#------------------------------------------------------------------------------
#$Date: 2021-08-01 02:51:52 +0300 (Sun, 01 Aug 2021) $
#$Revision: 267873 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/56/43/1564302.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_1564302
loop_
_publ_author_name
'Qian, Yin'
'Yao, Wan-Wan'
'Shao, Dong-Sheng'
'Zhang, Jin'
'Ren, Xiao-Ming'
_publ_section_title
;
 Two Ongoing Magnetic Transitions Originating from Spin-Peierls
 Dimerization and Cation Orientation Transformation in an S = 1/2 Spin
 Chain System
;
_journal_name_full               'The Journal of Physical Chemistry C'
_journal_paper_doi               10.1021/acs.jpcc.1c04863
_journal_year                    2021
_chemical_formula_sum            'C14 H14 N5 Ni S4'
_chemical_formula_weight         439.25
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.346(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   6.8750(4)
_cell_length_b                   19.7127(12)
_cell_length_c                   14.1318(8)
_cell_measurement_reflns_used    6675
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      27.00
_cell_measurement_theta_min      2.52
_cell_volume                     1915.17(19)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_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  0.0533
_diffrn_reflns_av_sigmaI/netI    0.0638
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            18576
_diffrn_reflns_theta_full        27.58
_diffrn_reflns_theta_max         27.58
_diffrn_reflns_theta_min         2.52
_exptl_absorpt_coefficient_mu    1.455
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.523
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             900
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.902
_refine_diff_density_min         -0.525
_refine_diff_density_rms         0.094
_refine_ls_extinction_coef       0.0035(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     220
_refine_ls_number_reflns         4400
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.1099
_refine_ls_R_factor_gt           0.0670
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0213P)²+9.9313P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1332
_refine_ls_wR_factor_ref         0.1467
_reflns_number_gt                2923
_reflns_number_total             4400
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jp1c04863_si_002.cif
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               1564302
loop_
_symmetry_equiv_pos_as_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.75861(10) 0.95204(3) 0.46126(5) 0.0366(2) Uani 1 1 d . . .
S1 S 0.7754(2) 0.84598(7) 0.42765(12) 0.0514(4) Uani 1 1 d . . .
S2 S 0.7636(2) 0.98123(7) 0.31469(11) 0.0463(4) Uani 1 1 d . . .
S3 S 0.7406(2) 0.92129(7) 0.60605(11) 0.0492(4) Uani 1 1 d . . .
S4 S 0.7461(2) 1.05775(6) 0.49728(10) 0.0391(3) Uani 1 1 d . . .
N1 N 0.8063(15) 0.7287(4) 0.2275(6) 0.130(3) Uani 1 1 d . . .
N2 N 0.7945(11) 0.9067(4) 0.0738(5) 0.093(2) Uani 1 1 d . . .
N3 N 0.7166(13) 0.9903(4) 0.8470(5) 0.105(3) Uani 1 1 d . . .
N4 N 0.7127(8) 1.1695(3) 0.7082(4) 0.0653(15) Uani 1 1 d . . .
N5 N 0.7248(9) 0.3469(3) 0.5855(5) 0.0714(18) Uani 1 1 d . . .
C1 C 0.7960(12) 0.7810(4) 0.2606(6) 0.077(2) Uani 1 1 d . . .
C2 C 0.7845(9) 0.8454(3) 0.3064(5) 0.0521(16) Uani 1 1 d . . .
C3 C 0.7784(9) 0.9045(3) 0.2554(5) 0.0523(15) Uani 1 1 d . . .
C4 C 0.7889(11) 0.9059(4) 0.1556(5) 0.0655(19) Uani 1 1 d . . .
C5 C 0.7198(11) 0.9941(4) 0.7667(5) 0.0656(19) Uani 1 1 d . . .
C6 C 0.7301(9) 0.9964(3) 0.6654(4) 0.0475(14) Uani 1 1 d . . .
C7 C 0.7323(8) 1.0567(3) 0.6178(4) 0.0416(13) Uani 1 1 d . . .
C8 C 0.7209(9) 1.1192(3) 0.6681(4) 0.0497(15) Uani 1 1 d . . .
C9 C 0.8834(12) 0.3027(4) 0.5529(6) 0.087(3) Uani 1 1 d . . .
H9A H 0.9067 0.2656 0.5978 0.104 Uiso 1 1 calc R . .
H9B H 1.0041 0.3285 0.5451 0.104 Uiso 1 1 calc R . .
C10 C 0.8104(16) 0.2753(5) 0.4576(7) 0.106(3) Uani 1 1 d . . .
