# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/2160 data_global # 1. SUBMISSION DETAILS _publ_contact_autor ; Dirk Walther Friedrich-Schiller-Universit\"at Jena Institut f\"ur Anorganische und Analytische Chemie August-Bebel-Str. 2 D-07743 Jena Germany ; _publ_contact_author_phone '03641 9-48110 ' _publ_contact_author_fax '03641 9-48102 ' _publ_requested_journal 'Dalton ' # 2. TITLE AND AUTHOR LIST _publ_section_title ; Bis (R-bipyridyl)ruthenium-bisbenzimidazole complexes (R: H, Me, t-But): Supramolecular arrangenment via hydrogen bonds, photo- and electrochemi- cal properties and reactivity towards carbon dioxide ; loop_ _publ_author_name _publ_author_address ' Walther, Dirk ' ; Friedrich-Schiller-Universit\"at Jena Institut f\"ur Anorganische und Analytische Chemie August-Bebel-Str. 2 D-07743 Jena Germany ; ' Ruben, Mario ' ; Friedrich-Schiller-Universit\"at Jena Institut f\"ur Anorganische und Analytische Chemie August-Bebel-Str. 2 D-07743 Jena Germany ; ' Rau, Sven ' ; Friedrich-Schiller-Universit\"at Jena Institut f\"ur Anorganische und Analytische Chemie August-Bebel-Str. 2 D-07743 Jena Germany ; ' B\"uttner, Torsten ' ; Friedrich-Schiller-Universit\"at Jena Institut f\"ur Anorganische und Analytische Chemie August-Bebel-Str. 2 D-07743 Jena Germany ; ' Temme, Christian ' ; Friedrich-Schiller-Universit\"at Jena Institut f\"ur Anorganische Chemie und Analytische Chemie August-Bebel-Str. 2 07743 Jena Germany ; ' Dautz, Sylvana ' ; Friedrich-Schiller-Universit\"at Jena Institut f\"ur Anorganische Chemie und Analytische Chemie August-Bebel-Str. 2 07743 Jena Germany ; ' Rudolph, Manfred ' ; Friedrich-Schiller-Universit\"at Jena Institut f\"ur Anorganische Chemie und Analytische Chemie August-Bebel-Str. 2 07743 Jena Germany ; ' Brodkorb, Andre ' ; Friedrich-Schiller-Universit\"at Jena Institut f\"ur Anorganische Chemie und Analytische Chemie August-Bebel-Str. 2 07743 Jena Germany ; ' G\"orls, Helmar ' ; Friedrich-Schiller-Universit\"at Jena Institut f\"ur Anorganische Chemie und Analytische Chemie August-Bebel-Str. 2 07743 Jena Germany ; ' OoConnor, Christine ' ; Dublin City University School of Chemical Sciences Glas Nevin Dublin 9 Ireland ; ' Duati, Marco ' ; Dublin City University School of Chemical Sciences Glas Nevin Dublin 9 Ireland ; ' Vos, Johan G. ' ; Dublin City University School of Chemical Sciences Glas Nevin Dublin 9 Ireland ; # data_FO637 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C44 H50 F12 N8 O4 P2 Ru' _chemical_formula_weight 1145.93 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' '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 C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 22.7551(5) _cell_length_b 23.9120(5) _cell_length_c 9.6410(3) _cell_angle_alpha 90.00 _cell_angle_beta 112.708(3) _cell_angle_gamma 90.00 _cell_volume 4839.2(2) _cell_formula_units_Z 4 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour dark-brown _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.573 _exptl_crystal_density_method ? _exptl_crystal_F_000 2336 _exptl_absorpt_coefficient_mu 0.488 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 183(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 KappaCCD _diffrn_measurement_method phi-scan _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6467 _diffrn_reflns_av_R_equivalents 0.0180 _diffrn_reflns_av_sigmaI/netI 0.0492 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 0 _diffrn_reflns_theta_min 3.03 _diffrn_reflns_theta_max 23.30 _reflns_number_total 3362 _reflns_number_observed 3075 _reflns_observed_criterion >2sigma(I) _computing_data_collection DENZO _computing_cell_refinement DENZO _computing_data_reduction DENZO _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics SHELXTL/PC _computing_publication_material SHELXL-93 _refine_special_details ; Refinement on F^2^ for ALL reflections except for 67 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0788P)^2^+10.5583P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom/difmap _refine_ls_hydrogen_treatment 'rigid-group /isotropically' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3295 _refine_ls_number_parameters 333 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0467 _refine_ls_R_factor_obs 0.0421 _refine_ls_wR_factor_all 0.1334 _refine_ls_wR_factor_obs 0.1233 _refine_ls_goodness_of_fit_all 1.040 _refine_ls_goodness_of_fit_obs 1.061 _refine_ls_restrained_S_all 1.093 _refine_ls_restrained_S_obs 1.061 _refine_ls_shift/esd_max 0.043 _refine_ls_shift/esd_mean 0.002 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Ru Ru 0.5000 0.29083(2) 0.7500 0.0271(2) Uani 1 d S . N1 N 0.46841(13) 0.35281(13) 0.5923(3) 0.0320(7) Uani 1 d . . N2 N 0.40525(14) 0.29413(12) 0.7147(3) 0.0305(7) Uani 1 d . . N3 N 0.47789(13) 0.22265(13) 0.6034(3) 0.0309(7) Uani 1 d . . N4 N 0.46856(14) 0.1305(2) 0.5677(4) 0.0376(7) Uani 1 d . . H1N4 H 0.4660(20) 0.0957(20) 0.5849(48) 0.044(13) Uiso 1 d . . C1 C 0.5043(2) 0.3819(2) 0.5332(4) 0.0389(9) Uani 1 d . . H1A H 0.5478(2) 0.3720(2) 0.5628(4) 0.047 Uiso 1 calc R . C2 C 0.4809(2) 0.4249(2) 0.4331(4) 0.0459(10) Uani 1 d . . H2A H 0.5080(2) 0.4436(2) 0.3939(4) 0.055 Uiso 1 calc R . C3 C 0.4173(2) 0.4413(2) 0.3885(5) 0.0469(10) Uani 1 d . . C4 C 0.3796(2) 0.4114(2) 0.4479(5) 0.0452(10) Uani 1 d . . H4B H 0.3360(2) 0.4207(2) 0.4192(5) 0.054 Uiso 1 calc R . C5 C 0.4060(2) 0.3679(2) 0.5490(4) 0.0356(8) Uani 1 d . . C6 C 0.3697(2) 0.3335(2) 0.6159(4) 0.0334(8) Uani 1 d . . C7 C 0.3048(2) 0.3387(2) 0.5800(4) 0.0411(9) Uani 1 d . . H7A H 0.2814(2) 0.3669(2) 0.5115(4) 0.049 Uiso 1 calc R . C8 C 0.2738(2) 0.3031(2) 0.6435(4) 0.0407(9) Uani 1 d . . C9 C 0.3103(2) 0.2630(2) 0.7425(4) 0.0393(9) Uani 1 d . . H9A H 0.2910(2) 0.2378(2) 0.7882(4) 0.047 Uiso 1 calc R . C10 C 0.3749(2) 0.2596(2) 0.7753(4) 0.0355(8) Uani 1 d . . H10A H 0.3989(2) 0.2316(2) 0.8436(4) 0.043 Uiso 1 calc R . C11 C 0.3901(3) 0.4888(2) 0.2776(6) 0.0682(14) Uani 1 d . . H11A H 0.4237(3) 0.5046(2) 0.2495(6) 0.102 Uiso 1 calc R . H11B H 0.3735(3) 0.5179(2) 0.3241(6) 0.102 Uiso 1 calc R . H11C H 0.3556(3) 0.4745(2) 0.1876(6) 0.102 Uiso 1 calc R . C12 C 0.2034(2) 0.3077(2) 0.6056(5) 0.0533(11) Uani 1 d . . H12A H 0.1857(2) 0.3383(2) 0.5340(5) 0.080 Uiso 1 calc R . H12B H 0.1959(2) 0.3151(2) 0.6974(5) 0.080 Uiso 1 calc R . H12C H 0.1826(2) 0.2725(2) 0.5607(5) 0.080 Uiso 1 calc R . C13 C 0.4536(2) 0.21262(15) 0.4502(4) 0.0318(8) Uani 1 d . . C14 C 0.4359(2) 0.2495(2) 0.3289(4) 0.0391(9) Uani 1 d . . H14A H 0.4397(2) 0.2888(2) 0.3437(4) 0.047 Uiso 1 calc R . C15 C 0.4124(2) 0.2264(2) 0.1855(4) 0.0467(10) Uani 1 d . . H15A H 0.3999(2) 0.2504(2) 0.1004(4) 0.056 Uiso 1 calc R . C16 C 0.4070(2) 0.1685(2) 0.1646(4) 0.0487(11) Uani 1 d . . H16A H 0.3909(2) 0.1542(2) 0.0649(4) 0.058 Uiso 1 calc R . C17 C 0.4242(2) 0.1314(2) 0.2828(5) 0.0468(10) Uani 1 d . . H17A H 0.4202(2) 0.0921(2) 0.2673(5) 0.056 Uiso 1 calc R . C18 C 0.4478(2) 0.1548(2) 0.4268(4) 0.0366(9) Uani 1 d . . C19 C 0.4867(2) 0.1724(2) 0.6688(4) 0.0322(8) Uani 1 d . . P P 0.16233(5) 0.43646(5) 0.24173(12) 0.0446(3) Uani 1 d . . F1 F 0.1407(2) 0.49886(13) 0.2413(4) 0.0849(10) Uani 1 d . . F2 F 0.1838(2) 0.37353(12) 0.2406(3) 0.0833(10) Uani 1 d . . F3 F 0.1426(2) 0.43940(14) 0.0655(3) 0.0874(10) Uani 1 d . . F4 F 0.0931(2) 0.4176(2) 0.2135(6) 0.1141(14) Uani 1 d . . F5 F 0.1834(3) 0.4342(2) 0.4151(4) 0.145(2) Uani 1 d . . F6 F 0.2317(2) 0.4556(2) 0.2629(7) 0.136(2) Uani 1 d . . O1 O 0.6338(2) 0.3767(2) 0.4719(6) 0.107(2) Uani 1 d . . C20 C 0.7344(3) 0.4214(3) 0.5866(9) 0.099(2) Uani 1 d . . H20A H 0.7111(3) 0.4476(3) 0.6249(9) 0.148 Uiso 1 calc R . H20B H 0.7523(3) 0.4417(3) 0.5235(9) 0.148 Uiso 1 calc R . H20C H 0.7690(3) 0.4041(3) 0.6712(9) 0.148 Uiso 1 calc R . C21 C 0.6901(3) 0.3771(2) 0.4953(7) 0.0712(14) Uani 1 d . . C22 C 0.7185(3) 0.3342(3) 0.4311(8) 0.083(2) Uani 1 d . . H22A H 0.6858(3) 0.3071(3) 0.3743(8) 0.125 Uiso 1 calc R . H22B H 0.7527(3) 0.3150(3) 0.5124(8) 0.125 Uiso 1 calc R . H22C H 0.7361(3) 0.3520(3) 0.3639(8) 0.125 Uiso 1 calc R . O2 O 0.4694(2) 0.01346(14) 0.5954(4) 0.0471(8) Uani 1 d . . H2O2 H 0.4399(27) 0.0030(22) 0.5699(60) 0.046(18) Uiso 1 d . . H1O2 H 0.4735(44) -0.0031(43) 0.5315(116) 0.155(43) Uiso 1 d . