# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Javier Cabeza' _publ_contact_author_email jac@uniovi.es loop_ _publ_author_name J.Cabeza V.Pruneda data_v37b _database_code_depnum_ccdc_archive 'CCDC 871262' #TrackingRef '- v37b.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C35 H12 N4 O19 Ru6' _chemical_formula_sum 'C35 H12 N4 O19 Ru6' _chemical_formula_weight 1398.91 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru 0.0552 3.2960 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting MONOCLINIC _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' 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 12.8725(2) _cell_length_b 23.8018(3) _cell_length_c 17.6715(2) _cell_angle_alpha 90.00 _cell_angle_beta 127.0880(10) _cell_angle_gamma 90.00 _cell_volume 4319.08(10) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 7080 _cell_measurement_theta_min 3.1303 _cell_measurement_theta_max 73.7583 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.07 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.151 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2664 _exptl_absorpt_coefficient_mu 17.284 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.71777 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.54180 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'Enhance (Cu) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type Xcalibur _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24915 _diffrn_reflns_av_R_equivalents 0.0511 _diffrn_reflns_av_sigmaI/netI 0.0697 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.64 _diffrn_reflns_theta_max 70.00 _reflns_number_total 8061 _reflns_number_gt 4715 _reflns_threshold_expression >2\s(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'PLATON (Spek, 2008)' _computing_publication_material 'SHELXL-97 (Sheldrick, 2008)' _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^ > 2\s(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 [0.00000+1.00000exp(2.00(sin\q/\l)^2^)]/ [\s^2^(Fo^2^)+0.0000+0.0000*P+(0.0407P)^2^+0.0000sin\q/\l] where P = 0.33333Fo^2^ + 0.66667Fc^2^ ; _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 8061 _refine_ls_number_parameters 585 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0684 _refine_ls_R_factor_gt 0.0342 _refine_ls_wR_factor_ref 0.0868 _refine_ls_wR_factor_gt 0.0747 _refine_ls_goodness_of_fit_ref 1.015 _refine_ls_restrained_S_all 1.015 _refine_ls_shift/su_max 0.000 _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 C1 C 0.0757(7) -0.1140(3) 0.2854(5) 0.0494(15) Uani 1 1 d . . . C2 C 0.1909(7) -0.0773(3) 0.2333(5) 0.0515(16) Uani 1 1 d . . . H2 H 0.2385 -0.0856 0.2107 0.062 Uiso 1 1 calc R . . C3 C 0.1017(7) -0.0127(3) 0.2732(5) 0.0512(16) Uani 1 1 d . . . C4 C 0.0753(8) 0.0420(3) 0.2835(6) 0.071(2) Uani 1 1 d . . . H4 H 0.1092 0.0717 0.2705 0.085 Uiso 1 1 calc R . . C5 C 0.0001(9) 0.0530(4) 0.3127(8) 0.090(3) Uani 1 1 d . . . H5 H -0.0158 0.0903 0.3187 0.108 Uiso 1 1 calc R . . C6 C -0.0528(9) 0.0114(4) 0.3335(7) 0.079(3) Uani 1 1 d . . . H6 H -0.1054 0.0201 0.3517 0.094 Uiso 1 1 calc R . . C7 C -0.0264(8) -0.0430(4) 0.3268(6) 0.073(2) Uani 1 1 d . . . H7 H -0.0591 -0.0716 0.3430 0.087 Uiso 1 1 calc R . . C8 C 0.0492(7) -0.0573(3) 0.2961(5) 0.0536(17) Uani 1 1 d . . . C9 C 0.4882(6) -0.0364(3) 0.2696(5) 0.0467(14) Uani 1 1 d . . . C10 C 0.4923(7) -0.0111(3) 0.4010(5) 0.0545(17) Uani 1 1 d . . . H10 H 0.4584 0.0124 0.4233 0.065 Uiso 1 1 calc R . . C11 C 0.6336(7) -0.0792(3) 0.4271(5) 0.0543(17) Uani 1 1 d . . . C12 C 0.7248(8) -0.1191(4) 0.4862(6) 0.071(2) Uani 1 1 d . . . H12 H 0.7530 -0.1216 0.5485 0.086 Uiso 1 1 calc R . . C13 C 0.7746(9) -0.1550(4) 0.4553(7) 0.082(3) Uani 1 1 d . . . H13 H 0.8353 -0.1821 0.4959 0.098 Uiso 1 1 calc R . . C14 C 0.7347(9) -0.1507(3) 0.3644(7) 0.076(2) Uani 1 1 d . . . H14 H 0.7681 -0.1753 0.3430 0.092 Uiso 1 1 calc R . . C15 C 0.6461(8) -0.1107(3) 0.3042(6) 0.065(2) Uani 1 1 d . . . H15 H 0.6227 -0.1077 0.2432 0.078 Uiso 1 1 calc R . . C16 C 0.5903(7) -0.0744(3) 0.3321(6) 0.0550(17) Uani 1 1 d . . . C101 C 0.0832(9) -0.2013(3) 0.1062(6) 0.070(2) Uani 1 1 d . . . C102 C 0.3490(9) -0.1984(3) 0.2853(6) 0.066(2) Uani 1 1 d . . . C103 C 0.1863(9) -0.2871(3) 0.2316(6) 0.070(2) Uani 1 1 d . . . C201 C -0.1566(8) -0.1660(4) 0.2131(6) 0.065(2) Uani 1 1 d . . . C202 C 0.0457(8) -0.1668(4) 0.4218(7) 0.075(2) Uani 1 1 d . . . C203 C -0.0397(10) -0.2658(4) 0.3117(8) 0.085(3) Uani 1 1 d . . . C301 C 0.3145(10) -0.2227(3) 0.5602(7) 0.076(2) Uani 1 1 d . . . C302 C 0.4607(9) -0.2418(4) 0.4872(7) 0.079(2) Uani 1 1 d . . . C303 C 0.3249(8) -0.1414(3) 0.4508(6) 0.065(2) Uani 1 1 d . . . C304 C 0.2181(10) -0.2987(4) 0.4045(6) 0.079(2) Uani 1 1 d . . . C402 C 0.3162(8) 0.0973(3) 0.2856(6) 0.0638(19) Uani 1 1 d . . . C403 C 0.1083(8) 0.0687(3) 0.1064(6) 0.0605(19) Uani 1 1 d . . . C501 C 0.3488(9) -0.1033(3) 0.1095(6) 0.067(2) Uani 1 1 d . . . C502 C 0.5257(8) -0.0232(3) 0.1252(6) 0.068(2) Uani 1 1 d . . . C503 C 0.2579(9) -0.0149(4) -0.0130(6) 0.071(2) Uani 1 1 d . . . C601 C 0.5592(9) 0.0789(4) 0.2685(7) 0.074(2) Uani 1 1 d . . . C602 C 0.2320(9) 0.0970(4) 0.0227(7) 0.082(3) Uani 1 1 d . . . C603 C 0.4930(10) 0.1091(4) 0.0933(8) 0.088(3) Uani 1 1 d . . . C604 C 0.3851(12) 0.1682(4) 0.1744(8) 0.097(3) Uani 1 1 d . . . N1 N 0.1453(6) -0.1215(2) 0.2533(4) 0.0490(13) Uani 1 1 d . . . N2 N 0.1748(6) -0.0238(2) 0.2425(4) 0.0489(12) Uani 1 1 d . . . N3 N 0.4409(5) -0.0066(2) 0.3066(4) 0.0456(12) Uani 1 1 d . . . N4 N 0.5833(6) -0.0451(3) 0.4608(4) 0.0613(16) Uani 1 1 d . . . O101 O 0.0358(9) -0.2038(3) 0.0281(5) 0.111(3) Uani 1 1 d . . . O102 O 0.4533(7) -0.1942(3) 0.3106(5) 0.0910(19) Uani 1 1 d . . . O103 O 0.1926(8) -0.3329(2) 0.2224(6) 0.101(2) Uani 1 1 d . . . O201 O -0.2607(7) -0.1506(3) 0.1603(5) 0.099(2) Uani 1 1 d . . . O202 O 0.0623(8) -0.1522(4) 0.4899(5) 0.109(2) Uani 1 1 d . . . O203 O -0.0830(9) -0.3080(3) 0.3069(7) 0.133(3) Uani 1 1 d . . . O301 O 0.3281(8) -0.2215(3) 0.6262(5) 0.100(2) Uani 1 1 d . . . O302 O 0.5632(8) -0.2527(4) 0.5171(6) 0.123(3) Uani 1 1 d . . . O303 O 0.3546(7) -0.0962(2) 0.4652(5) 0.0871(18) Uani 1 1 d . . . O304 O 0.1903(8) -0.3445(3) 0.3931(5) 0.095(2) Uani 1 1 d . . . O402 O 0.3494(7) 0.1350(3) 0.3367(5) 0.0900(19) Uani 1 1 d . . . O403 O 0.0071(6) 0.0842(3) 0.0488(5) 0.094(2) Uani 1 1 d . . . O501 O 0.3367(9) -0.1507(3) 0.1040(5) 0.109(3) Uani 1 1 d . . . O502 O 0.6159(7) -0.0202(3) 0.1263(6) 0.103(2) Uani 1 1 d . . . O503 O 0.1866(8) -0.0128(4) -0.0935(5) 0.110(2) Uani 1 1 d . . . O601 O 0.6560(7) 0.0728(3) 0.3416(5) 0.102(2) Uani 1 1 d . . . O602 O 0.1360(8) 0.1038(4) -0.0486(6) 0.112(3) Uani 1 1 d . . . O603 O 0.5428(8) 0.1168(4) 0.0580(6) 0.121(3) Uani 1 1 d . . . O604 O 0.3696(10) 0.2128(3) 0.1907(8) 0.147(4) Uani 1 1 d . . . Ru1 Ru 0.17373(6) -0.20782(2) 0.24160(4) 0.05207(14) Uani 1 1 d . . . Ru2 Ru 0.01763(6) -0.19052(2) 0.30689(4) 0.05666(15) Uani 1 1 d . . . Ru3 Ru 0.28576(6) -0.22153(2) 0.43688(4) 0.05719(15) Uani 1 1 d . . . Ru4 Ru 0.27007(5) 0.03754(2) 0.20429(4) 0.04799(13) Uani 1 1 d . . . Ru5 Ru 0.37698(6) -0.02520(2) 0.12252(4) 0.05118(13) Uani 1 1 d . . . Ru6 Ru 0.40079(7) 0.09378(2) 0.14443(5) 0.06475(17) Uani 1 1 d . . . H100 H -0.022(10) -0.219(4) 0.175(7) 0.12(4) Uiso 1 1 d . . . H200 H 0.233(6) -0.017(2) 0.109(5) 0.045(17) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.042(4) 0.053(3) 0.053(4) 0.006(3) 0.028(4) 0.005(3) C2 0.057(4) 0.046(3) 0.063(5) 0.000(3) 0.042(4) 0.000(3) C3 0.044(4) 0.056(4) 0.045(4) -0.004(3) 0.022(3) 0.004(3) C4 0.072(5) 0.059(4) 0.081(6) -0.012(4) 0.046(5) 0.001(4) C5 0.074(6) 0.089(6) 0.123(9) -0.024(6) 0.068(7) 0.005(5) C6 0.072(6) 0.082(5) 0.103(8) -0.011(5) 0.064(6) 0.006(5) C7 0.070(5) 0.081(5) 0.086(6) 0.006(5) 0.057(5) 0.010(4) C8 0.046(4) 0.067(4) 0.046(4) 0.003(3) 0.026(4) 0.009(3) C9 0.047(4) 0.049(3) 0.048(4) -0.001(3) 0.030(3) -0.001(3) C10 0.057(4) 0.059(4) 0.049(4) -0.013(3) 0.032(4) -0.004(4) C11 0.047(4) 0.064(4) 0.047(4) 0.001(3) 0.026(4) 0.003(3) C12 0.052(4) 0.096(6) 0.060(5) 0.010(4) 0.030(4) 0.023(4) C13 0.062(5) 0.093(6) 0.078(7) 0.016(5) 0.036(5) 0.027(5) C14 0.076(6) 0.071(5) 0.090(7) -0.007(5) 0.054(6) 0.011(5) C15 0.070(5) 0.068(4) 0.071(6) 0.007(4) 0.050(5) 0.013(4) C16 0.050(4) 0.057(4) 0.060(5) -0.006(3) 0.034(4) -0.004(3) C101 0.095(7) 0.057(4) 0.062(6) 0.002(4) 0.050(5) 0.009(4) C102 0.073(6) 0.061(4) 0.072(6) 0.000(4) 0.047(5) 0.004(4) C103 0.090(6) 0.055(4) 0.075(6) -0.003(4) 0.056(6) -0.007(4) C201 0.051(5) 0.083(5) 0.068(6) -0.004(4) 0.039(5) -0.006(4) C202 0.053(5) 0.103(6) 0.070(6) -0.005(5) 0.039(5) -0.013(5) C203 0.078(6) 0.082(6) 0.102(8) 0.007(5) 0.058(6) -0.016(5) C301 0.090(7) 0.069(5) 0.057(5) 0.004(4) 0.039(5) -0.009(5) C302 0.060(6) 0.073(5) 0.093(7) 0.008(5) 0.040(6) 0.006(5) C303 0.058(5) 0.060(5) 0.068(6) 0.009(4) 0.033(5) -0.001(4) C304 0.091(7) 0.078(6) 0.061(6) 0.004(5) 0.042(5) -0.010(5) C402 0.063(5) 0.054(4) 0.061(5) 0.004(4) 0.030(4) 0.006(4) C403 0.059(5) 0.054(4) 0.060(5) 0.014(4) 0.032(5) 0.007(4) C501 0.080(6) 0.072(5) 0.050(5) -0.014(4) 0.040(5) -0.012(4) C502 0.066(5) 0.073(5) 0.069(6) 0.009(4) 0.044(5) 0.001(4) C503 0.066(5) 0.100(6) 0.052(5) 0.007(4) 0.038(5) 0.000(5) C601 0.055(5) 0.073(5) 0.081(7) 0.009(5) 0.034(5) -0.011(4) C602 0.059(6) 0.098(7) 0.073(6) 0.024(5) 0.031(5) 0.003(5) C603 0.081(7) 0.097(7) 0.094(8) 0.012(6) 0.057(7) -0.011(5) C604 0.115(9) 0.060(5) 0.106(9) 0.003(5) 0.061(8) -0.014(6) N1 0.051(3) 0.046(3) 0.055(4) -0.002(2) 0.035(3) -0.001(2) N2 0.049(3) 0.045(3) 0.049(3) 0.000(2) 0.027(3) -0.003(2) N3 0.043(3) 0.045(3) 0.040(3) 0.000(2) 0.021(3) 0.000(2) N4 0.060(4) 0.070(4) 0.043(3) -0.002(3) 0.025(3) 0.013(3) O101 0.156(8) 0.105(5) 0.063(5) 0.001(4) 0.061(5) 0.007(5) O102 0.076(4) 0.111(5) 0.102(5) -0.004(4) 0.062(4) -0.001(4) O103 0.156(7) 0.051(3) 0.121(6) -0.009(3) 0.096(6) -0.006(4) O201 0.058(4) 0.143(6) 0.082(5) -0.002(4) 0.034(4) 0.014(4) O202 0.102(6) 0.166(7) 0.078(5) -0.005(5) 0.065(5) 0.009(5) O203 0.122(7) 