Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Javier Cabeza' 'del Rio, Ignacio' 'D. Miguel' 'Enrique Perez-Carreno' 'M. Gabriela Sanchez-Vega' _publ_contact_author_name 'Javier A. Cabeza' _publ_contact_author_address ; Quimica Organica e Inorganica Universidad de Oviedo-CSIC Facultad de Quimica Oviedo 33071 SPAIN ; _publ_contact_author_email JAC@UNIOVI.ES _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Activation of two C-H bonds of NHC N-methyl groups on triosmium and triruthenium carbonyl clusters ; #-------------------------- data section of block --------------------------- data_4b_g64f4am _database_code_depnum_ccdc_archive 'CCDC 676043' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H8 N2 O15 Ru5' _chemical_formula_sum 'C20 H8 N2 O15 Ru5' _chemical_formula_weight 1021.63 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/c' _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 11.474(3) _cell_length_b 16.127(4) _cell_length_c 15.209(3) _cell_angle_alpha 90.00 _cell_angle_beta 96.326(4) _cell_angle_gamma 90.00 _cell_volume 2796.9(10) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 3400 _cell_measurement_theta_min 1.90 _cell_measurement_theta_max 23.52 _exptl_crystal_description BLOCK _exptl_crystal_colour BLACK _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.426 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1928 _exptl_absorpt_coefficient_mu 2.712 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.495 _exptl_absorpt_correction_T_max 0.580 _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 12031 _diffrn_reflns_av_R_equivalents 0.0216 _diffrn_reflns_av_sigmaI/netI 0.0169 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.79 _diffrn_reflns_theta_max 23.29 _reflns_number_total 4010 _reflns_number_gt 3620 _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^)+(0.0190P)^2^+5.3441P] 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 SHELXL _refine_ls_extinction_coef 0.00049(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4010 _refine_ls_number_parameters 382 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0265 _refine_ls_R_factor_gt 0.0221 _refine_ls_wR_factor_ref 0.0522 _refine_ls_wR_factor_gt 0.0491 _refine_ls_goodness_of_fit_ref 1.110 _refine_ls_restrained_S_all 1.110 _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 0.90837(3) 0.94367(2) 0.27604(2) 0.03134(10) Uani 1 1 d . . . Ru2 Ru 0.67185(3) 0.98440(2) 0.20438(2) 0.02942(10) Uani 1 1 d . . . Ru3 Ru 0.76461(3) 1.05652(2) 0.36169(2) 0.02962(10) Uani 1 1 d . . . Ru4 Ru 0.52640(3) 1.07956(2) 0.30012(2) 0.03799(11) Uani 1 1 d . . . Ru5 Ru 0.69706(3) 1.15888(2) 0.21489(2) 0.03394(10) Uani 1 1 d . . . N1 N 1.0607(3) 0.9091(2) 0.1276(3) 0.0498(10) Uani 1 1 d . . . N2 N 0.9439(3) 0.8066(2) 0.1365(3) 0.0478(10) Uani 1 1 d . . . C100 C 0.8195(4) 1.0694(2) 0.2299(3) 0.0336(9) Uani 1 1 d . . . O100 O 0.9209(2) 1.05836(17) 0.20913(19) 0.0366(7) Uani 1 1 d . . . C101 C 1.0579(4) 0.9429(3) 0.3368(3) 0.0418(11) Uani 1 1 d . . . O101 O 1.1489(3) 0.9423(3) 0.3752(3) 0.0694(11) Uani 1 1 d . . . C102 C 0.8729(4) 0.8504(3) 0.3407(3) 0.0408(11) Uani 1 1 d . . . O102 O 0.8536(3) 0.7948(2) 0.3830(3) 0.0643(10) Uani 1 1 d . . . C201 C 0.7367(4) 0.9445(3) 0.1008(3) 0.0460(11) Uani 1 1 d . . . O201 O 0.7650(4) 0.9228(3) 0.0359(2) 0.0802(13) Uani 1 1 d . . . C202 C 0.6312(4) 0.8825(3) 0.2540(3) 0.0422(11) Uani 1 1 d . . . O202 O 0.6047(3) 0.8206(2) 0.2830(3) 0.0674(11) Uani 1 1 d . . . C203 C 0.5198(4) 0.9922(3) 0.1386(3) 0.0421(11) Uani 1 1 d . . . O203 O 0.4372(3) 0.9862(2) 0.0901(2) 0.0613(10) Uani 