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru 0.0190(3) 0.0360(3) 0.0248(3) 0.000 0.0069(2) 0.000 N1 0.0235(15) 0.043(2) 0.029(2) -0.0035(13) 0.0086(12) -0.0024(12) N2 0.025(2) 0.039(2) 0.027(2) -0.0012(12) 0.0096(13) -0.0008(12) N3 0.0196(15) 0.042(2) 0.031(2) -0.0004(13) 0.0096(13) -0.0013(12) N4 0.028(2) 0.038(2) 0.044(2) -0.0036(15) 0.0105(14) -0.0014(13) C1 0.027(2) 0.051(2) 0.039(2) 0.002(2) 0.013(2) -0.004(2) C2 0.044(2) 0.055(3) 0.040(2) 0.010(2) 0.017(2) -0.008(2) C3 0.048(2) 0.048(3) 0.040(2) 0.008(2) 0.012(2) 0.000(2) C4 0.035(2) 0.053(3) 0.044(2) 0.009(2) 0.012(2) 0.006(2) C5 0.028(2) 0.043(2) 0.032(2) 0.002(2) 0.008(2) -0.001(2) C6 0.026(2) 0.043(2) 0.030(2) 0.002(2) 0.010(2) 0.000(2) C7 0.025(2) 0.055(3) 0.040(2) 0.006(2) 0.010(2) 0.005(2) C8 0.025(2) 0.059(3) 0.038(2) -0.004(2) 0.012(2) -0.002(2) C9 0.029(2) 0.052(3) 0.040(2) 0.001(2) 0.016(2) -0.007(2) C10 0.029(2) 0.046(2) 0.031(2) 0.001(2) 0.011(2) 0.000(2) C11 0.065(3) 0.060(3) 0.070(3) 0.022(3) 0.015(3) 0.004(2) C12 0.026(2) 0.080(3) 0.056(3) 0.000(2) 0.017(2) -0.002(2) C13 0.019(2) 0.046(2) 0.030(2) -0.0072(15) 0.0091(15) -0.0018(14) C14 0.030(2) 0.051(2) 0.036(2) -0.003(2) 0.013(2) -0.002(2) C15 0.039(2) 0.069(3) 0.031(2) -0.003(2) 0.013(2) -0.003(2) C16 0.035(2) 0.078(3) 0.032(2) -0.016(2) 0.011(2) -0.004(2) C17 0.032(2) 0.059(3) 0.049(2) -0.022(2) 0.015(2) -0.003(2) C18 0.024(2) 0.049(2) 0.036(2) -0.007(2) 0.011(2) -0.002(2) C19 0.022(2) 0.040(2) 0.034(2) -0.005(2) 0.0092(14) -0.0019(14) P 0.0346(6) 0.0460(7) 0.0456(6) -0.0022(5) 0.0072(5) 0.0055(4) F1 0.081(2) 0.061(2) 0.088(2) -0.0146(15) 0.005(2) 0.026(2) F2 0.114(3) 0.052(2) 0.074(2) 0.0034(14) 0.026(2) 0.029(2) F3 0.122(3) 0.083(2) 0.058(2) 0.011(2) 0.035(2) 0.033(2) F4 0.069(2) 0.121(3) 0.170(4) -0.004(3) 0.066(3) -0.025(2) F5 0.222(5) 0.131(4) 0.043(2) -0.003(2) 0.009(2) 0.094(4) F6 0.046(2) 0.113(3) 0.232(6) -0.031(3) 0.036(3) -0.013(2) O1 0.056(3) 0.125(4) 0.153(4) 0.012(3) 0.056(3) 0.001(2) C20 0.095(5) 0.085(5) 0.119(5) -0.027(4) 0.043(4) -0.018(4) C21 0.064(3) 0.077(4) 0.081(4) 0.010(3) 0.037(3) -0.001(3) C22 0.068(4) 0.089(4) 0.100(4) -0.014(3) 0.038(3) -0.009(3) O2 0.044(2) 0.050(2) 0.044(2) -0.0088(14) 0.013(2) -0.006(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru N1 2.045(3) 2_656 ? Ru N1 2.045(3) . ? Ru N2 2.051(3) 2_656 ? Ru N2 2.051(3) . ? Ru N3 2.088(3) . ? Ru N3 2.088(3) 2_656 ? N1 C1 1.354(5) . ? N1 C5 1.365(5) . ? N2 C10 1.347(5) . ? N2 C6 1.360(5) . ? N3 C19 1.337(5) . ? N3 C13 1.384(5) . ? N4 C19 1.346(5) . ? N4 C18 1.382(5) . ? C1 C2 1.369(6) . ? C2 C3 1.396(6) . ? C3 C4 1.398(6) . ? C3 C11 1.517(6) . ? C4 C5 1.394(5) . ? C5 C6 1.477(5) . ? C6 C7 1.387(5) . ? C7 C8 1.390(6) . ? C8 C9 1.382(6) . ? C8 C12 1.503(5) . ? C9 C10 1.381(5) . ? C13 C14 1.394(5) . ? C13 C18 1.399(5) . ? C14 C15 1.389(6) . ? C15 C16 1.398(6) . ? C16 C17 1.377(6) . ? C17 C18 1.397(5) . ? C19 C19 1.443(7) 2_656 ? P F5 1.552(4) . ? P F4 1.559(3) . ? P F1 1.570(3) . ? P F2 1.584(3) . ? P F3 1.582(3) . ? P F6 1.579(4) . ? O1 C21 1.210(7) . ? C20 C21 1.495(8) . ? C21 C22 1.470(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ru N1 87.1(2) 2_656 . ? N1 Ru N2 78.66(11) 2_656 2_656 ? N1 Ru N2 98.10(11) . 2_656 ? N1 Ru N2 98.10(11) 2_656 . ? N1 Ru N2 78.66(11) . . ? N2 Ru N2 175.6(2) 2_656 . ? N1 Ru N3 173.19(11) 2_656 . ? N1 Ru N3 97.99(12) . . ? N2 Ru N3 96.06(11) 2_656 . ? N2 Ru N3 87.40(11) . . ? N1 Ru N3 97.99(12) 2_656 2_656 ? N1 Ru N3 173.19(11) . 2_656 ? N2 Ru N3 87.40(11) 2_656 2_656 ? N2 Ru N3 96.06(11) . 2_656 ? N3 Ru N3 77.3(2) . 2_656 ? C1 N1 C5 117.4(3) . . ? C1 N1 Ru 126.1(2) . . ? C5 N1 Ru 116.4(2) . . ? C10 N2 C6 117.6(3) . . ? C10 N2 Ru 125.9(2) . . ? C6 N2 Ru 116.4(2) . . ? C19 N3 C13 105.9(3) . . ? C19 N3 Ru 115.5(2) . . ? C13 N3 Ru 138.6(2) . . ? C19 N4 C18 107.0(3) . . ? C2 C1 N1 123.3(3) . . ? C1 C2 C3 120.2(4) . . ? C4 C3 C2 117.1(4) . . ? C4 C3 C11 121.6(4) . . ? C2 C3 C11 121.3(4) . . ? C5 C4 C3 120.2(4) . . ? N1 C5 C4 121.8(3) . . ? N1 C5 C6 114.2(3) . . ? C4 C5 C6 124.0(3) . . ? N2 C6 C7 121.6(3) . . ? N2 C6 C5 114.2(3) . . ? C7 C6 C5 124.1(3) . . ? C6 C7 C8 120.6(4) . . ? C9 C8 C7 117.1(3) . . ? C9 C8 C12 121.2(4) . . ? C7 C8 C12 121.6(4) . . ? C8 C9 C10 120.2(3) . . ? N2 C10 C9 122.8(3) . . ? N3 C13 C14 130.8(3) . . ? N3 C13 C18 108.5(3) . . ? C14 C13 C18 120.8(3) . . ? C13 C14 C15 117.3(4) . . ? C14 C15 C16 121.0(4) . . ? C17 C16 C15 122.5(4) . . ? C16 C17 C18 116.3(4) . . ? N4 C18 C17 131.6(4) . . ? N4 C18 C13 106.4(3) . . ? C17 C18 C13 122.1(4) . . ? N3 C19 N4 112.3(3) . . ? N3 C19 C19 115.8(2) . 2_656 ? N4 C19 C19 131.9(2) . 2_656 ? F5 P F4 92.8(3) . . ? F5 P F1 90.1(2) . . ? F4 P F1 88.9(2) . . ? F5 P F2 90.4(2) . . ? F4 P F2 91.0(2) . . ? F1 P F2 179.5(2) . . ? F5 P F3 178.5(3) . . ? F4 P F3 88.6(2) . . ? F1 P F3 89.8(2) . . ? F2 P F3 89.7(2) . . ? F5 P F6 89.6(3) . . ? F4 P F6 177.6(3) . . ? F1 P F6 91.2(2) . . ? F2 P F6 88.9(2) . . ? F3 P F6 88.9(3) . . ? O1 C21 C22 121.5(6) . . ? O1 C21 C20 122.7(6) . . ? C22 C21 C20 115.8(5) . . ? _refine_diff_density_max 0.884 _refine_diff_density_min -0.625 _refine_diff_density_rms 0.082 #===END data_FO785 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C53 H66 N8 O3 Ru' _chemical_formula_weight 964.21 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 '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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' '-x, -y, -z' '-x, y, -z-1/2' '-x+1/2, -y+1/2, -z' '-x+1/2, y+1/2, -z-1/2' _cell_length_a 11.7219(5) _cell_length_b 17.5925(8) _cell_length_c 24.522(1) _cell_angle_alpha 90.00 _cell_angle_beta 101.083(3) _cell_angle_gamma 90.00 _cell_volume 4962.6(4) _cell_formula_units_Z 4 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour brown _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.28 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.291 _exptl_crystal_density_method ? _exptl_crystal_F_000 2032 _exptl_absorpt_coefficient_mu 0.366 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 183(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 KappaCCD _diffrn_measurement_method phi-scan _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5809 _diffrn_reflns_av_R_equivalents 0.0448 _diffrn_reflns_av_sigmaI/netI 0.0530 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.12 _diffrn_reflns_theta_max 23.30 _reflns_number_total 3209 _reflns_number_observed 2786 _reflns_observed_criterion >2sigma(I) _computing_data_collection DENZO _computing_cell_refinement DENZO _computing_data_reduction DENZO _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics SHELXTL/PC _computing_publication_material SHELXL-93 _refine_special_details ; Refinement on F^2^ for ALL reflections except for 127 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.1000P)^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 rigid-group _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0027(9) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 3082 _refine_ls_number_parameters 313 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0693 _refine_ls_R_factor_obs 0.0526 _refine_ls_wR_factor_all 0.1741 _refine_ls_wR_factor_obs 0.1482 _refine_ls_goodness_of_fit_all 1.231 _refine_ls_goodness_of_fit_obs 1.260 _refine_ls_restrained_S_all 1.371 _refine_ls_restrained_S_obs 1.260 _refine_ls_shift/esd_max -0.158 _refine_ls_shift/esd_mean 0.034 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Ru Ru 1.0000 1.01465(3) 0.7500 0.0352(3) Uani 1 d S . N1 N 0.8993(4) 0.9213(2) 0.71602(14) 0.0431(9) Uani 1 d . . N2 N 0.8804(5) 0.7917(3) 0.7102(2) 0.0609(13) Uani 1 d . . N3 N 0.8930(3) 1.0953(2) 0.70618(14) 0.0411(9) Uani 1 d . . N4 N 1.0695(3) 1.0234(2) 0.67939(14) 0.0368(8) Uani 1 d . . C1 C 0.9437(5) 0.8517(3) 0.7313(2) 0.0472(11) Uani 1 d . . C2 C 0.7852(6) 0.8245(4) 0.6773(2) 0.060(2) Uani 1 d . . C3 C 0.6845(7) 0.7913(5) 0.6438(3) 0.082(2) Uani 1 d . . H3 H 0.6750(7) 0.7377(5) 0.6422(3) 0.099 Uiso 1 calc R . C4 C 0.6014(7) 0.8383(6) 0.6139(3) 0.089(3) Uani 1 d . . H4 H 0.5353(7) 0.8164(6) 0.5908(3) 0.106 Uiso 1 calc R . C5 C 0.6121(5) 0.9172(6) 0.6168(2) 0.081(2) Uani 1 d . . H5 H 0.5525(5) 0.9477(6) 0.5958(2) 0.098 Uiso 1 calc R . C6 C 0.7084(5) 0.9527(4) 0.6499(2) 0.062(2) Uani 1 d . . H6 H 0.7153(5) 1.0065(4) 0.6517(2) 0.075 Uiso 1 calc R . C7 C 0.7936(5) 0.9056(3) 0.6800(2) 0.0511(13) Uani 1 d . . C8 C 0.8042(5) 1.1303(3) 0.7223(2) 0.0486(12) Uani 1 d . . H8 H 0.7918(5) 1.1210(3) 0.7589(2) 0.058 Uiso 1 calc R . C9 C 0.7293(5) 1.1792(3) 