#------------------------------------------------------------------------------
#$Date: 2021-05-05 11:54:51 +0300 (Wed, 05 May 2021) $
#$Revision: 264921 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/06/04/7060460.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_7060460
loop_
_publ_author_name
'Chen, Xuan-Rong'
'Luo, Min'
'Zhang, Zhen-Min'
'Xu, Xiao-Yi'
'Jiang, Yi'
'Liu, Hang'
_publ_section_title
;
 Magnetism, dielectrics and ion conduction in two polymorphs of a
 heteroleptic bis(dithiolato)nickelate molecular solid
;
_journal_issue                   13
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              5971
_journal_page_last               5980
_journal_paper_doi               10.1039/D1NJ00491C
_journal_volume                  45
_journal_year                    2021
_chemical_formula_sum            'C16 H22 N3 Ni S7'
_chemical_formula_weight         539.49
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_audit_block_doi                 10.5517/ccdc.csd.cc26qv3x
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2021-02-23 deposited with the CCDC.	2021-03-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.828(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.878(2)
_cell_length_b                   17.576(2)
_cell_length_c                   7.5597(8)
_cell_measurement_reflns_used    5361
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.60
_cell_measurement_theta_min      1.63
_cell_volume                     2347.3(4)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0434
_diffrn_reflns_av_unetI/netI     0.0398
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            35822
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.598
_diffrn_reflns_theta_min         1.634
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.457
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.527
_exptl_crystal_description       needle
_exptl_crystal_F_000             1116
_refine_diff_density_max         1.234
_refine_diff_density_min         -0.430
_refine_diff_density_rms         0.104
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.62(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     249
_refine_ls_number_reflns         5361
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0884
_refine_ls_R_factor_gt           0.0543
_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/[σ²(Fo²)+(0.0857P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1214
_refine_ls_wR_factor_ref         0.1360
_reflns_Friedel_coverage         0.996
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.995
_reflns_number_gt                3850
_reflns_number_total             5361
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d1nj00491c2.cif
_cod_data_source_block           1_CCDC1
_cod_depositor_comments
'Adding full bibliography for 7060459--7060460.cif.'
_cod_original_sg_symbol_H-M      'C c'
_cod_database_code               7060460
_shelx_shelxl_version_number     2014/7
_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.
;
loop_
_space_group_symop_operation_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'
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
Ni1 Ni 0.70080(6) 0.44789(4) 0.44148(13) 0.0460(2) Uani 1 1 d . . . . .
S1 S 0.62354(10) 0.35833(12) 0.3413(3) 0.0565(6) Uani 1 1 d . . . . .
S2 S 0.62100(11) 0.53498(13) 0.3440(2) 0.0565(5) Uani 1 1 d . . . . .
S3 S 0.78236(11) 0.36094(12) 0.5408(3) 0.0538(5) Uani 1 1 d . . . . .
S4 S 0.77659(12) 0.53880(12) 0.5408(3) 0.0537(5) Uani 1 1 d . . . . .
S5 S 0.94317(12) 0.37373(12) 0.7350(3) 0.0648(6) Uani 1 1 d . . . . .
S6 S 0.93623(12) 0.53731(12) 0.7390(3) 0.0616(6) Uani 1 1 d . . . . .
S7 S 1.07690(15) 0.46225(16) 0.9061(4) 0.0929(8) Uani 1 1 d . . . . .
N1 N 0.4278(5) 0.3285(6) 0.1125(15) 0.113(3) Uani 1 1 d . . . . .
N2 N 0.4266(6) 0.5590(6) 0.1030(16) 0.121(4) Uani 1 1 d . . . . .
C1 C 0.4793(5) 0.3659(6) 0.1668(13) 0.072(3) Uani 1 1 d . . . . .
C2 C 0.5428(4) 0.4070(5) 0.2458(10) 0.058(2) Uani 1 1 d . . . . .
C3 C 0.5434(4) 0.4848(5) 0.2481(10) 0.060(2) Uani 1 1 d . . . . .
C4 C 0.4777(5) 0.5268(6) 0.1649(12) 0.072(3) Uani 1 1 d . . . . .
C5 C 0.8587(4) 0.4138(4) 0.6357(10) 0.0434(16) Uani 1 1 d . . . . .
C6 C 0.8561(4) 0.4913(4) 0.6351(9) 0.0463(17) Uani 1 1 d . . . . .
C7 C 0.9915(5) 0.4585(4) 0.8017(12) 0.065(2) Uani 1 1 d . . . . .
N3 N 0.7389(3) 0.1837(3) 0.9926(7) 0.0356(11) Uani 1 1 d . . . . .
C8 C 0.6546(3) 0.1923(4) 0.9319(9) 0.0491(16) Uani 1 1 d . . . . .
H8A H 0.6327 0.1419 0.9150 0.059 Uiso 1 1 calc R U . . .
H8B H 0.6329 0.2164 1.0278 0.059 Uiso 1 1 calc R U . . .
