Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Mike Ward' _publ_contact_author_address ; Department of Chemistry University of Sheffield Dainton Building Sheffield S3 7HF UNITED KINGDOM ; _publ_contact_author_email M.D.WARD@SHEFFIELD.AC.UK _publ_section_title ; New members of the [Ru(diimine)(CN)4]2- family: structural, electrochemical and photophysical properties ; loop_ _publ_author_name 'Mike Ward' 'Harry Adams' 'Wassim Alsindi' 'Graham M. Davies' 'Martin B. Duriska' 'Timothy L. Easun' ; H.E.Fenton ; 'M. George' 'Juan-Manuel Herrera' 'Kate L. Ronayne' 'Xue-Zhong Sun' 'Michael Towrie' data_imw105m _database_code_depnum_ccdc_archive 'CCDC 276244' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H16 K2 N6 O4 Ru' _chemical_formula_weight 535.62 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' K K 0.2009 0.2494 '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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M Cc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 10.2914(16) _cell_length_b 30.116(5) _cell_length_c 6.6628(11) _cell_angle_alpha 90.00 _cell_angle_beta 101.862(3) _cell_angle_gamma 90.00 _cell_volume 2020.9(6) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.760 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1072 _exptl_absorpt_coefficient_mu 1.224 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7919 _exptl_absorpt_correction_T_max 0.8874 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker smart1000' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11718 _diffrn_reflns_av_R_equivalents 0.0847 _diffrn_reflns_av_sigmaI/netI 0.1416 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -39 _diffrn_reflns_limit_k_max 39 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 1.35 _diffrn_reflns_theta_max 27.54 _reflns_number_total 4539 _reflns_number_gt 2877 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0473P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.29(8) _refine_ls_number_reflns 4539 _refine_ls_number_parameters 281 _refine_ls_number_restraints 63 _refine_ls_R_factor_all 0.1008 _refine_ls_R_factor_gt 0.0548 _refine_ls_wR_factor_ref 0.1191 _refine_ls_wR_factor_gt 0.1051 _refine_ls_goodness_of_fit_ref 0.903 _refine_ls_restrained_S_all 0.897 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.78851(19) 0.628981(17) 0.8827(3) 0.01659(15) Uani 1 1 d . . . K2 K 0.5967(2) 0.46420(13) 0.6464(3) 0.0269(9) Uani 1 1 d . . . K3 K 0.9678(2) 0.53440(13) 0.6031(3) 0.0263(9) Uani 1 1 d . . . N1 N 0.7268(12) 0.6844(4) 0.6956(17) 0.0208(17) Uani 1 1 d U . . N2 N 0.5138(13) 0.6296(4) 1.031(2) 0.026(4) Uani 1 1 d . . . N3 N 1.0681(14) 0.6262(4) 0.735(2) 0.028(4) Uani 1 1 d . . . N4 N 0.8569(10) 0.6822(4) 1.0838(16) 0.014(2) Uani 1 1 d . . . N5 N 0.6751(11) 0.5541(4) 0.5646(16) 0.024(3) Uani 1 1 d . . . N6 N 0.8874(12) 0.5509(4) 1.1862(17) 0.027(3) Uani 1 1 d . . . C1 C 0.6614(13) 0.6860(5) 0.502(2) 0.0218(17) Uani 1 1 d U . . H1A H 0.6380 0.6593 0.4346 0.026 Uiso 1 1 calc R . . C2 C 0.6254(13) 0.7250(5) 0.392(2) 0.0234(17) Uani 1 1 d U . . H2A H 0.5779 0.7242 0.2577 0.028 Uiso 1 1 calc R . . C3 C 0.6621(12) 0.7644(5) 0.489(2) 0.0233(17) Uani 1 1 d U . . H3B H 0.6416 0.7909 0.4179 0.028 Uiso 1 1 calc R . . C4 C 0.7296(13) 0.7656(5) 0.6926(19) 0.0215(17) Uani 1 1 d U . . C5 C 0.7625(14) 0.7246(5) 0.792(2) 0.0209(17) Uani 1 1 d U . . C6 C 0.8300(11) 0.7233(4) 1.0012(17) 0.013(2) Uani 1 1 d . . . C7 C 0.7685(13) 0.8055(5) 0.8117(18) 0.021(3) Uani 1 1 d . . . H7A H 0.7516 0.8331 0.7489 0.026 Uiso 1 1 calc R . . C8 C 0.8297(14) 0.8035(5) 1.015(2) 0.028(3) Uani 1 1 d . . . H8A H 0.8480 0.8296 1.0897 0.033 Uiso 1 1 calc R . . C9 C 0.8650(12) 0.7626(4) 1.1113(17) 0.021(3) Uani 1 1 d . . . C10 C 0.9334(11) 0.7589(4) 1.3163(17) 0.024(3) Uani 1 1 d . . . H10A H 0.9589 0.7842 1.3947 0.029 Uiso 1 1 calc R . . C11 C 0.9622(13) 0.7171(4) 1.3995(19) 0.028(3) Uani 1 1 d . . . H11A H 1.0079 0.7140 1.5344 0.033 Uiso 1 1 calc R . . C12 C 0.9220(11) 0.6797(4) 1.2788(17) 0.014(2) Uani 1 1 d . . . H12A H 0.9413 0.6518 1.3369 0.017 Uiso 1 1 calc R . . C13 C 0.9657(15) 0.6282(4) 0.785(2) 0.020(4) Uani 1 1 d . . . C14 C 0.6117(15) 0.6299(4) 0.975(2) 0.017(4) Uani 1 1 d . . . C15 C 0.7129(13) 0.5829(5) 0.6788(17) 0.014(3) Uani 1 1 d . . . C16 C 0.8503(14) 0.5798(6) 1.077(2) 0.023(4) Uani 1 1 d . . . O100 O 1.2322(7) 0.5790(2) 0.5010(10) 0.0332(16) Uani 1 1 d D . . H103 H 1.236(8) 0.587(2) 0.380(6) 0.040 Uiso 1 1 d D . . H102 H 1.186(8) 0.598(2) 0.552(10) 0.040 Uiso 1 1 d D . . O101 O 1.1736(8) 0.5112(3) 0.9097(11) 0.038(2) Uani 1 1 d D . . H101 H 1.183(10) 0.531(2) 1.005(10) 0.046 Uiso 1 1 d D . . H100 H 1.207(9) 0.4866(15) 0.960(11) 0.046 Uiso 1 1 d D . . O102 O 1.2682(6) 0.5927(2) 1.0915(10) 0.0314(15) Uani 1 1 d D . . H104 H 1.328(5) 0.611(2) 1.073(13) 0.038 Uiso 1 1 d D . . H105 H 1.195(4) 0.600(3) 1.012(11) 0.038 Uiso 1 1 d D . . O103 O 0.4358(8) 0.5262(3) 0.7646(12) 0.052(3) Uani 1 1 d D . . H107 H 0.4295 0.5498 0.6933 0.063 Uiso 1 1 d RD . . H106 H 0.3593 0.5162 0.7692 0.063 Uiso 1 1 d RD . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.0145(3) 0.0173(3) 0.0168(3) 0.0003(7) 0.00054(19) -0.0003(7) K2 0.0291(18) 0.0249(19) 0.0252(16) -0.0005(14) 0.0023(14) 0.0022(15) K3 0.0231(18) 0.0256(19) 0.0277(17) 0.0012(14) -0.0008(14) 0.0019(14) N1 0.019(3) 0.027(4) 0.018(3) 0.009(3) 0.007(3) 0.004(3) N2 0.011(6) 0.030(9) 0.043(9) 0.004(6) 0.015(6) 0.006(5) N3 0.027(8) 0.030(9) 0.022(7) 0.000(5) -0.002(6) 0.005(6) N4 0.009(4) 0.015(4) 0.017(4) 0.003(3) 0.002(3) 0.000(4) N5 0.023(6) 0.028(7) 0.021(6) -0.002(5) 0.007(5) -0.004(5) N6 0.023(6) 0.019(7) 0.035(7) 0.015(5) -0.004(5) 0.002(5) C1 0.019(3) 0.028(4) 0.019(3) 0.008(3) 0.006(3) 0.005(3) C2 0.019(3) 0.031(4) 0.021(3) 0.011(3) 0.006(3) 0.007(3) C3 0.019(3) 0.031(4) 0.022(3) 0.010(3) 0.008(3) 0.008(3) C4 0.019(3) 0.029(4) 0.020(3) 0.009(3) 0.010(3) 0.006(3) C5 0.019(3) 0.026(4) 0.020(3) 0.008(3) 0.009(3) 0.004(3) C6 0.002(4) 0.017(5) 0.019(5) 0.004(4) 0.001(4) 0.002(4) C7 0.034(8) 0.009(5) 0.027(6) -0.002(4) 0.019(6) 0.003(5) C8 0.018(6) 0.023(7) 0.043(8) -0.008(6) 0.009(5) -0.007(5) C9 0.019(6) 0.020(5) 0.028(7) -0.004(5) 0.012(5) -0.006(4) C10 0.011(5) 0.031(7) 0.032(7) -0.015(5) 0.005(5) -0.007(5) C11 0.021(6) 0.035(7) 0.025(6) -0.010(5) 0.002(5) -0.006(5) C12 0.012(5) 0.016(5) 0.011(4) 0.004(4) -0.004(4) 0.000(4) C13 0.011(8) 0.008(8) 0.034(9) 0.001(6) -0.013(7) 0.003(6) C14 0.021(9) 0.022(9) 0.010(7) 0.002(5) 0.009(6) 0.006(6) C15 0.014(6) 0.023(7) 0.007(6) -0.008(5) 0.001(5) 0.000(5) C16 0.013(7) 0.025(8) 0.037(8) -0.021(6) 0.014(6) -0.012(6) O100 0.035(4) 0.029(4) 0.035(4) 0.002(3) 0.005(3) 0.004(3) O101 0.034(5) 0.034(4) 0.043(5) 0.002(4) 0.000(4) -0.003(4) O102 0.020(4) 0.030(4) 0.042(4) -0.008(3) 0.003(3) 0.001(3) O103 0.036(5) 0.062(6) 0.049(5) -0.027(4) -0.012(4) 0.020(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 C16 1.983(17) . ? Ru1 C15 1.985(12) . ? Ru1 C14 2.036(15) . ? Ru1 C13 2.057(18) . ? Ru1 N1 2.101(11) . ? Ru1 N4 2.115(11) . ? Ru1 K2 4.035(4) 2_565 ? Ru1 K3 4.050(4) . ? K2 O103 2.716(8) . ? K2 O103 2.751(8) 2_564 ? K2 N5 2.791(11) 2_565 ? K2 N5 2.908(13) . ? K2 N6 2.983(13) 2_564 ? K2 N2 3.005(13) 2_564 ? K2 C16 3.046(16) 2_564 ? K2 C14 3.073(14) 2_564 ? K2 K2 3.968(4) 2_565 ? K2 K2 3.968(4) 2_564 ? K2 Ru1 4.035(4) 2_564 ? K2 K3 4.367(3) 2_565 ? K3 O101 2.714(8) . ? K3 N6 2.775(11) 1_554 ? K3 N6 2.788(13) 2_564 ? K3 N3 3.017(14) . ? K3 O101 3.025(9) 2_564 ? K3 N5 3.029(12) . ? K3 C13 3.077(14) . ? K3 C15 3.133(15) . ? K3 O100 3.229(7) . ? K3 K3 3.923(4) 2_564 ? K3 K3 3.923(4) 2_565 ? N1 C1 1.329(17) . ? N1 C5 1.384(17) . ? N2 C14 1.144(19) . ? N2 K2 3.005(13) 2_565 ? N3 C13 1.17(2) . ? N4 C12 1.336(14) . ? N4 C6 1.359(14) . ? N5 C15 1.167(16) . ? N5 K2 2.791(11) 2_564 ? N6 C16 1.150(19) . ? N6 K3 2.775(11) 1_556 ? N6 K3 2.788(13) 2_565 ? N6 K2 2.983(13) 2_565 ? C1 C2 1.390(18) . ? C2 C3 1.367(18) . ? C3 C4 1.390(16) . ? C4 C5 1.410(19) . ? C4 C7 1.451(18) . ? C5 C6 1.424(10) . ? C6 C9 1.400(17) . ? C7 C8 1.372(13) . ? C8 C9 1.402(19) . ? C9 C10 1.407(14) . ? C10 C11 1.381(15) . ? C11 C12 1.398(16) . ? C14 K2 3.073(14) 2_565 ? C16 K2 3.046(16) 2_565 ? O101 K3 3.025(9) 2_565 ? O103 K2 2.751(8) 2_565 ? 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 C16 Ru1 C15 87.3(3) . . ? C16 Ru1 C14 90.1(6) . . ? C15 Ru1 C14 88.1(6) . . ? C16 Ru1 C13 90.6(6) . . ? C15 Ru1 C13 91.4(6) . . ? C14 Ru1 C13 179.1(8) . . ? C16 Ru1 N1 175.7(6) . . ? C15 Ru1 N1 96.9(5) . . ? C14 Ru1 N1 89.3(5) . . ? C13 Ru1 N1 90.1(5) . . ? C16 Ru1 N4 97.6(5) . . ? C15 Ru1 N4 174.8(5) . . ? C14 Ru1 N4 90.0(5) . . ? C13 Ru1 N4 90.4(5) . . ? N1 Ru1 N4 78.2(2) . . ? C16 Ru1 K2 46.9(4) . 2_565 ? C15 Ru1 K2 69.8(4) . 2_565 ? C14 Ru1 K2 48.0(4) . 2_565 ? C13 Ru1 K2 132.4(4) . 2_565 ? N1 Ru1 K2 134.0(3) . 2_565 ? N4 Ru1 K2 112.3(3) . 2_565 ? C16 Ru1 K3 70.1(4) . . ? C15 Ru1 K3 49.1(4) . . ? C14 Ru1 K3 131.9(4) . . ? C13 Ru1 K3 47.9(4) . . ? N1 Ru1 K3 113.3(3) . . ? N4 Ru1 K3 134.5(3) . . ? K2 Ru1 K3 91.22(3) 2_565 . ? O103 K2 O103 84.8(2) . 2_564 ? O103 K2 N5 85.1(3) . 2_565 ? O103 K2 N5 160.0(3) 2_564 2_565 ? O103 K2 N5 67.9(3) . . ? O103 K2 N5 82.3(3) 2_564 . ? N5 K2 N5 109.7(4) 2_565 . ? O103 K2 N6 137.6(3) . 2_564 ? O103 K2 N6 120.0(3) 2_564 2_564 ? N5 K2 N6 78.6(3) 2_565 2_564 ? N5 K2 N6 81.2(3) . 2_564 ? O103 K2 N2 124.2(4) . 2_564 ? O103 K2 N2 77.1(3) 2_564 2_564 ? N5 K2 N2 94.6(4) 2_565 2_564 ? N5 K2 N2 154.4(4) . 2_564 ? N6 K2 N2 96.1(4) 2_564 2_564 ? O103 K2 C16 159.3(4) . 2_564 ? O103 K2 C16 106.1(3) 2_564 2_564 ? N5 K2 C16 89.2(4) 2_565 2_564 ? N5 K2 C16 95.6(4) . 2_564 ? N6 K2 C16 22.0(3) 2_564 2_564 ? N2 K2 C16 76.1(4) 2_564 2_564 ? O103 K2 C14 145.3(4) . 2_564 ? O103 K2 C14 79.6(3) 2_564 2_564 ? N5 K2 C14 99.4(4) 2_565 2_564 ? N5 K2 C14 138.7(4) . 2_564 ? N6 K2 C14 76.5(4) 2_564 2_564 ? N2 K2 C14 21.7(4) 2_564 2_564 ? C16 K2 C14 55.4(4) 2_564 2_564 ? O103 K2 K2 43.80(18) . 2_565 ? O103 K2 K2 128.0(2) 2_564 2_565 ? N5 K2 K2 47.1(3) 2_565 2_565 ? N5 K2 K2 72.5(2) . 2_565 ? N6 K2 K2 100.4(2) 2_564 2_565 ? N2 K2 K2 132.6(3) 2_564 2_565 ? C16 K2 K2 120.8(3) 2_564 2_565 ? C14 K2 K2 145.4(3) 2_564 2_565 ? O103 K2 K2 88.6(2) . 2_564 ? O103 K2 K2 43.12(16) 2_564 2_564 ? N5 K2 K2 153.5(3) 2_565 2_564 ? N5 K2 K2 44.7(2) . 2_564 ? N6 K2 K2 89.1(2) 2_564 2_564 ? N2 K2 K2 110.1(3) 2_564 2_564 ? C16 K2 K2 87.8(3) 2_564 2_564 ? C14 K2 K2 100.4(3) 2_564 2_564 ? K2 K2 K2 114.17(19) 2_565 2_564 ? O103 K2 Ru1 170.31(19) . 2_564 ? O103 K2 Ru1 85.7(2) 2_564 2_564 ? N5 K2 Ru1 103.3(3) 2_565 2_564 ? N5 K2 Ru1 112.7(3) . 2_564 ? N6 K2 Ru1 50.3(2) 2_564 2_564 ? N2 K2 Ru1 51.2(3) 2_564 2_564 ? C16 K2 Ru1 28.4(3) 2_564 2_564 ? C14 K2 Ru1 29.5(3) 2_564 2_564 ? K2 K2 Ru1 145.87(7) 2_565 2_564 ? K2 K2 Ru1 85.87(6) 2_564 2_564 ? O103 K2 K3 106.82(19) . 2_565 ? O103 K2 K3 156.53(18) 2_564 2_565 ? N5 K2 K3 43.5(3) 2_565 2_565 ? N5 K2 K3 83.4(2) . 2_565 ? N6 K2 K3 38.9(2) 2_564 2_565 ? N2 K2 K3 110.5(3) 2_564 2_565 ? C16 K2 K3 57.1(3) 2_564 2_565 ? C14 K2 K3 99.5(3) 2_564 2_565 ? K2 K2 K3 63.95(4) 2_565 2_565 ? K2 K2 K3 115.38(9) 2_564 2_565 ? Ru1 K2 K3 82.76(8) 2_564 2_565 ? O101 K3 N6 145.6(3) . 1_554 ? O101 K3 N6 80.3(3) . 2_564 ? N6 K3 N6 108.9(4) 1_554 2_564 ? O101 K3 N3 81.3(3) . . ? N6 K3 N3 98.1(4) 1_554 . ? N6 K3 N3 152.1(4) 2_564 . ? O101 K3 O101 72.42(19) . 2_564 ? N6 K3 O101 75.3(3) 1_554 2_564 ? N6 K3 O101 85.9(3) 2_564 2_564 ? N3 K3 O101 108.2(4) . 2_564 ? O101 K3 N5 136.3(3) . . ? N6 K3 N5 78.1(3) 1_554 . ? N6 K3 N5 82.3(3) 2_564 . ? N3 K3 N5 96.9(4) . . ? O101 K3 N5 145.5(3) 2_564 . ? O101 K3 C13 90.4(3) . . ? N6 K3 C13 101.9(4) 1_554 . ? N6 K3 C13 137.8(4) 2_564 . ? N3 K3 C13 22.2(4) . . ? O101 K3 C13 130.4(4) 2_564 . ? N5 K3 C13 76.5(4) . . ? O101 K3 C15 123.2(3) . . ? N6 K3 C15 89.4(4) 1_554 . ? N6 K3 C15 96.0(4) 2_564 . ? N3 K3 C15 76.9(4) . . ? O101 K3 C15 164.3(3) 2_564 . ? N5 K3 C15 21.8(3) . . ? C13 K3 C15 55.5(4) . . ? O101 K3 O100 72.8(2) . . ? N6 K3 O100 78.8(3) 1_554 . ? N6 K3 O100 136.3(3) 2_564 . ? N3 K3 O100 55.1(3) . . ? O101 K3 O100 53.55(19) 2_564 . ? N5 K3 O100 140.1(3) . . ? C13 K3 O100 77.0(3) . . ? C15 K3 O100 127.6(3) . . ? O101 K3 K3 111.6(2) . 2_564 ? N6 K3 K3 45.3(3) 1_554 2_564 ? N6 K3 K3 74.6(3) 2_564 2_564 ? N3 K3 K3 132.2(3) . 2_564 ? O101 K3 K3 43.64(15) 2_564 2_564 ? N5 K3 K3 101.8(2) . 2_564 ? C13 K3 K3 145.2(3) . 2_564 ? C15 K3 K3 122.0(2) . 2_564 ? O100 K3 K3 83.91(12) . 2_564 ? O101 K3 K3 50.30(19) . 2_565 ? N6 K3 K3 153.1(3) 1_554 2_565 ? N6 K3 K3 45.0(2) 2_564 2_565 ? N3 K3 K3 107.3(3) . 2_565 ? O101 K3 K3 104.11(18) 2_564 2_565 ? N5 K3 K3 90.1(2) . 2_565 ? C13 K3 K3 98.5(3) . 2_565 ? C15 K3 K3 87.9(3) . 2_565 ? O100 K3 K3 123.06(12) . 2_565 ? K3 K3 K3 116.24(19) 2_564 2_565 ? O101 K3 Ru1 101.14(18) . . ? N6 K3 Ru1 105.3(3) 1_554 . ? N6 K3 Ru1 112.0(3) 2_564 . ? N3 K3 Ru1 51.9(3) . . ? O101 K3 Ru1 160.11(18) 2_564 . ? N5 K3 Ru1 50.4(2) . . ? C13 K3 Ru1 29.7(3) . . ? C15 K3 Ru1 28.6(2) . . ? O100 K3 Ru1 106.71(14) . . ? K3 K3 Ru1 147.31(7) 2_564 . ? K3 K3 Ru1 84.33(7) 2_565 . ? C1 N1 C5 116.8(11) . . ? C1 N1 Ru1 129.6(10) . . ? C5 N1 Ru1 113.6(9) . . ? C14 N2 K2 82.5(9) . 2_565 ? C13 N3 K3 81.8(10) . . ? C12 N4 C6 117.8(10) . . ? C12 N4 Ru1 127.4(8) . . ? C6 N4 Ru1 114.8(8) . . ? C15 N5 K2 141.9(11) . 2_564 ? C15 N5 K2 129.6(10) . . ? K2 N5 K2 88.2(3) 2_564 . ? C15 N5 K3 84.1(9) . . ? K2 N5 K3 97.1(4) 2_564 . ? K2 N5 K3 96.4(4) . . ? C16 N6 K3 139.6(12) . 1_556 ? C16 N6 K3 130.2(11) . 2_565 ? K3 N6 K3 89.7(3) 1_556 2_565 ? C16 N6 K2 82.1(10) . 2_565 ? K3 N6 K2 98.6(4) 1_556 2_565 ? K3 N6 K2 100.1(4) 2_565 2_565 ? N1 C1 C2 124.6(13) . . ? C3 C2 C1 117.9(14) . . ? C2 C3 C4 121.1(14) . . ? C3 C4 C5 117.3(14) . . ? C3 C4 C7 125.5(14) . . ? C5 C4 C7 117.2(12) . . ? N1 C5 C4 122.3(12) . . ? N1 C5 C6 117.4(15) . . ? C4 C5 C6 120.3(16) . . ? N4 C6 C9 123.2(10) . . ? N4 C6 C5 116.0(15) . . ? C9 C6 C5 120.7(15) . . ? C8 C7 C4 121.4(16) . . ? C7 C8 C9 121.0(16) . . ? C6 C9 C8 119.2(10) . . ? C6 C9 C10 117.7(11) . . ? C8 C9 C10 123.1(12) . . ? C11 C10 C9 119.1(12) . . ? C10 C11 C12 119.3(11) . . ? N4 C12 C11 122.9(10) . . ? N3 C13 Ru1 177.1(13) . . ? N3 C13 K3 76.0(10) . . ? Ru1 C13 K3 102.3(5) . . ? N2 C14 Ru1 178.0(13) . . ? N2 C14 K2 75.8(9) . 2_565 ? Ru1 C14 K2 102.4(5) . 2_565 ? N5 C15 Ru1 175.7(13) . . ? N5 C15 K3 74.1(9) . . ? Ru1 C15 K3 102.3(5) . . ? N6 C16 Ru1 178.5(14) . . ? N6 C16 K2 75.9(10) . 2_565 ? Ru1 C16 K2 104.7(6) . 2_565 ? K3 O101 K3 86.1(2) . 2_565 ? K2 O103 K2 93.1(2) . 2_565 ? 