#------------------------------------------------------------------------------ #$Date: 2017-06-05 03:42:40 +0300 (Mon, 05 Jun 2017) $ #$Revision: 197476 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/08/72/4087261.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_4087261 loop_ _publ_author_name 'Hartmann, Nathaniel J.' 'Wu, Guang' 'Hayton, Trevor W.' _publ_section_title ; Trapping of an NiII Sulfide by a CoI Fulvene Complex ; _journal_issue 9 _journal_name_full Organometallics _journal_page_first 1765 _journal_paper_doi 10.1021/acs.organomet.7b00123 _journal_volume 36 _journal_year 2017 _chemical_formula_moiety 'C55 H82 Co N2 Ni S, C4 H10 O' _chemical_formula_sum 'C59 H92 Co N2 Ni O S' _chemical_formula_weight 995.04 _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' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2014/7 _cell_angle_alpha 90 _cell_angle_beta 102.645(5) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 12.2784(8) _cell_length_b 25.957(2) _cell_length_c 17.8363(12) _cell_measurement_reflns_used 315 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 25.4 _cell_measurement_theta_min 2.13 _cell_volume 5546.7(7) _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _diffrn_ambient_temperature 100(2) _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.989 _diffrn_measurement_device_type 'Bruker Kappa Apex II' _diffrn_measurement_method 'Omega scan' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.1760 _diffrn_reflns_av_unetI/netI 0.1997 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.989 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_number 34753 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.989 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 26.526 _diffrn_reflns_theta_min 1.409 _exptl_absorpt_coefficient_mu 0.715 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details sadabs _exptl_crystal_colour Brown _exptl_crystal_density_diffrn 1.192 _exptl_crystal_description Plate _exptl_crystal_F_000 2156 _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.05 _exptl_transmission_factor_max 0.7454 _exptl_transmission_factor_min 0.6070 _refine_diff_density_max 1.217 _refine_diff_density_min -0.684 _refine_diff_density_rms 0.089 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.984 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 611 _refine_ls_number_reflns 11410 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 0.984 _refine_ls_R_factor_all 0.2038 _refine_ls_R_factor_gt 0.0802 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0350P)^2^+10.3436P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1283 _refine_ls_wR_factor_ref 0.1654 _reflns_Friedel_coverage 0.000 _reflns_number_gt 5043 _reflns_number_total 11410 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file om7b00123_si_002.cif _cod_data_source_block Complex_1 _cod_depositor_comments 'Adding full bibliography for 4087261.cif.' _cod_original_cell_volume 5546.8(7) _cod_database_code 4087261 _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_res_file ; NH_4_104a_0m_a.res created by SHELXL-2014/7 TITL NH_4_104a_0m_a.res in P2(1)/c CELL 0.71073 12.2784 25.9575 17.8363 90.000 102.645 90.000 ZERR 4.000 0.0008 0.0020 0.0012 0.000 0.005 0.000 LATT 1 SYMM -X, 1/2+Y, 1/2-Z SFAC C H N O Co Ni S UNIT 236 368 8 4 4 4 4 L.S. 10 ACTA BOND $H FMAP 2 PLAN 20 TEMP -173.100 WGHT 0.035000 10.343600 FVAR 0.23021 C1 1 0.214066 0.506703 0.711245 11.00000 0.04184 0.05556 = 0.04030 -0.00390 -0.00448 0.01162 AFIX 23 H1A 2 0.191276 0.506056 0.761154 11.00000 -1.20000 H1B 2 0.283384 0.527250 0.717354 11.00000 -1.20000 AFIX 0 C2 1 0.537764 0.481156 0.763009 11.00000 0.01738 0.03300 = 0.02769 0.00766 0.00026 -0.00401 C3 1 0.543170 0.483584 0.684451 11.00000 0.02917 0.04061 = 0.03076 0.00334 0.00416 -0.01022 C4 1 0.550178 0.435529 0.638438 11.00000 0.03863 0.05117 = 0.02957 0.00992 0.00889 -0.00983 AFIX 13 H4 2 0.542841 0.405183 0.671517 11.00000 -1.20000 AFIX 0 C5 1 0.661989 0.431442 0.615423 11.00000 0.06273 0.06500 = 0.05292 -0.00103 0.02466 -0.01176 AFIX 137 H5A 2 0.668475 0.459205 0.579422 11.00000 -1.50000 H5B 2 0.667092 0.398067 0.590738 11.00000 -1.50000 H5C 2 0.722474 0.434420 0.661273 11.00000 -1.50000 AFIX 0 C6 1 0.455018 0.432777 0.566115 11.00000 0.07451 0.08026 = 0.02749 0.00781 0.00082 -0.00837 AFIX 137 H6A 2 0.383033 0.435867 0.580971 11.00000 -1.50000 H6B 2 0.458395 0.399728 0.540158 11.00000 -1.50000 H6C 2 0.463106 0.460984 0.531221 11.00000 -1.50000 AFIX 0 C7 1 0.541684 0.532976 0.651599 11.00000 0.03555 0.05543 = 0.02740 0.01845 -0.00088 -0.00761 AFIX 43 H7 2 0.546310 0.535551 0.599257 11.00000 -1.20000 AFIX 0 C8 1 0.534038 0.576720 0.690627 11.00000 0.03502 0.03312 = 0.05636 0.01329 0.00237 -0.01456 AFIX 43 H8 2 0.533605 0.609230 0.666103 11.00000 -1.20000 AFIX 0 C9 1 0.526877 0.573865 0.766195 11.00000 0.02504 0.03251 = 0.06459 0.00474 -0.00584 -0.00268 AFIX 43 H9 2 0.521693 0.604796 0.793671 11.00000 -1.20000 AFIX 0 C10 1 0.527011 0.526591 0.803828 11.00000 0.02251 0.02692 = 0.03924 0.01168 -0.00390 -0.00483 C11 1 0.396829 0.516238 0.892761 11.00000 0.04514 0.07952 = 0.03620 -0.00116 0.00353 0.01978 AFIX 137 H11A 2 0.350634 0.545138 0.868855 11.00000 -1.50000 H11B 2 0.393392 0.513793 0.947023 11.00000 -1.50000 H11C 2 0.368994 0.484178 0.866378 11.00000 -1.50000 AFIX 0 C12 1 0.516313 0.524884 0.886632 11.00000 0.04817 0.03640 = 0.02388 -0.00419 -0.00678 0.00388 AFIX 13 H12 2 0.560218 0.494435 0.910856 11.00000 -1.20000 AFIX 0 C13 1 0.564401 0.572237 0.933578 11.00000 0.12134 0.06012 = 0.05502 -0.02263 -0.00644 -0.01300 AFIX 137 H13A 2 0.641891 0.577438 0.929368 11.00000 -1.50000 H13B 2 0.562005 0.566908 0.987587 11.00000 -1.50000 H13C 2 0.520089 0.602673 0.913828 11.00000 -1.50000 AFIX 0 C14 1 0.608630 0.406711 0.846126 11.00000 0.01557 0.02879 = 0.01753 -0.00368 0.00298 -0.00027 C15 1 0.734782 0.423960 0.869653 11.00000 0.01922 0.04278 = 0.02051 0.00250 0.00013 -0.00484 C16 1 0.767575 0.474373 0.837231 11.00000 0.02528 0.04779 = 0.04366 0.00945 0.00324 -0.01158 AFIX 137 H16A 2 0.848805 0.478532 0.851748 11.00000 -1.50000 H16B 2 0.731583 0.503127 0.857947 11.00000 -1.50000 H16C 2 0.743477 0.473959 0.781098 11.00000 -1.50000 AFIX 0 C17 1 0.770772 0.428852 0.958343 11.00000 0.02278 0.04413 = 0.03184 0.00258 -0.00245 0.00078 AFIX 137 H17A 2 0.749605 0.397522 0.982315 11.00000 -1.50000 H17B 2 0.733588 0.458651 0.975418 11.00000 -1.50000 H17C 2 0.851853 0.433473 0.973310 11.00000 -1.50000 AFIX 0 C18 1 0.805278 0.381849 0.843599 11.00000 0.02297 0.06023 = 0.04677 -0.00786 0.01147 -0.00837 AFIX 137 H18A 2 0.787171 0.379795 0.787372 11.00000 -1.50000 H18B 2 0.789253 0.348687 0.865138 11.00000 -1.50000 H18C 2 0.884611 0.390065 0.861581 11.00000 -1.50000 AFIX 0 C19 1 0.585057 0.360644 0.879445 11.00000 0.01430 0.02479 = 0.02052 0.00818 0.00054 0.00592 AFIX 43 H19 2 0.646870 0.346753 0.915299 11.00000 -1.20000 AFIX 0 C20 1 0.488557 0.331035 0.870402 11.00000 0.02046 0.02176 = 0.01498 -0.00083 