#------------------------------------------------------------------------------ #$Date: 2019-11-17 07:46:35 +0200 (Sun, 17 Nov 2019) $ #$Revision: 228730 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/54/86/1548654.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_1548654 loop_ _publ_author_name 'Clarke, Ryan M.' 'Jeen, Tiffany' 'Rigo, Serena' 'Thompson, John R.' 'Kaake, Loren G.' 'Thomas, Fabrice' 'Storr, Tim' _publ_section_title ; Exploiting exciton coupling of ligand radical intervalence charge transfer transitions to tune NIR absorption. ; _journal_issue 6 _journal_name_full 'Chemical science' _journal_page_first 1610 _journal_page_last 1620 _journal_paper_doi 10.1039/c7sc04537a _journal_volume 9 _journal_year 2018 _chemical_formula_moiety 'C72 H96 N6 Ni2 O4' _chemical_formula_sum 'C72 H96 N6 Ni2 O4' _chemical_formula_weight 1226.96 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens geom _audit_update_record ; 2017-10-11 deposited with the CCDC. 2018-01-09 downloaded from the CCDC. ; _cell_angle_alpha 82.482(5) _cell_angle_beta 89.480(4) _cell_angle_gamma 67.190(5) _cell_formula_units_Z 2 _cell_length_a 11.4567(7) _cell_length_b 13.1358(10) _cell_length_c 25.5529(16) _cell_measurement_reflns_used 9866 _cell_measurement_temperature 150(2) _cell_measurement_theta_max 62.74 _cell_measurement_theta_min 3.49 _cell_volume 3510.7(4) _computing_cell_refinement 'Bruker SAINT (Bruker, 2013)' _computing_data_collection 'Bruker APEX2 (Bruker, 2014)' _computing_data_reduction 'Bruker SAINT (Bruker, 2013)' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2015), Shelxle (H\"ubschle et al., 2011)' _computing_structure_solution 'SHELXT (Sheldrick, 2015)' _diffrn_ambient_temperature 150(2) _diffrn_measured_fraction_theta_full 0.984 _diffrn_measured_fraction_theta_max 0.984 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _diffrn_reflns_av_R_equivalents 0.0709 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_number 50257 _diffrn_reflns_theta_full 61.164 _diffrn_reflns_theta_max 61.164 _diffrn_reflns_theta_min 1.746 _diffrn_source 'Microfocus sealed X-ray tub fitted with HELIOS multilayer optics' _exptl_absorpt_coefficient_mu 1.043 _exptl_absorpt_correction_T_max 0.7523 _exptl_absorpt_correction_T_min 0.6438 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(Sheldrick , 1996)' _exptl_crystal_colour 'light brown' _exptl_crystal_density_diffrn 1.161 _exptl_crystal_description plate _exptl_crystal_F_000 1316 _exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: Acetonitrile' _refine_diff_density_max 0.772 _refine_diff_density_min -0.548 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 842 _refine_ls_number_reflns 10599 _refine_ls_number_restraints 850 _refine_ls_restrained_S_all 1.031 _refine_ls_R_factor_all 0.0793 _refine_ls_R_factor_gt 0.0599 _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^)+(0.1240P)^2^+0.1324P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1685 _refine_ls_wR_factor_ref 0.1848 _reflns_Friedel_coverage 0.000 _reflns_number_gt 7887 _reflns_number_total 10599 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c7sc04537a2.cif _cod_data_source_block Compound_4 _cod_depositor_comments ; The following automatic conversions were performed: '_exptl_absorpt_correction_type' value 'Multi-scan' changed to 'multi-scan' according to /home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26. Automatic conversion script Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas Adding full bibliography for 1548653--1548655.cif. ; _cod_database_code 1548654 _shelx_res_file ; TITL cu_RMC_Ni2L5meta_0m_a.res in P-1 cu_RMC_Ni2L5meta_0m_2.res created by SHELXL-2016/6 at 15:19:26 on 10-Oct-2017 REM Old TITL cu_RMC_Ni2L5meta_0m in P-1 REM SHELXT solution in P-1 REM R1 0.192, Rweak 0.007, Alpha 0.052, Orientation as input REM Formula found by SHELXT: C66 N4 Ni2 O4 CELL 1.54178 11.4567 13.1358 25.5529 82.482 89.480 67.190 ZERR 2.000 0.0007 0.0010 0.0016 0.005 0.004 0.005 LATT 1 SFAC C H N NI O UNIT 144 192 12 4 8 TEMP -123.220 L.S. 10 DFIX 1.46 0.001 C69 C70 DFIX 1.16 0.001 C70 N5 DFIX 2.62 0.001 C69 N5 DFIX 1.46 0.005 C71 C72 DFIX 1.16 0.005 C71 N6 DFIX 2.62 0.001 C72 N6 DFIX 1.46 0.001 C73 C74 DFIX 1.16 0.001 C73 N7 DFIX 2.62 0.001 C74 N7 DFIX 2.05 0.01 H72B H54C ISOR 0.01 C69 C70 C71 C72 C73 C74 N5 N6 N7 C66A C68A BOND $H RIGU ACTA LIST 6 FMAP 2 PLAN 20 WGHT 0.124000 0.132400 FVAR 0.29159 0.41269 NI1 4 0.230362 0.441823 0.531017 11.00000 0.03792 0.04266 = 0.02781 -0.00521 0.00311 -0.01485 C1 1 0.083749 0.462726 0.622375 11.00000 0.03749 0.04193 = 0.03768 -0.01141 0.00529 -0.01532 NI2 4 0.873368 0.148586 0.052797 11.00000 0.03557 0.07611 = 0.02505 -0.00669 0.00421 -0.02999 C2 1 0.072601 0.418428 0.675613 11.00000 0.04360 0.04985 = 0.03673 -0.00674 0.00582 -0.02005 O1 5 0.170456 0.400313 0.593453 11.00000 0.04530 0.03886 = 0.03613 -0.00637 0.01021 -0.01041 O2 5 0.365461 0.304858 0.543963 11.00000 0.04086 0.05008 = 0.02702 -0.00637 0.00510 -0.01393 O3 5 0.769056 0.132990 0.106732 11.00000 0.03853 0.07922 = 0.02582 -0.00595 0.00333 -0.03127 C3 1 -0.017315 0.485722 0.705774 11.00000 0.04626 0.06197 = 0.03940 -0.01066 0.01109 -0.02065 AFIX 43 H3 2 -0.023349 0.455814 0.741132 11.00000 -1.20000 AFIX 0 O4 5 0.738247 0.173802 0.007914 11.00000 0.03799 0.09133 = 0.02702 -0.00296 0.00190 -0.03042 C4 1 -0.100324 0.595044 0.687915 11.00000 0.05081 0.05467 = 0.04892 -0.01326 0.01200 -0.01631 N1 3 0.092984 0.577888 0.518171 11.00000 0.04400 0.04256 = 0.03232 -0.00501 -0.00072 -0.01771 N2 3 0.289000 0.480062 0.467040 11.00000 0.03990 0.04105 = 0.03149 -0.00417 -0.00121 -0.01701 N3 3 1.003912 0.134576 0.099001 11.00000 0.03788 0.08426 = 0.03276 -0.00358 0.00217 -0.03725 N4 3 0.981924 0.148478 -0.001538 11.00000 0.03689 0.06860 = 0.03343 -0.00407 0.00251 -0.02882 N5 3 0.790124 0.367087 0.307092 11.00000 0.20613 0.26983 = 0.36982 -0.09010 0.10367 -0.14228 C5 1 -0.091972 0.634497 0.636311 11.00000 0.05272 0.04596 = 0.04796 -0.00965 0.00700 -0.00916 AFIX 43 H5 2 -0.149055 0.707682 0.622659 11.00000 -1.20000 AFIX 0 N6 3 0.709168 0.477176 -0.090390 10.50000 0.26266 0.24339 = 0.26472 -0.07280 0.04837 -0.07672 C6 1 -0.003165 0.572127 0.602531 11.00000 0.04231 0.04710 = 0.03880 -0.00751 0.00260 -0.01349 C7 1 0.159557 0.299225 0.698262 11.00000 0.04442 0.05466 = 0.03918 -0.00341 0.00848 -0.01153 N7 3 0.845223 0.431774 0.185679 