#------------------------------------------------------------------------------ #$Date: 2019-11-26 03:43:09 +0200 (Tue, 26 Nov 2019) $ #$Revision: 242529 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/13/25/4132579.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_4132579 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 'C26 H32 Cl2 N4 Ru' _chemical_formula_weight 572.52 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2014/7 _cell_angle_alpha 90 _cell_angle_beta 105.534(6) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 10.3321(14) _cell_length_b 15.1479(18) _cell_length_c 17.801(2) _cell_measurement_reflns_used 4680 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 22.69 _cell_measurement_theta_min 2.45 _cell_volume 2684.3(6) _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 0.999 _diffrn_measured_fraction_theta_max 0.993 _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 0.1334 _diffrn_reflns_av_unetI/netI 0.1622 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.993 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_number 26855 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.993 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 28.395 _diffrn_reflns_theta_min 2.375 _diffrn_source 'fine-focus sealed tube' _exptl_absorpt_coefficient_mu 0.804 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details '(Bera et al., 2017)' _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.417 _exptl_crystal_description block _exptl_crystal_F_000 1176 _exptl_crystal_size_max 0.200 _exptl_crystal_size_mid 0.180 _exptl_crystal_size_min 0.170 _exptl_transmission_factor_max 0.870 _exptl_transmission_factor_min 0.851 _refine_diff_density_max 1.084 _refine_diff_density_min -0.983 _refine_diff_density_rms 0.115 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 300 _refine_ls_number_reflns 6688 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.019 _refine_ls_R_factor_all 0.1840 _refine_ls_R_factor_gt 0.0744 _refine_ls_shift/su_max 0.035 _refine_ls_shift/su_mean 0.002 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0636P)^2^+2.1404P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1351 _refine_ls_wR_factor_ref 0.1666 _reflns_Friedel_coverage 0.000 _reflns_number_gt 3333 _reflns_number_total 6688 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file ja8b05009_si_002.cif _cod_data_source_block compound2 _cod_original_sg_symbol_H-M 'P 21/c' _cod_database_code 4132579 _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. Comments on CHECKCIF alerts: Isotropic non-H Atoms in Main Residue(s) ....... 1 Report Anisotropic treatment of C15 atom resulted in non-positive definite displacement tensors, and were therefore subjected to isotropic refinement. ; _shelx_estimated_absorpt_t_min 0.856 _shelx_estimated_absorpt_t_max 0.875 _exptl_absorpt_special_details SADABS _shelx_res_file ; C:\Users\user\Desktop\Final\4.res created by SHELXL-2014/7 REM 18aprc_0m in P2(1)/c REM R1 = 0.0702 for 3333 Fo > 4sig(Fo) and 0.1802 for all 6688 data REM 305 parameters refined using 0 restraints REM Highest difference peak 0.537, deepest hole -0.583, 1-sigma level 