Two Ongoing Magnetic Transitions Originating from Spin-Peierls Dimerization and Cation Orientation Transformation in an S = 1/2 Spin Chain System
Qian, Yin; Yao, Wan-Wan; Shao, Dong-Sheng; Zhang, Jin; Ren, Xiao-Ming; The Journal of Physical Chemistry C  (2021) –; doi:10.1021/acs.jpcc.1c04863

data_1564303
_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       '\f and \w 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 \l/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+0.001xFc^2^\l^3^/sin(2\q)]^-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/[\s^2^(Fo^2^)+(0.1319P)^2^] where P=(Fo^2^+2Fc^2^)/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 > 2\s(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
_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'