# Supplementary Material (ESI) for ChemComm # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 182/1819 # CIF file data_global #============================================================================== # 1. SUBMISSION DETAILS _publ_contact_author # Name and address of author for corresponding ; Philip Coppens Department of Chemistry State University of New York at Buffalo Buffalo, NY 14260-3000 USA ; _publ_contact_author_phone '+1 (716) 645-6800 ext 2217' _publ_contact_author_fax '+1 (716) 645-6948' _publ_contact_author_email 'coppens@acsu.buffalo.edu' _publ_contact_letter ; ; _publ_requested_journal 'Chemical Communications' _publ_section_title ; ; _publ_section_abstract ; ; #============================================================================== # 3. TITLE AND AUTHOR LIST loop_ _publ_author_name _publ_author_address 'Yuegang Zhang, Christopher D. Kim and Philip Coppens' ; Department of Chemistry Natural Sciences Complex State University of New York at Buffalo Buffalo, NY 14260-3000 USA ; #============================================================================== # data data_CMCRBIPYDMR _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C64 H71 N4 O10 Ru0.50' _chemical_formula_weight 1106.78 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 trclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.5878(4) _cell_length_b 13.5020(4) _cell_length_c 17.5000(6) _cell_angle_alpha 96.0730(10) _cell_angle_beta 108.9230(10) _cell_angle_gamma 96.7020(10) _cell_volume 2761.48(15) _cell_formula_units_Z 2 _cell_measurement_temperature 90(1) _cell_measurement_reflns_used 120 _cell_measurement_theta_min 2.5 _cell_measurement_theta_max 25.0 _exptl_crystal_description needle _exptl_crystal_colour orange _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.331 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1170 _exptl_absorpt_coefficient_mu 0.218 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'SMART 1K CCD diffractometer' _diffrn_measurement_method 'oscillation around \w and \f' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25037 _diffrn_reflns_av_R_equivalents 0.0346 _diffrn_reflns_av_sigmaI/netI 0.0594 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.12 _diffrn_reflns_theta_max 29.14 _reflns_number_total 13375 _reflns_number_gt 9166 _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 SHELX-XP _computing_publication_material SHELX-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^)+(0.1252P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0176(18) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 13375 _refine_ls_number_parameters 1008 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0906 _refine_ls_R_factor_gt 0.0653 _refine_ls_wR_factor_ref 0.2033 _refine_ls_wR_factor_gt 0.1881 _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_restrained_S_all 1.058 _refine_ls_shift/su_max 2.244 _refine_ls_shift/su_mean 0.049 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 0.5839(2) 0.83872(18) 0.42234(13) 0.0211(5) Uani 1 1 d . . . H1 H 0.579(2) 0.794(2) 0.3713(18) 0.028(7) Uiso 1 1 d . . . O1 O 0.74271(15) 1.07891(14) 0.54107(11) 0.0253(4) Uani 1 1 d . . . H1D H 0.730(3) 1.107(3) 0.573(2) 0.038(10) Uiso 1 1 d . . . C2 C 0.6599(2) 0.92940(18) 0.44519(13) 0.0200(5) Uani 1 1 d . . . O2 O 0.46184(17) 0.83612(14) 0.58333(11) 0.0254(4) Uani 1 1 d . . . H2D H 0.461(3) 0.871(3) 0.612(2) 0.036(11) Uiso 1 1 d . . . C3 C 0.6682(2) 0.98932(17) 0.51820(13) 0.0212(5) Uani 1 1 d . . . O3 O 0.28122(16) 0.79992(14) 0.32840(10) 0.0270(4) Uani 1 1 d . . . H3D H 0.224(3) 0.822(3) 0.293(2) 0.065(12) Uiso 1 1 d . . . C4 C 0.6040(2) 0.95880(18) 0.56496(13) 0.0211(5) Uani 1 1 d . . . H4 H 0.601(2) 1.009(2) 0.6047(18) 0.026(7) Uiso 1 1 d . . . O4 O 0.27060(16) 0.56452(15) 0.09921(10) 0.0296(4) Uani 1 1 d . . . H4D H 0.226(3) 0.595(3) 0.073(2) 0.058(12) Uiso 1 1 d . . . C5 C 0.5281(2) 0.86857(18) 0.53963(13) 0.0206(5) Uani 1 1 d . . . O5 O 0.46129(18) 0.32330(14) 0.07743(12) 0.0328(5) Uani 1 1 d . . . H5D H 0.456(3) 0.298(3) 0.036(2) 0.043(10) Uiso 1 1 d . . . C6 C 0.5171(2) 0.80617(17) 0.46713(13) 0.0203(5) Uani 1 1 d . . . O6 O 0.73766(18) 0.56601(15) 0.03303(12) 0.0361(5) Uani 1 1 d . . . H6D H 0.722(3) 0.532(3) -0.010(2) 0.047(10) Uiso 1 1 d . . . C7 C 0.4347(2) 0.70700(18) 0.44183(14) 0.0226(5) Uani 1 1 d . . . H7 H 0.366(2) 0.720(2) 0.4517(16) 0.022(7) Uiso 1 1 d . . . O7 O 0.52708(17) 0.79420(14) 0.05818(10) 0.0292(4) Uani 1 1 d . . . H7D H 0.469(3) 0.822(3) 0.039(2) 0.052(11) Uiso 1 1 d . . . C8 C 0.4860(3) 0.6290(2) 0.49346(16) 0.0306(6) Uani 1 1 d . . . H8A H 0.554(3) 0.618(3) 0.487(2) 0.046(10) Uiso 1 1 d . . . H8B H 0.505(3) 0.651(2) 0.548(2) 0.036(8) Uiso 1 1 d . . . H8C H 0.439(3) 0.576(3) 0.4807(18) 0.031(8) Uiso 1 1 d . . . O8 O 0.53573(16) 1.02382(14) 0.28917(10) 0.0275(4) Uani 1 1 d . . . H8D H 0.486(3) 1.046(3) 0.255(2) 0.055(11) Uiso 1 1 d . . . C9 C 0.4279(2) 0.58678(18) 0.31620(14) 0.0217(5) Uani 1 1 d . . . H9 H 0.473(3) 0.558(2) 0.3515(19) 0.034(8) Uiso 1 1 d . . . C10 C 0.3936(2) 0.66988(17) 0.35040(13) 0.0210(5) Uani 1 1 d . . . C11 C 0.3165(2) 0.71809(18) 0.29675(14) 0.0214(5) Uani 1 1 d . . . C12 C 0.2756(2) 0.68381(19) 0.21282(14) 0.0240(5) Uani 1 1 d . . . H12 H 0.221(2) 0.719(2) 0.1741(17) 0.024(7) Uiso 1 1 d . . . C13 C 0.3114(2) 0.59992(18) 0.18172(14) 0.0221(5) Uani 1 1 d . . . C14 C 0.3890(2) 0.54932(17) 0.23289(14) 0.0209(5) Uani 1 1 d . . . C15 C 0.4276(2) 0.45820(18) 0.19715(14) 0.0227(5) Uani 1 1 d . . . H15 H 0.357(2) 0.417(2) 0.1537(18) 0.030(8) Uiso 1 1 d . . . C16 C 0.4770(3) 0.3902(2) 0.26041(16) 0.0273(5) Uani 1 1 d . . . H16A H 0.551(2) 0.422(2) 0.3003(17) 0.022(7) Uiso 1 1 d . . . H16B H 0.422(2) 0.367(2) 0.2836(18) 0.027(7) Uiso 1 1 d . . . H16C H 0.494(3) 0.333(2) 0.2361(19) 0.037(8) Uiso 1 1 d . . . C17 C 0.5755(2) 0.58468(18) 0.17042(13) 0.0202(5) Uani 1 1 d . . . H17 H 0.569(2) 0.6309(19) 0.2110(16) 0.016(6) Uiso 1 1 d . . . C18 C 0.5111(2) 0.48817(18) 0.15404(13) 0.0216(5) Uani 1 1 d . . . C19 C 0.5262(2) 0.41829(18) 0.09516(15) 0.0258(5) Uani 1 1 d . . . C20 C 0.6019(2) 0.4423(2) 0.05572(15) 0.0287(6) Uani 1 1 d . . . H20 H 0.607(3) 0.394(2) 0.0105(19) 