# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_a _database_code_depnum_ccdc_archive 'CCDC 879990' #TrackingRef 'web_deposit_cif_file_0_Yu-WuZhong_1336015759.a.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C49 H49 N8 O2 Ru, F6 P' _chemical_formula_sum 'C49 H49 F6 N8 O2 P Ru' _chemical_formula_weight 1028.00 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' Ru Ru -1.2594 0.8363 '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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M P4(2)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-y, x+1/2, z+1/2' 'y+1/2, -x, z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'y, -x-1/2, -z-1/2' '-y-1/2, x, -z-1/2' _cell_length_a 12.0094(17) _cell_length_b 12.0094(17) _cell_length_c 32.467(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4682.5(13) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 13363 _cell_measurement_theta_min 1.2544 _cell_measurement_theta_max 27.4715 _exptl_crystal_description plate _exptl_crystal_colour black _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.458 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2112 _exptl_absorpt_coefficient_mu 0.442 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7855 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'CrystalClear (Rigaku Inc., 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Rotating Anode' _diffrn_radiation_monochromator Confocal _diffrn_measurement_device_type 'MM007HF + CCD (Saturn724+)' _diffrn_measurement_method '\w scans at fixed \c = 45\%' _diffrn_detector_area_resol_mean 28.5714 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 32058 _diffrn_reflns_av_R_equivalents 0.0728 _diffrn_reflns_av_sigmaI/netI 0.0442 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -41 _diffrn_reflns_limit_l_max 41 _diffrn_reflns_theta_min 1.81 _diffrn_reflns_theta_max 27.45 _reflns_number_total 5352 _reflns_number_gt 4793 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2008)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2008)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2008)' _computing_structure_solution 'SHELX-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELX-97 (Sheldrick, 2008)' _computing_molecular_graphics ; Mercury: visualization and analysis of crystal structures, C. F. Macrae, P. R. Edgington, P. McCabe, E. Pidcock, G. P. Shields, R. Taylor, M. Towler and J. van de Streek, J. Appl. Cryst., 39, 453-457, 2006. ; _computing_publication_material 'SHELX-97 (Sheldrick, 