0.00759 0.00741 C21 1 0.502911 0.279738 0.917136 11.00000 0.02625 0.02433 = 0.01726 0.00381 0.00382 0.00265 C22 1 0.592769 0.246495 0.892208 11.00000 0.03820 0.02499 = 0.04373 0.00801 0.00863 0.00820 AFIX 137 H22A 2 0.603832 0.214709 0.922578 11.00000 -1.50000 H22B 2 0.663094 0.265718 0.900605 11.00000 -1.50000 H22C 2 0.568530 0.237914 0.837586 11.00000 -1.50000 AFIX 0 C23 1 0.542780 0.293488 1.003570 11.00000 0.03583 0.03578 = 0.02879 0.00463 0.00290 -0.00073 AFIX 137 H23A 2 0.486886 0.315359 1.019563 11.00000 -1.50000 H23B 2 0.613966 0.311986 1.011512 11.00000 -1.50000 H23C 2 0.552639 0.261791 1.034161 11.00000 -1.50000 AFIX 0 C24 1 0.401093 0.245917 0.912112 11.00000 0.03382 0.03163 = 0.03103 0.01095 0.00489 -0.00396 AFIX 137 H24A 2 0.373982 0.234524 0.858912 11.00000 -1.50000 H24B 2 0.342384 0.265533 0.928738 11.00000 -1.50000 H24C 2 0.421014 0.215805 0.945436 11.00000 -1.50000 AFIX 0 C25 1 0.288128 0.320789 0.803747 11.00000 0.01943 0.02340 = 0.02561 0.00305 -0.00158 -0.00175 C26 1 0.267514 0.287948 0.739212 11.00000 0.02742 0.03793 = 0.02476 -0.00535 0.00190 -0.00905 C27 1 0.335890 0.303930 0.619067 11.00000 0.07740 0.06783 = 0.03904 0.00548 0.02230 -0.00586 AFIX 137 H27A 2 0.266556 0.291171 0.586142 11.00000 -1.50000 H27B 2 0.398111 0.297893 0.593875 11.00000 -1.50000 H27C 2 0.329018 0.340938 0.627872 11.00000 -1.50000 AFIX 0 C28 1 0.357810 0.275384 0.696359 11.00000 0.03743 0.03619 = 0.02742 -0.00396 0.00364 -0.00497 AFIX 13 H28 2 0.430184 0.288316 0.727902 11.00000 -1.20000 AFIX 0 C29 1 0.370645 0.217783 0.684208 11.00000 0.05238 0.04240 = 0.03974 -0.00927 0.01575 -0.00180 AFIX 137 H29A 2 0.385157 0.200150 0.733990 11.00000 -1.50000 H29B 2 0.433180 0.211893 0.659266 11.00000 -1.50000 H29C 2 0.301855 0.204264 0.651554 11.00000 -1.50000 AFIX 0 C30 1 0.160047 0.269342 0.712058 11.00000 0.03871 0.05426 = 0.02991 -0.01221 -0.00478 -0.01745 AFIX 43 H30 2 0.145261 0.247625 0.668124 11.00000 -1.20000 AFIX 0 C31 1 0.074669 0.281679 0.747387 11.00000 0.02518 0.06609 = 0.04853 -0.00997 -0.00737 -0.01653 AFIX 43 H31 2 0.001861 0.268395 0.727961 11.00000 -1.20000 AFIX 0 C32 1 0.094639 0.313403 0.811173 11.00000 0.02895 0.04318 = 0.03583 -0.00394 0.00287 -0.00058 AFIX 43 H32 2 0.035213 0.321913 0.835235 11.00000 -1.20000 AFIX 0 C33 1 0.201000 0.333017 0.840518 11.00000 0.01912 0.02645 = 0.02948 0.00156 0.00157 -0.00757 C34 1 0.219331 0.368401 0.910299 11.00000 0.02131 0.03517 = 0.02869 -0.00012 0.00419 0.00007 AFIX 13 H34 2 0.301512 0.374072 0.927985 11.00000 -1.20000 AFIX 0 C35 1 0.177234 0.344233 0.976807 11.00000 0.05014 0.05377 = 0.03054 0.00477 0.01880 -0.00129 AFIX 137 H35A 2 0.096342 0.339067 0.961442 11.00000 -1.50000 H35B 2 0.194263 0.367180 1.021479 11.00000 -1.50000 H35C 2 0.214106 0.310959 0.990143 11.00000 -1.50000 AFIX 0 C36 1 0.165317 0.420266 0.889149 11.00000 0.03673 0.04454 = 0.04797 -0.00549 0.01719 -0.00090 AFIX 137 H36A 2 0.194538 0.435388 0.847192 11.00000 -1.50000 H36B 2 0.182077 0.443120 0.933934 11.00000 -1.50000 H36C 2 0.084320 0.415914 0.872608 11.00000 -1.50000 AFIX 0 C37 1 0.123648 0.530291 0.650833 11.00000 0.02882 0.03801 = 0.03534 0.00004 -0.00100 0.01333 C38 1 0.006674 0.518847 0.640697 11.00000 0.03380 0.04309 = 0.03607 0.00844 -0.00057 -0.00107 C39 1 -0.044052 0.482969 0.688189 11.00000 0.05533 0.04258 = 0.05130 0.01049 0.01067 -0.00216 AFIX 137 H39A 2 -0.116218 0.496639 0.693846 11.00000 -1.50000 H39B 2 0.005652 0.479373 0.739001 11.00000 -1.50000 H39C 2 -0.055076 0.449210 0.663071 11.00000 -1.50000 AFIX 0 C40 1 -0.050264 0.547743 0.576289 11.00000 0.03364 0.02661 = 0.04897 0.00543 -0.00121 -0.00443 C41 1 -0.174419 0.547195 0.541816 11.00000 0.03756 0.05684 = 0.05056 0.00587 -0.01798 -0.01037 AFIX 137 H41A 2 -0.190713 0.521561 0.500536 11.00000 -1.50000 H41B 2 -0.197996 0.581326 0.520918 11.00000 -1.50000 H41C 2 -0.214921 0.538344 0.581678 11.00000 -1.50000 AFIX 0 C42 1 0.029108 0.576946 0.546466 11.00000 0.03933 0.04308 = 0.03234 0.00033 -0.00174 -0.00220 C43 1 0.004604 0.610774 0.476535 11.00000 0.08229 0.06419 = 0.03509 0.01029 0.00167 -0.01105 AFIX 137 H43A 2 0.074264 0.625958 0.468561 11.00000 -1.50000 H43B 2 -0.046720 0.638290 0.483861 11.00000 -1.50000 H43C 2 -0.029731 0.590158 0.431525 11.00000 -1.50000 AFIX 0 C44 1 0.136310 0.566037 0.592681 11.00000 0.03358 0.04399 = 0.03814 -0.00674 0.00069 -0.00592 C45 1 0.245561 0.586255 0.582739 11.00000 0.03891 0.07888 = 0.05293 -0.02190 0.02163 -0.00956 AFIX 137 H45A 2 0.294121 0.592660 0.633277 11.00000 -1.50000 H45B 2 0.233809 0.618507 0.553519 11.00000 -1.50000 H45C 2 0.280765 0.560924 0.554866 11.00000 -1.50000 AFIX 0 C46 1 -0.066917 0.625703 0.724688 11.00000 0.03683 0.04472 = 0.05928 -0.00145 0.02074 -0.00604 C47 1 -0.174508 0.605534 0.738061 11.00000 0.06378 0.07035 = 0.13248 -0.02081 0.05879 -0.01541 AFIX 137 H47A 2 -0.202314 0.628584 0.773173 11.00000 -1.50000 H47B 2 -0.162867 0.571048 0.760765 11.00000 -1.50000 H47C 2 -0.229203 0.603685 0.689052 11.00000 -1.50000 AFIX 0 C48 1 -0.054013 0.660968 0.666383 11.00000 0.03107 0.04498 = 0.05148 -0.00295 -0.00053 -0.00108 C49 1 -0.147193 0.684162 0.607350 11.00000 0.05440 0.06218 = 0.09550 -0.00217 -0.02080 0.02267 AFIX 137 H49A 2 -0.171174 0.716468 0.627165 11.00000 -1.50000 H49B 2 -0.210150 0.660086 0.596149 11.00000 -1.50000 H49C 2 -0.121096 0.691076 0.560192 11.00000 -1.50000 AFIX 0 C50 1 0.059480 0.673112 0.675845 11.00000 0.03986 0.03497 = 0.03303 0.00937 0.00830 -0.00040 C51 1 0.110057 0.709488 0.629880 11.00000 0.07162 0.05283 = 0.04776 0.00628 0.02028 -0.00158 AFIX 137 H51A 2 0.070647 0.707383 0.575891 11.00000 -1.50000 H51B 2 0.188826 0.700663 0.634363 11.00000 -1.50000 H51C 2 0.104327 0.744604 0.648822 11.00000 -1.50000 AFIX 0 C52 1 0.119928 0.644467 0.740159 11.00000 0.03125 0.04335 = 0.04060 -0.00776 -0.00251 0.00708 C53 1 0.243305 0.645307 0.772272 11.00000 0.04094 0.05868 = 0.06379 -0.01520 -0.01579 0.00821 AFIX 137 H53A 2 0.260019 0.668487 0.816682 11.00000 -1.50000 H53B 2 0.281525 0.657517 0.732820 11.00000 -1.50000 H53C 2 0.269094 0.610467 0.788324 11.00000 -1.50000 AFIX 0 C54 1 0.040029 0.615816 0.769783 11.00000 0.06404 0.03297 = 0.03493 -0.00220 0.01535 0.00295 C55 1 0.064140 0.579840 0.838386 11.00000 0.13040 0.05984 = 0.03914 0.00971 0.03071 0.00427 AFIX 137 H55A 2 0.142579 0.569191 0.848544 11.00000 -1.50000 H55B 2 0.016121 0.549383 0.827431 11.00000 -1.50000 H55C 2 0.049307 0.597691 0.883529 11.00000 -1.50000 AFIX 0 C56 1 0.084084 0.708276 0.936823 11.00000 0.05372 0.06153 = 0.05761 0.01373 0.02405 0.00347 AFIX 137 H56A 2 0.042824 0.695424 0.887006 11.00000 -1.50000 H56B 2 0.032512 0.713153 0.971106 11.00000 -1.50000 H56C 2 0.141696 0.683284 0.959591 11.00000 -1.50000 AFIX 0 C57 1 0.137663 0.758432 0.925821 11.00000 0.04076 0.06524 = 0.03659 -0.00011 0.00914 0.00800 AFIX 23 H57A 2 0.079731 0.785131 0.909554 11.00000 -1.20000 H57B 2 0.186822 0.769578 0.974790 11.00000 -1.20000 AFIX 0 C58 1 0.257276 0.797678 0.857994 11.00000 0.04804 0.05695 = 0.04351 0.00635 0.00653 -0.00049 AFIX 23 H58A 2 0.303226 0.809654 0.907632 11.00000 -1.20000 H58B 2 0.202720 0.825049 0.837475 11.00000 -1.20000 AFIX 0 C59 1 0.331127 0.787528 0.802230 11.00000 0.05212 0.07066 = 0.04493 0.00222 0.01812 -0.00853 AFIX 137 H59A 2 0.381905 0.758968 0.821196 11.00000 -1.50000 H59B 2 0.374656 0.818512 0.797357 11.00000 -1.50000 H59C 2 0.284795 0.778510 0.751911 11.00000 -1.50000 AFIX 0 CO1 5 0.033703 0.596751 0.657401 11.00000 0.02509 0.04152 = 0.03108 -0.00060 0.00313 -0.00242 N1 3 0.529091 0.432133 0.797102 11.00000 0.02362 0.02616 = 0.01918 0.00380 0.00231 -0.00323 N2 3 0.392754 0.346959 0.824790 11.00000 0.01534 0.02686 = 0.01910 -0.00240 0.00096 0.00130 NI01 6 0.378662 0.408542 0.765660 11.00000 0.01927 0.02907 = 0.02038 0.00416 -0.00037 -0.00018 O1 4 0.200509 0.752378 0.869383 11.00000 0.03890 0.04632 = 0.03398 0.00045 0.00942 0.00405 S1 7 0.238872 0.439615 0.680646 11.00000 0.04455 0.06501 = 0.03112 -0.00210 -0.00835 0.02305 HKLF 4 REM NH_4_104a_0m_a.res in P2(1)/c REM R1 = 0.0802 for 5043 Fo > 4sig(Fo) and 0.2038 for all 11410 data REM 611 parameters refined using 0 restraints END WGHT 0.0594 1.4673 REM Highest difference peak 1.217, deepest hole -0.684, 1-sigma level 0.089 Q1 1 0.2150 0.4003 0.6804 11.00000 0.05 1.22 Q2 1 0.0257 0.6325 0.6421 11.00000 0.05 0.64 Q3 1 0.0287 0.6324 0.6701 11.00000 0.05 0.63 Q4 1 -0.1250 0.5787 0.6230 11.00000 0.05 0.45 Q5 1 0.4125 0.3875 0.7406 11.00000 0.05 0.43 Q6 1 -0.0280 0.5569 0.6562 11.00000 0.05 0.43 Q7 1 -0.0373 0.6080 0.6210 11.00000 0.05 0.41 Q8 1 0.3165 0.4760 0.6987 11.00000 0.05 0.40 Q9 1 0.3268 0.4529 0.6807 11.00000 0.05 0.37 Q10 1 0.4208 0.4263 0.7455 11.00000 0.05 0.36 Q11 1 0.0200 0.6353 0.5399 11.00000 0.05 0.34 Q12 1 0.0181 0.6078 0.9781 11.00000 0.05 0.33 Q13 1 0.2397 0.6429 0.4625 11.00000 0.05 0.32 Q14 1 -0.1071 0.6267 0.6829 11.00000 0.05 0.32 Q15 1 0.1593 0.5999 0.5956 11.00000 0.05 0.32 Q16 1 -0.1055 0.5555 0.5591 11.00000 0.05 0.32 Q17 1 0.5537 0.6319 0.7982 11.00000 0.05 0.32 Q18 1 0.5817 0.4568 0.6692 11.00000 0.05 0.32 Q19 1 0.4529 0.3763 0.8019 11.00000 0.05 0.31 Q20 1 -0.2470 0.6333 0.6181 11.00000 0.05 0.31 ; _shelx_res_checksum 1042 _shelx_hkl_file ; 1 0 0 26.50 3.60 1 0 0 16.60 4.20 -1 0 0 9.90 4.40 2 0 0 1621.74 37.90 -2 0 0 1580.14 37.80 2 0 0 1603.44 36.30 3 0 0 339.37 15.70 -3 0 0 334.67 18.20 3 0 0 291.67 20.80 4 0 0 432.46 18.80 -4 0 0 420.66 21.40 -5 0 0 1459.45 42.20 5 0 0 1434.86 39.00 -6 0 0 46.70 14.70 6 0 0 69.89 12.50 -7 0 0 426.76 26.60 7 0 0 422.46 23.00 -8 0 0 285.27 20.60 8 0 0 339.07 22.50 -8 0 0 253.97 23.70 -9 0 0 278.07 22.00 9 0 0 229.78 21.50 -9 0 0 235.28 25.10 -10 0 0 76.79 21.90 10 0 0 88.99 18.90 -11 0 0 6.20 21.00 11 0 0 20.10 19.20 12 0 0 311.47 28.70 -12 0 0 318.27 33.50 13 0 0 72.79 23.10 -13 0 0 19.10 25.90 14 0 0 164.18 29.10 0 -1 0 -2.80 1.10 1 -1 0 219.58 9.30 -1 -1 0 223.38 8.70 1 -1 0 209.18 8.30 -1 1 0 221.08 9.40 1 1 0 218.08 8.90 2 -1 0 742.23 22.00 -2 -1 0 751.12 21.50 2 -1 0 703.83 19.70 2 1 0 740.73 21.60 2 1 0 733.33 19.50 -2 1 0 683.53 21.90 -3 -1 0 6.20 10.40 3 -1 0 17.90 8.70 -3 1 0 -5.40 11.20 3 1 0 19.90 8.10 3 1 0 9.10 11.10 4 -1 0 249.48 16.50 -4 -1 0 212.08 16.40 4 1 0 231.48 14.50 -4 1 0 257.27 17.30 -5 -1 0 616.94 27.50 5 -1 0 670.03 24.40 -5 1 0 611.54 27.60 5 1 0 618.34 22.90 6 -1 0 14.70 11.70 -6 -1 0 69.89 14.70 6 1 0 32.70 11.10 -6 1 0 29.50 14.00 -7 -1 0 106.29 17.20 7 -1 0 118.99 15.50 7 1 0 81.29 13.10 -7 1 0 92.99 17.40 -7 1 0 99.99 14.70 -8 -1 0 -2.20 16.00 -8 -1 0 29.00 13.00 8 -1 0 24.20 13.20 8 1 0 12.90 12.40 -8 1 0 5.50 15.40 -8 1 0 38.50 13.90 9 -1 0 10.80 14.90 -9 -1 0 34.00 14.10 -9 -1 0 0.10 16.70 -9 1 0 -14.10 16.90 9 1 0 28.80 15.00 -10 -1 0 492.65 34.50 10 -1 0 388.46 28.40 -10 1 0 457.75 33.70 10 1 0 403.76 27.60 -11 -1 0 -11.40 20.10 11 -1 0 -20.50 17.90 -11 1 0 -0.40 20.90 11 1 0 15.00 18.50 12 -1 0 60.19 22.00 -12 -1 0 28.40 23.70 12 1 0 70.29 21.20 -12 1 0 -21.20 21.60 13 -1 0 39.00 22.90 -13 -1 0 1.00 23.40 -13 1 0 0.20 25.00 13 1 0 34.90 22.10 14 -1 0 -13.40 22.30 14 1 0 78.89 25.90 -14 1 0 92.69 42.00 0 -2 0 1121.19 24.40 -1 -2 0 183.38 9.60 1 -2 0 214.48 10.90 1 -2 0 197.38 8.70 1 2 0 207.88 9.70 -1 2 0 190.08 10.80 2 -2 0 1034.10 28.50 2 -2 0 1073.69 27.00 -2 -2 0 1000.30 27.10 -2 2 0 966.70 28.40 2 2 0 1013.80 27.60 -3 -2 0 109.39 12.60 3 -2 0 110.69 12.00 -3 2 0 111.39 13.60 3 2 0 133.89 15.50 4 -2 0 1766.52 44.00 -4 -2 0 1682.73 45.00 -4 2 0 1684.03 46.10 4 2 0 1754.42 42.10 5 -2 0 211.38 15.50 -5 -2 0 218.98 17.40 -5 2 0 228.28 18.80 5 2 0 223.58 16.30 -6 -2 0 0.90 13.20 6 -2 0 -3.60 11.70 -6 2 0 18.40 14.10 6 2 0 3.00 10.20 7 -2 0 -5.20 12.00 -7 -2 0 18.30 14.40 -7 2 0 10.50 12.50 7 2 0 -13.70 10.90 -7 2 0 -28.70 13.20 8 -2 0 68.29 15.70 -8 -2 0 59.19 17.30 -8 -2 0 100.99 14.50 8 2 0 52.49 14.20 -8 2 0 65.59 17.90 -8 2 0 52.99 15.30 9 -2 0 -0.20 15.00 -9 -2 0 24.60 13.90 -9 -2 0 60.89 18.70 9 2 0 48.90 15.00 -9 2 0 24.30 18.30 -10 -2 0 139.69 23.80 10 -2 0 122.29 21.10 -10 2 0 166.28 24.70 10 2 0 128.39 19.20 -11 -2 0 -38.30 19.00 11 -2 0 -47.90 17.20 -11 2 0 19.50 20.50 11 2 0 2.10 17.60 12 -2 0 120.99 23.60 -12 -2 0 107.59 26.40 12 2 0 86.89 22.60 -12 2 0 81.99 25.70 13 -2 0 49.20 23.00 -13 -2 0 9.90 24.50 13 2 0 41.90 22.40 -13 2 0 74.19 27.80 14 -2 0 89.59 27.20 -14 2 0 78.79 28.70 14 2 0 56.69 25.10 0 -3 0 -8.90 4.90 1 -3 0 3.40 6.90 -1 -3 0 -1.90 7.00 -1 -3 0 6.30 4.60 1 3 0 -1.40 6.90 2 -3 0 287.17 15.50 2 -3 0 277.27 17.50 -2 -3 0 241.28 15.60 2 3 0 282.17 15.80 -2 3 0 240.68 15.80 -3 -3 0 20.50 11.40 3 -3 0 9.30 10.40 -3 3 0 7.30 11.20 -4 -3 0 1827.92 46.70 4 -3 0 1760.02 45.70 -4 3 0 1802.02 48.40 -5 -3 0 326.27 21.50 5 -3 0 331.07 20.30 -5 3 0 334.97 23.00 5 3 0 373.66 17.90 6 -3 0 -16.30 11.20 -6 -3 0 -12.10 12.40 -6 3 0 -8.90 13.30 6 3 0 14.50 9.80 7 -3 0 190.28 18.40 -7 -3 0 173.48 19.30 -7 3 0 201.68 18.40 7 3 0 185.98 15.40 -7 3 0 190.38 21.20 -8 -3 0 381.16 26.90 8 -3 0 374.86 25.60 -8 3 0 376.06 28.20 -8 3 0 360.06 24.30 8 3 0 334.37 22.30 -9 -3 0 63.59 14.80 -9 -3 0 77.79 19.90 9 -3 0 44.40 16.70 -9 3 0 97.99 20.70 9 3 0 63.29 15.30 10 -3 0 370.16 27.30 -10 -3 0 388.26 31.20 10 3 0 404.36 27.80 -10 3 0 405.56 32.90 -11 -3 0 9.40 20.90 11 -3 0 5.50 19.00 -11 3 0 1.00 20.60 11 3 0 -7.40 17.50 -12 -3 0 65.49 25.20 12 -3 0 89.49 23.20 12 3 0 70.79 20.70 -12 3 0 131.09 27.30 -13 -3 0 20.20 24.10 13 -3 0 40.60 24.00 -13 3 0 -0.40 25.60 13 3 0 14.70 20.90 14 -3 0 57.49 25.00 -14 3 0 -3.90 25.70 14 3 0 43.20 24.30 0 -4 0 104.49 8.10 -1 -4 0 1554.24 37.10 -1 -4 0 1466.05 33.50 1 -4 0 1551.34 36.00 1 4 0 1446.86 36.60 -2 -4 0 -15.60 10.20 2 -4 0 4.40 9.60 -2 4 0 18.90 12.10 2 4 0 7.50 10.60 -3 -4 0 676.93 24.80 3 -4 0 699.03 24.50 -3 4 0 702.23 27.20 -4 -4 0 20.50 12.00 4 -4 0 20.40 11.30 -4 4 0 14.00 11.10 5 -4 0 549.45 23.10 -5 -4 0 509.85 25.50 5 4 0 541.35 20.20 -5 4 0 565.04 27.50 -6 -4 0 -1.10 13.00 6 -4 0 5.20 12.00 6 4 0 2.50 9.00 -6 4 0 11.80 14.00 -6 4 0 1.10 12.40 -7 -4 0 64.99 16.20 7 -4 0 74.89 15.60 -7 4 0 85.69 17.10 7 4 0 77.29 