#------------------------------------------------------------------------------ #$Date: 2025-02-12 01:08:47 +0200 (Wed, 12 Feb 2025) $ #$Revision: 297685 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/38/1573881.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_1573881 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 'C56 H72 N4 Ni S4, 2 (C4 H8 O)' _chemical_formula_sum 'C64 H88 N4 Ni O2 S4' _chemical_formula_weight 1132.33 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' _space_group_name_H-M_alt 'P 1 21/n 1' _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 91.7210(10) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 10.36020(10) _cell_length_b 22.0224(2) _cell_length_c 13.63690(10) _cell_measurement_reflns_used 20512 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 76.6930 _cell_measurement_theta_min 3.8140 _cell_volume 3109.94(5) _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 0.994 _diffrn_measured_fraction_theta_max 0.972 _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 0.0359 _diffrn_reflns_av_unetI/netI 0.0255 _diffrn_reflns_Laue_measured_fraction_full 0.994 _diffrn_reflns_Laue_measured_fraction_max 0.972 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_number 30670 _diffrn_reflns_point_group_measured_fraction_full 0.994 _diffrn_reflns_point_group_measured_fraction_max 0.972 _diffrn_reflns_theta_full 72.000 _diffrn_reflns_theta_max 76.918 _diffrn_reflns_theta_min 3.814 _diffrn_source 'micro-focus sealed X-ray tube' _exptl_absorpt_coefficient_mu 2.037 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.527 _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 1.209 _exptl_crystal_description block _exptl_crystal_F_000 1216 _exptl_crystal_size_max 0.180 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_min 0.080 _refine_diff_density_max 0.272 _refine_diff_density_min -0.350 _refine_diff_density_rms 0.046 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.072 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 348 _refine_ls_number_reflns 6379 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.072 _refine_ls_R_factor_all 0.0333 _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^)+(0.0320P)^2^+1.5137P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0768 _refine_ls_wR_factor_ref 0.0785 _reflns_Friedel_coverage 0.000 _reflns_number_gt 5793 _reflns_number_total 6379 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4sc08449g2.cif _cod_data_source_block Compound_3b _cod_original_sg_symbol_H-M 'P 21/n' _cod_database_code 1573881 _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 0.710 _shelx_estimated_absorpt_t_max 0.854 _shelx_res_file ; TITL MaLu105_ref_a.res in P2(1)/n MaLu105_ref_a.res created by SHELXL-2018/3 at 19:20:50 on 12-Mar-2023 REM Old TITL MaLu105_ref in P2(1)/n REM SHELXT solution in P2(1)/n REM R1 0.101, Rweak 0.008, Alpha 0.033, Orientation as input REM Formula found by SHELXT: C64 N4 O2 S4 Ni CELL 1.54184 10.3602 22.0224 13.6369 90.000 91.721 90.000 ZERR 2.000 0.0001 0.0002 0.0001 0.000 0.001 0.000 LATT 1 SYMM 1/2-X, 1/2+Y, 1/2-Z SFAC C H N O S NI UNIT 128 176 8 4 8 2 TEMP -173 SIZE 0.08 0.10 0.18 L.S. 10 BOND $H LIST 4 ACTA 144 FMAP 2 PLAN 20 WGHT 0.032000 