# Copyright The Royal Society of Chemistry, 1998 # CCDC Number: 186/1067 data_global # 1. SUBMISSION DETAILS _publ_contact_author ; Alfonso Casti\~neiras Departamento de Quimica Inorganica Universidad de Santiago de Compostela E-15706 Santiago de Compostela (Spain) ; _publ_contact_author_phone +34-981594636 _publ_contact_author_fax +34-981547163 _publ_contact_author_email qiac01@usc.es _publ_requested_journal ? _publ_requested_coeditor_name ? _publ_contact_letter ; Dear Dr. Bardwell, For deposition on their ESI web site, please find enclosed the data of X-ray structure analyses of the compound: [Ru(acac)2(diim)].0.25H2O With thanks in advance, Yours sincerely, Alfonso Casti\~neiras ; #======================================================================= # 3. TITLE AND AUTHOR LIST _publ_section_title ; "Chemistry of ruthenium(II) complexes of N-substituted 1,2-benzoquinone diimines. Synthesis, structure and redox properties" ; # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. loop_ _publ_author_name _publ_author_address 'Mitra, K.N.' ; Indian Association for the Cultivation of Science Department of Inorganic Chemistry Jadavpur Calcuta 700 032 India ; 'Choudhury, S.' ; Indian Association for the Cultivation of Science Department of Inorganic Chemistry Jadavpur Calcuta 700 032 India ; 'Alfonso Castineiras' ; Universidad de Santiago de Compostela Departamento de Quimica Inorganica Facultad de Farmacia E-15706 Santiago de Compostela Spain ; 'Goswami, S.' ; Indian Association for the Cultivation of Science Department of Inorganic Chemistry Jadavpur Calcuta 700 032 India ; #======================================================================= data_95sg01 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety '[Ru(acac)2(diim)].1/4H2O' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C22 H24.50 N2 O4.25 Ru' _chemical_formula_weight 486.01 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Ru' 'Ru' -1.2594 .8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' .0106 .0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' .0061 .0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'C' 'C' .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' .0000 .0000 '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 33.578(9) _cell_length_b 9.9224(15) _cell_length_c 26.354(5) _cell_angle_alpha 90.00 _cell_angle_beta 93.114(10) _cell_angle_gamma 90.00 _cell_volume 8767.8(33) _cell_formula_units_Z 16 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 4.5 _cell_measurement_theta_max 11.2 _exptl_crystal_description irregular _exptl_crystal_colour brown _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.473 _exptl_crystal_density_method ? _exptl_crystal_F_000 3976 _exptl_absorpt_coefficient_mu 0.746 _exptl_absorpt_correction_type 'DIFABS (Walker & Stuart, 1983)' _exptl_absorpt_correction_T_min 0.9285 _exptl_absorpt_correction_T_max 1.0000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoKa _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'CAD4 Enraf Nonius' _diffrn_measurement_method '\w/2\q scans' _diffrn_standards_number 2 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 120 _diffrn_standards_decay_% none _diffrn_reflns_number 13038 _diffrn_reflns_av_R_equivalents 0.1951 _diffrn_reflns_av_sigmaI/netI 0.2574 _diffrn_reflns_limit_h_min -47 _diffrn_reflns_limit_h_max 46 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_theta_min 3.10 _diffrn_reflns_theta_max 32.40 _reflns_number_total 12707 _reflns_number_observed 4813 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'CAD4 Software (Enraf Nonius, 1989)' _computing_cell_refinement 'CAD4 Software (Enraf Nonius, 1989)' _computing_data_reduction 'HELENA (Spek, 1997)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'ZORTEP (Zsolnai, 1997)' _computing_publication_material 'SHELXL-93 (Sheldrick, 1993)' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 2 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[s^2^(Fo^2^)+( 0.0362P)^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 'riding model' _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00013(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^l^3^/sin(2q)]^-1/4^' _refine_ls_number_reflns 12705 _refine_ls_number_parameters 529 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2600 _refine_ls_R_factor_obs 0.0799 _refine_ls_wR_factor_all 0.1573 _refine_ls_wR_factor_obs 0.1122 _refine_ls_goodness_of_fit_all 1.009 _refine_ls_goodness_of_fit_obs 1.207 _refine_ls_restrained_S_all 1.010 _refine_ls_restrained_S_obs 1.207 _refine_ls_shift/esd_max 0.001 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Ru1 Ru -0.00059(2) 0.64035(6) 0.15051(2) 0.0386(2) Uani 1 d . . Ru2 Ru 0.27750(2) 1.29705(6) 0.41274(2) 0.0426(2) Uani 1 d . . O11 O -0.02932(13) 0.4695(5) 0.1288(2) 0.0478(13) Uani 1 d . . O13 O 0.04066(12) 0.5326(5) 0.1952(2) 0.0431(12) Uani 1 d . . O21 O 0.03656(13) 0.5983(5) 0.0933(2) 0.0501(13) Uani 1 d . . O23 O 0.03185(14) 0.8070(5) 0.1700(2) 0.0485(13) Uani 1 d . . O41 O 0.25337(13) 1.1151(5) 0.4309(2) 0.0464(13) Uani 1 d . . O43 O 0.31556(14) 1.1998(6) 0.3658(2) 0.0558(14) Uani 1 d . . O51 O 0.31694(13) 1.2640(5) 0.4736(2) 0.0490(13) Uani 1 d . . O53 O 0.30573(13) 1.4700(5) 0.3948(2) 0.0489(13) Uani 1 d . . N31 N -0.0373(2) 0.6761(5) 0.2036(2) 0.043(2) Uani 1 d . . H31 H -0.0325(2) 0.6460(5) 0.2339(2) 0.051 Uiso 1 calc R . N36 N -0.0423(2) 0.7497(5) 0.1124(2) 0.0393(14) Uani 1 d . . N61 N 0.2411(2) 1.3933(5) 0.4540(2) 0.043(2) Uani 1 d . . H61 H 0.2460(2) 1.4026(5) 0.4861(2) 0.052 Uiso 1 calc R . N66 N 0.2332(2) 1.3373(6) 0.3606(2) 0.046(2) Uani 1 d . . C11 C -0.0213(2) 0.3531(9) 0.1466(3) 0.051(2) Uani 1 d . . C12 C 0.0103(2) 0.3213(8) 0.1813(3) 0.058(2) Uani 1 d . . H12 H 0.0123(2) 0.2313(8) 0.1909(3) 0.070 Uiso 1 calc R . C13 C 0.0388(2) 0.4058(8) 0.2031(3) 0.044(2) Uani 1 d . . C21 C 0.0669(2) 0.6634(9) 0.0841(3) 0.061(2) Uani 1 d . . C22 C 0.0800(2) 0.7810(10) 0.1077(3) 0.070(3) Uani 1 d . . H22 H 0.1029(2) 0.8200(10) 0.0960(3) 0.084 Uiso 1 calc R . C23 C 0.0624(2) 0.8460(8) 0.1469(3) 0.051(2) Uani 1 d . . C31 C -0.0697(2) 0.7478(7) 0.1920(3) 0.041(2) Uani 1 d . . C32 C -0.0998(2) 0.7780(8) 0.2253(3) 0.056(2) Uani 1 d . . H32 H -0.0976(2) 0.7490(8) 0.2589(3) 0.067 Uiso 1 calc R . C33 C -0.1318(2) 0.8494(9) 0.2080(3) 0.062(2) Uani 1 d . . H33 H -0.1515(2) 0.8717(9) 0.2300(3) 0.074 Uiso 1 calc R . C34 C -0.1357(2) 0.8908(9) 0.1567(3) 0.069(3) Uani 1 d . . H34 H -0.1583(2) 0.9386(9) 0.1455(3) 0.083 Uiso 1 calc R . C35 C -0.1075(2) 0.8628(8) 0.1234(3) 0.055(2) Uani 1 d . . H35 H -0.1109(2) 0.8910(8) 0.0897(3) 0.066 Uiso 1 calc R . C36 C -0.0729(2) 0.7910(7) 0.1398(2) 0.041(2) Uani 1 d . . C37 C -0.0414(2) 0.7822(8) 0.0597(3) 0.041(2) Uani 1 d . . C38 C -0.0462(2) 0.9140(9) 0.0423(3) 0.056(2) Uani 1 d . . H38 H -0.0499(2) 0.9834(9) 0.0653(3) 0.068 Uiso 1 calc R . C39 C -0.0453(2) 0.9418(10) -0.0083(4) 0.073(3) Uani 1 d . . H39 H -0.0490(2) 1.0296(10) -0.0200(4) 0.087 Uiso 1 calc R . C41 C 0.2599(2) 1.0032(8) 0.4078(3) 0.052(2) Uani 1 d . . C42 C 0.2855(2) 0.9854(8) 0.3695(3) 0.059(2) Uani 1 d . . H42 H 0.2849(2) 0.9015(8) 0.3537(3) 0.071 Uiso 1 calc R . C43 C 0.3127(2) 1.0803(10) 0.3514(3) 0.057(2) Uani 1 d . . C51 C 0.3360(2) 1.3599(9) 0.4958(3) 0.048(2) Uani 1 d . . C52 C 0.3411(2) 1.4883(8) 0.4751(3) 0.059(2) Uani 1 d . . H52 H 0.3545(2) 1.5509(8) 0.4961(3) 0.071 Uiso 1 calc R . C53 C 0.3287(2) 1.5329(8) 0.4272(3) 0.052(2) Uani 1 d . . C61 C 0.2085(2) 1.4445(7) 0.4311(3) 0.044(2) Uani 1 d . . C62 C 0.1782(2) 1.5197(7) 0.4552(3) 0.056(2) Uani 1 d . . H62 H 0.1812(2) 1.5414(7) 0.4896(3) 0.068 Uiso 1 calc R . C63 C 0.1450(3) 1.5586(9) 0.4267(4) 0.078(3) Uani 1 d . . H63 H 0.1246(3) 1.6038(9) 0.4421(4) 0.094 Uiso 1 calc R . C64 C 0.1413(3) 1.5310(9) 0.3743(4) 0.082(3) Uani 1 d . . H64 H 0.1186(3) 1.5608(9) 0.3559(4) 0.099 Uiso 1 calc R . C65 C 0.1694(2) 1.4630(8) 0.3495(3) 0.062(2) Uani 1 d . . H65 H 0.1662(2) 1.4482(8) 0.3147(3) 0.074 Uiso 1 calc R . C66 C 0.2039(2) 1.4145(7) 0.3778(3) 0.044(2) Uani 1 d . . C67 C 0.2303(2) 1.2795(7) 0.3105(3) 0.046(2) Uani 1 d . . C68 C 0.2608(2) 1.2935(8) 0.2786(3) 0.057(2) Uani 1 d . . H68 H 0.2833(2) 1.3437(8) 0.2887(3) 0.069 Uiso 1 calc R . C69 C 0.2583(3) 1.2333(9) 0.2315(3) 0.071(3) Uani 1 d . . H69 H 0.2792(3) 1.2439(9) 0.2100(3) 0.085 Uiso 1 calc R . C110 C -0.0488(2) 0.2430(8) 0.1268(3) 0.075(3) Uani 1 d . . H111 H -0.0688(2) 0.2808(8) 0.1035(3) 0.113 Uiso 1 calc R . H112 H -0.0615(2) 0.2017(8) 0.1546(3) 0.113 Uiso 1 calc R . H113 H -0.0338(2) 0.1765(8) 0.1096(3) 0.113 Uiso 1 calc R . C130 C 0.0723(2) 0.3492(8) 0.2375(3) 0.068(2) Uani 1 d . . H131 H 0.0894(2) 0.4213(8) 0.2495(3) 0.102 Uiso 1 calc R . H132 H 0.0874(2) 0.2856(8) 0.2190(3) 0.102 Uiso 1 calc R . H133 H 0.0613(2) 0.3049(8) 0.2660(3) 0.102 Uiso 1 calc R . C210 C 0.0919(3) 0.6035(11) 0.0425(4) 0.120(4) Uani 1 d . . H211 H 0.0795(3) 0.5226(11) 0.0294(4) 0.180 Uiso 1 calc R . H212 H 0.1182(3) 0.5828(11) 0.0566(4) 0.180 Uiso 1 calc R . H213 H 0.0938(3) 0.6676(11) 0.0154(4) 0.180 Uiso 1 calc R . C230 C 