# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2003 data_global _journal_coden_Cambridge 182 loop_ _publ_author_name 'Philip Coppens' 'Bao-Qing Ma' _publ_contact_author_name 'Prof Philip Coppens' _publ_contact_author_address ; Chemistry State University of New York at Buf Buffalo New York 14260 UNITED STATES OF AMERICA ; _publ_contact_author_email COPPENS@ACSU.BUFFALO.EDU _publ_requested_journal 'Chemical Communications' _publ_section_title ; Transformation of a C-methylcalix[4]resorcinarene based host-guest complex from a wave-like to a novel triangular brick-wall architecture ; data_c2c _database_code_CSD 196014 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C66 H62 N4 O8 Ru' _chemical_formula_weight 1140.27 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 23.9761(12) _cell_length_b 17.1389(9) _cell_length_c 15.5942(8) _cell_angle_alpha 90.00 _cell_angle_beta 121.336(2) _cell_angle_gamma 90.00 _cell_volume 5473.3(5) _cell_formula_units_Z 4 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.384 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2376 _exptl_absorpt_coefficient_mu 0.349 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.792 _exptl_absorpt_correction_T_max 0.893 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 273(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 'SMART CCD 1000' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 42681 _diffrn_reflns_av_R_equivalents 0.0637 _diffrn_reflns_av_sigmaI/netI 0.0491 _diffrn_reflns_limit_h_min -34 _diffrn_reflns_limit_h_max 34 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.55 _diffrn_reflns_theta_max 31.03 _reflns_number_total 7979 _reflns_number_gt 5332 _reflns_threshold_expression >2sigma(I) _computing_data_collection SMART _computing_cell_refinement SMART _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics XP _computing_publication_material XCIF _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^)+(0.0914P)^2^+14.3211P] 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 0.00053(17) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 7979 _refine_ls_number_parameters 450 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0946 _refine_ls_R_factor_gt 0.0568 _refine_ls_wR_factor_ref 0.1883 _refine_ls_wR_factor_gt 0.1639 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.033 _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 0.0000 0.91211(2) 0.7500 0.04250(16) Uani 1 2 d S . . O1 O -0.23220(11) -0.34155(14) -0.13617(17) 0.0267(5) Uani 1 1 d . . . O2 O -0.26290(9) -0.34226(13) 0.14410(14) 0.0266(4) Uani 1 1 d D . . O3 O -0.39924(10) -0.14085(15) -0.00416(19) 0.0344(6) Uani 1 1 d . . . H3 H -0.4017(17) -0.106(2) -0.007(3) 0.012(9) Uiso 1 1 d . . . O4 O -0.62884(10) -0.14423(15) -0.24627(19) 0.0342(5) Uani 1 1 d . . . H4 H -0.6241(19) -0.108(2) -0.245(3) 0.030(11) Uiso 1 1 d . . . C1 C -0.36431(17) -0.3875(2) -0.3188(3) 0.0366(8) Uani 1 1 d . . . C2 C -0.36169(12) -0.30739(16) -0.27320(19) 0.0216(5) Uani 1 1 d . . . H2A H -0.3314(16) -0.2785(19) -0.277(2) 0.022(8) Uiso 1 1 d . . . H1C H -0.3759(16) -0.385(2) -0.378(3) 0.022(8) Uiso 1 1 d . . . H1B H -0.391(2) -0.419(2) -0.318(3) 0.037(11) Uiso 1 1 d . . . H1A H -0.327(2) -0.415(3) -0.292(4) 0.057(13) Uiso 1 1 d . . . C3 C -0.33697(11) -0.31677(14) -0.16263(19) 0.0189(5) Uani 1 1 d . . . C4 C -0.27137(11) -0.33516(14) -0.0968(2) 0.0197(5) Uani 1 1 d . . . C5 C -0.24630(12) -0.34572(15) 0.0052(2) 0.0211(5) Uani 1 1 d . . . H5A H -0.2014(16) -0.3570(18) 0.046(2) 0.021(8) Uiso 1 1 d . . . C6 C -0.28665(12) -0.33534(15) 0.04344(19) 0.0201(5) Uani 1 1 d . . . C7 C -0.35250(11) -0.31622(14) -0.01918(19) 0.0188(5) Uani 1 1 d . . . C8 C -0.37565(12) -0.30782(15) -0.1210(2) 0.0194(5) Uani 1 1 d . . . H8A H -0.4096(18) -0.294(2) -0.150(3) 0.030(9) Uiso 1 1 d . . . C9 C -0.39415(12) -0.30240(16) 0.02697(19) 0.0207(5) Uani 1 1 d . . . H9A H -0.3733(15) -0.2680(18) 0.080(2) 0.017(7) Uiso 1 1 d . . . C10 C -0.40466(16) -0.3778(2) 0.0694(3) 0.0327(7) Uani 1 1 d . . . H10C H -0.4204(18) -0.411(2) 0.027(3) 0.023(9) Uiso 1 1 d . . . H10B H -0.371(2) -0.402(2) 0.109(3) 0.042(11) Uiso 1 1 d . . . H10A H -0.431(2) -0.368(2) 0.094(3) 0.048(11) Uiso 1 1 d . . . C11 C -0.45711(11) -0.25969(15) -0.04379(19) 0.0193(5) Uani 1 1 d . . . C12 C -0.45714(12) -0.17952(15) -0.0578(2) 0.0216(5) Uani 1 1 d . . . C13 C -0.51446(13) -0.14071(16) -0.1250(2) 0.0254(6) Uani 1 1 d . . . H13A H -0.5145(17) -0.088(2) -0.135(3) 0.030(9) Uiso 1 1 d . . . C14 C -0.57244(12) -0.18189(16) -0.1798(2) 0.0225(5) Uani 1 1 d . . . C15 C -0.57492(11) -0.26220(15) -0.16877(18) 0.0193(5) Uani 1 1 d . . . C16 C -0.51639(12) -0.29837(16) -0.1007(2) 0.0204(5) Uani 1 1 d . . . H16A H -0.5154(17) -0.345(2) -0.090(3) 0.031(9) Uiso 1 1 d . . . C17 C -0.4049(2) 0.0770(2) -0.0461(4) 0.0613(12) Uani 1 1 d . . . H17A H -0.4455 0.0709 -0.1044 0.074 Uiso 1 1 calc R . . C18 C -0.3767(2) 0.1494(2) -0.0258(4) 0.0568(11) Uani 1 1 d . . . H18A H -0.3959(19) 0.181(2) -0.064(3) 0.036(10) Uiso 1 1 d . . . C19 C -0.31631(17) 0.16137(19) 0.0601(3) 0.0372(7) Uani 1 1 d . . . C20 C -0.2883(2) 0.0969(2) 0.1211(3) 0.0429(8) Uani 1 1 d . . . H20A H -0.2558(19) 0.096(2) 0.173(3) 0.032(10) Uiso 1 1 d . . . C21 C -0.3200(2) 0.0260(2) 0.0950(3) 0.0473(9) Uani 1 1 d . . . H21A H -0.3016(19) -0.012(3) 0.136(3) 0.043(11) Uiso 1 1 d . . . C22 C -0.28560(19) 0.23849(19) 0.0796(3) 0.0410(8) Uani 1 1 d . . . H22A H -0.3072(19) 0.273(2) 0.027(3) 0.042(11) Uiso 1 1 d . . . C23 C -0.23046(18) 0.25920(19) 0.1601(3) 0.0391(7) Uani 1 1 d . . . H23A H -0.2086 0.2215 0.2094 0.047 Uiso 1 1 calc R . . C24 C -0.20035(17) 0.33688(18) 0.1789(3) 0.0349(7) Uani 1 1 d . . . C25 C -0.2312(2) 0.4009(2) 0.1181(4) 0.0454(9) Uani 1 1 d . . . H25A H -0.259(2) 0.395(3) 0.075(3) 0.042(13) Uiso 1 1 d . . . C26 C -0.2006(2) 0.4726(2) 0.1416(3) 0.0500(9) Uani 1 1 d . . . H26A H -0.2186(19) 0.513(2) 0.093(3) 0.040(10) Uiso 1 1 d . . . C27 C -0.11227(19) 0.4234(2) 0.2804(3) 0.0448(8) Uani 1 1 d . . . H27A H -0.0711 0.4306 0.3373 0.054 Uiso 1 1 calc R . . C28 C -0.13861(19) 0.3498(2) 0.2622(3) 0.0413(8) Uani 1 1 d . . . H28A H -0.1206(18) 0.314(2) 0.299(3) 0.030(9) Uiso 1 1 d . . . C29 C 0.0523(3) 0.9380(3) 0.9090(3) 0.0680(13) Uani 1 1 d . . . H29A H 0.0333 0.9596 0.9465 0.082 Uiso 1 1 calc R . . C30 C 0.0803(3) 0.9815(4) 0.8631(4) 0.0877(19) Uani 1 1 d . . . H30A H 0.0838 1.0385 0.8631 0.105 Uiso 1 1 calc R . . C31 C 0.1047(3) 0.9290(4) 0.8222(4) 0.0828(18) Uani 1 1 d . . . H31A H 0.1282 0.9426 0.7884 0.099 Uiso 1 1 calc R . . C32 C 0.0914(3) 0.8521(4) 0.8413(4) 0.0717(14) Uani 1 1 d . . . H32A H 0.1048 0.8034 0.8243 0.086 Uiso 1 1 calc R . . C33 C 0.0592(2) 0.8591(3) 0.8951(3) 0.0645(12) Uani 1 1 d . . . H33A H 0.0459 0.8156 0.9215 0.077 Uiso 1 1 calc R . . N1 N -0.37850(16) 0.01569(18) 0.0112(3) 0.0480(8) Uani 1 1 d . . . N2 N -0.14146(16) 0.48472(17) 0.2224(3) 0.0475(8) Uani 1 1 d . . . H1 H -0.2060(15) -0.3410(17) -0.105(2) 0.001(8) Uiso 1 1 d . . . H2 H -0.2226(9) -0.338(2) 0.172(3) 0.034(10) Uiso 1 1 d 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 0.0573(3) 