data_2a _audit_creation_method 'manual editing of SHELXL template' _publ_contact_author_name 'Dr. Lisa Rosenberg' _publ_contact_author_address ; Department of Chemistry University of Victoria P.O. Box 3065 Victoria, BC V8W 3V6 Canada ; _publ_contact_author_email lisarose@uvic.ca _publ_contact_author_fax '1(250)7217147' _publ_contact_author_phone '1(250)7217173' _publ_contact_letter ; To: Cambridge Crystallographic Data Centre Please accept the following CIF data in support of a manuscript being submitted to the Journal of the American Chemical Society. Please forward any questions concerning this CIF to Bob McDonald (Bob.McDonald@ualberta.ca). ; _publ_requested_journal 'Journal of the American Chemical Society' _publ_section_title ; A highly reactive ruthenium phosphido complex exhibiting Ru-P \p-bonding ; loop_ _publ_author_name _publ_author_footnote _publ_author_address 'Derrah, Eric J.' . ; Department of Chemistry University of Victoria P.O. Box 3065 Victoria, BC V8W 3V6 Canada ; 'McDonald, Robert' 'X-ray Crystallography Laboratory' ; Department of Chemistry University of Alberta Edmonton, AB T6G 2G2 Canada ; 'Pantazis, Dimitrios A.' . ; Department of Chemistry University of Glasgow Glasgow G12 8QQ United Kingdom ; 'Rosenberg, Lisa' . ; Department of Chemistry University of Victoria P.O. Box 3065 Victoria, BC V8W 3V6 Canada ; _chemical_formula_moiety 'C39 H43 P2 Ru, 0.25(C5 H12)' _chemical_formula_sum 'C40.25 H47 P2 Ru' _chemical_formula_weight 693.79 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' '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/n' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.3907(13) _cell_length_b 13.5621(16) _cell_length_c 25.866(3) _cell_angle_alpha 90.00 _cell_angle_beta 100.432(2) _cell_angle_gamma 90.00 _cell_volume 3584.8(8) _cell_formula_units_Z 4 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 5560 _cell_measurement_theta_min 2.20 _cell_measurement_theta_max 25.91 _exptl_crystal_description prism _exptl_crystal_colour blue _exptl_crystal_size_max 0.46 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.285 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1450 _exptl_absorpt_coefficient_mu 0.553 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7851 _exptl_absorpt_correction_T_max 0.9316 _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 26806 _diffrn_reflns_av_R_equivalents 0.0956 _diffrn_reflns_av_sigmaI/netI 0.0899 _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 -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 1.60 _diffrn_reflns_theta_max 26.42 _reflns_number_total 7309 _reflns_number_gt 4859 _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. ; loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 -0.002 0.000 0.000 258.9 45.4 2 0.497 0.500 0.500 259.0 45.4 _platon_squeeze_details ; Attempts to refine peaks of residual electron density as solvent n-pentane carbon atoms were unsuccessful. The data were corrected for disordered electron density through use of the SQUEEZE procedure (Sluis, P. van der; Spek, A. L. Acta Crystallogr. 1990, A46, 194-201) as implemented in PLATON (Spek, A.L. Acta Crystallogr. 1990, A46, C34. PLATON - a multipurpose crystallographic tool. Utrecht University, Utrecht, The Netherlands). A total solvent-accessible void volume of 521.7 A^3^ with a total electron count of 91 (consistent with one molecule of solvent n-pentane) was found in the unit cell. ; _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^)+(0.0891P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7309 _refine_ls_number_parameters 379 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0940 _refine_ls_R_factor_gt 0.0603 _refine_ls_wR_factor_ref 0.1576 _refine_ls_wR_factor_gt 0.1434 _refine_ls_goodness_of_fit_ref 0.981 _refine_ls_restrained_S_all 0.981 _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 -0.10540(3) 0.04968(3) 0.376929(15) 0.02491(14) Uani 1 1 d . . . P1 P -0.00990(12) -0.09036(10) 0.37157(5) 0.0285(3) Uani 1 1 d . . . P2 P 0.04902(11) 0.13280(9) 0.34241(5) 0.0233(3) Uani 1 1 d . . . C1 C -0.2788(4) 0.0169(4) 0.41168(19) 0.0293(11) Uani 1 1 d . . . H1 H -0.3130 -0.0504 0.4174 0.035 Uiso 1 1 calc R . . C2 C -0.1865(5) 0.0703(4) 0.4481(2) 0.0347(12) Uani 1 1 d . . . H2 H -0.1456 0.0474 0.4841 0.042 Uiso 1 1 calc R . . C3 C -0.1694(5) 0.1654(4) 0.42641(19) 0.0298(11) Uani 1 1 d . . . H3 H -0.1135 0.2198 0.4444 0.036 Uiso 1 1 calc R . . C3A C -0.2605(4) 0.1736(4) 0.37740(18) 0.0269(11) Uani 1 1 d . . . C4 C -0.2908(4) 0.2514(4) 0.34145(19) 0.0306(11) Uani 1 1 d . . . H4 H -0.2475 0.3132 0.3475 0.037 Uiso 1 1 calc R . . C5 C -0.3848(4) 0.2362(4) 0.2972(2) 0.0350(12) Uani 1 1 d . . . H5 H -0.4058 0.2879 0.2723 0.042 Uiso 1 1 calc R . . C6 C -0.4499(4) 0.1457(4) 0.2883(2) 0.0364(13) Uani 1 1 d . . . H6 H -0.5148 0.1380 0.2576 0.044 Uiso 1 1 calc R . . C7 C -0.4237(4) 0.0690(4) 0.3216(2) 0.0314(12) Uani 1 1 d . . . H7 H -0.4691 0.0083 0.3145 0.038 Uiso 1 1 calc R . . C7A C -0.3266(5) 0.0806(4) 0.3680(2) 0.0308(12) Uani 1 1 d . . . C11 C 0.1586(4) -0.1167(4) 0.36175(19) 0.0268(10) Uani 1 1 d . . . H11 H 0.1972 -0.0517 0.3546 0.032 Uiso 1 1 calc R . . C12 C 0.1653(5) -0.1809(4) 0.3139(2) 0.0327(12) Uani 1 1 d . . . H12A H 0.1296 -0.2471 0.3191 0.039 Uiso 1 1 calc R . . H12B H 0.1109 -0.1511 0.2824 0.039 Uiso 1 1 calc R . . C13 C 0.3051(5) -0.1909(4) 0.3050(2) 0.0396(13) Uani 1 1 d . . . H13A H 0.3070 -0.2363 0.2752 0.048 Uiso 1 1 calc R . . H13B H 0.3367 -0.1257 0.2955 0.048 Uiso 1 1 calc R . . C14 C 0.3960(5) -0.2295(5) 0.3532(2) 0.0452(14) Uani 1 1 d . . . H14A H 0.3721 -0.2984 0.3599 0.054 Uiso 1 1 calc R . . H14B H 0.4870 -0.2294 0.3466 0.054 Uiso 1 1 calc R . . C15 C 0.3886(5) -0.1675(5) 0.4009(2) 0.0417(14) Uani 1 1 d . . . H15A H 0.4226 -0.1007 0.3958 0.050 Uiso 1 1 calc R . . H15B H 0.4448 -0.1971 0.4321 0.050 Uiso 1 1 calc R . . C16 C 0.2490(4) -0.1592(4) 0.41110(19) 0.0317(11) Uani 1 1 d . . . H16A H 0.2472 -0.1154 0.4416 0.038 Uiso 1 1 calc R . . H16B H 0.2171 -0.2251 0.4194 0.038 Uiso 1 1 calc R . . C21 C -0.0648(4) -0.2098(4) 0.3941(2) 0.0296(11) Uani 1 1 d . . . H21 H 0.0016 -0.2608 0.3892 0.036 Uiso 1 1 calc R . . C22 C -0.1955(5) -0.2399(4) 0.3607(2) 0.0313(11) Uani 1 1 d . . . H22A H -0.2601 -0.1865 0.3614 0.038 Uiso 1 1 calc R . . H22B H -0.1842 -0.2491 0.3238 0.038 Uiso 1 1 calc R . . C23 C -0.2475(5) -0.3353(4) 0.3807(3) 0.0462(15) Uani 1 1 d . . . H23A H -0.3344 -0.3503 0.3594 0.055 Uiso 1 1 calc R . . H23B H -0.1877 -0.3902 0.3762 0.055 Uiso 1 1 calc R . . C24 C -0.2598(6) -0.3285(5) 0.4378(3) 0.0526(16) Uani 1 1 d . . . H24A H -0.3256 -0.2778 0.4421 0.063 Uiso 1 1 calc R . . H24B H -0.2899 -0.3926 0.4496 0.063 Uiso 1 1 calc R . . C25 C -0.1296(7) -0.3019(5) 0.4709(3) 0.0599(18) Uani 1 1 d . . . H25A H -0.0671 -0.3566 0.4695 0.072 Uiso 1 1 calc R . . H25B H -0.1404 -0.2938 0.5079 0.072 Uiso 1 1 calc R . . C26 C -0.0734(6) -0.2074(4) 0.4523(2) 0.0453(15) Uani 1 1 d . . . H26A H 0.0151 -0.1964 0.4731 0.054 Uiso 1 1 calc R . . H26B H -0.1291 -0.1511 0.4588 0.054 Uiso 1 1 calc R . . C31 C 0.0829(5) 0.0822(3) 0.28043(19) 0.0270(11) Uani 1 1 d . . . C32 C -0.0247(5) 0.0442(4) 0.2447(2) 0.0319(11) Uani 1 1 d . . . H32 H -0.1101 0.0487 0.2528 0.038 Uiso 1 1 calc R . . C33 C -0.0073(6) 0.0009(4) 0.1983(2) 0.0394(13) Uani 1 1 d . . . H33 H -0.0810 -0.0224 0.1742 0.047 Uiso 1 1 calc R . . C34 C 0.1165(6) -0.0089(4) 0.1867(2) 0.0416(14) Uani 1 1 d . . . H34 H 0.1280 -0.0397 0.1549 0.050 Uiso 1 1 calc R . . C35 C 0.2221(5) 0.0254(4) 0.2208(2) 0.0386(13) Uani 1 1 d . . . H35 H 0.3073 0.0181 0.2128 0.046 Uiso 1 1 calc R . . C36 C 0.2060(5) 0.0713(4) 0.2675(2) 0.0330(12) Uani 1 1 d . . . H36 H 0.2805 0.0956 0.2908 0.040 Uiso 1 1 calc R . . C41 C 0.2118(4) 0.1514(3) 0.38260(18) 0.0249(10) Uani 1 1 d . . . C42 C 0.2441(5) 0.1003(4) 0.42995(19) 0.0296(11) Uani 1 1 d . . . H42 H 0.1818 0.0575 0.4409 0.036 Uiso 1 1 calc R . . C43 C 0.3667(5) 0.1116(4) 0.4613(2) 0.0378(13) Uani 1 1 d . . . H43 H 0.3885 0.0751 0.4930 0.045 Uiso 1 1 calc R . . C44 C 0.4566(5) 0.1752(4) 0.4466(2) 0.0387(13) Uani 1 1 d . . . H44 H 0.5406 0.1826 0.4680 0.046 Uiso 1 1 calc R . . C45 C 0.4240(5) 0.2281(4) 0.4007(2) 0.0362(12) Uani 1 1 d . . . H45 H 0.4854 0.2730 0.3908 0.043 Uiso 1 1 calc R . . C46 C 0.3037(4) 0.2169(4) 0.36901(19) 0.0300(11) Uani 1 1 d . . . H46 H 0.2829 0.2542 0.3375 0.036 Uiso 1 1 calc R . . C51 C 0.0050(4) 0.2614(4) 0.32533(19) 0.0253(10) Uani 1 1 d . . . C52 C 0.0291(5) 0.3345(4) 0.3635(2) 0.0345(12) Uani 1 1 d . . . H52 H 0.0776 0.3187 0.3972 0.041 Uiso 1 1 calc R . . C53 C -0.0156(5) 0.4288(4) 0.3534(2) 0.0397(13) Uani 1 1 d . . . H53 H 0.0024 0.4776 0.3801 0.048 Uiso 1 1 calc R . . C54 C -0.0869(5) 0.4534(4) 0.3045(2) 0.0401(13) Uani 1 1 d . . . H54 H -0.1194 0.5185 0.2978 0.048 Uiso 1 1 calc R . . C55 C -0.1102(5) 0.3830(4) 0.2660(2) 0.0340(12) Uani 1 1 d . . . H55 H -0.1577 0.4003 0.2323 0.041 Uiso 1 1 calc R . . C56 C -0.0661(4) 0.2876(4) 0.27511(19) 0.0294(11) Uani 1 1 d . . . H56 H -0.0831 0.2397 0.2479 0.035 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 0.0184(2) 0.0297(2) 0.0274(2) 0.00444(17) 0.00638(15) 0.00065(16) P1 0.0203(6) 0.0315(7) 0.0339(7) 0.0068(6) 0.0052(5) 0.0025(5) P2 0.0163(6) 0.0321(7) 0.0218(6) 0.0022(5) 0.0044(5) 0.0000(5) C1 0.023(2) 0.041(3) 0.027(3) 0.001(2) 0.013(2) -0.003(2) C2 0.039(3) 0.040(3) 0.028(3) 0.010(2) 0.011(2) 0.000(2) C3 0.030(3) 0.037(3) 0.025(3) -0.002(2) 0.010(2) -0.005(2) C3A 0.022(2) 0.036(3) 0.023(2) -0.004(2) 0.0057(19) -0.001(2) C4 0.021(2) 0.041(3) 0.032(3) 0.002(2) 0.010(2) 0.007(2) C5 0.023(3) 0.050(3) 0.033(3) 0.008(2) 0.008(2) 0.009(2) C6 0.019(2) 0.064(4) 0.025(3) -0.008(3) 0.000(2) 0.006(2) C7 0.017(2) 0.046(3) 0.033(3) -0.013(2) 0.008(2) -0.003(2) C7A 0.024(2) 0.036(3) 0.037(3) -0.007(2) 0.017(2) -0.001(2) C11 0.021(2) 0.032(3) 0.027(3) -0.001(2) 0.004(2) -0.001(2) C12 0.027(3) 0.041(3) 0.029(3) -0.006(2) 0.000(2) -0.001(2) C13 0.037(3) 0.046(3) 0.036(3) -0.011(3) 0.008(2) 0.008(2) C14 0.030(3) 0.059(4) 0.047(3) -0.005(3) 0.008(3) 0.018(3) C15 0.024(3) 0.064(4) 0.032(3) 0.001(3) -0.007(2) 0.010(2) C16 0.028(3) 0.042(3) 0.022(3) 0.002(2) -0.001(2) 0.004(2) C21 0.018(2) 0.034(3) 0.035(3) 0.003(2) -0.003(2) 0.001(2) C22 0.024(2) 0.043(3) 0.026(3) -0.004(2) 0.004(2) 0.000(2) C23 0.030(3) 0.037(3) 0.069(4) -0.004(3) 0.002(3) -0.008(2) C24 0.052(4) 0.048(4) 0.062(4) 0.016(3) 0.021(3) -0.012(3) C25 0.075(5) 0.062(4) 0.040(4) 0.019(3) 0.006(3) -0.015(4) C26 0.053(4) 0.053(4) 0.025(3) 0.011(3) -0.008(3) -0.015(3) C31 0.029(3) 0.028(3) 0.023(3) 0.003(2) 0.003(2) 0.000(2) C32 0.027(3) 0.035(3) 0.031(3) 0.008(2) -0.002(2) 0.002(2) C33 0.051(3) 0.036(3) 0.027(3) 0.001(2) -0.005(3) 0.001(3) C34 0.065(4) 0.036(3) 0.024(3) -0.001(2) 0.008(3) 0.007(3) C35 0.043(3) 0.050(4) 0.026(3) -0.004(2) 0.016(2) 0.002(3) C36 0.030(3) 0.038(3) 0.032(3) -0.002(2) 0.009(2) -0.003(2) C41 0.019(2) 0.035(3) 0.020(2) -0.003(2) 0.0038(18) 0.0030(19) C42 0.029(3) 0.038(3) 0.023(3) -0.001(2) 0.008(2) 0.000(2) C43 0.039(3) 0.054(4) 0.019(3) -0.001(2) 0.000(2) 0.004(3) C44 0.021(3) 0.067(4) 0.027(3) -0.014(3) -0.001(2) 0.002(2) C45 0.025(3) 0.048(3) 0.038(3) -0.005(3) 0.011(2) -0.009(2) C46 0.023(2) 0.046(3) 0.022(2) 0.000(2) 0.005(2) 0.001(2) C51 0.018(2) 0.031(3) 0.028(3) 0.002(2) 0.0065(19) -0.0025(19) C52 0.031(3) 0.041(3) 0.030(3) 0.000(2) 0.002(2) 0.000(2) C53 0.044(3) 0.033(3) 0.042(3) -0.007(2) 0.010(3) -0.003(2) C54 0.040(3) 0.032(3) 0.050(4) 0.012(3) 0.014(3) 0.003(2) C55 0.035(3) 0.041(3) 0.026(3) 0.008(2) 0.005(2) 0.000(2) C56 0.028(3) 0.033(3) 0.029(3) 0.005(2) 0.011(2) 0.000(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru P1 2.1589(14) . ? Ru C2 2.178(5) . ? Ru C1 2.200(4) . ? Ru C3 2.202(5) . ? Ru P2 2.2719(12) . ? Ru C7A 2.307(5) . ? Ru C3A 2.330(5) . ? P1 C21 1.847(5) . ? P1 C11 1.849(5) . ? P2 C41 1.835(5) . ? P2 C31 1.836(5) . ? P2 C51 1.837(5) . ? C1 C2 1.417(7) . ? C1 C7A 1.438(7) . ? C2 C3 1.430(7) . ? C3 C3A 1.443(7) . ? C3A C4 1.404(7) . ? C3A C7A 1.435(7) . ? C4 C5 1.380(7) . ? C5 C6 1.400(7) . ? C6 C7 1.347(7) . ? C7 C7A 1.429(7) . ? C11 C12 1.525(7) . ? C11 C16 1.552(6) . ? C12 C13 1.516(7) . ? C13 C14 1.514(7) . ? C14 C15 1.508(8) . ? C15 C16 1.525(7) . ? C21 C26 1.524(7) . ? C21 C22 1.528(7) . ? C22 C23 1.528(7) . ? C23 C24 1.508(9) . ? C24 C25 1.508(8) . ? C25 C26 1.523(8) . ? C31 C36 1.388(7) . ? C31 C32 1.412(7) . ? C32 C33 1.377(7) . ? C33 C34 1.379(8) . ? C34 C35 1.359(8) . ? C35 C36 1.394(7) . ? C41 C42 1.394(7) . ? C41 C46 1.396(7) . ? C42 C43 1.389(7) . ? C43 C44 1.374(8) . ? C44 C45 1.377(8) . ? C45 C46 1.373(7) . ? C51 C52 1.389(7) . ? C51 C56 1.418(7) . ? C52 C53 1.369(7) . ? C53 C54 1.386(8) . ? C54 C55 1.370(8) . ? C55 C56 1.379(7) . ? 