# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 #TrackingRef '- compnd_3_8b_cif.cif' # Ruthenium amino carboxylate complexes as asymmetric hydrogen transfer # catalysts # # # by Daniel Carmona, Fernando Viguri, M. Pilar Lamata, Joaquina Ferrer, # Elisa Bardaji, Fernando J. Lahoz, Pilar Garcia-Orduna and Luis A. Oro # # # Submitted to Dalton Transactions # ----------------------------------------------------------- # # Person for contact _publ_contact_author_name 'Dr. Fernando J. Lahoz' _publ_contact_author_address ; Dr. Fernando J. Lahoz Departamento de Qu\'imica Inorg\'anica - I.S.Q.C.H. Facultad de Ciencias Universidad de Zaragoza - C.S.I.C. 50009 Zaragoza, Spain ; _publ_contact_author_phone '+34 976 761147' _publ_contact_author_fax '+34 976 761187' _publ_contact_author_email lahoz@unizar.es _journal_volume ? _journal_page_first ? _journal_page_last ? _journal_year ? loop_ _publ_author_name 'Daniel Carmona' 'Fernando Viguri' 'Pilar Lamata' 'Joaquina Ferrer' F.Lahoz 'Pilar Garcia-Orduna' 'Luis Oro' 'Elisa Bardaji' # ---------------------------------------------------------- # data for compnd_3 (locally labelled as dan37as) data_compnd_3 _database_code_depnum_ccdc_archive 'CCDC 881059' #TrackingRef '- compnd_3_8b_cif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C12 H16 Cl N O2 Ru, H2 O' _chemical_formula_sum 'C12 H18 Cl N O3 Ru' _chemical_formula_weight 360.80 _chemical_absolute_configuration rmad loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0030 0.0020 '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 0.0060 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0110 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1480 0.1590 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2590 0.8360 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C 2' _symmetry_space_group_name_Hall 'C 2y' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' _cell_length_a 17.365(2) _cell_length_b 6.2660(9) _cell_length_c 24.847(3) _cell_angle_alpha 90.00 _cell_angle_beta 106.045(2) _cell_angle_gamma 90.00 _cell_volume 2598.2(6) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 3658 _cell_measurement_theta_min 2.441 _cell_measurement_theta_max 28.111 _exptl_crystal_description needle _exptl_crystal_colour 'dark yellow' _exptl_crystal_size_max 0.377 _exptl_crystal_size_mid 0.074 _exptl_crystal_size_min 0.030 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.845 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1456 _exptl_absorpt_coefficient_mu 1.412 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.758 _exptl_absorpt_correction_T_max 0.846 _exptl_absorpt_process_details ; SADABS: Area-Detector Absorption Correction. (1996) Bruker-AXS within APEX2 package. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'Bruker SMART APEX CCD system' _diffrn_measurement_method '\w rotations with narrow frames' _diffrn_detector_area_resol_mean 8.26 _diffrn_standards_decay_% ? _diffrn_reflns_number 8590 _diffrn_reflns_av_R_equivalents 0.0174 _diffrn_reflns_av_sigmaI/netI 0.0381 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 0.85 _diffrn_reflns_theta_max 28.39 _reflns_number_total 5562 _reflns_number_gt 5275 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART v. 5.611 (Bruker AXS, 2000)' _computing_cell_refinement 'APEX2 v. 2008.4 (Bruker AXS, 2008)' _computing_data_reduction 'APEX2 v. 2008.4 (Bruker AXS, 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ORTEP _computing_publication_material ENCIFER _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. Most of the hydrogen atoms have been calculated and refined with a riding model. The hydrogen atoms of the stereogenic centers (nitrogen and \a-carbon atoms of the aminoacid) have been included in the model in observed positions and freely refined. Hydrogen atoms of the water molecules have been included in the model in observed positions and refined with a restraint in O-H distance. Although PLATON program suggests the existence of a pseudo-symmetry and a change to a centrosymetric C2/c space group this option is not adequate, as the Ru complex has a stereogenic center coming from the starting L-amino acid. The solution and refinement of the structure in C2/c space group (with only one Ru complex molecule in the asymmetric unit) leads to unrealistic results, with a static disorder in the amino carboxylate ligand. ; _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^)+(0.0374P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.02(3) _refine_ls_number_reflns 5562 _refine_ls_number_parameters 357 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0322 _refine_ls_R_factor_gt 0.0296 _refine_ls_wR_factor_ref 0.0674 _refine_ls_wR_factor_gt 0.0656 _refine_ls_goodness_of_fit_ref 1.015 _refine_ls_restrained_S_all 1.015 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _iucr_refine_instructions_details ; TITL dan37as in C2 CELL 0.71073 17.3648 6.2660 24.8469 90.000 106.045 90.000 ZERR 8.00 0.0024 0.0009 0.0034 0.000 0.002 0.000 LATT -7 SYMM - X, Y, - Z SFAC C 2.31000 20.84392 1.02000 10.20751 1.58860 0.56870 = 0.86500 51.65125 0.21560 0.003 0.002 11.500 0.770 12.011 SFAC H 0.49300 10.51091 0.32291 26.12573 0.14019 3.14236 = 0.04081 57.79977 0.00304 0.000 0.000 0.620 0.320 1.008 SFAC N 12.21261 0.00570 3.13220 9.89331 2.01250 28.99754 = 1.16630 0.58260 -11.52901 0.006 0.003 19.600 0.700 14.007 SFAC O 3.04850 13.27711 2.28680 5.70111 1.54630 0.32390 = 0.86700 32.90894 0.25080 0.011 0.006 32.500 0.660 15.999 SFAC CL 11.46041 0.01040 7.19641 1.16620 6.25561 18.51942 = 1.64550 47.77846 -9.55741 0.148 0.159 678.000 0.990 35.453 SFAC RU 19.26743 0.80852 12.91821 8.43468 4.86337 24.79974 = 1.56756 94.29289 5.37875 -1.259 0.836 3640.000 1.390 101.070 UNIT 96 144 8 24 8 8 MERG 2 DFIX 0.820 0.020 H31 O3 H32 O3 FMAP 2 PLAN 15 ACTA 55.00 BOND CONF L.S. 4 TEMP -173.00 WGHT 0.037400 FVAR 0.06809 RU1 6 0.597317 0.567569 0.644952 11.00000 0.01169 0.01148 = 0.01258 -0.00139 0.00334 -0.00057 CL1 5 0.584526 0.791242 0.564286 11.00000 0.02014 0.01771 = 0.01673 0.00174 0.00661 -0.00120 O1 4 0.527479 0.796118 0.672221 11.00000 0.01597 0.01349 = 0.01303 -0.00444 0.00340 -0.00009 O2 4 0.405082 0.926926 0.660190 11.00000 0.02091 0.01907 = 0.01964 -0.00143 0.00549 0.00686 N1 3 0.476989 0.462557 0.609452 11.00000 0.01534 0.00994 = 0.01333 -0.00010 0.00610 -0.00127 C1 1 0.687876 0.582227 0.724310 11.00000 0.01814 0.03489 = 0.01400 -0.00585 -0.00307 0.00702 AFIX 43 H1 2 0.693767 0.681726 0.754024 11.00000 -1.20000 AFIX 0 C2 1 0.725389 0.620815 0.681660 11.00000 0.01352 0.02338 = 0.02750 -0.00590 0.00191 -0.00274 AFIX 43 H2 2 0.757858 0.743812 0.683015 11.00000 -1.20000 AFIX 0 C3 1 0.714308 0.476429 0.637452 11.00000 0.01216 0.02018 = 0.02671 0.00415 0.00730 0.00377 AFIX 43 H3 2 0.738621 0.503639 0.608265 11.00000 -1.20000 AFIX 0 C4 1 0.667957 0.291970 0.635323 11.00000 0.01758 0.02005 = 0.02490 -0.00505 0.00411 0.00746 AFIX 43 H4 2 0.661198 0.194165 0.605158 11.00000 -1.20000 AFIX 0 C5 1 0.631350 0.253225 0.678667 11.00000 0.01490 0.01386 = 0.03533 0.00707 -0.00012 0.00404 AFIX 43 H5 2 0.599633 0.128801 0.677388 11.00000 -1.20000 AFIX 0 C6 1 0.641172 0.394456 0.722962 11.00000 0.01826 0.02748 = 0.01802 0.01402 0.00402 0.00846 AFIX 43 H6 2 0.616977 0.366297 0.752161 