#------------------------------------------------------------------------------ #$Date: 2025-02-12 01:08:47 +0200 (Wed, 12 Feb 2025) $ #$Revision: 297685 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/38/1573885.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_1573885 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 'C44 H48 N4 Ni S4, 3(C6 H6)' _chemical_formula_sum 'C62 H66 N4 Ni S4' _chemical_formula_weight 1054.13 _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 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 101.8330(10) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 16.39960(10) _cell_length_b 12.50180(10) _cell_length_c 14.17110(10) _cell_measurement_reflns_used 25035 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 77.3080 _cell_measurement_theta_min 2.7520 _cell_volume 2843.68(4) _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 293(2) _diffrn_detector_area_resol_mean 10.0000 _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.990 _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 0.0222 _diffrn_reflns_av_unetI/netI 0.0146 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.990 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_number 30979 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.990 _diffrn_reflns_theta_full 72.000 _diffrn_reflns_theta_max 77.398 _diffrn_reflns_theta_min 2.753 _diffrn_source 'micro-focus sealed X-ray tube' _exptl_absorpt_coefficient_mu 2.177 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.257 _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 black _exptl_crystal_density_diffrn 1.231 _exptl_crystal_description block _exptl_crystal_F_000 1116 _exptl_crystal_size_max 0.330 _exptl_crystal_size_mid 0.240 _exptl_crystal_size_min 0.210 _refine_diff_density_max 0.311 _refine_diff_density_min -0.297 _refine_diff_density_rms 0.045 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 328 _refine_ls_number_reflns 5962 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.041 _refine_ls_R_factor_all 0.0295 _refine_ls_R_factor_gt 0.0288 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0367P)^2^+1.5619P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0764 _refine_ls_wR_factor_ref 0.0768 _reflns_Friedel_coverage 0.000 _reflns_number_gt 5778 _reflns_number_total 5962 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4sc08449g2.cif _cod_data_source_block Compound_3c _cod_original_sg_symbol_H-M 'P 21/c' _cod_database_code 1573885 _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 0.534 _shelx_estimated_absorpt_t_max 0.658 _shelx_res_file ; TITL MaLu115_ref_a.res in P2(1)/c MaLu115_ref_a.res created by SHELXL-2018/3 at 17:25:37 on 17-Apr-2023 REM Old TITL MaLu115_ref in P2(1)/c REM SHELXT solution in P2(1)/c REM R1 0.086, Rweak 0.005, Alpha 0.033, Orientation as input