# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Jason Lynam' _publ_contact_author_email JML12@YORK.AC.UK _publ_section_title ; Ruthenium Carbene, Alkenyl and Alkynyl Complexes Containing Pendant Uracil Groups: an Investigation into the Formation of Alkenyl-phosphonio Complexes. ; loop_ _publ_author_name 'Jason Lynam' 'Micheal J. Cowley' 'Robert S. Monneypenny' 'Adrian C. Whitwood' 'Alastair J. Wilson' # Attachment 'combinedcif.cif' data_CCDC737832_compound3c[OTf] _database_code_depnum_ccdc_archive 'CCDC 737832' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C50 H43 O P2 Ru, 0.75(C H2 Cl2), 0.25(C4 H10 O), C F3 O3 S' _chemical_formula_sum 'C52.75 H47 Cl1.50 F3 O4.25 P2 Ru S' _chemical_formula_weight 1054.15 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' S S 0.1246 0.1234 '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' Cl Cl 0.1484 0.1585 '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)/n _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.3192(10) _cell_length_b 12.4402(10) _cell_length_c 31.194(3) _cell_angle_alpha 90.00 _cell_angle_beta 94.150(2) _cell_angle_gamma 90.00 _cell_volume 4768.1(7) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 5995 _cell_measurement_theta_min 2.39 _cell_measurement_theta_max 28.14 _exptl_crystal_description Block _exptl_crystal_colour Red _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.468 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2160 _exptl_absorpt_coefficient_mu 0.582 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.843 _exptl_absorpt_correction_T_max 0.950 _exptl_absorpt_process_details 'SADABS v2.03; (Sheldrick)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 48327 _diffrn_reflns_av_R_equivalents 0.0386 _diffrn_reflns_av_sigmaI/netI 0.0358 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -41 _diffrn_reflns_limit_l_max 41 _diffrn_reflns_theta_min 1.31 _diffrn_reflns_theta_max 28.32 _reflns_number_total 11871 _reflns_number_gt 9876 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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. The disordered solvent was modelled as mixture of 75% CH2Cl2 : 25% Et2O. ; _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^)+(0.0353P)^2^+2.6072P] 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 11870 _refine_ls_number_parameters 639 _refine_ls_number_restraints 10 _refine_ls_R_factor_all 0.0447 _refine_ls_R_factor_gt 0.0334 _refine_ls_wR_factor_ref 0.0787 _refine_ls_wR_factor_gt 0.0745 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.038 _refine_ls_shift/su_max 0.004 _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 C1 C 0.62320(16) -0.05275(15) 0.77387(6) 0.0195(4) Uani 1 1 d . . . H1 H 0.6781 -0.0012 0.7656 0.023 Uiso 1 1 calc R . . C2 C 0.51608(16) -0.06210(16) 0.75534(6) 0.0205(4) Uani 1 1 d . . . H2 H 0.4829 -0.0162 0.7325 0.025 Uiso 1 1 calc R . . C3 C 0.46464(16) -0.15126(16) 0.77437(6) 0.0216(4) Uani 1 1 d . . . H3 H 0.3914 -0.1786 0.7662 0.026 Uiso 1 1 calc R . . C4 C 0.54256(16) -0.19932(15) 0.80436(6) 0.0201(4) Uani 1 1 d . . . H4 H 0.5328 -0.2662 0.8202 0.024 Uiso 1 1 calc R . . C5 C 0.63964(16) -0.13790(16) 0.80481(6) 0.0199(4) Uani 1 1 d . . . H5 H 0.7087 -0.1557 0.8208 0.024 Uiso 1 1 calc R . . C6 C 0.43741(15) -0.07989(15) 0.87397(6) 0.0174(4) Uani 1 1 d . . . C7 C 0.39925(16) -0.12586(16) 0.90803(7) 0.0206(4) Uani 1 1 d . . . H7 H 0.447(2) -0.1400(19) 0.9290(8) 0.028(6) Uiso 1 1 d . . . C8 C 0.28717(15) -0.15621(15) 0.91556(6) 0.0176(4) Uani 1 1 d . . . C9 C 0.26356(16) -0.18870(17) 0.95646(6) 0.0223(4) Uani 1 1 d . . . H9 H 0.3184 -0.1901 0.9786 0.027 Uiso 1 1 calc R . . C10 C 0.15844(17) -0.21904(19) 0.96457(7) 0.0268(5) Uani 1 1 d . . . C11 C 0.07554(17) -0.21746(19) 0.93207(7) 0.0292(5) Uani 1 1 d . . . H11 H 0.0050 -0.2369 0.9376 0.035 Uiso 1 1 calc R . . C12 C 0.09955(17) -0.18644(17) 0.89118(7) 0.0260(4) Uani 1 1 d . . . H12 H 0.0447 -0.1865 0.8691 0.031 Uiso 1 1 calc R . . C13 C 0.20362(16) -0.15535(16) 0.88270(6) 0.0209(4) Uani 1 1 d . . . H13 H 0.2181 -0.1339 0.8551 0.025 Uiso 1 1 calc R . . C14 C 0.0455(2) -0.2970(4) 1.01529(11) 0.0950(17) Uani 1 1 d . . . H14A H -0.0107 -0.2434 1.0134 0.142 Uiso 1 1 calc R . . H14B H 0.0518 -0.3269 1.0437 0.142 Uiso 1 1 calc R . . H14C H 0.0276 -0.3529 0.9948 0.142 Uiso 1 1 calc R . . C15 C 0.31264(14) 0.10034(14) 0.76468(6) 0.0145(3) Uani 1 1 d . . . C16 C 0.30363(16) 0.16362(16) 0.72782(6) 0.0207(4) Uani 1 1 d . . . H16 H 0.3518 0.2202 0.7248 0.025 Uiso 1 1 calc R . . C17 C 0.22262(18) 0.14235(17) 0.69553(7) 0.0263(5) Uani 1 1 d . . . H17 H 0.2184 0.1835 0.6706 0.032 Uiso 1 1 calc R . . C18 C 0.14844(17) 0.06075(16) 0.70012(6) 0.0227(4) Uani 1 1 d . . . H18 H 0.0939 0.0477 0.6785 0.027 Uiso 1 1 calc R . . C19 C 0.15549(16) -0.00166(16) 0.73696(6) 0.0194(4) Uani 1 1 d . . . H19 H 0.1051 -0.0560 0.7404 0.023 Uiso 1 1 calc R . . C20 C 0.23766(15) 0.01704(15) 0.76864(6) 0.0170(4) Uani 1 1 d . . . H20 H 0.2432 -0.0264 0.7930 0.020 Uiso 1 1 calc R . . C21 C 0.30372(14) 0.18143(15) 0.84497(6) 0.0156(4) Uani 1 1 d . . . C22 C 0.25803(15) 0.12373(16) 0.87716(6) 0.0193(4) Uani 1 1 d . . . H22 H 0.2887 0.0587 0.8864 0.023 Uiso 1 1 calc R . . C23 C 0.16649(17) 0.16286(19) 0.89560(7) 0.0261(4) Uani 1 1 d . . . H23 H 0.1358 0.1234 0.9170 0.031 Uiso 1 1 calc R . . C24 C 0.12071(17) 0.25983(19) 0.88249(7) 0.0286(5) Uani 1 1 d . . . H24 H 0.0596 0.2856 0.8950 0.034 Uiso 1 1 calc R . . C25 C 0.16622(17) 0.31855(17) 0.85063(7) 0.0251(4) Uani 1 1 d . . . H25 H 0.1362 0.3843 0.8419 0.030 Uiso 1 1 calc R . . C26 C 0.25652(15) 0.27924(16) 0.83171(6) 0.0197(4) Uani 1 1 d . . . H26 H 0.2860 0.3183 0.8100 0.024 Uiso 1 1 calc R . . C27 C 0.48949(14) 0.23934(15) 0.79913(6) 0.0159(4) Uani 1 1 d . . . C28 C 0.50946(15) 0.32150(15) 0.82902(6) 0.0178(4) Uani 1 1 d . . . H28 H 0.4759 0.3203 0.8548 0.021 Uiso 1 1 calc R . . C29 C 0.57936(15) 0.40528(16) 0.82050(7) 0.0217(4) Uani 1 1 d . . . H29 H 0.5946 0.4584 0.8410 0.026 Uiso 1 1 calc R . . C30 C 0.62630(16) 0.40978(17) 0.78155(7) 0.0248(4) Uani 1 1 d . . . H30 H 0.6708 0.4674 0.7755 0.030 Uiso 1 1 calc R . . C31 C 0.60701(16) 0.32841(17) 0.75157(7) 0.0231(4) Uani 1 1 d . . . H31 H 0.6381 0.3318 0.7253 0.028 Uiso 1 1 calc R . . C32 C 0.54124(15) 0.24178(16) 0.76073(6) 0.0192(4) Uani 1 1 d . . . H32 H 0.5317 0.1854 0.7413 0.023 Uiso 1 1 calc R . . C33 C 0.76542(15) 0.07893(15) 0.85059(6) 0.0169(4) Uani 1 1 d . . . C34 C 0.76668(15) 0.16851(17) 0.82363(7) 0.0221(4) Uani 1 1 d . . . H34 H 0.7061 0.2132 0.8206 0.027 Uiso 1 1 calc R . . C35 C 0.85705(17) 0.19153(17) 0.80130(7) 0.0249(4) Uani 1 1 d . . . H35 H 0.8571 0.2517 0.7836 0.030 Uiso 1 1 calc R . . C36 C 0.94722(17) 0.12500(17) 0.80527(7) 0.0257(4) Uani 1 1 d . . . H36 H 1.0077 0.1400 0.7901 0.031 Uiso 1 1 calc R . . C37 C 0.94697(17) 0.03659(17) 0.83176(7) 0.0270(5) Uani 1 1 d . . . H37 H 1.0078 -0.0078 0.8345 0.032 Uiso 1 1 calc R . . C38 C 0.85690(16) 0.01256(16) 0.85457(7) 0.0211(4) Uani 1 1 d . . . H38 H 0.8578 -0.0474 0.8724 0.025 Uiso 1 1 calc R . . C39 C 0.69011(15) -0.04561(16) 0.91975(6) 0.0193(4) Uani 1 1 d . . . C40 C 0.74578(19) -0.00175(19) 0.95629(7) 0.0302(5) Uani 1 1 d . . . H40 H 0.7571 0.0721 0.9582 0.036 Uiso 1 1 calc R . . C41 C 0.7841(2) -0.0680(2) 0.98961(8) 0.0381(6) Uani 1 1 d . . . H41 H 0.8209 -0.0384 1.0139 0.046 Uiso 1 1 calc R . . C42 C 0.76823(19) -0.1781(2) 0.98714(7) 0.0318(5) Uani 1 1 d . . . H42 H 0.7927 -0.2221 1.0099 0.038 Uiso 1 1 calc R . . C43 C 0.71603(18) -0.22211(18) 0.95074(7) 0.0280(5) Uani 1 1 d . . . H43 H 0.7075 -0.2962 0.9485 0.034 Uiso 1 1 calc R . . C44 C 0.67615(17) -0.15620(17) 0.91735(6) 0.0229(4) Uani 1 1 d . . . H44 H 0.6397 -0.1864 0.8931 0.028 Uiso 1 1 calc R . . C45 C 0.60678(15) 0.16389(16) 0.90657(6) 0.0185(4) Uani 1 1 d . . . C46 C 0.67335(17) 0.25436(17) 0.91137(7) 0.0234(4) Uani 1 1 d . . . H46 H 0.7382 0.2572 0.8979 0.028 Uiso 1 1 calc R . . C47 C 0.64292(19) 0.34030(18) 0.93628(7) 0.0296(5) Uani 1 1 d . . . H47 H 0.6872 0.4008 0.9391 0.036 Uiso 1 1 calc R . . C48 C 0.54757(19) 0.33661(19) 0.95679(7) 0.0312(5) Uani 1 1 d . . . H48 H 0.5277 0.3945 0.9734 0.037 Uiso 1 1 calc R . . C49 C 0.48146(18) 0.24687(19) 0.95273(7) 0.0295(5) Uani 1 1 d . . . H49 H 0.4173 0.2442 0.9667 0.035 Uiso 1 1 calc R . . C50 C 0.51097(16) 0.16083(17) 0.92781(6) 0.0230(4) Uani 1 1 d . . . H50 H 0.4664 0.1005 0.9252 0.028 Uiso 1 1 calc R . . O1 O 0.14598(14) -0.24916(17) 1.00626(5) 0.0435(5) Uani 1 1 d . . . P1 P 0.40750(4) 0.12391(4) 0.812193(15) 0.01335(9) Uani 1 1 d . . . P2 P 0.64136(4) 0.04523(4) 0.876261(15) 0.01509(10) Uani 1 1 d . . . Ru1 Ru 0.509899(11) -0.032252(11) 0.828034(5) 0.01325(4) Uani 1 1 d . . . C51 C 0.8961(2) 0.5392(2) 0.88057(10) 0.0417(6) Uani 1 1 d . . . F1 F 1.00038(14) 0.54331(14) 0.87185(8) 0.0722(6) Uani 1 1 d . . . F2 F 0.86316(15) 0.43753(12) 0.87499(6) 0.0622(5) Uani 1 1 d . . . F3 F 0.89163(17) 0.56272(15) 0.92213(6) 0.0669(5) Uani 1 1 d . . . O2 O 0.70625(12) 0.61645(13) 0.86068(6) 0.0341(4) Uani 1 1 d . . . O3 O 0.86145(12) 0.73435(11) 0.85582(5) 0.0276(3) Uani 1 1 d . . . O4 O 0.82852(16) 0.59046(15) 0.80409(5) 0.0447(5) Uani 1 1 d . . . S1 S 0.81321(4) 0.63073(4) 0.846265(16) 0.02157(10) Uani 1 1 d . . . C52 C 0.2157(5) 0.0416(4) 0.58250(13) 0.0629(13) Uani 0.75 1 d P A 1 H52A H 0.2322 -0.0080 0.6060 0.076 Uiso 0.75 1 calc PR A 1 H52B H 0.2624 0.1040 0.5871 0.076 Uiso 0.75 1 calc PR A 1 Cl1 Cl 0.24315(14) -0.02100(10) 0.53349(4) 0.0713(4) Uani 0.75 1 d P A 1 Cl2 Cl 0.07997(11) 0.08158(15) 0.58245(3) 0.0546(4) Uani 0.75 1 d P A 1 C53 C 0.3135(7) -0.0138(7) 0.5218(3) 0.031(2) Uani 0.25 1 d PD B 2 H53A H 0.2741 -0.0665 0.5044 0.047 Uiso 0.25 1 calc PR B 2 H53B H 0.3854 -0.0401 0.5298 0.047 Uiso 0.25 1 calc PR B 2 H53C H 0.3184 0.0516 0.5058 0.047 Uiso 0.25 1 calc PR B 2 C54 C 0.2547(6) 0.0076(12) 0.5617(3) 0.053(3) Uani 0.25 1 d PD B 2 H54A H 0.2511 -0.0569 0.5790 0.063 Uiso 0.25 1 calc PR B 2 H54B H 0.2908 0.0637 0.5790 0.063 Uiso 0.25 1 calc PR B 2 C55 C 0.0875(14) 0.055(2) 0.5824(4) 0.108(14) Uani 0.25 1 d PDU B 2 H55A H 0.1276 0.0995 0.6037 0.130 Uiso 0.25 1 calc PR B 2 H55B H 0.0727 -0.0137 0.5953 0.130 Uiso 0.25 1 calc PR B 2 C56 C -0.0179(9) 0.1100(8) 0.5667(3) 0.040(2) Uani 0.25 1 d PD B 2 H56A H -0.0021 0.1784 0.5544 0.060 Uiso 0.25 1 calc PR B 2 H56B H -0.0622 0.1204 0.5905 0.060 Uiso 0.25 1 calc PR B 2 H56C H -0.0563 0.0658 0.5455 0.060 Uiso 0.25 1 calc PR B 2 O5 O 0.1487(5) 0.0409(5) 0.5458(2) 0.0294(13) Uani 0.25 1 d PD B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0206(9) 0.0185(10) 0.0201(9) -0.0031(7) 0.0076(7) 0.0019(7) C2 0.0256(10) 0.0202(10) 0.0157(9) -0.0039(7) 0.0017(8) 0.0059(8) C3 0.0201(9) 0.0207(10) 0.0239(10) -0.0064(8) 0.0012(8) -0.0007(8) C4 0.0240(10) 0.0138(9) 0.0228(10) -0.0032(7) 0.0028(8) 0.0032(7) C5 0.0174(9) 0.0191(9) 0.0234(10) -0.0039(8) 0.0028(7) 0.0067(7) C6 0.0131(8) 0.0149(9) 0.0239(10) -0.0011(7) -0.0004(7) 0.0013(7) C7 0.0169(9) 0.0219(10) 0.0228(10) 0.0045(8) -0.0003(8) 0.0008(8) C8 0.0171(9) 0.0139(9) 0.0223(9) 0.0001(7) 0.0037(7) 0.0008(7) C9 0.0204(9) 0.0269(11) 0.0197(10) 0.0009(8) 0.0015(8) 0.0007(8) C10 0.0242(10) 0.0334(12) 0.0238(10) 0.0043(9) 0.0075(8) 0.0020(9) C11 0.0165(10) 0.0349(12) 0.0364(12) 0.0070(10) 0.0035(9) -0.0016(9) C12 0.0204(10) 0.0258(11) 0.0308(11) 0.0066(9) -0.0046(8) -0.0037(8) C13 0.0239(10) 0.0181(9) 0.0206(10) 0.0028(8) 0.0003(8) -0.0027(8) C14 0.0331(16) 0.200(5) 0.054(2) 0.058(3) 0.0149(15) -0.017(2) C15 0.0140(8) 0.0139(8) 0.0156(8) -0.0015(7) 0.0003(7) 0.0017(7) C16 0.0221(10) 0.0168(9) 0.0229(10) 0.0023(8) -0.0014(8) -0.0052(7) C17 0.0352(12) 0.0232(10) 0.0190(10) 0.0056(8) -0.0073(9) -0.0029(9) C18 0.0239(10) 0.0222(10) 0.0206(10) -0.0024(8) -0.0073(8) -0.0013(8) C19 0.0180(9) 0.0177(9) 0.0222(10) -0.0018(7) 0.0009(7) -0.0016(7) C20 0.0167(9) 0.0165(9) 0.0178(9) 0.0028(7) 0.0013(7) 0.0002(7) C21 0.0132(8) 0.0173(9) 0.0161(9) -0.0031(7) -0.0009(7) 0.0006(7) C22 0.0182(9) 0.0210(10) 0.0183(9) 0.0009(7) -0.0005(7) 0.0006(7) C23 0.0239(10) 0.0374(12) 0.0176(10) 0.0026(9) 0.0056(8) 0.0022(9) C24 0.0217(10) 0.0408(13) 0.0237(10) -0.0043(9) 0.0053(8) 0.0100(9) C25 0.0221(10) 0.0240(11) 0.0289(11) -0.0038(9) -0.0013(8) 0.0086(8) C26 0.0187(9) 0.0185(9) 0.0220(10) -0.0005(8) 0.0024(7) 0.0000(7) C27 0.0120(8) 0.0140(9) 0.0214(9) 0.0026(7) 0.0004(7) 0.0003(7) C28 0.0141(8) 0.0165(9) 0.0223(9) 0.0012(8) -0.0008(7) 0.0015(7) C29 0.0152(9) 0.0159(9) 0.0330(11) 0.0010(8) -0.0048(8) 0.0004(7) C30 0.0139(9) 0.0192(10) 0.0410(12) 0.0090(9) 0.0003(8) -0.0029(7) C31 0.0162(9) 0.0251(11) 0.0286(11) 0.0064(8) 0.0059(8) 0.0014(8) C32 0.0159(9) 0.0171(9) 0.0245(10) 0.0013(8) 0.0025(7) 0.0018(7) C33 0.0137(8) 0.0182(9) 0.0185(9) -0.0029(7) 0.0005(7) -0.0014(7) C34 0.0141(9) 0.0256(11) 0.0266(10) 0.0048(8) 0.0009(8) 0.0025(8) C35 0.0224(10) 0.0234(10) 0.0292(11) 0.0074(9) 0.0035(8) -0.0019(8) C36 0.0176(9) 0.0287(11) 0.0315(11) 0.0002(9) 0.0070(8) -0.0024(8) C37 0.0180(9) 0.0235(10) 0.0401(12) 0.0025(9) 0.0061(9) 0.0043(8) C38 0.0185(9) 0.0175(10) 0.0270(10) 0.0018(8) 0.0008(8) 0.0007(7) C39 0.0179(9) 0.0236(10) 0.0165(9) 0.0039(8) 0.0026(7) 0.0053(8) C40 0.0365(12) 0.0274(11) 0.0256(11) 0.0022(9) -0.0064(9) -0.0012(9) C41 0.0498(15) 0.0395(14) 0.0228(11) 0.0034(10) -0.0126(10) 0.0029(12) C42 0.0355(12) 0.0372(13) 0.0223(11) 0.0101(9) -0.0002(9) 0.0123(10) C43 0.0313(11) 0.0252(11) 0.0281(11) 0.0058(9) 0.0054(9) 0.0097(9) C44 0.0261(10) 0.0239(10) 0.0190(10) 0.0008(8) 0.0028(8) 0.0062(8) C45 0.0197(9) 0.0196(9) 0.0155(9) -0.0011(7) -0.0028(7) 0.0038(7) C46 0.0198(10) 0.0240(10) 0.0260(10) -0.0015(8) -0.0004(8) 0.0011(8) C47 0.0320(12) 0.0227(11) 0.0332(12) -0.0070(9) -0.0051(9) 0.0010(9) C48 0.0377(13) 0.0286(12) 0.0266(11) -0.0087(9) -0.0017(9) 0.0101(10) C49 0.0267(11) 0.0366(13) 0.0257(11) -0.0061(9) 0.0055(9) 0.0087(9) C50 0.0210(10) 0.0265(11) 0.0214(10) -0.0023(8) 0.0004(8) 0.0022(8) O1 0.0302(9) 0.0754(14) 0.0263(9) 0.0130(9) 0.0112(7) -0.0050(9) P1 0.0119(2) 0.0125(2) 0.0156(2) 0.00018(17) 0.00094(17) 0.00000(17) P2 0.0133(2) 0.0157(2) 0.0162(2) 0.00056(18) 0.00068(17) 0.00171(17) Ru1 0.01209(7) 0.01231(7) 0.01540(7) 0.00043(6) 0.00135(5) 0.00092(5) C51 0.0396(14) 0.0235(12) 0.0611(18) 0.0046(12) -0.0022(12) 0.0051(10) F1 0.0329(9) 0.0447(10) 0.1370(19) -0.0048(11) -0.0080(10) 0.0170(7) F2 0.0716(12) 0.0197(7) 0.0934(14) 0.0105(8) -0.0066(10) 0.0028(7) F3 0.0941(15) 0.0604(11) 0.0420(10) 0.0162(8) -0.0240(9) 0.0000(10) O2 0.0228(8) 0.0284(9) 0.0514(10) -0.0107(7) 0.0055(7) -0.0063(6) O3 0.0247(8) 0.0171(7) 0.0402(9) -0.0025(6) -0.0041(6) -0.0033(6) O4 0.0672(13) 0.0390(10) 0.0291(9) -0.0075(8) 0.0123(8) -0.0204(9) S1 0.0231(2) 0.0166(2) 0.0247(2) -0.00162(19) -0.00018(19) -0.00235(19) C52 0.111(4) 0.044(2) 0.031(2) 0.0034(18) -0.013(2) 0.004(2) Cl1 0.1118(12) 0.0500(7) 0.0519(7) 0.0012(5) 0.0040(7) -0.0010(7) Cl2 0.0794(9) 0.0456(7) 0.0368(6) 0.0041(4) -0.0103(5) -0.0237(5) C53 0.013(4) 0.019(4) 0.061(7) -0.005(4) -0.002(4) 0.007(3) C54 0.055(8) 0.071(9) 0.029(7) 0.008(6) -0.016(6) 0.002(7) C55 0.111(14) 0.108(15) 0.105(14) -0.004(5) 0.001(5) -0.010(5) C56 0.053(7) 0.035(5) 0.032(5) -0.011(4) 0.011(5) -0.011(5) O5 0.030(3) 0.028(3) 0.030(3) -0.003(3) -0.001(3) 0.004(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 C1 C2 1.407(3) . ? C1 C5 1.438(3) . ? C1 Ru1 2.2824(19) . ? C1 H1 0.9800 . ? C2 C3 1.428(3) . ? C2 Ru1 2.3045(19) . ? C2 H2 0.9800 . ? C3 C4 1.423(3) . ? C3 Ru1 2.2738(19) . ? C3 H3 0.9800 . ? C4 C5 1.418(3) . ? C4 Ru1 2.2516(19) . ? C4 H4 0.9800 . ? C5 Ru1 2.2303(18) . ? C5 H5 0.9800 . ? C6 C7 1.322(3) . ? C6 Ru1 1.8405(19) . ? C7 C8 1.467(3) . ? C7 H7 0.87(2) . ? C8 C9 1.389(3) . ? C8 C13 1.399(3) . ? C9 C10 1.390(3) . ? C9 H9 0.9300 . ? C10 O1 1.373(3) . ? C10 C11 1.386(3) . ? C11 C12 1.385(3) . ? C11 H11 0.9300 . ? C12 C13 1.383(3) . ? C12 H12 0.9300 . ? C13 H13 0.9300 . ? C14 O1 1.419(3) . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 C16 1.391(3) . ? C15 C20 1.400(3) . ? C15 P1 1.8432(18) . ? C16 C17 1.391(3) . ? C16 H16 0.9300 . ? C17 C18 1.380(3) . ? C17 H17 0.9300 . ? C18 C19 1.384(3) . ? C18 H18 0.9300 . ? C19 C20 1.382(3) . ? C19 H19 0.9300 . ? C20 H20 0.9300 . ? C21 C22 1.387(3) . ? C21 C26 1.398(3) . ? C21 P1 1.8387(19) . ? C22 C23 1.390(3) . ? C22 H22 0.9300 . ? C23 C24 1.381(3) . ? C23 H23 0.9300 . ? C24 C25 1.384(3) . ? C24 H24 0.9300 . ? C25 C26 1.386(3) . ? C25 H25 0.9300 . ? C26 H26 0.9300 . ? C27 C28 1.393(3) . ? C27 C32 1.397(3) . ? C27 P1 1.8189(19) . ? C28 C29 1.390(3) . ? C28 H28 0.9300 . ? C29 C30 1.384(3) . ? C29 H29 0.9300 . ? C30 C31 1.387(3) . ? C30 H30 0.9300 . ? C31 C32 1.390(3) . ? C31 H31 0.9300 . ? C32 H32 0.9300 . ? C33 C38 1.395(3) . ? C33 C34 1.397(3) . ? C33 P2 1.8248(19) . ? C34 C35 1.385(3) . ? C34 H34 0.9300 . ? C35 C36 1.384(3) . ? C35 H35 0.9300 . ? C36 C37 1.376(3) . ? C36 H36 0.9300 . ? C37 C38 1.393(3) . ? C37 H37 0.9300 . ? C38 H38 0.9300 . ? C39 C44 1.388(3) . ? C39 C40 1.398(3) . ? C39 P2 1.8332(19) . ? C40 C41 1.383(3) . ? C40 H40 0.9300 . ? C41 C42 1.384(4) . ? C41 H41 0.9300 . ? C42 C43 1.377(3) . ? C42 H42 0.9300 . ? C43 C44 1.387(3) . ? C43 H43 0.9300 . ? C44 H44 0.9300 . ? C45 C46 1.394(3) . ? C45 C50 1.395(3) . ? C45 P2 1.820(2) . ? C46 C47 1.389(3) . ? C46 H46 0.9300 . ? C47 C48 1.378(3) . ? C47 H47 0.9300 . ? C48 C49 1.382(3) . ? C48 H48 0.9300 . ? C49 C50 1.387(3) . ? C49 H49 0.9300 . ? C50 H50 0.9300 . ? P1 Ru1 2.3493(5) . ? P2 Ru1 2.3372(5) . ? C51 F1 1.333(3) . ? C51 F3 1.334(3) . ? C51 F2 1.336(3) . ? C51 S1 1.824(3) . ? O2 S1 1.4337(16) . ? O3 S1 1.4416(15) . ? O4 S1 1.4329(17) . ? C52 Cl2 1.744(6) . ? C52 Cl1 1.770(5) . ? C52 H52A 0.9700 . ? C52 H52B 0.9700 . ? C53 C54 1.509(5) . ? C53 H53A 0.9600 . ? C53 H53B 0.9600 . ? C53 H53C 0.9600 . ? C54 O5 1.425(5) . ? C54 H54A 0.9700 . ? C54 H54B 0.9700 . ? C55 O5 1.424(5) . ? C55 C56 1.516(5) . ? C55 H55A 0.9700 . ? C55 H55B 0.9700 . ? C56 H56A 0.9600 . ? C56 H56B 0.9600 . ? C56 H56C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 C5 107.30(17) . . ? C2 C1 Ru1 73.00(11) . . ? C5 C1 Ru1 69.47(10) . . ? C2 C1 H1 126.3 . . ? C5 C1 H1 126.3 . . ? Ru1 C1 H1 126.3 . . ? C1 C2 C3 108.96(17) . . ? C1 C2 Ru1 71.29(11) . . ? C3 C2 Ru1 70.66(11) . . ? C1 C2 H2 125.5 . . ? C3 C2 H2 125.5 . . ? Ru1 C2 H2 125.5 . . ? C4 C3 C2 107.53(18) . . ? C4 C3 Ru1 70.83(11) . . ? C2 C3 Ru1 73.01(11) . . ? C4 C3 H3 126.1 . . ? C2 C3 H3 126.1 . . ? Ru1 C3 H3 126.1 . . ? C5 C4 C3 107.97(18) . . ? C5 C4 Ru1 70.74(11) . . ? C3 C4 Ru1 72.52(11) . . ? C5 C4 H4 125.9 . . ? C3 C4 H4 125.9 . . ? Ru1 C4 H4 125.9 . . ? C4 C5 C1 108.21(17) . . ? C4 C5 Ru1 72.37(11) . . ? C1 C5 Ru1 73.40(10) . . ? C4 C5 H5 125.7 . . ? C1 C5 H5 125.7 . . ? Ru1 C5 H5 125.7 . . ? C7 C6 Ru1 170.20(16) . . ? C6 C7 C8 129.31(19) . . ? C6 C7 H7 115.5(16) . . ? C8 C7 H7 115.2(16) . . ? C9 C8 C13 118.90(18) . . ? C9 C8 C7 118.96(18) . . ? C13 C8 C7 122.13(18) . . ? C8 C9 C10 120.41(19) . . ? C8 C9 H9 119.8 . . ? C10 C9 H9 119.8 . . ? O1 C10 C11 124.7(2) . . ? O1 C10 C9 114.60(19) . . ? C11 C10 C9 120.7(2) . . ? C12 C11 C10 118.8(2) . . ? C12 C11 H11 120.6 . . ? C10 C11 H11 120.6 . . ? C13 C12 C11 121.13(19) . . ? C13 C12 H12 119.4 . . ? C11 C12 H12 119.4 . . ? C12 C13 C8 120.04(19) . . ? C12 C13 H13 120.0 . . ? C8 C13 H13 120.0 . . ? O1 C14 H14A 109.5 . . ? O1 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? O1 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C16 C15 C20 118.57(17) . . ? C16 C15 P1 125.63(14) . . ? C20 C15 P1 115.52(14) . . ? C17 C16 C15 120.06(18) . . ? C17 C16 H16 120.0 . . ? C15 C16 H16 120.0 . . ? C18 C17 C16 120.69(19) . . ? C18 C17 H17 119.7 . . ? C16 C17 H17 119.7 . . ? C17 C18 C19 119.76(18) . . ? C17 C18 H18 120.1 . . ? C19 C18 H18 120.1 . . ? C20 C19 C18 119.85(18) . . ? C20 C19 H19 120.1 . . ? C18 C19 H19 120.1 . . ? C19 C20 C15 121.03(17) . . ? C19 C20 H20 119.5 . . ? C15 C20 H20 119.5 . . ? C22 C21 C26 118.87(17) . . ? C22 C21 P1 122.43(14) . . ? C26 C21 P1 117.72(14) . . ? C21 C22 C23 120.15(19) . . ? C21 C22 H22 119.9 . . ? C23 C22 H22 119.9 . . ? C24 C23 C22 120.6(2) . . ? C24 C23 H23 119.7 . . ? C22 C23 H23 119.7 . . ? C23 C24 C25 119.71(19) . . ? C23 C24 H24 120.1 . . ? C25 C24 H24 120.1 . . ? C24 C25 C26 119.9(2) . . ? C24 C25 H25 120.0 . . ? C26 C25 H25 120.0 . . ? C25 C26 C21 120.70(19) . . ? C25 C26 H26 119.7 . . ? C21 C26 H26 119.7 . . ? C28 C27 C32 119.23(17) . . ? C28 C27 P1 120.21(14) . . ? C32 C27 P1 120.30(15) . . ? C29 C28 C27 120.26(18) . . ? C29 C28 H28 119.9 . . ? C27 C28 H28 119.9 . . ? C30 C29 C28 120.14(19) . . ? C30 C29 H29 119.9 . . ? C28 C29 H29 119.9 . . ? C29 C30 C31 120.02(18) . . ? C29 C30 H30 120.0 . . ? C31 C30 H30 120.0 . . ? C30 C31 C32 120.08(19) . . ? C30 C31 H31 120.0 . . ? C32 C31 H31 120.0 . . ? C31 C32 C27 120.11(19) . . ? C31 C32 H32 119.9 . . ? C27 C32 H32 119.9 . . ? C38 C33 C34 118.79(17) . . ? C38 C33 P2 121.45(15) . . ? C34 C33 P2 119.58(14) . . ? C35 C34 C33 120.80(18) . . ? C35 C34 H34 119.6 . . ? C33 C34 H34 119.6 . . ? C36 C35 C34 120.0(2) . . ? C36 C35 H35 120.0 . . ? C34 C35 H35 120.0 . . ? C37 C36 C35 119.68(19) . . ? C37 C36 H36 120.2 . . ? C35 C36 H36 120.2 . . ? C36 C37 C38 120.99(19) . . ? C36 C37 H37 119.5 . . ? C38 C37 H37 119.5 . . ? C37 C38 C33 119.70(19) . . ? C37 C38 H38 120.1 . . ? C33 C38 H38 120.1 . . ? C44 C39 C40 118.86(18) . . ? C44 C39 P2 122.58(15) . . ? C40 C39 P2 118.55(16) . . ? C41 C40 C39 120.0(2) . . ? C41 C40 H40 120.0 . . ? C39 C40 H40 120.0 . . ? C40 C41 C42 120.6(2) . . ? C40 C41 H41 119.7 . . ? C42 C41 H41 119.7 . . ? C43 C42 C41 119.6(2) . . ? C43 C42 H42 120.2 . . ? C41 C42 H42 120.2 . . ? C42 C43 C44 120.2(2) . . ? C42 C43 H43 119.9 . . ? C44 C43 H43 119.9 . . ? C43 C44 C39 120.6(2) . . ? C43 C44 H44 119.7 . . ? C39 C44 H44 119.7 . . ? C46 C45 C50 118.83(18) . . ? C46 C45 P2 123.54(15) . . ? C50 C45 P2 117.54(15) . . ? C47 C46 C45 120.1(2) . . ? C47 C46 H46 120.0 . . ? C45 C46 H46 120.0 . . ? C48 C47 C46 120.5(2) . . ? C48 C47 H47 119.7 . . ? C46 C47 H47 119.7 . . ? C47 C48 C49 120.0(2) . . ? C47 C48 H48 120.0 . . ? C49 C48 H48 120.0 . . ? C48 C49 C50 119.9(2) . . ? C48 C49 H49 120.1 . . ? C50 C49 H49 120.1 . . ? C49 C50 C45 120.7(2) . . ? C49 C50 H50 119.7 . . ? C45 C50 H50 119.7 . . ? C10 O1 C14 117.5(2) . . ? C27 P1 C21 103.71(9) . . ? C27 P1 C15 105.99(8) . . ? C21 P1 C15 94.77(8) . . ? C27 P1 Ru1 113.68(6) . . ? C21 P1 Ru1 126.10(6) . . ? C15 P1 Ru1 109.70(6) . . ? C45 P2 C33 106.06(9) . . ? C45 P2 C39 101.07(9) . . ? C33 P2 C39 103.09(9) . . ? C45 P2 Ru1 119.44(6) . . ? C33 P2 Ru1 112.06(6) . . ? C39 P2 Ru1 113.38(7) . . ? C6 Ru1 C5 117.56(8) . . ? C6 Ru1 C4 93.81(8) . . ? C5 Ru1 C4 36.89(7) . . ? C6 Ru1 C3 104.87(8) . . ? C5 Ru1 C3 61.35(7) . . ? C4 Ru1 C3 36.64(7) . . ? C6 Ru1 C1 153.84(8) . . ? C5 Ru1 C1 37.13(7) . . ? C4 Ru1 C1 61.36(7) . . ? C3 Ru1 C1 60.84(7) . . ? C6 Ru1 C2 140.06(8) . . ? C5 Ru1 C2 60.66(7) . . ? C4 Ru1 C2 60.60(7) . . ? C3 Ru1 C2 36.34(7) . . ? C1 Ru1 C2 35.71(7) . . ? C6 Ru1 P2 89.10(6) . . ? C5 Ru1 P2 88.43(5) . . ? C4 Ru1 P2 117.38(5) . . ? C3 Ru1 P2 149.77(5) . . ? C1 Ru1 P2 95.18(5) . . ? C2 Ru1 P2 128.99(5) . . ? C6 Ru1 P1 98.43(6) . . ? C5 Ru1 P1 143.66(5) . . ? C4 Ru1 P1 143.16(5) . . ? C3 Ru1 P1 106.51(5) . . ? C1 Ru1 P1 106.53(5) . . ? C2 Ru1 P1 88.95(5) . . ? P2 Ru1 P1 97.522(18) . . ? F1 C51 F3 107.3(2) . . ? F1 C51 F2 107.3(2) . . ? F3 C51 F2 107.5(2) . . ? F1 C51 S1 111.3(2) . . ? F3 C51 S1 111.89(18) . . ? F2 C51 S1 111.26(19) . . ? O4 S1 O2 115.44(11) . . ? O4 S1 O3 115.01(10) . . ? O2 S1 O3 114.86(9) . . ? O4 S1 C51 102.43(13) . . ? O2 S1 C51 103.12(12) . . ? O3 S1 C51 103.41(11) . . ? Cl2 C52 Cl1 111.6(3) . . ? Cl2 C52 H52A 109.3 . . ? Cl1 C52 H52A 109.3 . . ? Cl2 C52 H52B 109.3 . . ? Cl1 C52 H52B 109.3 . . ? H52A C52 H52B 108.0 . . ? C54 C53 H53A 109.5 . . ? C54 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C54 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? O5 C54 C53 104.2(7) . . ? O5 C54 H54A 110.9 . . ? C53 C54 H54A 110.9 . . ? O5 C54 H54B 110.9 . . ? C53 C54 H54B 110.9 . . ? H54A C54 H54B 108.9 . . ? O5 C55 C56 106.8(9) . . ? O5 C55 H55A 110.4 . . ? C56 C55 H55A 110.4 . . ? O5 C55 H55B 110.4 . . ? C56 C55 H55B 110.4 . . ? H55A C55 H55B 108.6 . . ? C55 C56 H56A 109.5 . . ? C55 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C55 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? C55 O5 C54 106.3(8) . . ? 