# 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 'Lau, Tai-Chu' _publ_contact_author_email bhtclau@cityu.edu.hk _publ_section_title ; Addition of [CH(CN)2]- and [TCNE] to RuVI N bearing 8-quinolinolato ligands ; _publ_author_name T.-C.Lau # Attachment '- 779197.cif' data_040810a_fai _database_code_depnum_ccdc_archive 'CCDC 779197' #TrackingRef '- 779197.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H29 Cl N6 O2 Ru' _chemical_formula_weight 618.09 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.1223(5) _cell_length_b 10.4936(6) _cell_length_c 14.8426(9) _cell_angle_alpha 79.785(5) _cell_angle_beta 86.546(5) _cell_angle_gamma 72.825(5) _cell_volume 1335.90(13) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 3949 _cell_measurement_theta_min 3.1287 _cell_measurement_theta_max 28.9901 _exptl_crystal_description rectangle _exptl_crystal_colour red _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.537 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 632 _exptl_absorpt_coefficient_mu 0.725 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.88379 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details 'CrysAlisPro, Oxford Diffraction Ltd' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Sapphire3, Gemini ultra' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.1270 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9441 _diffrn_reflns_av_R_equivalents 0.0614 _diffrn_reflns_av_sigmaI/netI 0.1142 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.14 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4543 _reflns_number_gt 3206 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlisPro, Oxford Diffraction Ltd' _computing_cell_refinement 'CrysAlisPro, Oxford Diffraction Ltd' _computing_data_reduction 'CrysAlisPro, Oxford Diffraction Ltd' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics Ortep-3 _computing_publication_material Wingx _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0265P)^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 4543 _refine_ls_number_parameters 345 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0761 _refine_ls_R_factor_gt 0.0448 _refine_ls_wR_factor_ref 0.0732 _refine_ls_wR_factor_gt 0.0687 _refine_ls_goodness_of_fit_ref 0.906 _refine_ls_restrained_S_all 0.906 _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 0.72369(4) 0.80067(4) 0.72904(3) 0.01591(11) Uani 1 1 d . . . Cl1 Cl 0.71088(12) 0.61719(10) 0.65771(8) 0.0275(3) Uani 1 1 d . . . O1 O 0.9328(3) 0.8050(3) 0.66942(17) 0.0194(7) Uani 1 1 d . . . O2 O 0.6293(3) 0.9288(3) 0.61609(18) 0.0213(7) Uani 1 1 d . . . N1 N 0.8755(3) 0.6385(3) 0.8184(2) 0.0175(8) Uani 1 1 d . . . N2 N 0.7288(3) 0.9814(3) 0.7688(2) 0.0165(8) Uani 1 1 d . . . N3 N 0.5321(3) 0.7978(3) 0.7863(2) 0.0203(9) Uani 1 1 d . . . H3N H 0.5053 0.7258 0.7759 0.024 Uiso 1 1 d R . . N4 N 0.2051(4) 0.7791(4) 0.9122(3) 0.0484(12) Uani 1 1 d . . . N5 N 0.4189(4) 1.0989(4) 0.8789(3) 0.0456(12) Uani 1 1 d . . . N6 N 0.8668(4) 0.8070(3) 0.4947(2) 0.0312(9) Uani 1 1 d . . . H6NA H 0.7626 0.8241 0.5042 0.037 Uiso 1 1 calc R . . H6NB H 0.9112 0.8023 0.5497 0.037 Uiso 1 1 calc R . . C1 C 0.4245(4) 0.8709(4) 0.8378(3) 0.0232(10) Uani 1 1 d . . . C2 C 0.4269(4) 0.9956(5) 0.8596(3) 0.0293(11) Uani 1 1 d . . . C3 C 0.3019(5) 0.8198(4) 0.8773(3) 0.0277(11) Uani 1 1 d . . . C4 C 0.8976(5) 0.9194(5) 0.4271(3) 0.0375(12) Uani 1 1 d . . . H4A H 1.0097 0.9027 0.4181 0.045 Uiso 1 1 calc R . . H4B H 0.8563 1.0057 0.4507 0.045 Uiso 1 1 calc R . . C5 C 0.8241(6) 0.9293(5) 0.3380(3) 0.0541(16) Uani 1 1 d . . . H5A H 0.8498 1.0009 0.2926 0.065 Uiso 1 1 calc R . . H5B H 0.7112 0.9550 0.3461 0.065 Uiso 1 1 calc R . . C6 C 0.8773(6) 0.7962(6) 0.3020(3) 0.0538(16) Uani 1 1 d . . . H6A H 0.8188 0.8030 0.2464 0.065 Uiso 1 1 calc R . . H6B H 0.9874 0.7771 0.2850 0.065 Uiso 1 1 calc R . . C7 C 0.8541(6) 0.6814(6) 0.3739(4) 0.0583(16) Uani 1 1 d . . . H7A H 0.7429 0.6944 0.3847 0.070 Uiso 1 1 calc R . . H7B H 0.8977 0.5946 0.3511 0.070 Uiso 1 1 calc R . . C8 C 0.9291(6) 0.6752(5) 0.4616(4) 0.0494(14) Uani 1 1 d . . . H8A H 1.0414 0.6556 0.4521 0.059 Uiso 1 1 calc R . . H8B H 0.9094 0.6016 0.5079 0.059 Uiso 1 1 calc R . . C9 C 1.0513(4) 0.7047(4) 0.7072(3) 0.0192(10) Uani 1 1 d . . . C10 C 1.1999(5) 0.6856(4) 0.6738(3) 0.0293(11) Uani 1 1 d . . . H10 H 1.2208 0.7477 0.6235 0.035 Uiso 1 1 calc R . . C11 C 1.3199(5) 0.5755(4) 0.7135(3) 0.0324(12) Uani 1 1 d . . . H11 H 1.4214 0.5655 0.6905 0.039 Uiso 1 1 calc R . . C12 C 1.2937(5) 0.4826(4) 0.7844(3) 0.0285(11) Uani 1 1 d . . . H12 H 1.3761 0.4077 0.8094 0.034 Uiso 1 1 calc R . . C13 C 1.1446(4) 0.4978(4) 0.8203(3) 0.0222(10) Uani 1 1 d . . . C14 C 1.0239(4) 0.6130(4) 0.7837(3) 0.0151(9) Uani 1 1 d . . . C15 C 1.1052(5) 0.4037(4) 0.8888(3) 0.0276(11) Uani 1 1 d . . . H15 H 1.1809 0.3229 0.9131 0.033 Uiso 1 1 calc R . . C16 C 0.9591(5) 0.4275(4) 0.9208(3) 0.0254(11) Uani 1 1 d . . . H16 H 0.9333 0.3626 0.9672 0.031 Uiso 1 1 calc R . . C17 C 0.8445(4) 0.5470(4) 0.8863(3) 0.0195(10) Uani 1 1 d . . . C18 C 0.6864(5) 0.5674(4) 0.9275(3) 0.0329(12) Uani 1 1 d . . . H18A H 0.6448 0.6614 0.9373 0.049 Uiso 1 1 calc R . . H18B H 0.6917 0.5064 0.9862 0.049 Uiso 1 1 calc R . . H18C H 0.6196 0.5479 0.8859 0.049 Uiso 1 1 calc R . . C19 C 0.6298(4) 1.0560(4) 0.6161(3) 0.0169(9) Uani 1 1 d . . . C20 C 0.5795(4) 1.1572(4) 0.5417(3) 0.0244(10) Uani 1 1 d . . . H20 H 0.5429 1.1374 0.4887 0.029 Uiso 1 1 calc R . . C21 C 0.5827(5) 1.2887(4) 0.5449(3) 0.0279(11) Uani 1 1 d . . . H21 H 0.5497 1.3572 0.4931 0.033 Uiso 1 1 calc R . . C22 C 0.6318(5) 1.3210(4) 0.6202(3) 0.0295(11) Uani 1 1 d . . . H22 H 0.6329 1.4113 0.6202 0.035 Uiso 1 1 calc R . . C23 C 0.6814(4) 1.2213(4) 0.6989(3) 0.0223(10) Uani 1 1 d . . . C24 C 0.6805(4) 1.0880(4) 0.6947(3) 0.0166(9) Uani 1 1 d . . . C25 C 0.7305(5) 1.2444(4) 0.7804(3) 0.0281(11) Uani 1 1 d . . . H25 H 0.7325 1.3326 0.7863 0.034 Uiso 1 1 calc R . . C26 C 0.7752(5) 1.1402(5) 0.8513(3) 0.0290(11) Uani 1 1 d . . . H26 H 0.8071 1.1568 0.9068 0.035 Uiso 1 1 calc R . . C27 C 0.7751(4) 1.0075(4) 0.8441(3) 0.0216(10) Uani 1 1 d . . . C28 C 0.8195(5) 0.8953(4) 0.9242(3) 0.0292(11) Uani 1 1 d . . . H28A H 0.7341 0.8567 0.9407 0.044 Uiso 1 1 calc R . . H28B H 0.8439 0.9309 0.9763 0.044 Uiso 1 1 calc R . . H28C H 0.9096 0.8249 0.9079 0.044 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 0.0173(2) 0.01486(19) 0.01548(19) -0.00140(14) 0.00222(13) -0.00566(14) Cl1 0.0349(7) 0.0212(6) 0.0303(7) -0.0075(5) 0.0005(5) -0.0123(5) O1 0.0198(16) 0.0176(16) 0.0181(16) 0.0020(13) 0.0042(13) -0.0050(13) O2 0.0270(17) 0.0164(17) 0.0213(17) -0.0016(13) -0.0060(13) -0.0073(13) N1 0.0144(19) 0.016(2) 0.021(2) 0.0000(16) 0.0025(15) -0.0051(14) N2 0.0139(18) 0.021(2) 0.016(2) -0.0072(16) 0.0012(15) -0.0060(15) N3 0.020(2) 0.021(2) 0.020(2) -0.0028(17) 0.0003(16) -0.0071(16) N4 0.039(3) 0.068(3) 0.044(3) -0.014(2) 0.018(2) -0.025(2) N5 0.036(3) 0.042(3) 0.059(3) -0.021(2) 0.025(2) -0.010(2) N6 0.039(2) 0.029(2) 0.019(2) -0.0057(17) 0.0039(17) 0.0008(18) C1 0.021(2) 0.024(3) 0.021(2) -0.002(2) 0.0007(19) -0.004(2) C2 0.016(2) 0.031(3) 0.034(3) -0.001(2) 0.008(2) -0.001(2) C3 0.023(3) 0.034(3) 0.022(3) -0.008(2) 0.005(2) -0.002(2) C4 0.052(3) 0.025(3) 0.033(3) 0.002(2) 0.002(2) -0.013(2) C5 0.074(4) 0.046(4) 0.033(3) 0.007(3) -0.011(3) -0.010(3) C6 0.051(4) 0.083(5) 0.027(3) -0.021(3) -0.006(3) -0.011(3) C7 0.061(4) 0.069(4) 0.061(4) -0.041(3) 0.023(3) -0.031(3) C8 0.075(4) 