#------------------------------------------------------------------------------ #$Date: 2025-02-12 01:08:47 +0200 (Wed, 12 Feb 2025) $ #$Revision: 297685 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/38/1573884.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_1573884 loop_ _publ_author_name 'Luff, Martin Simon' 'Filipovic, Tin M.' 'Corsei, Celine S.' 'Oppel, Kai' 'Krummenacher, Ivo' 'Bertermann, R\"udiger' 'Finze, Maik' 'Braunschweig, Holger' 'Radius, Udo' _publ_section_title ; Azolium-2-dithiocarboxylates as redox active ligands in nickel chemistry ; _journal_name_full 'Chemical Science' _journal_paper_doi 10.1039/D4SC08449G _journal_year 2025 _chemical_formula_moiety 'C40 H56 N6 Ni S2, C4 H10 O' _chemical_formula_sum 'C44 H66 N6 Ni O S2' _chemical_formula_weight 817.85 _space_group_crystal_system orthorhombic _space_group_IT_number 19 _space_group_name_Hall 'P 2ac 2ab' _space_group_name_H-M_alt 'P 21 21 21' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-2018/3 _audit_update_record ; 2024-12-12 deposited with the CCDC. 2025-02-10 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 12.6464(2) _cell_length_b 14.4357(2) _cell_length_c 24.9817(3) _cell_measurement_reflns_used 13055 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 76.2630 _cell_measurement_theta_min 3.5380 _cell_volume 4560.65(11) _computing_cell_refinement 'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)' _computing_data_reduction 'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)' _computing_molecular_graphics 'ShelXLe (Huebschle et all, 2011)' _computing_publication_material 'SHELXL-2014/6 (Sheldrick, 2014)' _computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _diffrn_ambient_temperature 100(2) _diffrn_detector_area_resol_mean 10.0000 _diffrn_measured_fraction_theta_full 0.991 _diffrn_measured_fraction_theta_max 0.963 _diffrn_measurement_device_type 'XtaLAB Synergy, Dualflex, HyPix' _diffrn_measurement_method '\w scans' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0389 _diffrn_reflns_av_unetI/netI 0.0404 _diffrn_reflns_Laue_measured_fraction_full 0.991 _diffrn_reflns_Laue_measured_fraction_max 0.963 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 23671 _diffrn_reflns_point_group_measured_fraction_full 0.914 _diffrn_reflns_point_group_measured_fraction_max 0.876 _diffrn_reflns_theta_full 72.000 _diffrn_reflns_theta_max 76.962 _diffrn_reflns_theta_min 3.536 _diffrn_source 'micro-focus sealed X-ray tube' _exptl_absorpt_coefficient_mu 1.753 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.380 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; CrysAlisPro 1.171.41.92a (Rigaku Oxford Diffraction, 2020) Numerical absorption correction based on gaussian integration over a multifaceted crystal model Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.191 _exptl_crystal_description block _exptl_crystal_F_000 1760 _exptl_crystal_size_max 0.310 _exptl_crystal_size_mid 0.160 _exptl_crystal_size_min 0.140 _refine_diff_density_max 0.456 _refine_diff_density_min -0.237 _refine_diff_density_rms 0.041 _refine_ls_abs_structure_details ; Flack x determined using 2916 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack -0.003(8) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 503 _refine_ls_number_reflns 8444 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.048 _refine_ls_R_factor_all 0.0351 _refine_ls_R_factor_gt 0.0304 _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^)+(0.0348P)^2^+0.7084P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0723 _refine_ls_wR_factor_ref 0.0742 _reflns_Friedel_coverage 0.642 _reflns_Friedel_fraction_full 0.819 _reflns_Friedel_fraction_max 0.768 _reflns_number_gt 7764 _reflns_number_total 8444 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4sc08449g2.cif _cod_data_source_block Compound_2c _cod_database_code 1573884 _shelx_shelxl_version_number 2018/3 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_min 0.612 _shelx_estimated_absorpt_t_max 0.791 _shelx_res_file ; TITL MaLu127_ref_a.res in P2(1)2(1)2(1) MaLu127_ref_a.res created by SHELXL-2018/3 at 14:57:56 on 31-Aug-2023 REM Old TITL MaLu127_ref in P2(1)2(1)2(1) REM SHELXT solution in P2(1)2(1)2(1) REM R1 0.075, Rweak 0.026, Alpha 0.005, Orientation as input REM Flack x = 0.006 ( 0.008 ) from Parsons' quotients REM Formula found by SHELXT: C44 N6 O S2 Ni CELL 1.54184 12.6464 14.4357 24.9817 90.000 90.000 90.000 ZERR 4.000 0.0002 0.0002 0.0003 0.000 0.000 0.000 LATT -1 SYMM 1/2-X, -Y, 1/2+Z SYMM -X, 1/2+Y, 1/2-Z SYMM 1/2+X, 1/2-Y, -Z SFAC C H N