Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2004 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Helmut Werner' 'Carsten D. Brandt' 'Stefan Jung' 'Justin Wolf' _publ_contact_author_name 'Prof Helmut Werner' _publ_contact_author_address ; Inorganic Chemistry Department Universitaet Wuerzburg Am Hubland Wuerzburg D-97074 GERMANY ; _publ_contact_author_phone '049 931 888 5261' _publ_contact_author_fax '049 931 888 4605' _publ_contact_author_email helmut.werner@mail.uni-wuerzburg.de _publ_requested_coeditor_name ? _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Vinyl and carbene ruthenium(II) complexes from hydridoruthenium(II) precursors ; _publ_section_abstract ; The reactions of the hydrido compounds [RuHCl(CO)(L)2] (L = PiPr3 1, PCy3 2) with HCºCR (R = H, Ph, tBu) afforded by insertion of the alkyne into the Ru-H bond the corresponding vinyl complexes [RuCl(CH=CHR)(CO)(L)2] 3-8, which upon protonation with HBF4 gave the cationic five-coordinated ruthenium carbenes [RuCl(=CHCH2R)(CO)(L)2]BF4 9-14. Subsequent reactions of the carbene complexes with PR3 (R = Me, iPr) and CH3CN led either to deprotonation and re-generation of the vinyl compounds or to cleavage of the ruthenium-carbene bond and the formation of the six-coordinated complexes [RuCl(CO)(CH3CN)2(PiPr3)2]BF4 17 and [RuH(CO)(CH3CN)2(PiPr3)2]X 18a,b. The acetato derivative [RuH(k2-O2CCH3)(CO)(PCy3)2] 19 also reacted with acetylene and phenylacetylene by insertion to yield the related vinyl complexes [Ru(CH=CHR)(k2-O2CCH3)(CO)(PCy3)2] 20, 21, of which that with R = H was protonated with HBF4 to yield the corresponding cationic ruthenium carbene 22. With [RuHCl(H2)(PCy3)2] 25 as the starting material, the five-coordinated chloro(hydrido)ruthenium(II) compounds [RuHCl(PCy3)(dppf)] 26 (dppf = [Fe(h5-C5H4PPh2)2]), [RuHCl{Sb(CH2Ph)3}(PCy3)2] 27 and [RuHCl(CH3CN)(PCy3)2] 30 were prepared. The reactions of 27 with HCºCR (R = H, Ph) gave the hydrido(vinylidene) complexes [RuHCl(=C=CHR)(PCy3)2] 28, 29, whereas treatment of 30 with HC CPh afforded the vinyl compound [RuCl(CH=CHPh)(CH3CN)(PCy3)2] 31. The molecular structures of 13 (R = Ph, L = PCy3) and 26 were determined crystallographically. ; _publ_section_exptl_prep ; Crystals were grown from a solution in dichlormethane layered with pentane at room temerature ; _publ_section_exptl_refinement ; The asymmetric unit contains half a molecule of dichlormethane. ; data_sj3cb _database_code_depnum_ccdc_archive 'CCDC 224060' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C52.50 H63 Cl2 Fe P3 Ru' _chemical_formula_weight 1014.76 _chemical_compound_source ? 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 '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_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.696(2) _cell_length_b 13.138(3) _cell_length_c 17.222(3) _cell_angle_alpha 77.15(3) _cell_angle_beta 80.40(3) _cell_angle_gamma 82.02(3) _cell_volume 2313.5(8) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 5000 _cell_measurement_theta_min 2.38 _cell_measurement_theta_max 25.00 _exptl_crystal_description plates _exptl_crystal_colour red-violett _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.457 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1054 _exptl_absorpt_coefficient_mu 0.896 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'IPDS (STOE)' _diffrn_measurement_method 'IPDS (STOE)' _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 23315 _diffrn_reflns_av_R_equivalents 0.1346 _diffrn_reflns_av_sigmaI/netI 0.1287 _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 -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.38 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7671 _reflns_number_gt 4869 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'IPDS (STOE)' _computing_cell_refinement 'IPDS (STOE)' _computing_data_reduction 'IPDS (STOE)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XSHELL in SHELXTL-97' _computing_publication_material 'XSHELL in SHELXTL-97' _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^)+(0.0100P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7671 _refine_ls_number_parameters 541 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0787 _refine_ls_R_factor_gt 0.0411 _refine_ls_wR_factor_ref 0.0844 _refine_ls_wR_factor_gt 0.0780 _refine_ls_goodness_of_fit_ref 0.817 _refine_ls_restrained_S_all 0.817 _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 0.83488(4) 0.27897(3) 0.23995(2) 0.01378(10) Uani 1 1 d . . . Fe Fe 0.73712(6) 0.33897(6) 0.48440(3) 0.01885(17) Uani 1 1 d . . . Cl1 Cl 0.78024(11) 0.39790(9) 0.11535(6) 0.0212(3) Uani 1 1 d . . . Cl2 Cl 0.4947(2) 0.39336(18) -0.00892(14) 0.0921(7) Uani 1 1 d . . . P1 P 0.89734(12) 0.13993(9) 0.16513(6) 0.0154(3) Uani 1 1 d . . . P2 P 0.69509(11) 0.20593(9) 0.33773(6) 0.0153(3) Uani 1 1 d . . . P3 P 0.85085(11) 0.42462(9) 0.29003(6) 0.0142(3) Uani 1 1 d . . . C10 C 1.0100(4) 0.2035(3) 0.0807(2) 0.0149(10) Uani 1 1 d . . . H10 H 0.9543 0.2581 0.0480 0.018 Uiso 1 1 calc R . . C11 C 1.0836(4) 0.1384(4) 0.0196(2) 0.0185(10) Uani 1 1 d . . . H11A H 1.1510 0.0886 0.0446 0.022 Uiso 1 1 calc R . . H11B H 1.0245 0.0974 0.0038 0.022 Uiso 1 1 calc R . . C12 C 1.1445(5) 0.2126(4) -0.0556(2) 0.0223(11) Uani 1 1 d . . . H12A H 1.1958 0.1702 -0.0928 0.027 Uiso 1 1 calc R . . H12B H 1.0760 0.2565 -0.0838 0.027 Uiso 1 1 calc R . . C13 C 1.2292(5) 0.2837(4) -0.0348(3) 0.0277(12) Uani 1 1 d . . . H13A H 1.2584 0.3346 -0.0839 0.033 Uiso 1 1 calc R . . H13B H 1.3055 0.2407 -0.0149 0.033 Uiso 1 1 calc R . . C14 C 1.1592(5) 0.3434(4) 0.0295(2) 0.0214(11) Uani 1 1 d . . . H14A H 1.0903 0.3942 0.0071 0.026 Uiso 1 1 calc R . . H14B H 1.2195 0.3833 0.0454 0.026 Uiso 1 1 calc R . . C15 C 1.1014(4) 0.2662(4) 0.1046(2) 0.0183(10) Uani 1 1 d . . . H15A H 1.1706 0.2179 0.1289 0.022 Uiso 1 1 calc R . . H15B H 1.0553 0.3060 0.1452 0.022 Uiso 1 1 calc R . . C20 C 0.9810(5) 0.0155(4) 0.2171(2) 0.0196(11) Uani 1 1 d . . . H20 H 0.9251 -0.0064 0.2693 0.024 Uiso 1 1 calc R . . C21 C 1.0012(5) -0.0797(4) 0.1758(3) 0.0251(12) Uani 1 1 d . . . H21A H 0.9183 -0.0935 0.1642 0.030 Uiso 1 1 calc R . . H21B H 1.0580 -0.0633 0.1240 0.030 Uiso 1 1 calc R . . C22 C 