#------------------------------------------------------------------------------ #$Date: 2020-05-07 00:15:04 +0300 (Thu, 07 May 2020) $ #$Revision: 251826 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/24/04/7240457.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_7240457 loop_ _publ_author_name 'Hachem, Hadi' 'Jeannin, olivier' 'Fourmigue, Marc' 'Barriere, Frederic' 'Lorcy, Dominique' _publ_section_title ; Halogen bonded metal bis(dithiolene) 2D frameworks ; _journal_name_full CrystEngComm _journal_paper_doi 10.1039/D0CE00512F _journal_year 2020 _chemical_formula_moiety 'C6 I2 N2 Ni S6, C16 H36 N' _chemical_formula_sum 'C22 H36 I2 N3 Ni S6' _chemical_formula_weight 847.41 _space_group_IT_number 15 _space_group_name_Hall '-C 2yc' _space_group_name_H-M_alt 'C 1 2/c 1' _symmetry_cell_setting monoclinic _symmetry_Int_Tables_number 15 _symmetry_space_group_name_Hall '-C 2yc' _symmetry_space_group_name_H-M 'C 1 2/c 1' _atom_sites_solution_hydrogens geom _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.4.3 _audit_creation_date 2019-04-29T15:31:22-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_update_record ; 2020-04-02 deposited with the CCDC. 2020-05-06 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 92.452(6) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 15.9488(17) _cell_length_b 12.5276(12) _cell_length_c 16.2505(18) _cell_measurement_reflns_used 2488 _cell_measurement_temperature 296(2) _cell_measurement_theta_max 26.26 _cell_measurement_theta_min 2.39 _cell_measurement_wavelength 0.71073 _cell_volume 3243.9(6) _computing_cell_refinement 'Bruker APEX2 (Bruker, 2014)' _computing_data_collection 'Bruker APEX2 (Bruker, 2014)' _computing_data_reduction 'Bruker APEX2 (Bruker, 2014)' _computing_molecular_graphics 'Ortep for Windows (Farrugia, 2012)' _computing_publication_material 'WinGX publication routines (Farrugia, 2012)' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _diffrn_ambient_temperature 296(2) _diffrn_detector 'CCD plate' _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.988 _diffrn_measurement_device_type 'APEXII, Bruker-AXS' _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_orient_matrix_UB_11 -0.015896 _diffrn_orient_matrix_UB_12 -0.006296 _diffrn_orient_matrix_UB_13 -0.059999 _diffrn_orient_matrix_UB_21 0.053116 _diffrn_orient_matrix_UB_22 0.037089 _diffrn_orient_matrix_UB_23 -0.01379 _diffrn_orient_matrix_UB_31 0.029404 _diffrn_orient_matrix_UB_32 -0.070403 _diffrn_orient_matrix_UB_33 -0.001899 _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0593 _diffrn_reflns_av_unetI/netI 0.0913 _diffrn_reflns_Laue_measured_fraction_full 0.997 _diffrn_reflns_Laue_measured_fraction_max 0.988 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_number 