0.037(8) Uiso 1 1 d . . . C21 C 0.6637(2) 0.53937(19) 0.07298(15) 0.0266(5) Uani 1 1 d . . . C22 C 0.6515(2) 0.61277(17) 0.13101(13) 0.0205(5) Uani 1 1 d . . . C23 C 0.7212(2) 0.71794(17) 0.14806(13) 0.0199(5) Uani 1 1 d . . . H23 H 0.712(2) 0.738(2) 0.0934(17) 0.027(7) Uiso 1 1 d . . . C24 C 0.8464(2) 0.7151(2) 0.19754(16) 0.0254(5) Uani 1 1 d . . . H24A H 0.888(3) 0.673(2) 0.1694(19) 0.037(8) Uiso 1 1 d . . . H24B H 0.890(2) 0.779(2) 0.2122(17) 0.026(7) Uiso 1 1 d . . . H24C H 0.857(2) 0.693(2) 0.2469(19) 0.027(7) Uiso 1 1 d . . . C25 C 0.7199(2) 0.84271(17) 0.26884(13) 0.0197(5) Uani 1 1 d . . . H25 H 0.789(3) 0.821(2) 0.3004(18) 0.030(7) Uiso 1 1 d . . . C26 C 0.67172(19) 0.79842(17) 0.18697(13) 0.0189(4) Uani 1 1 d . . . C27 C 0.5752(2) 0.83338(18) 0.13973(13) 0.0214(5) Uani 1 1 d . . . C28 C 0.5287(2) 0.90788(18) 0.17357(14) 0.0226(5) Uani 1 1 d . . . H28 H 0.461(2) 0.928(2) 0.1395(16) 0.020(6) Uiso 1 1 d . . . C29 C 0.5799(2) 0.94979(17) 0.25571(13) 0.0204(5) Uani 1 1 d . . . C30 C 0.67757(19) 0.91796(17) 0.30530(13) 0.0189(4) Uani 1 1 d . . . C31 C 0.7304(2) 0.96515(19) 0.39442(13) 0.0215(5) Uani 1 1 d . . . H31 H 0.730(2) 1.043(2) 0.3932(17) 0.026(7) Uiso 1 1 d . . . C32 C 0.8543(2) 0.9497(2) 0.43315(16) 0.0309(6) Uani 1 1 d . . . H32A H 0.862(2) 0.881(2) 0.4368(18) 0.030(8) Uiso 1 1 d . . . H32B H 0.902(3) 0.974(2) 0.402(2) 0.040(9) Uiso 1 1 d . . . H32C H 0.885(3) 0.983(2) 0.4897(19) 0.032(8) Uiso 1 1 d . . . C33 C 0.1811(2) 0.2108(2) 0.12534(17) 0.0335(6) Uani 1 1 d . . . C34 C 0.1950(2) 0.1812(2) 0.20187(17) 0.0342(6) Uani 1 1 d . . . H34 H 0.145(3) 0.192(2) 0.234(2) 0.037(8) Uiso 1 1 d . . . C35 C 0.2816(3) 0.1280(2) 0.23490(17) 0.0358(6) Uani 1 1 d . . . H35 H 0.301(3) 0.104(3) 0.293(2) 0.047(9) Uiso 1 1 d . . . C36 C 0.3405(3) 0.1307(3) 0.1257(2) 0.0415(7) Uani 1 1 d . . . H36 H 0.400(4) 0.121(4) 0.108(3) 0.102(18) Uiso 1 1 d . . . C37 C 0.2574(2) 0.1838(3) 0.08803(19) 0.0425(8) Uani 1 1 d . . . H37 H 0.2522 0.2020 0.0373 0.051 Uiso 1 1 calc R . . C38 C 0.0881(2) 0.2663(2) 0.08488(17) 0.0355(6) Uani 1 1 d . . . C39 C -0.0072(3) 0.2707(4) 0.1089(2) 0.0613(11) Uani 1 1 d . . . H39 H 0.001(4) 0.253(4) 0.168(3) 0.090(15) Uiso 1 1 d . . . C40 C -0.0940(3) 0.3171(4) 0.0645(2) 0.0666(12) Uani 1 1 d . . . H40 H -0.1567 0.3197 0.0812 0.080 Uiso 1 1 calc R . . C41 C -0.0003(3) 0.3587(2) -0.02033(17) 0.0381(7) Uani 1 1 d . . . H41 H 0.0048 0..3916 -0.0634 0.046 Uiso 1 1 calc R . . C42 C 0.0903(3) 0.3130(2) 0.01975(18) 0.0373(6) Uani 1 1 d . . . H42 H 0.175(4) 0.317(4) 0.008(3) 0.106(17) Uiso 1 1 d . . . N1 N 0.35385(19) 0.10068(18) 0.19759(14) 0.0334(5) Uani 1 1 d . . . N2 N -0.0929(2) 0.3584(2) -0.00142(14) 0.0408(6) Uani 1 1 d . . . C43 C 0.9365(2) -0.0175(2) 0.14859(18) 0.0371(7) Uani 1 1 d . . . C44 C 0.9805(2) -0.0054(2) 0.23439(19) 0.0341(6) Uani 1 1 d . . . H44 H 0.963(2) 0.0146(19) 0.2724(16) 0.010(6) Uiso 1 1 d . . . C45 C 1.0724(2) -0.0507(2) 0.27229(17) 0.0319(6) Uani 1 1 d . . . H45 H 1.095(2) -0.048(2) 0.3259(19) 0.029(8) Uiso 1 1 d . . . C46 C 1.0787(3) -0.1163(3) 0.14835(19) 0.0468(8) Uani 1 1 d . . . H46 H 1.110(4) -0.164(3) 0.110(3) 0.075(13) Uiso 1 1 d . . . C47 C 0.9884(3) -0.0744(3) 0.1060(2) 0.0512(9) Uani 1 1 d . . . H47 H 0.953(4) -0.084(3) 0.044(3) 0.073(13) Uiso 1 1 d . . . C48 C 0.8374(3) 0.0301(2) 0.10536(17) 0.0386(7) Uani 1 1 d . . . C49 C 0.7522(3) 0.0426(2) 0.1356(2) 0.0408(7) Uani 1 1 d . . . H49 H 0.7539 0.0209 0.1846 0.049 Uiso 1 1 calc R . . C50 C 0.6617(3) 0.0887(3) 0.09194(19) 0.0409(7) Uani 1 1 d . . . H50 H 0.6045 0.0969 0.1137 0.049 Uiso 1 1 calc R . . C51 C 0.7350(3) 0.1058(3) -0.0080(2) 0.0578(10) Uani 1 1 d . . . H51 H 0.7301 0.1274 -0.0576 0.101(17) Uiso 1 1 calc R . . C52 C 0.8270(3) 0.0603(4) 0.0297(2) 0.0590(10) Uani 1 1 d . . . H52 H 0.900(4) 0.057(3) 0.001(2) 0.072(13) Uiso 1 1 d . . . N3 N 1.1216(2) -0.10573(19) 0.22989(14) 0.0334(5) Uani 1 1 d . . . N4 N 0.6528(2) 0.1207(2) 0.02276(15) 0.0422(6) Uani 1 1 d . . . Ru1 Ru 0.00650(4) 0.41722(3) 0.41333(3) 0.02964(14) Uani 0.50 1 d P . . C53 C -0.0039(6) 0.4162(4) 0.2866(4) 0.0393(14) Uani 0.50 1 d PD . . C54 C 0.0936(4) 0.3756(4) 0.3288(3) 0.0284(11) Uani 0.50 1 d PD . . C55 C 0.0566(5) 0.2878(5) 0.3575(4) 0.0292(13) Uani 0.50 1 d PD . . C56 C -0.0672(4) 0.2756(4) 0.3324(3) 0.0329(12) Uani 0.50 1 d PD . . C57 C -0.0999(5) 0.3577(5) 0.2916(3) 0.0360(13) Uani 0.50 1 d PD . . C58 C -0.0087(11) 0.5605(9) 0.4724(8) 0.052(4) Uani 0.50 1 d PD . . C59 C 0.1046(10) 0.5361(7) 0.5103(6) 0.0284(18) Uani 0.50 1 d PD . . C60 C 0.0958(7) 0.4498(5) 0.5465(4) 0.0407(15) Uani 0.50 1 d PD . . C61 C -0.0202(13) 0.4121(9) 0.5347(8) 0.050(3) Uani 0.50 1 d PD . . C62 C -0.0796(13) 0.4797(13) 0.4868(11) 0.075(6) Uani 0.50 1 d PD . . C63 C 0.0035(13) 0.5077(9) 0.2475(7) 0.076(4) Uani 0.50 1 d P . . C64 C 0.2148(5) 0.4136(5) 0.3379(4) 0.0465(17) Uani 0.50 1 d P . . C65 C 0.1383(9) 0.2194(7) 0.4041(5) 0.043(2) Uani 0.50 1 d P . . C66 C -0.1417(6) 0.1957(5) 0.3518(4) 0.0512(19) Uani 0.50 1 d P . . C67 C -0.2316(7) 0.3562(10) 0.2563(6) 0.091(5) Uani 0.50 1 d P . . C68 C -0.0497(15) 0.6466(8) 0.4252(6) 0.113(5) Uani 0.50 1 d P . . C69 C 0.2091(11) 0.6086(8) 0.5114(9) 0.104(5) Uani 0.50 1 d P . . C70 C 0.1972(7) 0.4074(8) 0.5944(4) 0.071(3) Uani 0.50 1 d P . . C71 C -0.0590(8) 0.3213(6) 0.5672(5) 0.060(2) Uani 0.50 1 d P . . C72 C -0.2182(8) 0.4683(12) 0.4621(6) 0.096(4) Uani 0.50 1 d P . . O9 O 0.0769(8) 0.5190(7) 0.8042(9) 0.149(5) Uani 0.50 1 d P . . C73 C -0.0363(10) 0.4874(10) 0.7885(9) 0.089(3) Uani 0.50 1 d P . . C74 C -0.1063(10) 0.5340(10) 0.7186(7) 0.104(4) Uani 0.50 1 d P . . O10 O -0.0193(7) 0.7776(6) 0.7014(5) 0.103(3) Uani 0.50 1 d P . . C75 C -0.0747(15) 0.7524(11) 0.6159(8) 0.101(5) Uani 0.50 1 d P . . C76 C -0.1970(12) 0.7431(13) 0.5873(9) 0.111(6) Uani 0.50 1 d P . . O11 O 0.1895(13) 0.6846(10) 0.7699(7) 0.188(6) Uani 0.50 1 d P . . O12 O 0.2763(15) 0.7620(16) 0.7060(15) 0.348(14) Uani 0.50 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0301(12) 0.0192(11) 0.0131(9) -0.0003(8) 0.0059(9) 0.0078(9) O1 0.0313(9) 0.0232(9) 0.0182(8) -0.0061(7) 0.0076(7) 0.0028(7) C2 0.0255(11) 0.0213(11) 0.0123(9) 0.0007(8) 0.0047(8) 0.0076(9) O2 0.0400(10) 