1.513700 FVAR 0.39328 NI01 6 0.500000 0.500000 0.500000 10.50000 0.01155 0.01310 = 0.01522 -0.00451 -0.00064 -0.00119 S002 5 0.555607 0.425390 0.405421 11.00000 0.01089 0.01648 = 0.01970 -0.00659 -0.00062 -0.00072 S003 5 0.310939 0.470836 0.443345 11.00000 0.01164 0.01629 = 0.01888 -0.00654 -0.00015 0.00003 O004 4 0.021559 0.187269 0.198658 11.00000 0.02792 0.02320 = 0.03956 -0.00575 -0.00864 -0.00231 N005 3 0.207541 0.356744 0.307058 11.00000 0.01136 0.01342 = 0.01604 -0.00238 -0.00161 -0.00049 N006 3 0.401132 0.326144 0.269003 11.00000 0.01189 0.01215 = 0.01405 -0.00235 -0.00150 0.00045 C007 1 0.337111 0.369602 0.321578 11.00000 0.01225 0.01219 = 0.01314 0.00133 0.00037 0.00078 C008 1 0.099367 0.394984 0.330820 11.00000 0.00957 0.01434 = 0.01687 -0.00300 -0.00147 -0.00116 C009 1 0.193553 0.305576 0.248009 11.00000 0.01674 0.01490 = 0.01980 -0.00371 -0.00300 -0.00303 AFIX 43 H009 2 0.114248 0.287239 0.227507 11.00000 -1.20000 AFIX 0 C00A 1 0.311826 0.286745 0.225183 11.00000 0.01787 0.01316 = 0.01708 -0.00386 -0.00256 -0.00166 AFIX 43 H00A 2 0.331283 0.252489 0.185948 11.00000 -1.20000 AFIX 0 C00B 1 0.538216 0.318823 0.258009 11.00000 0.01236 0.01440 = 0.01591 -0.00543 -0.00122 0.00094 C00C 1 0.060829 0.439227 0.262756 11.00000 0.01359 0.01820 = 0.01658 -0.00093 -0.00131 -0.00095 C00D 1 0.035716 0.384603 0.418469 11.00000 0.01387 0.01833 = 0.01802 -0.00005 -0.00184 -0.00320 C00E 1 0.392240 0.415541 0.379505 11.00000 0.01186 0.01459 = 0.01471 -0.00083 -0.00013 -0.00006 C00F 1 0.600876 0.274002 0.314091 11.00000 0.02092 0.01636 = 0.01832 -0.00509 -0.00515 0.00323 C00G 1 -0.115460 0.462881 0.367790 11.00000 0.01525 0.02527 = 0.02827 -0.00190 0.00265 0.00532 AFIX 43 H00G 2 -0.190916 0.485854 0.379972 11.00000 -1.20000 AFIX 0 C00H 1 0.600390 0.354913 0.189266 11.00000 0.01873 0.01531 = 0.02163 -0.00539 0.00356 -0.00185 C00I 1 0.085357 0.337934 0.492438 11.00000 0.01844 0.02459 = 0.02082 0.00612 0.00129 -0.00181 AFIX 13 H00I 2 0.180668 0.334108 0.484569 11.00000 -1.20000 AFIX 0 C00J 1 -0.048729 0.472973 0.283088 11.00000 0.01792 0.01969 = 0.02379 0.00224 -0.00257 0.00300 AFIX 43 H00J 2 -0.078008 0.503322 0.238185 11.00000 -1.20000 AFIX 0 C00K 1 0.532704 0.239949 0.394125 11.00000 0.03277 0.02226 = 0.01835 0.00301 -0.00326 0.00738 AFIX 13 H00K 2 0.448753 0.260957 0.404950 11.00000 -1.20000 AFIX 0 C00L 1 0.135185 0.451689 0.170496 11.00000 0.01924 0.02827 = 0.01830 0.00542 0.00011 0.00503 AFIX 13 H00L 2 0.217937 0.428352 0.175238 11.00000 -1.20000 AFIX 0 C00M 1 -0.073393 0.419643 0.434977 11.00000 0.01636 0.02842 = 0.02191 0.00072 0.00536 0.00059 AFIX 43 H00M 2 -0.119657 0.413749 0.493320 11.00000 -1.20000 AFIX 0 C00N 1 0.529301 0.405498 0.134751 11.00000 0.02856 0.01644 = 0.02252 0.00233 0.00712 -0.00040 AFIX 13 H00N 2 0.464681 0.422447 0.180396 11.00000 -1.20000 AFIX 0 C00O 1 0.730368 0.342929 0.175211 11.00000 0.02048 0.02475 = 0.03781 -0.00644 0.01052 -0.00470 AFIX 43 H00O 2 0.776149 0.366415 0.129290 11.00000 -1.20000 AFIX 0 C00P 1 0.730893 0.263566 0.296029 11.00000 0.02034 0.02521 = 0.03405 -0.00920 -0.00948 0.00811 AFIX 43 H00P 2 0.776422 0.232844 0.331655 11.00000 -1.20000 AFIX 0 C00Q 1 0.794066 0.297319 0.227080 11.00000 0.01309 0.03102 = 0.04811 -0.01434 