0.0360(2) 0.0359(2) 0.000 0.0254(2) 0.000 O1 0.0106(9) 0.0404(12) 0.0233(11) 0.0020(9) 0.0048(9) 0.0034(9) O2 0.0142(8) 0.0399(11) 0.0163(9) 0.0046(8) 0.0014(7) 0.0024(8) O3 0.0141(9) 0.0228(11) 0.0428(14) -0.0017(10) -0.0016(9) -0.0033(8) O4 0.0138(9) 0.0252(12) 0.0407(13) 0.0009(10) -0.0019(9) 0.0041(8) C1 0.0261(15) 0.0424(18) 0.0263(17) -0.0063(14) 0.0030(13) 0.0131(14) C2 0.0129(10) 0.0279(13) 0.0186(12) 0.0023(10) 0.0044(9) 0.0035(9) C3 0.0112(10) 0.0203(11) 0.0183(11) 0.0015(9) 0.0028(9) 0.0005(8) C4 0.0114(10) 0.0186(11) 0.0230(12) 0.0007(9) 0.0047(9) 0.0002(8) C5 0.0119(10) 0.0212(12) 0.0215(12) 0.0021(9) 0.0027(9) 0.0021(9) C6 0.0136(10) 0.0205(11) 0.0180(12) 0.0020(9) 0.0026(9) 0.0006(9) C7 0.0129(10) 0.0196(11) 0.0178(11) 0.0016(9) 0.0037(9) 0.0004(8) C8 0.0099(10) 0.0209(11) 0.0204(12) 0.0029(9) 0.0030(9) 0.0025(9) C9 0.0146(11) 0.0252(12) 0.0170(12) 0.0018(10) 0.0046(9) 0.0022(9) C10 0.0246(14) 0.0377(17) 0.0329(17) 0.0139(15) 0.0128(13) 0.0048(13) C11 0.0130(10) 0.0233(12) 0.0171(11) -0.0006(9) 0.0046(9) 0.0017(9) C12 0.0116(10) 0.0227(12) 0.0222(12) -0.0044(10) 0.0030(9) -0.0025(9) C13 0.0164(11) 0.0189(12) 0.0292(14) -0.0015(10) 0.0036(11) 0.0003(9) C14 0.0116(10) 0.0248(12) 0.0215(12) -0.0024(10) 0.0019(9) 0.0025(9) C15 0.0121(10) 0.0249(12) 0.0162(11) -0.0041(9) 0.0040(9) -0.0020(9) C16 0.0165(11) 0.0200(12) 0.0207(12) -0.0014(10) 0.0068(10) -0.0004(9) C17 0.040(2) 0.045(2) 0.069(3) -0.002(2) 0.008(2) -0.0110(17) C18 0.046(2) 0.0349(19) 0.067(3) 0.008(2) 0.014(2) 0.0004(17) C19 0.0421(18) 0.0271(14) 0.0469(19) -0.0068(13) 0.0263(16) -0.0072(13) C20 0.043(2) 0.0362(18) 0.041(2) -0.0060(15) 0.0157(17) -0.0099(15) C21 0.057(2) 0.0275(17) 0.051(2) -0.0011(15) 0.0232(19) -0.0064(15) C22 0.050(2) 0.0245(15) 0.047(2) -0.0006(14) 0.0247(17) -0.0053(14) C23 0.0491(19) 0.0267(15) 0.0436(19) 0.0010(13) 0.0254(17) -0.0068(14) C24 0.0439(18) 0.0269(14) 0.0396(17) -0.0051(12) 0.0257(15) -0.0090(13) C25 0.041(2) 0.0331(18) 0.051(2) -0.0043(16) 0.0157(19) -0.0077(15) C26 0.053(2) 0.0273(17) 0.061(3) 0.0034(16) 0.023(2) -0.0033(15) C27 0.0432(19) 0.0425(19) 0.045(2) -0.0060(16) 0.0200(17) -0.0118(15) C28 0.048(2) 0.0351(18) 0.0411(19) 0.0040(15) 0.0228(17) -0.0058(15) C29 0.086(3) 0.076(3) 0.043(2) -0.016(2) 0.034(2) -0.020(3) C30 0.115(5) 0.081(4) 0.065(3) -0.027(3) 0.044(3) -0.053(4) C31 0.065(3) 0.129(5) 0.054(3) -0.012(3) 0.030(3) -0.029(3) C32 0.059(3) 0.087(4) 0.055(3) 0.007(3) 0.020(2) 0.018(3) C33 0.066(3) 0.076(3) 0.039(2) 0.011(2) 0.018(2) 0.000(2) N1 0.0445(17) 0.0316(14) 0.061(2) -0.0063(14) 0.0227(16) -0.0118(13) N2 0.0483(18) 0.0291(14) 0.062(2) -0.0068(14) 0.0262(16) -0.0122(12) _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 C33 2.150(4) 2_556 ? Ru1 C33 2.150(4) . ? Ru1 C32 2.155(5) 2_556 ? Ru1 C32 2.155(5) . ? Ru1 C29 2.165(4) 2_556 ? Ru1 C29 2.165(4) . ? Ru1 C30 2.169(5) . ? Ru1 C30 2.169(5) 2_556 ? Ru1 C31 2.171(5) . ? Ru1 C31 2.171(5) 2_556 ? O1 C4 1.368(3) . ? O2 C6 1.369(3) . ? O3 C12 1.363(3) . ? O4 C14 1.364(3) . ? C1 C2 1.532(4) . ? C2 C3 1.512(4) . ? C2 C15 1.516(3) 2_454 ? C3 C8 1.390(4) . ? C3 C4 1.396(3) . ? C4 C5 1.389(4) . ? C5 C6 1.387(4) . ? C6 C7 1.396(3) . ? C7 C8 1.390(4) . ? C7 C9 1.523(4) . ? C9 C11 1.516(3) . ? C9 C10 1.531(4) . ? C11 C16 1.391(3) . ? C11 C12 1.391(4) . ? C12 C13 1.390(4) . ? C13 C14 1.387(4) . ? C14 C15 1.392(4) . ? C15 C16 1.390(4) . ? C15 C2 1.516(3) 2_454 ? C17 N1 1.309(5) . ? C17 C18 1.370(6) . ? C18 C19 1.384(6) . ? C19 C20 1.384(5) . ? C19 C22 1.466(4) . ? C20 C21 1.377(5) . ? C21 N1 1.341(5) . ? C22 C23 1.312(5) . ? C23 C24 1.469(4) . ? C24 C25 1.385(5) . ? C24 C28 1.389(5) . ? C25 C26 1.379(5) . ? C26 N2 1.336(5) . ? C27 N2 1.324(5) . ? C27 C28 1.371(5) . ? C29 C33 1.394(7) . ? C29 C30 1.422(8) . ? C30 C31 1.395(9) . ? C31 C32 1.423(8) . ? C32 C33 1.411(7) . ? 