#------------------------------------------------------------------------------ #$Date: 2019-11-08 06:19:29 +0200 (Fri, 08 Nov 2019) $ #$Revision: 225388 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/05/90/7059029.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_7059029 loop_ _publ_author_name 'Li, Shasha' 'Xu, Lei' 'Jiang, Liping' 'Zhang, Guofang' 'Zhang, Wei-Qiang' 'Gao, Ziwei' _publ_section_title ; Activation reactions of 2-pyridyl and 2-pyrimidinyl alkynes with Ru3(CO)12 ; _journal_name_full 'New Journal of Chemistry' _journal_paper_doi 10.1039/C9NJ04958D _journal_year 2019 _chemical_formula_sum 'C22 H11 N O8 Ru3' _chemical_formula_weight 720.53 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2014/7 _audit_update_record ; 2019-11-04 deposited with the CCDC. 2019-11-07 downloaded from the CCDC. ; _cell_angle_alpha 91.735(5) _cell_angle_beta 94.157(5) _cell_angle_gamma 102.600(5) _cell_formula_units_Z 2 _cell_length_a 8.1534(15) _cell_length_b 9.9791(19) _cell_length_c 14.213(3) _cell_measurement_reflns_used 36025 _cell_measurement_temperature 153(2) _cell_measurement_theta_max 26.38 _cell_measurement_theta_min 3.70 _cell_volume 1124.3(4) _computing_cell_refinement 'SAINT (Bruker AXS Inc., 2012)' _computing_data_collection 'APEX2 (Bruker AXS Inc., 2012)' _computing_data_reduction 'SAINT (Bruker AXS Inc., 2012)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2014)' _computing_publication_material 'SHELXTL (Sheldrick, 2014)' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_structure_solution 'SHELXS (Sheldrick, 2014)' _diffrn_ambient_temperature 153(2) _diffrn_measured_fraction_theta_full 0.981 _diffrn_measured_fraction_theta_max 0.983 _diffrn_measurement_device_type 'Bruker APEX II CCD' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0283 _diffrn_reflns_av_unetI/netI 0.0136 _diffrn_reflns_Laue_measured_fraction_full 0.981 _diffrn_reflns_Laue_measured_fraction_max 0.983 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_number 40777 _diffrn_reflns_point_group_measured_fraction_full 0.981 _diffrn_reflns_point_group_measured_fraction_max 0.983 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 26.000 _diffrn_reflns_theta_min 3.478 _exptl_absorpt_coefficient_mu 2.038 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details sadabs _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 2.128 _exptl_crystal_description prism _exptl_crystal_F_000 692 _exptl_crystal_size_max 0.150 _exptl_crystal_size_mid 0.130 _exptl_crystal_size_min 0.100 _exptl_transmission_factor_max 0.7454 _exptl_transmission_factor_min 0.6061 _refine_diff_density_max 0.375 _refine_diff_density_min -0.566 _refine_diff_density_rms 0.076 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.136 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 308 _refine_ls_number_reflns 4338 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.136 _refine_ls_R_factor_all 0.0166 _refine_ls_R_factor_gt 0.0163 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0194P)^2^+0.9006P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0411 _refine_ls_wR_factor_ref 0.0413 _reflns_Friedel_coverage 0.000 _reflns_number_gt 4287 _reflns_number_total 4338 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c9nj04958d2.cif _cod_data_source_block 2a _cod_original_cell_volume 1124.4(4) _cod_database_code 7059029 _shelx_shelxl_version_number 2014/7 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_min 0.750 _shelx_estimated_absorpt_t_max 0.822 _shelx_res_file ; 2a.res created by SHELXL-2014/7 TITL 1 in P-1 CELL 0.71073 8.1534 9.9791 14.2133 91.735 94.157 102.600 ZERR 2.00 0.0015 0.0019 0.0027 0.005 0.005 0.005 LATT 1 SFAC C H N O Ru UNIT 44 22 2 16 6 OMIT 3 2 1 OMIT -3.00 52.00 L.S. 4 ACTA BOND FMAP 2 PLAN 5 size 0.15 0.13 0.10 TEMP -120.150 WGHT 0.019400 0.900600 FVAR 0.21641 RU2 5 0.747652 0.748958 0.665989 11.00000 0.01423 0.01016 = 0.01499 -0.00089 0.00200 0.00143 RU1 5 0.631425 1.000857 0.661485 11.00000 0.01100 0.01291 = 0.01599 0.00177 0.00038 0.00277 RU3 5 0.667309 0.860179 0.834071 11.00000 0.01162 0.01026 = 0.01359 0.00136 0.00187 0.00167 N1 3 0.894283 1.103731 0.685494 11.00000 0.01338 0.01387 = 0.01878 0.00208 0.00257 0.00231 O2 4 0.566294 1.137157 0.837004 11.00000 0.02937 0.01895 = 0.02585 -0.00167 0.00130 0.01142 O3 4 0.269207 0.846540 0.618060 11.00000 0.01582 0.02979 = 0.04041 -0.00090 -0.00419 -0.00142 O8 4 0.685561 0.990385 1.030713 11.00000 0.02443 0.04519 = 0.01728 -0.00687 -0.00014 0.00908 O7 4 0.296621 0.721915 0.835998 11.00000 0.01792 0.03825 = 0.05093 0.00719 0.00566 -0.00536 O1 4 0.542359 1.255368 0.583503 11.00000 0.03069 0.02537 = 0.03933 0.01407 -0.00286 0.01057 C16 1 0.602184 1.045417 0.795400 11.00000 0.01064 0.01381 = 0.01931 0.00256 -0.00032 0.00087 