . . . ? C13 Ru1 C12 C17 119.3(3) . . . . ? C14 Ru1 C12 C17 155.8(3) . . . . ? O1 Ru1 C12 C17 27.4(2) . . . . ? P1 Ru1 C12 C17 -54.2(3) . . . . ? Cl1 Ru1 C12 C17 114.5(2) . . . . ? C11 C12 C13 C14 0.1(3) . . . . ? C17 C12 C13 C14 173.5(2) . . . . ? Ru1 C12 C13 C14 -61.69(16) . . . . ? C11 C12 C13 C18 -179.9(2) . . . . ? C17 C12 C13 C18 -6.5(4) . . . . ? Ru1 C12 C13 C18 118.3(2) . . . . ? C11 C12 C13 Ru1 61.80(15) . . . . ? C17 C12 C13 Ru1 -124.8(2) . . . . ? C10 Ru1 C13 C14 36.74(14) . . . . ? C12 Ru1 C13 C14 118.4(2) . . . . ? C11 Ru1 C13 C14 80.48(15) . . . . ? O1 Ru1 C13 C14 -148.43(14) . . . . ? P1 Ru1 C13 C14 134.28(17) . . . . ? Cl1 Ru1 C13 C14 -64.18(15) . . . . ? C10 Ru1 C13 C12 -81.71(15) . . . . ? C11 Ru1 C13 C12 -37.96(14) . . . . ? C14 Ru1 C13 C12 -118.4(2) . . . . ? O1 Ru1 C13 C12 93.12(13) . . . . ? P1 Ru1 C13 C12 15.8(3) . . . . ? Cl1 Ru1 C13 C12 177.37(11) . . . . ? C10 Ru1 C13 C18 158.7(3) . . . . ? C12 Ru1 C13 C18 -119.5(3) . . . . ? C11 Ru1 C13 C18 -157.5(2) . . . . ? C14 Ru1 C13 C18 122.0(3) . . . . ? O1 Ru1 C13 C18 -26.4(2) . . . . ? P1 Ru1 C13 C18 -103.7(3) . . . . ? Cl1 Ru1 C13 C18 57.8(2) . . . . ? C12 C13 C14 C10 2.0(3) . . . . ? C18 C13 C14 C10 -178.0(2) . . . . ? Ru1 C13 C14 C10 -58.04(15) . . . . ? C12 C13 C14 C19 -177.7(2) . . . . ? C18 C13 C14 C19 2.3(4) . . . . ? Ru1 C13 C14 C19 122.3(2) . . . . ? C12 C13 C14 Ru1 60.01(15) . . . . ? C18 C13 C14 Ru1 -120.0(2) . . . . ? C11 C10 C14 C13 -3.3(2) . . . . ? C15 C10 C14 C13 -172.0(2) . . . . ? Ru1 C10 C14 C13 59.28(16) . . . . ? C11 C10 C14 C19 176.4(2) . . . . ? C15 C10 C14 C19 7.7(4) . . . . ? Ru1 C10 C14 C19 -121.0(2) . . . . ? C11 C10 C14 Ru1 -62.55(15) . . . . ? C15 C10 C14 Ru1 128.7(2) . . . . ? C10 Ru1 C14 C13 -120.1(2) . . . . ? C12 Ru1 C14 C13 -37.84(14) . . . . ? C11 Ru1 C14 C13 -81.05(15) . . . . ? O1 Ru1 C14 C13 41.00(17) . . . . ? P1 Ru1 C14 C13 -145.55(13) . . . . ? Cl1 Ru1 C14 C13 122.00(14) . . . . ? C12 Ru1 C14 C10 82.31(15) . . . . ? C11 Ru1 C14 C10 39.10(14) . . . . ? C13 Ru1 C14 C10 120.1(2) . . . . ? O1 Ru1 C14 C10 161.15(12) . . . . ? P1 Ru1 C14 C10 -25.4(2) . . . . ? Cl1 Ru1 C14 C10 -117.86(13) . . . . ? C10 Ru1 C14 C19 118.9(3) . . . . ? C12 Ru1 C14 C19 -158.8(3) . . . . ? C11 Ru1 C14 C19 158.0(3) . . . . ? C13 Ru1 C14 C19 -121.0(3) . . . . ? O1 Ru1 C14 C19 -80.0(3) . . . . ? P1 Ru1 C14 C19 93.5(3) . . . . ? Cl1 Ru1 C14 C19 1.0(2) . . . . ? C24 P1 C21 C22 -163.71(18) . . . . ? C1 P1 C21 C22 -53.8(2) . . . . ? Ru1 P1 C21 C22 54.02(19) . . . . ? C24 P1 C21 C23 -36.5(2) . . . . ? C1 P1 C21 C23 73.4(2) . . . . ? Ru1 P1 C21 C23 -178.76(17) . . . . ? C21 P1 C24 C26 168.7(2) . . . . ? C1 P1 C24 C26 57.1(2) . . . . ? Ru1 P1 C24 C26 -52.9(2) . . . . ? C21 P1 C24 C25 -67.5(2) . . . . ? C1 P1 C24 C25 -179.05(19) . . . . ? Ru1 P1 C24 C25 70.9(2) . . . . ? C33 C31 C32 C33 0.7(5) . . . 3_576 ? C32 C31 C33 C32 -0.7(5) . . . 3_576 ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.94 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.809 _refine_diff_density_min -0.718 _refine_diff_density_rms 0.083 #===END data_damsmr0706 _database_code_depnum_ccdc_archive 'CCDC 654074' # CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C50 H70 N2 O2 P2 Ru2' _chemical_formula_sum 'C50 H70 N2 O2 P2 Ru2' _chemical_formula_weight 995.16 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' 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' Ru Ru -1.2594 0.8363 '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' # Crystal Data _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/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 17.4049(11) _cell_length_b 13.5276(8) _cell_length_c 23.1490(19) _cell_angle_alpha 90.00 _cell_angle_beta 118.873(3) _cell_angle_gamma 90.00 _cell_volume 4772.8(6) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9489 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 24.11 _exptl_crystal_description rod _exptl_crystal_colour yellow _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.385 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2072 _exptl_absorpt_coefficient_mu 0.739 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9432 _exptl_absorpt_correction_T_max 0.9640 _exptl_absorpt_process_details 'HKL Scalepack (Otwinowski & Minor 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Nonius FR590D, fine-focus sealed tube' _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type 'KappaCCD (BruKer AXS-Nonius, FR540C)' _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 'no decay' _diffrn_reflns_number 16933 _diffrn_reflns_av_R_equivalents 0.1289 _diffrn_reflns_av_sigmaI/netI 0.1058 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.51 _diffrn_reflns_theta_max 21.97 _reflns_number_total 5742 _reflns_number_gt 3537 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT, Bruker AXS/Nonius' _computing_cell_refinement 'HKL DENZO and SCALEPACK, Bruker AXS/Nonius' _computing_data_reduction 'HKL DENZO and SCALEPACK, Bruker AXS/Nonius' _computing_structure_solution ; SIR-97 (A. Altomare, G. Cascarano, C. Giacovazzo et al., 1999) ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; Cameron (WinGX v1.70-01), Ortep (SHELXTL-NT v6.14, Bruker AXS) ; _computing_publication_material 'WinGX v1.70.01 (L. J. Farrugia)' # REFINEMENT DATA _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^)+(0.0000P)^2^+15.8609P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5742 _refine_ls_number_parameters 541 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1098 _refine_ls_R_factor_gt 0.0557 _refine_ls_wR_factor_ref 0.1136 _refine_ls_wR_factor_gt 0.0936 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.023 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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 0.23926(4) 0.00860(6) 0.13225(3) 0.0219(2) Uani 1 1 d . . . Ru2 Ru 0.14282(4) -0.00675(6) 0.30458(3) 0.0255(2) Uani 1 1 d . . . N1 N 0.2228(4) 0.0185(5) 0.2116(4) 0.0223(17) Uani 1 1 d . . . N2 N 0.2061(4) 0.0048(6) 0.2525(3) 0.0246(16) Uani 1 1 d . . . P1 P 0.32628(15) 0.15256(18) 0.15821(13) 0.0253(6) Uani 1 1 d . . . P2 P 0.25950(15) -0.08383(18) 0.39746(13) 0.0287(6) Uani 1 1 d . . . O1 O 0.1365(3) 0.1151(4) 0.0828(3) 0.0262(15) Uani 1 1 d . . . O2 O 0.1196(4) -0.1577(5) 0.2712(3) 0.0357(17) Uani 1 1 d . . . C1 C 0.0935(6) 0.2923(6) 0.0648(4) 0.029(2) Uani 1 1 d . . . H1A H 0.0631 0.2905 0.0159 0.035 Uiso 1 1 calc R . . H1B H 0.0495 0.2905 0.0802 0.035 Uiso 1 1 calc R . . C2 C 0.1588(5) 0.2083(7) 0.0940(4) 0.025(2) Uani 1 1 d . . . C3A C 0.2404(6) 0.3524(6) 0.1315(5) 0.028(2) Uani 1 1 d . . . C3 C 0.2435(5) 0.2434(6) 0.1314(4) 0.025(2) Uani 1 1 d . . . C4 C 0.3028(6) 0.4237(7) 0.1608(5) 0.036(3) Uani 1 1 d . . . H4 H 0.3624 0.4052 0.1875 0.044 Uiso 1 1 calc . . . C5 C 0.2804(7) 0.5225(7) 0.1522(6) 0.048(3) Uani 1 1 d . . . H5 H 0.3242 0.5714 0.1738 0.058 Uiso 1 1 calc . . . C6 C 0.1945(8) 0.5501(7) 0.1122(6) 0.048(3) Uani 1 1 d . . . H6 H 0.1797 0.6183 0.1056 0.058 Uiso 1 1 calc . . . C7 C 0.1296(6) 0.4800(7) 0.0816(5) 0.037(3) Uani 1 1 d . . . H7 H 0.0704 0.4994 0.0543 0.044 Uiso 1 1 calc . . . C7A C 0.1521(6) 0.3821(6) 0.0910(5) 0.030(2) Uani 1 1 d . . . C10 C 0.1728(5) -0.0932(6) 0.0485(5) 0.027(2) Uani 1 1 d . . . C11 C 0.2579(6) -0.0719(6) 0.0577(5) 0.027(2) Uani 1 1 d . . . C12 C 0.3209(6) -0.1055(7) 0.1224(5) 0.033(2) Uani 1 1 d . . . C13 C 0.2732(6) -0.1463(6) 0.1530(4) 0.029(2) Uani 1 1 d . . . C14 C 0.1794(6) -0.1393(7) 0.1056(5) 0.030(2) Uani 1 1 d . . . C15 C 0.0895(6) -0.0718(7) -0.0118(5) 0.043(3) Uani 1 1 d . . . H15A H 0.0404 -0.0806 -0.0028 0.051 Uiso 1 1 calc R . . H15B H 0.0826 -0.1171 -0.0470 0.051 Uiso 1 1 calc R . . H15C H 0.0902 -0.0035 -0.0257 0.051 Uiso 1 1 calc R . . C16 C 0.2788(7) -0.0417(7) 0.0044(5) 0.043(3) Uani 1 1 d . . . H16A H 0.3348 -0.0061 0.0241 0.052 Uiso 1 1 calc R . . H16B H 0.2321 0.0014 -0.0271 0.052 Uiso 1 1 calc R . . H16C H 0.2830 -0.1007 -0.0184 0.052 Uiso 1 1 calc R . . C17 C 0.4182(6) -0.1126(7) 0.1497(5) 0.040(3) Uani 1 1 d . . . H17A H 0.4331 -0.1776 0.1390 0.049 Uiso 1 1 calc R . . H17B H 0.4474 -0.1043 0.1977 0.049 Uiso 1 1 calc R . . H17C H 0.4379 -0.0607 0.1303 0.049 Uiso 1 1 calc R . . C18 C 0.3117(5) -0.1934(6) 0.2184(4) 0.030(2) Uani 1 1 d . . . H18A H 0.3138 -0.2652 0.2136 0.037 Uiso 1 1 calc R . . H18B H 0.2756 -0.1782 0.2392 0.037 Uiso 1 1 calc R . . H18C H 0.3713 -0.1682 0.2461 0.037 Uiso 1 1 calc R . . C19 C 0.1054(5) -0.1754(6) 0.1158(5) 0.030(2) Uani 1 1 d . . . H19A H 0.0534 -0.1344 0.0903 0.036 Uiso 1 1 calc R . . H19B H 0.1224 -0.1713 0.1627 0.036 Uiso 1 1 calc R . . H19C H 0.0920 -0.2443 0.1011 0.036 Uiso 1 1 calc R . . C21 C 0.4094(5) 0.1810(7) 0.2440(5) 0.036(3) Uani 1 1 d . . . H21 H 0.4427 0.2404 0.2427 0.043 Uiso 1 1 calc R . . C22 C 0.3660(6) 0.2078(7) 0.2869(5) 0.044(3) Uani 1 1 d . . . H22A H 0.3283 0.1533 0.2858 0.053 Uiso 1 1 calc R . . H22B H 0.3306 0.2678 0.2695 0.053 Uiso 1 1 calc R . . H22C H 0.4117 0.2194 0.3325 0.053 Uiso 1 1 calc R . . C23 C 0.4743(6) 0.0976(8) 0.2740(5) 0.050(3) Uani 1 1 d . . . H23A H 0.5200 0.1167 0.3182 0.060 Uiso 1 1 calc R . . H23B H 0.5012 0.0833 0.2462 0.060 Uiso 1 1 calc R . . H23C H 0.4439 0.0385 0.2771 0.060 Uiso 1 1 calc R . . C24 C 0.3846(6) 0.1744(7) 0.1094(5) 0.033(2) Uani 1 1 d . . . H24 H 0.4106 0.1097 0.1067 0.040 Uiso 1 1 calc R . . C25 C 0.3178(6) 0.2029(7) 0.0395(5) 0.045(3) Uani 1 1 d . . . H25A H 0.2972 0.2704 0.0393 0.054 Uiso 1 1 calc R . . H25B H 0.2679 0.1572 0.0230 0.054 Uiso 1 1 calc R . . H25C H 0.3450 0.1996 0.0111 0.054 Uiso 1 1 calc R . . C26 C 0.4596(6) 0.2500(8) 0.1380(6) 0.057(3) Uani 1 1 d . . . H26A H 0.4854 0.2558 0.1087 0.069 Uiso 1 1 calc R . . H26B H 0.5046 0.2281 0.1817 0.069 Uiso 1 1 calc R . . H26C H 0.4366 0.3144 0.1418 0.069 Uiso 1 1 calc R . . C31 C 0.1818(6) -0.3248(7) 0.2805(5) 0.042(3) Uani 1 1 d . . . H31A H 0.1332 -0.3635 0.2800 0.050 Uiso 1 1 calc R . . H31B H 0.1762 -0.3259 0.2358 0.050 Uiso 1 1 calc R . . C32 C 0.1824(6) -0.2195(7) 0.3035(5) 0.030(2) Uani 1 1 d . . . C33A C 0.3130(6) -0.2915(7) 0.3799(5) 0.034(3) Uani 1 1 d . . . C33 C 0.2581(6) -0.2024(6) 0.3619(5) 0.029(2) Uani 1 1 d . . . C34 C 0.3965(6) -0.3095(7) 0.4327(5) 0.035(3) Uani 1 1 d . . . H34 H 0.4264 -0.2604 0.4653 0.042 Uiso 1 1 calc . . . C35 C 0.4350(7) -0.4018(9) 0.4363(6) 0.052(3) Uani 1 1 d . . . H35 H 0.4910 -0.4168 0.4723 0.063 Uiso 1 1 calc . . . C36 C 0.3910(9) -0.4715(8) 0.3869(7) 0.060(4) Uani 1 1 d . . . H36 H 0.4189 -0.5327 0.3888 0.072 Uiso 1 1 calc . . . C37A C 0.2693(6) -0.3637(7) 0.3311(5) 0.040(3) Uani 1 1 d . . . C37 C 0.3087(8) -0.4543(7) 0.3358(6) 0.055(3) Uani 1 1 d . . . H37 H 0.2789 -0.5042 0.3038 0.066 Uiso 1 1 calc . . . C41 C 0.2450(6) -0.1093(8) 0.4694(5) 0.041(3) Uani 1 1 d . . . H41 H 0.2319 -0.0448 0.4839 0.050 Uiso 1 1 calc R . . C42 C 0.1650(6) -0.1762(7) 0.4495(5) 0.047(3) Uani 1 1 d . . . H42A H 0.1808 -0.2447 0.4461 0.056 Uiso 1 1 calc R . . H42B H 0.1172 -0.1548 0.4067 0.056 Uiso 1 1 calc R . . H42C H 0.1459 -0.1721 0.4829 0.056 Uiso 1 1 calc R . . C43 C 0.3248(6) -0.1552(8) 0.5300(5) 0.045(3) Uani 1 1 d . . . H43A H 0.3072 -0.1756 0.5626 0.054 Uiso 1 1 calc R . . H43B H 0.3719 -0.1062 0.5498 0.054 Uiso 1 1 calc R . . H43C H 0.3457 -0.2130 0.5160 0.054 Uiso 1 1 calc R . . C44 C 0.3727(6) -0.0328(7) 0.4347(5) 0.038(3) Uani 1 1 d . . . H44 H 0.4121 -0.0748 0.4733 0.045 Uiso 1 1 calc R . . C45 C 0.3729(7) 0.0729(8) 0.4595(6) 0.055(3) Uani 1 1 d . . . H45A H 0.4320 0.1009 0.4778 0.066 Uiso 1 1 calc R . . H45B H 0.3553 0.0710 0.4938 0.066 Uiso 1 1 calc R . . H45C H 0.3316 0.1139 0.4227 0.066 Uiso 1 1 calc R . . C46 C 0.4065(6) -0.0346(7) 0.3849(5) 0.042(3) Uani 1 1 d . . . H46A H 0.3666 0.0030 0.3456 0.051 Uiso 1 1 calc R . . H46B H 0.4097 -0.1031 0.3725 0.051 Uiso 1 1 calc R . . H46C H 0.4651 -0.0049 0.4048 0.051 Uiso 1 1 calc R . . C50 C 0.0080(6) 0.0408(7) 0.2405(5) 0.035(3) Uani 1 1 d . . . C51 C 0.0202(6) 0.0176(8) 0.3040(5) 0.040(3) Uani 1 1 d . . . C52 C 0.0794(7) 0.0822(9) 0.3491(5) 0.046(3) Uani 1 1 d . . . C53 C 0.1110(7) 0.1457(7) 0.3158(6) 0.050(3) Uani 1 1 d . . . C54 C 0.0630(6) 0.1191(7) 0.2466(5) 0.035(3) Uani 1 1 d . . . C55 C -0.0522(6) -0.0126(9) 0.1769(5) 0.059(3) Uani 1 1 d . . . H55A H -0.1103 0.0184 0.1565 0.071 Uiso 1 1 calc R . . H55B H -0.0574 -0.0821 0.1865 0.071 Uiso 1 1 calc R . . H55C H -0.0279 -0.0087 0.1466 0.071 Uiso 1 1 calc R . . C56 C -0.0371(7) -0.0602(9) 0.3124(7) 0.073(4) Uani 1 1 d . . . H56A H -0.0129 -0.0760 0.3593 0.088 Uiso 1 1 calc R . . H56B H -0.0384 -0.1201 0.2881 0.088 Uiso 1 1 calc R . . H56C H -0.0969 -0.0345 0.2951 0.088 Uiso 1 1 calc R . . C57 C 0.0998(9) 0.0926(10) 0.4196(6) 0.089(5) Uani 1 1 d . . . H57A H 0.0581 0.1386 0.4222 0.106 Uiso 1 1 calc R . . H57B H 0.1595 0.1181 0.4460 0.106 Uiso 1 1 calc R . . H57C H 0.0951 0.0279 0.4366 0.106 Uiso 1 1 calc R . . C58 C 0.1691(8) 0.2341(8) 0.3448(7) 0.084(4) Uani 1 1 d . . . H58A H 0.1329 0.2926 0.3392 0.100 Uiso 1 1 calc R . . H58B H 0.2037 0.2447 0.3222 0.100 Uiso 1 1 calc R . . H58C H 0.2087 0.2229 0.3918 0.100 Uiso 1 1 calc R . . C59 C 0.0697(6) 0.1717(7) 0.1922(5) 0.045(3) Uani 1 1 d . . . H59A H 0.0639 0.1238 0.1586 0.054 Uiso 1 1 calc R . . H59B H 0.1267 0.2048 0.2102 0.054 Uiso 1 1 calc R . . H59C H 0.0227 0.2210 0.1722 0.054 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.0200(4) 0.0238(5) 0.0192(4) -0.0011(4) 0.0074(3) 0.0008(4) Ru2 0.0267(4) 0.0280(5) 0.0208(4) 0.0016(4) 0.0107(3) 0.0048(4) N1 0.019(4) 0.019(4) 0.023(5) -0.007(4) 0.005(3) 0.000(3) N2 0.025(4) 0.017(4) 0.027(5) -0.007(4) 0.008(4) -0.007(4) P1 0.0210(13) 0.0244(14) 0.0263(16) 0.0012(12) 0.0080(12) -0.0012(11) P2 0.0283(14) 0.0311(15) 0.0219(15) 0.0024(12) 0.0083(12) 0.0024(12) O1 0.022(3) 0.028(4) 0.025(4) 0.000(3) 0.008(3) -0.003(3) O2 0.030(4) 0.033(4) 0.040(5) 0.002(4) 0.014(4) -0.002(3) C1 0.036(5) 0.029(6) 0.019(6) 0.010(5) 0.010(5) 0.009(5) C2 0.029(5) 0.031(6) 0.018(6) 0.005(5) 0.014(5) 0.001(5) C3A 0.024(5) 0.030(6) 0.036(6) 0.005(5) 0.019(5) 0.007(5) C3 0.027(5) 0.019(5) 0.031(6) 0.001(5) 0.016(5) 0.000(4) C4 0.030(6) 0.035(6) 0.037(7) -0.002(5) 0.011(5) -0.001(5) C5 0.048(7) 0.024(7) 0.068(8) -0.005(6) 0.025(6) -0.010(5) C6 0.068(8) 0.025(6) 0.060(8) 0.001(6) 0.038(7) 0.008(6) C7 0.043(6) 0.031(7) 0.046(7) 0.003(6) 0.030(5) 0.014(5) C7A 0.045(6) 0.020(6) 0.040(7) -0.001(5) 0.032(6) -0.003(5) C10 0.029(6) 0.020(5) 0.026(6) -0.013(5) 0.009(5) -0.001(4) C11 0.036(6) 0.022(5) 0.028(6) -0.004(5) 0.018(5) 0.000(4) C12 0.023(5) 0.045(7) 0.034(7) -0.007(5) 0.017(5) -0.005(5) C13 0.034(6) 0.023(6) 0.023(6) -0.002(5) 0.009(5) 0.009(5) C14 0.035(6) 0.026(6) 0.023(6) -0.008(5) 0.010(5) -0.001(5) C15 0.041(6) 0.034(6) 0.043(7) -0.020(6) 0.012(6) 0.000(5) C16 0.053(7) 0.044(7) 0.037(7) -0.012(5) 0.024(6) -0.002(5) C17 0.042(6) 0.029(6) 0.053(8) 0.006(5) 0.025(6) 0.013(5) C18 0.026(5) 0.025(6) 0.026(6) -0.004(5) 0.002(5) 0.000(4) C19 0.026(5) 0.025(6) 0.035(6) -0.003(5) 0.012(5) 0.001(4) C21 0.020(5) 0.051(7) 0.029(6) -0.003(5) 0.006(5) -0.001(5) C22 0.041(6) 0.050(7) 0.030(7) -0.021(6) 0.007(5) -0.017(5) C23 0.031(6) 0.054(8) 0.040(7) -0.005(6) -0.002(5) 0.007(6) C24 0.043(6) 0.026(6) 0.042(7) 0.001(5) 0.028(5) -0.009(5) C25 0.055(7) 0.043(7) 0.047(8) 0.013(6) 0.032(6) 0.013(6) C26 0.043(6) 0.058(8) 0.083(10) -0.023(7) 0.041(7) -0.027(6) C31 0.045(6) 0.035(6) 0.048(7) -0.004(6) 0.025(6) -0.009(5) C32 0.029(6) 0.031(6) 0.040(7) -0.001(5) 0.024(6) -0.007(5) C33A 0.040(6) 0.035(6) 0.041(7) 0.021(6) 0.030(6) 0.007(5) C33 0.034(6) 0.018(5) 0.038(7) -0.003(5) 0.019(5) -0.003(5) C34 0.031(6) 0.032(6) 0.042(7) 0.015(5) 0.018(5) 0.010(5) C35 0.046(7) 0.055(8) 0.069(9) 0.029(7) 0.038(7) 0.017(7) C36 0.088(10) 0.029(7) 0.093(11) 0.020(7) 0.067(9) 0.027(7) C37A 0.039(6) 0.033(7) 0.053(8) 0.014(6) 0.026(6) -0.001(5) C37 0.067(8) 0.030(7) 0.080(10) 0.004(6) 0.045(8) 0.009(6) C41 0.038(6) 0.049(7) 0.036(7) 0.011(6) 0.017(5) 0.010(5) C42 0.050(7) 0.050(7) 0.053(8) 0.007(6) 0.035(6) 0.000(6) C43 0.044(6) 0.065(8) 0.026(6) 0.015(6) 0.017(5) 0.018(6) C44 0.029(5) 0.042(7) 0.031(6) -0.003(5) 0.005(5) -0.001(5) C45 0.044(7) 0.047(8) 0.057(9) -0.022(6) 0.011(6) -0.004(6) C46 0.028(5) 0.055(8) 0.034(7) 0.002(5) 0.007(5) -0.006(5) C50 0.022(5) 0.052(7) 0.028(7) 0.000(5) 0.009(5) 0.013(5) C51 0.035(6) 0.055(8) 0.035(6) 0.012(6) 0.022(5) 0.019(6) C52 0.061(8) 0.063(8) 0.016(6) 0.010(6) 0.019(6) 0.035(7) C53 0.040(6) 0.027(6) 0.070(9) 0.000(6) 0.016(7) 0.019(5) C54 0.033(6) 0.041(7) 0.036(7) 0.004(5) 0.020(6) 0.014(5) C55 0.039(6) 0.079(9) 0.051(8) -0.004(8) 0.015(6) 0.001(7) C56 0.059(8) 0.080(9) 0.097(11) 0.033(8) 0.052(8) 0.018(7) C57 0.103(11) 0.110(12) 0.056(10) 0.004(9) 0.041(8) 0.066(9) C58 0.071(9) 0.043(8) 0.085(11) -0.023(8) -0.004(8) 0.013(7) C59 0.050(7) 0.045(7) 0.048(7) 0.024(6) 0.030(6) 0.017(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. ; # MOLECULAR GEOMETRY 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 N1 1.996(7) . ? Ru1 O1 2.147(6) . ? Ru1 C13 2.167(9) . ? Ru1 C12 2.183(9) . ? Ru1 C11 2.193(8) . ? Ru1 C10 2.197(8) . ? Ru1 C14 2.202(9) . ? Ru1 P1 2.360(2) . ? Ru2 N2 1.994(7) . ? Ru2 O2 2.151(6) . ? Ru2 C51 2.154(8) . ? Ru2 C50 2.182(9) . ? Ru2 C53 2.183(10) . ? Ru2 C52 2.197(9) . ? Ru2 C54 2.198(9) . ? Ru2 P2 2.370(3) . ? N1 N2 1.131(8) . ? P1 C3 1.763(8) . ? P1 C21 1.846(9) . ? P1 C24 1.872(8) . ? P2 C33 1.797(9) . ? P2 C41 1.833(9) . ? P2 C44 1.861(9) . ? O1 C2 1.307(10) . ? O2 C32 1.291(10) . ? C1 C7A 1.512(12) . ? C1 C2 1.515(12) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C3 1.385(12) . ? C3A C4 1.364(12) . ? C3A C7A 1.417(12) . ? C3A C3 1.476(12) . ? C4 C5 1.378(13) . ? C4 H4 0.9500 . ? C5 C6 1.376(14) . ? C5 H5 0.9500 . ? C6 C7 1.380(13) . ? C6 H6 0.9500 . ? C7 C7A 1.368(12) . ? C7 H7 0.9500 . ? C10 C14 1.415(12) . ? C10 C11 1.421(11) . ? C10 C15 1.478(12) . ? C11 C12 1.436(13) . ? C11 C16 1.501(12) . ? C12 C13 1.437(12) . ? C12 C17 1.498(11) . ? C13 C14 1.466(12) . ? C13 C18 1.473(12) . ? C14 C19 1.499(11) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C21 C23 1.507(12) . ? C21 C22 1.555(12) . ? C21 H21 1.0000 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 C25 1.516(13) . ? C24 C26 1.534(12) . ? C24 H24 1.0000 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C31 C37A 1.499(13) . ? C31 C32 1.519(12) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 C33 1.377(13) . ? C33A C34 1.395(13) . ? C33A C37A 1.408(14) . ? C33A C33 1.469(12) . ? C34 C35 1.401(14) . ? C34 H34 0.9500 . ? C35 C36 1.391(16) . ? C35 H35 0.9500 . ? C36 C37 1.367(16) . ? C36 H36 0.9500 . ? C37A C37 1.384(13) . ? C37 H37 0.9500 . ? C41 C42 1.533(12) . ? C41 C43 1.550(12) . ? C41 H41 1.0000 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 C46 1.526(12) . ? C44 C45 1.539(13) . ? C44 H44 1.0000 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C50 C54 1.388(13) . ? C50 C51 1.417(12) . ? C50 C55 1.516(13) . ? C51 C52 1.370(14) . ? C51 C56 1.524(13) . ? C52 C53 1.429(14) . ? C52 C57 1.500(14) . ? C53 C54 1.450(14) . ? C53 C58 1.500(14) . ? C54 C59 1.499(12) . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? C57 H57A 0.9800 . ? C57 H57B 0.9800 . ? C57 H57C 0.9800 . ? C58 H58A 0.9800 . ? C58 H58B 0.9800 . ? C58 H58C 0.9800 . ? C59 H59A 0.9800 . ? C59 H59B 0.9800 . ? C59 H59C 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 N1 Ru1 O1 89.6(2) . . ? N1 Ru1 C13 90.3(3) . . ? O1 Ru1 C13 146.6(3) . . ? N1 Ru1 C12 122.3(3) . . ? O1 Ru1 C12 146.7(3) . . ? C13 Ru1 C12 38.6(3) . . ? N1 Ru1 C11 154.0(3) . . ? O1 Ru1 C11 108.4(3) . . ? C13 Ru1 C11 64.3(3) . . ? C12 Ru1 C11 38.3(3) . . ? N1 Ru1 C10 127.3(3) . . ? O1 Ru1 C10 90.1(3) . . ? C13 Ru1 C10 63.9(3) . . ? C12 Ru1 C10 63.7(3) . . ? C11 Ru1 C10 37.8(3) . . ? N1 Ru1 C14 93.4(3) . . ? O1 Ru1 C14 107.5(3) . . ? C13 Ru1 C14 39.2(3) . . ? C12 Ru1 C14 64.7(3) . . ? C11 Ru1 C14 63.8(3) . . ? C10 Ru1 C14 37.5(3) . . ? N1 Ru1 P1 94.0(2) . . ? O1 Ru1 P1 81.32(16) . . ? C13 Ru1 P1 132.0(2) . . ? C12 Ru1 P1 103.9(2) . . ? C11 Ru1 P1 106.8(2) . . ? C10 Ru1 P1 137.9(2) . . ? C14 Ru1 P1 168.5(2) . . ? N2 Ru2 O2 85.4(3) . . ? N2 Ru2 C51 145.1(3) . . ? O2 Ru2 C51 97.4(3) . . ? N2 Ru2 C50 107.0(3) . . ? O2 Ru2 C50 94.7(3) . . ? C51 Ru2 C50 38.1(3) . . ? N2 Ru2 C53 104.1(4) . . ? O2 Ru2 C53 157.6(3) . . ? C51 Ru2 C53 63.2(4) . . ? C50 Ru2 C53 63.3(4) . . ? N2 Ru2 C52 142.2(4) . . ? O2 Ru2 C52 129.7(4) . . ? C51 Ru2 C52 36.7(4) . . ? C50 Ru2 C52 62.5(4) . . ? C53 Ru2 C52 38.1(4) . . ? N2 Ru2 C54 86.6(3) . . ? O2 Ru2 C54 124.2(3) . . ? C51 Ru2 C54 63.0(3) . . ? C50 Ru2 C54 37.0(3) . . ? C53 Ru2 C54 38.6(4) . . ? C52 Ru2 C54 63.2(3) . . ? N2 Ru2 P2 95.8(2) . . ? O2 Ru2 P2 80.72(18) . . ? C51 Ru2 P2 119.0(3) . . ? C50 Ru2 P2 156.3(3) . . ? C53 Ru2 P2 117.6(3) . . ? C52 Ru2 P2 102.7(3) . . ? C54 Ru2 P2 155.1(3) . . ? N2 N1 Ru1 165.5(7) . . ? N1 N2 Ru2 163.5(6) . . ? C3 P1 C21 108.4(4) . . ? C3 P1 C24 105.5(4) . . ? C21 P1 C24 104.2(4) . . ? C3 P1 Ru1 99.8(3) . . ? C21 P1 Ru1 121.3(3) . . ? C24 P1 Ru1 116.4(3) . . ? C33 P2 C41 105.7(5) . . ? C33 P2 C44 108.7(4) . . ? C41 P2 C44 103.2(4) . . ? C33 P2 Ru2 99.2(3) . . ? C41 P2 Ru2 118.2(3) . . ? C44 P2 Ru2 120.6(3) . . ? C2 O1 Ru1 116.8(5) . . ? C32 O2 Ru2 116.5(6) . . ? C7A C1 C2 102.1(7) . . ? C7A C1 H1A 111.4 . . ? C2 C1 H1A 111.4 . . ? C7A C1 H1B 111.4 . . ? C2 C1 H1B 111.4 . . ? H1A C1 H1B 109.2 . . ? O1 C2 C3 125.4(8) . . ? O1 C2 C1 123.2(8) . . ? C3 C2 C1 111.3(8) . . ? C4 C3A C7A 118.5(8) . . ? C4 C3A C3 133.4(8) . . ? C7A C3A C3 108.2(8) . . ? C2 C3 C3A 108.3(8) . . ? C2 C3 P1 115.1(6) . . ? C3A C3 P1 136.1(6) . . ? C3A C4 C5 120.8(9) . . ? C3A C4 H4 119.6 . . ? C5 C4 H4 119.6 . . ? C6 C5 C4 120.0(9) . . ? C6 C5 H5 120.0 . . ? C4 C5 H5 120.0 . . ? C5 C6 C7 120.8(9) . . ? C5 C6 H6 119.6 . . ? C7 C6 H6 119.6 . . ? C7A C7 C6 118.9(9) . . ? C7A C7 H7 120.5 . . ? C6 C7 H7 120.5 . . ? C7 C7A C3A 121.0(9) . . ? C7 C7A C1 128.9(9) . . ? C3A C7A C1 110.1(8) . . ? C14 C10 C11 110.0(8) . . ? C14 C10 C15 124.7(8) . . ? C11 C10 C15 125.3(9) . . ? C14 C10 Ru1 71.4(5) . . ? C11 C10 Ru1 71.0(5) . . ? C15 C10 Ru1 124.7(6) . . ? C10 C11 C12 107.9(8) . . ? C10 C11 C16 125.5(9) . . ? C12 C11 C16 125.2(8) . . ? C10 C11 Ru1 71.3(5) . . ? C12 C11 Ru1 70.5(5) . . ? C16 C11 Ru1 134.3(6) . . ? C11 C12 C13 107.7(7) . . ? C11 C12 C17 126.8(8) . . ? C13 C12 C17 124.8(9) . . ? C11 C12 Ru1 71.2(5) . . ? C13 C12 Ru1 70.1(5) . . ? C17 C12 Ru1 131.4(7) . . ? C12 C13 C14 107.8(8) . . ? C12 C13 C18 126.1(8) . . ? C14 C13 C18 125.9(8) . . ? C12 C13 Ru1 71.3(5) . . ? C14 C13 Ru1 71.7(5) . . ? C18 C13 Ru1 125.9(6) . . ? C10 C14 C13 106.6(7) . . ? C10 C14 C19 127.1(8) . . ? C13 C14 C19 126.4(8) . . ? C10 C14 Ru1 71.0(5) . . ? C13 C14 Ru1 69.1(5) . . ? C19 C14 Ru1 125.4(6) . . ? C10 C15 H15A 109.5 . . ? C10 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C10 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C11 C16 H16A 109.5 . . ? C11 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C11 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C12 C17 H17A 109.5 . . ? C12 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C12 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C13 C18 H18A 109.5 . . ? C13 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C13 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C14 C19 H19A 109.5 . . ? C14 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C14 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C23 C21 C22 111.6(8) . . ? C23 C21 P1 111.3(7) . . ? C22 C21 P1 111.5(6) . . ? C23 C21 H21 107.4 . . ? C22 C21 H21 107.4 . . ? P1 C21 H21 107.4 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C25 C24 C26 110.2(8) . . ? C25 C24 P1 108.9(6) . . ? C26 C24 P1 116.1(7) . . ? C25 C24 H24 107.1 . . ? C26 C24 H24 107.1 . . ? P1 C24 H24 107.1 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C37A C31 C32 102.9(8) . . ? C37A C31 H31A 111.2 . . ? C32 C31 H31A 111.2 . . ? C37A C31 H31B 111.2 . . ? C32 C31 H31B 111.2 . . ? H31A C31 H31B 109.1 . . ? O2 C32 C33 126.9(9) . . ? O2 C32 C31 122.9(9) . . ? C33 C32 C31 110.1(9) . . ? C34 C33A C37A 120.9(9) . . ? C34 C33A C33 130.7(10) . . ? C37A C33A C33 108.4(9) . . ? C32 C33 C33A 108.9(8) . . ? C32 C33 P2 113.3(7) . . ? C33A C33 P2 137.7(8) . . ? C33A C34 C35 118.3(10) . . ? C33A C34 H34 120.9 . . ? C35 C34 H34 120.9 . . ? C36 C35 C34 119.8(10) . . ? C36 C35 H35 120.1 . . ? C34 C35 H35 120.1 . . ? C37 C36 C35 121.8(10) . . ? C37 C36 H36 119.1 . . ? C35 C36 H36 119.1 . . ? C37 C37A C33A 119.7(10) . . ? C37 C37A C31 130.7(11) . . ? C33A C37A C31 109.6(8) . . ? C36 C37 C37A 119.5(11) . . ? C36 C37 H37 120.3 . . ? C37A C37 H37 120.3 . . ? C42 C41 C43 108.8(8) . . ? C42 C41 P2 109.9(7) . . ? C43 C41 P2 116.2(6) . . ? C42 C41 H41 107.2 . . ? C43 C41 H41 107.2 . . ? P2 C41 H41 107.2 . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C41 C43 H43A 109.5 . . ? C41 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C41 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C46 C44 C45 111.3(8) . . ? C46 C44 P2 110.6(6) . . ? C45 C44 P2 109.2(6) . . ? C46 C44 H44 108.5 . . ? C45 C44 H44 108.5 . . ? P2 C44 H44 108.5 . . ? C44 C45 H45A 109.5 . . ? C44 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C44 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C44 C46 H46A 109.5 . . ? C44 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C44 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C54 C50 C51 108.3(9) . . ? C54 C50 C55 125.6(9) . . ? C51 C50 C55 126.0(9) . . ? C54 C50 Ru2 72.2(5) . . ? C51 C50 Ru2 69.9(5) . . ? C55 C50 Ru2 122.1(6) . . ? C52 C51 C50 109.2(9) . . ? C52 C51 C56 130.0(10) . . ? C50 C51 C56 120.4(10) . . ? C52 C51 Ru2 73.4(5) . . ? C50 C51 Ru2 72.0(5) . . ? C56 C51 Ru2 126.9(7) . . ? C51 C52 C53 108.5(9) . . ? C51 C52 C57 125.7(11) . . ? C53 C52 C57 125.5(12) . . ? C51 C52 Ru2 69.9(5) . . ? C53 C52 Ru2 70.4(5) . . ? C57 C52 Ru2 130.7(7) . . ? C52 C53 C54 106.3(9) . . ? C52 C53 C58 126.2(12) . . ? C54 C53 C58 126.6(11) . . ? C52 C53 Ru2 71.5(6) . . ? C54 C53 Ru2 71.2(6) . . ? C58 C53 Ru2 130.6(7) . . ? C50 C54 C53 107.6(9) . . ? C50 C54 C59 127.3(10) . . ? C53 C54 C59 125.1(10) . . ? C50 C54 Ru2 70.9(5) . . ? C53 C54 Ru2 70.1(6) . . ? C59 C54 Ru2 126.8(6) . . ? C50 C55 H55A 109.5 . . ? C50 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? C50 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? C51 C56 H56A 109.5 . . ? C51 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C51 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? C52 C57 H57A 109.5 . . ? C52 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? C52 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? C53 C58 H58A 109.5 . . ? C53 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? C53 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? C54 C59 H59A 109.5 . . ? C54 C59 H59B 109.5 . . ? H59A C59 H59B 109.5 . . ? C54 C59 H59C 109.5 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Ru1 N1 N2 108(3) . . . . ? C13 Ru1 N1 N2 -38(3) . . . . ? C12 Ru1 N1 N2 -61(3) . . . . ? C11 Ru1 N1 N2 -27(3) . . . . ? C10 Ru1 N1 N2 18(3) . . . . ? C14 Ru1 N1 N2 1(3) . . . . ? P1 Ru1 N1 N2 -170(3) . . . . ? Ru1 N1 N2 Ru2 -82(4) . . . . ? O2 Ru2 N2 N1 92(2) . . . . ? C51 Ru2 N2 N1 -4(3) . . . . ? C50 Ru2 N2 N1 -1(3) . . . . ? C53 Ru2 N2 N1 -67(3) . . . . ? C52 Ru2 N2 N1 -68(3) . . . . ? C54 Ru2 N2 N1 -33(2) . . . . ? P2 Ru2 N2 N1 172(2) . . . . ? N1 Ru1 P1 C3 -78.8(4) . . . . ? O1 Ru1 P1 C3 10.1(3) . . . . ? C13 Ru1 P1 C3 -172.9(4) . . . . ? C12 Ru1 P1 C3 156.5(4) . . . . ? C11 Ru1 P1 C3 116.9(4) . . . . ? C10 Ru1 P1 C3 90.6(5) . . . . ? C14 Ru1 P1 C3 151.0(13) . . . . ? N1 Ru1 P1 C21 39.9(4) . . . . ? O1 Ru1 P1 C21 128.9(4) . . . . ? C13 Ru1 P1 C21 -54.2(5) . . . . ? C12 Ru1 P1 C21 -84.7(4) . . . . ? C11 Ru1 P1 C21 -124.4(4) . . . . ? C10 Ru1 P1 C21 -150.6(5) . . . . ? C14 Ru1 P1 C21 -90.2(13) . . . . ? N1 Ru1 P1 C24 168.4(4) . . . . ? O1 Ru1 P1 C24 -102.7(4) . . . . ? C13 Ru1 P1 C24 74.3(5) . . . . ? C12 Ru1 P1 C24 43.7(4) . . . . ? C11 Ru1 P1 C24 4.0(4) . . . . ? C10 Ru1 P1 C24 -22.2(5) . . . . ? C14 Ru1 P1 C24 38.2(14) . . . . ? N2 Ru2 P2 C33 -70.1(4) . . . . ? O2 Ru2 P2 C33 14.3(3) . . . . ? C51 Ru2 P2 C33 107.6(5) . . . . ? C50 Ru2 P2 C33 94.7(7) . . . . ? C53 Ru2 P2 C33 -179.4(4) . . . . ? C52 Ru2 P2 C33 143.0(4) . . . . ? C54 Ru2 P2 C33 -164.6(6) . . . . ? N2 Ru2 P2 C41 176.3(4) . . . . ? O2 Ru2 P2 C41 -99.3(4) . . . . ? C51 Ru2 P2 C41 -5.9(5) . . . . ? C50 Ru2 P2 C41 -18.9(8) . . . . ? C53 Ru2 P2 C41 67.1(5) . . . . ? C52 Ru2 P2 C41 29.5(5) . . . . ? C54 Ru2 P2 C41 81.9(7) . . . . ? N2 Ru2 P2 C44 48.1(4) . . . . ? O2 Ru2 P2 C44 132.5(4) . . . . ? C51 Ru2 P2 C44 -134.1(5) . . . . ? C50 Ru2 P2 C44 -147.1(7) . . . . ? C53 Ru2 P2 C44 -61.1(5) . . . . ? C52 Ru2 P2 C44 -98.7(5) . . . . ? C54 Ru2 P2 C44 -46.3(7) . . . . ? N1 Ru1 O1 C2 84.7(6) . . . . ? C13 Ru1 O1 C2 174.7(6) . . . . ? C12 Ru1 O1 C2 -111.5(7) . . . . ? C11 Ru1 O1 C2 -114.4(6) . . . . ? C10 Ru1 O1 C2 -148.0(6) . . . . ? C14 Ru1 O1 C2 178.2(6) . . . . ? P1 Ru1 O1 C2 -9.4(5) . . . . ? N2 Ru2 O2 C32 82.0(6) . . . . ? C51 Ru2 O2 C32 -133.0(6) . . . . ? C50 Ru2 O2 C32 -171.2(6) . . . . ? C53 Ru2 O2 C32 -161.3(10) . . . . ? C52 Ru2 O2 C32 -113.5(6) . . . . ? C54 Ru2 O2 C32 164.8(6) . . . . ? P2 Ru2 O2 C32 -14.6(6) . . . . ? Ru1 O1 C2 C3 4.4(11) . . . . ? Ru1 O1 C2 C1 -177.9(6) . . . . ? C7A C1 C2 O1 -178.6(8) . . . . ? C7A C1 C2 C3 -0.6(9) . . . . ? O1 C2 C3 C3A 179.7(8) . . . . ? C1 C2 C3 C3A 1.8(10) . . . . ? O1 C2 C3 P1 6.4(11) . . . . ? C1 C2 C3 P1 -171.5(6) . . . . ? C4 C3A C3 C2 178.4(10) . . . . ? C7A C3A C3 C2 -2.3(10) . . . . ? C4 C3A C3 P1 -10.4(17) . . . . ? C7A C3A C3 P1 168.9(8) . . . . ? C21 P1 C3 C2 -139.6(7) . . . . ? C24 P1 C3 C2 109.2(7) . . . . ? Ru1 P1 C3 C2 -11.8(7) . . . . ? C21 P1 C3 C3A 49.6(11) . . . . ? C24 P1 C3 C3A -61.6(10) . . . . ? Ru1 P1 C3 C3A 177.4(9) . . . . ? C7A C3A C4 C5 1.0(14) . . . . ? C3 C3A C4 C5 -179.8(10) . . . . ? C3A C4 C5 C6 -1.7(16) . . . . ? C4 C5 C6 C7 1.5(16) . . . . ? C5 C6 C7 C7A -0.6(15) . . . . ? C6 C7 C7A C3A -0.1(14) . . . . ? C6 C7 C7A C1 178.2(9) . . . . ? C4 C3A C7A C7 -0.1(13) . . . . ? C3 C3A C7A C7 -179.5(8) . . . . ? C4 C3A C7A C1 -178.6(8) . . . . ? C3 C3A C7A C1 1.9(10) . . . . ? C2 C1 C7A C7 -179.3(9) . . . . ? C2 C1 C7A C3A -0.9(9) . . . . ? N1 Ru1 C10 C14 -29.8(6) . . . . ? O1 Ru1 C10 C14 -119.4(5) . . . . ? C13 Ru1 C10 C14 38.8(5) . . . . ? C12 Ru1 C10 C14 82.0(6) . . . . ? C11 Ru1 C10 C14 119.8(8) . . . . ? P1 Ru1 C10 C14 163.5(4) . . . . ? N1 Ru1 C10 C11 -149.6(5) . . . . ? O1 Ru1 C10 C11 120.8(5) . . . . ? C13 Ru1 C10 C11 -81.0(6) . . . . ? C12 Ru1 C10 C11 -37.8(5) . . . . ? C14 Ru1 C10 C11 -119.8(8) . . . . ? P1 Ru1 C10 C11 43.7(7) . . . . ? N1 Ru1 C10 C15 90.1(8) . . . . ? O1 Ru1 C10 C15 0.5(8) . . . . ? C13 Ru1 C10 C15 158.7(9) . . . . ? C12 