Supplementary Material (ESI) for Chemical Communications This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_coden_Cambridge 182 _journal_volume ? _journal_page_first ? _journal_year ? loop_ _publ_author_name 'Lisa Rosenberg' 'Eric J. Derrah' 'Robert McDonald' _publ_contact_author_name 'Lisa Rosenberg' _publ_contact_author_email LISAROSE@UVIC.CA _publ_section_title ; The [2+2] Cycloaddition of Alkynes at a Ru-P pi-Bond ; # Attachment 'lrcc0.cif' data_2a _database_code_depnum_ccdc_archive 'CCDC 765663' #TrackingRef 'lrcc0.cif' _vrf_PLAT331_2a ; RESPONSE: This error refers to the solvent benzene molecule, which is located upon the inversion center [0, 0, 1/2] and appears to possess a small degree of rotational and translational disorder. Splitting the atoms to model the disorder created more problems than it solved (a much greater range of bond lengths and angles, wildly diverging displacement parameters due to correlation effects) so the molecule was left in the present form. ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C47 H50 P2 Ru, 0.5(C6 H6)' _chemical_formula_sum 'C50 H53 P2 Ru' _chemical_formula_weight 816.93 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/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.1439(9) _cell_length_b 20.4714(18) _cell_length_c 19.6785(18) _cell_angle_alpha 90.00 _cell_angle_beta 104.5062(14) _cell_angle_gamma 90.00 _cell_volume 3956.2(6) _cell_formula_units_Z 4 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 5520 _cell_measurement_theta_min 2.26 _cell_measurement_theta_max 26.35 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.53 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.372 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1708 _exptl_absorpt_coefficient_mu 0.512 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7729 _exptl_absorpt_correction_T_max 0.9271 _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 30708 _diffrn_reflns_av_R_equivalents 0.0373 _diffrn_reflns_av_sigmaI/netI 0.0305 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.46 _diffrn_reflns_theta_max 26.40 _reflns_number_total 8114 _reflns_number_gt 6898 _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^)+(0.0432P)^2^+2.2972P] 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 8114 _refine_ls_number_parameters 478 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0391 _refine_ls_R_factor_gt 0.0302 _refine_ls_wR_factor_ref 0.0832 _refine_ls_wR_factor_gt 0.0767 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.051 _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 0.239025(16) 0.156059(8) 0.215513(8) 0.01752(6) Uani 1 1 d . . . P1 P 0.22015(5) 0.06932(3) 0.13682(3) 0.01849(12) Uani 1 1 d . . . P2 P 0.17755(5) 0.09089(3) 0.29756(3) 0.01843(12) Uani 1 1 d . . . C1 C 0.3603(2) 0.23112(11) 0.17531(12) 0.0277(5) Uani 1 1 d . . . H1 H 0.3746 0.2328 0.1269 0.033 Uiso 1 1 calc R . . C2 C 0.2540(3) 0.26216(11) 0.19773(13) 0.0295(5) Uani 1 1 d . . . H2 H 0.1809 0.2897 0.1675 0.035 Uiso 1 1 calc R . . C3 C 0.2735(2) 0.25255(11) 0.27098(12) 0.0276(5) Uani 1 1 d . . . H3 H 0.2164 0.2716 0.3007 0.033 Uiso 1 1 calc R . . C3A C 0.4015(2) 0.21919(10) 0.29629(12) 0.0246(5) Uani 1 1 d . . . C4 C 0.4764(2) 0.20117(11) 0.36440(12) 0.0284(5) Uani 1 1 d . . . H4 H 0.4433 0.2114 0.4042 0.034 Uiso 1 1 calc R . . C5 C 0.5969(2) 0.16895(12) 0.37217(13) 0.0318(5) Uani 1 1 d . . . H5 H 0.6470 0.1562 0.4178 0.038 Uiso 1 1 calc R . . C6 C 0.6487(2) 0.15412(12) 0.31372(14) 0.0322(5) Uani 1 1 d . . . H6 H 0.7325 0.1312 0.3208 0.039 Uiso 1 1 calc R . . C7 C 0.5808(2) 0.17201(11) 0.24710(13) 0.0283(5) Uani 1 1 d . . . H7 H 0.6175 0.1622 0.2084 0.034 Uiso 1 1 calc R . . C7A C 0.4554(2) 0.20534(10) 0.23684(12) 0.0248(5) Uani 1 1 d . . . C8 C 0.0498(2) 0.14731(10) 0.14621(11) 0.0208(4) Uani 1 1 d . . . C9 C 0.0446(2) 0.09115(10) 0.10995(11) 0.0220(4) Uani 1 1 d . . . H9 H -0.0301 0.0697 0.0793 0.026 Uiso 1 1 calc R . . C11 C -0.0656(2) 0.19442(10) 0.13266(11) 0.0228(4) Uani 1 1 d . . . C12 C -0.1585(2) 0.19670(12) 0.06667(13) 0.0315(5) Uani 1 1 d . . . H12 H -0.1465 0.1683 0.0305 0.038 Uiso 1 1 calc R . . C13 C -0.2671(3) 0.23945(13) 0.05337(15) 0.0421(7) Uani 1 1 d . . . H13 H -0.3280 0.2406 0.0080 0.051 Uiso 1 1 calc R . . C14 C -0.2884(3) 0.28048(14) 0.10520(16) 0.0453(7) Uani 1 1 d . . . H14 H -0.3650 0.3088 0.0962 0.054 Uiso 1 1 calc R . . C15 C -0.1967(3) 0.27995(13) 0.17035(15) 0.0405(6) Uani 1 1 d . . . H15 H -0.2097 0.3086 0.2061 0.049 Uiso 1 1 calc R . . C16 C -0.0856(2) 0.23769(11) 0.18394(13) 0.0308(5) Uani 1 1 d . . . H16 H -0.0227 0.2383 0.2287 0.037 Uiso 1 1 calc R . . C21 C 0.2843(2) 0.07626(10) 0.05611(11) 0.0235(5) Uani 1 1 d . . . H21 H 0.2654 0.0338 0.0304 0.028 Uiso 1 1 calc R . . C22 C 0.4382(2) 0.08823(12) 0.07217(12) 0.0285(5) Uani 1 1 d . . . H22A H 0.4608 0.1287 0.1003 0.034 Uiso 1 1 calc R . . H22B H 0.4866 0.0515 0.1004 0.034 Uiso 1 1 calc R . . C23 C 0.4865(3) 0.09475(13) 0.00472(15) 0.0393(6) Uani 1 1 d . . . H23A H 0.5853 0.1045 0.0169 0.047 Uiso 1 1 calc R . . H23B H 0.4720 0.0529 -0.0212 0.047 Uiso 1 1 calc R . . C24 C 0.4098(3) 0.14897(14) -0.04196(15) 0.0431(7) Uani 1 1 d . . . H24A H 0.4308 0.1915 -0.0177 0.052 Uiso 1 1 calc R . . H24B H 0.4399 0.1509 -0.0860 0.052 Uiso 1 1 calc R . . C25 C 0.2573(3) 0.13686(15) -0.05895(13) 0.0416(6) Uani 1 1 d . . . H25A H 0.2356 0.0967 -0.0875 0.050 Uiso 1 1 calc R . . H25B H 0.2092 0.1738 -0.0871 0.050 Uiso 1 1 calc R . . C26 C 0.2070(3) 0.12953(12) 0.00741(12) 0.0293(5) Uani 1 1 d . . . H26A H 0.1088 0.1187 -0.0058 0.035 Uiso 1 1 calc R . . H26B H 0.2181 0.1717 0.0329 0.035 Uiso 1 1 calc R . . C31 C 0.2389(2) -0.01876(10) 0.15880(11) 0.0202(4) Uani 1 1 d . . . H31 H 0.2230 -0.0230 0.2067 0.024 Uiso 1 1 calc R . . C32 C 0.3806(2) -0.04764(10) 0.16403(12) 0.0234(5) Uani 1 1 d . . . H32A H 0.3993 -0.0479 0.1170 0.028 Uiso 1 1 calc R . . H32B H 0.4505 -0.0202 0.1954 0.028 Uiso 1 1 calc R . . C33 C 0.3883(2) -0.11744(11) 0.19282(13) 0.0293(5) Uani 1 1 d . . . H33A H 0.4797 -0.1358 0.1954 0.035 Uiso 1 1 calc R . . H33B H 0.3747 -0.1167 0.2409 0.035 Uiso 1 1 calc R . . C34 C 0.2804(3) -0.16062(11) 0.14621(14) 0.0331(6) Uani 1 1 d . . . H34A H 0.2831 -0.2045 0.1676 0.040 Uiso 1 1 calc R . . H34B H 0.3007 -0.1656 0.0998 0.040 Uiso 1 1 calc R . . C35 C 