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 C16 Ru1 K3 O101 -39.4(5) . . . . ? C15 Ru1 K3 O101 -143.7(6) . . . . ? C14 Ru1 K3 O101 -110.5(5) . . . . ? C13 Ru1 K3 O101 70.7(6) . . . . ? N1 Ru1 K3 O101 137.9(4) . . . . ? N4 Ru1 K3 O101 41.5(4) . . . . ? K2 Ru1 K3 O101 -82.1(2) 2_565 . . . ? C16 Ru1 K3 N6 162.7(5) . . . 1_554 ? C15 Ru1 K3 N6 58.5(6) . . . 1_554 ? C14 Ru1 K3 N6 91.6(6) . . . 1_554 ? C13 Ru1 K3 N6 -87.2(6) . . . 1_554 ? N1 Ru1 K3 N6 -20.0(5) . . . 1_554 ? N4 Ru1 K3 N6 -116.4(5) . . . 1_554 ? K2 Ru1 K3 N6 120.0(3) 2_565 . . 1_554 ? C16 Ru1 K3 N6 44.6(5) . . . 2_564 ? C15 Ru1 K3 N6 -59.7(6) . . . 2_564 ? C14 Ru1 K3 N6 -26.5(6) . . . 2_564 ? C13 Ru1 K3 N6 154.6(6) . . . 2_564 ? N1 Ru1 K3 N6 -138.2(4) . . . 2_564 ? N4 Ru1 K3 N6 125.4(5) . . . 2_564 ? K2 Ru1 K3 N6 1.8(3) 2_565 . . 2_564 ? C16 Ru1 K3 N3 -108.9(5) . . . . ? C15 Ru1 K3 N3 146.8(6) . . . . ? C14 Ru1 K3 N3 180.0(6) . . . . ? C13 Ru1 K3 N3 1.2(6) . . . . ? N1 Ru1 K3 N3 68.3(5) . . . . ? N4 Ru1 K3 N3 -28.0(5) . . . . ? K2 Ru1 K3 N3 -151.6(3) 2_565 . . . ? C16 Ru1 K3 O101 -108.2(6) . . . 2_564 ? C15 Ru1 K3 O101 147.5(7) . . . 2_564 ? C14 Ru1 K3 O101 -179.3(7) . . . 2_564 ? C13 Ru1 K3 O101 1.9(7) . . . 2_564 ? N1 Ru1 K3 O101 69.0(6) . . . 2_564 ? N4 Ru1 K3 O101 -27.3(6) . . . 2_564 ? K2 Ru1 K3 O101 -150.9(5) 2_565 . . 2_564 ? C16 Ru1 K3 N5 103.1(5) . . . . ? C15 Ru1 K3 N5 -1.2(6) . . . . ? C14 Ru1 K3 N5 32.0(6) . . . . ? C13 Ru1 K3 N5 -146.8(6) . . . . ? N1 Ru1 K3 N5 -79.7(4) . . . . ? N4 Ru1 K3 N5 -176.0(4) . . . . ? K2 Ru1 K3 N5 60.4(3) 2_565 . . . ? C16 Ru1 K3 C13 -110.1(7) . . . . ? C15 Ru1 K3 C13 145.6(8) . . . . ? C14 Ru1 K3 C13 178.8(10) . . . . ? N1 Ru1 K3 C13 67.2(6) . . . . ? N4 Ru1 K3 C13 -29.2(7) . . . . ? K2 Ru1 K3 C13 -152.8(5) 2_565 . . . ? C16 Ru1 K3 C15 104.3(6) . . . . ? C14 Ru1 K3 C15 33.2(8) . . . . ? C13 Ru1 K3 C15 -145.6(8) . . . . ? N1 Ru1 K3 C15 -78.5(7) . . . . ? N4 Ru1 K3 C15 -174.8(7) . . . . ? K2 Ru1 K3 C15 61.6(5) 2_565 . . . ? C16 Ru1 K3 O100 -114.6(4) . . . . ? C15 Ru1 K3 O100 141.1(6) . . . . ? C14 Ru1 K3 O100 174.3(5) . . . . ? C13 Ru1 K3 O100 -4.5(6) . . . . ? N1 Ru1 K3 O100 62.6(4) . . . . ? N4 Ru1 K3 O100 -33.7(4) . . . . ? K2 Ru1 K3 O100 -157.32(13) 2_565 . . . ? C16 Ru1 K3 K3 140.2(5) . . . 2_564 ? C15 Ru1 K3 K3 35.9(5) . . . 2_564 ? C14 Ru1 K3 K3 69.1(6) . . . 2_564 ? C13 Ru1 K3 K3 -109.7(6) . . . 2_564 ? N1 Ru1 K3 K3 -42.6(4) . . . 2_564 ? N4 Ru1 K3 K3 -138.9(4) . . . 2_564 ? K2 Ru1 K3 K3 97.5(2) 2_565 . . 2_564 ? C16 Ru1 K3 K3 8.3(4) . . . 2_565 ? C15 Ru1 K3 K3 -96.0(5) . . . 2_565 ? C14 Ru1 K3 K3 -62.8(5) . . . 2_565 ? C13 Ru1 K3 K3 118.3(5) . . . 2_565 ? N1 Ru1 K3 K3 -174.5(4) . . . 2_565 ? N4 Ru1 K3 K3 89.2(4) . . . 2_565 ? K2 Ru1 K3 K3 -34.46(6) 2_565 . . 2_565 ? C16 Ru1 N1 C1 -171(7) . . . . ? C15 Ru1 N1 C1 -1.5(13) . . . . ? C14 Ru1 N1 C1 -89.5(13) . . . . ? C13 Ru1 N1 C1 89.9(13) . . . . ? N4 Ru1 N1 C1 -179.7(11) . . . . ? K2 Ru1 N1 C1 -70.0(13) 2_565 . . . ? K3 Ru1 N1 C1 46.7(13) . . . . ? C16 Ru1 N1 C5 10(8) . . . . ? C15 Ru1 N1 C5 179.3(10) . . . . ? C14 Ru1 N1 C5 91.3(11) . . . . ? C13 Ru1 N1 C5 -89.3(11) . . . . ? N4 Ru1 N1 C5 1.1(12) . . . . ? K2 Ru1 N1 C5 110.9(10) 2_565 . . . ? K3 Ru1 N1 C5 -132.4(9) . . . . ? O101 K3 N3 C13 -113.1(10) . . . . ? N6 K3 N3 C13 101.6(10) 1_554 . . . ? N6 K3 N3 C13 -63.8(13) 2_564 . . . ? O101 K3 N3 C13 178.7(9) 2_564 . . . ? N5 K3 N3 C13 22.7(10) . . . . ? C15 K3 N3 C13 14.1(10) . . . . ? O100 K3 N3 C13 171.8(11) . . . . ? K3 K3 N3 C13 135.6(9) 2_564 . . . ? K3 K3 N3 C13 -69.5(10) 2_565 . . . ? Ru1 K3 N3 C13 -1.5(9) . . . . ? C16 Ru1 N4 C12 0.5(12) . . . . ? C15 Ru1 N4 C12 160(6) . . . . ? C14 Ru1 N4 C12 90.6(11) . . . . ? C13 Ru1 N4 C12 -90.2(11) . . . . ? N1 Ru1 N4 C12 179.8(9) . . . . ? K2 Ru1 N4 C12 46.8(11) 2_565 . . . ? K3 Ru1 N4 C12 -69.0(12) . . . . ? C16 Ru1 N4 C6 -179.3(9) . . . . ? C15 Ru1 N4 C6 -20(6) . . . . ? C14 Ru1 N4 C6 -89.3(10) . . . . ? C13 Ru1 N4 C6 90.0(10) . . . . ? N1 Ru1 N4 C6 0.0(11) . . . . ? K2 Ru1 N4 C6 -133.0(8) 2_565 . . . ? K3 Ru1 N4 C6 111.2(8) . . . . ? O103 K2 N5 C15 63.5(13) . . . . ? O103 K2 N5 C15 150.9(13) 2_564 . . . ? N5 K2 N5 C15 -12.5(15) 2_565 . . . ? N6 K2 N5 C15 -86.9(13) 2_564 . . . ? N2 K2 N5 C15 -172.6(12) 2_564 . . . ? C16 K2 N5 C15 -103.6(13) 2_564 . . . ? C14 K2 N5 C15 -144.6(12) 2_564 . . . ? K2 K2 N5 C15 17.0(12) 2_565 . . . ? K2 K2 N5 C15 175.3(15) 2_564 . . . ? Ru1 K2 N5 C15 -127.0(13) 2_564 . . . ? K3 K2 N5 C15 -47.7(13) 2_565 . . . ? O103 K2 N5 K2 -111.9(3) . . . 2_564 ? O103 K2 N5 K2 -24.4(3) 2_564 . . 2_564 ? N5 K2 N5 K2 172.19(19) 2_565 . . 2_564 ? N6 K2 N5 K2 97.7(3) 2_564 . . 2_564 ? N2 K2 N5 K2 12.0(10) 2_564 . . 2_564 ? C16 K2 N5 K2 81.1(4) 2_564 . . 2_564 ? C14 K2 N5 K2 40.1(6) 2_564 . . 2_564 ? K2 K2 N5 K2 -158.3(3) 2_565 . . 2_564 ? Ru1 K2 N5 K2 57.7(3) 2_564 . . 2_564 ? K3 K2 N5 K2 137.0(3) 2_565 . . 2_564 ? O103 K2 N5 K3 151.2(3) . . . . ? O103 K2 N5 K3 -121.4(3) 2_564 . . . ? N5 K2 N5 K3 75.2(4) 2_565 . . . ? N6 K2 N5 K3 0.7(4) 2_564 . . . ? N2 K2 N5 K3 -85.0(9) 2_564 . . . ? C16 K2 N5 K3 -15.9(4) 2_564 . . . ? C14 K2 N5 K3 -56.9(6) 2_564 . . . ? K2 K2 N5 K3 104.7(3) 2_565 . . . ? K2 K2 N5 K3 -97.0(4) 2_564 . . . ? Ru1 K2 N5 K3 -39.3(3) 2_564 . . . ? K3 K2 N5 K3 40.0(2) 2_565 . . . ? O101 K3 N5 C15 61.3(10) . . . . ? N6 K3 N5 C15 -120.2(10) 1_554 . . . ? N6 K3 N5 C15 128.5(9) 2_564 . . . ? N3 K3 N5 C15 -23.3(9) . . . . ? O101 K3 N5 C15 -160.3(8) 2_564 . . . ? C13 K3 N5 C15 -14.7(9) . . . . ? O100 K3 N5 C15 -64.4(10) . . . . ? K3 K3 N5 C15 -159.1(9) 2_564 . . . ? K3 K3 N5 C15 84.1(9) 2_565 . . . ? Ru1 K3 N5 C15 1.5(8) . . . . ? O101 K3 N5 K2 -157.0(4) . . . 2_564 ? N6 K3 N5 K2 21.4(2) 1_554 . . 2_564 ? N6 K3 N5 K2 -89.8(4) 2_564 . . 2_564 ? N3 K3 N5 K2 118.3(4) . . . 2_564 ? O101 K3 N5 K2 -18.6(7) 2_564 . . 2_564 ? C13 K3 N5 K2 127.0(5) . . . 2_564 ? C15 K3 N5 K2 141.7(11) . . . 2_564 ? O100 K3 N5 K2 77.3(5) . . . 2_564 ? K3 K3 N5 K2 -17.4(3) 2_564 . . 2_564 ? K3 K3 N5 K2 -134.3(3) 2_565 . . 2_564 ? Ru1 K3 N5 K2 143.2(5) . . . 2_564 ? O101 K3 N5 K2 -68.0(5) . . . . ? N6 K3 N5 K2 110.5(4) 1_554 . . . ? N6 K3 N5 K2 -0.8(4) 2_564 . . . ? N3 K3 N5 K2 -152.7(4) . . . . ? O101 K3 N5 K2 70.4(6) 2_564 . . . ? C13 K3 N5 K2 -144.0(4) . . . . ? C15 K3 N5 K2 -129.3(10) . . . . ? O100 K3 N5 K2 166.3(2) . . . . ? K3 K3 N5 K2 71.6(3) 2_564 . . . ? K3 K3 N5 K2 -45.3(3) 2_565 . . . ? Ru1 K3 N5 K2 -127.8(4) . . . . ? C5 N1 C1 C2 -1(2) . . . . ? Ru1 N1 C1 C2 179.9(11) . . . . ? N1 C1 C2 C3 1(2) . . . . ? C1 C2 C3 C4 -2(2) . . . . ? C2 C3 C4 C5 2(2) . . . . ? C2 C3 C4 C7 -177.5(13) . . . . ? C1 N1 C5 C4 1(2) . . . . ? Ru1 N1 C5 C4 -179.6(11) . . . . ? C1 N1 C5 C6 178.6(9) . . . . ? Ru1 N1 C5 C6 -2.2(12) . . . . ? C3 C4 C5 N1 -2(2) . . . . ? C7 C4 C5 N1 178.0(13) . . . . ? C3 C4 C5 C6 -179.1(9) . . . . ? C7 C4 C5 C6 0.6(16) . . . . ? C12 N4 C6 C9 -1.1(19) . . . . ? Ru1 N4 C6 C9 178.8(10) . . . . ? C12 N4 C6 C5 179.0(9) . . . . ? Ru1 N4 C6 C5 -1.2(10) . . . . ? N1 C5 C6 N4 2.2(8) . . . . ? C4 C5 C6 N4 179.7(15) . . . . ? N1 C5 C6 C9 -177.7(15) . . . . ? C4 C5 C6 C9 -0.2(9) . . . . ? C3 C4 C7 C8 177.0(12) . . . . ? C5 C4 C7 C8 -2.7(17) . . . . ? C4 C7 C8 C9 4.4(13) . . . . ? N4 C6 C9 C8 -178.2(13) . . . . ? C5 C6 C9 C8 1.7(16) . . . . ? N4 C6 C9 C10 1.1(19) . . . . ? C5 C6 C9 C10 -179.0(9) . . . . ? C7 C8 C9 C6 -3.9(18) . . . . ? C7 C8 C9 C10 176.9(10) . . . . ? C6 C9 C10 C11 -0.3(18) . . . . ? C8 C9 C10 C11 179.0(13) . . . . ? C9 C10 C11 C12 -0.5(19) . . . . ? C6 N4 C12 C11 0.3(19) . . . . ? Ru1 N4 C12 C11 -179.6(10) . . . . ? C10 C11 C12 N4 1(2) . . . . ? K3 N3 C13 Ru1 56(28) . . . . ? C16 Ru1 C13 N3 7(28) . . . . ? C15 Ru1 C13 N3 -81(28) . . . . ? C14 Ru1 C13 N3 -136(24) . . . . ? N1 Ru1 C13 N3 -178(100) . . . . ? N4 Ru1 C13 N3 104(28) . . . . ? K2 Ru1 C13 N3 -17(28) 2_565 . . . ? K3 Ru1 C13 N3 -55(27) . . . . ? C16 Ru1 C13 K3 62.0(5) . . . . ? C15 Ru1 C13 K3 -25.3(5) . . . . ? C14 Ru1 C13 K3 -80(19) . . . . ? N1 Ru1 C13 K3 -122.2(5) . . . . ? N4 Ru1 C13 K3 159.6(4) . . . . ? K2 Ru1 C13 K3 38.2(7) 2_565 . . . ? O101 K3 C13 N3 65.4(10) . . . . ? N6 K3 C13 N3 -82.3(10) 1_554 . . . ? N6 K3 C13 N3 141.3(10) 2_564 . . . ? O101 K3 C13 N3 -1.6(12) 2_564 . . . ? N5 K3 C13 N3 -156.7(11) . . . . ? C15 K3 C13 N3 -163.3(11) . . . . ? O100 K3 C13 N3 -6.9(9) . . . . ? K3 K3 C13 N3 -65.4(11) 2_564 . . . ? K3 K3 C13 N3 115.2(10) 2_565 . . . ? Ru1 K3 C13 N3 177.6(14) . . . . ? O101 K3 C13 Ru1 -112.2(5) . . . . ? N6 K3 C13 Ru1 100.1(5) 1_554 . . . ? N6 K3 C13 Ru1 -36.3(8) 2_564 . . . ? N3 K3 C13 Ru1 -177.6(14) . . . . ? O101 K3 C13 Ru1 -179.2(3) 2_564 . . . ? N5 K3 C13 Ru1 25.7(4) . . . . ? C15 K3 C13 Ru1 19.1(4) . . . . ? O100 K3 C13 Ru1 175.6(5) . . . . ? K3 K3 C13 Ru1 117.0(6) 2_564 . . . ? K3 K3 C13 Ru1 -62.3(5) 2_565 . . . ? K2 N2 C14 Ru1 -29(42) 2_565 . . . ? C16 Ru1 C14 N2 6(42) . . . . ? C15 Ru1 C14 N2 93(42) . . . . ? C13 Ru1 C14 N2 149(33) . . . . ? N1 Ru1 C14 N2 -170(41) . . . . ? N4 Ru1 C14 N2 -92(41) . . . . ? K2 Ru1 C14 N2 29(41) 2_565 . . . ? K3 Ru1 C14 N2 69(42) . . . . ? C16 Ru1 C14 K2 -23.1(5) . . . 2_565 ? C15 Ru1 C14 K2 64.2(5) . . . 2_565 ? C13 Ru1 C14 K2 119(19) . . . 2_565 ? N1 Ru1 C14 K2 161.1(5) . . . 2_565 ? N4 Ru1 C14 K2 -120.7(4) . . . 2_565 ? K3 Ru1 C14 K2 39.7(7) . . . 2_565 ? K2 N5 C15 Ru1 -128(16) 2_564 . . . ? K2 N5 C15 Ru1 60(17) . . . . ? K3 N5 C15 Ru1 -34(17) . . . . ? K2 N5 C15 K3 -94.1(14) 2_564 . . . ? K2 N5 C15 K3 93.4(10) . . . . ? C16 Ru1 C15 N5 -33(17) . . . . ? C14 Ru1 C15 N5 -123(17) . . . . ? C13 Ru1 C15 N5 58(17) . . . . ? N1 Ru1 C15 N5 148(17) . . . . ? N4 Ru1 C15 N5 168(13) . . . . ? K2 Ru1 C15 N5 -77(17) 2_565 . . . ? K3 Ru1 C15 N5 33(17) . . . . ? C16 Ru1 C15 K3 -65.8(7) . . . . ? C14 Ru1 C15 K3 -156.0(5) . . . . ? C13 Ru1 C15 K3 24.8(5) . . . . ? N1 Ru1 C15 K3 115.0(5) . . . . ? N4 Ru1 C15 K3 135(6) . . . . ? K2 Ru1 C15 K3 -110.4(4) 2_565 . . . ? O101 K3 C15 N5 -133.5(8) . . . . ? N6 K3 C15 N5 57.7(10) 1_554 . . . ? N6 K3 C15 N5 -51.2(8) 2_564 . . . ? N3 K3 C15 N5 156.2(10) . . . . ? O101 K3 C15 N5 45.1(18) 2_564 . . . ? C13 K3 C15 N5 162.6(10) . . . . ? O100 K3 C15 N5 133.1(8) . . . . ? K3 K3 C15 N5 24.4(10) 2_564 . . . ? K3 K3 C15 N5 -95.6(9) 2_565 . . . ? Ru1 K3 C15 N5 -177.6(13) . . . . ? O101 K3 C15 Ru1 44.0(7) . . . . ? N6 K3 C15 Ru1 -124.7(5) 1_554 . . . ? N6 K3 C15 Ru1 126.3(5) 2_564 . . . ? N3 K3 C15 Ru1 -26.3(5) . . . . ? O101 K3 C15 Ru1 -137.4(10) 2_564 . . . ? N5 K3 C15 Ru1 177.6(13) . . . . ? C13 K3 C15 Ru1 -19.9(5) . . . . ? O100 K3 C15 Ru1 -49.3(6) . . . . ? K3 K3 C15 Ru1 -158.1(3) 2_564 . . . ? K3 K3 C15 Ru1 82.0(5) 2_565 . . . ? K3 N6 C16 Ru1 150(55) 1_556 . . . ? K3 N6 C16 Ru1 -19(57) 2_565 . . . ? K2 N6 C16 Ru1 -116(56) 2_565 . . . ? K3 N6 C16 K2 -94.0(15) 1_556 . . 2_565 ? K3 N6 C16 K2 96.6(11) 2_565 . . 2_565 ? C15 Ru1 C16 N6 51(56) . . . . ? C14 Ru1 C16 N6 139(56) . . . . ? C13 Ru1 C16 N6 -40(56) . . . . ? N1 Ru1 C16 N6 -140(52) . . . . ? N4 Ru1 C16 N6 -131(56) . . . . ? K2 Ru1 C16 N6 115(56) 2_565 . . . ? K3 Ru1 C16 N6 4(56) . . . . ? C15 Ru1 C16 K2 -64.5(6) . . . 2_565 ? C14 Ru1 C16 K2 23.6(6) . . . 2_565 ? C13 Ru1 C16 K2 -155.9(6) . . . 2_565 ? N1 Ru1 C16 K2 105(8) . . . 2_565 ? N4 Ru1 C16 K2 113.6(5) . . . 2_565 ? K3 Ru1 C16 K2 -111.7(4) . . . 2_565 ? N6 K3 O101 K3 -147.2(6) 1_554 . . 2_565 ? N6 K3 O101 K3 -37.8(3) 2_564 . . 2_565 ? N3 K3 O101 K3 121.1(4) . . . 2_565 ? O101 K3 O101 K3 -126.6(3) 2_564 . . 2_565 ? N5 K3 O101 K3 30.2(5) . . . 2_565 ? C13 K3 O101 K3 100.8(4) . . . 2_565 ? C15 K3 O101 K3 53.1(4) . . . 2_565 ? O100 K3 O101 K3 177.1(2) . . . 2_565 ? K3 K3 O101 K3 -106.9(2) 2_564 . . 2_565 ? Ru1 K3 O101 K3 72.89(15) . . . 2_565 ? O103 K2 O103 K2 -171.2(3) 2_564 . . 2_565 ? N5 K2 O103 K2 26.1(3) 2_565 . . 2_565 ? N5 K2 O103 K2 -87.4(3) . . . 2_565 ? N6 K2 O103 K2 -41.1(6) 2_564 . . 2_565 ? N2 K2 O103 K2 118.3(4) 2_564 . . 2_565 ? C16 K2 O103 K2 -48.3(10) 2_564 . . 2_565 ? C14 K2 O103 K2 125.6(5) 2_564 . . 2_565 ? K2 K2 O103 K2 -128.2(2) 2_564 . . 2_565 ? Ru1 K2 O103 K2 176.9(13) 2_564 . . 2_565 ? K3 K2 O103 K2 -12.0(3) 2_565 . . 2_565 ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.54 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.021 _refine_diff_density_min -0.983 _refine_diff_density_rms 0.141 #===END data_imw176 _database_code_depnum_ccdc_archive 'CCDC 276245' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H12 K2 N8 O3 Ru' _chemical_formula_weight 495.57 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' K K 0.2009 0.2494 '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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 6.5658(7) _cell_length_b 23.435(2) _cell_length_c 11.7021(12) _cell_angle_alpha 90.00 _cell_angle_beta 93.836(2) _cell_angle_gamma 90.00 _cell_volume 1796.6(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 6651 _cell_measurement_theta_min 4.925 _cell_measurement_theta_max 54.784 _exptl_crystal_description needle _exptl_crystal_colour red _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.832 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 984 _exptl_absorpt_coefficient_mu 1.367 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6853 _exptl_absorpt_correction_T_max 0.8499 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker smart1000' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 100 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19966 _diffrn_reflns_av_R_equivalents 0.0587 _diffrn_reflns_av_sigmaI/netI 0.0436 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.74 _diffrn_reflns_theta_max 27.58 _reflns_number_total 4104 _reflns_number_gt 3260 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0267P)^2^+1.7100P] 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 4104 _refine_ls_number_parameters 235 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0451 _refine_ls_R_factor_gt 0.0296 _refine_ls_wR_factor_ref 0.0670 _refine_ls_wR_factor_gt 0.0612 _refine_ls_goodness_of_fit_ref 0.994 _refine_ls_restrained_S_all 0.994 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru Ru 0.74186(3) 0.873207(9) 0.773547(18) 0.01205(7) Uani 1 1 d . . . K1 K 0.64031(10) 0.74516(3) 0.97849(6) 0.02523(16) Uani 1 1 d . . . K2 K 0.61429(9) 1.14832(3) 0.77948(5) 0.01779(14) Uani 1 1 d . . . C1 C 0.3711(4) 0.92962(13) 0.6379(2) 0.0179(6) Uani 1 1 d . . . H1 H 0.3185 0.8922 0.6263 0.021 Uiso 1 1 calc R . . C2 C 0.2640(4) 0.97532(13) 0.5914(2) 0.0205(6) Uani 1 1 d . . . H2 H 0.1392 0.9700 0.5467 0.025 Uiso 1 1 calc R . . C3 C 0.3435(4) 1.02910(13) 0.6117(3) 0.0215(6) Uani 1 1 d . . . H3 H 0.2709 1.0612 0.5805 0.026 Uiso 1 1 calc R . . C4 C 0.6160(4) 0.99129(12) 0.7140(2) 0.0145(6) Uani 1 1 d . . . C5 C 0.8176(4) 0.99753(12) 0.7803(2) 0.0145(6) Uani 1 1 d . . . C6 C 1.0753(4) 