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 P1 Ru C2 114.84(14) . . ? P1 Ru C1 105.58(14) . . ? C2 Ru C1 37.76(19) . . ? P1 Ru C3 148.72(14) . . ? C2 Ru C3 38.11(18) . . ? C1 Ru C3 63.30(18) . . ? P1 Ru P2 92.62(5) . . ? C2 Ru P2 132.65(14) . . ? C1 Ru P2 161.79(14) . . ? C3 Ru P2 100.60(13) . . ? P1 Ru C7A 127.94(13) . . ? C2 Ru C7A 61.99(19) . . ? C1 Ru C7A 37.12(18) . . ? C3 Ru C7A 61.87(18) . . ? P2 Ru C7A 129.21(13) . . ? P1 Ru C3A 164.00(12) . . ? C2 Ru C3A 61.91(18) . . ? C1 Ru C3A 61.64(18) . . ? C3 Ru C3A 36.99(17) . . ? P2 Ru C3A 100.52(12) . . ? C7A Ru C3A 36.07(17) . . ? C21 P1 C11 103.2(2) . . ? C21 P1 Ru 125.44(17) . . ? C11 P1 Ru 129.54(17) . . ? C41 P2 C31 104.1(2) . . ? C41 P2 C51 99.8(2) . . ? C31 P2 C51 102.9(2) . . ? C41 P2 Ru 119.30(16) . . ? C31 P2 Ru 114.72(16) . . ? C51 P2 Ru 113.76(14) . . ? C2 C1 C7A 108.2(4) . . ? C2 C1 Ru 70.3(3) . . ? C7A C1 Ru 75.5(3) . . ? C1 C2 C3 108.5(5) . . ? C1 C2 Ru 72.0(3) . . ? C3 C2 Ru 71.9(3) . . ? C2 C3 C3A 107.8(4) . . ? C2 C3 Ru 70.0(3) . . ? C3A C3 Ru 76.3(3) . . ? C4 C3A C7A 120.3(4) . . ? C4 C3A C3 132.3(5) . . ? C7A C3A C3 107.4(4) . . ? C4 C3A Ru 127.7(3) . . ? C7A C3A Ru 71.1(3) . . ? C3 C3A Ru 66.7(3) . . ? C5 C4 C3A 118.5(5) . . ? C4 C5 C6 121.1(5) . . ? C7 C6 C5 122.4(5) . . ? C6 C7 C7A 118.9(5) . . ? C7 C7A C3A 118.8(5) . . ? C7 C7A C1 133.2(5) . . ? C3A C7A C1 107.9(4) . . ? C7 C7A Ru 127.1(3) . . ? C3A C7A Ru 72.8(3) . . ? C1 C7A Ru 67.4(3) . . ? C12 C11 C16 110.2(4) . . ? C12 C11 P1 113.9(3) . . ? C16 C11 P1 113.9(3) . . ? C13 C12 C11 111.1(4) . . ? C14 C13 C12 112.3(5) . . ? C15 C14 C13 111.3(4) . . ? C14 C15 C16 111.9(4) . . ? C15 C16 C11 109.8(4) . . ? C26 C21 C22 111.1(4) . . ? C26 C21 P1 111.7(4) . . ? C22 C21 P1 110.4(3) . . ? C23 C22 C21 111.5(4) . . ? C24 C23 C22 112.2(5) . . ? C25 C24 C23 110.1(5) . . ? C24 C25 C26 112.2(5) . . ? C25 C26 C21 112.8(5) . . ? C36 C31 C32 117.3(5) . . ? C36 C31 P2 125.6(4) . . ? C32 C31 P2 117.0(4) . . ? C33 C32 C31 120.8(5) . . ? C32 C33 C34 120.3(5) . . ? C35 C34 C33 120.1(5) . . ? C34 C35 C36 120.3(5) . . ? C31 C36 C35 121.1(5) . . ? C42 C41 C46 118.1(4) . . ? C42 C41 P2 118.7(4) . . ? C46 C41 P2 123.2(4) . . ? C43 C42 C41 120.6(5) . . ? C44 C43 C42 120.3(5) . . ? C43 C44 C45 119.5(5) . . ? C46 C45 C44 120.9(5) . . ? C45 C46 C41 120.7(5) . . ? C52 C51 C56 118.0(5) . . ? C52 C51 P2 120.1(4) . . ? C56 C51 P2 121.6(4) . . ? C53 C52 C51 121.3(5) . . ? C52 C53 C54 120.3(5) . . ? C55 C54 C53 119.5(5) . . ? C54 C55 C56 121.3(5) . . ? C55 C56 C51 119.6(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 C2 Ru P1 C21 37.5(3) . . . . ? C1 Ru P1 C21 -1.7(2) . . . . ? C3 Ru P1 C21 62.3(3) . . . . ? P2 Ru P1 C21 177.7(2) . . . . ? C7A Ru P1 C21 -35.3(3) . . . . ? C3A Ru P1 C21 -36.9(5) . . . . ? C2 Ru P1 C11 -124.3(3) . . . . ? C1 Ru P1 C11 -163.5(2) . . . . ? C3 Ru P1 C11 -99.6(3) . . . . ? P2 Ru P1 C11 15.9(2) . . . . ? C7A Ru P1 C11 162.9(3) . . . . ? C3A Ru P1 C11 161.3(5) . . . . ? P1 Ru P2 C41 -73.16(18) . . . . ? C2 Ru P2 C41 54.7(3) . . . . ? C1 Ru P2 C41 105.0(5) . . . . ? C3 Ru P2 C41 78.4(2) . . . . ? C7A Ru P2 C41 140.6(2) . . . . ? C3A Ru P2 C41 116.0(2) . . . . ? P1 Ru P2 C31 51.30(17) . . . . ? C2 Ru P2 C31 179.2(2) . . . . ? C1 Ru P2 C31 -130.6(4) . . . . ? C3 Ru P2 C31 -157.2(2) . . . . ? C7A Ru P2 C31 -95.0(2) . . . . ? C3A Ru P2 C31 -119.5(2) . . . . ? P1 Ru P2 C51 169.48(17) . . . . ? C2 Ru P2 C51 -62.7(3) . . . . ? C1 Ru P2 C51 -12.4(5) . . . . ? C3 Ru P2 C51 -39.0(2) . . . . ? C7A Ru P2 C51 23.2(2) . . . . ? C3A Ru P2 C51 -1.4(2) . . . . ? P1 Ru C1 C2 110.6(3) . . . . ? C3 Ru C1 C2 -37.9(3) . . . . ? P2 Ru C1 C2 -67.4(5) . . . . ? C7A Ru C1 C2 -115.8(4) . . . . ? C3A Ru C1 C2 -79.8(3) . . . . ? P1 Ru C1 C7A -133.6(3) . . . . ? C2 Ru C1 C7A 115.8(4) . . . . ? C3 Ru C1 C7A 77.9(3) . . . . ? P2 Ru C1 C7A 48.4(6) . . . . ? C3A Ru C1 C7A 36.0(3) . . . . ? C7A C1 C2 C3 -3.5(6) . . . . ? Ru C1 C2 C3 63.0(3) . . . . ? C7A C1 C2 Ru -66.5(3) . . . . ? P1 Ru C2 C1 -83.4(3) . . . . ? C3 Ru C2 C1 117.2(4) . . . . ? P2 Ru C2 C1 156.9(2) . . . . ? C7A Ru C2 C1 38.0(3) . . . . ? C3A Ru C2 C1 79.0(3) . . . . ? P1 Ru C2 C3 159.4(2) . . . . ? C1 Ru C2 C3 -117.2(4) . . . . ? P2 Ru C2 C3 39.7(4) . . . . ? C7A Ru C2 C3 -79.2(3) . . . . ? C3A Ru C2 C3 -38.1(3) . . . . ? C1 C2 C3 C3A 4.5(6) . . . . ? Ru C2 C3 C3A 67.6(3) . . . . ? C1 C2 C3 Ru -63.1(3) . . . . ? P1 Ru C3 C2 -38.0(4) . . . . ? C1 Ru C3 C2 37.6(3) . . . . ? P2 Ru C3 C2 -151.4(3) . . . . ? C7A Ru C3 C2 79.6(3) . . . . ? C3A Ru C3 C2 115.1(4) . . . . ? P1 Ru C3 C3A -153.1(2) . . . . ? C2 Ru C3 C3A -115.1(4) . . . . ? C1 Ru C3 C3A -77.5(3) . . . . ? P2 Ru C3 C3A 93.5(3) . . . . ? C7A Ru C3 C3A -35.5(3) . . . . ? C2 C3 C3A C4 176.1(5) . . . . ? Ru C3 C3A C4 -120.5(5) . . . . ? C2 C3 C3A C7A -3.7(5) . . . . ? Ru C3 C3A C7A 59.7(3) . . . . ? C2 C3 C3A Ru -63.4(3) . . . . ? P1 Ru C3A C4 -112.1(5) . . . . ? C2 Ru C3A C4 165.6(5) . . . . ? C1 Ru C3A C4 -151.3(5) . . . . ? C3 Ru C3A C4 126.3(6) . . . . ? P2 Ru C3A C4 32.6(4) . . . . ? C7A Ru C3A C4 -114.2(5) . . . . ? P1 Ru C3A C7A 2.1(6) . . . . ? C2 Ru C3A C7A -80.1(3) . . . . ? C1 Ru C3A C7A -37.0(3) . . . . ? C3 Ru C3A C7A -119.5(4) . . . . ? P2 Ru C3A C7A 146.9(3) . . . . ? P1 Ru C3A C3 121.6(4) . . . . ? C2 Ru C3A C3 39.3(3) . . . . ? C1 Ru C3A C3 82.4(3) . . . . ? P2 Ru C3A C3 -93.7(3) . . . . ? C7A Ru C3A C3 119.5(4) . . . . ? C7A C3A C4 C5 -0.1(7) . . . . ? C3 C3A C4 C5 -179.9(5) . . . . ? Ru C3A C4 C5 88.6(5) . . . . ? C3A C4 C5 C6 0.6(7) . . . . ? C4 C5 C6 C7 -0.7(8) . . . . ? C5 C6 C7 C7A 0.3(7) . . . . ? C6 C7 C7A C3A 0.1(7) . . . . ? C6 C7 C7A C1 177.6(5) . . . . ? C6 C7 C7A Ru -89.6(5) . . . . ? C4 C3A C7A C7 -0.2(7) . . . . ? C3 C3A C7A C7 179.6(4) . . . . ? Ru C3A C7A C7 -123.5(4) . . . . ? C4 C3A C7A C1 -178.3(4) . . . . ? C3 C3A C7A C1 1.6(5) . . . . ? Ru C3A C7A C1 58.5(3) . . . . ? C4 C3A C7A Ru 123.2(4) . . . . ? C3 C3A C7A Ru -56.9(3) . . . . ? C2 C1 C7A C7 -176.4(5) . . . . ? Ru C1 C7A C7 120.4(5) . . . . ? C2 C1 C7A C3A 1.2(5) . . . . ? Ru C1 C7A C3A -61.9(3) . . . . ? C2 C1 C7A Ru 63.1(3) . . . . ? P1 Ru C7A C7 -65.7(5) . . . . ? C2 Ru C7A C7 -166.6(5) . . . . ? C1 Ru C7A C7 -127.9(6) . . . . ? C3 Ru C7A C7 150.0(5) . . . . ? P2 Ru C7A C7 69.6(5) . . . . ? C3A Ru C7A C7 113.6(6) . . . . ? P1 Ru C7A C3A -179.3(2) . . . . ? C2 Ru C7A C3A 79.9(3) . . . . ? C1 Ru C7A C3A 118.5(4) . . . . ? C3 Ru C7A C3A 36.4(3) . . . . ? P2 Ru C7A C3A -43.9(3) . . . . ? P1 Ru C7A C1 62.2(3) . . . . ? C2 Ru C7A C1 -38.6(3) . . . . ? C3 Ru C7A C1 -82.1(3) . . . . ? P2 Ru C7A C1 -162.5(2) . . . . ? C3A Ru C7A C1 -118.5(4) . . . . ? C21 P1 C11 C12 72.0(4) . . . . ? Ru P1 C11 C12 -123.1(3) . . . . ? C21 P1 C11 C16 -55.7(4) . . . . ? Ru P1 C11 C16 109.2(3) . . . . ? C16 C11 C12 C13 -56.2(6) . . . . ? P1 C11 C12 C13 174.2(4) . . . . ? C11 C12 C13 C14 55.2(6) . . . . ? C12 C13 C14 C15 -54.2(7) . . . . ? C13 C14 C15 C16 55.4(7) . . . . ? C14 C15 C16 C11 -56.6(6) . . . . ? C12 C11 C16 C15 56.7(5) . . . . ? P1 C11 C16 C15 -173.7(4) . . . . ? C11 P1 C21 C26 108.2(4) . . . . ? Ru P1 C21 C26 -57.5(4) . . . . ? C11 P1 C21 C22 -127.7(4) . . . . ? Ru P1 C21 C22 66.6(4) . . . . ? C26 C21 C22 C23 -51.9(6) . . . . ? P1 C21 C22 C23 -176.4(4) . . . . ? C21 C22 C23 C24 55.7(6) . . . . ? C22 C23 C24 C25 -56.8(7) . . . . ? C23 C24 C25 C26 55.4(7) . . . . ? C24 C25 C26 C21 -53.7(7) . . . . ? C22 C21 C26 C25 51.3(6) . . . . ? P1 C21 C26 C25 175.0(4) . . . . ? C41 P2 C31 C36 -5.6(5) . . . . ? C51 P2 C31 C36 98.2(4) . . . . ? Ru P2 C31 C36 -137.7(4) . . . . ? C41 P2 C31 C32 169.3(4) . . . . ? C51 P2 C31 C32 -87.0(4) . . . . ? Ru P2 C31 C32 37.2(4) . . . . ? C36 C31 C32 C33 -1.8(7) . . . . ? P2 C31 C32 C33 -177.1(4) . . . . ? C31 C32 C33 C34 2.0(8) . . . . ? C32 C33 C34 C35 -0.9(8) . . . . ? C33 C34 C35 C36 -0.4(8) . . . . ? C32 C31 C36 C35 0.5(7) . . . . ? P2 C31 C36 C35 175.4(4) . . . . ? C34 C35 C36 C31 0.6(8) . . . . ? C31 P2 C41 C42 -118.9(4) . . . . ? C51 P2 C41 C42 135.0(4) . . . . ? Ru P2 C41 C42 10.6(4) . . . . ? C31 P2 C41 C46 63.4(4) . . . . ? C51 P2 C41 C46 -42.7(4) . . . . ? Ru P2 C41 C46 -167.1(3) . . . . ? C46 C41 C42 C43 -2.8(7) . . . . ? P2 C41 C42 C43 179.4(4) . . . . ? C41 C42 C43 C44 1.7(8) . . . . ? C42 C43 C44 C45 0.3(8) . . . . ? C43 C44 C45 C46 -1.1(8) . . . . ? C44 C45 C46 C41 -0.2(8) . . . . ? C42 C41 C46 C45 2.1(7) . . . . ? P2 C41 C46 C45 179.8(4) . . . . ? C41 P2 C51 C52 -43.9(4) . . . . ? C31 P2 C51 C52 -150.9(4) . . . . ? Ru P2 C51 C52 84.3(4) . . . . ? C41 P2 C51 C56 142.9(4) . . . . ? C31 P2 C51 C56 35.8(4) . . . . ? Ru P2 C51 C56 -88.9(4) . . . . ? C56 C51 C52 C53 0.9(7) . . . . ? P2 C51 C52 C53 -172.6(4) . . . . ? C51 C52 C53 C54 0.2(8) . . . . ? C52 C53 C54 C55 -1.3(8) . . . . ? C53 C54 C55 C56 1.2(8) . . . . ? C54 C55 C56 C51 -0.1(7) . . . . ? C52 C51 C56 C55 -1.0(7) . . . . ? P2 C51 C56 C55 172.5(4) . . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 26.42 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.929 _refine_diff_density_min -1.062 _refine_diff_density_rms 0.130 #===END data_3a _audit_creation_method 'manual editing of SHELXL template' _publ_contact_author_name 'Dr. Lisa Rosenberg' _publ_contact_author_address ; Department of Chemistry University of Victoria P.O. Box 3065 Victoria, BC V8W 3V6 Canada ; _publ_contact_author_email lisarose@uvic.ca _publ_contact_author_fax '1(250)7217147' _publ_contact_author_phone '1(250)7217173' _publ_contact_letter ; To: Cambridge Crystallographic Data Centre Please accept the following CIF data in support of a manuscript being submitted to the Journal of the American Chemical Society. Please forward any questions concerning this CIF to Bob McDonald (Bob.McDonald@ualberta.ca). ; _publ_requested_journal 'Journal of the American Chemical Society' _publ_section_title ; A highly reactive ruthenium phosphido complex exhibiting Ru-P \p-bonding ; loop_ _publ_author_name _publ_author_footnote _publ_author_address 'Derrah, Eric J.' . ; Department of Chemistry University of Victoria P.O. Box 3065 Victoria, BC V8W 3V6 Canada ; 'McDonald, Robert' 'X-ray Crystallography Laboratory' ; Department of Chemistry University of Alberta Edmonton, AB T6G 2G2 Canada ; 'Pantazis, Dimitrios A.' . ; Department of Chemistry University of Glasgow Glasgow G12 8QQ United Kingdom ; 'Rosenberg, Lisa' . ; Department of Chemistry University of Victoria P.O. Box 3065 Victoria, BC V8W 3V6 Canada ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C40 H44 O P2 Ru' _chemical_formula_sum 'C40 H44 O P2 Ru' _chemical_formula_weight 703.76 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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.8311(12) _cell_length_b 12.3025(15) _cell_length_c 15.6685(19) _cell_angle_alpha 97.7025(17) _cell_angle_beta 101.4607(17) _cell_angle_gamma 110.8896(16) _cell_volume 1691.2(4) _cell_formula_units_Z 2 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 6144 _cell_measurement_theta_min 2.30 _cell_measurement_theta_max 26.39 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.382 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 732 _exptl_absorpt_coefficient_mu 0.589 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.7377 _exptl_absorpt_correction_T_max 0.9489 _exptl_absorpt_process_details 'Bruker