0.1380(3) -0.13169(11) 0.13631(14) 0.0329(5) Uani 1 1 d . . . H35A H 0.0720 -0.1586 0.1020 0.039 Uiso 1 1 calc R . . H35B H 0.1121 -0.1333 0.1815 0.039 Uiso 1 1 calc R . . C36 C 0.1300(2) -0.06121(11) 0.11042(13) 0.0287(5) Uani 1 1 d . . . H36A H 0.0386 -0.0433 0.1088 0.034 Uiso 1 1 calc R . . H36B H 0.1430 -0.0601 0.0622 0.034 Uiso 1 1 calc R . . C41 C 0.1415(2) 0.13602(10) 0.37277(11) 0.0219(4) Uani 1 1 d . . . C42 C 0.2373(2) 0.14093(11) 0.43686(12) 0.0278(5) Uani 1 1 d . . . H42 H 0.3227 0.1196 0.4432 0.033 Uiso 1 1 calc R . . C43 C 0.2099(3) 0.17674(13) 0.49186(13) 0.0364(6) Uani 1 1 d . . . H43 H 0.2772 0.1802 0.5351 0.044 Uiso 1 1 calc R . . C44 C 0.0861(3) 0.20719(12) 0.48411(14) 0.0372(6) Uani 1 1 d . . . H44 H 0.0668 0.2308 0.5221 0.045 Uiso 1 1 calc R . . C45 C -0.0094(3) 0.20311(12) 0.42092(14) 0.0341(6) Uani 1 1 d . . . H45 H -0.0951 0.2240 0.4152 0.041 Uiso 1 1 calc R . . C46 C 0.0182(2) 0.16870(11) 0.36540(12) 0.0271(5) Uani 1 1 d . . . H46 H -0.0479 0.1674 0.3217 0.033 Uiso 1 1 calc R . . C51 C 0.3129(2) 0.03513(10) 0.34410(11) 0.0212(4) Uani 1 1 d . . . C52 C 0.4320(2) 0.03103(11) 0.32154(11) 0.0243(5) Uani 1 1 d . . . H52 H 0.4424 0.0573 0.2834 0.029 Uiso 1 1 calc R . . C53 C 0.5355(3) -0.01097(13) 0.35411(13) 0.0357(6) Uani 1 1 d . . . H53 H 0.6163 -0.0136 0.3381 0.043 Uiso 1 1 calc R . . C54 C 0.5220(3) -0.04895(13) 0.40966(14) 0.0420(7) Uani 1 1 d . . . H54 H 0.5925 -0.0783 0.4314 0.050 Uiso 1 1 calc R . . C55 C 0.4055(3) -0.04430(12) 0.43366(13) 0.0376(6) Uani 1 1 d . . . H55 H 0.3968 -0.0699 0.4726 0.045 Uiso 1 1 calc R . . C56 C 0.3017(3) -0.00259(11) 0.40122(12) 0.0293(5) Uani 1 1 d . . . H56 H 0.2219 0.0004 0.4181 0.035 Uiso 1 1 calc R . . C61 C 0.0291(2) 0.03485(11) 0.27282(11) 0.0228(4) Uani 1 1 d . . . C62 C -0.0986(2) 0.05997(12) 0.23955(12) 0.0280(5) Uani 1 1 d . . . H62 H -0.1079 0.1054 0.2298 0.034 Uiso 1 1 calc R . . C63 C -0.2124(2) 0.02007(14) 0.22039(13) 0.0356(6) Uani 1 1 d . . . H63 H -0.2989 0.0386 0.1992 0.043 Uiso 1 1 calc R . . C64 C -0.2005(3) -0.04641(14) 0.23204(14) 0.0398(6) Uani 1 1 d . . . H64 H -0.2786 -0.0737 0.2192 0.048 Uiso 1 1 calc R . . C65 C -0.0748(3) -0.07293(13) 0.26247(14) 0.0374(6) Uani 1 1 d . . . H65 H -0.0656 -0.1188 0.2697 0.045 Uiso 1 1 calc R . . C66 C 0.0394(2) -0.03256(11) 0.28278(12) 0.0289(5) Uani 1 1 d . . . H66 H 0.1255 -0.0514 0.3038 0.035 Uiso 1 1 calc R . . C1S C 0.1032(5) -0.0376(3) 0.5354(3) 0.0932(15) Uani 1 1 d . . . H1S H 0.1766 -0.0644 0.5596 0.112 Uiso 1 1 calc R . . C2S C 0.0246(6) -0.0572(3) 0.4709(3) 0.1050(17) Uani 1 1 d . . . H2S H 0.0402 -0.0975 0.4502 0.126 Uiso 1 1 calc R . . C3S C -0.0794(5) -0.0146(4) 0.4376(3) 0.1012(17) Uani 1 1 d . . . H3S H -0.1340 -0.0259 0.3925 0.121 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 0.01858(10) 0.01571(9) 0.01832(10) -0.00046(6) 0.00470(7) 0.00082(6) P1 0.0200(3) 0.0176(3) 0.0181(3) -0.0002(2) 0.0052(2) 0.0016(2) P2 0.0168(3) 0.0199(3) 0.0186(3) -0.0008(2) 0.0044(2) 0.0002(2) C1 0.0342(13) 0.0206(11) 0.0288(12) 0.0026(9) 0.0089(10) -0.0058(9) C2 0.0348(13) 0.0162(11) 0.0362(13) 0.0026(9) 0.0065(10) 0.0009(9) C3 0.0315(13) 0.0185(11) 0.0331(13) -0.0061(9) 0.0085(10) 0.0001(9) C3A 0.0264(11) 0.0178(10) 0.0309(12) -0.0041(9) 0.0094(9) -0.0062(9) C4 0.0317(13) 0.0261(12) 0.0267(12) -0.0074(9) 0.0062(10) -0.0082(10) C5 0.0264(12) 0.0334(13) 0.0306(13) -0.0031(10) -0.0022(10) -0.0068(10) C6 0.0187(11) 0.0334(13) 0.0433(14) -0.0065(11) 0.0054(10) -0.0036(10) C7 0.0233(11) 0.0289(12) 0.0349(13) -0.0056(10) 0.0113(10) -0.0079(9) C7A 0.0264(12) 0.0195(11) 0.0292(12) -0.0028(9) 0.0084(9) -0.0066(9) C8 0.0211(11) 0.0237(11) 0.0181(10) 0.0034(8) 0.0055(8) 0.0021(8) C9 0.0197(10) 0.0247(11) 0.0209(10) -0.0018(8) 0.0038(8) 0.0016(9) C11 0.0216(11) 0.0213(11) 0.0262(11) 0.0036(9) 0.0070(9) 0.0023(9) C12 0.0310(13) 0.0305(13) 0.0307(12) 0.0019(10) 0.0037(10) 0.0052(10) C13 0.0331(14) 0.0392(15) 0.0466(16) 0.0085(12) -0.0039(12) 0.0096(11) C14 0.0337(15) 0.0346(15) 0.0651(19) 0.0053(13) 0.0076(13) 0.0158(12) C15 0.0399(15) 0.0327(14) 0.0518(16) -0.0047(12) 0.0167(13) 0.0119(12) C16 0.0309(13) 0.0278(12) 0.0333(13) -0.0004(10) 0.0074(10) 0.0059(10) C21 0.0298(12) 0.0212(11) 0.0212(11) -0.0004(8) 0.0096(9) 0.0003(9) C22 0.0297(12) 0.0286(12) 0.0303(12) 0.0029(10) 0.0134(10) 0.0027(10) C23 0.0453(16) 0.0333(14) 0.0494(16) 0.0073(12) 0.0308(13) 0.0054(12) C24 0.0554(18) 0.0406(15) 0.0430(16) 0.0130(12) 0.0304(14) 0.0045(13) C25 0.0548(18) 0.0465(16) 0.0260(13) 0.0116(11) 0.0151(12) 0.0045(13) C26 0.0330(13) 0.0324(13) 0.0230(11) 0.0052(10) 0.0078(10) 0.0027(10) C31 0.0225(11) 0.0186(10) 0.0197(10) -0.0009(8) 0.0061(8) 0.0005(8) C32 0.0244(11) 0.0222(11) 0.0245(11) -0.0010(8) 0.0076(9) 0.0026(9) C33 0.0279(12) 0.0250(12) 0.0351(13) 0.0035(10) 0.0081(10) 0.0052(9) C34 0.0410(14) 0.0193(11) 0.0379(14) -0.0007(10) 0.0078(11) 0.0054(10) C35 0.0331(13) 0.0210(11) 0.0416(14) -0.0023(10) 0.0038(11) -0.0041(10) C36 0.0285(12) 0.0206(11) 0.0325(13) -0.0015(9) -0.0011(10) -0.0006(9) C41 0.0243(11) 0.0198(10) 0.0230(11) -0.0011(8) 0.0087(9) -0.0015(9) C42 0.0272(12) 0.0278(12) 0.0272(12) -0.0034(9) 0.0044(9) 0.0035(9) C43 0.0433(15) 0.0374(14) 0.0252(12) -0.0084(10) 0.0022(11) 0.0029(12) C44 0.0470(16) 0.0330(14) 0.0342(14) -0.0096(11) 0.0151(12) 0.0027(12) C45 0.0334(13) 0.0295(13) 0.0418(14) -0.0046(11) 0.0139(11) 0.0057(10) C46 0.0256(12) 0.0280(12) 0.0276(12) -0.0011(9) 0.0065(9) 0.0027(9) C51 0.0223(11) 0.0177(10) 0.0211(10) -0.0008(8) 0.0011(8) 0.0004(8) C52 0.0235(11) 0.0251(11) 0.0226(11) -0.0015(9) 0.0025(9) 0.0004(9) C53 0.0281(13) 0.0413(15) 0.0347(14) -0.0034(11) 0.0019(10) 0.0111(11) C54 0.0452(16) 0.0381(15) 0.0351(14) 0.0012(11) -0.0041(12) 0.0200(12) C55 0.0532(17) 0.0292(13) 0.0262(13) 0.0062(10) 0.0022(11) 0.0051(12) C56 0.0346(13) 0.0283(12) 0.0249(12) -0.0001(9) 0.0073(10) -0.0022(10) C61 0.0216(11) 0.0289(12) 0.0203(10) -0.0044(9) 0.0097(8) -0.0052(9) C62 0.0251(12) 0.0337(13) 0.0256(12) -0.0024(9) 0.0074(9) -0.0019(10) C63 0.0199(12) 0.0495(16) 0.0369(14) -0.0097(12) 0.0058(10) -0.0057(11) C64 0.0285(13) 0.0466(16) 0.0468(16) -0.0166(13) 0.0141(12) -0.0169(12) C65 0.0389(15) 0.0293(13) 0.0474(16) -0.0087(11) 0.0174(12) -0.0119(11) C66 0.0264(12) 0.0297(12) 0.0327(13) -0.0050(10) 0.0111(10) -0.0037(10) C1S 0.088(3) 0.129(5) 0.072(3) 0.031(3) 