#------------------------------------------------------------------------------ #$Date: 2020-04-24 04:34:37 +0300 (Fri, 24 Apr 2020) $ #$Revision: 251124 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/24/03/7240393.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_7240393 loop_ _publ_author_name 'Kyoden, Yukiya' 'Ishida, Takayuki' _publ_section_title ; An indication of spin-transition accompanied by an order-disorder structural transformation in [Ni(phpyNO)2(NCS)2] (phpyNO = tert-butyl 5-phenyl-2-pyridyl nitroxide) ; _journal_issue 27 _journal_name_full 'RSC Advances' _journal_page_first 16009 _journal_paper_doi 10.1039/D0RA02041A _journal_volume 10 _journal_year 2020 _chemical_formula_moiety 'C32 H34 N6 Ni O2 S2' _chemical_formula_sum 'C32 H34 N6 Ni O2 S2' _chemical_formula_weight 657.48 _chemical_name_systematic '[Ni(phpyNO)2(NCS)2]' _space_group_crystal_system orthorhombic _space_group_IT_number 61 _space_group_name_Hall '-P 2ac 2ab' _space_group_name_H-M_alt 'P b c a' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_block_doi 10.5517/ccdc.csd.cc24lhpy _audit_update_record ; 2020-02-14 deposited with the CCDC. 2020-04-06 downloaded from the CCDC. ; _cell_angle_alpha 90.0000 _cell_angle_beta 90.0000 _cell_angle_gamma 90.0000 _cell_formula_units_Z 8 _cell_length_a 17.0732(19) _cell_length_b 19.194(3) _cell_length_c 20.667(3) _cell_measurement_reflns_used 25622 _cell_measurement_temperature 400 _cell_measurement_theta_max 27.56 _cell_measurement_theta_min 3.10 _cell_volume 6772.6(16) _computing_cell_refinement PROCESS-AUTO _computing_data_collection PROCESS-AUTO _computing_data_reduction PROCESS-AUTO _computing_molecular_graphics 'CrystalStructure 4.2.1' _computing_publication_material 'CrystalStructure 4.2.1 (Rigaku, 2016)' _computing_structure_refinement 'SHELXL Version 2014/7 (Sheldrick, 2008)' _computing_structure_solution 'Superflip (Palatinus, et al., 2007)' _diffrn_ambient_temperature 400 _diffrn_detector_area_resol_mean 29.412 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_device_type 'Rigaku Saturn70' _diffrn_measurement_method \w _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.1293 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_number 75566 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 26.596 _diffrn_reflns_theta_min 3.095 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.733 _exptl_absorpt_correction_T_max 0.878 _exptl_absorpt_correction_T_min 0.725 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'REQAB (Rigaku, 1998)' _exptl_crystal_colour Blue _exptl_crystal_density_diffrn 1.290 _exptl_crystal_density_method 'not measured' _exptl_crystal_description Block _exptl_crystal_F_000 2752.00 _exptl_crystal_preparation 'Magnetic properties' _exptl_crystal_recrystallization_method 'Re-crystallisation from solvent' _exptl_crystal_size_max 0.415 _exptl_crystal_size_mid 0.257 _exptl_crystal_size_min 0.177 _refine_diff_density_max 0.18 _refine_diff_density_min -0.27 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.015 _refine_ls_hydrogen_treatment constr _refine_ls_number_parameters 416 _refine_ls_number_reflns 7078 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1954 _refine_ls_R_factor_gt 0.0698 _refine_ls_shift/su_max 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.0514P)^2^+2.6054P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1227 _refine_ls_wR_factor_ref 0.1563 _reflns_Friedel_coverage 0.000 _reflns_number_gt 3016 _reflns_number_total 7078 _reflns_threshold_expression F^2^>2.0\s(F^2^) _cod_data_source_file d0ra02041a1.cif _cod_data_source_block phpyNO_Ni_NCS2_400K _cod_original_cell_volume 6772.7(16) _cod_database_code 7240393 _shelx_res_file ; shelxl.res created by SHELXL-2014/7 TITL User-defined CELL 0.71073 17.07320 19.19400 20.66720 90.000 90.000 90.000 ZERR 8 0.00190 0.00300 0.00280 0.000 0.000 0.000 LATT 1 SYMM 1/2+X, 1/2-Y, -Z SYMM -X, 1/2+Y, 1/2-Z SYMM 1/2-X, -Y, 1/2+Z SFAC C H N NI O S UNIT 256 272 48 8 16 16 SHEL 99999.000000 0.793652 L.S. 20 FMAP 