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 C33 Ru1 C33 130.0(3) 2_556 . ? C33 Ru1 C32 38.3(2) 2_556 2_556 ? C33 Ru1 C32 112.4(2) . 2_556 ? C33 Ru1 C32 112.4(2) 2_556 . ? C33 Ru1 C32 38.3(2) . . ? C32 Ru1 C32 123.0(3) 2_556 . ? C33 Ru1 C29 37.7(2) 2_556 2_556 ? C33 Ru1 C29 164.8(2) . 2_556 ? C32 Ru1 C29 63.7(2) 2_556 2_556 ? C32 Ru1 C29 129.7(2) . 2_556 ? C33 Ru1 C29 164.8(2) 2_556 . ? C33 Ru1 C29 37.7(2) . . ? C32 Ru1 C29 129.7(2) 2_556 . ? C32 Ru1 C29 63.7(2) . . ? C29 Ru1 C29 156.3(3) 2_556 . ? C33 Ru1 C30 155.4(2) 2_556 . ? C33 Ru1 C30 63.5(2) . . ? C32 Ru1 C30 165.3(2) 2_556 . ? C32 Ru1 C30 63.7(3) . . ? C29 Ru1 C30 124.0(2) 2_556 . ? C29 Ru1 C30 38.3(2) . . ? C33 Ru1 C30 63.5(2) 2_556 2_556 ? C33 Ru1 C30 155.4(2) . 2_556 ? C32 Ru1 C30 63.7(3) 2_556 2_556 ? C32 Ru1 C30 165.3(2) . 2_556 ? C29 Ru1 C30 38.3(2) 2_556 2_556 ? C29 Ru1 C30 124.0(2) . 2_556 ? C30 Ru1 C30 113.4(4) . 2_556 ? C33 Ru1 C31 123.7(2) 2_556 . ? C33 Ru1 C31 63.8(2) . . ? C32 Ru1 C31 155.6(3) 2_556 . ? C32 Ru1 C31 38.4(2) . . ? C29 Ru1 C31 113.0(2) 2_556 . ? C29 Ru1 C31 63.5(2) . . ? C30 Ru1 C31 37.5(2) . . ? C30 Ru1 C31 130.3(3) 2_556 . ? C33 Ru1 C31 63.8(2) 2_556 2_556 ? C33 Ru1 C31 123.7(2) . 2_556 ? C32 Ru1 C31 38.4(2) 2_556 2_556 ? C32 Ru1 C31 155.6(3) . 2_556 ? C29 Ru1 C31 63.5(2) 2_556 2_556 ? C29 Ru1 C31 113.0(2) . 2_556 ? C30 Ru1 C31 130.3(3) . 2_556 ? C30 Ru1 C31 37.5(3) 2_556 2_556 ? C31 Ru1 C31 164.7(4) . 2_556 ? C3 C2 C15 114.3(2) . 2_454 ? C3 C2 C1 109.3(2) . . ? C15 C2 C1 113.2(2) 2_454 . ? C8 C3 C4 116.9(2) . . ? C8 C3 C2 124.0(2) . . ? C4 C3 C2 119.1(2) . . ? O1 C4 C5 120.9(2) . . ? O1 C4 C3 117.5(2) . . ? C5 C4 C3 121.5(2) . . ? C6 C5 C4 119.5(2) . . ? O2 C6 C5 121.0(2) . . ? O2 C6 C7 117.8(2) . . ? C5 C6 C7 121.1(2) . . ? C8 C7 C6 117.2(2) . . ? C8 C7 C9 123.6(2) . . ? C6 C7 C9 119.1(2) . . ? C3 C8 C7 123.7(2) . . ? C11 C9 C7 112.4(2) . . ? C11 C9 C10 113.4(2) . . ? C7 C9 C10 111.6(2) . . ? C16 C11 C12 117.0(2) . . ? C16 C11 C9 122.3(2) . . ? C12 C11 C9 120.7(2) . . ? O3 C12 C13 121.5(2) . . ? O3 C12 C11 117.8(2) . . ? C13 C12 C11 120.7(2) . . ? C14 C13 C12 120.1(3) . . ? O4 C14 C13 120.5(3) . . ? O4 C14 C15 118.2(2) . . ? C13 C14 C15 121.4(2) . . ? C16 C15 C14 116.4(2) . . ? C16 C15 C2 121.9(2) . 2_454 ? C14 C15 C2 121.7(2) . 2_454 ? C15 C16 C11 124.4(2) . . ? N1 C17 C18 124.4(4) . . ? C17 C18 C19 120.0(4) . . ? C20 C19 C18 115.9(3) . . ? C20 C19 C22 124.4(3) . . ? C18 C19 C22 119.6(3) . . ? C21 C20 C19 120.3(4) . . ? N1 C21 C20 122.8(4) . . ? C23 C22 C19 126.2(4) . . ? C22 C23 C24 125.6(3) . . ? C25 C24 C28 116.3(3) . . ? C25 C24 C23 123.3(3) . . ? C28 C24 C23 120.4(3) . . ? C26 C25 C24 120.2(4) . . ? N2 C26 C25 123.1(4) . . ? N2 C27 C28 124.4(4) . . ? C27 C28 C24 119.5(4) . . ? C33 C29 C30 107.7(5) . . ? C33 C29 Ru1 70.6(3) . . ? C30 C29 Ru1 71.0(3) . . ? C31 C30 C29 108.2(5) . . ? C31 C30 Ru1 71.3(3) . . ? C29 C30 Ru1 70.7(3) . . ? C30 C31 C32 108.1(5) . . ? C30 C31 Ru1 71.2(3) . . ? C32 C31 Ru1 70.2(3) . . ? C33 C32 C31 107.3(5) . . ? C33 C32 Ru1 70.7(3) . . ? C31 C32 Ru1 71.4(3) . . ? C29 C33 C32 108.8(5) . . ? C29 C33 Ru1 71.8(3) . . ? C32 C33 Ru1 71.1(3) . . ? C17 N1 C21 116.6(3) . . ? C27 N2 C26 116.5(3) . . ? _diffrn_measured_fraction_theta_max 0.911 _diffrn_reflns_theta_full 31.03 _diffrn_measured_fraction_theta_full 0.911 _refine_diff_density_max 0.491 _refine_diff_density_min -1.533 _refine_diff_density_rms 0.091 data_c2c_b _database_code_CSD 196015 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C68 H68 N4 O9 Ru' _chemical_formula_weight 1186.33 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 C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 15.0614(18) _cell_length_b 14.6928(18) _cell_length_c 26.775(4) _cell_angle_alpha 90.00 _cell_angle_beta 95.622(5) _cell_angle_gamma 90.00 _cell_volume 5896.7(13) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prismatic _exptl_crystal_colour yellow _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.336 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2480 _exptl_absorpt_coefficient_mu 0.328 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.784 _exptl_absorpt_correction_T_max 0.913 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'SMART CCD 1000' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 51747 _diffrn_reflns_av_R_equivalents 0.0804 _diffrn_reflns_av_sigmaI/netI 0.0770 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -38 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_theta_min 1.53 _diffrn_reflns_theta_max 31.17 _reflns_number_total 8818 _reflns_number_gt 4015 _reflns_threshold_expression >2sigma(I) _computing_data_collection SMART _computing_cell_refinement SMART _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics XP _computing_publication_material XCIF _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^)+(0.1163P)^2^+7.1546P] 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 0.0040(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 8818 _refine_ls_number_parameters 449 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1629 _refine_ls_R_factor_gt 0.0703 _refine_ls_wR_factor_ref 0.2444 _refine_ls_wR_factor_gt 0.1906 _refine_ls_goodness_of_fit_ref 1.012 _refine_ls_restrained_S_all 1.012 _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 0.0000 0.75514(4) 0.2500 0.0610(2) Uani 1 2 d S . . O1 O -0.1470(2) 1.4887(2) 0.56361(12) 0.0618(8) Uani 1 1 d D . . O2 O 0.1714(2) 1.4669(2) 0.59000(14) 0.0596(9) Uani 1 1 d . . . H2 H 0.161(4) 1.437(4) 0.5741(19) 0.062(18) Uiso 1 1 d . . . O3 O 0.2670(3) 1.4222(3) 0.68786(17) 0.0761(11) Uani 1 1 d . . . H3 H 0.249(3) 1.437(3) 0.6665(15) 0.031(13) Uiso 1 1 d . . . O4 O 0.2482(3) 1.4365(3) 0.86011(15) 0.0783(11) Uani 1 1 d . . . H4 H 0.221(4) 1.459(4) 0.8784(19) 0.067(18) Uiso 1 1 d . . . O5 O -0.9457(16) 1.0511(10) 0.3591(6) 0.213(8) Uani 0.50 1 d P . . H5B H -0.9490 1.0475 0.3895 0.320 Uiso 0.50 1 calc PR . . N1 N -0.1350(2) 0.6940(2) 0.46095(14) 0.0597(9) Uani 1 1 d . . . N2 N -0.1315(3) 1.3227(2) 0.52248(15) 0.0602(9) Uani 1 1 d . . . C1 C -0.1521(5) 1.7159(3) 0.6517(2) 0.0596(12) Uani 1 1 d . . . C2 C -0.1552(3) 1.6124(2) 0.64451(15) 0.0477(9) Uani 1 1 d . . . H2A H -0.203(3) 1.600(3) 0.6160(16) 0.062(12) Uiso 1 1 d . . . H1C H -0.124(4) 1.744(3) 0.616(2) 0.10(2) Uiso 1 1 d . . . H1B H -0.199(3) 1.740(3) 0.6575(17) 0.047(12) Uiso 1 1 d . . . H1A H -0.114(4) 1.738(3) 0.675(2) 0.067(16) Uiso 1 1 d . . . C3 C -0.0680(3) 1.5752(2) 0.62857(14) 0.0431(8) Uani 1 1 d . . . C4 C -0.0671(3) 1.5141(2) 0.58912(14) 0.0452(8) Uani 1 1 d . . . C5 C 0.0119(3) 1.4791(3) 0.57565(15) 0.0477(9) Uani 1 1 d . . . H5A H 0.008(3) 1.438(3) 0.5521(17) 0.066(13) Uiso 1 1 d . . . C6 C 0.0921(3) 1.5038(2) 0.60143(14) 0.0444(8) Uani 1 1 d . . . C7 C 0.0951(3) 1.5672(2) 0.63996(13) 0.0427(8) Uani 1 1 d . . . C8 C 