#------------------------------------------------------------------------------
#$Date: 2021-06-04 04:05:48 +0300 (Fri, 04 Jun 2021) $
#$Revision: 265767 $
#$URL: file:///home/coder/svn-repositories/cod/cif/8/00/05/8000504.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_8000504
loop_
_publ_author_name
'Huang, Xue-Qin'
'Zhang, Hua'
'Wang, Fang'
'Gan, Tian'
'Xu, Zhe-Kun'
'Wang, Zhong-Xia'
_publ_section_title
;
 A Photoluminescent Lead Bromide Hybrid Perovskite Molecular Ferroelastic
 Semiconductor with Sequential High-Tc Phase
 Transitions.
;
_journal_issue                   21
_journal_name_full               'The journal of physical chemistry letters'
_journal_page_first              5221
_journal_page_last               5227
_journal_paper_doi               10.1021/acs.jpclett.1c01473
_journal_volume                  12
_journal_year                    2021
_chemical_formula_sum            'C3.2 H8 Br1.2 N0.4 O0.4 Pb0.4'
_chemical_formula_weight         237.27
_space_group_crystal_system      hexagonal
_space_group_IT_number           194
_space_group_name_Hall           '-P 6c 2c'
_space_group_name_H-M_alt        'P 63/m m c'
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            5
_cell_length_a                   9.556(4)
_cell_length_b                   9.556(4)
_cell_length_c                   7.900(2)
_cell_measurement_reflns_used    198
_cell_measurement_temperature    473(2)
_cell_measurement_theta_max      17.3960
_cell_measurement_theta_min      2.4070
_cell_volume                     624.8(4)
_computing_cell_refinement       'CrysAlisPro 1.171.40.14e (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.14e (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.14e (Rigaku OD, 2018)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      473(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.905
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       ω
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.2741
_diffrn_reflns_av_unetI/netI     0.1253
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.905
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            3009
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.905
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.548
_diffrn_reflns_theta_min         2.461
_diffrn_source                   'Rotating-anode X-ray tube'
_exptl_absorpt_coefficient_mu    23.068
_exptl_absorpt_correction_T_max  0.026
_exptl_absorpt_correction_T_min  0.017
_exptl_absorpt_process_details   'CrysAlisPro 1.171.40.14e (Rigaku OD, 2018)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    3.153
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             540
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.490
_refine_diff_density_min         -0.545
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.273
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     19
_refine_ls_number_reflns         363
_refine_ls_number_restraints     54
_refine_ls_restrained_S_all      1.183
_refine_ls_R_factor_all          0.4816
_refine_ls_R_factor_gt           0.3061
_refine_ls_shift/su_max          0.012
_refine_ls_shift/su_mean         0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+38.1180P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3010
_refine_ls_wR_factor_ref         0.3588
_reflns_Friedel_coverage         0.000
_reflns_number_gt                158
_reflns_number_total             363
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            jz1c01473_si_003.cif
_cod_data_source_block           DeanolPbBr3_463K
_cod_depositor_comments
'Adding full bibliography for 8000502--8000504.cif.'
_cod_original_cell_volume        624.7(5)
_cod_original_formula_sum        'C3.20 H8 Br1.20 N0.40 O0.40 Pb0.40'
_cod_database_code               8000504
_shelx_shelxl_version_number     2014/7
_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-y, z'
'-x+y, -x, z'
'-x, -y, z+1/2'
'y, -x+y, z+1/2'
'x-y, x, z+1/2'
'y, x, -z'
'x-y, -y, -z'
'-x, -x+y, -z'
'-y, -x, -z+1/2'
'-x+y, y, -z+1/2'
'x, x-y, -z+1/2'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'x, y, -z-1/2'
'-y, x-y, -z-1/2'
'-x+y, -x, -z-1/2'
'-y, -x, z'
'-x+y, y, z'
'x, x-y, z'
'y, x, z-1/2'
'x-y, -y, z-1/2'
'-x, -x+y, 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 0.0000 0.0000 0.5000 0.219(6) Uani 1 12 d S T P . .
Br1 Br 0.1367(11) 0.273(2) 0.2500 0.356(13) Uani 1 4 d S T P . .
