#------------------------------------------------------------------------------
#$Date: 2019-11-23 09:03:39 +0200 (Sat, 23 Nov 2019) $
#$Revision: 232637 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/80/4348007.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_4348007
loop_
_publ_author_name
'Yang, Hao'
'Liu, Jian-Lan'
'Zhou, Lan-Cheng'
'Ren, Xiao-Ming'
_publ_section_title
;
 Experimental and theoretical investigation of the magnetic and
 photoconductive nature of a novel two-dimensional, mixed-valence
 bis(2-thioxo-1,3-dithiole-4,5-dithiolato)nickelate molecular solid
;
_journal_issue                   5
_journal_name_full               'Inorg. Chem. Front.'
_journal_page_first              426
_journal_paper_doi               10.1039/C3QI00106G
_journal_volume                  1
_journal_year                    2014
_chemical_formula_sum            'C44 H46 N4 Ni3 S30'
_chemical_formula_weight         1768.78
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                109.910(3)
_cell_angle_beta                 105.249(3)
_cell_angle_gamma                103.361(3)
_cell_formula_units_Z            1
_cell_length_a                   11.6986(12)
_cell_length_b                   12.1197(12)
_cell_length_c                   14.0622(14)
_cell_measurement_temperature    296(2)
_cell_volume                     1691.9(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0452
_diffrn_reflns_av_sigmaI/netI    0.0433
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            34520
_diffrn_reflns_theta_full        27.55
_diffrn_reflns_theta_max         27.55
_diffrn_reflns_theta_min         1.92
_exptl_absorpt_coefficient_mu    1.790
_exptl_absorpt_correction_T_max  0.9158
_exptl_absorpt_correction_T_min  0.7160
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_density_diffrn    1.736
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             902
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.337
_refine_diff_density_min         -0.424
_refine_diff_density_rms         0.096
_refine_ls_extinction_coef       0.00148(17)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     369
_refine_ls_number_reflns         7788
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0827
_refine_ls_R_factor_gt           0.0423
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0295P)²+1.0249P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0760
_refine_ls_wR_factor_ref         0.0894
_reflns_number_gt                5220
_reflns_number_total             7788
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3qi00106g2.cif
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4348007
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Ni1 Ni 0.35830(3) 0.03764(3) 0.67495(3) 0.03346(10) Uani 1 1 d .
S1 S 0.29448(7) 0.19530(7) 0.72001(6) 0.04118(18) Uani 1 1 d .
S2 S 0.39366(7) 0.06585(6) 0.54034(6) 0.03872(18) Uani 1 1 d .
S3 S 0.34057(8) 0.02319(7) 0.81926(6) 0.0460(2) Uani 1 1 d .
S4 S 0.41068(8) -0.12791(7) 0.62542(6) 0.04071(18) Uani 1 1 d .
S5 S 0.38557(8) -0.16070(7) 0.91279(6) 0.0480(2) Uani 1 1 d .
S6 S 0.44706(8) -0.30103(7) 0.73522(6) 0.04338(19) Uani 1 1 d .
S7 S 0.45523(9) -0.38104(8) 0.91375(7) 0.0578(2) Uani 1 1 d .
S8 S 0.27380(7) 0.38160(6) 0.62363(6) 0.03864(18) Uani 1 1 d .
S9 S 0.36955(8) 0.26513(7) 0.46106(6) 0.04246(19) Uani 1 1 d .
S10 S 0.29917(9) 0.48596(8) 0.46488(7) 0.0560(2) Uani 1 1 d .
C1 C 0.3128(3) 0.3827(2) 0.5140(2) 0.0376(6) Uani 1 1 d .
C2 C 0.3110(2) 0.2511(2) 0.6266(2) 0.0325(6) Uani 1 1 d .
C3 C 0.3542(2) 0.1955(2) 0.5488(2) 0.0335(6) Uani 1 1 d .
C4 C 0.3797(3) -0.1072(3) 0.8122(2) 0.0369(6) Uani 1 1 d .
C5 C 0.4098(3) -0.1717(2) 0.7293(2) 0.0342(6) Uani 1 1 d .
C6 C 0.4307(3) -0.2852(3) 0.8572(2) 0.0395(7) Uani 1 1 d .
