High-Temperature Antiferroelectric of Lead Iodide Hybrid Perovskites.
Han, Shiguo; Liu, Xitao; Liu, Yi; Xu, Zhiyun; Li, Yaobin; Hong, Maochun; Luo, Junhua; Sun, Zhihua; Journal of the American Chemical Society 141 (2019) 12470–12474; doi:10.1021/jacs.9b05124

data_4127751
_publ_section_title
;
 High-Temperature Antiferroelectric of Lead Iodide Hybrid Perovskites.
;
_journal_issue                   32
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12470
_journal_page_last               12474
_journal_paper_doi               10.1021/jacs.9b05124
_journal_volume                  141
_journal_year                    2019
_chemical_formula_moiety         '0.5(I20 Pb6), 2(C4 H12 N), 2(C2 H8 N)'
_chemical_formula_sum            'C12 H40 I10 N4 Pb3'
_chemical_formula_weight         2131.05
_space_group_crystal_system      orthorhombic
_space_group_IT_number           36
_space_group_name_Hall           'C 2c -2'
_space_group_name_H-M_alt        'C m c 21'
_symmetry_space_group_name_Hall  'C 2c -2'
_symmetry_space_group_name_H-M   'C m c 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2018-12-11
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   51.236(5)
_cell_length_b                   8.7266(9)
_cell_length_c                   9.1242(9)
_cell_measurement_reflns_used    4656
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      25.017
_cell_measurement_theta_min      2.368
_cell_volume                     4079.6(7)
_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 0.992
_diffrn_measured_fraction_theta_max 0.992
_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  0.0654
_diffrn_reflns_av_unetI/netI     0.0785
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       60
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            8318
_diffrn_reflns_point_group_measured_fraction_full 0.798
_diffrn_reflns_point_group_measured_fraction_max 0.798
_diffrn_reflns_theta_full        25.080
_diffrn_reflns_theta_max         25.080
_diffrn_reflns_theta_min         2.621
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    19.928
_exptl_absorpt_correction_T_max  0.4899
_exptl_absorpt_correction_T_min  0.2652
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1308 before and 0.0591 after correction. The Ratio of minimum to maximum transmission is 0.3562. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    3.470
_exptl_crystal_description       block
_exptl_crystal_F_000             3664
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         3.097
_refine_diff_density_min         -3.496
_refine_diff_density_rms         0.414
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.077(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     141
_refine_ls_number_reflns         2926
_refine_ls_number_restraints     37
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0779
_refine_ls_R_factor_gt           0.0546
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0365P)^2^+240.5399P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1161
_refine_ls_wR_factor_ref         0.1297
_reflns_Friedel_coverage         0.499
_reflns_Friedel_fraction_full    0.573
_reflns_Friedel_fraction_max     0.573
_reflns_number_gt                2345
_reflns_number_total             2926
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b05124_si_002.cif
_cod_data_source_block           x1
_cod_original_cell_volume        4079.5(7)
_cod_database_code               4127751
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.436
_shelx_estimated_absorpt_t_min   0.241
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.923(9)
 0.077(9)
2. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Uiso/Uaniso restraints and constraints
C1 \\sim N1 \\sim C2: within 2A with sigma of 0.01 and sigma for terminal atoms
of 0.02
N2 \\sim C3 \\sim C4 \\sim C5 \\sim C6: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02
4.a Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C2(H2D,H2E)
4.b Idealised Me refined as rotating group:
 N2(H2A,H2B,H2C), C6(H6A,H6B,H6C), C1(H1A,H1B,H1C), N1(H1D,H1E,H1F)
;
_olex2_submission_special_instructions 'No special instructions were received'