13.10 -7 4 0 82.79 15.00 -8 -4 0 19.10 15.40 8 -4 0 12.80 13.80 8 4 0 8.40 11.30 -8 4 0 13.70 16.40 -9 -4 0 161.78 17.60 -9 -4 0 183.88 22.80 9 -4 0 133.19 19.40 -9 4 0 147.79 22.60 9 4 0 167.58 18.30 10 -4 0 35.60 18.30 -10 -4 0 -6.30 18.50 10 4 0 20.60 16.40 -10 4 0 23.00 20.00 -11 -4 0 34.00 21.70 11 -4 0 42.90 19.50 11 4 0 21.20 18.30 -11 4 0 20.20 20.60 -12 -4 0 69.89 25.50 12 -4 0 72.39 22.60 12 4 0 83.59 20.80 -12 4 0 65.99 25.40 13 -4 0 -12.10 22.00 -13 -4 0 29.70 24.90 13 4 0 -5.40 21.10 -13 4 0 20.70 24.40 14 -4 0 33.00 25.60 -14 4 0 14.70 26.40 14 4 0 60.19 24.50 0 -5 0 -7.80 8.00 -1 -5 0 174.78 12.30 1 -5 0 204.48 12.90 -1 -5 0 182.38 14.30 1 5 0 225.78 14.50 2 -5 0 388.96 19.60 -2 -5 0 413.36 19.70 -2 5 0 330.47 22.00 -3 -5 0 14.10 10.50 3 -5 0 11.00 10.60 -3 5 0 -17.50 11.80 -4 -5 0 65.49 12.80 4 -5 0 36.30 12.00 -4 5 0 48.60 14.30 5 -5 0 16.10 10.80 -5 -5 0 6.70 12.90 -5 5 0 -2.20 13.10 6 -5 0 -1.60 10.90 -6 -5 0 -7.30 12.70 6 5 0 11.10 9.20 -6 5 0 -20.40 11.30 -6 5 0 6.70 13.90 -7 -5 0 32.10 14.70 7 -5 0 19.20 12.20 -7 5 0 52.69 16.60 7 5 0 34.80 11.00 -8 -5 0 -13.60 15.10 8 -5 0 3.80 12.70 8 5 0 1.10 11.60 -8 5 0 11.60 16.50 -9 -5 0 24.10 18.00 9 -5 0 41.20 17.20 -9 -5 0 16.90 13.60 -9 5 0 -8.00 17.00 9 5 0 26.30 14.00 10 -5 0 -13.10 17.00 -10 -5 0 52.89 20.80 -10 5 0 42.40 20.40 10 5 0 23.90 16.00 11 -5 0 19.20 19.70 -11 -5 0 36.80 21.70 11 5 0 23.60 18.20 -11 5 0 14.60 21.60 12 -5 0 -19.80 18.80 -12 -5 0 -7.60 22.60 -12 5 0 -32.70 21.00 12 5 0 -32.80 18.20 -13 -5 0 18.10 24.50 13 -5 0 -11.10 22.40 13 5 0 20.30 21.50 -13 5 0 -4.50 24.30 14 -5 0 2.20 24.10 -14 5 0 53.29 29.70 0 -6 0 5450.15 114.29 -1 -6 0 125.59 9.90 1 -6 0 143.39 12.80 2 -6 0 156.48 14.00 -2 -6 0 126.89 14.00 -2 -6 0 146.99 9.90 -3 -6 0 377.96 20.50 3 -6 0 350.06 20.50 -3 6 0 350.46 21.10 4 -6 0 60.29 12.80 -4 -6 0 72.79 13.80 -4 6 0 49.00 14.40 5 -6 0 734.13 29.30 -5 -6 0 764.72 30.10 -5 6 0 740.73 32.50 -6 -6 0 13.30 13.90 6 -6 0 11.90 11.40 -6 6 0 29.40 15.60 -7 -6 0 0.90 14.20 7 -6 0 16.50 13.90 7 6 0 18.40 10.70 -7 6 0 14.30 16.10 -8 -6 0 227.68 22.40 8 -6 0 167.38 19.10 -8 6 0 187.68 23.50 8 6 0 206.18 17.40 -9 -6 0 111.99 21.00 9 -6 0 108.69 20.10 -9 6 0 115.59 23.10 9 6 0 94.79 16.00 10 -6 0 26.60 17.70 -10 -6 0 76.69 22.10 10 6 0 82.79 18.00 -10 6 0 79.49 22.50 -11 -6 0 -0.50 20.10 11 -6 0 12.40 19.10 11 6 0 -2.90 16.90 -11 6 0 -5.30 20.30 -12 -6 0 75.39 25.50 12 -6 0 79.29 23.20 12 6 0 89.99 20.70 -12 6 0 52.49 25.90 13 -6 0 -16.20 22.70 -13 6 0 54.39 26.50 13 6 0 28.60 20.90 14 -6 0 56.19 27.10 -14 6 0 109.69 30.40 0 -7 0 -7.20 9.60 1 -7 0 94.89 11.00 -1 -7 0 107.99 10.20 -2 -7 0 659.93 19.80 2 -7 0 650.93 24.40 -2 -7 0 626.84 25.90 -3 -7 0 38.40 12.30 3 -7 0 27.10 10.90 -3 7 0 51.49 14.50 -4 -7 0 29.90 12.90 4 -7 0 74.09 14.00 -4 7 0 73.69 16.40 5 -7 0 599.74 27.40 -5 -7 0 638.44 29.30 -5 7 0 656.93 31.90 6 -7 0 23.40 12.70 -6 -7 0 2.50 13.30 -6 7 0 18.40 15.10 -7 -7 0 542.45 30.40 7 -7 0 517.85 26.90 7 7 0 545.95 23.40 -7 7 0 526.85 32.00 -8 -7 0 98.79 19.20 8 -7 0 74.19 15.90 -8 7 0 70.09 19.90 8 7 0 96.29 13.80 9 -7 0 -26.20 14.70 -9 -7 0 7.30 17.10 9 7 0 0.40 12.80 -9 7 0 -21.90 18.40 -10 -7 0 130.19 24.30 10 -7 0 181.38 24.30 -10 7 0 219.78 28.00 10 7 0 150.18 20.40 11 -7 0 39.00 20.60 -11 -7 0 -8.90 20.00 -11 7 0 7.90 21.40 11 7 0 13.30 16.90 12 -7 0 34.00 22.50 -12 -7 0 15.80 22.90 -12 7 0 4.80 22.90 12 7 0 25.90 19.60 13 -7 0 15.40 24.10 -13 7 0 68.79 28.00 14 -7 0 56.69 27.10 -14 7 0 104.59 29.50 0 -8 0 748.33 25.20 1 -8 0 183.08 13.90 -1 -8 0 205.48 13.30 2 -8 0 46.30 11.90 -2 -8 0 83.39 14.20 -2 -8 0 49.00 9.00 -3 -8 0 25.70 12.30 3 -8 0 18.70 11.90 -3 8 0 14.40 14.40 4 -8 0 75.79 13.40 -4 -8 0 91.09 15.50 -4 8 0 71.69 16.80 5 -8 0 592.84 28.10 -5 -8 0 634.34 29.80 -5 8 0 639.84 32.30 -6 -8 0 -2.60 13.90 6 -8 0 17.50 13.80 -6 8 0 22.20 15.60 7 -8 0 -5.30 14.30 -7 -8 0 4.40 14.50 -7 8 0 3.30 16.40 -8 -8 0 30.70 17.20 8 -8 0 40.90 15.60 -8 8 0 26.90 17.90 8 8 0 -2.40 11.40 9 -8 0 -18.10 16.60 -9 -8 0 -3.40 17.40 -9 8 0 -5.20 18.90 9 8 0 2.10 13.20 10 -8 0 112.29 22.60 -10 -8 0 125.69 24.60 -10 8 0 133.19 24.80 10 8 0 170.48 19.50 11 -8 0 -6.10 20.00 -11 -8 0 20.80 22.10 -11 8 0 33.10 23.10 11 8 0 -11.80 16.20 12 -8 0 -29.20 20.50 -12 -8 0 7.70 23.10 -12 8 0 11.80 23.80 12 8 0 -23.80 18.10 13 -8 0 47.10 25.50 -13 8 0 28.00 25.80 14 -8 0 6.00 24.90 -14 8 0 -44.50 24.90 0 -9 0 14.20 10.30 -1 -9 0 378.76 17.70 1 -9 0 390.56 20.00 2 -9 0 307.37 17.90 -2 -9 0 302.17 15.30 -3 -9 0 25.30 13.60 -3 -9 0 34.60 9.50 3 -9 0 26.00 12.80 -3 9 0 47.50 16.20 4 -9 0 561.94 26.20 -4 -9 0 509.75 26.60 -4 9 0 501.65 29.70 -5 -9 0 485.25 28.20 5 -9 0 485.15 24.80 -5 9 0 576.84 31.80 6 -9 0 -17.00 11.40 -6 -9 0 28.90 14.70 -6 9 0 3.80 15.70 -7 -9 0 366.66 27.40 7 -9 0 381.26 26.80 -7 9 0 435.86 31.10 -8 -9 0 45.50 18.30 8 -9 0 25.90 17.00 -8 9 0 50.29 19.80 8 9 0 27.50 12.30 -9 -9 0 -11.60 18.00 9 -9 0 8.60 16.70 9 9 0 -8.80 12.80 -9 9 0 12.50 19.80 -10 -9 0 35.00 20.70 10 -9 0 52.09 20.50 -10 9 0 46.50 23.50 10 9 0 58.89 16.30 11 -9 0 7.70 20.60 -11 -9 0 20.50 21.90 11 9 0 -2.90 16.80 -11 9 0 33.00 23.30 12 -9 0 2.00 20.80 -12 -9 0 2.50 22.60 -12 9 0 44.80 25.70 13 -9 0 30.70 23.90 -13 9 0 75.69 28.80 14 -9 0 -6.60 24.20 -14 9 0 9.40 28.20 0 -10 0 766.02 26.80 -1 -10 0 79.19 11.10 1 -10 0 59.29 12.70 2 -10 0 572.04 24.70 -2 -10 0 578.54 20.60 -3 -10 0 1267.27 34.30 -3 -10 0 1336.67 42.10 3 -10 0 1380.86 40.40 -3 10 0 1358.16 45.70 4 -10 0 9.00 13.20 -4 -10 0 14.70 14.20 -4 10 0 10.50 15.20 -5 -10 0 43.20 15.00 5 -10 0 10.40 13.10 -5 10 0 26.70 17.50 -6 -10 0 43.60 15.60 6 -10 0 47.30 15.40 -6 10 0 27.00 18.40 7 -10 0 20.10 16.00 -7 -10 0 -1.10 15.30 -7 10 0 34.60 18.20 -8 -10 0 55.69 19.10 8 -10 0 85.79 19.90 8 10 0 64.89 13.90 -8 10 0 76.99 21.20 9 -10 0 102.79 21.90 -9 -10 0 127.49 22.60 -9 10 0 103.09 23.70 9 10 0 131.99 16.70 -10 -10 0 21.60 20.20 10 -10 0 0.80 18.20 -10 10 0 0.70 21.90 10 10 0 25.50 15.10 -11 -10 0 23.30 21.50 11 -10 0 79.79 21.50 -11 10 0 24.90 23.50 11 10 0 36.00 18.20 12 -10 0 95.69 25.10 -12 -10 0 172.18 29.30 -12 10 0 71.19 26.80 13 -10 0 -5.00 23.20 -13 10 0 38.60 25.90 14 -10 0 -1.90 25.50 -14 10 0 16.70 27.80 0 -11 0 -4.50 10.60 1 -11 0 43.30 11.90 -1 -11 0 72.49 11.20 2 -11 0 25.30 12.80 -2 -11 0 38.80 9.80 -3 -11 0 30.50 15.20 -3 -11 0 63.29 10.10 3 -11 0 55.39 13.80 4 -11 0 -2.30 12.90 -4 -11 0 9.50 14.30 -4 11 0 7.70 14.20 5 -11 0 174.28 18.90 -5 -11 0 122.89 18.80 -5 11 0 125.59 19.60 6 -11 0 87.09 17.30 -6 -11 0 109.29 18.50 -6 11 0 87.29 20.50 -7 -11 0 17.10 17.10 7 -11 0 42.80 16.50 -7 11 0 40.70 21.20 -8 -11 0 10.60 18.60 8 -11 0 12.20 15.20 -8 11 0 10.40 19.50 -9 -11 0 5.30 19.20 9 -11 0 25.00 18.60 -9 11 0 -9.80 20.90 9 11 0 0.10 12.80 -10 -11 0 -1.30 19.70 10 -11 0 3.90 17.00 -10 11 0 9.60 22.30 10 11 0 21.20 15.50 -11 -11 0 -11.20 20.60 11 -11 0 32.80 19.60 -11 11 0 -12.70 23.30 12 -11 0 5.20 22.70 -12 -11 0 -31.10 25.20 -12 11 0 19.70 23.90 13 -11 0 19.80 25.10 -13 11 0 13.90 26.30 14 -11 0 -43.80 