REM Formula found by SHELXT: C62 N4 S4 Ni CELL 1.54184 16.3996 12.5018 14.1711 90.000 101.833 90.000 ZERR 2.000 0.0001 0.0001 0.0001 0.000 0.001 0.000 LATT 1 SYMM -X, 1/2+Y, 1/2-Z SFAC C H N S NI UNIT 124 132 8 8 2 SIZE 0.21 0.24 0.33 L.S. 10 BOND $H LIST 4 ACTA 144 FMAP 2 PLAN 20 WGHT 0.036700 1.561900 FVAR 0.38375 NI01 5 0.500000 0.500000 0.500000 10.50000 0.01539 0.01176 = 0.01788 0.00098 0.00630 -0.00018 S002 4 0.590037 0.604224 0.453022 11.00000 0.01451 0.01441 = 0.01939 0.00253 0.00521 0.00014 S003 4 0.417312 0.621299 0.421602 11.00000 0.01462 0.01517 = 0.02488 0.00306 0.00680 0.00009 N004 3 0.445002 0.844297 0.308379 11.00000 0.01790 0.01955 = 0.02031 0.00488 0.00559 0.00364 N005 3 0.578424 0.817002 0.316334 11.00000 0.01708 0.01701 = 0.02069 0.00388 0.00735 0.00055 C006 1 0.509312 0.775414 0.344574 11.00000 0.01514 0.01736 = 0.01603 -0.00031 0.00429 0.00054 C007 1 0.338783 0.870750 0.404798 11.00000 0.02070 0.01362 = 0.01847 0.00342 0.00313 0.00163 C008 1 0.722848 0.769778 0.391090 11.00000 0.01915 0.01692 = 0.01917 0.00018 0.00654 -0.00313 C009 1 0.654008 0.758154 0.315573 11.00000 0.01585 0.01552 = 0.01887 0.00350 0.00778 -0.00066 C00A 1 0.359493 0.837581 0.318990 11.00000 0.01609 0.01872 = 0.02083 0.00209 0.00384 0.00371 C00B 1 0.654111 0.689138 0.238057 11.00000 0.02017 0.01833 = 0.01745 0.00250 0.00631 -0.00402 C00C 1 0.725525 0.629363 0.238245 11.00000 0.02463 0.01886 = 0.02033 -0.00279 0.00888 -0.00196 AFIX 43 H00C 2 0.726469 0.581904 0.187945 11.00000 -1.20000 AFIX 0 C00D 1 0.506041 0.681600 0.397498 11.00000 0.01561 0.01535 = 0.01726 -0.00031 0.00532 0.00028 C00E 1 0.255441 0.865521 0.411904 11.00000 0.02228 0.01919 = 0.02086 0.00373 0.00747 0.00441 AFIX 43 H00E 2 0.240348 0.888427 0.468374 11.00000 -1.20000 AFIX 0 C00F 1 0.795765 0.638845 0.312020 11.00000 0.02064 0.01878 = 0.02629 0.00070 0.00833 0.00101 C00G 1 0.405127 0.906028 0.488148 11.00000 0.02553 0.02424 = 0.01946 -0.00017 0.00294 -0.00275 AFIX 137 H00A 2 0.442523 0.954281 0.465672 11.00000 -1.50000 H00B 2 0.435534 0.844753 0.517292 11.00000 -1.50000 H00D 2 0.379816 0.941644 0.534868 11.00000 -1.50000 AFIX 0 C00H 1 0.793244 0.708966 0.387338 11.00000 0.01706 0.02095 = 0.02333 0.00022 0.00261 -0.00103 AFIX 43 H00H 2 0.839985 0.715517 0.436778 11.00000 -1.20000 AFIX 0 C00I 1 0.299884 0.800515 0.241364 11.00000 0.02404 0.03664 = 0.02251 -0.00662 0.00161 0.00490 C00J 1 0.720824 0.841327 0.475597 11.00000 0.02414 0.02801 = 0.02702 -0.00889 0.00577 -0.00100 AFIX 137 H00F 2 0.725924 0.914517 0.457142 11.00000 -1.50000 H00G 2 0.766213 0.823485 0.527579 11.00000 -1.50000 H00I 2 0.669040 0.831752 0.496133 11.00000 -1.50000 AFIX 0 C00K 1 0.474163 0.925340 0.256819 11.00000 0.02666 0.02149 = 0.02358 0.00927 0.00787 0.00514 AFIX 43 H00K 2 0.442746 0.981334 0.224861 11.00000 -1.20000 AFIX 0 C00L 1 0.578682 0.679610 