#------------------------------------------------------------------------------ #$Date: 2019-11-26 03:43:09 +0200 (Tue, 26 Nov 2019) $ #$Revision: 242529 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/13/25/4132578.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_4132578 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 'C28 H36 Cl8 N4 Ru' _chemical_formula_weight 813.28 _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 mixed _audit_creation_method SHELXL-2014/7 _cell_angle_alpha 90 _cell_angle_beta 104.621(4) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 15.255(3) _cell_length_b 13.690(3) _cell_length_c 16.939(3) _cell_measurement_reflns_used 9890 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 28.29 _cell_measurement_theta_min 2.49 _cell_volume 3423.0(12) _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 0.999 _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 0.0485 _diffrn_reflns_av_unetI/netI 0.0477 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 22162 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_theta_full 24.712 _diffrn_reflns_theta_max 24.712 _diffrn_reflns_theta_min 2.520 _diffrn_source 'fine-focus sealed tube' _exptl_absorpt_coefficient_mu 1.109 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details '(Bera et al., 2017)' _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.578 _exptl_crystal_description needle _exptl_crystal_F_000 1648 _exptl_crystal_size_max 0.210 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.190 _exptl_transmission_factor_max 0.811 _exptl_transmission_factor_min 0.795 _refine_diff_density_max 1.406 _refine_diff_density_min -1.777 _refine_diff_density_rms 0.170 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.072 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 380 _refine_ls_number_reflns 5815 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.072 _refine_ls_R_factor_all 0.0799 _refine_ls_R_factor_gt 0.0624 _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^)+(0.0825P)^2^+32.7951P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1695 _refine_ls_wR_factor_ref 0.1811 _reflns_Friedel_coverage 0.000 _reflns_number_gt 4698 _reflns_number_total 5815 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file ja8b05009_si_002.cif _cod_data_source_block compound1 _cod_original_sg_symbol_H-M 'P 21/c' _cod_database_code 4132578 _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 0.801 _shelx_estimated_absorpt_t_max 0.817 _exptl_absorpt_special_details SADABS _shelx_res_file ; C:\Users\user\Desktop\RU(P-C~1.CL2\25novf.res created by SHELXL-2014/7 REM 25novf_0m in P2(1)/c REM R1 = 0.0624 for 4698 Fo > 4sig(Fo) and 0.0799 for all 5815 data REM 380 parameters refined using 0 restraints REM Instructions for potential hydrogen bonds REM Highest difference peak 1.406, deepest hole -1.775, 1-sigma level 0.170 REM 25novf_0m in P2(1)/c REM R1 = 0.0624 for 4698 Fo > 4sig(Fo) and 0.0799 for all 5815 data REM 380 parameters refined using 0 restraints REM Instructions for potential hydrogen bonds REM Highest difference peak 1.406, deepest hole -1.777, 1-sigma level 0.170 TITL 25novf_0m in P2(1)/c CELL 0.71073 15.2546 13.6903 16.9392 90.000 104.621 90.000 ZERR 4.0000 0.0030 0.0027 0.0034 0.000 0.004 0.000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C RU N H CL UNIT 112 4 16 144 32 MERG 2 OMIT -2 50.1 SHEL 99999.00 0.85 FMAP 2 GRID PLAN 2 0 0 TEMP -173 SIZE 0.19 0.2 0.21 HTAB BOND $H CONF EQIV $1 -x, y+1/2, -z+1/2 HTAB C1 Cl2_$1 EQIV $2 x, -y+1/2, z+1/2 HTAB C10 Cl2_$2 HTAB C1S Cl5S HTAB C1S Cl2 HTAB C3S Cl2S HTAB N4 Cl2 HTAB C1 Cl2_$1 HTAB C10 Cl2_$2 HTAB C1S Cl5S HTAB C1S Cl2 HTAB C3S Cl2S HTAB N4 Cl2 L.S. 20 ACTA WGHT 0.082500 32.795101 FVAR 0.08013 RU1 2 0.084921 0.507902 0.244818 11.00000 0.01782 0.01065 = 0.00978 0.00102 0.00552 0.00171 N2 3 0.104552 0.521031 0.375147 11.00000 0.01536 0.01304 = 0.01169 0.00172 0.00354 0.00231 C8 1 0.152226 0.448534 0.419378 11.00000 0.01497 0.01551 = 0.01265 0.00041 0.00319 -0.00259 C7 1 0.167749 0.441697 0.505479 11.00000 0.02180 0.01621 = 0.01677 0.00308 0.00275 0.00237 AFIX 43 H7 4 0.201210 0.388686 0.534521 11.00000 -1.20000 AFIX 0 C6 1 0.133908 0.512200 0.545208 11.00000 0.02209 0.02033 = 0.01178 0.00209 0.00508 0.00167 AFIX 43 H6 4 0.144142 0.509733 0.602868 11.00000 -1.20000 AFIX 0 C4 1 0.083159 0.589718 0.500527 11.00000 0.01433 0.01598 = 0.01647 -0.00021 0.00572 -0.00196 C5 1 0.067823 0.590490 0.415136 11.00000 0.01373 0.01376 = 0.01354 -0.00055 0.00411 -0.00174 N1 3 0.016339 0.659169 0.367576 11.00000 0.02086 0.01446 = 0.01541 -0.00085 0.00587 0.00075 C1 1 -0.018031 0.728618 0.404607 11.00000 0.01838 0.01456 = 0.02491 0.00132 0.01018 0.00099 AFIX 43 H1 4 -0.054252 0.777064 0.371554 11.00000 -1.20000 AFIX 0 C2 1 -0.004947 0.735920 0.488790 11.00000 0.02268 0.01725 = 0.01725 -0.00417 0.01053 0.00159 AFIX 43 H2 4 -0.030446 0.788554 0.512012 11.00000 -1.20000 AFIX 0 C3 1 0.045489 0.665571 0.537421 11.00000 0.02144 0.02212 = 0.01190 -0.00128 0.00797 -0.00270 AFIX 43 H3 4 0.054854 0.667967 0.595002 11.00000 -1.20000 AFIX 0 C9 1 0.189925 0.377993 0.373570 11.00000 0.01823 0.01454 = 0.01710 0.00348 0.00739 0.00193 N3 3 0.173248 0.395381 0.293237 11.00000 0.02341 0.01534 = 0.01220 -0.00031 0.00695 0.00591 N4 3 0.214526 0.323609 0.262352 11.00000 0.02162 0.01565 = 0.01213 -0.00056 0.00666 0.00413 C11 1 0.257927 0.260236 0.321323 11.00000 0.01631 0.01911 = 0.01592 0.00149 0.00473 0.00053 C10 1 0.242068 0.293339 0.394433 11.00000 0.02284 0.01622 = 0.01630 0.00259 0.00652 0.00108 AFIX 43 H10 4 0.262283 0.264633 0.446953 11.00000 -1.20000 AFIX 0 C12 1 0.310625 0.174108 0.303659 11.00000 0.02294 0.01810 = 0.02410 0.00400 0.01067 0.00774 C14 1 0.348166 0.118479 0.382609 11.00000 0.02923 0.02147 = 0.02366 -0.00025 0.00757 0.01031 AFIX 137 H14A 4 0.391597 0.159775 0.420782 11.00000 -1.50000 H14B 4 0.378680 0.059125 0.371137 11.00000 -1.50000 H14C 4 0.298427 0.100667 0.406818 11.00000 -1.50000 AFIX 0 C13 1 0.249486 0.108194 0.240252 11.00000 0.02957 0.01997 = 0.02514 -0.00220 0.01057 0.00710 