0.0814(2) 0.9770(8) 0.1671(3) 0.077(3) Uani 1 d . . H231 H 0.0663(2) 1.0115(8) 0.1942(3) 0.116 Uiso 1 calc R . H232 H 0.0816(2) 1.0421(8) 0.1402(3) 0.116 Uiso 1 calc R . H233 H 0.1083(2) 0.9596(8) 0.1797(3) 0.116 Uiso 1 calc R . C310 C -0.0391(3) 0.8379(13) -0.0421(4) 0.083(3) Uani 1 d . . H310 H -0.0383(3) 0.8563(13) -0.0767(4) 0.100 Uiso 1 calc R . C311 C -0.0342(2) 0.7099(11) -0.0252(3) 0.071(3) Uani 1 d . . H311 H -0.0297(2) 0.6412(11) -0.0482(3) 0.085 Uiso 1 calc R . C312 C -0.0358(2) 0.6802(8) 0.0257(3) 0.054(2) Uani 1 d . . H312 H -0.0330(2) 0.5916(8) 0.0369(3) 0.064 Uiso 1 calc R . C410 C 0.2372(2) 0.8842(8) 0.4268(3) 0.072(3) Uani 1 d . . H411 H 0.2207(2) 0.9129(8) 0.4534(3) 0.108 Uiso 1 calc R . H412 H 0.2557(2) 0.8172(8) 0.4398(3) 0.108 Uiso 1 calc R . H413 H 0.2208(2) 0.8467(8) 0.3994(3) 0.108 Uiso 1 calc R . C430 C 0.3410(3) 1.0338(10) 0.3125(3) 0.096(3) Uani 1 d . . H431 H 0.3577(3) 1.1076(10) 0.3035(3) 0.143 Uiso 1 calc R . H432 H 0.3261(3) 1.0024(10) 0.2828(3) 0.143 Uiso 1 calc R . H433 H 0.3573(3) 0.9619(10) 0.3265(3) 0.143 Uiso 1 calc R . C510 C 0.3544(2) 1.3274(8) 0.5480(3) 0.072(3) Uani 1 d . . H511 H 0.3482(2) 1.2360(8) 0.5566(3) 0.109 Uiso 1 calc R . H512 H 0.3439(2) 1.3873(8) 0.5725(3) 0.109 Uiso 1 calc R . H513 H 0.3828(2) 1.3382(8) 0.5480(3) 0.109 Uiso 1 calc R . C530 C 0.3424(2) 1.6697(7) 0.4106(3) 0.071(3) Uani 1 d . . H531 H 0.3316(2) 1.6877(7) 0.3768(3) 0.106 Uiso 1 calc R . H532 H 0.3710(2) 1.6713(7) 0.4109(3) 0.106 Uiso 1 calc R . H533 H 0.3333(2) 1.7371(7) 0.4333(3) 0.106 Uiso 1 calc R . C610 C 0.2260(3) 1.1586(9) 0.2154(3) 0.073(3) Uani 1 d . . H610 H 0.2249(3) 1.1171(9) 0.1837(3) 0.087 Uiso 1 calc R . C611 C 0.1954(3) 1.1461(9) 0.2468(4) 0.076(3) Uani 1 d . . H611 H 0.1730(3) 1.0965(9) 0.2359(4) 0.091 Uiso 1 calc R . C612 C 0.1966(2) 1.2060(8) 0.2951(3) 0.065(2) Uani 1 d . . H612 H 0.1754(2) 1.1968(8) 0.3161(3) 0.079 Uiso 1 calc R . O1 O 0.0000 0.9849(8) 0.2500 0.100(3) Uani 1 d S . 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 0.0383(3) 0.0392(4) 0.0385(3) -0.0020(3) 0.0036(3) -0.0026(3) Ru2 0.0430(4) 0.0440(4) 0.0406(4) -0.0031(3) -0.0007(3) 0.0081(3) O11 0.049(3) 0.046(3) 0.048(3) -0.003(3) 0.004(2) -0.005(3) O13 0.042(3) 0.039(3) 0.049(3) 0.001(3) 0.002(2) 0.004(2) O21 0.040(3) 0.061(4) 0.050(3) -0.008(3) 0.015(2) -0.008(3) O23 0.050(3) 0.043(3) 0.052(3) -0.003(3) 0.001(3) -0.007(3) O41 0.050(3) 0.041(3) 0.048(3) -0.004(3) 0.003(2) 0.004(2) O43 0.052(3) 0.057(4) 0.059(3) -0.012(3) 0.013(3) 0.011(3) O51 0.047(3) 0.045(3) 0.053(3) -0.004(3) -0.010(2) 0.007(3) O53 0.048(3) 0.045(3) 0.054(3) 0.006(3) 0.001(3) 0.006(3) N31 0.045(3) 0.044(4) 0.040(3) 0.000(3) 0.000(3) -0.002(3) N36 0.038(3) 0.039(4) 0.041(4) -0.004(3) 0.003(3) -0.008(3) N61 0.050(4) 0.039(4) 0.040(4) -0.001(3) 0.001(3) 0.007(3) N66 0.046(3) 0.042(4) 0.049(4) 0.005(3) -0.001(3) 0.000(3) C11 0.049(5) 0.053(5) 0.052(5) -0.013(5) 0.010(4) -0.004(4) C12 0.066(5) 0.039(5) 0.070(6) -0.003(4) 0.013(5) -0.002(4) C13 0.047(5) 0.040(5) 0.045(5) 0.007(4) 0.011(4) 0.005(4) C21 0.052(5) 0.066(7) 0.065(6) -0.006(5) 0.014(4) -0.007(5) C22 0.055(5) 0.082(7) 0.075(6) 0.002(6) 0.023(5) -0.030(5) C23 0.054(5) 0.039(5) 0.059(5) 0.016(4) -0.014(4) -0.013(4) C31 0.045(4) 0.034(4) 0.043(4) -0.007(3) 0.001(4) -0.004(3) C32 0.049(5) 0.078(6) 0.042(5) -0.014(4) 0.010(4) 0.001(5) C33 0.050(5) 0.078(6) 0.058(5) -0.018(5) 0.014(4) 0.008(5) C34 0.050(5) 0.075(7) 0.082(7) -0.004(5) 0.008(5) 0.027(5) C35 0.057(5) 0.054(5) 0.053(5) -0.005(4) 0.000(4) 0.013(4) C36 0.041(4) 0.045(5) 0.034(4) -0.004(4) -0.006(3) -0.001(4) C37 0.037(4) 0.045(5) 0.041(4) 0.001(4) 0.002(3) -0.004(4) C38 0.066(5) 0.058(6) 0.045(5) 0.006(4) 0.003(4) -0.005(4) C39 0.071(6) 0.074(7) 0.073(7) 0.027(6) 0.007(5) 0.004(5) C41 0.049(5) 0.046(5) 0.058(5) 0.000(4) -0.008(4) 0.009(4) C42 0.071(6) 0.050(6) 0.059(6) -0.019(4) 0.011(5) 0.007(5) C43 0.058(5) 0.062(6) 0.050(5) -0.002(5) 0.004(4) 0.023(5) C51 0.040(4) 0.055(5) 0.048(5) -0.003(4) -0.002(3) 0.007(4) C52 0.059(5) 0.047(6) 0.071(6) -0.006(5) -0.012(4) 0.000(4) C53 0.053(5) 0.044(5) 0.058(5) 0.000(4) 0.009(4) 0.011(4) C61 0.051(5) 0.039(5) 0.043(5) 0.002(4) 0.006(4) -0.001(4) C62 0.065(5) 0.047(5) 0.059(5) -0.004(4) 0.012(4) 0.015(4) C63 0.078(7) 0.067(7) 0.091(8) 0.015(6) 0.016(6) 0.037(5) C64 0.075(6) 0.078(7) 0.093(8) 0.011(6) -0.009(6) 0.038(5) C65 0.061(5) 0.063(6) 0.061(5) 0.009(5) -0.011(4) 0.019(5) C66 0.048(4) 0.041(5) 0.042(4) 0.002(4) -0.003(4) 0.004(4) C67 0.054(5) 0.040(5) 0.043(5) 0.003(4) -0.010(4) 0.005(4) C68 0.054(5) 