0.6890(2) 0.0517(13) Uani 1 d . . H9 H 0.6674(5) 1.2024(3) 0.7028(2) 0.062 Uiso 1 calc R . C10 C 0.7447(4) 1.1947(3) 0.6344(2) 0.0450(11) Uani 1 d . . C11 C 0.8386(4) 1.1598(3) 0.6184(2) 0.0407(10) Uani 1 d . . H11 H 0.8525(4) 1.1688(3) 0.5820(2) 0.049 Uiso 1 calc R . C12 C 0.9136(4) 1.1117(3) 0.6538(2) 0.0383(10) Uani 1 d . . C13 C 1.0168(4) 1.0744(3) 0.64017(15) 0.0351(10) Uani 1 d . . C14 C 1.0622(4) 1.0905(3) 0.5927(2) 0.0366(10) Uani 1 d . . H14 H 1.0245(4) 1.1265(3) 0.5664(2) 0.044 Uiso 1 calc R . C15 C 1.1631(4) 1.0538(3) 0.5836(2) 0.0397(10) Uani 1 d . . C16 C 1.2142(4) 1.0025(3) 0.6236(2) 0.0429(11) Uani 1 d . . H16 H 1.2834(4) 0.9769(3) 0.6194(2) 0.051 Uiso 1 calc R . C17 C 1.1655(5) 0.9879(3) 0.6700(2) 0.0446(11) Uani 1 d . . H17 H 1.2015(5) 0.9512(3) 0.6962(2) 0.054 Uiso 1 calc R . C18 C 0.6605(5) 1.2442(4) 0.5940(2) 0.0558(14) Uani 1 d . . C19 C 0.5928(6) 1.1930(5) 0.5484(2) 0.073(2) Uani 1 d . . H19A H 0.5385(6) 1.2240(5) 0.5221(2) 0.110 Uiso 1 calc R . H19B H 0.5493(6) 1.1549(5) 0.5652(2) 0.110 Uiso 1 calc R . H19C H 0.6473(6) 1.1675(5) 0.5287(2) 0.110 Uiso 1 calc R . C20 C 0.5737(7) 1.2864(5) 0.6235(2) 0.082(2) Uani 1 d . . H20A H 0.5215(7) 1.3176(5) 0.5964(2) 0.123 Uiso 1 calc R . H20B H 0.6166(7) 1.3191(5) 0.6528(2) 0.123 Uiso 1 calc R . H20C H 0.5280(7) 1.2493(5) 0.6400(2) 0.123 Uiso 1 calc R . C21 C 0.7292(6) 1.3038(4) 0.5686(2) 0.071(2) Uani 1 d . . H21A H 0.6754(6) 1.3357(4) 0.5428(2) 0.106 Uiso 1 calc R . H21B H 0.7832(6) 1.2784(4) 0.5486(2) 0.106 Uiso 1 calc R . H21C H 0.7731(6) 1.3356(4) 0.5982(2) 0.106 Uiso 1 calc R . C22 C 1.2144(4) 1.0714(3) 0.5312(2) 0.0473(12) Uani 1 d . . C23 C 1.1302(7) 1.0435(7) 0.4803(3) 0.102(3) Uani 1 d . . H23A H 1.1192(7) 0.9885(7) 0.4833(3) 0.154 Uiso 1 calc R . H23B H 1.1616(7) 1.0545(7) 0.4469(3) 0.154 Uiso 1 calc R . H23C H 1.0553(7) 1.0693(7) 0.4779(3) 0.154 Uiso 1 calc R . C24 C 1.3342(7) 1.0333(5) 0.5343(3) 0.085(2) Uani 1 d . . H24A H 1.3881(7) 1.0517(5) 0.5672(3) 0.127 Uiso 1 calc R . H24B H 1.3646(7) 1.0459(5) 0.5009(3) 0.127 Uiso 1 calc R . H24C H 1.3258(7) 0.9780(5) 0.5367(3) 0.127 Uiso 1 calc R . C25 C 1.2344(8) 1.1575(5) 0.5281(3) 0.091(2) Uani 1 d . . H25A H 1.2889(8) 1.1741(5) 0.5615(3) 0.137 Uiso 1 calc R . H25B H 1.1603(8) 1.1843(5) 0.5259(3) 0.137 Uiso 1 calc R . H25C H 1.2668(8) 1.1692(5) 0.4951(3) 0.137 Uiso 1 calc R . O2 O 0.3725(10) 0.8712(9) 0.6973(4) 0.109(4) Uani 0.50 d P -1 C26 C 0.5096(33) 0.9409(15) 0.7565(16) 0.136(13) Uani 0.50 d P -1 H26A H 0.4632(33) 0.9838(15) 0.7390(16) 0.204 Uiso 0.50 calc PR -1 H26B H 0.5894(33) 0.9455(15) 0.7503(16) 0.204 Uiso 0.50 calc PR -1 H26C H 0.5100(33) 0.9409(15) 0.7965(16) 0.204 Uiso 0.50 calc PR -1 C27 C 0.4587(11) 0.8695(8) 0.7320(5) 0.062(3) Uani 0.50 d P -1 C28 C 0.5157(41) 0.7976(14) 0.7518(17) 0.119(12) Uani 0.50 d P -1 H28A H 0.4727(41) 0.7551(14) 0.7316(17) 0.178 Uiso 0.50 calc PR -1 H28B H 0.5169(41) 0.7921(14) 0.7916(17) 0.178 Uiso 0.50 calc PR -1 H28C H 0.5956(41) 0.7977(14) 0.7452(17) 0.178 Uiso 0.50 calc PR -1 O1 O 0.9061(8) 0.6337(4) 0.6979(4) 0.144(3) Uani 1 d . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru 0.0377(4) 0.0415(4) 0.0284(4) 0.000 0.0118(2) 0.000 N1 0.051(2) 0.047(3) 0.035(2) -0.009(2) 0.017(2) -0.003(2) N2 0.082(3) 0.057(3) 0.053(2) -0.009(2) 0.037(2) -0.013(3) N3 0.043(2) 0.051(3) 0.032(2) 0.001(2) 0.0159(15) 0.001(2) N4 0.037(2) 0.038(2) 0.036(2) -0.0017(15) 0.0096(14) 0.002(2) C1 0.066(3) 0.041(3) 0.042(2) -0.008(2) 0.030(2) -0.008(2) C2 0.075(4) 0.067(4) 0.048(3) -0.022(3) 0.036(3) -0.031(3) C3 0.086(5) 0.103(6) 0.066(4) -0.035(4) 0.034(4) -0.050(5) C4 0.070(5) 0.137(8) 0.063(4) -0.035(4) 0.024(3) -0.053(5) C5 0.052(4) 0.151(8) 0.044(3) -0.009(3) 0.015(2) -0.019(4) C6 0.053(3) 0.096(5) 0.040(3) -0.011(3) 0.013(2) -0.013(3) C7 0.047(3) 0.078(4) 0.033(2) -0.011(2) 0.020(2) -0.012(3) C8 0.059(3) 0.060(3) 0.032(2) 0.002(2) 0.021(2) 0.009(3) C9 0.054(3) 0.064(3) 0.043(2) 0.005(2) 0.024(2) 0.019(3) C10 0.045(3) 0.051(3) 0.042(2) 0.001(2) 0.013(2) 0.008(2) C11 0.043(3) 0.049(3) 0.033(2) -0.002(2) 0.015(2) 0.004(2) C12 0.044(3) 0.044(3) 0.029(2) -0.003(2) 0.013(2) -0.002(2) C13 0.037(2) 0.044(3) 0.026(2) -0.007(2) 0.009(2) 0.001(2) C14 0.038(2) 0.043(3) 0.031(2) 0.003(2) 0.011(2) -0.001(2) C15 0.041(2) 0.041(3) 0.041(2) -0.002(2) 0.017(2) -0.003(2) C16 0.040(3) 0.052(3) 0.040(2) -0.001(2) 0.016(2) 0.009(2) C17 0.047(3) 0.050(3) 0.039(2) 0.003(2) 0.012(2) 0.005(2) C18 0.058(3) 0.070(4) 0.042(2) 0.009(2) 0.018(2) 0.023(3) C19 0.058(4) 0.100(5) 0.058(3) 0.013(3) 0.002(2) 0.008(3) C20 0.089(5) 0.105(6) 0.063(3) 0.024(3) 0.041(3) 0.052(4) C21 0.090(4) 0.064(4) 0.062(3) 0.019(3) 0.026(3) 0.023(3) C22 0.048(3) 0.058(3) 0.043(2) 0.009(2) 0.026(2) 0.006(2) C23 0.086(5) 0.168(9) 0.060(4) -0.003(4) 0.030(3) -0.019(6) C24 0.081(5) 0.092(5) 0.094(5) 0.012(4) 0.047(4) 0.009(4) C25 0.105(6) 0.077(5) 0.112(5) 0.016(4) 0.069(5) 0.004(4) O2 0.080(7) 0.162(13) 0.079(6) 0.002(6) 0.004(6) 0.041(8) C26 0.166(22) 0.149(21) 0.112(18) -0.052(20) 0.075(16) -0.113(24) C27 0.050(7) 0.068(10) 0.071(8) 0.007(6) 0.015(5) 0.018(7) C28 0.151(28) 0.129(17) 0.089(10) 0.056(20) 0.054(13) 0.070(24) O1 0.137(6) 0.075(4) 0.242(8) -0.016(5) 0.090(6) -0.024(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 Ru N4 2.056(4) . ? Ru N4 2.056(4) 6_757 ? Ru N3 2.055(4) 6_757 ? Ru N3 2.055(4) . ? Ru N1 2.099(4) . ? Ru N1 2.099(4) 6_757 ? N1 C1 1.356(7) . ? N1 C7 1.404(7) . ? N2 C1 1.336(7) . ? N2 C2 1.372(9) . ? N3 C8 1.334(7) . ? N3 C12 1.381(5) . ? N4 C17 1.345(7) . ? N4 C13 1.372(6) . ? C1 C1 1.454(11) 6_757 ? C2 C3 1.426(9) . ? C2 C7 1.432(9) . ? C3 C4 1.376(13) . ? C4 C5 1.394(14) . ? C5 C6 1.405(9) . ? C6 C7 1.394(9) . ? C8 C9 1.379(7) . ? C9 C10 1.411(7) . ? C10 C11 1.381(7) . ? C10 C18 1.530(7) . ? C11 C12 1.397(7) . ? C12 C13 1.470(6) . ? C13 C14 1.399(6) . ? C14 C15 1.402(7) . ? C15 C16 1.382(7) . ? C15 C22 1.552(6) . ? C16 C17 1.393(7) . ? C18 C21 1.525(9) . ? C18 C19 1.534(9) . ? C18 C20 1.546(8) . ? C22 C23 1.516(10) . ? C22 C25 1.537(10) . ? C22 C24 1.545(9) . ? O2 C27 1.19(2) . ? C26 C27 1.47(3) . ? C27 C28 1.47(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N4 Ru N4 171.4(2) . 6_757 ? N4 Ru N3 95.04(14) . 6_757 ? N4 Ru N3 78.95(14) 6_757 6_757 ? N4 Ru N3 78.95(14) . . ? N4 Ru N3 95.04(14) 6_757 . ? N3 Ru N3 92.6(2) 6_757 . ? N4 Ru N1 90.46(14) . . ? N4 Ru N1 96.29(14) 6_757 . ? N3 Ru N1 171.07(14) 6_757 . ? N3 Ru N1 95.3(2) . . ? N4 Ru N1 96.29(14) . 6_757 ? N4 Ru N1 90.46(14) 6_757 6_757 ? N3 Ru N1 95.3(2) 6_757 6_757 ? N3 Ru N1 171.07(14) . 6_757 ? N1 Ru N1 77.0(2) . 6_757 ? C1 N1 C7 104.0(4) . . ? C1 N1 Ru 116.1(3) . . ? C7 N1 Ru 139.9(4) . . ? C1 N2 C2 103.0(5) . . ? C8 N3 C12 117.8(4) . . ? C8 N3 Ru 126.6(3) . . ? C12 N3 Ru 115.6(3) . . ? C17 N4 C13 117.6(4) . . ? C17 N4 Ru 126.0(3) . . ? C13 N4 Ru 116.2(3) . . ? N2 C1 N1 116.8(5) . . ? N2 C1 C1 127.8(3) . 6_757 ? N1 C1 C1 115.3(3) . 6_757 ? N2 C2 C3 131.0(7) . . ? N2 C2 C7 110.5(5) . . ? C3 C2 C7 118.5(7) . . ? C4 C3 C2 118.9(8) . . ? C3 C4 C5 121.6(6) . . ? C4 C5 C6 121.8(8) . . ? C7 C6 C5 117.1(7) . . ? C6 C7 N1 132.2(6) . . ? C6 C7 C2 122.1(5) . . ? N1 C7 C2 105.7(5) . . ? N3 C8 C9 123.8(4) . . ? C8 C9 C10 119.9(4) . . ? C11 C10 C9 116.0(4) . . ? C11 C10 C18 121.2(4) . . ? C9 C10 C18 122.7(4) . . ? C10 C11 C12 122.2(4) . . ? N3 C12 C11 120.2(4) . . ? N3 C12 C13 114.6(4) . . ? C11 C12 C13 125.2(3) . . ? N4 C13 C14 121.6(4) . . ? N4 C13 C12 114.3(3) . . ? C14 C13 C12 124.1(4) . . ? C13 C14 C15 120.4(4) . . ? C16 C15 C14 116.9(4) . . ? C16 C15 C22 122.3(4) . . ? C14 C15 C22 120.8(4) . . ? C15 C16 C17 120.7(4) . . ? N4 C17 C16 122.8(4) . . ? C10 C18 C21 109.3(5) . . ? C10 C18 C19 108.5(5) . . ? C21 C18 C19 110.2(4) . . ? C10 C18 C20 111.8(4) . . ? C21 C18 C20 107.9(6) . . ? C19 C18 C20 109.2(5) . . ? C23 C22 C25 111.2(6) . . ? C23 C22 C15 108.8(5) . . ? C25 C22 C15 108.9(4) . . ? C23 C22 C24 110.0(6) . . ? C25 C22 C24 106.5(6) . . ? C15 C22 C24 111.4(4) . . ? O2 C27 C28 121.9(23) . . ? O2 C27 C26 119.5(20) . . ? C28 C27 C26 118.6(26) . . ? _refine_diff_density_max 0.896 _refine_diff_density_min -0.392 _refine_diff_density_rms 0.066 #===END data_fo966 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C104 H140 F12 N12 O6 P2 Ru2' _chemical_formula_weight 2146.36 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' '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 