#------------------------------------------------------------------------------
#$Date: 2021-08-01 02:54:00 +0300 (Sun, 01 Aug 2021) $
#$Revision: 267875 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/56/43/1564304.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_1564304
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           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P n m a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.3949(8)
_cell_length_b                   6.9372(3)
_cell_length_c                   19.6112(11)
_cell_measurement_reflns_used    4663
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.29
_cell_measurement_theta_min      2.51
_cell_volume                     1958.38(18)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0684
_diffrn_reflns_av_sigmaI/netI    0.0540
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            19362
_diffrn_reflns_theta_full        27.54
_diffrn_reflns_theta_max         27.54
_diffrn_reflns_theta_min         2.51
_exptl_absorpt_coefficient_mu    1.423
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.490
_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         0.275
_refine_diff_density_min         -0.375
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.173
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     141
_refine_ls_number_reflns         2430
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.173
_refine_ls_R_factor_all          0.1205
_refine_ls_R_factor_gt           0.0544
_refine_ls_shift/su_max          1.821
_refine_ls_shift/su_mean         0.029
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0584P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1128
_refine_ls_wR_factor_ref         0.1310
_reflns_number_gt                1383
_reflns_number_total             2430
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jp1c04863_si_003.cif
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      Pnma
_cod_database_code               1564304
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.03697(3) 0.7500 0.951998(19) 0.05967(13) Uani 1 2 d S . .
S3 S -0.00215(7) 0.7500 1.05747(4) 0.0651(2) Uani 1 2 d S . .
S1 S 0.17971(7) 0.7500 0.98366(5) 0.0745(3) Uani 1 2 d S . .
S4 S -0.10472(7) 0.7500 0.91904(5) 0.0789(3) Uani 1 2 d S . .
S2 S 0.07337(8) 0.7500 0.84614(5) 0.0830(3) Uani 1 2 d S . .
C5 C -0.1717(3) 0.7500 1.11817(19) 0.0815(12) Uani 1 2 d S . .
C2 C 0.2396(3) 0.7500 0.90716(19) 0.0821(12) Uani 1 2 d S . .
C6 C -0.1206(3) 0.7500 1.05449(17) 0.0674(10) Uani 1 2 d S . .
C3 C 0.1920(3) 0.7500 0.84759(18) 0.0874(13) Uani 1 2 d S . .
C7 C -0.1647(3) 0.7500 0.99401(18) 0.0733(11) Uani 1 2 d S . .
C8 C -0.2648(3) 0.7500 0.9894(2) 0.1032(15) Uani 1 2 d S . .
C1 C 0.3388(3) 0.7500 0.9095(2) 0.1096(16) Uani 1 2 d S . .
C4 C 0.2388(4) 0.7500 0.7830(2) 0.1276(18) Uani 1 2 d S . .
N1 N 0.4162(3) 0.7500 0.9098(3) 0.154(2) Uani 1 2 d S . .
N3 N -0.2111(2) 0.7500 1.16814(17) 0.1112(13) Uani 1 2 d S . .
N4 N -0.3425(3) 0.7500 0.9841(2) 0.1510(18) Uani 1 2 d S . .
N2 N 0.2736(4) 0.7500 0.7319(2) 0.206(3) Uani 1 2 d S . .
N5 N 0.9257(3) 0.7500 0.34766(18) 0.1347(16) Uani 1 2 d S . .
C9 C 0.9458(3) 0.9190(6) 0.3106(2) 0.1838(19) Uani 1 1 d . . .
H9A H 0.9529 1.0307 0.3399 0.221 Uiso 1 1 calc R . .
H9B H 0.8999 0.9452 0.2756 0.221 Uiso 1 1 calc R . .
C10 C 1.0419(3) 0.8483(7) 0.2797(3) 0.229(3) Uani 1 1 d . . .
H10A H 1.0492 0.8963 0.2336 0.275 Uiso 1 1 calc R . .
H10B H 1.0931 0.8963 0.3071 0.275 Uiso 1 1 calc R . .
C11 C 0.9725(6) 0.7500 0.4131(3) 0.250(4) Uani 1 2 d S . .
H11A H 1.0377 0.7277 0.4064 0.375 Uiso 0.50 1 calc PR . .
H11B H 0.9472 0.6498 0.4413 0.375 Uiso 0.50 1 calc PR . .
H11C H 0.9637 0.8725 0.4350 0.375 Uiso 0.50 1 calc PR . .
C12 C 0.8154(4) 0.7500 0.3521(3) 0.240(5) Uani 1 2 d S . .
H12A H 0.7957 0.6602 0.3864 0.361 Uiso 0.50 1 calc PR . .
H12B H 0.7899 0.7129 0.3088 0.361 Uiso 0.50 1 calc PR . .
H12C H 0.7940 0.8769 0.3637 0.361 Uiso 0.50 1 calc PR . .
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
S4 Ni1 S2 86.58(4) . . ?
S4 Ni1 S3 92.35(4) . . ?
S2 Ni1 S3 178.94(5) . . ?
S4 Ni1 S1 179.23(4) . . ?
S2 Ni1 S1 92.65(4) . . ?
S3 Ni1 S1 88.41(4) . . ?
C6 S3 Ni1 103.26(12) . . ?
C2 S1 Ni1 103.05(14) . . ?
C7 S4 Ni1 102.83(13) . . ?
C3 S2 Ni1 103.22(13) . . ?
N3 C5 C6 179.6(4) . . ?
C3 C2 C1 122.2(4) . . ?
C3 C2 S1 119.8(3) . . ?
C1 C2 S1 118.0(3) . . ?
C7 C6 C5 121.4(3) . . ?
C7 C6 S3 120.1(3) . . ?
C5 C6 S3 118.5(3) . . ?
C2 C3 C4 121.6(4) . . ?
C2 C3 S2 121.3(3) . . ?
C4 C3 S2 117.1(3) . . ?
C6 C7 C8 121.7(4) . . ?
C6 C7 S4 121.5(3) . . ?
C8 C7 S4 116.9(3) . . ?
N4 C8 C7 178.2(5) . . ?
N1 C1 C2 178.4(6) . . ?
N2 C4 C3 178.5(6) . . ?
C9 N5 C9 112.6(4) . 7_575 ?
C9 N5 C11 111.1(3) . . ?
C9 N5 C11 111.1(3) 7_575 . ?
C9 N5 C12 103.5(3) . . ?
C9 N5 C12 103.5(3) 7_575 . ?
C11 N5 C12 114.6(5) . . ?
N5 C9 C10 96.8(3) . . ?
C10 C10 C9 108.0(2) 7_575 . ?
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 S4 2.1396(11) . ?
Ni1 S2 2.1410(10) . ?
Ni1 S3 2.1437(9) . ?
Ni1 S1 2.1465(11) . ?
S3 C6 1.706(4) . ?
S1 C2 1.730(4) . ?
S4 C7 1.705(4) . ?
S2 C3 1.708(4) . ?
C5 N3 1.133(5) . ?
C5 C6 1.449(5) . ?
C2 C3 1.354(5) . ?
C2 C1 1.429(6) . ?
C6 C7 1.345(5) . ?
C3 C4 1.435(6) . ?
C7 C8 1.444(6) . ?
C8 N4 1.123(6) . ?
C1 N1 1.115(6) . ?
C4 N2 1.120(6) . ?
N5 C9 1.409(4) . ?
N5 C9 1.409(4) 7_575 ?
N5 C11 1.450(7) . ?
N5 C12 1.590(7) . ?
C9 C10 1.588(6) . ?
C10 C10 1.363(9) 7_575 ?