0.037(3) 0.018(3) C2S 0.106(4) 0.101(4) 0.131(5) 0.011(3) 0.073(4) -0.022(3) C3S 0.056(3) 0.170(6) 0.081(3) -0.003(4) 0.024(2) -0.005(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 C8 2.065(2) . ? Ru C2 2.211(2) . ? Ru C1 2.234(2) . ? Ru C3 2.241(2) . ? Ru P2 2.2978(6) . ? Ru P1 2.3323(6) . ? Ru C7A 2.356(2) . ? Ru C3A 2.367(2) . ? P1 C9 1.783(2) . ? P1 C31 1.853(2) . ? P1 C21 1.866(2) . ? P2 C51 1.843(2) . ? P2 C41 1.857(2) . ? P2 C61 1.858(2) . ? C1 C2 1.414(3) . ? C1 C7A 1.446(3) . ? C2 C3 1.419(3) . ? C3 C3A 1.441(3) . ? C3A C4 1.414(3) . ? C3A C7A 1.439(3) . ? C4 C5 1.363(3) . ? C5 C6 1.412(4) . ? C6 C7 1.369(4) . ? C7 C7A 1.413(3) . ? C8 C9 1.347(3) . ? C8 C11 1.488(3) . ? C11 C16 1.395(3) . ? C11 C12 1.401(3) . ? C12 C13 1.380(3) . ? C13 C14 1.379(4) . ? C14 C15 1.382(4) . ? C15 C16 1.392(3) . ? C21 C26 1.532(3) . ? C21 C22 1.533(3) . ? C22 C23 1.532(3) . ? C23 C24 1.524(4) . ? C24 C25 1.518(4) . ? C25 C26 1.524(3) . ? C31 C32 1.533(3) . ? C31 C36 1.535(3) . ? C32 C33 1.532(3) . ? C33 C34 1.522(3) . ? C34 C35 1.527(4) . ? C35 C36 1.525(3) . ? C41 C42 1.390(3) . ? C41 C46 1.393(3) . ? C42 C43 1.392(3) . ? C43 C44 1.376(4) . ? C44 C45 1.374(4) . ? C45 C46 1.386(3) . ? C51 C52 1.390(3) . ? C51 C56 1.392(3) . ? C52 C53 1.384(3) . ? C53 C54 1.376(4) . ? C54 C55 1.381(4) . ? C55 C56 1.382(3) . ? C61 C66 1.394(3) . ? C61 C62 1.396(3) . ? C62 C63 1.387(3) . ? C63 C64 1.381(4) . ? C64 C65 1.378(4) . ? C65 C66 1.397(3) . ? C1S C3S 1.243(7) 3_556 ? C1S C2S 1.379(7) . ? C2S C3S 1.400(7) . ? C3S C1S 1.244(7) 3_556 ? 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 C8 Ru C2 94.01(9) . . ? C8 Ru C1 109.22(8) . . ? C2 Ru C1 37.11(9) . . ? C8 Ru C3 113.82(8) . . ? C2 Ru C3 37.15(9) . . ? C1 Ru C3 62.20(9) . . ? C8 Ru P2 92.45(6) . . ? C2 Ru P2 136.30(7) . . ? C1 Ru P2 156.76(6) . . ? C3 Ru P2 101.90(6) . . ? C8 Ru P1 65.63(6) . . ? C2 Ru P1 129.81(7) . . ? C1 Ru P1 104.45(6) . . ? C3 Ru P1 166.20(6) . . ? P2 Ru P1 91.89(2) . . ? C8 Ru C7A 145.60(8) . . ? C2 Ru C7A 60.65(8) . . ? C1 Ru C7A 36.59(8) . . ? C3 Ru C7A 60.73(8) . . ? P2 Ru C7A 121.88(6) . . ? P1 Ru C7A 111.23(6) . . ? C8 Ru C3A 150.06(8) . . ? C2 Ru C3A 60.40(8) . . ? C1 Ru C3A 60.62(8) . . ? C3 Ru C3A 36.31(8) . . ? P2 Ru C3A 96.37(6) . . ? P1 Ru C3A 142.12(6) . . ? C7A Ru C3A 35.47(7) . . ? C9 P1 C31 110.48(10) . . ? C9 P1 C21 105.29(10) . . ? C31 P1 C21 103.61(10) . . ? C9 P1 Ru 85.17(7) . . ? C31 P1 Ru 126.82(7) . . ? C21 P1 Ru 121.26(7) . . ? C51 P2 C41 100.55(10) . . ? C51 P2 C61 101.63(10) . . ? C41 P2 C61 101.97(10) . . ? C51 P2 Ru 114.16(7) . . ? C41 P2 Ru 114.42(7) . . ? C61 P2 Ru 121.27(7) . . ? C2 C1 C7A 107.7(2) . . ? C2 C1 Ru 70.59(13) . . ? C7A C1 Ru 76.32(12) . . ? C1 C2 C3 109.3(2) . . ? C1 C2 Ru 72.30(13) . . ? C3 C2 Ru 72.57(13) . . ? C2 C3 C3A 107.5(2) . . ? C2 C3 Ru 70.27(12) . . ? C3A C3 Ru 76.58(13) . . ? C4 C3A C7A 119.7(2) . . ? C4 C3A C3 132.5(2) . . ? C7A C3A C3 107.8(2) . . ? C4 C3A Ru 127.79(15) . . ? C7A C3A Ru 71.88(12) . . ? C3 C3A Ru 67.11(12) . . ? C5 C4 C3A 119.1(2) . . ? C4 C5 C6 121.2(2) . . ? C7 C6 C5 121.5(2) . . ? C6 C7 C7A 119.0(2) . . ? C7 C7A C3A 119.4(2) . . ? C7 C7A C1 133.2(2) . . ? C3A C7A C1 107.4(2) . . ? C7 C7A Ru 125.73(15) . . ? C3A C7A Ru 72.66(12) . . ? C1 C7A Ru 67.08(12) . . ? C9 C8 C11 122.2(2) . . ? C9 C8 Ru 109.30(15) . . ? C11 C8 Ru 128.42(15) . . ? C8 C9 P1 98.80(15) . . ? C16 C11 C12 117.6(2) . . ? C16 C11 C8 122.2(2) . . ? C12 C11 C8 120.2(2) . . ? C13 C12 C11 121.1(2) . . ? C14 C13 C12 120.7(3) . . ? C13 C14 C15 119.2(2) . . ? C14 C15 C16 120.5(2) . . ? C15 C16 C11 120.9(2) . . ? C26 C21 C22 110.50(19) . . ? C26 C21 P1 110.73(15) . . ? C22 C21 P1 113.00(15) . . ? C23 C22 C21 111.5(2) . . ? C24 C23 C22 111.1(2) . . ? C25 C24 C23 110.6(2) . . ? C24 C25 C26 111.6(2) . . ? C25 C26 C21 112.2(2) . . ? C32 C31 C36 109.90(17) . . ? C32 C31 P1 115.52(15) . . ? C36 C31 P1 112.97(15) . . ? C33 C32 C31 110.17(18) . . ? C34 C33 C32 110.87(19) . . ? C33 C34 C35 111.45(19) . . ? C36 C35 C34 112.3(2) . . ? C35 C36 C31 111.00(18) . . ? C42 C41 C46 117.7(2) . . ? C42 C41 P2 121.74(17) . . ? C46 C41 P2 120.45(17) . . ? C41 C42 C43 120.9(2) . . ? C44 C43 C42 120.5(2) . . ? C45 C44 C43 119.3(2) . . ? C44 C45 C46 120.5(2) . . ? C45 C46 C41 121.0(2) . . ? C52 C51 C56 118.5(2) . . ? C52 C51 P2 118.52(16) . . ? C56 C51 P2 122.94(17) . . ? C53 C52 C51 120.6(2) . . ? C54 C53 C52 120.2(2) . . ? C53 C54 C55 119.8(2) . . ? C54 C55 C56 120.2(2) . . ? C55 C56 C51 120.6(2) . . ? C66 C61 C62 117.3(2) . . ? C66 C61 P2 123.20(17) . . ? C62 C61 P2 119.46(17) . . ? C63 C62 C61 121.5(2) . . ? C64 C63 C62 120.2(2) . . ? C65 C64 C63 119.6(2) . . ? C64 C65 C66 120.1(2) . . ? C61 C66 C65 121.2(2) . . ? C3S C1S C2S 120.9(6) 3_556 . ? C1S C2S C3S 116.4(5) . . ? C1S C3S C2S 122.7(6) 3_556 . ? 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 C8 Ru P1 C9 -5.87(9) . . . . ? C2 Ru P1 C9 -79.75(11) . . . . ? C1 Ru P1 C9 -110.73(10) . . . . ? C3 Ru P1 C9 -96.7(3) . . . . ? P2 Ru P1 C9 85.96(7) . . . . ? C7A Ru P1 C9 -148.60(9) . . . . ? C3A Ru P1 C9 -171.14(11) . . . . ? C8 Ru P1 C31 -117.91(11) . . . . ? C2 Ru P1 C31 168.20(12) . . . . ? C1 Ru P1 C31 137.23(11) . . . . ? C3 Ru P1 C31 151.3(3) . . . . ? P2 Ru P1 C31 -26.08(9) . . . . ? C7A Ru P1 C31 99.35(11) . . . . ? C3A Ru P1 C31 76.82(13) . . . . ? C8 Ru P1 C21 99.10(11) . . . . ? C2 Ru P1 C21 25.22(12) . . . . ? C1 Ru P1 C21 -5.76(11) . . . . ? C3 Ru P1 C21 8.3(3) . . . . ? P2 Ru P1 C21 -169.06(9) . . . . ? C7A Ru P1 C21 -43.63(10) . . . . ? C3A Ru P1 C21 -66.17(12) . . . . ? C8 Ru P2 C51 141.20(9) . . . . ? C2 Ru P2 C51 -120.40(12) . . . . ? C1 Ru P2 C51 -59.65(18) . . . . ? C3 Ru P2 C51 -103.83(10) . . . . ? P1 Ru P2 C51 75.52(7) . . . . ? C7A Ru P2 C51 -41.04(10) . . . . ? C3A Ru P2 C51 -67.45(9) . . . . ? C8 Ru P2 C41 -103.71(10) . . . . ? C2 Ru P2 C41 -5.31(12) . . . . ? C1 Ru P2 C41 55.44(18) . . . . ? C3 Ru P2 C41 11.26(10) . . . . ? P1 Ru P2 C41 -169.39(8) . . . . ? C7A Ru P2 C41 74.05(10) . . . . ? C3A Ru P2 C41 47.64(10) . . . . ? C8 Ru P2 C61 19.13(10) . . . . ? C2 Ru P2 C61 117.53(12) . . . . ? C1 Ru P2 C61 178.28(18) . . . . ? C3 Ru P2 C61 134.10(10) . . . . ? P1 Ru P2 C61 -46.55(9) . . . . ? C7A Ru P2 C61 -163.12(10) . . . . ? C3A Ru P2 C61 170.48(10) . . . . ? C8 Ru C1 C2 70.24(15) . . . . ? C3 Ru C1 C2 -37.20(14) . . . . ? P2 Ru C1 C2 -87.6(2) . . . . ? P1 Ru C1 C2 139.05(13) . . . . ? C7A Ru C1 C2 -114.67(19) . . . . ? C3A Ru C1 C2 -78.73(15) . . . . ? C8 Ru C1 C7A -175.09(12) . . . . ? C2 Ru C1 C7A 114.67(19) . . . . ? C3 Ru C1 C7A 77.47(14) . . . . ? P2 Ru C1 C7A 27.0(2) . . . . ? P1 Ru C1 C7A -106.28(12) . . . . ? C3A Ru C1 C7A 35.94(12) . . . . ? C7A C1 C2 C3 -4.4(3) . . . . ? Ru C1 C2 C3 63.57(16) . . . . ? C7A C1 C2 Ru -67.94(15) . . . . ? C8 Ru C2 C1 -117.02(14) . . . . ? C3 Ru C2 C1 117.7(2) . . . . ? P2 Ru C2 C1 145.20(12) . . . . ? P1 Ru C2 C1 -55.71(16) . . . . ? C7A Ru C2 C1 38.43(13) . . . . ? C3A Ru C2 C1 79.39(15) . . . . ? C8 Ru C2 C3 125.30(14) . . . . ? C1 Ru C2 C3 -117.7(2) . . . . ? P2 Ru C2 C3 27.52(18) . . . . ? P1 Ru C2 C3 -173.39(11) . . . . ? C7A Ru C2 C3 -79.25(15) . . . . ? C3A Ru C2 C3 -38.29(13) . . . . ? C1 C2 C3 C3A 4.8(3) . . . . ? Ru C2 C3 C3A 68.16(15) . . . . ? C1 C2 C3 Ru -63.40(16) . . . . ? C8 Ru C3 C2 -62.86(16) . . . . ? C1 Ru C3 C2 37.16(14) . . . . ? P2 Ru C3 C2 -160.96(13) . . . . ? P1 Ru C3 C2 21.8(3) . . . . ? C7A Ru C3 C2 79.00(15) . . . . ? C3A Ru C3 C2 114.5(2) . . . . ? C8 Ru C3 C3A -177.37(13) . . . . ? C2 Ru C3 C3A -114.5(2) . . . . ? C1 Ru C3 C3A -77.35(14) . . . . ? P2 Ru C3 C3A 84.53(13) . . . . ? P1 Ru C3 C3A -92.7(3) . . . . ? C7A Ru C3 C3A -35.51(13) . . . . ? C2 C3 C3A C4 175.0(2) . . . . ? Ru C3 C3A C4 -121.0(2) . . . . ? C2 C3 C3A C7A -3.3(2) . . . . ? Ru C3 C3A C7A 60.65(15) . . . . ? C2 C3 C3A Ru -63.94(15) . . . . ? C8 Ru C3A C4 131.7(2) . . . . ? C2 Ru C3A C4 166.1(2) . . . . ? C1 Ru C3A C4 -151.0(2) . . . . ? C3 Ru C3A C4 126.9(3) . . . . ? P2 Ru C3A C4 25.4(2) . . . . ? P1 Ru C3A C4 -76.0(2) . . . . ? C7A Ru C3A C4 -114.0(3) . . . . ? C8 Ru C3A C7A -114.34(18) . . . . ? C2 Ru C3A C7A -79.97(14) . . . . ? C1 Ru C3A C7A -37.09(13) . . . . ? C3 Ru C3A C7A -119.16(19) . . . . ? P2 Ru C3A C7A 139.39(12) . . . . ? P1 Ru C3A C7A 38.00(17) . . . . ? C8 Ru C3A C3 4.8(2) . . . . ? C2 Ru C3A C3 39.20(14) . . . . ? C1 Ru C3A C3 82.08(15) . . . . ? P2 Ru C3A C3 -101.45(13) . . . . ? P1 Ru C3A C3 157.16(11) . . . . ? C7A Ru C3A C3 119.16(19) . . . . ? C7A C3A C4 C5 -2.1(3) . . . . ? C3 C3A C4 C5 179.7(2) . . . . ? Ru C3A C4 C5 87.2(3) . . . . ? C3A C4 C5 C6 0.9(3) . . . . ? C4 C5 C6 C7 0.6(4) . . . . ? C5 C6 C7 C7A -0.8(3) . . . . ? C6 C7 C7A C3A -0.5(3) . . . . ? C6 C7 C7A C1 179.4(2) . . . . ? C6 C7 C7A Ru -89.6(3) . . . . ? C4 C3A C7A C7 2.0(3) . . . . ? C3 C3A C7A C7 -179.4(2) . . . . ? Ru C3A C7A C7 -121.8(2) . . . . ? C4 C3A C7A C1 -177.9(2) . . . . ? C3 C3A C7A C1 0.6(2) . . . . ? Ru C3A C7A C1 58.30(14) . . . . ? C4 C3A C7A Ru 123.8(2) . . . . ? C3 C3A C7A Ru -57.66(15) . . . . ? C2 C1 C7A C7 -177.7(2) . . . . ? Ru C1 C7A C7 118.2(3) . . . . ? C2 C1 C7A C3A 2.3(2) . . . . ? Ru C1 C7A C3A -61.85(15) . . . . ? C2 C1 C7A Ru 64.11(15) . . . . ? C8 Ru C7A C7 -119.4(2) . . . . ? C2 Ru C7A C7 -166.6(2) . . . . ? C1 Ru C7A C7 -127.6(3) . . . . ? C3 Ru C7A C7 150.5(2) . . . . ? P2 Ru C7A C7 64.6(2) . . . . ? P1 Ru C7A C7 -41.9(2) . . . . ? C3A Ru C7A C7 114.2(3) . . . . ? C8 Ru C7A C3A 126.41(16) . . . . ? C2 Ru C7A C3A 79.21(14) . . . . ? C1 Ru C7A C3A 118.18(19) . . . . ? C3 Ru C7A C3A 36.35(13) . . . . ? P2 Ru C7A C3A -49.62(14) . . . . ? P1 Ru C7A C3A -156.08(11) . . . . ? C8 Ru C7A C1 8.2(2) . . . . ? C2 Ru C7A C1 -38.98(14) . . . . ? C3 Ru C7A C1 -81.83(14) . . . . ? P2 Ru C7A C1 -167.81(11) . . . . ? P1 Ru C7A C1 85.74(13) . . . . ? C3A Ru C7A C1 -118.18(19) . . . . ? C2 Ru C8 C9 140.50(16) . . . . ? C1 Ru C8 C9 105.81(16) . . . . ? C3 Ru C8 C9 173.10(15) . . . . ? P2 Ru C8 C9 -82.74(15) . . . . ? P1 Ru C8 C9 8.22(13) . . . . ? C7A Ru C8 C9 100.63(19) . . . . ? C3A Ru C8 C9 169.99(15) . . . . ? C2 Ru C8 C11 -36.8(2) . . . . ? C1 Ru C8 C11 -71.5(2) . . . . ? C3 Ru C8 C11 -4.2(2) . . . . ? P2 Ru C8 C11 99.98(18) . . . . ? P1 Ru C8 C11 -169.1(2) . . . . ? C7A Ru C8 C11 -76.6(2) . . . . ? C3A Ru C8 C11 -7.3(3) . . . . ? C11 C8 C9 P1 167.55(17) . . . . ? Ru C8 C9 P1 -9.93(16) . . . . ? C31 P1 C9 C8 135.94(14) . . . . ? C21 P1 C9 C8 -112.81(15) . . . . ? Ru P1 C9 C8 8.31(13) . . . . ? C9 C8 C11 C16 154.7(2) . . . . ? Ru C8 C11 C16 -28.3(3) . . . . ? C9 C8 C11 C12 -25.6(3) . . . . ? Ru C8 C11 C12 151.38(18) . . . . ? C16 C11 C12 C13 -1.1(4) . . . . ? C8 C11 C12 C13 179.2(2) . . . . ? C11 C12 C13 C14 -1.0(4) . . . . ? C12 C13 C14 C15 2.1(5) . . . . ? C13 C14 C15 C16 -1.1(4) . . . . ? C14 C15 C16 C11 -1.0(4) . . . . ? C12 C11 C16 C15 2.1(4) . . . . ? C8 C11 C16 C15 -178.2(2) . . . . ? C9 P1 C21 C26 30.93(18) . . . . ? C31 P1 C21 C26 146.99(16) . . . . ? Ru P1 C21 C26 -62.73(18) . . . . ? C9 P1 C21 C22 155.50(16) . . . . ? C31 P1 C21 C22 -88.44(17) . . . . ? Ru P1 C21 C22 61.84(17) . . . . ? C26 C21 C22 C23 -54.4(3) . . . . ? P1 C21 C22 C23 -179.07(16) . . . . ? C21 C22 C23 C24 56.5(3) . . . . ? C22 C23 C24 C25 -56.7(3) . . . . ? C23 C24 C25 C26 55.9(3) . . . . ? C24 C25 C26 C21 -55.0(3) . . . . ? C22 C21 C26 C25 53.7(3) . . . . ? P1 C21 C26 C25 179.67(18) . . . . ? C9 P1 C31 C32 164.71(15) . . . . ? C21 P1 C31 C32 52.37(18) . . . . ? Ru P1 C31 C32 -95.66(16) . . . . ? C9 P1 C31 C36 36.98(19) . . . . ? C21 P1 C31 C36 -75.36(18) . . . . ? Ru P1 C31 C36 136.61(14) . . . . ? C36 C31 C32 C33 -59.1(2) . . . . ? P1 C31 C32 C33 171.70(15) . . . . ? C31 C32 C33 C34 58.4(2) . . . . ? C32 C33 C34 C35 -55.0(3) . . . . ? C33 C34 C35 C36 53.2(3) . . . . ? C34 C35 C36 C31 -54.1(3) . . . . ? C32 C31 C36 C35 56.8(3) . . . . ? P1 C31 C36 C35 -172.54(17) . . . . ? C51 P2 C41 C42 23.4(2) . . . . ? C61 P2 C41 C42 127.81(19) . . . . ? Ru P2 C41 C42 -99.42(19) . . . . ? C51 P2 C41 C46 -159.48(18) . . . . ? C61 P2 C41 C46 -55.1(2) . . . . ? Ru P2 C41 C46 77.71(19) . . . . ? C46 C41 C42 C43 0.7(4) . . . . ? P2 C41 C42 C43 177.91(19) . . . . ? C41 C42 C43 C44 1.0(4) . . . . ? C42 C43 C44 C45 -1.4(4) . . . . ? C43 C44 C45 C46 0.0(4) . . . . ? C44 C45 C46 C41 1.8(4) . . . . ? C42 C41 C46 C45 -2.1(3) . . . . ? P2 C41 C46 C45 -179.35(19) . . . . ? C41 P2 C51 C52 -130.21(17) . . . . ? C61 P2 C51 C52 125.09(17) . . . . ? Ru P2 C51 C52 -7.22(19) . . . . ? C41 P2 C51 C56 49.2(2) . . . . ? C61 P2 C51 C56 -55.5(2) . . . . ? Ru P2 C51 C56 172.17(16) . . . . ? C56 C51 C52 C53 1.7(3) . . . . ? P2 C51 C52 C53 -178.92(18) . . . . ? C51 C52 C53 C54 -0.4(4) . . . . ? C52 C53 C54 C55 -1.1(4) . . . . ? C53 C54 C55 C56 1.2(4) . . . . ? C54 C55 C56 C51 0.0(4) . . . . ? C52 C51 C56 C55 -1.5(3) . . . . ? P2 C51 C56 C55 179.12(18) . . . . ? C51 P2 C61 C66 -7.1(2) . . . . ? C41 P2 C61 C66 -110.71(19) . . . . ? Ru P2 C61 C66 120.73(18) . . . . ? C51 P2 C61 C62 176.04(17) . . . . ? C41 P2 C61 C62 72.46(19) . . . . ? Ru P2 C61 C62 -56.09(19) . . . . ? C66 C61 C62 C63 3.3(3) . . . . ? P2 C61 C62 C63 -179.71(18) . . . . ? C61 C62 C63 C64 -2.1(4) . . . . ? C62 C63 C64 C65 -0.3(4) . . . . ? C63 C64 C65 C66 1.4(4) . . . . ? C62 C61 C66 C65 -2.2(3) . . . . ? P2 C61 C66 C65 -179.10(18) . . . . ? C64 C65 C66 C61 -0.1(4) . . . . ? C3S C1S C2S C3S 1.6(8) 3_556 . . . ? C1S C2S C3S C1S -1.7(8) . . . 