C22 1 0.678825 0.937005 0.958124 11.00000 0.01396 0.02199 = 0.02160 0.00521 0.00174 0.00605 C1 1 0.993813 1.032650 0.733894 11.00000 0.01391 0.01283 = 0.01362 -0.00023 0.00306 0.00264 C6 1 0.910266 0.893328 0.757932 11.00000 0.01086 0.01163 = 0.01850 0.00036 0.00246 0.00362 C3 1 1.231797 1.222922 0.735330 11.00000 0.01441 0.01962 = 0.02960 0.00024 0.00292 -0.00204 AFIX 43 H3 2 1.347167 1.263618 0.752311 11.00000 -1.20000 AFIX 0 C2 1 1.163662 1.089993 0.758993 11.00000 0.01491 0.01737 = 0.01807 0.00041 0.00120 0.00338 AFIX 43 H2 2 1.232111 1.038196 0.792094 11.00000 -1.20000 AFIX 0 C21 1 0.434252 0.777080 0.834617 11.00000 0.02345 0.01977 = 0.02206 0.00407 0.00254 0.00433 C17 1 0.405527 0.904511 0.634713 11.00000 0.02256 0.01777 = 0.02003 0.00162 0.00187 0.00735 C15 1 0.578176 1.157247 0.609764 11.00000 0.01451 0.02484 = 0.01869 0.00262 -0.00042 0.00203 O6 4 0.980555 0.563976 0.610254 11.00000 0.04835 0.03159 = 0.06639 -0.00025 0.01849 0.02432 C9 1 0.731764 0.649635 0.795101 11.00000 0.02139 0.01111 = 0.02127 0.00211 0.00369 0.00511 C13 1 0.866064 0.656488 0.961010 11.00000 0.02761 0.01942 = 0.02064 0.00465 0.00455 0.01246 C8 1 0.849337 0.716308 0.870898 11.00000 0.01720 0.01317 = 0.02069 0.00326 0.00446 0.00767 C5 1 0.962236 1.232649 0.662680 11.00000 0.01821 0.01578 = 0.03104 0.00799 0.00360 0.00346 AFIX 43 H5 2 0.892351 1.282423 0.628720 11.00000 -1.20000 AFIX 0 C18 1 0.788635 0.855758 0.553037 11.00000 0.01463 0.01997 = 0.01969 -0.00307 -0.00019 0.00285 C4 1 1.129115 1.296082 0.686372 11.00000 0.02104 0.01352 = 0.03840 0.00744 0.00646 -0.00165 AFIX 43 H4 2 1.172659 1.387673 0.669559 11.00000 -1.20000 AFIX 0 C10 1 0.630647 0.518741 0.813861 11.00000 0.03262 0.01450 = 0.03025 0.00164 0.00422 -0.00035 AFIX 43 H10 2 0.550962 0.469985 0.765833 11.00000 -1.20000 AFIX 0 C20 1 0.893253 0.633265 0.630091 11.00000 0.02769 0.01812 = 0.02961 0.00140 0.00543 0.00425 C11 1 0.646283 0.462300 0.899507 11.00000 0.04466 0.01212 = 0.03680 0.00744 0.01077 -0.00059 AFIX 43 H11 2 0.576745 0.375370 0.910122 11.00000 -1.20000 AFIX 0 O4 4 0.827701 0.906195 0.484891 11.00000 0.03012 0.03279 = 0.02066 0.00561 0.00756 0.00543 O5 4 0.412564 0.558007 0.587524 11.00000 0.02618 0.02832 = 0.03482 -0.00129 -0.00220 -0.01002 C7 1 0.941849 0.852395 0.849728 11.00000 0.01197 0.01405 = 0.01924 0.00094 0.00029 0.00487 AFIX 13 H7 2 1.023919 0.912453 0.897356 11.00000 -1.20000 AFIX 0 C14 1 0.993000 0.730550 1.037730 11.00000 0.03581 0.02806 = 0.02040 0.00494 -0.00009 0.01366 AFIX 137 H14A 2 0.990201 0.673990 1.093017 11.00000 -1.50000 H14B 2 0.965606 0.818372 1.055280 11.00000 -1.50000 H14C 2 1.105935 0.747564 1.014904 11.00000 -1.50000 AFIX 0 C19 1 0.538172 0.628682 0.612589 11.00000 0.02779 0.01771 = 0.01841 -0.00025 0.00441 0.00438 C12 1 0.764103 0.530981 0.972586 11.00000 0.04244 0.02016 = 0.02678 0.01110 0.00850 0.01128 AFIX 43 H12 2 0.772600 0.488797 1.031235 11.00000 -1.20000 AFIX 0 HKLF 4 REM 1 in P-1 REM R1 = 0.0163 for 4287 Fo > 4sig(Fo) and 0.0166 for all 4338 data REM 308 parameters refined using 0 restraints END WGHT 0.0193 0.9064 REM Highest difference peak 0.375, deepest hole -0.566, 1-sigma level 0.076 Q1 1 0.7823 0.6939 0.8394 11.00000 0.05 0.37 Q2 1 0.7831 0.6541 0.5968 11.00000 0.05 0.35 Q3 1 0.6381 0.9474 0.8984 11.00000 0.05 0.34 Q4 1 0.6730 1.1174 0.6196 11.00000 0.05 0.33 Q5 1 1.1861 1.2519 0.6959 11.00000 0.05 0.33 ; _shelx_res_checksum 96784 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' 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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp Ru2 Ru 0.74765(2) 0.74896(2) 0.66599(2) 0.01331(5) Uani 1 1 d . . Ru1 Ru 0.63142(2) 1.00086(2) 0.66149(2) 0.01329(5) Uani 1 1 d . . Ru3 Ru 0.66731(2) 0.86018(2) 0.83407(2) 0.01188(5) Uani 1 1 d . . N1 N 0.89428(19) 1.10373(15) 0.68549(11) 0.0154(3) Uani 1 1 d . . O2 O 0.56629(19) 1.13716(14) 0.83700(10) 0.0239(3) Uani 1 1 d . . O3 O 0.26921(18) 0.84654(16) 0.61806(11) 0.0300(3) Uani 1 1 d . . O8 O 0.68556(19) 0.99039(17) 1.03071(10) 0.0290(3) Uani 1 1 d . . O7 O 0.29662(19) 0.72192(18) 0.83600(13) 0.0372(4) Uani 1 1 d . . O1 O 0.5424(2) 1.25537(16) 0.58350(12) 0.0311(3) Uani 1 1 d . . C16 C 0.6022(2) 1.04542(18) 0.79540(13) 0.0149(3) Uani 1 1 d . . C22 C 0.6788(2) 0.9370(2) 0.95812(13) 0.0188(4) Uani 1 1 d . . C1 C 0.9938(2) 1.03265(18) 0.73389(12) 0.0134(3) Uani 1 1 d . . C6 C 0.9103(2) 0.89333(17) 0.75793(12) 0.0134(3) Uani 1 1 d . . C3 C 1.2318(2) 1.2229(2) 0.73533(14) 0.0221(4) Uani 1 1 d . . H3 H 1.3472 1.2636 0.7523 0.026 Uiso 1 1 calc R U C2 C 1.1637(2) 1.08999(19) 0.75899(13) 0.0168(3) Uani 1 1 d . . H2 H 1.2321 1.0382 0.7921 0.020 Uiso 1 1 calc R U C21 C 0.4343(3) 0.7771(2) 0.83462(14) 0.0217(4) Uani 1 1 d . . C17 C 0.4055(2) 0.90451(19) 0.63471(13) 0.0197(4) Uani 1 1 