#------------------------------------------------------------------------------ #$Date: 2024-11-23 03:09:45 +0200 (Sat, 23 Nov 2024) $ #$Revision: 296077 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/32/1573259.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_1573259 loop_ _publ_author_name 'Abherv\'e, Alexandre' 'Mroweh, Nabil' 'Cui, Hengbo' 'Kato, Reizo' 'Vanthuyne, Nicolas' 'Alemany, Pere' 'Canadell, Enric' 'Avarvari, Narcis' _publ_section_title ; Enantiomorphic single component conducting nickel(II) and platinum(II) bis(diethyl-dddt) crystalline complexes† ; _journal_name_full Nanoscale _journal_paper_doi 10.1039/D4NR04048A _journal_year 2024 _chemical_absolute_configuration syn _chemical_formula_moiety 'C16 H24 Ni S8' _chemical_formula_sum 'C16 H24 Ni S8' _chemical_formula_weight 531.54 _space_group_crystal_system tetragonal _space_group_IT_number 92 _space_group_name_Hall 'P 4abw 2nw' _space_group_name_H-M_alt 'P 41 21 2' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2018/3 _audit_update_record ; 2024-09-26 deposited with the CCDC. 2024-11-22 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 14.2738(7) _cell_length_b 14.2738(7) _cell_length_c 21.7030(11) _cell_measurement_reflns_used 2054 _cell_measurement_temperature 149.9(4) _cell_measurement_theta_max 69.2880 _cell_measurement_theta_min 4.3670 _cell_volume 4421.8(4) _computing_cell_refinement 'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)' _computing_data_collection 'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)' _computing_data_reduction 'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)' _computing_molecular_graphics 'DIAMOND 3.2k (Crystal Impact GbR, 2014)' _computing_publication_material 'WinGX publication routines (Farrugia, 2012)' _computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)' _computing_structure_solution 'SHELXL-2018/3 (Sheldrick, 2018)' _diffrn_ambient_temperature 149.9(4) _diffrn_detector_area_resol_mean 5.1990 _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.986 _diffrn_measurement_device_type 'SuperNova, Single source at offset, AtlasS2' _diffrn_measurement_method '\w scans' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0558 _diffrn_reflns_av_unetI/netI 0.0649 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.986 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_number 9610 _diffrn_reflns_point_group_measured_fraction_full 0.993 _diffrn_reflns_point_group_measured_fraction_max 0.971 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 73.368 _diffrn_reflns_theta_min 3.706 _diffrn_source 'micro-focus sealed X-ray tube' _exptl_absorpt_coefficient_mu 8.318 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.73585 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour black _exptl_crystal_density_diffrn 1.597 _exptl_crystal_description needle _exptl_crystal_F_000 