10918 _diffrn_reflns_point_group_measured_fraction_full 0.997 _diffrn_reflns_point_group_measured_fraction_max 0.988 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.447 _diffrn_reflns_theta_min 2.447 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 2.905 _exptl_absorpt_correction_T_max 0.748 _exptl_absorpt_correction_T_min 0.688 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [Sheldrick, G.M. (2014). SADABS Bruker AXS Inc., Madison, Wisconsin, USA] ; _exptl_crystal_colour black _exptl_crystal_density_diffrn 1.735 _exptl_crystal_density_method 'not measured' _exptl_crystal_description prism _exptl_crystal_F_000 1676 _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.10 _refine_diff_density_max 0.923 _refine_diff_density_min -0.525 _refine_diff_density_rms 0.118 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.983 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_constraints 0 _refine_ls_number_parameters 184 _refine_ls_number_reflns 3668 _refine_ls_number_restraints 64 _refine_ls_restrained_S_all 0.981 _refine_ls_R_factor_all 0.1443 _refine_ls_R_factor_gt 0.0562 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0788P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1314 _refine_ls_wR_factor_ref 0.1621 _reflns_Friedel_coverage 0 _reflns_number_gt 1765 _reflns_number_total 3668 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d0ce00512f2.cif _cod_data_source_block trans-Ni _cod_original_sg_symbol_H-M 'C 2/c' _cod_database_code 7240457 _shelx_res_file ; shelx.res created by SHELXL-2014/7 TITL SIR97 run in space group C 2/c CELL 0.71073 15.9488 12.5276 16.2505 90.000 92.452 90.000 ZERR 4.00 0.0017 0.0012 0.0018 0.000 0.006 0.000 LATT 7 SYMM - X, Y, 1/2 - Z SFAC C H N S I NI UNIT 88 144 12 24 8 4 MERG 2 OMIT 1 1 0 DFIX 1.500 0.020 C11 C10 DFIX 1.500 0.020 C10B C11B DFIX 1.500 0.020 C10B C9B DFIX 1.500 0.020 C9B C8 EXYZ C8 C8A EADP C8 C8A DELU 0.0050 0.0050 C9 C10 C11 C9B C10B C11B SIMU 0.020 0.040 1.700 C9 C10 C11 C9B C10B C11B FMAP 2 PLAN 25 ACTA BOND $H CONF L.S. 10 TEMP 23.00 WGHT 0.078800 FVAR 0.16132 0.59790 C1 1 0.654569 0.410756 0.099350 11.00000 0.05729 0.05504 = 0.04603 -0.00085 0.00538 -0.01819 C2 1 0.735381 0.437844 0.116616 11.00000 0.05870 0.04457 = 0.04124 -0.00057 0.00117 -0.01168 C3 1 0.677816 0.555527 0.196215 11.00000 0.07357 0.04734 = 0.05757 -0.01377 0.01248 -0.01124 C4 1 0.923004 0.682241 0.230610 11.00000 0.05687 0.07229 = 0.07914 0.00200 -0.00446 -0.00967 AFIX 23 H4A 2 0.877748 0.633613 0.214981 11.00000 -1.20000 H4B 2 0.907482 0.718432 0.280485 11.00000 -1.20000 AFIX 0 C5 1 0.929425 0.763462 0.164306 11.00000 0.07901 0.08720 = 0.08067 0.01901 0.00838 -0.00246 AFIX 23 H5A 2 0.951817 0.729200 0.116428 11.00000 -1.20000 H5B 2 0.969320 