0.157565 11.00000 0.02445 0.02809 = 0.01899 -0.00074 0.00303 -0.00303 AFIX 137 H00J 2 0.570589 0.745462 0.122026 11.00000 -1.50000 H00L 2 0.530478 0.664883 0.184065 11.00000 -1.50000 H00M 2 0.586883 0.622411 0.115279 11.00000 -1.50000 AFIX 0 C00M 1 0.555533 0.908490 0.261324 11.00000 0.02669 0.02011 = 0.02448 0.00832 0.01075 0.00154 AFIX 43 H00N 2 0.590542 0.950501 0.232743 11.00000 -1.20000 AFIX 0 C00N 1 0.194221 0.827039 0.336979 11.00000 0.01822 0.02543 = 0.03302 0.00451 0.00462 0.00336 C00O 1 0.217757 0.795282 0.252481 11.00000 0.02063 0.04112 = 0.02974 -0.00784 -0.00423 0.00058 AFIX 43 H00O 2 0.177242 0.769704 0.201735 11.00000 -1.20000 AFIX 0 C00P 1 0.872631 0.573267 0.310354 11.00000 0.02691 0.03110 = 0.03923 -0.00364 0.00865 0.00871 AFIX 137 H00P 2 0.880000 0.566543 0.245137 11.00000 -1.50000 H00Q 2 0.866426 0.503503 0.336300 11.00000 -1.50000 H00R 2 0.920403 0.608007 0.348563 11.00000 -1.50000 AFIX 0 C00Q 1 0.108425 0.353440 0.330099 11.00000 0.02825 0.02932 = 0.03928 -0.00377 0.00361 -0.00106 AFIX 43 H00S 2 0.086664 0.290949 0.299243 11.00000 -1.20000 AFIX 0 C00R 1 0.187165 0.386277 0.324612 11.00000 0.02729 0.03843 = 0.04695 -0.00608 0.01268 0.00503 AFIX 43 H00T 2 0.218768 0.346133 0.290026 11.00000 -1.20000 AFIX 0 C00S 1 0.061497 0.413050 0.381355 11.00000 0.02484 0.04806 = 0.04420 0.00294 0.01149 0.00343 AFIX 43 H00U 2 0.008171 0.390638 0.385061 11.00000 -1.20000 AFIX 0 C00T 1 0.104529 0.819913 0.347438 11.00000 0.01833 0.04270 = 0.04839 0.00579 0.00694 0.00219 AFIX 137 H00V 2 0.072018 0.872556 0.306916 11.00000 -1.50000 H00W 2 0.101384 0.832776 0.413383 11.00000 -1.50000 H00X 2 0.083198 0.749879 0.328660 11.00000 -1.50000 AFIX 0 C00U 1 -0.068652 0.951647 0.442711 11.00000 0.03327 0.04470 = 0.05113 -0.01182 0.01420 -0.01259 AFIX 43 H00Y 2 -0.114718 0.918893 0.404403 11.00000 -1.20000 AFIX 0 C00V 1 -0.032693 1.039634 0.408584 11.00000 0.04122 0.04425 = 0.04618 -0.00405 0.01471 -0.00386 AFIX 43 H00Z 2 -0.054459 1.066503 0.347408 11.00000 -1.20000 AFIX 0 C00W 1 -0.036197 0.912389 0.533644 11.00000 0.04357 0.03887 = 0.05690 -0.00481 0.02122 -0.01493 AFIX 43 H010 2 -0.060683 0.853274 0.556433 11.00000 -1.20000 AFIX 0 C00X 1 0.093480 0.505522 0.426942 11.00000 0.04372 0.04789 = 0.03991 -0.00732 0.00817 0.01996 AFIX 43 H011 2 0.061856 0.545428 0.461678 11.00000 -1.20000 AFIX 0 C00Y 1 0.219256 0.478692 0.370373 11.00000 0.02476 0.04427 = 0.07039 -0.00674 0.00733 -0.00586 AFIX 43 H012 2 0.272794 0.500588 0.367066 11.00000 -1.20000 AFIX 0 C00Z 1 0.324519 0.763411 0.150026 11.00000 0.03653 0.09030 = 0.03074 -0.02869 0.00434 0.00384 AFIX 137 H013 2 0.276028 0.738686 0.105401 11.00000 -1.50000 H014 2 0.364068 0.706108 0.164606 11.00000 -1.50000 H015 2 0.349165 0.821787 0.121850 11.00000 -1.50000 AFIX 0 C010 1 0.172370 0.539164 0.421227 11.00000 0.04822 0.03257 = 0.05833 -0.01362 -0.00638 0.00193 AFIX 43 H01A 2 0.193888 0.602123 0.451389 11.00000 -1.20000 AFIX 0 HKLF 4 REM MaLu115_ref_a.res in P2(1)/c REM wR2 = 0.076826, GooF = S = 1.04139, Restrained GooF = 1.04139 for all data REM R1 = 0.028845 for 5778 Fo > 4sig(Fo) and 0.029528 for all 5962 data REM 328 parameters refined using 0 restraints END WGHT 0.0367 1.5619 REM Highest difference peak 0.311, deepest hole -0.297, 1-sigma level 0.045 Q1 1 0.7739 0.8801 0.5039 11.00000 0.05 0.31 Q2 1 0.4022 0.8401 0.3145 11.00000 0.05 0.30 Q3 1 0.6678 0.8851 0.4708 11.00000 0.05 0.28 Q4 1 0.5677 0.8613 0.2859 11.00000 0.05 0.25 Q5 1 0.7111 0.7878 0.5345 11.00000 0.05 0.25 Q6 1 0.5577 0.5000 0.4974 11.00000 0.05 0.25 Q7 1 0.7619 0.7530 0.3812 11.00000 0.05 0.25 Q8 1 0.3484 0.8558 0.3608 11.00000 0.05 0.24 Q9 1 0.0903 0.4429 0.4262 11.00000 0.05 0.24 Q10 1 0.3024 0.8595 0.4111 11.00000 0.05 0.24 Q11 1 0.6893 0.7555 0.3614 11.00000 0.05 0.24 Q12 1 0.7214 0.7989 0.4310 11.00000 0.05 0.23 Q13 1 0.7503 0.7267 0.3970 11.00000 0.05 0.23 Q14 1 0.1523 0.8210 0.3429 11.00000 0.05 0.23 Q15 1 0.4747 0.8097 0.3257 11.00000 0.05 0.23 Q16 1 0.2074 0.4218 0.3686 11.00000 0.05 0.23 Q17 1 0.6889 0.6693 0.2407 11.00000 0.05 0.23 Q18 1 0.5093 0.7378 0.3833 11.00000 0.05 0.22 Q19 1 0.5407 0.6555 0.4160 11.00000 0.05 0.22 Q20 1 0.6481 0.7086 0.2806 11.00000 0.05 0.22 ; _shelx_res_checksum 66481 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -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 0.01460(8) Uani 1 2 d S . P . . S002 S 0.59004(2) 0.60422(2) 0.45302(2) 0.01586(7) Uani 1 1 d . . . . . S003 S 0.41731(2) 0.62130(2) 0.42160(2) 0.01783(8) Uani 1 1 d . . . . . N004 N 0.44500(6) 0.84430(9) 0.30838(7) 0.0190(2) Uani 1 1 d . . . . . N005 N 0.57842(6) 0.81700(8) 0.31633(7) 0.0178(2) Uani 1 1 d . . . . . C006 C 0.50931(7) 0.77541(10) 0.34457(8) 0.0160(2) Uani 1 1 d . . . . . C007 C 0.33878(8) 0.87075(9) 0.40480(9) 0.0177(2) Uani 1 1 d . . . . . C008 C 0.72285(8) 0.76978(10) 0.39109(9) 0.0180(2) Uani 1 1 d . . . . . C009 C 0.65401(7) 0.75815(9) 0.31557(8) 0.0161(2) Uani 1 1 d . . . . . C00A C 0.35949(7) 0.83758(10) 0.31899(9) 0.0185(2) Uani 1 1 d . . . . . C00B C 0.65411(8) 0.68914(10) 0.23806(9) 0.0183(2) Uani 1 1 d . . . . . C00C C 0.72552(8) 0.62936(10) 0.23825(9) 0.0207(2) Uani 1 1 d . . . . . H00C H 0.726469 0.581904 0.187945 0.025 Uiso 1 1 calc R U . . . C00D C 0.50604(7) 0.68160(9) 0.39750(8) 0.0158(2) Uani 1 1 d . . . . . C00E C 0.25544(8) 0.86552(10) 0.41190(9) 0.0203(2) Uani 1 1 d . . . . . H00E H 0.240348 0.888427 0.468374 0.024 Uiso 1 1 calc R U . . . C00F C 0.79576(8) 0.63885(10) 0.31202(9) 0.0214(3) Uani 1 1 d . . . . . C00G C 0.40513(8) 0.90603(11) 0.48815(9) 0.0233(3) Uani 1 1 d . . . . . H00A H 0.442523 0.954281 0.465672 0.035 Uiso 1 1 calc R U . . . H00B H 0.435534 0.844753 0.517292 0.035 Uiso 