2208 _refine_diff_density_max 2.496 _refine_diff_density_min -0.604 _refine_diff_density_rms 0.179 _refine_ls_abs_structure_details ; Refined as an inversion twin. ; _refine_ls_abs_structure_Flack 0.47(11) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 232 _refine_ls_number_reflns 4320 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.027 _refine_ls_R_factor_all 0.1196 _refine_ls_R_factor_gt 0.0981 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.1902P)^2^+7.7253P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2576 _refine_ls_wR_factor_ref 0.2900 _reflns_Friedel_coverage 0.691 _reflns_Friedel_fraction_full 0.984 _reflns_Friedel_fraction_max 0.950 _reflns_number_gt 3300 _reflns_number_total 4320 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4nr04048a2.cif _cod_data_source_block shelx_CCDC1 _cod_original_cell_volume 4421.8(5) _cod_database_code 1573259 _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. ; _oxdiff_exptl_absorpt_empirical_full_min 0.807 _oxdiff_exptl_absorpt_empirical_full_max 1.332 _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; _shelx_res_file ; TITL aa299a in P 41 21 2 shelx.res created by SHELXL-2018/3 at 15:15:24 on 23-Sep-2024 CELL 1.54184 14.2738 14.2738 21.7030 90.000 90.000 90.000 ZERR 8.00 0.0007 0.0007 0.0011 0.000 0.000 0.000 LATT -1 SYMM - X, - Y, 1/2 + Z SYMM 1/2 + X, 1/2 - Y, 3/4 - Z SYMM 1/2 - X, 1/2 + Y, 1/4 - Z SYMM - Y, - X, 1/2 - Z SYMM Y, X, - Z SYMM 1/2 + Y, 1/2 - X, 3/4 + Z SYMM 1/2 - Y, 1/2 + X, 1/4 + Z SFAC C H S NI UNIT 128 192 64 8 MERG 2 TWIN FMAP 2 PLAN 25 ACTA L.S. 8 WGHT 0.190200 7.725300 BASF 0.47458 FVAR 1.89675 C1 1 0.580785 0.151168 0.962956 11.00000 0.06294 0.07158 = 0.07335 0.00840 -0.01428 0.00779 AFIX 13 H1 2 0.550731 0.199621 0.937801 11.00000 -1.20000 AFIX 0 C2 1 0.623574 0.201411 1.014123 11.00000 0.06247 0.06291 = 0.05965 0.00690 0.00432 0.01061 AFIX 13 H2 2 0.572929 0.234517 1.035464 11.00000 -1.20000 AFIX 0 C3 1 0.735767 0.030049 0.962791 11.00000 0.04397 0.04254 = 0.06583 0.00293 -0.00509 0.00840 C4 1 0.739912 0.040667 1.025464 11.00000 0.03936 0.04286 = 0.05288 0.00286 0.00091 0.00350 C5 1 0.503027 0.087658 0.982468 11.00000 0.06861 0.11216 = 0.09990 0.00370 -0.01570 -0.00256 AFIX 23 H5A 2 0.457824 0.122637 1.006645 11.00000 -1.20000 H5B 2 0.527917 0.037841 1.008083 11.00000 -1.20000 AFIX 0 C6 1 0.453336 0.044316 0.924619 11.00000 0.07668 0.22130 = 0.17663 -0.08650 -0.04418 0.01085 AFIX 33 H6A 2 0.403607 0.003728 0.937822 11.00000 -1.50000 H6B 2 0.428020 0.093670 0.899604 11.00000 -1.50000 H6C 2 0.497980 0.009034 0.901039 11.00000 -1.50000 AFIX 0 C7 1 0.693726 0.276264 0.992693 11.00000 0.09814 0.08513 = 0.05269 0.00873 0.00727 0.01008 AFIX 23 H7A 2 0.747553 0.245445 0.974431 11.00000 -1.20000 H7B 2 0.664560 0.314366 0.961044 11.00000 -1.20000 AFIX 0 C8 1 0.725074 0.335912 1.041462 11.00000 0.24015 0.08412 = 0.19016 -0.07094 