24.50 -14 11 0 3.70 27.00 0 -12 0 1005.80 32.60 -1 -12 0 103.19 12.60 1 -12 0 81.89 14.30 -2 -12 0 59.29 10.70 2 -12 0 67.39 14.50 3 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-20 20.90 22.40 1 -13 -20 62.29 30.10 -1 -13 20 130.79 30.40 1 13 -20 71.19 27.00 4 -14 -20 40.30 28.60 3 -14 -20 8.50 27.80 3 14 -20 -31.00 25.10 2 -14 -20 -9.90 27.80 -2 -14 20 -10.30 27.20 2 14 -20 -14.00 23.10 8 0 -21 -21.60 21.20 -8 0 21 86.99 43.90 7 0 -21 -14.10 21.80 6 0 -21 8.10 23.00 5 0 -21 3.70 21.20 4 0 -21 -5.70 22.10 3 0 -21 5.70 22.70 2 0 -21 0.80 23.90 1 0 -21 44.40 26.30 0 0 -21 29.90 25.40 -1 0 -21 12.20 27.80 -8 -1 21 -15.80 25.90 8 -1 -21 -35.80 21.60 8 1 -21 19.80 22.50 7 -1 -21 84.09 25.00 7 1 -21 60.69 25.30 6 -1 -21 4.80 22.50 6 1 -21 -28.20 19.10 5 -1 -21 16.70 22.30 5 1 -21 -33.10 19.50 4 -1 -21 41.70 24.30 4 1 -21 62.79 25.60 3 -1 -21 9.00 22.80 3 1 -21 26.00 23.40 2 -1 -21 18.30 23.30 2 1 -21 28.80 24.90 1 -1 -21 12.50 23.00 1 1 -21 21.50 25.50 0 -1 -21 -34.30 25.40 0 1 -21 9.50 26.20 -1 -1 -21 38.30 27.40 -1 1 -21 47.80 26.70 8 -2 -21 37.40 24.40 -8 -2 21 64.49 28.10 8 2 -21 -5.00 21.30 7 -2 -21 7.80 24.00 7 2 -21 -21.50 20.80 6 -2 -21 19.60 23.30 6 2 -21 26.00 22.60 5 -2 -21 6.80 23.90 5 2 -21 -2.20 22.20 4 -2 -21 -18.60 22.70 4 2 -21 6.20 22.50 3 -2 -21 29.80 24.90 3 2 -21 0.60 21.40 2 -2 -21 46.40 26.30 2 2 -21 22.00 24.70 1 -2 -21 16.00 26.00 1 2 -21 41.50 27.70 0 -2 -21 21.20 26.20 0 2 -21 62.39 28.30 -1 -2 -21 5.40 27.80 -1 2 -21 4.30 26.30 -8 -3 21 21.20 26.20 8 -3 -21 -2.40 23.80 8 3 -21 8.60 22.10 7 -3 -21 -40.70 22.10 7 3 -21 -14.20 20.40 6 -3 -21 -25.10 21.60 6 3 -21 -2.80 20.70 5 -3 -21 38.00 24.80 5 3 -21 29.30 22.60 4 -3 -21 -14.70 22.40 4 3 -21 -19.60 20.30 3 -3 -21 -8.00 24.20 3 3 -21 19.70 24.10 2 -3 -21 -10.60 23.10 2 3 -21 -15.80 22.80 1 -3 -21 -6.70 23.40 1 3 -21 -21.20 24.60 0 -3 -21 34.70 27.40 0 3 -21 -2.60 26.00 -1 -3 -21 -35.90 23.70 -1 3 -21 37.10 28.00 7 -4 -21 -2.40 22.90 7 4 -21 -23.10 20.70 6 -4 -21 20.90 24.80 6 4 -21 56.49 23.60 5 -4 -21 18.60 23.30 5 4 -21 18.70 22.80 4 -4 -21 -14.20 23.70 4 4 -21 16.40 22.90 3 -4 -21 -12.30 23.40 3 4 -21 9.80 23.80 2 -4 -21 11.60 25.20 2 4 -21 6.30 24.70 1 -4 -21 -12.20 25.20 1 4 -21 17.20 25.10 0 -4 -21 19.90 23.10 0 4 -21 50.89 27.70 -1 -4 -21 25.50 27.60 -1 4 -21 -14.60 25.60 -7 -5 21 114.89 46.10 7 -5 -21 46.80 25.40 7 5 -21 48.30 23.40 6 -5 -21 43.40 25.00 6 5 -21 -4.30 21.40 5 -5 -21 31.00 25.10 5 5 -21 9.50 22.30 4 -5 -21 19.80 22.50 4 5 -21 53.29 24.90 3 -5 -21 59.09 24.60 3 5 -21 80.19 27.20 2 -5 -21 30.80 24.50 2 5 -21 14.10 25.40 1 -5 -21 35.30 27.10 1 5 -21 27.80 24.50 0 -5 -21 -0.70 25.80 0 5 -21 33.20 26.70 -1 -5 -21 41.80 30.00 -1 5 -21 9.40 26.60 -7 -6 21 20.60 26.80 7 -6 -21 -15.70 23.60 7 6 -21 26.90 22.00 6 -6 -21 -21.40 22.50 6 6 -21 -18.80 20.20 5 -6 -21 -12.10 23.50 5 6 -21 17.00 22.80 4 -6 -21 61.59 26.00 4 6 -21 11.70 22.60 3 -6 -21 22.40 25.90 3 6 -21 -4.80 22.80 2 -6 -21 -14.10 24.70 2 6 -21 4.10 22.60 1 -6 -21 3.30 25.10 1 6 -21 -24.10 24.30 0 -6 -21 0.50 26.20 0 6 -21 -28.70 23.00 -1 -6 -21 -2.60 27.50 -1 6 -21 70.69 29.00 -7 -7 21 16.90 26.70 7 -7 -21 10.10 25.10 6 -7 -21 -17.70 24.20 6 7 -21 -21.30 19.90 5 -7 -21 -18.20 23.60 5 7 -21 28.20 23.20 4 -7 -21 39.70 26.00 4 7 -21 54.89 25.20 3 -7 -21 -11.00 25.60 3 7 -21 31.80 24.60 2 -7 -21 -15.10 24.30 2 7 -21 47.30 25.50 1 -7 -21 -23.50 25.20 1 7 -21 -9.50 22.50 0 -7 -21 57.39 27.70 0 7 -21 8.80 25.90 6 -8 -21 -19.70 23.80 6 8 -21 45.50 24.40 5 -8 -21 77.29 28.40 5 8 -21 55.39 24.60 4 -8 -21 37.50 27.00 4 8 -21 3.40 21.80 3 -8 -21 24.80 26.40 3 8 -21 -13.20 21.90 2 -8 -21 71.79 27.50 2 8 -21 55.79 25.50 1 -8 -21 -42.50 24.60 1 8 -21 3.90 24.60 0 -8 -21 -8.10 25.50 0 8 -21 -14.50 24.10 6 -9 -21 18.00 26.50 5 -9 -21 -4.90 26.10 5 9 -21 -0.50 20.90 4 -9 -21 36.10 25.80 4 9 -21 5.30 23.40 3 -9 -21 25.50 26.60 3 9 -21 -12.00 21.50 2 -9 -21 0.00 25.30 2 9 -21 37.80 24.70 1 -9 -21 11.30 27.20 1 9 -21 1.80 24.60 5 -10 -21 32.10 26.50 5 10 -21 20.60 26.70 4 -10 -21 24.10 27.80 4 10 -21 -0.50 22.80 3 -10 -21 9.70 26.60 3 10 -21 -16.00 20.70 2 -10 -21 40.00 29.20 2 10 -21 18.90 24.80 3 -11 -21 32.20 28.30 5 0 -22 -3.40 22.70 4 0 -22 -12.00 22.20 3 0 -22 2.50 23.90 2 0 -22 5.80 24.40 1 0 -22 59.99 28.50 5 -1 -22 9.40 22.20 5 1 -22 1.50 22.40 4 -1 -22 -14.00 23.40 4 1 -22 -13.30 21.90 3 -1 -22 0.20 25.30 3 1 -22 15.90 25.00 2 -1 -22 1.30 25.00 2 1 -22 19.90 26.30 1 -1 -22 -26.90 22.90 1 1 -22 -18.90 26.20 5 -2 -22 -19.20 22.60 5 2 -22 -1.20 22.10 4 -2 -22 -27.50 23.20 4 2 -22 7.70 23.10 3 -2 -22 11.70 23.40 3 2 -22 7.30 24.50 2 -2 -22 -27.60 24.60 2 2 -22 13.80 25.90 5 -3 -22 17.90 24.30 5 3 -22 4.40 23.90 4 -3 -22 -19.60 22.00 4 3 -22 17.90 25.00 3 -3 -22 21.20 25.20 3 3 -22 7.00 24.80 2 -3 -22 -17.20 24.00 2 3 -22 -3.30 25.50 4 -4 -22 17.90 25.90 4 4 -22 3.90 24.50 3 -4 -22 29.80 25.20 3 4 -22 -6.90 25.10 2 -4 -22 -21.40 23.80 2 4 -22 1.60 25.50 4 -5 -22 16.80 25.40 4 5 -22 -21.50 24.80 3 -5 -22 17.70 25.70 3 5 -22 13.00 24.50 _computing_structure_solution 'SHELXT 2014/4 (Sheldrick, 2014)' ; _shelx_hkl_checksum 64545 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 C1 C 0.2141(6) 0.5067(3) 0.7112(4) 0.048(2) Uani 1 1 d . . H1A H 0.1913 0.5061 0.7612 0.058 Uiso 1 1 calc R U H1B H 0.2834 0.5273 0.7174 0.058 Uiso 1 1 calc R U C2 C 0.5378(4) 0.4812(2) 0.7630(3) 0.0267(14) Uani 1 1 d . . C3 C 0.5432(5) 0.4836(3) 0.6845(3) 0.0339(16) Uani 1 1 d . . C4 C 0.5502(5) 0.4355(3) 0.6384(3) 0.0396(17) Uani 1 1 d . . H4 H 0.5428 0.4052 0.6715 0.047 Uiso 1 1 calc R U C5 C 0.6620(6) 0.4314(3) 0.6154(4) 0.058(2) Uani 1 1 d . . H5A H 0.6685 0.4592 0.5794 0.088 Uiso 1 1 calc R U H5B H 0.6671 0.3981 0.5907 0.088 Uiso 1 1 calc R U H5C H 0.7225 0.4344 0.6613 0.088 Uiso 1 1 calc R U C6 C 0.4550(6) 0.4328(3) 0.5661(4) 0.062(2) Uani 1 1 d . . H6A H 0.3830 0.4359 0.5810 0.094 Uiso 1 1 calc R U H6B H 0.4584 0.3997 0.5402 0.094 Uiso 1 1 calc R U H6C H 0.4631 0.4610 0.5312 0.094 Uiso 1 1 calc R U C7 C 0.5417(5) 0.5330(3) 0.6516(4) 0.0407(18) Uani 1 1 d . . H7 H 0.5463 0.5356 0.5993 0.049 Uiso 1 1 calc R U C8 C 0.5340(5) 0.5767(3) 0.6906(4) 0.0427(18) Uani 1 1 d . . H8 H 0.5336 0.6092 0.6661 0.051 Uiso 1 1 calc R U C9 C 0.5269(5) 0.5739(3) 0.7662(4) 0.0431(18) Uani 1 1 d . . H9 H 0.5217 0.6048 0.7937 0.052 Uiso 1 1 calc R U C10 C 0.5270(5) 0.5266(3) 0.8038(3) 0.0312(16) Uani 1 1 d . . C11 C 0.3968(5) 0.5162(3) 0.8928(4) 0.054(2) Uani 1 1 d . . H11A H 0.3506 0.5451 0.8689 0.082 Uiso 1 1 calc R U H11B H 0.3934 0.5138 0.9470 0.082 Uiso 1 1 calc R U H11C H 0.3690 0.4842 0.8664 0.082 Uiso 1 1 calc R U C12 C 0.5163(5) 0.5249(3) 0.8866(3) 0.0384(17) Uani 1 1 d . . H12 H 0.5602 0.4944 0.9109 0.046 Uiso 1 1 calc R U C13 C 0.5644(8) 0.5722(3) 0.9336(4) 0.083(3) Uani 1 1 d . . H13A H 0.6419 0.5774 0.9294 0.124 Uiso 1 1 calc R U H13B H 0.5620 0.5669 0.9876 0.124 Uiso 1 1 calc R U H13C H 0.5201 0.6027 0.9138 0.124 Uiso 1 1 calc R U C14 C 0.6086(4) 0.4067(2) 0.8461(3) 0.0207(12) Uani 1 1 d . . C15 C 0.7348(4) 0.4240(2) 