#------------------------------------------------------------------------------
#$Date: 2021-08-01 02:53:19 +0300 (Sun, 01 Aug 2021) $
#$Revision: 267874 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/56/43/1564303.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_1564303
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_moiety         'C8 N4 Ni S4, C6 N'
_chemical_formula_sum            'C14 H N5 Ni S4'
_chemical_formula_weight         426.15
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_audit_creation_date             2021-01-27
_audit_creation_method
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.054(3)
_cell_length_b                   7.0712(12)
_cell_length_c                   18.941(4)
_cell_measurement_reflns_used    2712
_cell_measurement_temperature    353.15
_cell_measurement_theta_max      17.69
_cell_measurement_theta_min      2.54
_cell_volume                     2016.3(7)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_diffrn_ambient_temperature      353.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1919
_diffrn_reflns_av_unetI/netI     0.1615
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            19785
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.701
_diffrn_reflns_theta_min         1.728
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.380
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6055
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0673 before and 0.0499 after correction.
The Ratio of minimum to maximum transmission is 0.8121.
The λ/2 correction factor is Not present.
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.404
_exptl_crystal_description       plate
_exptl_crystal_F_000             848
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.667
_refine_diff_density_min         -0.583
_refine_diff_density_rms         0.245
_refine_ls_extinction_coef       0.027(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     140
_refine_ls_number_reflns         2521
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.3065
_refine_ls_R_factor_gt           0.1049
_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)+(0.1319P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2042
_refine_ls_wR_factor_ref         0.2965
_reflns_Friedel_coverage         0.000
_reflns_number_gt                786
_reflns_number_total             2521
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            jp1c04863_si_004.cif
_cod_data_source_block           1
_cod_original_cell_volume        2016.3(6)
_cod_database_code               1564303
_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.
;
_olex2_refinement_description
;
1. Restrained distances
 N5-C9 = N5-C11
 1.4 with sigma of 0.02
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_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_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 0.53820(12) 0.2500 0.54523(9) 0.0994(10) Uani 1 2 d S T P . .
S1 S 0.4834(3) 0.2500 0.44164(17) 0.1046(14) Uani 1 2 d S T P . .
S2 S 0.4096(3) 0.2500 0.5929(2) 0.1235(15) Uani 1 2 d S T P . .
S3 S 0.6679(3) 0.2500 0.4976(2) 0.1130(14) Uani 1 2 d S T P . .
S4 S 0.5920(4) 0.2500 0.6499(2) 0.1420(18) Uani 1 2 d S T P . .
N1 N 0.2705(12) 0.2500 0.3481(11) 0.182(7) Uani 1 2 d S T P . .
N2 N 0.1728(13) 0.2500 0.5473(13) 0.223(10) Uani 1 2 d S T P . .
N3 N 0.9075(14) 0.2500 0.5478(16) 0.259(13) Uani 1 2 d S T P . .
N4 N 0.806(2) 0.2500 0.7413(13) 0.39(2) Uani 1 2 d S T P . .
C1 C 0.3130(12) 0.2500 0.3949(11) 0.131(6) Uani 1 2 d S T P . .
C2 C 0.3714(11) 0.2500 0.4553(11) 0.112(5) Uani 1 2 d S T P . .
C3 C 0.3417(12) 0.2500 0.5207(13) 0.131(6) Uani 1 2 d S T P . .
C4 C 0.2477(16) 0.2500 0.5338(12) 0.149(6) Uani 1 2 d S T P . .
C5 C 0.835(2) 0.2500 0.5531(14) 0.193(10) Uani 1 2 d S T P . .
C6 C 0.7351(15) 0.2500 0.5683(13) 0.135(7) Uani 1 2 d S T P . .
C7 C 0.7062(15) 0.2500 0.6307(13) 0.146(7) Uani 1 2 d S T P . .
C8 C 0.762(2) 0.2500 0.6925(13) 0.227(11) Uani 1 2 d S T P . .
N5 N 0.9838(19) 0.2500 0.3216(14) 0.258(14) Uani 1 2 d DS T P . .
C9 C 0.966(2) 0.051(3) 0.3243(19) 0.39(2) Uani 1 1 d D . . . .
C12 C 1.029(2) 0.2500 0.3919(19) 0.32(2) Uani 1 2 d S T P . .
C11 C 1.037(2) 0.2500 0.2572(16) 0.34(3) Uani 1 2 d DS T P . .
