# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/2041 #Redox and Photochemical Behaviour of Ru(II)Complexes with H2dcbpy Ligands #(H2dcbpy = 4,4'-Dicarboxylic Acid-2,2'-Bipyridine) data_global _publ_contact_author ; Tapani A. Pakkanen Department of Chemistry University of Joensuu P.O. Box 111 FIN-80101, Joensuu Finland ; _publ_contact_author_phone '358 13 2513345' _publ_contact_author_fax '358 13 2513344' _publ_contact_author_email 'tapani.pakkanen@joensuu.fi' _publ_requested_journal 'J.Chem.Soc., Dalton Transactions' _publ_requested_coeditor_name 'Dr. Claire White' _publ_section_title ; Redox and Photochemical Behaviour of Ru(II)Complexes with H2dcbpy Ligands (H2dcbpy = 4,4'-Dicarboxylic Acid-2,2'-Bipyridine) ; loop_ _publ_author_name _publ_author_address 'Esa Eskelinen' ; Department of Chemistry University of Joensuu P.O. Box 111 FIN-80101, Joensuu Finland ; 'Saija Luukkanen' ; Department of Chemistry University of Joensuu P.O. Box 111 FIN-80101, Joensuu Finland ; 'Matti Haukka' ; Department of Chemistry University of Joensuu P.O. Box 111 FIN-80101, Joensuu Finland ; 'Markku Ahlgren' ; Department of Chemistry University of Joensuu P.O. Box 111 FIN-80101, Joensuu Finland ; 'Tapani A. Pakkanen' ; Department of Chemistry University of Joensuu P.O. Box 111 FIN-80101, Joensuu Finland ; _publ_section_summary ; The electrochemical redox properties of Ru(II) complexes Ru(H2dcbpy)(CO)2Cl2 (1), Ru(H2dcbpy)2Cl2 (2), Ru(H2dcbpy)2Br2 (3), Ru(H2dcbpy)2(dcbpy) (4) and [Ru(H2dcbpy)3]2+(Cl-)2 (5) [H2dcbpy = 4,4'-dicarboxylic acid-2,2'-bipyridine; dcbpy = 4,4'-dicarboxylate-2,2'-bipyridine] were studied in CH3CN and DMSO by cyclic voltammetry. The metal-based Ru(II)/Ru(III) oxidations are observed at variable positive potentials (E1/2 = 0.15 V - 1.62 V vs. Ag+/Ag). The H2dcbpy ligands withdraw electron density from ruthenium centre and make the oxidation more difficult (seen as positive shifts at E1/2 values). At negative potentials the first irreversible ligand-based reductions (Epc = -1.37 V - -1.57 V) are due to the deprotonation of carboxylic acid groups whereas the subsequent reversible reactions at high negative potentials are assigned as bipyridine ring based reductions. Based on CV and UV-Vis studies, photoirradiation in coordinating solvent (CH3CN) revealed the tendency to the light-induced CH3CN coordination for the studied complexes 1-5. The photochemical products were also identified by using Lever's E(L) parameters. For example, under photoirradiation of 1, the principal product is Ru(H2dcbpy)(CO)(CH3CN)Cl2. The structures of 1 and 3-5 were determined by single-crystal X-ray crystallography. ; data_Ru(H2dcbpy)(CO)2Cl2.(H2O)(1) _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'Ru(H2dcbpy)(CO)2Cl2.(H2O)' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H10 Cl2 N2 O7 Ru' _chemical_formula_weight 490.21 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 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.1339(2) _cell_length_b 15.9462(5) _cell_length_c 13.3650(4) _cell_angle_alpha 90.00 _cell_angle_beta 95.520(2) _cell_angle_gamma 90.00 _cell_volume 1725.47(9) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'needle' _exptl_crystal_colour 'orange red' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.887 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 968 _exptl_absorpt_coefficient_mu 1.259 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.7869 _exptl_absorpt_correction_T_max 0.8845 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Nonius KappaCCD' _diffrn_measurement_method 'phi/omega-scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11496 _diffrn_reflns_av_R_equivalents 0.0759 _diffrn_reflns_av_sigmaI/netI 0.0628 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.32 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3028 _reflns_number_gt 2095 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius, 1998)' _computing_cell_refinement 'Denzo/Scalepack (Otwinowski & Minor, 1997)' _computing_data_reduction 'Denzo/Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP in SHELXTL v.5.1 (Bruker Axs, 1998)' _computing_publication_material 'SHELXL-97' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0271P)^2^+1.0286P] 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 3028 _refine_ls_number_parameters 247 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0763 _refine_ls_R_factor_gt 0.0380 _refine_ls_wR_factor_ref 0.0711 _refine_ls_wR_factor_gt 0.0630 _refine_ls_goodness_of_fit_ref 1.010 _refine_ls_restrained_S_all 1.010 _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 0.42639(4) 0.19187(2) 0.92689(3) 0.03348(12) Uani 1 1 d . . . Cl1 Cl 0.29745(14) 0.32800(7) 0.93712(9) 0.0493(3) Uani 1 1 d . . . Cl2 Cl 0.59149(14) 0.24575(7) 0.80477(9) 0.0552(3) Uani 1 1 d . . . C1 C 0.5992(5) 0.2294(3) 1.0268(3) 0.0295(10) Uani 1 1 d . . . O1 O 0.6979(5) 0.2510(2) 1.0751(3) 0.0673(10) Uani 1 1 d . . . C3 C 0.5296(5) 0.0876(3) 0.9170(3) 0.0336(10) Uani 1 1 d . . . O3 O 0.5985(4) 0.02779(19) 0.9092(2) 0.0495(8) Uani 1 1 d . . . N1 N 0.2299(4) 0.1541(2) 0.8206(3) 0.0340(8) Uani 1 1 d . . . N2 N 0.2527(4) 0.15067(19) 1.0208(2) 0.0313(8) Uani 1 1 d . . . C10 C 0.2330(5) 0.1511(3) 0.7210(3) 0.0408(11) Uani 1 1 d . . . H10 H 0.3285 0.1675 0.6933 0.049 Uiso 1 1 calc R . . C11 C 0.0992(5) 0.1246(3) 0.6582(3) 0.0418(11) Uani 1 1 d . . . H11 H 0.1051 0.1226 0.5891 0.050 Uiso 1 1 calc R . . C12 C -0.0429(5) 0.1010(2) 0.6982(3) 0.0368(10) Uani 1 1 d . . . C13 C -0.0468(5) 0.1048(2) 0.8016(3) 0.0357(10) Uani 1 1 d . . . H13 H -0.1426 0.0904 0.8303 0.043 Uiso 1 1 calc R . . C14 C 0.0912(5) 0.1301(2) 0.8618(3) 0.0326(10) Uani 1 1 d . . . C15 C 0.1041(5) 0.1294(2) 0.9726(3) 0.0316(9) Uani 1 1 d . . . C16 C -0.0245(5) 0.1068(3) 1.0273(3) 0.0389(11) Uani 1 1 d . . . H16 H -0.1254 0.0913 0.9938 0.047 Uiso 1 1 calc R . . C17 C -0.0054(5) 0.1067(2) 1.1309(3) 0.0355(10) Uani 1 1 d . . . C18 C 0.1459(5) 0.1287(2) 1.1789(3) 0.0382(10) Uani 1 1 d . . . H18 H 0.1627 0.1294 1.2487 0.046 Uiso 1 1 calc R . . C19 C 0.2727(5) 0.1495(2) 1.1212(3) 0.0382(10) Uani 1 1 d . . . H19 H 0.3755 0.1633 1.1536 0.046 Uiso 1 1 calc R . . C40 C -0.1912(6) 0.0688(3) 0.6346(3) 0.0434(11) Uani 1 1 d . . . O40 O -0.1668(4) 0.0646(2) 0.5398(3) 0.0687(11) Uani 1 1 d . . . O41 O -0.3193(4) 0.0514(2) 0.6690(2) 0.0663(10) Uani 1 1 d . . . C50 C -0.1520(6) 0.0823(3) 1.1853(4) 0.0427(11) Uani 1 1 d . . . O50 O -0.1237(4) 0.0896(2) 1.2824(3) 0.0591(10) Uani 1 1 d . . . O51 O -0.2787(4) 0.0581(2) 1.1413(3) 0.0717(11) Uani 1 1 d . . . O94 O -0.3985(4) 0.0497(2) 0.3859(3) 0.0552(10) Uani 1 1 d . . . H40 H -0.258(5) 0.052(3) 0.502(4) 0.060 Uiso 1 1 d . . . H50 H -0.200(5) 0.078(3) 1.307(4) 0.060 Uiso 1 1 d . . . H941 H -0.451(6) 0.005(3) 0.385(4) 0.080 Uiso 1 1 d . . . H942 H -0.445(7) 0.086(3) 0.383(5) 0.080 Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.02875(19) 0.0342(2) 0.0378(2) 0.00208(18) 0.00481(14) -0.00238(17) Cl1 0.0518(7) 0.0424(7) 0.0551(8) 0.0039(5) 0.0120(6) 0.0087(5) Cl2 0.0509(7) 0.0600(8) 0.0562(8) 0.0029(6) 0.0136(6) -0.0058(6) C1 0.025(2) 0.029(2) 0.034(3) 0.0030(19) 0.002(2) -0.0026(19) O1 0.068(2) 0.067(3) 0.068(3) -0.002(2) 0.009(2) -0.003(2) C3 0.026(2) 0.039(3) 0.035(3) 0.002(2) 0.0005(19) -0.007(2) O3 0.0439(19) 0.0407(19) 0.064(2) -0.0002(16) 0.0084(16) -0.0001(16) N1 0.0288(19) 0.038(2) 0.036(2) 0.0052(16) 0.0062(17) 0.0004(15) N2 0.0292(19) 0.0329(19) 0.032(2) 0.0030(15) 0.0029(16) 0.0013(15) C10 0.041(3) 0.048(3) 0.034(3) 0.003(2) 0.009(2) -0.005(2) C11 0.050(3) 0.046(3) 0.030(3) 0.004(2) 0.004(2) -0.005(2) C12 0.039(3) 0.038(3) 0.033(3) 0.001(2) 0.001(2) -0.001(2) C13 0.029(2) 0.040(3) 0.038(3) 0.001(2) 0.001(2) 0.0016(19) C14 0.031(2) 0.030(2) 0.037(3) 0.0028(19) 0.002(2) 0.0026(19) C15 0.031(2) 0.034(2) 0.031(2) -0.0012(19) 0.004(2) 0.0011(19) C16 0.030(2) 0.046(3) 0.040(3) -0.002(2) 0.003(2) -0.003(2) C17 0.037(3) 0.036(2) 0.034(3) 0.001(2) 0.008(2) 0.001(2) C18 0.043(3) 0.041(3) 0.032(2) 0.002(2) 0.008(2) -0.003(2) C19 0.037(2) 0.041(3) 0.035(3) -0.002(2) -0.005(2) -0.002(2) C40 0.047(3) 0.048(3) 0.035(3) -0.001(2) 0.003(2) -0.001(2) O40 0.058(2) 0.098(3) 0.049(3) -0.011(2) -0.0049(18) -0.007(2) O41 0.052(2) 0.085(3) 0.061(2) -0.0077(19) 0.0023(18) -0.0168(19) C50 0.046(3) 0.049(3) 0.034(3) 0.000(2) 0.007(2) 0.000(2) O50 0.048(2) 0.085(3) 0.046(2) 0.0040(18) 0.0135(17) -0.0037(19) O51 0.056(2) 0.106(3) 0.054(2) -0.006(2) 0.0111(19) -0.031(2) O94 0.046(2) 0.055(3) 0.064(2) -0.007(2) 0.0019(18) -0.0049(17) _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 C3 1.873(5) . ? Ru1 C1 1.937(5) . ? Ru1 N2 2.084(3) . ? Ru1 N1 2.121(3) . ? Ru1 Cl2 2.3722(11) . ? Ru1 Cl1 2.4205(11) . ? C1 O1 1.040(5) . ? C3 O3 1.116(4) . ? N1 C10 1.335(5) . ? N1 C14 1.357(5) . ? N2 C19 1.336(5) . ? N2 C15 1.357(5) . ? C10 C11 1.376(6) . ? C10 H10 0.9300 . ? C11 C12 1.372(5) . ? C11 H11 0.9300 . ? C12 C13 1.387(5) . ? C12 C40 1.498(6) . ? C13 C14 1.377(5) . ? C13 H13 0.9300 . ? C14 C15 1.474(5) . ? C15 C16 1.380(5) . ? C16 C17 1.377(5) . ? C16 H16 0.9300 . ? C17 C18 1.377(5) . ? C17 C50 1.508(5) . ? C18 C19 1.386(5) . ? C18 H18 0.9300 . ? C19 H19 0.9300 . ? C40 O41 1.211(5) . ? C40 O40 1.304(5) . ? O40 H40 0.88(5) . ? C50 O51 1.200(5) . ? C50 O50 1.300(5) . ? O50 H50 0.75(4) . ? O94 H941 0.83(5) . ? O94 H942 0.69(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C3 Ru1 C1 91.28(17) . . ? C3 Ru1 N2 95.55(14) . . ? C1 Ru1 N2 99.85(15) . . ? C3 Ru1 N1 90.86(15) . . ? C1 Ru1 N1 177.49(14) . . ? N2 Ru1 N1 78.64(12) . . ? C3 Ru1 Cl2 89.20(12) . . ? C1 Ru1 Cl2 86.62(12) . . ? N2 Ru1 Cl2 171.85(9) . . ? N1 Ru1 Cl2 94.72(9) . . ? C3 Ru1 Cl1 178.68(12) . . ? C1 Ru1 Cl1 88.49(12) . . ? N2 Ru1 Cl1 85.77(9) . . ? N1 Ru1 Cl1 89.40(9) . . ? Cl2 Ru1 Cl1 89.49(4) . . ? O1 C1 Ru1 174.9(4) . . ? O3 C3 Ru1 176.0(3) . . ? C10 N1 C14 119.4(4) . . ? C10 N1 Ru1 126.3(3) . . ? C14 N1 Ru1 114.3(3) . . ? C19 N2 C15 119.3(3) . . ? C19 N2 Ru1 125.8(3) . . ? C15 N2 Ru1 114.7(2) . . ? N1 C10 C11 122.0(4) . . ? N1 C10 H10 119.0 . . ? C11 C10 H10 119.0 . . ? C12 C11 C10 119.5(4) . . ? C12 C11 H11 120.2 . . ? C10 C11 H11 120.2 . . ? C11 C12 C13 118.5(4) . . ? C11 C12 C40 122.4(4) . . ? C13 C12 C40 119.1(4) . . ? C14 C13 C12 120.0(4) . . ? C14 C13 H13 120.0 . . ? C12 C13 H13 120.0 . . ? N1 C14 C13 120.5(4) . . ? N1 C14 C15 115.3(3) . . ? C13 C14 C15 124.1(4) . . ? N2 C15 C16 120.0(4) . . ? N2 C15 C14 116.7(3) . . ? C16 C15 C14 123.3(4) . . ? C17 C16 C15 120.9(4) . . ? C17 C16 H16 119.5 . . ? C15 C16 H16 119.5 . . ? C18 C17 C16 118.5(4) . . ? C18 C17 C50 123.6(4) . . ? C16 C17 C50 117.9(4) . . ? C17 C18 C19 118.7(4) . . ? C17 C18 H18 120.6 . . ? C19 C18 H18 120.6 . . ? N2 C19 C18 122.5(4) . . ? N2 C19 H19 118.8 . . ? C18 C19 H19 118.8 . . ? O41 C40 O40 125.1(4) . . ? O41 C40 C12 122.6(4) . . ? O40 C40 C12 112.3(4) . . ? C40 O40 H40 112(3) . . ? O51 C50 O50 125.4(4) . . ? O51 C50 C17 121.9(4) . . ? O50 C50 C17 112.7(4) . . ? C50 O50 H50 110(4) . . ? H941 O94 H942 116(6) . . ? 