Electronic Supplementary Material for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'del Rio,Ignacio' 'Javier Cabeza' 'da Silva,Ivan' 'Rob Gossage' 'D. Miguel' 'Marta Suarez' _publ_contact_author_name 'Ignacio del Rio' _publ_contact_author_address ; Quimica Organica e Inorganica Universidad de Oviedo C./ Julian Claveria, 6 Oviedo 33071 SPAIN ; _publ_contact_author_email IRC@FQ.UNIOVI.ES _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Triruthenium carbonyl clusters derived from chiral aminooxazolines: Synthesis and catalytic activity ; data_1_(ids221am) _database_code_depnum_ccdc_archive 'CCDC 293020' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C18 H10 N2 O10 Ru3' _chemical_formula_sum 'C18 H10 N2 O10 Ru3' _chemical_formula_weight 717.49 _chemical_absolute_configuration rmad 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 orthorhombic _symmetry_space_group_name_H-M 'P21 21 21' _symmetry_space_group_name_Hall 'P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 8.579(3) _cell_length_b 13.436(6) _cell_length_c 19.870(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2290.5(16) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description BLOCK _exptl_crystal_colour ORANGE _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.081 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1376 _exptl_absorpt_coefficient_mu 2.008 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.687 _exptl_absorpt_correction_T_max 0.818 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14753 _diffrn_reflns_av_R_equivalents 0.0313 _diffrn_reflns_av_sigmaI/netI 0.0199 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.83 _diffrn_reflns_theta_max 23.31 _reflns_number_total 3303 _reflns_number_gt 3177 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0234P)^2^+2.1245P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.05(4) _refine_ls_number_reflns 3303 _refine_ls_number_parameters 306 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0248 _refine_ls_R_factor_gt 0.0228 _refine_ls_wR_factor_ref 0.0525 _refine_ls_wR_factor_gt 0.0513 _refine_ls_goodness_of_fit_ref 1.086 _refine_ls_restrained_S_all 1.086 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.42260(5) 0.65747(3) 0.85440(2) 0.04786(12) Uani 1 1 d . . . Ru2 Ru 0.11987(5) 0.72386(3) 0.86398(2) 0.04731(12) Uani 1 1 d . . . Ru3 Ru 0.31835(5) 0.80992(3) 0.77144(2) 0.04185(11) Uani 1 1 d . . . C101 C 0.5578(7) 0.6303(4) 0.7812(3) 0.0586(15) Uani 1 1 d . . . O101 O 0.6368(6) 0.6136(3) 0.7374(3) 0.0849(14) Uani 1 1 d . . . C102 C 0.4537(8) 0.5415(5) 0.9116(3) 0.0690(18) Uani 1 1 d . . . O102 O 0.4731(8) 0.4742(4) 0.9443(3) 0.113(2) Uani 1 1 d . . . C103 C 0.5729(7) 0.7377(5) 0.8953(3) 0.0619(15) Uani 1 1 d . . . O103 O 0.6639(5) 0.7864(4) 0.9208(2) 0.0879(14) Uani 1 1 d . . . C201 C -0.0386(7) 0.7622(4) 0.8032(3) 0.0594(15) Uani 1 1 d . . . O201 O -0.1388(5) 0.7865(4) 0.7693(2) 0.0860(14) Uani 1 1 d . . . C202 C -0.0081(8) 0.6500(5) 0.9280(3) 0.0711(17) Uani 1 1 d . . . O202 O -0.0927(7) 0.6172(4) 0.9646(3) 0.112(2) Uani 1 1 d . . . C203 C 0.0971(7) 0.8433(5) 0.9110(3) 0.0661(16) Uani 1 1 d . . . O203 O 0.0826(7) 0.9148(4) 0.9398(3) 0.1024(18) Uani 1 1 d . . . C301 C 0.1818(7) 0.9043(4) 0.7279(3) 0.0531(13) Uani 1 1 d . . . O301 O 0.1077(6) 0.9639(3) 0.7034(2) 0.0806(13) Uani 1 1 d . . . C302 C 0.4976(7) 0.8379(4) 0.7165(3) 0.0536(14) Uani 1 1 d . . . O302 O 0.6007(6) 0.8597(4) 0.6854(2) 0.0937(16) Uani 1 1 d . . . C303 C 0.3831(7) 0.9015(4) 0.8366(3) 0.0585(14) Uani 1 1 d . . . O303 O 0.4240(6) 0.9587(3) 0.8752(2) 0.0853(14) Uani 1 1 d . . . N1 N 0.2117(5) 0.5982(3) 0.8090(2) 0.0508(12) Uani 1 1 d . . . N2 N 0.2443(5) 0.6871(3) 0.7110(2) 0.0475(11) Uani 1 1 d . . . O1 O 0.1839(5) 0.5267(3) 0.7029(2) 0.0659(11) Uani 1 1 d . . . C1 C 0.2125(6) 0.6057(4) 0.7408(3) 0.0497(13) Uani 1 1 d . . . C2 C 0.1895(9) 0.5608(4) 0.6341(3) 0.0732(17) Uani 1 1 d . . . H2A H 0.0870 0.5576 0.6136 0.088 Uiso 1 1 calc R . . H2B H 0.2608 0.5204 0.6078 0.088 Uiso 1 1 calc R . . C3 C 0.2470(6) 0.6691(4) 0.6376(3) 0.0527(13) Uani 1 1 d . . . H3 H 0.3549 0.6722 0.6216 0.063 Uiso 1 1 calc R . . C4 C 0.1510(7) 0.7429(4) 0.5996(3) 0.0544(14) Uani 1 1 d . . . C5 C -0.0094(8) 0.7495(5) 0.6090(3) 0.0720(18) Uani 1 1 d . . . H5 H -0.0584 0.7060 0.6387 0.086 Uiso 1 1 calc R . . C6 C -0.0971(9) 0.8195(6) 0.5749(4) 0.091(2) Uani 1 1 d . . . H6 H -0.2040 0.8242 0.5819 0.109 Uiso 1 1 calc R . . C7 C -0.0231(12) 0.8821(7) 0.5307(4) 0.099(3) Uani 1 1 d . . . H7 H -0.0812 0.9293 0.5074 0.119 Uiso 1 1 calc R . . C8 C 0.1303(12) 0.8767(5) 0.5204(4) 0.093(2) Uani 1 1 d . . . H8 H 0.1782 0.9193 0.4898 0.111 Uiso 1 1 calc R . . C9 C 0.2171(8) 0.8077(5) 0.5551(3) 0.0744(18) Uani 1 1 d . . . H9 H 0.3242 0.8051 0.5480 0.089 Uiso 1 1 calc R . . H1 H 0.188(5) 0.541(4) 0.824(2) 0.049(18) Uiso 1 1 d . . . H100 H 0.302(7) 0.703(5) 0.907(3) 0.087(19) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.0476(2) 0.0433(2) 0.0527(2) -0.0043(2) -0.0096(2) 0.00892(18) Ru2 0.0435(2) 0.0501(2) 0.0483(2) 0.0027(2) 0.00060(19) 0.00271(18) Ru3 0.0443(2) 0.0366(2) 0.0447(2) -0.00233(18) -0.00486(19) -0.00290(18) C101 0.051(3) 0.048(3) 0.077(4) -0.011(3) -0.009(3) 0.014(3) O101 0.075(3) 0.081(3) 0.098(3) -0.025(3) 0.021(3) 0.017(2) C102 0.097(5) 0.052(4) 0.058(4) -0.009(3) -0.026(3) 0.011(3) O102 0.190(6) 0.065(3) 0.082(3) 0.006(3) -0.054(4) 0.022(4) C103 0.052(3) 0.068(4) 0.066(3) -0.013(3) -0.007(3) 0.017(3) O103 0.064(3) 0.103(4) 0.097(3) -0.033(3) -0.024(3) -0.002(3) C201 0.049(3) 0.059(4) 0.070(4) 0.000(3) -0.001(3) -0.011(3) O201 0.049(2) 0.117(4) 