0.12192 -0.08926 AFIX 33 H8A 2 0.768548 0.381057 1.025415 11.00000 -1.50000 H8B 2 0.672344 0.367834 1.059158 11.00000 -1.50000 H8C 2 0.755372 0.298885 1.072551 11.00000 -1.50000 AFIX 0 C10 1 0.770763 0.253399 0.780165 11.00000 0.05879 0.05624 = 0.04363 0.00636 0.00844 0.01254 C11 1 1.061872 -0.045267 0.781964 11.00000 0.05620 0.06006 = 0.04083 0.00784 0.00355 -0.00428 C12 1 1.218280 -0.164971 0.774834 11.00000 0.05554 0.06734 = 0.07931 0.01361 0.00441 0.01118 AFIX 13 H12 2 1.251151 -0.212907 0.798869 11.00000 -1.20000 AFIX 0 C13 1 0.531998 0.285939 0.790838 11.00000 0.12153 0.13449 = 0.10809 -0.02864 0.00827 0.06063 AFIX 23 H13A 2 0.556128 0.225710 0.777549 11.00000 -1.20000 H13B 2 0.516999 0.280735 0.834295 11.00000 -1.20000 AFIX 0 C14 1 0.695675 0.552142 0.741970 11.00000 0.19826 0.08157 = 0.10000 0.02155 0.04930 0.06592 C15 1 1.293614 -0.098732 0.752459 11.00000 0.06743 0.07508 = 0.13919 -0.02650 0.04563 0.00448 AFIX 23 H15A 2 1.264929 -0.050152 0.727542 11.00000 -1.20000 H15B 2 1.337017 -0.132976 0.726469 11.00000 -1.20000 AFIX 0 C16 1 1.348281 -0.052737 0.805407 11.00000 0.06579 0.10186 = 0.19870 -0.02160 -0.00814 -0.03089 AFIX 33 H16A 2 1.395035 -0.011544 0.788761 11.00000 -1.50000 H16B 2 1.305934 -0.017546 0.830809 11.00000 -1.50000 H16C 2 1.378031 -0.100381 0.829735 11.00000 -1.50000 AFIX 0 S1 3 0.666347 0.093974 0.911033 11.00000 0.07736 0.07011 = 0.05505 0.00682 -0.00800 0.02287 S2 3 0.675314 0.118269 1.070695 11.00000 0.06581 0.07210 = 0.04890 -0.00232 -0.00099 0.02444 S3 3 0.810395 -0.046851 0.927165 11.00000 0.05622 0.05413 = 0.04786 0.00220 0.00098 0.01129 S4 3 0.812316 -0.032940 1.066457 11.00000 0.06094 0.06115 = 0.04377 -0.00120 -0.00396 0.01633 S5 3 0.716390 0.335078 0.826270 11.00000 0.07121 0.08972 = 0.04872 -0.00566 0.00510 0.02773 S6 3 0.855288 0.188143 0.817115 11.00000 0.05377 0.07290 = 0.04593 -0.00752 -0.00225 0.01647 S7 3 0.997907 0.037491 0.818731 11.00000 0.05573 0.07015 = 0.04198 -0.00176 -0.00176 0.01494 S8 3 1.138074 -0.108011 0.829063 11.00000 0.06163 0.08958 = 0.04619 0.00346 0.00067 0.02889 NI1 4 0.885969 -0.114031 1.000000 10.50000 0.04834 0.04834 = 0.04224 0.00111 -0.00111 0.00807 NI2 4 0.906648 0.093352 0.750000 10.50000 0.05660 0.05660 = 0.04036 -0.00014 -0.00014 0.00941 PART 1 C9 1 0.612204 0.361335 0.783137 10.50000 0.02894 0.04044 = 0.03377 0.01592 0.00185 0.02486 AFIX 13 H9 2 0.587224 0.418879 0.801488 10.50000 -1.20000 PART 2 AFIX 0 C9B 1 0.642618 0.401109 0.769463 10.50000 0.10468 AFIX 13 H9B 2 0.600662 0.444220 0.791226 10.50000 -1.20000 AFIX 0 HKLF 4 REM aa299a in P 41 21 2 REM wR2 = 0.2900, GooF = S = 1.027, Restrained GooF = 1.027 for all data REM R1 = 0.0981 for 3300 Fo > 4sig(Fo) and 0.1196 for all 4320 data REM 232 parameters refined using 0 restraints END WGHT 0.1901 7.7154 REM Highest difference peak 2.496, deepest hole -0.604, 1-sigma level 0.179 Q1 1 0.8614 