#------------------------------------------------------------------------------
#$Date: 2019-11-02 07:20:04 +0200 (Sat, 02 Nov 2019) $
#$Revision: 220924 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/12/77/4127753.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4127753
loop_
_publ_author_name
'Han, Shiguo'
'Liu, Xitao'
'Liu, Yi'
'Xu, Zhiyun'
'Li, Yaobin'
'Hong, Maochun'
'Luo, Junhua'
'Sun, Zhihua'
_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_sum            'C12 H40 I10 N4 Pb3'
_chemical_formula_weight         2131.05
_space_group_crystal_system      tetragonal
_space_group_IT_number           139
_space_group_name_Hall           '-I 4 2'
_space_group_name_H-M_alt        'I 4/m m m'
_symmetry_space_group_name_Hall  '-I 4 2'
_symmetry_space_group_name_H-M   'I 4/m m m'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2016/6
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   6.3937(6)
_cell_length_b                   6.3937(6)
_cell_length_c                   52.791(8)
_cell_measurement_reflns_used    2009
_cell_measurement_temperature    373(2)
_cell_measurement_theta_max      26.40
_cell_measurement_theta_min      2.38
_cell_volume                     2158.1(4)
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_diffrn_ambient_temperature      373(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0584
_diffrn_reflns_av_unetI/netI     0.0324
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       68
_diffrn_reflns_limit_l_min       -62
_diffrn_reflns_number            7002
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.513
_diffrn_reflns_theta_min         3.087
_exptl_absorpt_coefficient_mu    18.835
_exptl_crystal_density_diffrn    3.279
_exptl_crystal_description       block
_exptl_crystal_F_000             1832
_refine_diff_density_max         2.598
_refine_diff_density_min         -2.220
_refine_diff_density_rms         0.201
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     118
_refine_ls_number_reflns         833
_refine_ls_number_restraints     229
_refine_ls_restrained_S_all      0.908
_refine_ls_R_factor_all          0.0795
_refine_ls_R_factor_gt           0.0510
_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/[σ²(Fo²)+(0.0100P)²+99.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0900
_refine_ls_wR_factor_ref         0.1024
_reflns_Friedel_coverage         0.000
_reflns_number_gt                591
_reflns_number_total             833
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ja9b05124_si_004.cif
_cod_data_source_block           x
_cod_original_cell_volume        2158.1(5)
_cod_database_code               4127753
_shelx_shelxl_version_number     2016/6
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x, z'
'-x, -y, z'
'y, -x, z'
'x, -y, -z'
'-x, y, -z'
'y, x, -z'
'-y, -x, -z'
'x+1/2, y+1/2, z+1/2'
'-y+1/2, x+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'y+1/2, -x+1/2, z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'y+1/2, x+1/2, -z+1/2'
'-y+1/2, -x+1/2, -z+1/2'
'-x, -y, -z'
'y, -x, -z'
'x, y, -z'
'-y, x, -z'
'-x, y, z'
'x, -y, z'
'-y, -x, z'
'y, x, z'
'-x+1/2, -y+1/2, -z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'x+1/2, y+1/2, -z+1/2'
'-y+1/2, x+1/2, -z+1/2'
'-x+1/2, y+1/2, z+1/2'
'x+1/2, -y+1/2, z+1/2'
'-y+1/2, -x+1/2, z+1/2'
'y+1/2, x+1/2, z+1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.000000 0.000000 0.000000 0.0546(5) Uani 1 16 d S T P . .
Pb2 Pb 0.000000 0.000000 0.12586(3) 0.0567(4) Uani 1 8 d S T P . .
I1 I 0.000000 0.500000 0.000000 0.1187(14) Uani 1 8 d S T P . .
I2 I 0.000000 0.500000 0.12562(6) 0.1321(12) Uani 1 4 d DS T P . .
I3 I 0.000000 0.000000 0.18239(7) 0.214(3) Uani 1 8 d S T P . .
I4 I 0.000000 0.000000 0.06071(5) 0.1055(11) Uani 1 8 d S T P . .