0.092(3) 0.008(3) -0.020(2) 0.004(3) C202 0.068(4) 0.076(4) 0.070(4) 0.015(3) 0.008(3) 0.009(3) O202 0.106(4) 0.113(4) 0.116(4) 0.043(4) 0.055(4) 0.000(3) C203 0.067(4) 0.076(4) 0.055(3) -0.004(3) -0.006(3) 0.021(3) O203 0.126(4) 0.092(3) 0.089(3) -0.037(3) -0.002(3) 0.045(3) C301 0.056(3) 0.044(3) 0.059(3) -0.004(3) -0.003(3) -0.005(3) O301 0.081(3) 0.065(3) 0.096(3) 0.012(2) -0.017(3) 0.026(3) C302 0.049(3) 0.056(3) 0.055(3) 0.007(3) -0.013(3) -0.003(3) O302 0.067(3) 0.122(4) 0.092(3) 0.038(3) 0.011(3) -0.010(3) C303 0.070(4) 0.051(3) 0.055(3) 0.004(3) -0.005(3) 0.001(3) O303 0.128(4) 0.058(3) 0.070(3) -0.020(2) -0.019(3) -0.019(3) N1 0.056(3) 0.038(3) 0.059(3) 0.007(2) -0.004(2) -0.011(2) N2 0.051(2) 0.046(3) 0.046(2) -0.006(2) -0.0095(19) -0.004(2) O1 0.092(3) 0.041(2) 0.065(2) -0.0139(18) -0.005(2) -0.013(2) C1 0.046(3) 0.044(3) 0.059(4) -0.009(3) -0.005(3) -0.003(2) C2 0.098(5) 0.061(4) 0.060(4) -0.015(3) -0.010(4) -0.009(4) C3 0.058(3) 0.054(3) 0.046(3) -0.012(3) 0.001(3) -0.003(2) C4 0.070(4) 0.054(3) 0.039(3) -0.010(2) -0.011(3) -0.010(3) C5 0.063(4) 0.096(5) 0.056(3) -0.005(3) -0.008(3) -0.005(4) C6 0.073(5) 0.121(6) 0.078(5) -0.024(5) -0.027(4) 0.018(5) C7 0.118(8) 0.096(6) 0.082(5) -0.008(5) -0.043(6) 0.019(5) C8 0.135(8) 0.070(5) 0.073(5) 0.009(4) -0.011(5) -0.008(5) C9 0.093(5) 0.072(4) 0.058(4) -0.008(4) -0.002(3) -0.004(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 C103 1.867(7) . ? Ru1 C101 1.895(6) . ? Ru1 C102 1.947(6) . ? Ru1 N1 2.173(5) . ? Ru1 Ru2 2.7528(11) . ? Ru1 Ru3 2.7773(9) . ? Ru1 H100 1.59(6) . ? Ru2 C203 1.867(7) . ? Ru2 C201 1.889(6) . ? Ru2 C202 1.951(7) . ? Ru2 N1 2.159(5) . ? Ru2 Ru3 2.7600(9) . ? Ru2 H100 1.81(6) . ? Ru3 C303 1.871(6) . ? Ru3 C302 1.923(6) . ? Ru3 C301 1.930(6) . ? Ru3 N2 2.137(4) . ? C101 O101 1.127(7) . ? C102 O102 1.126(7) . ? C103 O103 1.138(7) . ? C201 O201 1.141(7) . ? C202 O202 1.118(7) . ? C203 O203 1.125(7) . ? C301 O301 1.133(6) . ? C302 O302 1.118(7) . ? C303 O303 1.140(7) . ? N1 C1 1.359(7) . ? N1 H1 0.84(5) . ? N2 C1 1.274(7) . ? N2 C3 1.479(6) . ? O1 C1 1.324(6) . ? O1 C2 1.444(7) . ? C2 C3 1.538(7) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C4 1.494(8) . ? C3 H3 0.9800 . ? C4 C9 1.364(8) . ? C4 C5 1.392(8) . ? C5 C6 1.382(10) . ? C5 H5 0.9300 . ? C6 C7 1.372(12) . ? C6 H6 0.9300 . ? C7 C8 1.334(12) . ? C7 H7 0.9300 . ? C8 C9 1.375(10) . ? C8 H8 0.9300 . ? C9 H9 0.9300 . ? 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 C103 Ru1 C101 91.3(3) . . ? C103 Ru1 C102 96.5(3) . . ? C101 Ru1 C102 102.1(3) . . ? C103 Ru1 N1 165.3(2) . . ? C101 Ru1 N1 96.9(2) . . ? C102 Ru1 N1 93.6(2) . . ? C103 Ru1 Ru2 115.76(17) . . ? C101 Ru1 Ru2 133.86(17) . . ? C102 Ru1 Ru2 110.4(2) . . ? N1 Ru1 Ru2 50.33(13) . . ? C103 Ru1 Ru3 93.14(18) . . ? C101 Ru1 Ru3 83.33(17) . . ? C102 Ru1 Ru3 168.8(2) . . ? N1 Ru1 Ru3 75.86(13) . . ? Ru2 Ru1 Ru3 59.878(17) . . ? C103 Ru1 H100 87(2) . . ? C101 Ru1 H100 167(2) . . ? C102 Ru1 H100 91(2) . . ? N1 Ru1 H100 83(2) . . ? Ru2 Ru1 H100 39(2) . . ? Ru3 Ru1 H100 84(2) . . ? C203 Ru2 C201 90.6(3) . . ? C203 Ru2 C202 93.0(3) . . ? C201 Ru2 C202 98.7(3) . . ? C203 Ru2 N1 164.4(2) . . ? C201 Ru2 N1 98.8(2) . . ? C202 Ru2 N1 97.9(2) . . ? C203 Ru2 Ru1 114.3(2) . . ? C201 Ru2 Ru1 136.30(17) . . ? C202 Ru2 Ru1 114.27(19) . . ? N1 Ru2 Ru1 50.76(12) . . ? C203 Ru2 Ru3 92.1(2) . . ? C201 Ru2 Ru3 84.50(17) . . ? C202 Ru2 Ru3 173.95(19) . . ? N1 Ru2 Ru3 76.44(13) . . ? Ru1 Ru2 Ru3 60.50(2) . . ? C203 Ru2 H100 89(2) . . ? C201 Ru2 H100 166(2) . . ? C202 Ru2 H100 95.7(19) . . ? N1 Ru2 H100 79(2) . . ? Ru1 Ru2 H100 33.3(19) . . ? Ru3 Ru2 H100 81.2(19) . . ? C303 Ru3 C302 91.6(3) . . ? C303 Ru3 C301 93.3(2) . . ? C302 Ru3 C301 95.9(2) . . ? C303 Ru3 N2 170.0(2) . . ? C302 Ru3 N2 94.0(2) . . ? C301 Ru3 N2 94.3(2) . . ? C303 Ru3 Ru2 89.84(18) . . ? C302 Ru3 Ru2 162.43(16) . . ? C301 Ru3 Ru2 101.48(18) . . ? N2 Ru3 Ru2 82.37(12) . . ? C303 Ru3 Ru1 88.76(17) . . ? C302 Ru3 Ru1 102.90(16) . . ? C301 Ru3 Ru1 161.01(17) . . ? N2 Ru3 Ru1 81.92(12) . . ? Ru2 Ru3 Ru1 59.62(1) . . ? O101 C101 Ru1 179.2(6) . . ? O102 C102 Ru1 179.3(7) . . ? O103 C103 Ru1 179.3(6) . . ? O201 C201 Ru2 176.6(5) . . ? O202 C202 Ru2 171.8(6) . . ? O203 C203 Ru2 179.3(7) . . ? O301 C301 Ru3 176.0(5) . . ? O302 C302 Ru3 176.0(6) . . ? O303 C303 Ru3 178.4(5) . . ? C1 N1 Ru2 116.7(4) . . ? C1 N1 Ru1 112.5(4) . . ? Ru2 N1 Ru1 78.91(15) . . ? C1 N1 H1 114(3) . . ? Ru2 N1 H1 117(3) . . ? Ru1 N1 H1 113(3) . . ? C1 N2 C3 108.7(4) . . ? C1 N2 Ru3 117.8(4) . . ? C3 N2 Ru3 132.5(4) . . ? C1 O1 C2 106.1(4) . . ? N2 C1 O1 117.7(5) . . ? N2 C1 N1 121.8(5) . . ? O1 C1 N1 120.5(5) . . ? O1 C2 C3 105.5(4) . . ? O1 C2 H2A 110.6 . . ? C3 C2 H2A 110.6 . . ? O1 C2 H2B 110.6 . . ? C3 C2 H2B 110.6 . . ? H2A C2 H2B 108.8 . . ? N2 C3 C4 112.4(4) . . ? N2 C3 C2 101.3(5) . . ? C4 C3 C2 115.3(5) . . ? N2 C3 H3 109.2 . . ? C4 C3 H3 109.2 . . ? C2 C3 H3 109.2 . . ? C9 C4 C5 117.3(6) . . ? C9 C4 C3 121.5(6) . . ? C5 C4 C3 121.3(6) . . ? C6 C5 C4 121.0(7) . . ? C6 C5 H5 119.5 . . ? C4 C5 H5 119.5 . . ? C7 C6 C5 118.7(7) . . ? C7 C6 H6 120.7 . . ? C5 C6 H6 120.7 . . ? C8 C7 C6 121.4(8) . . ? C8 C7 H7 119.3 . . ? C6 C7 H7 119.3 . . ? C7 C8 C9 119.7(8) . . ? C7 C8 H8 120.2 . . ? C9 C8 H8 120.2 . . ? C4 C9 C8 122.0(7) . . ? C4 C9 H9 119.0 . . ? C8 C9 H9 119.0 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 23.31 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.303 _refine_diff_density_min -0.375 _refine_diff_density_rms 0.061 #===END data_3_(ids229am) _database_code_depnum_ccdc_archive 'CCDC 293021' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C19 