1 1 d . . . C301 C 0.9220(4) 1.0694(3) 0.4128(3) 0.0400(10) Uani 1 1 d . . . O301 O 1.0103(3) 1.0861(2) 0.4520(2) 0.0552(9) Uani 1 1 d . . . C302 C 0.7170(4) 1.1437(3) 0.4347(3) 0.0460(11) Uani 1 1 d . . . O302 O 0.7047(3) 1.1948(2) 0.4840(2) 0.0658(10) Uani 1 1 d . . . C303 C 0.7258(4) 0.9712(3) 0.4406(3) 0.0435(11) Uani 1 1 d . . . O303 O 0.7037(4) 0.9211(2) 0.4881(3) 0.0699(11) Uani 1 1 d . . . C401 C 0.3897(4) 1.1073(3) 0.2266(3) 0.0490(12) Uani 1 1 d . . . O401 O 0.3055(3) 1.1258(3) 0.1852(3) 0.0779(12) Uani 1 1 d . . . C402 C 0.4774(4) 1.1615(3) 0.3760(4) 0.0548(13) Uani 1 1 d . . . O402 O 0.4399(4) 1.2101(3) 0.4185(3) 0.0860(14) Uani 1 1 d . . . C403 C 0.4637(4) 0.9881(3) 0.3588(4) 0.0570(14) Uani 1 1 d . . . O403 O 0.4254(4) 0.9342(3) 0.3943(4) 0.0943(15) Uani 1 1 d . . . C501 C 0.6599(4) 1.2557(3) 0.2803(4) 0.0538(13) Uani 1 1 d . . . O501 O 0.6447(4) 1.3146(2) 0.3182(3) 0.0831(13) Uani 1 1 d . . . C502 C 0.5779(5) 1.1733(3) 0.1180(4) 0.0631(15) Uani 1 1 d . . . O502 O 0.5097(4) 1.1804(3) 0.0589(3) 0.1084(19) Uani 1 1 d . . . C503 C 0.8164(4) 1.2155(3) 0.1614(3) 0.0440(11) Uani 1 1 d . . . O503 O 0.8891(3) 1.2496(2) 0.1315(3) 0.0680(10) Uani 1 1 d . . . C1 C 0.9759(4) 0.8801(3) 0.1747(3) 0.0382(10) Uani 1 1 d . . . C2 C 1.0069(5) 0.7919(4) 0.0654(4) 0.0664(16) Uani 1 1 d . . . H2 H 1.0000 0.7460 0.0283 0.080 Uiso 1 1 calc R . . C3 C 1.0790(5) 0.8556(4) 0.0603(4) 0.0706(16) Uani 1 1 d . . . H3 H 1.1321 0.8626 0.0189 0.085 Uiso 1 1 calc R . . C4 C 0.8558(5) 0.7499(3) 0.1621(4) 0.0721(17) Uani 1 1 d . . . H4A H 0.8874 0.7190 0.2132 0.108 Uiso 1 1 calc R . . H4B H 0.8332 0.7124 0.1143 0.108 Uiso 1 1 calc R . . H4C H 0.7886 0.7807 0.1758 0.108 Uiso 1 1 calc R . . C5 C 1.1312(5) 0.9840(3) 0.1435(4) 0.0713(17) Uani 1 1 d . . . H5A H 1.0871 1.0311 0.1199 0.107 Uiso 1 1 calc R . . H5B H 1.2015 0.9790 0.1151 0.107 Uiso 1 1 calc R . . H5C H 1.1513 0.9912 0.2060 0.107 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.02469(18) 0.03292(19) 0.03615(19) 0.00113(14) 0.00218(14) 0.00292(14) Ru2 0.02524(18) 0.03247(19) 0.02987(18) -0.00084(14) -0.00005(13) -0.00132(14) Ru3 0.02602(18) 0.03473(19) 0.02772(18) -0.00090(13) 0.00112(13) 0.00038(14) Ru4 0.02450(18) 0.0421(2) 0.0481(2) -0.00064(16) 0.00746(15) 0.00130(15) Ru5 0.02927(19) 0.03107(19) 0.0407(2) 0.00616(14) 0.00026(15) 0.00052(14) N1 0.047(2) 0.052(2) 0.053(2) -0.0102(19) 0.018(2) -0.004(2) N2 0.043(2) 0.042(2) 0.058(3) -0.0107(19) 0.0035(19) -0.0010(18) C100 0.032(2) 0.031(2) 0.037(2) 0.0053(18) 0.0016(19) -0.0016(18) O100 0.0281(16) 0.0376(16) 0.0456(17) 0.0044(13) 0.0101(13) -0.0003(13) C101 0.039(3) 0.041(3) 0.045(3) -0.004(2) 0.003(2) 0.007(2) O101 0.040(2) 0.090(3) 0.074(3) -0.006(2) -0.0150(19) 0.0096(19) C102 0.027(2) 0.045(3) 0.051(3) 0.005(2) 0.005(2) 0.006(2) O102 0.058(2) 0.057(2) 0.078(3) 0.032(2) 0.0071(19) -0.0001(18) C201 0.035(2) 0.060(3) 0.042(3) 0.001(2) -0.002(2) 0.006(2) O201 0.078(3) 0.127(4) 0.036(2) -0.014(2) 0.0086(19) 0.037(3) C202 0.027(2) 0.050(3) 0.048(3) -0.005(2) -0.005(2) 0.000(2) O202 0.056(2) 0.047(2) 0.097(3) 0.023(2) -0.001(2) -0.0149(18) C203 0.034(3) 0.045(3) 0.048(3) 0.000(2) 0.003(2) 0.000(2) O203 0.0389(19) 0.081(3) 0.059(2) -0.0086(19) -0.0168(18) 0.0047(18) C301 0.040(3) 0.040(2) 0.040(2) 0.0030(19) 0.001(2) 0.000(2) O301 0.042(2) 0.054(2) 0.065(2) -0.0064(17) -0.0141(18) -0.0007(16) C302 0.038(3) 0.053(3) 0.046(3) -0.009(2) 0.000(2) 0.007(2) O302 0.064(2) 0.071(2) 0.060(2) -0.029(2) -0.0046(18) 0.011(2) C303 0.038(3) 0.050(3) 0.043(3) 0.000(2) 0.006(2) -0.003(2) O303 0.078(3) 0.071(3) 