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 C5 C1 C2 C3 0.4(2) . . . . ? Ru1 C1 C2 C3 -60.92(14) . . . . ? C5 C1 C2 Ru1 61.35(13) . . . . ? C1 C2 C3 C4 -1.5(2) . . . . ? Ru1 C2 C3 C4 -62.83(13) . . . . ? C1 C2 C3 Ru1 61.31(13) . . . . ? C2 C3 C4 C5 2.0(2) . . . . ? Ru1 C3 C4 C5 -62.24(13) . . . . ? C2 C3 C4 Ru1 64.26(13) . . . . ? C3 C4 C5 C1 -1.8(2) . . . . ? Ru1 C4 C5 C1 -65.16(13) . . . . ? C3 C4 C5 Ru1 63.40(13) . . . . ? C2 C1 C5 C4 0.8(2) . . . . ? Ru1 C1 C5 C4 64.48(13) . . . . ? C2 C1 C5 Ru1 -63.66(13) . . . . ? Ru1 C6 C7 C8 -138.6(9) . . . . ? C6 C7 C8 C9 -170.2(2) . . . . ? C6 C7 C8 C13 10.9(3) . . . . ? C13 C8 C9 C10 -0.5(3) . . . . ? C7 C8 C9 C10 -179.34(19) . . . . ? C8 C9 C10 O1 -179.9(2) . . . . ? C8 C9 C10 C11 0.0(3) . . . . ? O1 C10 C11 C12 -179.3(2) . . . . ? C9 C10 C11 C12 0.8(3) . . . . ? C10 C11 C12 C13 -1.3(3) . . . . ? C11 C12 C13 C8 0.8(3) . . . . ? C9 C8 C13 C12 0.0(3) . . . . ? C7 C8 C13 C12 178.87(19) . . . . ? C20 C15 C16 C17 -1.1(3) . . . . ? P1 C15 C16 C17 -174.77(16) . . . . ? C15 C16 C17 C18 2.0(3) . . . . ? C16 C17 C18 C19 -0.9(3) . . . . ? C17 C18 C19 C20 -0.9(3) . . . . ? C18 C19 C20 C15 1.8(3) . . . . ? C16 C15 C20 C19 -0.7(3) . . . . ? P1 C15 C20 C19 173.56(15) . . . . ? C26 C21 C22 C23 0.3(3) . . . . ? P1 C21 C22 C23 -168.13(15) . . . . ? C21 C22 C23 C24 -0.7(3) . . . . ? C22 C23 C24 C25 0.1(3) . . . . ? C23 C24 C25 C26 0.8(3) . . . . ? C24 C25 C26 C21 -1.2(3) . . . . ? C22 C21 C26 C25 0.6(3) . . . . ? P1 C21 C26 C25 169.59(15) . . . . ? C32 C27 C28 C29 0.5(3) . . . . ? P1 C27 C28 C29 174.66(14) . . . . ? C27 C28 C29 C30 2.5(3) . . . . ? C28 C29 C30 C31 -2.5(3) . . . . ? C29 C30 C31 C32 -0.5(3) . . . . ? C30 C31 C32 C27 3.6(3) . . . . ? C28 C27 C32 C31 -3.6(3) . . . . ? P1 C27 C32 C31 -177.68(14) . . . . ? C38 C33 C34 C35 -0.2(3) . . . . ? P2 C33 C34 C35 -175.30(16) . . . . ? C33 C34 C35 C36 0.5(3) . . . . ? C34 C35 C36 C37 -0.6(3) . . . . ? C35 C36 C37 C38 0.3(3) . . . . ? C36 C37 C38 C33 0.0(3) . . . . ? C34 C33 C38 C37 -0.1(3) . . . . ? P2 C33 C38 C37 174.95(16) . . . . ? C44 C39 C40 C41 -1.2(3) . . . . ? P2 C39 C40 C41 -179.70(19) . . . . ? C39 C40 C41 C42 0.2(4) . . . . ? C40 C41 C42 C43 1.5(4) . . . . ? C41 C42 C43 C44 -2.3(4) . . . . ? C42 C43 C44 C39 1.3(3) . . . . ? C40 C39 C44 C43 0.5(3) . . . . ? P2 C39 C44 C43 178.88(16) . . . . ? C50 C45 C46 C47 -1.2(3) . . . . ? P2 C45 C46 C47 -177.75(16) . . . . ? C45 C46 C47 C48 0.7(3) . . . . ? C46 C47 C48 C49 0.1(3) . . . . ? C47 C48 C49 C50 -0.3(3) . . . . ? C48 C49 C50 C45 -0.2(3) . . . . ? C46 C45 C50 C49 1.0(3) . . . . ? P2 C45 C50 C49 177.74(16) . . . . ? C11 C10 O1 C14 9.8(4) . . . . ? C9 C10 O1 C14 -170.3(3) . . . . ? C28 C27 P1 C21 35.83(17) . . . . ? C32 C27 P1 C21 -150.12(15) . . . . ? C28 C27 P1 C15 134.98(15) . . . . ? C32 C27 P1 C15 -50.97(17) . . . . ? C28 C27 P1 Ru1 -104.46(14) . . . . ? C32 C27 P1 Ru1 69.60(16) . . . . ? C22 C21 P1 C27 -149.30(15) . . . . ? C26 C21 P1 C27 42.12(16) . . . . ? C22 C21 P1 C15 102.95(16) . . . . ? C26 C21 P1 C15 -65.62(16) . . . . ? C22 C21 P1 Ru1 -15.71(19) . . . . ? C26 C21 P1 Ru1 175.72(12) . . . . ? C16 C15 P1 C27 -3.36(19) . . . . ? C20 C15 P1 C27 -177.16(14) . . . . ? C16 C15 P1 C21 102.38(18) . . . . ? C20 C15 P1 C21 -71.41(15) . . . . ? C16 C15 P1 Ru1 -126.47(16) . . . . ? C20 C15 P1 Ru1 59.73(15) . . . . ? C46 C45 P2 C33 -6.43(19) . . . . ? C50 C45 P2 C33 176.99(15) . . . . ? C46 C45 P2 C39 100.81(18) . . . . ? C50 C45 P2 C39 -75.77(16) . . . . ? C46 C45 P2 Ru1 -134.11(15) . . . . ? C50 C45 P2 Ru1 49.30(17) . . . . ? C38 C33 P2 C45 128.22(16) . . . . ? C34 C33 P2 C45 -56.80(18) . . . . ? C38 C33 P2 C39 22.44(18) . . . . ? C34 C33 P2 C39 -162.59(16) . . . . ? C38 C33 P2 Ru1 -99.82(16) . . . . ? C34 C33 P2 Ru1 75.15(16) . . . . ? C44 C39 P2 C45 147.30(17) . . . . ? C40 C39 P2 C45 -34.28(19) . . . . ? C44 C39 P2 C33 -103.13(18) . . . . ? C40 C39 P2 C33 75.29(18) . . . . ? C44 C39 P2 Ru1 18.24(19) . . . . ? C40 C39 P2 Ru1 -163.34(15) . . . . ? C7 C6 Ru1 C5 16.0(10) . . . . ? C7 C6 Ru1 C4 45.6(10) . . . . ? C7 C6 Ru1 C3 81.1(10) . . . . ? C7 C6 Ru1 C1 28.2(11) . . . . ? C7 C6 Ru1 C2 92.2(10) . . . . ? C7 C6 Ru1 P2 -71.8(10) . . . . ? C7 C6 Ru1 P1 -169.2(10) . . . . ? C4 C5 Ru1 C6 55.23(14) . . . . ? C1 C5 Ru1 C6 171.13(11) . . . . ? C1 C5 Ru1 C4 115.90(17) . . . . ? C4 C5 Ru1 C3 -37.33(11) . . . . ? C1 C5 Ru1 C3 78.57(12) . . . . ? C4 C5 Ru1 C1 -115.90(17) . . . . ? C4 C5 Ru1 C2 -79.09(12) . . . . ? C1 C5 Ru1 C2 36.81(11) . . . . ? C4 C5 Ru1 P2 143.39(11) . . . . ? C1 C5 Ru1 P2 -100.70(11) . . . . ? C4 C5 Ru1 P1 -116.02(12) . . . . ? C1 C5 Ru1 P1 -0.12(16) . . . . ? C5 C4 Ru1 C6 -133.12(12) . . . . ? C3 C4 Ru1 C6 109.96(12) . . . . ? C3 C4 Ru1 C5 -116.92(17) . . . . ? C5 C4 Ru1 C3 116.92(17) . . . . ? C5 C4 Ru1 C1 38.22(11) . . . . ? C3 C4 Ru1 C1 -78.69(13) . . . . ? C5 C4 Ru1 C2 79.27(12) . . . . ? C3 C4 Ru1 C2 -37.65(12) . . . . ? C5 C4 Ru1 P2 -42.16(12) . . . . ? C3 C4 Ru1 P2 -159.08(10) . . . . ? C5 C4 Ru1 P1 117.37(11) . . . . ? C3 C4 Ru1 P1 0.46(17) . . . . ? C4 C3 Ru1 C6 -76.01(13) . . . . ? C2 C3 Ru1 C6 167.91(12) . . . . ? C4 C3 Ru1 C5 37.59(12) . . . . ? C2 C3 Ru1 C5 -78.49(12) . . . . ? C2 C3 Ru1 C4 -116.08(17) . . . . ? C4 C3 Ru1 C1 80.24(12) . . . . ? C2 C3 Ru1 C1 -35.84(11) . . . . ? C4 C3 Ru1 C2 116.08(17) . . . . ? C4 C3 Ru1 P2 39.04(18) . . . . ? C2 C3 Ru1 P2 -77.04(15) . . . . ? C4 C3 Ru1 P1 -179.71(10) . . . . ? C2 C3 Ru1 P1 64.20(11) . . . . ? C2 C1 Ru1 C6 98.47(19) . . . . ? C5 C1 Ru1 C6 -18.1(2) . . . . ? C2 C1 Ru1 C5 116.52(17) . . . . ? C2 C1 Ru1 C4 78.55(12) . . . . ? C5 C1 Ru1 C4 -37.97(11) . . . . ? C2 C1 Ru1 C3 36.47(11) . . . . ? C5 C1 Ru1 C3 -80.06(12) . . . . ? C5 C1 Ru1 C2 -116.52(17) . . . . ? C2 C1 Ru1 P2 -162.99(11) . . . . ? C5 C1 Ru1 P2 80.49(11) . . . . ? C2 C1 Ru1 P1 -63.55(12) . . . . ? C5 C1 Ru1 P1 179.93(10) . . . . ? C1 C2 Ru1 C6 -137.22(13) . . . . ? C3 C2 Ru1 C6 -18.38(18) . . . . ? C1 C2 Ru1 C5 -38.29(11) . . . . ? C3 C2 Ru1 C5 80.56(12) . . . . ? C1 C2 Ru1 C4 -80.87(12) . . . . ? C3 C2 Ru1 C4 37.97(11) . . . . ? C1 C2 Ru1 C3 -118.84(17) . . . . ? C3 C2 Ru1 C1 118.84(17) . . . . ? C1 C2 Ru1 P2 22.02(14) . . . . ? C3 C2 Ru1 P2 140.86(10) . . . . ? C1 C2 Ru1 P1 120.86(11) . . . . ? C3 C2 Ru1 P1 -120.30(11) . . . . ? C45 P2 Ru1 C6 -71.20(9) . . . . ? C33 P2 Ru1 C6 163.95(9) . . . . ? C39 P2 Ru1 C6 47.75(9) . . . . ? C45 P2 Ru1 C5 171.20(9) . . . . ? C33 P2 Ru1 C5 46.35(9) . . . . ? C39 P2 Ru1 C5 -69.85(9) . . . . ? C45 P2 Ru1 C4 -165.03(9) . . . . ? C33 P2 Ru1 C4 70.12(9) . . . . ? C39 P2 Ru1 C4 -46.07(9) . . . . ? C45 P2 Ru1 C3 169.93(13) . . . . ? C33 P2 Ru1 C3 45.08(13) . . . . ? C39 P2 Ru1 C3 -71.12(13) . . . . ? C45 P2 Ru1 C1 134.65(9) . . . . ? C33 P2 Ru1 C1 9.79(8) . . . . ? C39 P2 Ru1 C1 -106.40(8) . . . . ? C45 P2 Ru1 C2 121.95(10) . . . . ? C33 P2 Ru1 C2 -2.90(10) . . . . ? C39 P2 Ru1 C2 -119.09(9) . . . . ? C45 P2 Ru1 P1 27.18(8) . . . . ? C33 P2 Ru1 P1 -97.67(7) . . . . ? C39 P2 Ru1 P1 146.14(7) . . . . ? C27 P1 Ru1 C6 138.49(9) . . . . ? C21 P1 Ru1 C6 8.70(9) . . . . ? C15 P1 Ru1 C6 -103.05(9) . . . . ? C27 P1 Ru1 C5 -49.34(11) . . . . ? C21 P1 Ru1 C5 -179.14(11) . . . . ? C15 P1 Ru1 C5 69.11(11) . . . . ? C27 P1 Ru1 C4 -113.46(11) . . . . ? C21 P1 Ru1 C4 116.74(11) . . . . ? C15 P1 Ru1 C4 4.99(11) . . . . ? C27 P1 Ru1 C3 -113.17(9) . . . . ? C21 P1 Ru1 C3 117.03(9) . . . . ? C15 P1 Ru1 C3 5.28(8) . . . . ? C27 P1 Ru1 C1 -49.42(9) . . . . ? C21 P1 Ru1 C1 -179.21(9) . . . . ? C15 P1 Ru1 C1 69.04(8) . . . . ? C27 P1 Ru1 C2 -80.93(9) . . . . ? C21 P1 Ru1 C2 149.27(9) . . . . ? C15 P1 Ru1 C2 37.52(8) . . . . ? C27 P1 Ru1 P2 48.29(7) . . . . ? C21 P1 Ru1 P2 -81.51(7) . . . . ? C15 P1 Ru1 P2 166.74(6) . . . . ? F1 C51 S1 O4 60.7(2) . . . . ? F3 C51 S1 O4 -179.18(19) . . . . ? F2 C51 S1 O4 -58.9(2) . . . . ? F1 C51 S1 O2 -179.08(19) . . . . ? F3 C51 S1 O2 -59.0(2) . . . . ? F2 C51 S1 O2 61.3(2) . . . . ? F1 C51 S1 O3 -59.1(2) . . . . ? F3 C51 S1 O3 61.0(2) . . . . ? F2 C51 S1 O3 -178.76(19) . . . . ? C56 C55 O5 C54 169.8(16) . . . . ? C53 C54 O5 C55 176.2(16) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 28.32 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.677 _refine_diff_density_min -0.574 _refine_diff_density_rms 0.071 data_CCDC737833_compound5a[OTf] _database_code_depnum_ccdc_archive 'CCDC 737833' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C48 H43 N2 O3 P2 Ru, C7 H8, C F3 O3 S' _chemical_formula_sum 'C56 H51 F3 N2 O6 P2 Ru S' _chemical_formula_weight 1100.06 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' S S 0.1246 0.1234 '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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.6129(5) _cell_length_b 14.4787(6) _cell_length_c 15.9001(6) _cell_angle_alpha 95.0100(10) _cell_angle_beta 92.9140(10) _cell_angle_gamma 108.1500(10) _cell_volume 2522.10(18) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 8129 _cell_measurement_theta_min 2.36 _cell_measurement_theta_max 29.98 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.449 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1132 _exptl_absorpt_coefficient_mu 0.480 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.848 _exptl_absorpt_correction_T_max 0.977 _exptl_absorpt_process_details 'SADABS v2.03; (Sheldrick)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 38454 _diffrn_reflns_av_R_equivalents 0.0207 _diffrn_reflns_av_sigmaI/netI 0.0280 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.49 _diffrn_reflns_theta_max 30.02 _reflns_number_total 14406 _reflns_number_gt 12729 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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. The triflate anion was disordered and modelled over two sites, the relative occupancy of which refined to 55%:45%. S=O bond lengths were restrained to 1.43 angstroms, C-F bond lengths were restrained to 1.32 angstroms. The toluene of crystallization was disordered and modelled over two sites, the relative occupancy of which refined to 50%:50%. The phenyl rings of the toluene were restrained to regular hexagons of 1.36 angstroms. ; _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^)+(0.0491P)^2^+1.1565P] 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 14406 _refine_ls_number_parameters 738 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0411 _refine_ls_R_factor_gt 0.0351 _refine_ls_wR_factor_ref 0.0924 _refine_ls_wR_factor_gt 0.0889 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.057 _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 C1 C 0.41365(18) 0.57529(14) 0.63897(12) 0.0336(4) Uani 1 1 d . . . H1 H 0.3628 0.5312 0.6774 0.040 Uiso 1 1 calc R . . C2 C 0.39967(17) 0.66514(14) 0.61558(12) 0.0336(4) Uani 1 1 d . . . H2 H 0.3356 0.6936 0.6338 0.040 Uiso 1 1 calc R . . C3 C 0.48256(18) 0.69977(14) 0.55457(12) 0.0335(4) Uani 1 1 d . . . H3 H 0.4878 0.7574 0.5228 0.040 Uiso 1 1 calc R . . C4 C 0.55223(19) 0.63580(14) 0.54284(11) 0.0338(4) Uani 1 1 d . . . H4 H 0.6148 0.6399 0.5011 0.041 Uiso 1 1 calc R . . C5 C 0.50856(19) 0.55892(13) 0.59512(12) 0.0332(4) Uani 1 1 d . . . H5 H 0.5370 0.5006 0.5971 0.040 Uiso 1 1 calc R . . C6 C 0.70274(15) 0.83358(12) 0.67620(11) 0.0235(3) Uani 1 1 d . . . C7 C 0.76717(17) 0.86615(13) 0.59734(12) 0.0284(3) Uani 1 1 d . . . H7A H 0.8518 0.8655 0.6070 0.034 Uiso 1 1 calc R . . H7B H 0.7279 0.8152 0.5499 0.034 Uiso 1 1 calc R . . C8 C 0.77366(17) 0.96351(13) 0.56699(12) 0.0296(4) Uani 1 1 d . . . C9 C 0.87960(18) 1.03236(14) 0.55807(13) 0.0335(4) Uani 1 1 d . . . H9 H 0.9531 1.0221 0.5772 0.040 Uiso 1 1 calc R . . C10 C 0.78610(19) 1.13784(14) 0.49198(13) 0.0337(4) Uani 1 1 d . . . C11 C 0.66296(17) 0.98074(13) 0.53796(12) 0.0306(4) Uani 1 1 d . . . C12 C 0.8310(2) 0.98991(16) 0.75374(15) 0.0468(5) Uani 1 1 d . . . H12A H 0.9016 0.9836 0.7255 0.070 Uiso 1 1 calc R . . H12B H 0.8551 1.0129 0.8138 0.070 Uiso 1 1 calc R . . H12C H 0.8000 1.0370 0.7272 0.070 Uiso 1 1 calc R . . C13 C 0.85044(18) 0.56582(17) 0.49106(13) 0.0375(4) Uani 1 1 d . . . H13 H 0.8691 0.5940 0.4397 0.045 Uiso 1 1 calc R . . C14 C 0.61259(16) 0.77482(16) 0.90708(11) 0.0330(4) Uani 1 1 d . . . C15 C 0.6159(2) 0.7012(2) 0.95633(13) 0.0438(5) Uani 1 1 d . . . H15 H 0.5656 0.6359 0.9395 0.053 Uiso 1 1 calc R . . C16 C 0.6937(3) 0.7230(3) 1.03126(15) 0.0595(7) Uani 1 1 d . . . H16 H 0.6951 0.6722 1.0649 0.071 Uiso 1 1 calc R . . C17 C 0.7677(2) 0.8168(3) 1.05618(15) 0.0642(9) Uani 1 1 d . . . H17 H 0.8197 0.8310 1.1069 0.077 Uiso 1 1 calc R . . C18 C 0.7659(2) 0.8897(2) 1.00755(15) 0.0544(7) Uani 1 1 d . . . H18 H 0.8172 0.9546 1.0246 0.065 Uiso 1 1 calc R . . C19 C 0.68981(18) 0.86986(18) 0.93344(13) 0.0416(5) Uani 1 1 d . . . H19 H 0.6901 0.9213 0.9002 0.050 Uiso 1 1 calc R . . C20 C 0.26602(19) 0.69152(18) 0.80909(18) 0.0486(6) Uani 1 1 d . . . H20 H 0.2725 0.7557 0.7962 0.058 Uiso 1 1 calc R . . C21 C 0.1518(2) 0.6240(2) 0.8130(2) 0.0662(8) Uani 1 1 d . . . H21 H 0.0813 0.6424 0.8016 0.079 Uiso 1 1 calc R . . C22 C 0.1391(2) 0.5321(2) 0.8329(2) 0.0616(8) Uani 1 1 d . . . H22 H 0.0608 0.4869 0.8368 0.074 Uiso 1 1 calc R . . C23 C 0.2420(2) 0.5060(2) 0.84736(19) 0.0564(7) Uani 1 1 d . . . H23 H 0.2344 0.4420 0.8613 0.068 Uiso 1 1 calc R . . C24 C 0.35654(19) 0.57179(17) 0.84180(15) 0.0428(5) Uani 1 1 d . . . H24 H 0.4263 0.5517 0.8506 0.051 Uiso 1 1 calc R . . C25 C 0.37093(16) 0.66651(14) 0.82367(12) 0.0309(4) Uani 1 1 d . . . C26 C 0.48170(16) 0.86555(14) 0.80642(12) 0.0305(4) Uani 1 1 d . . . C27 C 0.47289(17) 0.90819(14) 0.73284(14) 0.0342(4) Uani 1 1 d . . . H27 H 0.4917 0.8804 0.6811 0.041 Uiso 1 1 calc R . . C28 C 0.4368(2) 0.99145(16) 0.73389(18) 0.0459(5) Uani 1 1 d . . . H28 H 0.4306 1.0202 0.6831 0.055 Uiso 1 1 calc R . . C29 C 0.4099(2) 1.03207(17) 0.8098(2) 0.0540(7) Uani 1 1 d . . . H29 H 0.3861 1.0893 0.8110 0.065 Uiso 1 1 calc R . . C30 C 0.4175(2) 0.98992(19) 0.88282(18) 0.0524(6) Uani 1 1 d . . . H30 H 0.3989 1.0181 0.9345 0.063 Uiso 1 1 calc R . . C31 C 0.45201(19) 0.90647(17) 0.88196(15) 0.0420(5) Uani 1 1 d . . . H31 H 0.4555 0.8770 0.9327 0.050 Uiso 1 1 calc R . . C32 C 0.72923(18) 0.56887(14) 0.80559(12) 0.0312(4) Uani 1 1 d . . . C33 C 0.8208(2) 0.57266(19) 0.86690(14) 0.0438(5) Uani 1 1 d . . . H33 H 0.8978 0.6216 0.8685 0.053 Uiso 1 1 calc R . . C34 C 0.7999(3) 0.5050(2) 0.92598(17) 0.0596(7) Uani 1 1 d . . . H34 H 0.8629 0.5082 0.9678 0.072 Uiso 1 1 calc R . . C35 C 0.6897(3) 0.4337(2) 0.92443(18) 0.0598(7) Uani 1 1 d . . . H35 H 0.6758 0.3883 0.9655 0.072 Uiso 1 1 calc R . . C36 C 0.5988(3) 0.42800(18) 0.86300(17) 0.0525(6) Uani 1 1 d . . . H36 H 0.5228 0.3777 0.8610 0.063 Uiso 1 1 calc R . . C37 C 0.6179(2) 0.49557(15) 0.80399(14) 0.0401(4) Uani 1 1 d . . . H37 H 0.5546 0.4916 0.7623 0.048 Uiso 1 1 calc R . . C38 C 0.79450(16) 0.57970(13) 0.63566(12) 0.0289(3) Uani 1 1 d . . . C39 C 0.7993(2) 0.48545(15) 0.64247(15) 0.0389(4) Uani 1 1 d . . . H39 H 0.7836 0.4575 0.6943 0.047 Uiso 1 1 calc R . . C40 C 0.8270(2) 0.43216(16) 0.57343(17) 0.0462(5) Uani 1 1 d . . . H40 H 0.8284 0.3676 0.5783 0.055 Uiso 1 1 calc R . . C41 C 0.85224(18) 0.47203(16) 0.49845(15) 0.0415(5) Uani 1 1 d . . . H41 H 0.8709 0.4351 0.4518 0.050 Uiso 1 1 calc R . . C42 C 0.82117(17) 0.61886(14) 0.55918(12) 0.0320(4) Uani 1 1 d . . . H42 H 0.8193 0.6832 0.5535 0.038 Uiso 1 1 calc R . . C43 C 0.89451(15) 0.74709(13) 0.75831(11) 0.0257(3) Uani 1 1 d . . . C44 C 0.90182(17) 0.80011(16) 0.83667(13) 0.0375(4) Uani 1 1 d . . . H44 H 0.8369 0.7815 0.8721 0.045 Uiso 1 1 calc R . . C45 C 1.00315(19) 0.87994(19) 0.86339(15) 0.0480(6) Uani 1 1 d . . . H45 H 1.0075 0.9153 0.9173 0.058 Uiso 1 1 calc R . . C46 C 1.09817(19) 0.90862(18) 0.81224(15) 0.0468(5) Uani 1 1 d . . . H46 H 1.1664 0.9646 0.8301 0.056 Uiso 1 1 calc R . . C47 C 0.99227(17) 0.77448(14) 0.70823(12) 0.0318(4) Uani 1 1 d . . . H47 H 0.9900 0.7377 0.6553 0.038 Uiso 1 1 calc R . . C48 C 1.09294(18) 0.85539(16) 0.73543(14) 0.0390(4) Uani 1 1 d . . . H48 H 1.1587 0.8740 0.7006 0.047 Uiso 1 1 calc R . . N1 N 0.88650(15) 1.11665(12) 0.52259(11) 0.0350(3) Uani 1 1 d . . . H1A H 0.9536 1.1625 0.5264 0.042 Uiso 1 1 d R . . N2 N 0.67768(15) 1.06723(12) 0.50248(11) 0.0326(3) Uani 1 1 d . . . H2A H 0.6128 1.0748 0.4796 0.039 Uiso 1 1 d R . . O1 O 0.73612(12) 0.89503(9) 0.74589(8) 0.0300(3) Uani 1 1 d . . . O2 O 0.79157(15) 1.21166(11) 0.45909(10) 0.0421(3) Uani 1 1 d . . . O3 O 0.56009(13) 0.92449(10) 0.54358(10) 0.0392(3) Uani 1 1 d . . . P1 P 0.52070(4) 0.75177(3) 0.80478(3) 0.02418(9) Uani 1 1 d . . . P2 P 0.75107(4) 0.65119(3) 0.72235(3) 0.02331(9) Uani 1 1 d . . . Ru1 Ru 0.587432(11) 0.702754(9) 0.678431(8) 0.02050(4) Uani 1 1 d . . . C49 C 0.3320(4) 0.2393(3) 0.6755(2) 0.0534(12) Uani 0.556(4) 1 d PD A 1 F1 F 0.3686(7) 0.1828(6) 0.6223(3) 0.154(3) Uani 0.556(4) 1 d PD A 1 F2 F 0.3887(7) 0.3191(6) 0.6472(5) 0.154(4) Uani 0.556(4) 1 d PD A 1 F3 F 0.3811(5) 0.2373(5) 0.7519(3) 0.0731(14) Uani 0.556(4) 1 d PD A 1 O4 O 0.1193(3) 0.1217(3) 0.6978(2) 0.179(2) Uani 0.556(4) 1 d PD A 1 O5 O 0.13926(15) 0.20678(14) 0.57481(10) 0.0503(4) Uani 0.556(4) 1 d PD A 1 O6 O 0.1575(7) 0.2798(7) 0.7297(4) 0.211(7) Uani 0.556(4) 1 d PD A 1 S1 S 0.17468(16) 0.2126(2) 0.66637(9) 0.0731(7) Uani 0.556(4) 1 d PD A 1 C49A C 0.2700(6) 0.2711(6) 0.6968(5) 0.100(3) Uani 0.444(4) 1 d PD A 2 F1A F 0.3291(9) 0.2589(7) 0.7666(4) 0.116(3) Uani 0.444(4) 1 d PD A 2 F2A F 0.3518(8) 0.3392(3) 0.6643(5) 0.110(4) Uani 0.444(4) 1 d PD A 2 F3A F 0.1997(12) 0.3259(6) 0.7105(5) 0.187(6) Uani 0.444(4) 1 d PD A 2 O4A O 0.13926(15) 0.20678(14) 0.57481(10) 0.0503(4) Uani 0.444(4) 1 d PD A 2 O5A O 0.1193(3) 0.1217(3) 0.6978(2) 0.179(2) Uani 0.444(4) 1 d PD A 2 O6A O 0.2759(9) 0.1177(8) 0.6213(5) 0.164(6) Uani 0.444(4) 1 d PD A 2 S1A S 0.19133(15) 0.16641(11) 0.64073(14) 0.0469(5) Uani 0.444(4) 1 d PD A 2 C50 C 0.1503(6) 0.7596(4) 0.1891(2) 0.0483(15) Uani 0.507(7) 1 d PG B 3 C51 C 0.2654(5) 0.7990(5) 0.1616(4) 0.064(2) Uani 0.507(7) 1 d PG B 3 H51 H 0.3356 0.8109 0.1996 0.077 Uiso 0.507(7) 1 calc PR B 3 C52 C 0.2778(4) 0.8209(5) 0.0785(5) 0.077(2) Uani 0.507(7) 1 d PG B 3 H52 H 0.3565 0.8478 0.0596 0.092 Uiso 0.507(7) 1 calc PR B 3 C53 C 0.1752(5) 0.8034(6) 0.0229(3) 0.068(2) Uani 0.507(7) 1 d PG B 3 H53 H 0.1837 0.8184 -0.0339 0.082 Uiso 0.507(7) 1 calc PR B 3 C54 C 0.0601(4) 0.7641(7) 0.0505(3) 0.074(3) Uani 0.507(7) 1 d PG B 3 H54 H -0.0101 0.7521 0.0125 0.089 Uiso 0.507(7) 1 calc PR B 3 C55 C 0.0476(4) 0.7422(5) 0.1336(3) 0.0496(17) Uani 0.507(7) 1 d PG B 3 H55 H -0.0310 0.7153 0.1524 0.060 Uiso 0.507(7) 1 calc PR B 3 C56 C 0.1382(8) 0.7380(5) 0.2775(4) 0.083(3) Uani 0.507(7) 1 d P B 3 H56A H 0.0778 0.7648 0.3016 0.125 Uiso 0.507(7) 1 calc PR B 3 H56B H 0.2168 0.7677 0.3104 0.125 Uiso 0.507(7) 1 calc PR B 3 H56C H 0.1119 0.6670 0.2793 0.125 Uiso 0.507(7) 1 calc PR B 3 C50A C 0.1065(7) 0.7376(5) 0.1994(5) 0.073(3) Uani 0.493(7) 1 d PG B 4 H50A H 0.0726 0.7172 0.2504 0.088 Uiso 0.493(7) 1 calc PR B 4 C51A C 0.2320(6) 0.7723(4) 0.1966(4) 0.0596(18) Uani 0.493(7) 1 d PG B 4 C52A C 0.2817(4) 0.8022(5) 0.1219(5) 0.073(2) Uani 0.493(7) 1 d PG B 4 H52A H 0.3674 0.8259 0.1200 0.088 Uiso 0.493(7) 1 calc PR B 4 C53A C 0.2058(8) 0.7973(7) 0.0500(4) 0.085(3) Uani 0.493(7) 1 d PG B 4 H53A H 0.2397 0.8177 -0.0010 0.102 Uiso 0.493(7) 1 calc PR B 4 C54A C 0.0803(8) 0.7626(8) 0.0528(5) 0.097(5) Uani 0.493(7) 1 d PG B 4 H54A H 0.0285 0.7592 0.0037 0.117 Uiso 0.493(7) 1 calc PR B 4 C55A C 0.0307(4) 0.7327(7) 0.1275(7) 0.124(6) Uani 0.493(7) 1 d PG B 4 H55A H -0.0551 0.7090 0.1294 0.149 Uiso 0.493(7) 1 calc PR B 4 C56A C 0.3194(8) 0.7776(5) 0.2723(6) 0.091(3) Uani 0.493(7) 1 d P B 4 H56D H 0.3469 0.8442 0.3013 0.137 Uiso 0.493(7) 1 calc PR B 4 H56E H 0.3896 0.7604 0.2531 0.137 Uiso 0.493(7) 1 calc PR B 4 H56F H 0.2781 0.7318 0.3113 0.137 Uiso 0.493(7) 1 calc PR B 4 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 C1 0.0348(9) 0.0287(9) 0.0286(9) -0.0043(7) -0.0082(7) 0.0013(7) C2 0.0297(9) 0.0347(9) 0.0327(9) -0.0080(7) -0.0106(7) 0.0100(7) C3 0.0417(10) 