1 1 calc R U . . . H00D H 0.379816 0.941644 0.534868 0.035 Uiso 1 1 calc R U . . . C00H C 0.79324(8) 0.70897(10) 0.38734(9) 0.0207(2) Uani 1 1 d . . . . . H00H H 0.839985 0.715517 0.436778 0.025 Uiso 1 1 calc R U . . . C00I C 0.29988(9) 0.80051(12) 0.24136(10) 0.0282(3) Uani 1 1 d . . . . . C00J C 0.72082(8) 0.84133(12) 0.47560(10) 0.0263(3) Uani 1 1 d . . . . . H00F H 0.725924 0.914517 0.457142 0.039 Uiso 1 1 calc R U . . . H00G H 0.766213 0.823485 0.527579 0.039 Uiso 1 1 calc R U . . . H00I H 0.669040 0.831752 0.496133 0.039 Uiso 1 1 calc R U . . . C00K C 0.47416(8) 0.92534(11) 0.25682(9) 0.0235(3) Uani 1 1 d . . . . . H00K H 0.442746 0.981334 0.224861 0.028 Uiso 1 1 calc R U . . . C00L C 0.57868(8) 0.67961(11) 0.15756(9) 0.0240(3) Uani 1 1 d . . . . . H00J H 0.570589 0.745462 0.122026 0.036 Uiso 1 1 calc R U . . . H00L H 0.530478 0.664883 0.184065 0.036 Uiso 1 1 calc R U . . . H00M H 0.586883 0.622411 0.115279 0.036 Uiso 1 1 calc R U . . . C00M C 0.55553(8) 0.90849(11) 0.26132(9) 0.0230(3) Uani 1 1 d . . . . . H00N H 0.590542 0.950501 0.232743 0.028 Uiso 1 1 calc R U . . . C00N C 0.19422(8) 0.82704(11) 0.33698(10) 0.0256(3) Uani 1 1 d . . . . . C00O C 0.21776(9) 0.79528(13) 0.25248(11) 0.0318(3) Uani 1 1 d . . . . . H00O H 0.177242 0.769704 0.201735 0.038 Uiso 1 1 calc R U . . . C00P C 0.87263(9) 0.57327(13) 0.31035(11) 0.0321(3) Uani 1 1 d . . . . . H00P H 0.880000 0.566543 0.245137 0.048 Uiso 1 1 calc R U . . . H00Q H 0.866426 0.503503 0.336300 0.048 Uiso 1 1 calc R U . . . H00R H 0.920403 0.608007 0.348563 0.048 Uiso 1 1 calc R U . . . C00Q C 0.10842(9) 0.35344(13) 0.33010(12) 0.0328(3) Uani 1 1 d . . . . . H00S H 0.086664 0.290949 0.299243 0.039 Uiso 1 1 calc R U . . . C00R C 0.18716(10) 0.38628(14) 0.32461(13) 0.0368(4) Uani 1 1 d . . . . . H00T H 0.218768 0.346133 0.290026 0.044 Uiso 1 1 calc R U . . . C00S C 0.06150(10) 0.41305(15) 0.38135(12) 0.0384(4) Uani 1 1 d . . . . . H00U H 0.008171 0.390638 0.385061 0.046 Uiso 1 1 calc R U . . . C00T C 0.10453(9) 0.81991(14) 0.34744(13) 0.0365(3) Uani 1 1 d . . . . . H00V H 0.072018 0.872556 0.306916 0.055 Uiso 1 1 calc R U . . . H00W H 0.101384 0.832776 0.413383 0.055 Uiso 1 1 calc R U . . . H00X H 0.083198 0.749879 0.328660 0.055 Uiso 1 1 calc R U . . . C00U C -0.06865(11) 0.95165(15) 0.44271(13) 0.0422(4) Uani 1 1 d . . . . . H00Y H -0.114718 0.918893 0.404403 0.051 Uiso 1 1 calc R U . . . C00V C -0.03269(11) 1.03963(15) 0.40858(14) 0.0431(4) Uani 1 1 d . . . . . H00Z H -0.054459 1.066503 0.347408 0.052 Uiso 1 1 calc R U . . . C00W C -0.03620(11) 0.91239(15) 0.53364(14) 0.0449(4) Uani 1 1 d . . . . . H010 H -0.060683 0.853274 0.556433 0.054 Uiso 1 1 calc R U . . . C00X C 0.09348(11) 0.50552(15) 0.42694(13) 0.0439(4) Uani 1 1 d . . . . . H011 H 0.061856 0.545428 0.461678 0.053 Uiso 1 1 calc R U . . . C00Y C 0.21926(10) 