Ni2 Ni 0.0000 1.0000 0.5000 0.03743(14) Uani 1 2 d S
S11 S -0.03404(8) 0.97838(7) 0.63645(7) 0.0469(2) Uani 1 1 d .
S12 S 0.05807(7) 0.83957(7) 0.45833(6) 0.04487(19) Uani 1 1 d .
S13 S 0.08137(8) 0.66063(7) 0.56120(7) 0.0497(2) Uani 1 1 d .
S14 S -0.00211(9) 0.79132(8) 0.72888(7) 0.0550(2) Uani 1 1 d .
S15 S 0.06435(11) 0.57012(10) 0.72978(9) 0.0783(3) Uani 1 1 d .
C7 C 0.0052(3) 0.8516(3) 0.6344(2) 0.0394(7) Uani 1 1 d .
C8 C 0.0454(2) 0.7902(2) 0.5553(2) 0.0371(7) Uani 1 1 d .
C9 C 0.0489(3) 0.6683(3) 0.6761(3) 0.0492(8) Uani 1 1 d .
N1 N 0.2797(2) 0.8002(2) 0.22088(18) 0.0399(6) Uani 1 1 d .
N2 N 0.3849(2) 0.5089(2) 0.2506(2) 0.0539(7) Uani 1 1 d .
H2A H 0.4212 0.4736 0.2097 0.065 Uiso 1 1 calc R
H2B H 0.3715 0.4839 0.2984 0.065 Uiso 1 1 calc R
C10 C 0.3494(3) 0.6024(3) 0.2401(2) 0.0402(7) Uani 1 1 d .
C11 C 0.3694(3) 0.6459(3) 0.1638(2) 0.0467(7) Uani 1 1 d .
H11 H 0.4065 0.6078 0.1173 0.056 Uiso 1 1 calc R
C12 C 0.2907(3) 0.6637(3) 0.3062(3) 0.0514(8) Uani 1 1 d .
H12 H 0.2738 0.6375 0.3576 0.062 Uiso 1 1 calc R
C13 C 0.3352(3) 0.7431(3) 0.1567(2) 0.0467(8) Uani 1 1 d .
H13 H 0.3507 0.7711 0.1059 0.056 Uiso 1 1 calc R
C14 C 0.2592(3) 0.7596(3) 0.2954(2) 0.0501(8) Uani 1 1 d .
H14 H 0.2219 0.7996 0.3407 0.060 Uiso 1 1 calc R
C15 C 0.2498(3) 0.9418(3) 0.1267(2) 0.0450(7) Uani 1 1 d .
H15A H 0.1979 0.8689 0.0583 0.054 Uiso 1 1 calc R
H15B H 0.3362 0.9660 0.1297 0.054 Uiso 1 1 calc R
C16 C 0.2453(3) 0.9103(3) 0.2207(3) 0.0515(8) Uani 1 1 d .
H16A H 0.3019 0.9828 0.2880 0.062 Uiso 1 1 calc R
H16B H 0.1602 0.8956 0.2208 0.062 Uiso 1 1 calc R
C17 C 0.2010(3) 1.0904(3) 0.0433(3) 0.0529(8) Uani 1 1 d .
H17A H 0.1513 1.0187 -0.0265 0.063 Uiso 1 1 calc R
H17B H 0.2871 1.1192 0.0466 0.063 Uiso 1 1 calc R
C18 C 0.2010(3) 1.0494(3) 0.1333(3) 0.0499(8) Uani 1 1 d .
H18A H 0.1153 1.0240 0.1316 0.060 Uiso 1 1 calc R
H18B H 0.2529 1.1207 0.2028 0.060 Uiso 1 1 calc R
C19 C 0.1475(3) 1.1942(3) 0.0501(3) 0.0549(9) Uani 1 1 d .
H19A H 0.0607 1.1640 0.0448 0.066 Uiso 1 1 calc R
H19B H 0.1954 1.2643 0.1211 0.066 Uiso 1 1 calc R
C20 C 0.1493(3) 1.2409(3) -0.0362(3) 0.0630(10) Uani 1 1 d .
H20A H 0.1040 1.1706 -0.1075 0.076 Uiso 1 1 calc R
H20B H 0.2363 1.2747 -0.0292 0.076 Uiso 1 1 calc R
C21 C 0.0902(4) 1.3415(3) -0.0297(3) 0.0731(11) Uani 1 1 d .
