#------------------------------------------------------------------------------ #$Date: 2020-04-24 04:34:37 +0300 (Fri, 24 Apr 2020) $ #$Revision: 251124 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/24/03/7240392.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_7240392 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 monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_block_doi 10.5517/ccdc.csd.cc24lhnx _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 90.338(10) _cell_angle_gamma 90.0000 _cell_formula_units_Z 8 _cell_length_a 19.990(4) _cell_length_b 16.865(3) _cell_length_c 18.965(3) _cell_measurement_reflns_used 14879 _cell_measurement_temperature 140 _cell_measurement_theta_max 27.48 _cell_measurement_theta_min 3.16 _cell_volume 6394(2) _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 'SIR2004 (Burla, et al., 2005)' _diffrn_ambient_temperature 140 _diffrn_detector_area_resol_mean 29.412 _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.997 _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 0.1492 _diffrn_reflns_Laue_measured_fraction_full 0.997 _diffrn_reflns_Laue_measured_fraction_max 0.997 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_number 32607 _diffrn_reflns_point_group_measured_fraction_full 0.997 _diffrn_reflns_point_group_measured_fraction_max 0.997 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 25.399 _diffrn_reflns_theta_min 3.057 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.777 _exptl_absorpt_correction_T_max 0.946 _exptl_absorpt_correction_T_min 0.946 _exptl_absorpt_correction_type none _exptl_crystal_colour Blue _exptl_crystal_density_diffrn 1.366 _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 0.465 _exptl_crystal_size_mid 0.156 _exptl_crystal_size_min 0.071 _refine_diff_density_max 1.38 _refine_diff_density_min -0.59 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.015 _refine_ls_hydrogen_treatment constr _refine_ls_number_parameters 775 _refine_ls_number_reflns 11745 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2057 _refine_ls_R_factor_gt 0.0997 _refine_ls_shift/su_max 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.0245P)^2^+63.8805P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1914 _refine_ls_wR_factor_ref 0.2298 _reflns_Friedel_coverage 0.000 _reflns_number_gt 5664 _reflns_number_total 11745 _reflns_threshold_expression F^2^>2.0\s(F^2^) _cod_data_source_file d0ra02041a1.cif _cod_data_source_block phpyNO_Ni_NCS2_140K _cod_database_code 7240392 _shelx_res_file ; shelxl.res created by SHELXL-2014/7 TITL NiNCS140K CELL 0.71073 19.99040 16.86520 18.96530 90.00000 90.33770 90.00000 ZERR 8 0.00410 0.00280 0.00320 0.00000 0.01020 0.00000 LATT 1 SYMM -X, .50+Y, .50-Z SFAC C H N NI O S UNIT 256 272 48 8 16 16 SHEL 99999.000000 0.828482 L.S. 10 FMAP 2 PLAN 53 WPDB -2 HTAB BOND $H CONF LIST 4 TEMP -133.0 ACTA SIZE 0.465 0.156 0.071 WGHT 0.024500 63.880501 FVAR 0.54900 NI1 4 0.229557 0.441759 0.537015 11.00000 0.02835 0.02023 = 0.02446 -0.00286 -0.00130 -0.00184 NI2 4 0.730830 0.057023 0.488454 11.00000 0.03365 0.02070 = 0.02762 -0.00546 -0.00087 0.00438 S1 6 0.044643 0.390982 0.684766 11.00000 0.05028 0.06740 = 0.04491 0.01099 0.01073 0.00651 S2 6 0.329339 0.318059 0.734803 11.00000 0.04712 0.06171 = 0.03627 0.01935 -0.00623 -0.00108 S3 6 0.580868 0.097646 0.306517 11.00000 0.05516 0.04793 = 0.03407 0.00279 -0.00926 0.00510 S4 6 0.824282 0.172601 0.284455 11.00000 0.06457 0.03928 = 0.03452 0.00358 0.00105 0.00044 O1 5 0.305954 0.431688 0.465682 11.00000 0.03371 0.03473 = 0.02047 -0.00521 -0.00451 -0.00232 O2 5 0.187414 0.527310 0.474453 11.00000 0.04011 0.02379 = 0.03524 -0.00914 -0.00211 0.00345 O3 5 0.809792 0.070614 0.556762 11.00000 0.02778 0.03499 = 0.03812 -0.00800 -0.00141 0.00425 O4 5 0.696648 -0.031894 0.552709 11.00000 0.04089 0.02221 = 0.03034 -0.00569 0.00586 0.00186 N1 3 0.285783 0.408954 0.404871 11.00000 0.02605 0.02410 = 0.02003 0.00015 0.00510 0.00698 N2 3 0.196118 0.361048 0.464731 11.00000 0.01800 0.02118 = 0.02393 0.00747 0.00217 0.00252 N3 3 0.183203 0.595031 0.507884 11.00000 0.03070 0.02134 = 0.03214 0.00175 0.00080 -0.00169 N4 3 0.268725 0.543970 0.577178 11.00000 0.01664 0.02058 = 0.02231 -0.00139 -0.00436 -0.00136 N5 3 0.148274 0.439454 0.599006 11.00000 0.02940 0.03851 = 0.03046 -0.00690 0.00299 -0.00678 N6 3 0.280958 0.370199 0.604210 11.00000 0.03533 0.02466 = 0.03430 -0.00487 0.00000 -0.00596 N7 3 0.788157 0.091432 0.619234 11.00000 0.02656 0.02374 = 0.01903 -0.00326 0.00763 -0.00007 N8 3 0.697236 0.138822 0.558667 11.00000 0.02822 0.02183 = 0.02117 -0.00350 0.00240 0.00563 N9 3 0.685748 -0.095818 0.515942 11.00000 0.02785 0.03056 = 0.02178 -0.00034 0.00254 0.00380 N10 3 0.766443 -0.044547 0.444109 11.00000 0.02926 0.01580 = 0.02438 -0.00168 -0.00313 -0.00281 N11 3 0.646384 0.055611 0.429556 11.00000 0.05259 0.03244 = 0.03027 -0.00790 0.00333 0.00909 N12 3 0.776466 0.128494 0.418115 11.00000 0.04933 0.01617 = 0.03118 0.00220 -0.00242 0.00811 C1 1 0.230709 0.355444 0.405605 11.00000 0.01973 0.01689 = 0.02501 0.00124 -0.00151 -0.00151 C2 1 0.216034 0.300248 0.352673 11.00000 0.02788 0.03182 = 0.02168 -0.00820 0.00502 0.00217 AFIX 43 H2 2 0.241244 0.298176 0.310407 11.00000 -1.20000 AFIX 0 C3 1 0.163079 0.248541 0.364392 11.00000 0.03626 0.01744 = 0.01925 -0.00971 -0.00773 -0.00091 AFIX 43 H3 2 0.152281 0.210058 0.329561 11.00000 -1.20000 AFIX 0 C4 1 0.125740 0.251722 0.425463 11.00000 0.02340 0.02123 = 0.02130 -0.00124 -0.00298 0.00178 C5 1 0.144283 0.311123 0.473317 11.00000 0.02589 0.03116 = 0.02594 -0.00466 0.00144 0.00552 AFIX 43 H5 2 0.118384 0.316578 0.514875 11.00000 -1.20000 AFIX 0 C6 1 0.069255 0.197881 0.439634 11.00000 0.01923 0.01621 = 0.04101 -0.00572 -0.00358 0.00506 C7 1 0.033852 0.162225 0.383818 11.00000 0.02351 0.02755 = 0.03531 0.00105 -0.00465 0.00652 AFIX 43 H7 2 0.045618 0.173045 0.336323 11.00000 -1.20000 AFIX 0 C8 1 -0.018871 0.110657 0.398971 11.00000 0.02960 0.02813 = 0.05735 -0.01008 -0.00100 -0.00108 AFIX 43 H8 2 -0.042489 0.085923 0.361333 11.00000 -1.20000 AFIX 0 C9 1 -0.036997 0.095226 0.466644 11.00000 0.01228 0.03850 = 0.06443 -0.00241 0.01211 -0.00515 AFIX 43 H9 2 -0.073883 0.061297 0.475752 11.00000 -1.20000 AFIX 0 C10 1 -0.002181 0.128506 0.521833 11.00000 0.03277 0.03919 = 0.04152 0.00553 0.01480 -0.01055 AFIX 43 H10 2 -0.013883 0.116164 0.569052 11.00000 -1.20000 AFIX 0 C11 1 0.050283 0.180354 0.508267 11.00000 0.03512 0.03708 = 0.02280 -0.01024 -0.00397 0.00799 AFIX 43 H11 2 0.073559 0.204209 0.546586 11.00000 -1.20000 AFIX 0 C12 1 0.316000 0.455516 0.343158 11.00000 0.02505 0.02878 = 0.02487 0.00154 0.00536 -0.00623 C13 1 0.390681 0.460334 0.360619 11.00000 0.03409 0.08117 = 0.02983 0.00510 0.00146 -0.00632 AFIX 33 H13A 2 0.396826 0.485688 0.406699 11.00000 -1.20000 H13B 2 0.409640 0.406764 0.361922 11.00000 -1.20000 H13C 2 0.413429 0.491638 0.324424 11.00000 -1.20000 AFIX 0 C14 1 0.285052 0.537525 0.345079 11.00000 0.06906 0.03267 = 0.03383 0.01412 0.00319 0.00697 AFIX 33 H14A 2 0.292813 0.561353 0.391541 11.00000 -1.20000 H14B 2 0.305505 0.570784 0.308728 11.00000 -1.20000 H14C 2 0.236828 0.533464 0.336211 11.00000 -1.20000 AFIX 0 C15 1 0.305369 0.417404 0.273726 11.00000 0.04164 0.04448 = 0.02559 0.00441 0.00331 -0.00913 AFIX 33 H15A 2 0.325827 0.364598 0.273942 11.00000 -1.20000 H15B 2 0.257280 0.412525 0.264364 11.00000 -1.20000 H15C 2 0.325957 0.449845 0.236882 11.00000 -1.20000 AFIX 0 C16 1 0.237294 0.610640 0.554244 11.00000 0.01350 0.01501 = 0.03126 -0.00072 0.01057 0.00429 C17 1 0.259111 0.686144 0.574112 11.00000 0.02464 0.01358 = 0.04544 -0.00344 0.00909 -0.00116 AFIX 43 H17 2 0.236996 0.732129 0.556841 11.00000 -1.20000 AFIX 0 C18 1 0.311341 0.692724 0.617599 11.00000 0.02866 0.01822 = 0.03964 -0.00750 0.00482 0.00299 AFIX 43 H18 2 0.325540 0.744014 0.632000 11.00000 -1.20000 AFIX 0 C19 1 0.346486 0.625118 0.643108 11.00000 0.02591 0.02748 = 0.03465 0.00236 0.00384 -0.00173 C20 1 0.321705 0.552141 0.618647 11.00000 0.03573 0.02274 = 0.02367 -0.00297 0.00885 0.00142 AFIX 43 H20 2 0.344593 0.505388 0.632881 11.00000 -1.20000 AFIX 0 C21 1 0.404602 0.630258 0.689917 11.00000 0.02623 0.03207 = 0.02776 -0.01123 -0.00373 0.00109 C22 1 0.448774 0.694535 0.682472 11.00000 0.03328 0.03996 = 0.03152 -0.00992 -0.00482 -0.00053 AFIX 43 H22 2 0.440084 0.733754 0.647650 11.00000 -1.20000 AFIX 0 C23 1 0.505298 0.701389 0.725696 11.00000 0.05014 0.04978 = 0.04148 -0.01522 0.00109 -0.00123 AFIX 43 H23 2 0.535133 0.744658 0.719579 11.00000 -1.20000 AFIX 0 C24 1 0.517974 0.645480 0.777305 11.00000 0.03399 0.07635 = 0.05770 -0.02418 0.00555 -0.00067 AFIX 43 H24 2 0.556023 0.650760 0.807186 11.00000 -1.20000 AFIX 0 C25 1 0.474947 0.581563 0.785370 11.00000 0.05146 0.06430 = 0.03088 -0.00484 -0.00109 0.02248 AFIX 43 H25 2 0.483635 0.543022 0.820789 11.00000 -1.20000 AFIX 0 C26 1 0.418136 0.573627 0.740962 11.00000 0.03232 0.04313 = 0.04472 -0.00238 0.00068 0.00364 AFIX 43 H26 2 0.389221 0.529340 0.746190 11.00000 -1.20000 AFIX 0 C27 1 0.120424 0.642931 0.497932 11.00000 0.02551 0.02951 = 0.03528 0.00000 -0.00570 0.00581 C28 1 0.065136 0.586664 0.482004 11.00000 0.05169 0.06758 = 0.09396 -0.02277 -0.03950 0.02565 AFIX 33 H28A 2 0.023392 0.616236 0.475220 11.00000 -1.20000 H28B 2 0.075501 0.557126 0.438931 11.00000 -1.20000 H28C 2 0.060064 0.549533 0.521358 11.00000 -1.20000 AFIX 0 C29 1 0.132148 0.698441 0.434836 11.00000 0.08738 0.09797 = 0.07464 0.05945 0.03120 0.05382 AFIX 33 H29A 2 0.168677 0.735187 0.446013 11.00000 -1.20000 H29B 2 0.144002 0.666924 0.393335 11.00000 -1.20000 H29C 2 0.091235 0.728573 0.424967 11.00000 -1.20000 AFIX 0 C30 1 0.104753 0.688232 0.565180 11.00000 0.01843 0.07044 = 0.06170 -0.02409 0.00809 0.01070 AFIX 33 H30A 2 0.141236 0.725307 0.575627 11.00000 -1.20000 H30B 2 0.062933 0.717788 0.558897 11.00000 -1.20000 H30C 2 0.099993 0.650790 0.604347 11.00000 -1.20000 AFIX 0 C31 1 0.106198 0.419342 0.634310 11.00000 0.02862 0.03015 = 0.03123 -0.00851 -0.01162 0.00825 C32 1 0.300532 0.348814 0.659612 11.00000 0.02235 0.01895 = 0.04270 -0.01274 0.00926 -0.00827 C33 1 0.734901 0.143726 0.617708 11.00000 0.02627 0.02431 = 0.02108 0.00008 0.00770 0.00866 C34 1 0.719145 0.198353 0.671486 11.00000 0.02132 0.01874 = 0.02401 -0.00422 0.00164 0.00753 AFIX 43 H34 2 0.744722 0.199724 0.713846 11.00000 -1.20000 AFIX 0 C35 1 0.666598 0.249327 0.661914 11.00000 0.03358 0.02388 = 0.02098 -0.00194 0.00995 -0.00710 AFIX 43 H35 2 0.655963 0.286668 0.697637 11.00000 -1.20000 AFIX 0 C36 1 0.628527 0.246823 0.600023 11.00000 0.02184 0.01723 = 0.02916 0.00119 0.00465 0.00360 C37 1 0.646646 0.189635 0.550214 11.00000 0.02835 0.02576 = 0.03121 -0.00208 -0.00228 0.00659 AFIX 43 H37 2 0.621354 0.186802 0.507723 11.00000 -1.20000 AFIX 0 C38 1 0.572044 0.301963 0.584177 11.00000 0.02292 0.02010 = 0.02271 -0.00141 0.00179 -0.00358 C39 1 0.530390 0.330350 0.636876 11.00000 0.02841 0.02638 = 0.02708 -0.00017 0.00559 0.00107 AFIX 43 H39 2 0.538681 0.315077 0.684344 11.00000 -1.20000 AFIX 0 C40 1 0.476797 0.380598 0.622014 11.00000 0.03364 0.03655 = 0.03740 0.00066 0.01132 0.01006 AFIX 43 H40 2 0.448553 0.398684 0.658774 11.00000 -1.20000 AFIX 0 C41 1 0.465414 0.403471 0.554055 11.00000 0.02681 0.03908 = 0.03690 -0.00017 0.00282 0.01112 AFIX 43 H41 2 0.429164 0.438039 0.543619 11.00000 -1.20000 AFIX 0 C42 1 0.506327 0.376762 0.499608 11.00000 0.04672 0.05360 = 0.03314 0.01441 0.00259 0.01448 AFIX 43 H42 2 0.497994 0.392514 0.452272 11.00000 -1.20000 AFIX 0 C43 1 0.558598 0.327543 0.515573 11.00000 0.03672 0.03851 = 0.02250 -0.00399 0.00130 0.01259 AFIX 43 H43 2 0.586834 0.310097 0.478563 11.00000 -1.20000 AFIX 0 C44 1 0.820522 0.050076 0.680959 11.00000 0.02703 0.02516 = 0.03094 0.00326 0.00196 0.00464 C45 1 0.854884 -0.020664 0.653902 11.00000 0.16270 0.08935 = 0.04887 0.00568 -0.00667 0.07338 AFIX 33 H45A 2 0.889770 -0.004484 0.620787 11.00000 -1.20000 H45B 2 0.875266 -0.049756 0.693263 11.00000 -1.20000 H45C 2 0.822515 -0.054893 