0.817660 0.182924 11.00000 -1.20000 AFIX 0 C6 1 0.848391 0.817402 0.138519 11.00000 0.07349 0.09640 = 0.09483 0.01952 -0.00565 0.01475 AFIX 23 H6A 2 0.807673 0.763143 0.122000 11.00000 -1.20000 H6B 2 0.827174 0.854467 0.185729 11.00000 -1.20000 AFIX 0 C7 1 0.855176 0.894632 0.070154 11.00000 0.10649 0.10242 = 0.12213 0.04518 -0.01133 0.01809 AFIX 33 H7A 2 0.801126 0.925573 0.057299 11.00000 -1.50000 H7B 2 0.894166 0.949925 0.086328 11.00000 -1.50000 H7C 2 0.874637 0.858470 0.022508 11.00000 -1.50000 AFIX 0 PART 1 C8 1 0.983875 0.545634 0.325731 21.00000 0.09208 0.08133 = 0.07328 0.00407 -0.01399 -0.00959 AFIX 23 H8A 2 1.034876 0.505569 0.338270 21.00000 -1.20000 H8B 2 0.975212 0.592103 0.372351 21.00000 -1.20000 AFIX 0 C9 1 0.911987 0.466969 0.320573 21.00000 0.13453 0.12241 = 0.11447 0.06467 0.03328 -0.03283 AFIX 23 H9A 2 0.923158 0.414910 0.278236 21.00000 -1.20000 H9B 2 0.861327 0.505062 0.303179 21.00000 -1.20000 AFIX 0 C10 1 0.895331 0.406891 0.400799 21.00000 0.13995 0.12454 = 0.13848 0.09526 0.02045 -0.02282 AFIX 23 H10A 2 0.900369 0.455289 0.447341 21.00000 -1.20000 H10B 2 0.839024 0.377464 0.398289 21.00000 -1.20000 AFIX 0 C11 1 0.955908 0.322737 0.410215 21.00000 0.12294 0.17223 = 0.19267 0.09210 -0.01277 -0.00634 AFIX 33 H11A 2 0.946642 0.284106 0.460029 21.00000 -1.50000 H11B 2 0.950266 0.275114 0.364027 21.00000 -1.50000 H11C 2 1.011377 0.352643 0.412892 21.00000 -1.50000 AFIX 0 PART 2 C8A 1 0.983875 0.545634 0.325731 -21.00000 0.09208 0.08133 = 0.07328 0.00407 -0.01399 -0.00959 AFIX 23 H8AA 2 1.036625 0.521856 0.351431 -21.00000 -1.20000 H8AB 2 0.952921 0.584510 0.366188 -21.00000 -1.20000 AFIX 0 C9B 1 0.934100 0.452682 0.293834 -21.00000 0.14838 0.12729 = 0.13305 0.06893 0.00819 -0.02767 AFIX 23 H9B1 2 0.896601 0.471173 0.247452 -21.00000 -1.20000 H9B2 2 0.969072 0.392574 0.279812 -21.00000 -1.20000 AFIX 0 C10B 1 0.889076 0.434943 0.370688 -21.00000 0.14188 0.14072 = 0.13648 0.06684 0.01023 -0.03171 AFIX 23 H10C 2 0.879083 0.506690 0.390462 -21.00000 -1.20000 H10D 2 0.834552 0.408911 0.351022 -21.00000 -1.20000 AFIX 0 C11B 1 0.906188 0.373432 0.447044 -21.00000 0.16314 0.17478 = 0.12927 0.06904 0.03596 0.03340 AFIX 33 H11D 2 0.860573 0.382502 0.483083 -21.00000 -1.50000 H11E 2 0.911919 0.299181 0.433801 -21.00000 -1.50000 H11F 2 0.957201 0.398610 0.473907 -21.00000 -1.50000 AFIX 0 PART 0 N1 3 0.748859 0.521972 0.171281 11.00000 0.06252 0.05547 = 0.05908 -0.01043 0.00151 -0.01390 N6 3 1.000000 0.617980 0.250000 10.50000 0.05946 0.05394 = 0.05992 0.00000 -0.02011 0.00000 S1 4 0.627296 0.306480 0.034750 11.00000 0.05501 0.07137 = 0.06462 -0.02086 0.00855 -0.01696 S2 4 0.817082 0.371905 0.070814 11.00000 0.05350 0.05947 = 0.06465 -0.01008 0.00461 -0.01508 S3 4 0.589891 0.492668 