0.101(6) 0.146(8) 0.015(5) 0.065(6) -0.041(5) O301 0.137(7) 0.110(5) 0.066(4) 0.003(4) 0.069(5) -0.014(4) O302 0.073(5) 0.130(7) 0.139(8) 0.022(6) 0.050(5) 0.031(5) O303 0.089(5) 0.061(3) 0.086(5) -0.001(3) 0.039(4) -0.016(3) O304 0.121(6) 0.061(4) 0.098(5) -0.001(3) 0.063(5) -0.015(4) O402 0.097(5) 0.064(3) 0.086(5) -0.018(3) 0.043(4) 0.001(3) O403 0.065(4) 0.091(4) 0.090(5) 0.024(4) 0.029(4) 0.017(4) O501 0.176(8) 0.070(4) 0.089(5) -0.026(4) 0.085(6) -0.030(4) O502 0.086(5) 0.130(6) 0.124(6) 0.019(5) 0.080(5) 0.005(4) O503 0.092(5) 0.156(7) 0.060(5) 0.007(4) 0.034(4) -0.009(5) O601 0.068(4) 0.107(5) 0.091(5) 0.011(4) 0.026(4) -0.025(4) O602 0.085(5) 0.141(7) 0.085(5) 0.034(5) 0.039(5) 0.017(5) O603 0.117(6) 0.146(7) 0.139(8) 0.011(6) 0.097(7) -0.024(5) O604 0.159(9) 0.070(5) 0.206(11) -0.002(6) 0.107(9) 0.002(5) Ru1 0.0592(3) 0.0472(3) 0.0551(3) -0.0004(2) 0.0373(3) -0.0025(2) Ru2 0.0503(3) 0.0638(3) 0.0582(4) 0.0021(3) 0.0340(3) -0.0062(3) Ru3 0.0570(3) 0.0549(3) 0.0536(3) 0.0055(3) 0.0302(3) -0.0003(3) Ru4 0.0469(3) 0.0444(2) 0.0493(3) 0.0029(2) 0.0272(3) 0.0005(2) Ru5 0.0522(3) 0.0597(3) 0.0453(3) -0.0010(2) 0.0313(3) -0.0059(2) Ru6 0.0620(4) 0.0588(3) 0.0691(4) 0.0103(3) 0.0373(4) -0.0080(3) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 C1 N1 1.330(8) . ? C1 C8 1.433(9) . ? C1 Ru2 2.088(6) . ? C2 N2 1.316(8) . ? C2 N1 1.351(8) . ? C3 N2 1.366(9) . ? C3 C4 1.386(10) . ? C3 C8 1.441(10) . ? C4 C5 1.369(12) . ? C5 C6 1.373(13) . ? C6 C7 1.361(12) . ? C7 C8 1.413(10) . ? C9 N3 1.336(8) . ? C9 C16 1.421(10) . ? C9 Ru5 2.094(7) . ? C10 N4 1.286(9) . ? C10 N3 1.378(9) . ? C11 C12 1.375(11) . ? C11 N4 1.376(9) . ? C11 C16 1.419(10) . ? C12 C13 1.364(12) . ? C13 C14 1.365(13) . ? C14 C15 1.369(12) . ? C15 C16 1.390(10) . ? C101 O101 1.124(10) . ? C101 Ru1 1.936(9) . ? C102 O102 1.135(10) . ? C102 Ru1 1.907(9) . ? C103 O103 1.113(9) . ? C103 Ru1 1.910(8) . ? C201 O201 1.137(10) . ? C201 Ru2 1.906(9) . ? C202 O202 1.142(11) . ? C202 Ru2 1.921(10) . ? C203 O203 1.126(11) . ? C203 Ru2 1.959(9) . ? C301 O301 1.070(10) . ? C301 Ru3 1.978(9) . ? C302 O302 1.116(11) . ? C302 Ru3 1.918(9) . ? C303 O303 1.118(9) . ? C303 Ru3 1.950(8) . ? C304 O304 1.128(10) . ? C304 Ru3 1.963(9) . ? C402 O402 1.158(9) . ? C402 Ru4 1.846(8) . ? C403 O403 1.127(9) . ? C403 Ru4 1.880(8) . ? C501 O501 1.135(10) . ? C501 Ru5 1.882(8) . ? C502 O502 1.152(10) . ? C502 Ru5 1.887(8) . ? C503 O503 1.138(10) . ? C503 Ru5 1.928(9) . ? C601 O601 1.141(11) . ? C601 Ru6 1.923(10) . ? C602 O602 1.124(11) . ? C602 Ru6 1.928(10) . ? C603 O603 1.148(11) . ? C603 Ru6 1.911(9) . ? C604 O604 1.147(13) . ? C604 Ru6 1.895(10) . ? N1 Ru1 2.119(5) . ? N2 Ru4 2.257(5) . ? N3 Ru4 2.100(5) . ? Ru1 Ru3 2.8447(8) . ? Ru1 Ru2 2.8870(8) . ? Ru2 Ru3 2.8587(9) . ? Ru4 Ru6 2.8088(8) . ? Ru4 Ru5 2.9345(7) . ? Ru5 Ru6 2.8495(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C8 117.2(6) . . ? N1 C1 Ru2 111.6(4) . . ? C8 C1 Ru2 131.1(5) . . ? N2 C2 N1 126.5(6) . . ? N2 C3 C4 121.1(7) . . ? N2 C3 C8 121.4(6) . . ? C4 C3 C8 117.5(7) . . ? C5 C4 C3 121.0(8) . . ? C4 C5 C6 122.7(8) . . ? C7 C6 C5 118.3(8) . . ? C6 C7 C8 121.9(8) . . ? C7 C8 C1 123.5(7) . . ? C7 C8 C3 118.6(7) . . ? C1 C8 C3 117.9(6) . . ? N3 C9 C16 116.0(6) . . ? N3 C9 Ru5 111.6(5) . . ? C16 C9 Ru5 131.7(5) . . ? N4 C10 N3 125.4(6) . . ? C12 C11 N4 119.1(7) . . ? C12 C11 C16 120.0(7) . . ? N4 C11 C16 120.9(7) . . ? C13 C12 C11 121.4(8) . . ? C12 C13 C14 119.4(9) . . ? C13 C14 C15 120.8(8) . . ? C14 C15 C16 121.6(8) . . ? C15 C16 C11 116.9(7) . . ? C15 C16 C9 123.6(7) . . ? C11 C16 C9 119.4(6) . . ? O101 C101 Ru1 171.8(7) . . ? O102 C102 Ru1 178.1(7) . . ? O103 C103 Ru1 177.3(8) . . ? O201 C201 Ru2 177.0(8) . . ? O202 C202 Ru2 179.4(9) . . ? O203 C203 Ru2 173.9(10) . . ? O301 C301 Ru3 177.4(9) . . ? O302 C302 Ru3 178.8(10) . . ? O303 C303 Ru3 175.1(8) . . ? O304 C304 Ru3 173.6(9) . . ? O402 C402 Ru4 177.4(8) . . ? O403 C403 Ru4 174.8(7) . . ? O501 C501 Ru5 177.4(10) . . ? O502 C502 Ru5 177.9(7) . . ? O503 C503 Ru5 175.1(9) . . ? O601 C601 Ru6 176.1(7) . . ? O602 C602 Ru6 173.9(9) . . ? O603 C603 Ru6 176.1(10) . . ? O604 C604 Ru6 176.8(11) . . ? C1 N1 C2 121.3(5) . . ? C1 N1 Ru1 111.8(4) . . ? C2 N1 Ru1 126.9(4) . . ? C2 N2 C3 115.8(5) . . ? C2 N2 Ru4 115.7(4) . . ? C3 N2 Ru4 128.5(4) . . ? C9 N3 C10 121.6(6) . . ? C9 N3 Ru4 113.1(4) . . ? C10 N3 Ru4 124.8(4) . . ? C10 N4 C11 116.7(6) . . ? C102 Ru1 C103 90.5(3) . . ? C102 Ru1 C101 100.0(4) . . ? C103 Ru1 C101 89.2(3) . . ? C102 Ru1 N1 94.5(3) . . ? C103 Ru1 N1 174.7(3) . . ? C101 Ru1 N1 91.8(3) . . ? C102 Ru1 Ru3 84.9(3) . . ? C103 Ru1 Ru3 89.4(3) . . ? C101 Ru1 Ru3 174.8(3) . . ? N1 Ru1 Ru3 89.10(16) . . ? C102 Ru1 Ru2 139.5(3) . . ? C103 Ru1 Ru2 107.2(2) . . ? C101 Ru1 Ru2 116.0(3) . . ? N1 Ru1 Ru2 67.67(14) . . ? Ru3 Ru1 Ru2 59.83(2) . . ? C201 Ru2 C202 101.6(4) . . ? C201 Ru2 C203 92.4(4) . . ? C202 Ru2 C203 93.4(4) . . ? C201 Ru2 C1 86.4(3) . . ? C202 Ru2 C1 94.4(3) . . ? C203 Ru2 C1 172.2(4) . . ? C201 Ru2 Ru3 174.2(2) . . ? C202 Ru2 Ru3 82.0(3) . . ? C203 Ru2 Ru3 91.9(3) . . ? C1 Ru2 Ru3 88.87(19) . . ? C201 Ru2 Ru1 115.7(2) . . ? C202 Ru2 Ru1 137.1(2) . . ? C203 Ru2 Ru1 104.9(3) . . ? C1 Ru2 Ru1 68.89(18) . . ? Ru3 Ru2 Ru1 59.35(2) . . ? C302 Ru3 C303 92.6(4) . . ? C302 Ru3 C304 95.2(4) . . ? C303 Ru3 C304 170.6(4) . . ? C302 Ru3 C301 95.6(4) . . ? C303 Ru3 C301 90.7(3) . . ? C304 Ru3 C301 93.6(3) . . ? C302 Ru3 Ru1 100.7(3) . . ? C303 Ru3 Ru1 86.8(3) . . ? C304 Ru3 Ru1 86.7(3) . . ? C301 Ru3 Ru1 163.5(3) . . ? C302 Ru3 Ru2 161.5(3) . . ? C303 Ru3 Ru2 86.8(2) . . ? C304 Ru3 Ru2 84.2(3) . . ? C301 Ru3 Ru2 102.8(3) . . ? Ru1 Ru3 Ru2 60.82(2) . . ? C402 Ru4 C403 94.0(3) . . ? C402 Ru4 N3 92.1(3) . . ? C403 Ru4 N3 173.3(3) . . ? C402 Ru4 N2 104.1(3) . . ? C403 Ru4 N2 91.8(3) . . ? N3 Ru4 N2 83.9(2) . . ? C402 Ru4 Ru6 86.6(3) . . ? C403 Ru4 Ru6 92.7(2) . . ? N3 Ru4 Ru6 90.50(14) . . ? N2 Ru4 Ru6 168.04(14) . . ? C402 Ru4 Ru5 138.5(3) . . ? C403 Ru4 Ru5 109.6(2) . . ? N3 Ru4 Ru5 67.13(15) . . ? N2 Ru4 Ru5 108.60(14) . . ? Ru6 Ru4 Ru5 59.444(19) . . ? C501 Ru5 C502 98.4(4) . . ? C501 Ru5 C503 91.4(4) . . ? C502 Ru5 C503 93.6(4) . . ? C501 Ru5 C9 87.9(3) . . ? C502 Ru5 C9 92.8(3) . . ? C503 Ru5 C9 173.7(3) . . ? C501 Ru5 Ru6 174.6(3) . . ? C502 Ru5 Ru6 87.0(2) . . ? C503 Ru5 Ru6 89.0(3) . . ? C9 Ru5 Ru6 91.17(17) . . ? C501 Ru5 Ru4 116.7(2) . . ? C502 Ru5 Ru4 138.1(3) . . ? C503 Ru5 Ru4 106.8(3) . . ? C9 Ru5 Ru4 68.04(17) . . ? Ru6 Ru5 Ru4 58.083(19) . . ? C604 Ru6 C603 98.9(5) . . ? C604 Ru6 C601 94.1(5) . . ? C603 Ru6 C601 92.3(4) . . ? C604 Ru6 C602 92.0(5) . . ? C603 Ru6 C602 93.9(4) . . ? C601 Ru6 C602 170.4(4) . . ? C604 Ru6 Ru4 98.7(3) . . ? C603 Ru6 Ru4 162.4(3) . . ? C601 Ru6 Ru4 86.9(2) . . ? C602 Ru6 Ru4 84.9(3) . . ? C604 Ru6 Ru5 161.2(3) . . ? C603 Ru6 Ru5 99.9(3) . . ? C601 Ru6 Ru5 85.7(3) . . ? C602 Ru6 Ru5 86.1(3) . . ? Ru4 Ru6 Ru5 62.473(18) . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 70.00 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 1.465 _refine_diff_density_min -0.761 _refine_diff_density_rms 0.109 # Attachment '- v37c.cif' data_v37c _database_code_depnum_ccdc_archive 'CCDC 871263' #TrackingRef '- v37c.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C18 H6 N2 O10 Ru3), C H2 Cl2' _chemical_formula_sum 'C37 H14 Cl2 N4 O20 Ru6' _chemical_formula_weight 1511.85 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0030 0.0020 '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' Cl Cl 0.1480 0.1590 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0060 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0110 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2590 0.8360 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' 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 39.17940(10) _cell_length_b 7.74830(10) _cell_length_c 16.9502(2) _cell_angle_alpha 90.00 _cell_angle_beta 112.3980(10) _cell_angle_gamma 90.00 _cell_volume 4757.44(8) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 6987 _cell_measurement_theta_min 2.6078 _cell_measurement_theta_max 73.7624 _exptl_crystal_description needle _exptl_crystal_colour orange _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.111 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2888 _exptl_absorpt_coefficient_mu 16.781 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.46995 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.54180 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'Enhance (Cu) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type Xcalibur _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11710 _diffrn_reflns_av_R_equivalents 0.0267 _diffrn_reflns_av_sigmaI/netI 0.0270 _diffrn_reflns_limit_h_min -46 _diffrn_reflns_limit_h_max 47 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 4.88 _diffrn_reflns_theta_max 69.97 _reflns_number_total 4403 _reflns_number_gt 3466 _reflns_threshold_expression >2\s(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'PLATON (Spek, 2008)' _computing_publication_material 'SHELXL-97 (Sheldrick, 2008)' _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^ > 2\s(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^)+(0.0569P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4403 _refine_ls_number_parameters 316 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0383 _refine_ls_R_factor_gt 0.0290 _refine_ls_wR_factor_ref 0.0870 _refine_ls_wR_factor_gt 0.0756 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.041 _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 C1 C 0.40576(12) 0.2247(6) 0.4750(3) 0.0490(10) Uani 1 1 d . . . C2 C 0.41540(13) 0.2023(7) 0.6198(3) 0.0615(12) Uani 1 1 d . . . H2 H 0.4044 0.2001 0.6597 0.074 Uiso 1 1 calc R . . C3 C 0.46667(13) 0.2016(7) 0.5895(3) 0.0622(12) Uani 1 1 d . . . C4 C 0.44510(11) 0.2212(6) 0.5015(3) 0.0504(10) Uani 1 1 d . . . C5 C 0.46372(13) 0.2374(7) 0.4449(4) 0.0642(13) Uani 1 1 d . . . H5 H 0.4502 0.2504 0.3867 0.077 Uiso 1 1 calc R . . C6 C 