O S NI UNIT 176 264 24 4 8 4 TEMP -173 SIZE 0.14 0.16 0.31 L.S. 10 BOND $H LIST 4 ACTA 144 FMAP 2 PLAN 20 WGHT 0.034800 0.708400 FVAR 0.32651 NI01 6 0.627632 0.515698 0.246191 11.00000 0.01759 0.01896 = 0.01440 0.00057 -0.00025 -0.00123 S002 5 0.745426 0.616811 0.273132 11.00000 0.02051 0.02111 = 0.01733 0.00220 -0.00103 -0.00321 S003 5 0.643787 0.476983 0.330156 11.00000 0.02499 0.02765 = 0.01515 0.00317 -0.00178 -0.00845 O004 4 0.167429 0.490649 0.447883 11.00000 0.03538 0.03736 = 0.03224 0.00204 0.00459 -0.00399 N005 3 0.530853 0.347200 0.201391 11.00000 0.02381 0.02193 = 0.01779 -0.00205 0.00072 -0.00027 N006 3 0.553283 0.605010 0.147076 11.00000 0.02372 0.02488 = 0.01768 0.00294 -0.00285 0.00156 N007 3 0.427063 0.409606 0.258750 11.00000 0.01945 0.01968 = 0.02244 -0.00047 0.00004 -0.00177 N008 3 0.862409 0.664886 0.389792 11.00000 0.02320 0.02912 = 0.02245 -0.00191 -0.00254 -0.00602 N009 3 0.776368 0.551862 0.434017 11.00000 0.02255 0.03503 = 0.01674 0.00029 -0.00373 -0.00663 N00A 3 0.716417 0.564625 0.139859 11.00000 0.02113 0.03030 = 0.01594 0.00291 0.00196 0.00215 C00B 1 0.621599 0.328383 0.166411 11.00000 0.02931 0.02535 = 0.02167 -0.00105 0.00653 -0.00053 AFIX 13 H00B 2 0.678548 0.373873 0.175370 11.00000 -1.20000 AFIX 0 C00C 1 0.685537 0.409291 0.457774 11.00000 0.02801 0.02909 = 0.01745 0.00151 -0.00457 0.00154 C00D 1 0.523356 0.421670 0.234596 11.00000 0.02224 0.01724 = 0.01485 0.00004 -0.00159 0.00047 C00E 1 0.785808 0.593884 0.382949 11.00000 0.01882 0.02290 = 0.02036 0.00017 0.00163 0.00015 C00F 1 0.734748 0.569676 0.338255 11.00000 0.01770 0.02229 = 0.01939 -0.00156 0.00003 -0.00300 C00G 1 0.595237 0.364676 0.476309 11.00000 0.03520 0.02908 = 0.02303 0.00499 -0.00473 -0.00279 AFIX 43 H00G 2 0.596606 0.299380 0.480994 11.00000 -1.20000 AFIX 0 C00H 1 0.683073 0.505016 0.452230 11.00000 0.02151 0.02980 = 0.01303 0.00055 -0.00225 -0.00204 C00I 1 0.924423 0.702962 0.347471 11.00000 0.01812 0.02682 = 0.02354 -0.00114 -0.00526 -0.00475 C00J 1 0.688385 0.607966 0.092678 11.00000 0.03339 0.03784 = 0.01759 0.00644 0.00263 0.00037 AFIX 43 H00J 2 0.733015 0.618024 0.062647 11.00000 -1.20000 AFIX 0 C00K 1 0.442927 0.290563 0.204897 11.00000 0.03126 0.02205 = 0.02498 -0.00504 -0.00102 -0.00695 AFIX 43 H00K 2 0.430802 0.234879 0.185582 11.00000 -1.20000 AFIX 0 C00L 1 0.380837 0.469467 0.300123 11.00000 0.01864 0.02462 = 0.02881 -0.00483 0.00345 0.00018 AFIX 13 H00L 2 0.428411 0.524090 0.305228 11.00000 -1.20000 AFIX 0 C00M 1 0.591523 0.555833 0.463448 11.00000 0.02716 0.03117 = 0.01910 0.00172 -0.00180 0.00335 C00N 1 0.378372 0.329484 0.240762 11.00000 0.02289 0.02293 = 0.03095 -0.00112 -0.00150 -0.00604 AFIX 43 H00N 2 0.311495 0.306482 0.251866 11.00000 -1.20000 AFIX 0 C00O 1 0.587184 0.633167 0.096930 11.00000 0.03035 0.04002 = 0.01806 0.00811 -0.00262 0.00441 AFIX 43 H00O 2 0.546287 0.664399 0.070629 11.00000 -1.20000 AFIX 0 C00P 1 0.992163 0.645812 0.318304 11.00000 0.01920 0.02566 = 0.02878 0.00057 -0.00402 -0.00020 C00Q 1 0.632549 0.562193 0.174322 11.00000 0.02068 0.02032 = 0.01824 -0.00213 -0.00319 -0.00079 C00R 1 0.502937 0.507853 0.481534 11.00000 0.02294 0.04143 = 0.02176 0.00121 0.00055 0.00294 AFIX 43 H00R 2 0.440356 0.541491 0.489576 11.00000 -1.20000 AFIX 0 C00S 1 0.664651 0.231693 0.176444 11.00000 0.04416 0.03070 = 0.03574 0.00164 0.01228 0.00792 AFIX 137 H00A 2 0.613078 0.185646 0.164228 11.00000 -1.50000 H00C 2 0.677612 0.223422 0.214824 11.00000 -1.50000 H00D 2 0.731040 0.223634 0.156754 11.00000 -1.50000 AFIX 0 C00T 1 0.368330 0.558112 0.137864 11.00000 0.02848 0.03975 = 0.03739 -0.00051 -0.00499 -0.00598 AFIX 137 H00E 2 0.368304 0.575145 0.099890 11.00000 -1.50000 H00F 2 0.297167 0.566425 0.152630 11.00000 -1.50000 H00H 2 0.389633 0.493169 0.141642 11.00000 -1.50000 AFIX 0 C00U 1 0.445724 0.619544 0.168008 11.00000 0.02051 0.02802 = 0.02207 0.00174 -0.00067 0.00011 AFIX 13 H00U 2 0.445171 0.600126 0.206431 11.00000 -1.20000 AFIX 0 C00V 1 0.503253 0.412752 0.488149 11.00000 0.02810 0.04278 = 0.02203 0.00743 -0.00218 -0.00726 C00W 1 1.050656 0.684375 0.276821 11.00000 0.01933 0.03597 = 0.03461 0.00158 -0.00042 0.00052 AFIX 43 H00W 2 1.096507 0.645640 0.256662 11.00000 -1.20000 AFIX 0 C00X 1 0.415900 0.721147 0.165613 11.00000 0.03232 0.03110 = 0.03152 0.00198 0.00055 0.00455 AFIX 137 H00I 2 0.416981 0.742141 0.128311 11.00000 -1.50000 H00M 2 0.466654 0.757443 0.186562 11.00000 -1.50000 H00P 2 0.344782 0.729554 0.180417 11.00000 -1.50000 AFIX 0 C00Y 1 1.044175 0.777676 0.263929 11.00000 0.02137 0.04196 = 0.03832 0.01296 -0.00389 -0.00274 C00Z 1 