0.00164 0.00334 AFIX 43 H00Q 2 0.882240 0.289186 0.215048 11.00000 -1.20000 AFIX 0 C00R 1 0.063178 0.356848 0.598404 11.00000 0.03322 0.04248 = 0.01986 0.00657 -0.00004 0.00189 AFIX 137 H00B 2 0.100312 0.397212 0.610219 11.00000 -1.50000 H00C 2 0.104733 0.327477 0.643158 11.00000 -1.50000 H00D 2 -0.029736 0.357987 0.609802 11.00000 -1.50000 AFIX 0 C00S 1 -0.081879 0.155844 0.148058 11.00000 0.02668 0.03308 = 0.03713 -0.01541 -0.00577 -0.00035 AFIX 23 H00E 2 -0.055276 0.142094 0.082565 11.00000 -1.20000 H00F 2 -0.158815 0.182243 0.140017 11.00000 -1.20000 AFIX 0 C00T 1 0.059681 0.429870 0.079469 11.00000 0.05282 0.03553 = 0.01919 -0.00362 0.00245 -0.00636 AFIX 137 H00H 2 0.110322 0.437396 0.021145 11.00000 -1.50000 H00R 2 -0.022346 0.451920 0.073545 11.00000 -1.50000 H00S 2 0.042544 0.386271 0.085219 11.00000 -1.50000 AFIX 0 C00U 1 0.453878 0.382103 0.044070 11.00000 0.04607 0.02356 = 0.02916 0.00550 -0.00449 0.00050 AFIX 137 H00T 2 0.401576 0.415107 0.015559 11.00000 -1.50000 H00U 2 0.397297 0.348722 0.063084 11.00000 -1.50000 H00V 2 0.514514 0.367514 -0.004438 11.00000 -1.50000 AFIX 0 C00V 1 0.618757 0.457678 0.107416 11.00000 0.04860 0.02322 = 0.03914 0.00538 0.01112 -0.00814 AFIX 137 H00W 2 0.677611 0.443945 0.057037 11.00000 -1.50000 H00X 2 0.668934 0.470739 0.165724 11.00000 -1.50000 H00Y 2 0.567046 0.491784 0.081972 11.00000 -1.50000 AFIX 0 C00W 1 0.502442 0.174407 0.364466 11.00000 0.05021 0.02705 = 0.02489 0.00371 -0.00363 -0.00655 AFIX 137 H00Z 2 0.450220 0.174183 0.303344 11.00000 -1.50000 H010 2 0.454439 0.154607 0.416409 11.00000 -1.50000 H011 2 0.583272 0.152422 0.354634 11.00000 -1.50000 AFIX 0 C00X 1 0.024860 0.084844 0.253999 11.00000 0.03948 0.02658 = 0.03444 -0.00546 0.00479 -0.00365 AFIX 23 H012 2 0.023288 0.076610 0.325322 11.00000 -1.20000 H013 2 0.057933 0.048506 0.220171 11.00000 -1.20000 AFIX 0 C00Y 1 0.025623 0.275449 0.473024 11.00000 0.05398 0.02594 = 0.03523 0.01140 -0.00831 -0.00990 AFIX 137 H014 2 0.045193 0.262256 0.406466 11.00000 -1.50000 H015 2 -0.068184 0.277840 0.479549 11.00000 -1.50000 H016 2 0.061566 0.246193 0.520612 11.00000 -1.50000 AFIX 0 C00Z 1 0.168430 0.518861 0.161648 11.00000 0.05223 0.04228 = 0.02722 0.00211 0.00716 -0.02334 AFIX 137 H017 2 0.225713 0.524786 0.106558 11.00000 -1.50000 H018 2 0.211949 0.532664 0.222436 11.00000 -1.50000 H019 2 0.088999 0.542315 0.150263 11.00000 -1.50000 AFIX 0 C010 1 -0.109513 0.102352 0.213481 11.00000 0.02957 0.03454 = 0.04902 -0.01485 0.00729 -0.00824 AFIX 23 H01A 2 -0.149559 0.068572 0.175556 11.00000 -1.20000 H01B 2 -0.167130 0.114037 0.266937 11.00000 -1.20000 AFIX 0 C011 1 0.611594 0.241926 0.490928 11.00000 0.06670 0.03134 = 0.02283 0.00069 -0.01467 0.00647 AFIX 137 H01C 2 0.689350 0.216995 0.485152 11.00000 -1.50000 H01D 2 0.559366 0.226091 0.543935 11.00000 -1.50000 H01E 2 0.636523 0.283955 0.505610 11.00000 -1.50000 AFIX 0 C012 1 0.107006 0.140548 0.232826 11.00000 0.02634 0.03063 = 0.05875 0.00321 -0.00577 -0.00050 AFIX 23 H01F 2 0.154449 0.153831 0.293173 11.00000 -1.20000 H01G 2 0.170556 0.130933 0.182310 11.00000 -1.20000 AFIX 0 HKLF 4 REM MaLu105_ref_a.res in P2(1)/n REM wR2 = 0.078503, GooF = S = 1.07243, Restrained GooF = 1.07243 for all data REM R1 = 0.030391 