0.8697(3) 0.0281(15) Uani 1 1 d . . C16 C 0.7676(5) 0.4744(3) 0.8372(4) 0.0396(17) Uani 1 1 d . . H16A H 0.8488 0.4785 0.8517 0.059 Uiso 1 1 calc R U H16B H 0.7316 0.5031 0.8579 0.059 Uiso 1 1 calc R U H16C H 0.7435 0.4740 0.7811 0.059 Uiso 1 1 calc R U C17 C 0.7708(5) 0.4289(3) 0.9583(3) 0.0342(16) Uani 1 1 d . . H17A H 0.7496 0.3975 0.9823 0.051 Uiso 1 1 calc R U H17B H 0.7336 0.4587 0.9754 0.051 Uiso 1 1 calc R U H17C H 0.8519 0.4335 0.9733 0.051 Uiso 1 1 calc R U C18 C 0.8053(5) 0.3818(3) 0.8436(4) 0.0427(18) Uani 1 1 d . . H18A H 0.7872 0.3798 0.7874 0.064 Uiso 1 1 calc R U H18B H 0.7893 0.3487 0.8651 0.064 Uiso 1 1 calc R U H18C H 0.8846 0.3901 0.8616 0.064 Uiso 1 1 calc R U C19 C 0.5851(4) 0.3606(2) 0.8794(3) 0.0204(13) Uani 1 1 d . . H19 H 0.6469 0.3468 0.9153 0.024 Uiso 1 1 calc R U C20 C 0.4886(4) 0.3310(2) 0.8704(3) 0.0185(13) Uani 1 1 d . . C21 C 0.5029(5) 0.2797(2) 0.9171(3) 0.0228(13) Uani 1 1 d . . C22 C 0.5928(5) 0.2465(2) 0.8922(3) 0.0357(16) Uani 1 1 d . . H22A H 0.6038 0.2147 0.9226 0.054 Uiso 1 1 calc R U H22B H 0.6631 0.2657 0.9006 0.054 Uiso 1 1 calc R U H22C H 0.5685 0.2379 0.8376 0.054 Uiso 1 1 calc R U C23 C 0.5428(5) 0.2935(3) 1.0036(3) 0.0341(16) Uani 1 1 d . . H23A H 0.4869 0.3154 1.0196 0.051 Uiso 1 1 calc R U H23B H 0.6140 0.3120 1.0115 0.051 Uiso 1 1 calc R U H23C H 0.5526 0.2618 1.0342 0.051 Uiso 1 1 calc R U C24 C 0.4011(5) 0.2459(2) 0.9121(3) 0.0325(16) Uani 1 1 d . . H24A H 0.3740 0.2345 0.8589 0.049 Uiso 1 1 calc R U H24B H 0.3424 0.2655 0.9287 0.049 Uiso 1 1 calc R U H24C H 0.4210 0.2158 0.9454 0.049 Uiso 1 1 calc R U C25 C 0.2881(4) 0.3208(2) 0.8037(3) 0.0238(14) Uani 1 1 d . . C26 C 0.2675(5) 0.2879(2) 0.7392(3) 0.0306(15) Uani 1 1 d . . C27 C 0.3359(7) 0.3039(3) 0.6191(4) 0.060(2) Uani 1 1 d . . H27A H 0.2666 0.2912 0.5861 0.090 Uiso 1 1 calc R U H27B H 0.3981 0.2979 0.5939 0.090 Uiso 1 1 calc R U H27C H 0.3290 0.3409 0.6279 0.090 Uiso 1 1 calc R U C28 C 0.3578(5) 0.2754(3) 0.6964(3) 0.0342(16) Uani 1 1 d . . H28 H 0.4302 0.2883 0.7279 0.041 Uiso 1 1 calc R U C29 C 0.3706(6) 0.2178(3) 0.6842(4) 0.0440(18) Uani 1 1 d . . H29A H 0.3852 0.2002 0.7340 0.066 Uiso 1 1 calc R U H29B H 0.4332 0.2119 0.6593 0.066 Uiso 1 1 calc R U H29C H 0.3019 0.2043 0.6516 0.066 Uiso 1 1 calc R U C30 C 0.1600(5) 0.2693(3) 0.7121(4) 0.0428(19) Uani 1 1 d . . H30 H 0.1453 0.2476 0.6681 0.051 Uiso 1 1 calc R U C31 C 0.0747(5) 0.2817(3) 0.7474(4) 0.049(2) Uani 1 1 d . . H31 H 0.0019 0.2684 0.7280 0.059 Uiso 1 1 calc R U C32 C 0.0946(5) 0.3134(3) 0.8112(3) 0.0366(17) Uani 1 1 d . . H32 H 0.0352 0.3219 0.8352 0.044 Uiso 1 1 calc R U C33 C 0.2010(4) 0.3330(2) 0.8405(3) 0.0256(14) Uani 1 1 d . . C34 C 0.2193(5) 0.3684(2) 0.9103(3) 0.0286(15) Uani 1 1 d . . H34 H 0.3015 0.3741 0.9280 0.034 Uiso 1 1 calc R U C35 C 0.1772(6) 0.3442(3) 0.9768(3) 0.0433(18) Uani 1 1 d . . H35A H 0.0963 0.3391 0.9614 0.065 Uiso 1 1 calc R U H35B H 0.1943 0.3672 1.0215 0.065 Uiso 1 1 calc R U H35C H 0.2141 0.3110 0.9901 0.065 Uiso 1 1 calc R U C36 C 0.1653(5) 0.4203(2) 0.8891(4) 0.0419(18) Uani 1 1 d . . H36A H 0.1945 0.4354 0.8472 0.063 Uiso 1 1 calc R U H36B H 0.1821 0.4431 0.9339 0.063 Uiso 1 1 calc R U H36C H 0.0843 0.4159 0.8726 0.063 Uiso 1 1 calc R U C37 C 0.1236(5) 0.5303(3) 0.6508(3) 0.0353(16) Uani 1 1 d . . C38 C 0.0067(5) 0.5188(3) 0.6407(4) 0.0389(17) Uani 1 1 d . . C39 C -0.0441(6) 0.4830(3) 0.6882(4) 0.050(2) Uani 1 1 d . . H39A H -0.1162 0.4966 0.6938 0.075 Uiso 1 1 calc R U H39B H 0.0057 0.4794 0.7390 0.075 Uiso 1 1 calc R U H39C H -0.0551 0.4492 0.6631 0.075 Uiso 1 1 calc R U C40 C -0.0503(5) 0.5477(3) 0.5763(4) 0.0380(17) Uani 1 1 d . . C41 C -0.1744(5) 0.5472(3) 0.5418(4) 0.053(2) Uani 1 1 d . . H41A H -0.1907 0.5216 0.5005 0.079 Uiso 1 1 calc R U H41B H -0.1980 0.5813 0.5209 0.079 Uiso 1 1 calc R U H41C H -0.2149 0.5383 0.5817 0.079 Uiso 1 1 calc R U C42 C 0.0291(5) 0.5769(3) 0.5465(3) 0.0397(18) Uani 1 1 d . . C43 C 0.0046(7) 0.6108(3) 0.4765(4) 0.062(2) Uani 1 1 d . . H43A H 0.0743 0.6260 0.4686 0.093 Uiso 1 1 calc R U H43B H -0.0467 0.6383 0.4839 0.093 Uiso 1 1 calc R U H43C H -0.0297 0.5902 0.4315 0.093 Uiso 1 1 calc R U C44 C 0.1363(5) 0.5660(3) 0.5927(4) 0.0397(17) Uani 1 1 d . . C45 C 0.2456(5) 0.5863(3) 0.5827(4) 0.055(2) Uani 1 1 d . . H45A H 0.2941 0.5927 0.6333 0.083 Uiso 1 1 calc R U H45B H 0.2338 0.6185 0.5535 0.083 Uiso 1 1 calc R U H45C H 0.2808 0.5609 0.5549 0.083 Uiso 1 1 calc R U C46 C -0.0669(6) 0.6257(3) 0.7247(4) 0.0454(19) Uani 1 1 d . . C47 C -0.1745(6) 0.6055(3) 0.7381(5) 0.083(3) Uani 1 1 d . . H47A H -0.2023 0.6286 0.7732 0.125 Uiso 1 1 calc R U H47B H -0.1629 0.5710 0.7608 0.125 Uiso 1 1 calc R U H47C H -0.2292 0.6037 0.6891 0.125 Uiso 1 1 calc R U C48 C -0.0540(5) 0.6610(3) 0.6664(4) 0.0440(19) Uani 1 1 d . . C49 C -0.1472(6) 0.6842(3) 0.6074(5) 0.076(3) Uani 1 1 d . . H49A H -0.1712 0.7165 0.6272 0.115 Uiso 1 1 calc R U H49B H -0.2101 0.6601 0.5961 0.115 Uiso 1 1 calc R U H49C H -0.1211 0.6911 0.5602 0.115 Uiso 1 1 calc R U C50 C 0.0595(5) 0.6731(3) 0.6758(3) 0.0359(16) Uani 1 1 d . . C51 C 0.1101(6) 0.7095(3) 0.6299(4) 0.056(2) Uani 1 1 d . . H51A H 0.0706 0.7074 0.5759 0.084 Uiso 1 1 calc R U H51B H 0.1888 0.7007 0.6344 0.084 Uiso 1 1 calc R U H51C H 0.1043 0.7446 0.6488 0.084 Uiso 1 1 calc R U C52 C 0.1199(5) 0.6445(3) 0.7402(4) 0.0400(17) Uani 1 1 d . . C53 C 0.2433(5) 0.6453(3) 0.7723(4) 0.059(2) Uani 1 1 d . . H53A H 0.2600 0.6685 0.8167 0.088 Uiso 1 1 calc R U H53B H 0.2815 0.6575 0.7328 0.088 Uiso 1 1 calc R U H53C H 0.2691 0.6105 0.7883 0.088 Uiso 1 1 calc R U C54 C 0.0400(6) 0.6158(3) 0.7698(4) 0.0433(18) Uani 1 1 d . . C55 C 0.0641(8) 0.5798(3) 0.8384(4) 0.075(3) Uani 1 1 d . . H55A H 0.1426 0.5692 0.8485 0.112 Uiso 1 1 calc R U H55B H 0.0161 0.5494 0.8274 0.112 Uiso 1 1 calc R U H55C H 0.0493 0.5977 0.8835 0.112 Uiso 1 1 calc R U C56 C 0.0841(6) 0.7083(3) 0.9368(4) 0.056(2) Uani 1 1 d . . H56A H 0.0428 0.6954 0.8870 0.084 Uiso 1 1 calc R U H56B H 0.0325 0.7132 0.9711 0.084 Uiso 1 1 calc R U H56C H 0.1417 0.6833 0.9596 0.084 Uiso 1 1 calc R U C57 C 0.1377(6) 0.7584(3) 0.9258(4) 0.047(2) Uani 1 1 d . . H57A H 0.0797 0.7851 0.9096 0.057 Uiso 1 1 calc R U H57B H 0.1868 0.7696 0.9748 0.057 Uiso 1 1 calc R U C58 C 0.2573(6) 0.7977(3) 0.8580(4) 0.050(2) Uani 1 1 d . . H58A H 0.3032 0.8097 0.9076 0.060 Uiso 1 1 calc R U H58B H 0.2027 0.8250 0.8375 0.060 Uiso 1 1 calc R U C59 C 0.3311(6) 0.7875(3) 0.8022(4) 0.055(2) Uani 1 1 d . . H59A H 0.3819 0.7590 0.8212 0.082 Uiso 1 1 calc R U H59B H 0.3747 0.8185 0.7974 0.082 Uiso 1 1 calc R U H59C H 0.2848 0.7785 0.7519 0.082 Uiso 1 1 calc R U Co1 Co 0.03370(6) 0.59675(4) 0.65740(4) 0.0330(2) Uani 1 1 d . . N1 N 0.5291(4) 0.43213(19) 0.7971(2) 0.0234(11) Uani 1 1 d . . N2 N 0.3928(3) 0.34696(18) 0.8248(2) 0.0209(11) Uani 1 1 d . . Ni01 Ni 0.37866(6) 0.40854(3) 0.76566(4) 0.0236(2) Uani 1 1 d . . O1 O 0.2005(4) 0.75238(18) 0.8694(2) 0.0395(11) Uani 1 1 d . . S1 S 0.23887(15) 0.43962(8) 0.68065(10) 0.0494(5) Uani 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 