0.106 REM 18aprc_0m in P2(1)/c REM R1 = 0.0744 for 3333 Fo > 4sig(Fo) and 0.1839 for all 6688 data REM 300 parameters refined using 0 restraints REM Highest difference peak 1.085, deepest hole -0.982, 1-sigma level 0.115 REM 18aprc_0m in P2(1)/c REM R1 = 0.0744 for 3333 Fo > 4sig(Fo) and 0.1839 for all 6688 data REM 300 parameters refined using 0 restraints REM Highest difference peak 1.085, deepest hole -0.982, 1-sigma level 0.115 TITL 18aprc_0m in P2(1)/c CELL 0.71073 10.3321 15.1479 17.8014 90.000 105.534 90.000 ZERR 4.0000 0.0014 0.0018 0.0021 0.000 0.006 0.000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H CL N RU UNIT 104 128 8 16 4 MERG 2 FMAP 2 GRID PLAN 10 TEMP -173 SIZE 0.17 0.18 0.2 L.S. 2 ACTA WGHT 0.063600 2.140400 FVAR 0.09613 RU1 5 0.359028 0.680611 0.188377 11.00000 0.03125 0.04262 = 0.02549 -0.00362 0.00276 0.00340 CL1 3 0.307709 0.576874 0.277101 11.00000 0.07522 0.06135 = 0.04428 0.00636 0.01319 -0.01060 N3 4 0.542765 0.689115 0.271878 11.00000 0.03214 0.04584 = 0.03098 -0.00064 0.00294 0.00757 N2 4 0.331089 0.778863 0.270064 11.00000 0.03992 0.04245 = 0.03422 -0.00126 0.01035 0.00625 C26 1 0.377143 0.596907 0.090575 11.00000 0.05795 0.04633 = 0.03013 -0.00481 0.01195 0.00125 AFIX 43 H26 2 0.421435 0.541898 0.090873 11.00000 -1.20000 AFIX 0 C11 1 0.747131 0.676547 0.350412 11.00000 0.04070 0.05503 = 0.04338 -0.00623 -0.00202 -0.00172 C21 1 0.385122 0.759365 0.088578 11.00000 0.05812 0.04841 = 0.02769 0.00634 0.00748 0.00287 C25 1 0.450241 0.676767 0.091108 11.00000 0.03737 0.05287 = 0.02647 -0.00625 0.00754 -0.00133 AFIX 43 H25 2 0.543018 0.674575 0.093168 11.00000 -1.20000 AFIX 0 C19 1 0.179143 0.680370 0.090090 11.00000 0.02966 0.09862 = 0.03208 -0.00751 0.00023 0.00182 AFIX 43 H19 2 0.087133 0.683140 0.089755 11.00000 -1.20000 AFIX 0 N4 4 0.659799 0.644389 0.285784 11.00000 0.03867 0.04688 = 0.03185 -0.00183 0.00153 0.00889 C5 1 0.210626 0.821481 0.267205 11.00000 0.04378 0.05024 = 0.04195 0.00968 0.01524 0.00823 C6 1 0.320905 0.902559 0.385296 11.00000 0.07965 0.04597 = 0.03538 -0.00295 0.01766 0.00681 AFIX 43 H6 2 0.318543 0.945243 0.424006 11.00000 -1.20000 AFIX 0 N1 4 0.105094 0.799317 0.208850 11.00000 0.03935 0.08395 = 0.04980 -0.00563 0.00720 0.01624 C9 1 0.556351 0.747085 0.328997 11.00000 0.04277 0.03756 = 0.02213 -0.00346 0.00474 0.00220 C8 1 0.438744 0.797487 0.328932 11.00000 0.04469 0.03491 = 0.02629 -0.00058 0.00676 0.00518 C10 1 0.682919 0.742292 0.378450 11.00000 0.04759 0.05205 = 0.03557 -0.01463 -0.00555 -0.00387 AFIX 43 H10 2 0.718781 0.777651 0.423274 11.00000 -1.20000 AFIX 0 C17 1 0.241682 0.598038 0.089623 11.00000 0.04644 0.07308 = 0.02580 -0.01191 0.00650 -0.01970 C20 1 0.252826 0.758697 0.091055 11.00000 0.04095 0.06880 = 0.03851 0.00387 -0.00094 0.01687 AFIX 43 H20 2 0.209537 0.813534 0.093520 11.00000 -1.20000 AFIX 0 C4 1 0.206023 0.884813 0.325113 11.00000 0.06354 0.04496 = 0.05035 0.00010 0.03280 0.01841 C7 1 0.435406 0.858335 0.387827 11.00000 0.06426 0.03877 = 0.03911 -0.00465 0.01080 -0.00153 AFIX 43 H7 2 0.513560 0.868378 0.429384 11.00000 -1.20000 AFIX 0 C22 1 0.457716 0.846052 0.086320 11.00000 0.09469 0.06221 = 0.06255 0.00717 