0.0210(9) 0.0172(8) -0.0016(7) 0.0138(7) 0.0055(8) C3 0.0259(11) 0.0188(11) 0.0155(10) -0.0008(8) 0.0029(8) 0.0062(9) O3 0.0329(10) 0.0271(10) 0.0197(8) -0.0040(7) 0.0067(7) 0.0128(8) C4 0.0302(12) 0.0191(11) 0.0126(9) -0.0012(8) 0.0053(8) 0.0074(9) O4 0.0332(10) 0.0358(11) 0.0158(8) -0.0064(7) 0.0046(7) 0.0104(8) C5 0.0294(12) 0.0201(11) 0.0137(10) 0.0027(8) 0.0071(8) 0.0098(9) O5 0.0541(12) 0.0197(9) 0.0258(9) -0.0081(8) 0.0221(9) -0.0036(8) C6 0.0291(12) 0.0172(11) 0.0139(9) 0.0006(8) 0.0054(8) 0.0080(9) O6 0.0501(12) 0.0314(11) 0.0301(10) -0.0118(8) 0.0279(9) -0.0072(9) C7 0.0337(13) 0.0185(11) 0.0166(10) 0.0001(9) 0.0098(9) 0.0061(10) O7 0.0375(10) 0.0314(10) 0.0144(8) -0.0038(7) 0.0026(7) 0.0139(8) C8 0.0526(18) 0.0205(13) 0.0218(12) 0.0041(10) 0.0153(12) 0.0092(13) O8 0.0321(9) 0.0295(10) 0.0182(8) -0.0043(7) 0.0040(7) 0.0156(8) C9 0.0308(12) 0.0163(11) 0.0182(10) -0.0003(9) 0.0097(9) 0.0033(9) C10 0.0299(12) 0.0156(11) 0.0178(10) -0.0004(8) 0.0102(9) 0.0010(9) C11 0.0257(11) 0.0197(11) 0.0188(10) -0.0030(9) 0.0098(9) 0.0024(9) C12 0.0261(12) 0.0257(13) 0.0199(11) -0.0014(9) 0.0082(9) 0.0063(10) C13 0.0245(11) 0.0227(12) 0.0168(10) -0.0047(9) 0.0078(9) 0.0000(9) C14 0.0262(11) 0.0172(11) 0.0208(11) -0.0013(9) 0.0122(9) 0.0005(9) C15 0.0310(12) 0.0185(11) 0.0188(10) -0.0031(9) 0.0112(9) 0.0010(9) C16 0.0437(15) 0.0182(12) 0.0245(12) 0.0011(10) 0.0180(11) 0.0057(11) C17 0.0288(12) 0.0172(11) 0.0142(9) -0.0011(8) 0.0072(8) 0.0059(9) C18 0.0303(12) 0.0183(11) 0.0168(10) 0.0000(9) 0.0096(9) 0.0034(9) C19 0.0379(14) 0.0180(11) 0.0219(11) -0.0019(9) 0.0132(10) 0.0019(10) C20 0.0426(15) 0.0227(12) 0.0226(11) -0.0059(10) 0.0175(11) 0.0016(11) C21 0.0344(13) 0.0251(13) 0.0232(11) -0.0023(10) 0.0164(10) 0.0021(10) C22 0.0274(12) 0.0182(11) 0.0157(10) -0.0011(8) 0.0079(8) 0.0039(9) C23 0.0277(12) 0.0170(11) 0.0168(10) 0.0010(8) 0.0100(9) 0.0046(9) C24 0.0273(12) 0.0227(13) 0.0259(12) -0.0007(10) 0.0091(10) 0.0068(10) C25 0.0237(11) 0.0179(11) 0.0177(10) 0.0021(8) 0.0075(9) 0.0041(9) C26 0.0245(11) 0.0172(11) 0.0166(10) 0.0014(8) 0.0095(8) 0.0040(9) C27 0.0288(12) 0.0194(11) 0.0150(10) -0.0021(8) 0.0078(9) 0.0036(9) C28 0.0253(12) 0.0224(12) 0.0177(10) -0.0015(9) 0.0044(9) 0.0071(9) C29 0.0252(11) 0.0189(11) 0.0170(10) -0.0013(8) 0.0074(9) 0.0065(9) C30 0.0242(11) 0.0177(11) 0.0146(9) -0.0004(8) 0.0075(8) 0.0025(9) C31 0.0251(11) 0.0224(12) 0.0148(10) -0.0023(9) 0.0048(8) 0.0055(9) C32 0.0262(13) 0.0425(17) 0.0203(12) -0.0049(11) 0.0045(10) 0.0095(12) C33 0.0253(13) 0.0415(16) 0.0332(14) 0.0110(12) 0.0088(10) 0.0021(11) C34 0.0342(14) 0.0398(16) 0.0309(13) 0.0090(12) 0.0124(11) 0.0078(12) C35 0.0386(15) 0.0385(16) 0.0310(14) 0.0092(12) 0.0111(12) 0.0078(12) C36 0.0276(14) 0.059(2) 0.0408(16) 0.0134(15) 0.0130(12) 0.0094(14) C37 0.0302(14) 0.067(2) 0.0366(15) 0.0231(15) 0.0132(12) 0.0110(14) C38 0.0270(13) 0.0472(17) 0.0316(14) 0.0101(12) 0.0074(11) 0.0064(12) C39 0.0395(18) 0.112(4) 0.048(2) 0.039(2) 0.0221(15) 0.026(2) C40 0.0384(18) 0.122(4) 0.055(2) 0.041(2) 0.0215(16) 0.031(2) C41 0.0477(17) 0.0387(16) 0.0316(14) 0.0106(12) 0.0151(12) 0.0115(13) C42 0.0349(15) 0.0410(17) 0.0394(15) 0.0112(13) 0.0151(12) 0.0070(12) N1 0.0315(12) 0.0337(13) 0.0320(12) 0.0050(10) 0.0073(9) 0.0041(10) N2 0.0361(13) 0.0573(17) 0.0280(12) 0.0087(11) 0.0068(10) 0.0137(12) C43 0.0285(14) 0.0436(17) 0.0354(14) 0.0123(13) 0.0030(11) 0.0078(12) C44 0.0317(14) 0.0330(15) 0.0356(15) 0.0018(12) 0.0091(12) 0.0065(11) C45 0.0256(13) 0.0344(15) 0.0302(13) 0.0029(11) 0.0035(10) 0.0032(11) C46 0.0477(18) 0.062(2) 0.0298(14) 0.0054(14) 0.0092(13) 0.0177(16) C47 0.0518(19) 0.071(2) 0.0290(15) 0.0038(15) 0.0083(14) 0.0211(18) C48 0.0359(15) 0.0448(17) 0.0299(14) 0.0014(12) 0.0045(11) 0.0097(13) C49 0.0407(16) 0.0435(18) 0.0431(16) 0.0111(14) 0.0181(13) 0.0105(14) C50 0.0347(15) 0.0503(19) 0.0431(16) 0.0101(14) 0.0186(13) 0.0098(14) C51 0.051(2) 0.095(3) 0.0353(17) 0.0240(18) 0.0165(15) 0.026(2) C52 0.0473(19) 0.099(3) 0.0367(17) 0.0177(19) 0.0145(15) 0.026(2) N3 0.0322(12) 0.0369(13) 0.0288(11) 0.0030(10) 0.0073(9) 0.0072(10) N4 0.0394(14) 0.0516(16) 0.0317(12) 0.0036(11) 0.0053(10) 0.0140(12) Ru1 0.0266(2) 0.0335(3) 0.0295(2) -0.00217(17) 0.01390(17) 0.00096(17) C53 0.060(4) 0.029(3) 0.037(3) 0.009(2) 0.022(3) 0.021(3) C54 0.028(3) 0.028(3) 0.032(3) -0.001(2) 0.017(2) 0.002(2) C55 0.026(3) 0.034(4) 0.027(3) 0.002(2) 0.010(2) 0.001(2) C56 0.032(3) 0.039(3) 0.027(2) -0.007(2) 0.015(2) -0.006(2) C57 0.029(3) 0.058(4) 0.029(3) 0.006(3) 0.015(2) 0.025(3) C58 0.085(11) 0.047(7) 0.043(5) 0.014(5) 0.035(6) 0.044(7) C59 0.031(5) 0.030(3) 0.027(3) -0.006(3) 0.018(3) 0.002(3) C60 0.059(5) 0.037(4) 0.026(3) -0.005(3) 0.016(3) 0.010(3) C61 0.062(6) 0.054(7) 0.028(4) -0.004(4) 0.016(4) -0.006(5) C62 0.034(6) 0.113(13) 0.072(8) -0.031(8) 0.031(5) -0.012(7) C63 0.116(10) 0.073(7) 0.075(7) 0.047(6) 0.059(7) 0.053(7) C64 0.036(3) 0.043(3) 0.064(4) -0.020(3) 0.037(3) -0.013(3) C65 0.057(5) 0.050(5) 0.027(3) 0.019(3) 0.007(4) 0.037(4) C66 0.044(3) 0.050(4) 0.058(4) -0.024(3) 0.038(3) -0.028(3) C67 0.035(4) 0.139(11) 0.068(6) -0.060(6) -0.017(4) 0.062(6) C68 0.242(17) 0.075(7) 0.075(6) 0.044(6) 0.092(9) 0.100(10) C69 0.114(9) 0.061(6) 0.154(12) -0.036(7) 0.100(9) -0.032(6) C70 0.058(5) 0.104(7) 0.036(4) -0.009(4) -0.005(3) 0.039(5) C71 0.085(6) 0.049(4) 0.052(4) 0.002(3) 0.040(4) -0.006(4) C72 0.045(5) 0.161(12) 0.065(6) -0.042(7) 0.005(4) 0.047(6) O9 0.087(6) 0.096(7) 0.256(14) 0.036(8) 0.048(8) 0.010(5) C73 0.072(7) 0.084(8) 0.099(9) 0.017(7) 0.007(6) 0.024(6) C74 0.083(7) 0.118(10) 0.095(8) 0.013(7) 0.015(6) -0.003(7) O10 0.130(6) 0.113(6) 0.079(5) 0.001(4) 0.044(5) 0.061(5) C75 0.146(14) 0.090(11) 0.052(8) -0.022(7) 0.030(8) 0.000(10) C76 0.077(8) 0.147(14) 0.096(9) -0.015(9) 0.013(8) 0.049(9) O11 0.227(14) 0.162(11) 0.117(9) 0.077(8) -0.008(9) -0.059(10) O12 0.197(16) 0.34(2) 0.47(3) -0.24(2) 0.178(19) -0.006(15) _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 C6 1.389(3) . ? C1 C2 1.396(3) . ? O1 C3 1.375(3) . ? C2 C3 1.404(3) . ? C2 C31 1.521(3) . ? O2 C5 1.368(3) . ? C3 C4 1.385(3) . ? O3 C11 1.367(3) . ? C4 C5 1.390(3) . ? O4 C13 1.376(3) . ? C5 C6 1.404(3) . ? O5 C19 1.384(3) . ? C6 