2 PLAN -55 WPDB -2 BOND $H CONF LIST 4 TEMP 127.0 ACTA SIZE 0.415 0.257 0.177 REM HTAB HTAB WGHT 0.051400 2.605400 FVAR 0.41847 0.60929 PART 0 NI1 4 0.433670 0.469609 0.767391 11.00000 0.06760 0.08569 = 0.10522 0.00706 0.01210 0.01311 S1 6 0.407751 0.310159 0.936695 11.00000 0.21671 0.14481 = 0.15655 0.05316 -0.00765 -0.00163 S2 6 0.321270 0.277680 0.666599 11.00000 0.16061 0.12048 = 0.20211 -0.01572 0.01549 -0.03550 O1 5 0.433020 0.543781 0.696524 11.00000 0.12405 0.08863 = 0.10417 0.01181 0.03683 0.02245 O2 5 0.518089 0.527148 0.815121 11.00000 0.09407 0.10629 = 0.15078 -0.03036 -0.00574 0.02062 N1 3 0.406472 0.603401 0.714750 11.00000 0.08033 0.07812 = 0.08754 0.00566 0.01031 0.00756 N2 3 0.352833 0.541595 0.799022 11.00000 0.06949 0.08042 = 0.08607 0.00711 0.01125 0.01081 N3 3 0.584958 0.495897 0.818781 11.00000 0.07587 0.08939 = 0.11063 -0.00294 -0.00166 0.00298 N4 3 0.537811 0.428988 0.735726 11.00000 0.05828 0.08270 = 0.09671 0.00117 0.00238 0.00705 N5 3 0.425158 0.406770 0.844058 11.00000 0.13134 0.10545 = 0.12499 0.02980 0.02107 0.03148 N6 3 0.365808 0.405785 0.712717 11.00000 0.06380 0.10973 = 0.14281 -0.00667 0.00638 -0.00253 C1 1 0.352599 0.602057 0.766658 11.00000 0.06373 0.08203 = 0.08147 0.00151 0.00661 0.00554 C2 1 0.300693 0.654370 0.781888 11.00000 0.08958 0.07462 = 0.10058 0.00902 0.01630 0.00822 AFIX 43 H2 2 0.299808 0.695513 0.758132 11.00000 -1.20000 AFIX 0 C3 1 0.249832 0.644618 0.833215 11.00000 0.08246 0.07265 = 0.10520 -0.00087 0.01159 0.01453 AFIX 43 H3 2 0.215016 0.679903 0.844341 11.00000 -1.20000 AFIX 0 C4 1 0.249960 0.583613 0.868006 11.00000 0.06568 0.07355 = 0.08221 -0.01305 0.00161 0.00355 C5 1 0.303558 0.534058 0.848154 11.00000 0.07885 0.08085 = 0.08606 0.00880 0.01004 0.00855 AFIX 43 H5 2 0.305198 0.492306 0.870946 11.00000 -1.20000 AFIX 0 C6 1 0.197076 0.570524 0.923309 11.00000 0.06904 0.07768 = 0.08048 -0.00839 0.00360 -0.00230 C7 1 0.167981 0.622951 0.960375 11.00000 0.09811 0.09709 = 0.10629 -0.01994 0.01930 0.00186 AFIX 43 H7 2 0.180785 0.668769 0.950258 11.00000 -1.20000 AFIX 0 C8 1 0.119850 0.609879 1.012717 11.00000 0.12200 0.14257 = 0.11196 -0.02862 0.03499 0.01260 AFIX 43 H8 2 0.101054 0.646618 1.037608 11.00000 -1.20000 AFIX 0 C9 1 0.100082 0.543509 1.027727 11.00000 0.12981 0.16480 = 0.09604 0.00025 0.03732 -0.00381 AFIX 43 H9 2 0.067731 0.534466 1.062942 11.00000 -1.20000 AFIX 0 C10 1 0.127510 0.490728 0.991404 11.00000 0.17976 0.10938 = 0.13456 -0.00007 0.06503 -0.01611 AFIX 43 H10 2 0.114075 0.445030 1.001431 11.00000 -1.20000 AFIX 0 C11 1 0.175506 0.504381 0.939348 11.00000 0.13446 0.09834 = 0.10849 -0.00787 0.05201 0.00134 AFIX 43 H11 2 0.193705 0.467414 0.914444 11.00000 -1.20000 AFIX 0 C12 1 0.444561 0.664621 0.683079 11.00000 0.11007 0.08572 = 0.10066 0.00290 0.02795 -0.01346 C16 1 0.601148 0.448128 0.769757 11.00000 0.06772 0.07308 = 0.09190 0.00460 0.00150 0.00257 C17 1 0.675118 0.423343 0.754975 11.00000 0.05914 0.10654 = 0.11595 -0.00840 -0.00704 0.00436 AFIX 43 H17 2 0.718542 0.437371 0.778814 11.00000 -1.20000 AFIX 0 C18 1 0.682890 0.378134 0.704943 11.00000 0.06244 0.09816 = 0.11794 0.00055 0.00435 0.01539 AFIX 43 H18 2 0.732250 0.360457 0.695317 11.00000 -1.20000 AFIX 0 C19 1 0.619704 0.357578 0.667882 11.00000 0.06640 0.07172 = 0.09822 0.01060 0.00178 0.01067 C20 1 0.548039 0.385747 0.686430 11.00000 0.06923 0.08327 = 0.09470 0.00725 -0.00384 0.00559 AFIX 43 H20 2 0.504088 0.373324 0.662483 11.00000 -1.20000 AFIX 0 C21 1 0.626151 0.310353 0.612996 11.00000 0.10905 0.07856 = 0.10109 -0.00244 -0.01356 0.01858 C22 1 0.692719 0.308988 0.574307 11.00000 0.12646 0.11507 = 0.11952 -0.00019 0.01549 0.04853 AFIX 43 H22 2 0.734512 0.338398 0.583625 11.00000 -1.20000 AFIX 0 C23 1 0.697169 0.264507 0.522432 11.00000 0.21340 0.14181 = 0.11893 -0.02088 0.00787 0.09307 AFIX 43 H23 2 0.741539 0.264693 0.496329 11.00000 -1.20000 AFIX 0 C24 1 0.638235 0.220902 0.509107 11.00000 0.27149 0.13152 = 0.14823 -0.04459 -0.07423 0.06046 AFIX 43 H24 2 0.642096 0.190475 0.474232 11.00000 -1.20000 