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 C3 Ru1 C1 O1 84(5) . . . . ? N2 Ru1 C1 O1 -180(100) . . . . ? N1 Ru1 C1 O1 -127(4) . . . . ? Cl2 Ru1 C1 O1 -5(5) . . . . ? Cl1 Ru1 C1 O1 -94(5) . . . . ? C1 Ru1 C3 O3 -63(6) . . . . ? N2 Ru1 C3 O3 -163(6) . . . . ? N1 Ru1 C3 O3 118(6) . . . . ? Cl2 Ru1 C3 O3 24(6) . . . . ? Cl1 Ru1 C3 O3 17(11) . . . . ? C3 Ru1 N1 C10 -78.4(3) . . . . ? C1 Ru1 N1 C10 133(3) . . . . ? N2 Ru1 N1 C10 -173.9(3) . . . . ? Cl2 Ru1 N1 C10 10.9(3) . . . . ? Cl1 Ru1 N1 C10 100.3(3) . . . . ? C3 Ru1 N1 C14 100.5(3) . . . . ? C1 Ru1 N1 C14 -48(3) . . . . ? N2 Ru1 N1 C14 5.1(3) . . . . ? Cl2 Ru1 N1 C14 -170.2(2) . . . . ? Cl1 Ru1 N1 C14 -80.7(2) . . . . ? C3 Ru1 N2 C19 89.3(3) . . . . ? C1 Ru1 N2 C19 -3.0(3) . . . . ? N1 Ru1 N2 C19 179.1(3) . . . . ? Cl2 Ru1 N2 C19 -145.2(5) . . . . ? Cl1 Ru1 N2 C19 -90.7(3) . . . . ? C3 Ru1 N2 C15 -95.7(3) . . . . ? C1 Ru1 N2 C15 172.0(3) . . . . ? N1 Ru1 N2 C15 -5.9(3) . . . . ? Cl2 Ru1 N2 C15 29.8(8) . . . . ? Cl1 Ru1 N2 C15 84.3(3) . . . . ? C14 N1 C10 C11 0.2(6) . . . . ? Ru1 N1 C10 C11 179.1(3) . . . . ? N1 C10 C11 C12 0.6(6) . . . . ? C10 C11 C12 C13 0.0(6) . . . . ? C10 C11 C12 C40 -178.0(4) . . . . ? C11 C12 C13 C14 -1.4(6) . . . . ? C40 C12 C13 C14 176.6(4) . . . . ? C10 N1 C14 C13 -1.7(5) . . . . ? Ru1 N1 C14 C13 179.3(3) . . . . ? C10 N1 C14 C15 175.5(3) . . . . ? Ru1 N1 C14 C15 -3.5(4) . . . . ? C12 C13 C14 N1 2.3(6) . . . . ? C12 C13 C14 C15 -174.7(4) . . . . ? C19 N2 C15 C16 -0.2(5) . . . . ? Ru1 N2 C15 C16 -175.5(3) . . . . ? C19 N2 C15 C14 -178.6(3) . . . . ? Ru1 N2 C15 C14 6.0(4) . . . . ? N1 C14 C15 N2 -1.6(5) . . . . ? C13 C14 C15 N2 175.5(4) . . . . ? N1 C14 C15 C16 180.0(4) . . . . ? C13 C14 C15 C16 -2.9(6) . . . . ? N2 C15 C16 C17 1.2(6) . . . . ? C14 C15 C16 C17 179.5(4) . . . . ? C15 C16 C17 C18 -1.0(6) . . . . ? C15 C16 C17 C50 179.3(4) . . . . ? C16 C17 C18 C19 -0.2(6) . . . . ? C50 C17 C18 C19 179.6(4) . . . . ? C15 N2 C19 C18 -1.0(6) . . . . ? Ru1 N2 C19 C18 173.8(3) . . . . ? C17 C18 C19 N2 1.2(6) . . . . ? C11 C12 C40 O41 -176.7(4) . . . . ? C13 C12 C40 O41 5.3(6) . . . . ? C11 C12 C40 O40 1.3(6) . . . . ? C13 C12 C40 O40 -176.6(4) . . . . ? C18 C17 C50 O51 -174.9(4) . . . . ? C16 C17 C50 O51 4.9(6) . . . . ? C18 C17 C50 O50 4.4(6) . . . . ? C16 C17 C50 O50 -175.8(4) . . . . ? 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 O40 H40 O94 0.88(5) 1.84(5) 2.663(5) 156(4) . _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.502 _refine_diff_density_min -0.377 _refine_diff_density_rms 0.083 #===END========================================================================= data_Ru(H2dcbpy)2(dcbpy).6(H2O)(4) _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'Ru(H2dcbpy)2(dcbpy).6(H2O)' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H34 N6 O18 Ru' _chemical_formula_weight 939.76 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ru' 'Ru' -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'Monoclinic' _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.1410(2) _cell_length_b 18.2804(6) _cell_length_c 21.0357(7) _cell_angle_alpha 90.00 _cell_angle_beta 100.998(2) _cell_angle_gamma 90.00 _cell_volume 3828.01(19) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'needle' _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.631 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1920 _exptl_absorpt_coefficient_mu 0.499 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.9067 _exptl_absorpt_correction_T_max 0.9518 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(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 'Nonius KappaCCD' _diffrn_measurement_method 'phi-scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12543 _diffrn_reflns_av_R_equivalents 0.0384 _diffrn_reflns_av_sigmaI/netI 0.0534 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 3.82 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6383 _reflns_number_gt 4694 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius, 1998)' _computing_cell_refinement 'Denzo/Scalepack (Otwinowski & Minor, 1997)' _computing_data_reduction 'Denzo/Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP in SHELXTL v.5.1 (Bruker Axs, 1998)' _computing_publication_material 'SHELXL-97' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0296P)^2^+15.8284P] 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 6383 _refine_ls_number_parameters 562 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0735 _refine_ls_R_factor_gt 0.0458 _refine_ls_wR_factor_ref 0.1229 _refine_ls_wR_factor_gt 0.1069 _refine_ls_goodness_of_fit_ref 1.076 _refine_ls_restrained_S_all 1.076 _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 0.02072(4) 0.24686(2) 0.441764(17) 0.02024(12) Uani 1 1 d . . . O40 O 0.4129(4) 0.0739(3) 0.2502(2) 0.0467(11) Uani 1 1 d . . . O41 O 0.2628(4) 0.1237(3) 0.16970(18) 0.0504(12) Uani 1 1 d . . . O50 O -0.3740(5) 0.4205(3) 0.1805(2) 0.0611(14) Uani 1 1 d . . . O51 O -0.2403(4) 0.3617(2) 0.12487(18) 0.0396(9) Uani 1 1 d . . . O60 O 0.3310(4) 0.5832(2) 0.53111(19) 0.0344(10) Uani 1 1 d . . . O61 O 0.4236(3) 0.55919(19) 0.44494(17) 0.0308(8) Uani 1 1 d . . . O70 O -0.1109(4) 0.4721(2) 0.6858(2) 0.0443(10) Uani 1 1 d . . . O71 O -0.2107(4) 0.3721(2) 0.71583(19) 0.0474(11) Uani 1 1 d . . . O80 O 0.1187(4) 0.0256(2) 0.7097(2) 0.0533(12) Uani 1 1 d . . . O81 O 0.2988(4) 0.0935(2) 0.74661(18) 0.0418(10) Uani 1 1 d . . . O90 O -0.3471(4) -0.0684(2) 0.48280(18) 0.0374(9) Uani 1 1 d . . . O91 O -0.5004(4) -0.0084(2) 0.4116(2) 0.0421(10) Uani 1 1 d . . . N1 N 0.1148(4) 0.1986(2) 0.37471(19) 0.0217(9) Uani 1 1 d . . . N2 N -0.0725(4) 0.2971(2) 0.35832(19) 0.0229(9) Uani 1 1 d . . . N3 N 0.1442(4) 0.3373(2) 0.45773(18) 0.0222(9) Uani 1 1 d . . . N4 N -0.0631(4) 0.3031(2) 0.50955(18) 0.0209(8) Uani 1 1 d . . . N5 N 0.1050(4) 0.1881(2) 0.52266(19) 0.0224(9) Uani 1 1 d . . . N6 N -0.1085(4) 0.1590(2) 0.43460(18) 0.0240(9) Uani 1 1 d . . . C40 C 0.3045(5) 0.1123(3) 0.2266(3) 0.0344(13) Uani 1 1 d . . . C50 C -0.2719(6) 0.3795(3) 0.1744(3) 0.0353(13) Uani 1 1 d . . . C60 C 0.3514(5) 0.5426(3) 0.4857(2) 0.0261(11) Uani 1 1 d . . . C70 C -0.1530(5) 0.4065(3) 0.6785(3) 0.0312(12) Uani 1 1 d . . . C80 C 0.2007(5) 0.0760(3) 0.7053(2) 0.0316(12) Uani 1 1 d . . . C90 C -0.3855(5) -0.0160(3) 0.4451(3) 0.0326(12) Uani 1 1 d . . . C10 C 0.2106(5) 0.1479(3) 0.3886(2) 0.0282(11) Uani 1 1 d . . . H10 H 0.2345 0.1309 0.4320 0.034 Uiso 1 1 calc R . . C11 C 0.2767(5) 0.1189(3) 0.3425(3) 0.0306(12) Uani 1 1 d . . . H11 H 0.3467 0.0841 0.3542 0.037 Uiso 1 1 calc R . . C12 C 0.2380(5) 0.1420(3) 0.2786(2) 0.0256(11) Uani 1 1 d . . . C13 C 0.1352(5) 0.1931(3) 0.2632(2) 0.0259(11) Uani 1 1 d . . . H13 H 0.1062 0.2089 0.2198 0.031 Uiso 1 1 calc R . . C14 C 0.0758(5) 0.2206(3) 0.3125(2) 0.0224(10) Uani 1 1 d . . . C15 C -0.0318(5) 0.2763(3) 0.3031(2) 0.0226(10) Uani 1 1 d . . . C16 C -0.0928(5) 0.3039(3) 0.2434(2) 0.0256(11) Uani 1 1 d . . . H16 H -0.0634 0.2890 0.2052 0.031 Uiso 1 1 calc R . . C18 C -0.2367(5) 0.3757(3) 0.2969(2) 0.0312(12) Uani 1 1 d . . . H18 H -0.3074 0.4100 0.2961 0.037 Uiso 1 1 calc R . . C19 C -0.1707(5) 0.3468(3) 0.3549(2) 0.0285(11) Uani 1 1 d . . . H19 H -0.1959 0.3627 0.3939 0.034 Uiso 1 1 calc R . . C20 C 0.2435(5) 0.3526(3) 0.4264(2) 0.0260(11) Uani 1 1 d . . . H20 H 0.2674 0.3170 0.3976 0.031 Uiso 1 1 calc R . . C21 C 0.3134(5) 0.4183(3) 0.4341(2) 0.0265(11) Uani 1 1 d . . . H21 H 0.3823 0.4280 0.4103 0.032 Uiso 1 1 calc R . . C22 C 0.2806(5) 0.4697(3) 0.4773(2) 0.0225(10) Uani 1 1 d . . . C23 C 0.1815(5) 0.4530(3) 0.5116(2) 0.0247(11) Uani 1 1 d . . . H23 H 0.1597 0.4867 0.5424 0.030 Uiso 1 1 calc R . . C24 C 0.1131(5) 0.3865(3) 0.5010(2) 0.0206(10) Uani 1 1 d . . . C25 C 0.0046(4) 0.3639(3) 0.5337(2) 0.0200(10) Uani 1 1 d . . . C26 C -0.0268(5) 0.3997(3) 0.5872(2) 0.0241(11) Uani 1 1 d . . . H26 H 0.0186 0.4436 0.6024 0.029 Uiso 1 1 calc R . . C27 C -0.1239(5) 0.3715(3) 0.6184(2) 0.0257(11) Uani 1 1 d . . . C28 C -0.1911(5) 0.3084(3) 0.5937(2) 0.0253(11) Uani 1 1 d . . . H28 H -0.2573 0.2871 0.6144 0.030 Uiso 1 1 calc R . . C29 C -0.1599(5) 0.2770(3) 0.5384(2) 0.0245(11) Uani 1 1 d . . . H29 H -0.2093 0.2353 0.5203 0.029 Uiso 1 1 calc R . . C30 C 0.2113(5) 0.2082(3) 0.5672(2) 0.0290(12) Uani 1 1 d . . . H30 H 0.2641 0.2482 0.5578 0.035 Uiso 1 1 calc R . . C31 C 0.2480(5) 0.1733(3) 0.6265(2) 0.0312(12) Uani 1 1 d . . . H31 H 0.3247 0.1890 0.6567 0.037 Uiso 1 1 calc R . . C32 C 0.1714(5) 0.1156(3) 0.6408(2) 0.0263(11) Uani 1 1 d . . . C33 C 0.0620(5) 0.0936(3) 0.5948(2) 0.0242(11) Uani 1 1 d . . . H33 H 0.0090 0.0533 0.6034 0.029 Uiso 1 1 calc R . . C34 C 0.0298(5) 0.1301(3) 0.5365(2) 0.0216(10) Uani 1 1 d . . . C35 C -0.0875(5) 0.1124(3) 0.4858(2) 0.0230(10) Uani 1 1 d . . . C36 C -0.1741(5) 0.0542(3) 0.4903(2) 0.0227(10) Uani 1 1 d . . . H36 H -0.1572 0.0221 0.5264 0.027 Uiso 1 1 calc R . . C37 C -0.2855(5) 0.0440(3) 0.4413(2) 0.0250(11) Uani 1 1 d . . . C38 C -0.3045(5) 0.0912(3) 0.3878(3) 0.0298(12) Uani 1 1 d . . . H38 H -0.3788 0.0849 0.3532 0.036 Uiso 1 1 calc R . . C39 C -0.2133(5) 0.1470(3) 0.3863(2) 0.0284(11) Uani 1 1 d . . . H39 H -0.2253 0.1781 0.3495 0.034 Uiso 1 1 calc R . . C17 C -0.1989(5) 0.3543(3) 0.2401(2) 0.0294(12) Uani 1 1 d . . . O94 O 0.5244(4) -0.0013(2) 0.17440(19) 0.0438(10) Uani 1 1 d . . . O95 O 0.4406(4) 0.7189(2) 0.5717(2) 0.0544(12) Uani 1 1 d . . . O96 O -0.5374(4) -0.1741(3) 0.4825(2) 0.0541(12) Uani 1 1 d . . . O97 O 0.4501(5) 0.2174(3) 0.7967(3) 0.0749(16) Uani 1 1 d . . . O98 O 0.5456(6) 0.6832(4) 0.4194(4) 0.115(3) Uani 1 1 d . . . O99 O -0.4240(5) 0.2718(3) 0.7005(3) 0.0782(16) Uani 1 1 d . . . H40 H 0.446(7) 0.039(4) 0.224(3) 0.060 Uiso 1 1 d . . . H50 H -0.422(7) 0.438(4) 0.132(3) 0.060 Uiso 1 1 d . . . H60 H 0.327(8) 0.560(4) 0.556(4) 0.060 Uiso 1 1 d . . . H70 H -0.117(7) 0.493(4) 0.724(4) 0.060 Uiso 1 1 d . . . H941 H 0.5464 0.0134 0.1376 0.080 Uiso 1 1 d . . . H942 H 0.5975 -0.0260 0.1998 0.080 Uiso 1 1 d . . . H951 H 0.4230 0.6882 0.5536 0.080 Uiso 1 1 d . . . H952 H 0.4701 0.7260 0.6040 0.080 Uiso 1 1 d . . . H961 H -0.5138 -0.1394 0.4811 0.080 Uiso 1 1 d . . . H962 H -0.5046 -0.1967 0.4708 0.080 Uiso 1 1 d . . . H971 H 0.4231 0.1652 0.7805 0.080 Uiso 1 1 d . . . H972 H 0.4372 0.2547 0.7740 0.080 Uiso 1 1 d . . . H981 H 0.5023 0.6611 0.4408 0.080 Uiso 1 1 d . . . H982 H 0.5693 0.6552 0.4071 0.080 Uiso 1 1 d . . . H991 H -0.3626 0.3036 0.7114 0.080 Uiso 1 1 d . . . H992 H -0.4891 0.2640 0.6637 0.080 Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.0219(2) 0.0204(2) 0.01828(19) 0.00106(18) 0.00324(13) 0.00003(16) O40 0.047(3) 0.059(3) 0.036(2) 0.003(2) 0.0143(18) 0.029(2) O41 0.043(3) 0.084(3) 0.024(2) -0.004(2) 0.0057(17) 0.021(2) O50 0.063(3) 0.076(3) 0.041(3) 0.009(2) 0.002(2) 0.043(3) O51 0.048(2) 0.045(2) 0.025(2) 0.0052(18) 0.0042(17) 0.0117(18) O60 0.037(2) 0.031(2) 0.036(2) -0.0041(18) 0.0089(18) -0.0031(17) O61 0.030(2) 0.027(2) 0.037(2) 0.0048(16) 0.0113(16) -0.0039(15) O70 0.062(3) 0.041(3) 0.034(2) -0.0163(19) 0.018(2) -0.001(2) O71 0.054(3) 0.060(3) 0.035(2) -0.012(2) 0.024(2) -0.016(2) O80 0.062(3) 0.057(3) 0.034(2) 0.022(2) -0.0078(19) -0.025(2) O81 0.044(2) 0.047(3) 0.028(2) 0.0086(18) -0.0064(17) -0.0095(18) O90 0.033(2) 0.038(2) 0.038(2) 0.0152(19) -0.0034(16) -0.0067(16) O91 0.033(2) 0.034(2) 0.051(3) 0.0011(19) -0.0141(18) -0.0039(16) N1 0.025(2) 0.019(2) 0.021(2) 0.0033(17) 0.0019(16) 0.0001(16) N2 0.024(2) 0.020(2) 0.024(2) -0.0016(17) 0.0043(16) 0.0015(16) N3 0.022(2) 0.024(2) 0.019(2) 0.0044(17) 0.0028(16) 0.0031(16) N4 0.024(2) 0.019(2) 0.019(2) 0.0032(17) 0.0036(16) -0.0018(16) N5 0.022(2) 0.021(2) 0.024(2) 0.0008(17) 0.0041(16) -0.0027(16) N6 0.028(2) 0.026(2) 0.017(2) -0.0018(17) 0.0014(16) 0.0028(17) C40 0.027(3) 0.044(3) 0.031(3) -0.002(3) 0.003(2) 0.010(2) C50 0.038(3) 0.032(3) 0.035(3) 0.001(3) 0.002(2) 0.014(2) C60 0.022(3) 0.029(3) 0.026(3) 0.003(2) 0.000(2) 0.002(2) C70 0.026(3) 0.040(3) 0.028(3) -0.006(2) 0.007(2) 0.001(2) C80 0.036(3) 0.036(3) 0.022(3) 0.004(2) 0.003(2) -0.004(2) C90 0.030(3) 0.033(3) 0.034(3) -0.009(3) 0.002(2) -0.001(2) C10 0.032(3) 0.031(3) 0.022(3) 0.005(2) 0.002(2) 0.004(2) C11 0.028(3) 0.031(3) 0.033(3) 0.003(2) 0.007(2) 0.010(2) C12 0.029(3) 0.026(3) 0.023(3) 0.000(2) 0.006(2) 0.003(2) C13 0.026(3) 0.031(3) 0.020(3) -0.001(2) 0.0029(19) 0.001(2) C14 0.019(3) 0.023(2) 0.024(3) 0.001(2) 0.0031(19) 0.0002(18) C15 0.021(3) 0.021(2) 0.027(3) 0.004(2) 0.0054(19) 0.0000(18) C16 0.028(3) 0.027(3) 0.022(3) 0.001(2) 0.004(2) 0.007(2) C18 0.037(3) 0.029(3) 0.027(3) 0.004(2) 0.004(2) 0.012(2) C19 0.032(3) 0.026(3) 0.028(3) 0.000(2) 0.007(2) 0.005(2) C20 0.028(3) 0.026(3) 0.025(3) -0.002(2) 0.008(2) 0.000(2) C21 0.029(3) 0.027(3) 0.027(3) 0.000(2) 0.012(2) -0.002(2) C22 0.024(3) 0.022(3) 0.020(2) 0.004(2) 0.0003(19) 0.0003(19) C23 0.024(3) 0.025(3) 0.025(3) -0.003(2) 0.0047(19) 0.0022(19) C24 0.020(3) 0.020(2) 0.021(2) 0.000(2) 0.0039(18) 0.0022(18) C25 0.021(3) 0.020(3) 0.018(2) 0.001(2) 0.0030(18) 0.0012(19) C26 0.028(3) 0.021(3) 0.022(3) 0.001(2) 0.003(2) 0.0002(19) C27 0.026(3) 0.029(3) 0.022(3) 0.002(2) 0.0045(19) 0.003(2) C28 0.023(3) 0.029(3) 0.026(3) 0.002(2) 0.0084(19) 0.002(2) C29 0.024(3) 0.022(2) 0.028(3) 