10.50000 0.24058 0.25549 = 0.29470 -0.04750 -0.05913 -0.11332 C8 1 0.134872 0.216682 0.667327 11.00000 0.05326 0.04984 = 0.06324 -0.00212 0.00938 -0.01739 AFIX 137 H8A 2 0.193561 0.140623 0.680644 11.00000 -1.50000 H8B 2 0.147821 0.233786 0.629768 11.00000 -1.50000 H8C 2 0.047442 0.222830 0.671778 11.00000 -1.50000 AFIX 0 C10 1 0.135318 0.268507 0.756250 11.00000 0.07310 0.07778 = 0.04849 0.00930 0.01547 -0.00666 AFIX 137 H10A 2 0.193428 0.191881 0.768935 11.00000 -1.50000 H10B 2 0.047624 0.274413 0.759093 11.00000 -1.50000 H10C 2 0.149434 0.319626 0.777725 11.00000 -1.50000 AFIX 0 C9 1 0.298210 0.286068 0.696205 11.00000 0.04958 0.07061 = 0.04909 -0.00323 -0.00139 -0.01529 AFIX 137 H9A 2 0.353453 0.208990 0.709704 11.00000 -1.50000 H9B 2 0.312190 0.336749 0.718002 11.00000 -1.50000 H9C 2 0.317739 0.304045 0.659594 11.00000 -1.50000 AFIX 0 C11 1 -0.198608 0.667045 0.723382 11.00000 0.05840 0.06684 = 0.05814 -0.02147 0.01762 -0.01239 C12 1 -0.187740 0.609634 0.779761 11.00000 0.09923 0.10022 = 0.06378 -0.02112 0.03728 0.00121 AFIX 137 H12A 2 -0.252384 0.658740 0.800599 11.00000 -1.50000 H12B 2 -0.103383 0.593090 0.795297 11.00000 -1.50000 H12C 2 -0.200439 0.540022 0.779774 11.00000 -1.50000 AFIX 0 C13 1 -0.179688 0.774752 0.724885 11.00000 0.05961 0.08082 = 0.09558 -0.04854 0.01765 -0.02266 AFIX 137 H13A 2 -0.242822 0.821398 0.747088 11.00000 -1.50000 H13B 2 -0.189611 0.814724 0.688969 11.00000 -1.50000 H13C 2 -0.094413 0.757697 0.739568 11.00000 -1.50000 AFIX 0 C15 1 -0.001143 0.621778 0.548281 11.00000 0.04439 0.04306 = 0.03982 -0.00823 0.00069 -0.01730 C14 1 -0.331803 0.692396 0.700049 11.00000 0.05224 0.09372 = 0.09486 -0.04135 0.02600 -0.02635 AFIX 137 H14A 2 -0.395698 0.738022 0.722319 11.00000 -1.50000 H14B 2 -0.342572 0.622312 0.698699 11.00000 -1.50000 H14C 2 -0.342008 0.733008 0.664263 11.00000 -1.50000 AFIX 0 C16 1 -0.112637 0.726847 0.526273 11.00000 0.05214 0.04703 = 0.05220 -0.00456 0.00051 -0.00653 AFIX 137 H16A 2 -0.188940 0.729323 0.544656 11.00000 -1.50000 H16B 2 -0.125943 0.726912 0.488436 11.00000 -1.50000 H16C 2 -0.095142 0.792265 0.531493 11.00000 -1.50000 AFIX 0 C17 1 0.091144 0.633426 0.463893 11.00000 0.04838 0.04523 = 0.03537 -0.00044 -0.00072 -0.01673 AFIX 23 H17A 2 0.050753 0.715346 0.462968 11.00000 -1.20000 H17B 2 0.041267 0.610959 0.439718 11.00000 -1.20000 AFIX 0 C18 1 0.225363 0.600553 0.446260 11.00000 0.05133 0.04719 = 0.03419 0.00067 -0.00176 -0.02018 C19 1 0.294669 0.660297 0.473459 11.00000 0.07545 0.06664 = 0.06708 0.00044 -0.00809 -0.04404 AFIX 137 H19A 2 0.253700 0.740850 0.462204 11.00000 -1.50000 H19B 2 0.383349 0.633432 0.463630 11.00000 -1.50000 H19C 2 0.291121 0.644678 0.511875 11.00000 -1.50000 AFIX 0 C20 1 0.224067 0.627151 0.386184 11.00000 0.06015 0.06556 = 0.04188 0.00944 0.00309 -0.01488 AFIX 137 H20A 2 0.168904 0.705467 0.375157 11.00000 -1.50000 H20B 2 0.192133 0.579156 0.369679 11.00000 -1.50000 H20C 2 0.310335 0.613887 0.375186 11.00000 -1.50000 AFIX 0 C21 1 0.380024 0.416078 0.441975 11.00000 0.04438 0.05281 = 0.02889 -0.00332 0.00117 -0.02091 AFIX 43 H21 2 0.394342 0.446659 0.407921 11.00000 -1.20000 AFIX 0 C22 1 0.461516 0.303607 0.460420 11.00000 0.03786 0.05268 = 0.02639 -0.00758 0.00065 -0.01777 C23 1 0.561293 0.249546 0.428444 11.00000 0.04717 0.05664 = 0.02267 -0.00793 0.00408 -0.02320 AFIX 43 H23 2 0.564157 0.284719 0.393798 11.00000 -1.20000 AFIX 0 C24 1 0.653922 0.147970 0.445951 11.00000 0.03887 0.05606 = 0.02708 -0.01334 0.00389 -0.02182 C25 1 0.642525 0.097770 0.496882 11.00000 0.03934 0.04796 = 0.03153 -0.00971 0.00043 -0.01701 AFIX 43 H25 2 0.705720 0.026518 0.509355 11.00000 -1.20000 AFIX 0 C28 1 0.543810 0.084052 0.585219 11.00000 0.04652 0.05053 = 0.03499 -0.00257 0.01084 -0.01203 C27 1 0.452434 0.253438 0.512428 11.00000 0.03523 0.04653 = 0.02612 -0.00818 0.00155 -0.01709 C26 1 0.546000 0.144736 0.530015 11.00000 0.04064 0.05042 = 0.02751 -0.01105 0.00588 -0.02125 C29 1 0.636735 -0.038376 0.591502 11.00000 0.07952 0.05860 = 0.06212 0.01260 0.03138 0.00114 AFIX 137 H29A 2 0.625381 -0.076855 0.625482 11.00000 -1.50000 H29B 2 0.723825 -0.042154 0.590298 11.00000 -1.50000 H29C 2 0.620359 -0.074327 0.562740 11.00000 -1.50000 AFIX 0 C30 1 0.581035 0.143622 0.625722 11.00000 0.05171 0.09038 = 0.02872 -0.00305 0.00067 -0.02612 AFIX 137 H30A 2 0.578312 0.107170 0.661450 11.00000 -1.50000 H30B 2 0.521585 0.221778 0.622002 11.00000 -1.50000 H30C 2 0.667035 0.140048 0.619640 11.00000 -1.50000 AFIX 0 C32 1 0.766068 0.095260 0.414232 11.00000 0.04069 0.05553 = 0.02733 -0.00920 0.00322 -0.02186 C31 1 0.412805 0.082353 0.595592 11.00000 0.05967 0.05810 = 0.04721 -0.00603 0.01584 -0.02840 AFIX 137 H31A 2 0.414710 0.040840 0.630572 11.00000 -1.50000 H31B 2 0.389603 0.046165 0.568575 11.00000 -1.50000 H31C 2 0.350183 0.158967 0.594272 11.00000 -1.50000 AFIX 0 C33 1 0.885770 0.037095 0.438194 11.00000 0.04406 0.08432 = 0.02669 -0.01465 0.00282 -0.02069 AFIX 43 H33 2 0.896625 0.028272 0.475558 11.00000 -1.20000 AFIX 0 C34 1 0.989657 -0.008255 0.408109 11.00000 0.03834 0.09380 = 0.03398 -0.01121 -0.00102 -0.01732 AFIX 43 H34 2 1.071038 -0.048590 0.425092 11.00000 -1.20000 AFIX 0 C35 1 0.976442 0.004416 0.353749 11.00000 0.03931 0.07595 = 0.03482 -0.01482 0.00610 -0.02071 AFIX 43 H35 2 1.048873 -0.025568 0.333537 11.00000 -1.20000 AFIX 0 C36 1 0.857170 0.061062 0.328407 11.00000 0.04082 0.05499 = 0.02693 -0.01019 0.00326 -0.02429 C37 1 0.754043 0.106006 0.359231 11.00000 0.03709 0.05464 = 0.02938 -0.00997 0.00384 -0.01995 AFIX 43 H37 2 0.672447 0.145448 0.342308 11.00000 -1.20000 AFIX 0 C38 1 0.793600 0.110046 0.157707 11.00000 0.03597 0.06347 = 0.02489 -0.01103 0.00371 -0.02315 C39 1 0.703949 0.088152 0.192557 11.00000 0.03208 0.05650 = 0.02853 -0.01035 0.00653 -0.01866 C40 1 0.730637 0.072934 0.246308 11.00000 0.03633 0.05639 = 0.02926 -0.01001 0.00890 -0.02082 AFIX 43 H40 2 0.669951 0.060781 0.269102 11.00000 -1.20000 AFIX 0 C44 1 0.581736 0.084287 0.170223 11.00000 0.03200 0.07005 = 0.03226 -0.00977 0.00534 -0.02207 C43 1 0.907626 0.105300 0.181244 11.00000 0.04153 0.06873 = 0.02871 -0.01033 0.00572 -0.02912 C42 1 0.928209 0.088366 0.236498 11.00000 0.03838 0.07181 = 0.02914 -0.01091 0.00013 -0.02944 AFIX 43 H42 2 1.005043 0.086881 0.250959 11.00000 -1.20000 AFIX 0 C41 1 0.839899 0.073976 0.269894 11.00000 0.03876 0.05294 = 0.02833 -0.01219 0.00551 -0.01916 C45 1 0.499416 