0.0308(9) 0.0263(8) -0.0005(7) -0.0104(7) 0.0122(8) C4 0.0470(11) 0.0353(9) 0.0183(8) -0.0056(7) -0.0041(7) 0.0155(8) C5 0.0465(11) 0.0241(8) 0.0256(8) -0.0084(6) -0.0122(8) 0.0116(8) C6 0.0226(7) 0.0248(7) 0.0259(8) 0.0028(6) 0.0023(6) 0.0115(6) C7 0.0305(8) 0.0281(8) 0.0328(9) 0.0098(7) 0.0099(7) 0.0150(7) C8 0.0326(9) 0.0290(8) 0.0323(9) 0.0093(7) 0.0080(7) 0.0146(7) C9 0.0348(9) 0.0347(9) 0.0367(10) 0.0112(8) 0.0103(8) 0.0161(8) C10 0.0417(10) 0.0289(9) 0.0340(9) 0.0060(7) 0.0095(8) 0.0143(8) C11 0.0345(9) 0.0270(8) 0.0352(9) 0.0096(7) 0.0085(7) 0.0143(7) C12 0.0524(13) 0.0306(10) 0.0403(11) 0.0017(8) -0.0070(10) -0.0092(9) C13 0.0333(9) 0.0507(12) 0.0292(9) -0.0075(8) 0.0022(7) 0.0176(9) C14 0.0259(8) 0.0522(11) 0.0219(8) -0.0066(7) 0.0020(6) 0.0169(8) C15 0.0416(11) 0.0666(15) 0.0286(10) 0.0025(9) 0.0007(8) 0.0261(11) C16 0.0584(15) 0.101(2) 0.0320(11) 0.0041(13) -0.0031(10) 0.0450(16) C17 0.0476(13) 0.118(3) 0.0294(11) -0.0254(14) -0.0114(10) 0.0406(16) C18 0.0345(11) 0.0853(19) 0.0370(12) -0.0287(12) -0.0043(9) 0.0205(12) C19 0.0301(9) 0.0602(14) 0.0301(9) -0.0176(9) 0.0018(7) 0.0142(9) C20 0.0278(10) 0.0446(12) 0.0764(17) 0.0165(12) 0.0087(10) 0.0122(9) C21 0.0254(10) 0.0626(17) 0.114(3) 0.0300(17) 0.0116(13) 0.0131(11) C22 0.0282(10) 0.0630(16) 0.089(2) 0.0315(15) 0.0084(12) 0.0013(10) C23 0.0391(12) 0.0531(14) 0.0758(18) 0.0348(13) 0.0052(11) 0.0056(10) C24 0.0308(10) 0.0485(12) 0.0510(13) 0.0209(10) 0.0039(9) 0.0110(9) C25 0.0240(8) 0.0391(10) 0.0288(9) 0.0051(7) 0.0044(6) 0.0082(7) C26 0.0237(8) 0.0305(9) 0.0358(9) -0.0074(7) 0.0029(7) 0.0092(7) C27 0.0293(9) 0.0286(9) 0.0452(11) -0.0019(8) 0.0046(8) 0.0112(7) C28 0.0386(11) 0.0326(10) 0.0699(16) 0.0041(10) 0.0079(10) 0.0159(9) C29 0.0380(11) 0.0307(10) 0.093(2) -0.0134(12) 0.0109(12) 0.0150(9) C30 0.0390(11) 0.0496(13) 0.0662(16) -0.0257(12) 0.0058(11) 0.0188(10) C31 0.0348(10) 0.0467(12) 0.0431(11) -0.0141(9) 0.0051(8) 0.0159(9) C32 0.0380(9) 0.0329(9) 0.0291(9) 0.0078(7) 0.0092(7) 0.0183(8) C33 0.0409(11) 0.0587(14) 0.0404(11) 0.0201(10) 0.0078(9) 0.0233(10) C34 0.0612(16) 0.0810(19) 0.0510(14) 0.0343(14) 0.0072(12) 0.0353(15) C35 0.0816(19) 0.0597(16) 0.0523(15) 0.0329(13) 0.0209(14) 0.0331(15) C36 0.0648(16) 0.0407(12) 0.0508(14) 0.0170(10) 0.0157(12) 0.0101(11) C37 0.0479(12) 0.0347(10) 0.0375(11) 0.0095(8) 0.0071(9) 0.0111(9) C38 0.0297(8) 0.0268(8) 0.0311(9) -0.0031(7) 0.0031(7) 0.0121(7) C39 0.0438(11) 0.0288(9) 0.0475(12) 0.0024(8) 0.0133(9) 0.0154(8) C40 0.0468(12) 0.0298(10) 0.0639(15) -0.0079(10) 0.0130(11) 0.0168(9) C41 0.0311(9) 0.0450(11) 0.0456(12) -0.0184(9) 0.0039(8) 0.0140(8) C42 0.0356(9) 0.0339(9) 0.0286(9) -0.0022(7) 0.0039(7) 0.0153(8) C43 0.0241(7) 0.0288(8) 0.0262(8) 0.0009(6) -0.0005(6) 0.0122(6) C44 0.0249(8) 0.0505(12) 0.0339(10) -0.0105(9) 0.0018(7) 0.0117(8) C45 0.0302(10) 0.0606(14) 0.0425(12) -0.0213(10) -0.0002(8) 0.0067(9) C46 0.0282(9) 0.0522(13) 0.0495(13) -0.0123(10) -0.0030(9) 0.0035(9) C47 0.0330(9) 0.0346(9) 0.0278(9) 0.0019(7) 0.0046(7) 0.0109(7) C48 0.0303(9) 0.0457(11) 0.0378(10) 0.0031(9) 0.0066(8) 0.0075(8) N1 0.0345(8) 0.0298(8) 0.0424(9) 0.0121(7) 0.0091(7) 0.0095(7) N2 0.0358(8) 0.0293(8) 0.0381(9) 0.0113(6) 0.0058(7) 0.0158(7) O1 0.0302(6) 0.0241(6) 0.0295(6) -0.0021(5) -0.0002(5) 0.0017(5) O2 0.0508(9) 0.0306(7) 0.0495(9) 0.0164(6) 0.0110(7) 0.0151(6) O3 0.0324(7) 0.0335(7) 0.0578(9) 0.0199(7) 0.0088(6) 0.0143(6) P1 0.02126(19) 0.0291(2) 0.02135(19) -0.00211(16) 0.00192(15) 0.00807(16) P2 0.0267(2) 0.02311(19) 0.02190(19) 0.00110(15) 0.00313(15) 0.01062(16) Ru1 0.02361(7) 0.01932(6) 0.01813(6) -0.00164(4) -0.00022(4) 0.00746(5) C49 0.046(2) 0.079(3) 0.035(2) 0.016(2) -0.0037(18) 0.018(2) F1 0.182(6) 0.245(9) 0.081(3) -0.071(4) -0.046(4) 0.168(7) F2 0.072(3) 0.260(10) 0.076(4) 0.098(5) -0.010(3) -0.044(4) F3 0.071(3) 0.084(3) 0.053(2) 0.023(2) -0.0225(19) 0.009(2) O4 0.126(3) 0.191(4) 0.140(3) 0.126(3) -0.055(2) -0.081(3) O5 0.0402(8) 0.0681(11) 0.0452(9) 0.0204(8) 0.0066(7) 0.0166(8) O6 0.111(5) 0.48(2) 0.069(4) -0.024(7) 0.033(4) 0.152(9) S1 0.0713(10) 0.0967(17) 0.0341(6) 0.0075(8) 0.0081(6) 0.0014(10) C49A 0.107(8) 0.116(8) 0.087(7) 0.054(6) 0.035(6) 0.036(7) F1A 0.156(9) 0.109(6) 0.044(3) 0.024(3) -0.024(4) -0.015(5) F2A 0.159(8) 0.0287(19) 0.092(5) 0.022(2) -0.015(4) -0.041(3) F3A 0.425(18) 0.101(5) 0.095(5) 0.009(4) 0.082(7) 0.161(8) O4A 0.0402(8) 0.0681(11) 0.0452(9) 0.0204(8) 0.0066(7) 0.0166(8) O5A 0.126(3) 0.191(4) 0.140(3) 0.126(3) -0.055(2) -0.081(3) O6A 0.256(12) 0.185(9) 0.102(5) -0.094(6) -0.110(8) 0.190(10) S1A 0.0509(8) 0.0313(7) 0.0527(10) 0.0042(6) -0.0132(7) 0.0077(6) C50 0.064(5) 0.034(3) 0.048(3) 0.004(2) 0.008(3) 0.016(3) C51 0.055(4) 0.080(5) 0.055(5) -0.001(4) -0.002(3) 0.021(4) C52 0.051(4) 0.110(7) 0.064(5) 0.002(5) -0.001(4) 0.020(4) C53 0.062(5) 0.097(6) 0.049(4) 0.010(4) 0.003(3) 0.030(4) C54 0.058(4) 0.122(10) 0.040(4) 0.004(5) 0.005(3) 0.027(5) C55 0.049(3) 0.053(4) 0.047(4) 0.007(3) 0.006(3) 0.014(3) C56 0.143(7) 0.069(4) 0.049(3) 0.020(3) 0.013(4) 0.045(4) C50A 0.060(5) 0.045(4) 0.111(7) 0.023(4) 0.039(5) 0.004(3) C51A 0.062(4) 0.033(3) 0.076(5) 0.002(3) 0.027(4) 0.002(3) C52A 0.063(4) 0.082(5) 0.065(6) 0.010(5) 0.015(4) 0.007(4) C53A 0.080(7) 0.105(7) 0.068(6) 0.017(5) 0.015(6) 0.022(6) C54A 0.070(6) 0.087(9) 0.116(11) 0.028(7) -0.025(6) -0.001(5) C55A 0.070(7) 0.114(11) 0.171(16) 0.039(10) -0.003(8) 0.001(7) C56A 0.087(5) 0.064(4) 0.106(6) 0.019(4) -0.009(4) 0.000(4) _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 C1 C5 1.403(3) . ? C1 C2 1.438(3) . ? C1 Ru1 2.2849(18) . ? C1 H1 1.0000 . ? C2 C3 1.414(3) . ? C2 Ru1 2.2345(18) . ? C2 H2 1.0000 . ? C3 C4 1.414(3) . ? C3 Ru1 2.2521(18) . ? C3 H3 1.0000 . ? C4 C5 1.428(3) . ? C4 Ru1 2.2480(17) . ? C4 H4 1.0000 . ? C5 Ru1 2.2665(17) . ? C5 H5 1.0000 . ? C6 O1 1.319(2) . ? C6 C7 1.527(2) . ? C6 Ru1 1.9541(17) . ? C7 C8 1.511(2) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.344(3) . ? C8 C11 1.445(3) . ? C9 N1 1.370(2) . ? C9 H9 0.9500 . ? C10 O2 1.216(2) . ? C10 N1 1.372(3) . ? C10 N2 1.381(3) . ? C11 O3 1.231(2) . ? C11 N2 1.384(2) . ? C12 O1 1.459(2) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C41 1.380(3) . ? C13 C42 1.390(3) . ? C13 H13 0.9500 . ? C14 C15 1.386(3) . ? C14 C19 1.402(3) . ? C14 P1 1.8447(18) . ? C15 C16 1.408(3) . ? C15 H15 0.9500 . ? C16 C17 1.373(5) . ? C16 H16 0.9500 . ? C17 C18 1.366(4) . ? C17 H17 0.9500 . ? C18 C19 1.389(3) . ? C18 H18 0.9500 . ? C19 H19 0.9500 . ? C20 C25 1.389(3) . ? C20 C21 1.390(3) . ? C20 H20 0.9500 . ? C21 C22 1.359(4) . ? C21 H21 0.9500 . ? C22 C23 1.375(4) . ? C22 H22 0.9500 . ? C23 C24 1.387(3) . ? C23 H23 0.9500 . ? C24 C25 1.387(3) . ? C24 H24 0.9500 . ? C25 P1 1.8492(19) . ? C26 C27 1.383(3) . ? C26 C31 1.399(3) . ? C26 P1 1.8381(19) . ? C27 C28 1.394(3) . ? C27 H27 0.9500 . ? C28 C29 1.389(4) . ? C28 H28 0.9500 . ? C29 C30 1.370(4) . ? C29 H29 0.9500 . ? C30 C31 1.386(3) . ? C30 H30 0.9500 . ? C31 H31 0.9500 . ? C32 C33 1.390(3) . ? C32 C37 1.391(3) . ? C32 P2 1.8325(19) . ? C33 C34 1.392(3) . ? C33 H33 0.9500 . ? C34 C35 1.369(4) . ? C34 H34 0.9500 . ? C35 C36 1.379(4) . ? C35 H35 0.9500 . ? C36 C37 1.390(3) . ? C36 H36 0.9500 . ? C37 H37 0.9500 . ? C38 C42 1.395(3) . ? C38 C39 1.396(3) . ? C38 P2 1.8364(18) . ? C39 C40 1.395(3) . ? C39 H39 0.9500 . ? C40 C41 1.375(4) . ? C40 H40 0.9500 . ? C41 H41 0.9500 . ? C42 H42 0.9500 . ? C43 C44 1.389(2) . ? C43 C47 1.395(2) . ? C43 P2 1.8311(18) . ? C44 C45 1.385(3) . ? C44 H44 0.9500 . ? C45 C46 1.384(3) . ? C45 H45 0.9500 . ? C46 C48 1.374(3) . ? C46 H46 0.9500 . ? C47 C48 1.390(3) . ? C47 H47 0.9500 . ? C48 H48 0.9500 . ? N1 H1A 0.8472 . ? N2 H2A 0.8617 . ? P1 Ru1 2.3220(4) . ? P2 Ru1 2.3444(4) . ? C49 F2 1.272(4) . ? C49 F1 1.303(4) . ? C49 F3 1.322(4) . ? C49 S1 1.741(5) . ? O4 S1 1.421(3) . ? O5 S1 1.481(2) . ? O6 S1 1.404(5) . ? C49A F2A 1.302(5) . ? C49A F3A 1.317(5) . ? C49A F1A 1.328(5) . ? C49A S1A 1.658(9) . ? O6A S1A 1.408(4) . ? C50 C51 1.3900 . ? C50 C55 1.3900 . ? C50 C56 1.470(7) . ? C51 C52 1.3900 . ? C51 H51 0.9500 . ? C52 C53 1.3900 . ? C52 H52 0.9500 . ? C53 C54 1.3900 . ? C53 H53 0.9500 . ? C54 C55 1.3900 . ? C54 H54 0.9500 . ? C55 H55 0.9500 . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? C50A C51A 1.3900 . ? C50A C55A 1.3900 . ? C50A H50A 0.9500 . ? C51A C52A 1.3900 . ? C51A C56A 1.514(9) . ? C52A C53A 1.3900 . ? C52A H52A 0.9500 . ? C53A C54A 1.3900 . ? C53A H53A 0.9500 . ? C54A C55A 1.3900 . ? C54A H54A 0.9500 . ? C55A H55A 0.9500 . ? C56A H56D 0.9800 . ? C56A H56E 0.9800 . ? C56A H56F 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C5 C1 C2 107.30(18) . . ? C5 C1 Ru1 71.33(11) . . ? C2 C1 Ru1 69.56(10) . . ? C5 C1 H1 126.3 . . ? C2 C1 H1 126.3 . . ? Ru1 C1 H1 126.3 . . ? C3 C2 C1 108.02(17) . . ? C3 C2 Ru1 72.31(11) . . ? C1 C2 Ru1 73.37(10) . . ? C3 C2 H2 125.8 . . ? C1 C2 H2 125.8 . . ? Ru1 C2 H2 125.8 . . ? C2 C3 C4 108.23(17) . . ? C2 C3 Ru1 70.96(10) . . ? C4 C3 Ru1 71.53(10) . . ? C2 C3 H3 125.8 . . ? C4 C3 H3 125.8 . . ? Ru1 C3 H3 125.8 . . ? C3 C4 C5 107.58(18) . . ? C3 C4 Ru1 71.85(10) . . ? C5 C4 Ru1 72.26(10) . . ? C3 C4 H4 126.1 . . ? C5 C4 H4 126.1 . . ? Ru1 C4 H4 126.1 . . ? C1 C5 C4 108.78(17) . . ? C1 C5 Ru1 72.76(10) . . ? C4 C5 Ru1 70.86(10) . . ? C1 C5 H5 125.5 . . ? C4 C5 H5 125.5 . . ? Ru1 C5 H5 125.5 . . ? O1 C6 C7 116.85(15) . . ? O1 C6 Ru1 120.55(12) . . ? C7 C6 Ru1 122.35(12) . . ? C8 C7 C6 120.88(15) . . ? C8 C7 H7A 107.1 . . ? C6 C7 H7A 107.1 . . ? C8 C7 H7B 107.1 . . ? C6 C7 H7B 107.1 . . ? H7A C7 H7B 106.8 . . ? C9 C8 C11 117.65(16) . . ? C9 C8 C7 122.58(17) . . ? C11 C8 C7 119.47(16) . . ? C8 C9 N1 122.99(18) . . ? C8 C9 H9 118.5 . . ? N1 C9 H9 118.5 . . ? O2 C10 N1 123.49(19) . . ? O2 C10 N2 123.09(19) . . ? N1 C10 N2 113.42(16) . . ? O3 C11 N2 119.92(17) . . ? O3 C11 C8 124.25(16) . . ? N2 C11 C8 115.83(16) . . ? O1 C12 H12A 109.5 . . ? O1 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? O1 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C41 C13 C42 119.7(2) . . ? C41 C13 H13 120.2 . . ? C42 C13 H13 120.2 . . ? C15 C14 C19 118.09(19) . . ? C15 C14 P1 123.01(17) . . ? C19 C14 P1 118.71(17) . . ? C14 C15 C16 120.1(3) . . ? C14 C15 H15 120.0 . . ? C16 C15 H15 120.0 . . ? C17 C16 C15 120.7(3) . . ? C17 C16 H16 119.6 . . ? C15 C16 H16 119.6 . . ? C18 C17 C16 119.6(2) . . ? C18 C17 H17 120.2 . . ? C16 C17 H17 120.2 . . ? C17 C18 C19 120.7(3) . . ? C17 C18 H18 119.7 . . ? C19 C18 H18 119.7 . . ? C18 C19 C14 120.8(3) . . ? C18 C19 H19 119.6 . . ? C14 C19 H19 119.6 . . ? C25 C20 C21 121.0(2) . . ? C25 C20 H20 119.5 . . ? C21 C20 H20 119.5 . . ? C22 C21 C20 121.1(2) . . ? C22 C21 H21 119.4 . . ? C20 C21 H21 119.4 . . ? C21 C22 C23 118.7(2) . . ? C21 C22 H22 120.6 . . ? C23 C22 H22 120.6 . . ? C22 C23 C24 120.8(2) . . ? C22 C23 H23 119.6 . . ? C24 C23 H23 119.6 . . ? C25 C24 C23 121.0(2) . . ? C25 C24 H24 119.5 . . ? C23 C24 H24 119.5 . . ? C24 C25 C20 117.26(18) . . ? C24 C25 P1 121.98(15) . . ? C20 C25 P1 120.24(16) . . ? C27 C26 C31 118.97(19) . . ? C27 C26 P1 121.08(14) . . ? C31 C26 P1 119.80(17) . . ? C26 C27 C28 120.7(2) . . ? C26 C27 H27 119.6 . . ? C28 C27 H27 119.6 . . ? C29 C28 C27 119.5(2) . . ? C29 C28 H28 120.3 . . ? C27 C28 H28 120.3 . . ? C30 C29 C28 120.2(2) . . ? C30 C29 H29 119.9 . . ? C28 C29 H29 119.9 . . ? C29 C30 C31 120.5(2) . . ? C29 C30 H30 119.7 . . ? C31 C30 H30 119.7 . . ? C30 C31 C26 120.1(2) . . ? C30 C31 H31 120.0 . . ? C26 C31 H31 120.0 . . ? C33 C32 C37 118.68(19) . . ? C33 C32 P2 123.07(16) . . ? C37 C32 P2 118.14(15) . . ? C32 C33 C34 120.2(2) . . ? C32 C33 H33 119.9 . . ? C34 C33 H33 119.9 . . ? C35 C34 C33 120.7(2) . . ? C35 C34 H34 119.6 . . ? C33 C34 H34 119.6 . . ? C34 C35 C36 119.7(2) . . ? C34 C35 H35 120.2 . . ? C36 C35 H35 120.2 . . ? C35 C36 C37 120.2(2) . . ? C35 C36 H36 119.9 . . ? C37 C36 H36 119.9 . . ? C36 C37 C32 120.5(2) . . ? C36 C37 H37 119.8 . . ? C32 C37 H37 119.8 . . ? C42 C38 C39 118.03(17) . . ? C42 C38 P2 119.65(14) . . ? C39 C38 P2 122.30(15) . . ? C40 C39 C38 120.2(2) . . ? C40 C39 H39 119.9 . . ? C38 C39 H39 119.9 . . ? C41 C40 C39 120.8(2) . . ? C41 C40 H40 119.6 . . ? C39 C40 H40 119.6 . . ? C40 C41 C13 119.88(19) . . ? C40 C41 H41 120.1 . . ? C13 C41 H41 120.1 . . ? C13 C42 C38 121.42(19) . . ? C13 C42 H42 119.3 . . ? C38 C42 H42 119.3 . . ? C44 C43 C47 118.72(17) . . ? C44 C43 P2 117.82(14) . . ? C47 C43 P2 123.25(14) . . ? C45 C44 C43 120.41(19) . . ? C45 C44 H44 119.8 . . ? C43 C44 H44 119.8 . . ? C46 C45 C44 120.6(2) . . ? C46 C45 H45 119.7 . . ? C44 C45 H45 119.7 . . ? C48 C46 C45 119.4(2) . . ? C48 C46 H46 120.3 . . ? C45 C46 H46 120.3 . . ? C48 C47 C43 120.26(18) . . ? C48 C47 H47 119.9 . . ? C43 C47 H47 119.9 . . ? C46 C48 C47 120.56(19) . . ? C46 C48 H48 119.7 . . ? C47 C48 H48 119.7 . . ? C9 N1 C10 123.10(17) . . ? C9 N1 H1A 119.6 . . ? C10 N1 H1A 116.5 . . ? C10 N2 C11 126.99(17) . . ? C10 N2 H2A 116.4 . . ? C11 N2 H2A 116.3 . . ? C6 O1 C12 125.20(16) . . ? C26 P1 C14 100.03(9) . . ? C26 P1 C25 99.33(9) . . ? C14 P1 C25 105.19(9) . . ? C26 P1 Ru1 115.34(6) . . ? C14 P1 Ru1 122.77(6) . . ? C25 P1 Ru1 111.15(6) . . ? C43 P2 C32 103.76(9) . . ? C43 P2 C38 102.81(8) . . ? C32 P2 C38 101.81(8) . . ? C43 P2 Ru1 116.74(6) . . ? C32 P2 Ru1 118.03(6) . . ? C38 P2 Ru1 111.63(6) . . ? C6 Ru1 C2 119.86(7) . . ? C6 Ru1 C4 105.34(7) . . ? C2 Ru1 C4 61.47(7) . . ? C6 Ru1 C3 95.85(7) . . ? C2 Ru1 C3 36.73(8) . . ? C4 Ru1 C3 36.62(7) . . ? C6 Ru1 C5 140.43(7) . . ? C2 Ru1 C5 61.11(7) . . ? C4 Ru1 C5 36.88(7) . . ? C3 Ru1 C5 60.99(7) . . ? C6 Ru1 C1 155.97(7) . . ? C2 Ru1 C1 37.07(7) . . ? C4 Ru1 C1 61.03(8) . . ? C3 Ru1 C1 61.12(7) . . ? C5 Ru1 C1 35.91(8) . . ? C6 Ru1 P1 90.91(5) . . ? C2 Ru1 P1 90.14(5) . . ? C4 Ru1 P1 151.46(6) . . ? C3 Ru1 P1 119.92(5) . . ? C5 Ru1 P1 128.01(6) . . ? C1 Ru1 P1 94.99(5) . . ? C6 Ru1 P2 88.33(5) . . ? C2 Ru1 P2 148.73(5) . . ? C4 Ru1 P2 100.26(5) . . ? C3 Ru1 P2 136.14(5) . . ? C5 Ru1 P2 88.81(5) . . ? C1 Ru1 P2 112.72(5) . . ? P1 Ru1 P2 103.585(16) . . ? F2 C49 F1 96.2(7) . . ? F2 C49 F3 109.3(5) . . ? F1 C49 F3 107.8(5) . . ? F2 C49 S1 113.6(5) . . ? F1 C49 S1 112.5(5) . . ? F3 C49 S1 115.6(4) . . ? O6 S1 O4 102.3(5) . . ? O6 S1 O5 125.6(4) . . ? O4 S1 O5 110.6(2) . . ? O6 S1 C49 102.1(4) . . ? O4 S1 C49 109.5(3) . . ? O5 S1 C49 105.96(17) . . ? F2A C49A F3A 93.6(9) . . ? F2A C49A F1A 103.2(7) . . ? F3A C49A F1A 113.9(10) . . ? F2A C49A S1A 122.0(7) . . ? F3A C49A S1A 110.0(7) . . ? F1A C49A S1A 112.9(7) . . ? O6A S1A C49A 106.0(5) . . ? C51 C50 C55 120.0 . . ? C51 C50 C56 119.5(6) . . ? C55 C50 C56 120.5(6) . . ? C50 C51 C52 120.0 . . ? C50 C51 H51 120.0 . . ? C52 C51 H51 120.0 . . ? C51 C52 C53 120.0 . . ? C51 C52 H52 120.0 . . ? C53 C52 H52 120.0 . . ? C52 C53 C54 120.0 . . ? C52 C53 H53 120.0 . . ? C54 C53 H53 120.0 . . ? C55 C54 C53 120.0 . . ? C55 C54 H54 120.0 . . ? C53 C54 H54 120.0 . . ? C54 C55 C50 120.0 . . ? C54 C55 H55 120.0 . . ? C50 C55 H55 120.0 . . ? C51A C50A C55A 120.0 . . ? C51A C50A H50A 120.0 . . ? C55A C50A H50A 120.0 . . ? C50A C51A C52A 120.0 . . ? C50A C51A C56A 122.5(7) . . ? C52A C51A C56A 117.5(7) . . ? C53A C52A C51A 120.0 . . ? C53A C52A H52A 120.0 . . ? C51A C52A H52A 120.0 . . ? C52A C53A C54A 120.0 . . ? C52A C53A H53A 120.0 . . ? C54A C53A H53A 120.0 . . ? C53A C54A C55A 120.0 . . ? C53A C54A H54A 120.0 . . ? C55A C54A H54A 120.0 . . ? C54A C55A C50A 120.0 . . ? C54A C55A H55A 120.0 . . ? C50A C55A H55A 120.0 . . ? 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 C5 C1 C2 C3 2.79(19) . . . . ? Ru1 C1 C2 C3 64.49(12) . . . . ? C5 C1 C2 Ru1 -61.71(12) . . . . ? C1 C2 C3 C4 -3.0(2) . . . . ? Ru1 C2 C3 C4 62.19(13) . . . . ? C1 C2 C3 Ru1 -65.19(12) . . . . ? C2 C3 C4 C5 2.1(2) . . . . ? Ru1 C3 C4 C5 63.88(12) . . . . ? C2 C3 C4 Ru1 -61.82(13) . . . . ? C2 C1 C5 C4 -1.5(2) . . . . ? Ru1 C1 C5 C4 -62.08(12) . . . . ? C2 C1 C5 Ru1 60.57(12) . . . . ? C3 C4 C5 C1 -0.3(2) . . . . ? Ru1 C4 C5 C1 63.30(12) . . . . ? C3 C4 C5 Ru1 -63.61(12) . . . . ? O1 C6 C7 C8 -52.6(2) . . . . ? Ru1 C6 C7 C8 133.10(15) . . . . ? C6 C7 C8 C9 122.0(2) . . . . ? C6 C7 C8 C11 -64.5(2) . . . . ? C11 C8 C9 N1 -0.4(3) . . . . ? C7 C8 C9 N1 173.20(18) . . . . ? C9 C8 C11 O3 -178.8(2) . . . . ? C7 C8 C11 O3 7.4(3) . . . . ? C9 C8 C11 N2 0.7(3) . . . . ? C7 C8 C11 N2 -173.06(17) . . . . ? C19 C14 C15 C16 1.1(3) . . . . ? P1 C14 C15 C16 176.10(17) . . . . ? C14 C15 C16 C17 -0.5(4) . . . . ? C15 C16 C17 C18 -0.2(4) . . . . ? C16 C17 C18 C19 0.2(4) . . . . ? C17 C18 C19 C14 0.4(3) . . . . ? C15 C14 C19 C18 -1.1(3) . . . . ? P1 C14 C19 C18 -176.28(15) . . . . ? C25 C20 C21 C22 1.3(5) . . . . ? C20 C21 C22 C23 -1.5(5) . . . . ? C21 C22 C23 C24 0.0(5) . . . . ? C22 C23 C24 C25 1.7(4) . . . . ? C23 C24 C25 C20 -1.7(4) . . . . ? C23 C24 C25 P1 -173.5(2) . . . . ? C21 C20 C25 C24 0.3(4) . . . . ? C21 C20 C25 P1 172.1(2) . . . . ? C31 C26 C27 C28 0.9(3) . . . . ? P1 C26 C27 C28 176.44(16) . . . . ? C26 C27 C28 C29 0.3(3) . . . . ? C27 C28 C29 C30 -0.7(3) . . . . ? C28 C29 C30 C31 0.0(4) . . . . ? C29 C30 C31 C26 1.2(3) . . . . ? C27 C26 C31 C30 -1.7(3) . . . . ? P1 C26 C31 C30 -177.24(17) . . . . ? C37 C32 C33 C34 -0.9(3) . . . . ? P2 C32 C33 C34 -176.9(2) . . . . ? C32 C33 C34 C35 0.3(4) . . . . ? C33 C34 C35 C36 0.9(5) . . . . ? C34 C35 C36 C37 -1.4(4) . . . . ? C35 C36 C37 C32 0.7(4) . . . . ? C33 C32 C37 C36 0.4(3) . . . . ? P2 C32 C37 C36 176.63(18) . . . . ? C42 C38 C39 C40 -1.6(3) . . . . ? P2 C38 C39 C40 176.84(17) . . . . ? C38 C39 C40 C41 1.3(3) . . . . ? C39 C40 C41 C13 0.1(3) . . . . ? C42 C13 C41 C40 -1.0(3) . . . . ? C41 C13 C42 C38 0.6(3) . . . . ? C39 C38 C42 C13 0.7(3) . . . . ? P2 C38 C42 C13 -177.82(15) . . . . ? C47 C43 C44 C45 1.5(3) . . . . ? P2 C43 C44 C45 -173.34(18) . . . . ? C43 C44 C45 C46 0.5(4) . . . . ? C44 C45 C46 C48 -1.9(4) . . . . ? C44 C43 C47 C48 -2.2(3) . . . . ? P2 C43 C47 C48 172.38(16) . . . . ? C45 C46 C48 C47 1.3(4) . . . . ? C43 C47 C48 C46 0.8(3) . . . . ? C8 C9 N1 C10 -0.9(3) . . . . ? O2 C10 N1 C9 -178.7(2) . . . . ? N2 C10 N1 C9 1.6(3) . . . . ? O2 C10 N2 C11 179.04(19) . . . . ? N1 C10 N2 C11 -1.3(3) . . . . ? O3 C11 N2 C10 179.69(19) . . . . ? C8 C11 N2 C10 0.1(3) . . . . ? C7 C6 O1 C12 -1.5(2) . . . . ? Ru1 C6 O1 C12 172.89(16) . . . . ? C27 C26 P1 C14 144.55(16) . . . . ? C31 C26 P1 C14 -39.98(17) . . . . ? C27 C26 P1 C25 -108.07(16) . . . . ? C31 C26 P1 C25 67.40(17) . . . . ? C27 C26 P1 Ru1 10.77(17) . . . . ? C31 C26 P1 Ru1 -173.76(13) . . . . ? C15 C14 P1 C26 147.55(17) . . . . ? C19 C14 P1 C26 -37.47(16) . . . . ? C15 C14 P1 C25 44.92(18) . . . . ? C19 C14 P1 C25 -140.09(15) . . . . ? C15 C14 P1 Ru1 -83.35(17) . . . . ? C19 C14 P1 Ru1 91.63(15) . . . . ? C24 C25 P1 C26 -169.33(18) . . . . ? C20 C25 P1 C26 19.2(2) . . . . ? C24 C25 P1 C14 -66.18(19) . . . . ? C20 C25 P1 C14 122.34(19) . . . . ? C24 C25 P1 Ru1 68.76(18) . . . . ? C20 C25 P1 Ru1 -102.72(18) . . . . ? C44 C43 P2 C32 -58.63(17) . . . . ? C47 C43 P2 C32 126.78(16) . . . . ? C44 C43 P2 C38 -164.39(15) . . . . ? C47 C43 P2 C38 21.02(17) . . . . ? C44 C43 P2 Ru1 73.07(16) . . . . ? C47 C43 P2 Ru1 -101.52(15) . . . . ? C33 C32 P2 C43 -13.77(19) . . . . ? C37 C32 P2 C43 170.21(16) . . . . ? C33 C32 P2 C38 92.75(19) . . . . ? C37 C32 P2 C38 -83.27(17) . . . . ? C33 C32 P2 Ru1 -144.70(16) . . . . ? C37 C32 P2 Ru1 39.27(18) . . . . ? C42 C38 P2 C43 -71.88(16) . . . . ? C39 C38 P2 C43 109.68(17) . . . . ? C42 C38 P2 C32 -179.15(16) . . . . ? C39 C38 P2 C32 2.42(19) . . . . ? C42 C38 P2 Ru1 54.03(16) . . . . ? C39 C38 P2 Ru1 -124.40(16) . . . . ? O1 C6 Ru1 C2 109.88(14) . . . . ? C7 C6 Ru1 C2 -76.07(15) . . . . ? O1 C6 Ru1 C4 175.45(13) . . . . ? C7 C6 Ru1 C4 -10.50(15) . . . . ? O1 C6 Ru1 C3 139.39(13) . . . . ? C7 C6 Ru1 C3 -46.56(14) . . . . ? O1 C6 Ru1 C5 -170.48(11) . . . . ? C7 C6 Ru1 C5 3.57(19) . . . . ? O1 C6 Ru1 C1 123.61(18) . . . . ? C7 C6 Ru1 C1 -62.3(2) . . . . ? O1 C6 Ru1 P1 19.19(13) . . . . ? C7 C6 Ru1 P1 -166.76(12) . . . . ? O1 C6 Ru1 P2 -84.37(13) . . . . ? C7 C6 Ru1 P2 89.68(13) . . . . ? C3 C2 Ru1 C6 55.04(13) . . . . ? C1 C2 Ru1 C6 170.77(11) . . . . ? C3 C2 Ru1 C4 -36.97(11) . . . . ? C1 C2 Ru1 C4 78.76(12) . . . . ? C1 C2 Ru1 C3 115.73(16) . . . . ? C3 C2 Ru1 C5 -79.25(12) . . . . ? C1 C2 Ru1 C5 36.48(11) . . . . ? C3 C2 Ru1 C1 -115.73(16) . . . . ? C3 C2 Ru1 P1 146.16(11) . . . . ? C1 C2 Ru1 P1 -98.10(11) . . . . ? C3 C2 Ru1 P2 -96.67(14) . . . . ? C1 C2 Ru1 P2 19.06(18) . . . . ? C3 C4 Ru1 C6 -78.94(13) . . . . ? C5 C4 Ru1 C6 165.05(11) . . . . ? C3 C4 Ru1 C2 37.07(12) . . . . ? C5 C4 Ru1 C2 -78.94(13) . . . . ? C5 C4 Ru1 C3 -116.01(18) . . . . ? C3 C4 Ru1 C5 116.01(18) . . . . ? C3 C4 Ru1 C1 79.59(13) . . . . ? C5 C4 Ru1 C1 -36.42(12) . . . . ? C3 C4 Ru1 P1 43.65(18) . . . . ? C5 C4 Ru1 P1 -72.37(16) . . . . ? C3 C4 Ru1 P2 -170.02(11) . . . . ? C5 C4 Ru1 P2 73.97(12) . . . . ? C2 C3 Ru1 C6 -134.41(11) . . . . ? C4 C3 Ru1 C6 107.93(13) . . . . ? C4 C3 Ru1 C2 -117.66(17) . . . . ? C2 C3 Ru1 C4 117.66(17) . . . . ? C2 C3 Ru1 C5 79.58(12) . . . . ? C4 C3 Ru1 C5 -38.08(12) . . . . ? C2 C3 Ru1 C1 38.33(11) . . . . ? C4 C3 Ru1 C1 -79.33(13) . . . . ? C2 C3 Ru1 P1 -39.97(12) . . . . ? C4 C3 Ru1 P1 -157.64(10) . . . . ? C2 C3 Ru1 P2 131.91(10) . . . . ? C4 C3 Ru1 P2 14.25(16) . . . . ? C1 C5 Ru1 C6 -140.67(12) . . . . ? C4 C5 Ru1 C6 -22.99(17) . . . . ? C1 C5 Ru1 C2 -37.66(11) . . . . ? C4 C5 Ru1 C2 80.01(13) . . . . ? C1 C5 Ru1 C4 -117.68(17) . . . . ? C1 C5 Ru1 C3 -79.87(13) . . . . ? C4 C5 Ru1 C3 37.81(12) . . . . ? C4 C5 Ru1 C1 117.68(17) . . . . ? C1 C5 Ru1 P1 27.02(13) . . . . ? C4 C5 Ru1 P1 144.69(10) . . . . ? C1 C5 Ru1 P2 133.40(11) . . . . ? C4 C5 Ru1 P2 -108.93(11) . . . . ? C5 C1 Ru1 C6 97.48(19) . . . . ? C2 C1 Ru1 C6 -20.0(2) . . . . ? C5 C1 Ru1 C2 117.45(17) . . . . ? C5 C1 Ru1 C4 37.41(11) . . . . ? C2 C1 Ru1 C4 -80.04(12) . . . . ? C5 C1 Ru1 C3 79.48(12) . . . . ? C2 C1 Ru1 C3 -37.97(11) . . . . ? C2 C1 Ru1 C5 -117.45(17) . . . . ? C5 C1 Ru1 P1 -158.94(11) . . . . ? C2 C1 Ru1 P1 83.61(11) . . . . ? C5 C1 Ru1 P2 -51.96(12) . . . . ? C2 C1 Ru1 P2 -169.41(10) . . . . ? C26 P1 Ru1 C6 49.32(8) . . . . ? C14 P1 Ru1 C6 -72.96(10) . . . . ? C25 P1 Ru1 C6 161.37(8) . . . . ? C26 P1 Ru1 C2 -70.55(8) . . . . ? C14 P1 Ru1 C2 167.17(10) . . . . ? C25 P1 Ru1 C2 41.50(9) . . . . ? C26 P1 Ru1 C4 -76.32(13) . . . . ? C14 P1 Ru1 C4 161.40(13) . . . . ? C25 P1 Ru1 C4 35.73(13) . . . . ? C26 P1 Ru1 C3 -47.96(9) . . . . ? C14 P1 Ru1 C3 -170.24(10) . . . . ? C25 P1 Ru1 C3 64.09(9) . . . . ? C26 P1 Ru1 C5 -122.87(9) . . . . ? C14 P1 Ru1 C5 114.85(10) . . . . ? C25 P1 Ru1 C5 -10.82(9) . . . . ? C26 P1 Ru1 C1 -107.36(8) . . . . ? C14 P1 Ru1 C1 130.37(10) . . . . ? C25 P1 Ru1 C1 4.70(8) . . . . ? C26 P1 Ru1 P2 137.81(6) . . . . ? C14 P1 Ru1 P2 15.54(9) . . . . ? C25 P1 Ru1 P2 -110.13(7) . . . . ? C43 P2 Ru1 C6 13.57(8) . . . . ? C32 P2 Ru1 C6 138.32(9) . . . . ? C38 P2 Ru1 C6 -104.26(8) . . . . ? C43 P2 Ru1 C2 169.29(12) . . . . ? C32 P2 Ru1 C2 -65.96(13) . . . . ? C38 P2 Ru1 C2 51.46(13) . . . . ? C43 P2 Ru1 C4 118.86(8) . . . . ? C32 P2 Ru1 C4 -116.39(9) . . . . ? C38 P2 Ru1 C4 1.03(9) . . . . ? C43 P2 Ru1 C3 110.28(10) . . . . ? C32 P2 Ru1 C3 -124.97(10) . . . . ? C38 P2 Ru1 C3 -7.56(10) . . . . ? C43 P2 Ru1 C5 154.09(8) . . . . ? C32 P2 Ru1 C5 -81.15(9) . . . . ? C38 P2 Ru1 C5 36.26(8) . . . . ? C43 P2 Ru1 C1 -178.39(8) . . . . ? C32 P2 Ru1 C1 -53.64(9) . . . . ? C38 P2 Ru1 C1 63.78(9) . . . . ? C43 P2 Ru1 P1 -76.96(7) . . . . ? C32 P2 Ru1 P1 47.79(7) . . . . ? C38 P2 Ru1 P1 165.21(7) . . . . ? F2 C49 S1 O6 -73.4(7) . . . . ? F1 C49 S1 O6 178.7(6) . . . . ? F3 C49 S1 O6 54.2(7) . . . . ? F2 C49 S1 O4 178.8(5) . . . . ? F1 C49 S1 O4 70.8(5) . . . . ? F3 C49 S1 O4 -53.7(5) . . . . ? F2 C49 S1 O5 59.5(5) . . . . ? F1 C49 S1 O5 -48.5(5) . . . . ? F3 C49 S1 O5 -173.0(4) . . . . ? F2A C49A S1A O6A 65.9(9) . . . . ? F3A C49A S1A O6A 173.7(7) . . . . ? F1A C49A S1A O6A -57.8(8) . . . . ? C55 C50 C51 C52 0.0 . . . . ? C56 C50 C51 C52 -179.2(5) . . . . ? C50 C51 C52 C53 0.0 . . . . ? C51 C52 C53 C54 0.0 . . . . ? C52 C53 C54 C55 0.0 . . . . ? C53 C54 C55 C50 0.0 . . . . ? C51 C50 C55 C54 0.0 . . . . ? C56 C50 C55 C54 179.2(6) . . . . ? C55A C50A C51A C52A 0.0 . . . . ? C55A C50A C51A C56A -178.9(6) . . . . ? C50A C51A C52A C53A 0.0 . . . . ? C56A C51A C52A C53A 178.9(6) . . . . ? C51A C52A C53A C54A 0.0 . . . . ? C52A C53A C54A C55A 0.0 . . . . ? C53A C54A C55A C50A 0.0 . . . . ? C51A C50A C55A C54A 0.0 . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N2 H2A O3 0.86 2.03 2.862(2) 163.3 2_676 N1 H1A O5A 0.85 3.46 3.762(3) 104.8 1_665 N1 H1A O4A 0.85 2.13 2.861(2) 144.4 1_665 _diffrn_measured_fraction_theta_max 0.977 _diffrn_reflns_theta_full 30.02 _diffrn_measured_fraction_theta_full 0.977 _refine_diff_density_max 1.083 _refine_diff_density_min -0.625 _refine_diff_density_rms 0.069 data_CCDC737834_compound6a[OTf] _database_code_depnum_ccdc_archive 'CCDC 737834' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C65 H54 N2 O2 P3 Ru, C F3 O3 S' _chemical_formula_sum 'C66 H54 F3 N2 O5 P3 Ru S' _chemical_formula_weight 1238.15 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' S S 0.1246 0.1234 '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)/n _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 13.375(2) _cell_length_b 18.319(3) _cell_length_c 23.489(4) _cell_angle_alpha 90.00 _cell_angle_beta 101.392(4) _cell_angle_gamma 90.00 _cell_volume 5641.5(16) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 1924 _cell_measurement_theta_min 2.22 _cell_measurement_theta_max 20.34 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.458 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2544 _exptl_absorpt_coefficient_mu 0.464 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.789 _exptl_absorpt_correction_T_max 0.986 _exptl_absorpt_process_details 'SADABS v2.03; (Sheldrick)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 31806 _diffrn_reflns_av_R_equivalents 0.1291 _diffrn_reflns_av_sigmaI/netI 0.1410 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.42 _diffrn_reflns_theta_max 25.09 _reflns_number_total 9957 _reflns_number_gt 5746 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0371P)^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 9957 _refine_ls_number_parameters 737 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1234 _refine_ls_R_factor_gt 0.0529 _refine_ls_wR_factor_ref 0.1175 _refine_ls_wR_factor_gt 0.0951 _refine_ls_goodness_of_fit_ref 0.952 _refine_ls_restrained_S_all 0.952 _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 C1 C 1.0175(4) 0.7848(3) 0.5178(2) 0.0256(13) Uani 1 1 d . . . H1 H 1.0317 0.7323 0.5107 0.031 Uiso 1 1 calc R . . C2 C 1.0548(4) 0.8239(3) 0.5693(2) 0.0258(12) Uani 1 1 d . . . H2 H 1.0998 0.8037 0.6049 0.031 Uiso 1 1 calc R . . C3 C 1.0248(4) 0.8983(3) 0.5604(2) 0.0251(13) Uani 1 1 d . . . H3 H 1.0445 0.9396 0.5881 0.030 Uiso 1 1 calc R . . C4 C 0.9683(4) 0.9030(3) 0.5033(2) 0.0230(13) Uani 1 1 d . . . H4 H 0.9397 0.9492 0.4838 0.028 Uiso 1 1 calc R . . C5 C 0.9622(4) 0.8336(3) 0.4765(2) 0.0222(12) Uani 1 1 d . . . H5 H 0.9314 0.8223 0.4351 0.027 Uiso 1 1 calc R . . C6 C 0.7892(4) 0.7379(2) 0.5346(2) 0.0184(12) Uani 1 1 d . . . H6 H 0.7342 0.7394 0.5548 0.022 Uiso 1 1 calc R . . C7 C 0.7868(4) 0.6765(3) 0.50056(19) 0.0190(11) Uani 1 1 d . . . C8 C 0.8579(4) 0.6558(2) 0.4630(2) 0.0180(12) Uani 1 1 d . . . C9 C 0.8627(4) 0.6892(3) 0.4118(2) 0.0244(13) Uani 1 1 d . . . H9 H 0.8155 0.7270 0.3980 0.029 Uiso 1 1 calc R . . C10 C 1.0009(5) 0.6134(3) 0.3933(2) 0.0332(15) Uani 1 1 d . . . C11 C 0.9284(4) 0.5961(3) 0.4804(2) 0.0200(12) Uani 1 1 d . . . C12 C 0.7101(4) 0.5236(3) 0.4729(2) 0.0217(12) Uani 1 1 d . . . C13 C 0.7267(5) 0.4642(3) 0.5102(2) 0.0313(14) Uani 1 1 d . . . H13 H 0.7218 0.4702 0.5497 0.038 Uiso 1 1 calc R . . C14 C 0.7504(5) 0.3966(3) 0.4906(2) 0.0334(15) Uani 1 1 d . . . H14 H 0.7605 0.3561 0.5164 0.040 Uiso 1 1 calc R . . C15 C 0.7593(5) 0.3879(3) 0.4342(3) 0.0374(16) Uani 1 1 d . . . H15 H 0.7768 0.3415 0.4211 0.045 Uiso 1 1 calc R . . C16 C 0.7435(5) 0.4454(3) 0.3962(2) 0.0346(15) Uani 1 1 d . . . H16 H 0.7504 0.4388 0.3570 0.041 Uiso 1 1 calc R . . C17 C 0.7171(4) 0.5137(3) 0.4154(2) 0.0281(14) Uani 1 1 d . . . H17 H 0.7040 0.5534 0.3889 0.034 Uiso 1 1 calc R . . C18 C 0.5734(4) 0.6450(3) 0.4468(2) 0.0206(12) Uani 1 1 d . . . C19 C 0.5694(5) 0.7170(3) 0.4266(2) 0.0287(14) Uani 1 1 d . . . H19 H 0.6235 0.7499 0.4407 0.034 Uiso 1 1 calc R . . C20 C 0.4853(5) 0.7400(3) 0.3858(2) 0.0366(16) Uani 1 1 d . . . H20 H 0.4823 0.7887 0.3717 0.044 Uiso 1 1 calc R . . C21 C 0.4068(5) 0.6927(3) 0.3656(2) 0.0333(15) Uani 1 1 d . . . H21 H 0.3494 0.7091 0.3381 0.040 Uiso 1 1 calc R . . C22 C 0.4103(5) 0.6218(3) 0.3850(2) 0.0356(15) Uani 1 1 d . . . H22 H 0.3559 0.5893 0.3706 0.043 Uiso 1 1 calc R . . C23 C 0.4938(5) 0.5977(3) 0.4258(2) 0.0330(15) Uani 1 1 d . . . H23 H 0.4962 0.5487 0.4393 0.040 Uiso 1 1 calc R . . C24 C 0.6534(4) 0.6012(2) 0.5686(2) 0.0211(12) Uani 1 1 d . . . C25 C 0.7333(5) 0.5806(2) 0.6139(2) 0.0254(13) Uani 1 1 d . . . H25 H 0.8010 0.5779 0.6072 0.030 Uiso 1 1 calc R . . C26 C 0.7142(5) 0.5644(3) 0.6677(2) 0.0325(15) Uani 1 1 d . . . H26 H 0.7684 0.5496 0.6981 0.039 Uiso 1 1 calc R . . C27 C 0.6161(5) 0.5697(3) 0.6778(2) 0.0341(16) Uani 1 1 d . . . H27 H 0.6031 0.5585 0.7152 0.041 Uiso 1 1 calc R . . C28 C 0.5363(5) 0.5911(3) 0.6337(2) 0.0299(14) Uani 1 1 d . . . H28 H 0.4691 0.5950 0.6410 0.036 Uiso 1 1 calc R . . C29 C 0.5552(4) 0.6067(3) 0.5792(2) 0.0253(13) Uani 1 1 d . . . H29 H 0.5008 0.6211 0.5489 0.030 Uiso 1 1 calc R . . C30 C 0.6134(4) 0.8737(3) 0.5272(2) 0.0207(12) Uani 1 1 d . . . C31 C 0.5921(4) 0.8256(3) 0.5696(2) 0.0233(12) Uani 1 1 d . . . H31 H 0.6449 0.8124 0.6012 0.028 Uiso 1 1 calc R . . C32 C 0.4955(5) 0.7972(3) 0.5662(2) 0.0331(15) Uani 1 1 d . . . H32 H 0.4826 0.7644 0.5953 0.040 Uiso 1 1 calc R . . C33 C 0.4180(4) 0.8159(3) 0.5210(2) 0.0332(14) Uani 1 1 d . . . H33 H 0.3517 0.7960 0.5185 0.040 Uiso 1 1 calc R . . C34 C 0.4372(5) 0.8642(3) 0.4790(2) 0.0323(14) Uani 1 1 d . . . H34 H 0.3839 0.8776 0.4477 0.039 Uiso 1 1 calc R . . C35 C 0.5331(4) 0.8928(3) 0.4825(2) 0.0272(14) Uani 1 1 d . . . H35 H 0.5449 0.9264 0.4537 0.033 Uiso 1 1 calc R . . C36 C 0.7305(4) 0.9472(2) 0.4599(2) 0.0192(12) Uani 1 1 d . . . C37 C 0.7332(4) 0.9023(3) 0.4122(2) 0.0258(13) Uani 1 1 d . . . H37 H 0.7463 0.8516 0.4181 0.031 Uiso 1 1 calc R . . C38 C 0.7171(5) 0.9304(3) 0.3566(2) 0.0318(15) Uani 1 1 d . . . H38 H 0.7177 0.8989 0.3246 0.038 Uiso 1 1 calc R . . C39 C 0.7001(5) 1.0044(3) 0.3474(2) 0.0360(15) Uani 1 1 d . . . H39 H 0.6915 1.0242 0.3094 0.043 Uiso 1 1 calc R . . C40 C 0.6957(5) 1.0487(3) 0.3939(2) 0.0382(17) Uani 1 1 d . . . H40 H 0.6821 1.0993 0.3876 0.046 Uiso 1 1 calc R . . C41 C 0.7107(5) 1.0211(3) 0.4495(2) 0.0318(15) Uani 1 1 d . . . H41 H 0.7075 1.0529 0.4811 0.038 Uiso 1 1 calc R . . C42 C 0.7519(4) 0.9847(3) 0.5797(2) 0.0240(13) Uani 1 1 d . . . C43 C 0.6877(5) 0.9935(3) 0.6194(2) 0.0290(14) Uani 1 1 d . . . H43 H 0.6342 0.9595 0.6199 0.035 Uiso 1 1 calc R . . C44 C 0.7014(5) 1.0515(3) 0.6582(2) 0.0388(17) Uani 1 1 d . . . H44 H 0.6584 1.0558 0.6858 0.047 Uiso 1 1 calc R . . C45 C 0.7755(6) 1.1025(3) 0.6575(2) 0.0441(18) Uani 1 1 d . . . H45 H 0.7830 1.1423 0.6839 0.053 Uiso 1 1 calc R . . C46 C 0.8404(5) 1.0959(3) 0.6176(2) 0.0360(15) Uani 1 1 d . . . H46 H 0.8919 1.1313 0.6164 0.043 Uiso 1 1 calc R . . C47 C 0.8284(5) 1.0370(3) 0.5800(2) 0.0292(14) Uani 1 1 d . . . H47 H 0.8734 1.0318 0.5536 0.035 Uiso 1 1 calc R . . C48 C 0.9937(4) 0.8651(3) 0.6953(2) 0.0211(12) Uani 1 1 d . . . C49 C 1.0781(4) 0.8395(3) 0.7340(2) 0.0290(14) Uani 1 1 d . . . H49 H 1.0881 0.7885 0.7397 0.035 Uiso 1 1 calc R . . C50 C 1.1475(5) 0.8880(3) 0.7641(2) 0.0354(15) Uani 1 1 d . . . H50 H 1.2051 0.8701 0.7908 0.042 Uiso 1 1 calc R . . C51 C 1.1345(5) 0.9626(3) 0.7562(2) 0.0323(14) Uani 1 1 d . . . H51 H 1.1835 0.9956 0.7768 0.039 Uiso 1 1 calc R . . C52 C 1.0499(4) 0.9887(3) 0.7181(2) 0.0285(14) Uani 1 1 d . . . H52 H 1.0398 1.0397 0.7128 0.034 Uiso 1 1 calc R . . C53 C 0.9807(4) 0.9406(3) 0.6880(2) 0.0237(13) Uani 1 1 d . . . H53 H 0.9229 0.9588 0.6617 0.028 Uiso 1 1 calc R . . C54 C 0.7928(4) 0.8124(2) 0.6922(2) 0.0177(12) Uani 1 1 d . . . C55 C 0.7749(4) 0.8749(3) 0.7226(2) 0.0241(13) Uani 1 1 d . . . H55 H 0.8178 0.9163 0.7229 0.029 Uiso 1 1 calc R . . C56 C 0.6961(4) 0.8772(3) 0.7522(2) 0.0266(13) Uani 1 1 d . . . H56 H 0.6858 0.9201 0.7730 0.032 Uiso 1 1 calc R . . C57 C 0.6317(4) 0.8187(3) 0.7524(2) 0.0282(13) Uani 1 1 d . . . H57 H 0.5767 0.8212 0.7725 0.034 Uiso 1 1 calc R . . C58 C 0.6484(4) 0.7559(3) 0.7227(2) 0.0246(13) Uani 1 1 d . . . H58 H 0.6055 0.7146 0.7229 0.029 Uiso 1 1 calc R . . C59 C 0.7273(4) 0.7535(3) 0.6928(2) 0.0216(12) Uani 1 1 d . . . H59 H 0.7373 0.7105 0.6720 0.026 Uiso 1 1 calc R . . C60 C 0.9456(4) 0.7141(3) 0.6756(2) 0.0193(12) Uani 1 1 d . . . C61 C 0.9522(4) 0.6919(3) 0.7328(2) 0.0277(14) Uani 1 1 d . . . H61 H 0.9286 0.7235 0.7594 0.033 Uiso 1 1 calc R . . C62 C 0.9928(4) 0.6243(3) 0.7518(2) 0.0317(14) Uani 1 1 d . . . H62 H 0.9987 0.6105 0.7913 0.038 Uiso 1 1 calc R . . C63 C 1.0244(4) 0.5771(3) 0.7130(2) 0.0340(15) Uani 1 1 d . . . H63 H 1.0507 0.5304 0.7256 0.041 Uiso 1 1 calc R . . C64 C 1.0177(4) 0.5980(3) 0.6558(2) 0.0313(14) Uani 1 1 d . . . H64 H 1.0395 0.5658 0.6290 0.038 Uiso 1 1 calc R . . C65 C 0.9787(4) 0.6667(3) 0.6376(2) 0.0232(12) Uani 1 1 d . . . H65 H 0.9749 0.6811 0.5983 0.028 Uiso 1 1 calc R . . N1 N 0.9333(4) 0.6700(3) 0.3797(2) 0.0329(13) Uani 1 1 d . . . N2 N 0.9918(4) 0.5782(2) 0.44391(19) 0.0257(12) Uani 1 1 d . . . H2A H 1.031(4) 0.543(3) 0.453(2) 0.031 Uiso 1 1 d . . . O1 O 1.0633(4) 0.5959(2) 0.36470(18) 0.0486(13) Uani 1 1 d . . . O2 O 0.9283(3) 0.56064(17) 0.52572(15) 0.0268(9) Uani 1 1 d . . . P1 P 0.74482(11) 0.90476(7) 0.53196(6) 0.0196(3) Uani 1 1 d . . . P2 P 0.89720(11) 0.80536(7) 0.65154(6) 0.0182(3) Uani 1 1 d . . . P3 P 0.68331(11) 0.61399(7) 0.49792(6) 0.0201(3) Uani 1 1 d . . . Ru1 Ru 0.88416(3) 0.82718(2) 0.552296(17) 0.01670(11) Uani 1 1 d . . . C66 C 0.3356(6) 0.7617(4) 0.7055(3) 0.0446(18) Uani 1 1 d . . . F1 F 0.3571(3) 0.8304(2) 0.72168(18) 0.0712(12) Uani 1 1 d . . . F2 F 0.3989(3) 0.7421(2) 0.67124(16) 0.0784(14) Uani 1 1 d . . . F3 F 0.2424(3) 0.7629(2) 0.67178(15) 0.0633(12) Uani 1 1 d . . . O3 O 0.4465(3) 0.7127(2) 0.79713(16) 0.0391(10) Uani 1 1 d . . . O4 O 0.2680(3) 0.72937(19) 0.79655(15) 0.0362(10) Uani 1 1 d . . . O5 O 0.3212(4) 0.63193(19) 0.73896(17) 0.0478(12) Uani 1 1 d . . . S1 S 0.34362(12) 0.70169(7) 0.76591(6) 0.0289(4) Uani 1 1 d . . . H1A H 0.915(6) 0.686(4) 0.346(3) 0.09(3) 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 C1 0.021(3) 0.026(3) 0.033(3) 0.000(3) 0.012(3) -0.001(3) C2 0.016(3) 0.035(3) 0.025(3) -0.001(3) 0.004(2) 0.002(3) C3 0.025(4) 0.020(3) 0.031(3) -0.006(2) 0.009(3) -0.008(3) C4 0.022(3) 0.018(3) 0.031(3) 0.001(2) 0.010(3) -0.003(2) C5 0.023(3) 0.026(3) 0.020(3) -0.005(2) 0.009(2) -0.007(3) C6 0.020(3) 0.018(3) 0.017(3) 0.003(2) 0.003(2) 0.003(2) C7 0.029(3) 0.015(3) 0.012(3) 0.001(2) 0.002(2) -0.001(3) C8 0.025(3) 0.010(3) 0.018(3) -0.005(2) 0.002(2) -0.004(2) C9 0.035(4) 0.018(3) 0.022(3) -0.005(2) 0.010(3) -0.001(2) C10 0.051(5) 0.021(3) 0.034(4) 0.003(3) 0.024(3) 0.007(3) C11 0.026(3) 0.014(3) 0.021(3) -0.010(2) 0.005(2) -0.002(2) C12 0.029(4) 0.016(3) 0.019(3) 0.000(2) 0.000(2) -0.002(2) C13 0.042(4) 0.024(3) 0.028(3) 0.000(3) 0.008(3) -0.002(3) C14 0.048(4) 0.020(3) 0.032(4) -0.001(3) 0.006(3) -0.002(3) C15 0.042(4) 0.021(3) 0.046(4) -0.009(3) 0.000(3) 0.006(3) C16 0.045(4) 0.032(4) 0.027(3) -0.007(3) 0.009(3) 0.005(3) C17 0.042(4) 0.018(3) 0.022(3) 0.000(2) 0.002(3) 0.001(3) C18 0.025(3) 0.020(3) 0.016(3) -0.001(2) 0.003(2) -0.004(2) C19 0.036(4) 0.017(3) 0.029(3) 0.002(2) -0.003(3) -0.005(3) C20 0.051(5) 0.024(3) 0.027(3) 0.004(3) -0.010(3) -0.003(3) C21 0.036(4) 0.033(4) 0.026(3) 0.004(3) -0.008(3) 0.002(3) C22 0.042(4) 0.027(3) 0.032(4) 0.001(3) -0.007(3) -0.009(3) C23 0.042(4) 0.022(3) 0.034(4) 0.008(3) 0.004(3) -0.005(3) C24 0.031(4) 0.012(3) 0.022(3) -0.006(2) 0.010(3) -0.009(2) C25 0.035(4) 0.017(3) 0.023(3) -0.004(2) 0.003(3) -0.005(3) C26 0.052(5) 0.022(3) 0.023(3) 0.002(2) 0.005(3) -0.006(3) C27 0.065(5) 0.021(3) 0.020(3) -0.008(2) 0.015(3) -0.018(3) C28 0.033(4) 0.027(3) 0.034(4) -0.009(3) 0.017(3) -0.008(3) C29 0.032(4) 0.017(3) 0.028(3) -0.003(2) 0.007(3) -0.006(3) C30 0.027(3) 0.020(3) 0.018(3) -0.001(2) 0.011(2) 0.003(2) C31 0.024(3) 0.024(3) 0.023(3) 0.003(2) 0.008(2) 0.012(3) C32 0.037(4) 0.030(3) 0.036(4) 0.007(3) 0.019(3) 0.000(3) C33 0.023(4) 0.036(4) 0.044(4) 0.006(3) 0.014(3) 0.001(3) C34 0.029(4) 0.037(3) 0.032(4) 0.006(3) 0.008(3) 0.006(3) C35 0.031(4) 0.026(3) 0.025(3) 0.007(2) 0.008(3) 0.006(3) C36 0.026(3) 0.012(3) 0.020(3) -0.003(2) 0.006(2) -0.001(2) C37 0.032(4) 0.021(3) 0.024(3) -0.004(2) 0.004(3) 0.007(3) C38 0.045(4) 0.034(3) 0.018(3) -0.006(3) 0.011(3) 0.009(3) C39 0.048(5) 0.041(4) 0.020(3) 0.000(3) 0.008(3) -0.001(3) C40 0.069(5) 0.020(3) 0.024(3) 0.008(3) 0.006(3) 0.001(3) C41 0.062(5) 0.018(3) 0.018(3) -0.003(2) 0.015(3) 0.003(3) C42 0.031(4) 0.018(3) 0.021(3) 0.005(2) 0.001(3) 0.007(3) C43 0.041(4) 0.023(3) 0.023(3) 0.000(2) 0.007(3) 0.006(3) C44 0.063(5) 0.030(4) 0.024(3) -0.003(3) 0.010(3) 0.018(3) C45 0.077(6) 0.024(3) 0.025(4) -0.010(3) -0.006(3) 0.019(4) C46 0.048(4) 0.017(3) 0.037(4) -0.006(3) -0.004(3) 0.004(3) C47 0.038(4) 0.022(3) 0.026(3) -0.002(2) 0.002(3) 0.006(3) C48 0.024(3) 0.023(3) 0.018(3) -0.004(2) 0.008(2) -0.005(2) C49 0.032(4) 0.029(3) 0.027(3) -0.004(2) 0.007(3) 0.004(3) C50 0.030(4) 0.037(4) 0.032(4) -0.008(3) -0.008(3) 0.002(3) C51 0.031(4) 0.032(3) 0.032(3) -0.008(3) 0.001(3) -0.009(3) C52 0.033(4) 0.026(3) 0.028(3) -0.003(3) 0.010(3) -0.005(3) C53 0.029(4) 0.021(3) 0.022(3) -0.004(2) 0.006(3) -0.001(3) C54 0.016(3) 0.021(3) 0.016(3) 0.000(2) 0.003(2) 0.004(2) C55 0.029(4) 0.022(3) 0.021(3) 0.002(2) 0.003(3) 0.004(3) C56 0.031(4) 0.022(3) 0.028(3) -0.007(2) 0.009(3) 0.005(3) C57 0.026(3) 0.032(3) 0.028(3) 0.000(3) 0.009(2) 0.005(3) C58 0.026(4) 0.022(3) 0.025(3) 0.007(2) 0.004(3) 0.001(3) C59 0.025(3) 0.021(3) 0.017(3) -0.001(2) 0.002(2) 0.001(3) C60 0.019(3) 0.019(3) 0.019(3) -0.001(2) 0.002(2) 0.000(2) C61 0.026(4) 0.033(3) 0.024(3) -0.001(2) 0.007(3) 0.003(3) C62 0.032(4) 0.033(3) 0.029(3) 0.009(3) 0.004(3) 0.003(3) C63 0.034(4) 0.026(3) 0.039(4) 0.007(3) -0.001(3) 0.011(3) C64 0.034(4) 0.021(3) 0.034(4) -0.007(3) -0.004(3) 0.005(3) C65 0.023(3) 0.023(3) 0.022(3) 0.001(2) -0.001(2) 0.000(3) N1 0.058(4) 0.023(3) 0.022(3) 0.008(2) 0.018(3) 0.009(3) N2 0.035(3) 0.019(3) 0.026(3) 0.005(2) 0.013(2) 0.009(2) O1 0.070(4) 0.043(3) 0.047(3) 0.011(2) 0.043(3) 0.022(2) O2 0.038(3) 0.022(2) 0.022(2) 0.0015(16) 0.0101(18) 0.0006(18) P1 0.0260(9) 0.0159(7) 0.0178(8) -0.0001(6) 0.0066(6) 0.0014(6) P2 0.0221(8) 0.0171(7) 0.0158(7) -0.0010(5) 0.0046(6) -0.0003(6) P3 0.0267(9) 0.0152(7) 0.0183(8) 0.0000(6) 0.0039(6) -0.0028(6) Ru1 0.0198(2) 0.0144(2) 0.0166(2) -0.00083(19) 0.00539(16) -0.0006(2) C66 0.045(5) 0.051(4) 0.042(4) 0.015(3) 0.022(4) 0.004(4) F1 0.081(3) 0.048(2) 0.087(3) 0.039(2) 0.021(2) -0.003(2) F2 0.068(3) 0.130(4) 0.047(3) 0.036(2) 0.035(2) 0.033(3) F3 0.053(3) 0.100(3) 0.034(2) 0.019(2) 0.001(2) 0.033(2) O3 0.041(3) 0.041(2) 0.032(2) -0.0024(19) 0.001(2) 0.008(2) O4 0.050(3) 0.033(2) 0.029(2) -0.0040(18) 0.015(2) 0.001(2) O5 0.069(4) 0.025(2) 0.048(3) -0.0126(19) 0.007(2) 0.008(2) S1 0.0373(10) 0.0225(7) 0.0256(8) 0.0010(6) 0.0027(7) 0.0011(7) _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 C30 C35 1.391(7) . ? C30 C31 1.399(6) . ? C30 P1 1.830(5) . ? C31 C32 1.381(7) . ? C31 H31 0.9500 . ? C32 C33 1.373(8) . ? C32 H32 0.9500 . ? C33 C34 1.387(7) . ? C33 H33 0.9500 . ? C34 C35 1.372(7) . ? C34 H34 0.9500 . ? C35 H35 0.9500 . ? C42 C43 1.397(7) . ? C42 C47 1.400(7) . ? C42 P1 1.835(5) . ? C43 C44 1.389(7) . ? C43 H43 0.9500 . ? C44 C45 1.364(8) . ? C44 H44 0.9500 . ? C45 C46 1.403(8) . ? C45 H45 0.9500 . ? C46 C47 1.383(7) . ? C46 H46 0.9500 . ? C47 H47 0.9500 . ? C36 C41 1.392(6) . ? C36 C37 1.396(6) . ? C36 P1 1.838(5) . ? C37 C38 1.381(7) . ? C37 H37 0.9500 . ? C38 C39 1.385(7) . ? C38 H38 0.9500 . ? C39 C40 1.371(7) . ? C39 H39 0.9500 . ? C40 C41 1.378(7) . ? C40 H40 0.9500 . ? C41 H41 0.9500 . ? C54 C59 1.390(7) . ? C54 C55 1.394(6) . ? C54 P2 1.846(5) . ? C59 C58 1.380(7) . ? C59 H59 0.9500 . ? C58 C57 1.386(7) . ? C58 H58 0.9500 . ? C57 C56 1.376(7) . ? C57 H57 0.9500 . ? C56 C55 1.373(7) . ? C56 H56 0.9500 . ? C55 H55 0.9500 . ? C48 C49 1.383(7) . ? C48 C53 1.401(6) . ? C48 P2 1.843(5) . ? C53 C52 1.368(7) . ? C53 H53 0.9500 . ? C52 C51 1.382(8) . ? C52 H52 0.9500 . ? C51 C50 1.385(7) . ? C51 H51 0.9500 . ? C50 C49 1.375(7) . ? C50 H50 0.9500 . ? C49 H49 0.9500 . ? C60 C65 1.379(6) . ? C60 C61 1.390(7) . ? C60 P2 1.841(5) . ? C61 C62 1.391(7) . ? C61 H61 0.9500 . ? C62 C63 1.381(7) . ? C62 H62 0.9500 . ? C63 C64 1.382(7) . ? C63 H63 0.9500 . ? C64 C65 1.397(7) . ? C64 H64 0.9500 . ? C65 H65 0.9500 . ? C18 C23 1.386(7) . ? C18 C19 1.398(7) . ? C18 P3 1.797(5) . ? C19 C20 1.392(8) . ? C19 H19 0.9500 . ? C20 C21 1.371(8) . ? C20 H20 0.9500 . ? C21 C22 1.374(7) . ? C21 H21 0.9500 . ? C22 C23 1.392(8) . ? C22 H22 0.9500 . ? C23 H23 0.9500 . ? C24 C29 1.387(7) . ? C24 C25 1.402(7) . ? C24 P3 1.798(5) . ? C29 C28 1.383(7) . ? C29 H29 0.9500 . ? C28 C27 1.389(8) . ? C28 H28 0.9500 . ? C27 C26 1.382(8) . ? C27 H27 0.9500 . ? C26 C25 1.371(7) . ? C26 H26 0.9500 . ? C25 H25 0.9500 . ? C12 C17 1.385(6) . ? C12 C13 1.386(7) . ? C12 P3 1.816(5) . ? C13 C14 1.380(7) . ? C13 H13 0.9500 . ? C14 C15 1.362(7) . ? C14 H14 0.9500 . ? C15 C16 1.369(7) . ? C15 H15 0.9500 . ? C16 C17 1.399(7) . ? C16 H16 0.9500 . ? C17 H17 0.9500 . ? C5 C4 1.414(6) . ? C5 C1 1.415(7) . ? C5 Ru1 2.238(5) . ? C5 H5 1.0000 . ? C4 C3 1.406(7) . ? C4 Ru1 2.243(5) . ? C4 H4 1.0000 . ? C3 C2 1.424(7) . ? C3 Ru1 2.265(5) . ? C3 H3 1.0000 . ? C2 C1 1.410(7) . ? C2 Ru1 2.238(5) . ? C2 H2 1.0000 . ? C1 Ru1 2.239(5) . ? C1 H1 1.0000 . ? C6 C7 1.377(6) . ? C6 Ru1 2.063(5) . ? C6 H6 0.9500 . ? C7 C8 1.468(6) . ? C7 P3 1.788(5) . ? C8 C9 1.362(6) . ? C8 C11 1.450(7) . ? C9 N1 1.367(7) . ? C9 H9 0.9500 . ? C10 O1 1.213(6) . ? C10 N1 1.371(7) . ? C10 N2 1.379(6) . ? C11 O2 1.246(5) . ? C11 N2 1.361(6) . ? N1 H1A 0.83(7) . ? N2 H2A 0.83(5) . ? P1 Ru1 2.3172(15) . ? P2 Ru1 2.3375(14) . ? C66 F2 1.329(7) . ? C66 F1 1.329(7) . ? C66 F3 1.339(8) . ? C66 S1 1.781(6) . ? O3 S1 1.440(4) . ? O4 S1 1.444(4) . ? O5 S1 1.431(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C35 C30 C31 117.4(5) . . ? C35 C30 P1 123.8(4) . . ? C31 C30 P1 118.7(4) . . ? C32 C31 C30 121.1(5) . . ? C32 C31 H31 119.5 . . ? C30 C31 H31 119.5 . . ? C33 C32 C31 120.3(5) . . ? C33 C32 H32 119.9 . . ? C31 C32 H32 119.9 . . ? C32 C33 C34 119.5(6) . . ? C32 C33 H33 120.2 . . ? C34 C33 H33 120.2 . . ? C35 C34 C33 120.2(6) . . ? C35 C34 H34 119.9 . . ? C33 C34 H34 119.9 . . ? C34 C35 C30 121.5(5) . . ? C34 C35 H35 119.3 . . ? C30 C35 H35 119.3 . . ? C43 C42 C47 117.5(5) . . ? C43 C42 P1 122.4(4) . . ? C47 C42 P1 119.9(4) . . ? C44 C43 C42 120.5(6) . . ? C44 C43 H43 119.7 . . ? C42 C43 H43 119.7 . . ? C45 C44 C43 121.2(6) . . ? C45 C44 H44 119.4 . . ? C43 C44 H44 119.4 . . ? C44 C45 C46 119.8(5) . . ? C44 C45 H45 120.1 . . ? C46 C45 H45 120.1 . . ? C47 C46 C45 118.9(6) . . ? C47 C46 H46 120.5 . . ? C45 C46 H46 120.5 . . ? C46 C47 C42 122.0(5) . . ? C46 C47 H47 119.0 . . ? C42 C47 H47 119.0 . . ? C41 C36 C37 117.9(5) . . ? C41 C36 P1 123.7(4) . . ? C37 C36 P1 118.4(4) . . ? C38 C37 C36 121.0(5) . . ? C38 C37 H37 119.5 . . ? C36 C37 H37 119.5 . . ? C37 C38 C39 120.2(5) . . ? C37 C38 H38 119.9 . . ? C39 C38 H38 119.9 . . ? C40 C39 C38 119.1(5) . . ? C40 C39 H39 120.4 . . ? C38 C39 H39 120.4 . . ? C39 C40 C41 121.1(5) . . ? C39 C40 H40 119.4 . . ? C41 C40 H40 119.4 . . ? C40 C41 C36 120.6(5) . . ? C40 C41 H41 119.7 . . ? C36 C41 H41 119.7 . . ? C59 C54 C55 117.4(5) . . ? C59 C54 P2 119.5(4) . . ? C55 C54 P2 123.1(4) . . ? C58 C59 C54 121.8(5) . . ? C58 C59 H59 119.1 . . ? C54 C59 H59 119.1 . . ? C59 C58 C57 119.8(5) . . ? C59 C58 H58 120.1 . . ? C57 C58 H58 120.1 . . ? C56 C57 C58 118.8(5) . . ? C56 C57 H57 120.6 . . ? C58 C57 H57 120.6 . . ? C55 C56 C57 121.4(5) . . ? C55 C56 H56 119.3 . . ? C57 C56 H56 119.3 . . ? C56 C55 C54 120.7(5) . . ? C56 C55 H55 119.6 . . ? C54 C55 H55 119.6 . . ? C49 C48 C53 118.7(5) . . ? C49 C48 P2 123.8(4) . . ? C53 C48 P2 117.5(4) . . ? C52 C53 C48 121.1(5) . . ? C52 C53 H53 119.4 . . ? C48 C53 H53 119.4 . . ? C53 C52 C51 119.7(5) . . ? C53 C52 H52 120.1 . . ? C51 C52 H52 120.1 . . ? C52 C51 C50 119.5(5) . . ? C52 C51 H51 120.3 . . ? C50 C51 H51 120.3 . . ? C49 C50 C51 120.9(6) . . ? C49 C50 H50 119.5 . . ? C51 C50 H50 119.5 . . ? C50 C49 C48 120.0(5) . . ? C50 C49 H49 120.0 . . ? C48 C49 H49 120.0 . . ? C65 C60 C61 118.4(5) . . ? C65 C60 P2 120.7(4) . . ? C61 C60 P2 120.9(4) . . ? C60 C61 C62 121.0(5) . . ? C60 C61 H61 119.5 . . ? C62 C61 H61 119.5 . . ? C63 C62 C61 119.8(5) . . ? C63 C62 H62 120.1 . . ? C61 C62 H62 120.1 . . ? C62 C63 C64 119.9(5) . . ? C62 C63 H63 120.0 . . ? C64 C63 H63 120.0 . . ? C63 C64 C65 119.7(5) . . ? C63 C64 H64 120.1 . . ? C65 C64 H64 120.1 . . ? C60 C65 C64 121.1(5) . . ? C60 C65 H65 119.5 . . ? C64 C65 H65 119.5 . . ? C23 C18 C19 119.6(5) . . ? C23 C18 P3 120.6(4) . . ? C19 C18 P3 119.8(4) . . ? C20 C19 C18 119.5(5) . . ? C20 C19 H19 120.3 . . ? C18 C19 H19 120.3 . . ? C21 C20 C19 120.4(5) . . ? C21 C20 H20 119.8 . . ? C19 C20 H20 119.8 . . ? C20 C21 C22 120.6(6) . . ? C20 C21 H21 119.7 . . ? C22 C21 H21 119.7 . . ? C21 C22 C23 119.9(6) . . ? C21 C22 H22 120.0 . . ? C23 C22 H22 120.0 . . ? C18 C23 C22 120.1(5) . . ? C18 C23 H23 119.9 . . ? C22 C23 H23 119.9 . . ? C29 C24 C25 119.3(5) . . ? C29 C24 P3 123.2(4) . . ? C25 C24 P3 117.4(4) . . ? C28 C29 C24 120.3(5) . . ? C28 C29 H29 119.8 . . ? C24 C29 H29 119.8 . . ? C29 C28 C27 119.6(5) . . ? C29 C28 H28 120.2 . . ? C27 C28 H28 120.2 . . ? C26 C27 C28 120.5(5) . . ? C26 C27 H27 119.7 . . ? C28 C27 H27 119.7 . . ? C25 C26 C27 119.9(6) . . ? C25 C26 H26 120.0 . . ? C27 C26 H26 120.0 . . ? C26 C25 C24 120.3(5) . . ? C26 C25 H25 119.8 . . ? C24 C25 H25 119.8 . . ? C17 C12 C13 118.7(5) . . ? C17 C12 P3 119.4(4) . . ? C13 C12 P3 121.9(4) . . ? C14 C13 C12 120.9(5) . . ? C14 C13 H13 119.6 . . ? C12 C13 H13 119.6 . . ? C15 C14 C13 119.9(5) . . ? C15 C14 H14 120.1 . . ? C13 C14 H14 120.1 . . ? C14 C15 C16 120.8(5) . . ? C14 C15 H15 119.6 . . ? C16 C15 H15 119.6 . . ? C15 C16 C17 119.6(5) . . ? C15 C16 H16 120.2 . . ? C17 C16 H16 120.2 . . ? C12 C17 C16 120.1(5) . . ? C12 C17 H17 119.9 . . ? C16 C17 H17 119.9 . . ? C4 C5 C1 106.7(5) . . ? C4 C5 Ru1 71.8(3) . . ? C1 C5 Ru1 71.6(3) . . ? C4 C5 H5 126.5 . . ? C1 C5 H5 126.5 . . ? Ru1 C5 H5 126.5 . . ? C3 C4 C5 109.9(5) . . ? C3 C4 Ru1 72.6(3) . . ? C5 C4 Ru1 71.4(3) . . ? C3 C4 H4 125.0 . . ? C5 C4 H4 125.0 . . ? Ru1 C4 H4 125.0 . . ? C4 C3 C2 106.4(4) . . ? C4 C3 Ru1 71.0(3) . . ? C2 C3 Ru1 70.6(3) . . ? C4 C3 H3 126.7 . . ? C2 C3 H3 126.7 . . ? Ru1 C3 H3 126.7 . . ? C1 C2 C3 108.5(5) . . ? C1 C2 Ru1 71.6(3) . . ? C3 C2 Ru1 72.6(3) . . ? C1 C2 H2 125.7 . . ? C3 C2 H2 125.7 . . ? Ru1 C2 H2 125.7 . . ? C2 C1 C5 108.4(5) . . ? C2 C1 Ru1 71.6(3) . . ? C5 C1 Ru1 71.6(3) . . ? C2 C1 H1 125.7 . . ? C5 C1 H1 125.7 . . ? Ru1 C1 H1 125.7 . . ? C7 C6 Ru1 135.0(4) . . ? C7 C6 H6 112.5 . . ? Ru1 C6 H6 112.5 . . ? C6 C7 C8 128.1(5) . . ? C6 C7 P3 118.2(4) . . ? C8 C7 P3 113.7(3) . . ? C9 C8 C11 116.5(5) . . ? C9 C8 C7 124.3(5) . . ? C11 C8 C7 119.2(4) . . ? C8 C9 N1 122.0(5) . . ? C8 C9 H9 119.0 . . ? N1 C9 H9 119.0 . . ? O1 C10 N1 124.4(5) . . ? O1 C10 N2 122.7(5) . . ? N1 C10 N2 112.8(5) . . ? O2 C11 N2 121.2(5) . . ? O2 C11 C8 121.6(4) . . ? N2 C11 C8 117.1(5) . . ? C9 N1 C10 124.2(5) . . ? C9 N1 H1A 109(5) . . ? C10 N1 H1A 123(5) . . ? C11 N2 C10 127.1(5) . . ? C11 N2 H2A 117(4) . . ? C10 N2 H2A 116(4) . . ? C30 P1 C42 102.6(2) . . ? C30 P1 C36 98.7(2) . . ? C42 P1 C36 102.0(2) . . ? C30 P1 Ru1 123.05(16) . . ? C42 P1 Ru1 114.90(18) . . ? C36 P1 Ru1 112.48(17) . . ? C60 P2 C48 101.7(2) . . ? C60 P2 C54 99.3(2) . . ? C48 P2 C54 100.8(2) . . ? C60 P2 Ru1 114.44(16) . . ? C48 P2 Ru1 111.18(16) . . ? C54 P2 Ru1 126.09(17) . . ? C7 P3 C18 110.2(2) . . ? C7 P3 C24 111.3(2) . . ? C18 P3 C24 110.9(2) . . ? C7 P3 C12 113.2(2) . . ? C18 P3 C12 105.1(2) . . ? C24 P3 C12 105.9(2) . . ? C6 Ru1 C5 104.32(18) . . ? C6 Ru1 C2 125.45(19) . . ? C5 Ru1 C2 61.58(19) . . ? C6 Ru1 C1 98.92(19) . . ? C5 Ru1 C1 36.85(18) . . ? C2 Ru1 C1 36.72(18) . . ? C6 Ru1 C4 137.68(18) . . ? C5 Ru1 C4 36.79(17) . . ? C2 Ru1 C4 60.8(2) . . ? C1 Ru1 C4 60.84(19) . . ? C6 Ru1 C3 160.25(19) . . ? C5 Ru1 C3 61.71(18) . . ? C2 Ru1 C3 36.86(18) . . ? C1 Ru1 C3 61.43(19) . . ? C4 Ru1 C3 36.34(18) . . ? C6 Ru1 P1 90.40(15) . . ? C5 Ru1 P1 106.63(14) . . ? C2 Ru1 P1 143.45(14) . . ? C1 Ru1 P1 143.48(14) . . ? C4 Ru1 P1 88.77(14) . . ? C3 Ru1 P1 106.59(14) . . ? C6 Ru1 P2 89.23(13) . . ? C5 Ru1 P2 147.98(14) . . ? C2 Ru1 P2 86.83(13) . . ? C1 Ru1 P2 113.22(15) . . ? C4 Ru1 P2 132.18(14) . . ? C3 Ru1 P2 96.76(14) . . ? P1 Ru1 P2 102.06(5) . . ? F2 C66 F1 107.5(5) . . ? F2 C66 F3 106.0(5) . . ? F1 C66 F3 106.1(5) . . ? F2 C66 S1 111.7(5) . . ? F1 C66 S1 112.4(5) . . ? F3 C66 S1 112.6(5) . . ? O5 S1 O3 116.5(2) . . ? O5 S1 O4 115.3(3) . . ? O3 S1 O4 112.9(2) . . ? O5 S1 C66 103.0(3) . . ? O3 S1 C66 102.7(3) . . ? O4 S1 C66 104.0(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C35 C30 C31 C32 1.4(7) . . . . ? P1 C30 C31 C32 -176.2(4) . . . . ? C30 C31 C32 C33 -0.3(8) . . . . ? C31 C32 C33 C34 -0.6(8) . . . . ? C32 C33 C34 C35 0.3(8) . . . . ? C33 C34 C35 C30 0.9(8) . . . . ? C31 C30 C35 C34 -1.7(7) . . . . ? P1 C30 C35 C34 175.7(4) . . . . ? C47 C42 C43 C44 -1.1(8) . . . . ? P1 C42 C43 C44 174.4(4) . . . . ? C42 C43 C44 C45 2.0(9) . . . . ? C43 C44 C45 C46 -1.1(9) . . . . ? C44 C45 C46 C47 -0.6(9) . . . . ? C45 C46 C47 C42 1.5(8) . . . . ? C43 C42 C47 C46 -0.6(8) . . . . ? P1 C42 C47 C46 -176.2(4) . . . . ? C41 C36 C37 C38 0.2(8) . . . . ? P1 C36 C37 C38 176.3(4) . . . . ? C36 C37 C38 C39 1.4(9) . . . . ? C37 C38 C39 C40 -2.4(9) . . . . ? C38 C39 C40 C41 1.8(10) . . . . ? C39 C40 C41 C36 -0.2(10) . . . . ? C37 C36 C41 C40 -0.8(9) . . . . ? P1 C36 C41 C40 -176.6(5) . . . . ? C55 C54 C59 C58 -0.8(8) . . . . ? P2 C54 C59 C58 179.7(4) . . . . ? C54 C59 C58 C57 1.1(8) . . . . ? C59 C58 C57 C56 -1.2(8) . . . . ? C58 C57 C56 C55 1.0(8) . . . . ? C57 C56 C55 C54 -0.7(8) . . . . ? C59 C54 C55 C56 0.5(8) . . . . ? P2 C54 C55 C56 -180.0(4) . . . . ? C49 C48 C53 C52 0.3(7) . . . . ? P2 C48 C53 C52 -178.8(4) . . . . ? C48 C53 C52 C51 0.4(8) . . . . ? C53 C52 C51 C50 -1.0(8) . . . . ? C52 C51 C50 C49 0.9(8) . . . . ? C51 C50 C49 C48 -0.3(8) . . . . ? C53 C48 C49 C50 -0.3(8) . . . . ? P2 C48 C49 C50 178.7(4) . . . . ? C65 C60 C61 C62 1.1(8) . . . . ? P2 C60 C61 C62 -177.2(4) . . . . ? C60 C61 C62 C63 -2.0(8) . . . . ? C61 C62 C63 C64 1.4(9) . . . . ? C62 C63 C64 C65 -0.1(9) . . . . ? C61 C60 C65 C64 0.2(8) . . . . ? P2 C60 C65 C64 178.5(4) . . . . ? C63 C64 C65 C60 -0.7(8) . . . . ? C23 C18 C19 C20 0.0(8) . . . . ? P3 C18 C19 C20 178.1(4) . . . . ? C18 C19 C20 C21 0.4(9) . . . . ? C19 C20 C21 C22 -0.7(9) . . . . ? C20 C21 C22 C23 0.6(9) . . . . ? C19 C18 C23 C22 -0.1(8) . . . . ? P3 C18 C23 C22 -178.2(4) . . . . ? C21 C22 C23 C18 -0.2(9) . . . . ? C25 C24 C29 C28 -0.8(7) . . . . ? P3 C24 C29 C28 175.4(4) . . . . ? C24 C29 C28 C27 -0.3(7) . . . . ? C29 C28 C27 C26 0.6(8) . . . . ? C28 C27 C26 C25 0.2(8) . . . . ? C27 C26 C25 C24 -1.2(7) . . . . ? C29 C24 C25 C26 1.5(7) . . . . ? P3 C24 C25 C26 -174.8(4) . . . . ? C17 C12 C13 C14 0.3(9) . . . . ? P3 C12 C13 C14 -177.8(5) . . . . ? C12 C13 C14 C15 1.1(9) . . . . ? C13 C14 C15 C16 -1.1(9) . . . . ? C14 C15 C16 C17 -0.4(9) . . . . ? C13 C12 C17 C16 -1.8(8) . . . . ? P3 C12 C17 C16 176.3(5) . . . . ? C15 C16 C17 C12 1.9(9) . . . . ? C1 C5 C4 C3 -0.7(6) . . . . ? Ru1 C5 C4 C3 62.8(4) . . . . ? C1 C5 C4 Ru1 -63.6(3) . . . . ? C5 C4 C3 C2 0.0(6) . . . . ? Ru1 C4 C3 C2 62.1(3) . . . . ? C5 C4 C3 Ru1 -62.0(4) . . . . ? C4 C3 C2 C1 0.7(6) . . . . ? Ru1 C3 C2 C1 63.1(4) . . . . ? C4 C3 C2 Ru1 -62.4(4) . . . . ? C3 C2 C1 C5 -1.2(6) . . . . ? Ru1 C2 C1 C5 62.5(4) . . . . ? C3 C2 C1 Ru1 -63.6(4) . . . . ? C4 C5 C1 C2 1.2(6) . . . . ? Ru1 C5 C1 C2 -62.5(4) . . . . ? C4 C5 C1 Ru1 63.7(3) . . . . ? Ru1 C6 C7 C8 -0.7(8) . . . . ? Ru1 C6 C7 P3 -178.1(3) . . . . ? C6 C7 C8 C9 -72.0(7) . . . . ? P3 C7 C8 C9 105.5(5) . . . . ? C6 C7 C8 C11 108.0(6) . . . . ? P3 C7 C8 C11 -74.5(5) . . . . ? C11 C8 C9 N1 -3.0(7) . . . . ? C7 C8 C9 N1 177.0(5) . . . . ? C9 C8 C11 O2 -178.1(5) . . . . ? C7 C8 C11 O2 1.9(7) . . . . ? C9 C8 C11 N2 -0.8(7) . . . . ? C7 C8 C11 N2 179.2(4) . . . . ? C8 C9 N1 C10 4.3(9) . . . . ? O1 C10 N1 C9 179.5(6) . . . . ? N2 C10 N1 C9 -1.3(8) . . . . ? O2 C11 N2 C10 -178.7(5) . . . . ? C8 C11 N2 C10 4.0(8) . . . . ? O1 C10 N2 C11 176.3(6) . . . . ? N1 C10 N2 C11 -2.9(8) . . . . ? C35 C30 P1 C42 95.6(4) . . . . ? C31 C30 P1 C42 -87.0(4) . . . . ? C35 C30 P1 C36 -9.0(5) . . . . ? C31 C30 P1 C36 168.5(4) . . . . ? C35 C30 P1 Ru1 -133.1(4) . . . . ? C31 C30 P1 Ru1 44.3(4) . . . . ? C43 C42 P1 C30 24.4(5) . . . . ? C47 C42 P1 C30 -160.2(4) . . . . ? C43 C42 P1 C36 126.3(5) . . . . ? C47 C42 P1 C36 -58.3(5) . . . . ? C43 C42 P1 Ru1 -111.7(4) . . . . ? C47 C42 P1 Ru1 63.7(4) . . . . ? C41 C36 P1 C30 94.2(5) . . . . ? C37 C36 P1 C30 -81.6(5) . . . . ? C41 C36 P1 C42 -10.8(5) . . . . ? C37 C36 P1 C42 173.4(4) . . . . ? C41 C36 P1 Ru1 -134.4(5) . . . . ? C37 C36 P1 Ru1 49.8(5) . . . . ? C65 C60 P2 C48 -114.7(4) . . . . ? C61 C60 P2 C48 63.6(5) . . . . ? C65 C60 P2 C54 142.1(4) . . . . ? C61 C60 P2 C54 -39.6(5) . . . . ? C65 C60 P2 Ru1 5.2(5) . . . . ? C61 C60 P2 Ru1 -176.5(4) . . . . ? C49 C48 P2 C60 1.0(5) . . . . ? C53 C48 P2 C60 -180.0(4) . . . . ? C49 C48 P2 C54 102.9(5) . . . . ? C53 C48 P2 C54 -78.1(4) . . . . ? C49 C48 P2 Ru1 -121.3(4) . . . . ? C53 C48 P2 Ru1 57.8(4) . . . . ? C59 C54 P2 C60 -45.4(4) . . . . ? C55 C54 P2 C60 135.1(4) . . . . ? C59 C54 P2 C48 -149.3(4) . . . . ? C55 C54 P2 C48 31.2(5) . . . . ? C59 C54 P2 Ru1 84.2(4) . . . . ? C55 C54 P2 Ru1 -95.3(4) . . . . ? C6 C7 P3 C18 82.3(4) . . . . ? C8 C7 P3 C18 -95.5(4) . . . . ? C6 C7 P3 C24 -41.2(5) . . . . ? C8 C7 P3 C24 141.0(4) . . . . ? C6 C7 P3 C12 -160.3(4) . . . . ? C8 C7 P3 C12 21.9(4) . . . . ? C23 C18 P3 C7 162.9(4) . . . . ? C19 C18 P3 C7 -15.2(5) . . . . ? C23 C18 P3 C24 -73.4(5) . . . . ? C19 C18 P3 C24 108.5(4) . . . . ? C23 C18 P3 C12 40.6(5) . . . . ? C19 C18 P3 C12 -137.5(4) . . . . ? C29 C24 P3 C7 130.1(4) . . . . ? C25 C24 P3 C7 -53.7(4) . . . . ? C29 C24 P3 C18 7.0(5) . . . . ? C25 C24 P3 C18 -176.8(4) . . . . ? C29 C24 P3 C12 -106.4(4) . . . . ? C25 C24 P3 C12 69.8(4) . . . . ? C17 C12 P3 C7 -69.7(5) . . . . ? C13 C12 P3 C7 108.3(5) . . . . ? C17 C12 P3 C18 50.6(5) . . . . ? C13 C12 P3 C18 -131.3(5) . . . . ? C17 C12 P3 C24 168.0(4) . . . . ? C13 C12 P3 C24 -13.9(6) . . . . ? C7 C6 Ru1 C5 22.3(5) . . . . ? C7 C6 Ru1 C2 -42.8(6) . . . . ? C7 C6 Ru1 C1 -15.0(5) . . . . ? C7 C6 Ru1 C4 41.0(6) . . . . ? C7 C6 Ru1 C3 -20.2(9) . . . . ? C7 C6 Ru1 P1 129.6(5) . . . . ? C7 C6 Ru1 P2 -128.3(5) . . . . ? C4 C5 Ru1 C6 158.9(3) . . . . ? C1 C5 Ru1 C6 -85.8(3) . . . . ? C4 C5 Ru1 C2 -78.2(3) . . . . ? C1 C5 Ru1 C2 37.1(3) . . . . ? C4 C5 Ru1 C1 -115.3(5) . . . . ? C1 C5 Ru1 C4 115.3(5) . . . . ? C4 C5 Ru1 C3 -36.1(3) . . . . ? C1 C5 Ru1 C3 79.2(3) . . . . ? C4 C5 Ru1 P1 64.1(3) . . . . ? C1 C5 Ru1 P1 179.4(3) . . . . ? C4 C5 Ru1 P2 -88.6(4) . . . . ? C1 C5 Ru1 P2 26.7(4) . . . . ? C1 C2 Ru1 C6 50.5(4) . . . . ? C3 C2 Ru1 C6 167.5(3) . . . . ? C1 C2 Ru1 C5 -37.2(3) . . . . ? C3 C2 Ru1 C5 79.8(3) . . . . ? C3 C2 Ru1 C1 117.0(4) . . . . ? C1 C2 Ru1 C4 -79.4(3) . . . . ? C3 C2 Ru1 C4 37.6(3) . . . . ? C1 C2 Ru1 C3 -117.0(4) . . . . ? C1 C2 Ru1 P1 -116.6(3) . . . . ? C3 C2 Ru1 P1 0.4(4) . . . . ? C1 C2 Ru1 P2 137.3(3) . . . . ? C3 C2 Ru1 P2 -105.7(3) . . . . ? C2 C1 Ru1 C6 -140.5(3) . . . . ? C5 C1 Ru1 C6 102.0(3) . . . . ? C2 C1 Ru1 C5 117.5(4) . . . . ? C5 C1 Ru1 C2 -117.5(4) . . . . ? C2 C1 Ru1 C4 79.2(3) . . . . ? C5 C1 Ru1 C4 -38.3(3) . . . . ? C2 C1 Ru1 C3 37.5(3) . . . . ? C5 C1 Ru1 C3 -80.0(3) . . . . ? C2 C1 Ru1 P1 116.6(3) . . . . ? C5 C1 Ru1 P1 -0.9(4) . . . . ? C2 C1 Ru1 P2 -47.5(3) . . . . ? C5 C1 Ru1 P2 -165.0(3) . . . . ? C3 C4 Ru1 C6 -150.0(3) . . . . ? C5 C4 Ru1 C6 -31.2(5) . . . . ? C3 C4 Ru1 C5 -118.8(5) . . . . ? C3 C4 Ru1 C2 -38.2(3) . . . . ? C5 C4 Ru1 C2 80.7(3) . . . . ? C3 C4 Ru1 C1 -80.5(3) . . . . ? C5 C4 Ru1 C1 38.4(3) . . . . ? C5 C4 Ru1 C3 118.8(5) . . . . ? C3 C4 Ru1 P1 120.7(3) . . . . ? C5 C4 Ru1 P1 -120.4(3) . . . . ? C3 C4 Ru1 P2 15.5(4) . . . . ? C5 C4 Ru1 P2 134.3(3) . . . . ? C4 C3 Ru1 C6 84.6(6) . . . . ? C2 C3 Ru1 C6 -31.4(7) . . . . ? C4 C3 Ru1 C5 36.6(3) . . . . ? C2 C3 Ru1 C5 -79.5(3) . . . . ? C4 C3 Ru1 C2 116.0(4) . . . . ? C4 C3 Ru1 C1 78.7(3) . . . . ? C2 C3 Ru1 C1 -37.3(3) . . . . ? C2 C3 Ru1 C4 -116.0(4) . . . . ? C4 C3 Ru1 P1 -63.7(3) . . . . ? C2 C3 Ru1 P1 -179.8(2) . . . . ? C4 C3 Ru1 P2 -168.5(3) . . . . ? C2 C3 Ru1 P2 75.5(3) . . . . ? C30 P1 Ru1 C6 15.2(2) . . . . ? C42 P1 Ru1 C6 141.3(2) . . . . ? C36 P1 Ru1 C6 -102.5(2) . . . . ? C30 P1 Ru1 C5 120.3(2) . . . . ? C42 P1 Ru1 C5 -113.6(2) . . . . ? C36 P1 Ru1 C5 2.6(2) . . . . ? C30 P1 Ru1 C2 -175.2(3) . . . . ? C42 P1 Ru1 C2 -49.1(3) . . . . ? C36 P1 Ru1 C2 67.0(3) . . . . ? C30 P1 Ru1 C1 120.9(3) . . . . ? C42 P1 Ru1 C1 -113.0(3) . . . . ? C36 P1 Ru1 C1 3.2(3) . . . . ? C30 P1 Ru1 C4 152.9(2) . . . . ? C42 P1 Ru1 C4 -81.0(2) . . . . ? C36 P1 Ru1 C4 35.2(2) . . . . ? C30 P1 Ru1 C3 -175.0(2) . . . . ? C42 P1 Ru1 C3 -48.9(2) . . . . ? C36 P1 Ru1 C3 67.3(2) . . . . ? C30 P1 Ru1 P2 -74.06(19) . . . . ? C42 P1 Ru1 P2 52.04(19) . . . . ? C36 P1 Ru1 P2 168.20(17) . . . . ? C60 P2 Ru1 C6 57.6(2) . . . . ? C48 P2 Ru1 C6 172.1(2) . . . . ? C54 P2 Ru1 C6 -65.8(2) . . . . ? C60 P2 Ru1 C5 -58.8(3) . . . . ? C48 P2 Ru1 C5 55.7(3) . . . . ? C54 P2 Ru1 C5 177.8(3) . . . . ? C60 P2 Ru1 C2 -68.0(2) . . . . ? C48 P2 Ru1 C2 46.5(2) . . . . ? C54 P2 Ru1 C2 168.7(2) . . . . ? C60 P2 Ru1 C1 -41.8(2) . . . . ? C48 P2 Ru1 C1 72.7(2) . . . . ? C54 P2 Ru1 C1 -165.2(2) . . . . ? C60 P2 Ru1 C4 -112.7(3) . . . . ? C48 P2 Ru1 C4 1.8(3) . . . . ? C54 P2 Ru1 C4 123.9(3) . . . . ? C60 P2 Ru1 C3 -103.6(2) . . . . ? C48 P2 Ru1 C3 10.9(2) . . . . ? C54 P2 Ru1 C3 133.1(2) . . . . ? C60 P2 Ru1 P1 147.83(19) . . . . ? C48 P2 Ru1 P1 -97.67(19) . . . . ? C54 P2 Ru1 P1 24.5(2) . . . . ? F2 C66 S1 O5 -57.2(6) . . . . ? F1 C66 S1 O5 -178.2(5) . . . . ? F3 C66 S1 O5 62.0(5) . . . . ? F2 C66 S1 O3 64.2(6) . . . . ? F1 C66 S1 O3 -56.8(5) . . . . ? F3 C66 S1 O3 -176.6(4) . . . . ? F2 C66 S1 O4 -177.9(5) . . . . ? F1 C66 S1 O4 61.1(5) . . . . ? F3 C66 S1 O4 -58.7(5) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N2 H2A O2 0.83(5) 2.01(5) 2.796(5) 157(5) 3_766 N1 H1A O4 0.83(7) 2.59(7) 3.224(6) 134(6) 4_675 N1 H1A O3 0.83(7) 2.27(7) 2.922(6) 136(7) 4_675 _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.09 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.738 _refine_diff_density_min -0.972 _refine_diff_density_rms 0.100 ###END data_CCDC737835_compound6b[OTf] _database_code_depnum_ccdc_archive 'CCDC 737835' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C67 H56 P3 Ru, C F3 O3 S, C H2 Cl2' _chemical_formula_sum 'C69 H58 Cl2 F3 O3 P3 Ru S' _chemical_formula_weight 1289.09 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' S S 0.1246 0.1234 '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' Cl Cl 0.1484 0.1585 '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 10.2678(14) _cell_length_b 14.522(2) _cell_length_c 20.112(3) _cell_angle_alpha 82.415(3) _cell_angle_beta 88.372(3) _cell_angle_gamma 80.570(3) _cell_volume 2932.5(7) _cell_formula_units_Z 2 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 6296 _cell_measurement_theta_min 2.26 _cell_measurement_theta_max 28.14 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.296 _exptl_crystal_size_mid 0.116 _exptl_crystal_size_min 0.096 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.460 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1324 _exptl_absorpt_coefficient_mu 0.535 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.687 _exptl_absorpt_correction_T_max 0.950 _exptl_absorpt_process_details 'SADABS v2.03; (Sheldrick)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26119 _diffrn_reflns_av_R_equivalents 0.0354 _diffrn_reflns_av_sigmaI/netI 0.0689 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.86 _diffrn_reflns_theta_max 28.35 _reflns_number_total 14178 _reflns_number_gt 10478 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0548P)^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 14178 _refine_ls_number_parameters 743 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0716 _refine_ls_R_factor_gt 0.0428 _refine_ls_wR_factor_ref 0.1062 _refine_ls_wR_factor_gt 0.0959 _refine_ls_goodness_of_fit_ref 1.003 _refine_ls_restrained_S_all 1.003 _refine_ls_shift/su_max 0.002 _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 C1 C 0.3353(3) 0.87165(19) 0.58349(13) 0.0194(6) Uani 1 1 d . . . H1 H 0.2884 0.8362 0.5565 0.023 Uiso 1 1 calc R . . C2 C 0.3005(3) 0.89141(19) 0.64944(13) 0.0194(6) Uani 1 1 d . . . H2 H 0.2258 0.8716 0.6758 0.023 Uiso 1 1 calc R . . C3 C 0.3869(3) 0.94945(19) 0.66907(13) 0.0200(6) Uani 1 1 d . . . H3 H 0.3823 0.9772 0.7111 0.024 Uiso 1 1 calc R . . C4 C 0.4753(3) 0.96603(19) 0.61442(13) 0.0206(6) Uani 1 1 d . . . H4 H 0.5424 1.0071 0.6127 0.025 Uiso 1 1 calc R . . C5 C 0.4436(3) 0.91861(18) 0.56095(13) 0.0193(6) Uani 1 1 d . . . H5 H 0.4839 0.9215 0.5161 0.023 Uiso 1 1 calc R . . C6 C 0.4970(2) 0.72649(18) 0.74220(12) 0.0135(5) Uani 1 1 d . . . C7 C 0.4375(3) 0.74155(18) 0.80179(12) 0.0150(5) Uani 1 1 d . . . C8 C 0.3613(3) 0.83166(18) 0.82144(12) 0.0168(6) Uani 1 1 d . . . C9 C 0.2259(3) 0.8556(2) 0.80880(13) 0.0213(6) Uani 1 1 d . . . H9 H 0.1842 0.8184 0.7848 0.026 Uiso 1 1 calc R . . C10 C 0.1532(3) 0.9347(2) 0.83186(15) 0.0315(8) Uani 1 1 d . . . H10 H 0.0635 0.9504 0.8226 0.038 Uiso 1 1 calc R . . C11 C 0.2129(4) 0.9900(2) 0.86835(16) 0.0363(9) Uani 1 1 d . . . H11 H 0.1635 1.0424 0.8841 0.044 Uiso 1 1 calc R . . C12 C 0.3462(4) 0.9670(2) 0.88138(15) 0.0320(8) Uani 1 1 d . . . H12 H 0.3868 1.0047 0.9056 0.038 Uiso 1 1 calc R . . C13 C 0.4208(3) 0.88799(19) 0.85857(13) 0.0225(6) Uani 1 1 d . . . H13 H 0.5104 0.8727 0.8681 0.027 Uiso 1 1 calc R . . C14 C 0.3060(2) 0.64062(18) 0.92247(12) 0.0141(5) Uani 1 1 d . . . C15 C 0.2404(3) 0.71810(19) 0.95178(13) 0.0170(5) Uani 1 1 d . . . H15 H 0.2665 0.7767 0.9415 0.020 Uiso 1 1 calc R . . C16 C 0.1361(3) 0.7070(2) 0.99632(13) 0.0185(6) Uani 1 1 d . . . H16 H 0.0915 0.7587 1.0149 0.022 Uiso 1 1 calc R . . C17 C 0.0981(3) 0.6195(2) 1.01323(13) 0.0191(6) Uani 1 1 d . . . H17 H 0.0295 0.6125 1.0437 0.023 Uiso 1 1 calc R . . C18 C 0.1623(3) 0.5427(2) 0.98471(13) 0.0198(6) Uani 1 1 d . . . H18 H 0.1366 0.4840 0.9958 0.024 Uiso 1 1 calc R . . C19 C 0.2656(3) 0.55336(19) 0.93936(13) 0.0171(6) Uani 1 1 d . . . H19 H 0.3082 0.5016 0.9201 0.021 Uiso 1 1 calc R . . C20 C 0.5736(3) 0.67398(18) 0.92947(12) 0.0155(5) Uani 1 1 d . . . C21 C 0.5491(3) 0.67083(19) 0.99837(13) 0.0180(6) Uani 1 1 d . . . H21 H 0.4726 0.6508 1.0165 0.022 Uiso 1 1 calc R . . C22 C 0.6380(3) 0.6974(2) 1.03980(13) 0.0213(6) Uani 1 1 d . . . H22 H 0.6204 0.6957 1.0855 0.026 Uiso 1 1 calc R . . C23 C 0.7530(3) 0.7265(2) 1.01355(14) 0.0217(6) Uani 1 1 d . . . H23 H 0.8121 0.7448 1.0415 0.026 Uiso 1 1 calc R . . C24 C 0.7795(3) 0.7283(2) 0.94511(14) 0.0209(6) Uani 1 1 d . . . H24 H 0.8572 0.7469 0.9275 0.025 Uiso 1 1 calc R . . C25 C 0.6910(3) 0.70253(19) 0.90322(13) 0.0185(6) Uani 1 1 d . . . H25 H 0.7093 0.7041 0.8576 0.022 Uiso 1 1 calc R . . C26 C 0.5052(3) 0.53581(18) 0.84434(12) 0.0146(5) Uani 1 1 d . . . C27 C 0.6218(3) 0.47822(19) 0.86647(13) 0.0182(6) Uani 1 1 d . . . H27 H 0.6795 0.4999 0.8933 0.022 Uiso 1 1 calc R . . C28 C 0.6516(3) 0.3881(2) 0.84827(14) 0.0229(6) Uani 1 1 d . . . H28 H 0.7296 0.3494 0.8627 0.027 Uiso 1 1 calc R . . C29 C 0.5649(3) 0.3559(2) 0.80861(14) 0.0254(7) Uani 1 1 d . . . H29 H 0.5846 0.2951 0.7972 0.030 Uiso 1 1 calc R . . C30 C 0.4488(3) 0.4134(2) 0.78576(14) 0.0236(6) Uani 1 1 d . . . H30 H 0.3917 0.3917 0.7586 0.028 Uiso 1 1 calc R . . C31 C 0.4188(3) 0.50367(19) 0.80381(13) 0.0190(6) Uani 1 1 d . . . H31 H 0.3412 0.5426 0.7889 0.023 Uiso 1 1 calc R . . C32 C 0.7546(3) 0.92689(19) 0.69879(13) 0.0194(6) Uani 1 1 d . . . C33 C 0.6690(3) 0.9613(2) 0.74781(14) 0.0258(7) Uani 1 1 d . . . H33 H 0.5990 0.9302 0.7623 0.031 Uiso 1 1 calc R . . C34 C 0.6857(4) 1.0410(2) 0.77553(17) 0.0363(8) Uani 1 1 d . . . H34 H 0.6262 1.0633 0.8077 0.044 Uiso 1 1 calc R . . C35 C 0.7905(4) 1.0875(2) 0.75550(17) 0.0395(9) Uani 1 1 d . . . H35 H 0.8023 1.1407 0.7743 0.047 Uiso 1 1 calc R . . C36 C 0.8775(4) 1.0539(2) 0.70705(17) 0.0364(8) Uani 1 1 d . . . H36 H 0.9476 1.0852 0.6931 0.044 Uiso 1 1 calc R . . C37 C 0.8611(3) 0.9739(2) 0.67912(15) 0.0266(7) Uani 1 1 d . . . H37 H 0.9211 0.9515 0.6472 0.032 Uiso 1 1 calc R . . C38 C 0.8308(3) 0.73008(19) 0.72917(12) 0.0163(5) Uani 1 1 d . . . C39 C 0.8185(3) 0.63514(19) 0.73202(13) 0.0176(6) Uani 1 1 d . . . H39 H 0.7598 0.6177 0.7035 0.021 Uiso 1 1 calc R . . C40 C 0.8925(3) 0.56611(19) 0.77675(13) 0.0185(6) Uani 1 1 d . . . H40 H 0.8835 0.5033 0.7775 0.022 Uiso 1 1 calc R . . C41 C 0.9793(3) 0.5909(2) 0.81999(13) 0.0198(6) Uani 1 1 d . . . H41 H 1.0279 0.5450 0.8503 0.024 Uiso 1 1 calc R . . C42 C 0.9935(3) 0.6852(2) 0.81789(13) 0.0197(6) Uani 1 1 d . . . H42 H 1.0522 0.7022 0.8466 0.024 Uiso 1 1 calc R . . C43 C 0.9196(3) 0.7543(2) 0.77267(13) 0.0183(6) Uani 1 1 d . . . H43 H 0.9296 0.8169 0.7716 0.022 Uiso 1 1 calc R . . C44 C 0.8339(3) 0.8190(2) 0.59227(13) 0.0185(6) Uani 1 1 d . . . C45 C 0.9339(3) 0.7449(2) 0.58243(14) 0.0254(7) Uani 1 1 d . . . H45 H 0.9511 0.6934 0.6155 0.030 Uiso 1 1 calc R . . C46 C 1.0089(3) 0.7472(2) 0.52342(16) 0.0351(8) Uani 1 1 d . . . H46 H 1.0750 0.6970 0.5172 0.042 Uiso 1 1 calc R . . C47 C 0.9851(3) 0.8241(2) 0.47405(15) 0.0358(8) Uani 1 1 d . . . H47 H 1.0359 0.8258 0.4350 0.043 Uiso 1 1 calc R . . C48 C 0.8856(3) 0.8982(2) 0.48297(15) 0.0310(7) Uani 1 1 d . . . H48 H 0.8692 0.9497 0.4498 0.037 Uiso 1 1 calc R . . C49 C 0.8103(3) 0.8958(2) 0.54146(14) 0.0230(6) Uani 1 1 d . . . H49 H 0.7433 0.9457 0.5470 0.028 Uiso 1 1 calc R . . C50 C 0.3826(3) 0.61435(19) 0.61207(12) 0.0160(5) Uani 1 1 d . . . C51 C 0.3791(3) 0.5285(2) 0.58713(14) 0.0215(6) Uani 1 1 d . . . H51 H 0.4443 0.5067 0.5574 0.026 Uiso 1 1 calc R . . C52 C 0.2796(3) 0.4762(2) 0.60642(14) 0.0251(6) Uani 1 1 d . . . H52 H 0.2795 0.4191 0.5903 0.030 Uiso 1 1 calc R . . C53 C 0.1798(3) 0.5092(2) 0.64984(14) 0.0244(6) Uani 1 1 d . . . H53 H 0.1135 0.4738 0.6632 0.029 Uiso 1 1 calc R . . C54 C 0.1798(3) 0.5942(2) 0.67281(14) 0.0212(6) Uani 1 1 d . . . H54 H 0.1121 0.6171 0.7009 0.025 Uiso 1 1 calc R . . C55 C 0.2801(3) 0.64629(19) 0.65439(13) 0.0177(6) Uani 1 1 d . . . H55 H 0.2788 0.7035 0.6706 0.021 Uiso 1 1 calc R . . C56 C 0.5147(3) 0.71384(18) 0.50268(13) 0.0176(6) Uani 1 1 d . . . C57 C 0.6147(3) 0.75935(19) 0.47179(13) 0.0203(6) Uani 1 1 d . . . H57 H 0.6855 0.7675 0.4971 0.024 Uiso 1 1 calc R . . C58 C 0.6097(3) 0.79262(19) 0.40375(13) 0.0234(6) Uani 1 1 d . . . H58 H 0.6781 0.8213 0.3837 0.028 Uiso 1 1 calc R . . C59 C 0.5040(3) 0.7833(2) 0.36587(14) 0.0283(7) Uani 1 1 d . . . H59 H 0.5007 0.8061 0.3204 0.034 Uiso 1 1 calc R . . C60 C 0.4031(3) 0.7401(2) 0.39558(14) 0.0292(7) Uani 1 1 d . . . H60 H 0.3309 0.7351 0.3702 0.035 Uiso 1 1 calc R . . C61 C 0.4086(3) 0.7036(2) 0.46403(14) 0.0236(6) Uani 1 1 d . . . H61 H 0.3417 0.6727 0.4834 0.028 Uiso 1 1 calc R . . C62 C 0.6561(3) 0.57597(19) 0.60287(12) 0.0163(5) Uani 1 1 d . . . C63 C 0.7673(3) 0.5682(2) 0.56122(14) 0.0251(7) Uani 1 1 d . . . H63 H 0.7741 0.6145 0.5252 0.030 Uiso 1 1 calc R . . C64 C 0.8679(3) 0.4915(2) 0.57339(15) 0.0338(8) Uani 1 1 d . . . H64 H 0.9414 0.4872 0.5452 0.041 Uiso 1 1 calc R . . C65 C 0.8612(3) 0.4217(2) 0.62636(14) 0.0258(7) Uani 1 1 d . . . H65 H 0.9293 0.3709 0.6340 0.031 Uiso 1 1 calc R . . C66 C 0.7514(3) 0.42839(19) 0.66799(14) 0.0199(6) Uani 1 1 d . . . H66 H 0.7454 0.3818 0.7039 0.024 Uiso 1 1 calc R . . C67 C 0.6502(3) 0.50459(19) 0.65636(13) 0.0179(6) Uani 1 1 d . . . H67 H 0.5769 0.5083 0.6847 0.021 Uiso 1 1 calc R . . P1 P 0.72884(7) 0.81696(5) 0.66829(3) 0.01534(14) Uani 1 1 d . . . P2 P 0.52206(7) 0.67858(5) 0.59440(3) 0.01412(14) Uani 1 1 d . . . P3 P 0.45489(6) 0.64999(5) 0.87199(3) 0.01294(14) Uani 1 1 d . . . Ru1 Ru 0.50765(2) 0.811001(15) 0.650329(10) 0.01263(6) Uani 1 1 d . . . C68 C 0.1809(3) 0.2298(2) 0.76897(15) 0.0256(7) Uani 1 1 d . . . F1 F 0.29127(18) 0.20974(15) 0.80549(11) 0.0444(5) Uani 1 1 d . . . F2 F 0.1660(2) 0.15124(13) 0.74399(9) 0.0371(5) Uani 1 1 d . . . F3 F 0.2020(2) 0.29369(13) 0.71709(10) 0.0451(6) Uani 1 1 d . . . S1 S 0.03798(7) 0.27402(5) 0.81828(3) 0.02327(16) Uani 1 1 d . . . O1 O 0.0335(2) 0.19982(14) 0.87310(10) 0.0294(5) Uani 1 1 d . . . O2 O 0.0725(3) 0.35909(15) 0.83714(11) 0.0412(6) Uani 1 1 d . . . O3 O -0.0681(2) 0.28649(19) 0.77143(12) 0.0457(7) Uani 1 1 d . . . C69 C 0.1762(4) 0.9294(2) 0.05237(19) 0.0410(9) Uani 1 1 d . . . H69A H 0.1211 0.9054 0.0883 0.049 Uiso 1 1 calc R . . H69B H 0.1420 0.9178 0.0103 0.049 Uiso 1 1 calc R . . Cl1 Cl 0.33843(10) 0.86865(6) 0.06283(4) 0.0438(2) Uani 1 1 d . . . Cl2 Cl 0.16708(12) 1.05135(6) 0.05229(5) 0.0564(3) Uani 1 1 d . . . H6 H 0.541(3) 0.6649(19) 0.7390(13) 0.011(7) 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 C1 0.0192(14) 0.0188(14) 0.0178(13) 0.0014(11) -0.0086(11) 0.0021(11) C2 0.0193(13) 0.0179(14) 0.0185(13) -0.0002(11) -0.0025(11) 0.0032(11) C3 0.0254(15) 0.0170(14) 0.0148(13) 0.0006(10) -0.0038(11) 0.0033(11) C4 0.0250(15) 0.0143(13) 0.0206(14) 0.0020(11) -0.0016(11) -0.0007(11) C5 0.0300(15) 0.0146(13) 0.0104(12) 0.0036(10) -0.0027(11) 0.0010(11) C6 0.0144(12) 0.0134(13) 0.0116(11) 0.0016(9) -0.0013(9) -0.0014(10) C7 0.0168(13) 0.0145(13) 0.0133(12) -0.0001(10) -0.0038(10) -0.0026(10) C8 0.0219(14) 0.0146(13) 0.0122(12) 0.0023(10) 0.0018(10) -0.0020(11) C9 0.0214(14) 0.0232(15) 0.0153(13) 0.0052(11) 0.0013(11) 0.0019(12) C10 0.0281(16) 0.0313(18) 0.0269(16) 0.0067(13) 0.0049(13) 0.0106(14) C11 0.051(2) 0.0205(16) 0.0290(17) 0.0011(13) 0.0103(16) 0.0136(15) C12 0.056(2) 0.0170(15) 0.0227(15) -0.0031(12) 0.0018(15) -0.0039(15) C13 0.0326(16) 0.0178(14) 0.0157(13) 0.0021(11) 0.0015(12) -0.0040(12) C14 0.0106(12) 0.0193(13) 0.0117(12) 0.0007(10) -0.0007(9) -0.0025(10) C15 0.0188(13) 0.0158(13) 0.0165(13) 0.0004(10) -0.0026(10) -0.0046(11) C16 0.0162(13) 0.0234(15) 0.0151(12) -0.0035(11) -0.0007(10) 0.0003(11) C17 0.0132(12) 0.0295(16) 0.0138(12) -0.0006(11) -0.0001(10) -0.0026(11) C18 0.0188(14) 0.0210(14) 0.0193(13) 0.0028(11) -0.0025(11) -0.0064(11) C19 0.0174(13) 0.0174(13) 0.0156(12) -0.0011(10) -0.0021(10) -0.0003(11) C20 0.0164(13) 0.0134(13) 0.0150(12) 0.0002(10) -0.0036(10) 0.0014(10) C21 0.0191(13) 0.0198(14) 0.0139(12) 0.0021(10) 0.0009(10) -0.0031(11) C22 0.0275(15) 0.0219(15) 0.0135(12) -0.0030(11) -0.0037(11) -0.0001(12) C23 0.0236(15) 0.0226(15) 0.0195(13) -0.0053(11) -0.0076(11) -0.0021(12) C24 0.0171(13) 0.0233(15) 0.0233(14) -0.0060(11) -0.0008(11) -0.0033(11) C25 0.0178(13) 0.0224(14) 0.0154(12) -0.0032(11) 0.0018(10) -0.0029(11) C26 0.0188(13) 0.0123(12) 0.0118(12) 0.0002(9) 0.0025(10) -0.0017(10) C27 0.0186(13) 0.0199(14) 0.0158(13) 0.0004(10) 0.0004(10) -0.0050(11) C28 0.0236(15) 0.0196(14) 0.0219(14) 0.0001(11) 0.0036(12) 0.0042(12) C29 0.0389(18) 0.0122(13) 0.0251(15) -0.0045(11) 0.0098(13) -0.0045(12) C30 0.0342(17) 0.0247(15) 0.0150(13) -0.0044(11) 0.0020(12) -0.0127(13) C31 0.0209(14) 0.0211(14) 0.0145(12) 0.0020(10) -0.0010(11) -0.0052(11) C32 0.0233(14) 0.0182(14) 0.0175(13) 0.0006(11) -0.0072(11) -0.0072(11) C33 0.0292(16) 0.0269(16) 0.0231(15) -0.0054(12) -0.0055(12) -0.0069(13) C34 0.045(2) 0.0350(19) 0.0298(17) -0.0146(14) -0.0114(15) 0.0006(16) C35 0.062(2) 0.0226(17) 0.0359(19) -0.0067(14) -0.0249(18) -0.0056(16) C36 0.048(2) 0.0296(18) 0.0338(18) 0.0063(14) -0.0162(16) -0.0185(16) C37 0.0319(17) 0.0263(16) 0.0234(15) 0.0002(12) -0.0050(13) -0.0118(13) C38 0.0156(12) 0.0212(14) 0.0117(12) -0.0002(10) 0.0009(10) -0.0038(11) C39 0.0159(13) 0.0220(14) 0.0148(12) -0.0007(10) -0.0001(10) -0.0040(11) C40 0.0193(13) 0.0173(14) 0.0179(13) 0.0011(11) 0.0010(11) -0.0025(11) C41 0.0177(13) 0.0245(15) 0.0151(13) 0.0018(11) -0.0036(10) -0.0005(11) C42 0.0155(13) 0.0291(16) 0.0148(13) -0.0037(11) -0.0034(10) -0.0036(12) C43 0.0186(13) 0.0195(14) 0.0176(13) -0.0019(11) -0.0005(10) -0.0058(11) C44 0.0180(13) 0.0235(15) 0.0138(12) 0.0002(11) -0.0002(10) -0.0049(11) C45 0.0254(15) 0.0282(16) 0.0194(14) 0.0045(12) 0.0003(12) -0.0009(13) C46 0.0278(17) 0.044(2) 0.0283(17) 0.0006(15) 0.0063(14) 0.0042(15) C47 0.0335(18) 0.050(2) 0.0203(15) 0.0025(14) 0.0098(13) -0.0031(16) C48 0.0331(17) 0.0361(18) 0.0211(15) 0.0082(13) 0.0029(13) -0.0080(14) C49 0.0223(14) 0.0233(15) 0.0215(14) 0.0027(11) -0.0009(11) -0.0023(12) C50 0.0180(13) 0.0177(13) 0.0126(12) 0.0000(10) -0.0019(10) -0.0053(11) C51 0.0233(14) 0.0216(15) 0.0198(14) -0.0048(11) 0.0001(11) -0.0020(12) C52 0.0317(16) 0.0202(15) 0.0261(15) -0.0049(12) -0.0083(13) -0.0092(13) C53 0.0196(14) 0.0283(16) 0.0253(15) 0.0054(12) -0.0051(12) -0.0103(12) C54 0.0165(13) 0.0285(16) 0.0177(13) 0.0003(11) -0.0007(11) -0.0035(12) C55 0.0197(13) 0.0181(14) 0.0147(12) -0.0010(10) -0.0037(10) -0.0013(11) C56 0.0235(14) 0.0150(13) 0.0137(12) -0.0038(10) 0.0002(10) -0.0001(11) C57 0.0243(15) 0.0183(14) 0.0180(13) -0.0031(11) 0.0008(11) -0.0022(12) C58 0.0342(16) 0.0170(14) 0.0178(13) -0.0006(11) 0.0045(12) -0.0030(12) C59 0.0470(19) 0.0227(16) 0.0139(13) 0.0008(11) -0.0032(13) -0.0041(14) C60 0.0415(19) 0.0292(17) 0.0179(14) -0.0017(12) -0.0127(13) -0.0078(14) C61 0.0288(16) 0.0234(15) 0.0189(14) -0.0012(11) -0.0023(12) -0.0059(12) C62 0.0180(13) 0.0175(13) 0.0138(12) -0.0033(10) -0.0022(10) -0.0023(11) C63 0.0239(15) 0.0312(17) 0.0168(13) 0.0029(12) 0.0035(11) 0.0002(13) C64 0.0231(16) 0.046(2) 0.0246(15) 0.0024(14) 0.0086(13) 0.0089(15) C65 0.0217(15) 0.0279(16) 0.0250(15) -0.0041(12) -0.0037(12) 0.0053(12) C66 0.0233(14) 0.0180(14) 0.0189(13) -0.0026(11) -0.0031(11) -0.0040(11) C67 0.0182(13) 0.0189(14) 0.0173(13) -0.0049(11) 0.0029(10) -0.0036(11) P1 0.0170(3) 0.0159(3) 0.0129(3) 0.0006(3) -0.0012(3) -0.0038(3) P2 0.0162(3) 0.0146(3) 0.0113(3) -0.0013(2) -0.0002(2) -0.0022(3) P3 0.0138(3) 0.0132(3) 0.0113(3) -0.0004(2) -0.0009(2) -0.0014(3) Ru1 0.01518(11) 0.01227(11) 0.00973(10) 0.00009(7) -0.00114(7) -0.00114(8) C68 0.0310(17) 0.0197(15) 0.0256(15) -0.0018(12) 0.0068(13) -0.0049(13) F1 0.0225(10) 0.0488(13) 0.0614(14) -0.0081(11) -0.0009(9) -0.0033(9) F2 0.0534(12) 0.0270(10) 0.0326(10) -0.0123(8) 0.0120(9) -0.0065(9) F3 0.0657(14) 0.0306(11) 0.0370(11) 0.0020(9) 0.0255(10) -0.0117(10) S1 0.0256(4) 0.0203(4) 0.0201(3) 0.0004(3) 0.0018(3) 0.0046(3) O1 0.0364(12) 0.0223(11) 0.0250(11) 0.0027(9) 0.0104(9) 0.0017(9) O2 0.0660(17) 0.0211(12) 0.0349(13) -0.0068(10) 0.0102(12) -0.0020(11) O3 0.0299(13) 0.0610(18) 0.0391(14) 0.0061(12) -0.0126(11) 0.0058(12) C69 0.052(2) 0.0260(18) 0.044(2) -0.0008(15) -0.0005(18) -0.0090(16) Cl1 0.0587(6) 0.0387(5) 0.0340(4) -0.0146(4) -0.0082(4) 0.0010(4) Cl2 0.0885(8) 0.0231(4) 0.0559(6) -0.0056(4) 0.0035(6) -0.0046(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 C6 C7 1.357(3) . ? C6 Ru1 2.090(2) . ? C6 H6 0.94(3) . ? C7 C8 1.505(3) . ? C7 P3 1.798(3) . ? C8 C13 1.397(4) . ? C8 C9 1.400(4) . ? C9 C10 1.389(4) . ? C9 H9 0.9300 . ? C10 C11 1.379(5) . ? C10 H10 0.9300 . ? C11 C12 1.379(5) . ? C11 H11 0.9300 . ? C12 C13 1.395(4) . ? C12 H12 0.9300 . ? C13 H13 0.9300 . ? C2 C3 1.416(4) . ? C2 C1 1.418(4) . ? C2 Ru1 2.252(3) . ? C2 H2 0.9800 . ? C1 C5 1.430(4) . ? C1 Ru1 2.242(3) . ? C1 H1 0.9800 . ? C5 C4 1.423(4) . ? C5 Ru1 2.257(2) . ? C5 H5 0.9800 . ? C4 C3 1.426(4) . ? C4 Ru1 2.245(3) . ? C4 H4 0.9800 . ? C3 Ru1 2.254(3) . ? C3 H3 0.9800 . ? C14 C19 1.394(4) . ? C14 C15 1.404(4) . ? C14 P3 1.825(2) . ? C15 C16 1.393(3) . ? C15 H15 0.9300 . ? C16 C17 1.386(4) . ? C16 H16 0.9300 . ? C17 C18 1.384(4) . ? C17 H17 0.9300 . ? C18 C19 1.394(4) . ? C18 H18 0.9300 . ? C19 H19 0.9300 . ? C20 C21 1.397(3) . ? C20 C25 1.405(4) . ? C20 P3 1.808(3) . ? C21 C22 1.386(4) . ? C21 H21 0.9300 . ? C22 C23 1.386(4) . ? C22 H22 0.9300 . ? C23 C24 1.393(4) . ? C23 H23 0.9300 . ? C24 C25 1.383(4) . ? C24 H24 0.9300 . ? C25 H25 0.9300 . ? C26 C27 1.391(4) . ? C26 C31 1.395(4) . ? C26 P3 1.809(3) . ? C27 C28 1.389(4) . ? C27 H27 0.9300 . ? C28 C29 1.387(4) . ? C28 H28 0.9300 . ? C29 C30 1.391(4) . ? C29 H29 0.9300 . ? C30 C31 1.390(4) . ? C30 H30 0.9300 . ? C31 H31 0.9300 . ? C32 C33 1.390(4) . ? C32 C37 1.403(4) . ? C32 P1 1.844(3) . ? C33 C34 1.386(4) . ? C33 H33 0.9300 . ? C34 C35 1.386(5) . ? C34 H34 0.9300 . ? C35 C36 1.385(5) . ? C35 H35 0.9300 . ? C36 C37 1.392(4) . ? C36 H36 0.9300 . ? C37 H37 0.9300 . ? C38 C43 1.397(4) . ? C38 C39 1.398(4) . ? C38 P1 1.849(3) . ? C39 C40 1.394(3) . ? C39 H39 0.9300 . ? C40 C41 1.382(4) . ? C40 H40 0.9300 . ? C41 C42 1.396(4) . ? C41 H41 0.9300 . ? C42 C43 1.399(4) . ? C42 H42 0.9300 . ? C43 H43 0.9300 . ? C44 C45 1.391(4) . ? C44 C49 1.404(4) . ? C44 P1 1.846(3) . ? C45 C46 1.396(4) . ? C45 H45 0.9300 . ? C46 C47 1.387(4) . ? C46 H46 0.9300 . ? C47 C48 1.384(4) . ? C47 H47 0.9300 . ? C48 C49 1.389(4) . ? C48 H48 0.9300 . ? C49 H49 0.9300 . ? C50 C55 1.393(3) . ? C50 C51 1.410(4) . ? C50 P2 1.835(3) . ? C51 C52 1.387(4) . ? C51 H51 0.9300 . ? C52 C53 1.393(4) . ? C52 H52 0.9300 . ? C53 C54 1.375(4) . ? C53 H53 0.9300 . ? C54 C55 1.389(4) . ? C54 H54 0.9300 . ? C55 H55 0.9300 . ? C56 C61 1.395(4) . ? C56 C57 1.398(4) . ? C56 P2 1.848(3) . ? C57 C58 1.389(4) . ? C57 H57 0.9300 . ? C58 C59 1.378(4) . ? C58 H58 0.9300 . ? C59 C60 1.379(5) . ? C59 H59 0.9300 . ? C60 C61 1.408(4) . ? C60 H60 0.9300 . ? C61 H61 0.9300 . ? C62 C63 1.395(4) . ? C62 C67 1.399(4) . ? C62 P2 1.849(3) . ? C63 C64 1.391(4) . ? C63 H63 0.9300 . ? C64 C65 1.379(4) . ? C64 H64 0.9300 . ? C65 C66 1.383(4) . ? C65 H65 0.9300 . ? C66 C67 1.389(4) . ? C66 H66 0.9300 . ? C67 H67 0.9300 . ? P1 Ru1 2.3271(8) . ? P2 Ru1 2.3354(8) . ? C68 F2 1.337(3) . ? C68 F3 1.340(3) . ? C68 F1 1.338(4) . ? C68 S1 1.824(3) . ? S1 O3 1.433(2) . ? S1 O2 1.439(3) . ? S1 O1 1.442(2) . ? C69 Cl1 1.757(4) . ? C69 Cl2 1.757(3) . ? C69 H69A 0.9700 . ? C69 H69B 0.9700 . ? 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 C7 C6 Ru1 133.59(19) . . ? C7 C6 H6 116.5(16) . . ? Ru1 C6 H6 109.9(16) . . ? C6 C7 C8 128.2(2) . . ? C6 C7 P3 120.63(19) . . ? C8 C7 P3 110.96(17) . . ? C13 C8 C9 118.5(2) . . ? C13 C8 C7 120.8(2) . . ? C9 C8 C7 120.4(3) . . ? C10 C9 C8 120.5(3) . . ? C10 C9 H9 119.8 . . ? C8 C9 H9 119.8 . . ? C11 C10 C9 120.6(3) . . ? C11 C10 H10 119.7 . . ? C9 C10 H10 119.7 . . ? C12 C11 C10 119.6(3) . . ? C12 C11 H11 120.2 . . ? C10 C11 H11 120.2 . . ? C11 C12 C13 120.6(3) . . ? C11 C12 H12 119.7 . . ? C13 C12 H12 119.7 . . ? C12 C13 C8 120.2(3) . . ? C12 C13 H13 119.9 . . ? C8 C13 H13 119.9 . . ? C3 C2 C1 108.4(2) . . ? C3 C2 Ru1 71.74(15) . . ? C1 C2 Ru1 71.22(15) . . ? C3 C2 H2 125.8 . . ? C1 C2 H2 125.8 . . ? Ru1 C2 H2 125.8 . . ? C2 C1 C5 108.5(3) . . ? C2 C1 Ru1 72.00(15) . . ? C5 C1 Ru1 72.04(15) . . ? C2 C1 H1 125.7 . . ? C5 C1 H1 125.7 . . ? Ru1 C1 H1 125.7 . . ? C4 C5 C1 106.9(2) . . ? C4 C5 Ru1 71.12(14) . . ? C1 C5 Ru1 70.89(14) . . ? C4 C5 H5 126.5 . . ? C1 C5 H5 126.5 . . ? Ru1 C5 H5 126.5 . . ? C3 C4 C5 108.8(3) . . ? C3 C4 Ru1 71.85(15) . . ? C5 C4 Ru1 72.04(15) . . ? C3 C4 H4 125.5 . . ? C5 C4 H4 125.5 . . ? Ru1 C4 H4 125.5 . . ? C2 C3 C4 107.5(2) . . ? C2 C3 Ru1 71.61(15) . . ? C4 C3 Ru1 71.18(15) . . ? C2 C3 H3 126.2 . . ? C4 C3 H3 126.2 . . ? Ru1 C3 H3 126.2 . . ? C19 C14 C15 118.8(2) . . ? C19 C14 P3 120.08(19) . . ? C15 C14 P3 120.6(2) . . ? C16 C15 C14 119.9(3) . . ? C16 C15 H15 120.1 . . ? C14 C15 H15 120.1 . . ? C17 C16 C15 120.6(2) . . ? C17 C16 H16 119.7 . . ? C15 C16 H16 119.7 . . ? C18 C17 C16 119.9(2) . . ? C18 C17 H17 120.0 . . ? C16 C17 H17 120.0 . . ? C17 C18 C19 119.9(3) . . ? C17 C18 H18 120.1 . . ? C19 C18 H18 120.1 . . ? C18 C19 C14 120.9(2) . . ? C18 C19 H19 119.6 . . ? C14 C19 H19 119.6 . . ? C21 C20 C25 118.9(3) . . ? C21 C20 P3 122.3(2) . . ? C25 C20 P3 118.59(19) . . ? C22 C21 C20 120.4(3) . . ? C22 C21 H21 119.8 . . ? C20 C21 H21 119.8 . . ? C23 C22 C21 120.4(2) . . ? C23 C22 H22 119.8 . . ? C21 C22 H22 119.8 . . ? C22 C23 C24 119.6(3) . . ? C22 C23 H23 120.2 . . ? C24 C23 H23 120.2 . . ? C25 C24 C23 120.4(3) . . ? C25 C24 H24 119.8 . . ? C23 C24 H24 119.8 . . ? C24 C25 C20 120.2(2) . . ? C24 C25 H25 119.9 . . ? C20 C25 H25 119.9 . . ? C27 C26 C31 120.4(2) . . ? C27 C26 P3 121.4(2) . . ? C31 C26 P3 118.02(19) . . ? C28 C27 C26 119.6(3) . . ? C28 C27 H27 120.2 . . ? C26 C27 H27 120.2 . . ? C29 C28 C27 120.0(3) . . ? C29 C28 H28 120.0 . . ? C27 C28 H28 120.0 . . ? C28 C29 C30 120.7(3) . . ? C28 C29 H29 119.6 . . ? C30 C29 H29 119.6 . . ? C29 C30 C31 119.4(3) . . ? C29 C30 H30 120.3 . . ? C31 C30 H30 120.3 . . ? C30 C31 C26 119.9(3) . . ? C30 C31 H31 120.0 . . ? C26 C31 H31 120.0 . . ? C33 C32 C37 118.0(3) . . ? C33 C32 P1 118.0(2) . . ? C37 C32 P1 123.8(2) . . ? C34 C33 C32 121.4(3) . . ? C34 C33 H33 119.3 . . ? C32 C33 H33 119.3 . . ? C33 C34 C35 120.3(3) . . ? C33 C34 H34 119.9 . . ? C35 C34 H34 119.9 . . ? C36 C35 C34 119.2(3) . . ? C36 C35 H35 120.4 . . ? C34 C35 H35 120.4 . . ? C35 C36 C37 120.6(3) . . ? C35 C36 H36 119.7 . . ? C37 C36 H36 119.7 . . ? C36 C37 C32 120.4(3) . . ? C36 C37 H37 119.8 . . ? C32 C37 H37 119.8 . . ? C43 C38 C39 118.1(2) . . ? C43 C38 P1 123.4(2) . . ? C39 C38 P1 118.5(2) . . ? C40 C39 C38 121.4(3) . . ? C40 C39 H39 119.3 . . ? C38 C39 H39 119.3 . . ? C41 C40 C39 120.1(3) . . ? C41 C40 H40 120.0 . . ? C39 C40 H40 120.0 . . ? C40 C41 C42 119.6(2) . . ? C40 C41 H41 120.2 . . ? C42 C41 H41 120.2 . . ? C41 C42 C43 120.2(3) . . ? C41 C42 H42 119.9 . . ? C43 C42 H42 119.9 . . ? C38 C43 C42 120.7(3) . . ? C38 C43 H43 119.6 . . ? C42 C43 H43 119.6 . . ? C45 C44 C49 118.4(2) . . ? C45 C44 P1 122.0(2) . . ? C49 C44 P1 119.6(2) . . ? C44 C45 C46 120.6(3) . . ? C44 C45 H45 119.7 . . ? C46 C45 H45 119.7 . . ? C47 C46 C45 120.2(3) . . ? C47 C46 H46 119.9 . . ? C45 C46 H46 119.9 . . ? C48 C47 C46 119.9(3) . . ? C48 C47 H47 120.0 . . ? C46 C47 H47 120.0 . . ? C47 C48 C49 120.0(3) . . ? C47 C48 H48 120.0 . . ? C49 C48 H48 120.0 . . ? C48 C49 C44 120.9(3) . . ? C48 C49 H49 119.5 . . ? C44 C49 H49 119.5 . . ? C55 C50 C51 117.6(2) . . ? C55 C50 P2 120.6(2) . . ? C51 C50 P2 121.65(19) . . ? C52 C51 C50 120.8(3) . . ? C52 C51 H51 119.6 . . ? C50 C51 H51 119.6 . . ? C51 C52 C53 120.1(3) . . ? C51 C52 H52 119.9 . . ? C53 C52 H52 119.9 . . ? C54 C53 C52 119.5(3) . . ? C54 C53 H53 120.2 . . ? C52 C53 H53 120.2 . . ? C53 C54 C55 120.6(3) . . ? C53 C54 H54 119.7 . . ? C55 C54 H54 119.7 . . ? C54 C55 C50 121.2(3) . . ? C54 C55 H55 119.4 . . ? C50 C55 H55 119.4 . . ? C61 C56 C57 118.7(2) . . ? C61 C56 P2 122.7(2) . . ? C57 C56 P2 118.4(2) . . ? C58 C57 C56 120.8(3) . . ? C58 C57 H57 119.6 . . ? C56 C57 H57 119.6 . . ? C59 C58 C57 120.4(3) . . ? C59 C58 H58 119.8 . . ? C57 C58 H58 119.8 . . ? C60 C59 C58 119.8(3) . . ? C60 C59 H59 120.1 . . ? C58 C59 H59 120.1 . . ? C59 C60 C61 120.5(3) . . ? C59 C60 H60 119.7 . . ? C61 C60 H60 119.7 . . ? C56 C61 C60 119.8(3) . . ? C56 C61 H61 120.1 . . ? C60 C61 H61 120.1 . . ? C63 C62 C67 117.9(2) . . ? C63 C62 P2 123.6(2) . . ? C67 C62 P2 118.43(19) . . ? C64 C63 C62 120.2(3) . . ? C64 C63 H63 119.9 . . ? C62 C63 H63 119.9 . . ? C65 C64 C63 121.4(3) . . ? C65 C64 H64 119.3 . . ? C63 C64 H64 119.3 . . ? C64 C65 C66 119.0(3) . . ? C64 C65 H65 120.5 . . ? C66 C65 H65 120.5 . . ? C65 C66 C67 120.1(3) . . ? C65 C66 H66 119.9 . . ? C67 C66 H66 119.9 . . ? C66 C67 C62 121.4(2) . . ? C66 C67 H67 119.3 . . ? C62 C67 H67 119.3 . . ? C32 P1 C44 100.74(13) . . ? C32 P1 C38 99.87(13) . . ? C44 P1 C38 102.64(12) . . ? C32 P1 Ru1 113.09(9) . . ? C44 P1 Ru1 115.10(9) . . ? C38 P1 Ru1 122.30(9) . . ? C50 P2 C56 103.79(13) . . ? C50 P2 C62 97.88(12) . . ? C56 P2 C62 102.60(11) . . ? C50 P2 Ru1 113.46(8) . . ? C56 P2 Ru1 110.37(9) . . ? C62 P2 Ru1 126.07(9) . . ? C7 P3 C20 108.80(13) . . ? C7 P3 C26 110.84(12) . . ? C20 P3 C26 111.03(12) . . ? C7 P3 C14 115.46(11) . . ? C20 P3 C14 104.76(12) . . ? C26 P3 C14 105.78(12) . . ? C6 Ru1 C1 125.01(10) . . ? C6 Ru1 C4 136.17(10) . . ? C1 Ru1 C4 61.43(11) . . ? C6 Ru1 C2 97.95(10) . . ? C1 Ru1 C2 36.77(9) . . ? C4 Ru1 C2 61.29(10) . . ? C6 Ru1 C3 103.00(10) . . ? C1 Ru1 C3 61.48(10) . . ? C4 Ru1 C3 36.97(9) . . ? C2 Ru1 C3 36.64(10) . . ? C6 Ru1 C5 159.59(10) . . ? C1 Ru1 C5 37.08(10) . . ? C4 Ru1 C5 36.85(10) . . ? C2 Ru1 C5 61.66(10) . . ? C3 Ru1 C5 61.82(9) . . ? C6 Ru1 P1 90.75(7) . . ? C1 Ru1 P1 143.69(8) . . ? C4 Ru1 P1 89.33(8) . . ? C2 Ru1 P1 145.13(8) . . ? C3 Ru1 P1 108.49(8) . . ? C5 Ru1 P1 106.63(8) . . ? C6 Ru1 P2 90.06(8) . . ? C1 Ru1 P2 85.65(8) . . ? C4 Ru1 P2 132.62(7) . . ? C2 Ru1 P2 111.68(8) . . ? C3 Ru1 P2 146.48(8) . . ? C5 Ru1 P2 96.51(7) . . ? P1 Ru1 P2 101.96(3) . . ? F2 C68 F3 107.4(2) . . ? F2 C68 F1 107.1(2) . . ? F3 C68 F1 107.1(3) . . ? F2 C68 S1 112.3(2) . . ? F3 C68 S1 110.9(2) . . ? F1 C68 S1 111.8(2) . . ? O3 S1 O2 115.72(16) . . ? O3 S1 O1 114.76(15) . . ? O2 S1 O1 114.63(14) . . ? O3 S1 C68 102.68(15) . . ? O2 S1 C68 102.74(14) . . ? O1 S1 C68 103.81(12) . . ? Cl1 C69 Cl2 112.4(2) . . ? Cl1 C69 H69A 109.1 . . ? Cl2 C69 H69A 109.1 . . ? Cl1 C69 H69B 109.1 . . ? Cl2 C69 H69B 109.1 . . ? H69A C69 H69B 107.9 . . ? 