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_4127752
_publ_section_title
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 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(C2 H8 N), 2(C4 H12 N)'
_chemical_formula_sum            'C12 H40 I10 N4 Pb3'
_chemical_formula_weight         2131.05
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2019-04-20
_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                   9.0291(9)
_cell_length_b                   8.9825(9)
_cell_length_c                   52.666(6)
_cell_measurement_reflns_used    2513
_cell_measurement_temperature    340(2)
_cell_measurement_theta_max      21.69
_cell_measurement_theta_min      2.38
_cell_volume                     4271.4(8)
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      340.01
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1071
_diffrn_reflns_av_unetI/netI     0.0886
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       68
_diffrn_reflns_limit_l_min       -68
_diffrn_reflns_number            26125
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.626
_diffrn_reflns_theta_min         2.256
_exptl_absorpt_coefficient_mu    19.033
_exptl_crystal_colour            dark
_exptl_crystal_density_diffrn    3.314
_exptl_crystal_description       block
_exptl_crystal_F_000             3664
_refine_diff_density_max         11.945
_refine_diff_density_min         -10.828
_refine_diff_density_rms         1.221
_refine_ls_extinction_coef       0.000021(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     137
_refine_ls_number_reflns         5226
_refine_ls_number_restraints     93
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.2133
_refine_ls_R_factor_gt           0.1064
_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^)+520.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2053
_refine_ls_wR_factor_ref         0.2453
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2179
_reflns_number_total             5226
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b05124_si_003.cif
_cod_data_source_block           x
_cod_database_code               4127752
_shelx_shelxl_version_number     2016/6
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.024(2)
 0.976(2)
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. Restrained distances
 C5-C6 = C5-C4 = C4-C3 = C3-N2
 1.5 with sigma of 0.02
 C2-C1
 1.48 with sigma of 0.02
 N1-C2
 1.47 with sigma of 0.02
 C1-N1
 2.3 with sigma of 0.02
 C6-C4
 2.4 with sigma of 0.02
 C5-C3
 2.5 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
N2 \\sim C3 \\sim C4 \\sim C5 \\sim C6: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02
C1 \\sim C2 \\sim N1: within 2A with sigma of 0.005 and sigma for terminal
atoms of 0.01
Uanis(C2) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C6) \\sim
Ueq, Uanis(C4) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(N1) \\sim Ueq, Uanis(N2)
\\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
5.a Secondary CH2 refined with riding coordinates:
 C2(H2D,H2E), C5(H5A,H5B), C4(H4A,H4B), C3(H3A,H3B)
5.b Me refined with riding coordinates:
 C6(H6A,H6B,H6C), N2(H2A,H2B,H2C)
5.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), N1(H1D,H1E,H1F)
;
_shelx_res_checksum              28582
_shelx_hkl_checksum              17443
_olex2_submission_special_instructions 'No special instructions were received'