C7 1.522(3) . ? O6 C21 1.372(3) . ? C7 C10 1.520(3) . ? C7 C8 1.524(3) . ? O7 C27 1.374(3) . ? O8 C29 1.366(3) . ? C9 C10 1.393(3) . ? C9 C14 1.394(3) . ? C10 C11 1.391(3) . ? C11 C12 1.395(3) . ? C12 C13 1.390(3) . ? C13 C14 1.393(3) . ? C14 C15 1.521(3) . ? C15 C18 1.523(3) . ? C15 C16 1.535(3) . ? C17 C22 1.390(3) . ? C17 C18 1.400(3) . ? C18 C19 1.396(3) . ? C19 C20 1.376(4) . ? C20 C21 1.393(4) . ? C21 C22 1.400(3) . ? C22 C23 1.525(3) . ? C23 C26 1.520(3) . ? C23 C24 1.540(3) . ? C25 C30 1.391(3) . ? C25 C26 1.396(3) . ? C26 C27 1.396(3) . ? C27 C28 1.393(3) . ? C28 C29 1.394(3) . ? C29 C30 1.400(3) . ? C30 C31 1.516(3) . ? C31 C32 1.534(3) . ? C33 C37 1.386(4) . ? C33 C34 1.401(4) . ? C33 C38 1.487(4) . ? C34 C35 1.378(4) . ? C35 N1 1.343(4) . ? C36 N1 1.328(4) . ? C36 C37 1.368(4) . ? C38 C42 1.366(4) . ? C38 C39 1.400(4) . ? C39 C40 1.379(5) . ? C40 N2 1.337(4) . ? C41 N2 1.310(4) . ? C41 C42 1.381(4) . ? C43 C47 1.373(5) . ? C43 C44 1.406(4) . ? C43 C48 1.490(4) . ? C44 C45 1.381(4) . ? C45 N3 1.332(4) . ? C46 N3 1.337(4) . ? C46 C47 1.363(5) . ? C48 C49 1.360(4) . ? C48 C52 1.397(5) . ? C49 C50 1.404(4) . ? C50 N4 1.304(4) . ? C51 N4 1.336(4) . ? C51 C52 1.381(5) . ? Ru1 C58 1.981(12) 2_566 ? Ru1 C62 1.996(17) 2_566 ? Ru1 C62 2.104(16) . ? Ru1 C57 2.125(6) . ? Ru1 C59 2.141(11) . ? Ru1 C58 2.154(11) . ? Ru1 C56 2.164(5) . ? Ru1 C55 2.168(7) . ? Ru1 C54 2.174(5) . ? Ru1 C53 2.177(6) . ? Ru1 C60 2..204(6) . ? Ru1 C61 2.263(11) . ? C53 C57 1.398(9) . ? C53 C54 1.417(8) . ? C53 C63 1.482(12) . ? C53 C74 1.503(14) 2_566 ? C53 O9 1.915(14) 2_566 ? C54 C55 1.422(8) . ? C54 C64 1.503(7) . ? C54 C74 1.567(14) 2_566 ? C55 C75 0.759(16) 2_566 ? C55 O10 1.208(10) 2_566 ? C55 C56 1.460(8) . ? C55 C65 1.553(8) . ? C55 C76 1.838(14) 2_566 ? C56 C57 1.412(8) . ? C56 C66 1.485(8) . ? C56 O10 1.602(9) 2_566 ? C56 C75 1.83(2) 2_566 ? C57 O11 1.300(12) 2_566 ? C57 C67 1.567(9) . ? C58 C61 0.541(15) 2_566 ? C58 C60 1.025(14) 2_566 ? C58 C62 1.32(3) 2_566 ? C58 C62 1.425(15) . ? C58 C59 1.457(13) . ? C58 C68 1.538(14) . ? C58 C59 1.789(19) 2_566 ? C58 Ru1 1.981(12) 2_566 ? C58 C58 1.98(2) 2_566 ? C58 C71 2.013(15) 2_566 ? C59 C62 0.38(2) 2_566 ? C59 C72 1.364(14) 2_566 ? C59 C60 1.393(12) . ? C59 C61 1.41(2) 2_566 ? C59 C69 1.540(15) . ? C59 C58 1.789(19) 2_566 ? C59 Ru1 2.319(11) 2_566 ? C60 C58 1.025(14) 2_566 ? C60 C62 1.17(2) 2_566 ? C60 C61 1.430(13) . ? C60 C70 1.496(11) . ? C60 C68 1.556(14) 2_566 ? C60 C72 1.845(17) 2_566 ? C60 Ru1 2.497(7) 2_566 ? C61 C58 0.541(15) 2_566 ? C61 C68 1.332(19) 2_566 ? C61 C59 1.41(2) 2_566 ? C61 C62 1.418(16) . ? C61 C71 1.501(13) . ? C61 C62 1.963(18) 2_566 ? C61 Ru1 2.352(13) 2_566 ? C62 C59 0.38(2) 2_566 ? C62 C60 1.17(2) 2_566 ? C62 C58 1.32(3) 2_566 ? C62 C72 1.639(18) . ? C62 C62 1.90(3) 2_566 ? C62 C69 1.915(17) 2_566 ? C62 C61 1.963(18) 2_566 ? C62 Ru1 1.996(17) 2_566 ? C63 C73 0.862(14) 2_566 ? C63 O9 1.106(16) 2_566 ? C63 C74 1.445(17) 2_566 ? C64 C74 1.685(15) 2_566 ? C65 C76 0.806(16) 2_566 ? C65 C75 0.909(17) 2_566 ? C66 O12 1.86(2) 2_566 ? C67 O11 0.98(2) 2_566 ? C68 C71 1.345(17) 2_566 ? C68 C61 1.332(19) 2_566 ? C68 C60 1.556(14) 2_566 ? C68 C70 1.821(19) 2_566 ? C69 C72 1.184(17) 2_566 ? C69 C62 1.915(17) 2_566 ? C70 C68 1.821(19) 2_566 ? C71 C68 1.345(17) 2_566 ? C71 C58 2.013(15) 2_566 ? C72 C69 1.184(17) 2_566 ? C72 C59 1.364(14) 2_566 ? C72 C60 1.845(17) 2_566 ? O9 C63 1.106(16) 2_566 ? O9 C73 1.367(15) . ? O9 C53 1.915(14) 2_566 ? C73 C63 0.862(14) 2_566 ? C73 C74 1.504(17) . ? C74 C63 1.445(17) 2_566 ? C74 C53 1.503(14) 2_566 ? C74 C54 1.567(14) 2_566 ? C74 C64 1.685(15) 2_566 ? O10 C55 1.208(10) 2_566 ? O10 C75 1.415(14) . ? O10 C56 1.602(9) 2_566 ? C75 C55 0.759(16) 2_566 ? C75 C65 0.909(17) 2_566 ? C75 C76 1.442(19) . ? C75 C56 1.83(2) 2_566 ? C75 Ru1 2.596(17) 2_566 ? C76 C65 0.806(16) 2_566 ? C76 C55 1.838(14) 2_566 ? O11 C67 0.98(2) 2_566 ? O11 C57 1.300(12) 2_566 ? O12 C66 1.86(2) 2_566 ? 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 C6 C1 C2 123.7(2) . . ? C1 C2 C3 116.9(2) . . ? C1 C2 C31 123.1(2) . . ? C3 C2 C31 120.0(2) . . ? O1 C3 C4 121.7(2) . . ? O1 C3 C2 117.3(2) . . ? C4 C3 C2 121.0(2) . . ? C3 C4 C5 120.4(2) . . ? O2 C5 C4 122.4(2) . . ? O2 C5 C6 117.0(2) . . ? C4 C5 C6 120.6(2) . . ? C1 C6 C5 117.4(2) . . ? C1 C6 C7 123.3(2) . . ? C5 C6 C7 119.3(2) . . ? C10 C7 C6 113.21(19) . . ? C10 C7 C8 113.4(2) . . ? C6 C7 C8 109.9(2) . . ? C10 C9 C14 124.3(2) . . ? C11 C10 C9 116.8(2) . . ? C11 C10 C7 120.1(2) . . ? C9 C10 C7 123.1(2) . . ? O3 C11 C10 118.3(2) . . ? O3 C11 C12 120.7(2) . . ? C10 C11 C12 121.0(2) . . ? C13 C12 C11 120.0(2) . . ? O4 C13 C12 120.6(2) . . ? O4 C13 C14 118.2(2) . . ? C12 C13 C14 121.2(2) . . ? C13 C14 C9 116.7(2) . . ? C13 C14 C15 120.1(2) . . ? C9 C14 C15 123.2(2) . . ? C14 C15 C18 112.1(2) . . ? C14 C15 C16 113.08(19) . . ? C18 C15 C16 110.4(2) . . ? C22 C17 C18 123.2(2) . . ? C19 C18 C17 117.0(2) . . ? C19 C18 C15 120.1(2) . . ? C17 C18 C15 122.9(2) . . ? C20 C19 O5 120.9(2) . . ? C20 C19 C18 121.7(2) . . ? O5 C19 C18 117.4(2) . . ? C19 C20 C21 119.7(2) . . ? O6 C21 C20 120.9(2) . . ? O6 C21 C22 118.1(2) . . ? C20 C21 C22 121.0(2) . . ? C17 C22 C21 117.3(2) . . ? C17 C22 C23 123.5(2) . . ? C21 C22 C23 119.2(2) . . ? C26 C23 C22 113.4(2) . . ? C26 C23 C24 112.78(19) . . ? C22 C23 C24 110.0(2) . . ? C30 C25 C26 124.2(2) . . ? C27 C26 C25 116.9(2) . . ? C27 C26 C23 119.92(19) . . ? C25 C26 C23 123.2(2) . . ? O7 C27 C28 120.0(2) . . ? O7 C27 C26 118.8(2) . . ? C28 C27 C26 121.2(2) . . ? C27 C28 C29 119.9(2) . . ? O8 C29 C28 120.3(2) . . ? O8 C29 C30 118.69(19) . . ? C28 C29 C30 121.0(2) . . ? C25 C30 C29 116.9(2) . . ? C25 C30 C31 123.7(2) . . ? C29 C30 C31 119.4(2) . . ? C30 C31 C2 112.12(19) . . ? C30 C31 C32 113.2(2) . . ? C2 C31 C32 110.4(2) . . ? C37 C33 C34 116.5(3) . . ? C37 C33 C38 121.3(3) . . ? C34 C33 C38 122.2(3) . . ? C35 C34 C33 119.1(3) . . ? N1 C35 C34 124.0(3) . . ? N1 C36 C37 124.2(3) . . ? C36 C37 C33 120.2(3) . . ? C42 C38 C39 116.5(3) . . ? C42 C38 C33 120.9(3) . . ? C39 C38 C33 122.6(3) . . ? C40 C39 C38 119.2(3) . . ? N2 C40 C39 123.5(3) . . ? N2 C41 C42 124.0(3) . . ? C38 C42 C41 120.1(3) . . ? C36 N1 C35 