AFIX 137 H13A 4 0.198439 0.085771 0.260898 11.00000 -1.50000 H13B 4 0.284222 0.051658 0.229626 11.00000 -1.50000 H13C 4 0.226560 0.144854 0.189542 11.00000 -1.50000 AFIX 0 C15 1 0.389918 0.210279 0.270468 11.00000 0.02723 0.03035 = 0.02815 0.00202 0.01109 0.00867 AFIX 137 H15A 4 0.366115 0.243166 0.218042 11.00000 -1.50000 H15B 4 0.427213 0.154503 0.262855 11.00000 -1.50000 H15C 4 0.426926 0.256204 0.309367 11.00000 -1.50000 AFIX 0 C18 1 0.007055 0.635393 0.186567 11.00000 0.02614 0.01623 = 0.01531 0.00748 0.00833 0.00556 AFIX 43 H18 4 -0.042910 0.668600 0.198217 11.00000 -1.20000 AFIX 0 C17 1 -0.008503 0.557105 0.128853 11.00000 0.01976 0.01419 = 0.01152 0.00379 0.00592 -0.00242 C16 1 0.066445 0.510351 0.112480 11.00000 0.03232 0.01477 = 0.01305 0.00341 0.01078 0.00209 AFIX 43 H16 4 0.057545 0.457735 0.074725 11.00000 -1.20000 AFIX 0 C21 1 0.156705 0.541150 0.152212 11.00000 0.02116 0.01801 = 0.01092 0.00508 0.00832 0.00336 AFIX 43 H21 4 0.206683 0.507990 0.140542 11.00000 -1.20000 AFIX 0 C20 1 0.172995 0.618967 0.207835 11.00000 0.02016 0.02246 = 0.01500 0.00571 0.00559 -0.00079 C19 1 0.095430 0.663339 0.225955 11.00000 0.02702 0.01084 = 0.01543 0.00160 0.00811 -0.00060 AFIX 43 H19 4 0.104252 0.713394 0.266034 11.00000 -1.20000 AFIX 0 C22 1 0.267480 0.654818 0.249479 11.00000 0.02403 0.03330 = 0.02365 0.00158 0.00327 -0.00419 AFIX 13 H22 4 0.269510 0.669111 0.307807 11.00000 -1.20000 AFIX 0 C24 1 0.341621 0.579427 0.247686 11.00000 0.02707 0.05890 = 0.04424 -0.00699 0.00759 -0.00176 AFIX 137 H24A 4 0.325410 0.516435 0.267574 11.00000 -1.50000 H24B 4 0.399489 0.601763 0.282716 11.00000 -1.50000 H24C 4 0.347233 0.572017 0.191627 11.00000 -1.50000 AFIX 0 C23 1 0.283363 0.751020 0.208295 11.00000 0.03847 0.04925 = 0.04722 0.00870 0.00170 -0.02402 AFIX 137 H23A 4 0.280540 0.738825 0.150699 11.00000 -1.50000 H23B 4 0.343141 0.777165 0.235567 11.00000 -1.50000 H23C 4 0.236527 0.798371 0.212377 11.00000 -1.50000 AFIX 0 C25 1 -0.102717 0.523782 0.089782 11.00000 0.02835 0.03148 = 0.01344 0.00503 0.00547 -0.00611 AFIX 137 H25A 4 -0.132781 0.571926 0.049084 11.00000 -1.50000 H25B 4 -0.136608 0.516940 0.131518 11.00000 -1.50000 H25C 4 -0.100568 0.460618 0.063113 11.00000 -1.50000 AFIX 0 CL1 5 -0.032485 0.397480 0.257607 11.00000 0.02947 0.01645 = 0.01735 0.00178 0.00770 -0.00622 CL1S 5 0.508864 0.417456 0.191749 11.00000 0.03793 0.03729 = 0.04493 0.00289 0.01072 -0.00505 CL2S 5 0.484179 0.245145 0.086655 11.00000 0.05625 0.03527 = 0.05084 0.00349 0.02220 0.00345 CL5S 5 0.621757 0.394497 -0.023408 11.00000 0.06544 0.05811 = 0.06020 0.01901 0.02920 0.02629 CL3S 5 0.599399 0.497974 0.380355 11.00000 0.09855 0.14258 = 0.07721 0.01854 0.02048 -0.01029 C1S 1 0.452246 0.368679 0.096632 11.00000 0.03036 0.04246 = 0.04031 0.00853 0.01246 -0.00008 AFIX 23 H1S1 4 0.466617 0.408296 0.052636 11.00000 -1.20000 H1S2 4 0.386031 0.372088 0.090467 11.00000 -1.20000 AFIX 0 CL6S 5 0.778103 0.272737 0.045621 11.00000 0.04379 0.05696 = 0.07235 -0.00518 0.01202 0.01598 C3S 1 0.697775 0.351215 0.066973 11.00000 0.03779 0.05727 = 0.05531 -0.00631 0.01377 0.00282 AFIX 23 H3S1 4 0.728789 0.407449 0.098919 11.00000 -1.20000 H3S2 4 0.663214 0.316570 0.100646 11.00000 -1.20000 AFIX 0 CL2 5 0.226350 0.322971 0.083803 11.00000 0.02228 0.02333 = 0.01421 -0.00109 0.00697 0.00225 CL4S 5 0.621969 0.451714 0.548086 11.00000 0.09415 0.15280 = 0.07400 0.01101 0.01723 -0.02880 C2S 1 0.586891 0.412430 0.446844 11.00000 0.16175 0.08646 = 0.08200 0.01717 -0.01568 -0.01443 AFIX 23 H2S1 4 0.622396 0.354009 0.439773 11.00000 -1.20000 H2S2 4 0.522328 0.393123 0.434841 11.00000 -1.20000 AFIX 0 H4A 4 0.211193 0.321162 0.204967 11.00000 0.01118 HKLF 4 REM 25novf_0m in P2(1)/c REM R1 = 0.0624 for 4698 Fo > 4sig(Fo) and 0.0799 for all 5815 data REM 380 parameters refined using 0 restraints END WGHT 0.0824 32.8079 REM Instructions for potential hydrogen bonds HTAB C1 Cl2_$1 HTAB C10 Cl2_$2 HTAB C1S Cl5S HTAB C1S Cl2 HTAB C3S Cl2S HTAB N4 Cl2 REM Highest difference peak 1.406, deepest hole -1.777, 1-sigma level 0.170 Q1 1 0.5000 0.5000 0.5000 10.50000 0.05 1.41 Q2 1 0.1416 0.5145 0.2643 11.00000 0.05 1.16 ; _shelx_res_checksum 1588 _shelx_hkl_file ; 2 0 0 106.01 4.12 -2 0 0 108.86 4.13 -2 0 0 100.18 4.11 3 0 0 1.03 0.19 -3 0 0 0.97 0.18 -4 0 0 19.85 0.92 -4 0 0 19.78 0.92 4 0 0 21.26 0.93 -5 0 0 1.92 0.34 5 0 0 2.72 0.34 -5 0 0 2.51 0.32 6 0 0 53.08 2.25 -6 0 0 53.19 2.25 -6 0 0 52.70 2.25 -7 0 0 263.22 10.04 7 0 0 253.71 10.02 -7 0 0 245.67 10.01 -8 0 0 46.92 2.11 -9 0 0 3.75 0.54 -10 0 0 70.99 3.13 -11 0 0 10.31 1.04 -12 0 0 55.64 2.69 -13 0 0 61.19 2.97 -14 0 0 5.04 0.96 -15 0 0 16.34 1.79 -16 0 0 16.02 1.94 -17 0 0 22.20 2.23 -18 0 0 3.95 1.53 -19 0 0 8.94 1.85 2 -1 0 0.13 0.15 -2 -1 0 -0.13 0.14 -2 1 0 0.27 0.16 -2 1 0 0.33 0.17 2 1 0 0.26 0.15 2 1 0 0.19 0.14 3 -1 0 92.54 3.71 -3 -1 0 92.34 3.67 3 -1 0 98.31 3.68 3 -1 0 92.69 3.71 -3 -1 0 89.65 3.69 3 1 0 90.54 3.66 -3 1 0 91.06 3.71 -3 1 0 99.96 3.67 3 1 0 90.45 3.68 -3 1 0 95.72 3.71 -4 -1 0 153.91 6.01 4 -1 0 153.25 6.06 4 -1 0 151.80 6.06 -4 -1 0 150.27 6.04 -4 1 0 151.51 6.05 4 1 0 155.23 5.99 4 1 0 149.86 6.03 -4 1 0 153.21 6.06 -4 1 0 162.66 6.00 5 -1 0 2.61 0.38 -5 -1 0 3.49 0.29 5 -1 0 3.01 0.37 -5 -1 0 2.97 0.35 5 1 0 3.58 0.29 -5 1 0 3.00 0.36 5 1 0 2.72 0.35 -6 -1 0 5.16 0.48 -6 -1 0 5.33 0.49 6 -1 0 4.09 0.50 -6 1 0 4.97 0.50 6 1 0 5.21 0.48 -7 -1 0 0.34 0.30 7 -1 0 0.51 0.33 -7 -1 0 1.05 0.30 -7 1 0 0.60 0.33 7 1 0 0.06 0.23 7 1 0 0.69 0.33 -8 -1 0 16.17 1.27 -8 -1 0 14.67 0.91 -8 1 0 13.65 0.91 -9 -1 0 1.92 0.45 -9 1 0 1.40 0.41 -10 -1 0 2.59 0.54 -10 1 0 2.34 0.57 -11 -1 0 2.26 0.60 -11 1 0 2.75 0.62 -12 -1 0 4.79 0.81 -12 1 0 4.54 0.75 -13 -1 0 1.62 0.81 -13 1 0 2.41 0.78 -14 -1 0 -0.78 0.86 -14 1 0 0.49 0.93 -15 -1 0 0.94 0.98 -15 1 0 0.54 1.01 -16 -1 0 0.41 2.12 -16 1 0 -0.04 1.13 -17 -1 0 -0.42 1.31 -18 -1 0 3.54 1.56 -18 1 0 -0.28 1.40 -19 -1 0 1.37 1.78 -19 1 0 -0.70 1.61 0 -2 0 191.35 7.37 0 -2 0 174.24 7.33 0 2 0 198.76 7.37 0 2 0 189.61 7.35 -1 -2 0 185.42 7.34 -1 -2 0 177.50 7.31 1 -2 0 184.83 7.32 1 -2 0 197.06 