11.00000 -1.20000 AFIX 0 C7 1 0.452331 0.803477 0.647327 11.00000 0.02107 0.01137 = 0.01135 -0.00081 0.00504 -0.00332 C8 1 0.422983 0.650906 0.597994 11.00000 0.01568 0.01468 = 0.01249 -0.00203 0.00319 0.00033 C9 1 0.457929 0.319093 0.560161 11.00000 0.01484 0.01711 = 0.02015 -0.00571 0.00323 0.00308 AFIX 23 H9A 2 0.493182 0.192178 0.568562 11.00000 -1.20000 H9B 2 0.468837 0.394339 0.528008 11.00000 -1.20000 AFIX 0 C10 1 0.370733 0.247172 0.544236 11.00000 0.02171 0.01921 = 0.02343 -0.00518 0.00453 -0.00441 AFIX 23 H10A 2 0.359546 0.160072 0.509693 11.00000 -1.20000 H10B 2 0.361447 0.156663 0.574500 11.00000 -1.20000 AFIX 0 C11 1 0.314023 0.435893 0.534672 11.00000 0.01571 0.02020 = 0.01493 -0.00107 0.00058 -0.00119 AFIX 23 H11A 2 0.258386 0.384120 0.528476 11.00000 -1.20000 H11B 2 0.317106 0.513814 0.500668 11.00000 -1.20000 AFIX 0 C12 1 0.334890 0.586598 0.584571 11.00000 0.01215 0.01376 = 0.01670 -0.00162 0.00034 0.00320 AFIX 23 H12A 2 0.324623 0.515378 0.617480 11.00000 -1.20000 H12B 2 0.300695 0.715460 0.575961 11.00000 -1.20000 AFIX 0 RU21 6 0.403408 0.616936 0.860466 11.00000 0.01099 0.01012 = 0.01326 -0.00175 0.00216 -0.00064 CL21 5 0.399784 0.396821 0.938985 11.00000 0.02193 0.01500 = 0.02101 0.00220 0.00842 -0.00216 O21 4 0.475091 0.380209 0.839203 11.00000 0.01541 0.01285 = 0.01896 -0.00491 0.00182 -0.00093 O22 4 0.600254 0.286962 0.843887 11.00000 0.01860 0.01893 = 0.02123 -0.00554 0.00537 0.00387 N21 3 0.518447 0.692282 0.913312 11.00000 0.01394 0.00922 = 0.01332 0.00191 0.00406 0.00038 C21 1 0.316321 0.590961 0.779341 11.00000 0.02174 0.02103 = 0.02293 -0.00582 -0.00667 0.00488 AFIX 43 H21 2 0.307437 0.479541 0.752391 11.00000 -1.20000 AFIX 0 C22 1 0.275188 0.588914 0.819663 11.00000 0.01244 0.01835 = 0.03816 0.00126 -0.00249 0.00039 AFIX 43 H22 2 0.238499 0.477475 0.820627 11.00000 -1.20000 AFIX 0 C23 1 0.288939 0.757981 0.859953 11.00000 0.01638 0.02853 = 0.02652 -0.00097 0.00553 0.01175 AFIX 43 H23 2 0.260957 0.758196 0.887844 11.00000 -1.20000 AFIX 0 C24 1 0.342020 0.920360 0.859001 11.00000 0.02619 0.01211 = 0.02627 -0.00148 -0.00603 0.00829 AFIX 43 H24 2 0.350335 1.032206 0.885808 11.00000 -1.20000 AFIX 0 C25 1 0.384347 0.918685 0.817327 11.00000 0.01481 0.02186 = 0.03354 0.01672 -0.00579 -0.00400 AFIX 43 H25 2 0.421614 1.028920 0.816619 11.00000 -1.20000 AFIX 0 C26 1 0.371083 0.754331 0.777275 11.00000 0.02473 0.03907 = 0.01579 0.00691 0.00358 0.01202 AFIX 43 H26 2 0.398718 0.753551 0.749187 11.00000 -1.20000 AFIX 0 C27 1 0.552663 0.410730 0.855581 11.00000 0.01250 0.01490 = 0.01099 0.00312 0.00274 0.00176 C28 1 0.579727 0.618436 0.885440 11.00000 0.01466 0.01745 = 0.01737 -0.00612 0.00614 -0.00214 C29 1 0.538073 0.912457 0.935515 11.00000 0.02030 0.00768 = 0.01250 -0.00352 0.00476 -0.00124 AFIX 23 H29A 2 0.497562 0.960008 0.954211 11.00000 -1.20000 H29B 2 0.536244 1.011273 0.904096 11.00000 -1.20000 AFIX 0 C30 1 0.620509 0.920265 0.976860 11.00000 0.01788 0.01779 = 0.02112 -0.00608 0.00252 0.00018 AFIX 23 H30A 2 0.620860 0.831814 1.009942 11.00000 -1.20000 H30B 2 0.633155 1.069022 0.989698 11.00000 -1.20000 AFIX 0 C31 1 0.684198 0.838552 0.950280 11.00000 0.01678 0.03021 = 0.02933 -0.01362 0.00444 -0.00465 AFIX 23 H31A 2 0.689022 0.938246 0.920472 11.00000 -1.20000 H31B 2 0.736657 0.832830 0.978962 11.00000 -1.20000 AFIX 0 C32 1 0.662747 0.618790 0.925597 11.00000 0.01204 0.02920 = 0.02495 -0.00759 0.00345 0.00250 AFIX 23 H32A 2 0.702132 0.574125 0.905620 11.00000 -1.20000 H32B 2 0.665062 0.515122 0.956072 11.00000 -1.20000 AFIX 0 O4 4 0.591298 0.908971 0.784499 11.00000 0.03897 0.01812 = 0.01494 -0.00140 0.00235 0.00003 O3 4 0.431302 0.315160 0.713967 11.00000 0.03668 0.01879 = 0.01631 -0.00444 0.00455 -0.00381 H21N 2 0.525846 0.612970 0.939185 11.00000 0.01322 H28 2 0.580280 0.726275 0.854027 11.00000 0.01007 H1N 2 0.458798 0.392316 0.634470 11.00000 0.01366 H31 2 0.428375 0.192328 0.701435 11.00000 0.03008 H32 2 0.454767 0.321045 0.746536 11.00000 0.03216 H41 2 0.582588 1.044720 0.789352 11.00000 0.03885 H42 2 0.562096 0.918697 0.752377 11.00000 0.04288 H8 2 0.435506 0.730460 0.567239 11.00000 0.00931 HKLF 4 REM dan37as in C2 REM R1 = 0.0296 for 5275 Fo > 4sig(Fo) and 0.0322 for all 5562 data REM 357 parameters refined using 3 restraints END ; 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 0.597317(16) 0.56757(4) 0.644952(12) 0.01192(9) Uani 1 1 d . . . Cl1 Cl 0.58453(6) 0.79124(18) 0.56429(4) 0.0179(2) Uani 1 1 d . . . O1 O 0.52748(15) 0.7961(5) 0.67222(10) 0.0143(6) Uani 1 1 d . . . O2 O 0.40508(17) 0.9269(5) 0.66019(12) 0.0199(7) Uani 1 1 d . . . N1 N 0.47699(18) 0.4626(5) 0.60945(13) 0.0124(7) Uani 1 1 d . . . C1 C 0.6879(2) 0.5822(10) 0.72431(15) 0.0238(11) Uani 1 1 d . . . H1 H 0.6938 0.6817 0.7540 0.029 Uiso 1 1 calc R . . C2 C 0.7254(2) 0.6208(10) 0.68166(17) 0.0222(10) Uani 1 1 d . . . H2 H 0.7579 0.7438 0.6830 0.027 Uiso 1 1 calc R . . C3 C 0.7143(2) 0.4764(8) 0.63745(18) 0.0193(10) Uani 1 1 d . . . H3 H 0.7386 0.5036 0.6083 0.023 Uiso 1 1 calc R . . C4 C 0.6680(2) 0.2920(8) 0.63532(18) 0.0212(10) Uani 1 1 d . . . H4 H 0.6612 0.1942 0.6052 0.025 Uiso 1 1 calc R . . C5 C 0.6314(2) 0.2532(8) 0.67867(18) 0.0228(10) Uani 1 1 d . . . H5 H 0.5996 0.1288 0.6774 0.027 Uiso 1 1 calc R . . C6 C 0.6412(2) 0.3945(8) 0.72296(17) 0.0215(10) Uani 1 1 d . . . H6 H 0.6170 0.3663 0.7522 0.026 Uiso 1 1 calc R . . C7 C 0.4523(3) 0.8035(8) 0.64733(17) 0.0145(9) Uani 1 1 d . . . C8 C 0.4230(2) 0.6509(6) 0.59799(15) 0.0144(8) Uani 1 1 d . . . C9 C 0.4579(2) 0.3191(8) 0.56016(17) 0.0177(9) Uani 1 1 d . . . H9A H 0.4932 0.1922 0.5686 0.021 Uiso 1 1 calc R . . H9B H 0.4688 0.3943 0.5280 0.021 Uiso 1 1 calc R . . C10 C 0.3707(2) 0.2472(7) 0.54424(17) 0.0218(9) Uani 1 1 d . . . H10A H 0.3595 0.1601 0.5097 0.026 Uiso 1 1 calc R . . H10B H 0.3614 0.1567 0.5745 0.026 Uiso 1 1 calc R . . C11 C 0.3140(2) 0.4359(6) 0.53467(15) 0.0177(9) Uani 1 1 d . . . H11A H 0.2584 0.3841 0.5285 0.021 Uiso 1 1 calc R . . H11B H 0.3171 0.5138 0.5007 0.021 Uiso 1 1 calc R . . C12 C 0.3349(2) 0.5866(8) 0.58457(14) 0.0149(8) Uani 1 1 d . . . H12A H 0.3246 0.5154 0.6175 0.018 Uiso 1 1 calc R . . H12B H 0.3007 0.7155 0.5760 0.018 Uiso 1 1 calc R . . Ru21 Ru 0.403408(16) 0.61694(4) 0.860466(12) 0.01169(9) Uani 1 1 d . . . Cl21 Cl 0.39978(6) 0.39682(18) 0.93899(4) 0.0188(2) Uani 1 1 d . . . O21 O 0.47509(16) 0.3802(5) 0.83920(11) 0.0163(6) Uani 1 1 d . . . O22 O 0.60025(17) 0.2870(5) 0.84389(12) 0.0196(7) Uani 1 1 d . . . N21 N 0.51845(19) 0.6923(5) 0.91331(13) 0.0121(7) Uani 1 1 d . . . C21 C 0.3163(2) 0.5910(10) 0.77934(16) 0.0245(10) Uani 1 1 d . . . H21 H 0.3074 0.4795 0.7524 0.029 Uiso 1 1 calc R . . C22 C 0.2752(2) 0.5889(10) 0.81966(18) 0.0249(10) Uani 1 1 d . . . H22 H 0.2385 0.4775 0.8206 0.030 Uiso 1 1 calc R . . C23 C 0.2889(3) 0.7580(8) 0.85995(19) 0.0239(11) Uani 1 1 d . . . H23 H 0.2610 0.7582 0.8878 0.029 Uiso 1 1 calc R . . C24 C 0.3420(3) 0.9204(8) 0.85900(18) 0.0242(10) Uani 1 1 d . . . H24 H 0.3503 1.0322 0.8858 0.029 Uiso 1 1 calc R . . C25 C 0.3843(3) 0.9187(8) 0.81733(19) 0.0259(11) Uani 1 1 d . . . H25 H 0.4216 1.0289 0.8166 0.031 Uiso 1 1 calc R . . C26 C 0.3711(3) 0.7543(9) 0.77727(18) 0.0269(12) Uani 1 1 d . . . H26 H 0.3987 0.7536 0.7492 0.032 Uiso 1 1 calc R . . C27 C 0.5527(2) 0.4107(7) 0.85558(16) 