12.3749(3) _cell_length_b 14.4512(4) _cell_length_c 16.6108(5) _cell_angle_alpha 80.763(2) _cell_angle_beta 88.971(2) _cell_angle_gamma 75.717(2) _cell_volume 2840.67(14) _cell_formula_units_Z 1 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour red-brown _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.255 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1122 _exptl_absorpt_coefficient_mu 0.367 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.8915 _exptl_absorpt_correction_T_max 0.9302 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 183(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 KappaCCD _diffrn_measurement_method 'phi- + omega-scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20676 _diffrn_reflns_av_R_equivalents 0.0474 _diffrn_reflns_av_sigmaI/netI 0.0699 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.54 _diffrn_reflns_theta_max 26.38 _reflns_number_total 11432 _reflns_number_gt 9084 _reflns_threshold_expression >2sigma(I) _computing_data_collection COLLECT _computing_cell_refinement DENZO _computing_data_reduction DENZO _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL/PC _computing_publication_material SHELXL-97 _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0807P)^2^+3.7959P] 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 rigid-group _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11432 _refine_ls_number_parameters 603 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0855 _refine_ls_R_factor_gt 0.0635 _refine_ls_wR_factor_ref 0.1686 _refine_ls_wR_factor_gt 0.1552 _refine_ls_goodness_of_fit_ref 1.081 _refine_ls_restrained_S_all 1.085 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru Ru 0.98051(3) 0.56544(2) 0.650226(18) 0.02725(11) Uani 1 1 d . . . N1 N 0.8995(3) 0.6017(2) 0.53122(19) 0.0306(7) Uani 1 1 d . . . N2 N 0.9136(3) 0.5461(2) 0.4085(2) 0.0311(7) Uani 1 1 d . . . N3 N 1.0684(3) 0.6694(2) 0.61724(19) 0.0301(7) Uani 1 1 d . . . N4 N 0.8770(3) 0.6826(2) 0.68860(19) 0.0287(7) Uani 1 1 d . . . N5 N 1.0610(3) 0.5106(2) 0.76042(19) 0.0309(7) Uani 1 1 d . . . N6 N 0.8887(3) 0.4702(2) 0.6998(2) 0.0312(7) Uani 1 1 d . . . C1 C 0.9523(3) 0.5370(3) 0.4846(2) 0.0310(8) Uani 1 1 d . . . C2 C 0.8150(3) 0.6607(3) 0.4798(2) 0.0315(8) Uani 1 1 d . . . C3 C 0.7311(4) 0.7426(3) 0.4913(3) 0.0401(10) Uani 1 1 d . . . H3A H 0.7247 0.7664 0.5417 0.048 Uiso 1 1 calc R . . C4 C 0.6576(4) 0.7875(3) 0.4262(3) 0.0491(12) Uani 1 1 d . . . H4A H 0.6002 0.8430 0.4327 0.059 Uiso 1 1 calc R . . C5 C 0.6655(4) 0.7537(3) 0.3517(3) 0.0486(11) Uani 1 1 d . . . H5A H 0.6131 0.7863 0.3091 0.058 Uiso 1 1 calc R . . C6 C 0.7480(4) 0.6737(3) 0.3384(3) 0.0410(10) Uani 1 1 d . . . H6A H 0.7530 0.6517 0.2872 0.049 Uiso 1 1 calc R . . C7 C 0.8236(3) 0.6260(3) 0.4024(2) 0.0301(8) Uani 1 1 d . . . C8 C 1.1701(4) 0.6565(3) 0.5851(3) 0.0365(9) Uani 1 1 d . . . H8A H 1.2042 0.5951 0.5706 0.044 Uiso 1 1 calc R . . C9 C 1.2283(4) 0.7281(3) 0.5717(3) 0.0382(9) Uani 1 1 d . . . H9A H 1.3009 0.7145 0.5498 0.046 Uiso 1 1 calc R . . C10 C 1.1804(3) 0.8200(3) 0.5903(3) 0.0346(9) Uani 1 1 d . . . C11 C 1.0734(3) 0.8346(3) 0.6230(2) 0.0329(8) Uani 1 1 d . . . H11A H 1.0372 0.8960 0.6364 0.039 Uiso 1 1 calc R . . C12 C 1.0198(3) 0.7590(3) 0.6359(2) 0.0299(8) Uani 1 1 d . . . C13 C 0.9087(3) 0.7675(3) 0.6723(2) 0.0288(8) Uani 1 1 d . . . C14 C 0.8385(3) 0.8552(3) 0.6876(2) 0.0316(8) Uani 1 1 d . . . H14A H 0.8630 0.9132 0.6758 0.038 Uiso 1 1 calc R . . C15 C 0.7335(3) 0.8576(3) 0.7199(2) 0.0322(8) Uani 1 1 d . . . C16 C 0.7039(4) 0.7690(3) 0.7375(3) 0.0346(9) Uani 1 1 d . . . H16A H 0.6336 0.7669 0.7606 0.041 Uiso 1 1 calc R . . C17 C 0.7759(3) 0.6852(3) 0.7217(2) 0.0324(8) Uani 1 1 d . . . H17A H 0.7535 0.6263 0.7346 0.039 Uiso 1 1 calc R . . C18 C 1.2383(4) 0.9035(3) 0.5776(3) 0.0408(10) Uani 1 1 d . . . C19 C 1.3553(4) 0.8730(4) 0.5409(4) 0.0537(13) Uani 1 1 d . . . H19A H 1.3479 0.8539 0.4877 0.081 Uiso 1 1 calc R . . H19B H 1.4017 0.8183 0.5776 0.081 Uiso 1 1 calc R . . H19C H 1.3904 0.9275 0.5342 0.081 Uiso 1 1 calc R . . C20 C 1.2530(4) 0.9328(4) 0.6615(3) 0.0514(12) Uani 1 1 d . . . H20A H 1.1798 0.9524 0.6858 0.077 Uiso 1 1 calc R . . H20B H 1.2887 0.9870 0.6543 0.077 Uiso 1 1 calc R . . H20C H 1.2998 0.8776 0.6975 0.077 Uiso 1 1 calc R . . C21 C 1.1647(4) 0.9895(3) 0.5202(3) 0.0494(12) Uani 1 1 d . . . H21A H 1.0909 1.0085 0.5438 0.074 Uiso 1 1 calc R . . H21B H 1.1569 0.9706 0.4670 0.074 Uiso 1 1 calc R . . H21C H 1.1994 1.0442 0.5134 0.074 Uiso 1 1 calc R . . C22 C 0.6517(4) 0.9505(3) 0.7359(3) 0.0405(10) Uani 1 1 d . . . C23 C 0.6385(6) 0.9449(5) 0.8291(4) 0.0753(19) Uani 1 1 d . . . H23A H 0.7108 0.9401 0.8547 0.113 Uiso 1 1 calc R . . H23B H 0.6114 0.8878 0.8510 0.113 Uiso 1 1 calc R . . H23C H 0.5848 1.0033 0.8406 0.113 Uiso 1 1 calc R . . C24 C 0.5397(5) 0.9583(4) 0.6950(5) 0.0742(19) Uani 1 1 d . . . H24A H 0.5489 0.9623 0.6359 0.111 Uiso 1 1 calc R . . H24B H 0.4858 1.0164 0.7066 0.111 Uiso 1 1 calc R . . H24C H 0.5126 0.9010 0.7162 0.111 Uiso 1 1 calc R . . C25 C 0.6924(5) 1.0401(4) 0.7028(4) 0.0644(16) Uani 1 1 d . . . H25A H 0.6998 1.0451 0.6436 0.097 Uiso 1 1 calc R . . H25B H 0.7650 1.0352 0.7280 0.097 Uiso 1 1 calc R . . H25C H 0.6386 1.0978 0.7156 0.097 Uiso 1 1 calc R . . C26 C 1.1520(4) 0.5333(3) 0.7866(3) 0.0389(10) Uani 1 1 d . . . H26A H 1.1809 0.5807 0.7528 0.047 Uiso 1 1 calc R . . C27 C 1.2053(4) 0.4905(3) 0.8607(3) 0.0402(10) Uani 1 1 d . . . H27A H 1.2693 0.5089 0.8766 0.048 Uiso 1 1 calc R . . C28 C 1.1659(4) 0.4206(3) 0.9123(2) 0.0360(9) Uani 1 1 d . . . C29 C 1.0722(4) 0.3970(3) 0.8848(2) 0.0342(9) Uani 1 1 d . . . H29A H 1.0430 0.3490 0.9175 0.041 Uiso 1 1 calc R . . C30 C 1.0203(3) 0.4427(3) 0.8099(2) 0.0291(8) Uani 1 1 d . . . C31 C 0.9194(3) 0.4230(3) 0.7772(2) 0.0293(8) Uani 1 1 d . . . C32 C 0.8566(4) 0.3655(3) 0.8207(3) 0.0349(9) Uani 1 1 d . . . H32A H 0.8804 0.3336 0.8743 0.042 Uiso 1 1 calc R . . C33 C 0.7583(4) 0.3536(3) 0.7870(3) 0.0370(9) Uani 1 1 d . . . C34 C 0.7305(4) 0.4002(3) 0.7075(3) 0.0416(10) Uani 1 1 d . . . H34A H 0.6659 0.3935 0.6811 0.050 Uiso 1 1 calc R . . C35 C 0.7971(4) 0.4569(3) 0.6662(3) 0.0380(9) Uani 1 1 d . . . H35A H 0.7765 0.4874 0.6117 0.046 Uiso 1 1 calc R . . C36 C 1.2239(4) 0.3773(4) 0.9953(3) 0.0454(11) Uani 1 1 d . . . C37 C 1.3459(6) 0.3296(6) 0.9841(5) 0.089(2) Uani 1 1 d . . . H37A H 1.3514 0.2757 0.9539 0.133 Uiso 1 1 calc R . . H37B H 1.3830 0.3053 1.0377 0.133 Uiso 1 1 calc R . . H37C H 1.3820 0.3772 0.9535 0.133 Uiso 1 1 calc R . . C38 C 1.2208(7) 0.4598(5) 1.0434(4) 0.083(2) Uani 1 1 d . . . H38A H 1.1431 0.4921 1.0524 0.124 Uiso 1 1 calc R . . H38B H 1.2576 0.5065 1.0125 0.124 Uiso 1 1 calc R . . H38C H 1.2596 0.4336 1.0961 0.124 Uiso 1 1 calc R . . C39 C 1.1666(7) 0.3053(7) 1.0446(4) 0.102(3) Uani 1 1 d . . . H39A H 1.1678 0.2521 1.0144 0.152 Uiso 1 1 calc R . . H39B H 1.0892 0.3380 1.0539 0.152 Uiso 1 1 calc R . . H39C H 1.2060 0.2796 1.0971 0.152 Uiso 1 1 calc R . . C40 C 0.6887(4) 0.2923(3) 0.8367(3) 0.0428(10) Uani 1 1 d . . . C41 C 0.7606(5) 0.1874(3) 0.8582(4) 0.0546(13) Uani 1 1 d . . . H41A H 0.7826 0.1610 0.8079 0.082 Uiso 1 1 calc R . . H41B H 0.7172 0.1475 0.8912 0.082 Uiso 1 1 calc R . . H41C H 0.8274 0.1870 0.8891 0.082 Uiso 1 1 calc R . . C42 C 0.5831(5) 0.2919(4) 0.7893(4) 0.0603(14) Uani 1 1 d . . . H42A H 0.5370 0.3582 0.7757 0.090 Uiso 1 1 calc R . . H42B H 0.5406 0.2518 0.8231 0.090 Uiso 1 1 calc R . . H42C H 0.6044 0.2653 0.7390 0.090 Uiso 1 1 calc R . . C43 C 0.6537(5) 0.3330(4) 0.9166(4) 0.0585(14) Uani 1 1 d . . . H43A H 0.6079 0.3995 0.9034 0.088 Uiso 1 1 calc R . . H43B H 0.7204 0.3326 0.9477 0.088 Uiso 1 1 calc R . . H43C H 0.6105 0.2928 0.9494 0.088 Uiso 1 1 calc R . . P P 0.55062(12) 0.36639(10) 0.21938(10) 0.0558(4) Uani 1 1 d . . . F6 F 0.4212(3) 0.4137(3) 0.2063(3) 0.0901(13) Uani 1 1 d . . . F5 F 0.6805(3) 0.3180(3) 0.2333(4) 0.1069(16) Uani 1 1 d . . . F4 F 0.5272(4) 0.3151(4) 0.3067(3) 0.1130(17) Uani 1 1 d . . . F3 F 0.5326(4) 0.2751(4) 0.1854(4) 0.1168(18) Uani 1 1 d . . . F2 F 0.5752(4) 0.4142(4) 0.1313(3) 0.1173(18) Uani 1 1 d . . . F1 F 0.5694(5) 0.4561(4) 0.2535(4) 0.1249(19) Uani 1 1 d . . . O1 O 0.9651(4) 1.0615(3) 0.6871(3) 0.0686(11) Uani 1 1 d . . . C44 C 0.9694(8) 1.2139(5) 0.6097(5) 0.091(2) Uani 1 1 d . . . H44A H 0.9245 1.1957 0.5697 0.136 Uiso 1 1 calc R . . H44B H 1.0391 1.2234 0.5850 0.136 