7.35 -1 2 0 180.34 7.34 -1 2 0 186.81 7.32 -1 2 0 191.87 7.34 1 2 0 193.18 7.34 1 2 0 193.56 7.34 2 -2 0 313.74 11.52 -2 -2 0 291.21 11.51 -2 -2 0 284.99 11.48 2 -2 0 293.73 11.51 2 2 0 298.30 11.48 -2 2 0 290.46 11.52 -2 2 0 305.75 11.52 -2 2 0 295.89 11.51 2 2 0 289.18 11.50 3 -2 0 16.47 0.78 -3 -2 0 16.34 0.75 3 -2 0 14.86 0.76 -3 -2 0 17.00 0.77 3 2 0 17.03 0.74 -3 2 0 15.41 0.77 -3 2 0 16.61 0.78 -3 2 0 16.93 0.79 3 2 0 15.24 0.74 4 -2 0 896.15 35.23 -4 -2 0 887.94 35.23 -4 -2 0 878.10 35.23 4 -2 0 851.87 35.25 4 2 0 893.58 35.22 -4 2 0 942.20 35.27 4 2 0 918.08 35.22 -4 2 0 1000.00 35.24 -4 2 0 928.22 35.27 -5 -2 0 165.09 6.69 5 -2 0 167.33 6.69 5 -2 0 172.43 6.75 -5 -2 0 163.78 6.70 5 2 0 165.00 6.69 -5 2 0 167.64 6.74 -5 2 0 183.22 6.69 5 2 0 172.52 6.67 -5 2 0 172.51 6.75 -6 -2 0 54.05 2.31 6 -2 0 53.40 2.34 -6 -2 0 53.83 2.28 6 2 0 56.83 2.25 -6 2 0 53.96 2.35 6 2 0 53.35 2.30 -6 2 0 59.53 2.27 -6 2 0 53.76 2.36 7 -2 0 21.53 1.20 -7 -2 0 22.14 1.09 -7 -2 0 23.96 1.16 7 2 0 23.92 1.16 -7 2 0 24.70 1.50 7 2 0 25.11 1.07 -7 2 0 20.97 1.17 -8 -2 0 27.27 1.47 -8 -2 0 28.84 1.37 -8 -2 0 29.26 1.46 8 2 0 32.85 1.35 8 2 0 30.50 1.48 -8 2 0 28.39 1.48 -9 -2 0 25.30 1.41 -9 -2 0 26.26 1.32 9 2 0 27.58 1.26 -9 2 0 27.54 1.43 -10 -2 0 10.95 0.98 -10 2 0 12.86 0.97 10 2 0 12.88 0.84 -11 -2 0 64.57 2.95 -11 2 0 65.08 2.96 -12 -2 0 53.44 2.58 -12 2 0 53.04 2.62 -13 -2 0 9.03 1.24 -13 2 0 8.88 1.28 -14 -2 0 0.94 0.96 -14 2 0 0.58 0.86 -15 -2 0 -0.94 0.99 -15 2 0 0.69 1.08 -16 -2 0 4.28 2.06 -16 2 0 2.47 1.21 -17 -2 0 20.27 2.30 -17 2 0 19.96 2.24 -18 -2 0 14.77 2.47 -18 2 0 15.25 2.40 -19 -2 0 10.24 2.05 0 -3 0 0.18 0.15 0 -3 0 0.39 0.16 0 3 0 0.37 0.16 0 3 0 0.25 0.16 1 -3 0 25.30 1.17 -1 -3 0 26.30 1.17 1 -3 0 25.73 1.13 -1 -3 0 26.56 1.13 -1 3 0 25.18 1.17 1 3 0 26.06 1.12 -1 3 0 27.34 1.17 -1 3 0 26.59 1.14 1 3 0 27.32 1.18 2 -3 0 39.79 1.68 2 -3 0 41.65 1.73 -2 -3 0 38.43 1.67 -2 -3 0 40.41 1.71 -2 3 0 40.96 1.73 -2 3 0 40.83 1.70 2 3 0 39.97 1.70 -2 3 0 38.72 1.70 2 3 0 40.18 1.65 -3 -3 0 308.94 12.35 -3 -3 0 311.86 12.39 3 -3 0 330.70 12.40 3 -3 0 315.78 12.38 -3 3 0 322.63 12.39 3 3 0 316.23 12.33 -3 3 0 319.47 12.40 3 3 0 308.32 12.37 -3 3 0 318.43 12.39 -4 -3 0 78.69 3.31 4 -3 0 81.48 3.32 -4 -3 0 78.20 3.28 4 -3 0 85.48 3.32 -4 3 0 82.96 3.34 4 3 0 77.49 3.28 -4 3 0 80.21 3.31 4 3 0 82.65 3.26 -4 3 0 81.69 3.32 -4 3 0 84.81 3.33 -5 -3 0 28.83 1.34 5 -3 0 29.61 1.34 5 -3 0 28.43 1.34 -5 -3 0 28.97 1.33 -5 3 0 30.63 1.37 -5 3 0 33.11 1.37 5 3 0 28.20 1.29 -5 3 0 30.81 1.40 5 3 0 28.16 1.30 -5 3 0 28.03 1.35 -6 -3 0 24.56 1.19 -6 -3 0 25.23 1.19 6 -3 0 25.35 1.34 6 -3 0 24.04 1.19 -6 3 0 24.37 1.26 6 3 0 23.59 1.13 -6 3 0 26.83 1.20 6 3 0 24.25 1.15 -6 3 0 24.01 1.31 -7 -3 0 0.13 0.32 -7 -3 0 0.82 0.30 7 -3 0 0.55 0.32 7 -3 0 -0.05 0.30 -7 3 0 0.74 0.31 7 3 0 0.00 0.32 7 3 0 1.10 0.28 -8 -3 0 0.12 0.35 8 -3 0 0.49 0.36 -8 -3 0 0.53 0.51 8 -3 0 0.36 0.36 -8 3 0 0.87 0.31 -8 3 0 0.36 0.36 8 3 0 0.51 0.32 8 3 0 0.18 0.38 -9 -3 0 26.59 1.47 -9 -3 0 30.01 1.45 9 3 0 30.03 1.36 -9 3 0 25.77 1.50 -10 -3 0 13.82 1.10 -10 -3 0 16.88 1.07 10 3 0 13.57 0.97 -10 3 0 14.79 1.09 -11 -3 0 17.33 1.31 11 3 0 18.55 1.12 -11 3 0 18.27 1.26 -12 -3 0 2.39 0.76 -12 3 0 1.89 0.69 12 3 0 3.05 0.61 -13 -3 0 15.65 1.50 -13 3 0 13.36 1.41 -14 -3 0 -0.73 0.91 -14 3 0 -1.13 0.87 -15 -3 0 2.75 1.14 -15 3 0 2.77 1.33 -16 -3 0 -0.52 1.25 -16 3 0 -1.03 1.17 -17 -3 0 10.29 1.78 -17 3 0 7.13 1.56 -18 -3 0 4.49 1.79 -18 3 0 5.03 1.56 -19 -3 0 1.64 1.99 -19 3 0 -1.88 1.75 0 -4 0 58.62 2.43 0 -4 0 59.56 2.50 0 4 0 60.82 2.50 0 4 0 58.26 2.44 1 -4 0 65.20 2.78 -1 -4 0 65.40 2.72 1 -4 0 71.02 2.73 -1 -4 0 64.53 2.78 -1 4 0 64.14 2.73 -1 4 0 67.41 2.78 -1 4 0 66.75 2.79 1 4 0 68.84 2.73 1 4 0 68.61 2.79 2 -4 0 30.00 1.37 -2 -4 0 29.64 1.31 -2 -4 0 29.33 1.36 2 -4 0 28.08 1.29 2 4 0 29.52 1.28 -2 4 0 28.40 1.35 -2 4 0 30.51 1.38 2 4 0 28.55 1.34 -2 4 0 31.75 1.34 -3 -4 0 59.19 2.49 3 -4 0 60.29 2.49 -3 -4 0 60.31 2.43 3 -4 0 59.35 2.44 3 4 0 59.09 2.40 -3 4 0 57.60 2.46 -3 4 0 57.57 2.47 -3 4 0 57.70 2.48 3 4 0 57.24 2.46 -4 -4 0 44.74 1.86 4 -4 0 43.05 1.90 -4 -4 0 44.40 1.92 4 -4 0 42.99 1.87 -4 4 0 44.74 1.92 -4 4 0 41.55 1.89 4 4 0 41.55 1.86 -4 4 0 42.99 1.91 4 4 0 44.38 1.82 -5 -4 0 181.84 7.42 5 -4 0 189.92 7.46 5 -4 0 192.19 7.47 -5 -4 0 186.16 7.47 -5 4 0 189.04 7.46 5 4 0 191.85 7.38 -5 4 0 184.61 7.46 -5 4 0 198.72 7.49 -5 4 0 184.46 7.48 5 4 0 177.40 7.41 6 -4 0 204.28 7.78 -6 -4 0 200.91 7.78 -6 -4 0 195.10 7.75 6 -4 0 172.88 7.74 6 4 0 193.88 7.69 6 4 0 198.62 7.72 -6 4 0 213.99 7.81 -6 4 0 183.69 7.78 -6 4 0 193.66 7.77 -7 -4 0 34.31 1.62 7 -4 0 37.18 1.67 7 -4 0 32.26 1.63 -7 -4 0 32.61 1.62 7 4 0 32.89 1.55 -7 4 0 34.51 1.68 -7 4 0 37.29 1.67 -7 4 0 32.46 1.64 7 4 0 34.45 1.56 -8 -4 0 0.95 0.40 8 -4 0 1.50 0.40 8 -4 0 0.74 0.44 -8 -4 0 0.65 0.59 8 4 0 1.40 0.37 -8 4 0 0.37 0.49 -8 4 0 1.61 0.44 8 4 0 0.82 0.40 -8 4 0 0.89 0.41 -9 -4 0 6.24 0.83 9 -4 0 5.90 0.90 9 -4 0 5.52 0.78 -9 -4 0 7.91 0.82 -9 4 0 5.47 0.80 -9 4 0 7.13 0.76 -9 4 0 5.59 0.73 10 -4 0 36.65 1.91 -10 -4 0 36.13 1.91 -10 -4 0 37.33 1.97 -10 4 0 36.64 1.74 -10 4 0 37.46 1.91 10 4 0 36.56 1.76 -11 -4 0 11.96 1.25 -11 -4 0 13.28 1.17 -11 4 0 12.16 1.16 -12 -4 0 40.03 2.22 -12 -4 0 40.35 2.13 -12 4 0 41.38 2.17 -13 -4 0 29.74 2.02 -13 4 0 32.63 1.93 -14 -4 0 12.69 1.71 -14 4 0 13.81 1.62 -15 -4 0 1.93 1.22 -15 4 0 4.18 1.10 -16 -4 0 11.33 2.09 -16 4 0 12.14 1.88 -17 -4 0 7.96 1.78 -17 4 0 7.20 1.55 -18 -4 0 4.81 1.94 -18 4 0 9.14 1.83 -19 -4 0 0.70 2.00 -19 4 0 2.47 1.74 0 -5 0 -0.02 0.23 0 -5 0 0.41 0.26 0 5 0 0.78 0.30 0 5 0 0.31 0.29 1 -5 0 45.97 2.10 -1 -5 0 49.32 2.05 -1 -5 0 46.46 2.10 1 -5 0 50.65 2.04 -1 5 0 49.79 2.11 1 5 0 49.36 2.12 1 5 0 50.97 2.05 -1 5 0 42.48 2.13 -1 5 0 46.55 2.11 -2 -5 0 1.37 0.30 -2 -5 0 0.87 0.29 2 -5 0 0.97 0.32 2 -5 0 1.11 0.25 -2 5 0 0.88 0.29 -2 5 0 0.98 0.30 2 5 0 0.92 0.29 -2 5 0 0.99 0.29 2 5 0 0.74 0.29 3 -5 0 2.63 0.46 3 -5 0 2.48 0.40 -3 -5 0 3.60 0.49 -3 -5 0 2.53 0.49 -3 5 0 3.46 0.54 -3 5 0 3.10 0.51 3 5 0 3.55 0.41 -3 5 0 2.57 0.52 3 5 0 