0.0129(9) Uani 1 1 d . . . C28 C 0.5797(2) 0.6184(7) 0.88544(15) 0.0162(8) Uani 1 1 d . . . C29 C 0.5381(2) 0.9125(7) 0.93551(16) 0.0134(8) Uani 1 1 d . . . H29A H 0.4976 0.9600 0.9542 0.016 Uiso 1 1 calc R . . H29B H 0.5362 1.0113 0.9041 0.016 Uiso 1 1 calc R . . C30 C 0.6205(2) 0.9203(7) 0.97686(17) 0.0195(9) Uani 1 1 d . . . H30A H 0.6209 0.8318 1.0099 0.023 Uiso 1 1 calc R . . H30B H 0.6332 1.0690 0.9897 0.023 Uiso 1 1 calc R . . C31 C 0.6842(2) 0.8386(8) 0.95028(18) 0.0258(10) Uani 1 1 d . . . H31A H 0.6890 0.9382 0.9205 0.031 Uiso 1 1 calc R . . H31B H 0.7367 0.8328 0.9790 0.031 Uiso 1 1 calc R . . C32 C 0.6627(2) 0.6188(9) 0.92560(17) 0.0224(10) Uani 1 1 d . . . H32A H 0.7021 0.5741 0.9056 0.027 Uiso 1 1 calc R . . H32B H 0.6651 0.5151 0.9561 0.027 Uiso 1 1 calc R . . O4 O 0.5913(2) 0.9090(6) 0.78450(13) 0.0250(8) Uani 1 1 d . . . O3 O 0.4313(2) 0.3152(6) 0.71397(13) 0.0245(7) Uani 1 1 d D . . H21N H 0.526(2) 0.613(7) 0.9392(16) 0.013(11) Uiso 1 1 d . . . H28 H 0.580(2) 0.726(6) 0.8540(16) 0.010(10) Uiso 1 1 d . . . H1N H 0.459(2) 0.392(7) 0.6345(17) 0.014(11) Uiso 1 1 d . . . H31 H 0.428(3) 0.192(4) 0.7014(18) 0.030(15) Uiso 1 1 d D . . H32 H 0.455(3) 0.321(9) 0.7465(9) 0.032(14) Uiso 1 1 d D . . H41 H 0.583(3) 1.045(10) 0.789(2) 0.039(15) Uiso 1 1 d . . . H42 H 0.562(3) 0.919(9) 0.752(2) 0.043(17) Uiso 1 1 d . . . H8 H 0.436(2) 0.730(6) 0.5672(15) 0.009(10) 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 0.01169(16) 0.0115(2) 0.01258(15) -0.00139(12) 0.00334(12) -0.00057(13) Cl1 0.0201(5) 0.0177(6) 0.0167(5) 0.0017(4) 0.0066(4) -0.0012(4) O1 0.0160(14) 0.0135(17) 0.0130(14) -0.0044(11) 0.0034(11) -0.0001(13) O2 0.0209(15) 0.0191(18) 0.0196(15) -0.0014(13) 0.0055(12) 0.0069(14) N1 0.0153(16) 0.0099(16) 0.0133(17) -0.0001(13) 0.0061(13) -0.0013(13) C1 0.0181(19) 0.035(3) 0.0140(18) -0.006(2) -0.0031(14) 0.007(3) C2 0.0135(19) 0.023(3) 0.028(2) -0.006(2) 0.0019(16) -0.003(2) C3 0.0122(19) 0.020(2) 0.027(2) 0.0041(18) 0.0073(16) 0.0038(17) C4 0.018(2) 0.020(3) 0.025(2) -0.0051(19) 0.0041(17) 0.007(2) C5 0.015(2) 0.014(2) 0.035(3) 0.0071(19) -0.0001(18) 0.0040(18) C6 0.018(2) 0.027(3) 0.018(2) 0.0140(19) 0.0040(16) 0.008(2) C7 0.021(2) 0.011(2) 0.011(2) -0.0008(16) 0.0050(16) -0.0033(18) C8 0.0157(18) 0.015(2) 0.0125(18) -0.0020(15) 0.0032(15) 0.0003(16) C9 0.0148(19) 0.017(2) 0.020(2) -0.0057(17) 0.0032(16) 0.0031(17) C10 0.022(2) 0.019(2) 0.023(2) -0.0052(18) 0.0045(17) -0.0044(18) C11 0.0157(19) 0.020(2) 0.015(2) -0.0011(16) 0.0006(15) -0.0012(17) C12 0.0122(17) 0.014(2) 0.0167(17) -0.0016(17) 0.0003(13) 0.0032(18) Ru21 0.01099(15) 0.0101(2) 0.01326(15) -0.00175(12) 0.00216(11) -0.00064(13) Cl21 0.0219(5) 0.0150(5) 0.0210(5) 0.0022(4) 0.0084(4) -0.0022(4) O21 0.0154(14) 0.0128(16) 0.0190(15) -0.0049(12) 0.0018(11) -0.0009(13) O22 0.0186(15) 0.0189(18) 0.0212(16) -0.0055(13) 0.0054(12) 0.0039(14) N21 0.0139(16) 0.0092(16) 0.0133(17) 0.0019(13) 0.0041(13) 0.0004(12) C21 0.022(2) 0.021(3) 0.023(2) -0.006(2) -0.0067(16) 0.005(2) C22 0.0124(19) 0.018(3) 0.038(2) 0.001(2) -0.0025(16) 0.000(2) C23 0.016(2) 0.029(3) 0.027(2) -0.001(2) 0.0055(18) 0.012(2) C24 0.026(2) 0.012(2) 0.026(2) -0.0015(18) -0.0060(18) 0.008(2) C25 0.015(2) 0.022(3) 0.034(3) 0.017(2) -0.0058(17) -0.0040(19) C26 0.025(2) 0.039(3) 0.016(2) 0.007(2) 0.0036(18) 0.012(2) C27 0.0125(18) 0.015(2) 0.0110(19) 0.0031(16) 0.0027(14) 0.0018(17) C28 0.0147(17) 0.017(2) 0.0174(19) -0.0061(17) 0.0061(14) -0.0021(17) C29 0.020(2) 0.008(2) 0.0125(19) -0.0035(14) 0.0048(15) -0.0012(16) C30 0.018(2) 0.018(2) 0.021(2) -0.0061(17) 0.0025(16) 0.0002(17) C31 0.017(2) 0.030(3) 0.029(2) -0.014(2) 0.0044(18) -0.005(2) C32 0.0120(18) 0.029(3) 0.025(2) -0.008(2) 0.0034(15) 0.002(2) O4 0.039(2) 0.0181(18) 0.0149(16) -0.0014(13) 0.0023(14) 0.0000(16) O3 0.0367(18) 0.0188(18) 0.0163(17) -0.0044(13) 0.0046(14) -0.0038(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 Ru1 O1 2.106(3) . ? Ru1 N1 2.135(3) . ? Ru1 C1 2.158(4) . ? Ru1 C5 2.158(5) . ? Ru1 C3 2.167(4) . ? Ru1 C6 2.167(4) . ? Ru1 C4 2.169(5) . ? Ru1 C2 2.184(4) . ? Ru1 Cl1 2.4051(11) . ? O1 C7 1.281(5) . ? O2 C7 1.232(5) . ? N1 C9 1.481(5) . ? N1 C8 1.485(5) . ? C1 C2 1.410(5) . ? C1 C6 1.424(7) . ? C2 C3 1.395(6) . ? C3 C4 1.401(6) . ? C4 C5 1.415(6) . ? C5 C6 1.386(6) . ? C7 C8 1.527(6) . ? C8 C12 1.527(5) . ? C9 C10 1.524(5) . ? C10 C11 1.515(6) . ? C11 C12 1.521(5) . ? Ru21 O21 2.096(3) . ? Ru21 N21 2.118(3) . ? Ru21 C25 2.153(5) . ? Ru21 C26 2.165(4) . ? Ru21 C21 2.166(4) . ? Ru21 C23 2.172(4) . ? Ru21 C24 2.175(5) . ? Ru21 C22 2.184(4) . ? Ru21 Cl21 2.4042(11) . ? O21 C27 1.309(5) . ? O22 C27 1.225(5) . ? N21 C29 1.490(5) . ? N21 C28 1.494(4) . ? C21 C22 1.382(6) . ? C21 C26 1.408(7) . ? C22 C23 1.432(7) . ? C23 C24 1.377(7) . ? C24 C25 1.426(6) . ? C25 C26 1.406(7) . ? C27 C28 1.507(6) . ? C28 C32 1.510(5) . ? C29 C30 1.515(5) . ? C30 C31 1.525(5) . ? C31 C32 1.512(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Ru1 N1 75.97(11) . . ? O1 Ru1 C1 90.92(16) . . ? N1 Ru1 C1 140.67(15) . . ? O1 Ru1 C5 128.03(14) . . ? N1 Ru1 C5 90.62(15) . . ? C1 Ru1 C5 68.4(2) . . ? O1 Ru1 C3 147.53(16) . . ? N1 Ru1 C3 135.80(15) . . ? C1 Ru1 C3 68.04(16) . . ? C5 Ru1 C3 68.30(17) . . ? O1 Ru1 C6 98.27(14) . . ? N1 Ru1 C6 106.09(15) . . ? C1 Ru1 C6 38.4(2) . . ? C5 Ru1 C6 37.36(17) . . ? C3 Ru1 C6 80.74(16) . . ? O1 Ru1 C4 165.99(14) . . ? N1 Ru1 C4 103.16(15) . . ? C1 Ru1 C4 80.98(19) . . ? C5 Ru1 C4 38.16(15) . . ? C3 Ru1 C4 37.70(17) . . ? C6 Ru1 C4 68.32(17) . . ? O1 Ru1 C2 111.86(16) . . ? N1 Ru1 C2 170.81(18) . . ? C1 Ru1 C2 37.89(15) . . ? C5 Ru1 C2 80.8(2) . . ? C3 Ru1 C2 37.39(17) . . ? C6 Ru1 C2 68.74(17) . . ? C4 Ru1 C2 68.04(19) . . ? O1 Ru1 Cl1 86.74(8) . . ? N1 Ru1 Cl1 88.90(9) . . ? C1 Ru1 Cl1 127.80(16) . . ? C5 Ru1 Cl1 143.87(12) . . ? C3 Ru1 Cl1 87.41(12) . . ? C6 Ru1 Cl1 164.92(12) . . ? C4 Ru1 Cl1 107.26(12) . . ? C2 Ru1 Cl1 96.19(14) . . ? C7 O1 Ru1 118.0(3) . . ? C9 N1 C8 109.8(3) . . ? C9 N1 Ru1 119.9(2) . . ? C8 N1 Ru1 109.2(2) . . ? C2 C1 C6 120.2(5) . . ? C2 C1 Ru1 72.0(2) . . ? C6 C1 Ru1 71.1(2) . . ? C3 C2 C1 119.3(5) . . ? C3 C2 Ru1 70.7(2) . . ? C1 C2 Ru1 70.1(2) . . ? C2 C3 C4 121.2(4) . . ? C2 C3 Ru1 71.9(2) . . ? C4 C3 Ru1 71.2(2) . . ? C3 C4 C5 119.2(4) . . ? C3 C4 Ru1 71.1(3) . . ? C5 C4 Ru1 70.5(3) . . ? C6 C5 C4 120.8(4) . . ? C6 C5 Ru1 71.7(3) . . ? C4 C5 Ru1 71.4(3) . . ? C5 C6 C1 119.4(4) . . ? C5 C6 Ru1 70.9(2) . . ? C1 C6 Ru1 70.4(2) . . ? O2 C7 O1 124.0(4) . . ? O2 C7 C8 120.2(4) . . ? O1 C7 C8 115.8(4) . . ? N1 C8 C7 106.9(3) . . ? N1 C8 C12 111.9(3) . . ? C7 C8 C12 115.6(3) . . ? N1 C9 C10 111.9(3) . . ? C11 C10 C9 111.5(4) . . ? C10 C11 C12 111.0(3) . . ? C11 C12 C8 109.9(3) . . ? O21 Ru21 N21 77.88(12) . . ? O21 Ru21 C25 121.08(16) . . ? N21 Ru21 C25 95.84(15) . . ? O21 Ru21 C26 93.21(15) . . ? N21 Ru21 C26 117.02(16) . . ? C25 Ru21 C26 38.00(19) . . ? O21 Ru21 C21 91.30(15) . . ? N21 Ru21 C21 152.85(15) . . ? C25 Ru21 C21 68.3(2) . . ? C26 Ru21 C21 37.94(19) . . ? O21 Ru21 C23 153.23(17) . . ? N21 Ru21 C23 128.14(16) . . ? C25 Ru21 C23 68.00(18) . . ? C26 Ru21 C23 80.63(17) . . ? C21 Ru21 C23 67.83(17) . . ? O21 Ru21 C24 159.54(15) . . ? N21 Ru21 C24 100.92(15) . . ? C25 Ru21 C24 38.46(17) . . ? C26 Ru21 C24 68.89(18) . . ? C21 Ru21 C24 80.63(19) . . ? C23 Ru21 C24 