#------------------------------------------------------------------------------ #$Date: 2019-11-26 03:43:09 +0200 (Tue, 26 Nov 2019) $ #$Revision: 242529 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/13/25/4132581.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_4132581 loop_ _publ_author_name 'Dutta, Indranil' 'Yadav, Sudhir' 'Sarbajna, Abir' 'De, Subhabrata' 'H\"olscher, Markus' 'Leitner, Walter' 'Bera, Jitendra K.' _publ_section_title ; Double Dehydrogenation of Primary Amines to Nitriles by a Ruthenium Complex Featuring Pyrazole Functionality. ; _journal_issue 28 _journal_name_full 'Journal of the American Chemical Society' _journal_page_first 8662 _journal_page_last 8666 _journal_paper_doi 10.1021/jacs.8b05009 _journal_volume 140 _journal_year 2018 _chemical_formula_sum 'C22 H29 Cl2 N3 Ru' _chemical_formula_weight 507.45 _space_group_crystal_system orthorhombic _space_group_IT_number 33 _space_group_name_Hall 'P 2c -2n' _space_group_name_H-M_alt 'P n a 21' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2014/7 _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 19.270(2) _cell_length_b 9.9659(12) _cell_length_c 11.8072(14) _cell_measurement_reflns_used 4622 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 28.11 _cell_measurement_theta_min 2.30 _cell_volume 2267.5(4) _computing_cell_refinement 'Bruker SAINT' _computing_data_collection 'Bruker APEX2' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics DIAMOND _computing_publication_material ciftab _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_structure_solution 'SHELXL-2014/7 (Sheldrick, 2014)' _diffrn_ambient_temperature 100(2) _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.996 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0552 _diffrn_reflns_av_unetI/netI 0.0635 _diffrn_reflns_Laue_measured_fraction_full 0.996 _diffrn_reflns_Laue_measured_fraction_max 0.996 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_number 8672 _diffrn_reflns_point_group_measured_fraction_full 0.795 _diffrn_reflns_point_group_measured_fraction_max 0.795 _diffrn_reflns_theta_full 25.047 _diffrn_reflns_theta_max 25.047 _diffrn_reflns_theta_min 2.114 _diffrn_source 'fine-focus sealed tube' _exptl_absorpt_coefficient_mu 0.940 _exptl_absorpt_correction_T_max 0.841 _exptl_absorpt_correction_T_min 0.819 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details '(Bera et al., 2017)' _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.487 _exptl_crystal_description block _exptl_crystal_F_000 1040 _exptl_crystal_size_max 0.210 _exptl_crystal_size_mid 0.190 _exptl_crystal_size_min 0.180 _refine_diff_density_max 0.934 _refine_diff_density_min -1.071 _refine_diff_density_rms 0.123 _refine_ls_abs_structure_details ; Flack x determined using 799 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack 0.03(4) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.090 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 229 _refine_ls_number_reflns 3194 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.090 _refine_ls_R_factor_all 0.0589 _refine_ls_R_factor_gt 0.0440 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0384P)^2^+2.5305P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0893 _refine_ls_wR_factor_ref 0.0952 _reflns_Friedel_coverage 0.517 _reflns_Friedel_fraction_full 0.571 _reflns_Friedel_fraction_max 0.571 _reflns_number_gt 2721 _reflns_number_total 3194 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file ja8b05009_si_002.cif _cod_data_source_block compound4 _cod_original_cell_volume 2267.4(5) _cod_database_code 4132581 _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 0.827 _shelx_estimated_absorpt_t_max 0.849 _exptl_absorpt_special_details SADABS _shelx_res_file ; D:\Indranil\PAPERW~1\AMINED~1\Xray\PY-RU-~1\Final\8FEBA.res created by SHELXL-2014/7 REM 8Feba.res in Pna2(1) REM R1 = 0.0427 for 2721 Fo > 4sig(Fo) and 0.0575 for all 3194 data REM 241 parameters refined using 1 restraints REM Highest difference peak 0.944, deepest