1.05307(13) 0.8569(3) 0.0221(6) Uani 1 1 d . . . H6 H 1.1335 1.0896 0.8728 0.027 Uiso 1 1 calc R . . C7 C 1.1827(4) 1.00472(12) 0.8938(2) 0.0185(6) Uani 1 1 d . . . H7 H 1.3134 1.0077 0.9333 0.022 Uiso 1 1 calc R . . C8 C 1.0933(4) 0.95210(12) 0.8710(2) 0.0168(6) Uani 1 1 d . . . H8 H 1.1629 0.9183 0.8958 0.020 Uiso 1 1 calc R . . C9 C 0.8771(4) 0.86599(11) 0.6223(2) 0.0154(6) Uani 1 1 d . . . C10 C 0.9431(4) 0.82076(12) 0.8511(2) 0.0173(6) Uani 1 1 d . . . C11 C 0.5626(4) 0.80700(12) 0.7276(2) 0.0161(6) Uani 1 1 d . . . C12 C 0.5987(4) 0.87916(12) 0.9234(2) 0.0161(6) Uani 1 1 d . . . N1 N 0.5500(3) 0.93710(10) 0.69973(19) 0.0138(5) Uani 1 1 d . . . N2 N 0.5199(3) 1.03774(10) 0.6741(2) 0.0172(5) Uani 1 1 d . . . N3 N 0.8918(3) 1.04982(10) 0.7996(2) 0.0183(5) Uani 1 1 d . . . N4 N 0.9083(3) 0.94832(9) 0.81415(18) 0.0129(5) Uani 1 1 d . . . N5 N 0.9466(4) 0.86312(11) 0.5347(2) 0.0214(5) Uani 1 1 d . . . N6 N 1.0577(4) 0.79127(11) 0.9016(2) 0.0246(6) Uani 1 1 d . . . N7 N 0.4592(4) 0.76891(10) 0.6997(2) 0.0228(6) Uani 1 1 d . . . N8 N 0.5188(4) 0.88164(11) 1.0085(2) 0.0247(6) Uani 1 1 d . . . O1 O 1.0305(3) 0.78386(9) 1.14380(18) 0.0288(5) Uani 1 1 d . . . H5 H 1.0946 0.7558 1.1614 0.035 Uiso 1 1 d R . . H4 H 1.0559 0.7835 1.0780 0.035 Uiso 1 1 d R . . O2 O 0.2214(3) 1.16701(9) 0.69340(18) 0.0258(5) Uani 1 1 d . . . H10 H 0.1410 1.1559 0.6419 0.031 Uiso 1 1 d R . . H9 H 0.1571 1.1821 0.7403 0.031 Uiso 1 1 d R . . O3 O 0.7170(3) 1.18957(9) 0.57830(16) 0.0217(4) Uani 1 1 d . . . H12 H 0.7899 1.1686 0.5376 0.026 Uiso 1 1 d R . . H11 H 0.7741 1.2232 0.5863 0.026 Uiso 1 1 d 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 0.01353(10) 0.01127(12) 0.01122(11) -0.00011(9) -0.00023(8) -0.00008(9) K1 0.0297(4) 0.0218(4) 0.0248(4) -0.0005(3) 0.0070(3) -0.0055(3) K2 0.0210(3) 0.0153(3) 0.0172(3) 0.0009(2) 0.0022(2) 0.0013(2) C1 0.0158(13) 0.0198(15) 0.0179(15) -0.0016(12) -0.0003(11) -0.0027(11) C2 0.0157(13) 0.0239(16) 0.0210(15) 0.0011(13) -0.0062(11) 0.0023(12) C3 0.0234(15) 0.0195(16) 0.0210(15) 0.0033(12) -0.0036(12) 0.0063(12) C4 0.0157(13) 0.0146(14) 0.0132(13) -0.0018(11) 0.0010(11) -0.0007(11) C5 0.0158(12) 0.0153(14) 0.0126(13) -0.0006(11) 0.0017(11) 0.0003(11) C6 0.0231(15) 0.0225(16) 0.0206(15) -0.0011(13) 0.0004(12) -0.0070(12) C7 0.0152(13) 0.0225(16) 0.0172(14) -0.0023(12) -0.0038(11) -0.0023(11) C8 0.0178(13) 0.0195(15) 0.0132(14) -0.0011(12) 0.0002(11) 0.0012(11) C9 0.0151(12) 0.0102(14) 0.0206(15) -0.0006(11) -0.0015(11) -0.0006(10) C10 0.0216(14) 0.0134(14) 0.0173(14) -0.0013(12) 0.0032(12) -0.0032(11) C11 0.0174(13) 0.0168(15) 0.0140(14) 0.0019(11) 0.0011(11) 0.0031(11) C12 0.0133(12) 0.0153(15) 0.0186(15) 0.0007(12) -0.0060(11) -0.0019(11) N1 0.0143(11) 0.0138(12) 0.0135(11) -0.0008(9) 0.0013(9) 0.0005(9) N2 0.0186(11) 0.0150(12) 0.0176(12) -0.0010(10) -0.0024(10) 0.0020(9) N3 0.0202(12) 0.0152(12) 0.0192(13) -0.0014(10) -0.0010(10) -0.0024(10) N4 0.0132(10) 0.0149(12) 0.0108(11) -0.0011(9) 0.0009(9) 0.0004(9) N5 0.0212(12) 0.0249(14) 0.0181(13) -0.0023(11) 0.0023(10) 0.0006(10) N6 0.0251(13) 0.0231(14) 0.0251(14) 0.0071(11) -0.0011(11) 0.0052(11) N7 0.0292(14) 0.0168(13) 0.0221(13) 0.0003(11) -0.0006(11) -0.0047(11) N8 0.0248(13) 0.0309(16) 0.0183(13) 0.0004(11) 0.0022(11) -0.0037(11) O1 0.0350(12) 0.0291(13) 0.0226(11) -0.0013(10) 0.0041(10) 0.0073(10) O2 0.0233(11) 0.0306(13) 0.0230(11) -0.0060(10) -0.0025(9) 0.0027(9) O3 0.0241(10) 0.0215(11) 0.0200(11) -0.0042(9) 0.0061(9) -0.0029(9) _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 C10 1.980(3) . ? Ru C11 2.000(3) . ? Ru C9 2.040(3) . ? Ru C12 2.049(3) . ? Ru N1 2.105(2) . ? Ru N4 2.109(2) . ? Ru K1 3.9261(8) . ? K1 O3 2.727(2) 2_646 ? K1 O2 2.910(2) 2_646 ? K1 N7 2.938(3) 4_576 ? K1 C10 3.116(3) . ? K1 N6 3.133(3) . ? K1 C12 3.214(3) . ? K1 C11 3.232(3) 4_576 ? K1 O1 3.235(2) . ? K1 N5 3.277(3) 4_576 ? K1 C11 3.284(3) . ? K1 N8 3.320(3) . ? K1 C9 3.418(3) 4_576 ? K1 H4 3.0312 . ? K2 O3 2.673(2) . ? K2 O2 2.741(2) . ? K2 N8 2.776(3) 3_677 ? K2 N7 2.880(3) 2_656 ? K2 O1 2.914(2) 3_777 ? K2 N2 2.919(2) . ? K2 N3 2.940(2) . ? K2 K1 4.0476(9) 2_656 ? K2 K1 4.2049(10) 3_677 ? C1 N1 1.349(3) . ? C1 C2 1.374(4) . ? C1 H1 0.9500 . ? C2 C3 1.379(4) . ? C2 H2 0.9500 . ? C3 N2 1.342(3) . ? C3 H3 0.9500 . ? C4 N2 1.328(3) . ? C4 N1 1.349(3) . ? C4 C5 1.496(4) . ? C5 N3 1.332(3) . ? C5 N4 1.345(3) . ? C6 N3 1.342(4) . ? C6 C7 1.388(4) . ? C6 H6 0.9500 . ? C7 C8 1.384(4) . ? C7 H7 0.9500 . ? C8 N4 1.349(3) . ? C8 H8 0.9500 . ? C9 N5 1.152(4) . ? C9 K1 3.418(3) 4_575 ? C10 N6 1.155(4) . ? C11 N7 1.155(4) . ? C11 K1 3.232(3) 4_575 ? C12 N8 1.157(4) . ? N5 K1 3.277(3) 4_575 ? N7 K2 2.880(3) 2_646 ? N7 K1 2.938(3) 4_575 ? N8 K2 2.776(3) 3_677 ? O1 K2 2.914(2) 3_777 ? O1 H5 0.7997 . ? O1 H4 0.7983 . ? O2 K1 2.910(2) 2_656 ? O2 H10 0.8164 . ? O2 H9 0.7977 . ? O3 K1 2.727(2) 2_656 ? O3 H12 0.8526 . ? O3 H11 0.8759 . ? 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 C10 Ru C11 90.25(11) . . ? C10 Ru C9 91.73(11) . . ? C11 Ru C9 89.13(11) . . ? C10 Ru C12 88.87(11) . . ? C11 Ru C12 89.30(11) . . ? C9 Ru C12 178.32(11) . . ? C10 Ru N1 173.03(10) . . ? C11 Ru N1 96.67(10) . . ? C9 Ru N1 89.22(10) . . ? C12 Ru N1 90.38(10) . . ? C10 Ru N4 95.46(10) . . ? C11 Ru N4 174.28(10) . . ? C9 Ru N4 90.89(9) . . ? C12 Ru N4 90.61(9) . . ? N1 Ru N4 77.62(9) . . ? C10 Ru K1 51.75(8) . . ? C11 Ru K1 56.66(8) . . ? C9 Ru K1 124.63(8) . . ? C12 Ru K1 54.75(8) . . ? N1 Ru K1 132.30(6) . . ? N4 Ru K1 127.36(6) . . ? O3 K1 O2 80.45(6) 2_646 2_646 ? O3 K1 N7 76.62(7) 2_646 4_576 ? O2 K1 N7 134.55(7) 2_646 4_576 ? O3 K1 C10 136.15(7) 2_646 . ? O2 K1 C10 77.79(7) 2_646 . ? N7 K1 C10 142.56(7) 4_576 . ? O3 K1 N6 148.18(7) 2_646 . ? O2 K1 N6 72.50(6) 2_646 . ? N7 K1 N6 134.82(7) 4_576 . ? C10 K1 N6 21.30(7) . . ? O3 K1 C12 110.97(7) 2_646 . ? O2 K1 C12 120.18(7) 2_646 . ? N7 K1 C12 104.61(7) 4_576 . ? C10 K1 C12 52.91(7) . . ? N6 K1 C12 70.71(7) . . ? O3 K1 C11 81.59(6) 2_646 4_576 ? O2 K1 C11 117.43(7) 2_646 4_576 ? N7 K1 C11 20.89(7) 4_576 4_576 ? C10 K1 C11 142.25(7) . 4_576 ? N6 K1 C11 125.67(7) . 4_576 ? C12 K1 C11 122.27(8) . 4_576 ? O3 K1 O1 156.03(6) 2_646 . ? O2 K1 O1 108.57(6) 2_646 . ? N7 K1 O1 81.71(6) 4_576 . ? C10 K1 O1 67.77(7) . . ? N6 K1 O1 53.27(6) . . ? C12 K1 O1 84.22(6) . . ? C11 K1 O1 74.54(6) 4_576 . ? O3 K1 N5 100.69(6) 2_646 4_576 ? O2 K1 N5 55.64(6) 2_646 4_576 ? N7 K1 N5 90.89(7) 4_576 4_576 ? C10 K1 N5 97.68(7) . 4_576 ? N6 K1 N5 77.75(6) . 4_576 ? C12 K1 N5 147.10(7) . 4_576 ? C11 K1 N5 70.01(7) 4_576 4_576 ? O1 K1 N5 69.28(6) . 4_576 ? O3 K1 C11 85.02(7) 2_646 . ? O2 K1 C11 72.34(7) 2_646 . ? N7 K1 C11 142.12(7) 4_576 . ? C10 K1 C11 52.21(7) . . ? N6 K1 C11 71.20(7) . . ? C12 K1 C11 51.93(7) . . ? C11 K1 C11 161.57(9) 4_576 . ? O1 K1 C11 118.72(7) . . ? N5 K1 C11 125.29(7) 4_576 . ? O3 K1 N8 106.09(6) 2_646 . ? O2 K1 N8 140.12(7) 2_646 . ? N7 K1 N8 84.31(7) 4_576 . ? C10 K1 N8 70.63(7) . . ? N6 K1 N8 85.35(7) . . ? C12 K1 N8 20.31(6) . . ? C11 K1 N8 102.44(7) 4_576 . ? O1 K1 N8 81.55(6) . . ? N5 K1 N8 150.83(7) 4_576 . ? C11 K1 N8 69.23(7) . . ? O3 K1 C9 96.40(6) 2_646 4_576 ? O2 K1 C9 73.02(6) 2_646 4_576 ? N7 K1 C9 71.24(7) 4_576 4_576 ? C10 K1 C9 112.65(7) . 4_576 ? N6 K1 C9 91.51(7) . 4_576 ? C12 K1 C9 150.82(7) . 4_576 ? C11 K1 C9 50.36(7) 4_576 4_576 ? O1 K1 C9 66.63(6) . 4_576 ? N5 K1 C9 19.67(6) 4_576 4_576 ? C11 K1 C9 144.58(7) . 4_576 ? N8 K1 C9 141.86(7) . 4_576 ? O3 K1 H4 166.7 2_646 . ? O2 K1 H4 97.9 2_646 . ? N7 K1 H4 95.8 4_576 . ? C10 K1 H4 55.1 . . ? N6 K1 H4 39.3 . . ? C12 K1 H4 81.3 . . ? C11 K1 H4 87.6 4_576 . ? O1 K1 H4 14.2 . . ? N5 K1 H4 68.2 4_576 . ? C11 K1 H4 107.1 . . ? N8 K1 H4 83.7 . . ? C9 K1 H4 70.7 4_576 . ? O3 K2 O2 84.57(6) . . ? O3 K2 N8 172.74(7) . 3_677 ? O2 K2 N8 91.38(7) . 3_677 ? O3 K2 N7 76.90(7) . 2_656 ? O2 K2 N7 73.47(7) . 2_656 ? N8 K2 N7 96.19(8) 3_677 2_656 ? O3 K2 O1 80.22(6) . 3_777 ? O2 K2 O1 137.75(6) . 3_777 ? N8 K2 O1 98.97(7) 3_677 3_777 ? N7 K2 O1 64.77(7) 2_656 3_777 ? O3 K2 N2 90.44(7) . . ? O2 K2 N2 79.55(6) . . ? N8 K2 N2 94.74(7) 3_677 . ? N7 K2 N2 151.05(7) 2_656 . ? O1 K2 N2 139.23(7) 3_777 . ? O3 K2 N3 99.37(7) . . ? O2 K2 N3 135.86(7) . . ? N8 K2 N3 87.73(7) 3_677 . ? N7 K2 N3 150.45(7) 2_656 . ? O1 K2 N3 85.68(6) 3_777 . ? N2 K2 N3 56.61(6) . . ? O3 K2 K1 41.95(4) . 2_656 ? O2 K2 K1 45.95(5) . 2_656 ? N8 K2 K1 132.03(6) 3_677 2_656 ? N7 K2 K1 56.63(5) 2_656 2_656 ? O1 K2 K1 101.89(5) 3_777 2_656 ? N2 K2 K1 96.73(5) . 2_656 ? N3 K2 K1 136.27(5) . 2_656 ? O3 K2 K1 120.91(5) . 3_677 ? O2 K2 K1 75.28(5) . 3_677 ? N8 K2 K1 52.03(6) 3_677 3_677 ? N7 K2 K1 44.27(5) 2_656 3_677 ? O1 K2 K1 79.32(5) 3_777 3_677 ? N2 K2 K1 136.81(5) . 3_677 ? N3 K2 K1 133.18(5) . 3_677 ? K1 K2 K1 90.374(16) 2_656 3_677 ? N1 C1 C2 121.0(3) . . ? N1 C1 H1 119.5 . . ? C2 C1 H1 119.5 . . ? C1 C2 C3 117.8(3) . . ? C1 C2 H2 121.1 . . ? C3 C2 H2 121.1 . . ? N2 C3 C2 122.3(3) . . ? N2 C3 H3 118.8 . . ? C2 C3 H3 118.8 . . ? N2 C4 N1 125.9(2) . . ? N2 C4 C5 119.1(2) . . ? N1 C4 C5 115.0(2) . . ? N3 C5 N4 126.1(2) . . ? N3 C5 C4 118.6(2) . . ? N4 C5 C4 115.3(2) . . ? N3 C6 C7 122.0(3) . . ? N3 C6 H6 119.0 . . ? C7 C6 H6 119.0 . . ? C8 C7 C6 117.9(2) . . ? C8 C7 H7 121.1 . . ? C6 C7 H7 121.1 . . ? N4 C8 C7 120.7(3) . . ? N4 C8 H8 119.7 . . ? C7 C8 H8 119.7 . . ? N5 C9 Ru 177.1(2) . . ? N5 C9 K1 73.22(18) . 4_575 ? Ru C9 K1 106.27(10) . 4_575 ? N6 C10 Ru 176.5(3) . . ? N6 C10 K1 80.19(19) . . ? Ru C10 K1 98.32(10) . . ? N7 C11 Ru 179.2(3) . . ? N7 C11 K1 65.06(18) . 4_575 ? Ru C11 K1 114.24(11) . 4_575 ? N7 C11 K1 87.99(19) . . ? Ru C11 K1 92.76(9) . . ? K1 C11 K1 127.95(9) 4_575 . ? N8 C12 Ru 178.9(3) . . ? N8 C12 K1 85.06(19) . . ? Ru C12 K1 93.86(10) . . ? C4 N1 C1 116.7(2) . . ? C4 N1 Ru 116.12(17) . . ? C1 N1 Ru 127.12(19) . . ? C4 N2 C3 116.1(2) . . ? C4 N2 K2 119.77(17) . . ? C3 N2 K2 120.98(18) . . ? C5 N3 C6 116.3(2) . . ? C5 N3 K2 119.41(17) . . ? C6 N3 K2 121.76(19) . . ? C5 N4 C8 117.1(2) . . ? C5 N4 Ru 115.90(17) . . ? C8 N4 Ru 127.02(19) . . ? C9 N5 K1 87.11(18) . 4_575 ? C10 N6 K1 78.51(19) . . ? C11 N7 K2 146.4(2) . 2_646 ? C11 N7 K1 94.1(2) . 4_575 ? K2 N7 K1 92.55(7) 2_646 4_575 ? C11 N7 K1 72.41(18) . . ? K2 N7 K1 79.06(6) 2_646 . ? K1 N7 K1 133.01(9) 4_575 . ? C12 N8 K2 160.8(2) . 3_677 ? C12 N8 K1 74.63(19) . . ? K2 N8 K1 86.73(7) 3_677 . ? K2 O1 K1 157.32(8) 3_777 . ? K2 O1 H5 88.4 3_777 . ? K1 O1 H5 107.8 . . ? K2 O1 H4 95.0 3_777 . ? K1 O1 H4 68.2 . . ? H5 O1 H4 95.8 . . ? K2 O2 K1 91.44(6) . 2_656 ? K2 O2 H10 140.0 . . ? K1 O2 H10 84.6 2_656 . ? K2 O2 H9 110.3 . . ? K1 O2 H9 113.6 2_656 . ? H10 O2 H9 107.7 . . ? K2 O3 K1 97.11(6) . 2_656 ? K2 O3 H12 117.9 . . ? K1 O3 H12 130.2 2_656 . ? K2 O3 H11 111.3 . . ? K1 O3 H11 87.2 2_656 . ? H12 O3 H11 109.0 . . ? 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 O3 H11 N6 0.88 1.94 2.807(3) 170.4 2_756 O1 H4 N6 0.80 2.07 2.856(3) 167.0 . _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 27.58 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.636 _refine_diff_density_min -0.616 _refine_diff_density_rms 0.100 #===END data_md21a _database_code_depnum_ccdc_archive 'CCDC 276246' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H16 K2 N7 O1.50 Ru' _chemical_formula_weight 557.67 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' K K 0.2009 0.2494 '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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M I2/a loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y, -z' 'x+1/2, y+1/2, z+1/2' '-x+1, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y, z' '-x+1/2, -y+1/2, -z+1/2' 'x, -y+1/2, z+1/2' _cell_length_a 17.648(3) _cell_length_b 8.9779(16) _cell_length_c 29.053(6) _cell_angle_alpha 90.00 _cell_angle_beta 105.468(3) _cell_angle_gamma 90.00 _cell_volume 4436.5(14) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.670 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2232 _exptl_absorpt_coefficient_mu 1.112 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.70 _exptl_absorpt_correction_T_max 0.81 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker smart1000' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14915 _diffrn_reflns_av_R_equivalents 0.0650 _diffrn_reflns_av_sigmaI/netI 0.1029 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -37 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_theta_min 1.45 _diffrn_reflns_theta_max 27.56 _reflns_number_total 4950 _reflns_number_gt 3269 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0000P)^2^+19.4700P] 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 4950 _refine_ls_number_parameters 285 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0998 _refine_ls_R_factor_gt 0.0586 _refine_ls_wR_factor_ref 0.1476 _refine_ls_wR_factor_gt 0.1269 _refine_ls_goodness_of_fit_ref 1.105 _refine_ls_restrained_S_all 1.105 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.01986(3) 0.40696(5) 0.136515(15) 0.02999(15) Uani 1 1 d . . . K1 K 0.18418(8) 0.89575(17) 0.23485(6) 0.0489(4) Uani 1 1 d . . . K2 K 0.04469(9) 0.57373(17) 0.28085(6) 0.0500(4) Uani 1 1 d . . . C1 C 0.0662(4) 0.2188(8) 0.1659(2) 0.0370(14) Uani 1 1 d . . . N1 N 0.0944(3) 0.1085(7) 0.1824(2) 0.0500(14) Uani 1 1 d . . . C2 C 0.1062(3) 0.5254(7) 0.1830(2) 0.0339(13) Uani 1 1 d . . . N2 N 0.1526(3) 0.5928(6) 0.21067(18) 0.0445(13) Uani 1 1 d . . . C3 C -0.0715(4) 0.2901(7) 0.0925(2) 0.0386(14) Uani 1 1 d . . . N3 N -0.1235(3) 0.2277(7) 0.0678(2) 0.0599(17) Uani 1 1 d . . . C4 C -0.0387(3) 0.4085(6) 0.1858(2) 0.0345(13) Uani 1 1 d . . . N4 N -0.0698(3) 0.3941(6) 0.21588(19) 0.0480(14) Uani 1 1 d . . . N11 N 0.0799(3) 0.3967(6) 0.08300(16) 0.0354(11) Uani 1 1 d . . . C12 C 0.0797(3) 0.5196(8) 0.0569(2) 0.0372(14) Uani 1 1 d . . . C13 C 0.1164(4) 0.5247(9) 0.0201(2) 0.0522(19) Uani 1 1 d . . . H13 H 0.1166 0.6120 0.0029 0.063 Uiso 1 1 calc R . . C14 C 0.1526(4) 0.3970(10) 0.0096(2) 0.060(2) Uani 1 1 d . . . H14 H 0.1766 0.3972 -0.0153 0.071 Uiso 1 1 calc R . . C15 C 0.1530(4) 0.2701(10) 0.0361(2) 0.0544(19) Uani 1 1 d . . . H15 H 0.1775 0.1837 0.0298 0.065 Uiso 1 1 calc R . . C16 C 0.1161(3) 0.2743(9) 0.0724(2) 0.0459(17) Uani 1 1 d . . . H16 H 0.1161 0.1886 0.0904 0.055 Uiso 1 1 calc R . . N21 N -0.0100(3) 0.6200(6) 0.09936(15) 0.0325(11) Uani 1 1 d . . . C22 C -0.0531(3) 0.7332(7) 0.1096(2) 0.0364(14) Uani 1 1 d . . . C23 C -0.0499(4) 0.8754(8) 0.0923(2) 0.0477(17) Uani 1 1 d . . . H23 H -0.0792 0.9519 0.1007 0.057 Uiso 1 1 calc R . . C24 C -0.0025(4) 0.9026(9) 0.0622(2) 0.0566(19) Uani 1 1 d . . . H24 H 0.0004 0.9978 0.0502 0.068 Uiso 1 1 calc R . . C25 C 