0.199969 0.142482 11.00000 0.03763 0.08241 = 0.04811 -0.00772 0.00172 -0.02048 AFIX 137 H45A 2 0.419887 0.199334 0.129048 11.00000 -1.50000 H45B 2 0.544501 0.220968 0.112974 11.00000 -1.50000 H45C 2 0.480898 0.254034 0.167576 11.00000 -1.50000 AFIX 0 C47 1 0.506581 0.050556 0.214228 11.00000 0.03871 0.09665 = 0.03971 -0.01310 0.00928 -0.03535 AFIX 137 H47A 2 0.430487 0.047112 0.198731 11.00000 -1.50000 H47B 2 0.481789 0.105772 0.238887 11.00000 -1.50000 H47C 2 0.559422 -0.022779 0.233197 11.00000 -1.50000 AFIX 0 C46 1 0.612520 -0.001785 0.131992 11.00000 0.04301 0.08591 = 0.04103 -0.02050 0.00333 -0.03274 AFIX 137 H46A 2 0.533725 -0.004433 0.118929 11.00000 -1.50000 H46B 2 0.666780 -0.075312 0.150342 11.00000 -1.50000 H46C 2 0.656817 0.019138 0.102162 11.00000 -1.50000 AFIX 0 C48 1 1.003688 0.120845 0.149512 11.00000 0.04459 0.09038 = 0.03150 -0.01046 0.00201 -0.04054 AFIX 43 H48 2 1.075403 0.121052 0.167800 11.00000 -1.20000 AFIX 0 C49 1 1.111336 0.154158 0.072406 11.00000 0.05184 0.11350 = 0.03885 -0.00684 0.00591 -0.05666 C50 1 1.238408 0.086546 0.101553 11.00000 0.04848 0.18652 = 0.04309 0.00080 0.00050 -0.06454 AFIX 137 H50A 2 1.306906 0.084488 0.077923 11.00000 -1.50000 H50B 2 1.244683 0.010389 0.113102 11.00000 -1.50000 H50C 2 1.245624 0.121138 0.132440 11.00000 -1.50000 AFIX 0 C52 1 1.113704 0.115848 0.018984 11.00000 0.03601 0.09524 = 0.03749 -0.00170 0.00361 -0.03497 AFIX 23 H52A 2 1.159072 0.150432 -0.005823 11.00000 -1.20000 H52B 2 1.158980 0.033851 0.022303 11.00000 -1.20000 AFIX 0 C51 1 1.078676 0.278932 0.066474 11.00000 0.11095 0.13056 = 0.06777 -0.02856 0.02882 -0.09155 AFIX 137 H51A 2 1.147265 0.295385 0.049154 11.00000 -1.50000 H51B 2 1.068052 0.303461 0.101451 11.00000 -1.50000 H51C 2 0.999652 0.318407 0.044992 11.00000 -1.50000 AFIX 0 C53 1 0.960463 0.157059 -0.052273 11.00000 0.04272 0.06350 = 0.03071 -0.00575 0.00717 -0.02454 C54 1 1.069568 0.137465 -0.088723 11.00000 0.04871 0.11043 = 0.03778 -0.01324 0.01141 -0.03570 AFIX 137 H54A 2 1.056240 0.101731 -0.118182 11.00000 -1.50000 H54B 2 1.149011 0.088984 -0.069113 11.00000 -1.50000 H54C 2 1.074133 0.208987 -0.102488 11.00000 -1.50000 AFIX 0 C55 1 0.834258 0.186888 -0.075142 11.00000 0.04222 0.07715 = 0.03047 -0.00903 0.00325 -0.03056 C56 1 0.815302 0.207376 -0.131073 11.00000 0.05347 0.09177 = 0.02788 -0.00320 0.00468 -0.03983 AFIX 43 H56 2 0.886636 0.199091 -0.151944 11.00000 -1.20000 AFIX 0 C57 1 0.700182 0.238225 -0.156157 11.00000 0.05964 0.09199 = 0.03091 0.00047 -0.00147 -0.04181 C58 1 0.596784 0.251124 -0.123880 11.00000 0.04774 0.09240 = 0.03480 0.00285 -0.00610 -0.03347 AFIX 43 H58 2 0.515411 0.273258 -0.140686 11.00000 -1.20000 AFIX 0 C59 1 0.605744 0.233789 -0.069556 11.00000 0.04640 0.08667 = 0.03474 -0.00359 -0.00023 -0.03398 C60 1 0.729214 0.197200 -0.043729 11.00000 0.04228 0.07005 = 0.02841 -0.00342 0.00132 -0.02739 C61 1 0.486295 0.253712 -0.036986 11.00000 0.04416 0.10994 = 0.03974 -0.00301 0.00046 -0.03297 C62 1 0.474034 0.340880 -0.000728 11.00000 0.06086 0.11735 = 0.06539 -0.01941 0.01010 -0.01987 AFIX 137 H62A 2 0.395130 0.357638 0.018013 11.00000 -1.50000 H62B 2 0.472856 0.409107 -0.021921 11.00000 -1.50000 H62C 2 0.546260 0.311742 0.024952 11.00000 -1.50000 AFIX 0 C63 1 0.496629 0.144783 -0.005363 11.00000 0.05718 0.13292 = 0.04866 0.00728 0.00716 -0.05479 AFIX 137 H63A 2 0.421657 0.157283 0.015721 11.00000 -1.50000 H63B 2 0.572853 0.115370 0.018162 11.00000 -1.50000 H63C 2 0.502081 0.091033 -0.029460 11.00000 -1.50000 AFIX 0 C64 1 0.365139 0.295236 -0.073033 11.00000 0.04776 0.16755 = 0.05868 0.00100 -0.00360 -0.04065 AFIX 137 H64A 2 0.291384 0.307035 -0.051248 11.00000 -1.50000 H64B 2 0.371592 0.239440 -0.096102 11.00000 -1.50000 H64C 2 0.355433 0.365627 -0.094660 11.00000 -1.50000 AFIX 0 C65 1 0.681975 0.257778 -0.216540 11.00000 0.07564 0.12925 = 0.02905 -0.00034 -0.00088 -0.05512 C69 1 0.578642 0.479563 0.349817 11.00000 0.29154 0.19987 = 0.32230 0.11072 0.09906 -0.10016 AFIX 137 H69A 2 0.504250 0.470295 0.336137 11.00000 -1.50000 H69B 2 0.566914 0.558095 0.342247 11.00000 -1.50000 H69C 2 0.589101 0.456157 0.388094 11.00000 -1.50000 AFIX 0 C70 1 0.691593 0.411104 0.324399 11.00000 0.22911 0.20489 = 0.27228 0.07269 0.07062 -0.11305 C71 1 0.817526 0.455323 -0.083374 10.50000 0.27324 0.24327 = 0.26405 -0.03379 0.01188 -0.10467 C72 1 0.954480 0.424204 -0.087523 10.50000 0.27096 0.15510 = 0.24573 -0.00226 -0.02984 -0.10004 AFIX 137 H72A 2 0.972273 0.491776 -0.094796 10.50000 -1.50000 H72B 2 0.984320 0.379220 -0.116328 10.50000 -1.50000 H72C 2 0.998353 0.380824 -0.054219 10.50000 -1.50000 AFIX 0 C73 1 0.765033 0.417141 0.164486 10.50000 0.18471 0.17761 = 0.19609 -0.01380 -0.00160 -0.07731 C74 1 0.656895 0.402565 0.141778 10.50000 0.24696 0.20038 = 0.27212 -0.01466 -0.03420 -0.12662 AFIX 137 H74A 2 0.672303 0.389252 0.105013 10.50000 -1.50000 H74B 2 0.580221 0.470001 0.142957 10.50000 -1.50000 H74C 2 0.645619 0.338664 0.162133 10.50000 -1.50000 AFIX 0 PART 1 C66 1 0.779131 0.162894 -0.241116 21.00000 0.09268 0.12259 = 0.03266 -0.01187 -0.01116 -0.01599 AFIX 137 H66A 2 0.772166 0.181873 -0.279662 21.00000 -1.50000 H66B 2 0.763526 0.094755 -0.231319 21.00000 -1.50000 H66C 2 0.864439 0.150784 -0.228238 21.00000 -1.50000 AFIX 0 C67 1 0.715934 0.361799 -0.235254 21.00000 0.10277 0.12731 = 0.03231 0.01237 0.00134 -0.06797 AFIX 137 H67A 2 0.698502 0.383186 -0.273465 21.00000 -1.50000 H67B 2 0.805962 0.342649 -0.227012 21.00000 -1.50000 H67C 2 0.664448 0.424230 -0.216921 21.00000 -1.50000 AFIX 0 C68 1 0.558141 0.279915 -0.237745 21.00000 0.07385 0.11513 = 0.02432 0.00174 -0.00908 -0.04467 AFIX 137 H68A 2 0.555666 0.298076 -0.276266 21.00000 -1.50000 H68B 2 0.495752 0.342995 -0.222864 21.00000 -1.50000 H68C 2 0.538119 0.213850 -0.228643 21.00000 -1.50000 AFIX 0 PART 2 C66A 1 0.804275 0.241302 -0.243808 -21.00000 0.09918 0.18204 = 0.04133 -0.00237 0.01151 -0.06723 AFIX 137 H66D 2 0.787195 0.258112 -0.282152 -21.00000 -1.50000 H66E 2 0.864131 0.163800 -0.234710 -21.00000 -1.50000 H66F 2 0.840836 0.291306 -0.232252 -21.00000 -1.50000 AFIX 0 C67A 1 0.579982 0.368720 -0.234894 -21.00000 0.09431 0.18352 = 0.07028 0.05285 -0.02316 -0.05078 AFIX 137 H67D 2 0.562252 0.375384 -0.272916 -21.00000 -1.50000 H67E 2 0.607614 0.427720 -0.227893 -21.00000 -1.50000 H67F 2 0.502994 0.376028 -0.215945 -21.00000 -1.50000 AFIX 0 C68A 1 0.640558 0.160017 -0.230163 -21.00000 0.15747 0.20050 = 0.04802 -0.02310 -0.00536 -0.11176 AFIX 137 H68D 2 0.627877 0.166368 -0.268518 -21.00000 -1.50000 H68E 2 0.561381 0.166716 -0.213156 -21.00000 -1.50000 H68F 2 0.707185 0.087410 -0.217115 -21.00000 -1.50000 PART 0 AFIX 0 HKLF 4 REM cu_RMC_Ni2L5meta_0m_a.res in P-1 REM R1 = 0.0599 for 7887 Fo > 4sig(Fo) and 0.0793 for all 10599 data REM 842 parameters refined using 850 restraints END WGHT 0.1240 0.1324 REM Highest difference peak 0.772, deepest hole -0.548, 1-sigma level 0.075 Q1 1 0.8229 0.2504 0.0519 11.00000 0.05 0.77 Q2 1 0.6162 0.3749 0.2800 11.00000 0.05 0.72 Q3 1 0.3043 0.4601 0.5292 11.00000 0.05 0.66 Q4 1 0.6656 0.4475 0.3443 11.00000 0.05 0.64 Q5 1 0.2507 0.3367 0.5305 11.00000 0.05 0.55 Q6 1 0.2882 0.3745 0.5160 11.00000 0.05 0.48 Q7 1 0.9406 0.1828 0.0727 11.00000 0.05 0.44 Q8 1 0.1410 0.4267 0.5412 11.00000 0.05 0.43 Q9 1 0.9597 0.1618 0.0487 11.00000 0.05 0.42 Q10 1 0.1874 0.5584 0.5322 11.00000 0.05 0.36 Q11 1 0.7806 0.4297 0.2303 11.00000 0.05 0.34 Q12 1 0.4370 0.3206 0.5440 11.00000 0.05 0.32 Q13 1 0.6800 0.2668 0.0085 11.00000 0.05 0.31 Q14 1 1.1841 0.1913 0.1014 11.00000 0.05 0.31 Q15 1 0.2570 0.6273 0.4605 11.00000 0.05 0.31 Q16 1 0.8191 0.1174 0.0216 11.00000 0.05 0.31 Q17 1 0.5509 0.1045 0.6024 11.00000 0.05 0.30 Q18 1 0.2784 0.5562 0.4598 11.00000 0.05 0.29 Q19 1 0.7796 0.1373 0.0603 11.00000 0.05 0.29 Q20 1 0.8924 0.0301 0.0585 11.00000 0.05 0.29 ; _shelx_res_checksum 66362 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.23036(5) 0.44182(4) 0.53102(2) 0.03637(18) Uani 1 1 d . . . . . C1 C 0.0837(3) 0.4627(3) 0.62238(12) 0.0385(7) Uani 1 1 d . . . . . Ni2 Ni 0.87337(5) 0.14859(5) 0.05280(2) 0.04310(19) Uani 1 1 d . . . . . C2 C 0.0726(3) 0.4184(3) 0.67561(13) 0.0428(7) Uani 1 1 d . . . . . O1 O 0.1705(2) 0.40031(18) 0.59345(8) 0.0419(5) Uani 1 1 d . . . . . O2 O 0.36546(19) 0.30486(18) 0.54396(8) 0.0404(5) Uani 1 1 d . . . . . O3 O 0.7691(2) 0.1330(2) 0.10673(8) 0.0454(6) Uani 1 1 d . . . . . C3 C -0.0173(3) 0.4857(3) 0.70577(14) 0.0491(8) Uani 1 1 d . . . . . H3 H -0.023349 0.455814 0.741132 0.059 Uiso 1 1 calc R U . . . O4 O 0.7382(2) 0.1738(2) 0.00791(8) 0.0510(6) Uani 1 1 d . . . . . C4 C -0.1003(3) 0.5950(3) 0.68791(14) 0.0522(9) Uani 1 1 d . . . . . N1 N 0.0930(2) 0.5779(2) 0.51817(10) 0.0394(6) Uani 1 1 d . . . . . N2 N 0.2890(2) 0.4801(2) 0.46704(10) 0.0372(6) Uani 1 1 d . . . . . N3 N 1.0039(2) 0.1346(3) 0.09900(10) 0.0479(7) Uani 1 1 d . . . . . N4 N 0.9819(2) 0.1485(3) -0.00154(10) 0.0441(7) Uani 1 1 d . . . . . N5 N 0.7901(10) 0.3671(10) 0.3071(6) 0.263(6) Uani 1 1 d D U . . . C5 C -0.0920(3) 0.6345(3) 0.63631(14) 0.0517(9) Uani 1 1 d . . . . . H5 H -0.149055 0.707682 0.622659 0.062 Uiso 1 1 calc R U . . . N6 N 0.7092(17) 0.477(2) -0.0904(10) 0.260(9) Uani 0.5 1 d D U P . . C6 C -0.0032(3) 0.5721(3) 0.60253(13) 0.0438(7) Uani 1 1 d . . . . . C7 C 0.1596(3) 0.2992(3) 0.69826(13) 0.0488(8) Uani 1 1 d . . . . . N7 N 0.8452(15) 0.4318(18) 0.1857(9) 0.257(10) Uani 0.5 1 d D U P . . C8 C 0.1349(4) 0.2167(3) 0.66733(16) 0.0569(9) Uani 1 1 d . . . . . H8A H 0.193561 0.140623 0.680644 0.085 Uiso 1 1 calc R U . . . H8B H 0.147821 0.233786 0.629768 0.085 Uiso 1 1 calc R U . . . H8C H 0.047442 0.222830 0.671778 0.085 Uiso 1 1 calc R U . . . C10 C 0.1353(4) 0.2685(4) 0.75625(16) 0.0753(13) Uani 1 1 d . . . . . H10A H 0.193428 0.191881 0.768935 0.113 Uiso 1 1 calc R U . . . H10B H 0.047624 0.274413 0.759093 0.113 Uiso 1 1 calc R U . . . H10C H 0.149434 0.319626 0.777725 0.113 Uiso 1 1 calc R U . . . C9 C 0.2982(3) 0.2861(4) 0.69621(15) 0.0594(10) Uani 1 1 d . . . . . H9A H 0.353453 0.208990 0.709704 0.089 Uiso 1 1 calc R U . . . H9B H 0.312190 0.336749 0.718002 0.089 Uiso 1 1 calc R U . . . H9C H 0.317739 0.304045 0.659594 0.089 Uiso 1 1 calc R U . . . C11 C -0.1986(4) 0.6670(4) 0.72338(16) 0.0637(10) Uani 1 1 d . . . . . C12 C -0.1877(5) 0.6096(5) 0.77976(19) 0.0993(18) Uani 1 1 d . . . . . H12A H -0.252384 0.658740 0.800599 0.149 Uiso 1 1 calc R U . . . H12B H -0.103383 0.593090 0.795297 0.149 Uiso 1 1 calc R U . . . H12C H -0.200439 0.540022 0.779774 0.149 Uiso 1 1 calc R U . . . C13 C -0.1797(4) 0.7748(4) 0.7249(2) 0.0767(13) Uani 1 1 d . . . . . H13A H -0.242822 0.821398 0.747088 0.115 Uiso 1 1 calc R U . . . H13B H -0.189611 0.814724 0.688969 0.115 Uiso 1 1 calc R U . . . H13C H -0.094413 0.757697 0.739568 0.115 Uiso 1 1 calc R U . . . C15 C -0.0011(3) 0.6218(3) 0.54828(13) 0.0421(7) Uani 1 1 d . . . . . C14 C -0.3318(4) 0.6924(4) 0.7000(2) 0.0783(13) Uani 1 1 d . . . . . H14A H -0.395698 0.738022 0.722319 0.118 Uiso 1 1 calc R U . . . H14B H -0.342572 0.622312 0.698699 0.118 Uiso 1 1 calc R U . . . H14C H -0.342008 0.733008 0.664263 0.118 Uiso 1 1 calc R U . . . C16 C -0.1126(3) 0.7268(3) 0.52627(15) 0.0546(9) Uani 1 1 d . . . . . H16A H -0.188940 0.729323 0.544656 0.082 Uiso 1 1 calc R U . . . H16B H -0.125943 0.726912 0.488436 0.082 Uiso 1 1 calc R U . . . H16C H -0.095142 0.792265 0.531493 0.082 Uiso 1 1 calc R U . . . C17 C 0.0911(3) 0.6334(3) 0.46389(12) 0.0439(7) Uani 1 1 d . . . . . H17A H 0.050753 0.715346 0.462968 0.053 Uiso 1 1 calc R U . . . H17B H 0.041267 0.610959 0.439718 0.053 Uiso 1 1 calc R U . . . C18 C 0.2254(3) 0.6006(3) 0.44626(12) 0.0445(8) Uani 1 1 d . . . . . C19 C 0.2947(4) 0.6603(4) 0.47346(17) 0.0656(11) Uani 1 1 d . . . . . H19A H 0.253700 0.740850 0.462204 0.098 Uiso 1 1 calc R U . . . H19B H 0.383349 0.633432 0.463630 0.098 Uiso 1 1 calc R U . . . H19C H 0.291121 0.644678 0.511875 0.098 Uiso 1 1 calc R U . . . C20 C 0.2241(4) 0.6272(3) 0.38618(14) 0.0605(10) Uani 1 1 d . . . . . H20A H 0.168904 0.705467 0.375157 0.091 Uiso 1 1 calc R U . . . H20B H 0.192133 0.579156 0.369679 0.091 Uiso 1 1 calc R U . . . H20C H 0.310335 0.613887 0.375186 0.091 Uiso 1 1 calc R U . . . C21 C 0.3800(3) 0.4161(3) 0.44197(12) 0.0416(7) Uani 1 1 d . . . . . H21 H 0.394342 0.446659 0.407921 0.050 Uiso 1 1 calc R U . . . C22 C 0.4615(3) 0.3036(3) 0.46042(11) 0.0387(7) Uani 1 1 d . . . . . C23 C 0.5613(3) 0.2495(3) 0.42844(12) 0.0410(7) Uani 1 1 d . . . . . H23 H 0.564157 0.284719 0.393798 0.049 Uiso 1 1 calc R U . . . C24 C 0.6539(3) 0.1480(3) 0.44595(11) 0.0389(7) Uani 1 1 d . . . . . C25 C 0.6425(3) 0.0978(3) 0.49688(12) 0.0392(7) Uani 1 1 d . . . . . H25 H 0.705720 0.026518 0.509355 0.047 Uiso 1 1 calc R U . . . C28 C 0.5438(3) 0.0841(3) 0.58522(13) 