116.1(3) . . ? C41 N2 C40 116.5(3) . . ? C47 C43 C44 117.7(3) . . ? C47 C43 C48 121.1(3) . . ? C44 C43 C48 121.2(3) . . ? C45 C44 C43 119.6(3) . . ? N3 C45 C44 121.9(3) . . ? N3 C46 C47 124.3(3) . . ? C46 C47 C43 118.9(3) . . ? C49 C48 C52 117.4(3) . . ? C49 C48 C43 122.2(3) . . ? C52 C48 C43 120.4(3) . . ? C48 C49 C50 119.2(3) . . ? N4 C50 C49 124.1(3) . . ? N4 C51 C52 123.8(3) . . ? C51 C52 C48 118.8(3) . . ? C45 N3 C46 117.7(3) . . ? C50 N4 C51 116.6(3) . . ? C58 Ru1 C62 42.0(5) 2_566 2_566 ? C58 Ru1 C62 37.6(7) 2_566 . ? C62 Ru1 C62 55.3(7) 2_566 . ? C58 Ru1 C57 143.0(4) 2_566 . ? C62 Ru1 C57 157.4(6) 2_566 . ? C62 Ru1 C57 114.1(5) . . ? C58 Ru1 C59 51.3(5) 2_566 . ? C62 Ru1 C59 9.7(6) 2_566 . ? C62 Ru1 C59 63.8(5) . . ? C57 Ru1 C59 154.2(3) . . ? C58 Ru1 C58 57.1(6) 2_566 . ? C62 Ru1 C58 36.9(7) 2_566 . ? C62 Ru1 C58 39.1(4) . . ? C57 Ru1 C58 121.3(4) . . ? C59 Ru1 C58 39.7(4) . . ? C58 Ru1 C56 122.9(4) 2_566 . ? C62 Ru1 C56 162.7(6) 2_566 . ? C62 Ru1 C56 120.3(4) . . ? C57 Ru1 C56 38.4(2) . . ? C59 Ru1 C56 166.6(3) . . ? C58 Ru1 C56 151.5(4) . . ? C58 Ru1 C55 125.2(4) 2_566 . ? C62 Ru1 C55 135.2(6) 2_566 . ? C62 Ru1 C55 150.7(5) . . ? C57 Ru1 C55 64.8(2) . . ? C59 Ru1 C55 130.7(3) . . ? C58 Ru1 C55 168.3(4) . . ? C56 Ru1 C55 39.4(2) . . ? C58 Ru1 C54 148.3(4) 2_566 . ? C62 Ru1 C54 122.5(4) 2_566 . ? C62 Ru1 C54 170.5(5) . . ? C57 Ru1 C54 64.19(19) . . ? C59 Ru1 C54 113.3(4) . . ? C58 Ru1 C54 132.8(4) . . ? C56 Ru1 C54 64.73(19) . . ? C55 Ru1 C54 38.2(2) . . ? C58 Ru1 C53 170.9(3) 2_566 . ? C62 Ru1 C53 132.3(5) 2_566 . ? C62 Ru1 C53 134.9(6) . . ? C57 Ru1 C53 37.9(2) . . ? C59 Ru1 C53 123.6(3) . . ? C58 Ru1 C53 113.9(4) . . ? C56 Ru1 C53 63.8(2) . . ? C55 Ru1 C53 63.8(2) . . ? C54 Ru1 C53 38.0(2) . . ? C58 Ru1 C60 27.7(4) 2_566 . ? C62 Ru1 C60 31.9(6) 2_566 . ? C62 Ru1 C60 62.0(5) . . ? C57 Ru1 C60 167.1(3) . . ? C59 Ru1 C60 37.4(3) . . ? C58 Ru1 C60 64.5(4) . . ? C56 Ru1 C60 131.0(2) . . ? C55 Ru1 C60 111.9(3) . . ? C54 Ru1 C60 121.8(3) . . ? C53 Ru1 C60 153.6(3) . . ? C58 Ru1 C61 12.5(5) 2_566 . ? C62 Ru1 C61 54.5(5) 2_566 . ? C62 Ru1 C61 37.7(4) . . ? C57 Ru1 C61 131.8(4) . . ? C59 Ru1 C61 63.8(4) . . ? C58 Ru1 C61 65.5(5) . . ? C56 Ru1 C61 110.8(3) . . ? C55 Ru1 C61 119.1(4) . . ? C54 Ru1 C61 150.6(4) . . ? C53 Ru1 C61 168.8(4) . . ? C60 Ru1 C61 37.3(3) . . ? C57 C53 C54 108.5(5) . . ? C57 C53 C63 129.0(8) . . ? C54 C53 C63 122.5(8) . . ? C57 C53 C74 172.1(7) . 2_566 ? C54 C53 C74 64.8(6) . 2_566 ? C63 C53 C74 57.9(8) . 2_566 ? C57 C53 O9 99.0(5) . 2_566 ? C54 C53 O9 146.9(6) . 2_566 ? C63 C53 O9 35.2(6) . 2_566 ? C74 C53 O9 86.1(6) 2_566 2_566 ? C57 C53 Ru1 69.0(3) . . ? C54 C53 Ru1 70.9(3) . . ? C63 C53 Ru1 124.7(6) . . ? C74 C53 Ru1 111.0(6) 2_566 . ? O9 C53 Ru1 138.4(5) 2_566 . ? C53 C54 C55 108.0(5) . . ? C53 C54 C64 126.7(6) . . ? C55 C54 C64 125.2(5) . . ? C53 C54 C74 60.2(6) . 2_566 ? C55 C54 C74 166.6(6) . 2_566 ? C64 C54 C74 66.6(6) . 2_566 ? C53 C54 Ru1 71.1(3) . . ? C55 C54 Ru1 70.7(4) . . ? C64 C54 Ru1 126.6(4) . . ? C74 C54 Ru1 108.5(6) 2_566 . ? C75 C55 O10 88.9(12) 2_566 2_566 ? C75 C55 C54 145.8(15) 2_566 . ? O10 C55 C54 106.0(7) 2_566 . ? C75 C55 C56 106.4(15) 2_566 . ? O10 C55 C56 73.1(5) 2_566 . ? C54 C55 C56 107.3(5) . . ? C75 C55 C65 23.5(14) 2_566 . ? O10 C55 C65 90.3(7) 2_566 . ? C54 C55 C65 123.7(6) . . ? C56 C55 C65 129.0(7) . . ? C75 C55 C76 47.8(15) 2_566 2_566 ? O10 C55 C76 103.4(8) 2_566 2_566 ? C54 C55 C76 98.3(7) . 2_566 ? C56 C55 C76 154.1(8) . 2_566 ? C65 C55 C76 25.8(6) . 2_566 ? C75 C55 Ru1 116.3(13) 2_566 . ? O10 C55 Ru1 139.9(6) 2_566 . ? C54 C55 Ru1 71.1(4) . . ? C56 C55 Ru1 70.1(3) . . ? C65 C55 Ru1 125.5(5) . . ? C76 C55 Ru1 116.7(6) 2_566 . ? C57 C56 C55 106.5(5) . . ? C57 C56 C66 127.5(6) . . ? C55 C56 C66 125.9(6) . . ? C57 C56 O10 110.9(5) . 2_566 ? C55 C56 O10 46.2(4) . 2_566 ? C66 C56 O10 107.9(6) . 2_566 ? C57 C56 C75 129.8(6) . 2_566 ? C55 C56 C75 23.5(5) . 2_566 ? C66 C56 C75 102.4(7) . 2_566 ? O10 C56 C75 48.2(5) 2_566 2_566 ? C57 C56 Ru1 69.3(3) . . ? C55 C56 Ru1 70.5(3) . . ? C66 C56 Ru1 122.1(4) . . ? O10 C56 Ru1 114.9(4) 2_566 . ? C75 C56 Ru1 80.7(4) 2_566 . ? O11 C57 C53 125.7(8) 2_566 . ? O11 C57 C56 102.5(7) 2_566 . ? C53 C57 C56 109.6(5) . . ? O11 C57 C67 38.7(9) 2_566 . ? C53 C57 C67 135.6(8) . . ? C56 C57 C67 114.5(8) . . ? O11 C57 Ru1 160.4(8) 2_566 . ? C53 C57 Ru1 73.1(4) . . ? C56 C57 Ru1 72.3(3) . . ? C67 C57 Ru1 125.3(4) . . ? C61 C58 C60 129(3) 2_566 2_566 ? C61 C58 C62 89(3) 2_566 2_566 ? C60 C58 C62 141.9(16) 2_566 2_566 ? C61 C58 C62 173(3) 2_566 . ? C60 C58 C62 54.2(11) 2_566 . ? C62 C58 C62 87.7(11) 2_566 . ? C61 C58 C59 74(3) 2_566 . ? C60 C58 C59 156.3(12) 2_566 . ? C62 C58 C59 14.6(10) 2_566 . ? C62 C58 C59 102.2(9) . . ? C61 C58 C68 58(3) 2_566 . ? C60 C58 C68 71.6(10) 2_566 . ? C62 C58 C68 146.5(16) 2_566 . ? C62 C58 C68 125.8(12) . . ? C59 C58 C68 132.0(12) . . ? C61 C58 C59 176(3) 2_566 2_566 ? C60 C58 C59 50.9(7) 2_566 2_566 ? C62 C58 C59 90.9(12) 2_566 2_566 ? C62 C58 C59 3.6(9) . 2_566 ? C59 C58 C59 105.5(9) . 2_566 ? C68 C58 C59 122.5(11) . 2_566 ? C61 C58 Ru1 115(3) 2_566 2_566 ? C60 C58 Ru1 88.4(8) 2_566 2_566 ? C62 C58 Ru1 76.2(10) 2_566 2_566 ? C62 C58 Ru1 69.6(8) . 2_566 ? C59 C58 Ru1 83.3(7) . 2_566 ? C68 C58 Ru1 112.8(7) . 2_566 ? C59 C58 Ru1 69.0(6) 2_566 2_566 ? C61 C58 C58 134(3) 2_566 2_566 ? C60 C58 C58 96.0(12) 2_566 2_566 ? C62 C58 C58 45.9(8) 2_566 2_566 ? C62 C58 C58 41.8(8) . 2_566 ? C59 C58 C58 60.4(8) . 2_566 ? C68 C58 C58 167.6(14) . 2_566 ? C59 C58 C58 45.1(6) 2_566 2_566 ? Ru1 C58 C58 65.8(7) 2_566 2_566 ? C61 C58 C71 16(2) 2_566 2_566 ? C60 C58 C71 113.4(10) 2_566 2_566 ? C62 C58 C71 104.7(12) 2_566 2_566 ? C62 C58 C71 167.1(10) . 2_566 ? C59 C58 C71 90.1(7) . 2_566 ? C68 C58 C71 41.9(8) . 2_566 ? C59 C58 C71 164.2(10) 2_566 2_566 ? Ru1 C58 C71 116.5(7) 2_566 2_566 ? C58 C58 C71 150.4(10) 2_566 2_566 ? C61 C58 Ru1 105(3) 2_566 . ? C60 C58 Ru1 97.0(9) 2_566 . ? C62 C58 Ru1 65.0(9) 2_566 . ? C62 C58 Ru1 68.6(8) . . ? C59 C58 Ru1 69.7(6) . . ? C68 C58 Ru1 122.9(8) . . ? C59 C58 Ru1 71.3(5) 2_566 . ? Ru1 C58 Ru1 122.9(6) 2_566 . ? C58 C58 Ru1 57.0(6) 2_566 . ? C71 C58 Ru1 112.9(6) 2_566 . ? C62 C59 C72 131(4) 2_566 2_566 ? C62 C59 C60 48(4) 2_566 . ? C72 C59 C60 84.0(9) 2_566 . ? C62 C59 C61 84(4) 2_566 2_566 ? C72 C59 C61 144.9(13) 2_566 2_566 ? C60 C59 C61 130.9(11) . 