# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/2037 data_global # 1. SUBMISSION DETAILS _publ_contact_author ; K. Mereiter Institute of Mineralogy, Crystallography and Structural Chemistry Technical University of Vienna Getreidemarkt 9 A-1060 Vienna Austria ; _publ_contact_author_phone '++43 1 58801-17111' _publ_contact_author_fax '++43 1 58801-17199' _publ_contact_author_email 'Kurt.Mereiter+e171@tuwien.ac.at' _publ_requested_journal 'J. Chem. Soc. Dalton Trans.' _publ_requested_coeditor_name ? _publ_contact_letter ; The subsequent crystal structure data are to be deposited in context with a publication in J. Chem. Soc. Dalton Transactions. The paper contains and this CIF contains **four** crystal structures with the following CIF-codes: kinx304 compound 1 in text kipi431 compound 4 in text kiny305 compound 5 in text kipx478 compound 6.CHCl~3~ in text Journal J. Chem. Soc. Dalton Trans. Title Synthesis and characterization of ruthenium 8-quinolinate complexes. Unexpected formation of a \k^1^-hydrido tris(pyrazolyl)borate complex. Authors C. Gemel, R. John, C. Slugovc, K. Mereiter, R. Schmid, K. Kirchner Superscript, subscript, greek and umlaut characters in this CIF-file are in accordance with IUCR CIF conventions (Acta Cryst. C53 (1997) 147-162). Yours sincerely, Kurt Mereiter Vienna, 15.3.2000 ; #====== kinx304 compound 1 in text ================== data_kinx304 _audit_creation_method SHELXL _chemical_name_systematic ; chloro-(8-hydroxyquinolinato-N,O)-(eta$6!-p-cymene)-ruthenium(II) ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C19 H20 Cl N O Ru' _chemical_formula_weight 414.88 _chemical_melting_point ? _chemical_compound_source ? 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 P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.757(2) _cell_length_b 13.287(3) _cell_length_c 12.309(2) _cell_angle_alpha 90.00 _cell_angle_beta 102.97(1) _cell_angle_gamma 90.00 _cell_volume 1714.4(6) _cell_formula_units_Z 4 _cell_measurement_temperature 300(2) _cell_measurement_reflns_used 18 _cell_measurement_theta_min 16 _cell_measurement_theta_max 25 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.607 _exptl_crystal_density_method ? _exptl_crystal_F_000 840 _exptl_absorpt_coefficient_mu 1.074 _exptl_absorpt_correction_type 'sphere' _exptl_absorpt_correction_T_min 0.79 _exptl_absorpt_correction_T_max 0.80 _exptl_absorpt_process_details ? _exptl_special_details ; Philips PW1100 four-circle diffractometer with szintillation detector, Mo Kalfa radiation, sealed X-ray tube, graphite monochromator, omega-twotheta scans, scan width in omega = [0.9 + 0.33 x tan(theta)] deg., stationary background. 3 reference reflections each 120 minutes, fluctutations +/-0.7%. Goniometer control program Philips PW1100 (internal) and SERVER4 (external PC program; author H. V\"ollenkle, Vienna University of Technology, 1990, unpublished). Raw data evaluation with program PW114 (K. Mereiter, Vienna University of Technology, 1990, unpublished). Lattice parameters by least-squares refinement of the +/- omega angles of 18 reflections, theta = 16 to 25 deg, program LLSQ4 (K. Mereiter, Vienna University of Technology, 1990, unpublished). Crystal sphere-like in shape. Therefore correction for absorption of a sphere, transmission factors 0.79 to 0.80. Data reduction with program XPREP (Siemens/Bruker). ; _diffrn_ambient_temperature 300(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 'Philips PW1100 four circle diffractometer' _diffrn_measurement_method 'omega-2theta-scans' _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 120 _diffrn_standards_decay_% 0.7 _diffrn_reflns_number 3164 _diffrn_reflns_av_R_equivalents 0.0128 _diffrn_reflns_av_sigmaI/netI 0.0201 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.28 _diffrn_reflns_theta_max 24.99 _reflns_number_total 3023 _reflns_number_observed 2629 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Philips PW1100 and SERVER4 (V\"ollenkle, 1990)' _computing_cell_refinement 'LLSQ4 (Mereiter, 1990)' _computing_data_reduction 'PW114 (Mereiter, 1990) and Siemens XPREP' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; 1) 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. 2) H(2), H(3), H(5), and H(6) were refined in x,y,z with a C-H distance restrained at 0.93 Angstroems; All other H atoms inserted in idealized positions and refined riding with the atoms to which they were bonded. The methyl group C(7)H~3~ was allowed to rotate about the C-C bond (AFIX 137 of program SHELXL97). All hydrogens had U~iso~ = U~eq~ x 1.2 (x 1.5 for CH~3~) of their carrier atoms. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0183P)^2^+0.7299P] 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 SHELXL _refine_ls_extinction_coef 0.00027(12) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 3012 _refine_ls_number_parameters 222 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0272 _refine_ls_R_factor_obs 0.0202 _refine_ls_wR_factor_all 0.0483 _refine_ls_wR_factor_obs 0.0431 _refine_ls_goodness_of_fit_all 1.037 _refine_ls_goodness_of_fit_obs 1.049 _refine_ls_restrained_S_all 1.091 _refine_ls_restrained_S_obs 1.048 _refine_ls_shift/esd_max -0.002 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Ru Ru 0.09744(2) 0.176600(12) 0.580745(13) 0.03200(7) Uani 1 d . . Cl Cl -0.12499(5) 0.22301(4) 0.51915(5) 0.04391(14) Uani 1 d . . C1 C 0.2535(2) 0.0697(2) 0.6257(2) 0.0446(6) Uani 1 d . . C2 C 0.1373(2) 0.0188(2) 0.6276(2) 0.0442(6) Uani 1 d D . H2 H 0.1138(22) -0.0358(11) 0.5802(16) 0.053 Uiso 1 d D . C3 C 0.0534(2) 0.0566(2) 0.6878(2) 0.0422(6) Uani 1 d D . H3 H -0.0261(11) 0.0265(17) 0.6801(19) 0.051 Uiso 1 d D . C4 C 0.0798(2) 0.1465(2) 0.7527(2) 0.0383(5) Uani 1 d . . C5 C 0.1966(2) 0.1950(2) 0.7536(2) 0.0398(5) Uani 1 d D . H5 H 0.2173(22) 0.2541(9) 0.7942(16) 0.048 Uiso 1 d D . C6 C 0.2826(2) 0.1570(2) 0.6913(2) 0.0430(6) Uani 1 d D . H6 H 0.3572(13) 0.1923(16) 0.6909(21) 0.052 Uiso 1 d D . C7 C 0.3361(3) 0.0343(2) 0.5499(2) 0.0664(8) Uani 1 d . . H7A H 0.2833(3) 0.0070(14) 0.4830(8) 0.100 Uiso 1 calc R . H7B H 0.3934(14) -0.0167(11) 0.5870(7) 0.100 Uiso 1 calc R . H7C H 0.3843(15) 0.0900(4) 0.5314(14) 0.100 Uiso 1 calc R . C8 C -0.0160(2) 0.1844(2) 0.8152(2) 0.0485(6) Uani 1 d . . H8 H -0.1010(2) 0.1669(2) 0.7713(2) 0.058 Uiso 1 calc R . C9 C -0.0132(3) 0.2970(2) 0.8327(3) 0.0779(9) Uani 1 d . . H9A H -0.0765(3) 0.3155(2) 0.8730(3) 0.117 Uiso 1 calc R . H9B H -0.0308(3) 0.3303(2) 0.7617(3) 0.117 Uiso 1 calc R . H9C H 0.0696(3) 0.3167(2) 0.8746(3) 0.117 Uiso 1 calc R . C10 C 0.0026(3) 0.1291(3) 0.9264(2) 0.0805(10) Uani 1 d . . H10A H -0.0585(3) 0.1532(3) 0.9665(2) 0.121 Uiso 1 calc R . H10B H 0.0873(3) 0.1412(3) 0.9696(2) 0.121 Uiso 1 calc R . H10C H -0.0094(3) 0.0582(3) 0.9131(2) 0.121 Uiso 1 calc R . N N 0.1319(2) 0.32124(13) 0.52662(14) 0.0369(4) Uani 1 d . . O O 0.0944(2) 0.15012(11) 0.41419(12) 0.0429(4) Uani 1 d . . C11 C 0.1497(2) 0.4056(2) 0.5850(2) 0.0474(6) Uani 1 d . . H11 H 0.1513(2) 0.4032(2) 0.6608(2) 0.057 Uiso 1 calc R . C12 C 0.1661(3) 0.4984(2) 0.5362(2) 0.0540(7) Uani 1 d . . H12 H 0.1771(3) 0.5566(2) 0.5794(2) 0.065 Uiso 1 calc R . C13 C 0.1661(2) 0.5038(2) 0.4261(2) 0.0529(7) Uani 1 d . . H13 H 0.1777(2) 0.5653(2) 0.3939(2) 0.063 Uiso 1 calc R . C14 C 0.1483(2) 0.4157(2) 0.3610(2) 0.0440(6) Uani 1 d . . C15 C 0.1486(2) 0.4115(2) 0.2465(2) 0.0560(7) Uani 1 d . . H15 H 0.1601(2) 0.4698(2) 0.2082(2) 0.067 Uiso 1 calc R . C16 C 0.1320(3) 0.3216(2) 0.1925(2) 0.0584(7) Uani 1 d . . H16 H 0.1336(3) 0.3199(2) 0.1173(2) 0.070 Uiso 1 calc R . C17 C 0.1126(2) 0.2312(2) 0.2453(2) 0.0494(6) Uani 1 d . . H17 H 0.1012(2) 0.1714(2) 0.2051(2) 0.059 Uiso 1 calc R . C18 C 0.1104(2) 0.2313(2) 0.3583(2) 0.0385(5) Uani 1 d . . C19 C 0.1301(2) 0.3248(2) 0.4148(2) 0.0361(5) Uani 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 Ru 0.03918(11) 0.02693(10) 0.02631(10) -0.00047(7) -0.00020(7) -0.00333(8) Cl 0.0426(3) 0.0417(3) 0.0418(3) 0.0015(3) -0.0025(2) 0.0024(3) C1 0.0495(14) 0.0409(13) 0.0393(12) 0.0069(11) 0.0011(11) 0.0115(11) C2 0.060(2) 0.0272(12) 0.0389(12) 0.0027(10) -0.0025(11) 0.0010(11) C3 0.0500(14) 0.0367(13) 0.0348(12) 0.0080(10) -0.0011(11) -0.0077(11) C4 0.0427(13) 0.0397(13) 0.0283(11) 0.0046(9) -0.0012(9) -0.0026(10) C5 0.0440(13) 0.0397(13) 0.0286(11) -0.0013(10) -0.0069(9) -0.0044(10) C6 0.0366(12) 0.0485(15) 0.0383(12) 0.0038(11) -0.0036(10) -0.0031(11) C7 0.070(2) 0.067(2) 0.063(2) 0.002(2) 0.0190(15) 0.023(2) C8 0.0467(14) 0.062(2) 0.0345(12) 0.0044(12) 0.0044(10) -0.0017(12) C9 0.097(3) 0.071(2) 0.074(2) -0.010(2) 0.036(2) 0.015(2) C10 0.089(2) 0.105(3) 0.056(2) 0.026(2) 0.033(2) 0.015(2) N 0.0424(10) 0.0329(10) 0.0326(9) 0.0014(8) 0.0023(8) -0.0042(8) O 0.0596(10) 0.0356(9) 0.0313(8) -0.0054(7) 0.0056(7) -0.0002(7) C11 0.061(2) 0.0368(13) 0.0409(13) -0.0070(10) 0.0046(11) -0.0088(11) C12 0.064(2) 0.0341(13) 0.061(2) -0.0036(12) 0.0063(13) -0.0107(12) C13 0.052(2) 0.0385(14) 0.064(2) 0.0129(12) 0.0055(13) -0.0057(11) C14 0.0355(12) 0.0464(14) 0.0484(14) 0.0119(11) 0.0055(10) -0.0009(10) C15 0.055(2) 0.067(2) 0.0474(15) 0.0208(14) 0.0144(12) 0.0026(14) C16 0.058(2) 0.084(2) 0.0360(13) 0.0125(14) 0.0160(12) 0.006(2) C17 0.0510(15) 0.062(2) 0.0340(12) -0.0034(12) 0.0065(11) 0.0081(13) C18 0.0355(12) 0.0449(14) 0.0334(11) 0.0021(10) 0.0038(9) 0.0038(10) C19 0.0340(11) 0.0387(12) 0.0340(11) 0.0042(10) 0.0042(9) 0.0003(10) _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 Ru O 2.0731(15) . ? Ru N 2.094(2) . ? Ru C6 2.162(2) . ? Ru C5 2.170(2) . ? Ru C1 2.173(2) . ? Ru C3 2.187(2) . ? Ru C2 2.191(2) . ? Ru C4 2.203(2) . ? Ru Cl 2.4219(7) . ? C1 C6 1.408(3) . ? C1 C2 1.426(4) . ? C1 C7 1.501(4) . ? C2 C3 1.385(4) . ? C2 H2 0.9299(11) . ? C3 C4 1.429(3) . ? C3 H3 0.9300(11) . ? C4 C5 1.410(3) . ? C4 C8 1.505(3) . ? C5 C6 1.421(4) . ? C5 H5 0.9299(11) . ? C6 H6 0.9300(11) . ? C7 H7A 0.96 . ? C7 H7B 0.96 . ? C7 H7C 0.96 . ? C8 C9 1.511(4) . ? C8 C10 1.526(3) . ? C8 H8 0.98 . ? C9 H9A 0.96 . ? C9 H9B 0.96 . ? C9 H9C 0.96 . ? C10 H10A 0.96 . ? C10 H10B 0.96 . ? C10 H10C 0.96 . ? N C11 1.322(3) . ? N C19 1.373(3) . ? O C18 1.311(3) . ? C11 C12 1.401(3) . ? C11 H11 0.93 . ? C12 C13 1.356(4) . ? C12 H12 0.93 . ? C13 C14 1.407(4) . ? C13 H13 0.93 . ? C14 C15 1.411(3) . ? C14 C19 1.412(3) . ? C15 C16 1.359(4) . ? C15 H15 0.93 . ? C16 C17 1.403(4) . ? C16 H16 0.93 . ? C17 C18 1.396(3) . ? C17 H17 0.93 . ? C18 C19 1.417(3) . ? 