Plastic/Ferroelectric Crystals with Easily Switchable Polarization: Low-Voltage Operation, Unprecedentedly High Pyroelectric Performance, and Large Piezoelectric Effect in Polycrystalline Forms.
Harada, Jun; Kawamura, Yuto; Takahashi, Yukihiro; Uemura, Yohei; Hasegawa, Tatsuo; Taniguchi, Hiroki; Maruyama, Koji; Journal of the American Chemical Society 141 (2019) 9349–9357; doi:10.1021/jacs.9b03369

data_4128704
_publ_section_title
;
 Plastic/Ferroelectric Crystals with Easily Switchable Polarization:
 Low-Voltage Operation, Unprecedentedly High Pyroelectric Performance, and
 Large Piezoelectric Effect in Polycrystalline Forms.
;
_journal_issue                   23
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9349
_journal_page_last               9357
_journal_paper_doi               10.1021/jacs.9b03369
_journal_volume                  141
_journal_year                    2019
_chemical_formula_moiety         '2(O2 Re0.5), C5 H8 N1, C1 H4'
_chemical_formula_sum            'C6 H12 N O4 Re'
_chemical_formula_weight         348.37
_space_group_crystal_system      rhombohedral
_space_group_IT_number           160
_space_group_name_Hall           'P 3* -2'
_space_group_name_H-M_alt        'R 3 m :R'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2019-02-10
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                89.8460(10)
_cell_angle_beta                 89.8460(10)
_cell_angle_gamma                89.8460(10)
_cell_formula_units_Z            1
_cell_length_a                   6.1776(7)
_cell_length_b                   6.1776(7)
_cell_length_c                   6.1776(7)
_cell_measurement_reflns_used    2663
_cell_measurement_temperature    300
_cell_measurement_theta_max      26.881
_cell_measurement_theta_min      3.298
_cell_volume                     235.75(5)
_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    'Mercury (Macrae et al., 2006)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_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 1.000
_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  0.0341
_diffrn_reflns_av_unetI/netI     0.0173
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            3410
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.400
_diffrn_reflns_theta_min         3.298
_diffrn_source                   'rotating-anode X-ray tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    12.864
_exptl_absorpt_correction_T_max  0.4659
_exptl_absorpt_correction_T_min  0.3323
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/4 (Bruker,2014/4) was used for absorption correction. wR2(int) was 0.1009 before and 0.0417 after correction. The Ratio of minimum to maximum transmission is 0.7132. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.454
_exptl_crystal_description       block
_exptl_crystal_F_000             162
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.171
_refine_diff_density_min         -0.642
_refine_diff_density_rms         0.106
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.23(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.171
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     32
_refine_ls_number_reflns         421
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.185
_refine_ls_R_factor_all          0.0168
_refine_ls_R_factor_gt           0.0168
_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^)+(0.0267P)^2^+0.0124P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0415
_refine_ls_wR_factor_ref         0.0415
_reflns_Friedel_coverage         0.967
_reflns_Friedel_fraction_full    0.994
_reflns_Friedel_fraction_max     0.990
_reflns_number_gt                421
_reflns_number_total             421
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b03369_si_002.cif
_cod_data_source_block           1-ABCH_ReO4_300K
_cod_original_cell_volume        235.75(8)
_cod_original_sg_symbol_H-M      'R 3 m:r'
_cod_database_code               4128704
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.627
_shelx_estimated_absorpt_t_min   0.286
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.77(9)
 0.23(9)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
3. Shared sites
{C2, C3}
4. Restrained distances
 C3-H2
 0.97 with sigma of 0.02
5. Uiso/Uaniso restraints and constraints
Uanis(C2) = Uanis(C3)
6. 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
7. Others
 Fixed Sof: H1A(0.5) H1B(0.5) C2(0.33333) H3(0.16667) C3(0.16667) H2(0.66667)
8.a Ternary CH refined with riding coordinates:
 N1(H1N), C2(H3)
8.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B)
;
_olex2_submission_special_instructions 'No special instructions were received'