2_566 ? C62 C59 C58 62(4) 2_566 . ? C72 C59 C58 166.6(12) 2_566 . ? C60 C59 C58 109.3(9) . . ? C61 C59 C58 21.7(6) 2_566 . ? C62 C59 C69 171(4) 2_566 . ? C72 C59 C69 47.7(8) 2_566 . ? C60 C59 C69 131.3(10) . . ? C61 C59 C69 97.7(10) 2_566 . ? C58 C59 C69 119.1(9) . . ? C62 C59 C58 14(4) 2_566 2_566 ? C72 C59 C58 118.8(11) 2_566 2_566 ? C60 C59 C58 34.8(6) . 2_566 ? C61 C59 C58 96.1(11) 2_566 2_566 ? C58 C59 C58 74.5(9) . 2_566 ? C69 C59 C58 165.9(11) . 2_566 ? C62 C59 Ru1 63(4) 2_566 . ? C72 C59 Ru1 113.8(7) 2_566 . ? C60 C59 Ru1 73.8(5) . . ? C61 C59 Ru1 80.1(8) 2_566 . ? C58 C59 Ru1 70.7(6) . . ? C69 C59 Ru1 125.8(7) . . ? C58 C59 Ru1 59.7(6) 2_566 . ? C62 C59 Ru1 52(4) 2_566 2_566 ? C72 C59 Ru1 127..7(7) 2_566 2_566 ? C60 C59 Ru1 80.3(6) . 2_566 ? C61 C59 Ru1 69.9(7) 2_566 2_566 ? C58 C59 Ru1 58.1(6) . 2_566 ? C69 C59 Ru1 121.0(7) . 2_566 ? C58 C59 Ru1 61.7(5) 2_566 2_566 ? Ru1 C59 Ru1 109.0(5) . 2_566 ? C58 C60 C62 80.6(13) 2_566 2_566 ? C58 C60 C59 94.2(10) 2_566 . ? C62 C60 C59 13.8(11) 2_566 . ? C58 C60 C61 17.0(11) 2_566 . ? C62 C60 C61 97.5(9) 2_566 . ? C59 C60 C61 111.2(9) . . ? C58 C60 C70 142.8(10) 2_566 . ? C62 C60 C70 136.5(11) 2_566 . ? C59 C60 C70 122.9(9) . . ? C61 C60 C70 125.8(9) . . ? C58 C60 C68 69.7(9) 2_566 2_566 ? C62 C60 C68 150.3(13) 2_566 2_566 ? C59 C60 C68 163.9(10) . 2_566 ? C61 C60 C68 52.8(9) . 2_566 ? C70 C60 C68 73.2(8) . 2_566 ? C58 C60 C72 141.4(10) 2_566 2_566 ? C62 C60 C72 61.1(9) 2_566 2_566 ? C59 C60 C72 47.3(6) . 2_566 ? C61 C60 C72 158.5(8) . 2_566 ? C70 C60 C72 75.7(7) . 2_566 ? C68 C60 C72 148.6(9) 2_566 2_566 ? C58 C60 Ru1 63.9(8) 2_566 . ? C62 C60 Ru1 64.2(9) 2_566 . ? C59 C60 Ru1 68.8(5) . . ? C61 C60 Ru1 73.6(5) . . ? C70 C60 Ru1 126.8(5) . . ? C68 C60 Ru1 101.5(6) 2_566 . ? C72 C60 Ru1 93.8(4) 2_566 . ? C58 C60 Ru1 58.9(8) 2_566 2_566 ? C62 C60 Ru1 57.1(8) 2_566 2_566 ? C59 C60 Ru1 66.3(5) . 2_566 ? C61 C60 Ru1 67.4(6) . 2_566 ? C70 C60 Ru1 131.9(4) . 2_566 ? C68 C60 Ru1 104.5(6) 2_566 2_566 ? C72 C60 Ru1 99.1(4) 2_566 2_566 ? Ru1 C60 Ru1 101.0(3) . 2_566 ? C58 C61 C68 102(3) 2_566 2_566 ? C58 C61 C59 84(3) 2_566 2_566 ? C68 C61 C59 173.1(13) 2_566 2_566 ? C58 C61 C62 69(3) 2_566 . ? C68 C61 C62 170.2(13) 2_566 . ? C59 C61 C62 15.4(9) 2_566 . ? C58 C61 C60 34(2) 2_566 . ? C68 C61 C60 68.5(11) 2_566 . ? C59 C61 C60 117.8(9) 2_566 . ? C62 C61 C60 102.5(9) . . ? C58 C61 C71 158(3) 2_566 . ? C68 C61 C71 56.3(9) 2_566 . ? C59 C61 C71 117.4(12) 2_566 . ? C62 C61 C71 132.8(12) . . ? C60 C61 C71 124.7(12) . . ? C58 C61 C62 5(2) 2_566 2_566 ? C68 C61 C62 104.8(14) 2_566 2_566 ? C59 C61 C62 81.6(10) 2_566 2_566 ? C62 C61 C62 66.3(11) . 2_566 ? C60 C61 C62 36.3(7) . 2_566 ? C71 C61 C62 160.9(15) . 2_566 ? C58 C61 Ru1 53(2) 2_566 . ? C68 C61 Ru1 106.9(9) 2_566 . ? C59 C61 Ru1 74.3(7) 2_566 . ? C62 C61 Ru1 65.1(8) . . ? C60 C61 Ru1 69.1(5) . . ? C71 C61 Ru1 127.8(8) . . ? C62 C61 Ru1 55.8(6) 2_566 . ? C58 C61 Ru1 62(2) 2_566 2_566 ? C68 C61 Ru1 121.8(10) 2_566 2_566 ? C59 C61 Ru1 63.7(6) 2_566 2_566 ? C62 C61 Ru1 57.8(9) . 2_566 ? C60 C61 Ru1 78.5(6) . 2_566 ? C71 C61 Ru1 127.4(8) . 2_566 ? C62 C61 Ru1 57.5(6) 2_566 2_566 ? Ru1 C61 Ru1 103.9(4) . 2_566 ? C59 C62 C60 119(5) 2_566 2_566 ? C59 C62 C58 103(5) 2_566 2_566 ? C60 C62 C58 137.6(14) 2_566 2_566 ? C59 C62 C58 163(5) 2_566 . ? C60 C62 C58 45.2(7) 2_566 . ? C58 C62 C58 92.3(11) 2_566 . ? C59 C62 C61 81(4) 2_566 . ? C60 C62 C61 159.7(13) 2_566 . ? C58 C62 C61 22.4(7) 2_566 . ? C58 C62 C61 114.6(11) . . ? C59 C62 C72 39(4) 2_566 . ? C60 C62 C72 80.2(14) 2_566 . ? C58 C62 C72 142.0(16) 2_566 . ? C58 C62 C72 125.3(14) . . ? C61 C62 C72 119.6(13) . . ? C59 C62 C62 151(5) 2_566 2_566 ? C60 C62 C62 89.2(11) 2_566 2_566 ? C58 C62 C62 48.4(9) 2_566 2_566 ? C58 C62 C62 44.0(8) . 2_566 ? C61 C62 C62 70.7(11) . 2_566 ? C72 C62 C62 168.6(18) . 2_566 ? C59 C62 C69 7(4) 2_566 2_566 ? C60 C62 C69 118.0(15) 2_566 2_566 ? C58 C62 C69 104.5(15) 2_566 2_566 ? C58 C62 C69 163.2(14) . 2_566 ? C61 C62 C69 82.2(11) . 2_566 ? C72 C62 C69 37.9(7) . 2_566 ? C62 C62 C69 152.9(18) 2_566 2_566 ? C59 C62 C61 164(5) 2_566 2_566 ? C60 C62 C61 46.2(7) 2_566 2_566 ? C58 C62 C61 91.4(11) 2_566 2_566 ? C58 C62 C61 1.8(8) . 2_566 ? C61 C62 C61 113.7(11) . 2_566 ? C72 C62 C61 126.4(16) . 2_566 ? C62 C62 C61 43.0(7) 2_566 2_566 ? C69 C62 C61 164.1(16) 2_566 2_566 ? C59 C62 Ru1 108(4) 2_566 2_566 ? C60 C62 Ru1 83.9(9) 2_566 2_566 ? C58 C62 Ru1 78.1(11) 2_566 2_566 ? C58 C62 Ru1 68.5(7) . 2_566 ? C61 C62 Ru1 85.3(10) . 2_566 ? C72 C62 Ru1 109.0(9) . 2_566 ? C62 C62 Ru1 65.3(9) 2_566 2_566 ? C69 C62 Ru1 114.4(9) 2_566 2_566 ? C61 C62 Ru1 69.7(6) 2_566 2_566 ? C59 C62 Ru1 120(4) 2_566 . ? C60 C62 Ru1 95.0(10) 2_566 . ? C58 C62 Ru1 66.1(8) 2_566 . ? C58 C62 Ru1 72.4(7) . . ? C61 C62 Ru1 77.2(8) . . ? C72 C62 Ru1 125.3(10) . . ? C62 C62 Ru1 59.5(8) 2_566 . ? C69 C62 Ru1 114.4(9) 2_566 . ? C61 C62 Ru1 70.6(6) 2_566 . ? Ru1 C62 Ru1 124.7(7) 2_566 . ? C73 C63 O9 87.1(16) 2_566 2_566 ? C73 C63 C74 76.8(14) 2_566 2_566 ? O9 C63 C74 134.2(13) 2_566 2_566 ? C73 C63 C53 122.7(15) 2_566 . ? O9 C63 C53 94.4(13) 2_566 . ? C74 C63 C53 61.8(7) 2_566 . ? C54 C64 C74 58.5(5) . 2_566 ? C76 C65 C75 114.3(18) 2_566 2_566 ? C76 C65 C55 97.3(15) 2_566 . ? C75 C65 C55 19.5(11) 2_566 . ? C56 C66 O12 94.6(9) . 2_566 ? O11 C67 C57 55.8(8) 2_566 . ? C71 C68 C61 68.2(10) 2_566 2_566 ? C71 C68 C58 88.3(10) 2_566 . ? C61 C68 C58 20.1(7) 2_566 . ? C71 C68 C60 126.8(10) 2_566 2_566 ? C61 C68 C60 58.7(6) 2_566 2_566 ? C58 C68 C60 38.7(5) . 2_566 ? C71 C68 C70 173.6(9) 2_566 2_566 ? C61 C68 C70 110.5(10) 2_566 2_566 ? C58 C68 C70 90.6(9) . 2_566 ? C60 C68 C70 51.9(7) 2_566 2_566 ? C72 C69 C59 58.3(7) 2_566 . ? C72 C69 C62 58.3(9) 2_566 2_566 ? C59 C69 C62 1.7(9) . 2_566 ? C60 C70 C68 54.9(5) . 2_566 ? C68 C71 C61 55.5(8) 2_566 . ? C68 C71 C58 49.8(6) 2_566 2_566 ? C61 C71 C58 5.7(9) . 2_566 ? C69 C72 C59 74.0(9) 2_566 2_566 ? C69 C72 C62 83.8(10) 2_566 . ? C59 C72 C62 10.0(9) 2_566 . ? C69 C72 C60 122.3(9) 2_566 2_566 ? C59 C72 C60 48.7(6) 2_566 2_566 ? C62 C72 C60 38.7(8) . 