0.0130(3) 1.6001(2) 0.65206(14) 0.0423(8) Uani 1 1 d . . . H8A H 0.010(2) 1.634(3) 0.6768(15) 0.042(10) Uiso 1 1 d . . . C9 C 0.1825(3) 1.5985(2) 0.66757(14) 0.0441(8) Uani 1 1 d . . . H9A H 0.226(2) 1.577(2) 0.6502(12) 0.030(8) Uiso 1 1 d . . . C10 C 0.1915(4) 1.7023(3) 0.66867(18) 0.0549(10) Uani 1 1 d . . . H10C H 0.151(3) 1.727(3) 0.6827(19) 0.058(14) Uiso 1 1 d . . . C11 C 0.1976(2) 1.5565(2) 0.71927(15) 0.0454(8) Uani 1 1 d . . . C12 C 0.2389(3) 1.4723(3) 0.72639(17) 0.0532(10) Uani 1 1 d . . . C13 C 0.2536(3) 1.4356(3) 0.7732(2) 0.0641(12) Uani 1 1 d . . . H13A H 0.286(4) 1.386(4) 0.778(2) 0.102(19) Uiso 1 1 d . . . C14 C 0.2277(3) 1.4790(3) 0.81477(17) 0.0570(10) Uani 1 1 d . . . C15 C 0.1847(2) 1.5631(2) 0.81003(14) 0.0435(8) Uani 1 1 d . . . C16 C 0.1714(2) 1.5980(2) 0.76218(14) 0.0420(8) Uani 1 1 d . . . H16A H 0.141(2) 1.652(3) 0.7595(13) 0.042(10) Uiso 1 1 d . . . C17 C -0.1439(4) 0.7232(3) 0.50723(19) 0.0742(14) Uani 1 1 d . . . H17A H -0.1515 0.6800 0.5319 0.089 Uiso 1 1 calc R . . C18 C -0.1425(4) 0.8129(3) 0.5206(2) 0.0797(15) Uani 1 1 d . . . H18A H -0.1493 0.8295 0.5535 0.096 Uiso 1 1 calc R . . C19 C -0.1309(3) 0.8791(3) 0.48496(19) 0.0667(13) Uani 1 1 d . . . C20 C -0.1208(4) 0.8495(3) 0.4379(2) 0.0767(14) Uani 1 1 d . . . H20A H -0.1125 0.8912 0.4127 0.092 Uiso 1 1 calc R . . C21 C -0.1230(4) 0.7570(3) 0.42737(19) 0.0717(13) Uani 1 1 d . . . H21A H -0.1155 0.7386 0.3948 0.086 Uiso 1 1 calc R . . C22 C -0.1350(4) 0.9769(4) 0.5026(3) 0.0921(18) Uani 1 1 d . . . H22A H -0.1517 0.9867 0.5347 0.111 Uiso 1 1 calc R . . C23 C -0.1190(4) 1.0412(4) 0.4791(2) 0.0856(16) Uani 1 1 d . . . H23A H -0.1016 1.0312 0.4472 0.103 Uiso 1 1 calc R . . C24 C -0.1242(3) 1.1409(4) 0.4965(2) 0.0747(15) Uani 1 1 d . . . C25 C -0.1596(4) 1.1681(4) 0.5402(2) 0.0855(17) Uani 1 1 d . . . H25A H -0.1811 1.1254 0.5616 0.103 Uiso 1 1 calc R . . C26 C -0.1621(4) 1.2617(3) 0.5514(2) 0.0754(14) Uani 1 1 d . . . H26A H -0.1864 1.2803 0.5803 0.090 Uiso 1 1 calc R . . C27 C -0.0987(4) 1.2928(4) 0.4815(2) 0.0761(14) Uani 1 1 d . . . H27A H -0.0769 1.3359 0.4605 0.091 Uiso 1 1 calc R . . C28 C -0.0944(4) 1.2057(4) 0.4679(2) 0.0803(15) Uani 1 1 d . . . H28A H -0.0705 1.1903 0.4383 0.096 Uiso 1 1 calc R . . C29 C -0.0743(5) 0.8238(5) 0.3041(2) 0.0903(18) Uani 1 1 d . . . H29A H -0.1062 0.8818 0.2994 0.108 Uiso 1 1 calc R . . C30 C -0.1102(4) 0.7359(5) 0.2949(2) 0.0887(18) Uani 1 1 d . . . H30A H -0.1719 0.7226 0.2817 0.106 Uiso 1 1 calc R . . C31 C -0.0443(5) 0.6705(5) 0.3084(2) 0.0898(18) Uani 1 1 d . . . H31A H -0.0521 0.6043 0.3071 0.108 Uiso 1 1 calc R . . C32 C 0.0317(5) 0.7161(6) 0.3269(2) 0.098(2) Uani 1 1 d . . . H32A H 0.0875 0.6869 0.3404 0.118 Uiso 1 1 calc R . . C33 C 0.0169(5) 0.8114(5) 0.3250(2) 0.099(2) Uani 1 1 d . . . H33A H 0.0590 0.8590 0.3374 0.118 Uiso 1 1 calc R . . C34 C -0.9968(14) 1.0847(19) 0.2790(7) 0.209(13) Uani 0.50 1 d P . . H34A H -1.0477 1.1070 0.2582 0.314 Uiso 0.50 1 calc PR . . H34B H -0.9829 1.0242 0.2688 0.314 Uiso 0.50 1 calc PR . . H34C H -0.9466 1.1238 0.2757 0.314 Uiso 0.50 1 calc PR . . C35 C -1.0191(12) 1.0835(13) 0.3377(10) 0.176(13) Uani 0.50 1 d P . . H35A H -1.0309 1.1442 0.3498 0.211 Uiso 0.50 1 calc PR . . H35B H -1.0694 1.0442 0.3425 0.211 Uiso 0.50 1 calc PR . . H10B H 0.182(3) 1.727(3) 0.6355(19) 0.060(13) Uiso 1 1 d . . . H10A H 0.261(3) 1.720(3) 0.6857(16) 0.056(12) Uiso 1 1 d . . . H1 H -0.160(5) 1.4318(19) 0.568(3) 0.12(3) Uiso 1 1 d 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 0.0589(3) 0.0743(4) 0.0510(3) 0.000 