hole -1.074, 1-sigma level 0.120 REM 26jana_b.res in Pna2(1) REM R1 = 0.0439 for 2721 Fo > 4sig(Fo) and 0.0587 for all 3194 data REM 229 parameters refined using 1 restraints REM Highest difference peak 0.928, deepest hole -1.074, 1-sigma level 0.123 REM 26jana_b.res in Pna2(1) REM R1 = 0.0439 for 2721 Fo > 4sig(Fo) and 0.0587 for all 3194 data REM 229 parameters refined using 1 restraints REM Highest difference peak 0.929, deepest hole -1.075, 1-sigma level 0.123 REM 26jana_b.res in Pna2(1) REM R1 = 0.0439 for 2721 Fo > 4sig(Fo) and 0.0587 for all 3194 data REM 229 parameters refined using 1 restraints REM Highest difference peak 0.929, deepest hole -1.075, 1-sigma level 0.123 REM 26jana_b.res in Pna2(1) REM R1 = 0.0439 for 2721 Fo > 4sig(Fo) and 0.0587 for all 3194 data REM 229 parameters refined using 1 restraints REM Highest difference peak 0.929, deepest hole -1.075, 1-sigma level 0.123 REM 26jana_b.res in Pna2(1) REM R1 = 0.0440 for 2721 Fo > 4sig(Fo) and 0.0589 for all 3194 data REM 229 parameters refined using 1 restraints REM Highest difference peak 0.934, deepest hole -1.069, 1-sigma level 0.123 REM 26jana_b.res in Pna2(1) REM R1 = 0.0440 for 2721 Fo > 4sig(Fo) and 0.0589 for all 3194 data REM 229 parameters refined using 1 restraints REM Highest difference peak 0.934, deepest hole -1.070, 1-sigma level 0.123 REM 26jana_b.res in Pna2(1) REM R1 = 0.0440 for 2721 Fo > 4sig(Fo) and 0.0589 for all 3194 data REM 229 parameters refined using 1 restraints REM Highest difference peak 0.934, deepest hole -1.071, 1-sigma level 0.123 TITL 26jana_b.res in Pna2(1) CELL 0.71073 19.2695 9.9659 11.8072 90.000 90.000 90.000 ZERR 4.0000 0.0023 0.0012 0.0014 0.000 0.000 0.000 LATT -1 SYMM -X, -Y, 0.5+Z SYMM 0.5-X, 0.5+Y, 0.5+Z SYMM 0.5+X, 0.5-Y, Z SFAC C CL N RU H UNIT 88 8 12 4 116 MERG 2 OMIT -2 50.1 FMAP 2 GRID PLAN 20 TEMP -173 SIZE 0.18 0.19 0.21 BOND OMIT 4 1 2 OMIT 4 1 -2 OMIT 5 1 3 OMIT 8 0 0 OMIT 4 1 0 OMIT 5 1 -3 OMIT 10 3 7 OMIT 2 5 3 OMIT 1 4 1 OMIT 2 5 -2 OMIT 2 5 -3 EADP C19 C18 EADP C21 C22 EADP C17 C13 EADP C9 C10 EADP C2 C3 L.S. 5 ACTA WGHT 0.038400 2.530500 FVAR 0.40564 RU1 4 0.083741 0.989331 0.525110 11.00000 0.00386 0.01682 = 0.00844 0.00129 0.00056 0.00007 CL1 2 0.034038 1.142057 0.659370 11.00000 0.01759 0.02287 = 0.02196 -0.00397 0.01033 0.00182 C8 1 0.071866 0.666228 0.763835 11.00000 0.01881 0.00902 = 0.01005 0.00240 -0.00478 0.00029 C18 1 0.195276 1.036725 0.526384 11.00000 0.00730 0.02819 = 0.01157 0.00687 0.00465 -0.00364 AFIX 43 H18 5 0.226856 1.048678 0.587340 11.00000 -1.20000 AFIX 0 C21 1 0.113772 1.125655 0.388876 11.00000 0.01291 0.01832 = 0.00920 0.00490 0.00457 -0.00197 AFIX 43 H21 5 0.089212 1.198783 0.356359 11.00000 -1.20000 AFIX 0 C19 1 0.159865 1.149302 0.479863 11.00000 0.00730 0.02819 = 0.01157 0.00687 0.00465 -0.00364 C13 1 0.138944 0.883023 0.389481 11.00000 0.00979 0.01933 = 0.01163 -0.00027 0.00650 -0.00303 N3 3 0.107769 0.768125 0.714284 11.00000 0.00723 0.02039 = 0.01347 0.00373 -0.00306 0.00250 AFIX 43 H3 5 0.151947 0.784866 0.726817 11.00000 -1.20000 AFIX 0 C17 1 0.183301 0.906080 0.481417 11.00000 0.00979 0.01933 = 0.01163 -0.00027 0.00650 -0.00303 AFIX 43 H17 5 0.206282 0.831774 0.515083 11.00000 -1.20000 AFIX 0 C22 1 0.103756 0.996174 0.345952 11.00000 0.01291 0.01832 = 0.00920 0.00490 0.00457 -0.00197 AFIX 43 H22 5 0.072067 0.983914 0.285191 11.00000 -1.20000 AFIX 0 C6 1 0.003758 0.781941 0.648150 11.00000 0.00826 0.01686 = 0.00637 -0.00345 -0.00049 -0.00331 N2 3 0.067544 0.840050 0.643896 11.00000 0.01058 0.01302 = 0.00659 0.00235 -0.00125 0.00182 C7 1 0.005235 0.674454 0.721693 11.00000 0.00757 0.01485 = 0.02334 -0.00054 0.00382 -0.00004 AFIX 43 H7 5 -0.032485 0.616980 0.739879 11.00000 -1.20000 AFIX 0 C9 1 0.104667 0.570124 0.846605 11.00000 0.03273 0.03545 = 0.05791 0.03255 -0.02297 -0.00877 C20 1 0.168966 1.284881 0.530500 11.00000 0.01979 0.02615 = 0.02212 0.00003 0.00423 -0.00220 AFIX 137 H20A 5 0.203055 1.335627 0.486236 11.00000 -1.50000 H20B 5 0.185382 1.275866 0.608688 11.00000 -1.50000 H20C 5 0.124455 1.332446 0.529928 11.00000 -1.50000 AFIX 0 C2 1 -0.135995 0.967726 0.428506 11.00000 0.00649 0.03175 = 0.02148 0.00076 -0.00709 0.00049 AFIX 43 H2 5 -0.166023 1.011931 0.376738 11.00000 -1.20000 AFIX 0 N1 3 -0.021388 0.933568 0.500805 11.00000 0.01372 0.02153 = 0.01132 0.00037 0.00278 0.00209 C3 1 -0.161509 0.876317 0.504104 11.00000 0.00649 0.03175 = 0.02148 0.00076 -0.00709 0.00049 AFIX 43 H5 5 -0.209815 0.857350 0.505616 11.00000 -1.20000 AFIX 0 C5 1 -0.046941 0.842128 0.573702 11.00000 0.01039 0.00751 = 0.01714 -0.00484 -0.00448 0.00135 C4 1 -0.118019 0.812237 0.577327 11.00000 0.01141 0.01471 = 0.01902 0.00326 0.00185 -0.00492 AFIX 43 H4 5 -0.135538 0.748480 0.629865 11.00000 -1.20000 AFIX 0 C1 1 -0.064607 0.994924 0.428915 11.00000 0.00888 0.02320 = 0.01888 0.01295 -0.00548 -0.00479 AFIX 43 H1 5 -0.046486 1.058545 0.376805 11.00000 -1.20000 AFIX 0 C15 1 0.182097 0.724461 0.245579 11.00000 0.04485 0.03071 = 0.02956 -0.01542 0.01256 -0.00970 AFIX 137 H15A 5 0.228579 0.736409 0.277716 11.00000 -1.50000 H15B 5 0.174748 0.790197 0.185026 11.00000 -1.50000 H15C 5 0.177835 0.633601 0.214609 11.00000 -1.50000 AFIX 0 C14 1 0.128073 0.744878 0.337586 11.00000 0.01064 0.02808 = 0.01806 -0.00175 -0.00097 0.00077 AFIX 13 H14 5 0.081538 0.745225 0.300099 11.00000 -1.20000 AFIX 0 C12 1 0.168319 0.506092 0.793565 11.00000 0.05110 0.03881 = 0.03660 -0.01017 -0.01952 0.02835 AFIX 137 H12A 5 0.154552 0.455460 0.726053 11.00000 -1.50000 H12B 5 0.190046 0.445249 0.848287 11.00000 -1.50000 H12C 5 0.201456 0.576223 0.772110 11.00000 -1.50000 AFIX 0 C10 1 0.052369 0.463935 0.878819 11.00000 0.03273 0.03545 = 0.05791 0.03255 -0.02297 -0.00877 AFIX 137 H10A 5 0.014569 0.505183 0.922076 11.00000 -1.50000 H10B 5 0.075040 0.395177 0.925209 11.00000 -1.50000 H10C 5 0.033558 0.422528 0.810080 11.00000 -1.50000 AFIX 0 C11 1 0.127025 0.646734 0.953348 11.00000 0.03010 0.04716 = 0.02113 0.01032 -0.00166 0.01616 AFIX 137 H11A 5 0.163635 0.710941 0.933796 11.00000 -1.50000 H11B 5 0.144625 0.583126 1.009754 11.00000 -1.50000 H11C 5 0.087088 0.695036 0.984633 11.00000 -1.50000 AFIX 0 CL2 2 0.259759 0.848399 0.747447 11.00000 0.00849 0.02970 = 0.01842 -0.00111 -0.00206 0.00517 C16 1 0.128358 0.631258 0.422147 11.00000 0.01795 0.02633 = 0.03231 -0.00738 -0.00597 -0.00800 AFIX 137 H16A 5 0.175012 0.621402 0.454127 11.00000 -1.50000 H16B 5 0.114933 0.547760 0.384173 11.00000 -1.50000 H16C 5 0.095316 0.650854 0.483036 11.00000 -1.50000 AFIX 0 HKLF 4 REM 26jana_b.res in Pna2(1) REM R1 = 0.0440 for 2721 Fo > 4sig(Fo) and 0.0589 for all 3194 data REM 229 parameters refined using 1 restraints END WGHT 0.0384 2.5357 REM Highest difference peak 0.934, deepest hole -1.071, 1-sigma level 0.123 Q1 1 0.0846 1.0609 0.4604 11.00000 0.05 0.93 Q2 1 0.0793 0.9226 0.6013 11.00000 0.05 0.87 Q3 1 0.0866 1.0556 0.5999 11.00000 0.05 0.85 Q4 1 0.0805 0.9202 0.4574 11.00000 0.05 0.76 Q5 1 0.0795 1.1422 0.5132 11.00000 0.05 0.54 Q6 1 0.0296 1.0811 0.7263 11.00000 0.05 0.45 Q7 1 0.0397 0.5158 0.9260 11.00000 0.05 0.45 Q8 1 0.0810 0.7941 0.5348 11.00000 0.05 0.44 Q9 1 0.0515 0.9719 0.5822 11.00000 0.05 0.44 Q10 1 0.1101 0.3664 0.8499 11.00000 0.05 0.42 Q11 1 -0.1141 0.6400 0.7009 11.00000 0.05 0.41 Q12 1 0.2545 0.8133 0.8468 11.00000 0.05 0.41 Q13 1 0.0559 0.8707 0.5239 11.00000 0.05 0.41 Q14 1 0.0222 1.2423 0.6039 11.00000 0.05 0.40 Q15 1 0.1023 0.4143 1.0257 11.00000 0.05 0.40 Q16 1 0.1900 0.8581 0.5377 11.00000 0.05 0.40 Q17 1 0.2047 0.5201 0.5259 11.00000 0.05 0.40 Q18 1 -0.0004 1.1821 0.5360 11.00000 0.05 0.39 Q19 1 0.0691 0.4302 0.8331 11.00000 0.05 0.39 Q20 1 0.1912 1.0946 0.4991 11.00000 0.05 0.39 ; _shelx_res_checksum 61806 _shelx_hkl_file ; 0 1 0 -2.90 1.50 0 -1 0 -3.00 1.30 0 -2 0 1668.63 62.29 0 2 0 1694.33 61.49 0 2 0 1792.82 62.79 0 -2 0 1708.13 61.59 0 3 0 -2.90 5.20 0 -3 0 -2.20 4.00 0 -4 0 377.16 18.30 0 4 0 418.66 21.40 0 5 0 -0.50 8.10 0 6 0 4838.12 178.28 0 7 0 10.40 14.20 0 8 0 2009.60 85.59 0 9 0 -10.50 20.90 0 10 0 -21.30 26.20 0 11 0 -7.10 33.40 