H10 N2 O10 Ru3' _chemical_formula_sum 'C19 H10 N2 O10 Ru3' _chemical_formula_weight 729.50 _chemical_absolute_configuration rmad 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 orthorhombic _symmetry_space_group_name_H-M 'P21 21 21' _symmetry_space_group_name_Hall 'P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 7.4658(13) _cell_length_b 15.525(3) _cell_length_c 19.898(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2306.3(8) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description BLOCK _exptl_crystal_colour ORANGE _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.101 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1400 _exptl_absorpt_coefficient_mu 1.996 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.629 _exptl_absorpt_correction_T_max 0.819 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15461 _diffrn_reflns_av_R_equivalents 0.0232 _diffrn_reflns_av_sigmaI/netI 0.0128 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.66 _diffrn_reflns_theta_max 23.27 _reflns_number_total 3316 _reflns_number_gt 3278 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0206P)^2^+0.9327P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00223(10) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.04(3) _refine_ls_number_reflns 3316 _refine_ls_number_parameters 316 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0150 _refine_ls_R_factor_gt 0.0147 _refine_ls_wR_factor_ref 0.0367 _refine_ls_wR_factor_gt 0.0365 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.030 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.83093(4) 1.000312(15) 0.291058(12) 0.04154(8) Uani 1 1 d . . . Ru2 Ru 0.82860(4) 0.823000(15) 0.305775(13) 0.04425(8) Uani 1 1 d . . . Ru3 Ru 0.56605(3) 0.922551(16) 0.366734(14) 0.04300(8) Uani 1 1 d . . . C101 C 0.7922(5) 1.0930(2) 0.35196(17) 0.0523(8) Uani 1 1 d . . . O101 O 0.7712(4) 1.14817(16) 0.38828(14) 0.0743(8) Uani 1 1 d . . . C102 C 1.0380(6) 1.0399(2) 0.2414(2) 0.0585(10) Uani 1 1 d . . . O102 O 1.1491(5) 1.0689(2) 0.21076(19) 0.0974(11) Uani 1 1 d . . . C103 C 0.6758(6) 1.0497(2) 0.22825(18) 0.0546(9) Uani 1 1 d . . . O103 O 0.5836(5) 1.07998(19) 0.18934(14) 0.0799(8) Uani 1 1 d . . . C201 C 0.7985(6) 0.7440(2) 0.3771(2) 0.0615(10) Uani 1 1 d . . . O201 O 0.7846(6) 0.6956(2) 0.41976(15) 0.0928(11) Uani 1 1 d . . . C202 C 1.0413(6) 0.7728(2) 0.2664(2) 0.0615(10) Uani 1 1 d . . . O202 O 1.1619(5) 0.73918(19) 0.2468(2) 0.1025(12) Uani 1 1 d . . . C203 C 0.6715(6) 0.7592(2) 0.25118(19) 0.0568(9) Uani 1 1 d . . . O203 O 0.5783(5) 0.72002(19) 0.21764(16) 0.0797(8) Uani 1 1 d . . . C301 C 0.4346(6) 0.8307(2) 0.40953(19) 0.0602(9) Uani 1 1 d . . . O301 O 0.3508(5) 0.77530(19) 0.42900(18) 0.0964(11) Uani 1 1 d . . . C302 C 0.4233(6) 1.0214(2) 0.39117(18) 0.0566(9) Uani 1 1 d . . . O302 O 0.3256(4) 1.07698(18) 0.39815(15) 0.0805(8) Uani 1 1 d . . . C303 C 0.4461(5) 0.9102(2) 0.2855(2) 0.0558(9) Uani 1 1 d . . . O303 O 0.3699(4) 0.90413(18) 0.23569(16) 0.0758(8) Uani 1 1 d . . . N1 N 0.9730(4) 0.91915(18) 0.35991(14) 0.0451(6) Uani 1 1 d . . . N2 N 0.7641(4) 0.93477(17) 0.44599(13) 0.0431(6) Uani 1 1 d . . . C1 C 0.9264(5) 0.92897(19) 0.42617(15) 0.0425(7) Uani 1 1 d . . . O1 O 1.0574(3) 0.93128(17) 0.47150(11) 0.0580(6) Uani 1 1 d . . . C2 C 0.9693(5) 0.9529(3) 0.53504(18) 0.0626(11) Uani 1 1 d . . . H2 H 1.0048 0.9131 0.5709 0.075 Uiso 1 1 calc R . . C3 C 0.7669(5) 0.9460(2) 0.51988(17) 0.0516(9) Uani 1 1 d . . . H3 H 0.7112 0.8973 0.5433 0.062 Uiso 1 1 calc R . . C4 C 0.6930(5) 1.0307(2) 0.54293(16) 0.0533(9) Uani 1 1 d . . . C5 C 0.5160(6) 1.0559(3) 0.5486(2) 0.0720(12) Uani 1 1 d . . . H5 H 0.4233 1.0176 0.5395 0.086 Uiso 1 1 calc R . . C6 C 0.4808(7) 1.1401(4) 0.5681(3) 0.0958(17) Uani 1 1 d . . . H6 H 0.3626 1.1585 0.5716 0.115 Uiso 1 1 calc R . . C7 C 0.6143(7) 1.1957(3) 0.5821(3) 0.0957(17) Uani 1 1 d . . . H7 H 0.5865 1.2518 0.5947 0.115 Uiso 1 1 calc R . . C8 C 0.7910(7) 1.1710(3) 0.5782(2) 0.0802(13) Uani 1 1 d . . . H8 H 0.8824 1.2095 0.5883 0.096 Uiso 1 1 calc R . . C9 C 0.8294(5) 1.0873(3) 0.55890(17) 0.0586(9) Uani 1 1 d . . . C10 C 1.0081(6) 1.0451(3) 0.5539(2) 0.0713(12) Uani 1 1 d . . . H10A H 1.0707 1.0479 0.5966 0.086 Uiso 1 1 calc R . . H10B H 1.0810 1.0727 0.5198 0.086 Uiso 1 1 calc R . . H100 H 0.821(6) 0.911(3) 0.246(2) 0.091(13) Uiso 1 1 d . . . H1 H 1.072(4) 0.9179(16) 0.3594(12) 0.061(6) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.05000(16) 0.02836(13) 0.04625(14) 0.00111(10) 0.00668(12) -0.00491(13) Ru2 0.05273(16) 0.02753(12) 0.05249(15) -0.00186(11) 0.01402(13) -0.00138(12) Ru3 0.04280(14) 0.03322(13) 0.05296(15) -0.00085(12) 0.00870(12) -0.00166(12) C101 0.069(2) 0.0323(17) 0.0555(19) 0.0020(16) -0.0020(17) -0.0049(17) O101 0.107(2) 0.0442(14) 0.0717(17) -0.0145(14) 0.0067(16) -0.0095(15) C102 0.063(2) 0.0379(17) 0.074(2) 0.0106(17) 0.016(2) -0.0037(18) O102 0.083(2) 0.0674(18) 0.142(3) 0.0345(19) 0.048(2) -0.0008(18) C103 0.072(2) 0.0405(18) 0.0508(19) -0.0019(15) 0.006(2) -0.008(2) O103 0.100(2) 0.0734(18) 0.0666(17) 0.0056(15) -0.0189(17) 0.0108(19) C201 0.079(3) 0.0394(17) 0.067(2) -0.0022(18) 0.012(2) -0.0078(19) O201 0.138(3) 0.0660(18) 0.0737(18) 0.0221(16) 0.010(2) -0.015(2) C202 0.067(3) 0.0308(17) 0.086(3) -0.0144(17) 0.024(2) -0.0043(18) O202 0.082(2) 0.0600(18) 0.165(3) -0.039(2) 0.054(3) 0.0008(19) C203 0.068(2) 0.0382(18) 0.064(2) -0.0021(17) 0.019(2) -0.004(2) O203 0.090(2) 0.0621(16) 0.087(2) -0.0087(15) -0.0011(19) -0.0204(17) C301 0.063(2) 0.051(2) 0.067(2) -0.0030(18) 0.012(2) 0.002(2) O301 0.103(3) 0.0609(18) 0.125(3) 0.0123(17) 