# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Brooker, S.' _publ_contact_author_email sbrooker@alkali.otago.ac.nz _publ_section_title ; Heteroleptic N6 coordinated ruthenium(II) complexes as building blocks for the formation of discrete Ru2Ag2 complexes ; _publ_author_name S.Brooker # Attachment '- hw081.cif' data_hw081 _database_code_depnum_ccdc_archive 'CCDC 777613' #TrackingRef '- hw081.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27 H22 Cl N7 O Ru' _chemical_formula_weight 597.04 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 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 25.991(7) _cell_length_b 13.823(5) _cell_length_c 19.904(7) _cell_angle_alpha 90.00 _cell_angle_beta 106.586(14) _cell_angle_gamma 90.00 _cell_volume 6853(4) _cell_formula_units_Z 8 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 1153 _cell_measurement_theta_min 2.536 _cell_measurement_theta_max 21.916 _exptl_crystal_description plate _exptl_crystal_colour dark-red _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.157 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2416 _exptl_absorpt_coefficient_mu 0.562 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9155 _exptl_absorpt_correction_T_max 0.9779 _exptl_absorpt_process_details 'SCALE (Bruker AXS Inc)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Kappa Apex II area detector' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24626 _diffrn_reflns_av_R_equivalents 0.1493 _diffrn_reflns_av_sigmaI/netI 0.1392 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.68 _diffrn_reflns_theta_max 23.82 _reflns_number_total 5261 _reflns_number_gt 3390 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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. [Ru(II) (terpy) (terdentate amide ligand bound only via 2 donors) Cl]; asymmetric unit contains all of this. Solvents, CHCl3 and water, of crystallisation present but modelling of these was not ideal. R1 went from 10.78% to 8.21% post-SQUEEZE. SQUEEZE found 346 e/cell and a void volume of 2395 A3/cell. This is consistent with approx. 1/2CHCl3 and 1H2O per cell. Data was weak so SHEL 1000 0.88 was employed to cut at 2theta = 47.6 degrees. All non-H ANIS. No disorder. All H calc and ride. Top 4 Q's are approx 1Angstrom from Ru1; Q5 peak height only 0.60 vs deepest hole is -0.57. ; _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^)+(0.1172P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5261 _refine_ls_number_parameters 334 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1252 _refine_ls_R_factor_gt 0.0821 _refine_ls_wR_factor_ref 0.2202 _refine_ls_wR_factor_gt 0.2003 _refine_ls_goodness_of_fit_ref 0.971 _refine_ls_restrained_S_all 0.971 _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 Ru1 Ru 0.26958(3) 0.98174(5) 0.85831(3) 0.0277(3) Uani 1 1 d . . . Cl1 Cl 0.19200(9) 0.99851(15) 0.75667(11) 0.0351(6) Uani 1 1 d . . . O1 O 0.3505(2) 1.0182(5) 1.0693(3) 0.0416(16) Uani 1 1 d . . . N3 N 0.2463(3) 0.8406(5) 0.8696(3) 0.0318(18) Uani 1 1 d . . . N6 N 0.3280(3) 0.9695(5) 0.9535(3) 0.0326(18) Uani 1 1 d . . . N1 N 0.3096(3) 1.0934(5) 0.8255(3) 0.0260(16) Uani 1 1 d . . . N2 N 0.3073(3) 0.9110(5) 0.8018(3) 0.0265(16) Uani 1 1 d . . . N4 N 0.2360(3) 1.0594(5) 0.9223(4) 0.0353(19) Uani 1 1 d . . . C6 C 0.3390(3) 0.9590(6) 0.7705(4) 0.027(2) Uani 1 1 d . . . C5 C 0.3406(3) 1.0641(7) 0.7853(4) 0.028(2) Uani 1 1 d . . . C10 C 0.3019(3) 0.8140(6) 0.7956(4) 0.026(2) Uani 1 1 d . . . C14 C 0.2031(4) 0.7154(7) 0.9175(5) 0.043(2) Uani 1 1 d . . . H14 H 0.1797 0.6969 0.9443 0.051 Uiso 1 1 calc R . . C12 C 0.2586(3) 0.6773(6) 0.8429(4) 0.031(2) Uani 1 1 d . . . H12 H 0.2740 0.6319 0.8184 0.037 Uiso 1 1 calc R . . C4 C 0.3712(3) 1.1305(6) 0.7587(4) 0.033(2) Uani 1 1 d . . . H4 H 0.3932 1.1087 0.7310 0.040 Uiso 1 1 calc R . . C2 C 0.3356(4) 1.2567(6) 0.8168(5) 0.037(2) Uani 1 1 d . . . H2 H 0.3329 1.3229 0.8279 0.044 Uiso 1 1 calc R . . C13 C 0.2272(4) 0.6449(7) 0.8851(4) 0.041(2) Uani 1 1 d . . . H13 H 0.2223 0.5778 0.8916 0.050 Uiso 1 1 calc R . . C11 C 0.2673(3) 0.7747(6) 0.8369(4) 0.027(2) Uani 1 1 d . . . C15 C 0.2140(4) 0.8120(6) 0.9097(4) 0.037(2) Uani 1 1 d . . . H15 H 0.1988 0.8596 0.9326 0.045 Uiso 1 1 calc R . . C8 C 0.3612(4) 0.8105(6) 0.7237(5) 0.038(2) Uani 1 1 d . . . H8 H 0.3795 0.7756 0.6964 0.046 Uiso 1 1 calc R . . C7 C 0.3670(4) 0.9109(7) 0.7304(4) 0.034(2) Uani 1 1 d . . . H7 H 0.3893 0.9453 0.7083 0.041 Uiso 1 1 calc R . . C9 C 0.3287(3) 0.7621(6) 0.7571(4) 0.034(2) Uani 1 1 d . . . H9 H 0.3250 0.6937 0.7534 0.040 Uiso 1 1 calc R . . C1 C 0.3082(4) 1.1878(6) 0.8413(5) 0.039(2) Uani 1 1 d . . . H1 H 0.2871 1.2073 0.8708 0.046 Uiso 1 1 calc R . . C3 C 0.3689(4) 1.2271(7) 0.7737(5) 0.040(2) Uani 1 1 d . . . H3 H 0.3887 1.2734 0.7560 0.048 Uiso 1 1 calc R . . N7 N 0.4887(3) 0.8548(7) 1.0348(4) 0.059(3) Uani 1 1 d . . . C21 C 0.3740(4) 0.9034(8) 0.9642(5) 0.051(3) Uani 1 1 d . . . H21A H 0.3646 0.8496 0.9301 0.061 Uiso 1 1 calc R . . H21B H 0.3828 0.8757 1.0120 0.061 Uiso 1 1 calc R . . C27 C 0.5340(4) 0.8041(8) 1.0515(5) 0.047(3) Uani 1 1 d . . . H27 H 0.5482 0.7822 1.0984 0.056 Uiso 1 1 calc R . . C23 C 0.4703(4) 0.8928(8) 0.9692(5) 0.053(3) Uani 1 1 d . . . C22 C 0.4213(4) 0.9567(8) 0.9549(5) 0.049(3) Uani 1 1 d . . . H22A H 0.4292 1.0128 0.9871 0.059 Uiso 1 1 calc R . . H22B H 0.4128 0.9816 0.9063 0.059 Uiso 1 1 calc R . . C24 C 0.4949(4) 0.8670(8) 0.9191(5) 0.054(3) Uani 1 1 d . . . H24 H 0.4804 0.8894 0.8724 0.064 Uiso 1 1 calc R . . C25 C 0.5383(5) 0.8119(9) 0.9346(6) 0.063(3) Uani 1 1 d . . . H25 H 0.5538 0.7927 0.8989 0.076 Uiso 1 1 calc R . . C26 C 0.5610(4) 0.7821(8) 1.0033(5) 0.048(3) Uani 1 1 d . . . H26 H 0.5940 0.7478 1.0166 0.057 Uiso 1 1 calc R . . C20 C 0.3199(4) 1.0160(7) 1.0073(5) 0.038(2) Uani 1 1 d . . . C19 C 0.2683(4) 1.0685(7) 0.9896(4) 0.035(2) Uani 1 1 d . . . N5 N 0.2062(5) 1.1739(8) 1.0229(5) 0.088(4) Uani 1 1 d . . . C17 C 0.1745(6) 1.1615(10) 0.9558(6) 0.093(5) Uani 1 1 d . . . H17 H 0.1405 1.1927 0.9422 0.111 Uiso 1 1 calc R . . C18 C 0.2521(5) 1.1255(8) 1.0384(6) 0.063(3) Uani 1 1 d . . . H18 H 0.2752 1.1295 1.0848 0.075 Uiso 1 1 calc R . . C16 C 0.1891(4) 1.1060(8) 0.9068(5) 0.053(3) Uani 1 1 d . . . H16 H 0.1653 1.1009 0.8609 0.064 Uiso 1 1 calc R . . 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 0.0356(5) 0.0302(4) 0.0189(4) 0.0021(3) 0.0104(3) 0.0073(4) Cl1 0.0390(13) 0.0352(14) 0.0300(12) 0.0055(9) 0.0081(10) 0.0007(10) O1 0.043(4) 0.060(4) 0.023(3) -0.003(3) 0.012(3) 0.002(3) N3 0.050(5) 0.028(4) 0.027(4) 0.003(3) 0.026(4) -0.002(4) N6 0.037(4) 0.047(5) 0.015(4) -0.007(3) 0.008(3) 0.013(4) N1 0.026(4) 0.041(5) 0.006(3) 0.006(3) -0.003(3) 0.003(3) N2 0.032(4) 0.036(4) 0.010(3) 0.005(3) 0.003(3) 0.004(3) N4 0.048(5) 0.037(4) 0.028(4) 0.005(3) 0.022(4) 0.014(4) C6 0.028(5) 0.035(6) 0.014(4) 0.002(4) 0.000(4) -0.001(4) C5 0.026(5) 0.043(6) 0.011(4) 0.001(4) -0.002(4) 0.000(4) C10 0.035(5) 0.027(5) 0.015(4) 0.001(4) 0.002(4) 0.002(4) C14 0.049(6) 0.053(7) 0.024(5) 0.006(5) 0.006(5) -0.006(5) C12 0.027(5) 0.038(6) 0.021(5) 0.002(4) -0.003(4) 0.005(4) C4 0.032(5) 0.035(6) 0.031(5) 0.003(4) 0.005(4) -0.003(4) C2 0.049(6) 0.020(5) 0.036(5) -0.001(4) 0.003(5) 0.004(4) C13 0.052(6) 0.037(6) 0.027(5) 0.003(4) -0.001(5) -0.003(5) C11 0.031(5) 0.036(5) 0.012(4) -0.001(4) 0.002(4) -0.002(4) C15 0.059(7) 0.032(5) 0.025(5) -0.004(4) 0.018(5) 0.001(5) C8 0.055(6) 0.038(6) 0.033(5) -0.001(4) 0.032(5) -0.003(5) C7 0.042(6) 0.049(6) 0.015(4) -0.003(4) 0.014(4) 0.003(5) C9 0.038(6) 0.027(5) 0.034(5) -0.004(4) 0.008(4) 0.010(4) C1 0.051(6) 0.030(6) 0.033(5) 0.005(4) 0.008(5) 0.014(5) C3 0.053(6) 0.032(6) 0.032(5) 0.006(4) 0.006(5) -0.011(5) N7 0.046(6) 0.104(8) 0.025(5) 0.002(5) 0.006(4) 0.024(5) C21 0.041(6) 0.096(9) 0.013(5) 0.004(5) 0.002(4) -0.003(6) C27 