0.064(2) 0.023(2) 0.024(2) -0.010(2) C401 0.032(3) 0.046(3) 0.067(3) -0.013(2) 0.000(2) 0.000(2) O401 0.045(2) 0.072(3) 0.110(3) -0.011(2) -0.025(2) 0.008(2) C402 0.029(2) 0.073(4) 0.062(3) -0.019(3) 0.002(2) -0.002(2) O402 0.064(3) 0.099(3) 0.097(3) -0.052(3) 0.018(2) 0.004(2) C403 0.039(3) 0.064(3) 0.071(4) 0.011(3) 0.022(3) 0.002(3) O403 0.073(3) 0.088(3) 0.130(4) 0.038(3) 0.047(3) -0.002(2) C501 0.044(3) 0.051(3) 0.067(3) 0.008(3) 0.007(2) 0.010(2) O501 0.094(3) 0.051(2) 0.104(3) -0.023(2) 0.012(3) 0.020(2) C502 0.049(3) 0.060(3) 0.076(4) 0.031(3) -0.014(3) -0.017(3) O502 0.089(3) 0.118(4) 0.104(4) 0.061(3) -0.052(3) -0.036(3) C503 0.046(3) 0.034(2) 0.051(3) 0.007(2) 0.003(2) -0.001(2) O503 0.056(2) 0.061(2) 0.090(3) 0.016(2) 0.020(2) -0.014(2) C1 0.028(2) 0.042(3) 0.044(2) -0.004(2) 0.0007(19) 0.0021(19) C2 0.078(4) 0.062(4) 0.061(3) -0.030(3) 0.013(3) 0.005(3) C3 0.076(4) 0.069(4) 0.073(4) -0.021(3) 0.036(3) 0.000(3) C4 0.066(4) 0.050(3) 0.102(5) -0.029(3) 0.019(3) -0.019(3) C5 0.063(4) 0.064(4) 0.095(4) -0.016(3) 0.044(3) -0.024(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 C101 1.857(5) . ? Ru1 C102 1.866(5) . ? Ru1 C1 2.072(4) . ? Ru1 O100 2.123(3) . ? Ru1 C100 2.342(4) . ? Ru1 Ru3 2.8641(6) . ? Ru1 Ru2 2.8866(7) . ? Ru2 C202 1.888(5) . ? Ru2 C203 1.917(5) . ? Ru2 C201 1.925(5) . ? Ru2 C100 2.181(4) . ? Ru2 Ru3 2.7655(6) . ? Ru2 Ru4 2.7920(6) . ? Ru2 Ru5 2.8314(7) . ? Ru3 C301 1.897(5) . ? Ru3 C302 1.908(5) . ? Ru3 C303 1.911(5) . ? Ru3 C100 2.176(4) . ? Ru3 Ru4 2.8145(7) . ? Ru3 Ru5 2.8159(6) . ? Ru4 C401 1.877(5) . ? Ru4 C402 1.881(5) . ? Ru4 C403 1.906(5) . ? Ru4 Ru5 2.7768(6) . ? Ru5 C503 1.902(5) . ? Ru5 C502 1.911(5) . ? Ru5 C501 1.925(6) . ? Ru5 C100 2.010(4) . ? N1 C1 1.353(6) . ? N1 C3 1.372(6) . ? N1 C5 1.459(6) . ? N2 C1 1.353(6) . ? N2 C2 1.386(6) . ? N2 C4 1.447(6) . ? C100 O100 1.251(5) . ? C101 O101 1.139(5) . ? C102 O102 1.139(5) . ? C201 O201 1.129(6) . ? C202 O202 1.146(5) . ? C203 O203 1.139(5) . ? C301 O301 1.149(5) . ? C302 O302 1.134(5) . ? C303 O303 1.130(5) . ? C401 O401 1.134(6) . ? C402 O402 1.130(6) . ? C403 O403 1.137(6) . ? C501 O501 1.134(6) . ? C502 O502 1.130(6) . ? C503 O503 1.134(5) . ? C2 C3 1.326(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 C101 Ru1 C102 88.59(19) . . ? C101 Ru1 C1 88.08(18) . . ? C102 Ru1 C1 96.55(18) . . ? C101 Ru1 O100 97.88(16) . . ? C102 Ru1 O100 169.96(15) . . ? C1 Ru1 O100 91.36(14) . . ? C101 Ru1 C100 120.19(17) . . ? C102 Ru1 C100 137.97(16) . . ? C1 Ru1 C100 113.04(16) . . ? O100 Ru1 C100 32.06(12) . . ? C101 Ru1 Ru3 108.94(13) . . ? C102 Ru1 Ru3 95.91(13) . . ? C1 Ru1 Ru3 159.11(12) . . ? O100 Ru1 Ru3 74.76(8) . . ? C100 Ru1 Ru3 48.15(10) . . ? C101 Ru1 Ru2 165.47(13) . . ? C102 Ru1 Ru2 97.58(13) . . ? C1 Ru1 Ru2 104.17(12) . . ? O100 Ru1 Ru2 74.41(7) . . ? C100 Ru1 Ru2 47.91(10) . . ? Ru3 Ru1 Ru2 57.487(15) . . ? C202 Ru2 C203 90.84(18) . . ? C202 Ru2 C201 99.9(2) . . ? C203 Ru2 C201 90.35(19) . . ? C202 Ru2 C100 134.21(16) . . ? C203 Ru2 C100 134.13(17) . . ? C201 Ru2 C100 89.58(18) . . ? C202 Ru2 Ru3 96.23(13) . . ? C203 Ru2 Ru3 131.70(14) . . ? C201 Ru2 Ru3 134.57(14) . . ? C100 Ru2 Ru3 50.53(11) . . ? C202 Ru2 Ru4 94.67(14) . . ? C203 Ru2 Ru4 71.00(14) . . ? C201 Ru2 Ru4 156.52(14) . . ? C100 Ru2 Ru4 93.40(11) . . ? Ru3 Ru2 Ru4 60.849(17) . . ? C202 Ru2 Ru5 150.51(14) . . ? C203 Ru2 Ru5 92.63(14) . . ? C201 Ru2 Ru5 109.37(15) . . ? C100 Ru2 Ru5 44.99(11) . . ? Ru3 Ru2 Ru5 60.399(13) . . ? Ru4 Ru2 Ru5 59.175(14) . . ? C202 Ru2 Ru1 85.10(13) . . ? C203 Ru2 Ru1 167.29(14) . . ? C201 Ru2 Ru1 