0.47869(15) 0.37037(15) 0.0468(4) Uani 1 1 d . . . . . H012 H 0.272794 0.500588 0.367066 0.056 Uiso 1 1 calc R U . . . C00Z C 0.32452(11) 0.7634(2) 0.15003(12) 0.0529(5) Uani 1 1 d . . . . . H013 H 0.276028 0.738686 0.105401 0.079 Uiso 1 1 calc R U . . . H014 H 0.364068 0.706108 0.164606 0.079 Uiso 1 1 calc R U . . . H015 H 0.349165 0.821787 0.121850 0.079 Uiso 1 1 calc R U . . . C010 C 0.17237(12) 0.53916(15) 0.42123(15) 0.0488(5) Uani 1 1 d . . . . . H01A H 0.193888 0.602123 0.451389 0.059 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 0.01539(14) 0.01176(14) 0.01788(15) 0.00098(10) 0.00630(11) -0.00018(10) S002 0.01451(13) 0.01441(14) 0.01939(14) 0.00253(10) 0.00521(10) 0.00014(10) S003 0.01462(14) 0.01517(14) 0.02488(15) 0.00306(10) 0.00680(11) 0.00009(10) N004 0.0179(5) 0.0196(5) 0.0203(5) 0.0049(4) 0.0056(4) 0.0036(4) N005 0.0171(5) 0.0170(5) 0.0207(5) 0.0039(4) 0.0073(4) 0.0006(4) C006 0.0151(5) 0.0174(6) 0.0160(5) -0.0003(4) 0.0043(4) 0.0005(4) C007 0.0207(6) 0.0136(5) 0.0185(6) 0.0034(4) 0.0031(5) 0.0016(4) C008 0.0191(6) 0.0169(6) 0.0192(6) 0.0002(4) 0.0065(4) -0.0031(4) C009 0.0158(5) 0.0155(5) 0.0189(5) 0.0035(4) 0.0078(4) -0.0007(4) C00A 0.0161(5) 0.0187(6) 0.0208(6) 0.0021(5) 0.0038(4) 0.0037(4) C00B 0.0202(6) 0.0183(6) 0.0175(5) 0.0025(4) 0.0063(4) -0.0040(5) C00C 0.0246(6) 0.0189(6) 0.0203(6) -0.0028(5) 0.0089(5) -0.0020(5) C00D 0.0156(5) 0.0154(5) 0.0173(5) -0.0003(4) 0.0053(4) 0.0003(4) C00E 0.0223(6) 0.0192(6) 0.0209(6) 0.0037(5) 0.0075(5) 0.0044(5) C00F 0.0206(6) 0.0188(6) 0.0263(6) 0.0007(5) 0.0083(5) 0.0010(5) C00G 0.0255(6) 0.0242(6) 0.0195(6) -0.0002(5) 0.0029(5) -0.0027(5) C00H 0.0171(6) 0.0209(6) 0.0233(6) 0.0002(5) 0.0026(5) -0.0010(5) C00I 0.0240(7) 0.0366(8) 0.0225(6) -0.0066(6) 0.0016(5) 0.0049(6) C00J 0.0241(6) 0.0280(7) 0.0270(7) -0.0089(5) 0.0058(5) -0.0010(5) C00K 0.0267(6) 0.0215(6) 0.0236(6) 0.0093(5) 0.0079(5) 0.0051(5) C00L 0.0245(6) 0.0281(7) 0.0190(6) -0.0007(5) 0.0030(5) -0.0030(5) C00M 0.0267(6) 0.0201(6) 0.0245(6) 0.0083(5) 0.0108(5) 0.0015(5) C00N 0.0182(6) 0.0254(7) 0.0330(7) 0.0045(5) 0.0046(5) 0.0034(5) C00O 0.0206(6) 0.0411(8) 0.0297(7) -0.0078(6) -0.0042(5) 0.0006(6) C00P 0.0269(7) 0.0311(8) 0.0392(8) -0.0036(6) 0.0086(6) 0.0087(6) C00Q 0.0283(7) 0.0293(7) 0.0393(8) -0.0038(6) 0.0036(6) -0.0011(6) C00R 0.0273(7) 0.0384(9) 0.0469(9) -0.0061(7) 0.0127(7) 0.0050(6) C00S 0.0248(7) 0.0481(10) 0.0442(9) 0.0029(7) 0.0115(6) 0.0034(7) C00T 0.0183(7) 0.0427(9) 0.0484(9) 0.0058(7) 0.0069(6) 0.0022(6) C00U 0.0333(8) 0.0447(10) 0.0511(10) -0.0118(8) 0.0142(7) -0.0126(7) C00V 0.0412(9) 0.0442(10) 0.0462(9) -0.0040(8) 0.0147(7) -0.0039(8) C00W 0.0436(9) 0.0389(9) 0.0569(11) -0.0048(8) 0.0212(8) -0.0149(8) C00X 0.0437(9) 0.0479(10) 0.0399(9) -0.0073(7) 0.0082(7) 0.0200(8) C00Y 0.0248(7) 0.0443(10) 0.0704(12) -0.0067(9) 0.0073(8) -0.0059(7) C00Z 0.0365(9) 0.0903(16) 0.0307(8) -0.0287(9) 0.0043(7) 0.0038(9) C010 0.0482(10) 0.0326(9) 0.0583(11) -0.0136(8) -0.0064(8) 0.0019(8) 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' 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 79.490(10) . . ? S002 Ni01 S003 100.511(10) 3_666 . ? S002 Ni01 S003 100.510(10) . 