0.046(2) -0.0264(19) C302 0.056(2) 0.048(2) 0.066(2) -0.0019(16) 0.0068(19) -0.004(2) O302 0.0764(18) 0.0590(16) 0.106(2) -0.0008(15) 0.0123(17) 0.0269(19) C303 0.053(2) 0.0387(18) 0.076(2) 0.0027(17) 0.008(2) 0.0002(18) O303 0.077(2) 0.0686(18) 0.0820(19) -0.0003(15) -0.0225(16) -0.0096(15) N1 0.0355(16) 0.0407(14) 0.0591(18) 0.0013(13) 0.0089(13) 0.0009(14) N2 0.0465(16) 0.0385(15) 0.0444(13) -0.0020(12) 0.0074(12) 0.0019(12) C1 0.0496(19) 0.0343(16) 0.0438(17) 0.0022(13) 0.0004(16) 0.0047(16) O1 0.0516(13) 0.0765(17) 0.0459(12) -0.0025(12) 0.0051(12) 0.0163(14) C2 0.061(2) 0.084(3) 0.0434(19) 0.0043(18) 0.0037(18) 0.022(2) C3 0.062(2) 0.047(2) 0.0449(18) 0.0063(15) 0.0089(16) 0.0044(16) C4 0.055(2) 0.061(2) 0.0440(17) -0.0069(15) 0.0039(17) 0.0017(18) C5 0.054(2) 0.078(3) 0.083(3) -0.025(2) 0.008(2) 0.005(2) C6 0.067(3) 0.103(4) 0.117(4) -0.052(3) -0.001(3) 0.028(3) C7 0.096(4) 0.075(3) 0.116(4) -0.050(3) -0.002(3) 0.020(3) C8 0.084(4) 0.075(3) 0.081(3) -0.032(2) 0.005(3) -0.015(3) C9 0.055(2) 0.070(2) 0.0507(18) -0.0127(18) 0.0052(18) 0.001(2) C10 0.055(2) 0.098(3) 0.061(2) -0.020(2) -0.0012(19) 0.003(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 C103 1.869(4) . ? Ru1 C101 1.904(4) . ? Ru1 C102 1.935(4) . ? Ru1 N1 2.142(3) . ? Ru1 Ru3 2.7633(5) . ? Ru1 Ru2 2.7684(6) . ? Ru1 H100 1.65(4) . ? Ru2 C203 1.881(5) . ? Ru2 C201 1.889(4) . ? Ru2 C202 1.935(4) . ? Ru2 N1 2.133(3) . ? Ru2 Ru3 2.7753(5) . ? Ru2 H100 1.81(4) . ? Ru3 C303 1.857(4) . ? Ru3 C301 1.929(4) . ? Ru3 C302 1.931(4) . ? Ru3 N2 2.170(3) . ? C101 O101 1.131(4) . ? C102 O102 1.124(5) . ? C103 O103 1.137(5) . ? C201 O201 1.139(4) . ? C202 O202 1.111(5) . ? C203 O203 1.140(5) . ? C301 O301 1.133(4) . ? C302 O302 1.137(4) . ? C303 O303 1.147(4) . ? N1 C1 1.372(4) . ? N1 H1 0.74(3) . ? N2 C1 1.278(4) . ? N2 C3 1.481(4) . ? C1 O1 1.331(4) . ? O1 C2 1.464(4) . ? C2 C10 1.508(6) . ? C2 C3 1.544(6) . ? C2 H2 0.9800 . ? C3 C4 1.498(5) . ? C3 H3 0.9800 . ? C4 C9 1.382(6) . ? C4 C5 1.383(6) . ? C5 C6 1.388(6) . ? C5 H5 0.9300 . ? C6 C7 1.348(7) . ? C6 H6 0.9300 . ? C7 C8 1.376(7) . ? C7 H7 0.9300 . ? C8 C9 1.384(6) . ? C8 H8 0.9300 . ? C9 C10 1.490(6) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? 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 C103 Ru1 C101 91.22(15) . . ? C103 Ru1 C102 91.32(18) . . ? C101 Ru1 C102 101.90(16) . . ? C103 Ru1 N1 167.42(14) . . ? C101 Ru1 N1 96.48(13) . . ? C102 Ru1 N1 96.79(14) . . ? C103 Ru1 Ru3 95.75(12) . . ? C101 Ru1 Ru3 82.81(11) . . ? C102 Ru1 Ru3 171.44(11) . . ? N1 Ru1 Ru3 75.45(8) . . ? C103 Ru1 Ru2 118.36(10) . . ? C101 Ru1 Ru2 133.13(10) . . ? C102 Ru1 Ru2 112.03(11) . . ? N1 Ru1 Ru2 49.50(8) . . ? Ru3 Ru1 Ru2 60.227(10) . . ? C103 Ru1 H100 87.5(15) . . ? C101 Ru1 H100 166.6(16) . . ? C102 Ru1 H100 91.5(16) . . ? N1 Ru1 H100 82.7(15) . . ? Ru3 Ru1 H100 84.0(15) . . ? Ru2 Ru1 H100 38.8(15) . . ? C203 Ru2 C201 91.04(16) . . ? C203 Ru2 C202 93.80(17) . . ? C201 Ru2 C202 98.07(17) . . ? C203 Ru2 N1 167.24(14) . . ? C201 Ru2 N1 97.76(14) . . ? C202 Ru2 N1 94.10(14) . . ? C203 Ru2 Ru1 117.79(11) . . ? C201 Ru2 Ru1 136.53(11) . . ? C202 Ru2 Ru1 110.63(10) . . ? N1 Ru2 Ru1 49.79(8) . . ? C203 Ru2 Ru3 96.03(12) . . ? C201 Ru2 Ru3 87.09(12) . . ? C202 Ru2 Ru3 168.82(11) . . ? N1 Ru2 Ru3 75.31(8) . . ? Ru1 Ru2 Ru3 59.795(11) . . ? C203 Ru2 H100 90.1(14) . . ? C201 Ru2 H100 168.1(14) . . ? C202 Ru2 H100 93.7(14) . . ? N1 Ru2 H100 79.4(14) . . ? Ru1 Ru2 H100 34.9(13) . . ? Ru3 Ru2 H100 81.0(14) . . ? C303 Ru3 C301 93.57(16) . . ? C303 Ru3 C302 92.02(16) . . ? C301 Ru3 C302 101.28(16) . . ? C303 Ru3 N2 165.87(13) . . ? C301 Ru3 N2 95.19(14) . . ? C302 Ru3 N2 97.10(13) . . ? C303 Ru3 Ru1 85.19(11) . . ? C301 Ru3 Ru1 158.06(12) . . ? C302 Ru3 Ru1 100.66(11) . . ? N2 Ru3 Ru1 82.54(7) . . ? C303 Ru3 Ru2 84.41(11) . . ? C301 Ru3 Ru2 98.09(12) . . ? C302 Ru3 Ru2 160.49(11) . . ? N2 Ru3 Ru2 83.40(7) . . ? Ru1 Ru3 Ru2 59.978(14) . . ? O101 C101 Ru1 179.2(3) . . ? O102 C102 Ru1 173.8(3) . . ? O103 C103 Ru1 178.9(4) . . ? O201 C201 Ru2 178.3(4) . . ? O202 C202 Ru2 175.0(4) . . ? O203 C203 Ru2 179.0(4) . . ? O301 C301 Ru3 173.7(4) . . ? O302 C302 Ru3 170.7(4) . . ? O303 C303 Ru3 178.5(3) . . ? C1 N1 Ru2 115.8(2) . . ? C1 N1 Ru1 115.1(2) . . ? Ru2 N1 Ru1 80.71(11) . . ? C1 N1 H1 105.6(19) . . ? Ru2 N1 H1 119(2) . . ? Ru1 N1 H1 120(2) . . ? C1 N2 C3 107.5(3) . . ? C1 N2 Ru3 114.6(2) . . ? C3 N2 Ru3 137.9(2) . . ? N2 C1 O1 119.1(3) . . ? N2 C1 N1 123.0(3) . . ? O1 C1 N1 117.9(3) . . ? C1 O1 C2 105.1(3) . . ? O1 C2 C10 110.2(3) . . ? O1 C2 C3 104.8(3) . . ? C10 C2 C3 107.6(3) . . ? O1 C2 H2 111.3 . . ? C10 C2 H2 111.3 . . ? C3 C2 H2 111.3 . . ? N2 C3 C4 113.7(3) . . ? N2 C3 C2 102.5(3) . . ? C4 C3 C2 103.9(3) . . ? N2 C3 H3 112.0 . . ? C4 C3 H3 112.0 . . ? C2 C3 H3 112.0 . . ? C9 C4 C5 120.4(4) . . ? C9 C4 C3 110.9(3) . . ? C5 C4 C3 128.7(4) . . ? C4 C5 C6 118.1(4) . . ? C4 C5 H5 121.0 . . ? C6 C5 H5 121.0 . . ? C7 C6 C5 121.3(4) . . ? C7 C6 H6 119.3 . . ? C5 C6 H6 119.3 . . ? C6 C7 C8 121.3(4) . . ? C6 C7 H7 119.4 . . ? C8 C7 H7 119.4 . . ? C7 C8 C9 118.4(5) . . ? C7 C8 H8 120.8 . . ? C9 C8 H8 120.8 . . ? C4 C9 C8 120.5(4) . . ? C4 C9 C10 111.4(3) . . ? C8 C9 C10 128.1(4) . . ? C9 C10 C2 105.2(3) . . ? C9 C10 H10A 110.7 . . ? C2 C10 H10A 110.7 . . ? C9 C10 H10B 110.7 . . ? C2 C10 H10B 110.7 . . ? H10A C10 H10B 108.8 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C103 Ru1 Ru2 C203 0.47(19) . . . . ? C101 Ru1 Ru2 C203 123.1(2) . . . . ? C102 Ru1 Ru2 C203 -103.80(19) . . . . ? N1 Ru1 Ru2 C203 176.44(16) . . . . ? Ru3 Ru1 Ru2 C203 80.24(13) . . . . ? C103 Ru1 Ru2 C201 -125.4(2) . . . . ? C101 Ru1 Ru2 C201 -2.8(3) . . . . ? C102 Ru1 Ru2 C201 130.3(2) . . . . ? N1 Ru1 Ru2 C201 50.6(2) . . . . ? Ru3 Ru1 Ru2 C201 -45.6(2) . . . . ? C103 Ru1 Ru2 C202 106.64(19) . . . . ? C101 Ru1 Ru2 C202 -130.8(2) . . . . ? C102 Ru1 Ru2 C202 2.4(2) . . . . ? N1 Ru1 Ru2 C202 -77.39(17) . . . . ? Ru3 Ru1 Ru2 C202 -173.59(14) . . . . ? C103 Ru1 Ru2 N1 -175.97(17) . . . . ? C101 Ru1 Ru2 N1 -53.38(18) . . . . ? C102 Ru1 Ru2 N1 79.75(17) . . . . ? Ru3 Ru1 Ru2 N1 -96.20(10) . . . . ? C103 Ru1 Ru2 Ru3 -79.77(13) . . . . ? C101 Ru1 Ru2 Ru3 42.82(15) . . . . ? C102 Ru1 Ru2 Ru3 175.95(14) . . . . ? N1 Ru1 Ru2 Ru3 96.20(10) . . . . ? C103 Ru1 Ru3 C303 33.18(15) . . . . ? C101 Ru1 Ru3 C303 123.68(15) . . . . ? N1 Ru1 Ru3 C303 -137.67(13) . . . . ? Ru2 Ru1 Ru3 C303 -86.31(10) . . . . ? C103 Ru1 Ru3 C301 120.8(3) . . . . ? C101 Ru1 Ru3 C301 -148.7(4) . . . . ? N1 Ru1 Ru3 C301 -50.1(3) . . . . ? Ru2 Ru1 Ru3 C301 1.3(3) . . . . ? C103 Ru1 Ru3 C302 -57.97(15) . . . . ? C101 Ru1 Ru3 C302 32.53(16) . . . . ? N1 Ru1 Ru3 C302 131.18(14) . . . . ? Ru2 Ru1 Ru3 C302 -177.47(12) . . . . ? C103 Ru1 Ru3 N2 -153.84(12) . . . . ? C101 Ru1 Ru3 N2 -63.34(13) . . . . ? N1 Ru1 Ru3 N2 35.31(11) . . . . ? Ru2 Ru1 Ru3 N2 86.66(7) . . . . ? C103 Ru1 Ru3 Ru2 119.49(10) . . . . ? C101 Ru1 Ru3 Ru2 -150.00(11) . . . . ? N1 Ru1 Ru3 Ru2 -51.36(8) . . . . ? C203 Ru2 Ru3 C303 -31.09(15) . . . . ? C201 Ru2 Ru3 C303 -121.82(16) . . . . ? C202 Ru2 Ru3 C303 120.3(7) . . . . ? N1 Ru2 Ru3 C303 139.37(13) . . . . ? Ru1 Ru2 Ru3 C303 87.67(11) . . . . ? C203 Ru2 Ru3 C301 61.74(16) . . . . ? C201 Ru2 Ru3 C301 -29.00(18) . . . . ? C202 Ru2 Ru3 C301 -146.9(7) . . . . ? N1 Ru2 Ru3 C301 -127.80(15) . . . . ? Ru1 Ru2 Ru3 C301 -179.51(13) . . . . ? C203 Ru2 Ru3 C302 -111.3(4) . . . . ? C201 Ru2 Ru3 C302 158.0(4) . . . . ? C202 Ru2 Ru3 C302 40.1(8) . . . . ? N1 Ru2 Ru3 C302 59.2(4) . . . . ? Ru1 Ru2 Ru3 C302 7.5(4) . . . . ? C203 Ru2 Ru3 N2 156.07(13) . . . . ? C201 Ru2 Ru3 N2 65.33(14) . . . . ? C202 Ru2 Ru3 N2 -52.6(7) . . . . ? N1 Ru2 Ru3 N2 -33.47(11) . . . . ? Ru1 Ru2 Ru3 N2 -85.18(7) . . . . ? C203 Ru2 Ru3 Ru1 -118.75(11) . . . . ? C201 Ru2 Ru3 Ru1 150.51(12) . . . . ? C202 Ru2 Ru3 Ru1 32.6(7) . . . . ? N1 Ru2 Ru3 Ru1 51.71(8) . . . . ? C203 Ru2 N1 C1 99.1(6) . . . . ? C201 Ru2 N1 C1 -34.1(3) . . . . ? C202 Ru2 N1 C1 -132.8(3) . . . . ? Ru1 Ru2 N1 C1 113.5(3) . . . . ? Ru3 Ru2 N1 C1 50.8(2) . . . . ? C203 Ru2 N1 Ru1 -14.4(6) . . . . ? C201 Ru2 N1 Ru1 -147.57(14) . . . . ? C202 Ru2 N1 Ru1 113.70(14) . . . . ? Ru3 Ru2 N1 Ru1 -62.65(6) . . . . ? C103 Ru1 N1 C1 -97.7(7) . . . . ? C101 Ru1 N1 C1 29.7(3) . . . . ? C102 Ru1 N1 C1 132.5(2) . . . . ? Ru3 Ru1 N1 C1 -51.2(2) . . . . ? Ru2 Ru1 N1 C1 -114.2(3) . . . . ? C103 Ru1 N1 Ru2 16.5(7) . . . . ? C101 Ru1 N1 Ru2 143.88(12) . . . . ? C102 Ru1 N1 Ru2 -113.27(13) . . . . ? Ru3 Ru1 N1 Ru2 63.06(6) . . . . ? C303 Ru3 N2 C1 -2.3(6) . . . . ? C301 Ru3 N2 C1 125.7(2) . . . . ? C302 Ru3 N2 C1 -132.2(2) . . . . ? Ru1 Ru3 N2 C1 -32.3(2) . . . . ? Ru2 Ru3 N2 C1 28.2(2) . . . . ? C303 Ru3 N2 C3 179.9(5) . . . . ? C301 Ru3 N2 C3 -52.0(3) . . . . ? C302 Ru3 N2 C3 50.1(3) . . . . ? Ru1 Ru3 N2 C3 149.9(3) . . . . ? Ru2 Ru3 N2 C3 -149.6(3) . . . . ? C3 N2 C1 O1 1.8(4) . . . . ? Ru3 N2 C1 O1 -176.6(2) . . . . ? C3 N2 C1 N1 -179.2(3) . . . . ? Ru3 N2 C1 N1 2.4(4) . . . . ? Ru2 N1 C1 N2 -47.4(4) . . . . ? Ru1 N1 C1 N2 44.2(4) . . . . ? Ru2 N1 C1 O1 131.6(3) . . . . ? Ru1 N1 C1 O1 -136.7(2) . . . . ? N2 C1 O1 C2 -7.8(4) . . . . ? N1 C1 O1 C2 173.1(3) . . . . ? C1 O1 C2 C10 -105.7(3) . . . . ? C1 O1 C2 C3 9.8(4) . . . . ? C1 N2 C3 C4 116.1(3) . . . . ? Ru3 N2 C3 C4 -66.0(4) . . . . ? C1 N2 C3 C2 4.7(4) . . . . ? Ru3 N2 C3 C2 -177.4(3) . . . . ? O1 C2 C3 N2 -8.7(4) . . . . ? C10 C2 C3 N2 108.6(3) . . . . ? O1 C2 C3 C4 -127.4(3) . . . . ? C10 C2 C3 C4 -10.0(4) . . . . ? N2 C3 C4 C9 -101.5(4) . . . . ? C2 C3 C4 C9 9.1(4) . . . . ? N2 C3 C4 C5 77.8(5) . . . . ? C2 C3 C4 C5 -171.6(4) . . . . ? C9 C4 C5 C6 2.4(6) . . . . ? C3 C4 C5 C6 -176.8(4) . . . . ? C4 C5 C6 C7 -0.9(8) . . . . ? C5 C6 C7 C8 -0.6(9) . . . . ? C6 C7 C8 C9 0.5(9) . . . . ? C5 C4 C9 C8 -2.5(6) . . . . ? C3 C4 C9 C8 176.8(4) . . . . ? C5 C4 C9 C10 175.9(4) . . . . ? C3 C4 C9 C10 -4.7(4) . . . . ? C7 C8 C9 C4 1.0(7) . . . . ? C7 C8 C9 C10 -177.1(5) . . . . ? C4 C9 C10 C2 -1.9(4) . . . . ? C8 C9 C10 C2 176.4(4) . . . . ? O1 C2 C10 C9 121.2(3) . . . . ? C3 C2 C10 C9 7.5(4) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 23.27 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.224 _refine_diff_density_min -0.215 _refine_diff_density_rms 0.043 #===END data_3_(ids227am) _database_code_depnum_ccdc_archive 'CCDC 293022' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C25 H14 N2 O10 Ru3' _chemical_formula_sum 'C25 H14 N2 O10 Ru3' _chemical_formula_weight 805.59 _chemical_absolute_configuration rmad loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Ru Ru -1.2594 0.8363 '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' C C 0.0033 0.0016 '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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' _symmetry_space_group_name_Hall 'P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 7.758(3) _cell_length_b 17.703(7) _cell_length_c 19.581(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2689.3(18) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description NEEDLE _exptl_crystal_colour ORANGE _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.990 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1560 _exptl_absorpt_coefficient_mu 1.722 