36.95(18) . . ? O21 Ru21 C22 115.24(17) . . ? N21 Ru21 C22 166.29(16) . . ? C25 Ru21 C22 80.95(19) . . ? C26 Ru21 C22 68.08(17) . . ? C21 Ru21 C22 37.05(15) . . ? C23 Ru21 C22 38.37(19) . . ? C24 Ru21 C22 68.3(2) . . ? O21 Ru21 Cl21 87.08(8) . . ? N21 Ru21 Cl21 81.75(9) . . ? C25 Ru21 Cl21 150.77(14) . . ? C26 Ru21 Cl21 160.88(14) . . ? C21 Ru21 Cl21 122.95(15) . . ? C23 Ru21 Cl21 90.52(13) . . ? C24 Ru21 Cl21 113.10(12) . . ? C22 Ru21 Cl21 94.51(14) . . ? C27 O21 Ru21 116.7(3) . . ? C29 N21 C28 109.8(3) . . ? C29 N21 Ru21 121.1(3) . . ? C28 N21 Ru21 108.3(2) . . ? C22 C21 C26 121.5(5) . . ? C22 C21 Ru21 72.2(2) . . ? C26 C21 Ru21 71.0(2) . . ? C21 C22 C23 118.7(5) . . ? C21 C22 Ru21 70.8(2) . . ? C23 C22 Ru21 70.4(2) . . ? C24 C23 C22 121.2(4) . . ? C24 C23 Ru21 71.6(2) . . ? C22 C23 Ru21 71.2(2) . . ? C23 C24 C25 119.3(4) . . ? C23 C24 Ru21 71.4(3) . . ? C25 C24 Ru21 69.9(3) . . ? C26 C25 C24 120.2(4) . . ? C26 C25 Ru21 71.4(3) . . ? C24 C25 Ru21 71.6(3) . . ? C25 C26 C21 119.1(4) . . ? C25 C26 Ru21 70.5(2) . . ? C21 C26 Ru21 71.1(3) . . ? O22 C27 O21 122.5(4) . . ? O22 C27 C28 121.6(4) . . ? O21 C27 C28 115.7(4) . . ? N21 C28 C27 109.3(3) . . ? N21 C28 C32 111.4(3) . . ? C27 C28 C32 115.9(4) . . ? N21 C29 C30 111.0(4) . . ? C29 C30 C31 111.0(3) . . ? C32 C31 C30 110.8(4) . . ? C28 C32 C31 110.7(4) . . ? 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 C7 -15.7(3) . . . . ? C1 Ru1 O1 C7 -158.2(3) . . . . ? C5 Ru1 O1 C7 -95.3(3) . . . . ? C3 Ru1 O1 C7 153.9(3) . . . . ? C6 Ru1 O1 C7 -120.3(3) . . . . ? C4 Ru1 O1 C7 -103.9(6) . . . . ? C2 Ru1 O1 C7 169.3(3) . . . . ? Cl1 Ru1 O1 C7 73.9(3) . . . . ? O1 Ru1 N1 C9 158.5(3) . . . . ? C1 Ru1 N1 C9 -127.7(4) . . . . ? C5 Ru1 N1 C9 -72.3(3) . . . . ? C3 Ru1 N1 C9 -13.6(4) . . . . ? C6 Ru1 N1 C9 -106.8(3) . . . . ? C4 Ru1 N1 C9 -35.9(3) . . . . ? Cl1 Ru1 N1 C9 71.6(3) . . . . ? O1 Ru1 N1 C8 30.6(2) . . . . ? C1 Ru1 N1 C8 104.5(3) . . . . ? C5 Ru1 N1 C8 159.9(3) . . . . ? C3 Ru1 N1 C8 -141.4(2) . . . . ? C6 Ru1 N1 C8 125.4(3) . . . . ? C4 Ru1 N1 C8 -163.7(2) . . . . ? O1 Ru1 C1 C2 -125.8(3) . . . . ? N1 Ru1 C1 C2 165.4(3) . . . . ? C5 Ru1 C1 C2 103.1(4) . . . . ? C3 Ru1 C1 C2 28.8(3) . . . . ? C6 Ru1 C1 C2 132.0(5) . . . . ? C4 Ru1 C1 C2 65.6(3) . . . . ? Cl1 Ru1 C1 C2 -39.3(4) . . . . ? O1 Ru1 C1 C6 102.2(2) . . . . ? N1 Ru1 C1 C6 33.5(4) . . . . ? C5 Ru1 C1 C6 -28.8(2) . . . . ? C3 Ru1 C1 C6 -103.2(3) . . . . ? C4 Ru1 C1 C6 -66.3(3) . . . . ? C2 Ru1 C1 C6 -132.0(5) . . . . ? Cl1 Ru1 C1 C6 -171.2(2) . . . . ? C6 C1 C2 C3 1.8(7) . . . . ? Ru1 C1 C2 C3 -52.6(4) . . . . ? C6 C1 C2 Ru1 54.5(4) . . . . ? O1 Ru1 C2 C3 -166.4(3) . . . . ? C1 Ru1 C2 C3 132.7(5) . . . . ? C5 Ru1 C2 C3 66.2(3) . . . . ? C6 Ru1 C2 C3 103.0(3) . . . . ? C4 Ru1 C2 C3 28.7(3) . . . . ? Cl1 Ru1 C2 C3 -77.5(3) . . . . ? O1 Ru1 C2 C1 60.8(4) . . . . ? C5 Ru1 C2 C1 -66.5(4) . . . . ? C3 Ru1 C2 C1 -132.7(5) . . . . ? C6 Ru1 C2 C1 -29.7(3) . . . . ? C4 Ru1 C2 C1 -104.0(4) . . . . ? Cl1 Ru1 C2 C1 149.8(3) . . . . ? C1 C2 C3 C4 -1.3(7) . . . . ? Ru1 C2 C3 C4 -53.6(4) . . . . ? C1 C2 C3 Ru1 52.3(4) . . . . ? O1 Ru1 C3 C2 23.9(4) . . . . ? N1 Ru1 C3 C2 -170.5(3) . . . . ? C1 Ru1 C3 C2 -29.1(3) . . . . ? C5 Ru1 C3 C2 -103.6(3) . . . . ? C6 Ru1 C3 C2 -66.9(3) . . . . ? C4 Ru1 C3 C2 -133.3(4) . . . . ? Cl1 Ru1 C3 C2 103.7(3) . . . . ? O1 Ru1 C3 C4 157.2(3) . . . . ? N1 Ru1 C3 C4 -37.2(4) . . . . ? C1 Ru1 C3 C4 104.2(3) . . . . ? C5 Ru1 C3 C4 29.7(3) . . . . ? C6 Ru1 C3 C4 66.4(3) . . . . ? C2 Ru1 C3 C4 133.3(4) . . . . ? Cl1 Ru1 C3 C4 -123.0(3) . . . . ? C2 C3 C4 C5 0.5(6) . . . . ? Ru1 C3 C4 C5 -53.4(4) . . . . ? C2 C3 C4 Ru1 54.0(4) . . . . ? O1 Ru1 C4 C3 -120.9(6) . . . . ? N1 Ru1 C4 C3 154.3(3) . . . . ? C1 Ru1 C4 C3 -65.6(3) . . . . ? C5 Ru1 C4 C3 -131.9(4) . . . . ? C6 Ru1 C4 C3 -103.4(3) . . . . ? C2 Ru1 C4 C3 -28.5(3) . . . . ? Cl1 Ru1 C4 C3 61.3(3) . . . . ? O1 Ru1 C4 C5 11.0(7) . . . . ? N1 Ru1 C4 C5 -73.8(3) . . . . ? C1 Ru1 C4 C5 66.3(3) . . . . ? C3 Ru1 C4 C5 131.9(4) . . . . ? C6 Ru1 C4 C5 28.6(3) . . . . ? C2 Ru1 C4 C5 103.5(3) . . . . ? Cl1 Ru1 C4 C5 -166.7(2) . . . . ? C3 C4 C5 C6 -0.3(6) . . . . ? Ru1 C4 C5 C6 -54.0(4) . . . . ? C3 C4 C5 Ru1 53.7(4) . . . . ? O1 Ru1 C5 C6 -43.7(3) . . . . ? N1 Ru1 C5 C6 -116.3(2) . . . . ? C1 Ru1 C5 C6 29.6(2) . . . . ? C3 Ru1 C5 C6 103.6(3) . . . . ? C4 Ru1 C5 C6 133.0(4) . . . . ? C2 Ru1 C5 C6 66.9(3) . . . . ? Cl1 Ru1 C5 C6 154.8(2) . . . . ? O1 Ru1 C5 C4 -176.6(2) . . . . ? N1 Ru1 C5 C4 110.8(3) . . . . ? C1 Ru1 C5 C4 -103.3(3) . . . . ? C3 Ru1 C5 C4 -29.3(3) . . . . ? C6 Ru1 C5 C4 -133.0(4) . . . . ? C2 Ru1 C5 C4 -66.0(3) . . . . ? Cl1 Ru1 C5 C4 21.8(4) . . . . ? C4 C5 C6 C1 0.8(6) . . . . ? Ru1 C5 C6 C1 -53.0(4) . . . . ? C4 C5 C6 Ru1 53.9(4) . . . . ? C2 C1 C6 C5 -1.6(6) . . . . ? Ru1 C1 C6 C5 53.3(4) . . . . ? C2 C1 C6 Ru1 -54.9(4) . . . . ? O1 Ru1 C6 C5 146.7(2) . . . . ? N1 Ru1 C6 C5 69.0(3) . . . . ? C1 Ru1 C6 C5 -132.4(4) . . . . ? C3 Ru1 C6 C5 -66.2(3) . . . . ? C4 Ru1 C6 C5 -29.1(2) . . . . ? C2 Ru1 C6 C5 -103.0(3) . . . . ? Cl1 Ru1 C6 C5 -104.8(5) . . . . ? O1 Ru1 C6 C1 -81.0(3) . . . . ? N1 Ru1 C6 C1 -158.7(2) . . . . ? C5 Ru1 C6 C1 132.4(4) . . . . ? C3 Ru1 C6 C1 66.2(3) . . . . ? C4 Ru1 C6 C1 103.3(3) . . . . ? C2 Ru1 C6 C1 29.3(3) . . . . ? Cl1 Ru1 C6 C1 27.6(7) . . . . ? Ru1 O1 C7 O2 178.5(3) . . . . ? Ru1 O1 C7 C8 -3.2(5) . . . . ? C9 N1 C8 C7 -173.4(3) . . . . ? Ru1 N1 C8 C7 -40.1(3) . . . . ? C9 N1 C8 C12 59.1(4) . . . . ? Ru1 N1 C8 C12 -167.6(2) . . . . ? O2 C7 C8 N1 -152.5(4) . . . . ? O1 C7 C8 N1 29.2(5) . . . . ? O2 C7 C8 C12 -27.1(6) . . . . ? O1 C7 C8 C12 154.5(4) . . . . ? C8 N1 C9 C10 -57.4(4) . . . . ? Ru1 N1 C9 C10 175.1(3) . . . . ? N1 C9 C10 C11 55.1(5) . . . . ? C9 C10 C11 C12 -53.0(4) . . . . ? C10 C11 C12 C8 53.7(4) . . . . ? N1 C8 C12 C11 -57.5(4) . . . . ? C7 C8 C12 C11 179.8(3) . . . . ? N21 Ru21 O21 C27 -14.9(3) . . . . ? C25 Ru21 O21 C27 74.6(3) . . . . ? C26 Ru21 O21 C27 102.1(3) . . . . ? C21 Ru21 O21 C27 140.0(3) . . . . ? C23 Ru21 O21 C27 177.6(3) . . . . ? C24 Ru21 O21 C27 73.9(5) . . . . ? C22 Ru21 O21 C27 169.3(3) . . . . ? Cl21 Ru21 O21 C27 -97.1(3) . . . . ? O21 Ru21 N21 C29 156.2(3) . . . . ? C25 Ru21 N21 C29 35.6(3) . . . . ? C26 Ru21 N21 C29 68.7(3) . . . . ? C21 Ru21 N21 C29 87.7(5) . . . . ? C23 Ru21 N21 C29 -30.9(4) . . . . ? C24 Ru21 N21 C29 -3.0(3) . . . . ? C22 Ru21 N21 C29 -40.1(9) . . . . ? Cl21 Ru21 N21 C29 -115.1(3) . . . . ? O21 Ru21 N21 C28 28.1(2) . . . . ? C25 Ru21 N21 C28 -92.5(3) . . . . ? C26 Ru21 N21 C28 -59.3(3) . . . . ? C21 Ru21 N21 C28 -40.3(5) . . . . ? C23 Ru21 N21 C28 -159.0(3) . . . . ? C24 Ru21 N21 C28 -131.0(3) . . . . ? C22 Ru21 N21 C28 -168.1(7) . . . . ? Cl21 Ru21 N21 C28 116.9(2) . . . . ? O21 Ru21 C21 C22 132.7(4) . . . . ? N21 Ru21 C21 C22 -161.9(3) . . . . ? C25 Ru21 C21 C22 -104.2(4) . . . . ? C26 Ru21 C21 C22 -133.8(5) . . . . ? C23 Ru21 C21 C22 -30.1(4) . . . . ? C24 Ru21 C21 C22 -66.2(4) . . . . ? Cl21 Ru21 C21 C22 45.3(4) . . . . ? O21 Ru21 C21 C26 -93.6(3) . . . . ? N21 Ru21 C21 C26 -28.1(5) . . . . ? C25 Ru21 C21 C26 29.6(3) . . . . ? C23 Ru21 C21 C26 103.7(3) . . . . ? C24 Ru21 C21 C26 67.5(3) . . . . ? C22 Ru21 C21 C26 133.8(5) . . . . ? Cl21 Ru21 C21 C26 179.1(2) . . . . ? C26 C21 C22 C23 0.2(7) . . . . ? Ru21 C21 C22 C23 53.4(4) . . . . ? C26 C21 C22 Ru21 -53.2(4) . . . . ? O21 