Uiso 1 1 calc R . . H44C H 0.9276 1.2742 0.6270 0.136 Uiso 1 1 calc R . . C45 C 0.9949(4) 1.1360(4) 0.6816(4) 0.0543(13) Uani 1 1 d . . . C46 C 1.0643(6) 1.1525(5) 0.7500(5) 0.083(2) Uani 1 1 d . . . H46A H 1.0760 1.0968 0.7941 0.124 Uiso 1 1 calc R . . H46B H 1.0251 1.2111 0.7711 0.124 Uiso 1 1 calc R . . H46C H 1.1367 1.1603 0.7291 0.124 Uiso 1 1 calc R . . O2 O 0.9597(6) 0.2077(5) 0.9970(3) 0.116(2) Uani 1 1 d . . . C47 C 1.0272(12) 0.0776(10) 1.0976(8) 0.160(5) Uiso 1 1 d . . . H47A H 1.0655 0.0497 1.0517 0.240 Uiso 1 1 calc R . . H47B H 0.9791 0.0371 1.1229 0.240 Uiso 1 1 calc R . . H47C H 1.0825 0.0808 1.1379 0.240 Uiso 1 1 calc R . . C48 C 0.9597(6) 0.1748(5) 1.0682(5) 0.0783(18) Uiso 1 1 d . . . C49 C 0.8998(12) 0.2284(10) 1.1298(8) 0.158(5) Uiso 1 1 d . . . H49A H 0.8578 0.2924 1.1033 0.237 Uiso 1 1 calc R . . H49B H 0.9534 0.2357 1.1696 0.237 Uiso 1 1 calc R . . H49C H 0.8482 0.1929 1.1577 0.237 Uiso 1 1 calc R . . O3 O 0.6573(15) 1.1009(13) 1.0862(11) 0.153(6) Uiso 0.50 1 d PD . . C50 C 0.5581(15) 1.0676(13) 1.0042(11) 0.103(5) Uiso 0.50 1 d PD . . H50A H 0.5517 1.1373 0.9900 0.154 Uiso 0.50 1 calc PR . . H50B H 0.4866 1.0569 1.0245 0.154 Uiso 0.50 1 calc PR . . H50C H 0.5777 1.0369 0.9556 0.154 Uiso 0.50 1 calc PR . . C51 C 0.6471(15) 1.0246(13) 1.0690(10) 0.142(8) Uiso 0.50 1 d PD . . C52 C 0.6781(16) 0.9187(12) 1.1043(12) 0.108(5) Uiso 0.50 1 d PD . . H52A H 0.7360 0.9067 1.1468 0.161 Uiso 0.50 1 calc PR . . H52B H 0.7064 0.8808 1.0611 0.161 Uiso 0.50 1 calc PR . . H52C H 0.6122 0.8997 1.1280 0.161 Uiso 0.50 1 calc PR . . O4 O 0.6311(9) 0.4331(7) 0.5279(6) 0.081(3) Uiso 0.50 1 d PD A -1 C53 C 0.539(3) 0.5764(13) 0.4537(17) 0.170(12) Uiso 0.50 1 d PD A -1 H53A H 0.6153 0.5850 0.4478 0.255 Uiso 0.50 1 calc PR A -1 H53B H 0.4941 0.6272 0.4814 0.255 Uiso 0.50 1 calc PR A -1 H53C H 0.5064 0.5805 0.3996 0.255 Uiso 0.50 1 calc PR A -1 C54 C 0.5425(10) 0.4790(9) 0.5030(7) 0.067(3) Uiso 0.50 1 d PD A -1 C55 C 0.4534(15) 0.4266(14) 0.4944(15) 0.115(6) Uiso 0.50 1 d PD A -1 H55A H 0.4802 0.3585 0.5189 0.172 Uiso 0.50 1 calc PR A -1 H55B H 0.4357 0.4309 0.4364 0.172 Uiso 0.50 1 calc PR A -1 H55C H 0.3862 0.4562 0.5221 0.172 Uiso 0.50 1 calc PR 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 Ru 0.02998(18) 0.02578(17) 0.02587(17) -0.00389(11) -0.00071(11) -0.00678(12) N1 0.0329(18) 0.0262(16) 0.0296(17) -0.0037(12) -0.0012(14) -0.0017(13) N2 0.0343(18) 0.0281(16) 0.0284(16) -0.0031(13) -0.0030(13) -0.0037(14) N3 0.0296(17) 0.0299(16) 0.0286(16) -0.0021(13) 0.0010(13) -0.0048(13) N4 0.0294(17) 0.0342(17) 0.0252(15) -0.0048(12) 0.0012(13) -0.0128(14) N5 0.0356(19) 0.0307(17) 0.0284(16) -0.0064(13) 0.0034(14) -0.0107(14) N6 0.0347(18) 0.0266(16) 0.0327(17) -0.0080(13) -0.0033(14) -0.0062(14) C1 0.034(2) 0.0281(19) 0.0280(19) -0.0038(15) -0.0039(16) -0.0016(16) C2 0.033(2) 0.0266(19) 0.033(2) -0.0023(15) -0.0025(16) -0.0058(16) C3 0.040(2) 0.034(2) 0.041(2) -0.0060(17) -0.0007(19) -0.0003(18) C4 0.043(3) 0.036(2) 0.058(3) -0.007(2) -0.008(2) 0.011(2) C5 0.044(3) 0.044(3) 0.050(3) -0.001(2) -0.016(2) 0.002(2) C6 0.041(2) 0.040(2) 0.037(2) 0.0005(17) -0.0121(19) -0.0028(19) C7 0.031(2) 0.0266(18) 0.0304(19) -0.0002(14) -0.0046(16) -0.0049(15) C8 0.032(2) 0.036(2) 0.039(2) -0.0034(17) 0.0047(17) -0.0056(17) C9 0.029(2) 0.039(2) 0.045(2) -0.0027(18) 0.0091(18) -0.0070(17) C10 0.030(2) 0.036(2) 0.036(2) 0.0021(16) 0.0001(17) -0.0089(17) C11 0.029(2) 0.031(2) 0.037(2) -0.0014(16) 0.0015(16) -0.0055(16) C12 0.029(2) 0.0317(19) 0.0288(19) -0.0019(15) 0.0005(15) -0.0093(16) C13 0.029(2) 0.0298(19) 0.0270(18) -0.0029(14) -0.0013(15) -0.0071(15) C14 0.033(2) 0.0296(19) 0.034(2) -0.0070(15) 0.0020(16) -0.0111(16) C15 0.028(2) 0.034(2) 0.034(2) -0.0076(16) 0.0010(16) -0.0059(16) C16 0.031(2) 0.038(2) 0.038(2) -0.0116(17) 0.0063(17) -0.0129(17) C17 0.033(2) 0.032(2) 0.034(2) -0.0056(16) 0.0052(16) -0.0118(16) C18 0.026(2) 0.041(2) 0.054(3) 0.0026(19) 0.0007(19) -0.0131(18) C19 0.035(3) 0.054(3) 0.069(3) 0.003(2) 0.013(2) -0.015(2) C20 0.045(3) 0.048(3) 0.066(3) -0.008(2) -0.003(2) -0.021(2) C21 0.039(3) 0.038(2) 0.066(3) 0.012(2) -0.001(2) -0.012(2) C22 0.032(2) 0.036(2) 0.054(3) -0.0142(19) 0.0077(19) -0.0038(18) C23 0.087(5) 0.069(4) 0.059(4) -0.024(3) 0.024(3) 0.008(3) C24 0.041(3) 0.053(3) 0.123(6) -0.016(3) -0.018(3) 0.001(2) C25 0.066(4) 0.031(2) 0.094(4) -0.018(3) 0.023(3) -0.006(2) C26 0.040(2) 0.044(2) 0.035(2) -0.0009(18) -0.0044(18) -0.020(2) C27 0.038(2) 0.052(3) 0.035(2) -0.0044(19) -0.0084(18) -0.020(2) C28 0.036(2) 0.042(2) 0.029(2) -0.0030(17) -0.0036(17) -0.0093(18) C29 0.037(2) 0.036(2) 0.030(2) -0.0014(16) -0.0014(17) -0.0124(17) C30 0.031(2) 0.0270(18) 0.0293(19) -0.0057(14) 0.0011(15) -0.0070(15) C31 0.033(2) 0.0258(18) 0.0304(19) -0.0053(14) -0.0023(16) -0.0081(15) C32 0.039(2) 0.031(2) 0.038(2) -0.0041(16) -0.0009(18) -0.0149(17) C33 0.040(2) 0.030(2) 0.043(2) -0.0066(17) -0.0026(19) -0.0104(18) C34 0.039(2) 0.040(2) 0.049(3) -0.0077(19) -0.009(2) -0.0147(19) C35 0.040(2) 0.035(2) 0.042(2) -0.0055(17) -0.0099(18) -0.0136(18) C36 0.046(3) 0.052(3) 0.036(2) 0.0031(19) -0.013(2) -0.013(2) C37 0.058(4) 0.099(5) 0.087(5) 0.001(4) -0.026(4) 0.014(4) C38 0.114(6) 0.088(5) 0.048(3) -0.013(3) -0.031(4) -0.023(4) C39 0.113(6) 0.133(7) 0.061(4) 0.044(4) -0.047(4) -0.070(6) C40 0.038(2) 0.039(2) 0.056(3) -0.005(2) 0.001(2) -0.021(2) C41 0.057(3) 0.040(3) 0.070(3) -0.003(2) 0.000(3) -0.021(2) C42 0.047(3) 0.061(3) 0.079(4) -0.004(3) -0.003(3) -0.029(3) C43 0.055(3) 0.064(3) 0.064(3) -0.015(3) 0.014(3) -0.028(3) P 0.0403(7) 0.0538(8) 0.0724(9) 0.0062(6) -0.0072(6) -0.0200(6) F6 0.047(2) 0.077(2) 0.133(4) 0.015(2) -0.009(2) -0.0109(18) F5 0.043(2) 0.084(3) 0.182(5) 0.014(3) -0.009(2) -0.0159(19) F4 0.094(3) 0.156(4) 0.082(3) 0.035(3) -0.011(2) -0.051(3) F3 0.087(3) 0.117(4) 0.182(5) -0.077(4) 0.045(3) -0.062(3) F2 0.091(3) 0.179(5) 0.087(3) 0.034(3) -0.005(2) -0.079(3) F1 0.107(4) 0.100(3) 0.194(6) -0.060(4) 0.007(4) -0.054(3) O1 0.063(3) 0.056(2) 0.094(3) -0.014(2) 0.009(2) -0.027(2) C44 0.126(7) 0.050(4) 0.093(5) -0.006(3) -0.004(5) -0.018(4) C45 0.046(3) 0.040(3) 0.075(4) -0.016(2) 0.008(3) -0.005(2) C46 0.077(5) 0.074(4) 0.104(6) -0.031(4) -0.006(4) -0.020(4) O2 0.155(6) 0.140(5) 0.063(3) 0.030(3) -0.039(3) -0.083(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 Ru N4 2.040(3) . ? Ru N5 2.045(3) . ? Ru N6 2.058(3) . ? Ru N3 2.064(3) . ? Ru N1 2.160(3) . ? Ru N2 2.163(3) 2_766 ? N1 C1 1.346(5) . ? N1 C2 1.382(5) . ? N2 C1 1.336(5) . ? N2 C7 1.384(5) . ? N2 Ru 2.163(3) 2_766 ? N3 C8 1.341(5) . ? N3 C12 1.367(5) . ? N4 C17 1.352(5) . ? N4 C13 1.364(5) . ? N5 C26 1.345(5) . ? N5 C30 1.365(5) . ? N6 C35 1.341(5) . ? N6 C31 1.368(5) . ? C1 C1 1.422(8) 2_766 ? C2 C3 1.404(6) . ? C2 C7 1.448(6) . ? C3 C4 1.391(7) . ? C4 C5 1.395(7) . ? C5 C6 1.385(7) . ? C6 C7 1.401(6) . ? C8 C9 1.388(6) . ? C9 C10 1.395(6) . ? C10 C11 1.402(6) . ? C10 C18 1.534(6) . ? C11 C12 1.400(6) . ? C12 C13 1.477(5) . ? C13 C14 1.406(5) . ? C14 C15 1.392(6) . ? C15 C16 1.402(6) . ? C15 C22 1.527(6) . ? C16 C17 1.376(6) . ? C18 C21 1.542(6) . ? C18 C20 1.546(7) . ? C18 C19 1.549(6) . ? C22 C25 1.522(7) . ? C22 C24 1.525(7) . ? C22 C23 1.544(7) . ? C26 C27 1.385(6) . ? C27 C28 1.393(6) . ? C28 C29 1.391(6) . ? C28 C36 1.531(6) . ? C29 C30 1.397(6) . ? C30 C31 1.478(5) . ? C31 C32 1.387(6) . ? C32 C33 1.408(6) . ? C33 C34 1.390(6) . ? C33 C40 1.525(6) . ? C34 C35 1.398(6) . ? C36 C37 1.518(8) . ? C36 C39 1.524(8) . ? C36 C38 1.531(8) . ? C40 C42 1.540(7) . ? C40 C43 1.550(7) . ? C40 C41 1.546(7) . ? P F1 1.563(5) . ? P F2 1.573(4) . ? P F4 1.576(4) . ? P F3 1.580(4) . ? P F6 1.583(4) . ? P F5 1.591(4) . ? O1 C45 1.211(6) . ? C44 C45 1.483(9) . ? C45 C46 1.521(9) . ? O2 C48 1.202(8) . ? C47 C48 1.457(14) . ? C48 C49 1.462(14) . ? O3 C51 1.22(2) . ? C50 C51 1.500(5) . ? C51 C52 1.504(5) . ? O4 C54 1.176(14) . ? C53 C54 1.503(5) . ? C54 C55 1.504(5) . ? 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 N4 Ru N5 95.49(13) . . ? N4 Ru N6 94.64(13) . . ? N5 Ru N6 78.81(13) . . ? N4 Ru N3 78.89(13) . . ? N5 Ru N3 95.66(13) . . ? N6 Ru N3 171.13(12) . . ? N4 Ru N1 91.61(12) . . ? N5 Ru N1 171.64(12) . . ? N6 Ru N1 96.25(13) . . ? N3 Ru N1 90.03(13) . . ? N4 Ru N2 171.44(12) . 2_766 ? N5 Ru N2 92.32(12) . 2_766 ? N6 Ru N2 90.31(13) . 2_766 ? N3 Ru N2 96.87(13) . 2_766 ? N1 Ru N2 80.90(12) . 