SHELXTL (Bruker, 1997)' _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 13520 _diffrn_reflns_av_R_equivalents 0.0231 _diffrn_reflns_av_sigmaI/netI 0.0342 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.36 _diffrn_reflns_theta_max 26.42 _reflns_number_total 6929 _reflns_number_gt 6285 _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^)+(0.0235P)^2^+1.6166P] 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 6929 _refine_ls_number_parameters 397 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0345 _refine_ls_R_factor_gt 0.0298 _refine_ls_wR_factor_ref 0.0772 _refine_ls_wR_factor_gt 0.0752 _refine_ls_goodness_of_fit_ref 1.137 _refine_ls_restrained_S_all 1.137 _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 -0.02132(2) 0.196298(16) 0.202321(12) 0.01879(6) Uani 1 1 d . . . P1 P -0.04326(7) 0.01231(5) 0.25148(4) 0.01996(13) Uani 1 1 d . . . P2 P 0.17690(7) 0.30739(5) 0.32720(4) 0.01899(13) Uani 1 1 d . . . O O -0.2483(2) 0.18775(19) 0.30649(14) 0.0423(5) Uani 1 1 d . . . C1 C 0.0859(3) 0.2007(2) 0.08580(16) 0.0302(6) Uani 1 1 d . . . H1 H 0.1796 0.1864 0.0847 0.036 Uiso 1 1 calc R . . C2 C -0.0632(3) 0.1127(2) 0.05913(16) 0.0329(6) Uani 1 1 d . . . H2 H -0.0922 0.0258 0.0346 0.039 Uiso 1 1 calc R . . C3 C -0.1656(3) 0.1681(2) 0.06463(16) 0.0323(6) Uani 1 1 d . . . H3 H -0.2782 0.1272 0.0446 0.039 Uiso 1 1 calc R . . C3A C -0.0801(3) 0.2955(2) 0.08669(16) 0.0283(5) Uani 1 1 d . . . C4 C -0.1236(3) 0.3941(3) 0.09279(17) 0.0341(6) Uani 1 1 d . . . H4 H -0.2265 0.3822 0.0856 0.041 Uiso 1 1 calc R . . C5 C -0.0143(4) 0.5063(3) 0.10927(18) 0.0382(7) Uani 1 1 d . . . H5 H -0.0424 0.5727 0.1118 0.046 Uiso 1 1 calc R . . C6 C 0.1395(4) 0.5258(3) 0.12260(18) 0.0373(7) Uani 1 1 d . . . H6 H 0.2124 0.6052 0.1340 0.045 Uiso 1 1 calc R . . C7 C 0.1865(3) 0.4337(2) 0.11961(16) 0.0311(6) Uani 1 1 d . . . H7 H 0.2908 0.4485 0.1303 0.037 Uiso 1 1 calc R . . C7A C 0.0759(3) 0.3154(2) 0.10010(16) 0.0275(5) Uani 1 1 d . . . C10 C -0.1591(3) 0.1934(2) 0.26760(16) 0.0253(5) Uani 1 1 d . . . C11 C -0.1752(3) -0.1157(2) 0.15607(16) 0.0229(5) Uani 1 1 d . . . H11 H -0.1335 -0.1094 0.1028 0.027 Uiso 1 1 calc R . . C12 C -0.3311(3) -0.1098(2) 0.13241(19) 0.0310(6) Uani 1 1 d . . . H12A H -0.3707 -0.1118 0.1858 0.037 Uiso 1 1 calc R . . H12B H -0.3206 -0.0332 0.1153 0.037 Uiso 1 1 calc R . . C13 C -0.4441(3) -0.2126(3) 0.0560(2) 0.0435(7) Uani 1 1 d . . . H13A H -0.5441 -0.2077 0.0457 0.052 Uiso 1 1 calc R . . H13B H -0.4109 -0.2055 0.0006 0.052 Uiso 1 1 calc R . . C14 C -0.4580(3) -0.3328(3) 0.0766(2) 0.0467(8) Uani 1 1 d . . . H14A H -0.5049 -0.3450 0.1267 0.056 Uiso 1 1 calc R . . H14B H -0.5244 -0.3972 0.0237 0.056 Uiso 1 1 calc R . . C15 C -0.3046(3) -0.3399(2) 0.10104(19) 0.0350(6) Uani 1 1 d . . . H15A H -0.2630 -0.3373 0.0484 0.042 Uiso 1 1 calc R . . H15B H -0.3163 -0.4168 0.1179 0.042 Uiso 1 1 calc R . . C16 C -0.1934(3) -0.2368(2) 0.17900(17) 0.0298(6) Uani 1 1 d . . . H16A H -0.2309 -0.2427 0.2331 0.036 Uiso 1 1 calc R . . H16B H -0.0939 -0.2428 0.1921 0.036 Uiso 1 1 calc R . . C21 C 0.1428(3) -0.0038(2) 0.26058(15) 0.0224(5) Uani 1 1 d . . . H21 H 0.2215 0.0792 0.2843 0.027 Uiso 1 1 calc R . . C22 C 0.1758(3) -0.0497(3) 0.17465(17) 0.0304(6) Uani 1 1 d . . . H22A H 0.1681 0.0024 0.1326 0.037 Uiso 1 1 calc R . . H22B H 0.0991 -0.1312 0.1462 0.037 Uiso 1 1 calc R . . C23 C 0.3338(3) -0.0524(3) 0.1928(2) 0.0446(8) Uani 1 1 d . . . H23A H 0.3479 -0.0888 0.1367 0.054 Uiso 1 1 calc R . . H23B H 0.4112 0.0303 0.2137 0.054 Uiso 1 1 calc R . . C24 C 0.3548(4) -0.1234(3) 0.2629(2) 0.0532(9) Uani 1 1 d . . . H24A H 0.4585 -0.1215 0.2749 0.064 Uiso 1 1 calc R . . H24B H 0.2829 -0.2077 0.2399 0.064 Uiso 1 1 calc R . . C25 C 0.3288(4) -0.0725(3) 0.3492(2) 0.0425(7) Uani 1 1 d . . . H25A H 0.4052 0.0099 0.3743 0.051 Uiso 1 1 calc R . . H25B H 0.3410 -0.1212 0.3933 0.051 Uiso 1 1 calc R . . C26 C 0.1712(3) -0.0717(2) 0.33279(17) 0.0296(6) Uani 1 1 d . . . H26A H 0.1593 -0.0339 0.3891 0.036 Uiso 1 1 calc R . . H26B H 0.0951 -0.1549 0.3141 0.036 Uiso 1 1 calc R . . C31 C 0.3591(3) 0.3727(2) 0.30057(15) 0.0231(5) Uani 1 1 d . . . C32 C 0.4073(3) 0.2984(2) 0.24982(17) 0.0287(5) Uani 1 1 d . . . H32 H 0.3445 0.2160 0.2287 0.034 Uiso 1 1 calc R . . C33 C 0.5448(3) 0.3432(3) 0.22998(19) 0.0357(6) Uani 1 1 d . . . H33 H 0.5764 0.2912 0.1962 0.043 Uiso 1 1 calc R . . C34 C 0.6360(3) 0.4626(3) 0.2588(2) 0.0410(7) Uani 1 1 d . . . H34 H 0.7301 0.4934 0.2447 0.049 Uiso 1 1 calc R . . C35 C 0.5896(3) 0.5379(3) 0.30864(19) 0.0408(7) Uani 1 1 d . . . H35 H 0.6524 0.6205 0.3289 0.049 Uiso 1 1 calc R . . C36 C 0.4518(3) 0.4931(2) 0.32912(17) 0.0308(6) Uani 1 1 d . . . H36 H 0.4207 0.5455 0.3630 0.037 Uiso 1 1 calc R . . C41 C 0.1564(3) 0.4391(2) 0.38380(16) 0.0226(5) Uani 1 1 d . . . C42 C 0.0747(3) 0.4919(2) 0.33415(18) 0.0301(6) Uani 1 1 d . . . H42 H 0.0241 0.4561 0.2729 0.036 Uiso 1 1 calc R . . C43 C 0.0666(3) 0.5963(3) 0.3735(2) 0.0385(7) Uani 1 1 d . . . H43 H 0.0123 0.6328 0.3388 0.046 Uiso 1 1 calc R . . C44 C 0.1372(3) 0.6476(2) 0.4630(2) 0.0379(7) Uani 1 1 d . . . H44 H 0.1317 0.7194 0.4898 0.045 Uiso 1 1 calc R . . C45 C 0.2151(3) 0.5948(2) 0.51306(18) 0.0348(6) Uani 1 1 d . . . H45 H 0.2617 0.6292 0.5749 0.042 Uiso 1 1 calc R . . C46 C 0.2262(3) 0.4916(2) 0.47388(17) 0.0297(6) Uani 1 1 d . . . H46 H 0.2820 0.4564 0.5088 0.036 Uiso 1 1 calc R . . C51 C 0.2245(3) 0.2431(2) 0.42216(15) 0.0212(5) Uani 1 1 d . . . C52 C 0.1112(3) 0.1878(2) 0.46200(16) 0.0262(5) Uani 1 1 d . . . H52 H 0.0113 0.1819 0.4384 0.031 Uiso 1 1 calc R . . C53 C 0.1432(3) 0.1413(2) 0.53575(17) 0.0331(6) Uani 1 1 d . . . H53 H 0.0656 0.1055 0.5632 0.040 Uiso 1 1 calc R . . C54 C 0.2863(4) 0.1468(3) 0.56954(18) 0.0384(7) Uani 1 1 d . . . H54 H 0.3069 0.1130 0.6192 0.046 Uiso 1 1 calc R . . C55 C 0.4002(3) 0.2016(3) 0.53086(18) 0.0368(6) Uani 1 1 d . . . H55 H 0.4994 0.2061 0.5544 0.044 Uiso 1 1 calc R . . C56 C 0.3697(3) 0.2501(2) 0.45758(17) 0.0285(5) Uani 1 1 d . . . H56 H 0.4485 0.2881 0.4316 0.034 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 0.01980(10) 0.01950(10) 0.01577(10) 0.00173(7) 0.00148(7) 0.00879(8) P1 0.0200(3) 0.0197(3) 0.0202(3) 0.0023(2) 0.0044(2) 0.0091(2) P2 0.0194(3) 0.0195(3) 0.0171(3) 0.0027(2) 0.0024(2) 0.0083(2) O 0.0346(11) 0.0522(13) 0.0473(12) 0.0072(10) 0.0186(10) 0.0226(10) C1 0.0419(15) 0.0326(14) 0.0201(12) 0.0060(10) 0.0109(11) 0.0180(12) C2 0.0501(17) 0.0292(14) 0.0157(11) 0.0025(10) 0.0051(11) 0.0141(13) C3 0.0340(14) 0.0340(14) 0.0189(12) 0.0047(10) -0.0045(10) 0.0084(12) C3A 0.0338(14) 0.0328(14) 0.0155(11) 0.0070(10) 0.0009(10) 0.0123(11) C4 0.0378(15) 0.0431(16) 0.0256(13) 0.0114(12) 0.0032(11) 0.0222(13) C5 0.0587(19) 0.0343(15) 0.0302(14) 0.0136(12) 0.0102(13) 0.0267(15) C6 0.0479(18) 0.0284(14) 0.0284(14) 0.0079(11) 0.0073(12) 0.0077(13) C7 0.0347(14) 0.0340(14) 0.0222(12) 0.0097(11) 0.0071(11) 0.0096(12) C7A 0.0344(14) 0.0327(14) 0.0169(11) 0.0072(10) 0.0069(10) 0.0143(12) C10 0.0228(12) 0.0251(13) 0.0264(12) 0.0005(10) 0.0006(10) 0.0127(10) C11 0.0204(12) 0.0206(12) 0.0247(12) 0.0015(9) 0.0042(9) 0.0069(10) C12 0.0210(12) 0.0260(13) 0.0420(15) 0.0012(11) 0.0040(11) 0.0093(11) C13 0.0245(14) 0.0399(17) 0.0529(19) -0.0039(14) -0.0068(13) 0.0116(13) C14 0.0299(15) 0.0295(15) 0.061(2) -0.0051(14) -0.0006(14) 0.0016(12) C15 0.0365(15) 0.0208(13) 0.0396(15) 0.0009(11) 0.0040(12) 0.0073(12) C16 0.0349(14) 0.0217(12) 0.0316(14) 0.0055(10) 0.0079(11) 0.0104(11) C21 0.0206(11) 0.0234(12) 0.0231(12) 0.0027(9) 0.0036(9) 0.0107(10) C22 0.0294(14) 0.0392(15) 0.0254(13) 0.0035(11) 0.0062(11) 0.0187(12) C23 0.0378(17) 0.068(2) 0.0367(16) 0.0023(15) 0.0112(13) 0.0341(16) C24 0.055(2) 0.075(2) 0.0494(19) 0.0077(17) 0.0103(16) 0.052(2) C25 0.0431(17) 0.059(2) 0.0374(16) 0.0135(14) 0.0052(13) 0.0355(16) C26 0.0326(14) 0.0316(14) 0.0284(13) 0.0078(11) 0.0055(11) 0.0179(12) C31 0.0198(12) 0.0270(12) 0.0205(11) 0.0077(10) 0.0025(9) 0.0079(10) C32 0.0286(13) 0.0290(13) 0.0302(13) 0.0085(11) 0.0094(11) 0.0118(11) C33 0.0326(15) 0.0487(17) 0.0347(15) 0.0152(13) 0.0137(12) 0.0218(13) C34 0.0237(14) 0.057(2) 0.0382(16) 0.0184(14) 0.0113(12) 0.0068(13) C35 0.0328(15) 0.0382(16) 0.0350(15) 0.0061(13) 0.0061(12) -0.0025(13) C36 0.0306(14) 0.0309(14) 0.0246(12) 0.0041(11) 0.0052(11) 0.0069(11) C41 0.0217(12) 0.0197(12) 0.0249(12) 0.0015(9) 0.0063(10) 0.0076(10) C42 0.0340(14) 0.0264(13) 0.0280(13) 0.0037(11) 0.0028(11) 0.0134(11) C43 0.0434(17) 0.0300(15) 0.0454(17) 0.0074(13) 0.0067(13) 0.0213(13) C44 0.0382(16) 0.0266(14) 0.0459(17) -0.0047(12) 0.0129(13) 0.0131(12) C45 0.0375(15) 0.0327(15) 0.0270(13) -0.0054(11) 0.0068(12) 0.0108(12) C46 0.0314(14) 0.0293(13) 0.0255(13) 0.0009(10) 0.0033(11) 0.0128(11) C51 0.0243(12) 0.0205(11) 0.0176(11) 0.0013(9) 0.0018(9) 0.0104(10) C52 0.0260(13) 0.0281(13) 0.0214(12) 0.0019(10) 0.0039(10) 0.0097(11) C53 0.0449(16) 0.0289(14) 0.0230(13) 0.0055(11) 0.0121(12) 0.0100(12) C54 0.0559(19) 0.0354(15) 0.0235(13) 0.0098(11) 0.0031(13) 0.0203(14) C55 0.0381(16) 0.0439(17) 0.0302(14) 0.0080(12) -0.0010(12) 0.0238(14) C56 0.0260(13) 0.0315(14) 0.0267(13) 0.0058(11) 0.0038(10) 0.0120(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 C10 1.846(2) . ? Ru C2 2.230(2) . ? Ru C3 2.240(2) . ? Ru C1 2.280(2) . ? Ru P2 2.3158(6) . ? Ru C3A 2.406(2) . ? Ru C7A 2.422(2) . ? Ru P1 2.4390(7) . ? P1 C11 1.881(2) . ? P1 C21 1.889(2) . ? P2 C51 1.833(2) . ? P2 C41 1.836(2) . ? P2 C31 1.841(2) . ? O C10 1.151(3) . ? C1 C2 1.414(4) . ? C1 C7A 1.440(4) . ? C2 C3 1.412(4) . ? C3 C3A 1.443(4) . ? C3A C4 1.420(4) . ? C3A C7A 1.431(4) . ? C4 C5 1.365(4) . ? C5 C6 1.410(4) . ? C6 C7 1.367(4) . ? C7 C7A 1.419(4) . ? C11 C12 1.534(3) . ? C11 C16 1.535(3) . ? C12 C13 1.527(4) . ? C13 C14 1.520(4) . ? C14 C15 1.517(4) . ? C15 C16 1.537(4) . ? C21 C22 1.529(3) . ? C21 C26 1.533(3) . ? C22 C23 1.536(4) . ? C23 C24 1.519(5) . ? C24 C25 1.520(4) . ? C25 C26 1.524(4) . ? C31 C36 1.387(4) . ? C31 C32 1.398(3) . ? C32 C33 1.382(4) . ? C33 C34 1.374(4) . ? C34 C35 1.387(4) . ? C35 C36 1.389(4) . ? C41 C42 1.389(3) . ? C41 C46 1.391(3) . ? C42 C43 1.384(4) . ? C43 C44 1.383(4) . ? C44 C45 1.370(4) . ? C45 C46 1.385(4) . ? C51 C56 1.393(3) . ? C51 C52 1.394(3) . ? C52 C53 1.386(4) . ? C53 C54 1.376(4) . ? C54 C55 1.385(4) . ? C55 C56 1.392(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 C10 Ru C2 129.03(11) . . ? C10 Ru C3 99.95(11) . . ? C2 Ru C3 36.83(10) . . ? C10 Ru C1 161.01(10) . . ? C2 Ru C1 36.52(10) . . ? C3 Ru C1 61.33(10) . . ? C10 Ru P2 90.66(8) . . ? C2 Ru P2 140.29(8) . . ? C3 Ru P2 153.78(7) . . ? C1 Ru P2 105.13(7) . . ? C10 Ru C3A 104.05(10) . . ? C2 Ru C3A 59.47(9) . . ? C3 Ru C3A 35.97(9) . . ? C1 Ru C3A 59.33(9) . . ? P2 Ru C3A 118.19(6) . . ? C10 Ru C7A 133.90(10) . . ? C2 Ru C7A 59.11(9) . . ? C3 Ru C7A 59.44(9) . . ? C1 Ru C7A 35.52(9) . . ? P2 Ru C7A 96.09(6) . . ? C3A Ru C7A 34.49(9) . . ? C10 Ru P1 81.95(8) . . ? C2 Ru P1 93.47(7) . . ? C3 Ru P1 114.16(7) . . ? C1 Ru P1 107.79(7) . . ? P2 Ru P1 90.92(2) . . ? C3A Ru P1 149.82(6) . . ? C7A Ru P1 143.11(6) . . ? C11 P1 C21 102.47(10) . . ? C11 P1 Ru 107.36(8) . . ? C21 P1 Ru 107.88(8) . . ? C51 P2 C41 100.88(11) . . ? C51 P2 C31 102.71(11) . . ? C41 P2 C31 102.71(11) . . ? C51 P2 Ru 121.85(8) . . ? C41 P2 Ru 113.23(8) . . ? C31 P2 Ru 113.09(8) . . ? C2 C1 C7A 107.4(2) . . ? C2 C1 Ru 69.82(14) . . ? C7A C1 Ru 77.61(14) . . ? C3 C2 C1 109.3(2) . . ? C3 C2 Ru 71.97(14) . . ? C1 C2 Ru 73.65(14) . . ? C2 C3 C3A 107.6(2) . . ? C2 C3 Ru 71.20(14) . . ? C3A C3 Ru 78.26(14) . . ? C4 C3A C7A 119.9(2) . . ? C4 C3A C3 132.6(3) . . ? C7A C3A C3 107.4(2) . . ? C4 C3A Ru 128.48(18) . . ? C7A C3A Ru 73.37(14) . . ? C3 C3A Ru 65.76(13) . . ? C5 C4 C3A 118.5(3) . . ? C4 C5 C6 121.5(3) . . ? C7 C6 C5 121.8(3) . . ? C6 C7 C7A 118.5(3) . . ? C7 C7A C3A 119.7(2) . . ? C7 C7A C1 132.3(3) . . ? C3A C7A C1 107.9(2) . . ? C7 C7A Ru 128.91(17) . . ? C3A C7A Ru 72.14(14) . . ? C1 C7A Ru 66.87(13) . . ? O C10 Ru 177.6(2) . . ? C12 C11 C16 108.8(2) . . ? C12 C11 P1 109.99(16) . . ? C16 C11 P1 111.70(17) . . ? C13 C12 C11 112.4(2) . . ? C14 C13 C12 111.3(3) . . ? C15 C14 C13 111.1(2) . . ? C14 C15 C16 111.6(2) . . ? C11 C16 C15 110.8(2) . . ? C22 C21 C26 111.8(2) . . ? C22 C21 P1 118.09(17) . . ? C26 C21 P1 110.82(16) . . ? C21 C22 C23 111.7(2) . . ? C24 C23 C22 111.0(3) . . ? C23 C24 C25 110.9(3) . . ? C24 C25 C26 110.9(2) . . ? C25 C26 C21 111.6(2) . . ? C36 C31 C32 118.2(2) . . ? C36 C31 P2 122.69(19) . . ? C32 C31 P2 119.08(19) . . ? C33 C32 C31 121.0(3) . . ? C34 C33 C32 120.3(3) . . ? C33 C34 C35 119.5(3) . . ? C34 C35 C36 120.3(3) . . ? C31 C36 C35 120.6(3) . . ? C42 C41 C46 118.7(2) . . ? C42 C41 P2 118.99(18) . . ? C46 C41 P2 122.21(19) . . ? C43 C42 C41 120.3(2) . . ? C44 C43 C42 120.3(3) . . ? C45 C44 C43 119.9(3) . . ? C44 C45 C46 120.3(3) . . ? C45 C46 C41 120.6(2) . . ? C56 C51 C52 118.7(2) . . ? C56 C51 P2 122.77(19) . . ? C52 C51 P2 118.49(18) . . ? C53 C52 C51 120.4(2) . . ? C54 C53 C52 120.6(3) . . ? C53 C54 C55 119.7(3) . . ? C54 C55 C56 120.2(3) . . ? C55 C56 C51 120.4(2) . . ? 