3.66 0.52 -4 -5 0 4.48 0.54 4 -5 0 3.97 0.46 -4 -5 0 3.83 0.55 4 5 0 3.52 0.44 -4 5 0 2.51 0.44 4 5 0 4.01 0.53 -4 5 0 4.03 0.60 -4 5 0 3.04 0.57 -5 -5 0 0.86 0.36 5 -5 0 1.36 0.34 -5 -5 0 1.04 0.35 5 -5 0 0.77 0.36 5 5 0 0.95 0.32 -5 5 0 0.54 0.36 -5 5 0 0.41 0.34 -5 5 0 1.17 0.43 5 5 0 0.80 0.28 6 -5 0 13.25 0.91 -6 -5 0 13.45 0.91 6 -5 0 10.90 0.79 -6 -5 0 12.82 0.84 -6 5 0 13.57 0.93 6 5 0 11.49 0.83 6 5 0 10.41 0.74 -6 5 0 12.13 0.93 -6 5 0 11.30 0.82 7 -5 0 22.99 1.29 -7 -5 0 22.90 1.85 7 -5 0 25.94 1.40 -7 -5 0 25.02 1.31 -7 5 0 22.92 1.34 -7 5 0 25.05 1.39 -7 5 0 26.05 1.42 7 5 0 25.67 1.29 7 5 0 24.59 1.23 8 -5 0 83.09 3.43 -8 -5 0 74.33 3.38 8 -5 0 75.93 3.38 -8 -5 0 72.87 3.39 -8 5 0 75.90 3.39 -8 5 0 81.41 3.41 8 5 0 77.02 3.29 -8 5 0 85.52 3.41 8 5 0 78.67 3.40 -9 -5 0 18.51 1.29 9 -5 0 18.84 1.21 9 -5 0 21.56 1.40 -9 -5 0 19.21 1.27 -9 5 0 20.12 1.39 -9 5 0 17.49 1.22 -9 5 0 20.09 1.28 10 -5 0 1.20 0.69 -10 -5 0 0.36 0.59 -10 -5 0 0.76 0.66 10 -5 0 0.62 0.52 -10 5 0 0.68 0.55 -10 5 0 0.72 0.67 -10 5 0 0.54 0.72 -11 -5 0 2.04 0.74 -11 -5 0 2.06 0.81 -11 5 0 1.10 0.72 -11 5 0 1.98 0.68 -11 5 0 1.82 0.80 -12 -5 0 6.44 0.97 -12 -5 0 8.58 1.36 -12 5 0 5.54 0.88 -13 -5 0 15.36 1.69 -13 -5 0 14.66 1.60 -13 5 0 17.06 1.49 -14 -5 0 4.07 1.21 -14 -5 0 4.23 1.05 -15 -5 0 4.11 1.33 -16 -5 0 2.92 1.53 -16 5 0 2.34 1.24 -17 -5 0 2.35 1.78 -17 5 0 2.82 1.44 -18 -5 0 0.15 1.90 -18 5 0 0.74 1.58 0 -6 0 11.05 0.77 0 6 0 14.63 0.92 -1 -6 0 225.46 9.28 1 -6 0 229.62 9.28 -1 -6 0 232.91 9.19 1 -6 0 244.03 9.20 -1 6 0 234.78 9.29 -1 6 0 227.50 9.21 -1 6 0 229.06 9.30 1 6 0 239.33 9.20 1 6 0 235.49 9.29 -2 -6 0 8.12 0.74 2 -6 0 9.61 0.65 -2 -6 0 8.50 0.71 2 -6 0 10.00 0.78 2 6 0 9.17 0.69 -2 6 0 10.52 0.78 -2 6 0 8.39 0.75 2 6 0 8.79 0.76 -3 -6 0 1.05 0.39 3 -6 0 1.31 0.39 3 -6 0 1.39 0.30 -3 -6 0 1.32 0.38 3 6 0 1.11 0.32 -3 6 0 1.23 0.37 -3 6 0 1.04 0.37 3 6 0 1.65 0.37 -3 6 0 1.26 0.44 -4 -6 0 101.55 3.90 -4 -6 0 85.57 4.11 4 -6 0 82.81 4.19 -4 6 0 98.02 3.98 -4 6 0 98.12 3.99 4 6 0 91.73 3.92 -4 6 0 96.05 3.96 4 6 0 99.33 3.82 -5 -6 0 35.83 1.84 5 -6 0 34.60 1.74 -5 -6 0 39.35 1.79 5 6 0 38.53 1.69 -5 6 0 38.49 1.86 -5 6 0 40.73 1.88 -6 -6 0 296.78 10.62 -6 -6 0 257.77 10.65 6 -6 0 252.34 10.59 -6 6 0 260.17 10.63 -6 6 0 254.71 10.59 6 6 0 275.69 10.50 -6 6 0 274.09 10.87 -7 -6 0 12.57 1.03 7 -6 0 12.57 0.89 -7 -6 0 11.65 0.99 -7 6 0 12.31 1.07 7 6 0 11.56 0.87 -7 6 0 12.66 0.94 -8 -6 0 44.62 2.15 8 -6 0 43.37 2.11 -8 -6 0 44.62 2.19 -8 6 0 44.30 2.13 -8 6 0 41.92 2.18 -8 6 0 46.58 2.22 9 -6 0 45.57 2.21 -9 -6 0 43.27 2.22 -9 -6 0 45.52 2.27 -9 6 0 45.78 2.29 -9 6 0 45.20 2.21 -10 -6 0 21.29 1.49 10 -6 0 20.69 1.38 -10 -6 0 19.90 1.49 -10 6 0 18.61 1.48 -10 6 0 21.26 1.42 -11 -6 0 10.67 1.36 11 -6 0 13.04 1.28 -11 -6 0 14.82 1.43 -11 6 0 11.47 1.22 -11 6 0 10.94 1.31 -12 -6 0 8.71 1.45 -12 -6 0 6.42 0.98 -12 6 0 6.01 1.17 -12 6 0 7.23 1.22 -13 -6 0 34.74 2.26 -13 -6 0 38.34 2.39 -13 6 0 35.52 2.15 -14 -6 0 -0.12 1.03 -14 -6 0 1.50 1.20 -14 6 0 0.87 0.96 -15 -6 0 -1.48 1.19 -15 -6 0 -1.14 1.38 -15 6 0 0.31 1.08 -16 -6 0 13.47 1.86 -16 6 0 9.73 1.58 -17 -6 0 8.13 1.93 -17 6 0 4.53 1.58 -18 -6 0 4.97 2.10 -18 6 0 2.67 1.69 0 -7 0 -0.15 0.34 0 -7 0 0.38 0.34 0 7 0 0.34 0.42 1 -7 0 6.96 0.61 1 -7 0 5.50 0.73 -1 -7 0 5.75 0.76 -1 7 0 6.22 0.75 -1 7 0 6.48 0.76 1 7 0 6.06 0.71 2 -7 0 9.56 0.69 -2 -7 0 8.38 0.80 2 -7 0 7.34 0.87 -2 -7 0 9.34 0.76 -2 7 0 6.82 0.82 -2 7 0 6.84 0.84 2 7 0 9.27 0.78 3 -7 0 29.23 1.56 3 -7 0 29.38 1.63 -3 -7 0 28.09 1.56 -3 -7 0 31.05 1.49 3 7 0 30.77 1.45 -3 7 0 30.80 1.56 -3 7 0 29.55 1.62 4 -7 0 3.56 0.57 -4 -7 0 4.16 0.70 4 -7 0 3.13 0.59 -4 -7 0 4.37 0.58 -4 7 0 3.20 0.56 4 7 0 3.12 0.45 -5 -7 0 2.48 0.55 -5 -7 0 2.12 0.51 5 -7 0 2.50 0.45 -5 7 0 2.16 0.52 5 7 0 1.87 0.43 -6 -7 0 45.75 2.10 -6 -7 0 42.26 2.14 6 -7 0 43.82 2.03 -6 7 0 43.19 2.17 6 7 0 42.28 1.93 -7 -7 0 2.61 0.75 7 -7 0 1.45 0.45 -7 -7 0 1.16 0.56 -7 7 0 0.59 0.58 -7 7 0 1.10 0.47 7 7 0 0.81 0.43 -8 -7 0 3.63 0.72 -8 -7 0 3.19 0.68 8 -7 0 4.63 0.81 -8 7 0 2.86 0.71 -8 7 0 3.98 0.66 -9 -7 0 2.20 0.74 9 -7 0 2.84 0.64 -9 -7 0 2.40 0.75 -9 7 0 2.44 0.75 -9 7 0 3.79 0.68 -10 -7 0 33.08 1.97 10 -7 0 32.14 1.84 -10 -7 0 31.28 1.98 -10 7 0 32.90 1.89 -10 7 0 33.52 2.00 -11 -7 0 4.89 0.99 11 -7 0 4.67 0.86 -11 -7 0 4.06 0.92 -11 7 0 4.88 0.90 -11 7 0 6.12 0.99 -12 -7 0 7.91 1.50 12 -7 0 11.03 1.40 -12 -7 0 10.43 1.65 -12 7 0 7.09 1.09 -12 7 0 10.39 1.34 -13 -7 0 8.92 1.34 -13 -7 0 8.74 1.69 -13 7 0 7.40 1.07 -14 -7 0 2.07 1.15 -14 -7 0 2.78 1.35 -14 7 0 4.42 1.04 -15 -7 0 0.69 1.27 -15 -7 0 1.87 1.49 -15 7 0 1.94 1.11 -16 -7 0 6.09 1.71 -16 7 0 2.64 1.40 -17 -7 0 5.62 1.93 -17 7 0 5.88 1.62 -18 -7 0 0.79 2.19 -18 7 0 4.05 1.78 0 -8 0 186.73 6.91 0 -8 0 162.22 7.02 0 8 0 174.14 6.93 0 8 0 163.78 7.04 -1 -8 0 37.19 1.92 1 -8 0 39.41 1.79 1 -8 0 37.07 1.94 -1 -8 0 38.83 1.79 -1 8 0 32.93 1.87 1 8 0 39.39 1.84 -1 8 0 38.14 1.95 -2 -8 0 62.96 2.92 2 -8 0 62.05 2.76 2 -8 0 61.03 2.92 -2 -8 0 66.30 2.78 2 8 0 67.66 2.80 -2 8 0 62.61 2.95 -2 8 0 64.85 2.92 -3 -8 0 0.37 0.50 3 -8 0 0.22 0.46 3 -8 0 0.66 0.39 -3 -8 0 0.82 0.46 -3 8 0 0.63 0.46 3 8 0 1.01 0.47 -4 -8 0 13.50 1.04 4 -8 0 11.73 0.88 -4 -8 0 12.08 1.08 4 -8 0 11.92 1.11 4 8 0 12.06 0.89 -4 8 0 10.79 1.03 -5 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6.63 1.84 -7 2 20 9.10 1.87 6 -2 -20 12.35 1.86 -6 -2 20 14.74 2.67 -6 2 20 9.86 1.82 5 -2 -20 16.51 1.97 -5 -2 20 18.08 2.81 5 2 -20 16.09 1.90 -5 2 20 19.37 2.61 4 -2 -20 26.91 2.30 -4 -2 20 29.89 2.90 4 2 -20 28.44 2.23 -4 2 20 29.07 2.75 3 -2 -20 5.67 1.31 -3 2 20 10.22 1.79 3 2 -20 5.19 1.28 2 -2 -20 0.84 1.26 -2 -2 20 0.10 1.55 2 2 -20 -2.00 1.11 -1 -2 20 4.91 1.73 1 -2 -20 6.98 1.43 1 2 -20 4.75 1.34 0 -2 20 14.77 1.91 0 -2 -20 11.96 2.04 0 2 -20 11.66 1.89 1 -2 20 7.81 1.58 -1 -2 -20 7.55 1.53 -1 2 -20 6.78 1.44 2 -2 20 8.92 1.52 -2 -2 -20 7.75 1.60 -2 2 -20 7.07 1.49 -3 -2 -20 -0.92 1.40 3 -2 20 1.39 1.46 -3 2 -20 -0.77 1.36 4 -2 20 2.02 2.16 -4 -2 -20 3.49 1.56 -4 2 -20 -0.42 1.42 -13 -3 20 -0.67 2.34 -13 3 20 2.33 2.37 -12 -3 20 -2.55 