C10 C 0.867(2) 0.158(4) 0.333(2) 0.41(3) Uani 1 1 d . . . . .
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
S1 Ni1 S2 92.23(18) . . ?
S1 Ni1 S3 88.00(17) . . ?
S1 Ni1 S4 179.4(2) . . ?
S2 Ni1 S3 179.77(19) . . ?
S2 Ni1 S4 87.2(2) . . ?
S4 Ni1 S3 92.6(2) . . ?
C2 S1 Ni1 104.0(7) . . ?
C3 S2 Ni1 101.7(8) . . ?
C6 S3 Ni1 102.3(10) . . ?
C7 S4 Ni1 100.3(8) . . ?
N1 C1 C2 178(2) . . ?
C1 C2 S1 118.8(14) . . ?
C3 C2 S1 118.6(15) . . ?
C3 C2 C1 122.6(16) . . ?
C2 C3 S2 123.4(15) . . ?
C2 C3 C4 120(2) . . ?
C4 C3 S2 116.8(18) . . ?
N2 C4 C3 177(3) . . ?
N3 C5 C6 174(3) . . ?
C5 C6 S3 116(2) . . ?
C7 C6 S3 123(2) . . ?
C7 C6 C5 121(2) . . ?
C6 C7 S4 122.1(18) . . ?
C6 C7 C8 124(2) . . ?
C8 C7 S4 114(2) . . ?
N4 C8 C7 180(3) . . ?
C9 N5 C9 158(4) 7_565 . ?
C9 N5 C12 93(2) . . ?
C9 N5 C12 93(2) 7_565 . ?
C9 N5 C11 97.7(19) 7_565 . ?
C9 N5 C11 97.7(19) . . ?
C9 N5 C10 99(3) . 7_565 ?
C9 N5 C10 58.8(16) 7_565 7_565 ?
C12 N5 C10 109(2) . 7_565 ?
C11 N5 C12 119(3) . . ?
C11 N5 C10 127(2) . 7_565 ?
N5 C9 C10 74.2(19) . . ?
C10 C10 C9 116.9(13) 7_565 . ?
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 S1 2.128(4) . ?
Ni1 S2 2.137(5) . ?
Ni1 S3 2.151(4) . ?
Ni1 S4 2.141(5) . ?
S1 C2 1.706(17) . ?
S2 C3 1.71(2) . ?
S3 C6 1.68(2) . ?
S4 C7 1.76(2) . ?
N1 C1 1.09(2) . ?
N2 C4 1.16(2) . ?
N3 C5 1.10(3) . ?
N4 C8 1.14(3) . ?
C1 C2 1.44(2) . ?
C2 C3 1.32(2) . ?
C3 C4 1.44(2) . ?
C5 C6 1.53(4) . ?
C6 C7 1.26(2) . ?
C7 C8 1.45(3) . ?
N5 C9 1.435(19) . ?
N5 C9 1.435(19) 7_565 ?
N5 C12 1.50(4) . ?
N5 C11 1.461(18) . ?
N5 C10 1.89(4) 7_565 ?
C9 C10 1.68(3) . ?
C10 C10 1.29(6) 7_565 ?
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 C1 180.000(2) . . . . ?
Ni1 S1 C2 C3 0.000(3) . . . . ?
Ni1 S2 C3 C2 0.000(3) . . . . ?
Ni1 S2 C3 C4 180.000(3) . . . . ?
Ni1 S3 C6 C5 180.000(4) . . . . ?
Ni1 S3 C6 C7 0.000(4) . . . . ?
Ni1 S4 C7 C6 0.000(4) . . . . ?
Ni1 S4 C7 C8 180.000(5) . . . . ?
S1 C2 C3 S2 0.000(3) . . . . ?
S1 C2 C3 C4 180.000(3) . . . . ?
S3 C6 C7 S4 0.000(4) . . . . ?
S3 C6 C7 C8 180.000(6) . . . . ?
C1 C2 C3 S2 180.000(2) . . . . ?
C1 C2 C3 C4 0.000(5) . . . . ?
C5 C6 C7 S4 180.000(2) . . . . ?
C5 C6 C7 C8 0.000(6) . . . . ?
N5 C9 C10 C10 -1(2) . . . 7_565 ?
C9 N5 C9 C10 4(11) 7_565 . . . ?
C12 N5 C9 C10 111(3) . . . . ?
C11 N5 C9 C10 -129(3) . . . . ?
C10 N5 C9 C10 0.6(15) 7_565 . . . ?