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 O Ru N 78.80(6) . . ? O Ru C6 114.20(8) . . ? N Ru C6 96.13(8) . . ? O Ru C5 152.16(8) . . ? N Ru C5 97.19(8) . . ? C6 Ru C5 38.30(9) . . ? O Ru C1 88.90(8) . . ? N Ru C1 119.92(9) . . ? C6 Ru C1 37.91(9) . . ? C5 Ru C1 69.05(9) . . ? O Ru C3 120.99(8) . . ? N Ru C3 159.77(8) . . ? C6 Ru C3 80.01(9) . . ? C5 Ru C3 67.45(9) . . ? C1 Ru C3 68.27(9) . . ? O Ru C2 93.25(8) . . ? N Ru C2 157.48(9) . . ? C6 Ru C2 67.73(9) . . ? C5 Ru C2 79.97(9) . . ? C1 Ru C2 38.15(9) . . ? C3 Ru C2 36.87(9) . . ? O Ru C4 158.97(7) . . ? N Ru C4 122.12(8) . . ? C6 Ru C4 68.84(9) . . ? C5 Ru C4 37.60(9) . . ? C1 Ru C4 82.22(9) . . ? C3 Ru C4 37.98(8) . . ? C2 Ru C4 68.12(9) . . ? O Ru Cl 86.48(5) . . ? N Ru Cl 84.25(5) . . ? C6 Ru Cl 159.06(7) . . ? C5 Ru Cl 120.79(7) . . ? C1 Ru Cl 153.94(7) . . ? C3 Ru Cl 92.39(7) . . ? C2 Ru Cl 116.55(7) . . ? C4 Ru Cl 93.16(6) . . ? C6 C1 C2 117.7(2) . . ? C6 C1 C7 121.9(2) . . ? C2 C1 C7 120.3(2) . . ? C6 C1 Ru 70.60(13) . . ? C2 C1 Ru 71.61(13) . . ? C7 C1 Ru 125.3(2) . . ? C3 C2 C1 121.0(2) . . ? C3 C2 Ru 71.40(13) . . ? C1 C2 Ru 70.25(13) . . ? C3 C2 H2 120.1(15) . . ? C1 C2 H2 118.4(15) . . ? Ru C2 H2 124.9(15) . . ? C2 C3 C4 122.0(2) . . ? C2 C3 Ru 71.73(14) . . ? C4 C3 Ru 71.62(13) . . ? C2 C3 H3 118.9(15) . . ? C4 C3 H3 118.7(15) . . ? Ru C3 H3 124.8(15) . . ? C5 C4 C3 116.9(2) . . ? C5 C4 C8 123.6(2) . . ? C3 C4 C8 119.4(2) . . ? C5 C4 Ru 69.92(12) . . ? C3 C4 Ru 70.40(12) . . ? C8 C4 Ru 130.3(2) . . ? C4 C5 C6 121.3(2) . . ? C4 C5 Ru 72.48(12) . . ? C6 C5 Ru 70.54(13) . . ? C4 C5 H5 119.7(15) . . ? C6 C5 H5 118.9(15) . . ? Ru C5 H5 128.9(15) . . ? C1 C6 C5 120.9(2) . . ? C1 C6 Ru 71.50(13) . . ? C5 C6 Ru 71.16(13) . . ? C1 C6 H6 119.6(16) . . ? C5 C6 H6 119.4(16) . . ? Ru C6 H6 127.6(15) . . ? C1 C7 H7A 109.5(2) . . ? C1 C7 H7B 109.47(14) . . ? H7A C7 H7B 109.5 . . ? C1 C7 H7C 109.5(2) . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C4 C8 C9 114.2(2) . . ? C4 C8 C10 109.4(2) . . ? C9 C8 C10 110.7(2) . . ? C4 C8 H8 107.43(12) . . ? C9 C8 H8 107.4(2) . . ? C10 C8 H8 107.4(2) . . ? C8 C9 H9A 109.5(2) . . ? C8 C9 H9B 109.5(2) . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5(2) . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C8 C10 H10A 109.5(2) . . ? C8 C10 H10B 109.5(2) . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.5(2) . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C11 N C19 118.9(2) . . ? C11 N Ru 128.3(2) . . ? C19 N Ru 112.78(14) . . ? C18 O Ru 113.87(13) . . ? N C11 C12 122.0(2) . . ? N C11 H11 118.99(13) . . ? C12 C11 H11 118.99(15) . . ? C13 C12 C11 120.2(2) . . ? C13 C12 H12 119.91(15) . . ? C11 C12 H12 119.91(15) . . ? C12 C13 C14 119.7(2) . . ? C12 C13 H13 120.15(15) . . ? C14 C13 H13 120.15(14) . . ? C13 C14 C15 124.9(2) . . ? C13 C14 C19 117.4(2) . . ? C15 C14 C19 117.8(2) . . ? C16 C15 C14 119.6(2) . . ? C16 C15 H15 120.20(15) . . ? C14 C15 H15 120.2(2) . . ? C15 C16 C17 122.9(2) . . ? C15 C16 H16 118.57(15) . . ? C17 C16 H16 118.6(2) . . ? C18 C17 C16 119.9(2) . . ? C18 C17 H17 120.0(2) . . ? C16 C17 H17 120.0(2) . . ? O C18 C17 123.8(2) . . ? O C18 C19 119.1(2) . . ? C17 C18 C19 117.1(2) . . ? N C19 C14 121.8(2) . . ? N C19 C18 115.4(2) . . ? C14 C19 C18 122.8(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O Ru C1 C6 133.80(15) . . . . ? N Ru C1 C6 57.4(2) . . . . ? C6 Ru C1 C6 0.0 . . . . ? C5 Ru C1 C6 -28.83(14) . . . . ? C3 Ru C1 C6 -102.0(2) . . . . ? C2 Ru C1 C6 -129.5(2) . . . . ? C4 Ru C1 C6 -65.31(15) . . . . ? Cl Ru C1 C6 -146.53(14) . . . . ? O Ru C1 C2 -96.68(14) . . . . ? N Ru C1 C2 -173.07(12) . . . . ? C6 Ru C1 C2 129.5(2) . . . . ? C5 Ru C1 C2 100.69(15) . . . . ? C3 Ru C1 C2 27.52(13) . . . . ? C2 Ru C1 C2 0.0 . . . . ? C4 Ru C1 C2 64.21(14) . . . . ? Cl Ru C1 C2 -17.0(2) . . . . ? O Ru C1 C7 17.9(2) . . . . ? N Ru C1 C7 -58.5(3) . . . . ? C6 Ru C1 C7 -115.9(3) . . . . ? C5 Ru C1 C7 -144.7(3) . . . . ? C3 Ru C1 C7 142.1(3) . . . . ? C2 Ru C1 C7 114.6(3) . . . . ? C4 Ru C1 C7 178.8(2) . . . . ? Cl Ru C1 C7 97.6(3) . . . . ? C6 C1 C2 C3 3.0(3) . . . . ? C7 C1 C2 C3 -173.0(2) . . . . ? Ru C1 C2 C3 -52.3(2) . . . . ? C6 C1 C2 Ru 55.3(2) . . . . ? C7 C1 C2 Ru -120.7(2) . . . . ? Ru C1 C2 Ru 0.0 . . . . ? O Ru C2 C3 -141.62(14) . . . . ? N Ru C2 C3 150.2(2) . . . . ? C6 Ru C2 C3 103.5(2) . . . . ? C5 Ru C2 C3 65.58(14) . . . . ? C1 Ru C2 C3 134.3(2) . . . . ? C3 Ru C2 C3 0.0 . . . . ? C4 Ru C2 C3 28.34(13) . . . . ? Cl Ru C2 C3 -53.94(14) . . . . ? O Ru C2 C1 84.06(14) . . . . ? N Ru C2 C1 15.8(3) . . . . ? C6 Ru C2 C1 -30.81(14) . . . . ? C5 Ru C2 C1 -68.74(14) . . . . ? C1 Ru C2 C1 0.0 . . . . ? C3 Ru C2 C1 -134.3(2) . . . . ? C4 Ru C2 C1 -105.98(15) . . . . ? Cl Ru C2 C1 171.74(11) . . . . ? C1 C2 C3 C4 -1.5(3) . . . . ? Ru C2 C3 C4 -53.3(2) . . . . ? C1 C2 C3 Ru 51.8(2) . . . . ? Ru C2 C3 Ru 0.0 . . . . ? O Ru C3 C2 46.3(2) . . . . ? N Ru C3 C2 -146.5(2) . . . . ? C6 Ru C3 C2 -66.01(15) . . . . ? C5 Ru C3 C2 -103.9(2) . . . . ? C1 Ru C3 C2 -28.41(14) . . . . ? C2 Ru C3 C2 0.0 . . . . ? C4 Ru C3 C2 -134.3(2) . . . . ? Cl Ru C3 C2 133.63(13) . . . . ? O Ru C3 C4 -179.40(12) . . . . ? N Ru C3 C4 -12.2(3) . . . . ? C6 Ru C3 C4 68.28(14) . . . . ? C5 Ru C3 C4 30.44(14) . . . . ? C1 Ru C3 C4 105.89(15) . . . . ? C2 Ru C3 C4 134.3(2) . . . . ? C4 Ru C3 C4 0.0 . . . . ? Cl Ru C3 C4 -92.07(13) . . . . ? C2 C3 C4 C5 -0.6(3) . . . . ? Ru C3 C4 C5 -53.9(2) . . . . ? C2 C3 C4 C8 179.3(2) . . . . ? Ru C3 C4 C8 126.0(2) . . . . ? C2 C3 C4 Ru 53.3(2) . . . . ? Ru C3 C4 Ru 0.0 . . . . ? O Ru C4 C5 131.4(2) . . . . ? N Ru C4 C5 -55.0(2) . . . . ? C6 Ru C4 C5 28.77(14) . . . . ? C5 Ru C4 C5 0.0 . . . . ? C1 Ru C4 C5 65.54(14) . . . . ? C3 Ru C4 C5 129.9(2) . . . . ? C2 Ru C4 C5 102.4(2) . . . . ? Cl Ru C4 C5 -140.23(13) . . . . ? O Ru C4 C3 1.4(3) . . . . ? N Ru C4 C3 175.03(13) . . . . ? C6 Ru C4 C3 -101.2(2) . . . . ? C5 Ru C4 C3 -129.9(2) . . . . ? C1 Ru C4 C3 -64.39(14) . . . . ? C3 Ru C4 C3 0.0 . . . . ? C2 Ru C4 C3 -27.57(14) . . . . ? Cl Ru C4 C3 89.84(13) . . . . ? O Ru C4 C8 -111.0(3) . . . . ? N Ru C4 C8 62.6(2) . . . . ? C6 Ru C4 C8 146.4(2) . . . . ? C5 Ru C4 C8 117.6(3) . . . . ? C1 Ru C4 C8 -176.9(2) . . . . ? C3 Ru C4 C8 -112.5(3) . . . . ? C2 Ru C4 C8 -140.0(2) . . . . ? Cl Ru C4 C8 -22.6(2) . . . . ? C3 C4 C5 C6 1.1(3) . . . . ? C8 C4 C5 C6 -178.8(2) . . . . ? Ru C4 C5 C6 -53.1(2) . . . . ? C3 C4 C5 Ru 54.1(2) . . . . ? C8 C4 C5 Ru -125.8(2) . . . . ? Ru C4 C5 Ru 0.0 . . . . ? O Ru C5 C4 -144.8(2) . . . . ? N Ru C5 C4 135.60(14) . . . . ? C6 Ru C5 C4 -133.6(2) . . . . ? C1 Ru C5 C4 -105.1(2) . . . . ? C3 Ru C5 C4 -30.73(14) . . . . ? C2 Ru C5 C4 -67.00(14) . . . . ? C4 Ru C5 C4 0.0 . . . . ? Cl Ru C5 C4 48.03(15) . . . . ? O Ru C5 C6 -11.2(2) . . . . ? N Ru C5 C6 -90.79(14) . . . . ? C6 Ru C5 C6 0.0 . . . . ? C1 Ru C5 C6 28.55(14) . . . . ? C3 Ru C5 C6 102.9(2) . . . . ? C2 Ru C5 C6 66.60(15) . . . . ? C4 Ru C5 C6 133.6(2) . . . . ? Cl Ru C5 C6 -178.37(11) . . . . ? C2 C1 C6 C5 -2.5(3) . . . . ? C7 C1 C6 C5 173.4(2) . . . . ? Ru C1 C6 C5 53.3(2) . . . . ? C2 C1 C6 Ru -55.8(2) . . . . ? C7 C1 C6 Ru 120.1(2) . . . . ? Ru C1 C6 Ru 0.0 . . . . ? C4 C5 C6 C1 0.5(3) . . . . ? Ru C5 C6 C1 -53.4(2) . . . . ? C4 C5 C6 Ru 53.9(2) . . . . ? Ru C5 C6 Ru 0.0 . . . . ? O Ru C6 C1 -52.3(2) . . . . ? N Ru C6 C1 -132.74(14) . . . . ? C5 Ru C6 C1 133.4(2) . . . . ? C1 Ru C6 C1 0.0 . . . . ? C3 Ru C6 C1 67.32(15) . . . . ? C2 Ru C6 C1 30.99(14) . . . . ? C4 Ru C6 C1 105.1(2) . . . . ? Cl Ru C6 C1 137.3(2) . . . . ? O Ru C6 C5 174.30(12) . . . . ? N Ru C6 C5 93.85(14) . . . . ? C5 Ru C6 C5 0.000(1) . . . . ? C1 Ru C6 C5 -133.4(2) . . . . ? C3 Ru C6 C5 -66.09(14) . . . . ? C2 Ru C6 C5 -102.4(2) . . . . ? C4 Ru C6 C5 -28.28(13) . . . . ? Cl Ru C6 C5 3.9(3) . . . . ? C5 C4 C8 C9 28.0(3) . . . . ? C3 C4 C8 C9 -151.9(2) . . . . ? Ru C4 C8 C9 -63.4(3) . . . . ? C5 C4 C8 C10 -96.7(3) . . . . ? C3 C4 C8 C10 83.4(3) . . . . ? Ru C4 C8 C10 171.9(2) . . . . ? O Ru N C11 179.6(2) . . . . ? C6 Ru N C11 -66.9(2) . . . . ? C5 Ru N C11 -28.3(2) . . . . ? C1 Ru N C11 -98.2(2) . . . . ? C3 Ru N C11 10.8(4) . . . . ? C2 Ru N C11 -109.4(3) . . . . ? C4 Ru N C11 2.0(2) . . . . ? Cl Ru N C11 92.1(2) . . . . ? O Ru N C19 2.19(14) . . . . ? C6 Ru N C19 115.7(2) . . . . ? C5 Ru N C19 154.3(2) . . . . ? C1 Ru N C19 84.3(2) . . . . ? C3 Ru N C19 -166.6(2) . . . . ? C2 Ru N C19 73.1(2) . . . . ? C4 Ru N C19 -175.47(14) . . . . ? Cl Ru N C19 -85.35(14) . . . . ? N Ru O C18 -1.92(15) . . . . ? C6 Ru O C18 -93.7(2) . . . . ? C5 Ru O C18 -86.1(2) . . . . ? C1 Ru O C18 -122.7(2) . . . . ? C3 Ru O C18 173.59(15) . . . . ? C2 Ru O C18 -160.7(2) . . . . ? C4 Ru O C18 172.6(2) . . . . ? Cl Ru O C18 82.91(14) . . . . ? C19 N C11 C12 0.3(4) . . . . ? Ru N C11 C12 -177.0(2) . . . . ? N C11 C12 C13 -1.0(4) . . . . ? C11 C12 C13 C14 0.6(4) . . . . ? C12 C13 C14 C15 -178.8(2) . . . . ? C12 C13 C14 C19 0.5(4) . . . . ? C13 C14 C15 C16 179.1(3) . . . . ? C19 C14 C15 C16 -0.1(4) . . . . ? C14 C15 C16 C17 0.8(4) . . . . ? C15 C16 C17 C18 -0.3(4) . . . . ? Ru O C18 C17 179.5(2) . . . . ? Ru O C18 C19 1.4(3) . . . . ? C16 C17 C18 O -179.1(2) . . . . ? C16 C17 C18 C19 -0.9(3) . . . . ? C11 N C19 C14 0.8(3) . . . . ? Ru N C19 C14 178.5(2) . . . . ? C11 N C19 C18 -179.9(2) . . . . ? Ru N C19 C18 -2.2(2) . . . . ? C13 C14 C19 N -1.2(3) . . . . ? C15 C14 C19 N 178.2(2) . . . . ? C13 C14 C19 C18 179.5(2) . . . . ? C15 C14 C19 C18 -1.1(3) . . . . ? O C18 C19 N 0.6(3) . . . . ? C17 C18 C19 N -177.7(2) . . . . ? O C18 C19 C14 179.9(2) . . . . ? C17 C18 C19 C14 1.6(3) . . . . ? _refine_diff_density_max 0.210 _refine_diff_density_min -0.284 _refine_diff_density_rms 0.044 #===END #====== kipi431 compound 4 in text ================== data_kipi431 _audit_creation_method SHELXL-97 _chemical_name_systematic ; trans(O,O),cis(N,N)-bis(8-hydroxyquinolinato-N,O)-(eta$4!-cyclo-octa- 1,5-diene)-ruthenium(II) ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H24 N2 O2 Ru' _chemical_formula_weight 497.54 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 P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.412(4) _cell_length_b 12.927(5) _cell_length_c 19.141(8) _cell_angle_alpha 90.00 _cell_angle_beta 92.47(2) _cell_angle_gamma 90.00 _cell_volume 2079.5(15) _cell_formula_units_Z 4 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 8192 _cell_measurement_theta_min 2 _cell_measurement_theta_max 25 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.589 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1016 _exptl_absorpt_coefficient_mu 0.781 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.90 _exptl_absorpt_correction_T_max 0.98 _exptl_absorpt_process_details ? _exptl_special_details ; Siemens SMART platform 3-circle diffractometer with CCD area detector, sealed X-ray tube, graphite monochromator. One complete sphere of the reciprocal space up to theta(max) = 25 deg was measured by omega scan frames with delta(omega) = 0.30 deg and 30 sec per frame, 4 x 606 frames recorded using program SMART (Siemens/Bruker). Frame data evaluation with program SAINT (Siemens/Bruker); lattice parameters by least-squares refinement of the geometric parameters of the strongest reflections. Correction for absorption and crystal decay (insignificant) by semi-empirical method from equivalents (multi-scan method) using program SADABS (G.M. Sheldrick, 1996, Univ. of Goettingen, Germany). Data reduction with program XPREP (Siemens/Bruker). ; _diffrn_ambient_temperature 295(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 'Siemens SMART 3-circle with CCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16365 _diffrn_reflns_av_R_equivalents 0.0346 _diffrn_reflns_av_sigmaI/netI 0.0287 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.90 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3651 _reflns_number_gt 2938 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART' _computing_cell_refinement 'Siemens SAINT' _computing_data_reduction 'Siemens SAINT and SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; 1) 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. 