0 12 0 324.27 58.79 0 13 0 69.29 51.29 0 -1 -1 1552.54 51.09 0 1 -1 1176.58 50.79 0 -1 1 1378.56 49.60 0 2 -1 -2.50 3.40 0 -2 -1 -4.30 3.20 0 2 1 0.10 3.40 0 -2 1 0.40 2.80 0 2 -1 -2.10 3.10 0 2 1 -5.00 2.70 0 -2 1 -1.20 3.10 0 3 1 476.65 20.80 0 -3 1 519.65 21.10 0 3 1 527.55 23.10 0 3 -1 508.85 22.80 0 4 1 0.40 6.50 0 4 -1 -1.10 6.70 0 -4 1 -1.20 4.80 0 -5 1 926.31 38.50 0 5 -1 986.40 41.60 0 5 1 933.41 41.80 0 6 1 5.90 11.30 0 -6 1 5.20 8.60 0 6 -1 6.80 11.40 0 7 -1 488.05 34.00 0 -7 1 533.25 28.60 0 7 1 519.85 34.80 0 8 -1 8.40 16.90 0 8 1 20.40 17.20 0 9 -1 148.79 25.50 0 9 1 133.89 24.40 0 10 1 11.60 26.20 0 10 -1 -8.70 25.50 0 11 1 249.58 40.00 0 11 -1 368.06 53.79 0 12 1 -20.10 63.19 0 12 -1 -32.30 50.69 0 13 -1 624.54 79.69 0 13 1 424.26 79.19 0 0 2 3034.60 110.89 0 0 -2 3198.68 110.89 0 1 2 -5.00 2.70 0 -1 2 -0.50 2.70 0 -1 2 -3.00 2.90 0 -1 -2 -4.20 2.90 0 1 -2 -7.40 2.30 0 2 2 9999.00 340.67 0 2 2 9641.33 340.77 0 -2 -2 9632.64 340.17 0 -2 2 9316.37 340.07 0 -2 -2 9780.32 340.67 0 2 -2 9752.42 340.27 0 3 2 -3.60 5.40 0 -3 2 -1.70 4.00 0 3 2 -3.90 4.60 0 4 2 1444.96 54.89 0 4 -2 1408.76 54.39 0 4 2 1369.26 52.89 0 -4 2 1298.57 52.09 0 5 2 -10.30 7.80 0 5 -2 -0.40 8.60 0 -5 2 -10.20 6.30 0 5 2 4.20 9.20 0 6 2 1110.69 48.70 0 -6 2 1073.39 43.80 0 6 -2 942.91 46.80 0 6 2 1086.29 44.30 0 7 2 8.20 15.10 0 7 -2 9.50 14.10 0 -7 2 -3.20 10.90 0 8 2 456.85 38.10 0 8 -2 468.25 36.90 0 9 -2 -1.40 22.30 0 9 2 -21.10 22.70 0 10 2 799.62 59.39 0 10 -2 757.82 56.79 0 11 2 3.00 34.50 0 11 -2 22.30 35.10 0 13 -2 50.89 51.29 0 13 2 17.60 53.29 0 0 -3 -2.10 3.80 0 0 3 1.30 3.80 0 -1 -3 361.56 16.50 0 1 3 364.26 16.70 0 -1 3 339.87 15.80 0 1 -3 335.47 15.70 0 -2 3 2.50 4.40 0 2 3 -5.20 4.50 0 -3 3 2438.26 92.59 0 3 3 2528.65 93.89 0 3 3 2679.13 93.89 0 4 3 -1.10 8.00 0 -4 3 -4.00 5.80 0 4 3 -1.40 7.00 0 -5 3 100.79 11.60 0 5 3 124.19 17.60 0 5 3 88.39 14.70 0 5 -3 82.39 11.90 0 -6 3 10.80 8.60 0 6 -3 6.70 10.70 0 6 3 -1.30 11.30 0 6 3 14.80 12.70 0 7 3 104.89 20.00 0 7 3 71.19 15.70 0 7 -3 57.59 16.40 0 8 3 -2.30 16.80 0 8 -3 0.40 18.40 0 8 3 10.80 19.50 0 9 3 208.88 29.80 0 9 -3 206.18 38.80 0 10 3 -22.80 29.70 0 10 -3 0.10 27.60 0 11 -3 187.28 39.00 0 11 3 235.58 43.00 0 13 -3 75.59 55.49 0 13 3 114.79 57.19 0 0 4 4144.69 148.99 0 -1 4 -7.00 4.80 0 1 4 -5.40 5.30 0 2 -4 1823.32 75.99 0 2 4 2214.28 78.79 0 -2 4 2193.38 77.39 0 -2 4 2126.19 76.89 0 -3 4 -0.10 6.20 0 4 4 3328.27 123.19 0 5 4 -5.40 11.10 0 5 -4 -5.20 10.00 0 5 4 -11.40 10.50 0 -6 4 1054.09 46.10 0 6 4 1114.99 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385.26 46.60 -10 6 6 419.46 40.90 10 6 -6 431.56 47.60 10 -7 6 58.39 20.40 -10 7 6 75.09 27.30 10 7 -6 25.90 30.40 -10 7 -6 61.09 25.80 10 7 6 75.59 29.80 10 7 6 100.49 25.90 10 8 -6 127.89 37.40 -10 8 6 143.39 35.50 -10 8 6 171.58 34.20 10 8 6 126.99 35.90 10 8 6 176.58 31.20 -10 8 -6 162.78 32.70 -10 9 6 109.99 40.70 10 9 -6 147.09 41.60 -10 9 6 101.29 39.30 -10 9 -6 123.69 36.00 10 9 6 192.48 35.00 10 9 6 149.88 41.90 10 10 -6 31.60 47.10 -10 10 6 -3.00 43.70 -10 10 6 44.60 44.30 10 10 6 86.59 46.30 10 10 6 61.39 37.80 -10 10 -6 -37.50 38.50 -10 11 6 58.49 53.09 10 11 -6 110.79 56.59 -10 11 6 161.08 56.29 10 11 6 238.78 56.09 -10 11 -6 51.09 48.60 10 0 7 331.57 27.10 10 -1 7 127.39 23.00 -10 -1 7 113.39 23.40 10 1 7 97.59 17.40 10 -2 7 1171.78 53.49 -10 -2 7 1097.59 51.99 10 2 7 1071.49 52.79 10 -3 7 51.99 17.70 10 3 7 63.69 17.00 -10 -3 7 28.90 16.60 -10 4 7 2534.25 105.19 10 -4 7 2617.44 102.59 10 4 7 2465.95 102.49 10 -5 7 28.30 18.70 -10 5 7 -15.40 20.50 10 5 7 75.09 20.10 10 -6 7 168.28 25.30 -10 6 7 180.38 29.10 -10 6 7 120.19 31.20 -10 7 7 5.40 29.60 10 7 -7 97.09 34.10 -10 7 7 11.40 32.20 10 -7 7 68.99 23.20 -10 8 7 148.19 37.80 10 -8 7 158.78 26.70 10 8 -7 80.29 38.70 -10 8 7 159.18 37.00 10 9 -7 81.19 46.80 -10 9 7 131.29 41.60 -10 9 7 102.89 41.10 10 9 7 90.29 44.00 10 10 -7 483.45 80.19 -10 10 7 340.27 60.69 -10 10 7 344.27 55.19 10 10 7 518.35 70.79 10 10 7 356.46 57.19 -10 0 8 60.29 19.00 10 0 8 54.29 