0.629626 11.00000 -1.20000 AFIX 0 C46 1 0.870104 0.106937 0.714194 11.00000 0.11751 0.08902 = 0.10969 0.02347 -0.08500 -0.00867 AFIX 33 H46A 2 0.846304 0.153612 0.731879 11.00000 -1.20000 H46B 2 0.893266 0.080556 0.753374 11.00000 -1.20000 H46C 2 0.902838 0.123450 0.678844 11.00000 -1.20000 AFIX 0 C47 1 0.766784 0.028717 0.731741 11.00000 0.09359 0.13475 = 0.07228 0.07502 0.01482 0.04436 AFIX 33 H47A 2 0.745008 0.077117 0.748658 11.00000 -1.20000 H47B 2 0.733639 -0.005070 0.708151 11.00000 -1.20000 H47C 2 0.786389 0.000067 0.771787 11.00000 -1.20000 AFIX 0 C48 1 0.733829 -0.109341 0.462325 11.00000 0.03129 0.01905 = 0.02697 -0.00705 -0.00308 -0.00004 C49 1 0.748466 -0.184581 0.432877 11.00000 0.03321 0.02851 = 0.02552 0.00065 0.00240 -0.00167 AFIX 43 H49 2 0.726262 -0.231214 0.448285 11.00000 -1.20000 AFIX 0 C50 1 0.795974 -0.187085 0.381291 11.00000 0.04655 0.02204 = 0.02864 -0.00402 0.00238 0.00703 AFIX 43 H50 2 0.805940 -0.236434 0.359605 11.00000 -1.20000 AFIX 0 C51 1 0.829622 -0.120557 0.359955 11.00000 0.01691 0.02498 = 0.02879 -0.00360 -0.01192 0.00454 C52 1 0.813841 -0.049500 0.394968 11.00000 0.02306 0.02800 = 0.02758 0.00153 -0.00152 -0.01180 AFIX 43 H52 2 0.838002 -0.002910 0.383116 11.00000 -1.20000 AFIX 0 C53 1 0.878264 -0.119564 0.302850 11.00000 0.02985 0.04123 = 0.02619 -0.01552 0.00285 -0.01019 C54 1 0.922832 -0.180767 0.291955 11.00000 0.03726 0.05543 = 0.04226 -0.02312 -0.00178 0.00959 AFIX 43 H54 2 0.921474 -0.225898 0.321887 11.00000 -1.20000 AFIX 0 C55 1 0.970048 -0.177799 0.237704 11.00000 0.05147 0.07288 = 0.06072 -0.04046 -0.00566 0.00436 AFIX 43 H55 2 1.000972 -0.219972 0.231554 11.00000 -1.20000 AFIX 0 C56 1 0.971161 -0.113773 0.193830 11.00000 0.04812 0.09874 = 0.05840 -0.02995 0.01346 -0.01443 AFIX 43 H56 2 1.002804 -0.111794 0.156695 11.00000 -1.20000 AFIX 0 C57 1 0.927360 -0.052433 0.202586 11.00000 0.07797 0.05255 = 0.05214 -0.01922 0.01780 -0.03251 AFIX 43 H57 2 0.927689 -0.009044 0.170646 11.00000 -1.20000 AFIX 0 C58 1 0.882629 -0.053362 0.257738 11.00000 0.06295 0.05504 = 0.03213 -0.01711 0.00584 -0.01157 AFIX 43 H58 2 0.854452 -0.008864 0.265387 11.00000 -1.20000 AFIX 0 C59 1 0.619688 -0.141567 0.525149 11.00000 0.03912 0.03550 = 0.02866 -0.00061 0.00674 -0.00366 C60 1 0.576545 -0.087774 0.569352 11.00000 0.04824 0.04881 = 0.06484 -0.01248 0.00884 -0.00448 AFIX 33 H60A 2 0.597475 -0.080320 0.615736 11.00000 -1.20000 H60B 2 0.571873 -0.036294 0.545869 11.00000 -1.20000 H60C 2 0.532273 -0.111782 0.575150 11.00000 -1.20000 AFIX 0 C61 1 0.589709 -0.155447 0.452234 11.00000 0.04067 0.06001 = 0.03904 0.00317 -0.01539 -0.00728 AFIX 33 H61A 2 0.619086 -0.190534 0.425253 11.00000 -1.20000 H61B 2 0.545569 -0.180117 0.456891 11.00000 -1.20000 H61C 2 0.585169 -0.104629 0.427609 11.00000 -1.20000 AFIX 0 C62 1 0.634330 -0.219941 0.562706 11.00000 0.05792 0.04287 = 0.03894 0.00714 -0.00244 -0.00752 AFIX 33 H62A 2 0.662361 -0.253297 0.532593 11.00000 -1.20000 H62B 2 0.657846 -0.209362 0.607205 11.00000 -1.20000 H62C 2 0.592167 -0.247399 0.572392 11.00000 -1.20000 AFIX 0 C63 1 0.620468 0.072991 0.379279 11.00000 0.02535 0.02023 = 0.03025 -0.00486 0.00290 -0.00257 C64 1 0.796019 0.145101 0.362562 11.00000 0.03793 0.01134 = 0.03933 -0.01034 -0.00780 -0.00156 HKLF 4 REM NiNCS140K REM R1 = 0.0997 for 5664 Fo > 4sig(Fo) and 0.2057 for all 11745 data REM 775 parameters refined using 0 restraints END WGHT 0.0230 64.7426 REM Instructions for potential hydrogen bonds EQIV $1 x, -y+1/2, z-1/2 HTAB C2 S2_$1 HTAB C5 N5 EQIV $2 -x+1, -y+1, -z+1 HTAB C17 N12_$2 HTAB C20 N6 EQIV $3 x, -y+1/2, z+1/2 HTAB C34 S4_$3 EQIV $4 -x+1, y-1/2, -z+3/2 HTAB C45 S1_$4 EQIV $5 -x+1, -y, -z+1 HTAB C49 N6_$5 HTAB C52 N12 REM Highest difference peak 1.380, deepest hole -0.589, 1-sigma level 0.121 Q1 1 0.7320 0.0585 0.4348 11.00000 0.05 1.38 Q2 1 0.2300 0.4432 0.4879 11.00000 0.05 1.24 Q3 1 0.8990 0.0430 0.6750 11.00000 0.05 0.80 Q4 1 0.8105 0.0614 0.5050 11.00000 0.05 0.79 Q5 1 0.8065 0.0882 0.7562 11.00000 0.05 0.77 Q6 1 0.3072 0.4419 0.5477 11.00000 0.05 0.68 Q7 1 0.1488 0.4381 0.5137 11.00000 0.05 0.55 Q8 1 0.5916 -0.0176 0.6797 11.00000 0.05 0.52 Q9 1 0.7967 -0.0407 0.6881 11.00000 0.05 0.51 Q10 1 0.8955 -0.0173 0.7131 11.00000 0.05 0.49 Q11 1 -0.0261 0.1195 0.3515 11.00000 0.05 0.49 Q12 1 0.3734 0.4400 0.5806 11.00000 0.05 0.48 Q13 1 0.3657 0.3795 0.3198 11.00000 0.05 0.47 Q14 1 0.5424 0.7782 0.7483 11.00000 0.05 0.46 Q15 1 0.1799 0.4797 0.4803 11.00000 0.05 0.46 Q16 1 0.5853 -0.0621 0.4726 11.00000 0.05 0.45 Q17 1 0.2604 0.4761 0.2302 11.00000 0.05 0.45 Q18 1 0.4512 0.4035 0.7484 11.00000 0.05 0.45 Q19 1 0.4920 -0.1190 0.4788 11.00000 0.05 0.43 Q20 1 0.4876 0.3179 0.4006 11.00000 0.05 0.43 Q21 1 0.3619 0.5248 0.3716 11.00000 0.05 0.43 Q22 1 0.3798 0.5392 0.7689 11.00000 0.05 0.43 Q23 1 0.4172 0.5855 0.8096 11.00000 0.05 0.42 Q24 1 0.9875 -0.1808 0.3080 11.00000 0.05 0.42 Q25 1 0.0774 0.1402 0.4756 11.00000 0.05 0.42 Q26 1 0.9470 0.0612 0.7807 11.00000 0.05 0.41 Q27 1 0.8001 -0.1129 0.7974 11.00000 0.05 0.41 Q28 1 0.5920 0.3416 0.6131 11.00000 0.05 0.41 Q29 1 0.1301 0.4554 0.5271 11.00000 0.05 0.41 Q30 1 1.0002 -0.0444 0.2121 11.00000 0.05 0.41 Q31 1 0.3073 0.4032 0.4312 11.00000 0.05 0.41 Q32 1 0.8971 0.1004 0.2827 11.00000 0.05 0.40 Q33 1 0.4168 0.3459 0.4833 11.00000 0.05 0.40 Q34 1 0.8673 -0.1138 0.6096 11.00000 0.05 0.39 Q35 1 0.7237 0.0571 0.5925 11.00000 0.05 0.39 Q36 1 0.8527 -0.1401 0.3943 11.00000 0.05 0.39 Q37 1 0.0252 0.4211 0.6051 11.00000 0.05 0.39 Q38 1 0.0345 0.5545 0.3967 11.00000 0.05 0.38 Q39 1 0.3269 0.5581 0.4801 11.00000 0.05 0.38 Q40 1 1.0479 -0.2391 0.2989 11.00000 0.05 0.38 Q41 1 0.6328 -0.0255 0.3479 11.00000 0.05 0.38 Q42 1 0.4222 0.7843 0.6359 11.00000 0.05 0.38 Q43 1 0.7763 0.1200 0.4620 11.00000 0.05 0.38 Q44 1 0.6744 0.0682 0.5574 11.00000 0.05 0.38 Q45 1 0.4518 0.4595 0.3115 11.00000 0.05 0.38 Q46 1 0.1175 0.6155 0.6346 11.00000 0.05 0.38 Q47 1 0.3339 0.3461 0.5126 11.00000 0.05 0.38 Q48 1 0.1456 0.6219 0.3688 11.00000 