2) All hydrogen atoms inserted in idealized positions and refined riding with the atoms to which they were bonded. All hydrogen atoms had U~iso~ = U~eq~ x 1.2 of their carrier atoms. ; _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^)+(0.0259P)^2^+1.5178P] 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 SHELXL _refine_ls_extinction_coef 0.00027(16) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 3651 _refine_ls_number_parameters 281 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0434 _refine_ls_R_factor_gt 0.0290 _refine_ls_wR_factor_ref 0.0697 _refine_ls_wR_factor_gt 0.0623 _refine_ls_goodness_of_fit_ref 1.096 _refine_ls_restrained_S_all 1.096 _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 Ru Ru 0.71595(3) 0.256331(17) 0.364765(11) 0.02968(9) Uani 1 1 d . . . O1 O 0.5019(2) 0.30000(15) 0.31423(10) 0.0364(5) Uani 1 1 d . . . O2 O 0.8871(2) 0.23414(16) 0.44598(11) 0.0413(5) Uani 1 1 d . . . N1 N 0.6869(3) 0.40408(18) 0.40727(12) 0.0339(6) Uani 1 1 d . . . N2 N 0.5766(3) 0.18953(18) 0.44020(13) 0.0346(6) Uani 1 1 d . . . C1 C 0.9312(4) 0.3067(2) 0.31467(17) 0.0407(8) Uani 1 1 d . . . H1 H 0.9760 0.3714 0.3336 0.049 Uiso 1 1 calc R . . C2 C 0.8052(4) 0.3205(2) 0.26761(16) 0.0385(7) Uani 1 1 d . . . H2 H 0.7765 0.3931 0.2593 0.046 Uiso 1 1 calc R . . C3 C 0.7704(4) 0.2503(3) 0.20559(17) 0.0513(9) Uani 1 1 d . . . H3A H 0.8704 0.2234 0.1897 0.062 Uiso 1 1 calc R . . H3B H 0.7221 0.2910 0.1678 0.062 Uiso 1 1 calc R . . C4 C 0.6610(5) 0.1592(3) 0.22031(17) 0.0516(9) Uani 1 1 d . . . H4A H 0.5522 0.1788 0.2077 0.062 Uiso 1 1 calc R . . H4B H 0.6888 0.1015 0.1908 0.062 Uiso 1 1 calc R . . C5 C 0.6699(4) 0.1245(2) 0.29565(17) 0.0426(8) Uani 1 1 d . . . H5 H 0.5796 0.0819 0.3087 0.051 Uiso 1 1 calc R . . C6 C 0.8087(4) 0.1053(2) 0.33523(18) 0.0429(8) Uani 1 1 d . . . H6 H 0.7983 0.0516 0.3709 0.052 Uiso 1 1 calc R . . C7 C 0.9734(4) 0.1129(3) 0.3065(2) 0.0574(10) Uani 1 1 d . . . H7A H 1.0421 0.0627 0.3303 0.069 Uiso 1 1 calc R . . H7B H 0.9667 0.0948 0.2573 0.069 Uiso 1 1 calc R . . C8 C 1.0486(4) 0.2184(3) 0.3142(2) 0.0555(10) Uani 1 1 d . . . H8A H 1.1191 0.2290 0.2761 0.067 Uiso 1 1 calc R . . H8B H 1.1129 0.2201 0.3575 0.067 Uiso 1 1 calc R . . C9 C 0.7823(4) 0.4546(2) 0.45187(17) 0.0440(8) Uani 1 1 d . . . H9 H 0.8756 0.4229 0.4686 0.053 Uiso 1 1 calc R . . C10 C 0.7472(5) 0.5549(3) 0.47490(18) 0.0512(9) Uani 1 1 d . . . H10 H 0.8170 0.5889 0.5061 0.061 Uiso 1 1 calc R . . C11 C 0.6111(5) 0.6020(3) 0.45146(18) 0.0512(9) Uani 1 1 d . . . H11 H 0.5879 0.6684 0.4668 0.061 Uiso 1 1 calc R . . C12 C 0.5046(4) 0.5515(2) 0.40420(16) 0.0398(8) Uani 1 1 d . . . C13 C 0.3607(4) 0.5923(3) 0.37770(19) 0.0520(9) Uani 1 1 d . . . H13 H 0.3294 0.6584 0.3905 0.062 Uiso 1 1 calc R . . C14 C 0.2663(4) 0.5348(3) 0.3330(2) 0.0532(9) Uani 1 1 d . . . H14 H 0.1694 0.5620 0.3166 0.064 Uiso 1 1 calc R . . C15 C 0.3106(4) 0.4359(3) 0.31083(17) 0.0446(8) Uani 1 1 d . . . H15 H 0.2434 0.3993 0.2799 0.054 Uiso 1 1 calc R . . C16 C 0.4532(3) 0.3921(2) 0.33435(15) 0.0322(7) Uani 1 1 d . . . C17 C 0.5495(3) 0.4507(2) 0.38244(14) 0.0322(7) Uani 1 1 d . . . C18 C 0.4243(4) 0.1654(2) 0.43464(17) 0.0414(8) Uani 1 1 d . . . H18 H 0.3679 0.1779 0.3926 0.050 Uiso 1 1 calc R . . C19 C 0.3448(4) 0.1212(3) 0.49052(19) 0.0491(9) Uani 1 1 d . . . H19 H 0.2376 0.1042 0.4851 0.059 Uiso 1 1 calc R . . C20 C 0.4249(5) 0.1036(2) 0.55222(19) 0.0515(9) Uani 1 1 d . . . H20 H 0.3718 0.0755 0.5894 0.062 Uiso 1 1 calc R . . C21 C 0.5881(4) 0.1277(2) 0.56059(17) 0.0433(8) Uani 1 1 d . . . C22 C 0.6826(5) 0.1137(3) 0.62218(18) 0.0549(10) Uani 1 1 d . . . H22 H 0.6385 0.0853 0.6616 0.066 Uiso 1 1 calc R . . C23 C 0.8399(5) 0.1418(3) 0.62415(19) 0.0587(10) Uani 1 1 d . . . H23 H 0.9001 0.1343 0.6657 0.070 Uiso 1 1 calc R . . C24 C 0.9123(4) 0.1815(3) 0.56557(18) 0.0519(9) Uani 1 1 d . . . H24 H 1.0199 0.1982 0.5686 0.062 Uiso 1 1 calc R . . C25 C 0.8261(4) 0.1962(2) 0.50281(16) 0.0399(7) Uani 1 1 d . . . C26 C 0.6614(4) 0.1699(2) 0.50153(15) 0.0354(7) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru 0.02876(14) 0.02847(14) 0.03202(14) -0.00018(11) 0.00390(9) 0.00111(11) O1 0.0337(11) 0.0358(11) 0.0394(12) -0.0044(9) -0.0025(9) 0.0002(9) O2 0.0339(11) 0.0499(13) 0.0400(12) 0.0069(10) 0.0002(9) 0.0043(10) N1 0.0328(14) 0.0343(13) 0.0347(14) -0.0011(11) 0.0037(11) -0.0008(11) N2 0.0368(15) 0.0306(13) 0.0370(14) -0.0015(11) 0.0079(11) 0.0026(11) C1 0.0342(18) 0.0407(18) 0.0480(19) 0.0004(15) 0.0110(15) -0.0079(14) C2 0.0424(19) 0.0357(17) 0.0383(17) 0.0049(14) 0.0113(14) -0.0023(14) C3 0.055(2) 0.062(2) 0.0367(17) 0.0033(17) 0.0085(15) -0.0059(18) C4 0.066(2) 0.046(2) 0.043(2) -0.0125(16) 0.0034(17) -0.0059(17) C5 0.051(2) 0.0283(16) 0.049(2) -0.0088(14) 0.0121(16) -0.0050(15) C6 0.051(2) 0.0266(16) 0.053(2) 0.0009(14) 0.0172(16) 0.0038(14) C7 0.052(2) 0.043(2) 0.079(3) 0.0002(19) 0.018(2) 0.0134(17) C8 0.0346(19) 0.064(2) 0.069(2) 0.0058(19) 0.0124(17) 0.0066(17) C9 0.0431(19) 0.0455(19) 0.0431(19) -0.0079(15) -0.0009(15) -0.0051(15) C10 0.065(2) 0.045(2) 0.043(2) -0.0133(16) 0.0019(17) -0.0117(18) C11 0.071(3) 0.0333(18) 0.051(2) -0.0083(16) 0.0178(19) -0.0045(17) C12 0.051(2) 0.0300(16) 0.0393(18) 0.0045(13) 0.0174(15) 0.0020(14) C13 0.059(2) 0.0386(19) 0.060(2) 0.0030(17) 0.0170(19) 0.0150(17) C14 0.044(2) 0.055(2) 0.062(2) 0.0163(19) 0.0160(18) 0.0190(17) C15 0.0361(18) 0.052(2) 0.0461(19) 0.0074(16) 0.0033(15) 0.0027(15) C16 0.0318(16) 0.0325(16) 0.0329(16) 0.0041(12) 0.0072(12) 0.0020(13) C17 0.0351(17) 0.0302(16) 0.0321(16) 0.0051(12) 0.0090(13) -0.0001(12) C18 0.0399(19) 0.0375(17) 0.047(2) -0.0052(15) 0.0083(15) -0.0007(14) C19 0.048(2) 0.0415(19) 0.059(2) -0.0117(17) 0.0205(18) -0.0111(16) C20 0.075(3) 0.0334(18) 0.048(2) -0.0045(15) 0.0277(19) -0.0068(17) C21 0.062(2) 0.0260(16) 0.0428(19) -0.0019(14) 0.0164(16) 0.0017(15) C22 0.089(3) 0.0401(19) 0.036(2) 0.0054(15) 0.0090(19) 0.0007(19) C23 0.085(3) 0.053(2) 0.038(2) 0.0072(17) -0.0064(19) 0.017(2) C24 0.053(2) 0.056(2) 0.046(2) -0.0005(17) -0.0069(17) 0.0126(17) C25 0.0433(19) 0.0354(17) 0.0412(18) 0.0000(14) 0.0044(14) 0.0104(14) C26 0.0485(19) 0.0248(15) 0.0331(16) -0.0016(12) 0.0051(14) 0.0052(13) _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 Ru O1 2.085(2) . ? Ru N2 2.086(2) . ? Ru O2 2.093(2) . ? Ru N1 2.094(2) . ? Ru C5 2.182(3) . ? Ru C1 2.184(3) . ? Ru C6 2.186(3) . ? Ru C2 2.198(3) . ? O1 C16 1.321(3) . ? O2 C25 1.317(4) . ? N1 C9 1.319(4) . ? N1 C17 1.370(4) . ? N2 C18 1.318(4) . ? N2 C26 1.371(4) . ? C1 C2 1.373(4) . ? C1 C8 1.509(5) . ? C1 H1 0.9800 . ? C2 C3 1.513(4) . ? C2 H2 0.9800 . ? C3 C4 1.528(5) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 C5 1.509(5) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C6 1.386(5) . ? C5 H5 0.9800 . ? C6 C7 1.516(5) . ? C6 H6 0.9800 . ? C7 C8 1.508(5) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.405(5) . ? C9 H9 0.9300 . ? C10 C11 1.356(5) . ? C10 H10 0.9300 . ? C11 C12 1.406(5) . ? C11 H11 0.9300 . ? C12 C13 1.396(5) . ? C12 C17 1.424(4) . ? C13 C14 1.363(5) . ? C13 H13 0.9300 . ? C14 C15 1.402(5) . ? C14 H14 0.9300 . ? C15 C16 1.384(4) . ? C15 H15 0.9300 . ? C16 C17 1.419(4) . ? C18 C19 1.406(5) . ? C18 H18 0.9300 . ? C19 C20 1.353(5) . ? C19 H19 0.9300 . ? C20 C21 1.411(5) . ? C20 H20 0.9300 . ? C21 C22 1.405(5) . ? C21 C26 1.420(4) . ? C22 C23 1.371(5) . ? C22 H22 0.9300 . ? C23 C24 1.396(5) . ? C23 H23 0.9300 . ? C24 C25 1.389(4) . ? C24 H24 0.9300 . ? C25 C26 1.425(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Ru N2 86.17(9) . . ? O1 Ru O2 159.17(8) . . ? N2 Ru O2 79.53(10) . . ? O1 Ru N1 79.66(9) . . ? N2 Ru N1 91.73(9) . . ? O2 Ru N1 85.67(9) . . ? O1 Ru C5 78.64(11) . . ? N2 Ru C5 90.34(11) . . ? O2 Ru C5 116.22(11) . . ? N1 Ru C5 158.01(11) . . ? O1 Ru C1 115.55(11) . . ? N2 Ru C1 158.22(11) . . ? O2 Ru C1 79.06(11) . . ? N1 Ru C1 90.65(11) . . ? C5 Ru C1 95.48(12) . . ? O1 Ru C6 115.63(11) . . ? N2 Ru C6 91.53(11) . . ? O2 Ru C6 80.09(11) . . ? N1 Ru C6 164.56(12) . . ? C5 Ru C6 37.01(12) . . ? C1 Ru C6 80.85(12) . . ? O1 Ru C2 79.91(10) . . ? N2 Ru C2 164.71(11) . . ? O2 Ru C2 115.55(11) . . ? N1 Ru C2 91.96(11) . . ? C5 Ru C2 80.79(12) . . ? C1 Ru C2 36.51(11) . . ? C6 Ru C2 88.84(12) . . ? C16 O1 Ru 112.38(17) . . ? C25 O2 Ru 112.60(19) . . ? C9 N1 C17 119.1(3) . . ? C9 N1 Ru 128.7(2) . . ? C17 N1 Ru 112.15(19) . . ? C18 N2 C26 119.6(3) . . ? C18 N2 Ru 128.0(2) . . ? C26 N2 Ru 112.4(2) . . ? C2 C1 C8 125.6(3) . . ? C2 C1 Ru 72.28(17) . . ? C8 C1 Ru 109.4(2) . . ? C2 C1 H1 113.9 . . ? C8 C1 H1 113.9 . . ? Ru C1 H1 113.9 . . ? C1 C2 C3 123.7(3) . . ? C1 C2 Ru 71.21(18) . . ? C3 C2 Ru 112.1(2) . . ? C1 C2 H2 114.1 . . ? C3 C2 H2 114.1 . . ? Ru C2 H2 114.1 . . ? C2 C3 C4 114.5(3) . . ? C2 C3 H3A 108.6 . . ? C4 C3 H3A 108.6 . . ? C2 C3 H3B 108.6 . . ? C4 C3 H3B 108.6 . . ? H3A C3 H3B 107.6 . . ? C5 C4 C3 113.6(3) . . ? C5 C4 H4A 108.9 . . ? C3 C4 H4A 108.9 . . ? C5 C4 H4B 108.9 . . ? C3 C4 H4B 108.9 . . ? H4A C4 H4B 107.7 . . ? C6 C5 C4 125.6(3) . . ? C6 C5 Ru 71.65(18) . . ? C4 C5 Ru 110.3(2) . . ? C6 C5 H5 113.8 . . ? C4 C5 H5 113.8 . . ? Ru C5 H5 113.8 . . ? C5 C6 C7 123.4(3) . . ? C5 C6 Ru 71.34(17) . . ? C7 C6 Ru 112.2(2) . . ? C5 C6 H6 114.2 . . ? C7 C6 H6 114.2 . . ? Ru C6 H6 114.2 . . ? C8 C7 C6 114.1(3) . . ? C8 C7 H7A 108.7 . . ? C6 C7 H7A 108.7 . . ? C8 C7 H7B 108.7 . . ? C6 C7 H7B 108.7 . . ? H7A C7 H7B 107.6 . . ? C7 C8 C1 114.4(3) . . ? C7 C8 H8A 108.7 . . ? C1 C8 H8A 108.7 . . ? C7 C8 H8B 108.7 . . ? C1 C8 H8B 108.7 . . ? H8A C8 H8B 107.6 . . ? N1 C9 C10 122.0(3) . . ? N1 C9 H9 119.0 . . ? C10 C9 H9 119.0 . . ? C11 C10 C9 119.8(3) . . ? C11 C10 H10 120.1 . . ? C9 C10 H10 120.1 . . ? C10 C11 C12 120.6(3) . . ? C10 C11 H11 119.7 . . ? C12 C11 H11 119.7 . . ? C13 C12 C11 125.2(3) . . ? C13 C12 C17 118.5(3) . . ? C11 C12 C17 116.3(3) . . ? C14 C13 C12 119.6(3) . . ? C14 C13 H13 120.2 . . ? C12 C13 H13 120.2 . . ? C13 C14 C15 122.1(3) . . ? C13 C14 H14 118.9 . . ? C15 C14 H14 118.9 . . ? C16 C15 C14 120.9(3) . . ? C16 C15 H15 119.6 . . ? C14 C15 H15 119.6 . . ? O1 C16 C15 123.3(3) . . ? O1 C16 C17 119.7(3) . . ? C15 C16 C17 117.0(3) . . ? N1 C17 C16 116.1(3) . . ? N1 C17 C12 122.1(3) . . ? C16 C17 C12 121.8(3) . . ? N2 C18 C19 121.8(3) . . ? N2 C18 H18 119.1 . . ? C19 C18 H18 119.1 . . ? C20 C19 C18 119.8(3) . . ? C20 C19 H19 120.1 . . ? C18 C19 H19 120.1 . . ? C19 C20 C21 120.5(3) . . ? C19 C20 H20 119.8 . . ? C21 C20 H20 119.8 . . ? C22 C21 C20 125.4(3) . . ? C22 C21 C26 117.9(3) . . ? C20 C21 C26 116.6(3) . . ? C23 C22 C21 120.0(3) . . ? C23 C22 H22 120.0 . . ? C21 C22 H22 120.0 . . ? C22 C23 C24 121.9(3) . . ? C22 C23 H23 119.0 . . ? C24 C23 H23 119.0 . . ? C25 C24 C23 121.0(4) . . ? C25 C24 H24 119.5 . . ? C23 C24 H24 119.5 . . ? O2 C25 C24 123.9(3) . . ? O2 C25 C26 119.2(3) . . ? C24 C25 C26 116.9(3) . . ? N2 C26 C21 121.6(3) . . ? N2 C26 C25 116.1(3) . . ? C21 C26 C25 