0.028(3) 0.042(3) -0.012(2) 0.019(3) -0.010(3) C9 0.023(2) 0.017(2) 0.021(2) -0.0097(19) 0.0050(19) -0.0087(19) C10 0.028(3) 0.026(3) 0.035(3) -0.009(2) 0.010(2) -0.010(2) C11 0.015(2) 0.035(3) 0.049(3) -0.019(3) 0.008(2) -0.005(2) C12 0.021(2) 0.026(3) 0.034(3) -0.009(2) -0.004(2) 0.003(2) C13 0.025(3) 0.021(2) 0.022(2) -0.010(2) -0.0016(19) -0.0047(19) C14 0.018(2) 0.015(2) 0.016(2) -0.0104(18) 0.0027(17) -0.0060(18) C15 0.034(3) 0.022(3) 0.019(2) -0.003(2) -0.008(2) 0.004(2) C16 0.038(3) 0.020(3) 0.017(2) 0.0022(19) 0.000(2) -0.011(2) C17 0.028(2) 0.020(2) 0.010(2) -0.0029(19) -0.0022(19) -0.0059(19) C18 0.032(3) 0.031(3) 0.027(3) 0.016(2) 0.000(2) -0.008(2) C19 0.015(2) 0.021(2) 0.016(2) -0.0086(19) 0.0003(18) -0.0041(18) C20 0.021(2) 0.022(3) 0.028(3) 0.001(2) -0.005(2) -0.0043(19) C21 0.032(3) 0.020(3) 0.029(3) 0.003(2) 0.004(2) -0.007(2) C22 0.035(3) 0.011(2) 0.041(3) -0.003(2) 0.006(2) -0.006(2) C23 0.021(2) 0.018(2) 0.030(3) -0.009(2) 0.008(2) -0.0088(19) C24 0.011(2) 0.019(2) 0.021(2) -0.0028(19) 0.0017(17) -0.0051(17) C25 0.035(3) 0.024(3) 0.032(3) -0.015(2) 0.001(2) -0.012(2) C26 0.028(3) 0.038(3) 0.029(3) -0.018(2) 0.003(2) -0.015(2) C27 0.019(2) 0.032(3) 0.017(2) -0.010(2) 0.0008(18) -0.009(2) C28 0.041(3) 0.033(3) 0.016(2) -0.007(2) -0.002(2) -0.012(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 N3 1.903(3) . ? Ru1 O2 2.012(3) . ? Ru1 O1 2.063(2) . ? Ru1 N2 2.098(3) . ? Ru1 N1 2.145(3) . ? Ru1 Cl1 2.3901(12) . ? O1 C9 1.335(4) . ? O2 C19 1.336(5) . ? N1 C17 1.342(5) . ? N1 C14 1.386(5) . ? N2 C27 1.318(5) . ? N2 C24 1.409(5) . ? N3 C1 1.344(5) . ? N3 H3N 0.9001 . ? N4 C3 1.149(5) . ? N5 C2 1.150(6) . ? N6 C4 1.490(5) . ? N6 C8 1.490(6) . ? N6 H6NA 0.9200 . ? N6 H6NB 0.9200 . ? C1 C2 1.409(6) . ? C1 C3 1.431(6) . ? C4 C5 1.493(6) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.517(7) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C7 1.517(7) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.489(7) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.384(5) . ? C9 C14 1.414(5) . ? C10 C11 1.404(6) . ? C10 H10 0.9500 . ? C11 C12 1.363(6) . ? C11 H11 0.9500 . ? C12 C13 1.405(5) . ? C12 H12 0.9500 . ? C13 C15 1.395(6) . ? C13 C14 1.422(5) . ? C15 C16 1.354(5) . ? C15 H15 0.9500 . ? C16 C17 1.410(5) . ? C16 H16 0.9500 . ? C17 C18 1.502(5) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C20 1.384(5) . ? C19 C24 1.408(5) . ? C20 C21 1.398(6) . ? C20 H20 0.9500 . ? C21 C22 1.361(6) . ? C21 H21 0.9500 . ? C22 C23 1.418(6) . ? C22 H22 0.9500 . ? C23 C25 1.399(6) . ? C23 C24 1.415(5) . ? C25 C26 1.360(6) . ? C25 H25 0.9500 . ? C26 C27 1.416(6) . ? C26 H26 0.9500 . ? C27 C28 1.497(5) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 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 N3 Ru1 O2 94.52(12) . . ? N3 Ru1 O1 178.75(14) . . ? O2 Ru1 O1 86.20(10) . . ? N3 Ru1 N2 95.64(13) . . ? O2 Ru1 N2 81.87(12) . . ? O1 Ru1 N2 83.44(11) . . ? N3 Ru1 N1 99.98(13) . . ? O2 Ru1 N1 162.10(11) . . ? O1 Ru1 N1 79.50(11) . . ? N2 Ru1 N1 106.86(13) . . ? N3 Ru1 Cl1 87.77(11) . . ? O2 Ru1 Cl1 88.60(9) . . ? O1 Ru1 Cl1 93.27(8) . . ? N2 Ru1 Cl1 170.09(9) . . ? N1 Ru1 Cl1 81.60(9) . . ? C9 O1 Ru1 113.9(2) . . ? C19 O2 Ru1 113.1(2) . . ? C17 N1 C14 118.1(3) . . ? C17 N1 Ru1 130.2(3) . . ? C14 N1 Ru1 109.9(2) . . ? C27 N2 C24 118.8(3) . . ? C27 N2 Ru1 132.3(3) . . ? C24 N2 Ru1 108.7(3) . . ? C1 N3 Ru1 139.1(3) . . ? C1 N3 H3N 110.3 . . ? Ru1 N3 H3N 110.5 . . ? C4 N6 C8 111.0(3) . . ? C4 N6 H6NA 109.4 . . ? C8 N6 H6NA 109.4 . . ? C4 N6 H6NB 109.4 . . ? C8 N6 H6NB 109.4 . . ? H6NA N6 H6NB 108.0 . . ? N3 C1 C2 124.0(4) . . ? N3 C1 C3 119.8(4) . . ? C2 C1 C3 116.1(4) . . ? N5 C2 C1 175.5(4) . . ? N4 C3 C1 177.4(5) . . ? N6 C4 C5 109.9(4) . . ? N6 C4 H4A 109.7 . . ? C5 C4 H4A 109.7 . . ? N6 C4 H4B 109.7 . . ? C5 C4 H4B 109.7 . . ? H4A C4 H4B 108.2 . . ? C4 C5 C6 111.4(4) . . ? C4 C5 H5A 109.3 . . ? C6 C5 H5A 109.3 . . ? C4 C5 H5B 109.3 . . ? C6 C5 H5B 109.3 . . ? H5A C5 H5B 108.0 . . ? C7 C6 C5 110.7(4) . . ? C7 C6 H6A 109.5 . . ? C5 C6 H6A 109.5 . . ? C7 C6 H6B 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 108.1 . . ? C8 C7 C6 111.3(4) . . ? C8 C7 H7A 109.4 . . ? C6 C7 H7A 109.4 . . ? C8 C7 H7B 109.4 . . ? C6 C7 H7B 109.4 . . ? H7A C7 H7B 108.0 . . ? C7 C8 N6 109.5(4) . . ? C7 C8 H8A 109.8 . . ? N6 C8 H8A 109.8 . . ? C7 C8 H8B 109.8 . . ? N6 C8 H8B 109.8 . . ? H8A C8 H8B 108.2 . . ? O1 C9 C10 122.7(4) . . ? O1 C9 C14 118.8(3) . . ? C10 C9 C14 118.5(4) . . ? C9 C10 C11 120.7(4) . . ? C9 C10 H10 119.6 . . ? C11 C10 H10 119.6 . . ? C12 C11 C10 121.3(4) . . ? C12 C11 H11 119.3 . . ? C10 C11 H11 119.3 . . ? C11 C12 C13 119.9(4) . . ? C11 C12 H12 120.0 . . ? C13 C12 H12 120.0 . . ? C15 C13 C12 124.0(4) . . ? C15 C13 C14 117.0(4) . . ? C12 C13 C14 119.0(4) . . ? N1 C14 C9 117.2(3) . . ? N1 C14 C13 122.5(3) . . ? C9 C14 C13 120.3(4) . . ? C16 C15 C13 120.1(4) . . ? C16 C15 H15 119.9 . . ? C13 C15 H15 119.9 . . ? C15 C16 C17 121.1(4) . . ? C15 C16 H16 119.4 . . ? C17 C16 H16 119.4 . . ? N1 C17 C16 121.0(4) . . ? N1 C17 C18 121.2(3) . . ? C16 C17 C18 117.8(4) . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? O2 C19 C20 121.8(4) . . ? O2 C19 C24 118.9(3) . . ? C20 C19 C24 119.3(4) . . ? C19 C20 C21 119.7(4) . . ? C19 C20 H20 120.2 . . ? C21 C20 H20 120.2 . . ? C22 C21 C20 121.7(4) . . ? C22 C21 H21 119.1 . . ? C20 C21 H21 119.1 . . ? C21 C22 C23 120.7(4) . . ? C21 C22 H22 119.7 . . ? C23 C22 H22 119.7 . . ? C25 C23 C24 117.3(4) . . ? C25 C23 C22 125.3(4) . . ? C24 C23 C22 117.4(4) . . ? C19 C24 N2 116.9(4) . . ? C19 C24 C23 121.3(4) . . ? N2 C24 C23 121.8(4) . . ? C26 C25 C23 119.8(4) . . ? C26 C25 H25 120.1 . . ? C23 C25 H25 120.1 . . ? C25 C26 C27 121.3(4) . . ? C25 C26 H26 119.3 . . ? C27 C26 H26 119.3 . . ? N2 C27 C26 120.9(4) . . ? N2 C27 C28 118.6(4) . . ? C26 C27 C28 120.4(4) . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N6 H6NB O1 0.92 1.81 2.693(4) 161.0 . N6 H6NA O2 0.92 2.25 2.878(4) 125.1 . _diffrn_measured_fraction_theta_max 0.966 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.966 _refine_diff_density_max 0.610 _refine_diff_density_min -0.724 _refine_diff_density_rms 0.095 # Attachment '- 779198.cif' data_102809a _database_code_depnum_ccdc_archive 'CCDC 779198' #TrackingRef '- 779198.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22.50 H19.75 N5 O3.88 Ru' _chemical_formula_weight 523.25 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru 0.0552 3.2960 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M I-4 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'y, -x, -z' '-y, x, -z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-y+1/2, x+1/2, -z+1/2' _cell_length_a 31.5680(2) _cell_length_b 31.5680(2) _cell_length_c 11.1516(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 11113.0(2) _cell_formula_units_Z 16 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 13987 _cell_measurement_theta_min 3.9619 _cell_measurement_theta_max 71.3302 _exptl_crystal_description rectangle _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.251 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4236 _exptl_absorpt_coefficient_mu 4.835 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.71916 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details 'CrysAlisPro, Oxford Diffraction Ltd' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'Enhance Ultra (Cu) X-ray Source' _diffrn_radiation_monochromator mirror _diffrn_measurement_device_type 'Xcalibur, Sapphire3, Gemini ultra' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.1270 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19101 _diffrn_reflns_av_R_equivalents 0.0349 _diffrn_reflns_av_sigmaI/netI 0.0412 _diffrn_reflns_limit_h_min -37 _diffrn_reflns_limit_h_max 37 _diffrn_reflns_limit_k_min -34 _diffrn_reflns_limit_k_max 37 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 3.96 _diffrn_reflns_theta_max 66.89 _reflns_number_total 8921 _reflns_number_gt 7920 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlisPro, Oxford Diffraction Ltd' _computing_cell_refinement 'CrysAlisPro, Oxford Diffraction Ltd' _computing_data_reduction 'CrysAlisPro, Oxford Diffraction Ltd' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics Ortep-3 _computing_publication_material Wingx _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. Displacement parameter restraints such as ISOR and DELU have been applied to those carbon atoms which are badly behaved on the 8-hydroxyquinoline ligand. ADPs and bond distances of the ethanol solvent molecule have been restrained to more appropriate values using distance and displacement parameter restraints. The atom O2W on special position was assigned to be a water molecule with 0.25 sof. No hydrogen bonding was found surrounding O2W and this makes difficult to determine the direction of hydrogen atoms pointing. For this reason, no hydrogens were added. The partial occupancy of O2W inside the crystal lattice is probably due to lack of H-bonding surrounding. ; _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^)+(0.0708P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.017(9) _refine_ls_number_reflns 8921 _refine_ls_number_parameters 600 _refine_ls_number_restraints 52 _refine_ls_R_factor_all 0.0421 _refine_ls_R_factor_gt 0.0350 _refine_ls_wR_factor_ref 0.1070 _refine_ls_wR_factor_gt 0.1043 _refine_ls_goodness_of_fit_ref 1.086 _refine_ls_restrained_S_all 1.098 _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 0.195300(12) 0.219229(12) 0.46370(4) 0.03294(11) Uani 1 1 d . . . Ru2 Ru 0.923128(11) 0.160963(12) 0.76568(4) 0.03528(12) Uani 1 1 d . . . O1 O 0.18300(12) 0.24525(12) 0.2983(4) 0.0402(9) Uani 1 1 d . . . O2 O 0.13860(10) 0.18560(11) 0.4528(4) 0.0362(8) Uani 1 1 d . . . O3 O 0.30652(12) 0.15967(14) 0.3580(5) 0.0503(11) Uani 1 1 d . . . O4 O 0.89586(11) 0.20403(12) 0.8765(4) 0.0396(9) Uani 1 1 d . . . O5 O 0.91190(12) 0.20375(12) 0.6283(4) 0.0416(10) Uani 1 1 d . . . O6 O 0.83229(12) 0.06881(12) 0.8386(4) 0.0451(10) Uani 1 1 d . . . N1 N 0.16215(14) 0.27193(15) 0.5175(5) 0.0397(11) Uani 1 1 d . . . N2 N 0.19554(14) 0.19028(14) 0.6270(4) 0.0351(10) Uani 1 1 d . . . N3 N 0.23450(13) 0.17201(13) 0.4001(5) 0.0339(10) Uani 1 1 d . . . H3N H 0.2251 0.1469 0.3788 0.041 Uiso 1 1 calc R . . N4 N 0.25000(15) 0.24553(14) 0.4776(5) 0.0375(10) Uani 1 1 d . . . H4N H 0.2527 0.2707 0.5106 0.045 Uiso 1 1 calc R . . N5 N 0.35870(17) 0.2553(2) 0.4311(6) 0.0639(17) Uani 1 1 d . . . N6 N 0.97645(14) 0.19396(14) 0.8151(5) 0.0420(12) Uani 1 1 d . . . N7 N 0.95271(13) 0.13136(16) 0.6227(6) 0.0487(14) Uani 1 1 d . . . N8 N 0.86763(13) 0.12691(13) 0.7492(5) 0.0360(11) Uani 1 1 d . . . H8N H 0.8478 0.1334 0.6969 0.043 Uiso 1 1 calc R . . N9 N 0.93220(15) 0.11586(14) 0.8804(5) 0.0453(13) Uani 1 1 d . . . H9N H 0.9559 0.1142 0.9215 0.054 Uiso 1 1 calc R . . N10 N 0.9109(2) 0.02153(19) 1.0285(8) 0.078(2) Uani 1 1 d . . . C1 C 0.15306(19) 0.29793(19) 0.4237(6) 0.0453(15) Uani 1 1 d . . . C2 C 0.16468(19) 0.28264(18) 0.3070(6) 0.0429(14) Uani 1 1 d . . . C3 C 0.1564(2) 0.3082(2) 0.2092(7) 0.0580(18) Uani 1 1 d . . . H3A H 0.1639 0.2992 0.1307 0.070 Uiso 1 1 calc R . . C4 C 0.1363(3) 0.3484(3) 0.2269(9) 0.079(2) Uani 1 1 d . . . H4A H 0.1310 0.3658 0.1592 0.094 Uiso 1 1 calc R . . C5 C 0.1247(3) 0.3625(2) 0.3379(9) 0.071(2) Uani 1 1 d . . . H5A H 0.1110 0.3892 0.3463 0.085 Uiso 1 1 calc R . . C6 C 0.1330(2) 0.3373(2) 0.4404(7) 0.0536(18) Uani 1 1 d . . . C7 C 0.1204(2) 0.3477(2) 0.5578(8) 0.063(2) Uani 1 1 d . . . H7A H 0.1058 0.3735 0.5731 0.076 Uiso 1 1 calc R . . C8 C 0.1291(2) 0.3211(2) 0.6482(7) 0.060(2) Uani 1 1 d . . . H8A H 0.1206 0.3281 0.7275 0.072 Uiso 1 1 calc R . . C9 C 0.1505(2) 0.2829(2) 0.6266(6) 0.0491(16) Uani 1 1 d . . . H9A H 0.1566 0.2647 0.6920 0.059 Uiso 1 1 calc R . . C10 C 0.16004(16) 0.16540(16) 0.6462(5) 0.0347(12) Uani 1 1 d . . . C11 C 0.13058(16) 0.16384(15) 0.5526(6) 0.0350(12) Uani 1 1 d . . . C12 C 0.09525(16) 0.13837(17) 0.5673(6) 0.0416(14) Uani 1 1 d . . . H12A H 0.0748 0.1362 0.5050 0.050 Uiso 1 1 calc R . . C13 C 0.08970(17) 0.11580(19) 0.6747(7) 0.0469(15) Uani 1 1 d . . . H13A H 0.0654 0.0984 0.6838 0.056 Uiso 1 1 calc R . . C14 C 0.11788(18) 0.11809(18) 0.7653(7) 0.0452(15) Uani 1 1 d . . . H14A H 0.1129 0.1028 0.8373 0.054 Uiso 1 1 calc R . . C15 C 0.15435(17) 0.14281(16) 0.7539(6) 0.0388(13) Uani 1 1 d . . . C16 C 0.1865(2) 0.1460(2) 0.8398(7) 0.0505(16) Uani 1 1 d . . . H16A H 0.1840 0.1313 0.9139 0.061 Uiso 1 1 calc R . . C17 C 0.2218(2) 0.17027(19) 0.8172(6) 0.0457(15) Uani 1 1 d . . . H17A H 0.2438 0.1721 0.8753 0.055 Uiso 1 1 calc R . . C18 C 0.22537(17) 0.19179(17) 0.7112(6) 0.0393(13) Uani 1 1 d . . . H18A H 0.2500 0.2084 0.6973 0.047 Uiso 1 1 calc R . . C19 C 0.2972(2) 0.1184(2) 0.3090(9) 0.067(2) Uani 1 1 d . . . H19A H 0.3236 0.1046 0.2846 0.101 Uiso 1 1 calc R . . H19B H 0.2786 0.1215 0.2392 0.101 Uiso 1 1 calc R . . H19C H 0.2830 0.1011 0.3700 0.101 Uiso 1 1 calc R . . C20 C 0.27376(16) 0.18241(17) 0.3943(6) 0.0372(12) Uani 1 1 d . . . C21 C 0.28359(17) 0.22497(18) 0.4364(5) 0.0387(13) Uani 1 1 d . . . C22 C 0.32497(18) 0.24172(19) 0.4338(6) 0.0449(15) Uani 1 1 d . . . C23 C 0.96731(18) 0.22592(17) 0.8946(6) 0.0427(14) Uani 1 1 d . . . C24 C 0.92377(18) 0.23137(18) 0.9224(6) 0.0435(14) Uani 1 1 d . . . C25 C 0.9129(2) 0.2649(2) 0.9950(7) 0.0554(19) Uani 1 1 d . . . H25A H 0.8839 0.2704 1.0113 0.067 Uiso 1 1 calc R . . C26 C 0.9440(2) 0.2911(2) 1.0453(8) 0.0641(19) Uani 1 1 d . . . H26A H 0.9356 0.3137 1.0963 0.077 Uiso 1 1 calc R . . C27 C 0.9863(2) 0.2848(2) 1.0226(9) 0.067(2) Uani 1 1 d . . . H27A H 1.0069 0.3026 1.0588 0.081 Uiso 1 1 calc R . . C28 C 0.99883(19) 0.2522(2) 0.9463(8) 0.0542(18) Uani 1 1 d . . . C29 C 1.0414(2) 0.2426(2) 0.9165(8) 0.063(2) Uani 1 1 d . . . H29A H 1.0639 0.2583 0.9512 0.075 Uiso 1 1 calc R . . C30 C 1.04950(19) 0.2109(2) 0.8385(8) 0.065(2) Uani 1 1 d . . . H30A H 1.0780 0.2049 0.8173 0.078 Uiso 1 1 calc R . . C31 C 1.01710(17) 0.1871(2) 0.7886(8) 0.058(2) Uani 1 1 d . . . H31A H 1.0241 0.1652 0.7337 0.069 Uiso 1 1 calc R . . C32 C 0.95312(17) 0.1554(2) 0.5219(7) 0.0495(16) Uani 1 1 d . . . C33 C 0.93061(17) 0.1938(2) 0.5270(7) 0.0481(15) Uani 1 1 d . . . C34 C 0.9295(2) 0.2183(3) 0.4229(7) 0.064(2) Uani 1 1 d . . . H34A H 0.9135 0.2438 0.4226 0.076 Uiso 1 1 calc R . . C35 C 0.9507(3) 0.2066(3) 0.3212(8) 0.078(2) Uani 1 1 d U . . H35A H 0.9497 0.2246 0.2529 0.093 Uiso 1 1 calc R . . C36 C 0.9723(3) 0.1714(4) 0.3152(10) 0.084(2) Uani 1 1 d U . . H36A H 0.9870 0.1647 0.2432 0.101 Uiso 1 1 calc R . . C37 C 0.9747(2) 0.1420(3) 0.4162(8) 0.0697(18) Uani 1 1 d U . . C38 C 0.9950(2) 0.1011(3) 0.4266(10) 0.083(2) Uani 1 1 d U . . H38A H 1.0096 0.0900 0.3591 0.099 Uiso 1 1 calc R . . C39 C 0.9940(2) 0.0784(3) 0.5269(12) 0.085(3) Uani 1 1 d . . . H39A H 1.0083 0.0519 0.5307 0.102 Uiso 1 1 calc R . . C40 C 0.97224(18) 0.0932(2) 0.6254(9) 0.064(2) Uani 1 