#------------------------------------------------------------------------------ #$Date: 2019-11-08 06:19:29 +0200 (Fri, 08 Nov 2019) $ #$Revision: 225388 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/05/90/7059028.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_7059028 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 Br Cl2 N2 O9 Ru3' _chemical_formula_weight 901.35 _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 ; 2019-10-30 deposited with the CCDC. 2019-11-07 downloaded from the CCDC. ; _cell_angle_alpha 91.869(7) _cell_angle_beta 94.132(7) _cell_angle_gamma 106.036(7) _cell_formula_units_Z 2 _cell_length_a 8.0005(16) _cell_length_b 11.922(2) _cell_length_c 14.299(3) _cell_measurement_reflns_used 6687 _cell_measurement_temperature 296(2) _cell_measurement_theta_max 26.37 _cell_measurement_theta_min 2.65 _cell_volume 1305.4(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 296(2) _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device_type 'Bruker APEX II CCD' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0430 _diffrn_reflns_av_unetI/netI 0.0455 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_number 15372 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 25.998 _diffrn_reflns_theta_min 2.222 _exptl_absorpt_coefficient_mu 3.504 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details sadabs _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 2.293 _exptl_crystal_description block _exptl_crystal_F_000 860 _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 0.6242 _refine_diff_density_max 0.821 _refine_diff_density_min -0.771 _refine_diff_density_rms 0.127 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 353 _refine_ls_number_reflns 5137 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.025 _refine_ls_R_factor_all 0.0415 _refine_ls_R_factor_gt 0.0300 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0309P)^2^+1.1581P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0660 _refine_ls_wR_factor_ref 0.0702 _reflns_Friedel_coverage 0.000 _reflns_number_gt 4306 _reflns_number_total 5137 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c9nj04958d2.cif _cod_data_source_block 8a _cod_database_code 7059028 _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 0.622 _shelx_estimated_absorpt_t_max 0.721 _shelx_res_file ; 8a.res created by SHELXL-2014/7 TITL 1 in P-1 CELL 0.71073 8.0005 11.9216 14.2987 91.869 94.132 106.036 ZERR 2.00 0.0016 0.0022 0.0027 0.007 0.007 0.007 