C9 C 0.6305(4) 0.2373(5) 0.7627(12) 0.067(2) Uani 1 1 d . . . . .
H9A H 0.6522 0.2879 0.7763 0.081 Uiso 1 1 calc R U . . .
H9B H 0.6494 0.2127 0.6636 0.081 Uiso 1 1 calc R U . . .
C10 C 0.5465(5) 0.2429(6) 0.7230(15) 0.094(3) Uani 1 1 d . . . . .
H10A H 0.5253 0.1930 0.7014 0.141 Uiso 1 1 calc R U . . .
H10B H 0.5324 0.2740 0.6187 0.141 Uiso 1 1 calc R U . . .
H10C H 0.5277 0.2654 0.8231 0.141 Uiso 1 1 calc R U . . .
C11 C 0.7729(4) 0.2613(4) 1.0371(9) 0.0454(15) Uani 1 1 d . . . . .
H11A H 0.7451 0.2859 1.1216 0.055 Uiso 1 1 calc R U . . .
H11B H 0.7663 0.2918 0.9288 0.055 Uiso 1 1 calc R U . . .
C12 C 0.8560(4) 0.2609(5) 1.1152(13) 0.068(2) Uani 1 1 d . . . . .
H12A H 0.8642 0.2269 1.2158 0.102 Uiso 1 1 calc R U . . .
H12B H 0.8715 0.3113 1.1536 0.102 Uiso 1 1 calc R U . . .
H12C H 0.8852 0.2441 1.0259 0.102 Uiso 1 1 calc R U . . .
C13 C 0.7503(4) 0.1321(3) 1.1554(8) 0.0488(15) Uani 1 1 d . . . . .
H13A H 0.7201 0.0866 1.1273 0.059 Uiso 1 1 calc R U . . .
H13B H 0.8029 0.1166 1.1778 0.059 Uiso 1 1 calc R U . . .
C14 C 0.7301(5) 0.1661(5) 1.3250(9) 0.069(2) Uani 1 1 d . . . . .
H14A H 0.7599 0.2110 1.3554 0.104 Uiso 1 1 calc R U . . .
H14B H 0.7403 0.1298 1.4205 0.104 Uiso 1 1 calc R U . . .
H14C H 0.6774 0.1792 1.3072 0.104 Uiso 1 1 calc R U . . .
C15 C 0.7772(4) 0.1481(3) 0.8494(9) 0.0475(14) Uani 1 1 d . . . . .
H15A H 0.7710 0.1819 0.7467 0.057 Uiso 1 1 calc R U . . .
H15B H 0.8310 0.1448 0.8937 0.057 Uiso 1 1 calc R U . . .
C16 C 0.7499(5) 0.0709(4) 0.7874(11) 0.070(2) Uani 1 1 d . . . . .
H16A H 0.7556 0.0366 0.8874 0.105 Uiso 1 1 calc R U . . .
H16B H 0.7791 0.0527 0.6995 0.105 Uiso 1 1 calc R U . . .
H16C H 0.6975 0.0737 0.7354 0.105 Uiso 1 1 calc R U . . .
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
_geom_angle_publ_flag
S2 Ni1 S1 92.51(10) . . ?
S2 Ni1 S4 86.56(7) . . ?
S1 Ni1 S4 179.06(10) . . ?
S2 Ni1 S3 179.34(11) . . ?
S1 Ni1 S3 88.14(6) . . ?
S4 Ni1 S3 92.78(10) . . ?
C2 S1 Ni1 103.5(3) . . ?
C3 S2 Ni1 103.4(3) . . ?
C5 S3 Ni1 102.3(3) . . ?
C6 S4 Ni1 102.8(3) . . ?
C5 S5 C7 97.9(4) . . ?
C7 S6 C6 98.6(4) . . ?
N1 C1 C2 174.9(11) . . ?
C3 C2 C1 121.7(7) . . ?
C3 C2 S1 118.9(6) . . ?
C1 C2 S1 119.5(7) . . ?
C2 C3 C4 120.0(8) . . ?
C2 C3 S2 121.7(5) . . ?
C4 C3 S2 118.3(7) . . ?
N2 C4 C3 179.0(11) . . ?
C6 C5 S3 121.1(5) . . ?
C6 C5 S5 115.8(5) . . ?
S3 C5 S5 123.1(5) . . ?
C5 C6 S4 121.1(5) . . ?
C5 C6 S6 116.2(5) . . ?
S4 C6 S6 122.7(4) . . ?
S7 C7 S6 124.2(5) . . ?
S7 C7 S5 124.3(5) . . ?
S6 C7 S5 111.5(5) . . ?
C15 N3 C11 108.9(5) . . ?
C15 N3 C8 111.5(5) . . ?
C11 N3 C8 108.9(5) . . ?
C15 N3 C13 108.5(5) . . ?
C11 N3 C13 111.1(5) . . ?
C8 N3 C13 108.0(5) . . ?