0.067(6) 0.051(5) 0.002(5) 0.003(4) 0.001(5) C69 0.092(7) 0.078(7) 0.043(5) 0.003(5) 0.008(5) -0.006(6) C110 0.076(6) 0.051(6) 0.100(8) -0.020(5) 0.006(5) -0.018(5) C130 0.060(5) 0.062(6) 0.081(6) 0.021(5) 0.003(5) 0.001(5) C210 0.075(7) 0.163(11) 0.128(9) -0.059(9) 0.062(7) -0.050(7) C230 0.100(7) 0.054(6) 0.076(6) 0.014(5) -0.012(5) -0.031(5) C310 0.069(6) 0.129(10) 0.052(6) 0.024(7) 0.008(5) -0.001(7) C311 0.084(6) 0.088(8) 0.042(5) -0.014(5) 0.002(5) -0.002(6) C312 0.061(5) 0.056(6) 0.044(5) 0.000(4) 0.003(4) -0.003(4) C410 0.081(6) 0.059(6) 0.077(7) -0.004(5) 0.007(5) -0.002(5) C430 0.112(8) 0.090(8) 0.089(7) -0.010(6) 0.046(6) 0.033(6) C510 0.086(6) 0.069(7) 0.058(6) -0.001(5) -0.031(5) -0.003(5) C530 0.080(6) 0.047(6) 0.085(7) 0.009(5) 0.003(5) 0.000(5) C610 0.120(8) 0.052(6) 0.046(5) -0.009(5) -0.005(6) 0.002(6) C611 0.093(7) 0.059(6) 0.072(7) 0.008(6) -0.025(6) -0.022(6) C612 0.075(6) 0.060(6) 0.061(6) 0.003(5) -0.003(5) -0.008(5) O1 0.130(8) 0.044(5) 0.130(8) 0.000 0.030(6) 0.000 _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 N31 1.946(5) . y Ru1 N36 1.997(5) . y Ru1 O11 2.018(5) . y Ru1 O23 2.030(5) . y Ru1 O21 2.050(4) . y Ru1 O13 2.067(4) . y Ru2 N61 1.930(5) . y Ru2 N66 2.008(5) . y Ru2 O53 2.029(5) . y Ru2 O41 2.046(5) . y Ru2 O51 2.050(4) . y Ru2 O43 2.065(5) . y O11 C11 1.269(9) . ? O13 C13 1.277(8) . ? O21 C21 1.241(8) . ? O23 C23 1.281(8) . ? O41 C41 1.291(8) . ? O43 C43 1.247(9) . ? O51 C51 1.271(8) . ? O53 C53 1.282(8) . ? N31 C31 1.323(8) . ? N31 H31 0.86 . ? N36 C36 1.351(8) . ? N36 C37 1.429(8) . ? N61 C61 1.322(8) . ? N61 H61 0.86 . ? N66 C66 1.346(8) . ? N66 C67 1.438(8) . ? C11 C12 1.400(10) . ? C11 C110 1.506(10) . ? C12 C13 1.373(9) . ? C12 H12 0.93 . ? C13 C130 1.515(9) . ? C21 C22 1.384(11) . ? C21 C210 1.537(10) . ? C22 C23 1.377(11) . ? C22 H22 0.93 . ? C23 C230 1.532(10) . ? C31 C32 1.405(9) . ? C31 C36 1.441(9) . ? C32 C33 1.345(9) . ? C32 H32 0.93 . ? C33 C34 1.411(10) . ? C33 H33 0.93 . ? C34 C35 1.356(9) . ? C34 H34 0.93 . ? C35 C36 1.410(9) . ? C35 H35 0.93 . ? C37 C312 1.373(9) . ? C37 C38 1.392(10) . ? C38 C39 1.363(10) . ? C38 H38 0.93 . ? C39 C310 1.386(12) . ? C39 H39 0.93 . ? C41 C42 1.374(10) . ? C41 C410 1.505(10) . ? C42 C43 1.412(10) . ? C42 H42 0.93 . ? C43 C430 1.507(10) . ? C51 C52 1.400(10) . ? C51 C510 1.513(9) . ? C52 C53 1.381(10) . ? C52 H52 0.93 . ? C53 C530 1.506(10) . ? C61 C66 1.437(9) . ? C61 C62 1.438(9) . ? C62 C63 1.367(10) . ? C62 H62 0.93 . ? C63 C64 1.407(11) . ? C63 H63 0.93 . ? C64 C65 1.357(10) . ? C64 H64 0.93 . ? C65 C66 1.426(9) . ? C65 H65 0.93 . ? C67 C68 1.369(9) . ? C67 C612 1.389(10) . ? C68 C69 1.377(10) . ? C68 H68 0.93 . ? C69 C610 1.363(11) . ? C69 H69 0.93 . ? C110 H111 0.96 . ? C110 H112 0.96 . ? C110 H113 0.96 . ? C130 H131 0.96 . ? C130 H132 0.96 . ? C130 H133 0.96 . ? C210 H211 0.96 . ? C210 H212 0.96 . ? C210 H213 0.96 . ? C230 H231 0.96 . ? C230 H232 0.96 . ? C230 H233 0.96 . ? C310 C311 1.354(12) . ? C310 H310 0.93 . ? C311 C312 1.377(10) . ? C311 H311 0.93 . ? C312 H312 0.93 . ? C410 H411 0.96 . ? C410 H412 0.96 . ? C410 H413 0.96 . ? C430 H431 0.96 . ? C430 H432 0.96 . ? C430 H433 0.96 . ? C510 H511 0.96 . ? C510 H512 0.96 . ? C510 H513 0.96 . ? C530 H531 0.96 . ? C530 H532 0.96 . ? C530 H533 0.96 . ? C610 C611 1.358(11) . ? C610 H610 0.93 . ? C611 C612 1.402(11) . ? C611 H611 0.93 . ? C612 H612 0.93 . ? 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 N31 Ru1 N36 78.9(2) . . y N31 Ru1 O11 92.6(2) . . y N36 Ru1 O11 90.2(2) . . y N31 Ru1 O23 91.2(2) . . y N36 Ru1 O23 92.1(2) . . y O11 Ru1 O23 175.9(2) . . y N31 Ru1 O21 178.0(2) . . y N36 Ru1 O21 100.3(2) . . y O11 Ru1 O21 85.5(2) . . y O23 Ru1 O21 90.7(2) . . y N31 Ru1 O13 96.6(2) . . y N36 Ru1 O13 175.4(2) . . y O11 Ru1 O13 91.3(2) . . y O23 Ru1 O13 86.8(2) . . y O21 Ru1 O13 84.2(2) . . y N61 Ru2 N66 79.6(2) . . y N61 Ru2 O53 91.7(2) . . y N66 Ru2 O53 90.6(2) . . y N61 Ru2 O41 92.0(2) . . y N66 Ru2 O41 92.7(2) . . y O53 Ru2 O41 175.4(2) . . y N61 Ru2 O51 92.3(2) . . y N66 Ru2 O51 171.7(2) . . y O53 Ru2 O51 91.6(2) . . y O41 Ru2 O51 85.6(2) . . y N61 Ru2 O43 177.3(2) . . y N66 Ru2 O43 98.2(2) . . y O53 Ru2 O43 86.8(2) . . y O41 Ru2 O43 89.6(2) . . y O51 Ru2 O43 89.9(2) . . y C11 O11 Ru1 124.8(5) . . ? C13 O13 Ru1 124.4(5) . . ? C21 O21 Ru1 125.3(5) . . ? C23 O23 Ru1 124.0(5) . . ? C41 O41 Ru2 124.7(5) . . ? C43 O43 Ru2 125.9(5) . . ? C51 O51 Ru2 121.9(5) . . ? C53 O53 Ru2 121.8(5) . . ? C31 N31 Ru1 118.6(5) . . ? C31 N31 H31 120.7(4) . . ? Ru1 N31 H31 120.7(2) . . ? C36 