# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # 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_13018 _database_code_depnum_ccdc_archive 'CCDC 916867' #TrackingRef '13018.cif' _vrf_PLAT230_Alert_2_B ; Problem: Hirshfeld Test Diff for C11 -- C12 .. 7.5 su Response: There are no problems with the model related to atom type or disorder in this area--thus the likely problem is with the data. Data were collected with an average redundancy of about 3.8. ; _audit_creation_method SHELXL-2012 _chemical_name_systematic ; ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C50 H36 F3 N5 O7 Ru' _chemical_formula_sum 'C50 H36 F3 N5 O7 Ru' _chemical_formula_weight 976.91 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' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.5563(4) _cell_length_b 9.6307(4) _cell_length_c 12.6223(5) _cell_angle_alpha 83.241(2) _cell_angle_beta 74.191(2) _cell_angle_gamma 76.385(3) _cell_volume 1084.55(8) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 7226 _cell_measurement_theta_min 2.18 _cell_measurement_theta_max 28.30 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.496 _exptl_crystal_F_000 498 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.500 _exptl_crystal_size_mid 0.440 _exptl_crystal_size_min 0.150 _exptl_absorpt_coefficient_mu 0.435 _shelx_estimated_absorpt_T_min 0.812 _shelx_estimated_absorpt_T_max 0.938 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.812 _exptl_absorpt_correction_T_max 0.938 _exptl_absorpt_process_details 'SADABS (Bruker, 2002)' _exptl_special_details ; ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source ? _diffrn_measurement_device_type 'CCD Bruker APEX' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 20468 _diffrn_reflns_av_unetI/netI 0.0144 _diffrn_reflns_av_R_equivalents 0.0176 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.680 _diffrn_reflns_theta_max 28.295 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measured_fraction_theta_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.997 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.997 _diffrn_reflns_point_group_measured_fraction_full 1.000 _reflns_number_total 5377 _reflns_number_gt 5330 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection 'SMART (Bruker, 2007)' _computing_cell_refinement 'SAINT (Bruker, 2007)' _computing_data_reduction 'SAINT (Bruker, 2007)' _computing_structure_solution 'SHELXTL (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-2012 (Sheldrick, 2012)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'SHELXL-2012 (Sheldrick, 2012)' _refine_special_details ; ? ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; w=1/[\s^2^(Fo^2^)+(0.0800P)^2^+4.6000P] where P=(Fo^2^+2Fc^2^)/3 ; _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 5377 _refine_ls_number_parameters 350 _refine_ls_number_restraints 22 _refine_ls_R_factor_all 0.0694 _refine_ls_R_factor_gt 0.0691 _refine_ls_wR_factor_ref 0.1928 _refine_ls_wR_factor_gt 0.1927 _refine_ls_goodness_of_fit_ref 1.084 _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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.5000 0.5000 0.5000 0.0470(2) Uani 1 2 d S . P . . F1 F 0.0230(8) 0.4721(9) 0.5955(6) 0.069(2) Uani 0.5 1 d . . P A -1 F2 F 0.0827(10) 0.4604(10) 0.4186(6) 0.083(3) Uani 0.5 1 d . . P A -1 F3 F 0.0658(13) 0.2749(8) 0.5262(10) 0.105(3) Uani 0.5 1 d . . P A -1 O1 O -0.0175(4) 0.8591(3) 1.1663(3) 0.0415(8) Uani 1 1 d D U . . . O2 O 0.7736(3) -0.3665(3) 0.8478(2) 0.0333(6) Uani 1 1 d . . . . . O3 O 0.7805(12) 0.6180(14) 0.5027(9) 0.055(3) Uani 0.5 1 d . . P B -1 O4 O 0.3364(12) 0.4619(9) 0.4805(7) 0.031(2) Uani 0.5 1 d . U P A -1 O5 O 0.3311(9) 0.2417(8) 0.5493(6) 0.0528(18) Uani 0.5 1 d . . P A -1 N1 N 0.3698(4) 0.6940(3) 0.5514(3) 0.0281(7) Uani 1 1 d . . . . . N2 N 0.4650(4) 0.4198(3) 0.6611(3) 0.0278(7) Uani 1 1 d . . . . . N3 N 0.6771(11) 0.5742(11) 0.4999(8) 0.0176(18) Uani 0.5 1 d . U P B -1 C1 C 0.3340(5) 0.8130(4) 0.4844(3) 0.0289(8) Uani 1 1 d . . . . . C2 C 0.2297(5) 0.9228(4) 0.5516(3) 0.0298(8) Uani 1 1 d . . . . . H2 H 0.1869 1.0157 0.5261 0.036 Uiso 1 1 calc R U . . . C3 C 0.2039(5) 0.8689(4) 0.6578(3) 0.0298(8) Uani 1 1 d . . . . . H3 H 0.1392 0.9166 0.7203 0.036 Uiso 1 1 calc R U . . . C4 C 0.2932(4) 0.7253(4) 0.6579(3) 0.0271(8) Uani 1 1 d . . . . . C5 C 0.2983(4) 0.6341(4) 0.7525(3) 0.0258(7) Uani 1 1 d . . . . . C6 C 0.3790(5) 0.4922(4) 0.7525(3) 0.0276(8) Uani 1 1 d . . . . . C7 C 0.3841(4) 0.3975(4) 0.8494(3) 0.0268(7) Uani 1 1 d . . . . . H7 H 0.3352 0.4203 0.9235 0.032 Uiso 1 1 calc R U . . . C8 C 0.4716(5) 0.2698(4) 0.8153(3) 0.0288(8) Uani 1 1 d . . . . . H8 H 0.4950 0.1867 0.8611 0.035 Uiso 1 1 calc R U . . . C9 C 0.5225(5) 0.2831(4) 0.6970(3) 0.0297(8) Uani 1 1 d . . . . . C10 C 0.6141(5) 0.1732(4) 0.6304(3) 0.0293(8) Uani 1 1 d . . . . . C11 C 0.2117(4) 0.6939(4) 0.8615(3) 0.0264(7) Uani 1 1 d . . . . . C12 C 0.0821(4) 0.6508(4) 0.9197(3) 0.0255(7) Uani 1 1 d . . . . . H12 H 0.0479 0.5827 0.8900 0.031 Uiso 1 1 calc R U . . . C13 C 0.0012(5) 0.7056(4) 1.0211(3) 0.0297(8) Uani 1 1 d . . . . . H13 H -0.0879 0.6757 1.0598 0.036 Uiso 1 1 calc R U . . . C14 C 0.0512(5) 0.8039(4) 1.0651(3) 0.0280(8) Uani 1 1 d D . . . . C15 C 0.1790(5) 0.8514(4) 1.0065(3) 0.0283(8) Uani 1 1 d . . . . . H15 H 0.2120 0.9207 1.0357 0.034 Uiso 1 1 calc R U . . . C16 C 0.2577(4) 0.7969(4) 0.9054(3) 0.0278(7) Uani 1 1 d . . . . . H16 H 0.3443 0.8301 0.8652 0.033 Uiso 1 1 calc R U . . . C17 C -0.1624(12) 0.8226(15) 1.2180(10) 0.055(4) Uani 0.56(2) 1 d D U P C 1 H17A H -0.2309 0.8621 1.1713 0.082 Uiso 0.56(2) 1 d R U P C 1 H17B H -0.2029 0.8631 1.2905 0.082 Uiso 0.56(2) 1 d R U P C 1 H17C H -0.1503 0.7184 1.2266 0.082 Uiso 0.56(2) 1 d R U P C 1 C17' C -0.102(2) 0.7697(13) 1.2484(8) 0.043(4) Uani 0.44(2) 1 d D U P C 2 H17D H -0.1984 0.7752 1.2323 0.065 Uiso 0.44(2) 1 d R U P C 2 H17E H -0.1195 0.8037 1.3219 0.065 Uiso 0.44(2) 1 d R U P C 2 H17F H -0.0466 0.6703 1.2459 0.065 Uiso 0.44(2) 1 d R U P C 2 C18 C 0.6560(4) 0.0285(4) 0.6855(3) 0.0265(7) Uani 1 1 d . . . . . C19 C 0.5937(4) -0.0813(4) 0.6753(3) 0.0294(8) Uani 1 1 d . . . . . H19 H 0.5242 -0.0657 0.6315 0.035 Uiso 1 1 calc R U . . . C20 C 0.6296(4) -0.2167(4) 0.7277(3) 0.0273(7) Uani 1 1 d . . . . . H20 H 0.5849 -0.2918 0.7199 0.033 Uiso 1 1 calc R U . . . C21 C 0.7322(4) -0.2391(4) 0.7915(3) 0.0260(7) Uani 1 1 d . . . . . C22 C 0.7986(5) -0.1299(4) 0.8008(3) 0.0307(8) Uani 1 1 d . . . . . H22 H 0.8696 -0.1462 0.8433 0.037 Uiso 1 1 calc R U . . . C23 C 0.7623(5) 0.0039(4) 0.7481(3) 0.0301(8) Uani 1 1 d . . . . . H23 H 0.8088 0.0785 0.7543 0.036 Uiso 1 1 calc R U . . . C24 C 0.6990(6) -0.4776(5) 0.8454(4) 0.0399(10) Uani 1 1 d . . . . . H24A H 0.5913 -0.4428 0.8724 0.060 Uiso 1 1 d R U . . . H24B H 0.7324 -0.5600 0.8926 0.060 Uiso 1 1 d R U . . . H24C H 0.7219 -0.5063 0.7696 0.060 Uiso 1 1 d R U . . . C25 C 0.2719(13) 0.3628(13) 0.5113(9) 0.027(2) Uani 0.5 1 d . . P A -1 C26 C 0.1051(13) 0.3955(10) 0.5109(8) 0.043(2) Uani 0.5 1 d . . P 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 Ru1 0.0781(4) 0.0300(3) 0.0163(2) -0.00573(16) -0.0178(2) 0.0296(2) F1 0.062(4) 0.075(5) 0.046(4) -0.011(3) -0.005(3) 0.024(4) F2 0.093(6) 0.088(6) 0.048(4) -0.009(4) -0.029(4) 0.035(5) F3 0.139(9) 0.037(4) 0.133(9) 0.009(5) -0.022(7) -0.031(5) O1 