Structural dimension engineering and high-temperature dielectric–optical switching in fluorine-substituted lead bromide hybrid perovskites
Gan, Tian; Xu, Zhe-Kun; Gan, Jia-Qi; Wang, Zhong-Xia; CrystEngComm 25 (2023) 5029–5034; doi:10.1039/D3CE00644A

data_7247228
_publ_section_title
;
 Structural dimension engineering and high-temperature dielectric--optical
 switching in fluorine-substituted lead bromide hybrid perovskites
;
_journal_issue                   35
_journal_name_full               CrystEngComm
_journal_page_first              5029
_journal_page_last               5034
_journal_paper_doi               10.1039/D3CE00644A
_journal_volume                  25
_journal_year                    2023
_chemical_absolute_configuration rmad
_chemical_formula_moiety         'Br3 Pb, C5 H11 F N'
_chemical_formula_sum            'C5 H11 Br3 F N Pb'
_chemical_formula_weight         551.07
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2022-01-03
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2023-06-24 deposited with the CCDC.	2023-08-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.8341(5)
_cell_length_b                   10.1533(6)
_cell_length_c                   14.2642(9)
_cell_measurement_reflns_used    3683
_cell_measurement_temperature    293(10)
_cell_measurement_theta_max      29.5290
_cell_measurement_theta_min      2.4510
_cell_volume                     1134.60(12)
_computing_cell_refinement       'CrysAlisPro 1.171.41.108a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.108a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.108a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      293(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.824
_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    -38.00 -12.00   0.50    0.62    --   -5.29 103.00  29.00   52
  2  \w     15.00  78.00   0.50    0.62    --    5.13  38.00 177.00  126
  3  \w    -14.00  25.00   0.50    0.62    --   -5.29 -99.00   0.00   78
  4  \w    -15.00  28.00   0.50    0.62    --   -5.29 -99.00  30.00   86
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0811532000
_diffrn_orient_matrix_UB_12      -0.0056989000
_diffrn_orient_matrix_UB_13      0.0217428000
_diffrn_orient_matrix_UB_21      -0.0317865000
_diffrn_orient_matrix_UB_22      0.0328989000
_diffrn_orient_matrix_UB_23      0.0402054000
_diffrn_orient_matrix_UB_31      -0.0246218000
_diffrn_orient_matrix_UB_32      -0.0613601000
_diffrn_orient_matrix_UB_33      0.0195492000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0778
_diffrn_reflns_av_unetI/netI     0.0867
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.824
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            6359
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.778
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.639
_diffrn_reflns_theta_min         2.462
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    25.396
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.01919
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.108a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic brownish brown'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   brownish
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    3.226
_exptl_crystal_description       block
_exptl_crystal_F_000             976
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         3.537
_refine_diff_density_min         -5.231
_refine_diff_density_rms         0.492
_refine_ls_abs_structure_details
;
 Flack x determined using 695 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.03(3)
_refine_ls_extinction_coef       0.0138(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     101
_refine_ls_number_reflns         2731
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.0790
_refine_ls_R_factor_gt           0.0658
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1101P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1615
_refine_ls_wR_factor_ref         0.1687
_reflns_Friedel_coverage         0.644
_reflns_Friedel_fraction_full    0.970
_reflns_Friedel_fraction_max     0.717
_reflns_number_gt                2186
_reflns_number_total             2731
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ce00644a2.cif
_cod_data_source_block           (R_3_FPD)PbBr3
_cod_depositor_comments
'Adding full bibliography for 7247228--7247229.cif.'
_cod_database_code               7247228
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C N H F Pb Br'
_chemical_oxdiff_usercomment     \
_shelx_estimated_absorpt_t_max   0.785
_shelx_estimated_absorpt_t_min   0.516
_olex2_refinement_description
;
1.a Ternary CH refined with riding coordinates:
 C8(H8)
1.b Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C2(H2A,H2B), N1(H1A,H1B), C5(H5A,H5B), C6(H6A,H6B)
;
_shelx_res_checksum              21030
_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 11.935
_oxdiff_exptl_absorpt_empirical_full_min 0.353