0.50166(14) 0.2340(8) 0.4753(4) 0.0759(16) Uani 1 1 d . . . H6 H 0.5137 0.2466 0.4378 0.091 Uiso 1 1 calc R . . C7 C 0.52211(14) 0.2118(9) 0.5619(4) 0.0793(17) Uani 1 1 d . . . H7 H 0.5477 0.2071 0.5813 0.095 Uiso 1 1 calc R . . C8 C 0.50559(14) 0.1970(9) 0.6185(4) 0.0751(15) Uani 1 1 d . . . H8 H 0.5198 0.1838 0.6763 0.090 Uiso 1 1 calc R . . C10 C 0.5000 0.4296(18) 0.2500 0.193(9) Uani 1 2 d S . . H10A H 0.4993 0.5038 0.2954 0.232 Uiso 0.50 1 calc PR . . H10B H 0.5007 0.5038 0.2046 0.232 Uiso 0.50 1 calc PR . . C101 C 0.34484(14) 0.4543(8) 0.5617(3) 0.0664(13) Uani 1 1 d . . . C102 C 0.32784(13) 0.0843(7) 0.5658(3) 0.0585(12) Uani 1 1 d . . . C103 C 0.28341(14) 0.2972(7) 0.4387(4) 0.0637(13) Uani 1 1 d . . . C201 C 0.38534(12) 0.0969(7) 0.3039(3) 0.0589(12) Uani 1 1 d . . . C202 C 0.38819(12) 0.4589(7) 0.3393(3) 0.0584(11) Uani 1 1 d . . . C203 C 0.32043(12) 0.3073(7) 0.2493(3) 0.0529(10) Uani 1 1 d . . . C301 C 0.37250(13) -0.1159(6) 0.4595(3) 0.0565(11) Uani 1 1 d . . . C302 C 0.29741(13) -0.1866(7) 0.4251(3) 0.0594(11) Uani 1 1 d . . . C303 C 0.32603(13) -0.1866(7) 0.2906(3) 0.0571(11) Uani 1 1 d . . . C304 C 0.27954(13) 0.0666(6) 0.3030(3) 0.0572(11) Uani 1 1 d . . . Cl1 Cl 0.46042(13) 0.3153(7) 0.2123(3) 0.228(2) Uani 1 1 d . . . N1 N 0.39259(10) 0.2170(5) 0.5363(2) 0.0519(9) Uani 1 1 d . . . N2 N 0.45072(11) 0.1912(7) 0.6484(3) 0.0708(12) Uani 1 1 d . . . O101 O 0.35175(14) 0.5703(6) 0.6058(3) 0.0945(14) Uani 1 1 d . . . O102 O 0.32372(12) -0.0129(6) 0.6100(2) 0.0797(11) Uani 1 1 d . . . O103 O 0.25300(10) 0.3293(7) 0.4103(3) 0.0952(14) Uani 1 1 d . . . O201 O 0.39949(11) 0.0023(6) 0.2749(3) 0.0829(12) Uani 1 1 d . . . O203 O 0.29683(9) 0.3428(5) 0.1883(2) 0.0736(10) Uani 1 1 d . . . O301 O 0.39978(10) -0.1720(6) 0.5040(3) 0.0834(12) Uani 1 1 d . . . O302 O 0.28150(12) -0.2765(6) 0.4512(3) 0.0841(12) Uani 1 1 d . . . O303 O 0.32639(13) -0.2736(5) 0.2368(3) 0.0808(11) Uani 1 1 d . . . O304 O 0.25185(9) 0.1147(6) 0.2563(3) 0.0804(11) Uani 1 1 d . . . 0202 O 0.40282(11) 0.5733(6) 0.3257(4) 0.0985(16) Uani 1 1 d . . . Ru2 Ru 0.363417(8) 0.25712(4) 0.35443(2) 0.03889(10) Uani 1 1 d . . . H100 H 0.3437(14) 0.371(7) 0.408(4) 0.077(16) Uiso 1 1 d . . . Ru1 Ru 0.334753(9) 0.25137(4) 0.48900(2) 0.04416(11) Uani 1 1 d . . . Ru3 Ru 0.324692(8) -0.03824(4) 0.37965(2) 0.04353(11) 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 C1 0.047(2) 0.058(3) 0.038(2) -0.0043(19) 0.0122(18) 0.0000(19) C2 0.056(3) 0.084(3) 0.038(2) 0.002(2) 0.010(2) -0.005(2) C3 0.045(2) 0.075(3) 0.058(3) -0.008(3) 0.010(2) 0.001(2) C4 0.0374(19) 0.062(3) 0.044(2) -0.002(2) 0.0075(18) 0.0001(19) C5 0.043(2) 0.081(4) 0.063(3) -0.002(3) 0.014(2) -0.002(2) C6 0.046(3) 0.100(4) 0.080(4) -0.013(3) 0.023(3) -0.006(3) C7 0.041(2) 0.109(5) 0.078(4) -0.022(4) 0.013(3) -0.003(3) C8 0.049(2) 0.099(4) 0.060(3) -0.019(3) 0.001(2) 0.000(3) C10 0.26(2) 0.089(9) 0.172(18) 0.000 0.016(16) 0.000 C101 0.059(3) 0.084(4) 0.058(3) 0.004(3) 0.024(2) 0.011(3) C102 0.054(2) 0.071(3) 0.048(3) -0.001(2) 0.017(2) 0.010(2) C103 0.050(3) 0.071(3) 0.072(3) 0.004(3) 0.026(2) 0.007(2) C201 0.046(2) 0.072(3) 0.055(3) -0.003(2) 0.014(2) -0.004(2) C202 0.050(2) 0.059(3) 0.060(3) 0.006(2) 0.015(2) -0.003(2) C203 0.046(2) 0.064(3) 0.049(3) 0.006(2) 0.017(2) 0.000(2) C301 0.055(2) 0.054(2) 0.053(3) 0.002(2) 0.012(2) 0.008(2) C302 0.054(2) 0.063(3) 0.051(3) 0.009(2) 0.009(2) -0.006(2) C303 0.054(2) 0.052(3) 0.056(3) 0.008(2) 0.011(2) 0.007(2) C304 0.050(2) 0.057(3) 0.061(3) 0.009(2) 0.017(2) 0.000(2) Cl1 0.259(5) 0.296(5) 0.157(3) -0.077(3) 0.109(3) -0.125(4) N1 0.0445(18) 0.069(2) 0.0393(19) -0.0007(17) 0.0123(15) 0.0006(17) N2 0.052(2) 0.103(3) 0.046(2) -0.002(2) 0.0055(18) 0.000(2) O101 0.108(3) 0.088(3) 0.084(3) -0.032(3) 0.032(3) 0.005(3) O102 0.096(3) 0.093(3) 0.054(2) 0.020(2) 0.033(2) -0.006(2) O103 0.050(2) 0.121(4) 0.109(4) 0.003(3) 0.024(2) 0.015(2) O201 0.069(2) 0.099(3) 0.087(3) -0.027(2) 0.038(2) 0.010(2) O203 0.0572(18) 0.092(3) 0.054(2) 0.007(2) 0.0020(17) 0.0005(19) O301 0.059(2) 0.083(3) 0.090(3) 0.015(2) 0.008(2) 0.016(2) O302 0.080(3) 0.087(3) 0.084(3) 0.021(2) 0.029(2) -0.016(2) O303 0.095(3) 0.072(2) 0.074(3) -0.013(2) 0.030(2) 0.004(2) O304 0.0510(18) 0.095(3) 0.081(3) 0.025(2) 0.0088(18) 0.0129(19) 0202 0.073(2) 0.081(3) 0.131(4) 0.018(3) 0.027(3) -0.027(2) Ru2 0.03405(17) 0.04573(19) 0.03397(18) -0.00075(13) 0.00970(13) -0.00102(12) Ru1 0.03941(18) 0.0543(2) 0.03905(19) -0.00130(15) 0.01524(14) 0.00339(14) Ru3 0.03743(16) 0.04387(18) 0.04409(18) 0.00195(15) 0.00972(13) -0.00026(14) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 C1 N1 1.327(6) . ? C1 C4 1.432(6) . ? C1 Ru2 2.099(4) . ? C2 N2 1.283(6) . ? C2 N1 1.360(6) . ? C3 N2 1.367(7) . ? C3 C8 1.413(7) . ? C3 C4 1.414(7) . ? C4 C5 1.415(7) . ? C5 C6 1.376(7) . ? C6 C7 1.389(9) . ? C7 C8 1.351(9) . ? C10 Cl1 1.686(8) . ? C10 Cl1 1.686(8) 2_655 ? C101 O101 1.133(7) . ? C101 Ru1 1.944(6) . ? C102 O102 1.117(6) . ? C102 Ru1 1.926(5) . ? C103 O103 1.130(6) . ? C103 Ru1 1.895(5) . ? C201 O201 1.137(6) . ? C201 Ru2 1.891(5) . ? C202 0202 1.126(6) . ? C202 Ru2 1.908(5) . ? C203 O203 1.127(6) . ? C203 Ru2 1.969(5) . ? C301 O301 1.134(6) . ? C301 Ru3 1.942(5) . ? C302 O302 1.132(6) . ? C302 Ru3 1.919(5) . ? C303 O303 1.138(7) . ? C303 Ru3 1.914(6) . ? C304 O304 1.135(6) . ? C304 Ru3 1.930(5) . ? N1 Ru1 2.113(4) . ? Ru2 Ru3 2.8664(4) . ? Ru2 Ru1 2.9014(5) . ? Ru1 Ru3 2.8407(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C4 116.5(4) . . ? N1 C1 Ru2 111.7(3) . . ? C4 C1 Ru2 131.7(3) . . ? N2 C2 N1 125.9(5) . . ? N2 C3 C8 118.5(5) . . ? N2 C3 C4 121.4(4) . . ? C8 C3 C4 120.1(5) . . ? C3 C4 C5 118.0(4) . . ? C3 C4 C1 118.2(4) . . ? C5 C4 C1 123.8(4) . . ? C6 C5 C4 120.4(5) . . ? C5 C6 C7 120.3(6) . . ? C8 C7 C6 121.4(5) . . ? C7 C8 C3 119.7(5) . . ? Cl1 C10 Cl1 116.6(9) . 2_655 ? O101 C101 Ru1 177.8(5) . . ? O102 C102 Ru1 179.7(6) . . ? O103 C103 Ru1 177.7(6) . . ? O201 C201 Ru2 178.0(4) . . ? 0202 C202 Ru2 175.5(5) . . ? O203 C203 Ru2 176.4(4) . . ? O301 C301 Ru3 175.4(5) . . ? O302 C302 Ru3 178.8(6) . . ? O303 C303 Ru3 179.0(5) . . ? O304 C304 Ru3 174.3(5) . . ? C1 N1 C2 121.4(4) . . ? C1 N1 Ru1 112.2(3) . . ? C2 N1 Ru1 126.2(3) . . ? C2 N2 C3 116.6(4) . . ? C201 Ru2 C202 97.8(2) . . ? C201 Ru2 C203 95.7(2) . . ? C202 Ru2 C203 91.2(2) . . ? C201 Ru2 C1 92.04(19) . . ? C202 Ru2 C1 88.56(19) . . ? C203 Ru2 C1 172.25(18) . . ? C201 Ru2 Ru3 84.32(15) . . ? C202 Ru2 Ru3 177.91(15) . . ? C203 Ru2 Ru3 88.49(14) . . ? C1 Ru2 Ru3 91.51(13) . . ? C201 Ru2 Ru1 136.47(16) . . ? C202 Ru2 Ru1 119.15(16) . . ? C203 Ru2 Ru1 105.12(13) . . ? C1 Ru2 Ru1 68.42(12) . . ? Ru3 Ru2 Ru1 59.008(11) . . ? C103 Ru1 C102 91.8(2) . . ? C103 Ru1 C101 93.3(2) . . ? C102 Ru1 C101 99.3(2) . . ? C103 Ru1 N1 174.5(2) . . ? C102 Ru1 N1 93.74(17) . . ? C101 Ru1 N1 86.08(18) . . ? C103 Ru1 Ru3 89.71(18) . . ? C102 Ru1 Ru3 83.66(15) . . ? C101 Ru1 Ru3 175.66(15) . . ? N1 Ru1 Ru3 90.60(11) . . ? C103 Ru1 Ru2 107.83(17) . . ? C102 Ru1 Ru2 137.52(14) . . ? C101 Ru1 Ru2 116.12(16) . . ? N1 Ru1 Ru2 67.68(10) . . ? Ru3 Ru1 Ru2 59.882(11) . . ? C303 Ru3 C302 98.2(2) . . ? C303 Ru3 C304 90.9(2) . . ? C302 Ru3 C304 90.8(2) . . ? C303 Ru3 C301 93.1(2) . . ? C302 Ru3 C301 94.1(2) . . ? C304 Ru3 C301 173.1(2) . . ? C303 Ru3 Ru1 161.89(15) . . ? C302 Ru3 Ru1 99.86(17) . . ? C304 Ru3 Ru1 88.29(15) . . ? C301 Ru3 Ru1 86.13(15) . . ? C303 Ru3 Ru2 100.78(15) . . ? C302 Ru3 Ru2 160.96(17) . . ? C304 Ru3 Ru2 88.01(14) . . ? C301 Ru3 Ru2 85.79(15) . . ? Ru1 Ru3 Ru2 61.110(11) . . ? _diffrn_measured_fraction_theta_max 0.973 _diffrn_reflns_theta_full 69.97 _diffrn_measured_fraction_theta_full 0.973 _refine_diff_density_max 0.602 _refine_diff_density_min -0.672 _refine_diff_density_rms 0.108 # Attachment '- v40b.cif' data_v40b _database_code_depnum_ccdc_archive 'CCDC 871264' #TrackingRef '- v40b.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C25 H12 N4 O9 Ru3), C3 H6 O' _chemical_formula_sum 'C53 H30 N8 O19 Ru6' _chemical_formula_weight 1689.27 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting TRICLINIC _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.9629(3) _cell_length_b 14.4595(3) _cell_length_c 15.7626(4) _cell_angle_alpha 79.6630(10) _cell_angle_beta 88.8720(10) _cell_angle_gamma 74.6150(10) _cell_volume 2801.17(11) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 8161 _cell_measurement_theta_min 0.407 _cell_measurement_theta_max 25.350 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.003 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1640 _exptl_absorpt_coefficient_mu 1.659 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7325 _exptl_absorpt_correction_T_max 0.8927 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _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 'horizonally mounted graphite crystal' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10249 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0539 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.31 _diffrn_reflns_theta_max 25.34 _reflns_number_total 10249 _reflns_number_gt 8499 _reflns_threshold_expression >2\s(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'PLATON (Spek, 2008)' _computing_publication_material 'SHELXL-97 (Sheldrick, 2008)' _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^ > 2\s(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^)+(0.0680P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10249 _refine_ls_number_parameters 777 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0435 _refine_ls_R_factor_gt 0.0289 _refine_ls_wR_factor_ref 0.1140 _refine_ls_wR_factor_gt 0.0813 _refine_ls_goodness_of_fit_ref 1.082 _refine_ls_restrained_S_all 1.082 _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 C1 C -0.1302(4) 0.0901(4) 0.3756(3) 0.0181(11) Uani 1 1 d . . . H1 H -0.1021 0.0245 0.3682 0.022 Uiso 1 1 calc R . . C2 C -0.2425(4) 0.1250(4) 0.3828(3) 0.0196(11) Uani 1 1 d . . . C3 C -0.3132(4) 0.0671(4) 0.3816(4) 0.0254(13) Uani 