2.26 -12 3 20 -1.17 2.16 -11 -3 20 2.87 2.10 -11 3 20 2.17 2.06 -10 -3 20 0.18 2.08 -10 3 20 1.88 1.97 9 -3 -20 0.32 1.58 -9 -3 20 5.11 2.03 -9 3 20 -0.18 2.30 9 3 -20 -1.34 1.26 8 -3 -20 -1.76 1.24 -8 -3 20 0.66 2.04 -8 3 20 -0.36 1.76 -7 -3 20 6.97 2.01 -7 3 20 8.60 1.81 7 3 -20 4.53 1.34 -6 -3 20 2.64 1.81 6 -3 -20 0.25 1.30 6 3 -20 0.81 1.22 -6 3 20 0.40 1.59 5 -3 -20 0.95 1.29 -5 -3 20 1.77 1.84 -5 3 20 1.83 1.73 -4 -3 20 7.21 1.88 4 -3 -20 8.43 1.48 3 -3 -20 12.35 1.97 -3 -3 20 8.12 1.78 2 -3 -20 4.11 1.30 -2 -3 20 2.66 1.68 2 3 -20 2.73 1.27 1 -3 -20 3.54 1.30 -1 -3 20 4.30 1.77 1 3 -20 4.20 1.37 0 -3 20 0.22 1.56 0 -3 -20 0.55 1.30 0 3 -20 1.25 1.29 1 -3 20 0.25 1.44 -1 -3 -20 2.73 1.40 -1 3 -20 1.25 1.37 2 -3 20 0.18 1.34 -2 3 -20 -1.09 1.37 -3 -3 -20 5.88 1.60 3 -3 20 -1.01 1.47 -4 -3 -20 6.28 1.72 -12 -4 20 9.00 2.47 -12 4 20 9.56 2.46 -11 -4 20 9.70 2.44 -11 4 20 14.96 2.46 -10 -4 20 37.56 3.72 -10 4 20 38.26 3.40 -9 -4 20 17.04 2.58 9 4 -20 17.85 3.01 -9 4 20 19.06 3.34 8 -4 -20 9.21 1.62 -8 -4 20 8.12 2.10 8 4 -20 11.15 2.03 -8 4 20 10.15 1.99 7 -4 -20 5.14 1.43 -7 -4 20 8.82 2.01 -7 4 20 9.09 3.00 7 4 -20 7.13 1.39 -6 -4 20 3.36 1.95 6 4 -20 3.33 1.29 -5 -4 20 7.36 2.00 5 -4 -20 4.63 1.50 -4 -4 20 10.12 1.97 4 -4 -20 7.82 1.58 4 4 -20 13.49 1.90 3 -4 -20 6.87 1.56 -3 -4 20 9.08 1.93 3 4 -20 10.81 1.88 2 -4 -20 0.91 1.43 -2 -4 20 2.85 1.68 2 4 -20 5.67 1.36 -1 -4 20 7.40 1.91 1 -4 -20 8.14 1.63 1 4 -20 12.16 2.03 0 -4 -20 8.58 1.69 0 -4 20 8.39 1.82 0 4 -20 10.75 2.02 1 -4 20 7.79 1.71 -1 -4 -20 9.23 1.77 -1 4 -20 8.31 1.52 2 -4 20 5.17 1.56 -2 -4 -20 7.68 1.74 -2 4 -20 6.04 1.56 3 -4 20 4.41 1.56 -3 -4 -20 2.88 1.82 -3 4 -20 3.72 1.54 -11 -5 20 4.19 2.34 -11 5 20 0.29 2.23 -10 -5 20 0.73 2.20 -10 5 20 5.04 2.94 -9 -5 20 2.77 2.22 9 5 -20 4.79 1.41 8 -5 -20 0.90 1.50 -8 -5 20 2.04 2.08 8 5 -20 -0.56 1.32 7 -5 -20 1.27 1.37 -7 -5 20 0.97 2.08 7 5 -20 0.02 1.29 -6 -5 20 3.93 2.14 6 -5 -20 2.83 1.34 6 5 -20 1.60 1.36 5 -5 -20 0.81 1.34 -5 -5 20 2.47 1.82 5 5 -20 -1.20 1.28 4 -5 -20 -0.47 1.38 -4 -5 20 1.29 1.79 4 5 -20 -0.61 1.25 -3 -5 20 1.97 1.73 3 -5 -20 1.35 1.39 3 5 -20 -0.01 1.29 -2 -5 20 3.66 1.74 2 -5 -20 0.90 1.45 2 5 -20 -0.30 1.31 1 -5 -20 0.23 1.51 -1 -5 20 3.94 1.91 1 5 -20 7.59 1.44 0 -5 20 0.74 1.72 0 5 -20 4.14 1.39 1 -5 20 -1.81 1.83 -1 -5 -20 -1.02 1.59 -1 5 -20 2.20 1.39 2 -5 20 0.29 1.49 -2 -5 -20 0.06 1.61 -2 5 -20 2.58 1.48 -11 -6 20 30.18 3.92 -10 -6 20 9.19 2.62 -9 -6 20 2.88 2.28 9 6 -20 1.55 1.54 8 -6 -20 0.90 1.53 -8 -6 20 8.50 2.24 8 6 -20 3.27 1.49 -7 -6 20 2.84 2.15 7 -6 -20 2.33 1.50 7 6 -20 2.17 1.45 -6 -6 20 10.45 2.41 6 -6 -20 7.54 1.60 6 6 -20 8.15 1.71 -5 -6 20 22.95 3.29 5 -6 -20 26.62 2.59 5 6 -20 24.90 2.46 4 -6 -20 18.57 2.38 -4 -6 20 14.63 2.29 4 6 -20 17.76 2.21 3 -6 -20 4.00 1.46 -3 -6 20 -0.20 1.83 3 6 -20 2.51 1.43 -2 -6 20 6.49 1.86 2 -6 -20 2.92 1.53 2 6 -20 1.37 1.41 -1 -6 20 -0.43 1.84 1 -6 -20 0.23 1.54 1 6 -20 0.59 1.40 0 -6 -20 0.12 1.59 0 -6 20 -0.03 1.69 0 6 -20 2.04 1.47 -1 -6 -20 10.56 1.85 1 -6 20 7.99 1.87 -1 6 -20 15.08 2.19 -9 -7 20 6.97 2.44 9 7 -20 4.31 1.68 8 -7 -20 0.23 1.70 -8 -7 20 1.24 2.37 8 7 -20 3.14 1.55 7 -7 -20 6.71 1.76 -7 -7 20 5.96 2.41 7 7 -20 11.94 2.24 -6 -7 20 0.25 2.05 6 -7 -20 -1.40 1.59 6 7 -20 1.70 1.48 -5 -7 20 11.75 2.34 5 -7 -20 13.94 2.57 5 7 -20 14.91 2.26 -4 -7 20 7.26 2.11 4 7 -20 5.78 1.55 3 -7 -20 2.23 1.61 -3 -7 20 1.91 1.98 3 7 -20 -0.71 1.43 -2 -7 20 3.73 2.11 2 -7 -20 0.32 1.59 2 7 -20 0.80 1.42 1 -7 -20 -0.15 1.64 -1 -7 20 2.21 1.89 1 7 -20 0.88 1.48 0 -7 20 -1.09 1.76 0 -7 -20 1.22 1.76 0 7 -20 1.84 1.54 7 -8 -20 3.29 1.92 -7 -8 20 3.00 2.35 7 8 -20 5.94 1.68 6 -8 -20 5.00 1.78 -6 -8 20 1.70 2.27 6 8 -20 5.41 1.63 5 -8 -20 5.47 1.80 -5 -8 20 8.47 2.15 5 8 -20 6.66 1.64 4 -8 -20 4.46 1.81 -4 -8 20 5.02 2.18 -3 -8 20 12.99 2.39 3 -8 -20 9.64 2.01 3 8 -20 16.18 2.40 -2 -8 20 -1.97 2.08 2 -8 -20 -0.10 1.77 2 8 -20 -0.50 1.51 -12 0 21 2.62 2.41 -11 0 21 0.71 2.30 -10 0 21 1.48 2.07 -9 0 21 2.12 2.07 8 0 -21 -2.23 1.37 -8 0 21 0.60 1.99 -7 0 21 0.57 1.86 7 0 -21 -1.14 1.42 6 0 -21 -0.52 1.36 -6 0 21 0.63 1.95 5 0 -21 1.15 1.34 -5 0 21 2.46 1.99 4 0 -21 2.00 1.35 -4 0 21 -1.58 3.23 3 0 -21 -0.42 1.28 -3 0 21 1.20 2.23 2 0 -21 3.01 1.38 -2 0 21 2.93 1.70 -1 0 21 -0.10 2.19 1 0 -21 1.58 1.43 0 0 -21 3.70 1.45 -1 0 -21 2.30 1.53 -2 0 -21 -1.33 1.53 -11 -1 21 -0.62 2.25 -11 1 21 2.49 2.24 -10 -1 21 -3.57 2.46 -10 1 21 0.65 2.19 -9 -1 21 8.40 2.24 -9 1 21 6.40 2.18 8 -1 -21 15.28 2.11 -8 -1 21 13.25 2.37 -8 1 21 13.99 2.28 8 1 -21 15.36 2.13 7 -1 -21 15.71 2.13 -7 -1 21 20.27 3.04 7 1 -21 18.27 2.14 -7 1 21 13.63 2.18 -6 -1 21 12.05 2.20 6 1 -21 13.15 2.04 -6 1 21 13.42 2.80 -5 -1 21 12.84 2.17 5 -1 -21 7.08 1.55 5 1 -21 9.10 1.49 -5 1 21 10.95 2.17 -4 -1 21 3.28 1.88 4 -1 -21 0.78 1.36 4 1 -21 2.97 1.37 -4 1 21 3.73 1.86 -3 -1 21 2.98 1.75 3 -1 -21 2.86 1.43 -3 1 21 4.01 1.96 3 1 -21 4.76 1.36 -2 -1 21 17.00 2.61 2 -1 -21 10.54 1.72 2 1 -21 10.29 1.97 1 -1 -21 -0.27 1.55 -1 -1 21 4.28 1.76 1 1 -21 0.64 1.39 0 -1 -21 0.33 1.54 0 -1 21 -2.59 1.55 0 1 -21 0.44 1.40 -1 -1 -21 -0.94 1.50 -1 1 -21 -2.20 1.42 -2 -1 -21 -1.44 1.55 -2 1 -21 2.17 1.56 -11 -2 21 1.33 2.32 -11 2 21 2.27 2.26 -10 -2 21 5.67 2.26 -10 2 21 0.66 2.22 -9 -2 21 0.61 2.30 9 2 -21 -0.39 1.80 -9 2 21 -2.15 2.08 -8 -2 21 -0.65 1.95 8 -2 -21 0.58 1.46 -8 2 21 6.04 2.01 -7 -2 21 3.27 2.01 7 -2 -21 2.41 1.44 -7 2 21 0.98 3.16 6 -2 -21 2.74 1.35 -6 -2 21 2.10 1.98 6 2 -21 -0.39 1.30 -6 2 21 3.81 1.89 -5 -2 21 2.89 1.94 5 -2 -21 2.30 1.33 5 2 -21 0.86 1.34 -5 2 21 0.47 2.18 4 -2 -21 1.76 1.32 -4 -2 21 -3.06 1.73 4 2 -21 -0.42 1.29 3 -2 -21 0.17 1.32 -3 -2 21 2.59 1.77 2 -2 -21 6.98 1.53 2 2 -21 3.54 1.43 -1 -2 21 -0.78 1.77 1 -2 -21 -0.71 1.45 1 2 -21 0.25 1.35 0 -2 21 -2.15 1.60 0 -2 -21 -0.17 1.48 0 2 -21 1.66 1.41 -1 -2 -21 -1.97 1.45 1 -2 21 1.62 1.58 -1 2 -21 1.85 1.47 2 -2 21 6.12 2.11 -2 -2 -21 7.24 1.68 -2 2 -21 7.47 1.65 -11 -3 21 0.64 2.40 -11 3 21 2.42 2.27 -10 -3 21 8.93 2.35 -10 3 21 0.78 2.25 -9 -3 21 8.10 2.43 9 3 -21 9.46 1.83 -9 3 21 11.39 2.27 8 -3 -21 19.80 