C1 C 0.6668(11) 0.333(2) 0.2500 1.378(10) Uani 1 12 d R TU P . .
C2 C 0.5847(11) 0.415(2) 0.2500 1.378(11) Uani 1 4 d R TU P . .
C3 C 0.6176(11) 0.382(2) 0.0614 1.378(12) Uani 1 2 d R TU P . .
C6 C 0.4565(11) 0.228(2) 0.2500 1.378(12) Uani 1 4 d R TU P . .
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'
Br Br -0.2901 2.4595 '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'
O O 0.0106 0.0060 '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
_geom_angle_publ_flag
Br1 Pb1 Br1 180.0 14_556 2 ?
Br1 Pb1 Br1 81.5(3) 14_556 15_556 ?
Br1 Pb1 Br1 98.5(3) 2 15_556 ?
Br1 Pb1 Br1 98.5(3) 14_556 3 ?
Br1 Pb1 Br1 81.5(3) 2 3 ?
Br1 Pb1 Br1 180.0 15_556 3 ?
Br1 Pb1 Br1 81.5(3) 14_556 13_556 ?
Br1 Pb1 Br1 98.5(4) 2 13_556 ?
Br1 Pb1 Br1 81.5(3) 15_556 13_556 ?
Br1 Pb1 Br1 98.5(3) 3 13_556 ?
Br1 Pb1 Br1 98.5(4) 14_556 . ?
Br1 Pb1 Br1 81.5(3) 2 . ?
Br1 Pb1 Br1 98.5(3) 15_556 . ?
Br1 Pb1 Br1 81.5(3) 3 . ?
Br1 Pb1 Br1 180.0 13_556 . ?
Pb1 Br1 Pb1 82.2(5) 4_554 . ?
C2 C1 C2 120.1(7) 3_665 2_655 ?
C2 C1 C2 120.0(13) 3_665 . ?
C2 C1 C2 119.9(7) 2_655 . ?
C2 C1 C3 61.4 3_665 18_666 ?
C2 C1 C3 103.9(7) 2_655 18_666 ?
C2 C1 C3 103.8(10) . 18_666 ?
C2 C1 C3 61.4 3_665 3_665 ?
C2 C1 C3 103.9(7) 2_655 3_665 ?
C2 C1 C3 103.8(10) . 3_665 ?
C3 C1 C3 122.8 18_666 3_665 ?
C2 C1 C3 103.9(3) 3_665 2_655 ?
C2 C1 C3 61.4(8) 2_655 2_655 ?
C2 C1 C3 103.81(11) . 2_655 ?
C3 C1 C3 152.3(9) 18_666 2_655 ?
C3 C1 C3 49.0(4) 3_665 2_655 ?
C2 C1 C3 103.9(3) 3_665 17_656 ?
C2 C1 C3 61.4(8) 2_655 17_656 ?
C2 C1 C3 103.81(11) . 17_656 ?
C3 C1 C3 49.0(4) 18_666 17_656 ?
C3 C1 C3 152.3(9) 3_665 17_656 ?
C3 C1 C3 122.8(16) 2_655 17_656 ?
C2 C1 C3 103.9(6) 3_665 16_556 ?
C2 C1 C3 103.8(3) 2_655 16_556 ?
C2 C1 C3 61.4 . 16_556 ?
C3 C1 C3 49.0(6) 18_666 16_556 ?
C3 C1 C3 152.3(10) 3_665 16_556 ?
C3 C1 C3 152.2(8) 2_655 16_556 ?
C3 C1 C3 49.0(4) 17_656 16_556 ?
C2 C1 C3 103.9(6) 3_665 . ?
C2 C1 C3 103.8(3) 2_655 . ?
C2 C1 C3 61.4 . . ?
C3 C1 C3 152.3(10) 18_666 . ?
C3 C1 C3 49.0(6) 3_665 . ?
C3 C1 C3 49.0(4) 2_655 . ?
C3 C1 C3 152.2(8) 17_656 . ?
C3 C1 C3 122.7 16_556 . ?
C2 C1 C6 60.0(3) 3_665 2_655 ?