78.53(13) . . ? C100 Ru2 Ru1 52.85(11) . . ? Ru3 Ru2 Ru1 60.847(13) . . ? Ru4 Ru2 Ru1 121.283(18) . . ? Ru5 Ru2 Ru1 96.828(14) . . ? C301 Ru3 C302 90.07(19) . . ? C301 Ru3 C303 95.64(19) . . ? C302 Ru3 C303 93.6(2) . . ? C301 Ru3 C100 90.47(17) . . ? C302 Ru3 C100 126.61(18) . . ? C303 Ru3 C100 139.31(18) . . ? C301 Ru3 Ru2 131.23(13) . . ? C302 Ru3 Ru2 134.88(14) . . ? C303 Ru3 Ru2 98.42(14) . . ? C100 Ru3 Ru2 50.66(11) . . ? C301 Ru3 Ru4 165.34(13) . . ? C302 Ru3 Ru4 76.49(14) . . ? C303 Ru3 Ru4 91.11(14) . . ? C100 Ru3 Ru4 92.87(11) . . ? Ru2 Ru3 Ru4 60.041(12) . . ? C301 Ru3 Ru5 115.29(13) . . ? C302 Ru3 Ru5 87.60(15) . . ? C303 Ru3 Ru5 149.05(14) . . ? C100 Ru3 Ru5 45.27(11) . . ? Ru2 Ru3 Ru5 60.959(18) . . ? Ru4 Ru3 Ru5 59.100(12) . . ? C301 Ru3 Ru1 71.73(13) . . ? C302 Ru3 Ru1 161.62(14) . . ? C303 Ru3 Ru1 90.78(14) . . ? C100 Ru3 Ru1 53.27(11) . . ? Ru2 Ru3 Ru1 61.665(16) . . ? Ru4 Ru3 Ru1 121.293(18) . . ? Ru5 Ru3 Ru1 97.696(19) . . ? C401 Ru4 C402 84.9(2) . . ? C401 Ru4 C403 97.4(2) . . ? C402 Ru4 C403 95.9(2) . . ? C401 Ru4 Ru5 101.42(16) . . ? C402 Ru4 Ru5 103.69(16) . . ? C403 Ru4 Ru5 153.82(15) . . ? C401 Ru4 Ru2 109.17(15) . . ? C402 Ru4 Ru2 160.48(14) . . ? C403 Ru4 Ru2 95.59(16) . . ? Ru5 Ru4 Ru2 61.118(18) . . ? C401 Ru4 Ru3 161.20(16) . . ? C402 Ru4 Ru3 103.53(14) . . ? C403 Ru4 Ru3 98.33(16) . . ? Ru5 Ru4 Ru3 60.476(17) . . ? Ru2 Ru4 Ru3 59.110(15) . . ? C503 Ru5 C502 95.7(2) . . ? C503 Ru5 C501 92.5(2) . . ? C502 Ru5 C501 96.9(2) . . ? C503 Ru5 C100 82.28(18) . . ? C502 Ru5 C100 127.3(2) . . ? C501 Ru5 C100 135.71(19) . . ? C503 Ru5 Ru4 177.46(14) . . ? C502 Ru5 Ru4 86.25(15) . . ? C501 Ru5 Ru4 85.69(15) . . ? C100 Ru5 Ru4 97.84(12) . . ? C503 Ru5 Ru3 118.19(14) . . ? C502 Ru5 Ru3 142.55(14) . . ? C501 Ru5 Ru3 97.06(15) . . ? C100 Ru5 Ru3 50.29(12) . . ? Ru4 Ru5 Ru3 60.425(16) . . ? C503 Ru5 Ru2 121.77(14) . . ? C502 Ru5 Ru2 90.99(16) . . ? C501 Ru5 Ru2 143.95(15) . . ? C100 Ru5 Ru2 50.09(12) . . ? Ru4 Ru5 Ru2 59.707(13) . . ? Ru3 Ru5 Ru2 58.643(14) . . ? C1 N1 C3 110.8(4) . . ? C1 N1 C5 128.0(4) . . ? C3 N1 C5 121.2(4) . . ? C1 N2 C2 110.1(4) . . ? C1 N2 C4 127.1(4) . . ? C2 N2 C4 122.8(4) . . ? O100 C100 Ru5 137.0(3) . . ? O100 C100 Ru3 126.2(3) . . ? Ru5 C100 Ru3 84.44(15) . . ? O100 C100 Ru2 126.3(3) . . ? Ru5 C100 Ru2 84.91(15) . . ? Ru3 C100 Ru2 78.80(13) . . ? O100 C100 Ru1 64.3(2) . . ? Ru5 C100 Ru1 158.7(2) . . ? Ru3 C100 Ru1 78.58(13) . . ? Ru2 C100 Ru1 79.24(13) . . ? C100 O100 Ru1 83.6(2) . . ? O101 C101 Ru1 179.1(4) . . ? O102 C102 Ru1 177.3(4) . . ? O201 C201 Ru2 173.7(4) . . ? O202 C202 Ru2 178.7(4) . . ? O203 C203 Ru2 167.6(4) . . ? O301 C301 Ru3 169.5(4) . . ? O302 C302 Ru3 170.1(4) . . ? O303 C303 Ru3 179.2(5) . . ? O401 C401 Ru4 177.0(5) . . ? O402 C402 Ru4 175.0(4) . . ? O403 C403 Ru4 179.2(5) . . ? O501 C501 Ru5 175.8(5) . . ? O502 C502 Ru5 177.7(6) . . ? O503 C503 Ru5 178.2(4) . . ? N2 C1 N1 104.7(4) . . ? N2 C1 Ru1 130.3(3) . . ? N1 C1 Ru1 124.9(3) . . ? C3 C2 N2 107.2(4) . . ? C2 C3 N1 107.2(5) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 23.29 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.374 _refine_diff_density_min -0.333 _refine_diff_density_rms 0.076 #===END data_5b_g64f6bm _database_code_depnum_ccdc_archive 'CCDC 676044' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H16 N4 O14 Ru5' _chemical_formula_sum 'C24 H16 N4 O14 Ru5' _chemical_formula_weight 1089.76 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 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 11.016(4) _cell_length_b 11.274(4) _cell_length_c 14.241(5) _cell_angle_alpha 