Ferroelectricity and Piezoelectricity in Free-Standing Polycrystalline Films of Plastic Crystals.
Harada, Jun; Yoneyama, Naho; Yokokura, Seiya; Takahashi, Yukihiro; Miura, Atsushi; Kitamura, Noboru; Inabe, Tamotsu; Journal of the American Chemical Society  (2017) –; doi:10.1021/jacs.7b10539

data_4126953
_publ_section_title
;
 Ferroelectricity and Piezoelectricity in Free-Standing Polycrystalline
 Films of Plastic Crystals.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.7b10539
_journal_year                    2017
_chemical_formula_moiety         'Cl4 Fe, 0.5(C8 H12 N2)'
_chemical_formula_sum            'C4 H12 Cl4 Fe N'
_chemical_formula_weight         271.80
_space_group_crystal_system      orthorhombic
_space_group_IT_number           28
_space_group_name_Hall           'P 2 -2a'
_space_group_name_H-M_alt        'P m a 2'
_symmetry_space_group_name_Hall  'P 2 -2a'
_symmetry_space_group_name_H-M   'P m a 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2017-08-03
_audit_creation_method
;
Olex2 1.2
(compiled 2017.07.20 svn.r3457 for OlexSys, GUI svn.r5370)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.268(5)
_cell_length_b                   6.442(2)
_cell_length_c                   6.451(2)
_cell_measurement_reflns_used    5996
_cell_measurement_temperature    300
_cell_measurement_theta_max      27.346
_cell_measurement_theta_min      2.855
_cell_volume                     592.9(3)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'Bruker APEX2 2014.1-1 (Bruker, 2014)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      300
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_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  0.0154
_diffrn_reflns_av_unetI/netI     0.0174
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            8298
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.508
_diffrn_reflns_theta_min         2.855
_diffrn_source                   'rotating-anode X-ray tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.117
_exptl_absorpt_correction_T_max  0.7041
_exptl_absorpt_correction_T_min  0.6083
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/4 (Bruker,2014/4) was used for absorption correction. wR2(int) was 0.0873 before and 0.0412 after correction. The Ratio of minimum to maximum transmission is 0.8639. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.522
_exptl_crystal_description       block
_exptl_crystal_F_000             274
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.188
_exptl_crystal_size_min          0.125
_refine_diff_density_max         0.241
_refine_diff_density_min         -0.170
_refine_diff_density_rms         0.048
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.06(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     74
_refine_ls_number_reflns         1419
_refine_ls_number_restraints     49
_refine_ls_restrained_S_all      1.161
_refine_ls_R_factor_all          0.0249
_refine_ls_R_factor_gt           0.0246
_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^)+(0.0465P)^2^+0.0512P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0714
_refine_ls_wR_factor_ref         0.0720
_reflns_Friedel_coverage         0.837
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.997
_reflns_number_gt                1397
_reflns_number_total             1419
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b10539_si_003.cif
_cod_data_source_block           TMA_FeCl4_300K
_cod_original_cell_volume        592.9(4)
_cod_database_code               4126953
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.778
_shelx_estimated_absorpt_t_min   0.620
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.94(3)
 0.06(3)
2. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
3. 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
4. Others
 Fixed Sof: C1(0.5) H1A(0.5) H1B(0.5) H1C(0.5) C2(0.5) H2A(0.5) H2B(0.5)
 H2C(0.5) C3(0.5) H3A(0.5) H3B(0.5) H3C(0.5) C4(0.5) H4A(0.5) H4B(0.5) H4C(0.5)
5.a Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C4(H4A,H4B,H4C)
;
_olex2_submission_special_instructions 'No special instructions were received'