AFIX 0 C25 1 0.572015 0.220987 0.546852 11.00000 0.19282 0.16767 = 0.17715 -0.03132 -0.06070 0.00291 AFIX 43 H25 2 0.531259 0.190396 0.537677 11.00000 -1.20000 AFIX 0 C26 1 0.565878 0.266396 0.598361 11.00000 0.14040 0.12201 = 0.12444 -0.03019 -0.03049 0.01510 AFIX 43 H26 2 0.520471 0.267048 0.623210 11.00000 -1.20000 AFIX 0 C27 1 0.634033 0.512569 0.877014 11.00000 0.11607 0.11482 = 0.10158 -0.01154 -0.01217 -0.00120 C28 1 0.584139 0.550181 0.922888 11.00000 0.22322 0.37579 = 0.16241 -0.14477 -0.04789 0.10181 AFIX 33 H28A 2 0.613930 0.561641 0.960818 11.00000 -1.20000 H28B 2 0.565270 0.592198 0.903091 11.00000 -1.20000 H28C 2 0.540519 0.521354 0.934819 11.00000 -1.20000 AFIX 0 C29 1 0.661067 0.444894 0.907134 11.00000 0.21703 0.17930 = 0.13121 0.03282 -0.04258 0.01712 AFIX 33 H29A 2 0.693759 0.420283 0.877037 11.00000 -1.20000 H29B 2 0.690258 0.454653 0.945787 11.00000 -1.20000 H29C 2 0.616343 0.416795 0.917697 11.00000 -1.20000 AFIX 0 C30 1 0.704017 0.555370 0.856289 11.00000 0.18902 0.18596 = 0.22224 0.00063 -0.04537 -0.09080 AFIX 33 H30A 2 0.735132 0.528989 0.826345 11.00000 -1.20000 H30B 2 0.686344 0.597425 0.835818 11.00000 -1.20000 H30C 2 0.735009 0.566873 0.893545 11.00000 -1.20000 AFIX 0 C31 1 0.418468 0.367777 0.881673 11.00000 0.08778 0.08023 = 0.08851 0.01230 -0.00124 0.02627 C32 1 0.347290 0.352506 0.693932 11.00000 0.06199 0.10860 = 0.12369 0.01096 0.01127 0.00257 PART 1 C13A 1 0.466775 0.716394 0.734228 21.00000 0.17768 0.14499 = 0.19875 -0.04945 0.04089 -0.07794 AFIX 33 H13A 2 0.420573 0.731566 0.756640 21.00000 -1.20000 H13B 2 0.502144 0.695006 0.764383 21.00000 -1.20000 H13C 2 0.491829 0.755755 0.714403 21.00000 -1.20000 AFIX 0 C14A 1 0.513330 0.638928 0.646459 21.00000 0.14385 0.14774 = 0.22413 -0.02097 0.11000 -0.03323 AFIX 33 H14A 2 0.538878 0.677411 0.625605 21.00000 -1.20000 H14B 2 0.549258 0.616719 0.675635 21.00000 -1.20000 H14C 2 0.496418 0.606005 0.614404 21.00000 -1.20000 AFIX 0 C15A 1 0.384492 0.695363 0.637488 21.00000 0.21086 0.22369 = 0.13301 0.10493 0.00747 0.02837 AFIX 33 H15A 2 0.340335 0.711768 0.661878 21.00000 -1.20000 H15B 2 0.407432 0.733528 0.614203 21.00000 -1.20000 H15C 2 0.367584 0.660305 0.607447 21.00000 -1.20000 AFIX 0 PART 2 C13B 1 0.532318 0.664941 0.708124 -21.00000 0.10116 0.13864 = 0.22242 0.02050 -0.04429 -0.04372 AFIX 33 H13D 2 0.555439 0.620047 0.700747 -21.00000 -1.20000 H13E 2 0.561572 0.699803 0.685203 -21.00000 -1.20000 H13F 2 0.533088 0.675168 0.753588 -21.00000 -1.20000 AFIX 0 C14B 1 0.448261 0.650862 0.611041 -21.00000 0.18292 0.12156 = 0.09404 0.01920 0.02235 -0.04026 AFIX 33 H14D 2 0.470723 0.605730 0.603524 -21.00000 -1.20000 H14E 2 0.396352 0.652334 0.593240 -21.00000 -1.20000 H14F 2 0.480056 0.685794 0.590661 -21.00000 -1.20000 AFIX 0 C15B 1 0.409795 0.734494 0.694907 -21.00000 0.12636 0.08552 = 0.15887 0.01857 0.04299 -0.01426 AFIX 33 H15D 2 0.439431 0.769134 0.672031 -21.00000 -1.20000 H15E 2 0.356578 0.734968 0.679918 -21.00000 -1.20000 H15F 2 0.410931 0.744494 0.740410 -21.00000 -1.20000 AFIX 0 HKLF 4 REM User-defined REM R1 = 0.0698 for 3016 Fo > 4sig(Fo) and 0.1954 for all 7078 data REM 416 parameters refined using 0 restraints END WGHT 0.0515 2.5981 REM Instructions for potential hydrogen bonds HTAB C5 N5 EQIV $1 x+1/2, y, -z+3/2 HTAB C17 N6_$1 HTAB C20 N6 EQIV $2 -x+1, y+1/2, -z+3/2 HTAB C14A S1_$2 REM Highest difference peak 0.180, deepest hole -0.271, 1-sigma level 0.033 Q1 1 0.2817 0.3153 0.6516 11.00000 0.05 0.18 Q2 1 0.3835 0.2861 0.8889 11.00000 0.05 0.18 Q3 1 0.4685 0.3330 0.9389 11.00000 0.05 0.18 Q4 1 0.3593 0.3603 0.9500 11.00000 0.05 0.16 Q5 1 0.3825 0.4723 0.7635 11.00000 0.05 0.16 Q6 1 0.7225 0.4755 0.8815 11.00000 0.05 0.15 Q7 1 0.4524 0.4184 0.8917 11.00000 0.05 0.13 Q8 1 0.6250 0.6081 0.8616 11.00000 0.05 0.13 Q9 1 0.4439 0.4883 0.8117 11.00000 0.05 0.13 Q10 1 0.3320 0.2790 0.7197 11.00000 0.05 0.12 Q11 1 0.4660 0.5505 0.7401 11.00000 0.05 0.12 Q12 1 0.4251 0.4079 0.7013 11.00000 0.05 0.12 Q13 1 0.5213 0.5676 0.8326 11.00000 0.05 0.12 Q14 1 0.5302 