N36 C37 120.4(6) . . ? C36 N36 Ru1 115.5(4) . . ? C37 N36 Ru1 124.1(4) . . ? C61 N61 Ru2 117.8(5) . . ? C61 N61 H61 121.1(4) . . ? Ru2 N61 H61 121.1(2) . . ? C66 N66 C67 121.4(6) . . ? C66 N66 Ru2 114.3(5) . . ? C67 N66 Ru2 124.0(5) . . ? O11 C11 C12 125.8(7) . . ? O11 C11 C110 114.7(7) . . ? C12 C11 C110 119.5(8) . . ? C13 C12 C11 128.4(8) . . ? C13 C12 H12 115.8(5) . . ? C11 C12 H12 115.8(5) . . ? O13 C13 C12 125.0(7) . . ? O13 C13 C130 114.9(7) . . ? C12 C13 C130 120.1(7) . . ? O21 C21 C22 126.4(8) . . ? O21 C21 C210 115.2(8) . . ? C22 C21 C210 118.3(8) . . ? C23 C22 C21 126.5(7) . . ? C23 C22 H22 116.8(5) . . ? C21 C22 H22 116.8(5) . . ? O23 C23 C22 127.0(7) . . ? O23 C23 C230 114.9(8) . . ? C22 C23 C230 118.1(8) . . ? N31 C31 C32 125.5(7) . . ? N31 C31 C36 113.4(6) . . ? C32 C31 C36 121.1(7) . . ? C33 C32 C31 119.1(7) . . ? C33 C32 H32 120.4(5) . . ? C31 C32 H32 120.4(4) . . ? C32 C33 C34 120.7(7) . . ? C32 C33 H33 119.7(5) . . ? C34 C33 H33 119.7(5) . . ? C35 C34 C33 121.9(7) . . ? C35 C34 H34 119.0(5) . . ? C33 C34 H34 119.0(5) . . ? C34 C35 C36 119.8(7) . . ? C34 C35 H35 120.1(5) . . ? C36 C35 H35 120.1(4) . . ? N36 C36 C35 128.9(7) . . ? N36 C36 C31 113.6(6) . . ? C35 C36 C31 117.4(7) . . ? C312 C37 C38 119.7(7) . . ? C312 C37 N36 118.7(7) . . ? C38 C37 N36 121.6(7) . . ? C39 C38 C37 120.3(8) . . ? C39 C38 H38 119.9(6) . . ? C37 C38 H38 119.9(4) . . ? C38 C39 C310 119.4(9) . . ? C38 C39 H39 120.3(6) . . ? C310 C39 H39 120.3(6) . . ? O41 C41 C42 125.9(8) . . ? O41 C41 C410 114.6(7) . . ? C42 C41 C410 119.5(8) . . ? C41 C42 C43 127.2(8) . . ? C41 C42 H42 116.4(5) . . ? C43 C42 H42 116.4(5) . . ? O43 C43 C42 124.9(8) . . ? O43 C43 C430 117.2(8) . . ? C42 C43 C430 117.9(8) . . ? O51 C51 C52 124.9(7) . . ? O51 C51 C510 115.4(7) . . ? C52 C51 C510 119.6(7) . . ? C53 C52 C51 127.5(8) . . ? C53 C52 H52 116.3(5) . . ? C51 C52 H52 116.3(5) . . ? O53 C53 C52 126.6(8) . . ? O53 C53 C530 115.2(7) . . ? C52 C53 C530 118.2(8) . . ? N61 C61 C66 114.2(6) . . ? N61 C61 C62 125.9(7) . . ? C66 C61 C62 119.9(7) . . ? C63 C62 C61 118.7(8) . . ? C63 C62 H62 120.7(5) . . ? C61 C62 H62 120.7(4) . . ? C62 C63 C64 120.7(8) . . ? C62 C63 H63 119.7(5) . . ? C64 C63 H63 119.7(5) . . ? C65 C64 C63 123.0(8) . . ? C65 C64 H64 118.5(5) . . ? C63 C64 H64 118.5(5) . . ? C64 C65 C66 118.8(8) . . ? C64 C65 H65 120.6(5) . . ? C66 C65 H65 120.6(5) . . ? N66 C66 C65 127.3(7) . . ? N66 C66 C61 113.8(6) . . ? C65 C66 C61 118.9(7) . . ? C68 C67 C612 119.9(8) . . ? C68 C67 N66 120.5(7) . . ? C612 C67 N66 119.5(7) . . ? C67 C68 C69 120.0(8) . . ? C67 C68 H68 120.0(5) . . ? C69 C68 H68 120.0(5) . . ? C610 C69 C68 121.6(9) . . ? C610 C69 H69 119.2(5) . . ? C68 C69 H69 119.2(5) . . ? C11 C110 H111 109.5(5) . . ? C11 C110 H112 109.5(5) . . ? H111 C110 H112 109.5 . . ? C11 C110 H113 109.5(4) . . ? H111 C110 H113 109.5 . . ? H112 C110 H113 109.5 . . ? C13 C130 H131 109.5(4) . . ? C13 C130 H132 109.5(4) . . ? H131 C130 H132 109.5 . . ? C13 C130 H133 109.5(4) . . ? H131 C130 H133 109.5 . . ? H132 C130 H133 109.5 . . ? C21 C210 H211 109.5(5) . . ? C21 C210 H212 109.5(5) . . ? H211 C210 H212 109.5 . . ? C21 C210 H213 109.5(6) . . ? H211 C210 H213 109.5 . . ? H212 C210 H213 109.5 . . ? C23 C230 H231 109.5(5) . . ? C23 C230 H232 109.5(4) . . ? H231 C230 H232 109.5 . . ? C23 C230 H233 109.5(4) . . ? H231 C230 H233 109.5 . . ? H232 C230 H233 109.5 . . ? C311 C310 C39 120.4(9) . . ? C311 C310 H310 119.8(6) . . ? C39 C310 H310 119.8(6) . . ? C310 C311 C312 120.7(9) . . ? C310 C311 H311 119.6(6) . . ? C312 C311 H311 119.6(6) . . ? C37 C312 C311 119.5(8) . . ? C37 C312 H312 120.2(5) . . ? C311 C312 H312 120.2(6) . . ? C41 C410 H411 109.5(4) . . ? C41 C410 H412 109.5(4) . . ? H411 C410 H412 109.5 . . ? C41 C410 H413 109.5(4) . . ? H411 C410 H413 109.5 . . ? H412 C410 H413 109.5 . . ? C43 C430 H431 109.5(5) . . ? C43 C430 H432 109.5(5) . . ? H431 C430 H432 109.5 . . ? C43 C430 H433 109.5(5) . . ? H431 C430 H433 109.5 . . ? H432 C430 H433 109.5 . . ? C51 C510 H511 109.5(5) . . ? C51 C510 H512 109.5(4) . . ? H511 C510 H512 109.5 . . ? C51 C510 H513 109.5(4) . . ? H511 C510 H513 109.5 . . ? H512 C510 H513 109.5 . . ? C53 C530 H531 109.5(5) . . ? C53 C530 H532 109.5(4) . . ? H531 C530 H532 109.5 . . ? C53 C530 H533 109.5(4) . . ? H531 C530 H533 109.5 . . ? H532 C530 H533 109.5 . . ? C611 C610 C69 118.5(8) . . ? C611 C610 H610 120.7(6) . . ? C69 C610 H610 120.7(6) . . ? C610 C611 C612 121.9(8) . . ? C610 C611 H611 119.1(6) . . ? C612 C611 H611 119.1(5) . . ? C67 C612 C611 118.1(8) . . ? C67 