0.915793 0.797335 0.335689 11.00000 0.02352 0.02650 = 0.03507 0.00072 -0.00720 -0.00270 C010 1 0.843589 0.598650 0.469695 11.00000 0.03140 0.05051 = 0.01716 -0.00270 -0.00682 -0.00814 AFIX 43 H010 2 0.850393 0.585819 0.506833 11.00000 -1.20000 AFIX 0 C011 1 1.000898 0.544390 0.331653 11.00000 0.02964 0.02638 = 0.04368 0.00334 0.00547 0.00310 AFIX 137 H01A 2 0.932182 0.514441 0.326237 11.00000 -1.50000 H01B 2 1.022532 0.537308 0.369099 11.00000 -1.50000 H01C 2 1.053666 0.515406 0.308312 11.00000 -1.50000 AFIX 0 C012 1 0.372978 0.417819 0.353151 11.00000 0.03293 0.03671 = 0.02722 -0.00417 0.00666 -0.00274 AFIX 137 H01D 2 0.330978 0.361403 0.348246 11.00000 -1.50000 H01E 2 0.338846 0.457604 0.379831 11.00000 -1.50000 H01F 2 0.444057 0.401225 0.365491 11.00000 -1.50000 AFIX 0 C013 1 0.782024 0.354802 0.442100 11.00000 0.03753 0.03771 = 0.03607 -0.00133 -0.00388 0.00912 AFIX 137 H01G 2 0.796289 0.363841 0.403897 11.00000 -1.50000 H01H 2 0.769818 0.288882 0.449151 11.00000 -1.50000 H01I 2 0.842850 0.376169 0.463035 11.00000 -1.50000 AFIX 0 C014 1 0.896029 0.663636 0.443157 11.00000 0.03108 0.03898 = 0.02424 -0.00635 -0.00463 -0.01147 AFIX 43 H014 2 0.948321 0.703211 0.458071 11.00000 -1.20000 AFIX 0 C015 1 0.842019 0.858482 0.367092 11.00000 0.03698 0.02717 = 0.05614 -0.00376 -0.00177 0.00289 AFIX 137 H01J 2 0.835844 0.918732 0.349288 11.00000 -1.50000 H01K 2 0.869999 0.867249 0.403322 11.00000 -1.50000 H01L 2 0.772176 0.829281 0.369116 11.00000 -1.50000 AFIX 0 C016 1 0.823380 0.528116 0.150907 11.00000 0.02221 0.04271 = 0.02185 0.00270 0.00200 0.00438 AFIX 13 H016 2 0.822188 0.497211 0.186727 11.00000 -1.20000 AFIX 0 C017 1 0.590239 0.343335 0.108279 11.00000 0.04916 0.03153 = 0.02270 -0.00051 0.00451 -0.00359 AFIX 137 H01M 2 0.649596 0.326738 0.084954 11.00000 -1.50000 H01N 2 0.571787 0.408569 0.102738 11.00000 -1.50000 H01O 2 0.529127 0.304332 0.099683 11.00000 -1.50000 AFIX 0 C018 1 0.177709 0.562663 0.486272 11.00000 0.03953 0.04336 = 0.04026 -0.00455 0.00703 0.00022 AFIX 23 H01P 2 0.221305 0.541411 0.516811 11.00000 -1.20000 H01Q 2 0.107230 0.580774 0.499983 11.00000 -1.20000 AFIX 0 C019 1 0.853925 0.456160 0.109169 11.00000 0.03092 0.05276 = 0.02802 0.00174 0.00731 0.00744 AFIX 137 H01R 2 0.856984 0.485433 0.073809 11.00000 -1.50000 H01S 2 0.801107 0.406489 0.108774 11.00000 -1.50000 H01T 2 0.923356 0.430215 0.118043 11.00000 -1.50000 AFIX 0 C01A 1 0.902638 0.606866 0.153074 11.00000 0.02514 0.05579 = 0.03367 0.00097 0.00369 -0.00649 AFIX 137 H01U 2 0.906815 0.636725 0.117907 11.00000 -1.50000 H01V 2 0.972308 0.582433 0.162854 11.00000 -1.50000 H01W 2 0.880007 0.652328 0.179860 11.00000 -1.50000 AFIX 0 C01B 1 0.273225 0.504509 0.281658 11.00000 0.02190 0.03168 = 0.04553 -0.00581 0.00368 0.00196 AFIX 137 H01X 2 0.281199 0.537962 0.247762 11.00000 -1.50000 H01Y 2 0.243866 0.546267 0.308783 11.00000 -1.50000 H01Z 2 0.225383 0.451841 0.276551 11.00000 -1.50000 AFIX 0 C01C 1 0.976787 0.832868 0.294032 11.00000 0.03118 0.02366 = 0.04526 0.00921 -0.00742 -0.00376 AFIX 43 H011 2 0.972096 0.897045 0.285957 11.00000 -1.20000 AFIX 0 C01D 1 0.588923 0.658586 0.455194 11.00000 0.03967 0.03129 = 0.04721 0.00051 -0.00003 0.00632 AFIX 137 H012 2 0.597254 0.672417 0.417021 11.00000 -1.50000 H013 2 0.646692 0.687409 0.475350 11.00000 -1.50000 H015 2 0.521120 0.683157 0.467812 11.00000 -1.50000 AFIX 0 C01E 1 0.102464 0.417067 0.465535 11.00000 0.03433 0.04100 = 0.04406 0.00714 0.00533 -0.00293 AFIX 23 H017 2 0.030132 0.440135 0.472748 11.00000 -1.20000 H018 2 0.131167 0.390593 0.499081 11.00000 -1.20000 AFIX 0 C01F 1 0.099301 0.343920 0.422692 11.00000 0.05034 0.03678 = 0.04695 0.00832 -0.00666 -0.00763 AFIX 137 H019 2 0.073625 0.371254 0.389219 11.00000 -1.50000 H020 2 0.051676 0.293894 0.433738 11.00000 -1.50000 H021 2 0.170541 0.318949 0.417205 11.00000 -1.50000 AFIX 0 C01G 1 1.108078 0.816786 0.218236 11.00000 0.03767 0.05949 = 0.05733 0.02756 0.00740 -0.00054 AFIX 137 H022 2 1.060348 0.836879 0.189595 11.00000 -1.50000 H023 2 1.156011 0.769041 0.204492 11.00000 -1.50000 H024 2 1.149395 0.869851 0.230932 11.00000 -1.50000 AFIX 0 C01H 1 0.229687 0.643603 0.459196 11.00000 0.04432 0.03449 = 0.05531 -0.00045 0.00870 0.00011 AFIX 137 H025 2 0.294627 0.622898 0.441448 11.00000 -1.50000 H026 2 0.247023 0.690917 0.485923 11.00000 -1.50000 H027 2 0.181332 0.669817 0.432546 11.00000 -1.50000 AFIX 0 C01I 1 0.404974 0.362637 0.507098 11.00000 0.03576 0.06241 = 0.04605 0.01504 0.00158 -0.01414 AFIX 137 H028 2 0.343596 0.384703 0.486828 11.00000 -1.50000 H029 2 0.394106 0.374884 0.545289 11.00000 -1.50000 H02A 2 0.413606 0.295886 0.501444 11.00000 -1.50000 AFIX 0 HKLF 4 REM MaLu127_ref_a.res in P2(1)2(1)2(1) REM wR2 = 0.074225, GooF = S = 1.04818, Restrained GooF = 1.04818 for all data REM R1 = 0.030426 for 7764 Fo > 4sig(Fo) and 0.035051 for all 8444 data REM 503 parameters refined using 0 restraints END WGHT 0.0348 0.7082 REM Highest difference peak 0.456, deepest hole -0.237, 1-sigma level 0.041 Q1 1 0.6332 0.5027 0.2887 11.00000 0.05 0.46 Q2 1 0.6309 0.5210 0.2076 11.00000 0.05 0.43 Q3 1 0.7404 0.6072 0.3096 11.00000 0.05 0.30 Q4 1 0.6425 0.4742 0.3683 11.00000 0.05 0.27 Q5 1 0.7480 0.6141 0.2332 11.00000 0.05 0.22 Q6 1 0.6683 0.4644 0.2116 11.00000 0.05 0.20 Q7 1 0.5748 0.4613 0.2190 11.00000 0.05 0.18 Q8 1 0.6200 0.4428 0.2482 11.00000 0.05 0.18 Q9 1 1.0013 0.6611 0.2898 11.00000 0.05 0.18 Q10 1 0.6859 0.5410 0.3402 11.00000 0.05 0.18 Q11 1 0.3808 0.4462 0.3242 11.00000 0.05 0.17 Q12 1 0.6138 0.3357 0.1348 11.00000 0.05 0.17 Q13 1 1.1206 0.9250 0.2488 11.00000 0.05 0.17 Q14 1 0.6856 0.5546 0.2857 11.00000 0.05 0.17 Q15 1 0.6393 0.4075 0.1910 11.00000 0.05 0.16 Q16 1 0.7960 0.5613 0.2427 11.00000 0.05 0.16 Q17 1 0.7436 0.5175 0.4419 11.00000 0.05 0.16 Q18 1 0.5795 0.4652 0.2826 11.00000 0.05 0.16 Q19 1 0.6394 0.3748 0.2735 11.00000 0.05 0.15 Q20 1 0.7808 0.5560 0.4105 11.00000 0.05 0.15 ; _shelx_res_checksum 57714 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' '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 Ni01 Ni 0.62763(3) 0.51570(3) 0.24619(2) 0.01698(10) Uani 1 1 d . . . . . S002 S 0.74543(5) 0.61681(4) 0.27313(2) 0.01965(13) Uani 1 1 d . . . . . S003 S 0.64379(5) 0.47698(5) 0.33016(2) 0.02260(14) Uani 1 1 d . . . . . O004 O 0.16743(16) 0.49065(16) 0.44788(8) 0.0350(5) Uani 1 1 d . . . . . N005 N 0.53085(18) 0.34720(16) 0.20139(8) 0.0212(5) Uani 1 1 d . . . . . N006 N 0.55328(18) 0.60501(16) 0.14708(8) 0.0221(5) Uani 1 1 d . . . . . N007 N 0.42706(16) 0.40961(14) 0.25875(8) 0.0205(4) Uani 1 1 d . . . . . N008 N 0.86241(19) 0.66489(17) 0.38979(9) 0.0249(5) Uani 1 1 d . . . . . N009 N 0.77637(18) 0.55186(17) 0.43402(8) 0.0248(5) Uani 1 1 d . . . . . N00A N 0.71642(17) 0.56462(17) 0.13986(9) 0.0225(5) Uani 1 1 d . . . . . C00B C 0.6216(2) 0.32838(19) 0.16641(10) 0.0254(6) Uani 1 1 d . . . . . H00B H 0.678548 0.373873 0.175370 0.031 Uiso 1 1 calc R U . . . C00C C 0.6855(2) 0.4093(2) 0.45777(11) 0.0248(6) Uani 1 1 d . . . . . C00D C 0.5234(2) 0.42167(17) 0.23460(10) 0.0181(5) Uani 1 1 d . . . . . C00E C 0.7858(2) 0.59388(19) 0.38295(10) 0.0207(5) Uani 1 1 d . . . . . C00F C 0.7347(2) 0.56968(18) 0.33825(10) 0.0198(5) Uani 1 1 d . . . . . C00G C 0.5952(2) 0.3647(2) 0.47631(11) 0.0291(6) Uani 1 1 d . . . . . H00G H 0.596606 0.299380 0.480994 0.035 Uiso 1 1 calc R U . . . C00H C 0.6831(2) 0.5050(2) 0.45223(10) 0.0214(5) Uani 1 1 d . . . . . C00I C 0.9244(2) 0.7030(2) 0.34747(11) 0.0228(6) Uani 1 1 d . . . . . C00J C 0.6884(2) 0.6080(2) 0.09268(11) 0.0296(6) Uani 1 1 d . . . . . H00J H 0.733015 0.618024 0.062647 0.036 Uiso 1 1 calc R U . . . C00K C 0.4429(2) 0.2906(2) 0.20490(11) 0.0261(6) Uani 1 1 d . . . . . H00K H 0.430802 0.234879 0.185582 0.031 Uiso 1 1 calc R U . . . C00L C 0.3808(2) 0.46947(19) 0.30012(11) 0.0240(5) Uani 1 1 d . . . . . H00L H 0.428411 0.524090 0.305228 0.029 Uiso 1 1 calc R U . . . C00M C 0.5915(2) 0.5558(2) 0.46345(11) 0.0258(6) Uani 1 1 d . . . . . C00N C 0.3784(2) 0.32948(19) 0.24076(11) 0.0256(6) Uani 1 1 d . . . . . H00N H 0.311495 0.306482 0.251866 0.031 Uiso 1 1 calc R U . . . C00O C 0.5872(2) 0.6332(2) 0.09693(11) 0.0295(6) Uani 1 1 d . . . . . H00O H 0.546287 0.664399 0.070629 0.035 Uiso 1 1 calc R U . . . C00P C 0.9922(2) 0.64581(19) 0.31830(11) 0.0245(6) Uani 1 1 d . . . . . C00Q C 0.6325(2) 0.56219(17) 0.17432(10) 0.0197(5) Uani 1 1 d . . . . . C00R C 0.5029(2) 0.5079(2) 0.48153(10) 0.0287(6) Uani 1 1 d . . . . . H00R H 0.440356 0.541491 0.489576 0.034 Uiso 1 1 calc R U . . . C00S C 0.6647(3) 0.2317(2) 0.17644(13) 0.0369(7) Uani 1 1 d . . . . . H00A H 0.613078 0.185646 0.164228 0.055 Uiso 1 1 calc R U . . . H00C H 0.677612 0.223422 0.214824 0.055 Uiso 1 1 calc R U . . . H00D H 0.731040 0.223634 0.156754 0.055 Uiso 1 1 calc R U . . . C00T C 0.3683(3) 0.5581(2) 0.13786(12) 0.0352(7) Uani 1 1 d . . . . . H00E H 0.368304 0.575145 0.099890 0.053 Uiso 1 1 calc R U . . . H00F H 0.297167 0.566425 0.152630 0.053 Uiso 1 1 calc R U . . . H00H H 0.389633 0.493169 0.141642 0.053 Uiso 1 1 calc R U . . . C00U C 0.4457(2) 0.6195(2) 0.16801(11) 0.0235(5) Uani 1 1 d . . . . . H00U H 0.445171 0.600126 0.206431 0.028 Uiso 1 1 calc