Room-temperature antiferroelectric in hybrid perovskite enables highly-efficient energy storage at low electric fields
Liu, Yi; Xu, Haojie; Liu, Xitao; Han, Shiguo; Guo, Wuqian; Ma, Yu; Fan, Qingshun; Hu, Xinxin; Sun, Zhihua; Luo, Junhua; Chemical Science  (2022) –; doi:10.1039/D2SC05285G

data_1567879
_publ_section_title
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 Room-temperature antiferroelectric in hybrid perovskite enables
 highly-efficient energy storage at low electric fields
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D2SC05285G
_journal_year                    2022
_chemical_formula_moiety         '0.5(Br14 Pb4), 2(C4 H12 N), C H5 N2'
_chemical_formula_sum            'C9 H29 Br7 N4 Pb2'
_chemical_formula_weight         1167.11
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2021-10-01
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-03-10 deposited with the CCDC.	2022-10-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.3299(4)
_cell_length_b                   37.549(3)
_cell_length_c                   8.4639(5)
_cell_measurement_reflns_used    5443
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      27.423
_cell_measurement_theta_min      2.905
_cell_volume                     2647.3(3)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_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    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      200.0
_diffrn_detector                 'Bruker APEX3 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX3 area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0758
_diffrn_reflns_av_unetI/netI     0.0517
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       43
_diffrn_reflns_limit_k_min       -48
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            21033
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.498
_diffrn_reflns_theta_min         2.467
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    23.269
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.2918
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1415 before and 0.0761 after correction. The Ratio of minimum to maximum transmission is 0.3914. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.928
_exptl_crystal_description       plate
_exptl_crystal_F_000             2080
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.056
_refine_diff_density_min         -1.763
_refine_diff_density_rms         0.311
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     109
_refine_ls_number_reflns         3070
_refine_ls_number_restraints     38
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0774
_refine_ls_R_factor_gt           0.0554
_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^)+(0.0697P)^2^+39.4185P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1474
_refine_ls_wR_factor_ref         0.1605
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2289
_reflns_number_total             3070
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc05285g2.cif
_cod_data_source_block           x1
_cod_database_code               1567879
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.389
_shelx_estimated_absorpt_t_min   0.204
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 3(10)
 -2(10)
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
3. Restrained distances
 N1-C1 = N2-C1
 1.35 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
N1 \\sim C1 \\sim N2: within 2A with sigma of 0.01 and sigma for terminal atoms
of 0.02
N3 \\sim C2 \\sim C3 \\sim C4 \\sim C5: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02
5.a Riding coordinates:
 N3(H3A,H3B,H3C), N1(H1A,H1B), N2(H2C,H2D)
5.b Ternary CH refined with riding coordinates:
 C3(H3)
5.c Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B)
5.d Aromatic/amide H refined with riding coordinates:
 C1(H1)
5.e Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C5(H5A,H5B,H5C)
;
_olex2_submission_special_instructions 'No special instructions were received'