122.2(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Ru O1 C16 90.38(19) . . . . ? O2 Ru O1 C16 43.9(3) . . . . ? N1 Ru O1 C16 -2.08(18) . . . . ? C5 Ru O1 C16 -178.5(2) . . . . ? C1 Ru O1 C16 -87.8(2) . . . . ? C6 Ru O1 C16 -179.75(18) . . . . ? C2 Ru O1 C16 -96.0(2) . . . . ? O1 Ru O2 C25 44.3(3) . . . . ? N2 Ru O2 C25 -3.1(2) . . . . ? N1 Ru O2 C25 89.5(2) . . . . ? C5 Ru O2 C25 -88.3(2) . . . . ? C1 Ru O2 C25 -179.0(2) . . . . ? C6 Ru O2 C25 -96.5(2) . . . . ? C2 Ru O2 C25 179.6(2) . . . . ? O1 Ru N1 C9 -178.1(3) . . . . ? N2 Ru N1 C9 96.1(3) . . . . ? O2 Ru N1 C9 16.7(3) . . . . ? C5 Ru N1 C9 -168.7(3) . . . . ? C1 Ru N1 C9 -62.3(3) . . . . ? C6 Ru N1 C9 -6.0(5) . . . . ? C2 Ru N1 C9 -98.8(3) . . . . ? O1 Ru N1 C17 0.76(18) . . . . ? N2 Ru N1 C17 -85.0(2) . . . . ? O2 Ru N1 C17 -164.39(19) . . . . ? C5 Ru N1 C17 10.2(4) . . . . ? C1 Ru N1 C17 116.6(2) . . . . ? C6 Ru N1 C17 172.9(4) . . . . ? C2 Ru N1 C17 80.1(2) . . . . ? O1 Ru N2 C18 17.8(2) . . . . ? O2 Ru N2 C18 -177.5(3) . . . . ? N1 Ru N2 C18 97.3(3) . . . . ? C5 Ru N2 C18 -60.8(3) . . . . ? C1 Ru N2 C18 -166.6(3) . . . . ? C6 Ru N2 C18 -97.8(3) . . . . ? C2 Ru N2 C18 -6.6(5) . . . . ? O1 Ru N2 C26 -162.64(19) . . . . ? O2 Ru N2 C26 2.14(18) . . . . ? N1 Ru N2 C26 -83.13(19) . . . . ? C5 Ru N2 C26 118.8(2) . . . . ? C1 Ru N2 C26 13.0(4) . . . . ? C6 Ru N2 C26 81.8(2) . . . . ? C2 Ru N2 C26 173.0(3) . . . . ? O1 Ru C1 C2 -13.6(2) . . . . ? N2 Ru C1 C2 171.3(2) . . . . ? O2 Ru C1 C2 -177.9(2) . . . . ? N1 Ru C1 C2 -92.41(19) . . . . ? C5 Ru C1 C2 66.4(2) . . . . ? C6 Ru C1 C2 100.5(2) . . . . ? O1 Ru C1 C8 -135.9(2) . . . . ? N2 Ru C1 C8 49.0(4) . . . . ? O2 Ru C1 C8 59.8(2) . . . . ? N1 Ru C1 C8 145.3(2) . . . . ? C5 Ru C1 C8 -55.9(3) . . . . ? C6 Ru C1 C8 -21.8(2) . . . . ? C2 Ru C1 C8 -122.3(3) . . . . ? C8 C1 C2 C3 -3.0(5) . . . . ? Ru C1 C2 C3 -104.5(3) . . . . ? C8 C1 C2 Ru 101.5(3) . . . . ? O1 Ru C2 C1 167.6(2) . . . . ? N2 Ru C2 C1 -167.7(3) . . . . ? O2 Ru C2 C1 2.3(2) . . . . ? N1 Ru C2 C1 88.45(19) . . . . ? C5 Ru C2 C1 -112.4(2) . . . . ? C6 Ru C2 C1 -76.1(2) . . . . ? O1 Ru C2 C3 -72.8(2) . . . . ? N2 Ru C2 C3 -48.1(5) . . . . ? O2 Ru C2 C3 121.9(2) . . . . ? N1 Ru C2 C3 -152.0(2) . . . . ? C5 Ru C2 C3 7.2(2) . . . . ? C1 Ru C2 C3 119.6(3) . . . . ? C6 Ru C2 C3 43.5(2) . . . . ? C1 C2 C3 C4 90.3(4) . . . . ? Ru C2 C3 C4 8.7(4) . . . . ? C2 C3 C4 C5 -27.9(4) . . . . ? C3 C4 C5 C6 -48.5(4) . . . . ? C3 C4 C5 Ru 33.0(4) . . . . ? O1 Ru C5 C6 -178.1(2) . . . . ? N2 Ru C5 C6 -92.09(19) . . . . ? O2 Ru C5 C6 -13.6(2) . . . . ? N1 Ru C5 C6 172.4(2) . . . . ? C1 Ru C5 C6 66.9(2) . . . . ? C2 Ru C5 C6 100.4(2) . . . . ? O1 Ru C5 C4 59.8(2) . . . . ? N2 Ru C5 C4 145.9(2) . . . . ? O2 Ru C5 C4 -135.6(2) . . . . ? N1 Ru C5 C4 50.4(4) . . . . ? C1 Ru C5 C4 -55.2(3) . . . . ? C6 Ru C5 C4 -122.0(3) . . . . ? C2 Ru C5 C4 -21.6(2) . . . . ? C4 C5 C6 C7 -2.5(5) . . . . ? Ru C5 C6 C7 -104.8(3) . . . . ? C4 C5 C6 Ru 102.3(3) . . . . ? O1 Ru C6 C5 2.1(2) . . . . ? N2 Ru C6 C5 88.5(2) . . . . ? O2 Ru C6 C5 167.6(2) . . . . ? N1 Ru C6 C5 -169.3(3) . . . . ? C1 Ru C6 C5 -112.0(2) . . . . ? C2 Ru C6 C5 -76.2(2) . . . . ? O1 Ru C6 C7 121.4(2) . . . . ? N2 Ru C6 C7 -152.1(3) . . . . ? O2 Ru C6 C7 -73.0(3) . . . . ? N1 Ru C6 C7 -50.0(5) . . . . ? C5 Ru C6 C7 119.4(3) . . . . ? C1 Ru C6 C7 7.4(3) . . . . ? C2 Ru C6 C7 43.2(3) . . . . ? C5 C6 C7 C8 90.5(4) . . . . ? Ru C6 C7 C8 8.8(4) . . . . ? C6 C7 C8 C1 -28.6(5) . . . . ? C2 C1 C8 C7 -48.0(5) . . . . ? Ru C1 C8 C7 33.6(4) . . . . ? C17 N1 C9 C10 0.1(5) . . . . ? Ru N1 C9 C10 179.0(2) . . . . ? N1 C9 C10 C11 0.5(5) . . . . ? C9 C10 C11 C12 -0.1(5) . . . . ? C10 C11 C12 C13 179.1(3) . . . . ? C10 C11 C12 C17 -0.9(5) . . . . ? C11 C12 C13 C14 -178.9(3) . . . . ? C17 C12 C13 C14 1.0(5) . . . . ? C12 C13 C14 C15 -1.7(5) . . . . ? C13 C14 C15 C16 0.5(5) . . . . ? Ru O1 C16 C15 -176.8(2) . . . . ? Ru O1 C16 C17 3.2(3) . . . . ? C14 C15 C16 O1 -178.8(3) . . . . ? C14 C15 C16 C17 1.2(4) . . . . ? C9 N1 C17 C16 179.6(3) . . . . ? Ru N1 C17 C16 0.6(3) . . . . ? C9 N1 C17 C12 -1.2(4) . . . . ? Ru N1 C17 C12 179.8(2) . . . . ? O1 C16 C17 N1 -2.6(4) . . . . ? C15 C16 C17 N1 177.4(3) . . . . ? O1 C16 C17 C12 178.2(3) . . . . ? C15 C16 C17 C12 -1.8(4) . . . . ? C13 C12 C17 N1 -178.4(3) . . . . ? C11 C12 C17 N1 1.5(4) . . . . ? C13 C12 C17 C16 0.7(4) . . . . ? C11 C12 C17 C16 -179.3(3) . . . . ? C26 N2 C18 C19 1.0(4) . . . . ? Ru N2 C18 C19 -179.4(2) . . . . ? N2 C18 C19 C20 0.7(5) . . . . ? C18 C19 C20 C21 -1.0(5) . . . . ? C19 C20 C21 C22 179.4(3) . . . . ? C19 C20 C21 C26 -0.3(5) . . . . ? C20 C21 C22 C23 -178.8(3) . . . . ? C26 C21 C22 C23 0.8(5) . . . . ? C21 C22 C23 C24 -2.2(5) . . . . ? C22 C23 C24 C25 1.5(5) . . . . ? Ru O2 C25 C24 -175.2(3) . . . . ? Ru O2 C25 C26 3.7(3) . . . . ? C23 C24 C25 O2 179.4(3) . . . . ? C23 C24 C25 C26 0.5(5) . . . . ? C18 N2 C26 C21 -2.4(4) . . . . ? Ru N2 C26 C21 177.9(2) . . . . ? C18 N2 C26 C25 178.7(3) . . . . ? Ru N2 C26 C25 -1.0(3) . . . . ? C22 C21 C26 N2 -177.6(3) . . . . ? C20 C21 C26 N2 2.1(4) . . . . ? C22 C21 C26 C25 1.2(4) . . . . ? C20 C21 C26 C25 -179.1(3) . . . . ? O2 C25 C26 N2 -1.9(4) . . . . ? C24 C25 C26 N2 177.1(3) . . . . ? O2 C25 C26 C21 179.3(3) . . . . ? C24 C25 C26 C21 -1.8(4) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.368 _refine_diff_density_min -0.410 _refine_diff_density_rms 0.060 #===END #====== kinx305 compound 5 in text ================== data_kiny305 _audit_creation_method SHELXL _chemical_name_systematic ; (hydrogen tris(pyrazolyl)borato-N)-(8-hydroxyquinolinato-N,O)- (eta$6!-p-cymene)-ruthenium(II) ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C28 H30 B N7 O Ru' _chemical_formula_weight 592.47 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ru' 'Ru' -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.980(1) _cell_length_b 10.672(1) _cell_length_c 12.548(2) _cell_angle_alpha 92.58(1) _cell_angle_beta 91.70(1) _cell_angle_gamma 98.78(1) _cell_volume 1318.5(3) _cell_formula_units_Z 2 _cell_measurement_temperature 301(2) _cell_measurement_reflns_used 8192 _cell_measurement_theta_min 2 _cell_measurement_theta_max 30 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.492 _exptl_crystal_density_method ? _exptl_crystal_F_000 608 _exptl_absorpt_coefficient_mu 0.631 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.962 _exptl_absorpt_correction_T_max 0.873 _exptl_absorpt_process_details ? _exptl_special_details ; Siemens SMART platform 3-circle diffractometer with CCD area detector, sealed X-ray tube, graphite monochromator. An incomplete sphere of the reciprocal space up to theta(max) = 30 deg was measured by omega scan frames with delta(omega) = 0.30 deg and 20 sec per frame, 3 x 606 frames (Phi = 0, 90, and 180 deg.) recorded using program SMART (Siemens/Bruker). Frame data evaluation with program SAINT (Siemens/Bruker); lattice parameters by least-squares refinement of the geometric parameters of the strongest reflections. Correction for absorption and crystal decay (insignificant) by semi-empirical method from equivalents (multi-scan method) using program SADABS (G.M. Sheldrick, 1996, Univ. of Goettingen, Germany). Data reduction with program XPREP (Siemens/Bruker). ; _diffrn_ambient_temperature 301(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 'Siemens SMART 3-circle with CCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15883 _diffrn_reflns_av_R_equivalents 0.0211 _diffrn_reflns_av_sigmaI/netI 0.0372 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.63 _diffrn_reflns_theta_max 30.04 _reflns_number_total 7617 _reflns_number_observed 6337 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens SMART' _computing_cell_refinement 'Siemens SAINT' _computing_data_reduction 'Siemens SAINT and SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; 1) Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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. 2) H(2), H(3), H(5), and H(6) were refined in x,y,z using a C-H distance restraint. All other hydrogen were inserted in idealized positions and were refined riding with the atoms to which they were bonded. All hydrogens had U~iso~ = U~eq~ x 1.2 (x 1.5 for CH~3~) of their carrier atoms. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0326P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7617 _refine_ls_number_parameters 358 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0380 _refine_ls_R_factor_obs 0.0263 _refine_ls_wR_factor_all 0.0615 _refine_ls_wR_factor_obs 0.0576 _refine_ls_goodness_of_fit_all 0.986 _refine_ls_goodness_of_fit_obs 1.017 _refine_ls_restrained_S_all 0.986 _refine_ls_restrained_S_obs 1.017 _refine_ls_shift/esd_max -0.006 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Ru Ru 0.500433(12) 0.211384(11) 0.241526(10) 0.02668(4) Uani 1 d . . C1 C 0.5672(2) 0.1024(2) 0.10556(13) 0.0359(4) Uani 1 d . . C2 C 0.4789(2) 0.0219(2) 0.16578(14) 0.0370(4) Uani 1 d D . H2 H 0.5087(18) -0.0444(12) 0.2006(14) 0.044 Uiso 1 d D . C3 C 0.3467(2) 0.0497(2) 0.19031(14) 0.0358(4) Uani 1 d D . H3 H 0.2938(16) 0.0010(15) 0.2377(12) 0.043 Uiso 1 d D . C4 C 0.3020(2) 0.15981(15) 0.15367(13) 0.0337(3) Uani 1 d . . C5 C 0.3926(2) 0.2420(2) 0.09166(13) 0.0347(3) Uani 1 d D . H5 H 0.3632(18) 0.3167(9) 0.0724(15) 0.042 Uiso 1 d D . C6 C 0.5220(2) 0.2147(2) 0.06889(13) 0.0360(4) Uani 1 d D . H6 H 0.5829(14) 0.2699(14) 0.0319(13) 0.043 Uiso 1 d D . C7 C 0.7092(2) 0.0771(2) 0.0872(2) 0.0527(5) Uani 1 d . . H7A H 0.7106(4) 0.0288(13) 0.0209(6) 0.079 Uiso 1 calc R . H7B H 0.7386(6) 0.0300(13) 0.1445(7) 0.079 Uiso 1 calc R . H7C H 0.7690(3) 0.1563(2) 0.0844(12) 0.079 Uiso 1 calc R . C8 C 0.1660(2) 0.1977(2) 0.1788(2) 0.0459(4) Uani 1 d . . H8 H 0.1827(2) 0.2856(2) 0.2081(2) 0.055 Uiso 1 calc R . C9 C 0.0825(2) 0.1957(3) 0.0734(2) 0.0779(8) Uani 1 d . . H9A H 0.0008(10) 0.2303(18) 0.0865(4) 0.117 Uiso 1 calc R . H9B H 0.0597(18) 0.1099(4) 0.0449(9) 0.117 Uiso 1 calc R . H9C H 0.1348(8) 0.2458(16) 0.0231(6) 0.117 Uiso 1 calc R . C10 C 0.0888(2) 0.1181(2) 0.2598(2) 0.0683(6) Uani 1 d . . H10A H 0.1444(7) 0.1194(14) 0.3238(6) 0.102 Uiso 1 calc R . H10B H 0.0654(16) 0.0323(5) 0.2313(6) 0.102 Uiso 1 calc R . H10C H 0.0076(10) 0.1518(11) 0.2761(11) 0.102 Uiso 1 calc R . N1 N 0.69549(13) 0.30453(12) 0.28461(10) 0.0314(3) Uani 1 d . . C11 C 0.7732(2) 0.3910(2) 0.23251(15) 0.0407(4) Uani 1 d . . H11 H 0.7402(2) 0.4179(2) 0.16876(15) 0.049 Uiso 1 calc R . C12 C 0.9048(2) 0.4434(2) 0.2710(2) 0.0492(5) Uani 1 d . . H12 H 0.9569(2) 0.5049(2) 0.2332(2) 0.059 Uiso 1 calc R . C13 C 0.9556(2) 0.4044(2) 0.3628(2) 0.0503(5) Uani 1 d . . H13 H 1.0428(2) 0.4387(2) 0.3876(2) 0.060 Uiso 1 calc R . C14 C 0.8770(2) 0.3120(2) 0.42115(15) 0.0412(4) Uani 1 d . . C15 C 0.9196(2) 0.2627(2) 0.5172(2) 0.0546(5) Uani 1 d . . H15 H 1.0055(2) 0.2915(2) 0.5476(2) 0.065 Uiso 1 calc R . C16 C 0.8323(2) 0.1719(2) 0.5649(2) 0.0540(5) Uani 1 d . . H16 H 0.8620(2) 0.1391(2) 0.6272(2) 0.065 Uiso 1 calc R . C17 C 0.7011(2) 0.1261(2) 0.52460(14) 0.0449(4) Uani 1 d . . H17 H 0.6454(2) 0.0650(2) 0.56023(14) 0.054 Uiso 1 calc R . C18 C 0.6540(2) 0.17267(15) 0.43062(13) 0.0330(3) Uani 1 d . . C19 