0.0465(8) Uani 1 1 d . . . . . C27 C 0.4524(3) 0.2534(3) 0.51243(11) 0.0353(7) Uani 1 1 d . . . . . C26 C 0.5460(3) 0.1447(3) 0.53002(11) 0.0379(7) Uani 1 1 d . . . . . C29 C 0.6367(4) -0.0384(4) 0.59150(17) 0.0776(14) Uani 1 1 d . . . . . H29A H 0.625381 -0.076855 0.625482 0.116 Uiso 1 1 calc R U . . . H29B H 0.723825 -0.042154 0.590298 0.116 Uiso 1 1 calc R U . . . H29C H 0.620359 -0.074327 0.562740 0.116 Uiso 1 1 calc R U . . . C30 C 0.5810(4) 0.1436(4) 0.62572(13) 0.0579(10) Uani 1 1 d . . . . . H30A H 0.578312 0.107170 0.661450 0.087 Uiso 1 1 calc R U . . . H30B H 0.521585 0.221778 0.622002 0.087 Uiso 1 1 calc R U . . . H30C H 0.667035 0.140048 0.619640 0.087 Uiso 1 1 calc R U . . . C32 C 0.7661(3) 0.0953(3) 0.41423(12) 0.0399(7) Uani 1 1 d . . . . . C31 C 0.4128(4) 0.0824(3) 0.59559(14) 0.0535(9) Uani 1 1 d . . . . . H31A H 0.414710 0.040840 0.630572 0.080 Uiso 1 1 calc R U . . . H31B H 0.389603 0.046165 0.568575 0.080 Uiso 1 1 calc R U . . . H31C H 0.350183 0.158967 0.594272 0.080 Uiso 1 1 calc R U . . . C33 C 0.8858(3) 0.0371(3) 0.43819(13) 0.0524(9) Uani 1 1 d . . . . . H33 H 0.896625 0.028272 0.475558 0.063 Uiso 1 1 calc R U . . . C34 C 0.9897(3) -0.0083(4) 0.40811(13) 0.0577(10) Uani 1 1 d . . . . . H34 H 1.071038 -0.048590 0.425092 0.069 Uiso 1 1 calc R U . . . C35 C 0.9764(3) 0.0044(3) 0.35375(13) 0.0499(9) Uani 1 1 d . . . . . H35 H 1.048873 -0.025568 0.333537 0.060 Uiso 1 1 calc R U . . . C36 C 0.8572(3) 0.0611(3) 0.32841(11) 0.0388(7) Uani 1 1 d . . . . . C37 C 0.7540(3) 0.1060(3) 0.35923(12) 0.0393(7) Uani 1 1 d . . . . . H37 H 0.672447 0.145448 0.342308 0.047 Uiso 1 1 calc R U . . . C38 C 0.7936(3) 0.1100(3) 0.15771(11) 0.0398(7) Uani 1 1 d . . . . . C39 C 0.7039(3) 0.0882(3) 0.19256(11) 0.0382(7) Uani 1 1 d . . . . . C40 C 0.7306(3) 0.0729(3) 0.24631(11) 0.0395(7) Uani 1 1 d . . . . . H40 H 0.669951 0.060781 0.269102 0.047 Uiso 1 1 calc R U . . . C44 C 0.5817(3) 0.0843(3) 0.17022(12) 0.0439(8) Uani 1 1 d . . . . . C43 C 0.9076(3) 0.1053(3) 0.18124(12) 0.0437(8) Uani 1 1 d . . . . . C42 C 0.9282(3) 0.0884(3) 0.23650(12) 0.0436(8) Uani 1 1 d . . . . . H42 H 1.005043 0.086881 0.250959 0.052 Uiso 1 1 calc R U . . . C41 C 0.8399(3) 0.0740(3) 0.26989(12) 0.0390(7) Uani 1 1 d . . . . . C45 C 0.4994(3) 0.2000(4) 0.14248(15) 0.0571(9) Uani 1 1 d . . . . . H45A H 0.419887 0.199334 0.129048 0.086 Uiso 1 1 calc R U . . . H45B H 0.544501 0.220968 0.112974 0.086 Uiso 1 1 calc R U . . . H45C H 0.480898 0.254034 0.167576 0.086 Uiso 1 1 calc R U . . . C47 C 0.5066(3) 0.0506(4) 0.21423(14) 0.0553(10) Uani 1 1 d . . . . . H47A H 0.430487 0.047112 0.198731 0.083 Uiso 1 1 calc R U . . . H47B H 0.481789 0.105772 0.238887 0.083 Uiso 1 1 calc R U . . . H47C H 0.559422 -0.022779 0.233197 0.083 Uiso 1 1 calc R U . . . C46 C 0.6125(3) -0.0018(4) 0.13199(14) 0.0532(9) Uani 1 1 d . . . . . H46A H 0.533725 -0.004433 0.118929 0.080 Uiso 1 1 calc R U . . . H46B H 0.666780 -0.075312 0.150342 0.080 Uiso 1 1 calc R U . . . H46C H 0.656817 0.019138 0.102162 0.080 Uiso 1 1 calc R U . . . C48 C 1.0037(3) 0.1208(3) 0.14951(13) 0.0509(9) Uani 1 1 d . . . . . H48 H 1.075403 0.121052 0.167800 0.061 Uiso 1 1 calc R U . . . C49 C 1.1113(4) 0.1542(4) 0.07241(14) 0.0609(10) Uani 1 1 d . . . . . C50 C 1.2384(4) 0.0865(5) 0.10155(16) 0.0885(17) Uani 1 1 d . . . . . H50A H 1.306906 0.084488 0.077923 0.133 Uiso 1 1 calc R U . . . H50B H 1.244683 0.010389 0.113102 0.133 Uiso 1 1 calc R U . . . H50C H 1.245624 0.121138 0.132440 0.133 Uiso 1 1 calc R U . . . C52 C 1.1137(3) 0.1158(4) 0.01898(13) 0.0541(9) Uani 1 1 d . . . . . H52A H 1.159072 0.150432 -0.005823 0.065 Uiso 1 1 calc R U . . . H52B H 1.158980 0.033851 0.022303 0.065 Uiso 1 1 calc R U . . . C51 C 1.0787(5) 0.2789(5) 0.06647(19) 0.0881(15) Uani 1 1 d . . . . . H51A H 1.147265 0.295385 0.049154 0.132 Uiso 1 1 calc R U . . . H51B H 1.068052 0.303461 0.101451 0.132 Uiso 1 1 calc R U . . . H51C H 0.999652 0.318407 0.044992 0.132 Uiso 1 1 calc R U . . . C53 C 0.9605(3) 0.1571(3) -0.05227(12) 0.0446(8) Uani 1 1 d . . . . . C54 C 1.0696(4) 0.1375(4) -0.08872(14) 0.0640(11) Uani 1 1 d . . . . . H54A H 1.056240 0.101731 -0.118182 0.096 Uiso 1 1 calc R U . . . H54B H 1.149011 0.088984 -0.069113 0.096 Uiso 1 1 calc R U . . . H54C H 1.074133 0.208987 -0.102488 0.096 Uiso 1 1 calc DR U . . . C55 C 0.8343(3) 0.1869(3) -0.07514(12) 0.0476(8) Uani 1 1 d . . . . . C56 C 0.8153(3) 0.2074(4) -0.13107(13) 0.0547(9) Uani 1 1 d . . . . . H56 H 0.886636 0.199091 -0.151944 0.066 Uiso 1 1 calc R U . . . C57 C 0.7002(4) 0.2382(4) -0.15616(13) 0.0579(10) Uani 1 1 d . . . . . C58 C 0.5968(3) 0.2511(4) -0.12388(13) 0.0575(10) Uani 1 1 d . . . . . H58 H 0.515411 0.273258 -0.140686 0.069 Uiso 1 1 calc R U . . . C59 C 0.6057(3) 0.2338(4) -0.06956(13) 0.0539(9) Uani 1 1 d . . . . . C60 C 0.7292(3) 0.1972(3) -0.04373(12) 0.0455(8) Uani 1 1 d . . . . . C61 C 0.4863(3) 0.2537(4) -0.03699(14) 0.0644(11) Uani 1 1 d . . . . . C62 C 0.4740(4) 0.3409(5) -0.00073(19) 0.0852(14) Uani 1 1 d . . . . . H62A H 0.395130 0.357638 0.018013 0.128 Uiso 1 1 calc R U . . . H62B H 0.472856 0.409107 -0.021921 0.128 Uiso 1 1 calc R U . . . H62C H 0.546260 0.311742 0.024952 0.128 Uiso 1 1 calc R U . . . C63 C 0.4966(4) 0.1448(5) -0.00536(16) 0.0761(13) Uani 1 1 d . . . . . H63A H 0.421657 0.157283 0.015721 0.114 Uiso 1 1 calc R U . . . H63B H 0.572853 0.115370 0.018162 0.114 Uiso 1 1 calc R U . . . H63C H 0.502081 0.091033 -0.029460 0.114 Uiso 1 1 calc R U . . . C64 C 0.3651(4) 0.2952(6) -0.07303(18) 0.0933(17) Uani 1 1 d . . . . . H64A H 0.291384 0.307035 -0.051248 0.140 Uiso 1 1 calc R U . . . H64B H 0.371592 0.239440 -0.096102 0.140 Uiso 1 1 calc R U . . . H64C H 0.355433 0.365627 -0.094660 0.140 Uiso 1 1 calc R U . . . C65 C 0.6820(4) 0.2578(5) -0.21654(14) 0.0743(12) Uani 1 1 d . . . . . C69 C 0.5786(11) 0.4796(8) 0.3498(5) 0.285(8) Uani 1 1 d D U . . . H69A H 0.504250 0.470295 0.336137 0.427 Uiso 1 1 calc R U . . . H69B H 0.566914 0.558095 0.342247 0.427 Uiso 1 1 calc R U . . . H69C H 0.589101 0.456157 0.388094 0.427 Uiso 1 1 calc R U . . . C70 C 0.6916(9) 0.4111(8) 0.3244(5) 0.237(6) Uani 1 1 d D U . . . C71 C 0.8175(19) 0.455(3) -0.0834(10) 0.259(12) Uani 0.5 1 d D U P . . C72 C 0.9545(17) 0.4242(18) -0.0875(10) 0.221(9) Uani 0.5 1 d D U P . . H72A H 0.972273 0.491776 -0.094796 0.331 Uiso 0.5 1 calc R U P . . H72B H 0.984320 0.379220 -0.116328 0.331 Uiso 