0.02561 -0.01015 AFIX 13 H22 2 0.410475 0.892216 0.109220 11.00000 -1.20000 AFIX 0 C16 1 0.669772 0.568998 0.237674 11.00000 0.05345 0.06687 = 0.04625 -0.00510 0.00351 0.01735 AFIX 137 H16A 2 0.582013 0.540005 0.220343 11.00000 -1.50000 H16B 2 0.735853 0.527217 0.267975 11.00000 -1.50000 H16C 2 0.698203 0.588733 0.192134 11.00000 -1.50000 AFIX 0 C23 1 0.599797 0.847891 0.130499 11.00000 0.13058 0.09389 = 0.18290 -0.01182 0.01068 -0.04777 AFIX 137 H23A 2 0.608142 0.830342 0.184578 11.00000 -1.50000 H23B 2 0.635294 0.907751 0.129533 11.00000 -1.50000 H23C 2 0.650785 0.806807 0.106873 11.00000 -1.50000 AFIX 0 C3 1 0.083475 0.928188 0.317141 11.00000 0.07040 0.06848 = 0.07853 0.00277 0.03620 0.02372 AFIX 43 H3 2 0.075363 0.972601 0.353285 11.00000 -1.20000 AFIX 0 C1 1 -0.008578 0.840982 0.204835 11.00000 0.04929 0.10751 = 0.06449 -0.00438 0.00997 0.03408 AFIX 43 H1 2 -0.085073 0.825808 0.163766 11.00000 -1.20000 AFIX 0 C18 1 0.169235 0.511964 0.091680 11.00000 0.08993 0.10298 = 0.05774 -0.02862 0.02713 -0.04575 AFIX 137 H18A 2 0.160931 0.479863 0.042818 11.00000 -1.50000 H18B 2 0.079545 0.523945 0.098017 11.00000 -1.50000 H18C 2 0.220171 0.476176 0.135541 11.00000 -1.50000 AFIX 0 C2 1 -0.023007 0.906257 0.257586 11.00000 0.06038 0.11843 = 0.09479 0.01111 0.03056 0.04563 AFIX 43 H2 2 -0.106997 0.934875 0.251531 11.00000 -1.20000 AFIX 0 CL2 3 0.766624 0.627763 0.060250 11.00000 0.06947 0.08184 = 0.06276 0.02325 0.03051 0.02190 C14 1 0.967547 0.641469 0.320278 11.00000 0.05720 0.15300 = 0.18186 -0.00274 0.04480 0.01805 AFIX 137 H14A 2 0.976463 0.702442 0.303949 11.00000 -1.50000 H14B 2 0.919672 0.606457 0.275069 11.00000 -1.50000 H14C 2 1.056997 0.616239 0.342408 11.00000 -1.50000 AFIX 0 C12 1 0.887831 0.640313 0.382494 11.00000 0.05112 0.10050 = 0.09369 -0.03156 -0.03832 0.02667 C13 1 0.884486 0.544577 0.411641 11.00000 0.15034 0.18422 = 0.12869 0.08584 -0.00843 0.08649 AFIX 137 H13A 2 0.976283 0.521440 0.428723 11.00000 -1.50000 H13B 2 0.831187 0.507824 0.369235 11.00000 -1.50000 H13C 2 0.843864 0.543693 0.455467 11.00000 -1.50000 AFIX 0 C24 1 0.439940 0.870009 0.001847 11.00000 0.29300 0.11327 = 0.09804 0.02783 0.04877 -0.09271 AFIX 137 H24A 2 0.451580 0.933824 -0.002631 11.00000 -1.50000 H24B 2 0.349657 0.853012 -0.028697 11.00000 -1.50000 H24C 2 0.507041 0.838745 -0.017970 11.00000 -1.50000 AFIX 0 C15 1 0.963654 0.699940 0.445331 11.00000 0.19573 AFIX 137 H15A 2 0.961114 0.760275 0.425117 11.00000 -1.50000 H15B 2 1.057141 0.680066 0.463279 11.00000 -1.50000 H15C 2 0.922676 0.698775 0.489008 11.00000 -1.50000 AFIX 0 HKLF 4 REM 18aprc_0m in P2(1)/c REM R1 = 0.0744 for 3333 Fo > 4sig(Fo) and 0.1840 for all 6688 data REM 300 parameters refined using 0 restraints END WGHT 0.0637 2.1345 REM Highest difference peak 1.084, deepest hole -0.983, 1-sigma level 0.115 Q1 1 0.9366 0.6765 0.4735 11.00000 0.05 1.08 Q2 1 0.9794 0.7386 0.4252 11.00000 0.05 0.95 Q3 1 0.4038 0.9236 0.1180 11.00000 0.05 0.55 Q4 1 0.6870 0.6188 0.0794 11.00000 0.05 0.46 Q5 1 0.4261 0.6859 0.1521 11.00000 0.05 0.42 Q6 1 0.4249 0.6352 0.1088 11.00000 0.05 0.41 Q7 1 0.6364 0.5762 0.0296 11.00000 0.05 0.41 Q8 1 0.5033 0.6168 0.0717 11.00000 