16.00 -10 1 8 238.68 33.70 10 -1 8 207.58 27.20 10 1 8 209.08 28.30 -10 -1 8 188.58 30.90 -10 2 8 395.36 36.70 10 -2 8 367.46 33.60 -10 -2 8 371.36 35.30 10 2 8 370.26 33.90 -10 3 8 109.39 23.20 10 -3 8 96.69 20.60 10 3 8 177.08 31.50 -10 -3 8 59.49 22.10 -10 4 8 382.96 41.60 10 -4 8 409.86 35.60 10 4 8 437.46 36.60 10 -5 8 42.00 19.80 10 5 8 22.20 21.20 10 -6 8 104.89 25.20 -10 6 8 67.89 28.60 10 6 8 125.39 25.80 10 -7 8 140.69 28.80 -10 7 8 152.38 35.20 -10 8 8 151.08 39.30 -10 8 8 45.50 41.60 10 9 -8 521.05 75.89 -10 9 8 380.86 69.89 -10 9 8 392.06 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12 153.18 33.40 10 -2 12 398.76 54.99 -10 2 12 393.66 62.79 10 2 12 473.05 53.79 10 -3 12 14.30 33.20 -10 3 12 73.19 38.90 10 3 12 82.19 30.80 -10 -3 12 44.40 37.80 10 -4 12 155.38 36.70 10 4 12 62.29 51.89 -10 -4 12 158.48 38.50 10 -5 12 120.29 36.90 -10 5 12 183.58 49.30 10 5 12 185.48 39.70 -10 6 12 464.95 81.89 10 -6 12 486.55 58.69 10 6 12 467.75 66.89 10 0 13 620.14 73.59 -10 0 13 675.23 70.79 -10 1 13 66.69 43.40 10 -1 13 79.79 36.80 -10 -1 13 47.30 42.00 10 -2 13 373.26 61.49 10 2 13 395.46 60.99 10 -3 13 50.19 38.50 -10 3 13 42.00 47.00 10 3 13 81.99 36.90 -10 -3 13 71.99 42.30 -10 4 13 437.56 78.69 10 -4 13 498.55 66.49 10 4 13 527.45 64.19 10 -5 13 -34.80 39.30 -10 5 13 -18.10 53.89 10 5 13 30.40 41.50 -10 0 14 -43.70 58.59 10 0 14 -64.89 43.60 -10 1 14 37.70 50.39 10 -1 14 36.80 42.90 10 1 14 84.09 43.50 -10 -1 14 89.89 53.39 -10 2 14 268.87 55.89 10 -2 14 444.26 72.09 -10 -2 14 307.47 55.49 10 2 14 525.05 93.99 -10 3 14 75.49 55.79 10 -3 14 34.80 44.40 -10 -3 14 12.50 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6 0 148.79 26.30 14 6 0 241.78 38.50 14 7 0 321.67 48.10 -14 7 0 442.46 45.90 14 8 0 27.50 29.90 -14 8 0 26.20 30.40 14 9 0 -20.00 34.70 -14 10 0 116.79 41.80 14 10 0 140.49 46.80 14 11 0 231.18 55.59 -14 11 0 203.68 53.09 14 0 1 1270.67 56.09 -14 1 1 134.69 30.00 14 1 -1 125.99 23.50 14 -1 1 144.99 19.70 -14 1 1 117.89 20.90 14 1 1 144.89 23.10 -14 1 -1 154.68 29.20 14 1 1 106.89 19.90 -14 1 -1 126.39 20.40 14 2 -1 812.02 49.80 -14 2 1 802.12 46.40 14 -2 1 802.92 41.30 14 2 1 822.12 49.00 14 2 1 744.93 42.30 -14 2 -1 830.02 46.30 -14 3 1 54.79 19.30 14 3 -1 45.90 20.50 14 3 1 49.40 20.00 -14 3 -1 17.30 18.00 14 4 -1 1235.98 65.39 -14 4 1 1275.77 63.49 14 4 1 1246.88 65.29 -14 4 -1 1300.37 62.29 -14 5 1 51.29 21.80 14 5 -1 82.39 23.00 14 5 1 83.39 22.80 14 5 1 66.49 16.30 -14 5 -1 21.40 20.70 14 6 -1 1139.19 65.89 -14 6 1 1101.29 64.49 14 6 1 1201.38 65.69 14 6 1 1246.18 53.19 -14 6 -1 1191.48 62.49 -14 7 1 74.79 27.50 14 7 -1 0.90 26.70 -14 7 -1 48.60 26.00 14 7 1 5.30 27.60 -14 8 1 371.26 54.29 14 8 -1 408.56 51.59 -14 8 -1 337.77 52.79 14 8 1 382.86 52.29 14 9 -1 138.29 37.50 -14 9 1 83.99 39.40 -14 9 -1 110.79 37.50 14 9 1 128.59 39.70 -14 10 1 217.58 45.60 14 10 -1 218.28 49.10 14 10 1 225.58 48.60 -14 10 -1 224.48 42.90 -14 11 1 14.60 49.30 14 11 -1 -15.10 52.29 -14 11 -1 47.80 48.20 14 11 1 -9.60 52.19 14 0 2 850.01 42.60 14 -1 2 63.39 14.60 14 1 -2 33.30 20.30 -14 1 2 82.39 27.80 -14 1 2 52.89 19.10 -14 1 -2 81.09 18.20 -14 1 -2 83.99 25.20 14 1 2 70.89 14.50 14 1 2 56.39 20.30 14 2 -2 366.76 40.00 14 -2 2 399.16 28.80 -14 2 2 395.06 37.00 14 2 2 378.06 37.90 -14 2 -2 409.16 33.10 14 2 2 376.96 27.80 14 3 -2 0.70 20.70 14 -3 2 29.40 12.80 -14 3 2 -11.80 18.30 14 3 2 26.50 13.80 -14 3 -2 32.10 16.90 14 3 2 31.50 20.20 14 4 -2 372.96 41.30 -14 4 2 401.26 38.70 14 4 2 352.46 28.80 14 4 2 408.56 40.20 -14 4 -2 363.56 36.00 14 5 -2 60.59 23.30 -14 5 2 62.99 23.90 -14 5 -2 48.40 21.90 14 5 2 54.69 16.20 14 5 2 78.89 24.30 14 6 -2 346.37 43.40 -14 6 2 322.97 43.10 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738.93 51.19 14 4 -3 880.81 54.39 14 -4 3 714.03 41.70 14 4 3 749.33 40.80 14 4 3 711.03 49.90 -14 4 -3 809.02 48.00 -14 5 3 284.57 41.40 14 5 -3 269.27 44.20 14 -5 3 242.08 28.50 -14 5 -3 254.67 37.10 14 5 3 310.37 30.00 14 5 3 308.07 41.20 -14 6 3 819.02 56.69 14 6 -3 817.42 58.49 14 6 3 901.31 