R U . . . C00V C 0.5033(2) 0.4128(2) 0.48815(11) 0.0310(7) Uani 1 1 d . . . . . C00W C 1.0507(2) 0.6844(2) 0.27682(12) 0.0300(6) Uani 1 1 d . . . . . H00W H 1.096507 0.645640 0.256662 0.036 Uiso 1 1 calc R U . . . C00X C 0.4159(2) 0.7211(2) 0.16561(12) 0.0316(7) Uani 1 1 d . . . . . H00I H 0.416981 0.742141 0.128311 0.047 Uiso 1 1 calc R U . . . H00M H 0.466654 0.757443 0.186562 0.047 Uiso 1 1 calc R U . . . H00P H 0.344782 0.729554 0.180417 0.047 Uiso 1 1 calc R U . . . C00Y C 1.0442(2) 0.7777(2) 0.26393(12) 0.0339(7) Uani 1 1 d . . . . . C00Z C 0.9158(2) 0.7973(2) 0.33569(12) 0.0284(6) Uani 1 1 d . . . . . C010 C 0.8436(2) 0.5986(2) 0.46969(11) 0.0330(7) Uani 1 1 d . . . . . H010 H 0.850393 0.585819 0.506833 0.040 Uiso 1 1 calc R U . . . C011 C 1.0009(2) 0.5444(2) 0.33165(14) 0.0332(7) Uani 1 1 d . . . . . H01A H 0.932182 0.514441 0.326237 0.050 Uiso 1 1 calc R U . . . H01B H 1.022532 0.537308 0.369099 0.050 Uiso 1 1 calc R U . . . H01C H 1.053666 0.515406 0.308312 0.050 Uiso 1 1 calc R U . . . C012 C 0.3730(3) 0.4178(2) 0.35315(11) 0.0323(6) Uani 1 1 d . . . . . H01D H 0.330978 0.361403 0.348246 0.048 Uiso 1 1 calc R U . . . H01E H 0.338846 0.457604 0.379831 0.048 Uiso 1 1 calc R U . . . H01F H 0.444057 0.401225 0.365491 0.048 Uiso 1 1 calc R U . . . C013 C 0.7820(3) 0.3548(2) 0.44210(13) 0.0371(7) Uani 1 1 d . . . . . H01G H 0.796289 0.363841 0.403897 0.056 Uiso 1 1 calc R U . . . H01H H 0.769818 0.288882 0.449151 0.056 Uiso 1 1 calc R U . . . H01I H 0.842850 0.376169 0.463035 0.056 Uiso 1 1 calc R U . . . C014 C 0.8960(2) 0.6636(2) 0.44316(11) 0.0314(7) Uani 1 1 d . . . . . H014 H 0.948321 0.703211 0.458071 0.038 Uiso 1 1 calc R U . . . C015 C 0.8420(3) 0.8585(2) 0.36709(15) 0.0401(8) Uani 1 1 d . . . . . H01J H 0.835844 0.918732 0.349288 0.060 Uiso 1 1 calc R U . . . H01K H 0.869999 0.867249 0.403322 0.060 Uiso 1 1 calc R U . . . H01L H 0.772176 0.829281 0.369116 0.060 Uiso 1 1 calc R U . . . C016 C 0.8234(2) 0.5281(2) 0.15091(11) 0.0289(6) Uani 1 1 d . . . . . H016 H 0.822188 0.497211 0.186727 0.035 Uiso 1 1 calc R U . . . C017 C 0.5902(3) 0.3433(2) 0.10828(11) 0.0345(7) Uani 1 1 d . . . . . H01M H 0.649596 0.326738 0.084954 0.052 Uiso 1 1 calc R U . . . H01N H 0.571787 0.408569 0.102738 0.052 Uiso 1 1 calc R U . . . H01O H 0.529127 0.304332 0.099683 0.052 Uiso 1 1 calc R U . . . C018 C 0.1777(3) 0.5627(3) 0.48627(14) 0.0410(8) Uani 1 1 d . . . . . H01P H 0.221305 0.541411 0.516811 0.049 Uiso 1 1 calc R U . . . H01Q H 0.107230 0.580774 0.499983 0.049 Uiso 1 1 calc R U . . . C019 C 0.8539(3) 0.4562(2) 0.10917(12) 0.0372(7) Uani 1 1 d . . . . . H01R H 0.856984 0.485433 0.073809 0.056 Uiso 1 1 calc R U . . . H01S H 0.801107 0.406489 0.108774 0.056 Uiso 1 1 calc R U . . . H01T H 0.923356 0.430215 0.118043 0.056 Uiso 1 1 calc R U . . . C01A C 0.9026(2) 0.6069(3) 0.15307(13) 0.0382(8) Uani 1 1 d . . . . . H01U H 0.906815 0.636725 0.117907 0.057 Uiso 1 1 calc R U . . . H01V H 0.972308 0.582433 0.162854 0.057 Uiso 1 1 calc R U . . . H01W H 0.880007 0.652328 0.179860 0.057 Uiso 1 1 calc R U . . . C01B C 0.2732(2) 0.5045(2) 0.28166(13) 0.0330(7) Uani 1 1 d . . . . . H01X H 0.281199 0.537962 0.247762 0.050 Uiso 1 1 calc R U . . . H01Y H 0.243866 0.546267 0.308783 0.050 Uiso 1 1 calc R U . . . H01Z H 0.225383 0.451841 0.276551 0.050 Uiso 1 1 calc R U . . . C01C C 0.9768(2) 0.8329(2) 0.29403(13) 0.0334(7) Uani 1 1 d . . . . . H011 H 0.972096 0.897045 0.285957 0.040 Uiso 1 1 calc R U . . . C01D C 0.5889(3) 0.6586(2) 0.45519(15) 0.0394(8) Uani 1 1 d . . . . . H012 H 0.597254 0.672417 0.417021 0.059 Uiso 1 1 calc R U . . . H013 H 0.646692 0.687409 0.475350 0.059 Uiso 1 1 calc R U . . . H015 H 0.521120 0.683157 0.467812 0.059 Uiso 1 1 calc R U . . . C01E C 0.1025(3) 0.4171(2) 0.46554(14) 0.0398(8) Uani 1 1 d . . . . . H017 H 0.030132 0.440135 0.472748 0.048 Uiso 1 1 calc R U . . . H018 H 0.131167 0.390593 0.499081 0.048 Uiso 1 1 calc R U . . . C01F C 0.0993(3) 0.3439(2) 0.42269(14) 0.0447(8) Uani 1 1 d . . . . . H019 H 0.073625 0.371254 0.389219 0.067 Uiso 1 1 calc R U . . . H020 H 0.051676 0.293894 0.433738 0.067 Uiso 1 1 calc R U . . . H021 H 0.170541 0.318949 0.417205 0.067 Uiso 1 1 calc R U . . . C01G C 1.1081(3) 0.8168(3) 0.21824(16) 0.0515(10) Uani 1 1 d . . . . . H022 H 1.060348 0.836879 0.189595 0.077 Uiso 1 1 calc R U . . . H023 H 1.156011 0.769041 0.204492 0.077 Uiso 1 1 calc R U . . . H024 H 1.149395 0.869851 0.230932 0.077 Uiso 1 1 calc R U . . . C01H C 0.2297(3) 0.6436(2) 0.45920(15) 0.0447(8) Uani 1 1 d . . . . . H025 H 0.294627 0.622898 0.441448 0.067 Uiso 1 1 calc R U . . . H026 H 0.247023 0.690917 0.485923 0.067 Uiso 1 1 calc R U . . . H027 H 0.181332 0.669817 0.432546 0.067 Uiso 1 1 calc R U . . . C01I C 0.4050(3) 0.3626(3) 0.50710(15) 0.0481(9) Uani 1 1 d . . . . . H028 H 0.343596 0.384703 0.486828 0.072 Uiso 1 1 calc R U . . . H029 H 0.394106 0.374884 0.545289 0.072 Uiso 1 1 calc R U . . . H02A H 0.413606 0.295886 0.501444 0.072 Uiso 1 1 calc R U . . . 