0.004(2) 0.005(2) -0.0013(19) C30 0.030(3) 0.027(3) 0.028(3) 0.002(2) 0.001(2) -0.006(2) C31 0.029(3) 0.035(3) 0.026(3) 0.005(2) -0.003(2) -0.004(2) C32 0.027(3) 0.027(3) 0.023(3) 0.004(2) 0.001(2) 0.004(2) C33 0.027(3) 0.023(3) 0.022(3) 0.001(2) 0.0020(19) -0.0010(19) C34 0.023(3) 0.020(3) 0.022(3) 0.002(2) 0.0045(19) 0.0017(19) C35 0.024(3) 0.020(3) 0.025(3) 0.001(2) 0.0030(19) 0.0021(19) C36 0.026(3) 0.017(2) 0.024(3) 0.002(2) 0.0045(19) -0.0007(19) C37 0.024(3) 0.023(3) 0.026(3) -0.004(2) 0.001(2) 0.0010(19) C38 0.029(3) 0.029(3) 0.029(3) 0.002(2) -0.002(2) -0.002(2) C39 0.034(3) 0.026(3) 0.022(3) 0.004(2) -0.001(2) 0.002(2) C17 0.032(3) 0.025(3) 0.031(3) 0.003(2) 0.005(2) 0.007(2) O94 0.045(3) 0.053(3) 0.036(2) 0.0036(19) 0.0139(18) 0.0158(19) O95 0.038(3) 0.052(3) 0.068(3) 0.005(2) -0.003(2) -0.0014(19) O96 0.043(3) 0.057(3) 0.058(3) 0.005(2) 0.000(2) -0.011(2) O97 0.053(3) 0.050(3) 0.118(5) -0.013(3) 0.006(3) -0.001(2) O98 0.087(5) 0.098(5) 0.135(6) 0.043(4) -0.043(4) -0.059(4) O99 0.052(3) 0.079(4) 0.100(4) 0.000(3) 0.007(3) -0.016(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 N2 2.045(4) . ? Ru1 N1 2.047(4) . ? Ru1 N5 2.056(4) . ? Ru1 N6 2.060(4) . ? Ru1 N3 2.062(4) . ? Ru1 N4 2.067(4) . ? O40 C40 1.319(6) . ? O40 H40 0.94(7) . ? O41 C40 1.209(6) . ? O50 C50 1.305(6) . ? O50 H50 1.10(7) . ? O51 C50 1.193(6) . ? O60 C60 1.259(6) . ? O60 H60 0.68(7) . ? O61 C60 1.266(6) . ? O70 C70 1.272(7) . ? O70 H70 0.90(7) . ? O71 C70 1.237(7) . ? O80 C80 1.258(6) . ? O81 C80 1.232(6) . ? O90 C90 1.258(7) . ? O91 C90 1.249(6) . ? N1 C10 1.335(6) . ? N1 C14 1.355(6) . ? N2 C19 1.340(6) . ? N2 C15 1.359(6) . ? N3 C20 1.334(6) . ? N3 C24 1.359(6) . ? N4 C29 1.337(6) . ? N4 C25 1.354(6) . ? N5 C30 1.339(6) . ? N5 C34 1.368(6) . ? N6 C39 1.341(6) . ? N6 C35 1.357(6) . ? C40 C12 1.492(7) . ? C50 C17 1.508(7) . ? C60 C22 1.507(7) . ? C60 H60 1.57(8) . ? C70 C27 1.497(7) . ? C80 C32 1.515(7) . ? C90 C37 1.506(7) . ? C10 C11 1.386(7) . ? C10 H10 0.9500 . ? C11 C12 1.391(7) . ? C11 H11 0.9500 . ? C12 C13 1.392(7) . ? C13 C14 1.388(7) . ? C13 H13 0.9500 . ? C14 C15 1.478(6) . ? C15 C16 1.383(7) . ? C16 C17 1.408(7) . ? C16 H16 0.9500 . ? C18 C19 1.380(7) . ? C18 C17 1.380(7) . ? C18 H18 0.9500 . ? C19 H19 0.9500 . ? C20 C21 1.390(7) . ? C20 H20 0.9500 . ? C21 C22 1.391(7) . ? C21 H21 0.9500 . ? C22 C23 1.378(7) . ? C23 C24 1.397(7) . ? C23 H23 0.9500 . ? C24 C25 1.464(6) . ? C25 C26 1.391(7) . ? C26 C27 1.383(7) . ? C26 H26 0.9500 . ? C27 C28 1.390(7) . ? C28 C29 1.386(7) . ? C28 H28 0.9500 . ? C29 H29 0.9500 . ? C30 C31 1.386(7) . ? C30 H30 0.9500 . ? C31 C32 1.378(7) . ? C31 H31 0.9500 . ? C32 C33 1.385(7) . ? C33 C34 1.380(7) . ? C33 H33 0.9500 . ? C34 C35 1.474(6) . ? C35 C36 1.395(7) . ? C36 C37 1.388(7) . ? C36 H36 0.9500 . ? C37 C38 1.403(7) . ? C38 C39 1.381(7) . ? C38 H38 0.9500 . ? C39 H39 0.9500 . ? O94 H941 0.8865 . ? O94 H942 0.9431 . ? O95 H951 0.6825 . ? O95 H952 0.6991 . ? O96 H961 0.6810 . ? O96 H962 0.6102 . ? O97 H971 1.0329 . ? O97 H972 0.8287 . ? O98 H981 0.7956 . ? O98 H982 0.6415 . ? O99 H991 0.8504 . ? O99 H992 0.9271 . ? 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 N1 78.55(15) . . ? N2 Ru1 N5 174.85(15) . . ? N1 Ru1 N5 99.82(15) . . ? N2 Ru1 N6 95.94(15) . . ? N1 Ru1 N6 89.28(15) . . ? N5 Ru1 N6 79.11(15) . . ? N2 Ru1 N3 86.96(15) . . ? N1 Ru1 N3 96.26(15) . . ? N5 Ru1 N3 98.09(15) . . ? N6 Ru1 N3 174.17(15) . . ? N2 Ru1 N4 100.69(15) . . ? N1 Ru1 N4 175.07(15) . . ? N5 Ru1 N4 81.34(15) . . ? N6 Ru1 N4 95.64(15) . . ? N3 Ru1 N4 78.82(15) . . ? C40 O40 H40 121(4) . . ? C50 O50 H50 108(3) . . ? C60 O60 H60 105(7) . . ? C70 O70 H70 115(4) . . ? C10 N1 C14 119.0(4) . . ? C10 N1 Ru1 124.3(3) . . ? C14 N1 Ru1 116.7(3) . . ? C19 N2 C15 119.1(4) . . ? C19 N2 Ru1 124.6(3) . . ? C15 N2 Ru1 116.3(3) . . ? C20 N3 C24 119.1(4) . . ? C20 N3 Ru1 125.4(3) . . ? C24 N3 Ru1 115.4(3) . . ? C29 N4 C25 119.1(4) . . ? C29 N4 Ru1 124.8(3) . . ? C25 N4 Ru1 114.9(3) . . ? C30 N5 C34 118.1(4) . . ? C30 N5 Ru1 126.0(3) . . ? C34 N5 Ru1 114.9(3) . . ? C39 N6 C35 118.7(4) . . ? C39 N6 Ru1 125.8(3) . . ? C35 N6 Ru1 115.4(3) . . ? O41 C40 O40 125.1(5) . . ? O41 C40 C12 122.7(5) . . ? O40 C40 C12 112.2(5) . . ? O51 C50 O50 126.4(5) . . ? O51 C50 C17 123.4(5) . . ? O50 C50 C17 110.2(5) . . ? O60 C60 O61 124.9(5) . . ? O60 C60 C22 117.8(4) . . ? O61 C60 C22 117.2(4) . . ? O60 C60 H60 25(3) . . ? O61 C60 H60 143(3) . . ? C22 C60 H60 98(3) . . ? O71 C70 O70 126.3(5) . . ? O71 C70 C27 120.8(5) . . ? O70 C70 C27 112.9(5) . . ? O81 C80 O80 126.5(5) . . ? O81 C80 C32 120.1(5) . . ? O80 C80 C32 113.3(4) . . ? O91 C90 O90 125.8(5) . . ? O91 C90 C37 117.1(5) . . ? O90 C90 C37 117.2(4) . . ? N1 C10 C11 122.7(5) . . ? N1 C10 H10 118.6 . . ? C11 C10 H10 118.6 . . ? C10 C11 C12 118.4(5) . . ? C10 C11 H11 120.8 . . ? C12 C11 H11 120.8 . . ? C11 C12 C13 119.3(4) . . ? C11 C12 C40 121.0(4) . . ? C13 C12 C40 119.8(4) . . ? C14 C13 C12 118.8(4) . . ? C14 C13 H13 120.6 . . ? C12 C13 H13 120.6 . . ? N1 C14 C13 121.7(4) . . ? N1 C14 C15 113.9(4) . . ? C13 C14 C15 124.3(4) . . ? N2 C15 C16 121.2(4) . . ? N2 C15 C14 114.5(4) . . ? C16 C15 C14 124.3(4) . . ? C15 C16 C17 119.3(5) . . ? C15 C16 H16 120.4 . . ? C17 C16 H16 120.4 . . ? C19 C18 C17 119.3(5) . . ? C19 C18 H18 120.3 . . ? C17 C18 H18 120.3 . . ? N2 C19 C18 122.5(5) . . ? N2 C19 H19 118.7 . . ? C18 C19 H19 118.7 . . ? N3 C20 C21 122.7(5) . . ? N3 C20 H20 118.7 . . ? C21 C20 H20 118.7 . . ? C20 C21 C22 118.7(5) . . ? C20 C21 H21 120.7 . . ? C22 C21 H21 120.7 . . ? C23 C22 C21 118.8(4) . . ? C23 C22 C60 120.9(4) . . ? C21 C22 C60 120.3(4) . . ? C22 C23 C24 119.9(4) . . ? C22 C23 H23 120.1 . . ? C24 C23 H23 120.1 . . ? N3 C24 C23 120.8(4) . . ? N3 C24 C25 114.8(4) . . ? C23 C24 C25 124.4(4) . . ? N4 C25 C26 120.8(4) . . ? N4 C25 C24 115.4(4) . . ? C26 C25 C24 123.8(4) . . ? C27 C26 C25 120.1(5) . . ? C27 C26 H26 119.9 . . ? C25 C26 H26 119.9 . . ? C26 C27 C28 118.4(5) . . ? C26 C27 C70 121.0(5) . . ? C28 C27 C70 120.6(5) . . ? C29 C28 C27 118.9(5) . . ? C29 C28 H28 120.5 . . ? C27 C28 H28 120.5 . . ? N4 C29 C28 122.5(5) . . ? N4 C29 H29 118.7 . . ? C28 C29 H29 118.7 . . ? N5 C30 C31 123.1(5) . . ? N5 C30 H30 118.5 . . ? C31 C30 H30 118.5 . . ? C32 C31 C30 118.9(5) . . ? C32 C31 H31 120.5 . . ? C30 C31 H31 120.5 . . ? C31 C32 C33 118.6(5) . . ? C31 C32 C80 122.6(5) . . ? C33 C32 C80 118.8(4) . . ? C34 C33 C32 120.3(5) . . ? C34 C33 H33 119.9 . . ? C32 C33 H33 119.9 . . ? N5 C34 C33 121.1(4) . . ? N5 C34 C35 114.9(4) . . ? C33 C34 C35 124.0(4) . . ? N6 C35 C36 121.8(4) . . ? N6 C35 C34 114.8(4) . . ? C36 C35 C34 123.3(4) . . ? C37 C36 C35 119.1(4) . . ? C37 C36 H36 120.5 . . ? C35 C36 H36 120.5 . . ? C36 C37 C38 118.7(4) . . ? C36 C37 C90 121.4(4) . . ? C38 C37 C90 119.9(4) . . ? C39 C38 C37 118.9(5) . . ? C39 C38 H38 120.6 . . ? C37 C38 H38 120.6 . . ? N6 C39 C38 122.7(5) . . ? N6 C39 H39 118.6 . . ? C38 C39 H39 118.6 . . ? C18 C17 C16 118.5(5) . . ? C18 C17 C50 122.5(5) . . ? C16 C17 C50 118.8(5) . . ? H941 O94 H942 109.8 . . ? H951 O95 H952 135.6 . . ? H961 O96 H962 112.9 . . ? H971 O97 H972 124.5 . . ? H981 O98 H982 96.4 . . ? H991 O99 H992 134.4 . . ? 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 O40 H40 O94 0.94(7) 1.61(7) 2.531(5) 165(6) . O50 H50 O91 1.10(7) 1.46(7) 2.474(6) 151(6) 2_455 O70 H70 O80 0.90(7) 1.52(7) 2.420(5) 176(7) 2_556 O95 H951 O60 0.68 2.15 2.785(6) 156.0 . O96 H961 O90 0.68 2.13 2.730(5) 148.5 . O99 H991 O71 0.85 1.97 2.807(6) 166.1 . O97 H971 O81 1.03 1.86 2.824(6) 153.3 . O98 H981 O61 0.80 2.04 2.686(6) 138.8 . _diffrn_measured_fraction_theta_max 0.949 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.949 _refine_diff_density_max 0.410 _refine_diff_density_min -0.565 _refine_diff_density_rms 0.090 #===END========================================================================= data_(Ru(H2dcbpy))Cl2.2 #(5) _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '(Ru(H2dcbpy))Cl2.2 3/4H2O' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H29.50 Cl2 N6 O14.75 Ru' _chemical_formula_weight 954.13 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 'C 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' _cell_length_a 22.1485(3) _cell_length_b 18.7892(3) _cell_length_c 21.4865(2) _cell_angle_alpha 90.00 _cell_angle_beta 118.5930(10) _cell_angle_gamma 90.00 _cell_volume 7851.15(18) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'block' _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.614 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3868 _exptl_absorpt_coefficient_mu 0.614 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.3141 _exptl_absorpt_correction_T_max 0.3599 _exptl_absorpt_process_details 'Xprep in Shelxtl v. 5.1 (Bruker AXS, 1998)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Nonius KappaCCD' _diffrn_measurement_method 'phi-scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 51929 _diffrn_reflns_av_R_equivalents 0.0290 _diffrn_reflns_av_sigmaI/netI 0.0346 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.13 _diffrn_reflns_theta_max 27.49 _reflns_number_total 17064 _reflns_number_gt 16504 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius, 1999)' _computing_cell_refinement 'Denzo/Scalepack (Otwinowski & Minor, 1997)' _computing_data_reduction 'Denzo/Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP in SHELXTL v.5.1 (Bruker Axs, 1998)' _computing_publication_material 'SHELXL-97' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0281P)^2^+8.1223P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.272(11) _refine_ls_number_reflns 17064 _refine_ls_number_parameters 1082 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0265 _refine_ls_R_factor_gt 0.0249 _refine_ls_wR_factor_ref 0.0634 _refine_ls_wR_factor_gt 0.0624 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.041 _refine_ls_shift/su_max 0.013 _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 0.896205(8) 0.977180(9) 0.510931(8) 0.01224(4) Uani 1 1 d . . . N1 N 0.84410(11) 0.99839(11) 0.40383(12) 0.0148(4) Uani 1 1 d . . . N2 N 0.94354(11) 1.07025(10) 0.50523(11) 0.0145(4) Uani 1 1 d . . . N6 N 0.95015(10) 0.90538(10) 0.48471(11) 0.0128(4) Uani 1 1 d . . . N5 N 0.84764(11) 0.88356(10) 0.50932(11) 0.0142(4) Uani 1 1 d . . . N4 N 0.94800(11) 0.96004(11) 0.61852(11) 0.0145(4) Uani 1 1 d . . . N3 N 0.84202(11) 1.04148(10) 0.54436(11) 0.0151(4) Uani 1 1 d . . . C10 C 0.79668(13) 0.95570(13) 0.35451(13) 0.0181(5) Uani 1 1 d . . . H10 H 0.7831 0.9141 0.3697 0.022 Uiso 1 1 calc R . . C11 C 0.76681(15) 0.96949(14) 0.28288(15) 0.0209(5) Uani 1 1 d . . . H11 H 0.7326 0.9386 0.2496 0.025 Uiso 1 1 calc R . . C12 C 0.78754(13) 1.02928(13) 0.26022(13) 0.0177(5) Uani 1 1 d . . . C13 C 0.83819(14) 1.07276(13) 0.31066(14) 0.0201(5) Uani 1 1 d . . . H13 H 0.8541 1.1132 0.2963 0.024 Uiso 1 1 calc R . . C14 C 0.91877(13) 1.09895(12) 0.43914(13) 0.0160(5) Uani 1 1 d . . . C15 C 0.86538(13) 1.05659(12) 0.38226(13) 0.0157(5) Uani 1 1 d . . . C16 C 0.94339(14) 1.16239(13) 0.42788(14) 0.0199(5) Uani 1 1 d . . . H16 H 0.9252 1.1810 0.3813 0.024 Uiso 1 1 calc R . . C17 C 0.99487(14) 1.19904(13) 0.48476(14) 0.0201(5) Uani 1 1 d . . . C18 C 1.01910(14) 1.17075(13) 0.55257(14) 0.0224(5) Uani 1 1 d . . . H18 H 1.0534 1.1950 0.5928 0.027 Uiso 1 1 calc R . . C19 C 0.99234(13) 1.10649(13) 0.56050(14) 0.0184(5) Uani 1 1 d . . . H19 H 1.0092 1.0874 0.6068 0.022 Uiso 1 1 calc R . . C39 C 0.99948(13) 0.92261(12) 0.46739(13) 0.0162(5) Uani 1 1 d . . . H39 H 1.0114 0.9713 0.4681 0.019 Uiso 1 1 calc R . . C38 C 1.03319(13) 0.87201(13) 0.44868(13) 0.0166(5) Uani 1 1 d . . . H38 H 1.0668 0.8859 0.4355 0.020 Uiso 1 1 calc R . . C37 C 1.01742(13) 0.80137(13) 0.44935(13) 0.0156(5) Uani 1 1 d . . . C36 C 0.96488(13) 0.78272(13) 0.46463(13) 0.0155(5) Uani 1 1 d . . . H36 H 0.9521 0.7343 0.4637 0.019 Uiso 1 1 calc R . . C35 C 0.93180(13) 0.83579(12) 0.48104(12) 0.0139(5) Uani 1 1 d . . . C34 C 0.87428(12) 0.82304(12) 0.49683(12) 0.0136(5) Uani 1 1 d . . . C33 C 0.84804(13) 0.75643(12) 0.49840(13) 0.0166(5) Uani 1 1 d . . . H33 H 0.8666 0.7148 0.4888 0.020 Uiso 1 1 