0.05 0.38 Q49 1 0.4844 0.4803 0.4169 11.00000 0.05 0.38 Q50 1 0.7712 0.1337 0.5243 11.00000 0.05 0.37 Q51 1 0.3363 0.5355 0.5121 11.00000 0.05 0.37 Q52 1 0.7310 0.1586 0.2800 11.00000 0.05 0.37 Q53 1 0.5822 0.4013 0.6876 11.00000 0.05 0.37 ; _shelx_res_checksum 18603 loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 +X,+Y,+Z 2 -X,1/2+Y,1/2-Z 3 -X,-Y,-Z 4 +X,-1/2-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 0.22956(6) 0.44176(6) 0.53701(6) 0.0244(3) Uani 1 1 d . . . . . Ni2 Ni 0.73083(6) 0.05702(7) 0.48845(6) 0.0273(3) Uani 1 1 d . . . . . S1 S 0.04464(15) 0.39098(19) 0.68477(15) 0.0542(8) Uani 1 1 d . . . . . S2 S 0.32934(14) 0.31806(18) 0.73480(14) 0.0484(8) Uani 1 1 d . . . . . S3 S 0.58087(15) 0.09765(16) 0.30652(13) 0.0458(7) Uani 1 1 d . . . . . S4 S 0.82428(15) 0.17260(16) 0.28445(13) 0.0461(7) Uani 1 1 d . . . . . O1 O 0.3060(3) 0.4317(3) 0.4657(3) 0.0297(15) Uani 1 1 d . . . . . O2 O 0.1874(3) 0.5273(3) 0.4745(3) 0.0331(16) Uani 1 1 d . . . . . O3 O 0.8098(3) 0.0706(4) 0.5568(3) 0.0336(16) Uani 1 1 d . . . . . O4 O 0.6966(3) -0.0319(3) 0.5527(3) 0.0311(15) Uani 1 1 d . . . . . N1 N 0.2858(3) 0.4090(4) 0.4049(3) 0.0234(17) Uani 1 1 d . . . . . N2 N 0.1961(3) 0.3610(4) 0.4647(3) 0.0210(16) Uani 1 1 d . . . . . N3 N 0.1832(4) 0.5950(4) 0.5079(4) 0.0281(18) Uani 1 1 d . . . . . N4 N 0.2687(3) 0.5440(4) 0.5772(3) 0.0199(16) Uani 1 1 d . . . . . N5 N 0.1483(4) 0.4395(5) 0.5990(4) 0.0328(19) Uani 1 1 d . . . . . N6 N 0.2810(4) 0.3702(4) 0.6042(4) 0.0314(19) Uani 1 1 d . . . . . N7 N 0.7882(4) 0.0914(4) 0.6192(3) 0.0231(17) Uani 1 1 d . . . . . N8 N 0.6972(4) 0.1388(4) 0.5587(3) 0.0237(17) Uani 1 1 d . . . . . N9 N 0.6857(4) -0.0958(4) 0.5159(3) 0.0267(18) Uani 1 1 d . . . . . N10 N 0.7664(4) -0.0445(4) 0.4441(3) 0.0232(17) Uani 1 1 d . . . . . N11 N 0.6464(4) 0.0556(5) 0.4296(4) 0.038(2) Uani 1 1 d . . . . . N12 N 0.7765(4) 0.1285(4) 0.4181(4) 0.032(2) Uani 1 1 d . . . . . C1 C 0.2307(4) 0.3554(5) 0.4056(4) 0.021(2) Uani 1 1 d . . . . . C2 C 0.2160(4) 0.3002(5) 0.3527(4) 0.027(2) Uani 1 1 d . . . . . H2 H 0.2412 0.2982 0.3104 0.033 Uiso 1 1 calc R U . . . C3 C 0.1631(4) 0.2485(5) 0.3644(4) 0.024(2) Uani 1 1 d . . . . . H3 H 0.1523 0.2101 0.3296 0.029 Uiso 1 1 calc R U . . . C4 C 0.1257(4) 0.2517(5) 0.4255(4) 0.022(2) Uani 1 1 d . . . . . C5 C 0.1443(4) 0.3111(5) 0.4733(4) 0.028(2) Uani 1 1 d . . . . . H5 H 0.1184 0.3166 0.5149 0.033 Uiso 1 1 calc R U . . . C6 C 0.0693(4) 0.1979(5) 0.4396(5) 0.025(2) Uani 1 1 d . . . . . C7 C 0.0339(4) 0.1622(5) 0.3838(5) 0.029(2) Uani 1 1 d . . . . . H7 H 0.0456 0.1730 0.3363 0.035 Uiso 1 1 calc R U . . . C8 C -0.0189(5) 0.1107(5) 0.3990(6) 0.038(3) Uani 1 1 d . . . . . H8 H -0.0425 0.0859 0.3613 0.046 Uiso 1 1 calc R U . . . C9 C -0.0370(5) 0.0952(6) 0.4666(6) 0.038(3) Uani 1 1 d . . . . . H9 H -0.0739 0.0613 0.4758 0.046 Uiso 1 1 calc R U . . . C10 C -0.0022(5) 0.1285(6) 0.5218(5) 0.038(3) Uani 1 1 d . . . . . H10 H -0.0139 0.1162 0.5691 0.045 Uiso 1 1 calc R U . . . C11 C 0.0503(5) 0.1804(5) 0.5083(5) 0.032(2) Uani 1 1 d . . . . . H11 H 0.0736 0.2042 0.5466 0.038 Uiso 1 1 calc R U . . . C12 C 0.3160(4) 0.4555(5) 0.3432(4) 0.026(2) Uani 1 1 d . . . . . C13 C 0.3907(5) 0.4603(7) 0.3606(5) 0.048(3) Uani 1 1 d . . . . . H13A H 0.3968 0.4857 0.4067 0.058 Uiso 1 1 calc R U . . . H13B H 0.4096 0.4068 0.3619 0.058 Uiso 1 1 calc R U . . . H13C H 0.4134 0.4916 0.3244 0.058 Uiso 1 1 calc R U . . . C14 C 0.2851(6) 0.5375(5) 0.3451(5) 0.045(3) Uani 1 1 d . . . . . H14A H 0.2928 0.5614 0.3915 0.054 Uiso 1 1 calc R U . . . H14B H 0.3055 0.5708 0.3087 0.054 Uiso 1 1 calc R U . . . H14C H 0.2368 0.5335 0.3362 0.054 Uiso 1 1 calc R U . . . C15 C 0.3054(5) 0.4174(6) 0.2737(4) 0.037(2) Uani 1 1 d . . . . . H15A H 0.3258 0.3646 0.2739 0.045 Uiso 1 1 calc R U . . . H15B H 0.2573 0.4125 0.2644 0.045 Uiso 1 1 calc R U . . . H15C H 0.3260 0.4498 0.2369 0.045 Uiso 1 1 calc R U . . . C16 C 0.2373(4) 0.6106(5) 0.5542(4) 0.020(2) Uani 1 1 d . . . . . C17 C 0.2591(4) 0.6861(5) 0.5741(5) 0.028(2) Uani 1 1 d . . . . . H17 H 0.2370 0.7321 0.5568 0.033 Uiso 1 1 calc R U . . . C18 C 0.3113(5) 0.6927(5) 0.6176(5) 0.029(2) Uani 1 1 d . . . . . H18 H 0.3255 0.7440 0.6320 0.035 Uiso 1 1 calc R U . . . C19 C 0.3465(4) 0.6251(5) 0.6431(5) 0.029(2) Uani 1 1 d . . . . . C20 C 0.3217(5) 0.5521(5) 0.6186(4) 0.027(2) Uani 1 1 d . . . . . H20 H 0.3446 0.5054 0.6329 0.033 Uiso 1 1 calc R U . . . C21 C 0.4046(4) 0.6303(5) 0.6899(5) 0.029(2) Uani 1 1 d . . . . . C22 C 0.4488(5) 0.6945(6) 0.6825(5) 0.035(2) Uani 1 1 d . . . . . H22 H 0.4401 0.7338 0.6476 0.042 Uiso 1 1 calc R U . . . C23 C 0.5053(5) 0.7014(7) 0.7257(5) 0.047(3) Uani 1 1 d . . . . . H23 H 0.5351 0.7447 0.7196 0.057 Uiso 1 1 calc R U . . . C24 C 0.5180(6) 0.6455(8) 0.7773(6) 0.056(3) Uani 1 1 d . . . . . H24 H 0.5560 0.6508 0.8072 0.067 Uiso 1 1 calc R U . . . C25 C 0.4749(6) 0.5816(7) 0.7854(5) 0.049(3) Uani 1 1 d . . . . . H25 H 0.4836 0.5430 0.8208 0.059 Uiso 1 1 calc R U . . . C26 C 0.4181(5) 0.5736(6) 0.7410(5) 0.040(3) Uani 1 1 d . . . . . H26 H 0.3892 0.5293 0.7462 0.048 Uiso 1 1 calc R U . . . C27 C 0.1204(5) 0.6429(5) 0.4979(5) 0.030(2) Uani 1 1 d . . . . . C28 C 0.0651(6) 0.5867(7) 0.4820(7) 0.071(4) Uani 1 1 d . . . . . H28A H 0.0234 0.6162 0.4752 0.085 Uiso 1 1 calc R U . . . H28B H 0.0755 0.5571 0.4389 0.085 Uiso 1 1 calc R U . . . H28C H 0.0601 0.5495 0.5214 0.085 Uiso 1 1 calc R U . . . C29 C 0.1321(7) 0.6984(8) 0.4348(6) 0.087(5) Uani 1 1 d . . . . . H29A H 0.1687 0.7352 0.4460 0.104 Uiso 1 1 calc R U . . . H29B H 0.1440 0.6669 0.3933 0.104 Uiso 1 1 calc R U . . . H29C H 0.0912 0.7286 0.4250 0.104 Uiso 1 1 calc R U . . . C30 C 0.1048(5) 0.6882(7) 0.5652(5) 0.050(3) Uani 1 1 d . . . . . H30A H 0.1412 0.7253 0.5756 0.060 Uiso 1 1 calc R U . . . H30B H 0.0629 0.7178 0.5589 0.060 Uiso 1 1 calc R U . . . H30C H 0.1000 0.6508 0.6043 0.060 Uiso 1 1 calc R U . . . C31 C 0.1062(5) 0.4193(5) 0.6343(5) 0.030(2) Uani 1 1 d . . . . . C32 C 0.3005(4) 0.3488(5) 0.6596(5) 