1 d . . . H40A H 0.9709 0.0764 0.6960 0.077 Uiso 1 1 calc R . . C41 C 0.79327(18) 0.0786(2) 0.7779(8) 0.0568(18) Uani 1 1 d . . . H41A H 0.7720 0.0570 0.7971 0.085 Uiso 1 1 calc R . . H41B H 0.7981 0.0791 0.6911 0.085 Uiso 1 1 calc R . . H41C H 0.7831 0.1064 0.8041 0.085 Uiso 1 1 calc R . . C42 C 0.86432(17) 0.09526(16) 0.8220(6) 0.0368(12) Uani 1 1 d . . . C43 C 0.90161(18) 0.08747(17) 0.8954(6) 0.0411(13) Uani 1 1 d . . . C44 C 0.90636(19) 0.05131(19) 0.9684(7) 0.0515(16) Uani 1 1 d . . . O1W O 0.80936(13) 0.22146(17) 0.8748(4) 0.0578(13) Uani 1 1 d . . . H1WA H 0.8353 0.2144 0.8690 0.069 Uiso 1 1 d R . . H1WB H 0.7955 0.2087 0.8204 0.069 Uiso 1 1 d R . . O2W O 0.0000 0.0000 0.1997(18) 0.083(5) Uani 0.50 2 d SP . . O1S O 0.0368(5) 0.2595(6) 0.5144(18) 0.131(5) Uani 0.50 1 d PDU . . H1SA H 0.0416 0.2433 0.5726 0.197 Uiso 0.50 1 calc PR . . C1S C 0.0109(8) 0.2940(8) 0.553(3) 0.141(7) Uani 0.50 1 d PDU . . H1SB H 0.0255 0.3105 0.6163 0.169 Uiso 0.50 1 calc PR . . H1SC H -0.0162 0.2833 0.5860 0.169 Uiso 0.50 1 calc PR . . C2S C 0.0027(10) 0.3218(10) 0.443(3) 0.154(8) Uani 0.50 1 d PDU . . H2SA H -0.0150 0.3459 0.4659 0.230 Uiso 0.50 1 calc PR . . H2SB H -0.0118 0.3051 0.3813 0.230 Uiso 0.50 1 calc PR . . H2SC H 0.0298 0.3321 0.4113 0.230 Uiso 0.50 1 calc PR . . 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 0.02930(19) 0.03211(19) 0.0374(3) -0.00307(17) -0.00055(16) -0.00692(15) Ru2 0.02370(18) 0.02945(18) 0.0527(3) 0.00350(17) -0.00286(17) 0.00281(14) O1 0.045(2) 0.041(2) 0.035(3) 0.0013(16) 0.0009(17) -0.0027(16) O2 0.0289(16) 0.0400(19) 0.040(3) -0.0037(17) 0.0005(16) -0.0073(14) O3 0.0318(19) 0.049(2) 0.070(4) -0.006(2) 0.0024(19) -0.0043(17) O4 0.0312(18) 0.0382(19) 0.049(3) -0.0017(17) 0.0032(16) 0.0008(15) O5 0.0326(19) 0.042(2) 0.050(3) 0.0116(18) 0.0061(17) 0.0037(16) O6 0.040(2) 0.039(2) 0.056(3) 0.0089(19) -0.0036(18) -0.0070(16) N1 0.034(2) 0.043(2) 0.043(3) -0.008(2) -0.006(2) -0.0049(19) N2 0.035(2) 0.034(2) 0.036(3) -0.0038(19) -0.0004(19) -0.0022(18) N3 0.031(2) 0.030(2) 0.040(3) -0.0006(19) -0.0018(19) -0.0056(17) N4 0.038(2) 0.034(2) 0.040(3) -0.002(2) 0.003(2) -0.0132(17) N5 0.039(3) 0.072(4) 0.081(5) 0.005(3) 0.005(3) -0.018(3) N6 0.028(2) 0.032(2) 0.066(4) 0.001(2) -0.005(2) 0.0026(18) N7 0.021(2) 0.047(3) 0.078(5) -0.021(3) -0.002(2) -0.0014(18) N8 0.0281(19) 0.032(2) 0.049(3) 0.007(2) 0.000(2) 0.0021(16) N9 0.038(2) 0.036(2) 0.062(4) 0.009(2) -0.018(2) 0.0025(19) N10 0.087(5) 0.052(3) 0.094(6) 0.029(4) 0.001(4) 0.008(3) C1 0.040(3) 0.043(3) 0.053(5) -0.005(3) 0.000(3) -0.007(2) C2 0.046(3) 0.038(3) 0.044(4) -0.002(2) 0.007(3) -0.004(2) C3 0.071(4) 0.058(4) 0.044(5) 0.008(3) -0.005(3) 0.009(3) C4 0.103(6) 0.062(4) 0.071(7) 0.019(4) -0.004(5) 0.018(4) C5 0.080(5) 0.052(4) 0.080(7) 0.003(4) -0.008(5) 0.019(4) C6 0.045(3) 0.049(3) 0.067(6) -0.009(3) -0.006(3) 0.004(3) C7 0.060(4) 0.059(4) 0.071(6) -0.024(4) -0.014(4) 0.018(3) C8 0.057(4) 0.073(5) 0.050(5) -0.029(4) -0.005(3) 0.010(3) C9 0.046(3) 0.057(4) 0.044(4) -0.012(3) -0.006(3) 0.003(3) C10 0.034(3) 0.029(2) 0.041(4) -0.004(2) 0.003(2) -0.001(2) C11 0.032(2) 0.031(2) 0.042(4) -0.004(2) 0.004(2) 0.0028(19) C12 0.027(2) 0.040(3) 0.058(5) -0.006(3) 0.002(2) -0.002(2) C13 0.029(3) 0.042(3) 0.070(5) 0.002(3) 0.016(3) -0.003(2) C14 0.046(3) 0.041(3) 0.048(4) 0.009(3) 0.014(3) 0.001(2) C15 0.041(3) 0.033(2) 0.042(4) 0.000(2) 0.005(3) 0.004(2) C16 0.064(4) 0.044(3) 0.043(4) 0.002(3) 0.002(3) 0.009(3) C17 0.052(3) 0.045(3) 0.040(4) -0.001(3) -0.014(3) -0.001(3) C18 0.040(3) 0.036(3) 0.042(4) -0.003(2) -0.014(2) -0.005(2) C19 0.038(3) 0.057(4) 0.106(7) -0.025(4) 0.009(4) 0.001(3) C20 0.032(3) 0.040(3) 0.040(4) 0.004(2) 0.003(2) -0.003(2) C21 0.033(3) 0.044(3) 0.038(4) 0.001(2) 0.001(2) -0.010(2) C22 0.037(3) 0.048(3) 0.050(4) 0.001(3) -0.004(3) -0.006(2) C23 0.037(3) 0.035(3) 0.056(4) 0.001(3) -0.007(3) 0.001(2) C24 0.040(3) 0.037(3) 0.053(4) 0.008(3) 0.002(3) 0.000(2) C25 0.043(3) 0.053(4) 0.071(6) -0.006(3) 0.011(3) -0.001(3) C26 0.069(4) 0.060(4) 0.062(5) -0.023(4) 0.004(4) -0.002(3) C27 0.055(4) 0.063(4) 0.083(6) -0.017(4) -0.008(4) -0.009(3) C28 0.040(3) 0.046(3) 0.077(6) -0.006(3) -0.004(3) -0.005(2) C29 0.034(3) 0.056(4) 0.098(7) -0.012(4) -0.010(3) -0.006(3) C30 0.028(3) 0.056(4) 0.111(7) -0.015(4) -0.004(3) 0.000(3) C31 0.026(3) 0.045(3) 0.102(6) -0.018(3) 0.001(3) 0.002(2) C32 0.027(3) 0.059(4) 0.062(5) -0.016(3) 0.005(3) -0.011(2) C33 0.028(2) 0.059(3) 0.057(5) -0.002(3) 0.001(3) -0.014(2) C34 0.050(4) 0.087(5) 0.054(5) 0.010(4) 0.003(3) -0.027(4) C35 0.067(4) 0.109(5) 0.057(5) -0.001(4) 0.003(4) -0.037(3) C36 0.058(4) 0.123(5) 0.072(5) -0.028(4) 0.014(4) -0.036(4) C37 0.036(3) 0.088(4) 0.085(5) -0.035(3) 0.002(3) -0.020(3) C38 0.042(3) 0.096(4) 0.110(6) -0.068(4) 0.006(4) -0.008(3) C39 0.034(3) 0.072(5) 0.148(10) -0.054(6) -0.003(5) 0.000(3) C40 0.027(3) 0.046(3) 0.120(7) -0.032(4) -0.006(3) 0.001(2) C41 0.033(3) 0.060(4) 0.077(5) 0.016(4) -0.005(3) -0.010(3) C42 0.036(3) 0.031(3) 0.043(4) -0.001(2) -0.001(2) 0.004(2) C43 0.042(3) 0.033(3) 0.048(4) 0.002(2) -0.009(3) 0.003(2) C44 0.051(3) 0.040(3) 0.064(5) 0.010(3) -0.007(3) 0.002(2) O1W 0.034(2) 0.093(4) 0.047(3) -0.021(2) 0.0005(19) 0.014(2) O2W 0.089(12) 0.087(11) 0.073(14) 0.000 0.000 0.010(10) O1S 0.116(8) 0.147(8) 0.131(10) -0.043(7) -0.001(7) -0.034(6) C1S 0.123(11) 0.141(10) 0.158(11) -0.016(8) -0.014(9) -0.017(8) C2S 0.140(12) 0.165(11) 0.156(12) -0.004(9) -0.013(9) -0.038(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 N4 1.922(4) . ? Ru1 N2 2.037(5) . ? Ru1 N1 2.055(5) . ? Ru1 O1 2.056(4) . ? Ru1 N3 2.063(4) . ? Ru1 O2 2.085(3) . ? Ru2 N9 1.936(5) . ? Ru2 O4 2.029(4) . ? Ru2 N6 2.055(5) . ? Ru2 N8 2.064(4) . ? Ru2 N7 2.071(5) . ? Ru2 O5 2.073(4) . ? O1 C2 1.318(7) . ? O2 C11 1.332(7) . ? O3 C20 1.322(7) . ? O3 C19 1.442(8) . ? O4 C24 1.335(7) . ? O5 C33 1.312(8) . ? O6 C42 1.324(7) . ? O6 C41 1.439(7) . ? N1 C9 1.318(8) . ? N1 C1 1.360(8) . ? N2 C18 1.331(7) . ? N2 C10 1.385(7) . ? N3 C20 1.284(7) . ? N3 H3N 0.8800 . ? N4 C21 1.326(8) . ? N4 H4N 0.8800 . ? N5 C22 1.149(8) . ? N6 C31 1.335(7) . ? N6 C23 1.374(8) . ? N7 C40 1.355(8) . ? N7 C32 1.357(10) . ? N8 C42 1.291(7) . ? N8 H8N 0.8800 . ? N9 C43 1.328(7) . ? N9 H9N 0.8800 . ? N10 C44 1.163(9) . ? C1 C6 1.409(9) . ? C1 C2 1.435(9) . ? C2 C3 1.383(9) . ? C3 C4 1.430(10) . ? C3 H3A 0.9500 . ? C4 C5 1.366(13) . ? C4 H4A 0.9500 . ? C5 C6 1.417(11) . ? C5 H5A 0.9500 . ? C6 C7 1.407(12) . ? C7 C8 1.341(12) . ? C7 H7A 0.9500 . ? C8 C9 1.400(10) . ? C8 H8A 0.9500 . ? C9 H9A 0.9500 . ? C10 C11 1.399(8) . ? C10 C15 1.408(8) . ? C11 C12 1.385(7) . ? C12 C13 1.404(9) . ? C12 H12A 0.9500 . ? C13 C14 1.348(10) . ? C13 H13A 0.9500 . ? C14 C15 1.397(8) . ? C14 H14A 0.9500 . ? C15 C16 1.401(9) . ? C16 C17 1.377(9) . ? C16 H16A 0.9500 . ? C17 C18 1.368(9) . ? C17 H17A 0.9500 . ? C18 H18A 0.9500 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 C21 1.457(8) . ? C21 C22 1.410(7) . ? C23 C28 1.418(9) . ? C23 C24 1.419(8) . ? C24 C25 1.376(9) . ? C25 C26 1.399(10) . ? C25 H25A 0.9500 . ? C26 C27 1.374(10) . ? C26 H26A 0.9500 . ? C27 C28 1.393(10) . ? C27 H27A 0.9500 . ? C28 C29 1.416(9) . ? C29 C30 1.350(11) . ? C29 H29A 0.9500 . ? C30 C31 1.386(9) . ? C30 H30A 0.9500 . ? C31 H31A 0.9500 . ? C32 C33 1.408(9) . ? C32 C37 1.425(10) . ? C33 C34 1.395(11) . ? C34 C35 1.369(12) . ? C34 H34A 0.9500 . ? C35 C36 1.305(14) . ? C35 H35A 0.9500 . ? C36 C37 1.462(14) . ? C36 H36A 0.9500 . ? C37 C38 1.447(13) . ? C38 