C 0.7446(2) 0.26480(15) 0.37891(12) 0.0317(3) Uani 1 d . . O O 0.53297(12) 0.13465(10) 0.38654(9) 0.0358(3) Uani 1 d . . B B 0.4699(2) 0.5498(2) 0.2116(2) 0.0348(4) Uani 1 d . . H0B H 0.5090(2) 0.4826(2) 0.1561(2) 0.042 Uiso 1 calc R . N2 N 0.41859(14) 0.48002(12) 0.31350(11) 0.0340(3) Uani 1 d . . N3 N 0.42972(13) 0.35755(12) 0.33494(10) 0.0297(3) Uani 1 d . . C20 C 0.3740(2) 0.3362(2) 0.42931(13) 0.0375(4) Uani 1 d . . H20 H 0.3686(2) 0.2600(2) 0.46324(13) 0.045 Uiso 1 calc R . C21 C 0.3258(2) 0.4416(2) 0.46934(14) 0.0394(4) Uani 1 d . . H21 H 0.2822(2) 0.4508(2) 0.53305(14) 0.047 Uiso 1 calc R . C22 C 0.3560(2) 0.5301(2) 0.39502(15) 0.0419(4) Uani 1 d . . H22 H 0.3363(2) 0.6126(2) 0.39992(15) 0.050 Uiso 1 calc R . N4 N 0.3472(2) 0.59879(14) 0.15767(11) 0.0393(3) Uani 1 d . . N5 N 0.2735(2) 0.5301(2) 0.07503(13) 0.0524(4) Uani 1 d . . C23 C 0.1701(2) 0.5921(3) 0.0567(2) 0.0637(6) Uani 1 d . . H23 H 0.1026(2) 0.5671(3) 0.0040(2) 0.076 Uiso 1 calc R . C24 C 0.1742(2) 0.6978(2) 0.1248(2) 0.0619(6) Uani 1 d . . H24 H 0.1130(2) 0.7554(2) 0.1272(2) 0.074 Uiso 1 calc R . C25 C 0.2883(2) 0.6990(2) 0.1879(2) 0.0514(5) Uani 1 d . . H25 H 0.3198(2) 0.7590(2) 0.2425(2) 0.062 Uiso 1 calc R . N6 N 0.5830(2) 0.66245(14) 0.24175(12) 0.0414(3) Uani 1 d . . N7 N 0.5732(2) 0.7520(2) 0.32064(14) 0.0607(5) Uani 1 d . . C26 C 0.6916(3) 0.8306(2) 0.3225(2) 0.0761(8) Uani 1 d . . H26 H 0.7149(3) 0.9007(2) 0.3698(2) 0.091 Uiso 1 calc R . C27 C 0.7739(3) 0.7937(3) 0.2451(3) 0.0854(9) Uani 1 d . . H27 H 0.8604(3) 0.8334(3) 0.2301(3) 0.102 Uiso 1 calc R . C28 C 0.7033(2) 0.6869(2) 0.1947(2) 0.0631(6) Uani 1 d . . H28 H 0.7326(2) 0.6397(2) 0.1384(2) 0.076 Uiso 1 calc R . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru 0.02732(7) 0.02445(6) 0.02722(6) 0.00114(4) -0.00117(4) 0.00106(4) C1 0.0338(8) 0.0391(9) 0.0335(8) -0.0089(7) 0.0002(7) 0.0041(7) C2 0.0389(9) 0.0271(8) 0.0434(9) -0.0059(7) -0.0061(7) 0.0038(7) C3 0.0348(9) 0.0278(8) 0.0422(9) -0.0024(7) 0.0000(7) -0.0017(6) C4 0.0308(8) 0.0317(8) 0.0365(8) -0.0037(6) -0.0049(7) 0.0006(6) C5 0.0369(9) 0.0319(8) 0.0336(8) 0.0005(6) -0.0099(7) 0.0021(7) C6 0.0373(9) 0.0394(9) 0.0286(8) -0.0005(7) -0.0004(7) -0.0019(7) C7 0.0390(10) 0.0645(13) 0.0550(12) -0.0083(10) 0.0040(9) 0.0117(9) C8 0.0330(9) 0.0436(10) 0.0605(12) -0.0045(9) -0.0009(8) 0.0060(8) C9 0.0385(11) 0.104(2) 0.090(2) 0.005(2) -0.0181(12) 0.0136(13) C10 0.0467(12) 0.074(2) 0.086(2) 0.0040(13) 0.0213(12) 0.0119(11) N1 0.0313(7) 0.0296(6) 0.0323(7) -0.0013(5) -0.0010(5) 0.0026(5) C11 0.0401(9) 0.0380(9) 0.0418(9) 0.0042(7) 0.0019(8) -0.0014(7) C12 0.0386(10) 0.0472(11) 0.0576(12) 0.0035(9) 0.0059(9) -0.0084(8) C13 0.0315(9) 0.0519(11) 0.0633(13) -0.0068(10) -0.0054(9) -0.0029(8) C14 0.0351(9) 0.0419(9) 0.0456(10) -0.0080(8) -0.0067(8) 0.0072(7) C15 0.0447(11) 0.0648(13) 0.0531(12) -0.0063(10) -0.0197(9) 0.0117(10) C16 0.0612(13) 0.0596(12) 0.0426(10) 0.0053(9) -0.0153(9) 0.0168(10) C17 0.0569(11) 0.0435(10) 0.0357(9) 0.0054(8) -0.0046(8) 0.0118(9) C18 0.0388(9) 0.0294(8) 0.0314(8) -0.0025(6) -0.0013(7) 0.0088(7) C19 0.0335(8) 0.0318(8) 0.0297(8) -0.0040(6) -0.0028(6) 0.0074(6) O 0.0375(6) 0.0329(6) 0.0357(6) 0.0088(5) -0.0027(5) 0.0001(5) B 0.0393(10) 0.0300(9) 0.0348(9) 0.0026(7) 0.0014(8) 0.0040(7) N2 0.0397(7) 0.0281(6) 0.0345(7) 0.0020(5) 0.0033(6) 0.0053(6) N3 0.0342(7) 0.0268(6) 0.0277(6) 0.0025(5) 0.0016(5) 0.0030(5) C20 0.0428(9) 0.0383(9) 0.0312(8) 0.0058(7) 0.0050(7) 0.0037(7) C21 0.0385(9) 0.0466(10) 0.0329(8) -0.0017(7) 0.0068(7) 0.0059(8) C22 0.0486(10) 0.0353(9) 0.0431(10) -0.0038(7) 0.0061(8) 0.0118(8) N4 0.0445(8) 0.0360(7) 0.0368(7) 0.0052(6) -0.0018(6) 0.0043(6) N5 0.0526(10) 0.0527(10) 0.0476(9) 0.0031(8) -0.0047(8) -0.0047(8) C23 0.0446(11) 0.088(2) 0.0537(12) 0.0198(12) -0.0098(10) -0.0085(11) C24 0.0552(13) 0.075(2) 0.0626(14) 0.0219(12) 0.0042(11) 0.0266(12) C25 0.0613(13) 0.0476(11) 0.0485(11) 0.0028(9) -0.0043(9) 0.0198(10) N6 0.0450(8) 0.0340(7) 0.0436(8) 0.0058(6) -0.0028(7) 0.0012(6) N7 0.0818(13) 0.0435(9) 0.0501(10) -0.0025(8) -0.0057(9) -0.0085(9) C26 0.101(2) 0.0445(12) 0.072(2) 0.0121(11) -0.034(2) -0.0213(13) C27 0.0558(15) 0.060(2) 0.135(3) 0.030(2) -0.005(2) -0.0157(12) C28 0.0501(12) 0.0471(12) 0.092(2) 0.0179(12) 0.0180(12) 0.0009(10) _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 Ru O 2.0658(11) . ? Ru N1 2.0900(13) . ? Ru N3 2.1274(13) . ? Ru C2 2.173(2) . ? Ru C6 2.185(2) . ? Ru C3 2.186(2) . ? Ru C1 2.199(2) . ? Ru C5 2.201(2) . ? Ru C4 2.219(2) . ? C1 C2 1.398(2) . ? C1 C6 1.433(2) . ? C1 C7 1.505(2) . ? C2 C3 1.435(2) . ? C2 H2 0.9301(10) . ? C3 C4 1.409(2) . ? C3 H3 0.9301(10) . ? C4 C5 1.434(2) . ? C4 C8 1.512(2) . ? C5 C6 1.401(2) . ? C5 H5 0.9301(10) . ? C6 H6 0.9301(10) . ? C7 H7A 0.96 . ? C7 H7B 0.96 . ? C7 H7C 0.96 . ? C8 C10 1.509(3) . ? C8 C9 1.539(3) . ? C8 H8 0.98 . ? C9 H9A 0.96 . ? C9 H9B 0.96 . ? C9 H9C 0.96 . ? C10 H10A 0.96 . ? C10 H10B 0.96 . ? C10 H10C 0.96 . ? N1 C11 1.321(2) . ? N1 C19 1.376(2) . ? C11 C12 1.409(3) . ? C11 H11 0.93 . ? C12 C13 1.353(3) . ? C12 H12 0.93 . ? C13 C14 1.410(3) . ? C13 H13 0.93 . ? C14 C15 1.416(3) . ? C14 C19 1.418(2) . ? C15 C16 1.371(3) . ? C15 H15 0.93 . ? C16 C17 1.397(3) . ? C16 H16 0.93 . ? C17 C18 1.396(2) . ? C17 H17 0.93 . ? C18 O 1.312(2) . ? C18 C19 1.423(2) . ? B N6 1.543(2) . ? B N4 1.552(2) . ? B N2 1.568(2) . ? B H0B 1.10 . ? N2 C22 1.347(2) . ? N2 N3 1.367(2) . ? N3 C20 1.337(2) . ? C20 C21 1.371(2) . ? C20 H20 0.93 . ? C21 C22 1.364(3) . ? C21 H21 0.93 . ? C22 H22 0.93 . ? N4 C25 1.342(2) . ? N4 N5 1.369(2) . ? N5 C23 1.328(3) . ? C23 C24 1.378(4) . ? C23 H23 0.93 . ? C24 C25 1.366(3) . ? C24 H24 0.93 . ? C25 H25 0.93 . ? N6 C28 1.348(3) . ? N6 N7 1.361(2) . ? N7 C26 1.340(3) . ? C26 C27 1.373(4) . ? C26 H26 0.93 . ? C27 C28 1.364(4) . ? C27 H27 0.93 . ? C28 H28 0.93 . ? 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 O Ru N1 79.00(5) . . ? O Ru N3 84.74(5) . . ? N1 Ru N3 86.04(5) . . ? O Ru C2 88.96(6) . . ? N1 Ru C2 118.39(6) . . ? N3 Ru C2 153.10(6) . . ? O Ru C6 151.06(6) . . ? N1 Ru C6 96.82(6) . . ? N3 Ru C6 123.81(6) . . ? C2 Ru C6 67.65(7) . . ? O Ru C3 91.96(6) . . ? N1 Ru C3 155.94(6) . . ? N3 Ru C3 115.56(6) . . ? C2 Ru C3 38.44(6) . . ? C6 Ru C3 80.30(7) . . ? O Ru C1 113.10(6) . . ? N1 Ru C1 94.29(6) . . ? N3 Ru C1 161.93(6) . . ? C2 Ru C1 37.29(7) . . ? C6 Ru C1 38.17(6) . . ? C3 Ru C1 68.61(6) . . ? O Ru C5 157.81(6) . . ? N1 Ru C5 123.18(6) . . ? N3 Ru C5 96.51(6) . . ? C2 Ru C5 79.93(6) . . ? C6 Ru C5 37.26(6) . . ? C3 Ru C5 67.44(6) . . ? C1 Ru C5 68.22(6) . . ? O Ru C4 120.07(5) . . ? N1 Ru C4 160.67(6) . . ? N3 Ru C4 92.29(6) . . ? C2 Ru C4 68.45(6) . . ? C6 Ru C4 68.22(6) . . ? C3 Ru C4 37.32(6) . . ? C1 Ru C4 81.44(6) . . ? C5 Ru C4 37.85(6) . . ? C2 C1 C6 117.9(2) . . ? C2 C1 C7 120.9(2) . . ? C6 C1 C7 121.0(2) . . ? C2 C1 Ru 70.36(10) . . ? C6 C1 Ru 70.38(9) . . ? C7 C1 Ru 126.65(13) . . ? C1 C2 C3 121.5(2) . . ? C1 C2 Ru 72.35(9) . . ? C3 C2 Ru 71.25(9) . . ? C1 C2 H2 120.8(12) . . ? C3 C2 H2 117.0(12) . . ? Ru C2 H2 121.0(12) . . ? C4 C3 C2 120.6(2) . . ? C4 C3 Ru 72.62(9) . . ? C2 C3 Ru 70.31(9) . . ? C4 C3 H3 118.8(12) . . ? C2 C3 H3 120.2(12) . . ? Ru C3 H3 123.2(12) . . ? C3 C4 C5 117.85(15) . . ? C3 C4 C8 123.8(2) . . ? C5 C4 C8 118.36(15) . . ? C3 C4 Ru 70.06(9) . . ? C5 C4 Ru 70.39(9) . . ? C8 C4 Ru 129.37(12) . . ? C6 C5 C4 121.19(15) . . ? C6 C5 Ru 70.74(9) . . ? C4 C5 Ru 71.76(9) . . ? C6 C5 H5 122.5(12) . . ? C4 C5 H5 116.2(12) . . ? Ru C5 H5 126.7(12) . . ? C5 C6 C1 121.0(2) . . ? C5 C6 Ru 72.00(10) . . ? C1 C6 Ru 71.44(9) . . ? C5 C6 H6 121.5(12) . . ? C1 C6 H6 117.4(11) . . ? Ru C6 H6 127.4(12) . . ? C1 C7 H7A 109.47(10) . . ? C1 C7 H7B 109.47(11) . . ? H7A C7 H7B 109.5 . . ? C1 C7 H7C 109.47(11) . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C10 C8 C4 114.2(2) . . ? C10 C8 C9 111.5(2) . . ? C4 C8 C9 108.3(2) . . ? C10 C8 H8 107.52(13) . . ? C4 C8 H8 107.52(9) . . ? C9 C8 H8 107.52(14) . . ? C8 C9 H9A 109.47(13) . . ? C8 C9 H9B 109.47(14) . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.47(13) . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C8 C10 H10A 109.47(12) . . ? C8 C10 H10B 109.47(13) . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.47(11) . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C11 N1 C19 119.03(14) . . ? C11 N1 Ru 128.36(11) . . ? C19 N1 Ru 112.60(10) . . ? N1 C11 C12 121.7(2) . . ? N1 C11 H11 119.15(10) . . ? C12 C11 H11 119.15(11) . . ? C13 C12 C11 120.2(2) . . ? C13 C12 H12 119.92(11) . . ? C11 C12 H12 119.92(11) . . ? C12 C13 C14 120.4(2) . . ? C12 C13 H13 119.82(11) . . ? C14 C13 H13 119.82(11) . . ? C13 C14 C15 125.5(2) . . ? C13 C14 C19 116.6(2) . . ? C15 C14 C19 117.9(2) . . ? C16 C15 C14 119.1(2) . . ? C16 C15 H15 120.46(11) . . ? C14 C15 H15 120.46(12) . . ? C15 C16 C17 123.4(2) . . ? C15 C16 H16 118.31(11) . . ? C17 C16 H16 118.31(11) . . ? C18 C17 C16 119.7(2) . . ? C18 C17 H17 120.17(11) . . ? C16 C17 H17 120.17(11) . . ? O C18 C17 123.9(2) . . ? O C18 C19 118.50(13) . . ? C17 C18 C19 117.6(2) . . ? N1 C19 C14 122.1(2) . . ? N1 C19 C18 115.51(14) . . ? C14 C19 C18 122.34(15) . . ? C18 O Ru 114.27(10) . . ? N6 B N4 109.80(13) . . ? N6 B N2 110.87(14) . . ? N4 B N2 107.75(14) . . ? N6 B H0B 109.46(10) . . ? N4 B H0B 109.46(9) . . ? N2 B H0B 109.46(9) . . ? C22 N2 N3 108.09(13) . . ? C22 N2 B 126.04(14) . . ? N3 N2 B 125.86(13) . . ? C20 N3 N2 106.55(13) . . ? C20 N3 Ru 121.97(11) . . ? N2 N3 Ru 131.26(10) . . ? N3 C20 C21 110.94(15) . . ? N3 C20 H20 124.53(9) . . ? C21 C20 H20 124.53(10) . . ? C22 C21 C20 104.7(2) . . ? C22 C21 H21 127.64(10) . . ? C20 C21 H21 127.64(10) . . ? N2 C22 C21 109.7(2) . . ? N2 C22 H22 125.15(10) . . ? C21 C22 H22 125.15(10) . . ? C25 N4 N5 110.3(2) . . ? C25 N4 B 128.4(2) . . ? N5 N4 B 120.90(15) . . ? C23 N5 N4 104.6(2) . . ? N5 C23 C24 112.3(2) . . ? N5 C23 H23 123.86(14) . . ? C24 C23 H23 123.86(13) . . ? C25 C24 C23 104.5(2) . . ? C25 C24 H24 127.76(14) . . ? C23 C24 H24 127.76(13) . . ? N4 C25 C24 108.4(2) . . ? N4 C25 H25 125.82(11) . . ? C24 C25 H25 125.82(14) . . ? C28 N6 N7 110.6(2) . . ? C28 N6 B 125.7(2) . . ? N7 N6 B 123.7(2) . . ? C26 N7 N6 105.1(2) . . ? N7 C26 C27 110.9(2) . . ? N7 C26 H26 124.6(2) . . ? C27 C26 H26 124.6(2) . . ? C28 C27 C26 106.1(2) . . ? C28 C27 H27 127.0(2) . . ? C26 C27 H27 127.0(2) . . ? N6 C28 C27 107.3(2) . . ? N6 C28 H28 126.35(13) . . ? C27 C28 H28 126.3(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O Ru C1 C2 53.65(11) . . . . ? N1 Ru C1 C2 133.51(10) . . . . ? N3 Ru C1 C2 -136.1(2) . . . . ? C2 Ru C1 C2 0.0 . . . . ? C6 Ru C1 C2 -130.90(14) . . . . ? C3 Ru C1 C2 -29.05(10) . . . . ? C5 Ru C1 C2 -102.36(11) . . . . ? C4 Ru C1 C2 -65.46(10) . . . . ? O Ru C1 C6 -175.44(9) . . . . ? N1 Ru C1 C6 -95.58(10) . . . . ? N3 Ru C1 C6 -5.2(2) . . . . ? C2 Ru C1 C6 130.90(14) . . . . ? C6 Ru C1 C6 0.0 . . . . ? C3 Ru C1 C6 101.85(11) . . . . ? C5 Ru C1 C6 28.54(9) . . . . ? C4 Ru C1 C6 65.44(10) . . . . ? O Ru C1 C7 -60.8(2) . . . . ? N1 Ru C1 C7 19.0(2) . . . . ? N3 Ru C1 C7 109.4(2) . . . . ? C2 Ru C1 C7 -114.5(2) . . . . ? C6 Ru C1 C7 114.6(2) . . . . ? C3 Ru C1 C7 -143.5(2) . . . . ? C5 Ru C1 C7 