0.0400(4) 0.7893(8) 0.0503(2) 0.0477(17) Uani 1 1 d . . . H25 H 0.0716 0.8062 0.0298 0.057 Uiso 1 1 calc R . . C26 C 0.0353(3) 0.6486(7) 0.06898(19) 0.0363(14) Uani 1 1 d . . . N31 N -0.1075(3) 0.7973(6) 0.1746(2) 0.0491(14) Uani 1 1 d . . . C32 C -0.1103(3) 0.7030(7) 0.1374(2) 0.0332(13) Uani 1 1 d . . . C33 C -0.1681(3) 0.5953(7) 0.1236(2) 0.0397(14) Uani 1 1 d . . . H33 H -0.1679 0.5312 0.0985 0.048 Uiso 1 1 calc R . . C34 C -0.2257(4) 0.5837(8) 0.1473(2) 0.0455(16) Uani 1 1 d . . . H34 H -0.2655 0.5132 0.1380 0.055 Uiso 1 1 calc R . . C35 C -0.2235(4) 0.6779(8) 0.1849(3) 0.0505(18) Uani 1 1 d . . . H35 H -0.2620 0.6738 0.2014 0.061 Uiso 1 1 calc R . . C36 C -0.1631(5) 0.7779(9) 0.1974(3) 0.060(2) Uani 1 1 d . . . H36 H -0.1605 0.8374 0.2240 0.072 Uiso 1 1 calc R . . C100 C 0.2585(6) 0.6198(14) 0.3713(3) 0.116(4) Uani 1 1 d . . . H10A H 0.2330 0.5557 0.3890 0.173 Uiso 1 1 calc R . . H10B H 0.2828 0.7014 0.3912 0.173 Uiso 1 1 calc R . . H10C H 0.2979 0.5646 0.3613 0.173 Uiso 1 1 calc R . . O100 O 0.7500 0.0523(10) 0.0000 0.107(3) Uani 1 2 d S . . O101 O 0.2040(4) 0.6738(8) 0.3319(3) 0.103(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.0302(3) 0.0324(3) 0.0286(2) 0.0028(2) 0.00978(17) 0.0014(2) K1 0.0385(8) 0.0412(9) 0.0643(9) 0.0022(7) 0.0090(7) 0.0057(7) K2 0.0465(8) 0.0432(9) 0.0651(10) -0.0042(7) 0.0231(7) -0.0003(7) C1 0.041(3) 0.041(4) 0.034(3) -0.003(3) 0.017(3) -0.007(3) N1 0.054(3) 0.044(4) 0.056(3) 0.011(3) 0.022(3) 0.011(3) C2 0.037(3) 0.037(4) 0.031(3) 0.007(3) 0.015(3) 0.014(3) N2 0.041(3) 0.048(4) 0.043(3) -0.007(3) 0.008(2) -0.003(3) C3 0.046(4) 0.038(4) 0.036(3) 0.010(3) 0.018(3) 0.008(3) N3 0.051(4) 0.054(4) 0.064(4) 0.004(3) -0.004(3) -0.014(3) C4 0.039(3) 0.023(3) 0.043(3) 0.001(3) 0.014(3) 0.006(3) N4 0.049(3) 0.047(4) 0.053(3) 0.010(3) 0.024(3) 0.010(3) N11 0.032(3) 0.038(3) 0.037(3) 0.000(2) 0.010(2) -0.003(2) C12 0.022(3) 0.054(4) 0.035(3) 0.004(3) 0.006(2) -0.001(3) C13 0.040(4) 0.081(6) 0.037(3) 0.015(4) 0.013(3) -0.004(4) C14 0.043(4) 0.107(7) 0.032(3) -0.003(4) 0.015(3) 0.006(4) C15 0.043(4) 0.080(6) 0.040(4) -0.009(4) 0.011(3) 0.008(4) C16 0.034(3) 0.062(5) 0.042(4) -0.008(3) 0.011(3) 0.003(3) N21 0.026(2) 0.045(3) 0.027(2) 0.005(2) 0.0063(18) -0.002(2) C22 0.034(3) 0.039(4) 0.034(3) 0.011(3) 0.006(2) -0.002(3) C23 0.053(4) 0.042(4) 0.047(4) 0.009(3) 0.011(3) 0.003(3) C24 0.063(5) 0.048(5) 0.056(4) 0.016(4) 0.013(4) -0.010(4) C25 0.044(4) 0.057(5) 0.043(4) 0.017(3) 0.013(3) -0.004(3) C26 0.031(3) 0.048(4) 0.028(3) 0.007(3) 0.004(2) -0.006(3) N31 0.055(4) 0.040(3) 0.059(4) -0.003(3) 0.027(3) -0.007(3) C32 0.034(3) 0.030(3) 0.034(3) 0.010(3) 0.007(2) 0.006(3) C33 0.033(3) 0.042(4) 0.041(3) 0.005(3) 0.004(3) 0.006(3) C34 0.032(3) 0.047(4) 0.056(4) 0.012(3) 0.009(3) 0.000(3) C35 0.041(4) 0.050(5) 0.068(5) 0.006(4) 0.027(3) 0.007(3) C36 0.075(5) 0.047(5) 0.069(5) -0.011(4) 0.039(4) -0.003(4) C100 0.084(7) 0.204(14) 0.057(5) -0.014(7) 0.017(5) 0.012(8) O100 0.121(8) 0.073(7) 0.100(7) 0.000 -0.020(6) 0.000 O101 0.077(4) 0.103(6) 0.110(5) -0.022(4) -0.010(4) 0.003(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 C1 1.970(7) . ? Ru1 C4 1.977(6) . ? Ru1 C2 2.045(7) . ? Ru1 C3 2.057(7) . ? Ru1 N11 2.105(5) . ? Ru1 N21 2.190(5) . ? K1 N1 2.681(6) 1_565 ? K1 N4 2.769(5) 4_455 ? K1 N2 2.827(6) . ? K1 N2 2.895(5) 7_565 ? K1 O101 3.176(8) 7_565 ? K1 O101 3.395(8) . ? K1 C35 3.386(7) 4_455 ? K1 K1 3.454(3) 7_565 ? K1 C100 3.495(9) 7_565 ? K1 K2 4.238(2) . ? K1 K2 4.254(2) 4_455 ? K1 K2 4.934(2) 7_565 ? K2 N4 2.866(6) . ? K2 N31 2.881(6) 4_445 ? K2 N4 2.908(6) 4_455 ? K2 N1 2.943(6) 4_455 ? K2 O101 2.948(7) . ? K2 C1 3.086(6) 4_455 ? K2 C4 3.134(6) . ? K2 N2 3.144(5) . ? K2 C4 3.168(6) 4_455 ? K2 C2 3.330(6) . ? K2 C36 3.334(8) 4_445 ? C1 N1 1.154(8) . ? C1 K2 3.086(6) 4_445 ? N1 K1 2.681(6) 1_545 ? N1 K2 2.943(6) 4_445 ? C2 N2 1.153(7) . ? N2 K1 2.895(5) 7_565 ? C3 N3 1.149(8) . ? C4 N4 1.157(7) . ? C4 K2 3.168(6) 4_445 ? N4 K1 2.769(5) 4_445 ? N4 K2 2.908(6) 4_445 ? N11 C12 1.339(8) . ? N11 C16 1.346(8) . ? C12 C13 1.390(8) . ? C12 C26 1.491(9) . ? C13 C14 1.386(10) . ? C14 C15 1.375(11) . ? C15 C16 1.380(9) . ? N21 C22 1.349(7) . ? N21 C26 1.364(7) . ? C22 C23 1.380(8) . ? C22 C32 1.478(8) . ? C23 C24 1.381(9) . ? C24 C25 1.362(10) . ? C25 C26 1.387(9) . ? N31 C36 1.335(8) . ? N31 C32 1.362(8) . ? N31 K2 2.881(6) 4_455 ? C32 C33 1.385(8) . ? C33 C34 1.375(8) . ? C34 C35 1.375(9) . ? C35 C36 1.367(10) . ? C35 K1 3.386(7) 4_445 ? C36 K2 3.334(8) 4_455 ? C100 O101 1.371(10) . ? C100 K1 3.495(9) 7_565 ? O101 K1 3.176(8) 7_565 ? 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 C1 Ru1 C4 85.9(2) . . ? C1 Ru1 C2 90.5(2) . . ? C4 Ru1 C2 87.7(2) . . ? C1 Ru1 C3 89.9(2) . . ? C4 Ru1 C3 88.8(2) . . ? C2 Ru1 C3 176.4(2) . . ? C1 Ru1 N11 92.9(2) . . ? C4 Ru1 N11 177.6(2) . . ? C2 Ru1 N11 94.4(2) . . ? C3 Ru1 N11 89.1(2) . . ? C1 Ru1 N21 168.6(2) . . ? C4 Ru1 N21 104.3(2) . . ? C2 Ru1 N21 84.9(2) . . ? C3 Ru1 N21 95.4(2) . . ? N11 Ru1 N21 77.08(18) . . ? N1 K1 N4 84.03(17) 1_565 4_455 ? N1 K1 N2 119.78(18) 1_565 . ? N4 K1 N2 90.05(16) 4_455 . ? N1 K1 N2 129.50(18) 1_565 7_565 ? N4 K1 N2 118.28(16) 4_455 7_565 ? N2 K1 N2 105.75(14) . 7_565 ? N1 K1 O101 99.32(18) 1_565 7_565 ? N4 K1 O101 166.43(18) 4_455 7_565 ? N2 K1 O101 76.84(17) . 7_565 ? N2 K1 O101 69.61(16) 7_565 7_565 ? N1 K1 O101 143.58(17) 1_565 . ? N4 K1 O101 59.68(17) 4_455 . ? N2 K1 O101 67.14(16) . . ? N2 K1 O101 72.50(16) 7_565 . ? O101 K1 O101 116.68(15) 7_565 . ? N1 K1 C35 80.79(18) 1_565 4_455 ? N4 K1 C35 72.07(16) 4_455 4_455 ? N2 K1 C35 151.80(17) . 4_455 ? N2 K1 C35 66.77(16) 7_565 4_455 ? O101 K1 C35 121.38(17) 7_565 4_455 ? O101 K1 C35 84.86(18) . 4_455 ? N1 K1 K1 160.00(14) 1_565 7_565 ? N4 K1 K1 113.44(14) 4_455 7_565 ? N2 K1 K1 53.77(11) . 7_565 ? N2 K1 K1 51.98(12) 7_565 7_565 ? O101 K1 K1 61.42(14) 7_565 7_565 ? O101 K1 K1 55.25(12) . 7_565 ? C35 K1 K1 113.00(14) 4_455 7_565 ? N1 K1 C100 78.1(2) 1_565 7_565 ? N4 K1 C100 151.5(2) 4_455 7_565 ? N2 K1 C100 80.0(2) . 7_565 ? N2 K1 C100 90.2(2) 7_565 7_565 ? O101 K1 C100 23.09(18) 7_565 7_565 ? O101 K1 C100 136.0(2) . 7_565 ? C35 K1 C100 125.6(2) 4_455 7_565 ? K1 K1 C100 82.0(2) 7_565 7_565 ? N1 K1 K2 111.12(13) 1_565 . ? N4 K1 K2 42.98(12) 4_455 . ? N2 K1 K2 47.89(11) . . ? N2 K1 K2 115.39(12) 7_565 . ? O101 K1 K2 124.48(14) 7_565 . ? O101 K1 K2 43.73(11) . . ? C35 K1 K2 108.85(12) 4_455 . ? K1 K1 K2 79.08(6) 7_565 . ? C100 K1 K2 125.5(2) 7_565 . ? N1 K1 K2 43.23(12) 1_565 4_455 ? N4 K1 K2 41.84(12) 4_455 4_455 ? N2 K1 K2 102.49(11) . 4_455 ? N2 K1 K2 145.40(12) 7_565 4_455 ? O101 K1 K2 137.31(13) 7_565 4_455 ? O101 K1 K2 101.20(12) . 4_455 ? C35 K1 K2 78.90(12) 4_455 4_455 ? K1 K1 K2 150.09(7) 7_565 4_455 ? C100 K1 K2 114.23(18) 7_565 4_455 ? K2 K1 K2 71.05(3) . 4_455 ? N1 K1 K2 110.39(13) 1_565 7_565 ? N4 K1 K2 155.08(12) 4_455 7_565 ? N2 K1 K2 99.33(11) . 7_565 ? N2 K1 K2 36.92(11) 7_565 7_565 ? O101 K1 K2 34.80(12) 7_565 7_565 ? O101 K1 K2 102.81(12) . 7_565 ? C35 K1 K2 89.78(11) 4_455 7_565 ? K1 K1 K2 57.50(5) 7_565 7_565 ? C100 K1 K2 53.46(17) 7_565 7_565 ? K2 K1 K2 136.58(4) . 7_565 ? K2 K1 K2 152.35(4) 4_455 7_565 ? N4 K2 N31 86.02(16) . 4_445 ? N4 K2 N4 130.74(13) . 4_455 ? N31 K2 N4 143.17(17) 4_445 4_455 ? N4 K2 N1 77.80(16) . 4_455 ? N31 K2 N1 100.73(16) 4_445 4_455 ? N4 K2 N1 91.03(16) 4_455 4_455 ? N4 K2 O101 155.99(18) . . ? N31 K2 O101 80.52(19) 4_445 . ? N4 K2 O101 64.24(18) 4_455 . ? N1 K2 O101 124.13(19) 4_455 . ? N4 K2 C1 97.91(17) . 4_455 ? N31 K2 C1 110.95(16) 4_445 4_455 ? N4 K2 C1 71.20(17) 4_455 4_455 ? N1 K2 C1 21.90(14) 4_455 4_455 ? O101 K2 C1 105.43(19) . 4_455 ? N4 K2 C4 21.64(14) . . ? N31 K2 C4 91.28(16) 4_445 . ? N4 K2 C4 121.91(16) 4_455 . ? N1 K2 C4 97.39(16) 4_455 . ? O101 K2 C4 138.45(18) . . ? C1 K2 C4 115.45(17) 4_455 . ? N4 K2 N2 92.65(15) . . ? N31 K2 N2 96.41(15) 4_445 . ? N4 K2 N2 81.60(15) 4_455 . ? N1 K2 N2 159.66(16) 4_455 . ? O101 K2 N2 69.42(18) . . ? C1 K2 N2 151.20(17) 4_455 . ? C4 K2 N2 71.19(15) . . ? N4 K2 C4 131.30(16) . 4_455 ? N31 K2 C4 136.05(17) 4_445 4_455 ? N4 K2 C4 21.40(14) 4_455 4_455 ? N1 K2 C4 71.90(16) 4_455 4_455 ? O101 K2 C4 70.26(17) . 4_455 ? C1 K2 C4 50.88(17) 4_455 4_455 ? C4 K2 C4 132.24(14) . 4_455 ? N2 K2 C4 102.84(15) . 4_455 ? N4 K2 C2 72.41(16) . . ? N31 K2 C2 95.60(15) 4_445 . ? N4 K2 C2 94.31(16) 4_455 . ? N1 K2 C2 144.76(16) 4_455 . ? O101 K2 C2 89.14(19) . . ? C1 K2 C2 151.27(16) 4_455 . ? C4 K2 C2 50.94(16) . . ? N2 K2 C2 20.26(13) . . ? C4 K2 C2 115.45(16) 4_455 . ? N4 K2 C36 88.44(18) . 4_445 ? N31 K2 C36 23.37(15) 4_445 4_445 ? N4 K2 C36 134.38(18) 4_455 4_445 ? N1 K2 C36 123.85(18) 4_455 4_445 ? O101 K2 C36 71.5(2) . 4_445 ? C1 K2 C36 133.65(17) 4_455 4_445 ? C4 K2 C36 85.01(17) . 4_445 ? N2 K2 C36 73.07(16) . 4_445 ? C4 K2 C36 140.19(18) 4_455 4_445 ? C2 K2 C36 74.18(16) . 4_445 ? N4 K2 K1 122.89(12) . . ? N31 K2 K1 122.92(12) 4_445 . ? N4 K2 K1 40.47(11) 4_455 . ? N1 K2 K1 130.77(13) 4_455 . ? O101 K2 K1 52.74(16) . . ? C1 K2 K1 111.66(13) 4_455 . ? C4 K2 K1 102.75(12) . . ? N2 K2 K1 41.85(11) . . ? C4 K2 K1 61.25(11) 4_455 . ? C2 K2 K1 58.04(12) . . ? C36 K2 K1 102.46(13) 4_445 . ? N1 C1 Ru1 178.3(5) . . ? N1 C1 K2 72.1(4) . 4_445 ? Ru1 C1 K2 109.5(2) . 4_445 ? C1 N1 K1 166.3(5) . 1_545 ? C1 N1 K2 86.0(4) . 4_445 ? K1 N1 K2 98.16(18) 1_545 4_445 ? N2 C2 Ru1 176.8(5) . . ? N2 C2 K2 70.7(4) . . ? Ru1 C2 K2 106.0(2) . . ? C2 N2 K1 137.2(5) . . ? C2 N2 K1 144.8(5) . 7_565 ? K1 N2 K1 74.25(14) . 7_565 ? C2 N2 K2 89.0(4) . . ? K1 N2 K2 90.26(15) . . ? K1 N2 K2 109.50(16) 7_565 . ? N3 C3 Ru1 178.5(6) . . ? N4 C4 Ru1 172.6(5) . . ? N4 C4 K2 66.0(4) . . ? Ru1 C4 K2 115.4(2) . . ? N4 C4 K2 66.5(4) . 4_445 ? Ru1 C4 K2 106.4(2) . 4_445 ? K2 C4 K2 103.05(17) . 4_445 ? C4 N4 K1 161.6(5) . 4_445 ? C4 N4 K2 92.4(4) . . ? K1 N4 K2 98.03(17) 4_445 . ? C4 N4 K2 92.1(4) . 4_445 ? K1 N4 K2 96.56(17) 4_445 4_445 ? K2 N4 K2 117.42(18) . 4_445 ? C12 N11 C16 118.3(5) . . ? C12 N11 Ru1 117.1(4) . . ? C16 N11 Ru1 124.5(4) . . ? N11 C12 C13 122.1(6) . . ? N11 C12 C26 115.4(5) . . ? C13 C12 C26 122.5(6) . . ? C14 C13 C12 118.6(7) . . ? C15 C14 C13 119.8(6) . . ? C14 C15 C16 118.2(7) . . ? N11 C16 C15 123.1(7) . . ? C22 N21 C26 117.6(5) . . ? C22 N21 Ru1 128.7(4) . . ? C26 N21 Ru1 112.2(4) . . ? N21 C22 C23 122.5(6) . . ? N21 C22 C32 119.4(5) . . ? C23 C22 C32 118.0(6) . . ? C22 C23 C24 118.9(7) . . ? C25 C24 C23 119.8(7) . . ? C24 C25 C26 119.0(6) . . ? N21 C26 C25 122.1(6) . . ? N21 C26 C12 116.2(5) . . ? C25 C26 C12 121.7(6) . . ? C36 N31 C32 115.9(6) . . ? C36 N31 K2 97.7(4) . 4_455 ? C32 N31 K2 145.1(4) . 4_455 ? N31 C32 C33 122.2(6) . . ? N31 C32 C22 115.7(5) . . ? C33 C32 C22 121.8(5) . . ? C34 C33 C32 119.6(6) . . ? C33 C34 C35 118.9(6) . . ? C36 C35 C34 118.0(6) . . ? C36 C35 K1 107.9(5) . 4_445 ? C34 C35 K1 92.5(4) . 4_445 ? N31 C36 C35 125.4(7) . . ? N31 C36 K2 58.9(4) . 4_455 ? C35 C36 K2 168.2(6) . 4_455 ? O101 C100 K1 65.3(5) . 7_565 ? C100 O101 K2 132.4(7) . . ? C100 O101 K1 91.6(5) . 7_565 ? K2 O101 K1 107.3(2) . 7_565 ? C100 O101 K1 142.6(6) . . ? K2 O101 K1 83.53(17) . . ? K1 O101 K1 63.32(15) 7_565 . ? _diffrn_measured_fraction_theta_max 0.965 _diffrn_reflns_theta_full 27.56 _diffrn_measured_fraction_theta_full 0.965 _refine_diff_density_max 1.167 _refine_diff_density_min -0.916 _refine_diff_density_rms 0.133 #===END data_md22 _database_code_depnum_ccdc_archive 'CCDC 276247' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H23 Er0.50 K0.50 N7.50 O4.50 Ru' _chemical_formula_weight 620.69 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' K K 0.2009 0.2494 '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' Er Er -0.2586 4.9576 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 28.636(6) _cell_length_b 14.487(3) _cell_length_c 15.487(3) _cell_angle_alpha 90.00 _cell_angle_beta 103.05(3) _cell_angle_gamma 90.00 _cell_volume 6259(2) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour orange _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.317 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2456 _exptl_absorpt_coefficient_mu 1.921 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.57 _exptl_absorpt_correction_T_max 0.91 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30015 _diffrn_reflns_av_R_equivalents 0.1580 _diffrn_reflns_av_sigmaI/netI 0.1164 _diffrn_reflns_limit_h_min -34 _diffrn_reflns_limit_h_max 34 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.46 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5504 _reflns_number_gt 2817 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.1900P)^2^+1.4100P] 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 5504 _refine_ls_number_parameters 331 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1668 _refine_ls_R_factor_gt 0.0915 _refine_ls_wR_factor_ref 0.3235 _refine_ls_wR_factor_gt 0.2636 _refine_ls_goodness_of_fit_ref 1.062 _refine_ls_restrained_S_all 1.062 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru2 Ru 0.13022(4) 0.58141(10) 0.05957(9) 0.0513(5) Uani 1 1 d . . . Er1 Er 0.0000 0.46886(8) 0.2500 0.0539(4) Uani 1 2 d S . . K1 K -0.0222(3) 0.6031(6) 0.0100(6) 0.074(2) Uani 0.50 1 d P . . C4 C 0.2668(6) 0.6567(12) -0.1395(12) 0.063(5) Uani 1 1 d . . . H4 H 0.3004 0.6631 -0.1337 0.076 Uiso 1 1 calc R . . C5 C 0.1988(6) 0.6359(11) -0.0755(10) 0.051(4) Uani 1 1 d . A . C6 C 0.1852(6) 0.5746(12) 0.2564(12) 0.059(4) Uani 1 1 d . A . H6 H 0.1541 0.5646 0.2665 0.070 Uiso 1 1 calc R . . C7 C 0.0822(6) 0.5419(11) 0.1245(11) 0.057(4) Uani 1 1 d . . . C8 C 0.2734(6) 0.6013(12) 0.2268(12) 0.064(5) Uani 1 1 d . . . H8 H 0.3043 0.6109 0.2157 0.076 Uiso 1 1 calc R . . C9 C 0.2314(5) 0.6174(11) 0.0625(10) 0.049(4) Uani 1 1 d . A . C10 C 0.0793(7) 0.5814(15) -0.0465(12) 0.067(5) Uani 1 1 d . . . C11 C 0.3196(5) 0.6319(13) 0.0571(13) 0.068(5) Uani 1 1 d . . . H11A H 0.3264 0.6622 0.1159 0.082 Uiso 1 1 calc R . . H11B H 0.3359 0.6679 0.0182 0.082 Uiso 1 1 calc R . . C12 C 0.2478(5) 0.6427(10) -0.0680(10) 0.046(4) Uani 1 1 d . . . C13 C 0.1447(7) 0.4544(17) 0.0361(13) 0.072(6) Uani 1 1 d . . . C14 C 0.1145(6) 0.7097(15) 0.0798(12) 0.065(5) Uani 1 1 d . . . C15 C 0.1677(6) 0.6382(12) -0.1573(11) 0.058(4) Uani 1 1 d . . . H15 H 0.1342 0.6306 -0.1635 0.070 Uiso 1 1 calc R . . C16 C 0.1874(7) 0.6522(11) -0.2313(12) 0.061(5) Uani 1 1 d . . . H16 H 0.1671 0.6553 -0.2889 0.073 Uiso 1 1 calc R . . C17 C 0.3402(8) 0.5343(14) 0.0672(17) 0.096(7) Uani 1 1 d . . . H17A H 0.3301 0.5030 0.1161 0.144 Uiso 1 1 calc R . . H17B H 0.3753 0.5374 0.0800 0.144 Uiso 1 1 calc R . . H17C H 0.3285 0.4999 0.0121 0.144 Uiso 1 1 calc