1 1 d . . . H3 H -0.2876 0.0011 0.3748 0.030 Uiso 1 1 calc R . . C4 C -0.4200(4) 0.1076(4) 0.3905(4) 0.0372(16) Uani 1 1 d . . . H4 H -0.4685 0.0685 0.3908 0.045 Uiso 1 1 calc R . . C5 C -0.4597(4) 0.2055(4) 0.3993(4) 0.0372(16) Uani 1 1 d . . . H5 H -0.5346 0.2321 0.4032 0.045 Uiso 1 1 calc R . . C6 C -0.3921(4) 0.2629(4) 0.4022(4) 0.0320(14) Uani 1 1 d . . . H6 H -0.4191 0.3287 0.4094 0.038 Uiso 1 1 calc R . . C7 C -0.2805(4) 0.2224(4) 0.3943(3) 0.0196(12) Uani 1 1 d . . . C8 C -0.2047(4) 0.2749(4) 0.3982(3) 0.0193(11) Uani 1 1 d . . . H7 H -0.2292 0.3405 0.4066 0.023 Uiso 1 1 calc R . . C9 C -0.1616(4) 0.1273(4) 0.1592(4) 0.0253(13) Uani 1 1 d . . . H9 H -0.1566 0.0637 0.1484 0.030 Uiso 1 1 calc R . . C10 C -0.2635(4) 0.1952(4) 0.1484(4) 0.0229(12) Uani 1 1 d . . . C11 C -0.3565(4) 0.1748(4) 0.1223(4) 0.0282(13) Uani 1 1 d . . . H11 H -0.3543 0.1112 0.1132 0.034 Uiso 1 1 calc R . . C12 C -0.4508(4) 0.2470(4) 0.1100(4) 0.0363(15) Uani 1 1 d . . . H12 H -0.5138 0.2335 0.0916 0.044 Uiso 1 1 calc R . . C13 C -0.4544(4) 0.3401(5) 0.1244(4) 0.0399(16) Uani 1 1 d . . . H13 H -0.5202 0.3896 0.1157 0.048 Uiso 1 1 calc R . . C14 C -0.3654(4) 0.3616(4) 0.1508(4) 0.0341(15) Uani 1 1 d . . . H14 H -0.3695 0.4254 0.1607 0.041 Uiso 1 1 calc R . . C15 C -0.2679(4) 0.2897(4) 0.1632(4) 0.0237(12) Uani 1 1 d . . . C16 C -0.1700(4) 0.3039(4) 0.1882(3) 0.0211(12) Uani 1 1 d . . . H16 H -0.1710 0.3669 0.1985 0.025 Uiso 1 1 calc R . . C17 C 0.3745(4) -0.3291(4) 0.3572(4) 0.0227(12) Uani 1 1 d . . . H17 H 0.3964 -0.3875 0.3987 0.027 Uiso 1 1 calc R . . C18 C 0.2660(4) -0.2966(4) 0.3284(4) 0.0222(12) Uani 1 1 d . . . C19 C 0.1916(4) -0.3498(4) 0.3540(4) 0.0341(15) Uani 1 1 d . . . H19 H 0.2118 -0.4091 0.3945 0.041 Uiso 1 1 calc R . . C20 C 0.0892(4) -0.3155(5) 0.3201(4) 0.0416(17) Uani 1 1 d . . . H20 H 0.0387 -0.3521 0.3365 0.050 Uiso 1 1 calc R . . C21 C 0.0579(4) -0.2269(5) 0.2615(4) 0.0360(15) Uani 1 1 d . . . H21 H -0.0141 -0.2035 0.2401 0.043 Uiso 1 1 calc R . . C22 C 0.1296(4) -0.1734(4) 0.2345(4) 0.0299(14) Uani 1 1 d . . . H22 H 0.1084 -0.1141 0.1941 0.036 Uiso 1 1 calc R . . C23 C 0.2354(4) -0.2089(4) 0.2685(4) 0.0222(12) Uani 1 1 d . . . C24 C 0.3166(4) -0.1615(4) 0.2422(4) 0.0208(12) Uani 1 1 d . . . H24 H 0.2980 -0.1018 0.2020 0.025 Uiso 1 1 calc R . . C25 C 0.3809(4) -0.4826(4) 0.2197(4) 0.0319(14) Uani 1 1 d . . . H25 H 0.3806 -0.5421 0.2569 0.038 Uiso 1 1 calc R . . C26 C 0.2908(4) -0.4373(4) 0.1628(4) 0.0265(13) Uani 1 1 d . . . C27 C 0.2005(4) -0.4743(4) 0.1587(5) 0.0394(16) Uani 1 1 d . . . H27 H 0.1976 -0.5340 0.1943 0.047 Uiso 1 1 calc R . . C28 C 0.1176(4) -0.4227(4) 0.1028(4) 0.0361(15) Uani 1 1 d . . . H28 H 0.0576 -0.4479 0.0984 0.043 Uiso 1 1 calc R . . C29 C 0.1195(4) -0.3344(4) 0.0523(4) 0.0323(14) Uani 1 1 d . . . H29 H 0.0605 -0.3000 0.0142 0.039 Uiso 1 1 calc R . . C30 C 0.2042(4) -0.2953(4) 0.0559(4) 0.0290(13) Uani 1 1 d . . . H30 H 0.2035 -0.2337 0.0220 0.035 Uiso 1 1 calc R . . C31 C 0.2920(4) -0.3479(4) 0.1106(4) 0.0219(12) Uani 1 1 d . . . C32 C 0.3850(4) -0.3150(4) 0.1181(4) 0.0221(12) Uani 1 1 d . . . H32 H 0.3886 -0.2554 0.0827 0.026 Uiso 1 1 calc R . . C33 C -0.2827(5) -0.0669(5) -0.0204(4) 0.0409(16) Uani 1 1 d . . . H33A H -0.3477 -0.0134 -0.0356 0.061 Uiso 1 1 calc R . . H33B H -0.2913 -0.1063 0.0354 0.061 Uiso 1 1 calc R . . H33C H -0.2704 -0.1078 -0.0648 0.061 Uiso 1 1 calc R . . C34 C -0.1897(5) -0.0260(4) -0.0146(4) 0.0328(14) Uani 1 1 d . . . C35 C -0.0836(5) -0.0982(5) 0.0085(5) 0.0427(16) Uani 1 1 d . . . H35A H -0.0535 -0.1233 -0.0429 0.064 Uiso 1 1 calc R . . H35B H -0.0929 -0.1522 0.0527 0.064 Uiso 1 1 calc R . . H35C H -0.0348 -0.0663 0.0311 0.064 Uiso 1 1 calc R . . C101 C -0.0477(4) 0.3969(4) 0.4580(4) 0.0234(12) Uani 1 1 d . . . C102 C 0.1552(4) 0.3396(4) 0.4094(4) 0.0259(13) Uani 1 1 d . . . C103 C 0.0040(4) 0.3896(4) 0.2732(4) 0.0188(11) Uani 1 1 d . . . C201 C 0.1220(4) -0.0292(4) 0.4127(3) 0.0158(11) Uani 1 1 d . . . C202 C 0.2574(4) 0.0807(4) 0.3923(4) 0.0230(12) Uani 1 1 d . . . C203 C 0.0908(4) 0.1717(4) 0.4925(4) 0.0202(12) Uani 1 1 d . . . C301 C 0.0927(4) 0.3045(4) 0.1111(4) 0.0239(12) Uani 1 1 d . . . C302 C 0.2184(4) 0.2658(4) 0.2457(3) 0.0210(12) Uani 1 1 d . . . C303 C 0.1349(4) 0.1044(4) 0.2442(4) 0.0197(12) Uani 1 1 d . . . C401 C 0.6513(4) -0.3883(4) 0.0737(4) 0.0294(14) Uani 1 1 d . . . C402 C 0.7592(4) -0.3083(4) 0.1648(4) 0.0245(12) Uani 1 1 d . . . C403 C 0.6663(4) -0.4380(4) 0.2787(4) 0.0236(12) Uani 1 1 d . . . C501 C 0.6075(4) -0.3993(4) 0.4601(4) 0.0220(12) Uani 1 1 d . . . C502 C 0.7625(4) -0.3353(4) 0.3674(4) 0.0241(12) Uani 1 1 d . . . C503 C 0.5878(4) -0.1769(4) 0.3739(4) 0.0234(12) Uani 1 1 d . . . C601 C 0.6822(4) -0.1109(4) 0.2176(3) 0.0207(12) Uani 1 1 d . . . C602 C 0.4762(4) -0.0123(4) 0.2159(4) 0.0245(12) Uani 1 1 d . . . C603 C 0.5461(4) -0.1778(4) 0.1099(4) 0.0221(12) Uani 1 1 d . . . N1 N -0.1010(3) 0.2379(3) 0.3907(3) 0.0157(9) Uani 1 1 d . . . N2 N -0.0631(3) 0.1429(3) 0.3786(3) 0.0140(9) Uani 1 1 d . . . N3 N -0.0791(3) 0.2383(3) 0.1982(3) 0.0201(10) Uani 1 1 d . . . N4 N -0.0739(3) 0.1450(3) 0.1828(3) 0.0250(11) Uani 1 1 d . . . N5 N 0.4156(3) -0.1962(3) 0.2707(3) 0.0167(9) Uani 1 1 d . . . N6 N 0.4461(3) -0.2826(3) 0.3295(3) 0.0175(9) Uani 1 1 d . . . N7 N 0.4664(3) -0.3624(3) 0.1714(3) 0.0228(10) Uani 1 1 d . . . N8 N 0.4638(3) -0.4489(3) 0.2248(3) 0.0272(11) Uani 1 1 d . . . O99 O -0.1986(4) 0.0615(3) -0.0286(3) 0.0500(12) Uani 1 1 d . . . O101 O -0.0954(3) 0.4589(3) 0.4900(3) 0.0378(11) Uani 1 1 d . . . O102 O 0.2314(3) 0.3637(3) 0.4167(3) 0.0405(11) Uani 1 1 d . . . O103 O -0.0317(3) 0.4716(3) 0.2444(3) 0.0324(10) Uani 1 1 d . . . O201 O 0.1339(3) -0.1117(3) 0.4286(2) 0.0283(9) Uani 1 1 d . . . O202 O 0.3472(3) 0.0627(3) 0.4030(3) 0.0399(11) Uani 1 1 d . . . O203 O 0.1147(3) 0.1493(3) 0.5658(3) 0.0281(9) Uani 1 1 d . . . O301 O 0.1084(3) 0.3363(3) 0.0417(3) 0.0434(11) Uani 1 1 d . . . O302 O 0.3040(3) 0.2721(3) 0.2528(3) 0.0330(10) Uani 1 1 d . . . O303 O 0.1752(3) 0.0443(3) 0.2040(2) 0.0276(9) Uani 1 1 d . . . O401 O 0.6716(3) -0.4242(4) 0.0154(3) 0.0516(13) Uani 1 1 d . . . O402 O 0.8445(3) -0.2987(3) 0.1598(3) 0.0342(10) Uani 1 1 d . . . O403 O 0.7109(3) -0.5199(3) 0.2966(3) 0.0333(10) Uani 1 1 d . . . O501 O 0.6008(3) -0.4490(3) 0.5236(3) 0.0411(11) Uani 1 1 d . . . O502 O 0.8510(3) -0.3415(3) 0.3776(3) 0.0345(10) Uani 1 1 d . . . O503 O 0.5978(3) -0.1336(3) 0.4273(3) 0.0341(10) Uani 1 1 d . . . O601 O 0.7603(3) -0.0868(3) 0.2083(3) 0.0358(10) Uani 1 1 d . . . O602 O 0.4314(3) 0.0680(3) 0.2052(3) 0.0394(11) Uani 1 1 d . . . O603 O 0.5117(3) -0.1380(3) 0.0418(3) 0.0288(9) Uani 1 1 d . . . Ru1 Ru 0.03046(3) 0.29895(3) 0.39748(3) 0.01534(11) Uani 1 1 d . . . Ru2 Ru 0.10773(3) 0.10637(3) 0.37904(3) 0.01458(11) Uani 1 1 d . . . Ru3 Ru 0.07948(3) 0.25651(3) 0.22916(3) 0.01544(11) Uani 1 1 d . . . Ru4 Ru 0.62213(3) -0.32634(3) 0.17106(3) 0.01812(12) Uani 1 1 d . . . Ru5 Ru 0.61501(3) -0.31979(3) 0.35131(3) 0.01693(12) Uani 1 1 d . . . Ru6 Ru 0.55410(3) -0.14683(3) 0.23563(3) 0.01705(12) 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 C1 0.019(3) 0.020(3) 0.016(3) -0.002(2) 0.003(2) -0.007(2) C2 0.017(3) 0.028(3) 0.014(3) 0.002(2) -0.001(2) -0.010(2) C3 0.022(3) 0.028(3) 0.031(4) -0.003(3) 0.000(2) -0.015(2) C4 0.021(3) 0.042(4) 0.051(5) -0.003(3) -0.005(3) -0.017(3) C5 0.011(3) 0.047(4) 0.050(4) 0.000(3) -0.003(3) -0.005(3) C6 0.019(3) 0.031(3) 0.041(4) -0.001(3) 0.002(3) -0.002(2) C7 0.012(2) 0.022(3) 0.021(3) 0.005(2) -0.001(2) -0.003(2) C8 0.015(3) 0.019(3) 0.019(3) 0.000(2) -0.002(2) 0.001(2) C9 0.026(3) 0.026(3) 0.028(3) -0.010(3) 0.002(2) -0.010(2) C10 0.024(3) 0.026(3) 0.019(3) -0.001(2) 0.004(2) -0.009(2) C11 0.025(3) 0.032(3) 0.033(4) -0.011(3) 0.000(3) -0.014(3) C12 0.025(3) 0.051(4) 0.038(4) -0.016(3) 0.000(3) -0.013(3) C13 0.022(3) 0.046(4) 0.052(5) -0.023(3) -0.010(3) 0.000(3) C14 0.025(3) 0.027(3) 0.047(4) -0.013(3) -0.007(3) 0.003(2) C15 0.025(3) 0.029(3) 0.020(3) -0.009(2) -0.004(2) -0.009(2) C16 0.024(3) 0.026(3) 0.016(3) -0.008(2) -0.001(2) -0.009(2) C17 0.019(3) 0.025(3) 0.023(3) 0.002(2) 0.002(2) -0.007(2) C18 0.014(3) 0.028(3) 0.024(3) -0.006(3) 0.004(2) -0.004(2) C19 0.022(3) 0.041(4) 0.038(4) 0.005(3) 0.007(3) -0.014(3) C20 0.022(3) 0.055(4) 0.050(5) -0.002(4) 0.010(3) -0.017(3) C21 0.015(3) 0.054(4) 0.040(4) -0.011(3) 0.001(3) -0.010(3) C22 0.020(3) 0.039(3) 0.031(4) -0.009(3) -0.003(2) -0.005(3) C23 0.012(2) 0.027(3) 0.027(3) -0.011(3) -0.001(2) -0.001(2) C24 0.016(3) 0.018(3) 0.027(3) -0.004(2) 0.000(2) -0.001(2) C25 0.023(3) 0.022(3) 0.051(4) -0.004(3) 0.001(3) -0.006(2) C26 0.021(3) 0.020(3) 0.040(4) -0.005(3) 0.002(3) -0.009(2) C27 0.027(3) 0.032(3) 0.061(5) -0.002(3) 0.000(3) -0.014(3) C28 0.025(3) 0.036(4) 0.052(5) -0.010(3) 0.001(3) -0.016(3) C29 0.024(3) 0.038(4) 0.037(4) -0.009(3) -0.006(3) -0.011(3) C30 0.029(3) 0.034(3) 0.025(4) -0.005(3) 0.000(3) -0.012(3) C31 0.021(3) 0.026(3) 0.021(3) -0.008(2) 0.003(2) -0.007(2) C32 0.025(3) 0.022(3) 0.022(3) -0.004(2) 0.004(2) -0.010(2) C33 0.036(4) 0.051(4) 0.033(4) 0.003(3) 0.004(3) -0.014(3) C34 0.037(3) 0.040(4) 0.022(4) -0.004(3) 0.005(3) -0.013(3) C35 0.036(4) 0.047(4) 0.045(4) -0.001(3) 0.000(3) -0.014(3) C101 0.022(3) 0.025(3) 0.027(3) -0.006(3) 0.003(2) -0.012(2) C102 0.030(3) 0.026(3) 0.022(3) -0.009(3) 0.005(2) -0.006(3) C103 0.013(2) 0.018(3) 0.027(3) -0.004(2) -0.003(2) -0.009(2) C201 0.012(2) 0.023(3) 0.012(3) -0.002(2) 0.001(2) -0.003(2) C202 0.020(3) 0.027(3) 0.023(3) -0.004(2) 0.002(2) -0.008(2) C203 0.015(3) 0.023(3) 0.026(4) -0.007(3) 0.004(2) -0.010(2) C301 0.019(3) 0.034(3) 0.022(4) -0.006(3) -0.001(2) -0.012(2) C302 0.024(3) 0.017(3) 0.020(3) -0.002(2) 0.004(2) -0.003(2) C303 0.014(2) 0.022(3) 0.023(3) -0.002(2) -0.001(2) -0.006(2) C401 0.019(3) 0.032(3) 0.037(4) -0.011(3) 0.002(3) -0.004(2) C402 0.027(3) 0.024(3) 0.023(3) -0.007(2) 0.004(2) -0.005(2) C403 0.016(3) 0.023(3) 0.031(4) -0.005(3) -0.005(2) -0.004(2) C501 0.014(3) 0.026(3) 0.027(4) 