Ru1 C10 C15 -158.1(9) . . . . ? C11 Ru1 C10 C15 -120.3(10) . . . . ? C14 Ru1 C10 C15 119.9(10) . . . . ? P1 Ru1 C10 C15 -76.7(8) . . . . ? C14 C10 C11 C12 0.2(10) . . . . ? C15 C10 C11 C12 -179.1(8) . . . . ? Ru1 C10 C11 C12 61.3(6) . . . . ? C14 C10 C11 C16 167.4(8) . . . . ? C15 C10 C11 C16 -12.0(14) . . . . ? Ru1 C10 C11 C16 -131.6(9) . . . . ? C14 C10 C11 Ru1 -61.1(6) . . . . ? C15 C10 C11 Ru1 119.6(9) . . . . ? N1 Ru1 C11 C10 66.9(9) . . . . ? O1 Ru1 C11 C10 -64.8(5) . . . . ? C13 Ru1 C11 C10 79.9(6) . . . . ? C12 Ru1 C11 C10 117.7(7) . . . . ? C14 Ru1 C11 C10 36.1(5) . . . . ? P1 Ru1 C11 C10 -151.1(5) . . . . ? N1 Ru1 C11 C12 -50.8(9) . . . . ? O1 Ru1 C11 C12 177.5(5) . . . . ? C13 Ru1 C11 C12 -37.8(5) . . . . ? C10 Ru1 C11 C12 -117.7(7) . . . . ? C14 Ru1 C11 C12 -81.6(5) . . . . ? P1 Ru1 C11 C12 91.2(5) . . . . ? N1 Ru1 C11 C16 -171.4(7) . . . . ? O1 Ru1 C11 C16 56.9(10) . . . . ? C13 Ru1 C11 C16 -158.4(10) . . . . ? C12 Ru1 C11 C16 -120.6(11) . . . . ? C10 Ru1 C11 C16 121.7(12) . . . . ? C14 Ru1 C11 C16 157.8(10) . . . . ? P1 Ru1 C11 C16 -29.4(10) . . . . ? C10 C11 C12 C13 -0.9(10) . . . . ? C16 C11 C12 C13 -168.0(8) . . . . ? Ru1 C11 C12 C13 60.9(6) . . . . ? C10 C11 C12 C17 170.0(9) . . . . ? C16 C11 C12 C17 2.8(15) . . . . ? Ru1 C11 C12 C17 -128.2(10) . . . . ? C10 C11 C12 Ru1 -61.8(6) . . . . ? C16 C11 C12 Ru1 131.0(9) . . . . ? N1 Ru1 C12 C11 156.4(5) . . . . ? O1 Ru1 C12 C11 -4.4(8) . . . . ? C13 Ru1 C12 C11 117.7(7) . . . . ? C10 Ru1 C12 C11 37.2(5) . . . . ? C14 Ru1 C12 C11 79.1(5) . . . . ? P1 Ru1 C12 C11 -99.7(5) . . . . ? N1 Ru1 C12 C13 38.7(6) . . . . ? O1 Ru1 C12 C13 -122.0(6) . . . . ? C11 Ru1 C12 C13 -117.7(7) . . . . ? C10 Ru1 C12 C13 -80.4(6) . . . . ? C14 Ru1 C12 C13 -38.6(5) . . . . ? P1 Ru1 C12 C13 142.7(5) . . . . ? N1 Ru1 C12 C17 -80.7(9) . . . . ? O1 Ru1 C12 C17 118.6(9) . . . . ? C13 Ru1 C12 C17 -119.4(11) . . . . ? C11 Ru1 C12 C17 122.9(11) . . . . ? C10 Ru1 C12 C17 160.2(10) . . . . ? C14 Ru1 C12 C17 -158.0(10) . . . . ? P1 Ru1 C12 C17 23.2(9) . . . . ? C11 C12 C13 C14 1.2(10) . . . . ? C17 C12 C13 C14 -169.9(9) . . . . ? Ru1 C12 C13 C14 62.8(6) . . . . ? C11 C12 C13 C18 177.1(8) . . . . ? C17 C12 C13 C18 6.0(15) . . . . ? Ru1 C12 C13 C18 -121.3(9) . . . . ? C11 C12 C13 Ru1 -61.6(6) . . . . ? C17 C12 C13 Ru1 127.3(9) . . . . ? N1 Ru1 C13 C12 -148.1(5) . . . . ? O1 Ru1 C13 C12 122.2(6) . . . . ? C11 Ru1 C13 C12 37.5(5) . . . . ? C10 Ru1 C13 C12 79.7(6) . . . . ? C14 Ru1 C13 C12 116.9(7) . . . . ? P1 Ru1 C13 C12 -52.4(6) . . . . ? N1 Ru1 C13 C14 95.0(5) . . . . ? O1 Ru1 C13 C14 5.3(8) . . . . ? C12 Ru1 C13 C14 -116.9(7) . . . . ? C11 Ru1 C13 C14 -79.4(5) . . . . ? C10 Ru1 C13 C14 -37.2(5) . . . . ? P1 Ru1 C13 C14 -169.3(4) . . . . ? N1 Ru1 C13 C18 -26.5(7) . . . . ? O1 Ru1 C13 C18 -116.2(7) . . . . ? C12 Ru1 C13 C18 121.6(10) . . . . ? C11 Ru1 C13 C18 159.1(8) . . . . ? C10 Ru1 C13 C18 -158.7(8) . . . . ? C14 Ru1 C13 C18 -121.5(9) . . . . ? P1 Ru1 C13 C18 69.2(8) . . . . ? C11 C10 C14 C13 0.5(10) . . . . ? C15 C10 C14 C13 179.8(8) . . . . ? Ru1 C10 C14 C13 -60.3(6) . . . . ? C11 C10 C14 C19 -178.7(8) . . . . ? C15 C10 C14 C19 0.6(14) . . . . ? Ru1 C10 C14 C19 120.5(9) . . . . ? C11 C10 C14 Ru1 60.8(6) . . . . ? C15 C10 C14 Ru1 -119.9(8) . . . . ? C12 C13 C14 C10 -1.0(10) . . . . ? C18 C13 C14 C10 -177.0(8) . . . . ? Ru1 C13 C14 C10 61.5(6) . . . . ? C12 C13 C14 C19 178.2(8) . . . . ? C18 C13 C14 C19 2.2(14) . . . . ? Ru1 C13 C14 C19 -119.2(9) . . . . ? C12 C13 C14 Ru1 -62.6(6) . . . . ? C18 C13 C14 Ru1 121.5(9) . . . . ? N1 Ru1 C14 C10 156.7(5) . . . . ? O1 Ru1 C14 C10 66.0(5) . . . . ? C13 Ru1 C14 C10 -117.0(7) . . . . ? C12 Ru1 C14 C10 -79.0(5) . . . . ? C11 Ru1 C14 C10 -36.3(5) . . . . ? P1 Ru1 C14 C10 -73.1(15) . . . . ? N1 Ru1 C14 C13 -86.3(5) . . . . ? O1 Ru1 C14 C13 -177.0(5) . . . . ? C12 Ru1 C14 C13 38.0(5) . . . . ? C11 Ru1 C14 C13 80.7(5) . . . . ? C10 Ru1 C14 C13 117.0(7) . . . . ? P1 Ru1 C14 C13 43.9(15) . . . . ? N1 Ru1 C14 C19 34.1(8) . . . . ? O1 Ru1 C14 C19 -56.5(8) . . . . ? C13 Ru1 C14 C19 120.5(10) . . . . ? C12 Ru1 C14 C19 158.4(9) . . . . ? C11 Ru1 C14 C19 -158.8(9) . . . . ? C10 Ru1 C14 C19 -122.5(10) . . . . ? P1 Ru1 C14 C19 164.4(8) . . . . ? C3 P1 C21 C23 170.6(6) . . . . ? C24 P1 C21 C23 -77.4(7) . . . . ? Ru1 P1 C21 C23 56.2(7) . . . . ? C3 P1 C21 C22 45.3(8) . . . . ? C24 P1 C21 C22 157.3(7) . . . . ? Ru1 P1 C21 C22 -69.1(7) . . . . ? C3 P1 C24 C25 -38.3(8) . . . . ? C21 P1 C24 C25 -152.5(7) . . . . ? Ru1 P1 C24 C25 71.2(7) . . . . ? C3 P1 C24 C26 86.7(8) . . . . ? C21 P1 C24 C26 -27.4(8) . . . . ? Ru1 P1 C24 C26 -163.7(6) . . . . ? Ru2 O2 C32 C33 8.9(11) . . . . ? Ru2 O2 C32 C31 -170.8(6) . . . . ? C37A C31 C32 O2 176.6(8) . . . . ? C37A C31 C32 C33 -3.2(10) . . . . ? O2 C32 C33 C33A -177.8(8) . . . . ? C31 C32 C33 C33A 2.0(10) . . . . ? O2 C32 C33 P2 6.3(12) . . . . ? C31 C32 C33 P2 -173.9(6) . . . . ? C34 C33A C33 C32 177.1(9) . . . . ? C37A C33A C33 C32 0.1(10) . . . . ? C34 C33A C33 P2 -8.5(16) . . . . ? C37A C33A C33 P2 174.6(8) . . . . ? C41 P2 C33 C32 107.6(7) . . . . ? C44 P2 C33 C32 -142.2(7) . . . . ? Ru2 P2 C33 C32 -15.4(7) . . . . ? C41 P2 C33 C33A -66.7(10) . . . . ? C44 P2 C33 C33A 43.5(11) . . . . ? Ru2 P2 C33 C33A 170.4(9) . . . . ? C37A C33A C34 C35 -1.0(13) . . . . ? C33 C33A C34 C35 -177.6(9) . . . . ? C33A C34 C35 C36 1.8(14) . . . . ? C34 C35 C36 C37 -2.9(16) . . . . ? C34 C33A C37A C37 1.0(14) . . . . ? C33 C33A C37A C37 178.4(8) . . . . ? C34 C33A C37A C31 -179.6(8) . . . . ? C33 C33A C37A C31 -2.3(10) . . . . ? C32 C31 C37A C37 -177.4(10) . . . . ? C32 C31 C37A C33A 3.3(10) . . . . ? C35 C36 C37 C37A 2.9(17) . . . . ? C33A C37A C37 C36 -2.0(15) . . . . ? C31 C37A C37 C36 178.8(10) . . . . ? C33 P2 C41 C42 -51.2(7) . . . . ? C44 P2 C41 C42 -165.3(7) . . . . ? Ru2 P2 C41 C42 58.7(7) . . . . ? C33 P2 C41 C43 72.8(9) . . . . ? C44 P2 C41 C43 -41.2(9) . . . . ? Ru2 P2 C41 C43 -177.2(6) . . . . ? C33 P2 C44 C46 51.8(8) . . . . ? C41 P2 C44 C46 163.7(7) . . . . ? Ru2 P2 C44 C46 -61.6(7) . . . . ? C33 P2 C44 C45 174.7(7) . . . . ? C41 P2 C44 C45 -73.4(8) . . . . ? Ru2 P2 C44 C45 61.3(8) . . . . ? N2 Ru2 C50 C54 -59.3(6) . . . . ? O2 Ru2 C50 C54 -146.0(5) . . . . ? C51 Ru2 C50 C54 118.0(9) . . . . ? C53 Ru2 C50 C54 38.2(6) . . . . ? C52 Ru2 C50 C54 81.2(6) . . . . ? P2 Ru2 C50 C54 136.5(6) . . . . ? N2 Ru2 C50 C51 -177.3(6) . . . . ? O2 Ru2 C50 C51 96.0(6) . . . . ? C53 Ru2 C50 C51 -79.8(7) . . . . ? C52 Ru2 C50 C51 -36.8(6) . . . . ? C54 Ru2 C50 C51 -118.0(9) . . . . ? P2 Ru2 C50 C51 18.5(10) . . . . ? N2 Ru2 C50 C55 62.0(8) . . . . ? O2 Ru2 C50 C55 -24.6(8) . . . . ? C51 Ru2 C50 C55 -120.6(11) . . . . ? C53 Ru2 C50 C55 159.6(10) . . . . ? C52 Ru2 C50 C55 -157.4(10) . . . . ? C54 Ru2 C50 C55 121.4(10) . . . . ? P2 Ru2 C50 C55 -102.1(9) . . . . ? C54 C50 C51 C52 2.1(10) . . . . ? C55 C50 C51 C52 -179.8(9) . . . . ? Ru2 C50 C51 C52 64.4(7) . . . . ? C54 C50 C51 C56 174.9(8) . . . . ? C55 C50 C51 C56 -7.1(14) . . . . ? Ru2 C50 C51 C56 -122.8(9) . . . . ? C54 C50 C51 Ru2 -62.3(6) . . . . ? C55 C50 C51 Ru2 115.7(9) . . . . ? N2 Ru2 C51 C52 -112.8(8) . . . . ? O2 Ru2 C51 C52 154.6(6) . . . . ? C50 Ru2 C51 C52 -117.2(9) . . . . ? C53 Ru2 C51 C52 -37.1(6) . . . . ? C54 Ru2 C51 C52 -80.7(7) . . . . ? P2 Ru2 C51 C52 71.1(6) . . . . ? N2 Ru2 C51 C50 4.5(10) . . . . ? O2 Ru2 C51 C50 -88.2(6) . . . . ? C53 Ru2 C51 C50 80.1(7) . . . . ? C52 Ru2 C51 C50 117.2(9) . . . . ? C54 Ru2 C51 C50 36.6(6) . . . . ? P2 Ru2 C51 C50 -171.6(5) . . . . ? N2 Ru2 C51 C56 119.3(9) . . . . ? O2 Ru2 C51 C56 26.7(10) . . . . ? C50 Ru2 C51 C56 114.9(12) . . . . ? C53 Ru2 C51 C56 -165.0(11) . . . . ? C52 Ru2 C51 C56 -127.9(12) . . . . ? C54 Ru2 C51 C56 151.5(11) . . . . ? P2 Ru2 C51 C56 -56.7(10) . . . . ? C50 C51 C52 C53 -3.4(11) . . . . ? C56 C51 C52 C53 -175.3(9) . . . . ? Ru2 C51 C52 C53 60.1(7) . . . . ? C50 C51 C52 C57 170.1(9) . . . . ? C56 C51 C52 C57 -1.8(17) . . . . ? Ru2 C51 C52 C57 -126.4(10) . . . . ? C50 C51 C52 Ru2 -63.5(6) . . . . ? C56 C51 C52 Ru2 124.6(10) . . . . ? N2 Ru2 C52 C51 120.6(7) . . . . ? O2 Ru2 C52 C51 -33.6(7) . . . . ? C50 Ru2 C52 C51 38.3(6) . . . . ? C53 Ru2 C52 C51 119.2(9) . . . . ? C54 Ru2 C52 C51 80.0(6) . . . . ? P2 Ru2 C52 C51 -122.0(6) . . . . ? N2 Ru2 C52 C53 1.4(10) . . . . ? O2 Ru2 C52 C53 -152.8(6) . . . . ? C51 Ru2 C52 C53 -119.2(9) . . . . ? C50 Ru2 C52 C53 -81.0(7) . . . . ? C54 Ru2 C52 C53 -39.2(6) . . . . ? P2 Ru2 C52 C53 118.8(6) . . . . ? N2 Ru2 C52 C57 -119.0(11) . . . . ? O2 Ru2 C52 C57 86.8(13) . . . . ? C51 Ru2 C52 C57 120.4(15) . . . . ? C50 Ru2 C52 C57 158.6(14) . . . . ? C53 Ru2 C52 C57 -120.4(16) . . . . ? C54 Ru2 C52 C57 -159.7(14) . . . . ? P2 Ru2 C52 C57 -1.6(13) . . . . ? C51 C52 C53 C54 3.3(11) . . . . ? C57 C52 C53 C54 -170.2(9) . . . . ? Ru2 C52 C53 C54 63.2(6) . . . . ? C51 C52 C53 C58 172.9(9) . . . . ? C57 C52 C53 C58 -0.6(16) . . . . ? Ru2 C52 C53 C58 -127.3(10) . . . . ? C51 C52 C53 Ru2 -59.8(7) . . . . ? C57 C52 C53 Ru2 126.7(10) . . . . ? N2 Ru2 C53 C52 -179.1(6) . . . . ? O2 Ru2 C53 C52 67.6(13) . . . . ? C51 Ru2 C53 C52 35.8(6) . . . . ? C50 Ru2 C53 C52 78.7(7) . . . . ? C54 Ru2 C53 C52 115.3(9) . . . . ? P2 Ru2 C53 C52 -74.7(7) . . . . ? N2 Ru2 C53 C54 65.6(6) . . . . ? O2 Ru2 C53 C54 -47.7(13) . . . . ? C51 Ru2 C53 C54 -79.5(6) . . . . ? C50 Ru2 C53 C54 -36.6(5) . . . . ? C52 Ru2 C53 C54 -115.3(9) . . . . ? P2 Ru2 C53 C54 170.1(4) . . . . ? N2 Ru2 C53 C58 -56.9(13) . . . . ? O2 Ru2 C53 C58 -170.2(9) . . . . ? C51 Ru2 C53 C58 158.0(14) . . . . ? C50 Ru2 C53 C58 -159.1(14) . . . . ? C52 Ru2 C53 C58 122.2(16) . . . . ? C54 Ru2 C53 C58 -122.5(15) . . . . ? P2 Ru2 C53 C58 47.6(13) . . . . ? C51 C50 C54 C53 0.0(10) . . . . ? C55 C50 C54 C53 -178.0(8) . . . . ? Ru2 C50 C54 C53 -60.8(6) . . . . ? C51 C50 C54 C59 -177.0(8) . . . . ? C55 C50 C54 C59 5.0(15) . . . . ? Ru2 C50 C54 C59 122.2(9) . . . . ? C51 C50 C54 Ru2 60.8(6) . . . . ? C55 C50 C54 Ru2 -117.2(9) . . . . ? C52 C53 C54 C50 -2.0(10) . . . . ? C58 C53 C54 C50 -171.5(9) . . . . ? Ru2 C53 C54 C50 61.3(6) . . . . ? C52 C53 C54 C59 175.1(8) . . . . ? C58 C53 C54 C59 5.6(15) . . . . ? Ru2 C53 C54 C59 -121.6(9) . . . . ? C52 C53 C54 Ru2 -63.3(6) . . . . ? C58 C53 C54 Ru2 127.2(10) . . . . ? N2 Ru2 C54 C50 124.5(6) . . . . ? O2 Ru2 C54 C50 42.4(6) . . . . ? C51 Ru2 C54 C50 -37.7(6) . . . . ? C53 Ru2 C54 C50 -117.7(8) . . . . ? C52 Ru2 C54 C50 -79.1(6) . . . . ? P2 Ru2 C54 C50 -139.0(6) . . . . ? N2 Ru2 C54 C53 -117.8(6) . . . . ? O2 Ru2 C54 C53 160.1(5) . . . . ? C51 Ru2 C54 C53 80.0(6) . . . . ? C50 Ru2 C54 C53 117.7(8) . . . . ? C52 Ru2 C54 C53 38.7(6) . . . . ? P2 Ru2 C54 C53 -21.3(9) . . . . ? N2 Ru2 C54 C59 1.7(9) . . . . ? O2 Ru2 C54 C59 -80.4(10) . . . . ? C51 Ru2 C54 C59 -160.5(11) . . . . ? C50 Ru2 C54 C59 -122.8(12) . . . . ? C53 Ru2 C54 C59 119.5(12) . . . . ? C52 Ru2 C54 C59 158.1(11) . . . . ? P2 Ru2 C54 C59 98.2(10) . . . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 21.97 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.466 _refine_diff_density_min -0.455 _refine_diff_density_rms 0.103 #===END data_dal0740 _database_code_depnum_ccdc_archive 'CCDC 654072' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C37 H47 O P Ru Si' _chemical_formula_sum 'C37 H47 O P Ru Si' _chemical_formula_weight 667.88 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' O O 0.0106 0.0060 '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' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' _symmetry_space_group_name_Hall 'P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 13.0305(12) _cell_length_b 14.5399(13) _cell_length_c 17.6901(16) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3351.6(5) _cell_formula_units_Z 4 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 6217 _cell_measurement_theta_min 2.39 _cell_measurement_theta_max 27.35 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.45 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.324 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1400 _exptl_absorpt_coefficient_mu 0.579 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7687 _exptl_absorpt_correction_T_max 0.8833 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(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 PLATFORM diffractometer/SMART 1000 CCD area detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 8.192 _diffrn_standards_number 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 29235 _diffrn_reflns_av_R_equivalents 0.0224 _diffrn_reflns_av_sigmaI/netI 0.0191 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.81 _diffrn_reflns_theta_max 27.51 _reflns_number_total 7686 _reflns_number_gt 7361 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART (Bruker, 1997)' _computing_cell_refinement 'Bruker SAINT (Bruker, 1997)' _computing_data_reduction 'Bruker SAINT (Bruker, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL (Bruker, 1997)' _computing_publication_material 'Bruker SHELXTL (Bruker, 1997)' _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^)+(0.0444P)^2^+0.5916P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.024(19) _refine_ls_number_reflns 7686 _refine_ls_number_parameters 382 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0290 _refine_ls_R_factor_gt 0.0270 _refine_ls_wR_factor_ref 0.0712 _refine_ls_wR_factor_gt 0.0695 _refine_ls_goodness_of_fit_ref 1.098 _refine_ls_restrained_S_all 1.098 _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 Ru Ru 0.139204(13) 0.007881(10) 0.452673(9) 0.02834(5) Uani 1 1 d D . . H1 H 0.2276(17) 0.062(2) 0.4911(18) 0.075(8) Uiso 1 1 d D . . H2 H 0.156(3) -0.008(2) 0.3670(4) 0.075(8) Uiso 1 1 d D . . P P 0.13871(5) 0.15231(3) 0.39853(3) 0.02904(11) Uani 1 1 d . . . Si Si 0.30451(5) -0.02910(4) 0.41654(3) 0.02903(12) Uani 1 1 d . . . O O 0.35426(14) 0.03933(10) 0.34736(9) 0.0372(3) Uani 1 1 d . . . C1 C 0.42053(19) 0.17622(16) 0.28992(14) 0.0367(5) Uani 1 1 d . . . H1A H 0.4838 0.1800 0.3207 0.044 Uiso 1 1 calc R . . H1B H 0.4362 0.1450 0.2416 0.044 Uiso 1 1 calc R . . C2 C 0.33593(17) 0.12759(15) 0.33207(13) 0.0319(5) Uani 1 1 d . . . C3 C 0.25368(18) 0.18273(15) 0.34568(12) 0.0317(4) Uani 1 1 d . . . C3A C 0.27642(18) 0.27268(15) 0.30889(12) 0.0317(4) Uani 1 1 d . . . C4 C 0.2180(2) 0.35219(16) 0.29959(14) 0.0388(5) Uani 1 1 d . . . H4 H 0.1505 0.3557 0.3197 0.047 Uiso 1 1 calc R . . C5 C 0.2597(2) 0.42662(16) 0.26040(14) 0.0426(6) Uani 1 1 d . . . H5 H 0.2201 0.4809 0.2541 0.051 Uiso 1 1 calc R . . C6 C 0.3573(2) 0.42301(16) 0.23061(14) 0.0444(5) Uani 1 1 d . . . H6 H 0.3847 0.4749 0.2050 0.053 Uiso 1 1 calc R . . C7 C 0.4158(2) 0.34350(17) 0.23804(14) 0.0415(5) Uani 1 1 d . . . H7 H 0.4827 0.3401 0.2168 0.050 Uiso 1 1 calc R . . C7A C 0.37498(19) 0.26965(14) 0.27683(12) 0.0345(5) Uani 1 1 d . . . C10 C 0.1252(2) -0.10421(15) 0.53874(14) 0.0407(5) Uani 1 1 d . . . C11 C 0.0739(2) -0.02471(16) 0.56932(13) 0.0397(5) Uani 1 1 d . . . C12 C -0.01302(18) -0.00573(16) 0.52416(14) 0.0402(5) Uani 1 1 d . . . C13 C -0.01423(19) -0.06894(17) 0.46271(16) 0.0421(5) Uani 1 1 d . . . C14 C 0.0709(2) -0.13118(16) 0.47257(15) 0.0422(5) Uani 1 1 d . . . C15 C 0.2074(2) -0.1599(2) 0.57743(18) 0.0566(7) Uani 1 1 d . . . H15A H 0.1761 -0.1988 0.6164 0.068 Uiso 1 1 calc R . . H15B H 0.2573 -0.1184 0.6009 0.068 Uiso 1 1 calc R . . H15C H 0.2422 -0.1988 0.5401 0.068 Uiso 1 1 calc R . . C16 C 0.1003(3) 0.0211(2) 0.64290(14) 0.0559(7) Uani 1 1 d . . . H16A H 0.0959 0.0880 0.6369 0.067 Uiso 1 1 calc R . . H16B H 0.1703 0.0042 0.6577 0.067 Uiso 1 1 calc R . . H16C H 0.0521 0.0011 0.6820 0.067 Uiso 1 1 calc R . . C17 C -0.1003(2) 0.0561(2) 0.54572(19) 0.0540(7) Uani 1 1 d . . . H17A H -0.1547 0.0197 0.5695 0.065 Uiso 1 1 calc R . . H17B H -0.1273 0.0863 0.5004 0.065 Uiso 1 1 calc R . . H17C H -0.0758 0.1028 0.5814 0.065 Uiso 1 1 calc R . . C18 C -0.1005(2) -0.0861(3) 0.4094(2) 0.0641(8) Uani 1 1 d . . . H18A H -0.1394 -0.0291 0.4021 0.077 Uiso 1 1 calc R . . H18B H -0.1457 -0.1336 0.4302 0.077 Uiso 1 1 calc R . . H18C H -0.0730 -0.1068 0.3607 0.077 Uiso 1 1 calc R . . C19 C 0.0852(3) -0.21713(18) 0.4268(2) 0.0570(8) Uani 1 1 d . . . H19A H 0.1566 -0.2378 0.4308 0.068 Uiso 1 1 calc R . . H19B H 0.0688 -0.2044 0.3737 0.068 Uiso 1 1 calc R . . H19C H 0.0394 -0.2653 0.4459 0.068 Uiso 1 1 calc R . . C21 C 0.13276(19) 0.25276(14) 0.46397(13) 0.0358(5) Uani 1 1 d . . . H21 H 0.1401 0.3093 0.4322 0.043 Uiso 1 1 calc R . . C22 C 0.2227(3) 0.2518(2) 0.5185(2) 0.0623(8) Uani 1 1 d . . . H22A H 0.2868 0.2457 0.4900 0.075 Uiso 1 1 calc R . . H22B H 0.2156 0.1997 0.5532 0.075 Uiso 1 1 calc R . . H22C H 0.2237 0.3093 0.5473 0.075 Uiso 1 1 calc R . . C23 C 0.0322(3) 0.2614(2) 0.5061(2) 0.0693(10) Uani 1 1 d . . . H23A H -0.0248 0.2609 0.4699 0.083 Uiso 1 1 calc R . . H23B H 0.0313 0.3192 0.5346 0.083 Uiso 1 1 calc R . . H23C H 0.0248 0.2096 0.5412 0.083 Uiso 1 1 calc R . . C24 C 0.0371(2) 0.1767(2) 0.32680(17) 0.0501(7) Uani 1 1 d . . . H24 H 0.0299 0.2449 0.3218 0.060 Uiso 1 1 calc R . . C25 C -0.0633(3) 0.1383(4) 0.3452(3) 0.0988(16) Uani 1 1 d . . . H25A H -0.0851 0.1607 0.3949 0.119 Uiso 1 1 calc R . . H25B H -0.0589 0.0710 0.3461 0.119 Uiso 1 1 calc R . . H25C H -0.1133 0.1574 0.3069 0.119 Uiso 1 1 calc R . . C26 C 0.0678(4) 0.1381(4) 0.2506(2) 0.1089(19) Uani 1 1 d . . . H26A H 0.1341 0.1639 0.2355 0.131 Uiso 1 1 calc R . . H26B H 0.0157 0.1543 0.2129 0.131 Uiso 1 1 calc R . . H26C H 0.0734 0.0710 0.2541 0.131 Uiso 1 1 calc R . . C31 C 0.41619(18) -0.02411(15) 0.48596(13) 0.0353(5) Uani 1 1 d . . . C32 C 0.4101(2) 0.00970(18) 0.55906(13) 0.0446(5) Uani 1 1 d . . . H32 H 0.3456 0.0292 0.5784 0.053 Uiso 1 1 calc R . . C33 C 0.4971(2) 0.0156(2) 0.60476(16) 0.0558(7) Uani 1 1 d . . . H33 H 0.4913 0.0387 0.6548 0.067 Uiso 1 1 calc R . . C34 C 0.5907(2) -0.0117(2) 0.57808(19) 0.0600(7) Uani 1 1 d . . . H34 H 0.6493 -0.0085 0.6099 0.072 Uiso 1 1 calc R . . C35 C 0.6000(2) -0.0436(2) 0.5057(2) 0.0594(8) Uani 1 1 d . . . H35 H 0.6652 -0.0614 0.4866 0.071 Uiso 1 1 calc R . . C36 C 0.5137(2) -0.04963(19) 0.46043(18) 0.0485(6) Uani 1 1 d . . . H36 H 0.5208 -0.0719 0.4102 0.058 Uiso 1 1 calc R . . C41 C 0.32035(17) -0.14441(15) 0.36772(13) 0.0320(4) Uani 1 1 d . . . C42 C 0.2824(2) -0.15483(18) 0.29460(15) 0.0411(5) Uani 1 1 d . . . H42 H 0.2518 -0.1036 0.2700 0.049 Uiso 1 1 calc R . . C43 C 0.2883(2) -0.2381(2) 0.25696(17) 0.0562(8) Uani 1 1 d . . . H43 H 0.2625 -0.2438 0.2069 0.067 Uiso 1 1 calc R . . C44 C 0.3319(2) -0.3131(2) 0.2927(2) 0.0610(9) Uani 1 1 d . . . H44 H 0.3347 -0.3707 0.2675 0.073 Uiso 1 1 calc R . . C45 C 0.3713(2) -0.30491(17) 0.3644(2) 0.0558(7) Uani 1 1 d . . . H45 H 0.4019 -0.3564 0.3885 0.067 Uiso 1 1 calc R . . C46 C 0.3660(2) -0.22088(16) 0.40152(15) 0.0426(5) Uani 1 1 d . . . H46 H 0.3941 -0.2153 0.4509 0.051 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 0.02953(8) 0.02317(7) 0.03232(8) 0.00102(6) 0.00429(6) -0.00024(6) P 0.0289(2) 0.0240(2) 0.0343(2) 0.00151(18) 0.0026(2) 0.0016(2) Si 0.0318(3) 0.0232(3) 0.0321(3) 0.0010(2) 0.0030(2) 0.0014(2) O 0.0409(8) 0.0268(7) 0.0438(8) 0.0060(6) 0.0143(7) 0.0048(7) C1 0.0397(12) 0.0334(11) 0.0370(11) 0.0015(9) 0.0104(10) 0.0002(10) C2 0.0375(12) 0.0254(9) 0.0327(10) 0.0009(8) 0.0040(9) -0.0007(8) C3 0.0388(12) 0.0245(10) 0.0319(10) 0.0028(8) 0.0065(9) -0.0016(9) C3A 0.0388(11) 0.0256(10) 0.0307(10) 0.0015(8) 0.0037(9) -0.0028(9) C4 0.0436(12) 0.0314(11) 0.0415(12) 0.0054(9) 0.0042(10) 0.0016(10) C5 0.0586(15) 0.0265(11) 0.0426(13) 0.0051(9) 0.0019(11) 0.0010(10) C6 0.0616(15) 0.0312(11) 0.0406(12) 0.0058(9) 0.0099(12) -0.0045(12) C7 0.0497(14) 0.0356(12) 0.0393(12) 0.0004(10) 0.0123(11) -0.0061(11) C7A 0.0437(13) 0.0276(10) 0.0322(10) -0.0003(8) 0.0061(9) -0.0027(9) C10 0.0446(13) 0.0315(10) 0.0459(12) 0.0104(9) 0.0112(11) -0.0011(9) C11 0.0456(13) 0.0340(11) 0.0394(11) 0.0058(9) 0.0115(9) -0.0027(10) C12 0.0399(11) 0.0304(10) 0.0503(12) 0.0060(10) 0.0145(9) -0.0046(10) C13 0.0376(12) 0.0381(12) 0.0507(14) 0.0014(11) 0.0069(10) -0.0090(9) C14 0.0438(13) 0.0288(10) 0.0539(14) 0.0019(10) 0.0133(11) -0.0078(10) C15 0.0595(17) 0.0505(16) 0.0599(17) 0.0252(13) 0.0101(14) 0.0120(14) C16 0.078(2) 0.0571(17) 0.0330(12) 0.0004(12) 0.0077(12) -0.0067(15) C17 0.0470(15) 0.0442(13) 0.0707(18) 0.0067(15) 0.0212(14) 0.0045(11) C18 0.0471(16) 0.067(2) 0.078(2) -0.0034(17) -0.0070(15) -0.0127(14) C19 0.0607(17) 0.0296(12) 0.081(2) -0.0117(12) 0.0221(16) -0.0110(12) C21 0.0418(12) 0.0244(9) 0.0411(12) -0.0005(8) 0.0097(11) 0.0007(9) C22 0.066(2) 0.0528(17) 