C612 H612 121.0(5) . . ? C611 C612 H612 121.0(5) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N31 Ru1 O11 C11 -90.4(6) . . . . ? N36 Ru1 O11 C11 -169.3(6) . . . . ? O23 Ru1 O11 C11 67.7(29) . . . . ? O21 Ru1 O11 C11 90.3(5) . . . . ? O13 Ru1 O11 C11 6.3(6) . . . . ? N31 Ru1 O13 C13 87.1(5) . . . . ? N36 Ru1 O13 C13 102.6(25) . . . . ? O11 Ru1 O13 C13 -5.6(5) . . . . ? O23 Ru1 O13 C13 178.0(5) . . . . ? O21 Ru1 O13 C13 -91.0(5) . . . . ? N31 Ru1 O21 C21 163.5(61) . . . . ? N36 Ru1 O21 C21 95.4(6) . . . . ? O11 Ru1 O21 C21 -175.3(6) . . . . ? O23 Ru1 O21 C21 3.2(6) . . . . ? O13 Ru1 O21 C21 -83.5(6) . . . . ? N31 Ru1 O23 C23 -178.3(5) . . . . ? N36 Ru1 O23 C23 -99.4(5) . . . . ? O11 Ru1 O23 C23 23.5(30) . . . . ? O21 Ru1 O23 C23 1.0(5) . . . . ? O13 Ru1 O23 C23 85.1(5) . . . . ? N61 Ru2 O41 C41 166.8(5) . . . . ? N66 Ru2 O41 C41 87.1(5) . . . . ? O53 Ru2 O41 C41 -49.4(26) . . . . ? O51 Ru2 O41 C41 -101.0(5) . . . . ? O43 Ru2 O41 C41 -11.1(5) . . . . ? N61 Ru2 O43 C43 -113.8(47) . . . . ? N66 Ru2 O43 C43 -79.6(6) . . . . ? O53 Ru2 O43 C43 -169.7(6) . . . . ? O41 Ru2 O43 C43 13.1(6) . . . . ? O51 Ru2 O43 C43 98.7(6) . . . . ? N61 Ru2 O51 C51 -66.9(5) . . . . ? N66 Ru2 O51 C51 -80.2(16) . . . . ? O53 Ru2 O51 C51 24.9(5) . . . . ? O41 Ru2 O51 C51 -158.7(5) . . . . ? O43 Ru2 O51 C51 111.6(5) . . . . ? N61 Ru2 O53 C53 72.4(5) . . . . ? N66 Ru2 O53 C53 152.0(5) . . . . ? O41 Ru2 O53 C53 -71.4(26) . . . . ? O51 Ru2 O53 C53 -19.9(5) . . . . ? O43 Ru2 O53 C53 -109.8(5) . . . . ? N36 Ru1 N31 C31 0.3(5) . . . . ? O11 Ru1 N31 C31 -89.3(5) . . . . ? O23 Ru1 N31 C31 92.2(5) . . . . ? O21 Ru1 N31 C31 -68.2(65) . . . . ? O13 Ru1 N31 C31 179.1(5) . . . . ? N31 Ru1 N36 C36 -0.1(5) . . . . ? O11 Ru1 N36 C36 92.5(5) . . . . ? O23 Ru1 N36 C36 -91.0(5) . . . . ? O21 Ru1 N36 C36 177.9(5) . . . . ? O13 Ru1 N36 C36 -15.8(27) . . . . ? N31 Ru1 N36 C37 -178.9(5) . . . . ? O11 Ru1 N36 C37 -86.3(5) . . . . ? O23 Ru1 N36 C37 90.2(5) . . . . ? O21 Ru1 N36 C37 -0.9(5) . . . . ? O13 Ru1 N36 C37 165.4(23) . . . . ? N66 Ru2 N61 C61 -4.1(5) . . . . ? O53 Ru2 N61 C61 86.1(5) . . . . ? O41 Ru2 N61 C61 -96.6(5) . . . . ? O51 Ru2 N61 C61 177.8(5) . . . . ? O43 Ru2 N61 C61 30.3(50) . . . . ? N61 Ru2 N66 C66 4.6(5) . . . . ? O53 Ru2 N66 C66 -87.0(5) . . . . ? O41 Ru2 N66 C66 96.1(5) . . . . ? O51 Ru2 N66 C66 18.1(18) . . . . ? O43 Ru2 N66 C66 -173.8(5) . . . . ? N61 Ru2 N66 C67 -169.5(6) . . . . ? O53 Ru2 N66 C67 98.8(6) . . . . ? O41 Ru2 N66 C67 -78.0(6) . . . . ? O51 Ru2 N66 C67 -156.0(13) . . . . ? O43 Ru2 N66 C67 12.0(6) . . . . ? Ru1 O11 C11 C12 -4.7(10) . . . . ? Ru1 O11 C11 C110 176.0(5) . . . . ? O11 C11 C12 C13 -0.2(13) . . . . ? C110 C11 C12 C13 179.0(7) . . . . ? Ru1 O13 C13 C12 3.2(10) . . . . ? Ru1 O13 C13 C130 -179.6(4) . . . . ? C11 C12 C13 O13 1.0(13) . . . . ? C11 C12 C13 C130 -176.1(7) . . . . ? Ru1 O21 C21 C22 -4.8(12) . . . . ? Ru1 O21 C21 C210 174.3(6) . . . . ? O21 C21 C22 C23 1.9(15) . . . . ? C210 C21 C22 C23 -177.3(9) . . . . ? Ru1 O23 C23 C22 -3.8(11) . . . . ? Ru1 O23 C23 C230 178.1(4) . . . . ? C21 C22 C23 O23 3.1(14) . . . . ? C21 C22 C23 C230 -178.9(8) . . . . ? Ru1 N31 C31 C32 177.5(5) . . . . ? Ru1 N31 C31 C36 -0.5(8) . . . . ? N31 C31 C32 C33 -178.4(7) . . . . ? C36 C31 C32 C33 -0.6(11) . . . . ? C31 C32 C33 C34 1.6(12) . . . . ? C32 C33 C34 C35 -1.2(14) . . . . ? C33 C34 C35 C36 -0.3(13) . . . . ? C37 N36 C36 C35 2.4(11) . . . . ? Ru1 N36 C36 C35 -176.4(6) . . . . ? C37 N36 C36 C31 178.8(6) . . . . ? Ru1 N36 C36 C31 -0.1(7) . . . . ? C34 C35 C36 N36 177.6(7) . . . . ? C34 C35 C36 C31 1.3(11) . . . . ? N31 C31 C36 N36 0.3(9) . . . . ? C32 C31 C36 N36 -177.7(6) . . . . ? N31 C31 C36 C35 177.2(6) . . . . ? C32 C31 C36 C35 -0.9(10) . . . . ? C36 N36 C37 C312 -128.0(7) . . . . ? Ru1 N36 C37 C312 50.7(8) . . . . ? C36 N36 C37 C38 52.1(9) . . . . ? Ru1 N36 C37 C38 -129.2(6) . . . . ? C312 C37 C38 C39 0.3(11) . . . . ? N36 C37 C38 C39 -179.8(7) . . . . ? C37 C38 C39 C310 -1.1(13) . . . . ? Ru2 O41 C41 C42 4.0(10) . . . . ? Ru2 O41 C41 C410 -177.4(5) . . . . ? O41 C41 C42 C43 7.2(13) . . . . ? C410 C41 C42 C43 -171.4(7) . . . . ? Ru2 O43 C43 C42 -7.8(11) . . . . ? Ru2 O43 C43 C430 173.4(5) . . . . ? C41 C42 C43 O43 -5.0(14) . . . . ? C41 C42 C43 C430 173.8(8) . . . . ? Ru2 O51 C51 C52 -17.7(10) . . . . ? Ru2 O51 C51 C510 163.1(5) . . . . ? O51 C51 C52 C53 -3.5(13) . . . . ? C510 C51 C52 C53 175.7(7) . . . . ? Ru2 O53 C53 C52 7.8(10) . . . . ? Ru2 O53 C53 C530 -171.2(4) . . . . ? C51 C52 C53 O53 9.4(13) . . . . ? C51 C52 C53 C530 -171.7(7) . . . . ? Ru2 N61 C61 C66 3.0(8) . . . . ? Ru2 N61 C61 C62 -179.6(6) . . . . ? N61 C61 C62 C63 -175.9(8) . . . . ? C66 C61 C62 C63 1.3(11) . . . . ? C61 C62 C63 C64 -2.8(13) . . . . ? C62 C63 C64 C65 1.5(15) . . . . ? C63 C64 C65 C66 1.4(14) . . . . ? C67 N66 C66 C65 -7.8(11) . . . . ? Ru2 N66 C66 C65 177.9(6) . . . . ? C67 N66 C66 C61 169.9(6) . . . . ? Ru2 N66 C66 C61 -4.4(8) . . . . ? C64 C65 C66 N66 174.8(8) . . . . ? C64 C65 C66 C61 -2.7(11) . . . . ? N61 C61 C66 N66 1.1(9) . . . . ? C62 C61 C66 N66 -176.5(6) . . . . ? N61 C61 C66 C65 179.0(6) . . . . ? C62 C61 C66 C65 1.4(11) . . . . ? C66 N66 C67 C68 129.8(8) . . . . ? Ru2 N66 C67 C68 -56.4(9) . . . . ? C66 N66 C67 C612 -51.8(10) . . . . ? Ru2 N66 C67 C612 122.0(6) . . . . ? C612 C67 C68 C69 -0.9(12) . . . . ? N66 C67 C68 C69 177.5(7) . . . . ? C67 C68 C69 C610 -0.2(13) . . . . ? C38 C39 C310 C311 0.5(14) . . . . ? C39 C310 C311 C312 0.8(14) . . . . ? C38 C37 C312 C311 1.0(11) . . . . ? N36 C37 C312 C311 -178.9(6) . . . . ? C310 C311 C312 C37 -1.6(13) . . . . ? C68 C69 C610 C611 1.2(14) . . . . ? C69 C610 C611 C612 -1.0(14) . . . . ? C68 C67 C612 C611 1.1(12) . . . . ? N66 C67 C612 C611 -177.3(7) . . . . ? C610 C611 C612 C67 -0.2(13) . . . . ? _refine_diff_density_max 0.623 _refine_diff_density_min -0.824 _refine_diff_density_rms 0.118 #======================================================================= #===END data_96sg01 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H20 N2 O4 Ru' _chemical_formula_weight 405.41 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Ru' 'Ru' -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 '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 16.0057(17) _cell_length_b 10.6005(12) _cell_length_c 10.3858(10) _cell_angle_alpha 90.00 _cell_angle_beta 111.069(4) _cell_angle_gamma 90.00 _cell_volume 1644.3(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 9.17 _cell_measurement_theta_max 18.34 _exptl_crystal_description prism _exptl_crystal_colour caramel _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.638 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 824 _exptl_absorpt_coefficient_mu 0.974 _exptl_absorpt_correction_type 'psi scan' _exptl_absorpt_correction_T_min 0.926 _exptl_absorpt_correction_T_max 0.976 _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 'MACH3 Enraf Nonius' _diffrn_measurement_method omega _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 120 _diffrn_standards_decay_% 0 _diffrn_reflns_number 1762 _diffrn_reflns_av_R_equivalents 0.0111 _diffrn_reflns_av_sigmaI/netI 0.0243 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 0 _diffrn_reflns_theta_min 2.36 _diffrn_reflns_theta_max 26.28 _reflns_number_total 1663 _reflns_number_gt 1469 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CAD4-Express Software (Nonius, 1994)' _computing_cell_refinement 'CAD4-Express Software (Nonius, 1994)' _computing_data_reduction 'GENHKL (Kretschmar, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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 w=1/[\s^2^(Fo^2^)+(0.0341P)^2^+0.4364P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment isotropically _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1663 _refine_ls_number_parameters 145 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0317 _refine_ls_R_factor_gt 0.0227 _refine_ls_wR_factor_ref 0.0603 _refine_ls_wR_factor_gt 0.0574 _refine_ls_goodness_of_fit_ref 1.091 _refine_ls_restrained_S_all 1.091 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.5000 0.54177(3) 0.7500 0.03573(10) Uani 1 d S . . O1 O 0.61159(11) 0.54921(16) 0.92362(16) 0.0425(4) Uani 1 d . . . O2 O 0.55496(10) 0.67852(17) 0.66136(16) 0.0429(4) Uani 1 d . . . N1 N 0.45752(13) 0.3994(2) 0.8298(2) 0.0421(5) Uani 1 d . . . C1 C 0.76601(17) 0.5520(3) 1.0506(3) 0.0458(6) Uani 1 d . . . C2 C 0.68849(14) 0.5801(2) 0.9208(2) 0.0359(5) Uani 1 d . . . C3 C 0.70364(15) 0.6355(2) 0.8104(2) 0.0421(5) Uani 1 d . . . C4 C 0.63868(14) 0.6889(2) 0.6932(2) 0.0384(5) Uani 1 d . . . C5 C 0.6693(2) 0.7684(3) 0.6002(3) 0.0519(6) Uani 1 d . . . C11 C 0.47671(14) 0.2850(2) 0.7983(2) 0.0415(5) Uani 1 d . . . C12 C 0.45712(17) 0.1669(3) 0.8474(3) 0.0544(7) Uani 1 d . . . C13 C 0.4786(2) 0.0577(3) 0.8005(3) 0.0650(8) Uani 1 d . . . H3 H 0.7622(19) 0.647(3) 0.819(3) 0.055(8) Uiso 1 d . . . H1 H 0.4346(19) 0.406(3) 0.885(3) 0.049(8) Uiso 1 d . . . H5A H 0.732(2) 0.789(3) 0.637(3) 0.068(9) Uiso 1 d . . . H12 H 0.4302(19) 0.172(3) 0.913(3) 0.056(8) Uiso 1 d . . . H1C H 0.823(3) 