0.7282 0.7287 11.00000 0.05 0.11 Q15 1 0.3615 0.2713 0.6411 11.00000 0.05 0.11 Q16 1 0.6223 0.7033 0.7043 11.00000 0.05 0.11 Q17 1 0.3449 0.2626 0.6498 11.00000 0.05 0.11 Q18 1 0.1547 0.6633 0.9278 11.00000 0.05 0.11 Q19 1 0.5983 0.5413 0.9606 11.00000 0.05 0.11 Q20 1 0.5349 0.5479 0.9396 11.00000 0.05 0.11 Q21 1 0.5619 0.1712 0.5007 11.00000 0.05 0.11 Q22 1 0.4365 0.5248 0.6792 11.00000 0.05 0.11 Q23 1 0.5824 0.5767 0.9207 11.00000 0.05 0.11 Q24 1 0.4990 0.4272 0.7296 11.00000 0.05 0.11 Q25 1 0.5183 0.3871 0.6392 11.00000 0.05 0.10 Q26 1 0.3812 0.3926 0.7597 11.00000 0.05 0.10 Q27 1 0.6964 0.5670 0.7988 11.00000 0.05 0.10 Q28 1 0.3407 0.4013 0.6869 11.00000 0.05 0.10 Q29 1 0.2964 0.6116 0.7640 11.00000 0.05 0.10 Q30 1 0.3558 0.4069 0.6763 11.00000 0.05 0.10 Q31 1 0.4357 0.4228 0.7793 11.00000 0.05 0.10 Q32 1 0.4299 0.6381 0.7008 11.00000 0.05 0.10 Q33 1 0.7004 0.4769 0.7711 11.00000 0.05 0.10 Q34 1 0.3465 0.3554 0.7295 11.00000 0.05 0.10 Q35 1 0.3770 0.4867 0.7010 11.00000 0.05 0.10 Q36 1 0.5919 0.3953 0.6737 11.00000 0.05 0.10 Q37 1 0.5401 0.4263 0.7064 11.00000 0.05 0.10 Q38 1 0.5123 0.2104 0.5477 11.00000 0.05 0.10 Q39 1 0.4648 0.6666 0.7619 11.00000 0.05 0.10 Q40 1 0.5198 0.5854 0.7394 11.00000 0.05 0.10 Q41 1 0.5027 0.2092 0.5341 11.00000 0.05 0.09 Q42 1 0.2555 0.3099 0.6078 11.00000 0.05 0.09 Q43 1 0.3963 0.6606 0.6316 11.00000 0.05 0.09 Q44 1 0.3231 0.6739 0.6609 11.00000 0.05 0.09 Q45 1 0.5428 0.4377 0.7691 11.00000 0.05 0.09 Q46 1 0.7621 0.3274 0.6335 11.00000 0.05 0.09 Q47 1 0.4376 0.6969 0.5847 11.00000 0.05 0.09 Q48 1 0.2600 0.6124 0.8741 11.00000 0.05 0.09 Q49 1 0.3446 0.5118 0.7998 11.00000 0.05 0.09 Q50 1 0.3805 0.2410 0.8503 11.00000 0.05 0.09 Q51 1 0.6308 0.5789 0.9487 11.00000 0.05 0.09 Q52 1 0.3513 0.6023 0.7338 11.00000 0.05 0.09 Q53 1 0.3397 0.4377 0.7468 11.00000 0.05 0.09 Q54 1 0.2562 0.4381 0.9175 11.00000 0.05 0.09 Q55 1 0.2397 0.6074 0.8536 11.00000 0.05 0.09 ; _shelx_res_checksum 63108 loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 +X,+Y,+Z 2 1/2+X,1/2-Y,-Z 3 -X,1/2+Y,1/2-Z 4 1/2-X,-Y,1/2+Z 5 -X,-Y,-Z 6 -1/2-X,-1/2+Y,+Z 7 +X,-1/2-Y,-1/2+Z 8 -1/2+X,+Y,-1/2-Z loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.43367(3) 0.46961(3) 0.76739(3) 0.0862(2) Uani 1 1 d . . . . . S1 S 0.40775(13) 0.31016(9) 0.93669(9) 0.1727(8) Uani 1 1 d . . . . . S2 S 0.32127(10) 0.27768(9) 0.66660(10) 0.1611(7) Uani 1 1 d . . . . . O1 O 0.43302(18) 0.54378(16) 0.69652(15) 0.1056(10) Uani 1 1 d . . . . . O2 O 0.51809(19) 0.52715(16) 0.81512(17) 0.1170(11) Uani 1 1 d . . . . . N1 N 0.40647(19) 0.60340(19) 0.71475(16) 0.0820(9) Uani 1 1 d . . . . . N2 N 0.35283(18) 0.54160(18) 0.79902(17) 0.0787(9) Uani 1 1 d . . . . . N3 N 0.5850(2) 0.4959(2) 0.8188(2) 0.0920(10) Uani 1 1 d . . . . . N4 N 0.53781(17) 0.42899(18) 0.73573(18) 0.0792(9) Uani 1 1 d . . . . . N5 N 0.4252(2) 0.4068(2) 0.8441(2) 0.1206(15) Uani 1 1 d . . . . . N6 N 0.3658(2) 0.4058(2) 0.7127(2) 0.1054(13) Uani 1 1 d . . . . . C1 C 0.3526(2) 0.6021(2) 0.7667(2) 0.0757(11) Uani 1 1 d . . . . . C2 C 0.3007(2) 0.6544(2) 0.7819(2) 0.0883(12) Uani 1 1 d . . . . . H2 H 0.2998 0.6955 0.7581 0.106 Uiso 1 1 calc R U . . . C3 C 0.2498(2) 0.6446(2) 0.8332(2) 0.0868(12) Uani 1 1 d . . . . . H3 H 0.2150 0.6799 0.8443 0.104 Uiso 1 1 calc R U . . . C4 C 0.2500(2) 0.5836(2) 0.8680(2) 0.0738(11) Uani 1 1 d . . . . . C5 C 0.3036(2) 0.5341(2) 0.8482(2) 0.0819(12) Uani 1 1 d . . . . . H5 H 0.3052 0.4923 0.8709 0.098 Uiso 1 1 calc R U . . . C6 C 0.1971(2) 0.5705(2) 0.9233(2) 0.0757(11) Uani 1 1 d . . . . . C7 C 0.1680(3) 0.6230(3) 0.9604(2) 0.1005(14) Uani 1 1 d . . . . . H7 H 0.1808 0.6688 0.9503 0.121 Uiso 1 1 calc R U . . . C8 C 0.1199(3) 0.6099(4) 1.0127(3) 0.1255(18) Uani 1 1 d . . . . . H8 H 0.1011 0.6466 1.0376 0.151 Uiso 1 1 calc R U . . . C9 C 0.1001(3) 0.5435(4) 1.0277(3) 0.130(2) Uani 1 1 d . . . . . H9 H 0.0677 0.5345 1.0629 0.156 Uiso 1 1 calc R U . . . C10 C 0.1275(4) 0.4907(3) 0.9914(3) 0.141(2) Uani 1 1 d . . . . . H10 H 0.1141 0.4450 1.0014 0.169 Uiso 1 1 calc R U . . . C11 C 0.1755(3) 0.5044(3) 0.9393(2) 0.1138(16) Uani 1 1 d . . . . . H11 H 0.1937 0.4674 0.9144 0.137 Uiso 1 1 calc R U . . . C12 C 0.4446(3) 0.6646(3) 0.6831(3) 0.0988(14) Uani 1 1 d . . . . . C16 C 0.6011(2) 0.4481(2) 0.7698(2) 0.0776(11) Uani 1 1 d . . . . . C17 C 0.6751(2) 0.4233(3) 0.7550(2) 0.0939(13) Uani 1 1 d . . . . . H17 H 0.7185 0.4374 0.7788 0.113 Uiso 1 1 calc R U . . . C18 C 0.6829(2) 0.3781(2) 0.7049(2) 0.0928(13) Uani 1 1 d . . . . . H18 H 0.7323 0.3605 0.6953 0.111 Uiso 1 1 calc R U . . . C19 C 0.6197(2) 0.3576(2) 0.6679(2) 0.0788(11) Uani 1 1 d . . . . . C20 C 0.5480(2) 0.3857(2) 0.6864(2) 0.0824(12) Uani 1 1 d . . . . . H20 H 0.5041 0.3733 0.6625 0.099 Uiso 1 1 calc R U . . . C21 C 0.6262(3) 0.3104(3) 0.6130(2) 0.0962(14) Uani 1 1 d . . . . . C22 C 0.6927(3) 0.3090(3) 0.5743(3) 0.1204(18) Uani 1 1 d . . . . . H22 H 0.7345 0.3384 0.5836 0.144 Uiso 1 1 calc R U . . . C23 C 0.6972(5) 0.2645(4) 0.5224(4) 0.158(3) Uani 1 1 d . . . . . H23 H 0.7415 0.2647 0.4963 0.190 Uiso 1 1 calc R U . . . C24 C 0.6382(8) 0.2209(5) 0.5091(5) 0.184(4) Uani 1 1 d . . . . . H24 H 0.6421 0.1905 0.4742 0.220 Uiso 1 1 calc R U . . . C25 C 0.5720(6) 0.2210(5) 0.5469(5) 0.179(3) Uani 1 1 d . . . . . H25 H 0.5313 0.1904 0.5377 0.215 Uiso 1 1 calc R U . . . C26 C 0.5659(4) 0.2664(3) 0.5984(3) 0.1289(19) Uani 1 1 d . . . . . H26 H 0.5205 0.2670 0.6232 0.155 Uiso 1 1 calc R U . . . C27 C 0.6340(3) 0.5126(3) 0.8770(3) 0.1108(15) Uani 1 1 d . . . . . C28 C 0.5841(5) 0.5502(5) 0.9229(3) 0.254(5) Uani 1 1 d . . . . . H28A H 0.6139 0.5616 0.9608 0.305 Uiso 1 1 calc R U . . . H28B H 0.5653 0.5922 0.9031 0.305 Uiso 1 1 calc R U . . . H28C H 0.5405 0.5214 0.9348 0.305 Uiso 1 1 calc R U . . . C29 C 0.6611(4) 0.4449(3) 0.9071(3) 0.176(3) Uani 1 1 d . . . . . H29A H 0.6938 0.4203 0.8770 0.211 Uiso 1 1 calc R U . . . H29B H 0.6903 0.4547 0.9458 0.211 Uiso 1 1 calc R U . . . H29C H 0.6163 0.4168 0.9177 0.211 Uiso 1 1 calc R U . . . C30 C 0.7040(4) 0.5554(4) 0.8563(4) 0.199(3) Uani 1 1 d . . . . . H30A H 0.7351 0.5290 0.8263 0.239 Uiso 1 1 calc R U . . . H30B H 0.6863 0.5974 0.8358 0.239 Uiso 1 1 calc R U . . . H30C H 0.7350 0.5669 0.8935 0.239 Uiso 1 1 calc R U . . . C31 C 0.4185(2) 0.3678(2) 0.8817(2) 0.0855(13) Uani 1 1 d . . . . . C32 C 0.3473(2) 0.3525(3) 0.6939(3) 0.0981(15) Uani 1 1 d . . . . . C13A C 0.4668(11) 0.7164(8) 0.7342(7) 0.174(9) Uani 0.61(2) 1 d . . P A 1 H13A H 0.4206 0.7316 0.7566 0.209 Uiso 0.61(2) 1 calc R U P A 1 H13B H 0.5021 0.6950 0.7644 0.209 Uiso 0.61(2) 1 calc R U P A 1 H13C H 0.4918 0.7558 0.7144 0.209 Uiso 0.61(2) 1 calc R U P A 1 C14A C 0.5133(9) 0.6389(6) 0.6465(9) 0.172(10) Uani 0.61(2) 1 d . . P A 1 H14A H 0.5389 0.6774 0.6256 0.206 Uiso 0.61(2) 1 calc R U P A 1 H14B H 0.5493 0.6167 0.6756 0.206 Uiso 0.61(2) 1 calc R U P A 1 H14C H 0.4964 0.6060 0.6144 0.206 Uiso 0.61(2) 1 calc R U P A 1 C15A C 0.3845(9) 0.6954(10) 0.6375(8) 0.189(9) Uani 0.61(2) 1 d . . P A 1 H15A H 0.3403 0.7118 0.6619 0.227 Uiso 0.61(2) 1 calc R U P A 1 H15B H 0.4074 0.7335 0.6142 0.227 Uiso 0.61(2) 1 calc R U P A 1 H15C H 0.3676 0.6603 0.6074 0.227 Uiso 0.61(2) 1 calc R U P A 1 C13B C 0.5323(10) 0.6649(11) 0.7081(13) 0.154(12) Uani 0.39(2) 1 d . . P A 2 H13D H 0.5554 0.6200 0.7007 0.185 Uiso 0.39(2) 1 calc R U P A 2 H13E H 0.5616 0.6998 0.6852 0.185 Uiso 0.39(2) 1 calc R U P A 2 H13F H 0.5331 0.6752 0.7536 0.185 Uiso 0.39(2) 1 calc R U P A 2 C14B C 0.4483(17) 0.6509(9) 0.6110(7) 0.133(9) Uani 0.39(2) 1 d . . P A 2 H14D H 0.4707 0.6057 0.6035 0.159 Uiso 0.39(2) 1 calc R U P A 2 H14E H 0.3964 0.6523 0.5932 0.159 Uiso 0.39(2) 1 calc R U P A 2 H14F H 0.4801 0.6858 0.5907 0.159 Uiso 0.39(2) 1 calc R U P A 2 C15B C 0.4098(12) 0.7345(8) 0.6949(12) 0.124(9) Uani 0.39(2) 1 d . . P A 2 H15D H 0.4394 0.7691 0.6720 0.148 Uiso 0.39(2) 1 calc R U P A 2 H15E H 0.3566 0.7350 0.6799 0.148 Uiso 0.39(2) 1 calc R U P A 2 H15F H 0.4109 0.7445 0.7404 0.148 Uiso 0.39(2) 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 0.0676(3) 0.0857(4) 0.1052(5) 0.0071(3) 0.0121(3) 