2_766 ? C1 N1 C2 102.9(3) . . ? C1 N1 Ru 108.5(2) . . ? C2 N1 Ru 148.5(3) . . ? C1 N2 C7 103.4(3) . . ? C1 N2 Ru 108.4(2) . 2_766 ? C7 N2 Ru 148.1(3) . 2_766 ? C8 N3 C12 117.4(3) . . ? C8 N3 Ru 126.9(3) . . ? C12 N3 Ru 115.6(3) . . ? C17 N4 C13 117.5(3) . . ? C17 N4 Ru 125.7(3) . . ? C13 N4 Ru 116.5(3) . . ? C26 N5 C30 117.8(3) . . ? C26 N5 Ru 125.7(3) . . ? C30 N5 Ru 116.5(3) . . ? C35 N6 C31 117.7(4) . . ? C35 N6 Ru 126.1(3) . . ? C31 N6 Ru 116.0(3) . . ? N2 C1 N1 117.9(3) . . ? N2 C1 C1 121.4(4) . 2_766 ? N1 C1 C1 120.7(4) . 2_766 ? N1 C2 C3 131.5(4) . . ? N1 C2 C7 108.2(3) . . ? C3 C2 C7 120.3(4) . . ? C4 C3 C2 117.7(4) . . ? C3 C4 C5 122.0(4) . . ? C6 C5 C4 121.6(4) . . ? C5 C6 C7 118.3(4) . . ? N2 C7 C6 132.3(4) . . ? N2 C7 C2 107.6(3) . . ? C6 C7 C2 120.1(4) . . ? N3 C8 C9 123.4(4) . . ? C8 C9 C10 120.2(4) . . ? C9 C10 C11 116.8(4) . . ? C9 C10 C18 123.8(4) . . ? C11 C10 C18 119.4(4) . . ? C12 C11 C10 120.2(4) . . ? N3 C12 C11 122.0(4) . . ? N3 C12 C13 114.4(3) . . ? C11 C12 C13 123.6(4) . . ? N4 C13 C14 121.7(4) . . ? N4 C13 C12 114.4(3) . . ? C14 C13 C12 124.0(3) . . ? C15 C14 C13 120.4(4) . . ? C14 C15 C16 116.7(4) . . ? C14 C15 C22 123.3(4) . . ? C16 C15 C22 120.0(4) . . ? C17 C16 C15 120.5(4) . . ? N4 C17 C16 123.1(4) . . ? C10 C18 C21 108.8(4) . . ? C10 C18 C20 108.4(4) . . ? C21 C18 C20 110.1(4) . . ? C10 C18 C19 111.5(4) . . ? C21 C18 C19 109.9(4) . . ? C20 C18 C19 108.2(4) . . ? C15 C22 C25 112.1(4) . . ? C15 C22 C24 108.8(4) . . ? C25 C22 C24 108.9(5) . . ? C15 C22 C23 108.2(4) . . ? C25 C22 C23 108.7(5) . . ? C24 C22 C23 110.1(5) . . ? N5 C26 C27 122.7(4) . . ? C26 C27 C28 120.7(4) . . ? C29 C28 C27 116.4(4) . . ? C29 C28 C36 124.1(4) . . ? C27 C28 C36 119.5(4) . . ? C28 C29 C30 121.0(4) . . ? N5 C30 C29 121.3(4) . . ? N5 C30 C31 114.4(3) . . ? C29 C30 C31 124.3(4) . . ? N6 C31 C32 121.5(4) . . ? N6 C31 C30 114.2(3) . . ? C32 C31 C30 124.3(4) . . ? C31 C32 C33 121.2(4) . . ? C34 C33 C32 116.2(4) . . ? C34 C33 C40 123.4(4) . . ? C32 C33 C40 120.4(4) . . ? C33 C34 C35 120.2(4) . . ? N6 C35 C34 123.2(4) . . ? C37 C36 C39 110.4(6) . . ? C37 C36 C28 110.2(4) . . ? C39 C36 C28 112.1(4) . . ? C37 C36 C38 107.0(6) . . ? C39 C36 C38 108.6(6) . . ? C28 C36 C38 108.3(4) . . ? C33 C40 C42 111.8(4) . . ? C33 C40 C43 109.3(4) . . ? C42 C40 C43 108.8(4) . . ? C33 C40 C41 108.8(4) . . ? C42 C40 C41 109.0(4) . . ? C43 C40 C41 109.1(4) . . ? F1 P F2 89.3(3) . . ? F1 P F4 92.4(3) . . ? F2 P F4 178.1(3) . . ? F1 P F3 179.5(4) . . ? F2 P F3 90.9(3) . . ? F4 P F3 87.3(3) . . ? F1 P F6 91.9(3) . . ? F2 P F6 91.4(3) . . ? F4 P F6 89.3(3) . . ? F3 P F6 88.5(3) . . ? F1 P F5 88.3(3) . . ? F2 P F5 89.2(3) . . ? F4 P F5 90.1(3) . . ? F3 P F5 91.2(3) . . ? F6 P F5 179.4(3) . . ? O1 C45 C44 123.7(6) . . ? O1 C45 C46 119.9(6) . . ? C44 C45 C46 116.5(6) . . ? O2 C48 C49 123.9(9) . . ? O2 C48 C47 119.4(9) . . ? C49 C48 C47 116.6(10) . . ? O3 C51 C50 96.6(15) . . ? O3 C51 C52 138.7(19) . . ? C50 C51 C52 123.0(18) . . ? O4 C54 C53 115.6(16) . . ? O4 C54 C55 118.2(14) . . ? C53 C54 C55 122.0(17) . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 26.38 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.963 _refine_diff_density_min -0.635 _refine_diff_density_rms 0.089 #===END data_FO698 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C60 H53 F12 N15 O2 P2 Ru2' _chemical_formula_weight 1508.25 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ru' 'Ru' -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 24.474(2) _cell_length_b 13.921(1) _cell_length_c 19.433(1) _cell_angle_alpha 90.00 _cell_angle_beta 106.843(3) _cell_angle_gamma 90.00 _cell_volume 6336.9(8) _cell_formula_units_Z 4 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour red-brown _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.581 _exptl_crystal_density_method ? _exptl_crystal_F_000 3040 _exptl_absorpt_coefficient_mu 0.619 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 183(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 KappaCCD _diffrn_measurement_method phi-scan _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8224 _diffrn_reflns_av_R_equivalents 0.0449 _diffrn_reflns_av_sigmaI/netI 0.0689 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 5.07 _diffrn_reflns_theta_max 23.32 _reflns_number_total 4504 _reflns_number_observed 3666 _reflns_observed_criterion >2sigma(I) _computing_data_collection DENZO _computing_cell_refinement DENZO _computing_data_reduction DENZO _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics SHELXTL/PC _computing_publication_material SHELXL-93 _refine_special_details ; Refinement on F^2^ for ALL reflections except for 247 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0590P)^2^+18.5575P] 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 rigid-group _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4257 _refine_ls_number_parameters 405 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0635 _refine_ls_R_factor_obs 0.0483 _refine_ls_wR_factor_all 0.1411 _refine_ls_wR_factor_obs 0.1246 _refine_ls_goodness_of_fit_all 1.078 _refine_ls_goodness_of_fit_obs 1.107 _refine_ls_restrained_S_all 1.120 _refine_ls_restrained_S_obs 1.107 _refine_ls_shift/esd_max -0.001 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Ru Ru 0.52671(2) 0.69061(3) 0.53441(2) 0.0335(2) Uani 1 d . . N1 N 0.4457(2) 0.4493(3) 0.4253(2) 0.0358(9) Uani 1 d . . N2 N 0.4677(2) 0.6073(3) 0.4537(2) 0.0381(10) Uani 1 d . . N3 N 0.5917(2) 0.6793(3) 0.4885(2) 0.0405(10) Uani 1 d . . N4 N 0.5906(2) 0.7568(3) 0.6091(2) 0.0367(9) Uani 1 d . . N5 N 0.4866(2) 0.8140(3) 0.4916(2) 0.0393(10) Uani 1 d . . N6 N 0.4653(2) 0.7000(3) 0.5857(2) 0.0395(10) Uani 1 d . . C1 C 0.4782(2) 0.5143(3) 0.4694(3) 0.0354(11) Uani 1 d . . C2 C 0.4091(2) 0.5064(3) 0.3731(2) 0.0343(11) Uani 1 d . . C3 C 0.3645(2) 0.4816(4) 0.3116(3) 0.0392(11) Uani 1 d . . H3A H 0.3544(2) 0.4164(4) 0.3001(3) 0.047 Uiso 1 calc R . C4 C 0.3364(2) 0.5549(4) 0.2690(3) 0.0482(13) Uani 1 d . . H4A H 0.3062(2) 0.5401(4) 0.2271(3) 0.058 Uiso 1 calc R . C5 C 0.3509(2) 0.6516(4) 0.2855(3) 0.0514(14) Uani 1 d . . H5A H 0.3308(2) 0.7002(4) 0.2539(3) 0.062 Uiso 1 calc R . C6 C 0.3932(2) 0.6778(4) 0.3460(3) 0.0447(13) Uani 1 d . . H6A H 0.4019(2) 0.7435(4) 0.3575(3) 0.054 Uiso 1 calc R . C7 C 0.4232(2) 0.6043(3) 0.3899(2) 0.0344(11) Uani 1 d . . C8 C 0.5889(3) 0.6344(4) 0.4253(3) 0.0471(13) Uani 1 d . . H8A H 0.5524(3) 0.6195(4) 0.3936(3) 0.056 Uiso 1 calc R . C9 C 0.6364(3) 0.6098(4) 0.4055(3) 0.0543(15) Uani 1 d . . H9A H 0.6329(3) 0.5775(4) 0.3614(3) 0.065 Uiso 1 calc R . C10 C 0.6893(3) 0.6325(5) 0.4507(3) 0.058(2) Uani 1 d . . H10A H 0.7228(3) 0.6162(5) 0.4379(3) 0.070 Uiso 1 calc R . C11 C 0.6935(2) 0.6791(4) 0.5148(3) 0.0515(14) Uani 1 d . . H11A H 0.7298(2) 0.6947(4) 0.5466(3) 0.062 Uiso 1 calc R . C12 C 0.6442(2) 0.7027(4) 0.5321(3) 0.0383(11) Uani 1 d . . C13 C 0.6433(2) 0.7512(4) 0.5982(3) 0.0404(12) Uani 1 d . . C14 C 0.6912(2) 0.7911(4) 0.6485(3) 0.0532(15) Uani 1 d . . H14A H 0.7278(2) 0.7858(4) 0.6412(3) 0.064 Uiso 1 calc R . C15 C 0.6852(3) 0.8378(5) 0.7083(3) 0.057(2) Uani 1 d . . H15A H 0.7175(3) 0.8643(5) 0.7428(3) 0.068 Uiso 1 calc R . C16 C 0.6312(3) 0.8457(4) 0.7174(3) 0.0515(14) Uani 1 d . . H16A H 0.6258(3) 0.8798(4) 0.7573(3) 0.062 Uiso 1 calc R . C17 C 0.5854(2) 0.8036(4) 0.6680(3) 0.0432(12) Uani 1 d . . H17A H 0.5488(2) 0.8075(4) 0.6755(3) 0.052 Uiso 1 calc R . C18 C 0.5011(2) 0.8707(4) 0.4433(3) 0.0451(13) Uani 1 d . . H18A H 0.5352(2) 0.8571(4) 0.4311(3) 0.054 Uiso 1 calc R . C19 C 0.4680(3) 0.9482(4) 0.4107(3) 0.0551(15) Uani 1 d . . H19A H 0.4798(3) 0.9880(4) 0.3780(3) 0.066 Uiso 1 calc R . C20 C 0.4174(3) 0.9665(4) 0.4265(4) 0.060(2) Uani 1 d . . H20A H 0.3930(3) 1.0168(4) 0.4025(4) 0.072 Uiso 1 calc R . C21 C 0.4025(3) 0.9111(4) 0.4776(3) 0.0521(14) Uani 1 d . . H21A H 0.3690(3) 0.9247(4) 0.4910(3) 0.063 Uiso 1 calc R . C22 C 0.4379(2) 0.8354(4) 0.5086(3) 0.0421(12) Uani 1 d . . C23 C 0.4254(2) 0.7701(4) 0.5628(3) 0.0420(12) Uani 1 d . . C24 C 0.3784(3) 0.7778(4) 0.5886(3) 0.0525(14) Uani 1 d . . H24A H 0.3510(3) 0.8271(4) 0.5716(3) 0.063 Uiso 1 calc R . C25 C 0.3719(3) 0.7127(5) 0.6394(3) 0.057(2) Uani 1 d . . H25A H 0.3394(3) 0.7156(5) 0.6567(3) 0.069 Uiso 1 calc R . C26 C 0.4131(3) 0.6437(5) 0.6647(3) 0.0523(14) Uani 1 d . . H26A H 0.4098(3) 0.5994(5) 0.7005(3) 0.063 Uiso 1 calc R . C27 