0.05 0.40 Q9 1 0.7333 0.5801 0.0273 11.00000 0.05 0.39 Q10 1 0.7685 0.6367 0.4645 11.00000 0.05 0.38 ; _shelx_res_checksum 78103 _shelx_hkl_file ; 2 0 0 54.71 2.22 -2 0 0 55.06 2.22 -2 0 0 54.47 2.44 2 0 0 54.89 2.38 3 0 0 312.99 11.14 -3 0 0 289.05 11.45 -3 0 0 308.39 11.15 3 0 0 313.01 11.37 4 0 0 62.51 2.96 4 0 0 58.53 2.66 -4 0 0 54.02 3.07 -4 0 0 60.31 2.70 5 0 0 6.49 1.18 5 0 0 7.01 0.95 -5 0 0 5.89 1.41 -5 0 0 6.81 1.13 -6 0 0 15.70 2.16 6 0 0 11.51 1.39 -7 0 0 53.13 3.85 7 0 0 58.68 3.16 8 0 0 5.25 1.59 -8 0 0 9.99 2.16 -9 0 0 34.85 4.40 9 0 0 23.32 2.43 -10 0 0 25.20 4.48 10 0 0 20.56 2.90 11 0 0 14.17 2.91 -11 0 0 10.53 4.32 -12 0 0 -0.17 4.89 12 0 0 -0.92 2.82 13 0 0 2.12 3.73 -13 0 0 3.07 6.12 2 -1 0 290.16 10.49 -2 -1 0 289.61 10.23 -2 -1 0 271.16 10.24 2 -1 0 272.83 10.13 -2 1 0 284.67 10.15 2 1 0 287.17 10.24 2 1 0 287.24 10.21 -2 1 0 278.99 10.54 3 -1 0 41.91 2.32 3 -1 0 44.75 1.95 -3 -1 0 46.66 2.10 -3 -1 0 42.34 2.21 3 1 0 45.74 2.05 -3 1 0 40.71 2.37 -3 1 0 46.16 2.02 -4 -1 0 0.34 0.59 -4 -1 0 0.60 0.64 4 -1 0 -0.36 0.39 4 -1 0 -0.84 0.76 4 1 0 -0.35 0.58 4 1 0 -0.40 0.46 -4 1 0 0.16 0.47 -4 1 0 1.07 0.80 5 -1 0 139.54 5.42 -5 -1 0 134.40 5.54 -5 -1 0 120.39 5.84 5 -1 0 129.81 5.83 5 1 0 138.42 5.53 5 1 0 136.48 5.65 -5 1 0 133.23 6.21 -5 1 0 133.92 5.48 6 -1 0 27.71 1.85 -6 -1 0 28.73 2.48 -6 1 0 26.61 2.22 -6 1 0 24.89 2.49 6 1 0 24.59 1.97 -7 -1 0 0.38 1.52 7 -1 0 0.41 0.92 7 1 0 0.84 0.99 -7 1 0 2.63 1.79 8 -1 0 19.08 1.79 -8 -1 0 18.91 2.87 8 1 0 14.60 1.96 -8 1 0 25.31 3.29 -9 -1 0 4.28 2.21 9 -1 0 5.22 1.63 9 1 0 7.57 1.88 -9 1 0 9.34 2.82 10 -1 0 10.88 2.17 -10 -1 0 13.26 3.54 10 1 0 5.50 1.96 -10 1 0 11.50 3.86 11 -1 0 -0.21 2.23 -11 1 0 0.97 3.51 11 1 0 2.76 2.16 -12 -1 0 7.57 5.05 12 -1 0 10.49 3.17 12 1 0 6.10 2.81 -12 1 0 8.88 5.23 13 -1 0 3.10 3.59 -13 -1 0 9.70 5.44 13 1 0 5.97 3.76 -13 1 0 4.37 5.27 0 -2 0 378.64 14.36 0 2 0 385.90 14.37 0 2 0 452.53 14.52 -1 -2 0 183.31 6.29 1 -2 0 153.31 6.12 1 -2 0 167.77 6.49 -1 -2 0 175.30 6.18 1 2 0 177.22 6.28 1 2 0 178.23 6.22 -1 2 0 157.93 6.19 -1 2 0 173.61 6.52 -2 -2 0 13.35 0.78 2 -2 0 14.29 0.78 2 -2 0 14.79 1.19 -2 -2 0 15.95 0.92 2 2 0 14.84 0.93 -2 2 0 12.82 1.16 -2 2 0 15.70 0.82 2 2 0 15.08 0.83 -3 -2 0 36.92 1.86 3 -2 0 37.00 2.23 -3 -2 0 37.77 1.85 3 -2 0 36.69 1.70 3 2 0 39.09 1.90 -3 2 0 36.60 2.30 -3 2 0 35.42 1.72 3 2 0 38.13 1.80 -4 -2 0 20.28 1.35 4 -2 0 19.38 1.17 4 -2 0 19.03 1.78 -4 -2 0 17.52 1.46 4 2 0 19.79 1.28 4 2 0 18.41 1.32 -4 2 0 16.54 1.80 -4 2 0 16.97 1.23 5 -2 0 14.57 1.17 -5 -2 0 14.27 1.36 -5 -2 0 14.87 1.61 -5 2 0 13.39 1.31 -5 2 0 16.30 1.90 5 2 0 14.95 1.44 5 2 0 12.41 1.59 -6 -2 0 1.47 1.26 -6 2 0 0.60 1.36 6 2 0 0.40 0.81 -6 2 0 0.52 1.01 -7 -2 0 17.70 2.31 7 -2 0 16.99 1.72 -7 2 0 19.88 2.82 7 2 0 22.44 2.10 8 -2 0 7.05 1.44 -8 -2 0 4.45 1.84 -8 2 0 7.21 2.24 8 2 0 5.93 1.57 9 -2 0 4.06 1.53 -9 -2 0 2.78 2.39 9 2 0 4.01 1.71 -9 2 0 3.79 2.51 10 -2 0 11.27 2.29 -10 -2 0 7.15 3.14 10 2 0 12.00 2.24 -10 2 0 10.55 3.71 11 -2 0 9.06 2.40 -11 2 0 6.31 4.05 -12 -2 0 2.23 4.78 12 2 0 9.94 3.33 -12 2 0 -8.34 4.92 -13 -2 0 1.60 5.92 13 -2 0 2.27 3.43 13 2 0 -0.40 3.64 -13 2 0 -4.23 