0.5 1 calc DR U P . . H72C H 0.998353 0.380824 -0.054219 0.331 Uiso 0.5 1 calc R U P . . C73 C 0.7650(13) 0.4171(17) 0.1645(7) 0.185(8) Uani 0.5 1 d D U P . . C74 C 0.6569(16) 0.4026(18) 0.1418(9) 0.229(10) Uani 0.5 1 d D U P . . H74A H 0.672303 0.389252 0.105013 0.344 Uiso 0.5 1 calc R U P . . H74B H 0.580221 0.470001 0.142957 0.344 Uiso 0.5 1 calc R U P . . H74C H 0.645619 0.338664 0.162133 0.344 Uiso 0.5 1 calc R U P . . C66 C 0.7791(14) 0.1629(14) -0.2411(4) 0.090(5) Uani 0.413(10) 1 d . . P A 1 H66A H 0.772166 0.181873 -0.279662 0.136 Uiso 0.413(10) 1 calc R U P A 1 H66B H 0.763526 0.094755 -0.231319 0.136 Uiso 0.413(10) 1 calc R U P A 1 H66C H 0.864439 0.150784 -0.228238 0.136 Uiso 0.413(10) 1 calc R U P A 1 C67 C 0.7159(13) 0.3618(12) -0.2353(4) 0.083(4) Uani 0.413(10) 1 d . . P A 1 H67A H 0.698502 0.383186 -0.273465 0.124 Uiso 0.413(10) 1 calc R U P A 1 H67B H 0.805962 0.342649 -0.227012 0.124 Uiso 0.413(10) 1 calc R U P A 1 H67C H 0.664448 0.424230 -0.216921 0.124 Uiso 0.413(10) 1 calc R U P A 1 C68 C 0.5581(11) 0.2799(13) -0.2377(3) 0.070(4) Uani 0.413(10) 1 d . . P A 1 H68A H 0.555666 0.298076 -0.276266 0.105 Uiso 0.413(10) 1 calc R U P A 1 H68B H 0.495752 0.342995 -0.222864 0.105 Uiso 0.413(10) 1 calc R U P A 1 H68C H 0.538119 0.213850 -0.228643 0.105 Uiso 0.413(10) 1 calc R U P A 1 C66A C 0.8043(10) 0.2413(14) -0.2438(3) 0.105(4) Uani 0.587(10) 1 d . U P A 2 H66D H 0.787195 0.258112 -0.282152 0.158 Uiso 0.587(10) 1 calc R U P A 2 H66E H 0.864131 0.163800 -0.234710 0.158 Uiso 0.587(10) 1 calc R U P A 2 H66F H 0.840836 0.291306 -0.232252 0.158 Uiso 0.587(10) 1 calc R U P A 2 C67A C 0.5800(10) 0.3687(13) -0.2349(4) 0.124(5) Uani 0.587(10) 1 d . . P A 2 H67D H 0.562252 0.375384 -0.272916 0.186 Uiso 0.587(10) 1 calc R U P A 2 H67E H 0.607614 0.427720 -0.227893 0.186 Uiso 0.587(10) 1 calc R U P A 2 H67F H 0.502994 0.376028 -0.215945 0.186 Uiso 0.587(10) 1 calc R U P A 2 C68A C 0.6406(13) 0.1600(13) -0.2302(3) 0.122(4) Uani 0.587(10) 1 d . U P A 2 H68D H 0.627877 0.166368 -0.268518 0.183 Uiso 0.587(10) 1 calc R U P A 2 H68E H 0.561381 0.166716 -0.213156 0.183 Uiso 0.587(10) 1 calc R U P A 2 H68F H 0.707185 0.087410 -0.217115 0.183 Uiso 0.587(10) 1 calc R U P A 2 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 Ni1 0.0379(3) 0.0427(3) 0.0278(3) -0.0052(2) 0.0031(2) -0.0149(2) C1 0.0375(16) 0.0419(18) 0.0377(16) -0.0114(13) 0.0053(13) -0.0153(14) Ni2 0.0356(3) 0.0761(4) 0.0251(3) -0.0067(2) 0.0042(2) -0.0300(3) C2 0.0436(17) 0.0499(19) 0.0367(17) -0.0067(14) 0.0058(13) -0.0200(15) O1 0.0453(12) 0.0389(12) 0.0361(12) -0.0064(9) 0.0102(9) -0.0104(10) O2 0.0409(12) 0.0501(13) 0.0270(10) -0.0064(9) 0.0051(9) -0.0139(10) O3 0.0385(12) 0.0792(17) 0.0258(11) -0.0060(10) 0.0033(9) -0.0313(11) C3 0.0463(19) 0.062(2) 0.0394(18) -0.0107(15) 0.0111(14) -0.0207(16) O4 0.0380(12) 0.0913(19) 0.0270(11) -0.0030(11) 0.0019(9) -0.0304(12) C4 0.051(2) 0.055(2) 0.049(2) -0.0133(16) 0.0120(15) -0.0163(16) N1 0.0440(14) 0.0426(15) 0.0323(13) -0.0050(11) -0.0007(11) -0.0177(12) N2 0.0399(14) 0.0410(15) 0.0315(13) -0.0042(11) -0.0012(11) -0.0170(11) N3 0.0379(14) 0.084(2) 0.0328(14) -0.0036(13) 0.0022(11) -0.0372(15) N4 0.0369(14) 0.0686(19) 0.0334(14) -0.0041(12) 0.0025(11) -0.0288(13) N5 0.206(9) 0.270(11) 0.370(14) -0.090(10) 0.104(9) -0.142(8) C5 0.053(2) 0.046(2) 0.048(2) -0.0097(15) 0.0070(15) -0.0092(16) N6 0.263(14) 0.243(17) 0.265(17) -0.073(14) 0.048(13) -0.077(13) C6 0.0423(17) 0.0471(19) 0.0388(17) -0.0075(14) 0.0026(13) -0.0135(15) C7 0.0444(18) 0.055(2) 0.0392(18) -0.0034(15) 0.0085(14) -0.0115(16) N7 0.241(16) 0.255(17) 0.295(18) -0.047(14) -0.059(13) -0.113(13) C8 0.053(2) 0.050(2) 0.063(2) -0.0021(17) 0.0094(17) -0.0174(17) C10 0.073(3) 0.078(3) 0.048(2) 0.009(2) 0.015(2) -0.007(2) C9 0.050(2) 0.071(3) 0.049(2) -0.0032(18) -0.0014(16) -0.0153(18) C11 0.058(2) 0.067(3) 0.058(2) -0.0215(19) 0.0176(18) -0.0124(19) C12 0.099(4) 0.100(4) 0.064(3) -0.021(3) 0.037(3) 0.001(3) C13 0.060(2) 0.081(3) 0.096(3) -0.049(3) 0.018(2) -0.023(2) C15 0.0444(17) 0.0431(19) 0.0398(17) -0.0082(14) 0.0007(13) -0.0173(14) C14 0.052(2) 0.094(3) 0.095(3) -0.041(3) 0.026(2) -0.026(2) C16 0.052(2) 0.047(2) 0.052(2) -0.0046(16) 0.0005(16) -0.0065(16) C17 0.0484(18) 0.0452(19) 0.0354(17) -0.0004(14) -0.0007(13) -0.0167(15) C18 0.0513(19) 0.0472(19) 0.0342(17) 0.0007(14) -0.0018(14) -0.0202(15) C19 0.075(3) 0.067(3) 0.067(3) 0.000(2) -0.008(2) -0.044(2) C20 0.060(2) 0.066(3) 0.042(2) 0.0094(17) 0.0031(16) -0.0149(19) C21 0.0444(18) 0.053(2) 0.0289(16) -0.0033(14) 0.0012(13) -0.0209(15) C22 0.0379(16) 0.0527(19) 0.0264(15) -0.0076(13) 0.0007(12) -0.0178(14) C23 0.0472(18) 0.057(2) 0.0227(15) -0.0079(13) 0.0041(13) -0.0232(15) C24 0.0389(16) 0.056(2) 0.0271(15) -0.0133(13) 0.0039(12) -0.0218(15) C25 0.0393(16) 0.0480(19) 0.0315(16) -0.0097(13) 0.0004(12) -0.0170(14) C28 0.0465(18) 0.051(2) 0.0350(17) -0.0026(14) 0.0108(14) -0.0120(15) C27 0.0352(15) 0.0465(18) 0.0261(15) -0.0082(12) 0.0016(12) -0.0171(13) C26 0.0406(16) 0.0504(19) 0.0275(15) -0.0111(13) 0.0059(12) -0.0213(14) C29 0.080(3) 0.059(3) 0.062(3) 0.013(2) 0.031(2) 0.001(2) C30 0.052(2) 0.090(3) 0.0287(17) -0.0031(17) 0.0007(15) -0.026(2) C32 0.0407(16) 0.056(2) 0.0273(15) -0.0092(13) 0.0032(12) -0.0219(15) C31 0.060(2) 0.058(2) 0.047(2) -0.0060(16) 0.0158(16) -0.0284(18) C33 0.0441(18) 0.084(3) 0.0267(16) -0.0147(16) 0.0028(13) -0.0207(18) C34 0.0383(18) 0.094(3) 0.0340(18) -0.0112(18) -0.0010(14) -0.0173(18) C35 0.0393(17) 0.076(3) 0.0348(17) -0.0148(16) 0.0061(13) -0.0207(17) C36 0.0408(17) 0.055(2) 0.0269(15) -0.0102(13) 0.0033(12) -0.0243(15) C37 0.0371(16) 0.055(2) 0.0294(15) -0.0100(13) 0.0038(12) -0.0200(14) C38 0.0360(16) 0.063(2) 0.0249(15) -0.0110(14) 0.0037(12) -0.0231(15) C39 0.0321(15) 0.056(2) 0.0285(15) -0.0104(13) 0.0065(12) -0.0187(14) C40 0.0363(16) 0.056(2) 0.0293(15) -0.0100(14) 0.0089(12) -0.0208(15) C44 0.0320(16) 0.070(2) 0.0323(16) -0.0098(15) 0.0053(12) -0.0221(15) C43 0.0415(17) 0.069(2) 0.0287(16) -0.0103(14) 0.0057(13) -0.0291(16) C42 0.0384(17) 0.072(2) 0.0291(16) -0.0109(15) 0.0001(12) -0.0294(16) C41 0.0388(16) 0.053(2) 0.0283(15) -0.0122(13) 0.0055(12) -0.0192(14) C45 0.0376(18) 0.082(3) 0.048(2) -0.0077(18) 0.0017(15) -0.0205(18) C47 0.0387(18) 0.097(3) 0.0397(19) -0.0131(18) 0.0093(14) -0.0354(19) C46 0.0430(18) 0.086(3) 0.0410(19) -0.0205(18) 0.0033(14) -0.0327(18) C48 