calc R . . C32 C 0.79376(13) 0.75136(12) 0.51433(13) 0.0171(5) Uani 1 1 d . . . C31 C 0.76861(14) 0.81286(13) 0.52855(14) 0.0199(5) Uani 1 1 d . . . H31 H 0.7327 0.8107 0.5407 0.024 Uiso 1 1 calc R . . C30 C 0.79600(13) 0.87725(13) 0.52494(14) 0.0172(5) Uani 1 1 d . . . H30 H 0.7776 0.9193 0.5339 0.021 Uiso 1 1 calc R . . C29 C 0.99806(13) 0.91120(12) 0.65147(14) 0.0169(5) Uani 1 1 d . . . H29 H 1.0151 0.8866 0.6245 0.020 Uiso 1 1 calc R . . C28 C 1.02552(13) 0.89543(13) 0.72253(13) 0.0173(5) Uani 1 1 d . . . H28 H 1.0598 0.8597 0.7436 0.021 Uiso 1 1 calc R . . C27 C 1.00231(13) 0.93244(12) 0.76289(13) 0.0159(5) Uani 1 1 d . . . C26 C 0.95036(15) 0.98268(12) 0.72950(15) 0.0163(5) Uani 1 1 d . . . H26 H 0.9334 1.0083 0.7560 0.020 Uiso 1 1 calc R . . C25 C 0.92340(13) 0.99518(13) 0.65727(14) 0.0153(5) Uani 1 1 d . . . C24 C 0.86580(13) 1.04317(12) 0.61606(13) 0.0143(5) Uani 1 1 d . . . C23 C 0.83486(14) 1.08652(12) 0.64498(14) 0.0185(5) Uani 1 1 d . . . H23 H 0.8515 1.0871 0.6948 0.022 Uiso 1 1 calc R . . C22 C 0.77952(14) 1.12907(13) 0.60095(14) 0.0188(5) Uani 1 1 d . . . C21 C 0.75606(15) 1.12693(14) 0.52829(15) 0.0229(6) Uani 1 1 d . . . H21 H 0.7182 1.1553 0.4969 0.028 Uiso 1 1 calc R . . C20 C 0.78870(14) 1.08295(14) 0.50261(14) 0.0200(5) Uani 1 1 d . . . H20 H 0.7727 1.0820 0.4529 0.024 Uiso 1 1 calc R . . C40 C 0.75698(15) 1.05011(15) 0.18363(15) 0.0242(6) Uani 1 1 d . . . O40 O 0.70210(12) 1.01206(11) 0.14216(11) 0.0295(5) Uani 1 1 d . . . O41 O 0.78167(13) 1.09590(13) 0.16355(12) 0.0414(6) Uani 1 1 d . . . C50 C 1.02094(15) 1.26648(14) 0.46913(15) 0.0261(6) Uani 1 1 d . . . O50 O 1.07267(12) 1.29532(11) 0.52583(11) 0.0353(5) Uani 1 1 d . . . O51 O 0.99537(12) 1.29203(11) 0.41028(11) 0.0376(5) Uani 1 1 d . . . C90 C 1.05807(13) 0.74568(13) 0.43517(13) 0.0165(5) Uani 1 1 d . . . O90 O 1.10443(11) 0.76112(10) 0.42299(12) 0.0277(4) Uani 1 1 d . . . O91 O 1.03808(10) 0.68061(9) 0.43805(11) 0.0230(4) Uani 1 1 d . . . C80 C 0.76275(14) 0.67967(13) 0.51165(15) 0.0202(5) Uani 1 1 d . . . O80 O 0.72162(12) 0.68062(10) 0.54047(13) 0.0338(5) Uani 1 1 d . . . O81 O 0.77303(11) 0.62888(10) 0.48386(11) 0.0279(4) Uani 1 1 d . . . C70 C 1.03106(14) 0.92360(14) 0.84151(14) 0.0208(5) Uani 1 1 d . . . O70 O 1.07846(10) 0.87382(11) 0.87593(10) 0.0314(5) Uani 1 1 d . . . O71 O 1.01289(11) 0.96032(11) 0.87520(11) 0.0298(5) Uani 1 1 d . . . C60 C 0.74745(14) 1.17596(14) 0.63412(15) 0.0217(6) Uani 1 1 d . . . O60 O 0.69833(13) 1.21650(13) 0.58636(12) 0.0401(6) Uani 1 1 d . . . O61 O 0.76566(11) 1.17554(10) 0.69632(11) 0.0266(4) Uani 1 1 d . . . Ru1B Ru 1.360347(8) 0.991129(9) 0.767546(8) 0.01226(4) Uani 1 1 d . . . N1B N 1.41670(11) 1.05505(10) 0.73607(11) 0.0138(4) Uani 1 1 d . . . N2B N 1.30994(11) 0.97350(10) 0.65976(11) 0.0138(4) Uani 1 1 d . . . N6B N 1.31293(11) 1.08457(10) 0.77277(11) 0.0149(4) Uani 1 1 d . . . N5B N 1.41127(11) 1.01191(11) 0.87380(12) 0.0140(4) Uani 1 1 d . . . N4B N 1.30324(10) 0.91999(10) 0.78971(11) 0.0133(4) Uani 1 1 d . . . N3B N 1.40879(11) 0.89724(10) 0.77058(11) 0.0130(4) Uani 1 1 d . . . C10B C 1.46757(14) 1.09986(13) 0.77752(14) 0.0187(5) Uani 1 1 d . . . H10B H 1.4809 1.1025 0.8266 0.022 Uiso 1 1 calc R . . C11B C 1.50140(14) 1.14273(14) 0.75055(14) 0.0198(5) Uani 1 1 d . . . H11B H 1.5368 1.1744 0.7807 0.024 Uiso 1 1 calc R . . C12B C 1.48230(13) 1.13820(12) 0.67918(14) 0.0179(5) Uani 1 1 d . . . C13B C 1.42908(14) 1.09267(13) 0.63610(14) 0.0175(5) Uani 1 1 d . . . H13B H 1.4148 1.0895 0.5869 0.021 Uiso 1 1 calc R . . C14B C 1.39712(12) 1.05206(12) 0.66533(13) 0.0146(5) Uani 1 1 d . . . C15B C 1.33924(13) 1.00366(13) 0.62332(13) 0.0141(5) Uani 1 1 d . . . C16B C 1.31482(14) 0.99049(12) 0.55193(15) 0.0165(5) Uani 1 1 d . . . H16B H 1.3371 1.0109 0.5278 0.020 Uiso 1 1 calc R . . C17B C 1.25770(13) 0.94739(12) 0.51577(13) 0.0167(5) Uani 1 1 d . . . C18B C 1.22825(13) 0.91550(13) 0.55311(13) 0.0186(5) Uani 1 1 d . . . H18B H 1.1894 0.8853 0.5297 0.022 Uiso 1 1 calc R . . C19B C 1.25667(13) 0.92865(13) 0.62516(13) 0.0173(5) Uani 1 1 d . . . H19B H 1.2379 0.9051 0.6511 0.021 Uiso 1 1 calc R . . C39B C 1.26293(14) 1.11988(13) 0.71796(14) 0.0198(5) Uani 1 1 d . . . H39B H 1.2446 1.0995 0.6720 0.024 Uiso 1 1 calc R . . C38B C 1.23684(14) 1.18410(13) 0.72504(15) 0.0226(5) Uani 1 1 d . . . H38B H 1.2011 1.2071 0.6850 0.027 Uiso 1 1 calc R . . C37B C 1.26388(14) 1.21453(13) 0.79184(15) 0.0218(5) Uani 1 1 d . . . C36B C 1.31594(15) 1.17917(13) 0.84873(15) 0.0214(5) Uani 1 1 d . . . H35B H 1.3354 1.1992 0.8949 0.026 Uiso 1 1 calc R . . C35B C 1.33962(13) 1.11444(12) 0.83813(13) 0.0165(5) Uani 1 1 d . . . C34B C 1.39320(13) 1.07211(12) 0.89649(13) 0.0161(5) Uani 1 1 d . . . C33B C 1.42153(14) 1.08881(13) 0.96746(14) 0.0210(5) Uani 1 1 d . . . H33B H 1.4083 1.1312 0.9819 0.025 Uiso 1 1 calc R . . C32B C 1.46917(14) 1.04351(14) 1.01738(14) 0.0207(5) Uani 1 1 d . . . C31B C 1.48708(15) 0.98113(13) 0.99504(15) 0.0197(6) Uani 1 1 d . . . H31B H 1.5192 0.9487 1.0285 0.024 Uiso 1 1 calc R . . C30B C 1.45715(13) 0.96748(13) 0.92324(14) 0.0188(5) Uani 1 1 d . . . H30B H 1.4693 0.9250 0.9080 0.023 Uiso 1 1 calc R . . C29B C 1.25148(13) 0.93792(12) 0.80257(13) 0.0149(5) Uani 1 1 d . . . H29B H 1.2392 0.9867 0.8005 0.018 Uiso 1 1 calc R . . C28B C 1.21538(13) 0.88753(12) 0.81879(13) 0.0172(5) Uani 1 1 d . . . H28B H 1.1795 0.9017 0.8285 0.021 Uiso 1 1 calc R . . C27B C 1.23243(13) 0.81597(12) 0.82063(13) 0.0147(5) Uani 1 1 d . . . C26B C 1.28620(13) 0.79712(12) 0.80791(13) 0.0153(5) Uani 1 1 d . . . H26B H 1.2989 0.7486 0.8094 0.018 Uiso 1 1 calc R . . C25B C 1.32136(12) 0.85020(12) 0.79298(13) 0.0133(5) Uani 1 1 d . . . C24B C 1.37979(12) 0.83684(12) 0.77956(13) 0.0144(5) Uani 1 1 d . . . C23B C 1.40475(13) 0.77004(12) 0.77676(13) 0.0156(5) Uani 1 1 d . . . H23B H 1.3843 0.7286 0.7839 0.019 Uiso 1 1 calc R . . C22B C 1.46024(13) 0.76418(13) 0.76330(13) 0.0166(5) Uani 1 1 d . . . C21B C 1.48966(13) 0.82549(13) 0.75420(14) 0.0178(5) Uani 1 1 d . . . H21B H 1.5276 0.8227 0.7451 0.021 Uiso 1 1 calc R . . C20B C 1.46326(13) 0.89127(13) 0.75850(14) 0.0176(5) Uani 1 1 d . . . H20B H 1.4840 0.9333 0.7528 0.021 Uiso 1 1 calc R . . C40B C 1.51629(14) 1.18050(13) 0.64542(15) 0.0207(5) Uani 1 1 d . . . O40B O 1.56482(12) 1.22246(12) 0.69004(11) 0.0365(6) Uani 1 1 d . . . O41B O 1.49954(12) 1.17429(11) 0.58282(11) 0.0306(5) Uani 1 1 d . . . C50B C 1.22938(14) 0.94053(13) 0.43747(14) 0.0201(5) Uani 1 1 d . . . O50B O 1.16298(9) 0.92559(11) 0.40371(9) 0.0291(4) Uani 1 1 d . . . O51B O 1.26464(10) 0.95098(11) 0.40941(10) 0.0259(4) Uani 1 1 d . . . C90B C 1.23868(15) 1.28292(13) 0.80686(15) 0.0239(6) Uani 1 1 d . . . O90B O 1.18853(12) 1.31277(11) 0.74947(12) 0.0369(5) Uani 1 1 d . . . O91B O 1.26243(12) 1.30806(11) 0.86555(12) 0.0356(5) Uani 1 1 d . . . C80B C 1.50031(16) 1.06259(16) 1.09411(15) 0.0265(6) Uani 1 1 d . . . O80B O 1.54867(13) 1.01702(11) 1.13496(12) 0.0347(6) Uani 1 1 d . . . O81B O 1.48304(16) 1.11333(16) 1.11541(13) 0.0596(8) Uani 1 1 d . . . C70B C 1.19227(13) 0.76096(12) 0.83488(13) 0.0161(5) Uani 1 1 d . . . O70B O 1.21562(10) 0.69618(9) 0.83899(11) 0.0216(4) Uani 1 1 d . . . O71B O 1.14186(9) 0.77519(9) 0.84227(10) 0.0200(4) Uani 1 1 d . . . C60B C 1.48773(14) 0.69230(13) 0.76148(14) 0.0201(5) Uani 1 1 d . . . O60B O 1.53429(12) 0.69548(10) 0.73914(13) 0.0324(5) Uani 1 1 d . . . O61B O 1.46973(10) 0.63871(9) 0.77896(11) 0.0257(4) Uani 1 1 d . . . Cl1 Cl 0.62608(3) 1.06839(3) -0.00893(3) 0.02101(12) Uani 1 1 d . . . Cl2 Cl 1.63004(4) 1.32496(3) 0.63447(4) 0.01917(11) Uani 1 1 d . . . Cl3 Cl 1.63238(3) 1.05472(3) 1.28959(3) 0.02084(12) Uani 1 1 d . . . Cl4 Cl 1.61087(4) 0.56321(3) 0.74517(3) 0.02422(13) Uani 1 1 d . . . O94 O 1.25040(16) 1.21429(16) 0.96572(16) 0.0661(8) Uani 1 1 d . . . O95 O 0.64533(11) 0.57028(11) 0.52476(11) 0.0333(5) Uani 1 1 d . . . O96 O 0.62081(12) 0.49520(10) 0.61742(10) 0.0325(5) Uani 1 1 d . . . O97 O 1.15604(12) 0.59429(10) 0.86477(12) 0.0319(5) Uani 1 1 d . . . O98 O 1.10014(13) 0.57881(11) 0.41427(12) 0.0364(5) Uani 1 1 d . . . O99 O 1.3858(4) 1.2379(4) 1.0688(6) 0.178(6) Uani 0.50 1 d P . . H40 H 0.6833 1.0276 0.0984 0.050 Uiso 1 1 d . . . H50 H 1.0836 1.3394 0.5131 0.050 Uiso 1 1 d . . . H61 H 1.0649 0.6520 0.4325 0.050 Uiso 1 1 d . . . H70 H 0.7089 0.6368 0.5419 0.050 Uiso 1 1 d . . . H80 H 1.0948 0.8465 0.8456 0.050 Uiso 1 1 d . . . H90 H 0.6711 1.2469 0.6011 0.050 Uiso 1 1 d . . . H40B H 1.5849 1.2481 0.6693 0.050 Uiso 1 1 d . . . H50B H 1.1439 0.9292 0.3575 0.050 Uiso 1 1 d . . . H60B H 1.1732 1.3520 0.7607 0.050 Uiso 1 1 d . . . H70B H 1.5751 1.0287 1.1805 0.050 Uiso 1 1 d . . . H80B H 1.1928 0.6616 0.8489 0.050 Uiso 1 1 d . . . H90B H 1.5387 0.6544 0.7336 0.050 Uiso 1 1 d . . . H941 H 1.2530 1.2511 0.9280 0.050 Uiso 1 1 d . . . H942 H 1.2098 1.2091 0.9827 0.050 Uiso 1 1 d . . . H951 H 0.6109 0.5667 0.4812 0.050 Uiso 1 1 d . . . H952 H 0.6392 0.5420 0.5454 0.050 Uiso 1 1 d . . . H961 H 0.6241 0.4461 0.6247 0.050 Uiso 1 1 d . . . H962 H 0.6140 0.5110 0.6472 0.050 Uiso 1 1 d . . . H971 H 1.1479 0.5903 0.8981 0.050 Uiso 1 1 d . . . H972 H 1.1462 0.5529 0.8384 0.050 Uiso 1 1 d . . . H981 H 1.1096 0.5431 0.4375 0.050 Uiso 1 1 d . . . H982 H 1.1124 0.5806 0.3756 0.050 Uiso 1 1 d . . . H991 H 1.3485 1.2239 1.0464 0.050 Uiso 0.50 1 d P . . H992 H 1.3832 1.2800 1.0693 0.050 Uiso 0.50 1 d P . . 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 0.01394(9) 0.01153(8) 0.01281(9) 0.00022(6) 0.00766(7) 0.00067(7) N1 0.0165(11) 0.0127(9) 0.0169(12) 0.0006(8) 0.0094(9) 0.0006(8) N2 0.0145(10) 0.0125(9) 0.0171(11) 0.0000(7) 0.0079(8) -0.0003(8) N6 0.0138(10) 0.0122(9) 0.0129(10) 0.0010(7) 0.0067(8) -0.0002(7) N5 0.0178(11) 0.0125(9) 0.0125(11) 0.0002(7) 0.0075(9) 0.0002(7) N4 0.0155(10) 0.0116(9) 0.0190(11) -0.0004(8) 0.0104(9) 0.0002(8) N3 0.0189(11) 0.0125(9) 0.0174(11) 0.0034(8) 0.0114(9) 0.0037(8) C10 0.0184(12) 0.0173(12) 0.0188(13) -0.0021(9) 0.0090(10) -0.0032(9) C11 0.0182(14) 0.0229(12) 0.0205(15) -0.0018(10) 0.0083(11) -0.0015(10) C12 0.0160(13) 0.0216(12) 0.0143(13) -0.0002(9) 0.0063(10) 0.0014(9) C13 0.0246(13) 0.0186(12) 0.0194(13) 0.0027(9) 0.0123(11) -0.0011(10) C14 0.0181(12) 0.0146(11) 0.0171(13) 0.0007(9) 0.0098(10) 0.0012(9) C15 0.0169(12) 0.0142(11) 0.0162(12) 0.0007(8) 0.0079(10) 0.0009(9) C16 0.0227(13) 0.0175(12) 0.0171(13) 0.0017(9) 0.0075(10) -0.0012(10) C17 0.0219(14) 0.0147(11) 0.0239(14) 0.0013(9) 0.0113(11) -0.0008(10) C18 0.0224(14) 0.0191(12) 0.0204(14) -0.0016(9) 0.0059(11) -0.0039(10) C19 0.0191(13) 0.0188(12) 0.0151(13) 0.0003(9) 0.0065(10) -0.0015(9) C39 0.0195(12) 0.0140(11) 0.0155(12) -0.0009(8) 0.0086(9) -0.0025(9) C38 0.0145(12) 0.0212(12) 0.0164(12) -0.0013(9) 0.0093(9) -0.0013(9) C37 0.0150(12) 0.0187(11) 0.0133(12) -0.0008(9) 0.0069(9) 0.0003(9) C36 0.0171(12) 0.0155(11) 0.0150(12) 0.0008(8) 0.0085(10) -0.0018(9) C35 0.0179(12) 0.0131(10) 0.0105(11) 0.0011(8) 0.0065(9) 0.0000(9) C34 0.0151(12) 0.0153(10) 0.0117(12) 0.0004(8) 0.0073(9) 0.0014(8) C33 0.0201(13) 0.0131(11) 0.0197(13) -0.0002(8) 0.0120(10) 0.0012(9) C32 0.0206(13) 0.0164(11) 0.0154(12) 0.0015(9) 0.0096(10) -0.0007(9) C31 0.0204(13) 0.0220(13) 0.0222(14) 0.0008(10) 0.0143(11) -0.0008(10) C30 0.0165(13) 0.0186(12) 0.0197(13) -0.0001(9) 0.0111(10) 0.0040(9) C29 0.0163(12) 0.0162(11) 0.0199(13) 0.0011(9) 0.0099(10) 0.0052(9) C28 0.0172(12) 0.0175(11) 0.0174(13) 0.0019(9) 0.0086(10) 0.0049(9) C27 0.0153(12) 0.0162(11) 0.0159(13) 0.0005(8) 0.0073(9) 0.0000(9) C26 0.0208(14) 0.0155(12) 0.0159(14) -0.0011(8) 0.0114(11) 0.0011(9) C25 0.0163(12) 0.0114(11) 0.0183(13) -0.0014(9) 0.0085(10) -0.0016(9) C24 0.0172(12) 0.0133(10) 0.0165(13) -0.0021(8) 0.0113(10) -0.0019(9) C23 0.0201(13) 0.0154(11) 0.0215(14) 0.0010(9) 0.0111(11) 0.0018(9) C22 0.0210(13) 0.0172(11) 0.0203(14) -0.0020(9) 0.0115(11) 0.0025(9) C21 0.0223(14) 0.0233(13) 0.0203(14) 0.0017(10) 0.0079(11) 0.0083(10) C20 0.0217(13) 0.0229(13) 0.0178(13) -0.0003(9) 0.0113(11) 0.0030(10) C40 0.0237(15) 0.0311(14) 0.0154(14) 0.0010(10) 0.0075(11) -0.0020(11) O40 0.0286(12) 0.0386(12) 0.0137(11) 0.0033(7) 0.0039(9) -0.0058(8) O41 0.0431(14) 