0.153970 11.00000 0.06179 0.07473 = 0.08048 -0.01971 0.01367 -0.00979 I1 5 0.668920 0.671621 0.287485 11.00000 0.09369 0.07108 = 0.08340 -0.02405 0.01747 -0.00873 NI1 6 0.750000 0.250000 0.000000 10.50000 0.05254 0.05128 = 0.04072 -0.00282 0.00630 -0.01465 HKLF 4 REM SIR97 run in space group C 2/c REM R1 = 0.0562 for 1765 Fo > 4sig(Fo) and 0.1443 for all 3668 data REM 184 parameters refined using 64 restraints END WGHT 0.0788 0.0000 REM Highest difference peak 0.923, deepest hole -0.525, 1-sigma level 0.118 Q1 1 0.6838 0.6064 0.3200 11.00000 0.05 0.92 Q2 1 0.5964 0.6737 0.2815 11.00000 0.05 0.68 Q3 1 0.6185 0.6766 0.2333 11.00000 0.05 0.68 Q4 1 0.9259 0.3617 0.3630 11.00000 0.05 0.62 Q5 1 0.6737 0.6375 0.2289 11.00000 0.05 0.60 Q6 1 0.7989 0.2551 -0.0014 11.00000 0.05 0.58 Q7 1 0.7193 0.2865 0.0349 11.00000 0.05 0.54 Q8 1 0.7480 0.2194 0.0317 11.00000 0.05 0.46 Q9 1 0.9432 0.4287 0.4246 11.00000 0.05 0.45 Q10 1 1.0000 0.6712 0.2500 10.50000 0.05 0.44 Q11 1 0.9091 0.2532 0.4258 11.00000 0.05 0.43 Q12 1 0.9541 0.7777 0.1436 11.00000 0.05 0.42 Q13 1 0.7785 0.3150 0.0317 11.00000 0.05 0.42 Q14 1 0.8693 0.3225 0.4010 11.00000 0.05 0.42 Q15 1 0.8884 0.7823 0.2056 11.00000 0.05 0.41 Q16 1 1.0647 0.6162 0.2138 11.00000 0.05 0.40 Q17 1 0.6306 0.3645 0.0518 11.00000 0.05 0.40 Q18 1 0.9038 0.3992 0.4286 11.00000 0.05 0.37 Q19 1 0.9065 0.5405 0.3699 11.00000 0.05 0.37 Q20 1 0.6893 0.7001 0.2233 11.00000 0.05 0.37 Q21 1 0.9292 0.4569 0.4597 11.00000 0.05 0.36 Q22 1 0.5691 0.5009 0.1508 11.00000 0.05 0.35 Q23 1 0.8054 0.3499 0.1171 11.00000 0.05 0.35 Q24 1 0.8855 0.4743 0.3337 11.00000 0.05 0.34 Q25 1 0.6294 0.5479 0.1525 11.00000 0.05 0.34 ; _shelx_res_checksum 69898 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -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 C1 C 0.6546(4) 0.4108(5) 0.0994(4) 0.0527(18) Uani 1 1 d . . . . . C2 C 0.7354(5) 0.4378(5) 0.1166(4) 0.0482(17) Uani 1 1 d . . . . . C3 C 0.6778(5) 0.5555(5) 0.1962(4) 0.059(2) Uani 1 1 d . . . . . C4 C 0.9230(5) 0.6822(6) 0.2306(5) 0.070(2) Uani 1 1 d . . . . . H4A H 0.8777 0.6336 0.215 0.084 Uiso 1 1 calc R U . . . H4B H 0.9075 0.7184 0.2805 0.084 Uiso 1 1 calc R U . . . C5 C 0.9294(6) 0.7635(7) 0.1643(5) 0.082(3) Uani 1 1 d . . . . . H5A H 0.9518 0.7292 0.1164 0.099 Uiso 1 1 calc R U . . . H5B H 0.9693 0.8177 0.1829 0.099 Uiso 1 1 calc R U . . . C6 C 0.8484(6) 0.8174(7) 0.1385(6) 0.089(3) Uani 1 1 d . . . . . H6A H 0.8077 0.7631 0.122 0.106 Uiso 1 1 calc R U . . . H6B H 0.8272 0.8545 0.1857 0.106 Uiso 1 1 calc R U . . . C7 C 0.8552(6) 0.8946(8) 0.0702(7) 0.111(3) Uani 1 1 d . . . . . H7A H 0.8011 0.9256 0.0573 0.166 Uiso 1 1 calc R U . . . H7B H 0.8942 0.9499 0.0863 0.166 Uiso 1 1 calc R U . . . H7C H 0.8746 0.8585 0.0225 0.166 Uiso 1 1 