C2 C1 C6 60.1(4) 2_655 2_655 ?
C2 C1 C6 180.0(11) . 2_655 ?
C3 C1 C6 76.2(5) 18_666 2_655 ?
C3 C1 C6 76.2(5) 3_665 2_655 ?
C3 C1 C6 76.2(3) 2_655 2_655 ?
C3 C1 C6 76.2(3) 17_656 2_655 ?
C3 C1 C6 118.6 16_556 2_655 ?
C3 C1 C6 118.6 . 2_655 ?
C2 C1 C6 60.0(8) 3_665 3_665 ?
C2 C1 C6 179.89(14) 2_655 3_665 ?
C2 C1 C6 59.9(5) . 3_665 ?
C3 C1 C6 76.2(7) 18_666 3_665 ?
C3 C1 C6 76.2(7) 3_665 3_665 ?
C3 C1 C6 118.6(8) 2_655 3_665 ?
C3 C1 C6 118.6(8) 17_656 3_665 ?
C3 C1 C6 76.1(2) 16_556 3_665 ?
C3 C1 C6 76.1(2) . 3_665 ?
C6 C1 C6 120.0(5) 2_655 3_665 ?
C2 C1 C6 180.0(13) 3_665 . ?
C2 C1 C6 59.9(7) 2_655 . ?
C2 C1 C6 60.0 . . ?
C3 C1 C6 118.6 18_666 . ?
C3 C1 C6 118.6 3_665 . ?
C3 C1 C6 76.1(9) 2_655 . ?
C3 C1 C6 76.1(9) 17_656 . ?
C3 C1 C6 76.1 16_556 . ?
C3 C1 C6 76.1 . . ?
C6 C1 C6 120.0(11) 2_655 . ?
C6 C1 C6 119.9(5) 3_665 . ?
C1 C2 C6 72.0(11) . 3_665 ?
C1 C2 C3 69.9 . . ?
C6 C2 C3 83.9(4) 3_665 . ?
C1 C2 C3 69.9 . 16_556 ?
C6 C2 C3 83.9(4) 3_665 16_556 ?
C3 C2 C3 139.8 . 16_556 ?
C1 C2 C6 72.0 . . ?
C6 C2 C6 144.1(11) 3_665 . ?
C3 C2 C6 83.9 . . ?
C3 C2 C6 83.9 16_556 . ?
C3 C3 C3 60.0 2_655 3_665 ?
C3 C3 C2 107.3(2) 2_655 . ?
C3 C3 C2 107.3(2) 3_665 . ?
C3 C3 C1 65.5(3) 2_655 . ?
C3 C3 C1 65.5(3) 3_665 . ?
C2 C3 C1 48.8 . . ?
C2 C6 C2 95.9(11) 2_655 . ?
C2 C6 C1 48.0(11) 2_655 . ?
C2 C6 C1 48.0 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb1 Br1 3.004(14) 14_556 ?
Pb1 Br1 3.004(14) 2 ?
Pb1 Br1 3.004(14) 15_556 ?
Pb1 Br1 3.004(14) 3 ?
Pb1 Br1 3.004(14) 13_556 ?
Pb1 Br1 3.004(14) . ?
Br1 Pb1 3.004(14) 4_554 ?
C1 C2 1.3574 3_665 ?
C1 C2 1.36(3) 2_655 ?
C1 C2 1.3591 . ?
C1 C3 1.6966 18_666 ?
C1 C3 1.6966 3_665 ?
C1 C3 1.697(13) 2_655 ?
C1 C3 1.697(13) 17_656 ?
C1 C3 1.6975 16_556 ?
C1 C3 1.6975 . ?
C1 C6 1.7384 2_655 ?
C1 C6 1.74(3) 3_665 ?
C1 C6 1.7402 . ?
C2 C6 1.583(7) 3_665 ?
C2 C3 1.5865 . ?
C2 C3 1.5865 16_556 ?
C2 C6 1.5844 . ?
C3 C3 1.408(16) 2_655 ?
C3 C3 1.408(16) 3_665 ?
C6 C2 1.583(7) 2_655 ?