0.0564(15) 0.0175(11) 0.0063(9) 0.0087(10) -0.0207(11) C50 0.0277(15) 0.0185(12) 0.0297(16) 0.0007(10) 0.0119(12) -0.0048(10) O50 0.0395(13) 0.0277(11) 0.0299(12) 0.0010(8) 0.0096(10) -0.0182(9) O51 0.0443(14) 0.0282(11) 0.0286(12) 0.0092(8) 0.0080(10) -0.0123(9) C90 0.0172(12) 0.0179(11) 0.0155(12) -0.0006(9) 0.0088(9) 0.0008(9) O90 0.0283(11) 0.0242(9) 0.0445(12) 0.0012(8) 0.0287(10) 0.0006(8) O91 0.0254(10) 0.0162(9) 0.0351(11) -0.0021(7) 0.0206(9) 0.0013(7) C80 0.0207(13) 0.0188(12) 0.0235(14) 0.0050(9) 0.0125(11) -0.0011(9) O80 0.0452(14) 0.0247(10) 0.0502(14) -0.0028(9) 0.0379(12) -0.0088(9) O81 0.0359(11) 0.0176(9) 0.0384(12) -0.0002(8) 0.0245(9) -0.0022(8) C70 0.0245(14) 0.0211(12) 0.0171(13) 0.0006(9) 0.0103(11) 0.0025(10) O70 0.0390(11) 0.0362(11) 0.0184(9) 0.0062(8) 0.0133(8) 0.0205(9) O71 0.0398(12) 0.0310(11) 0.0208(10) 0.0015(8) 0.0162(9) 0.0137(9) C60 0.0207(14) 0.0212(13) 0.0239(16) -0.0009(9) 0.0112(11) 0.0055(10) O60 0.0455(14) 0.0506(14) 0.0256(12) 0.0072(10) 0.0181(10) 0.0339(11) O61 0.0302(11) 0.0301(10) 0.0219(11) -0.0016(8) 0.0144(9) 0.0088(8) Ru1B 0.01409(9) 0.01160(8) 0.01296(9) 0.00007(7) 0.00799(7) -0.00030(7) N1B 0.0147(10) 0.0129(9) 0.0149(11) -0.0007(7) 0.0080(8) -0.0010(7) N2B 0.0136(10) 0.0134(9) 0.0150(11) -0.0002(7) 0.0072(8) -0.0011(8) N6B 0.0188(11) 0.0113(9) 0.0180(11) 0.0017(7) 0.0115(9) -0.0013(7) N5B 0.0126(11) 0.0142(10) 0.0169(11) 0.0003(8) 0.0084(9) -0.0013(8) N4B 0.0154(10) 0.0134(9) 0.0120(10) 0.0008(7) 0.0072(8) 0.0010(7) N3B 0.0133(9) 0.0143(9) 0.0125(10) -0.0010(7) 0.0072(8) -0.0019(8) C10B 0.0227(13) 0.0174(11) 0.0152(13) -0.0028(9) 0.0085(10) -0.0063(9) C11B 0.0200(13) 0.0202(12) 0.0201(14) -0.0033(10) 0.0103(11) -0.0069(10) C12B 0.0175(12) 0.0149(11) 0.0228(14) 0.0026(9) 0.0108(10) -0.0011(9) C13B 0.0208(13) 0.0194(12) 0.0140(13) 0.0003(9) 0.0096(10) -0.0026(9) C14B 0.0131(11) 0.0138(10) 0.0158(12) -0.0003(8) 0.0061(9) -0.0010(8) C15B 0.0146(12) 0.0135(11) 0.0150(13) 0.0014(9) 0.0078(10) 0.0000(9) C16B 0.0156(13) 0.0180(12) 0.0181(14) 0.0016(9) 0.0098(11) -0.0006(9) C17B 0.0196(13) 0.0173(11) 0.0144(13) 0.0001(9) 0.0092(10) -0.0002(9) C18B 0.0183(12) 0.0191(12) 0.0172(13) -0.0027(9) 0.0075(10) -0.0048(9) C19B 0.0178(12) 0.0186(12) 0.0179(13) 0.0000(9) 0.0105(10) -0.0029(9) C39B 0.0219(14) 0.0179(12) 0.0173(13) -0.0001(9) 0.0076(10) 0.0011(9) C38B 0.0198(13) 0.0190(12) 0.0256(15) 0.0023(10) 0.0082(11) 0.0054(10) C37B 0.0250(14) 0.0171(12) 0.0258(15) -0.0008(10) 0.0141(11) -0.0007(10) C36B 0.0284(14) 0.0178(12) 0.0219(14) -0.0029(9) 0.0151(11) -0.0006(10) C35B 0.0192(13) 0.0159(11) 0.0160(13) 0.0018(9) 0.0098(10) 0.0008(9) C34B 0.0193(12) 0.0155(11) 0.0160(13) -0.0009(8) 0.0105(10) -0.0009(9) C33B 0.0239(13) 0.0207(12) 0.0199(14) -0.0025(9) 0.0117(11) 0.0003(10) C32B 0.0235(14) 0.0231(13) 0.0197(14) -0.0028(10) 0.0137(11) -0.0037(10) C31B 0.0172(14) 0.0260(13) 0.0146(14) 0.0011(9) 0.0065(11) 0.0022(9) C30B 0.0191(13) 0.0184(12) 0.0191(14) -0.0001(9) 0.0092(11) 0.0019(9) C29B 0.0170(12) 0.0142(10) 0.0165(12) -0.0013(8) 0.0104(9) 0.0008(9) C28B 0.0193(12) 0.0148(11) 0.0220(13) -0.0008(9) 0.0136(10) 0.0011(9) C27B 0.0168(12) 0.0134(11) 0.0161(12) -0.0001(8) 0.0096(10) -0.0003(9) C26B 0.0177(12) 0.0119(11) 0.0177(12) -0.0002(8) 0.0096(10) 0.0006(9) C25B 0.0148(12) 0.0121(10) 0.0153(12) -0.0001(8) 0.0091(9) 0.0016(9) C24B 0.0146(12) 0.0142(11) 0.0150(12) -0.0008(8) 0.0074(10) 0.0003(8) C23B 0.0171(12) 0.0127(10) 0.0181(12) -0.0003(9) 0.0095(9) 0.0002(9) C22B 0.0156(12) 0.0170(11) 0.0168(13) 0.0007(9) 0.0075(10) 0.0043(9) C21B 0.0160(12) 0.0191(12) 0.0222(14) 0.0026(9) 0.0122(10) 0.0037(9) C20B 0.0176(13) 0.0175(12) 0.0225(13) 0.0002(9) 0.0135(10) 0.0009(9) C40B 0.0219(13) 0.0188(12) 0.0238(16) 0.0010(9) 0.0128(11) -0.0047(9) O40B 0.0422(13) 0.0446(13) 0.0254(12) -0.0074(9) 0.0184(10) -0.0310(10) O41B 0.0351(12) 0.0359(11) 0.0221(12) -0.0008(8) 0.0148(9) -0.0146(9) C50B 0.0196(13) 0.0206(12) 0.0184(14) -0.0019(9) 0.0077(11) -0.0022(9) O50B 0.0208(9) 0.0482(12) 0.0158(9) -0.0035(8) 0.0065(7) -0.0123(8) O51B 0.0242(10) 0.0391(11) 0.0184(10) -0.0019(8) 0.0134(8) -0.0051(8) C90B 0.0266(14) 0.0169(12) 0.0305(16) 0.0000(10) 0.0155(12) 0.0022(10) O90B 0.0415(13) 0.0263(10) 0.0328(12) -0.0020(8) 0.0096(10) 0.0184(9) O91B 0.0477(14) 0.0241(10) 0.0324(13) -0.0032(8) 0.0171(10) 0.0097(9) C80B 0.0261(15) 0.0368(15) 0.0177(15) 0.0007(11) 0.0113(12) 0.0026(12) O80B 0.0356(14) 0.0402(13) 0.0169(12) -0.0041(8) 0.0034(10) 0.0049(9) O81B 0.0668(18) 0.0724(18) 0.0216(13) -0.0116(11) 0.0066(12) 0.0351(15) C70B 0.0180(12) 0.0149(11) 0.0161(12) 0.0008(8) 0.0087(10) 0.0008(9) O70B 0.0232(10) 0.0127(8) 0.0370(11) 0.0038(7) 0.0210(9) 0.0012(7) O71B 0.0190(9) 0.0193(9) 0.0279(10) 0.0007(7) 0.0162(8) -0.0001(7) C60B 0.0204(13) 0.0207(12) 0.0207(13) -0.0023(10) 0.0111(10) 0.0020(10) O60B 0.0405(13) 0.0207(10) 0.0540(14) 0.0054(9) 0.0372(11) 0.0127(8) O61B 0.0262(10) 0.0154(9) 0.0385(11) -0.0005(7) 0.0177(9) 0.0017(7) Cl1 0.0243(3) 0.0192(3) 0.0199(3) 0.0000(2) 0.0109(2) 0.0010(2) Cl2 0.0197(2) 0.0148(2) 0.0280(3) 0.0001(2) 0.0155(2) 0.0001(2) Cl3 0.0240(3) 0.0195(3) 0.0196(3) 0.0009(2) 0.0109(2) 0.0001(2) Cl4 0.0253(3) 0.0269(3) 0.0179(3) -0.0008(2) 0.0083(2) 0.0101(2) O94 0.073(2) 0.0557(17) 0.083(2) 0.0055(14) 0.0481(17) 0.0031(14) O95 0.0326(12) 0.0339(11) 0.0284(12) 0.0068(8) 0.0105(9) -0.0120(9) O96 0.0572(14) 0.0202(9) 0.0356(12) 0.0016(7) 0.0346(12) 0.0036(9) O97 0.0512(14) 0.0188(9) 0.0415(13) -0.0067(8) 0.0349(11) -0.0122(9) O98 0.0617(16) 0.0233(10) 0.0431(13) 0.0107(9) 0.0405(12) 0.0187(10) O99 0.053(4) 0.063(5) 0.257(12) 0.005(6) -0.056(6) 0.026(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 N6 2.052(2) . ? Ru1 N5 2.054(2) . ? Ru1 N4 2.056(2) . ? Ru1 N3 2.059(2) . ? Ru1 N1 2.060(2) . ? Ru1 N2 2.072(2) . ? N1 C10 1.343(3) . ? N1 C15 1.357(3) . ? N2 C19 1.347(3) . ? N2 C14 1.365(3) . ? N6 C39 1.351(3) . ? N6 C35 1.360(3) . ? N5 C30 1.342(3) . ? N5 C34 1.366(3) . ? N4 C29 1.350(3) . ? N4 C25 1.364(3) . ? N3 C20 1.339(3) . ? N3 C24 1.369(3) . ? C10 C11 1.378(4) . ? C10 H10 0.9500 . ? C11 C12 1.387(4) . ? C11 H11 0.9500 . ? C12 C13 1.392(4) . ? C12 C40 1.501(4) . ? C13 C15 1.391(4) . ? C13 H13 0.9500 . ? C14 C16 1.379(3) . ? C14 C15 1.464(3) . ? C16 C17 1.391(4) . ? C16 H16 0.9500 . ? C17 C18 1.395(4) . ? C17 C50 1.496(4) . ? C18 C19 1.391(3) . ? C18 H18 0.9500 . ? C19 H19 0.9500 . ? C39 C38 1.382(3) . ? C39 H39 0.9500 . ? C38 C37 1.374(3) . ? C38 H38 0.9500 . ? C37 C36 1.397(3) . ? C37 C90 1.504(3) . ? C36 C35 1.379(3) . ? C36 H36 0.9500 . ? C35 C34 1.486(3) . ? C34 C33 1.387(3) . ? C33 C32 1.402(4) . ? C33 H33 0.9500 . ? C32 C31 1.379(4) . ? C32 C80 1.500(3) . ? C31 C30 1.372(4) . ? C31 H31 0.9500 . ? C30 H30 0.9500 . ? C29 C28 1.378(4) . ? C29 H29 0.9500 . ? C28 C27 1.388(3) . ? C28 H28 0.9500 . ? C27 C26 1.393(4) . ? C27 C70 1.502(4) . ? C26 C25 1.391(4) . ? C26 H26 0.9500 . ? C25 C24 1.464(3) . ? C24 C23 1.388(3) . ? C23 C22 1.388(4) . ? C23 H23 0.9500 . ? C22 C21 1.390(4) . ? C22 C60 1.508(3) . ? C21 C20 1.376(4) . ? C21 H21 0.9500 . ? C20 H20 0.9500 . ? C40 O41 1.205(4) . ? C40 O40 1.321(4) . ? O40 H40 0.8762 . ? C50 O51 1.210(4) . ? C50 O50 1.325(4) . ? O50 H50 0.9396 . ? C90 O90 1.210(3) . ? C90 O91 1.312(3) . ? O91 H61 0.8509 . ? C80 O81 1.204(3) . ? C80 O80 1.324(3) . ? O80 H70 0.8755 . ? C70 O71 1.200(3) . ? C70 O70 1.334(3) . ? O70 H80 1.0223 . ? C60 O61 1.197(3) . ? C60 O60 1.322(3) . ? O60 H90 0.9864 . ? Ru1B N5B 2.043(2) . ? Ru1B N4B 2.047(2) . ? Ru1B N3B 2.049(2) . ? Ru1B N2B 2.060(2) . ? Ru1B N1B 2.065(2) . ? Ru1B N6B 2.076(2) . ? N1B C10B 1.346(3) . ? N1B C14B 1.368(3) . ? N2B C19B 1.347(3) . ? N2B C15B 1.357(3) . ? N6B C39B 1.344(3) . ? N6B C35B 1.357(3) . ? N5B C30B 1.351(3) . ? N5B C34B 1.365(3) . ? N4B C29B 1.344(3) . ? N4B C25B 1.363(3) . ? N3B C20B 1.355(3) . ? N3B C24B 1.363(3) . ? C10B C11B 1.401(4) . ? C10B H10B 0.9500 . ? C11B C12B 1.384(4) . ? C11B H11B 0.9500 . ? C12B C13B 1.391(4) . ? C12B C40B 1.499(3) . ? C13B C14B 1.379(3) . ? C13B H13B 0.9500 . ? C14B C15B 1.476(3) . ? C15B C16B 1.383(4) . ? C16B C17B 1.385(4) . ? C16B H16B 0.9500 . ? C17B C18B 1.389(3) . ? C17B C50B 1.493(4) . ? C18B C19B 1.386(4) . ? C18B H18B 0.9500 . ? C19B H19B 0.9500 . ? C39B C38B 1.377(3) . ? C39B H39B 0.9500 . ? C38B C37B 1.387(4) . ? C38B H38B 0.9500 . ? C37B C36B 1.384(4) . ? C37B C90B 1.497(4) . ? C36B C35B 1.386(3) . ? C36B H35B 0.9500 . ? C35B C34B 1.480(3) . ? C34B C33B 1.379(4) . ? C33B C32B 1.380(4) . ? C33B H33B 0.9500 . ? C32B C31B 1.394(4) . ? C32B C80B 1.495(4) . ? C31B C30B 1.381(4) . ? C31B H31B 0.9500 . ? C30B H30B 0.9500 . ? C29B C28B 1.387(3) . ? C29B H29B 0.9500 . ? C28B C27B 1.392(3) . ? C28B H28B 0.9500 . ? C27B C26B 1.389(3) . ? C27B C70B 1.488(3) . ? C26B C25B 1.394(3) . ? C26B H26B 0.9500 . ? C25B C24B 1.476(3) . ? C24B C23B 1.384(3) . ? C23B C22B 1.395(3) . ? C23B H23B 0.9500 . ? C22B C21B 1.383(3) . ? C22B C60B 1.490(3) . ? C21B C20B 1.389(3) . ? C21B H21B 0.9500 . ? C20B H20B 0.9500 . ? C40B O41B 1.218(3) . ? C40B O40B 1.308(3) . ? O40B H40B 0.9045 . ? C50B O51B 1.209(3) . ? C50B O50B 1.322(3) . ? O50B H50B 0.8761 . ? C90B O91B 1.206(4) . ? C90B O90B 1.326(4) . ? O90B H60B 0.8918 . ? C80B O81B 1.197(4) . ? C80B O80B 1.323(4) . ? O80B H70B 0.8945 . ? C70B O71B 1.230(3) . ? C70B O70B 1.309(3) . ? O70B H80B 0.9088 . ? C60B O61B 1.207(3) . ? C60B O60B 1.331(3) . ? O60B H90B 0.7942 . ? O94 H941 1.0878 . ? O94 H942 1.1249 . ? O95 H951 0.8826 . ? O95 H952 0.7450 . ? O96 H961 0.9327 . ? O96 H962 0.7828 . ? O97 H971 0.8214 . ? O97 H972 0.9247 . ? O98 H981 0.8020 . ? O98 H982 0.9906 . ? O99 H991 0.7768 . ? O99 H992 0.7928 . ? 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 N5 78.54(8) . . ? N6 Ru1 N4 96.94(8) . . ? N5 Ru1 N4 83.72(8) . . ? N6 Ru1 N3 174.11(8) . . ? N5 Ru1 N3 96.91(8) . . ? N4 Ru1 N3 78.72(8) . . ? N6 Ru1 N1 84.78(8) . . ? N5 Ru1 N1 97.93(8) . . ? N4 Ru1 N1 177.83(9) . . ? N3 Ru1 N1 99.65(8) . . ? N6 Ru1 N2 99.27(8) . . ? N5 Ru1 N2 175.97(9) . . ? N4 Ru1 N2 99.95(8) . . ? N3 Ru1 N2 85.49(8) . . ? N1 Ru1 N2 78.44(8) . . ? C10 N1 C15 118.7(2) . . ? C10 N1 Ru1 125.06(17) . . ? C15 N1 Ru1 115.90(17) . . ? C19 N2 C14 118.1(2) . . ? C19 N2 Ru1 126.14(17) . . ? C14 N2 Ru1 115.60(16) . . ? C39 N6 C35 118.2(2) . . ? C39 N6 Ru1 124.89(16) . . ? C35 N6 Ru1 116.79(16) . . ? C30 N5 C34 118.4(2) . . ? C30 N5 Ru1 125.00(16) . . ? C34 N5 Ru1 116.38(16) . . ? C29 N4 C25 118.5(2) . . ? C29 N4 Ru1 124.94(17) . . ? C25 N4 Ru1 116.08(17) . . ? C20 N3 C24 118.8(2) . . ? C20 N3 Ru1 125.60(17) . . ? C24 N3 Ru1 115.55(16) . . ? N1 C10 C11 123.0(2) . . ? N1 C10 H10 118.5 . . ? C11 C10 H10 118.5 . . ? C10 C11 C12 118.8(2) . . ? C10 C11 H11 120.6 . . ? C12 C11 H11 120.6 . . ? C11 C12 C13 118.8(2) . . ? C11 C12 C40 123.0(2) . . ? C13 C12 C40 118.2(2) . . ? C15 C13 C12 119.6(2) . . ? C15 C13 H13 120.2 . . ? C12 C13 H13 120.2 . . ? N2 C14 C16 121.9(2) . . ? N2 C14 C15 114.6(2) . . ? C16 C14 C15 123.6(2) . . ? N1 C15 C13 121.1(2) . . ? N1 C15 C14 115.3(2) . . ? C13 C15 C14 123.6(2) . . ? C14 C16 C17 120.0(2) . . ? C14 C16 H16 120.0 . . ? C17 C16 H16 120.0 . . ? C16 C17 C18 118.2(2) . . ? C16 C17 C50 117.7(2) . . ? C18 C17 C50 124.1(2) . . ? C19 C18 C17 119.0(2) . . ? C19 C18 H18 120.5 . . ? C17 C18 H18 120.5 . . ? N2 C19 C18 122.7(2) . . ? N2 C19 H19 118.7 . . ? C18 C19 H19 118.7 . . ? N6 C39 C38 122.4(2) . . ? N6 C39 H39 118.8 . . ? C38 C39 H39 118.8 . . ? C37 C38 C39 119.1(2) . . ? C37 C38 H38 120.5 . . ? C39 C38 H38 120.5 . . ? C38 C37 C36 119.3(2) . . ? C38 C37 C90 119.4(2) . . ? C36 C37 C90 121.3(2) . . ? C35 C36 C37 118.9(2) . . ? C35 C36 H36 120.6 . . ? C37 C36 H36 120.6 . . ? N6 C35 C36 121.9(2) . . ? N6 C35 C34 114.0(2) . . ? C36 C35 C34 124.1(2) . . ? N5 C34 C33 121.4(2) . . ? N5 C34 C35 114.1(2) . . ? C33 C34 C35 124.5(2) . . ? C34 C33 C32 119.1(2) . . ? C34 C33 H33 120.5 . . ? C32 C33 H33 120.5 . . ? C31 C32 C33 118.8(2) . . ? C31 C32 C80 122.3(2) . . ? C33 C32 C80 118.8(2) . . ? C30 C31 C32 119.3(2) . . ? C30 C31 H31 120.3 . . ? C32 C31 H31 120.3 . . ? N5 C30 C31 123.0(2) . . ? N5 C30 H30 118.5 . . ? C31 C30 H30 118.5 . . ? N4 C29 C28 