LATT 1 SFAC C H N O Br Ru Cl UNIT 44 22 4 18 2 6 4 OMIT -3.00 52.00 L.S. 4 ACTA BOND $h size 0.15 0.13 0.10 FMAP 2 temp 23 PLAN 5 WGHT 0.030900 1.158100 FVAR 0.09437 BR1 5 1.043654 0.704306 1.256250 11.00000 0.03768 0.04704 = 0.01539 0.00499 -0.00466 0.01976 RU1 6 0.751810 0.864244 0.790887 11.00000 0.01020 0.01144 = 0.01281 0.00292 0.00187 0.00320 RU2 6 0.555685 0.632377 0.793734 11.00000 0.01013 0.01222 = 0.01343 0.00241 0.00099 0.00259 RU3 6 0.559195 0.792502 0.946356 11.00000 0.00921 0.01478 = 0.01450 0.00305 0.00267 0.00434 CL1 7 0.153254 0.677485 0.488886 11.00000 0.06458 0.04446 = 0.03144 0.00048 0.00879 0.02875 CL2 7 0.156754 0.918971 0.474018 11.00000 0.15376 0.04503 = 0.05164 0.00575 0.00959 0.04145 N1 3 0.792008 0.754166 1.008542 11.00000 0.01065 0.01449 = 0.01375 0.00487 0.00117 0.00115 N2 3 1.016041 0.667890 0.968732 11.00000 0.01294 0.01957 = 0.01904 0.00529 -0.00031 0.00669 O1 4 0.600406 0.690722 0.416869 11.00000 0.04409 0.02015 = 0.01563 0.00191 0.00026 0.01181 O2 4 0.447972 0.857068 1.132821 11.00000 0.03595 0.03976 = 0.02411 -0.00001 0.00766 0.02278 O3 4 0.253844 0.860666 0.852414 11.00000 0.02236 0.03887 = 0.03422 0.01342 0.00413 0.01839 O4 4 0.343298 0.547548 0.962858 11.00000 0.02212 0.02108 = 0.01966 0.00395 0.00772 0.00516 O5 4 0.851976 1.045153 0.959534 11.00000 0.01888 0.01785 = 0.02298 -0.00446 -0.00025 -0.00220 O6 4 1.091624 1.000875 0.716679 11.00000 0.02167 0.03921 = 0.04377 0.01628 0.01567 0.00327 O7 4 0.501210 0.982517 0.687528 11.00000 0.03449 0.03187 = 0.02523 0.00326 -0.00596 0.02110 O8 4 0.195260 0.623240 0.705563 11.00000 0.01770 0.07627 = 0.03181 0.01037 -0.00483 0.01527 O9 4 0.477795 0.370651 0.805095 11.00000 0.04893 0.01393 = 0.03790 0.00308 0.01610 0.00162 C1 1 0.885576 0.714598 0.945697 11.00000 0.00892 0.00985 = 0.01715 0.00376 0.00168 -0.00096 C2 1 0.841418 0.751451 1.100108 11.00000 0.01927 0.01754 = 0.01573 0.00259 0.00494 0.00257 AFIX 43 H2 2 0.783337 0.780373 1.145052 11.00000 -1.20000 AFIX 0 C3 1 0.975968 0.706733 1.128124 11.00000 0.01737 0.01928 = 0.01432 0.00644 0.00135 0.00299 C4 1 1.060502 0.662541 1.059719 11.00000 0.01493 0.02290 = 0.01873 0.00546 -0.00080 0.00605 AFIX 43 H4 2 1.148915 0.628967 1.077910 11.00000 -1.20000 AFIX 0 C5 1 0.832416 0.724969 0.847357 11.00000 0.00414 0.01665 = 0.01647 0.00574 0.00083 0.00277 C6 1 0.834565 0.634393 0.783318 11.00000 0.01123 0.01500 = 0.01629 0.00386 0.00541 0.00511 AFIX 13 H6 2 0.878799 0.568710 0.801671 11.00000 -1.20000 AFIX 0 C7 1 