2008)' _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^)+(0.1217P)^2^+38.1533P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5352 _refine_ls_number_parameters 289 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1190 _refine_ls_R_factor_gt 0.1079 _refine_ls_wR_factor_ref 0.2820 _refine_ls_wR_factor_gt 0.2735 _refine_ls_goodness_of_fit_ref 1.142 _refine_ls_restrained_S_all 1.142 _refine_ls_shift/su_max 0.007 _refine_ls_shift/su_mean 0.001 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 Ru1 Ru 0.7500 0.2500 0.22387(2) 0.0194(2) Uani 1 2 d S . . O1 O 0.9340(5) 0.6081(5) -0.05328(17) 0.0462(14) Uani 1 1 d . . . N1 N 0.6817(5) 0.4295(5) 0.28127(17) 0.0253(11) Uani 1 1 d . . . N2 N 0.6453(5) 0.4990(5) 0.22201(17) 0.0280(12) Uani 1 1 d . . . N3 N 0.7500 0.2500 0.1616(2) 0.0230(15) Uani 1 2 d S . . N4 N 0.9045(4) 0.3183(4) 0.21030(15) 0.0197(10) Uani 1 1 d . . . C1 C 0.7500 0.2500 0.2863(3) 0.0233(17) Uani 1 2 d S . . C2 C 0.7159(5) 0.3421(6) 0.3084(2) 0.0262(13) Uani 1 1 d . . . C3 C 0.7159(6) 0.3458(7) 0.3513(2) 0.0347(16) Uani 1 1 d . . . H3 H 0.6936 0.4107 0.3659 0.042 Uiso 1 1 calc R . . C4 C 0.7500 0.2500 0.3717(3) 0.041(3) Uani 1 2 d S . . H4 H 0.7500 0.2500 0.4010 0.049 Uiso 1 2 calc SR . . C5 C 0.6838(5) 0.4055(5) 0.2397(2) 0.0235(13) Uani 1 1 d . . . C6 C 0.6428(5) 0.5360(6) 0.2882(2) 0.0300(14) Uani 1 1 d . . . H6 H 0.6340 0.5715 0.3142 0.036 Uiso 1 1 calc R . . C7 C 0.6197(6) 0.5796(6) 0.2511(2) 0.0324(15) Uani 1 1 d . . . H7 H 0.5913 0.6520 0.2458 0.039 Uiso 1 1 calc R . . C8 C 0.6269(6) 0.5114(6) 0.1773(2) 0.0350(16) Uani 1 1 d . . . H8A H 0.6787 0.4616 0.1623 0.042 Uiso 1 1 calc R . . H8B H 0.6438 0.5890 0.1691 0.042 Uiso 1 1 calc R . . C9 C 0.5066(6) 0.4832(7) 0.1649(2) 0.0350(16) Uani 1 1 d . . . H9A H 0.4876 0.4082 0.1754 0.042 Uiso 1 1 calc R . . H9B H 0.4555 0.5373 0.1780 0.042 Uiso 1 1 calc R . . C10 C 0.4890(7) 0.4856(7) 0.1190(2) 0.0437(19) Uani 1 1 d . . . H10A H 0.5379 0.4294 0.1060 0.052 Uiso 1 1 calc R . . H10B H 0.5107 0.5597 0.1083 0.052 Uiso 1 1 calc R . . C11 C 0.3681(7) 0.4620(9) 0.1070(3) 0.053(2) Uani 1 1 d . . . H11B H 0.3619 0.4593 0.0769 0.080 Uiso 1 1 calc R . . H11C H 0.3201 0.5212 0.1178 0.080 Uiso 1 1 calc R . . H11A H 0.3450 0.3903 0.1186 0.080 Uiso 1 1 calc R . . C12 C 0.9841(5) 0.3454(5) 0.2374(2) 0.0240(12) Uani 1 1 d . . . H12 H 0.9699 0.3350 0.2660 0.029 Uiso 1 1 calc R . . C13 C 1.0862(6) 0.3881(6) 0.2255(2) 0.0301(15) Uani 1 1 d . . . H13 H 1.1414 0.4046 0.2456 0.036 Uiso 1 1 calc R . . C14 C 1.1077(6) 0.4065(6) 0.1841(2) 0.0345(16) Uani 1 1 d . . . H14 H 1.1774 0.4356 