6.42 0 -3 0 -0.27 0.42 0 -3 0 -0.17 0.24 0 3 0 -0.19 0.35 0 3 0 0.07 0.26 1 -3 0 1.76 0.34 1 -3 0 2.35 0.62 -1 -3 0 2.28 0.41 -1 -3 0 1.69 0.34 1 -3 0 1.92 0.29 1 3 0 1.92 0.41 -1 3 0 2.00 0.56 -1 3 0 1.54 0.29 1 3 0 2.02 0.40 2 -3 0 8.76 0.62 -2 -3 0 9.19 0.65 2 -3 0 9.53 1.18 -2 -3 0 9.32 0.79 2 3 0 9.17 0.79 -2 3 0 9.43 0.64 -2 3 0 8.34 1.07 2 3 0 9.54 0.74 -3 -3 0 1.06 0.57 3 -3 0 3.62 0.94 -3 -3 0 1.81 0.44 3 -3 0 2.35 0.44 -3 3 0 1.56 0.88 -3 3 0 1.89 0.44 3 3 0 2.28 0.58 3 3 0 1.66 0.47 4 -3 0 -0.43 0.40 -4 -3 0 0.96 0.63 -4 -3 0 -0.01 0.58 4 -3 0 -1.51 0.97 -4 3 0 -0.14 1.02 4 3 0 0.26 0.56 -4 3 0 1.03 0.51 4 3 0 -0.33 0.51 5 -3 0 8.95 1.03 -5 -3 0 8.40 1.36 -5 3 0 9.68 1.24 5 3 0 9.25 1.24 -5 3 0 8.34 1.59 5 3 0 8.80 1.26 6 -3 0 23.30 1.61 -6 -3 0 17.79 2.00 -6 3 0 22.32 1.78 -6 3 0 22.23 2.59 6 3 0 19.62 1.81 7 -3 0 9.31 1.38 -7 -3 0 9.87 1.81 -7 3 0 8.55 2.19 7 3 0 9.63 1.71 8 -3 0 2.83 1.16 -8 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4.46 5.09 0 -6 0 64.44 3.24 0 -6 0 60.68 3.13 0 -6 0 65.26 2.85 0 6 0 57.97 3.08 0 6 0 64.18 2.90 1 -6 0 15.01 1.82 -1 -6 0 12.77 1.43 1 -6 0 15.25 1.12 1 -6 0 11.88 0.96 -1 -6 0 13.53 1.12 -1 -6 0 13.41 1.21 1 6 0 13.62 1.18 -1 6 0 13.05 1.04 -1 6 0 11.79 1.56 -2 -6 0 18.34 1.58 2 -6 0 15.23 1.19 -2 -6 0 17.31 1.34 2 -6 0 17.90 1.11 -2 -6 0 14.74 1.13 2 -6 0 15.94 2.15 -2 6 0 15.52 1.09 2 6 0 17.16 1.35 2 6 0 14.71 1.40 -2 6 0 13.55 1.70 -3 -6 0 6.16 0.83 3 -6 0 5.67 0.72 3 -6 0 6.10 0.89 3 -6 0 6.01 1.59 3 6 0 5.79 0.97 -3 6 0 6.04 0.82 -3 6 0 5.95 1.39 3 6 0 6.20 1.09 4 -6 0 37.05 1.95 -4 -6 0 34.89 1.92 -4 6 0 36.64 1.99 -4 6 0 37.95 3.00 4 6 0 32.69 2.26 4 6 0 34.62 2.16 -5 -6 0 29.87 1.94 5 -6 0 30.22 1.82 5 6 0 25.48 2.18 -5 6 0 27.88 3.00 -5 6 0 29.20 1.94 5 6 0 30.53 2.13 -6 -6 0 10.37 1.46 6 -6 0 9.16 1.22 -6 6 0 7.31 1.35 -6 6 0 11.56 2.64 6 6 0 10.04 1.85 7 -6 0 32.17 2.21 -7 -6 0 32.68 2.69 7 6 0 25.36 2.60 -7 6 0 33.10 3.92 8 -6 0 13.24 1.79 -8 -6 0 12.21 2.27 8 6 0 12.02 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3.32 7 -5 -22 0.59 3.49 7 -5 -22 0.03 3.40 7 5 -22 4.07 3.55 6 -5 -22 -0.98 2.97 6 -5 -22 0.62 3.38 6 5 -22 -0.12 3.29 5 -5 -22 -2.36 2.81 5 -5 -22 5.66 3.54 4 -5 -22 2.66 2.66 4 -5 -22 7.28 3.78 3 -5 -22 -5.48 2.99 3 -5 -22 3.26 2.63 2 -5 -22 -3.11 2.23 2 -5 -22 -1.35 3.22 1 -5 -22 3.29 2.82 1 -5 -22 1.30 3.44 0 -5 -22 2.93 3.62 0 -5 -22 0.14 2.99 6 -6 -22 4.46 3.75 6 -6 -22 -0.67 3.26 6 6 -22 5.52 4.32 5 -6 -22 0.85 3.60 5 -6 -22 -2.04 3.02 4 -6 -22 -0.35 3.55 4 -6 -22 0.35 2.98 3 -6 -22 0.22 3.63 3 -6 -22 3.60 2.74 2 -6 -22 4.95 2.79 2 -6 -22 0.75 3.40 1 -6 -22 0.23 2.81 1 -6 -22 6.28 3.73 5 -7 -22 7.11 3.08 5 -7 -22 5.31 3.67 4 -7 -22 1.99 3.73 4 -7 -22 9.70 3.46 3 -7 -22 1.31 2.70 3 -7 -22 0.75 3.25 2 -7 -22 -1.27 3.74 2 -7 -22 1.64 2.95 7 0 -23 2.61 4.18 6 0 -23 -1.54 3.81 5 0 -23 7.94 3.57 4 0 -23 2.34 3.35 3 0 -23 0.44 3.28 3 0 -23 -3.65 2.47 2 0 -23 -0.17 2.59 1 0 -23 -3.23 2.99 6 -1 -23 4.97 3.78 6 1 -23 -0.33 3.69 5 -1 -23 1.92 3.60 5 1 -23 -0.20 3.41 4 -1 -23 2.14 2.45 4 -1 -23 0.17 3.52 4 1 -23 3.71 3.49 3 -1 -23 3.04 3.31 3 -1 -23 2.14 2.62 2 -1 -23 -4.41 2.45 2 -1 -23 11.09 3.73 2 1 -23 -5.28 