2.41 8 3 -21 20.56 2.34 -8 3 21 28.42 3.58 7 -3 -21 17.84 2.43 7 3 -21 21.67 2.26 -6 -3 21 6.34 2.16 6 -3 -21 4.43 1.61 6 3 -21 3.81 1.44 5 -3 -21 0.72 1.46 -5 -3 21 1.29 1.92 -4 -3 21 3.26 1.89 4 -3 -21 4.49 1.48 4 3 -21 1.09 1.34 -3 -3 21 10.54 2.01 3 3 -21 10.60 1.59 -2 -3 21 34.22 3.14 2 -3 -21 28.64 2.68 -1 -3 21 23.70 3.14 1 -3 -21 35.44 2.75 1 3 -21 28.85 2.55 0 -3 -21 13.71 2.31 0 -3 21 6.48 1.90 0 3 -21 9.33 1.67 1 -3 21 0.11 1.56 -1 3 -21 -2.50 1.41 -10 -4 21 1.27 2.36 -9 -4 21 -0.61 2.23 9 4 -21 -0.03 1.97 8 -4 -21 1.01 1.52 -8 -4 21 0.19 2.10 8 4 -21 0.30 1.50 7 -4 -21 0.19 1.49 -7 -4 21 0.64 2.13 6 -4 -21 2.32 1.50 -6 -4 21 7.08 2.25 6 4 -21 4.91 1.58 -5 -4 21 1.53 2.26 5 -4 -21 -1.98 1.71 5 4 -21 0.43 1.48 -4 -4 21 10.25 2.13 4 -4 -21 4.96 1.63 4 4 -21 4.47 1.57 3 -4 -21 -1.18 1.60 -3 -4 21 -2.68 1.86 3 4 -21 0.28 1.52 2 -4 -21 -1.39 1.60 -2 -4 21 3.15 1.88 2 4 -21 -0.87 1.50 -1 -4 21 0.09 1.85 1 -4 -21 -1.43 1.66 1 4 -21 0.25 1.53 0 -4 -21 -1.13 1.71 0 -4 21 -2.12 1.71 0 4 -21 -0.44 1.54 -1 -4 -21 -0.41 1.79 -1 4 -21 1.68 1.57 -9 -5 21 10.82 2.53 9 5 -21 9.76 2.28 8 -5 -21 8.16 1.76 -8 -5 21 10.79 2.49 8 5 -21 8.82 1.67 -7 -5 21 13.16 2.53 7 -5 -21 12.40 1.81 6 -5 -21 14.20 2.44 -6 -5 21 13.05 2.44 6 5 -21 19.35 2.33 5 -5 -21 0.53 1.50 -5 -5 21 0.14 2.02 -4 -5 21 4.13 2.00 4 -5 -21 5.11 1.61 4 5 -21 6.98 1.54 3 -5 -21 41.94 3.16 -3 -5 21 44.87 3.73 3 5 -21 45.47 3.03 -2 -5 21 24.64 3.30 2 5 -21 25.83 2.51 -1 -5 21 15.98 2.24 1 -5 -21 9.85 1.88 0 -5 -21 9.71 2.00 0 -5 21 11.43 2.03 -8 -6 21 0.56 2.40 -7 -6 21 2.76 2.47 7 -6 -21 3.79 1.66 -6 -6 21 4.73 2.20 6 -6 -21 3.58 1.62 6 6 -21 -0.02 1.55 5 -6 -21 1.37 1.59 -5 -6 21 -0.35 2.14 5 6 -21 1.05 1.54 4 -6 -21 2.95 1.66 -4 -6 21 0.79 2.05 4 6 -21 -2.04 1.55 3 -6 -21 3.05 1.73 -3 -6 21 1.50 2.03 3 6 -21 -1.74 1.54 -2 -6 21 -0.81 2.03 2 -6 -21 1.87 1.68 2 6 -21 -0.16 1.51 -9 0 22 2.13 2.39 8 0 -22 13.00 2.36 -8 0 22 13.29 2.47 -7 0 22 7.83 2.27 7 0 -22 3.52 1.65 -6 0 22 5.37 2.33 6 0 -22 3.52 1.72 5 0 -22 11.41 1.85 -5 0 22 9.22 2.30 -4 0 22 50.16 3.82 4 0 -22 45.80 3.19 3 0 -22 14.01 2.34 2 0 -22 16.66 2.42 1 0 -22 2.33 1.59 -9 -1 22 5.31 2.54 -9 1 22 9.28 2.56 8 -1 -22 3.23 1.61 -8 -1 22 0.92 2.22 8 1 -22 -0.07 1.66 -8 1 22 1.11 2.20 7 -1 -22 3.96 1.54 -7 -1 22 5.11 2.26 7 1 -22 4.74 1.64 -7 1 22 3.81 2.26 6 -1 -22 -1.26 1.49 -6 -1 22 3.07 2.32 -6 1 22 5.51 2.27 6 1 -22 2.39 1.55 -5 -1 22 -0.01 2.06 5 -1 -22 0.05 1.55 5 1 -22 0.72 1.55 -4 -1 22 3.77 1.99 4 -1 -22 -0.24 1.55 4 1 -22 0.22 1.52 3 -1 -22 0.10 1.56 -3 -1 22 0.45 2.01 3 1 -22 1.10 1.50 -2 -1 22 -0.21 2.07 2 -1 -22 -0.57 1.62 2 1 -22 1.87 1.54 1 1 -22 0.97 1.51 8 -2 -22 4.57 1.93 -8 -2 22 9.07 2.36 -8 2 22 5.85 2.54 8 2 -22 6.27 1.70 -7 -2 22 6.57 2.48 7 -2 -22 5.67 1.73 7 2 -22 3.74 1.60 -6 -2 22 14.91 2.58 6 2 -22 10.25 1.72 -5 -2 22 12.73 2.42 5 -2 -22 19.62 2.43 5 2 -22 17.51 2.31 4 -2 -22 6.88 1.61 -4 -2 22 7.63 2.15 4 2 -22 5.33 1.55 3 -2 -22 6.23 1.63 -3 -2 22 5.12 2.11 3 2 -22 4.43 1.54 2 -2 -22 6.44 1.70 -2 -2 22 5.12 2.17 2 2 -22 5.50 1.62 1 -2 -22 0.60 1.55 -8 -3 22 3.48 2.41 8 -3 -22 -4.49 2.40 -7 -3 22 2.61 2.28 7 -3 -22 -2.72 1.63 7 3 -22 0.86 1.56 6 -3 -22 -2.94 1.60 -6 -3 22 2.15 2.18 6 3 -22 -2.30 1.52 5 -3 -22 -0.05 1.66 -5 -3 22 -2.79 2.15 -4 -3 22 2.98 2.12 4 -3 -22 0.36 1.64 4 3 -22 -1.66 1.51 3 -3 -22 10.01 1.95 -3 -3 22 11.56 2.26 2 -3 -22 8.26 1.81 -2 -3 22 4.61 2.24 2 3 -22 1.00 1.64 -6 -4 22 8.66 2.46 6 -4 -22 6.25 1.74 5 -4 -22 8.86 1.83 -5 -4 22 8.71 2.44 5 4 -22 13.85 2.40 -4 -4 22 14.66 2.44 4 -4 -22 9.09 1.90 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 95866 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 0.08492(4) 0.50790(3) 0.24482(3) 0.01238(18) Uani 1 1 d . . N2 N 0.1046(4) 0.5210(4) 0.3751(3) 0.0133(11) Uani 1 1 d . . C8 C 0.1522(4) 0.4485(5) 0.4194(4) 0.0144(13) Uani 1 1 d . . C7 C 0.1677(5) 0.4417(5) 0.5055(4) 0.0186(14) Uani 1 1 d . . H7 H 0.2012 0.3887 0.5345 0.022 Uiso 1 1 calc R U C6 C 0.1339(5) 0.5122(5) 0.5452(4) 0.0179(14) Uani 1 1 d . . H6 H 0.1441 0.5097 0.6029 0.022 Uiso 1 1 calc R U C4 C 0.0832(4) 0.5897(5) 0.5005(4) 0.0153(14) Uani 1 1 d . . C5 C 0.0678(4) 0.5905(5) 0.4151(4) 0.0136(13) Uani 1 1 d . . N1 N 0.0163(4) 0.6592(4) 0.3676(3) 0.0167(12) Uani 1 1 d . . C1 C -0.0180(5) 0.7286(5) 0.4046(4) 0.0184(14) Uani 1 1 d . . H1 H -0.0543 0.7771 0.3716 0.022 Uiso 1 1 calc R U C2 C -0.0049(5) 0.7359(5) 0.4888(4) 0.0181(14) Uani 1 1 d . . H2 H -0.0304 0.7886 0.5120 0.022 Uiso 1 1 calc R U C3 C 0.0455(4) 0.6656(5) 0.5374(4) 0.0178(14) Uani 1 1 d . . H3 H 0.0549 0.6680 0.5950 0.021 Uiso 1 1 calc R U C9 C 0.1899(4) 0.3780(5) 0.3736(4) 0.0161(14) Uani 1 1 d . . N3 N 0.1732(4) 0.3954(4) 0.2932(3) 0.0165(12) Uani 1 1 d . . N4 N 0.2145(4) 0.3236(4) 0.2624(3) 0.0160(12) Uani 1 1 d . . C11 C 0.2579(4) 0.2602(5) 0.3213(4) 0.0170(14) Uani 1 1 d . . C10 C 0.2421(5) 0.2933(5) 0.3944(4) 0.0182(14) Uani 1 1 d . . H10 H 0.2623 0.2646 0.4470 0.022 Uiso 1 1 calc R U C12 C 0.3106(5) 0.1741(5) 0.3037(4) 0.0209(15) Uani 1 1 d . . C14 C 0.3482(5) 0.1185(5) 0.3826(4) 0.0246(16) Uani 1 1 d . . H14A H 0.3916 0.1598 0.4208 0.037 Uiso 1 1 calc R U H14B H 0.3787 0.0591 0.3711 0.037 Uiso 1 1 calc R U H14C H 0.2984 0.1007 0.4068 0.037 Uiso 1 1 calc R U C13 C 0.2495(5) 0.1082(5) 0.2403(4) 0.0242(16) Uani 1 1 d . . H13A H 0.1984 0.0858 0.2609 0.036 Uiso 1 1 calc R U H13B H 0.2842 0.0517 0.2296 0.036 Uiso 1 1 calc R U H13C H 0.2266 0.1449 0.1895 0.036 Uiso 1 1 calc R U C15 C 0.3899(5) 0.2103(6) 0.2705(5) 0.0278(17) Uani 1 1 d . . H15A H 0.3661 0.2432 0.2180 0.042 Uiso 1 1 calc R U H15B H 0.4272 0.1545 0.2629 0.042 Uiso 1 1 calc R U H15C H 0.4269 0.2562 0.3094 0.042 Uiso 1 1 calc R U C18 C 0.0071(5) 0.6354(5) 0.1866(4) 0.0187(15) Uani 1 1 d . . H18 H -0.0429 0.6686 0.1982 0.022 Uiso 1 1 calc R U C17 C -0.0085(4) 0.5571(5) 0.1289(4) 0.0148(13) Uani 1 1 d . . C16 C 0.0664(5) 0.5104(5) 0.1125(4) 0.0191(15) Uani 1 1 d . . H16 H 0.0575 0.4577 0.0747 0.023 Uiso 1 1 calc R U C21 C 0.1567(5) 0.5412(5) 0.1522(4) 0.0159(14) Uani 1 1 d . . H21 H 0.2067 0.5080 0.1405 0.019 Uiso 1 1 calc R U