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 Ru P1 C11 99.97(11) . . . . ? C2 Ru P1 C11 -28.97(11) . . . . ? C3 Ru P1 C11 2.63(11) . . . . ? C1 Ru P1 C11 -63.28(11) . . . . ? P2 Ru P1 C11 -169.49(8) . . . . ? C3A Ru P1 C11 -4.19(16) . . . . ? C7A Ru P1 C11 -68.07(13) . . . . ? C10 Ru P1 C21 -150.24(11) . . . . ? C2 Ru P1 C21 80.82(11) . . . . ? C3 Ru P1 C21 112.42(11) . . . . ? C1 Ru P1 C21 46.52(11) . . . . ? P2 Ru P1 C21 -59.70(8) . . . . ? C3A Ru P1 C21 105.60(15) . . . . ? C7A Ru P1 C21 41.72(13) . . . . ? C10 Ru P2 C51 70.01(12) . . . . ? C2 Ru P2 C51 -108.51(14) . . . . ? C3 Ru P2 C51 -175.51(19) . . . . ? C1 Ru P2 C51 -120.67(11) . . . . ? C3A Ru P2 C51 176.37(11) . . . . ? C7A Ru P2 C51 -155.68(11) . . . . ? P1 Ru P2 C51 -11.95(9) . . . . ? C10 Ru P2 C41 -50.56(11) . . . . ? C2 Ru P2 C41 130.93(14) . . . . ? C3 Ru P2 C41 63.93(19) . . . . ? C1 Ru P2 C41 118.76(11) . . . . ? C3A Ru P2 C41 55.81(11) . . . . ? C7A Ru P2 C41 83.76(10) . . . . ? P1 Ru P2 C41 -132.52(9) . . . . ? C10 Ru P2 C31 -166.87(12) . . . . ? C2 Ru P2 C31 14.62(14) . . . . ? C3 Ru P2 C31 -52.39(19) . . . . ? C1 Ru P2 C31 2.45(11) . . . . ? C3A Ru P2 C31 -60.51(11) . . . . ? C7A Ru P2 C31 -32.55(11) . . . . ? P1 Ru P2 C31 111.17(9) . . . . ? C10 Ru C1 C2 -47.8(4) . . . . ? C3 Ru C1 C2 -37.39(16) . . . . ? P2 Ru C1 C2 166.93(14) . . . . ? C3A Ru C1 C2 -78.96(17) . . . . ? C7A Ru C1 C2 -114.0(2) . . . . ? P1 Ru C1 C2 70.94(16) . . . . ? C10 Ru C1 C7A 66.2(4) . . . . ? C2 Ru C1 C7A 114.0(2) . . . . ? C3 Ru C1 C7A 76.62(16) . . . . ? P2 Ru C1 C7A -79.07(15) . . . . ? C3A Ru C1 C7A 35.05(14) . . . . ? P1 Ru C1 C7A -175.05(13) . . . . ? C7A C1 C2 C3 -5.6(3) . . . . ? Ru C1 C2 C3 63.60(18) . . . . ? C7A C1 C2 Ru -69.23(17) . . . . ? C10 Ru C2 C3 44.6(2) . . . . ? C1 Ru C2 C3 -117.3(2) . . . . ? P2 Ru C2 C3 -137.27(14) . . . . ? C3A Ru C2 C3 -38.74(16) . . . . ? C7A Ru C2 C3 -79.08(17) . . . . ? P1 Ru C2 C3 127.10(15) . . . . ? C10 Ru C2 C1 161.92(16) . . . . ? C3 Ru C2 C1 117.3(2) . . . . ? P2 Ru C2 C1 -20.0(2) . . . . ? C3A Ru C2 C1 78.53(17) . . . . ? C7A Ru C2 C1 38.20(15) . . . . ? P1 Ru C2 C1 -115.63(15) . . . . ? C1 C2 C3 C3A 5.9(3) . . . . ? Ru C2 C3 C3A 70.52(17) . . . . ? C1 C2 C3 Ru -64.67(18) . . . . ? C10 Ru C3 C2 -146.34(17) . . . . ? C1 Ru C3 C2 37.08(16) . . . . ? P2 Ru C3 C2 101.2(2) . . . . ? C3A Ru C3 C2 113.4(2) . . . . ? C7A Ru C3 C2 78.10(17) . . . . ? P1 Ru C3 C2 -60.76(17) . . . . ? C10 Ru C3 C3A 100.26(17) . . . . ? C2 Ru C3 C3A -113.4(2) . . . . ? C1 Ru C3 C3A -76.33(17) . . . . ? P2 Ru C3 C3A -12.2(3) . . . . ? C7A Ru C3 C3A -35.30(15) . . . . ? P1 Ru C3 C3A -174.17(13) . . . . ? C2 C3 C3A C4 173.4(3) . . . . ? Ru C3 C3A C4 -120.9(3) . . . . ? C2 C3 C3A C7A -3.8(3) . . . . ? Ru C3 C3A C7A 61.96(17) . . . . ? C2 C3 C3A Ru -65.71(17) . . . . ? C10 Ru C3A C4 38.6(3) . . . . ? C2 Ru C3A C4 165.9(3) . . . . ? C3 Ru C3A C4 126.2(3) . . . . ? C1 Ru C3A C4 -151.4(3) . . . . ? P2 Ru C3A C4 -59.9(3) . . . . ? C7A Ru C3A C4 -115.3(3) . . . . ? P1 Ru C3A C4 136.8(2) . . . . ? C10 Ru C3A C7A 153.90(15) . . . . ? C2 Ru C3A C7A -78.80(17) . . . . ? C3 Ru C3A C7A -118.5(2) . . . . ? C1 Ru C3A C7A -36.10(15) . . . . ? P2 Ru C3A C7A 55.41(16) . . . . ? P1 Ru C3A C7A -107.86(16) . . . . ? C10 Ru C3A C3 -87.61(17) . . . . ? C2 Ru C3A C3 39.69(17) . . . . ? C1 Ru C3A C3 82.39(17) . . . . ? P2 Ru C3A C3 173.90(14) . . . . ? C7A Ru C3A C3 118.5(2) . . . . ? P1 Ru C3A C3 10.6(2) . . . . ? C7A C3A C4 C5 1.6(4) . . . . ? C3 C3A C4 C5 -175.2(3) . . . . ? Ru C3A C4 C5 93.7(3) . . . . ? C3A C4 C5 C6 -1.8(4) . . . . ? C4 C5 C6 C7 0.1(4) . . . . ? C5 C6 C7 C7A 1.7(4) . . . . ? C6 C7 C7A C3A -1.8(4) . . . . ? C6 C7 C7A C1 174.9(3) . . . . ? C6 C7 C7A Ru -92.2(3) . . . . ? C4 C3A C7A C7 0.1(3) . . . . ? C3 C3A C7A C7 177.7(2) . . . . ? Ru C3A C7A C7 -125.2(2) . . . . ? C4 C3A C7A C1 -177.3(2) . . . . ? C3 C3A C7A C1 0.3(3) . . . . ? Ru C3A C7A C1 57.47(16) . . . . ? C4 C3A C7A Ru 125.3(2) . . . . ? C3 C3A C7A Ru -57.13(16) . . . . ? C2 C1 C7A C7 -173.7(3) . . . . ? Ru C1 C7A C7 122.3(3) . . . . ? C2 C1 C7A C3A 3.2(3) . . . . ? Ru C1 C7A C3A -60.76(17) . . . . ? C2 C1 C7A Ru 63.97(17) . . . . ? C10 Ru C7A C7 77.9(3) . . . . ? C2 Ru C7A C7 -165.9(3) . . . . ? C3 Ru C7A C7 151.0(3) . . . . ? C1 Ru C7A C7 -126.6(3) . . . . ? P2 Ru C7A C7 -19.0(2) . . . . ? C3A Ru C7A C7 114.2(3) . . . . ? P1 Ru C7A C7 -118.7(2) . . . . ? C10 Ru C7A C3A -36.3(2) . . . . ? C2 Ru C7A C3A 79.95(17) . . . . ? C3 Ru C7A C3A 36.84(15) . . . . ? C1 Ru C7A C3A 119.3(2) . . . . ? P2 Ru C7A C3A -133.14(14) . . . . ? P1 Ru C7A C3A 127.13(14) . . . . ? C10 Ru C7A C1 -155.58(16) . . . . ? C2 Ru C7A C1 -39.31(16) . . . . ? C3 Ru C7A C1 -82.43(17) . . . . ? P2 Ru C7A C1 107.60(15) . . . . ? C3A Ru C7A C1 -119.3(2) . . . . ? P1 Ru C7A C1 7.9(2) . . . . ? C2 Ru C10 O 31(6) . . . . ? C3 Ru C10 O 56(6) . . . . ? C1 Ru C10 O 65(6) . . . . ? P2 Ru C10 O -148(6) . . . . ? C3A Ru C10 O 92(6) . . . . ? C7A Ru C10 O 113(6) . . . . ? P1 Ru C10 O -57(6) . . . . ? C21 P1 C11 C12 -174.37(18) . . . . ? Ru P1 C11 C12 -60.87(18) . . . . ? C21 P1 C11 C16 64.75(19) . . . . ? Ru P1 C11 C16 178.25(15) . . . . ? C16 C11 C12 C13 -56.6(3) . . . . ? P1 C11 C12 C13 -179.3(2) . . . . ? C11 C12 C13 C14 55.6(3) . . . . ? C12 C13 C14 C15 -53.8(4) . . . . ? C13 C14 C15 C16 55.3(4) . . . . ? C12 C11 C16 C15 57.0(3) . . . . ? P1 C11 C16 C15 178.59(18) . . . . ? C14 C15 C16 C11 -57.6(3) . . . . ? C11 P1 C21 C22 34.3(2) . . . . ? Ru P1 C21 C22 -78.8(2) . . . . ? C11 P1 C21 C26 -96.54(18) . . . . ? Ru P1 C21 C26 150.36(15) . . . . ? C26 C21 C22 C23 -52.2(3) . . . . ? P1 C21 C22 C23 177.4(2) . . . . ? C21 C22 C23 C24 54.4(3) . . . . ? C22 C23 C24 C25 -57.2(4) . . . . ? C23 C24 C25 C26 57.9(4) . . . . ? C24 C25 C26 C21 -55.6(3) . . . . ? C22 C21 C26 C25 52.9(3) . . . . ? P1 C21 C26 C25 -173.04(19) . . . . ? C51 P2 C31 C36 -99.0(2) . . . . ? C41 P2 C31 C36 5.4(2) . . . . ? Ru P2 C31 C36 127.79(19) . . . . ? C51 P2 C31 C32 80.7(2) . . . . ? C41 P2 C31 C32 -174.8(2) . . . . ? Ru P2 C31 C32 -52.5(2) . . . . ? C36 C31 C32 C33 1.2(4) . . . . ? P2 C31 C32 C33 -178.5(2) . . . . ? C31 C32 C33 C34 -1.1(4) . . . . ? C32 C33 C34 C35 0.5(4) . . . . ? C33 C34 C35 C36 -0.2(4) . . . . ? C32 C31 C36 C35 -0.9(4) . . . . ? P2 C31 C36 C35 178.9(2) . . . . ? C34 C35 C36 C31 0.4(4) . . . . ? C51 P2 C41 C42 -159.6(2) . . . . ? C31 P2 C41 C42 94.6(2) . . . . ? Ru P2 C41 C42 -27.7(2) . . . . ? C51 P2 C41 C46 23.7(2) . . . . ? C31 P2 C41 C46 -82.1(2) . . . . ? Ru P2 C41 C46 155.57(19) . . . . ? C46 C41 C42 C43 1.6(4) . . . . ? P2 C41 C42 C43 -175.2(2) . . . . ? C41 C42 C43 C44 -1.3(4) . . . . ? C42 C43 C44 C45 -0.2(5) . . . . ? C43 C44 C45 C46 1.4(4) . . . . ? C44 C45 C46 C41 -1.1(4) . . . . ? C42 C41 C46 C45 -0.4(4) . . . . ? P2 C41 C46 C45 176.4(2) . . . . ? C41 P2 C51 C56 -105.8(2) . . . . ? C31 P2 C51 C56 0.1(2) . . . . ? Ru P2 C51 C56 127.90(19) . . . . ? C41 P2 C51 C52 72.4(2) . . . . ? C31 P2 C51 C52 178.28(19) . . . . ? Ru P2 C51 C52 -53.9(2) . . . . ? C56 C51 C52 C53 0.4(4) . . . . ? P2 C51 C52 C53 -177.93(19) . . . . ? C51 C52 C53 C54 -1.4(4) . . . . ? C52 C53 C54 C55 1.5(4) . . . . ? C53 C54 C55 C56 -0.6(4) . . . . ? C54 C55 C56 C51 -0.5(4) . . . . ? C52 C51 C56 C55 0.6(4) . . . . ? P2 C51 C56 C55 178.8(2) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.42 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.501 _refine_diff_density_min -0.299 _refine_diff_density_rms 0.068 #===END data_5a.NH3 _audit_creation_method 'manual editing of SHELXL template' _publ_contact_author_name 'Dr. Lisa Rosenberg' _publ_contact_author_address ; Department of Chemistry University of Victoria P.O. Box 3065 Victoria, BC V8W 3V6 Canada ; _publ_contact_author_email lisarose@uvic.ca _publ_contact_author_fax '1(250)7217147' _publ_contact_author_phone '1(250)7217173' _publ_contact_letter ; To: Cambridge Crystallographic Data Centre Please accept the following CIF data in support of a manuscript being submitted to the Journal of the American Chemical Society. Please forward any questions concerning this CIF to Bob McDonald (Bob.McDonald@ualberta.ca). ; _publ_requested_journal 'Journal of the American Chemical Society' _publ_section_title ; A highly reactive ruthenium phosphido complex exhibiting Ru-P \p-bonding ; loop_ _publ_author_name _publ_author_footnote _publ_author_address 'Derrah, Eric J.' . ; Department of Chemistry University of Victoria P.O. Box 3065 Victoria, BC V8W 3V6 Canada ; 'McDonald, Robert' 'X-ray Crystallography Laboratory' ; Department of Chemistry University of Alberta Edmonton, AB T6G 2G2 Canada ; 'Pantazis, Dimitrios A.' . ; Department of Chemistry University of Glasgow Glasgow G12 8QQ United Kingdom ; 'Rosenberg, Lisa' . ; Department of Chemistry University of Victoria P.O. Box 3065 Victoria, BC V8W 3V6 Canada ; _chemical_formula_moiety 'C39 H48 N P2 Ru, F6 P' _chemical_formula_sum 'C39 H48 F6 N P3 Ru' _chemical_formula_weight 838.76 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ru' 'Ru' -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.1385(4) _cell_length_b 10.8856(5) _cell_length_c 20.1951(8) _cell_angle_alpha 100.9043(7) _cell_angle_beta 92.2008(7) _cell_angle_gamma 107.7646(6) _cell_volume 1868.68(14) _cell_formula_units_Z 2 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 6511 _cell_measurement_theta_min 2.35 _cell_measurement_theta_max 26.38 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.64 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.491 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 864 _exptl_absorpt_coefficient_mu 0.608 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.6971 _exptl_absorpt_correction_T_max 0.9090 _exptl_absorpt_process_details 'Bruker SHELXTL (Bruker, 1997)' _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 14476 _diffrn_reflns_av_R_equivalents 0.0187 _diffrn_reflns_av_sigmaI/netI 0.0277 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.03 _diffrn_reflns_theta_max 26.39 _reflns_number_total 7611 _reflns_number_gt 6961 _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^)+(0.0467P)^2^+0.7394P] 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 7611 _refine_ls_number_parameters 456 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0323 _refine_ls_R_factor_gt 0.0286 _refine_ls_wR_factor_ref 0.0816 _refine_ls_wR_factor_gt 0.0752 _refine_ls_goodness_of_fit_ref 1.091 _refine_ls_restrained_S_all 1.091 _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 0.293348(17) 0.359012(14) 0.212114(7) 0.01966(6) Uani 1 1 d . . . P1 P 0.49186(6) 0.27060(5) 0.18654(3) 0.02165(11) Uani 1 1 d . . . H1P H 0.629(3) 0.353(2) 0.2069(11) 0.024(6) Uiso 1 1 d . . . P2 P 0.37447(6) 0.41088(5) 0.32462(2) 0.02128(11) Uani 1 1 d . . . N N 0.4407(2) 0.55021(17) 0.19720(9) 0.0293(4) Uani 1 1 d . . . H1NA H 0.4065 0.5659 0.1577 0.035 Uiso 1 1 calc R . . H1NB H 0.5397 0.5492 0.1953 0.035 Uiso 1 1 calc R . . H1NC H 0.4373 0.6149 0.2324 0.035 