46.40 -14 6 -3 848.62 53.59 14 6 3 808.82 56.49 14 7 -3 29.70 29.10 -14 7 3 28.10 29.70 -14 7 -3 -6.10 26.70 14 7 3 21.80 28.40 14 7 3 56.19 19.80 -14 8 3 465.95 60.59 14 8 -3 469.35 59.29 14 8 3 579.04 56.69 -14 8 -3 374.16 55.79 -14 9 3 -25.20 38.40 14 9 -3 102.59 37.90 14 9 3 63.59 37.40 -14 9 -3 -12.90 34.20 14 10 -3 156.68 47.00 -14 10 3 74.29 44.60 -14 10 -3 130.59 43.30 14 10 3 137.09 48.90 14 0 4 94.69 17.80 -14 0 4 112.79 31.60 -14 0 4 88.39 21.90 -14 0 -4 101.59 19.70 -14 1 4 130.69 24.80 14 1 -4 94.09 26.90 14 -1 4 174.98 23.30 -14 1 4 244.98 55.59 -14 1 -4 161.18 28.50 14 1 4 145.29 26.40 14 1 4 165.58 22.30 14 2 -4 438.46 45.70 14 -2 4 429.36 31.20 -14 2 4 373.86 42.30 -14 2 -4 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288.17 59.59 -23 -2 -6 91.09 42.90 -23 2 6 46.20 55.99 23 -2 6 35.30 33.90 -23 -2 6 -44.40 56.59 23 2 6 9.90 32.80 -23 -2 6 54.59 84.49 -23 2 -6 113.29 51.49 -24 0 0 820.62 131.09 -24 0 0 771.92 78.19 -24 1 0 253.37 46.50 -24 -1 0 164.68 75.49 -24 -1 0 206.58 46.40 -24 2 0 144.59 46.60 -24 -2 0 212.68 71.19 -24 -2 0 228.08 44.60 -24 3 0 98.49 45.60 -24 4 0 247.58 50.59 24 4 0 128.59 64.39 -24 0 -1 45.30 39.30 -24 0 1 68.69 43.10 -24 0 1 33.00 70.29 -24 0 -1 94.09 68.49 -24 -1 -1 -14.80 40.20 -24 1 1 58.99 42.50 -24 -1 -1 3.40 68.09 -24 1 -1 3.20 40.50 -24 -1 1 19.70 41.90 -24 -1 1 -76.09 69.59 -24 2 1 -67.99 43.70 -24 -2 -1 38.70 65.79 -24 -2 -1 44.60 40.50 -24 2 -1 -55.19 41.60 -24 -2 1 97.49 42.20 -24 -2 1 -47.30 66.39 -24 3 1 72.59 45.40 -24 3 -1 19.60 42.40 -24 4 1 32.20 49.70 -24 4 -1 44.50 45.50 -24 0 -2 707.13 129.09 -24 0 2 733.93 81.69 -24 0 -2 751.82 74.99 -24 0 2 853.91 140.79 -24 -1 -2 -39.90 38.10 -24 1 2 24.60 46.70 -24 -1 -2 78.19 67.29 -24 -1 2 -7.70 72.69 -24 -1 2 12.70 45.80 -24 1 -2 -36.80 40.10 -24 -2 -2 517.45 116.69 -24 2 2 328.77 58.19 -24 -2 -2 412.36 68.19 -24 -2 2 474.95 74.79 -24 2 -2 404.46 71.89 -24 -2 2 454.35 83.69 -24 3 2 67.69 47.70 -24 3 -2 6.30 42.10 24 4 -2 132.49 62.99 24 4 2 272.57 58.19 -24 0 3 18.00 77.69 -24 0 -3 15.40 39.30 -24 0 3 81.69 45.90 24 0 3 37.70 29.50 -24 -1 -3 -28.70 39.60 -24 1 3 57.19 49.10 -24 -1 -3 133.49 69.29 -24 -1 3 71.39 75.99 24 1 3 -27.90 27.60 -24 1 -3 -33.20 39.20 -24 -1 3 6.90 45.70 -24 2 3 2.10 51.79 -24 -2 -3 -14.00 40.80 -24 -2 -3 39.20 64.69 -24 -2 3 -22.40 72.39 -24 2 -3 -29.60 40.40 -24 -2 3 -7.90 46.20 24 2 3 -20.50 28.60 -24 3 3 96.29 53.89 -24 3 -3 49.00 44.20 24 3 3 55.59 30.30 24 0 4 617.14 55.49 -24 0 4 520.25 86.09 -24 0 -4 502.85 69.99 -24 -1 -4 50.59 40.20 -24 1 4 -15.70 51.99 24 -1 4 -4.30 30.20 -24 -1 4 197.68 82.99 24 1 4 17.80 28.50 -24 1 -4 59.59 38.50 -24 -1 4 22.00 51.29 -24 -2 -4 567.14 126.19 24 -2 4 535.25 58.19 -24 -2 -4 500.35 77.89 -24 2 4 455.85 66.69 24 2 4 472.95 52.69 -24 2 -4 529.75 72.09 -24 -2 4 496.25 89.79 -24 -2 4 516.35 95.79 -24 3 4 59.89 56.09 -24 3 -4 -42.90 42.60 24 3 4 16.90 30.80 -24 0 5 179.68 55.29 24 0 5 117.69 34.60 -24 1 5 88.59 53.59 24 -1 5 64.79 32.10 -24 -1 -5 -11.40 41.10 -24 1 -5 53.49 40.80 -24 -1 5 79.19 56.09 24 1 5 12.80 30.80 -24 2 5 -59.69 56.79 -24 -2 -5 -44.20 74.09 24 -2 5 -24.70 33.30 -24 -2 -5 20.70 45.70 -24 -2 5 -88.19 55.49 -24 2 -5 20.10 39.60 -24 -2 5 6.50 82.49 24 2 5 -33.30 30.60 -25 0 0 -63.49 73.69 -25 -1 0 321.27 81.29 -25 -1 0 137.79 50.39 -25 1 0 178.68 50.39 -25 2 0 -37.70 49.60 -25 -2 0 -27.30 47.30 -25 -2 0 -12.50 74.69 -25 0 1 -28.80 46.90 -25 0 -1 -26.90 43.90 -25 0 1 -67.19 78.49 -25 1 1 19.10 50.29 -25 -1 -1 -23.50 44.20 -25 -1 -1 101.89 72.69 -25 1 -1 12.90 44.20 -25 -1 1 -20.90 49.80 -25 -1 1 79.59 81.59 -25 -2 -1 14.80 73.19 -25 -2 -1 29.10 47.80 -25 2 1 38.20 53.49 -25 -2 1 26.20 50.29 -25 2 -1 17.90 48.40 -25 -2 1 -32.20 76.69 -25 0 -2 -52.39 42.00 -25 0 2 -79.49 50.09 -25 1 2 583.64 88.39 -25 -1 -2 539.75 79.59 -25 1 -2 598.94 78.19 -25 -1 2 604.24 89.09 -25 2 2 -31.20 53.39 -25 -2 -2 14.70 72.69 -25 -2 -2 -21.70 47.50 -25 -2 2 -13.20 52.39 -25 2 -2 -67.19 44.50 -25 -2 2 -54.89 78.59 -25 0 -3 -35.00 42.40 -25 0 3 -50.89 50.09 -25 -1 -3 