H21A H 0.0024 1.3070 -0.0388 0.088 Uiso 1 1 calc R
H21B H 0.1339 1.4108 0.0423 0.088 Uiso 1 1 calc R
C22 C 0.0952(5) 1.3911(4) -0.1143(4) 0.1068(17) Uani 1 1 d .
H22A H 0.1816 1.4237 -0.1070 0.160 Uiso 1 1 calc R
H22B H 0.0603 1.4567 -0.1037 0.160 Uiso 1 1 calc R
H22C H 0.0469 1.3243 -0.1858 0.160 Uiso 1 1 calc R
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 0.0000 0.0000 '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'
Ni Ni 0.3393 1.1124 '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'
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
S3 Ni1 S2 174.51(4) . .
S3 Ni1 S1 86.09(3) . .
S2 Ni1 S1 93.20(3) . .
S3 Ni1 S4 93.44(3) . .
S2 Ni1 S4 87.58(3) . .
S1 Ni1 S4 176.60(3) . .
C2 S1 Ni1 101.96(9) . .
C3 S2 Ni1 101.94(9) . .
C4 S3 Ni1 101.84(9) . .
C5 S4 Ni1 101.53(10) . .
C6 S5 C4 97.41(13) . .
C6 S6 C5 97.40(13) . .
C1 S8 C2 97.24(13) . .
C1 S9 C3 97.04(13) . .
S10 C1 S8 123.42(17) . .
S10 C1 S9 122.97(17) . .
S8 C1 S9 113.60(15) . .
C3 C2 S1 121.5(2) . .
C3 C2 S8 115.8(2) . .
S1 C2 S8 122.68(16) . .
C2 C3 S2 121.4(2) . .
C2 C3 S9 116.3(2) . .
S2 C3 S9 122.35(16) . .
C5 C4 S3 121.6(2) . .
C5 C4 S5 116.5(2) . .
S3 C4 S5 121.89(16) . .
C4 C5 S4 121.6(2) . .
C4 C5 S6 115.5(2) . .
S4 C5 S6 122.91(16) . .
S7 C6 S5 123.72(17) . .
S7 C6 S6 123.12(17) . .
S5 C6 S6 113.17(15) . .
S11 Ni2 S11 180.0 . 2_576
S11 Ni2 S12 87.40(3) . 2_576
S11 Ni2 S12 92.60(3) 2_576 2_576
S11 Ni2 S12 92.60(3) . .
S11 Ni2 S12 87.40(3) 2_576 .
S12 Ni2 S12 180.00(5) 2_576 .
C7 S11 Ni2 102.96(10) . .
C8 S12 Ni2 102.82(10) . .
C9 S13 C8 97.06(14) . .
C7 S14 C9 97.39(15) . .
C8 C7 S11 120.7(2) . .
C8 C7 S14 115.9(2) . .
S11 C7 S14 123.42(18) . .
C7 C8 S12 120.9(2) . .
C7 C8 S13 116.3(2) . .
S12 C8 S13 122.77(17) . .
S15 C9 S13 123.5(2) . .
S15 C9 S14 123.1(2) . .
S13 C9 S14 113.36(17) . .
C13 N1 C14 118.4(3) . .
C13 N1 C16 124.8(2) . .
C14 N1 C16 116.7(2) . .
C10 N2 H2A 120.0 . .
C10 N2 H2B 120.0 . .
H2A N2 H2B 120.0 . .
N2 C10 C11 121.9(3) . .
N2 C10 C12 121.9(3) . .
C11 C10 C12 116.2(3) . .
C13 C11 C10 120.6(3) . .
C13 C11 H11 119.7 . .
C10 C11 H11 119.7 . .
C14 C12 C10 120.3(3) . .
C14 C12 H12 119.8 . .
C10 C12 H12 119.8 . .
N1 C13 C11 122.0(3) . .
N1 C13 H13 119.0 . .
C11 C13 H13 119.0 . .
C12 C14 N1 122.3(3) . .
C12 C14 H14 118.8 . .
N1 C14 H14 118.8 . .
C16 C15 C18 109.2(2) . .
C16 C15 H15A 109.8 . .
C18 C15 H15A 109.8 . .
C16 C15 H15B 109.8 . .
C18 C15 H15B 109.8 . .
H15A C15 H15B 108.3 . .