d . . C15 C 0.5782(2) 1.1572(2) 0.60976(13) 0.0198(4) Uani 1 1 d . . O6 O 0.9806(2) 0.56398(18) 0.61025(15) 0.0458(5) Uani 1 1 d . . C9 C 0.7318(2) 0.64963(18) 0.79510(13) 0.0176(4) Uani 1 1 d . . C13 C 0.8661(3) 0.6565(2) 0.96101(14) 0.0212(4) Uani 1 1 d . . C8 C 0.8493(2) 0.71631(18) 0.87090(13) 0.0162(4) Uani 1 1 d . . C5 C 0.9622(2) 1.23265(19) 0.66268(15) 0.0215(4) Uani 1 1 d . . H5 H 0.8924 1.2824 0.6287 0.026 Uiso 1 1 calc R U C18 C 0.7886(2) 0.85576(19) 0.55304(13) 0.0184(4) Uani 1 1 d . . C4 C 1.1291(3) 1.2961(2) 0.68637(16) 0.0248(4) Uani 1 1 d . . H4 H 1.1727 1.3877 0.6696 0.030 Uiso 1 1 calc R U C10 C 0.6306(3) 0.5187(2) 0.81386(15) 0.0265(4) Uani 1 1 d . . H10 H 0.5510 0.4700 0.7658 0.032 Uiso 1 1 calc R U C20 C 0.8933(3) 0.6333(2) 0.63009(15) 0.0251(4) Uani 1 1 d . . C11 C 0.6463(3) 0.4623(2) 0.89951(16) 0.0317(5) Uani 1 1 d . . H11 H 0.5767 0.3754 0.9101 0.038 Uiso 1 1 calc R U O4 O 0.82770(19) 0.90620(16) 0.48489(10) 0.0277(3) Uani 1 1 d . . O5 O 0.4126(2) 0.55801(16) 0.58752(11) 0.0325(4) Uani 1 1 d . . C7 C 0.9418(2) 0.85239(18) 0.84973(13) 0.0148(3) Uani 1 1 d . . H7 H 1.0239 0.9125 0.8974 0.018 Uiso 1 1 calc R U C14 C 0.9930(3) 0.7305(2) 1.03773(14) 0.0271(4) Uani 1 1 d . . H14A H 0.9902 0.6740 1.0930 0.041 Uiso 1 1 calc R U H14B H 0.9656 0.8184 1.0553 0.041 Uiso 1 1 calc R U H14C H 1.1059 0.7476 1.0149 0.041 Uiso 1 1 calc R U C19 C 0.5382(3) 0.6287(2) 0.61259(13) 0.0213(4) Uani 1 1 d . . C12 C 0.7641(3) 0.5310(2) 0.97259(15) 0.0286(5) Uani 1 1 d . . H12 H 0.7726 0.4888 1.0312 0.034 Uiso 1 1 calc R U 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 Ru2 0.01423(8) 0.01016(7) 0.01499(8) -0.00089(5) 0.00200(5) 0.00143(5) Ru1 0.01100(8) 0.01291(8) 0.01599(8) 0.00177(5) 0.00038(5) 0.00277(5) Ru3 0.01162(8) 0.01026(7) 0.01359(8) 0.00136(5) 0.00187(5) 0.00167(5) N1 0.0134(7) 0.0139(7) 0.0188(7) 0.0021(6) 0.0026(6) 0.0023(6) O2 0.0294(8) 0.0190(7) 0.0258(7) -0.0017(6) 0.0013(6) 0.0114(6) O3 0.0158(7) 0.0298(8) 0.0404(9) -0.0009(7) -0.0042(6) -0.0014(6) O8 0.0244(8) 0.0452(9) 0.0173(7) -0.0069(6) -0.0001(6) 0.0091(7) O7 0.0179(8) 0.0382(9) 0.0509(10) 0.0072(8) 0.0057(7) -0.0054(7) O1 0.0307(8) 0.0254(8) 0.0393(9) 0.0141(7) -0.0029(7) 0.0106(6) C16 0.0106(8) 0.0138(8) 0.0193(9) 0.0026(7) -0.0003(6) 0.0009(6) C22 0.0140(8) 0.0220(9) 0.0216(10) 0.0052(8) 0.0017(7) 0.0061(7) C1 0.0139(8) 0.0128(8) 0.0136(8) -0.0002(6) 