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 Ni01 0.01759(19) 0.0190(2) 0.01440(19) 0.00057(17) -0.00025(16) -0.00123(17) S002 0.0205(3) 0.0211(3) 0.0173(3) 0.0022(2) -0.0010(2) -0.0032(3) S003 0.0250(3) 0.0276(3) 0.0152(3) 0.0032(3) -0.0018(2) -0.0084(3) O004 0.0354(11) 0.0374(12) 0.0322(10) 0.0020(10) 0.0046(9) -0.0040(9) N005 0.0238(11) 0.0219(11) 0.0178(10) -0.0021(9) 0.0007(9) -0.0003(9) N006 0.0237(11) 0.0249(12) 0.0177(10) 0.0029(9) -0.0028(9) 0.0016(9) N007 0.0195(10) 0.0197(10) 0.0224(11) -0.0005(9) 0.0000(9) -0.0018(8) N008 0.0232(11) 0.0291(12) 0.0225(11) -0.0019(9) -0.0025(10) -0.0060(10) N009 0.0226(11) 0.0350(13) 0.0167(10) 0.0003(10) -0.0037(9) -0.0066(10) N00A 0.0211(11) 0.0303(12) 0.0159(10) 0.0029(10) 0.0020(9) 0.0021(9) C00B 0.0293(14) 0.0254(13) 0.0217(13) -0.0011(11) 0.0065(12) -0.0005(12) C00C 0.0280(14) 0.0291(15) 0.0174(13) 0.0015(11) -0.0046(11) 0.0015(12) C00D 0.0222(12) 0.0172(11) 0.0148(12) 0.0000(10) -0.0016(10) 0.0005(10) C00E 0.0188(12) 0.0229(13) 0.0204(12) 0.0002(11) 0.0016(10) 0.0002(10) C00F 0.0177(12) 0.0223(13) 0.0194(12) -0.0016(10) 0.0000(10) -0.0030(10) C00G 0.0352(16) 0.0291(15) 0.0230(13) 0.0050(12) -0.0047(12) -0.0028(13) C00H 0.0215(12) 0.0298(15) 0.0130(11) 0.0006(11) -0.0022(9) -0.0020(11) C00I 0.0181(12) 0.0268(13) 0.0235(13) -0.0011(11) -0.0053(10) -0.0047(11) C00J 0.0334(15) 0.0378(17) 0.0176(13) 0.0064(13) 0.0026(11) 0.0004(13) C00K 0.0313(15) 0.0220(13) 0.0250(13) -0.0050(11) -0.0010(12) -0.0069(12) C00L 0.0186(12) 0.0246(14) 0.0288(13) -0.0048(11) 0.0034(11) 0.0002(11) C00M 0.0272(14) 0.0312(15) 0.0191(13) 0.0017(12) -0.0018(11) 0.0034(12) C00N 0.0229(13) 0.0229(12) 0.0310(15) -0.0011(11) -0.0015(12) -0.0060(11) C00O 0.0303(15) 0.0400(17) 0.0181(13) 0.0081(13) -0.0026(11) 0.0044(13) C00P 0.0192(12) 0.0257(14) 0.0288(14) 0.0006(12) -0.0040(11) -0.0002(11) C00Q 0.0207(12) 0.0203(12) 0.0182(11) -0.0021(10) -0.0032(11) -0.0008(10) C00R 0.0229(13) 0.0414(17) 0.0218(13) 0.0012(13) 0.0005(10) 0.0029(13) C00S 0.0442(18) 0.0307(16) 0.0357(16) 0.0016(14) 0.0123(14) 0.0079(14) C00T 0.0285(15) 0.0397(17) 0.0374(16) -0.0005(14) -0.0050(14) -0.0060(14) C00U 0.0205(12) 0.0280(14) 0.0221(12) 0.0017(12) -0.0007(11) 0.0001(11) C00V 0.0281(15) 0.0428(17) 0.0220(14) 0.0074(13) -0.0022(12) -0.0073(14) C00W 0.0193(13) 0.0360(16) 0.0346(15) 0.0016(14) -0.0004(12) 0.0005(12) C00X 0.0323(15) 0.0311(16) 0.0315(15) 0.0020(13) 0.0005(13) 0.0045(13) C00Y 0.0214(13) 0.0420(18) 0.0383(17) 0.0130(15) -0.0039(13) -0.0027(12) C00Z 0.0235(13) 0.0265(14) 0.0351(15) 0.0007(13) -0.0072(12) -0.0027(12) C010 0.0314(16) 0.051(2) 0.0172(13) -0.0027(13) -0.0068(11) -0.0081(14) C011 0.0296(15) 0.0264(15) 0.0437(17) 0.0033(14) 0.0055(14) 0.0031(12) C012 0.0329(15) 0.0367(16) 0.0272(14) -0.0042(13) 0.0067(13) -0.0027(14) C013 0.0375(17) 0.0377(18) 0.0361(17) -0.0013(14) -0.0039(14) 0.0091(14) C014 0.0311(15) 0.0390(17) 0.0242(14) -0.0063(13) -0.0046(12) -0.0115(13) C015 0.0370(18) 0.0272(15) 0.056(2) -0.0038(15) -0.0018(15) 0.0029(13) C016 0.0222(13) 0.0427(18) 0.0218(13) 0.0027(13) 0.0020(11) 0.0044(13) C017 0.0492(19) 0.0315(16) 0.0227(14) -0.0005(13) 0.0045(13) -0.0036(14) C018 0.0395(18) 0.0434(19) 0.0403(18) -0.0046(16) 0.0070(15) 0.0002(15) C019 0.0309(16) 0.053(2) 0.0280(15) 0.0017(14) 0.0073(13) 0.0074(15) C01A 0.0251(14) 0.056(2) 0.0337(16) 0.0010(16) 0.0037(12) -0.0065(15) C01B 0.0219(13) 0.0317(16) 0.0455(17) -0.0058(14) 0.0037(12) 0.0020(12) C01C 0.0312(15) 0.0237(15) 0.0453(18) 0.0092(13) -0.0074(14) -0.0038(13) C01D 0.0397(17) 0.0313(16) 0.0472(19) 0.0005(15) 0.0000(15) 0.0063(14) C01E 0.0343(17) 0.0410(18) 0.0441(18) 0.0071(15) 0.0053(14) -0.0029(15) C01F 0.050(2) 0.0368(18) 0.0469(19) 0.0083(16) -0.0067(16) -0.0076(16) C01G 0.0377(19) 0.059(2) 0.057(2) 0.0276(19) 0.0074(17) -0.0005(17) C01H 0.0443(19) 0.0345(18) 0.055(2) -0.0004(16) 0.0087(17) 0.0001(15) C01I 0.0358(18) 0.062(2) 0.0460(19) 0.0150(18) 0.0016(15) -0.0141(17) 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' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 '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' 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 C00D