1.0599(6) -0.1772(4) 0.2288(3) 0.0336(13) Uani 1 1 d . . . H22A H 1.0727 -0.2366 0.2005 0.040 Uiso 1 1 calc R . . H22B H 1.0006 -0.1961 0.2791 0.040 Uiso 1 1 calc R . . C23 C 1.1884(5) -0.1589(4) 0.2493(3) 0.0346(14) Uani 1 1 d . . . H23A H 1.2231 -0.2227 0.2850 0.042 Uiso 1 1 calc R . . H23B H 1.2498 -0.1451 0.1993 0.042 Uiso 1 1 calc R . . C24 C 1.1716(5) -0.0669(4) 0.2904(3) 0.0301(13) Uani 1 1 d . . . H24A H 1.2560 -0.0533 0.2998 0.036 Uiso 1 1 calc R . . H24B H 1.1184 -0.0846 0.3434 0.036 Uiso 1 1 calc R . . C25 C 1.1086(5) 0.0330(4) 0.2402(3) 0.0252(12) Uani 1 1 d . . . H25A H 1.1676 0.0564 0.1906 0.030 Uiso 1 1 calc R . . H25B H 1.0933 0.0895 0.2713 0.030 Uiso 1 1 calc R . . C30 C 0.7864(5) 0.0919(4) 0.1109(2) 0.0192(10) Uani 1 1 d . . . H30 H 0.8361 0.0351 0.0848 0.023 Uiso 1 1 calc R . . C31 C 0.7319(5) 0.1760(4) 0.0445(3) 0.0270(12) Uani 1 1 d . . . H31A H 0.8027 0.2017 0.0031 0.032 Uiso 1 1 calc R . . H31B H 0.6881 0.2362 0.0678 0.032 Uiso 1 1 calc R . . C32 C 0.6376(5) 0.1331(4) 0.0052(3) 0.0318(13) Uani 1 1 d . . . H32A H 0.6028 0.1898 -0.0364 0.038 Uiso 1 1 calc R . . H32B H 0.6826 0.0763 -0.0215 0.038 Uiso 1 1 calc R . . C33 C 0.5291(5) 0.0910(4) 0.0676(3) 0.0314(13) Uani 1 1 d . . . H33A H 0.4807 0.1489 0.0918 0.038 Uiso 1 1 calc R . . H33B H 0.4701 0.0625 0.0413 0.038 Uiso 1 1 calc R . . C34 C 0.5795(5) 0.0056(4) 0.1329(3) 0.0294(12) Uani 1 1 d . . . H34A H 0.6188 -0.0556 0.1095 0.035 Uiso 1 1 calc R . . H34B H 0.5076 -0.0172 0.1745 0.035 Uiso 1 1 calc R . . C35 C 0.6775(5) 0.0424(4) 0.1717(3) 0.0216(11) Uani 1 1 d . . . H35A H 0.7145 -0.0182 0.2094 0.026 Uiso 1 1 calc R . . H35B H 0.6340 0.0946 0.2035 0.026 Uiso 1 1 calc R . . C40 C 0.5326(4) 0.2181(4) 0.3116(2) 0.0193(10) Uani 1 1 d . . . C41 C 0.4302(5) 0.1791(4) 0.3689(3) 0.0301(13) Uani 1 1 d . . . H41 H 0.4457 0.1439 0.4214 0.036 Uiso 1 1 calc R . . C42 C 0.3085(5) 0.1917(5) 0.3492(3) 0.0333(14) Uani 1 1 d . . . H42 H 0.2413 0.1631 0.3877 0.040 Uiso 1 1 calc R . . C43 C 0.2834(5) 0.2462(4) 0.2735(3) 0.0292(13) Uani 1 1 d . . . H43 H 0.1990 0.2562 0.2605 0.035 Uiso 1 1 calc R . . C44 C 0.3820(5) 0.2855(4) 0.2174(3) 0.0260(12) Uani 1 1 d . . . H44 H 0.3653 0.3222 0.1654 0.031 Uiso 1 1 calc R . . C45 C 0.5054(5) 0.2721(4) 0.2361(3) 0.0210(11) Uani 1 1 d . . . H45 H 0.5721 0.3001 0.1969 0.025 Uiso 1 1 calc R . . C50 C 0.7307(5) 0.0641(4) 0.3788(2) 0.0196(11) Uani 1 1 d . . . C51 C 0.8430(5) 0.0329(4) 0.4138(2) 0.0234(11) Uani 1 1 d . . . H51 H 0.8972 0.0837 0.4152 0.028 Uiso 1 1 calc R . . C52 C 0.8751(5) -0.0728(4) 0.4467(3) 0.0308(13) Uani 1 1 d . . . H52 H 0.9506 -0.0929 0.4711 0.037 Uiso 1 1 calc R . . C53 C 0.7999(6) -0.1482(4) 0.4444(3) 0.0314(13) Uani 1 1 d . . . H53 H 0.8241 -0.2201 0.4655 0.038 Uiso 1 1 calc R . . C54 C 0.6879(6) -0.1178(4) 0.4108(3) 0.0328(13) Uani 1 1 d . . . H54 H 0.6345 -0.1694 0.4098 0.039 Uiso 1 1 calc R . . C55 C 0.6526(5) -0.0129(4) 0.3786(2) 0.0241(11) Uani 1 1 d . . . H55 H 0.5752 0.0066 0.3563 0.029 Uiso 1 1 calc R . . C60 C 1.0017(4) 0.4804(3) 0.2423(2) 0.0156(10) Uani 1 1 d . . . C61 C 1.0207(5) 0.5209(4) 0.1590(2) 0.0202(11) Uani 1 1 d . . . H61 H 0.9567 0.5180 0.1276 0.024 Uiso 1 1 calc R . . C62 C 1.1309(5) 0.5648(4) 0.1221(3) 0.0264(12) Uani 1 1 d . . . H62 H 1.1423 0.5916 0.0657 0.032 Uiso 1 1 calc R . . C63 C 1.2251(5) 0.5699(4) 0.1669(3) 0.0324(13) Uani 1 1 d . . . H63 H 1.3009 0.6003 0.1416 0.039 Uiso 1 1 calc R . . C64 C 1.2076(5) 0.5302(5) 0.2485(3) 0.0412(15) Uani 1 1 d . . . H64 H 1.2725 0.5331 0.2792 0.049 Uiso 1 1 calc R . . C65 C 1.0963(5) 0.4858(4) 0.2872(3) 0.0276(12) Uani 1 1 d . . . H65 H 1.0856 0.4595 0.3436 0.033 Uiso 1 1 calc R . . C70 C 0.7379(4) 0.5431(4) 0.2710(2) 0.0154(10) Uani 1 1 d . . . C71 C 0.6161(4) 0.5349(4) 0.2520(2) 0.0181(10) Uani 1 1 d . . . H71 H 0.5922 0.4684 0.2506 0.022 Uiso 1 1 calc R . . C72 C 0.5327(5) 0.6243(4) 0.2356(3) 0.0274(12) Uani 1 1 d . . . H72 H 0.4511 0.6188 0.2229 0.033 Uiso 1 1 calc R . . C73 C 0.5657(5) 0.7224(4) 0.2373(3) 0.0298(13) Uani 1 1 d . . . H73 H 0.5074 0.7834 0.2256 0.036 Uiso 1 1 calc R . . C74 C 0.6850(5) 0.7304(4) 0.2565(3) 0.0276(12) Uani 1 1 d . . . H74 H 0.7082 0.7970 0.2582 0.033 Uiso 1 1 calc R . . C75 C 0.7685(5) 0.6425(4) 0.2727(2) 0.0228(11) Uani 1 1 d . . . H75 H 0.8496 0.6490 0.2856 0.027 Uiso 1 1 calc R . . C80 C 0.8628(4) 0.4120(4) 0.3952(2) 0.0167(10) Uani 1 1 d . . . C81 C 0.9279(5) 0.3238(4) 0.4445(3) 0.0261(12) Uani 1 1 d . . . H81 H 0.9760 0.2650 0.4264 0.031 Uiso 1 1 calc R . . C82 C 0.9077(5) 0.3400(5) 0.5250(3) 0.0319(13) Uani 1 1 d . . . H82 H 0.9402 0.2940 0.5697 0.038 Uiso 1 1 calc R . . C83 C 0.8315(5) 0.4357(5) 0.5266(3) 0.0361(14) Uani 1 1 d . . . H83 H 0.8026 0.4650 0.5730 0.043 Uiso 1 1 calc R . . C84 C 0.8048(5) 0.4816(4) 0.4479(2) 0.0248(11) Uani 1 1 d . . . H84 H 0.7566 0.5473 0.4325 0.030 Uiso 1 1 calc R . . C85 C 0.6475(4) 0.2498(4) 0.4337(2) 0.0191(10) Uani 1 1 d . . . C86 C 0.6697(5) 0.1957(4) 0.5137(2) 0.0241(11) Uani 1 1 d . . . H86 H 0.7185 0.1296 0.5266 0.029 Uiso 1 1 calc R . . C87 C 0.6078(5) 0.2562(4) 0.5692(3) 0.0249(12) Uani 1 1 d . . . H87 H 0.6081 0.2382 0.6258 0.030 Uiso 1 1 calc R . . C88 C 0.5452(5) 0.3482(4) 0.5271(3) 0.0258(12) Uani 1 1 d . . . H88 H 0.4968 0.4032 0.5501 0.031 Uiso 1 1 calc R . . C89 C 0.5674(4) 0.3441(4) 0.4440(2) 0.0214(11) Uani 1 1 d . . . H89 H 0.5344 0.3955 0.4022 0.026 Uiso 1 1 calc R . . C90 C 0.4755(4) 0.5117(4) -0.0380(2) 0.112(8) Uani 0.50 1 d PR . . H90A H 0.3848 0.5279 -0.0462 0.134 Uiso 0.50 1 calc PR . . H90B H 0.5257 0.5258 -0.0923 0.134 Uiso 0.50 1 calc PR . . H1 H 0.924(10) 0.222(8) 0.298(5) 0.168 Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru 0.0188(2) 0.0120(2) 0.01072(18) -0.00255(14) -0.00021(14) -0.00442(16) Fe 0.0205(4) 0.0265(4) 0.0109(3) -0.0055(3) -0.0002(3) -0.0066(3) Cl1 0.0319(7) 0.0176(6) 0.0149(5) -0.0030(4) -0.0045(5) -0.0043(5) Cl2 0.0770(15) 0.0746(15) 0.1289(19) -0.0440(13) 0.0289(13) -0.0372(13) P1 0.0209(6) 0.0140(6) 0.0123(5) -0.0035(4) -0.0018(5) -0.0041(5) P2 0.0187(6) 0.0164(7) 0.0110(5) -0.0023(5) -0.0014(5) -0.0050(5) P3 0.0172(6) 0.0143(6) 0.0119(5) -0.0031(4) -0.0018(4) -0.0048(5) C10 0.021(2) 0.014(2) 0.012(2) -0.0094(17) 0.0008(18) -0.003(2) C11 0.020(3) 0.018(3) 0.018(2) -0.0064(18) 