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#$Date: 2025-11-05 01:45:53 +0200 (Wed, 05 Nov 2025) $
#$Revision: 303161 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/57/61/1576183.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_1576183
loop_
_publ_author_name
'Su, Chang-Yuan'
'Yi, Heng-Guan'
'Ni, Hao-Fei'
'Du, Guowei'
'Xia, San-Qiang'
'Liu, Zunqi'
'Zhang, Zhi-Xu'
'Fu, Da-Wei'
_publ_section_title
;
 Two-dimensional Lead-Free Double Perovskite Ferroelastic with Dynamic
 Thermochromism
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D5SC05158D
_journal_year                    2025
_chemical_formula_moiety         'Br4 Pb, 2(C5 H12 N)'
_chemical_formula_sum            'C10 H24 Br4 N2 Pb'
_chemical_formula_weight         699.14
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2023-07-19
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-09-04 deposited with the CCDC.	2025-10-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.762(12)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.339(7)
_cell_length_b                   8.289(3)
_cell_length_c                   8.232(3)
_cell_measurement_reflns_used    2945
_cell_measurement_temperature    283.00
_cell_measurement_theta_max      22.80
_cell_measurement_theta_min      2.88
_cell_volume                     964.3(7)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      283.00
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1442
_diffrn_reflns_av_unetI/netI     0.0626
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            23660
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.414
_diffrn_reflns_theta_min         2.849
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    17.021
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.3998
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1444 before and 0.0892 after correction.
The Ratio of minimum to maximum transmission is 0.5364.
The λ/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.408
_exptl_crystal_description       block
_exptl_crystal_F_000             640
_refine_diff_density_max         2.838
_refine_diff_density_min         -2.075
_refine_diff_density_rms         0.223
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     80
_refine_ls_number_reflns         1978
_refine_ls_number_restraints     27
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0662
_refine_ls_R_factor_gt           0.0447
_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)+(0.0657P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1076
_refine_ls_wR_factor_ref         0.1196
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1477
_reflns_number_total             1978
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d5sc05158d4.cif
_cod_data_source_block           mo_scy_pbbr_cba_0m_a
_cod_database_code               1576183
_shelx_shelxl_version_number     2018/3
_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.
;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H,H) groups
2. Restrained distances
 C8-C10 = C8-C1
 1.5 with sigma of 0.02
 C7-C10
 1.5 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C1 \\sim C8 \\sim C10 \\sim C7: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
4.a Ternary CH refined with riding coordinates:
 C8(H8)
4.b Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C10(H10A,H10B), C1(H1A,H1B), C7(H7A,H7B)
4.c Idealised Me refined as rotating group:
 N004(H00A,H00B,H00C)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-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
Pb01 Pb 0.500000 0.500000 0.500000 0.04098(9) Uani 1 2 d S . P . .
Br02 Br 0.49756(5) 0.30795(8) 0.19126(8) 0.05643(19) Uani 1 1 d . . . . .
Br03 Br 0.71163(6) 0.47333(9) 0.58161(10) 0.0597(2) Uani 1 1 d . . . . .
N004 N 0.6751(4) 0.4208(7) 0.9772(7) 0.0571(17) Uani 1 1 d . . . . .
H00A H 0.691414 0.433449 0.878318 0.069 Uiso 1 1 calc R U . . .
H00B H 0.612924 0.433832 0.969220 0.069 Uiso 1 1 calc R U . . .
H00C H 0.691181 0.322272 1.014762 0.069 Uiso 1 1 calc R U . . .
C5 C 0.7248(7) 0.5419(11) 1.0921(11) 0.079(3) Uani 1 1 d . . . . .
H5A H 0.702284 0.648674 1.056474 0.095 Uiso 1 1 calc R U . . .
H5B H 0.709578 0.523719 1.201031 0.095 Uiso 1 1 calc R U . . .
C8 C 0.8252(8) 0.5364(11) 1.1016(16) 0.128(4) Uani 1 1 d D U . . .
H8 H 0.838267 0.558712 0.990764 0.154 Uiso 1 1 calc R U . . .
C10 C 0.8881(7) 0.6477(11) 1.2193(16) 0.152(5) Uani 1 1 d D U . . .
H10A H 0.910775 0.741085 1.166500 0.183 Uiso 1 1 calc R U . . .
H10B H 0.861430 0.678752 1.315347 0.183 Uiso 1 1 calc R U . . .
C1 C 0.8824(9) 0.4014(14) 1.164(2) 0.180(6) Uani 1 1 d D U . . .
H1A H 0.904190 0.337383 1.078899 0.216 Uiso 1 1 calc R U . . .