81.390(7) _cell_angle_beta 82.044(7) _cell_angle_gamma 67.424(6) _cell_volume 1608.4(10) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 4567 _cell_measurement_theta_min 2.10 _cell_measurement_theta_max 23.45 _exptl_crystal_description BLOCK _exptl_crystal_colour BLACK _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.250 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1040 _exptl_absorpt_coefficient_mu 2.365 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.705 _exptl_absorpt_correction_T_max 0.790 _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 7191 _diffrn_reflns_av_R_equivalents 0.0198 _diffrn_reflns_av_sigmaI/netI 0.0263 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.97 _diffrn_reflns_theta_max 23.39 _reflns_number_total 4588 _reflns_number_gt 3931 _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^)+(0.0467P)^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 SHELXL _refine_ls_extinction_coef 0.00044(12) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4588 _refine_ls_number_parameters 428 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0335 _refine_ls_R_factor_gt 0.0272 _refine_ls_wR_factor_ref 0.0703 _refine_ls_wR_factor_gt 0.0672 _refine_ls_goodness_of_fit_ref 0.992 _refine_ls_restrained_S_all 0.992 _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 0.5427(4) 0.8707(4) 0.7476(3) 0.0361(11) Uani 1 1 d . . . C2 C 0.6611(5) 0.9805(5) 0.6598(4) 0.0562(15) Uani 1 1 d . . . H2 H 0.7199 1.0006 0.6129 0.067 Uiso 1 1 calc R . . C3 C 0.5863(6) 1.0537(5) 0.7264(5) 0.0616(16) Uani 1 1 d . . . H3 H 0.5829 1.1350 0.7354 0.074 Uiso 1 1 calc R . . C4 C 0.6983(5) 0.7684(5) 0.6092(4) 0.0503(13) Uani 1 1 d . . . H4A H 0.6354 0.7343 0.5964 0.075 Uiso 1 1 calc R . . H4B H 0.7703 0.7004 0.6386 0.075 Uiso 1 1 calc R . . H4C H 0.7310 0.8045 0.5505 0.075 Uiso 1 1 calc R . . C5 C 0.4141(6) 1.0418(6) 0.8567(4) 0.0696(17) Uani 1 1 d . . . H5A H 0.3279 1.0621 0.8370 0.104 Uiso 1 1 d R . . H5B H 0.4268 0.9810 0.9129 0.104 Uiso 1 1 d R . . H5C H 0.4219 1.1192 0.8705 0.104 Uiso 1 1 d R . . C6 C -0.0274(4) 0.9430(5) 0.8199(3) 0.0386(11) Uani 1 1 d . . . C7 C -0.1240(6) 1.1509(6) 0.8530(5) 0.0734(18) Uani 1 1 d . . . H7 H -0.1521 1.2405 0.8456 0.088 Uiso 1 1 calc R . . C8 C -0.1493(7) 1.0769(7) 0.9291(5) 0.083(2) Uani 1 1 d . . . H8 H -0.1977 1.1055 0.9857 0.100 Uiso 1 1 calc R . . C9 C 0.0096(6) 1.1127(5) 0.6961(4) 0.0632(16) Uani 1 1 d . . . H9A H -0.0540 1.1921 0.6701 0.095 Uiso 1 1 calc R . . H9B H 0.0330 1.0489 0.6522 0.095 Uiso 1 1 calc R . . H9C H 0.0870 1.1268 0.7066 0.095 Uiso 1 1 calc R . . C10 C -0.0964(7) 0.8407(7) 0.9773(4) 0.080(2) Uani 1 1 d . . . H10A H -0.1017 0.8617 1.0410 0.121 Uiso 1 1 calc R . . H10B H -0.0183 0.7659 0.9662 0.121 Uiso 1 1 calc R . . H10C H -0.1727 0.8231 0.9694 0.121 Uiso 1 1 calc R . . C100 C 0.2301(4) 0.7959(4) 0.7869(3) 0.0296(10) Uani 1 1 d . . . C101 C 0.5237(5) 0.7339(5) 0.9189(4) 0.0449(12) Uani 1 1 d . . . C102 C 0.6178(5) 0.5930(5) 0.7789(3) 0.0379(11) Uani 1 1 d . . . C201 C 0.3602(5) 0.8755(5) 0.6128(3) 0.0413(12) Uani 1 1 d . . . C202 C 0.4882(5) 0.5864(5) 0.6112(3) 0.0393(11) Uani 1 1 d . . . C203 C 0.2609(4) 0.7415(5) 0.5277(3) 0.0386(11) Uani 1 1 d . . . C301 C 0.3314(5) 0.6059(4) 0.9499(4) 0.0413(12) Uani 1 1 d . . . C302 C 0.1817(6) 0.5030(6) 0.8819(4) 0.0600(16) Uani 1 1 d . . . C303 C 0.4466(5) 0.4301(5) 0.8071(3) 0.0403(12) Uani 1 1 d . . . C401 C 0.1076(6) 0.5858(6) 0.5560(4) 0.0615(16) Uani 1 1 d . . . C402 C 0.0929(6) 0.4486(6) 0.7210(5) 0.0666(17) Uani 1 1 d . . . C403 C 0.3398(6) 0.3972(6) 