0.0006(19) -0.001(2) C12 0.029(3) 0.023(3) 0.015(2) -0.0089(19) 0.006(2) -0.005(2) C13 0.029(3) 0.032(3) 0.020(2) -0.004(2) 0.003(2) -0.005(2) C14 0.029(3) 0.015(3) 0.023(2) -0.0040(19) -0.002(2) -0.009(2) C15 0.020(2) 0.022(3) 0.013(2) -0.0033(18) -0.0033(18) -0.004(2) C20 0.030(3) 0.019(3) 0.011(2) -0.0021(17) -0.0016(19) -0.007(2) C21 0.039(3) 0.019(3) 0.020(2) -0.0064(19) -0.010(2) -0.002(2) C22 0.050(4) 0.017(3) 0.037(3) -0.007(2) -0.017(3) 0.001(3) C23 0.035(3) 0.027(3) 0.038(3) -0.003(2) -0.011(2) 0.009(3) C24 0.041(3) 0.022(3) 0.028(3) 0.001(2) -0.018(2) -0.002(3) C25 0.029(3) 0.020(3) 0.027(2) -0.003(2) -0.012(2) 0.000(2) C30 0.025(3) 0.012(2) 0.022(2) -0.0068(18) -0.004(2) -0.003(2) C31 0.033(3) 0.025(3) 0.028(3) -0.007(2) -0.010(2) -0.009(2) C32 0.038(3) 0.031(3) 0.035(3) -0.015(2) -0.022(3) 0.001(3) C33 0.028(3) 0.025(3) 0.051(3) -0.021(2) -0.017(3) -0.002(3) C34 0.025(3) 0.025(3) 0.043(3) -0.014(2) -0.002(2) -0.011(2) C35 0.024(3) 0.019(3) 0.022(2) -0.0032(19) -0.002(2) -0.005(2) C40 0.019(2) 0.025(3) 0.018(2) -0.0116(19) -0.0026(19) -0.006(2) C41 0.028(3) 0.045(4) 0.017(2) -0.002(2) -0.002(2) -0.012(3) C42 0.017(3) 0.058(4) 0.026(3) -0.010(2) 0.005(2) -0.016(3) C43 0.018(3) 0.041(3) 0.033(3) -0.012(2) -0.010(2) -0.001(2) C44 0.024(3) 0.033(3) 0.024(2) -0.008(2) -0.011(2) -0.002(2) C45 0.025(3) 0.019(3) 0.020(2) -0.0050(19) -0.002(2) -0.003(2) C50 0.026(3) 0.022(3) 0.010(2) -0.0021(18) 0.0020(18) -0.006(2) C51 0.024(3) 0.027(3) 0.017(2) -0.001(2) 0.003(2) -0.006(2) C52 0.042(3) 0.028(3) 0.017(2) 0.003(2) -0.001(2) -0.002(3) C53 0.048(4) 0.020(3) 0.020(2) 0.001(2) 0.003(2) 0.000(3) C54 0.053(4) 0.025(3) 0.019(2) -0.003(2) 0.008(2) -0.018(3) C55 0.035(3) 0.023(3) 0.016(2) -0.0022(19) 0.001(2) -0.013(2) C60 0.020(2) 0.010(2) 0.015(2) -0.0016(17) 0.0021(18) -0.007(2) C61 0.024(3) 0.021(3) 0.015(2) -0.0028(18) -0.0011(19) -0.006(2) C62 0.030(3) 0.025(3) 0.026(2) -0.006(2) -0.001(2) -0.008(2) C63 0.027(3) 0.040(4) 0.029(3) -0.005(2) 0.006(2) -0.017(3) C64 0.029(3) 0.072(5) 0.027(3) -0.008(3) -0.006(2) -0.023(3) C65 0.025(3) 0.045(4) 0.013(2) 0.000(2) -0.002(2) -0.015(3) C70 0.013(2) 0.020(3) 0.012(2) -0.0024(17) 0.0018(17) -0.004(2) C71 0.018(2) 0.018(3) 0.016(2) -0.0025(18) 0.0041(18) -0.006(2) C72 0.016(3) 0.038(3) 0.024(2) -0.004(2) 0.003(2) -0.002(2) C73 0.028(3) 0.022(3) 0.029(3) 0.002(2) 0.006(2) 0.007(2) C74 0.037(3) 0.018(3) 0.024(2) -0.006(2) 0.006(2) 0.002(2) C75 0.026(3) 0.021(3) 0.022(2) -0.0093(19) 0.001(2) -0.004(2) C80 0.017(2) 0.021(3) 0.013(2) -0.0038(18) -0.0038(18) -0.003(2) C81 0.019(3) 0.036(3) 0.021(2) -0.004(2) 0.003(2) -0.006(2) C82 0.035(3) 0.047(4) 0.015(2) -0.001(2) -0.010(2) -0.010(3) C83 0.044(4) 0.057(4) 0.013(2) -0.014(2) 0.003(2) -0.025(3) C84 0.035(3) 0.030(3) 0.014(2) -0.014(2) 0.003(2) -0.013(2) C85 0.020(3) 0.022(3) 0.014(2) 0.0036(18) -0.0037(18) -0.004(2) C86 0.028(3) 0.029(3) 0.014(2) -0.0005(19) -0.006(2) -0.003(2) C87 0.029(3) 0.032(3) 0.014(2) -0.005(2) 0.001(2) -0.008(2) C88 0.027(3) 0.027(3) 0.024(3) -0.012(2) 0.004(2) -0.006(2) C89 0.024(3) 0.026(3) 0.017(2) -0.0067(19) -0.0047(19) -0.006(2) C90 0.18(2) 0.055(11) 0.105(14) -0.004(10) -0.085(15) 0.028(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru P2 2.1983(15) . ? Ru P3 2.3040(14) . ? Ru P1 2.4218(14) . ? Ru Cl1 2.4619(13) . ? Fe C85 2.025(5) . ? Fe C80 2.025(5) . ? Fe C84 2.032(5) . ? Fe C89 2.037(5) . ? Fe C86 2.038(5) . ? Fe C81 2.038(5) . ? Fe C83 2.043(6) . ? Fe C88 2.058(5) . ? Fe C82 2.063(5) . ? Fe C87 2.066(5) . ? Cl2 C90 1.519(5) . ? Cl2 C90 1.720(5) 2_665 ? P1 C10 1.849(5) . ? P1 C20 1.866(4) . ? P1 C30 1.876(5) . ? P2 C85 1.840(5) . ? P2 C40 1.845(5) . ? P2 C50 1.850(5) . ? P3 C80 1.807(4) . ? P3 C70 1.836(4) . ? P3 C60 1.853(5) . ? C10 C15 1.521(6) . ? C10 C11 1.548(6) . ? C11 C12 1.544(6) . ? C12 C13 1.522(7) . ? C13 C14 1.534(6) . ? C14 C15 1.551(6) . ? C20 C25 1.544(7) . ? C20 C21 1.545(6) . ? C21 C22 1.521(6) . ? C22 C23 1.537(8) . ? C23 C24 1.508(7) . ? C24 C25 1.539(6) . ? C30 C31 1.532(6) . ? C30 C35 1.542(6) . ? C31 C32 1.533(7) . ? C32 C33 1.519(7) . ? C33 C34 1.512(7) . ? C34 C35 1.516(7) . ? C40 C45 1.391(6) . ? C40 C41 1.416(7) . ? C41 C42 1.378(7) . ? C42 C43 1.390(6) . ? C43 C44 1.380(7) . ? C44 C45 1.390(7) . ? C50 C55 1.399(7) . ? C50 C51 1.404(7) . ? C51 C52 1.396(7) . ? C52 C53 1.370(8) . ? C53 C54 1.387(8) . ? C54 C55 1.392(7) . ? C60 C65 1.390(7) . ? C60 C61 1.406(5) . ? C61 C62 1.379(7) . ? C62 C63 1.384(7) . ? C63 C64 1.378(6) . ? C64 C65 1.399(7) . ? C70 C75 1.397(7) . ? C70 C71 1.419(6) . ? C71 C72 1.378(6) . ? C72 C73 1.390(8) . ? C73 C74 1.393(8) . ? C74 C75 1.365(7) . ? C80 C84 1.439(6) . ? C80 C81 1.443(6) . ? C81 C82 1.425(6) . ? C82 C83 1.404(8) . ? C83 C84 1.413(6) . ? C85 C89 1.433(6) . ? C85 C86 1.444(5) . ? C86 C87 1.402(7) . ? C87 C88 1.408(7) . ? C88 C89 1.423(6) . ? C90 Cl2 1.720(5) 2_665 ? 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 P2 Ru P3 97.87(5) . . ? P2 Ru P1 101.11(5) . . ? P3 Ru P1 158.69(4) . . ? P2 Ru Cl1 124.58(5) . . ? P3 Ru Cl1 88.36(4) . . ? P1 Ru Cl1 88.80(4) . . ? C85 Fe C80 106.35(18) . . ? C85 Fe C84 135.08(17) . . ? C80 Fe C84 41.55(18) . . ? C85 Fe C89 41.32(18) . . ? C80 Fe C89 109.83(17) . . ? C84 Fe C89 109.9(2) . . ? C85 Fe C86 41.64(16) . . ? C80 Fe C86 135.62(19) . . ? C84 Fe C86 176.49(17) . . ? C89 Fe C86 68.39(19) . . ? C85 Fe C81 109.8(2) . . ? C80 Fe C81 41.60(18) . . ? C84 Fe C81 68.9(2) . . ? C89 Fe C81 139.95(18) . . ? C86 Fe C81 110.2(2) . . ? C85 Fe C83 175.45(18) . . ? C80 Fe C83 69.37(19) . . ? C84 Fe C83 40.57(18) . . ? C89 Fe C83 137.9(2) . . ? C86 Fe C83 142.66(18) . . ? C81 Fe C83 68.2(2) . . ? C85 Fe C88 69.4(2) . . ? C80 Fe C88 140.54(18) . . ? C84 Fe C88 113.2(2) . . ? C89 Fe C88 40.66(17) . . ? C86 Fe C88 67.7(2) . . ? C81 Fe C88 177.7(2) . . ? C83 Fe C88 112.8(2) . . ? C85 Fe C82 140.8(2) . . ? C80 Fe C82 69.38(18) . . ? C84 Fe C82 68.1(2) . . ? C89 Fe C82 177.8(2) . . ? C86 Fe C82 113.7(2) . . ? C81 Fe C82 40.66(19) . . ? C83 Fe C82 40.0(2) . . ? C88 Fe C82 138.85(19) . . ? C85 Fe C87 69.09(18) . . ? C80 Fe C87 175.3(2) . . ? C84 Fe C87 142.8(2) . . ? C89 Fe C87 67.79(18) . . ? C86 Fe C87 39.95(19) . . ? C81 Fe C87 137.8(2) . . ? C83 Fe C87 115.22(19) . . ? C88 Fe C87 39.93(19) . . ? C82 Fe C87 113.16(19) . . ? C90 Cl2 C90 52.6(3) . 