0.0677(19) -0.0259(15) -0.0092(16) 0.0001(14) C23 0.068(2) 0.0487(16) 0.091(2) -0.0208(17) 0.0383(19) -0.0035(15) C24 0.0482(15) 0.0413(14) 0.0608(17) 0.0048(12) -0.0176(13) 0.0051(12) C25 0.052(2) 0.133(4) 0.111(3) 0.046(3) -0.022(2) -0.008(2) C26 0.103(3) 0.146(5) 0.077(3) -0.050(3) -0.050(3) 0.047(3) C31 0.0370(11) 0.0289(10) 0.0399(11) 0.0020(9) -0.0008(9) -0.0041(9) C32 0.0472(13) 0.0441(13) 0.0425(12) -0.0013(11) -0.0008(10) -0.0101(11) C33 0.0682(18) 0.0556(17) 0.0435(13) 0.0042(13) -0.0104(12) -0.0178(15) C34 0.0515(15) 0.0524(16) 0.0760(18) 0.0043(16) -0.0233(14) -0.0100(14) C35 0.0388(14) 0.0498(16) 0.090(2) -0.0019(16) -0.0087(14) -0.0036(12) C36 0.0381(13) 0.0461(13) 0.0613(17) -0.0040(13) -0.0018(12) -0.0017(10) C41 0.0308(10) 0.0263(10) 0.0389(11) -0.0014(8) 0.0060(9) 0.0018(8) C42 0.0401(12) 0.0387(13) 0.0445(13) -0.0034(10) 0.0020(10) 0.0005(10) C43 0.0538(17) 0.0606(18) 0.0544(16) -0.0224(14) 0.0088(13) -0.0142(14) C44 0.0595(19) 0.0353(13) 0.088(2) -0.0223(14) 0.0225(17) -0.0076(12) C45 0.0481(15) 0.0277(11) 0.092(2) 0.0037(12) 0.0152(16) 0.0061(11) C46 0.0390(12) 0.0326(11) 0.0561(14) 0.0052(10) 0.0006(12) 0.0012(11) _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 C14 2.237(2) . ? Ru C10 2.238(2) . ? Ru C11 2.282(2) . ? Ru C13 2.297(2) . ? Ru P 2.3081(5) . ? Ru Si 2.3102(6) . ? Ru C12 2.361(2) . ? Ru H1 1.55 . ? Ru H2 1.55 . ? P C3 1.820(2) . ? P C21 1.865(2) . ? P C24 1.868(3) . ? Si O 1.7053(16) . ? Si C41 1.897(2) . ? Si C31 1.906(2) . ? O C2 1.333(3) . ? C1 C7A 1.500(3) . ? C1 C2 1.507(3) . ? C2 C3 1.360(3) . ? C3 C3A 1.491(3) . ? C3A C4 1.394(3) . ? C3A C7A 1.405(3) . ? C4 C5 1.396(3) . ? C5 C6 1.377(4) . ? C6 C7 1.391(4) . ? C7 C7A 1.381(3) . ? C10 C14 1.422(4) . ? C10 C11 1.440(3) . ? C10 C15 1.507(4) . ? C11 C12 1.414(4) . ? C11 C16 1.502(4) . ? C12 C13 1.424(4) . ? C12 C17 1.499(3) . ? C13 C14 1.443(4) . ? C13 C18 1.488(4) . ? C14 C19 1.501(4) . ? C21 C23 1.513(4) . ? C21 C22 1.517(4) . ? C24 C25 1.459(5) . ? C24 C26 1.514(5) . ? C31 C32 1.386(3) . ? C31 C36 1.398(4) . ? C32 C33 1.395(4) . ? C33 C34 1.366(5) . ? C34 C35 1.368(5) . ? C35 C36 1.384(4) . ? C41 C42 1.393(3) . ? C41 C46 1.396(3) . ? C42 C43 1.384(4) . ? C43 C44 1.382(5) . ? C44 C45 1.374(5) . ? C45 C46 1.388(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C14 Ru C10 37.07(10) . . ? C14 Ru C11 61.43(9) . . ? C10 Ru C11 37.15(9) . . ? C14 Ru C13 37.08(9) . . ? C10 Ru C13 61.45(10) . . ? C11 Ru C13 60.31(10) . . ? C14 Ru P 152.45(7) . . ? C10 Ru P 160.86(7) . . ? C11 Ru P 124.28(6) . . ? C13 Ru P 118.17(7) . . ? C14 Ru Si 101.76(7) . . ? C10 Ru Si 95.45(6) . . ? C11 Ru Si 123.32(7) . . ? C13 Ru Si 136.03(7) . . ? P Ru Si 95.71(2) . . ? C14 Ru C12 60.38(9) . . ? C10 Ru C12 60.38(9) . . ? C11 Ru C12 35.41(9) . . ? C13 Ru C12 35.56(9) . . ? P Ru C12 107.23(6) . . ? Si Ru C12 155.80(6) . . ? P Ru H1 74.0(13) . . ? P Ru H2 74.6(13) . . ? Si Ru H1 63.0(12) . . ? Si Ru H2 63.8(13) . . ? C10 Ru H1 97.5(13) . . ? C10 Ru H2 124.4(13) . . ? C11 Ru H1 89.1(13) . . ? C11 Ru H2 155.0(13) . . ? C12 Ru H1 115.6(12) . . ? C12 Ru H2 129.3(13) . . ? C13 Ru H1 149.1(13) . . ? C13 Ru H2 97.3(13) . . ? C14 Ru H1 133.1(13) . . ? C14 Ru H2 94.2(13) . . ? H1 Ru H2 113.5(18) . . ? C3 P C21 99.36(10) . . ? C3 P C24 100.85(12) . . ? C21 P C24 104.09(12) . . ? C3 P Ru 115.59(7) . . ? C21 P Ru 117.06(7) . . ? C24 P Ru 117.17(10) . . ? O Si C41 98.48(9) . . ? O Si C31 98.62(10) . . ? C41 Si C31 104.12(10) . . ? O Si Ru 114.66(6) . . ? C41 Si Ru 115.66(7) . . ? C31 Si Ru 121.66(8) . . ? C2 O Si 129.73(15) . . ? C7A C1 C2 102.23(18) . . ? O C2 C3 132.3(2) . . ? O C2 C1 114.89(19) . . ? C3 C2 C1 112.79(19) . . ? C2 C3 C3A 106.46(19) . . ? C2 C3 P 126.60(17) . . ? C3A C3 P 126.94(17) . . ? C4 C3A C7A 118.5(2) . . ? C4 C3A C3 132.1(2) . . ? C7A C3A C3 109.30(19) . . ? C3A C4 C5 119.2(2) . . ? C6 C5 C4 121.4(2) . . ? C5 C6 C7 120.1(2) . . ? C7A C7 C6 118.8(2) . . ? C7 C7A C3A 121.9(2) . . ? C7 C7A C1 128.9(2) . . ? C3A C7A C1 109.13(19) . . ? C14 C10 C11 107.5(2) . . ? C14 C10 C15 125.4(2) . . ? C11 C10 C15 126.2(3) . . ? C14 C10 Ru 71.43(13) . . ? C11 C10 Ru 73.08(12) . . ? C15 C10 Ru 129.95(18) . . ? C12 C11 C10 108.4(2) . . ? C12 C11 C16 125.9(2) . . ? C10 C11 C16 125.1(3) . . ? C12 C11 Ru 75.35(13) . . ? C10 C11 Ru 69.77(12) . . ? C16 C11 Ru 127.32(17) . . ? C11 C12 C13 108.3(2) . . ? C11 C12 C17 125.5(2) . . ? C13 C12 C17 125.0(2) . . ? C11 C12 Ru 69.24(13) . . ? C13 C12 Ru 69.78(12) . . ? C17 C12 Ru 136.32(17) . . ? C12 C13 C14 107.7(2) . . ? C12 C13 C18 126.9(2) . . ? C14 C13 C18 123.5(3) . . ? C12 C13 Ru 74.66(13) . . ? C14 C13 Ru 69.19(13) . . ? C18 C13 Ru 133.6(2) . . ? C10 C14 C13 108.0(2) . . ? C10 C14 C19 127.8(3) . . ? C13 C14 C19 123.5(3) . . ? C10 C14 Ru 71.50(13) . . ? C13 C14 Ru 73.73(13) . . ? C19 C14 Ru 128.22(18) . . ? C23 C21 C22 110.9(3) . . ? C23 C21 P 113.99(19) . . ? C22 C21 P 110.78(17) . . ? C25 C24 C26 107.0(4) . . ? C25 C24 P 114.3(2) . . ? C26 C24 P 110.3(2) . . ? C32 C31 C36 116.6(2) . . ? C32 C31 Si 124.83(19) . . ? C36 C31 Si 118.39(19) . . ? C31 C32 C33 121.1(3) . . ? C34 C33 C32 120.5(3) . . ? C33 C34 C35 120.1(3) . . ? C34 C35 C36 119.4(3) . . ? C35 C36 C31 122.4(3) . . ? C42 C41 C46 117.6(2) . . ? C42 C41 Si 118.70(17) . . ? C46 C41 Si 123.73(19) . . ? C43 C42 C41 121.5(3) . . ? C44 C43 C42 119.5(3) . . ? C45 C44 C43 120.5(3) . . ? C44 C45 C46 119.6(3) . . ? C45 C46 C41 121.3(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C14 Ru P C3 -125.93(17) . . . . ? C10 Ru P C3 128.9(2) . . . . ? C11 Ru P C3 140.90(12) . . . . ? C13 Ru P C3 -147.46(11) . . . . ? Si Ru P C3 3.47(9) . . . . ? C12 Ru P C3 175.68(11) . . . . ? C14 Ru P C21 117.51(17) . . . . ? C10 Ru P C21 12.3(2) . . . . ? C11 Ru P C21 24.34(12) . . . . ? C13 Ru P C21 95.98(12) . . . . ? Si Ru P C21 -113.09(9) . . . . ? C12 Ru P C21 59.12(11) . . . . ? C14 Ru P C24 -7.22(19) . . . . ? C10 Ru P C24 -112.4(2) . . . . ? C11 Ru P C24 -100.39(14) . . . . ? C13 Ru P C24 -28.74(14) . . . . ? Si Ru P C24 122.19(12) . . . . ? C12 Ru P C24 -65.61(13) . . . . ? C14 Ru Si O 142.56(10) . . . . ? C10 Ru Si O 179.54(10) . . . . ? C11 Ru Si O -154.04(10) . . . . ? C13 Ru Si O 125.88(12) . . . . ? P Ru Si O -16.03(7) . . . . ? C12 Ru Si O -177.61(17) . . . . ? C14 Ru Si C41 28.95(11) . . . . ? C10 Ru Si C41 65.93(11) . . . . ? C11 Ru Si C41 92.35(11) . . . . ? C13 Ru Si C41 12.27(13) . . . . ? P Ru Si C41 -129.64(8) . . . . ? C12 Ru Si C41 68.78(18) . . . . ? C14 Ru Si C31 -98.96(11) . . . . ? C10 Ru Si C31 -61.98(10) . . . . ? C11 Ru Si C31 -35.56(11) . . . . ? C13 Ru Si C31 -115.64(13) . . . . ? P Ru Si C31 102.45(8) . . . . ? C12 Ru Si C31 -59.13(18) . . . . ? C41 Si O C2 154.0(2) . . . . ? C31 Si O C2 -100.2(2) . . . . ? Ru Si O C2 30.6(2) . . . . ? Si O C2 C3 -25.7(4) . . . . ? Si O C2 C1 156.11(17) . . . . ? C7A C1 C2 O 176.26(19) . . . . ? C7A C1 C2 C3 -2.3(3) . . . . ? O C2 C3 C3A -175.2(2) . . . . ? C1 C2 C3 C3A 3.0(3) . . . . ? O C2 C3 P 4.8(4) . . . . ? C1 C2 C3 P -176.93(17) . . . . ? C21 P C3 C2 129.8(2) . . . . ? C24 P C3 C2 -123.7(2) . . . . ? Ru P C3 C2 3.7(2) . . . . ? C21 P C3 C3A -50.1(2) . . . . ? C24 P C3 C3A 56.3(2) . . . . ? Ru P C3 C3A -176.30(17) . . . . ? C2 C3 C3A C4 174.8(3) . . . . ? P C3 C3A C4 -5.3(4) . . . . ? C2 C3 C3A C7A -2.6(3) . . . . ? P C3 C3A C7A 177.36(17) . . . . ? C7A C3A C4 C5 -1.4(4) . . . . ? C3 C3A C4 C5 -178.6(2) . . . . ? C3A C4 C5 C6 0.2(4) . . . . ? C4 C5 C6 C7 1.2(4) . . . . ? C5 C6 C7 C7A -1.2(4) . . . . ? C6 C7 C7A C3A -0.1(4) . . . . ? C6 C7 C7A C1 177.5(2) . . . . ? C4 C3A C7A C7 1.4(3) . . . . ? C3 C3A C7A C7 179.2(2) . . . . ? C4 C3A C7A C1 -176.6(2) . . . . ? C3 C3A C7A C1 1.2(3) . . . . ? C2 C1 C7A C7 -177.2(2) . . . . ? C2 C1 C7A C3A 0.5(3) . . . . ? C11 Ru C10 C14 115.7(2) . . . . ? C13 Ru C10 C14 38.13(15) . . . . ? P Ru C10 C14 132.23(19) . . . . ? Si Ru C10 C14 -102.33(14) . . . . ? C12 Ru C10 C14 79.02(16) . . . . ? C14 Ru C10 C11 -115.7(2) . . . . ? C13 Ru C10 C11 -77.55(16) . . . . ? P Ru C10 C11 16.5(3) . . . . ? Si Ru C10 C11 141.99(14) . . . . ? C12 Ru C10 C11 -36.66(15) . . . . ? C14 Ru C10 C15 121.0(3) . . . . ? C11 Ru C10 C15 -123.3(3) . . . . ? C13 Ru C10 C15 159.1(3) . . . . ? P Ru C10 C15 -106.8(3) . . . . ? Si Ru C10 C15 18.7(3) . . . . ? C12 Ru C10 C15 -160.0(3) . . . . ? C14 C10 C11 C12 2.4(3) . . . . ? C15 C10 C11 C12 -166.5(2) . . . . ? Ru C10 C11 C12 66.00(16) . . . . ? C14 C10 C11 C16 174.4(2) . . . . ? C15 C10 C11 C16 5.5(4) . . . . ? Ru C10 C11 C16 -122.1(2) . . . . ? C14 C10 C11 Ru -63.59(15) . . . . ? C15 C10 C11 Ru 127.5(3) . . . . ? C14 Ru C11 C12 -78.16(16) . . . . ? C10 Ru C11 C12 -116.4(2) . . . . ? C13 Ru C11 C12 -35.49(14) . . . . ? P Ru C11 C12 70.11(15) . . . . ? Si Ru C11 C12 -163.56(12) . . . . ? C14 Ru C11 C10 38.21(15) . . . . ? C13 Ru C11 C10 80.89(16) . . . . ? P Ru C11 C10 -173.51(13) . . . . ? Si Ru C11 C10 -47.19(17) . . . . ? C12 Ru C11 C10 116.4(2) . . . . ? C14 Ru C11 C16 157.6(3) . . . . ? C10 Ru C11 C16 119.3(3) . . . . ? C13 Ru C11 C16 -159.8(3) . . . . ? P Ru C11 C16 -54.2(3) . . . . ? Si Ru C11 C16 72.2(3) . . . . ? C12 Ru C11 C16 -124.3(3) . . . . ? C10 C11 C12 C13 -3.4(3) . . . . ? C16 C11 C12 C13 -175.2(2) . . . . ? Ru C11 C12 C13 59.01(16) . . . . ? C10 C11 C12 C17 164.8(2) . . . . ? C16 C11 C12 C17 -7.1(4) . . . . ? Ru C11 C12 C17 -132.8(2) . . . . ? C10 C11 C12 Ru -62.38(15) . . . . ? C16 C11 C12 Ru 125.8(2) . . . . ? C14 Ru C12 C11 81.38(16) . . . . ? C10 Ru C12 C11 38.49(14) . . . . ? C13 Ru C12 C11 119.9(2) . . . . ? P Ru C12 C11 -125.56(13) . . . . ? Si Ru C12 C11 35.2(2) . . . . ? C14 Ru C12 C13 -38.48(15) . . . . ? C10 Ru C12 C13 -81.37(16) . . . . ? C11 Ru C12 C13 -119.9(2) . . . . ? P Ru C12 C13 114.58(14) . . . . ? Si Ru C12 C13 -84.6(2) . . . . ? C14 Ru C12 C17 -158.4(3) . . . . ? C10 Ru C12 C17 158.7(3) . . . . ? C11 Ru C12 C17 120.2(4) . . . . ? C13 Ru C12 C17 -119.9(4) . . . . ? P Ru C12 C17 -5.3(3) . . . . ? Si Ru C12 C17 155.4(2) . . . . ? C11 C12 C13 C14 3.0(2) . . . . ? C17 C12 C13 C14 -165.2(2) . . . . ? Ru C12 C13 C14 61.69(15) . . . . ? C11 C12 C13 C18 167.8(3) . . . . ? C17 C12 C13 C18 -0.4(4) . . . . ? Ru C12 C13 C18 -133.5(3) . . . . ? C11 C12 C13 Ru -58.68(16) . . . . ? C17 C12 C13 Ru 133.1(2) . . . . ? C14 Ru C13 C12 