0.591(4) 1.055(4) 0.098(12) Uiso 1 d . . . H1A H 0.753(3) 0.580(4) 1.129(5) 0.117(15) Uiso 1 d . . . H5B H 0.641(3) 0.840(4) 0.585(4) 0.099(14) Uiso 1 d . . . H1B H 0.775(3) 0.476(4) 1.058(4) 0.085(13) Uiso 1 d . . . H13 H 0.466(2) -0.018(3) 0.831(3) 0.058(9) Uiso 1 d . . . H5C H 0.655(2) 0.728(3) 0.519(4) 0.080(11) Uiso 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 0.02901(14) 0.05714(17) 0.02501(13) 0.000 0.01452(9) 0.000 O1 0.0360(8) 0.0668(10) 0.0283(7) 0.0028(7) 0.0159(6) 0.0008(7) O2 0.0350(8) 0.0627(10) 0.0340(8) 0.0065(7) 0.0160(6) 0.0024(7) N1 0.0340(9) 0.0682(13) 0.0303(9) 0.0001(9) 0.0191(8) -0.0036(9) C1 0.0396(13) 0.0547(15) 0.0382(12) 0.0004(12) 0.0080(10) 0.0018(12) C2 0.0328(10) 0.0428(11) 0.0325(11) -0.0045(9) 0.0123(9) 0.0027(9) C3 0.0328(11) 0.0565(14) 0.0402(12) 0.0004(11) 0.0171(9) -0.0031(10) C4 0.0389(11) 0.0466(12) 0.0334(11) -0.0017(9) 0.0176(9) -0.0018(10) C5 0.0483(15) 0.0680(18) 0.0441(15) 0.0100(13) 0.0224(12) -0.0062(14) C11 0.0286(10) 0.0619(15) 0.0311(11) 0.0024(10) 0.0072(9) -0.0035(10) C12 0.0395(12) 0.0733(18) 0.0464(14) 0.0071(13) 0.0107(11) -0.0105(12) C13 0.0527(17) 0.0618(18) 0.065(2) 0.0061(14) 0.0029(14) -0.0092(13) _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 N1 1.958(2) 2_656 y Ru1 N1 1.958(2) . y Ru1 O1 2.0328(16) . y Ru1 O1 2.0328(16) 2_656 y Ru1 O2 2.0748(17) . y Ru1 O2 2.0748(17) 2_656 y O1 C2 1.284(3) . ? O2 C4 1.264(3) . ? N1 C11 1.320(3) . ? N1 H1 0.79(3) . ? C1 C2 1.498(3) . ? C1 H1C 0.99(4) . ? C1 H1A 0.96(5) . ? C1 H1B 0.82(4) . ? C2 C3 1.385(3) . ? C3 C4 1.404(3) . ? C3 H3 0.92(3) . ? C4 C5 1.492(3) . ? C5 H5A 0.96(3) . ? C5 H5B 0.86(4) . ? C5 H5C 0.90(4) . ? C11 C12 1.429(4) . ? C11 C11 1.450(5) 2_656 ? C12 C13 1.347(5) . ? C12 H12 0.93(3) . ? C13 C13 1.444(8) 2_656 ? C13 H13 0.92(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 N1 Ru1 N1 79.09(13) 2_656 . y N1 Ru1 O1 94.43(7) 2_656 . y N1 Ru1 O1 89.00(7) . . y N1 Ru1 O1 89.00(7) 2_656 2_656 y N1 Ru1 O1 94.43(7) . 2_656 y O1 Ru1 O1 175.55(10) . 2_656 y N1 Ru1 O2 94.81(8) 2_656 . y N1 Ru1 O2 173.54(8) . . y O1 Ru1 O2 89.37(6) . . y O1 Ru1 O2 87.52(6) 2_656 . y N1 Ru1 O2 173.54(8) 2_656 2_656 y N1 Ru1 O2 94.81(8) . 2_656 y O1 Ru1 O2 87.52(6) . 2_656 y O1 Ru1 O2 89.37(6) 2_656 2_656 y O2 Ru1 O2 91.36(9) . 2_656 y C2 O1 Ru1 122.22(14) . . ? C4 O2 Ru1 121.53(15) . . ? C11 N1 Ru1 117.16(15) . . ? C11 N1 H1 118(2) . . ? Ru1 N1 H1 124(2) . . ? C2 C1 H1C 115(2) . . ? C2 C1 H1A 110(3) . . ? H1C C1 H1A 108(3) . . ? C2 C1 H1B 110(3) . . ? H1C C1 H1B 106(4) . . ? H1A C1 H1B 108(4) . . ? O1 C2 C3 125.6(2) . . ? O1 C2 C1 114.8(2) . . ? C3 C2 C1 119.6(2) . . ? C2 C3 C4 126.3(2) . . ? C2 C3 H3 117.1(17) . . ? C4 C3 H3 116.1(17) . . ? O2 C4 C3 125.2(2) . . ? O2 C4 C5 116.3(2) . . ? C3 C4 C5 118.4(2) . . ? C4 C5 H5A 113.9(19) . . ? C4 C5 H5B 110(3) . . ? H5A C5 H5B 106(3) . . ? C4 C5 H5C 108(2) . . ? H5A C5 H5C 111(3) . . ? H5B C5 H5C 108(3) . . ? N1 C11 C12 128.1(2) . . ? N1 C11 C11 113.24(13) . 2_656 ? C12 C11 C11 118.70(16) . 2_656 ? C13 C12 C11 120.4(3) . . ? C13 C12 H12 124.3(18) . . ? C11 C12 H12 115.2(18) . . ? C12 C13 C13 120.80(19) . 2_656 ? C12 C13 H13 121(2) . . ? C13 C13 H13 119(2) 2_656 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Ru1 O1 C2 66.51(18) 2_656 . . . ? N1 Ru1 O1 C2 145.49(18) . . . . ? O1 Ru1 O1 C2 -73.93(17) 2_656 . . . ? O2 Ru1 O1 C2 -28.26(18) . . . . ? O2 Ru1 O1 C2 -119.65(18) 2_656 . . . ? N1 Ru1 O2 C4 -64.72(18) 2_656 . . . ? N1 Ru1 O2 C4 -45.7(7) . . . . ? O1 Ru1 O2 C4 29.67(18) . . . . ? O1 Ru1 O2 C4 -153.51(18) 2_656 . . . ? O2 Ru1 O2 C4 117.18(19) 2_656 . . . ? N1 Ru1 N1 C11 1.19(12) 2_656 . . . ? O1 Ru1 N1 C11 -93.52(17) . . . . ? O1 Ru1 N1 C11 89.32(17) 2_656 . . . ? O2 Ru1 N1 C11 -18.1(7) . . . . ? O2 Ru1 N1 C11 179.05(17) 2_656 . . . ? Ru1 O1 C2 C3 13.8(3) . . . . ? Ru1 O1 C2 C1 -166.46(17) . . . . ? O1 C2 C3 C4 12.6(4) . . . . ? C1 C2 C3 C4 -167.2(3) . . . . ? Ru1 O2 C4 C3 -16.5(3) . . . . ? Ru1 O2 C4 C5 165.87(18) . . . . ? C2 C3 C4 O2 -10.7(4) . . . . ? C2 C3 C4 C5 166.9(3) . . . . ? Ru1 N1 C11 C12 176.99(19) . . . . ? Ru1 N1 C11 C11 -3.1(3) . . . 2_656 ? N1 C11 C12 C13 177.5(3) . . . . ? C11 C11 C12 C13 -2.4(4) 2_656 . . . ? C11 C12 C13 C13 -0.3(5) . . . 2_656 ? 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 N1 H1 O1 0.79(3) 2.40(3) 3.181(2) 169(3) 5_667 _diffrn_measured_fraction_theta_max 0.472 _diffrn_reflns_theta_full 26.28 _diffrn_measured_fraction_theta_full 0.472 _refine_diff_density_max 0.223 _refine_diff_density_min -0.472 _refine_diff_density_rms 0.073