Ni01 C00Q 97.40(11) . . ? C00D Ni01 S003 91.63(8) . . ? C00Q Ni01 S003 170.87(8) . . ? C00D Ni01 S002 170.72(8) . . ? C00Q Ni01 S002 91.85(8) . . ? S003 Ni01 S002 79.14(3) . . ? C00F S002 Ni01 88.53(9) . . ? C00F S003 Ni01 88.69(9) . . ? C01E O004 C018 113.1(2) . . ? C00D N005 C00K 111.9(2) . . ? C00D N005 C00B 124.3(2) . . ? C00K N005 C00B 123.8(2) . . ? C00Q N006 C00O 111.0(2) . . ? C00Q N006 C00U 124.6(2) . . ? C00O N006 C00U 124.4(2) . . ? C00D N007 C00N 111.0(2) . . ? C00D N007 C00L 126.1(2) . . ? C00N N007 C00L 122.9(2) . . ? C014 N008 C00E 108.2(2) . . ? C014 N008 C00I 123.0(2) . . ? C00E N008 C00I 124.3(2) . . ? C010 N009 C00E 108.3(2) . . ? C010 N009 C00H 121.6(2) . . ? C00E N009 C00H 123.8(2) . . ? C00Q N00A C00J 110.5(2) . . ? C00Q N00A C016 125.7(2) . . ? C00J N00A C016 123.8(2) . . ? N005 C00B C00S 110.6(2) . . ? N005 C00B C017 109.8(2) . . ? C00S C00B C017 112.4(3) . . ? N005 C00B H00B 108.0 . . ? C00S C00B H00B 108.0 . . ? C017 C00B H00B 108.0 . . ? C00H C00C C00G 118.4(3) . . ? C00H C00C C013 120.8(3) . . ? C00G C00C C013 120.7(3) . . ? N005 C00D N007 103.3(2) . . ? N005 C00D Ni01 127.17(19) . . ? N007 C00D Ni01 129.47(18) . . ? C00F C00E N009 126.8(2) . . ? C00F C00E N008 128.2(2) . . ? N009 C00E N008 104.9(2) . . ? C00E C00F S002 129.1(2) . . ? C00E C00F S003 127.2(2) . . ? S002 C00F S003 103.56(13) . . ? C00V C00G C00C 121.9(3) . . ? C00V C00G H00G 119.1 . . ? C00C C00G H00G 119.1 . . ? C00C C00H C00M 121.3(3) . . ? C00C C00H N009 118.8(2) . . ? C00M C00H N009 119.8(2) . . ? C00P C00I C00Z 121.0(3) . . ? C00P C00I N008 119.8(3) . . ? C00Z C00I N008 119.2(3) . . ? C00O C00J N00A 107.6(3) . . ? C00O C00J H00J 126.2 . . ? N00A C00J H00J 126.2 . . ? C00N C00K N005 106.6(2) . . ? C00N C00K H00K 126.7 . . ? N005 C00K H00K 126.7 . . ? N007 C00L C012 110.5(2) . . ? N007 C00L C01B 109.7(2) . . ? C012 C00L C01B 111.6(2) . . ? N007 C00L H00L 108.3 . . ? C012 C00L H00L 108.3 . . ? C01B C00L H00L 108.3 . . ? C00R C00M C00H 118.0(3) . . ? C00R C00M C01D 121.3(3) . . ? C00H C00M C01D 120.7(3) . . ? C00K C00N N007 107.3(2) . . ? C00K C00N H00N 126.4 . . ? N007 C00N H00N 126.4 . . ? C00J C00O N006 106.8(3) . . ? C00J C00O H00O 126.6 . . ? N006 C00O H00O 126.6 . . ? C00W C00P C00I 118.7(3) . . ? C00W C00P C011 121.0(3) . . ? C00I C00P C011 120.3(3) . . ? N006 C00Q N00A 104.2(2) . . ? N006 C00Q Ni01 127.13(19) . . ? N00A C00Q Ni01 128.61(19) . . ? C00V C00R C00M 122.0(3) . . ? C00V C00R H00R 119.0 . . ? C00M C00R H00R 119.0 . . ? C00B C00S H00A 109.5 . . ? C00B C00S H00C 109.5 . . ? H00A C00S H00C 109.5 . . ? C00B C00S H00D 109.5 . . ? H00A C00S H00D 109.5 . . ? H00C C00S H00D 109.5 . . ? C00U C00T H00E 109.5 . . ? C00U C00T H00F 109.5 . . ? H00E C00T H00F 109.5 . . ? C00U C00T H00H 109.5 . . ? H00E C00T H00H 109.5 . . ? H00F C00T H00H 109.5 . . ? N006 C00U C00X 110.7(2) . . ? N006 C00U C00T 109.6(2) . . ? C00X C00U C00T 112.6(2) . . ? N006 C00U H00U 107.9 . . ? C00X C00U H00U 107.9 . . ? C00T C00U H00U 107.9 . . ? C00R C00V C00G 118.3(3) . . ? C00R C00V C01I 120.6(3) . . ? C00G C00V C01I 121.1(3) . . ? C00Y C00W C00P 122.0(3) . . ? C00Y C00W H00W 119.0 . . ? C00P C00W H00W 119.0 . . ? C00U C00X H00I 109.5 . . ? C00U C00X H00M 109.5 . . ? H00I C00X H00M 109.5 . . ? C00U C00X H00P 109.5 . . ? H00I C00X H00P 109.5 . . ? H00M C00X H00P 109.5 . . ? C00W C00Y C01C 117.9(3) . . ? C00W C00Y C01G 120.5(3) . . ? C01C C00Y C01G 121.6(3) . . ? C01C C00Z C00I 118.2(3) . . ? C01C C00Z C015 121.1(3) . . ? C00I C00Z C015 120.7(3) . . ? C014 C010 N009 109.0(2) . . ? C014 C010 H010 125.5 . . ? N009 C010 H010 125.5 . . ? C00P C011 H01A 109.5 . . ? C00P C011 H01B 109.5 . . ? H01A C011 H01B 109.5 . . ? C00P C011 H01C 109.5 . . ? H01A C011 H01C 109.5 . . ? H01B C011 H01C 109.5 . . ? C00L C012 H01D 109.5 . . ? C00L C012 H01E 109.5 . . ? H01D C012 H01E 109.5 . . ? C00L C012 H01F 109.5 . . ? H01D C012 H01F 109.5 . . ? H01E C012 H01F 109.5 . . ? C00C C013 H01G 109.5 . . ? C00C C013 H01H 109.5 . . ? H01G C013 H01H 109.5 . . ? C00C C013 H01I 109.5 . . ? H01G C013 H01I 109.5 . . ? H01H C013 H01I 109.5 . . ? C010 C014 N008 109.5(2) . . ? C010 C014 H014 125.3 . . ? N008 C014 H014 125.3 . . ? C00Z C015 H01J 109.5 . . ? C00Z C015 H01K 109.5 . . ? H01J C015 H01K 109.5 . . ? C00Z C015 H01L 109.5 . . ? H01J C015 H01L 109.5 . . ? H01K C015 H01L 109.5 . . ? N00A C016 C01A 110.1(3) . . ? N00A C016 C019 110.4(2) . . ? C01A C016 C019 111.6(2) . . ? N00A C016 H016 108.2 . . ? C01A C016 H016 108.2 . . ? C019 C016 H016 108.2 . . ? C00B C017 H01M 109.5 . . ? C00B C017 H01N 109.5 . . ? H01M C017 H01N 109.5 . . ? C00B