0.0525(19) 0.0325(15) 0.0334(16) -0.0147(12) 0.0106(14) -0.0160(14) O2 0.0436(16) 0.0218(13) 0.0353(15) 0.0063(11) -0.0182(13) -0.0030(11) O3 0.038(6) 0.084(7) 0.046(5) -0.018(4) -0.016(4) -0.008(5) O4 0.037(3) 0.028(3) 0.025(3) -0.004(3) -0.008(2) -0.002(3) O5 0.070(5) 0.039(4) 0.043(4) 0.002(3) -0.016(3) 0.001(3) N1 0.0400(18) 0.0214(14) 0.0192(14) -0.0041(11) -0.0132(13) 0.0085(13) N2 0.0397(18) 0.0210(14) 0.0200(14) -0.0038(11) -0.0137(13) 0.0071(12) N3 0.018(3) 0.019(3) 0.016(3) 0.001(2) 0.001(2) -0.011(3) C1 0.040(2) 0.0212(16) 0.0226(17) -0.0040(13) -0.0142(15) 0.0070(15) C2 0.039(2) 0.0225(17) 0.0233(17) -0.0029(13) -0.0107(15) 0.0066(15) C3 0.042(2) 0.0204(16) 0.0232(17) -0.0045(13) -0.0106(15) 0.0055(15) C4 0.0357(19) 0.0221(16) 0.0206(16) -0.0041(13) -0.0102(14) 0.0042(14) C5 0.0351(19) 0.0201(16) 0.0211(16) -0.0048(12) -0.0118(14) 0.0031(14) C6 0.039(2) 0.0230(17) 0.0184(15) -0.0033(13) -0.0118(14) 0.0045(15) C7 0.0350(19) 0.0248(17) 0.0204(16) -0.0029(13) -0.0116(14) 0.0005(14) C8 0.039(2) 0.0239(17) 0.0211(16) -0.0021(13) -0.0127(15) 0.0043(15) C9 0.041(2) 0.0237(17) 0.0208(16) -0.0023(13) -0.0148(15) 0.0074(15) C10 0.042(2) 0.0208(16) 0.0219(16) -0.0024(13) -0.0145(15) 0.0074(15) C11 0.038(2) 0.0186(15) 0.0196(15) -0.0024(12) -0.0127(14) 0.0063(14) C12 0.0281(17) 0.0194(15) 0.0309(18) -0.0019(13) -0.0122(14) -0.0031(13) C13 0.0305(19) 0.0226(17) 0.0327(19) -0.0019(14) -0.0046(15) -0.0036(14) C14 0.037(2) 0.0184(15) 0.0256(17) -0.0055(13) -0.0061(15) -0.0002(14) C15 0.037(2) 0.0230(17) 0.0257(17) -0.0054(13) -0.0068(15) -0.0083(15) C16 0.0322(19) 0.0264(17) 0.0246(17) -0.0034(14) -0.0039(14) -0.0089(14) C17 0.066(6) 0.034(6) 0.048(6) -0.015(4) 0.024(5) -0.016(5) C17' 0.053(8) 0.034(6) 0.033(5) -0.010(4) 0.013(5) -0.012(5) C18 0.0361(19) 0.0213(16) 0.0184(15) -0.0018(12) -0.0103(14) 0.0057(14) C19 0.0334(19) 0.0307(19) 0.0229(16) -0.0032(14) -0.0123(14) 0.0026(15) C20 0.0316(19) 0.0266(17) 0.0251(17) -0.0043(14) -0.0110(14) -0.0030(14) C21 0.0319(18) 0.0207(16) 0.0223(16) 0.0006(13) -0.0087(14) 0.0018(13) C22 0.038(2) 0.0253(18) 0.0305(18) 0.0010(14) -0.0197(16) 0.0017(15) C23 0.042(2) 0.0217(17) 0.0289(18) -0.0007(14) -0.0179(16) 0.0002(15) C24 0.059(3) 0.0264(19) 0.037(2) 0.0050(16) -0.019(2) -0.0086(19) C25 0.020(5) 0.036(5) 0.027(4) -0.005(3) 0.001(4) -0.016(5) C26 0.048(6) 0.036(5) 0.038(5) -0.003(4) -0.009(4) 0.000(4) _geom_special_details ; ; 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 O4 1.773(11) . ? Ru1 N3 1.986(11) . ? Ru1 N1 2.052(3) . ? Ru1 N2 2.056(3) . ? F1 C26 1.325(11) . ? F2 C26 1.302(12) . ? F3 C26 1.280(13) . ? O1 C14 1.373(4) . ? O1 C17' 1.461(7) . ? O1 C17 1.466(7) . ? O2 C21 1.374(4) . ? O2 C24 1.426(5) . ? O3 N3 1.172(14) . ? O4 C25 1.225(13) . ? O5 C25 1.272(13) . ? N1 C1 1.375(5) . ? N1 C4 1.375(5) . ? N2 C9 1.376(5) . ? N2 C6 1.377(5) . ? C1 C10 1.399(5) 2_666 ? C1 C2 1.444(5) . ? C2 C3 1.358(5) . ? C2 H2 0.9500 . ? C3 C4 1.444(5) . ? C3 H3 0.9500 . ? C4 C5 1.401(5) . ? C5 C6 1.402(5) . ? C5 C11 1.501(5) . ? C6 C7 1.443(5) . ? C7 C8 1.357(5) . ? C7 H7 0.9500 . ? C8 C9 1.439(5) . ? C8 H8 0.9500 . ? C9 C10 1.402(5) . ? C10 C18 1.499(5) . ? C11 C12 1.385(6) . ? C11 C16 1.396(5) . ? C12 C13 1.393(5) . ? C12 H12 0.9500 . ? C13 C14 1.383(6) . ? C13 H13 0.9500 . ? C14 C15 1.393(6) . ? C15 C16 1.385(5) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C17' H17D 0.9800 . ? C17' H17E 0.9800 . ? C17' H17F 0.9800 . ? C18 C19 1.364(6) . ? C18 C23 1.411(5) . ? C19 C20 1.402(5) . ? C19 H19 0.9500 . ? C20 C21 1.395(5) . ? C20 H20 0.9500 . ? C21 C22 1.381(6) . ? C22 C23 1.391(5) . ? C22 H22 0.9500 . ? C23 H23 0.9500 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C26 1.551(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 O4 Ru1 N3 168.7(4) . . ? O4 Ru1 N1 86.1(3) . . ? N3 Ru1 N1 88.4(3) . . ? O4 Ru1 N1 93.8(3) . 2_666 ? N3 Ru1 N1 91.6(3) . 2_666 ? N1 Ru1 N1 180.0 . 2_666 ? O4 Ru1 N2 94.6(3) . . ? N3 Ru1 N2 95.3(3) . . ? N1 Ru1 N2 89.87(12) . . ? N1 Ru1 N2 90.13(12) 2_666 . ? O4 Ru1 N2 85.4(3) . 2_666 ? N3 Ru1 N2 84.7(3) . 2_666 ? N1 Ru1 N2 90.13(12) . 2_666 ? N1 Ru1 N2 89.87(12) 2_666 2_666 ? N2 Ru1 N2 180.0 . 2_666 ? C14 O1 C17' 116.6(5) . . ? C14 O1 C17 114.2(4) . . ? C21 O2 C24 117.0(3) . . ? C25 O4 Ru1 134.0(9) . . ? C1 N1 C4 107.5(3) . . ? C1 N1 Ru1 126.1(2) . . ? C4 N1 Ru1 126.3(2) . . ? C9 N2 C6 107.6(3) . . ? C9 N2 Ru1 126.1(2) . . ? C6 N2 Ru1 126.3(2) . . ? O3 N3 Ru1 178.3(9) . . ? N1 C1 C10 126.4(3) . 2_666 ? N1 C1 C2 108.9(3) . . ? C10 C1 C2 124.7(3) 2_666 . ? C3 C2 C1 107.4(3) . . ? C3 C2 H2 126.3 . . ? C1 C2 H2 126.3 . . ? C2 C3 C4 107.2(3) . . ? C2 C3 H3 126.4 . . ? C4 C3 H3 126.4 . . ? N1 C4 C5 126.4(3) . . ? N1 C4 C3 109.0(3) . . ? C5 C4 C3 124.6(3) . . ? C4 C5 C6 124.8(3) . . ? C4 C5 C11 117.3(3) . . ? C6 C5 C11 117.9(3) . . ? N2 C6 C5 126.2(3) . . ? N2 C6 C7 108.7(3) . . ? C5 C6 C7 125.1(3) . . ? C8 C7 C6 107.4(3) . . ? C8 C7 H7 126.3 . . ? C6 C7 H7 126.3 . . ? C7 C8 C9 107.5(3) . . ? C7 C8 H8 126.2 . . ? C9 C8 H8 126.2 . . ? N2 C9 C10 126.2(3) . . ? N2 C9 C8 108.8(3) . . ? C10 C9 C8 125.0(3) . . ? C1 C10 C9 125.0(3) 2_666 . ? C1 C10 C18 117.3(3) 2_666 . ? C9 C10 C18 117.7(3) . . ? C12 C11 C16 118.5(3) . . ? C12 C11 C5 120.7(3) . . ? C16 C11 C5 120.8(4) . . ? C11 C12 C13 121.0(3) . . ? C11 C12 H12 119.5 . . ? C13 C12 H12 119.5 . . ? C14 C13 C12 119.7(4) . . ? C14 C13 H13 120.1 . . ? C12 C13 H13 120.1 . . ? O1 C14 C13 123.8(4) . . ? O1 C14 C15 116.1(3) . . ? C13 C14 C15 120.1(3) . . ? C16 C15 C14 119.6(3) . . ? C16 C15 H15 120.2 . . ? C14 C15 H15 120.2 . . ? C15 C16 C11 121.1(4) . . ? C15 C16 H16 119.5 . . ? C11 C16 H16 119.5 . . ? O1 C17 H17A 109.5 . . ? O1 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? O1 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? O1 C17' H17D 109.5 . . ? O1 C17' H17E 109.5 . . ? H17D C17' H17E 109.5 . . ? O1 C17' H17F 109.5 . . ? H17D C17' H17F 109.5 . . ? H17E C17' H17F 109.5 . . ? C19 C18 C23 119.0(3) . . ? C19 C18 C10 120.8(3) . . ? C23 C18 C10 120.1(4) . . ? C18 C19 C20 121.7(3) . . ? C18 C19 H19 119.2 . . ? C20 C19 H19 119.2 . . ? C21 C20 C19 118.9(4) . . ? C21 C20 H20 120.6 . . ? C19 C20 H20 120.6 . . ? O2 C21 C22 116.1(3) . . ? O2 C21 C20 123.8(4) . . ? C22 C21 C20 120.1(3) . . ? C21 C22 C23 120.4(4) . . ? C21 C22 H22 119.8 . . ? C23 C22 H22 119.8 . . ? C22 C23 C18 119.8(4) . . ? C22 C23 H23 120.1 . . ? C18 C23 H23 120.1 . . ? O2 C24 H24A 109.5 . . ? O2 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? O2 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? O4 C25 O5 123.7(11) . . ? O4 C25 C26 116.2(10) . . ? O5 C25 C26 119.9(10) . . ? F3 C26 F2 110.5(11) . . ? F3 C26 F1 106.7(10) . . ? F2 C26 F1 110.4(8) . . ? F3 C26 C25 106.5(10) . . ? F2 C26 C25 112.0(9) . . ? F1 C26 C25 110.5(9) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N3 Ru1 O4 C25 171.3(19) . . . . ? N1 Ru1 O4 C25 -127.6(11) . . . . ? N1 Ru1 O4 C25 52.4(11) 2_666 . . . ? N2 Ru1 O4 C25 -38.0(11) . . . . ? N2 Ru1 O4 C25 142.0(11) 2_666 . . . ? C4 N1 C1 C10 -179.1(4) . . . 2_666 ? Ru1 N1 C1 C10 -3.8(6) . . . 