0.1754 0.041 Uiso 1 1 calc R . . C15 C 1.0252(6) 0.3816(6) 0.1555(2) 0.0292(14) Uani 1 1 d . . . H15 H 1.0371 0.3961 0.1271 0.035 Uiso 1 1 calc R . . C16 C 0.9251(6) 0.3355(5) 0.1687(2) 0.0259(13) Uani 1 1 d . . . C17 C 0.8357(5) 0.2973(5) 0.14104(19) 0.0254(13) Uani 1 1 d . . . C18 C 0.8355(6) 0.3034(5) 0.09820(19) 0.0279(14) Uani 1 1 d . . . H18 H 0.8922 0.3430 0.0840 0.034 Uiso 1 1 calc R . . C19 C 0.7500 0.2500 0.0763(3) 0.031(2) Uani 1 2 d S . . N5 N 0.7500 0.2500 0.0332(3) 0.040(2) Uani 1 2 d S . . C20 C 0.7941(6) 0.3417(6) 0.0109(2) 0.0315(15) Uani 1 1 d . . . C21 C 0.7658(7) 0.4498(7) 0.0214(2) 0.0390(18) Uani 1 1 d . . . H21 H 0.7141 0.4617 0.0431 0.047 Uiso 1 1 calc R . . C22 C 0.8102(6) 0.5414(7) 0.0012(2) 0.0391(17) Uani 1 1 d . . . H22 H 0.7912 0.6150 0.0093 0.047 Uiso 1 1 calc R . . C23 C 0.8836(6) 0.5222(7) -0.0313(2) 0.0355(17) Uani 1 1 d . . . C24 C 0.9118(7) 0.4164(7) -0.0432(2) 0.0422(19) Uani 1 1 d . . . H24 H 0.9613 0.4051 -0.0657 0.051 Uiso 1 1 calc R . . C25 C 0.8671(7) 0.3244(7) -0.0220(2) 0.0382(17) Uani 1 1 d . . . H25 H 0.8865 0.2509 -0.0300 0.046 Uiso 1 1 calc R . . C26 C 0.9106(9) 0.7179(9) -0.0413(4) 0.068(3) Uani 1 1 d . . . H26C H 0.9512 0.7697 -0.0591 0.102 Uiso 1 1 calc R . . H26B H 0.9338 0.7290 -0.0126 0.102 Uiso 1 1 calc R . . H26A H 0.8305 0.7317 -0.0437 0.102 Uiso 1 1 calc R . . P1 P 0.7500 0.7500 0.10012(11) 0.0496(8) Uiso 1 2 d S . . F1 F 0.7452(5) 0.8830(5) 0.0995(2) 0.0695(16) Uiso 1 1 d . . . F2 F 0.7500 0.7500 0.1484(5) 0.144(5) Uiso 1 2 d S . . F3 F 0.7500 0.7500 0.0562(10) 0.282(13) Uiso 1 2 d S . . F4 F 0.6226(13) 0.7459(13) 0.1160(4) 0.188(5) 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 Ru1 0.0240(4) 0.0186(4) 0.0157(4) 0.000 0.000 -0.0032(3) O1 0.047(3) 0.056(4) 0.036(3) 0.017(3) 0.008(2) -0.011(3) N1 0.026(3) 0.024(3) 0.025(3) -0.003(2) 0.004(2) -0.005(2) N2 0.031(3) 0.024(3) 0.030(3) 0.002(2) -0.001(2) 0.002(2) N3 0.021(4) 0.030(4) 0.018(3) 0.000 0.000 -0.001(3) N4 0.025(3) 0.015(2) 0.020(2) -0.0004(19) 0.000(2) -0.0023(19) C1 0.027(4) 0.025(4) 0.018(4) 0.000 0.000 0.003(4) C2 0.021(3) 0.028(3) 0.029(3) 0.001(3) 0.003(2) -0.002(3) C3 0.034(4) 0.048(4) 0.022(3) -0.010(3) 0.000(3) 0.001(3) C4 0.056(7) 0.044(6) 0.023(5) 0.000 0.000 0.006(5) C5 0.026(3) 0.018(3) 0.026(3) 0.001(2) -0.001(2) 0.000(2) C6 0.025(3) 0.028(3) 0.038(4) -0.010(3) 0.007(3) 0.000(3) C7 0.027(3) 0.021(3) 0.049(4) -0.007(3) 0.005(3) 0.003(3) C8 0.038(4) 0.033(4) 0.033(4) 0.013(3) 0.003(3) 0.005(3) C9 0.034(4) 0.041(4) 0.030(4) 0.001(3) 0.002(3) 0.008(3) C10 0.049(5) 