2.92 1 -1 -23 -3.48 2.79 1 1 -23 3.16 3.27 6 -2 -23 2.66 3.44 6 2 -23 5.75 3.61 5 -2 -23 -1.45 3.11 5 -2 -23 5.39 2.50 5 2 -23 0.46 3.62 4 -2 -23 8.18 3.57 4 -2 -23 1.60 2.47 4 2 -23 2.95 3.49 3 -2 -23 6.91 2.67 3 -2 -23 8.75 3.80 2 -2 -23 8.03 3.50 2 -2 -23 5.28 2.67 1 -2 -23 0.48 2.80 1 2 -23 2.89 3.87 6 -3 -23 4.62 2.93 6 -3 -23 -3.61 4.10 6 3 -23 -3.22 3.43 5 -3 -23 11.10 2.93 5 -3 -23 17.83 4.13 5 3 -23 1.13 3.40 4 -3 -23 8.39 4.07 4 -3 -23 1.44 2.57 3 -3 -23 1.73 2.59 3 -3 -23 5.51 3.39 2 -3 -23 -3.07 2.31 2 -3 -23 3.17 3.47 1 -3 -23 3.06 3.35 1 -3 -23 11.78 3.01 5 -4 -23 1.55 3.44 5 -4 -23 2.81 2.89 4 -4 -23 2.02 2.62 4 -4 -23 4.40 3.75 3 -4 -23 -1.97 2.67 3 -4 -23 4.43 3.61 2 -4 -23 -1.14 3.51 2 -4 -23 6.06 2.85 4 -5 -23 -3.48 3.94 3 -5 -23 -7.67 3.68 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 65051 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' 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 0.35903(5) 0.68061(3) 0.18838(2) 0.03405(17) Uani 1 1 d . . Cl1 Cl 0.30771(19) 0.57687(11) 0.27710(9) 0.0608(5) Uani 1 1 d . . N3 N 0.5428(4) 0.6891(3) 0.2719(2) 0.0374(11) Uani 1 1 d . . N2 N 0.3311(5) 0.7789(3) 0.2701(3) 0.0388(12) Uani 1 1 d . . C26 C 0.3771(7) 0.5969(4) 0.0906(3) 0.0448(16) Uani 1 1 d . . H26 H 0.4214 0.5419 0.0909 0.054 Uiso 1 1 calc R U C11 C 0.7471(6) 0.6765(4) 0.3504(3) 0.0489(16) Uani 1 1 d . . C21 C 0.3851(7) 0.7594(4) 0.0886(3) 0.0455(16) Uani 1 1 d . . C25 C 0.4502(6) 0.6768(4) 0.0911(3) 0.0391(14) Uani 1 1 d . . H25 H 0.5430 0.6746 0.0932 0.047 Uiso 1 1 calc R U C19 C 0.1791(6) 0.6804(6) 0.0901(3) 0.0550(18) Uani 1 1 d . . H19 H 0.0871 0.6831 0.0898 0.066 Uiso 1 1 calc R U N4 N 0.6598(5) 0.6444(3) 0.2858(3) 0.0407(12) Uani 1 1 d . . C5 C 0.2106(6) 0.8215(4) 0.2672(3) 0.0446(15) Uani 1 1 d . . C6 C 0.3209(7) 0.9026(4) 0.3853(4) 0.0532(18) Uani 1 1 d . . H6 H 0.3185 0.9452 0.4240 0.064 Uiso 1 1 calc R U N1 N 0.1051(5) 0.7993(4) 0.2088(3) 0.0586(16) Uani 1 1 d . . C9 C 0.5564(6) 0.7471(4) 0.3290(3) 0.0349(14) Uani 1 1 d . . C8 C 0.4387(6) 0.7975(3) 0.3289(3) 0.0358(14) Uani 1 1 d . . C10 C 0.6829(6) 0.7423(4) 0.3785(3) 0.0483(17) Uani 1 1 d . . H10 H 0.7188 0.7777 0.4233 0.058 Uiso 1 1 calc R U C17 C 0.2417(7) 0.5980(5) 0.0896(3) 0.0490(17) Uani 1 1 d . . C20 C 0.2528(7) 0.7587(5) 0.0911(3) 0.0516(18) Uani 1 1 d . . H20 H 0.2095 0.8135 0.0935 0.062 Uiso 1 1 calc R U C4 C 0.2060(7) 0.8848(4) 0.3251(4) 0.0496(17) Uani 1 1 d . . C7 C 0.4354(7) 0.8583(4) 0.3878(3) 0.0480(17) Uani 1 1 d . . H7 H 0.5136 0.8684 0.4294 0.058 Uiso 1 1 calc R U C22 C 0.4577(9) 0.8461(5) 0.0863(4) 0.072(2) Uani 1 1 d . . H22 H 0.4105 0.8922 0.1092 0.087 Uiso 1 1 calc R U C16 C 0.6698(7) 0.5690(4) 0.2377(4) 0.0574(19) Uani 1 1 d . . H16A H 0.5820 0.5400 0.2203 0.086 Uiso 1 1 calc R U H16B H 0.7359 0.5272 0.2680 0.086 Uiso 1 1 calc R U H16C H 0.6982 0.5887 0.1921 0.086 Uiso 1 1 calc R U C23 C 0.5998(11) 0.8479(6) 0.1305(7) 0.142(5) Uani 1 1 d . . H23A H 0.6081 0.8303 0.1846 0.213 Uiso 1 1 calc R U H23B H 0.6353 0.9078 0.1295 0.213 Uiso 1 1 calc R U H23C H 0.6508 0.8068 0.1069 0.213 Uiso 1 1 calc R U C3 C 0.0835(8) 0.9282(5) 0.3171(5) 0.069(2) Uani 1 1 d . . H3 H 0.0754 0.9726 