A Three-Dimensional Lead Halide Perovskite-Related Ferroelectric.
Zhang, Han-Yue; Song, Xian-Jiang; Cheng, Hao; Zeng, Yu-Ling; Zhang, Yi; Li, Peng-Fei; Liao, Wei-Qiang; Xiong, Ren-Gen; Journal of the American Chemical Society  (2020) –; doi:10.1021/jacs.0c00375

data_4134253
_publ_section_title
;
 A Three-Dimensional Lead Halide Perovskite-Related Ferroelectric.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.0c00375
_journal_year                    2020
_chemical_formula_moiety         '2(Cl3 Pb), C5 H16 N2'
_chemical_formula_sum            'C5 H16 Cl6 N2 Pb2'
_chemical_formula_weight         731.30
_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'
_atom_sites_solution_hydrogens   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.8771(9)
_cell_length_b                   9.4425(5)
_cell_length_c                   5.8322(4)
_cell_measurement_reflns_used    4468
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30.8840
_cell_measurement_theta_min      2.5510
_cell_volume                     819.29(9)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'DIAMOND (Brandenburg & Putz, 2005)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_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_measurement_method       'four-circle diffractometer'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0908
_diffrn_reflns_av_unetI/netI     0.0539
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            5551
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        24.991
_diffrn_reflns_theta_max         24.991
_diffrn_reflns_theta_min         2.555
_diffrn_source                   'Rotating-anode X-ray tube'
_exptl_absorpt_coefficient_mu    21.476
_exptl_absorpt_correction_T_max  0.019
_exptl_absorpt_correction_T_min  0.017
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    2.964
_exptl_crystal_description       Block
_exptl_crystal_F_000             652
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.190
_refine_diff_density_max         2.756
_refine_diff_density_min         -2.842
_refine_diff_density_rms         0.406
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.50(10)
_refine_ls_extinction_coef       0.0077(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     86
_refine_ls_number_reflns         1462
_refine_ls_number_restraints     61
_refine_ls_restrained_S_all      0.986
_refine_ls_R_factor_all          0.0585
_refine_ls_R_factor_gt           0.0545
_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^)+(0.0751P)^2^+50.8163P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1520
_refine_ls_wR_factor_ref         0.1569
_reflns_Friedel_coverage         0.807
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                1330
_reflns_number_total             1462
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c00375_si_002.cif
_cod_data_source_block           PMA2
_cod_database_code               4134253
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.099
_shelx_estimated_absorpt_t_max   0.106
_shelx_res_checksum              14910
_shelx_hkl_checksum              85814