calc R U . . . C8 C 0.9839(6) 0.5456(7) 0.3257(5) 0.083(3) Uani 0.60(2) 1 d D . P A 1 H8A H 1.0349 0.5056 0.3383 0.099 Uiso 0.60(2) 1 calc R U P A 1 H8B H 0.9752 0.5921 0.3724 0.099 Uiso 0.60(2) 1 calc R U P A 1 C9 C 0.9120(18) 0.467(2) 0.3206(16) 0.123(6) Uani 0.60(2) 1 d . U P A 1 H9A H 0.9232 0.4149 0.2782 0.148 Uiso 0.60(2) 1 calc R U P A 1 H9B H 0.8613 0.5051 0.3032 0.148 Uiso 0.60(2) 1 calc R U P A 1 C10 C 0.8953(16) 0.4069(18) 0.4008(18) 0.134(6) Uani 0.60(2) 1 d D U P A 1 H10A H 0.9004 0.4553 0.4473 0.161 Uiso 0.60(2) 1 calc R U P A 1 H10B H 0.839 0.3775 0.3983 0.161 Uiso 0.60(2) 1 calc R U P A 1 C11 C 0.9559(16) 0.3227(19) 0.410(2) 0.163(9) Uani 0.60(2) 1 d D U P A 1 H11A H 0.9466 0.2841 0.46 0.245 Uiso 0.60(2) 1 calc R U P A 1 H11B H 0.9503 0.2751 0.364 0.245 Uiso 0.60(2) 1 calc R U P A 1 H11C H 1.0114 0.3526 0.4129 0.245 Uiso 0.60(2) 1 calc R U P A 1 C8A C 0.9839(6) 0.5456(7) 0.3257(5) 0.083(3) Uani 0.40(2) 1 d . . P A 2 H8AA H 1.0366 0.5219 0.3514 0.099 Uiso 0.40(2) 1 calc R U P A 2 H8AB H 0.9529 0.5845 0.3662 0.099 Uiso 0.40(2) 1 calc R U P A 2 C9B C 0.934(3) 0.453(3) 0.294(2) 0.136(8) Uani 0.40(2) 1 d D U P A 2 H9B1 H 0.8966 0.4712 0.2475 0.163 Uiso 0.40(2) 1 calc R U P A 2 H9B2 H 0.9691 0.3926 0.2798 0.163 Uiso 0.40(2) 1 calc R U P A 2 C10B C 0.889(3) 0.435(3) 0.371(2) 0.140(7) Uani 0.40(2) 1 d D U P A 2 H10C H 0.8791 0.5067 0.3905 0.167 Uiso 0.40(2) 1 calc R U P A 2 H10D H 0.8346 0.4089 0.351 0.167 Uiso 0.40(2) 1 calc R U P A 2 C11B C 0.906(3) 0.373(4) 0.447(2) 0.155(10) Uani 0.40(2) 1 d D U P A 2 H11D H 0.8606 0.3825 0.4831 0.232 Uiso 0.40(2) 1 calc R U P A 2 H11E H 0.9119 0.2992 0.4338 0.232 Uiso 0.40(2) 1 calc R U P A 2 H11F H 0.9572 0.3986 0.4739 0.232 Uiso 0.40(2) 1 calc R U P A 2 N1 N 0.7489(4) 0.5220(4) 0.1713(4) 0.0591(16) Uani 1 1 d . . . . . N6 N 1 0.6180(6) 0.25 0.058(2) Uani 1 2 d S T P . . S1 S 0.62730(12) 0.30648(15) 0.03475(12) 0.0635(6) Uani 1 1 d . . . . . S2 S 0.81708(12) 0.37191(14) 0.07081(12) 0.0591(5) Uani 1 1 d . . . . . S3 S 0.58989(13) 0.49267(17) 0.15397(13) 0.0720(6) Uani 1 1 d . . . . . I1 I 0.66892(4) 0.67162(4) 0.28749(4) 0.0823(3) Uani 1 1 d . . . . . Ni1 Ni 0.75 0.25 0 0.0481(4) Uani 1 2 d S . P . . 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 C1 0.057(5) 0.055(4) 0.046(4) -0.001(3) 0.005(3) -0.018(4) C2 0.059(5) 0.045(4) 0.041(4) -0.001(3) 0.001(3) -0.012(3) C3 0.074(6) 0.047(4) 0.058(5) -0.014(3) 0.012(4) -0.011(4) C4 0.057(5) 0.072(5) 0.079(6) 0.002(4) -0.004(4) -0.010(4) C5 0.079(6) 0.087(6) 0.081(6) 0.019(5) 0.008(5) -0.002(5) C6 0.073(6) 0.096(7) 0.095(7) 0.020(5) -0.006(5) 0.015(5) C7 0.106(8) 0.102(7) 0.122(9) 0.045(7) -0.011(7) 0.018(6) C8 0.092(7) 0.081(6) 0.073(6) 0.004(5) -0.014(5) -0.010(5) C9 0.135(13) 0.122(11) 0.114(16) 0.065(9) 