Ru21 C22 C21 -54.3(4) . . . . ? N21 Ru21 C22 C21 143.2(6) . . . . ? C25 Ru21 C22 C21 65.8(4) . . . . ? C26 Ru21 C22 C21 28.6(3) . . . . ? C23 Ru21 C22 C21 131.6(5) . . . . ? C24 Ru21 C22 C21 103.7(4) . . . . ? Cl21 Ru21 C22 C21 -143.2(3) . . . . ? O21 Ru21 C22 C23 174.0(3) . . . . ? N21 Ru21 C22 C23 11.6(9) . . . . ? C25 Ru21 C22 C23 -65.8(3) . . . . ? C26 Ru21 C22 C23 -103.0(3) . . . . ? C21 Ru21 C22 C23 -131.6(5) . . . . ? C24 Ru21 C22 C23 -28.0(3) . . . . ? Cl21 Ru21 C22 C23 85.1(3) . . . . ? C21 C22 C23 C24 0.0(7) . . . . ? Ru21 C22 C23 C24 53.5(4) . . . . ? C21 C22 C23 Ru21 -53.6(4) . . . . ? O21 Ru21 C23 C24 -145.6(3) . . . . ? N21 Ru21 C23 C24 50.0(3) . . . . ? C25 Ru21 C23 C24 -29.8(3) . . . . ? C26 Ru21 C23 C24 -67.2(3) . . . . ? C21 Ru21 C23 C24 -104.4(3) . . . . ? C22 Ru21 C23 C24 -133.5(4) . . . . ? Cl21 Ru21 C23 C24 129.9(3) . . . . ? O21 Ru21 C23 C22 -12.1(5) . . . . ? N21 Ru21 C23 C22 -176.5(3) . . . . ? C25 Ru21 C23 C22 103.7(3) . . . . ? C26 Ru21 C23 C22 66.3(3) . . . . ? C21 Ru21 C23 C22 29.1(3) . . . . ? C24 Ru21 C23 C22 133.5(4) . . . . ? Cl21 Ru21 C23 C22 -96.6(3) . . . . ? C22 C23 C24 C25 -0.5(7) . . . . ? Ru21 C23 C24 C25 52.9(4) . . . . ? C22 C23 C24 Ru21 -53.4(4) . . . . ? O21 Ru21 C24 C23 133.3(4) . . . . ? N21 Ru21 C24 C23 -142.2(3) . . . . ? C25 Ru21 C24 C23 132.2(4) . . . . ? C26 Ru21 C24 C23 102.9(3) . . . . ? C21 Ru21 C24 C23 65.4(3) . . . . ? C22 Ru21 C24 C23 29.0(3) . . . . ? Cl21 Ru21 C24 C23 -56.6(3) . . . . ? O21 Ru21 C24 C25 1.1(5) . . . . ? N21 Ru21 C24 C25 85.6(3) . . . . ? C26 Ru21 C24 C25 -29.3(3) . . . . ? C21 Ru21 C24 C25 -66.8(3) . . . . ? C23 Ru21 C24 C25 -132.2(4) . . . . ? C22 Ru21 C24 C25 -103.2(3) . . . . ? Cl21 Ru21 C24 C25 171.2(2) . . . . ? C23 C24 C25 C26 0.8(6) . . . . ? Ru21 C24 C25 C26 54.4(4) . . . . ? C23 C24 C25 Ru21 -53.6(4) . . . . ? O21 Ru21 C25 C26 48.3(3) . . . . ? N21 Ru21 C25 C26 127.7(3) . . . . ? C21 Ru21 C25 C26 -29.5(2) . . . . ? C23 Ru21 C25 C26 -103.4(3) . . . . ? C24 Ru21 C25 C26 -132.1(4) . . . . ? C22 Ru21 C25 C26 -65.8(3) . . . . ? Cl21 Ru21 C25 C26 -148.8(2) . . . . ? O21 Ru21 C25 C24 -179.6(2) . . . . ? N21 Ru21 C25 C24 -100.2(3) . . . . ? C26 Ru21 C25 C24 132.1(4) . . . . ? C21 Ru21 C25 C24 102.6(3) . . . . ? C23 Ru21 C25 C24 28.7(3) . . . . ? C22 Ru21 C25 C24 66.3(3) . . . . ? Cl21 Ru21 C25 C24 -16.7(4) . . . . ? C24 C25 C26 C21 -0.7(7) . . . . ? Ru21 C25 C26 C21 53.8(4) . . . . ? C24 C25 C26 Ru21 -54.5(4) . . . . ? C22 C21 C26 C25 0.2(7) . . . . ? Ru21 C21 C26 C25 -53.5(4) . . . . ? C22 C21 C26 Ru21 53.8(4) . . . . ? O21 Ru21 C26 C25 -140.2(3) . . . . ? N21 Ru21 C26 C25 -62.1(3) . . . . ? C21 Ru21 C26 C25 131.8(4) . . . . ? C23 Ru21 C26 C25 66.1(3) . . . . ? C24 Ru21 C26 C25 29.6(3) . . . . ? C22 Ru21 C26 C25 103.9(3) . . . . ? Cl21 Ru21 C26 C25 129.5(4) . . . . ? O21 Ru21 C26 C21 88.0(3) . . . . ? N21 Ru21 C26 C21 166.0(3) . . . . ? C25 Ru21 C26 C21 -131.8(4) . . . . ? C23 Ru21 C26 C21 -65.8(3) . . . . ? C24 Ru21 C26 C21 -102.2(3) . . . . ? C22 Ru21 C26 C21 -28.0(3) . . . . ? Cl21 Ru21 C26 C21 -2.4(6) . . . . ? Ru21 O21 C27 O22 -177.4(3) . . . . ? Ru21 O21 C27 C28 -2.7(4) . . . . ? C29 N21 C28 C27 -171.4(3) . . . . ? Ru21 N21 C28 C27 -37.2(4) . . . . ? C29 N21 C28 C32 59.2(5) . . . . ? Ru21 N21 C28 C32 -166.7(3) . . . . ? O22 C27 C28 N21 -158.1(4) . . . . ? O21 C27 C28 N21 27.1(5) . . . . ? O22 C27 C28 C32 -31.2(6) . . . . ? O21 C27 C28 C32 154.1(3) . . . . ? C28 N21 C29 C30 -58.6(4) . . . . ? Ru21 N21 C29 C30 174.0(2) . . . . ? N21 C29 C30 C31 56.6(5) . . . . ? C29 C30 C31 C32 -54.1(5) . . . . ? N21 C28 C32 C31 -57.2(5) . . . . ? C27 C28 C32 C31 177.0(3) . . . . ? C30 C31 C32 C28 54.1(5) . . . . ? _diffrn_measured_fraction_theta_max 0.917 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 0.841 _refine_diff_density_min -0.346 _refine_diff_density_rms 0.095 # ---------------------------------------------------------- # data for compnd_8b (locally labelled as dan43as) data_compnd_8b _database_code_depnum_ccdc_archive 'CCDC 881060' #TrackingRef '- compnd_3_8b_cif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C51 H78 N3 O6 Ru3,3(B F4),3(C3 H6 O)' _chemical_formula_sum 'C60 H96 B3 F12 N3 O9 Ru3' _chemical_formula_weight 1567.04 _chemical_absolute_configuration rmad loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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 Hexagonal _symmetry_space_group_name_H-M P63 _symmetry_space_group_name_Hall 'P 6c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x-y, x, z+1/2' 'y, -x+y, z+1/2' '-y, x-y, z' '-x+y, -x, z' '-x, -y, z+1/2' _cell_length_a 19.161(3) _cell_length_b 19.161(3) _cell_length_c 10.4784(14) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 3331.6(8) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5667 _cell_measurement_theta_min 2.29 _cell_measurement_theta_max 27.17 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.352 _exptl_crystal_size_mid 0.137 _exptl_crystal_size_min 0.129 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.562 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1608 _exptl_absorpt_coefficient_mu 0.760 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.667 _exptl_absorpt_correction_T_max 0.890 _exptl_absorpt_process_details ; SADABS: Area-Detector Absorption Correction. (1996) Bruker-AXS within APEX2 package. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'Bruker SMART APEX CCD system' _diffrn_measurement_method '\w rotations with narrow frames' _diffrn_detector_area_resol_mean 8.26 _diffrn_standards_decay_% ? _diffrn_reflns_number 21325 _diffrn_reflns_av_R_equivalents 0.0524 _diffrn_reflns_av_sigmaI/netI 0.0534 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.13 _diffrn_reflns_theta_max 28.32 _reflns_number_total 4929 _reflns_number_gt 4289 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART v. 5.611 (Bruker AXS, 2000)' _computing_cell_refinement 'APEX2 v. 2008.4 (Bruker AXS, 2008)' _computing_data_reduction 'APEX2 v. 2008.4 (Bruker AXS, 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ORTEP _computing_publication_material ENCIFER _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. The asymmetric unit contains a third of a trinuclear Ru complex, a (B F4) counterion and an solvent (acetone) molecule. Free refinement of atomic positions and thermal parameters in acetone leads to unrealistic values. Therefore, atomic positions have been refined with restraints in C=O and C-C bond lenghts, atoms have been refined as isotropic. Hydrogen atoms of acetone molecule have not been included in the model. Hydrogen atoms of the cation have been included in the model in calculated positions and refined with a riding model. ; _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^)+(0.0373P)^2^+23.4217P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.06(10) _refine_ls_number_reflns 4929 _refine_ls_number_parameters 257 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.1011 _refine_ls_R_factor_gt 0.0890 _refine_ls_wR_factor_ref 0.1839 _refine_ls_wR_factor_gt 0.1784 _refine_ls_goodness_of_fit_ref 1.197 _refine_ls_restrained_S_all 1.199 _refine_ls_shift/su_max 0.037 _refine_ls_shift/su_mean 0.001 _iucr_refine_instructions_details ; TITL dan43as_P63 in P6(3) CELL 0.71073 19.1608 19.1608 10.4784 90.000 