C1 0.042(4) 0.056(5) 0.040(4) -0.004(4) -0.004(3) 0.012(4) C2 0.017(3) 0.033(4) 0.028(3) 0.008(3) 0.000(3) -0.004(3) C3 0.029(3) 0.041(5) 0.031(4) 0.003(3) 0.004(3) -0.010(3) C4 0.039(4) 0.051(5) 0.030(4) 0.010(3) 0.009(3) -0.010(4) C5 0.063(5) 0.065(6) 0.053(5) -0.001(4) 0.025(4) -0.012(5) C6 0.075(6) 0.080(6) 0.027(4) 0.008(4) 0.001(4) -0.008(5) C7 0.036(4) 0.055(5) 0.027(4) 0.018(4) -0.001(3) -0.008(4) C8 0.035(4) 0.033(5) 0.056(5) 0.013(4) 0.002(3) -0.015(3) C9 0.025(3) 0.033(5) 0.065(5) 0.005(4) -0.006(3) -0.003(3) C10 0.023(3) 0.027(4) 0.039(4) 0.012(3) -0.004(3) -0.005(3) C11 0.045(4) 0.080(6) 0.036(4) -0.001(4) 0.004(3) 0.020(4) C12 0.048(4) 0.036(4) 0.024(3) -0.004(3) -0.007(3) 0.004(4) C13 0.121(8) 0.060(6) 0.055(5) -0.023(4) -0.006(5) -0.013(6) C14 0.016(3) 0.029(4) 0.018(3) -0.004(3) 0.003(2) 0.000(3) C15 0.019(3) 0.043(5) 0.021(3) 0.002(3) 0.000(2) -0.005(3) C16 0.025(3) 0.048(5) 0.044(4) 0.009(3) 0.003(3) -0.012(3) C17 0.023(3) 0.044(5) 0.032(3) 0.003(3) -0.002(3) 0.001(3) C18 0.023(3) 0.060(5) 0.047(4) -0.008(4) 0.011(3) -0.008(3) C19 0.014(3) 0.025(4) 0.021(3) 0.008(3) 0.001(2) 0.006(3) C20 0.020(3) 0.022(4) 0.015(3) -0.001(2) 0.008(2) 0.007(3) C21 0.026(3) 0.024(4) 0.017(3) 0.004(3) 0.004(2) 0.003(3) C22 0.038(4) 0.025(4) 0.044(4) 0.008(3) 0.009(3) 0.008(3) C23 0.036(4) 0.036(4) 0.029(3) 0.005(3) 0.003(3) -0.001(3) C24 0.034(4) 0.032(4) 0.031(3) 0.011(3) 0.005(3) -0.004(3) C25 0.019(3) 0.023(4) 0.026(3) 0.003(3) -0.002(2) -0.002(3) C26 0.027(3) 0.038(4) 0.025(3) -0.005(3) 0.002(3) -0.009(3) C27 0.077(6) 0.068(6) 0.039(4) 0.005(4) 0.022(4) -0.006(5) C28 0.037(4) 0.036(4) 0.027(3) -0.004(3) 0.004(3) -0.005(3) C29 0.052(4) 0.042(5) 0.040(4) -0.009(3) 0.016(3) -0.002(4) C30 0.039(4) 0.054(5) 0.030(4) -0.012(3) -0.005(3) -0.017(4) C31 0.025(4) 0.066(6) 0.049(4) -0.010(4) -0.007(3) -0.017(4) C32 0.029(4) 0.043(5) 0.036(4) -0.004(3) 0.003(3) -0.001(3) C33 0.019(3) 0.026(4) 0.029(3) 0.002(3) 0.002(3) -0.008(3) C34 0.021(3) 0.035(4) 0.029(3) 0.000(3) 0.004(3) 0.000(3) C35 0.050(4) 0.054(5) 0.031(4) 0.005(3) 0.019(3) -0.001(4) C36 0.037(4) 0.045(5) 0.048(4) -0.005(3) 0.017(3) -0.001(3) C37 0.029(3) 0.038(4) 0.035(4) 0.000(3) -0.001(3) 0.013(3) C38 0.034(4) 0.043(5) 0.036(4) 0.008(3) -0.001(3) -0.001(3) C39 0.055(5) 0.043(5) 0.051(5) 0.010(4) 0.011(4) -0.002(4) C40 0.034(4) 0.027(4) 0.049(4) 0.005(3) -0.001(3) -0.004(3) C41 0.038(4) 0.057(6) 0.051(5) 0.006(4) -0.018(3) -0.010(4) C42 0.039(4) 0.043(5) 0.032(4) 0.000(3) -0.002(3) -0.002(3) C43 0.082(6) 0.064(6) 0.035(4) 0.010(4) 0.002(4) -0.011(5) C44 0.034(4) 0.044(5) 0.038(4) -0.007(3) 0.001(3) -0.006(3) C45 0.039(4) 0.079(6) 0.053(4) -0.022(4) 0.022(3) -0.010(4) C46 0.037(4) 0.045(5) 0.059(5) -0.001(4) 0.021(4) -0.006(4) C47 0.064(5) 0.070(7) 0.132(8) -0.021(6) 0.059(6) -0.015(5) C48 0.031(4) 0.045(5) 0.051(5) -0.003(4) -0.001(3) -0.001(4) C49 0.054(5) 0.062(6) 0.096(7) -0.002(5) -0.021(5) 0.023(5) C50 0.040(4) 0.035(4) 0.033(4) 0.009(3) 0.008(3) 0.000(3) C51 0.072(5) 0.053(5) 0.048(5) 0.006(4) 0.020(4) -0.002(5) C52 0.031(4) 0.043(5) 0.041(4) -0.008(3) -0.003(3) 0.007(4) C53 0.041(4) 0.059(6) 0.064(5) -0.015(4) -0.016(4) 0.008(4) C54 0.064(5) 0.033(4) 0.035(4) -0.002(3) 0.015(4) 0.003(4) C55 0.130(8) 0.060(6) 0.039(5) 0.010(4) 0.031(5) 0.004(6) C56 0.054(5) 0.062(6) 0.058(5) 0.014(4) 0.024(4) 0.003(4) C57 0.041(4) 0.065(6) 0.037(4) 0.000(4) 0.009(3) 0.008(4) C58 0.048(4) 0.057(6) 0.044(4) 0.006(4) 0.007(4) 0.000(4) C59 0.052(5) 0.071(6) 0.045(4) 0.002(4) 0.018(4) -0.009(4) Co1 0.0251(4) 0.0415(6) 0.0311(5) -0.0006(4) 0.0031(4) -0.0024(5) N1 0.024(3) 0.026(3) 0.019(2) 0.004(2) 0.002(2) -0.003(2) N2 0.015(2) 0.027(3) 0.019(2) -0.002(2) 0.001(2) 0.001(2) Ni01 0.0193(4) 0.0291(5) 0.0204(4) 0.0042(4) -0.0004(3) -0.0002(4) O1 0.039(3) 0.046(3) 0.034(3) 0.000(2) 0.009(2) 0.004(2) S1 0.0446(10) 0.0650(14) 0.0311(9) -0.0021(9) -0.0083(8) 0.0231(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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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 C37 C1 S1 108.2(4) C37 C1 H1A 110.0 S1 C1 H1A 110.0 C37 C1 H1B 110.0 S1 C1 H1B 110.0 H1A C1 H1B 108.4 C10 C2 C3 120.2(6) C10 C2 N1 120.2(5) C3 C2 N1 119.0(6) C7 C3 C2 116.9(6) C7 C3 C4 121.6(6) C2 C3 C4 121.5(6) C3 C4 C5 111.6(5) C3 C4 C6 111.8(6) C5 C4 C6 109.6(5) C3 C4 H4 107.9 C5 C4 H4 107.9 C6 C4 H4 107.9 C4 C5 H5A 109.5 C4 C5 H5B 109.5 H5A C5 H5B 109.5 C4 C5 H5C 109.5 H5A C5 H5C 109.5 H5B C5 H5C 109.5 C4 C6 H6A 109.5 C4 C6 H6B 109.5 H6A C6 H6B 109.5 C4 C6 H6C 109.5 H6A C6 H6C 109.5 H6B C6 H6C 109.5 C8 C7 C3 123.3(6) C8 C7 H7 118.4 C3 C7 H7 118.4 C7 C8 C9 119.3(6) C7 C8 H8 120.4 C9 C8 H8 120.4 C8 C9 C10 121.7(7) C8 C9 H9 119.2 C10 C9 H9 119.2 C9 C10 C2 118.5(6) C9 C10 C12 120.2(6) C2 C10 C12 121.3(5) C12 C11 H11A 109.5 C12 C11 H11B 109.5 H11A C11 H11B 109.5 C12 C11 H11C 109.5 H11A C11 H11C 109.5 H11B C11 H11C 109.5 C11 C12 C10 111.6(5) C11 C12 C13 110.1(6) C10 C12 C13 113.9(6) C11 C12 H12 106.9 C10 C12 H12 106.9 C13 C12 H12 106.9 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 N1 C14 C19 120.9(5) N1 C14 C15 124.7(5) C19 C14 C15 114.4(5) C16 C15 C18 106.6(5) C16 C15 C17 106.1(5) C18 C15 C17 108.3(5) C16 C15 C14 118.0(5) C18 C15 C14 107.7(5) C17 C15 C14 109.8(4) C15 C16 H16A 109.5 C15 C16 H16B 109.5 H16A C16 H16B 109.5 C15 C16 H16C 109.5 H16A C16 H16C 109.5 H16B C16 H16C 109.5 C15 C17 H17A 109.5 C15 C17 H17B 109.5 H17A C17 H17B 109.5 C15 C17 H17C 109.5 H17A C17 H17C 109.5 H17B C17 H17C 109.5 C15 C18 H18A 109.5 C15 C18 H18B 109.5 H18A C18 H18B 109.5 C15 C18 H18C 109.5 H18A C18 H18C 109.5 H18B C18 H18C 109.5 C20 C19 C14 132.5(5) C20 C19 H19 113.8 C14 C19 H19 113.8 N2 C20 C19 120.8(5) N2 C20 C21 124.7(5) C19 C20 C21 114.6(4) C24 C21 C22 107.0(5) C24 C21 C23 105.6(5) C22 C21 C23 109.0(4) C24 C21 C20 117.9(4) C22 C21 C20 109.1(5) C23 C21 C20 108.0(5) C21 C22 H22A 109.5 C21 C22 H22B 109.5 H22A C22 H22B 109.5 C21 C22 H22C 109.5 H22A C22 H22C 109.5 H22B C22 H22C 109.5 C21 C23 H23A 109.5 C21 C23 H23B 109.5 H23A C23 H23B 109.5 C21 C23 H23C 109.5 H23A C23 H23C 109.5 H23B C23 H23C 109.5 C21 C24 H24A 109.5 C21 C24 H24B 109.5 H24A C24 H24B 109.5 C21 C24 H24C 109.5 H24A C24 H24C 109.5 H24B C24 H24C 109.5 C33 C25 C26 119.8(5) C33 C25 N2 120.1(5) C26 C25 N2 119.5(5) C30 C26 C25 118.8(6) C30 C26 C28 119.6(5) C25 C26 C28 121.5(5) C28 C27 H27A 109.5 C28 C27 H27B 109.5 H27A C27 H27B 109.5 C28 C27 H27C 109.5 H27A C27 H27C 109.5 H27B C27 H27C 109.5 C26 C28 C29 113.2(5) C26 C28 C27 110.2(5) C29 C28 C27 110.4(5) C26 C28 H28 107.6 C29 C28 H28 107.6 C27 C28 H28 107.6 C28 C29 H29A 109.5 C28 C29 H29B 109.5 H29A C29 H29B 109.5 C28 C29 H29C 109.5 H29A C29 H29C 109.5 H29B C29 H29C 109.5 C31 C30 C26 121.4(6) C31 C30 H30 119.3 C26 C30 H30 119.3 C30 C31 C32 120.0(6) C30 C31 H31 120.0 C32 C31 H31 120.0 C31 C32 C33 120.7(6) C31 C32 H32 119.7 C33 C32 H32 119.7 C32 C33 C25 119.2(5) C32 C33 C34 119.1(5) C25 C33 C34 121.7(5) C36 C34 C33 110.8(5) C36 C34 C35 110.8(5) C33 C34 C35 111.8(5) C36 