0.6248(4) 0.0501(13) Uani 1 1 d . . . C501 C -0.0594(5) 0.7089(5) 0.7935(4) 0.0448(12) Uani 1 1 d . . . C502 C -0.0021(4) 0.8533(5) 0.6320(4) 0.0411(12) Uani 1 1 d . . . N1 N 0.5138(4) 0.9857(4) 0.7806(3) 0.0457(10) Uani 1 1 d . . . N2 N 0.6347(4) 0.8687(4) 0.6731(3) 0.0393(9) Uani 1 1 d . . . N3 N -0.0908(4) 0.9500(5) 0.9089(3) 0.0580(12) Uani 1 1 d . . . N4 N -0.0471(4) 1.0672(4) 0.7869(3) 0.0492(11) Uani 1 1 d . . . O100 O 0.2641(3) 0.8722(3) 0.8252(2) 0.0333(7) Uani 1 1 d . . . O101 O 0.5656(4) 0.7333(4) 0.9877(3) 0.0695(12) Uani 1 1 d . . . O102 O 0.7121(3) 0.5053(4) 0.7678(3) 0.0537(9) Uani 1 1 d . . . O201 O 0.3699(4) 0.9713(4) 0.5823(3) 0.0657(11) Uani 1 1 d . . . O202 O 0.5831(3) 0.5085(4) 0.5868(2) 0.0568(10) Uani 1 1 d . . . O203 O 0.2351(4) 0.7671(4) 0.4505(2) 0.0560(10) Uani 1 1 d . . . O301 O 0.3428(4) 0.6052(4) 1.0280(3) 0.0651(11) Uani 1 1 d . . . O302 O 0.1224(5) 0.4470(5) 0.9278(3) 0.0976(17) Uani 1 1 d . . . O303 O 0.5347(4) 0.3376(4) 0.7985(3) 0.0587(10) Uani 1 1 d . . . O401 O 0.0534(6) 0.6086(5) 0.4885(4) 0.107(2) Uani 1 1 d . . . O402 O 0.0346(6) 0.3852(5) 0.7521(4) 0.112(2) Uani 1 1 d . . . O403 O 0.4185(5) 0.3086(4) 0.5981(3) 0.0813(14) Uani 1 1 d . . . O501 O -0.1423(4) 0.6719(4) 0.8229(3) 0.0699(12) Uani 1 1 d . . . O502 O -0.0461(3) 0.8976(4) 0.5602(3) 0.0597(10) Uani 1 1 d . . . Ru1 Ru 0.46181(3) 0.73380(3) 0.80368(2) 0.02938(11) Uani 1 1 d . . . Ru2 Ru 0.32605(3) 0.71896(3) 0.64965(2) 0.02764(11) Uani 1 1 d . . . Ru3 Ru 0.29737(3) 0.58715(3) 0.82604(2) 0.02947(12) Uani 1 1 d . . . Ru4 Ru 0.19582(4) 0.54560(4) 0.66716(3) 0.03803(12) Uani 1 1 d . . . Ru5 Ru 0.07284(3) 0.77818(3) 0.74696(2) 0.03006(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 0.033(2) 0.030(3) 0.045(3) -0.005(2) -0.010(2) -0.009(2) C2 0.049(3) 0.044(4) 0.080(4) 0.013(3) -0.008(3) -0.027(3) C3 0.064(4) 0.031(3) 0.099(5) -0.001(3) -0.014(3) -0.028(3) C4 0.043(3) 0.057(4) 0.051(3) -0.011(3) 0.007(2) -0.020(3) C5 0.087(5) 0.049(4) 0.081(4) -0.027(3) 0.005(4) -0.031(4) C6 0.030(2) 0.038(3) 0.046(3) -0.009(2) -0.001(2) -0.010(2) C7 0.069(4) 0.039(4) 0.100(5) -0.026(4) 0.000(4) -0.003(3) C8 0.075(4) 0.072(5) 0.097(6) -0.043(4) 0.027(4) -0.020(4) C9 0.090(4) 0.038(3) 0.062(4) 0.004(3) -0.018(3) -0.023(3) C10 0.112(6) 0.091(5) 0.050(4) -0.023(3) 0.029(4) -0.057(5) C100 0.031(2) 0.026(3) 0.029(2) -0.0054(19) -0.0015(18) -0.008(2) C101 0.053(3) 0.044(3) 0.042(3) 0.002(2) -0.010(2) -0.023(3) C102 0.043(3) 0.036(3) 0.039(3) 0.001(2) -0.011(2) -0.018(3) C201 0.039(3) 0.050(3) 0.037(3) -0.002(2) -0.005(2) -0.018(3) C202 0.045(3) 0.043(3) 0.029(2) -0.004(2) -0.003(2) -0.016(3) C203 0.036(3) 0.042(3) 0.040(3) -0.012(2) -0.003(2) -0.014(2) C301 0.051(3) 0.023(3) 0.040(3) 0.003(2) -0.003(2) -0.007(2) C302 0.055(3) 0.058(4) 0.067(4) 0.018(3) -0.012(3) -0.028(3) C303 0.057(3) 0.037(3) 0.032(3) -0.002(2) -0.011(2) -0.021(3) C401 0.087(4) 0.045(4) 0.070(4) -0.006(3) -0.024(3) -0.038(3) C402 0.075(4) 0.057(4) 0.080(4) -0.027(3) 0.014(3) -0.038(4) C403 0.070(4) 0.040(3) 0.041(3) -0.006(2) -0.011(3) -0.018(3) C501 0.045(3) 0.036(3) 0.053(3) -0.001(2) -0.008(2) -0.015(3) C502 0.030(2) 0.045(3) 0.045(3) -0.003(2) 0.002(2) -0.013(2) N1 0.049(2) 0.035(3) 0.058(3) -0.008(2) -0.007(2) -0.019(2) N2 0.034(2) 0.036(2) 0.049(2) 0.0026(19) -0.0069(18) -0.0157(19) N3 0.056(3) 0.054(3) 0.057(3) -0.022(2) 0.019(2) -0.016(2) N4 0.045(2) 0.031(3) 0.062(3) -0.009(2) -0.006(2) -0.003(2) O100 0.0339(16) 0.0289(18) 0.0370(17) -0.0073(14) -0.0032(13) -0.0101(14) O101 0.096(3) 0.079(3) 0.045(2) -0.003(2) -0.033(2) -0.036(3) O102 0.040(2) 