0.767051 0.643553 0.689118 11.00000 0.01079 0.01530 = 0.01553 0.00520 0.00683 0.00186 C8 1 0.758167 0.559828 0.613630 11.00000 0.01922 0.01474 = 0.02010 -0.00018 0.00325 0.00776 AFIX 43 H8 2 0.790594 0.492028 0.624896 11.00000 -1.20000 AFIX 0 C9 1 0.702448 0.579663 0.525856 11.00000 0.02387 0.01977 = 0.02021 -0.00170 0.00410 0.00540 AFIX 43 H9 2 0.699114 0.526126 0.476486 11.00000 -1.20000 AFIX 0 C10 1 0.648900 0.681829 0.508501 11.00000 0.01578 0.01932 = 0.01539 0.00439 0.00122 0.00284 C11 1 0.647961 0.761660 0.579942 11.00000 0.01429 0.01729 = 0.01700 0.00122 0.00115 0.00199 AFIX 43 H11 2 0.608515 0.826421 0.567100 11.00000 -1.20000 AFIX 0 C12 1 0.707269 0.745480 0.673655 11.00000 0.01001 0.01406 = 0.01701 -0.00009 0.00254 0.00182 C13 1 0.573767 0.799481 0.389555 11.00000 0.05364 0.02710 = 0.01289 0.00617 -0.00073 0.01600 AFIX 137 H13A 2 0.476479 0.812560 0.419309 11.00000 -1.50000 H13B 2 0.550266 0.796825 0.322604 11.00000 -1.50000 H13C 2 0.676708 0.861929 0.408450 11.00000 -1.50000 AFIX 0 C14 1 0.494291 0.831998 1.063305 11.00000 0.01634 0.01702 = 0.02238 0.00308 0.00209 0.00784 C15 1 0.368590 0.833680 0.888794 11.00000 0.01417 0.01798 = 0.02023 0.00615 0.00583 0.00265 C16 1 0.439599 0.623212 0.927030 11.00000 0.01167 0.01750 = 0.01714 0.00062 -0.00131 0.00933 C17 1 0.802635 0.969615 0.904285 11.00000 0.00598 0.01850 = 0.02526 0.00534 0.00330 0.00429 C18 1 0.964533 0.950945 0.743818 11.00000 0.02223 0.01599 = 0.02110 0.00734 0.00359 0.00894 C19 1 0.597825 0.944303 0.728363 11.00000 0.02027 0.01733 = 0.01486 -0.00222 0.00329 0.00329 C20 1 0.329769 0.627544 0.739169 11.00000 0.02000 0.03129 = 0.01708 0.00717 -0.00065 0.00375 C21 1 0.503262 0.468108 0.798403 11.00000 0.01804 0.02547 = 0.01571 0.00155 0.00622 0.00297 C22 1 0.129436 0.803707 0.547804 11.00000 0.04569 0.04165 = 0.03783 -0.00660 0.01541 0.00715 AFIX 23 H22A 2 0.014291 0.786719 0.570644 11.00000 -1.20000 H22B 2 0.215077 0.825898 0.601557 11.00000 -1.20000 AFIX 0 HKLF 4 REM 1 in P-1 REM R1 = 0.0300 for 4306 Fo > 4sig(Fo) and 0.0415 for all 5137 data REM 353 parameters refined using 0 restraints END WGHT 0.0309 1.1532 REM Highest difference peak 0.821, deepest hole -0.771, 1-sigma level 0.127 Q1 1 0.6024 0.8625 0.9954 11.00000 0.05 0.82 Q2 1 0.7836 0.9350 0.8252 11.00000 0.05 0.76 Q3 1 0.7299 0.7922 0.7439 11.00000 0.05 0.72 Q4 1 0.5932 0.6996 0.8411 11.00000 0.05 0.70 Q5 1 1.0039 0.6388 1.2130 11.00000 0.05 0.69 ; _shelx_res_checksum 32097 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 