90.000 120.000 ZERR 2.00 0.0026 0.0026 0.0014 0.000 0.000 0.000 LATT -1 SYMM X - Y, X, 1/2 + Z SYMM Y, - X + Y, 1/2 + Z SYMM - Y, X - Y, Z SYMM - X + Y, - X, Z SYMM - X, - Y, 1/2 + Z SFAC C H N O B F RU UNIT 120 192 6 18 6 24 6 MERG 2 DFIX 1.540 0.020 C21 C20 DFIX 1.540 0.020 C20 C22 dfix 2.67 0.02 C21 C22 DFIX 1.21 0.02 C20 O3 FMAP 2 PLAN 20 ACTA 55.00 BOND $H CONF L.S. 4 TEMP -173.00 WGHT 0.037300 23.421700 FVAR 0.25322 RU 7 0.188351 0.706205 0.990334 11.00000 0.03388 0.05051 = 0.02016 0.00641 0.00491 0.02194 O1 4 0.316430 0.759109 0.997698 11.00000 0.04303 0.04784 = 0.02197 0.00668 0.00594 0.02429 O2 4 0.198557 0.622312 0.870531 11.00000 0.03241 0.04139 = 0.02278 0.00363 0.00320 0.02272 N1 3 0.225556 0.771121 0.813394 11.00000 0.02572 0.03398 = 0.02923 0.00522 0.00508 0.01431 AFIX 13 H1 2 0.189256 0.738475 0.751183 11.00000 -1.20000 AFIX 0 C1 1 0.178892 0.747267 1.178214 11.00000 0.03320 0.05759 = 0.02877 0.00111 0.00706 0.02526 C2 1 0.137145 0.772195 1.094777 11.00000 0.03986 0.05932 = 0.03664 0.00038 0.00613 0.02685 C3 1 0.079160 0.712906 1.008389 11.00000 0.05157 0.06781 = 0.02445 0.01850 0.01344 0.02618 C4 1 0.057700 0.631559 1.014109 11.00000 0.03124 0.05858 = 0.02711 0.00933 0.01310 0.01752 C5 1 0.095954 0.607357 1.107131 11.00000 0.02324 0.05828 = 0.02935 0.00057 0.01093 0.01622 C6 1 0.156311 0.664014 1.188155 11.00000 0.03178 0.04948 = 0.02327 0.00407 0.00577 0.02104 C7 1 0.243509 0.810516 1.262537 11.00000 0.04904 0.05477 = 0.02898 -0.00403 0.00271 0.02652 AFIX 137 H7A 2 0.220192 0.811275 1.345411 11.00000 -1.50000 H7B 2 0.265604 0.863480 1.221945 11.00000 -1.50000 H7C 2 0.286652 0.797827 1.274961 11.00000 -1.50000 AFIX 0 C8 1 0.153223 0.856970 1.098115 11.00000 0.08523 0.07386 = 0.04753 -0.00011 0.00608 0.05797 AFIX 137 H8A 2 0.152899 0.873037 1.186807 11.00000 -1.50000 H8B 2 0.111324 0.860564 1.049841 11.00000 -1.50000 H8C 2 0.205985 0.892889 1.059887 11.00000 -1.50000 AFIX 0 C9 1 0.034683 0.738563 0.911019 11.00000 0.06337 0.13727 = 0.03132 0.00827 -0.00175 0.06899 AFIX 137 H9A 2 0.030863 0.712785 0.828524 11.00000 -1.50000 H9B 2 0.064805 0.797251 0.900658 11.00000 -1.50000 H9C 2 -0.019595 0.721791 0.942636 11.00000 -1.50000 AFIX 0 C10 1 -0.001159 0.572364 0.919210 11.00000 0.03254 0.09502 = 0.03516 0.00465 0.00122 0.01979 AFIX 137 H10A 2 -0.051040 0.574791 0.920878 11.00000 -1.50000 H10B 2 -0.013093 0.517813 0.941514 11.00000 -1.50000 H10C 2 0.022356 0.585967 0.833484 11.00000 -1.50000 AFIX 0 C11 1 0.072698 0.520529 1.110228 11.00000 0.01956 0.04751 = 0.03128 0.00712 0.00425 -0.00414 AFIX 137 H11A 2 0.108385 0.513163 1.168779 11.00000 -1.50000 H11B 2 0.077592 0.503129 1.024380 11.00000 -1.50000 H11C 2 0.016844 0.488264 1.139561 11.00000 -1.50000 AFIX 0 C12 1 0.197859 0.638123 1.284705 11.00000 0.03319 0.05052 = 0.02719 0.00243 0.00165 0.01545 AFIX 137 H12A 2 0.157309 0.595439 1.338966 11.00000 -1.50000 H12B 2 0.234110 0.684353 1.337720 11.00000 -1.50000 H12C 2 0.229016 0.617842 1.239843 11.00000 -1.50000 AFIX 0 C13 1 0.351373 0.780089 0.893946 11.00000 0.03044 0.02779 = 0.02664 -0.00018 0.00397 0.01561 C14 1 0.306904 0.784516 0.775992 11.00000 0.04237 0.05329 = 0.02793 0.00935 0.00627 0.02706 AFIX 13 H14 2 0.300024 0.741830 0.714033 11.00000 -1.20000 AFIX 0 C15 1 0.232949 0.851643 0.802372 11.00000 0.08593 0.04951 = 0.04145 0.00809 0.00353 0.03591 AFIX 23 H15A 2 0.256183 0.883437 0.881185 11.00000 -1.20000 H15B 2 0.179697 0.846655 0.786589 11.00000 -1.20000 AFIX 0 C16 1 0.288540 0.890767 0.690234 11.00000 0.08036 0.04579 = 0.04477 0.01672 0.01692 0.03336 AFIX 23 H16A 2 0.259829 0.869651 0.608341 11.00000 -1.20000 H16B 2 0.312367 0.950040 0.691939 11.00000 -1.20000 AFIX 0 C17 1 0.351279 0.867582 0.709445 11.00000 0.06297 0.07152 = 0.04497 0.03201 0.00306 0.02148 AFIX 23 H17A 2 0.395553 0.907537 0.763751 11.00000 -1.20000 H17B 2 0.373990 0.863717 0.626629 11.00000 -1.20000 AFIX 0 B 5 0.075642 0.682962 0.531456 11.00000 0.03647 0.09994 = 0.04629 0.04612 0.02234 0.02354 F1 6 0.050287 0.644625 0.423441 11.00000 0.07147 0.13697 = 0.02530 0.00064 -0.00092 0.03454 F2 6 0.118920 0.768764 0.512083 11.00000 0.12683 0.08506 = 0.11384 0.03444 0.03836 0.02124 F3 6 0.010905 0.672928 0.608825 11.00000 0.06621 0.10886 = 0.04378 0.00188 0.02051 0.02754 F4 6 0.123862 0.668650 0.602586 11.00000 0.09548 0.12749 = 0.10964 -0.05335 -0.06236 0.06318 O3 4 -0.100080 0.838777 1.102494 11.00000 0.20827 C20 1 -0.082904 0.852092 0.986503 11.00000 0.16750 C21 1 -0.144060 0.830505 0.875757 11.00000 0.15323 C22 1 0.004425 0.890592 0.961461 11.00000 0.14803 HKLF 4 REM dan43am_P63 in P6(3) REM R1 = 0.0890 for 4289 Fo > 4sig(Fo) and 0.1011 for all 4929 data REM 257 parameters refined using 5 restraints END ; 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 Ru Ru 0.18835(4) 0.70620(4) 0.99033(13) 0.03448(19) Uani 1 1 d . . . O1 O 0.3164(3) 0.7591(3) 0.9977(9) 0.0369(13) Uani 1 1 d . . . O2 O 0.1986(4) 0.6223(4) 0.8705(6) 0.0303(13) Uani 1 1 d . . . N1 N 0.2256(5) 0.7711(5) 0.8134(7) 0.0299(16) Uani 1 1 d . . . H1 H 0.1893 0.7385 0.7512 0.036 Uiso 1 1 calc R . . C1 C 0.1789(6) 0.7473(7) 1.1782(9) 0.039(2) Uani 1 1 d . . . C2 C 0.1371(6) 0.7722(7) 1.0948(10) 0.044(3) Uani 1 1 d . . . C3 C 0.0792(6) 0.7129(7) 1.0084(11) 0.050(3) Uani 1 1 d . . . C4 C 0.0577(6) 0.6316(6) 1.0141(9) 0.041(3) Uani 1 1 d . . . C5 C 0.0960(5) 0.6074(7) 1.1071(9) 0.039(2) Uani 1 1 d . . . C6 C 0.1563(6) 0.6640(6) 1.1882(9) 0.035(2) Uani 1 1 d . . . C7 C 0.2435(7) 0.8105(7) 1.2625(10) 0.044(2) Uani 1 1 d . . . H7A H 0.2202 0.8113 1.3454 0.066 Uiso 1 1 calc R . . H7B H 0.2656 0.8635 1.2219 0.066 Uiso 1 1 calc R . . H7C H 0.2867 0.7978 1.2750 0.066 Uiso 1 1 calc R . . C8 C 0.1532(9) 0.8570(8) 1.0981(12) 0.061(3) Uani 1 1 d . . . H8A H 0.1529 0.8730 1.1868 0.091 Uiso 1 1 calc R . . H8B H 0.1113 0.8606 1.0498 0.091 Uiso 1 1 calc R . . H8C H 0.2060 0.8929 1.0599 0.091 Uiso 1 1 calc R . . C9 C 0.0347(8) 0.7386(10) 0.9110(11) 0.069(4) Uani 1 1 d . . . H9A H 0.0309 0.7128 0.8285 0.103 Uiso 1 1 calc R . . H9B H 0.0648 0.7973 0.9007 0.103 Uiso 1 1 calc R . . H9C H -0.0196 0.7218 0.9426 0.103 Uiso 1 1 calc R . . C10 C -0.0012(6) 0.5724(8) 0.9192(11) 0.060(3) Uani 1 1 d . . . H10A H -0.0510 0.5748 0.9209 0.089 Uiso 1 1 calc R . . H10B H -0.0131 0.5178 0.9415 0.089 Uiso 1 1 calc R . . H10C H 0.0224 0.5860 0.8335 0.089 Uiso 1 1 calc R . . C11 C 0.0727(5) 0.5205(6) 1.1102(10) 0.042(3) Uani 1 1 d . . . H11A H 0.1084 0.5132 1.1688 0.063 Uiso 1 1 calc R . . H11B H 0.0776 0.5031 1.0244 0.063 Uiso 1 1 calc R . . H11C H 0.0168 0.4883 1.1396 0.063 Uiso 1 1 calc R . . C12 C 0.1979(6) 0.6381(7) 1.2847(9) 0.039(2) Uani 1 1 d . . . H12A H 0.1573 0.5954 1.3390 0.059 Uiso 1 1 calc R . . H12B H 0.2341 0.6844 1.3377 0.059 Uiso 1 1 calc R . . H12C H 0.2290 0.6178 1.2398 0.059 Uiso 1 1 calc R . . C13 C 0.3514(5) 0.7801(5) 0.8939(8) 0.0278(18) Uani 1 1 d . . . C14 C 0.3069(6) 0.7845(7) 0.7760(9) 0.040(2) Uani 1 1 d . . . H14 H 0.3000 0.7418 0.7140 0.048 Uiso 1 1 calc R . . C15 C 0.2329(9) 0.8516(7) 0.8024(12) 0.058(3) Uani 1 1 d . . . H15A H 0.2562 0.8834 0.8812 0.070 Uiso 1 1 calc R . . H15B H 0.1797 0.8467 0.7866 0.070 Uiso 1 1 calc R . . C16 C 0.2885(8) 0.8908(7) 0.6902(11) 0.056(3) Uani 1 1 d . . . H16A H 0.2598 0.8697 0.6083 0.067 Uiso 1 1 calc R . . H16B H 0.3124 0.9500 0.6919 0.067 Uiso 