0.046(5) 0.036(4) -0.005(3) -0.003(4) 0.010(4) C11 0.043(5) 0.063(6) 0.055(5) -0.012(5) -0.019(4) 0.011(4) C12 0.028(3) 0.018(3) 0.025(3) 0.001(2) 0.000(3) 0.003(2) C13 0.030(4) 0.030(3) 0.030(4) -0.002(3) -0.005(3) -0.006(3) C14 0.026(3) 0.035(4) 0.042(4) -0.004(3) 0.006(3) -0.013(3) C15 0.029(3) 0.030(3) 0.029(3) 0.000(3) 0.004(3) -0.009(3) C16 0.034(3) 0.020(3) 0.024(3) -0.004(2) 0.005(3) -0.004(3) C17 0.029(3) 0.028(3) 0.019(3) 0.001(2) 0.002(2) -0.007(3) C18 0.037(4) 0.026(3) 0.021(3) 0.001(2) 0.004(3) -0.010(3) C19 0.045(6) 0.033(5) 0.016(4) 0.000 0.000 -0.015(4) N5 0.050(6) 0.049(6) 0.020(4) 0.000 0.000 -0.023(5) C20 0.035(4) 0.041(4) 0.018(3) 0.005(3) -0.001(3) -0.011(3) C21 0.040(4) 0.048(5) 0.029(4) 0.010(3) 0.010(3) -0.003(3) C22 0.033(4) 0.046(4) 0.039(4) 0.012(3) 0.004(3) 0.004(3) C23 0.025(3) 0.054(5) 0.027(3) 0.012(3) -0.004(3) -0.014(3) C24 0.044(4) 0.058(5) 0.024(3) -0.001(3) 0.008(3) -0.019(4) C25 0.042(4) 0.042(4) 0.031(4) -0.006(3) 0.003(3) -0.016(3) C26 0.052(6) 0.061(6) 0.092(8) 0.034(6) 0.030(6) 0.009(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 Ru1 N3 2.023(8) . ? Ru1 C1 2.028(9) . ? Ru1 N4 2.076(5) . ? Ru1 N4 2.076(5) 2_655 ? Ru1 C5 2.093(6) 2_655 ? Ru1 C5 2.093(6) . ? O1 C23 1.392(9) . ? O1 C26 1.404(12) . ? N1 C6 1.380(8) . ? N1 C5 1.381(8) . ? N1 C2 1.430(9) . ? N2 C5 1.344(8) . ? N2 C7 1.387(9) . ? N2 C8 1.477(9) . ? N3 C17 1.352(7) . ? N3 C17 1.352(7) 2_655 ? N4 C12 1.340(8) . ? N4 C16 1.390(8) . ? C1 C2 1.380(8) 2_655 ? C1 C2 1.380(8) . ? C2 C3 1.395(9) . ? C3 C4 1.390(9) . ? C3 H3 0.9500 . ? C4 C3 1.390(9) 2_655 ? C4 H4 0.9500 . ? C6 C7 1.341(11) . ? C6 H6 0.9500 . ? C7 H7 0.9500 . ? C8 C9 1.537(10) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.504(10) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C11 1.529(12) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C11 H11A 0.9800 . ? C12 C13 1.385(10) . ? C12 H12 0.9500 . ? C13 C14 1.387(10) . ? C13 H13 0.9500 . ? C14 C15 1.388(10) . ? C14 H14 0.9500 . ? C15 C16 1.391(9) . ? C15 H15 0.9500 . ? C16 C17 1.471(9) . ? C17 C18 1.393(9) . ? C18 C19 1.403(8) . ? C18 H18 0.9500 . ? C19 N5 1.401(12) . ? C19 C18 1.403(8) 2_655 ? N5 C20 1.419(8) . ? N5 C20 1.419(8) 2_655 ? C20 C21 1.384(11) . ? C20 C25 1.399(10) . ? C21 C22 1.387(11) . ? C21 H21 0.9500 . ? C22 C23 1.394(11) . ? C22 H22 0.9500 . ? C23 C24 1.371(12) . ? C24 C25 1.408(11) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? C26 H26C 0.9800 . ? C26 H26B 0.9800 . ? C26 H26A 0.9800 . ? P1 F3 1.43(3) . ? P1 F2 1.568(16) . ? P1 F1 1.599(6) 2_665 ? P1 F1 1.599(6) . ? P1 F4 1.615(15) 2_665 ? P1 F4 1.615(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 N3 Ru1 C1 180.000(1) . . ? N3 Ru1 N4 77.75(14) . . ? C1 Ru1 N4 102.25(14) . . ? N3 Ru1 N4 77.75(14) . 