C017 H01O 109.5 . . ? H01M C017 H01O 109.5 . . ? H01N C017 H01O 109.5 . . ? O004 C018 C01H 107.8(3) . . ? O004 C018 H01P 110.2 . . ? C01H C018 H01P 110.1 . . ? O004 C018 H01Q 110.1 . . ? C01H C018 H01Q 110.1 . . ? H01P C018 H01Q 108.5 . . ? C016 C019 H01R 109.5 . . ? C016 C019 H01S 109.5 . . ? H01R C019 H01S 109.5 . . ? C016 C019 H01T 109.5 . . ? H01R C019 H01T 109.5 . . ? H01S C019 H01T 109.5 . . ? C016 C01A H01U 109.5 . . ? C016 C01A H01V 109.5 . . ? H01U C01A H01V 109.5 . . ? C016 C01A H01W 109.5 . . ? H01U C01A H01W 109.5 . . ? H01V C01A H01W 109.5 . . ? C00L C01B H01X 109.5 . . ? C00L C01B H01Y 109.5 . . ? H01X C01B H01Y 109.5 . . ? C00L C01B H01Z 109.5 . . ? H01X C01B H01Z 109.5 . . ? H01Y C01B H01Z 109.5 . . ? C00Y C01C C00Z 122.2(3) . . ? C00Y C01C H011 118.9 . . ? C00Z C01C H011 118.9 . . ? C00M C01D H012 109.5 . . ? C00M C01D H013 109.5 . . ? H012 C01D H013 109.5 . . ? C00M C01D H015 109.5 . . ? H012 C01D H015 109.5 . . ? H013 C01D H015 109.5 . . ? O004 C01E C01F 108.7(3) . . ? O004 C01E H017 109.9 . . ? C01F C01E H017 109.9 . . ? O004 C01E H018 109.9 . . ? C01F C01E H018 109.9 . . ? H017 C01E H018 108.3 . . ? C01E C01F H019 109.5 . . ? C01E C01F H020 109.5 . . ? H019 C01F H020 109.5 . . ? C01E C01F H021 109.5 . . ? H019 C01F H021 109.5 . . ? H020 C01F H021 109.5 . . ? C00Y C01G H022 109.5 . . ? C00Y C01G H023 109.5 . . ? H022 C01G H023 109.5 . . ? C00Y C01G H024 109.5 . . ? H022 C01G H024 109.5 . . ? H023 C01G H024 109.5 . . ? C018 C01H H025 109.5 . . ? C018 C01H H026 109.5 . . ? H025 C01H H026 109.5 . . ? C018 C01H H027 109.5 . . ? H025 C01H H027 109.5 . . ? H026 C01H H027 109.5 . . ? C00V C01I H028 109.5 . . ? C00V C01I H029 109.5 . . ? H028 C01I H029 109.5 . . ? C00V C01I H02A 109.5 . . ? H028 C01I H02A 109.5 . . ? H029 C01I H02A 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 Ni01 C00D 1.914(3) . ? Ni01 C00Q 1.918(2) . ? Ni01 S003 2.1804(7) . ? Ni01 S002 2.1915(7) . ? S002 C00F 1.769(3) . ? S003 C00F 1.776(3) . ? O004 C01E 1.413(4) . ? O004 C018 1.420(4) . ? N005 C00D 1.361(3) . ? N005 C00K 1.383(4) . ? N005 C00B 1.468(3) . ? N006 C00Q 1.360(3) . ? N006 C00O 1.385(4) . ? N006 C00U 1.472(3) . ? N007 C00D 1.370(3) . ? N007 C00N 1.385(3) . ? N007 C00L 1.469(3) . ? N008 C014 1.399(4) . ? N008 C00E 1.421(3) . ? N008 C00I 1.427(4) . ? N009 C010 1.405(4) . ? N009 C00E 1.418(3) . ? N009 C00H 1.434(3) . ? N00A C00Q 1.367(3) . ? N00A C00J 1.381(4) . ? N00A C016 1.478(4) . ? C00B C00S 1.519(4) . ? C00B C017 1.521(4) . ? C00B H00B 1.0000 . ? C00C C00H 1.389(4) . ? C00C C00G 1.390(4) . ? C00C C013 1.504(4) . ? C00E C00F 1.336(4) . ? C00G C00V 1.386(4) . ? C00G H00G 0.9500 . ? C00H C00M 1.399(4) . ? C00I C00P 1.395(4) . ? C00I C00Z 1.398(4) . ? C00J C00O 1.335(4) . ? C00J H00J 0.9500 . ? C00K C00N 1.336(4) . ? C00K H00K 0.9500 . ? C00L C012 1.523(4) . ? C00L C01B 1.523(4) . ? C00L H00L 1.0000 . ? C00M C00R 1.392(4) . ? C00M C01D 1.498(4) . ? C00N H00N 0.9500 . ? C00O H00O 0.9500 . ? C00P C00W 1.390(4) . ? C00P C011 1.506(4) . ? C00R C00V 1.383(5) . ? C00R H00R 0.9500 . ? C00S H00A 0.9800 . ? C00S H00C 0.9800 . ? C00S H00D 0.9800 . ? C00T C00U 1.520(4) . ? C00T H00E 0.9800 . ? C00T H00F 0.9800 . ? C00T H00H 0.9800 . ? C00U C00X 1.516(4) . ? C00U H00U 1.0000 . ? C00V C01I 1.514(4) . ? C00W C00Y 1.387(4) . ? C00W H00W 0.9500 . ? C00X H00I 0.9800 . ? C00X H00M 0.9800 . ? C00X H00P 0.9800 . ? C00Y C01C 1.388(5) . ? C00Y C01G 1.508(5) . ? C00Z C01C 1.393(4) . ? C00Z C015 1.505(4) . ? C010 C014 1.326(4) . ? C010 H010 0.9500 . ? C011 H01A 0.9800 . ? C011 H01B 0.9800 . ? C011 H01C 0.9800 . ? C012 H01D 0.9800 . ? C012 H01E 0.9800 . ? C012 H01F 0.9800 . ? C013 H01G 0.9800 . ? C013 H01H 0.9800 . ? C013 H01I 0.9800 . ? C014 H014 0.9500 . ? C015 H01J 0.9800 . ? C015 H01K 0.9800 . ? C015 H01L 0.9800 . ? C016 C01A 1.517(4) . ? C016 C019 1.522(4) . ? C016 H016 1.0000 . ? C017 H01M 0.9800 . ? C017 H01N 0.9800 . ? C017 H01O 0.9800 . ? C018 C01H 1.502(5) . ? C018 H01P 0.9900 . ? C018 H01Q 0.9900 . ? C019 H01R 0.9800 . ? C019 H01S 0.9800 . ? C019 H01T 0.9800 . ? C01A H01U 0.9800 . ? C01A H01V 0.9800 . ? C01A H01W 0.9800 . ? C01B H01X 0.9800 . ? C01B H01Y 0.9800 . ? C01B H01Z 0.9800 . ? C01C H011 0.9500 . ? C01D H012 0.9800 . ? C01D H013 0.9800 . ? C01D H015 0.9800 . ? C01E C01F 1.504(5) . ? C01E H017 0.9900 . ? C01E H018 0.9900 . ? C01F H019 0.9800 . ? C01F H020 0.9800 . ? C01F H021 0.9800 . ? C01G H022 0.9800 . ? C01G H023 0.9800 . ? C01G H024 0.9800 . ? C01H H025 0.9800 . ? C01H H026 0.9800 . ? C01H H027 0.9800 . ? C01I H028 0.9800 . ? C01I H029 0.9800 . ? C01I H02A 0.9800 . ?