C 0.4593(2) 0.6395(4) 0.6373(3) 0.0448(12) Uani 1 d . . H27A H 0.4879(2) 0.5923(4) 0.6556(3) 0.054 Uiso 1 calc R . P P 0.14598(7) 0.42123(12) 0.35361(9) 0.0579(4) Uani 1 d . . F1 F 0.1915(2) 0.3457(4) 0.3474(3) 0.110(2) Uani 1 d . . F2 F 0.0985(2) 0.4955(4) 0.3611(3) 0.123(2) Uani 1 d . . F3 F 0.1833(2) 0.5077(4) 0.3458(3) 0.127(2) Uani 1 d . . F4 F 0.1054(2) 0.3390(4) 0.3658(3) 0.120(2) Uani 1 d . . F5 F 0.1167(2) 0.4201(4) 0.2698(2) 0.0990(15) Uani 1 d . . F6 F 0.1750(2) 0.4247(4) 0.4386(2) 0.0982(15) Uani 1 d . . O1 O 0.0000 0.5770(6) 0.2500 0.091(2) Uiso 1 d S . O2 O 0.2704(10) 0.9141(17) 0.3141(12) 0.092(6) Uiso 0.25 d P . C28 C 0.3019(4) 0.5928(6) 0.4585(5) 0.091(2) Uiso 1 d . . H28A H 0.2952(21) 0.5475(9) 0.4183(5) 0.109 Uiso 1 calc R 1 H28B H 0.2799(16) 0.5728(17) 0.4909(23) 0.109 Uiso 1 calc R 1 H28C H 0.3426(6) 0.5935(11) 0.4849(24) 0.109 Uiso 1 calc R 1 C29 C 0.2860(5) 0.6786(9) 0.4339(6) 0.077(3) Uiso 0.682(13) d P 1 N7 N 0.2732(5) 0.7574(10) 0.4153(7) 0.111(4) Uiso 0.682(13) d P 1 C29A C 0.2689(9) 0.6140(16) 0.5030(12) 0.064(6) Uiso 0.318(13) d P 2 N7A N 0.2449(10) 0.6164(17) 0.5419(12) 0.092(8) Uiso 0.318(13) d P 2 N8 N 0.0000 0.0528(6) 0.2500 0.069(2) Uiso 1 d S . C30 C 0.0000 0.2357(8) 0.2500 0.075(3) Uiso 1 d S . H30A H 0.0196(108) 0.2592(8) 0.2984(35) 0.090 Uiso 0.50 calc PR . H30B H -0.03944(3) 0.2592(8) 0.2355(151) 0.090 Uiso 0.50 calc PR . H30C H 0.0198(108) 0.2592(8) 0.2161(115) 0.090 Uiso 0.50 calc PR . C31 C 0.0000 0.1342(7) 0.2500 0.058(2) Uiso 1 d S . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru 0.0351(3) 0.0276(3) 0.0354(3) 0.0016(2) 0.0064(2) -0.0010(2) N1 0.037(2) 0.031(2) 0.036(2) 0.002(2) 0.006(2) 0.002(2) N2 0.036(2) 0.034(2) 0.041(2) 0.006(2) 0.007(2) 0.000(2) N3 0.045(3) 0.034(2) 0.040(2) 0.005(2) 0.009(2) 0.000(2) N4 0.045(2) 0.028(2) 0.038(2) 0.004(2) 0.013(2) -0.003(2) N5 0.042(2) 0.034(2) 0.040(2) 0.000(2) 0.009(2) -0.004(2) N6 0.040(2) 0.035(2) 0.039(2) 0.000(2) 0.005(2) -0.003(2) C1 0.036(3) 0.027(3) 0.038(3) 0.004(2) 0.003(2) 0.001(2) C2 0.032(2) 0.037(3) 0.035(3) 0.002(2) 0.011(2) 0.003(2) C3 0.037(3) 0.042(3) 0.039(3) -0.002(2) 0.010(2) 0.001(2) C4 0.038(3) 0.061(4) 0.039(3) 0.002(3) 0.000(2) 0.001(3) C5 0.048(3) 0.053(3) 0.047(3) 0.009(3) 0.004(3) 0.007(3) C6 0.044(3) 0.043(3) 0.043(3) 0.006(2) 0.007(2) 0.004(2) C7 0.034(2) 0.035(3) 0.035(2) 0.004(2) 0.012(2) 0.003(2) C8 0.058(3) 0.044(3) 0.040(3) -0.002(2) 0.016(3) -0.003(3) C9 0.067(4) 0.053(3) 0.049(3) -0.007(3) 0.027(3) -0.006(3) C10 0.054(4) 0.065(4) 0.062(4) 0.000(3) 0.026(3) -0.001(3) C11 0.040(3) 0.053(3) 0.063(4) 0.001(3) 0.017(3) -0.005(3) C12 0.038(3) 0.035(3) 0.040(3) 0.007(2) 0.008(2) 0.001(2) C13 0.038(3) 0.036(3) 0.044(3) 0.002(2) 0.006(2) -0.004(2) C14 0.043(3) 0.060(4) 0.053(3) -0.001(3) 0.008(3) -0.014(3) C15 0.054(4) 0.058(4) 0.050(3) -0.006(3) 0.002(3) -0.012(3) C16 0.065(4) 0.045(3) 0.040(3) -0.007(2) 0.009(3) -0.012(3) C17 0.053(3) 0.031(3) 0.045(3) -0.003(2) 0.014(2) -0.004(2) C18 0.054(3) 0.034(3) 0.046(3) 0.005(2) 0.013(3) -0.003(2) C19 0.072(4) 0.037(3) 0.054(3) 0.013(3) 0.015(3) 0.001(3) C20 0.062(4) 0.044(3) 0.073(4) 0.010(3) 0.016(3) 0.010(3) C21 0.052(3) 0.036(3) 0.067(4) 0.007(3) 0.016(3) 0.010(3) C22 0.045(3) 0.030(3) 0.049(3) -0.001(2) 0.010(2) -0.001(2) C23 0.043(3) 0.038(3) 0.043(3) -0.005(2) 0.010(2) 0.000(2) C24 0.050(3) 0.043(3) 0.065(4) -0.003(3) 0.017(3) 0.003(3) C25 0.051(3) 0.066(4) 0.060(4) -0.006(3) 0.023(3) -0.006(3) C26 0.057(4) 0.056(4) 0.051(3) 0.006(3) 0.027(3) -0.006(3) C27 0.048(3) 0.042(3) 0.042(3) 0.001(2) 0.010(2) -0.001(2) P 0.0581(10) 0.0432(8) 0.0657(10) 0.0068(7) 0.0073(8) 0.0015(7) F1 0.106(4) 0.134(4) 0.086(3) 0.001(3) 0.020(3) 0.064(3) F2 0.104(4) 0.104(4) 0.145(5) -0.012(3) 0.013(4) 0.043(3) F3 0.105(4) 0.103(4) 0.139(4) 0.049(3) -0.019(3) -0.053(3) F4 0.114(4) 0.089(3) 0.159(5) 0.026(3) 0.040(4) -0.030(3) F5 0.102(3) 0.108(3) 0.066(2) 0.004(2) -0.008(2) 0.003(3) F6 0.114(4) 0.101(3) 0.065(2) -0.001(2) 0.003(2) 0.020(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru N4 2.021(4) . ? Ru N6 2.034(4) . ? Ru N5 2.033(4) . ? Ru N3 2.043(4) . ? Ru N1 2.135(4) 5_666 ? Ru N2 2.139(4) . ? N1 C1 1.338(6) . ? N1 C2 1.391(6) . ? N1 Ru 2.135(4) 5_666 ? N2 C1 1.339(6) . ? N2 C7 1.393(6) . ? N3 C12 1.357(7) . ? N3 C8 1.362(7) . ? N4 C17 1.353(7) . ? N4 C13 1.369(7) . ? N5 C18 1.351(7) . ? N5 C22 1.358(7) . ? N6 C27 1.351(7) . ? N6 C23 1.361(7) . ? C1 C1 1.406(9) 5_666 ? C2 C3 1.408(7) . ? C2 C7 1.420(7) . ? C3 C4 1.368(8) . ? C4 C5 1.405(9) . ? C5 C6 1.372(8) . ? C6 C7 1.398(7) . ? C8 C9 1.371(8) . ? C9 C10 1.374(9) . ? C10 C11 1.382(9) . ? C11 C12 1.382(8) . ? C12 C13 1.457(7) . ? C13 C14 1.405(8) . ? C14 C15 1.378(9) . ? C15 C16 1.388(9) . ? C16 C17 1.377(8) . ? C18 C19 1.387(8) . ? C19 C20 1.382(9) . ? C20 C21 1.387(9) . ? C21 C22 1.386(8) . ? C22 C23 1.488(8) . ? C23 C24 1.386(8) . ? C24 C25 1.383(9) . ? C25 C26 1.376(9) . ? C26 C27 1.383(8) . ? P F3 1.543(5) . ? P F1 1.561(5) . ? P F4 1.577(5) . ? P F5 1.577(5) . ? P F2 1.593(5) . ? P F6 1.598(4) . ? C28 C29 1.304(14) . ? C29 N7 1.17(2) . ? C29A N7A 1.08(3) . ? N8 C31 1.132(11) . ? C30 C31 1.414(15) . ? 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 N4 Ru N6 98.4(2) . . ? N4 Ru N5 95.2(2) . . ? N6 Ru N5 79.0(2) . . ? N4 Ru N3 79.1(2) . . ? N6 Ru N3 176.7(2) . . ? N5 Ru N3 103.4(2) . . ? N4 Ru N1 93.2(2) . 5_666 ? N6 Ru N1 94.5(2) . 5_666 ? N5 Ru N1 170.1(2) . 5_666 ? N3 Ru N1 83.5(2) . 5_666 ? N4 Ru N2 172.3(2) . . ? N6 Ru N2 87.5(2) . . ? N5 Ru N2 90.8(2) . . ? N3 Ru N2 94.9(2) . . ? N1 Ru N2 81.32(15) 5_666 . ? C1 N1 C2 102.6(4) . . ? C1 N1 Ru 108.4(3) . 5_666 ? C2 N1 Ru 149.0(3) . 5_666 ? C1 N2 C7 102.8(4) . . ? C1 N2 Ru 108.3(3) . . ? C7 N2 Ru 148.9(3) . . ? C12 N3 C8 117.7(5) . . ? C12 N3 Ru 115.2(3) . . ? C8 N3 Ru 125.9(4) . . ? C17 N4 C13 118.8(4) . . ? C17 N4 Ru 125.7(4) . . ? C13 N4 Ru 115.5(3) . . ? C18 N5 C22 117.8(4) . . ? C18 N5 Ru 125.8(4) . . ? C22 N5 Ru 116.1(3) . . ? C27 N6 C23 117.9(5) . . ? C27 N6 Ru 125.4(4) . . ? C23 N6 Ru 116.6(3) . . ? N1 C1 N2 118.0(4) . . ? N1 C1 C1 121.0(6) . 5_666 ? N2 C1 C1 121.0(6) . 5_666 ? N1 C2 C3 131.0(5) . . ? N1 C2 C7 108.5(4) . . ? C3 C2 C7 120.5(4) . . ? C4 C3 C2 117.5(5) . . ? C3 C4 C5 121.8(5) . . ? C6 C5 C4 122.0(5) . . ? C5 C6 C7 117.4(5) . . ? N2 C7 C6 131.1(5) . . ? N2 C7 C2 108.0(4) . . ? C6 C7 C2 120.8(5) . . ? N3 C8 C9 122.8(5) . . ? C8 C9 C10 118.9(5) . . ? C9 C10 C11 119.5(6) . . ? C12 C11 C10 119.4(5) . . ? N3 C12 C11 121.7(5) . . ? N3 C12 C13 114.0(4) . . ? C11 C12 C13 124.3(5) . . ? N4 C13 C14 120.3(5) . . ? N4 C13 C12 114.8(4) . . ? C14 C13 C12 124.9(5) . . ? C15 C14 C13 120.1(5) . . ? C14 C15 C16 118.9(5) . . ? C17 C16 C15 119.4(5) . . ? N4 C17 C16 122.5(5) . . ? N5 C18 C19 122.4(5) . . ? C20 C19 C18 119.0(5) . . ? C19 C20 C21 119.6(5) . . ? C22 C21 C20 118.3(6) . . ? N5 C22 C21 122.9(5) . . ? N5 C22 C23 114.3(4) . . ? C21 C22 C23 122.8(5) . . ? N6 C23 C24 121.9(5) . . ? N6 C23 C22 113.3(5) . . ? C24 C23 C22 124.8(5) . . ? C25 C24 C23 119.2(5) . . ? C26 C25 C24 119.2(5) . . ? C25 C26 C27 119.2(5) . . ? N6 C27 C26 122.5(5) . . ? F3 P F1 93.6(4) . . ? F3 P F4 174.8(4) . . ? F1 P F4 90.9(4) . . ? F3 P F5 90.7(3) . . ? F1 P F5 92.0(3) . . ? F4 P F5 91.7(3) . . ? F3 P F2 88.3(4) . . ? F1 P F2 178.0(4) . . ? F4 P F2 87.1(4) . . ? F5 P F2 88.6(3) . . ? F3 P F6 88.8(3) . . ? F1 P F6 89.2(3) . . ? F4 P F6 88.7(3) . . ? F5 P F6 178.7(3) . . ? F2 P F6 90.2(3) . . ? N7 C29 C28 176.5(13) . . ? N8 C31 C30 180.000(2) . . ? _refine_diff_density_max 0.862 _refine_diff_density_min -0.747 _refine_diff_density_rms 0.080 data_fo1105 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H26 F6 N8 O6 Ru S2 * 3 H2 O' _chemical_formula_weight 999.34 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' '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 C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 22.0290(10) _cell_length_b 16.2900(10) _cell_length_c 13.3542(6) _cell_angle_alpha 90.00 _cell_angle_beta 122.214(2) _cell_angle_gamma 90.00 _cell_volume 4054.5(4) _cell_formula_units_Z 4 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour red-brown _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.629 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2002 _exptl_absorpt_coefficient_mu 0.581 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.8358 _exptl_absorpt_correction_T_max 