2_665 ? C10 P1 C20 108.6(2) . . ? C10 P1 C30 101.9(2) . . ? C20 P1 C30 102.8(2) . . ? C10 P1 Ru 101.01(15) . . ? C20 P1 Ru 117.16(14) . . ? C30 P1 Ru 123.65(15) . . ? C85 P2 C40 96.1(2) . . ? C85 P2 C50 98.20(19) . . ? C40 P2 C50 104.3(2) . . ? C85 P2 Ru 123.77(16) . . ? C40 P2 Ru 114.27(15) . . ? C50 P2 Ru 116.70(15) . . ? C80 P3 C70 101.88(19) . . ? C80 P3 C60 100.9(2) . . ? C70 P3 C60 99.7(2) . . ? C80 P3 Ru 120.38(16) . . ? C70 P3 Ru 121.06(15) . . ? C60 P3 Ru 109.35(15) . . ? C15 C10 C11 109.4(4) . . ? C15 C10 P1 114.7(3) . . ? C11 C10 P1 119.1(3) . . ? C12 C11 C10 109.7(4) . . ? C13 C12 C11 112.4(4) . . ? C12 C13 C14 111.8(4) . . ? C13 C14 C15 110.6(4) . . ? C10 C15 C14 109.9(3) . . ? C25 C20 C21 109.6(4) . . ? C25 C20 P1 112.1(3) . . ? C21 C20 P1 117.5(3) . . ? C22 C21 C20 111.2(4) . . ? C21 C22 C23 111.3(5) . . ? C24 C23 C22 110.3(4) . . ? C23 C24 C25 112.0(4) . . ? C24 C25 C20 112.4(4) . . ? C31 C30 C35 110.3(4) . . ? C31 C30 P1 114.2(3) . . ? C35 C30 P1 110.0(3) . . ? C30 C31 C32 111.6(4) . . ? C33 C32 C31 110.6(4) . . ? C34 C33 C32 110.8(4) . . ? C33 C34 C35 112.0(4) . . ? C34 C35 C30 113.7(4) . . ? C45 C40 C41 117.9(4) . . ? C45 C40 P2 120.6(3) . . ? C41 C40 P2 121.4(3) . . ? C42 C41 C40 120.7(4) . . ? C41 C42 C43 120.4(5) . . ? C44 C43 C42 119.4(4) . . ? C43 C44 C45 120.6(4) . . ? C44 C45 C40 120.8(4) . . ? C55 C50 C51 118.3(4) . . ? C55 C50 P2 124.7(4) . . ? C51 C50 P2 117.0(4) . . ? C52 C51 C50 120.1(5) . . ? C53 C52 C51 121.3(5) . . ? C52 C53 C54 119.0(5) . . ? C53 C54 C55 121.0(5) . . ? C54 C55 C50 120.3(5) . . ? C65 C60 C61 118.6(4) . . ? C65 C60 P3 121.7(3) . . ? C61 C60 P3 119.7(3) . . ? C62 C61 C60 121.0(4) . . ? C61 C62 C63 120.2(4) . . ? C64 C63 C62 119.2(5) . . ? C63 C64 C65 121.5(5) . . ? C60 C65 C64 119.5(4) . . ? C75 C70 C71 118.2(4) . . ? C75 C70 P3 122.3(3) . . ? C71 C70 P3 119.5(4) . . ? C72 C71 C70 119.5(5) . . ? C71 C72 C73 121.2(5) . . ? C72 C73 C74 119.4(5) . . ? C75 C74 C73 120.0(5) . . ? C74 C75 C70 121.8(5) . . ? C84 C80 C81 106.1(4) . . ? C84 C80 P3 128.3(3) . . ? C81 C80 P3 125.5(4) . . ? C84 C80 Fe 69.5(3) . . ? C81 C80 Fe 69.7(3) . . ? P3 C80 Fe 122.5(2) . . ? C82 C81 C80 108.4(5) . . ? C82 C81 Fe 70.6(3) . . ? C80 C81 Fe 68.7(3) . . ? C83 C82 C81 108.0(4) . . ? C83 C82 Fe 69.2(3) . . ? C81 C82 Fe 68.7(3) . . ? C82 C83 C84 108.9(4) . . ? C82 C83 Fe 70.8(3) . . ? C84 C83 Fe 69.3(3) . . ? C83 C84 C80 108.5(5) . . ? C83 C84 Fe 70.1(3) . . ? C80 C84 Fe 68.9(3) . . ? C89 C85 C86 105.5(4) . . ? C89 C85 P2 125.0(3) . . ? C86 C85 P2 129.2(4) . . ? C89 C85 Fe 69.8(3) . . ? C86 C85 Fe 69.7(3) . . ? P2 C85 Fe 129.2(2) . . ? C87 C86 C85 109.2(4) . . ? C87 C86 Fe 71.1(3) . . ? C85 C86 Fe 68.7(3) . . ? C86 C87 C88 108.5(4) . . ? C86 C87 Fe 68.9(3) . . ? C88 C87 Fe 69.7(3) . . ? C87 C88 C89 107.8(4) . . ? C87 C88 Fe 70.3(3) . . ? C89 C88 Fe 68.9(3) . . ? C88 C89 C85 108.9(4) . . ? C88 C89 Fe 70.5(3) . . ? C85 C89 Fe 68.9(3) . . ? Cl2 C90 Cl2 127.4(3) . 2_665 ? 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 P2 Ru P1 C10 177.84(15) . . . . ? P3 Ru P1 C10 -29.62(19) . . . . ? Cl1 Ru P1 C10 52.77(15) . . . . ? P2 Ru P1 C20 -64.45(18) . . . . ? P3 Ru P1 C20 88.1(2) . . . . ? Cl1 Ru P1 C20 170.49(18) . . . . ? P2 Ru P1 C30 65.45(17) . . . . ? P3 Ru P1 C30 -142.01(18) . . . . ? Cl1 Ru P1 C30 -59.61(17) . . . . ? P3 Ru P2 C85 -10.70(17) . . . . ? P1 Ru P2 C85 159.56(17) . . . . ? Cl1 Ru P2 C85 -104.15(17) . . . . ? P3 Ru P2 C40 105.45(17) . . . . ? P1 Ru P2 C40 -84.29(17) . . . . ? Cl1 Ru P2 C40 12.00(18) . . . . ? P3 Ru P2 C50 -132.60(17) . . . . ? P1 Ru P2 C50 37.65(17) . . . . ? Cl1 Ru P2 C50 133.94(16) . . . . ? P2 Ru P3 C80 43.84(18) . . . . ? P1 Ru P3 C80 -109.0(2) . . . . ? Cl1 Ru P3 C80 168.54(18) . . . . ? P2 Ru P3 C70 -85.32(16) . . . . ? P1 Ru P3 C70 121.85(18) . . . . ? Cl1 Ru P3 C70 39.38(16) . . . . ? P2 Ru P3 C60 159.83(14) . . . . ? P1 Ru P3 C60 7.01(18) . . . . ? Cl1 Ru P3 C60 -75.47(14) . . . . ? C20 P1 C10 C15 -81.2(4) . . . . ? C30 P1 C10 C15 170.8(3) . . . . ? Ru P1 C10 C15 42.6(3) . . . . ? C20 P1 C10 C11 51.3(4) . . . . ? C30 P1 C10 C11 -56.7(4) . . . . ? Ru P1 C10 C11 175.1(3) . . . . ? C15 C10 C11 C12 -59.4(5) . . . . ? P1 C10 C11 C12 165.9(3) . . . . ? C10 C11 C12 C13 55.3(5) . . . . ? C11 C12 C13 C14 -52.9(5) . . . . ? C12 C13 C14 C15 53.7(5) . . . . ? C11 C10 C15 C14 61.3(5) . . . . ? P1 C10 C15 C14 -161.8(3) . . . . ? C13 C14 C15 C10 -58.4(5) . . . . ? C10 P1 C20 C25 51.9(4) . . . . ? C30 P1 C20 C25 159.3(3) . . . . ? Ru P1 C20 C25 -61.7(4) . . . . ? C10 P1 C20 C21 -76.4(4) . . . . ? C30 P1 C20 C21 31.0(4) . . . . ? Ru P1 C20 C21 170.1(3) . . . . ? C25 C20 C21 C22 55.5(5) . . . . ? P1 C20 C21 C22 -175.0(4) . . . . ? C20 C21 C22 C23 -58.4(6) . . . . ? C21 C22 C23 C24 57.6(6) . . . . ? C22 C23 C24 C25 -55.1(6) . . . . ? C23 C24 C25 C20 54.3(6) . . . . ? C21 C20 C25 C24 -53.3(5) . . . . ? P1 C20 C25 C24 174.3(3) . . . . ? C10 P1 C30 C31 -51.3(4) . . . . ? C20 P1 C30 C31 -163.8(3) . . . . ? Ru P1 C30 C31 60.6(4) . . . . ? C10 P1 C30 C35 -176.0(3) . . . . ? C20 P1 C30 C35 71.6(3) . . . . ? Ru P1 C30 C35 -64.0(3) . . . . ? C35 C30 C31 C32 -53.1(5) . . . . ? P1 C30 C31 C32 -177.5(4) . . . . ? C30 C31 C32 C33 57.8(6) . . . . ? C31 C32 C33 C34 -58.1(6) . . . . ? C32 C33 C34 C35 55.2(6) . . . . ? C33 C34 C35 C30 -52.2(6) . . . . ? C31 C30 C35 C34 50.6(5) . . . . ? P1 C30 C35 C34 177.4(3) . . . . ? C85 P2 C40 C45 129.9(4) . . . . ? C50 P2 C40 C45 -130.1(4) . . . . ? Ru P2 C40 C45 -1.5(4) . . . . ? C85 P2 C40 C41 -46.0(5) . . . . ? C50 P2 C40 C41 54.1(5) . . . . ? Ru P2 C40 C41 -177.3(4) . . . . ? C45 C40 C41 C42 2.0(8) . . . . ? P2 C40 C41 C42 177.9(4) . . . . ? C40 C41 C42 C43 -2.2(9) . . . . ? C41 C42 C43 C44 1.5(8) . . . . ? C42 C43 C44 C45 -0.6(8) . . . . ? C43 C44 C45 C40 0.4(8) . . . . ? C41 C40 C45 C44 -1.1(7) . . . . ? P2 C40 C45 C44 -177.1(4) . . . . ? C85 P2 C50 C55 105.3(4) . . . . ? C40 P2 C50 C55 6.9(4) . . . . ? Ru P2 C50 C55 -120.2(4) . . . . ? C85 P2 C50 C51 -73.4(4) . . . . ? C40 P2 C50 C51 -171.8(3) . . . . ? Ru P2 C50 C51 61.1(4) . . . . ? C55 C50 C51 C52 0.6(6) . . . . ? P2 C50 C51 C52 179.4(3) . . . . ? C50 C51 C52 C53 