2_655 ? C1 Ru1 N4 102.25(14) . 2_655 ? N4 Ru1 N4 155.5(3) . 2_655 ? N3 Ru1 C5 104.20(17) . 2_655 ? C1 Ru1 C5 75.80(17) . 2_655 ? N4 Ru1 C5 93.7(2) . 2_655 ? N4 Ru1 C5 92.2(2) 2_655 2_655 ? N3 Ru1 C5 104.20(17) . . ? C1 Ru1 C5 75.80(17) . . ? N4 Ru1 C5 92.2(2) . . ? N4 Ru1 C5 93.7(2) 2_655 . ? C5 Ru1 C5 151.6(3) 2_655 . ? C23 O1 C26 117.8(7) . . ? C6 N1 C5 111.1(6) . . ? C6 N1 C2 132.6(6) . . ? C5 N1 C2 116.3(5) . . ? C5 N2 C7 111.6(6) . . ? C5 N2 C8 123.8(6) . . ? C7 N2 C8 124.6(6) . . ? C17 N3 C17 120.9(8) . 2_655 ? C17 N3 Ru1 119.5(4) . . ? C17 N3 Ru1 119.5(4) 2_655 . ? C12 N4 C16 118.5(5) . . ? C12 N4 Ru1 126.5(4) . . ? C16 N4 Ru1 115.1(4) . . ? C2 C1 C2 117.5(9) 2_655 . ? C2 C1 Ru1 121.3(4) 2_655 . ? C2 C1 Ru1 121.3(4) . . ? C1 C2 C3 123.0(7) . . ? C1 C2 N1 110.7(6) . . ? C3 C2 N1 126.3(6) . . ? C4 C3 C2 116.7(7) . . ? C4 C3 H3 121.6 . . ? C2 C3 H3 121.6 . . ? C3 C4 C3 123.1(10) . 2_655 ? C3 C4 H4 118.5 . . ? C3 C4 H4 118.5 2_655 . ? N2 C5 N1 103.7(5) . . ? N2 C5 Ru1 140.5(5) . . ? N1 C5 Ru1 115.7(4) . . ? C7 C6 N1 106.5(6) . . ? C7 C6 H6 126.7 . . ? N1 C6 H6 126.7 . . ? C6 C7 N2 107.1(6) . . ? C6 C7 H7 126.4 . . ? N2 C7 H7 126.4 . . ? N2 C8 C9 112.0(6) . . ? N2 C8 H8A 109.2 . . ? C9 C8 H8A 109.2 . . ? N2 C8 H8B 109.2 . . ? C9 C8 H8B 109.2 . . ? H8A C8 H8B 107.9 . . ? C10 C9 C8 112.8(6) . . ? C10 C9 H9A 109.0 . . ? C8 C9 H9A 109.0 . . ? C10 C9 H9B 109.0 . . ? C8 C9 H9B 109.0 . . ? H9A C9 H9B 107.8 . . ? C9 C10 C11 112.5(7) . . ? C9 C10 H10A 109.1 . . ? C11 C10 H10A 109.1 . . ? C9 C10 H10B 109.1 . . ? C11 C10 H10B 109.1 . . ? H10A C10 H10B 107.8 . . ? C10 C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C11 H11A 109.5 . . ? H11B C11 H11A 109.5 . . ? H11C C11 H11A 109.5 . . ? N4 C12 C13 122.5(6) . . ? N4 C12 H12 118.7 . . ? C13 C12 H12 118.7 . . ? C12 C13 C14 119.7(6) . . ? C12 C13 H13 120.2 . . ? C14 C13 H13 120.2 . . ? C13 C14 C15 118.7(6) . . ? C13 C14 H14 120.7 . . ? C15 C14 H14 120.7 . . ? C14 C15 C16 119.9(6) . . ? C14 C15 H15 120.1 . . ? C16 C15 H15 120.1 . . ? N4 C16 C15 120.7(6) . . ? N4 C16 C17 114.6(5) . . ? C15 C16 C17 124.6(6) . . ? N3 C17 C18 120.8(6) . . ? N3 C17 C16 112.7(6) . . ? C18 C17 C16 126.4(6) . . ? C17 C18 C19 118.9(6) . . ? C17 C18 H18 120.5 . . ? C19 C18 H18 120.5 . . ? N5 C19 C18 120.4(4) . 