Br1 Br 1.04365(7) 0.70431(5) 1.25625(3) 0.03206(13) Uani 1 1 d . . Ru1 Ru 0.75181(4) 0.86424(3) 0.79089(2) 0.01135(8) Uani 1 1 d . . Ru2 Ru 0.55569(4) 0.63238(3) 0.79373(2) 0.01200(8) Uani 1 1 d . . Ru3 Ru 0.55920(4) 0.79250(3) 0.94636(2) 0.01250(8) Uani 1 1 d . . Cl1 Cl 0.1533(2) 0.67748(12) 0.48889(9) 0.0439(3) Uani 1 1 d . . Cl2 Cl 0.1568(3) 0.91897(15) 0.47402(12) 0.0806(7) Uani 1 1 d . . N1 N 0.7920(4) 0.7542(3) 1.0085(2) 0.0133(7) Uani 1 1 d . . N2 N 1.0160(4) 0.6679(3) 0.9687(2) 0.0167(7) Uani 1 1 d . . O1 O 0.6004(5) 0.6907(3) 0.4169(2) 0.0261(7) Uani 1 1 d . . O2 O 0.4480(5) 0.8571(3) 1.1328(2) 0.0306(8) Uani 1 1 d . . O3 O 0.2538(4) 0.8607(3) 0.8524(2) 0.0295(8) Uani 1 1 d . . O4 O 0.3433(4) 0.5475(2) 0.9629(2) 0.0208(7) Uani 1 1 d . . O5 O 0.8520(4) 1.0452(2) 0.9595(2) 0.0216(7) Uani 1 1 d . . O6 O 1.0916(4) 1.0009(3) 0.7167(2) 0.0350(8) Uani 1 1 d . . O7 O 0.5012(4) 0.9825(3) 0.6875(2) 0.0285(8) Uani 1 1 d . . O8 O 0.1953(5) 0.6232(4) 0.7056(2) 0.0417(10) Uani 1 1 d . . O9 O 0.4778(5) 0.3707(3) 0.8051(2) 0.0344(9) Uani 1 1 d . . C1 C 0.8856(5) 0.7146(3) 0.9457(3) 0.0126(8) Uani 1 1 d . . C2 C 0.8414(6) 0.7515(3) 1.1001(3) 0.0178(9) Uani 1 1 d . . H2 H 0.7833 0.7804 1.1451 0.021 Uiso 1 1 calc R U C3 C 0.9760(6) 0.7067(4) 1.1281(3) 0.0173(9) Uani 1 1 d . . C4 C 1.0605(6) 0.6625(4) 1.0597(3) 0.0187(9) Uani 1 1 d . . H4 H 1.1489 0.6290 1.0779 0.022 Uiso 1 1 calc R U C5 C 0.8324(5) 0.7250(3) 0.8474(3) 0.0123(8) Uani 1 1 d . . C6 C 0.8346(5) 0.6344(3) 0.7833(3) 0.0136(8) Uani 1 1 d . . H6 H 0.8788 0.5687 0.8017 0.016 Uiso 1 1 calc R U C7 C 0.7671(5) 0.6436(3) 0.6891(3) 0.0138(8) Uani 1 1 d . . C8 C 0.7582(5) 0.5598(3) 0.6136(3) 0.0174(9) Uani 1 1 d . . H8 H 0.7906 0.4920 0.6249 0.021 Uiso 1 1 calc R U C9 C 0.7024(6) 0.5797(4) 0.5259(3) 0.0214(9) Uani 1 1 d . . H9 H 0.6991 0.5261 0.4765 0.026 Uiso 1 1 calc R U C10 C 0.6489(5) 0.6818(4) 0.5085(3) 0.0172(9) Uani 1 1 d . . C11 C 0.6480(5) 0.7617(4) 0.5799(3) 0.0167(9) Uani 1 1 d . . H11 H 0.6085 0.8264 0.5671 0.020 Uiso 1 1 calc R U C12 C 0.7073(5) 0.7455(3) 0.6737(3) 0.0140(8) Uani 1 1 d . . C13 C 0.5738(7) 0.7995(4) 0.3896(3) 0.0303(12) Uani 1 1 d . . H13A H 0.4765 0.8126 0.4193 0.045 Uiso 1 1 calc R U H13B H 0.5503 0.7968 0.3226 0.045 Uiso 1 1 calc R U H13C H 0.6767 0.8619 0.4085 0.045 Uiso 1 1 calc R U C14 C 0.4943(6) 0.8320(4) 1.0633(3) 0.0179(9) Uani 1 1 d . . C15 C 0.3686(6) 0.8337(4) 0.8888(3) 0.0175(9) Uani 1 1 d . . C16 C 0.4396(5) 0.6232(3) 0.9270(3) 0.0145(8) Uani 