1.1(7) . . . . ? C51 C52 C53 C54 -1.9(7) . . . . ? C52 C53 C54 C55 1.1(7) . . . . ? C53 C54 C55 C50 0.6(7) . . . . ? C51 C50 C55 C54 -1.4(7) . . . . ? P2 C50 C55 C54 179.9(3) . . . . ? C80 P3 C60 C65 10.1(5) . . . . ? C70 P3 C60 C65 114.3(4) . . . . ? Ru P3 C60 C65 -117.8(4) . . . . ? C80 P3 C60 C61 -168.3(4) . . . . ? C70 P3 C60 C61 -64.1(4) . . . . ? Ru P3 C60 C61 63.8(4) . . . . ? C65 C60 C61 C62 0.3(7) . . . . ? P3 C60 C61 C62 178.7(4) . . . . ? C60 C61 C62 C63 -0.1(7) . . . . ? C61 C62 C63 C64 0.3(8) . . . . ? C62 C63 C64 C65 -0.5(9) . . . . ? C61 C60 C65 C64 -0.5(8) . . . . ? P3 C60 C65 C64 -178.9(4) . . . . ? C63 C64 C65 C60 0.7(9) . . . . ? C80 P3 C70 C75 67.6(4) . . . . ? C60 P3 C70 C75 -35.8(4) . . . . ? Ru P3 C70 C75 -155.5(3) . . . . ? C80 P3 C70 C71 -113.9(4) . . . . ? C60 P3 C70 C71 142.7(3) . . . . ? Ru P3 C70 C71 23.0(4) . . . . ? C75 C70 C71 C72 0.3(6) . . . . ? P3 C70 C71 C72 -178.2(3) . . . . ? C70 C71 C72 C73 0.0(6) . . . . ? C71 C72 C73 C74 -0.4(7) . . . . ? C72 C73 C74 C75 0.5(7) . . . . ? C73 C74 C75 C70 -0.2(7) . . . . ? C71 C70 C75 C74 -0.2(6) . . . . ? P3 C70 C75 C74 178.3(3) . . . . ? C70 P3 C80 C84 -3.7(5) . . . . ? C60 P3 C80 C84 98.8(5) . . . . ? Ru P3 C80 C84 -141.0(4) . . . . ? C70 P3 C80 C81 172.0(4) . . . . ? C60 P3 C80 C81 -85.6(4) . . . . ? Ru P3 C80 C81 34.7(5) . . . . ? C70 P3 C80 Fe 84.8(3) . . . . ? C60 P3 C80 Fe -172.7(3) . . . . ? Ru P3 C80 Fe -52.4(3) . . . . ? C85 Fe C80 C84 141.4(3) . . . . ? C89 Fe C80 C84 98.0(3) . . . . ? C86 Fe C80 C84 177.0(3) . . . . ? C81 Fe C80 C84 -117.0(4) . . . . ? C83 Fe C80 C84 -37.0(3) . . . . ? C88 Fe C80 C84 64.2(4) . . . . ? C82 Fe C80 C84 -79.8(3) . . . . ? C87 Fe C80 C84 157(2) . . . . ? C85 Fe C80 C81 -101.6(3) . . . . ? C84 Fe C80 C81 117.0(4) . . . . ? C89 Fe C80 C81 -145.0(3) . . . . ? C86 Fe C80 C81 -66.1(4) . . . . ? C83 Fe C80 C81 80.0(3) . . . . ? C88 Fe C80 C81 -178.9(3) . . . . ? C82 Fe C80 C81 37.2(3) . . . . ? C87 Fe C80 C81 -86(2) . . . . ? C85 Fe C80 P3 18.3(3) . . . . ? C84 Fe C80 P3 -123.1(4) . . . . ? C89 Fe C80 P3 -25.1(3) . . . . ? C86 Fe C80 P3 53.8(4) . . . . ? C81 Fe C80 P3 119.9(4) . . . . ? C83 Fe C80 P3 -160.1(3) . . . . ? C88 Fe C80 P3 -59.0(4) . . . . ? C82 Fe C80 P3 157.1(3) . . . . ? C87 Fe C80 P3 34(2) . . . . ? C84 C80 C81 C82 0.7(6) . . . . ? P3 C80 C81 C82 -175.8(4) . . . . ? Fe C80 C81 C82 -59.6(4) . . . . ? C84 C80 C81 Fe 60.3(3) . . . . ? P3 C80 C81 Fe -116.2(4) . . . . ? C85 Fe C81 C82 -147.6(3) . . . . ? C80 Fe C81 C82 119.8(4) . . . . ? C84 Fe C81 C82 80.5(3) . . . . ? C89 Fe C81 C82 176.7(3) . . . . ? C86 Fe C81 C82 -103.1(3) . . . . ? C83 Fe C81 C82 36.8(3) . . . . ? C88 Fe C81 C82 -79(5) . . . . ? C87 Fe C81 C82 -67.2(4) . . . . ? C85 Fe C81 C80 92.6(3) . . . . ? C84 Fe C81 C80 -39.3(3) . . . . ? C89 Fe C81 C80 56.9(4) . . . . ? C86 Fe C81 C80 137.0(3) . . . . ? C83 Fe C81 C80 -83.0(3) . . . . ? C88 Fe C81 C80 161(5) . . . . ? C82 Fe C81 C80 -119.8(4) . . . . ? C87 Fe C81 C80 172.9(3) . . . . ? C80 C81 C82 C83 0.2(6) . . . . ? Fe C81 C82 C83 -58.3(4) . . . . ? C80 C81 C82 Fe 58.4(3) . . . . ? C85 Fe C82 C83 173.0(3) . . . . ? C80 Fe C82 C83 82.1(3) . . . . ? C84 Fe C82 C83 37.4(3) . . . . ? C89 Fe C82 C83 13(5) . . . . ? C86 Fe C82 C83 -145.9(3) . . . . ? C81 Fe C82 C83 120.1(4) . . . . ? C88 Fe C82 C83 -63.3(4) . . . . ? C87 Fe C82 C83 -102.2(3) . . . . ? C85 Fe C82 C81 52.9(4) . . . . ? C80 Fe C82 C81 -38.0(3) . . . . ? C84 Fe C82 C81 -82.7(3) . . . . ? C89 Fe C82 C81 -107(5) . . . . ? C86 Fe C82 C81 94.0(3) . . . . ? C83 Fe C82 C81 -120.1(4) . . . . ? C88 Fe C82 C81 176.6(3) . . . . ? C87 Fe C82 C81 137.7(3) . . . . ? C81 C82 C83 C84 -1.0(6) . . . . ? Fe C82 C83 C84 -59.0(4) . . . . ? C81 C82 C83 Fe 57.9(4) . . . . ? C85 Fe C83 C82 -102(3) . . . . ? C80 Fe C83 C82 -82.1(3) . . . . ? C84 Fe C83 C82 -120.0(4) . . . . ? C89 Fe C83 C82 -179.3(3) . . . . ? C86 Fe C83 C82 57.8(4) . . . . ? C81 Fe C83 C82 -37.4(3) . . . . ? C88 Fe C83 C82 140.4(3) . . . . ? C87 Fe C83 C82 96.6(3) . . . . ? C85 Fe C83 C84 18(3) . . . . ? C80 Fe C83 C84 37.8(3) . . . . ? C89 Fe C83 C84 -59.3(4) . . . . ? C86 Fe C83 C84 177.8(3) . . . . ? C81 Fe C83 C84 82.6(3) . . . . ? C88 Fe C83 C84 -99.6(3) . . . . ? C82 Fe C83 C84 120.0(4) . . . . ? C87 Fe C83 C84 -143.4(3) . . . . ? C82 C83 C84 C80 1.5(6) . . . . ? Fe C83 C84 C80 -58.4(3) . . . . ? C82 C83 C84 Fe 59.9(4) . . . . ? C81 C80 C84 C83 -1.3(6) . . . . ? P3 C80 C84 C83 175.0(4) . . . . ? Fe C80 C84 C83 59.1(4) . . . . ? C81 C80 C84 Fe -60.4(3) . . . . ? P3 C80 C84 Fe 115.9(4) . . . . ? C85 Fe C84 C83 -178.0(3) . . . . ? C80 Fe C84 C83 -120.1(4) . . . . ? C89 Fe C84 C83 142.1(3) . . . . ? C86 Fe C84 C83 -157(3) . . . . ? C81 Fe C84 C83 -80.7(3) . . . . ? C88 Fe C84 C83 98.4(3) . . . . ? C82 Fe C84 C83 -36.9(3) . . . . ? C87 Fe C84 C83 63.0(5) . . . . ? C85 Fe C84 C80 -58.0(4) . . . . ? C89 Fe C84 C80 -97.8(3) . . . . ? C86 Fe C84 C80 -37(3) . . . . ? C81 Fe C84 C80 39.4(3) . . . . ? C83 Fe C84 C80 120.1(4) . . . . ? C88 Fe C84 C80 -141.5(3) . . . . ? C82 Fe C84 C80 83.2(3) . . . . ? C87 Fe C84 C80 -176.9(3) . . . . ? C40 P2 C85 C89 -51.3(5) . . . . ? C50 P2 C85 C89 -156.7(4) . . . . ? Ru P2 C85 C89 73.3(5) . . . . ? C40 P2 C85 C86 122.0(5) . . . . ? C50 P2 C85 C86 16.6(5) . . . . ? Ru P2 C85 C86 -113.3(4) . . . . ? C40 P2 C85 Fe -142.9(3) . . . . ? C50 P2 C85 Fe 111.7(3) . . . . ? Ru P2 C85 Fe -18.3(4) . . . . ? C80 Fe C85 C89 -101.6(3) . . . . ? C84 Fe C85 C89 -65.8(4) . . . . ? C86 Fe C85 C89 116.1(4) . . . . ? C81 Fe C85 C89 -145.4(3) . . . . ? C83 Fe C85 C89 -82(3) . . . . ? C88 Fe C85 C89 36.9(2) . . . . ? C82 Fe C85 C89 -178.9(3) . . . . ? C87 Fe C85 C89 79.7(3) . . . . ? C80 Fe C85 C86 142.3(3) . . . . ? C84 Fe C85 C86 178.1(3) . . . . ? C89 Fe C85 C86 -116.1(4) . . . . ? C81 Fe C85 C86 98.5(3) . . . . ? C83 Fe C85 C86 162(3) . . . . ? C88 Fe C85 C86 -79.2(3) . . . . ? C82 Fe C85 C86 65.0(4) . . . . ? C87 Fe C85 C86 -36.4(3) . . . . ? C80 Fe C85 P2 17.7(3) . . . . ? C84 Fe C85 P2 53.5(4) . . . . ? C89 Fe C85 P2 119.3(4) . . . . ? C86 Fe C85 P2 -124.6(4) . . . . ? C81 Fe C85 P2 -26.1(3) . . . . ? C83 Fe C85 P2 37(3) . . . . ? C88 Fe C85 P2 156.2(3) . . . . ? C82 Fe C85 P2 -59.6(4) . . . . ? C87 Fe C85 P2 -161.0(3) . . . . ? C89 