0.039(2) 0.071(3) -0.0055(18) -0.0067(17) -0.0020(19) O201 0.087(3) 0.053(3) 0.071(3) 0.022(2) -0.027(2) -0.045(2) O202 0.045(2) 0.056(3) 0.049(2) -0.0171(19) 0.0004(17) 0.005(2) O203 0.063(2) 0.065(3) 0.037(2) -0.0068(18) -0.0177(17) -0.017(2) O301 0.100(3) 0.066(3) 0.030(2) -0.0021(18) -0.0115(19) -0.031(2) O302 0.090(3) 0.124(4) 0.095(3) 0.044(3) -0.012(3) -0.076(3) O303 0.062(2) 0.028(2) 0.070(3) -0.0137(18) -0.0121(19) 0.005(2) O401 0.157(5) 0.099(4) 0.103(4) 0.018(3) -0.083(4) -0.076(4) O402 0.139(5) 0.109(4) 0.129(4) -0.028(3) 0.031(4) -0.101(4) O403 0.101(3) 0.043(3) 0.070(3) -0.019(2) -0.003(2) 0.010(3) O501 0.062(3) 0.088(3) 0.077(3) -0.006(2) 0.003(2) -0.051(3) O502 0.050(2) 0.078(3) 0.043(2) 0.009(2) -0.0136(18) -0.018(2) Ru1 0.0322(2) 0.0262(2) 0.0315(2) -0.00278(15) -0.00534(15) -0.01201(17) Ru2 0.0313(2) 0.0266(2) 0.0250(2) -0.00272(14) -0.00112(14) -0.01118(17) Ru3 0.0357(2) 0.0238(2) 0.0285(2) 0.00122(15) -0.00381(15) -0.01175(17) Ru4 0.0454(2) 0.0313(2) 0.0438(2) -0.00903(17) -0.00629(18) -0.01873(19) Ru5 0.0280(2) 0.0279(2) 0.0337(2) -0.00269(15) -0.00191(15) -0.01023(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.352(6) . ? C1 N2 1.359(6) . ? C1 Ru1 2.074(5) . ? C2 C3 1.325(8) . ? C2 N2 1.379(6) . ? C3 N1 1.394(7) . ? C4 N2 1.456(6) . ? C5 N1 1.458(7) . ? C6 N4 1.351(6) . ? C6 N3 1.358(6) . ? C6 Ru5 2.106(5) . ? C7 C8 1.332(9) . ? C7 N4 1.387(7) . ? C8 N3 1.382(8) . ? C9 N4 1.467(7) . ? C10 N3 1.467(8) . ? C100 O100 1.274(5) . ? C100 Ru5 1.984(4) . ? C100 Ru3 2.186(4) . ? C100 Ru2 2.218(4) . ? C100 Ru1 2.411(4) . ? C101 O101 1.138(6) . ? C101 Ru1 1.862(5) . ? C102 O102 1.138(6) . ? C102 Ru1 1.872(5) . ? C201 O201 1.140(6) . ? C201 Ru2 1.926(6) . ? C202 O202 1.128(6) . ? C202 Ru2 1.910(5) . ? C203 O203 1.139(5) . ? C203 Ru2 1.916(5) . ? C301 O301 1.135(6) . ? C301 Ru3 1.911(5) . ? C302 O302 1.152(6) . ? C302 Ru3 1.891(6) . ? C303 O303 1.128(6) . ? C303 Ru3 1.922(6) . ? C401 O401 1.146(7) . ? C401 Ru4 1.879(6) . ? C402 O402 1.141(7) . ? C402 Ru4 1.878(6) . ? C403 O403 1.119(6) . ? C403 Ru4 1.918(6) . ? C501 O501 1.147(6) . ? C501 Ru5 1.904(5) . ? C502 O502 1.151(6) . ? C502 Ru5 1.872(5) . ? O100 Ru1 2.150(3) . ? Ru1 Ru3 2.8459(9) . ? Ru1 Ru2 2.8785(9) . ? Ru2 Ru3 2.7643(9) . ? Ru2 Ru4 2.8016(9) . ? Ru2 Ru5 2.8149(10) . ? Ru3 Ru5 2.8248(8) . ? Ru3 Ru4 2.8303(9) . ? Ru4 Ru5 2.7822(10) . ? 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 N2 103.8(4) . . ? N1 C1 Ru1 125.9(3) . . ? N2 C1 Ru1 130.3(3) . . ? C3 C2 N2 106.8(5) . . ? C2 C3 N1 107.0(5) . . ? N4 C6 N3 104.1(4) . . ? N4 C6 Ru5 127.5(3) . . ? N3 C6 Ru5 128.3(4) . . ? C8 C7 N4 106.1(6) . . ? C7 C8 N3 107.7(6) . . ? O100 C100 Ru5 141.6(3) . . ? O100 C100 Ru3 124.4(3) . . ? Ru5 C100 Ru3 85.13(16) . . ? O100 C100 Ru2 122.9(3) . . ? Ru5 C100 Ru2 83.92(15) . . ? Ru3 C100 Ru2 77.74(14) . . ? O100 C100 Ru1 62.8(2) . . ? Ru5 C100 Ru1 155.6(2) . . ? Ru3 C100 Ru1 76.33(13) . . ? Ru2 C100 Ru1 76.78(13) . . ? O101 C101 Ru1 177.8(5) . . ? O102 C102 Ru1 177.1(4) . . ? O201 C201 Ru2 171.4(4) . . ? O202 C202 Ru2 178.6(4) . . ? O203 C203 Ru2 168.3(4) . . ? O301 C301 Ru3 170.3(4) . . ? O302 C302 Ru3 169.5(5) . . ? O303 C303 Ru3 178.2(4) . . ? O401 C401 Ru4 178.9(5) . . ? O402 C402 Ru4 177.0(6) . . ? O403 C403 Ru4 175.8(5) . . ? O501 C501 Ru5 177.2(5) . . ? O502 C502 Ru5 178.6(5) . . ? C1 N1 C3 110.9(4) . . ? C1 N1 C5 127.2(4) . . ? C3 N1 C5 121.8(5) . . ? C1 N2 C2 111.5(4) . . ? C1 N2 C4 127.6(4) . . ? C2 N2 C4 120.9(4) . . ? C6 N3 C8 110.5(5) . . ? C6 N3 C10 126.4(5) . . ? C8 N3 C10 123.1(5) . . ? C6 N4 C7 111.5(5) . . ? C6 