C20 C 0.1730(5) 0.6190(5) 0.2078(4) 0.0190(15) Uani 1 1 d . . C19 C 0.0954(5) 0.6633(5) 0.2260(4) 0.0173(14) Uani 1 1 d . . H19 H 0.1043 0.7134 0.2660 0.021 Uiso 1 1 calc R U C22 C 0.2675(5) 0.6548(6) 0.2495(5) 0.0275(17) Uani 1 1 d . . H22 H 0.2695 0.6691 0.3078 0.033 Uiso 1 1 calc R U C24 C 0.3416(6) 0.5794(7) 0.2477(6) 0.044(2) Uani 1 1 d . . H24A H 0.3254 0.5164 0.2676 0.065 Uiso 1 1 calc R U H24B H 0.3995 0.6018 0.2827 0.065 Uiso 1 1 calc R U H24C H 0.3472 0.5720 0.1916 0.065 Uiso 1 1 calc R U C23 C 0.2834(6) 0.7510(7) 0.2083(6) 0.047(2) Uani 1 1 d . . H23A H 0.2805 0.7388 0.1507 0.070 Uiso 1 1 calc R U H23B H 0.3431 0.7772 0.2356 0.070 Uiso 1 1 calc R U H23C H 0.2365 0.7984 0.2124 0.070 Uiso 1 1 calc R U C25 C -0.1027(5) 0.5238(6) 0.0898(4) 0.0244(16) Uani 1 1 d . . H25A H -0.1328 0.5719 0.0491 0.037 Uiso 1 1 calc R U H25B H -0.1366 0.5169 0.1315 0.037 Uiso 1 1 calc R U H25C H -0.1006 0.4606 0.0631 0.037 Uiso 1 1 calc R U Cl1 Cl -0.03249(12) 0.39748(12) 0.25761(10) 0.0208(4) Uani 1 1 d . . Cl1S Cl 0.50886(15) 0.41746(16) 0.19175(14) 0.0400(5) Uani 1 1 d . . Cl2S Cl 0.48418(17) 0.24514(16) 0.08666(15) 0.0459(6) Uani 1 1 d . . Cl5S Cl 0.62176(19) 0.3945(2) -0.02341(17) 0.0589(7) Uani 1 1 d . . Cl3S Cl 0.5994(3) 0.4980(4) 0.3804(3) 0.1064(14) Uani 1 1 d . . C1S C 0.4522(6) 0.3687(6) 0.0966(5) 0.037(2) Uani 1 1 d . . H1S1 H 0.4666 0.4083 0.0526 0.044 Uiso 1 1 calc R U H1S2 H 0.3860 0.3721 0.0905 0.044 Uiso 1 1 calc R U Cl6S Cl 0.77810(17) 0.2727(2) 0.04562(18) 0.0582(7) Uani 1 1 d . . C3S C 0.6978(6) 0.3512(8) 0.0670(6) 0.050(2) Uani 1 1 d . . H3S1 H 0.7288 0.4074 0.0989 0.060 Uiso 1 1 calc R U H3S2 H 0.6632 0.3166 0.1006 0.060 Uiso 1 1 calc R U Cl2 Cl 0.22635(11) 0.32297(12) 0.08380(10) 0.0195(4) Uani 1 1 d . . Cl4S Cl 0.6220(3) 0.4517(4) 0.5481(2) 0.1077(14) Uani 1 1 d . . C2S C 0.5869(14) 0.4124(12) 0.4468(9) 0.118(7) Uani 1 1 d . . H2S1 H 0.6224 0.3540 0.4398 0.142 Uiso 1 1 calc R U H2S2 H 0.5223 0.3931 0.4348 0.142 Uiso 1 1 calc R U H4A H 0.211(4) 0.321(5) 0.205(4) 0.011(17) Uiso 1 1 d . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.0178(3) 0.0106(3) 0.0098(3) 0.0010(2) 0.0055(2) 0.0017(2) N2 0.015(3) 0.013(3) 0.012(3) 0.002(2) 0.004(2) 0.002(2) C8 0.015(3) 0.016(3) 0.013(3) 0.000(3) 0.003(3) -0.003(3) C7 0.022(4) 0.016(3) 0.017(3) 0.003(3) 0.003(3) 0.002(3) C6 0.022(4) 0.020(3) 0.012(3) 0.002(3) 0.005(3) 0.002(3) C4 0.014(3) 0.016(3) 0.016(3) 0.000(3) 0.006(3) -0.002(3) C5 0.014(3) 0.014(3) 0.014(3) -0.001(3) 0.004(3) -0.002(3) N1 0.021(3) 0.014(3) 0.015(3) -0.001(2) 0.006(2) 0.001(2) C1 0.018(4) 0.015(3) 0.025(4) 0.001(3) 0.010(3) 0.001(3) C2 0.023(4) 0.017(3) 0.017(3) -0.004(3) 0.011(3) 0.002(3) C3 0.021(4) 0.022(4) 0.012(3) -0.001(3) 0.008(3) -0.003(3) C9 0.018(3) 0.015(3) 0.017(3) 0.003(3) 0.007(3) 0.002(3) N3 0.023(3) 0.015(3) 0.012(3) 0.000(2) 0.007(2) 0.006(2) N4 0.022(3) 0.016(3) 0.012(3) -0.001(2) 0.007(2) 0.004(2) C11 0.016(3) 0.019(3) 0.016(3) 0.001(3) 0.005(3) 0.001(3) C10 0.023(4) 0.016(3) 0.016(3) 0.003(3) 0.007(3) 0.001(3) C12 0.023(4) 0.018(3) 0.024(4) 0.004(3) 0.011(3) 0.008(3) C14 0.029(4) 0.021(4) 0.024(4) 0.000(3) 0.008(3) 0.010(3) C13 0.030(4) 0.020(4) 0.025(4) -0.002(3) 0.011(3) 0.007(3) C15 0.027(4) 0.030(4) 0.028(4) 0.002(3) 0.011(3) 0.009(3) C18 0.026(4) 0.016(3) 0.015(3) 0.007(3) 0.008(3) 0.006(3) C17 0.020(4) 0.014(3) 0.012(3) 0.004(3) 0.006(3) -0.002(3) C16 0.032(4) 0.015(3) 0.013(3) 0.003(3) 0.011(3) 0.002(3) C21 0.021(4) 0.018(3) 0.011(3) 0.005(3) 0.008(3) 0.003(3) C20 0.020(4) 0.022(4) 0.015(3) 0.006(3) 0.006(3) -0.001(3) C19 0.027(4) 0.011(3) 0.015(3) 0.002(3) 0.008(3) -0.001(3) C22 0.024(4) 0.033(4) 0.024(4) 0.002(3) 0.003(3) -0.004(3) C24 0.027(5) 0.059(6) 0.044(5) -0.007(5) 0.008(4) -0.002(4) C23 0.038(5) 0.049(6) 0.047(5) 0.009(5) 0.002(4) -0.024(4) C25 0.028(4) 0.031(4) 0.013(3) 0.005(3) 0.005(3) -0.006(3) Cl1 0.0295(10) 0.0165(8) 0.0173(8) 0.0018(6) 0.0077(7) -0.0062(7) Cl1S 0.0379(12) 0.0373(11) 0.0449(12) 0.0029(10) 0.0107(10) -0.0050(9) Cl2S 0.0562(15) 0.0353(12) 0.0508(14) 0.0035(10) 0.0222(11) 0.0034(10) Cl5S 0.0654(17) 0.0581(16) 0.0602(16) 0.0190(13) 0.0292(13) 0.0263(13) Cl3S 0.099(3) 0.143(4) 0.077(2) 0.019(2) 0.020(2) -0.010(3) C1S 0.030(5) 0.042(5) 0.040(5) 0.009(4) 0.012(4) 0.000(4) Cl6S 0.0438(14) 0.0570(15) 0.0724(18) -0.0052(13) 0.0120(13) 0.0160(12) C3S 0.038(5) 0.057(6) 0.055(6) -0.006(5) 0.014(5) 0.003(5) Cl2 0.0223(9) 0.0233(8) 0.0142(8) -0.0011(7) 0.0070(6) 0.0023(7) Cl4S 0.094(3) 0.153(4) 0.074(2) 0.011(3) 0.017(2) -0.029(3) C2S 0.162(17) 0.086(11) 0.082(11) 0.017(9) -0.016(11) -0.014(11) 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' Ru Ru -1.2594 0.8363 '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' 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' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle N3 Ru1 N2 75.5(2) N3 Ru1 C19 136.4(2) N2 Ru1 C19 94.2(2) N3 Ru1 C21 92.6(2) N2 Ru1 C21 139.0(2) C19 Ru1 C21 67.6(2) N3 Ru1 C16 108.6(2) N2 Ru1 C16 174.3(2) C19 Ru1 C16 80.1(2) C21 Ru1 C16 38.4(3) N3 Ru1 C18 171.8(2) N2 Ru1 C18 108.2(2) C19 Ru1 C18 37.4(3) C21 Ru1 C18 79.8(2) C16 Ru1 C18 67.2(2) N3 Ru1 C17 141.5(2) N2 Ru1 C17 140.5(2) C19 Ru1 C17 68.0(2) C21 Ru1 C17 68.0(2) C16 Ru1 C17 37.0(3) C18 Ru1 C17 37.7(2) N3 Ru1 C20 104.0(2) N2 Ru1 C20 107.1(2) C19 Ru1 C20 38.1(3) C21 Ru1 C20 37.2(3) C16 Ru1 C20 68.4(3) C18 Ru1 C20 68.1(3) C17 Ru1 C20 80.9(2) N3 Ru1 Cl1 85.49(16) N2 Ru1 Cl1 82.76(15) C19 Ru1 Cl1 135.98(19) C21 Ru1 Cl1 136.15(18) C16 Ru1 Cl1 101.33(19) C18 Ru1 Cl1 102.12(19) C17 Ru1 Cl1 86.78(17) C20 Ru1 Cl1 167.67(18) C8 N2 C5 118.0(5) C8 N2 Ru1 115.2(4) C5 N2 Ru1 126.6(4) N2 C8 C7 123.3(6) N2 C8 C9 115.3(6) C7 C8 C9 121.4(6) C6 C7 C8 118.6(6) C6 C7 H7 120.7 C8 C7 H7 120.7 C7 C6 C4 119.7(6) C7 C6 H6 120.2 C4 C6 H6 120.2 C5 C4 C3 118.1(6) C5 C4 C6 118.8(6) C3 C4 C6 123.1(6) N1 C5 N2 115.9(5) N1 C5 C4 122.6(6) N2 C5 C4 121.5(6) C1 N1 C5 117.3(6) N1 C1 C2 124.6(6) N1 C1 H1 117.7 C2 C1 H1 117.7 C3 C2 C1 118.6(6) C3 C2 H2 120.7 C1 C2 H2 120.7 C2 C3 C4 118.8(6) C2 C3 H3 120.6 C4 C3 H3 120.6 N3 C9 C10 110.7(6) N3 C9 C8 115.3(6) C10 C9 