R . . C18 C 0.2325(5) 0.5991(11) 0.1572(11) 0.051(4) Uani 1 1 d . A . C19 C 0.2673(7) 0.5887(14) 0.3140(13) 0.075(6) Uani 1 1 d . . . H19 H 0.2945 0.5884 0.3623 0.090 Uiso 1 1 calc R . . C20 C 0.2230(6) 0.5772(12) 0.3291(12) 0.061(4) Uani 1 1 d . . . H20 H 0.2181 0.5712 0.3875 0.073 Uiso 1 1 calc R . . C22 C 0.2356(6) 0.6612(12) -0.2204(12) 0.062(5) Uani 1 1 d . . . H22 H 0.2482 0.6711 -0.2714 0.075 Uiso 1 1 calc R . . N1 N 0.2684(5) 0.6335(9) 0.0202(10) 0.058(4) Uani 1 1 d . . . N2 N 0.1893(4) 0.6180(10) 0.0071(8) 0.055(3) Uani 1 1 d . . . N3 N 0.1046(6) 0.7868(15) 0.0960(13) 0.095(6) Uani 1 1 d . A . N4 N 0.0516(5) 0.5194(10) 0.1600(9) 0.062(4) Uani 1 1 d . . . N6 N 0.0476(6) 0.5771(14) -0.1109(11) 0.087(6) Uani 1 1 d . . . N8 N 0.1891(5) 0.5852(9) 0.1716(9) 0.053(3) Uani 1 1 d . . . N12 N 0.1518(7) 0.3746(17) 0.0182(12) 0.104(6) Uani 1 1 d . A . O1 O 0.0443(4) 0.3369(8) 0.2249(8) 0.069(3) Uani 1 1 d . A . O2 O 0.0484(8) 0.1706(16) 0.301(2) 0.085(9) Uani 0.50 1 d P . . O3 O -0.0257(10) 0.623(2) 0.195(2) 0.086(9) Uani 0.50 1 d P A 1 O4 O -0.0771(12) 0.710(2) -0.0767(17) 0.103(10) Uani 0.50 1 d P . . O5 O 0.3882(9) 0.595(2) 0.2859(19) 0.098(10) Uani 0.50 1 d P . . O6 O 0.9126(14) 0.751(2) 0.225(2) 0.132(15) Uani 0.50 1 d P . . O7 O -0.0606(13) 0.581(2) 0.1671(18) 0.095(10) Uani 0.50 1 d P A 2 O8 O 0.1639(14) 0.206(2) 0.941(3) 0.143(14) Uani 0.50 1 d P . . O9 O 0.0461(12) 0.104(3) 0.466(2) 0.147(17) Uani 0.50 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru2 0.0365(8) 0.0687(10) 0.0525(8) -0.0011(6) 0.0186(6) -0.0059(6) Er1 0.0489(7) 0.0670(8) 0.0528(7) 0.000 0.0261(5) 0.000 K1 0.066(5) 0.086(6) 0.080(6) -0.004(5) 0.034(4) -0.001(4) C4 0.054(10) 0.074(12) 0.069(12) -0.018(9) 0.030(9) -0.014(9) C5 0.059(10) 0.053(10) 0.045(9) 0.002(7) 0.022(8) 0.004(8) C6 0.057(11) 0.053(10) 0.069(12) 0.003(9) 0.019(9) -0.007(8) C7 0.053(10) 0.055(11) 0.064(11) -0.015(8) 0.018(9) 0.004(8) C8 0.061(11) 0.060(11) 0.070(12) 0.004(9) 0.015(9) -0.005(9) C9 0.036(9) 0.054(10) 0.058(10) -0.002(8) 0.011(7) 0.000(7) C10 0.049(11) 0.107(16) 0.053(11) 0.012(10) 0.029(9) -0.012(10) C11 0.029(8) 0.084(13) 0.099(14) -0.004(11) 0.029(9) 0.004(8) C12 0.044(9) 0.049(9) 0.054(10) -0.006(7) 0.028(7) -0.010(7) C13 0.058(12) 0.098(17) 0.057(11) -0.026(11) 0.007(9) -0.009(11) C14 0.055(11) 0.075(13) 0.078(12) 0.010(11) 0.045(10) -0.005(10) C15 0.060(10) 0.063(11) 0.060(10) -0.003(8) 0.027(9) -0.014(9) C16 0.079(13) 0.055(11) 0.058(10) -0.006(8) 0.036(9) -0.004(9) C17 0.073(14) 0.071(14) 0.14(2) -0.015(13) 0.015(14) 0.015(11) C18 0.039(9) 0.049(10) 0.069(11) 0.003(8) 0.020(8) -0.001(7) C19 0.062(12) 0.088(15) 0.071(13) 0.010(11) 0.010(10) -0.017(10) C20 0.063(12) 0.059(11) 0.059(11) 0.002(9) 0.013(9) 0.000(9) C22 0.064(12) 0.061(11) 0.073(12) 0.006(9) 0.039(10) 0.005(9) N1 0.051(8) 0.054(8) 0.081(10) -0.020(7) 0.038(7) -0.012(6) N2 0.044(8) 0.075(10) 0.051(8) -0.015(7) 0.021(6) -0.004(7) N3 0.066(11) 0.106(15) 0.126(16) 0.024(13) 0.049(11) 0.010(11) N4 0.053(8) 0.080(11) 0.062(9) -0.009(8) 0.032(7) -0.026(7) N6 0.049(9) 0.148(17) 0.070(11) 0.027(11) 0.022(8) -0.014(10) N8 0.051(8) 0.057(9) 0.055(8) -0.004(7) 0.021(7) -0.006(6) N12 0.094(15) 0.137(19) 0.086(13) -0.001(13) 0.034(11) -0.028(14) O1 0.061(7) 0.075(8) 0.072(8) -0.013(6) 0.016(6) 0.009(6) O2 0.059(15) 0.049(14) 0.15(3) 0.032(15) 0.041(16) 0.048(12) O3 0.052(16) 0.12(3) 0.10(2) 0.028(19) 0.041(15) -0.005(16) O4 0.15(3) 0.10(2) 0.072(18) -0.044(16) 0.057(18) -0.04(2) O5 0.064(18) 0.14(3) 0.09(2) 0.038(19) 0.026(15) -0.003(17) O6 0.19(3) 0.068(19) 0.20(3) -0.03(2) 0.17(3) -0.02(2) O7 0.12(3) 0.10(3) 0.067(19) 0.005(16) 0.016(18) 0.04(2) O8 0.16(3) 0.06(2) 0.21(4) -0.03(2) 0.06(3) -0.01(2) O9 0.09(2) 0.21(4) 0.15(3) -0.11(3) 0.06(2) -0.06(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru2 C13 1.94(2) . ? Ru2 C10 1.93(2) . ? Ru2 C14 1.95(2) . ? Ru2 C7 1.964(17) . ? Ru2 N2 2.104(12) . ? Ru2 N8 2.129(14) . ? Ru2 K1 4.046(9) 5_565 ? Er1 N4 2.365(12) 2 ? Er1 N4 2.365(12) . ? Er1 N6 2.370(18) 5_565 ? Er1 N6 2.370(18) 6_566 ? Er1 O1 2.374(12) 2 ? Er1 O1 2.374(12) . ? Er1 O3 2.44(3) 2 ? Er1 O3 2.44(3) . ? Er1 O7 2.51(3) . ? Er1 O7 2.51(3) 2 ? Er1 K1 4.115(9) 2 ? Er1 K1 4.115(9) . ? K1 O4 2.39(4) . ? K1 O3 2.90(3) . ? K1 O7 2.90(3) . ? K1 N4 3.019(18) . ? K1 N6 3.054(18) . ? K1 N4 3.129(16) 5_565 ? K1 C7 3.175(19) 5_565 ? K1 N6 3.208(19) 5_565 ? K1 C10 3.235(18) . ? K1 C7 3.235(19) . ? K1 C10 3.25(2) 5_565 ? K1 K1 3.288(18) 5_565 ? C4 C22 1.37(2) . ? C4 C12 1.36(2) . ? C5 C15 1.37(2) . ? C5 N2 1.391(18) . ? C5 C12 1.39(2) . ? C6 N8 1.35(2) . ? C6 C20 1.37(2) . ? C7 N4 1.18(2) . ? C7 K1 3.175(19) 5_565 ? C8 C18 1.40(2) . ? C8 C19 1.41(2) . ? C9 N2 1.311(18) . ? C9 N1 1.387(18) . ? C9 C18 1.48(2) . ? C10 N6 1.19(2) . ? C10 K1 3.25(2) 5_565 ? C11 N1 1.45(2) . ? C11 C17 1.53(2) . ? C12 N1 1.37(2) . ? C13 N12 1.22(3) . ? C13 K1 3.52(2) 5_565 ? C14 N3 1.19(2) . ? C15 C16 1.40(2) . ? C16 C22 1.36(2) . ? C18 N8 1.326(19) . ? C19 C20 1.35(2) . ? N4 K1 3.129(16) 5_565 ? N6 Er1 2.370(18) 5_565 ? N6 K1 3.208(19) 5_565 ? 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 C13 Ru2 C10 89.6(8) . . ? C13 Ru2 C14 178.4(8) . . ? C10 Ru2 C14 88.8(8) . . ? C13 Ru2 C7 91.3(8) . . ? C10 Ru2 C7 87.4(7) . . ? C14 Ru2 C7 88.9(6) . . ? C13 Ru2 N2 86.7(7) . . ? C10 Ru2 N2 100.9(6) . . ? C14 Ru2 N2 93.3(6) . . ? C7 Ru2 N2 171.4(6) . . ? C13 Ru2 N8 90.8(7) . . ? C10 Ru2 N8 176.4(6) . . ? C14 Ru2 N8 90.8(7) . . ? C7 Ru2 N8 96.2(6) . . ? N2 Ru2 N8 75.5(5) . . ? C13 Ru2 K1 60.4(6) . 5_565 ? C10 Ru2 K1 52.4(6) . 5_565 ? C14 Ru2 K1 118.8(5) . 5_565 ? C7 Ru2 K1 50.3(5) . 5_565 ? N2 Ru2 K1 134.2(4) . 5_565 ? N8 Ru2 K1 130.6(4) . 5_565 ? N4 Er1 N4 143.9(7) 2 . ? N4 Er1 N6 108.4(5) 2 5_565 ? N4 Er1 N6 81.9(5) . 5_565 ? N4 Er1 N6 81.9(5) 2 6_566 ? N4 Er1 N6 108.4(5) . 6_566 ? N6 Er1 N6 147.4(10) 5_565 6_566 ? N4 Er1 O1 74.1(5) 2 2 ? N4 Er1 O1 140.7(5) . 2 ? N6 Er1 O1 72.8(5) 5_565 2 ? N6 Er1 O1 81.0(6) 6_566 2 ? N4 Er1 O1 140.7(5) 2 . ? N4 Er1 O1 74.1(5) . . ? N6 Er1 O1 81.0(6) 5_565 . ? N6 Er1 O1 72.8(5) 6_566 . ? O1 Er1 O1 72.7(6) 2 . ? N4 Er1 O3 71.9(7) 2 2 ? N4 Er1 O3 75.2(7) . 2 ? N6 Er1 O3 129.9(9) 5_565 2 ? N6 Er1 O3 82.6(9) 6_566 2 ? O1 Er1 O3 143.9(7) 2 2 ? O1 Er1 O3 131.5(7) . 2 ? N4 Er1 O3 75.2(7) 2 . ? N4 Er1 O3 71.9(7) . . ? N6 Er1 O3 82.6(9) 5_565 . ? N6 Er1 O3 129.9(9) 6_566 . ? O1 Er1 O3 131.5(7) 2 . ? O1 Er1 O3 143.9(7) . . ? O3 Er1 O3 48.1(16) 2 . ? N4 Er1 O7 69.4(8) 2 . ? N4 Er1 O7 87.1(9) . . ? N6 Er1 O7 61.8(9) 5_565 . ? N6 Er1 O7 146.7(8) 6_566 . ? O1 Er1 O7 105.8(10) 2 . ? O1 Er1 O7 140.5(7) . . ? O3 Er1 O7 72.9(13) 2 . ? O3 Er1 O7 27.1(9) . . ? N4 Er1 O7 87.1(9) 2 2 ? N4 Er1 O7 69.4(8) . 2 ? N6 Er1 O7 146.7(8) 5_565 2 ? N6 Er1 O7 61.8(9) 6_566 2 ? O1 Er1 O7 140.5(7) 2 2 ? O1 Er1 O7 105.8(10) . 2 ? O3 Er1 O7 27.1(9) 2 2 ? O3 Er1 O7 72.9(13) . 2 ? O7 Er1 O7 99.2(18) . 2 ? N4 Er1 K1 46.5(4) 2 2 ? N4 Er1 K1 113.3(3) . 2 ? N6 Er1 K1 153.3(5) 5_565 2 ? N6 Er1 K1 51.1(4) 6_566 2 ? O1 Er1 K1 102.2(3) 2 2 ? O1 Er1 K1 123.3(3) . 2 ? O3 Er1 K1 43.8(7) 2 2 ? O3 Er1 K1 81.9(8) . 2 ? O7 Er1 K1 96.0(7) . 2 ? O7 Er1 K1 44.2(7) 2 2 ? N4 Er1 K1 113.3(3) 2 . ? N4 Er1 K1 46.5(4) . . ? N6 Er1 K1 51.1(4) 5_565 . ? N6 Er1 K1 153.3(5) 6_566 . ? O1 Er1 K1 123.3(3) 2 . ? O1 Er1 K1 102.2(3) . . ? O3 Er1 K1 81.9(8) 2 . ? O3 Er1 K1 43.8(7) . . ? O7 Er1 K1 44.2(7) . . ? O7 Er1 K1 96.0(7) 2 . ? K1 Er1 K1 123.6(3) 2 . ? O4 K1 O3 109.0(9) . . ? O4 K1 O7 102.5(9) . . ? O3 K1 O7 23.1(7) . . ? O4 K1 N4 161.7(7) . . ? O3 K1 N4 56.9(6) . . ? O7 K1 N4 69.1(7) . . ? O4 K1 N6 100.0(8) . . ? O3 K1 N6 142.2(7) . . ? O7 K1 N6 157.5(8) . . ? N4 K1 N6 88.9(5) . . ? O4 K1 N4 82.9(7) . 5_565 ? O3 K1 N4 145.4(7) . 5_565 ? O7 K1 N4 124.2(8) . 5_565 ? N4 K1 N4 115.4(4) . 5_565 ? N6 K1 N4 60.2(4) . 5_565 ? O4 K1 C7 82.5(7) . 5_565 ? O3 K1 C7 125.3(7) . 5_565 ? O7 K1 C7 103.1(9) . 5_565 ? N4 K1 C7 114.9(5) . 5_565 ? N6 K1 C7 81.3(5) . 5_565 ? N4 K1 C7 21.5(4) 5_565 5_565 ? O4 K1 N6 127.4(8) . 5_565 ? O3 K1 N6 62.4(8) . 5_565 ? O7 K1 N6 48.2(7) . 5_565 ? N4 K1 N6 59.7(4) . 5_565 ? N6 K1 N6 116.7(4) . 5_565 ? N4 K1 N6 84.3(5) 5_565 5_565 ? C7 K1 N6 68.5(5) 5_565 5_565 ? O4 K1 C10 115.3(8) . . ? O3 K1 C10 120.7(7) . . ? O7 K1 C10 138.5(8) . . ? N4 K1 C10 69.7(5) . . ? N6 K1 C10 21.5(4) . . ? N4 K1 C10 78.7(5) 5_565 . ? C7 K1 C10 98.3(5) 5_565 . ? N6 K1 C10 111.7(5) 5_565 . ? O4 K1 C7 153.4(8) . . ? O3 K1 C7 73.7(6) . . ? O7 K1 C7 89.3(7) . . ? N4 K1 C7 21.4(4) . . ? N6 K1 C7 69.6(5) . . ? N4 K1 C7 110.2(5) 5_565 . ? C7 K1 C7 118.3(4) 5_565 . ? N6 K1 C7 78.1(5) 5_565 . ? C10 K1 C7 49.2(5) . . ? O4 K1 C10 109.7(8) . 5_565 ? O3 K1 C10 77.2(7) . 5_565 ? O7 K1 C10 57.6(8) . 5_565 ? N4 K1 C10 80.1(5) . 5_565 ? N6 K1 C10 115.5(6) . 5_565 ? N4 K1 C10 68.2(4) 5_565 5_565 ? C7 K1 C10 49.6(5) 5_565 5_565 ? N6 K1 C10 21.2(4) 5_565 5_565 ? C10 K1 C10 119.1(4) . 5_565 ? C7 K1 C10 96.8(5) . 5_565 ? O4 K1 K1 138.9(8) . 5_565 ? O3 K1 K1 106.4(7) . 5_565 ? O7 K1 K1 102.0(7) . 5_565 ? N4 K1 K1 59.3(4) . 5_565 ? N6 K1 K1 60.6(4) . 5_565 ? N4 K1 K1 56.1(4) 5_565 5_565 ? C7 K1 K1 60.0(4) 5_565 5_565 ? N6 K1 K1 56.1(4) 5_565 5_565 ? C10 K1 K1 59.8(4) . 5_565 ? C7 K1 K1 58.3(4) . 5_565 ? C10 K1 K1 59.3(4) 5_565 5_565 ? C22 C4 C12 117.2(16) . . ? C15 C5 N2 129.3(15) . . ? C15 C5 C12 120.6(14) . . ? N2 C5 C12 109.8(14) . . ? N8 C6 C20 124.7(16) . . ? N4 C7 Ru2 176.8(16) . . ? N4 C7 K1 77.0(11) . 5_565 ? Ru2 C7 K1 101.2(6) . 5_565 ? N4 C7 K1 68.9(11) . . ? Ru2 C7 K1 107.9(7) . . ? K1 C7 K1 61.7(4) 5_565 . ? C18 C8 C19 118.0(17) . . ? N2 C9 N1 112.1(14) . . ? N2 C9 C18 117.4(13) . . ? N1 C9 C18 130.5(14) . . ? N6 C10 Ru2 176.8(19) . . ? N6 C10 K1 70.6(11) . . ? Ru2 C10 K1 108.7(7) . . ? N6 C10 K1 77.4(13) . 5_565 ? Ru2 C10 K1 99.5(7) . 5_565 ? K1 C10 K1 60.9(4) . 5_565 ? N1 C11 C17 112.9(15) . . ? N1 C12 C4 132.0(15) . . ? N1 C12 C5 106.1(12) . . ? C4 C12 C5 121.8(16) . . ? N12 C13 Ru2 176.9(19) . . ? N12 C13 K1 86.5(14) . 5_565 ? Ru2 C13 K1 91.0(7) . 5_565 ? N3 C14 Ru2 176.9(16) . . ? C5 C15 C16 117.4(16) . . ? C22 C16 C15 119.9(17) . . ? N8 C18 C8 121.8(15) . . ? N8 C18 C9 112.4(14) . . ? C8 C18 C9 125.7(14) . . ? C20 C19 C8 120.3(18) . . ? C19 C20 C6 117.3(18) . . ? C16 C22 C4 123.0(16) . . ? C12 N1 C9 106.6(13) . . ? C12 N1 C11 124.5(13) . . ? C9 N1 C11 128.7(15) . . ? C9 N2 C5 105.2(13) . . ? C9 N2 Ru2 116.5(10) . . ? C5 N2 Ru2 138.0(11) . . ? C7 N4 Er1 171.2(15) . . ? C7 N4 K1 89.7(12) . . ? Er1 N4 K1 98.9(5) . . ? C7 N4 K1 81.4(11) . 5_565 ? Er1 N4 K1 103.6(5) . 5_565 ? K1 N4 K1 64.6(4) . 5_565 ? C10 N6 Er1 161.9(18) . 5_565 ? C10 N6 K1 87.8(12) . . ? Er1 N6 K1 105.7(6) 5_565 . ? C10 N6 K1 81.3(13) . 5_565 ? Er1 N6 K1 93.8(6) 5_565 5_565 ? K1 N6 K1 63.3(4) . 5_565 ? C18 N8 C6 117.8(15) . . ? C18 N8 Ru2 117.8(11) . . ? C6 N8 Ru2 124.4(11) . . ? Er1 O3 K1 100.5(11) . . ? Er1 O7 K1 98.7(10) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.877 _refine_diff_density_min -1.897 _refine_diff_density_rms 0.245 #===END data_imw123m _database_code_depnum_ccdc_archive 'CCDC 276248' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H70 Eu2 K2 N28 O21 Ru4' _chemical_formula_weight 2161.72 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' K K 0.2009 0.2494 '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' Eu Eu -0.1578 3.6682 '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 14.0042(16) _cell_length_b 16.3639(19) _cell_length_c 18.520(2) _cell_angle_alpha 113.599(2) _cell_angle_beta 103.578(2) _cell_angle_gamma 91.274(2) _cell_volume 3748.2(7) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 6381 _cell_measurement_theta_min 4.333 _cell_measurement_theta_max 55.020 _exptl_crystal_description Block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.915 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2124 _exptl_absorpt_coefficient_mu 2.630 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4047 _exptl_absorpt_correction_T_max 0.6783 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker smart1000' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 100 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 42204 _diffrn_reflns_av_R_equivalents 0.0360 _diffrn_reflns_av_sigmaI/netI 0.0469 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.24 _diffrn_reflns_theta_max 27.54 _reflns_number_total 16650 _reflns_number_gt 13752 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker smart' _computing_cell_refinement 'Bruker smart' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0313P)^2^+15.7530P] 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 16650 _refine_ls_number_parameters 946 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0512 _refine_ls_R_factor_gt 0.0396 _refine_ls_wR_factor_ref 0.0952 _refine_ls_wR_factor_gt 0.0907 _refine_ls_goodness_of_fit_ref 1.102 _refine_ls_restrained_S_all 1.102 _refine_ls_shift/su_max 0.032 _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 Eu1 Eu 0.475171(18) 0.694456(16) 0.454203(15) 0.01479(6) Uani 1 1 d . . . Eu2 Eu 0.535154(18) 0.251561(16) 0.061549(15) 0.01396(6) Uani 1 1 d . . . Ru1 Ru 0.75015(3) 0.85392(3) 0.35926(2) 0.01302(8) Uani 1 1 d . . . Ru2 Ru 0.76315(3) 0.33877(3) 0.37120(2) 0.01315(8) Uani 1 1 d . . . Ru3 Ru 0.25654(3) 0.48141(3) 0.14606(2) 0.01335(8) Uani 1 1 d . . . Ru4 Ru 0.75802(3) 0.05022(3) -0.12752(2) 0.01581(9) Uani 1 1 d . . . N1 N 0.8622(3) 0.8523(3) 0.4599(3) 0.0169(9) Uani 1 1 d . . . N2 N 0.9109(3) 0.9250(3) 0.2918(3) 0.0196(9) Uani 1 1 d . . . H2N H 0.8695 0.9324 0.2517 0.024 Uiso 1 1 calc R . . N3 N 0.8832(3) 0.9043(3) 0.3476(3) 0.0170(9) Uani 1 1 d . . . N4 N 0.6953(4) 1.0466(3) 0.4612(3) 0.0272(11) Uani 1 1 d . . . N5 N 0.7876(3) 0.6644(3) 0.2344(3) 0.0235(10) Uani 1 1 d . . . N6 N 0.6018(3) 0.8665(3) 0.2100(3) 0.0262(10) Uani 1 1 d . . . N7 N 0.5837(3) 0.7639(3) 0.4012(3) 0.0258(10) Uani 1 1 d . . . N8 N 0.8833(3) 0.3434(3) 0.4699(3) 0.0158(8) Uani 1 1 d . . . N9 N 0.9079(3) 0.4195(3) 0.2969(3) 0.0179(9) Uani 1 1 d . . . H9N H 0.8623 0.4239 0.2573 0.021 Uiso 1 1 calc R . . N10 N 0.8887(3) 0.3943(3) 0.3534(2) 0.0157(8) Uani 1 1 d . . . N11 N 0.7790(4) 0.1413(3) 0.2459(3) 0.0276(11) Uani 1 1 d . . . N12 N 0.7040(3) 0.5221(3) 0.4867(3) 0.0222(10) Uani 1 1 d . . . N13 N 0.6092(3) 0.2600(3) 0.4325(3) 0.0187(9) Uani 1 1 d . . . N14 N 0.6189(3) 0.3302(3) 0.2107(3) 0.0192(9) Uani 1 1 d . . . N15 N 0.1558(3) 0.3788(3) 0.0399(3) 0.0177(9) Uani 1 1 d . . . N16 N 0.0807(3) 0.5921(3) 0.2017(3) 0.0202(9) Uani 1 1 d . . . H16N H 0.1175 0.6372 0.2455 0.024 Uiso 1 1 calc R . . N17 N 0.1165(3) 0.5245(3) 0.1503(3) 0.0187(9) Uani 1 1 d . . . N18 N 0.2447(4) 0.3890(3) 0.2669(3) 