143.2(2) . . . . ? C4 Ru C1 C7 -179.9(2) . . . . ? C6 C1 C2 C3 0.2(2) . . . . ? C7 C1 C2 C3 175.5(2) . . . . ? Ru C1 C2 C3 53.84(14) . . . . ? C6 C1 C2 Ru -53.67(13) . . . . ? C7 C1 C2 Ru 121.7(2) . . . . ? Ru C1 C2 Ru 0.0 . . . . ? O Ru C2 C1 -132.18(10) . . . . ? N1 Ru C2 C1 -55.29(11) . . . . ? N3 Ru C2 C1 151.63(11) . . . . ? C6 Ru C2 C1 30.34(10) . . . . ? C3 Ru C2 C1 133.34(15) . . . . ? C1 Ru C2 C1 0.0 . . . . ? C5 Ru C2 C1 67.11(10) . . . . ? C4 Ru C2 C1 104.73(11) . . . . ? O Ru C2 C3 94.48(10) . . . . ? N1 Ru C2 C3 171.37(9) . . . . ? N3 Ru C2 C3 18.3(2) . . . . ? C6 Ru C2 C3 -103.01(11) . . . . ? C3 Ru C2 C3 0.0 . . . . ? C1 Ru C2 C3 -133.34(15) . . . . ? C5 Ru C2 C3 -66.23(10) . . . . ? C4 Ru C2 C3 -28.61(10) . . . . ? C1 C2 C3 C4 0.2(3) . . . . ? Ru C2 C3 C4 54.55(14) . . . . ? C1 C2 C3 Ru -54.34(15) . . . . ? Ru C2 C3 Ru 0.0 . . . . ? O Ru C3 C4 141.44(10) . . . . ? N1 Ru C3 C4 -151.61(13) . . . . ? N3 Ru C3 C4 56.34(11) . . . . ? C2 Ru C3 C4 -132.7(2) . . . . ? C6 Ru C3 C4 -66.62(11) . . . . ? C1 Ru C3 C4 -104.47(11) . . . . ? C5 Ru C3 C4 -30.07(10) . . . . ? C4 Ru C3 C4 0.0 . . . . ? O Ru C3 C2 -85.84(10) . . . . ? N1 Ru C3 C2 -18.9(2) . . . . ? N3 Ru C3 C2 -170.95(9) . . . . ? C2 Ru C3 C2 0.0 . . . . ? C6 Ru C3 C2 66.09(11) . . . . ? C1 Ru C3 C2 28.24(10) . . . . ? C5 Ru C3 C2 102.64(11) . . . . ? C4 Ru C3 C2 132.7(2) . . . . ? C2 C3 C4 C5 0.0(2) . . . . ? Ru C3 C4 C5 53.46(13) . . . . ? C2 C3 C4 C8 -178.2(2) . . . . ? Ru C3 C4 C8 -124.7(2) . . . . ? C2 C3 C4 Ru -53.48(14) . . . . ? Ru C3 C4 Ru 0.0 . . . . ? O Ru C4 C3 -46.04(12) . . . . ? N1 Ru C4 C3 144.2(2) . . . . ? N3 Ru C4 C3 -131.28(10) . . . . ? C2 Ru C4 C3 29.41(10) . . . . ? C6 Ru C4 C3 103.01(11) . . . . ? C3 Ru C4 C3 0.0 . . . . ? C1 Ru C4 C3 65.75(11) . . . . ? C5 Ru C4 C3 131.06(15) . . . . ? O Ru C4 C5 -177.09(9) . . . . ? N1 Ru C4 C5 13.1(2) . . . . ? N3 Ru C4 C5 97.66(10) . . . . ? C2 Ru C4 C5 -101.64(11) . . . . ? C6 Ru C4 C5 -28.05(10) . . . . ? C3 Ru C4 C5 -131.06(15) . . . . ? C1 Ru C4 C5 -65.30(10) . . . . ? C5 Ru C4 C5 0.0 . . . . ? O Ru C4 C8 71.8(2) . . . . ? N1 Ru C4 C8 -98.0(2) . . . . ? N3 Ru C4 C8 -13.4(2) . . . . ? C2 Ru C4 C8 147.3(2) . . . . ? C6 Ru C4 C8 -139.1(2) . . . . ? C3 Ru C4 C8 117.8(2) . . . . ? C1 Ru C4 C8 -176.4(2) . . . . ? C5 Ru C4 C8 -111.1(2) . . . . ? C3 C4 C5 C6 -0.6(2) . . . . ? C8 C4 C5 C6 177.7(2) . . . . ? Ru C4 C5 C6 52.74(14) . . . . ? C3 C4 C5 Ru -53.29(13) . . . . ? C8 C4 C5 Ru 124.96(15) . . . . ? Ru C4 C5 Ru 0.0 . . . . ? O Ru C5 C6 -127.17(15) . . . . ? N1 Ru C5 C6 51.30(12) . . . . ? N3 Ru C5 C6 140.81(10) . . . . ? C2 Ru C5 C6 -66.14(10) . . . . ? C6 Ru C5 C6 0.0 . . . . ? C3 Ru C5 C6 -104.17(11) . . . . ? C1 Ru C5 C6 -29.20(10) . . . . ? C4 Ru C5 C6 -133.84(15) . . . . ? O Ru C5 C4 6.7(2) . . . . ? N1 Ru C5 C4 -174.85(8) . . . . ? N3 Ru C5 C4 -85.34(10) . . . . ? C2 Ru C5 C4 67.70(10) . . . . ? C6 Ru C5 C4 133.84(15) . . . . ? C3 Ru C5 C4 29.67(9) . . . . ? C1 Ru C5 C4 104.65(11) . . . . ? C4 Ru C5 C4 0.0 . . . . ? C4 C5 C6 C1 1.0(2) . . . . ? Ru C5 C6 C1 54.15(14) . . . . ? C4 C5 C6 Ru -53.20(14) . . . . ? Ru C5 C6 Ru 0.0 . . . . ? C2 C1 C6 C5 -0.7(2) . . . . ? C7 C1 C6 C5 -176.1(2) . . . . ? Ru C1 C6 C5 -54.41(14) . . . . ? C2 C1 C6 Ru 53.66(14) . . . . ? C7 C1 C6 Ru -121.7(2) . . . . ? Ru C1 C6 Ru 0.0 . . . . ? O Ru C6 C5 141.56(11) . . . . ? N1 Ru C6 C5 -138.86(10) . . . . ? N3 Ru C6 C5 -49.07(12) . . . . ? C2 Ru C6 C5 103.20(11) . . . . ? C3 Ru C6 C5 65.28(10) . . . . ? C1 Ru C6 C5 132.87(15) . . . . ? C5 Ru C6 C5 0.0 . . . . ? C4 Ru C6 C5 28.46(9) . . . . ? O Ru C6 C1 8.7(2) . . . . ? N1 Ru C6 C1 88.26(10) . . . . ? N3 Ru C6 C1 178.05(9) . . . . ? C2 Ru C6 C1 -29.68(9) . . . . ? C3 Ru C6 C1 -67.59(10) . . . . ? C1 Ru C6 C1 0.0 . . . . ? C5 Ru C6 C1 -132.87(15) . . . . ? C4 Ru C6 C1 -104.41(11) . . . . ? C3 C4 C8 C10 8.4(3) . . . . ? C5 C4 C8 C10 -169.8(2) . . . . ? Ru C4 C8 C10 -82.6(2) . . . . ? C3 C4 C8 C9 -116.5(2) . . . . ? C5 C4 C8 C9 65.4(2) . . . . ? Ru C4 C8 C9 152.5(2) . . . . ? O Ru N1 C11 -178.6(2) . . . . ? N3 Ru N1 C11 -93.24(15) . . . . ? C2 Ru N1 C11 98.6(2) . . . . ? C6 Ru N1 C11 30.4(2) . . . . ? C3 Ru N1 C11 111.8(2) . . . . ? C1 Ru N1 C11 68.6(2) . . . . ? C5 Ru N1 C11 1.9(2) . . . . ? C4 Ru N1 C11 -7.6(3) . . . . ? O Ru N1 C19 2.76(10) . . . . ? N3 Ru N1 C19 88.16(11) . . . . ? C2 Ru N1 C19 -80.00(12) . . . . ? C6 Ru N1 C19 -148.24(11) . . . . ? C3 Ru N1 C19 -66.8(2) . . . . ? C1 Ru N1 C19 -109.96(11) . . . . ? C5 Ru N1 C19 -176.65(10) . . . . ? C4 Ru N1 C19 173.78(15) . . . . ? C19 N1 C11 C12 0.0(3) . . . . ? Ru N1 C11 C12 -178.54(13) . . . . ? N1 C11 C12 C13 0.9(3) . . . . ? C11 C12 C13 C14 -0.6(3) . . . . ? C12 C13 C14 C15 179.2(2) . . . . ? C12 C13 C14 C19 -0.5(3) . . . . ? C13 C14 C15 C16 -179.4(2) . . . . ? C19 C14 C15 C16 0.3(3) . . . . ? C14 C15 C16 C17 -1.2(3) . . . . ? C15 C16 C17 C18 0.6(3) . . . . ? C16 C17 C18 O 179.4(2) . . . . ? C16 C17 C18 C19 0.9(3) . . . . ? C11 N1 C19 C14 -1.1(2) . . . . ? Ru N1 C19 C14 177.60(12) . . . . ? C11 N1 C19 C18 179.30(15) . . . . ? Ru N1 C19 C18 -2.0(2) . . . . ? C13 C14 C19 N1 1.4(2) . . . . ? C15 C14 C19 N1 -178.3(2) . . . . ? C13 C14 C19 C18 -179.1(2) . . . . ? C15 C14 C19 C18 1.2(3) . . . . ? O C18 C19 N1 -0.9(2) . . . . ? C17 C18 C19 N1 177.78(15) . . . . ? O C18 C19 C14 179.56(15) . . . . ? C17 C18 C19 C14 -1.8(2) . . . . ? C17 C18 O Ru -175.26(13) . . . . ? C19 C18 O Ru 3.3(2) . . . . ? N1 Ru O C18 -3.28(10) . . . . ? N3 Ru O C18 -90.25(11) . . . . ? C2 Ru O C18 115.93(11) . . . . ? C6 Ru O C18 80.89(15) . . . . ? C3 Ru O C18 154.26(11) . . . . ? C1 Ru O C18 86.72(11) . . . . ? C5 Ru O C18 175.42(14) . . . . ? C4 Ru O C18 -179.86(10) . . . . ? N6 B N2 C22 63.9(2) . . . . ? N4 B N2 C22 -56.3(2) . . . . ? N6 B N2 N3 -116.1(2) . . . . ? N4 B N2 N3 123.7(2) . . . . ? C22 N2 N3 C20 -0.2(2) . . . . ? B N2 N3 C20 179.8(2) . . . . ? C22 N2 N3 Ru 174.29(12) . . . . ? B N2 N3 Ru -5.7(2) . . . . ? O Ru N3 C20 -28.60(13) . . . . ? N1 Ru N3 C20 -107.89(13) . . . . ? C2 Ru N3 C20 48.6(2) . . . . ? C6 Ru N3 C20 156.55(13) . . . . ? C3 Ru N3 C20 61.06(14) . . . . ? C1 Ru N3 C20 160.4(2) . . . . ? C5 Ru N3 C20 129.13(13) . . . . ? C4 Ru N3 C20 91.39(13) . . . . ? O Ru N3 N2 157.63(13) . . . . ? N1 Ru N3 N2 78.33(13) . . . . ? C2 Ru N3 N2 -125.2(2) . . . . ? C6 Ru N3 N2 -17.2(2) . . . . ? C3 Ru N3 N2 -112.71(13) . . . . ? C1 Ru N3 N2 -13.4(3) . . . . ? C5 Ru N3 N2 -44.64(14) . . . . ? C4 Ru N3 N2 -82.38(14) . . . . ? N2 N3 C20 C21 0.5(2) . . . . ? Ru N3 C20 C21 -174.62(11) . . . . ? N3 C20 C21 C22 -0.6(2) . . . . ? N3 N2 C22 C21 -0.2(2) . . . . ? B N2 C22 C21 179.9(2) . . . . ? C20 C21 C22 N2 0.5(2) . . . . ? N6 B N4 C25 -45.0(2) . . . . ? N2 B N4 C25 75.9(2) . . . . ? N6 B N4 N5 143.0(2) . . . . ? N2 B N4 N5 -96.1(2) . . . . ? C25 N4 N5 C23 0.3(2) . . . . ? B N4 N5 C23 173.6(2) . . . . ? N4 N5 C23 C24 -0.2(2) . . . . ? N5 C23 C24 C25 0.1(3) . . . . ? N5 N4 C25 C24 -0.2(2) . . . . ? B N4 C25 C24 -172.9(2) . . . . ? C23 C24 C25 N4 0.0(2) . . . . ? N4 B N6 C28 -109.8(2) . . . . ? N2 B N6 C28 131.2(2) . . . . ? N4 B N6 N7 69.8(2) . . . . ? N2 B N6 N7 -49.2(2) . . . . ? C28 N6 N7 C26 -1.3(2) . . . . ? B N6 N7 C26 179.0(2) . . . . ? N6 N7 C26 C27 1.2(3) . . . . ? N7 C26 C27 C28 -0.8(3) . . . . ? N7 N6 C28 C27 0.8(3) . . . . ? B N6 C28 C27 -179.5(2) . . . . ? C26 C27 C28 N6 -0.1(3) . . . . ? _refine_diff_density_max 0.339 _refine_diff_density_min -0.294 _refine_diff_density_rms 0.056 #===END #====== kipx478 compound 6.CHCl~3~ in text ================== data_kipx478 _audit_creation_method SHELXL-97 _chemical_name_systematic ; (8-hydroxyquinolinato-N,O)-(eta$6!-p-cymene)-(pyrrole-N)-ruthenium(II) trifluoromethanesulfonate chloroform solvate (1:1) ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H25 Cl3 F3 N3 O4 Ru S' _chemical_formula_weight 715.95 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ru' 'Ru' -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.899(4) _cell_length_b 12.855(6) _cell_length_c 12.936(6) _cell_angle_alpha 115.46(2) _cell_angle_beta 99.12(2) _cell_angle_gamma 93.28(2) _cell_volume 1452.9(11) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 8192 _cell_measurement_theta_min 2 _cell_measurement_theta_max 30 _exptl_crystal_description oval _exptl_crystal_colour orange _exptl_crystal_size_max 0.6 _exptl_crystal_size_mid 0.5 _exptl_crystal_size_min 0.4 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.637 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 720 _exptl_absorpt_coefficient_mu 0.942 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.54 _exptl_absorpt_correction_T_max 0.60 _exptl_absorpt_process_details ? _exptl_special_details ; Siemens SMART platform 3-circle diffractometer with CCD area detector, sealed X-ray tube, graphite monochromator. One complete sphere of the reciprocal space up to theta(max) = 30 deg was measured by omega scan frames with delta(omega) = 0.30 deg and 20 sec per frame, 4 x 606 frames recorded using program SMART (Siemens/Bruker). Data collection at 223(2) K using a nitrogen gas stream cooling device. Frame data evaluation with program SAINT (Siemens/Bruker); lattice parameters by least-squares refinement of the geometric parameters of the strongest reflections. Correction for absorption and crystal decay (insignificant) by semi-empirical method from equivalents (multi-scan method) using program SADABS (G.M. Sheldrick, 1996, Univ. of Goettingen, Germany). Data reduction with program XPREP (Siemens/Bruker). ; _diffrn_ambient_temperature 223(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 'Siemens SMART 3-circle with CCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20908 _diffrn_reflns_av_R_equivalents 0.0166 _diffrn_reflns_av_sigmaI/netI 0.0184 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.78 _diffrn_reflns_theta_max 29.99 _reflns_number_total 8201 _reflns_number_gt 7754 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART' _computing_cell_refinement 'Siemens SAINT' _computing_data_reduction 'Siemens SAINT and SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; 1) 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. 2) Hydrogen atoms were inserted in calculated positions and were refined riding with the atoms to which they were bonded. The phenyl bonded C(7)H~3~ group was allowed to rotate about the C-C(H~3~) bond axis, using instruction AFIX 137 of program SHELXL97. 3) The 2-propyl residue of the cymene moiety is disordered and adopts two orientations - one consisting of C(8a), C9a), and C(10a), and one consisting of C(8b), C(9b), and C(10b). The refined population parameters for A- and B-orientation are 0.560(6) and 0.440(6), respectively. SADI distance restraints of program SHELXL97 have been used for these atoms during refinement. Anisotropic thermal parameters of C(8a)/C(8b) and C(10a)/C(10b) have been equivalenced. 