#------------------------------------------------------------------------------
#$Date: 2019-11-04 18:01:47 +0200 (Mon, 04 Nov 2019) $
#$Revision: 223200 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/12/72/4127235.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_4127235
loop_
_publ_author_name
'Wang, Sasa'
'Liu, Xitao'
'Li, Lina'
'Ji, Chengmin'
'Sun, Zhihua'
'Wu, Zhenyue'
'Hong, Maochun'
'Luo, Junhua'
_publ_section_title
;
 An Unprecedented Biaxial Trilayered Hybrid Perovskite Ferroelectric with
 Directionally Tunable Photovoltaic Effects.
;
_journal_issue                   19
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7693
_journal_page_last               7697
_journal_paper_doi               10.1021/jacs.9b02558
_journal_volume                  141
_journal_year                    2019
_chemical_formula_sum            'C8 H32 Br10 N4 Pb3'
_chemical_formula_weight         1605.05
_space_group_IT_number           139
_space_group_name_Hall           '-I 4 2'
_space_group_name_H-M_alt        'I 4/m m m'
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-I 4 2'
_symmetry_space_group_name_H-M   'I 4/m m m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   6.0080(15)
_cell_length_b                   6.0080(15)
_cell_length_c                   46.843(15)
_cell_measurement_reflns_used    2077
_cell_measurement_temperature    390(2)
_cell_measurement_theta_max      26.4652
_cell_measurement_theta_min      2.5371
_cell_volume                     1690.8(8)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      390(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0679
_diffrn_reflns_av_sigmaI/netI    0.0332
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       60
_diffrn_reflns_limit_l_min       -59
_diffrn_reflns_number            5638
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         3.42
_exptl_absorpt_coefficient_mu    26.719
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    3.153
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       slice
_exptl_crystal_F_000             1408
_refine_diff_density_max         2.198
_refine_diff_density_min         -3.464
_refine_diff_density_rms         0.238
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     43
_refine_ls_number_reflns         653
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0623
_refine_ls_R_factor_gt           0.0475
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0794P)²+28.4442P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1375
_refine_ls_wR_factor_ref         0.1518
_reflns_number_gt                520
_reflns_number_total             653
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja9b02558_si_003.cif
_cod_data_source_block           c:\users\wu\desktop\22\2
_cod_depositor_comments
'Adding full bibliography for 4127235--4127236.cif.'
_cod_original_sg_symbol_H-M      I4/mmm
_cod_database_code               4127235
loop_
_symmetry_equiv_pos_as_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Pb1 Pb 0.0000 0.0000 0.0000 0.0491(4) Uani 1 16 d S
Pb2 Pb 0.0000 0.0000 0.13492(2) 0.0530(4) Uani 1 8 d S
Br1 Br 0.0000 0.0000 0.06423(8) 0.119(2) Uani 1 8 d S
Br5 Br 0.0000 0.5000 0.13772(11) 0.1421(18) Uani 1 4 d S
Br4 Br 0.0000 0.0000 0.19375(11) 0.238(6) Uani 1 8 d S
Br2 Br 0.0000 -0.5000 0.0000 0.1159(18) Uani 1 8 d S
C3 C 0.5000 0.639(2) 0.2061(8) 0.17(6) Uani 0.25 2 d SPDU
H3A H 0.3708 0.7326 0.2062 0.207 Uiso 0.13 1 d PR
H3B H 0.6292 0.7326 0.2062 0.207 Uiso 0.13 1 d PR
N2 N 0.5000 0.5000 0.1794(8) 0.16(2) Uani 1 8 d SD
H2A H 0.5000 0.5896 0.1640 0.235 Uiso 0.25 2 d SPR
H2B H 0.6223 0.4135 0.1791 0.235 Uiso 0.13 1 d PR
H2C H 0.3777 0.4135 0.1791 0.235 Uiso 0.13 1 d PR
C4 C 0.5000 0.5000 0.2318(8) 0.42(12) Uani 1 8 d SD
H4A H 0.5000 0.5936 0.2484 0.627 Uiso 0.25 2 d SPR
H4B H 0.3695 0.4078 0.2319 0.627 Uiso 0.13 1 d PR
H4C H 0.6305 0.4078 0.2319 0.627 Uiso 0.13 1 d PR
N1 N -0.5000 0.5000 0.0421(15) 0.53(13) Uani 1 8 d SD
H1A H -0.5000 0.4111 0.0266 0.800 Uiso 0.25 2 d SPR
H1B H -0.6223 0.5865 0.0418 0.800 Uiso 0.13 1 d PR
H1C H -0.3777 0.5865 0.0418 0.800 Uiso 0.13 1 d PR
C1 C -0.5000 0.360(2) 0.0685(15) 0.12(5) Uani 0.25 2 d SPD
H1D H -0.3707 0.2663 0.0686 0.148 Uiso 0.13 1 d PR
H1E H -0.6293 0.2663 0.0686 0.148 Uiso 0.13 1 d PR
C2 C -0.5000 0.5000 0.0943(15) 0.53(19) Uani 1 8 d SD
H2D H -0.5000 0.4068 0.1110 0.788 Uiso 0.25 2 d SPR
H2E H -0.3695 0.5922 0.0944 0.788 Uiso 0.13 1 d PR
H2F H -0.6305 0.5922 0.0944 0.788 Uiso 0.13 1 d PR
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'
Br Br -0.2901 2.4595 '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'
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
Br2 Pb1 Br2 180.0 2 2_455
Br2 Pb1 Br2 90.0 2 .