116.2(2) . . . . ? C10 Ru C13 C12 78.09(16) . . . . ? C11 Ru C13 C12 35.34(14) . . . . ? P Ru C13 C12 -80.14(15) . . . . ? Si Ru C13 C12 143.99(12) . . . . ? C10 Ru C13 C14 -38.12(15) . . . . ? C11 Ru C13 C14 -80.87(17) . . . . ? P Ru C13 C14 163.65(13) . . . . ? Si Ru C13 C14 27.8(2) . . . . ? C12 Ru C13 C14 -116.2(2) . . . . ? C14 Ru C13 C18 -117.0(3) . . . . ? C10 Ru C13 C18 -155.2(3) . . . . ? C11 Ru C13 C18 162.1(3) . . . . ? P Ru C13 C18 46.6(3) . . . . ? Si Ru C13 C18 -89.2(3) . . . . ? C12 Ru C13 C18 126.8(3) . . . . ? C11 C10 C14 C13 -0.5(3) . . . . ? C15 C10 C14 C13 168.5(2) . . . . ? Ru C10 C14 C13 -65.22(16) . . . . ? C11 C10 C14 C19 -170.8(2) . . . . ? C15 C10 C14 C19 -1.8(4) . . . . ? Ru C10 C14 C19 124.5(3) . . . . ? C11 C10 C14 Ru 64.68(15) . . . . ? C15 C10 C14 Ru -126.3(2) . . . . ? C12 C13 C14 C10 -1.5(3) . . . . ? C18 C13 C14 C10 -167.0(2) . . . . ? Ru C13 C14 C10 63.76(15) . . . . ? C12 C13 C14 C19 169.3(2) . . . . ? C18 C13 C14 C19 3.9(4) . . . . ? Ru C13 C14 C19 -125.4(2) . . . . ? C12 C13 C14 Ru -65.27(16) . . . . ? C18 C13 C14 Ru 129.3(3) . . . . ? C11 Ru C14 C10 -38.29(14) . . . . ? C13 Ru C14 C10 -115.9(2) . . . . ? P Ru C14 C10 -148.34(13) . . . . ? Si Ru C14 C10 83.41(14) . . . . ? C12 Ru C14 C10 -79.01(15) . . . . ? C10 Ru C14 C13 115.9(2) . . . . ? C11 Ru C14 C13 77.60(16) . . . . ? P Ru C14 C13 -32.4(2) . . . . ? Si Ru C14 C13 -160.70(14) . . . . ? C12 Ru C14 C13 36.88(15) . . . . ? C10 Ru C14 C19 -124.0(3) . . . . ? C11 Ru C14 C19 -162.3(3) . . . . ? C13 Ru C14 C19 120.1(3) . . . . ? P Ru C14 C19 87.7(3) . . . . ? Si Ru C14 C19 -40.5(3) . . . . ? C12 Ru C14 C19 157.0(3) . . . . ? C3 P C21 C23 167.4(2) . . . . ? C24 P C21 C23 63.6(3) . . . . ? Ru P C21 C23 -67.5(2) . . . . ? C3 P C21 C22 -66.7(2) . . . . ? C24 P C21 C22 -170.5(2) . . . . ? Ru P C21 C22 58.4(2) . . . . ? C3 P C24 C25 165.8(3) . . . . ? C21 P C24 C25 -91.5(3) . . . . ? Ru P C24 C25 39.5(4) . . . . ? C3 P C24 C26 45.1(3) . . . . ? C21 P C24 C26 147.8(3) . . . . ? Ru P C24 C26 -81.2(3) . . . . ? O Si C31 C32 119.4(2) . . . . ? C41 Si C31 C32 -139.5(2) . . . . ? Ru Si C31 C32 -6.7(2) . . . . ? O Si C31 C36 -55.4(2) . . . . ? C41 Si C31 C36 45.6(2) . . . . ? Ru Si C31 C36 178.47(16) . . . . ? C36 C31 C32 C33 -1.4(4) . . . . ? Si C31 C32 C33 -176.4(2) . . . . ? C31 C32 C33 C34 0.3(4) . . . . ? C32 C33 C34 C35 1.2(5) . . . . ? C33 C34 C35 C36 -1.3(5) . . . . ? C34 C35 C36 C31 0.1(5) . . . . ? C32 C31 C36 C35 1.2(4) . . . . ? Si C31 C36 C35 176.5(2) . . . . ? O Si C41 C42 -51.6(2) . . . . ? C31 Si C41 C42 -152.80(19) . . . . ? Ru Si C41 C42 71.0(2) . . . . ? O Si C41 C46 129.9(2) . . . . ? C31 Si C41 C46 28.8(2) . . . . ? Ru Si C41 C46 -107.4(2) . . . . ? C46 C41 C42 C43 0.9(4) . . . . ? Si C41 C42 C43 -177.7(2) . . . . ? C41 C42 C43 C44 0.6(4) . . . . ? C42 C43 C44 C45 -1.4(5) . . . . ? C43 C44 C45 C46 0.7(5) . . . . ? C44 C45 C46 C41 0.8(4) . . . . ? C42 C41 C46 C45 -1.5(4) . . . . ? Si C41 C46 C45 176.9(2) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.889 _refine_diff_density_min -0.287 _refine_diff_density_rms 0.078 #===END data_dal07e3 _database_code_depnum_ccdc_archive 'CCDC 719567' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C34 H48 B O P Ru' _chemical_formula_sum 'C34 H48 B O P Ru' _chemical_formula_weight 615.57 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' B B 0.0013 0.0007 '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' 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 21/m' _symmetry_space_group_name_Hall '-P 2yb' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' '-x, -y, -z' 'x, -y-1/2, z' _cell_length_a 9.6050(6) _cell_length_b 12.3491(8) _cell_length_c 13.2765(9) _cell_angle_alpha 90.00 _cell_angle_beta 96.8204(8) _cell_angle_gamma 90.00 _cell_volume 1563.62(18) _cell_formula_units_Z 2 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 6224 _cell_measurement_theta_min 2.26 _cell_measurement_theta_max 27.47 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.64 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.26 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.307 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 648 _exptl_absorpt_coefficient_mu 0.577 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7091 _exptl_absorpt_correction_T_max 0.8645 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(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 PLATFORM diffractometer/SMART 1000 CCD area detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 8.192 _diffrn_standards_number 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 13179 _diffrn_reflns_av_R_equivalents 0.0151 _diffrn_reflns_av_sigmaI/netI 0.0133 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.54 _diffrn_reflns_theta_max 27.48 _reflns_number_total 3751 _reflns_number_gt 3556 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART (Bruker, 1997)' _computing_cell_refinement 'Bruker SAINT (Bruker, 1997)' _computing_data_reduction 'Bruker SAINT (Bruker, 1997)' _computing_structure_solution 'DIRDIF-96 (Beurskens et al., 1996)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL (Bruker, 1997)' _computing_publication_material 'Bruker SHELXTL (Bruker, 1997)' _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^)+(0.0406P)^2^+0.5359P] 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 3751 _refine_ls_number_parameters 239 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0281 _refine_ls_R_factor_gt 0.0263 _refine_ls_wR_factor_ref 0.0733 _refine_ls_wR_factor_gt 0.0716 _refine_ls_goodness_of_fit_ref 1.140 _refine_ls_restrained_S_all 1.140 _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 Ru Ru 0.145187(16) 0.2500 0.295056(11) 0.02995(7) Uani 1 2 d S . . H1 H 0.033(2) 0.3402(18) 0.3104(17) 0.052(6) Uiso 1 1 d . . . P P 0.18203(7) 0.27161(5) 0.46893(5) 0.0194(2) Uani 0.50 1 d P A -1 O O -0.15482(15) 0.2500 0.37774(11) 0.0312(3) Uani 1 2 d S . . C1 C -0.2229(2) 0.2500 0.54532(15) 0.0274(4) Uani 1 2 d S . . H1A H -0.2826 0.3154 0.5346 0.033 Uiso 0.50 1 calc PR A . H1B H -0.2826 0.1846 0.5346 0.033 Uiso 0.50 1 calc PR . . C2 C -0.1087(2) 0.2500 0.47679(15) 0.0254(4) Uani 1 2 d S A . C3 C 0.0226(2) 0.2500 0.52869(14) 0.0243(4) Uani 1 2 d S . . C3A C 0.0032(2) 0.2500 0.63827(16) 0.0298(4) Uani 1 2 d S A . C4 C 0.0980(3) 0.2500 0.72608(18) 0.0489(7) Uani 1 2 d S . . H4 H 0.1960 0.2500 0.7216 0.059 Uiso 1 2 calc SR A . C5 C 0.0486(3) 0.2500 0.8206(2) 0.0614(9) Uani 1 2 d S A . H5 H 0.1138 0.2500 0.8802 0.074 Uiso 1 2 calc SR . . C6 C -0.0938(3) 0.2500 0.82939(19) 0.0547(8) Uani 1 2 d S . . H6 H -0.1255 0.2500 0.8945 0.066 Uiso 1 2 calc SR A . C7 C -0.1900(3) 0.2500 0.74225(18) 0.0398(5) Uani 1 2 d S A . H7 H -0.2878 0.2500 0.7472 0.048 Uiso 1 2 calc SR . . C7A C -0.1411(2) 0.2500 0.64852(16) 0.0293(4) Uani 1 2 d S A . C10 C 0.3711(2) 0.2500 0.25561(17) 0.0382(5) Uani 1 2 d S . . C11 C 0.29966(17) 0.34302(15) 0.21455(13) 0.0379(4) Uani 1 1 d . . . C12 C 0.18512(16) 0.30722(13) 0.14202(11) 0.0311(3) Uani 1 1 d . . . C13 C 0.5122(2) 0.2500 0.3186(2) 0.0554(8) Uani 1 2 d S . . H13A H 0.5826 0.2803 0.2789 0.067 Uiso 0.50 1 calc PR A . H13B H 0.5382 0.1756 0.3385 0.067 Uiso 0.50 1 calc PR . . H13C H 0.5077 0.2941 0.3796 0.067 Uiso 0.50 1 calc PR . . C14 C 0.3488(3) 0.4578(2) 0.2267(2) 0.0762(8) Uani 1 1 d . . . H14A H 0.4106 0.4653 0.2905 0.091 Uiso 1 1 calc R A . H14B H 0.2677 0.5058 0.2276 0.091 Uiso 1 1 calc R . . H14C H 0.4002 0.4775 0.1699 0.091 Uiso 1 1 calc R . . C15 C 0.0948(2) 0.38083(18) 0.07209(15) 0.0491(5) Uani 1 1 d . . . H15A H 0.1402 0.3942 0.0110 0.059 Uiso 1 1 calc R A . H15B H 0.0818 0.4497 0.1065 0.059 Uiso 1 1 calc R . . H15C H 0.0033 0.3467 0.0531 0.059 Uiso 1 1 calc R . . C21 C 0.2510(4) 0.3979(3) 0.5318(2) 0.0233(7) Uani 0.50 1 d P A -1 H21 H 0.2658 0.3841 0.6065 0.028 Uiso 0.50 1 calc PR A -1 C22 C 0.1420(4) 0.4881(3) 0.5126(3) 0.0382(7) Uani 0.50 1 d P A -1 H22A H 0.0529 0.4638 0.5342 0.046 Uiso 0.50 1 calc PR A -1 H22B H 0.1282 0.5055 0.4401 0.046 Uiso 0.50 1 calc PR A -1 H22C H 0.1748 0.5526 0.5513 0.046 Uiso 0.50 1 calc PR A -1 C23 C 0.3904(3) 0.4345(3) 0.4997(3) 0.0369(7) Uani 0.50 1 d P A -1 H23A H 0.4597 0.3765 0.5132 0.044 Uiso 0.50 1 calc PR A -1 H23B H 0.4229 0.4992 0.5382 0.044 Uiso 0.50 1 calc PR A -1 H23C H 0.3782 0.4513 0.4271 0.044 Uiso 0.50 1 calc PR A -1 C24 C 0.3078(3) 0.1639(3) 0.5210(2) 0.0247(5) Uani 0.50 1 d P A -1 H24 H 0.3779 0.1585 0.4713 0.030 Uiso 0.50 1 calc PR A -1 C25 C 0.2332(5) 0.0548(4) 0.5157(3) 0.0368(9) Uani 0.50 1 d P A -1 H25A H 0.1779 0.0467 0.4491 0.044 Uiso 0.50 1 calc PR A -1 H25B H 0.1708 0.0510 0.5689 0.044 Uiso 0.50 1 calc PR A -1 H25C H 0.3027 -0.0034 0.5255 0.044 Uiso 0.50 1 calc PR A -1 C26 C 0.3951(4) 0.1776(3) 0.6246(3) 0.0381(7) Uani 0.50 1 d P A -1 H26A H 0.4428 0.2479 0.6273 0.046 Uiso 0.50 1 calc SR A -1 H26B H 0.4650 0.1195 0.6346 0.046 Uiso 0.50 1 calc PR A -1 H26C H 0.3334 0.1740 0.6783 0.046 Uiso 0.50 1 calc PR A -1 C31 C -0.1841(2) 0.2500 0.19269(15) 0.0291(4) Uani 1 2 d S . . C32 C -0.23951(16) 0.15241(15) 0.15030(11) 0.0340(3) Uani 1 1 d . A . C33 C -0.34220(18) 0.15408(17) 0.06586(13) 0.0427(4) Uani 1 1 d . . . H33 H -0.3772 0.0874 0.0374 0.051 Uiso 1 1 calc R A . C34 C -0.3937(3) 0.2500 0.02298(19) 0.0484(7) Uani 1 2 d S . . C35 C -0.1996(2) 0.04410(16) 0.19758(14) 0.0447(4) Uani 1 1 d . . . H35A H -0.2398 0.0371 0.2617 0.054 Uiso 1 1 calc R A . H35B H -0.0972 0.0387 0.2105 0.054 Uiso 1 1 calc R . . H35C H -0.2357 -0.0139 0.1513 0.054 Uiso 1 1 calc R . . C36 C -0.5086(4) 0.2500 -0.0661(3) 0.0733(11) Uani 1 2 d S . . H36A H -0.5932 0.2837 -0.0456 0.088 Uiso 0.50 1 calc PR A . H36B H -0.5295 0.1753 -0.0878 0.088 Uiso 0.50 1 calc PR . . H36C H -0.4772 0.2910 -0.1224 0.088 Uiso 0.50 1 calc PR . . B B -0.0741(2) 0.2500 0.29334(18) 0.0292(5) Uani 1 2 d S 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 Ru 0.01702(10) 0.05566(13) 0.01713(10) 0.000 0.00184(6) 0.000 P 0.0163(3) 0.0239(7) 0.0176(3) 0.0003(2) 0.0008(2) 0.0004(2) O 0.0178(6) 0.0566(10) 0.0186(7) 0.000 -0.0003(5) 0.000 C1 0.0196(9) 0.0406(11) 0.0228(9) 0.000 0.0054(7) 0.000 C2 0.0210(9) 0.0351(10) 0.0205(9) 0.000 0.0044(7) 0.000 C3 0.0201(9) 0.0337(10) 0.0193(9) 0.000 0.0028(7) 0.000 C3A 0.0271(10) 0.0428(12) 0.0199(9) 