for 5793 Fo > 4sig(Fo) and 0.033281 for all 6379 data REM 348 parameters refined using 0 restraints END WGHT 0.0320 1.5137 REM Highest difference peak 0.272, deepest hole -0.350, 1-sigma level 0.046 Q1 1 0.2771 0.3649 0.3162 11.00000 0.05 0.27 Q2 1 0.1031 0.4454 0.2208 11.00000 0.05 0.26 Q3 1 0.0758 0.3945 0.3823 11.00000 0.05 0.26 Q4 1 0.3517 0.4283 0.4227 11.00000 0.05 0.26 Q5 1 0.0599 0.3604 0.4572 11.00000 0.05 0.25 Q6 1 0.0762 0.3470 0.5420 11.00000 0.05 0.25 Q7 1 0.1550 0.3763 0.3175 11.00000 0.05 0.24 Q8 1 0.3645 0.3990 0.3364 11.00000 0.05 0.23 Q9 1 0.2012 0.3317 0.2759 11.00000 0.05 0.23 Q10 1 0.6617 0.2632 0.2970 11.00000 0.05 0.23 Q11 1 -0.0268 0.3955 0.4217 11.00000 0.05 0.22 Q12 1 0.5785 0.3431 0.2364 11.00000 0.05 0.22 Q13 1 0.5674 0.3827 0.1660 11.00000 0.05 0.22 Q14 1 0.1999 0.1551 0.2451 11.00000 0.05 0.22 Q15 1 0.4829 0.5537 0.5141 11.00000 0.05 0.22 Q16 1 0.0632 0.3078 0.4812 11.00000 0.05 0.21 Q17 1 0.5682 0.2589 0.3536 11.00000 0.05 0.21 Q18 1 0.0219 0.4600 0.2788 11.00000 0.05 0.21 Q19 1 0.3742 0.3490 0.2896 11.00000 0.05 0.21 Q20 1 0.5774 0.3047 0.2994 11.00000 0.05 0.21 ; _shelx_res_checksum 58697 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Ni01 Ni 0.500000 0.500000 0.500000 0.01331(8) Uani 1 2 d S . P . . S002 S 0.55561(3) 0.42539(2) 0.40542(2) 0.01571(8) Uani 1 1 d . . . . . S003 S 0.31094(3) 0.47084(2) 0.44334(2) 0.01561(8) Uani 1 1 d . . . . . O004 O 0.02156(10) 0.18727(5) 0.19866(9) 0.0304(2) Uani 1 1 d . . . . . N005 N 0.20754(10) 0.35674(5) 0.30706(8) 0.0136(2) Uani 1 1 d . . . . . N006 N 0.40113(10) 0.32614(5) 0.26900(7) 0.0127(2) Uani 1 1 d . . . . . C007 C 0.33711(12) 0.36960(6) 0.32158(9) 0.0125(2) Uani 1 1 d . . . . . C008 C 0.09937(11) 0.39498(6) 0.33082(9) 0.0136(2) Uani 1 1 d . . . . . C009 C 0.19355(13) 0.30558(6) 0.24801(10) 0.0172(3) Uani 1 1 d . . . . . H009 H 0.114248 0.287239 0.227507 0.021 Uiso 1 1 calc R U . . . C00A C 0.31183(13) 0.28675(6) 0.22518(9) 0.0161(3) Uani 1 1 d . . . . . H00A H 0.331283 0.252489 0.185948 0.019 Uiso 1 1 calc R U . . . C00B C 0.53822(12) 0.31882(6) 0.25801(9) 0.0143(2) Uani 1 1 d . . . . . C00C C 0.06083(12) 0.43923(6) 0.26276(9) 0.0162(3) Uani 1 1 d . . . . . C00D C 0.03572(12) 0.38460(6) 0.41847(10) 0.0168(3) Uani 1 1 d . . . . . C00E C 0.39224(12) 0.41554(6) 0.37950(9) 0.0137(2) Uani 1 1 d . . . . . C00F C 0.60088(13) 0.27400(6) 0.31409(10) 0.0186(3) Uani 1 1 d . . . . . C00G C -0.11546(13) 0.46288(7) 0.36779(11) 0.0229(3) Uani 1 1 d . . . . . H00G H -0.190916 0.485854 0.379972 0.027 Uiso 1 1 calc R U . . . C00H C 0.60039(13) 0.35491(6) 0.18927(10) 0.0185(3) Uani 1 1 d . . . . . C00I C 0.08536(13) 0.33793(7) 0.49244(10) 0.0213(3) Uani 1 1 d . . . . . H00I H 0.180668 0.334108 0.484569 0.026 Uiso 1 1 calc R U . . . C00J C -0.04873(13) 0.47297(6) 0.28309(10) 0.0205(3) Uani 1 1 d . . . . . H00J H -0.078008 0.503322 0.238185 0.025 Uiso 1 1 calc R U . . . C00K C 0.53270(15) 0.23995(7) 0.39412(10) 0.0245(3) Uani 1 1 d . . . . . H00K H 0.448753 0.260957 0.404950 0.029 Uiso 1 1 calc R U . . . C00L C 0.13518(14) 0.45169(7) 0.17050(10) 0.0219(3) Uani 1 1 d . . . . . H00L H 0.217937 0.428352 0.175238 0.026 Uiso 1 1 calc R U . . . C00M C -0.07339(13) 0.41964(7) 0.43498(10) 0.0221(3) Uani 