4) Population parameter of CHCl~3~ solvent molecule consisting of C(24), H(24), Cl(1), Cl(2), and Cl(3), was refined to 0.976(3). ; _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^)+(0.0402P)^2^+1.6429P] 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 SHELXL _refine_ls_extinction_coef 0.0125(7) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 8201 _refine_ls_number_parameters 371 _refine_ls_number_restraints 13 _refine_ls_R_factor_all 0.0373 _refine_ls_R_factor_gt 0.0348 _refine_ls_wR_factor_ref 0.0891 _refine_ls_wR_factor_gt 0.0857 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.052 _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 Ru Ru 0.428671(15) 0.248590(12) 0.136289(12) 0.02399(6) Uani 1 1 d . A . C1 C 0.5617(3) 0.3169(2) 0.31348(19) 0.0385(5) Uani 1 1 d . A . C2 C 0.4232(3) 0.3178(2) 0.3230(2) 0.0415(5) Uani 1 1 d . . . H2 H 0.3939 0.3866 0.3730 0.050 Uiso 1 1 calc R . . C3 C 0.3269(3) 0.2157(3) 0.2577(2) 0.0467(6) Uani 1 1 d . A . H3 H 0.2338 0.2186 0.2642 0.056 Uiso 1 1 calc R . . C4 C 0.3655(3) 0.1103(2) 0.1838(2) 0.0453(6) Uani 1 1 d D . . C5 C 0.5060(3) 0.1100(2) 0.1734(2) 0.0418(5) Uani 1 1 d . A . H5 H 0.5346 0.0408 0.1233 0.050 Uiso 1 1 calc R . . C6 C 0.6033(3) 0.2107(2) 0.2362(2) 0.0386(5) Uani 1 1 d . . . H6 H 0.6958 0.2084 0.2277 0.046 Uiso 1 1 calc R A . C7 C 0.6640(4) 0.4262(3) 0.3807(3) 0.0629(9) Uani 1 1 d . . . H7A H 0.7085 0.4290 0.4545 0.094 Uiso 1 1 calc R A . H7B H 0.6163 0.4934 0.3955 0.094 Uiso 1 1 calc R . . H7C H 0.7332 0.4265 0.3354 0.094 Uiso 1 1 calc R . . C8A C 0.2864(5) -0.0146(4) 0.1054(4) 0.0429(9) Uani 0.560(6) 1 d PD A 1 H8A H 0.3398 -0.0594 0.0463 0.051 Uiso 0.560(6) 1 calc PR A 1 C9A C 0.1456(6) -0.0061(6) 0.0443(7) 0.076(2) Uani 0.560(6) 1 d PD A 1 H9A H 0.1558 0.0060 -0.0233 0.114 Uiso 0.560(6) 1 calc PR A 1 H9B H 0.1076 0.0588 0.0981 0.114 Uiso 0.560(6) 1 calc PR A 1 H9C H 0.0838 -0.0776 0.0193 0.114 Uiso 0.560(6) 1 calc PR A 1 C10A C 0.2728(9) -0.0721(7) 0.1857(7) 0.057(2) Uani 0.560(6) 1 d PD A 1 H10A H 0.2101 -0.1446 0.1430 0.086 Uiso 0.560(6) 1 calc PR A 1 H10B H 0.2369 -0.0204 0.2523 0.086 Uiso 0.560(6) 1 calc PR A 1 H10C H 0.3629 -0.0878 0.2129 0.086 Uiso 0.560(6) 1 calc PR A 1 C8B C 0.2346(7) 0.0178(5) 0.1364(4) 0.0429(9) Uani 0.44 1 d PD A 2 H8B H 0.1505 0.0564 0.1426 0.051 Uiso 0.440(6) 1 calc PR A 2 C9B C 0.2333(7) -0.0632(5) 0.0086(5) 0.0501(16) Uani 0.440(6) 1 d PD A 2 H9D H 0.1977 -0.0268 -0.0400 0.075 Uiso 0.440(6) 1 calc PR A 2 H9E H 0.1748 -0.1360 -0.0147 0.075 Uiso 0.440(6) 1 calc PR A 2 H9F H 0.3266 -0.0784 -0.0007 0.075 Uiso 0.440(6) 1 calc PR A 2 C10B C 0.2447(13) -0.0476(9) 0.2113(8) 0.057(2) Uani 0.44 1 d PD A 2 H10D H 0.1789 -0.1185 0.1724 0.086 Uiso 0.440(6) 1 calc PR A 2 H10E H 0.2240 0.0011 0.2868 0.086 Uiso 0.440(6) 1 calc PR A 2 H10F H 0.3375 -0.0671 0.2221 0.086 Uiso 0.440(6) 1 calc PR A 2 O1 O 0.41993(17) 0.14963(12) -0.03995(13) 0.0310(3) Uani 1 1 d . . . N1 N 0.24897(17) 0.29262(15) 0.06538(16) 0.0279(3) Uani 1 1 d . . . C11 C 0.1652(2) 0.3635(2) 0.1217(2) 0.0357(4) Uani 1 1 d . A . H11 H 0.1856 0.4009 0.2039 0.043 Uiso 1 1 calc R . . C12 C 0.0457(3) 0.3846(2) 0.0615(3) 0.0456(6) Uani 1 1 d . . . H12 H -0.0124 0.4348 0.1038 0.055 Uiso 1 1 calc R A . C13 C 0.0149(2) 0.3323(2) -0.0575(3) 0.0465(6) Uani 1 1 d . A . H13 H -0.0648 0.3457 -0.0975 0.056 Uiso 1 1 calc R . . C14 C 0.1038(2) 0.2573(2) -0.1213(2) 0.0391(5) Uani 1 1 d . . . C15 C 0.0848(3) 0.2011(3) -0.2445(3) 0.0515(7) Uani 1 1 d . A . H15 H 0.0090 0.2117 -0.2911 0.062 Uiso 1 1 calc R . . C16 C 0.1779(4) 0.1314(2) -0.2950(2) 0.0536(7) Uani 1 1 d . . . H16 H 0.1647 0.0947 -0.3770 0.064 Uiso 1 1 calc R A . C17 C 0.2929(3) 0.1118(2) -0.2297(2) 0.0434(5) Uani 1 1 d . A . H17 H 0.3542 0.0628 -0.2684 0.052 Uiso 1 1 calc R . . C18 C 0.3162(2) 0.16470(17) -0.10811(18) 0.0310(4) Uani 1 1 d . A . C19 C 0.2204(2) 0.23888(17) -0.05493(18) 0.0301(4) Uani 1 1 d . A . N2 N 0.53367(18) 0.37807(14) 0.10627(15) 0.0276(3) Uani 1 1 d . . . N3 N 0.5422(2) 0.49381(15) 0.17329(16) 0.0317(3) Uani 1 1 d . A . H3N H 0.4984 0.5251 0.2301 0.038 Uiso 1 1 calc R . . C20 C 0.6155(2) 0.3666(2) 0.0302(2) 0.0346(4) Uani 1 1 d . A . H20 H 0.6301 0.2951 -0.0276 0.041 Uiso 1 1 calc R . . C21 C 0.6763(2) 0.4756(2) 0.0486(2) 0.0391(5) Uani 1 1 d . . . H21 H 0.7375 0.4915 0.0069 0.047 Uiso 1 1 calc R A . C22 C 0.6272(3) 0.5544(2) 0.1407(2) 0.0378(5) Uani 1 1 d . A . H22 H 0.6490 0.6358 0.1749 0.045 Uiso 1 1 calc R . . S S 0.29923(7) 0.66819(5) 0.34258(5) 0.04041(13) Uani 1 1 d . . . O2 O 0.4037(2) 0.60053(19) 0.36116(18) 0.0558(5) Uani 1 1 d . . . O3 O 0.1779(3) 0.6537(3) 0.3845(3) 0.0855(9) Uani 1 1 d . . . O4 O 0.2759(3) 0.6631(2) 0.22799(18) 0.0603(6) Uani 1 1 d . . . C23 C 0.3763(4) 0.8179(3) 0.4382(3) 0.0591(8) Uani 1 1 d . . . F1 F 0.2896(4) 0.89082(19) 0.4332(2) 0.0980(9) Uani 1 1 d . . . F2 F 0.4881(3) 0.8447(3) 0.4062(3) 0.1086(10) Uani 1 1 d . . . F3 F 0.4102(4) 0.8365(2) 0.54799(17) 0.1032(10) Uani 1 1 d . . . C24 C -0.0289(5) 0.7215(4) 0.5504(4) 0.0864(15) Uani 0.976(3) 1 d P . . H24 H 0.0268 0.6891 0.4895 0.104 Uiso 0.976(3) 1 calc PR . . Cl1 Cl -0.03829(14) 0.63083(13) 0.62010(14) 0.0972(5) Uani 0.976(3) 1 d P . . Cl2 Cl 0.04710(15) 0.86279(11) 0.64885(17) 0.1223(7) Uani 0.976(3) 1 d P . . Cl3 Cl -0.19972(17) 0.72488(12) 0.48227(10) 0.1024(5) Uani 0.976(3) 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 Ru 0.02993(9) 0.02075(8) 0.02440(8) 0.01199(6) 0.00728(5) 0.00637(5) C1 0.0533(13) 0.0334(10) 0.0285(10) 0.0171(8) -0.0013(9) 0.0038(9) C2 0.0628(15) 0.0419(12) 0.0288(10) 0.0193(9) 0.0181(10) 0.0227(11) C3 0.0463(13) 0.0689(17) 0.0471(13) 0.0422(13) 0.0191(11) 0.0129(12) C4 0.0606(15) 0.0393(12) 0.0426(12) 0.0294(11) 0.0005(11) -0.0070(11) C5 0.0712(16) 0.0282(10) 0.0334(10) 0.0190(9) 0.0105(10) 0.0191(10) C6 0.0412(11) 0.0447(12) 0.0391(11) 0.0256(10) 0.0084(9) 0.0172(10) C7 0.077(2) 0.0491(16) 0.0483(15) 0.0234(13) -0.0216(15) -0.0149(14) C8A 0.048(2) 0.035(2) 0.051(2) 0.0233(18) 0.0153(16) 0.0010(14) C9A 0.080(5) 0.052(3) 0.083(5) 0.034(3) -0.017(4) -0.015(3) C10A 0.069(4) 0.047(4) 0.075(4) 0.041(3) 0.027(3) 0.002(3) C8B 0.048(2) 0.035(2) 0.051(2) 0.0233(18) 0.0153(16) 0.0010(14) C9B 0.056(4) 0.043(3) 0.047(3) 0.020(3) 0.005(3) -0.005(3) C10B 0.069(4) 0.047(4) 0.075(4) 0.041(3) 0.027(3) 0.002(3) O1 0.0424(8) 0.0248(6) 0.0266(7) 0.0110(5) 0.0084(6) 0.0093(6) N1 0.0278(7) 0.0256(7) 0.0342(8) 0.0169(7) 0.0064(6) 0.0041(6) C11 0.0336(10) 0.0342(10) 0.0464(12) 0.0222(9) 0.0129(9) 0.0093(8) C12 0.0323(11) 0.0468(13) 0.0714(18) 0.0369(13) 0.0139(11) 0.0131(10) C13 0.0310(11) 0.0466(13) 0.0716(18) 0.0394(13) -0.0013(11) 0.0032(9) C14 0.0347(10) 0.0362(11) 0.0487(13) 0.0271(10) -0.0058(9) -0.0053(8) C15 0.0552(15) 0.0482(14) 0.0471(14) 0.0282(12) -0.0160(12) -0.0083(12) C16 0.077(2) 0.0429(13) 0.0329(12) 0.0182(10) -0.0087(12) -0.0072(13) C17 0.0661(16) 0.0309(10) 0.0289(10) 0.0120(9) 0.0038(10) 0.0019(10) C18 0.0436(11) 0.0213(8) 0.0273(9) 0.0118(7) 0.0036(8) 0.0004(7) C19 0.0328(9) 0.0259(9) 0.0336(10) 0.0175(8) 0.0014(7) -0.0017(7) N2 0.0320(8) 0.0238(7) 0.0294(8) 0.0132(6) 0.0087(6) 0.0052(6) N3 0.0420(9) 0.0237(8) 0.0315(8) 0.0121(7) 0.0127(7) 0.0072(7) C20 0.0369(10) 0.0328(10) 0.0381(11) 0.0165(9) 0.0159(9) 0.0078(8) C21 0.0372(11) 0.0404(12) 0.0469(12) 0.0246(10) 0.0149(9) 0.0014(9) C22 0.0448(12) 0.0284(10) 0.0423(12) 0.0185(9) 0.0087(9) -0.0011(8) S 0.0456(3) 0.0399(3) 0.0398(3) 0.0174(2) 0.0168(2) 0.0168(2) O2 0.0762(14) 0.0532(11) 0.0484(11) 0.0255(9) 0.0228(10) 0.0366(11) O3 0.0738(17) 0.089(2) 0.114(2) 0.0488(18) 0.0589(17) 0.0250(15) O4 0.0710(14) 0.0657(13) 0.0367(10) 0.0180(9) 0.0010(9) 0.0186(11) C23 0.096(2) 0.0440(14) 0.0372(13) 0.0196(11) 0.0074(14) 0.0124(15) F1 0.171(3) 0.0505(11) 0.0762(15) 0.0295(11) 0.0186(16) 0.0505(15) F2 0.109(2) 0.096(2) 0.105(2) 0.0414(17) 0.0092(17) -0.0364(16) F3 0.196(3) 0.0635(13) 0.0350(9) 0.0161(9) -0.0037(13) 0.0242(16) C24 0.094(3) 0.066(2) 0.084(3) 0.007(2) 0.058(2) -0.011(2) Cl1 0.0895(8) 0.1025(9) 0.1206(11) 0.0544(8) 0.0552(8) 0.0381(7) Cl2 0.0870(8) 0.0673(7) 0.1560(15) 0.0001(8) 0.0265(9) -0.0151(6) Cl3 0.1377(12) 0.1017(9) 0.0647(6) 0.0440(6) 0.0099(6) -0.0343(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru O1 2.0627(17) . ? Ru N1 2.0905(18) . ? Ru N2 2.1184(18) . ? Ru C3 2.165(2) . ? Ru C5 2.183(2) . ? Ru C2 2.197(2) . ? Ru C6 2.197(2) . ? Ru C4 2.205(2) . ? Ru C1 2.223(2) . ? C1 C2 1.397(4) . ? C1 C6 1.433(3) . ? C1 C7 1.504(4) . ? C2 C3 1.411(4) . ? C2 H2 0.9400 . ? C3 C4 1.398(4) . ? C3 H3 0.9400 . ? C4 C5 1.419(4) . ? C4 C8B 1.553(7) . ? C4 C8A 1.557(5) . ? C5 C6 1.402(4) . ? C5 H5 0.9400 . ? C6 H6 0.9400 . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C7 H7C 0.9700 . ? C8A C9A 1.523(4) . ? C8A C10A 1.529(4) . ? C8A H8A 0.9900 . ? C9A H9A 0.9700 . ? C9A H9B 0.9700 . ? C9A H9C 0.9700 . ? C10A H10A 0.9700 . ? C10A H10B 0.9700 . ? C10A H10C 0.9700 . ? C8B C9B 1.526(5) . ? C8B C10B 1.528(4) . ? C8B H8B 0.9900 . ? C9B H9D 0.9700 . ? C9B H9E 0.9700 . ? C9B H9F 0.9700 . ? C10B H10D 0.9700 . ? C10B H10E 0.9700 . ? C10B H10F 0.9700 . ? O1 C18 1.323(3) . ? N1 C11 1.326(3) . ? N1 C19 1.376(3) . ? C11 C12 1.416(3) . ? C11 H11 0.9400 . ? C12 C13 1.361(4) . ? C12 H12 0.9400 . ? C13 C14 1.424(4) . ? C13 H13 0.9400 . ? C14 C15 1.414(4) . ? C14 C19 1.420(3) . ? C15 C16 1.365(5) . ? C15 H15 0.9400 . ? C16 C17 1.408(4) . ? C16 H16 0.9400 . ? C17 C18 1.392(3) . ? C17 H17 0.9400 . ? C18 C19 1.425(3) . ? N2 C20 1.337(3) . ? N2 N3 1.351(2) . ? N3 C22 1.346(3) . ? N3 H3N 0.8700 . ? C20 C21 1.399(3) . ? C20 H20 0.9400 . ? C21 C22 1.373(4) . ? C21 H21 0.9400 . ? C22 H22 0.9400 . ? S O3 1.428(3) . ? S O4 1.436(2) . ? S O2 1.445(2) . ? S C23 1.817(3) . ? C23 F3 1.317(3) . ? C23 F2 1.319(5) . ? C23 F1 1.321(4) . ? C24 Cl2 1.743(4) . ? C24 Cl1 1.760(5) . ? C24 Cl3 1.791(6) . ? C24 H24 0.9900 . ? 