1 1 calc R . . C17 C 0.3513(8) 0.8676(8) 0.7094(12) 0.065(4) Uani 1 1 d . . . H17A H 0.3956 0.9075 0.7638 0.078 Uiso 1 1 calc R . . H17B H 0.3740 0.8637 0.6266 0.078 Uiso 1 1 calc R . . B B 0.0756(9) 0.6830(12) 0.5315(14) 0.066(5) Uani 1 1 d . . . F1 F 0.0503(5) 0.6446(6) 0.4234(7) 0.086(3) Uani 1 1 d . . . F2 F 0.1189(6) 0.7688(5) 0.5121(14) 0.123(4) Uani 1 1 d . . . F3 F 0.0109(5) 0.6729(5) 0.6088(7) 0.080(2) Uani 1 1 d . . . F4 F 0.1239(6) 0.6687(6) 0.6026(11) 0.108(4) Uani 1 1 d . . . O3 O -0.1001(14) 0.8388(15) 1.102(2) 0.208(9) Uiso 1 1 d D . . C20 C -0.0829(14) 0.8521(16) 0.987(2) 0.167(9) Uiso 1 1 d D . . C21 C -0.1441(13) 0.8305(17) 0.876(3) 0.153(10) Uiso 1 1 d D . . C22 C 0.0044(13) 0.8906(14) 0.961(3) 0.148(9) Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru 0.0339(3) 0.0505(4) 0.0202(3) 0.0064(5) 0.0049(5) 0.0219(3) O1 0.043(3) 0.048(3) 0.022(3) 0.007(4) 0.006(4) 0.024(3) O2 0.032(3) 0.041(4) 0.023(3) 0.004(3) 0.003(2) 0.023(3) N1 0.026(4) 0.034(4) 0.029(4) 0.005(3) 0.005(3) 0.014(4) C1 0.033(5) 0.058(7) 0.029(5) 0.001(4) 0.007(4) 0.025(5) C2 0.040(6) 0.059(7) 0.037(6) 0.000(5) 0.006(4) 0.027(5) C3 0.052(6) 0.068(6) 0.024(7) 0.018(5) 0.013(5) 0.026(5) C4 0.031(4) 0.059(6) 0.027(7) 0.009(4) 0.013(4) 0.018(4) C5 0.023(5) 0.058(7) 0.029(5) 0.001(4) 0.011(4) 0.016(5) C6 0.032(5) 0.049(6) 0.023(5) 0.004(4) 0.006(4) 0.021(4) C7 0.049(6) 0.055(7) 0.029(5) -0.004(4) 0.003(4) 0.027(5) C8 0.085(10) 0.074(9) 0.048(7) 0.000(6) 0.006(6) 0.058(8) C9 0.063(8) 0.137(13) 0.031(6) 0.008(7) -0.002(5) 0.069(9) C10 0.033(6) 0.095(10) 0.035(6) 0.005(6) 0.001(5) 0.020(6) C11 0.020(4) 0.048(6) 0.031(5) 0.007(4) 0.004(4) -0.004(4) C12 0.033(5) 0.051(6) 0.027(5) 0.002(4) 0.002(4) 0.015(5) C13 0.030(5) 0.028(4) 0.027(4) 0.000(4) 0.004(4) 0.016(4) C14 0.042(6) 0.053(6) 0.028(5) 0.009(4) 0.006(4) 0.027(5) C15 0.086(10) 0.050(7) 0.041(7) 0.008(5) 0.004(6) 0.036(7) C16 0.080(9) 0.046(6) 0.045(7) 0.017(5) 0.017(6) 0.033(7) C17 0.063(8) 0.072(9) 0.045(7) 0.032(6) 0.003(6) 0.021(7) B 0.036(7) 0.100(13) 0.046(8) 0.046(8) 0.022(6) 0.024(8) F1 0.071(6) 0.137(9) 0.025(4) 0.001(4) -0.001(4) 0.035(6) F2 0.127(8) 0.085(6) 0.114(11) 0.034(7) 0.038(8) 0.021(5) F3 0.066(5) 0.109(7) 0.044(4) 0.002(4) 0.021(4) 0.028(5) F4 0.095(7) 0.127(8) 0.110(8) -0.053(7) -0.062(6) 0.063(7) _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 Ru O2 2.124(6) . ? Ru O1 2.137(6) . ? Ru N1 2.146(7) . ? Ru C1 2.161(10) . ? Ru C3 2.168(11) . ? Ru C4 2.190(9) . ? Ru C6 2.198(9) . ? Ru C5 2.206(10) . ? Ru C2 2.236(11) . ? O1 C13 1.234(12) . ? O2 C13 1.258(10) 4_665 ? N1 C15 1.482(14) . ? N1 C14 1.500(12) . ? N1 H1 0.9300 . ? C1 C2 1.419(15) . ? C1 C6 1.433(15) . ? C1 C7 1.511(14) . ? C2 C3 1.443(16) . ? C2 C8 1.495(16) . ? C3 C4 1.400(15) . ? C3 C9 1.558(16) . ? C4 C5 1.429(14) . ? C4 C10 1.506(15) . ? C5 C6 1.408(14) . ? C5 C11 1.492(15) . ? C6 C12 1.516(13) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 O2 1.258(10) 5_565 ? C13 C14 1.527(13) . ? C14 C17 1.546(15) . ? C14 H14 1.0000 . ? C15 C16 1.510(16) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.489(18) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? B F1 1.304(19) . ? B F4 1.318(17) . ? B F3 1.412(16) . ? B F2 1.438(19) . ? O3 C20 1.252(18) . ? C20 C22 1.476(17) . ? C20 C21 1.551(17) . ? 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 O2 Ru O1 82.1(3) . . ? O2 Ru N1 78.4(3) . . ? O1 Ru N1 77.7(3) . . ? O2 Ru C1 150.5(3) . . ? O1 Ru C1 94.6(4) . . ? N1 Ru C1 129.8(4) . . ? O2 Ru C3 123.6(4) . . ? O1 Ru C3 151.9(4) . . ? N1 Ru C3 95.3(4) . . ? C1 Ru C3 68.9(4) . . ? O2 Ru C4 94.6(3) . . ? O1 Ru C4 166.5(3) . . ? N1 Ru C4 114.6(3) . . ? C1 Ru C4 81.8(4) . . ? C3 Ru C4 37.5(4) . . ? O2 Ru C6 113.2(3) . . ? O1 Ru C6 100.6(3) . . ? N1 Ru C6 168.1(4) . . ? C1 Ru C6 38.4(4) . . ? C3 Ru C6 80.7(4) . . ? C4 Ru C6 68.6(4) . . ? O2 Ru C5 90.9(3) . . ? O1 Ru C5 128.7(3) . . ? N1 Ru C5 150.3(3) . . ? C1 Ru C5 68.3(4) . . ? C3 Ru C5 67.6(4) . . ? C4 Ru C5 37.9(4) . . ? C6 Ru C5 37.3(4) . . ? O2 Ru C2 161.7(3) . . ? O1 Ru C2 116.0(4) . . ? N1 Ru C2 102.0(4) . . ? C1 Ru C2 37.6(4) . . ? C3 Ru C2 38.2(4) . . ? C4 Ru C2 68.4(4) . . ? C6 Ru C2 68.0(4) . . ? C5 Ru C2 79.8(4) . . ? C13 O1 Ru 115.5(7) . . ? C13 O2 Ru 131.4(6) 4_665 . ? C15 N1 C14 104.6(9) . . ? C15 N1 Ru 120.1(6) . . ? C14 N1 Ru 109.9(5) . . ? C15 N1 H1 107.2 . . ? C14 N1 H1 107.2 . . ? Ru N1 H1 107.2 . . ? C2 C1 C6 120.8(10) . . ? C2 C1 C7 117.7(10) . . ? C6 C1 C7 121.4(9) . . ? C2 C1 Ru 74.1(6) . . ? C6 C1 Ru 72.2(6) . . ? C7 C1 Ru 129.8(7) . . ? C1 C2 C3 117.6(10) . . ? C1 C2 C8 120.4(10) . . ? C3 C2 C8 122.0(10) . . ? C1 C2 Ru 68.3(6) . . ? C3 C2 Ru 68.3(6) . . ? C8 C2 Ru 135.7(8) . . ? C4 C3 C2 122.1(10) . . ? C4 C3 C9 118.5(11) . . ? C2 C3 C9 119.3(11) . . ? C4 C3 Ru 72.1(6) . . ? C2 C3 Ru 73.5(6) . . ? C9 C3 Ru 131.1(8) . . ? C3 C4 C5 118.5(10) . . ? C3 C4 C10 120.2(10) . . ? C5 C4 C10 121.2(10) . . ? C3 C4 Ru 70.4(6) . . ? C5 C4 Ru 71.6(5) . . ? C10 C4 Ru 126.7(7) . . ? C6 C5 C4 121.2(10) . . ? C6 C5 C11 121.3(9) . . ? C4 C5 C11 117.5(9) . . ? C6 C5 Ru 71.0(5) . . ? C4 C5 Ru 70.4(6) . . ? C11 C5 Ru 129.3(6) . . ? C5 C6 C1 119.3(9) . . ? C5 C6 C12 120.9(10) . . ? C1 C6 C12 119.8(9) . . ? C5 C6 Ru 71.7(5) . . ? C1 C6 Ru 69.4(5) . . ? C12 C6 Ru 130.8(6) . . ? C1 C7 H7A 109.5 . . ? C1 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C1 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C2 C8 H8A 109.5 . . ? C2 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C2 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C3 C9 H9A 109.5 . . ? C3 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C3 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C4 C10 H10A 109.5 . . ? C4 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C4 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C5 C11 H11A 109.5 . . ? C5 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C5 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C6 C12 H12A 109.5 . . ? C6 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C6 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? O1 C13 O2 127.4(9) . 5_565 ? O1 C13 C14 120.3(8) . . ? O2 C13 C14 112.3(8) 5_565 . ? N1 C14 C13 109.9(7) . . ? N1 C14 C17 106.5(9) . . ? C13 C14 C17 112.8(9) . . ? N1 C14 H14 109.2 . . ? C13 C14 H14 109.2 . . ? C17 C14 H14 109.2 . . ? N1 C15 C16 104.7(10) . . ? N1 C15 H15A 110.8 . . ? C16 C15 H15A 110.8 . . ? N1 C15 H15B 110.8 . . ? C16 C15 H15B 110.8 . . ? H15A C15 H15B 108.9 . . ? C17 C16 C15 102.8(10) . . ? C17 C16 H16A 111.2 . . ? C15 C16 H16A 111.2 . . ? C17 C16 H16B 111.2 . . ? C15 C16 H16B 111.2 . . ? H16A C16 H16B 109.1 . . ? C16 C17 C14 104.9(10) . . ? C16 C17 H17A 110.8 . . ? C14 C17 H17A 110.8 . . ? C16 C17 H17B 110.8 . . ? C14 C17 H17B 110.8 . . ? H17A C17 H17B 108.8 . . ? F1 B F4 118.4(18) . . ? F1 B F3 111.5(13) . . ? F4 B F3 107.8(12) . . ? F1 B F2 111.2(11) . . ? F4 B F2 104.7(14) . . ? F3 B F2 101.6(15) . . ? O3 C20 C22 113(2) . . ? O3 C20 C21 126(2) . . ? C22 C20 C21 121.1(18) . . ? 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 O2 Ru O1 C13 59.4(6) . . . . ? N1 Ru O1 C13 -20.3(6) . . . . ? C1 Ru O1 C13 -150.1(6) . . . . ? C3 Ru O1 C13 -98.2(10) . . . . ? C4 Ru O1 C13 136.0(14) . . . . ? C6 Ru O1 C13 171.6(6) . . . . ? C5 Ru O1 C13 144.2(6) . . . . ? C2 Ru O1 C13 -117.8(7) . . . . ? O1 Ru O2 C13 67.1(8) . . . 