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.713 _exptl_absorpt_correction_T_max 0.886 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17278 _diffrn_reflns_av_R_equivalents 0.0270 _diffrn_reflns_av_sigmaI/netI 0.0192 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.55 _diffrn_reflns_theta_max 23.25 _reflns_number_total 3872 _reflns_number_gt 3683 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0234P)^2^+2.4025P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.03(4) _refine_ls_number_reflns 3872 _refine_ls_number_parameters 359 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0241 _refine_ls_R_factor_gt 0.0212 _refine_ls_wR_factor_ref 0.0495 _refine_ls_wR_factor_gt 0.0480 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.047 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.08072(5) 0.181331(18) 0.765068(17) 0.03267(9) Uani 1 1 d . . . Ru2 Ru 0.16594(5) 0.07607(2) 0.665126(18) 0.03834(10) Uani 1 1 d . . . Ru3 Ru 0.08293(6) 0.22589(2) 0.628137(18) 0.04025(10) Uani 1 1 d . . . N1 N 0.3189(5) 0.1266(2) 0.74584(19) 0.0360(9) Uani 1 1 d . . . N2 N 0.0746(5) 0.12160(19) 0.85906(16) 0.0358(8) Uani 1 1 d . . . C101 C 0.1625(7) 0.2750(3) 0.7925(2) 0.0482(12) Uani 1 1 d . . . O101 O 0.2110(6) 0.3346(2) 0.8061(2) 0.0736(12) Uani 1 1 d . . . C102 C -0.1453(7) 0.2164(3) 0.7710(2) 0.0406(11) Uani 1 1 d . . . O102 O -0.2854(5) 0.2361(2) 0.77562(19) 0.0580(10) Uani 1 1 d . . . C201 C 0.2065(8) -0.0265(3) 0.6965(3) 0.0557(15) Uani 1 1 d . . . O201 O 0.2279(8) -0.0869(2) 0.7085(3) 0.1009(17) Uani 1 1 d . . . C202 C 0.3373(7) 0.0826(3) 0.5948(3) 0.0526(13) Uani 1 1 d . . . O202 O 0.4351(6) 0.0860(3) 0.5520(2) 0.0765(12) Uani 1 1 d . . . C203 C 0.0004(8) 0.0432(3) 0.6015(3) 0.0562(14) Uani 1 1 d . . . O203 O -0.0967(7) 0.0219(3) 0.5625(2) 0.0921(15) Uani 1 1 d . . . C301 C 0.3184(8) 0.2553(3) 0.6498(3) 0.0483(13) Uani 1 1 d . . . O301 O 0.4512(5) 0.2763(2) 0.6635(2) 0.0677(11) Uani 1 1 d . . . C302 C 0.1141(8) 0.2157(3) 0.5313(3) 0.0646(16) Uani 1 1 d . . . O302 O 0.1345(8) 0.2069(3) 0.4747(2) 0.116(2) Uani 1 1 d . . . C303 C 0.0040(7) 0.3262(3) 0.6362(3) 0.0606(14) Uiso 1 1 d . . . O303 O -0.0386(6) 0.3887(3) 0.6411(2) 0.0917(14) Uiso 1 1 d . . . C304 C -0.1481(7) 0.1854(3) 0.6284(2) 0.0474(12) Uani 1 1 d . . . O304 O -0.2860(5) 0.1641(2) 0.6271(2) 0.0670(11) Uani 1 1 d . . . O1 O 0.1375(5) 0.03561(18) 0.93885(16) 0.0496(9) Uani 1 1 d . . . C1 C 0.4070(6) 0.0751(2) 0.7886(2) 0.0349(10) Uani 1 1 d . . . C2 C 0.5734(7) 0.0524(2) 0.7688(3) 0.0474(11) Uani 1 1 d . . . H2 H 0.6233 0.0739 0.7303 0.057 Uiso 1 1 calc R . . C3 C 0.6630(8) -0.0003(3) 0.8049(3) 0.0590(14) Uani 1 1 d . . . H3 H 0.7729 -0.0142 0.7907 0.071 Uiso 1 1 calc R . . C4 C 0.5922(8) -0.0331(3) 0.8622(3) 0.0560(13) Uani 1 1 d . . . H4 H 0.6529 -0.0697 0.8863 0.067 Uiso 1 1 calc R . . C5 C 0.4324(7) -0.0112(2) 0.8831(2) 0.0478(12) Uani 1 1 d . . . H5 H 0.3851 -0.0335 0.9219 0.057 Uiso 1 1 calc R . . C6 C 0.3373(6) 0.0436(2) 0.8483(2) 0.0374(11) Uani 1 1 d . . . C7 C 0.1773(6) 0.0698(2) 0.8793(2) 0.0350(10) Uani 1 1 d . . . C8 C -0.0290(6) 0.0648(3) 0.9605(2) 0.0467(13) Uani 1 1 d . . . H8 H -0.1192 0.0264 0.9562 0.056 Uiso 1 1 calc R . . C9 C -0.0609(6) 0.1309(2) 0.9119(2) 0.0399(11) Uani 1 1 d . . . H9 H -0.1764 0.1284 0.8918 0.048 Uiso 1 1 calc R . . C10 C -0.0405(6) 0.2002(3) 0.9565(2) 0.0429(12) Uani 1 1 d . . . C11 C -0.0143(6) 0.1783(3) 1.0239(3) 0.0534(13) Uani 1 1 d . . . C12 C -0.0193(8) 0.0951(3) 1.0330(3) 0.0640(16) Uani 1 1 d . . . H12A H -0.1196 0.0800 1.0592 0.077 Uiso 1 1 calc R . . H12B H 0.0837 0.0772 1.0559 0.077 Uiso 1 1 calc R . . C13 C -0.0496(7) 0.2758(3) 0.9391(3) 0.0582(14) Uani 1 1 d . . . H13 H -0.0688 0.2906 0.8942 0.070 Uiso 1 1 calc R . . C14 C -0.0293(8) 0.3290(4) 0.9904(4) 0.0754(19) Uani 1 1 d . . . H14 H -0.0362 0.3801 0.9798 0.090 Uiso 1 1 calc R . . C15 C 0.0008(8) 0.3074(5) 1.0562(4) 0.080(2) Uani 1 1 d . . . H15 H 0.0173 0.3442 1.0894 0.097 Uiso 1 1 calc R . . C16 C 0.0071(7) 0.2333(5) 1.0742(3) 0.0722(19) Uani 1 1 d . . . H16 H 0.0255 0.2195 1.1195 0.087 Uiso 1 1 calc R . . H100 H 0.002(5) 0.098(2) 0.729(2) 0.034(11) Uiso 1 1 d . . . H1 H 0.386(5) 0.151(2) 0.729(2) 0.048(12) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.03787(19) 0.02958(18) 0.03057(18) 0.00099(15) -0.00105(17) 0.00287(17) Ru2 0.0458(2) 0.0352(2) 0.03402(19) -0.00405(17) -0.00133(18) 0.00035(18) Ru3 0.0430(2) 0.0426(2) 0.03513(19) 0.00958(17) -0.00072(19) 0.0020(2) N1 0.037(2) 0.033(2) 0.038(2) 0.0053(18) 0.0008(19) -0.0025(19) N2 0.042(2) 0.0342(19) 0.0309(19) 0.0018(15) 0.0024(18) 0.000(2) C101 0.047(3) 0.048(3) 0.049(3) 0.004(2) 0.000(3) 0.001(3) O101 0.091(3) 0.042(2) 0.088(3) -0.009(2) -0.001(2) -0.013(2) C102 0.050(3) 0.041(3) 0.030(2) 0.003(2) -0.003(2) 0.001(2) O102 0.040(2) 0.072(3) 0.061(2) -0.005(2) 0.0006(18) 0.0161(19) C201 0.082(4) 0.037(3) 0.049(3) -0.009(2) -0.006(3) 0.005(3) O201 0.151(5) 0.034(2) 0.118(4) 0.003(2) -0.018(3) 0.005(3) C202 0.057(3) 0.056(3) 0.045(3) -0.020(3) -0.005(3) 0.001(3) O202 0.070(3) 0.097(3) 0.063(2) -0.027(2) 0.023(2) -0.011(3) C203 0.063(4) 0.057(3) 0.048(3) -0.015(3) -0.002(3) -0.006(3) O203 0.083(3) 0.100(3) 0.093(3) -0.040(3) -0.036(3) 0.002(3) C301 0.056(4) 0.041(3) 0.047(3) 0.014(2) 0.008(3) 0.007(3) O301 0.044(2) 0.069(2) 0.090(3) 0.019(2) -0.004(2) -0.004(2) C302 0.076(4) 0.075(4) 0.043(3) 0.016(3) -0.003(3) 0.003(3) O302 0.146(5) 0.161(5) 0.040(3) 0.010(3) 0.003(3) -0.007(4) C304 0.048(3) 0.053(3) 0.041(3) 0.007(2) -0.006(2) 0.005(3) O304 0.046(2) 0.084(3) 0.071(3) 0.005(2) -0.013(2) -0.008(2) O1 0.064(3) 0.0423(18) 0.0422(19) 