3_556 ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.40 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.666 _refine_diff_density_min -0.519 _refine_diff_density_rms 0.071 #===END data_3a _database_code_depnum_ccdc_archive 'CCDC 765664' #TrackingRef 'lrcc0.cif' _vrf_REFLT03_3a ; RESPONSE: The crystal used for data collection was found to display non-merohedral twinning. Both components of the twin were indexed with the program CELL_NOW (Bruker AXS Inc., Madison, WI, 2004). The second twin component can be related to the first component by 180 deg rotation about the [0.15 -0.82 1] axis in real space and about the [0 0 1] axis in reciprocal space. Integrated intensities for the reflections from the two components were written into a SHELXL-97 HKLF 5 reflection file with the data integration program SAINT (version 7.60A), using all reflection data (exactly overlapped, partially overlapped and non-overlapped). ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C47 H50 P2 Ru' _chemical_formula_sum 'C47 H50 P2 Ru' _chemical_formula_weight 777.88 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 9.8234(11) _cell_length_b 10.0881(11) _cell_length_c 22.744(2) _cell_angle_alpha 70.4887(12) _cell_angle_beta 84.1365(12) _cell_angle_gamma 62.9065(11) _cell_volume 1888.0(4) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9972 _cell_measurement_theta_min 2.27 _cell_measurement_theta_max 27.55 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.63 _exptl_crystal_size_mid 0.42 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.368 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 812 _exptl_absorpt_coefficient_mu 0.533 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.7297 _exptl_absorpt_correction_T_max 0.9253 _exptl_absorpt_process_details 'TWINABS (Sheldrick, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 14796 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0138 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 0.95 _diffrn_reflns_theta_max 27.54 _reflns_number_total 14796 _reflns_number_gt 14570 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'DIRDIF-2008 (Beurskens et al., 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0283P)^2^+0.9754P] 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 14796 _refine_ls_number_parameters 456 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0225 _refine_ls_R_factor_gt 0.0220 _refine_ls_wR_factor_ref 0.0628 _refine_ls_wR_factor_gt 0.0599 _refine_ls_goodness_of_fit_ref 1.136 _refine_ls_restrained_S_all 1.136 _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 0.261583(12) 0.362364(13) 0.289017(6) 0.01545(3) Uani 1 1 d . . . P1 P 0.39857(4) 0.41209(4) 0.206149(18) 0.01796(8) Uani 1 1 d . . . H1P H 0.367(2) 0.563(2) 0.1823(9) 0.030(5) Uiso 1 1 d . . . P2 P 0.29647(4) 0.52329(4) 0.330505(18) 0.01686(7) Uani 1 1 d . . . C1 C 0.19200(17) 0.17969(17) 0.28936(8) 0.0243(3) Uani 1 1 d . . . H1 H 0.1422 0.1791 0.2533 0.029 Uiso 1 1 calc R . . C2 C 0.35246(18) 0.10575(17) 0.30470(8) 0.0250(3) Uani 1 1 d . . . H2 H 0.4340 0.0453 0.2807 0.030 Uiso 1 1 calc R . . C3 C 0.37802(17) 0.12181(17) 0.36180(8) 0.0236(3) Uani 1 1 d . . . H3 H 0.4795 0.0757 0.3845 0.028 Uiso 1 1 calc R . . C3A C 0.22987(17) 0.19829(17) 0.38491(7) 0.0216(3) Uani 1 1 d . . . C4 C 0.18511(19) 0.23342(19) 0.44148(8) 0.0264(3) Uani 1 1 d . . . H4 H 0.2598 0.2103 0.4716 0.032 Uiso 1 1 calc R . . C5 C 0.0323(2) 0.3012(2) 0.45171(8) 0.0311(4) Uani 1 1 d . . . H5 H 0.0015 0.3243 0.4895 0.037 Uiso 1 1 calc R . . C6 C -0.08048(19) 0.3377(2) 0.40718(9) 0.0307(4) Uani 1 1 d . . . H6 H -0.1855 0.3848 0.4158 0.037 Uiso 1 1 calc R . . C7 C -0.04235(18) 0.30691(19) 0.35224(8) 0.0268(3) Uani 1 1 d . . . H7 H -0.1198 0.3338 0.3225 0.032 Uiso 1 1 calc R . . C7A C 0.11492(17) 0.23393(17) 0.34001(8) 0.0217(3) Uani 1 1 d . . . C10 C 0.09687(16) 0.55089(18) 0.22791(7) 0.0205(3) Uani 1 1 d . . . C11 C 0.00682(17) 0.65908(18) 0.18580(8) 0.0238(3) Uani 1 1 d . . . C12 C -0.08962(18) 0.77931(18) 0.13233(8) 0.0254(3) Uani 1 1 d . . . C13 C -0.2122(2) 0.7715(2) 0.10989(9) 0.0348(4) Uani 1 1 d . . . H13 H -0.2342 0.6855 0.1312 0.042 Uiso 1 1 calc R . . C14 C -0.3024(2) 0.8867(3) 0.05709(11) 0.0503(5) Uani 1 1 d . . . H14 H -0.3846 0.8783 0.0427 0.060 Uiso 1 1 calc R . . C15 C -0.2740(3) 1.0123(3) 0.02564(11) 0.0572(6) Uani 1 1 d . . . H15 H -0.3375 1.0922 -0.0099 0.069 Uiso 1 1 calc R . . C16 C -0.1524(3) 1.0218(3) 0.04597(12) 0.0573(6) Uani 1 1 d . . . H16 H -0.1307 1.1075 0.0237 0.069 Uiso 1 1 calc R . . C17 C -0.0612(2) 0.9069(2) 0.09878(10) 0.0421(5) Uani 1 1 d . . . H17 H 0.0220 0.9155 0.1123 0.051 Uiso 1 1 calc R . . C21 C 0.36940(17) 0.38504(18) 0.13197(7) 0.0223(3) Uani 1 1 d . . . H21 H 0.4722 0.3127 0.1218 0.027 Uiso 1 1 calc R . . C22 C 0.31430(19) 0.54040(19) 0.07757(8) 0.0262(3) Uani 1 1 d . . . H22A H 0.2127 0.6163 0.0858 0.031 Uiso 1 1 calc R . . H22B H 0.3866 0.5856 0.0743 0.031 Uiso 1 1 calc R . . C23 C 0.3029(2) 0.5155(2) 0.01622(8) 0.0362(4) Uani 1 1 d . . . H23A H 0.2636 0.6180 -0.0178 0.043 Uiso 1 1 calc R . . H23B H 0.4062 0.4468 0.0061 0.043 Uiso 1 1 calc R . . C24 C 0.1977(2) 0.4410(3) 0.02011(9) 0.0418(5) Uani 1 1 d . . . H24A H 0.1955 0.4223 -0.0198 0.050 Uiso 1 1 calc R . . H24B H 0.0924 0.5139 0.0265 0.050 Uiso 1 1 calc R . . C25 C 0.2511(2) 0.2855(2) 0.07368(9) 0.0372(4) Uani 1 1 d . . . H25A H 0.3519 0.2089 0.0651 0.045 Uiso 1 1 calc R . . H25B H 0.1773 0.2422 0.0767 0.045 Uiso 1 1 calc R . . C26 C 0.2646(2) 0.3080(2) 0.13590(8) 0.0305(4) Uani 1 1 d . . . H26A H 0.1616 0.3748 