0.000(3) -0.002(2) -0.010(2) C502 0.024(3) 0.023(3) 0.024(3) -0.003(2) -0.002(2) -0.005(2) C503 0.018(3) 0.023(3) 0.029(4) -0.001(3) 0.001(2) -0.009(2) C601 0.027(3) 0.018(3) 0.017(3) -0.001(2) 0.003(2) -0.006(2) C602 0.026(3) 0.025(3) 0.026(3) -0.006(3) 0.002(2) -0.010(3) C603 0.014(3) 0.027(3) 0.029(4) -0.007(3) 0.003(2) -0.010(2) N1 0.013(2) 0.015(2) 0.019(3) -0.0027(18) 0.0024(17) -0.0033(17) N2 0.013(2) 0.011(2) 0.018(2) -0.0015(17) 0.0006(17) -0.0035(16) N3 0.021(2) 0.021(2) 0.019(3) -0.005(2) 0.0022(19) -0.0069(19) N4 0.023(2) 0.022(2) 0.031(3) -0.009(2) 0.000(2) -0.0066(19) N5 0.015(2) 0.013(2) 0.020(3) -0.0011(18) -0.0004(18) -0.0011(17) N6 0.014(2) 0.018(2) 0.020(3) -0.0015(19) -0.0001(18) -0.0050(17) N7 0.019(2) 0.021(2) 0.029(3) -0.008(2) 0.003(2) -0.0055(19) N8 0.021(2) 0.017(2) 0.040(3) 0.001(2) -0.003(2) -0.0038(19) O99 0.063(3) 0.031(3) 0.056(3) -0.010(2) 0.004(3) -0.011(2) O101 0.047(3) 0.026(2) 0.045(3) -0.017(2) 0.020(2) -0.0110(19) O102 0.032(2) 0.058(3) 0.046(3) -0.020(2) 0.004(2) -0.032(2) O103 0.044(2) 0.017(2) 0.032(3) 0.0008(18) 0.0054(19) -0.0043(18) O201 0.041(2) 0.017(2) 0.025(2) -0.0024(17) 0.0020(18) -0.0061(17) O202 0.012(2) 0.061(3) 0.045(3) -0.004(2) -0.0003(18) -0.0103(19) O203 0.037(2) 0.024(2) 0.022(3) -0.0020(18) -0.0053(18) -0.0068(17) O301 0.049(3) 0.069(3) 0.020(3) 0.001(2) 0.001(2) -0.034(2) O302 0.017(2) 0.039(2) 0.047(3) -0.010(2) 0.0026(18) -0.0120(18) O303 0.031(2) 0.022(2) 0.027(2) -0.0078(18) 0.0042(18) -0.0008(16) O401 0.040(3) 0.073(3) 0.050(3) -0.041(3) 0.010(2) -0.012(2) O402 0.021(2) 0.039(2) 0.044(3) -0.007(2) 0.0043(19) -0.0093(18) O403 0.031(2) 0.017(2) 0.048(3) -0.0059(19) -0.0050(19) -0.0002(18) O501 0.041(3) 0.045(3) 0.035(3) 0.017(2) -0.009(2) -0.023(2) O502 0.016(2) 0.046(3) 0.041(3) -0.005(2) -0.0023(18) -0.0105(18) O503 0.046(3) 0.032(2) 0.028(3) -0.009(2) -0.0013(19) -0.0145(19) O601 0.028(2) 0.033(2) 0.051(3) -0.006(2) 0.006(2) -0.0182(19) O602 0.039(2) 0.019(2) 0.056(3) -0.006(2) -0.003(2) -0.0011(19) O603 0.031(2) 0.029(2) 0.024(3) 0.0019(19) -0.0044(18) -0.0080(17) Ru1 0.0138(2) 0.0152(2) 0.0186(3) -0.00462(18) 0.00119(17) -0.00563(16) Ru2 0.0096(2) 0.0145(2) 0.0192(3) -0.00217(17) 0.00026(16) -0.00292(16) Ru3 0.0127(2) 0.0166(2) 0.0171(2) -0.00244(18) 0.00068(16) -0.00444(16) Ru4 0.0139(2) 0.0179(2) 0.0229(3) -0.00521(19) 0.00130(17) -0.00390(17) Ru5 0.0120(2) 0.0172(2) 0.0204(3) 0.00021(18) -0.00120(17) -0.00412(16) Ru6 0.0148(2) 0.0138(2) 0.0222(3) -0.00144(18) 0.00085(17) -0.00434(16) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 C1 N2 1.306(6) . ? C1 C2 1.418(7) . ? C1 H1 0.9500 . ? C2 C3 1.398(7) . ? C2 C7 1.407(7) . ? C3 C4 1.368(7) . ? C3 H3 0.9500 . ? C4 C5 1.402(8) . ? C4 H4 0.9500 . ? C5 C6 1.364(8) . ? C5 H5 0.9500 . ? C6 C7 1.421(7) . ? C6 H6 0.9500 . ? C7 C8 1.400(7) . ? C8 N1 1.319(6) . ? C8 H7 0.9500 . ? C9 N4 1.305(6) . ? C9 C10 1.413(7) . ? C9 H9 0.9500 . ? C10 C11 1.400(7) . ? C10 C15 1.414(7) . ? C11 C12 1.371(8) . ? C11 H11 0.9500 . ? C12 C13 1.395(8) . ? C12 H12 0.9500 . ? C13 C14 1.362(8) . ? C13 H13 0.9500 . ? C14 C15 1.399(7) . ? C14 H14 0.9500 . ? C15 C16 1.412(7) . ? C16 N3 1.295(6) . ? C16 H16 0.9500 . ? C17 N6 1.310(6) . ? C17 C18 1.415(7) . ? C17 H17 0.9500 . ? C18 C19 1.397(7) . ? C18 C23 1.407(8) . ? C19 C20 1.371(8) . ? C19 H19 0.9500 . ? C20 C21 1.405(9) . ? C20 H20 0.9500 . ? C21 C22 1.375(8) . ? C21 H21 0.9500 . ? C22 C23 1.410(7) . ? C22 H22 0.9500 . ? C23 C24 1.418(7) . ? C24 N5 1.305(6) . ? C24 H24 0.9500 . ? C25 N8 1.301(7) . ? C25 C26 1.423(8) . ? C25 H25 0.9500 . ? C26 C31 1.406(8) . ? C26 C27 1.418(7) . ? C27 C28 1.365(9) . ? C27 H27 0.9500 . ? C28 C29 1.385(8) . ? C28 H28 0.9500 . ? C29 C30 1.369(7) . ? C29 H29 0.9500 . ? C30 C31 1.400(8) . ? C30 H30 0.9500 . ? C31 C32 1.423(7) . ? C32 N7 1.316(7) . ? C32 H32 0.9500 . ? C33 C34 1.488(8) . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 O99 1.219(7) . ? C34 C35 1.495(8) . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C101 O101 1.139(6) . ? C101 Ru1 1.904(5) . ? C102 O102 1.145(6) . ? C102 Ru1 1.884(6) . ? C103 O103 1.161(6) . ? C103 Ru1 2.131(6) . ? C103 Ru3 2.144(5) . ? C201 O201 1.143(6) . ? C201 Ru2 1.897(5) . ? C202 O202 1.132(6) . ? C202 Ru2 1.885(5) . ? C203 O203 1.167(6) . ? C203 Ru1 2.130(6) . ? C203 Ru2 2.150(5) . ? C301 O301 1.144(7) . ? C301 Ru3 1.887(6) . ? C302 O302 1.147(6) . ? C302 Ru3 1.867(5) . ? C303 O303 1.172(6) . ? C303 Ru3 2.096(5) . ? C303 Ru2 2.151(5) . ? C401 O401 1.128(7) . ? C401 Ru4 1.895(6) . ? C402 O402 1.149(6) . ? C402 Ru4 1.862(5) . ? C403 O403 1.158(6) . ? C403 Ru4 2.092(6) . ? C403 Ru5 2.177(5) . ? C501 O501 1.139(6) . ? C501 Ru5 1.903(6) . ? C502 O502 1.138(6) . ? C502 Ru5 1.882(5) . ? C503 O503 1.163(6) . ? C503 Ru5 2.096(5) . ? C503 Ru6 2.173(6) . ? C601 O601 1.154(6) . ? C601 Ru6 1.869(5) . ? C602 O602 1.135(6) . ? C602 Ru6 1.911(5) . ? C603 O603 1.159(7) . ? C603 Ru6 2.120(6) . ? C603 Ru4 2.164(6) . ? N1 N2 1.377(5) . ? N1 Ru1 2.130(4) . ? N2 Ru2 2.136(4) . ? N3 N4 1.397(6) . ? N3 Ru3 2.215(4) . ? N5 N6 1.383(6) . ? N5 Ru6 2.130(4) . ? N6 Ru5 2.131(4) . ? N7 N8 1.385(6) . ? N7 Ru4 2.215(4) . ? Ru1 Ru2 2.7643(5) . ? Ru1 Ru3 2.8514(6) . ? Ru2 Ru3 2.8635(6) . ? Ru4 Ru5 2.8585(6) . ? Ru4 Ru6 2.8721(5) . ? Ru5 Ru6 2.7523(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 C1 C2 124.0(5) . . ? N2 C1 H1 118.0 . . ? C2 C1 H1 118.0 . . ? C3 C2 C7 120.5(4) . . ? C3 C2 C1 123.4(5) . . ? C7 C2 C1 116.1(4) . . ? C4 C3 C2 118.7(5) . . ? C4 C3 H3 120.7 . . ? C2 C3 H3 120.7 . . ? C3 C4 C5 121.6(5) . . ? C3 C4 H4 119.2 . . ? C5 C4 H4 119.2 . . ? C6 C5 C4 120.8(5) . . ? C6 C5 H5 119.6 . . ? C4 C5 H5 119.6 . . ? C5 C6 C7 118.8(5) . . ? C5 C6 H6 120.6 . . ? C7 C6 H6 120.6 . . ? C8 C7 C2 117.4(4) . . ? C8 C7 C6 123.0(5) . . ? C2 C7 C6 119.6(5) . . ? N1 C8 C7 123.4(4) . . ? N1 C8 H7 118.3 . . ? C7 C8 H7 118.3 . . ? N4 C9 C10 125.2(5) . . ? N4 C9 H9 117.4 . . ? C10 C9 H9 117.4 . . ? C11 C10 C9 124.3(5) . . ? C11 C10 C15 119.7(5) . . ? C9 C10 C15 116.0(5) . . ? C12 C11 C10 119.9(5) . . ? C12 C11 H11 120.1 . . ? C10 C11 H11 120.1 . . ? C11 C12 C13 120.1(5) . . ? C11 C12 H12 120.0 . . ? C13 C12 H12 120.0 . . ? C14 C13 C12 121.3(5) . . ? C14 C13 H13 119.4 . . ? C12 C13 H13 119.4 . . ? C13 C14 C15 119.9(5) . . ? C13 C14 H14 120.0 . . ? C15 C14 H14 120.0 . . ? C14 C15 C16 125.0(5) . . ? C14 C15 C10 119.2(5) . . ? C16 C15 C10 115.8(5) . . ? N3 C16 C15 125.4(5) . . ? N3 C16 H16 117.3 . . ? C15 C16 H16 117.3 . . ? N6 C17 C18 123.1(5) . . ? N6 C17 H17 118.4 . . ? C18 C17 H17 118.4 . . ? C19 C18 C23 119.9(5) . . ? C19 C18 C17 122.9(5) . . ? C23 C18 C17 117.1(5) . . ? C20 C19 C18 119.3(6) . . ? C20 C19 H19 120.3 . . ? C18 C19 H19 120.3 . . ? C19 C20 C21 120.8(5) . . ? C19 C20 H20 119.6 . . ? C21 C20 H20 119.6 . . ? C22 C21 C20 121.2(6) . . ? C22 C21 H21 119.4 . . ? C20 C21 H21 119.4 . . ? C21 C22 C23 118.2(6) . . ? C21 C22 H22 120.9 . . ? C23 C22 H22 120.9 . . ? C18 C23 C22 120.5(5) . . ? C18 C23 C24 116.8(5) . . ? C22 C23 C24 122.7(5) . . ? N5 C24 C23 122.9(5) . . ? N5 C24 H24 118.5 . . ? C23 C24 H24 118.5 . . ? N8 C25 C26 125.0(5) . . ? N8 C25 H25 117.5 . . ? C26 C25 H25 117.5 . . ? C31 C26 C27 119.4(5) . . ? C31 C26 C25 116.2(5) . . ? C27 C26 C25 124.4(5) . . ? C28 C27 C26 118.9(6) . . ? C28 C27 H27 120.6 . . ? C26 C27 H27 120.6 . . ? C27 C28 C29 121.1(5) . . ? C27 C28 H28 119.4 . . ? C29 C28 H28 119.4 . . ? C30 C29 C28 121.7(6) . . ? C30 C29 H29 119.2 . . ? C28 C29 H29 119.2 . . ? C29 C30 C31 118.6(5) . . ? C29 C30 H30 120.7 . . ? C31 C30 H30 120.7 . . ? C30 C31 C26 120.3(5) . . ? C30 C31 C32 123.3(5) . . ? C26 C31 C32 116.4(5) . . ? N7 C32 C31 123.7(5) . . ? N7 C32 H32 118.2 . . ? C31 C32 H32 118.2 . . ? C34 C33 H33A 109.5 . . ? C34 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C34 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? O99 C34 C33 122.2(6) . . ? O99 C34 C35 121.4(6) . . ? C33 C34 C35 116.4(5) . . ? C34 C35 H35A 109.5 . . ? C34 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C34 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? O101 C101 Ru1 176.2(5) . . ? O102 C102 Ru1 179.5(5) . . ? O103 C103 Ru1 137.7(4) . . ? O103 C103 Ru3 138.6(4) . . ? Ru1 C103 Ru3 83.68(19) . . ? O201 C201 Ru2 175.9(4) . . ? O202 C202 Ru2 177.3(5) . . ? O203 C203 Ru1 140.2(4) . . ? O203 C203 Ru2 138.8(4) . . ? Ru1 C203 Ru2 80.5(2) . . ? O301 C301 Ru3 173.8(5) . . ? O302 C302 Ru3 177.6(5) . . ? O303 C303 Ru3 139.6(4) . . ? O303 C303 Ru2 134.9(4) . . ? Ru3 C303 Ru2 84.79(18) . . ? O401 C401 Ru4 177.7(5) . . ? O402 C402 Ru4 178.5(5) . . ? O403 C403 Ru4 140.7(5) . . ? O403 C403 Ru5 134.4(5) . . ? Ru4 C403 Ru5 84.03(19) . . ? O501 C501 Ru5 177.2(5) . . ? O502 C502 Ru5 177.7(5) . . ? O503 C503 Ru5 141.4(5) . . ? O503 C503 Ru6 137.6(4) . . ? Ru5 C503 Ru6 80.3(2) . . ? O601 C601 Ru6 177.9(5) . . ? O602 C602 Ru6 178.6(5) . . ? O603 C603 Ru6 139.0(4) . . ? O603 C603 Ru4 136.6(4) . . ? Ru6 C603 Ru4 84.2(2) . . ? C8 N1 N2 119.7(4) . . ? C8 N1 Ru1 131.1(3) . . ? N2 N1 Ru1 109.2(3) . . ? C1 N2 N1 119.5(4) . . ? C1 N2 Ru2 131.5(3) . . ? N1 N2 Ru2 108.7(3) . . ? C16 N3 N4 119.1(4) . . ? C16 N3 Ru3 127.8(3) . . ? N4 N3 Ru3 112.9(3) . . ? C9 N4 N3 118.4(4) . . ? C24 N5 N6 120.5(4) . . ? C24 N5 Ru6 130.7(4) . . ? N6 N5 Ru6 108.7(3) . . ? C17 N6 N5 119.6(4) . . ? C17 N6 Ru5 131.5(4) . . ? N5 N6 Ru5 108.8(3) . . ? C32 N7 N8 120.0(4) . . ? C32 N7 Ru4 124.7(4) . . ? N8 N7 Ru4 114.8(3) . . ? C25 N8 N7 118.7(5) . . ? C102 Ru1 C101 90.0(2) . . ? C102 Ru1 C203 90.8(2) . . ? C101 Ru1 C203 106.2(2) . . ? C102 Ru1 N1 173.9(2) . . ? C101 Ru1 N1 93.36(18) . . ? C203 Ru1 N1 83.35(17) . . ? C102 Ru1 C103 88.1(2) . . ? C101 Ru1 C103 95.5(2) . . ? C203 Ru1 C103 158.32(19) . . ? N1 Ru1 C103 96.62(17) . . ? C102 Ru1 Ru2 103.80(15) . . ? C101 Ru1 Ru2 151.71(16) . . ? C203 Ru1 Ru2 50.08(14) . . ? N1 Ru1 Ru2 71.02(10) . . ? C103 Ru1 Ru2 109.32(13) . . ? C102 Ru1 Ru3 94.06(16) . . ? C101 Ru1 Ru3 143.33(17) . . ? C203 Ru1 Ru3 110.20(14) . . ? N1 Ru1 Ru3 86.29(11) . . ? C103 Ru1 Ru3 