0.033(11) -0.033(10) C10 0.140(11) 0.125(12) 0.138(17) 0.095(10) 0.020(12) -0.023(9) C11 0.123(18) 0.172(18) 0.19(2) 0.092(15) -0.013(16) -0.006(11) C8A 0.092(7) 0.081(6) 0.073(6) 0.004(5) -0.014(5) -0.010(5) C9B 0.148(17) 0.127(13) 0.133(18) 0.069(13) 0.008(13) -0.028(14) C10B 0.142(13) 0.141(14) 0.136(18) 0.067(11) 0.010(13) -0.032(12) C11B 0.16(2) 0.17(2) 0.13(2) 0.069(16) 0.036(18) 0.033(19) N1 0.063(4) 0.055(4) 0.059(4) -0.010(3) 0.002(3) -0.014(3) N6 0.059(6) 0.054(5) 0.060(6) 0 -0.020(4) 0 S1 0.0550(12) 0.0714(12) 0.0646(13) -0.0209(10) 0.0086(10) -0.0170(10) S2 0.0535(12) 0.0595(11) 0.0647(13) -0.0101(9) 0.0046(10) -0.0151(9) S3 0.0618(14) 0.0747(13) 0.0805(15) -0.0197(11) 0.0137(11) -0.0098(11) I1 0.0937(5) 0.0711(4) 0.0834(5) -0.0241(3) 0.0175(3) -0.0087(3) Ni1 0.0525(8) 0.0513(7) 0.0407(7) -0.0028(5) 0.0063(6) -0.0146(6) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 '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 C2 C1 S1 122.1(5) . . ? C2 C1 S3 109.2(5) . . ? S1 C1 S3 128.6(4) . . ? C1 C2 N1 116.3(6) . . ? C1 C2 S2 121.2(5) . . ? N1 C2 S2 122.4(6) . . ? N1 C3 S3 115.9(5) . . ? N1 C3 I1 122.5(5) . . ? S3 C3 I1 121.5(4) . . ? C5 C4 N6 116.1(7) . . ? C5 C4 H4A 108.3 . . ? N6 C4 H4A 108.3 . . ? C5 C4 H4B 108.3 . . ? N6 C4 H4B 108.3 . . ? H4A C4 H4B 107.4 . . ? C4 C5 C6 115.1(8) . . ? C4 C5 H5A 108.5 . . ? C6 C5 H5A 108.5 . . ? C4 C5 H5B 108.5 . . ? C6 C5 H5B 108.5 . . ? H5A C5 H5B 107.5 . . ? C7 C6 C5 114.4(8) . . ? C7 C6 H6A 108.7 . . ? C5 C6 H6A 108.7 . . ? C7 C6 H6B 108.7 . . ? C5 C6 H6B 108.7 . . ? H6A C6 H6B 107.6 . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C9 C8 N6 119.1(13) . . ? C9 C8 H8A 107.6 . . ? N6 C8 H8A 107.6 . . ? C9 C8 H8B 107.6 . . ? N6 C8 H8B 107.6 . . ? H8A C8 H8B 107 . . ? C8 C9 C10 115(2) . . ? C8 C9 H9A 108.4 . . ? C10 C9 H9A 108.4 . . ? C8 C9 H9B 108.4 . . ? C10 C9 H9B 108.4 . . ? H9A C9 H9B 107.5 . . ? C11 C10 C9 108(2) . . ? C11 C10 H10A 110.1 . . ? C9 C10 H10A 110.1 . . ? C11 C10 H10B 110.1 . . ? C9 C10 H10B 110.1 . . ? H10A C10 H10B 108.4 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C9B C8A N6 106.5(18) . . ? C9B C8A H8AA 110.4 . . ? N6 C8A H8AA 110.4 . . ? C9B C8A H8AB 110.4 . . ? N6 C8A H8AB 110.4 . . ? H8AA C8A H8AB 108.6 . . ? C10B C9B C8A 95(3) . . ? C10B C9B H9B1 112.7 . . ? C8A C9B H9B1 112.7 . . ? C10B C9B H9B2 112.7 . . ? C8A C9B H9B2 112.7 . . ? H9B1 C9B H9B2 110.1 . . ? C11B C10B C9B 135(5) . . ? C11B C10B H10C 103.4 . . ? C9B C10B H10C 103.4 . . ? C11B C10B H10D 103.4 . . ? C9B C10B H10D 103.4 . . ? H10C C10B H10D 105.2 . . ? C10B C11B H11D 109.5 . . ? C10B C11B H11E 109.5 . . ? H11D C11B H11E 109.5 . . ? C10B C11B H11F 109.5 . . ? H11D C11B H11F 109.5 . . ? H11E C11B H11F 109.5 . . ? C3 N1 C2 109.5(6) . . ? C4 N6 C4 114.6(8) . 