0.3533 0.083 Uiso 1 1 calc R U C1 C -0.0086(7) 0.8410(5) 0.2048(4) 0.075(2) Uani 1 1 d . . H1 H -0.0851 0.8258 0.1638 0.090 Uiso 1 1 calc R U C18 C 0.1692(8) 0.5120(5) 0.0917(4) 0.082(3) Uani 1 1 d . . H18A H 0.1609 0.4799 0.0428 0.123 Uiso 1 1 calc R U H18B H 0.0795 0.5239 0.0980 0.123 Uiso 1 1 calc R U H18C H 0.2202 0.4762 0.1355 0.123 Uiso 1 1 calc R U C2 C -0.0230(8) 0.9063(6) 0.2576(5) 0.089(3) Uani 1 1 d . . H2 H -0.1070 0.9349 0.2515 0.107 Uiso 1 1 calc R U Cl2 Cl 0.76662(19) 0.62776(13) 0.06025(10) 0.0689(6) Uani 1 1 d . . C14 C 0.9675(9) 0.6415(7) 0.3203(7) 0.128(4) Uani 1 1 d . . H14A H 0.9765 0.7024 0.3039 0.192 Uiso 1 1 calc R U H14B H 0.9197 0.6065 0.2751 0.192 Uiso 1 1 calc R U H14C H 1.0570 0.6162 0.3424 0.192 Uiso 1 1 calc R U C12 C 0.8878(8) 0.6403(6) 0.3825(5) 0.093(3) Uani 1 1 d . . C13 C 0.8845(11) 0.5446(8) 0.4116(6) 0.163(5) Uani 1 1 d . . H13A H 0.9763 0.5214 0.4287 0.245 Uiso 1 1 calc R U H13B H 0.8312 0.5078 0.3692 0.245 Uiso 1 1 calc R U H13C H 0.8439 0.5437 0.4555 0.245 Uiso 1 1 calc R U C24 C 0.4399(14) 0.8700(7) 0.0018(6) 0.169(6) Uani 1 1 d . . H24A H 0.4516 0.9338 -0.0026 0.253 Uiso 1 1 calc R U H24B H 0.3497 0.8530 -0.0287 0.253 Uiso 1 1 calc R U H24C H 0.5070 0.8387 -0.0180 0.253 Uiso 1 1 calc R U C15 C 0.9637(15) 0.6999(9) 0.4453(8) 0.196(6) Uiso 1 1 d . . H15A H 0.9611 0.7603 0.4251 0.294 Uiso 1 1 calc R U H15B H 1.0571 0.6801 0.4633 0.294 Uiso 1 1 calc R U H15C H 0.9227 0.6988 0.4890 0.294 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 0.0312(3) 0.0426(3) 0.0255(2) -0.0036(2) 0.00276(18) 0.0034(3) Cl1 0.0752(13) 0.0613(11) 0.0443(9) 0.0064(8) 0.0132(9) -0.0106(10) N3 0.032(3) 0.046(3) 0.031(2) -0.001(2) 0.003(2) 0.008(3) N2 0.040(3) 0.042(3) 0.034(3) -0.001(2) 0.010(2) 0.006(3) C26 0.058(5) 0.046(4) 0.030(3) -0.005(3) 0.012(3) 0.001(3) C11 0.041(4) 0.055(4) 0.043(4) -0.006(3) -0.002(3) -0.002(4) C21 0.058(5) 0.048(4) 0.028(3) 0.006(3) 0.007(3) 0.003(4) C25 0.037(3) 0.053(4) 0.026(3) -0.006(3) 0.008(2) -0.001(3) C19 0.030(4) 0.099(6) 0.032(3) -0.008(4) 0.000(3) 0.002(4) N4 0.039(3) 0.047(3) 0.032(3) -0.002(2) 0.002(2) 0.009(3) C5 0.044(4) 0.050(4) 0.042(3) 0.010(3) 0.015(3) 0.008(4) C6 0.080(5) 0.046(4) 0.035(4) -0.003(3) 0.018(4) 0.007(4) N1 0.039(3) 0.084(4) 0.050(3) -0.006(3) 0.007(3) 0.016(3) C9 0.043(4) 0.038(3) 0.022(3) -0.003(3) 0.005(3) 0.002(3) C8 0.045(4) 0.035(3) 0.026(3) -0.001(2) 0.007(3) 0.005(3) C10 0.048(4) 0.052(4) 0.036(3) -0.015(3) -0.006(3) -0.004(3) C17 0.046(4) 0.073(5) 0.026(3) -0.012(3) 0.006(3) -0.020(4) C20 0.041(4) 0.069(5) 0.039(4) 0.004(3) -0.001(3) 0.017(4) C4 0.064(5) 0.045(4) 0.050(4) 0.000(3) 0.033(4) 0.018(4) C7 0.064(5) 0.039(4) 0.039(4) -0.005(3) 0.011(3) -0.002(4) C22 0.095(7) 0.062(5) 0.063(5) 0.007(4) 0.026(5) -0.010(5) C16 0.053(4) 0.067(5) 0.046(4) -0.005(4) 0.004(3) 0.017(4) C23 0.131(10) 0.094(8) 0.183(12) -0.012(8) 0.011(9) -0.048(7) C3 0.070(6) 0.068(5) 0.079(6) 0.003(4) 0.036(5) 0.024(5) C1 0.049(5) 0.108(7) 0.064(5) -0.004(5) 0.010(4) 0.034(5) C18 0.090(6) 0.103(7) 0.058(5) -0.029(5) 0.027(4) -0.046(5) C2 0.060(6) 0.118(8) 0.095(7) 0.011(6) 0.031(5) 0.046(5) Cl2 0.0695(13) 0.0818(14) 0.0628(11) 0.0232(10) 