C39 1.329(14) . ? C38 H38A 0.9500 . ? C39 C40 1.376(13) . ? C39 H39A 0.9500 . ? C40 H40A 0.9500 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 C43 1.455(8) . ? C43 C44 1.410(9) . ? O1W H1WA 0.8500 . ? O1W H1WB 0.8501 . ? O1S C1S 1.429(17) . ? O1S H1SA 0.8400 . ? C1S C2S 1.531(19) . ? C1S H1SB 0.9900 . ? C1S H1SC 0.9900 . ? C2S H2SA 0.9800 . ? C2S H2SB 0.9800 . ? C2S H2SC 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 N4 Ru1 N2 96.8(2) . . ? N4 Ru1 N1 94.83(19) . . ? N2 Ru1 N1 95.98(19) . . ? N4 Ru1 O1 93.97(19) . . ? N2 Ru1 O1 169.01(16) . . ? N1 Ru1 O1 80.93(19) . . ? N4 Ru1 N3 78.52(18) . . ? N2 Ru1 N3 88.90(18) . . ? N1 Ru1 N3 172.21(18) . . ? O1 Ru1 N3 95.37(18) . . ? N4 Ru1 O2 174.87(18) . . ? N2 Ru1 O2 80.03(17) . . ? N1 Ru1 O2 89.54(16) . . ? O1 Ru1 O2 89.37(16) . . ? N3 Ru1 O2 97.30(15) . . ? N9 Ru2 O4 98.8(2) . . ? N9 Ru2 N6 94.3(2) . . ? O4 Ru2 N6 81.05(18) . . ? N9 Ru2 N8 78.53(19) . . ? O4 Ru2 N8 92.46(17) . . ? N6 Ru2 N8 169.5(2) . . ? N9 Ru2 N7 96.3(2) . . ? O4 Ru2 N7 164.3(2) . . ? N6 Ru2 N7 93.78(19) . . ? N8 Ru2 N7 94.55(19) . . ? N9 Ru2 O5 173.3(2) . . ? O4 Ru2 O5 86.62(16) . . ? N6 Ru2 O5 90.47(18) . . ? N8 Ru2 O5 97.39(17) . . ? N7 Ru2 O5 78.6(2) . . ? C2 O1 Ru1 112.0(4) . . ? C11 O2 Ru1 112.2(3) . . ? C20 O3 C19 116.5(5) . . ? C24 O4 Ru2 112.8(3) . . ? C33 O5 Ru2 113.8(4) . . ? C42 O6 C41 116.9(5) . . ? C9 N1 C1 119.4(5) . . ? C9 N1 Ru1 128.7(5) . . ? C1 N1 Ru1 111.8(4) . . ? C18 N2 C10 118.9(5) . . ? C18 N2 Ru1 128.1(4) . . ? C10 N2 Ru1 112.9(4) . . ? C20 N3 Ru1 114.3(4) . . ? C20 N3 H3N 122.8 . . ? Ru1 N3 H3N 122.8 . . ? C21 N4 Ru1 118.6(4) . . ? C21 N4 H4N 120.7 . . ? Ru1 N4 H4N 120.7 . . ? C31 N6 C23 117.7(5) . . ? C31 N6 Ru2 130.2(4) . . ? C23 N6 Ru2 111.9(4) . . ? C40 N7 C32 120.8(7) . . ? C40 N7 Ru2 126.2(6) . . ? C32 N7 Ru2 113.0(4) . . ? C42 N8 Ru2 114.6(4) . . ? C42 N8 H8N 122.7 . . ? Ru2 N8 H8N 122.7 . . ? C43 N9 Ru2 118.2(4) . . ? C43 N9 H9N 120.9 . . ? Ru2 N9 H9N 120.9 . . ? N1 C1 C6 121.7(6) . . ? N1 C1 C2 116.1(5) . . ? C6 C1 C2 122.1(6) . . ? O1 C2 C3 123.2(6) . . ? O1 C2 C1 118.7(6) . . ? C3 C2 C1 118.1(6) . . ? C2 C3 C4 119.5(7) . . ? C2 C3 H3A 120.3 . . ? C4 C3 H3A 120.3 . . ? C5 C4 C3 122.3(8) . . ? C5 C4 H4A 118.8 . . ? C3 C4 H4A 118.8 . . ? C4 C5 C6 119.9(7) . . ? C4 C5 H5A 120.1 . . ? C6 C5 H5A 120.1 . . ? C7 C6 C1 117.2(7) . . ? C7 C6 C5 124.6(7) . . ? C1 C6 C5 118.1(7) . . ? C8 C7 C6 119.7(6) . . ? C8 C7 H7A 120.2 . . ? C6 C7 H7A 120.2 . . ? C7 C8 C9 120.6(7) . . ? C7 C8 H8A 119.7 . . ? C9 C8 H8A 119.7 . . ? N1 C9 C8 121.3(7) . . ? N1 C9 H9A 119.3 . . ? C8 C9 H9A 119.3 . . ? N2 C10 C11 116.3(5) . . ? N2 C10 C15 121.5(5) . . ? C11 C10 C15 122.3(5) . . ? O2 C11 C12 123.5(5) . . ? O2 C11 C10 118.6(5) . . ? C12 C11 C10 117.8(5) . . ? C11 C12 C13 119.8(6) . . ? C11 C12 H12A 120.1 . . ? C13 C12 H12A 120.1 . . ? C14 C13 C12 122.0(5) . . ? C14 C13 H13A 119.0 . . ? C12 C13 H13A 119.0 . . ? C13 C14 C15 120.3(6) . . ? C13 C14 H14A 119.8 . . ? C15 C14 H14A 119.8 . . ? C14 C15 C16 125.1(6) . . ? C14 C15 C10 117.8(6) . . ? C16 C15 C10 117.1(5) . . ? C17 C16 C15 120.1(6) . . ? C17 C16 H16A 120.0 . . ? C15 C16 H16A 120.0 . . ? C18 C17 C16 120.1(6) . . ? C18 C17 H17A 120.0 . . ? C16 C17 H17A 120.0 . . ? N2 C18 C17 122.3(5) . . ? N2 C18 H18A 118.8 . . ? C17 C18 H18A 118.8 . . ? O3 C19 H19A 109.5 . . ? O3 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? O3 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? N3 C20 O3 129.2(5) . . ? N3 C20 C21 115.1(5) . . ? O3 C20 C21 115.6(5) . . ? N4 C21 C22 124.4(5) . . ? N4 C21 C20 113.1(5) . . ? C22 C21 C20 122.5(5) . . ? N5 C22 C21 179.7(9) . . ? N6 C23 C28 123.0(5) . . ? N6 C23 C24 115.7(5) . . ? C28 C23 C24 121.3(6) . . ? O4 C24 C25 124.0(5) . . ? O4 C24 C23 118.5(5) . . ? C25 C24 C23 117.5(6) . . ? C24 C25 C26 121.1(6) . . ? C24 C25 H25A 119.5 . . ? C26 C25 H25A 119.5 . . ? C27 C26 C25 121.4(7) . . ? C27 C26 H26A 119.3 . . ? C25 C26 H26A 119.3 . . ? C26 C27 C28 119.7(6) . . ? C26 C27 H27A 120.1 . . ? C28 C27 H27A 120.1 . . ? C27 C28 C29 124.9(6) . . ? C27 C28 C23 118.7(6) . . ? C29 C28 C23 116.4(6) . . ? C30 C29 C28 119.4(6) . . ? C30 C29 H29A 120.3 . . ? C28 C29 H29A 120.3 . . ? C29 C30 C31 121.4(6) . . ? C29 C30 H30A 119.3 . . ? C31 C30 H30A 119.3 . . ? N6 C31 C30 122.1(6) . . ? N6 C31 H31A 118.9 . . ? C30 C31 H31A 118.9 . . ? N7 C32 C33 116.3(6) . . ? N7 C32 C37 121.6(7) . . ? C33 C32 C37 122.0(8) . . ? O5 C33 C34 125.0(6) . . ? O5 C33 C32 117.9(7) . . ? C34 C33 C32 117.1(7) . . ? C35 C34 C33 121.9(9) . . ? C35 C34 H34A 119.1 . . ? C33 C34 H34A 119.1 . . ? C36 C35 C34 121.9(10) . . ? C36 C35 H35A 119.0 . . ? C34 C35 H35A 119.0 . . ? C35 C36 C37 121.8(9) . . ? C35 C36 H36A 119.1 . . ? C37 C36 H36A 119.1 . . ? C32 C37 C38 114.2(9) . . ? C32 C37 C36 115.2(8) . . ? C38 C37 C36 130.6(9) . . ? C39 C38 C37 122.6(8) . . ? C39 C38 H38A 118.7 . . ? C37 C38 H38A 118.7 . . ? C38 C39 C40 120.0(8) . . ? C38 C39 H39A 120.0 . . ? C40 C39 H39A 120.0 . . ? N7 C40 C39 120.8(9) . . ? N7 C40 H40A 119.6 . . ? C39 C40 H40A 119.6 . . ? O6 C41 H41A 109.5 . . ? O6 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? O6 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? N8 C42 O6 129.6(5) . . ? N8 C42 C43 114.8(5) . . ? O6 C42 C43 115.7(5) . . ? N9 C43 C44 122.8(5) . . ? N9 C43 C42 113.8(5) . . ? C44 C43 C42 123.2(5) . . ? N10 C44 C43 179.1(7) . . ? H1WA O1W H1WB 108.6 . . ? C1S O1S H1SA 109.5 . . ? O1S C1S C2S 107(2) . . ? O1S C1S H1SB 110.3 . . ? C2S C1S H1SB 110.3 . . ? O1S C1S H1SC 110.3 . . ? C2S C1S H1SC 110.3 . . ? H1SB C1S H1SC 108.6 . . ? C1S C2S H2SA 109.5 . . ? C1S C2S H2SB 109.5 . . ? H2SA C2S H2SB 109.5 . . ? C1S C2S H2SC 109.5 . . ? H2SA C2S H2SC 109.5 . . ? H2SB C2S H2SC 109.5 . . ? _diffrn_measured_fraction_theta_max 0.951 _diffrn_reflns_theta_full 66.89 _diffrn_measured_fraction_theta_full 0.951 _refine_diff_density_max 0.606 _refine_diff_density_min -0.358 _refine_diff_density_rms 0.096 # start Validation Reply Form _vrf_PLAT602_102809a ; PROBLEM: VERY LARGE Solvent Accessible VOID(S) in Structure ! RESPONSE: Some of the solvent molecules are lost easily. The residual electron densities are too weak (less than 0.61) to model the solvent molecules well. ; # end Validation Reply Form # Attachment '- 779199.cif' data_060809c _database_code_depnum_ccdc_archive 'CCDC 779199' #TrackingRef '- 779199.