C85 C86 C87 -1.2(6) . . . . ? P2 C85 C86 C87 -175.6(4) . . . . ? Fe C85 C86 C87 59.8(4) . . . . ? C89 C85 C86 Fe -61.0(3) . . . . ? P2 C85 C86 Fe 124.6(4) . . . . ? C85 Fe C86 C87 -120.4(4) . . . . ? C80 Fe C86 C87 -177.5(3) . . . . ? C84 Fe C86 C87 -142(3) . . . . ? C89 Fe C86 C87 -80.8(3) . . . . ? C81 Fe C86 C87 142.2(3) . . . . ? C83 Fe C86 C87 61.9(5) . . . . ? C88 Fe C86 C87 -36.8(3) . . . . ? C82 Fe C86 C87 98.4(3) . . . . ? C80 Fe C86 C85 -57.1(4) . . . . ? C84 Fe C86 C85 -22(3) . . . . ? C89 Fe C86 C85 39.6(3) . . . . ? C81 Fe C86 C85 -97.4(3) . . . . ? C83 Fe C86 C85 -177.7(3) . . . . ? C88 Fe C86 C85 83.6(3) . . . . ? C82 Fe C86 C85 -141.2(3) . . . . ? C87 Fe C86 C85 120.4(4) . . . . ? C85 C86 C87 C88 0.4(6) . . . . ? Fe C86 C87 C88 58.6(4) . . . . ? C85 C86 C87 Fe -58.3(3) . . . . ? C85 Fe C87 C86 37.8(3) . . . . ? C80 Fe C87 C86 22(2) . . . . ? C84 Fe C87 C86 176.5(3) . . . . ? C89 Fe C87 C86 82.4(3) . . . . ? C81 Fe C87 C86 -59.0(4) . . . . ? C83 Fe C87 C86 -143.7(3) . . . . ? C88 Fe C87 C86 120.3(4) . . . . ? C82 Fe C87 C86 -99.8(3) . . . . ? C85 Fe C87 C88 -82.5(3) . . . . ? C80 Fe C87 C88 -99(2) . . . . ? C84 Fe C87 C88 56.1(4) . . . . ? C89 Fe C87 C88 -37.9(3) . . . . ? C86 Fe C87 C88 -120.3(4) . . . . ? C81 Fe C87 C88 -179.3(3) . . . . ? C83 Fe C87 C88 95.9(3) . . . . ? C82 Fe C87 C88 139.9(3) . . . . ? C86 C87 C88 C89 0.7(6) . . . . ? Fe C87 C88 C89 58.9(3) . . . . ? C86 C87 C88 Fe -58.2(4) . . . . ? C85 Fe C88 C87 81.7(3) . . . . ? C80 Fe C88 C87 172.6(3) . . . . ? C84 Fe C88 C87 -146.9(3) . . . . ? C89 Fe C88 C87 119.1(4) . . . . ? C86 Fe C88 C87 36.8(3) . . . . ? C81 Fe C88 C87 12(5) . . . . ? C83 Fe C88 C87 -102.6(3) . . . . ? C82 Fe C88 C87 -64.2(4) . . . . ? C85 Fe C88 C89 -37.5(3) . . . . ? C80 Fe C88 C89 53.5(4) . . . . ? C84 Fe C88 C89 94.0(3) . . . . ? C86 Fe C88 C89 -82.3(3) . . . . ? C81 Fe C88 C89 -107(5) . . . . ? C83 Fe C88 C89 138.2(3) . . . . ? C82 Fe C88 C89 176.7(3) . . . . ? C87 Fe C88 C89 -119.1(4) . . . . ? C87 C88 C89 C85 -1.5(6) . . . . ? Fe C88 C89 C85 58.3(3) . . . . ? C87 C88 C89 Fe -59.8(4) . . . . ? C86 C85 C89 C88 1.7(5) . . . . ? P2 C85 C89 C88 176.3(4) . . . . ? Fe C85 C89 C88 -59.2(3) . . . . ? C86 C85 C89 Fe 60.9(3) . . . . ? P2 C85 C89 Fe -124.4(4) . . . . ? C85 Fe C89 C88 120.4(4) . . . . ? C80 Fe C89 C88 -147.1(3) . . . . ? C84 Fe C89 C88 -102.8(3) . . . . ? C86 Fe C89 C88 80.5(3) . . . . ? C81 Fe C89 C88 176.6(3) . . . . ? C83 Fe C89 C88 -66.3(4) . . . . ? C82 Fe C89 C88 -78(5) . . . . ? C87 Fe C89 C88 37.3(3) . . . . ? C80 Fe C89 C85 92.5(3) . . . . ? C84 Fe C89 C85 136.8(2) . . . . ? C86 Fe C89 C85 -39.9(2) . . . . ? C81 Fe C89 C85 56.2(4) . . . . ? C83 Fe C89 C85 173.3(3) . . . . ? C88 Fe C89 C85 -120.4(4) . . . . ? C82 Fe C89 C85 161(5) . . . . ? C87 Fe C89 C85 -83.1(3) . . . . ? C90 Cl2 C90 Cl2 0.0 2_665 . . 2_665 ? _diffrn_measured_fraction_theta_max 0.940 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.940 _refine_diff_density_max 0.561 _refine_diff_density_min -0.801 _refine_diff_density_rms 0.091 #===END data_sj5cb _database_code_depnum_ccdc_archive 'CCDC 224061' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point '55_C (dec.)' _chemical_formula_moiety ? _chemical_formula_sum 'C25 H54 B Cl F4 O P2 Ru' _chemical_formula_weight 655.95 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.4966(4) _cell_length_b 22.3036(11) _cell_length_c 17.4068(9) _cell_angle_alpha 90.00 _cell_angle_beta 103.7990(10) _cell_angle_gamma 90.00 _cell_volume 3203.5(3) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 6810 _cell_measurement_theta_min 2.410 _cell_measurement_theta_max 28.182 _exptl_crystal_description cube _exptl_crystal_colour orange _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.360 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1376 _exptl_absorpt_coefficient_mu 0.712 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details 'SADABS2.0 (Sheldrick 2000)' _exptl_special_details ; The BF4-counterion is rotational disordered (axis B1-F2). Two independent positions were found and refined anisotropically with an occupation of 60:40. ; _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 Smart Apex with D8-Goniometer' _diffrn_measurement_method 'omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 36984 _diffrn_reflns_av_R_equivalents 0.0255 _diffrn_reflns_av_sigmaI/netI 0.0158 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.51 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5638 _reflns_number_gt 5480 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART-NT V5.6' _computing_cell_refinement 'SAINT-NT V6.0' _computing_data_reduction 'SAINT-NT V6.0' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XSHELL in SHELXTL-97' _computing_publication_material 'XSHELL in SHELXTL-97' _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^)+(0.0294P)^2^+2.8130P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary Patterson _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 5638 _refine_ls_number_parameters 358 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0301 _refine_ls_R_factor_gt 0.0289 _refine_ls_wR_factor_ref 0.0690 _refine_ls_wR_factor_gt 0.0683 _refine_ls_goodness_of_fit_ref 1.142 _refine_ls_restrained_S_all 1.142 _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 B1 B 0.8719(5) 0.26661(16) 0.5202(2) 0.0470(8) Uani 1 1 d . . . C1 C 0.0605(3) 0.47190(10) 0.70299(15) 0.0279(5) Uani 1 1 d . . . C2 C 0.3569(3) 0.43231(10) 0.70927(13) 0.0248(5) Uani 1 1 d . . . H2 H 0.4663 0.4219 0.7327 0.030 Uiso 1 1 calc R . . C3 C 0.3057(3) 0.41419(11) 0.62451(13) 0.0276(5) Uani 1 1 d . . . H3A H 0.2696 0.4506 0.5927 0.033 Uiso 1 1 calc R . . H3B H 0.2105 0.3875 0.6183 0.033 Uiso 1 1 calc R . . C4 C 0.4335(3) 0.38197(12) 0.58877(15) 0.0346(6) Uani 1 1 d . . . C5 C 0.5889(4) 0.41827(19) 0.6011(2) 0.0701(12) Uani 1 1 d . . . H5A H 0.6628 0.3989 0.5732 0.105 Uiso 1 1 calc R . . H5B H 0.6406 0.4204 0.6577 0.105 Uiso 1 1 calc R . . H5C H 0.5636 0.4589 0.5803 0.105 Uiso 1 1 calc R . . C6 C 0.3595(4) 0.37490(13) 0.50018(15) 0.0435(7) Uani 1 1 d . . . H6A H 0.3362 0.4146 0.4759 0.065 Uiso 1 1 calc R . . H6B H 0.2588 0.3518 0.4921 0.065 Uiso 1 1 calc R . . H6C H 0.4361 0.3538 0.4756 