Organic ammonium modulated mixed-valence multiferroics exhibiting large spontaneous strain and exchange bias.
Yan, Qin-Yuan; Han, Song-De; Xu, Ting; Ji, Cui-Xian; Lv, Lin-Lin; Yao, Zhao-Quan; Zhao, Jiong-Peng; Liu, Fu-Chen; Chemical communications (Cambridge, England) 61 (2025) 16412–16415; doi:10.1039/d5cc03844h

data_7134983
_publ_section_title
;
 Organic ammonium modulated mixed-valence multiferroics exhibiting large
 spontaneous strain and exchange bias.
;
_journal_issue                   84
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              16412
_journal_page_last               16415
_journal_paper_doi               10.1039/d5cc03844h
_journal_volume                  61
_journal_year                    2025
_chemical_formula_moiety         'C9 H9 Fe3 O18, C3 H12 N2, H2 O'
_chemical_formula_sum            'C12 H23 Fe3 N2 O19'
_chemical_formula_weight         666.87
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2025-06-02
_audit_creation_method
;
Olex2 1.5-ac6-020
(compiled 2024.02.14 svn.r2f8d729c for Rigaku Oxford Diffraction, GUI svn.r6966)
;
_audit_update_record
;
2025-07-07 deposited with the CCDC.	2025-09-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.732(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.2657(10)
_cell_length_b                   8.2582(5)
_cell_length_c                   21.5884(12)
_cell_measurement_reflns_used    8565
_cell_measurement_temperature    110.00(10)
_cell_measurement_theta_max      30.0410
_cell_measurement_theta_min      3.2670
_cell_volume                     2480.8(3)
_computing_cell_refinement       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5-ac6-020 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-ac6-020 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      110.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.901
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -29.00   0.00   0.50    3.32    --    0.00 -37.00  60.00   58
  2  \w    -34.00   1.00   0.50    3.32    --    0.00  77.00 -90.00   70
  3  \w     16.00  88.00   0.50    3.32    --    0.00  77.00 -90.00  144
  4  \w    -28.00  49.00   0.50    3.32    --    0.00  57.00 150.00  154
  5  \w    -13.00  12.00   0.50    3.32    --    0.00  57.00   0.00   50
  6  \w     57.00  87.00   0.50    3.32    --    0.00  57.00   0.00   60
  7  \w    -89.00 -50.00   0.50    3.32    --    0.00 -37.00  60.00   78
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa dual offset/far'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0428318000
_diffrn_orient_matrix_UB_12      -0.0393792000
_diffrn_orient_matrix_UB_13      -0.0157186000
_diffrn_orient_matrix_UB_21      -0.0246094000
_diffrn_orient_matrix_UB_22      0.0337035000
_diffrn_orient_matrix_UB_23      0.0221405000
_diffrn_orient_matrix_UB_31      -0.0125798000
_diffrn_orient_matrix_UB_32      0.0684594000
_diffrn_orient_matrix_UB_33      -0.0199545000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0428
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.901
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            6438
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.901
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.863
_diffrn_reflns_theta_min         3.129
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.819
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.69218
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            BLACK
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.786
_exptl_crystal_description       block
_exptl_crystal_F_000             1356
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.11
_refine_diff_density_max         2.287
_refine_diff_density_min         -1.323
_refine_diff_density_rms         0.221
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.117
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     328
_refine_ls_number_reflns         6438
_refine_ls_number_restraints     72
_refine_ls_restrained_S_all      1.115
_refine_ls_R_factor_all          0.0863
_refine_ls_R_factor_gt           0.0764
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0921P)^2^+21.8890P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2293
_refine_ls_wR_factor_ref         0.2352
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5227
_reflns_number_total             6438
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc03844h2.cif
_cod_data_source_block           1LTP
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_crystal_colour_primary' value 'BLACK' was changed
to 'black' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas 

 Adding full bibliography for 7134983--7134988.cif.
;
_cod_database_code               7134983
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.825
_shelx_estimated_absorpt_t_min   0.712
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.578(5)
 0.422(5)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H) groups, All N(H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
3. Uiso/Uaniso restraints and constraints
O5 \\sim O4 \\sim C5 \\sim C10: within 3.8A with sigma of 0.01 and sigma for
terminal atoms of 0.03 within 3.8A
Uanis(C6) \\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(O5) \\sim Ueq, Uanis(O9) \\sim
Ueq, Uanis(C4) \\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(O4)
\\sim Ueq, Uanis(O15) \\sim Ueq: with sigma of 0.001 and sigma for terminal
atoms of 0.002
4.a Riding coordinates:
 O1(H1F,H1G)
4.b Secondary CH2 refined with riding coordinates:
 N2(H2A,H2B), C1(H1D,H1E), C2(H2C,H2D)
4.c Aromatic/amide H refined with riding coordinates:
 C9(H9), C5(H5), C10(H10), C7(H7), C8(H8), C6(H6), C12(H12), C11(H11), C4(H4)
4.d Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C), C3(H3A,H3B,H3C)
;
_shelx_res_checksum              51962
_shelx_hkl_checksum              98895
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.502
_oxdiff_exptl_absorpt_empirical_full_min 0.757