2_666 ? C4 N1 C1 C2 -0.6(5) . . . . ? Ru1 N1 C1 C2 174.8(3) . . . . ? N1 C1 C2 C3 0.0(5) . . . . ? C10 C1 C2 C3 178.6(4) 2_666 . . . ? C1 C2 C3 C4 0.6(5) . . . . ? C1 N1 C4 C5 -179.5(4) . . . . ? Ru1 N1 C4 C5 5.2(6) . . . . ? C1 N1 C4 C3 0.9(5) . . . . ? Ru1 N1 C4 C3 -174.4(3) . . . . ? C2 C3 C4 N1 -0.9(5) . . . . ? C2 C3 C4 C5 179.5(4) . . . . ? N1 C4 C5 C6 -2.9(7) . . . . ? C3 C4 C5 C6 176.7(4) . . . . ? N1 C4 C5 C11 176.6(4) . . . . ? C3 C4 C5 C11 -3.9(6) . . . . ? C9 N2 C6 C5 -178.9(4) . . . . ? Ru1 N2 C6 C5 0.5(6) . . . . ? C9 N2 C6 C7 0.5(5) . . . . ? Ru1 N2 C6 C7 180.0(3) . . . . ? C4 C5 C6 N2 -0.2(7) . . . . ? C11 C5 C6 N2 -179.6(4) . . . . ? C4 C5 C6 C7 -179.6(4) . . . . ? C11 C5 C6 C7 0.9(6) . . . . ? N2 C6 C7 C8 -0.4(5) . . . . ? C5 C6 C7 C8 179.1(4) . . . . ? C6 C7 C8 C9 0.1(5) . . . . ? C6 N2 C9 C10 178.7(4) . . . . ? Ru1 N2 C9 C10 -0.7(6) . . . . ? C6 N2 C9 C8 -0.5(5) . . . . ? Ru1 N2 C9 C8 -179.9(3) . . . . ? C7 C8 C9 N2 0.2(5) . . . . ? C7 C8 C9 C10 -179.0(4) . . . . ? N2 C9 C10 C1 2.3(7) . . . 2_666 ? C8 C9 C10 C1 -178.6(4) . . . 2_666 ? N2 C9 C10 C18 -175.8(4) . . . . ? C8 C9 C10 C18 3.3(7) . . . . ? C4 C5 C11 C12 107.7(4) . . . . ? C6 C5 C11 C12 -72.8(5) . . . . ? C4 C5 C11 C16 -70.6(5) . . . . ? C6 C5 C11 C16 108.9(4) . . . . ? C16 C11 C12 C13 -1.7(5) . . . . ? C5 C11 C12 C13 179.9(3) . . . . ? C11 C12 C13 C14 -0.5(6) . . . . ? C17' O1 C14 C13 27.0(11) . . . . ? C17 O1 C14 C13 -9.0(9) . . . . ? C17' O1 C14 C15 -152.4(10) . . . . ? C17 O1 C14 C15 171.6(8) . . . . ? C12 C13 C14 O1 -177.1(4) . . . . ? C12 C13 C14 C15 2.2(6) . . . . ? O1 C14 C15 C16 177.7(4) . . . . ? C13 C14 C15 C16 -1.7(6) . . . . ? C14 C15 C16 C11 -0.6(6) . . . . ? C12 C11 C16 C15 2.3(6) . . . . ? C5 C11 C16 C15 -179.4(3) . . . . ? C1 C10 C18 C19 -71.9(5) 2_666 . . . ? C9 C10 C18 C19 106.3(5) . . . . ? C1 C10 C18 C23 107.5(4) 2_666 . . . ? C9 C10 C18 C23 -74.3(5) . . . . ? C23 C18 C19 C20 1.7(6) . . . . ? C10 C18 C19 C20 -178.9(4) . . . . ? C18 C19 C20 C21 -0.2(6) . . . . ? C24 O2 C21 C22 175.9(4) . . . . ? C24 O2 C21 C20 -4.1(6) . . . . ? C19 C20 C21 O2 178.9(4) . . . . ? C19 C20 C21 C22 -1.1(6) . . . . ? O2 C21 C22 C23 -179.0(4) . . . . ? C20 C21 C22 C23 1.0(6) . . . . ? C21 C22 C23 C18 0.5(6) . . . . ? C19 C18 C23 C22 -1.8(6) . . . . ? C10 C18 C23 C22 178.8(4) . . . . ? Ru1 O4 C25 O5 -16.2(19) . . . . ? Ru1 O4 C25 C26 158.9(8) . . . . ? O4 C25 C26 F3 168.7(11) . . . . ? O5 C25 C26 F3 -15.9(14) . . . . ? O4 C25 C26 F2 47.8(14) . . . . ? O5 C25 C26 F2 -136.9(10) . . . . ? O4 C25 C26 F1 -75.8(12) . . . . ? O5 C25 C26 F1 99.6(12) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C2 H2 F3 0.95 2.49 3.402(10) 160.3 1_565 C3 H3 O1 0.95 2.59 3.462(5) 152.9 2_577 C17 H17B O5 0.98 2.31 3.012(13) 127.4 2_567 _refine_diff_density_max 1.476 _refine_diff_density_min -2.081 _refine_diff_density_rms 0.094 data_13017 _database_code_depnum_ccdc_archive 'CCDC 916868' #TrackingRef '13017.cif' _vrf_PLAT413_Alert_2_A ; Problem: Short Inter XH3 .. XHn H23 .. H6S6 .. 1.71 Ang. Short Inter XH3 .. XHn H52 .. H6S4 .. 1.71 Ang. Response: The H6S hydrogens are on the lower occupied part of the disordered solvent. ; _vrf_PLAT973_Alert_2_A ; Problem: Large Calcd. Positive Residual Density on Ru1 2.21 eA-3 Response: This large peak is believed due to the use of spherical scattering factors. This peak is > 0.8 \%A from the metal. ; _vrf_PLAT934_Alert_3_B ; Problem: Number of (Iobs-Icalc)/SigmaW .gt. 10 Outliers . 1 Response: There was a small amount of twinning in the selected crystal. This intensity is believed to be an artifact of this twinning. ; _audit_creation_method SHELXL-2012 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C54 H37 F4 N5 O6 Ru, C6 H14' _chemical_formula_sum 'C60 H51 F4 N5 O6 Ru' _chemical_formula_weight 1115.12 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' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.4322(6) _cell_length_b 16.2330(11) _cell_length_c 18.0081(12) _cell_angle_alpha 72.590(2) _cell_angle_beta 78.034(2) _cell_angle_gamma 74.000(3) _cell_volume 2505.5(3) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 6753 _cell_measurement_theta_min 2.27 _cell_measurement_theta_max 28.31 _exptl_crystal_description block _exptl_crystal_colour purple _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.478 _exptl_crystal_F_000 1148 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.380 _exptl_crystal_size_mid 0.260 _exptl_crystal_size_min 0.080 _exptl_absorpt_coefficient_mu 0.388 _shelx_estimated_absorpt_T_min 0.867 _shelx_estimated_absorpt_T_max 0.970 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.867 _exptl_absorpt_correction_T_max 0.970 _exptl_absorpt_process_details 'SADABS (Bruker, 2002)' _exptl_special_details ; ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source ? _diffrn_measurement_device_type CCD _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 41662 _diffrn_reflns_av_unetI/netI 0.0493 _diffrn_reflns_av_R_equivalents 0.0439 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.196 _diffrn_reflns_theta_max 28.334 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.994 _diffrn_measured_fraction_theta_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.994 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.994 _diffrn_reflns_point_group_measured_fraction_full 1.000 _reflns_number_total 12434 _reflns_number_gt 9328 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection 'SMART (Bruker, 2007)' _computing_cell_refinement 'SAINT (Bruker, 2007)' _computing_data_reduction 'SAINT (Bruker, 2007)' _computing_structure_solution 'SHELXTL (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-2012 (Sheldrick, 2012)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'SHELXL-2012 (Sheldrick, 2012)' _refine_special_details ; Restraints on disordered methoxyphenyl group sadi 0.006 c15 c35 c15 c35' c15 c35" sadi 0.006 c35 c36 c35 c40 c35' c36' c35' c40' c35" c36" c35" c40" sadi 0.006 c36 c37 c40 c39 c36' c37' c40' c39' c36" c37" c40" c39" sadi 0.006 c37 c38 c39 c38 c37' c38' c39' c38' c37" c38" c39" c38" sadi 0.006 c38 o3 c38' o3' c38" o3" sadi 0.006 o3 c41 o3' c41' o3" c41" sadi 0.010 c35 c37 c35 c39 c37 c39 c35' c37' c37' c39' c39' c35' sadi 0.010 c35" c37" c37" c39" c39" c35" c35 c37 sadi 0.010 c38 c41 c38' c41' c38" c41" delu 0.010 o3 c15 c35 c36 c37 c38 c39 c40 c41 delu 0.010 o3' c15 c35' c36' c37' c38' c39' c40' c41' delu 0.010 o3" c15 c35" c36" c37" c38" c39' c40" c41" simu 0.010 o3 o3' o3" c15 > c41" isor 0.010 c41 c35' c40' c41' sump 1 0.0004 1 2 1 3 1 4 Restraints on disordered n-hexane: dfix 1.52 0.006 c1s c2s c2s c3s c3s c4s c4s c5s c5s c6s c6s' c5s sadi 0.010 c1s c3s c3s c5s c2s c4s c4s c6s c6s' c4s delu 0.008 c5s c6s c6s' simu 0.008 c6s c6s' isor 0.008 c6s c6s' ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; w=1/[\s^2^(Fo^2^)+(0.1260P)^2^+3.2000P] where P=(Fo^2^+2Fc^2^)/3 ; _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 12434 _refine_ls_number_parameters 842 _refine_ls_number_restraints 910 _refine_ls_R_factor_all 0.0893 _refine_ls_R_factor_gt 0.0617 _refine_ls_wR_factor_ref 0.1954 _refine_ls_wR_factor_gt 0.1683 _refine_ls_goodness_of_fit_ref 1.005 _refine_ls_restrained_S_all 0.991 _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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.25589(3) 0.54413(2) 0.28640(2) 0.02404(11) Uani 1 1 d . . . . . F1 F -0.1114(3) 0.6777(2) 0.20251(15) 0.0477(7) Uani 1 1 d . . . . . F2 F -0.1862(3) 0.8328(2) 0.0986(2) 0.0634(9) Uani 1 1 d . . . . . F3 F 0.2957(4) 0.7810(2) -0.04567(16) 