0.1469 0.037 Uiso 1 1 calc R . . H26B H 0.3060 0.2045 0.1693 0.037 Uiso 1 1 calc R . . C31 C 0.61033(16) 0.32782(18) 0.21492(7) 0.0229(3) Uani 1 1 d . . . H31 H 0.6342 0.3410 0.2537 0.027 Uiso 1 1 calc R . . C32 C 0.67133(17) 0.42093(19) 0.16048(8) 0.0266(3) Uani 1 1 d . . . H32A H 0.6423 0.4180 0.1207 0.032 Uiso 1 1 calc R . . H32B H 0.6231 0.5323 0.1590 0.032 Uiso 1 1 calc R . . C33 C 0.84536(18) 0.3546(2) 0.16688(8) 0.0290(3) Uani 1 1 d . . . H33A H 0.8807 0.4138 0.1298 0.035 Uiso 1 1 calc R . . H33B H 0.8742 0.3679 0.2043 0.035 Uiso 1 1 calc R . . C34 C 0.92310(18) 0.1814(2) 0.17279(9) 0.0326(4) Uani 1 1 d . . . H34A H 1.0354 0.1400 0.1781 0.039 Uiso 1 1 calc R . . H34B H 0.9004 0.1689 0.1341 0.039 Uiso 1 1 calc R . . C35 C 0.86768(19) 0.0877(2) 0.22856(10) 0.0385(4) Uani 1 1 d . . . H35A H 0.8984 0.0929 0.2675 0.046 Uiso 1 1 calc R . . H35B H 0.9172 -0.0241 0.2306 0.046 Uiso 1 1 calc R . . C36 C 0.69347(18) 0.15085(19) 0.22396(9) 0.0299(4) Uani 1 1 d . . . H36A H 0.6610 0.0934 0.2626 0.036 Uiso 1 1 calc R . . H36B H 0.6641 0.1316 0.1883 0.036 Uiso 1 1 calc R . . C41 C 0.41024(16) 0.41517(17) 0.40562(7) 0.0197(3) Uani 1 1 d . . . C42 C 0.55626(17) 0.29010(18) 0.40813(8) 0.0243(3) Uani 1 1 d . . . H42 H 0.5964 0.2679 0.3709 0.029 Uiso 1 1 calc R . . C43 C 0.64248(19) 0.19874(19) 0.46425(9) 0.0296(4) Uani 1 1 d . . . H43 H 0.7418 0.1157 0.4651 0.035 Uiso 1 1 calc R . . C44 C 0.5846(2) 0.2279(2) 0.51901(8) 0.0316(4) Uani 1 1 d . . . H44 H 0.6432 0.1641 0.5575 0.038 Uiso 1 1 calc R . . C45 C 0.4410(2) 0.3504(2) 0.51754(8) 0.0315(4) Uani 1 1 d . . . H45 H 0.4010 0.3708 0.5551 0.038 Uiso 1 1 calc R . . C46 C 0.35521(18) 0.44373(19) 0.46114(8) 0.0258(3) Uani 1 1 d . . . H46 H 0.2573 0.5285 0.4606 0.031 Uiso 1 1 calc R . . C51 C 0.38629(16) 0.64842(17) 0.28592(8) 0.0200(3) Uani 1 1 d . . . C52 C 0.30196(18) 0.77479(18) 0.23376(8) 0.0247(3) Uani 1 1 d . . . H52 H 0.2008 0.7956 0.2242 0.030 Uiso 1 1 calc R . . C53 C 0.3645(2) 0.87059(19) 0.19568(9) 0.0308(4) Uani 1 1 d . . . H53 H 0.3062 0.9561 0.1602 0.037 Uiso 1 1 calc R . . C54 C 0.5117(2) 0.8414(2) 0.20944(9) 0.0347(4) Uani 1 1 d . . . H54 H 0.5543 0.9069 0.1835 0.042 Uiso 1 1 calc R . . C55 C 0.5965(2) 0.7166(2) 0.26100(10) 0.0348(4) Uani 1 1 d . . . H55 H 0.6974 0.6967 0.2705 0.042 Uiso 1 1 calc R . . C56 C 0.53456(18) 0.62027(19) 0.29906(8) 0.0283(4) Uani 1 1 d . . . H56 H 0.5937 0.5345 0.3343 0.034 Uiso 1 1 calc R . . C61 C 0.12209(16) 0.67255(17) 0.35071(7) 0.0195(3) Uani 1 1 d . . . C62 C -0.01579(17) 0.66491(18) 0.35085(7) 0.0228(3) Uani 1 1 d . . . H62 H -0.0202 0.5858 0.3384 0.027 Uiso 1 1 calc R . . C63 C -0.14728(18) 0.7725(2) 0.36912(8) 0.0282(3) Uani 1 1 d . . . H63 H -0.2410 0.7666 0.3691 0.034 Uiso 1 1 calc R . . C64 C -0.14232(19) 0.8881(2) 0.38731(8) 0.0299(4) Uani 1 1 d . . . H64 H -0.2324 0.9609 0.4000 0.036 Uiso 1 1 calc R . . C65 C -0.00583(19) 0.89775(19) 0.38708(8) 0.0286(3) Uani 1 1 d . . . H65 H -0.0023 0.9769 0.3997 0.034 Uiso 1 1 calc R . . C66 C 0.12567(18) 0.79165(18) 0.36834(8) 0.0243(3) Uani 1 1 d . . . H66 H 0.2185 0.7998 0.3674 0.029 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 0.01548(5) 0.01607(5) 0.01455(5) -0.00490(5) 0.00107(4) -0.00695(4) P1 0.01914(17) 0.01881(17) 0.01623(19) -0.00627(15) 0.00257(14) -0.00868(14) P2 0.01576(16) 0.01735(17) 0.01671(18) -0.00598(14) 0.00067(13) -0.00646(13) C1 0.0292(7) 0.0241(7) 0.0254(8) -0.0092(7) 0.0025(7) -0.0161(6) C2 0.0273(8) 0.0192(7) 0.0286(9) -0.0080(6) 0.0056(6) -0.0112(6) C3 0.0216(7) 0.0184(7) 0.0257(9) -0.0024(6) 0.0007(6) -0.0078(6) C3A 0.0240(7) 0.0172(7) 0.0218(8) -0.0020(6) 0.0007(6) -0.0107(6) C4 0.0346(8) 0.0276(8) 0.0165(8) -0.0014(6) 0.0010(6) -0.0175(7) C5 0.0391(9) 0.0333(9) 0.0214(9) -0.0075(7) 0.0108(7) -0.0194(8) C6 0.0254(8) 0.0298(9) 0.0349(10) -0.0081(8) 0.0112(7) -0.0141(7) C7 0.0230(7) 0.0269(8) 0.0317(9) -0.0059(7) 0.0015(6) -0.0147(6) C7A 0.0237(7) 0.0211(7) 0.0226(8) -0.0046(6) 0.0018(6) -0.0137(6) C10 0.0191(7) 0.0231(7) 0.0222(8) -0.0101(6) 0.0033(6) -0.0103(6) C11 0.0226(7) 0.0231(7) 0.0246(8) -0.0085(7) 0.0010(6) -0.0087(6) C12 0.0246(7) 0.0213(7) 0.0236(8) -0.0084(6) -0.0004(6) -0.0037(6) C13 0.0296(8) 0.0347(9) 0.0339(10) -0.0073(8) -0.0050(7) -0.0107(7) C14 0.0371(10) 0.0584(14) 0.0430(13) -0.0135(11) -0.0152(9) -0.0096(10) C15 0.0561(13) 0.0439(12) 0.0371(13) 0.0032(10) -0.0185(10) -0.0012(10) C16 0.0680(15) 0.0306(11) 0.0495(15) 0.0067(10) -0.0070(12) -0.0143(10) C17 0.0489(11) 0.0280(9) 0.0435(12) -0.0033(9) -0.0085(9) -0.0159(8) C21 0.0251(7) 0.0234(7) 0.0171(7) -0.0066(6) 0.0004(6) -0.0096(6) C22 0.0302(8) 0.0269(8) 0.0187(8) -0.0032(7) -0.0005(6) -0.0131(7) C23 0.0484(11) 0.0398(10) 0.0184(9) -0.0050(8) -0.0018(7) -0.0206(9) C24 0.0451(11) 0.0607(13) 0.0257(10) -0.0131(9) -0.0059(8) -0.0278(10) C25 0.0522(11) 0.0496(11) 0.0266(10) -0.0167(9) 0.0034(8) -0.0338(10) C26 0.0427(10) 0.0350(9) 0.0221(8) -0.0099(7) 0.0021(7) -0.0239(8) C31 0.0200(7) 0.0286(8) 0.0196(8) -0.0074(6) 0.0027(6) -0.0111(6) C32 0.0231(7) 0.0288(8) 0.0271(9) -0.0065(7) 0.0033(6) -0.0130(6) C33 0.0235(7) 0.0380(9) 0.0270(9) -0.0092(7) 0.0021(6) -0.0160(7) C34 0.0209(7) 0.0390(10) 0.0322(10) -0.0094(8) 0.0032(7) -0.0105(7) C35 0.0238(8) 0.0331(10) 0.0382(11) 0.0040(8) -0.0029(7) -0.0058(7) C36 0.0232(7) 0.0261(8) 0.0296(9) 0.0010(7) 0.0004(6) -0.0090(6) C41 0.0220(7) 0.0205(7) 0.0177(7) -0.0046(6) -0.0021(5) -0.0110(6) C42 0.0235(7) 0.0246(8) 0.0238(8) -0.0081(7) -0.0016(6) -0.0091(6) C43 0.0271(8) 0.0234(8) 0.0337(10) -0.0052(7) -0.0092(7) -0.0082(6) C44 0.0411(9) 0.0281(8) 0.0255(9) -0.0004(7) -0.0124(7) -0.0184(7) C45 0.0459(10) 0.0346(9) 0.0169(8) -0.0064(7) -0.0005(7) -0.0212(8) C46 0.0276(8) 0.0268(8) 0.0220(8) -0.0081(7) 0.0016(6) -0.0113(6) C51 0.0210(6) 0.0207(7) 0.0220(7) -0.0102(6) 0.0035(6) -0.0106(6) C52 0.0263(7) 0.0214(7) 0.0257(9) -0.0084(7) 0.0034(6) -0.0101(6) C53 0.0390(9) 0.0197(8) 0.0306(10) -0.0073(7) 0.0074(7) -0.0123(7) C54 0.0417(10) 0.0298(9) 0.0427(11) -0.0167(8) 0.0199(8) -0.0244(8) C55 0.0299(9) 0.0410(10) 0.0453(11) -0.0181(9) 0.0085(8) -0.0240(8) C56 0.0251(7) 0.0303(8) 0.0329(10) -0.0126(7) 0.0012(7) -0.0136(6) C61 0.0189(7) 0.0176(7) 0.0174(7) -0.0056(6) 0.0003(5) -0.0042(5) C62 0.0229(7) 0.0226(7) 0.0206(8) -0.0064(6) 0.0026(6) -0.0091(6) C63 0.0206(7) 0.0322(9) 0.0267(9) -0.0088(7) 