0.1386 0.7500 10.50000 0.05 2.50 Q2 1 0.6817 0.3912 0.8231 11.00000 0.05 1.54 Q3 1 0.8261 0.2434 0.8126 11.00000 0.05 1.44 Q4 1 1.1296 -0.0359 0.8173 11.00000 0.05 1.37 Q5 1 0.7964 0.5878 0.7506 11.00000 0.05 1.29 Q6 1 0.9731 0.0972 0.8128 11.00000 0.05 1.29 Q7 1 0.8032 0.3951 1.0006 11.00000 0.05 1.15 Q8 1 0.7123 0.1370 0.9260 11.00000 0.05 1.07 Q9 1 0.6573 0.0764 1.0839 11.00000 0.05 0.89 Q10 1 0.9629 0.0013 0.8166 11.00000 0.05 0.81 Q11 1 0.8467 -0.0058 1.0708 11.00000 0.05 0.76 Q12 1 0.8141 0.1462 0.8189 11.00000 0.05 0.75 Q13 1 0.6049 0.1657 1.0824 11.00000 0.05 0.74 Q14 1 0.5828 0.1770 0.9257 11.00000 0.05 0.68 Q15 1 0.4992 0.2594 0.8185 11.00000 0.05 0.68 Q16 1 0.4604 -0.1250 0.9331 11.00000 0.05 0.65 Q17 1 1.3761 0.0422 0.8226 11.00000 0.05 0.64 Q18 1 1.0966 -0.1357 0.8215 11.00000 0.05 0.63 Q19 1 0.6726 0.3027 0.8267 11.00000 0.05 0.62 Q20 1 0.6747 0.0979 1.0411 11.00000 0.05 0.60 Q21 1 0.7123 0.5113 0.8145 11.00000 0.05 0.57 Q22 1 0.6837 0.5150 0.7241 11.00000 0.05 0.57 Q23 1 0.6243 0.4612 0.7718 11.00000 0.05 0.57 Q24 1 0.7312 0.3137 0.9286 11.00000 0.05 0.55 Q25 1 0.7410 0.3256 1.0630 11.00000 0.05 0.54 ; _shelx_res_checksum 96812 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y+1/2, -z+3/4' '-x+1/2, y+1/2, -z+1/4' '-y, -x, -z+1/2' 'y, x, -z' 'y+1/2, -x+1/2, z+3/4' '-y+1/2, x+1/2, z+1/4' 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 0.5808(12) 0.1512(13) 0.9630(8) 0.069(4) Uani 1 1 d . . . . . H1 H 0.550731 0.199621 0.937801 0.083 Uiso 1 1 calc R U . . . C2 C 0.6236(12) 0.2014(11) 1.0141(7) 0.062(4) Uani 1 1 d . . . . . H2 H 0.572929 0.234517 1.035464 0.074 Uiso 1 1 calc R U . . . C3 C 0.7358(10) 0.0300(10) 0.9628(7) 0.051(3) Uani 1 1 d . . . . . C4 C 0.7399(9) 0.0407(9) 1.0255(6) 0.045(3) Uani 1 1 d . . . . . C5 C 0.5030(15) 0.0877(17) 0.9825(11) 0.094(6) Uani 1 1 d . . . . . H5A H 0.457824 0.122637 1.006645 0.112 Uiso 1 1 calc R U . . . H5B H 0.527917 0.037841 1.008083 0.112 Uiso 1 1 calc R U . . . C6 C 0.4533(18) 0.044(3) 0.9246(15) 0.158(15) Uani 1 1 d . . . . . H6A H 0.403607 0.003728 0.937822 0.237 Uiso 1 1 calc R U . . . H6B H 0.428020 0.093670 0.899604 0.237 Uiso 1 1 calc R U . . . H6C H 0.497980 0.009034 0.901039 0.237 Uiso 1 1 calc R U . . . C7 C 0.6937(15) 0.2763(14) 0.9927(7) 0.079(5) Uani 1 1 d . . . . . H7A H 0.747553 0.245445 0.974431 0.094 Uiso 1 1 calc R U . . . H7B H 0.664560 0.314366 0.961044 0.094 Uiso 1 1 calc R U . . . C8 C 0.725(3) 0.3359(18) 1.0415(15) 0.171(18) Uani 1 1 d . . . . . H8A H 0.768548 0.381057 1.025415 0.257 Uiso 1 1 calc R U . . . H8B H 0.672344 0.367834 1.059158 0.257 Uiso 1 1 calc R U . . . H8C H 0.755372 0.298885 1.072551 0.257 Uiso 1 1 calc R U . . . C10 C 0.7708(11) 0.2534(11) 0.7802(6) 0.053(3) Uani 1 1 d . . . . . C11 C 1.0619(10) -0.0453(10) 0.7820(6) 0.052(3) Uani 1 1 d . . . . . C12 C 1.2183(12) -0.1650(13) 0.7748(8) 0.067(4) Uani 1 1 d . . . . . H12 