3_666 ? S002 Ni01 S003 79.489(10) 3_666 3_666 ? S003 Ni01 S003 180.0 . 3_666 ? C00D S002 Ni01 86.97(4) . . ? C00D S003 Ni01 86.76(4) . . ? C006 N004 C00K 109.39(10) . . ? C006 N004 C00A 127.69(10) . . ? C00K N004 C00A 122.93(10) . . ? C006 N005 C00M 109.21(10) . . ? C006 N005 C009 124.63(10) . . ? C00M N005 C009 123.24(10) . . ? N004 C006 N005 105.58(10) . . ? N004 C006 C00D 127.84(11) . . ? N005 C006 C00D 126.57(11) . . ? C00A C007 C00E 117.93(11) . . ? C00A C007 C00G 120.58(11) . . ? C00E C007 C00G 121.43(11) . . ? C00H C008 C009 117.44(11) . . ? C00H C008 C00J 120.67(11) . . ? C009 C008 C00J 121.84(11) . . ? C008 C009 C00B 122.43(11) . . ? C008 C009 N005 120.16(11) . . ? C00B C009 N005 117.40(11) . . ? C007 C00A C00I 122.14(12) . . ? C007 C00A N004 119.36(11) . . ? C00I C00A N004 118.47(11) . . ? C00C C00B C009 117.89(11) . . ? C00C C00B C00L 121.36(11) . . ? C009 C00B C00L 120.75(11) . . ? C00B C00C C00F 121.53(12) . . ? C00B C00C H00C 119.2 . . ? C00F C00C H00C 119.2 . . ? C006 C00D S003 126.59(9) . . ? C006 C00D S002 126.63(9) . . ? S003 C00D S002 106.78(6) . . ? C00N C00E C007 121.82(12) . . ? C00N C00E H00E 119.1 . . ? C007 C00E H00E 119.1 . . ? C00H C00F C00C 118.71(12) . . ? C00H C00F C00P 120.80(12) . . ? C00C C00F C00P 120.48(12) . . ? C007 C00G H00A 109.5 . . ? C007 C00G H00B 109.5 . . ? H00A C00G H00B 109.5 . . ? C007 C00G H00D 109.5 . . ? H00A C00G H00D 109.5 . . ? H00B C00G H00D 109.5 . . ? C00F C00H C008 121.99(12) . . ? C00F C00H H00H 119.0 . . ? C008 C00H H00H 119.0 . . ? C00O C00I C00A 117.77(12) . . ? C00O C00I C00Z 121.34(13) . . ? C00A C00I C00Z 120.85(13) . . ? C008 C00J H00F 109.5 . . ? C008 C00J H00G 109.5 . . ? H00F C00J H00G 109.5 . . ? C008 C00J H00I 109.5 . . ? H00F C00J H00I 109.5 . . ? H00G C00J H00I 109.5 . . ? C00M C00K N004 107.88(11) . . ? C00M C00K H00K 126.1 . . ? N004 C00K H00K 126.1 . . ? C00B C00L H00J 109.5 . . ? C00B C00L H00L 109.5 . . ? H00J C00L H00L 109.5 . . ? C00B C00L H00M 109.5 . . ? H00J C00L H00M 109.5 . . ? H00L C00L H00M 109.5 . . ? C00K C00M N005 107.92(11) . . ? C00K C00M H00N 126.0 . . ? N005 C00M H00N 126.0 . . ? C00E C00N C00O 118.21(12) . . ? C00E C00N C00T 120.73(13) . . ? C00O C00N C00T 121.05(13) . . ? C00N C00O C00I 122.10(13) . . ? C00N C00O H00O 118.9 . . ? C00I C00O H00O 118.9 . . ? C00F C00P H00P 109.5 . . ? C00F C00P H00Q 109.5 . . ? H00P C00P H00Q 109.5 . . ? C00F C00P H00R 109.5 . . ? H00P C00P H00R 109.5 . . ? H00Q C00P H00R 109.5 . . ? C00R C00Q C00S 120.07(15) . . ? C00R