0.0113(2) 0.000 O1 0.0581(18) 0.0588(19) 0.0653(19) -0.0240(16) -0.0103(14) 0.0055(15) O2 0.0577(19) 0.0531(18) 0.070(2) -0.0252(17) 0.0164(15) -0.0030(14) O3 0.092(3) 0.056(2) 0.082(3) -0.008(2) 0.018(2) 0.0258(19) O4 0.096(3) 0.067(2) 0.070(2) 0.0235(19) 0.002(2) 0.023(2) O5 0.34(3) 0.157(13) 0.158(13) -0.055(11) 0.097(15) -0.077(15) N1 0.067(2) 0.049(2) 0.065(2) -0.0081(17) 0.0172(18) 0.0065(17) N2 0.063(2) 0.0474(19) 0.067(2) -0.0113(18) -0.0097(18) -0.0009(17) C1 0.085(3) 0.036(2) 0.059(3) 0.0020(19) 0.017(3) 0.018(2) C2 0.054(2) 0.0391(19) 0.049(2) -0.0049(16) -0.0002(18) 0.0105(17) C3 0.054(2) 0.0319(17) 0.0432(19) -0.0022(14) 0.0032(16) 0.0030(15) C4 0.051(2) 0.0341(17) 0.049(2) -0.0053(15) -0.0009(17) 0.0004(15) C5 0.058(2) 0.0385(19) 0.047(2) -0.0128(17) 0.0047(17) 0.0011(17) C6 0.054(2) 0.0348(17) 0.046(2) -0.0067(15) 0.0133(17) -0.0011(16) C7 0.055(2) 0.0315(16) 0.0428(18) -0.0015(14) 0.0115(16) -0.0047(15) C8 0.058(2) 0.0305(17) 0.0388(18) -0.0069(15) 0.0087(16) 0.0000(15) C9 0.048(2) 0.0370(18) 0.049(2) -0.0077(16) 0.0114(17) -0.0059(16) C10 0.069(3) 0.043(2) 0.054(3) -0.0019(19) 0.012(2) -0.014(2) C11 0.0413(19) 0.0355(18) 0.060(2) -0.0035(16) 0.0059(17) -0.0068(15) C12 0.048(2) 0.040(2) 0.073(3) -0.005(2) 0.0123(19) 0.0046(16) C13 0.059(3) 0.044(2) 0.089(4) 0.005(2) 0.006(2) 0.014(2) C14 0.051(2) 0.053(2) 0.065(3) 0.011(2) -0.001(2) 0.0038(19) C15 0.0391(18) 0.0378(18) 0.053(2) 0.0052(16) 0.0010(16) -0.0066(15) C16 0.0409(19) 0.0313(17) 0.054(2) -0.0001(15) 0.0056(16) -0.0038(15) C17 0.104(4) 0.058(3) 0.062(3) -0.003(2) 0.014(3) 0.009(3) C18 0.114(4) 0.063(3) 0.062(3) -0.014(2) 0.010(3) 0.013(3) C19 0.064(3) 0.051(2) 0.081(3) -0.018(2) -0.011(2) 0.009(2) C20 0.099(4) 0.058(3) 0.073(3) 0.013(2) 0.012(3) -0.008(3) C21 0.093(4) 0.069(3) 0.055(3) -0.014(2) 0.018(2) -0.001(3) C22 0.095(4) 0.082(4) 0.095(4) 0.015(3) -0.014(3) -0.004(3) C23 0.075(4) 0.104(5) 0.076(4) 0.002(3) -0.003(3) -0.004(3) C24 0.061(3) 0.063(3) 0.094(4) -0.026(3) -0.023(3) 0.012(2) C25 0.082(4) 0.064(3) 0.104(4) 0.025(3) -0.019(3) -0.017(3) C26 0.083(4) 0.067(3) 0.073(3) -0.009(3) -0.012(3) -0.001(3) C27 0.085(4) 0.060(3) 0.080(4) -0.010(3) -0.003(3) -0.002(3) C28 0.085(4) 0.060(3) 0.094(4) -0.022(3) -0.001(3) 0.004(3) C29 0.108(5) 0.092(4) 0.077(4) -0.014(3) 0.039(3) 0.014(4) C30 0.073(3) 0.123(5) 0.075(4) 0.000(3) 0.033(3) -0.006(4) C31 0.112(5) 0.096(4) 0.066(3) 0.017(3) 0.031(3) -0.010(4) C32 0.106(5) 0.140(6) 0.048(3) 0.008(3) 0.010(3) 0.011(5) C33 0.113(5) 0.121(6) 0.064(3) -0.032(3) 0.019(3) -0.034(4) C34 0.129(16) 0.35(4) 0.144(16) -0.109(19) -0.010(14) 0.04(2) C35 0.121(14) 0.096(11) 0.29(3) 0.045(15) -0.101(18) -0.013(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 C32 2.146(6) . ? Ru1 C32 2.146(6) 2 ? Ru1 C31 2.155(5) . ? Ru1 C31 2.155(5) 2 ? Ru1 C30 2.161(5) 2 ? Ru1 C30 2.161(5) . ? Ru1 C33 2.164(5) . ? Ru1 C33 2.164(5) 2 ? Ru1 C29 2.165(5) 2 ? Ru1 C29 2.165(5) . ? O1 C4 1.375(5) . ? O2 C6 1.374(5) . ? O3 C12 1.367(5) . ? O4 C14 1.373(5) . ? O5 C35 1.29(3) . ? N1 C21 1.315(6) . ? N1 C17 1.331(6) . ? N2 C26 1.298(7) . ? N2 C27 1.322(6) . ? C1 C2 1.532(6) . ? C2 C15 1.520(6) 2_556 ? C2 C3 1.522(5) . ? C3 C8 1.367(5) . ? C3 C4 1.387(5) . ? C4 C5 1.377(5) . ? C5 C6 1.380(5) . ? C6 C7 1.387(5) . ? C7 C8 1.394(5) . ? C7 C9 1.516(5) . ? C9 C11 1.512(5) . ? C9 C10 1.531(5) . ? C11 C12 1.390(5) . ? C11 C16 1.392(5) . ? C12 C13 1.363(6) . ? C13 C14 1.373(7) . ? C14 C15 1.395(5) . ? C15 C16 1.376(5) . ? C15 C2 1.520(5) 2_556 ? C17 C18 1.366(7) . ? C18 C19 1.385(7) . ? C19 C20 1.355(7) . ? C19 C22 1.515(7) . ? C20 C21 1.388(7) . ? C22 C23 1.174(8) . ? C23 C24 1.542(8) . ? C24 C28 1.327(8) . ? C24 C25 1.391(8) . ? C25 C26 1.408(7) . ? C27 C28 1.334(7) . ? C29 C30 1.413(8) . ? C29 C33 1.443(9) . ? C30 C31 1.404(9) . ? C31 C32 1.376(9) . ? C32 C33 1.417(10) . ? C34 C35 1.64(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C32 Ru1 C32 149.0(4) . 