122.9(2) . . ? N4 C29 H29 118.5 . . ? C28 C29 H29 118.5 . . ? C29 C28 C27 119.0(2) . . ? C29 C28 H28 120.5 . . ? C27 C28 H28 120.5 . . ? C28 C27 C26 118.6(2) . . ? C28 C27 C70 124.2(2) . . ? C26 C27 C70 117.1(2) . . ? C25 C26 C27 119.8(2) . . ? C25 C26 H26 120.1 . . ? C27 C26 H26 120.1 . . ? N4 C25 C26 121.1(2) . . ? N4 C25 C24 114.6(2) . . ? C26 C25 C24 124.3(2) . . ? N3 C24 C23 120.7(2) . . ? N3 C24 C25 114.9(2) . . ? C23 C24 C25 124.4(2) . . ? C22 C23 C24 119.8(2) . . ? C22 C23 H23 120.1 . . ? C24 C23 H23 120.1 . . ? C23 C22 C21 118.8(2) . . ? C23 C22 C60 118.5(2) . . ? C21 C22 C60 122.7(2) . . ? C20 C21 C22 118.8(2) . . ? C20 C21 H21 120.6 . . ? C22 C21 H21 120.6 . . ? N3 C20 C21 123.0(3) . . ? N3 C20 H20 118.5 . . ? C21 C20 H20 118.5 . . ? O41 C40 O40 125.0(3) . . ? O41 C40 C12 122.3(3) . . ? O40 C40 C12 112.6(2) . . ? C40 O40 H40 110.8 . . ? O51 C50 O50 124.4(2) . . ? O51 C50 C17 122.2(3) . . ? O50 C50 C17 113.4(2) . . ? C50 O50 H50 108.8 . . ? O90 C90 O91 125.0(2) . . ? O90 C90 C37 122.0(2) . . ? O91 C90 C37 113.0(2) . . ? C90 O91 H61 107.9 . . ? O81 C80 O80 125.3(2) . . ? O81 C80 C32 122.6(2) . . ? O80 C80 C32 112.0(2) . . ? C80 O80 H70 108.0 . . ? O71 C70 O70 118.1(2) . . ? O71 C70 C27 122.0(2) . . ? O70 C70 C27 119.9(2) . . ? C70 O70 H80 115.0 . . ? O61 C60 O60 125.6(2) . . ? O61 C60 C22 122.7(2) . . ? O60 C60 C22 111.6(2) . . ? C60 O60 H90 119.1 . . ? N5B Ru1B N4B 86.39(8) . . ? N5B Ru1B N3B 97.37(8) . . ? N4B Ru1B N3B 78.63(8) . . ? N5B Ru1B N2B 178.07(9) . . ? N4B Ru1B N2B 95.38(8) . . ? N3B Ru1B N2B 83.75(8) . . ? N5B Ru1B N1B 99.09(8) . . ? N4B Ru1B N1B 173.45(8) . . ? N3B Ru1B N1B 96.99(8) . . ? N2B Ru1B N1B 79.20(8) . . ? N5B Ru1B N6B 78.52(8) . . ? N4B Ru1B N6B 98.90(8) . . ? N3B Ru1B N6B 175.39(8) . . ? N2B Ru1B N6B 100.41(8) . . ? N1B Ru1B N6B 85.79(8) . . ? C10B N1B C14B 118.7(2) . . ? C10B N1B Ru1B 126.35(17) . . ? C14B N1B Ru1B 114.85(15) . . ? C19B N2B C15B 118.5(2) . . ? C19B N2B Ru1B 125.53(17) . . ? C15B N2B Ru1B 115.47(16) . . ? C39B N6B C35B 118.1(2) . . ? C39B N6B Ru1B 126.60(17) . . ? C35B N6B Ru1B 115.12(16) . . ? C30B N5B C34B 118.0(2) . . ? C30B N5B Ru1B 124.47(17) . . ? C34B N5B Ru1B 117.26(17) . . ? C29B N4B C25B 119.3(2) . . ? C29B N4B Ru1B 124.52(16) . . ? C25B N4B Ru1B 116.15(16) . . ? C20B N3B C24B 118.8(2) . . ? C20B N3B Ru1B 124.46(16) . . ? C24B N3B Ru1B 116.51(16) . . ? N1B C10B C11B 122.0(2) . . ? N1B C10B H10B 119.0 . . ? C11B C10B H10B 119.0 . . ? C12B C11B C10B 118.9(2) . . ? C12B C11B H11B 120.6 . . ? C10B C11B H11B 120.6 . . ? C11B C12B C13B 119.2(2) . . ? C11B C12B C40B 123.1(2) . . ? C13B C12B C40B 117.8(2) . . ? C14B C13B C12B 119.6(2) . . ? C14B C13B H13B 120.2 . . ? C12B C13B H13B 120.2 . . ? N1B C14B C13B 121.6(2) . . ? N1B C14B C15B 115.2(2) . . ? C13B C14B C15B 123.2(2) . . ? N2B C15B C16B 121.6(2) . . ? N2B C15B C14B 114.8(2) . . ? C16B C15B C14B 123.6(2) . . ? C15B C16B C17B 119.6(2) . . ? C15B C16B H16B 120.2 . . ? C17B C16B H16B 120.2 . . ? C16B C17B C18B 118.9(2) . . ? C16B C17B C50B 117.4(2) . . ? C18B C17B C50B 123.6(2) . . ? C19B C18B C17B 118.7(2) . . ? C19B C18B H18B 120.6 . . ? C17B C18B H18B 120.6 . . ? N2B C19B C18B 122.5(2) . . ? N2B C19B H19B 118.7 . . ? C18B C19B H19B 118.7 . . ? N6B C39B C38B 123.3(2) . . ? N6B C39B H39B 118.4 . . ? C38B C39B H39B 118.3 . . ? C39B C38B C37B 118.6(2) . . ? C39B C38B H38B 120.7 . . ? C37B C38B H38B 120.7 . . ? C36B C37B C38B 118.7(2) . . ? C36B C37B C90B 117.4(2) . . ? C38B C37B C90B 123.8(2) . . ? C37B C36B C35B 119.8(2) . . ? C37B C36B H35B 120.1 . . ? C35B C36B H35B 120.1 . . ? N6B C35B C36B 121.4(2) . . ? N6B C35B C34B 115.5(2) . . ? C36B C35B C34B 123.1(2) . . ? N5B C34B C33B 121.8(2) . . ? N5B C34B C35B 113.3(2) . . ? C33B C34B C35B 124.8(2) . . ? C34B C33B C32B 119.5(2) . . ? C34B C33B H33B 120.2 . . ? C32B C33B H33B 120.2 . . ? C33B C32B C31B 119.2(2) . . ? C33B C32B C80B 119.1(2) . . ? C31B C32B C80B 121.6(3) . . ? C30B C31B C32B 118.5(2) . . ? C30B C31B H31B 120.7 . . ? C32B C31B H31B 120.7 . . ? N5B C30B C31B 122.8(2) . . ? N5B C30B H30B 118.6 . . ? C31B C30B H30B 118.6 . . ? N4B C29B C28B 122.1(2) . . ? N4B C29B H29B 119.0 . . ? C28B C29B H29B 119.0 . . ? C29B C28B C27B 119.0(2) . . ? C29B C28B H28B 120.5 . . ? C27B C28B H28B 120.5 . . ? C26B C27B C28B 119.1(2) . . ? C26B C27B C70B 121.1(2) . . ? C28B C27B C70B 119.7(2) . . ? C27B C26B C25B 119.3(2) . . ? C27B C26B H26B 120.4 . . ? C25B C26B H26B 120.4 . . ? N4B C25B C26B 121.1(2) . . ? N4B C25B C24B 114.7(2) . . ? C26B C25B C24B 124.2(2) . . ? N3B C24B C23B 121.6(2) . . ? N3B C24B C25B 113.75(19) . . ? C23B C24B C25B 124.7(2) . . ? C24B C23B C22B 119.4(2) . . ? C24B C23B H23B 120.3 . . ? C22B C23B H23B 120.3 . . ? C21B C22B C23B 119.0(2) . . ? C21B C22B C60B 121.7(2) . . ? C23B C22B C60B 119.2(2) . . ? C22B C21B C20B 119.3(2) . . ? C22B C21B H21B 120.3 . . ? C20B C21B H21B 120.3 . . ? N3B C20B C21B 121.9(2) . . ? N3B C20B H20B 119.1 . . ? C21B C20B H20B 119.1 . . ? O41B C40B O40B 125.2(2) . . ? O41B C40B C12B 121.7(2) . . ? O40B C40B C12B 113.1(2) . . ? C40B O40B H40B 112.7 . . ? O51B C50B O50B 125.1(3) . . ? O51B C50B C17B 121.6(2) . . ? O50B C50B C17B 113.2(2) . . ? C50B O50B H50B 114.3 . . ? O91B C90B O90B 124.0(2) . . ? O91B C90B C37B 122.7(3) . . ? O90B C90B C37B 113.3(2) . . ? C90B O90B H60B 110.9 . . ? O81B C80B O80B 124.6(3) . . ? O81B C80B C32B 123.3(3) . . ? O80B C80B C32B 112.1(2) . . ? C80B O80B H70B 117.7 . . ? O71B C70B O70B 123.2(2) . . ? O71B C70B C27B 123.0(2) . . ? O70B C70B C27B 113.8(2) . . ? C70B O70B H80B 115.8 . . ? O61B C60B O60B 125.3(2) . . ? O61B C60B C22B 123.2(2) . . ? O60B C60B C22B 111.4(2) . . ? C60B O60B H90B 100.5 . . ? H941 O94 H942 129.2 . . ? H951 O95 H952 105.4 . . ? H961 O96 H962 105.6 . . ? H971 O97 H972 111.8 . . ? H981 O98 H982 117.1 . . ? H991 O99 H992 106.5 . . ? 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 C10 74.4(2) . . . . ? N5 Ru1 N1 C10 -3.2(2) . . . . ? N4 Ru1 N1 C10 -143(2) . . . . ? N3 Ru1 N1 C10 -101.7(2) . . . . ? N2 Ru1 N1 C10 175.0(2) . . . . ? N6 Ru1 N1 C15 -98.52(18) . . . . ? N5 Ru1 N1 C15 -176.16(18) . . . . ? N4 Ru1 N1 C15 44(2) . . . . ? N3 Ru1 N1 C15 85.39(18) . . . . ? N2 Ru1 N1 C15 2.07(17) . . . . ? N6 Ru1 N2 C19 -101.0(2) . . . . ? N5 Ru1 N2 C19 -157.8(11) . . . . ? N4 Ru1 N2 C19 -2.2(2) . . . . ? N3 Ru1 N2 C19 75.5(2) . . . . ? N1 Ru1 N2 C19 176.3(2) . . . . ? N6 Ru1 N2 C14 83.64(18) . . . . ? N5 Ru1 N2 C14 26.9(13) . . . . ? N4 Ru1 N2 C14 -177.56(17) . . . . ? N3 Ru1 N2 C14 -99.86(17) . . . . ? N1 Ru1 N2 C14 0.96(17) . . . . ? N5 Ru1 N6 C39 174.5(2) . . . . ? N4 Ru1 N6 C39 -103.4(2) . . . . ? N3 Ru1 N6 C39 -145.7(8) . . . . ? N1 Ru1 N6 C39 75.3(2) . . . . ? N2 Ru1 N6 C39 -2.1(2) . . . . ? N5 Ru1 N6 C35 -1.84(17) . . . . ? N4 Ru1 N6 C35 80.29(18) . . . . ? N3 Ru1 N6 C35 38.0(9) . . . . ? N1 Ru1 N6 C35 -101.03(18) . . . . ? N2 Ru1 N6 C35 -178.40(17) . . . . ? N6 Ru1 N5 C30 177.9(2) . . . . ? N4 Ru1 N5 C30 79.5(2) . . . . ? N3 Ru1 N5 C30 1.7(2) . . . . ? N1 Ru1 N5 C30 -99.1(2) . . . . ? N2 Ru1 N5 C30 -124.7(12) . . . . ? N6 Ru1 N5 C34 3.39(17) . . . . ? N4 Ru1 N5 C34 -95.03(18) . . . . ? N3 Ru1 N5 C34 -172.82(17) . . . . ? N1 Ru1 N5 C34 86.38(18) . . . . ? N2 Ru1 N5 C34 60.8(13) . . . . ? N6 Ru1 N4 C29 -3.2(2) . . . . ? N5 Ru1 N4 C29 74.4(2) . . . . ? N3 Ru1 N4 C29 172.8(2) . . . . ? N1 Ru1 N4 C29 -146(2) . . . . ? N2 Ru1 N4 C29 -103.9(2) . . . . ? N6 Ru1 N4 C25 -174.93(17) . . . . ? N5 Ru1 N4 C25 -97.33(18) . . . . ? N3 Ru1 N4 C25 1.03(17) . . . . ? N1 Ru1 N4 C25 42(2) . . . . ? N2 Ru1 N4 C25 84.35(18) . . . . ? N6 Ru1 N3 C20 -138.5(8) . . . . ? N5 Ru1 N3 C20 -99.3(2) . . . . ? N4 Ru1 N3 C20 178.6(2) . . . . ? N1 Ru1 N3 C20 0.0(2) . . . . ? N2 Ru1 N3 C20 77.5(2) . . . . ? N6 Ru1 N3 C24 44.6(9) . . . . ? N5 Ru1 N3 C24 83.80(17) . . . . ? N4 Ru1 N3 C24 1.64(16) . . . . ? N1 Ru1 N3 C24 -176.90(16) . . . . ? N2 Ru1 N3 C24 -99.45(17) . . . . ? C15 N1 C10 C11 -2.2(4) . . . . ? Ru1 N1 C10 C11 -175.0(2) . . . . ? N1 C10 C11 C12 1.5(4) . . . . ? C10 C11 C12 C13 0.6(4) . . . . ? C10 C11 C12 C40 -178.3(3) . . . . ? C11 C12 C13 C15 -1.8(4) . . . . ? C40 C12 C13 C15 177.2(2) . . . . ? C19 N2 C14 C16 1.5(4) . . . . ? Ru1 N2 C14 C16 177.18(19) . . . . ? C19 N2 C14 C15 -179.3(2) . . . . ? Ru1 N2 C14 C15 -3.6(3) . . . . ? C10 N1 C15 C13 0.9(4) . . . . ? Ru1 N1 C15 C13 174.37(19) . . . . ? C10 N1 C15 C14 -178.0(2) . . . . ? Ru1 N1 C15 C14 -4.6(3) . . . . ? C12 C13 C15 N1 1.0(4) . . . . ? C12 C13 C15 C14 179.9(2) . . . . ? N2 C14 C15 N1 5.4(3) . . . . ? C16 C14 C15 N1 -175.4(2) . . . . ? N2 C14 C15 C13 -173.6(2) . . . . ? C16 C14 C15 C13 5.6(4) . . . . ? N2 C14 C16 C17 -0.1(4) . . . . ? C15 C14 C16 C17 -179.2(2) . . . . ? C14 C16 C17 C18 -1.5(4) . . . . ? C14 C16 C17 C50 178.3(2) . . . . ? C16 C17 C18 C19 1.6(4) . . . . ? C50 C17 C18 C19 -178.2(3) . . . . ? C14 N2 C19 C18 -1.3(4) . . . . ? Ru1 N2 C19 C18 -176.53(19) . . . . ? C17 C18 C19 N2 -0.2(4) . . . . ? C35 N6 C39 C38 -2.3(4) . . . . ? Ru1 N6 C39 C38 -178.59(19) . . . . ? N6 C39 C38 C37 -1.7(4) . . . . ? C39 C38 C37 C36 3.9(4) . . . . ? C39 C38 C37 C90 -174.8(2) . . . . ? C38 C37 C36 C35 -2.2(4) . . . . ? C90 C37 C36 C35 176.5(2) . . . . ? C39 N6 C35 C36 4.1(4) . . . . ? Ru1 N6 C35 C36 -179.32(19) . . . . ? C39 N6 C35 C34 -176.4(2) . . . . ? Ru1 N6 C35 C34 0.2(3) . . . . ? C37 C36 C35 N6 -1.9(4) . . . . ? C37 C36 C35 C34 178.7(2) . . . . ? C30 N5 C34 C33 1.5(4) . . . . ? Ru1 N5 C34 C33 176.42(18) . . . . ? C30 N5 C34 C35 -179.2(2) . . . . ? Ru1 N5 C34 C35 -4.3(3) . . . . ? N6 C35 C34 N5 2.7(3) . . . . ? C36 C35 C34 N5 -177.9(2) . . . . ? N6 C35 C34 C33 -178.0(2) . . . . ? C36 C35 C34 C33 1.4(4) . . . . ? N5 C34 C33 C32 -1.1(4) . . . . ? C35 C34 C33 C32 179.7(2) . . . . ? C34 C33 C32 C31 -0.6(4) . . . . ? C34 C33 C32 C80 176.3(2) . . . . ? C33 C32 C31 C30 1.7(4) . . . . ? C80 C32 C31 C30 -175.1(3) . . . . ? C34 N5 C30 C31 -0.3(4) . . . . ? Ru1 N5 C30 C31 -174.8(2) . . . . ? C32 C31 C30 N5 -1.3(4) . . . . ? C25 N4 C29 C28 -0.2(4) . . . . ? Ru1 N4 C29 C28 -171.76(19) . . . . ? N4 C29 C28 C27 -1.8(4) . . . . ? C29 C28 C27 C26 2.1(4) . . . . ? C29 C28 C27 C70 -176.0(2) . . . . ? C28 C27 C26 C25 -0.6(4) . . . . ? C70 C27 C26 C25 177.7(2) . . . . ? C29 N4 C25 C26 1.8(4) . . . . ? Ru1 N4 C25 C26 174.09(19) . . . . ? C29 N4 C25 C24 -175.7(2) . . . . ? Ru1 N4 C25 C24 -3.4(3) . . . . ? C27 C26 C25 N4 -1.4(4) . . . . ? C27 C26 C25 C24 175.8(2) . . . . ? C20 N3 C24 C23 0.6(3) . . . . ? Ru1 N3 C24 C23 177.76(18) . . . . ? C20 N3 C24 C25 179.0(2) . . . . ? Ru1 N3 C24 C25 -3.9(3) . . . . ? N4 C25 C24 N3 4.7(3) . . . . ? C26 C25 C24 N3 -172.6(2) . . . . ? N4 C25 C24 C23 -177.0(2) . . . . ? C26 C25 C24 C23 5.7(4) . . . . ? N3 C24 C23 C22 -0.5(4) . . . . ? C25 C24 C23 C22 -178.7(2) . . . . ? C24 C23 C22 C21 0.3(4) . . . . ? C24 C23 C22 C60 -179.5(2) . . . . ? C23 C22 C21 C20 -0.3(4) . . . . ? C60 C22 C21 C20 179.5(3) . . . . ? C24 N3 C20 C21 -0.6(4) . . . . ? Ru1 N3 C20 C21 -177.4(2) . . . . ? C22 C21 C20 N3 0.5(4) . . . . ? C11 C12 C40 O41 -169.2(3) . . . . ? C13 C12 C40 O41 11.9(4) . . . . ? C11 C12 C40 O40 9.5(4) . . . . ? C13 C12 C40 O40 -169.4(2) . . . . ? C16 C17 C50 O51 5.5(4) . . . . ? C18 C17 C50 O51 -174.7(3) . . . . ? C16 C17 C50 O50 -176.1(3) . . . . ? C18 C17 C50 O50 3.7(4) . . . . ? C38 C37 C90 O90 -0.1(4) . . . . ? C36 C37 C90 O90 -178.8(3) . . . . ? C38 C37 C90 O91 179.4(2) . . . . ? C36 C37 C90 O91 0.7(3) . . . . ? C31 C32 C80 O81 162.3(3) . . . . ? C33 C32 C80 O81 -14.4(4) . . . . ? C31 C32 C80 O80 -15.1(4) . . . . ? C33 C32 C80 O80 168.1(2) . . . . ? C28 C27 C70 O71 174.5(3) . . . . ? C26 C27 C70 O71 -3.6(4) . . . . ? C28 C27 C70 O70 -5.3(4) . . . . ? C26 C27 C70 O70 176.6(2) . . . . ? C23 C22 C60 O61 -3.5(4) . . . . ? C21 C22 C60 O61 176.6(3) . . . . ? C23 C22 C60 O60 176.1(2) . . . . ? C21 C22 C60 O60 -3.7(4) . . . . ? N5B Ru1B N1B C10B -4.8(2) . . . . ? N4B Ru1B N1B C10B -151.1(7) . . . . ? N3B Ru1B N1B C10B -103.4(2) . . . . ? N2B Ru1B N1B C10B 174.3(2) . . . . ? N6B Ru1B N1B C10B 72.9(2) . . . . ? N5B Ru1B N1B C14B 177.89(16) . . . . ? N4B Ru1B N1B C14B 31.5(8) . . . . ? N3B Ru1B N1B C14B 79.23(17) . . . . ? N2B Ru1B N1B C14B -3.01(16) . . . . ? N6B Ru1B N1B C14B -104.46(17) . . . . ? N5B Ru1B N2B C19B -155(3) . . . . ? N4B Ru1B N2B C19B 1.4(2) . . . . ? N3B Ru1B N2B C19B 79.3(2) . . . . ? N1B Ru1B N2B C19B 177.6(2) . . . . ? N6B Ru1B N2B C19B -98.7(2) . . . . ? N5B Ru1B N2B C15B 33(3) . . . . ? N4B Ru1B N2B C15B -170.27(17) . . . . ? N3B Ru1B N2B C15B -92.36(17) . . . . ? N1B Ru1B N2B C15B 6.01(17) . . . . ? N6B Ru1B N2B C15B 89.64(17) . . . . ? N5B Ru1B N6B C39B 178.9(2) . . . . ? N4B Ru1B N6B C39B -96.7(2) . . . . ? N3B Ru1B N6B C39B -154.0(10) . . . . ? N2B Ru1B N6B C39B 0.5(2) . . . . ? N1B Ru1B N6B C39B 78.7(2) . . . . ? N5B Ru1B N6B C35B 3.98(17) . . . . ? N4B Ru1B N6B C35B 88.42(17) . . . . ? N3B Ru1B N6B C35B 31.1(11) . . . . ? N2B Ru1B N6B C35B -174.39(17) . . . . ? N1B Ru1B N6B C35B -96.19(17) . . . . ? N4B Ru1B N5B C30B 73.4(2) . . . . ? N3B Ru1B N5B C30B -4.6(2) . . . . ? N2B Ru1B N5B C30B -130(3) . . . . ? N1B Ru1B N5B C30B -103.0(2) . . . . ? N6B Ru1B N5B C30B 173.3(2) . . . . ? N4B Ru1B N5B C34B -100.87(18) . . . . ? N3B Ru1B N5B C34B -178.91(18) . . . . ? N2B Ru1B N5B C34B 56(3) . . . . ? N1B Ru1B N5B C34B 82.76(19) . . . . ? N6B Ru1B N5B C34B -1.02(18) . . . . ? N5B Ru1B N4B C29B 77.9(2) . . . . ? N3B Ru1B N4B C29B 176.1(2) . . . . ? N2B Ru1B N4B C29B -101.4(2) . . . . ? N1B Ru1B N4B C29B -135.4(7) . . . . ? N6B Ru1B N4B C29B 0.1(2) . . . . ? N5B Ru1B N4B C25B -100.45(18) . . . . ? N3B Ru1B N4B C25B -2.18(17) . . . . ? N2B Ru1B N4B C25B 80.32(18) . . . . ? N1B Ru1B N4B C25B 46.3(8) . . . . ? N6B Ru1B N4B C25B -178.23(17) . . . . ? N5B Ru1B N3B C20B -96.4(2) . . . . ? N4B Ru1B N3B C20B 178.8(2) . . . . ? N2B Ru1B N3B C20B 82.0(2) . . . . ? N1B Ru1B N3B C20B 3.7(2) . . . . ? N6B Ru1B N3B C20B -123.2(10) . . . . ? N5B Ru1B N3B C24B 89.30(18) . . . . ? N4B Ru1B N3B C24B 4.51(17) . . . . ? N2B Ru1B N3B C24B -92.28(18) . . . . ? N1B Ru1B N3B C24B -170.55(18) . . . . ? N6B Ru1B N3B C24B 62.5(11) . . . . ? C14B N1B C10B C11B -0.7(4) . . . . ? Ru1B N1B C10B C11B -177.99(19) . . . . ? N1B C10B C11B C12B -0.7(4) . . . . ? C10B C11B C12B C13B 1.6(4) . . . . ? C10B C11B C12B C40B -178.6(2) . . . . ? C11B C12B C13B C14B -1.1(4) . . . . ? C40B C12B C13B C14B 179.1(2) . . . . ? C10B N1B C14B C13B 1.3(3) . . . . ? Ru1B N1B C14B C13B 178.85(18) . . . . ? C10B N1B C14B C15B -177.7(2) . . . . ? Ru1B N1B C14B C15B -0.2(3) . . . . ? C12B C13B C14B N1B -0.4(4) . . . . ? C12B C13B C14B C15B 178.5(2) . . . . ? C19B N2B C15B C16B 1.3(4) . . . . ? Ru1B N2B C15B C16B 173.58(19) . . . . ? C19B N2B C15B C14B 179.9(2) . . . . ? Ru1B N2B C15B C14B -7.8(3) . . . . ? N1B C14B C15B N2B 5.2(3) . . . . ? C13B C14B C15B N2B -173.7(2) . . . . ? N1B C14B C15B C16B -176.2(2) . . . . ? C13B C14B C15B C16B 4.8(4) . . . . ? N2B C15B C16B C17B 2.2(4) . . . . ? C14B C15B C16B C17B -176.3(2) . . . . ? C15B C16B C17B C18B -3.1(4) . . . . ? C15B C16B C17B C50B 174.2(2) . . . . ? C16B C17B C18B C19B 0.7(4) . . . . ? C50B C17B C18B C19B -176.5(2) . . . . ? C15B N2B C19B C18B -3.9(4) . . . . ? Ru1B N2B C19B C18B -175.27(19) . . . . ? C17B C18B C19B N2B 2.9(4) . . . . ? C35B N6B C39B C38B -1.0(4) . . . . ? Ru1B N6B C39B C38B -175.8(2) . . . . ? N6B C39B C38B C37B 0.8(4) . . . . ? C39B C38B C37B C36B -0.1(4) . . . . ? C39B C38B C37B C90B -178.2(3) . . . . ? C38B C37B C36B C35B -0.4(4) . . . . ? C90B C37B C36B C35B 177.9(2) . . . . ? C39B N6B C35B C36B 0.6(4) . . . . ? Ru1B N6B C35B C36B 175.92(19) . . . . ? C39B N6B C35B C34B 178.5(2) . . . . ? Ru1B N6B C35B C34B -6.1(3) . . . . ? C37B C36B C35B N6B 0.1(4) . . . . ? C37B C36B C35B C34B -177.7(2) . . . . ? C30B N5B C34B C33B 1.5(4) . . . . ? Ru1B N5B C34B C33B 176.13(19) . . . . ? C30B N5B C34B C35B -176.5(2) . . . . ? Ru1B N5B C34B C35B -1.8(3) . . . . ? N6B C35B C34B N5B 5.2(3) . . . . ? C36B C35B C34B N5B -176.9(2) . . . . ? N6B C35B C34B C33B -172.6(2) . . . . ? C36B C35B C34B C33B 5.3(4) . . . . ? N5B C34B C33B C32B -0.5(4) . . . . ? C35B C34B C33B C32B 177.2(2) . . . . ? C34B C33B C32B C31B -0.8(4) . . . . ? C34B C33B C32B C80B 179.1(2) . . . . ? C33B C32B C31B C30B 1.1(4) . . . . ? C80B C32B C31B C30B -178.9(3) . . . . ? C34B N5B C30B C31B -1.2(4) . . . . ? Ru1B N5B C30B C31B -175.4(2) . . . . ? C32B C31B C30B N5B -0.1(4) . . . . ? C25B N4B C29B C28B -0.4(4) . . . . ? Ru1B N4B C29B C28B -178.62(18) . . . . ? N4B C29B C28B C27B -1.1(4) . . . . ? C29B C28B C27B C26B 1.6(4) . . . . ? C29B C28B C27B C70B -177.4(2) . . . . ? C28B C27B C26B C25B -0.6(4) . . . . ? C70B C27B C26B C25B 178.4(2) . . . . ? C29B N4B C25B C26B 1.4(4) . . . . ? Ru1B N4B C25B C26B 179.80(19) . . . . ? C29B N4B C25B C24B -178.7(2) . . . . ? Ru1B N4B C25B C24B -0.2(3) . . . . ? C27B C26B C25B N4B -0.9(4) . . . . ? C27B C26B C25B C24B 179.1(2) . . . . ? C20B N3B C24B C23B 0.1(4) . . . . ? Ru1B N3B C24B C23B 174.76(19) . . . . ? C20B N3B C24B C25B 179.5(2) . . . . ? Ru1B N3B C24B C25B -5.9(3) . . . . ? N4B C25B C24B N3B 4.0(3) . . . . ? C26B C25B C24B N3B -176.1(2) . . . . ? N4B C25B C24B C23B -176.7(2) . . . . ? C26B C25B C24B C23B 3.3(4) . . . . ? N3B C24B C23B C22B -1.0(4) . . . . ? C25B C24B C23B C22B 179.7(2) . . . . ? C24B C23B C22B C21B 1.0(4) . . . . ? C24B C23B C22B C60B 179.0(2) . . . . ? C23B C22B C21B C20B -0.2(4) . . . . ? C60B C22B C21B C20B -178.1(2) . . . . ? C24B N3B C20B C21B 0.8(4) . . . . ? Ru1B N3B C20B C21B -173.4(2) . . . . ? C22B C21B C20B N3B -0.8(4) . . . . ? C11B C12B C40B O41B 178.3(3) . . . . ? C13B C12B C40B O41B -1.9(4) . . . . ? C11B C12B C40B O40B -0.9(4) . . . . ? C13B C12B C40B O40B 179.0(2) . . . . ? C16B C17B C50B O51B 23.9(4) . . . . ? C18B C17B C50B O51B -158.9(3) . . . . ? C16B C17B C50B O50B -153.2(2) . . . . ? C18B C17B C50B O50B 24.0(4) . . . . ? C36B C37B C90B O91B 1.0(4) . . . . ? C38B C37B C90B O91B 179.1(3) . . . . ? C36B C37B C90B O90B -179.5(3) . . . . ? C38B C37B C90B O90B -1.4(4) . . . . ? C33B C32B C80B O81B 4.8(5) . . . . ? C31B C32B C80B O81B -175.2(3) . . . . ? C33B C32B C80B O80B -175.2(3) . . . . ? C31B C32B C80B O80B 4.8(4) . . . . ? C26B C27B C70B O71B -175.6(2) . . . . ? C28B C27B C70B O71B 3.3(4) . . . . ? C26B C27B C70B O70B 4.5(3) . . . . ? C28B C27B C70B O70B -176.5(2) . . . . ? C21B C22B C60B O61B 169.2(3) . . . . ? C23B C22B C60B O61B -8.7(4) . . . . ? C21B C22B C60B O60B -10.1(4) . . . . ? C23B C22B C60B O60B 172.0(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 O40 H40 Cl1 0.88 2.17 3.043(2) 173.4 . O60 H90 Cl2 0.99 2.03 3.001(2) 168.1 1_455 O91 H61 O98 0.85 1.72 2.546(3) 164.2 . O40B H40B Cl2 0.90 2.09 2.979(2) 167.8 . O80B H70B Cl3 0.89 2.12 3.014(2) 176.3 . O70B H80B O97 0.91 1.63 2.532(2) 174.6 . O60B H90B Cl4 0.79 2.27 2.9766(19) 147.8 . O94 H941 O91B 1.09 1.80 2.891(4) 175.7 . O95 H952 O96 0.75 1.98 2.699(3) 160.8 . O99 H991 O94 0.78 2.04 2.782(7) 160.4 . _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.738 _refine_diff_density_min -0.854 _refine_diff_density_rms 0.059 #===END========================================================================= data_Ru(H2dcbpy)2Br2.(H2O) (3) _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'Ru(H2dcbpy)2Br2.(H2O)' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H17 Br2 N4 O9 Ru' _chemical_formula_weight 766.31 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' 'Br' 'Br' -0.2901 2.4595 '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 'P 21/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 12.1882(2) _cell_length_b 11.27370(10) _cell_length_c 19.8150(3) _cell_angle_alpha 90.00 _cell_angle_beta 106.0100(10) _cell_angle_gamma 90.00 _cell_volume 2617.10(6) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'block' _exptl_crystal_colour 'black (dark red)' _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.945 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1500 _exptl_absorpt_coefficient_mu 3.714 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.4021 _exptl_absorpt_correction_T_max 0.7077 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Nonius KappaCCD' _diffrn_measurement_method 'phi/omega-scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9196 _diffrn_reflns_av_R_equivalents 0.0138 _diffrn_reflns_av_sigmaI/netI 0.0284 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.51 _diffrn_reflns_theta_max 25.25 _reflns_number_total 4730 _reflns_number_gt 4103 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius, 1999)' _computing_cell_refinement 'Denzo/Scalepack (Otwinowski & Minor, 1997)' _computing_data_reduction 'Denzo/Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP in SHELXTL v.5.1 (Bruker Axs, 1998)' _computing_publication_material 'SHELXL-97' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0325P)^2^+2.0649P] 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 4730 _refine_ls_number_parameters 370 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0340 _refine_ls_R_factor_gt 0.0274 _refine_ls_wR_factor_ref 0.0700 _refine_ls_wR_factor_gt 0.0663 _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 0.417758(18) 0.408993(19) 0.231607(11) 0.02354(8) Uani 1 1 d . . . Br2 Br 0.50240(3) 0.57898(3) 0.315950(15) 0.03300(9) Uani 1 1 d . . . Br1 Br 0.34187(3) 0.56932(3) 0.140346(16) 0.03662(10) Uani 1 1 d . . . N1 N 0.47521(19) 0.2953(2) 0.31168(12) 0.0270(5) Uani 1 1 d . . . N2 N 0.28405(19) 0.40931(19) 0.27549(12) 0.0265(5) Uani 1 1 d . . . N3 N 0.35758(18) 0.2830(2) 0.15751(12) 0.0251(5) Uani 1 1 d . . . N4 N 0.55401(19) 0.3887(2) 0.19106(12) 0.0268(5) Uani 1 1 d . . . C10 C 0.5729(3) 0.2342(3) 0.32389(15) 0.0338(7) Uani 1 1 d . . . H10 H 0.6122 0.2347 0.2898 0.041 Uiso 1 1 calc R . . C11 C 0.6175(3) 0.1710(3) 0.38411(16) 0.0345(7) Uani 1 1 d . . . H11 H 0.6863 0.1307 0.3910 0.041 Uiso 1 1 calc R . . C12 C 0.5581(2) 0.1679(2) 0.43493(15) 0.0290(6) Uani 1 1 d . . . C13 C 0.4548(2) 0.2273(2) 0.42225(14) 0.0285(6) Uani 1 1 d . . . H13 H 0.4129 0.2248 0.4550 0.034 Uiso 1 1 calc R . . C14 C 0.4145(2) 0.2907(2) 0.36019(14) 0.0263(6) Uani 1 1 d . . . C15 C 0.3049(2) 0.3544(2) 0.33924(14) 0.0261(6) Uani 1 1 d . . . C16 C 0.2258(2) 0.3550(2) 0.37778(14) 0.0273(6) Uani 1 1 d . . . H16 H 0.2426 0.3191 0.4217 0.033 Uiso 1 1 calc R . . C17 C 0.1206(2) 0.4102(2) 0.34982(15) 0.0288(6) Uani 1 1 d . . . C18 C 0.0989(2) 0.4628(3) 0.28445(15) 0.0336(7) Uani 1 1 d . . . H18 H 0.0287 0.4984 0.2643 0.040 Uiso 1 1 calc R . . C19 C 0.1819(2) 0.4619(3) 0.24948(15) 0.0322(6) Uani 1 1 d . . . H19 H 0.1669 0.4993 0.2060 0.039 Uiso 1 1 calc R . . C20 C 0.2557(2) 0.2278(3) 0.14504(15) 0.0293(6) Uani 1 1 d . . . H20 H 0.2124 0.2390 0.1765 0.035 Uiso 1 1 calc R . . C21 C 0.2131(2) 0.1554(3) 0.08778(15) 0.0304(6) Uani 1 1 d . . . H21 H 0.1429 0.1179 0.0813 0.037 Uiso 1 1 calc R . . C22 C 0.2764(2) 0.1391(3) 0.03977(15) 0.0286(6) Uani 1 1 d . . . C23 C 0.3832(2) 0.1911(3) 0.05352(15) 0.0293(6) Uani 1 1 d . . . H23 H 0.4284 0.1787 0.0233 0.035 Uiso 1 1 calc R . . C24 C 0.4227(2) 0.2619(2) 0.11271(14) 0.0269(6) Uani 1 1 d . . . C25 C 0.5364(2) 0.3165(2) 0.13369(14) 0.0273(6) Uani 1 1 d . . . C26 C 0.6220(2) 0.2936(3) 0.10180(15) 0.0311(6) Uani 1 1 d . . . H26 H 0.6080 0.2450 0.0624 0.037 Uiso 1 1 calc R . . C27 C 0.7289(2) 0.3439(3) 0.12927(15) 0.0301(6) Uani 1 1 d . . . C28 C 0.7468(3) 0.4154(3) 0.18868(16) 0.0376(7) Uani 1 1 d . . . H28 H 0.8181 0.4489 0.2086 0.045 Uiso 1 1 calc R . . C29 C 0.6585(3) 0.4358(3) 0.21747(16) 0.0351(7) Uani 1 1 d . . . H29 H 0.6714 0.4842 0.2569 0.042 Uiso 1 1 calc R . . C40 C 0.6066(2) 0.1035(3) 0.50179(15) 0.0303(6) Uani 1 1 d . . . O40 O 0.70336(19) 0.0502(2) 0.50342(12) 0.0448(6) Uani 1 1 d . . . O41 O 0.56488(19) 0.1016(2) 0.55050(11) 0.0406(5) Uani 1 1 d . . . C50 C 0.0364(3) 0.4084(3) 0.39201(17) 0.0359(7) Uani 1 1 d . . . O50 O -0.06046(19) 0.4627(3) 0.35977(13) 0.0580(7) Uani 1 1 d . . . O51 O 0.0548(2) 0.3657(3) 0.44876(13) 0.0639(8) Uani 1 1 d . . . C60 C 0.2322(3) 0.0675(3) -0.02559(16) 0.0329(7) Uani 1 1 d . . . O60 O 0.13191(19) 0.0202(2) -0.03038(12) 0.0456(6) Uani 1 1 d . . . O61 O 0.2808(2) 0.0583(3) -0.07021(13) 0.0562(7) Uani 1 1 d . . . C70 C 0.8206(2) 0.3217(3) 0.09409(15) 0.0327(7) Uani 1 1 d . . . O70 O 0.91632(17) 0.3777(2) 0.12536(11) 0.0397(5) Uani 1 1 d . . . O71 O 0.80694(19) 0.2608(2) 0.04243(12) 0.0473(6) Uani 1 1 d . . . O98 O 0.5584(8) 0.6010(8) 0.0590(6) 0.160(4) Uani 0.55 1 d P . . O99 O 0.6446(11) 0.7075(9) 0.1938(7) 0.165(5) Uani 0.45 1 d P . . H40 H 0.7379 0.0011 0.5479 0.050 Uiso 1 1 d . . . H50 H -0.1195 0.4585 0.3868 0.050 Uiso 1 1 d . . . H60 H 0.1039 -0.0197 -0.0735 0.050 Uiso 1 1 d . . . H70 H 0.9670 0.3649 0.0940 0.050 Uiso 1 1 d . . . H981 H 0.4765 0.5790 0.0489 0.050 Uiso 0.00 1 d P . . H982 H 0.6247 0.5436 0.0937 0.050 Uiso 0.00 1 d P . . H991 H 0.6818 0.7573 0.1707 0.050 Uiso 0.50 1 d P . . H992 H 0.6366 0.6402 0.1609 0.050 Uiso 0.50 1 d P . . 