C8 134.0(6) C9 N3 N4 106.1(5) C9 N3 Ru1 118.1(4) N4 N3 Ru1 135.3(4) N3 N4 C11 111.7(5) N3 N4 H4A 121(4) C11 N4 H4A 128(4) N4 C11 C10 106.4(6) N4 C11 C12 122.7(6) C10 C11 C12 130.9(6) C11 C10 C9 105.0(6) C11 C10 H10 127.5 C9 C10 H10 127.5 C11 C12 C14 108.7(6) C11 C12 C13 110.0(6) C14 C12 C13 110.5(6) C11 C12 C15 109.3(6) C14 C12 C15 109.1(6) C13 C12 C15 109.3(6) C12 C14 H14A 109.5 C12 C14 H14B 109.5 H14A C14 H14B 109.5 C12 C14 H14C 109.5 H14A C14 H14C 109.5 H14B C14 H14C 109.5 C12 C13 H13A 109.5 C12 C13 H13B 109.5 H13A C13 H13B 109.5 C12 C13 H13C 109.5 H13A C13 H13C 109.5 H13B C13 H13C 109.5 C12 C15 H15A 109.5 C12 C15 H15B 109.5 H15A C15 H15B 109.5 C12 C15 H15C 109.5 H15A C15 H15C 109.5 H15B C15 H15C 109.5 C19 C18 C17 120.3(6) C19 C18 Ru1 69.9(4) C17 C18 Ru1 71.9(4) C19 C18 H18 119.8 C17 C18 H18 119.8 Ru1 C18 H18 131.1 C16 C17 C18 118.4(6) C16 C17 C25 121.1(6) C18 C17 C25 120.5(6) C16 C17 Ru1 70.3(4) C18 C17 Ru1 70.4(4) C25 C17 Ru1 129.1(4) C17 C16 C21 120.6(6) C17 C16 Ru1 72.8(4) C21 C16 Ru1 70.3(4) C17 C16 H16 119.7 C21 C16 H16 119.7 Ru1 C16 H16 129.6 C20 C21 C16 121.7(6) C20 C21 Ru1 73.2(4) C16 C21 Ru1 71.3(4) C20 C21 H21 119.2 C16 C21 H21 119.2 Ru1 C21 H21 128.8 C21 C20 C19 116.8(6) C21 C20 C22 123.0(6) C19 C20 C22 120.2(6) C21 C20 Ru1 69.6(4) C19 C20 Ru1 68.8(4) C22 C20 Ru1 131.4(5) C18 C19 C20 122.1(6) C18 C19 Ru1 72.7(4) C20 C19 Ru1 73.2(4) C18 C19 H19 118.9 C20 C19 H19 118.9 Ru1 C19 H19 127.3 C20 C22 C24 113.0(7) C20 C22 C23 107.8(6) C24 C22 C23 111.4(7) C20 C22 H22 108.1 C24 C22 H22 108.1 C23 C22 H22 108.1 C22 C24 H24A 109.5 C22 C24 H24B 109.5 H24A C24 H24B 109.5 C22 C24 H24C 109.5 H24A C24 H24C 109.5 H24B C24 H24C 109.5 C22 C23 H23A 109.5 C22 C23 H23B 109.5 H23A C23 H23B 109.5 C22 C23 H23C 109.5 H23A C23 H23C 109.5 H23B C23 H23C 109.5 C17 C25 H25A 109.5 C17 C25 H25B 109.5 H25A C25 H25B 109.5 C17 C25 H25C 109.5 H25A C25 H25C 109.5 H25B C25 H25C 109.5 Cl1S C1S Cl2S 111.4(5) Cl1S C1S H1S1 109.3 Cl2S C1S H1S1 109.3 Cl1S C1S H1S2 109.3 Cl2S C1S H1S2 109.3 H1S1 C1S H1S2 108.0 Cl6S C3S Cl5S 111.7(6) Cl6S C3S H3S1 109.3 Cl5S C3S H3S1 109.3 Cl6S C3S H3S2 109.3 Cl5S C3S H3S2 109.3 H3S1 C3S H3S2 107.9 Cl3S C2S Cl4S 112.8(9) Cl3S C2S H2S1 109.0 Cl4S C2S H2S1 109.0 Cl3S C2S H2S2 109.0 Cl4S C2S H2S2 109.0 H2S1 C2S H2S2 107.8 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Ru1 N3 2.074(5) Ru1 N2 2.159(5) Ru1 C19 2.164(6) Ru1 C21 2.176(6) Ru1 C16 2.188(7) Ru1 C18 2.200(6) Ru1 C17 2.220(6) Ru1 C20 2.221(7) Ru1 Cl1 2.3949(17) N2 C8 1.342(8) N2 C5 1.367(8) C8 C7 1.420(9) C8 C9 1.446(9) C7 C6 1.351(10) C7 H7 0.9500 C6 C4 1.415(9) C6 H6 0.9500 C4 C5 1.406(9) C4 C3 1.407(9) C5 N1 1.353(8) N1 C1 1.318(9) C1 C2 1.393(10) C1 H1 0.9500 C2 C3 1.370(10) C2 H2 0.9500 C3 H3 0.9500 C9 N3 1.341(8) C9 C10 1.400(9) N3 N4 1.342(8) N4 C11 1.362(8) N4 H4A 0.96(7) C11 C10 1.396(9) C11 C12 1.499(9) C10 H10 0.9500 C12 C14 1.520(10) C12 C13 1.527(10) C12 C15 1.539(10) C14 H14A 0.9800 C14 H14B 0.9800 C14 H14C 0.9800 C13 H13A 0.9800 C13 H13B 0.9800 C13 H13C 0.9800 C15 H15A 0.9800 C15 H15B 0.9800 C15 H15C 0.9800 C18 C19 1.398(10) C18 C17 1.430(9) C18 H18 0.9500 C17 C16 1.398(10) C17 C25 1.494(10) C16 C21 1.435(10) C16 H16 0.9500 C21 C20 1.402(10) C21 H21 0.9500 C20 C19 1.431(10) C20 C22 1.517(10) C19 H19 0.9500 C22 C24 1.537(12) C22 C23 1.538(11) C22 H22 1.0000 C24 H24A 0.9800 C24 H24B 0.9800 C24 H24C 0.9800 C23 H23A 0.9800 C23 H23B 0.9800 C23 H23C 0.9800 C25 H25A 0.9800 C25 H25B 0.9800 C25 H25C 0.9800 Cl1S C1S 1.757(9) Cl2S C1S 1.780(9) Cl5S C3S 1.773(10) Cl3S C2S 1.669(16) C1S H1S1 0.9900 C1S H1S2 0.9900 Cl6S C3S 1.735(10) C3S H3S1 0.9900 C3S H3S2 0.9900 Cl4S C2S 1.747(16) C2S H2S1 0.9900 C2S H2S2 0.9900 loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C1 H1 Cl2 0.95 2.98 3.481(7) 114.6 2 C10 H10 Cl2 0.95 2.78 3.643(7) 150.7 4_566 C1S H1S1 Cl5S 0.99 2.97 3.688(9) 130.0 . C1S H1S2 Cl2 0.99 2.50 3.455(9) 161.4 . C3S H3S2 Cl2S 0.99 2.85 3.659(10) 138.9 . N4 H4A Cl2 0.96(7) 2.12(7) 3.075(6) 171(6) . C1 H1 Cl2 0.95 2.98 3.481(7) 114.6 2 C10 H10 Cl2 0.95 2.78 3.643(7) 150.7 4_566 C1S H1S1 Cl5S 0.99 2.97 3.688(9) 130.0 . C1S H1S2 Cl2 0.99 2.50 3.455(9) 161.4 . C3S H3S2 Cl2S 0.99 2.85 3.659(10) 138.9 . N4 H4A Cl2 0.96(7) 2.12(7) 3.075(6) 171(6) . loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion C5 N2 C8 C7 -1.3(9) Ru1 N2 C8 C7 -176.4(5) C5 N2 C8 C9 -179.5(6) Ru1 N2 C8 C9 5.4(7) N2 C8 C7 C6 -0.9(10) C9 C8 C7 C6 177.2(6) C8 C7 C6 C4 0.9(10) C7 C6 C4 C5 1.1(10) C7 C6 C4 C3 179.8(6) C8 N2 C5 N1 -176.6(6) Ru1 N2 C5 N1 -2.1(8) C8 N2 C5 C4 3.4(9) Ru1 N2 C5 C4 177.9(4) C3 C4 C5 N1 -2.1(9) C6 C4 C5 N1 176.7(6) C3 C4 C5 N2 177.9(6) C6 C4 C5 N2 -3.3(9) N2 C5 N1 C1 -178.3(6) C4 C5 N1 C1 1.8(9) C5 N1 C1 C2 0.0(10) N1 C1 C2 C3 -1.4(11) C1 C2 C3 C4 1.0(10) C5 C4 C3 C2 0.6(9) C6 C4 C3 C2 -178.1(6) N2 C8 C9 N3 0.9(9) C7 C8 C9 N3 -177.3(6) N2 C8 C9 C10 -179.6(7) C7 C8 C9 C10 2.2(12) C10 C9 N3 N4 -0.5(7) C8 C9 N3 N4 179.1(6) C10 C9 N3 Ru1 173.1(4) C8 C9 N3 Ru1 -7.3(8) C9 N3 N4 C11 -0.2(7) Ru1 N3 N4 C11 -172.2(5) N3 N4 C11 C10 0.8(8) N3 N4 C11 C12 -179.1(6) N4 C11 C10 C9 -1.1(7) C12 C11 C10 C9 178.9(7) N3 C9 C10 C11 1.0(8) C8 C9 C10 C11 -178.5(7) N4 C11 C12 C14 -178.9(6) C10 C11 C12 C14 1.2(10) N4 C11 C12 C13 -57.8(8) C10 C11 C12 C13 122.3(8) N4 C11 C12 C15 62.2(8) C10 C11 C12 C15 -117.7(8) C19 C18 C17 C16 -0.6(9) Ru1 C18 C17 C16 -53.0(5) C19 C18 C17 C25 176.9(6) Ru1 C18 C17 C25 124.5(6) C19 C18 C17 Ru1 52.4(5) C18 C17 C16 C21 -0.6(9) C25 C17 C16 C21 -178.1(6) Ru1 C17 C16 C21 -53.7(5) C18 C17 C16 Ru1 53.1(5) C25 C17 C16 Ru1 -124.4(6) C17 C16 C21 C20 -0.5(10) Ru1 C16 C21 C20 -55.4(6) C17 C16 C21 Ru1 54.8(5) C16 C21 C20 C19 2.8(9) Ru1 C21 C20 C19 -51.7(5) C16 C21 C20 C22 -178.6(6) Ru1 C21 C20 C22 126.9(6) C16 C21 C20 Ru1 54.5(5) C17 C18 C19 C20 3.0(10) Ru1 C18 C19 C20 56.4(6) C17 C18 C19 Ru1 -53.3(5) C21 C20 C19 C18 -4.1(9) C22 C20 C19 C18 177.3(6) Ru1 C20 C19 C18 -56.2(6) C21 C20 C19 Ru1 52.1(5) C22 C20 C19 Ru1 -126.5(6) C21 C20 C22 C24 -19.0(10) C19 C20 C22 C24 159.5(7) Ru1 C20 C22 C24 72.1(9) C21 C20 C22 C23 104.6(8) C19 C20 C22 C23 -76.9(8) Ru1 C20 C22 C23 -164.3(6)