0.033(6) 0.075(8) 0.031(5) 0.001(5) 0.007(5) 0.002(5) C23 0.043(7) 0.086(9) 0.027(5) -0.003(5) 0.007(5) 0.017(6) C22 0.062(7) 0.053(7) 0.027(5) -0.001(5) 0.003(5) 0.006(5) C24 0.054(7) 0.079(8) 0.027(6) -0.004(5) 0.010(5) 0.010(6) C25 0.055(7) 0.083(9) 0.054(7) 0.002(6) 0.022(6) 0.028(7) C26 0.044(6) 0.068(7) 0.027(5) 0.006(5) 0.002(5) 0.020(5) C20 0.041(6) 0.053(6) 0.024(5) 0.006(5) 0.017(4) -0.001(5) C19 0.042(6) 0.043(6) 0.020(5) -0.004(4) 0.010(4) -0.006(5) N5 0.131(10) 0.110(9) 0.026(5) 0.015(5) 0.028(6) 0.090(8) C17 0.129(12) 0.115(12) 0.043(8) 0.015(7) 0.039(8) 0.090(10) C18 0.097(9) 0.060(7) 0.042(6) 0.004(5) 0.037(7) 0.046(7) C16 0.054(7) 0.079(8) 0.030(6) -0.004(5) 0.018(5) 0.028(6) _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 N2 1.953(6) . y Ru1 N4 2.042(7) . y Ru1 N1 2.068(7) . y Ru1 N6 2.069(7) . y Ru1 N3 2.073(7) . y Ru1 Cl1 2.426(2) . y O1 C20 1.264(11) . ? N3 C11 1.326(10) . ? N3 C15 1.370(10) . ? N6 C20 1.317(11) . ? N6 C21 1.470(12) . ? N1 C1 1.345(11) . ? N1 C5 1.351(10) . ? N2 C6 1.341(10) . ? N2 C10 1.351(10) . ? N4 C16 1.335(11) . ? N4 C19 1.369(11) . ? C6 C7 1.391(11) . ? C6 C5 1.481(12) . ? C5 C4 1.412(11) . ? C10 C9 1.375(11) . ? C10 C11 1.483(11) . ? C14 C15 1.383(13) . ? C14 C13 1.411(13) . ? C14 H14 0.9500 . ? C12 C11 1.376(12) . ? C12 C13 1.402(12) . ? C12 H12 0.9500 . ? C4 C3 1.373(12) . ? C4 H4 0.9500 . ? C2 C1 1.360(12) . ? C2 C3 1.439(12) . ? C2 H2 0.9500 . ? C13 H13 0.9500 . ? C15 H15 0.9500 . ? C8 C9 1.387(11) . ? C8 C7 1.398(12) . ? C8 H8 0.9500 . ? C7 H7 0.9500 . ? C9 H9 0.9500 . ? C1 H1 0.9500 . ? C3 H3 0.9500 . ? N7 C27 1.328(12) . ? N7 C23 1.362(12) . ? C21 C22 1.491(13) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C27 C26 1.373(12) . ? C27 H27 0.9500 . ? C23 C24 1.375(13) . ? C23 C22 1.509(13) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C24 C25 1.321(14) . ? C24 H24 0.9500 . ? C25 C26 1.389(14) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C20 C19 1.476(13) . ? C19 C18 1.405(12) . ? N5 C18 1.324(13) . ? N5 C17 1.366(16) . ? C17 C16 1.376(13) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C16 H16 0.9500 . ? 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 N2 Ru1 N4 175.4(3) . . y N2 Ru1 N1 79.1(3) . . y N4 Ru1 N1 98.5(3) . . y N2 Ru1 N6 97.4(3) . . y N4 Ru1 N6 78.7(3) . . y N1 Ru1 N6 92.6(3) . . y N2 Ru1 N3 78.6(3) . . y N4 Ru1 N3 103.7(3) . . y N1 Ru1 N3 157.7(3) . . y N6 Ru1 N3 89.1(3) . . y N2 Ru1 Cl1 90.1(2) . . y N4 Ru1 Cl1 93.9(2) . . y N1 Ru1 Cl1 92.21(18) . . y N6 Ru1 Cl1 171.75(18) . . y N3 Ru1 Cl1 88.9(2) . . y C11 N3 C15 119.6(7) . . ? C11 N3 Ru1 114.8(5) . . ? C15 N3 Ru1 125.5(6) . . ? C20 N6 C21 119.9(7) . . ? C20 N6 Ru1 117.3(6) . . ? C21 N6 Ru1 122.5(5) . . ? C1 N1 C5 119.2(7) . . ? C1 N1 Ru1 127.0(6) . . ? C5 N1 Ru1 113.8(6) . . ? C6 N2 C10 120.7(7) . . ? C6 N2 Ru1 119.8(6) . . ? C10 N2 Ru1 119.5(5) . . ? C16 N4 C19 116.5(8) . . ? C16 N4 Ru1 129.4(6) . . ? C19 N4 Ru1 114.0(6) . . ? N2 C6 C7 121.4(8) . . ? N2 C6 C5 112.2(7) . . ? C7 C6 C5 126.4(8) . . ? N1 C5 C4 121.5(8) . . ? N1 C5 C6 115.1(7) . . ? C4 C5 C6 123.4(7) . . ? N2 C10 C9 120.8(7) . . ? N2 C10 C11 112.1(7) . . ? C9 C10 C11 127.0(8) . . ? C15 C14 C13 118.9(9) . . ? C15 C14 H14 120.6 . . ? C13 C14 H14 120.6 . . ? C11 C12 C13 120.2(8) . . ? C11 C12 H12 119.9 . . ? C13 C12 H12 119.9 . . ? C3 C4 C5 119.1(8) . . ? C3 C4 H4 120.5 . . ? C5 C4 H4 120.5 . . ? C1 C2 C3 118.7(8) . . ? C1 C2 H2 120.7 . . ? C3 C2 H2 120.7 . . ? C12 C13 C14 117.6(9) . . ? C12 C13 H13 121.2 . . ? C14 C13 H13 121.2 . . ? N3 C11 C12 121.9(7) . . ? N3 C11 C10 114.9(7) . . ? C12 C11 C10 123.1(8) . . ? N3 C15 C14 121.7(8) . . ? N3 C15 H15 119.2 . . ? C14 C15 H15 119.2 . . ? C9 C8 C7 119.8(8) . . ? C9 C8 H8 120.1 . . ? C7 C8 H8 120.1 . . ? C6 C7 C8 118.0(8) . . ? C6 C7 H7 121.0 . . ? C8 C7 H7 121.0 . . ? C10 C9 C8 119.3(8) . . ? C10 C9 H9 120.3 . . ? C8 C9 H9 120.3 . . ? N1 C1 C2 122.9(8) . . ? N1 C1 H1 118.5 . . ? C2 C1 H1 118.5 . . ? C4 C3 C2 118.5(8) . . ? C4 C3 H3 120.7 . . ? C2 C3 H3 120.7 . . ? C27 N7 C23 119.2(8) . . ? N6 C21 C22 109.9(9) . . ? N6 C21 H21A 109.7 . . ? C22 C21 H21A 109.7 . . ? N6 C21 H21B 109.7 . . ? C22 C21 H21B 109.7 . . ? H21A C21 H21B 108.2 . . ? N7 C27 C26 122.2(9) . . ? N7 C27 H27 118.9 . . ? C26 C27 H27 118.9 . . ? N7 C23 C24 119.1(9) . . ? N7 C23 C22 116.9(8) . . ? C24 C23 C22 123.8(9) . . ? C21 C22 C23 111.7(9) . . ? C21 C22 H22A 109.3 . . ? C23 C22 H22A 109.3 . . ? C21 C22 H22B 109.3 . . ? C23 C22 H22B 109.3 . . ? H22A C22 H22B 107.9 . . ? C25 C24 C23 121.4(10) . . ? C25 C24 H24 119.3 . . ? C23 C24 H24 119.3 . . ? C24 C25 C26 119.7(10) . . ? C24 C25 H25 120.2 . . ? C26 C25 H25 120.2 . . ? C27 C26 C25 117.7(9) . . ? C27 C26 H26 121.2 . . ? C25 C26 H26 121.2 . . ? O1 C20 N6 127.1(9) . . ? O1 C20 C19 119.8(8) . . ? N6 C20 C19 113.1(8) . . ? N4 C19 C18 120.5(9) . . ? N4 C19 C20 116.7(7) . . ? C18 C19 C20 122.8(9) . . ? C18 N5 C17 114.6(9) . . ? N5 C17 C16 123.4(11) . . ? N5 C17 H17 118.3 . . ? C16 C17 H17 118.3 . . ? N5 C18 C19 123.4(11) . . ? N5 C18 H18 118.3 . . ? C19 C18 H18 118.3 . . ? N4 C16 C17 121.6(10) . . ? N4 C16 H16 119.2 . . ? C17 C16 H16 119.2 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Ru1 N3 C11 1.2(6) . . . . ? N4 Ru1 N3 C11 -174.7(6) . . . . ? N1 Ru1 N3 C11 -1.7(11) . . . . ? N6 Ru1 N3 C11 -96.5(6) . . . . ? Cl1 Ru1 N3 C11 91.6(6) . . . . ? N2 Ru1 N3 C15 178.0(8) . . . . ? N4 Ru1 N3 C15 2.2(8) . . . . ? N1 Ru1 N3 C15 175.2(7) . . . . ? N6 Ru1 N3 C15 80.4(7) . . . . ? Cl1 Ru1 N3 C15 -91.6(7) . . . . ? N2 Ru1 N6 C20 174.8(7) . . . . ? N4 Ru1 N6 C20 -2.7(7) . . . . ? N1 Ru1 N6 C20 95.5(7) . . . . ? N3 Ru1 N6 C20 -106.8(7) . . . . ? Cl1 Ru1 N6 C20 -30(2) . . . . ? N2 Ru1 N6 C21 -12.3(7) . . . . ? N4 Ru1 N6 C21 170.2(7) . . . . ? N1 Ru1 N6 C21 -91.7(7) . . . . ? N3 Ru1 N6 C21 66.1(7) . . . . ? Cl1 Ru1 N6 C21 142.6(12) . . . . ? N2 Ru1 N1 C1 -179.8(7) . . . . ? N4 Ru1 N1 C1 -3.8(7) . . . . ? N6 Ru1 N1 C1 -82.8(7) . . . . ? N3 Ru1 N1 C1 -176.9(7) . . . . ? Cl1 Ru1 N1 C1 90.5(7) . . . . ? N2 Ru1 N1 C5 -1.1(5) . . . . ? N4 Ru1 N1 C5 174.9(5) . . . . ? N6 Ru1 N1 C5 95.9(5) . . . . ? N3 Ru1 N1 C5 1.8(10) . . . . ? Cl1 Ru1 N1 C5 -90.8(5) . . . . ? N4 Ru1 N2 C6 -59(4) . . . . ? N1 Ru1 N2 C6 0.3(6) . . . . ? N6 Ru1 N2 C6 -90.9(6) . . . . ? N3 Ru1 N2 C6 -178.6(6) . . . . ? Cl1 Ru1 N2 C6 92.6(6) . . . . ? N4 Ru1 N2 C10 120(3) . . . . ? N1 Ru1 N2 C10 179.3(6) . . . . ? N6 Ru1 N2 C10 88.0(6) . . . . ? N3 Ru1 N2 C10 0.4(6) . . . . ? Cl1 Ru1 N2 C10 -88.5(6) . . . . ? N2 Ru1 N4 C16 147(3) . . . . ? N1 Ru1 N4 C16 88.6(9) . . . . ? N6 Ru1 N4 C16 179.6(9) . . . . ? N3 Ru1 N4 C16 -94.1(9) . . . . ? Cl1 Ru1 N4 C16 -4.3(9) . . . . ? N2 Ru1 N4 C19 -29(4) . . . . ? N1 Ru1 N4 C19 -87.3(6) . . . . ? N6 Ru1 N4 C19 3.7(6) . . . . ? N3 Ru1 N4 C19 90.0(6) . . . . ? Cl1 Ru1 N4 C19 179.9(6) . . . . ? C10 N2 C6 C7 0.4(11) . . . . ? Ru1 N2 C6 C7 179.3(6) . . . . ? C10 N2 C6 C5 -178.5(7) . . . . ? Ru1 N2 C6 C5 0.4(9) . . . . ? C1 N1 C5 C4 -0.6(11) . . . . ? Ru1 N1 C5 C4 -179.4(6) . . . . ? C1 N1 C5 C6 -179.6(7) . . . . ? Ru1 N1 C5 C6 1.7(8) . . . . ? N2 C6 C5 N1 -1.4(10) . . . . ? C7 C6 C5 N1 179.8(7) . . . . ? N2 C6 C5 C4 179.7(7) . . . . ? C7 C6 C5 C4 0.8(13) . . . . ? C6 N2 C10 C9 0.1(12) . . . . ? Ru1 N2 C10 C9 -178.9(6) . . . . ? C6 N2 C10 C11 177.2(7) . . . . ? Ru1 N2 C10 C11 -1.8(9) . . . . ? N1 C5 C4 C3 -0.7(12) . . . . ? C6 C5 C4 C3 178.1(8) . . . . ? C11 C12 C13 C14 3.2(12) . . . . ? C15 C14 C13 C12 -3.8(13) . . . . ? C15 N3 C11 C12 -1.3(12) . . . . ? Ru1 N3 C11 C12 175.7(6) . . . . ? C15 N3 C11 C10 -179.5(7) . . . . ? Ru1 N3 C11 C10 -2.5(9) . . . . ? C13 C12 C11 N3 -0.6(12) . . . . ? C13 C12 C11 C10 177.4(7) . . . . ? N2 C10 C11 N3 2.8(10) . . . . ? C9 C10 C11 N3 179.6(8) . . . . ? N2 C10 C11 C12 -175.4(7) . . . . ? C9 C10 C11 C12 1.5(13) . . . . ? C11 