412.46 84.79 -25 1 3 253.77 57.59 -25 -1 -3 221.48 49.99 -25 1 -3 282.17 47.30 -25 -1 3 231.18 59.39 -25 -1 3 384.56 92.19 25 1 3 264.87 50.99 _computing_structure_solution 'SHELXT 2014/4 (Sheldrick, 2014)' ; _shelx_hkl_checksum 87866 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, z+1/2' '-x+1/2, y+1/2, z+1/2' 'x+1/2, -y+1/2, 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 Ru1 Ru 0.08374(2) 0.98933(5) 0.52511(10) 0.00971(17) Uani 1 1 d . . Cl1 Cl 0.03404(10) 1.1421(2) 0.6594(2) 0.0208(5) Uani 1 1 d . . C8 C 0.0719(4) 0.6662(8) 0.7638(7) 0.0126(18) Uani 1 1 d . . C18 C 0.1953(3) 1.0367(7) 0.5264(11) 0.0157(12) Uani 1 1 d . . H18 H 0.2269 1.0487 0.5873 0.019 Uiso 1 1 calc R U C21 C 0.1138(4) 1.1257(8) 0.3889(7) 0.0135(13) Uani 1 1 d . . H21 H 0.0892 1.1988 0.3564 0.016 Uiso 1 1 calc R U C19 C 0.1599(4) 1.1493(9) 0.4799(7) 0.0157(12) Uani 1 1 d . . C13 C 0.1389(4) 0.8830(8) 0.3895(8) 0.0136(13) Uani 1 1 d . . N3 N 0.1078(3) 0.7681(8) 0.7143(6) 0.0137(18) Uani 1 1 d . . H3 H 0.1519 0.7849 0.7268 0.016 Uiso 1 1 calc R U C17 C 0.1833(4) 0.9061(8) 0.4814(7) 0.0136(13) Uani 1 1 d . . H17 H 0.2063 0.8318 0.5151 0.016 Uiso 1 1 calc R U C22 C 0.1038(4) 0.9962(8) 0.3460(7) 0.0135(13) Uani 1 1 d . . H22 H 0.0721 0.9839 0.2852 0.016 Uiso 1 1 calc R U C6 C 0.0038(4) 0.7819(8) 0.6482(7) 0.0105(17) Uani 1 1 d . . N2 N 0.0675(3) 0.8400(6) 0.6439(6) 0.0101(15) Uani 1 1 d . . C7 C 0.0052(4) 0.6745(8) 0.7217(8) 0.0153(19) Uani 1 1 d . . H7 H -0.0325 0.6170 0.7399 0.018 Uiso 1 1 calc R U C9 C 0.1047(5) 0.5701(11) 0.8466(11) 0.042(2) Uani 1 1 d . . C20 C 0.1690(4) 1.2849(7) 0.5305(12) 0.0227(18) Uani 1 1 d . . H20A H 0.2031 1.3356 0.4862 0.034 Uiso 1 1 calc R U H20B H 0.1854 1.2759 0.6087 0.034 Uiso 1 1 calc R U H20C H 0.1245 1.3324 0.5299 0.034 Uiso 1 1 calc R U C2 C -0.1360(4) 0.9677(9) 0.4285(8) 0.0199(15) Uani 1 1 d . . H2 H -0.1660 1.0119 0.3767 0.024 Uiso 1 1 calc R U N1 N -0.0214(3) 0.9336(7) 0.5008(6) 0.0155(19) Uani 1 1 d . . C3 C -0.1615(4) 0.8763(8) 0.5041(8) 0.0199(15) Uani 1 1 d . . H5 H -0.2098 0.8573 0.5056 0.024 Uiso 1 1 calc R U C5 C -0.0469(4) 0.8421(8) 0.5737(7) 0.0117(18) Uani 1 1 d . . C4 C -0.1180(4) 0.8122(8) 0.5773(8) 0.0150(19) Uani 1 1 d . . H4 H -0.1355 0.7485 0.6299 0.018 Uiso 1 1 calc R U C1 C -0.0646(4) 0.9949(8) 0.4289(8) 0.017(2) Uani 1 1 d . . H1 H -0.0465 1.0585 0.3768 0.020 Uiso 1 1 calc R U C15 C 0.1821(5) 0.7245(9) 0.2456(10) 0.035(3) Uani 1 1 d . . H15A H 0.2286 0.7364 0.2777 0.053 Uiso 1 1 calc R U H15B H 0.1747 0.7902 0.1850 0.053 Uiso 1 1 calc R U H15C H 0.1778 0.6336 0.2146 0.053 Uiso 1 1 calc R U C14 C 0.1281(5) 0.7449(10) 0.3376(9) 0.019(2) Uani 1 1 d . . H14 H 0.0815 0.7452 0.3001 0.023 Uiso 1 1 calc R U C12 C 0.1683(5) 0.5061(10) 0.7936(10) 0.042(3) Uani 1 1 d . . H12A H 0.1546 0.4555 0.7261 0.063 Uiso 1 1 calc R U H12B H 0.1900 0.4452 0.8483 0.063 Uiso 1 1 calc R U H12C H 0.2015 0.5762 0.7721 0.063 Uiso 1 1 calc R U C10 C 0.0524(5) 0.4639(10) 0.8788(11) 0.042(2) Uani 1 1 d . . H10A H 0.0146 0.5052 0.9221 0.063 Uiso 1 1 calc R U H10B H 0.0750 0.3952 0.9252 0.063 Uiso 1 1 calc R U H10C H 0.0336 0.4225 0.8101 0.063 Uiso 1 1 calc R U C11 C 0.1270(5) 0.6467(10) 0.9533(9) 0.033(3) Uani 1 1 d . . H11A H 0.1636 0.7109 0.9338 0.049 Uiso 1 1 calc R U H11B H 0.1446 0.5831 1.0098 0.049 Uiso 1 1 calc R U H11C H 0.0871 0.6950 0.9846 0.049 Uiso 1 1 calc R U Cl2 Cl 0.25976(9) 0.8484(2) 0.74745(19) 0.0189(5) Uani 1 1 d . . C16 C 0.1284(5) 0.6313(9) 0.4221(9) 0.026(2) Uani 1 1 d . . H16A H 0.1750 0.6214 0.4541 0.038 Uiso 1 1 calc R U H16B H 0.1149 0.5478 0.3842 0.038 Uiso 1 1 calc R U H16C H 0.0953 0.6509 0.4830 0.038 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 Ru1 0.0039(2) 0.0168(3) 0.0084(3) 0.0013(4) 0.0006(4) 0.0001(2) Cl1 0.0176(10) 0.0229(12) 0.0220(13) -0.0040(11) 0.0103(10) 0.0018(9) C8 0.019(4) 0.009(4) 0.010(5) 0.002(4) -0.005(4) 0.000(3) C18 0.007(2) 0.028(3) 0.012(3) 0.007(3) 0.005(3) -0.004(2) C21 0.013(3) 0.018(3) 0.009(3) 0.005(3) 0.005(3) -0.002(3) C19 0.007(2) 0.028(3) 0.012(3) 0.007(3) 