1 1 d . . C17 C 0.8026(5) 0.9696(4) 0.9043(3) 0.0162(9) Uani 1 1 d . . C18 C 0.9645(6) 0.9509(4) 0.7438(3) 0.0188(9) Uani 1 1 d . . C19 C 0.5978(6) 0.9443(4) 0.7284(3) 0.0179(9) Uani 1 1 d . . C20 C 0.3298(6) 0.6275(4) 0.7392(3) 0.0235(10) Uani 1 1 d . . C21 C 0.5033(6) 0.4681(4) 0.7984(3) 0.0201(9) Uani 1 1 d . . C22 C 0.1294(8) 0.8037(5) 0.5478(4) 0.0423(14) Uani 1 1 d . . H22A H 0.0143 0.7867 0.5706 0.051 Uiso 1 1 calc R U H22B H 0.2151 0.8259 0.6016 0.051 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 Br1 0.0377(3) 0.0470(3) 0.0154(2) 0.0050(2) -0.0047(2) 0.0198(2) Ru1 0.01020(17) 0.01144(16) 0.01281(16) 0.00292(12) 0.00187(13) 0.00320(12) Ru2 0.01013(17) 0.01222(16) 0.01343(16) 0.00241(12) 0.00099(13) 0.00259(12) Ru3 0.00921(17) 0.01478(17) 0.01450(17) 0.00305(12) 0.00267(13) 0.00434(12) Cl1 0.0646(10) 0.0445(8) 0.0314(7) 0.0005(6) 0.0088(7) 0.0287(7) Cl2 0.154(2) 0.0450(9) 0.0516(10) 0.0057(8) 0.0096(11) 0.0414(12) N1 0.0107(18) 0.0145(17) 0.0137(17) 0.0049(13) 0.0012(14) 0.0012(13) N2 0.0129(18) 0.0196(18) 0.0190(18) 0.0053(14) -0.0003(15) 0.0067(14) O1 0.044(2) 0.0202(16) 0.0156(15) 0.0019(12) 0.0003(14) 0.0118(14) O2 0.036(2) 0.040(2) 0.0241(18) 0.0000(14) 0.0077(15) 0.0228(16) O3 0.0224(19) 0.039(2) 0.0342(19) 0.0134(15) 0.0041(15) 0.0184(15) O4 0.0221(17) 0.0211(16) 0.0197(15) 0.0039(12) 0.0077(13) 0.0052(13) O5 0.0189(17) 0.0178(15) 0.0230(16) -0.0045(13) -0.0003(13) -0.0022(13) O6 0.0217(19) 0.039(2) 0.044(2) 0.0163(16) 0.0157(16) 0.0033(15) O7 0.034(2) 0.0319(19) 0.0252(17) 0.0033(14) -0.0060(15) 0.0211(16) O8 0.018(2) 0.076(3) 0.032(2) 0.0104(18) -0.0048(16) 0.0153(18) O9 0.049(2) 0.0139(17) 0.038(2) 0.0031(14) 0.0161(17) 0.0016(15) C1 0.009(2) 0.0098(19) 0.017(2) 0.0038(15) 0.0017(16) -0.0010(15) C2 0.019(2) 0.018(2) 0.016(2) 0.0026(16) 0.0049(18) 0.0026(17) C3 0.017(2) 0.019(2) 0.014(2) 0.0064(16) 0.0013(17) 0.0030(17) C4 0.015(2) 0.023(2) 0.019(2) 0.0055(17) -0.0008(18) 0.0060(17) C5 0.0041(19) 0.017(2) 0.016(2) 0.0057(15) 0.0008(16) 0.0028(15) C6 0.011(2) 0.015(2) 0.016(2) 0.0039(15) 0.0054(16) 0.0051(16) C7 0.011(2) 0.015(2) 0.016(2) 0.0052(15) 0.0068(16) 0.0019(16) C8 0.019(2) 0.015(2) 0.020(2) -0.0002(16) 0.0033(18) 0.0078(17) C9 0.024(3) 0.020(2) 0.020(2) -0.0017(17) 0.0041(19) 0.0054(18) C10 0.016(2) 0.019(2) 0.015(2) 0.0044(16) 0.0012(17) 0.0028(17) C11 0.014(2) 0.017(2) 0.017(2) 0.0012(16) 0.0012(17) 0.0020(16) C12 0.010(2) 0.014(2) 0.017(2) -0.0001(15) 0.0025(16) 0.0018(15) C13 0.054(4) 0.027(3) 