0.0046(6) -0.0089(6) C64 0.0271(8) 0.0267(8) 0.0240(9) -0.0098(7) 0.0050(6) -0.0021(7) C65 0.0371(9) 0.0221(8) 0.0232(9) -0.0110(7) 0.0028(7) -0.0084(7) C66 0.0257(7) 0.0243(8) 0.0231(8) -0.0093(6) 0.0003(6) -0.0100(6) _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 2.0143(15) . ? Ru C2 2.2291(15) . ? Ru C1 2.2361(14) . ? Ru P1 2.2539(4) . ? Ru C3 2.2611(15) . ? Ru P2 2.2890(4) . ? Ru C7A 2.3356(14) . ? Ru C3A 2.3480(15) . ? P1 C31 1.8575(15) . ? P1 C21 1.8657(16) . ? P2 C61 1.8343(14) . ? P2 C51 1.8377(15) . ? P2 C41 1.8419(15) . ? C1 C2 1.425(2) . ? C1 C7A 1.437(2) . ? C2 C3 1.421(2) . ? C3 C3A 1.443(2) . ? C3A C4 1.422(2) . ? C3A C7A 1.438(2) . ? C4 C5 1.369(2) . ? C5 C6 1.414(3) . ? C6 C7 1.362(2) . ? C7 C7A 1.421(2) . ? C10 C11 1.219(2) . ? C11 C12 1.432(2) . ? C12 C17 1.395(3) . ? C12 C13 1.398(2) . ? C13 C14 1.387(3) . ? C14 C15 1.367(3) . ? C15 C16 1.377(4) . ? C16 C17 1.390(3) . ? C21 C26 1.528(2) . ? C21 C22 1.533(2) . ? C22 C23 1.521(2) . ? C23 C24 1.511(3) . ? C24 C25 1.525(3) . ? C25 C26 1.534(2) . ? C31 C36 1.535(2) . ? C31 C32 1.536(2) . ? C32 C33 1.528(2) . ? C33 C34 1.518(2) . ? C34 C35 1.525(2) . ? C35 C36 1.531(2) . ? C41 C46 1.390(2) . ? C41 C42 1.405(2) . ? C42 C43 1.386(2) . ? C43 C44 1.382(3) . ? C44 C45 1.382(3) . ? C45 C46 1.391(2) . ? C51 C56 1.395(2) . ? C51 C52 1.395(2) . ? C52 C53 1.391(2) . ? C53 C54 1.385(3) . ? C54 C55 1.383(3) . ? C55 C56 1.390(2) . ? C61 C62 1.391(2) . ? C61 C66 1.403(2) . ? C62 C63 1.391(2) . ? C63 C64 1.382(2) . ? C64 C65 1.387(2) . ? C65 C66 1.389(2) . ? 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 130.91(6) . . ? C10 Ru C1 98.78(6) . . ? C2 Ru C1 37.22(6) . . ? C10 Ru P1 78.79(4) . . ? C2 Ru P1 96.70(4) . . ? C1 Ru P1 111.54(4) . . ? C10 Ru C3 158.78(6) . . ? C2 Ru C3 36.90(6) . . ? C1 Ru C3 62.19(6) . . ? P1 Ru C3 115.72(4) . . ? C10 Ru P2 90.46(4) . . ? C2 Ru P2 138.61(4) . . ? C1 Ru P2 155.40(5) . . ? P1 Ru P2 92.553(15) . . ? C3 Ru P2 103.61(4) . . ? C10 Ru C7A 98.40(6) . . ? C2 Ru C7A 60.68(5) . . ? C1 Ru C7A 36.56(6) . . ? P1 Ru C7A 147.74(4) . . ? C3 Ru C7A 60.89(5) . . ? P2 Ru C7A 119.69(4) . . ? C10 Ru C3A 127.63(6) . . ? C2 Ru C3A 60.42(6) . . ? C1 Ru C3A 60.85(6) . . ? P1 Ru C3A 152.14(4) . . ? C3 Ru C3A 36.42(5) . . ? P2 Ru C3A 95.52(4) . . ? C7A Ru C3A 35.76(5) . . ? C31 P1 C21 102.53(7) . . ? C31 P1 Ru 120.85(5) . . ? C21 P1 Ru 120.54(5) . . ? C61 P2 C51 99.45(7) . . ? C61 P2 C41 102.11(7) . . ? C51 P2 C41 103.51(7) . . ? C61 P2 Ru 115.90(5) . . ? C51 P2 Ru 120.61(5) . . ? C41 P2 Ru 112.75(5) . . ? C2 C1 C7A 107.46(14) . . ? C2 C1 Ru 71.13(8) . . ? C7A C1 Ru 75.49(8) . . ? C3 C2 C1 109.39(14) . . ? C3 C2 Ru 72.78(8) . . ? C1 C2 Ru 71.66(8) . . ? C2 C3 C3A 107.21(14) . . ? C2 C3 Ru 70.33(9) . . ? C3A C3 Ru 75.07(9) . . ? C4 C3A C7A 119.70(14) . . ? C4 C3A C3 132.25(15) . . ? C7A C3A C3 107.97(14) . . ? C4 C3A Ru 127.80(11) . . ? C7A C3A Ru 71.65(9) . . ? C3 C3A Ru 68.51(8) . . ? C5 C4 C3A 118.75(16) . . ? C4 C5 C6 121.41(16) . . ? C7 C6 C5 121.63(15) . . ? C6 C7 C7A 119.02(16) . . ? C7 C7A C1 132.71(15) . . ? C7 C7A C3A 119.46(15) . . ? C1 C7A C3A 107.81(13) . . ? C7 C7A Ru 126.28(11) . . ? C1 C7A Ru 67.95(8) . . ? C3A C7A Ru 72.59(8) . . ? C11 C10 Ru 172.82(13) . . ? C10 C11 C12 174.59(17) . . ? C17 C12 C13 116.97(16) . . ? C17 C12 C11 121.06(16) . . ? C13 C12 C11 121.93(16) . . ? C14 C13 C12 121.37(19) . . ? C15 C14 C13 120.6(2) . . ? C14 C15 C16 119.4(2) . . ? C15 C16 C17 120.5(2) . . ? C16 C17 C12 121.1(2) . . ? C26 C21 C22 110.53(13) . . ? C26 C21 P1 114.67(11) . . ? C22 C21 P1 111.26(10) . . ? C23 C22 C21 111.12(14) . . ? C24 C23 C22 111.06(15) . . ? C23 C24 C25 111.04(15) . . ? C24 C25 C26 111.04(15) . . ? C21 C26 C25 111.20(14) . . ? C36 C31 C32 111.59(13) . . ? C36 C31 P1 113.41(11) . . ? C32 C31 P1 111.00(11) . . ? C33 C32 C31 112.02(13) . . ? C34 C33 C32 110.71(13) . . ? C33 C34 C35 110.76(15) . . ? C34 C35 C36 111.67(14) . . ? C35 C36 C31 111.64(14) . . ? C46 C41 C42 117.88(14) . . ? C46 C41 P2 123.38(12) . . ? C42 C41 P2 118.59(12) . . ? C43 C42 C41 120.86(15) . . ? C44 C43 C42 120.25(15) . . ? C43 C44 C45 119.77(15) . . ? C44 C45 C46 120.09(16) . . ? C41 C46 C45 121.14(15) . . ? C56 C51 C52 118.61(14) . . ? C56 C51 P2 124.31(13) . . ? C52 C51 P2 117.00(11) . . ? C53 C52 C51 120.67(15) . . ? C54 C53 C52 120.03(17) . . ? C55 C54 C53 119.90(16) . . ? C54 C55 C56 120.23(16) . . ? C55 C56 C51 120.56(16) . . ? C62 C61 C66 118.99(13) . . ? C62 C61 P2 119.66(11) . . ? C66 C61 P2 121.31(11) . . ? C63 C62 C61 120.27(15) . . ? C64 C63 C62 120.39(15) . . ? C63 C64 C65 120.00(14) . . ? C64 C65 C66 119.98(15) . . ? C65 C66 C61 120.35(15) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C10 Ru P1 C31 162.88(7) . . . . ? C2 Ru P1 C31 -66.67(7) . . . . ? C1 Ru P1 C31 -102.01(7) . . . . ? C3 Ru P1 C31 -33.51(8) . . . . ? P2 Ru P1 C31 72.92(6) . . . . ? C7A Ru P1 C31 -109.13(9) . . . . ? C3A Ru P1 C31 -33.97(10) . . . . ? C10 Ru P1 C21 -66.90(7) . . . . ? C2 Ru P1 C21 63.56(7) . . . . ? C1 Ru P1 C21 28.21(7) . . . . ? C3 Ru P1 C21 96.71(7) . . . . ? P2 Ru P1 C21 -156.86(6) . . . . ? C7A Ru P1 C21 21.10(9) . . . . ? C3A Ru P1 C21 96.26(10) . . . . ? C10 Ru P2 C61 49.09(7) . . . . ? C2 Ru P2 C61 -128.98(8) . . . . ? C1 Ru P2 C61 -63.50(11) . . . . ? P1 Ru P2 C61 127.89(6) . . . . ? C3 Ru P2 C61 -114.86(7) . . . . ? C7A Ru P2 C61 -50.85(7) . . . . ? C3A Ru P2 C61 -78.80(7) . . . . ? C10 Ru P2 C51 -70.87(7) . . . . ? C2 Ru P2 C51 111.05(8) . . . . ? C1 Ru P2 C51 176.53(11) . . . . ? P1 Ru P2 C51 7.93(6) . . . . ? C3 Ru P2 C51 125.17(7) . . . . ? C7A Ru P2 C51 -170.82(7) . . . . ? C3A Ru P2 C51 161.23(7) . . . . ? C10 Ru P2 C41 166.27(7) . . . . ? C2 Ru P2 C41 -11.81(8) . . . . ? C1 Ru P2 C41 53.67(11) . . . . ? P1 Ru P2 C41 -114.93(5) . . . . ? C3 Ru P2 C41 2.31(7) . . . . ? C7A Ru P2 C41 66.32(7) . . . . ? C3A Ru P2 C41 38.37(6) . . . . ? C10 Ru C1 C2 153.13(10) . . . . ? P1 Ru C1 C2 71.79(10) . . . . ? C3 Ru C1 C2 -36.83(9) . . . . ? P2 Ru C1 C2 -95.96(12) . . . . ? C7A Ru C1 C2 -114.58(14) . . . . ? C3A Ru C1 C2 -78.46(10) . . . . ? C10 Ru C1 C7A -92.28(10) . . . . ? C2 Ru C1 C7A 114.58(14) . . . . ? P1 Ru C1 C7A -173.63(8) . . . . ? C3 Ru C1 C7A 77.75(10) . . . . ? P2 Ru C1 C7A 18.62(16) . . . . ? C3A Ru C1 C7A 36.13(9) . . . . ? C7A C1 C2 C3 -3.93(17) . . . . ? Ru C1 C2 