1 1 d . . . . . H00M H -0.119657 0.413749 0.493320 0.027 Uiso 1 1 calc R U . . . C00N C 0.52930(14) 0.40550(6) 0.13475(10) 0.0224(3) Uani 1 1 d . . . . . H00N H 0.464681 0.422447 0.180396 0.027 Uiso 1 1 calc R U . . . C00O C 0.73037(14) 0.34293(7) 0.17521(12) 0.0275(3) Uani 1 1 d . . . . . H00O H 0.776149 0.366415 0.129290 0.033 Uiso 1 1 calc R U . . . C00P C 0.73089(14) 0.26357(7) 0.29603(12) 0.0267(3) Uani 1 1 d . . . . . H00P H 0.776422 0.232844 0.331655 0.032 Uiso 1 1 calc R U . . . C00Q C 0.79407(14) 0.29732(7) 0.22708(13) 0.0307(4) Uani 1 1 d . . . . . H00Q H 0.882240 0.289186 0.215048 0.037 Uiso 1 1 calc R U . . . C00R C 0.06318(16) 0.35685(8) 0.59840(11) 0.0319(4) Uani 1 1 d . . . . . H00B H 0.100312 0.397212 0.610219 0.048 Uiso 1 1 calc R U . . . H00C H 0.104733 0.327477 0.643158 0.048 Uiso 1 1 calc R U . . . H00D H -0.029736 0.357987 0.609802 0.048 Uiso 1 1 calc R U . . . C00S C -0.08188(16) 0.15584(8) 0.14806(13) 0.0324(4) Uani 1 1 d . . . . . H00E H -0.055276 0.142094 0.082565 0.039 Uiso 1 1 calc R U . . . H00F H -0.158815 0.182243 0.140017 0.039 Uiso 1 1 calc R U . . . C00T C 0.05968(19) 0.42987(8) 0.07947(11) 0.0358(4) Uani 1 1 d . . . . . H00H H 0.110322 0.437396 0.021145 0.054 Uiso 1 1 calc R U . . . H00R H -0.022346 0.451920 0.073545 0.054 Uiso 1 1 calc R U . . . H00S H 0.042544 0.386271 0.085219 0.054 Uiso 1 1 calc R U . . . C00U C 0.45388(18) 0.38210(7) 0.04407(12) 0.0330(4) Uani 1 1 d . . . . . H00T H 0.401576 0.415107 0.015559 0.050 Uiso 1 1 calc R U . . . H00U H 0.397297 0.348722 0.063084 0.050 Uiso 1 1 calc R U . . . H00V H 0.514514 0.367514 -0.004438 0.050 Uiso 1 1 calc R U . . . C00V C 0.61876(18) 0.45768(8) 0.10742(13) 0.0368(4) Uani 1 1 d . . . . . H00W H 0.677611 0.443945 0.057037 0.055 Uiso 1 1 calc R U . . . H00X H 0.668934 0.470739 0.165724 0.055 Uiso 1 1 calc R U . . . H00Y H 0.567046 0.491784 0.081972 0.055 Uiso 1 1 calc R U . . . C00W C 0.50244(18) 0.17441(8) 0.36447(12) 0.0341(4) Uani 1 1 d . . . . . H00Z H 0.450220 0.174183 0.303344 0.051 Uiso 1 1 calc R U . . . H010 H 0.454439 0.154607 0.416409 0.051 Uiso 1 1 calc R U . . . H011 H 0.583272 0.152422 0.354634 0.051 Uiso 1 1 calc R U . . . C00X C 0.02486(17) 0.08484(8) 0.25400(13) 0.0334(4) Uani 1 1 d . . . . . H012 H 0.023288 0.076610 0.325322 0.040 Uiso 1 1 calc R U . . . H013 H 0.057933 0.048506 0.220171 0.040 Uiso 1 1 calc R U . . . C00Y C 0.02562(19) 0.27545(8) 0.47302(13) 0.0386(4) Uani 1 1 d . . . . . H014 H 0.045193 0.262256 0.406466 0.058 Uiso 1 1 calc R U . . . H015 H -0.068184 0.277840 0.479549 0.058 Uiso 1 1 calc R U . . . H016 H 0.061566 0.246193 0.520612 0.058 Uiso 1 1 calc R U . . . C00Z C 0.1684(2) 0.51886(9) 0.16165(13) 0.0405(4) Uani 1 1 d . . . . . H017 H 0.225713 0.524786 0.106558 0.061 Uiso 1 1 calc R U . . . H018 H 0.211949 0.532664 0.222436 0.061 Uiso 1 1 calc R U . . . H019 H 0.088999 0.542315 0.150263 0.061 Uiso 1 1 calc R U . . . C010 C -0.10951(17) 0.10235(8) 0.21348(14) 0.0376(4) Uani 1 1 d . . . . . H01A H -0.149559 0.068572 0.175556 0.045 Uiso 1 1 calc R U . . . H01B H -0.167130 0.114037 0.266937 0.045 Uiso 1 1 calc R U . . . C011 C 0.6116(2) 0.24193(8) 0.49093(12) 0.0406(4) Uani 1 1 d . . . . . H01C H 0.689350 0.216995 0.485152 0.061 