Uiso 1 1 calc R . . C1 C 0.0861(2) 0.1839(2) 0.18968(11) 0.0288(4) Uani 1 1 d . . . H1 H 0.0771 0.0959 0.2002 0.035 Uiso 1 1 calc R . . C2 C 0.0527(2) 0.2902(2) 0.23282(11) 0.0303(5) Uani 1 1 d . . . H2 H 0.0166 0.2884 0.2789 0.036 Uiso 1 1 calc R . . C3 C 0.0678(2) 0.3947(2) 0.19833(11) 0.0292(4) Uani 1 1 d . . . H3 H 0.0460 0.4790 0.2158 0.035 Uiso 1 1 calc R . . C3A C 0.0993(2) 0.3489(2) 0.12998(11) 0.0269(4) Uani 1 1 d . . . C4 C 0.1166(3) 0.4087(2) 0.07300(12) 0.0349(5) Uani 1 1 d . . . H4 H 0.1158 0.4968 0.0769 0.042 Uiso 1 1 calc R . . C5 C 0.1344(3) 0.3374(3) 0.01254(12) 0.0424(6) Uani 1 1 d . . . H5 H 0.1445 0.3762 -0.0261 0.051 Uiso 1 1 calc R . . C6 C 0.1381(3) 0.2071(3) 0.00611(12) 0.0411(6) Uani 1 1 d . . . H6 H 0.1487 0.1597 -0.0370 0.049 Uiso 1 1 calc R . . C7 C 0.1267(2) 0.1469(2) 0.06049(12) 0.0349(5) Uani 1 1 d . . . H7 H 0.1316 0.0597 0.0555 0.042 Uiso 1 1 calc R . . C7A C 0.1072(2) 0.2182(2) 0.12450(11) 0.0273(4) Uani 1 1 d . . . C11 C 0.5205(2) 0.2266(2) 0.09586(10) 0.0258(4) Uani 1 1 d . . . H11 H 0.4289 0.1504 0.0733 0.031 Uiso 1 1 calc R . . C12 C 0.5256(3) 0.3444(2) 0.06341(11) 0.0291(4) Uani 1 1 d . . . H12A H 0.4272 0.3641 0.0680 0.035 Uiso 1 1 calc R . . H12B H 0.6101 0.4231 0.0878 0.035 Uiso 1 1 calc R . . C13 C 0.5511(3) 0.3166(2) -0.01185(11) 0.0374(5) Uani 1 1 d . . . H13A H 0.4619 0.2431 -0.0371 0.045 Uiso 1 1 calc R . . H13B H 0.5583 0.3957 -0.0306 0.045 Uiso 1 1 calc R . . C14 C 0.6980(3) 0.2805(2) -0.02128(12) 0.0396(6) Uani 1 1 d . . . H14A H 0.7882 0.3567 0.0007 0.048 Uiso 1 1 calc R . . H14B H 0.7101 0.2596 -0.0702 0.048 Uiso 1 1 calc R . . C15 C 0.6931(3) 0.1621(2) 0.00938(12) 0.0382(5) Uani 1 1 d . . . H15A H 0.7920 0.1432 0.0046 0.046 Uiso 1 1 calc R . . H15B H 0.6093 0.0838 -0.0158 0.046 Uiso 1 1 calc R . . C16 C 0.6661(3) 0.1863(2) 0.08441(11) 0.0322(5) Uani 1 1 d . . . H16A H 0.7568 0.2568 0.1106 0.039 Uiso 1 1 calc R . . H16B H 0.6557 0.1049 0.1015 0.039 Uiso 1 1 calc R . . C21 C 0.4990(2) 0.13417(19) 0.22772(10) 0.0247(4) Uani 1 1 d . . . H21 H 0.4518 0.1495 0.2711 0.030 Uiso 1 1 calc R . . C22 C 0.3963(3) -0.0020(2) 0.18802(12) 0.0304(5) Uani 1 1 d . . . H22A H 0.2918 0.0013 0.1759 0.036 Uiso 1 1 calc R . . H22B H 0.4408 -0.0272 0.1456 0.036 Uiso 1 1 calc R . . C23 C 0.3859(3) -0.1040(2) 0.23195(13) 0.0356(5) Uani 1 1 d . . . H23A H 0.3328 -0.0824 0.2722 0.043 Uiso 1 1 calc R . . H23B H 0.3234 -0.1924 0.2058 0.043 Uiso 1 1 calc R . . C24 C 0.5445(3) -0.1075(2) 0.25488(14) 0.0382(5) Uani 1 1 d . . . H24A H 0.5926 -0.1393 0.2149 0.046 Uiso 1 1 calc R . . H24B H 0.5333 -0.1705 0.2853 0.046 Uiso 1 1 calc R . . C25 C 0.6496(3) 0.0283(2) 0.29196(13) 0.0376(5) Uani 1 1 d . . . H25A H 0.7540 0.0236 0.3030 0.045 Uiso 1 1 calc R . . H25B H 0.6084 0.0553 0.3350 0.045 Uiso 1 1 calc R . . C26 C 0.6610(2) 0.1314(2) 0.24874(12) 0.0311(5) Uani 1 1 d . . . H26A H 0.7121 0.1097 0.2078 0.037 Uiso 1 1 calc R . . H26B H 0.7244 0.2194 0.2749 0.037 Uiso 1 1 calc R . . C31 C 0.2517(2) 0.3072(2) 0.37633(10) 0.0254(4) Uani 1 1 d . . . C32 C 0.1864(3) 0.1714(2) 0.34988(12) 0.0324(5) Uani 1 1 d . . . H32 H 0.2079 0.1345 0.3063 0.039 Uiso 1 1 calc R . . C33 C 0.0903(3) 0.0902(2) 0.38683(14) 0.0413(6) Uani 1 1 d . . . H33 H 0.0465 -0.0017 0.3686 0.050 Uiso 1 1 calc R . . C34 C 0.0589(3) 0.1443(3) 0.45032(14) 0.0452(6) Uani 1 1 d . . . H34 H -0.0087 0.0895 0.4752 0.054 Uiso 1 1 calc R . . C35 C 0.1248(3) 0.2765(3) 0.47740(12) 0.0412(6) Uani 1 1 d . . . H35 H 0.1042 0.3124 0.5214 0.049 Uiso 1 1 calc R . . C36 C 0.2218(3) 0.3586(2) 0.44084(11) 0.0315(5) Uani 1 1 d . . . H36 H 0.2674 0.4500 0.4601 0.038 Uiso 1 1 calc R . . C41 C 0.3833(2) 0.57951(19) 0.36756(10) 0.0247(4) Uani 1 1 d . . . C42 C 0.2683(3) 0.6288(2) 0.34923(11) 0.0316(5) Uani 1 1 d . . . H42 H 0.1878 0.5756 0.3150 0.038 Uiso 1 1 calc R . . C43 C 0.2682(3) 0.7546(2) 0.37995(12) 0.0379(5) Uani 1 1 d . . . H43 H 0.1872 0.7862 0.3674 0.045 Uiso 1 1 calc R . . C44 C 0.3862(3) 0.8331(2) 0.42865(13) 0.0415(6) Uani 1 1 d . . . H44 H 0.3875 0.9194 0.4495 0.050 Uiso 1 1 calc R . . C45 C 0.5027(3) 0.7860(2) 0.44716(13) 0.0432(6) Uani 1 1 d . . . H45 H 0.5846 0.8404 0.4804 0.052 Uiso 1 1 calc R . . C46 C 0.5006(3) 0.6595(2) 0.41734(12) 0.0359(5) Uani 1 1 d . . . H46 H 0.5799 0.6273 0.4311 0.043 Uiso 1 1 calc R . . C51 C 0.5675(2) 0.4123(2) 0.35434(10) 0.0251(4) Uani 1 1 d . . . C52 C 0.6948(3) 0.4966(2) 0.33169(11) 0.0313(5) Uani 1 1 d . . . H52 H 0.6792 0.5493 0.3013 0.038 Uiso 1 1 calc R . . C53 C 0.8434(3) 0.5040(3) 0.35329(12) 0.0384(5) Uani 1 1 d . . . H53 H 0.9292 0.5619 0.3378 0.046 Uiso 1 1 calc R . . C54 C 0.8677(3) 0.4277(3) 0.39714(13) 0.0432(6) Uani 1 1 d . . . H54 H 0.9699 0.4330 0.4117 0.052 Uiso 1 1 calc R . . C55 C 0.7433(3) 0.3438(3) 0.41985(13) 0.0405(6) Uani 1 1 d . . . H55 H 0.7600 0.2914 0.4502 0.049 Uiso 1 1 calc R . . C56 C 0.5932(3) 0.3354(2) 0.39841(11) 0.0314(5) Uani 1 1 d . . . H56 H 0.5081 0.2768 0.4140 0.038 Uiso 1 1 calc R . . P3 P 0.08544(7) 0.25681(7) 0.79667(3) 0.03685(14) Uani 1 1 d . . . F1 F -0.0187(3) 0.10984(17) 0.76780(13) 0.0844(7) Uani 1 1 d . . . F2 F 0.1883(3) 0.4074(2) 0.82004(15) 0.1095(10) Uani 1 1 d . . . F3 F -0.0222(2) 0.30163(18) 0.74915(9) 0.0598(4) Uani 1 1 d . . . F4 F 0.1939(3) 0.2157(4) 0.84401(12) 0.1133(11) Uani 1 1 d . . . F5 F 0.1937(2) 0.24385(19) 0.73716(9) 0.0597(5) Uani 1 1 d . . . F6 F -0.0222(2) 0.2702(3) 0.85464(9) 0.0798(7) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru 0.01972(9) 0.01729(9) 0.02131(9) 0.00209(6) 0.00082(6) 0.00631(6) P1 0.0212(2) 0.0189(2) 0.0239(2) 0.00197(19) 0.00261(19) 0.00641(19) P2 0.0212(2) 0.0199(2) 0.0223(2) 0.00262(19) 0.00093(19) 0.00729(19) N 0.0328(10) 0.0224(9) 0.0309(9) 0.0047(7) 0.0010(7) 0.0070(7) C1 0.0201(10) 0.0263(10) 0.0363(11) 0.0066(9) -0.0006(8) 0.0025(8) C2 0.0196(10) 0.0379(12) 0.0314(11) 0.0053(9) 0.0019(8) 0.0073(9) C3 0.0238(10) 0.0318(11) 0.0327(11) 0.0022(9) -0.0023(8) 0.0132(9) C3A 0.0221(10) 0.0265(10) 0.0292(10) 0.0017(8) -0.0043(8) 0.0069(8) C4 0.0321(12) 0.0348(12) 0.0352(12) 0.0108(10) -0.0070(9) 0.0060(9) C5 0.0353(13) 0.0549(16) 0.0309(12) 0.0138(11) -0.0047(10) 0.0035(11) C6 0.0313(12) 0.0535(15) 0.0256(11) -0.0076(10) -0.0022(9) 0.0051(11) C7 0.0256(11) 0.0314(11) 0.0373(12) -0.0087(9) -0.0044(9) 0.0044(9) C7A 0.0200(9) 0.0252(10) 0.0311(11) 0.0007(8) -0.0029(8) 0.0027(8) C11 0.0253(10) 0.0242(10) 0.0244(10) 0.0009(8) 0.0051(8) 0.0053(8) C12 0.0310(11) 0.0266(10) 0.0281(10) 0.0045(8) 0.0051(8) 0.0075(9) C13 0.0423(13) 0.0383(13) 0.0284(11) 0.0076(10) 0.0068(10) 0.0078(11) C14 0.0430(13) 0.0381(13) 0.0338(12) 0.0055(10) 0.0161(10) 0.0068(11) C15 0.0386(13) 0.0351(12) 0.0395(13) 0.0017(10) 0.0180(10) 0.0117(10) C16 0.0313(11) 0.0304(11) 0.0361(12) 0.0053(9) 0.0107(9) 0.0120(9) C21 0.0242(10) 0.0216(10) 0.0293(10) 0.0050(8) 0.0026(8) 0.0092(8) C22 0.0279(11) 0.0249(10) 0.0364(12) 0.0048(9) 0.0000(9) 0.0070(8) C23 0.0354(12) 0.0236(11) 0.0477(14) 0.0104(10) 0.0019(10) 0.0077(9) C24 0.0405(13) 0.0265(11) 0.0502(14) 0.0090(10) 0.0019(11) 0.0143(10) C25 0.0361(12) 0.0336(12) 0.0462(14) 0.0090(10) -0.0058(10) 0.0165(10) C26 0.0268(11) 0.0282(11) 0.0385(12) 0.0040(9) -0.0013(9) 0.0115(9) C31 0.0232(10) 0.0280(10) 0.0271(10) 0.0089(8) 0.0012(8) 0.0094(8) C32 0.0351(12) 0.0282(11) 0.0340(11) 0.0075(9) 0.0036(9) 0.0096(9) C33 0.0442(14) 0.0303(12) 0.0488(14) 0.0164(11) 0.0028(11) 0.0063(10) C34 0.0467(15) 0.0487(15) 0.0456(14) 0.0289(12) 0.0121(12) 0.0108(12) C35 0.0457(14) 0.0512(15) 0.0317(12) 0.0158(11) 0.0097(11) 0.0177(12) C36 0.0318(11) 0.0360(12) 0.0272(10) 0.0066(9) 0.0013(9) 0.0119(9) C41 0.0286(10) 0.0211(9) 0.0230(9) 0.0025(8) 0.0035(8) 0.0072(8) C42 0.0308(11) 0.0285(11) 0.0330(11) -0.0012(9) -0.0008(9) 0.0108(9) C43 0.0464(14) 0.0309(12) 0.0399(13) 0.0026(10) 0.0014(11) 0.0207(11) C44 0.0571(16) 0.0247(11) 0.0402(13) -0.0021(10) 0.0020(11) 0.0150(11) C45 0.0503(15) 0.0286(12) 0.0408(13) -0.0077(10) -0.0090(11) 0.0087(11) C46 0.0408(13) 0.0316(12) 0.0319(11) -0.0015(9) -0.0065(10) 0.0130(10) C51 0.0238(10) 0.0280(10) 0.0221(9) -0.0001(8) -0.0010(8) 0.0096(8) C52 0.0292(11) 0.0352(12) 0.0267(10) 0.0029(9) 0.0002(9) 0.0088(9) C53 0.0247(11) 0.0492(14) 0.0351(12) -0.0003(10) 0.0014(9) 0.0085(10) C54 0.0286(12) 0.0575(16) 0.0419(13) -0.0030(12) -0.0050(10) 0.0206(11) C55 0.0416(13) 0.0499(15) 0.0356(12) 0.0070(11) -0.0046(10) 0.0250(12) C56 0.0310(11) 0.0330(11) 0.0317(11) 0.0055(9) 0.0016(9) 0.0135(9) P3 0.0304(3) 0.0425(3) 0.0374(3) 0.0076(3) 0.0010(2) 0.0121(3) F1 0.0978(16) 0.0324(9) 0.1173(18) 0.0157(10) 0.0316(14) 0.0099(10) F2 0.0612(13) 0.0751(15) 0.140(2) -0.0407(15) -0.0044(14) -0.0134(11) F3 0.0544(10) 0.0656(11) 0.0711(12) 0.0280(9) 0.0013(8) 0.0285(9) F4 0.0862(16) 0.243(3) 0.0747(14) 0.0883(19) 0.0318(12) 0.109(2) F5 0.0651(11) 0.0766(12) 0.0583(10) 0.0322(9) 0.0269(9) 0.0393(10) F6 0.0519(11) 0.148(2) 0.0443(10) 0.0084(11) 0.0110(8) 0.0450(12) _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 C2 2.181(2) . ? Ru N 2.1896(17) . ? Ru C1 2.198(2) . ? Ru C3 2.228(2) . ? Ru P2 2.2717(5) . ? Ru P1 2.3309(5) . ? Ru C3A 2.344(2) . ? Ru C7A 2.351(2) . ? P1 C21 1.850(2) . ? P1 C11 1.853(2) . ? P1 H1P 1.30(2) . ? P2 C51 1.835(2) . ? P2 C31 1.840(2) . ? P2 C41 1.852(2) . ? C1 C2 1.430(3) . ? C1 C7A 1.439(3) . ? C2 C3 1.418(3) . ? C3 C3A 1.447(3) . ? C3A C4 1.417(3) . ? C3A C7A 1.430(3) . ? C4 C5 1.361(4) . ? C5 C6 1.411(4) . ? C6 C7 1.374(4) . ? C7 C7A 1.424(3) . ? C11 C12 1.536(3) . ? C11 C16 1.537(3) . ? C12 C13 1.534(3) . ? C13 C14 1.518(4) . ? C14 C15 1.522(3) . ? C15 C16 1.531(3) . ? C21 C26 1.535(3) . ? C21 C22 1.538(3) . ? C22 C23 1.531(3) . ? C23 C24 1.519(3) . ? C24 C25 1.526(3) . ? C25 C26 1.529(3) . ? C31 C36 1.390(3) . ? C31 C32 1.401(3) . ? C32 C33 1.391(3) . ? C33 C34 1.385(4) . ? C34 C35 1.371(4) . ? C35 C36 1.395(3) . ? C41 C42 1.385(3) . ? C41 C46 1.391(3) . ? C42 C43 1.393(3) . ? C43 C44 1.378(4) . ? C44 C45 1.383(4) . ? C45 C46 1.388(3) . ? C51 C56 1.391(3) . ? C51 C52 1.398(3) . ? C52 C53 1.385(3) . ? C53 C54 1.377(4) . ? C54 C55 1.379(4) . ? C55 C56 1.392(3) . ? P3 F4 1.567(2) . ? P3 F6 1.5718(18) . ? P3 F1 1.575(2) . ? P3 F3 1.5889(17) . ? P3 F2 1.589(2) . ? P3 F5 1.5988(17) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 Ru N 132.02(8) . . ? C2 Ru C1 38.13(8) . . ? N Ru C1 153.98(8) . . ? C2 Ru C3 37.50(8) . . ? N Ru C3 97.20(8) . . ? C1 Ru C3 63.41(8) . . ? C2 Ru P2 91.13(6) . . ? N Ru P2 92.13(5) . . ? C1 Ru P2 109.99(6) . . ? C3 Ru P2 108.71(6) . . ? C2 Ru P1 138.14(6) . . ? N Ru P1 89.60(5) . . ? C1 Ru P1 102.90(6) . . ? C3 Ru P1 158.28(6) . . ? P2 Ru P1 91.531(18) . . ? C2 Ru C3A 61.08(8) . . ? N Ru C3A 92.62(7) . . ? C1 Ru C3A 61.39(8) . . ? C3 Ru C3A 36.79(7) . . ? P2 Ru C3A 145.50(5) . . ? P1 Ru C3A 122.64(5) . . ? C2 Ru C7A 61.06(8) . . ? N Ru C7A 119.78(7) . . ? C1 Ru C7A 36.70(8) . . ? C3 Ru C7A 61.08(8) . . ? P2 Ru C7A 146.65(6) . . ? P1 Ru C7A 97.67(5) . . ? C3A Ru C7A 35.46(7) . . ? C21 P1 C11 108.89(9) . . ? C21 P1 Ru 116.28(7) . . ? C11 P1 Ru 117.21(7) . . ? C21 P1 H1P 100.2(10) . . ? C11 P1 H1P 97.4(10) . . ? Ru P1 H1P 114.0(10) . . ? C51 P2 C31 101.55(9) . . ? C51 P2 C41 99.62(9) . . ? C31 P2 C41 102.62(9) . . ? C51 P2 Ru 120.73(7) . . ? C31 P2 Ru 115.42(7) . . ? C41 P2 Ru 114.19(7) . . ? C2 C1 C7A 107.01(19) . . ? C2 C1 Ru 70.32(12) . . ? C7A C1 Ru 77.44(12) . . ? C3 C2 C1 109.49(19) . . ? C3 C2 Ru 73.04(12) . . ? C1 C2 Ru 71.56(12) . . ? C2 C3 C3A 107.03(18) . . ? C2 C3 Ru 69.46(12) . . ? C3A C3 Ru 75.98(12) . . ? C4 C3A C7A 120.4(2) . . ? C4 C3A C3 131.5(2) . . ? C7A C3A C3 108.09(19) . . ? C4 C3A Ru 127.59(15) . . ? C7A C3A Ru 72.51(11) . . ? C3 C3A Ru 67.23(11) . . ? C5 C4 C3A 118.7(2) . . ? C4 C5 C6 121.3(2) . . ? C7 C6 C5 121.8(2) . . ? C6 C7 C7A 118.4(2) . . ? C7 C7A C3A 119.3(2) . . ? C7 C7A C1 132.6(2) . . ? C3A C7A C1 108.06(18) . . ? C7 C7A Ru 129.92(15) . . ? C3A C7A Ru 72.03(11) . . ? C1 C7A Ru 65.86(11) . . ? C12 C11 C16 110.56(17) . . ? C12 C11 P1 108.39(13) . . ? C16 C11 P1 113.47(15) . . ? C13 C12 C11 111.68(18) . . ? C14 C13 C12 110.9(2) . . ? C13 C14 C15 110.75(19) . . ? C14 C15 C16 111.74(19) . . ? C15 C16 C11 111.89(19) . . ? C26 C21 C22 111.06(17) . . ? C26 C21 P1 115.95(14) . . ? C22 C21 P1 113.12(14) . . ? C23 C22 C21 109.16(18) . . ? C24 C23 C22 111.73(19) . . ? C23 C24 C25 111.71(19) . . ? C24 C25 C26 111.2(2) . . ? C25 C26 C21 110.01(18) . . ? C36 C31 C32 118.7(2) . . ? C36 C31 P2 122.32(17) . . ? C32 C31 P2 118.94(16) . . ? C33 C32 C31 120.6(2) . . ? C34 C33 C32 119.6(2) . . ? C35 C34 C33 120.4(2) . . ? C34 C35 C36 120.5(2) . . ? C31 C36 C35 120.2(2) . . ? C42 C41 C46 118.29(19) . . ? C42 C41 P2 118.67(16) . . ? C46 C41 P2 123.04(17) . . ? C41 C42 C43 121.3(2) . . ? C44 C43 C42 119.6(2) . . ? C43 C44 C45 119.9(2) . . ? C44 C45 C46 120.3(2) . . ? C45 C46 C41 120.6(2) . . ? C56 C51 C52 118.67(19) . . ? C56 C51 P2 123.59(16) . . ? C52 C51 P2 117.74(16) . . ? C53 C52 C51 120.5(2) . . ? C54 C53 C52 120.4(2) . . ? C53 C54 C55 119.9(2) . . ? C54 C55 C56 120.2(2) . . ? C51 C56 C55 120.3(2) . . ? F4 P3 F6 90.82(11) . . ? F4 P3 F1 93.11(17) . . ? F6 P3 F1 90.62(13) . . ? F4 P3 F3 178.79(16) . . ? F6 P3 F3 89.26(11) . . ? F1 P3 F3 88.10(12) . . ? F4 P3 F2 90.63(18) . . ? F6 P3 F2 91.90(14) . . ? F1 P3 F2 175.46(16) . . ? F3 P3 F2 88.16(14) . . ? F4 P3 F5 89.87(10) . . ? F6 P3 F5 179.30(11) . . ? F1 P3 F5 89.42(12) . . ? F3 P3 F5 90.04(10) . . ? F2 P3 F5 88.02(13) . . ? 