2_655 ? N5 C19 C18 120.4(4) . . ? C18 C19 C18 119.2(8) 2_655 . ? C19 N5 C20 120.6(4) . . ? C19 N5 C20 120.6(4) . 2_655 ? C20 N5 C20 118.9(8) . 2_655 ? C21 C20 C25 118.7(7) . . ? C21 C20 N5 120.8(6) . . ? C25 C20 N5 120.5(7) . . ? C20 C21 C22 122.3(7) . . ? C20 C21 H21 118.9 . . ? C22 C21 H21 118.9 . . ? C21 C22 C23 118.0(8) . . ? C21 C22 H22 121.0 . . ? C23 C22 H22 121.0 . . ? C24 C23 O1 115.8(7) . . ? C24 C23 C22 121.5(7) . . ? O1 C23 C22 122.7(8) . . ? C23 C24 C25 119.7(7) . . ? C23 C24 H24 120.2 . . ? C25 C24 H24 120.2 . . ? C20 C25 C24 119.8(8) . . ? C20 C25 H25 120.1 . . ? C24 C25 H25 120.1 . . ? O1 C26 H26C 109.5 . . ? O1 C26 H26B 109.5 . . ? H26C C26 H26B 109.5 . . ? O1 C26 H26A 109.5 . . ? H26C C26 H26A 109.5 . . ? H26B C26 H26A 109.5 . . ? F3 P1 F2 180.000(2) . . ? F3 P1 F1 89.3(3) . 2_665 ? F2 P1 F1 90.7(3) . 2_665 ? F3 P1 F1 89.3(3) . . ? F2 P1 F1 90.7(3) . . ? F1 P1 F1 178.6(5) 2_665 . ? F3 P1 F4 108.7(5) . 2_665 ? F2 P1 F4 71.3(5) . 2_665 ? F1 P1 F4 90.0(6) 2_665 2_665 ? F1 P1 F4 90.4(6) . 2_665 ? F3 P1 F4 108.7(5) . . ? F2 P1 F4 71.3(5) . . ? F1 P1 F4 90.4(6) 2_665 . ? F1 P1 F4 90.0(6) . . ? F4 P1 F4 142.7(11) 2_665 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 Ru1 N3 C17 151(100) . . . . ? N4 Ru1 N3 C17 -5.0(4) . . . . ? N4 Ru1 N3 C17 175.0(4) 2_655 . . . ? C5 Ru1 N3 C17 -95.8(4) 2_655 . . . ? C5 Ru1 N3 C17 84.2(4) . . . . ? C1 Ru1 N3 C17 -29(100) . . . 2_655 ? N4 Ru1 N3 C17 175.0(4) . . . 2_655 ? N4 Ru1 N3 C17 -5.0(4) 2_655 . . 2_655 ? C5 Ru1 N3 C17 84.2(4) 2_655 . . 2_655 ? C5 Ru1 N3 C17 -95.8(4) . . . 2_655 ? N3 Ru1 N4 C12 -175.3(5) . . . . ? C1 Ru1 N4 C12 4.7(5) . . . . ? N4 Ru1 N4 C12 -175.3(5) 2_655 . . . ? C5 Ru1 N4 C12 -71.6(5) 2_655 . . . ? C5 Ru1 N4 C12 80.6(5) . . . . ? N3 Ru1 N4 C16 4.1(4) . . . . ? C1 Ru1 N4 C16 -175.9(4) . . . . ? N4 Ru1 N4 C16 4.1(4) 2_655 . . . ? C5 Ru1 N4 C16 107.8(4) 2_655 . . . ? C5 Ru1 N4 C16 -100.0(4) . . . . ? N3 Ru1 C1 C2 110(100) . . . 2_655 ? N4 Ru1 C1 C2 -93.5(3) . . . 2_655 ? N4 Ru1 C1 C2 86.5(3) 2_655 . . 2_655 ? C5 Ru1 C1 C2 -2.8(4) 2_655 . . 2_655 ? C5 Ru1 C1 C2 177.2(4) . . . 2_655 ? N3 Ru1 C1 C2 -70(100) . . . . ? N4 Ru1 C1 C2 86.5(3) . . . . ? N4 Ru1 C1 C2 -93.5(3) 2_655 . . . ? C5 Ru1 C1 C2 177.2(4) 2_655 . . . ? C5 Ru1 C1 C2 -2.8(4) . . . . ? C2 C1 C2 C3 0.7(5) 2_655 . . . ? Ru1 C1 C2 C3 -179.3(5) . . . . ? C2 C1 C2 N1 -179.0(6) 2_655 . . . ? Ru1 C1 C2 N1 1.0(6) . . . . ? C6 N1 C2 C1 -179.2(6) . . . . ? C5 N1 C2 C1 2.7(7) . . . . ? C6 N1 C2 C3 1.0(11) . . . . ? C5 N1 C2 C3 -177.0(7) . . . . ? C1 C2 C3 C4 -1.4(10) . . . . ? N1 C2 C3 C4 178.3(5) . . . . ? C2 C3 C4 C3 0.7(5) . . . 