H 1.251151 -0.212907 0.798869 0.081 Uiso 1 1 calc R U . . . C13 C 0.532(2) 0.286(2) 0.7908(12) 0.121(10) Uani 1 1 d . . . . . H13A H 0.556128 0.225710 0.777549 0.146 Uiso 1 1 calc R U . A 1 H13B H 0.516999 0.280735 0.834295 0.146 Uiso 1 1 calc R U . A 1 C14 C 0.696(2) 0.5521(17) 0.7420(12) 0.127(11) Uani 1 1 d . . . . . C15 C 1.2936(13) -0.0987(14) 0.7525(12) 0.094(7) Uani 1 1 d . . . . . H15A H 1.264929 -0.050152 0.727542 0.113 Uiso 1 1 calc R U . . . H15B H 1.337017 -0.132976 0.726469 0.113 Uiso 1 1 calc R U . . . C16 C 1.3483(16) -0.0527(19) 0.8054(16) 0.122(10) Uani 1 1 d . . . . . H16A H 1.395035 -0.011544 0.788761 0.183 Uiso 1 1 calc R U . . . H16B H 1.305934 -0.017546 0.830809 0.183 Uiso 1 1 calc R U . . . H16C H 1.378031 -0.100381 0.829735 0.183 Uiso 1 1 calc R U . . . S1 S 0.6663(3) 0.0940(3) 0.91103(18) 0.0675(11) Uani 1 1 d . . . . . S2 S 0.6753(3) 0.1183(3) 1.07069(16) 0.0623(10) Uani 1 1 d . . . . . S3 S 0.8104(3) -0.0469(3) 0.92717(15) 0.0527(8) Uani 1 1 d . . . . . S4 S 0.8123(3) -0.0329(3) 1.06646(15) 0.0553(8) Uani 1 1 d . . . . . S5 S 0.7164(3) 0.3351(4) 0.82627(16) 0.0699(12) Uani 1 1 d . . . . . S6 S 0.8553(3) 0.1881(3) 0.81712(15) 0.0575(9) Uani 1 1 d . . . . . S7 S 0.9979(3) 0.0375(3) 0.81873(15) 0.0560(9) Uani 1 1 d . . . . . S8 S 1.1381(3) -0.1080(3) 0.82906(16) 0.0658(11) Uani 1 1 d . . . . . Ni1 Ni 0.88597(16) -0.11403(16) 1.000000 0.0463(7) Uani 1 2 d S T P . . Ni2 Ni 0.90665(16) 0.09335(16) 0.750000 0.0512(8) Uani 1 2 d S T P . . C9 C 0.6122(15) 0.3613(17) 0.7831(9) 0.034(5) Uani 0.5 1 d . . P B 1 H9 H 0.587224 0.418879 0.801488 0.041 Uiso 0.5 1 calc R U P B 1 C9B C 0.643(4) 0.401(4) 0.769(3) 0.105(17) Uiso 0.5 1 d . . P B 2 H9B H 0.600662 0.444220 0.791226 0.126 Uiso 0.5 1 calc R U P B 2 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 0.063(10) 0.072(10) 0.073(10) 0.008(8) -0.014(8) 0.008(8) C2 0.062(9) 0.063(9) 0.060(8) 0.007(7) 0.004(7) 0.011(7) C3 0.044(7) 0.043(7) 0.066(8) 0.003(6) -0.005(6) 0.008(5) C4 0.039(6) 0.043(7) 0.053(6) 0.003(5) 0.001(5) 0.004(5) C5 0.069(12) 0.112(17) 0.100(15) 0.004(13) -0.016(11) -0.003(11) C6 0.077(16) 0.22(4) 0.18(3) -0.09(3) -0.044(19) 0.01(2) C7 0.098(14) 0.085(12) 0.053(8) 0.009(8) 0.007(9) 0.010(10) C8 0.24(4) 0.084(17) 0.19(3) -0.071(19) 0.12(3) -0.09(2) C10 0.059(9) 0.056(8) 0.044(6) 0.006(6) 0.008(6) 0.013(7) C11 0.056(8) 0.060(9) 0.041(6) 0.008(6) 0.004(6) -0.004(6) C12 0.056(9) 0.067(10) 0.079(10) 0.014(8) 0.004(8) 0.011(7) C13 0.12(2) 0.13(2) 0.108(17) -0.029(17) 0.008(16) 0.061(18) C14 0.20(3) 0.082(15) 0.100(15) 0.022(13) 0.049(19) 0.066(18) C15 0.067(11) 0.075(12) 0.139(18) -0.027(13) 0.046(12) 0.004(9) C16 0.066(13) 0.102(18) 0.20(3) -0.02(2) -0.008(17) -0.031(12) S1 0.077(3) 0.070(2) 0.0551(19) 0.0068(17) -0.0080(18) 0.023(2) S2 0.066(2) 0.072(2) 0.0489(16) -0.0023(16) -0.0010(16) 0.0244(19) S3 0.0562(19) 0.0541(19) 0.0479(15) 