0.0110(16) 0.0038(17) -0.0044(17) C1 0.041(2) 0.025(2) 0.039(2) -0.0030(19) -0.007(2) 0.000(2) C2 0.043(3) 0.045(3) 0.054(3) 0.004(2) 0.001(3) 0.002(2) C3 0.046(3) 0.055(3) 0.076(4) -0.002(3) -0.005(3) 0.013(3) C4 0.059(3) 0.040(3) 0.069(3) 0.005(3) -0.011(3) 0.012(3) C5 0.061(3) 0.035(2) 0.048(3) 0.007(2) -0.004(3) -0.001(3) C6 0.049(3) 0.024(2) 0.040(3) 0.0033(18) -0.009(2) -0.001(2) C7 0.048(3) 0.029(2) 0.028(2) 0.001(2) -0.003(2) -0.007(2) C8 0.050(3) 0.051(3) 0.039(3) 0.003(2) 0.000(2) -0.015(2) C9 0.036(3) 0.050(3) 0.034(2) -0.003(2) 0.004(2) -0.004(2) C10 0.034(3) 0.055(3) 0.040(3) -0.011(2) 0.007(2) -0.007(2) C11 0.037(3) 0.074(4) 0.049(3) -0.018(3) 0.003(2) -0.003(3) C12 0.072(4) 0.080(4) 0.039(3) 0.003(3) 0.007(3) -0.004(3) C13 0.055(4) 0.051(3) 0.069(4) -0.013(3) 0.014(3) 0.000(3) C14 0.060(4) 0.059(4) 0.107(6) -0.032(4) 0.020(4) 0.002(3) C15 0.046(3) 0.101(6) 0.095(6) -0.061(5) 0.002(4) 0.010(4) C16 0.047(3) 0.118(6) 0.052(3) -0.038(4) -0.001(3) 0.012(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 C101 1.855(6) . ? Ru1 C102 1.864(5) . ? Ru1 N1 2.120(4) . ? Ru1 N2 2.123(3) . ? Ru1 Ru2 2.7819(9) . ? Ru1 Ru3 2.7950(12) . ? Ru1 H100 1.74(4) . ? Ru2 C203 1.882(6) . ? Ru2 C202 1.918(6) . ? Ru2 C201 1.943(6) . ? Ru2 N1 2.169(4) . ? Ru2 Ru3 2.8238(12) . ? Ru2 H100 1.83(4) . ? Ru3 C303 1.885(6) . ? Ru3 C302 1.920(6) . ? Ru3 C304 1.930(6) . ? Ru3 C301 1.947(6) . ? N1 C1 1.414(6) . ? N1 H1 0.75(4) . ? N2 C7 1.277(6) . ? N2 C9 1.484(6) . ? C101 O101 1.151(6) . ? C102 O102 1.145(6) . ? C201 O201 1.108(6) . ? C202 O202 1.133(6) . ? C203 O203 1.137(6) . ? C301 O301 1.127(6) . ? C302 O302 1.131(7) . ? C303 O303 1.158(7) . ? C304 O304 1.135(6) . ? O1 C7 1.349(5) . ? O1 C8 1.455(6) . ? C1 C6 1.405(6) . ? C1 C2 1.406(7) . ? C2 C3 1.361(7) . ? C2 H2 0.9300 . ? C3 C4 1.378(8) . ? C3 H3 0.9300 . ? C4 C5 1.362(8) . ? C4 H4 0.9300 . ? C5 C6 1.397(6) . ? C5 H5 0.9300 . ? C6 C7 1.458(7) . ? C8 C12 1.518(7) . ? C8 C9 1.529(6) . ? C8 H8 0.9800 . ? C9 C10 1.515(6) . ? C9 H9 0.9800 . ? C10 C13 1.383(7) . ? C10 C11 1.389(7) . ? C11 C16 1.396(8) . ? C11 C12 1.485(8) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 C14 1.385(8) . ? C13 H13 0.9300 . ? C14 C15 1.364(10) . ? C14 H14 0.9300 . ? C15 C16 1.359(10) . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? 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 C101 Ru1 C102 90.4(2) . . ? C101 Ru1 N1 99.3(2) . . ? C102 Ru1 N1 169.47(17) . . ? C101 Ru1 N2 101.64(17) . . ? C102 Ru1 N2 95.23(18) . . ? N1 Ru1 N2 86.88(15) . . ? C101 Ru1 Ru2 136.16(16) . . ? C102 Ru1 Ru2 119.35(14) . . ? N1 Ru1 Ru2 50.34(10) . . ? N2 Ru1 Ru2 106.35(10) . . ? C101 Ru1 Ru3 91.34(15) . . ? C102 Ru1 Ru3 88.36(14) . . ? N1 Ru1 Ru3 87.32(10) . . ? N2 Ru1 Ru3 166.48(9) . . ? Ru2 Ru1 Ru3 60.84(1) . . ? C101 Ru1 H100 173.0(13) . . ? C102 Ru1 H100 88.6(13) . . ? N1 Ru1 H100 81.3(13) . . ? N2 Ru1 H100 85.3(13) . . ? Ru2 Ru1 H100 40.1(13) . . ? Ru3 Ru1 H100 81.7(13) . . ? C203 Ru2 C202 90.9(2) . . ? C203 Ru2 C201 91.8(2) . . ? C202 Ru2 C201 99.8(2) . . ? C203 Ru2 N1 169.5(2) . . ? C202 Ru2 N1 96.86(19) . . ? C201 Ru2 N1 93.81(19) . . ? C203 Ru2 Ru1 120.71(17) . . ? C202 Ru2 Ru1 129.03(15) . . ? C201 Ru2 Ru1 116.26(16) . . ? N1 Ru2 Ru1 48.80(11) . . ? C203 Ru2 Ru3 87.98(18) . . ? C202 Ru2 Ru3 85.26(16) . . ? C201 Ru2 Ru3 174.90(17) . . ? N1 Ru2 Ru3 85.66(10) . . ? Ru1 Ru2 Ru3 59.81(1) . . ? C203 Ru2 H100 92.7(12) . . ? C202 Ru2 H100 164.1(12) . . ? C201 Ru2 H100 95.5(12) . . ? N1 Ru2 H100 77.9(12) . . ? Ru1 Ru2 H100 37.6(12) . . ? Ru3 Ru2 H100 79.4(12) . . ? C303 Ru3 C302 102.2(2) . . ? C303 Ru3 C304 92.7(2) . . ? C302 Ru3 C304 94.8(2) . . ? C303 Ru3 C301 92.0(2) . . ? C302 Ru3 C301 97.0(2) . . ? C304 Ru3 C301 166.01(19) . . ? C303 Ru3 Ru1 100.60(17) . . ? C302 Ru3 Ru1 157.15(18) . . ? C304 Ru3 Ru1 83.53(14) . . ? C301 Ru3 Ru1 82.66(14) . . ? C303 Ru3 Ru2 159.65(17) . . ? C302 Ru3 Ru2 97.82(17) . . ? C304 Ru3 Ru2 82.11(15) . . ? C301 Ru3 Ru2 88.95(14) . . ? Ru1 Ru3 Ru2 59.352(12) . . ? C1 N1 Ru1 127.7(3) . . ? C1 N1 Ru2 115.4(3) . . ? Ru1 N1 Ru2 80.86(14) . . ? C1 N1 H1 107(3) . . ? Ru1 N1 H1 115(3) . . ? Ru2 N1 H1 107(3) . . ? C7 N2 C9 107.7(3) . . ? C7 N2 Ru1 127.8(3) . . ? C9 N2 Ru1 124.4(3) . . ? O101 C101 Ru1 176.3(5) . . ? O102 C102 Ru1 178.0(4) . . ? O201 C201 Ru2 173.7(5) . . ? O202 C202 Ru2 178.1(5) . . ? O203 C203 Ru2 178.2(5) . . ? O301 C301 Ru3 176.1(5) . . ? O302 C302 Ru3 177.4(6) . . ? O303 C303 Ru3 177.6(5) . . ? O304 C304 Ru3 177.3(5) . . ? C7 O1 C8 107.2(4) . . ? C6 C1 C2 118.0(4) . . ? C6 C1 N1 124.2(4) . . ? C2 C1 N1 117.8(4) . . ? C3 C2 C1 121.5(5) . . ? C3 C2 H2 119.2 . . ? C1 C2 H2 119.2 . . ? C2 C3 C4 120.5(6) . . ? C2 C3 H3 119.8 . . ? C4 C3 H3 119.8 . . ? C5 C4 C3 119.2(5) . . ? C5 C4 H4 120.4 . . ? C3 C4 H4 120.4 . . ? C4 C5 C6 122.1(5) . . ? C4 C5 H5 119.0 . . ? C6 C5 H5 119.0 . . ? C5 C6 C1 118.6(5) . . ? C5 C6 C7 117.9(4) . . ? C1 C6 C7 123.3(4) . . ? N2 C7 O1 116.6(4) . . ? N2 C7 C6 129.0(4) . . ? O1 C7 C6 114.3(4) . . ? O1 C8 C12 110.7(4) . . ? O1 C8 C9 103.5(4) . . ? C12 C8 C9 108.7(4) . . ? O1 C8 H8 111.2 . . ? C12 C8 H8 111.2 . . ? C9 C8 H8 111.2 . . ? N2 C9 C10 114.7(4) . . ? N2 C9 C8 103.6(4) . . ? C10 C9 C8 104.1(4) . . ? N2 C9 H9 111.3 . . ? C10 C9 H9 111.3 . . ? C8 C9 H9 111.3 . . ? C13 C10 C11 120.7(5) . . ? C13 C10 C9 129.5(5) . . ? C11 C10 C9 109.7(4) . . ? C10 C11 C16 119.6(6) . . ? C10 C11 C12 112.7(5) . . ? C16 C11 C12 127.6(6) . . ? C11 C12 C8 103.8(4) . . ? C11 C12 H12A 111.0 . . ? C8 C12 H12A 111.0 . . ? C11 C12 H12B 111.0 . . ? C8 C12 H12B 111.0 . . ? H12A C12 H12B 109.0 . . ? C10 C13 C14 118.3(6) . . ? C10 C13 H13 120.9 . . ? C14 C13 H13 120.9 . . ? C15 C14 C13 120.9(7) . . ? C15 C14 H14 119.5 . . ? C13 C14 H14 119.5 . . ? C16 C15 C14 121.4(6) . . ? C16 C15 H15 119.3 . . ? C14 C15 H15 119.3 . . ? C15 C16 C11 119.0(6) . . ? C15 C16 H16 120.5 . . ? C11 C16 H16 120.