0.0257(10) Uani 1 1 d . . . N19 N 0.2914(3) 0.5906(3) 0.0435(3) 0.0270(10) Uani 1 1 d . . . N20 N 0.4387(3) 0.3795(3) 0.1126(3) 0.0215(9) Uani 1 1 d . . . N21 N 0.3846(3) 0.6399(3) 0.3061(3) 0.0176(9) Uani 1 1 d . . . N22 N 0.8800(3) 0.1339(3) -0.0276(3) 0.0197(9) Uani 1 1 d . . . N23 N 0.8981(3) -0.0941(3) -0.2090(3) 0.0223(10) Uani 1 1 d . . . H23N H 0.8518 -0.1334 -0.2504 0.027 Uiso 1 1 calc R . . N24 N 0.8811(3) -0.0187(3) -0.1508(3) 0.0191(9) Uani 1 1 d . . . N25 N 0.7101(4) -0.0480(4) -0.0210(3) 0.0328(12) Uani 1 1 d . . . N26 N 0.7774(4) 0.1428(3) -0.2466(3) 0.0310(11) Uani 1 1 d . . . N27 N 0.6080(3) 0.1765(3) -0.0560(3) 0.0206(9) Uani 1 1 d . . . N28 N 0.5884(4) -0.0823(4) -0.2765(3) 0.0365(13) Uani 1 1 d . . . O1 O 0.3953(3) 0.8183(3) 0.4451(3) 0.0317(10) Uani 1 1 d . . . H1A H 0.4218 0.8484 0.4247 0.038 Uiso 1 1 d R . . H1B H 0.3406 0.8361 0.4506 0.038 Uiso 1 1 d R . . O2 O 0.5954(3) 0.8106(3) 0.5692(2) 0.0352(10) Uani 1 1 d . . . H2A H 0.5913 0.8163 0.6155 0.042 Uiso 1 1 d R . . H2B H 0.6163 0.8628 0.5737 0.042 Uiso 1 1 d R . . O3 O 0.5512(3) 0.6271(3) 0.5456(2) 0.0334(10) Uani 1 1 d . . . H3A H 0.6140 0.6266 0.5544 0.040 Uiso 1 1 d R . . H3B H 0.5354 0.6301 0.5876 0.040 Uiso 1 1 d R . . O4 O 0.5552(3) 0.5723(3) 0.3861(3) 0.0359(10) Uani 1 1 d . . . H4A H 0.5357 0.5224 0.3858 0.043 Uiso 1 1 d R . . H4B H 0.5916 0.5612 0.3533 0.043 Uiso 1 1 d R . . O5 O 0.3419(3) 0.5736(2) 0.4160(2) 0.0277(9) Uani 1 1 d . . . H5A H 0.3033 0.5476 0.3644 0.033 Uiso 1 1 d R . . H5B H 0.3316 0.5549 0.4535 0.033 Uiso 1 1 d R . . O6 N 0.4389(3) 0.2022(3) 0.1364(2) 0.0141(8) Uani 1 1 d . . . H6A1 H 0.4845 0.1964 0.1826 0.017 Uiso 1 1 d R . . H6A3 H 0.3951 0.2468 0.1566 0.017 Uiso 1 1 d R . . O7 O 0.4423(3) 0.1063(3) -0.0222(3) 0.0351(10) Uani 1 1 d . . . H7AA H 0.3964 0.0986 -0.0016 0.042 Uiso 1 1 d R . . H7AB H 0.4169 0.1027 -0.0699 0.042 Uiso 1 1 d R . . O8 O 0.6505(3) 0.1512(2) 0.0971(2) 0.0235(8) Uani 1 1 d . . . H8AB H 0.6314 0.0973 0.0620 0.028 Uiso 1 1 d R . . H8AC H 0.7086 0.1674 0.0970 0.028 Uiso 1 1 d R . . O9 O 0.6615(3) 0.3556(3) 0.0704(2) 0.0273(9) Uani 1 1 d . . . H9A H 0.7024 0.3881 0.1155 0.033 Uiso 1 1 d R . . H9B H 0.6765 0.3671 0.0332 0.033 Uiso 1 1 d R . . O10 O 0.4302(4) 0.2668(3) -0.0505(2) 0.0435(12) Uani 1 1 d . . . H10A H 0.3691 0.2711 -0.0573 0.052 Uiso 1 1 d R . . H10B H 0.4523 0.2904 -0.0778 0.052 Uiso 1 1 d R . . O11 O 0.5308(3) 0.0383(3) 0.1490(2) 0.0274(9) Uani 1 1 d . . . H11A H 0.4587 0.0266 0.1379 0.033 Uiso 1 1 d R . . H11C H 0.5475 0.0904 0.1388 0.033 Uiso 1 1 d R . . O12 O 0.4671(3) 0.9154(3) 0.3708(3) 0.0462(12) Uani 1 1 d . . . H12A H 0.5304 0.9498 0.3802 0.055 Uiso 1 1 d R . . H12C H 0.4153 0.9550 0.3754 0.055 Uiso 1 1 d R . . O13 O 0.5073(4) 0.6244(3) 0.1525(3) 0.0511(13) Uani 1 1 d . . . H13A H 0.4740 0.5759 0.1077 0.061 Uiso 1 1 d R . . H13B H 0.5706 0.6236 0.1773 0.061 Uiso 1 1 d R . . O14 O 0.5844(3) 0.5314(3) 0.2418(3) 0.0323(9) Uani 1 1 d . . . O15 O 0.7633(3) 0.4879(2) 0.2153(2) 0.0217(8) Uani 1 1 d . . . O16 O 0.4433(3) 0.3367(3) 0.2916(3) 0.0315(9) Uani 1 1 d . . . O17 O 0.1927(3) 0.7454(3) 0.3236(3) 0.0296(9) Uani 1 1 d . . . O18 O 0.7726(3) 0.7532(3) 0.6738(3) 0.0360(10) Uani 1 1 d . . . O19 O 0.3160(3) 0.0213(3) 0.4061(3) 0.0357(10) Uani 1 1 d . . . O20 O 0.7702(3) 0.9507(3) 0.1753(3) 0.0312(9) Uani 1 1 d . . . O21 O 0.3424(3) 0.4049(3) 0.9243(3) 0.0354(10) Uani 1 1 d . . . K1 K 0.61772(10) 0.07312(9) 0.30881(8) 0.0309(3) Uani 1 1 d . . . K2 K 0.41746(12) 0.77423(11) 0.21308(12) 0.0482(4) Uani 1 1 d . . . C1 C 0.8465(4) 0.8293(4) 0.5182(3) 0.0226(11) Uani 1 1 d . . . H1 H 0.7804 0.8115 0.5158 0.027 Uiso 1 1 calc R . . C2 C 0.9223(5) 0.8305(4) 0.5818(3) 0.0276(13) Uani 1 1 d . . . H2 H 0.9083 0.8130 0.6218 0.033 Uiso 1 1 calc R . . C3 C 1.0186(4) 0.8572(4) 0.5865(3) 0.0275(13) Uani 1 1 d . . . H3 H 1.0718 0.8597 0.6303 0.033 Uiso 1 1 calc R . . C4 C 1.0361(4) 0.8802(3) 0.5265(3) 0.0242(12) Uani 1 1 d . . . H4 H 1.1017 0.8980 0.5279 0.029 Uiso 1 1 calc R . . C5 C 0.9564(4) 0.8770(3) 0.4637(3) 0.0195(11) Uani 1 1 d . . . C6 C 0.9674(4) 0.9001(3) 0.3975(3) 0.0191(11) Uani 1 1 d . . . C7 C 1.0499(4) 0.9178(4) 0.3727(4) 0.0255(12) Uani 1 1 d . . . H7 H 1.1178 0.9190 0.3975 0.031 Uiso 1 1 calc R . . C8 C 1.0105(4) 0.9329(3) 0.3048(3) 0.0236(12) Uani 1 1 d . . . H8 H 1.0466 0.9466 0.2727 0.028 Uiso 1 1 calc R . . C9 C 0.7201(4) 0.9779(4) 0.4281(3) 0.0179(10) Uani 1 1 d . . . C10 C 0.7742(4) 0.7314(3) 0.2820(3) 0.0172(10) Uani 1 1 d . . . C11 C 0.6570(4) 0.8606(3) 0.2647(3) 0.0161(10) Uani 1 1 d . . . C12 C 0.6429(4) 0.7972(3) 0.3836(3) 0.0181(10) Uani 1 1 d . . . C13 C 0.8770(4) 0.3220(3) 0.5317(3) 0.0197(11) Uani 1 1 d . . . H13 H 0.8135 0.3025 0.5334 0.024 Uiso 1 1 calc R . . C14 C 0.9585(4) 0.3271(3) 0.5926(3) 0.0219(11) Uani 1 1 d . . . H14 H 0.9509 0.3112 0.6351 0.026 Uiso 1 1 calc R . . C15 C 1.0520(4) 0.3558(3) 0.5911(3) 0.0250(12) Uani 1 1 d . . . H15 H 1.1092 0.3595 0.6324 0.030 Uiso 1 1 calc R . . C16 C 1.0598(4) 0.3786(3) 0.5290(3) 0.0205(11) Uani 1 1 d . . . H16 H 1.1227 0.3990 0.5269 0.025 Uiso 1 1 calc R . . C17 C 0.9755(4) 0.3716(3) 0.4695(3) 0.0184(10) Uani 1 1 d . . . C18 C 0.9769(3) 0.3947(3) 0.4013(3) 0.0153(10) Uani 1 1 d . . . C19 C 1.0530(4) 0.4206(3) 0.3744(3) 0.0221(11) Uani 1 1 d . . . H19 H 1.1223 0.4257 0.3970 0.027 Uiso 1 1 calc R . . C20 C 1.0064(4) 0.4371(3) 0.3090(3) 0.0216(11) Uani 1 1 d . . . H20 H 1.0376 0.4572 0.2777 0.026 Uiso 1 1 calc R . . C21 C 0.7806(4) 0.2131(3) 0.2944(3) 0.0160(10) Uani 1 1 d . . . C22 C 0.7308(4) 0.4589(3) 0.4434(3) 0.0172(10) Uani 1 1 d . . . C23 C 0.6625(4) 0.2869(3) 0.4052(3) 0.0164(10) Uani 1 1 d . . . C24 C 0.6682(3) 0.3366(3) 0.2728(3) 0.0150(10) Uani 1 1 d . . . C25 C 0.1799(4) 0.3071(4) -0.0167(3) 0.0229(11) Uani 1 1 d . . . H25 H 0.2474 0.2971 -0.0087 0.027 Uiso 1 1 calc R . . C26 C 0.1120(5) 0.2471(4) -0.0860(3) 0.0296(13) Uani 1 1 d . . . H26 H 0.1325 0.1972 -0.1247 0.036 Uiso 1 1 calc R . . C27 C 0.0137(4) 0.2607(4) -0.0984(4) 0.0294(13) Uani 1 1 d . . . H27 H -0.0345 0.2208 -0.1462 0.035 Uiso 1 1 calc R . . C28 C -0.0132(4) 0.3330(4) -0.0402(3) 0.0258(12) Uani 1 1 d . . . H28 H -0.0807 0.3431 -0.0468 0.031 Uiso 1 1 calc R . . C29 C 0.0587(4) 0.3909(3) 0.0281(3) 0.0199(11) Uani 1 1 d . . . C30 C 0.0378(4) 0.4696(4) 0.0920(3) 0.0199(11) Uani 1 1 d . . . C31 C -0.0500(4) 0.5046(4) 0.1082(4) 0.0269(12) Uani 1 1 d . . . H31 H -0.1162 0.4794 0.0772 0.032 Uiso 1 1 calc R . . C32 C -0.0193(4) 0.5824(4) 0.1779(4) 0.0284(13) Uani 1 1 d . . . H32 H -0.0608 0.6223 0.2047 0.034 Uiso 1 1 calc R . . C33 C 0.2444(4) 0.4189(3) 0.2200(3) 0.0175(10) Uani 1 1 d . . . C34 C 0.2761(4) 0.5498(3) 0.0788(3) 0.0180(10) Uani 1 1 d . . . C35 C 0.3735(4) 0.4202(3) 0.1264(3) 0.0173(10) Uani 1 1 d . . . C36 C 0.3381(3) 0.5824(3) 0.2455(3) 0.0154(10) Uani 1 1 d . . . C37 C 0.8748(4) 0.2082(4) 0.0368(3) 0.0254(12) Uani 1 1 d . . . H37 H 0.8123 0.2290 0.0385 0.031 Uiso 1 1 calc R . . C38 C 0.9559(5) 0.2555(4) 0.1005(4) 0.0306(13) Uani 1 1 d . . . H38 H 0.9489 0.3074 0.1456 0.037 Uiso 1 1 calc R . . C39 C 1.0479(5) 0.2271(4) 0.0986(4) 0.0336(14) Uani 1 1 d . . . H39 H 1.1049 0.2598 0.1419 0.040 Uiso 1 1 calc R . . C40 C 1.0560(4) 0.1510(4) 0.0333(4) 0.0274(12) Uani 1 1 d . . . H40 H 1.1183 0.1299 0.0309 0.033 Uiso 1 1 calc R . . C41 C 0.9710(4) 0.1053(4) -0.0293(3) 0.0217(11) Uani 1 1 d . . . C42 C 0.9698(4) 0.0226(4) -0.0998(3) 0.0211(11) Uani 1 1 d . . . C43 C 1.0451(4) -0.0269(4) -0.1262(4) 0.0270(12) Uani 1 1 d . . . H43 H 1.1144 -0.0124 -0.1016 0.032 Uiso 1 1 calc R . . C44 C 0.9962(4) -0.1010(4) -0.1953(4) 0.0271(12) Uani 1 1 d . . . H44 H 1.0261 -0.1487 -0.2277 0.033 Uiso 1 1 calc R . . C45 C 0.7310(4) -0.0139(4) -0.0596(3) 0.0208(11) Uani 1 1 d . . . C46 C 0.7750(4) 0.1125(4) -0.2001(3) 0.0203(11) Uani 1 1 d . . . C47 C 0.6526(4) -0.0347(4) -0.2221(3) 0.0228(11) Uani 1 1 d . . . C48 C 0.6612(4) 0.1296(3) -0.0865(3) 0.0178(10) 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 Eu1 0.01517(12) 0.01537(12) 0.01207(12) 0.00335(10) 0.00485(9) 0.00072(9) Eu2 0.01436(12) 0.01541(12) 0.01098(12) 0.00427(10) 0.00347(9) 0.00253(9) Ru1 0.01267(18) 0.01368(18) 0.01124(19) 0.00356(15) 0.00349(15) 0.00128(14) Ru2 0.01213(18) 0.01582(19) 0.01085(19) 0.00493(15) 0.00306(15) 0.00169(14) Ru3 0.01270(18) 0.01462(19) 0.01124(19) 0.00383(15) 0.00329(15) 0.00205(14) Ru4 0.01368(19) 0.0182(2) 0.01249(19) 0.00293(16) 0.00430(15) 0.00030(15) N1 0.018(2) 0.014(2) 0.016(2) 0.0036(17) 0.0031(17) 0.0043(16) N2 0.022(2) 0.019(2) 0.017(2) 0.0056(18) 0.0070(18) 0.0018(17) N3 0.019(2) 0.013(2) 0.019(2) 0.0059(17) 0.0056(18) 0.0012(16) N4 0.036(3) 0.023(2) 0.024(3) 0.008(2) 0.012(2) 0.011(2) N5 0.026(2) 0.019(2) 0.021(2) 0.004(2) 0.006(2) 0.0066(18) N6 0.026(3) 0.032(3) 0.019(2) 0.010(2) 0.005(2) 0.006(2) N7 0.023(2) 0.031(3) 0.019(2) 0.005(2) 0.0066(19) -0.003(2) N8 0.016(2) 0.015(2) 0.014(2) 0.0053(17) 0.0029(17) 0.0027(16) N9 0.020(2) 0.023(2) 0.013(2) 0.0089(18) 0.0038(17) 0.0014(17) N10 0.018(2) 0.018(2) 0.012(2) 0.0049(17) 0.0070(17) 0.0022(16) N11 0.025(3) 0.027(3) 0.026(3) 0.007(2) 0.003(2) 0.006(2) N12 0.020(2) 0.022(2) 0.022(2) 0.008(2) 0.0050(19) 0.0032(18) N13 0.017(2) 0.021(2) 0.017(2) 0.0056(18) 0.0083(18) 0.0025(17) N14 0.021(2) 0.019(2) 0.016(2) 0.0064(18) 0.0037(18) 0.0032(17) N15 0.018(2) 0.019(2) 0.014(2) 0.0050(18) 0.0031(17) 0.0015(17) N16 0.020(2) 0.023(2) 0.019(2) 0.0066(19) 0.0101(18) 0.0079(18) N17 0.017(2) 0.022(2) 0.020(2) 0.0105(19) 0.0068(18) 0.0044(17) N18 0.028(3) 0.027(3) 0.023(3) 0.012(2) 0.006(2) 0.001(2) N19 0.025(3) 0.035(3) 0.024(3) 0.015(2) 0.006(2) 0.002(2) N20 0.021(2) 0.024(2) 0.018(2) 0.0076(19) 0.0048(18) 0.0081(18) N21 0.019(2) 0.021(2) 0.013(2) 0.0056(18) 0.0081(18) 0.0011(17) N22 0.018(2) 0.021(2) 0.017(2) 0.0059(18) 0.0040(18) -0.0036(17) N23 0.023(2) 0.025(2) 0.017(2) 0.0036(19) 0.0098(19) 0.0049(18) N24 0.018(2) 0.021(2) 0.017(2) 0.0050(18) 0.0073(18) 0.0036(17) N25 0.026(3) 0.043(3) 0.029(3) 0.018(2) 0.002(2) -0.007(2) N26 0.029(3) 0.037(3) 0.031(3) 0.017(2) 0.009(2) 0.004(2) N27 0.022(2) 0.022(2) 0.016(2) 0.0049(19) 0.0069(18) 0.0022(18) N28 0.027(3) 0.050(3) 0.015(2) -0.001(2) 0.003(2) -0.011(2) O1 0.044(3) 0.029(2) 0.034(2) 0.0176(19) 0.022(2) 0.0185(19) O2 0.045(3) 0.033(2) 0.018(2) 0.0011(18) 0.0097(19) -0.0126(19) O3 0.043(3) 0.044(3) 0.021(2) 0.0164(19) 0.0181(19) 0.023(2) O4 0.043(3) 0.040(3) 0.030(2) 0.016(2) 0.018(2) 0.024(2) O5 0.039(2) 0.025(2) 0.0136(19) 0.0037(16) 0.0070(17) -0.0096(17) O6 0.018(2) 0.015(2) 0.0088(19) 0.0026(16) 0.0075(16) -0.0011(16) O7 0.040(3) 0.032(2) 0.022(2) -0.0016(18) 0.0146(19) -0.0136(19) O8 0.026(2) 0.0227(19) 0.019(2) 0.0060(16) 0.0065(16) 0.0074(15) O9 0.036(2) 0.028(2) 0.0133(19) 0.0054(16) 0.0048(17) -0.0122(17) O10 0.060(3) 0.048(3) 0.016(2) 0.009(2) 0.004(2) 0.026(2) O11 0.030(2) 0.027(2) 0.027(2) 0.0122(18) 0.0094(18) 0.0021(17) O12 0.035(3) 0.063(3) 0.062(3) 0.041(3) 0.024(2) 0.020(2) O13 0.043(3) 0.055(3) 0.054(3) 0.025(3) 0.006(2) 0.003(2) O14 0.032(2) 0.035(2) 0.026(2) 0.0055(19) 0.0120(18) 0.0073(18) O15 0.0230(19) 0.0202(19) 0.0198(19) 0.0068(16) 0.0049(16) 0.0006(15) O16 0.026(2) 0.043(2) 0.027(2) 0.015(2) 0.0100(18) 0.0095(18) O17 0.029(2) 0.029(2) 0.032(2) 0.0122(19) 0.0103(18) 0.0021(17) O18 0.033(2) 0.029(2) 0.043(3) 0.017(2) 0.001(2) -0.0022(18) O19 0.043(3) 0.034(2) 0.028(2) 0.0107(19) 0.011(2) 0.002(2) O20 0.034(2) 0.030(2) 0.034(2) 0.0186(19) 0.0067(19) 0.0038(18) O21 0.040(3) 0.039(2) 0.025(2) 0.012(2) 0.0067(19) 0.017(2) K1 0.0385(7) 0.0275(6) 0.0253(7) 0.0104(5) 0.0070(6) 0.0050(5) K2 0.0444(9) 0.0469(9) 0.0690(12) 0.0294(9) 0.0330(8) 0.0164(7) C1 0.024(3) 0.022(3) 0.019(3) 0.006(2) 0.005(2) 0.004(2) C2 0.043(4) 0.023(3) 0.015(3) 0.009(2) 0.003(2) 0.011(2) C3 0.031(3) 0.021(3) 0.019(3) 0.001(2) -0.003(2) 0.008(2) C4 0.022(3) 0.016(3) 0.023(3) 0.000(2) 0.000(2) 0.005(2) C5 0.018(3) 0.014(2) 0.021(3) 0.003(2) 0.002(2) 0.0038(19) C6 0.014(2) 0.015(2) 0.022(3) 0.003(2) 0.001(2) 0.0004(19) C7 0.017(3) 0.024(3) 0.029(3) 0.005(2) 0.005(2) 0.000(2) C8 0.023(3) 0.021(3) 0.026(3) 0.004(2) 0.013(2) 0.002(2) C9 0.014(2) 0.025(3) 0.016(3) 0.011(2) 0.002(2) 0.000(2) C10 0.016(2) 0.018(3) 0.018(3) 0.009(2) 0.005(2) 0.0016(19) C11 0.017(2) 0.015(2) 0.014(2) 0.001(2) 0.009(2) 0.0041(19) C12 0.018(3) 0.021(3) 0.014(2) 0.006(2) 0.004(2) 0.001(2) C13 0.023(3) 0.020(3) 0.015(3) 0.006(2) 0.006(2) 0.002(2) C14 0.031(3) 0.021(3) 0.013(3) 0.007(2) 0.004(2) 0.008(2) C15 0.028(3) 0.017(3) 0.022(3) 0.004(2) -0.003(2) 0.005(2) C16 0.017(3) 0.018(3) 0.021(3) 0.006(2) 0.001(2) 0.003(2) C17 0.019(3) 0.015(2) 0.016(3) 0.001(2) 0.003(2) 0.0043(19) C18 0.013(2) 0.015(2) 0.015(2) 0.004(2) 0.0029(19) 0.0016(18) C19 0.016(3) 0.022(3) 0.026(3) 0.007(2) 0.008(2) 0.003(2) C20 0.024(3) 0.020(3) 0.022(3) 0.008(2) 0.010(2) -0.001(2) C21 0.013(2) 0.022(3) 0.015(2) 0.009(2) 0.0030(19) 0.0034(19) C22 0.014(2) 0.021(3) 0.018(3) 0.010(2) 0.003(2) 0.0020(19) C23 0.018(2) 0.014(2) 0.012(2) 0.0012(19) 0.002(2) 0.0027(19) C24 0.012(2) 0.014(2) 0.017(3) 0.004(2) 0.005(2) -0.0005(18) C25 0.024(3) 0.022(3) 0.021(3) 0.006(2) 0.008(2) 0.002(2) C26 0.038(3) 0.022(3) 0.018(3) -0.002(2) 0.007(2) -0.001(2) C27 0.030(3) 0.029(3) 0.021(3) 0.006(2) -0.001(2) -0.010(2) C28 0.023(3) 0.027(3) 0.022(3) 0.010(2) -0.002(2) -0.006(2) C29 0.020(3) 0.021(3) 0.020(3) 0.011(2) 0.003(2) -0.001(2) C30 0.016(2) 0.026(3) 0.019(3) 0.012(2) 0.002(2) 0.002(2) C31 0.017(3) 0.036(3) 0.033(3) 0.020(3) 0.006(2) 0.007(2) C32 0.023(3) 0.035(3) 0.037(3) 0.019(3) 0.016(3) 0.014(2) C33 0.014(2) 0.016(2) 0.017(3) 0.004(2) 0.0005(19) 0.0001(19) C34 0.013(2) 0.022(3) 0.015(3) 0.005(2) 0.0009(19) 0.0011(19) C35 0.019(3) 0.016(2) 0.011(2) 0.003(2) -0.0010(19) -0.0023(19) C36 0.011(2) 0.024(3) 0.017(3) 0.013(2) 0.0056(19) 0.0048(19) C37 0.026(3) 0.028(3) 0.020(3) 0.007(2) 0.008(2) 0.000(2) C38 0.040(4) 0.022(3) 0.021(3) 0.001(2) 0.007(3) -0.004(2) C39 0.040(4) 0.031(3) 0.020(3) 0.008(3) -0.005(3) -0.011(3) C40 0.023(3) 0.031(3) 0.030(3) 0.018(3) 0.003(2) -0.003(2) C41 0.019(3) 0.025(3) 0.025(3) 0.016(2) 0.004(2) 0.001(2) C42 0.019(3) 0.025(3) 0.025(3) 0.015(2) 0.008(2) 0.002(2) C43 0.018(3) 0.039(3) 0.030(3) 0.018(3) 0.011(2) 0.007(2) C44 0.027(3) 0.035(3) 0.028(3) 0.015(3) 0.019(3) 0.014(2) C45 0.014(2) 0.025(3) 0.017(3) 0.005(2) 0.002(2) -0.002(2) C46 0.014(2) 0.025(3) 0.022(3) 0.009(2) 0.006(2) 0.003(2) C47 0.019(3) 0.031(3) 0.017(3) 0.007(2) 0.009(2) 0.003(2) C48 0.018(3) 0.022(3) 0.012(2) 0.005(2) 0.004(2) -0.001(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Eu1 O4 2.363(4) . ? Eu1 O1 2.382(4) . ? Eu1 O3 2.431(4) . ? Eu1 O2 