0.005(3) -0.004(2) C13 0.010(3) 0.019(3) 0.012(3) 0.000(3) 0.006(2) -0.003(2) N3 0.007(3) 0.020(4) 0.013(5) 0.004(3) -0.003(3) 0.002(3) C17 0.010(3) 0.019(3) 0.012(3) 0.000(3) 0.006(2) -0.003(2) C22 0.013(3) 0.018(3) 0.009(3) 0.005(3) 0.005(3) -0.002(3) C6 0.008(4) 0.017(4) 0.006(4) -0.003(4) 0.000(4) -0.003(3) N2 0.011(3) 0.013(4) 0.007(4) 0.002(3) -0.001(3) 0.002(3) C7 0.008(4) 0.015(4) 0.023(5) -0.001(4) 0.004(4) 0.000(3) C9 0.033(4) 0.035(4) 0.058(6) 0.033(4) -0.023(4) -0.009(3) C20 0.020(4) 0.026(4) 0.022(5) 0.000(7) 0.004(6) -0.002(3) C2 0.006(3) 0.032(4) 0.021(4) 0.001(3) -0.007(3) 0.000(2) N1 0.014(3) 0.022(4) 0.011(5) 0.000(3) 0.003(3) 0.002(3) C3 0.006(3) 0.032(4) 0.021(4) 0.001(3) -0.007(3) 0.000(2) C5 0.010(4) 0.008(4) 0.017(5) -0.005(4) -0.004(3) 0.001(3) C4 0.011(4) 0.015(5) 0.019(5) 0.003(4) 0.002(4) -0.005(4) C1 0.009(4) 0.023(5) 0.019(5) 0.013(4) -0.005(4) -0.005(4) C15 0.045(6) 0.031(6) 0.030(7) -0.015(5) 0.013(6) -0.010(5) C14 0.011(4) 0.028(6) 0.018(6) -0.002(4) -0.001(4) 0.001(4) C12 0.051(7) 0.039(7) 0.037(7) -0.010(6) -0.020(6) 0.028(6) C10 0.033(4) 0.035(4) 0.058(6) 0.033(4) -0.023(4) -0.009(3) C11 0.030(6) 0.047(6) 0.021(6) 0.010(5) -0.002(5) 0.016(5) Cl2 0.0085(9) 0.0297(12) 0.0184(12) -0.0011(10) -0.0021(9) 0.0052(9) C16 0.018(5) 0.026(5) 0.032(6) -0.007(5) -0.006(4) -0.008(4) 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' Cl Cl 0.1484 0.1585 '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' Ru Ru -1.2594 0.8363 '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' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle N2 Ru1 N1 76.1(3) N2 Ru1 C22 135.8(3) N1 Ru1 C22 92.7(3) N2 Ru1 C17 91.1(3) N1 Ru1 C17 135.9(3) C22 Ru1 C17 67.5(3) N2 Ru1 C21 170.8(3) N1 Ru1 C21 108.5(3) C22 Ru1 C21 37.7(3) C17 Ru1 C21 80.0(3) N2 Ru1 C13 102.7(3) N1 Ru1 C13 103.8(3) C22 Ru1 C13 37.9(3) C17 Ru1 C13 37.6(3) C21 Ru1 C13 68.6(3) N2 Ru1 C18 107.3(3) N1 Ru1 C18 172.1(4) C22 Ru1 C18 79.9(4) C17 Ru1 C18 38.2(3) C21 Ru1 C18 67.2(4) C13 Ru1 C18 68.6(4) N2 Ru1 C19 140.9(3) N1 Ru1 C19 141.5(3) C22 Ru1 C19 67.9(3) C17 Ru1 C19 68.4(3) C21 Ru1 C19 37.3(3) C13 Ru1 C19 81.5(3) C18 Ru1 C19 37.5(3) N2 Ru1 Cl1 87.0(2) N1 Ru1 Cl1 82.77(19) C22 Ru1 Cl1 134.6(2) C17 Ru1 Cl1 139.4(2) C21 Ru1 Cl1 101.4(2) C13 Ru1 Cl1 169.3(2) C18 Ru1 Cl1 104.4(3) C19 Ru1 Cl1 88.1(2) N3 C8 C7 105.9(7) N3 C8 C9 122.7(7) C7 C8 C9 131.4(8) C19 C18 C17 119.9(10) C19 C18 Ru1 72.4(4) C17 C18 Ru1 69.1(4) C22 C21 C19 121.0(8) C22 C21 Ru1 69.9(5) C19 C21 Ru1 73.2(5) C21 C19 C18 117.6(8) C21 C19 C20 122.1(8) C18 C19 C20 120.3(9) C21 C19 Ru1 69.5(5) C18 C19 Ru1 70.1(4) C20 C19 Ru1 129.1(6) C17 C13 C22 116.4(8) C17 C13 C14 123.0(8) C22 C13 C14 120.6(8) C17 C13 Ru1 69.6(5) C22 C13 Ru1 69.4(5) C14 C13 Ru1 131.6(6) N2 N3 C8 111.8(6) C13 C17 C18 122.5(8) C13 C17 Ru1 72.9(5) C18 C17 Ru1 72.7(4) C21 C22 C13 122.5(8) C21 C22 Ru1 72.4(5) C13 C22 Ru1 72.7(5) N2 C6 C7 109.6(7) N2 C6 C5 114.3(7) C7 C6 C5 136.0(7) N3 N2 C6 105.7(7) N3 N2 Ru1 135.7(5) C6 N2 Ru1 117.9(5) C6 C7 C8 107.0(7) C8 C9 C10 109.2(8) C8 C9 C12 109.8(10) C10 C9 C12 110.4(10) C8 C9 C11 109.5(9) C10 C9 C11 109.2(11) C12 C9 C11 108.7(8) C3 C2 C1 118.7(8) C1 N1 C5 119.2(7) C1 N1 Ru1 124.1(6) C5 N1 Ru1 116.1(5) C4 C3 C2 120.4(7) N1 C5 C4 121.4(8) N1 C5 C6 115.0(7) C4 C5 C6 123.6(8) C3 C4 C5 118.8(8) N1 C1 C2 121.7(8) C16 C14 C15 111.7(8) C16 C14 C13 114.3(8) C15 C14 C13 108.4(7) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Ru1 N2 2.068(7) Ru1 N1 2.120(7) Ru1 C22 2.151(9) Ru1 C17 2.153(8) Ru1 C21 2.184(8) Ru1 C13 2.195(8) Ru1 C18 2.201(6) Ru1 C19 2.231(8) Ru1 Cl1 2.397(2) C8 N3 1.361(11) C8 C7 1.379(11) C8 C9 1.507(13) C18 C19 1.423(11) C18 C17 1.425(12) C21 C22 1.400(11) C21 C19 1.414(12) C19 C20 1.488(12) C13 C17 1.401(12) C13 C22 1.413(11) C13 C14 1.521(13) N3 N2 1.344(10) C6 N2 1.360(10) C6 C7 1.379(12) C6 C5 1.445(11) C9 C10 1.510(15) C9 C12 1.518(16) C9 C11 1.535(16) C2 C3 1.367(12) C2 C1 1.402(11) N1 C1 1.337(11) N1 C5 1.347(10) C3 C4 1.363(11) C5 C4 1.402(11) C15 C14 1.518(13) C14 C16 1.510(13)