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_7247229
_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_formula_moiety         'Br8 Pb2, 4(C5 H10 F2 N)'
_chemical_formula_sum            'C20 H40 Br8 F8 N4 Pb2'
_chemical_formula_weight         1542.22
_space_group_crystal_system      tetragonal
_space_group_IT_number           92
_space_group_name_Hall           'P 4abw 2nw'
_space_group_name_H-M_alt        'P 41 21 2'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2021-12-27
_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            8
_cell_length_a                   12.2050(3)
_cell_length_b                   12.2050(3)
_cell_length_c                   51.295(3)
_cell_measurement_reflns_used    8032
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.4200
_cell_measurement_theta_min      2.3830
_cell_volume                     7641.0(5)
_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)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      293
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0948
_diffrn_reflns_av_unetI/netI     0.0798
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       63
_diffrn_reflns_limit_l_min       -52
_diffrn_reflns_number            34696
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_min         1.715
_exptl_absorpt_coefficient_mu    17.228
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.42968
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'metallic brownish colourless'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   brownish
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.681
_exptl_crystal_description       block
_exptl_crystal_F_000             5632
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         2.575
_refine_diff_density_min         -1.476
_refine_diff_density_rms         0.381
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.504(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     350
_refine_ls_number_reflns         7503
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.090
_refine_ls_R_factor_all          0.0979
_refine_ls_R_factor_gt           0.0710
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0648P)^2^+90.4424P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1473
_refine_ls_wR_factor_ref         0.1575
_reflns_Friedel_coverage         0.703
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                5695
_reflns_number_total             7503
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ce00644a2.cif
_cod_data_source_block           (3_3_DFPD)2PbBr4
_cod_depositor_comments
'Adding full bibliography for 7247228--7247229.cif.'
_cod_original_cell_volume        7641.0(6)
_cod_database_code               7247229
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.847
_shelx_estimated_absorpt_t_min   0.626
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.496(14)
 0.504(14)
2. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H) groups
3. Restrained distances
 C77-C18 = C77-C45 = C54-C45 = C7-C54
 1.54 with sigma of 0.02
 C2-H2A = N15-C18
 1.5 with sigma of 0.02
4. Rigid bond restraints
 C77
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C14, C19
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
5. Uiso/Uaniso restraints and constraints
F74 \\sim C77: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.01 within 2A
Uanis(C77) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(C18) = Uanis(N15) = Uanis(C7) = Uanis(C54) = Uanis(C45) = Uanis(C77)
6.a Secondary CH2 refined with riding coordinates:
 N3(H3A,H3B), C2(H2A,H2B), N1(H1A,H1B), C5(H5A,H5B), C1(H1C,H1D), C8(H8A,H8B),
 C10(H10A,H10B), C13(H13A,H13B), C17(H17A,H17B), C22(H22A,H22B), N4(H4A,H4B),
 C6(H6A,H6B), C3(H3C,H3D), N15(H15A,H15B), C14(H14A,H14B), C18(H18A,H18B),
 C7(H7A,H7B), C19(H19A,H19B), C45(H45A,H45B), C54(H54A,H54B)
;
_shelx_res_checksum              58256
_olex2_submission_special_instructions 'No special instructions were received'