0.0131(3) S1 0.2167(19) 0.1448(15) 0.1565(16) 0.0532(13) -0.0077(14) -0.0016(13) S2 0.1606(14) 0.1205(13) 0.2021(18) -0.0157(12) 0.0155(13) -0.0355(11) O1 0.124(2) 0.089(2) 0.104(2) 0.0118(18) 0.0368(19) 0.0224(19) O2 0.094(2) 0.106(2) 0.151(3) -0.030(2) -0.006(2) 0.0206(19) N1 0.080(2) 0.078(3) 0.088(3) 0.006(2) 0.0103(19) 0.008(2) N2 0.069(2) 0.080(3) 0.086(2) 0.007(2) 0.0112(19) 0.0108(17) N3 0.076(2) 0.089(3) 0.111(3) -0.003(2) -0.002(2) 0.003(2) N4 0.0583(19) 0.083(2) 0.097(3) 0.001(2) 0.0024(19) 0.0070(17) N5 0.131(3) 0.105(3) 0.125(4) 0.030(3) 0.021(3) 0.031(3) N6 0.064(2) 0.110(3) 0.143(4) -0.007(3) 0.006(2) -0.003(2) C1 0.064(2) 0.082(3) 0.081(3) 0.002(3) 0.007(2) 0.006(2) C2 0.090(3) 0.075(3) 0.101(3) 0.009(3) 0.016(3) 0.008(2) C3 0.082(3) 0.073(3) 0.105(3) -0.001(3) 0.012(3) 0.015(2) C4 0.066(2) 0.074(3) 0.082(3) -0.013(3) 0.002(2) 0.004(2) C5 0.079(3) 0.081(3) 0.086(3) 0.009(2) 0.010(2) 0.009(2) C6 0.069(2) 0.078(3) 0.080(3) -0.008(3) 0.004(2) -0.002(2) C7 0.098(3) 0.097(4) 0.106(4) -0.020(3) 0.019(3) 0.002(3) C8 0.122(4) 0.143(6) 0.112(5) -0.029(4) 0.035(4) 0.013(4) C9 0.130(4) 0.165(6) 0.096(4) 0.000(5) 0.037(3) -0.004(5) C10 0.180(6) 0.109(5) 0.135(5) 0.000(4) 0.065(5) -0.016(4) C11 0.134(4) 0.098(4) 0.108(4) -0.008(3) 0.052(3) 0.001(3) C12 0.110(4) 0.086(4) 0.101(4) 0.003(3) 0.028(3) -0.013(3) C16 0.068(3) 0.073(3) 0.092(3) 0.005(3) 0.001(2) 0.003(2) C17 0.059(3) 0.107(4) 0.116(4) -0.008(3) -0.007(2) 0.004(2) C18 0.062(3) 0.098(4) 0.118(4) 0.001(3) 0.004(3) 0.015(2) C19 0.066(3) 0.072(3) 0.098(3) 0.011(3) 0.002(2) 0.011(2) C20 0.069(3) 0.083(3) 0.095(3) 0.007(3) -0.004(2) 0.006(2) C21 0.109(4) 0.079(3) 0.101(4) -0.002(3) -0.014(3) 0.019(3) C22 0.126(4) 0.115(4) 0.120(5) 0.000(4) 0.015(4) 0.049(3) C23 0.213(8) 0.142(7) 0.119(6) -0.021(5) 0.008(5) 0.093(6) C24 0.271(13) 0.132(7) 0.148(8) -0.045(6) -0.074(8) 0.060(8) C25 0.193(9) 0.168(7) 0.177(9) -0.031(7) -0.061(7) 0.003(6) C26 0.140(5) 0.122(5) 0.124(5) -0.030(4) -0.030(4) 0.015(4) C27 0.116(4) 0.115(4) 0.102(4) -0.012(3) -0.012(3) -0.001(3) C28 0.223(8) 0.376(12) 0.162(7) -0.145(8) -0.048(6) 0.102(8) C29 0.217(7) 0.179(6) 0.131(5) 0.033(5) -0.043(5) 0.017(5) C30 0.189(7) 0.186(7) 0.222(8) 0.001(6) -0.045(6) -0.091(6) C31 0.088(3) 0.080(3) 0.089(3) 0.012(3) -0.001(3) 0.026(2) C32 0.062(3) 0.109(4) 0.124(4) 0.011(4) 0.011(3) 0.003(3) C13A 0.178(18) 0.145(14) 0.199(14) -0.049(11) 0.041(11) -0.078(15) C14A 0.144(14) 0.148(10) 0.22(2) -0.021(11) 0.110(17) -0.033(10) C15A 0.211(14) 0.224(19) 0.133(14) 0.105(15) 0.007(11) 0.028(13) C13B 0.101(12) 0.139(18) 0.22(3) 0.020(19) -0.044(15) -0.044(12) C14B 0.18(3) 0.122(13) 0.094(13) 0.019(10) 0.022(12) -0.040(16) C15B 0.126(14) 0.086(11) 0.16(2) 0.019(12) 0.043(15) -0.014(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 for Crystallography (Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.0000 0.0000 ; International Tables for Crystallography (Vol. C, Table 6.1.1.4) ; N N 0.0061 0.0033 ; International Tables for Crystallography (Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Ni Ni 0.3393 1.1124 ; International Tables for Crystallography (Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; O O 0.0106 0.0060 ; International Tables for Crystallography (Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; S S 0.1246 0.1234 ; International Tables for Crystallography (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 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N5 Ni1 N6 92.04(19) . . ? N5 Ni1 O1 171.77(15) . . ? N6 Ni1 O1 91.05(16) . . ? N5 Ni1 N4 94.98(15) . . ? N6 Ni1 N4 95.04(15) . . ? O1 Ni1 N4 92.34(13) . . ? N5 Ni1 N2 96.00(16) . . ? N6 Ni1 N2 101.48(14) . . ? O1 Ni1 N2 75.90(13) . . ? N4 Ni1 N2 159.77(14) . . ? N5 Ni1 O2 89.70(18) . . ? N6 Ni1 O2 170.56(14) . . ? O1 Ni1 O2 88.49(14) . . ? N4 Ni1 O2 75.56(14) . . ? N2 Ni1 O2 87.55(13) . . ? N1 O1 Ni1 114.3(2) . . ? N3 O2 Ni1 113.3(3) . . ? O1 N1 C1 115.8(3) . . ? O1 N1 C12 114.7(3) . . ? C1 N1 C12 129.1(4) . . ? C5 N2 C1 118.3(3) . . ? C5 N2 Ni1 