0.0446(19) 0.090(3) 0.0315(17) -0.0105(16) 0.0020(13) -0.0405(19) C49 0.052(2) 0.114(3) 0.0389(19) -0.0068(19) 0.0059(15) -0.057(2) C50 0.048(2) 0.187(5) 0.043(2) 0.001(3) 0.0005(17) -0.065(3) C52 0.0360(17) 0.095(3) 0.0375(18) -0.0017(17) 0.0036(13) -0.0350(19) C51 0.111(4) 0.131(4) 0.068(3) -0.029(3) 0.029(3) -0.092(3) C53 0.0427(17) 0.064(2) 0.0307(16) -0.0057(14) 0.0072(13) -0.0245(16) C54 0.049(2) 0.110(3) 0.0378(19) -0.013(2) 0.0114(16) -0.036(2) C55 0.0422(17) 0.077(3) 0.0305(16) -0.0090(15) 0.0033(13) -0.0306(17) C56 0.053(2) 0.092(3) 0.0279(16) -0.0032(17) 0.0047(14) -0.040(2) C57 0.060(2) 0.092(3) 0.0309(17) 0.0005(17) -0.0015(15) -0.042(2) C58 0.048(2) 0.092(3) 0.0348(18) 0.0029(18) -0.0061(15) -0.033(2) C59 0.0464(19) 0.087(3) 0.0347(17) -0.0036(17) -0.0002(14) -0.0340(19) C60 0.0423(17) 0.070(2) 0.0284(16) -0.0034(15) 0.0013(13) -0.0274(17) C61 0.044(2) 0.110(3) 0.040(2) -0.0030(19) 0.0005(15) -0.033(2) C62 0.061(3) 0.117(4) 0.065(3) -0.019(3) 0.010(2) -0.020(3) C63 0.057(2) 0.133(4) 0.049(2) 0.007(2) 0.0072(18) -0.055(3) C64 0.048(2) 0.168(5) 0.059(3) 0.001(3) -0.0036(19) -0.041(3) C65 0.076(3) 0.129(4) 0.0290(19) 0.000(2) -0.0009(17) -0.055(3) C69 0.292(13) 0.200(10) 0.322(14) 0.111(9) 0.099(10) -0.100(8) C70 0.229(8) 0.205(8) 0.272(9) 0.073(6) 0.071(7) -0.113(7) C71 0.273(13) 0.243(15) 0.264(16) -0.034(10) 0.012(10) -0.105(10) C72 0.271(14) 0.155(14) 0.246(18) -0.002(13) -0.030(14) -0.100(13) C73 0.185(11) 0.178(11) 0.196(12) -0.014(8) -0.002(8) -0.077(8) C74 0.247(17) 0.200(16) 0.272(19) -0.015(14) -0.034(13) -0.127(14) C66 0.093(8) 0.123(10) 0.033(5) -0.012(6) -0.011(5) -0.016(7) C67 0.103(9) 0.127(9) 0.032(5) 0.012(5) 0.001(5) -0.068(8) C68 0.074(6) 0.115(11) 0.024(4) 0.002(5) -0.009(4) -0.045(6) C66A 0.099(6) 0.182(12) 0.041(4) -0.002(6) 0.012(4) -0.067(7) C67A 0.094(7) 0.184(10) 0.070(6) 0.053(7) -0.023(5) -0.051(6) C68A 0.157(10) 0.201(10) 0.048(5) -0.023(6) -0.005(5) -0.112(9) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 '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 O1 Ni1 N2 177.94(10) O1 Ni1 O2 86.30(9) N2 Ni1 O2 93.12(10) O1 Ni1 N1 93.12(10) N2 Ni1 N1 87.43(11) O2 Ni1 N1 179.01(11) O1 C1 C6 122.6(3) O1 C1 C2 119.2(3) C6 C1 C2 118.2(3) O4 Ni2 N3 175.55(13) O4 Ni2 N4 93.82(10) N3 Ni2 N4 87.34(11) O4 Ni2 O3 85.71(9) N3 Ni2 O3 93.58(10) N4 Ni2 O3 174.00(12) C3 C2 C1 118.4(3) C3 C2 C7 121.1(3) C1 C2 C7 120.5(3) C1 O1 Ni1 128.8(2) C27 O2 Ni1 129.60(19) C38 O3 Ni2 129.33(19) C2 C3 C4 124.4(3) C2 C3 H3 117.8 C4 C3 H3 117.8 C60 O4 Ni2 128.47(19) C5 C4 C3 116.4(3) C5 C4 C11 121.2(3) C3 C4 C11 122.4(3) C15 N1 C17 119.6(3) C15 N1 Ni1 128.9(2) C17 N1 Ni1 111.3(2) C21 N2 C18 119.7(3) C21 N2 Ni1 127.0(2) C18 N2 Ni1 113.13(19) C48 N3 C49 119.5(3) C48 N3 Ni2 126.4(2) C49 N3 Ni2 113.7(2) C53 N4 C52 118.8(3) C53 N4 Ni2 128.8(2) C52 N4 Ni2 111.5(2) C4 C5 C6 123.3(3) C4 C5 H5 118.4 C6 C5 H5 118.4 C5 C6 C1 119.2(3) C5 C6 C15 119.2(3) C1 C6 C15 121.6(3) C2 C7 C9 109.9(3) C2 C7 C8 109.5(3) C9 C7 C8 111.4(3) C2 C7 C10 112.6(3) C9 C7 C10 107.0(3) C8 C7 C10 106.4(3) C7 C8 H8A 109.5 C7 C8 H8B 109.5 H8A C8 H8B 109.5 C7 C8 H8C 109.5 H8A C8 H8C 109.5 H8B C8 H8C 109.5 C7 C10 H10A 109.5 C7 C10 H10B 109.5 H10A C10 H10B 109.5 C7 C10 H10C 109.5 H10A C10 H10C 109.5 H10B C10 H10C 109.5 C7 C9 H9A 109.5 C7 C9 H9B 109.5 H9A C9 H9B 109.5 C7 C9 H9C 109.5 H9A C9 H9C 109.5 H9B C9 H9C 109.5 C13 C11 C12 108.1(4) C13 C11 C4 109.1(3) C12 C11 C4 112.7(3) C13 C11 C14 110.1(4) C12 C11 C14 108.4(4) C4 C11 C14 108.4(3) C11 C12 H12A 109.5 C11 C12 H12B 109.5 H12A C12 H12B 109.5 C11 C12 H12C 109.5 H12A C12 H12C 109.5 H12B C12 H12C 109.5 C11 C13 H13A 109.5 C11 C13 H13B 109.5 H13A C13 H13B 109.5 C11 C13 H13C 109.5 H13A C13 H13C 109.5 H13B C13 H13C 109.5 N1 C15 C6 122.0(3) N1 C15 C16 119.4(3) C6 C15 C16 118.6(3) C11 C14 H14A 109.5 C11 C14 H14B 109.5 H14A C14 H14B 109.5 C11 C14 H14C 109.5 H14A C14 H14C 109.5 H14B C14 H14C 109.5 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 N1 C17 C18 109.2(3) N1 C17 H17A 109.8 C18 C17 H17A 109.8 N1 C17 H17B 109.8 C18 C17 H17B 109.8 H17A C17 H17B 108.3 N2 C18 C17 104.6(2) N2 C18 C20 114.4(3) C17 C18 C20 109.6(3) N2 C18 C19 106.3(3) C17 C18 C19 110.8(3) C20 C18 C19 110.9(3) C18 C19 H19A 109.5 C18 C19 H19B 109.5 H19A C19 H19B 109.5 C18 C19 H19C 109.5 H19A C19 H19C 109.5 H19B C19 H19C 109.5 C18 C20 H20A 109.5 C18 C20 H20B 109.5 H20A C20 H20B 109.5 C18 C20 H20C 109.5 H20A C20 H20C 109.5 H20B C20 H20C 109.5 N2 C21 C22 126.2(3) N2 C21 H21 116.9 C22 C21 H21 116.9 C23 C22 C27 121.1(3) C23 C22 C21 117.6(3) C27 C22 C21 120.7(3) C24 C23 C22 121.7(3) C24 C23 H23 119.2 C22 C23 H23 119.2 C23 C24 C25 116.8(3) C23 C24 C32 121.8(3) C25 C24 C32 121.3(3) C26 C25 C24 124.7(3) C26 C25 H25 117.6 C24 C25 H25 117.6 C31 C28 C30 110.8(3) C31 C28 C26 111.1(3) C30 C28 C26 108.1(3) C31 C28 C29 106.0(3) C30 C28 C29 109.2(3) C26 C28 C29 111.7(3) O2 C27 C22 122.2(3) O2 C27 C26 120.4(3) C22 C27 C26 117.3(3) C25 C26 C27 118.3(3) C25 C26 C28 120.6(3) C27 C26 C28 121.1(3) 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 C28 C30 H30A 109.5 C28 C30 H30B 109.5 H30A C30 H30B 109.5 C28 C30 H30C 109.5 H30A C30 H30C 109.5 H30B C30 H30C 109.5 C33 C32 C37 118.0(3) C33 C32 C24 121.1(3) C37 C32 C24 120.9(3) C28 C31 H31A 109.5 C28 C31 H31B 109.5 H31A C31 H31B 109.5 C28 C31 H31C 109.5 H31A C31 H31C 109.5 H31B C31 H31C 109.5 C34 C33 C32 120.5(3) C34 C33 H33 119.7 C32 C33 H33 119.7 C35 C34 C33 120.8(3) C35 C34 H34 119.6 C33 C34 H34 119.6 C34 C35 C36 120.2(3) C34 C35 H35 119.9 C36 C35 H35 119.9 C37 C36 C35 118.2(3) C37 C36 C41 120.5(3) C35 C36 C41 121.3(3) C36 C37 C32 122.3(3) C36 C37 H37 118.8 C32 C37 H37 118.8 O3 C38 C43 122.4(3) O3 C38 C39 120.4(3) C43 C38 C39 117.2(3) C40 C39 C38 117.7(3) C40 C39 C44 121.6(3) C38 C39 C44 120.7(3) C39 C40 C41 125.3(3) C39 C40 H40 117.4 C41 C40 H40 117.4 C45 C44 C46 110.7(3) C45 C44 C47 108.6(3) C46 C44 C47 107.0(3) C45 C44 C39 108.6(3) C46 C44 C39 110.7(3) C47 C44 C39 111.4(3) C42 C43 C38 121.4(3) C42 C43 C48 117.8(3) C38 C43 C48 120.8(3) C41 C42 C43 121.5(3) C41 C42 H42 119.3 C43 C42 H42 119.3 C42 C41 C40 116.7(3) C42 C41 C36 122.4(3) C40 C41 C36 121.0(3) 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 C44 C47 H47A 109.5 C44 C47 H47B 109.5 H47A C47 H47B 109.5 C44 C47 H47C 109.5 H47A C47 H47C 109.5 H47B C47 H47C 109.5 C44 C46 H46A 109.5 C44 C46 H46B 109.5 H46A C46 H46B 109.5 C44 C46 H46C 109.5 H46A C46 