0.0022(14) 0.0010(14) 0.0113(15) S4 0.061(2) 0.061(2) 0.0438(14) -0.0012(14) -0.0040(14) 0.0163(16) S5 0.071(2) 0.090(3) 0.0487(17) -0.0057(19) 0.0051(17) 0.028(2) S6 0.0538(19) 0.073(2) 0.0459(15) -0.0075(16) -0.0022(14) 0.0165(16) S7 0.0557(18) 0.070(2) 0.0420(15) -0.0018(15) -0.0018(13) 0.0149(16) S8 0.062(2) 0.090(3) 0.0462(16) 0.0035(17) 0.0007(15) 0.029(2) Ni1 0.0483(10) 0.0483(10) 0.0422(14) 0.0011(8) -0.0011(8) 0.0081(13) Ni2 0.0566(12) 0.0566(12) 0.0404(14) -0.0001(10) -0.0001(10) 0.0094(14) C9 0.029(10) 0.040(12) 0.034(11) 0.016(8) 0.002(8) 0.025(9) 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' 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 C2 C1 C5 113.2(16) . . ? C2 C1 S1 113.9(12) . . ? C5 C1 S1 113.3(15) . . ? C1 C2 C7 112.6(14) . . ? C1 C2 S2 110.8(11) . . ? C7 C2 S2 112.6(12) . . ? C4 C3 S3 119.5(11) . . ? C4 C3 S1 127.1(11) . . ? S3 C3 S1 113.3(8) . . ? C3 C4 S4 118.1(11) . . ? C3 C4 S2 127.3(11) . . ? S4 C4 S2 114.5(7) . . ? C1 C5 C6 110(2) . . ? C8 C7 C2 113.2(15) . . ? C10 C10 S5 126.9(5) 5_666 . ? C10 C10 S6 118.4(5) 5_666 . ? S5 C10 S6 114.3(8) . . ? C11 C11 S7 119.0(5) 5_666 . ? C11 C11 S8 126.1(5) 5_666 . ? S7 C11 S8 114.8(7) . . ? C15 C12 C12 116.1(19) . 5_666 ? C15 C12 S8 111.9(13) . . ? C12 C12 S8 111.4(11) 5_666 . ? C14 C13 C9 116(3) 5_666 . ? C14 C13 C9B 89(2) 5_666 5_666 ? C9 C13 C9B 37.2(18) . 5_666 ? C12 C15 C16 113(2) . . ? C3 S1 C1 102.3(7) . . ? C4 S2 C2 104.1(7) . . ? C3 S3 Ni1 105.5(5) . . ? C4 S4 Ni1 106.2(5) . . ? C10 S5 C9 102.2(9) . . ? C10 S5 C9B 102.2(18) . . ? C10 S6 Ni2 105.5(5) . . ? C11 S7 Ni2 105.1(5) . . ? C11 S8 C12 104.0(7) . . ? S4 Ni1 S4 176.0(3) . 6_647 ? S4 Ni1 S3 89.71(12) . 6_647 ? S4 Ni1 S3 90.45(12) 6_647 6_647 ? S4 Ni1 S3 90.45(12) . . ? S4 Ni1 S3 89.71(12) 6_647 . ? S3 Ni1 S3 175.5(3) 6_647 . ? S6 Ni2 S6 91.8(2) . 5_666 ? S6 Ni2 S7 88.24(13) . . ? S6 Ni2 S7 177.65(16) 5_666 . ? S6 Ni2 S7 177.64(16) . 5_666 ? S6 Ni2 S7 88.24(13) 5_666 5_666 ? S7 Ni2 S7 91.9(2) . 5_666 ? C9 C9 C13 116(3) 5_666 . ? C9 C9 S5 109.6(17) 5_666 . ? C13 C9 S5 113.7(15) . . ? C9B C9B S5 119(4) 5_666 . ? C9B C9B C13 93(6) 5_666 5_666 ? S5 C9B C13 114(3) . 5_666 ? 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 1.46(2) . ? C1 C5 1.49(3) . ? C1 S1 1.851(19) . ? C2 C7 1.54(3) . ? C2 S2 1.860(15) . ? C3 C4 1.370(19) . ? C3 S3 1.714(14) . ? C3 S1 1.754(13) . ? C4 S4 1.721(13) . ? C4 S2 1.744(13) . ? C5 C6 1.57(3) . ? C7 C8 1.43(3) . ? C10 C10 1.40(3) 5_666 ? C10 S5 1.721(14) . ? C10 S6 1.722(14) . ? C11 C11 1.43(3) 5_666 ? C11 S7 1.693(15) . ? C11 S8 1.741(14) . ? C12 C15 1.51(3) . ? C12 C12 1.52(4) 5_666 ? C12 S8 1.832(17) . ? C13 C14 1.42(3) 5_666 ? C13 C9 1.58(4) . ? C13 C9B 1.91(7) 5_666 ? C15 C16 1.54(3) . ? S3 Ni1 2.141(3) . ? S4 Ni1 2.127(3) . ? S5 C9 1.80(2) . ? S5 C9B 1.88(6) . ? S6 Ni2 2.119(4) . ? S7 Ni2 2.135(4) . ? C9 C9 1.53(4) 5_666 ? C9B C9B 1.22(11) 5_666 ?