H10A H 0.8681 0.3011 0.4055 0.128 Uiso 1 1 calc R . .
H10B H 0.8467 0.2275 0.4506 0.128 Uiso 1 1 calc R . .
C11 C 0.6003(16) 0.2824(7) 0.4560(7) 0.127(4) Uani 1 1 d . . .
H11A H 0.5376 0.2385 0.4450 0.152 Uiso 1 1 calc R . .
H11B H 0.5594 0.3140 0.4062 0.152 Uiso 1 1 calc R . .
C12 C 0.5486(12) 0.3100(5) 0.5530(7) 0.095(3) Uani 1 1 d . . .
H12A H 0.4369 0.3407 0.5488 0.113 Uiso 1 1 calc R . .
H12B H 0.5172 0.2730 0.5966 0.113 Uiso 1 1 calc R . .
C13 C 0.7439(16) 0.4156(4) 0.5441(9) 0.141(5) Uani 1 1 d . . .
H13A H 0.8756 0.4320 0.5538 0.212 Uiso 1 1 calc R . .
H13B H 0.6531 0.4461 0.5745 0.212 Uiso 1 1 calc R . .
H13C H 0.7156 0.4136 0.4768 0.212 Uiso 1 1 calc R . .
C14 C 0.7250(16) 0.3511(5) 0.6931(7) 0.115(4) Uani 1 1 d . . .
H14A H 0.7152 0.3058 0.7194 0.172 Uiso 1 1 calc R . .
H14B H 0.6152 0.3781 0.7137 0.172 Uiso 1 1 calc R . .
H14C H 0.8450 0.3721 0.7147 0.172 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'
S S 0.1246 0.1234 '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
S3 Ni1 S4 92.62(6) . . ?
S3 Ni1 S1 86.51(7) . . ?
S4 Ni1 S1 178.79(8) . . ?
S3 Ni1 S2 177.39(7) . . ?
S4 Ni1 S2 88.26(6) . . ?
S1 Ni1 S2 92.65(7) . . ?
C2 S1 Ni1 103.3(2) . . ?
C3 S2 Ni1 103.5(2) . . ?
C6 S3 Ni1 103.2(2) . . ?
C7 S4 Ni1 103.13(19) . . ?
C9 N5 C13 110.5(7) . . ?
C9 N5 C12 102.6(7) . . ?
C13 N5 C12 113.6(7) . . ?
C9 N5 C14 110.4(6) . . ?
C13 N5 C14 110.2(8) . . ?
C12 N5 C14 109.3(7) . . ?
N1 C1 C2 177.4(10) . . ?
C3 C2 C1 121.3(7) . . ?
C3 C2 S1 121.3(5) . . ?
C1 C2 S1 117.5(5) . . ?
C2 C3 C4 122.7(6) . . ?
C2 C3 S2 119.3(5) . . ?
C4 C3 S2 118.0(5) . . ?
N2 C4 C3 178.9(9) . . ?
N3 C5 C6 177.4(9) . . ?
C7 C6 C5 121.4(6) . . ?
C7 C6 S3 120.9(5) . . ?
C5 C6 S3 117.8(5) . . ?
C6 C7 C8 120.4(5) . . ?
C6 C7 S4 120.2(5) . . ?
C8 C7 S4 119.4(4) . . ?
N4 C8 C7 179.6(8) . . ?
N5 C9 C10 104.1(7) . . ?
C11 C10 C9 107.5(8) . . ?
C10 C11 C12 105.0(8) . . ?
N5 C12 C11 105.0(7) . . ?
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 S3 2.1383(17) . ?
Ni1 S4 2.1469(15) . ?
Ni1 S1 2.1474(16) . ?
Ni1 S2 2.1503(17) . ?
S1 C2 1.714(7) . ?
S2 C3 1.732(6) . ?
S3 C6 1.704(6) . ?
S4 C7 1.706(6) . ?
N1 C1 1.134(9) . ?
N2 C4 1.157(9) . ?
N3 C5 1.137(9) . ?
N4 C8 1.143(7) . ?
N5 C9 1.473(9) . ?
N5 C13 1.481(9) . ?
N5 C12 1.483(10) . ?
N5 C14 1.522(10) . ?
C1 C2 1.428(9) . ?
C2 C3 1.371(8) . ?
C3 C4 1.413(9) . ?
C5 C6 1.435(9) . ?
C6 C7 1.366(8) . ?
C7 C8 1.425(8) . ?
C9 C10 1.532(12) . ?
C10 C11 1.451(13) . ?
C11 C12 1.519(12) . ?