0.028(2) Uani 1 1 d . . . . . C33 C 0.7349(4) 0.1437(5) 0.6177(4) 0.024(2) Uani 1 1 d . . . . . C34 C 0.7191(4) 0.1984(5) 0.6715(4) 0.021(2) Uani 1 1 d . . . . . H34 H 0.7447 0.1997 0.7138 0.026 Uiso 1 1 calc R U . . . C35 C 0.6666(4) 0.2493(5) 0.6619(4) 0.026(2) Uani 1 1 d . . . . . H35 H 0.6560 0.2867 0.6976 0.031 Uiso 1 1 calc R U . . . C36 C 0.6285(4) 0.2468(5) 0.6000(4) 0.023(2) Uani 1 1 d . . . . . C37 C 0.6466(4) 0.1896(5) 0.5502(5) 0.028(2) Uani 1 1 d . . . . . H37 H 0.6214 0.1868 0.5077 0.034 Uiso 1 1 calc R U . . . C38 C 0.5720(4) 0.3020(5) 0.5842(4) 0.022(2) Uani 1 1 d . . . . . C39 C 0.5304(4) 0.3303(5) 0.6369(5) 0.027(2) Uani 1 1 d . . . . . H39 H 0.5387 0.3151 0.6843 0.033 Uiso 1 1 calc R U . . . C40 C 0.4768(5) 0.3806(5) 0.6220(5) 0.036(2) Uani 1 1 d . . . . . H40 H 0.4486 0.3987 0.6588 0.043 Uiso 1 1 calc R U . . . C41 C 0.4654(5) 0.4035(6) 0.5541(5) 0.034(2) Uani 1 1 d . . . . . H41 H 0.4292 0.4380 0.5436 0.041 Uiso 1 1 calc R U . . . C42 C 0.5063(5) 0.3768(6) 0.4996(5) 0.044(3) Uani 1 1 d . . . . . H42 H 0.4980 0.3925 0.4523 0.053 Uiso 1 1 calc R U . . . C43 C 0.5586(5) 0.3275(5) 0.5156(4) 0.033(2) Uani 1 1 d . . . . . H43 H 0.5868 0.3101 0.4786 0.039 Uiso 1 1 calc R U . . . C44 C 0.8205(4) 0.0501(5) 0.6810(5) 0.028(2) Uani 1 1 d . . . . . C45 C 0.8549(8) -0.0207(8) 0.6539(6) 0.100(6) Uani 1 1 d . . . . . H45A H 0.8898 -0.0045 0.6208 0.120 Uiso 1 1 calc R U . . . H45B H 0.8753 -0.0498 0.6933 0.120 Uiso 1 1 calc R U . . . H45C H 0.8225 -0.0549 0.6296 0.120 Uiso 1 1 calc R U . . . C46 C 0.8701(7) 0.1069(8) 0.7142(8) 0.106(6) Uani 1 1 d . . . . . H46A H 0.8463 0.1536 0.7319 0.127 Uiso 1 1 calc R U . . . H46B H 0.8933 0.0806 0.7534 0.127 Uiso 1 1 calc R U . . . H46C H 0.9028 0.1234 0.6788 0.127 Uiso 1 1 calc R U . . . C47 C 0.7668(7) 0.0287(9) 0.7317(7) 0.100(6) Uani 1 1 d . . . . . H47A H 0.7450 0.0771 0.7487 0.120 Uiso 1 1 calc R U . . . H47B H 0.7336 -0.0051 0.7082 0.120 Uiso 1 1 calc R U . . . H47C H 0.7864 0.0001 0.7718 0.120 Uiso 1 1 calc R U . . . C48 C 0.7338(4) -0.1093(5) 0.4623(4) 0.026(2) Uani 1 1 d . . . . . C49 C 0.7485(5) -0.1846(5) 0.4329(4) 0.029(2) Uani 1 1 d . . . . . H49 H 0.7263 -0.2312 0.4483 0.035 Uiso 1 1 calc R U . . . C50 C 0.7960(5) -0.1871(5) 0.3813(5) 0.032(2) Uani 1 1 d . . . . . H50 H 0.8059 -0.2364 0.3596 0.039 Uiso 1 1 calc R U . . . C51 C 0.8296(4) -0.1206(5) 0.3600(4) 0.024(2) Uani 1 1 d . . . . . C52 C 0.8138(4) -0.0495(5) 0.3950(4) 0.026(2) Uani 1 1 d . . . . . H52 H 0.8380 -0.0029 0.3831 0.031 Uiso 1 1 calc R U . . . C53 C 0.8783(5) -0.1196(6) 0.3029(5) 0.032(2) Uani 1 1 d . . . . . C54 C 0.9228(5) -0.1808(7) 0.2920(5) 0.045(3) Uani 1 1 d . . . . . H54 H 0.9215 -0.2259 0.3219 0.054 Uiso 1 1 calc R U . . . C55 C 0.9700(6) -0.1778(8) 0.2377(6) 0.062(4) Uani 1 1 d . . . . . H55 H 1.0010 -0.2200 0.2316 0.074 Uiso 1 1 calc R U . . . C56 C 0.9712(6) -0.1138(9) 0.1938(7) 0.068(4) Uani 1 1 d . . . . . H56 H 1.0028 -0.1118 0.1567 0.082 Uiso 1 1 calc R U . . . C57 C 0.9274(6) -0.0524(7) 0.2026(6) 0.061(3) Uani 1 1 d . . . . . H57 H 0.9277 -0.0090 0.1706 0.073 Uiso 1 1 calc R U . . . C58 C 0.8826(6) -0.0534(7) 0.2577(5) 0.050(3) Uani 1 1 d . . . . . H58 H 0.8545 -0.0089 0.2654 0.060 Uiso 1 1 calc R U . . . C59 C 0.6197(5) -0.1416(6) 0.5251(5) 0.034(2) Uani 1 1 d . . . . . C60 C 0.5765(5) -0.0878(6) 0.5694(6) 0.054(3) Uani 1 1 d . . . . . H60A H 0.5975 -0.0803 0.6157 0.065 Uiso 1 1 calc R U . . . H60B H 0.5719 -0.0363 0.5459 0.065 Uiso 1 1 calc R U . . . H60C H 0.5323 -0.1118 0.5752 0.065 Uiso 1 1 calc R U . . . C61 C 0.5897(5) -0.1554(6) 0.4522(5) 0.047(3) Uani 1 1 d . . . . . H61A H 0.6191 -0.1905 0.4253 0.056 Uiso 1 1 calc R U . . . H61B H 0.5456 -0.1801 0.4569 0.056 Uiso 1 1 calc R U . . . H61C H 0.5852 -0.1046 0.4276 0.056 Uiso 1 1 calc R U . . . C62 C 0.6343(5) -0.2199(6) 0.5627(5) 0.047(3) Uani 1 1 d . . . . . H62A H 0.6624 -0.2533 0.5326 0.056 Uiso 1 1 calc R U . . . H62B H 0.6578 -0.2094 0.6072 0.056 Uiso 1 1 calc R U . . . H62C H 0.5922 -0.2474 0.5724 0.056 Uiso 1 1 calc R U . . . C63 C 0.6205(4) 0.0730(5) 0.3793(5) 0.025(2) Uani 1 1 d . . . . . C64 C 0.7960(5) 0.1451(5) 0.3626(5) 0.030(2) 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 Ni1 0.0284(7) 0.0202(6) 0.0245(6) -0.0029(5) -0.0013(5) -0.0018(5) Ni2 0.0336(7) 0.0207(6) 0.0276(6) -0.0055(5) -0.0009(5) 0.0044(6) S1 0.050(2) 0.067(2) 0.0449(17) 0.0110(15) 0.0107(14) 0.0065(16) S2 0.0471(18) 0.0617(19) 0.0363(15) 0.0193(14) -0.0062(13) -0.0011(15) S3 0.0552(19) 0.0479(17) 0.0341(14) 0.0028(13) -0.0093(13) 0.0051(14) S4 0.065(2) 0.0393(15) 0.0345(14) 0.0036(12) 0.0011(14) 0.0004(14) O1 0.034(4) 0.035(4) 0.020(3) -0.005(3) -0.005(3) -0.002(3) O2 0.040(4) 0.024(3) 0.035(4) -0.009(3) -0.002(3) 0.003(3) O3 0.028(4) 0.035(4) 0.038(4) -0.008(3) -0.001(3) 0.004(3) O4 0.041(4) 0.022(3) 0.030(3) -0.006(3) 0.006(3) 0.002(3) N1 0.026(4) 0.024(4) 0.020(4) 0.000(3) 0.005(3) 0.007(3) N2 0.018(4) 0.021(4) 0.024(4) 0.007(3) 0.002(3) 0.003(3) N3 0.031(5) 0.021(4) 0.032(4) 0.002(4) 0.001(4) -0.002(4) N4 0.017(4) 0.021(4) 0.022(4) -0.001(3) -0.004(3) -0.001(3) N5 0.029(5) 0.039(5) 0.030(4) -0.007(4) 0.003(4) -0.007(4) N6 0.035(5) 0.025(4) 0.034(5) -0.005(4) 0.000(4) -0.006(4) N7 0.027(4) 0.024(4) 0.019(4) -0.003(3) 0.008(3) 0.000(3) N8 0.028(5) 0.022(4) 0.021(4) -0.003(3) 0.002(3) 0.006(3) N9 0.028(5) 0.031(4) 0.022(4) 0.000(3) 0.003(3) 0.004(4) N10 0.029(5) 0.016(4) 0.024(4) -0.002(3) -0.003(4) -0.003(3) N11 0.053(6) 0.032(5) 0.030(5) -0.008(4) 0.003(4) 0.009(4) N12 0.049(6) 0.016(4) 0.031(5) 0.002(3) -0.002(4) 0.008(4) C1 0.020(5) 0.017(4) 0.025(5) 0.001(4) -0.002(4) -0.002(4) C2 0.028(6) 0.032(5) 0.022(5) -0.008(4) 0.005(4) 0.002(5) C3 0.036(6) 0.017(4) 0.019(5) -0.010(4) -0.008(4) -0.001(4) C4 0.023(5) 0.021(5) 0.021(5) -0.001(4) -0.003(4) 0.002(4) C5 0.026(6) 0.031(5) 0.026(5) -0.005(4) 0.001(4) 0.006(5) C6 0.019(5) 0.016(5) 0.041(6) -0.006(4) -0.004(4) 0.005(4) C7 0.024(6) 0.028(5) 0.035(5) 0.001(4) -0.005(4) 0.007(4) C8 0.030(6) 0.028(5) 