Br2 Pb1 Br2 90.0 2_455 .
Br2 Pb1 Br2 90.0 2 1_565
Br2 Pb1 Br2 90.0 2_455 1_565
Br2 Pb1 Br2 180.0 . 1_565
Br2 Pb1 Br1 90.0 2 .
Br2 Pb1 Br1 90.0 2_455 .
Br2 Pb1 Br1 90.0 . .
Br2 Pb1 Br1 90.0 1_565 .
Br2 Pb1 Br1 90.0 2 17
Br2 Pb1 Br1 90.0 2_455 17
Br2 Pb1 Br1 90.0 . 17
Br2 Pb1 Br1 90.0 1_565 17
Br1 Pb1 Br1 180.0 . 17
Br4 Pb2 Br5 87.50(10) . 2_655
Br4 Pb2 Br5 87.50(10) . 2
Br5 Pb2 Br5 175.0(2) 2_655 2
Br4 Pb2 Br5 87.50(10) . 1_545
Br5 Pb2 Br5 89.891(9) 2_655 1_545
Br5 Pb2 Br5 89.891(9) 2 1_545
Br4 Pb2 Br5 87.50(10) . .
Br5 Pb2 Br5 89.891(9) 2_655 .
Br5 Pb2 Br5 89.891(9) 2 .
Br5 Pb2 Br5 175.0(2) 1_545 .
Pb2 Br5 Pb2 175.0(2) 1_565 .
Pb1 Br2 Pb1 180.0 1_545 .
C3 C3 C3 89.999(17) 2_655 4_565
C3 C3 C4 66.3(4) 2_655 .
C3 C3 C4 66.3(4) 4_565 .
C3 C3 N2 66.9(4) 2_655 .
C3 C3 N2 66.9(4) 4_565 .
C4 C3 N2 111.6(11) . .
C3 C3 C3 44.999(8) 2_655 3_665
C3 C3 C3 44.999(11) 4_565 3_665
C4 C3 C3 55.4(6) . 3_665
N2 C3 C3 56.3(6) . 3_665
C3 C3 H3A 81.0 2_655 .
C3 C3 H3A 171.0 4_565 .
C4 C3 H3A 109.3 . .
N2 C3 H3A 109.3 . .
C3 C3 H3A 126.0 3_665 .
C3 C3 H3B 171.0 2_655 .
C3 C3 H3B 81.0 4_565 .
C4 C3 H3B 109.3 . .
N2 C3 H3B 109.3 . .
C3 C3 H3B 126.0 3_665 .
H3A C3 H3B 108.0 . .
C3 N2 C3 46.2(7) . 4_565
C3 N2 C3 46.2(7) . 2_655
C3 N2 C3 67.5(11) 4_565 2_655
C3 N2 C3 67.5(11) . 3_665
C3 N2 C3 46.2(7) 4_565 3_665
C3 N2 C3 46.2(7) 2_655 3_665
C3 N2 H2A 109.5 . .
C3 N2 H2A 131.8 4_565 .
C3 N2 H2A 131.8 2_655 .
C3 N2 H2A 177.0 3_665 .
C3 N2 H2B 109.5 . .
C3 N2 H2B 63.8 4_565 .
C3 N2 H2B 117.8 2_655 .
C3 N2 H2B 72.1 3_665 .
H2A N2 H2B 109.5 . .
C3 N2 H2C 109.5 . .
C3 N2 H2C 117.8 4_565 .
C3 N2 H2C 63.8 2_655 .
C3 N2 H2C 72.1 3_665 .
H2A N2 H2C 109.5 . .
H2B N2 H2C 109.5 . .
C3 C4 C3 47.4(7) 3_665 2_655
C3 C4 C3 47.4(7) 3_665 4_565
C3 C4 C3 69.3(12) 2_655 4_565
C3 C4 C3 69.3(12) 3_665 .