0.0621(9) Uani 1 1 d . . . . . F4 F 0.3681(3) 0.62506(19) 0.05808(14) 0.0421(6) Uani 1 1 d . . . . . O1 O 0.0879(5) -0.0070(2) 0.3654(2) 0.0588(10) Uani 1 1 d . . . . . O2 O -0.6826(3) 0.7426(2) 0.51895(18) 0.0388(7) Uani 1 1 d . . . . . O3 O 0.4001(14) 1.1073(6) 0.1339(6) 0.048(2) Uani 0.444(6) 1 d D U P A 1 O3' O 0.4192(17) 1.1009(8) 0.1165(7) 0.043(2) Uani 0.349(6) 1 d D U P A 2 O3" O 0.3379(19) 1.1166(8) 0.0525(8) 0.046(2) Uani 0.207(4) 1 d D U P A 3 O4 O 1.1927(3) 0.3846(2) 0.03670(16) 0.0338(6) Uani 1 1 d . . . . . O5 O 0.1704(3) 0.57040(18) 0.18681(15) 0.0289(5) Uani 1 1 d . . . . . O6 O 0.3983(3) 0.5113(2) 0.42320(17) 0.0397(7) Uani 1 1 d . . . . . N1 N 0.3736(3) 0.4269(2) 0.25918(17) 0.0257(6) Uani 1 1 d . . . . . N2 N 0.0790(3) 0.4865(2) 0.34024(18) 0.0254(6) Uani 1 1 d . . . . . N3 N 0.1286(3) 0.6640(2) 0.30270(18) 0.0249(6) Uani 1 1 d . . . . . N4 N 0.4233(3) 0.6048(2) 0.22133(17) 0.0231(6) Uani 1 1 d . . . . . N5 N 0.3368(3) 0.5204(2) 0.37101(17) 0.0259(6) Uani 1 1 d . . . . . C1 C 0.5182(4) 0.4105(2) 0.2228(2) 0.0268(7) Uani 1 1 d . . . . . C2 C 0.5644(4) 0.3183(3) 0.2217(2) 0.0315(8) Uani 1 1 d . . . . . H2 H 0.6597 0.2891 0.2012 0.038 Uiso 1 1 calc R U . . . C3 C 0.4455(5) 0.2811(3) 0.2558(3) 0.0351(9) Uani 1 1 d . . . . . H3 H 0.4418 0.2215 0.2621 0.042 Uiso 1 1 calc R U . . . C4 C 0.3264(4) 0.3492(3) 0.2805(2) 0.0311(8) Uani 1 1 d . . . . . C5 C 0.1867(4) 0.3359(3) 0.3206(2) 0.0320(8) Uani 1 1 d . . . . . C6 C 0.0746(4) 0.4001(3) 0.3486(2) 0.0308(8) Uani 1 1 d . . . . . C7 C -0.0666(4) 0.3853(3) 0.3922(2) 0.0352(9) Uani 1 1 d . . . . . H7 H -0.0987 0.3314 0.4067 0.042 Uiso 1 1 calc R U . . . C8 C -0.1451(4) 0.4629(3) 0.4087(2) 0.0332(8) Uani 1 1 d . . . . . H8 H -0.2426 0.4732 0.4368 0.040 Uiso 1 1 calc R U . . . C9 C -0.0539(4) 0.5271(2) 0.3758(2) 0.0257(7) Uani 1 1 d . . . . . C10 C -0.0973(4) 0.6156(2) 0.3779(2) 0.0252(7) Uani 1 1 d . . . . . C11 C -0.0116(4) 0.6785(2) 0.3442(2) 0.0247(7) Uani 1 1 d . . . . . C12 C -0.0615(4) 0.7714(3) 0.3416(2) 0.0327(8) Uani 1 1 d . . . . . H12 H -0.1547 0.7994 0.3653 0.039 Uiso 1 1 calc R U . . . C13 C 0.0487(4) 0.8115(3) 0.2993(3) 0.0364(9) Uani 1 1 d . . . . . H13 H 0.0473 0.8727 0.2883 0.044 Uiso 1 1 calc R U . . . C14 C 0.1683(4) 0.7444(3) 0.2741(2) 0.0300(8) Uani 1 1 d . . . . . C15 C 0.3014(4) 0.7595(3) 0.2261(2) 0.0310(8) Uani 1 1 d D U . . . C16 C 0.4174(4) 0.6941(2) 0.2025(2) 0.0273(7) Uani 1 1 d . U . . . C17 C 0.5533(4) 0.7100(3) 0.1528(2) 0.0303(8) Uani 1 1 d . U . . . H17 H 0.5785 0.7659 0.1306 0.036 Uiso 1 1 calc R U . . . C18 C 0.6384(4) 0.6306(2) 0.1434(2) 0.0271(7) Uani 1 1 d . U . . . H18 H 0.7343 0.6206 0.1135 0.032 Uiso 1 1 calc R U . . . C19 C 0.5565(4) 0.5641(2) 0.18704(19) 0.0226(7) Uani 1 1 d . U . . . C20 C 0.6052(4) 0.4737(2) 0.19014(19) 0.0232(7) Uani 1 1 d . U . . . C21 C 0.1594(5) 0.2446(3) 0.3346(3) 0.0367(9) Uani 1 1 d . U . . . C22 C 0.1002(7) 0.2240(3) 0.2804(3) 0.0554(12) Uani 1 1 d . U . . . H22 H 0.0748 0.2682 0.2339 0.067 Uiso 1 1 calc R U . . . C23 C 0.0773(7) 0.1398(4) 0.2929(3) 0.0601(13) Uani 1 1 d . U . . . H23 H 0.0351 0.1273 0.2551 0.072 Uiso 1 1 calc R U . . . C24 C 0.1140(6) 0.0756(3) 0.3579(3) 0.0462(11) Uani 1 1 d . U . . . C25 C 0.1690(8) 0.0937(4) 0.4133(4) 0.0689(15) Uani 1 1 d . U . . . H25 H 0.1941 0.0490 0.4596 0.083 Uiso 1 1 calc R U . . . C26 C 0.1885(7) 0.1805(4) 0.4013(4) 0.0643(15) Uani 1 1 d . U . . . H26 H 0.2231 0.1940 0.4412 0.077 Uiso 1 1 calc R U . . . C27 C 0.1458(9) -0.0779(4) 0.4257(5) 0.085(2) Uani 1 1 d . . . . . H27A H 0.2548 -0.0920 0.4149 0.127 Uiso 1 1 d R U . . . H27B H 0.1090 -0.1298 0.4286 0.127 Uiso 1 1 d R U . . . H27C H 0.1143 -0.0615 0.4757 0.127 Uiso 1 1 d R U . . . C28 C -0.2520(4) 0.6476(2) 0.4169(2) 0.0263(7) Uani 1 1 d . U . . . C29 C -0.3752(5) 0.6605(3) 0.3813(3) 0.0379(9) Uani 1 1 d . U . . . H29 H -0.3630 0.6477 0.3319 0.046 Uiso 1 1 calc R U . . . C30 C -0.5177(5) 0.6924(3) 0.4172(3) 0.0393(9) Uani 1 1 d . U . . . H30 H -0.6015 0.7014 0.3918 0.047 Uiso 1 1 calc R U . . . C31 C -0.5381(4) 0.7108(3) 0.4889(3) 0.0335(8) Uani 1 1 d . U . . . C32 C -0.4156(4) 0.6987(3) 0.5261(2) 0.0343(8) Uani 1 1 d . U . . . H32 H -0.4284 0.7114 0.5755 0.041 Uiso 1 1 calc R U . . . C33 C -0.2736(4) 0.6673(3) 0.4893(2) 0.0338(8) Uani 1 1 d . U . . . H33 H -0.1895 0.6591 0.5142 0.041 Uiso 1 1 calc R U . . . C34 C -0.7025(6) 0.7640(4) 0.5929(3) 0.0526(13) Uani 1 1 d . . . . . H34A H -0.6646 0.7106 0.6329 0.079 Uiso 1 1 d R U . . . H34B H -0.8086 0.7868 0.6087 0.079 Uiso 1 1 d R U . . . H34C H -0.6479 0.8093 0.5875 0.079 Uiso 1 1 d R U . . . C35 C 0.327(2) 0.8525(5) 0.2031(9) 0.0316(16) Uani 0.444(6) 1 d D U P A 1 C36 C 0.2489(11) 0.9168(6) 0.1476(6) 0.0381(16) Uani 0.444(6) 1 d D U P A 1 H36 H 0.1749 0.9028 0.1280 0.046 Uiso 0.444(6) 1 calc R U P A 1 C37 C 0.2748(11) 1.0017(5) 0.1192(6) 0.0423(17) Uani 0.444(6) 1 d D U P A 1 H37 H 0.2194 1.0452 0.0809 0.051 Uiso 0.444(6) 1 calc R U P A 1 C38 C 0.3838(15) 1.0215(6) 0.1482(8) 0.0395(17) Uani 0.444(6) 1 d D U P A 1 C39 C 0.4621(11) 0.9571(5) 0.2055(6) 0.0400(17) Uani 0.444(6) 1 d D U P A 1 H39 H 0.5346 0.9711 0.2264 0.048 Uiso 0.444(6) 1 calc R U P A 1 C40 C 0.4344(11) 0.8725(5) 0.2321(6) 0.0355(16) Uani 0.444(6) 1 d D U P A 1 H40 H 0.4895 0.8285 0.2703 0.043 Uiso 0.444(6) 1 calc R U P A 1 C41 C 0.343(2) 1.1718(8) 0.0683(9) 0.058(4) Uani 0.444(6) 1 d D U P A 1 H41A H 0.3683 1.1468 0.0227 0.087 Uiso 0.444(6) 1 d R U P A 1 H41B H 0.3854 1.2236 0.0567 0.087 Uiso 0.444(6) 1 d R U P A 1 H41C H 0.2340 1.1898 0.0802 0.087 Uiso 0.444(6) 1 d R U P A 1 C35' C 0.321(3) 0.8541(7) 0.2000(9) 0.0316(18) Uani 0.349(6) 1 d D U P A 2 C36' C 0.3060(17) 0.9011(7) 0.1234(7) 0.0369(18) Uani 0.349(6) 1 d D U P A 2 H36' H 0.2808 0.8741 0.0893 0.044 Uiso 0.349(6) 1 calc R U P A 2 C37' C 0.3267(17) 0.9871(7) 0.0950(6) 0.0383(18) Uani 0.349(6) 1 d D U P A 2 H37' H 0.3167 1.0189 0.0419 0.046 Uiso 0.349(6) 1 calc R U P A 2 C38' C 0.362(2) 1.0257(8) 0.1461(7) 0.0392(18) Uani 0.349(6) 1 d D U P A 2 C39' C 0.3842(17) 0.9778(6) 0.2228(6) 0.0388(18) Uani 0.349(6) 1 d D U P A 2 H39' H 0.4124 1.0036 0.2567 0.047 Uiso 0.349(6) 1 calc R U P A 2 C40' C 0.3641(17) 0.8915(7) 0.2488(6) 0.0366(17) Uani 0.349(6) 1 d D U P A 2 H40' H 0.3800 0.8579 0.3008 0.044 Uiso 0.349(6) 1 calc R U P A 2 C41' C 0.382(2) 1.1569(9) 0.0427(9) 0.048(3) Uani 0.349(6) 1 d D U P A 2 H41D H 0.4299 1.1262 0.0015 0.071 Uiso 0.349(6) 1 d R U P A 2 H41E H 0.4171 1.2114 0.0319 0.071 Uiso 0.349(6) 1 d R U P A 2 H41F H 0.2739 1.1718 0.0437 0.071 Uiso 0.349(6) 1 d R U P A 2 C35" C 0.308(3) 0.8544(6) 0.1770(7) 0.033(2) Uani 0.207(4) 1 d D U P A 3 C36" C 0.330(2) 0.8819(8) 0.0960(8) 0.038(2) Uani 0.207(4) 1 d D U P A 3 H36" H 0.3408 0.8397 0.0672 0.046 Uiso 0.207(4) 1 calc R U P A 3 C37" C 0.336(2) 0.9682(8) 0.0546(7) 0.041(2) Uani 0.207(4) 1 d D U P A 3 H37" H 0.3466 0.9845 -0.0012 0.049 Uiso 0.207(4) 1 calc R U P A 3 C38" C 0.328(3) 1.0311(8) 0.0951(8) 0.041(2) Uani 0.207(4) 1 d D U P A 3 C39" C 0.311(3) 1.0038(8) 0.1772(8) 0.040(2) Uani 0.207(4) 1 d D U P A 3 H39" H 0.3108 1.0437 0.2066 0.048 Uiso 0.207(4) 1 calc R U P A 3 C40" C 0.296(2) 0.9182(9) 0.2156(8) 0.0365(18) Uani 0.207(4) 1 d D U P A 3 H40" H 0.2757 0.9027 0.2713 0.044 Uiso 0.207(4) 1 calc R U P A 3 C41" C 0.340(5) 1.1760(12) 0.0959(14) 0.048(4) Uani 0.207(4) 1 d D U P A 3 