0.013(2) 0.0062(18) -0.001(2) 0.016(2) C14 0.016(2) 0.017(2) 0.022(2) 0.0031(17) 0.0021(18) 0.0078(17) C15 0.014(2) 0.018(2) 0.020(2) 0.0062(17) 0.0058(18) 0.0027(17) C16 0.012(2) 0.018(2) 0.017(2) 0.0006(16) -0.0013(17) 0.0093(16) C17 0.0060(19) 0.019(2) 0.025(2) 0.0053(18) 0.0033(17) 0.0043(16) C18 0.022(2) 0.016(2) 0.021(2) 0.0073(17) 0.0036(19) 0.0089(18) C19 0.020(2) 0.017(2) 0.015(2) -0.0022(16) 0.0033(18) 0.0033(18) C20 0.020(3) 0.031(3) 0.017(2) 0.0072(18) -0.0006(19) 0.0038(19) C21 0.018(2) 0.025(3) 0.016(2) 0.0015(17) 0.0062(18) 0.0030(18) C22 0.046(4) 0.042(3) 0.038(3) -0.007(2) 0.015(3) 0.007(3) 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' Br Br -0.2901 2.4595 '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' Cl Cl 0.1484 0.1585 '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 C18 Ru1 C19 97.80(17) C18 Ru1 C17 90.21(17) C19 Ru1 C17 94.13(17) C18 Ru1 C12 89.44(17) C19 Ru1 C12 89.47(16) C17 Ru1 C12 176.39(16) C18 Ru1 C5 99.98(16) C19 Ru1 C5 158.21(16) C17 Ru1 C5 98.28(16) C12 Ru1 C5 78.25(15) C18 Ru1 Ru2 138.02(12) C19 Ru1 Ru2 105.55(12) C17 Ru1 Ru2 121.61(12) C12 Ru1 Ru2 57.02(11) C5 Ru1 Ru2 52.66(11) C18 Ru1 Ru3 148.67(13) C19 Ru1 Ru3 98.26(12) C17 Ru1 Ru3 61.95(12) C12 Ru1 Ru3 117.40(11) C5 Ru1 Ru3 72.37(10) Ru2 Ru1 Ru3 61.114(13) C21 Ru2 C20 93.67(19) C21 Ru2 C16 84.42(16) C20 Ru2 C16 85.48(17) C21 Ru2 C6 87.40(17) C20 Ru2 C6 152.08(17) C16 Ru2 C6 122.34(14) C21 Ru2 C5 112.90(17) C20 Ru2 C5 153.39(17) C16 Ru2 C5 98.05(15) C6 Ru2 C5 36.27(14) C21 Ru2 C7 93.78(16) C20 Ru2 C7 115.59(16) C16 Ru2 C7 158.93(15) C6 Ru2 C7 36.62(14) C5 Ru2 C7 63.28(14) C21 Ru2 C12 125.21(16) C20 Ru2 C12 94.54(16) C16 Ru2 C12 150.22(14) C6 Ru2 C12 62.93(14) C5 Ru2 C12 69.46(14) C7 Ru2 C12 35.48(13) C21 Ru2 Ru1 159.52(14) C20 Ru2 Ru1 105.42(14) C16 Ru2 Ru1 104.10(11) C6 Ru2 Ru1 72.27(10) C5 Ru2 Ru1 48.07(9) C7 Ru2 Ru1 71.51(10) C12 Ru2 Ru1 47.18(9) C21 Ru2 Ru3 126.07(12) C20 Ru2 Ru3 96.06(14) C16 Ru2 Ru3 44.00(11) C6 Ru2 Ru3 105.80(10) C5 Ru2 Ru3 69.98(10) C7 Ru2 Ru3 127.73(10) C12 Ru2 Ru3 106.69(9) Ru1 Ru2 Ru3 60.102(15) C14 Ru3 C15 89.11(18) C14 Ru3 C16 103.45(17) C15 Ru3 C16 92.50(17) C14 Ru3 N1 92.58(16) C15 Ru3 N1 176.15(15) C16 Ru3 N1 90.47(14) C14 Ru3 C17 106.16(16) C15 Ru3 C17 98.34(15) C16 Ru3 C17 148.53(15) N1 Ru3 C17 77.87(12) C14 Ru3 Ru1 148.13(13) C15 Ru3 Ru1 90.47(12) C16 Ru3 Ru1 108.41(12) N1 Ru3 Ru1 86.27(8) C17 Ru3 Ru1 42.49(10) C14 Ru3 Ru2 153.08(13) C15 Ru3 Ru2 91.68(13) C16 Ru3 Ru2 49.64(12) N1 Ru3 Ru2 