0.000 0.0044(8) 0.000 C4 0.0285(11) 0.095(2) 0.0227(11) 0.000 0.0023(9) 0.000 C5 0.0423(15) 0.121(3) 0.0199(11) 0.000 -0.0006(10) 0.000 C6 0.0476(16) 0.097(2) 0.0210(11) 0.000 0.0113(11) 0.000 C7 0.0322(12) 0.0611(15) 0.0284(11) 0.000 0.0127(9) 0.000 C7A 0.0281(10) 0.0381(11) 0.0220(10) 0.000 0.0048(8) 0.000 C10 0.0207(10) 0.0709(16) 0.0241(10) 0.000 0.0072(8) 0.000 C11 0.0288(8) 0.0502(10) 0.0362(8) -0.0090(7) 0.0105(6) -0.0077(7) C12 0.0292(7) 0.0422(8) 0.0232(7) 0.0034(6) 0.0082(6) -0.0006(6) C13 0.0198(11) 0.112(3) 0.0348(13) 0.000 0.0057(10) 0.000 C14 0.0569(14) 0.0633(15) 0.110(2) -0.0268(15) 0.0152(14) -0.0236(11) C15 0.0463(10) 0.0591(12) 0.0431(10) 0.0217(9) 0.0107(8) 0.0081(9) C21 0.0226(15) 0.0224(18) 0.0241(15) -0.0015(14) -0.0001(11) -0.0002(17) C22 0.0364(17) 0.0252(14) 0.052(2) -0.0020(13) 0.0001(14) 0.0038(14) C23 0.0310(15) 0.0374(16) 0.0424(17) -0.0050(14) 0.0053(13) -0.0120(13) C24 0.0211(12) 0.0255(14) 0.0272(14) 0.0026(11) 0.0010(10) 0.0034(12) C25 0.037(2) 0.0232(19) 0.048(2) 0.0042(18) -0.0047(16) 0.000(2) C26 0.0367(17) 0.0384(16) 0.0359(16) 0.0018(13) -0.0100(13) 0.0086(13) C31 0.0193(9) 0.0496(12) 0.0187(9) 0.000 0.0032(7) 0.000 C32 0.0253(7) 0.0517(9) 0.0248(7) -0.0012(6) 0.0026(6) -0.0039(6) C33 0.0327(8) 0.0651(12) 0.0291(8) -0.0082(8) -0.0020(6) -0.0084(8) C34 0.0324(12) 0.083(2) 0.0270(12) 0.000 -0.0077(10) 0.000 C35 0.0428(10) 0.0489(10) 0.0410(9) 0.0026(8) -0.0008(7) -0.0103(8) C36 0.056(2) 0.113(3) 0.0437(17) 0.000 -0.0264(15) 0.000 B 0.0191(10) 0.0472(13) 0.0211(10) 0.000 0.0017(8) 0.000 _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 B 2.103(2) . ? Ru C12 2.2270(14) 4_565 ? Ru C12 2.2270(14) . ? Ru C11 2.2450(16) . ? Ru C11 2.2450(16) 4_565 ? Ru C10 2.292(2) . ? Ru P 2.3090(7) . ? P C3 1.826(2) . ? P C21 1.854(4) . ? P C24 1.873(3) . ? O C2 1.337(2) . ? O B 1.437(3) . ? C1 C7A 1.497(3) . ? C1 C2 1.506(3) . ? C2 C3 1.363(3) . ? C3 C3A 1.489(3) . ? C3A C4 1.391(3) . ? C3A C7A 1.408(3) . ? C4 C5 1.393(4) . ? C5 C6 1.386(4) . ? C6 C7 1.392(4) . ? C7 C7A 1.381(3) . ? C10 C11 1.414(2) 4_565 ? C10 C11 1.414(2) . ? C10 C13 1.506(3) . ? C11 C12 1.443(2) . ? C11 C14 1.497(3) . ? C12 C12 1.413(3) 4_565 ? C12 C15 1.500(2) . ? C21 C23 1.520(4) . ? C21 C22 1.529(5) . ? C24 C25 1.523(5) . ? C24 C26 1.534(4) . ? C31 C32 1.408(2) . ? C31 C32 1.408(2) 4_565 ? C31 B 1.602(3) . ? C32 C33 1.403(2) . ? C32 C35 1.508(3) . ? C33 C34 1.380(2) . ? C34 C33 1.380(2) 4_565 ? C34 C36 1.518(3) . ? 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 B Ru C12 105.71(7) . 4_565 ? B Ru C12 105.71(7) . . ? C12 Ru C12 37.00(8) 4_565 . ? B Ru C11 135.42(6) . . ? C12 Ru C11 62.15(6) 4_565 . ? C12 Ru C11 37.64(6) . . ? B Ru C11 135.42(6) . 4_565 ? C12 Ru C11 37.64(6) 4_565 4_565 ? C12 Ru C11 62.15(6) . 4_565 ? C11 Ru C11 61.55(9) . 4_565 ? B Ru C10 166.27(9) . . ? C12 Ru C10 61.39(7) 4_565 . ? C12 Ru C10 61.39(7) . . ? C11 Ru C10 36.30(6) . . ? C11 Ru C10 36.30(6) 4_565 . ? B Ru P 92.59(7) . . ? C12 Ru P 157.85(5) 4_565 . ? C12 Ru P 148.53(5) . . ? C11 Ru P 112.67(5) . . ? C11 Ru P 120.24(5) 4_565 . ? C10 Ru P 101.04(6) . . ? C3 P C21 101.58(11) . . ? C3 P C24 105.86(11) . . ? C21 P C24 104.53(17) . . ? C3 P Ru 112.36(7) . . ? C21 P Ru 123.48(12) . . ? C24 P Ru 107.60(9) . . ? C2 O B 128.37(16) . . ? C7A C1 C2 102.23(16) . . ? O C2 C3 132.52(18) . . ? O C2 C1 114.45(17) . . ? C3 C2 C1 113.02(17) . . ? C2 C3 C3A 106.17(17) . . ? C2 C3 P 123.61(15) . . ? C3A C3 P 129.29(15) . . ? C4 C3A C7A 118.2(2) . . ? C4 C3A C3 132.3(2) . . ? C7A C3A C3 109.46(18) . . ? C3A C4 C5 119.7(2) . . ? C6 C5 C4 121.4(2) . . ? C5 C6 C7 119.6(2) . . ? C7A C7 C6 119.1(2) . . ? C7 C7A C3A 122.0(2) . . ? C7 C7A C1 128.8(2) . . ? C3A C7A C1 109.12(18) . . ? C11 C10 C11 108.7(2) 4_565 . ? C11 C10 C13 125.31(10) 4_565 . ? C11 C10 C13 125.31(10) . . ? C11 C10 Ru 70.03(11) 4_565 . ? C11 C10 Ru 70.03(11) . . ? C13 C10 Ru 133.39(16) . . ? C10 C11 C12 107.77(15) . . ? C10 C11 C14 126.55(18) . . ? C12 C11 C14 124.59(19) . . ? C10 C11 Ru 73.67(11) . . ? C12 C11 Ru 70.51(9) . . ? C14 C11 Ru 130.62(15) . . ? C12 C12 C11 107.85(10) 4_565 . ? C12 C12 C15 127.31(11) 4_565 . ? C11 C12 C15 124.51(16) . . ? C12 C12 Ru 71.50(4) 4_565 . ? C11 C12 Ru 71.86(9) . . ? C15 C12 Ru 127.40(11) . . ? C23 C21 C22 110.2(3) . . ? C23 C21 P 113.8(2) . . ? C22 C21 P 109.6(2) . . ? C25 C24 C26 110.1(3) . . ? C25 C24 P 109.4(2) . . ? C26 C24 P 120.9(2) . . ? C32 C31 C32 117.8(2) . 4_565 ? C32 C31 B 120.94(10) . . ? C32 C31 B 120.94(10) 4_565 . ? C33 C32 C31 120.23(17) . . ? C33 C32 C35 117.76(16) . . ? C31 C32 C35 121.85(14) . . ? C34 C33 C32 121.73(18) . . ? C33 C34 C33 118.2(2) 4_565 . ? C33 C34 C36 120.85(11) 4_565 . ? C33 C34 C36 120.85(11) . . ? O B C31 106.67(17) . . ? O B Ru 128.62(15) . . ? C31 B Ru 124.71(15) . . ? 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 B Ru P C3 12.24(3) . . . . ? C12 Ru P C3 -133.90(12) 4_565 . . . ? C12 Ru P C3 138.63(8) . . . . ? C11 Ru P C3 154.58(6) . . . . ? C11 Ru P C3 -136.16(6) 4_565 . . . ? C10 Ru P C3 -169.36(3) . . . . ? B Ru P C21 -109.91(14) . . . . ? C12 Ru P C21 103.94(18) 4_565 . . . ? C12 Ru P C21 16.47(17) . . . . ? C11 Ru P C21 32.42(15) . . . . ? C11 Ru P C21 101.68(15) 4_565 . . . ? C10 Ru P C21 68.48(14) . . . . ? B Ru P C24 128.39(11) . . . . ? C12 Ru P C24 -17.76(16) 4_565 . . . ? C12 Ru P C24 -105.22(13) . . . . ? C11 Ru P C24 -89.27(12) . . . . ? C11 Ru P C24 -20.01(12) 4_565 . . . ? C10 Ru P C24 -53.22(11) . . . . ? B O C2 C3 0.0 . . . . ? B O C2 C1 180.0 . . . . ? C7A C1 C2 O 180.0 . . . . ? C7A C1 C2 C3 0.0 . . . . ? O C2 C3 C3A 180.0 . . . . ? C1 C2 C3 C3A 0.0 . . . . ? O C2 C3 P 10.10(3) . . . . ? C1 C2 C3 P -169.90(3) . . . . ? C21 P C3 C2 117.46(13) . . . . ? C24 P C3 C2 -133.60(10) . . . . ? Ru P C3 C2 -16.42(5) . . . . ? C21 P C3 C3A -49.96(14) . . . . ? C24 P C3 C3A 58.97(11) . . . . ? Ru P C3 C3A 176.16(3) . . . . ? C2 C3 C3A C4 180.0 . . . . ? P C3 C3A C4 -10.88(4) . . . . ? C2 C3 C3A C7A 0.0 . . . . ? P C3 C3A C7A 169.12(4) . . . . ? C7A C3A C4 C5 0.000(1) . . . . ? C3 C3A C4 C5 180.0 . . . . ? C3A C4 C5 C6 0.000(1) . . . . ? C4 C5 C6 C7 0.000(1) . . . . ? C5 C6 C7 C7A 0.000(1) . . . . ? C6 C7 C7A C3A 0.0 . . . . ? C6 C7 C7A C1 180.0 . . . . ? C4 C3A C7A C7 0.0 . . . . ? C3 C3A C7A C7 180.0 . . . . ? C4 C3A C7A C1 180.0 . . . . ? C3 C3A C7A C1 0.0 . . . . ? C2 C1 C7A C7 180.0 . . . . ? C2 C1 C7A C3A 0.0 . . . . ? B Ru C10 C11 -59.81(10) . . . 4_565 ? C12 Ru C10 C11 -38.63(10) 4_565 . . 4_565 ? C12 Ru C10 C11 -81.00(12) . . . 4_565 ? C11 Ru C10 C11 -119.6(2) . . . 4_565 ? P Ru C10 C11 126.95(10) . . . 4_565 ? B Ru C10 C11 59.81(10) . . . . ? C12 Ru C10 C11 81.00(12) 4_565 . . . ? C12 Ru C10 C11 38.63(10) . . . . ? C11 Ru C10 C11 119.6(2) 4_565 . . . ? P Ru C10 C11 -113.43(10) . . . . ? B Ru C10 C13 180.0 . . . . ? C12 Ru C10 C13 -158.81(5) 4_565 . . . ? C12 Ru C10 C13 158.81(5) . . . . ? C11 Ru C10 C13 120.19(10) . . . . ? C11 Ru C10 C13 -120.19(10) 4_565 . . . ? P Ru C10 C13 6.762(15) . . . . ? C11 C10 C11 C12 -3.1(2) 4_565 . . . ? C13 C10 C11 C12 167.7(2) . . . . ? Ru C10 C11 C12 -62.67(11) . . . . ? C11 C10 C11 C14 -171.56(16) 4_565 . . . ? C13 C10 C11 C14 -0.8(3) . . . . ? Ru C10 C11 C14 128.9(2) . . . . ? C11 C10 C11 Ru 59.59(15) 4_565 . . . ? C13 C10 C11 Ru -129.7(2) . . . . ? B Ru C11 C10 -163.00(11) . . . . ? C12 Ru C11 C10 -78.73(11) 4_565 . . . ? C12 Ru C11 C10 -116.17(15) . . . . ? C11 Ru C11 C10 -35.82(12) 4_565 . . . ? P Ru C11 C10 77.41(11) . . . . ? B Ru C11 C12 -46.83(14) . . . . ? C12 Ru C11 C12 37.44(10) 4_565 . . . ? C11 Ru C11 C12 80.36(10) 4_565 . . . ? C10 Ru C11 C12 116.17(15) . . . . ? P Ru C11 C12 -166.41(8) . . . . ? B Ru C11 C14 72.5(2) . . . . ? C12 Ru C11 C14 156.8(2) 4_565 . . . ? C12 Ru C11 C14 119.3(2) . . . . ? C11 Ru C11 C14 -160.31(19) 4_565 . . . ? C10 Ru C11 C14 -124.5(2) . . . . ? P Ru C11 C14 -47.1(2) . . . . ? C10 C11 C12 C12 1.89(15) . . . 4_565 ? C14 C11 C12 C12 170.65(17) . . . 4_565 ? Ru C11 C12 C12 -62.85(4) . . . 4_565 ? C10 C11 C12 C15 -171.86(16) . . . . ? C14 C11 C12 C15 -3.1(3) . . . . ? Ru C11 C12 C15 123.39(16) . . . . ? C10 C11 C12 Ru 64.74(13) . . . . ? C14 C11 C12 Ru -126.50(19) . . . . ? B Ru C12 C12 -95.40(3) . . . 4_565 ? C11 Ru C12 C12 116.72(9) . . . 4_565 ? C11 Ru C12 C12 38.09(6) 4_565 . . 4_565 ? C10 Ru C12 C12 79.49(4) . . . 4_565 ? P Ru C12 C12 141.26(8) . . . 4_565 ? B Ru C12 C11 147.88(9) . . . . ? C12 Ru C12 C11 -116.72(9) 4_565 . . . ? C11 Ru C12 C11 -78.63(14) 4_565 . . . ? C10 Ru C12 C11 -37.24(9) . . . . ? P Ru C12 C11 24.54(15) . . . . ? B Ru C12 C15 27.88(17) . . . . ? C12 Ru C12 C15 123.28(15) 4_565 . . . ? C11 Ru C12 C15 -120.0(2) . . . . ? C11 Ru C12 C15 161.37(18) 4_565 . . . ? C10 Ru C12 C15 -157.24(18) . . . . ? P Ru C12 C15 -95.47(17) . . . . ? C3 P C21 C23 177.6(3) . . . . ? C24 P C21 C23 67.6(3) . . . . ? Ru P C21 C23 -55.5(3) . . . . ? C3 P C21 C22 -58.5(2) . . . . ? C24 P C21 C22 -168.5(2) . . . . ? Ru P C21 C22 68.4(3) . . . . ? C3 P C24 C25 47.4(3) . . . . ? C21 P C24 C25 154.2(2) . . . . ? Ru P C24 C25 -72.9(2) . . . . ? C3 P C24 C26 -81.9(3) . . . . ? C21 P C24 C26 24.9(3) . . . . ? Ru P C24 C26 157.8(2) . . . . ? C32 C31 C32 C33 2.7(3) 4_565 . . . ? B C31 C32 C33 176.04(17) . . . . ? C32 C31 C32 C35 -172.75(12) 4_565 . . . ? B C31 C32 C35 0.6(3) . . . . ? C31 C32 C33 C34 -1.2(3) . . . . ? C35 C32 C33 C34 174.5(2) . . . . ? C32 C33 C34 C33 -0.5(4) . . . 4_565 ? C32 C33 C34 C36 -177.8(3) . . . . ? C2 O B C31 180.0 . . . . ? C2 O B Ru 0.0 . . . . ? C32 C31 B O -86.56(16) . . . . ? C32 C31 B O 86.56(16) 4_565 . . . ? C32 C31 B Ru 93.44(16) . . . . ? C32 C31 B Ru -93.44(16) 4_565 . . . ? C12 Ru B O 160.76(4) 4_565 . . . ? C12 Ru B O -160.76(4) . . . . ? C11 Ru B O -133.20(8) . . . . ? C11 Ru B O 133.20(8) 4_565 . . . ? C10 Ru B O 180.0 . . . . ? P Ru B O -6.643(15) . . . . ? C12 Ru B C31 -19.24(4) 4_565 . . . ? C12 Ru B C31 19.24(4) . . . . ? C11 Ru B C31 46.80(8) . . . . ? C11 Ru B C31 -46.80(8) 4_565 . . . ? C10 Ru B C31 0.0 . . . . ? P Ru B C31 173.357(15) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A B H1 Ru 1.51(2) 1.58(2) 2.103(2) 85.6(11) . _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.453 _refine_diff_density_min -0.585 _refine_diff_density_rms 0.069 #===END