2 ? C32 Ru1 C31 37.3(2) . . ? C32 Ru1 C31 119.2(3) 2 . ? C32 Ru1 C31 119.2(3) . 2 ? C32 Ru1 C31 37.3(2) 2 2 ? C31 Ru1 C31 109.5(4) . 2 ? C32 Ru1 C30 112.8(3) . 2 ? C32 Ru1 C30 62.8(3) 2 2 ? C31 Ru1 C30 129.6(3) . 2 ? C31 Ru1 C30 38.0(2) 2 2 ? C32 Ru1 C30 62.8(3) . . ? C32 Ru1 C30 112.8(3) 2 . ? C31 Ru1 C30 38.0(2) . . ? C31 Ru1 C30 129.6(3) 2 . ? C30 Ru1 C30 165.0(4) 2 . ? C32 Ru1 C33 38.4(3) . . ? C32 Ru1 C33 171.0(3) 2 . ? C31 Ru1 C33 64.1(3) . . ? C31 Ru1 C33 151.4(3) 2 . ? C30 Ru1 C33 122.6(3) 2 . ? C30 Ru1 C33 64.0(3) . . ? C32 Ru1 C33 171.0(4) . 2 ? C32 Ru1 C33 38.4(3) 2 2 ? C31 Ru1 C33 151.4(3) . 2 ? C31 Ru1 C33 64.1(3) 2 2 ? C30 Ru1 C33 64.0(3) 2 2 ? C30 Ru1 C33 122.6(3) . 2 ? C33 Ru1 C33 135.1(4) . 2 ? C32 Ru1 C29 133.3(3) . 2 ? C32 Ru1 C29 64.1(3) 2 2 ? C31 Ru1 C29 166.4(3) . 2 ? C31 Ru1 C29 64.3(3) 2 2 ? C30 Ru1 C29 38.1(2) 2 2 ? C30 Ru1 C29 155.3(3) . 2 ? C33 Ru1 C29 114.9(3) . 2 ? C33 Ru1 C29 38.9(3) 2 2 ? C32 Ru1 C29 64.1(3) . . ? C32 Ru1 C29 133.3(3) 2 . ? C31 Ru1 C29 64.3(3) . . ? C31 Ru1 C29 166.4(3) 2 . ? C30 Ru1 C29 155.3(3) 2 . ? C30 Ru1 C29 38.1(2) . . ? C33 Ru1 C29 38.9(3) . . ? C33 Ru1 C29 114.9(3) 2 . ? C29 Ru1 C29 124.4(4) 2 . ? C21 N1 C17 116.3(4) . . ? C26 N2 C27 116.6(4) . . ? C15 C2 C3 112.4(3) 2_556 . ? C15 C2 C1 112.3(3) 2_556 . ? C3 C2 C1 112.0(4) . . ? C8 C3 C4 116.7(3) . . ? C8 C3 C2 122.1(3) . . ? C4 C3 C2 121.2(3) . . ? O1 C4 C5 120.3(3) . . ? O1 C4 C3 118.8(3) . . ? C5 C4 C3 120.9(4) . . ? C4 C5 C6 120.5(3) . . ? O2 C6 C5 121.5(3) . . ? O2 C6 C7 117.7(4) . . ? C5 C6 C7 120.8(3) . . ? C6 C7 C8 116.1(3) . . ? C6 C7 C9 122.0(3) . . ? C8 C7 C9 121.9(3) . . ? C3 C8 C7 124.9(3) . . ? C11 C9 C7 111.6(3) . . ? C11 C9 C10 112.5(3) . . ? C7 C9 C10 112.5(3) . . ? C12 C11 C16 115.9(4) . . ? C12 C11 C9 120.9(3) . . ? C16 C11 C9 123.2(3) . . ? C13 C12 O3 116.5(4) . . ? C13 C12 C11 120.6(4) . . ? O3 C12 C11 122.9(4) . . ? C12 C13 C14 121.9(4) . . ? C13 C14 O4 116.6(4) . . ? C13 C14 C15 120.3(4) . . ? O4 C14 C15 123.1(4) . . ? C16 C15 C14 116.0(4) . . ? C16 C15 C2 122.7(3) . 2_556 ? C14 C15 C2 121.2(3) . 2_556 ? C15 C16 C11 125.3(4) . . ? N1 C17 C18 123.7(5) . . ? C17 C18 C19 119.8(5) . . ? C20 C19 C18 116.6(4) . . ? C20 C19 C22 127.3(5) . . ? C18 C19 C22 116.1(5) . . ? C19 C20 C21 120.1(5) . . ? N1 C21 C20 123.5(4) . . ? C23 C22 C19 125.4(7) . . ? C22 C23 C24 125.7(7) . . ? C28 C24 C25 117.3(5) . . ? C28 C24 C23 118.4(5) . . ? C25 C24 C23 124.3(6) . . ? C24 C25 C26 118.7(5) . . ? N2 C26 C25 121.9(6) . . ? N2 C27 C28 125.4(6) . . ? C24 C28 C27 120.1(6) . . ? C30 C29 C33 106.6(6) . . ? C30 C29 Ru1 70.7(3) . . ? C33 C29 Ru1 70.5(3) . . ? C31 C30 C29 109.3(6) . . ? C31 C30 Ru1 70.8(3) . . ? C29 C30 Ru1 71.1(3) . . ? C32 C31 C30 107.6(6) . . ? C32 C31 Ru1 71.0(3) . . ? C30 C31 Ru1 71.2(3) . . ? C31 C32 C33 110.2(6) . . ? C31 C32 Ru1 71.7(3) . . ? C33 C32 Ru1 71.5(3) . . ? C32 C33 C29 106.2(6) . . ? C32 C33 Ru1 70.1(3) . . ? C29 C33 Ru1 70.6(3) . . ? O5 C35 C34 101(2) . . ? _diffrn_measured_fraction_theta_max 0.923 _diffrn_reflns_theta_full 31.17 _diffrn_measured_fraction_theta_full 0.923 _refine_diff_density_max 1.209 _refine_diff_density_min -1.149 _refine_diff_density_rms 0.104