0.0305(10) 0.0219(11) C14 0.057(6) 0.153(10) 0.182(11) -0.003(9) 0.045(7) 0.018(6) C12 0.051(5) 0.100(7) 0.094(7) -0.032(6) -0.038(5) 0.027(5) C13 0.150(10) 0.184(12) 0.129(9) 0.086(9) -0.008(8) 0.086(9) C24 0.293(17) 0.113(9) 0.098(8) 0.028(7) 0.049(10) -0.093(10) 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' 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' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle N3 Ru1 C20 135.8(2) N3 Ru1 N2 74.70(18) C20 Ru1 N2 91.8(2) N3 Ru1 C25 93.63(19) C20 Ru1 C25 67.0(2) N2 Ru1 C25 135.9(2) N3 Ru1 C19 172.4(2) C20 Ru1 C19 37.9(2) N2 Ru1 C19 107.6(2) C25 Ru1 C19 79.6(2) N3 Ru1 C26 110.3(2) C20 Ru1 C26 79.2(2) N2 Ru1 C26 170.8(2) C25 Ru1 C26 37.9(2) C19 Ru1 C26 66.4(2) N3 Ru1 C21 104.8(2) C20 Ru1 C21 36.9(2) N2 Ru1 C21 103.7(2) C25 Ru1 C21 37.5(2) C19 Ru1 C21 67.6(2) C26 Ru1 C21 67.8(2) N3 Ru1 C17 142.9(2) C20 Ru1 C17 67.7(3) N2 Ru1 C17 140.9(2) C25 Ru1 C17 67.6(2) C19 Ru1 C17 37.1(2) C26 Ru1 C17 36.7(2) C21 Ru1 C17 80.1(2) N3 Ru1 Cl1 83.67(13) C20 Ru1 Cl1 138.0(2) N2 Ru1 Cl1 85.09(13) C25 Ru1 Cl1 136.66(17) C19 Ru1 Cl1 103.7(2) C26 Ru1 Cl1 103.01(17) C21 Ru1 Cl1 169.03(16) C17 Ru1 Cl1 88.98(17) C9 N3 N4 106.7(4) C9 N3 Ru1 118.7(4) N4 N3 Ru1 134.6(4) C8 N2 C5 118.6(5) C8 N2 Ru1 116.2(4) C5 N2 Ru1 125.2(4) C17 C26 C25 121.2(6) C17 C26 Ru1 72.9(3) C25 C26 Ru1 70.3(3) N4 C11 C10 107.2(5) N4 C11 C12 123.1(6) C10 C11 C12 129.7(6) C20 C21 C25 117.3(6) C20 C21 C22 120.5(7) C25 C21 C22 122.1(6) C20 C21 Ru1 68.7(4) C25 C21 Ru1 70.0(3) C22 C21 Ru1 130.8(4) C21 C25 C26 120.2(6) C21 C25 Ru1 72.5(3) C26 C25 Ru1 71.8(3) C17 C19 C20 120.0(6) C17 C19 Ru1 73.3(4) C20 C19 Ru1 69.4(3) C11 N4 N3 109.7(5) C11 N4 C16 130.7(5) N3 N4 C16 119.3(5) N1 C5 N2 116.7(5) N1 C5 C4 123.9(6) N2 C5 C4 119.4(6) C7 C6 C4 119.2(6) C1 N1 C5 116.9(6) N3 C9 C10 110.2(5) N3 C9 C8 115.9(5) C10 C9 C8 133.8(5) N2 C8 C7 122.8(5) N2 C8 C9 114.5(5) C7 C8 C9 122.6(5) C11 C10 C9 106.1(5) C26 C17 C19 118.2(6) C26 C17 C18 119.5(7) C19 C17 C18 122.3(7) C26 C17 Ru1 70.5(3) C19 C17 Ru1 69.6(3) C18 C17 Ru1 129.3(4) C21 C20 C19 122.9(6) C21 C20 Ru1 74.5(3) C19 C20 Ru1 72.7(4) C6 C4 C3 123.2(6) C6 C4 C5 120.1(6) C3 C4 C5 116.7(7) C6 C7 C8 119.9(6) C23 C22 C24 111.5(9) C23 C22 C21 115.6(7) C24 C22 C21 107.8(7) C2 C3 C4 119.3(7) N1 C1 C2 123.8(7) C3 C2 C1 119.4(7) C15 C12 C11 108.8(8) C15 C12 C13 111.9(9) C11 C12 C13 111.2(8) C15 C12 C14 104.9(9) C11 C12 C14 111.5(7) C13 C12 C14 108.4(8) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Ru1 N3 2.078(4) Ru1 C20 2.142(6) Ru1 N2 2.154(4) Ru1 C25 2.183(5) Ru1 C19 2.185(6) Ru1 C26 2.202(6) Ru1 C21 2.216(6) Ru1 C17 2.232(6) Ru1 Cl1 2.3861(17) N3 C9 1.322(6) N3 N4 1.350(6) N2 C8 1.338(7) N2 C5 1.391(7) C26 C17 1.395(8) C26 C25 1.425(8) C11 N4 1.349(7) C11 C10 1.363(8) C11 C12 1.515(9) C21 C20 1.379(8) C21 C25 1.416(8) C21 C22 1.518(9) C19 C17 1.406(9) C19 C20 1.407(9) N4 C16 1.448(7) C5 N1 1.332(8) C5 C4 1.418(8) C6 C7 1.350(8) C6 C4 1.396(9) N1 C1 1.318(8) C9 C10 1.369(8) C9 C8 1.435(7) C8 C7 1.403(8) C17 C18 1.509(9) C4 C3 1.400(9) C22 C23 1.468(12) C22 C24 1.510(11) C3 C2 1.349(10) C1 C2 1.399(10) C14 C12 1.547(12) C12 C15 1.487(14) C12 C13 1.544(13)