2_655 ? C7 N2 C5 N1 0.1(7) . . . . ? C8 N2 C5 N1 -176.8(6) . . . . ? C7 N2 C5 Ru1 -175.2(6) . . . . ? C8 N2 C5 Ru1 7.9(11) . . . . ? C6 N1 C5 N2 -0.2(7) . . . . ? C2 N1 C5 N2 178.2(5) . . . . ? C6 N1 C5 Ru1 176.5(4) . . . . ? C2 N1 C5 Ru1 -5.0(7) . . . . ? N3 Ru1 C5 N2 -0.9(8) . . . . ? C1 Ru1 C5 N2 179.1(8) . . . . ? N4 Ru1 C5 N2 77.0(8) . . . . ? N4 Ru1 C5 N2 -79.2(8) 2_655 . . . ? C5 Ru1 C5 N2 179.1(8) 2_655 . . . ? N3 Ru1 C5 N1 -175.9(4) . . . . ? C1 Ru1 C5 N1 4.1(4) . . . . ? N4 Ru1 C5 N1 -98.0(5) . . . . ? N4 Ru1 C5 N1 105.8(5) 2_655 . . . ? C5 Ru1 C5 N1 4.1(4) 2_655 . . . ? C5 N1 C6 C7 0.3(8) . . . . ? C2 N1 C6 C7 -177.9(6) . . . . ? N1 C6 C7 N2 -0.2(8) . . . . ? C5 N2 C7 C6 0.0(8) . . . . ? C8 N2 C7 C6 176.9(6) . . . . ? C5 N2 C8 C9 93.2(8) . . . . ? C7 N2 C8 C9 -83.3(8) . . . . ? N2 C8 C9 C10 -175.0(6) . . . . ? C8 C9 C10 C11 -177.8(7) . . . . ? C16 N4 C12 C13 -1.1(9) . . . . ? Ru1 N4 C12 C13 178.3(5) . . . . ? N4 C12 C13 C14 1.6(10) . . . . ? C12 C13 C14 C15 0.1(11) . . . . ? C13 C14 C15 C16 -2.2(11) . . . . ? C12 N4 C16 C15 -1.1(9) . . . . ? Ru1 N4 C16 C15 179.5(5) . . . . ? C12 N4 C16 C17 176.6(5) . . . . ? Ru1 N4 C16 C17 -2.8(7) . . . . ? C14 C15 C16 N4 2.8(10) . . . . ? C14 C15 C16 C17 -174.7(7) . . . . ? C17 N3 C17 C18 3.1(5) 2_655 . . . ? Ru1 N3 C17 C18 -176.9(5) . . . . ? C17 N3 C17 C16 -175.1(6) 2_655 . . . ? Ru1 N3 C17 C16 4.9(6) . . . . ? N4 C16 C17 N3 -1.2(8) . . . . ? C15 C16 C17 N3 176.4(6) . . . . ? N4 C16 C17 C18 -179.3(6) . . . . ? C15 C16 C17 C18 -1.7(11) . . . . ? N3 C17 C18 C19 -6.1(9) . . . . ? C16 C17 C18 C19 171.8(6) . . . . ? C17 C18 C19 N5 -177.0(5) . . . . ? C17 C18 C19 C18 3.0(5) . . . 2_655 ? C18 C19 N5 C20 147.6(5) 2_655 . . . ? C18 C19 N5 C20 -32.4(5) . . . . ? C18 C19 N5 C20 -32.4(5) 2_655 . . 2_655 ? C18 C19 N5 C20 147.6(5) . . . 2_655 ? C19 N5 C20 C21 -46.9(8) . . . . ? C20 N5 C20 C21 133.1(8) 2_655 . . . ? C19 N5 C20 C25 133.1(6) . . . . ? C20 N5 C20 C25 -46.9(6) 2_655 . . . ? C25 C20 C21 C22 -2.2(12) . . . . ? N5 C20 C21 C22 177.8(7) . . . . ? C20 C21 C22 C23 1.7(12) . . . . ? C26 O1 C23 C24 -177.9(8) . . . . ? C26 O1 C23 C22 1.2(11) . . . . ? C21 C22 C23 C24 -0.1(12) . . . . ? C21 C22 C23 O1 -179.1(7) . . . . ? O1 C23 C24 C25 178.3(7) . . . . ? C22 C23 C24 C25 -0.8(12) . . . . ? C21 C20 C25 C24 1.2(11) . . . . ? N5 C20 C25 C24 -178.8(7) . . . . ? C23 C24 C25 C20 0.2(12) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.45 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 3.504 _refine_diff_density_min -1.267 _refine_diff_density_rms 0.157