N1 N 0.479(7) 0.558(18) 0.1659(11) 0.16(3) Uani 0.125 1 d D U P A -1
H1A H 0.535968 0.599923 0.151324 0.245 Uiso 0.125 1 calc R U P A -1
H1B H 0.371816 0.473597 0.162664 0.245 Uiso 0.125 1 calc R U P A -1
H1C H 0.434719 0.668892 0.174514 0.245 Uiso 0.125 1 calc R U P A -1
C1 C 0.631(16) 0.45(3) 0.1803(16) 0.18(3) Uani 0.125 1 d D U P A -1
H1D H 0.748930 0.536631 0.185058 0.215 Uiso 0.125 1 calc R U P A -1
H1E H 0.680052 0.322788 0.172083 0.215 Uiso 0.125 1 calc R U P A -1
C2 C 0.483(17) 0.404(18) 0.2028(16) 0.18(3) Uani 0.125 1 d D U P A -1
H2D H 0.434048 0.260469 0.203515 0.212 Uiso 0.125 1 calc R U P A -1
H2E H 0.366194 0.501010 0.204010 0.212 Uiso 0.125 1 calc R U P A -1
C3 C 0.663(19) 0.45(3) 0.2216(18) 0.18(3) Uani 0.125 1 d D U P A -1
H3A H 0.798719 0.405393 0.215720 0.221 Uiso 0.125 1 calc R U P A -1
H3B H 0.668065 0.597426 0.226901 0.221 Uiso 0.125 1 calc R U P A -1
C4 C 0.56(3) 0.305(19) 0.2413(19) 0.18(4) Uani 0.125 1 d D U P A -1
H4A H 0.645558 0.302435 0.256385 0.274 Uiso 0.125 1 calc R U P A -1
H4B H 0.423796 0.354674 0.245410 0.274 Uiso 0.125 1 calc R U P A -1
H4C H 0.551968 0.166289 0.234442 0.274 Uiso 0.125 1 calc R U P A -1
N2 N 0.683(13) 0.445(17) 0.0604(18) 0.04(2) Uani 0.0625 1 d D U P B -1
H2A H 0.771707 0.480712 0.048125 0.054 Uiso 0.0625 1 calc R U P B -1
H2B H 0.731637 0.489419 0.075204 0.054 Uiso 0.0625 1 calc R U P B -1
H2C H 0.669843 0.306187 0.060732 0.054 Uiso 0.0625 1 calc R U P B -1
C5 C 0.485(17) 0.54(2) 0.0556(14) 0.05(2) Uani 0.0625 1 d D U P B -1
H5A H 0.421488 0.488036 0.040022 0.058 Uiso 0.0625 1 calc R U P B -1
H5B H 0.489162 0.688705 0.055871 0.058 Uiso 0.0625 1 calc R U P B -1
C6 C 0.380(13) 0.443(18) 0.0796(16) 0.04(2) Uani 0.0625 1 d D U P B -1
H6A H 0.236840 0.487432 0.080377 0.056 Uiso 0.0625 1 calc R U P B -1
H6B H 0.386208 0.293423 0.078808 0.056 Uiso 0.0625 1 calc R U P B -1
H6C H 0.452863 0.491067 0.094418 0.056 Uiso 0.0625 1 calc R U P B -1
N2B N 0.363(15) 0.46(2) 0.0461(18) 0.05(2) Uani 0.0625 1 d D U P C -2
H2BA H 0.300711 0.589563 0.046214 0.080 Uiso 0.0625 1 calc R U P C -2
H2BB H 0.438689 0.451386 0.032121 0.080 Uiso 0.0625 1 calc R U P C -2
H2BC H 0.265603 0.364998 0.046578 0.080 Uiso 0.0625 1 calc R U P C -2
C5B C 0.49(3) 0.447(16) 0.0677(17) 0.05(2) Uani 0.0625 1 d D U P C -2
H5BA H 0.417751 0.453263 0.083527 0.066 Uiso 0.0625 1 calc R U P C -2
H5BB H 0.607300 0.547867 0.067695 0.066 Uiso 0.0625 1 calc R U P C -2
C6B C 0.57(2) 0.222(16) 0.061(2) 0.04(2) Uani 0.0625 1 d D U P C -2
H6BA H 0.665290 0.175103 0.073912 0.064 Uiso 0.0625 1 calc R U P C -2
H6BB H 0.450902 0.129961 0.060580 0.064 Uiso 0.0625 1 calc R U P C -2
H6BC H 0.637602 0.223144 0.044986 0.064 Uiso 0.0625 1 calc R U P C -2
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
I1 Pb1 I1 90.0 2_655 .
I1 Pb1 I1 180.0 2_655 2
I1 Pb1 I1 90.0 . 2
I1 Pb1 I1 90.0 2_655 1_545
I1 Pb1 I1 180.0 . 1_545
I1 Pb1 I1 90.0 2 1_545
I1 Pb1 I4 90.0 2_655 17
I1 Pb1 I4 90.0 . 17
I1 Pb1 I4 90.0 2 17
I1 Pb1 I4 90.0 1_545 17
I1 Pb1 I4 90.0 2_655 .
I1 Pb1 I4 90.0 . .
I1 Pb1 I4 90.0 2 .
I1 Pb1 I4 90.0 1_545 .
I4 Pb1 I4 180.0 17 .
I3 Pb2 I2 90.22(7) . 2_655
I3 Pb2 I2 90.22(7) . 2
I2 Pb2 I2 179.56(14) 2_655 2
I3 Pb2 I2 90.22(7) . 1_545
I2 Pb2 I2 89.999(1) 2_655 1_545
I2 Pb2 I2 89.999(1) 2 1_545
I3 Pb2 I2 90.22(7) . .
I2 Pb2 I2 89.999(1) 2_655 .
I2 Pb2 I2 89.999(1) 2 .
I2 Pb2 I2 179.56(14) 1_545 .
Pb1 I1 Pb1 180.0 1_565 .
Pb2 I2 Pb2 179.55(14) . 1_565
N1 C1 C2 95(3) . .
C1 C2 C3 90(3) . .
C4 C3 C2 90(3) . .
N2 C5 C6 95(3) . .
N2B C5B C6B 95(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pb1 I1 3.1969(3) 2_655
Pb1 I1 3.1969(3) .
Pb1 I1 3.1969(3) 2
Pb1 I1 3.1969(3) 1_545
Pb1 I4 3.205(3) 17
Pb1 I4 3.205(3) .
Pb2 I3 2.984(4) .
Pb2 I2 3.1969(3) 2_655
Pb2 I2 3.1969(3) 2
Pb2 I2 3.1969(3) 1_545
Pb2 I2 3.1969(3) .
N1 C1 1.418(11) .
C1 C2 1.55(2) .
C2 C3 1.55(2) .
C3 C4 1.55(2) .
N2 C5 1.420(11) .
C5 C6 1.55(2) .
N2B C5B 1.420(11) .
C5B C6B 1.55(2) .