H46C 109.5 H46B C46 H46C 109.5 N3 C48 C43 127.0(3) N3 C48 H48 116.5 C43 C48 H48 116.5 N3 C49 C52 104.8(3) N3 C49 C50 112.9(3) C52 C49 C50 108.6(4) N3 C49 C51 106.9(3) C52 C49 C51 110.8(3) C50 C49 C51 112.6(4) C49 C50 H50A 109.5 C49 C50 H50B 109.5 H50A C50 H50B 109.5 C49 C50 H50C 109.5 H50A C50 H50C 109.5 H50B C50 H50C 109.5 N4 C52 C49 109.2(3) N4 C52 H52A 109.8 C49 C52 H52A 109.8 N4 C52 H52B 109.8 C49 C52 H52B 109.8 H52A C52 H52B 108.3 C49 C51 H51A 109.5 C49 C51 H51B 109.5 H51A C51 H51B 109.5 C49 C51 H51C 109.5 H51A C51 H51C 109.5 H51B C51 H51C 109.5 N4 C53 C55 121.9(3) N4 C53 C54 119.4(3) C55 C53 C54 118.7(3) C53 C54 H54A 109.5 C53 C54 H54B 109.5 H54A C54 H54B 109.5 C53 C54 H54C 109.5 H54A C54 H54C 109.5 H54B C54 H54C 109.5 C60 C55 C56 118.9(3) C60 C55 C53 122.2(3) C56 C55 C53 118.9(3) C57 C56 C55 123.3(3) C57 C56 H56 118.4 C55 C56 H56 118.4 C56 C57 C58 116.6(3) C56 C57 C65 122.5(3) C58 C57 C65 120.9(3) C59 C58 C57 124.3(3) C59 C58 H58 117.9 C57 C58 H58 117.9 C58 C59 C60 118.3(3) C58 C59 C61 120.9(3) C60 C59 C61 120.8(3) O4 C60 C55 123.4(3) O4 C60 C59 118.0(3) C55 C60 C59 118.6(3) C63 C61 C62 111.0(4) C63 C61 C64 106.8(4) C62 C61 C64 108.9(4) C63 C61 C59 109.2(4) C62 C61 C59 109.4(3) C64 C61 C59 111.5(3) C61 C62 H62A 109.5 C61 C62 H62B 109.5 H62A C62 H62B 109.5 C61 C62 H62C 109.5 H62A C62 H62C 109.5 H62B C62 H62C 109.5 C61 C63 H63A 109.5 C61 C63 H63B 109.5 H63A C63 H63B 109.5 C61 C63 H63C 109.5 H63A C63 H63C 109.5 H63B C63 H63C 109.5 C61 C64 H64A 109.5 C61 C64 H64B 109.5 H64A C64 H64B 109.5 C61 C64 H64C 109.5 H64A C64 H64C 109.5 H64B C64 H64C 109.5 C67A C65 C66A 112.3(8) C68 C65 C66 109.5(8) C68 C65 C57 116.7(5) C67A C65 C57 110.9(6) C66A C65 C57 112.5(5) C66 C65 C57 111.3(6) C68 C65 C67 108.5(8) C66 C65 C67 104.8(10) C57 C65 C67 105.3(5) C67A C65 C68A 110.1(8) C66A C65 C68A 106.2(8) C57 C65 C68A 104.5(5) C70 C69 H69A 109.5 C70 C69 H69B 109.5 H69A C69 H69B 109.5 C70 C69 H69C 109.5 H69A C69 H69C 109.5 H69B C69 H69C 109.5 N5 C70 C69 169.2(8) N6 C71 C72 167(2) C71 C72 H72A 109.5 C71 C72 H72B 109.5 H72A C72 H72B 109.5 C71 C72 H72C 109.5 H72A C72 H72C 109.5 H72B C72 H72C 109.5 N7 C73 C74 174.8(15) C73 C74 H74A 109.5 C73 C74 H74B 109.5 H74A C74 H74B 109.5 C73 C74 H74C 109.5 H74A C74 H74C 109.5 H74B C74 H74C 109.5 C65 C66 H66A 109.5 C65 C66 H66B 109.5 H66A C66 H66B 109.5 C65 C66 H66C 109.5 H66A C66 H66C 109.5 H66B C66 H66C 109.5 C65 C67 H67A 109.5 C65 C67 H67B 109.5 H67A C67 H67B 109.5 C65 C67 H67C 109.5 H67A C67 H67C 109.5 H67B C67 H67C 109.5 C65 C68 H68A 109.5 C65 C68 H68B 109.5 H68A C68 H68B 109.5 C65 C68 H68C 109.5 H68A C68 H68C 109.5 H68B C68 H68C 109.5 C65 C66A H66D 109.5 C65 C66A H66E 109.5 H66D C66A H66E 109.5 C65 C66A H66F 109.5 H66D C66A H66F 109.5 H66E C66A H66F 109.5 C65 C67A H67D 109.5 C65 C67A H67E 109.5 H67D C67A H67E 109.5 C65 C67A H67F 109.5 H67D C67A H67F 109.5 H67E C67A H67F 109.5 C65 C68A H68D 109.5 C65 C68A H68E 109.5 H68D C68A H68E 109.5 C65 C68A H68F 109.5 H68D C68A H68F 109.5 H68E C68A H68F 109.5 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Ni1 O1 1.832(2) Ni1 N2 1.845(2) Ni1 O2 1.854(2) Ni1 N1 1.859(3) C1 O1 1.311(4) C1 C6 1.422(5) C1 C2 1.433(4) Ni2 O4 1.832(2) Ni2 N3 1.851(3) Ni2 N4 1.855(3) Ni2 O3 1.859(2) C2 C3 1.376(5) C2 C7 1.531(5) O2 C27 1.306(4) O3 C38 1.306(4) C3 C4 1.397(5) C3 H3 0.9500 O4 C60 1.311(4) C4 C5 1.369(5) C4 C11 1.537(5) N1 C15 1.306(4) N1 C17 1.477(4) N2 C21 1.286(4) N2 C18 1.487(4) N3 C48 1.280(4) N3 C49 1.492(4) N4 C53 1.304(4) N4 C52 1.481(4) N5 C70 1.1645(10) C5 C6 1.405(5) C5 H5 0.9500 N6 C71 1.170(5) C6 C15 1.457(5) C7 C9 1.531(5) C7 C8 1.532(5) C7 C10 1.536(5) N7 C73 1.1608(10) C8 H8A 0.9800 C8 H8B 0.9800 C8 H8C 0.9800 C10 H10A 0.9800 C10 H10B 0.9800 C10 H10C 0.9800 C9 H9A 0.9800 C9 H9B 0.9800 C9 H9C 0.9800 C11 C13 1.517(6) C11 C12 1.519(6) C11 C14 1.538(6) C12 H12A 0.9800 C12 H12B 0.9800 C12 H12C 0.9800 C13 H13A 0.9800 C13 H13B 0.9800 C13 H13C 0.9800 C15 C16 1.515(5) C14 H14A 0.9800 C14 H14B 0.9800 C14 H14C 0.9800 C16 H16A 0.9800 C16 H16B 0.9800 C16 H16C 0.9800 C17 C18 1.509(5) C17 H17A 0.9900 C17 H17B 0.9900 C18 C20 1.528(5) C18 C19 1.538(5) C19 H19A 0.9800 C19 H19B 0.9800 C19 H19C 0.9800 C20 H20A 0.9800 C20 H20B 0.9800 C20 H20C 0.9800 C21 C22 1.426(5) C21 H21 0.9500 C22 C23 1.409(4) C22 C27 1.426(4) C23 C24 1.364(5) C23 H23 0.9500 C24 C25 1.409(4) C24 C32 1.492(4) C25 C26 1.382(4) C25 H25 0.9500 C28 C31 1.530(5) C28 C30 1.531(5) C28 C26 1.532(4) C28 C29 1.534(5) C27 C26 1.430(5) C29 H29A 0.9800 C29 H29B 0.9800 C29 H29C 0.9800 C30 H30A 0.9800 C30 H30B 0.9800 C30 H30C 0.9800 C32 C33 1.386(5) C32 C37 1.397(4) C31 H31A 0.9800 C31 H31B 0.9800 C31 H31C 0.9800 C33 C34 1.384(5) C33 H33 0.9500 C34 C35 1.380(5) C34 H34 0.9500 C35 C36 1.394(5) C35 H35 0.9500 C36 C37 1.389(4) C36 C41 1.489(4) C37 H37 0.9500 C38 C43 1.419(4) C38 C39 1.441(4) C39 C40 1.381(4) C39 C44 1.538(4) C40 C41 1.400(4) C40 H40 0.9500 C44 C45 1.523(5) C44 C46 1.527(5) C44 C47 1.533(4) C43 C42 1.408(4) C43 C48 1.423(4) C42 C41 1.370(4) C42 H42 0.9500 C45 H45A 0.9800 C45 H45B 0.9800 C45 H45C 0.9800 C47 H47A 0.9800 C47 H47B 0.9800 C47 H47C 0.9800 C46 H46A 0.9800 C46 H46B 0.9800 C46 H46C 0.9800 C48 H48 0.9500 C49 C52 1.512(5) C49 C50 1.519(6) C49 C51 1.520(7) C50 H50A 0.9800 C50 H50B 0.9800 C50 H50C 0.9800 C52 H52A 0.9900 C52 H52B 0.9900 C51 H51A 0.9800 C51 H51B 0.9800 C51 H51C 0.9800 C53 C55 1.450(5) C53 C54 1.513(4) C54 H54A 0.9800 C54 H54B 0.9800 C54 H54C 0.9800 C55 C60 1.413(4) C55 C56 1.422(5) C56 C57 1.359(5) C56 H56 0.9500 C57 C58 1.406(5) C57 C65 1.533(5) C58 C59 1.375(5) C58 H58 0.9500 C59 C60 1.440(5) C59 C61 1.547(5) C61 C63 1.511(6) C61 C62 1.530(7) C61 C64 1.542(6) C62 H62A 0.9800 C62 H62B 0.9800 C62 H62C 0.9800 C63 H63A 0.9800 C63 H63B 0.9800 C63 H63C 0.9800 C64 H64A 0.9800 C64 H64B 0.9800 C64 H64C 0.9800 C65 C68 1.430(11) C65 C67A 1.490(13) C65 C66A 1.511(10) C65 C66 1.518(14) C65 C67 1.576(13) C65 C68A 1.609(13) C69 C70 1.4630(10) C69 H69A 0.9800 C69 H69B 0.9800 C69 H69C 0.9800 C71 C72 1.467(5) C72 H72A 0.9800 C72 H72B 0.9800 C72 H72C 0.9800 C73 C74 1.4609(10) C74 H74A 0.9800 C74 H74B 0.9800 C74 H74C 0.9800 C66 H66A 0.9800 C66 H66B 0.9800 C66 H66C 0.9800 C67 H67A 0.9800 C67 H67B 0.9800 C67 H67C 0.9800 C68 H68A 0.9800 C68 H68B 0.9800 C68 H68C 0.9800 C66A H66D 0.9800 C66A H66E 0.9800 C66A H66F 0.9800 C67A H67D 0.9800 C67A H67E 0.9800 C67A H67F 0.9800 C68A H68D 0.9800 C68A H68E 0.9800 C68A H68F 0.9800