C3 C4 C3 47.4(7) 2_655 .
C3 C4 C3 47.4(7) 4_565 .
C3 C4 H4A 178.8 3_665 .
C3 C4 H4A 131.8 2_655 .
C3 C4 H4A 131.8 4_565 .
C3 C4 H4A 109.5 . .
C3 C4 H4B 71.1 3_665 .
C3 C4 H4B 62.7 2_655 .
C3 C4 H4B 118.0 4_565 .
C3 C4 H4B 109.5 . .
H4A C4 H4B 109.5 . .
C3 C4 H4C 71.1 3_665 .
C3 C4 H4C 118.0 2_655 .
C3 C4 H4C 62.7 4_565 .
C3 C4 H4C 109.5 . .
H4A C4 H4C 109.5 . .
H4B C4 H4C 109.5 . .
C1 N1 C1 68.2(11) . 3_465
C1 N1 C1 46.7(7) . 2_565
C1 N1 C1 46.7(7) 3_465 2_565
C1 N1 C1 46.7(7) . 4_455
C1 N1 C1 46.7(7) 3_465 4_455
C1 N1 C1 68.2(11) 2_565 4_455
C1 N1 H1A 109.5 . .
C1 N1 H1A 177.7 3_465 .
C1 N1 H1A 131.8 2_565 .
C1 N1 H1A 131.8 4_455 .
C1 N1 H1B 109.5 . .
C1 N1 H1B 71.7 3_465 .
C1 N1 H1B 117.9 2_565 .
C1 N1 H1B 63.4 4_455 .
H1A N1 H1B 109.5 . .
C1 N1 H1C 109.5 . .
C1 N1 H1C 71.7 3_465 .
C1 N1 H1C 63.4 2_565 .
C1 N1 H1C 117.9 4_455 .
H1A N1 H1C 109.5 . .
H1B N1 H1C 109.5 . .
C1 C1 C1 90.00(3) 2_565 4_455
C1 C1 C2 66.2(4) 2_565 .
C1 C1 C2 66.2(4) 4_455 .
C1 C1 N1 66.6(4) 2_565 .
C1 C1 N1 66.6(4) 4_455 .
C2 C1 N1 111.0(11) . .
C1 C1 C1 45.000(16) 2_565 3_465
C1 C1 C1 45.000(14) 4_455 3_465
C2 C1 C1 55.2(6) . 3_465
N1 C1 C1 55.9(6) . 3_465
C1 C1 H1D 81.0 2_565 .
C1 C1 H1D 171.0 4_455 .
C2 C1 H1D 109.4 . .
N1 C1 H1D 109.4 . .
C1 C1 H1D 126.0 3_465 .
C1 C1 H1E 171.0 2_565 .
C1 C1 H1E 81.0 4_455 .
C2 C1 H1E 109.4 . .
N1 C1 H1E 109.4 . .
C1 C1 H1E 126.0 3_465 .
H1D C1 H1E 108.0 . .
C1 C2 C1 47.6(7) 4_455 3_465
C1 C2 C1 69.7(11) 4_455 2_565
C1 C2 C1 47.6(7) 3_465 2_565
C1 C2 C1 47.6(7) 4_455 .
C1 C2 C1 69.7(11) 3_465 .
C1 C2 C1 47.6(7) 2_565 .
C1 C2 H2D 131.8 4_455 .
C1 C2 H2D 179.2 3_465 .
C1 C2 H2D 131.8 2_565 .
C1 C2 H2D 109.5 . .
C1 C2 H2E 118.0 4_455 .
C1 C2 H2E 71.0 3_465 .
C1 C2 H2E 62.4 2_565 .
C1 C2 H2E 109.5 . .
H2D C2 H2E 109.5 . .
C1 C2 H2F 62.4 4_455 .
C1 C2 H2F 71.0 3_465 .
C1 C2 H2F 118.0 2_565 .
C1 C2 H2F 109.5 . .
H2D C2 H2F 109.5 . .
H2E C2 H2F 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pb1 Br2 3.0040(8) 2
Pb1 Br2 3.0040(8) 2_455
Pb1 Br2 3.0040(8) .
Pb1 Br2 3.0040(8) 1_565
Pb1 Br1 3.009(4) .
Pb1 Br1 3.009(4) 17
Pb2 Br4 2.756(5) .
Pb2 Br5 3.0069(8) 2_655
Pb2 Br5 3.0069(8) 2
Pb2 Br5 3.0069(8) 1_545
Pb2 Br5 3.0069(8) .