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 C2 Ru P1 C21 -35.36(12) . . . . ? N Ru P1 C21 150.16(9) . . . . ? C1 Ru P1 C21 -52.87(9) . . . . ? C3 Ru P1 C21 -101.10(18) . . . . ? P2 Ru P1 C21 58.04(7) . . . . ? C3A Ru P1 C21 -116.98(10) . . . . ? C7A Ru P1 C21 -89.82(9) . . . . ? C2 Ru P1 C11 95.93(12) . . . . ? N Ru P1 C11 -78.54(9) . . . . ? C1 Ru P1 C11 78.43(10) . . . . ? C3 Ru P1 C11 30.20(18) . . . . ? P2 Ru P1 C11 -170.66(7) . . . . ? C3A Ru P1 C11 14.32(10) . . . . ? C7A Ru P1 C11 41.48(9) . . . . ? P2 Ru P1 H1P -57.8(11) . . . . ? N Ru P1 H1P 34.3(11) . . . . ? C2 Ru P2 C51 153.53(10) . . . . ? N Ru P2 C51 -74.35(9) . . . . ? C1 Ru P2 C51 119.63(10) . . . . ? C3 Ru P2 C51 -172.68(10) . . . . ? P1 Ru P2 C51 15.31(8) . . . . ? C3A Ru P2 C51 -172.10(12) . . . . ? C7A Ru P2 C51 121.78(12) . . . . ? C2 Ru P2 C31 30.82(9) . . . . ? N Ru P2 C31 162.95(9) . . . . ? C1 Ru P2 C31 -3.08(9) . . . . ? C3 Ru P2 C31 64.61(10) . . . . ? P1 Ru P2 C31 -107.40(7) . . . . ? C3A Ru P2 C31 65.19(12) . . . . ? C7A Ru P2 C31 -0.93(12) . . . . ? C2 Ru P2 C41 -87.77(10) . . . . ? N Ru P2 C41 44.36(9) . . . . ? C1 Ru P2 C41 -121.67(9) . . . . ? C3 Ru P2 C41 -53.98(10) . . . . ? P1 Ru P2 C41 134.01(7) . . . . ? C3A Ru P2 C41 -53.40(12) . . . . ? C7A Ru P2 C41 -119.52(12) . . . . ? N Ru C1 C2 -82.1(2) . . . . ? C3 Ru C1 C2 -36.95(13) . . . . ? P2 Ru C1 C2 64.57(13) . . . . ? P1 Ru C1 C2 161.03(12) . . . . ? C3A Ru C1 C2 -78.61(14) . . . . ? C7A Ru C1 C2 -113.46(18) . . . . ? C2 Ru C1 C7A 113.46(18) . . . . ? N Ru C1 C7A 31.4(2) . . . . ? C3 Ru C1 C7A 76.51(13) . . . . ? P2 Ru C1 C7A 178.03(10) . . . . ? P1 Ru C1 C7A -85.52(12) . . . . ? C3A Ru C1 C7A 34.84(12) . . . . ? C7A C1 C2 C3 -5.8(2) . . . . ? Ru C1 C2 C3 63.62(15) . . . . ? C7A C1 C2 Ru -69.45(14) . . . . ? N Ru C2 C3 26.20(17) . . . . ? C1 Ru C2 C3 -118.00(18) . . . . ? P2 Ru C2 C3 120.09(12) . . . . ? P1 Ru C2 C3 -146.35(10) . . . . ? C3A Ru C2 C3 -38.48(12) . . . . ? C7A Ru C2 C3 -79.21(13) . . . . ? N Ru C2 C1 144.20(13) . . . . ? C3 Ru C2 C1 118.00(18) . . . . ? P2 Ru C2 C1 -121.91(12) . . . . ? P1 Ru C2 C1 -28.35(17) . . . . ? C3A Ru C2 C1 79.51(13) . . . . ? C7A Ru C2 C1 38.79(12) . . . . ? C1 C2 C3 C3A 4.6(2) . . . . ? Ru C2 C3 C3A 67.33(14) . . . . ? C1 C2 C3 Ru -62.69(14) . . . . ? N Ru C3 C2 -160.69(12) . . . . ? C1 Ru C3 C2 37.56(13) . . . . ? P2 Ru C3 C2 -65.97(13) . . . . ? P1 Ru C3 C2 91.96(19) . . . . ? C3A Ru C3 C2 114.58(18) . . . . ? C7A Ru C3 C2 79.16(13) . . . . ? C2 Ru C3 C3A -114.58(18) . . . . ? N Ru C3 C3A 84.73(13) . . . . ? C1 Ru C3 C3A -77.01(13) . . . . ? P2 Ru C3 C3A 179.45(11) . . . . ? P1 Ru C3 C3A -22.6(2) . . . . ? C7A Ru C3 C3A -35.42(12) . . . . ? C2 C3 C3A C4 176.3(2) . . . . ? Ru C3 C3A C4 -120.8(2) . . . . ? C2 C3 C3A C7A -1.6(2) . . . . ? Ru C3 C3A C7A 61.31(14) . . . . ? C2 C3 C3A Ru -62.96(14) . . . . ? C2 Ru C3A C4 164.9(2) . . . . ? N Ru C3A C4 27.2(2) . . . . ? C1 Ru C3A C4 -151.3(2) . . . . ? C3 Ru C3A C4 125.7(3) . . . . ? P2 Ru C3A C4 124.79(18) . . . . ? P1 Ru C3A C4 -64.0(2) . . . . ? C7A Ru C3A C4 -115.3(2) . . . . ? C2 Ru C3A C7A -79.80(14) . . . . ? N Ru C3A C7A 142.44(12) . . . . ? C1 Ru C3A C7A -36.05(12) . . . . ? C3 Ru C3A C7A -119.04(18) . . . . ? P2 Ru C3A C7A -119.96(12) . . . . ? P1 Ru C3A C7A 51.23(13) . . . . ? C2 Ru C3A C3 39.24(13) . . . . ? N Ru C3A C3 -98.52(13) . . . . ? C1 Ru C3A C3 82.99(14) . . . . ? P2 Ru C3A C3 -0.92(18) . . . . ? P1 Ru C3A C3 170.27(11) . . . . ? C7A Ru C3A C3 119.04(18) . . . . ? C7A C3A C4 C5 2.7(3) . . . . ? C3 C3A C4 C5 -175.0(2) . . . . ? Ru C3A C4 C5 93.4(2) . . . . ? C3A C4 C5 C6 -0.9(3) . . . . ? C4 C5 C6 C7 -1.2(4) . . . . ? C5 C6 C7 C7A 1.4(3) . . . . ? C6 C7 C7A C3A 0.4(3) . . . . ? C6 C7 C7A C1 177.4(2) . . . . ? C6 C7 C7A Ru -90.1(3) . . . . ? C4 C3A C7A C7 -2.4(3) . . . . ? C3 C3A C7A C7 175.73(18) . . . . ? Ru C3A C7A C7 -126.27(18) . . . . ? C4 C3A C7A C1 179.90(18) . . . . ? C3 C3A C7A C1 -1.9(2) . . . . ? Ru C3A C7A C1 56.08(14) . . . . ? C4 C3A C7A Ru 123.82(19) . . . . ? C3 C3A C7A Ru -58.01(14) . . . . ? C2 C1 C7A C7 -172.5(2) . . . . ? Ru C1 C7A C7 122.9(2) . . . . ? C2 C1 C7A C3A 4.7(2) . . . . ? Ru C1 C7A C3A -59.88(14) . . . . ? C2 C1 C7A Ru 64.59(13) . . . . ? C2 Ru C7A C7 -166.6(2) . . . . ? N Ru C7A C7 69.0(2) . . . . ? C1 Ru C7A C7 -126.3(3) . . . . ? C3 Ru C7A C7 150.3(2) . . . . ? P2 Ru C7A C7 -129.70(19) . . . . ? P1 Ru C7A C7 -25.0(2) . . . . ? C3A Ru C7A C7 113.5(3) . . . . ? C2 Ru C7A C3A 79.84(14) . . . . ? N Ru C7A C3A -44.56(14) . . . . ? C1 Ru C7A C3A 120.17(18) . . . . ? C3 Ru C7A C3A 36.74(12) . . . . ? P2 Ru C7A C3A 116.79(12) . . . . ? P1 Ru C7A C3A -138.51(11) . . . . ? C2 Ru C7A C1 -40.33(13) . . . . ? N Ru C7A C1 -164.73(12) . . . . ? C3 Ru C7A C1 -83.42(14) . . . . ? P2 Ru C7A C1 -3.38(18) . . . . ? P1 Ru C7A C1 101.32(12) . . . . ? C3A Ru C7A C1 -120.17(18) . . . . ? C21 P1 C11 C12 -176.11(14) . . . . ? Ru P1 C11 C12 49.29(15) . . . . ? H1P P1 C11 C12 -72.6(10) . . . . ? C21 P1 C11 C16 -52.89(17) . . . . ? Ru P1 C11 C16 172.50(12) . . . . ? H1P P1 C11 C16 50.6(10) . . . . ? C16 C11 C12 C13 54.3(2) . . . . ? P1 C11 C12 C13 179.27(15) . . . . ? C11 C12 C13 C14 -56.7(2) . . . . ? C12 C13 C14 C15 57.0(3) . . . . ? C13 C14 C15 C16 -56.2(3) . . . . ? C14 C15 C16 C11 54.6(3) . . . . ? C12 C11 C16 C15 -53.1(2) . . . . ? P1 C11 C16 C15 -175.16(15) . . . . ? C11 P1 C21 C26 81.12(17) . . . . ? Ru P1 C21 C26 -143.80(13) . . . . ? H1P P1 C21 C26 -20.5(10) . . . . ? C11 P1 C21 C22 -48.84(17) . . . . ? H1P P1 C21 C22 -150.4(10) . . . . ? Ru P1 C21 C22 86.23(15) . . . . ? C26 C21 C22 C23 58.2(2) . . . . ? P1 C21 C22 C23 -169.43(15) . . . . ? C21 C22 C23 C24 -56.6(2) . . . . ? C22 C23 C24 C25 55.5(3) . . . . ? C23 C24 C25 C26 -54.8(3) . . . . ? C24 C25 C26 C21 55.8(3) . . . . ? C22 C21 C26 C25 -58.3(2) . . . . ? P1 C21 C26 C25 170.80(15) . . . . ? C51 P2 C31 C36 86.44(19) . . . . ? C41 P2 C31 C36 -16.3(2) . . . . ? Ru P2 C31 C36 -141.14(16) . . . . ? C51 P2 C31 C32 -93.41(18) . . . . ? C41 P2 C31 C32 163.85(17) . . . . ? Ru P2 C31 C32 39.01(19) . . . . ? C36 C31 C32 C33 1.5(3) . . . . ? P2 C31 C32 C33 -178.61(18) . . . . ? C31 C32 C33 C34 0.1(4) . . . . ? C32 C33 C34 C35 -1.5(4) . . . . ? C33 C34 C35 C36 1.3(4) . . . . ? C32 C31 C36 C35 -1.8(3) . . . . ? P2 C31 C36 C35 178.38(18) . . . . ? C34 C35 C36 C31 0.4(4) . . . . ? C51 P2 C41 C42 168.82(18) . . . . ? C31 P2 C41 C42 -86.93(18) . . . . ? Ru P2 C41 C42 38.70(19) . . . . ? C51 P2 C41 C46 -10.9(2) . . . . ? C31 P2 C41 C46 93.3(2) . . . . ? Ru P2 C41 C46 -141.06(18) . . . . ? C46 C41 C42 C43 -0.6(3) . . . . ? P2 C41 C42 C43 179.67(18) . . . . ? C41 C42 C43 C44 1.3(4) . . . . ? C42 C43 C44 C45 -0.7(4) . . . . ? C43 C44 C45 C46 -0.6(4) . . . . ? C44 C45 C46 C41 1.3(4) . . . . ? C42 C41 C46 C45 -0.7(4) . . . . ? P2 C41 C46 C45 179.0(2) . . . . ? C31 P2 C51 C56 7.2(2) . . . . ? C41 P2 C51 C56 112.27(18) . . . . ? Ru P2 C51 C56 -121.97(16) . . . . ? C31 P2 C51 C52 -172.19(16) . . . . ? C41 P2 C51 C52 -67.08(17) . . . . ? Ru P2 C51 C52 58.67(18) . . . . ? C56 C51 C52 C53 -0.6(3) . . . . ? P2 C51 C52 C53 178.83(17) . . . . ? C51 C52 C53 C54 0.3(3) . . . . ? C52 C53 C54 C55 -0.2(4) . . . . ? C53 C54 C55 C56 0.3(4) . . . . ? C52 C51 C56 C55 0.7(3) . . . . ? P2 C51 C56 C55 -178.69(17) . . . . ? C54 C55 C56 C51 -0.5(4) . . . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 26.39 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.749 _refine_diff_density_min -0.434 _refine_diff_density_rms 0.075 #===END data_8a _audit_creation_method 'manual editing of SHELXL template' _publ_contact_author_name 'Dr. Lisa Rosenberg' _publ_contact_author_address ; Department of Chemistry University of Victoria P.O. Box 3065 Victoria, BC V8W 3V6 Canada ; _publ_contact_author_email lisarose@uvic.ca _publ_contact_author_fax '1(250)7217147' _publ_contact_author_phone '1(250)7217173' _publ_contact_letter ; To: Cambridge Crystallographic Data Centre Please accept the following CIF data in support of a manuscript being submitted to the Journal of the American Chemical Society. Please forward any questions concerning this CIF to Bob McDonald (Bob.McDonald@ualberta.ca). ; _publ_requested_journal 'Journal of the American Chemical Society' _publ_section_title ; A highly reactive ruthenium phosphido complex exhibiting Ru-P \p-bonding ; loop_ _publ_author_name _publ_author_footnote _publ_author_address 'Derrah, Eric J.' . ; Department of Chemistry University of Victoria P.O. Box 3065 Victoria, BC V8W 3V6 Canada ; 'McDonald, Robert' 'X-ray Crystallography Laboratory' ; Department of Chemistry University of Alberta Edmonton, AB T6G 2G2 Canada ; 'Pantazis, Dimitrios A.' . ; Department of Chemistry University of Glasgow Glasgow G12 8QQ United Kingdom ; 'Rosenberg, Lisa' . ; Department of Chemistry University of Victoria P.O. Box 3065 Victoria, BC V8W 3V6 Canada ; _chemical_formula_moiety 'C45 H60 P2 Ru Si' _chemical_formula_sum 'C45 H60 P2 Ru Si' _chemical_formula_weight 792.03 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Si' 'Si' 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ru' 'Ru' -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.5039(14) _cell_length_b 12.0314(14) _cell_length_c 16.4281(19) _cell_angle_alpha 81.4603(17) _cell_angle_beta 89.8746(17) _cell_angle_gamma 64.4406(15) _cell_volume 2023.6(4) _cell_formula_units_Z 2 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 5019 _cell_measurement_theta_min 2.45 _cell_measurement_theta_max 26.21 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.300 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 836 _exptl_absorpt_coefficient_mu 0.526 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.8092 _exptl_absorpt_correction_T_max 0.9159 _exptl_absorpt_process_details 'Bruker SHELXTL (Bruker, 1997)' _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 15662 _diffrn_reflns_av_R_equivalents 0.0274 _diffrn_reflns_av_sigmaI/netI 0.0412 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.26 _diffrn_reflns_theta_max 26.28 _reflns_number_total 8117 _reflns_number_gt 6661 _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^)+(0.0439P)^2^+0.2208P] 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 8117 _refine_ls_number_parameters 452 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0462 _refine_ls_R_factor_gt 0.0315 _refine_ls_wR_factor_ref 0.0860 _refine_ls_wR_factor_gt 0.0749 _refine_ls_goodness_of_fit_ref 1.111 _refine_ls_restrained_S_all 1.111 _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 0.207282(18) 0.199113(18) 0.324181(12) 0.02058(7) Uani 1 1 d . A . P1 P 0.02997(6) 0.27348(6) 