48.36(13) . . ? Ru2 Ru1 Ru3 61.291(14) . . ? C202 Ru2 C201 88.7(2) . . ? C202 Ru2 N2 172.78(19) . . ? C201 Ru2 N2 93.41(17) . . ? C202 Ru2 C203 88.8(2) . . ? C201 Ru2 C203 108.8(2) . . ? N2 Ru2 C203 84.03(17) . . ? C202 Ru2 C303 86.3(2) . . ? C201 Ru2 C303 96.3(2) . . ? N2 Ru2 C303 100.31(17) . . ? C203 Ru2 C303 154.21(19) . . ? C202 Ru2 Ru1 104.36(16) . . ? C201 Ru2 Ru1 153.17(14) . . ? N2 Ru2 Ru1 71.01(10) . . ? C203 Ru2 Ru1 49.44(15) . . ? C303 Ru2 Ru1 107.64(13) . . ? C202 Ru2 Ru3 97.54(17) . . ? C201 Ru2 Ru3 141.60(15) . . ? N2 Ru2 Ru3 85.10(11) . . ? C203 Ru2 Ru3 109.15(15) . . ? C303 Ru2 Ru3 46.79(13) . . ? Ru1 Ru2 Ru3 60.855(14) . . ? C302 Ru3 C301 87.1(2) . . ? C302 Ru3 C303 90.8(2) . . ? C301 Ru3 C303 105.8(2) . . ? C302 Ru3 C103 94.46(19) . . ? C301 Ru3 C103 100.5(2) . . ? C303 Ru3 C103 153.5(2) . . ? C302 Ru3 N3 174.14(18) . . ? C301 Ru3 N3 88.84(19) . . ? C303 Ru3 N3 86.26(17) . . ? C103 Ru3 N3 90.45(16) . . ? C302 Ru3 Ru1 89.10(16) . . ? C301 Ru3 Ru1 147.77(16) . . ? C303 Ru3 Ru1 106.28(15) . . ? C103 Ru3 Ru1 47.96(15) . . ? N3 Ru3 Ru1 96.57(11) . . ? C302 Ru3 Ru2 90.00(16) . . ? C301 Ru3 Ru2 154.02(16) . . ? C303 Ru3 Ru2 48.42(15) . . ? C103 Ru3 Ru2 105.50(15) . . ? N3 Ru3 Ru2 91.78(11) . . ? Ru1 Ru3 Ru2 57.854(14) . . ? C402 Ru4 C401 88.7(2) . . ? C402 Ru4 C403 91.9(2) . . ? C401 Ru4 C403 105.7(2) . . ? C402 Ru4 C603 93.8(2) . . ? C401 Ru4 C603 101.0(2) . . ? C403 Ru4 C603 152.9(2) . . ? C402 Ru4 N7 173.46(19) . . ? C401 Ru4 N7 85.52(19) . . ? C403 Ru4 N7 86.88(18) . . ? C603 Ru4 N7 90.23(17) . . ? C402 Ru4 Ru5 91.63(17) . . ? C401 Ru4 Ru5 154.94(18) . . ? C403 Ru4 Ru5 49.25(14) . . ? C603 Ru4 Ru5 104.02(15) . . ? N7 Ru4 Ru5 92.39(12) . . ? C402 Ru4 Ru6 87.75(15) . . ? C401 Ru4 Ru6 147.59(18) . . ? C403 Ru4 Ru6 106.62(15) . . ? C603 Ru4 Ru6 47.24(15) . . ? N7 Ru4 Ru6 98.76(10) . . ? Ru5 Ru4 Ru6 57.408(14) . . ? C502 Ru5 C501 92.1(2) . . ? C502 Ru5 C503 88.4(2) . . ? C501 Ru5 C503 106.4(2) . . ? C502 Ru5 N6 172.60(19) . . ? C501 Ru5 N6 92.51(18) . . ? C503 Ru5 N6 84.78(17) . . ? C502 Ru5 C403 84.6(2) . . ? C501 Ru5 C403 96.7(2) . . ? C503 Ru5 C403 156.0(2) . . ? N6 Ru5 C403 100.62(17) . . ? C502 Ru5 Ru6 102.27(17) . . ? C501 Ru5 Ru6 152.10(15) . . ? C503 Ru5 Ru6 51.10(16) . . ? N6 Ru5 Ru6 71.20(11) . . ? C403 Ru5 Ru6 108.22(15) . . ? C502 Ru5 Ru4 96.10(17) . . ? C501 Ru5 Ru4 141.12(16) . . ? C503 Ru5 Ru4 111.73(16) . . ? N6 Ru5 Ru4 83.92(11) . . ? C403 Ru5 Ru4 46.71(15) . . ? Ru6 Ru5 Ru4 61.545(15) . . ? C601 Ru6 C602 89.9(2) . . ? C601 Ru6 C603 94.1(2) . . ? C602 Ru6 C603 100.1(2) . . ? C601 Ru6 N5 173.3(2) . . ? C602 Ru6 N5 93.51(18) . . ? C603 Ru6 N5 91.00(17) . . ? C601 Ru6 C503 89.4(2) . . ? C602 Ru6 C503 102.3(2) . . ? C603 Ru6 C503 157.4(2) . . ? N5 Ru6 C503 84.29(17) . . ? C601 Ru6 Ru5 102.87(16) . . ? C602 Ru6 Ru5 147.09(17) . . ? C603 Ru6 Ru5 108.92(15) . . ? N5 Ru6 Ru5 71.30(11) . . ? C503 Ru6 Ru5 48.63(14) . . ? C601 Ru6 Ru4 96.61(15) . . ? C602 Ru6 Ru4 148.25(17) . . ? C603 Ru6 Ru4 48.56(15) . . ? N5 Ru6 Ru4 83.48(10) . . ? C503 Ru6 Ru4 108.81(14) . . ? Ru5 Ru6 Ru4 61.048(15) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.34 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.019 _refine_diff_density_min -1.417 _refine_diff_density_rms 0.402 # Attachment '- v101f1b.cif' data_v101f1b _database_code_depnum_ccdc_archive 'CCDC 871265' #TrackingRef '- v101f1b.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H8 N2 O20 Ru6' _chemical_formula_sum 'C32 H8 N2 O20 Ru6' _chemical_formula_weight 1346.82 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru 0.0552 3.2960 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting MONOCLINIC _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall ' -P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 7.7728(3) _cell_length_b 33.3854(12) _cell_length_c 17.3761(6) _cell_angle_alpha 90.00 _cell_angle_beta 98.649(4) _cell_angle_gamma 90.00 _cell_volume 4457.8(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4864 _cell_measurement_theta_min 2.8857 _cell_measurement_theta_max 73.7304 _exptl_crystal_description fragment _exptl_crystal_colour orange _exptl_crystal_size_max 0.0438 _exptl_crystal_size_mid 0.0240 _exptl_crystal_size_min 0.0097 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.007 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2552 _exptl_absorpt_coefficient_mu 16.718 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.62536 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'Nova (Cu) X-ray Source' _diffrn_radiation_monochromator mirror _diffrn_measurement_device_type 'Xcalibur, Onyx, Nova' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 33283 _diffrn_reflns_av_R_equivalents 0.1046 _diffrn_reflns_av_sigmaI/netI 0.0914 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -40 _diffrn_reflns_limit_k_max 40 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.89 _diffrn_reflns_theta_max 69.98 _reflns_number_total 8435 _reflns_number_gt 4867 _reflns_threshold_expression >2\s(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'PLATON (Spek, 2008)' _computing_publication_material 'SHELXL-97 (Sheldrick, 2008)' _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^ > 2\s(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^)+(0.1160P)^2^+62.6530P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8435 _refine_ls_number_parameters 543 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1329 _refine_ls_R_factor_gt 0.0839 _refine_ls_wR_factor_ref 0.2627 _refine_ls_wR_factor_gt 0.2404 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.047 _refine_ls_shift/su_max 0.000 _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 C603 C 0.350(3) 0.4262(7) 0.2591(14) 0.067(6) Uani 1 1 d . . . C401 C 0.088(3) 0.3603(6) 0.2873(11) 0.058(5) Uani 1 1 d . . . C403 C -0.125(3) 0.4251(6) 0.3023(11) 0.059(5) Uani 1 1 d . . . C402 C -0.287(3) 0.3534(6) 0.2624(12) 0.064(6) Uani 1 1 d . . . C103 C 0.142(3) 0.0960(6) 0.2898(12) 0.062(5) Uani 1 1 d . . . C601 C 0.071(3) 0.4796(6) 0.2251(13) 0.065(5) Uani 1 1 d . . . C502 C -0.246(3) 0.4817(6) 0.1113(11) 0.061(5) Uani 1 1 d . . . C501 C -0.398(3) 0.4171(6) 0.0210(11) 0.058(5) Uani 1 1 d . . . C503 C -0.064(3) 0.4437(5) 0.0007(11) 0.059(5) Uani 1 1 d . . . C201 C 0.101(3) 0.0408(7) 0.0855(13) 0.069(6) Uani 1 1 d . . . C202 C -0.148(3) 0.0871(6) -0.0118(13) 0.067(6) Uani 1 1 d . . . C301 C -0.333(3) 0.1391(7) 0.1194(15) 0.079(7) Uani 1 1 d . . . C302 C -0.360(3) 0.0949(8) 0.2553(16) 0.082(7) Uani 1 1 d . . . C102 C -0.078(4) 0.1587(6) 0.2860(13) 0.074(6) Uani 1 1 d . . . C101 C 0.278(3) 0.1694(6) 0.2489(12) 0.066(6) Uani 1 1 d . . . C303 C -0.102(3) 0.0424(6) 0.2081(14) 0.072(6) Uani 1 1 d . . . C304 C -0.391(4) 0.0573(8) 0.0997(16) 0.083(7) Uani 1 1 d . . . C602 C 0.272(3) 0.4666(7) 0.1114(13) 0.067(5) Uani 1 1 d . . . C1 C -0.015(3) 0.1581(5) 0.0585(11) 0.058(5) Uani 1 1 d . . . C2 C -0.046(3) 0.1793(6) -0.0143(11) 0.063(5) Uani 1 1 d . . . H2 H -0.0546 0.1651 -0.0606 0.075 Uiso 1 1 calc R . . C3 C -0.063(3) 0.2190(6) -0.0166(11) 0.072(6) Uani 1 1 d . . . H3 H -0.0776 0.2321 -0.0644 0.086 Uiso 1 1 calc R . . C4 C -0.060(3) 0.2421(6) 0.0536(10) 0.060(5) Uani 1 1 d . . . C12 C -0.035(3) 0.2200(5) 0.1247(10) 0.056(5) Uani 1 1 d . . . C11 C -0.023(3) 0.2410(5) 0.1942(10) 0.058(5) Uani 1 1 d . . . H11 H 0.0036 0.2271 0.2408 0.070 Uiso 1 1 calc R . . C10 C -0.050(3) 0.2822(5) 0.1966(10) 0.059(5) Uani 1 1 d . . . H10 H -0.0528 0.2952 0.2437 0.070 Uiso 1 1 calc R . . C9 C -0.074(2) 0.3038(5) 0.1254(10) 0.048(4) Uani 1 1 d . . . C5 C -0.083(2) 0.2847(5) 0.0560(10) 0.049(4) Uani 1 1 d . . . C604 C 0.217(3) 0.3839(7) 0.1283(15) 0.080(7) Uani 1 1 d . . . C203 C 0.213(3) 0.1060(6) 0.0089(13) 0.065(5) Uani 1 1 d . . . C6 C -0.102(4) 0.3074(6) -0.0121(11) 0.081(8) Uani 1 1 d . . . H6 H -0.0967 0.2955 -0.0601 0.097 Uiso 1 1 calc R . . C7 C -0.131(3) 0.3493(6) -0.0061(10) 0.062(5) Uani 1 1 d . . . H7 H -0.1527 0.3648 -0.0510 0.074 Uiso 1 1 calc R . . C8 C -0.128(3) 0.3672(5) 0.0659(10) 0.054(4) Uani 1 1 d . . . N1 N -0.006(2) 0.1785(4) 0.1232(8) 0.054(4) Uani 1 1 d . . . N2 N -0.103(2) 0.3445(4) 0.1306(8) 0.051(4) Uani 1 1 d . . . O603 O 0.461(2) 0.4248(5) 0.3092(10) 0.087(5) Uani 1 1 d . . . O401 O 0.199(3) 0.3447(5) 0.3277(11) 0.101(6) Uani 1 1 d . . . O403 O -0.145(2) 0.4485(5) 0.3471(9) 0.084(5) Uani 1 1 d . . . O402 O -0.389(3) 0.3344(6) 0.2849(13) 0.107(6) Uani 1 1 d . . . O103 O 0.195(2) 0.0735(5) 0.3348(10) 0.092(5) Uani 1 1 d . . . O601 O 0.032(3) 0.5079(5) 0.2531(10) 0.091(5) Uani 1 1 d . . . O502 O -0.286(2) 0.5131(4) 0.1278(10) 0.080(4) Uani 1 1 d . . . O501 O -0.526(2) 0.4127(6) -0.0196(11) 0.097(5) Uani 1 1 d . . . O503 O 0.002(2) 0.4543(5) -0.0488(8) 0.079(4) Uani 1 1 d . . . O201 O 0.139(3) 0.0080(5) 0.0883(12) 0.102(6) Uani 1 1 d . . . O202 O -0.263(2) 0.0808(5) -0.0607(9) 0.086(5) Uani 1 1 d . . . O301 O -0.395(2) 0.1667(5) 0.0934(12) 0.101(6) Uani 1 1 d . . . O302 O -0.432(3) 0.0960(6) 0.3062(13) 0.121(8) Uani 1 1 d . . . O102 O -0.151(3) 0.1700(6) 0.3318(11) 0.109(7) Uani 1 1 d . . . O101 O 0.397(3) 0.1861(6) 0.2731(12) 0.112(7) Uani 1 1 d . . . O303 O -0.038(3) 0.0141(5) 0.2324(11) 0.096(5) Uani 1 1 d . . . O602 O 0.334(2) 0.4873(5) 0.0721(10) 0.084(5) Uani 1 1 d . . . O304 O -0.484(3) 0.0365(6) 0.0640(12) 0.119(8) Uani 1 1 d . . . O604 O 0.279(2) 0.3563(5) 0.1012(11) 0.099(6) Uani 1 1 d . . . O203 O 0.314(3) 0.1140(6) -0.0303(10) 0.103(6) Uani 1 1 d . . . Ru1 Ru 0.0698(2) 0.13778(4) 0.21831(8) 0.0525(4) Uani 1 1 d . . . Ru5 Ru -0.17897(19) 0.42735(4) 0.08402(8) 0.0491(4) Uani 1 1 d . . . Ru4 Ru -0.1067(2) 0.38380(4) 0.22764(8) 0.0492(4) Uani 1 1 d . . . Ru2 Ru 0.0363(2) 0.09704(4) 0.07004(8) 0.0536(4) Uani 1 1 d . . . Ru3 Ru -0.2273(2) 0.08978(4) 0.16720(10) 0.0608(4) Uani 1 1 d . . . Ru6 Ru 0.15827(19) 0.43235(4) 0.17706(9) 0.0532(4) Uani 1 1 d . . . H100 H 0.2001 0.1098 0.1552 0.11(8) Uiso 1 1 d . . . H200 H -0.2855 0.4113 0.1673 0.10(8) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C603 