N4 C9 126.3(4) . . ? C7 N4 C9 122.0(5) . . ? C100 O100 Ru1 85.5(2) . . ? C101 Ru1 C102 87.6(2) . . ? C101 Ru1 C1 86.9(2) . . ? C102 Ru1 C1 94.23(19) . . ? C101 Ru1 O100 99.44(18) . . ? C102 Ru1 O100 168.83(16) . . ? C1 Ru1 O100 94.78(15) . . ? C101 Ru1 C100 122.04(19) . . ? C102 Ru1 C100 137.18(18) . . ? C1 Ru1 C100 115.64(16) . . ? O100 Ru1 C100 31.79(12) . . ? C101 Ru1 Ru3 111.44(15) . . ? C102 Ru1 Ru3 94.44(14) . . ? C1 Ru1 Ru3 160.03(12) . . ? O100 Ru1 Ru3 74.97(8) . . ? C100 Ru1 Ru3 48.29(11) . . ? C101 Ru1 Ru2 168.44(15) . . ? C102 Ru1 Ru2 96.92(14) . . ? C1 Ru1 Ru2 103.32(13) . . ? O100 Ru1 Ru2 74.57(8) . . ? C100 Ru1 Ru2 48.61(10) . . ? Ru3 Ru1 Ru2 57.745(18) . . ? C202 Ru2 C203 92.09(19) . . ? C202 Ru2 C201 103.7(2) . . ? C203 Ru2 C201 88.1(2) . . ? C202 Ru2 C100 135.03(17) . . ? C203 Ru2 C100 132.09(18) . . ? C201 Ru2 C100 88.09(18) . . ? C202 Ru2 Ru3 93.80(14) . . ? C203 Ru2 Ru3 136.28(15) . . ? C201 Ru2 Ru3 131.89(14) . . ? C100 Ru2 Ru3 50.61(11) . . ? C202 Ru2 Ru4 90.21(15) . . ? C203 Ru2 Ru4 75.58(15) . . ? C201 Ru2 Ru4 159.00(14) . . ? C100 Ru2 Ru4 93.13(11) . . ? Ru3 Ru2 Ru4 61.126(18) . . ? C202 Ru2 Ru5 146.64(14) . . ? C203 Ru2 Ru5 92.96(14) . . ? C201 Ru2 Ru5 109.43(14) . . ? C100 Ru2 Ru5 44.49(11) . . ? Ru3 Ru2 Ru5 60.828(16) . . ? Ru4 Ru2 Ru5 59.39(2) . . ? C202 Ru2 Ru1 85.80(14) . . ? C203 Ru2 Ru1 163.19(15) . . ? C201 Ru2 Ru1 76.28(14) . . ? C100 Ru2 Ru1 54.61(11) . . ? Ru3 Ru2 Ru1 60.53(2) . . ? Ru4 Ru2 Ru1 121.05(2) . . ? Ru5 Ru2 Ru1 97.96(1) . . ? C302 Ru3 C301 90.2(2) . . ? C302 Ru3 C303 94.8(2) . . ? C301 Ru3 C303 96.92(19) . . ? C302 Ru3 C100 122.7(2) . . ? C301 Ru3 C100 91.27(17) . . ? C303 Ru3 C100 141.56(18) . . ? C302 Ru3 Ru2 134.12(17) . . ? C301 Ru3 Ru2 131.50(14) . . ? C303 Ru3 Ru2 97.45(14) . . ? C100 Ru3 Ru2 51.64(11) . . ? C302 Ru3 Ru5 85.67(17) . . ? C301 Ru3 Ru5 117.34(14) . . ? C303 Ru3 Ru5 145.74(13) . . ? C100 Ru3 Ru5 44.41(11) . . ? Ru2 Ru3 Ru5 60.47(2) . . ? C302 Ru3 Ru4 76.51(18) . . ? C301 Ru3 Ru4 166.22(15) . . ? C303 Ru3 Ru4 87.79(13) . . ? C100 Ru3 Ru4 93.04(11) . . ? Ru2 Ru3 Ru4 60.09(1) . . ? Ru5 Ru3 Ru4 58.94(2) . . ? C302 Ru3 Ru1 161.37(19) . . ? C301 Ru3 Ru1 71.76(14) . . ? C303 Ru3 Ru1 91.81(15) . . ? C100 Ru3 Ru1 55.39(11) . . ? Ru2 Ru3 Ru1 61.720(17) . . ? Ru5 Ru3 Ru1 98.50(3) . . ? Ru4 Ru3 Ru1 121.20(2) . . ? C401 Ru4 C402 89.0(3) . . ? C401 Ru4 C403 95.7(2) . . ? C402 Ru4 C403 93.2(2) . . ? C401 Ru4 Ru5 100.00(18) . . ? C402 Ru4 Ru5 103.72(18) . . ? C403 Ru4 Ru5 157.02(16) . . ? C401 Ru4 Ru2 104.91(17) . . ? C402 Ru4 Ru2 160.18(18) . . ? C403 Ru4 Ru2 99.24(17) . . ? Ru5 Ru4 Ru2 60.55(1) . . ? C401 Ru4 Ru3 158.40(17) . . ? C402 Ru4 Ru3 103.8(2) . . ? C403 Ru4 Ru3 100.74(16) . . ? Ru5 Ru4 Ru3 60.429(19) . . ? Ru2 Ru4 Ru3 58.787(17) . . ? C502 Ru5 C501 93.9(2) . . ? C502 Ru5 C100 124.94(19) . . ? C501 Ru5 C100 141.02(19) . . ? C502 Ru5 C6 95.2(2) . . ? C501 Ru5 C6 91.6(2) . . ? C100 Ru5 C6 82.42(17) . . ? C502 Ru5 Ru4 88.73(16) . . ? C501 Ru5 Ru4 83.41(16) . . ? C100 Ru5 Ru4 99.23(12) . . ? C6 Ru5 Ru4 173.84(13) . . ? C502 Ru5 Ru2 89.63(14) . . ? C501 Ru5 Ru2 143.24(16) . . ? C100 Ru5 Ru2 51.59(12) . . ? C6 Ru5 Ru2 124.56(12) . . ? Ru4 Ru5 Ru2 60.067(16) . . ? C502 Ru5 Ru3 143.36(14) . . ? C501 Ru5 Ru3 101.33(15) . . ? C100 Ru5 Ru3 50.46(13) . . ? C6 Ru5 Ru3 117.24(13) . . ? Ru4 Ru5 Ru3 60.63(2) . . ? Ru2 Ru5 Ru3 58.70(2) . . ? _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 23.39 _diffrn_measured_fraction_theta_full 0.978 _refine_diff_density_max 0.538 _refine_diff_density_min -0.695 _refine_diff_density_rms 0.099 #===END