N3 C15 C14 0.6(13) . . . . ? Ru1 N3 C15 C14 -176.1(7) . . . . ? C13 C14 C15 N3 2.0(14) . . . . ? N2 C6 C7 C8 -0.2(12) . . . . ? C5 C6 C7 C8 178.6(8) . . . . ? C9 C8 C7 C6 -0.5(13) . . . . ? N2 C10 C9 C8 -0.8(13) . . . . ? C11 C10 C9 C8 -177.4(8) . . . . ? C7 C8 C9 C10 1.0(13) . . . . ? C5 N1 C1 C2 1.9(13) . . . . ? Ru1 N1 C1 C2 -179.5(6) . . . . ? C3 C2 C1 N1 -1.8(14) . . . . ? C5 C4 C3 C2 0.8(13) . . . . ? C1 C2 C3 C4 0.4(13) . . . . ? C20 N6 C21 C22 -91.5(10) . . . . ? Ru1 N6 C21 C22 95.8(8) . . . . ? C23 N7 C27 C26 -5.1(16) . . . . ? C27 N7 C23 C24 8.7(17) . . . . ? C27 N7 C23 C22 -175.0(10) . . . . ? N6 C21 C22 C23 177.0(7) . . . . ? N7 C23 C22 C21 -61.0(13) . . . . ? C24 C23 C22 C21 115.1(12) . . . . ? N7 C23 C24 C25 -4.9(18) . . . . ? C22 C23 C24 C25 179.0(11) . . . . ? C23 C24 C25 C26 -2.6(19) . . . . ? N7 C27 C26 C25 -2.3(17) . . . . ? C24 C25 C26 C27 6.1(18) . . . . ? C21 N6 C20 O1 7.4(15) . . . . ? Ru1 N6 C20 O1 -179.6(7) . . . . ? C21 N6 C20 C19 -171.9(8) . . . . ? Ru1 N6 C20 C19 1.1(10) . . . . ? C16 N4 C19 C18 -0.8(13) . . . . ? Ru1 N4 C19 C18 175.6(8) . . . . ? C16 N4 C19 C20 179.2(8) . . . . ? Ru1 N4 C19 C20 -4.4(10) . . . . ? O1 C20 C19 N4 -177.2(8) . . . . ? N6 C20 C19 N4 2.2(12) . . . . ? O1 C20 C19 C18 2.8(14) . . . . ? N6 C20 C19 C18 -177.8(9) . . . . ? C18 N5 C17 C16 -2(2) . . . . ? C17 N5 C18 C19 2.3(19) . . . . ? N4 C19 C18 N5 -0.9(17) . . . . ? C20 C19 C18 N5 179.1(11) . . . . ? C19 N4 C16 C17 0.9(16) . . . . ? Ru1 N4 C16 C17 -174.9(10) . . . . ? N5 C17 C16 N4 1(2) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 23.82 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.374 _refine_diff_density_min -0.573 _refine_diff_density_rms 0.138 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.000 -0.005 -0.004 1191.8 173.2 2 0.500 -0.198 0.196 1191.8 173.2 _platon_squeeze_details ; ; # Attachment '- hw099.cif' data_hw099 _database_code_depnum_ccdc_archive 'CCDC 777614' #TrackingRef '- hw099.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C29 H26 B2 F8 N8 O Ru' _chemical_formula_weight 777.27 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' B B 0.0013 0.0007 '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' _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 9.9592(14) _cell_length_b 11.1964(18) _cell_length_c 15.636(3) _cell_angle_alpha 72.889(8) _cell_angle_beta 74.776(7) _cell_angle_gamma 78.295(7) _cell_volume 1592.9(4) _cell_formula_units_Z 2 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 9233 _cell_measurement_theta_min 2.648 _cell_measurement_theta_max 26.436 _exptl_crystal_description black _exptl_crystal_colour red _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.621 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 780 _exptl_absorpt_coefficient_mu 0.578 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6851 _exptl_absorpt_correction_T_max 0.7454 _exptl_absorpt_process_details 'SCALE (Bruker AXS Inc)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Kappa Apex II area detector' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 46188 _diffrn_reflns_av_R_equivalents 0.0406 _diffrn_reflns_av_sigmaI/netI 0.0275 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.40 _diffrn_reflns_theta_max 26.46 _reflns_number_total 6529 _reflns_number_gt 6020 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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. [Ru(II) (terpy) (HL) (MeCN)](BF4)2 in asym unit. No disorder or solvent of crystallisation. HL is neutral ligand; but H has relocated from amide N to unbound pyridine N. This proton was found and x,y,z,U all freely refined. It is involved in an intramolecular H-bond to O1, the amide oxygen atom. ; _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^)+(0.0271P)^2^+2.5002P] 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 6529 _refine_ls_number_parameters 447 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0390 _refine_ls_R_factor_gt 0.0348 _refine_ls_wR_factor_ref 0.0820 _refine_ls_wR_factor_gt 0.0787 _refine_ls_goodness_of_fit_ref 1.095 _refine_ls_restrained_S_all 1.095 _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 Ru1 Ru 0.75181(2) 0.608060(17) 0.752294(13) 0.01823(7) Uani 1 1 d . . . N2 N 0.7098(2) 0.72937(19) 0.63927(14) 0.0195(4) Uani 1 1 d . . . N4 N 0.7923(2) 0.49213(19) 0.87392(14) 0.0201(4) Uani 1 1 d . . . N6 N 0.5974(2) 0.68404(19) 0.84657(14) 0.0203(4) Uani 1 1 d . . . N5 N 0.9074(2) 0.51096(19) 0.67446(14) 0.0193(4) Uani 1 1 d . . . N1 N 0.8788(2) 0.74277(19) 0.73539(14) 0.0192(4) Uani 1 1 d . . . N3 N 0.6038(2) 0.5243(2) 0.72733(15) 0.0227(4) Uani 1 1 d . . . N8 N 0.6010(2) 0.9047(2) 0.92370(15) 0.0250(5) Uani 1 1 d . . . H8X H 0.561(3) 0.837(3) 0.951(2) 0.031(8) Uiso 1 1 d . . . N7 N 0.8386(3) 0.3670(2) 1.05014(16) 0.0349(6) Uani 1 1 d . . . C5 C 0.8696(3) 0.8415(2) 0.66046(16) 0.0201(5) Uani 1 1 d . . . C2 C 1.0348(3) 0.8455(3) 0.77408(19) 0.0288(6) Uani 1 1 d . . . H2 H 1.0928 0.8441 0.8140 0.035 Uiso 1 1 calc R . . C28 C 0.9891(3) 0.4497(2) 0.63353(17) 0.0207(5) Uani 1 1 d . . . C19 C 0.7142(3) 0.5276(2) 0.94969(17) 0.0215(5) Uani 1 1 d . . . C29 C 1.0943(3) 0.3705(2) 0.58229(18) 0.0252(5) Uani 1 1 d . . . H29A H 1.1345 0.2978 0.6252 0.038 Uiso 1 1 calc R . . H29B H 1.1689 0.4195 0.5427 0.038 Uiso 1 1 calc R . . H29C H 1.0502 0.3410 0.5446 0.038 Uiso 1 1 calc R . . C23 C 0.5953(3) 0.9633(2) 0.83612(17) 0.0232(5) Uani 1 1 d . . . C4 C 0.9402(3) 0.9445(2) 0.64167(18) 0.0245(5) Uani 1 1 d . . . H4 H 0.9322 1.0125 0.5892 0.029 Uiso 1 1 calc R . . C21 C 0.4799(3) 0.7824(2) 0.82610(18) 0.0243(5) Uani 1 1 d . . . H21A H 0.4078 0.7820 0.8834 0.029 Uiso 1 1 calc R . . H21B H 0.4369 0.7614 0.7830 0.029 Uiso 1 1 calc R . . C20 C 0.6032(3) 0.6370(2) 0.93351(17) 0.0225(5) Uani 1 1 d . . . C1 C 0.9618(3) 0.7457(2) 0.78971(18) 0.0231(5) Uani 1 1 d . . . H1 H 0.9708 0.6762 0.8412 0.028 Uiso 1 1 calc R . . C6 C 0.7765(3) 0.8324(2) 0.60388(17) 0.0216(5) Uani 1 1 d . . . C14 C 0.4504(3) 0.3726(3) 0.7543(2) 0.0360(7) Uani 1 1 d . . . H14 H 0.4142 0.2975 0.7918 0.043 Uiso 1 1 calc R . . C18 C 0.7395(3) 0.4660(2) 1.03557(18) 0.0284(6) Uani 1 1 d . . . H18 H 0.6838 0.4955 1.0867 0.034 Uiso 1 1 calc R . . C3 C 1.0221(3) 0.9473(3) 0.69970(19) 0.0287(6) Uani 1 1 d . . . H3 H 1.0690 1.0181 0.6886 0.034 Uiso 1 1 calc R . . C15 C 0.5506(3) 0.4189(3) 0.7788(2) 0.0276(6) Uani 1 1 d . . . H15 H 0.5821 0.3745 0.8334 0.033 Uiso 1 1 calc R . . C8 C 0.6573(3) 0.8951(3) 0.48050(18) 0.0307(6) Uani 1 1 d . . . H8 H 0.6396 0.9525 0.4250 0.037 Uiso 1 1 calc R . . C10 C 0.6183(3) 0.7053(3) 0.59848(18) 0.0240(5) Uani 1 1 d . . . C11 C 0.5572(3) 0.5883(3) 0.64970(18) 0.0260(6) Uani 1 1 d . . . C16 C 0.8919(3) 0.3915(2) 0.88794(19) 0.0268(6) Uani 1 1 d . . . H16 H 0.9485 0.3618 0.8372 0.032 Uiso 1 1 calc R . . C22 C 0.5203(3) 0.9151(2) 0.78472(18) 0.0249(5) Uani 1 1 d . . . H22A H 0.5802 0.9180 0.7228 0.030 Uiso 1 1 calc R . . H22B H 0.4333 0.9744 0.7768 0.030 Uiso 1 1 calc R . . C27 C 0.6734(3) 0.9413(3) 0.97110(19) 0.0300(6) Uani 1 1 d . . . H27 H 0.6770 0.8949 1.0322 0.036 Uiso 1 1 calc R . . C17 C 0.9126(3) 0.3311(3) 0.97509(19) 0.0327(6) Uani 1 1 d . . . H17 H 0.9833 0.2601 0.9821 0.039 Uiso 1 1 calc R . . C7 C 0.7501(3) 0.9181(2) 0.52402(17) 0.0257(5) Uani 1 1 d . . . H7 H 0.7951 0.9918 0.4994 0.031 Uiso 1 1 calc R . . C9 C 0.5900(3) 0.7884(3) 0.51768(18) 0.0292(6) Uani 1 1 d . . . H9 H 0.5256 0.7725 0.4884 0.035 Uiso 1 1 calc R . . C26 C 0.7417(3) 1.0449(3) 0.9316(2) 0.0329(6) Uani 1 1 d . . . H26 H 0.7924 1.0714 0.9648 0.039 Uiso 1 1 calc R . . C12 C 0.4575(3) 0.5462(3) 0.6221(2) 0.0355(7) Uani 1 1 d . . . H12 H 0.4265 0.5920 0.5675 0.043 Uiso 1 1 calc R . . C13 C 0.4042(3) 0.4367(3) 0.6752(2) 0.0403(7) Uani 1 1 d . . . H13 H 0.3364 0.4059 0.6574 0.048 Uiso 1 1 calc R . . C25 