0.041(11) 0.066(13) 0.093(16) -0.013(12) 0.008(11) 0.010(10) C401 0.069(13) 0.045(10) 0.057(11) -0.006(9) 0.005(10) 0.011(10) C403 0.070(13) 0.045(10) 0.057(11) 0.001(9) -0.004(9) -0.010(9) C402 0.087(16) 0.042(10) 0.071(13) 0.006(9) 0.042(12) 0.000(10) C103 0.059(12) 0.053(11) 0.065(12) 0.002(10) -0.016(10) -0.001(9) C601 0.062(13) 0.055(12) 0.077(14) -0.004(11) 0.004(11) -0.003(10) C502 0.059(12) 0.065(13) 0.056(11) 0.017(10) 0.000(9) 0.007(10) C501 0.073(14) 0.048(10) 0.048(10) -0.011(8) -0.005(10) 0.006(10) C503 0.075(14) 0.043(10) 0.050(10) 0.002(8) -0.020(10) -0.016(9) C201 0.060(13) 0.063(14) 0.086(15) 0.008(11) 0.015(11) 0.006(11) C202 0.090(16) 0.040(10) 0.074(14) -0.016(10) 0.019(12) -0.006(10) C301 0.089(18) 0.066(14) 0.091(16) 0.008(13) 0.041(14) -0.022(14) C302 0.082(17) 0.073(16) 0.094(18) 0.013(14) 0.018(14) 0.008(13) C102 0.11(2) 0.047(11) 0.064(13) 0.001(10) 0.021(13) 0.000(12) C101 0.080(15) 0.047(11) 0.065(12) -0.010(9) -0.007(11) -0.001(11) C303 0.091(17) 0.048(11) 0.088(15) 0.005(11) 0.050(13) 0.008(12) C304 0.082(17) 0.077(16) 0.096(18) 0.005(14) 0.033(15) -0.001(14) C602 0.056(13) 0.063(13) 0.083(15) -0.002(11) 0.020(11) 0.012(10) C1 0.070(13) 0.037(9) 0.058(11) 0.003(8) -0.016(9) 0.020(9) C2 0.086(15) 0.048(11) 0.053(10) -0.001(9) 0.007(10) 0.002(10) C3 0.118(19) 0.040(10) 0.051(11) -0.009(8) -0.011(11) 0.015(11) C4 0.086(15) 0.050(11) 0.039(9) 0.005(8) 0.000(9) -0.015(10) C12 0.092(15) 0.035(9) 0.045(9) 0.011(7) 0.016(9) 0.008(9) C11 0.089(15) 0.036(9) 0.045(9) 0.014(8) -0.006(9) 0.009(9) C10 0.093(15) 0.037(9) 0.045(9) -0.002(8) 0.010(10) -0.008(10) C9 0.055(11) 0.029(8) 0.055(10) -0.001(7) -0.002(8) -0.010(7) C5 0.065(12) 0.028(8) 0.056(10) 0.004(7) 0.012(9) 0.001(8) C604 0.077(16) 0.064(14) 0.092(16) -0.005(13) -0.010(13) -0.016(12) C203 0.061(13) 0.057(12) 0.083(14) -0.004(10) 0.030(11) -0.009(10) C6 0.15(2) 0.046(11) 0.044(10) -0.009(9) -0.009(12) 0.012(13) C7 0.092(16) 0.049(10) 0.044(9) -0.002(8) 0.009(10) 0.014(10) C8 0.070(13) 0.038(9) 0.054(10) 0.007(8) 0.014(9) 0.004(9) N1 0.073(11) 0.036(7) 0.049(8) 0.007(6) -0.008(7) 0.008(7) N2 0.077(11) 0.028(7) 0.046(8) -0.005(6) -0.001(7) 0.013(7) O603 0.081(12) 0.083(12) 0.089(11) 0.006(9) -0.008(9) 0.003(9) O401 0.118(15) 0.076(11) 0.099(13) 0.008(10) -0.019(11) -0.003(11) O403 0.118(14) 0.055(9) 0.083(10) -0.021(8) 0.028(10) -0.001(9) O402 0.094(14) 0.083(13) 0.150(18) 0.007(12) 0.039(13) -0.009(11) O103 0.120(15) 0.068(10) 0.087(11) 0.030(9) 0.009(10) 0.003(10) O601 0.126(15) 0.059(10) 0.090(11) -0.022(9) 0.018(10) 0.000(10) O502 0.083(11) 0.046(8) 0.114(12) -0.009(8) 0.030(9) 0.019(8) O501 0.075(11) 0.108(14) 0.099(12) 0.011(11) -0.011(10) -0.019(10) O503 0.096(12) 0.085(11) 0.057(8) 0.007(8) 0.014(8) -0.015(9) O201 0.129(16) 0.045(9) 0.130(15) 0.004(9) 0.021(12) 0.019(10) O202 0.092(12) 0.077(11) 0.081(10) -0.019(9) -0.015(9) -0.015(9) O301 0.091(13) 0.075(11) 0.135(16) 0.047(11) 0.014(11) 0.027(10) O302 0.15(2) 0.091(14) 0.143(18) 0.012(13) 0.095(17) 0.019(13) O102 0.144(19) 0.102(15) 0.093(13) -0.011(11) 0.050(13) 0.018(13) O101 0.103(15) 0.081(12) 0.140(17) -0.009(12) -0.024(13) -0.024(11) O303 0.119(15) 0.057(10) 0.110(13) 0.010(9) 0.011(11) 0.014(10) O602 0.075(11) 0.079(11) 0.097(12) 0.022(9) 0.011(9) -0.008(9) O304 0.108(15) 0.094(14) 0.138(17) -0.019(12) -0.034(13) -0.039(12) O604 0.107(14) 0.070(11) 0.126(15) -0.032(10) 0.032(11) 0.021(10) O203 0.132(16) 0.102(14) 0.092(12) -0.007(10) 0.073(12) 0.009(12) Ru1 0.0677(10) 0.0401(7) 0.0484(7) 0.0032(6) 0.0043(6) 0.0038(7) Ru5 0.0576(9) 0.0367(7) 0.0519(7) 0.0045(6) 0.0049(6) 0.0018(6) Ru4 0.0628(9) 0.0370(7) 0.0477(7) 0.0007(6) 0.0078(6) 0.0008(6) Ru2 0.0682(10) 0.0378(7) 0.0542(8) -0.0023(6) 0.0072(7) 0.0015(6) Ru3 0.0635(10) 0.0448(8) 0.0736(10) 0.0055(7) 0.0093(8) 0.0005(7) Ru6 0.0537(9) 0.0425(7) 0.0626(8) -0.0022(6) 0.0058(7) 0.0012(6) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 C603 O603 1.13(2) . ? C603 Ru6 1.91(2) . ? C401 O401 1.15(2) . ? C401 Ru4 1.87(2) . ? C403 O403 1.13(2) . ? C403 Ru4 1.91(2) . ? C402 O402 1.13(2) . ? C402 Ru4 1.90(2) . ? C103 O103 1.12(2) . ? C103 Ru1 1.90(2) . ? C601 O601 1.13(2) . ? C601 Ru6 1.95(2) . ? C502 O502 1.14(2) . ? C502 Ru5 1.96(2) . ? C501 O501 1.14(2) . ? C501 Ru5 1.91(2) . ? C503 O503 1.12(2) . ? C503 Ru5 1.89(2) . ? C201 O201 1.13(3) . ? C201 Ru2 1.95(2) . ? C202 O202 1.16(3) . ? C202 Ru2 1.89(2) . ? C301 O301 1.11(3) . ? C301 Ru3 1.97(3) . ? C302 O302 1.12(3) . ? C302 Ru3 1.98(3) . ? C102 O102 1.11(3) . ? C102 Ru1 1.90(2) . ? C101 O101 1.11(3) . ? C101 Ru1 1.94(2) . ? C303 O303 1.12(3) . ? C303 Ru3 1.94(2) . ? C304 O304 1.12(3) . ? C304 Ru3 1.93(3) . ? C602 O602 1.13(2) . ? C602 Ru6 1.92(2) . ? C1 N1 1.31(2) . ? C1 C2 1.44(3) . ? C1 Ru2 2.081(17) . ? C2 C3 1.33(3) . ? C3 C4 1.44(3) . ? C4 C12 1.43(2) . ? C4 C5 1.44(2) . ? C12 C11 1.39(2) . ? C12 N1 1.41(2) . ? C11 C10 1.39(2) . ? C10 C9 1.42(2) . ? C9 C5 1.36(2) . ? C9 N2 1.38(2) . ? C5 C6 1.39(3) . ? C604 O604 1.17(3) . ? C604 Ru6 1.91(3) . ? C203 O203 1.14(2) . ? C203 Ru2 1.88(2) . ? C6 C7 1.42(3) . ? C7 C8 1.38(2) . ? C8 N2 1.35(2) . ? C8 Ru5 2.080(18) . ? N1 Ru1 2.152(13) . ? N2 Ru4 2.140(13) . ? Ru1 Ru3 2.842(2) . ? Ru1 Ru2 2.890(2) . ? Ru5 Ru4 2.8699(19) . ? Ru5 Ru6 2.870(2) . ? Ru4 Ru6 2.861(2) . ? Ru2 Ru3 2.855(2) . ? 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 O603 C603 Ru6 176(2) . . ? O401 C401 Ru4 175(2) . . ? O403 C403 Ru4 175.6(19) . . ? O402 C402 Ru4 177(2) . . ? O103 C103 Ru1 174.2(19) . . ? O601 C601 Ru6 175(2) . . ? O502 C502 Ru5 179(2) . . ? O501 C501 Ru5 176(2) . . ? O503 C503 Ru5 178(2) . . ? O201 C201 Ru2 175(2) . . ? O202 C202 Ru2 179(2) . . ? O301 C301 Ru3 178(2) . . ? O302 C302 Ru3 177(2) . . ? O102 C102 Ru1 173(2) . . ? O101 C101 Ru1 173(2) . . ? O303 C303 Ru3 176(2) . . ? O304 C304 Ru3 175(3) . . ? O602 C602 Ru6 178(2) . . ? N1 C1 C2 118.6(16) . . ? N1 C1 Ru2 116.3(12) . . ? C2 C1 Ru2 124.9(14) . . ? C3 C2 C1 121.4(18) . . ? C2 C3 C4 121.2(19) . . ? C12 C4 C5 119.1(16) . . ? C12 C4 C3 116.2(17) . . ? C5 C4 C3 124.7(16) . . ? C11 C12 N1 121.6(15) . . ? C11 C12 C4 118.5(16) . . ? N1 C12 C4 119.6(16) . . ? C12 C11 C10 122.2(16) . . ? C11 C10 C9 118.5(16) . . ? C5 C9 N2 122.2(15) . . ? C5 C9 C10 121.1(15) . . ? N2 C9 C10 116.4(15) . . ? C9 C5 C6 118.9(16) . . ? C9 C5 C4 120.2(15) . . ? C6 C5 C4 120.8(16) . . ? O604 C604 Ru6 169(2) . . ? O203 C203 Ru2 175(2) . . ? C5 C6 C7 118.1(17) . . ? C8 C7 C6 120.6(17) . . ? N2 C8 C7 119.6(16) . . ? N2 C8 Ru5 115.1(12) . . ? C7 C8 Ru5 125.2(13) . . ? C1 N1 C12 122.8(14) . . ? C1 N1 Ru1 107.8(11) . . ? C12 N1 Ru1 129.4(11) . . ? C8 N2 C9 120.3(14) . . ? C8 N2 Ru4 107.3(11) . . ? C9 N2 Ru4 132.4(11) . . ? C103 Ru1 C102 90.7(9) . . ? C103 Ru1 C101 93.9(9) . . ? C102 Ru1 C101 100.8(10) . . ? C103 Ru1 N1 171.0(8) . . ? C102 Ru1 N1 97.1(8) . . ? C101 Ru1 N1 89.2(8) . . ? C103 Ru1 Ru3 86.4(6) . . ? C102 Ru1 Ru3 82.1(7) . . ? C101 Ru1 Ru3 177.1(7) . . ? N1 Ru1 Ru3 90.1(4) . . ? C103 Ru1 Ru2 102.5(6) . . ? C102 Ru1 Ru2 138.1(8) . . ? C101 Ru1 Ru2 117.4(6) . . ? N1 Ru1 Ru2 68.6(4) . . ? Ru3 Ru1 Ru2 59.73(5) . . ? C503 Ru5 C501 95.6(8) . . ? C503 Ru5 C502 95.2(8) . . ? C501 Ru5 C502 93.4(8) . . ? C503 Ru5 C8 92.3(8) . . ? C501 Ru5 C8 85.0(8) . . ? C502 Ru5 C8 172.5(8) . . ? C503 Ru5 Ru4 139.2(6) . . ? C501 Ru5 Ru4 116.7(6) . . ? C502 Ru5 Ru4 106.4(5) . . ? C8 Ru5 Ru4 68.0(5) . . ? C503 Ru5 Ru6 85.2(5) . . ? C501 Ru5 Ru6 172.9(6) . . ? C502 Ru5 Ru6 93.6(6) . . ? C8 Ru5 Ru6 87.9(6) . . ? Ru4 Ru5 Ru6 59.79(5) . . ? C401 Ru4 C402 99.9(9) . . ? C401 Ru4 C403 93.5(8) . . ? C402 Ru4 C403 92.2(9) . . ? C401 Ru4 N2 94.3(7) . . ? C402 Ru4 N2 91.2(8) . . ? C403 Ru4 N2 170.8(7) . . ? C401 Ru4 Ru6 81.3(7) . . ? C402 Ru4 Ru6 177.8(6) . . ? C403 Ru4 Ru6 85.9(6) . . ? N2 Ru4 Ru6 90.6(4) . . ? C401 Ru4 Ru5 136.9(6) . . ? C402 Ru4 Ru5 119.3(7) . . ? C403 Ru4 Ru5 101.5(6) . . ? N2 Ru4 Ru5 69.4(4) . . ? Ru6 Ru4 Ru5 60.11(5) . . ? C203 Ru2 C202 97.9(10) . . ? C203 Ru2 C201 92.0(9) . . ? C202 Ru2 C201 94.9(9) . . ? C203 Ru2 C1 86.4(9) . . ? C202 Ru2 C1 89.2(8) . . ? C201 Ru2 C1 175.7(9) . . ? C203 Ru2 Ru3 175.5(6) . . ? C202 Ru2 Ru3 84.3(7) . . ? C201 Ru2 Ru3 91.8(7) . . ? C1 Ru2 Ru3 89.7(6) . . ? C203 Ru2 Ru1 116.9(7) . . ? C202 Ru2 Ru1 135.3(6) . . ? C201 Ru2 Ru1 110.1(7) . . ? C1 Ru2 Ru1 67.4(5) . . ? Ru3 Ru2 Ru1 59.29(6) . . ? C304 Ru3 C303 90.7(11) . . ? C304 Ru3 C301 91.1(11) . . ? C303 Ru3 C301 173.7(9) . . ? C304 Ru3 C302 98.5(11) . . ? C303 Ru3 C302 94.5(9) . . ? C301 Ru3 C302 91.2(10) . . ? C304 Ru3 Ru1 159.6(7) . . ? C303 Ru3 Ru1 90.3(7) . . ? C301 Ru3 Ru1 85.9(7) . . ? C302 Ru3 Ru1 101.7(8) . . ? C304 Ru3 Ru2 98.8(7) . . ? C303 Ru3 Ru2 85.4(6) . . ? C301 Ru3 Ru2 88.3(6) . . ? C302 Ru3 Ru2 162.6(8) . . ? Ru1 Ru3 Ru2 60.98(5) . . ? C603 Ru6 C604 91.6(9) . . ? C603 Ru6 C602 97.5(10) . . ? C604 Ru6 C602 94.5(10) . . ? C603 Ru6 C601 92.8(9) . . ? C604 Ru6 C601 173.4(10) . . ? C602 Ru6 C601 89.7(9) . . ? C603 Ru6 Ru4 103.1(7) . . ? C604 Ru6 Ru4 83.6(8) . . ? C602 Ru6 Ru4 159.4(7) . . ? C601 Ru6 Ru4 90.7(6) . . ? C603 Ru6 Ru5 163.1(7) . . ? C604 Ru6 Ru5 87.7(7) . . ? C602 Ru6 Ru5 99.3(7) . . ? C601 Ru6 Ru5 86.6(6) . . ? Ru4 Ru6 Ru5 60.10(5) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 69.98 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 3.204 _refine_diff_density_min -0.933 _refine_diff_density_rms 0.226 # Attachment '- v102f1.cif' data_v102f1 _database_code_depnum_ccdc_archive 'CCDC 871266' #TrackingRef '- v102f1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C19 H8 N2 O9 Ru3' _chemical_formula_sum 'C19 H8 N2 O9 Ru3' _chemical_formula_weight 711.48 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru 0.0552 3.2960 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' 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 9.158 _cell_length_b 13.12980(10) _cell_length_c 18.18930(10) _cell_angle_alpha 90.00 _cell_angle_beta 91.7510(10) _cell_angle_gamma 90.00 _cell_volume 2186.11(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 