2_755 ? C4 N6 C8A 108.0(4) . 2_755 ? C4 N6 C8A 108.6(5) 2_755 2_755 ? C4 N6 C8 108.0(4) . 2_755 ? C4 N6 C8 108.6(5) 2_755 2_755 ? C4 N6 C8A 108.6(5) . . ? C4 N6 C8A 108.0(4) 2_755 . ? C8A N6 C8A 108.9(8) 2_755 . ? C4 N6 C8 108.6(5) . . ? C4 N6 C8 108.0(4) 2_755 . ? C8 N6 C8 108.9(8) 2_755 . ? C1 S1 Ni1 101.4(2) . . ? C2 S2 Ni1 101.6(2) . . ? C3 S3 C1 89.0(4) . . ? S2 Ni1 S2 180 . 7_655 ? S2 Ni1 S1 93.56(7) . . ? S2 Ni1 S1 86.44(7) 7_655 . ? S2 Ni1 S1 86.44(7) . 7_655 ? S2 Ni1 S1 93.56(7) 7_655 7_655 ? S1 Ni1 S1 180 . 7_655 ? 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 C1 C2 1.351(9) . ? C1 S1 1.720(7) . ? C1 S3 1.727(7) . ? C2 N1 1.389(8) . ? C2 S2 1.737(7) . ? C3 N1 1.290(9) . ? C3 S3 1.725(8) . ? C3 I1 2.086(7) . ? C4 C5 1.489(10) . ? C4 N6 1.491(9) . ? C4 H4A 0.97 . ? C4 H4B 0.97 . ? C5 C6 1.502(12) . ? C5 H5A 0.97 . ? C5 H5B 0.97 . ? C6 C7 1.481(12) . ? C6 H6A 0.97 . ? C6 H6B 0.97 . ? C7 H7A 0.96 . ? C7 H7B 0.96 . ? C7 H7C 0.96 . ? C8 C9 1.51(2) . ? C8 N6 1.559(9) . ? C8 H8A 0.97 . ? C8 H8B 0.97 . ? C9 C10 1.54(3) . ? C9 H9A 0.97 . ? C9 H9B 0.97 . ? C10 C11 1.434(17) . ? C10 H10A 0.97 . ? C10 H10B 0.97 . ? C11 H11A 0.96 . ? C11 H11B 0.96 . ? C11 H11C 0.96 . ? C8A C9B 1.490(19) . ? C8A N6 1.559(9) . ? C8A H8AA 0.97 . ? C8A H8AB 0.97 . ? C9B C10B 1.484(19) . ? C9B H9B1 0.97 . ? C9B H9B2 0.97 . ? C10B C11B 1.476(19) . ? C10B H10C 0.97 . ? C10B H10D 0.97 . ? C11B H11D 0.96 . ? C11B H11E 0.96 . ? C11B H11F 0.96 . ? N6 C4 1.491(9) 2_755 ? N6 C8A 1.559(9) 2_755 ? N6 C8 1.559(9) 2_755 ? S1 Ni1 2.178(2) . ? S2 Ni1 2.1670(18) . ? Ni1 S2 2.1670(18) 7_655 ? Ni1 S1 2.178(2) 7_655 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag S1 C1 C2 N1 -178.5(5) . . . . ? S3 C1 C2 N1 -0.5(7) . . . . ? S1 C1 C2 S2 2.7(8) . . . . ? S3 C1 C2 S2 -179.2(4) . . . . ? N6 C4 C5 C6 172.6(7) . . . . ? C4 C5 C6 C7 -177.6(8) . . . . ? N6 C8 C9 C10 -174.2(17) . . . . ? C8 C9 C10 C11 -79(3) . . . . ? N6 C8A C9B C10B -150(3) . . . . ? C8A C9B C10B C11B -88(6) . . . . ? S3 C3 N1 C2 -2.1(8) . . . . ? I1 C3 N1 C2 174.1(4) . . . . ? C1 C2 N1 C3 1.6(8) . . . . ? S2 C2 N1 C3 -179.6(5) . . . . ? C5 C4 N6 C4 53.9(6) . . . 2_755 ? C5 C4 N6 C8A -67.3(8) . . . 2_755 ? C5 C4 N6 C8 -67.3(8) . . . 2_755 ? C5 C4 N6 C8A 174.7(7) . . . . ? C5 C4 N6 C8 174.7(7) . . . . ? C9B C8A N6 C4 80(2) . . . . ? C9B C8A N6 C4 -155(2) . . . 2_755 ? C9B C8A N6 C8A -38(2) . . . 2_755 ? C9 C8 N6 C4 58.7(16) . . . . ? C9 C8 N6 C4 -176.4(15) . . . 2_755 ? C9 C8 N6 C8 -58.7(15) . . . 2_755 ? C2 C1 S1 Ni1 -0.2(6) . . . . ? S3 C1 S1 Ni1 -177.8(4) . . . . ? C1 C2 S2 Ni1 -3.6(6) . . . . ? N1 C2 S2 Ni1 177.7(5) . . . . ? N1 C3 S3 C1 1.6(6) . . . . ? I1 C3 S3 C1 -174.6(4) . . . . ? C2 C1 S3 C3 -0.6(5) . . . . ? S1 C1 S3 C3 177.3(5) . . . . ?