C 0.7355(3) 1.1103(3) 0.8423(2) 0.0336(6) Uani 1 1 d . . . H25 H 0.7813 1.1832 0.8137 0.040 Uiso 1 1 calc R . . C24 C 0.6628(3) 1.0695(3) 0.7952(2) 0.0291(6) Uani 1 1 d . . . H24 H 0.6587 1.1145 0.7339 0.035 Uiso 1 1 calc R . . O1 O 0.5270(2) 0.67817(17) 1.00099(12) 0.0291(4) Uani 1 1 d . . . B1 B 0.7818(3) 0.2729(3) 0.5540(2) 0.0262(6) Uani 1 1 d . . . F11 F 0.67422(19) 0.20176(17) 0.56893(13) 0.0420(4) Uani 1 1 d . . . F12 F 0.81296(19) 0.26228(18) 0.63761(12) 0.0420(4) Uani 1 1 d . . . F13 F 0.7401(2) 0.39785(17) 0.51506(15) 0.0501(5) Uani 1 1 d . . . F14 F 0.8996(2) 0.22712(19) 0.49796(13) 0.0492(5) Uani 1 1 d . . . B2 B 0.1703(3) 0.1291(3) 0.8150(2) 0.0300(7) Uani 1 1 d . . . F21 F 0.19865(18) 0.20887(16) 0.85966(12) 0.0380(4) Uani 1 1 d . . . F22 F 0.03508(18) 0.16567(19) 0.80132(16) 0.0501(5) Uani 1 1 d . . . F23 F 0.2633(2) 0.14094(19) 0.73005(12) 0.0500(5) Uani 1 1 d . . . F24 F 0.18731(19) 0.00565(16) 0.86717(12) 0.0409(4) 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 Ru1 0.01936(11) 0.01606(11) 0.01970(11) -0.00522(8) -0.00388(7) -0.00288(7) N2 0.0186(10) 0.0214(10) 0.0186(10) -0.0092(8) -0.0016(8) 0.0000(8) N4 0.0219(11) 0.0158(10) 0.0223(10) -0.0062(8) -0.0021(8) -0.0037(8) N6 0.0202(11) 0.0168(10) 0.0228(11) -0.0049(8) -0.0033(8) -0.0024(8) N5 0.0216(11) 0.0175(10) 0.0200(10) -0.0044(8) -0.0062(8) -0.0040(8) N1 0.0187(10) 0.0168(10) 0.0215(10) -0.0064(8) -0.0016(8) -0.0022(8) N3 0.0197(11) 0.0216(11) 0.0286(12) -0.0118(9) -0.0009(8) -0.0043(8) N8 0.0274(12) 0.0199(11) 0.0233(11) -0.0070(9) 0.0003(9) 0.0009(9) N7 0.0408(15) 0.0309(13) 0.0271(12) -0.0041(10) -0.0073(10) 0.0034(10) C5 0.0202(12) 0.0182(12) 0.0187(12) -0.0052(9) 0.0009(9) -0.0016(9) C2 0.0295(15) 0.0324(15) 0.0297(14) -0.0106(12) -0.0082(11) -0.0093(11) C28 0.0248(13) 0.0187(12) 0.0197(12) -0.0033(10) -0.0067(10) -0.0052(10) C19 0.0229(13) 0.0180(12) 0.0221(12) -0.0042(10) -0.0014(10) -0.0051(9) C29 0.0246(14) 0.0252(13) 0.0261(13) -0.0107(11) -0.0038(10) -0.0006(10) C23 0.0215(13) 0.0206(12) 0.0222(12) -0.0055(10) -0.0013(10) 0.0046(10) C4 0.0262(14) 0.0185(12) 0.0243(13) -0.0042(10) 0.0011(10) -0.0036(10) C21 0.0193(13) 0.0243(13) 0.0282(13) -0.0086(11) -0.0033(10) 0.0003(10) C20 0.0247(13) 0.0166(12) 0.0232(13) -0.0035(10) -0.0002(10) -0.0049(10) C1 0.0242(13) 0.0228(13) 0.0237(13) -0.0051(10) -0.0078(10) -0.0039(10) C6 0.0204(13) 0.0223(12) 0.0196(12) -0.0068(10) -0.0006(9) 0.0002(9) C14 0.0299(16) 0.0316(15) 0.0498(19) -0.0173(14) 0.0007(13) -0.0135(12) C18 0.0342(15) 0.0230(13) 0.0228(13) -0.0044(11) -0.0027(11) 0.0007(11) C3 0.0292(15) 0.0270(14) 0.0323(15) -0.0128(12) 0.0006(11) -0.0112(11) C15 0.0256(14) 0.0241(13) 0.0337(15) -0.0125(11) 0.0013(11) -0.0070(10) C8 0.0308(15) 0.0328(15) 0.0210(13) -0.0017(11) -0.0051(11) 0.0042(11) C10 0.0207(13) 0.0291(14) 0.0255(13) -0.0145(11) -0.0052(10) 0.0008(10) C11 0.0217(13) 0.0314(14) 0.0289(14) -0.0159(11) -0.0053(10) -0.0008(10) C16 0.0301(15) 0.0205(13) 0.0272(14) -0.0075(11) -0.0040(11) 0.0016(10) C22 0.0228(13) 0.0232(13) 0.0253(13) -0.0059(10) -0.0043(10) 0.0031(10) C27 0.0338(16) 0.0278(14) 0.0278(14) -0.0128(11) -0.0069(11) 0.0056(11) C17 0.0354(16) 0.0288(15) 0.0282(14) -0.0054(12) -0.0083(12) 0.0074(12) C7 0.0269(14) 0.0233(13) 0.0211(13) -0.0031(10) -0.0018(10) 0.0009(10) C9 0.0264(14) 0.0372(16) 0.0262(14) -0.0135(12) -0.0091(11) 0.0032(11) C26 0.0320(16) 0.0345(16) 0.0370(16) -0.0168(13) -0.0100(12) -0.0005(12) C12 0.0300(16) 0.0419(17) 0.0420(17) -0.0175(14) -0.0107(13) -0.0072(13) C13 0.0308(16) 0.0472(19) 0.055(2) -0.0254(16) -0.0100(14) -0.0135(14) C25 0.0304(15) 0.0282(15) 0.0411(17) -0.0128(13) -0.0028(12) -0.0021(11) C24 0.0262(14) 0.0270(14) 0.0302(14) -0.0049(11) -0.0044(11) -0.0004(11) O1 0.0337(11) 0.0247(10) 0.0214(9) -0.0056(8) 0.0022(8) 0.0015(8) B1 0.0310(16) 0.0228(15) 0.0253(15) -0.0032(12) -0.0084(12) -0.0062(12) F11 0.0448(11) 0.0415(10) 0.0486(11) -0.0069(8) -0.0205(8) -0.0187(8) F12 0.0497(11) 0.0533(11) 0.0302(9) -0.0051(8) -0.0098(8) -0.0301(9) F13 0.0582(13) 0.0265(9) 0.0651(13) -0.0018(9) -0.0274(10) -0.0009(8) F14 0.0480(12) 0.0493(12) 0.0433(11) -0.0185(9) 0.0058(9) -0.0016(9) B2 0.0240(16) 0.0336(17) 0.0348(17) -0.0145(14) -0.0074(13) 0.0008(12) F21 0.0391(10) 0.0395(10) 0.0431(10) -0.0122(8) -0.0130(8) -0.0145(8) F22 0.0289(10) 0.0522(12) 0.0880(15) -0.0452(11) -0.0250(10) 0.0089(8) F23 0.0483(12) 0.0568(12) 0.0278(9) -0.0066(8) -0.0050(8) 0.0200(9) F24 0.0466(11) 0.0325(9) 0.0429(10) -0.0110(8) -0.0064(8) -0.0061(8) _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 N2 1.972(2) . y Ru1 N5 2.042(2) . y Ru1 N4 2.050(2) . y Ru1 N6 2.068(2) . y Ru1 N3 2.069(2) . y Ru1 N1 2.076(2) . y N2 C10 1.348(3) . ? N2 C6 1.349(3) . ? N4 C16 1.348(3) . ? N4 C19 1.354(3) . ? N6 C20 1.318(3) . ? N6 C21 1.467(3) . ? N5 C28 1.141(3) . ? N1 C1 1.342(3) . ? N1 C5 1.363(3) . ? N3 C15 1.339(3) . ? N3 C11 1.361(3) . ? N8 C23 1.344(3) . ? N8 C27 1.348(4) . ? N8 H8X 0.87(3) . ? N7 C18 1.335(4) . ? N7 C17 1.336(4) . ? C5 C4 1.389(3) . ? C5 C6 1.475(4) . ? C2 C3 1.381(4) . ? C2 C1 1.383(4) . ? C2 H2 0.9500 . ? C28 C29 1.458(3) . ? C19 C18 1.380(4) . ? C19 C20 1.485(3) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C23 C24 1.387(4) . ? C23 C22 1.493(4) . ? C4 C3 1.380(4) . ? C4 H4 0.9500 . ? C21 C22 1.526(4) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C20 O1 1.275(3) . ? C1 H1 0.9500 . ? C6 C7 1.383(4) . ? C14 C13 1.378(5) . ? C14 C15 1.392(4) . ? C14 H14 0.9500 . ? C18 H18 0.9500 . ? C3 H3 0.9500 . ? C15 H15 0.9500 . ? C8 C7 1.383(4) . ? C8 C9 1.388(4) . ? C8 H8 0.9500 . ? C10 C9 1.389(4) . ? C10 C11 1.475(4) . ? C11 C12 1.389(4) . ? C16 C17 1.380(4) . ? C16 H16 0.9500 . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C27 C26 1.366(4) . ? C27 H27 0.9500 . ? C17 H17 0.9500 . ? C7 H7 0.9500 . ? C9 H9 0.9500 . ? C26 C25 1.385(4) . ? C26 H26 0.9500 . ? C12 C13 1.382(4) . ? C12 H12 0.9500 . ? C13 H13 0.9500 . ? C25 C24 1.374(4) . ? C25 H25 0.9500 . ? C24 H24 0.9500 . ? B1 F14 1.374(4) . ? B1 F13 1.377(3) . ? B1 F12 1.387(3) . ? B1 F11 1.394(3) . ? B2 F22 1.379(4) . ? B2 F24 1.385(4) . ? B2 F23 1.393(4) . ? B2 F21 1.393(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Ru1 N5 89.44(8) . . y N2 Ru1 N4 176.05(8) . . y N5 Ru1 N4 93.75(8) . . y N2 Ru1 N6 98.52(8) . . y N5 Ru1 N6 171.81(8) . . y N4 Ru1 N6 78.37(8) . . y N2 Ru1 N3 79.21(9) . . y N5 Ru1 N3 89.80(8) . . y N4 Ru1 N3 103.10(8) . . y N6 Ru1 N3 89.82(8) . . y N2 Ru1 N1 79.30(8) . . y N5 Ru1 N1 91.77(8) . . y N4 Ru1 N1 98.25(8) . . y N6 Ru1 N1 91.59(8) . . y N3 Ru1 N1 158.44(9) . . y C10 N2 C6 122.0(2) . . ? C10 N2 Ru1 119.08(17) . . ? C6 N2 Ru1 118.87(17) . . ? C16 N4 C19 116.2(2) . . ? C16 N4 Ru1 128.78(17) . . ? C19 N4 Ru1 114.89(16) . . ? C20 N6 C21 117.0(2) . . ? C20 N6 Ru1 116.78(17) . . ? C21 N6 Ru1 126.23(16) . . ? C28 N5 Ru1 175.2(2) . . ? C1 N1 C5 118.0(2) . . ? C1 N1 Ru1 128.42(17) . . ? C5 N1 Ru1 113.51(16) . . ? C15 N3 C11 118.9(2) . . ? C15 N3 Ru1 127.45(19) . . ? C11 N3 Ru1 113.66(17) . . ? C23 N8 C27 123.0(2) . . ? C23 N8 H8X 119(2) . . ? C27 N8 H8X 117(2) . . ? C18 N7 C17 115.1(2) . . ? N1 C5 C4 121.5(2) . . ? N1 C5 C6 115.2(2) . . ? C4 C5 C6 123.3(2) . . ? C3 C2 C1 119.0(3) . . ? C3 C2 H2 120.5 . . ? C1 C2 H2 120.5 . . ? N5 C28 C29 179.2(3) . . ? N4 C19 C18 121.3(2) . . ? N4 C19 C20 115.6(2) . . ? C18 C19 C20 123.0(2) . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? N8 C23 C24 117.5(3) . . ? N8 C23 C22 121.1(2) . . ? C24 C23 C22 121.4(2) . . ? C3 C4 C5 119.6(2) . . ? C3 C4 H4 120.2 . . ? C5 C4 H4 120.2 . . ? N6 C21 C22 114.4(2) . . ? N6 C21 H21A 108.6 . . ? C22 C21 H21A 108.6 . . ? N6 C21 H21B 108.6 . . ? C22 C21 H21B 108.6 . . ? H21A C21 H21B 107.6 . . ? O1 C20 N6 126.6(2) . . ? O1 C20 C19 119.6(2) . . ? N6 C20 C19 113.8(2) . . ? N1 C1 C2 122.9(2) . . ? N1 C1 H1 118.5 . . ? C2 C1 H1 118.5 . . ? N2 C6 C7 119.9(2) . . ? N2 C6 C5 113.0(2) . . ? C7 C6 C5 127.0(2) . . ? C13 C14 C15 119.4(3) . . ? C13 C14 H14 120.3 . . ? C15 C14 H14 120.3 . . ? N7 C18 C19 123.0(3) . . ? N7 C18 H18 118.5 . . ? C19 C18 H18 118.5 . . ? C4 C3 C2 118.9(2) . . ? C4 C3 H3 120.6 . . ? C2 C3 H3 120.6 . . ? N3 C15 C14 121.7(3) . . ? N3 C15 H15 119.1 . . ? C14 C15 H15 119.1 . . ? C7 C8 C9 120.2(2) . . ? C7 C8 H8 119.9 . . ? C9 C8 H8 119.9 . . ? N2 C10 C9 119.8(2) . . ? N2 C10 C11 112.6(2) . . ? C9 C10 C11 127.6(2) . . ? N3 C11 C12 121.7(3) . . ? N3 C11 C10 115.4(2) . . ? C12 C11 C10 122.9(3) . . ? N4 C16 C17 120.8(2) . . ? N4 C16 H16 119.6 . . ? C17 C16 H16 119.6 . . ? C23 C22 C21 117.7(2) . . ? C23 C22 H22A 107.9 . . ? C21 C22 H22A 107.9 . . ? C23 C22 H22B 107.9 . . ? C21 C22 H22B 107.9 . . ? H22A C22 H22B 107.2 . . ? N8 C27 C26 120.3(3) . . ? N8 C27 H27 119.9 . . ? C26 C27 H27 119.9 . . ? N7 C17 C16 123.6(3) . . ? N7 C17 H17 118.2 . . ? C16 C17 H17 118.2 . . ? C8 C7 C6 119.1(3) . . ? C8 C7 H7 120.4 . . ? C6 C7 H7 120.4 . . ? C8 C9 C10 118.9(3) . . ? C8 C9 H9 120.5 . . ? C10 C9 H9 120.5 . . ? C27 C26 C25 118.7(3) . . ? C27 C26 H26 120.7 . . ? C25 C26 H26 120.7 . . ? C13 C12 C11 118.9(3) . . ? C13 C12 H12 120.5 . . ? C11 C12 H12 120.5 . . ? C14 C13 C12 119.3(3) . . ? C14 C13 H13 120.3 . . ? C12 C13 H13 120.3 . . ? C24 C25 C26 119.7(3) . . ? C24 C25 H25 120.1 . . ? C26 C25 H25 120.1 . . ? C25 C24 C23 120.7(3) . . ? C25 C24 H24 119.6 . . ? C23 C24 H24 119.6 . . ? F14 B1 F13 110.2(2) . . ? F14 B1 F12 108.9(2) . . ? F13 B1 F12 109.2(2) . . ? F14 B1 F11 109.6(2) . . ? F13 B1 F11 110.2(2) . . ? F12 B1 F11 108.7(2) . . ? F22 B2 F24 111.2(3) . . ? F22 B2 F23 108.8(3) . . ? F24 B2 F23 109.8(2) . . ? F22 B2 F21 108.8(2) . . ? F24 B2 F21 109.5(2) . . ? F23 B2 F21 108.7(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N5 Ru1 N2 C10 87.78(18) . . . . ? N4 Ru1 N2 C10 -128.2(11) . . . . ? N6 Ru1 N2 C10 -90.30(18) . . . . ? N3 Ru1 N2 C10 -2.12(18) . . . . ? N1 Ru1 N2 C10 179.68(19) . . . . ? N5 Ru1 N2 C6 -90.54(18) . . . . ? N4 Ru1 N2 C6 53.5(12) . . . . ? N6 Ru1 N2 C6 91.38(18) . . . . ? N3 Ru1 N2 C6 179.55(19) . . . . ? N1 Ru1 N2 C6 1.36(17) . . . . ? N2 Ru1 N4 C16 -142.9(11) . . . . ? N5 Ru1 N4 C16 1.1(2) . . . . ? N6 Ru1 N4 C16 178.8(2) . . . . ? N3 Ru1 N4 C16 91.7(2) . . . . ? N1 Ru1 N4 C16 -91.3(2) . . . . ? N2 Ru1 N4 C19 32.1(13) . . . . ? N5 Ru1 N4 C19 176.01(17) . . . . ? N6 Ru1 N4 C19 -6.26(17) . . . . ? N3 Ru1 N4 C19 -93.32(18) . . . . ? N1 Ru1 N4 C19 83.67(18) . . . . ? N2 Ru1 N6 C20 -171.11(18) . . . . ? N5 Ru1 N6 C20 22.5(6) . . . . ? N4 Ru1 N6 C20 6.41(18) . . . . ? N3 Ru1 N6 C20 109.83(18) . . . . ? N1 Ru1 N6 C20 -91.69(18) . . . . ? N2 Ru1 N6 C21 10.9(2) . . . . ? N5 Ru1 N6 C21 -155.5(5) . . . . ? N4 Ru1 N6 C21 -171.6(2) . . . . ? N3 Ru1 N6 C21 -68.2(2) . . . . ? N1 Ru1 N6 C21 90.3(2) . . . . ? N2 Ru1 N5 C28 -117(2) . . . . ? N4 Ru1 N5 C28 65(2) . . . . ? N6 Ru1 N5 C28 49(3) . . . . ? N3 Ru1 N5 C28 -38(2) . . . . ? N1 Ru1 N5 C28 163(2) . . . . ? N2 Ru1 N1 C1 177.9(2) . . . . ? N5 Ru1 N1 C1 -93.0(2) . . . . ? N4 Ru1 N1 C1 1.1(2) . . . . ? N6 Ru1 N1 C1 79.6(2) . . . . ? N3 Ru1 N1 C1 173.1(2) . . . . ? N2 Ru1 N1 C5 0.56(16) . . . . ? N5 Ru1 N1 C5 89.66(17) . . . . ? N4 Ru1 N1 C5 -176.29(16) . . . . ? N6 Ru1 N1 C5 -97.81(17) . . . . ? N3 Ru1 N1 C5 -4.3(3) . . . . ? N2 Ru1 N3 C15 -177.5(2) . . . . ? N5 Ru1 N3 C15 93.0(2) . . . . ? N4 Ru1 N3 C15 -0.8(2) . . . . ? N6 Ru1 N3 C15 -78.8(2) . . . . ? N1 Ru1 N3 C15 -172.7(2) . . . . ? N2 Ru1 N3 C11 1.47(17) . . . . ? N5 Ru1 N3 C11 -88.00(18) . . . . ? N4 Ru1 N3 C11 178.20(17) . . . . ? N6 Ru1 N3 C11 100.19(18) . . . . ? N1 Ru1 N3 C11 6.3(3) . . . . ? C1 N1 C5 C4 -1.9(3) . . . . ? Ru1 N1 C5 C4 175.78(19) . . . . ? C1 N1 C5 C6 -179.9(2) . . . . ? Ru1 N1 C5 C6 -2.2(3) . . . . ? Ru1 N5 C28 C29 -80(22) . . . . ? C16 N4 C19 C18 2.1(4) . . . . ? Ru1 N4 C19 C18 -173.5(2) . . . . ? C16 N4 C19 C20 -178.9(2) . . . . ? Ru1 N4 C19 C20 5.5(3) . . . . ? C27 N8 C23 C24 -2.8(4) . . . . ? C27 N8 C23 C22 176.6(2) . . . . ? N1 C5 C4 C3 0.2(4) . . . . ? C6 C5 C4 C3 178.0(2) . . . . ? C20 N6 C21 C22 106.3(3) . . . . ? Ru1 N6 C21 C22 -75.7(3) . . . . ? C21 N6 C20 O1 -8.9(4) . . . . ? Ru1 N6 C20 O1 172.9(2) . . . . ? C21 N6 C20 C19 172.9(2) . . . . ? Ru1 N6 C20 C19 -5.3(3) . . . . ? N4 C19 C20 O1 -178.5(2) . . . . ? C18 C19 C20 O1 0.5(4) . . . . ? N4 C19 C20 N6 -0.1(3) . . . . ? C18 C19 C20 N6 178.8(2) . . . . ? C5 N1 C1 C2 1.7(4) . . . . ? Ru1 N1 C1 C2 -175.6(2) . . . . ? C3 C2 C1 N1 0.2(4) . . . . ? C10 N2 C6 C7 0.9(4) . . . . ? Ru1 N2 C6 C7 179.19(18) . . . . ? C10 N2 C6 C5 178.9(2) . . . . ? Ru1 N2 C6 C5 -2.9(3) . . . . ? N1 C5 C6 N2 3.3(3) . . . . ? C4 C5 C6 N2 -174.7(2) . . . . ? N1 C5 C6 C7 -179.0(2) . . . . ? C4 C5 C6 C7 3.1(4) . . . . ? C17 N7 C18 C19 0.0(4) . . . . ? N4 C19 C18 N7 -1.6(4) . . . . ? C20 C19 C18 N7 179.4(3) . . . . ? C5 C4 C3 C2 1.7(4) . . . . ? C1 C2 C3 C4 -1.9(4) . . . . ? C11 N3 C15 C14 0.7(4) . . . . ? Ru1 N3 C15 C14 179.7(2) . . . . ? C13 C14 C15 N3 -0.1(4) . . . . ? C6 N2 C10 C9 -0.3(4) . . . . ? Ru1 N2 C10 C9 -178.57(18) . . . . ? C6 N2 C10 C11 -179.4(2) . . . . ? Ru1 N2 C10 C11 2.3(3) . . . . ? C15 N3 C11 C12 -0.8(4) . . . . ? Ru1 N3 C11 C12 -179.9(2) . . . . ? C15 N3 C11 C10 178.3(2) . . . . ? Ru1 N3 C11 C10 -0.7(3) . . . . ? N2 C10 C11 N3 -0.9(3) . . . . ? C9 C10 C11 N3 -180.0(2) . . . . ? N2 C10 C11 C12 178.2(2) . . . . ? C9 C10 C11 C12 -0.8(4) . . . . ? C19 N4 C16 C17 -1.1(4) . . . . ? Ru1 N4 C16 C17 173.8(2) . . . . ? N8 C23 C22 C21 -13.8(4) . . . . ? C24 C23 C22 C21 165.6(2) . . . . ? N6 C21 C22 C23 -54.7(3) . . . . ? C23 N8 C27 C26 2.2(4) . . . . ? C18 N7 C17 C16 1.1(5) . . . . ? N4 C16 C17 N7 -0.5(5) . . . . ? C9 C8 C7 C6 1.1(4) . . . . ? N2 C6 C7 C8 -1.3(4) . . . . ? C5 C6 C7 C8 -178.9(2) . . . . ? C7 C8 C9 C10 -0.5(4) . . . . ? N2 C10 C9 C8 0.1(4) . . . . ? C11 C10 C9 C8 179.1(3) . . . . ? N8 C27 C26 C25 -0.4(4) . . . . ? N3 C11 C12 C13 0.3(4) . . . . ? C10 C11 C12 C13 -178.8(3) . . . . ? C15 C14 C13 C12 -0.5(5) . . . . ? C11 C12 C13 C14 0.4(5) . . . . ? C27 C26 C25 C24 -0.7(4) . . . . ? C26 C25 C24 C23 0.0(4) . . . . ? N8 C23 C24 C25 1.7(4) . . . . ? C22 C23 C24 C25 -177.8(2) . . . . ? 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 N8 H8X O1 0.87(3) 1.78(3) 2.631(3) 164(3) . _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 26.46 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.139 _refine_diff_density_min -0.793 _refine_diff_density_rms 0.078 # Attachment '- hw117.cif' data_hw117 _database_code_depnum_ccdc_archive 'CCDC 777615' #TrackingRef '- hw117.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C66 H66 Ag2 B4 F16 N18 O3 Ru2' _chemical_formula_weight 1924.49 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Ag Ag -0.8971 1.1015 '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/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z' _cell_length_a 18.8896(13) _cell_length_b 15.1926(13) _cell_length_c 16.4503(11) _cell_angle_alpha 90.00 _cell_angle_beta 114.623(4) _cell_angle_gamma 90.00 _cell_volume 4291.7(6) _cell_formula_units_Z 2 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 4951 _cell_measurement_theta_min 2.682 _cell_measurement_theta_max 25.286 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.489 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1916 _exptl_absorpt_coefficient_mu 0.881 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6617 _exptl_absorpt_correction_T_max 0.7452 _exptl_absorpt_process_details 'SCALE (Bruker AXS Inc)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Kappa Apex II area detector' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18411 _diffrn_reflns_av_R_equivalents 0.0430 _diffrn_reflns_av_sigmaI/netI 0.0400 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.53 _diffrn_reflns_theta_max 25.45 _reflns_number_total 4075 _reflns_number_gt 3339 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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. [Ru(II)(terpy)(MeCN)(deprotonated terdentate amide ligand)Ag(I)(MeCN)]2(BF4)4 (Et2O). The asymmetric unit contains a quarter of the tetranuclear complex as many atoms lie on the mirror plane. C3, as it is part of the pyrazine ring, as well as C10 and C11, as they are part of the terpy ligand, were left on the mirror plane despite the higher than usual temperature factors suggested splitting, as the other atoms in these rings were OK and it does not make chemical sense to split only some of the atoms in what should be a flat moiety. Disorder is present in the coordination sphere around Ag affecting both the Ag coordinated pyridine arm of the terdentate ligand and the Ag coordinated MeCN: (a) the pyridine arm does not lie on the mirror plane so is disordered across it (N4 ring, N4' ring) and (b) both parts of the disordered MeCN molecule (N40-C40-C41:N45-C45-C46 0.25:0.25) were SAMEd to N30 (well behaved MeCN coordinated to Ru) and left isotropic. The 1,2 and 1,3 distances in the 0.25 occupancy diethyl ether molecule of solvation were SADI'ed and it was left isotropic. B1, F12 and F13 are on the mirror plane and half occupancy, whereas F11 is not and is full occupancy; symm generates complete BF4. In the case of B2 and F21-F24 all atoms are half occupancy and a part command has been employed as it is close to its symmetry equivalent. Splitting of this BF4 anion (B2) did not improve the result so somewhat higher U values remain. Part commands were applied to the pyridine ring and its alkyl linker, the Ag bound MeCN, one of the BF4 anions (B2) and the Et2O molecule (which is close to its sym equiv). ; _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^)+(0.0958P)^2^+26.1853P] 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 4075 _refine_ls_number_parameters 352 _refine_ls_number_restraints 19 _refine_ls_R_factor_all 0.0754 _refine_ls_R_factor_gt 0.0615 _refine_ls_wR_factor_ref 0.1830 _refine_ls_wR_factor_gt 0.1691 _refine_ls_goodness_of_fit_ref 1.061 _refine_ls_restrained_S_all 1.061 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.67643(3) 0.5000 0.85284(4) 0.0354(2) Uani 1 2 d S . . Ag1 Ag 0.70054(4) 0.5000 0.49686(4) 0.0739(4) Uani 1 2 d SD . . N1 N 0.5633(3) 0.5000 0.7604(4) 0.0333(14) Uani 1 2 d S . . N2 N 0.4149(4) 0.5000 0.6194(4) 0.051(2) Uani 1 2 d S . . C1 C 0.4989(4) 0.5000 0.7732(5) 0.047(2) Uani 1 2 d S . . H1 H 0.5027 0.5000 0.8326 0.056 Uiso 1 2 calc SR . . C2 C 0.4265(4) 0.5000 0.7032(5) 0.043(2) Uani 1 2 d S . . H2 H 0.3822 0.5000 0.7167 0.052 Uiso 1 2 calc SR . . C3 C 0.4801(6) 0.5000 0.6063(7) 0.111(6) Uani 1 2 d S A . H3 H 0.4757 0.5000 0.5466 0.133 Uiso 1 2 calc SR . . C4 C 0.5533(5) 0.5000 0.6753(6) 0.065(3) Uani 1 2 d S . . C5 C 0.6270(6) 0.5262(7) 0.6612(7) 0.038(3) Uani 0.50 1 d P A -1 O1 O 0.6209(4) 0.5410(6) 0.5835(5) 0.058(3) Uani 0.50 1 d P A -1 N3 N 0.6899(4) 0.5000 0.7354(4) 0.059(2) Uani 1 2 d S . . C6 C 0.7640(5) 0.5000 0.7264(6) 0.069(4) Uani 1 2 d S . . H6A H 0.8063 0.4861 0.7854 0.083 Uiso 0.50 1 calc PR B -1 H6B H 0.7625 0.4521 0.6849 0.083 Uiso 0.50 1 calc PR B -1 C7 C 0.7815(7) 0.5728(9) 0.6977(8) 0.045(3) Uani 0.50 1 d P . -1 H7A H 0.7984 0.6163 0.7470 0.054 Uiso 0.50 1 calc PR . -1 H7B H 0.7337 0.5961 0.6489 0.054 Uiso 0.50 1 calc PR . -1 N4 N 0.8212(4) 0.5365(8) 0.5796(5) 0.061(4) Uani 0.50 1 d PG . -1 C8 C 0.8426(4) 0.5666(7) 0.6643(5) 0.048(3) Uani 0.50 1 d PG . -1 C9 C 0.9226(4) 0.5850(8) 0.7184(5) 0.065(4) Uani 0.50 1 d PG . -1 H9 H 0.9384 0.6060 0.7778 0.078 Uiso 0.50 1 calc PR . -1 C10 C 0.9752(4) 0.5724(14) 0.6851(8) 0.105(8) Uani 0.50 1 d PG . -1 H10 H 1.0286 0.5839 0.7214 0.126 Uiso 0.50 1 calc PR . -1 C11 C 0.9530(8) 0.5428(15) 0.5982(11) 0.111(11) Uani 0.50 1 d P . -1 H11 H 0.9903 0.5349 0.5740 0.133 Uiso 0.50 1 calc PR . -1 C12 C 0.8755(7) 0.5251(14) 0.5480(9) 0.070(9) Uani 0.50 1 d P . -1 H12 H 0.8598 0.5041 0.4887 0.084 Uiso 0.50 1 calc PR . -1 N5 N 0.6979(3) 0.6327(4) 0.8654(4) 0.0556(14) Uani 1 1 d . . . N6 N 0.7870(4) 0.5000 0.9345(4) 0.052(2) Uani 1 2 d S . . C13 C 0.6501(5) 0.6983(5) 0.8226(5) 0.076(2) Uani 1 1 d . A . H13 H 0.5976 0.6844 0.7848 0.091 Uiso 1 1 calc R . . C14 C 0.6731(7) 0.7861(6) 0.8304(7) 0.109(4) Uani 1 1 d . . . H14 H 0.6371 0.8302 0.7969 0.131 Uiso 1 1 calc R A . C15 C 0.7457(8) 0.8083(9) 0.8849(8) 0.126(5) Uani 1 1 d . A . H15 H 0.7614 0.8682 0.8920 0.151 Uiso 1 1 calc R . . C16 C 0.7976(7) 0.7430(8) 0.9309(7) 0.110(4) Uani 1 1 d . . . H16 H 0.8497 0.7579 0.9698 0.132 Uiso 1 1 calc R A . C17 C 0.7737(4) 0.6549(6) 0.9205(5) 0.071(2) Uani 1 1 d . A . C18 C 0.8239(4) 0.5780(6) 0.9623(4) 0.069(2) Uani 1 1 d . A . C19 C 0.9004(4) 0.5783(8) 1.0222(5) 0.092(3) Uani 1 1 d . . . H19 H 0.9268 0.6326 1.0429 0.111 Uiso 1 1 calc R A . C20 C 0.9389(6) 0.5000 1.0522(8) 0.109(6) Uani 1 2 d S . . H20 H 0.9921 0.5000 1.0937 0.131 Uiso 1 2 calc SR . . N30 N 0.6489(4) 0.5000 0.9604(4) 0.0450(17) Uani 1 2 d SD . . C30 C 0.6314(4) 0.5000 1.0181(5) 0.058(3) Uani 1 2 d SD A . C31 C 0.6071(7) 0.5000 1.0893(7) 0.141(9) Uani 1 2 d SD . . H31A H 0.5933 0.5600 1.0990 0.212 Uiso 0.50 1 calc PR A . H31B H 0.6497 0.4784 1.1440 0.212 Uiso 0.50 1 calc PR . . H31C H 0.5617 0.4615 1.0738 0.212 Uiso 0.50 1 calc PR . . N40 N 0.7220(17) 0.3472(15) 0.438(2) 0.080(4) Uiso 0.25 1 d PD A 1 C40 C 0.7312(18) 0.313(2) 0.3814(19) 0.080(4) Uiso 0.25 1 d PD A 1 C41 C 0.772(2) 0.263(2) 0.341(2) 0.080(4) Uiso 0.25 1 d PD A 1 H41A H 0.8000 0.2140 0.3800 0.120 Uiso 0.25 1 calc PR A 1 H41B H 0.8099 0.3009 0.3307 0.120 Uiso 0.25 1 calc PR A 1 H41C H 0.7352 0.2393 0.2831 0.120 Uiso 0.25 1 calc PR A 1 N45 N 0.7500(17) 0.3502(15) 0.463(2) 0.080(4) Uiso 0.25 1 d PD A 2 C45 C 0.7646(17) 0.303(2) 0.418(2) 0.080(4) Uiso 0.25 1 d PD A 2 C46 C 0.814(2) 0.253(2) 0.389(3) 0.080(4) Uiso 0.25 1 d PD A 2 H46A H 0.8564 0.2259 0.4405 0.120 Uiso 0.25 1 calc PR A 2 H46B H 0.8366 0.2921 0.3582 0.120 Uiso 0.25 1 calc PR A 2 H46C H 0.7837 0.2068 0.3475 0.120 Uiso 0.25 1 calc PR A 2 B1 B 0.8183(7) 0.5000 0.2896(8) 0.083(5) Uani 1 2 d S . . F11 F 0.8638(3) 0.5715(4) 0.3356(4) 0.1083(19) Uani 1 1 d . . . F12 F 0.7518(4) 0.5000 0.2977(5) 0.118(3) Uani 1 2 d S . . F13 F 0.8078(4) 0.5000 0.2017(4) 0.0812(19) Uani 1 2 d S . . B2 B 0.9742(12) 0.7933(15) 0.9029(16) 0.086(7) Uani 0.50 1 d P C -1 F21 F 0.9135(5) 0.8357(6) 0.8360(7) 0.078(3) Uani 0.50 1 d P C -1 F22 F 0.9686(5) 0.8239(10) 0.9849(8) 0.112(4) Uani 0.50 1 d P C -1 F23 F 0.9632(8) 0.7078(6) 0.9025(8) 0.106(4) Uani 0.50 1 d P C -1 F24 F 1.0439(6) 0.8210(10) 0.9133(8) 0.126(5) Uani 0.50 1 d P C -1 C50 C 0.925(3) 0.732(3) 0.794(3) 0.123(16) Uiso 0.25 1 d PD D -2 H50A H 0.9705 0.7666 0.8321 0.184 Uiso 0.25 1 calc PR D -2 H50B H 0.9167 0.6843 0.8294 0.184 Uiso 0.25 1 calc PR D -2 H50C H 0.8788 0.7704 0.7715 0.184 Uiso 0.25 1 calc PR D -2 C51 C 0.937(3) 0.696(3) 0.721(3) 0.121(15) Uiso 0.25 1 d PD D -2 H51A H 0.9760 0.6489 0.7443 0.145 Uiso 0.25 1 calc PR D -2 H51B H 0.8874 0.6688 0.6795 0.145 Uiso 0.25 1 calc PR D -2 O52 O 0.9612(18) 0.7555(17) 0.6721(17) 0.100(8) Uiso 0.25 1 d PD D -2 C53 C 0.969(4) 0.723(3) 0.596(3) 0.15(2) Uiso 0.25 1 d PD D -2 H53A H 0.9223 0.6870 0.5613 0.176 Uiso 0.25 1 calc PR D -2 H53B H 1.0144 0.6833 0.6162 0.176 Uiso 0.25 1 calc PR D -2 C54 C 0.978(5) 0.785(4) 0.537(5) 0.21(3) Uiso 0.25 1 d PD D -2 H54A H 0.9730 0.7554 0.4820 0.310 Uiso 0.25 1 calc PR D -2 H54B H 1.0290 0.8130 0.5655 0.310 Uiso 0.25 1 calc PR D -2 H54C H 0.9370 0.8302 0.5220 0.310 Uiso 0.25 1 calc PR D -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 0.0190(3) 0.0710(5) 0.0183(3) 0.000 0.0098(2) 0.000 Ag1 0.0194(4) 0.1781(10) 0.0239(4) 