0.0031(6) 0.0026(7) C6 0.0109(8) 0.0116(8) 0.0185(8) 0.0004(6) 0.0025(6) 0.0036(6) C3 0.0144(9) 0.0196(9) 0.0296(10) 0.0002(8) 0.0029(7) -0.0020(7) C2 0.0149(8) 0.0174(9) 0.0181(8) 0.0004(7) 0.0012(7) 0.0034(7) C21 0.0235(11) 0.0198(9) 0.0221(9) 0.0041(7) 0.0025(8) 0.0043(8) C17 0.0226(10) 0.0178(9) 0.0200(9) 0.0016(7) 0.0019(7) 0.0073(8) C15 0.0145(9) 0.0248(10) 0.0187(9) 0.0026(7) -0.0004(7) 0.0020(7) O6 0.0484(11) 0.0316(9) 0.0664(12) -0.0003(8) 0.0185(9) 0.0243(8) C9 0.0214(9) 0.0111(8) 0.0213(9) 0.0021(7) 0.0037(7) 0.0051(7) C13 0.0276(10) 0.0194(9) 0.0206(9) 0.0047(7) 0.0046(8) 0.0125(8) C8 0.0172(9) 0.0132(8) 0.0207(9) 0.0033(7) 0.0045(7) 0.0077(7) C5 0.0182(9) 0.0158(9) 0.0310(10) 0.0080(8) 0.0036(8) 0.0035(7) C18 0.0146(9) 0.0200(9) 0.0197(9) -0.0031(7) -0.0002(7) 0.0028(7) C4 0.0210(10) 0.0135(9) 0.0384(12) 0.0074(8) 0.0065(8) -0.0016(7) C10 0.0326(11) 0.0145(9) 0.0303(11) 0.0016(8) 0.0042(9) -0.0003(8) C20 0.0277(11) 0.0181(9) 0.0296(11) 0.0014(8) 0.0054(8) 0.0043(8) C11 0.0447(13) 0.0121(9) 0.0368(12) 0.0074(8) 0.0108(10) -0.0006(9) O4 0.0301(8) 0.0328(8) 0.0207(7) 0.0056(6) 0.0076(6) 0.0054(6) O5 0.0262(8) 0.0283(8) 0.0348(9) -0.0013(7) -0.0022(6) -0.0100(7) C7 0.0120(8) 0.0140(8) 0.0192(9) 0.0009(7) 0.0003(7) 0.0049(7) C14 0.0358(12) 0.0281(11) 0.0204(10) 0.0049(8) -0.0001(8) 0.0137(9) C19 0.0278(11) 0.0177(9) 0.0184(9) -0.0003(7) 0.0044(8) 0.0044(8) C12 0.0424(13) 0.0202(10) 0.0268(11) 0.0111(8) 0.0085(9) 0.0113(9) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle C20 Ru2 C19 96.43(9) C20 Ru2 C18 91.46(8) C19 Ru2 C18 95.42(8) C20 Ru2 C6 101.45(8) C19 Ru2 C6 158.83(7) C18 Ru2 C6 95.36(7) C20 Ru2 C9 87.66(8) C19 Ru2 C9 91.69(8) C18 Ru2 C9 172.89(8) C6 Ru2 C9 77.92(7) C20 Ru2 Ru3 136.50(6) C19 Ru2 Ru3 105.09(6) C18 Ru2 Ru3 122.77(6) C6 Ru2 Ru3 53.86(5) C9 Ru2 Ru3 54.91(5) C20 Ru2 Ru1 152.60(6) C19 Ru2 Ru1 96.83(6) C18 Ru2 Ru1 63.49(5) C6 Ru2 Ru1 71.99(5) C9 Ru2 Ru1 115.76(5) Ru3 Ru2 Ru1 61.423(9) C15 Ru1 C17 89.98(8) C15 Ru1 C16 97.94(8) C17 Ru1 C16 94.22(8) C15 Ru1 N1 91.14(7) C17 Ru1 N1 176.57(7) C16 Ru1 N1 88.84(7) C15 Ru1 Ru2 157.30(6) C17 Ru1 Ru2 91.65(6) C16 Ru1 Ru2 104.52(5) N1 Ru1 Ru2 86.07(4) C15 Ru1 Ru3 144.79(6) C17 Ru1 Ru3 92.46(6) C16 Ru1 Ru3 46.85(5) N1 Ru1 Ru3 88.50(4) Ru2 Ru1 Ru3 57.754(8) C22 Ru3 C21 92.85(8) C22 Ru3 C16 83.73(8) C21 Ru3 C16 89.25(8) C22 Ru3 C7 91.59(7) C21 Ru3 C7 152.00(7) C16 Ru3 C7 