4_665 ? N1 Ru O2 C13 146.0(8) . . . 4_665 ? C1 Ru O2 C13 -18.2(11) . . . 4_665 ? C3 Ru O2 C13 -125.4(8) . . . 4_665 ? C4 Ru O2 C13 -99.8(8) . . . 4_665 ? C6 Ru O2 C13 -31.1(8) . . . 4_665 ? C5 Ru O2 C13 -61.9(8) . . . 4_665 ? C2 Ru O2 C13 -120.9(12) . . . 4_665 ? O2 Ru N1 C15 177.1(9) . . . . ? O1 Ru N1 C15 -98.6(9) . . . . ? C1 Ru N1 C15 -13.0(11) . . . . ? C3 Ru N1 C15 53.8(9) . . . . ? C4 Ru N1 C15 87.3(9) . . . . ? C6 Ru N1 C15 -16(2) . . . . ? C5 Ru N1 C15 106.1(10) . . . . ? C2 Ru N1 C15 15.7(9) . . . . ? O2 Ru N1 C14 -61.6(6) . . . . ? O1 Ru N1 C14 22.7(6) . . . . ? C1 Ru N1 C14 108.3(7) . . . . ? C3 Ru N1 C14 175.1(7) . . . . ? C4 Ru N1 C14 -151.4(7) . . . . ? C6 Ru N1 C14 105.4(16) . . . . ? C5 Ru N1 C14 -132.6(8) . . . . ? C2 Ru N1 C14 137.0(7) . . . . ? O2 Ru C1 C2 -149.9(6) . . . . ? O1 Ru C1 C2 128.1(6) . . . . ? N1 Ru C1 C2 50.3(8) . . . . ? C3 Ru C1 C2 -28.5(6) . . . . ? C4 Ru C1 C2 -65.0(6) . . . . ? C6 Ru C1 C2 -130.6(9) . . . . ? C5 Ru C1 C2 -101.9(7) . . . . ? O2 Ru C1 C6 -19.3(10) . . . . ? O1 Ru C1 C6 -101.3(5) . . . . ? N1 Ru C1 C6 -179.0(5) . . . . ? C3 Ru C1 C6 102.1(6) . . . . ? C4 Ru C1 C6 65.6(6) . . . . ? C5 Ru C1 C6 28.8(5) . . . . ? C2 Ru C1 C6 130.6(9) . . . . ? O2 Ru C1 C7 97.1(11) . . . . ? O1 Ru C1 C7 15.1(10) . . . . ? N1 Ru C1 C7 -62.6(11) . . . . ? C3 Ru C1 C7 -141.5(11) . . . . ? C4 Ru C1 C7 -178.0(11) . . . . ? C6 Ru C1 C7 116.4(12) . . . . ? C5 Ru C1 C7 145.2(11) . . . . ? C2 Ru C1 C7 -113.0(13) . . . . ? C6 C1 C2 C3 -8.3(14) . . . . ? C7 C1 C2 C3 176.0(9) . . . . ? Ru C1 C2 C3 49.0(8) . . . . ? C6 C1 C2 C8 171.4(10) . . . . ? C7 C1 C2 C8 -4.2(15) . . . . ? Ru C1 C2 C8 -131.3(10) . . . . ? C6 C1 C2 Ru -57.3(8) . . . . ? C7 C1 C2 Ru 127.0(9) . . . . ? O2 Ru C2 C1 128.0(10) . . . . ? O1 Ru C2 C1 -60.8(7) . . . . ? N1 Ru C2 C1 -142.8(6) . . . . ? C3 Ru C2 C1 134.0(9) . . . . ? C4 Ru C2 C1 105.2(7) . . . . ? C6 Ru C2 C1 30.5(6) . . . . ? C5 Ru C2 C1 67.5(6) . . . . ? O2 Ru C2 C3 -5.9(14) . . . . ? O1 Ru C2 C3 165.2(6) . . . . ? N1 Ru C2 C3 83.2(6) . . . . ? C1 Ru C2 C3 -134.0(9) . . . . ? C4 Ru C2 C3 -28.7(6) . . . . ? C6 Ru C2 C3 -103.4(7) . . . . ? C5 Ru C2 C3 -66.5(6) . . . . ? O2 Ru C2 C8 -120.0(13) . . . . ? O1 Ru C2 C8 51.1(13) . . . . ? N1 Ru C2 C8 -30.9(12) . . . . ? C1 Ru C2 C8 111.9(14) . . . . ? C3 Ru C2 C8 -114.1(14) . . . . ? C4 Ru C2 C8 -142.8(13) . . . . ? C6 Ru C2 C8 142.5(13) . . . . ? C5 Ru C2 C8 179.4(12) . . . . ? C1 C2 C3 C4 6.6(15) . . . . ? C8 C2 C3 C4 -173.1(10) . . . . ? Ru C2 C3 C4 55.6(9) . . . . ? C1 C2 C3 C9 -177.3(9) . . . . ? C8 C2 C3 C9 2.9(16) . . . . ? Ru C2 C3 C9 -128.3(10) . . . . ? C1 C2 C3 Ru -49.0(8) . . . . ? C8 C2 C3 Ru 131.3(10) . . . . ? O2 Ru C3 C4 45.0(7) . . . . ? O1 Ru C3 C4 -161.8(7) . . . . ? N1 Ru C3 C4 124.6(6) . . . . ? C1 Ru C3 C4 -104.6(7) . . . . ? C6 Ru C3 C4 -66.7(6) . . . . ? C5 Ru C3 C4 -30.3(6) . . . . ? C2 Ru C3 C4 -132.7(9) . . . . ? O2 Ru C3 C2 177.8(5) . . . . ? O1 Ru C3 C2 -29.1(12) . . . . ? N1 Ru C3 C2 -102.7(6) . . . . ? C1 Ru C3 C2 28.1(6) . . . . ? C4 Ru C3 C2 132.7(9) . . . . ? C6 Ru C3 C2 66.0(6) . . . . ? C5 Ru C3 C2 102.4(7) . . . . ? O2 Ru C3 C9 -67.5(13) . . . . ? O1 Ru C3 C9 85.6(15) . . . . ? N1 Ru C3 C9 12.1(13) . . . . ? C1 Ru C3 C9 142.9(13) . . . . ? C4 Ru C3 C9 -112.5(15) . . . . ? C6 Ru C3 C9 -179.2(13) . . . . ? C5 Ru C3 C9 -142.8(14) . . . . ? C2 Ru C3 C9 114.8(14) . . . . ? C2 C3 C4 C5 -1.3(15) . . . . ? C9 C3 C4 C5 -177.3(9) . . . . ? Ru C3 C4 C5 55.0(8) . . . . ? C2 C3 C4 C10 -178.1(10) . . . . ? C9 C3 C4 C10 5.9(15) . . . . ? Ru C3 C4 C10 -121.8(9) . . . . ? C2 C3 C4 Ru -56.2(9) . . . . ? C9 C3 C4 Ru 127.7(10) . . . . ? O2 Ru C4 C3 -143.7(6) . . . . ? O1 Ru C4 C3 141.1(14) . . . . ? N1 Ru C4 C3 -64.4(7) . . . . ? C1 Ru C4 C3 65.8(7) . . . . ? C6 Ru C4 C3 103.2(7) . . . . ? C5 Ru C4 C3 130.7(9) . . . . ? C2 Ru C4 C3 29.3(7) . . . . ? O2 Ru C4 C5 85.6(6) . . . . ? O1 Ru C4 C5 10.4(18) . . . . ? N1 Ru C4 C5 164.9(5) . . . . ? C1 Ru C4 C5 -64.9(6) . . . . ? C3 Ru C4 C5 -130.7(9) . . . . ? C6 Ru C4 C5 -27.5(6) . . . . ? C2 Ru C4 C5 -101.4(7) . . . . ? O2 Ru C4 C10 -30.2(10) . . . . ? O1 Ru C4 C10 -105.3(16) . . . . ? N1 Ru C4 C10 49.2(11) . . . . ? C1 Ru C4 C10 179.3(11) . . . . ? C3 Ru C4 C10 113.6(12) . . . . ? C6 Ru C4 C10 -143.3(11) . . . . ? C5 Ru C4 C10 -115.7(12) . . . . ? C2 Ru C4 C10 142.8(11) . . . . ? C3 C4 C5 C6 -2.6(13) . . . . ? C10 C4 C5 C6 174.2(9) . . . . ? Ru C4 C5 C6 51.8(8) . . . . ? C3 C4 C5 C11 -179.3(9) . . . . ? C10 C4 C5 C11 -2.6(13) . . . . ? Ru C4 C5 C11 -124.9(8) . . . . ? C3 C4 C5 Ru -54.4(8) . . . . ? C10 C4 C5 Ru 122.4(9) . . . . ? O2 Ru C5 C6 128.9(6) . . . . ? O1 Ru C5 C6 48.4(7) . . . . ? N1 Ru C5 C6 -163.3(6) . . . . ? C1 Ru C5 C6 -29.5(6) . . . . ? C3 Ru C5 C6 -104.8(7) . . . . ? C4 Ru C5 C6 -134.7(9) . . . . ? C2 Ru C5 C6 -66.9(6) . . . . ? O2 Ru C5 C4 -96.3(6) . . . . ? O1 Ru C5 C4 -176.9(5) . . . . ? N1 Ru C5 C4 -28.6(10) . . . . ? C1 Ru C5 C4 105.2(7) . . . . ? C3 Ru C5 C4 29.9(6) . . . . ? C6 Ru C5 C4 134.7(9) . . . . ? C2 Ru C5 C4 67.8(6) . . . . ? O2 Ru C5 C11 13.6(9) . . . . ? O1 Ru C5 C11 -67.0(10) . . . . ? N1 Ru C5 C11 81.4(11) . . . . ? C1 Ru C5 C11 -144.9(10) . . . . ? C3 Ru C5 C11 139.9(10) . . . . ? C4 Ru C5 C11 109.9(11) . . . . ? C6 Ru C5 C11 -115.3(11) . . . . ? C2 Ru C5 C11 177.7(10) . . . . ? C4 C5 C6 C1 0.9(13) . . . . ? C11 C5 C6 C1 177.5(8) . . . . ? Ru C5 C6 C1 52.4(8) . . . . ? C4 C5 C6 C12 -178.7(8) . . . . ? C11 C5 C6 C12 -2.1(13) . . . . ? Ru C5 C6 C12 -127.2(8) . . . . ? C4 C5 C6 Ru -51.5(8) . . . . ? C11 C5 C6 Ru 125.1(8) . . . . ? C2 C1 C6 C5 4.7(14) . . . . ? C7 C1 C6 C5 -179.8(9) . . . . ? Ru C1 C6 C5 -53.4(8) . . . . ? C2 C1 C6 C12 -175.7(9) . . . . ? C7 C1 C6 C12 -0.2(14) . . . . ? Ru C1 C6 C12 126.2(8) . . . . ? C2 C1 C6 Ru 58.2(8) . . . . ? C7 C1 C6 Ru -126.3(9) . . . . ? O2 Ru C6 C5 -57.8(6) . . . . ? O1 Ru C6 C5 -143.6(6) . . . . ? N1 Ru C6 C5 136.0(15) . . . . ? C1 Ru C6 C5 132.4(9) . . . . ? C3 Ru C6 C5 64.9(6) . . . . ? C4 Ru C6 C5 28.0(6) . . . . ? C2 Ru C6 C5 102.5(7) . . . . ? O2 Ru C6 C1 169.8(5) . . . . ? O1 Ru C6 C1 84.0(6) . . . . ? N1 Ru C6 C1 3.6(18) . . . . ? C3 Ru C6 C1 -67.5(6) . . . . ? C4 Ru C6 C1 -104.4(6) . . . . ? C5 Ru C6 C1 -132.4(9) . . . . ? C2 Ru C6 C1 -30.0(6) . . . . ? O2 Ru C6 C12 57.6(10) . . . . ? O1 Ru C6 C12 -28.2(10) . . . . ? N1 Ru C6 C12 -108.6(17) . . . . ? C1 Ru C6 C12 -112.2(11) . . . . ? C3 Ru C6 C12 -179.7(10) . . . . ? C4 Ru C6 C12 143.4(11) . . . . ? C5 Ru C6 C12 115.4(12) . . . . ? C2 Ru C6 C12 -142.2(10) . . . . ? Ru O1 C13 O2 -168.8(7) . . . 5_565 ? Ru O1 C13 C14 13.0(10) . . . . ? C15 N1 C14 C13 107.2(9) . . . . ? Ru N1 C14 C13 -23.0(9) . . . . ? C15 N1 C14 C17 -15.2(11) . . . . ? Ru N1 C14 C17 -145.4(7) . . . . ? O1 C13 C14 N1 7.3(12) . . . . ? O2 C13 C14 N1 -171.2(8) 5_565 . . . ? O1 C13 C14 C17 125.9(10) . . . . ? O2 C13 C14 C17 -52.5(12) 5_565 . . . ? C14 N1 C15 C16 35.0(12) . . . . ? Ru N1 C15 C16 158.8(8) . . . . ? N1 C15 C16 C17 -41.5(13) . . . . ? C15 C16 C17 C14 31.0(13) . . . . ? N1 C14 C17 C16 -10.2(12) . . . . ? C13 C14 C17 C16 -130.8(10) . . . . ? _diffrn_measured_fraction_theta_max 0.964 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 2.134 _refine_diff_density_min -2.311 _refine_diff_density_rms 0.140