0.000 0.0086(3) 0.000 N1 0.021(3) 0.056(4) 0.027(3) 0.000 0.015(3) 0.000 N2 0.017(3) 0.113(6) 0.023(3) 0.000 0.007(3) 0.000 C1 0.025(4) 0.100(7) 0.022(4) 0.000 0.016(3) 0.000 C2 0.023(4) 0.087(6) 0.023(4) 0.000 0.012(3) 0.000 C3 0.031(5) 0.29(2) 0.022(5) 0.000 0.017(4) 0.000 C4 0.019(4) 0.155(10) 0.024(4) 0.000 0.012(3) 0.000 C5 0.024(5) 0.073(11) 0.018(4) 0.006(4) 0.010(4) 0.005(4) O1 0.023(4) 0.134(9) 0.023(4) 0.005(4) 0.015(3) 0.006(4) N3 0.019(3) 0.141(7) 0.020(3) 0.000 0.011(3) 0.000 C6 0.021(4) 0.172(12) 0.016(4) 0.000 0.010(3) 0.000 C7 0.040(6) 0.072(8) 0.031(6) 0.002(6) 0.023(5) -0.002(6) N4 0.028(5) 0.138(13) 0.019(4) -0.002(5) 0.011(4) -0.007(5) C8 0.034(6) 0.081(8) 0.030(6) 0.005(6) 0.016(5) -0.012(6) C9 0.029(6) 0.124(13) 0.038(7) -0.011(8) 0.009(5) -0.021(7) C10 0.032(7) 0.24(2) 0.049(9) -0.023(12) 0.018(7) -0.051(11) C11 0.033(7) 0.26(4) 0.053(9) -0.006(11) 0.032(7) -0.017(10) C12 0.027(5) 0.15(3) 0.043(6) -0.011(8) 0.018(5) -0.009(8) N5 0.040(3) 0.083(4) 0.034(3) -0.007(3) 0.005(2) -0.019(3) N6 0.022(3) 0.117(7) 0.019(3) 0.000 0.010(3) 0.000 C13 0.076(5) 0.073(5) 0.052(4) -0.004(4) 0.000(4) -0.016(4) C14 0.126(9) 0.071(5) 0.091(7) -0.010(5) 0.006(7) -0.037(6) C15 0.134(11) 0.104(8) 0.092(8) -0.016(7) -0.002(8) -0.059(8) C16 0.090(7) 0.149(10) 0.078(7) -0.049(7) 0.021(6) -0.089(8) C17 0.048(4) 0.119(7) 0.038(4) -0.016(4) 0.010(3) -0.030(4) C18 0.033(3) 0.149(8) 0.029(3) -0.014(4) 0.016(3) -0.025(4) C19 0.027(4) 0.203(11) 0.039(4) -0.012(5) 0.006(3) -0.029(5) C20 0.020(5) 0.27(2) 0.031(6) 0.000 0.004(5) 0.000 N30 0.019(3) 0.089(5) 0.026(3) 0.000 0.009(3) 0.000 C30 0.018(4) 0.136(9) 0.019(4) 0.000 0.008(3) 0.000 C31 0.038(6) 0.36(3) 0.032(6) 0.000 0.024(5) 0.000 B1 0.041(7) 0.169(15) 0.035(6) 0.000 0.012(5) 0.000 F11 0.065(3) 0.178(6) 0.072(3) -0.023(4) 0.019(3) -0.028(4) F12 0.036(3) 0.241(11) 0.074(5) 0.000 0.019(3) 0.000 F13 0.078(4) 0.126(5) 0.042(3) 0.000 0.027(3) 0.000 B2 0.062(12) 0.099(15) 0.094(16) 0.040(12) 0.029(11) 0.047(11) F21 0.051(5) 0.078(5) 0.098(7) 0.038(5) 0.024(5) 0.022(4) F22 0.057(5) 0.211(12) 0.075(7) -0.033(8) 0.034(6) -0.037(6) F23 0.158(11) 0.076(6) 0.128(10) 0.043(6) 0.104(9) 0.069(7) F24 0.064(6) 0.223(14) 0.112(9) 0.091(9) 0.059(6) 0.056(8) _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 N6 1.957(7) . y Ru1 N1 2.042(6) . y Ru1 N30 2.042(6) . y Ru1 N5 2.049(6) . y Ru1 N5 2.049(6) 6_565 ? Ru1 N3 2.051(6) . y Ag1 N4 2.184(6) 6_565 ? Ag1 N4 2.184(7) . y Ag1 N2 2.222(7) 5_666 y Ag1 O1 2.543(7) 6_565 ? Ag1 O1 2.543(7) . y Ag1 N45 2.605(17) . y Ag1 N45 2.605(17) 6_565 ? Ag1 N40 2.611(17) . y Ag1 N40 2.611(17) 6_565 ? N1 C1 1.318(9) . ? N1 C4 1.333(10) . ? N2 C2 1.303(10) . ? N2 C3 1.335(11) . ? N2 Ag1 2.222(7) 5_666 ? C1 C2 1.373(11) . ? C1 H1 0.9500 . ? C2 H2 0.9500 . ? C3 C4 1.376(13) . ? C3 H3 0.9500 . ? C4 C5 1.554(12) . ? C4 C5 1.554(12) 6_565 ? C5 O1 1.256(12) . ? C5 N3 1.361(12) . ? N3 C5 1.361(12) 6_565 ? N3 C6 1.468(10) . ? C6 C7 1.299(12) . ? C6 C7 1.299(12) 6_565 ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.473(12) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? N4 C12 1.341(14) . ? N4 C8 1.3582 . ? C8 C9 1.4264 . ? C9 C10 1.3334 . ? C9 H9 0.9500 . ? C10 C11 1.387(19) . ? C10 H10 0.9500 . ? C11 C12 1.374(19) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? N5 C13 1.332(10) . ? N5 C17 1.378(9) . ? N6 C18 1.354(9) 6_565 ? N6 C18 1.354(9) . ? C13 C14 1.393(12) . ? C13 H13 0.9500 . ? C14 C15 1.331(15) . ? C14 H14 0.9500 . ? C15 C16 1.378(17) . ? C15 H15 0.9500 . ? C16 C17 1.401(13) . ? C16 H16 0.9500 . ? C17 C18 1.482(12) . ? C18 C19 1.368(10) . ? C19 C20 1.375(12) . ? C19 H19 0.9500 . ? C20 C19 1.375(12) 6_565 ? C20 H20 0.9500 . ? N30 C30 1.127(10) . ? C30 C31 1.424(12) . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? N40 C40 1.143(13) . ? C40 C41 1.438(14) . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? N45 C45 1.144(13) . ? C45 C46 1.441(14) . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? B1 F12 1.318(14) . ? B1 F13 1.375(14) . ? B1 F11 1.396(9) . ? B1 F11 1.396(9) 6_565 ? B2 F23 1.32(3) . ? B2 F24 1.32(2) . ? B2 F21 1.38(2) . ? B2 F22 1.47(3) . ? C50 C51 1.42(3) . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? C51 O52 1.41(3) . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? O52 C53 1.41(3) . ? C53 C54 1.41(3) . ? C53 H53A 0.9900 . ? C53 H53B 0.9900 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N6 Ru1 N1 176.0(2) . . y N6 Ru1 N30 89.4(3) . . y N1 Ru1 N30 94.6(2) . . y N6 Ru1 N5 79.67(16) . . y N1 Ru1 N5 100.21(15) . . y N30 Ru1 N5 91.36(15) . . y N6 Ru1 N5 79.67(15) . 6_565 ? N1 Ru1 N5 100.21(16) . 6_565 ? N30 Ru1 N5 91.36(16) . 6_565 ? N5 Ru1 N5 159.1(3) . 6_565 y N6 Ru1 N3 97.5(3) . . y N1 Ru1 N3 78.5(2) . . y N30 Ru1 N3 173.1(3) . . y N5 Ru1 N3 89.90(15) . . y N5 Ru1 N3 89.89(15) 6_565 . ? N4 Ag1 N4 29.4(6) 6_565 . ? N4 Ag1 N2 158.7(3) 6_565 5_666 ? N4 Ag1 N2 158.7(3) . 5_666 y N4 Ag1 O1 107.2(3) 6_565 6_565 ? N4 Ag1 O1 114.9(3) . 6_565 ? N2 Ag1 O1 83.4(2) 5_666 6_565 ? N4 Ag1 O1 114.9(3) 6_565 . y N4 Ag1 O1 107.2(3) . . y N2 Ag1 O1 83.4(2) 5_666 . y O1 Ag1 O1 28.4(4) 6_565 . ? N4 Ag1 N45 62.4(7) 6_565 . ? N4 Ag1 N45 88.9(7) . . y N2 Ag1 N45 97.3(7) 5_666 . y O1 Ag1 N45 104.6(7) 6_565 . y O1 Ag1 N45 132.9(8) . . y N4 Ag1 N45 88.9(7) 6_565 6_565 ? N4 Ag1 N45 62.4(7) . 6_565 ? N2 Ag1 N45 97.3(7) 5_666 6_565 ? O1 Ag1 N45 132.9(7) 6_565 6_565 ? O1 Ag1 N45 104.7(7) . 6_565 ? N45 Ag1 N45 121.8(14) . 6_565 ? N4 Ag1 N40 73.9(7) 6_565 . ? N4 Ag1 N40 100.0(7) . . y N2 Ag1 N40 86.0(7) 5_666 . y O1 Ag1 N40 102.1(7) 6_565 . y O1 Ag1 N40 130.1(7) . . y N45 Ag1 N40 11.4(9) . . ? N45 Ag1 N40 125.0(7) 6_565 . ? N4 Ag1 N40 100.0(7) 6_565 6_565 ? N4 Ag1 N40 73.9(7) . 6_565 ? N2 Ag1 N40 86.0(7) 5_666 6_565 ? O1 Ag1 N40 130.1(7) 6_565 6_565 ? O1 Ag1 N40 102.1(7) . 6_565 ? N45 Ag1 N40 125.0(7) . 6_565 ? N45 Ag1 N40 11.4(9) 6_565 6_565 ? N40 Ag1 N40 125.6(14) . 6_565 ? C1 N1 C4 115.5(7) . . ? C1 N1 Ru1 129.1(5) . . ? C4 N1 Ru1 115.4(5) . . ? C2 N2 C3 114.3(7) . . ? C2 N2 Ag1 125.6(5) . 5_666 ? C3 N2 Ag1 120.1(6) . 5_666 ? N1 C1 C2 122.1(7) . . ? N1 C1 H1 119.0 . . ? C2 C1 H1 119.0 . . ? N2 C2 C1 123.8(7) . . ? N2 C2 H2 118.1 . . ? C1 C2 H2 118.1 . . ? N2 C3 C4 123.0(8) . . ? N2 C3 H3 118.5 . . ? C4 C3 H3 118.5 . . ? N1 C4 C3 121.4(7) . . ? N1 C4 C5 114.4(7) . . ? C3 C4 C5 122.1(7) . . ? N1 C4 C5 114.4(7) . 6_565 ? C3 C4 C5 122.1(7) . 6_565 ? C5 C4 C5 29.6(8) . 6_565 ? O1 C5 N3 129.9(9) . . ? O1 C5 C4 119.3(9) . . ? N3 C5 C4 107.0(7) . . ? C5 O1 Ag1 134.6(7) . . ? C5 N3 C5 34.0(9) 6_565 . ? C5 N3 C6 115.0(7) 6_565 . ? C5 N3 C6 115.0(7) . . ? C5 N3 Ru1 116.1(5) 6_565 . ? C5 N3 Ru1 116.1(5) . . ? C6 N3 Ru1 126.4(5) . . ? C7 C6 C7 116.8(12) . 6_565 ? C7 C6 N3 115.8(6) . . ? C7 C6 N3 115.8(6) 6_565 . ? C7 C6 H6A 108.3 . . ? C7 C6 H6A 87.2 6_565 . ? N3 C6 H6A 108.3 . . ? C7 C6 H6B 108.3 . . ? C7 C6 H6B 20.2 6_565 . ? N3 C6 H6B 108.3 . . ? H6A C6 H6B 107.4 . . ? C6 C7 C8 116.0(10) . . ? C6 C7 H7A 108.3 . . ? C8 C7 H7A 108.3 . . ? C6 C7 H7B 108.3 . . ? C8 C7 H7B 108.3 . . ? H7A C7 H7B 107.4 . . ? C12 N4 C8 119.4(7) . . ? C12 N4 Ag1 119.6(7) . . ? C8 N4 Ag1 120.8(4) . . ? N4 C8 C9 119.5 . . ? N4 C8 C7 117.3(7) . . ? C9 C8 C7 123.1(7) . . ? C10 C9 C8 119.5 . . ? C10 C9 H9 120.3 . . ? C8 C9 H9 120.3 . . ? C9 C10 C11 120.9(6) . . ? C9 C10 H10 119.5 . . ? C11 C10 H10 119.5 . . ? C12 C11 C10 118.1(11) . . ? C12 C11 H11 121.0 . . ? C10 C11 H11 121.0 . . ? N4 C12 C11 122.6(13) . . ? N4 C12 H12 118.7 . . ? C11 C12 H12 118.7 . . ? C13 N5 C17 117.0(7) . . ? C13 N5 Ru1 128.3(5) . . ? C17 N5 Ru1 114.5(6) . . ? C18 N6 C18 122.1(9) 6_565 . ? C18 N6 Ru1 119.0(4) 6_565 . ? C18 N6 Ru1 119.0(4) . . ? N5 C13 C14 123.5(8) . . ? N5 C13 H13 118.3 . . ? C14 C13 H13 118.3 . . ? C15 C14 C13 119.9(11) . . ? C15 C14 H14 120.0 . . ? C13 C14 H14 120.0 . . ? C14 C15 C16 119.1(10) . . ? C14 C15 H15 120.5 . . ? C16 C15 H15 120.5 . . ? C15 C16 C17 120.0(9) . . ? C15 C16 H16 120.0 . . ? C17 C16 H16 120.0 . . ? N5 C17 C16 120.5(9) . . ? N5 C17 C18 113.6(7) . . ? C16 C17 C18 125.8(8) . . ? N6 C18 C19 119.2(9) . . ? N6 C18 C17 113.1(6) . . ? C19 C18 C17 127.7(9) . . ? C18 C19 C20 119.8(10) . . ? C18 C19 H19 120.1 . . ? C20 C19 H19 120.1 . . ? C19 C20 C19 119.9(10) 6_565 . ? C19 C20 H20 120.0 6_565 . ? C19 C20 H20 120.0 . . ? C30 N30 Ru1 177.9(6) . . ? N30 C30 C31 178.5(10) . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C40 N40 Ag1 144(3) . . ? N40 C40 C41 157(3) . . ? C45 N45 Ag1 153(3) . . ? N45 C45 C46 156(3) . . ? C45 C46 H46A 109.5 . . ? C45 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C45 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? F12 B1 F13 112.4(10) . . ? F12 B1 F11 110.0(7) . . ? F13 B1 F11 110.9(7) . . ? F12 B1 F11 110.0(7) . 6_565 ? F13 B1 F11 110.9(7) . 6_565 ? F11 B1 F11 102.2(10) . 6_565 ? F23 B2 F24 117.5(15) . . ? F23 B2 F21 112(2) . . ? F24 B2 F21 114.0(17) . . ? F23 B2 F22 104.2(16) . . ? F24 B2 F22 103.3(19) . . ? F21 B2 F22 103.3(14) . . ? C51 C50 H50A 109.5 . . ? C51 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C51 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? O52 C51 C50 116(4) . . ? O52 C51 H51A 108.2 . . ? C50 C51 H51A 108.2 . . ? O52 C51 H51B 108.2 . . ? C50 C51 H51B 108.2 . . ? H51A C51 H51B 107.3 . . ? C53 O52 C51 118(4) . . ? O52 C53 C54 118(4) . . ? O52 C53 H53A 107.9 . . ? C54 C53 H53A 107.9 . . ? O52 C53 H53B 107.9 . . ? C54 C53 H53B 107.9 . . ? H53A C53 H53B 107.2 . . ? C53 C54 H54A 109.5 . . ? C53 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C53 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 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 N6 Ru1 N1 C1 180.000(10) . . . . ? N30 Ru1 N1 C1 0.000(3) . . . . ? N5 Ru1 N1 C1 -92.21(16) . . . . ? N5 Ru1 N1 C1 92.21(16) 6_565 . . . ? N3 Ru1 N1 C1 180.000(2) . . . . ? N6 Ru1 N1 C4 0.000(10) . . . . ? N30 Ru1 N1 C4 180.000(2) . . . . ? N5 Ru1 N1 C4 87.79(16) . . . . ? N5 Ru1 N1 C4 -87.79(16) 6_565 . . . ? N3 Ru1 N1 C4 0.000(2) . . . . ? C4 N1 C1 C2 0.000(4) . . . . ? Ru1 N1 C1 C2 180.000(3) . . . . ? C3 N2 C2 C1 0.000(3) . . . . ? Ag1 N2 C2 C1 180.000(2) 5_666 . . . ? N1 C1 C2 N2 0.000(4) . . . . ? C2 N2 C3 C4 0.000(4) . . . . ? Ag1 N2 C3 C4 180.000(3) 5_666 . . . ? C1 N1 C4 C3 0.000(4) . . . . ? Ru1 N1 C4 C3 180.000(3) . . . . ? C1 N1 C4 C5 163.7(4) . . . . ? Ru1 N1 C4 C5 -16.3(4) . . . . ? C1 N1 C4 C5 -163.7(4) . . . 6_565 ? Ru1 N1 C4 C5 16.3(4) . . . 6_565 ? N2 C3 C4 N1 0.000(4) . . . . ? N2 C3 C4 C5 -162.4(5) . . . . ? N2 C3 C4 C5 162.4(5) . . . 6_565 ? N1 C4 C5 O1 -169.4(8) . . . . ? C3 C4 C5 O1 -5.9(11) . . . . ? C5 C4 C5 O1 93.7(9) 6_565 . . . ? N1 C4 C5 N3 30.3(8) . . . . ? C3 C4 C5 N3 -166.2(4) . . . . ? C5 C4 C5 N3 -66.6(6) 6_565 . . . ? N3 C5 O1 Ag1 18.4(18) . . . . ? C4 C5 O1 Ag1 -136.7(7) . . . . ? N4 Ag1 O1 C5 -20.7(12) 6_565 . . . ? N4 Ag1 O1 C5 -51.2(11) . . . . ? N2 Ag1 O1 C5 147.7(11) 5_666 . . . ? O1 Ag1 O1 C5 59.4(11) 6_565 . . . ? N45 Ag1 O1 C5 53.9(14) . . . . ? N45 Ag1 O1 C5 -116.4(13) 6_565 . . . ? N40 Ag1 O1 C5 68.7(14) . . . . ? N40 Ag1 O1 C5 -127.9(12) 6_565 . . . ? O1 C5 N3 C5 -89.4(12) . . . 6_565 ? C4 C5 N3 C5 68.1(6) . . . 6_565 ? O1 C5 N3 C6 8.8(14) . . . . ? C4 C5 N3 C6 166.3(4) . . . . ? O1 C5 N3 Ru1 172.0(10) . . . . ? C4 C5 N3 Ru1 -30.5(8) . . . . ? N6 Ru1 N3 C5 161.0(5) . . . 6_565 ? N1 Ru1 N3 C5 -19.0(5) . . . 6_565 ? N30 Ru1 N3 C5 -19.0(5) . . . 6_565 ? N5 Ru1 N3 C5 -119.4(5) . . . 6_565 ? N5 Ru1 N3 C5 81.5(5) 6_565 . . 6_565 ? N6 Ru1 N3 C5 -161.0(5) . . . . ? N1 Ru1 N3 C5 19.0(5) . . . . ? N30 Ru1 N3 C5 19.0(5) . . . . ? N5 Ru1 N3 C5 -81.5(5) . . . . ? N5 Ru1 N3 C5 119.4(5) 6_565 . . . ? N6 Ru1 N3 C6 0.000(3) . . . . ? N1 Ru1 N3 C6 180.000(3) . . . . ? N30 Ru1 N3 C6 180.000(9) . . . . ? N5 Ru1 N3 C6 79.56(16) . . . . ? N5 Ru1 N3 C6 -79.56(16) 6_565 . . . ? C5 N3 C6 C7 89.9(9) 6_565 . . . ? C5 N3 C6 C7 52.3(10) . . . . ? Ru1 N3 C6 C7 -108.9(8) . . . . ? C5 N3 C6 C7 -52.3(10) 6_565 . . 6_565 ? C5 N3 C6 C7 -89.9(9) . . . 6_565 ? Ru1 N3 C6 C7 108.9(8) . . . 6_565 ? C7 C6 C7 C8 -21.5(19) 6_565 . . . ? N3 C6 C7 C8 -163.3(8) . . . . ? N4 Ag1 N4 C12 72.4(13) 6_565 . . . ? N2 Ag1 N4 C12 -59.9(17) 5_666 . . . ? O1 Ag1 N4 C12 153.3(12) 6_565 . . . ? O1 Ag1 N4 C12 -177.3(12) . . . . ? N45 Ag1 N4 C12 47.7(15) . . . . ? N45 Ag1 N4 C12 -79.5(15) 6_565 . . . ? N40 Ag1 N4 C12 44.9(15) . . . . ? N40 Ag1 N4 C12 -79.4(14) 6_565 . . . ? N4 Ag1 N4 C8 -104.4(9) 6_565 . . . ? N2 Ag1 N4 C8 123.3(8) 5_666 . . . ? O1 Ag1 N4 C8 -23.5(10) 6_565 . . . ? O1 Ag1 N4 C8 5.9(10) . . . . ? N45 Ag1 N4 C8 -129.1(11) . . . . ? N45 Ag1 N4 C8 103.7(12) 6_565 . . . ? N40 Ag1 N4 C8 -131.9(11) . . . . ? N40 Ag1 N4 C8 103.8(12) 6_565 . . . ? C12 N4 C8 C9 -0.5(16) . . . . ? Ag1 N4 C8 C9 176.3(7) . . . . ? C12 N4 C8 C7 -176.4(14) . . . . ? Ag1 N4 C8 C7 0.4(14) . . . . ? C6 C7 C8 N4 80.8(13) . . . . ? C6 C7 C8 C9 -94.9(12) . . . . ? N4 C8 C9 C10 0.0 . . . . ? C7 C8 C9 C10 175.7(15) . . . . ? C8 C9 C10 C11 0.8(18) . . . . ? C9 C10 C11 C12 -1(3) . . . . ? C8 N4 C12 C11 0(3) . . . . ? Ag1 N4 C12 C11 -176.8(16) . . . . ? C10 C11 C12 N4 1(3) . . . . ? N6 Ru1 N5 C13 174.8(7) . . . . ? N1 Ru1 N5 C13 -1.1(7) . . . . ? N30 Ru1 N5 C13 -96.0(7) . . . . ? N5 Ru1 N5 C13 166.6(7) 6_565 . . . ? N3 Ru1 N5 C13 77.2(7) . . . . ? N6 Ru1 N5 C17 0.3(5) . . . . ? N1 Ru1 N5 C17 -175.7(5) . . . . ? N30 Ru1 N5 C17 89.4(5) . . . . ? N5 Ru1 N5 C17 -8.0(12) 6_565 . . . ? N3 Ru1 N5 C17 -97.4(5) . . . . ? N1 Ru1 N6 C18 -90.4(5) . . . 6_565 ? N30 Ru1 N6 C18 89.6(5) . . . 6_565 ? N5 Ru1 N6 C18 -178.9(6) . . . 6_565 ? N5 Ru1 N6 C18 -1.9(5) 6_565 . . 6_565 ? N3 Ru1 N6 C18 -90.4(5) . . . 6_565 ? N1 Ru1 N6 C18 90.4(5) . . . . ? N30 Ru1 N6 C18 -89.6(5) . . . . ? N5 Ru1 N6 C18 1.9(5) . . . . ? N5 Ru1 N6 C18 178.9(6) 6_565 . . . ? N3 Ru1 N6 C18 90.4(5) . . . . ? C17 N5 C13 C14 0.5(13) . . . . ? Ru1 N5 C13 C14 -174.0(8) . . . . ? N5 C13 C14 C15 -2.0(18) . . . . ? C13 C14 C15 C16 2(2) . . . . ? C14 C15 C16 C17 0(2) . . . . ? C13 N5 C17 C16 1.0(11) . . . . ? Ru1 N5 C17 C16 176.2(7) . . . . ? C13 N5 C17 C18 -177.3(7) . . . . ? Ru1 N5 C17 C18 -2.1(8) . . . . ? C15 C16 C17 N5 -1.1(15) . . . . ? C15 C16 C17 C18 177.0(10) . . . . ? C18 N6 C18 C19 -1.7(12) 6_565 . . . ? Ru1 N6 C18 C19 177.4(5) . . . . ? C18 N6 C18 C17 177.3(5) 6_565 . . . ? Ru1 N6 C18 C17 -3.5(8) . . . . ? N5 C17 C18 N6 3.6(9) . . . . ? C16 C17 C18 N6 -174.6(8) . . . . ? N5 C17 C18 C19 -177.5(6) . . . . ? C16 C17 C18 C19 4.3(13) . . . . ? N6 C18 C19 C20 0.9(11) . . . . ? C17 C18 C19 C20 -178.0(8) . . . . ? C18 C19 C20 C19 -0.2(16) . . . 6_565 ? N6 Ru1 N30 C30 180.00(11) . . . . ? N1 Ru1 N30 C30 0.00(11) . . . . ? N5 Ru1 N30 C30 100.35(19) . . . . ? N5 Ru1 N30 C30 -100.35(19) 6_565 . . . ? N3 Ru1 N30 C30 0.00(11) . . . . ? Ru1 N30 C30 C31 0.0(3) . . . . ? N4 Ag1 N40 C40 -105(4) 6_565 . . . ? N4 Ag1 N40 C40 -91(4) . . . . ? N2 Ag1 N40 C40 68(4) 5_666 . . . ? O1 Ag1 N40 C40 151(4) 6_565 . . . ? O1 Ag1 N40 C40 146(4) . . . . ? N45 Ag1 N40 C40 -105(8) . . . . ? N45 Ag1 N40 C40 -28(5) 6_565 . . . ? N40 Ag1 N40 C40 -14(5) 6_565 . . . ? Ag1 N40 C40 C41 115(9) . . . . ? N4 Ag1 N45 C45 -117(5) 6_565 . . . ? N4 Ag1 N45 C45 -104(5) . . . . ? N2 Ag1 N45 C45 56(5) 5_666 . . . ? O1 Ag1 N45 C45 141(5) 6_565 . . . ? O1 Ag1 N45 C45 144(5) . . . . ? N45 Ag1 N45 C45 -48(6) 6_565 . . . ? N40 Ag1 N45 C45 62(7) . . . . ? N40 Ag1 N45 C45 -34(6) 6_565 . . . ? Ag1 N45 C45 C46 108(10) . . . . ? C50 C51 O52 C53 -176(5) . . . . ? C51 O52 C53 C54 167(6) . . . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 25.45 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.940 _refine_diff_density_min -1.588 _refine_diff_density_rms 0.134