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C25 H23.75 N4 O5.88 Ru' _chemical_formula_weight 575.30 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru 0.0552 3.2960 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 15.20680(10) _cell_length_b 18.9057(2) _cell_length_c 17.7568(2) _cell_angle_alpha 90.00 _cell_angle_beta 104.0680(10) _cell_angle_gamma 90.00 _cell_volume 4951.88(8) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 18957 _cell_measurement_theta_min 3.4383 _cell_measurement_theta_max 71.0579 _exptl_crystal_description rectangle _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.543 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2342 _exptl_absorpt_coefficient_mu 5.532 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.20669 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details 'CrysAlisPro, Oxford Diffraction Ltd' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'Enhance Ultra (Cu) X-ray Source' _diffrn_radiation_monochromator mirror _diffrn_measurement_device_type 'Xcalibur, Sapphire3, Gemini ultra' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.1270 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26771 _diffrn_reflns_av_R_equivalents 0.0201 _diffrn_reflns_av_sigmaI/netI 0.0197 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.44 _diffrn_reflns_theta_max 67.00 _reflns_number_total 8816 _reflns_number_gt 7420 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlisPro, Oxford Diffraction Ltd' _computing_cell_refinement 'CrysAlisPro, Oxford Diffraction Ltd' _computing_data_reduction 'CrysAlisPro, Oxford Diffraction Ltd' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics Ortep-3 _computing_publication_material Wingx _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The sof for O2W was assigned to be 0.75, this makes the anisotropic displacement parameters of O2W going to more appropriate values. ; _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^)+(0.0407P)^2^+0.9976P] 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 8816 _refine_ls_number_parameters 650 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0334 _refine_ls_R_factor_gt 0.0259 _refine_ls_wR_factor_ref 0.0699 _refine_ls_wR_factor_gt 0.0679 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.050 _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 0.516528(12) 0.168212(9) 0.263605(10) 0.03634(6) Uani 1 1 d . . . Ru2 Ru 0.842419(14) 0.140300(10) 0.202287(11) 0.04375(6) Uani 1 1 d . . . O1 O 0.47064(13) 0.13398(10) 0.15231(9) 0.0509(4) Uani 1 1 d . . . O2 O 0.61019(11) 0.08718(8) 0.27622(9) 0.0417(4) Uani 1 1 d . . . O3 O 0.59410(13) 0.36221(9) 0.18911(12) 0.0559(5) Uani 1 1 d . . . O4 O 0.40373(15) 0.42503(10) 0.18762(13) 0.0681(6) Uani 1 1 d . . . O5 O 0.32589(14) 0.33741(10) 0.22644(13) 0.0608(5) Uani 1 1 d . . . O6 O 0.76932(14) 0.18007(10) 0.09937(10) 0.0580(5) Uani 1 1 d . . . O7 O 0.78063(12) 0.21319(9) 0.25991(10) 0.0452(4) Uani 1 1 d . . . O8 O 0.71508(16) -0.05511(10) 0.14906(14) 0.0752(6) Uani 1 1 d . . . O9 O 0.8861(3) -0.10986(14) 0.0925(2) 0.1404(15) Uani 1 1 d . . . O10 O 0.9738(2) -0.01513(13) 0.0951(2) 0.1150(12) Uani 1 1 d . . . N1 N 0.42811(14) 0.09156(10) 0.28180(12) 0.0427(5) Uani 1 1 d . . . N2 N 0.57972(14) 0.17939(10) 0.37929(11) 0.0396(4) Uani 1 1 d . . . N3 N 0.59704(13) 0.24429(10) 0.23249(11) 0.0400(4) Uani 1 1 d . . . H3N H 0.6523 0.2361 0.2313 0.048 Uiso 1 1 calc R . . N4 N 0.43760(13) 0.25072(10) 0.24911(11) 0.0405(4) Uani 1 1 d . . . N5 N 0.92412(16) 0.22591(12) 0.19175(14) 0.0539(6) Uani 1 1 d . . . N6 N 0.90587(15) 0.11784(11) 0.31508(13) 0.0486(5) Uani 1 1 d . . . N7 N 0.74986(15) 0.06068(10) 0.19676(11) 0.0455(5) Uani 1 1 d . . . H7N H 0.7027 0.0658 0.2149 0.055 Uiso 1 1 calc R . . N8 N 0.89508(17) 0.06420(12) 0.15399(14) 0.0560(6) Uani 1 1 d . . . C1 C 0.38966(18) 0.05569(13) 0.21469(16) 0.0484(6) Uani 1 1 d . . . C2 C 0.41504(19) 0.07944(14) 0.14664(15) 0.0525(6) Uani 1 1 d . . . C3 C 0.3793(3) 0.04339(19) 0.07868(19) 0.0766(9) Uani 1 1 d . . . H3A H 0.3953 0.0565 0.0333 0.092 Uiso 1 1 calc R . . C4 C 0.3192(3) -0.0128(2) 0.0774(2) 0.0957(13) Uani 1 1 d . . . H4A H 0.2964 -0.0366 0.0309 0.115 Uiso 1 1 calc R . . C5 C 0.2928(3) -0.0339(2) 0.1415(3) 0.0921(12) Uani 1 1 d . . . H5A H 0.2516 -0.0708 0.1380 0.111 Uiso 1 1 calc R . . C6 C 0.3276(2) -0.00011(16) 0.2138(2) 0.0666(8) Uani 1 1 d . . . C7 C 0.3067(2) -0.01674(17) 0.2842(2) 0.0768(10) Uani 1 1 d . . . H7A H 0.2646 -0.0520 0.2857 0.092 Uiso 1 1 calc R . . C8 C 0.3473(2) 0.01802(17) 0.3506(2) 0.0723(9) Uani 1 1 d . . . H8A H 0.3347 0.0056 0.3976 0.087 Uiso 1 1 calc R . . C9 C 0.40794(19) 0.07234(14) 0.34735(16) 0.0533(7) Uani 1 1 d . . . H9A H 0.4353 0.0961 0.3929 0.064 Uiso 1 1 calc R . . C10 C 0.64131(16) 0.12620(12) 0.40611(13) 0.0382(5) Uani 1 1 d . . . C11 C 0.65505(17) 0.07752(12) 0.34882(14) 0.0399(5) Uani 1 1 d . . . C12 C 0.71698(19) 0.02388(14) 0.37361(16) 0.0530(7) Uani 1 1 d . . . H12A H 0.7269 -0.0093 0.3380 0.064 Uiso 1 1 calc R . . C13 C 0.7647(2) 0.01858(15) 0.45074(17) 0.0573(7) Uani 1 1 d . . . H13A H 0.8065 -0.0178 0.4653 0.069 Uiso 1 1 calc R . . C14 C 0.75206(19) 0.06518(15) 0.50556(16) 0.0543(7) Uani 1 1 d . . . H14A H 0.7849 0.0606 0.5568 0.065 Uiso 1 1 calc R . . C15 C 0.68903(18) 0.12021(14) 0.48405(14) 0.0460(6) Uani 1 1 d . . . C16 C 0.6708(2) 0.17202(16) 0.53538(16) 0.0603(7) Uani 1 1 d . . . H16A H 0.6986 0.1693 0.5881 0.072 Uiso 1 1 calc R . . C17 C 0.6129(2) 0.22562(17) 0.50794(17) 0.0670(8) Uani 1 1 d . . . H17A H 0.6026 0.2605 0.5417 0.080 Uiso 1 1 calc R . . C18 C 0.5685(2) 0.22886(14) 0.42920(16) 0.0535(7) Uani 1 1 d . . . H18A H 0.5300 0.2667 0.4113 0.064 Uiso 1 1 calc R . . C19 C 0.6792(2) 0.35310(17) 0.1698(2) 0.0737(10) Uani 1 1 d . . . H19A H 0.7255 0.3440 0.2162 0.111 Uiso 1 1 calc R . . H19B H 0.6940 0.3953 0.1454 0.111 Uiso 1 1 calc R . . H19C H 0.6754 0.3139 0.1348 0.111 Uiso 1 1 calc R . . C20 C 0.55992(17) 0.30485(13) 0.21500(14) 0.0415(5) Uani 1 1 d . . . C21 C 0.46840(17) 0.30952(13) 0.22404(14) 0.0438(6) Uani 1 1 d . . . C22 C 0.40272(19) 0.36566(14) 0.20970(16) 0.0506(6) Uani 1 1 d . . . C23 C 0.34237(18) 0.26469(14) 0.25388(17) 0.0542(7) Uani 1 1 d . . . C24 C 0.3331(2) 0.2627(2) 0.3364(2) 0.0821(11) Uani 1 1 d . . . H24A H 0.3767 0.2941 0.3677 0.123 Uiso 1 1 calc R . . H24B H 0.3436 0.2154 0.3562 0.123 Uiso 1 1 calc R . . H24C H 0.2731 0.2773 0.3378 0.123 Uiso 1 1 calc R . . C25 C 0.2774(2) 0.21735(17) 0.1995(2) 0.0721(9) Uani 1 1 d . . . H25A H 0.2871 0.2214 0.1483 0.108 Uiso 1 1 calc R . . H25B H 0.2164 0.2311 0.1986 0.108 Uiso 1 1 calc R . . H25C H 0.2871 0.1693 0.2169 0.108 Uiso 1 1 calc R . . C26 C 0.8843(2) 0.26580(14) 0.12711(17) 0.0570(7) Uani 1 1 d . . . C27 C 0.8035(2) 0.23961(15) 0.07941(16) 0.0582(7) Uani 1 1 d . . . C28 C 0.7623(3) 0.27778(18) 0.01354(18) 0.0751(10) Uani 1 1 d . . . H28A H 0.7099 0.2607 -0.0201 0.090 Uiso 1 1 calc R . . C29 C 0.7996(4) 0.3417(2) -0.0022(2) 0.0899(13) Uani 1 1 d . . . H29A H 0.7708 0.3670 -0.0462 0.108 Uiso 1 1 calc R . . C30 C 0.8760(3) 0.36813(19) 0.0442(2) 0.0891(13) Uani 1 1 d . . . H30A H 0.8988 0.4111 0.0319 0.107 Uiso 1 1 calc R . . C31 C 0.9216(3) 0.33121(17) 0.1113(2) 0.0730(10) Uani 1 1 d . . . C32 C 0.9994(3) 0.3540(2) 0.1645(3) 0.0917(13) Uani 1 1 d . . . H32A H 1.0258 0.3967 0.1561 0.110 Uiso 1 1 calc R . . C33 C 1.0372(3) 0.3156(2) 0.2278(3) 0.0879(11) Uani 1 1 d . . . H33A H 1.0889 0.3317 0.2631 0.106 Uiso 1 1 calc R . . C34 C 0.9974(2) 0.25026(18) 0.2398(2) 0.0689(8) Uani 1 1 d . . . H34A H 1.0241 0.2236 0.2834 0.083 Uiso 1 1 calc R . . C35 C 0.88622(18) 0.16592(14) 0.36713(15) 0.0476(6) Uani 1 1 d . . . C36 C 0.81891(17) 0.21662(13) 0.33472(15) 0.0442(6) Uani 1 1 d . . . C37 C 0.7972(2) 0.26671(15) 0.38483(17) 0.0566(7) Uani 1 1 d . . . H37A H 0.7533 0.3009 0.3659 0.068 Uiso 1 1 calc R . . C38 C 0.8418(3) 0.26540(18) 0.46407(19) 0.0716(9) Uani 1 1 d . . . H38A H 0.8270 0.2996 0.4966 0.086 Uiso 1 1 calc R . . C39 C 0.9052(3) 0.2165(2) 0.49491(18) 0.0761(10) Uani 1 1 d . . . H39A H 0.9335 0.2177 0.5476 0.091 Uiso 1 1 calc R . . C40 C 0.9283(2) 0.16385(17) 0.44708(18) 0.0651(8) Uani 1 1 d . . . C41 C 0.9908(3) 0.1089(2) 0.4725(2) 0.0843(11) Uani 1 1 d . . . H41A H 1.0212 0.1060 0.5246 0.101 Uiso 1 1 calc R . . C42 C 1.0068(3) 0.0601(2) 0.4213(2) 0.0857(11) Uani 1 1 d . . . H42A H 1.0468 0.0230 0.4386 0.103 Uiso 1 1 calc R . . C43 C 0.9636(2) 0.06560(17) 0.34311(19) 0.0660(8) Uani 1 1 d . . . H43A H 0.9753 0.0316 0.3090 0.079 Uiso 1 1 calc R . . C44 C 0.6235(3) -0.05085(19) 0.1566(2) 0.0815(10) Uani 1 1 d . . . H44A