2_566 ? C63 O9 C73 39.0(7) 2_566 . ? C63 O9 C53 50.5(9) 2_566 2_566 ? C73 O9 C53 76.5(9) . 2_566 ? C63 C73 O9 53.9(14) 2_566 . ? C63 C73 C74 69.3(14) 2_566 . ? O9 C73 C74 110.0(14) . . ? C63 C74 C53 60.3(7) 2_566 2_566 ? C63 C74 C73 33.9(6) 2_566 . ? C53 C74 C73 87.4(9) 2_566 . ? C63 C74 C54 115.0(10) 2_566 2_566 ? C53 C74 C54 54.9(5) 2_566 2_566 ? C73 C74 C54 139.6(10) . 2_566 ? C63 C74 C64 167.3(11) 2_566 2_566 ? C53 C74 C64 109.8(9) 2_566 2_566 ? C73 C74 C64 158.8(12) . 2_566 ? C54 C74 C64 54.9(5) 2_566 2_566 ? C55 O10 C75 32.5(7) 2_566 . ? C55 O10 C56 60.7(5) 2_566 2_566 ? C75 O10 C56 74.2(8) . 2_566 ? C55 C75 C65 137(2) 2_566 2_566 ? C55 C75 O10 58.6(11) 2_566 . ? C65 C75 O10 114.4(13) 2_566 . ? C55 C75 C76 109.3(19) 2_566 . ? C65 C75 C76 30.7(11) 2_566 . ? O10 C75 C76 116.0(12) . . ? C55 C75 C56 50.1(13) 2_566 2_566 ? C65 C75 C56 167.2(14) 2_566 2_566 ? O10 C75 C56 57.6(7) . 2_566 ? C76 C75 C56 159.4(15) . 2_566 ? C55 C75 Ru1 48.5(12) 2_566 2_566 ? C65 C75 Ru1 137.2(11) 2_566 2_566 ? O10 C75 Ru1 101.2(10) . 2_566 ? C76 C75 Ru1 112.3(10) . 2_566 ? C56 C75 Ru1 55.3(5) 2_566 2_566 ? C65 C76 C75 35.1(10) 2_566 . ? C65 C76 C55 56.9(10) 2_566 2_566 ? C75 C76 C55 22.9(7) . 2_566 ? C67 O11 C57 85.5(12) 2_566 2_566 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1 H1D O3 0.72(3) 2.07(4) 2.785(2) 171(4) 2_676 O2 H2D O8 0.65(3) 2.11(4) 2.758(3) 175(4) 2_676 O5 H5D O7 0.74(4) 2.05(4) 2.767(3) 164(4) 2_665 O6 H6D O4 0.79(4) 1.96(4) 2.722(3) 162(4) 2_665 O8 H8D N1 0.83(4) 1.91(4) 2.723(3) 165(4) 1_565 O4 H4D N2 0.78(4) 1.96(4) 2.730(3) 167(4) 2_565 O3 H3D N3 0.89(4) 1.85(4) 2.729(3) 168(4) 1_465 O7 H7D N4 0.85(4) 1.87(4) 2.707(3) 169(4) 2_665 _diffrn_measured_fraction_theta_max 0.899 _diffrn_reflns_theta_full 29.14 _diffrn_measured_fraction_theta_full 0.899 _refine_diff_density_max 0.904 _refine_diff_density_min -0.879 _refine_diff_density_rms 0.096 #====END data_decamethylruthenocene _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common decamethylruthenocene _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H30 Ru' _chemical_formula_weight 371.51 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' '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 P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 7.6071(12) _cell_length_b 14.478(2) _cell_length_c 16.481(3) _cell_angle_alpha 90.00 _cell_angle_beta 99.056(3) _cell_angle_gamma 90.00 _cell_volume 1792.5(5) _cell_formula_units_Z 4 _cell_measurement_temperature 90(1) _cell_measurement_reflns_used 120 _cell_measurement_theta_min 2.50 _cell_measurement_theta_max 25.0 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.377 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 776 _exptl_absorpt_coefficient_mu 0.868 _exptl_absorpt_correction_type gaussian _exptl_absorpt_correction_T_min 0.85837 _exptl_absorpt_correction_T_max 0.91285 _exptl_absorpt_process_details XPREP _exptl_special_details ; The Gaussian face-indexed absorption correction was done with SHELX-XPREP. ; _diffrn_ambient_temperature 90(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'SMART 1k CCD diffractometer' _diffrn_measurement_method 'oscillation around \w and \f' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12966 _diffrn_reflns_av_R_equivalents 0.0732 _diffrn_reflns_av_sigmaI/netI 0.0581 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.88 _diffrn_reflns_theta_max 27.44 _reflns_number_total 3745 _reflns_number_gt 2932 _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 SHELX-XP _computing_publication_material SHELX-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^)+(0.0254P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3745 _refine_ls_number_parameters 310 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0434 _refine_ls_R_factor_gt 0.0293 _refine_ls_wR_factor_ref 0.0672 _refine_ls_wR_factor_gt 0.0627 _refine_ls_goodness_of_fit_ref 0.992 _refine_ls_restrained_S_all 0.992 _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 0.43192(3) 0.738992(12) 0.851929(12) 0.01788(8) Uani 1 1 d . . . C1 C 0.5959(4) 0.69850(16) 0.76142(16) 0.0225(6) Uani 1 1 d . . . C2 C 0.5918(4) 0.79702(16) 0.76670(16) 0.0220(6) Uani 1 1 d . . . C3 C 0.6668(4) 0.82301(17) 0.84843(18) 0.0262(6) Uani 1 1 d . . . C4 C 0.7175(4) 0.74024(17) 0.89346(17) 0.0255(6) Uani 1 1 d . . . C5 C 0.6741(4) 0.66416(17) 0.83980(17) 0.0244(6) Uani 1 1 d . . . C6 C 0.1601(4) 0.68991(17) 0.81946(16) 0.0230(6) Uani 1 1 d . . . C7 C 0.1582(4) 0.78791(18) 0.82787(17) 0.0253(6) Uani 1 1 d . . . C8 C 0.2338(4) 0.81051(18) 0.91033(18) 0.0284(7) Uani 1 1 d . . . C9 C 0.2821(4) 0.72570(19) 0.95290(16) 0.0269(6) Uani 1 1 d . . . C10 C 0.2370(4) 0.65136(18) 0.89699(17) 0.0275(6) Uani 1 1 d . . . C11 C 0.5387(5) 0.6430(2) 0.6860(2) 0.0316(7) Uani 1 1 d . . . C12 C 0.5259(5) 0.8615(2) 0.6983(2) 0.0330(7) Uani 1 1 d . . . C13 C 0.6960(6) 0.9192(2) 0.8804(3) 0.0429(9) Uani 1 1 d . . . C14 C 0.8102(5) 0.7346(3) 0.9803(2) 0.0436(8) Uani 1 1 d . . . C15 C 0.7116(5) 0.5651(2) 0.8606(3) 0.0362(8) Uani 1 1 d . . . C16 C 0.0871(5) 0.6376(2) 0.7439(2) 0.0319(7) Uani 1 1 d . . . C17 C 0.0826(5) 0.8538(2) 0.7623(2) 0.0336(7) Uani 1 1 d . . . C18 C 0.2485(6) 0.9048(2) 0.9476(3) 0.0450(9) Uani 1 1 d . . . C19 C 0.3588(6) 0.7174(3) 1.0417(2) 0.0438(8) Uani 1 1 d . . . C20 C 0.2565(5) 0.5512(2) 0.9168(3) 0.0399(9) Uani 1 1 d . . . H11A H 0.435(4) 0.6725(18) 0.6503(18) 0.030(8) Uiso 1 1 d . . . H12A H 0.429(5) 0.833(2) 0.658(2) 0.037(9) Uiso 1 1 d . . . H13A H 0.814(5) 0.939(2) 0.878(2) 0.048(10) Uiso 1 1 d . . . H14A H 0.780(5) 0.783(2) 1.008(2) 0.053(11) Uiso 1 1 d . . . H15A H 0.697(5) 0.556(2) 0.912(2) 0.043(10) Uiso 1 1 d . . . H16A H 0.141(4) 0.577(2) 0.7400(18) 0.036(9) Uiso 1 1 d . . . H17A H 0.107(5) 0.838(2) 0.711(2) 0.046(10) Uiso 1 1 d . . . H18A H 0.262(6) 0.947(3) 0.908(2) 0.057(12) Uiso 1 1 d . . . H19A H 0.428(6) 0.769(2) 1.057(2) 0.056(11) Uiso 1 1 d . . . H20A H 0.279(5) 0.511(2) 0.871(2) 0.052(11) Uiso 1 1 d . . . H11B H 0.632(5) 0.635(2) 0.656(2) 0.042(10) Uiso 1 1 d . . . H12B H 0.616(5) 0.878(2) 0.667(2) 0.050(10) Uiso 1 1 d . . . H13B H 0.618(5) 0.960(2) 0.850(2) 0.051(11) Uiso 1 1 d . . . H14B H 0.930(6) 0.736(2) 0.979(2) 