H41G H 0.2400 1.2130 0.1044 0.072 Uiso 0.207(4) 1 d R U P A 3 H41H H 0.4089 1.2139 0.0665 0.072 Uiso 0.207(4) 1 d R U P A 3 H41I H 0.3734 1.1422 0.1467 0.072 Uiso 0.207(4) 1 d R U P A 3 C42 C 0.7620(4) 0.4440(2) 0.1534(2) 0.0229(7) Uani 1 1 d . . . . . C43 C 0.7950(4) 0.4053(2) 0.0904(2) 0.0264(7) Uani 1 1 d . . . . . H43 H 0.7172 0.3929 0.0725 0.032 Uiso 1 1 calc R U . . . C44 C 0.9399(4) 0.3848(3) 0.0536(2) 0.0269(7) Uani 1 1 d . . . . . H44 H 0.9608 0.3578 0.0112 0.032 Uiso 1 1 calc R U . . . C45 C 1.0555(4) 0.4037(3) 0.0789(2) 0.0277(7) Uani 1 1 d . . . . . C46 C 1.0247(4) 0.4416(3) 0.1414(2) 0.0315(8) Uani 1 1 d . . . . . H46 H 1.1024 0.4546 0.1590 0.038 Uiso 1 1 calc R U . . . C47 C 0.8790(4) 0.4607(3) 0.1785(2) 0.0293(8) Uani 1 1 d . . . . . H47 H 0.8588 0.4857 0.2220 0.035 Uiso 1 1 calc R U . . . C48 C 1.3116(4) 0.4060(3) 0.0598(3) 0.0419(10) Uani 1 1 d . . . . . H48A H 1.2880 0.4696 0.0560 0.063 Uiso 1 1 d R U . . . H48B H 1.4039 0.3904 0.0250 0.063 Uiso 1 1 d R U . . . H48C H 1.3243 0.3725 0.1141 0.063 Uiso 1 1 d R U . . . C49 C 0.1348(4) 0.6480(3) 0.1364(2) 0.0277(7) Uani 1 1 d . . . . . C50 C -0.0078(4) 0.7039(3) 0.1423(2) 0.0344(9) Uani 1 1 d . . . . . C51 C -0.0461(5) 0.7830(3) 0.0884(3) 0.0442(11) Uani 1 1 d . . . . . C52 C 0.0546(6) 0.8127(3) 0.0246(3) 0.0493(12) Uani 1 1 d . . . . . H52 H 0.0287 0.8684 -0.0120 0.059 Uiso 1 1 calc R U . . . C53 C 0.1939(5) 0.7576(3) 0.0168(2) 0.0416(10) Uani 1 1 d . . . . . C54 C 0.2333(4) 0.6776(3) 0.0702(2) 0.0322(8) Uani 1 1 d . . . . . C1S C 0.5565(11) -0.0660(5) 0.4261(5) 0.109(3) Uani 1 1 d D . . . . H1S1 H 0.5184 -0.0997 0.4009 0.164 Uiso 1 1 d R U . . . H1S2 H 0.4830 -0.0508 0.4700 0.164 Uiso 1 1 d R U . . . H1S3 H 0.6496 -0.1019 0.4459 0.164 Uiso 1 1 d R U . . . C2S C 0.5853(10) 0.0179(5) 0.3671(5) 0.114(3) Uani 1 1 d D . . . . H2S1 H 0.4993 0.0460 0.3375 0.136 Uiso 1 1 calc R U . . . H2S2 H 0.5933 0.0597 0.3955 0.136 Uiso 1 1 calc R U . . . C3S C 0.7234(8) 0.0024(5) 0.3105(4) 0.102(3) Uani 1 1 d D . . . . H3S1 H 0.8099 -0.0166 0.3397 0.122 Uiso 1 1 calc R U . . . H3S2 H 0.7225 -0.0474 0.2897 0.122 Uiso 1 1 calc R U . . . C4S C 0.7472(9) 0.0790(4) 0.2425(4) 0.113(3) Uani 1 1 d D . . . . H4S1 H 0.7582 0.1272 0.2624 0.136 Uiso 1 1 calc R U . . . H4S2 H 0.6581 0.1015 0.2150 0.136 Uiso 1 1 calc R U . . . C5S C 0.8833(8) 0.0554(5) 0.1843(4) 0.100(3) Uani 1 1 d D U . . . H5S1 H 0.9093 0.1106 0.1493 0.119 Uiso 0.792(15) 1 calc R U P B 1 H5S2 H 0.9685 0.0213 0.2133 0.119 Uiso 0.792(15) 1 calc R U P B 1 H5S3 H 0.8550 0.0329 0.1454 0.119 Uiso 0.208(15) 1 calc R U P B 2 H5S4 H 0.9590 0.0075 0.2125 0.119 Uiso 0.208(15) 1 calc R U P B 2 C6S C 0.8575(15) 0.0011(6) 0.1349(6) 0.119(5) Uani 0.792(15) 1 d D U P B 1 H6S1 H 0.7907 -0.0372 0.1663 0.178 Uiso 0.792(15) 1 d R U P B 1 H6S2 H 0.9527 -0.0356 0.1175 0.178 Uiso 0.792(15) 1 d R U P B 1 H6S3 H 0.8122 0.0411 0.0890 0.178 Uiso 0.792(15) 1 d R U P B 1 C6S' C 0.950(5) 0.1352(17) 0.142(3) 0.186(18) Uani 0.208(15) 1 d D U P B 2 H6S4 H 0.9039 0.1697 0.0945 0.279 Uiso 0.208(15) 1 d R U P B 2 H6S5 H 1.0572 0.1140 0.1269 0.279 Uiso 0.208(15) 1 d R U P B 2 H6S6 H 0.9345 0.1727 0.1777 0.279 Uiso 0.208(15) 1 d R U P B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.02285(16) 0.02700(17) 0.02325(16) -0.00563(11) -0.00051(10) -0.01017(11) F1 0.0247(12) 0.083(2) 0.0391(13) -0.0183(13) -0.0015(10) -0.0181(12) F2 0.0408(16) 0.066(2) 0.082(2) -0.0278(18) -0.0260(15) 0.0118(14) F3 0.0607(19) 0.081(2) 0.0400(15) 0.0101(15) -0.0031(13) -0.0395(17) F4 0.0267(12) 0.0664(18) 0.0306(12) -0.0147(12) 0.0003(9) -0.0074(11) O1 0.077(3) 0.0373(18) 0.069(2) -0.0017(17) -0.023(2) -0.0280(18) O2 0.0257(14) 0.0398(16) 0.0474(17) -0.0119(14) 0.0019(12) -0.0064(12) O3 0.056(4) 0.031(3) 0.051(4) -0.007(3) 0.010(3) -0.017(3) O3' 0.053(4) 0.032(3) 0.044(4) -0.008(3) 0.004(4) -0.021(3) O3" 0.051(4) 0.032(4) 0.052(4) -0.008(4) 0.001(4) -0.014(4) O4 0.0246(13) 0.0437(16) 0.0362(15) -0.0151(13) 0.0019(11) -0.0122(12) O5 0.0317(14) 0.0284(13) 0.0299(13) -0.0061(11) -0.0052(11) -0.0128(11) O6 0.0378(16) 0.0543(19) 0.0331(15) -0.0103(14) -0.0070(12) -0.0198(14) N1 0.0256(15) 0.0253(15) 0.0256(14) -0.0042(12) -0.0007(12) -0.0097(12) N2 0.0237(14) 0.0259(15) 0.0273(15) -0.0042(12) 0.0001(12) -0.0121(12) N3 0.0241(14) 0.0239(15) 0.0275(15) -0.0043(12) -0.0024(12) -0.0101(12) N4 0.0235(14) 0.0239(15) 0.0233(14) -0.0054(11) 0.0000(11) -0.0109(11) N5 0.0219(14) 0.0296(16) 0.0250(14) -0.0047(12) 0.0005(11) -0.0091(12) C1 0.0282(18) 0.0245(17) 0.0240(16) -0.0003(14) -0.0028(14) -0.0070(14) C2 0.0285(18) 0.0263(19) 0.036(2) -0.0040(16) -0.0001(15) -0.0077(15) C3 0.033(2) 0.0229(18) 0.045(2) -0.0046(17) 0.0026(17) -0.0089(15) C4 0.0307(19) 0.0239(18) 0.0339(19) -0.0041(15) 0.0029(15) -0.0074(15) C5 0.034(2) 0.0240(18) 0.035(2) -0.0023(15) 0.0012(16) -0.0134(15) C6 0.0295(19) 0.0287(19) 0.0338(19) -0.0044(16) 0.0022(15) -0.0150(15) C7 0.033(2) 0.031(2) 0.039(2) -0.0062(17) 0.0092(16) -0.0175(16) C8 0.0296(19) 0.031(2) 0.038(2) -0.0072(16) 0.0080(16) -0.0158(16) C9 0.0229(16) 0.0281(18) 0.0272(17) -0.0064(14) 0.0010(13) -0.0116(14) C10 0.0227(16) 0.0295(18) 0.0237(16) -0.0041(14) -0.0028(13) -0.0095(14) C11 0.0216(16) 0.0243(17) 0.0285(17) -0.0048(14) -0.0049(13) -0.0065(13) C12 0.0271(18) 0.0282(19) 0.042(2) -0.0100(16) 0.0043(16) -0.0105(15) C13 0.031(2) 0.0265(19) 0.052(2) -0.0119(18) 0.0051(18) -0.0126(16) C14 0.0249(17) 0.0278(19) 0.040(2) -0.0120(16) 0.0004(15) -0.0102(14) C15 0.0282(17) 0.0287(17) 0.0401(19) -0.0118(15) 0.0024(15) -0.0151(14) C16 0.0260(17) 0.0290(18) 0.0316(17) -0.0103(15) -0.0006(14) -0.0135(14) C17 0.0275(17) 0.0306(19) 0.0359(19) -0.0099(15) 0.0023(15) -0.0151(15) C18 0.0237(16) 0.0292(18) 0.0307(17) -0.0093(15) 0.0027(13) -0.0127(14) C19 0.0193(15) 0.0293(17) 0.0212(15) -0.0057(13) -0.0012(12) -0.0110(13) C20 0.0221(16) 0.0277(17) 0.0199(15) -0.0047(13) -0.0018(12) -0.0083(13) C21 0.0317(19) 0.033(2) 0.044(2) -0.0053(17) 0.0012(16) -0.0147(16) C22 0.086(4) 0.040(2) 0.046(3) -0.003(2) -0.013(2) -0.029(2) C23 0.088(4) 0.046(3) 0.057(3) -0.008(2) -0.021(3) -0.032(3) C24 0.050(2) 0.037(2) 0.055(3) -0.006(2) -0.011(2) -0.0195(19) C25 0.092(4) 0.043(3) 0.076(3) 0.007(3) -0.034(3) -0.029(3) C26 0.087(4) 0.041(3) 0.074(3) 0.001(2) -0.037(3) -0.027(3) C27 0.119(6) 0.040(3) 0.107(6) 0.006(3) -0.051(5) -0.038(4) C28 0.0260(17) 0.0237(17) 0.0293(17) -0.0045(14) 0.0003(13) -0.0115(13) C29 0.0291(19) 0.050(2) 0.038(2) -0.0183(19) -0.0049(16) -0.0078(17) C30 0.0291(19) 0.048(2) 0.046(2) -0.0167(19) -0.0073(17) -0.0105(17) C31 0.0274(18) 0.0270(18) 0.042(2) -0.0059(16) 0.0024(16) -0.0091(15) C32 0.0328(19) 0.036(2) 0.0306(18) -0.0050(16) -0.0009(15) -0.0085(16) C33 0.0270(18) 0.041(2) 0.0310(18) -0.0052(16) -0.0055(15) -0.0077(16) C34 0.040(2) 0.062(3) 0.065(3) -0.035(3) 0.005(2) -0.015(2) C35 0.029(3) 0.029(3) 0.039(3) -0.012(3) 0.004(3) -0.013(2) C36 0.032(3) 0.036(3) 0.047(3) -0.007(3) -0.002(3) -0.015(3) C37 0.037(3) 0.035(3) 0.049(3) -0.003(3) 0.001(3) -0.012(3) C38 0.040(3) 0.030(3) 0.048(3) -0.007(3) 0.002(3) -0.017(3) C39 0.039(3) 0.034(3) 0.051(3) -0.011(3) -0.003(3) -0.016(3) C40 0.032(3) 0.033(3) 0.044(3) -0.008(3) -0.004(3) -0.014(3) C41 0.065(7) 0.032(5) 0.066(8) 0.003(5) 0.000(7) -0.018(5) C35' 0.029(3) 0.030(3) 0.040(3) -0.013(3) 0.002(3) -0.015(3) C36' 0.037(3) 0.031(3) 