Uiso 1 1 calc R U . . . H01D H 0.559366 0.226091 0.543935 0.061 Uiso 1 1 calc R U . . . H01E H 0.636523 0.283955 0.505610 0.061 Uiso 1 1 calc R U . . . C012 C 0.10701(17) 0.14055(8) 0.23283(15) 0.0387(4) Uani 1 1 d . . . . . H01F H 0.154449 0.153831 0.293173 0.046 Uiso 1 1 calc R U . . . H01G H 0.170556 0.130933 0.182310 0.046 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 0.01155(15) 0.01310(16) 0.01522(16) -0.00451(12) -0.00064(11) -0.00119(11) S002 0.01089(14) 0.01648(16) 0.01970(16) -0.00659(12) -0.00062(11) -0.00072(11) S003 0.01164(14) 0.01629(16) 0.01888(16) -0.00654(12) -0.00015(11) 0.00003(11) O004 0.0279(6) 0.0232(5) 0.0396(6) -0.0058(5) -0.0086(5) -0.0023(4) N005 0.0114(5) 0.0134(5) 0.0160(5) -0.0024(4) -0.0016(4) -0.0005(4) N006 0.0119(5) 0.0122(5) 0.0140(5) -0.0024(4) -0.0015(4) 0.0004(4) C007 0.0123(6) 0.0122(6) 0.0131(6) 0.0013(5) 0.0004(4) 0.0008(5) C008 0.0096(5) 0.0143(6) 0.0169(6) -0.0030(5) -0.0015(4) -0.0012(5) C009 0.0167(6) 0.0149(6) 0.0198(6) -0.0037(5) -0.0030(5) -0.0030(5) C00A 0.0179(6) 0.0132(6) 0.0171(6) -0.0039(5) -0.0026(5) -0.0017(5) C00B 0.0124(6) 0.0144(6) 0.0159(6) -0.0054(5) -0.0012(5) 0.0009(5) C00C 0.0136(6) 0.0182(6) 0.0166(6) -0.0009(5) -0.0013(5) -0.0010(5) C00D 0.0139(6) 0.0183(6) 0.0180(6) 0.0000(5) -0.0018(5) -0.0032(5) C00E 0.0119(6) 0.0146(6) 0.0147(6) -0.0008(5) -0.0001(4) -0.0001(5) C00F 0.0209(7) 0.0164(6) 0.0183(6) -0.0051(5) -0.0051(5) 0.0032(5) C00G 0.0153(6) 0.0253(7) 0.0283(7) -0.0019(6) 0.0026(5) 0.0053(5) C00H 0.0187(6) 0.0153(6) 0.0216(6) -0.0054(5) 0.0036(5) -0.0019(5) C00I 0.0184(6) 0.0246(7) 0.0208(7) 0.0061(6) 0.0013(5) -0.0018(5) C00J 0.0179(7) 0.0197(7) 0.0238(7) 0.0022(5) -0.0026(5) 0.0030(5) C00K 0.0328(8) 0.0223(7) 0.0184(7) 0.0030(6) -0.0033(6) 0.0074(6) C00L 0.0192(7) 0.0283(8) 0.0183(7) 0.0054(6) 0.0001(5) 0.0050(6) C00M 0.0164(6) 0.0284(8) 0.0219(7) 0.0007(6) 0.0054(5) 0.0006(6) C00N 0.0286(7) 0.0164(7) 0.0225(7) 0.0023(5) 0.0071(6) -0.0004(6) C00O 0.0205(7) 0.0248(8) 0.0378(8) -0.0064(6) 0.0105(6) -0.0047(6) C00P 0.0203(7) 0.0252(8) 0.0341(8) -0.0092(6) -0.0095(6) 0.0081(6) C00Q 0.0131(7) 0.0310(8) 0.0481(10) -0.0143(7) 0.0016(6) 0.0033(6) C00R 0.0332(8) 0.0425(10) 0.0199(7) 0.0066(7) 0.0000(6) 0.0019(7) C00S 0.0267(8) 0.0331(9) 0.0371(9) -0.0154(7) -0.0058(6) -0.0004(7) C00T 0.0528(11) 0.0355(9) 0.0192(7) -0.0036(7) 0.0024(7) -0.0064(8) C00U 0.0461(10) 0.0236(8) 0.0292(8) 0.0055(6) -0.0045(7) 0.0005(7) C00V 0.0486(10) 0.0232(8) 0.0391(9) 0.0054(7) 0.0111(8) -0.0081(7) C00W 0.0502(10) 0.0271(8) 0.0249(8) 0.0037(6) -0.0036(7) -0.0066(7) C00X 0.0395(9) 0.0266(8) 0.0344(9) -0.0055(7) 0.0048(7) -0.0037(7) C00Y 0.0540(11) 0.0259(9) 0.0352(9) 0.0114(7) -0.0083(8) -0.0099(8) C00Z 0.0522(11) 0.0423(10) 0.0272(8) 0.0021(7) 0.0072(8) -0.0233(9) C010 0.0296(8) 0.0345(9) 0.0490(10) -0.0149(8) 0.0073(7) -0.0082(7) C011 0.0667(13) 0.0313(9) 0.0228(8) 0.0007(7) -0.0147(8) 0.0065(8) C012 0.0263(8) 0.0306(9) 0.0587(11) 0.0032(8) -0.0058(8) -0.0005(7) 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 S002 Ni01 S002 180.0 3_666 . ? S002 Ni01 S003 100.448(11) 3_666 . ? S002 Ni01 S003 79.553(11) . . ? S002 Ni01 S003 79.550(11) 3_666 3_666 ? S002 Ni01 S003 100.449(11) . 3_666 ? S003 Ni01 S003 180.0 . 