N1 C16 C15 115.8(2) . .
N1 C16 H16A 108.3 . .
C15 C16 H16A 108.3 . .
N1 C16 H16B 108.3 . .
C15 C16 H16B 108.3 . .
H16A C16 H16B 107.4 . .
C18 C17 C19 113.0(3) . .
C18 C17 H17A 109.0 . .
C19 C17 H17A 109.0 . .
C18 C17 H17B 109.0 . .
C19 C17 H17B 109.0 . .
H17A C17 H17B 107.8 . .
C17 C18 C15 114.5(3) . .
C17 C18 H18A 108.6 . .
C15 C18 H18A 108.6 . .
C17 C18 H18B 108.6 . .
C15 C18 H18B 108.6 . .
H18A C18 H18B 107.6 . .
C20 C19 C17 114.9(3) . .
C20 C19 H19A 108.6 . .
C17 C19 H19A 108.6 . .
C20 C19 H19B 108.6 . .
C17 C19 H19B 108.6 . .
H19A C19 H19B 107.5 . .
C19 C20 C21 113.4(3) . .
C19 C20 H20A 108.9 . .
C21 C20 H20A 108.9 . .
C19 C20 H20B 108.9 . .
C21 C20 H20B 108.9 . .
H20A C20 H20B 107.7 . .
C22 C21 C20 113.5(4) . .
C22 C21 H21A 108.9 . .
C20 C21 H21A 108.9 . .
C22 C21 H21B 108.9 . .
C20 C21 H21B 108.9 . .
H21A C21 H21B 107.7 . .
C21 C22 H22A 109.5 . .
C21 C22 H22B 109.5 . .
H22A C22 H22B 109.5 . .
C21 C22 H22C 109.5 . .
H22A C22 H22C 109.5 . .
H22B C22 H22C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni1 S3 2.1537(8) .
Ni1 S2 2.1585(8) .
Ni1 S1 2.1665(8) .
Ni1 S4 2.1742(8) .
S1 C2 1.703(3) .
S2 C3 1.712(3) .
S3 C4 1.723(3) .
S4 C5 1.717(3) .
S5 C6 1.717(3) .
S5 C4 1.737(3) .
S6 C6 1.727(3) .
S6 C5 1.744(3) .
S7 C6 1.651(3) .
S8 C1 1.722(3) .
S8 C2 1.746(3) .
S9 C1 1.732(3) .
S9 C3 1.738(3) .
S10 C1 1.641(3) .
C2 C3 1.361(4) .
C4 C5 1.349(4) .
Ni2 S11 2.1459(8) .
Ni2 S11 2.1459(8) 2_576
Ni2 S12 2.1515(8) 2_576
Ni2 S12 2.1516(8) .
S11 C7 1.695(3) .
S12 C8 1.692(3) .
S13 C9 1.732(3) .
S13 C8 1.739(3) .
S14 C7 1.732(3) .
S14 C9 1.738(3) .
S15 C9 1.631(3) .
C7 C8 1.372(4) .
N1 C13 1.344(3) .
N1 C14 1.351(4) .
N1 C16 1.481(4) .
N2 C10 1.333(4) .
N2 H2A 0.8600 .
N2 H2B 0.8600 .
C10 C11 1.394(4) .
C10 C12 1.410(4) .
C11 C13 1.353(4) .
C11 H11 0.9300 .
C12 C14 1.341(4) .
C12 H12 0.9300 .
C13 H13 0.9300 .
C14 H14 0.9300 .
C15 C16 1.505(4) .
C15 C18 1.525(4) .
C15 H15A 0.9700 .
C15 H15B 0.9700 .
C16 H16A 0.9700 .
C16 H16B 0.9700 .
C17 C18 1.510(4) .
C17 C19 1.515(4) .
C17 H17A 0.9700 .
C17 H17B 0.9700 .
C18 H18A 0.9700 .
C18 H18B 0.9700 .
C19 C20 1.507(4) .
C19 H19A 0.9700 .
C19 H19B 0.9700 .
C20 C21 1.524(5) .
C20 H20A 0.9700 .
C20 H20B 0.9700 .
C21 C22 1.512(5) .
C21 H21A 0.9700 .
C21 H21B 0.9700 .
C22 H22A 0.9600 .
C22 H22B 0.9600 .
C22 H22C 0.9600 .