0.9442 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 183(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 KappaCCD _diffrn_measurement_method 'phi- + omega-scan ' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20269 _diffrn_reflns_av_R_equivalents 0.1017 _diffrn_reflns_av_sigmaI/netI 0.0850 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.32 _diffrn_reflns_theta_max 27.48 _reflns_number_total 4590 _reflns_number_gt 3531 _reflns_threshold_expression >2sigma(I) _computing_data_collection COLLECT _computing_cell_refinement DENZO _computing_data_reduction DENZO _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL/PC _computing_publication_material SHELXL-97 _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1208P)^2^+26.6231P] 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 4590 _refine_ls_number_parameters 292 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.1283 _refine_ls_R_factor_gt 0.0954 _refine_ls_wR_factor_ref 0.2407 _refine_ls_wR_factor_gt 0.2229 _refine_ls_goodness_of_fit_ref 1.107 _refine_ls_restrained_S_all 1.109 _refine_ls_shift/su_max 0.006 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru Ru 0.0000 0.21538(4) 1.2500 0.0290(3) Uani 1 2 d S . . N1 N -0.0271(3) 0.1147(4) 1.1354(4) 0.0361(12) Uani 1 1 d . . . N2 N -0.0452(3) -0.0205(3) 1.1067(5) 0.0364(12) Uani 1 1 d . . . H1N2 H -0.0445 -0.0731 1.1224 0.044 Uiso 1 1 calc R . . N3 N 0.0999(3) 0.2197(3) 1.2712(4) 0.0366(12) Uani 1 1 d . . . N4 N -0.0156(3) 0.3035(3) 1.1293(5) 0.0376(13) Uani 1 1 d . . . C1 C -0.0175(3) 0.0413(4) 1.1859(5) 0.0320(13) Uani 1 1 d . . . C2 C -0.0641(3) 0.1004(4) 1.0126(5) 0.0339(14) Uani 1 1 d . . . C3 C -0.0889(4) 0.1535(5) 0.9163(5) 0.0416(16) Uani 1 1 d . . . H3A H -0.0805 0.2110 0.9271 0.050 Uiso 1 1 calc R . . C4 C -0.1268(4) 0.1185(5) 0.8030(6) 0.0463(17) Uani 1 1 d . . . H4A H -0.1451 0.1530 0.7356 0.056 Uiso 1 1 calc R . . C5 C -0.1382(4) 0.0334(5) 0.7869(6) 0.0479(18) Uani 1 1 d . . . H5A H -0.1643 0.0119 0.7087 0.057 Uiso 1 1 calc R . . C6 C -0.1126(4) -0.0201(5) 0.8817(6) 0.0431(16) Uani 1 1 d . . . H6A H -0.1199 -0.0777 0.8703 0.052 Uiso 1 1 calc R . . C7 C -0.0749(3) 0.0148(4) 0.9962(6) 0.0357(14) Uani 1 1 d . . . C8 C 0.1584(4) 0.1764(5) 1.3513(6) 0.0409(15) Uani 1 1 d . . . H8A H 0.1553 0.1428 1.4064 0.049 Uiso 1 1 calc R . . C9 C 0.2226(4) 0.1793(6) 1.3560(7) 0.0518(19) Uani 1 1 d . . . H9A H 0.2630 0.1492 1.4147 0.062 Uiso 1 1 calc R . . C10 C 0.2277(4) 0.2274(6) 1.2728(8) 0.058(2) Uani 1 1 d . . . H10A H 0.2706 0.2291 1.2721 0.069 Uiso 1 1 calc R . . C11 C 0.1682(5) 0.2719(5) 1.1929(7) 0.0523(19) Uani 1 1 d . . . H11A H 0.1703 0.3058 1.1369 0.063 Uiso 1 1 calc R . . C12 C 0.1051(4) 0.2679(4) 1.1928(6) 0.0415(16) Uani 1 1 d . . . C13 C 0.0391(4) 0.3148(4) 1.1110(6) 0.0408(16) Uani 1 1 d . . . C14 C 0.0322(5) 0.3662(5) 1.0225(7) 0.057(2) Uani 1 1 d . . . H14A H 0.0704 0.3719 1.0093 0.069 Uiso 1 1 calc R . . C15 C -0.0312(5) 0.4090(6) 0.9540(7) 0.067(3) Uani 1 1 d . . . H15A H -0.0372 0.4438 0.8923 0.080 Uiso 1 1 calc R . . C16 C -0.0857(5) 0.4013(6) 0.9752(7) 0.065(3) Uani 1 1 d . . . H16A H -0.1290 0.4315 0.9300 0.078 Uiso 1 1 calc R . . C17 C -0.0758(4) 0.3487(5) 1.0636(6) 0.0499(18) Uani 1 1 d . . . H17A H -0.1130 0.3439 1.0792 0.060 Uiso 1 1 calc R . . S S -0.29608(19) 0.1127(3) 0.4239(3) 0.1087(12) Uani 1 1 d D . . O1 O -0.3484(5) 0.1603(6) 0.3206(7) 0.138(4) Uani 1 1 d D A . O2 O -0.3173(6) 0.0951(8) 0.5090(8) 0.128(3) Uiso 1 1 d D A . O3 O -0.2199(3) 0.1288(11) 0.4741(9) 0.177(6) Uani 1 1 d D A . C18 C -0.2991(4) 0.0159(6) 0.3670(6) 0.074(3) Uani 1 1 d D A . F1 F -0.2880(4) 0.0187(5) 0.2765(5) 0.107(2) Uani 1 1 d D . . F2 F -0.2535(7) -0.0424(7) 0.4410(8) 0.177(5) Uani 1 1 d D . . F3 F -0.3642(5) -0.0223(6) 0.3101(8) 0.148(4) Uani 1 1 d D . . O4 O 0.0000 0.3089(7) 0.7500 0.103(4) Uani 1 2 d S . . O5 O 0.0739(3) 0.1829(4) 0.9127(6) 0.0641(16) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru 0.0273(4) 0.0311(4) 0.0182(3) 0.000 0.0052(3) 0.000 N1 0.031(3) 0.045(3) 0.024(2) -0.002(2) 0.009(2) -0.001(2) N2 0.035(3) 0.035(3) 0.035(3) -0.006(2) 0.015(2) -0.003(2) N3 0.037(3) 0.037(3) 0.024(2) -0.003(2) 0.009(2) -0.003(2) N4 0.040(3) 0.031(3) 0.024(3) -0.003(2) 0.005(2) -0.002(2) C1 0.024(3) 0.035(3) 0.027(3) -0.003(3) 0.008(2) 0.000(2) C2 0.030(3) 0.042(4) 0.026(3) -0.005(3) 0.012(3) -0.004(3) C3 0.044(4) 0.048(4) 0.024(3) -0.004(3) 0.012(3) -0.001(3) C4 0.042(4) 0.064(5) 0.026(3) -0.003(3) 0.013(3) 0.006(3) C5 0.035(4) 0.066(5) 0.032(3) -0.016(3) 0.010(3) 0.001(3) C6 0.037(4) 0.048(4) 0.037(4) -0.015(3) 0.015(3) -0.006(3) C7 0.032(3) 0.039(4) 0.031(3) -0.010(3) 0.014(3) -0.004(3) C8 0.033(3) 0.047(4) 0.030(3) 0.004(3) 0.008(3) 0.000(3) C9 0.031(4) 0.071(5) 0.041(4) 0.000(4) 0.011(3) -0.001(3) C10 0.040(4) 0.076(6) 0.055(5) -0.005(4) 0.024(4) -0.013(4) C11 0.055(5) 0.057(5) 0.046(4) 0.003(3) 0.028(4) -0.008(4) C12 0.046(4) 0.041(4) 0.030(3) -0.005(3) 0.015(3) -0.010(3) C13 0.048(4) 0.038(3) 0.026(3) 0.002(3) 0.013(3) -0.007(3) C14 0.062(5) 0.059(5) 0.038(4) 0.011(4) 0.018(4) -0.013(4) C15 0.063(5) 0.065(6) 0.034(4) 0.020(4) 0.000(4) -0.014(4) C16 0.055(5) 0.057(5) 0.038(4) 0.020(4) -0.004(4) -0.001(4) C17 0.042(4) 0.043(4) 0.040(4) 0.005(3) 0.005(3) -0.002(3) S 0.095(2) 0.140(3) 0.078(2) -0.018(2) 0.0370(19) -0.001(2) O1 0.104(7) 0.119(8) 0.122(8) -0.003(6) 0.014(6) 0.044(6) O3 0.053(5) 0.34(2) 0.099(7) 0.018(10) 0.012(5) -0.021(8) C18 0.068(6) 0.092(8) 0.063(6) 0.014(5) 0.035(5) 0.011(6) F1 0.109(5) 0.153(7) 0.062(4) 0.021(4) 0.048(4) 0.036(5) F2 0.228(12) 0.172(9) 0.114(7) 0.087(7) 0.079(7) 0.120(9) F3 0.181(9) 0.123(7) 0.112(7) -0.006(6) 0.060(7) -0.030(7) O4 0.160(12) 0.061(6) 0.054(6) 0.000 0.034(7) 0.000 O5 0.060(4) 0.052(3) 0.066(4) -0.006(3) 0.024(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 Ru N4 2.046(6) 2_557 ? Ru N4 2.046(6) . ? Ru N3 2.066(6) . ? Ru N3 2.066(6) 2_557 ? Ru N1 2.100(6) 2_557 ? Ru N1 2.101(6) . ? N1 C1 1.333(8) . ? N1 C2 1.408(8) . ? N2 C1 1.348(8) . ? N2 C7 1.381(9) . ? N3 C8 1.353(9) . ? N3 C12 1.361(9) . ? N4 C17 1.353(9) . ? N4 C13 1.363(9) . ? C1 C1 1.456(12) 2_557 ? C2 C3 1.398(9) . ? C2 C7 1.411(9) . ? C3 C4 1.402(9) . ? C4 C5 1.405(11) . ? C5 C6 1.385(11) . ? C6 C7 1.414(9) . ? C8 C9 1.382(10) . ? C9 C10 1.412(12) . ? C10 C11 1.374(12) . ? C11 C12 1.391(11) . ? C12 C13 1.482(10) . ? C13 C14 1.390(10) . ? C14 C15 1.382(12) . ? C15 C16 1.378(14) . ? C16 C17 1.379(11) . ? S O3 1.461(3) . ? S O1 1.462(3) . ? S O2 1.469(3) . ? S C18 1.736(10) . ? C18 F2 1.353(3) . ? C18 F1 1.355(3) . ? C18 F3 1.363(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N4 Ru N4 90.9(3) 2_557 . ? N4 Ru N3 98.6(2) 2_557 . ? N4 Ru N3 78.6(2) . . ? N4 Ru N3 78.6(2) 2_557 2_557 ? N4 Ru N3 98.6(2) . 2_557 ? N3 Ru N3 176.1(3) . 2_557 ? N4 Ru N1 96.3(2) 2_557 2_557 ? N4 Ru N1 169.9(2) . 2_557 ? N3 Ru N1 93.3(2) . 2_557 ? N3 Ru N1 89.7(2) 2_557 2_557 ? N4 Ru N1 169.9(2) 2_557 . ? N4 Ru N1 96.3(2) . . ? N3 Ru N1 89.7(2) . . ? N3 Ru N1 93.3(2) 2_557 . ? N1 Ru N1 77.4(3) 2_557 . ? C1 N1 C2 106.1(5) . . ? C1 N1 Ru 115.2(4) . . ? C2 N1 Ru 137.8(5) . . ? C1 N2 C7 106.5(5) . . ? C8 N3 C12 118.3(6) . . ? C8 N3 Ru 126.0(5) . . ? C12 N3 Ru 115.7(5) . . ? C17 N4 C13 117.8(6) . . ? C17 N4 Ru 125.9(5) . . ? C13 N4 Ru 116.3(4) . . ? N1 C1 N2 113.0(5) . . ? N1 C1 C1 115.9(3) . 2_557 ? N2 C1 C1 131.0(4) . 2_557 ? C3 C2 N1 131.9(6) . . ? C3 C2 C7 121.2(6) . . ? N1 C2 C7 106.8(6) . . ? C2 C3 C4 117.2(7) . . ? C3 C4 C5 121.5(7) . . ? C6 C5 C4 121.9(6) . . ? C5 C6 C7 117.0(7) . . ? N2 C7 C2 107.6(5) . . ? N2 C7 C6 131.2(7) . . ? C2 C7 C6 121.2(6) . . ? N3 C8 C9 122.6(7) . . ? C8 C9 C10 119.4(7) . . ? C11 C10 C9 117.4(7) . . ? C10 C11 C12 121.0(7) . . ? N3 C12 C11 121.2(7) . . ? N3 C12 C13 114.4(6) . . ? C11 C12 C13 124.4(6) . . ? N4 C13 C14 121.8(7) . . ? N4 C13 C12 114.4(6) . . ? C14 C13 C12 123.8(7) . . ? C15 C14 C13 118.7(8) . . ? C14 C15 C16 120.1(7) . . ? C17 C16 C15 118.4(8) . . ? N4 C17 C16 123.0(8) . . ? O3 S O1 118.3(8) . . ? O3 S O2 116.2(7) . . ? O1 S O2 114.6(7) . . ? O3 S C18 97.5(8) . . ? O1 S C18 104.0(5) . . ? O2 S C18 102.0(6) . . ? F2 C18 F1 105.0(7) . . ? F2 C18 F3 103.7(10) . . ? F1 C18 F3 98.9(8) . . ? F2 C18 S 118.5(8) . . ? F1 C18 S 112.1(6) . . ? F3 C18 S 116.2(6) . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 1.154 _refine_diff_density_min -1.579 _refine_diff_density_rms 0.148