88.37(9) C17 Ru3 Ru2 100.34(10) Ru1 Ru3 Ru2 58.784(15) C2 N1 C1 117.1(4) C2 N1 Ru3 128.1(3) C1 N1 Ru3 114.4(2) C4 N2 C1 117.6(4) C10 O1 C13 117.7(3) N2 C1 N1 124.7(4) N2 C1 C5 120.4(3) N1 C1 C5 114.9(3) N1 C2 C3 120.9(4) N1 C2 H2 119.5 C3 C2 H2 119.5 C2 C3 C4 118.8(4) C2 C3 Br1 120.3(3) C4 C3 Br1 120.9(3) N2 C4 C3 120.8(4) N2 C4 H4 119.6 C3 C4 H4 119.6 C6 C5 C1 117.7(3) C6 C5 Ru1 115.9(3) C1 C5 Ru1 126.4(3) C6 C5 Ru2 71.5(2) C1 C5 Ru2 117.9(3) Ru1 C5 Ru2 79.27(13) C5 C6 C7 115.6(4) C5 C6 Ru2 72.2(2) C7 C6 Ru2 74.6(2) C5 C6 H6 122.2 C7 C6 H6 122.2 Ru2 C6 H6 122.2 C8 C7 C6 124.0(4) C8 C7 C12 120.6(4) C6 C7 C12 115.3(3) C8 C7 Ru2 125.2(3) C6 C7 Ru2 68.8(2) C12 C7 Ru2 75.6(2) C9 C8 C7 119.7(4) C9 C8 H8 120.1 C7 C8 H8 120.1 C8 C9 C10 120.4(4) C8 C9 H9 119.8 C10 C9 H9 119.8 O1 C10 C11 124.9(4) O1 C10 C9 113.5(4) C11 C10 C9 121.5(4) C10 C11 C12 120.2(4) C10 C11 H11 119.9 C12 C11 H11 119.9 C11 C12 C7 117.3(4) C11 C12 Ru1 127.7(3) C7 C12 Ru1 114.4(3) C11 C12 Ru2 130.5(3) C7 C12 Ru2 68.9(2) Ru1 C12 Ru2 75.80(12) O1 C13 H13A 109.5 O1 C13 H13B 109.5 H13A C13 H13B 109.5 O1 C13 H13C 109.5 H13A C13 H13C 109.5 H13B C13 H13C 109.5 O2 C14 Ru3 176.9(4) O3 C15 Ru3 178.6(4) O4 C16 Ru3 140.6(3) O4 C16 Ru2 132.9(3) Ru3 C16 Ru2 86.36(15) O5 C17 Ru1 166.9(3) O5 C17 Ru3 117.4(3) Ru1 C17 Ru3 75.55(13) O6 C18 Ru1 178.8(4) O7 C19 Ru1 174.2(4) O8 C20 Ru2 178.8(5) O9 C21 Ru2 176.5(4) Cl2 C22 Cl1 111.2(3) Cl2 C22 H22A 109.4 Cl1 C22 H22A 109.4 Cl2 C22 H22B 109.4 Cl1 C22 H22B 109.4 H22A C22 H22B 108.0 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Br1 C3 1.876(4) Ru1 C18 1.912(4) Ru1 C19 1.943(4) Ru1 C17 1.965(4) Ru1 C12 2.103(4) Ru1 C5 2.104(4) Ru1 Ru2 2.7794(6) Ru1 Ru3 2.8174(6) Ru2 C21 1.891(4) Ru2 C20 1.901(5) Ru2 C16 2.173(4) Ru2 C6 2.240(4) Ru2 C5 2.249(4) Ru2 C7 2.317(4) Ru2 C12 2.405(4) Ru2 Ru3 2.8455(6) Ru3 C14 1.870(4) Ru3 C15 1.872(4) Ru3 C16 1.981(4) Ru3 N1 2.174(3) Ru3 C17 2.568(4) Cl1 C22 1.763(5) Cl2 C22 1.735(6) N1 C2 1.344(5) N1 C1 1.362(5) N2 C4 1.332(5) N2 C1 1.338(5) O1 C10 1.355(5) O1 C13 1.433(5) O2 C14 1.144(5) O3 C15 1.150(5) O4 C16 1.172(5) O5 C17 1.142(5) O6 C18 1.130(5) O7 C19 1.137(5) O8 C20 1.134(6) O9 C21 1.131(5) C1 C5 1.459(5) C2 C3 1.368(6) C2 H2 0.9300 C3 C4 1.396(6) C4 H4 0.9300 C5 C6 1.397(5) C6 C7 1.434(5) C6 H6 0.9800 C7 C8 1.430(6) C7 C12 1.441(5) C8 C9 1.352(6) C8 H8 0.9300 C9 C10 1.422(6) C9 H9 0.9300 C10 C11 1.375(6) C11 C12 1.426(6) C11 H11 0.9300 C13 H13A 0.9600 C13 H13B 0.9600 C13 H13C 0.9600 C22 H22A 0.9700 C22 H22B 0.9700