126.5(3) . . ? C1 N2 Ni1 115.1(3) . . ? O2 N3 C16 116.0(4) . . ? O2 N3 C27 116.2(4) . . ? C16 N3 C27 127.8(4) . . ? C20 N4 C16 117.9(3) . . ? C20 N4 Ni1 126.7(3) . . ? C16 N4 Ni1 115.3(3) . . ? C31 N5 Ni1 173.1(5) . . ? C32 N6 Ni1 152.9(4) . . ? N2 C1 C2 121.3(4) . . ? N2 C1 N1 113.1(4) . . ? C2 C1 N1 125.4(4) . . ? C1 C2 C3 118.7(4) . . ? C1 C2 H2 120.6 . . ? C3 C2 H2 120.6 . . ? C4 C3 C2 121.0(4) . . ? C4 C3 H3 119.5 . . ? C2 C3 H3 119.5 . . ? C3 C4 C5 115.6(4) . . ? C3 C4 C6 123.3(4) . . ? C5 C4 C6 121.1(4) . . ? N2 C5 C4 124.9(4) . . ? N2 C5 H5 117.6 . . ? C4 C5 H5 117.6 . . ? C7 C6 C11 117.0(4) . . ? C7 C6 C4 122.2(4) . . ? C11 C6 C4 120.8(4) . . ? C6 C7 C8 121.6(5) . . ? C6 C7 H7 119.2 . . ? C8 C7 H7 119.2 . . ? C9 C8 C7 119.9(5) . . ? C9 C8 H8 120.0 . . ? C7 C8 H8 120.0 . . ? C10 C9 C8 119.6(5) . . ? C10 C9 H9 120.2 . . ? C8 C9 H9 120.2 . . ? C9 C10 C11 120.0(5) . . ? C9 C10 H10 120.0 . . ? C11 C10 H10 120.0 . . ? C6 C11 C10 121.9(5) . . ? C6 C11 H11 119.1 . . ? C10 C11 H11 119.1 . . ? C14A C12 N1 107.9(6) . . ? C15B C12 N1 117.6(7) . . ? C14A C12 C13A 112.4(9) . . ? N1 C12 C13A 108.8(6) . . ? C14A C12 C15A 110.4(9) . . ? N1 C12 C15A 106.5(6) . . ? C13A C12 C15A 110.6(10) . . ? C15B C12 C14B 109.6(12) . . ? N1 C12 C14B 108.2(7) . . ? C15B C12 C13B 108.7(12) . . ? N1 C12 C13B 105.7(7) . . ? C14B C12 C13B 106.4(13) . . ? N4 C16 C17 121.7(4) . . ? N4 C16 N3 113.7(4) . . ? C17 C16 N3 124.6(4) . . ? C18 C17 C16 118.5(4) . . ? C18 C17 H17 120.7 . . ? C16 C17 H17 120.7 . . ? C17 C18 C19 122.0(4) . . ? C17 C18 H18 119.0 . . ? C19 C18 H18 119.0 . . ? C18 C19 C20 115.0(4) . . ? C18 C19 C21 123.4(4) . . ? C20 C19 C21 121.5(4) . . ? N4 C20 C19 124.8(4) . . ? N4 C20 H20 117.6 . . ? C19 C20 H20 117.6 . . ? C26 C21 C22 118.5(5) . . ? C26 C21 C19 120.0(5) . . ? C22 C21 C19 121.4(5) . . ? C23 C22 C21 120.4(6) . . ? C23 C22 H22 119.8 . . ? C21 C22 H22 119.8 . . ? C24 C23 C22 120.6(9) . . ? C24 C23 H23 119.7 . . ? C22 C23 H23 119.7 . . ? C23 C24 C25 120.1(10) . . ? C23 C24 H24 119.9 . . ? C25 C24 H24 119.9 . . ? C24 C25 C26 120.1(9) . . ? C24 C25 H25 120.0 . . ? C26 C25 H25 120.0 . . ? C21 C26 C25 120.3(7) . . ? C21 C26 H26 119.9 . . ? C25 C26 H26 119.9 . . ? C28 C27 N3 107.4(5) . . ? C28 C27 C30 112.0(6) . . ? N3 C27 C30 109.3(5) . . ? C28 C27 C29 109.5(6) . . ? N3 C27 C29 108.5(5) . . ? C30 C27 C29 110.0(5) . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C27 C30 H30A 109.5 . . ? C27 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C27 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? N5 C31 S1 179.4(6) . . ? N6 C32 S2 179.3(6) . . ? C12 C13A H13A 109.5 . . ? C12 C13A H13B 109.5 . . ? H13A C13A H13B 109.5 . . ? C12 C13A H13C 109.5 . . ? H13A C13A H13C 109.5 . . ? H13B C13A H13C 109.5 . . ? C12 C14A H14A 109.5 . . ? C12 C14A H14B 109.5 . . ? H14A C14A H14B 109.5 . . ? C12 C14A H14C 109.5 . . ? H14A C14A H14C 109.5 . . ? H14B C14A H14C 109.5 . . ? C12 C15A H15A 109.5 . . ? C12 C15A H15B 109.5 . . ? H15A C15A H15B 109.5 . . ? C12 C15A H15C 109.5 . . ? H15A C15A H15C 109.5 . . ? H15B C15A H15C 109.5 . . ? C12 C13B H13D 109.5 . . ? C12 C13B H13E 109.5 . . ? H13D C13B H13E 109.5 . . ? C12 C13B H13F 109.5 . . ? H13D C13B H13F 109.5 . . ? H13E C13B H13F 109.5 . . ? C12 C14B H14D 109.5 . . ? C12 C14B H14E 109.5 . . ? H14D C14B H14E 109.5 . . ? C12 C14B H14F 109.5 . . ? H14D C14B H14F 109.5 . . ? H14E C14B H14F 109.5 . . ? C12 C15B H15D 109.5 . . ? C12 C15B H15E 109.5 . . ? H15D C15B H15E 109.5 . . ? C12 C15B H15F 109.5 . . ? H15D C15B H15F 109.5 . . ? H15E C15B H15F 109.5 . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 N5 1.997(4) . ? Ni1 N6 2.030(4) . ? Ni1 O1 2.043(3) . ? Ni1 N4 2.049(3) . ? Ni1 N2 2.059(3) . ? Ni1 O2 2.066(3) . ? S1 C31 1.597(5) . ? S2 C32 1.606(6) . ? O1 N1 1.287(4) . ? O2 N3 1.292(4) . ? N1 C1 1.413(5) . ? N1 C12 1.494(5) . ? N2 C5 1.327(5) . ? N2 C1 1.339(5) . ? N3 C16 1.394(5) . ? N3 C27 1.501(6) . ? N4 C20 1.326(5) . ? N4 C16 1.341(5) . ? N5 C31 1.085(5) . ? N6 C32 1.139(5) . ? C1 C2 1.376(5) . ? C2 C3 1.384(5) . ? C2 H2 0.9300 . ? C3 C4 1.374(5) . ? C3 H3 0.9300 . ? C4 C5 1.382(5) . ? C4 C6 1.478(5) . ? C5 H5 0.9300 . ? C6 C7 1.359(5) . ? C6 C11 1.363(6) . ? C7 C8 1.381(6) . ? C7 H7 0.9300 . ? C8 C9 1.354(7) . ? C8 H8 0.9300 . ? C9 C10 1.345(7) . ? C9 H9 0.9300 . ? C10 C11 1.378(6) . ? C10 H10 0.9300 . ? C11 H11 0.9300 . ? C12 C14A 1.481(10) . ? C12 C15B 1.487(16) . ? C12 C13A 1.500(12) . ? C12 C15A 1.513(13) . ? C12 C14B 1.513(15) . ? C12 C13B 1.585(15) . ? C16 C17 1.384(5) . ? C17 C18 1.356(5) . ? C17 H17 0.9300 . ? C18 C19 1.381(5) . ? C18 H18 0.9300 . ? C19 C20 1.392(5) . ? C19 C21 1.456(6) . ? C20 H20 0.9300 . ? C21 C26 1.365(6) . ? C21 C22 1.390(6) . ? C22 C23 1.373(8) . ? C22 H22 0.9300 . ? C23 C24 1.337(10) . ? C23 H23 0.9300 . ? C24 C25 1.374(11) . ? C24 H24 0.9300 . ? C25 C26 1.380(9) . ? C25 H25 0.9300 . ? C26 H26 0.9300 . ? C27 C28 1.465(7) . ? C27 C30 1.512(7) . ? C27 C29 1.513(7) . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C13A H13A 0.9600 . ? C13A H13B 0.9600 . ? C13A H13C 0.9600 . ? C14A H14A 0.9600 . ? C14A H14B 0.9600 . ? C14A H14C 0.9600 . ? C15A H15A 0.9600 . ? C15A H15B 0.9600 . ? C15A H15C 0.9600 . ? C13B H13D 0.9600 . ? C13B H13E 0.9600 . ? C13B H13F 0.9600 . ? C14B H14D 0.9600 . ? C14B H14E 0.9600 . ? C14B H14F 0.9600 . ? C15B H15D 0.9600 . ? C15B H15E 0.9600 . ? C15B H15F 0.9600 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Ni1 O1 N1 C1 -26.8(4) . . . . ? Ni1 O1 N1 C12 146.2(3) . . . . ? Ni1 O2 N3 C16 27.3(4) . . . . ? Ni1 O2 N3 C27 -149.7(3) . . . . ? C5 N2 C1 C2 -2.6(6) . . . . ? Ni1 N2 C1 C2 178.8(3) . . . . ? C5 N2 C1 N1 -178.9(3) . . . . ? Ni1 N2 C1 N1 2.5(4) . . . . ? O1 N1 C1 N2 16.0(5) . . . . ? C12 N1 C1 N2 -155.8(4) . . . . ? O1 N1 C1 C2 -160.2(4) . . . . ? C12 N1 C1 C2 28.0(7) . . . . ? N2 C1 C2 C3 2.3(6) . . . . ? N1 C1 C2 C3 178.1(4) . . . . ? C1 C2 C3 C4 -0.9(6) . . . . ? C2 C3 C4 C5 0.0(6) . . . . ? C2 C3 C4 C6 179.9(4) . . . . ? C1 N2 C5 C4 1.6(6) . . . . ? Ni1 N2 C5 C4 -180.0(3) . . . . ? C3 C4 C5 N2 -0.3(6) . . . . ? C6 C4 C5 N2 179.8(4) . . . . ? C3 C4 C6 C7 -27.2(6) . . . . ? C5 C4 C6 C7 152.7(4) . . . . ? C3 C4 C6 C11 153.0(4) . . . . ? C5 C4 C6 C11 -27.2(6) . . . . ? C11 C6 C7 C8 1.2(7) . . . . ? C4 C6 C7 C8 -178.7(4) . . . . ? C6 C7 C8 C9 -0.6(8) . . . . ? C7 C8 C9 C10 -0.1(9) . . . . ? C8 C9 C10 C11 0.1(10) . . . . ? C7 C6 C11 C10 -1.1(7) . . . . ? C4 C6 C11 C10 178.7(5) . . . . ? C9 C10 C11 C6 0.5(9) . . . . ? O1 N1 C12 C14A -9.5(11) . . . . ? C1 N1 C12 C14A 162.3(10) . . . . ? O1 N1 C12 C15B 171.9(14) . . . . ? C1 N1 C12 C15B -16.3(15) . . . . ? O1 N1 C12 C13A -131.7(10) . . . . ? C1 N1 C12 C13A 40.2(11) . . . . ? O1 N1 C12 C15A 109.1(10) . . . . ? C1 N1 C12 C15A -79.1(10) . . . . ? O1 N1 C12 C14B 47.1(13) . . . . ? C1 N1 C12 C14B -141.1(13) . . . . ? O1 N1 C12 C13B -66.6(13) . . . . ? C1 N1 C12 C13B 105.2(13) . . . . ? C20 N4 C16 C17 -0.7(6) . . . . ? Ni1 N4 C16 C17 178.3(3) . . . . ? C20 N4 C16 N3 177.4(3) . . . . ? Ni1 N4 C16 N3 -3.5(4) . . . . ? O2 N3 C16 N4 -15.9(5) . . . . ? C27 N3 C16 N4 160.6(4) . . . . ? O2 N3 C16 C17 162.2(4) . . . . ? C27 N3 C16 C17 -21.3(7) . . . . ? N4 C16 C17 C18 -0.5(7) . . . . ? N3 C16 C17 C18 -178.5(4) . . . . ? C16 C17 C18 C19 1.4(7) . . . . ? C17 C18 C19 C20 -1.0(6) . . . . ? C17 C18 C19 C21 178.6(4) . . . . ? C16 N4 C20 C19 1.2(6) . . . . ? Ni1 N4 C20 C19 -177.8(3) . . . . ? C18 C19 C20 N4 -0.3(6) . . . . ? C21 C19 C20 N4 -180.0(4) . . . . ? C18 C19 C21 C26 148.1(5) . . . . ? C20 C19 C21 C26 -32.3(6) . . . . ? C18 C19 C21 C22 -32.3(7) . . . . ? C20 C19 C21 C22 147.3(4) . . . . ? C26 C21 C22 C23 0.3(7) . . . . ? C19 C21 C22 C23 -179.4(4) . . . . ? C21 C22 C23 C24 -1.3(10) . . . . ? C22 C23 C24 C25 0.9(13) . . . . ? C23 C24 C25 C26 0.4(14) . . . . ? C22 C21 C26 C25 1.1(8) . . . . ? C19 C21 C26 C25 -179.3(5) . . . . ? C24 C25 C26 C21 -1.5(12) . . . . ? O2 N3 C27 C28 12.2(7) . . . . ? C16 N3 C27 C28 -164.4(5) . . . . ? O2 N3 C27 C30 -109.6(5) . . . . ? C16 N3 C27 C30 73.9(6) . . . . ? O2 N3 C27 C29 130.5(5) . . . . ? C16 N3 C27 C29 -46.0(6) . . . . ?