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C101 Ru1 Ru2 C203 -124.0(3) . . . . ? C102 Ru1 Ru2 C203 2.6(3) . . . . ? N1 Ru1 Ru2 C203 180.0(2) . . . . ? N2 Ru1 Ru2 C203 108.5(2) . . . . ? Ru3 Ru1 Ru2 C203 -66.9(2) . . . . ? C101 Ru1 Ru2 C202 -3.7(3) . . . . ? C102 Ru1 Ru2 C202 122.9(3) . . . . ? N1 Ru1 Ru2 C202 -59.6(3) . . . . ? N2 Ru1 Ru2 C202 -131.2(2) . . . . ? Ru3 Ru1 Ru2 C202 53.5(2) . . . . ? C101 Ru1 Ru2 C201 126.5(3) . . . . ? C102 Ru1 Ru2 C201 -106.9(3) . . . . ? N1 Ru1 Ru2 C201 70.5(2) . . . . ? N2 Ru1 Ru2 C201 -1.0(2) . . . . ? Ru3 Ru1 Ru2 C201 -176.3(2) . . . . ? C101 Ru1 Ru2 N1 56.0(3) . . . . ? C102 Ru1 Ru2 N1 -177.4(2) . . . . ? N2 Ru1 Ru2 N1 -71.53(18) . . . . ? Ru3 Ru1 Ru2 N1 113.15(14) . . . . ? C101 Ru1 Ru2 Ru3 -57.2(2) . . . . ? C102 Ru1 Ru2 Ru3 69.43(16) . . . . ? N1 Ru1 Ru2 Ru3 -113.15(14) . . . . ? N2 Ru1 Ru2 Ru3 175.32(11) . . . . ? C101 Ru1 Ru3 C303 -39.4(2) . . . . ? C102 Ru1 Ru3 C303 51.0(2) . . . . ? N1 Ru1 Ru3 C303 -138.6(2) . . . . ? N2 Ru1 Ru3 C303 156.7(5) . . . . ? Ru2 Ru1 Ru3 C303 176.23(18) . . . . ? C101 Ru1 Ru3 C302 141.9(5) . . . . ? C102 Ru1 Ru3 C302 -127.7(5) . . . . ? N1 Ru1 Ru3 C302 42.7(5) . . . . ? N2 Ru1 Ru3 C302 -22.0(7) . . . . ? Ru2 Ru1 Ru3 C302 -2.5(5) . . . . ? C101 Ru1 Ru3 C304 -131.0(2) . . . . ? C102 Ru1 Ru3 C304 -40.6(2) . . . . ? N1 Ru1 Ru3 C304 129.76(19) . . . . ? N2 Ru1 Ru3 C304 65.1(5) . . . . ? Ru2 Ru1 Ru3 C304 84.64(16) . . . . ? C101 Ru1 Ru3 C301 51.3(2) . . . . ? C102 Ru1 Ru3 C301 141.6(2) . . . . ? N1 Ru1 Ru3 C301 -48.02(18) . . . . ? N2 Ru1 Ru3 C301 -112.7(5) . . . . ? Ru2 Ru1 Ru3 C301 -93.14(15) . . . . ? C101 Ru1 Ru3 Ru2 144.40(17) . . . . ? C102 Ru1 Ru3 Ru2 -125.27(14) . . . . ? N1 Ru1 Ru3 Ru2 45.12(11) . . . . ? N2 Ru1 Ru3 Ru2 -19.6(5) . . . . ? C203 Ru2 Ru3 C303 117.0(5) . . . . ? C202 Ru2 Ru3 C303 -151.9(5) . . . . ? N1 Ru2 Ru3 C303 -54.6(5) . . . . ? Ru1 Ru2 Ru3 C303 -10.7(5) . . . . ? C203 Ru2 Ru3 C302 -53.3(3) . . . . ? C202 Ru2 Ru3 C302 37.8(2) . . . . ? N1 Ru2 Ru3 C302 135.1(2) . . . . ? Ru1 Ru2 Ru3 C302 179.04(19) . . . . ? C203 Ru2 Ru3 C304 40.6(2) . . . . ? C202 Ru2 Ru3 C304 131.7(2) . . . . ? N1 Ru2 Ru3 C304 -131.06(19) . . . . ? Ru1 Ru2 Ru3 C304 -87.13(15) . . . . ? C203 Ru2 Ru3 C301 -150.2(2) . . . . ? C202 Ru2 Ru3 C301 -59.1(2) . . . . ? N1 Ru2 Ru3 C301 38.16(19) . . . . ? Ru1 Ru2 Ru3 C301 82.09(15) . . . . ? C203 Ru2 Ru3 Ru1 127.71(17) . . . . ? C202 Ru2 Ru3 Ru1 -141.20(15) . . . . ? N1 Ru2 Ru3 Ru1 -43.93(12) . . . . ? C101 Ru1 N1 C1 100.4(4) . . . . ? C102 Ru1 N1 C1 -102.8(10) . . . . ? N2 Ru1 N1 C1 -0.9(4) . . . . ? Ru2 Ru1 N1 C1 -115.2(4) . . . . ? Ru3 Ru1 N1 C1 -168.7(3) . . . . ? C101 Ru1 N1 Ru2 -144.42(17) . . . . ? C102 Ru1 N1 Ru2 12.4(10) . . . . ? N2 Ru1 N1 Ru2 114.29(14) . . . . ? Ru3 Ru1 N1 Ru2 -53.50(9) . . . . ? C203 Ru2 N1 C1 127.5(11) . . . . ? C202 Ru2 N1 C1 -94.9(4) . . . . ? C201 Ru2 N1 C1 5.5(4) . . . . ? Ru1 Ru2 N1 C1 127.5(4) . . . . ? Ru3 Ru2 N1 C1 -179.6(3) . . . . ? C203 Ru2 N1 Ru1 -0.1(12) . . . . ? C202 Ru2 N1 Ru1 137.53(19) . . . . ? C201 Ru2 N1 Ru1 -122.1(2) . . . . ? Ru3 Ru2 N1 Ru1 52.85(9) . . . . ? C101 Ru1 N2 C7 -106.1(4) . . . . ? C102 Ru1 N2 C7 162.4(4) . . . . ? N1 Ru1 N2 C7 -7.2(4) . . . . ? Ru2 Ru1 N2 C7 39.8(4) . . . . ? Ru3 Ru1 N2 C7 57.5(7) . . . . ? C101 Ru1 N2 C9 77.7(4) . . . . ? C102 Ru1 N2 C9 -13.8(4) . . . . ? N1 Ru1 N2 C9 176.6(3) . . . . ? Ru2 Ru1 N2 C9 -136.5(3) . . . . ? Ru3 Ru1 N2 C9 -118.7(4) . . . . ? Ru1 N1 C1 C6 9.0(6) . . . . ? Ru2 N1 C1 C6 -89.4(4) . . . . ? Ru1 N1 C1 C2 -172.8(3) . . . . ? Ru2 N1 C1 C2 88.9(4) . . . . ? C6 C1 C2 C3 2.2(7) . . . . ? N1 C1 C2 C3 -176.1(4) . . . . ? C1 C2 C3 C4 0.0(8) . . . . ? C2 C3 C4 C5 -1.1(8) . . . . ? C3 C4 C5 C6 0.0(8) . . . . ? C4 C5 C6 C1 2.3(7) . . . . ? C4 C5 C6 C7 -172.6(4) . . . . ? C2 C1 C6 C5 -3.3(6) . . . . ? N1 C1 C6 C5 175.0(4) . . . . ? C2 C1 C6 C7 171.3(4) . . . . ? N1 C1 C6 C7 -10.5(7) . . . . ? C9 N2 C7 O1 2.5(5) . . . . ? Ru1 N2 C7 O1 -174.3(3) . . . . ? C9 N2 C7 C6 -175.0(4) . . . . ? Ru1 N2 C7 C6 8.3(7) . . . . ? C8 O1 C7 N2 5.4(5) . . . . ? C8 O1 C7 C6 -176.7(4) . . . . ? C5 C6 C7 N2 176.1(4) . . . . ? C1 C6 C7 N2 1.5(7) . . . . ? C5 C6 C7 O1 -1.4(6) . . . . ? C1 C6 C7 O1 -176.1(4) . . . . ? C7 O1 C8 C12 -126.6(4) . . . . ? C7 O1 C8 C9 -10.3(4) . . . . ? C7 N2 C9 C10 104.0(5) . . . . ? Ru1 N2 C9 C10 -79.1(5) . . . . ? C7 N2 C9 C8 -8.7(5) . . . . ? Ru1 N2 C9 C8 168.1(3) . . . . ? O1 C8 C9 N2 11.3(4) . . . . ? C12 C8 C9 N2 129.0(4) . . . . ? O1 C8 C9 C10 -109.0(4) . . . . ? C12 C8 C9 C10 8.8(5) . . . . ? N2 C9 C10 C13 65.2(7) . . . . ? C8 C9 C10 C13 177.6(5) . . . . ? N2 C9 C10 C11 -116.8(4) . . . . ? C8 C9 C10 C11 -4.4(5) . . . . ? C13 C10 C11 C16 -1.5(8) . . . . ? C9 C10 C11 C16 -179.8(5) . . . . ? C13 C10 C11 C12 176.4(5) . . . . ? C9 C10 C11 C12 -1.8(6) . . . . ? C10 C11 C12 C8 7.2(6) . . . . ? C16 C11 C12 C8 -175.1(5) . . . . ? O1 C8 C12 C11 103.4(5) . . . . ? C9 C8 C12 C11 -9.7(6) . . . . ? C11 C10 C13 C14 0.9(8) . . . . ? C9 C10 C13 C14 178.8(5) . . . . ? C10 C13 C14 C15 0.7(9) . . . . ? C13 C14 C15 C16 -1.9(10) . . . . ? C14 C15 C16 C11 1.3(10) . . . . ? C10 C11 C16 C15 0.4(8) . . . . ? C12 C11 C16 C15 -177.2(6) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 23.25 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.488 _refine_diff_density_min -0.352 _refine_diff_density_rms 0.062 #===END