H 0.5941 -0.0956 0.1434 0.122 Uiso 1 1 calc R . . H44B H 0.5916 -0.0150 0.1223 0.122 Uiso 1 1 calc R . . H44C H 0.6236 -0.0390 0.2092 0.122 Uiso 1 1 calc R . . C45 C 0.7659(2) 0.00294(14) 0.16490(16) 0.0560(7) Uani 1 1 d . . . C46 C 0.8511(2) 0.00324(15) 0.14288(19) 0.0626(8) Uani 1 1 d . . . C47 C 0.8982(3) -0.04940(19) 0.1088(3) 0.0947(14) Uani 1 1 d . . . C48 C 0.9747(3) 0.05818(17) 0.1186(2) 0.0838(12) Uani 1 1 d . . . C49 C 0.9572(3) 0.1035(2) 0.0451(2) 0.1065(16) Uani 1 1 d . . . H49A H 0.8998 0.0907 0.0115 0.160 Uiso 1 1 calc R . . H49B H 1.0044 0.0956 0.0187 0.160 Uiso 1 1 calc R . . H49C H 0.9562 0.1525 0.0589 0.160 Uiso 1 1 calc R . . C50 C 1.0633(3) 0.0733(2) 0.1747(3) 0.1169(17) Uani 1 1 d . . . H50A H 1.0700 0.0433 0.2193 0.175 Uiso 1 1 calc R . . H50B H 1.0650 0.1220 0.1905 0.175 Uiso 1 1 calc R . . H50C H 1.1120 0.0644 0.1501 0.175 Uiso 1 1 calc R . . O1W O 0.5891(2) 0.1309(2) 0.05088(16) 0.1354(14) Uani 1 1 d . . . H1WA H 0.5582 0.1342 0.0847 0.163 Uiso 1 1 d R . . H1WB H 0.6418 0.1472 0.0701 0.163 Uiso 1 1 d R . . O2W O 0.0555(3) 0.3122(2) 0.4073(2) 0.1221(15) Uani 0.75 1 d P . . H2WA H 0.0728 0.3260 0.4541 0.147 Uiso 0.75 1 d PR . . H2WB H 0.0405 0.2689 0.4063 0.147 Uiso 0.75 1 d PR . . 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 0.04292(10) 0.02934(10) 0.03816(10) 0.00462(7) 0.01257(8) 0.00192(7) Ru2 0.05423(12) 0.03289(10) 0.04795(11) 0.00115(8) 0.01980(9) 0.00393(8) O1 0.0619(11) 0.0526(11) 0.0372(9) 0.0039(8) 0.0102(8) -0.0054(9) O2 0.0541(10) 0.0345(8) 0.0380(8) 0.0025(7) 0.0143(8) 0.0088(7) O3 0.0590(11) 0.0334(9) 0.0776(13) 0.0140(9) 0.0209(10) -0.0019(8) O4 0.0701(13) 0.0383(11) 0.0936(15) 0.0147(10) 0.0155(12) 0.0121(9) O5 0.0558(12) 0.0466(11) 0.0816(14) 0.0122(10) 0.0198(10) 0.0154(9) O6 0.0756(13) 0.0512(11) 0.0478(10) 0.0066(8) 0.0161(10) -0.0005(10) O7 0.0490(10) 0.0378(9) 0.0489(10) -0.0018(7) 0.0120(8) 0.0062(7) O8 0.0959(17) 0.0425(11) 0.1028(17) -0.0198(11) 0.0542(14) -0.0162(11) O9 0.196(4) 0.0502(15) 0.227(4) -0.040(2) 0.152(3) -0.0127(18) O10 0.149(3) 0.0587(15) 0.181(3) -0.0222(17) 0.125(2) -0.0005(16) N1 0.0468(11) 0.0319(10) 0.0516(12) 0.0052(9) 0.0161(10) -0.0001(9) N2 0.0459(11) 0.0310(10) 0.0429(10) 0.0006(8) 0.0128(9) 0.0001(8) N3 0.0416(11) 0.0330(10) 0.0468(11) 0.0052(8) 0.0137(9) 0.0011(8) N4 0.0405(11) 0.0387(11) 0.0423(10) 0.0066(9) 0.0102(9) 0.0067(9) N5 0.0599(14) 0.0422(12) 0.0670(14) -0.0047(11) 0.0299(12) 0.0012(11) N6 0.0468(12) 0.0429(12) 0.0567(13) 0.0052(10) 0.0137(10) 0.0060(10) N7 0.0595(13) 0.0359(11) 0.0467(11) 0.0005(9) 0.0240(10) 0.0004(9) N8 0.0696(15) 0.0415(12) 0.0675(14) -0.0018(11) 0.0374(12) 0.0041(11) C1 0.0501(15) 0.0353(13) 0.0581(15) -0.0003(11) 0.0099(12) -0.0005(11) C2 0.0574(16) 0.0460(15) 0.0504(15) -0.0021(12) 0.0061(13) 0.0003(13) C3 0.090(2) 0.076(2) 0.0567(18) -0.0097(16) 0.0050(17) -0.0078(19) C4 0.107(3) 0.085(3) 0.081(3) -0.030(2) -0.004(2) -0.017(2) C5 0.090(3) 0.067(2) 0.110(3) -0.017(2) 0.004(2) -0.028(2) C6 0.0586(18) 0.0449(16) 0.092(2) -0.0046(16) 0.0100(17) -0.0101(14) C7 0.071(2) 0.0517(18) 0.117(3) 0.0047(19) 0.042(2) -0.0187(16) C8 0.084(2) 0.0564(18) 0.090(2) 0.0103(18) 0.048(2) -0.0129(17) C9 0.0634(17) 0.0433(14) 0.0602(16) 0.0052(12) 0.0288(14) 0.0000(13) C10 0.0437(13) 0.0305(12) 0.0426(12) 0.0036(9) 0.0145(10) -0.0023(10) C11 0.0467(13) 0.0321(12) 0.0432(13) 0.0053(10) 0.0156(11) 0.0002(10) C12 0.0678(18) 0.0404(14) 0.0527(15) 0.0045(12) 0.0184(13) 0.0150(13) C13 0.0604(17) 0.0473(15) 0.0627(17) 0.0139(13) 0.0118(14) 0.0138(13) C14 0.0559(16) 0.0563(17) 0.0469(14) 0.0139(13) 0.0051(12) -0.0028(13) C15 0.0525(15) 0.0428(14) 0.0431(13) 0.0028(11) 0.0126(11) -0.0075(11) C16 0.072(2) 0.0625(18) 0.0414(14) -0.0046(13) 0.0041(14) -0.0010(16) C17 0.083(2) 0.0632(19) 0.0524(16) -0.0228(14) 0.0125(15) 0.0043(17) C18 0.0651(17) 0.0398(14) 0.0558(16) -0.0073(12) 0.0149(13) 0.0068(13) C19 0.065(2) 0.0546(18) 0.109(3) 0.0287(18) 0.0356(19) -0.0055(15) C20 0.0475(14) 0.0333(12) 0.0428(12) 0.0031(10) 0.0089(11) -0.0003(10) C21 0.0501(14) 0.0357(12) 0.0450(13) 0.0058(10) 0.0107(11) 0.0035(11) C22 0.0550(16) 0.0388(14) 0.0562(15) 0.0054(12) 0.0098(13) 0.0079(12) C23 0.0493(15) 0.0469(15) 0.0707(18) 0.0157(13) 0.0226(14) 0.0146(12) C24 0.080(2) 0.096(3) 0.083(2) 0.026(2) 0.044(2) 0.035(2) C25 0.0464(16) 0.0562(18) 0.108(3) 0.0169(18) 0.0079(17) 0.0047(14) C26 0.079(2) 0.0415(15) 0.0639(17) 0.0032(13) 0.0434(16) 0.0064(14) C27 0.084(2) 0.0479(16) 0.0520(16) 0.0029(13) 0.0352(16) 0.0072(15) C28 0.112(3) 0.067(2) 0.0544(17) 0.0108(15) 0.0350(18) 0.017(2) C29 0.146(4) 0.070(2) 0.068(2) 0.0221(19) 0.054(3) 0.019(3) C30 0.142(4) 0.055(2) 0.092(3) 0.020(2) 0.070(3) 0.005(2) C31 0.099(3) 0.0483(17) 0.088(2) -0.0023(17) 0.054(2) -0.0039(18) C32 0.113(3) 0.059(2) 0.118(3) -0.002(2) 0.057(3) -0.020(2) C33 0.077(2) 0.080(3) 0.113(3) -0.014(2) 0.034(2) -0.025(2) C34 0.065(2) 0.061(2) 0.084(2) -0.0053(16) 0.0242(18) -0.0047(15) C35 0.0509(15) 0.0435(14) 0.0496(14) 0.0010(11) 0.0143(12) -0.0060(12) C36 0.0466(14) 0.0353(13) 0.0530(15) -0.0021(11) 0.0163(12) -0.0040(11) C37 0.0676(18) 0.0421(14) 0.0652(18) -0.0077(13) 0.0258(15) -0.0066(13) C38 0.099(3) 0.0607(19) 0.0635(19) -0.0242(16) 0.0365(19) -0.0256(19) C39 0.096(3) 0.080(2) 0.0481(17) -0.0052(16) 0.0077(17) -0.020(2) C40 0.071(2) 0.0643(19) 0.0555(17) 0.0042(15) 0.0064(15) -0.0114(16) C41 0.083(3) 0.092(3) 0.064(2) 0.021(2) -0.0102(18) 0.001(2) C42 0.073(2) 0.081(3) 0.091(3) 0.026(2) -0.003(2) 0.021(2) C43 0.0632(19) 0.0549(18) 0.079(2) 0.0132(15) 0.0160(16) 0.0168(15) C44 0.091(3) 0.064(2) 0.099(3) -0.0210(19) 0.041(2) -0.0221(19) C45 0.080(2) 0.0359(14) 0.0597(16) -0.0016(12) 0.0322(15) -0.0025(13) C46 0.086(2) 0.0391(14) 0.0764(19) -0.0058(13) 0.0473(17) -0.0013(14) C47 0.129(3) 0.0485(19) 0.134(3) -0.018(2) 0.085(3) -0.001(2) C48 0.105(3) 0.0519(18) 0.121(3) -0.0110(19) 0.079(3) 0.0015(18) C49 0.159(4) 0.073(2) 0.124(3) -0.014(2) 0.107(3) -0.012(3) C50 0.076(3) 0.101(3) 0.196(5) -0.026(3) 0.075(3) 0.004(2) O1W 0.094(2) 0.245(4) 0.0729(18) -0.004(2) 0.0302(16) -0.011(2) O2W 0.148(4) 0.134(4) 0.075(2) -0.022(2) 0.007(2) -0.031(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 N4 1.9467(19) . ? Ru1 O1 2.0349(17) . ? Ru1 N3 2.0498(19) . ? Ru1 N1 2.0551(19) . ? Ru1 N2 2.056(2) . ? Ru1 O2 2.0666(16) . ? Ru2 N8 1.944(2) . ? Ru2 O6 2.0379(19) . ? Ru2 N6 2.045(2) . ? Ru2 N7 2.047(2) . ? Ru2 O7 2.0728(16) . ? Ru2 N5 2.076(2) . ? O1 C2 1.322(3) . ? O2 C11 1.316(3) . ? O3 C20 1.332(3) . ? O3 C19 1.428(4) . ? O4 C22 1.190(3) . ? O5 C22 1.381(3) . ? O5 C23 1.460(3) . ? O6 C27 1.324(3) . ? O7 C36 1.316(3) . ? O8 C45 1.332(3) . ? O8 C44 1.433(4) . ? O9 C47 1.183(4) . ? O10 C47 1.392(5) . ? O10 C48 1.447(4) . ? N1 C9 1.324(3) . ? N1 C1 1.372(3) . ? N2 C18 1.328(3) . ? N2 C10 1.378(3) . ? N3 C20 1.281(3) . ? N3 H3N 0.8600 . ? N4 C21 1.325(3) . ? N4 C23 1.495(3) . ? N5 C34 1.311(4) . ? N5 C26 1.384(4) . ? N6 C43 1.335(3) . ? N6 C35 1.380(3) . ? N7 C45 1.280(3) . ? N7 H7N 0.8600 . ? N8 C46 1.323(4) . ? N8 C48 1.498(4) . ? C1 C6 1.413(4) . ? C1 C2 1.427(4) . ? C2 C3 1.377(4) . ? C3 C4 1.398(5) . ? C3 H3A 0.9300 . ? C4 C5 1.355(6) . ? C4 H4A 0.9300 . ? C5 C6 1.415(5) . ? C5 H5A 0.9300 . ? C6 C7 1.399(5) . ? C7 C8 1.360(5) . ? C7 H7A 0.9300 . ? C8 C9 1.390(4) . ? C8 H8A 0.9300 . ? C9 H9A 0.9300 . ? C10 C15 1.402(3) . ? C10 C11 1.424(3) . ? C11 C12 1.381(3) . ? C12 C13 1.389(4) . ? C12 H12A 0.9300 . ? C13 C14 1.361(4) . ? C13 H13A 0.9300 . ? C14 C15 1.403(4) . ? C14 H14A 0.9300 . ? C15 C16 1.411(4) . ? C16 C17 1.353(4) . ? C16 H16A 0.9300 . ? C17 C18 1.399(4) . ? C17 H17A 0.9300 . ? C18 H18A 0.9300 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 C21 1.442(3) . ? C21 C22 1.437(3) . ? C23 C25 1.498(4) . ? C23 C24 1.506(4) . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 C27 1.402(4) . ? C26 C31 1.417(4) . ? C27 C28 1.387(4) . ? C28 C29 1.391(5) . ? C28 H28A 0.9300 . ? C29 C30 1.346(6) . ? C29 H29A 0.9300 . ? C30 C31 1.409(5) . ? C30 H30A 0.9300 . ? C31 C32 1.391(6) . ? C32 C33 1.344(6) . ? C32 H32A 0.9300 . ? C33 C34 1.414(5) . ? C33 H33A 0.9300 . ? C34 H34A 0.9300 . ? C35 C40 1.409(4) . ? C35 C36 1.418(4) . ? C36 C37 1.393(4) . ? C37 C38 1.406(4) . ? C37 H37A 0.9300 . ? C38 C39 1.352(5) . ? C38 H38A 0.9300 . ? C39 C40 1.407(5) . ? C39 H39A 0.9300 . ? C40 C41 1.406(5) . ? C41 C42 1.360(5) . ? C41 H41A 0.9300 . ? C42 C43 1.387(5) . ? C42 H42A 0.9300 . ? C43 H43A 0.9300 . ? C44 H44A 0.9600 . ? C44 H44B 0.9600 . ? C44 H44C 0.9600 . ? C45 C46 1.442(4) . ? C46 C47 1.442(4) . ? C48 C50 1.495(6) . ? C48 C49 1.530(5) . ? C49 H49A 0.9600 . ? C49 H49B 0.9600 . ? C49 H49C 0.9600 . ? C50 H50A 0.9600 . ? C50 H50B 0.9600 . ? C50 H50C 0.9600 . ? O1W H1WA 0.8499 . ? O1W H1WB 0.8500 . ? O2W H2WA 0.8499 . ? O2W H2WB 0.8500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N4 Ru1 O1 94.10(8) . . ? N4 Ru1 N3 77.97(8) . . ? O1 Ru1 N3 92.73(7) . . ? N4 Ru1 N1 100.36(8) . . ? O1 Ru1 N1 81.11(8) . . ? N3 Ru1 N1 173.52(8) . . ? N4 Ru1 N2 99.97(8) . . ? O1 Ru1 N2 165.82(7) . . ? N3 Ru1 N2 91.86(8) . . ? N1 Ru1 N2 94.60(8) . . ? N4 Ru1 O2 174.19(7) . . ? O1 Ru1 O2 86.22(7) . . ? N3 Ru1 O2 96.22(7) . . ? N1 Ru1 O2 85.42(7) . . ? N2 Ru1 O2 79.95(7) . . ? N8 Ru2 O6 94.06(9) . . ? N8 Ru2 N6 97.55(9) . . ? O6 Ru2 N6 168.35(8) . . ? N8 Ru2 N7 77.69(9) . . ? O6 Ru2 N7 90.54(8) . . ? N6 Ru2 N7 92.84(8) . . ? N8 Ru2 O7 173.94(8) . . ? O6 Ru2 O7 89.06(7) . . ? N6 Ru2 O7 79.47(8) . . ? N7 Ru2 O7 97.10(7) . . ? N8 Ru2 N5 102.56(9) . . ? O6 Ru2 N5 80.76(9) . . ? N6 Ru2 N5 95.73(9) . . ? N7 Ru2 N5 171.30(9) . . ? O7 Ru2 N5 83.06(8) . . ? C2 O1 Ru1 112.59(15) . . ? C11 O2 Ru1 112.85(14) . . ? C20 O3 C19 115.9(2) . . ? C22 O5 C23 110.5(2) . . ? C27 O6 Ru2 112.94(19) . . ? C36 O7 Ru2 112.87(15) . . ? C45 O8 C44 117.4(2) . . ? C47 O10 C48 110.2(2) . . ? C9 N1 C1 119.1(2) . . ? C9 N1 Ru1 129.17(19) . . ? C1 N1 Ru1 111.65(16) . . ? C18 N2 C10 118.0(2) . . ? C18 N2 Ru1 129.39(18) . . ? C10 N2 Ru1 112.56(15) . . ? C20 N3 Ru1 115.83(17) . . ? C20 N3 H3N 122.1 . . ? Ru1 N3 H3N 122.1 . . ? C21 N4 C23 107.3(2) . . ? C21 N4 Ru1 117.38(16) . . ? C23 N4 Ru1 135.14(16) . . ? C34 N5 C26 118.7(3) . . ? C34 N5 Ru2 130.3(2) . . ? C26 N5 Ru2 110.40(19) . . ? C43 N6 C35 117.9(2) . . ? C43 N6 Ru2 129.0(2) . . ? C35 N6 Ru2 113.06(17) . . ? C45 N7 Ru2 116.47(18) . . ? C45 N7 H7N 121.8 . . ? Ru2 N7 H7N 121.8 . . ? C46 N8 C48 107.6(2) . . ? C46 N8 Ru2 117.57(19) . . ? C48 N8 Ru2 134.65(19) . . ? N1 C1 C6 121.4(3) . . ? N1 C1 C2 115.7(2) . . ? C6 C1 C2 122.9(3) . . ? O1 C2 C3 124.2(3) . . ? O1 C2 C1 118.7(2) . . ? C3 C2 C1 117.1(3) . . ? C2 C3 C4 120.5(3) . . ? C2 C3 H3A 119.8 . . ? C4 C3 H3A 119.8 . . ? C5 C4 C3 122.4(3) . . ? C5 C4 H4A 118.8 . . ? C3 C4 H4A 118.8 . . ? C4 C5 C6 120.5(3) . . ? C4 C5 H5A 119.8 . . ? C6 C5 H5A 119.8 . . ? C7 C6 C1 117.0(3) . . ? C7 C6 C5 126.4(3) . . ? C1 C6 C5 116.6(3) . . ? C8 C7 C6 120.8(3) . . ? C8 C7 H7A 119.6 . . ? C6 C7 H7A 119.6 . . ? C7 C8 C9 119.1(3) . . ? C7 C8 H8A 120.4 . . ? C9 C8 H8A 120.4 . . ? N1 C9 C8 122.4(3) . . ? N1 C9 H9A 118.8 . . ? C8 C9 H9A 118.8 . . ? N2 C10 C15 123.0(2) . . ? N2 C10 C11 115.5(2) . . ? C15 C10 C11 121.5(2) . . ? O2 C11 C12 124.4(2) . . ? O2 C11 C10 118.6(2) . . ? C12 C11 C10 117.0(2) . . ? C11 C12 C13 121.3(2) . . ? C11 C12 H12A 119.3 . . ? C13 C12 H12A 119.3 . . ? C14 C13 C12 121.9(3) . . ? C14 C13 H13A 119.1 . . ? C12 C13 H13A 119.1 . . ? C13 C14 C15 119.4(2) . . ? C13 C14 H14A 120.3 . . ? C15 C14 H14A 120.3 . . ? C10 C15 C14 118.9(2) . . ? C10 C15 C16 116.5(2) . . ? C14 C15 C16 124.6(3) . . ? C17 C16 C15 120.0(3) . . ? C17 C16 H16A 120.0 . . ? C15 C16 H16A 120.0 . . ? C16 C17 C18 120.4(3) . . ? C16 C17 H17A 119.8 . . ? C18 C17 H17A 119.8 . . ? N2 C18 C17 121.8(3) . . ? N2 C18 H18A 119.1 . . ? C17 C18 H18A 119.1 . . ? O3 C19 H19A 109.5 . . ? O3 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? O3 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? N3 C20 O3 128.7(2) . . ? N3 C20 C21 114.1(2) . . ? O3 C20 C21 117.2(2) . . ? N4 C21 C22 113.1(2) . . ? N4 C21 C20 114.6(2) . . ? C22 C21 C20 132.3(2) . . ? O4 C22 O5 121.0(2) . . ? O4 C22 C21 133.7(3) . . ? O5 C22 C21 105.3(2) . . ? O5 C23 N4 103.7(2) . . ? O5 C23 C25 108.3(2) . . ? N4 C23 C25 110.7(2) . . ? O5 C23 C24 107.4(2) . . ? N4 C23 C24 111.8(2) . . ? C25 C23 C24 114.1(3) . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C23 C25 H25A 109.5 . . ? C23 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C23 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? N5 C26 C27 116.8(2) . . ? N5 C26 C31 121.6(3) . . ? C27 C26 C31 121.5(3) . . ? O6 C27 C28 122.8(3) . . ? O6 C27 C26 118.8(3) . . ? C28 C27 C26 118.4(3) . . ? C27 C28 C29 119.9(4) . . ? C27 C28 H28A 120.1 . . ? C29 C28 H28A 120.1 . . ? C30 C29 C28 122.2(4) . . ? C30 C29 H29A 118.9 . . ? C28 C29 H29A 118.9 . . ? C29 C30 C31 120.5(3) . . ? C29 C30 H30A 119.8 . . ? C31 C30 H30A 119.8 . . ? C32 C31 C30 125.7(4) . . ? C32 C31 C26 116.8(3) . . ? C30 C31 C26 117.5(4) . . ? C33 C32 C31 121.4(4) . . ? C33 C32 H32A 119.3 . . ? C31 C32 H32A 119.3 . . ? C32 C33 C34 119.1(4) . . ? C32 C33 H33A 120.5 . . ? C34 C33 H33A 120.5 . . ? N5 C34 C33 122.4(4) . . ? N5 C34 H34A 118.8 . . ? C33 C34 H34A 118.8 . . ? N6 C35 C40 122.5(3) . . ? N6 C35 C36 115.2(2) . . ? C40 C35 C36 122.3(3) . . ? O7 C36 C37 124.2(2) . . ? O7 C36 C35 118.4(2) . . ? C37 C36 C35 117.4(3) . . ? C36 C37 C38 119.7(3) . . ? C36 C37 H37A 120.1 . . ? C38 C37 H37A 120.1 . . ? C39 C38 C37 122.7(3) . . ? C39 C38 H38A 118.6 . . ? C37 C38 H38A 118.6 . . ? C38 C39 C40 119.8(3) . . ? C38 C39 H39A 120.1 . . ? C40 C39 H39A 120.1 . . ? C41 C40 C39 125.2(3) . . ? C41 C40 C35 116.8(3) . . ? C39 C40 C35 118.0(3) . . ? C42 C41 C40 120.2(3) . . ? C42 C41 H41A 119.9 . . ? C40 C41 H41A 119.9 . . ? C41 C42 C43 120.1(3) . . ? C41 C42 H42A 120.0 . . ? C43 C42 H42A 120.0 . . ? N6 C43 C42 122.5(3) . . ? N6 C43 H43A 118.8 . . ? C42 C43 H43A 118.8 . . ? O8 C44 H44A 109.5 . . ? O8 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? O8 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? N7 C45 O8 129.3(3) . . ? N7 C45 C46 113.4(3) . . ? O8 C45 C46 117.3(2) . . ? N8 C46 C45 114.7(2) . . ? N8 C46 C47 112.3(3) . . ? C45 C46 C47 133.0(3) . . ? O9 C47 O10 119.5(3) . . ? O9 C47 C46 134.9(4) . . ? O10 C47 C46 105.5(3) . . ? O10 C48 C50 108.7(3) . . ? O10 C48 N8 104.0(3) . . ? C50 C48 N8 113.4(3) . . ? O10 C48 C49 107.5(3) . . ? C50 C48 C49 113.8(4) . . ? N8 C48 C49 108.9(3) . . ? C48 C49 H49A 109.5 . . ? C48 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C48 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? C48 C50 H50A 109.5 . . ? C48 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C48 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? H1WA O1W H1WB 108.6 . . ? H2WA O2W H2WB 109.5 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 67.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.677 _refine_diff_density_min -0.445 _refine_diff_density_rms 0.048