118.72(7) C22 Ru3 C6 118.19(7) C21 Ru3 C6 148.87(8) C16 Ru3 C6 95.97(6) C7 Ru3 C6 35.93(6) C22 Ru3 C8 95.04(7) C21 Ru3 C8 115.01(8) C16 Ru3 C8 155.73(7) C7 Ru3 C8 37.02(6) C6 Ru3 C8 63.20(6) C22 Ru3 C9 124.87(7) C21 Ru3 C9 91.63(8) C16 Ru3 C9 151.27(7) C7 Ru3 C9 63.51(6) C6 Ru3 C9 69.51(6) C8 Ru3 C9 35.81(7) C22 Ru3 Ru2 163.45(6) C21 Ru3 Ru2 101.70(6) C16 Ru3 Ru2 104.09(5) C7 Ru3 Ru2 71.85(5) C6 Ru3 Ru2 47.26(4) C8 Ru3 Ru2 71.76(5) C9 Ru3 Ru2 47.71(5) C22 Ru3 Ru1 126.13(6) C21 Ru3 Ru1 95.20(6) C16 Ru3 Ru1 43.35(5) C7 Ru3 Ru1 104.34(5) C6 Ru3 Ru1 69.19(4) C8 Ru3 Ru1 127.97(5) C9 Ru3 Ru1 108.04(5) Ru2 Ru3 Ru1 60.823(13) C5 N1 C1 118.55(16) C5 N1 Ru1 125.91(13) C1 N1 Ru1 115.36(12) O2 C16 Ru1 135.64(14) O2 C16 Ru3 134.55(14) Ru1 C16 Ru3 89.80(7) O8 C22 Ru3 176.06(17) N1 C1 C2 121.34(16) N1 C1 C6 115.55(15) C2 C1 C6 123.10(16) C7 C6 C1 118.16(16) C7 C6 Ru2 116.53(12) C1 C6 Ru2 125.31(12) C7 C6 Ru3 70.49(10) C1 C6 Ru3 119.91(11) Ru2 C6 Ru3 78.88(6) C2 C3 C4 119.07(18) C3 C2 C1 119.49(17) O7 C21 Ru3 176.91(18) O3 C17 Ru1 179.63(19) O1 C15 Ru1 175.64(18) C10 C9 C8 115.99(17) C10 C9 Ru2 128.29(15) C8 C9 Ru2 115.42(13) C10 C9 Ru3 124.46(14) C8 C9 Ru3 71.69(10) Ru2 C9 Ru3 77.37(6) C12 C13 C8 117.29(19) C12 C13 C14 122.36(18) C8 C13 C14 120.35(18) C9 C8 C13 122.66(17) C9 C8 C7 113.57(16) C13 C8 C7 123.67(17) C9 C8 Ru3 72.51(10) C13 C8 Ru3 124.36(13) C7 C8 Ru3 68.80(9) N1 C5 C4 123.01(18) O4 C18 Ru2 170.33(17) C5 C4 C3 118.53(18) C11 C10 C9 121.3(2) O6 C20 Ru2 178.9(2) C10 C11 C12 121.14(19) C6 C7 C8 115.74(16) C6 C7 Ru3 73.58(10) C8 C7 Ru3 74.18(10) O5 C19 Ru2 175.32(17) C13 C12 C11 121.64(19) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Ru2 C20 1.911(2) Ru2 C19 1.948(2) Ru2 C18 1.962(2) Ru2 C6 2.0839(18) Ru2 C9 2.1108(19) Ru2 Ru3 2.7842(5) Ru2 Ru1 2.8742(5) Ru1 C15 1.866(2) Ru1 C17 1.888(2) Ru1 C16 1.9845(19) Ru1 N1 2.1625(16) Ru1 Ru3 2.8909(5) Ru3 C22 1.889(2) Ru3 C21 1.901(2) Ru3 C16 2.1091(18) Ru3 C7 2.2518(18) Ru3 C6 2.2915(17) Ru3 C8 2.3239(17) Ru3 C9 2.3347(18) N1 C5 1.344(2) N1 C1 1.355(2) O2 C16 1.176(2) O3 C17 1.140(3) O8 C22 1.139(2) O7 C21 1.139(3) O1 C15 1.146(2) C1 C2 1.394(3) C1 C6 1.471(2) C6 C7 1.402(2) C3 C2 1.383(3) C3 C4 1.390(3) O6 C20 1.139(3) C9 C10 1.428(3) C9 C8 1.432(3) C13 C12 1.366(3) C13 C8 1.439(3) C13 C14 1.503(3) C8 C7 1.454(2) C5 C4 1.382(3) C18 O4 1.139(2) C10 C11 1.366(3) C11 C12 1.413(3) O5 C19 1.136(3)