0.065 Uiso 1 1 calc R . . C7 C 0.4702(4) 0.31960(14) 0.62549(17) 0.0479(7) Uani 1 1 d . . . H7A H 0.3710 0.2955 0.6139 0.072 Uiso 1 1 calc R . . H7B H 0.5107 0.3234 0.6829 0.072 Uiso 1 1 calc R . . H7C H 0.5525 0.3000 0.6032 0.072 Uiso 1 1 calc R . . C8 C 0.2033(3) 0.61358(11) 0.66754(15) 0.0326(6) Uani 1 1 d . . . H8 H 0.2576 0.6531 0.6657 0.039 Uiso 1 1 calc R . . C9 C 0.2185(4) 0.57880(13) 0.59315(16) 0.0455(7) Uani 1 1 d . . . H9A H 0.1577 0.5412 0.5898 0.068 Uiso 1 1 calc R . . H9B H 0.3328 0.5700 0.5964 0.068 Uiso 1 1 calc R . . H9C H 0.1745 0.6031 0.5460 0.068 Uiso 1 1 calc R . . C10 C 0.0250(3) 0.62699(13) 0.66308(17) 0.0422(7) Uani 1 1 d . . . H10A H -0.0215 0.6492 0.6144 0.063 Uiso 1 1 calc R . . H10B H 0.0162 0.6511 0.7089 0.063 Uiso 1 1 calc R . . H10C H -0.0341 0.5892 0.6631 0.063 Uiso 1 1 calc R . . C11 C 0.5299(3) 0.59435(12) 0.77123(18) 0.0393(6) Uani 1 1 d . . . H11 H 0.5834 0.5875 0.8283 0.047 Uiso 1 1 calc R . . C12 C 0.6181(3) 0.55447(15) 0.7245(2) 0.0522(8) Uani 1 1 d . . . H12A H 0.5712 0.5599 0.6678 0.078 Uiso 1 1 calc R . . H12B H 0.6067 0.5125 0.7388 0.078 Uiso 1 1 calc R . . H12C H 0.7331 0.5653 0.7368 0.078 Uiso 1 1 calc R . . C13 C 0.5576(4) 0.66086(14) 0.7550(3) 0.0694(11) Uani 1 1 d . . . H13A H 0.6727 0.6706 0.7746 0.104 Uiso 1 1 calc R . . H13B H 0.4930 0.6859 0.7821 0.104 Uiso 1 1 calc R . . H13C H 0.5249 0.6684 0.6979 0.104 Uiso 1 1 calc R . . C14 C 0.2531(3) 0.62144(11) 0.83878(15) 0.0322(6) Uani 1 1 d . . . H14 H 0.2227 0.6623 0.8165 0.039 Uiso 1 1 calc R . . C15 C 0.1029(4) 0.59456(13) 0.85948(18) 0.0467(7) Uani 1 1 d . . . H15A H 0.1319 0.5567 0.8879 0.070 Uiso 1 1 calc R . . H15B H 0.0197 0.5871 0.8108 0.070 Uiso 1 1 calc R . . H15C H 0.0608 0.6226 0.8930 0.070 Uiso 1 1 calc R . . C16 C 0.3860(4) 0.62960(13) 0.91482(17) 0.0506(8) Uani 1 1 d . . . H16A H 0.3445 0.6542 0.9523 0.076 Uiso 1 1 calc R . . H16B H 0.4797 0.6495 0.9024 0.076 Uiso 1 1 calc R . . H16C H 0.4188 0.5903 0.9384 0.076 Uiso 1 1 calc R . . C17 C 0.0472(3) 0.40200(11) 0.90592(15) 0.0295(5) Uani 1 1 d . . . H17 H 0.0019 0.3644 0.9233 0.035 Uiso 1 1 calc R . . C18 C 0.1453(3) 0.43282(12) 0.98065(15) 0.0370(6) Uani 1 1 d . . . H18A H 0.2029 0.4673 0.9658 0.055 Uiso 1 1 calc R . . H18B H 0.2238 0.4044 1.0112 0.055 Uiso 1 1 calc R . . H18C H 0.0720 0.4464 1.0128 0.055 Uiso 1 1 calc R . . C19 C -0.0978(3) 0.44036(12) 0.86358(17) 0.0382(6) Uani 1 1 d . . . H19A H -0.1745 0.4443 0.8973 0.057 Uiso 1 1 calc R . . H19B H -0.1518 0.4211 0.8136 0.057 Uiso 1 1 calc R . . H19C H -0.0596 0.4802 0.8527 0.057 Uiso 1 1 calc R . . C20 C 0.3419(3) 0.33736(10) 0.89940(14) 0.0270(5) Uani 1 1 d . . . H20 H 0.3914 0.3654 0.9433 0.032 Uiso 1 1 calc R . . C21 C 0.4802(3) 0.32101(11) 0.86061(15) 0.0334(6) Uani 1 1 d . . . H21A H 0.5699 0.3035 0.9003 0.050 Uiso 1 1 calc R . . H21B H 0.5179 0.3572 0.8385 0.050 Uiso 1 1 calc R . . H21C H 0.4413 0.2919 0.8182 0.050 Uiso 1 1 calc R . . C22 C 0.2887(3) 0.28275(12) 0.94034(16) 0.0395(6) Uani 1 1 d . . . H22A H 0.2468 0.2517 0.9009 0.059 Uiso 1 1 calc R . . H22B H 0.2036 0.2947 0.9666 0.059 Uiso 1 1 calc R . . H22C H 0.3817 0.2669 0.9797 0.059 Uiso 1 1 calc R . . C23 C 0.0378(3) 0.32913(10) 0.76410(15) 0.0288(5) Uani 1 1 d . . . H23 H -0.0223 0.3553 0.7201 0.035 Uiso 1 1 calc R . . C24 C 0.1379(3) 0.28554(12) 0.72740(16) 0.0375(6) Uani 1 1 d . . . H24A H 0.1858 0.2550 0.7664 0.056 Uiso 1 1 calc R . . H24B H 0.2243 0.3075 0.7110 0.056 Uiso 1 1 calc R . . H24C H 0.0677 0.2662 0.6812 0.056 Uiso 1 1 calc R . . C25 C -0.0910(3) 0.29464(12) 0.79517(18) 0.0404(6) Uani 1 1 d . . . H25A H -0.1544 0.2694 0.7529 0.061 Uiso 1 1 calc R . . H25B H -0.1630 0.3232 0.8126 0.061 Uiso 1 1 calc R . . H25C H -0.0375 0.2694 0.8399 0.061 Uiso 1 1 calc R . . Cl1 Cl 0.48415(7) 0.47656(3) 0.88997(3) 0.02886(13) Uani 1 1 d . . . O1 O -0.0563(2) 0.47246(8) 0.65858(13) 0.0434(5) Uani 1 1 d . . . P1 P 0.31212(7) 0.57637(3) 0.75993(4) 0.02394(13) Uani 1 1 d . . . P2 P 0.17172(7) 0.37956(2) 0.83670(3) 0.02056(13) Uani 1 1 d . . . Ru1 Ru 0.25690(2) 0.470252(7) 0.779233(10) 0.01806(7) Uani 1 1 d . . . F1 F 0.9962(13) 0.3039(7) 0.5278(8) 0.073(3) Uani 0.60 1 d P A 1 F3 F 0.7290(7) 0.2869(3) 0.4630(4) 0.0690(16) Uani 0.60 1 d P A 1 F4 F 0.9084(9) 0.2099(4) 0.4979(4) 0.085(2) Uani 0.60 1 d P A 1 F1' F 0.977(2) 0.3169(10) 0.5404(12) 0.096(6) Uani 0.40 1 d P A 2 F3' F 0.7936(12) 0.2715(4) 0.4455(6) 0.080(3) Uani 0.40 1 d P A 2 F4' F 0.9750(15) 0.2152(6) 0.5323(6) 0.088(3) Uani 0.40 1 d P A 2 F2 F 0.8080(2) 0.26067(11) 0.58447(12) 0.0726(6) Uani 1 1 d . A . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 B1 0.062(2) 0.0372(18) 0.043(2) 0.0076(15) 0.0139(17) -0.0038(16) C1 0.0378(14) 0.0181(12) 0.0288(13) 0.0040(9) 0.0101(12) -0.0036(10) C2 0.0257(11) 0.0241(12) 0.0259(12) -0.0001(9) 0.0084(9) -0.0008(9) C3 0.0319(12) 0.0260(12) 0.0243(12) -0.0017(10) 0.0054(10) -0.0007(10) C4 0.0339(13) 0.0448(15) 0.0274(13) -0.0125(11) 0.0121(11) -0.0081(11) C5 0.056(2) 0.103(3) 0.065(2) -0.050(2) 0.0407(18) -0.042(2) C6 0.0602(18) 0.0442(17) 0.0273(14) -0.0077(12) 0.0129(13) -0.0062(14) C7 0.0520(17) 0.0569(19) 0.0368(16) -0.0049(14) 0.0142(13) 0.0233(15) C8 0.0435(14) 0.0227(12) 0.0302(13) 0.0089(10) 0.0058(11) -0.0004(11) C9 0.0656(19) 0.0416(16) 0.0295(14) 0.0080(12) 0.0119(13) 0.0034(14) C10 0.0438(15) 0.0346(15) 0.0405(16) 0.0052(12) -0.0051(12) 0.0089(12) C11 0.0302(13) 0.0305(14) 0.0551(18) 0.0067(12) 0.0058(12) -0.0097(11) C12 0.0310(14) 0.060(2) 0.070(2) 0.0060(17) 0.0217(14) -0.0050(14) C13 0.0495(19) 0.0369(18) 0.120(3) 0.0157(19) 0.016(2) -0.0186(15) C14 0.0422(14) 0.0186(12) 0.0338(14) -0.0023(10) 0.0052(11) 0.0025(10) C15 0.0614(19) 0.0383(16) 0.0485(17) -0.0056(13) 0.0288(15) -0.0023(14) C16 0.067(2) 0.0373(16) 0.0379(16) -0.0122(13) -0.0068(14) 0.0120(14) C17 0.0340(13) 0.0253(12) 0.0349(14) 0.0022(10) 0.0195(11) -0.0001(10) C18 0.0454(15) 0.0398(15) 0.0302(14) -0.0028(11) 0.0181(12) 0.0035(12) C19 0.0304(13) 0.0367(15) 0.0523(17) -0.0016(13) 0.0193(12) 0.0039(11) C20 0.0293(12) 0.0218(12) 0.0273(12) 0.0050(10) 0.0018(10) 0.0035(9) C21 0.0313(13) 0.0286(13) 0.0377(14) 0.0017(11) 0.0032(11) 0.0095(10) C22 0.0471(16) 0.0290(14) 0.0400(15) 0.0131(12) 0.0057(13) 0.0009(12) C23 0.0295(12) 