0.046(3) -0.014(3) -0.001(3) -0.013(3) C37' 0.038(3) 0.034(3) 0.046(3) -0.009(3) -0.002(3) -0.017(3) C38' 0.042(3) 0.030(3) 0.048(3) -0.008(3) 0.000(3) -0.018(3) C39' 0.044(4) 0.032(3) 0.046(3) -0.014(3) -0.001(3) -0.017(3) C40' 0.040(3) 0.032(3) 0.042(3) -0.012(3) 0.000(3) -0.015(3) C41' 0.052(7) 0.032(6) 0.051(6) 0.000(5) 0.002(5) -0.018(5) C35" 0.031(3) 0.029(3) 0.045(4) -0.013(3) 0.004(4) -0.018(3) C36" 0.036(4) 0.033(4) 0.046(4) -0.011(3) 0.004(4) -0.014(4) C37" 0.041(4) 0.035(4) 0.047(4) -0.010(4) 0.000(4) -0.013(4) C38" 0.042(4) 0.032(3) 0.048(4) -0.008(3) 0.003(4) -0.016(3) C39" 0.040(3) 0.032(3) 0.048(3) -0.010(3) 0.002(3) -0.015(3) C40" 0.035(3) 0.030(3) 0.047(3) -0.010(3) 0.001(3) -0.015(3) C41" 0.064(8) 0.029(6) 0.046(8) -0.008(6) 0.002(8) -0.013(7) C42 0.0221(16) 0.0244(17) 0.0234(16) -0.0055(13) -0.0010(13) -0.0096(13) C43 0.0241(17) 0.0299(19) 0.0284(17) -0.0082(15) -0.0040(14) -0.0103(14) C44 0.0245(17) 0.0327(19) 0.0264(17) -0.0122(15) 0.0015(13) -0.0101(14) C45 0.0228(17) 0.0318(19) 0.0284(18) -0.0074(15) -0.0001(14) -0.0087(14) C46 0.0244(18) 0.038(2) 0.037(2) -0.0130(17) -0.0073(15) -0.0079(15) C47 0.0280(18) 0.038(2) 0.0269(17) -0.0136(16) -0.0039(14) -0.0101(15) C48 0.0244(19) 0.056(3) 0.049(3) -0.015(2) -0.0005(17) -0.0168(18) C49 0.0272(17) 0.0322(19) 0.0287(18) -0.0086(15) -0.0055(14) -0.0128(15) C50 0.0250(18) 0.049(2) 0.034(2) -0.0152(18) -0.0054(15) -0.0098(17) C51 0.036(2) 0.054(3) 0.048(3) -0.020(2) -0.0171(19) -0.002(2) C52 0.056(3) 0.043(3) 0.049(3) -0.002(2) -0.023(2) -0.011(2) C53 0.047(3) 0.051(3) 0.030(2) -0.0011(19) -0.0072(18) -0.025(2) C54 0.0285(19) 0.041(2) 0.0282(18) -0.0067(16) -0.0039(15) -0.0127(16) C1S 0.136(8) 0.084(6) 0.097(6) -0.009(5) -0.029(6) -0.014(5) C2S 0.134(8) 0.092(6) 0.116(7) -0.016(5) -0.011(6) -0.044(6) C3S 0.095(6) 0.105(7) 0.094(6) -0.001(5) -0.017(5) -0.029(5) C4S 0.101(7) 0.091(6) 0.152(9) -0.054(6) -0.014(6) -0.005(5) C5S 0.131(8) 0.079(5) 0.081(5) -0.008(4) -0.038(5) -0.007(5) C6S 0.199(12) 0.066(6) 0.096(7) -0.017(5) -0.042(7) -0.027(7) C6S' 0.19(2) 0.161(19) 0.20(3) -0.017(14) -0.009(15) -0.078(17) _geom_special_details ; ; 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 N5 1.739(3) . ? Ru1 O5 2.000(3) . ? Ru1 N3 2.055(3) . ? Ru1 N4 2.059(3) . ? Ru1 N2 2.061(3) . ? Ru1 N1 2.064(3) . ? F1 C50 1.351(5) . ? F2 C51 1.353(5) . ? F3 C53 1.353(5) . ? F4 C54 1.338(5) . ? O1 C24 1.391(6) . ? O1 C27 1.398(7) . ? O2 C31 1.375(5) . ? O2 C34 1.437(6) . ? O3 C38 1.383(8) . ? O3 C41 1.413(10) . ? O3' C38' 1.384(8) . ? O3' C41' 1.417(10) . ? O3" C38" 1.389(9) . ? O3" C41" 1.418(11) . ? O4 C45 1.364(4) . ? O4 C48 1.429(5) . ? O5 C49 1.316(5) . ? O6 N5 1.156(4) . ? N1 C4 1.374(5) . ? N1 C1 1.377(5) . ? N2 C9 1.371(5) . ? N2 C6 1.376(5) . ? N3 C11 1.373(4) . ? N3 C14 1.377(5) . ? N4 C19 1.364(4) . ? N4 C16 1.374(5) . ? C1 C20 1.405(5) . ? C1 C2 1.442(5) . ? C2 C3 1.366(5) . ? C2 H2 0.9500 . ? C3 C4 1.443(5) . ? C3 H3 0.9500 . ? C4 C5 1.405(5) . ? C5 C6 1.394(6) . ? C5 C21 1.511(5) . ? C6 C7 1.441(5) . ? C7 C8 1.357(6) . ? C7 H7 0.9500 . ? C8 C9 1.446(5) . ? C8 H8 0.9500 . ? C9 C10 1.391(5) . ? C10 C11 1.394(5) . ? C10 C28 1.506(5) . ? C11 C12 1.440(5) . ? C12 C13 1.353(5) . ? C12 H12 0.9500 . ? C13 C14 1.438(5) . ? C13 H13 0.9500 . ? C14 C15 1.406(5) . ? C15 C16 1.393(5) . ? C15 C35 1.516(6) . ? C15 C35' 1.519(6) . ? C15 C35" 1.540(7) . ? C16 C17 1.442(5) . ? C17 C18 1.356(5) . ? C17 H17 0.9500 . ? C18 C19 1.442(5) . ? C18 H18 0.9500 . ? C19 C20 1.400(5) . ? C20 C42 1.500(5) . ? C21 C26 1.354(7) . ? C21 C22 1.378(7) . ? C22 C23 1.388(7) . ? C22 H22 0.9500 . ? C23 C24 1.348(7) . ? C23 H23 0.9500 . ? C24 C25 1.351(8) . ? C25 C26 1.418(7) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C27 H27A 0.9800 . ? C27 H27B 0.9801 . ? C27 H27C 0.9800 . ? C28 C29 1.378(5) . ? C28 C33 1.395(5) . ? C29 C30 1.396(6) . ? C29 H29 0.9500 . ? C30 C31 1.375(6) . ? C30 H30 0.9500 . ? C31 C32 1.392(6) . ? C32 C33 1.397(6) . ? C32 H32 0.9500 . ? C33 H33 0.9500 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 C36 1.375(6) . ? C35 C40 1.380(6) . ? C36 C37 1.390(7) . ? C36 H36 0.9500 . ? C37 C38 1.393(5) . ? C37 H37 0.9500 . ? C38 C39 1.396(5) . ? C39 C40 1.391(7) . ? C39 H39 0.9500 . ? C40 H40 0.9500 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C35' C36' 1.379(7) . ? C35' C40' 1.380(6) . ? C36' C37' 1.390(7) . ? C36' H36' 0.9500 . ? C37' C38' 1.393(6) . ? C37' H37' 0.9500 . ? C38' C39' 1.393(6) . ? C39' C40' 1.391(7) . ? C39' H39' 0.9500 . ? C40' H40' 0.9500 . ? C41' H41D 0.9799 . ? C41' H41E 0.9801 . ? C41' H41F 0.9800 . ? C35" C40" 1.379(7) . ? C35" C36" 1.381(7) . ? C36" C37" 1.387(8) . ? C36" H36" 0.9500 . ? C37" C38" 1.400(6) . ? C37" H37" 0.9500 . ? C38" C39" 1.399(6) . ? C39" C40" 1.389(8) . ? C39" H39" 0.9500 . ? C40" H40" 0.9500 . ? C41" H41G 0.9800 . ? C41" H41H 0.9800 . ? C41" H41I 0.9800 . ? C42 C47 1.392(5) . ? C42 C43 1.396(5) . ? C43 C44 1.386(5) . ? C43 H43 0.9500 . ? C44 C45 1.402(5) . ? C44 H44 0.9500 . ? C45 C46 1.382(5) . ? C46 C47 1.393(5) . ? C46 H46 0.9500 . ? C47 H47 0.9500 . ? C48 H48A 0.9801 . ? C48 H48B 0.9799 . ? C48 H48C 0.9801 . ? C49 C54 1.399(5) . ? C49 C50 1.403(5) . ? C50 C51 1.367(7) . ? C51 C52 1.386(7) . ? C52 C53 1.377(7) . ? C52 H52 0.9500 . ? C53 C54 1.373(6) . ? C1S C2S 1.508(5) . ? C1S H1S1 0.9800 . ? C1S H1S2 0.9800 . ? C1S H1S3 0.9800 . ? C2S C3S 1.491(5) . ? C2S H2S1 0.9900 . ? C2S H2S2 0.9900 . ? C3S C4S 1.490(5) . ? C3S H3S1 0.9900 . ? C3S H3S2 0.9900 . ? C4S C5S 1.518(5) . ? C4S H4S1 0.9900 . ? C4S H4S2 0.9900 . ? C5S C6S 1.518(6) . ? C5S C6S' 1.523(6) . ? C5S H5S1 0.9900 . ? C5S H5S2 0.9900 . ? C5S H5S3 0.9900 . ? C5S H5S4 0.9900 . ? C6S H6S1 0.9799 . ? C6S H6S2 0.9800 . ? C6S H6S3 0.9800 . ? C6S' H6S4 0.9800 . ? C6S' H6S5 0.9799 . ? C6S' H6S6 0.9799 . ? 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 N5 Ru1 O5 177.85(12) . . ? N5 Ru1 N3 92.56(13) . . ? O5 Ru1 N3 88.77(11) . . ? N5 Ru1 N4 90.34(13) . . ? O5 Ru1 N4 87.98(11) . . ? N3 Ru1 N4 90.12(12) . . ? N5 Ru1 N2 95.91(13) . . ? O5 Ru1 N2 85.77(11) . . ? N3 Ru1 N2 89.74(12) . . ? N4 Ru1 N2 173.75(11) . . ? N5 Ru1 N1 93.57(13) . . ? O5 Ru1 N1 85.09(12) . . ? N3 Ru1 N1 173.86(12) . . ? N4 Ru1 N1 89.74(12) . . ? N2 Ru1 N1 89.73(12) . . ? C24 O1 C27 117.8(4) . . ? C31 O2 C34 115.9(3) . . ? C38 O3 C41 118.6(7) . . ? C38' O3' C41' 117.5(8) . . ? C38" O3" C41" 116.9(9) . . ? C45 O4 C48 116.6(3) . . ? C49 O5 Ru1 127.5(2) . . ? C4 N1 C1 107.8(3) . . ? C4 N1 Ru1 126.0(2) . . ? C1 N1 Ru1 126.0(2) . . ? C9 N2 C6 108.0(3) . . ? C9 N2 Ru1 125.8(2) . . ? C6 N2 Ru1 126.2(2) . . ? C11 N3 C14 107.6(3) . . ? C11 N3 Ru1 126.1(2) . . ? C14 N3 Ru1 126.3(2) . . ? C19 N4 C16 108.3(3) . . ? C19 N4 Ru1 126.1(2) . . ? C16 N4 Ru1 125.6(2) . . ? O6 N5 Ru1 173.1(3) . . ? N1 C1 C20 125.5(3) . . ? N1 C1 C2 108.9(3) . . ? C20 C1 C2 125.6(3) . . ? C3 C2 C1 107.2(3) . . ? C3 C2 H2 126.4 . . ? C1 C2 H2 126.4 . . ? C2 C3 C4 107.3(3) . . ? C2 C3 H3 126.3 . . ? C4 C3 H3 126.3 . . ? N1 C4 C5 126.6(4) . . ? N1 C4 C3 108.8(3) . . ? C5 C4 C3 124.5(4) . . ? C6 C5 C4 124.7(4) . . ? C6 C5 C21 118.7(3) . . ? C4 C5 C21 116.6(4) . . ? N2 C6 C5 126.6(3) . . ? N2 C6 C7 108.8(3) . . ? C5 C6 C7 124.6(4) . . ? C8 C7 C6 107.1(3) . . ? C8 C7 H7 126.4 . . ? C6 C7 H7 126.4 . . ? C7 C8 C9 107.8(3) . . ? C7 C8 H8 126.1 . . ? C9 C8 H8 126.1 . . ? N2 C9 C10 126.4(3) . . ? N2 C9 C8 108.3(3) . . ? C10 C9 C8 125.2(3) . . ? C9 C10 C11 125.5(3) . . ? C9 C10 C28 117.6(3) . . ? C11 C10 C28 116.9(3) . . ? N3 C11 C10 126.0(3) . . ? N3 C11 C12 108.7(3) . . ? C10 C11 C12 125.1(3) . . ? C13 C12 C11 107.5(3) . . ? C13 C12 H12 126.2 . . ? C11 C12 H12 126.2 . . ? C12 C13 C14 107.5(3) . . ? C12 C13 H13 126.3 . . ? C14 C13 H13 126.3 . . ? N3 C14 C15 125.9(3) . . ? N3 C14 C13 108.7(3) . . ? C15 C14 C13 125.4(4) . . ? C16 C15 C14 125.0(4) . . ? C16 C15 C35 116.8(9) . . ? C14 C15 C35 117.9(9) . . ? C16 C15 C35' 117.8(12) . . ? C14 C15 C35' 117.1(12) . . ? C16 C15 C35" 113.9(9) . . ? C14 C15 C35" 118.9(10) . . ? N4 C16 C15 127.0(3) . . ? N4 C16 C17 108.3(3) . . ? C15 C16 C17 124.8(3) . . ? C18 C17 C16 107.5(3) . . ? C18 C17 H17 126.3 . . ? C16 C17 H17 126.3 . . ? C17 C18 C19 107.3(3) . . ? C17 C18 H18 126.3 . . ? C19 C18 H18 126.3 . . ? N4 C19 C20 126.5(3) . . ? N4 C19 C18 108.6(3) . . ? C20 C19 C18 124.8(3) . . ? C19 C20 C1 125.3(3) . . ? C19 C20 C42 116.2(3) . . ? C1 C20 C42 118.5(3) . . ? C26 C21 C22 117.2(4) . . ? C26 C21 C5 121.8(4) . . ? C22 C21 C5 121.0(4) . . ? C21 C22 C23 121.0(5) . . ? C21 C22 H22 119.5 . . ? C23 C22 H22 119.5 . . ? C24 C23 C22 120.9(5) . . ? C24 C23 H23 119.6 . . ? C22 C23 H23 119.6 . . ? C23 C24 C25 120.0(5) . . ? C23 C24 O1 117.0(5) . . ? C25 C24 O1 123.0(5) . . ? C24 C25 C26 118.9(5) . . ? C24 C25 H25 120.5 . . ? C26 C25 H25 120.5 . . ? C21 C26 C25 122.0(5) . . ? C21 C26 H26 119.0 . . ? C25 C26 H26 119.0 . . ? O1 C27 H27A 109.5 . . ? O1 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? O1 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C29 C28 C33 118.3(4) . . ? C29 C28 C10 121.1(3) . . ? C33 C28 C10 120.5(3) . . ? C28 C29 C30 120.5(4) . . ? C28 C29 H29 119.7 . . ? C30 C29 H29 119.7 . . ? C31 C30 C29 120.8(4) . . ? C31 C30 H30 119.6 . . ? C29 C30 H30 119.6 . . ? O2 C31 C30 116.3(4) . . ? O2 C31 C32 123.8(4) . . ? C30 C31 C32 119.9(4) . . ? C31 C32 C33 118.7(4) . . ? C31 C32 H32 120.7 . . ? C33 C32 H32 120.7 . . ? C28 C33 C32 121.7(4) . . ? C28 C33 H33 119.1 . . ? C32 C33 H33 119.1 . . ? O2 C34 H34A 109.5 . . ? O2 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? O2 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C36 C35 C40 119.3(6) . . ? C36 C35 C15 118.8(6) . . ? C40 C35 C15 121.7(6) . . ? C35 C36 C37 122.0(7) . . ? C35 C36 H36 119.0 . . ? C37 C36 H36 119.0 . . ? C36 C37 C38 118.5(6) . . ? C36 C37 H37 120.7 . . ? C38 C37 H37 120.7 . . ? O3 C38 C37 122.4(8) . . ? O3 C38 C39 116.6(7) . . ? C37 C38 C39 119.8(7) . . ? C40 C39 C38 120.2(6) . . ? C40 C39 H39 119.9 . . ? C38 C39 H39 119.9 . . ? C35 C40 C39 120.1(7) . . ? C35 C40 H40 120.0 . . ? C39 C40 H40 120.0 . . ? O3 C41 H41A 109.5 . . ? O3 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? O3 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C36' C35' C40' 119.6(7) . . ? C36' C35' C15 118.1(7) . . ? C40' C35' C15 122.1(7) . . ? C35' C36' C37' 121.3(8) . . ? C35' C36' H36' 119.4 . . ? C37' C36' H36' 119.4 . . ? C36' C37' C38' 118.5(7) . . ? C36' C37' H37' 120.8 . . ? C38' C37' H37' 120.8 . . ? O3' C38' C37' 119.9(10) . . ? O3' C38' C39' 116.5(9) . . ? C37' C38' C39' 120.9(8) . . ? C40' C39' C38' 119.0(7) . . ? C40' C39' H39' 120.5 . . ? C38' C39' H39' 120.5 . . ? C35' C40' C39' 120.7(7) . . ? C35' C40' H40' 119.7 . . ? C39' C40' H40' 119.7 . . ? O3' C41' H41D 109.5 . . ? O3' C41' H41E 109.5 . . ? H41D C41' H41E 109.5 . . ? O3' C41' H41F 109.5 . . ? H41D C41' H41F 109.5 . . ? H41E C41' H41F 109.5 . . ? C40" C35" C36" 115.7(8) . . ? C40" C35" C15 118.7(10) . . ? C36" C35" C15 125.6(10) . . ? C35" C36" C37" 123.4(9) . . ? C35" C36" H36" 118.3 . . ? C37" C36" H36" 118.3 . . ? C36" C37" C38" 119.9(8) . . ? C36" C37" H37" 120.1 . . ? C38" C37" H37" 120.1 . . ? O3" C38" C39" 123.2(10) . . ? O3" C38" C37" 119.0(11) . . ? C39" C38" C37" 117.8(8) . . ? C40" C39" C38" 119.8(8) . . ? C40" C39" H39" 120.1 . . ? C38" C39" H39" 120.1 . . ? C35" C40" C39" 123.4(9) . . ? C35" C40" H40" 118.3 . . ? C39" C40" H40" 118.3 . . ? O3" C41" H41G 109.4 . . ? O3" C41" H41H 109.5 . . ? H41G C41" H41H 109.5 . . ? O3" C41" H41I 109.5 . . ? H41G C41" H41I 109.5 . . ? H41H C41" H41I 109.5 . . ? C47 C42 C43 118.0(3) . . ? C47 C42 C20 119.7(3) . . ? C43 C42 C20 122.1(3) . . ? C44 C43 C42 120.9(3) . . ? C44 C43 H43 119.5 . . ? C42 C43 H43 119.5 . . ? C43 C44 C45 120.0(3) . . ? C43 C44 H44 120.0 . . ? C45 C44 H44 120.0 . . ? O4 C45 C46 124.7(3) . . ? O4 C45 C44 115.5(3) . . ? C46 C45 C44 119.7(3) . . ? C45 C46 C47 119.5(3) . . ? C45 C46 H46 120.2 . . ? C47 C46 H46 120.2 . . ? C42 C47 C46 121.7(3) . . ? C42 C47 H47 119.1 . . ? C46 C47 H47 119.1 . . ? O4 C48 H48A 109.5 . . ? O4 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? O4 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? O5 C49 C54 122.2(4) . . ? O5 C49 C50 122.3(3) . . ? C54 C49 C50 115.4(4) . . ? F1 C50 C51 119.0(4) . . ? F1 C50 C49 118.8(4) . . ? C51 C50 C49 122.2(4) . . ? F2 C51 C50 118.3(4) . . ? F2 C51 C52 120.1(5) . . ? C50 C51 C52 121.6(4) . . ? C53 C52 C51 117.0(4) . . ? C53 C52 H52 121.5 . . ? C51 C52 H52 121.5 . . ? F3 C53 C54 118.0(4) . . ? F3 C53 C52 120.0(4) . . ? C54 C53 C52 121.9(4) . . ? F4 C54 C53 119.4(4) . . ? F4 C54 C49 118.7(4) . . ? C53 C54 C49 121.9(4) . . ? C2S C1S H1S1 109.5 . . ? C2S C1S H1S2 109.5 . . ? H1S1 C1S H1S2 109.5 . . ? C2S C1S H1S3 109.4 . . ? H1S1 C1S H1S3 109.5 . . ? H1S2 C1S H1S3 109.5 . . ? C3S C2S C1S 113.2(6) . . ? C3S C2S H2S1 108.9 . . ? C1S C2S H2S1 108.9 . . ? C3S C2S H2S2 108.9 . . ? C1S C2S H2S2 108.9 . . ? H2S1 C2S H2S2 107.7 . . ? C4S C3S C2S 116.6(6) . . ? C4S C3S H3S1 108.1 . . ? C2S C3S H3S1 108.1 . . ? C4S C3S H3S2 108.1 . . ? C2S C3S H3S2 108.1 . . ? H3S1 C3S H3S2 107.3 . . ? C3S C4S C5S 113.1(5) . . ? C3S C4S H4S1 109.0 . . ? C5S C4S H4S1 109.0 . . ? C3S C4S H4S2 109.0 . . ? C5S C4S H4S2 109.0 . . ? H4S1 C4S H4S2 107.8 . . ? C6S C5S C4S 112.0(6) . . ? C4S C5S C6S' 111.6(7) . . ? C6S C5S H5S1 109.2 . . ? C4S C5S H5S1 109.2 . . ? C6S C5S H5S2 109.2 . . ? C4S C5S H5S2 109.2 . . ? H5S1 C5S H5S2 107.9 . . ? C4S C5S H5S3 109.3 . . ? C6S' C5S H5S3 109.3 . . ? C4S C5S H5S4 109.3 . . ? C6S' C5S H5S4 109.3 . . ? H5S3 C5S H5S4 108.0 . . ? C5S C6S H6S1 109.6 . . ? C5S C6S H6S2 109.6 . . ? H6S1 C6S H6S2 109.5 . . ? C5S C6S H6S3 109.3 . . ? H6S1 C6S H6S3 109.5 . . ? H6S2 C6S H6S3 109.5 . . ? C5S C6S' H6S4 111.4 . . ? C5S C6S' H6S5 108.6 . . ? H6S4 C6S' H6S5 109.5 . . ? C5S C6S' H6S6 108.4 . . ? H6S4 C6S' H6S6 109.5 . . ? H6S5 C6S' H6S6 109.5 . . ? 