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 0.02308(13) 0.02757(13) 0.02110(13) -0.00026(8) 0.00798(9) 0.00035(8) Br2 0.03383(18) 0.03598(18) 0.02834(17) -0.00590(12) 0.00713(13) -0.00072(12) Br1 0.04199(19) 0.03335(17) 0.03020(17) 0.00450(12) 0.00275(14) -0.00110(13) N1 0.0262(12) 0.0317(13) 0.0248(12) -0.0015(10) 0.0098(10) 0.0003(10) N2 0.0268(13) 0.0288(12) 0.0241(12) 0.0006(9) 0.0074(10) 0.0002(9) N3 0.0229(12) 0.0274(12) 0.0265(12) 0.0020(10) 0.0092(10) 0.0010(9) N4 0.0262(12) 0.0311(12) 0.0243(12) -0.0008(10) 0.0089(10) -0.0009(10) C10 0.0374(17) 0.0389(17) 0.0294(15) 0.0055(13) 0.0161(13) 0.0089(13) C11 0.0329(16) 0.0365(17) 0.0378(17) 0.0032(13) 0.0158(14) 0.0104(13) C12 0.0280(15) 0.0277(15) 0.0309(15) 0.0019(12) 0.0073(12) 0.0022(11) C13 0.0277(15) 0.0333(15) 0.0265(14) 0.0021(12) 0.0110(12) 0.0003(12) C14 0.0256(14) 0.0265(14) 0.0282(14) -0.0002(11) 0.0097(12) -0.0006(11) C15 0.0254(14) 0.0254(14) 0.0278(14) -0.0002(11) 0.0081(12) -0.0017(11) C16 0.0275(15) 0.0294(14) 0.0255(14) 0.0007(12) 0.0081(12) 0.0000(11) C17 0.0239(15) 0.0336(16) 0.0310(15) -0.0023(12) 0.0108(12) -0.0020(11) C18 0.0232(15) 0.0457(18) 0.0311(15) 0.0050(14) 0.0060(12) 0.0040(13) C19 0.0293(15) 0.0397(16) 0.0259(14) 0.0070(13) 0.0049(12) 0.0053(13) C20 0.0278(15) 0.0328(15) 0.0307(15) 0.0019(12) 0.0139(12) -0.0006(12) C21 0.0248(15) 0.0309(15) 0.0367(16) 0.0022(12) 0.0105(13) -0.0029(11) C22 0.0272(15) 0.0296(15) 0.0302(15) 0.0005(12) 0.0098(12) -0.0011(11) C23 0.0259(14) 0.0351(16) 0.0291(15) -0.0051(12) 0.0113(12) -0.0028(12) C24 0.0245(14) 0.0308(15) 0.0262(14) 0.0003(12) 0.0084(12) 0.0010(11) C25 0.0274(15) 0.0315(15) 0.0236(14) -0.0006(11) 0.0080(12) -0.0027(12) C26 0.0292(15) 0.0377(16) 0.0284(15) -0.0060(12) 0.0114(12) -0.0041(12) C27 0.0254(15) 0.0384(16) 0.0284(15) -0.0014(12) 0.0107(12) -0.0026(12) C28 0.0283(16) 0.051(2) 0.0343(17) -0.0102(14) 0.0109(13) -0.0087(13) C29 0.0312(16) 0.0453(18) 0.0297(16) -0.0117(13) 0.0100(13) -0.0077(13) C40 0.0257(15) 0.0317(15) 0.0328(16) -0.0018(12) 0.0069(13) -0.0022(12) O40 0.0379(13) 0.0618(15) 0.0364(12) 0.0130(11) 0.0131(10) 0.0219(11) O41 0.0356(12) 0.0552(15) 0.0342(12) 0.0095(10) 0.0147(10) 0.0076(10) C50 0.0310(17) 0.0426(18) 0.0375(18) 0.0028(14) 0.0149(14) 0.0015(13) O50 0.0302(13) 0.100(2) 0.0507(15) 0.0210(14) 0.0221(11) 0.0188(13) O51 0.0474(15) 0.103(2) 0.0503(15) 0.0336(15) 0.0295(13) 0.0252(15) C60 0.0271(16) 0.0378(17) 0.0336(16) -0.0045(13) 0.0079(13) -0.0027(12) O60 0.0364(12) 0.0602(15) 0.0431(13) -0.0196(11) 0.0159(10) -0.0197(11) O61 0.0386(14) 0.091(2) 0.0461(14) -0.0275(13) 0.0231(12) -0.0216(13) C70 0.0296(16) 0.0385(17) 0.0316(16) 0.0000(13) 0.0112(13) -0.0019(13) O70 0.0272(11) 0.0553(14) 0.0395(12) -0.0094(11) 0.0139(9) -0.0077(10) O71 0.0389(13) 0.0651(16) 0.0435(13) -0.0192(12) 0.0206(11) -0.0106(11) O98 0.161(9) 0.139(8) 0.217(10) 0.095(7) 0.117(8) 0.059(6) O99 0.206(12) 0.076(6) 0.242(14) 0.014(8) 0.111(11) -0.025(7) _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 N1 2.009(2) . ? Ru1 N3 2.029(2) . ? Ru1 N4 2.047(2) . ? Ru1 N2 2.048(2) . ? Ru1 Br1 2.5436(4) . ? Ru1 Br2 2.5650(4) . ? N1 C10 1.339(4) . ? N1 C14 1.366(3) . ? N2 C19 1.346(4) . ? N2 C15 1.366(3) . ? N3 C20 1.349(3) . ? N3 C24 1.365(3) . ? N4 C29 1.346(4) . ? N4 C25 1.367(3) . ? C10 C11 1.367(4) . ? C10 H10 0.9300 . ? C11 C12 1.394(4) . ? C11 H11 0.9300 . ? C12 C13 1.386(4) . ? C12 C40 1.484(4) . ? C13 C14 1.390(4) . ? C13 H13 0.9300 . ? C14 C15 1.471(4) . ? C15 C16 1.386(4) . ? C16 C17 1.395(4) . ? C16 H16 0.9300 . ? C17 C18 1.382(4) . ? C17 C50 1.492(4) . ? C18 C19 1.375(4) . ? C18 H18 0.9300 . ? C19 H19 0.9300 . ? C20 C21 1.378(4) . ? C20 H20 0.9300 . ? C21 C22 1.392(4) . ? C21 H21 0.9300 . ? C22 C23 1.385(4) . ? C22 C60 1.495(4) . ? C23 C24 1.390(4) . ? C23 H23 0.9300 . ? C24 C25 1.468(4) . ? C25 C26 1.385(4) . ? C26 C27 1.387(4) . ? C26 H26 0.9300 . ? C27 C28 1.393(4) . ? C27 C70 1.492(4) . ? C28 C29 1.369(4) . ? C28 H28 0.9300 . ? C29 H29 0.9300 . ? C40 O41 1.209(3) . ? C40 O40 1.316(3) . ? O40 H40 1.0273 . ? C50 O51 1.187(4) . ? C50 O50 1.327(4) . ? O50 H50 1.0098 . ? C60 O61 1.197(4) . ? C60 O60 1.313(4) . ? O60 H60 0.9425 . ? C70 O71 1.205(4) . ? C70 O70 1.321(4) . ? O70 H70 1.0001 . ? O98 H981 0.9943 . ? O98 H982 1.1127 . ? O99 H991 0.9189 . ? O99 H992 0.9868 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ru1 N3 95.90(9) . . ? N1 Ru1 N4 95.46(9) . . ? N3 Ru1 N4 78.96(9) . . ? N1 Ru1 N2 79.08(9) . . ? N3 Ru1 N2 97.89(9) . . ? N4 Ru1 N2 173.45(9) . . ? N1 Ru1 Br1 173.61(6) . . ? N3 Ru1 Br1 89.71(6) . . ? N4 Ru1 Br1 88.60(6) . . ? N2 Ru1 Br1 97.17(6) . . ? N1 Ru1 Br2 88.39(7) . . ? N3 Ru1 Br2 174.07(6) . . ? N4 Ru1 Br2 96.60(7) . . ? N2 Ru1 Br2 86.92(6) . . ? Br1 Ru1 Br2 86.235(12) . . ? C10 N1 C14 118.7(2) . . ? C10 N1 Ru1 124.75(18) . . ? C14 N1 Ru1 116.18(18) . . ? C19 N2 C15 118.1(2) . . ? C19 N2 Ru1 126.74(19) . . ? C15 N2 Ru1 115.13(18) . . ? C20 N3 C24 118.1(2) . . ? C20 N3 Ru1 125.90(18) . . ? C24 N3 Ru1 115.72(18) . . ? C29 N4 C25 118.3(2) . . ? C29 N4 Ru1 125.94(19) . . ? C25 N4 Ru1 115.75(18) . . ? N1 C10 C11 123.1(3) . . ? N1 C10 H10 118.4 . . ? C11 C10 H10 118.4 . . ? C10 C11 C12 118.8(3) . . ? C10 C11 H11 120.6 . . ? C12 C11 H11 120.6 . . ? C13 C12 C11 119.0(3) . . ? C13 C12 C40 121.1(3) . . ? C11 C12 C40 119.9(3) . . ? C12 C13 C14 119.4(2) . . ? C12 C13 H13 120.3 . . ? C14 C13 H13 120.3 . . ? N1 C14 C13 120.9(2) . . ? N1 C14 C15 114.1(2) . . ? C13 C14 C15 125.0(2) . . ? N2 C15 C16 121.8(2) . . ? N2 C15 C14 113.9(2) . . ? C16 C15 C14 124.2(2) . . ? C15 C16 C17 119.1(3) . . ? C15 C16 H16 120.4 . . ? C17 C16 H16 120.4 . . ? C18 C17 C16 118.8(3) . . ? C18 C17 C50 123.2(3) . . ? C16 C17 C50 118.1(3) . . ? C19 C18 C17 119.4(3) . . ? C19 C18 H18 120.3 . . ? C17 C18 H18 120.3 . . ? N2 C19 C18 122.8(3) . . ? N2 C19 H19 118.6 . . ? C18 C19 H19 118.6 . . ? N3 C20 C21 122.9(2) . . ? N3 C20 H20 118.5 . . ? C21 C20 H20 118.5 . . ? C20 C21 C22 119.1(3) . . ? C20 C21 H21 120.4 . . ? C22 C21 H21 120.4 . . ? C23 C22 C21 118.5(3) . . ? C23 C22 C60 119.5(2) . . ? C21 C22 C60 121.9(3) . . ? C22 C23 C24 119.8(3) . . ? C22 C23 H23 120.1 . . ? C24 C23 H23 120.1 . . ? N3 C24 C23 121.4(2) . . ? N3 C24 C25 114.5(2) . . ? C23 C24 C25 124.0(2) . . ? N4 C25 C26 121.7(3) . . ? N4 C25 C24 113.9(2) . . ? C26 C25 C24 124.3(2) . . ? C25 C26 C27 119.3(3) . . ? C25 C26 H26 120.4 . . ? C27 C26 H26 120.4 . . ? C26 C27 C28 118.6(3) . . ? C26 C27 C70 119.4(3) . . ? C28 C27 C70 121.9(3) . . ? C29 C28 C27 119.5(3) . . ? C29 C28 H28 120.3 . . ? C27 C28 H28 120.3 . . ? N4 C29 C28 122.7(3) . . ? N4 C29 H29 118.7 . . ? C28 C29 H29 118.7 . . ? O41 C40 O40 122.9(3) . . ? O41 C40 C12 124.7(3) . . ? O40 C40 C12 112.3(2) . . ? C40 O40 H40 114.8 . . ? O51 C50 O50 123.7(3) . . ? O51 C50 C17 123.8(3) . . ? O50 C50 C17 112.5(3) . . ? C50 O50 H50 113.1 . . ? O61 C60 O60 123.5(3) . . ? O61 C60 C22 123.6(3) . . ? O60 C60 C22 112.8(2) . . ? C60 O60 H60 110.9 . . ? O71 C70 O70 124.6(3) . . ? O71 C70 C27 123.1(3) . . ? O70 C70 C27 112.3(2) . . ? C70 O70 H70 104.9 . . ? H981 O98 H982 119.8 . . ? H991 O99 H992 96.5 . . ? 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 N3 Ru1 N1 C10 78.5(2) . . . . ? N4 Ru1 N1 C10 -0.9(2) . . . . ? N2 Ru1 N1 C10 175.5(3) . . . . ? Br1 Ru1 N1 C10 -130.1(5) . . . . ? Br2 Ru1 N1 C10 -97.4(2) . . . . ? N3 Ru1 N1 C14 -108.2(2) . . . . ? N4 Ru1 N1 C14 172.4(2) . . . . ? N2 Ru1 N1 C14 -11.30(19) . . . . ? Br1 Ru1 N1 C14 43.1(7) . . . . ? Br2 Ru1 N1 C14 75.87(19) . . . . ? N1 Ru1 N2 C19 -172.7(3) . . . . ? N3 Ru1 N2 C19 -78.2(2) . . . . ? N4 Ru1 N2 C19 -139.0(7) . . . . ? Br1 Ru1 N2 C19 12.5(2) . . . . ? Br2 Ru1 N2 C19 98.3(2) . . . . ? N1 Ru1 N2 C15 10.46(19) . . . . ? N3 Ru1 N2 C15 104.99(19) . . . . ? N4 Ru1 N2 C15 44.2(8) . . . . ? Br1 Ru1 N2 C15 -164.31(18) . . . . ? Br2 Ru1 N2 C15 -78.50(18) . . . . ? N1 Ru1 N3 C20 82.3(2) . . . . ? N4 Ru1 N3 C20 176.8(2) . . . . ? N2 Ru1 N3 C20 2.6(2) . . . . ? Br1 Ru1 N3 C20 -94.6(2) . . . . ? Br2 Ru1 N3 C20 -141.4(5) . . . . ? N1 Ru1 N3 C24 -104.14(19) . . . . ? N4 Ru1 N3 C24 -9.71(19) . . . . ? N2 Ru1 N3 C24 176.11(19) . . . . ? Br1 Ru1 N3 C24 78.91(18) . . . . ? Br2 Ru1 N3 C24 32.1(7) . . . . ? N1 Ru1 N4 C29 -75.8(3) . . . . ? N3 Ru1 N4 C29 -170.7(3) . . . . ? N2 Ru1 N4 C29 -109.0(8) . . . . ? Br1 Ru1 N4 C29 99.3(2) . . . . ? Br2 Ru1 N4 C29 13.2(2) . . . . ? N1 Ru1 N4 C25 101.3(2) . . . . ? N3 Ru1 N4 C25 6.36(19) . . . . ? N2 Ru1 N4 C25 68.1(8) . . . . ? Br1 Ru1 N4 C25 -83.62(19) . . . . ? Br2 Ru1 N4 C25 -169.66(18) . . . . ? C14 N1 C10 C11 -2.8(4) . . . . ? Ru1 N1 C10 C11 170.3(2) . . . . ? N1 C10 C11 C12 1.2(5) . . . . ? C10 C11 C12 C13 1.1(4) . . . . ? C10 C11 C12 C40 -177.9(3) . . . . ? C11 C12 C13 C14 -1.6(4) . . . . ? C40 C12 C13 C14 177.4(3) . . . . ? C10 N1 C14 C13 2.2(4) . . . . ? Ru1 N1 C14 C13 -171.4(2) . . . . ? C10 N1 C14 C15 -176.0(3) . . . . ? Ru1 N1 C14 C15 10.3(3) . . . . ? C12 C13 C14 N1 -0.1(4) . . . . ? C12 C13 C14 C15 178.0(3) . . . . ? C19 N2 C15 C16 -1.9(4) . . . . ? Ru1 N2 C15 C16 175.2(2) . . . . ? C19 N2 C15 C14 174.9(2) . . . . ? Ru1 N2 C15 C14 -8.0(3) . . . . ? N1 C14 C15 N2 -1.3(3) . . . . ? C13 C14 C15 N2 -179.5(3) . . . . ? N1 C14 C15 C16 175.4(3) . . . . ? C13 C14 C15 C16 -2.8(4) . . . . ? N2 C15 C16 C17 1.9(4) . . . . ? C14 C15 C16 C17 -174.6(3) . . . . ? C15 C16 C17 C18 -0.1(4) . . . . ? C15 C16 C17 C50 179.3(3) . . . . ? C16 C17 C18 C19 -1.6(5) . . . . ? C50 C17 C18 C19 179.0(3) . . . . ? C15 N2 C19 C18 0.2(4) . . . . ? Ru1 N2 C19 C18 -176.5(2) . . . . ? C17 C18 C19 N2 1.6(5) . . . . ? C24 N3 C20 C21 -2.8(4) . . . . ? Ru1 N3 C20 C21 170.6(2) . . . . ? N3 C20 C21 C22 -0.9(4) . . . . ? C20 C21 C22 C23 3.6(4) . . . . ? C20 C21 C22 C60 -176.4(3) . . . . ? C21 C22 C23 C24 -2.7(4) . . . . ? C60 C22 C23 C24 177.3(3) . . . . ? C20 N3 C24 C23 3.7(4) . . . . ? Ru1 N3 C24 C23 -170.4(2) . . . . ? C20 N3 C24 C25 -174.6(2) . . . . ? Ru1 N3 C24 C25 11.4(3) . . . . ? C22 C23 C24 N3 -1.0(4) . . . . ? C22 C23 C24 C25 177.1(3) . . . . ? C29 N4 C25 C26 -1.6(4) . . . . ? Ru1 N4 C25 C26 -178.9(2) . . . . ? C29 N4 C25 C24 175.1(3) . . . . ? Ru1 N4 C25 C24 -2.3(3) . . . . ? N3 C24 C25 N4 -5.9(3) . . . . ? C23 C24 C25 N4 175.9(3) . . . . ? N3 C24 C25 C26 170.7(3) . . . . ? C23 C24 C25 C26 -7.6(5) . . . . ? N4 C25 C26 C27 0.9(4) . . . . ? C24 C25 C26 C27 -175.4(3) . . . . ? C25 C26 C27 C28 0.5(4) . . . . ? C25 C26 C27 C70 -178.6(3) . . . . ? C26 C27 C28 C29 -1.2(5) . . . . ? C70 C27 C28 C29 177.9(3) . . . . ? C25 N4 C29 C28 0.9(5) . . . . ? Ru1 N4 C29 C28 177.9(2) . . . . ? C27 C28 C29 N4 0.5(5) . . . . ? C13 C12 C40 O41 -3.5(5) . . . . ? C11 C12 C40 O41 175.5(3) . . . . ? C13 C12 C40 O40 178.3(3) . . . . ? C11 C12 C40 O40 -2.7(4) . . . . ? C18 C17 C50 O51 -178.5(3) . . . . ? C16 C17 C50 O51 2.1(5) . . . . ? C18 C17 C50 O50 -0.1(4) . . . . ? C16 C17 C50 O50 -179.5(3) . . . . ? C23 C22 C60 O61 -5.3(5) . . . . ? C21 C22 C60 O61 174.7(3) . . . . ? C23 C22 C60 O60 177.7(3) . . . . ? C21 C22 C60 O60 -2.3(4) . . . . ? C26 C27 C70 O71 -0.5(5) . . . . ? C28 C27 C70 O71 -179.5(3) . . . . ? C26 C27 C70 O70 178.5(3) . . . . ? C28 C27 C70 O70 -0.6(4) . . . . ? 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 O99 H991 O50 0.92 2.72 3.140(11) 108.5 2 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.25 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.369 _refine_diff_density_min -0.686 _refine_diff_density_rms 0.075 #===END=========================================================================