0.23416(4) 0.02363(14) Uani 1 1 d . . . H1P H 0.026(3) 0.352(3) 0.1682(17) 0.044(8) Uiso 1 1 d . . . P2 P 0.35573(6) 0.13240(6) 0.22872(4) 0.02283(14) Uani 1 1 d . . . Si Si 0.18371(7) 0.41057(6) 0.30481(5) 0.02702(16) Uani 1 1 d D . . C1 C 0.3337(2) 0.1157(2) 0.44199(15) 0.0279(6) Uani 1 1 d . . . H1 H 0.4217 0.1110 0.4510 0.034 Uiso 1 1 calc R A . C2 C 0.2165(2) 0.2153(2) 0.45521(15) 0.0283(6) Uani 1 1 d . A . H2 H 0.2084 0.2917 0.4767 0.034 Uiso 1 1 calc R . . C3 C 0.1139(2) 0.1848(2) 0.44125(15) 0.0290(6) Uani 1 1 d . . . H3 H 0.0213 0.2363 0.4506 0.035 Uiso 1 1 calc R A . C3A C 0.1693(2) 0.0563(2) 0.42943(15) 0.0276(6) Uani 1 1 d . A . C4 C 0.1166(3) -0.0287(3) 0.42366(16) 0.0362(6) Uani 1 1 d . . . H4 H 0.0257 -0.0014 0.4211 0.043 Uiso 1 1 calc R A . C5 C 0.1974(3) -0.1499(3) 0.42178(18) 0.0455(8) Uani 1 1 d . A . H5 H 0.1622 -0.2079 0.4199 0.055 Uiso 1 1 calc R . . C6 C 0.3317(3) -0.1919(3) 0.42253(18) 0.0462(8) Uani 1 1 d . . . H6 H 0.3855 -0.2778 0.4218 0.055 Uiso 1 1 calc R A . C7 C 0.3863(3) -0.1115(3) 0.42433(17) 0.0365(7) Uani 1 1 d . A . H7 H 0.4770 -0.1399 0.4220 0.044 Uiso 1 1 calc R . . C7A C 0.3062(2) 0.0138(2) 0.42965(15) 0.0273(6) Uani 1 1 d . A . C11 C -0.1231(2) 0.3708(2) 0.27859(17) 0.0287(6) Uani 1 1 d . . . H11 H -0.0945 0.3977 0.3264 0.034 Uiso 1 1 calc R . . C12 C -0.2011(2) 0.3037(2) 0.31613(18) 0.0349(6) Uani 1 1 d . . . H12A H -0.1438 0.2272 0.3542 0.042 Uiso 1 1 calc R . . H12B H -0.2382 0.2786 0.2719 0.042 Uiso 1 1 calc R . . C13 C -0.3101(3) 0.3889(3) 0.3633(2) 0.0494(8) Uani 1 1 d . . . H13A H -0.3627 0.3455 0.3848 0.059 Uiso 1 1 calc R . . H13B H -0.2725 0.4070 0.4109 0.059 Uiso 1 1 calc R . . C14 C -0.3953(3) 0.5097(3) 0.3085(3) 0.0623(11) Uani 1 1 d . . . H14A H -0.4409 0.4921 0.2647 0.075 Uiso 1 1 calc R . . H14B H -0.4613 0.5647 0.3415 0.075 Uiso 1 1 calc R . . C15 C -0.3196(3) 0.5765(3) 0.2692(2) 0.0522(9) Uani 1 1 d . . . H15A H -0.2838 0.6045 0.3124 0.063 Uiso 1 1 calc R . . H15B H -0.3781 0.6514 0.2303 0.063 Uiso 1 1 calc R . . C16 C -0.2103(3) 0.4925(2) 0.22318(19) 0.0376(7) Uani 1 1 d . . . H16A H -0.1584 0.5368 0.2019 0.045 Uiso 1 1 calc R . . H16B H -0.2468 0.4737 0.1754 0.045 Uiso 1 1 calc R . . C21 C -0.0044(2) 0.1748(2) 0.17011(16) 0.0292(6) Uani 1 1 d . . . H21 H 0.0748 0.1370 0.1394 0.035 Uiso 1 1 calc R . . C22 C -0.0214(3) 0.0640(3) 0.21661(17) 0.0340(6) Uani 1 1 d . . . H22A H 0.0542 0.0131 0.2563 0.041 Uiso 1 1 calc R . . H22B H -0.0992 0.0949 0.2483 0.041 Uiso 1 1 calc R . . C23 C -0.0350(3) -0.0171(3) 0.1581(2) 0.0450(8) Uani 1 1 d . . . H23A H 0.0467 -0.0557 0.1310 0.054 Uiso 1 1 calc R . . H23B H -0.0510 -0.0851 0.1900 0.054 Uiso 1 1 calc R . . C24 C -0.1444(3) 0.0578(3) 0.0929(2) 0.0590(10) Uani 1 1 d . . . H24A H -0.2275 0.0895 0.1194 0.071 Uiso 1 1 calc R . . H24B H -0.1477 0.0034 0.0542 0.071 Uiso 1 1 calc R . . C25 C -0.1263(4) 0.1668(3) 0.0457(2) 0.0587(10) Uani 1 1 d . . . H25A H -0.2010 0.2169 0.0053 0.070 Uiso 1 1 calc R . . H25B H -0.0476 0.1346 0.0148 0.070 Uiso 1 1 calc R . . C26 C -0.1139(3) 0.2493(3) 0.10323(18) 0.0434(7) Uani 1 1 d . . . H26A H -0.1962 0.2887 0.1295 0.052 Uiso 1 1 calc R . . H26B H -0.0973 0.3166 0.0709 0.052 Uiso 1 1 calc R . . C31 C 0.5245(2) 0.0552(2) 0.27297(16) 0.0259(5) Uani 1 1 d . . . C32 C 0.5659(2) 0.1158(2) 0.32365(15) 0.0270(6) Uani 1 1 d . . . H32 H 0.5072 0.1961 0.3338 0.032 Uiso 1 1 calc R . . C33 C 0.6901(2) 0.0620(3) 0.35950(17) 0.0311(6) Uani 1 1 d . . . H33 H 0.7164 0.1056 0.3935 0.037 Uiso 1 1 calc R . . C34 C 0.7756(3) -0.0542(3) 0.34619(18) 0.0371(7) Uani 1 1 d . . . H34 H 0.8613 -0.0917 0.3708 0.044 Uiso 1 1 calc R . . C35 C 0.7360(3) -0.1166(3) 0.2966(2) 0.0428(7) Uani 1 1 d . . . H35 H 0.7948 -0.1976 0.2876 0.051 Uiso 1 1 calc R . . C36 C 0.6122(2) -0.0626(2) 0.26011(18) 0.0348(6) Uani 1 1 d . . . H36 H 0.5867 -0.1064 0.2258 0.042 Uiso 1 1 calc R . . C41 C 0.3541(2) 0.0068(2) 0.17772(15) 0.0264(5) Uani 1 1 d . . . C42 C 0.3105(2) -0.0736(2) 0.22104(16) 0.0299(6) Uani 1 1 d . . . H42 H 0.2722 -0.0558 0.2717 0.036 Uiso 1 1 calc R . . C43 C 0.3217(3) -0.1798(3) 0.19184(19) 0.0375(7) Uani 1 1 d . . . H43 H 0.2924 -0.2348 0.2228 0.045 Uiso 1 1 calc R . . C44 C 0.3750(3) -0.2055(3) 0.11817(19) 0.0398(7) Uani 1 1 d . . . H44 H 0.3837 -0.2787 0.0984 0.048 Uiso 1 1 calc R . . C45 C 0.4157(3) -0.1254(3) 0.07336(19) 0.0459(8) Uani 1 1 d . . . H45 H 0.4505 -0.1422 0.0217 0.055 Uiso 1 1 calc R . . C46 C 0.4067(3) -0.0195(3) 0.10254(17) 0.0385(7) Uani 1 1 d . . . H46 H 0.4365 0.0349 0.0712 0.046 Uiso 1 1 calc R . . C51 C 0.3660(2) 0.2380(2) 0.13882(16) 0.0281(6) Uani 1 1 d . . . C52 C 0.4598(3) 0.2811(3) 0.13406(18) 0.0357(6) Uani 1 1 d . . . H52 H 0.5262 0.2516 0.1771 0.043 Uiso 1 1 calc R . . C53 C 0.4579(3) 0.3673(3) 0.0668(2) 0.0479(8) Uani 1 1 d . . . H53 H 0.5225 0.3968 0.0641 0.057 Uiso 1 1 calc R . . C54 C 0.3630(3) 0.4095(3) 0.0046(2) 0.0483(8) Uani 1 1 d . . . H54 H 0.3613 0.4690 -0.0409 0.058 Uiso 1 1 calc R . . C55 C 0.2703(3) 0.3667(3) 0.00734(18) 0.0444(7) Uani 1 1 d . . . H55 H 0.2053 0.3957 -0.0365 0.053 Uiso 1 1 calc R . . C56 C 0.2714(3) 0.2811(3) 0.07384(17) 0.0353(6) Uani 1 1 d . . . H56 H 0.2071 0.2513 0.0753 0.042 Uiso 1 1 calc R . . C61 C 0.3244(3) 0.4376(3) 0.34244(19) 0.0369(7) Uani 1 1 d . A . H61A H 0.3981 0.3945 0.3096 0.044 Uiso 1 1 calc R . . H61B H 0.2997 0.5282 0.3276 0.044 Uiso 1 1 calc R . . C62 C 0.3748(3) 0.4000(3) 0.4317(2) 0.0466(8) Uani 1 1 d . . . H62A H 0.4457 0.4227 0.4392 0.056 Uiso 1 1 calc R A . H62B H 0.4062 0.3095 0.4477 0.056 Uiso 1 1 calc R . . H62C H 0.3051 0.4432 0.4662 0.056 Uiso 1 1 calc R . . C63 C 0.0420(3) 0.5133(3) 0.3632(2) 0.0400(7) Uani 1 1 d . A . H63A H -0.0378 0.5448 0.3267 0.048 Uiso 1 1 calc R . . H63B H 0.0331 0.4588 0.4118 0.048 Uiso 1 1 calc R . . C64 C 0.0471(3) 0.6241(3) 0.3930(2) 0.0520(9) Uani 1 1 d . . . H64A H -0.0309 0.6672 0.4214 0.062 Uiso 1 1 calc R A . H64B H 0.0520 0.6817 0.3457 0.062 Uiso 1 1 calc R . . H64C H 0.1235 0.5953 0.4312 0.062 Uiso 1 1 calc R . . C65A C 0.1545(17) 0.5023(9) 0.1952(3) 0.043(2) Uani 0.70 1 d PD A 1 H65A H 0.2396 0.4786 0.1716 0.052 Uiso 0.70 1 calc PR A 1 H65B H 0.1046 0.4732 0.1620 0.052 Uiso 0.70 1 calc PR A 1 C66A C 0.0859(6) 0.6428(4) 0.1824(3) 0.0641(14) Uani 0.70 1 d PD A 1 H66A H 0.0754 0.6758 0.1233 0.077 Uiso 0.70 1 calc PR A 1 H66B H 0.1369 0.6749 0.2108 0.077 Uiso 0.70 1 calc PR A 1 H66C H 0.0008 0.6692 0.2049 0.077 Uiso 0.70 1 calc PR A 1 C65B C 0.136(4) 0.509(2) 0.1968(8) 0.043(2) Uani 0.30 1 d PD A 2 H65C H 0.1665 0.4505 0.1563 0.052 Uiso 0.30 1 calc PR A 2 H65D H 0.0405 0.5502 0.1898 0.052 Uiso 0.30 1 calc PR A 2 C66B C 0.1830(14) 0.6075(9) 0.1733(6) 0.0641(14) Uani 0.30 1 d PD A 2 H66D H 0.1604 0.6419 0.1145 0.077 Uiso 0.30 1 calc PR A 2 H66E H 0.2769 0.5705 0.1840 0.077 Uiso 0.30 1 calc PR A 2 H66F H 0.1420 0.6745 0.2061 0.077 Uiso 0.30 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru 0.01665(10) 0.02215(11) 0.02234(11) -0.00581(8) 0.00197(7) -0.00723(8) P1 0.0184(3) 0.0265(3) 0.0253(3) -0.0035(3) 0.0005(3) -0.0093(3) P2 0.0192(3) 0.0238(3) 0.0244(3) -0.0054(3) 0.0029(3) -0.0079(3) Si 0.0227(4) 0.0235(4) 0.0359(4) -0.0097(3) 0.0043(3) -0.0095(3) C1 0.0280(13) 0.0354(15) 0.0221(13) -0.0047(11) -0.0009(10) -0.0154(12) C2 0.0333(14) 0.0329(14) 0.0218(13) -0.0077(11) 0.0036(11) -0.0163(12) C3 0.0284(14) 0.0385(15) 0.0200(13) -0.0099(11) 0.0080(11) -0.0129(12) C3A 0.0312(14) 0.0344(14) 0.0185(12) -0.0036(11) 0.0029(10) -0.0157(12) C4 0.0415(16) 0.0460(18) 0.0278(15) -0.0025(13) 0.0027(12) -0.0263(14) C5 0.069(2) 0.0400(18) 0.0379(17) -0.0029(14) -0.0023(16) -0.0351(17) C6 0.065(2) 0.0268(15) 0.0363(17) -0.0028(13) -0.0039(15) -0.0105(15) C7 0.0365(16) 0.0322(15) 0.0297(15) -0.0021(12) -0.0038(12) -0.0057(13) C7A 0.0286(13) 0.0309(14) 0.0187(12) -0.0011(10) -0.0010(10) -0.0105(11) C11 0.0198(12) 0.0270(13) 0.0359(15) -0.0051(11) 0.0011(11) -0.0071(11) C12 0.0248(14) 0.0302(15) 0.0470(17) -0.0066(13) 0.0086(12) -0.0093(12) C13 0.0365(17) 0.0413(18) 0.072(2) -0.0183(16) 0.0267(16) -0.0157(14) C14 0.0295(17) 0.0429(19) 0.109(3) -0.019(2) 0.0207(19) -0.0087(15) C15 0.0285(16) 0.0289(16) 0.088(3) -0.0058(16) -0.0008(16) -0.0032(13) C16 0.0295(15) 0.0294(15) 0.0493(18) -0.0006(13) -0.0043(13) -0.0103(12) C21 0.0252(13) 0.0349(15) 0.0281(14) -0.0100(11) 0.0007(11) -0.0123(12) C22 0.0305(14) 0.0367(15) 0.0375(16) -0.0130(13) 0.0028(12) -0.0149(12) C23 0.0394(17) 0.0423(17) 0.059(2) -0.0239(16) 0.0053(15) -0.0183(14) C24 0.048(2) 0.064(2) 0.073(3) -0.034(2) -0.0049(18) -0.0243(18) C25 0.053(2) 0.070(2) 0.047(2) -0.0198(18) -0.0177(16) -0.0179(18) C26 0.0396(17) 0.0482(18) 0.0384(17) -0.0056(14) -0.0114(13) -0.0158(14) C31 0.0192(12) 0.0283(13) 0.0291(13) -0.0036(11) 0.0046(10) -0.0096(11) C32 0.0237(13) 0.0271(13) 0.0294(14) -0.0061(11) 0.0058(11) -0.0099(11) C33 0.0267(14) 0.0358(15) 0.0343(15) -0.0036(12) 0.0012(11) -0.0175(12) C34 0.0246(14) 0.0371(16) 0.0445(17) 0.0029(13) -0.0040(12) -0.0118(12) C35 0.0279(15) 0.0291(15) 0.063(2) -0.0138(14) 0.0016(14) -0.0029(12) C36 0.0250(14) 0.0306(15) 0.0463(17) -0.0110(13) -0.0004(12) -0.0081(12) C41 0.0233(13) 0.0269(13) 0.0266(13) -0.0075(11) -0.0005(10) -0.0078(11) C42 0.0252(13) 0.0320(14) 0.0303(14) -0.0073(11) 0.0020(11) -0.0098(11) C43 0.0337(15) 0.0308(15) 0.0484(18) -0.0083(13) -0.0019(13) -0.0139(13) C44 0.0381(16) 0.0353(16) 0.0480(18) -0.0184(14) -0.0048(14) -0.0143(13) C45 0.0513(19) 0.0495(19) 0.0377(17) -0.0211(15) 0.0100(14) -0.0185(16) C46 0.0447(17) 0.0418(17) 0.0346(16) -0.0147(13) 0.0126(13) -0.0214(14) C51 0.0271(13) 0.0258(13) 0.0277(14) -0.0062(11) 0.0078(11) -0.0077(11) C52 0.0358(15) 0.0348(15) 0.0368(16) -0.0018(12) 0.0024(12) -0.0171(13) C53 0.053(2) 0.0481(19) 0.051(2) 0.0001(16) 0.0065(16) -0.0316(17) C54 0.060(2) 0.0413(18) 0.0419(18) 0.0034(14) 0.0096(16) -0.0234(16) C55 0.0430(18) 0.0483(19) 0.0330(16) 0.0028(14) -0.0012(14) -0.0144(15) C56 0.0313(15) 0.0407(16) 0.0310(15) -0.0032(12) 0.0025(12) -0.0137(13) C61 0.0257(14) 0.0310(15) 0.0574(19) -0.0145(14) 0.0062(13) -0.0131(12) C62 0.0345(17) 0.0476(19) 0.060(2) -0.0128(16) -0.0019(15) -0.0189(15) C63 0.0270(15) 0.0337(15) 0.061(2) -0.0206(14) 0.0070(14) -0.0107(12) C64 0.0378(17) 0.0419(18) 0.071(2) -0.0273(17) 0.0017(16) -0.0070(14) C65A 0.046(5) 0.0256(19) 0.049(2) -0.0027(15) 0.0010(18) -0.009(3) C66A 0.080(4) 0.042(3) 0.063(3) 0.001(2) 0.016(3) -0.023(3) C65B 0.046(5) 0.0256(19) 0.049(2) -0.0027(15) 0.0010(18) -0.009(3) C66B 0.080(4) 0.042(3) 0.063(3) 0.001(2) 0.016(3) -0.023(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru C2 2.197(2) . ? Ru C3 2.221(2) . ? Ru C1 2.246(2) . ? Ru P1 2.2790(7) . ? Ru P2 2.2802(7) . ? Ru Si 2.4108(8) . ? Ru C3A 2.428(2) . ? Ru C7A 2.437(2) . ? P1 C21 1.858(3) . ? P1 C11 1.864(3) . ? P1 H1P 1.32(3) . ? P2 C51 1.839(3) . ? P2 C41 1.840(3) . ? P2 C31 1.847(2) . ? Si C61 1.905(3) . ? Si C65B 1.915(4) . ? Si C65A 1.915(3) . ? Si C63 1.926(3) . ? C1 C2 1.408(4) . ? C1 C7A 1.434(4) . ? C2 C3 1.407(4) . ? C3 C3A 1.440(4) . ? C3A C4 1.409(4) . ? C3A C7A 1.431(4) . ? C4 C5 1.354(4) . ? C5 C6 1.402(5) . ? C6 C7 1.366(4) . ? C7 C7A 1.404(4) . ? C11 C12 1.520(4) . ? C11 C16 1.523(4) . ? C12 C13 1.531(4) . ? C13 C14 1.507(5) . ? C14 C15 1.506(4) . ? C15 C16 1.516(4) . ? C21 C22 1.523(4) . ? C21 C26 1.529(4) . ? C22 C23 1.520(4) . ? C23 C24 1.512(4) . ? C24 C25 1.515(5) . ? C25 C26 1.516(4) . ? C31 C36 1.387(4) . ? C31 C32 1.390(3) . ? C32 C33 1.379(4) . ? C33 C34 1.369(4) . ? C34 C35 1.383(4) . ? C35 C36 1.378(4) . ? C41 C42 1.381(4) . ? C41 C46 1.393(4) . ? C42 C43 1.385(4) . ? C43 C44 1.372(4) . ? C44 C45 1.366(4) . ? C45 C46 1.389(4) . ? C51 C52 1.382(4) . ? C51 C56 1.395(4) . ? C52 C53 1.393(4) . ? C53 C54 1.365(4) . ? C54 C55 1.368(4) . ? C55 C56 1.382(4) . ? C61 C62 1.506(4) . ? C63 C64 1.510(4) . ? C65A C66A 1.507(11) . ? C65B C66B 1.507(11) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 Ru C3 37.14(9) . . ? C2 Ru C1 36.92(9) . . ? C3 Ru C1 61.83(9) . . ? C2 Ru P1 128.60(7) . . ? C3 Ru P1 98.88(7) . . ? C1 Ru P1 