C34 H34 107.8 C33 C34 H34 107.8 C35 C34 H34 107.8 C34 C35 H35A 109.5 C34 C35 H35B 109.5 H35A C35 H35B 109.5 C34 C35 H35C 109.5 H35A C35 H35C 109.5 H35B C35 H35C 109.5 C34 C36 H36A 109.5 C34 C36 H36B 109.5 H36A C36 H36B 109.5 C34 C36 H36C 109.5 H36A C36 H36C 109.5 H36B C36 H36C 109.5 C44 C37 C38 107.9(5) C44 C37 C1 127.4(6) C38 C37 C1 124.6(6) C44 C37 Co1 69.0(4) C38 C37 Co1 69.4(4) C1 C37 Co1 128.4(5) C40 C38 C37 107.1(6) C40 C38 C39 126.8(6) C37 C38 C39 126.1(6) C40 C38 Co1 68.5(4) C37 C38 Co1 69.8(4) C39 C38 Co1 127.4(5) C38 C39 H39A 109.5 C38 C39 H39B 109.5 H39A C39 H39B 109.5 C38 C39 H39C 109.5 H39A C39 H39C 109.5 H39B C39 H39C 109.5 C38 C40 C42 109.1(5) C38 C40 C41 126.6(6) C42 C40 C41 124.3(6) C38 C40 Co1 70.8(4) C42 C40 Co1 69.6(4) C41 C40 Co1 127.2(5) C40 C41 H41A 109.5 C40 C41 H41B 109.5 H41A C41 H41B 109.5 C40 C41 H41C 109.5 H41A C41 H41C 109.5 H41B C41 H41C 109.5 C44 C42 C40 107.4(6) C44 C42 C43 126.2(6) C40 C42 C43 126.3(6) C44 C42 Co1 70.2(4) C40 C42 Co1 69.3(4) C43 C42 Co1 128.2(5) C42 C43 H43A 109.5 C42 C43 H43B 109.5 H43A C43 H43B 109.5 C42 C43 H43C 109.5 H43A C43 H43C 109.5 H43B C43 H43C 109.5 C42 C44 C37 108.5(6) C42 C44 C45 127.3(6) C37 C44 C45 124.2(6) C42 C44 Co1 69.1(4) C37 C44 Co1 70.4(4) C45 C44 Co1 127.8(5) C44 C45 H45A 109.5 C44 C45 H45B 109.5 H45A C45 H45B 109.5 C44 C45 H45C 109.5 H45A C45 H45C 109.5 H45B C45 H45C 109.5 C54 C46 C48 107.3(6) C54 C46 C47 126.5(7) C48 C46 C47 126.1(7) C54 C46 Co1 70.1(4) C48 C46 Co1 68.2(4) C47 C46 Co1 129.5(6) C46 C47 H47A 109.5 C46 C47 H47B 109.5 H47A C47 H47B 109.5 C46 C47 H47C 109.5 H47A C47 H47C 109.5 H47B C47 H47C 109.5 C50 C48 C46 108.9(6) C50 C48 C49 125.4(7) C46 C48 C49 125.6(7) C50 C48 Co1 70.1(4) C46 C48 Co1 70.8(4) C49 C48 Co1 128.0(5) C48 C49 H49A 109.5 C48 C49 H49B 109.5 H49A C49 H49B 109.5 C48 C49 H49C 109.5 H49A C49 H49C 109.5 H49B C49 H49C 109.5 C48 C50 C52 107.9(6) C48 C50 C51 127.3(6) C52 C50 C51 124.8(6) C48 C50 Co1 69.2(4) C52 C50 Co1 69.9(4) C51 C50 Co1 127.4(5) C50 C51 H51A 109.5 C50 C51 H51B 109.5 H51A C51 H51B 109.5 C50 C51 H51C 109.5 H51A C51 H51C 109.5 H51B C51 H51C 109.5 C54 C52 C50 106.9(6) C54 C52 C53 126.0(7) C50 C52 C53 127.1(7) C54 C52 Co1 70.1(4) C50 C52 Co1 68.8(4) C53 C52 Co1 127.4(5) C52 C53 H53A 109.5 C52 C53 H53B 109.5 H53A C53 H53B 109.5 C52 C53 H53C 109.5 H53A C53 H53C 109.5 H53B C53 H53C 109.5 C46 C54 C52 109.0(6) C46 C54 C55 124.6(7) C52 C54 C55 126.4(7) C46 C54 Co1 69.7(4) C52 C54 Co1 69.2(4) C55 C54 Co1 126.8(5) C54 C55 H55A 109.5 C54 C55 H55B 109.5 H55A C55 H55B 109.5 C54 C55 H55C 109.5 H55A C55 H55C 109.5 H55B C55 H55C 109.5 C57 C56 H56A 109.5 C57 C56 H56B 109.5 H56A C56 H56B 109.5 C57 C56 H56C 109.5 H56A C56 H56C 109.5 H56B C56 H56C 109.5 O1 C57 C56 108.9(6) O1 C57 H57A 109.9 C56 C57 H57A 109.9 O1 C57 H57B 109.9 C56 C57 H57B 109.9 H57A C57 H57B 108.3 O1 C58 C59 109.8(6) O1 C58 H58A 109.7 C59 C58 H58A 109.7 O1 C58 H58B 109.7 C59 C58 H58B 109.7 H58A C58 H58B 108.2 C58 C59 H59A 109.5 C58 C59 H59B 109.5 H59A C59 H59B 109.5 C58 C59 H59C 109.5 H59A C59 H59C 109.5 H59B C59 H59C 109.5 C48 Co1 C50 40.7(3) C48 Co1 C40 112.3(3) C50 Co1 C40 140.1(3) C48 Co1 C42 112.7(3) C50 Co1 C42 112.1(3) C40 Co1 C42 41.1(3) C48 Co1 C52 68.9(3) C50 Co1 C52 41.3(2) C40 Co1 C52 178.6(3) C42 Co1 C52 139.3(3) C48 Co1 C46 41.0(3) C50 Co1 C46 68.7(3) C40 Co1 C46 111.8(3) C42 Co1 C46 140.6(3) C52 Co1 C46 68.7(3) C48 Co1 C44 140.8(3) C50 Co1 C44 112.3(3) C40 Co1 C44 68.5(3) C42 Co1 C44 40.7(2) C52 Co1 C44 111.0(3) C46 Co1 C44 178.2(3) C48 Co1 C54 68.2(3) C50 Co1 C54 68.5(3) C40 Co1 C54 138.8(3) C42 Co1 C54 179.1(3) C52 Co1 C54 40.7(3) C46 Co1 C54 40.1(3) C44 Co1 C54 138.5(3) C48 Co1 C38 138.9(3) C50 Co1 C38 178.9(3) C40 Co1 C38 40.7(2) C42 Co1 C38 69.0(3) C52 Co1 C38 138.0(3) C46 Co1 C38 110.3(3) C44 Co1 C38 68.6(3) C54 Co1 C38 110.4(3) C48 Co1 C37 178.6(3) C50 Co1 C37 139.6(3) C40 Co1 C37 68.3(2) C42 Co1 C37 68.6(2) C52 Co1 C37 110.5(2) C46 Co1 C37 137.7(3) C44 Co1 C37 40.5(3) C54 Co1 C37 110.5(3) C38 Co1 C37 40.8(2) C14 N1 C2 127.5(5) C14 N1 Ni01 123.8(4) C2 N1 Ni01 108.6(3) C20 N2 C25 129.2(5) C20 N2 Ni01 123.8(4) C25 N2 Ni01 106.6(3) N2 Ni01 N1 98.16(19) N2 Ni01 S1 131.19(14) N1 Ni01 S1 130.46(15) C58 O1 C57 112.2(5) C1 S1 Ni01 107.2(2) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance C1 C37 1.498(8) C1 S1 1.870(7) C1 H1A 0.9900 C1 H1B 0.9900 C2 C10 1.407(8) C2 C3 1.419(8) C2 N1 1.424(7) C3 C7 1.408(9) C3 C4 1.506(9) C4 C5 1.520(9) C4 C6 1.541(8) C4 H4 1.0000 C5 H5A 0.9800 C5 H5B 0.9800 C5 H5C 0.9800 C6 H6A 0.9800 C6 H6B 0.9800 C6 H6C 0.9800 C7 C8 1.346(9) C7 H7 0.9500 C8 C9 1.372(9) C8 H8 0.9500 C9 C10 1.399(8) C9 H9 0.9500 C10 C12 1.512(8) C11 C12 1.512(9) C11 H11A 0.9800 C11 H11B 0.9800 C11 H11C 0.9800 C12 C13 1.531(9) C12 H12 1.0000 C13 H13A 0.9800 C13 H13B 0.9800 C13 H13C 0.9800 C14 N1 1.334(6) C14 C19 1.394(8) C14 C15 1.578(7) C15 C16 1.520(8) C15 C18 1.528(8) C15 C17 1.552(7) C16 H16A 0.9800 C16 H16B 0.9800 C16 H16C 0.9800 C17 H17A 0.9800 C17 H17B 0.9800 C17 H17C 0.9800 C18 H18A 0.9800 C18 H18B 0.9800 C18 H18C 0.9800 C19 C20 1.392(7) C19 H19 0.9500 C20 N2 1.341(6) C20 C21 1.560(8) C21 C24 1.514(8) C21 C22 1.541(8) C21 C23 1.553(7) C22 H22A 0.9800 C22 H22B 0.9800 C22 H22C 0.9800 C23 H23A 0.9800 C23 H23B 0.9800 C23 H23C 0.9800 C24 H24A 0.9800 C24 H24B 0.9800 C24 H24C 0.9800 C25 C33 1.408(8) C25 C26 1.410(8) C25 N2 1.429(7) C26 C30 1.389(8) C26 C28 1.514(8) C27 C28 1.536(8) C27 H27A 0.9800 C27 H27B 0.9800 C27 H27C 0.9800 C28 C29 1.524(9) C28 H28 1.0000 C29 H29A 0.9800 C29 H29B 0.9800 C29 H29C 0.9800 C30 C31 1.374(9) C30 H30 0.9500 C31 C32 1.382(9) C31 H31 0.9500 C32 C33 1.393(8) C32 H32 0.9500 C33 C34 1.523(8) C34 C36 1.512(8) C34 C35 1.529(8) C34 H34 1.0000 C35 H35A 0.9800 C35 H35B 0.9800 C35 H35C 0.9800 C36 H36A 0.9800 C36 H36B 0.9800 C36 H36C 0.9800 C37 C44 1.425(9) C37 C38 1.439(8) C37 Co1 2.065(6) C38 C40 1.421(8) C38 C39 1.485(9) C38 Co1 2.060(7) C39 H39A 0.9800 C39 H39B 0.9800 C39 H39C 0.9800 C40 C42 1.426(9) C40 C41 1.514(8) C40 Co1 2.030(6) C41 H41A 0.9800 C41 H41B 0.9800 C41 H41C 0.9800 C42 C44 1.420(8) C42 C43 1.501(9) C42 Co1 2.033(6) C43 H43A 0.9800 C43 H43B 0.9800 C43 H43C 0.9800 C44 C45 1.487(9) C44 Co1 2.047(7) C45 H45A 0.9800 C45 H45B 0.9800 C45 H45C 0.9800 C46 C54 1.405(9) C46 C48 1.420(9) C46 C47 1.488(9) C46 Co1 2.045(7) C47 H47A 0.9800 C47 H47B 0.9800 C47 H47C 0.9800 C48 C50 1.402(9) C48 C49 1.501(9) C48 Co1 2.010(7) C49 H49A 0.9800 C49 H49B 0.9800 C49 H49C 0.9800 C50 C52 1.431(8) C50 C51 1.474(9) C50 Co1 2.023(7) C51 H51A 0.9800 C51 H51B 0.9800 C51 H51C 0.9800 C52 C54 1.422(9) C52 C53 1.498(9) C52 Co1 2.037(6) C53 H53A 0.9800 C53 H53B 0.9800 C53 H53C 0.9800 C54 C55 1.516(9) C54 Co1 2.050(6) C55 H55A 0.9800 C55 H55B 0.9800 C55 H55C 0.9800 C56 C57 1.491(9) C56 H56A 0.9800 C56 H56B 0.9800 C56 H56C 0.9800 C57 O1 1.405(7) C57 H57A 0.9900 C57 H57B 0.9900 C58 O1 1.404(8) C58 C59 1.509(9) C58 H58A 0.9900 C58 H58B 0.9900 C59 H59A 0.9800 C59 H59B 0.9800 C59 H59C 0.9800 N1 Ni01 1.910(4) N2 Ni01 1.902(5) Ni01 S1 2.1809(17)