0.043(10) Uiso 1 1 d . . . H15B H 0.824(5) 0.547(2) 0.853(2) 0.047(10) Uiso 1 1 d . . . H16B H 0.105(4) 0.669(2) 0.694(2) 0.039(9) Uiso 1 1 d . . . H17B H -0.048(5) 0.8556(19) 0.7577(19) 0.040(9) Uiso 1 1 d . . . H18B H 0.139(6) 0.920(2) 0.969(2) 0.064(12) Uiso 1 1 d . . . H19B H 0.271(5) 0.722(2) 1.075(2) 0.044(10) Uiso 1 1 d . . . H20B H 0.345(5) 0.544(2) 0.958(2) 0.051(11) Uiso 1 1 d . . . H11C H 0.504(5) 0.580(3) 0.698(2) 0.063(11) Uiso 1 1 d . . . H12C H 0.483(4) 0.917(2) 0.720(2) 0.044(9) Uiso 1 1 d . . . H13C H 0.691(5) 0.922(2) 0.937(2) 0.053(11) Uiso 1 1 d . . . H14C H 0.775(6) 0.684(3) 1.005(3) 0.082(15) Uiso 1 1 d . . . H15C H 0.635(5) 0.523(2) 0.826(2) 0.055(11) Uiso 1 1 d . . . H16C H -0.038(5) 0.6309(19) 0.7405(19) 0.037(9) Uiso 1 1 d . . . H17C H 0.136(4) 0.917(2) 0.7758(18) 0.037(8) Uiso 1 1 d . . . H18C H 0.356(5) 0.912(2) 0.988(2) 0.053(11) Uiso 1 1 d . . . H19C H 0.431(6) 0.668(3) 1.050(2) 0.060(12) Uiso 1 1 d . . . H20C H 0.154(6) 0.529(2) 0.939(2) 0.065(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 0.01828(12) 0.01600(11) 0.01875(12) -0.00033(8) 0.00104(8) -0.00061(8) C1 0.0229(15) 0.0207(12) 0.0237(15) -0.0007(10) 0.0034(12) 0.0018(10) C2 0.0213(15) 0.0194(12) 0.0258(15) 0.0030(11) 0.0060(12) -0.0017(10) C3 0.0251(16) 0.0220(12) 0.0314(17) -0.0054(11) 0.0045(13) -0.0045(11) C4 0.0185(15) 0.0313(14) 0.0266(15) -0.0001(11) 0.0030(11) -0.0014(11) C5 0.0206(16) 0.0253(13) 0.0280(16) 0.0034(11) 0.0055(12) 0.0034(10) C6 0.0182(15) 0.0280(13) 0.0225(15) 0.0033(11) 0.0022(12) -0.0026(11) C7 0.0205(15) 0.0261(13) 0.0297(16) 0.0018(11) 0.0049(12) 0.0023(10) C8 0.0230(17) 0.0326(14) 0.0295(17) -0.0055(12) 0.0038(13) 0.0014(12) C9 0.0182(15) 0.0434(15) 0.0195(14) 0.0000(12) 0.0047(11) 0.0002(12) C10 0.0248(17) 0.0326(14) 0.0252(16) 0.0083(12) 0.0040(13) -0.0053(11) C11 0.037(2) 0.0296(15) 0.0291(18) -0.0070(13) 0.0081(16) -0.0008(13) C12 0.039(2) 0.0244(14) 0.0373(19) 0.0090(13) 0.0110(17) 0.0041(13) C13 0.042(2) 0.0302(17) 0.058(3) -0.0179(16) 0.013(2) -0.0156(15) C14 0.027(2) 0.072(3) 0.0294(18) -0.0031(18) -0.0027(14) -0.0026(18) C15 0.040(2) 0.0282(15) 0.042(2) 0.0123(14) 0.0103(18) 0.0128(14) C16 0.030(2) 0.0332(16) 0.0299(18) -0.0013(13) -0.0036(14) -0.0078(13) C17 0.0257(19) 0.0326(16) 0.042(2) 0.0076(14) 0.0037(16) 0.0078(13) C18 0.038(2) 0.045(2) 0.054(3) -0.0215(18) 0.012(2) 0.0032(16) C19 0.033(2) 0.072(3) 0.0257(18) -0.0024(17) 0.0043(15) -0.0044(19) C20 0.033(2) 0.0375(17) 0.046(2) 0.0177(16) -0.0033(18) -0.0104(14) _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 C2 2.167(3) . ? Ru1 C9 2.168(3) . ? Ru1 C10 2.169(3) . ? Ru1 C3 2.170(3) . ? Ru1 C1 2.171(3) . ? Ru1 C6 2.172(3) . ? Ru1 C8 2.174(3) . ? Ru1 C4 2.172(3) . ? Ru1 C5 2.173(3) . ? Ru1 C7 2.176(3) . ? C1 C5 1.424(4) . ? C1 C2 1.430(4) . ? C1 C11 1.487(4) . ? C2 C3 1.428(4) . ? C2 C12 1.489(4) . ? C3 C4 1.430(4) . ? C3 C13 1.493(4) . ? C4 C5 1.419(4) . ? C4 C14 1.495(4) . ? C5 C15 1.491(4) . ? C6 C7 1.426(4) . ? C6 C10 1.432(4) . ? C6 C16 1.488(4) . ? C7 C8 1.428(4) . ? C7 C17 1.487(4) . ? C8 C9 1.433(4) . ? C8 C18 1.494(4) . ? C9 C10 1.423(4) . ? C9 C19 1.492(4) . ? C10 C20 1.488(4) . ? 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 C2 Ru1 C9 161.48(9) . . ? C2 Ru1 C10 158.78(11) . . ? C9 Ru1 C10 38.31(10) . . ? C2 Ru1 C3 38.45(10) . . ? C9 Ru1 C3 127.20(11) . . ? C10 Ru1 C3 161.26(11) . . ? C2 Ru1 C1 38.49(10) . . ? C9 Ru1 C1 158.72(10) . . ? C10 Ru1 C1 125.10(10) . . ? C3 Ru1 C1 64.42(10) . . ? C2 Ru1 C6 125.22(10) . . ? C9 Ru1 C6 64.23(10) . . ? C10 Ru1 C6 38.53(10) . . ? C3 Ru1 C6 158.87(10) . . ? C1 Ru1 C6 111.73(10) . . ? C2 Ru1 C8 126.96(10) . . ? C9 Ru1 C8 38.54(10) . . ? C10 Ru1 C8 64.43(11) . . ? C3 Ru1 C8 112.08(10) . . ? C1 Ru1 C8 161.16(10) . . ? C6 Ru1 C8 64.26(10) . . ? C2 Ru1 C4 64.25(10) . . ? C9 Ru1 C4 112.28(11) . . ? C10 Ru1 C4 126.89(10) . . ? C3 Ru1 C4 38.46(10) . . ? C1 Ru1 C4 64.17(10) . . ? C6 Ru1 C4 161.11(10) . . ? C8 Ru1 C4 125.80(11) . . ? C2 Ru1 C5 64.11(10) . . ? C9 Ru1 C5 125.57(10) . . ? C10 Ru1 C5 112.01(10) . . ? C3 Ru1 C5 64.12(10) . . ? C1 Ru1 C5 38.27(10) . . ? C6 Ru1 C5 127.01(10) . . ? C8 Ru1 C5 159.20(11) . . ? C4 Ru1 C5 38.11(10) . . ? C2 Ru1 C7 111.98(10) . . ? C9 Ru1 C7 64.24(10) . . ? C10 Ru1 C7 64.33(10) . . ? C3 Ru1 C7 125.53(10) . . ? C1 Ru1 C7 126.85(10) . . ? C6 Ru1 C7 38.29(10) . . ? C8 Ru1 C7 38.33(10) . . ? C4 Ru1 C7 159.30(10) . . ? C5 Ru1 C7 161.12(11) . . ? C5 C1 C2 107.6(2) . . ? C5 C1 C11 126.5(2) . . ? C2 C1 C11 125.7(2) . . ? C5 C1 Ru1 70.96(16) . . ? C2 C1 Ru1 70.62(15) . . ? C11 C1 Ru1 126.6(2) . . ? C1 C2 C3 108.1(2) . . ? C1 C2 C12 126.0(2) . . ? C3 C2 C12 125.9(2) . . ? C1 C2 Ru1 70.89(15) . . ? C3 C2 Ru1 70.88(16) . . ? C12 C2 Ru1 125.3(2) . . ? C2 C3 C4 107.7(2) . . ? C2 C3 C13 126.4(3) . . ? C4 C3 C13 125.9(3) . . ? C2 C3 Ru1 70.66(15) . . ? C4 C3 Ru1 70.87(15) . . ? C13 C3 Ru1 126.2(2) . . ? C5 C4 C3 108.1(2) . . ? C5 C4 C14 125.7(3) . . ? C3 C4 C14 126.2(3) . . ? C5 C4 Ru1 70.98(16) . . ? C3 C4 Ru1 70.67(15) . . ? C14 C4 Ru1 126.8(2) . . ? C4 C5 C1 108.5(2) . . ? C4 C5 C15 125.9(3) . . ? C1 C5 C15 125.6(3) . . ? C4 C5 Ru1 70.92(15) . . ? C1 C5 Ru1 70.76(15) . . ? C15 C5 Ru1 126.4(2) . . ? C7 C6 C10 108.1(2) . . ? C7 C6 C16 125.4(2) . . ? C10 C6 C16 126.5(2) . . ? C7 C6 Ru1 71.01(15) . . ? C10 C6 Ru1 70.63(15) . . ? C16 C6 Ru1 126.0(2) . . ? C6 C7 C8 108.2(2) . . ? C6 C7 C17 125.2(3) . . ? C8 C7 C17 126.6(3) . . ? C6 C7 Ru1 70.70(15) . . ? C8 C7 Ru1 70.75(16) . . ? C17 C7 Ru1 126.2(2) . . ? C7 C8 C9 107.7(2) . . ? C7 C8 C18 126.4(3) . . ? C9 C8 C18 125.8(3) . . ? C7 C8 Ru1 70.92(16) . . ? C9 C8 Ru1 70.52(16) . . ? C18 C8 Ru1 127.3(2) . . ? C10 C9 C8 108.3(2) . . ? C10 C9 C19 126.2(3) . . ? C8 C9 C19 125.4(3) . . ? C10 C9 Ru1 70.88(16) . . ? C8 C9 Ru1 70.94(16) . . ? C19 C9 Ru1 126.0(2) . . ? C9 C10 C6 107.8(2) . . ? C9 C10 C20 126.1(3) . . ? C6 C10 C20 126.0(3) . . ? C9 C10 Ru1 70.81(16) . . ? C6 C10 Ru1 70.84(15) . . ? C20 C10 Ru1 126.5(2) . . ? _diffrn_measured_fraction_theta_max 0.915 _diffrn_reflns_theta_full 27.44 _diffrn_measured_fraction_theta_full 0.915 _refine_diff_density_max 0.392 _refine_diff_density_min -1.035 _refine_diff_density_rms 0.101 #====END