C00Q H00S 120.0 . . ? C00S C00Q H00S 120.0 . . ? C00Q C00R C00Y 119.87(15) . . ? C00Q C00R H00T 120.1 . . ? C00Y C00R H00T 120.1 . . ? C00X C00S C00Q 120.08(15) . . ? C00X C00S H00U 120.0 . . ? C00Q C00S H00U 120.0 . . ? C00N C00T H00V 109.5 . . ? C00N C00T H00W 109.5 . . ? H00V C00T H00W 109.5 . . ? C00N C00T H00X 109.5 . . ? H00V C00T H00X 109.5 . . ? H00W C00T H00X 109.5 . . ? C00W C00U C00V 119.97(16) . . ? C00W C00U H00Y 120.0 . . ? C00V C00U H00Y 120.0 . . ? C00U C00V C00W 119.46(18) . 3_576 ? C00U C00V H00Z 120.3 . . ? C00W C00V H00Z 120.3 3_576 . ? C00U C00W C00V 120.57(17) . 3_576 ? C00U C00W H010 119.7 . . ? C00V C00W H010 119.7 3_576 . ? C00S C00X C010 120.08(16) . . ? C00S C00X H011 120.0 . . ? C010 C00X H011 120.0 . . ? C00R C00Y C010 120.36(16) . . ? C00R C00Y H012 119.8 . . ? C010 C00Y H012 119.8 . . ? C00I C00Z H013 109.5 . . ? C00I C00Z H014 109.5 . . ? H013 C00Z H014 109.5 . . ? C00I C00Z H015 109.5 . . ? H013 C00Z H015 109.5 . . ? H014 C00Z H015 109.5 . . ? C00X C010 C00Y 119.54(16) . . ? C00X C010 H01A 120.2 . . ? C00Y C010 H01A 120.2 . . ? 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 2.1736(3) . ? Ni01 S002 2.1736(3) 3_666 ? Ni01 S003 2.1806(3) . ? Ni01 S003 2.1806(3) 3_666 ? S002 C00D 1.7343(12) . ? S003 C00D 1.7338(12) . ? N004 C006 1.3766(15) . ? N004 C00K 1.3901(16) . ? N004 C00A 1.4431(15) . ? N005 C006 1.3788(15) . ? N005 C00M 1.3917(16) . ? N005 C009 1.4434(15) . ? C006 C00D 1.3991(16) . ? C007 C00A 1.3912(17) . ? C007 C00E 1.3925(17) . ? C007 C00G 1.4988(17) . ? C008 C00H 1.3924(17) . ? C008 C009 1.3948(17) . ? C008 C00J 1.5005(17) . ? C009 C00B 1.3971(17) . ? C00A C00I 1.3926(18) . ? C00B C00C 1.3888(18) . ? C00B C00L 1.5056(17) . ? C00C C00F 1.3929(18) . ? C00C H00C 0.9300 . ? C00E C00N 1.3891(19) . ? C00E H00E 0.9300 . ? C00F C00H 1.3883(18) . ? C00F C00P 1.5080(18) . ? C00G H00A 0.9600 . ? C00G H00B 0.9600 . ? C00G H00D 0.9600 . ? C00H H00H 0.9300 . ? C00I C00O 1.389(2) . ? C00I C00Z 1.506(2) . ? C00J H00F 0.9600 . ? C00J H00G 0.9600 . ? C00J H00I 0.9600 . ? C00K C00M 1.3395(19) . ? C00K H00K 0.9300 . ? C00L H00J 0.9600 . ? C00L H00L 0.9600 . ? C00L H00M 0.9600 . ? C00M H00N 0.9300 . ? C00N C00O 1.389(2) . ? C00N C00T 1.5109(18) . ? C00O H00O 0.9300 . ? C00P H00P 0.9600 . ? C00P H00Q 0.9600 . ? C00P H00R 0.9600 . ? C00Q C00R 1.372(2) . ? C00Q C00S 1.380(2) . ? C00Q H00S 0.9300 . ? C00R C00Y 1.376(2) . ? C00R H00T 0.9300 . ? C00S C00X 1.375(3) . ? C00S H00U 0.9300 . ? C00T H00V 0.9600 . ? C00T H00W 0.9600 . ? C00T H00X 0.9600 . ? C00U C00W 1.380(3) . ? C00U C00V 1.382(3) . ? C00U H00Y 0.9300 . ? C00V C00W 1.388(3) 3_576 ? C00V H00Z 0.9300 . ? C00W H010 0.9300 . ? C00X C010 1.378(3) . ? C00X H011 0.9300 . ? C00Y C010 1.382(3) . ? C00Y H012 0.9300 . ? C00Z H013 0.9600 . ? C00Z H014 0.9600 . ? C00Z H015 0.9600 . ? C010 H01A 0.9300 . ?