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 O1 Ru N1 79.36(7) . . ? O1 Ru N2 82.75(7) . . ? N1 Ru N2 85.11(7) . . ? O1 Ru C3 131.01(10) . . ? N1 Ru C3 91.93(9) . . ? N2 Ru C3 144.99(10) . . ? O1 Ru C5 90.62(8) . . ? N1 Ru C5 141.87(9) . . ? N2 Ru C5 130.38(9) . . ? C3 Ru C5 67.22(11) . . ? O1 Ru C2 167.61(8) . . ? N1 Ru C2 103.69(9) . . ? N2 Ru C2 109.36(9) . . ? C3 Ru C2 37.75(11) . . ? C5 Ru C2 79.58(9) . . ? O1 Ru C6 109.08(8) . . ? N1 Ru C6 170.75(8) . . ? N2 Ru C6 99.47(9) . . ? C3 Ru C6 79.69(10) . . ? C5 Ru C6 37.34(10) . . ? C2 Ru C6 67.25(10) . . ? O1 Ru C4 99.66(9) . . ? N1 Ru C4 107.49(9) . . ? N2 Ru C4 167.40(9) . . ? C3 Ru C4 37.31(11) . . ? C5 Ru C4 37.73(11) . . ? C2 Ru C4 67.95(10) . . ? C6 Ru C4 68.01(10) . . ? O1 Ru C1 144.55(9) . . ? N1 Ru C1 134.83(9) . . ? N2 Ru C1 90.34(8) . . ? C3 Ru C1 67.42(11) . . ? C5 Ru C1 67.74(9) . . ? C2 Ru C1 36.84(10) . . ? C6 Ru C1 37.83(9) . . ? C4 Ru C1 80.52(10) . . ? C2 C1 C6 118.6(2) . . ? C2 C1 C7 120.5(3) . . ? C6 C1 C7 120.9(3) . . ? C2 C1 Ru 70.58(14) . . ? C6 C1 Ru 70.12(13) . . ? C7 C1 Ru 129.84(17) . . ? C1 C2 C3 120.3(2) . . ? C1 C2 Ru 72.59(13) . . ? C3 C2 Ru 69.89(14) . . ? C1 C2 H2 119.8 . . ? C3 C2 H2 119.8 . . ? Ru C2 H2 130.2 . . ? C4 C3 C2 122.2(2) . . ? C4 C3 Ru 72.91(14) . . ? C2 C3 Ru 72.36(14) . . ? C4 C3 H3 118.9 . . ? C2 C3 H3 118.9 . . ? Ru C3 H3 128.1 . . ? C3 C4 C5 117.3(2) . . ? C3 C4 C8B 106.7(3) . . ? C5 C4 C8B 135.9(3) . . ? C3 C4 C8A 134.0(3) . . ? C5 C4 C8A 108.7(3) . . ? C8B C4 C8A 27.4(3) . . ? C3 C4 Ru 69.78(14) . . ? C5 C4 Ru 70.29(13) . . ? C8B C4 Ru 131.8(3) . . ? C8A C4 Ru 130.1(2) . . ? C6 C5 C4 121.5(2) . . ? C6 C5 Ru 71.88(13) . . ? C4 C5 Ru 71.97(13) . . ? C6 C5 H5 119.2 . . ? C4 C5 H5 119.2 . . ? Ru C5 H5 129.4 . . ? C5 C6 C1 120.0(2) . . ? C5 C6 Ru 70.78(14) . . ? C1 C6 Ru 72.05(13) . . ? C5 C6 H6 120.0 . . ? C1 C6 H6 120.0 . . ? Ru C6 H6 129.6 . . ? C1 C7 H7A 109.5 . . ? C1 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C1 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C9A C8A C10A 111.7(5) . . ? C9A C8A C4 109.0(4) . . ? C10A C8A C4 107.0(5) . . ? C9A C8A H8A 109.7 . . ? C10A C8A H8A 109.7 . . ? C4 C8A H8A 109.7 . . ? C8A C9A H9A 109.5 . . ? C8A C9A H9B 109.5 . . ? H9A C9A H9B 109.5 . . ? C8A C9A H9C 109.5 . . ? H9A C9A H9C 109.5 . . ? H9B C9A H9C 109.5 . . ? C8A C10A H10A 109.5 . . ? C8A C10A H10B 109.5 . . ? H10A C10A H10B 109.5 . . ? C8A C10A H10C 109.5 . . ? H10A C10A H10C 109.5 . . ? H10B C10A H10C 109.5 . . ? C9B C8B C10B 111.6(5) . . ? C9B C8B C4 107.9(4) . . ? C10B C8B C4 107.3(6) . . ? C9B C8B H8B 110.0 . . ? C10B C8B H8B 110.0 . . ? C4 C8B H8B 110.0 . . ? C8B C9B H9D 109.5 . . ? C8B C9B H9E 109.5 . . ? H9D C9B H9E 109.5 . . ? C8B C9B H9F 109.5 . . ? H9D C9B H9F 109.5 . . ? H9E C9B H9F 109.5 . . ? C8B C10B H10D 109.5 . . ? C8B C10B H10E 109.5 . . ? H10D C10B H10E 109.5 . . ? C8B C10B H10F 109.5 . . ? H10D C10B H10F 109.5 . . ? H10E C10B H10F 109.5 . . ? C18 O1 Ru 113.84(13) . . ? C11 N1 C19 119.31(19) . . ? C11 N1 Ru 128.09(16) . . ? C19 N1 Ru 112.60(14) . . ? N1 C11 C12 121.8(2) . . ? N1 C11 H11 119.1 . . ? C12 C11 H11 119.1 . . ? C13 C12 C11 120.0(2) . . ? C13 C12 H12 120.0 . . ? C11 C12 H12 120.0 . . ? C12 C13 C14 119.9(2) . . ? C12 C13 H13 120.0 . . ? C14 C13 H13 120.0 . . ? C15 C14 C19 118.2(2) . . ? C15 C14 C13 125.0(2) . . ? C19 C14 C13 116.9(2) . . ? C16 C15 C14 119.1(2) . . ? C16 C15 H15 120.4 . . ? C14 C15 H15 120.4 . . ? C15 C16 C17 123.0(3) . . ? C15 C16 H16 118.5 . . ? C17 C16 H16 118.5 . . ? C18 C17 C16 120.2(3) . . ? C18 C17 H17 119.9 . . ? C16 C17 H17 119.9 . . ? O1 C18 C17 124.4(2) . . ? O1 C18 C19 118.59(18) . . ? C17 C18 C19 117.0(2) . . ? N1 C19 C14 122.1(2) . . ? N1 C19 C18 115.50(18) . . ? C14 C19 C18 122.4(2) . . ? C20 N2 N3 105.62(17) . . ? C20 N2 Ru 129.49(14) . . ? N3 N2 Ru 124.50(13) . . ? C22 N3 N2 111.22(18) . . ? C22 N3 H3N 124.4 . . ? N2 N3 H3N 124.4 . . ? N2 C20 C21 110.6(2) . . ? N2 C20 H20 124.7 . . ? C21 C20 H20 124.7 . . ? C22 C21 C20 105.0(2) . . ? C22 C21 H21 127.5 . . ? C20 C21 H21 127.5 . . ? N3 C22 C21 107.6(2) . . ? N3 C22 H22 126.2 . . ? C21 C22 H22 126.2 . . ? O3 S O4 115.64(18) . . ? O3 S O2 113.41(17) . . ? O4 S O2 113.92(13) . . ? O3 S C23 104.33(18) . . ? O4 S C23 103.81(14) . . ? O2 S C23 103.92(16) . . ? F3 C23 F2 108.5(3) . . ? F3 C23 F1 107.8(3) . . ? F2 C23 F1 107.0(3) . . ? F3 C23 S 111.8(2) . . ? F2 C23 S 110.8(2) . . ? F1 C23 S 110.8(3) . . ? Cl2 C24 Cl1 111.7(3) . . ? Cl2 C24 Cl3 109.3(3) . . ? Cl1 C24 Cl3 109.1(2) . . ? Cl2 C24 H24 108.9 . . ? Cl1 C24 H24 108.9 . . ? Cl3 C24 H24 108.9 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Ru C1 C2 -159.04(14) . . . . ? N1 Ru C1 C2 39.60(18) . . . . ? N2 Ru C1 C2 123.04(14) . . . . ? C3 Ru C1 C2 -29.17(15) . . . . ? C5 Ru C1 C2 -102.73(16) . . . . ? C6 Ru C1 C2 -131.9(2) . . . . ? C4 Ru C1 C2 -65.67(16) . . . . ? O1 Ru C1 C6 -27.2(2) . . . . ? N1 Ru C1 C6 171.46(13) . . . . ? N2 Ru C1 C6 -105.11(15) . . . . ? C3 Ru C1 C6 102.69(17) . . . . ? C5 Ru C1 C6 29.12(15) . . . . ? C2 Ru C1 C6 131.9(2) . . . . ? C4 Ru C1 C6 66.18(16) . . . . ? O1 Ru C1 C7 87.0(3) . . . . ? N1 Ru C1 C7 -74.4(3) . . . . ? N2 Ru C1 C7 9.1(3) . . . . ? C3 Ru C1 C7 -143.2(3) . . . . ? C5 Ru C1 C7 143.3(3) . . . . ? C2 Ru C1 C7 -114.0(3) . . . . ? C6 Ru C1 C7 114.2(3) . . . . ? C4 Ru C1 C7 -179.7(3) . . . . ? C6 C1 C2 C3 0.2(3) . . . . ? C7 C1 C2 C3 178.6(2) . . . . ? Ru C1 C2 C3 53.08(19) . . . . ? C6 C1 C2 Ru -52.92(18) . . . . ? C7 C1 C2 Ru 125.5(2) . . . . ? O1 Ru C2 C1 104.8(4) . . . . ? N1 Ru C2 C1 -152.27(13) . . . . ? N2 Ru C2 C1 -62.69(15) . . . . ? C3 Ru C2 C1 132.7(2) . . . . ? C5 Ru C2 C1 66.62(15) . . . . ? C6 Ru C2 C1 29.70(14) . . . . ? C4 Ru C2 C1 104.14(16) . . . . ? O1 Ru C2 C3 -27.9(5) . . . . ? N1 Ru C2 C3 75.04(16) . . . . ? N2 Ru C2 C3 164.62(14) . . . . ? C5 Ru C2 C3 -66.07(17) . . . . ? C6 Ru C2 C3 -102.99(17) . . . . ? C4 Ru C2 C3 -28.55(16) . . . . ? C1 Ru C2 C3 -132.7(2) . . . . ? C1 C2 C3 C4 1.3(3) . . . . ? Ru C2 C3 C4 55.6(2) . . . . ? C1 C2 C3 Ru -54.3(2) . . . . ? O1 Ru C3 C4 39.3(2) . . . . ? N1 Ru C3 C4 116.86(16) . . . . ? N2 Ru C3 C4 -158.92(15) . . . . ? C5 Ru C3 C4 -30.23(16) . . . . ? C2 Ru C3 C4 -133.1(2) . . . . ? C6 Ru C3 C4 -67.09(17) . . . . ? C1 Ru C3 C4 -104.55(17) . . . . ? O1 Ru C3 C2 172.36(12) . . . . ? N1 Ru C3 C2 -110.08(15) . . . . ? N2 Ru C3 C2 -25.9(2) . . . . ? C5 Ru C3 C2 102.83(17) . . . . ? C6 Ru C3 C2 65.97(16) . . . . ? C4 Ru C3 C2 133.1(2) . . . . ? C1 Ru C3 C2 28.51(14) . . . . ? C2 C3 C4 C5 -1.9(3) . . . . ? Ru C3 C4 C5 53.49(19) . . . . ? C2 C3 C4 C8B 175.4(3) . . . . ? Ru C3 C4 C8B -129.2(2) . . . . ? C2 C3 C4 C8A 177.9(3) . . . . ? Ru C3 C4 C8A -126.7(3) . . . . ? C2 C3 C4 Ru -55.4(2) . . . . ? O1 Ru C4 C3 -150.99(16) . . . . ? N1 Ru C4 C3 -69.20(17) . . . . ? N2 Ru C4 C3 108.9(4) . . . . ? C5 Ru C4 C3 130.7(2) . . . . ? C2 Ru C4 C3 28.86(16) . . . . ? C6 Ru C4 C3 102.21(18) . . . . ? C1 Ru C4 C3 64.97(17) . . . . ? O1 Ru C4 C5 78.34(15) . . . . ? N1 Ru C4 C5 160.13(14) . . . . ? N2 Ru C4 C5 -21.8(5) . . . . ? C3 Ru C4 C5 -130.7(2) . . . . ? C2 Ru C4 C5 -101.81(16) . . . . ? C6 Ru C4 C5 -28.46(14) . . . . ? C1 Ru C4 C5 -65.70(15) . . . . ? O1 Ru C4 C8B -56.4(4) . . . . ? N1 Ru C4 C8B 25.4(4) . . . . ? N2 Ru C4 C8B -156.5(4) . . . . ? C3 Ru C4 C8B 94.6(4) . . . . ? C5 Ru C4 C8B -134.7(4) . . . . ? C2 Ru C4 C8B 123.5(4) . . . . ? C6 Ru C4 C8B -163.2(4) . . . . ? C1 Ru C4 C8B 159.6(4) . . . . ? O1 Ru C4 C8A -19.9(3) . . . . ? N1 Ru C4 C8A 61.9(3) . . . . ? N2 Ru C4 C8A -120.0(4) . . . . ? C3 Ru C4 C8A 131.1(4) . . . . ? C5 Ru C4 C8A -98.2(4) . . . . ? C2 Ru C4 C8A 160.0(3) . . . . ? C6 Ru C4 C8A -126.7(3) . . . . ? C1 Ru C4 C8A -163.9(3) . . . . ? C3 C4 C5 C6 1.1(3) . . . . ? C8B C4 C5 C6 -175.3(3) . . . . ? C8A C4 C5 C6 -178.8(2) . . . . ? Ru C4 C5 C6 54.3(2) . . . . ? C3 C4 C5 Ru -53.24(19) . . . . ? C8B C4 C5 Ru 130.4(4) . . . . ? C8A C4 C5 Ru 126.9(2) . . . . ? O1 Ru C5 C6 121.66(15) . . . . ? N1 Ru C5 C6 -164.91(13) . . . . ? N2 Ru C5 C6 40.66(18) . . . . ? C3 Ru C5 C6 -103.33(17) . . . . ? C2 Ru C5 C6 -65.97(16) . . . . ? C4 Ru C5 C6 -133.2(2) . . . . ? C1 Ru C5 C6 -29.48(14) . . . . ? O1 Ru C5 C4 -105.09(15) . . . . ? N1 Ru C5 C4 -31.7(2) . . . . ? N2 Ru C5 C4 173.91(13) . . . . ? C3 Ru C5 C4 29.91(16) . . . . ? C2 Ru C5 C4 67.28(16) . . . . ? C6 Ru C5 C4 133.2(2) . . . . ? C1 Ru C5 C4 103.76(17) . . . . ? C4 C5 C6 C1 0.3(3) . . . . ? Ru C5 C6 C1 54.67(19) . . . . ? C4 C5 C6 Ru -54.4(2) . . . . ? C2 C1 C6 C5 -0.9(3) . . . . ? C7 C1 C6 C5 -179.3(2) . . . . ? Ru C1 C6 C5 -54.08(19) . . . . ? C2 C1 C6 Ru 53.14(19) . . . . ? C7 C1 C6 Ru -125.3(2) . . . . ? O1 Ru C6 C5 -64.24(16) . . . . ? N1 Ru C6 C5 91.1(5) . . . . ? N2 Ru C6 C5 -149.79(14) . . . . ? C3 Ru C6 C5 65.76(16) . . . . ? C2 Ru C6 C5 103.08(17) . . . . ? C4 Ru C6 C5 28.73(15) . . . . ? C1 Ru C6 C5 132.0(2) . . . . ? O1 Ru C6 C1 163.72(13) . . . . ? N1 Ru C6 C1 -40.9(6) . . . . ? N2 Ru C6 C1 78.17(15) . . . . ? C3 Ru C6 C1 -66.29(16) . . . . ? C5 Ru C6 C1 -132.0(2) . . . . ? C2 Ru C6 C1 -28.96(15) . . . . ? C4 Ru C6 C1 -103.31(17) . . . . ? C3 C4 C8A C9A 40.9(6) . . . . ? C5 C4 C8A C9A -139.3(4) . . . . ? C8B C4 C8A C9A 46.1(6) . . . . ? Ru C4 C8A C9A -59.7(5) . . . . ? C3 C4 C8A C10A -80.0(5) . . . . ? C5 C4 C8A C10A 99.8(4) . . . . ? C8B C4 C8A C10A -74.9(7) . . . . ? Ru C4 C8A C10A 179.4(4) . . . . ? C3 C4 C8B C9B 141.7(4) . . . . ? C5 C4 C8B C9B -41.7(6) . . . . ? C8A C4 C8B C9B -34.4(5) . . . . ? Ru C4 C8B C9B 64.2(6) . . . . ? C3 C4 C8B C10B -97.9(5) . . . . ? C5 C4 C8B C10B 78.7(6) . . . . ? C8A C4 C8B C10B 86.0(7) . . . . ? Ru C4 C8B C10B -175.4(4) . . . . ? N1 Ru O1 C18 2.82(13) . . . . ? N2 Ru O1 C18 -83.53(14) . . . . ? C3 Ru O1 C18 86.05(17) . . . . ? C5 Ru O1 C18 145.80(15) . . . . ? C2 Ru O1 C18 108.3(4) . . . . ? C6 Ru O1 C18 178.91(14) . . . . ? C4 Ru O1 C18 108.98(15) . . . . ? C1 Ru O1 C18 -163.84(15) . . . . ? O1 Ru N1 C11 178.88(19) . . . . ? N2 Ru N1 C11 -97.59(18) . . . . ? C3 Ru N1 C11 47.5(2) . . . . ? C5 Ru N1 C11 101.7(2) . . . . ? C2 Ru N1 C11 11.2(2) . . . . ? C6 Ru N1 C11 22.5(6) . . . . ? C4 Ru N1 C11 82.0(2) . . . . ? C1 Ru N1 C11 -12.0(2) . . . . ? O1 Ru N1 C19 -1.46(13) . . . . ? N2 Ru N1 C19 82.06(14) . . . . ? C3 Ru N1 C19 -132.89(15) . . . . ? C5 Ru N1 C19 -78.67(18) . . . . ? C2 Ru N1 C19 -169.18(14) . . . . ? C6 Ru N1 C19 -157.8(5) . . . . ? C4 Ru N1 C19 -98.35(15) . . . . ? C1 Ru N1 C19 167.66(13) . . . . ? C19 N1 C11 C12 0.8(3) . . . . ? Ru N1 C11 C12 -179.58(16) . . . . ? N1 C11 C12 C13 -0.6(4) . . . . ? C11 C12 C13 C14 -0.6(4) . . . . ? C12 C13 C14 C15 -178.0(2) . . . . ? C12 C13 C14 C19 1.6(3) . . . . ? C19 C14 C15 C16 0.3(4) . . . . ? C13 C14 C15 C16 179.9(3) . . . . ? C14 C15 C16 C17 0.3(4) . . . . ? C15 C16 C17 C18 -0.2(4) . . . . ? Ru O1 C18 C17 176.83(18) . . . . ? Ru O1 C18 C19 -3.8(2) . . . . ? C16 C17 C18 O1 178.7(2) . . . . ? C16 C17 C18 C19 -0.7(3) . . . . ? C11 N1 C19 C14 0.3(3) . . . . ? Ru N1 C19 C14 -179.41(15) . . . . ? C11 N1 C19 C18 179.68(18) . . . . ? Ru N1 C19 C18 0.0(2) . . . . ? C15 C14 C19 N1 178.1(2) . . . . ? C13 C14 C19 N1 -1.4(3) . . . . ? C15 C14 C19 C18 -1.2(3) . . . . ? C13 C14 C19 C18 179.2(2) . . . . ? O1 C18 C19 N1 2.6(3) . . . . ? C17 C18 C19 N1 -178.02(19) . . . . ? O1 C18 C19 C14 -178.03(18) . . . . ? C17 C18 C19 C14 1.4(3) . . . . ? O1 Ru N2 C20 -31.79(19) . . . . ? N1 Ru N2 C20 -111.7(2) . . . . ? C3 Ru N2 C20 162.0(2) . . . . ? C5 Ru N2 C20 52.8(2) . . . . ? C2 Ru N2 C20 145.5(2) . . . . ? C6 Ru N2 C20 76.5(2) . . . . ? C4 Ru N2 C20 70.2(5) . . . . ? C1 Ru N2 C20 113.3(2) . . . . ? O1 Ru N2 N3 156.37(17) . . . . ? N1 Ru N2 N3 76.50(17) . . . . ? C3 Ru N2 N3 -9.9(2) . . . . ? C5 Ru N2 N3 -119.01(17) . . . . ? C2 Ru N2 N3 -26.31(19) . . . . ? C6 Ru N2 N3 -95.39(17) . . . . ? C4 Ru N2 N3 -101.7(4) . . . . ? C1 Ru N2 N3 -58.50(17) . . . . ? C20 N2 N3 C22 0.0(2) . . . . ? Ru N2 N3 C22 173.46(15) . . . . ? N3 N2 C20 C21 -0.2(3) . . . . ? Ru N2 C20 C21 -173.19(16) . . . . ? N2 C20 C21 C22 0.3(3) . . . . ? N2 N3 C22 C21 0.2(3) . . . . ? C20 C21 C22 N3 -0.3(3) . . . . ? O3 S C23 F3 61.2(3) . . . . ? O4 S C23 F3 -177.3(3) . . . . ? O2 S C23 F3 -57.8(3) . . . . ? O3 S C23 F2 -177.7(3) . . . . ? O4 S C23 F2 -56.1(3) . . . . ? O2 S C23 F2 63.3(3) . . . . ? O3 S C23 F1 -59.0(3) . . . . ? O4 S C23 F1 62.5(3) . . . . ? O2 S C23 F1 -178.1(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 N3 H3N O2 0.87 1.97 2.841(3) 178.1 . C24 H24 O3 0.99 2.12 3.090(5) 167.1 . _diffrn_measured_fraction_theta_max 0.969 _diffrn_reflns_theta_full 29.99 _diffrn_measured_fraction_theta_full 0.969 _refine_diff_density_max 1.341 _refine_diff_density_min -1.183 _refine_diff_density_rms 0.077 #===END #============================ End of Crystallographic Information File