Solvent vapor-induced polarity and ferroelectricity switching.
Kobayashi, Fumiya; Akiyoshi, Ryohei; Kosumi, Daisuke; Nakamura, Masaaki; Lindoy, Leonard F.; Hayami, Shinya; Chemical communications (Cambridge, England) 56 (2020) 10509–10512; doi:10.1039/d0cc04497k

data_7127059
_publ_section_title
;
 Solvent vapor-induced polarity and ferroelectricity switching.
;
_journal_issue                   72
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              10509
_journal_page_last               10512
_journal_paper_doi               10.1039/d0cc04497k
_journal_volume                  56
_journal_year                    2020
_chemical_formula_moiety         'C23 H21 Fe N2 O4, C2.5 H2.5 N0.5'
_chemical_formula_sum            'C25.5 H23.5 Fe N2.5 O4'
_chemical_formula_weight         484.83
_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'
_symmetry_Int_Tables_number      14
_atom_sites_solution_primary     dual
_audit_creation_date             2020-03-22
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-04-14 deposited with the CCDC.	2020-08-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 111.89(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.3501(19)
_cell_length_b                   19.938(3)
_cell_length_c                   12.331(2)
_cell_measurement_reflns_used    2792
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      25.9730
_cell_measurement_theta_min      2.2650
_cell_volume                     2133.0(7)
_computing_cell_refinement       'CrysAlisPro 1.171.39.45i (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.45i (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.45i (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      298
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku Saturn724+'
_diffrn_measured_fraction_theta_full 0.9915
_diffrn_measured_fraction_theta_max 0.9915
_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    -25.00 110.00   0.50   60.00    --   20.00  54.00 120.00  270
  2  \w    -74.00 -38.00   0.50   60.00    --   20.00  54.00  30.00   72
  3  \w     10.00  45.00   0.50   60.00    --   20.00  54.00  30.00   70
  4  \w     84.00 110.00   0.50   60.00    --   20.00  54.00  30.00   52
  5  \w    -15.00  13.00   0.50   60.00    --   20.00  54.00 -60.00   56
  6  \w     23.00 108.00   0.50   60.00    --   20.00  54.00 -60.00  170
  7  \w    -74.00 -49.00   0.50   60.00    --   20.00  54.00-180.00   50
  8  \w      2.00  51.00   0.50   60.00    --   20.00  54.00-180.00   98
  9  \w     64.00  89.00   0.50   60.00    --   20.00  54.00-180.00   50
 10  \w    -64.00 -37.00   0.50   60.00    --   20.00  54.00  60.00   54
 11  \w    -26.00  -1.00   0.50   60.00    --   20.00  54.00  60.00   50
 12  \w     25.00  50.00   0.50   60.00    --   20.00  54.00  60.00   50
 13  \w    -67.00 -42.00   0.50   60.00    --   20.00  54.00 150.00   50
 14  \w     16.00  42.00   0.50   60.00    --   20.00  54.00 150.00   52
 15  \w    -71.00 -45.00   0.50   60.00    --   20.00  54.00 120.00   52
;
_diffrn_measurement_device       'two-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Mini II'
_diffrn_measurement_method       '\w scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0051226000
_diffrn_orient_matrix_UB_12      0.0354152000
_diffrn_orient_matrix_UB_13      0.0030345000
_diffrn_orient_matrix_UB_21      0.0127831000
_diffrn_orient_matrix_UB_22      0.0031104000
_diffrn_orient_matrix_UB_23      -0.0529102000
_diffrn_orient_matrix_UB_31      -0.0806360000
_diffrn_orient_matrix_UB_32      -0.0017731000
_diffrn_orient_matrix_UB_33      -0.0320769000
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0573
_diffrn_reflns_av_unetI/netI     0.0524
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            16956
_diffrn_reflns_theta_full        26.3683
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         2.36
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_target            Mo
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.746
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.59810
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.15 (Rigaku Oxford Diffraction, 2018)
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    1.5097
_exptl_crystal_description       block
_exptl_crystal_F_000             1009.8558
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.4414
_refine_diff_density_min         -0.4397
_refine_diff_density_rms         0.0865
_refine_ls_d_res_high            0.8001
_refine_ls_d_res_low             8.6346
_refine_ls_goodness_of_fit_ref   1.0139
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    46
_refine_ls_number_parameters     327
_refine_ls_number_reflns         4329
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.0131
_refine_ls_R_factor_all          0.0916
_refine_ls_R_factor_gt           0.0506
_refine_ls_shift/su_max          0.0000
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1001P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1368
_refine_ls_wR_factor_ref         0.1708
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              7
_reflns_limit_h_min              -11
_reflns_limit_k_max              24
_reflns_limit_k_min              0
_reflns_limit_l_max              15
_reflns_limit_l_min              -6
_reflns_number_gt                2689
_reflns_number_total             4329
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d0cc04497k2.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 7127058--7127059.cif.'
_cod_original_sg_symbol_Hall     '-P 2ybc (x-z,y,z)'
_cod_database_code               7127059
_chemical_oxdiff_formula         'Fe C20 N2 O4'
_chemical_oxdiff_usercomment     298K
_diffrn_oxdiff_ac4_digest_frames
;
01d94c3be668dbf1fb0f78bef6e3af389801196bfd1
;
_diffrn_oxdiff_ac4_digest_hkl
;
01f4de6664c0b5e05df67720e28c0842a599e3
;
_reflns_odcompleteness_completeness 99.07
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid bond restraints
 C26, C25, N3, C24
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Others
 Fixed Sof: N1a(0.5) C25(0.5) H25(0.5) C7a(0.5) H7a(0.5) N1b(0.5) C7b(0.5)
 H7b(0.5) N3(0.5)
4.a Aromatic/amide H refined with riding coordinates:
 C5(H5), C4(H4), C3(H3), C2(H2), C23(H23), C12(H12), C19(H19), C11(H11),
 C10(H10), C21(H21), C22(H22), C9(H9), C20(H20), C16(H16), C25(H25), C26(H26),
 C7a(H7a), C7b(H7b), C24(H24)
4.b Idealised Me refined as rotating group:
 C18(H18a,H18b,H18c), C14(H14a,H14b,H14c)
;
_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 1.777
_oxdiff_exptl_absorpt_empirical_full_min 0.759