2.432(4) . ? Eu1 O5 2.448(4) . ? Eu1 N7 2.467(5) . ? Eu1 N21 2.507(4) . ? Eu1 N13 2.511(4) 2_666 ? Eu2 O10 2.351(4) . ? Eu2 O9 2.359(4) . ? Eu2 O7 2.390(4) . ? Eu2 O6 2.473(4) . ? Eu2 O8 2.495(4) . ? Eu2 N14 2.496(4) . ? Eu2 N20 2.498(4) . ? Eu2 N27 2.499(4) . ? Eu2 H7AA 2.7894 . ? Eu2 H7AB 2.7894 . ? Ru1 C11 1.966(5) . ? Ru1 C12 1.977(5) . ? Ru1 C9 2.035(5) . ? Ru1 C10 2.034(5) . ? Ru1 N3 2.112(4) . ? Ru1 N1 2.146(4) . ? Ru2 C23 1.973(5) . ? Ru2 C24 1.974(5) . ? Ru2 C22 2.019(5) . ? Ru2 C21 2.038(5) . ? Ru2 N10 2.114(4) . ? Ru2 N8 2.149(4) . ? Ru3 C35 1.969(5) . ? Ru3 C36 1.980(5) . ? Ru3 C34 2.036(5) . ? Ru3 C33 2.043(5) . ? Ru3 N17 2.107(4) . ? Ru3 N15 2.150(4) . ? Ru4 C48 1.968(5) . ? Ru4 C47 1.981(5) . ? Ru4 C45 2.022(5) . ? Ru4 C46 2.033(5) . ? Ru4 N24 2.115(4) . ? Ru4 N22 2.145(4) . ? N1 C1 1.337(7) . ? N1 C5 1.350(7) . ? N2 N3 1.341(6) . ? N2 C8 1.353(7) . ? N2 H2N 0.8800 . ? N3 C6 1.339(6) . ? N4 C9 1.151(7) . ? N4 K1 2.981(5) 1_565 ? N5 C10 1.153(7) . ? N6 C11 1.161(7) . ? N6 K2 2.986(5) . ? N6 K1 3.107(5) 1_565 ? N7 C12 1.158(7) . ? N8 C13 1.343(6) . ? N8 C17 1.365(7) . ? N9 N10 1.345(6) . ? N9 C20 1.350(7) . ? N9 H9N 0.8800 . ? N10 C18 1.338(6) . ? N11 C21 1.154(7) . ? N11 K1 3.141(5) . ? N12 C22 1.160(7) . ? N13 C23 1.162(6) . ? N13 Eu1 2.511(4) 2_666 ? N13 K1 3.025(4) . ? N14 C24 1.157(6) . ? N15 C25 1.338(7) . ? N15 C29 1.358(7) . ? N16 N17 1.338(6) . ? N16 C32 1.351(7) . ? N16 H16N 0.8800 . ? N17 C30 1.344(7) . ? N18 C33 1.156(7) . ? N19 C34 1.151(7) . ? N19 K2 3.408(5) . ? N20 C35 1.160(7) . ? N21 C36 1.163(6) . ? N21 K2 3.371(4) . ? N22 C37 1.338(7) . ? N22 C41 1.370(7) . ? N23 N24 1.345(6) . ? N23 C44 1.354(7) . ? N23 H23N 0.8800 . ? N24 C42 1.339(7) . ? N25 C45 1.148(7) . ? N26 C46 1.160(7) . ? N26 K2 3.155(5) 2_665 ? N27 C48 1.157(7) . ? N27 K2 3.263(5) 2_665 ? N28 C47 1.160(7) . ? N28 K1 2.827(5) 2_655 ? O1 H1A 0.8533 . ? O1 H1B 0.8399 . ? O2 H2A 0.8406 . ? O2 H2B 0.8607 . ? O3 H3A 0.8564 . ? O3 H3B 0.8413 . ? O4 H4A 0.8533 . ? O4 H4B 0.8506 . ? O5 H5A 0.9000 . ? O5 H5B 0.9001 . ? O6 H6A1 0.9800 . ? O6 H6A3 0.9800 . ? O7 H7AA 0.8500 . ? O7 H7AB 0.8500 . ? O8 H8AB 0.8502 . ? O8 H8AC 0.8501 . ? O9 H9A 0.8454 . ? O9 H9B 0.8497 . ? O10 H10A 0.8438 . ? O10 H10B 0.8510 . ? O11 K1 2.737(4) . ? O11 H11A 0.9800 . ? O11 H11C 0.9800 . ? O12 K2 2.815(6) . ? O12 H12A 0.9800 . ? O12 H12C 0.9801 . ? O13 K2 2.730(5) . ? O13 H13A 0.9000 . ? O13 H13B 0.9001 . ? K1 N28 2.827(5) 2_655 ? K1 N4 2.981(5) 1_545 ? K1 N6 3.107(5) 1_545 ? K1 C23 3.193(5) . ? K1 C9 3.276(5) 1_545 ? K1 C21 3.327(5) . ? K1 C11 3.329(5) 1_545 ? K1 K2 5.004(2) 1_545 ? K2 N26 3.155(5) 2_665 ? K2 N27 3.263(5) 2_665 ? K2 C48 3.318(5) 2_665 ? K2 C46 3.322(5) 2_665 ? K2 C11 3.372(5) . ? K2 K1 5.004(2) 1_565 ? C1 C2 1.381(8) . ? C1 H1 0.9500 . ? C2 C3 1.381(9) . ? C2 H2 0.9500 . ? C3 C4 1.376(8) . ? C3 H3 0.9500 . ? C4 C5 1.392(7) . ? C4 H4 0.9500 . ? C5 C6 1.458(8) . ? C6 C7 1.403(7) . ? C7 C8 1.370(8) . ? C7 H7 0.9500 . ? C8 H8 0.9500 . ? C9 K1 3.276(5) 1_565 ? C11 K1 3.329(5) 1_565 ? C13 C14 1.378(7) . ? C13 H13 0.9500 . ? C14 C15 1.390(8) . ? C14 H14 0.9500 . ? C15 C16 1.371(8) . ? C15 H15 0.9500 . ? C16 C17 1.380(7) . ? C16 H16 0.9500 . ? C17 C18 1.461(7) . ? C18 C19 1.400(7) . ? C19 C20 1.365(8) . ? C19 H19 0.9500 . ? C20 H20 0.9500 . ? C25 C26 1.375(8) . ? C25 H25 0.9500 . ? C26 C27 1.379(9) . ? C26 H26 0.9500 . ? C27 C28 1.377(8) . ? C27 H27 0.9500 . ? C28 C29 1.382(7) . ? C28 H28 0.9500 . ? C29 C30 1.450(8) . ? C30 C31 1.413(7) . ? C31 C32 1.368(9) . ? C31 H31 0.9500 . ? C32 H32 0.9500 . ? C37 C38 1.372(8) . ? C37 H37 0.9500 . ? C38 C39 1.382(9) . ? C38 H38 0.9500 . ? C39 C40 1.377(9) . ? C39 H39 0.9500 . ? C40 C41 1.392(8) . ? C40 H40 0.9500 . ? C41 C42 1.453(8) . ? C42 C43 1.403(7) . ? C43 C44 1.373(8) . ? C43 H43 0.9500 . ? C44 H44 0.9500 . ? C46 K2 3.322(5) 2_665 ? C48 K2 3.318(5) 2_665 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 Eu1 O1 144.61(14) . . ? O4 Eu1 O3 69.60(14) . . ? O1 Eu1 O3 145.04(14) . . ? O4 Eu1 O2 110.03(16) . . ? O1 Eu1 O2 83.96(15) . . ? O3 Eu1 O2 72.81(15) . . ? O4 Eu1 O5 82.17(15) . . ? O1 Eu1 O5 105.81(15) . . ? O3 Eu1 O5 80.87(15) . . ? O2 Eu1 O5 144.02(13) . . ? O4 Eu1 N7 78.05(16) . . ? O1 Eu1 N7 76.16(15) . . ? O3 Eu1 N7 118.33(16) . . ? O2 Eu1 N7 71.23(15) . . ? O5 Eu1 N7 144.43(14) . . ? O4 Eu1 N21 75.44(14) . . ? O1 Eu1 N21 75.44(14) . . ? O3 Eu1 N21 136.69(14) . . ? O2 Eu1 N21 145.38(14) . . ? O5 Eu1 N21 69.59(13) . . ? N7 Eu1 N21 76.94(14) . . ? O4 Eu1 N13 137.57(15) . 2_666 ? O1 Eu1 N13 76.42(14) . 2_666 ? O3 Eu1 N13 72.97(14) . 2_666 ? O2 Eu1 N13 76.31(14) . 2_666 ? O5 Eu1 N13 72.76(13) . 2_666 ? N7 Eu1 N13 139.17(15) . 2_666 ? N21 Eu1 N13 123.69(14) . 2_666 ? O10 Eu2 O9 91.59(16) . . ? O10 Eu2 O7 74.74(16) . . ? O9 Eu2 O7 143.86(14) . . ? O10 Eu2 O6 111.22(16) . . ? O9 Eu2 O6 146.56(13) . . ? O7 Eu2 O6 68.35(13) . . ? O10 Eu2 O8 142.09(13) . . ? O9 Eu2 O8 94.88(14) . . ? O7 Eu2 O8 78.25(14) . . ? O6 Eu2 O8 82.10(13) . . ? O10 Eu2 N14 144.59(14) . . ? O9 Eu2 N14 75.61(13) . . ? O7 Eu2 N14 133.05(14) . . ? O6 Eu2 N14 71.68(14) . . ? O8 Eu2 N14 72.78(13) . . ? O10 Eu2 N20 70.78(15) . . ? O9 Eu2 N20 88.31(15) . . ? O7 Eu2 N20 116.89(15) . . ? O6 Eu2 N20 77.28(14) . . ? O8 Eu2 N20 146.58(13) . . ? N14 Eu2 N20 75.88(14) . . ? O10 Eu2 N27 74.11(15) . . ? O9 Eu2 N27 72.25(14) . . ? O7 Eu2 N27 71.85(14) . . ? O6 Eu2 N27 136.20(13) . . ? O8 Eu2 N27 72.50(13) . . ? N14 Eu2 N27 129.63(14) . . ? N20 Eu2 N27 139.11(14) . . ? O10 Eu2 H7AA 78.8 . . ? O9 Eu2 H7AA 160.4 . . ? O7 Eu2 H7AA 16.7 . . ? O6 Eu2 H7AA 52.7 . . ? O8 Eu2 H7AA 83.0 . . ? N14 Eu2 H7AA 121.7 . . ? N20 Eu2 H7AA 104.3 . . ? N27 Eu2 H7AA 88.6 . . ? O10 Eu2 H7AB 58.9 . . ? O9 Eu2 H7AB 132.2 . . ? O7 Eu2 H7AB 16.7 . . ? O6 Eu2 H7AB 81.2 . . ? O8 Eu2 H7AB 90.3 . . ? N14 Eu2 H7AB 149.5 . . ? N20 Eu2 H7AB 111.9 . . ? N27 Eu2 H7AB 64.2 . . ? H7AA Eu2 H7AB 28.8 . . ? C11 Ru1 C12 91.5(2) . . ? C11 Ru1 C9 87.38(19) . . ? C12 Ru1 C9 90.2(2) . . ? C11 Ru1 C10 87.9(2) . . ? C12 Ru1 C10 90.9(2) . . ? C9 Ru1 C10 175.2(2) . . ? C11 Ru1 N3 99.10(18) . . ? C12 Ru1 N3 168.79(18) . . ? C9 Ru1 N3 93.84(18) . . ? C10 Ru1 N3 85.97(18) . . ? C11 Ru1 N1 174.81(18) . . ? C12 Ru1 N1 93.67(19) . . ? C9 Ru1 N1 92.55(17) . . ? C10 Ru1 N1 92.04(18) . . ? N3 Ru1 N1 75.72(16) . . ? C23 Ru2 C24 94.2(2) . . ? C23 Ru2 C22 85.2(2) . . ? C24 Ru2 C22 92.4(2) . . ? C23 Ru2 C21 90.4(2) . . ? C24 Ru2 C21 83.99(19) . . ? C22 Ru2 C21 174.11(19) . . ? C23 Ru2 N10 169.84(18) . . ? C24 Ru2 N10 95.97(18) . . ? C22 Ru2 N10 94.49(18) . . ? C21 Ru2 N10 90.53(18) . . ? C23 Ru2 N8 93.96(18) . . ? C24 Ru2 N8 171.49(18) . . ? C22 Ru2 N8 90.74(18) . . ? C21 Ru2 N8 93.48(17) . . ? N10 Ru2 N8 75.89(16) . . ? C35 Ru3 C36 91.8(2) . . ? C35 Ru3 C34 91.2(2) . . ? C36 Ru3 C34 89.4(2) . . ? C35 Ru3 C33 88.0(2) . . ? C36 Ru3 C33 86.84(19) . . ? C34 Ru3 C33 176.1(2) . . ? C35 Ru3 N17 169.44(18) . . ? C36 Ru3 N17 98.60(18) . . ? C34 Ru3 N17 90.85(18) . . ? C33 Ru3 N17 90.57(18) . . ? C35 Ru3 N15 93.79(18) . . ? C36 Ru3 N15 174.42(18) . . ? C34 Ru3 N15 90.20(18) . . ? C33 Ru3 N15 93.65(18) . . ? N17 Ru3 N15 75.85(16) . . ? C48 Ru4 C47 91.4(2) . . ? C48 Ru4 C45 86.9(2) . . ? C47 Ru4 C45 89.9(2) . . ? C48 Ru4 C46 91.1(2) . . ? C47 Ru4 C46 86.8(2) . . ? C45 Ru4 C46 176.0(2) . . ? C48 Ru4 N24 169.22(19) . . ? C47 Ru4 N24 99.32(19) . . ? C45 Ru4 N24 91.85(19) . . ? C46 Ru4 N24 90.76(18) . . ? C48 Ru4 N22 93.17(19) . . ? C47 Ru4 N22 175.3(2) . . ? C45 Ru4 N22 89.44(18) . . ? C46 Ru4 N22 94.09(19) . . ? N24 Ru4 N22 76.11(17) . . ? C1 N1 C5 118.0(4) . . ? C1 N1 Ru1 125.9(4) . . ? C5 N1 Ru1 116.1(3) . . ? N3 N2 C8 111.4(4) . . ? N3 N2 H2N 124.3 . . ? C8 N2 H2N 124.3 . . ? C6 N3 N2 105.6(4) . . ? C6 N3 Ru1 116.6(3) . . ? N2 N3 Ru1 136.2(3) . . ? C9 N4 K1 94.3(4) . 1_565 ? C11 N6 K2 99.2(4) . . ? C11 N6 K1 90.6(3) . 1_565 ? K2 N6 K1 110.41(15) . 1_565 ? C12 N7 Eu1 172.5(4) . . ? C13 N8 C17 117.0(4) . . ? C13 N8 Ru2 127.0(3) . . ? C17 N8 Ru2 116.0(3) . . ? N10 N9 C20 110.9(4) . . ? N10 N9 H9N 124.6 . . ? C20 N9 H9N 124.6 . . ? C18 N10 N9 106.2(4) . . ? C18 N10 Ru2 116.6(3) . . ? N9 N10 Ru2 136.4(3) . . ? C21 N11 K1 89.0(4) . . ? C23 N13 Eu1 143.5(4) . 2_666 ? C23 N13 K1 87.5(3) . . ? Eu1 N13 K1 128.73(16) 2_666 . ? C24 N14 Eu2 155.4(4) . . ? C25 N15 C29 117.4(5) . . ? C25 N15 Ru3 126.5(4) . . ? C29 N15 Ru3 116.0(3) . . ? N17 N16 C32 111.3(5) . . ? N17 N16 H16N 124.4 . . ? C32 N16 H16N 124.4 . . ? N16 N17 C30 106.6(4) . . ? N16 N17 Ru3 136.3(3) . . ? C30 N17 Ru3 116.8(3) . . ? C34 N19 K2 95.1(4) . . ? C35 N20 Eu2 161.7(4) . . ? C36 N21 Eu1 149.6(4) . . ? C36 N21 K2 92.9(3) . . ? Eu1 N21 K2 116.98(15) . . ? C37 N22 C41 117.7(5) . . ? C37 N22 Ru4 126.4(4) . . ? C41 N22 Ru4 115.8(3) . . ? N24 N23 C44 110.6(5) . . ? N24 N23 H23N 124.7 . . ? C44 N23 H23N 124.7 . . ? C42 N24 N23 106.3(4) . . ? C42 N24 Ru4 116.5(3) . . ? N23 N24 Ru4 137.0(3) . . ? C46 N26 K2 87.9(4) . 2_665 ? C48 N27 Eu2 151.4(4) . . ? C48 N27 K2 82.6(3) . 2_665 ? Eu2 N27 K2 125.50(16) . 2_665 ? C47 N28 K1 129.8(4) . 2_655 ? Eu1 O1 H1A 116.2 . . ? Eu1 O1 H1B 134.7 . . ? H1A O1 H1B 108.3 . . ? Eu1 O2 H2A 115.0 . . ? Eu1 O2 H2B 127.7 . . ? H2A O2 H2B 107.6 . . ? Eu1 O3 H3A 116.6 . . ? Eu1 O3 H3B 126.7 . . ? H3A O3 H3B 107.9 . . ? Eu1 O4 H4A 114.7 . . ? Eu1 O4 H4B 136.7 . . ? H4A O4 H4B 107.4 . . ? Eu1 O5 H5A 119.9 . . ? Eu1 O5 H5B 120.1 . . ? H5A O5 H5B 120.0 . . ? Eu2 O6 H6A1 109.4 . . ? Eu2 O6 H6A3 109.4 . . ? H6A1 O6 H6A3 109.5 . . ? Eu2 O7 H7AA 109.3 . . ? Eu2 O7 H7AB 109.4 . . ? H7AA O7 H7AB 109.5 . . ? Eu2 O8 H8AB 109.4 . . ? Eu2 O8 H8AC 109.3 . . ? H8AB O8 H8AC 109.5 . . ? Eu2 O9 H9A 121.4 . . ? Eu2 O9 H9B 130.4 . . ? H9A O9 H9B 108.2 . . ? Eu2 O10 H10A 125.6 . . ? Eu2 O10 H10B 121.6 . . ? H10A O10 H10B 108.2 . . ? K1 O11 H11A 109.4 . . ? K1 O11 H11C 109.4 . . ? H11A O11 H11C 109.5 . . ? K2 O12 H12A 109.4 . . ? K2 O12 H12C 109.4 . . ? H12A O12 H12C 109.5 . . ? K2 O13 H13A 120.3 . . ? K2 O13 H13B 119.8 . . ? H13A O13 H13B 120.0 . . ? O11 K1 N28 66.93(14) . 2_655 ? O11 K1 N4 161.34(13) . 1_545 ? N28 K1 N4 111.78(15) 2_655 1_545 ? O11 K1 N13 115.62(12) . . ? N28 K1 N13 78.14(14) 2_655 . ? N4 K1 N13 81.23(13) 1_545 . ? O11 K1 N6 73.47(12) . 1_545 ? N28 K1 N6 96.26(15) 2_655 1_545 ? N4 K1 N6 88.43(13) 1_545 1_545 ? N13 K1 N6 165.30(13) . 1_545 ? O11 K1 N11 73.71(12) . . ? N28 K1 N11 130.16(15) 2_655 . ? N4 K1 N11 115.17(14) 1_545 . ? N13 K1 N11 93.15(12) . . ? N6 K1 N11 100.73(13) 1_545 . ? O11 K1 C23 106.21(13) . . ? N28 K1 C23 90.66(15) 2_655 . ? N4 K1 C23 92.34(13) 1_545 . ? N13 K1 C23 21.31(12) . . ? N6 K1 C23 172.21(14) 1_545 . ? N11 K1 C23 71.94(13) . . ? O11 K1 C9 142.72(13) . 1_545 ? N28 K1 C9 119.82(15) 2_655 1_545 ? N4 K1 C9 20.52(13) 1_545 1_545 ? N13 K1 C9 101.39(13) . 1_545 ? N6 K1 C9 69.38(13) 1_545 1_545 ? N11 K1 C9 110.02(13) . 1_545 ? C23 K1 C9 110.15(13) . 1_545 ? O11 K1 C21 83.94(12) . . ? N28 K1 C21 123.84(15) 2_655 . ? N4 K1 C21 109.93(13) 1_545 . ? N13 K1 C21 72.87(12) . . ? N6 K1 C21 120.84(13) 1_545 . ? N11 K1 C21 20.30(12) . . ? C23 K1 C21 51.72(13) . . ? C9 K1 C21 112.50(12) 1_545 . ? O11 K1 C11 93.25(12) . 1_545 ? N28 K1 C11 109.26(15) 2_655 1_545 ? N4 K1 C11 69.23(13) 1_545 1_545 ? N13 K1 C11 150.27(13) . 1_545 ? N6 K1 C11 20.41(12) 1_545 1_545 ? N11 K1 C11 102.14(12) . 1_545 ? C23 K1 C11 156.56(13) . 1_545 ? C9 K1 C11 49.47(13) 1_545 1_545 ? C21 K1 C11 119.76(13) . 1_545 ? O11 K1 K2 78.94(9) . 1_545 ? N28 K1 K2 67.30(12) 2_655 1_545 ? N4 K1 K2 83.50(10) 1_545 1_545 ? N13 K1 K2 133.35(9) . 1_545 ? N6 K1 K2 34.00(9) 1_545 1_545 ? N11 K1 K2 133.03(10) . 1_545 ? C23 K1 K2 153.77(10) . 1_545 ? C9 K1 K2 72.20(9) 1_545 1_545 ? C21 K1 K2 153.21(10) . 1_545 ? C11 K1 K2 42.01(9) 1_545 1_545 ? O13 K2 O12 129.31(16) . . ? O13 K2 N6 82.74(15) . . ? O12 K2 N6 79.83(14) . . ? O13 K2 N26 148.28(16) . 2_665 ? O12 K2 N26 71.78(14) . 2_665 ? N6 K2 N26 127.81(14) . 2_665 ? O13 K2 N27 96.00(14) . 2_665 ? O12 K2 N27 118.69(13) . 2_665 ? N6 K2 N27 65.98(12) . 2_665 ? N26 K2 N27 90.60(13) 2_665 2_665 ? O13 K2 C48 115.57(15) . 2_665 ? O12 K2 C48 105.41(14) . 2_665 ? N6 K2 C48 75.55(13) . 2_665 ? N26 K2 C48 71.29(13) 2_665 2_665 ? N27 K2 C48 20.23(11) 2_665 2_665 ? O13 K2 C46 150.69(16) . 2_665 ? O12 K2 C46 79.18(14) . 2_665 ? N6 K2 C46 112.94(14) . 2_665 ? N26 K2 C46 20.42(13) 2_665 2_665 ? N27 K2 C46 70.62(13) 2_665 2_665 ? C48 K2 C46 50.98(13) 2_665 2_665 ? O13 K2 N21 71.06(13) . . ? O12 K2 N21 85.75(13) . . ? N6 K2 N21 131.00(13) . . ? N26 K2 N21 90.00(12) 2_665 . ? N27 K2 N21 154.34(12) 2_665 . ? C48 K2 N21 153.21(12) 2_665 . ? C46 K2 N21 109.78(12) 2_665 . ? O13 K2 C11 77.46(14) . . ? O12 K2 C11 70.26(13) . . ? N6 K2 C11 19.87(12) . . ? N26 K2 C11 134.09(13) 2_665 . ? N27 K2 C11 85.72(12) 2_665 . ? C48 K2 C11 95.02(13) 2_665 . ? C46 K2 C11 125.37(13) 2_665 . ? N21 K2 C11 111.74(12) . . ? O13 K2 N19 59.72(14) . . ? O12 K2 N19 160.89(14) . . ? N6 K2 N19 119.25(13) . . ? N26 K2 N19 93.43(13) 2_665 . ? N27 K2 N19 72.23(12) 2_665 . ? C48 K2 N19 80.12(12) 2_665 . ? C46 K2 N19 91.07(13) 2_665 . ? N21 K2 N19 82.13(11) . . ? C11 K2 N19 128.14(12) . . ? O13 K2 K1 117.39(12) . 1_565 ? O12 K2 K1 52.19(10) . 1_565 ? N6 K2 K1 35.59(9) . 1_565 ? N26 K2 K1 94.18(10) 2_665 1_565 ? N27 K2 K1 72.30(8) 2_665 1_565 ? C48 K2 K1 69.01(9) 2_665 1_565 ? C46 K2 K1 84.15(10) 2_665 1_565 ? N21 K2 K1 133.22(9) . 1_565 ? C11 K2 K1 41.36(8) . 1_565 ? N19 K2 K1 143.74(9) . 1_565 ? N1 C1 C2 122.8(5) . . ? N1 C1 H1 118.6 . . ? C2 C1 H1 118.6 . . ? C3 C2 C1 119.2(5) . . ? C3 C2 H2 120.4 . . ? C1 C2 H2 120.4 . . ? C4 C3 C2 118.7(5) . . ? C4 C3 H3 120.7 . . ? C2 C3 H3 120.7 . . ? C3 C4 C5 119.3(5) . . ? C3 C4 H4 120.4 . . ? C5 C4 H4 120.4 . . ? N1 C5 C4 122.0(5) . . ? N1 C5 C6 114.7(4) . . ? C4 C5 C6 123.3(5) . . ? N3 C6 C7 110.8(5) . . ? N3 C6 C5 116.0(4) . . ? C7 C6 C5 133.2(5) . . ? C8 C7 C6 104.6(5) . . ? C8 C7 H7 127.7 . . ? C6 C7 H7 127.7 . . ? N2 C8 C7 107.6(5) . . ? N2 C8 H8 126.2 . . ? C7 C8 H8 126.2 . . ? N4 C9 Ru1 173.5(5) . . ? N4 C9 K1 65.2(3) . 1_565 ? Ru1 C9 K1 109.60(19) . 1_565 ? N5 C10 Ru1 175.4(4) . . ? N6 C11 Ru1 178.6(5) . . ? N6 C11 K1 69.0(3) . 1_565 ? Ru1 C11 K1 109.62(19) . 