0.057(7) -0.010(5) -0.001(5) -0.001(5) C9 0.012(5) 0.039(6) 0.064(7) -0.002(6) 0.012(5) -0.005(5) C10 0.033(6) 0.039(6) 0.042(6) 0.006(5) 0.015(5) -0.011(5) C11 0.035(6) 0.037(6) 0.023(5) -0.010(4) -0.004(4) 0.008(5) C12 0.025(5) 0.029(5) 0.025(5) 0.002(4) 0.005(4) -0.006(4) C13 0.034(7) 0.081(9) 0.030(6) 0.005(6) 0.001(5) -0.006(6) C14 0.069(8) 0.033(6) 0.034(6) 0.014(5) 0.003(5) 0.007(5) C15 0.042(7) 0.044(6) 0.026(5) 0.004(4) 0.003(5) -0.009(5) C16 0.014(5) 0.015(4) 0.031(5) -0.001(4) 0.011(4) 0.004(4) C17 0.025(6) 0.014(5) 0.045(6) -0.003(4) 0.009(5) -0.001(4) C18 0.029(6) 0.018(5) 0.040(6) -0.007(4) 0.005(5) 0.003(4) C19 0.026(6) 0.027(5) 0.035(5) 0.002(4) 0.004(4) -0.002(4) C20 0.036(6) 0.023(5) 0.024(5) -0.003(4) 0.009(4) 0.001(5) C21 0.026(6) 0.032(5) 0.028(5) -0.011(4) -0.004(4) 0.001(4) C22 0.033(6) 0.040(6) 0.032(5) -0.010(5) -0.005(5) -0.001(5) C23 0.050(8) 0.050(7) 0.041(6) -0.015(6) 0.001(6) -0.001(6) C24 0.034(7) 0.076(9) 0.058(8) -0.024(7) 0.006(6) -0.001(7) C25 0.051(8) 0.064(8) 0.031(6) -0.005(5) -0.001(5) 0.022(6) C26 0.032(6) 0.043(6) 0.045(6) -0.002(5) 0.001(5) 0.004(5) C27 0.026(6) 0.030(5) 0.035(5) 0.000(4) -0.006(4) 0.006(4) C28 0.052(8) 0.068(8) 0.094(10) -0.023(7) -0.040(7) 0.026(7) C29 0.087(11) 0.098(11) 0.075(9) 0.059(8) 0.031(8) 0.054(9) C30 0.018(6) 0.070(8) 0.062(7) -0.024(6) 0.008(5) 0.011(5) C31 0.029(6) 0.030(5) 0.031(5) -0.009(4) -0.012(5) 0.008(5) C32 0.022(6) 0.019(5) 0.043(6) -0.013(4) 0.009(5) -0.008(4) C33 0.026(5) 0.024(5) 0.021(5) 0.000(4) 0.008(4) 0.009(4) C34 0.021(5) 0.019(4) 0.024(5) -0.004(4) 0.002(4) 0.008(4) C35 0.034(6) 0.024(5) 0.021(5) -0.002(4) 0.010(4) -0.007(4) C36 0.022(5) 0.017(4) 0.029(5) 0.001(4) 0.005(4) 0.004(4) C37 0.028(6) 0.026(5) 0.031(5) -0.002(4) -0.002(4) 0.007(4) C38 0.023(5) 0.020(5) 0.023(5) -0.001(4) 0.002(4) -0.004(4) C39 0.028(6) 0.026(5) 0.027(5) 0.000(4) 0.006(4) 0.001(4) C40 0.034(6) 0.037(6) 0.037(6) 0.001(5) 0.011(5) 0.010(5) C41 0.027(6) 0.039(6) 0.037(6) 0.000(5) 0.003(5) 0.011(5) C42 0.047(7) 0.054(7) 0.033(6) 0.014(5) 0.003(5) 0.014(6) C43 0.037(6) 0.039(6) 0.022(5) -0.004(4) 0.001(4) 0.013(5) C44 0.027(5) 0.025(5) 0.031(5) 0.003(4) 0.002(4) 0.005(4) C45 0.163(16) 0.089(11) 0.049(8) 0.006(7) -0.007(9) 0.073(11) C46 0.118(13) 0.089(11) 0.110(12) 0.023(10) -0.085(11) -0.009(10) C47 0.094(12) 0.135(14) 0.072(9) 0.075(10) 0.015(8) 0.044(10) C48 0.031(6) 0.019(5) 0.027(5) -0.007(4) -0.003(4) 0.000(4) C49 0.033(6) 0.029(5) 0.026(5) 0.001(4) 0.002(4) -0.002(4) C50 0.047(7) 0.022(5) 0.029(5) -0.004(4) 0.002(5) 0.007(5) C51 0.017(5) 0.025(5) 0.029(5) -0.004(4) -0.012(4) 0.005(4) C52 0.023(5) 0.028(5) 0.028(5) 0.002(4) -0.002(4) -0.012(4) C53 0.030(6) 0.041(6) 0.026(5) -0.016(5) 0.003(4) -0.010(5) C54 0.037(7) 0.055(7) 0.042(6) -0.023(5) -0.002(5) 0.010(6) C55 0.051(8) 0.073(9) 0.061(8) -0.040(7) -0.006(7) 0.004(7) C56 0.048(9) 0.099(11) 0.058(8) -0.030(9) 0.013(7) -0.014(8) C57 0.078(9) 0.053(8) 0.052(7) -0.019(6) 0.018(7) -0.033(7) C58 0.063(8) 0.055(7) 0.032(6) -0.017(6) 0.006(6) -0.012(6) C59 0.039(6) 0.035(6) 0.029(5) -0.001(4) 0.007(5) -0.004(5) C60 0.048(8) 0.049(7) 0.065(8) -0.012(6) 0.009(6) -0.004(6) C61 0.041(7) 0.060(7) 0.039(6) 0.003(5) -0.015(5) -0.007(6) C62 0.058(8) 0.043(6) 0.039(6) 0.007(5) -0.002(6) -0.008(6) C63 0.025(5) 0.020(5) 0.030(5) -0.005(4) 0.003(4) -0.003(4) C64 0.038(6) 0.011(4) 0.039(6) -0.010(4) -0.008(5) -0.002(4) 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 91.7(3) . . ? N5 Ni1 N4 96.2(3) . . ? N6 Ni1 N4 94.4(3) . . ? N5 Ni1 N2 96.7(3) . . ? N6 Ni1 N2 100.8(3) . . ? N4 Ni1 N2 159.7(3) . . ? N5 Ni1 O2 91.2(3) . . ? N6 Ni1 O2 171.2(3) . . ? N4 Ni1 O2 77.1(2) . . ? N2 Ni1 O2 87.1(2) . . ? N5 Ni1 O1 171.9(3) . . ? N6 Ni1 O1 89.4(3) . . ? N4 Ni1 O1 91.8(2) . . ? N2 Ni1 O1 75.2(3) . . ? O2 Ni1 O1 88.9(2) . . ? N11 Ni2 N12 91.2(3) . . ? N11 Ni2 N8 95.3(3) . . ? N12 Ni2 N8 100.4(3) . . ? N11 Ni2 N10 93.1(3) . . ? N12 Ni2 N10 93.9(3) . . ? N8 Ni2 N10 163.2(3) . . ? N11 Ni2 O3 171.8(3) . . ? N12 Ni2 O3 90.1(3) . . ? N8 Ni2 O3 76.5(3) . . ? N10 Ni2 O3 94.9(3) . . ? N11 Ni2 O4 92.3(3) . . ? N12 Ni2 O4 169.0(3) . . ? N8 Ni2 O4 89.7(2) . . ? N10 Ni2 O4 75.5(3) . . ? O3 Ni2 O4 88.0(2) . . ? N1 O1 Ni1 112.8(5) . . ? N3 O2 Ni1 111.2(5) . . ? N7 O3 Ni2 110.1(5) . . ? N9 O4 Ni2 110.0(5) . . ? O1 N1 C1 114.9(6) . . ? O1 N1 C12 114.2(6) . . ? C1 N1 C12 129.7(6) . . ? C1 N2 C5 117.7(7) . . ? C1 N2 Ni1 116.5(6) . . ? C5 N2 Ni1 125.8(6) . . ? O2 N3 C16 114.4(7) . . ? O2 N3 C27 117.6(7) . . ? C16 N3 C27 127.8(7) . . ? C20 N4 C16 118.1(7) . . ? C20 N4 Ni1 127.9(6) . . ? C16 N4 Ni1 113.8(5) . . ? C31 N5 Ni1 163.4(8) . . ? C32 N6 Ni1 155.2(7) . . ? O3 N7 C33 114.2(6) . . ? O3 N7 C44 115.8(6) . . ? C33 N7 C44 129.7(7) . . ? C37 N8 C33 118.7(7) . . ? C37 N8 Ni2 127.6(6) . . ? C33 N8 Ni2 113.6(5) . . ? O4 N9 C48 113.8(7) . . ? O4 N9 C59 119.7(7) . . ? C48 N9 C59 125.8(7) . . ? C48 N10 C52 119.0(7) . . ? C48 N10 Ni2 114.4(6) . . ? C52 N10 Ni2 126.3(6) . . ? C63 N11 Ni2 148.0(8) . . ? C64 N12 Ni2 154.1(7) . . ? N2 C1 C2 123.1(8) . . ? N2 C1 N1 111.8(7) . . ? C2 C1 N1 125.0(8) . . ? C3 C2 C1 117.3(8) . . ? C3 C2 H2 121.3 . . ? C1 C2 H2 121.3 . . ? C4 C3 C2 121.7(8) . . ? C4 C3 H3 119.2 . . ? C2 C3 H3 119.2 . . ? C3 C4 C5 115.4(8) . . ? C3 C4 C6 123.1(8) . . ? C5 C4 C6 121.5(8) . . ? N2 C5 C4 124.8(8) . . ? N2 C5 H5 117.6 . . ? C4 C5 H5 117.6 . . ? C11 C6 C7 118.4(8) . . ? C11 C6 C4 121.0(8) . . ? C7 C6 C4 120.6(8) . . ? C8 C7 C6 119.2(9) . . ? C8 C7 H7 120.4 . . ? C6 C7 H7 120.4 . . ? C9 C8 C7 121.2(9) . . ? C9 C8 H8 119.4 . . ? C7 C8 H8 119.4 . . ? C8 C9 C10 120.3(9) . . ? C8 C9 H9 119.9 . . ? C10 C9 H9 119.9 . . ? C9 C10 C11 119.7(9) . . ? C9 C10 H10 120.2 . . ? C11 C10 H10 120.2 . . ? C6 C11 C10 121.2(8) . . ? C6 C11 H11 119.4 . . ? C10 C11 H11 119.4 . . ? C15 C12 C14 111.2(8) . . ? C15 C12 C13 110.5(8) . . ? C14 C12 C13 110.1(8) . . ? C15 C12 N1 113.6(7) . . ? C14 C12 N1 106.6(7) . . ? C13 C12 N1 104.5(7) . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C12 C15 H15A 109.5 . . ? C12 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C12 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N4 C16 C17 121.7(8) . . ? N4 C16 N3 113.3(7) . . ? C17 C16 N3 125.0(8) . . ? C18 C17 C16 119.0(8) . . ? C18 C17 H17 120.5 . . ? C16 C17 H17 120.5 . . ? C17 C18 C19 121.9(8) . . ? C17 C18 H18 119.1 . . ? C19 C18 H18 119.1 . . ? C20 C19 C18 114.7(8) . . ? C20 C19 C21 122.0(8) . . ? C18 C19 C21 123.3(8) . . ? N4 C20 C19 124.6(8) . . ? N4 C20 H20 117.7 . . ? C19 C20 H20 117.7 . . ? C26 C21 C22 118.8(9) . . ? C26 C21 C19 122.4(9) . . ? C22 C21 C19 118.9(8) . . ? C23 C22 C21 120.7(9) . . ? C23 C22 H22 119.6 . . ? C21 C22 H22 119.6 . . ? C24 C23 C22 120.2(11) . . ? C24 C23 H23 119.9 . . ? C22 C23 H23 119.9 . . ? C23 C24 C25 119.8(11) . . ? C23 C24 H24 120.1 . . ? C25 C24 H24 120.1 . . ? C24 C25 C26 120.2(10) . . ? C24 C25 H25 119.9 . . ? C26 C25 H25 119.9 . . ? C21 C26 C25 120.2(10) . . ? C21 C26 H26 119.9 . . ? C25 C26 H26 119.9 . . ? C28 C27 N3 107.6(8) . . ? C28 C27 C30 109.5(9) . . ? N3 C27 C30 109.9(7) . . ? C28 C27 C29 110.3(9) . . ? N3 C27 C29 107.1(8) . . ? C30 C27 C29 112.3(9) . . ? 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 179.2(10) . . ? N6 C32 S2 178.3(9) . . ? N8 C33 N7 113.9(7) . . ? N8 C33 C34 121.0(7) . . ? N7 C33 C34 125.2(8) . . ? C35 C34 C33 119.2(8) . . ? C35 C34 H34 120.4 . . ? C33 C34 H34 120.4 . . ? C34 C35 C36 120.5(8) . . ? C34 C35 H35 119.8 . . ? C36 C35 H35 119.8 . . ? C35 C36 C37 116.5(8) . . ? C35 C36 C38 124.0(7) . . ? C37 C36 C38 119.5(7) . . ? N8 C37 C36 124.1(8) . . ? N8 C37 H37 118.0 . . ? C36 C37 H37 118.0 . . ? C39 C38 C43 116.8(8) . . ? C39 C38 C36 121.7(7) . . ? C43 C38 C36 121.5(8) . . ? C38 C39 C40 121.8(8) . . ? C38 C39 H39 119.1 . . ? C40 C39 H39 119.1 . . ? C41 C40 C39 119.2(9) . . ? C41 C40 H40 120.4 . . ? C39 C40 H40 120.4 . . ? C40 C41 C42 120.9(9) . . ? C40 C41 H41 119.6 . . ? C42 C41 H41 119.6 . . ? C43 C42 C41 118.9(9) . . ? C43 C42 H42 120.6 . . ? C41 C42 H42 120.6 . . ? C42 C43 C38 122.5(9) . . ? C42 C43 H43 118.8 . . ? C38 C43 H43 118.8 . . ? C45 C44 C47 111.7(10) . . ? C45 C44 N7 107.7(8) . . ? C47 C44 N7 107.8(8) . . ? C45 C44 C46 110.7(11) . . ? C47 C44 C46 110.9(11) . . ? N7 C44 C46 107.9(8) . . ? 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 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 . . ? 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 . . ? N10 C48 C49 122.3(8) . . ? N10 C48 N9 113.1(7) . . ? C49 C48 N9 124.6(8) . . ? C50 C49 C48 117.1(8) . . ? C50 C49 H49 121.5 . . ? C48 C49 H49 121.5 . . ? C49 C50 C51 122.0(8) . . ? C49 C50 H50 119.0 . . ? C51 C50 H50 119.0 . . ? C50 C51 C52 116.5(8) . . ? C50 C51 C53 124.0(8) . . ? C52 C51 C53 119.5(8) . . ? N10 C52 C51 123.0(8) . . ? N10 C52 H52 118.5 . . ? C51 C52 H52 118.5 . . ? C54 C53 C58 117.3(9) . . ? C54 C53 C51 122.4(9) . . ? C58 C53 C51 120.2(9) . . ? C53 C54 C55 121.4(11) . . ? C53 C54 H54 119.3 . . ? C55 C54 H54 119.3 . . ? C56 C55 C54 119.3(12) . . ? C56 C55 H55 120.3 . . ? C54 C55 H55 120.3 . . ? C55 C56 C57 120.8(12) . . ? C55 C56 H56 119.6 . . ? C57 C56 H56 119.6 . . ? C56 C57 C58 120.1(12) . . ? C56 C57 H57 119.9 . . ? C58 C57 H57 119.9 . . ? C57 C58 C53 120.8(11) . . ? C57 C58 H58 119.6 . . ? C53 C58 H58 119.6 . . ? C60 C59 C61 112.0(9) . . ? C60 C59 C62 111.7(8) . . ? C61 C59 C62 111.3(8) . . ? C60 C59 N9 104.8(8) . . ? C61 C59 N9 107.9(7) . . ? C62 C59 N9 108.9(8) . . ? C59 C60 H60A 109.5 . . ? C59 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? C59 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? C59 C61 H61A 109.5 . . ? C59 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? C59 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? C59 C62 H62A 109.5 . . ? C59 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C59 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? N11 C63 S3 178.6(9) . . ? N12 C64 S4 177.6(8) . . ? 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 2.012(8) . ? Ni1 N6 2.030(8) . ? Ni1 N4 2.039(6) . ? Ni1 N2 2.042(7) . ? Ni1 O2 2.046(6) . ? Ni1 O1 2.053(6) . ? Ni2 N11 2.019(9) . ? Ni2 N12 2.020(8) . ? Ni2 N8 2.034(7) . ? Ni2 N10 2.039(7) . ? Ni2 O3 2.049(6) . ? Ni2 O4 2.052(6) . ? S1 C31 1.635(11) . ? S2 C32 1.620(10) . ? S3 C63 1.640(10) . ? S4 C64 1.655(11) . ? O1 N1 1.278(8) . ? O2 N3 1.309(8) . ? O3 N7 1.312(8) . ? O4 N9 1.302(8) . ? N1 C1 1.424(10) . ? N1 C12 1.536(10) . ? N2 C1 1.324(10) . ? N2 C5 1.346(11) . ? N3 C16 1.414(10) . ? N3 C27 1.503(11) . ? N4 C20 1.323(10) . ? N4 C16 1.358(10) . ? N5 C31 1.130(11) . ? N6 C32 1.176(11) . ? N7 C33 1.383(10) . ? N7 C44 1.505(10) . ? N8 C37 1.335(10) . ? N8 C33 1.348(10) . ? N9 C48 1.422(11) . ? N9 C59 1.540(12) . ? N10 C48 1.320(10) . ? N10 C52 1.336(10) . ? N11 C63 1.121(10) . ? N12 C64 1.160(11) . ? C1 C2 1.399(11) . ? C2 C3 1.390(12) . ? C2 H2 0.9500 . ? C3 C4 1.383(11) . ? C3 H3 0.9500 . ? C4 C5 1.400(11) . ? C4 C6 1.475(12) . ? C5 H5 0.9500 . ? C6 C11 1.390(12) . ? C6 C7 1.405(12) . ? C7 C8 1.398(12) . ? C7 H7 0.9500 . ? C8 C9 1.361(13) . ? C8 H8 0.9500 . ? C9 C10 1.373(13) . ? C9 H9 0.9500 . ? C10 C11 1.391(12) . ? C10 H10 0.9500 . ? C11 H11 0.9500 . ? C12 C15 1.480(11) . ? C12 C14 1.516(12) . ? C12 C13 1.529(12) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.397(11) . ? C17 C18 1.331(12) . ? C17 H17 0.9500 . ? C18 C19 1.423(12) . ? C18 H18 0.9500 . ? C19 C20 1.405(12) . ? C19 C21 1.461(12) . ? C20 H20 0.9500 . ? C21 C26 1.385(13) . ? C21 C22 1.406(13) . ? C22 C23 1.397(13) . ? C22 H22 0.9500 . ? C23 C24 1.381(15) . ? C23 H23 0.9500 . ? C24 C25 1.388(15) . ? C24 H24 0.9500 . ? C25 C26 1.416(13) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C27 C28 1.486(14) . ? C27 C30 1.521(12) . ? C27 C29 1.538(13) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C33 C34 1.411(11) . ? C34 C35 1.369(11) . ? C34 H34 0.9500 . ? C35 C36 1.396(11) . ? C35 H35 0.9500 . ? C36 C37 1.399(11) . ? C36 C38 1.492(11) . ? C37 H37 0.9500 . ? C38 C39 1.390(11) . ? C38 C43 1.395(11) . ? C39 C40 1.393(12) . ? C39 H39 0.9500 . ? C40 C41 1.363(12) . ? C40 H40 0.9500 . ? C41 C42 1.396(13) . ? C41 H41 0.9500 . ? C42 C43 1.367(12) . ? C42 H42 0.9500 . ? C43 H43 0.9500 . ? C44 C45 1.471(14) . ? C44 C47 1.491(14) . ? C44 C46 1.514(15) . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 C49 1.418(12) . ? C49 C50 1.368(12) . ? C49 H49 0.9500 . ? C50 C51 1.371(12) . ? C50 H50 0.9500 . ? C51 C52 1.407(11) . ? C51 C53 1.460(12) . ? C52 H52 0.9500 . ? C53 C54 1.380(13) . ? C53 C58 1.410(13) . ? C54 C55 1.401(15) . ? C54 H54 0.9500 . ? C55 C56 1.363(17) . ? C55 H55 0.9500 . ? C56 C57 1.366(17) . ? C56 H56 0.9500 . ? C57 C58 1.380(14) . ? C57 H57 0.9500 . ? C58 H58 0.9500 . ? C59 C60 1.509(13) . ? C59 C61 1.522(12) . ? C59 C62 1.529(13) . ? C60 H60A 0.9800 . ? C60 H60B 0.9800 . ? C60 H60C 0.9800 . ? C61 H61A 0.9800 . ? C61 H61B 0.9800 . ? C61 H61C 0.9800 . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C62 H62C 0.9800 . ? 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 -33.7(8) . . . . ? Ni1 O1 N1 C12 135.3(5) . . . . ? Ni1 O2 N3 C16 35.8(8) . . . . ? Ni1 O2 N3 C27 -139.1(6) . . . . ? Ni2 O3 N7 C33 -38.2(8) . . . . ? Ni2 O3 N7 C44 136.8(6) . . . . ? Ni2 O4 N9 C48 38.2(7) . . . . ? Ni2 O4 N9 C59 -132.6(6) . . . . ? C5 N2 C1 C2 -0.4(12) . . . . ? Ni1 N2 C1 C2 176.7(6) . . . . ? C5 N2 C1 N1 -177.3(7) . . . . ? Ni1 N2 C1 N1 -0.1(9) . . . . ? O1 N1 C1 N2 22.6(10) . . . . ? C12 N1 C1 N2 -144.5(8) . . . . ? O1 N1 C1 C2 -154.2(8) . . . . ? C12 N1 C1 C2 38.7(13) . . . . ? N2 C1 C2 C3 -1.1(13) . . . . ? N1 C1 C2 C3 175.3(8) . . . . ? C1 C2 C3 C4 0.7(13) . . . . ? C2 C3 C4 C5 1.1(12) . . . . ? C2 C3 C4 C6 180.0(8) . . . . ? C1 N2 C5 C4 2.5(12) . . . . ? Ni1 N2 C5 C4 -174.3(6) . . . . ? C3 C4 C5 N2 -2.8(12) . . . . ? C6 C4 C5 N2 178.3(8) . . . . ? C3 C4 C6 C11 154.2(8) . . . . ? C5 C4 C6 C11 -27.0(12) . . . . ? C3 C4 C6 C7 -24.9(12) . . . . ? C5 C4 C6 C7 153.8(8) . . . . ? C11 C6 C7 C8 0.0(13) . . . . ? C4 C6 C7 C8 179.2(8) . . . . ? C6 C7 C8 C9 0.8(14) . . . . ? C7 C8 C9 C10 -2.0(15) . . . . ? C8 C9 C10 C11 2.3(15) . . . . ? C7 C6 C11 C10 0.3(13) . . . . ? C4 C6 C11 C10 -178.8(8) . . . . ? C9 C10 C11 C6 -1.5(14) . . . . ? O1 N1 C12 C15 166.3(7) . . . . ? C1 N1 C12 C15 -26.6(12) . . . . ? O1 N1 C12 C14 -70.9(9) . . . . ? C1 N1 C12 C14 96.2(10) . . . . ? O1 N1 C12 C13 45.7(9) . . . . ? C1 N1 C12 C13 -147.2(8) . . . . ? C20 N4 C16 C17 -0.8(12) . . . . ? Ni1 N4 C16 C17 -177.4(6) . . . . ? C20 N4 C16 N3 177.4(7) . . . . ? Ni1 N4 C16 N3 0.8(8) . . . . ? O2 N3 C16 N4 -24.6(10) . . . . ? C27 N3 C16 N4 149.7(8) . . . . ? O2 N3 C16 C17 153.6(8) . . . . ? C27 N3 C16 C17 -32.1(13) . . . . ? N4 C16 C17 C18 -1.2(13) . . . . ? N3 C16 C17 C18 -179.2(8) . . . . ? C16 C17 C18 C19 1.5(14) . . . . ? C17 C18 C19 C20 0.1(13) . . . . ? C17 C18 C19 C21 179.0(9) . . . . ? C16 N4 C20 C19 2.6(12) . . . . ? Ni1 N4 C20 C19 178.7(6) . . . . ? C18 C19 C20 N4 -2.3(13) . . . . ? C21 C19 C20 N4 178.9(8) . . . . ? C20 C19 C21 C26 -34.5(13) . . . . ? C18 C19 C21 C26 146.7(9) . . . . ? C20 C19 C21 C22 144.9(9) . . . . ? C18 C19 C21 C22 -33.9(13) . . . . ? C26 C21 C22 C23 0.0(14) . . . . ? C19 C21 C22 C23 -179.4(8) . . . . ? C21 C22 C23 C24 -1.0(15) . . . . ? C22 C23 C24 C25 1.1(16) . . . . ? C23 C24 C25 C26 -0.1(15) . . . . ? C22 C21 C26 C25 1.0(14) . . . . ? C19 C21 C26 C25 -179.6(8) . . . . ? C24 C25 C26 C21 -1.0(15) . . . . ? O2 N3 C27 C28 28.0(11) . . . . ? C16 N3 C27 C28 -146.1(9) . . . . ? O2 N3 C27 C30 147.2(8) . . . . ? C16 N3 C27 C30 -26.9(12) . . . . ? O2 N3 C27 C29 -90.5(10) . . . . ? C16 N3 C27 C29 95.4(11) . . . . ? C37 N8 C33 N7 -176.5(7) . . . . ? Ni2 N8 C33 N7 -0.9(9) . . . . ? C37 N8 C33 C34 3.5(12) . . . . ? Ni2 N8 C33 C34 179.1(6) . . . . ? O3 N7 C33 N8 26.4(10) . . . . ? C44 N7 C33 N8 -147.7(8) . . . . ? O3 N7 C33 C34 -153.6(8) . . . . ? C44 N7 C33 C34 32.3(14) . . . . ? N8 C33 C34 C35 -2.9(13) . . . . ? N7 C33 C34 C35 177.1(8) . . . . ? C33 C34 C35 C36 0.7(13) . . . . ? C34 C35 C36 C37 0.8(12) . . . . ? C34 C35 C36 C38 -177.7(8) . . . . ? C33 N8 C37 C36 -2.0(13) . . . . ? Ni2 N8 C37 C36 -176.9(6) . . . . ? C35 C36 C37 N8 -0.1(13) . . . . ? C38 C36 C37 N8 178.5(8) . . . . ? C35 C36 C38 C39 -34.3(13) . . . . ? C37 C36 C38 C39 147.3(9) . . . . ? C35 C36 C38 C43 145.7(9) . . . . ? C37 C36 C38 C43 -32.8(12) . . . . ? C43 C38 C39 C40 1.4(13) . . . . ? C36 C38 C39 C40 -178.7(8) . . . . ? C38 C39 C40 C41 -0.9(14) . . . . ? C39 C40 C41 C42 0.5(15) . . . . ? C40 C41 C42 C43 -0.5(16) . . . . ? C41 C42 C43 C38 1.0(15) . . . . ? C39 C38 C43 C42 -1.4(14) . . . . ? C36 C38 C43 C42 178.7(9) . . . . ? O3 N7 C44 C45 -16.5(12) . . . . ? C33 N7 C44 C45 157.5(10) . . . . ? O3 N7 C44 C47 -137.1(9) . . . . ? C33 N7 C44 C47 36.9(13) . . . . ? O3 N7 C44 C46 103.0(10) . . . . ? C33 N7 C44 C46 -83.0(12) . . . . ? C52 N10 C48 C49 1.7(12) . . . . ? Ni2 N10 C48 C49 175.5(6) . . . . ? C52 N10 C48 N9 178.9(7) . . . . ? Ni2 N10 C48 N9 -7.3(9) . . . . ? O4 N9 C48 N10 -21.1(10) . . . . ? C59 N9 C48 N10 149.1(8) . . . . ? O4 N9 C48 C49 156.1(8) . . . . ? C59 N9 C48 C49 -33.7(13) . . . . ? N10 C48 C49 C50 -3.4(13) . . . . ? N9 C48 C49 C50 179.6(8) . . . . ? C48 C49 C50 C51 1.8(13) . . . . ? C49 C50 C51 C52 1.3(13) . . . . ? C49 C50 C51 C53 -176.9(8) . . . . ? C48 N10 C52 C51 1.8(12) . . . . ? Ni2 N10 C52 C51 -171.2(6) . . . . ? C50 C51 C52 N10 -3.3(12) . . . . ? C53 C51 C52 N10 175.0(8) . . . . ? C50 C51 C53 C54 -38.3(13) . . . . ? C52 C51 C53 C54 143.5(9) . . . . ? C50 C51 C53 C58 143.9(9) . . . . ? C52 C51 C53 C58 -34.3(12) . . . . ? C58 C53 C54 C55 -0.8(14) . . . . ? C51 C53 C54 C55 -178.6(9) . . . . ? C53 C54 C55 C56 -1.3(16) . . . . ? C54 C55 C56 C57 0.6(18) . . . . ? C55 C56 C57 C58 2.2(18) . . . . ? C56 C57 C58 C53 -4.3(16) . . . . ? C54 C53 C58 C57 3.6(14) . . . . ? C51 C53 C58 C57 -178.5(9) . . . . ? O4 N9 C59 C60 10.1(10) . . . . ? C48 N9 C59 C60 -159.6(8) . . . . ? O4 N9 C59 C61 129.5(8) . . . . ? C48 N9 C59 C61 -40.2(11) . . . . ? O4 N9 C59 C62 -109.6(8) . . . . ? C48 N9 C59 C62 80.8(10) . . . . ?