160.27(7) . . ? C2 Ru P2 134.93(7) . . ? C3 Ru P2 156.52(7) . . ? C1 Ru P2 101.08(7) . . ? P1 Ru P2 96.05(3) . . ? C2 Ru Si 82.64(7) . . ? C3 Ru Si 102.75(7) . . ? C1 Ru Si 101.42(7) . . ? P1 Ru Si 86.27(2) . . ? P2 Ru Si 96.19(2) . . ? C2 Ru C3A 59.29(9) . . ? C3 Ru C3A 35.74(9) . . ? C1 Ru C3A 59.13(9) . . ? P1 Ru C3A 103.15(6) . . ? P2 Ru C3A 122.70(6) . . ? Si Ru C3A 137.97(6) . . ? C2 Ru C7A 59.07(9) . . ? C3 Ru C7A 59.33(9) . . ? C1 Ru C7A 35.35(9) . . ? P1 Ru C7A 132.72(6) . . ? P2 Ru C7A 97.30(6) . . ? Si Ru C7A 136.54(6) . . ? C3A Ru C7A 34.20(8) . . ? C21 P1 C11 107.96(12) . . ? C21 P1 Ru 123.23(9) . . ? C11 P1 Ru 113.48(9) . . ? C21 P1 H1P 91.3(12) . . ? C11 P1 H1P 99.9(12) . . ? Ru P1 H1P 116.8(12) . . ? C51 P2 C41 100.20(12) . . ? C51 P2 C31 101.43(11) . . ? C41 P2 C31 99.33(11) . . ? C51 P2 Ru 122.73(8) . . ? C41 P2 Ru 115.96(8) . . ? C31 P2 Ru 113.67(8) . . ? C61 Si C65B 103.3(8) . . ? C61 Si C65A 98.9(3) . . ? C61 Si C63 103.36(12) . . ? C65B Si C63 99.7(14) . . ? C65A Si C63 104.7(5) . . ? C61 Si Ru 117.90(9) . . ? C65B Si Ru 119.2(5) . . ? C65A Si Ru 119.1(2) . . ? C63 Si Ru 110.85(9) . . ? C2 C1 C7A 107.7(2) . . ? C2 C1 Ru 69.65(14) . . ? C7A C1 Ru 79.64(15) . . ? C3 C2 C1 109.2(2) . . ? C3 C2 Ru 72.37(14) . . ? C1 C2 Ru 73.43(14) . . ? C2 C3 C3A 107.5(2) . . ? C2 C3 Ru 70.48(14) . . ? C3A C3 Ru 79.98(14) . . ? C4 C3A C7A 119.3(2) . . ? C4 C3A C3 133.2(3) . . ? C7A C3A C3 107.4(2) . . ? C4 C3A Ru 131.33(18) . . ? C7A C3A Ru 73.26(14) . . ? C3 C3A Ru 64.28(13) . . ? C5 C4 C3A 119.0(3) . . ? C4 C5 C6 121.7(3) . . ? C7 C6 C5 121.1(3) . . ? C6 C7 C7A 118.8(3) . . ? C7 C7A C3A 119.9(2) . . ? C7 C7A C1 132.3(3) . . ? C3A C7A C1 107.6(2) . . ? C7 C7A Ru 131.72(18) . . ? C3A C7A Ru 72.55(14) . . ? C1 C7A Ru 65.01(14) . . ? C12 C11 C16 110.7(2) . . ? C12 C11 P1 116.44(18) . . ? C16 C11 P1 115.00(19) . . ? C11 C12 C13 110.5(2) . . ? C14 C13 C12 111.1(3) . . ? C15 C14 C13 112.1(3) . . ? C14 C15 C16 111.3(3) . . ? C15 C16 C11 111.6(3) . . ? C22 C21 C26 110.6(2) . . ? C22 C21 P1 116.37(18) . . ? C26 C21 P1 113.69(19) . . ? C23 C22 C21 111.5(2) . . ? C24 C23 C22 111.6(3) . . ? C23 C24 C25 110.7(3) . . ? C24 C25 C26 111.4(3) . . ? C25 C26 C21 111.6(3) . . ? C36 C31 C32 117.8(2) . . ? C36 C31 P2 123.3(2) . . ? C32 C31 P2 118.87(19) . . ? C33 C32 C31 121.5(2) . . ? C34 C33 C32 120.1(3) . . ? C33 C34 C35 119.3(3) . . ? C36 C35 C34 120.8(3) . . ? C35 C36 C31 120.5(3) . . ? C42 C41 C46 118.4(2) . . ? C42 C41 P2 117.44(19) . . ? C46 C41 P2 123.8(2) . . ? C41 C42 C43 121.1(3) . . ? C44 C43 C42 120.0(3) . . ? C45 C44 C43 119.8(3) . . ? C44 C45 C46 120.8(3) . . ? C45 C46 C41 120.0(3) . . ? C52 C51 C56 118.3(2) . . ? C52 C51 P2 123.1(2) . . ? C56 C51 P2 118.5(2) . . ? C51 C52 C53 120.6(3) . . ? C54 C53 C52 119.9(3) . . ? C53 C54 C55 120.6(3) . . ? C54 C55 C56 120.0(3) . . ? C55 C56 C51 120.6(3) . . ? C62 C61 Si 121.4(2) . . ? C64 C63 Si 118.6(2) . . ? C66A C65A Si 119.1(7) . . ? C66B C65B Si 119.1(7) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C2 Ru P1 C21 -128.02(13) . . . . ? C3 Ru P1 C21 -103.18(12) . . . . ? C1 Ru P1 C21 -91.6(2) . . . . ? P2 Ru P1 C21 58.64(10) . . . . ? Si Ru P1 C21 154.48(10) . . . . ? C3A Ru P1 C21 -67.00(12) . . . . ? C7A Ru P1 C21 -47.12(13) . . . . ? C2 Ru P1 C11 5.32(13) . . . . ? C3 Ru P1 C11 30.16(11) . . . . ? C1 Ru P1 C11 41.8(2) . . . . ? P2 Ru P1 C11 -168.02(9) . . . . ? Si Ru P1 C11 -72.18(9) . . . . ? C3A Ru P1 C11 66.34(11) . . . . ? C7A Ru P1 C11 86.22(12) . . . . ? P2 Ru P1 H1P -52.6(14) . . . . ? Si Ru P1 H1P 43.3(14) . . . . ? C1 Ru P1 H1P 157.2(14) . . . . ? C2 Ru P1 H1P 120.8(14) . . . . ? C3 Ru P1 H1P 145.6(14) . . . . ? C3A Ru P1 H1P -178.2(14) . . . . ? C7A Ru P1 H1P -158.3(14) . . . . ? C2 Ru P2 C51 -113.11(14) . . . . ? C3 Ru P2 C51 -171.2(2) . . . . ? C1 Ru P2 C51 -130.31(12) . . . . ? P1 Ru P2 C51 59.53(11) . . . . ? Si Ru P2 C51 -27.35(11) . . . . ? C3A Ru P2 C51 169.40(12) . . . . ? C7A Ru P2 C51 -165.94(12) . . . . ? C2 Ru P2 C41 123.72(13) . . . . ? C3 Ru P2 C41 65.7(2) . . . . ? C1 Ru P2 C41 106.53(11) . . . . ? P1 Ru P2 C41 -63.63(9) . . . . ? Si Ru P2 C41 -150.52(9) . . . . ? C3A Ru P2 C41 46.23(12) . . . . ? C7A Ru P2 C41 70.90(11) . . . . ? C2 Ru P2 C31 9.50(13) . . . . ? C3 Ru P2 C31 -48.5(2) . . . . ? C1 Ru P2 C31 -7.70(11) . . . . ? P1 Ru P2 C31 -177.85(9) . . . . ? Si Ru P2 C31 95.26(9) . . . . ? C3A Ru P2 C31 -67.99(11) . . . . ? C7A Ru P2 C31 -43.32(11) . . . . ? C2 Ru Si C61 64.20(13) . . . . ? C3 Ru Si C61 95.62(13) . . . . ? C1 Ru Si C61 32.25(13) . . . . ? P1 Ru Si C61 -166.10(11) . . . . ? P2 Ru Si C61 -70.41(11) . . . . ? C3A Ru Si C61 88.35(14) . . . . ? C7A Ru Si C61 37.05(14) . . . . ? C2 Ru Si C65B -169.4(16) . . . . ? C3 Ru Si C65B -138.0(16) . . . . ? C1 Ru Si C65B 158.6(16) . . . . ? P1 Ru Si C65B -39.7(16) . . . . ? P2 Ru Si C65B 56.0(16) . . . . ? C3A Ru Si C65B -145.3(16) . . . . ? C7A Ru Si C65B 163.4(16) . . . . ? C2 Ru Si C65A -176.1(6) . . . . ? C3 Ru Si C65A -144.7(6) . . . . ? C1 Ru Si C65A 151.9(6) . . . . ? P1 Ru Si C65A -46.4(6) . . . . ? P2 Ru Si C65A 49.3(6) . . . . ? C3A Ru Si C65A -151.9(6) . . . . ? C7A Ru Si C65A 156.8(6) . . . . ? C2 Ru Si C63 -54.58(12) . . . . ? C3 Ru Si C63 -23.16(13) . . . . ? C1 Ru Si C63 -86.53(12) . . . . ? P1 Ru Si C63 75.12(11) . . . . ? P2 Ru Si C63 170.81(10) . . . . ? C3A Ru Si C63 -30.43(14) . . . . ? C7A Ru Si C63 -81.73(14) . . . . ? C3 Ru C1 C2 -37.58(15) . . . . ? P1 Ru C1 C2 -50.6(3) . . . . ? P2 Ru C1 C2 159.61(14) . . . . ? Si Ru C1 C2 60.89(15) . . . . ? C3A Ru C1 C2 -78.77(16) . . . . ? C7A Ru C1 C2 -113.4(2) . . . . ? C2 Ru C1 C7A 113.4(2) . . . . ? C3 Ru C1 C7A 75.82(16) . . . . ? P1 Ru C1 C7A 62.8(3) . . . . ? P2 Ru C1 C7A -86.99(14) . . . . ? Si Ru C1 C7A 174.29(13) . . . . ? C3A Ru C1 C7A 34.63(14) . . . . ? C7A C1 C2 C3 -7.4(3) . . . . ? Ru C1 C2 C3 64.00(18) . . . . ? C7A C1 C2 Ru -71.36(17) . . . . ? C1 Ru C2 C3 -117.1(2) . . . . ? P1 Ru C2 C3 43.42(18) . . . . ? P2 Ru C2 C3 -145.96(13) . . . . ? Si Ru C2 C3 122.63(15) . . . . ? C3A Ru C2 C3 -38.79(15) . . . . ? C7A Ru C2 C3 -78.83(16) . . . . ? C3 Ru C2 C1 117.1(2) . . . . ? P1 Ru C2 C1 160.50(12) . . . . ? P2 Ru C2 C1 -28.88(19) . . . . ? Si Ru C2 C1 -120.29(15) . . . . ? C3A Ru C2 C1 78.29(16) . . . . ? C7A Ru C2 C1 38.25(14) . . . . ? C1 C2 C3 C3A 7.6(3) . . . . ? Ru C2 C3 C3A 72.22(17) . . . . ? C1 C2 C3 Ru -64.67(18) . . . . ? C1 Ru C3 C2 37.36(15) . . . . ? P1 Ru C3 C2 -147.06(14) . . . . ? P2 Ru C3 C2 84.1(2) . . . . ? Si Ru C3 C2 -58.91(15) . . . . ? C3A Ru C3 C2 112.7(2) . . . . ? C7A Ru C3 C2 78.06(16) . . . . ? C2 Ru C3 C3A -112.7(2) . . . . ? C1 Ru C3 C3A -75.39(16) . . . . ? P1 Ru C3 C3A 100.19(14) . . . . ? P2 Ru C3 C3A -28.7(3) . . . . ? Si Ru C3 C3A -171.66(13) . . . . ? C7A Ru C3 C3A -34.69(14) . . . . ? C2 C3 C3A C4 170.7(3) . . . . ? Ru C3 C3A C4 -123.6(3) . . . . ? C2 C3 C3A C7A -4.8(3) . . . . ? Ru C3 C3A C7A 60.93(18) . . . . ? C2 C3 C3A Ru -65.70(17) . . . . ? C2 Ru C3A C4 166.4(3) . . . . ? C3 Ru C3A C4 126.0(3) . . . . ? C1 Ru C3A C4 -150.4(3) . . . . ? P1 Ru C3A C4 39.0(3) . . . . ? P2 Ru C3A C4 -67.1(3) . . . . ? Si Ru C3A C4 138.2(2) . . . . ? C7A Ru C3A C4 -114.6(3) . . . . ? C2 Ru C3A C7A -79.06(16) . . . . ? C3 Ru C3A C7A -119.4(2) . . . . ? C1 Ru C3A C7A -35.81(14) . . . . ? P1 Ru C3A C7A 153.61(13) . . . . ? P2 Ru C3A C7A 47.44(16) . . . . ? Si Ru C3A C7A -107.22(15) . . . . ? C2 Ru C3A C3 40.37(15) . . . . ? C1 Ru C3A C3 83.62(16) . . . . ? P1 Ru C3A C3 -86.96(14) . . . . ? P2 Ru C3A C3 166.87(13) . . . . ? Si Ru C3A C3 12.21(19) . . . . ? C7A Ru C3A C3 119.4(2) . . . . ? C7A C3A C4 C5 2.6(4) . . . . ? C3 C3A C4 C5 -172.4(3) . . . . ? Ru C3A C4 C5 95.7(3) . . . . ? C3A C4 C5 C6 -2.2(4) . . . . ? C4 C5 C6 C7 -0.7(5) . . . . ? C5 C6 C7 C7A 3.2(4) . . . . ? C6 C7 C7A C3A -2.7(4) . . . . ? C6 C7 C7A C1 171.8(3) . . . . ? C6 C7 C7A Ru -95.5(3) . . . . ? C4 C3A C7A C7 -0.1(4) . . . . ? C3 C3A C7A C7 176.1(2) . . . . ? Ru C3A C7A C7 -128.6(2) . . . . ? C4 C3A C7A C1 -175.9(2) . . . . ? C3 C3A C7A C1 0.3(3) . . . . ? Ru C3A C7A C1 55.63(17) . . . . ? C4 C3A C7A Ru 128.5(2) . . . . ? C3 C3A C7A Ru -55.31(16) . . . . ? C2 C1 C7A C7 -170.8(3) . . . . ? Ru C1 C7A C7 124.7(3) . . . . ? C2 C1 C7A C3A 4.3(3) . . . . ? Ru C1 C7A C3A -60.31(18) . . . . ? C2 C1 C7A Ru 64.58(17) . . . . ? C2 Ru C7A C7 -165.4(3) . . . . ? C3 Ru C7A C7 151.1(3) . . . . ? C1 Ru C7A C7 -125.4(3) . . . . ? P1 Ru C7A C7 78.7(3) . . . . ? P2 Ru C7A C7 -26.5(3) . . . . ? Si Ru C7A C7 -133.6(2) . . . . ? C3A Ru C7A C7 114.8(3) . . . . ? C2 Ru C7A C3A 79.79(16) . . . . ? C3 Ru C7A C3A 36.26(15) . . . . ? C1 Ru C7A C3A 119.8(2) . . . . ? P1 Ru C7A C3A -36.10(18) . . . . ? P2 Ru C7A C3A -141.33(14) . . . . ? Si Ru C7A C3A 111.63(14) . . . . ? C2 Ru C7A C1 -40.00(15) . . . . ? C3 Ru C7A C1 -83.52(16) . . . . ? P1 Ru C7A C1 -155.88(12) . . . . ? P2 Ru C7A C1 98.89(14) . . . . ? Si Ru C7A C1 -8.16(19) . . . . ? C3A Ru C7A C1 -119.8(2) . . . . ? H1P P1 C11 C12 140.8(12) . . . . ? H1P P1 C11 C16 9.0(13) . . . . ? C21 P1 C11 C12 46.1(2) . . . . ? Ru P1 C11 C12 -94.1(2) . . . . ? C21 P1 C11 C16 -85.7(2) . . . . ? Ru P1 C11 C16 134.06(18) . . . . ? C16 C11 C12 C13 -56.3(3) . . . . ? P1 C11 C12 C13 170.0(2) . . . . ? C11 C12 C13 C14 56.1(4) . . . . ? C12 C13 C14 C15 -55.3(4) . . . . ? C13 C14 C15 C16 54.4(4) . . . . ? C14 C15 C16 C11 -54.6(4) . . . . ? C12 C11 C16 C15 55.9(3) . . . . ? P1 C11 C16 C15 -169.6(2) . . . . ? H1P P1 C21 C22 -175.8(12) . . . . ? H1P P1 C21 C26 -45.5(12) . . . . ? C11 P1 C21 C22 -74.9(2) . . . . ? Ru P1 C21 C22 60.5(2) . . . . ? C11 P1 C21 C26 55.4(2) . . . . ? Ru P1 C21 C26 -169.13(17) . . . . ? C26 C21 C22 C23 54.2(3) . . . . ? P1 C21 C22 C23 -174.04(19) . . . . ? C21 C22 C23 C24 -55.7(3) . . . . ? C22 C23 C24 C25 56.2(4) . . . . ? C23 C24 C25 C26 -56.3(4) . . . . ? C24 C25 C26 C21 55.8(4) . . . . ? C22 C21 C26 C25 -54.4(3) . . . . ? P1 C21 C26 C25 172.4(2) . . . . ? C51 P2 C31 C36 -99.5(2) . . . . ? C41 P2 C31 C36 3.0(2) . . . . ? Ru P2 C31 C36 126.8(2) . . . . ? C51 P2 C31 C32 82.4(2) . . . . ? C41 P2 C31 C32 -175.1(2) . . . . ? Ru P2 C31 C32 -51.3(2) . . . . ? C36 C31 C32 C33 0.7(4) . . . . ? P2 C31 C32 C33 179.0(2) . . . . ? C31 C32 C33 C34 -0.6(4) . . . . ? C32 C33 C34 C35 0.0(4) . . . . ? C33 C34 C35 C36 0.6(5) . . . . ? C34 C35 C36 C31 -0.5(5) . . . . ? C32 C31 C36 C35 -0.1(4) . . . . ? P2 C31 C36 C35 -178.3(2) . . . . ? C51 P2 C41 C42 -161.9(2) . . . . ? C31 P2 C41 C42 94.6(2) . . . . ? Ru P2 C41 C42 -27.6(2) . . . . ? C51 P2 C41 C46 25.2(3) . . . . ? C31 P2 C41 C46 -78.3(2) . . . . ? Ru P2 C41 C46 159.5(2) . . . . ? C46 C41 C42 C43 1.7(4) . . . . ? P2 C41 C42 C43 -171.6(2) . . . . ? C41 C42 C43 C44 -1.0(4) . . . . ? C42 C43 C44 C45 -0.7(4) . . . . ? C43 C44 C45 C46 1.7(5) . . . . ? C44 C45 C46 C41 -0.9(5) . . . . ? C42 C41 C46 C45 -0.8(4) . . . . ? P2 C41 C46 C45 172.0(2) . . . . ? C41 P2 C51 C52 -126.5(2) . . . . ? C31 P2 C51 C52 -24.7(2) . . . . ? Ru P2 C51 C52 103.3(2) . . . . ? C41 P2 C51 C56 56.3(2) . . . . ? C31 P2 C51 C56 158.1(2) . . . . ? Ru P2 C51 C56 -73.8(2) . . . . ? C56 C51 C52 C53 1.3(4) . . . . ? P2 C51 C52 C53 -175.8(2) . . . . ? C51 C52 C53 C54 -0.3(5) . . . . ? C52 C53 C54 C55 -0.7(5) . . . . ? C53 C54 C55 C56 0.7(5) . . . . ? C54 C55 C56 C51 0.3(5) . . . . ? C52 C51 C56 C55 -1.3(4) . . . . ? P2 C51 C56 C55 175.9(2) . . . . ? C65B Si C61 C62 167.0(13) . . . . ? C65A Si C61 C62 171.0(5) . . . . ? C63 Si C61 C62 63.4(3) . . . . ? Ru Si C61 C62 -59.3(3) . . . . ? C61 Si C63 C64 24.4(3) . . . . ? C65B Si C63 C64 -81.9(5) . . . . ? C65A Si C63 C64 -78.8(3) . . . . ? Ru Si C63 C64 151.6(2) . . . . ? C61 Si C65A C66A -76.6(10) . . . . ? C63 Si C65A C66A 29.9(9) . . . . ? Ru Si C65A C66A 154.4(6) . . . . ? C61 Si C65B C66B -17(3) . . . . ? C63 Si C65B C66B 90(3) . . . . ? Ru Si C65B C66B -150(2) . . . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 26.28 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.483 _refine_diff_density_min -0.463 _refine_diff_density_rms 0.079 #===END