1_565 ? N6 C11 K2 61.0(3) . . ? Ru1 C11 K2 119.3(2) . . ? K1 C11 K2 96.63(13) 1_565 . ? N7 C12 Ru1 176.4(5) . . ? N8 C13 C14 122.9(5) . . ? N8 C13 H13 118.5 . . ? C14 C13 H13 118.5 . . ? C13 C14 C15 119.3(5) . . ? C13 C14 H14 120.3 . . ? C15 C14 H14 120.3 . . ? C16 C15 C14 118.6(5) . . ? C16 C15 H15 120.7 . . ? C14 C15 H15 120.7 . . ? C15 C16 C17 119.4(5) . . ? C15 C16 H16 120.3 . . ? C17 C16 H16 120.3 . . ? N8 C17 C16 122.7(5) . . ? N8 C17 C18 114.2(4) . . ? C16 C17 C18 123.1(5) . . ? N10 C18 C19 109.9(4) . . ? N10 C18 C17 116.5(4) . . ? C19 C18 C17 133.5(5) . . ? C20 C19 C18 105.4(5) . . ? C20 C19 H19 127.3 . . ? C18 C19 H19 127.3 . . ? N9 C20 C19 107.6(5) . . ? N9 C20 H20 126.2 . . ? C19 C20 H20 126.2 . . ? N11 C21 Ru2 171.9(4) . . ? N11 C21 K1 70.7(3) . . ? Ru2 C21 K1 105.55(18) . . ? N12 C22 Ru2 171.8(4) . . ? N13 C23 Ru2 173.6(4) . . ? N13 C23 K1 71.1(3) . . ? Ru2 C23 K1 112.24(19) . . ? N14 C24 Ru2 173.0(4) . . ? N15 C25 C26 123.4(5) . . ? N15 C25 H25 118.3 . . ? C26 C25 H25 118.3 . . ? C25 C26 C27 118.9(5) . . ? C25 C26 H26 120.5 . . ? C27 C26 H26 120.5 . . ? C26 C27 C28 118.7(5) . . ? C26 C27 H27 120.6 . . ? C28 C27 H27 120.6 . . ? C27 C28 C29 119.4(5) . . ? C27 C28 H28 120.3 . . ? C29 C28 H28 120.3 . . ? N15 C29 C28 122.1(5) . . ? N15 C29 C30 114.4(4) . . ? C28 C29 C30 123.5(5) . . ? N17 C30 C31 109.3(5) . . ? N17 C30 C29 116.6(5) . . ? C31 C30 C29 134.1(5) . . ? C32 C31 C30 105.3(5) . . ? C32 C31 H31 127.3 . . ? C30 C31 H31 127.3 . . ? N16 C32 C31 107.5(5) . . ? N16 C32 H32 126.2 . . ? C31 C32 H32 126.2 . . ? N18 C33 Ru3 173.8(4) . . ? N19 C34 Ru3 176.7(5) . . ? N20 C35 Ru3 176.0(4) . . ? N21 C36 Ru3 176.9(4) . . ? N22 C37 C38 122.8(5) . . ? N22 C37 H37 118.6 . . ? C38 C37 H37 118.6 . . ? C37 C38 C39 119.5(6) . . ? C37 C38 H38 120.2 . . ? C39 C38 H38 120.2 . . ? C40 C39 C38 119.2(5) . . ? C40 C39 H39 120.4 . . ? C38 C39 H39 120.4 . . ? C39 C40 C41 118.7(6) . . ? C39 C40 H40 120.6 . . ? C41 C40 H40 120.6 . . ? N22 C41 C40 122.0(5) . . ? N22 C41 C42 114.3(5) . . ? C40 C41 C42 123.6(5) . . ? N24 C42 C43 110.4(5) . . ? N24 C42 C41 116.9(5) . . ? C43 C42 C41 132.7(5) . . ? C44 C43 C42 104.7(5) . . ? C44 C43 H43 127.6 . . ? C42 C43 H43 127.6 . . ? N23 C44 C43 108.0(5) . . ? N23 C44 H44 126.0 . . ? C43 C44 H44 126.0 . . ? N25 C45 Ru4 175.6(5) . . ? N26 C46 Ru4 173.9(5) . . ? N26 C46 K2 71.6(4) . 2_665 ? Ru4 C46 K2 106.16(19) . 2_665 ? N28 C47 Ru4 177.5(5) . . ? N27 C48 Ru4 174.3(5) . . ? N27 C48 K2 77.2(3) . 2_665 ? Ru4 C48 K2 108.07(19) . 2_665 ? 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 N2 H2N O20 0.88 1.86 2.735(6) 172.5 . N9 H9N O15 0.88 1.96 2.766(6) 152.1 . N16 H16N O17 0.88 1.87 2.733(6) 167.8 . N23 H23N O18 0.88 1.93 2.778(6) 160.4 1_544 O1 H1A O12 0.85 1.94 2.785(6) 173.6 . O1 H1B N4 0.84 2.13 2.755(6) 131.5 2_676 O1 H1B O17 0.84 2.61 3.040(6) 113.3 . O2 H2B O19 0.86 1.95 2.808(6) 170.9 2_666 O3 H3A N12 0.86 2.28 2.912(6) 130.5 . O3 H3B O16 0.84 2.02 2.812(6) 155.8 2_666 O4 H4B O14 0.85 1.90 2.616(6) 141.3 . O5 H5A N18 0.90 2.48 3.159(6) 132.9 . O5 H5B N12 0.90 2.10 2.978(6) 164.5 2_666 O7 H7AA N25 0.85 1.90 2.725(6) 163.8 2_655 O8 H8AB O11 0.85 2.79 3.032(5) 98.6 . O9 H9A O15 0.85 1.90 2.709(5) 161.0 . O9 H9B N19 0.85 1.94 2.788(6) 172.7 2_665 O10 H10B O13 0.85 2.46 3.302(7) 169.9 2_665 O11 H11C O8 0.98 2.18 3.032(5) 145.0 . O12 H12C O19 0.98 1.84 2.797(6) 165.0 1_565 O12 H12A N4 0.98 2.53 3.453(7) 157.2 . O13 H13A N19 0.90 2.61 3.112(7) 115.7 . O13 H13B O14 0.90 2.26 2.732(7) 112.7 . _diffrn_measured_fraction_theta_max 0.963 _diffrn_reflns_theta_full 27.54 _diffrn_measured_fraction_theta_full 0.963 _refine_diff_density_max 2.191 _refine_diff_density_min -0.967 _refine_diff_density_rms 0.167 #===END data_imw215j _database_code_depnum_ccdc_archive 'CCDC 276249' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H16 Eu N9 O8 Ru' _chemical_formula_weight 667.37 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' Eu Eu -0.1578 3.6682 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pna2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z+1/2' _cell_length_a 24.791(2) _cell_length_b 6.5425(6) _cell_length_c 12.4486(12) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2019.1(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 6924 _cell_measurement_theta_min 6.441 _cell_measurement_theta_max 55.004 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.195 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1288 _exptl_absorpt_coefficient_mu 3.888 _exptl_absorpt_correction_type multi-scans _exptl_absorpt_correction_T_min 0.2920 _exptl_absorpt_correction_T_max 0.5751 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker smart1000' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21936 _diffrn_reflns_av_R_equivalents 0.0299 _diffrn_reflns_av_sigmaI/netI 0.0246 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.64 _diffrn_reflns_theta_max 27.55 _reflns_number_total 4622 _reflns_number_gt 4376 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0228P)^2^+0.4211P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00 _refine_ls_number_reflns 4622 _refine_ls_number_parameters 280 _refine_ls_number_restraints 21 _refine_ls_R_factor_all 0.0208 _refine_ls_R_factor_gt 0.0185 _refine_ls_wR_factor_ref 0.0425 _refine_ls_wR_factor_gt 0.0417 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.046 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.349565(9) 0.99596(4) 0.38457(2) 0.01249(5) Uani 1 1 d . . . Eu2 Eu 0.515691(5) 0.62034(2) 0.598874(16) 0.01353(4) Uani 1 1 d . . . N1 N 0.27934(12) 1.1584(4) 0.3393(2) 0.0149(6) Uani 1 1 d . . . N2 N 0.18330(13) 1.1386(5) 0.3407(3) 0.0251(7) Uani 1 1 d . . . N3 N 0.28699(12) 0.8183(4) 0.4529(2) 0.0140(6) Uani 1 1 d . . . N4 N 0.19156(12) 0.7846(5) 0.4614(2) 0.0215(7) Uani 1 1 d . . . N5 N 0.33305(13) 0.7281(5) 0.1736(2) 0.0225(7) Uani 1 1 d . . . N6 N 0.44154(12) 0.7242(5) 0.4809(2) 0.0196(7) Uani 1 1 d . . . N7 N 0.43485(12) 1.2641(5) 0.2624(2) 0.0193(7) Uani 1 1 d . . . N8 N 0.36600(11) 1.2518(5) 0.6014(4) 0.0265(6) Uani 1 1 d . . . N9 N 0.55908(12) 0.9090(5) 0.4302(2) 0.0211(7) Uani 1 1 d . . . O1 O 0.43628(11) 0.5183(4) 0.7012(2) 0.0224(6) Uani 1 1 d D . . H11 H 0.4419 0.4552 0.7606 0.027 Uiso 1 1 d RD . . H12 H 0.4121 0.4433 0.6743 0.027 Uiso 1 1 d RD . . O2 O 0.60095(11) 0.4939(4) 0.5427(2) 0.0239(6) Uani 1 1 d D . . H22 H 0.6235 0.4276 0.5778 0.029 Uiso 1 1 d RD . . H21 H 0.6189 0.5478 0.4939 0.029 Uiso 1 1 d RD . . O3 O 0.47308(10) 0.9558(4) 0.6665(2) 0.0205(5) Uani 1 1 d D . . H31 H 0.4593 0.9612 0.7273 0.025 Uiso 1 1 d RD . . H32 H 0.4487 0.9993 0.6257 0.025 Uiso 1 1 d RD . . O4 O 0.53652(10) 0.3116(4) 0.7013(2) 0.0202(5) Uani 1 1 d D . . H41 H 0.5610 0.2942 0.7445 0.024 Uiso 1 1 d RD . . H42 H 0.5210 0.1964 0.6981 0.024 Uiso 1 1 d RD . . O5 O 0.56014(11) 0.9337(4) 0.5304(2) 0.0234(6) Uani 1 1 d . . . O6 O 0.54934(11) 0.7349(4) 0.3951(2) 0.0271(6) Uani 1 1 d . . . O7 O 0.56668(12) 1.0598(4) 0.3706(2) 0.0320(6) Uani 1 1 d . . . O8 O 0.49490(12) 0.3338(4) 0.4848(2) 0.0264(6) Uani 1 1 d D . . H81 H 0.5226 0.2714 0.4674 0.032 Uiso 1 1 d RD . . H82 H 0.4756 0.3371 0.4322 0.032 Uiso 1 1 d RD . . C1 C 0.23191(14) 1.0704(5) 0.3667(3) 0.0173(7) Uani 1 1 d . . . C3 C 0.18160(16) 1.3096(6) 0.2810(3) 0.0270(9) Uani 1 1 d . . . H3 H 0.1475 1.3617 0.2592 0.032 Uiso 1 1 calc R . . C4 C 0.22764(17) 1.4116(6) 0.2505(3) 0.0235(8) Uani 1 1 d . . . H4 H 0.2257 1.5343 0.2098 0.028 Uiso 1 1 calc R . . C5 C 0.27658(17) 1.3311(6) 0.2804(3) 0.0192(8) Uani 1 1 d . . . H5 H 0.3089 1.3980 0.2593 0.023 Uiso 1 1 calc R . . C6 C 0.23649(17) 0.8795(5) 0.4315(3) 0.0167(8) Uani 1 1 d . . . C7 C 0.29235(15) 0.6436(5) 0.5092(3) 0.0189(7) Uani 1 1 d . . . H7 H 0.3274 0.5950 0.5263 0.023 Uiso 1 1 calc R . . C8 C 0.24818(16) 0.5349(6) 0.5423(3) 0.0229(8) Uani 1 1 d . . . H8 H 0.2521 0.4105 0.5809 0.028 Uiso 1 1 calc R . . C9 C 0.19782(15) 0.6113(5) 0.5179(3) 0.0224(8) Uani 1 1 d . . . H9 H 0.1667 0.5395 0.5417 0.027 Uiso 1 1 calc R . . C10 C 0.34067(13) 0.8240(5) 0.2493(3) 0.0156(7) Uani 1 1 d . . . C11 C 0.40841(14) 0.8242(5) 0.4402(3) 0.0161(7) Uani 1 1 d . . . C12 C 0.40300(14) 1.1694(5) 0.3089(3) 0.0156(7) Uani 1 1 d . . . C13 C 0.35847(14) 1.1636(5) 0.5228(3) 0.0164(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 Ru1 0.00970(11) 0.01321(11) 0.01456(11) 0.00220(10) 0.00019(11) 0.00022(10) Eu2 0.01178(7) 0.01262(7) 0.01620(7) -0.00049(8) -0.00183(8) -0.00005(6) N1 0.0165(15) 0.0128(13) 0.0154(13) -0.0003(11) -0.0008(11) 0.0021(12) N2 0.0176(16) 0.0298(17) 0.0278(17) 0.0064(13) -0.0015(13) 0.0060(14) N3 0.0129(15) 0.0139(13) 0.0153(14) -0.0004(12) 0.0011(12) 0.0021(12) N4 0.0173(16) 0.0244(16) 0.0226(15) 0.0029(14) 0.0030(13) -0.0019(13) N5 0.0224(16) 0.0210(15) 0.0242(16) 0.0012(14) 0.0017(13) 0.0013(13) N6 0.0172(16) 0.0253(16) 0.0165(14) 0.0013(13) -0.0024(12) 0.0013(13) N7 0.0178(16) 0.0190(15) 0.0210(15) 0.0014(13) 0.0019(13) -0.0026(14) N8 0.0268(14) 0.0273(14) 0.0254(14) -0.0015(19) -0.0022(19) -0.0014(13) N9 0.0142(15) 0.0268(17) 0.0222(16) 0.0020(13) 0.0003(12) 0.0005(13) O1 0.0190(14) 0.0265(14) 0.0217(14) 0.0041(11) -0.0006(10) -0.0060(11) O2 0.0180(14) 0.0274(14) 0.0264(13) 0.0101(11) 0.0034(11) 0.0042(11) O3 0.0203(13) 0.0208(12) 0.0205(13) -0.0013(10) 0.0009(10) 0.0023(10) O4 0.0177(13) 0.0159(12) 0.0271(14) 0.0040(10) -0.0050(11) -0.0013(11) O5 0.0287(15) 0.0211(12) 0.0205(13) -0.0012(11) 0.0048(11) -0.0022(12) O6 0.0290(14) 0.0259(13) 0.0266(14) -0.0038(12) -0.0056(13) 0.0007(12) O7 0.0366(16) 0.0357(14) 0.0236(15) 0.0137(13) 0.0012(13) -0.0087(13) O8 0.0251(15) 0.0218(13) 0.0324(15) -0.0097(12) -0.0121(12) 0.0068(12) C1 0.0127(16) 0.0191(15) 0.0202(18) -0.0012(14) 0.0016(14) 0.0025(13) C3 0.019(2) 0.032(2) 0.030(2) 0.0064(17) -0.0026(16) 0.0092(17) C4 0.025(2) 0.0208(19) 0.025(2) 0.0051(16) -0.0026(17) 0.0094(17) C5 0.024(2) 0.0172(18) 0.0168(18) 0.0004(14) -0.0012(15) -0.0003(17) C6 0.018(2) 0.0172(19) 0.0152(17) -0.0008(14) 0.0014(15) -0.0001(14) C7 0.0167(18) 0.0194(17) 0.0205(18) 0.0053(14) 0.0008(14) 0.0020(14) C8 0.023(2) 0.0208(18) 0.0251(19) 0.0046(15) 0.0029(16) 0.0008(16) C9 0.0177(18) 0.0232(19) 0.0265(19) 0.0057(15) 0.0029(15) -0.0052(15) C10 0.0110(16) 0.0159(16) 0.0199(17) 0.0056(14) 0.0012(14) 0.0020(14) C11 0.0138(17) 0.0188(17) 0.0158(16) -0.0013(13) 0.0033(14) -0.0003(14) C12 0.0158(17) 0.0172(16) 0.0138(15) -0.0003(13) -0.0028(14) 0.0047(14) C13 0.0124(17) 0.0138(16) 0.0230(18) 0.0042(14) 0.0017(14) -0.0016(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 Ru1 C11 1.968(4) . ? Ru1 C12 1.982(4) . ? Ru1 C10 2.037(4) . ? Ru1 C13 2.052(4) . ? Ru1 N1 2.116(3) . ? Ru1 N3 2.117(3) . ? Eu2 O2 2.375(3) . ? Eu2 O8 2.407(3) . ? Eu2 O1 2.438(3) . ? Eu2 O4 2.444(2) . ? Eu2 N6 2.449(3) . ? Eu2 O5 2.479(3) . ? Eu2 N7 2.494(3) 2_675 ? Eu2 O3 2.577(3) . ? Eu2 O6 2.774(3) . ? Eu2 N9 3.022(3) . ? Eu2 H81 2.8139 . ? N1 C5 1.349(5) . ? N1 C1 1.353(4) . ? N2 C1 1.325(5) . ? N2 C3 1.344(5) . ? N3 C6 1.341(5) . ? N3 C7 1.347(4) . ? N4 C6 1.328(5) . ? N4 C9 1.343(5) . ? N5 C10 1.148(5) . ? N6 C11 1.166(4) . ? N7 C12 1.159(5) . ? N7 Eu2 2.494(3) 2_674 ? N8 C13 1.152(5) . ? N9 O6 1.243(4) . ? N9 O7 1.249(4) . ? N9 O5 1.258(4) . ? O1 H11 0.8589 . ? O1 H12 0.8446 . ? O2 H22 0.8313 . ? O2 H21 0.8316 . ? O3 H31 0.8301 . ? O3 H32 0.8391 . ? O4 H41 0.8181 . ? O4 H42 0.8471 . ? O8 H81 0.8270 . ? O8 H82 0.8121 . ? C1 C6 1.491(5) . ? C3 C4 1.376(6) . ? C3 H3 0.9500 . ? C4 C5 1.374(5) . ? C4 H4 0.9500 . ? C5 H5 0.9500 . ? C7 C8 1.369(5) . ? C7 H7 0.9500 . ? C8 C9 1.379(5) . ? C8 H8 0.9500 . ? C9 H9 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C11 Ru1 C12 89.93(13) . . ? C11 Ru1 C10 93.20(14) . . ? C12 Ru1 C10 89.76(14) . . ? C11 Ru1 C13 85.99(14) . . ? C12 Ru1 C13 91.18(13) . . ? C10 Ru1 C13 178.76(14) . . ? C11 Ru1 N1 172.14(13) . . ? C12 Ru1 N1 97.82(12) . . ? C10 Ru1 N1 88.19(12) . . ? C13 Ru1 N1 92.49(12) . . ? C11 Ru1 N3 95.06(13) . . ? C12 Ru1 N3 174.24(13) . . ? C10 Ru1 N3 87.09(12) . . ? C13 Ru1 N3 92.04(12) . . ? N1 Ru1 N3 77.27(11) . . ? O2 Eu2 O8 75.27(9) . . ? O2 Eu2 O1 140.99(8) . . ? O8 Eu2 O1 85.52(9) . . ? O2 Eu2 O4 71.21(8) . . ? O8 Eu2 O4 73.11(9) . . ? O1 Eu2 O4 70.83(9) . . ? O2 Eu2 N6 126.03(9) . . ? O8 Eu2 N6 72.65(10) . . ? O1 Eu2 N6 77.47(9) . . ? O4 Eu2 N6 134.50(9) . . ? O2 Eu2 O5 77.95(9) . . ? O8 Eu2 O5 122.45(9) . . ? O1 Eu2 O5 139.92(9) . . ? O4 Eu2 O5 140.28(9) . . ? N6 Eu2 O5 84.14(10) . . ? O2 Eu2 N7 84.75(10) . 2_675 ? O8 Eu2 N7 145.36(10) . 2_675 ? O1 Eu2 N7 93.07(9) . 2_675 ? O4 Eu2 N7 73.78(9) . 2_675 ? N6 Eu2 N7 140.74(10) . 2_675 ? O5 Eu2 N7 79.13(9) . 2_675 ? O2 Eu2 O3 139.25(8) . . ? O8 Eu2 O3 140.19(9) . . ? O1 Eu2 O3 74.43(8) . . ? O4 Eu2 O3 128.30(8) . . ? N6 Eu2 O3 69.63(9) . . ? O5 Eu2 O3 65.81(8) . . ? N7 Eu2 O3 71.12(9) 2_675 . ? O2 Eu2 O6 63.72(8) . . ? O8 Eu2 O6 74.67(9) . . ? O1 Eu2 O6 142.63(8) . . ? O4 Eu2 O6 129.58(8) . . ? N6 Eu2 O6 66.57(9) . . ? O5 Eu2 O6 47.80(8) . . ? N7 Eu2 O6 121.12(10) 2_675 . ? O3 Eu2 O6 101.07(8) . . ? O2 Eu2 N9 72.32(8) . . ? O8 Eu2 N9 98.81(9) . . ? O1 Eu2 N9 145.25(8) . . ? O4 Eu2 N9 143.50(8) . . ? N6 Eu2 N9 71.17(9) . . ? O5 Eu2 N9 23.93(8) . . ? N7 Eu2 N9 101.69(9) 2_675 . ? O3 Eu2 N9 80.84(8) . . ? O6 Eu2 N9 24.29(8) . . ? O2 Eu2 H81 59.5 . . ? O8 Eu2 H81 15.9 . . ? O1 Eu2 H81 97.5 . . ? O4 Eu2 H81 67.7 . . ? N6 Eu2 H81 85.5 . . ? O5 Eu2 H81 116.4 . . ? N7 Eu2 H81 133.7 2_675 . ? O3 Eu2 H81 154.9 . . ? O6 Eu2 H81 70.7 . . ? N9 Eu2 H81 94.7 . . ? C5 N1 C1 116.7(3) . . ? C5 N1 Ru1 127.4(3) . . ? C1 N1 Ru1 115.7(2) . . ? C1 N2 C3 116.4(3) . . ? C6 N3 C7 116.7(3) . . ? C6 N3 Ru1 116.1(2) . . ? C7 N3 Ru1 127.0(2) . . ? C6 N4 C9 116.4(3) . . ? C11 N6 Eu2 160.9(3) . . ? C12 N7 Eu2 154.8(3) . 2_674 ? O6 N9 O7 122.9(3) . . ? O6 N9 O5 118.1(3) . . ? O7 N9 O5 119.0(3) . . ? O6 N9 Eu2 66.61(18) . . ? O7 N9 Eu2 163.8(2) . . ? O5 N9 Eu2 53.06(17) . . ? Eu2 O1 H11 116.7 . . ? Eu2 O1 H12 121.7 . . ? H11 O1 H12 100.3 . . ? Eu2 O2 H22 128.7 . . ? Eu2 O2 H21 122.9 . . ? H22 O2 H21 104.2 . . ? Eu2 O3 H31 120.1 . . ? Eu2 O3 H32 112.7 . . ? H31 O3 H32 104.0 . . ? Eu2 O4 H41 127.9 . . ? Eu2 O4 H42 127.9 . . ? H41 O4 H42 104.1 . . ? N9 O5 Eu2 103.0(2) . . ? N9 O6 Eu2 89.1(2) . . ? Eu2 O8 H81 111.2 . . ? Eu2 O8 H82 125.6 . . ? H81 O8 H82 106.9 . . ? N2 C1 N1 125.8(3) . . ? N2 C1 C6 118.9(3) . . ? N1 C1 C6 115.2(3) . . ? N2 C3 C4 122.1(4) . . ? N2 C3 H3 119.0 . . ? C4 C3 H3 119.0 . . ? C5 C4 C3 118.1(4) . . ? C5 C4 H4 120.9 . . ? C3 C4 H4 120.9 . . ? N1 C5 C4 120.9(4) . . ? N1 C5 H5 119.6 . . ? C4 C5 H5 119.6 . . ? N4 C6 N3 126.0(3) . . ? N4 C6 C1 118.6(4) . . ? N3 C6 C1 115.4(3) . . ? N3 C7 C8 121.2(3) . . ? N3 C7 H7 119.4 . . ? C8 C7 H7 119.4 . . ? C7 C8 C9 118.0(3) . . ? C7 C8 H8 121.0 . . ? C9 C8 H8 121.0 . . ? N4 C9 C8 121.7(3) . . ? N4 C9 H9 119.1 . . ? C8 C9 H9 119.1 . . ? N5 C10 Ru1 176.7(3) . . ? N6 C11 Ru1 174.8(3) . . ? N7 C12 Ru1 177.3(3) . . ? N8 C13 Ru1 176.3(3) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.55 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.808 _refine_diff_density_min -0.411 _refine_diff_density_rms 0.085 #===END