H1B H 0.854459 0.333791 1.238806 0.216 Uiso 1 1 calc R U . . .
C7 C 0.9548(10) 0.5185(14) 1.248(3) 0.204(7) Uani 1 1 d D U . . .
H7A H 0.975470 0.495134 1.364352 0.244 Uiso 1 1 calc R U . . .
H7B H 1.008740 0.532035 1.192588 0.244 Uiso 1 1 calc R U . . .
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
_geom_angle_publ_flag
Br02 Pb01 Br02 180.0 3_666 . ?
Br02 Pb01 Br02 90.37(3) . 2_655 ?
Br02 Pb01 Br02 89.63(3) 3_666 2_655 ?
Br02 Pb01 Br02 90.37(3) 3_666 4_566 ?
Br02 Pb01 Br02 89.63(3) . 4_566 ?
Br02 Pb01 Br02 180.0 4_566 2_655 ?
Br02 Pb01 Br03 94.51(2) 4_566 3_666 ?
Br02 Pb01 Br03 90.96(2) 3_666 3_666 ?
Br02 Pb01 Br03 94.51(2) 2_655 . ?
Br02 Pb01 Br03 90.95(2) . . ?
Br02 Pb01 Br03 89.05(2) . 3_666 ?
Br02 Pb01 Br03 85.49(2) 4_566 . ?
Br02 Pb01 Br03 89.04(2) 3_666 . ?
Br02 Pb01 Br03 85.49(2) 2_655 3_666 ?
Br03 Pb01 Br03 180.0 . 3_666 ?
Pb01 Br02 Pb01 153.85(2) . 2_645 ?
H00A N004 H00B 109.5 . . ?
H00A N004 H00C 109.5 . . ?
H00B N004 H00C 109.5 . . ?
C5 N004 H00A 109.5 . . ?
C5 N004 H00B 109.5 . . ?
C5 N004 H00C 109.5 . . ?
N004 C5 H5A 109.1 . . ?
N004 C5 H5B 109.1 . . ?
H5A C5 H5B 107.8 . . ?
C8 C5 N004 112.6(8) . . ?
C8 C5 H5A 109.1 . . ?
C8 C5 H5B 109.1 . . ?
C5 C8 H8 107.0 . . ?
C5 C8 C10 119.9(10) . . ?
C5 C8 C1 123.8(11) . . ?
C10 C8 H8 107.0 . . ?
C1 C8 H8 107.0 . . ?
C1 C8 C10 90.3(9) . . ?
C8 C10 H10A 114.0 . . ?
C8 C10 H10B 114.0 . . ?
H10A C10 H10B 111.2 . . ?
C7 C10 C8 87.7(9) . . ?
C7 C10 H10A 114.0 . . ?
C7 C10 H10B 114.0 . . ?
C8 C1 H1A 113.9 . . ?
C8 C1 H1B 113.9 . . ?
C8 C1 C7 88.3(9) . . ?
H1A C1 H1B 111.1 . . ?
C7 C1 H1A 113.9 . . ?
C7 C1 H1B 113.9 . . ?
C10 C7 C1 90.9(10) . . ?
C10 C7 H7A 113.5 . . ?
C10 C7 H7B 113.5 . . ?
C1 C7 H7A 113.5 . . ?
C1 C7 H7B 113.5 . . ?
H7A C7 H7B 110.8 . . ?
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
Pb01 Br02 2.9942(10) 3_666 ?
Pb01 Br02 3.0026(10) 2_655 ?
Pb01 Br02 2.9942(10) . ?
Pb01 Br02 3.0026(10) 4_566 ?
Pb01 Br03 3.0030(16) 3_666 ?
Pb01 Br03 3.0030(16) . ?
N004 H00A 0.8900 . ?
N004 H00B 0.8900 . ?
N004 H00C 0.8900 . ?
N004 C5 1.477(10) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C5 C8 1.429(15) . ?
C8 H8 0.9800 . ?
C8 C10 1.519(12) . ?
C8 C1 1.430(13) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C10 C7 1.429(13) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C1 C7 1.503(19) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
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_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N004 C5 C8 C10 -177.5(9) . . . . ?
N004 C5 C8 C1 -64.3(15) . . . . ?
C5 C8 C10 C7 143.2(14) . . . . ?
C5 C8 C1 C7 -139.5(14) . . . . ?
C8 C10 C7 C1 -12.4(14) . . . . ?
C8 C1 C7 C10 13.1(15) . . . . ?
C10 C8 C1 C7 -12.3(14) . . . . ?
C1 C8 C10 C7 13.0(15) . . . . ?