20549 _cell_measurement_theta_min 3.3645 _cell_measurement_theta_max 73.8779 _exptl_crystal_description fragment _exptl_crystal_colour orange _exptl_crystal_size_max 0.1550 _exptl_crystal_size_mid 0.0877 _exptl_crystal_size_min 0.0326 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.162 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1360 _exptl_absorpt_coefficient_mu 17.071 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.30491 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.32 (release 27-01-2009 CrysAlis171 .NET) (compiled Jan 27 2009,14:17:37) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.54180 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'Nova (Cu) X-ray Source' _diffrn_radiation_monochromator mirror _diffrn_measurement_device_type 'Goniometer Xcalibur, detector: Onyx (Nova)' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25507 _diffrn_reflns_av_R_equivalents 0.0453 _diffrn_reflns_av_sigmaI/netI 0.0223 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 4.15 _diffrn_reflns_theta_max 74.03 _reflns_number_total 4435 _reflns_number_gt 4245 _reflns_threshold_expression >2\s(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'PLATON (Spek, 2008)' _computing_publication_material 'SHELXL-97 (Sheldrick, 2008)' _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^ > 2\s(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^)+(0.0460P)^2^+0.6960P] 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 4435 _refine_ls_number_parameters 301 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0268 _refine_ls_R_factor_gt 0.0257 _refine_ls_wR_factor_ref 0.0669 _refine_ls_wR_factor_gt 0.0659 _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_restrained_S_all 1.063 _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 C1 C 0.2257(3) 0.33024(19) 0.07914(14) 0.0367(5) Uani 1 1 d . . . C2 C 0.1202(3) 0.4910(2) 0.07596(16) 0.0447(6) Uani 1 1 d . . . H2 H 0.0541 0.5371 0.0951 0.054 Uiso 1 1 calc R . . C3 C 0.2052(3) 0.5201(2) 0.01784(17) 0.0498(6) Uani 1 1 d . . . H3 H 0.1925 0.5839 -0.0038 0.060 Uiso 1 1 calc R . . C4 C 0.3091(3) 0.4535(2) -0.00775(15) 0.0467(6) Uani 1 1 d . . . H4 H 0.3694 0.4729 -0.0455 0.056 Uiso 1 1 calc R . . C5 C 0.3223(3) 0.3576(2) 0.02348(14) 0.0397(5) Uani 1 1 d . . . C6 C 0.4342(3) 0.2806(2) 0.01161(14) 0.0410(6) Uani 1 1 d . . . C7 C 0.5469(4) 0.2898(3) -0.03809(18) 0.0531(7) Uani 1 1 d . . . H7 H 0.5508 0.3461 -0.0690 0.064 Uiso 1 1 calc R . . C8 C 0.6524(4) 0.2148(3) -0.0410(2) 0.0653(10) Uani 1 1 d . . . H8 H 0.7278 0.2201 -0.0739 0.078 Uiso 1 1 calc R . . C9 C 0.6446(4) 0.1327(3) 0.0051(2) 0.0650(9) Uani 1 1 d . . . H9 H 0.7156 0.0820 0.0045 0.078 Uiso 1 1 calc R . . C10 C 0.5302(3) 0.1259(3) 0.05249(19) 0.0529(7) Uani 1 1 d . . . H10 H 0.5254 0.0696 0.0833 0.063 Uiso 1 1 calc R . . C101 C 0.1140(3) 0.1436(3) 0.04073(18) 0.0512(7) Uani 1 1 d . . . C102 C 0.2605(3) 0.0495(2) 0.15869(17) 0.0503(7) Uani 1 1 d . . . C201 C -0.1488(3) 0.3379(2) 0.15958(17) 0.0472(6) Uani 1 1 d . . . C202 C 0.0673(3) 0.4509(2) 0.25366(17) 0.0482(6) Uani 1 1 d . . . C203 C -0.0139(3) 0.2599(2) 0.28619(17) 0.0483(6) Uani 1 1 d . . . C301 C 0.3995(3) 0.4004(2) 0.19737(15) 0.0434(6) Uani 1 1 d . . . C302 C 0.5261(4) 0.2208(3) 0.2516(2) 0.0634(9) Uani 1 1 d . . . C303 C 0.3366(3) 0.3592(2) 0.34463(17) 0.0493(6) Uani 1 1 d . . . C304 C 0.2581(3) 0.1603(3) 0.29399(16) 0.0481(6) Uani 1 1 d . . . N1 N 0.4257(3) 0.19710(18) 0.05593(13) 0.0418(5) Uani 1 1 d . . . N2 N 0.1317(2) 0.39795(17) 0.10495(12) 0.0383(4) Uani 1 1 d . . . O101 O 0.0336(4) 0.1219(3) -0.00514(18) 0.0883(9) Uani 1 1 d . . . O102 O 0.2770(4) -0.0327(2) 0.17693(18) 0.0823(9) Uani 1 1 d . . . O201 O -0.2657(3) 0.3449(2) 0.13921(17) 0.0719(7) Uani 1 1 d . . . O202 O 0.0803(3) 0.5255(2) 0.28553(18) 0.0752(7) Uani 1 1 d . . . O203 O -0.0579(3) 0.2242(2) 0.33772(15) 0.0709(7) Uani 1 1 d . . . O301 O 0.4406(3) 0.47108(19) 0.16804(14) 0.0608(6) Uani 1 1 d . . . O302 O 0.6357(3) 0.1819(3) 0.2508(3) 0.1108(16) Uani 1 1 d . . . O303 O 0.3334(4) 0.4042(2) 0.39726(14) 0.0739(7) Uani 1 1 d . . . O304 O 0.2170(3) 0.08836(19) 0.32227(14) 0.0636(6) Uani 1 1 d . . . Ru1 Ru 0.23460(2) 0.187264(14) 0.119941(10) 0.03468(7) Uani 1 1 d . . . Ru2 Ru 0.049103(19) 0.326691(14) 0.200937(10) 0.03551(7) Uani 1 1 d . . . Ru3 Ru 0.337980(19) 0.283071(15) 0.253637(10) 0.03675(7) Uani 1 1 d . . . H100 H 0.069(4) 0.205(3) 0.163(2) 0.050 Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0379(12) 0.0382(12) 0.0344(11) 0.0002(9) 0.0036(9) -0.0051(9) C2 0.0428(13) 0.0388(13) 0.0524(15) 0.0053(11) -0.0028(11) 0.0007(10) C3 0.0539(16) 0.0438(15) 0.0513(15) 0.0139(12) -0.0062(12) -0.0061(12) C4 0.0494(14) 0.0529(16) 0.0379(12) 0.0086(11) 0.0005(10) -0.0169(12) C5 0.0409(12) 0.0437(14) 0.0346(11) -0.0006(10) 0.0034(9) -0.0099(10) C6 0.0415(13) 0.0484(15) 0.0335(12) -0.0068(10) 0.0083(10) -0.0109(11) C7 0.0565(17) 0.0569(18) 0.0472(16) -0.0089(13) 0.0210(13) -0.0169(14) C8 0.0549(18) 0.077(2) 0.066(2) -0.0172(18) 0.0337(16) -0.0131(16) C9 0.0494(17) 0.068(2) 0.079(2) -0.0172(18) 0.0219(16) 0.0051(15) C10 0.0491(15) 0.0508(16) 0.0596(17) -0.0064(14) 0.0170(13) 0.0048(13) C101 0.0499(15) 0.0495(16) 0.0546(16) -0.0057(13) 0.0070(13) -0.0087(13) C102 0.0566(16) 0.0442(16) 0.0512(15) 0.0000(12) 0.0193(13) 0.0016(12) C201 0.0402(15) 0.0522(16) 0.0495(15) 0.0069(12) 0.0085(11) -0.0020(12) C202 0.0441(14) 0.0449(15) 0.0561(16) -0.0029(13) 0.0106(12) 0.0063(11) C203 0.0455(14) 0.0498(16) 0.0503(15) -0.0018(13) 0.0138(12) 0.0049(12) C301 0.0398(12) 0.0469(15) 0.0435(13) -0.0008(12) 0.0008(10) -0.0031(11) C302 0.0480(17) 0.058(2) 0.084(2) 0.0187(17) 0.0132(16) 0.0011(14) C303 0.0542(16) 0.0498(16) 0.0440(14) 0.0013(13) 0.0019(12) -0.0018(12) C304 0.0446(14) 0.0548(17) 0.0447(14) 0.0066(13) 0.0003(11) 0.0018(12) N1 0.0404(11) 0.0444(12) 0.0412(11) -0.0070(9) 0.0115(9) -0.0029(9) N2 0.0357(10) 0.0382(11) 0.0409(10) 0.0032(9) 0.0020(8) -0.0011(8) O101 0.0803(19) 0.105(2) 0.0781(18) -0.0223(17) -0.0185(15) -0.0218(18) O102 0.120(2) 0.0414(13) 0.0872(19) 0.0153(13) 0.0281(17) 0.0152(14) O201 0.0390(12) 0.097(2) 0.0794(17) 0.0203(16) -0.0024(11) -0.0025(12) O202 0.0776(17) 0.0557(15) 0.0927(19) -0.0261(14) 0.0049(14) 0.0084(12) O203 0.0758(16) 0.0790(18) 0.0598(14) 0.0184(13) 0.0309(13) 0.0042(13) O301 0.0656(14) 0.0544(13) 0.0622(13) 0.0130(11) -0.0029(10) -0.0178(11) O302 0.0503(16) 0.102(3) 0.182(4) 0.058(3) 0.033(2) 0.0294(16) O303 0.101(2) 0.0700(16) 0.0503(13) -0.0136(12) -0.0011(12) 0.0000(15) O304 0.0732(15) 0.0552(14) 0.0627(14) 0.0178(11) 0.0069(11) -0.0092(11) Ru1 0.03631(11) 0.03131(11) 0.03699(11) -0.00067(6) 0.01050(8) -0.00274(6) Ru2 0.03172(11) 0.03560(11) 0.03967(12) 0.00086(7) 0.00881(8) 0.00160(6) Ru3 0.03462(11) 0.03909(12) 0.03666(11) 0.00222(7) 0.00325(7) -0.00094(7) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 C1 N2 1.333(3) . ? C1 C5 1.411(4) . ? C1 Ru1 2.019(3) . ? C2 N2 1.334(4) . ? C2 C3 1.385(4) . ? C3 C4 1.384(5) . ? C4 C5 1.385(4) . ? C5 C6 1.460(4) . ? C6 N1 1.364(4) . ? C6 C7 1.398(4) . ? C7 C8 1.382(5) . ? C8 C9 1.370(6) . ? C9 C10 1.380(4) . ? C10 N1 1.341(4) . ? C101 O101 1.132(5) . ? C101 Ru1 1.878(3) . ? C102 O102 1.138(4) . ? C102 Ru1 1.953(3) . ? C201 O201 1.126(4) . ? C201 Ru2 1.947(3) . ? C202 O202 1.143(4) . ? C202 Ru2 1.896(3) . ? C203 O203 1.133(4) . ? C203 Ru2 1.887(3) . ? C301 O301 1.140(4) . ? C301 Ru3 1.943(3) . ? C302 O302 1.126(5) . ? C302 Ru3 1.909(3) . ? C303 O303 1.126(4) . ? C303 Ru3 1.934(3) . ? C304 O304 1.145(4) . ? C304 Ru3 1.925(3) . ? N1 Ru1 2.135(2) . ? N2 Ru2 2.139(2) . ? Ru1 Ru3 2.8726(3) . ? Ru1 Ru2 2.9258(3) . ? Ru2 Ru3 2.8444(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 C1 C5 120.6(2) . . ? N2 C1 Ru1 120.64(18) . . ? C5 C1 Ru1 118.8(2) . . ? N2 C2 C3 121.0(3) . . ? C4 C3 C2 119.4(3) . . ? C3 C4 C5 119.3(2) . . ? C4 C5 C1 118.5(3) . . ? C4 C5 C6 128.4(2) . . ? C1 C5 C6 112.8(2) . . ? N1 C6 C7 120.6(3) . . ? N1 C6 C5 114.6(2) . . ? C7 C6 C5 124.8(3) . . ? C8 C7 C6 119.6(3) . . ? C9 C8 C7 119.2(3) . . ? C8 C9 C10 119.2(3) . . ? N1 C10 C9 122.7(3) . . ? O101 C101 Ru1 175.0(3) . . ? O102 C102 Ru1 175.8(3) . . ? O201 C201 Ru2 176.5(3) . . ? O202 C202 Ru2 179.0(3) . . ? O203 C203 Ru2 175.9(3) . . ? O301 C301 Ru3 175.8(3) . . ? O302 C302 Ru3 178.4(3) . . ? O303 C303 Ru3 178.8(3) . . ? O304 C304 Ru3 175.1(3) . . ? C10 N1 C6 118.6(2) . . ? C10 N1 Ru1 125.5(2) . . ? C6 N1 Ru1 115.69(18) . . ? C1 N2 C2 121.0(2) . . ? C1 N2 Ru2 104.13(17) . . ? C2 N2 Ru2 134.24(19) . . ? C101 Ru1 C102 93.25(15) . . ? C101 Ru1 C1 89.16(13) . . ? C102 Ru1 C1 175.31(12) . . ? C101 Ru1 N1 94.16(11) . . ? C102 Ru1 N1 99.22(11) . . ? C1 Ru1 N1 76.57(10) . . ? C101 Ru1 Ru3 162.55(10) . . ? C102 Ru1 Ru3 93.83(10) . . ? C1 Ru1 Ru3 84.99(7) . . ? N1 Ru1 Ru3 100.41(7) . . ? C101 Ru1 Ru2 103.90(10) . . ? C102 Ru1 Ru2 117.63(8) . . ? C1 Ru1 Ru2 65.54(7) . . ? N1 Ru1 Ru2 137.29(6) . . ? Ru3 Ru1 Ru2 58.745(6) . . ? C203 Ru2 C202 90.46(14) . . ? C203 Ru2 C201 92.76(13) . . ? C202 Ru2 C201 101.35(13) . . ? C203 Ru2 N2 176.84(11) . . ? C202 Ru2 N2 90.52(11) . . ? C201 Ru2 N2 89.99(10) . . ? C203 Ru2 Ru3 86.22(9) . . ? C202 Ru2 Ru3 86.36(9) . . ? C201 Ru2 Ru3 172.24(10) . . ? N2 Ru2 Ru3 90.85(6) . . ? C203 Ru2 Ru1 108.66(9) . . ? C202 Ru2 Ru1 138.53(9) . . ? C201 Ru2 Ru1 113.62(9) . . ? N2 Ru2 Ru1 68.75(6) . . ? Ru3 Ru2 Ru1 59.693(6) . . ? C302 Ru3 C304 90.12(14) . . ? C302 Ru3 C303 105.50(17) . . ? C304 Ru3 C303 95.40(13) . . ? C302 Ru3 C301 93.05(13) . . ? C304 Ru3 C301 170.00(12) . . ? C303 Ru3 C301 92.89(13) . . ? C302 Ru3 Ru2 155.61(14) . . ? C304 Ru3 Ru2 86.38(9) . . ? C303 Ru3 Ru2 98.86(9) . . ? C301 Ru3 Ru2 86.82(8) . . ? C302 Ru3 Ru1 94.05(14) . . ? C304 Ru3 Ru1 80.61(9) . . ? C303 Ru3 Ru1 160.10(9) . . ? C301 Ru3 Ru1 89.70(8) . . ? Ru2 Ru3 Ru1 61.562(7) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 74.03 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.364 _refine_diff_density_min -0.734 _refine_diff_density_rms 0.116