C3 63.42(11) . . . . ? C7A C1 C2 Ru -67.35(10) . . . . ? C10 Ru C2 C3 -154.20(9) . . . . ? C1 Ru C2 C3 -117.97(13) . . . . ? P1 Ru C2 C3 124.85(8) . . . . ? P2 Ru C2 C3 23.25(12) . . . . ? C7A Ru C2 C3 -79.56(10) . . . . ? C3A Ru C2 C3 -38.27(9) . . . . ? C10 Ru C2 C1 -36.22(13) . . . . ? P1 Ru C2 C1 -117.17(9) . . . . ? C3 Ru C2 C1 117.97(13) . . . . ? P2 Ru C2 C1 141.23(8) . . . . ? C7A Ru C2 C1 38.41(9) . . . . ? C3A Ru C2 C1 79.70(10) . . . . ? C1 C2 C3 C3A 3.89(17) . . . . ? Ru C2 C3 C3A 66.60(10) . . . . ? C1 C2 C3 Ru -62.71(11) . . . . ? C10 Ru C3 C2 65.35(19) . . . . ? C1 Ru C3 C2 37.15(9) . . . . ? P1 Ru C3 C2 -64.78(9) . . . . ? P2 Ru C3 C2 -164.42(8) . . . . ? C7A Ru C3 C2 78.93(10) . . . . ? C3A Ru C3 C2 114.86(13) . . . . ? C10 Ru C3 C3A -49.5(2) . . . . ? C2 Ru C3 C3A -114.86(13) . . . . ? C1 Ru C3 C3A -77.71(10) . . . . ? P1 Ru C3 C3A -179.64(7) . . . . ? P2 Ru C3 C3A 80.72(9) . . . . ? C7A Ru C3 C3A -35.93(9) . . . . ? C2 C3 C3A C4 174.41(16) . . . . ? Ru C3 C3A C4 -122.16(17) . . . . ? C2 C3 C3A C7A -2.33(16) . . . . ? Ru C3 C3A C7A 61.10(10) . . . . ? C2 C3 C3A Ru -63.43(10) . . . . ? C10 Ru C3A C4 -72.82(15) . . . . ? C2 Ru C3A C4 166.31(16) . . . . ? C1 Ru C3A C4 -150.74(16) . . . . ? P1 Ru C3A C4 128.21(12) . . . . ? C3 Ru C3A C4 127.53(18) . . . . ? P2 Ru C3A C4 22.04(14) . . . . ? C7A Ru C3A C4 -113.79(17) . . . . ? C10 Ru C3A C7A 40.98(11) . . . . ? C2 Ru C3A C7A -79.90(10) . . . . ? C1 Ru C3A C7A -36.94(9) . . . . ? P1 Ru C3A C7A -117.99(9) . . . . ? C3 Ru C3A C7A -118.68(13) . . . . ? P2 Ru C3A C7A 135.83(8) . . . . ? C10 Ru C3A C3 159.66(9) . . . . ? C2 Ru C3A C3 38.78(9) . . . . ? C1 Ru C3A C3 81.74(10) . . . . ? P1 Ru C3A C3 0.69(14) . . . . ? P2 Ru C3A C3 -105.49(9) . . . . ? C7A Ru C3A C3 118.68(13) . . . . ? C7A C3A C4 C5 -0.2(2) . . . . ? C3 C3A C4 C5 -176.61(16) . . . . ? Ru C3A C4 C5 88.90(18) . . . . ? C3A C4 C5 C6 -0.5(2) . . . . ? C4 C5 C6 C7 0.1(3) . . . . ? C5 C6 C7 C7A 1.1(2) . . . . ? C6 C7 C7A C1 176.43(16) . . . . ? C6 C7 C7A C3A -1.7(2) . . . . ? C6 C7 C7A Ru -91.06(18) . . . . ? C2 C1 C7A C7 -175.91(16) . . . . ? Ru C1 C7A C7 119.67(17) . . . . ? C2 C1 C7A C3A 2.41(17) . . . . ? Ru C1 C7A C3A -62.01(10) . . . . ? C2 C1 C7A Ru 64.43(10) . . . . ? C4 C3A C7A C7 1.3(2) . . . . ? C3 C3A C7A C7 178.53(13) . . . . ? Ru C3A C7A C7 -122.35(14) . . . . ? C4 C3A C7A C1 -177.28(13) . . . . ? C3 C3A C7A C1 -0.05(16) . . . . ? Ru C3A C7A C1 59.07(10) . . . . ? C4 C3A C7A Ru 123.65(13) . . . . ? C3 C3A C7A Ru -59.12(10) . . . . ? C10 Ru C7A C7 -34.18(15) . . . . ? C2 Ru C7A C7 -166.73(17) . . . . ? C1 Ru C7A C7 -127.62(19) . . . . ? P1 Ru C7A C7 -116.47(13) . . . . ? C3 Ru C7A C7 150.75(16) . . . . ? P2 Ru C7A C7 61.18(15) . . . . ? C3A Ru C7A C7 114.16(18) . . . . ? C10 Ru C7A C1 93.44(10) . . . . ? C2 Ru C7A C1 -39.11(9) . . . . ? P1 Ru C7A C1 11.15(13) . . . . ? C3 Ru C7A C1 -81.63(10) . . . . ? P2 Ru C7A C1 -171.20(8) . . . . ? C3A Ru C7A C1 -118.22(13) . . . . ? C10 Ru C7A C3A -148.34(9) . . . . ? C2 Ru C7A C3A 79.11(10) . . . . ? C1 Ru C7A C3A 118.22(13) . . . . ? P1 Ru C7A C3A 129.38(8) . . . . ? C3 Ru C7A C3A 36.60(9) . . . . ? P2 Ru C7A C3A -52.97(9) . . . . ? C2 Ru C10 C11 -58.5(11) . . . . ? C1 Ru C10 C11 -79.7(10) . . . . ? P1 Ru C10 C11 30.6(10) . . . . ? C3 Ru C10 C11 -104.7(10) . . . . ? P2 Ru C10 C11 123.2(10) . . . . ? C7A Ru C10 C11 -116.7(10) . . . . ? C3A Ru C10 C11 -139.5(10) . . . . ? Ru C10 C11 C12 2(3) . . . . ? C10 C11 C12 C17 -84.6(18) . . . . ? C10 C11 C12 C13 92.9(18) . . . . ? C17 C12 C13 C14 -0.8(3) . . . . ? C11 C12 C13 C14 -178.33(18) . . . . ? C12 C13 C14 C15 -0.4(3) . . . . ? C13 C14 C15 C16 1.5(4) . . . . ? C14 C15 C16 C17 -1.4(4) . . . . ? C15 C16 C17 C12 0.2(4) . . . . ? C13 C12 C17 C16 0.9(3) . . . . ? C11 C12 C17 C16 178.42(19) . . . . ? C31 P1 C21 C26 130.13(12) . . . . ? Ru P1 C21 C26 -7.69(14) . . . . ? C31 P1 C21 C22 -103.51(11) . . . . ? Ru P1 C21 C22 118.68(10) . . . . ? C26 C21 C22 C23 -55.95(18) . . . . ? P1 C21 C22 C23 175.43(12) . . . . ? C21 C22 C23 C24 57.0(2) . . . . ? C22 C23 C24 C25 -56.9(2) . . . . ? C23 C24 C25 C26 56.0(2) . . . . ? C22 C21 C26 C25 55.10(19) . . . . ? P1 C21 C26 C25 -178.17(12) . . . . ? C24 C25 C26 C21 -55.3(2) . . . . ? C21 P1 C31 C36 -63.99(13) . . . . ? Ru P1 C31 C36 73.66(13) . . . . ? C21 P1 C31 C32 62.57(12) . . . . ? Ru P1 C31 C32 -159.78(9) . . . . ? C36 C31 C32 C33 -52.89(18) . . . . ? P1 C31 C32 C33 179.55(11) . . . . ? C31 C32 C33 C34 55.90(19) . . . . ? C32 C33 C34 C35 -57.61(19) . . . . ? C33 C34 C35 C36 57.1(2) . . . . ? C34 C35 C36 C31 -54.1(2) . . . . ? C32 C31 C36 C35 51.65(19) . . . . ? P1 C31 C36 C35 177.90(13) . . . . ? C61 P2 C41 C46 5.47(14) . . . . ? C51 P2 C41 C46 108.43(13) . . . . ? Ru P2 C41 C46 -119.60(12) . . . . ? C61 P2 C41 C42 -179.07(12) . . . . ? C51 P2 C41 C42 -76.10(13) . . . . ? Ru P2 C41 C42 55.87(13) . . . . ? C46 C41 C42 C43 -0.2(2) . . . . ? P2 C41 C42 C43 -175.92(12) . . . . ? C41 C42 C43 C44 1.1(2) . . . . ? C42 C43 C44 C45 -1.0(3) . . . . ? C43 C44 C45 C46 0.1(3) . . . . ? C42 C41 C46 C45 -0.8(2) . . . . ? P2 C41 C46 C45 174.73(12) . . . . ? C44 C45 C46 C41 0.8(3) . . . . ? C61 P2 C51 C56 125.31(14) . . . . ? C41 P2 C51 C56 20.31(15) . . . . ? Ru P2 C51 C56 -106.88(13) . . . . ? C61 P2 C51 C52 -58.08(13) . . . . ? C41 P2 C51 C52 -163.08(12) . . . . ? Ru P2 C51 C52 69.73(12) . . . . ? C56 C51 C52 C53 0.0(2) . . . . ? P2 C51 C52 C53 -176.79(12) . . . . ? C51 C52 C53 C54 -0.2(2) . . . . ? C52 C53 C54 C55 0.1(3) . . . . ? C53 C54 C55 C56 0.1(3) . . . . ? C54 C55 C56 C51 -0.3(3) . . . . ? C52 C51 C56 C55 0.2(2) . . . . ? P2 C51 C56 C55 176.76(13) . . . . ? C51 P2 C61 C62 142.13(13) . . . . ? C41 P2 C61 C62 -111.73(13) . . . . ? Ru P2 C61 C62 11.23(14) . . . . ? C51 P2 C61 C66 -40.23(14) . . . . ? C41 P2 C61 C66 65.91(14) . . . . ? Ru P2 C61 C66 -171.13(11) . . . . ? C66 C61 C62 C63 -0.9(2) . . . . ? P2 C61 C62 C63 176.75(13) . . . . ? C61 C62 C63 C64 0.0(3) . . . . ? C62 C63 C64 C65 0.4(3) . . . . ? C63 C64 C65 C66 0.3(3) . . . . ? C64 C65 C66 C61 -1.2(3) . . . . ? C62 C61 C66 C65 1.6(2) . . . . ? P2 C61 C66 C65 -176.10(13) . . . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 27.54 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.403 _refine_diff_density_min -0.411 _refine_diff_density_rms 0.060 #===END