High-Tc Fe-based ferroelectric compound with large spontaneous polarization and narrow bandgap
Tan, Yu-Xin; Ying, Ting-Ting; Fan, Xiao-Wei; Huang, Yan-Le; Wan, Ming-Yang; Wang, Fang-Xin; Li, Qiao-Lin; Wang, Meng-Na; New Journal of Chemistry 47 (2023) 20619–20625; doi:10.1039/D3NJ03461E

data_7062852
_publ_section_title
;
 High-Tc Fe-based ferroelectric compound with large spontaneous
 polarization and narrow bandgap
;
_journal_issue                   44
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              20619
_journal_page_last               20625
_journal_paper_doi               10.1039/D3NJ03461E
_journal_volume                  47
_journal_year                    2023
_chemical_formula_moiety         'Br4 Fe, C6 H16 N'
_chemical_formula_sum            'C6 H16 Br4 Fe N'
_chemical_formula_weight         477.69
_space_group_crystal_system      orthorhombic
_space_group_IT_number           36
_space_group_name_Hall           'C 2c -2'
_space_group_name_H-M_alt        'C m c 21'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2023-03-22
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2023-10-12 deposited with the CCDC.	2023-10-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.769(3)
_cell_length_b                   12.709(4)
_cell_length_c                   13.551(5)
_cell_measurement_reflns_used    430
_cell_measurement_temperature    400.0
_cell_measurement_theta_max      19.36
_cell_measurement_theta_min      3.20
_cell_volume                     1510.2(9)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_collection       'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      400.0
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.976
_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  0.1075
_diffrn_reflns_av_unetI/netI     0.1243
_diffrn_reflns_Laue_measured_fraction_full 0.978
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            4543
_diffrn_reflns_point_group_measured_fraction_full 0.935
_diffrn_reflns_point_group_measured_fraction_max 0.922
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.959
_diffrn_reflns_theta_min         3.198
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    11.544
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.4519
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1343 before and 0.0841 after correction.
The Ratio of minimum to maximum transmission is 0.6063.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'dull brownish brown'
_exptl_crystal_colour_lustre     dull
_exptl_crystal_colour_modifier   brownish
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    2.101
_exptl_crystal_description       block
_exptl_crystal_F_000             900
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.719
_refine_diff_density_min         -0.643
_refine_diff_density_rms         0.158
_refine_ls_abs_structure_details
;
 Flack x determined using 252 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.01(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     160
_refine_ls_number_reflns         1461
_refine_ls_number_restraints     296
_refine_ls_restrained_S_all      0.959
_refine_ls_R_factor_all          0.1223
_refine_ls_R_factor_gt           0.0689
_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^)+(0.0992P)^2^+4.0141P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1728
_refine_ls_wR_factor_ref         0.2296
_reflns_Friedel_coverage         0.808
_reflns_Friedel_fraction_full    0.887
_reflns_Friedel_fraction_max     0.864
_reflns_number_gt                834
_reflns_number_total             1461
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3nj03461e2.cif
_cod_data_source_block           1-HTP
_cod_depositor_comments
'Adding full bibliography for 7062852--7062853.cif.'
_cod_original_cell_volume        1510.4(9)
_cod_database_code               7062852
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.206
_shelx_estimated_absorpt_t_min   0.129
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C2-C3
 1.42 with sigma of 0.02
 C5-N8 = C7-N8
 1.49 with sigma of 0.02
 C3-C4
 1.47 with sigma of 0.02
 C4-N8
 1.6 with sigma of 0.02
 C6-N8
 1.5 with sigma of 0.02
 C1-C8
 1.42 with sigma of 0.02
 C8-C9
 1.47 with sigma of 0.02
 C9-N1
 1.6 with sigma of 0.02
 C10-N1 = C12-N1
 1.49 with sigma of 0.02
 C11-N1
 1.5 with sigma of 0.02
 C5-C7 = C6-C7
 2.42 with sigma of 0.04
 C4-C7
 2.66 with sigma of 0.04
 C1-C9
 2.51 with sigma of 0.04
 C5-C6
 2.41 with sigma of 0.04
 C4-C5
 2.26 with sigma of 0.04
 C10-C11
 2.41 with sigma of 0.04
 C9-C10
 2.26 with sigma of 0.04
 C8-N1 = C9-C11
 2.65 with sigma of 0.04
 C9-C12
 2.66 with sigma of 0.04
 C10-C12 = C11-C12
 2.42 with sigma of 0.04
 C2-C4
 2.51 with sigma of 0.04
 C3-N8 = C4-C6
 2.65 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 2A
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: C2(0.25) H2A(0.25) H2B(0.25) H2C(0.25) C3(0.25) H3A(0.25)
 H3B(0.25) C4(0.25) H4A(0.25) H4B(0.25) C5(0.25) H5A(0.25) H5B(0.25) H5C(0.25)
 C6(0.25) H6A(0.25) H6B(0.25) H6C(0.25) C7(0.25) H7A(0.25) H7B(0.25) H7C(0.25)
 N8(0.25) C1(0.25) H1A(0.25) H1B(0.25) H1C(0.25) C8(0.25) H8A(0.25) H8B(0.25)
 C9(0.25) H9A(0.25) H9B(0.25) C10(0.25) H10A(0.25) H10B(0.25) H10C(0.25)
 C11(0.25) H11A(0.25) H11B(0.25) H11C(0.25) C12(0.25) H12A(0.25) H12B(0.25)
 H12C(0.25) N1(0.25)
6.a Riding coordinates:
 C5(H5A,H5B,H5C), C7(H7A,H7B,H7C)
6.b Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C4(H4A,H4B), C8(H8A,H8B), C9(H9A,H9B)
6.c Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C6(H6A,H6B,H6C), C1(H1A,H1B,H1C), C10(H10A,H10B,H10C),
 C11(H11A,H11B,H11C), C12(H12A,H12B,H12C)
;
_olex2_submission_special_instructions 'No special instructions were received'