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 C4 N1 C1 C20 178.0(4) . . . . ? Ru1 N1 C1 C20 -7.4(5) . . . . ? C4 N1 C1 C2 -0.5(4) . . . . ? Ru1 N1 C1 C2 174.1(2) . . . . ? N1 C1 C2 C3 1.5(4) . . . . ? C20 C1 C2 C3 -177.0(4) . . . . ? C1 C2 C3 C4 -1.8(5) . . . . ? C1 N1 C4 C5 178.7(4) . . . . ? Ru1 N1 C4 C5 4.1(6) . . . . ? C1 N1 C4 C3 -0.6(4) . . . . ? Ru1 N1 C4 C3 -175.2(3) . . . . ? C2 C3 C4 N1 1.6(5) . . . . ? C2 C3 C4 C5 -177.7(4) . . . . ? N1 C4 C5 C6 -3.2(7) . . . . ? C3 C4 C5 C6 176.0(4) . . . . ? N1 C4 C5 C21 177.7(4) . . . . ? C3 C4 C5 C21 -3.1(6) . . . . ? C9 N2 C6 C5 179.6(4) . . . . ? Ru1 N2 C6 C5 -1.9(6) . . . . ? C9 N2 C6 C7 -0.7(4) . . . . ? Ru1 N2 C6 C7 177.8(3) . . . . ? C4 C5 C6 N2 2.0(7) . . . . ? C21 C5 C6 N2 -178.9(4) . . . . ? C4 C5 C6 C7 -177.6(4) . . . . ? C21 C5 C6 C7 1.5(6) . . . . ? N2 C6 C7 C8 0.5(5) . . . . ? C5 C6 C7 C8 -179.8(4) . . . . ? C6 C7 C8 C9 -0.1(5) . . . . ? C6 N2 C9 C10 -177.3(4) . . . . ? Ru1 N2 C9 C10 4.2(5) . . . . ? C6 N2 C9 C8 0.6(4) . . . . ? Ru1 N2 C9 C8 -177.9(3) . . . . ? C7 C8 C9 N2 -0.3(5) . . . . ? C7 C8 C9 C10 177.6(4) . . . . ? N2 C9 C10 C11 -0.3(6) . . . . ? C8 C9 C10 C11 -177.9(4) . . . . ? N2 C9 C10 C28 177.0(3) . . . . ? C8 C9 C10 C28 -0.6(6) . . . . ? C14 N3 C11 C10 175.1(4) . . . . ? Ru1 N3 C11 C10 -4.9(5) . . . . ? C14 N3 C11 C12 -0.2(4) . . . . ? Ru1 N3 C11 C12 179.8(3) . . . . ? C9 C10 C11 N3 0.6(6) . . . . ? C28 C10 C11 N3 -176.6(3) . . . . ? C9 C10 C11 C12 175.1(4) . . . . ? C28 C10 C11 C12 -2.1(5) . . . . ? N3 C11 C12 C13 -0.3(5) . . . . ? C10 C11 C12 C13 -175.6(4) . . . . ? C11 C12 C13 C14 0.6(5) . . . . ? C11 N3 C14 C15 -177.5(4) . . . . ? Ru1 N3 C14 C15 2.5(6) . . . . ? C11 N3 C14 C13 0.5(4) . . . . ? Ru1 N3 C14 C13 -179.5(3) . . . . ? C12 C13 C14 N3 -0.7(5) . . . . ? C12 C13 C14 C15 177.4(4) . . . . ? N3 C14 C15 C16 -2.9(7) . . . . ? C13 C14 C15 C16 179.4(4) . . . . ? N3 C14 C15 C35 -177.7(5) . . . . ? C13 C14 C15 C35 4.6(7) . . . . ? N3 C14 C15 C35' 179.0(5) . . . . ? C13 C14 C15 C35' 1.3(7) . . . . ? N3 C14 C15 C35" 159.6(8) . . . . ? C13 C14 C15 C35" -18.1(9) . . . . ? C19 N4 C16 C15 -179.4(4) . . . . ? Ru1 N4 C16 C15 2.9(6) . . . . ? C19 N4 C16 C17 0.9(4) . . . . ? Ru1 N4 C16 C17 -176.8(2) . . . . ? C14 C15 C16 N4 0.0(7) . . . . ? C35 C15 C16 N4 174.9(5) . . . . ? C35' C15 C16 N4 178.1(5) . . . . ? C35" C15 C16 N4 -163.3(9) . . . . ? C14 C15 C16 C17 179.6(4) . . . . ? C35 C15 C16 C17 -5.5(7) . . . . ? C35' C15 C16 C17 -2.3(7) . . . . ? C35" C15 C16 C17 16.3(10) . . . . ? N4 C16 C17 C18 -0.6(4) . . . . ? C15 C16 C17 C18 179.7(4) . . . . ? C16 C17 C18 C19 0.1(4) . . . . ? C16 N4 C19 C20 -178.4(3) . . . . ? Ru1 N4 C19 C20 -0.7(5) . . . . ? C16 N4 C19 C18 -0.9(4) . . . . ? Ru1 N4 C19 C18 176.8(2) . . . . ? C17 C18 C19 N4 0.5(4) . . . . ? C17 C18 C19 C20 178.0(3) . . . . ? N4 C19 C20 C1 6.9(6) . . . . ? C18 C19 C20 C1 -170.2(4) . . . . ? N4 C19 C20 C42 -174.8(3) . . . . ? C18 C19 C20 C42 8.1(5) . . . . ? N1 C1 C20 C19 -2.4(6) . . . . ? C2 C1 C20 C19 175.8(4) . . . . ? N1 C1 C20 C42 179.3(3) . . . . ? C2 C1 C20 C42 -2.5(5) . . . . ? C6 C5 C21 C26 -87.0(6) . . . . ? C4 C5 C21 C26 92.1(6) . . . . ? C6 C5 C21 C22 91.4(6) . . . . ? C4 C5 C21 C22 -89.4(6) . . . . ? C26 C21 C22 C23 -2.4(9) . . . . ? C5 C21 C22 C23 179.1(5) . . . . ? C21 C22 C23 C24 -0.8(10) . . . . ? C22 C23 C24 C25 2.4(10) . . . . ? C22 C23 C24 O1 -179.7(6) . . . . ? C27 O1 C24 C23 170.3(6) . . . . ? C27 O1 C24 C25 -11.9(9) . . . . ? C23 C24 C25 C26 -0.7(10) . . . . ? O1 C24 C25 C26 -178.5(6) . . . . ? C22 C21 C26 C25 4.2(9) . . . . ? C5 C21 C26 C25 -177.3(6) . . . . ? C24 C25 C26 C21 -2.7(11) . . . . ? C9 C10 C28 C29 -73.3(5) . . . . ? C11 C10 C28 C29 104.2(4) . . . . ? C9 C10 C28 C33 108.6(4) . . . . ? C11 C10 C28 C33 -73.9(5) . . . . ? C33 C28 C29 C30 -0.2(6) . . . . ? C10 C28 C29 C30 -178.3(4) . . . . ? C28 C29 C30 C31 -0.4(7) . . . . ? C34 O2 C31 C30 -178.4(4) . . . . ? C34 O2 C31 C32 0.4(6) . . . . ? C29 C30 C31 O2 179.5(4) . . . . ? C29 C30 C31 C32 0.6(7) . . . . ? O2 C31 C32 C33 -179.0(4) . . . . ? C30 C31 C32 C33 -0.2(6) . . . . ? C29 C28 C33 C32 0.6(6) . . . . ? C10 C28 C33 C32 178.8(4) . . . . ? C31 C32 C33 C28 -0.4(6) . . . . ? C16 C15 C35 C36 110.3(16) . . . . ? C14 C15 C35 C36 -74.4(18) . . . . ? C35' C15 C35 C36 1(34) . . . . ? C35" C15 C35 C36 24(3) . . . . ? C16 C15 C35 C40 -64.8(19) . . . . ? C14 C15 C35 C40 110.4(16) . . . . ? C35' C15 C35 C40 -174(37) . . . . ? C35" C15 C35 C40 -151(5) . . . . ? C40 C35 C36 C37 0(3) . . . . ? C15 C35 C36 C37 -175.0(12) . . . . ? C35 C36 C37 C38 0(2) . . . . ? C41 O3 C38 C37 -22(2) . . . . ? C41 O3 C38 C39 170.1(14) . . . . ? C36 C37 C38 O3 -168.8(13) . . . . ? C36 C37 C38 C39 -1(2) . . . . ? O3 C38 C39 C40 170.1(12) . . . . ? C37 C38 C39 C40 2(2) . . . . ? C36 C35 C40 C39 0(3) . . . . ? C15 C35 C40 C39 175.4(13) . . . . ? C38 C39 C40 C35 -1(2) . . . . ? C16 C15 C35' C36' 76(2) . . . . ? C14 C15 C35' C36' -105(2) . . . . ? C35 C15 C35' C36' 149(38) . . . . ? C35" C15 C35' C36' -5(4) . . . . ? C16 C15 C35' C40' -99(2) . . . . ? C14 C15 C35' C40' 79(2) . . . . ? C35 C15 C35' C40' -27(34) . . . . ? C35" C15 C35' C40' 180(8) . . . . ? C40' C35' C36' C37' -3(3) . . . . ? C15 C35' C36' C37' -178.3(16) . . . . ? C35' C36' C37' C38' -1(3) . . . . ? C41' O3' C38' C37' 26(3) . . . . ? C41' O3' C38' C39' -172.1(16) . . . . ? C36' C37' C38' O3' 164.0(17) . . . . ? C36' C37' C38' C39' 3(3) . . . . ? O3' C38' C39' C40' -164.0(17) . . . . ? C37' C38' C39' C40' -3(3) . . . . ? C36' C35' C40' C39' 3(3) . . . . ? C15 C35' C40' C39' 178.8(17) . . . . ? C38' C39' C40' C35' -1(3) . . . . ? C16 C15 C35" C40" -129.6(19) . . . . ? C14 C15 C35" C40" 66(2) . . . . ? C35 C15 C35" C40" -27(3) . . . . ? C35' C15 C35" C40" -23(5) . . . . ? C16 C15 C35" C36" 48(3) . . . . ? C14 C15 C35" C36" -116(2) . . . . ? C35 C15 C35" C36" 151(5) . . . . ? C35' C15 C35" C36" 155(7) . . . . ? C40" C35" C36" C37" -2(4) . . . . ? C15 C35" C36" C37" -179(2) . . . . ? C35" C36" C37" C38" 3(4) . . . . ? C41" O3" C38" C39" 4(4) . . . . ? C41" O3" C38" C37" -175(3) . . . . ? C36" C37" C38" O3" 179(2) . . . . ? C36" C37" C38" C39" 0(3) . . . . ? O3" C38" C39" C40" 177(2) . . . . ? C37" C38" C39" C40" -4(3) . . . . ? C36" C35" C40" C39" -3(4) . . . . ? C15 C35" C40" C39" 174.9(19) . . . . ? C38" C39" C40" C35" 6(4) . . . . ? C19 C20 C42 C47 56.3(5) . . . . ? C1 C20 C42 C47 -125.2(4) . . . . ? C19 C20 C42 C43 -119.0(4) . . . . ? C1 C20 C42 C43 59.4(5) . . . . ? C47 C42 C43 C44 -0.5(5) . . . . ? C20 C42 C43 C44 175.0(3) . . . . ? C42 C43 C44 C45 -0.7(6) . . . . ? C48 O4 C45 C46 -0.1(6) . . . . ? C48 O4 C45 C44 178.0(4) . . . . ? C43 C44 C45 O4 -177.2(3) . . . . ? C43 C44 C45 C46 1.0(6) . . . . ? O4 C45 C46 C47 178.0(4) . . . . ? C44 C45 C46 C47 -0.1(6) . . . . ? C43 C42 C47 C46 1.4(6) . . . . ? C20 C42 C47 C46 -174.1(4) . . . . ? C45 C46 C47 C42 -1.1(6) . . . . ? Ru1 O5 C49 C54 93.9(4) . . . . ? Ru1 O5 C49 C50 -90.5(4) . . . . ? O5 C49 C50 F1 1.0(6) . . . . ? C54 C49 C50 F1 176.8(3) . . . . ? O5 C49 C50 C51 -177.7(4) . . . . ? C54 C49 C50 C51 -1.9(6) . . . . ? F1 C50 C51 F2 1.2(6) . . . . ? C49 C50 C51 F2 180.0(4) . . . . ? F1 C50 C51 C52 -178.9(4) . . . . ? C49 C50 C51 C52 -0.2(7) . . . . ? F2 C51 C52 C53 -178.4(4) . . . . ? C50 C51 C52 C53 1.7(7) . . . . ? C51 C52 C53 F3 177.5(4) . . . . ? C51 C52 C53 C54 -1.1(7) . . . . ? F3 C53 C54 F4 -1.4(6) . . . . ? C52 C53 C54 F4 177.2(4) . . . . ? F3 C53 C54 C49 -179.7(4) . . . . ? C52 C53 C54 C49 -1.0(7) . . . . ? O5 C49 C54 F4 0.1(6) . . . . ? C50 C49 C54 F4 -175.8(3) . . . . ? O5 C49 C54 C53 178.3(4) . . . . ? C50 C49 C54 C53 2.5(6) . . . . ? C1S C2S C3S C4S 170.4(9) . . . . ? C2S C3S C4S C5S -175.2(8) . . . . ? C3S C4S C5S C6S 74.4(10) . . . . ? C3S C4S C5S C6S' -151(3) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C7 H7 O2 0.95 2.60 3.408(5) 143.5 2_466 C17 H17 F2 0.95 2.62 3.392(5) 138.8 1_655 C41' H41F F2 0.98 2.88 3.383(19) 113.0 2_575 C46 H46 O5 0.95 2.36 3.163(5) 142.1 1_655 C48 H48B F4 0.98 2.35 3.321(5) 170.8 2_765 _refine_diff_density_max 2.519 _refine_diff_density_min -1.193 _refine_diff_density_rms 0.131