Br5 Pb2 3.0069(8) 1_565
Br2 Pb1 3.0040(8) 1_545
C3 C3 1.18(2) 2_655
C3 C3 1.18(2) 4_565
C3 C4 1.465(10) .
C3 N2 1.500(10) .
C3 C3 1.67(3) 3_665
C3 H3A 0.9600 .
C3 H3B 0.9600 .
N2 C3 1.500(10) 4_565
N2 C3 1.500(10) 2_655
N2 C3 1.500(10) 3_665
N2 H2A 0.9001 .
N2 H2B 0.9000 .
N2 H2C 0.9000 .
C4 C3 1.465(10) 3_665
C4 C3 1.465(10) 2_655
C4 C3 1.465(10) 4_565
C4 H4A 0.9601 .
C4 H4B 0.9600 .
C4 H4C 0.9600 .
N1 C1 1.498(10) .
N1 C1 1.498(10) 3_465
N1 C1 1.498(10) 2_565
N1 C1 1.498(10) 4_455
N1 H1A 0.9000 .
N1 H1B 0.9000 .
N1 H1C 0.9000 .
C1 C1 1.19(2) 2_565
C1 C1 1.19(2) 4_455
C1 C2 1.471(10) .
C1 C1 1.68(3) 3_465
C1 H1D 0.9600 .
C1 H1E 0.9600 .
C2 C1 1.471(10) 4_455
C2 C1 1.471(10) 3_465
C2 C1 1.471(10) 2_565
C2 H2D 0.9601 .
C2 H2E 0.9600 .
C2 H2F 0.9600 .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
Br4 Pb2 Br5 Pb2 180.0 . 1_565
Br5 Pb2 Br5 Pb2 92.49(10) 2_655 1_565
Br5 Pb2 Br5 Pb2 -92.49(10) 2 1_565
Br5 Pb2 Br5 Pb2 180.0 1_545 1_565
Br2 Pb1 Br2 Pb1 0.0 2 1_545
Br2 Pb1 Br2 Pb1 0.0 2_455 1_545
Br2 Pb1 Br2 Pb1 0.0 1_565 1_545
Br1 Pb1 Br2 Pb1 0.0 . 1_545
Br1 Pb1 Br2 Pb1 0.0 17 1_545
C3 C3 N2 C3 -100.5(4) 2_655 4_565
C4 C3 N2 C3 -50.25(19) . 4_565
C3 C3 N2 C3 -50.25(19) 3_665 4_565
C3 C3 N2 C3 100.5(4) 4_565 2_655
C4 C3 N2 C3 50.25(18) . 2_655
C3 C3 N2 C3 50.25(18) 3_665 2_655
C3 C3 N2 C3 -50.25(18) 2_655 3_665
C3 C3 N2 C3 50.25(18) 4_565 3_665
C4 C3 N2 C3 0.000(3) . 3_665
C3 C3 C4 C3 50.56(19) 2_655 3_665
C3 C3 C4 C3 -50.6(2) 4_565 3_665
N2 C3 C4 C3 0.000(3) . 3_665
C3 C3 C4 C3 -101.1(4) 4_565 2_655
N2 C3 C4 C3 -50.56(19) . 2_655
C3 C3 C4 C3 -50.56(19) 3_665 2_655
C3 C3 C4 C3 101.1(4) 2_655 4_565
N2 C3 C4 C3 50.6(2) . 4_565
C3 C3 C4 C3 50.6(2) 3_665 4_565
C1 N1 C1 C1 -50.38(19) 3_465 2_565
C1 N1 C1 C1 -100.8(4) 4_455 2_565
C1 N1 C1 C1 50.38(19) 3_465 4_455
C1 N1 C1 C1 100.8(4) 2_565 4_455
C1 N1 C1 C2 0.000(3) 3_465 .
C1 N1 C1 C2 50.38(19) 2_565 .
C1 N1 C1 C2 -50.38(19) 4_455 .
C1 N1 C1 C1 50.38(18) 2_565 3_465
C1 N1 C1 C1 -50.38(18) 4_455 3_465
C1 C1 C2 C1 101.2(4) 2_565 4_455
N1 C1 C2 C1 50.6(2) . 4_455
C1 C1 C2 C1 50.6(2) 3_465 4_455
C1 C1 C2 C1 50.62(19) 2_565 3_465
C1 C1 C2 C1 -50.6(2) 4_455 3_465
N1 C1 C2 C1 0.000(3) . 3_465
C1 C1 C2 C1 -101.2(4) 4_455 2_565
N1 C1 C2 C1 -50.62(19) . 2_565
C1 C1 C2 C1 -50.62(19) 3_465 2_565