3_666 ? C00E S002 Ni01 86.62(4) . . ? C00E S003 Ni01 86.55(4) . . ? C012 O004 C00S 104.86(12) . . ? C007 N005 C009 109.48(10) . . ? C007 N005 C008 127.24(10) . . ? C009 N005 C008 122.26(10) . . ? C007 N006 C00A 109.43(10) . . ? C007 N006 C00B 128.53(10) . . ? C00A N006 C00B 122.04(10) . . ? N006 C007 N005 105.32(10) . . ? N006 C007 C00E 127.09(11) . . ? N005 C007 C00E 127.57(11) . . ? C00C C008 C00D 123.28(12) . . ? C00C C008 N005 117.75(11) . . ? C00D C008 N005 118.93(11) . . ? C00A C009 N005 107.79(11) . . ? C00A C009 H009 126.1 . . ? N005 C009 H009 126.1 . . ? C009 C00A N006 107.98(11) . . ? C009 C00A H00A 126.0 . . ? N006 C00A H00A 126.0 . . ? C00F C00B C00H 123.50(12) . . ? C00F C00B N006 117.72(11) . . ? C00H C00B N006 118.72(11) . . ? C00J C00C C008 117.33(12) . . ? C00J C00C C00L 120.35(12) . . ? C008 C00C C00L 122.32(12) . . ? C00M C00D C008 116.91(12) . . ? C00M C00D C00I 121.86(12) . . ? C008 C00D C00I 121.22(12) . . ? C007 C00E S003 126.72(10) . . ? C007 C00E S002 125.96(10) . . ? S003 C00E S002 107.25(7) . . ? C00P C00F C00B 117.06(13) . . ? C00P C00F C00K 121.23(13) . . ? C00B C00F C00K 121.66(12) . . ? C00J C00G C00M 120.60(13) . . ? C00J C00G H00G 119.7 . . ? C00M C00G H00G 119.7 . . ? C00O C00H C00B 116.81(13) . . ? C00O C00H C00N 121.96(13) . . ? C00B C00H C00N 121.21(12) . . ? C00D C00I C00R 112.71(12) . . ? C00D C00I C00Y 111.52(12) . . ? C00R C00I C00Y 109.73(13) . . ? C00D C00I H00I 107.5 . . ? C00R C00I H00I 107.5 . . ? C00Y C00I H00I 107.5 . . ? C00G C00J C00C 120.81(13) . . ? C00G C00J H00J 119.6 . . ? C00C C00J H00J 119.6 . . ? C00F C00K C00W 111.89(12) . . ? C00F C00K C011 110.99(14) . . ? C00W C00K C011 110.77(13) . . ? C00F C00K H00K 107.7 . . ? C00W C00K H00K 107.7 . . ? C011 C00K H00K 107.7 . . ? C00C C00L C00Z 111.23(12) . . ? C00C C00L C00T 110.89(12) . . ? C00Z C00L C00T 110.67(13) . . ? C00C C00L H00L 108.0 . . ? C00Z C00L H00L 108.0 . . ? C00T C00L H00L 108.0 . . ? C00G C00M C00D 121.04(13) . . ? C00G C00M H00M 119.5 . . ? C00D C00M H00M 119.5 . . ? C00H C00N C00V 112.47(13) . . ? C00H C00N C00U 112.13(12) . . ? C00V C00N C00U 110.74(13) . . ? C00H C00N H00N 107.0 . . ? C00V C00N H00N 107.0 . . ? C00U C00N H00N 107.0 . . ? C00Q C00O C00H 121.05(14) . . ? C00Q C00O H00O 119.5 . . ? C00H C00O H00O 119.5 . . ? C00Q C00P C00F 120.79(14) . . ? C00Q C00P H00P 119.6 . . ? C00F C00P H00P 119.6 . . ? C00P C00Q C00O 120.71(14) . . ? C00P C00Q H00Q 119.6 . . ? C00O C00Q H00Q 119.6 . . ? C00I C00R H00B 109.5 . . ? C00I C00R H00C 109.5 . . ? H00B C00R H00C 109.5 . . ? C00I C00R H00D 109.5 . . ? H00B C00R H00D 109.5 . . ? H00C C00R H00D 109.5 . . ? O004 C00S C010 104.14(13) . . ? O004 C00S H00E 110.9 . . ? C010 C00S H00E 110.9 . . ? O004 C00S H00F 110.9 . . ? C010 C00S H00F 110.9 . . ? H00E C00S H00F 108.9 . . ? C00L C00T H00H 109.5 . . ? C00L C00T H00R 109.5 . . ? H00H C00T H00R 109.5 . . ? C00L C00T H00S 109.5 . . ? H00H C00T H00S 109.5 . . ? H00R C00T H00S 109.5 . . ? C00N C00U H00T 109.5 . . ? C00N C00U H00U 109.5 . . ? H00T C00U H00U 109.5 . . ? C00N C00U H00V 109.5 . . ? H00T C00U H00V 109.5 . . ? H00U C00U H00V 109.5 . . ? C00N C00V H00W 109.5 . . ? C00N C00V H00X 109.5 . . ? H00W C00V H00X 109.5 . . ? C00N C00V H00Y 109.5 . . ? H00W C00V H00Y 109.5 . . ? H00X C00V H00Y 109.5 . . ? C00K C00W H00Z 109.5 . . ? C00K C00W H010 109.5 . . ? H00Z C00W H010 109.5 . . ? C00K C00W H011 109.5 . . ? H00Z C00W H011 109.5 . . ? H010 C00W H011 109.5 . . ? C012 C00X C010 103.62(14) . . ? C012 C00X H012 111.0 . . ? C010 C00X H012 111.0 . . ? C012 C00X H013 111.0 . . ? C010 C00X H013 111.0 . . ? H012 C00X H013 109.0 . . ? C00I C00Y H014 109.5 . . ? C00I C00Y H015 109.5 . . ? H014 C00Y H015 109.5 . . ? C00I C00Y H016 109.5 . . ? H014 C00Y H016 109.5 . . ? H015 C00Y H016 109.5 . . ? C00L C00Z H017 109.5 . . ? C00L C00Z H018 109.5 . . ? H017 C00Z H018 109.5 . . ? C00L C00Z H019 109.5 . . ? H017 C00Z H019 109.5 . . ? H018 C00Z H019 109.5 . . ? C00S C010 C00X 102.89(13) . . ? C00S C010 H01A 111.2 . . ? C00X C010 H01A 111.2 . . ? C00S C010 H01B 111.2 . . ? C00X C010 H01B 111.2 . . ? H01A C010 H01B 109.1 . . ? C00K C011 H01C 109.5 . . ? C00K C011 H01D 109.5 . . ? H01C C011 H01D 109.5 . . ? C00K C011 H01E 109.5 . . ? H01C C011 H01E 109.5 . . ? H01D C011 H01E 109.5 . . ? O004 C012 C00X 107.31(14) . . ? O004 C012 H01F 110.3 . . ? C00X C012 H01F 110.3 . . ? O004 C012 H01G 110.3 . . ? C00X C012 H01G 110.3 . . ? H01F C012 H01G 108.5 . . ? 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 S002 2.1771(3) 3_666 ? Ni01 S002 2.1771(3) . ? Ni01 S003 2.1806(3) . ? Ni01 S003 2.1807(3) 3_666 ? S002 C00E 1.7322(13) . ? S003 C00E 1.7304(13) . ? O004 C012 1.426(2) . ? O004 C00S 1.4349(18) . ? N005 C007 1.3804(16) . ? N005 C009 1.3900(16) . ? N005 C008 1.4464(16) . ? N006 C007 1.3778(16) . ? N006 C00A 1.3902(16) . ? N006 C00B 1.4416(16) . ? C007 C00E 1.3952(18) . ? C008 C00C 1.3957(19) . ? C008 C00D 1.4011(18) . ? C009 C00A 1.3391(19) . ? C009 H009 0.9500 . ? C00A H00A 0.9500 . ? C00B C00F 1.3967(19) . ? C00B C00H 1.4006(19) . ? C00C C00J 1.3915(19) . ? C00C C00L 1.5198(18) . ? C00D C00M 1.3926(19) . ? C00D C00I 1.5189(19) . ? C00F C00P 1.396(2) . ? C00F C00K 1.516(2) . ? C00G C00J 1.382(2) . ? C00G C00M 1.383(2) . ? C00G H00G 0.9500 . ? C00H C00O 1.391(2) . ? C00H C00N 1.518(2) . ? C00I C00R 1.528(2) . ? C00I C00Y 1.529(2) . ? C00I H00I 1.0000 . ? C00J H00J 0.9500 . ? C00K C00W 1.529(2) . ? C00K C011 1.532(2) . ? C00K H00K 1.0000 . ? C00L C00Z 1.524(2) . ? C00L C00T 1.525(2) . ? C00L H00L 1.0000 . ? C00M H00M 0.9500 . ? C00N C00V 1.529(2) . ? C00N C00U 1.532(2) . ? C00N H00N 1.0000 . ? C00O C00Q 1.384(2) . ? C00O H00O 0.9500 . ? C00P C00Q 1.379(2) . ? C00P H00P 0.9500 . ? C00Q H00Q 0.9500 . ? C00R H00B 0.9800 . ? C00R H00C 0.9800 . ? C00R H00D 0.9800 . ? C00S C010 1.510(3) . ? C00S H00E 0.9900 . ? C00S H00F 0.9900 . ? C00T H00H 0.9800 . ? C00T H00R 0.9800 . ? C00T H00S 0.9800 . ? C00U H00T 0.9800 . ? C00U H00U 0.9800 . ? C00U H00V 0.9800 . ? C00V H00W 0.9800 . ? C00V H00X 0.9800 . ? C00V H00Y 0.9800 . ? C00W H00Z 0.9800 . ? C00W H010 0.9800 . ? C00W H011 0.9800 . ? C00X C012 1.526(2) . ? C00X C010 1.532(3) . ? C00X H012 0.9900 . ? C00X H013 0.9900 . ? C00Y H014 0.9800 . ? C00Y H015 0.9800 . ? C00Y H016 0.9800 . ? C00Z H017 0.9800 . ? C00Z H018 0.9800 . ? C00Z H019 0.9800 . ? C010 H01A 0.9900 . ? C010 H01B 0.9900 . ? C011 H01C 0.9800 . ? C011 H01D 0.9800 . ? C011 H01E 0.9800 . ? C012 H01F 0.9900 . ? C012 H01G 0.9900 . ?