0.0212(12) 0.0318(13) 0.0019(10) 0.0000(10) -0.0029(9) C24 0.0444(15) 0.0316(14) 0.0349(14) -0.0091(11) 0.0067(12) -0.0021(12) C25 0.0381(14) 0.0275(14) 0.0553(18) -0.0035(12) 0.0108(13) -0.0101(11) Cl1 0.0300(3) 0.0273(3) 0.0268(3) 0.0002(2) 0.0018(2) -0.0009(2) O1 0.0278(10) 0.0400(11) 0.0575(13) 0.0099(9) 0.0008(10) -0.0026(8) P1 0.0253(3) 0.0185(3) 0.0269(3) 0.0037(2) 0.0039(2) -0.0024(2) P2 0.0226(3) 0.0167(3) 0.0230(3) 0.0020(2) 0.0065(2) 0.0008(2) Ru1 0.01854(10) 0.01646(10) 0.01928(10) 0.00087(7) 0.00472(7) -0.00011(6) F1 0.050(3) 0.074(7) 0.091(5) 0.028(4) 0.009(3) -0.017(3) F3 0.066(3) 0.055(3) 0.068(4) 0.015(3) -0.019(2) -0.014(2) F4 0.122(6) 0.063(3) 0.092(5) -0.013(4) 0.066(4) 0.018(4) F1' 0.107(12) 0.061(8) 0.082(8) 0.041(7) -0.051(8) -0.050(8) F3' 0.110(8) 0.068(6) 0.048(4) 0.003(4) -0.005(5) -0.044(5) F4' 0.117(9) 0.064(5) 0.093(8) 0.001(6) 0.044(6) 0.021(6) F2 0.0589(12) 0.0974(16) 0.0702(14) -0.0176(12) 0.0328(10) -0.0064(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 B1 F3' 1.317(10) . ? B1 F1 1.326(13) . ? B1 F2 1.361(4) . ? B1 F4 1.381(9) . ? B1 F1' 1.42(2) . ? B1 F4' 1.428(14) . ? B1 F3 1.447(7) . ? C1 O1 1.103(3) . ? C1 Ru1 1.868(3) . ? C2 C3 1.491(3) . ? C2 Ru1 1.848(2) . ? C3 C4 1.551(3) . ? C4 C5 1.520(4) . ? C4 C6 1.528(3) . ? C4 C7 1.532(4) . ? C8 C10 1.528(4) . ? C8 C9 1.541(4) . ? C8 P1 1.849(2) . ? C11 C12 1.518(4) . ? C11 C13 1.539(4) . ? C11 P1 1.858(3) . ? C14 C15 1.529(4) . ? C14 C16 1.532(4) . ? C14 P1 1.864(3) . ? C17 C18 1.531(4) . ? C17 C19 1.536(3) . ? C17 P2 1.852(2) . ? C20 C21 1.532(3) . ? C20 C22 1.533(3) . ? C20 P2 1.848(2) . ? C23 C24 1.528(3) . ? C23 C25 1.537(3) . ? C23 P2 1.863(2) . ? Cl1 Ru1 2.3850(6) . ? P1 Ru1 2.4516(6) . ? P2 Ru1 2.4416(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag F3' B1 F1 104.4(8) . . ? F3' B1 F2 127.8(5) . . ? F1 B1 F2 116.4(7) . . ? F3' B1 F4 83.8(5) . . ? F1 B1 F4 112.1(7) . . ? F2 B1 F4 107.6(4) . . ? F3' B1 F1' 108.6(9) . . ? F1 B1 F1' 17.2(14) . . ? F2 B1 F1' 102.8(9) . . ? F4 B1 F1' 128.5(9) . . ? F3' B1 F4' 111.0(6) . . ? F1 B1 F4' 92.5(8) . . ? F2 B1 F4' 98.8(6) . . ? F4 B1 F4' 30.0(4) . . ? F1' B1 F4' 105.7(10) . . ? F3' B1 F3 31.9(4) . . ? F1 B1 F3 112.9(7) . . ? F2 B1 F3 99.4(4) . . ? F4 B1 F3 107.5(4) . . ? F1' B1 F3 107.2(8) . . ? F4' B1 F3 137.5(5) . . ? O1 C1 Ru1 179.1(2) . . ? C3 C2 Ru1 134.80(18) . . ? C2 C3 C4 117.1(2) . . ? C5 C4 C6 109.4(2) . . ? C5 C4 C7 110.0(3) . . ? C6 C4 C7 108.7(2) . . ? C5 C4 C3 111.4(2) . . ? C6 C4 C3 107.1(2) . . ? C7 C4 C3 110.2(2) . . ? C10 C8 C9 109.6(2) . . ? C10 C8 P1 114.58(18) . . ? C9 C8 P1 112.36(18) . . ? C12 C11 C13 110.5(3) . . ? C12 C11 P1 115.0(2) . . ? C13 C11 P1 112.4(2) . . ? C15 C14 C16 109.1(2) . . ? C15 C14 P1 110.39(17) . . ? C16 C14 P1 115.35(19) . . ? C18 C17 C19 111.7(2) . . ? C18 C17 P2 113.22(17) . . ? C19 C17 P2 110.83(17) . . ? C21 C20 C22 111.0(2) . . ? C21 C20 P2 115.80(17) . . ? C22 C20 P2 113.77(17) . . ? C24 C23 C25 110.0(2) . . ? C24 C23 P2 110.92(17) . . ? C25 C23 P2 115.73(18) . . ? C8 P1 C11 105.89(13) . . ? C8 P1 C14 103.41(11) . . ? C11 P1 C14 103.99(12) . . ? C8 P1 Ru1 118.69(8) . . ? C11 P1 Ru1 114.35(9) . . ? C14 P1 Ru1 109.02(8) . . ? C20 P2 C17 103.98(11) . . ? C20 P2 C23 111.00(11) . . ? C17 P2 C23 104.66(11) . . ? C20 P2 Ru1 113.40(8) . . ? C17 P2 Ru1 108.29(8) . . ? C23 P2 Ru1 114.52(8) . . ? C2 Ru1 C1 90.81(10) . . ? C2 Ru1 Cl1 98.56(7) . . ? C1 Ru1 Cl1 170.63(8) . . ? C2 Ru1 P2 96.80(7) . . ? C1 Ru1 P2 90.31(7) . . ? Cl1 Ru1 P2 88.84(2) . . ? C2 Ru1 P1 102.63(7) . . ? C1 Ru1 P1 92.94(7) . . ? Cl1 Ru1 P1 84.80(2) . . ? P2 Ru1 P1 160.24(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 Ru1 C2 C3 C4 -179.64(19) . . . . ? C2 C3 C4 C5 -53.9(3) . . . . ? C2 C3 C4 C6 -173.4(2) . . . . ? C2 C3 C4 C7 68.5(3) . . . . ? C10 C8 P1 C11 -156.14(19) . . . . ? C9 C8 P1 C11 77.8(2) . . . . ? C10 C8 P1 C14 -47.1(2) . . . . ? C9 C8 P1 C14 -173.10(19) . . . . ? C10 C8 P1 Ru1 73.7(2) . . . . ? C9 C8 P1 Ru1 -52.3(2) . . . . ? C12 C11 P1 C8 -82.7(2) . . . . ? C13 C11 P1 C8 44.9(3) . . . . ? C12 C11 P1 C14 168.7(2) . . . . ? C13 C11 P1 C14 -63.8(3) . . . . ? C12 C11 P1 Ru1 49.9(2) . . . . ? C13 C11 P1 Ru1 177.5(2) . . . . ? C15 C14 P1 C8 91.7(2) . . . . ? C16 C14 P1 C8 -144.0(2) . . . . ? C15 C14 P1 C11 -157.79(19) . . . . ? C16 C14 P1 C11 -33.5(2) . . . . ? C15 C14 P1 Ru1 -35.4(2) . . . . ? C16 C14 P1 Ru1 88.8(2) . . . . ? C21 C20 P2 C17 -171.05(18) . . . . ? C22 C20 P2 C17 58.6(2) . . . . ? C21 C20 P2 C23 76.9(2) . . . . ? C22 C20 P2 C23 -53.4(2) . . . . ? C21 C20 P2 Ru1 -53.7(2) . . . . ? C22 C20 P2 Ru1 175.99(16) . . . . ? C18 C17 P2 C20 51.2(2) . . . . ? C19 C17 P2 C20 177.55(18) . . . . ? C18 C17 P2 C23 167.69(18) . . . . ? C19 C17 P2 C23 -65.91(19) . . . . ? C18 C17 P2 Ru1 -69.74(18) . . . . ? C19 C17 P2 Ru1 56.66(18) . . . . ? C24 C23 P2 C20 -42.8(2) . . . . ? C25 C23 P2 C20 83.5(2) . . . . ? C24 C23 P2 C17 -154.36(18) . . . . ? C25 C23 P2 C17 -28.1(2) . . . . ? C24 C23 P2 Ru1 87.22(17) . . . . ? C25 C23 P2 Ru1 -146.55(16) . . . . ? C3 C2 Ru1 C1 3.8(2) . . . . ? C3 C2 Ru1 Cl1 -175.9(2) . . . . ? C3 C2 Ru1 P2 94.3(2) . . . . ? C3 C2 Ru1 P1 -89.4(2) . . . . ? O1 C1 Ru1 C2 120(18) . . . . ? O1 C1 Ru1 Cl1 -62(18) . . . . ? O1 C1 Ru1 P2 23(18) . . . . ? O1 C1 Ru1 P1 -137(18) . . . . ? C20 P2 Ru1 C2 70.16(11) . . . . ? C17 P2 Ru1 C2 -174.98(11) . . . . ? C23 P2 Ru1 C2 -58.63(11) . . . . ? C20 P2 Ru1 C1 161.02(11) . . . . ? C17 P2 Ru1 C1 -84.13(11) . . . . ? C23 P2 Ru1 C1 32.22(11) . . . . ? C20 P2 Ru1 Cl1 -28.31(9) . . . . ? C17 P2 Ru1 Cl1 86.54(9) . . . . ? C23 P2 Ru1 Cl1 -157.11(9) . . . . ? C20 P2 Ru1 P1 -99.36(10) . . . . ? C17 P2 Ru1 P1 15.50(11) . . . . ? C23 P2 Ru1 P1 131.85(10) . . . . ? C8 P1 Ru1 C2 72.35(12) . . . . ? C11 P1 Ru1 C2 -53.83(13) . . . . ? C14 P1 Ru1 C2 -169.73(11) . . . . ? C8 P1 Ru1 C1 -19.14(12) . . . . ? C11 P1 Ru1 C1 -145.32(13) . . . . ? C14 P1 Ru1 C1 98.78(11) . . . . ? C8 P1 Ru1 Cl1 169.97(10) . . . . ? C11 P1 Ru1 Cl1 43.79(11) . . . . ? C14 P1 Ru1 Cl1 -72.10(9) . . . . ? C8 P1 Ru1 P2 -118.31(11) . . . . ? C11 P1 Ru1 P2 115.51(12) . . . . ? C14 P1 Ru1 P2 -0.39(11) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.446 _refine_diff_density_min -0.305 _refine_diff_density_rms 0.058