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 C6 C7 C8 -3.4(5) . . . . ? Ru1 C6 C7 P3 -178.24(16) . . . . ? C6 C7 C8 C13 -98.9(3) . . . . ? P3 C7 C8 C13 76.3(3) . . . . ? C6 C7 C8 C9 87.7(4) . . . . ? P3 C7 C8 C9 -97.1(3) . . . . ? C13 C8 C9 C10 1.1(4) . . . . ? C7 C8 C9 C10 174.6(2) . . . . ? C8 C9 C10 C11 -0.9(4) . . . . ? C9 C10 C11 C12 0.7(4) . . . . ? C10 C11 C12 C13 -0.7(5) . . . . ? C11 C12 C13 C8 0.8(4) . . . . ? C9 C8 C13 C12 -1.0(4) . . . . ? C7 C8 C13 C12 -174.5(2) . . . . ? C3 C2 C1 C5 -0.7(3) . . . . ? Ru1 C2 C1 C5 -63.23(18) . . . . ? C3 C2 C1 Ru1 62.51(18) . . . . ? C2 C1 C5 C4 0.8(3) . . . . ? Ru1 C1 C5 C4 -62.42(17) . . . . ? C2 C1 C5 Ru1 63.21(18) . . . . ? C1 C5 C4 C3 -0.6(3) . . . . ? Ru1 C5 C4 C3 -62.84(18) . . . . ? C1 C5 C4 Ru1 62.27(17) . . . . ? C1 C2 C3 C4 0.4(3) . . . . ? Ru1 C2 C3 C4 62.54(17) . . . . ? C1 C2 C3 Ru1 -62.18(17) . . . . ? C5 C4 C3 C2 0.1(3) . . . . ? Ru1 C4 C3 C2 -62.82(18) . . . . ? C5 C4 C3 Ru1 62.96(18) . . . . ? C19 C14 C15 C16 -0.6(4) . . . . ? P3 C14 C15 C16 -172.6(2) . . . . ? C14 C15 C16 C17 1.4(4) . . . . ? C15 C16 C17 C18 -1.3(4) . . . . ? C16 C17 C18 C19 0.4(4) . . . . ? C17 C18 C19 C14 0.4(4) . . . . ? C15 C14 C19 C18 -0.3(4) . . . . ? P3 C14 C19 C18 171.8(2) . . . . ? C25 C20 C21 C22 1.4(4) . . . . ? P3 C20 C21 C22 -174.5(2) . . . . ? C20 C21 C22 C23 -0.7(4) . . . . ? C21 C22 C23 C24 -0.5(4) . . . . ? C22 C23 C24 C25 0.9(4) . . . . ? C23 C24 C25 C20 -0.2(4) . . . . ? C21 C20 C25 C24 -0.9(4) . . . . ? P3 C20 C25 C24 175.1(2) . . . . ? C31 C26 C27 C28 -0.3(4) . . . . ? P3 C26 C27 C28 174.9(2) . . . . ? C26 C27 C28 C29 -0.4(4) . . . . ? C27 C28 C29 C30 1.0(4) . . . . ? C28 C29 C30 C31 -1.0(4) . . . . ? C29 C30 C31 C26 0.2(4) . . . . ? C27 C26 C31 C30 0.4(4) . . . . ? P3 C26 C31 C30 -175.0(2) . . . . ? C37 C32 C33 C34 1.6(4) . . . . ? P1 C32 C33 C34 176.9(2) . . . . ? C32 C33 C34 C35 -1.1(5) . . . . ? C33 C34 C35 C36 0.6(5) . . . . ? C34 C35 C36 C37 -0.6(5) . . . . ? C35 C36 C37 C32 1.1(5) . . . . ? C33 C32 C37 C36 -1.6(4) . . . . ? P1 C32 C37 C36 -176.6(2) . . . . ? C43 C38 C39 C40 -0.1(4) . . . . ? P1 C38 C39 C40 179.99(19) . . . . ? C38 C39 C40 C41 0.6(4) . . . . ? C39 C40 C41 C42 -0.8(4) . . . . ? C40 C41 C42 C43 0.5(4) . . . . ? C39 C38 C43 C42 -0.3(4) . . . . ? P1 C38 C43 C42 179.65(19) . . . . ? C41 C42 C43 C38 0.1(4) . . . . ? C49 C44 C45 C46 0.0(5) . . . . ? P1 C44 C45 C46 177.9(3) . . . . ? C44 C45 C46 C47 0.6(5) . . . . ? C45 C46 C47 C48 -0.8(6) . . . . ? C46 C47 C48 C49 0.4(5) . . . . ? C47 C48 C49 C44 0.3(5) . . . . ? C45 C44 C49 C48 -0.5(5) . . . . ? P1 C44 C49 C48 -178.4(3) . . . . ? C55 C50 C51 C52 -2.5(4) . . . . ? P2 C50 C51 C52 173.5(2) . . . . ? C50 C51 C52 C53 1.4(4) . . . . ? C51 C52 C53 C54 0.7(4) . . . . ? C52 C53 C54 C55 -1.6(4) . . . . ? C53 C54 C55 C50 0.3(4) . . . . ? C51 C50 C55 C54 1.7(4) . . . . ? P2 C50 C55 C54 -174.4(2) . . . . ? C61 C56 C57 C58 -0.9(4) . . . . ? P2 C56 C57 C58 -175.9(2) . . . . ? C56 C57 C58 C59 1.6(4) . . . . ? C57 C58 C59 C60 -0.5(4) . . . . ? C58 C59 C60 C61 -1.4(5) . . . . ? C57 C56 C61 C60 -1.0(4) . . . . ? P2 C56 C61 C60 173.8(2) . . . . ? C59 C60 C61 C56 2.1(4) . . . . ? C67 C62 C63 C64 -0.1(4) . . . . ? P2 C62 C63 C64 175.9(3) . . . . ? C62 C63 C64 C65 -0.1(5) . . . . ? C63 C64 C65 C66 0.2(5) . . . . ? C64 C65 C66 C67 -0.1(5) . . . . ? C65 C66 C67 C62 0.0(4) . . . . ? C63 C62 C67 C66 0.1(4) . . . . ? P2 C62 C67 C66 -176.1(2) . . . . ? C33 C32 P1 C44 166.2(2) . . . . ? C37 C32 P1 C44 -18.8(3) . . . . ? C33 C32 P1 C38 -88.8(2) . . . . ? C37 C32 P1 C38 86.2(3) . . . . ? C33 C32 P1 Ru1 42.8(2) . . . . ? C37 C32 P1 Ru1 -142.2(2) . . . . ? C45 C44 P1 C32 124.3(3) . . . . ? C49 C44 P1 C32 -57.9(3) . . . . ? C45 C44 P1 C38 21.5(3) . . . . ? C49 C44 P1 C38 -160.7(2) . . . . ? C45 C44 P1 Ru1 -113.7(2) . . . . ? C49 C44 P1 Ru1 64.1(3) . . . . ? C43 C38 P1 C32 -12.2(2) . . . . ? C39 C38 P1 C32 167.7(2) . . . . ? C43 C38 P1 C44 91.3(2) . . . . ? C39 C38 P1 C44 -88.8(2) . . . . ? C43 C38 P1 Ru1 -137.70(19) . . . . ? C39 C38 P1 Ru1 42.2(2) . . . . ? C55 C50 P2 C56 -118.8(2) . . . . ? C51 C50 P2 C56 65.3(2) . . . . ? C55 C50 P2 C62 136.1(2) . . . . ? C51 C50 P2 C62 -39.8(2) . . . . ? C55 C50 P2 Ru1 1.0(2) . . . . ? C51 C50 P2 Ru1 -174.90(19) . . . . ? C61 C56 P2 C50 9.5(3) . . . . ? C57 C56 P2 C50 -175.6(2) . . . . ? C61 C56 P2 C62 111.0(2) . . . . ? C57 C56 P2 C62 -74.1(2) . . . . ? C61 C56 P2 Ru1 -112.4(2) . . . . ? C57 C56 P2 Ru1 62.5(2) . . . . ? C63 C62 P2 C50 140.8(3) . . . . ? C67 C62 P2 C50 -43.2(2) . . . . ? C63 C62 P2 C56 34.7(3) . . . . ? C67 C62 P2 C56 -149.3(2) . . . . ? C63 C62 P2 Ru1 -92.5(2) . . . . ? C67 C62 P2 Ru1 83.6(2) . . . . ? C6 C7 P3 C20 102.5(2) . . . . ? C8 C7 P3 C20 -73.2(2) . . . . ? C6 C7 P3 C26 -19.9(3) . . . . ? C8 C7 P3 C26 164.46(19) . . . . ? C6 C7 P3 C14 -140.1(2) . . . . ? C8 C7 P3 C14 44.2(2) . . . . ? C21 C20 P3 C7 131.7(2) . . . . ? C25 C20 P3 C7 -44.2(2) . . . . ? C21 C20 P3 C26 -106.0(2) . . . . ? C25 C20 P3 C26 78.0(2) . . . . ? C21 C20 P3 C14 7.7(2) . . . . ? C25 C20 P3 C14 -168.2(2) . . . . ? C27 C26 P3 C7 120.8(2) . . . . ? C31 C26 P3 C7 -63.9(2) . . . . ? C27 C26 P3 C20 -0.3(2) . . . . ? C31 C26 P3 C20 175.08(19) . . . . ? C27 C26 P3 C14 -113.4(2) . . . . ? C31 C26 P3 C14 62.0(2) . . . . ? C19 C14 P3 C7 131.3(2) . . . . ? C15 C14 P3 C7 -56.8(3) . . . . ? C19 C14 P3 C20 -109.1(2) . . . . ? C15 C14 P3 C20 62.8(2) . . . . ? C19 C14 P3 C26 8.3(2) . . . . ? C15 C14 P3 C26 -179.8(2) . . . . ? C7 C6 Ru1 C1 -64.4(3) . . . . ? C7 C6 Ru1 C4 19.0(4) . . . . ? C7 C6 Ru1 C2 -37.3(3) . . . . ? C7 C6 Ru1 C3 -0.3(3) . . . . ? C7 C6 Ru1 C5 -40.0(5) . . . . ? C7 C6 Ru1 P1 108.9(3) . . . . ? C7 C6 Ru1 P2 -149.2(3) . . . . ? C2 C1 Ru1 C6 49.1(2) . . . . ? C5 C1 Ru1 C6 166.16(15) . . . . ? C2 C1 Ru1 C4 -79.34(18) . . . . ? C5 C1 Ru1 C4 37.74(15) . . . . ? C5 C1 Ru1 C2 117.1(2) . . . . ? C2 C1 Ru1 C3 -37.03(16) . . . . ? C5 C1 Ru1 C3 80.06(17) . . . . ? C2 C1 Ru1 C5 -117.1(2) . . . . ? C2 C1 Ru1 P1 -119.57(16) . . . . ? C5 C1 Ru1 P1 -2.5(2) . . . . ? C2 C1 Ru1 P2 136.10(17) . . . . ? C5 C1 Ru1 P2 -106.81(15) . . . . ? C3 C4 Ru1 C6 -32.5(2) . . . . ? C5 C4 Ru1 C6 -150.07(17) . . . . ? C3 C4 Ru1 C1 79.60(18) . . . . ? C5 C4 Ru1 C1 -37.98(16) . . . . ? C3 C4 Ru1 C2 37.48(16) . . . . ? C5 C4 Ru1 C2 -80.11(18) . . . . ? C5 C4 Ru1 C3 -117.6(2) . . . . ? C3 C4 Ru1 C5 117.6(2) . . . . ? C3 C4 Ru1 P1 -122.88(16) . . . . ? C5 C4 Ru1 P1 119.53(16) . . . . ? C3 C4 Ru1 P2 131.40(15) . . . . ? C5 C4 Ru1 P2 13.8(2) . . . . ? C3 C2 Ru1 C6 101.11(16) . . . . ? C1 C2 Ru1 C6 -141.33(18) . . . . ? C3 C2 Ru1 C1 -117.6(2) . . . . ? C3 C2 Ru1 C4 -37.82(15) . . . . ? C1 C2 Ru1 C4 79.74(18) . . . . ? C1 C2 Ru1 C3 117.6(2) . . . . ? C3 C2 Ru1 C5 -79.98(17) . . . . ? C1 C2 Ru1 C5 37.58(17) . . . . ? C3 C2 Ru1 P1 -1.8(2) . . . . ? C1 C2 Ru1 P1 115.74(17) . . . . ? C3 C2 Ru1 P2 -165.63(13) . . . . ? C1 C2 Ru1 P2 -48.08(18) . . . . ? C2 C3 Ru1 C6 -85.84(17) . . . . ? C4 C3 Ru1 C6 157.56(17) . . . . ? C2 C3 Ru1 C1 37.16(15) . . . . ? C4 C3 Ru1 C1 -79.44(18) . . . . ? C2 C3 Ru1 C4 116.6(2) . . . . ? C4 C3 Ru1 C2 -116.6(2) . . . . ? C2 C3 Ru1 C5 79.51(17) . . . . ? C4 C3 Ru1 C5 -37.08(17) . . . . ? C2 C3 Ru1 P1 178.91(13) . . . . ? C4 C3 Ru1 P1 62.31(17) . . . . ? C2 C3 Ru1 P2 24.7(2) . . . . ? C4 C3 Ru1 P2 -91.9(2) . . . . ? C4 C5 Ru1 C6 82.1(3) . . . . ? C1 C5 Ru1 C6 -34.2(4) . . . . ? C4 C5 Ru1 C1 116.3(2) . . . . ? C1 C5 Ru1 C4 -116.3(2) . . . . ? C4 C5 Ru1 C2 79.03(17) . . . . ? C1 C5 Ru1 C2 -37.27(16) . . . . ? C4 C5 Ru1 C3 37.21(16) . . . . ? C1 C5 Ru1 C3 -79.09(17) . . . . ? C4 C5 Ru1 P1 -65.23(16) . . . . ? C1 C5 Ru1 P1 178.46(14) . . . . ? C4 C5 Ru1 P2 -169.81(15) . . . . ? C1 C5 Ru1 P2 73.88(15) . . . . ? C32 P1 Ru1 C6 -99.99(12) . . . . ? C44 P1 Ru1 C6 144.95(12) . . . . ? C38 P1 Ru1 C6 19.35(12) . . . . ? C32 P1 Ru1 C1 70.73(16) . . . . ? C44 P1 Ru1 C1 -44.33(16) . . . . ? C38 P1 Ru1 C1 -169.92(15) . . . . ? C32 P1 Ru1 C4 36.17(11) . . . . ? C44 P1 Ru1 C4 -78.89(12) . . . . ? C38 P1 Ru1 C4 155.52(12) . . . . ? C32 P1 Ru1 C2 5.13(16) . . . . ? C44 P1 Ru1 C2 -109.92(15) . . . . ? C38 P1 Ru1 C2 124.48(16) . . . . ? C32 P1 Ru1 C3 3.99(12) . . . . ? C44 P1 Ru1 C3 -111.07(12) . . . . ? C38 P1 Ru1 C3 123.34(12) . . . . ? C32 P1 Ru1 C5 69.17(12) . . . . ? C44 P1 Ru1 C5 -45.89(12) . . . . ? C38 P1 Ru1 C5 -171.49(12) . . . . ? C32 P1 Ru1 P2 169.78(9) . . . . ? C44 P1 Ru1 P2 54.73(10) . . . . ? C38 P1 Ru1 P2 -70.87(10) . . . . ? C50 P2 Ru1 C6 57.25(12) . . . . ? C56 P2 Ru1 C6 173.25(12) . . . . ? C62 P2 Ru1 C6 -62.82(13) . . . . ? C50 P2 Ru1 C1 -67.87(12) . . . . ? C56 P2 Ru1 C1 48.12(12) . . . . ? C62 P2 Ru1 C1 172.06(13) . . . . ? C50 P2 Ru1 C4 -111.67(14) . . . . ? C56 P2 Ru1 C4 4.33(14) . . . . ? C62 P2 Ru1 C4 128.27(14) . . . . ? C50 P2 Ru1 C2 -41.34(12) . . . . ? C56 P2 Ru1 C2 74.66(12) . . . . ? C62 P2 Ru1 C2 -161.40(13) . . . . ? C50 P2 Ru1 C3 -56.89(16) . . . . ? C56 P2 Ru1 C3 59.10(16) . . . . ? C62 P2 Ru1 C3 -176.96(16) . . . . ? C50 P2 Ru1 C5 -103.38(12) . . . . ? C56 P2 Ru1 C5 12.61(12) . . . . ? C62 P2 Ru1 C5 136.55(13) . . . . ? C50 P2 Ru1 P1 148.04(9) . . . . ? C56 P2 Ru1 P1 -95.97(10) . . . . ? C62 P2 Ru1 P1 27.97(11) . . . . ? F2 C68 S1 O3 -57.1(2) . . . . ? F3 C68 S1 O3 63.0(3) . . . . ? F1 C68 S1 O3 -177.4(2) . . . . ? F2 C68 S1 O2 -177.5(2) . . . . ? F3 C68 S1 O2 -57.4(3) . . . . ? F1 C68 S1 O2 62.1(2) . . . . ? F2 C68 S1 O1 62.8(2) . . . . ? F3 C68 S1 O1 -177.1(2) . . . . ? F1 C68 S1 O1 -57.6(2) . . . . ? _diffrn_measured_fraction_theta_max 0.968 _diffrn_reflns_theta_full 28.35 _diffrn_measured_fraction_theta_full 0.968 _refine_diff_density_max 1.311 _refine_diff_density_min -1.017 _refine_diff_density_rms 0.099 ###END data_CCDC737836_compound6c[OTf] _database_code_depnum_ccdc_archive 'CCDC 737836' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C68 H58 O P3 Ru, C F3 O3 S, 0.56(C H2 Cl2)' _chemical_formula_sum 'C69.56 H59.11 Cl1.11 F3 O4 P3 Ru S' _chemical_formula_weight 1281.43 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' S S 0.1246 0.1234 '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' Cl Cl 0.1484 0.1585 '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 10.3173(14) _cell_length_b 14.380(2) _cell_length_c 20.203(3) _cell_angle_alpha 82.335(3) _cell_angle_beta 88.087(3) _cell_angle_gamma 80.744(3) _cell_volume 2931.7(7) _cell_formula_units_Z 2 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 2202 _cell_measurement_theta_min 2.23 _cell_measurement_theta_max 21.12 _exptl_crystal_description needles _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.452 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1318.2 _exptl_absorpt_coefficient_mu 0.496 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.880 _exptl_absorpt_correction_T_max 0.985 _exptl_absorpt_process_details 'SADABS v2.03; (Sheldrick)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18538 _diffrn_reflns_av_R_equivalents 0.0670 _diffrn_reflns_av_sigmaI/netI 0.1142 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.02 _diffrn_reflns_theta_max 22.61 _reflns_number_total 7692 _reflns_number_gt 5731 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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. H6 was located by difference map after all other atoms were located. The position of the methoxy group as disordered over two sites with a refined relative occupancy of 56:44. With the major form, a dichloromethane (DCM) of crystallisation was observed which was included in the model. An equivalent DCM could not be located for the minor form. In the minor form, the C-O distances for the methoxy group were restrained to be 1.415 angstroms. The C-Cl distances in the DCM were restrained to be equal; the distances were lower than expected due to libration. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+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 7691 _refine_ls_number_parameters 783 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0784 _refine_ls_R_factor_gt 0.0503 _refine_ls_wR_factor_ref 0.1213 _refine_ls_wR_factor_gt 0.1093 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.046 _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 C1 C 0.4446(5) 0.9180(4) 0.5629(3) 0.0227(13) Uani 1 1 d . . . H1 H 0.4841 0.9202 0.5169 0.027 Uiso 1 1 calc R . . C2 C 0.4781(5) 0.9673(4) 0.6143(2) 0.0220(13) Uani 1 1 d . . . H2 H 0.5460 1.0102 0.6111 0.026 Uiso 1 1 calc R . . C3 C 0.3916(5) 0.9513(4) 0.6696(3) 0.0219(13) Uani 1 1 d . . . H3 H 0.3879 0.9807 0.7119 0.026 Uiso 1 1 calc R . . C4 C 0.3065(5) 0.8919(4) 0.6517(3) 0.0241(13) Uani 1 1 d . . . H4 H 0.2318 0.8714 0.6797 0.029 Uiso 1 1 calc R . . C5 C 0.3379(5) 0.8706(4) 0.5866(3) 0.0214(13) Uani 1 1 d . . . H5 H 0.2889 0.8338 0.5602 0.026 Uiso 1 1 calc R . . C6 C 0.5007(5) 0.7264(4) 0.7413(3) 0.0204(13) Uani 1 1 d . . . H6 H 0.541(5) 0.664(3) 0.744(2) 0.016(14) Uiso 1 1 d . . . C7 C 0.4410(5) 0.7413(4) 0.8015(3) 0.0204(13) Uani 1 1 d . . . C8 C 0.3694(5) 0.8322(4) 0.8214(3) 0.0236(14) Uani 1 1 d . . . C9 C 0.2335(6) 0.8573(4) 0.8129(3) 0.0322(15) Uani 1 1 d . A . H9 H 0.1888 0.8197 0.7889 0.039 Uiso 1 1 calc R . . C10 C 0.1625(7) 0.9347(5) 0.8383(4) 0.056(2) Uani 1 1 d D . . H10 H 0.0698 0.9489 0.8341 0.067 Uiso 0.556(4) 1 calc PR A 1 C11 C 0.2315(8) 0.9917(4) 0.8704(3) 0.053(2) Uani 1 1 d . A . H11 H 0.1850 1.0472 0.8861 0.064 Uiso 1 1 calc R . . C12 C 0.3635(8) 0.9696(5) 0.8797(3) 0.0493(19) Uani 1 1 d . . . H12 H 0.4079 1.0087 0.9024 0.059 Uiso 0.444(4) 1 calc PR A 2 C13 C 0.4336(6) 0.8887(4) 0.8556(3) 0.0338(15) Uani 1 1 d . A . H13 H 0.5254 0.8725 0.8627 0.041 Uiso 1 1 calc R . . C14 C 0.3949(17) 1.0910(8) 0.9416(7) 0.089(6) Uani 0.556(4) 1 d P A 1 H14A H 0.3613 1.1413 0.9059 0.133 Uiso 0.556(4) 1 calc PR A 1 H14B H 0.4597 1.1133 0.9675 0.133 Uiso 0.556(4) 1 calc PR A 1 H14C H 0.3222 1.0748 0.9710 0.133 Uiso 0.556(4) 1 calc PR A 1 C14A C -0.0558(15) 0.9873(11) 0.8881(7) 0.075(6) Uani 0.444(4) 1 d PD A 2 H14D H -0.0161 0.9795 0.9323 0.112 Uiso 0.444(4) 1 calc PR A 2 H14E H -0.1431 0.9683 0.8925 0.112 Uiso 0.444(4) 1 calc PR A 2 H14F H -0.0639 1.0540 0.8684 0.112 Uiso 0.444(4) 1 calc PR A 2 C16 C 0.5026(5) 0.5346(4) 0.8444(2) 0.0209(13) Uani 1 1 d . . . C17 C 0.4135(5) 0.5027(4) 0.8039(2) 0.0249(14) Uani 1 1 d . . . H17 H 0.3351 0.5436 0.7894 0.030 Uiso 1 1 calc R . . C18 C 0.4405(6) 0.4131(4) 0.7857(3) 0.0286(14) Uani 1 1 d . . . H18 H 0.3810 0.3918 0.7584 0.034 Uiso 1 1 calc R . . C19 C 0.5551(6) 0.3535(4) 0.8071(3) 0.0336(15) Uani 1 1 d . . . H19 H 0.5726 0.2911 0.7951 0.040 Uiso 1 1 calc R . . C20 C 0.6450(6) 0.3842(4) 0.8462(3) 0.0309(15) Uani 1 1 d . . . H20 H 0.7244 0.3437 0.8595 0.037 Uiso 1 1 calc R . . C21 C 0.6171(5) 0.4744(4) 0.8652(3) 0.0235(13) Uani 1 1 d . . . H21 H 0.6767 0.4952 0.8927 0.028 Uiso 1 1 calc R . . C22 C 0.3092(5) 0.6442(4) 0.9229(2) 0.0195(13) Uani 1 1 d . . . C23 C 0.2604(5) 0.5599(4) 0.9381(2) 0.0265(14) Uani 1 1 d . . . H23 H 0.2975 0.5066 0.9168 0.032 Uiso 1 1 calc R . . C24 C 0.1582(5) 0.5516(4) 0.9838(3) 0.0294(15) Uani 1 1 d . . . H24 H 0.1271 0.4926 0.9943 0.035 Uiso 1 1 calc R . . C25 C 0.1022(5) 0.6286(5) 1.0138(3) 0.0334(16) Uani 1 1 d . . . H25 H 0.0316 0.6233 1.0448 0.040 Uiso 1 1 calc R . . C26 C 0.1485(5) 0.7131(4) 0.9989(3) 0.0336(15) Uani 1 1 d . . . H26 H 0.1087 0.7666 1.0194 0.040 Uiso 1 1 calc R . . C27 C 0.2532(5) 0.7219(4) 0.9542(3) 0.0303(15) Uani 1 1 d . . . H27 H 0.2860 0.7804 0.9452 0.036 Uiso 1 1 calc R . . C28 C 0.5783(5) 0.6711(4) 0.9269(2) 0.0229(13) Uani 1 1 d . . . C29 C 0.5583(5) 0.6616(4) 0.9958(3) 0.0270(14) Uani 1 1 d . . . H29 H 0.4828 0.6378 1.0148 0.032 Uiso 1 1 calc R . . C30 C 0.6488(6) 0.6869(4) 1.0370(3) 0.0347(16) Uani 1 1 d . . . H30 H 0.6348 0.6802 1.0840 0.042 Uiso 1 1 calc R . . C31 C 0.7574(6) 0.7213(5) 1.0102(3) 0.0399(17) Uani 1 1 d . . . H31 H 0.8172 0.7405 1.0385 0.048 Uiso 1 1 calc R . . C32 C 0.7808(6) 0.7284(5) 0.9424(3) 0.0396(17) Uani 1 1 d . . . H32 H 0.8583 0.7499 0.9240 0.048 Uiso 1 1 calc R . . C33 C 0.6910(6) 0.7040(4) 0.9009(3) 0.0344(16) Uani 1 1 d . . . H33 H 0.7068 0.7099 0.8540 0.041 Uiso 1 1 calc R . . C34 C 0.5174(5) 0.7122(4) 0.5055(2) 0.0212(13) Uani 1 1 d . . . C35 C 0.6161(5) 0.7574(4) 0.4735(3) 0.0237(13) Uani 1 1 d . . . H35 H 0.6884 0.7652 0.4989 0.028 Uiso 1 1 calc R . . C36 C 0.6131(6) 0.7913(4) 0.4061(3) 0.0264(14) Uani 1 1 d . . . H36 H 0.6829 0.8207 0.3855 0.032 Uiso 1 1 calc R . . C37 C 0.5069(6) 0.7816(4) 0.3694(3) 0.0268(14) Uani 1 1 d . . . H37 H 0.5031 0.8048 0.3231 0.032 Uiso 1 1 calc R . . C38 C 0.4056(6) 0.7382(4) 0.3997(3) 0.0324(15) Uani 1 1 d . . . H38 H 0.3319 0.7326 0.3743 0.039 Uiso 1 1 calc R . . C39 C 0.4121(5) 0.7027(4) 0.4675(3) 0.0247(13) Uani 1 1 d . . . H39 H 0.3434 0.6717 0.4878 0.030 Uiso 1 1 calc R . . C40 C 0.3850(5) 0.6128(4) 0.6136(2) 0.0172(12) Uani 1 1 d . . . C41 C 0.3811(5) 0.5270(4) 0.5893(3) 0.0247(14) Uani 1 1 d . . . H41 H 0.4489 0.5031 0.5602 0.030 Uiso 1 1 calc R . . C42 C 0.2793(6) 0.4765(4) 0.6071(3) 0.0277(14) Uani 1 1 d . . . H42 H 0.2779 0.4178 0.5906 0.033 Uiso 1 1 calc R . . C43 C 0.1795(5) 0.5112(4) 0.6490(3) 0.0285(14) Uani 1 1 d . . . H43 H 0.1095 0.4764 0.6612 0.034 Uiso 1 1 calc R . . C44 C 0.1819(5) 0.5958(4) 0.6727(3) 0.0256(14) Uani 1 1 d . . . H44 H 0.1130 0.6199 0.7012 0.031 Uiso 1 1 calc R . . C45 C 0.2837(5) 0.6461(4) 0.6557(2) 0.0212(13) Uani 1 1 d . . . H45 H 0.2846 0.7043 0.6729 0.025 Uiso 1 1 calc R . . C46 C 0.6572(5) 0.5742(3) 0.6043(2) 0.0183(12) Uani 1 1 d . . . C47 C 0.6525(5) 0.5030(4) 0.6588(3) 0.0217(13) Uani 1 1 d . . . H47 H 0.5792 0.5074 0.6886 0.026 Uiso 1 1 calc R . . C48 C 0.7534(5) 0.4262(4) 0.6698(2) 0.0205(13) Uani 1 1 d . . . H48 H 0.7485 0.3789 0.7070 0.025 Uiso 1 1 calc R . . C49 C 0.8603(5) 0.4183(4) 0.6272(3) 0.0271(14) Uani 1 1 d . . . H49 H 0.9294 0.3660 0.6348 0.032 Uiso 1 1 calc R . . C50 C 0.8654(6) 0.4869(4) 0.5737(3) 0.0363(16) Uani 1 1 d . . . H50 H 0.9384 0.4812 0.5437 0.044 Uiso 1 1 calc R . . C51 C 0.7663(5) 0.5645(4) 0.5623(3) 0.0261(14) Uani 1 1 d . . . H51 H 0.7733 0.6117 0.5252 0.031 Uiso 1 1 calc R . . C52 C 0.7591(5) 0.9300(4) 0.6960(2) 0.0229(13) Uani 1 1 d . . . C53 C 0.6739(6) 0.9697(4) 0.7432(3) 0.0341(15) Uani 1 1 d . . . H53 H 0.6005 0.9401 0.7586 0.041 Uiso 1 1 calc R . . C54 C 0.6935(7) 1.0508(5) 0.7681(3) 0.0492(19) Uani 1 1 d . . . H54 H 0.6325 1.0776 0.7993 0.059 Uiso 1 1 calc R . . C55 C 0.8004(8) 1.0930(5) 0.7480(4) 0.054(2) Uani 1 1 d . . . H55 H 0.8148 1.1482 0.7660 0.065 Uiso 1 1 calc R . . C56 C 0.8865(7) 1.0555(5) 0.7020(3) 0.049(2) Uani 1 1 d . . . H56 H 0.9598 1.0856 0.6875 0.059 Uiso 1 1 calc R . . C57 C 0.8680(6) 0.9736(4) 0.6762(3) 0.0319(15) Uani 1 1 d . . . H57 H 0.9296 0.9474 0.6450 0.038 Uiso 1 1 calc R . . C58 C 0.8324(5) 0.7312(4) 0.7288(2) 0.0195(13) Uani 1 1 d . . . C59 C 0.9208(5) 0.7557(4) 0.7718(2) 0.0232(13) Uani 1 1 d . . . H59 H 0.9312 0.8204 0.7704 0.028 Uiso 1 1 calc R . . C60 C 0.9929(5) 0.6881(4) 0.8163(3) 0.0260(14) Uani 1 1 d . . . H60 H 1.0520 0.7065 0.8453 0.031 Uiso 1 1 calc R . . C61 C 0.9802(5) 0.5922(4) 0.8191(3) 0.0257(14) Uani 1 1 d . . . H61 H 1.0299 0.5454 0.8499 0.031 Uiso 1 1 calc R . . C62 C 0.8945(5) 0.5668(4) 0.7766(2) 0.0236(13) Uani 1 1 d . . . H62 H 0.8858 0.5019 0.7775 0.028 Uiso 1 1 calc R . . C63 C 0.8207(5) 0.6358(4) 0.7324(2) 0.0208(13) Uani 1 1 d . . . H63 H 0.7607 0.6173 0.7039 0.025 Uiso 1 1 calc R . . C64 C 0.8364(5) 0.8179(4) 0.5920(2) 0.0196(13) Uani 1 1 d . . . C65 C 0.8129(5) 0.8946(4) 0.5409(3) 0.0274(14) Uani 1 1 d . . . H65 H 0.7444 0.9458 0.5462 0.033 Uiso 1 1 calc R . . C66 C 0.8880(6) 0.8967(4) 0.4830(3) 0.0364(16) Uani 1 1 d . . . H66 H 0.8720 0.9496 0.4491 0.044 Uiso 1 1 calc R . . C67 C 0.9866(6) 0.8216(4) 0.4744(3) 0.0389(16) Uani 1 1 d . . . H67 H 1.0382 0.8225 0.4345 0.047 Uiso 1 1 calc R . . C68 C 1.0092(6) 0.7459(4) 0.5236(3) 0.0376(16) Uani 1 1 d . . . H68 H 1.0769 0.6944 0.5177 0.045 Uiso 1 1 calc R . . C69 C 0.9342(5) 0.7435(4) 0.5826(3) 0.0284(14) Uani 1 1 d . . . H69 H 0.9508 0.6904 0.6163 0.034 Uiso 1 1 calc R . . C70 C 0.1768(6) 0.2302(4) 0.7630(3) 0.0343(15) Uani 1 1 d . . . F1 F 0.2947(3) 0.2108(3) 0.7910(2) 0.0561(11) Uani 1 1 d . . . F2 F 0.1513(3) 0.1518(2) 0.74257(16) 0.0426(9) Uani 1 1 d . . . F3 F 0.1856(4) 0.2936(3) 0.70864(18) 0.0625(12) Uani 1 1 d . . . O1 O 0.4545(9) 1.0104(5) 0.9135(4) 0.054(3) Uani 0.556(4) 1 d P A 1 O1A O 0.0248(8) 0.9294(8) 0.8463(6) 0.071(4) Uani 0.444(4) 1 d PD A 2 O2 O -0.0655(4) 0.2948(3) 0.7811(2) 0.0448(11) Uani 1 1 d . . . O3 O 0.0969(4) 0.3621(3) 0.8360(2) 0.0432(11) Uani 1 1 d . . . O4 O 0.0545(4) 0.2035(3) 0.87528(17) 0.0322(10) Uani 1 1 d . . . P1 P 0.52541(13) 0.67743(10) 0.59625(6) 0.0179(3) Uani 1 1 d . . . P2 P 0.73116(14) 0.81815(10) 0.66793(7) 0.0201(3) Uani 1 1 d . . . P3 P 0.45672(13) 0.64955(10) 0.87133(7) 0.0201(3) Uani 1 1 d . . . Ru1 Ru 0.51142(4) 0.81129(3) 0.65111(2) 0.01667(15) Uani 1 1 d . . . S1 S 0.05105(14) 0.27855(10) 0.82042(7) 0.0254(4) Uani 1 1 d . . . C71 C -0.1551(14) 1.0616(7) 0.9372(10) 0.118(7) Uani 0.556(4) 1 d PD A 1 H71A H -0.1074 1.0910 0.8987 0.142 Uiso 0.556(4) 1 calc PR A 1 H71B H -0.1145 1.0747 0.9780 0.142 Uiso 0.556(4) 1 calc PR A 1 Cl1 Cl -0.3071(7) 1.1204(3) 0.9352(2) 0.116(2) Uani 0.556(4) 1 d PD A 1 Cl2 Cl -0.1231(7) 0.9457(4) 0.9361(3) 0.135(3) Uani 0.556(4) 1 d PD A 1 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 C6 0.013(3) 0.020(3) 0.026(3) 0.006(3) -0.007(3) 0.000(3) C1 0.032(3) 0.018(3) 0.015(3) 0.006(2) -0.001(3) -0.001(3) C2 0.029(3) 0.015(3) 0.020(3) 0.006(2) -0.005(3) -0.003(3) C3 0.023(3) 0.017(3) 0.021(3) 0.004(2) -0.003(3) 0.005(3) C4 0.019(3) 0.020(3) 0.030(3) 0.006(3) 0.001(3) 0.002(3) C5 0.022(3) 0.017(3) 0.024(3) 0.001(2) -0.006(3) -0.001(3) C7 0.009(3) 0.028(3) 0.022(3) 0.004(3) -0.002(2) -0.004(3) C8 0.029(4) 0.020(3) 0.018(3) 0.010(2) 0.003(3) -0.003(3) C9 0.031(4) 0.035(4) 0.028(3) -0.004(3) -0.005(3) 0.004(3) C10 0.046(5) 0.051(5) 0.066(5) -0.021(4) -0.018(4) 0.019(4) C11 0.073(6) 0.022(4) 0.053(5) 0.000(3) -0.013(4) 0.024(4) C12 0.084(6) 0.034(4) 0.031(4) -0.001(3) -0.006(4) -0.011(4) C13 0.038(4) 0.035(4) 0.028(4) 0.005(3) -0.007(3) -0.013(3) C14 0.184(18) 0.018(7) 0.060(9) -0.025(7) -0.036(10) 0.024(9) C14A 0.054(12) 0.099(16) 0.058(12) 0.040(12) -0.030(10) -0.006(12) C16 0.017(3) 0.025(3) 0.019(3) 0.007(2) 0.007(2) -0.010(3) C17 0.023(3) 0.029(4) 0.020(3) 0.008(3) 0.006(3) -0.008(3) C18 0.036(4) 0.030(4) 0.021(3) 0.004(3) 0.002(3) -0.015(3) C19 0.044(4) 0.026(4) 0.028(4) 0.003(3) 0.016(3) -0.007(3) C20 0.032(4) 0.030(4) 0.024(3) 0.008(3) 0.010(3) 0.003(3) C21 0.019(3) 0.029(4) 0.021(3) 0.006(3) 0.002(2) -0.007(3) C22 0.014(3) 0.029(3) 0.012(3) 0.008(2) 0.000(2) -0.003(3) C23 0.022(3) 0.037(4) 0.017(3) 0.006(3) 0.001(3) -0.004(3) C24 0.015(3) 0.046(4) 0.026(3) 0.009(3) 0.000(3) -0.010(3) C25 0.007(3) 0.064(5) 0.024(3) 0.008(3) 0.008(3) -0.006(3) C26 0.026(3) 0.046(4) 0.023(3) 0.007(3) 0.008(3) 0.003(3) C27 0.029(4) 0.031(4) 0.025(3) 0.007(3) 0.008(3) 0.001(3) C28 0.018(3) 0.032(3) 0.017(3) 0.000(2) 0.001(2) -0.001(3) C29 0.021(3) 0.036(4) 0.019(3) 0.005(3) 0.004(3) 0.002(3) C30 0.039(4) 0.049(4) 0.015(3) 0.005(3) -0.006(3) -0.009(3) C31 0.030(4) 0.067(5) 0.023(4) -0.005(3) -0.005(3) -0.007(4) C32 0.020(3) 0.072(5) 0.028(4) -0.006(3) 0.003(3) -0.014(3) C33 0.029(4) 0.058(4) 0.016(3) -0.006(3) 0.002(3) -0.006(3) C34 0.025(3) 0.021(3) 0.018(3) 0.001(2) 0.000(3) -0.006(3) C35 0.032(3) 0.018(3) 0.023(3) -0.004(2) -0.004(3) -0.006(3) C36 0.039(4) 0.021(3) 0.018(3) -0.003(2) 0.009(3) -0.005(3) C37 0.041(4) 0.020(3) 0.018(3) 0.002(2) 0.000(3) -0.003(3) C38 0.042(4) 0.029(4) 0.028(4) -0.004(3) -0.011(3) -0.008(3) C39 0.026(3) 0.023(3) 0.025(3) 0.001(3) -0.004(3) -0.004(3) C40 0.015(3) 0.020(3) 0.018(3) 0.001(2) -0.005(2) -0.007(2) C41 0.020(3) 0.031(4) 0.022(3) 0.000(3) -0.004(2) -0.002(3) C42 0.034(4) 0.023(3) 0.026(3) 0.003(3) -0.006(3) -0.010(3) C43 0.020(3) 0.035(4) 0.030(3) 0.009(3) -0.004(3) -0.013(3) C44 0.018(3) 0.028(4) 0.028(3) 0.006(3) 0.001(3) -0.003(3) C45 0.023(3) 0.020(3) 0.020(3) 0.004(2) -0.004(3) -0.007(3) C46 0.020(3) 0.019(3) 0.016(3) 0.001(2) -0.004(2) -0.006(3) C47 0.020(3) 0.025(3) 0.020(3) -0.003(3) -0.001(2) -0.002(3) C48 0.027(3) 0.017(3) 0.019(3) 0.000(2) -0.002(3) -0.009(3) C49 0.022(3) 0.031(4) 0.029(3) -0.003(3) -0.002(3) -0.006(3) C50 0.022(3) 0.050(4) 0.031(4) -0.001(3) 0.010(3) 0.005(3) C51 0.026(3) 0.037(4) 0.014(3) 0.004(3) 0.001(3) -0.006(3) C52 0.025(3) 0.023(3) 0.019(3) 0.009(2) -0.005(3) -0.007(3) C53 0.034(4) 0.045(4) 0.026(3) -0.009(3) -0.004(3) -0.009(3) C54 0.047(5) 0.052(5) 0.051(5) -0.024(4) -0.011(4) 0.002(4) C55 0.082(6) 0.035(4) 0.047(5) -0.009(4) -0.028(4) -0.006(4) C56 0.073(5) 0.038(4) 0.041(4) 0.013(3) -0.020(4) -0.037(4) C57 0.039(4) 0.032(4) 0.026(3) 0.004(3) -0.008(3) -0.013(3) C58 0.013(3) 0.027(3) 0.017(3) 0.002(2) 0.006(2) -0.005(3) C59 0.019(3) 0.030(3) 0.022(3) 0.001(3) 0.002(3) -0.011(3) C60 0.019(3) 