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_7127058
_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_absolute_configuration unk
_chemical_formula_moiety         'C20 H22 Fe N O5 S'
_chemical_formula_sum            'C20 H22 Fe N O5 S'
_chemical_formula_weight         444.31
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_symmetry_Int_Tables_number      9
_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                 128.002(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.1583(10)
_cell_length_b                   17.6762(5)
_cell_length_c                   8.0886(5)
_cell_measurement_reflns_used    9236
_cell_measurement_temperature    298
_cell_measurement_theta_max      29.7530
_cell_measurement_theta_min      2.3330
_cell_volume                     2045.8(3)
_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 0.9098
_diffrn_measured_fraction_theta_max 0.9098
_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    -28.00 109.00   0.50   40.00    --   20.00  54.00   0.00  274
  2  \w     67.00  93.00   0.50   40.00    --   20.00  54.00-120.00   52
  3  \w    -73.00 -46.00   0.50   40.00    --   20.00  54.00  60.00   54
  4  \w    -31.00 108.00   0.50   40.00    --   20.00  54.00  60.00  278
  5  \w    -74.00 -15.00   0.50   40.00    --   20.00  54.00 150.00  118
  6  \w     16.00 108.00   0.50   40.00    --   20.00  54.00 150.00  184
  7  \w    -73.00 -48.00   0.50   40.00    --   20.00  54.00-150.00   50
  8  \w    -72.00 -47.00   0.50   40.00    --   20.00  54.00  90.00   50
  9  \w      0.00  26.00   0.50   40.00    --   20.00  54.00  90.00   52
 10  \w    -71.00 -46.00   0.50   40.00    --   20.00  54.00   0.00   50
 11  \w      2.00  58.00   0.50   10.00    --   20.00  54.00 120.00  112
 12  \w     63.00 110.00   0.50   10.00    --   20.00  54.00 120.00   94
 13  \w    -71.00 -45.00   0.50   10.00    --   20.00  54.00  90.00   52
 14  \w     41.00  67.00   0.50   10.00    --   20.00  54.00  90.00   52
 15  \w    -72.00 -46.00   0.50   10.00    --   20.00  54.00 -30.00   52
 16  \w     23.00  49.00   0.50   10.00    --   20.00  54.00 -30.00   52
 17  \w    -70.00 -44.00   0.50   10.00    --   20.00  54.00-180.00   52
 18  \w     -2.00  24.00   0.50   10.00    --   20.00  54.00-180.00   52
 19  \w     15.00  51.00   0.50   10.00    --   20.00  54.00-150.00   72
 20  \w    -64.00 -38.00   0.50   10.00    --   20.00  54.00   0.00   52
 21  \w    -64.00 -16.00   0.50   10.00    --   20.00  54.00 120.00   96
 22  \w     -4.00  22.00   0.50   20.00    --   20.00  54.00 120.00   52
 23  \w     61.00 109.50   0.50   20.00    --   20.00  54.00 120.00   97
 24  \w    -70.00 -19.00   0.50   20.00    --   20.00  54.00-180.00  102
 25  \w    -71.00 -45.00   0.50   20.00    --   20.00  54.00 -30.00   52
 26  \w     -1.00  25.00   0.50   20.00    --   20.00  54.00 -30.00   52
 27  \w    -61.00 -35.00   0.50   20.00    --   20.00  54.00  60.00   52
 28  \w    -64.00 -38.00   0.50   20.00    --   20.00  54.00   0.00   52
 29  \w    -63.00 -37.00   0.50   20.00    --   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      0.0000154000
_diffrn_orient_matrix_UB_12      -0.0400465000
_diffrn_orient_matrix_UB_13      0.0062537000
_diffrn_orient_matrix_UB_21      0.0179514000
_diffrn_orient_matrix_UB_22      0.0026448000
_diffrn_orient_matrix_UB_23      0.1063427000
_diffrn_orient_matrix_UB_31      -0.0461838000
_diffrn_orient_matrix_UB_32      0.0010218000
_diffrn_orient_matrix_UB_33      -0.0321626000
_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  0.0267
_diffrn_reflns_av_unetI/netI     0.0182
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            18664
_diffrn_reflns_theta_full        27.4818
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.30
_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    0.870
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.93444
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.45i (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    1.4425
_exptl_crystal_description       block
_exptl_crystal_F_000             926.3333
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.1520
_refine_diff_density_min         -0.1357
_refine_diff_density_rms         0.0385
_refine_ls_abs_structure_details
'Flack, H. D. (1983). Acta Cryst. A39, 876-881.'
_refine_ls_abs_structure_Flack   0.009(10)
_refine_ls_d_res_high            0.7701
_refine_ls_d_res_low             8.8381
_refine_ls_goodness_of_fit_ref   1.0335
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    38
_refine_ls_number_parameters     275
_refine_ls_number_reflns         4266
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.0335
_refine_ls_R_factor_all          0.0256
_refine_ls_R_factor_gt           0.0235
_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^)+(0.0432P)^2^+0.0872P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0620
_refine_ls_wR_factor_ref         0.0630
_reflns_Friedel_coverage         0.828
_reflns_limit_h_max              23
_reflns_limit_h_min              -22
_reflns_limit_k_max              22
_reflns_limit_k_min              -22
_reflns_limit_l_max              10
_reflns_limit_l_min              -10
_reflns_number_gt                4051
_reflns_number_total             4266
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d0cc04497k2.cif
_cod_data_source_block           2a
_cod_depositor_comments
'Adding full bibliography for 7127058--7127059.cif.'
_cod_original_sg_symbol_Hall     ' C -2yc'
_cod_database_code               7127058
_chemical_oxdiff_formula         'C20 N1 O5 S1 Fe1'
_chemical_oxdiff_usercomment     298K
_reflns_odcompleteness_completeness 99.05
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_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. Others
 Fixed Sof: N1b(0.5) C7b(0.5) H7b(0.5) N1a(0.5) C7a(0.5) H7a(0.5)
3.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C12(H12), C3(H3), C16(H16), C11(H11), C5(H5), C4(H4), C9(H9),
 C10(H10), C7b(H7b), C7a(H7a)
3.b Idealised Me refined as rotating group:
 C19(H19a,H19b,H19c), C20(H20a,H20b,H20c), C14(H14a,H14b,H14c), C18(H18a,H18b,
 H18c)
;
_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 1.117
_oxdiff_exptl_absorpt_empirical_full_min 0.897