C9 C8 N3 116.8(5) . . ?
C9 C8 H8A 108.1 . . ?
N3 C8 H8A 108.1 . . ?
C9 C8 H8B 108.1 . . ?
N3 C8 H8B 108.1 . . ?
H8A C8 H8B 107.3 . . ?
C10 C9 C8 110.7(7) . . ?
C10 C9 H9A 109.5 . . ?
C8 C9 H9A 109.5 . . ?
C10 C9 H9B 109.5 . . ?
C8 C9 H9B 109.5 . . ?
H9A C9 H9B 108.1 . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N3 C11 C12 114.8(6) . . ?
N3 C11 H11A 108.6 . . ?
C12 C11 H11A 108.6 . . ?
N3 C11 H11B 108.6 . . ?
C12 C11 H11B 108.6 . . ?
H11A C11 H11B 107.5 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C14 C13 N3 115.7(5) . . ?
C14 C13 H13A 108.3 . . ?
N3 C13 H13A 108.3 . . ?
C14 C13 H13B 108.3 . . ?
N3 C13 H13B 108.3 . . ?
H13A C13 H13B 107.4 . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C16 C15 N3 116.2(6) . . ?
C16 C15 H15A 108.2 . . ?
N3 C15 H15A 108.2 . . ?
C16 C15 H15B 108.2 . . ?
N3 C15 H15B 108.2 . . ?
H15A C15 H15B 107.4 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
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
Ni1 S2 2.145(2) . ?
Ni1 S1 2.154(2) . ?
Ni1 S4 2.154(2) . ?
Ni1 S3 2.165(2) . ?
S1 C2 1.737(8) . ?
S2 C3 1.708(9) . ?
S3 C5 1.715(7) . ?
S4 C6 1.708(7) . ?
S5 C5 1.730(7) . ?
S5 C7 1.757(9) . ?
S6 C7 1.725(8) . ?
S6 C6 1.726(7) . ?
S7 C7 1.609(10) . ?
N1 C1 1.155(13) . ?
N2 C4 1.114(12) . ?
C1 C2 1.399(14) . ?
C2 C3 1.369(14) . ?
C3 C4 1.446(11) . ?
C5 C6 1.362(11) . ?
N3 C15 1.503(8) . ?
N3 C11 1.511(8) . ?
N3 C8 1.515(7) . ?
N3 C13 1.516(7) . ?
C8 C9 1.508(10) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 C10 1.489(10) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 C12 1.512(10) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C13 C14 1.508(9) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C15 C16 1.493(10) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
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
Ni1 S1 C2 C3 1.2(6) . . . . ?
Ni1 S1 C2 C1 -179.6(6) . . . . ?
C1 C2 C3 C4 -1.0(10) . . . . ?
S1 C2 C3 C4 178.2(6) . . . . ?
C1 C2 C3 S2 -179.8(7) . . . . ?
S1 C2 C3 S2 -0.6(8) . . . . ?
Ni1 S2 C3 C2 -0.3(6) . . . . ?
Ni1 S2 C3 C4 -179.2(5) . . . . ?
Ni1 S3 C5 C6 0.5(6) . . . . ?
Ni1 S3 C5 S5 -178.8(4) . . . . ?
C7 S5 C5 C6 1.5(6) . . . . ?
C7 S5 C5 S3 -179.1(5) . . . . ?
S3 C5 C6 S4 0.3(8) . . . . ?
S5 C5 C6 S4 179.7(4) . . . . ?
S3 C5 C6 S6 178.8(4) . . . . ?
S5 C5 C6 S6 -1.8(7) . . . . ?
Ni1 S4 C6 C5 -1.0(6) . . . . ?
Ni1 S4 C6 S6 -179.3(4) . . . . ?
C7 S6 C6 C5 1.2(6) . . . . ?
C7 S6 C6 S4 179.6(4) . . . . ?
C6 S6 C7 S7 179.2(5) . . . . ?
C6 S6 C7 S5 -0.1(5) . . . . ?
C5 S5 C7 S7 -179.9(5) . . . . ?
C5 S5 C7 S6 -0.6(5) . . . . ?
C15 N3 C8 C9 -56.8(8) . . . . ?
C11 N3 C8 C9 63.4(8) . . . . ?
C13 N3 C8 C9 -175.8(6) . . . . ?
N3 C8 C9 C10 -178.3(7) . . . . ?
C15 N3 C11 C12 -63.3(7) . . . . ?
C8 N3 C11 C12 174.9(6) . . . . ?
C13 N3 C11 C12 56.1(8) . . . . ?
C15 N3 C13 C14 167.6(6) . . . . ?
C11 N3 C13 C14 47.9(8) . . . . ?
C8 N3 C13 C14 -71.4(7) . . . . ?
C11 N3 C15 C16 -179.4(6) . . . . ?
C8 N3 C15 C16 -59.2(7) . . . . ?
C13 N3 C15 C16 59.5(7) . . . . ?