0.042(4) 0.016(3) -0.001(3) 0.000(2) -0.004(3) C61 0.021(3) 0.031(4) 0.023(3) 0.004(3) -0.002(3) -0.004(3) C62 0.024(3) 0.028(3) 0.019(3) 0.000(3) 0.004(3) -0.011(3) C63 0.013(3) 0.029(4) 0.021(3) 0.001(3) 0.001(2) -0.008(3) C64 0.014(3) 0.029(3) 0.018(3) -0.001(3) -0.002(2) -0.012(3) C65 0.022(3) 0.035(4) 0.024(3) 0.005(3) 0.001(3) -0.008(3) C66 0.040(4) 0.039(4) 0.027(4) 0.011(3) 0.006(3) -0.011(3) C67 0.039(4) 0.048(4) 0.027(4) 0.007(3) 0.017(3) -0.012(4) C68 0.028(4) 0.045(4) 0.035(4) 0.002(3) 0.011(3) 0.002(3) C69 0.023(3) 0.033(4) 0.026(3) 0.007(3) 0.004(3) -0.006(3) C70 0.037(4) 0.029(4) 0.039(4) -0.003(3) 0.010(3) -0.015(3) F1 0.021(2) 0.062(3) 0.088(3) -0.019(2) 0.009(2) -0.0088(19) F2 0.055(2) 0.032(2) 0.045(2) -0.0193(17) 0.0146(18) -0.0129(18) F3 0.093(3) 0.048(2) 0.048(2) -0.0032(19) 0.037(2) -0.025(2) O1 0.113(8) 0.017(4) 0.035(5) -0.014(4) -0.018(5) -0.006(5) O1A 0.040(8) 0.077(9) 0.095(10) -0.037(7) -0.010(7) 0.022(6) O2 0.028(2) 0.056(3) 0.047(3) -0.007(2) -0.013(2) 0.007(2) O3 0.061(3) 0.029(3) 0.041(3) -0.011(2) 0.006(2) -0.008(2) O4 0.042(3) 0.026(2) 0.024(2) 0.0045(18) 0.0026(19) 0.002(2) P1 0.0158(8) 0.0201(8) 0.0164(8) 0.0023(6) 0.0013(6) -0.0032(7) P2 0.0206(8) 0.0224(8) 0.0177(8) 0.0012(6) 0.0012(6) -0.0077(7) P3 0.0155(8) 0.0262(9) 0.0164(8) 0.0050(6) 0.0014(6) -0.0036(7) Ru1 0.0158(3) 0.0185(3) 0.0146(2) 0.00367(18) 0.00063(18) -0.0045(2) S1 0.0245(8) 0.0250(8) 0.0251(8) -0.0022(6) 0.0008(7) 0.0001(7) C71 0.121(18) 0.113(17) 0.130(18) -0.024(13) 0.026(14) -0.046(15) Cl1 0.214(6) 0.080(3) 0.059(3) -0.027(2) -0.021(3) -0.020(4) Cl2 0.196(7) 0.090(4) 0.120(5) -0.001(3) 0.047(4) -0.043(4) _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 C6 C7 1.372(7) . ? C6 Ru1 2.063(5) . ? C6 H6 0.92(5) . ? C1 C2 1.415(7) . ? C1 C5 1.423(7) . ? C1 Ru1 2.240(5) . ? C1 H1 1.0000 . ? C2 C3 1.424(7) . ? C2 Ru1 2.243(5) . ? C2 H2 1.0000 . ? C3 C4 1.406(7) . ? C3 Ru1 2.256(5) . ? C3 H3 1.0000 . ? C4 C5 1.406(7) . ? C4 Ru1 2.243(5) . ? C4 H4 1.0000 . ? C5 Ru1 2.236(5) . ? C5 H5 1.0000 . ? C7 C8 1.493(7) . ? C7 P3 1.791(5) . ? C8 C13 1.388(8) . ? C8 C9 1.401(8) . ? C9 C10 1.379(8) . ? C9 H9 0.9500 . ? C10 C11 1.400(9) . ? C10 O1A 1.438(5) . ? C10 H10 0.9500 . ? C11 C12 1.361(9) . ? C11 H11 0.9500 . ? C12 C13 1.403(9) . ? C12 O1 1.421(10) . ? C12 H12 0.9500 . ? C13 H13 0.9500 . ? C14 O1 1.402(13) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C14A O1A 1.421(5) . ? C14A H14D 0.9800 . ? C14A H14E 0.9800 . ? C14A H14F 0.9800 . ? C16 C21 1.388(7) . ? C16 C17 1.417(7) . ? C16 P3 1.796(5) . ? C17 C18 1.370(7) . ? C17 H17 0.9500 . ? C18 C19 1.389(8) . ? C18 H18 0.9500 . ? C19 C20 1.396(8) . ? C19 H19 0.9500 . ? C20 C21 1.386(7) . ? C20 H20 0.9500 . ? C21 H21 0.9500 . ? C22 C23 1.379(7) . ? C22 C27 1.393(7) . ? C22 P3 1.821(5) . ? C23 C24 1.388(7) . ? C23 H23 0.9500 . ? C24 C25 1.370(8) . ? C24 H24 0.9500 . ? C25 C26 1.370(8) . ? C25 H25 0.9500 . ? C26 C27 1.395(7) . ? C26 H26 0.9500 . ? C27 H27 0.9500 . ? C28 C33 1.387(7) . ? C28 C29 1.393(7) . ? C28 P3 1.800(5) . ? C29 C30 1.392(8) . ? C29 H29 0.9500 . ? C30 C31 1.364(8) . ? C30 H30 0.9500 . ? C31 C32 1.377(8) . ? C31 H31 0.9500 . ? C32 C33 1.385(8) . ? C32 H32 0.9500 . ? C33 H33 0.9500 . ? C34 C39 1.386(7) . ? C34 C35 1.390(7) . ? C34 P1 1.837(5) . ? C35 C36 1.383(7) . ? C35 H35 0.9500 . ? C36 C37 1.378(7) . ? C36 H36 0.9500 . ? C37 C38 1.386(8) . ? C37 H37 0.9500 . ? C38 C39 1.397(7) . ? C38 H38 0.9500 . ? C39 H39 0.9500 . ? C40 C45 1.390(7) . ? C40 C41 1.395(7) . ? C40 P1 1.844(5) . ? C41 C42 1.382(7) . ? C41 H41 0.9500 . ? C42 C43 1.383(8) . ? C42 H42 0.9500 . ? C43 C44 1.371(7) . ? C43 H43 0.9500 . ? C44 C45 1.377(7) . ? C44 H44 0.9500 . ? C45 H45 0.9500 . ? C46 C51 1.387(7) . ? C46 C47 1.405(7) . ? C46 P1 1.838(5) . ? C47 C48 1.390(7) . ? C47 H47 0.9500 . ? C48 C49 1.375(7) . ? C48 H48 0.9500 . ? C49 C50 1.369(7) . ? C49 H49 0.9500 . ? C50 C51 1.388(7) . ? C50 H50 0.9500 . ? C51 H51 0.9500 . ? C52 C53 1.390(7) . ? C52 C57 1.394(7) . ? C52 P2 1.843(5) . ? C53 C54 1.377(8) . ? C53 H53 0.9500 . ? C54 C55 1.367(9) . ? C54 H54 0.9500 . ? C55 C56 1.366(9) . ? C55 H55 0.9500 . ? C56 C57 1.392(8) . ? C56 H56 0.9500 . ? C57 H57 0.9500 . ? C58 C63 1.388(7) . ? C58 C59 1.396(7) . ? C58 P2 1.850(5) . ? C59 C60 1.373(7) . ? C59 H59 0.9500 . ? C60 C61 1.399(7) . ? C60 H60 0.9500 . ? C61 C62 1.375(7) . ? C61 H61 0.9500 . ? C62 C63 1.388(7) . ? C62 H62 0.9500 . ? C63 H63 0.9500 . ? C64 C69 1.376(7) . ? C64 C65 1.402(7) . ? C64 P2 1.850(5) . ? C65 C66 1.381(7) . ? C65 H65 0.9500 . ? C66 C67 1.384(8) . ? C66 H66 0.9500 . ? C67 C68 1.369(8) . ? C67 H67 0.9500 . ? C68 C69 1.399(7) . ? C68 H68 0.9500 . ? C69 H69 0.9500 . ? C70 F2 1.318(6) . ? C70 F1 1.331(7) . ? C70 F3 1.342(6) . ? C70 S1 1.827(6) . ? O2 S1 1.433(4) . ? O3 S1 1.434(4) . ? O4 S1 1.437(4) . ? P1 Ru1 2.3288(15) . ? P2 Ru1 2.3232(15) . ? C71 Cl2 1.648(9) . ? C71 Cl1 1.657(10) . ? C71 H71A 0.9900 . ? C71 H71B 0.9900 . ? 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 C7 C6 Ru1 133.6(4) . . ? C7 C6 H6 109(3) . . ? Ru1 C6 H6 117(3) . . ? C2 C1 C5 107.6(5) . . ? C2 C1 Ru1 71.7(3) . . ? C5 C1 Ru1 71.3(3) . . ? C2 C1 H1 126.1 . . ? C5 C1 H1 126.1 . . ? Ru1 C1 H1 126.1 . . ? C1 C2 C3 108.3(5) . . ? C1 C2 Ru1 71.5(3) . . ? C3 C2 Ru1 72.1(3) . . ? C1 C2 H2 125.8 . . ? C3 C2 H2 125.8 . . ? Ru1 C2 H2 125.8 . . ? C4 C3 C2 107.2(5) . . ? C4 C3 Ru1 71.3(3) . . ? C2 C3 Ru1 71.0(3) . . ? C4 C3 H3 126.3 . . ? C2 C3 H3 126.3 . . ? Ru1 C3 H3 126.3 . . ? C5 C4 C3 109.2(5) . . ? C5 C4 Ru1 71.5(3) . . ? C3 C4 Ru1 72.3(3) . . ? C5 C4 H4 125.3 . . ? C3 C4 H4 125.3 . . ? Ru1 C4 H4 125.3 . . ? C4 C5 C1 107.7(5) . . ? C4 C5 Ru1 72.0(3) . . ? C1 C5 Ru1 71.6(3) . . ? C4 C5 H5 126.1 . . ? C1 C5 H5 126.1 . . ? Ru1 C5 H5 126.1 . . ? C6 C7 C8 127.8(5) . . ? C6 C7 P3 121.3(4) . . ? C8 C7 P3 110.6(4) . . ? C13 C8 C9 118.3(5) . . ? C13 C8 C7 120.5(5) . . ? C9 C8 C7 120.9(5) . . ? C10 C9 C8 122.0(6) . . ? C10 C9 H9 119.0 . . ? C8 C9 H9 119.0 . . ? C9 C10 C11 117.9(6) . . ? C9 C10 O1A 113.3(7) . . ? C11 C10 O1A 125.9(7) . . ? C9 C10 H10 121.0 . . ? C11 C10 H10 121.0 . . ? O1A C10 H10 17.9 . . ? C12 C11 C10 121.7(6) . . ? C12 C11 H11 119.2 . . ? C10 C11 H11 119.2 . . ? C11 C12 C13 119.7(7) . . ? C11 C12 O1 133.2(7) . . ? C13 C12 O1 107.1(7) . . ? C11 C12 H12 120.2 . . ? C13 C12 H12 120.2 . . ? O1 C12 H12 13.3 . . ? C8 C13 C12 120.4(6) . . ? C8 C13 H13 119.8 . . ? C12 C13 H13 119.8 . . ? O1A C14A H14D 109.5 . . ? O1A C14A H14E 109.5 . . ? H14D C14A H14E 109.5 . . ? O1A C14A H14F 109.5 . . ? H14D C14A H14F 109.5 . . ? H14E C14A H14F 109.5 . . ? C21 C16 C17 119.5(5) . . ? C21 C16 P3 122.4(4) . . ? C17 C16 P3 118.0(4) . . ? C18 C17 C16 120.0(5) . . ? C18 C17 H17 120.0 . . ? C16 C17 H17 120.0 . . ? C17 C18 C19 119.9(6) . . ? C17 C18 H18 120.1 . . ? C19 C18 H18 120.1 . . ? C18 C19 C20 120.9(6) . . ? C18 C19 H19 119.5 . . ? C20 C19 H19 119.5 . . ? C21 C20 C19 119.2(6) . . ? C21 C20 H20 120.4 . . ? C19 C20 H20 120.4 . . ? C20 C21 C16 120.4(5) . . ? C20 C21 H21 119.8 . . ? C16 C21 H21 119.8 . . ? C23 C22 C27 118.6(5) . . ? C23 C22 P3 120.6(4) . . ? C27 C22 P3 120.4(4) . . ? C22 C23 C24 121.3(6) . . ? C22 C23 H23 119.3 . . ? C24 C23 H23 119.3 . . ? C25 C24 C23 119.9(6) . . ? C25 C24 H24 120.0 . . ? C23 C24 H24 120.0 . . ? C26 C25 C24 119.6(5) . . ? C26 C25 H25 120.2 . . ? C24 C25 H25 120.2 . . ? C25 C26 C27 121.1(6) . . ? C25 C26 H26 119.5 . . ? C27 C26 H26 119.5 . . ? C22 C27 C26 119.5(6) . . ? C22 C27 H27 120.3 . . ? C26 C27 H27 120.3 . . ? C33 C28 C29 118.5(5) . . ? C33 C28 P3 119.8(4) . . ? C29 C28 P3 121.6(4) . . ? C30 C29 C28 120.2(5) . . ? C30 C29 H29 119.9 . . ? C28 C29 H29 119.9 . . ? C31 C30 C29 120.3(5) . . ? C31 C30 H30 119.8 . . ? C29 C30 H30 119.8 . . ? C30 C31 C32 120.2(6) . . ? C30 C31 H31 119.9 . . ? C32 C31 H31 119.9 . . ? C31 C32 C33 119.9(6) . . ? C31 C32 H32 120.0 . . ? C33 C32 H32 120.0 . . ? C32 C33 C28 120.8(5) . . ? C32 C33 H33 119.6 . . ? C28 C33 H33 119.6 . . ? C39 C34 C35 117.6(5) . . ? C39 C34 P1 123.2(4) . . ? C35 C34 P1 119.0(4) . . ? C36 C35 C34 122.6(5) . . ? C36 C35 H35 118.7 . . ? C34 C35 H35 118.7 . . ? C37 C36 C35 118.8(5) . . ? C37 C36 H36 120.6 . . ? C35 C36 H36 120.6 . . ? C36 C37 C38 120.4(5) . . ? C36 C37 H37 119.8 . . ? C38 C37 H37 119.8 . . ? C37 C38 C39 119.8(5) . . ? C37 C38 H38 120.1 . . ? C39 C38 H38 120.1 . . ? C34 C39 C38 120.8(5) . . ? C34 C39 H39 119.6 . . ? C38 C39 H39 119.6 . . ? C45 C40 C41 118.3(5) . . ? C45 C40 P1 119.9(4) . . ? C41 C40 P1 121.7(4) . . ? C42 C41 C40 120.5(5) . . ? C42 C41 H41 119.7 . . ? C40 C41 H41 119.7 . . ? C41 C42 C43 120.2(5) . . ? C41 C42 H42 119.9 . . ? C43 C42 H42 119.9 . . ? C44 C43 C42 119.8(5) . . ? C44 C43 H43 120.1 . . ? C42 C43 H43 120.1 . . ? C43 C44 C45 120.4(5) . . ? C43 C44 H44 119.8 . . ? C45 C44 H44 119.8 . . ? C44 C45 C40 120.9(5) . . ? C44 C45 H45 119.6 . . ? C40 C45 H45 119.6 . . ? C51 C46 C47 117.2(5) . . ? C51 C46 P1 124.2(4) . . ? C47 C46 P1 118.5(4) . . ? C48 C47 C46 121.1(5) . . ? C48 C47 H47 119.5 . . ? C46 C47 H47 119.5 . . ? C49 C48 C47 120.4(5) . . ? C49 C48 H48 119.8 . . ? C47 C48 H48 119.8 . . ? C50 C49 C48 119.0(5) . . ? C50 C49 H49 120.5 . . ? C48 C49 H49 120.5 . . ? C49 C50 C51 121.3(5) . . ? C49 C50 H50 119.3 . . ? C51 C50 H50 119.3 . . ? C46 C51 C50 120.9(5) . . ? C46 C51 H51 119.6 . . ? C50 C51 H51 119.6 . . ? C53 C52 C57 117.7(5) . . ? C53 C52 P2 119.0(4) . . ? C57 C52 P2 123.1(4) . . ? C54 C53 C52 121.4(6) . . ? C54 C53 H53 119.3 . . ? C52 C53 H53 119.3 . . ? C55 C54 C53 120.2(7) . . ? C55 C54 H54 119.9 . . ? C53 C54 H54 119.9 . . ? C56 C55 C54 119.8(6) . . ? C56 C55 H55 120.1 . . ? C54 C55 H55 120.1 . . ? C55 C56 C57 120.7(7) . . ? C55 C56 H56 119.6 . . ? C57 C56 H56 119.6 . . ? C56 C57 C52 120.1(6) . . ? C56 C57 H57 119.9 . . ? C52 C57 H57 119.9 . . ? C63 C58 C59 117.6(5) . . ? C63 C58 P2 118.6(4) . . ? C59 C58 P2 123.8(4) . . ? C60 C59 C58 121.2(5) . . ? C60 C59 H59 119.4 . . ? C58 C59 H59 119.4 . . ? C59 C60 C61 120.5(5) . . ? C59 C60 H60 119.7 . . ? C61 C60 H60 119.7 . . ? C62 C61 C60 119.0(5) . . ? C62 C61 H61 120.5 . . ? C60 C61 H61 120.5 . . ? C61 C62 C63 120.2(5) . . ? C61 C62 H62 119.9 . . ? C63 C62 H62 119.9 . . ? C58 C63 C62 121.6(5) . . ? C58 C63 H63 119.2 . . ? C62 C63 H63 119.2 . . ? C69 C64 C65 118.6(5) . . ? C69 C64 P2 122.3(4) . . ? C65 C64 P2 119.0(4) . . ? C66 C65 C64 120.9(6) . . ? C66 C65 H65 119.5 . . ? C64 C65 H65 119.5 . . ? C65 C66 C67 119.9(5) . . ? C65 C66 H66 120.1 . . ? C67 C66 H66 120.1 . . ? C68 C67 C66 119.6(5) . . ? C68 C67 H67 120.2 . . ? C66 C67 H67 120.2 . . ? C67 C68 C69 120.9(6) . . ? C67 C68 H68 119.5 . . ? C69 C68 H68 119.5 . . ? C64 C69 C68 120.1(5) . . ? C64 C69 H69 120.0 . . ? C68 C69 H69 120.0 . . ? F2 C70 F1 107.9(5) . . ? F2 C70 F3 107.4(5) . . ? F1 C70 F3 107.0(5) . . ? F2 C70 S1 112.5(4) . . ? F1 C70 S1 111.5(4) . . ? F3 C70 S1 110.2(4) . . ? C14 O1 C12 112.5(10) . . ? C14A O1A C10 120.6(11) . . ? C34 P1 C46 102.6(2) . . ? C34 P1 C40 102.9(2) . . ? C46 P1 C40 98.0(2) . . ? C34 P1 Ru1 110.33(17) . . ? C46 P1 Ru1 126.47(16) . . ? C40 P1 Ru1 113.62(17) . . ? C52 P2 C64 100.3(2) . . ? C52 P2 C58 100.1(2) . . ? C64 P2 C58 102.2(2) . . ? C52 P2 Ru1 113.73(18) . . ? C64 P2 Ru1 115.22(16) . . ? C58 P2 Ru1 122.16(17) . . ? C7 P3 C16 111.0(2) . . ? C7 P3 C28 109.0(2) . . ? C16 P3 C28 110.1(2) . . ? C7 P3 C22 115.1(2) . . ? C16 P3 C22 106.7(2) . . ? C28 P3 C22 104.8(2) . . ? C6 Ru1 C5 123.8(2) . . ? C6 Ru1 C1 158.8(2) . . ? C5 Ru1 C1 37.06(18) . . ? C6 Ru1 C2 136.9(2) . . ? C5 Ru1 C2 61.52(19) . . ? C1 Ru1 C2 36.80(18) . . ? C6 Ru1 C4 97.6(2) . . ? C5 Ru1 C4 36.59(18) . . ? C1 Ru1 C4 61.24(19) . . ? C2 Ru1 C4 61.05(19) . . ? C6 Ru1 C3 103.5(2) . . ? C5 Ru1 C3 61.36(19) . . ? C1 Ru1 C3 61.54(19) . . ? C2 Ru1 C3 36.89(18) . . ? C4 Ru1 C3 36.42(18) . . ? C6 Ru1 P2 91.12(15) . . ? C5 Ru1 P2 144.55(14) . . ? C1 Ru1 P2 107.50(14) . . ? C2 Ru1 P2 89.64(14) . . ? C4 Ru1 P2 144.78(15) . . ? C3 Ru1 P2 108.36(14) . . ? C6 Ru1 P1 89.43(17) . . ? C5 Ru1 P1 85.75(14) . . ? C1 Ru1 P1 96.38(14) . . ? C2 Ru1 P1 132.35(13) . . ? C4 Ru1 P1 112.10(15) . . ? C3 Ru1 P1 146.57(14) . . ? P2 Ru1 P1 101.98(5) . . ? O2 S1 O3 115.8(3) . . ? O2 S1 O4 114.7(3) . . ? O3 S1 O4 114.5(2) . . ? O2 S1 C70 102.5(3) . . ? O3 S1 C70 103.4(3) . . ? O4 S1 C70 103.3(2) . . ? Cl2 C71 Cl1 122.2(12) . . ? Cl2 C71 H71A 106.8 . . ? Cl1 C71 H71A 106.8 . . ? Cl2 C71 H71B 106.8 . . ? Cl1 C71 H71B 106.8 . . ? H71A C71 H71B 106.6 . . ? 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 C5 C1 C2 C3 -0.5(6) . . . . ? Ru1 C1 C2 C3 -63.1(3) . . . . ? C5 C1 C2 Ru1 62.7(3) . . . . ? C1 C2 C3 C4 0.3(6) . . . . ? Ru1 C2 C3 C4 -62.5(3) . . . . ? C1 C2 C3 Ru1 62.8(4) . . . . ? C2 C3 C4 C5 0.0(6) . . . . ? Ru1 C3 C4 C5 -62.3(4) . . . . ? C2 C3 C4 Ru1 62.3(3) . . . . ? C3 C4 C5 C1 -0.3(6) . . . . ? Ru1 C4 C5 C1 -63.1(3) . . . . ? C3 C4 C5 Ru1 62.9(4) . . . . ? C2 C1 C5 C4 0.5(6) . . . . ? Ru1 C1 C5 C4 63.4(4) . . . . ? C2 C1 C5 Ru1 -62.9(3) . . . . ? Ru1 C6 C7 C8 -5.1(9) . . . . ? Ru1 C6 C7 P3 -178.3(3) . . . . ? C6 C7 C8 C13 -95.4(7) . . . . ? P3 C7 C8 C13 78.4(5) . . . . ? C6 C7 C8 C9 91.9(7) . . . . ? P3 C7 C8 C9 -94.3(5) . . . . ? C13 C8 C9 C10 -1.1(8) . . . . ? C7 C8 C9 C10 171.9(5) . . . . ? C8 C9 C10 C11 3.2(10) . . . . ? C8 C9 C10 O1A -158.6(7) . . . . ? C9 C10 C11 C12 -3.3(11) . . . . ? O1A C10 C11 C12 155.9(9) . . . . ? C10 C11 C12 C13 1.2(10) . . . . ? C10 C11 C12 O1 -175.4(7) . . . . ? C9 C8 C13 C12 -1.2(8) . . . . ? C7 C8 C13 C12 -174.1(5) . . . . ? C11 C12 C13 C8 1.1(9) . . . . ? O1 C12 C13 C8 178.5(6) . . . . ? C21 C16 C17 C18 0.1(7) . . . . ? P3 C16 C17 C18 -175.9(4) . . . . ? C16 C17 C18 C19 0.2(7) . . . . ? C17 C18 C19 C20 -1.2(8) . . . . ? C18 C19 C20 C21 1.9(8) . . . . ? C19 C20 C21 C16 -1.6(7) . . . . ? C17 C16 C21 C20 0.6(7) . . . . ? P3 C16 C21 C20 176.4(4) . . . . ? C27 C22 C23 C24 -0.3(8) . . . . ? P3 C22 C23 C24 171.9(4) . . . . ? C22 C23 C24 C25 1.2(8) . . . . ? C23 C24 C25 C26 -0.6(8) . . . . ? C24 C25 C26 C27 -0.8(8) . . . . ? C23 C22 C27 C26 -1.1(8) . . . . ? P3 C22 C27 C26 -173.4(4) . . . . ? C25 C26 C27 C22 1.7(8) . . . . ? C33 C28 C29 C30 1.4(8) . . . . ? P3 C28 C29 C30 -174.2(4) . . . . ? C28 C29 C30 C31 0.1(9) . . . . ? C29 C30 C31 C32 -2.1(10) . . . . ? C30 C31 C32 C33 2.6(10) . . . . ? C31 C32 C33 C28 -1.0(10) . . . . ? C29 C28 C33 C32 -1.0(9) . . . . ? P3 C28 C33 C32 174.7(5) . . . . ? C39 C34 C35 C36 -0.8(8) . . . . ? P1 C34 C35 C36 -175.8(4) . . . . ? C34 C35 C36 C37 1.3(8) . . . . ? C35 C36 C37 C38 -0.3(8) . . . . ? C36 C37 C38 C39 -1.0(8) . . . . ? C35 C34 C39 C38 -0.5(8) . . . . ? P1 C34 C39 C38 174.2(4) . . . . ? C37 C38 C39 C34 1.4(8) . . . . ? C45 C40 C41 C42 -0.5(7) . . . . ? P1 C40 C41 C42 175.2(4) . . . . ? C40 C41 C42 C43 0.6(8) . . . . ? C41 C42 C43 C44 -0.1(8) . . . . ? C42 C43 C44 C45 -0.6(8) . . . . ? C43 C44 C45 C40 0.6(8) . . . . ? C41 C40 C45 C44 -0.1(7) . . . . ? P1 C40 C45 C44 -175.9(4) . . . . ? C51 C46 C47 C48 0.0(7) . . . . ? P1 C46 C47 C48 -176.0(4) . . . . ? C46 C47 C48 C49 -0.2(8) . . . . ? C47 C48 C49 C50 -0.3(8) . . . . ? C48 C49 C50 C51 1.0(9) . . . . ? C47 C46 C51 C50 0.7(8) . . . . ? P1 C46 C51 C50 176.5(4) . . . . ? C49 C50 C51 C46 -1.2(9) . . . . ? C57 C52 C53 C54 2.0(8) . . . . ? P2 C52 C53 C54 177.1(5) . . . . ? C52 C53 C54 C55 -1.8(9) . . . . ? C53 C54 C55 C56 1.4(10) . . . . ? C54 C55 C56 C57 -1.2(10) . . . . ? C55 C56 C57 C52 1.4(9) . . . . ? C53 C52 C57 C56 -1.8(8) . . . . ? P2 C52 C57 C56 -176.7(4) . . . . ? C63 C58 C59 C60 -0.3(7) . . . . ? P2 C58 C59 C60 179.7(4) . . . . ? C58 C59 C60 C61 0.5(8) . . . . ? C59 C60 C61 C62 0.2(8) . . . . ? C60 C61 C62 C63 -1.0(8) . . . . ? C59 C58 C63 C62 -0.5(7) . . . . ? P2 C58 C63 C62 179.5(4) . . . . ? C61 C62 C63 C58 1.2(8) . . . . ? C69 C64 C65 C66 -1.4(8) . . . . ? P2 C64 C65 C66 -179.1(4) . . . . ? C64 C65 C66 C67 1.1(9) . . . . ? C65 C66 C67 C68 -0.4(9) . . . . ? C66 C67 C68 C69 0.0(10) . . . . ? C65 C64 C69 C68 1.0(8) . . . . ? P2 C64 C69 C68 178.7(4) . . . . ? C67 C68 C69 C64 -0.3(9) . . . . ? C11 C12 O1 C14 -1.5(13) . . . . ? C13 C12 O1 C14 -178.4(8) . . . . ? C9 C10 O1A C14A 162.2(11) . . . . ? C11 C10 O1A C14A 2.1(17) . . . . ? C39 C34 P1 C46 111.4(5) . . . . ? C35 C34 P1 C46 -74.0(5) . . . . ? C39 C34 P1 C40 10.0(5) . . . . ? C35 C34 P1 C40 -175.4(4) . . . . ? C39 C34 P1 Ru1 -111.5(4) . . . . ? C35 C34 P1 Ru1 63.1(4) . . . . ? C51 C46 P1 C34 33.8(5) . . . . ? C47 C46 P1 C34 -150.4(4) . . . . ? C51 C46 P1 C40 139.0(5) . . . . ? C47 C46 P1 C40 -45.2(4) . . . . ? C51 C46 P1 Ru1 -93.6(5) . . . . ? C47 C46 P1 Ru1 82.2(4) . . . . ? C45 C40 P1 C34 -118.7(4) . . . . ? C41 C40 P1 C34 65.7(5) . . . . ? C45 C40 P1 C46 136.3(4) . . . . ? C41 C40 P1 C46 -39.3(4) . . . . ? C45 C40 P1 Ru1 0.6(4) . . . . ? C41 C40 P1 Ru1 -175.1(4) . . . . ? C53 C52 P2 C64 164.6(4) . . . . ? C57 C52 P2 C64 -20.5(5) . . . . ? C53 C52 P2 C58 -90.9(5) . . . . ? C57 C52 P2 C58 83.9(5) . . . . ? C53 C52 P2 Ru1 41.0(5) . . . . ? C57 C52 P2 Ru1 -144.1(4) . . . . ? C69 C64 P2 C52 124.3(4) . . . . ? C65 C64 P2 C52 -58.0(5) . . . . ? C69 C64 P2 C58 21.5(5) . . . . ? C65 C64 P2 C58 -160.8(4) . . . . ? C69 C64 P2 Ru1 -113.2(4) . . . . ? C65 C64 P2 Ru1 64.5(4) . . . . ? C63 C58 P2 C52 169.0(4) . . . . ? C59 C58 P2 C52 -11.0(5) . . . . ? C63 C58 P2 C64 -88.1(4) . . . . ? C59 C58 P2 C64 91.9(5) . . . . ? C63 C58 P2 Ru1 42.5(5) . . . . ? C59 C58 P2 Ru1 -137.5(4) . . . . ? C6 C7 P3 C16 -20.9(5) . . . . ? C8 C7 P3 C16 164.9(4) . . . . ? C6 C7 P3 C28 100.6(5) . . . . ? C8 C7 P3 C28 -73.7(4) . . . . ? C6 C7 P3 C22 -142.1(4) . . . . ? C8 C7 P3 C22 43.6(4) . . . . ? C21 C16 P3 C7 120.6(4) . . . . ? C17 C16 P3 C7 -63.5(4) . . . . ? C21 C16 P3 C28 -0.2(5) . . . . ? C17 C16 P3 C28 175.7(4) . . . . ? C21 C16 P3 C22 -113.4(4) . . . . ? C17 C16 P3 C22 62.5(4) . . . . ? C33 C28 P3 C7 -39.2(5) . . . . ? C29 C28 P3 C7 136.4(5) . . . . ? C33 C28 P3 C16 82.7(5) . . . . ? C29 C28 P3 C16 -101.7(5) . . . . ? C33 C28 P3 C22 -162.9(5) . . . . ? C29 C28 P3 C22 12.7(5) . . . . ? C23 C22 P3 C7 128.1(4) . . . . ? C27 C22 P3 C7 -59.8(5) . . . . ? C23 C22 P3 C16 4.5(5) . . . . ? C27 C22 P3 C16 176.7(4) . . . . ? C23 C22 P3 C28 -112.3(4) . . . . ? C27 C22 P3 C28 59.9(5) . . . . ? C7 C6 Ru1 C5 -64.8(6) . . . . ? C7 C6 Ru1 C1 -43.0(9) . . . . ? C7 C6 Ru1 C2 18.0(7) . . . . ? C7 C6 Ru1 C4 -37.1(6) . . . . ? C7 C6 Ru1 C3 -0.5(6) . . . . ? C7 C6 Ru1 P2 108.7(5) . . . . ? C7 C6 Ru1 P1 -149.3(5) . . . . ? C4 C5 Ru1 C6 50.7(4) . . . . ? C1 C5 Ru1 C6 167.1(3) . . . . ? C4 C5 Ru1 C1 -116.4(4) . . . . ? C4 C5 Ru1 C2 -78.9(3) . . . . ? C1 C5 Ru1 C2 37.5(3) . . . . ? C1 C5 Ru1 C4 116.4(4) . . . . ? C4 C5 Ru1 C3 -36.6(3) . . . . ? C1 C5 Ru1 C3 79.7(3) . . . . ? C4 C5 Ru1 P2 -118.1(3) . . . . ? C1 C5 Ru1 P2 -1.7(4) . . . . ? C4 C5 Ru1 P1 137.2(3) . . . . ? C1 C5 Ru1 P1 -106.5(3) . . . . ? C2 C1 Ru1 C6 85.8(6) . . . . ? C5 C1 Ru1 C6 -30.9(7) . . . . ? C2 C1 Ru1 C5 116.7(5) . . . . ? C5 C1 Ru1 C2 -116.7(5) . . . . ? C2 C1 Ru1 C4 79.1(3) . . . . ? C5 C1 Ru1 C4 -37.5(3) . . . . ? C2 C1 Ru1 C3 37.4(3) . . . . ? C5 C1 Ru1 C3 -79.2(3) . . . . ? C2 C1 Ru1 P2 -64.4(3) . . . . ? C5 C1 Ru1 P2 178.9(3) . . . . ? C2 C1 Ru1 P1 -169.1(3) . . . . ? C5 C1 Ru1 P1 74.2(3) . . . . ? C1 C2 Ru1 C6 -148.1(3) . . . . ? C3 C2 Ru1 C6 -31.0(4) . . . . ? C1 C2 Ru1 C5 -37.8(3) . . . . ? C3 C2 Ru1 C5 79.3(3) . . . . ? C3 C2 Ru1 C1 117.1(5) . . . . ? C1 C2 Ru1 C4 -79.7(3) . . . . ? C3 C2 Ru1 C4 37.4(3) . . . . ? C1 C2 Ru1 C3 -117.1(5) . . . . ? C1 C2 Ru1 P2 120.7(3) . . . . ? C3 C2 Ru1 P2 -122.2(3) . . . . ? C1 C2 Ru1 P1 14.7(4) . . . . ? C3 C2 Ru1 P1 131.8(3) . . . . ? C5 C4 Ru1 C6 -139.6(3) . . . . ? C3 C4 Ru1 C6 102.3(3) . . . . ? C3 C4 Ru1 C5 -118.1(4) . . . . ? C5 C4 Ru1 C1 38.0(3) . . . . ? C3 C4 Ru1 C1 -80.1(3) . . . . ? C5 C4 Ru1 C2 80.3(3) . . . . ? C3 C4 Ru1 C2 -37.9(3) . . . . ? C5 C4 Ru1 C3 118.1(4) . . . . ? C5 C4 Ru1 P2 117.5(3) . . . . ? C3 C4 Ru1 P2 -0.6(4) . . . . ? C5 C4 Ru1 P1 -47.0(3) . . . . ? C3 C4 Ru1 P1 -165.2(3) . . . . ? C4 C3 Ru1 C6 -84.6(3) . . . . ? C2 C3 Ru1 C6 158.8(3) . . . . ? C4 C3 Ru1 C5 36.8(3) . . . . ? C2 C3 Ru1 C5 -79.8(3) . . . . ? C4 C3 Ru1 C1 79.2(3) . . . . ? C2 C3 Ru1 C1 -37.3(3) . . . . ? C4 C3 Ru1 C2 116.6(4) . . . . ? C2 C3 Ru1 C4 -116.6(4) . . . . ? C4 C3 Ru1 P2 179.6(3) . . . . ? C2 C3 Ru1 P2 63.0(3) . . . . ? C4 C3 Ru1 P1 25.5(4) . . . . ? C2 C3 Ru1 P1 -91.1(4) . . . . ? C52 P2 Ru1 C6 -101.7(2) . . . . ? C64 P2 Ru1 C6 143.4(3) . . . . ? C58 P2 Ru1 C6 18.5(3) . . . . ? C52 P2 Ru1 C5 69.1(3) . . . . ? C64 P2 Ru1 C5 -45.9(3) . . . . ? C58 P2 Ru1 C5 -170.8(3) . . . . ? C52 P2 Ru1 C1 68.0(2) . . . . ? C64 P2 Ru1 C1 -47.0(2) . . . . ? C58 P2 Ru1 C1 -171.9(2) . . . . ? C52 P2 Ru1 C2 35.3(2) . . . . ? C64 P2 Ru1 C2 -79.7(2) . . . . ? C58 P2 Ru1 C2 155.5(2) . . . . ? C52 P2 Ru1 C4 3.3(3) . . . . ? C64 P2 Ru1 C4 -111.7(3) . . . . ? C58 P2 Ru1 C4 123.5(3) . . . . ? C52 P2 Ru1 C3 2.9(2) . . . . ? C64 P2 Ru1 C3 -112.0(2) . . . . ? C58 P2 Ru1 C3 123.1(2) . . . . ? C52 P2 Ru1 P1 168.69(18) . . . . ? C64 P2 Ru1 P1 53.7(2) . . . . ? C58 P2 Ru1 P1 -71.1(2) . . . . ? C34 P1 Ru1 C6 172.9(2) . . . . ? C46 P1 Ru1 C6 -62.9(2) . . . . ? C40 P1 Ru1 C6 58.0(2) . . . . ? C34 P1 Ru1 C5 48.9(2) . . . . ? C46 P1 Ru1 C5 173.2(2) . . . . ? C40 P1 Ru1 C5 -66.0(2) . . . . ? C34 P1 Ru1 C1 13.4(2) . . . . ? C46 P1 Ru1 C1 137.6(2) . . . . ? C40 P1 Ru1 C1 -101.6(2) . . . . ? C34 P1 Ru1 C2 4.6(3) . . . . ? C46 P1 Ru1 C2 128.8(3) . . . . ? C40 P1 Ru1 C2 -110.4(3) . . . . ? C34 P1 Ru1 C4 74.9(2) . . . . ? C46 P1 Ru1 C4 -160.9(2) . . . . ? C40 P1 Ru1 C4 -40.1(2) . . . . ? C34 P1 Ru1 C3 58.9(3) . . . . ? C46 P1 Ru1 C3 -176.9(3) . . . . ? C40 P1 Ru1 C3 -56.1(3) . . . . ? C34 P1 Ru1 P2 -96.06(18) . . . . ? C46 P1 Ru1 P2 28.2(2) . . . . ? C40 P1 Ru1 P2 148.99(17) . . . . ? F2 C70 S1 O2 -59.1(5) . . . . ? F1 C70 S1 O2 179.5(4) . . . . ? F3 C70 S1 O2 60.8(5) . . . . ? F2 C70 S1 O3 -179.8(4) . . . . ? F1 C70 S1 O3 58.8(4) . . . . ? F3 C70 S1 O3 -59.9(5) . . . . ? F2 C70 S1 O4 60.5(5) . . . . ? F1 C70 S1 O4 -60.9(4) . . . . ? F3 C70 S1 O4 -179.6(4) . . . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 22.61 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.675 _refine_diff_density_min -0.652 _refine_diff_density_rms 0.083 ###End