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#$Date: 2025-09-10 01:21:40 +0300 (Wed, 10 Sep 2025) $
#$Revision: 302077 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/57/56/1575647.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_1575647
loop_
_publ_author_name
'Yang, Gang'
'Ye, Wei'
'Shen, Yueqi'
'Shao, Dongsheng'
'Liu, Jian-Lan'
'Tian, Zhengfang'
'Ning, Weihua'
'Ren, Xiaoming'
_publ_section_title
;
 Thermally Responsive Multistate Fluorescence Coupled with Uniaxial
 Negative Thermal Expansion in 1D Lead Halide Hybrids
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D5SC05322F
_journal_year                    2025
_chemical_formula_moiety         'Br3 Pb, C7 H18 Br N'
_chemical_formula_sum            'C7 H15 Br4 N Pb'
_chemical_formula_weight         640.03
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2025-07-24
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2025-07-24 deposited with the CCDC.	2025-09-08 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.3257(3)
_cell_length_b                   9.4769(3)
_cell_length_c                   17.6231(6)
_cell_measurement_reflns_used    5045
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.6880
_cell_measurement_theta_min      2.1750
_cell_volume                     1390.49(8)
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      150.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  Rigaku
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0210
_diffrn_reflns_av_unetI/netI     0.0169
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            6875
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         2.31
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    23.591
_exptl_crystal_density_diffrn    3.057
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1144
_refine_diff_density_max         1.924
_refine_diff_density_min         -1.595
_refine_diff_density_rms         0.223
_refine_ls_extinction_coef       0.00044(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     72
_refine_ls_number_reflns         1297
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0311
_refine_ls_R_factor_gt           0.0284
_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)+(0.0469P)²+12.0344P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0761
_refine_ls_wR_factor_ref         0.0776
_reflns_number_gt                1211
_reflns_number_total             1297
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            d5sc05322f2.cif
_cod_data_source_block           1
_cod_database_code               1575647
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N1-C3 = N1-C2
 1.4 with sigma of 0.01
 C2-C1
 1.5 with sigma of 0.01
3. Rigid bond restraints
 Br3, C1, C2, C3
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C3 \\sim N1 \\sim C2 \\sim C1 \\sim Br3: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 2A
5. Others
 Fixed Sof: H1A(0.5) H1B(0.5) H2A(0.5) H2B(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C4(H4A,H4B), C5(H5A,H5B)
6.b Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x+1/2, -y, z+1/2'
3 '-x, y+1/2, -z'
4 'x+1/2, -y+1/2, -z+1/2'
5 '-x, -y, -z'
6 'x-1/2, y, -z-1/2'
7 'x, -y-1/2, z'
8 '-x-1/2, 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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.16245(4) 0.2500 0.24405(2) 0.01534(18) Uani 1 2 d S . .
Br1 Br 0.00642(12) 0.2500 0.38333(6) 0.0223(3) Uani 1 2 d S . .
Br2 Br 0.40223(8) 0.46212(7) 0.30304(4) 0.0214(2) Uani 1 1 d . . .
Br3 Br 0.63750(15) 0.2500 0.46026(7) 0.0507(4) Uani 1 2 d SU . .
N1 N 0.2364(11) 0.2500 0.6032(5) 0.033(2) Uani 1 2 d SDU . .
C1 C 0.4070(17) 0.2500 0.4859(8) 0.066(4) Uani 1 2 d SDU . .
H1A H 0.3541 0.3348 0.4646 0.079 Uiso 0.50 1 calc PR . .
H1B H 0.3541 0.1652 0.4646 0.079 Uiso 0.50 1 calc PR . .
C2 C 0.3937(14) 0.2500 0.5701(8) 0.059(3) Uani 1 2 d SDU . .
H2A H 0.4514 0.1660 0.5893 0.071 Uiso 0.50 1 calc PR . .
H2B H 0.4514 0.3340 0.5893 0.071 Uiso 0.50 1 calc PR . .
C3 C 0.2716(15) 0.2500 0.6822(6) 0.036(3) Uani 1 2 d SDU . .
H3A H 0.1753 0.2231 0.7107 0.055 Uiso 1 1 calc R A -1
H3B H 0.3059 0.3446 0.6977 0.055 Uiso 1 1 calc R A -1
H3C H 0.3579 0.1823 0.6926 0.055 Uiso 1 1 calc R A -1
C4 C 0.1280(11) 0.3736(9) 0.5834(5) 0.038(2) Uani 1 1 d . . .
H4A H 0.1635 0.4603 0.6099 0.046 Uiso 1 1 calc R . .
H4B H 0.1285 0.3914 0.5280 0.046 Uiso 1 1 calc R . .
C5 C -0.0378(10) 0.3299(10) 0.6098(5) 0.040(2) Uani 1 1 d . . .
H5A H -0.1211 0.3666 0.5749 0.048 Uiso 1 1 calc R . .
H5B H -0.0593 0.3666 0.6614 0.048 Uiso 1 1 calc R . .
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
Br1 Pb1 Br2 90.28(2) . . ?
Br1 Pb1 Br2 84.77(2) . 4_455 ?
Br1 Pb1 Br2 90.28(2) . 7_565 ?
Br1 Pb1 Br2 84.77(2) . 6_556 ?
Br2 Pb1 Br2 81.81(3) 4_455 6_556 ?
Br2 Pb1 Br2 97.11(2) 7_565 4_455 ?
Br2 Pb1 Br2 97.11(2) . 6_556 ?
Br2 Pb1 Br2 83.54(3) . 7_565 ?
Br2 Pb1 Br2 175.009(18) . 4_455 ?
Br2 Pb1 Br2 175.009(18) 7_565 6_556 ?
Pb1 Br2 Pb1 86.419(18) . 6_656 ?
C2 N1 C4 116.7(6) . . ?
C2 N1 C4 116.7(6) . 7_565 ?
C3 N1 C2 102.1(10) . . ?
C3 N1 C4 110.3(6) . . ?
C3 N1 C4 110.3(6) . 7_565 ?
C4 N1 C4 100.9(9) 7_565 . ?
Br3 C1 H1A 110.2 . . ?
Br3 C1 H1B 110.2 . . ?
H1A C1 H1B 108.5 . . ?
C2 C1 Br3 107.5(9) . . ?
C2 C1 H1A 110.2 . . ?
C2 C1 H1B 110.2 . . ?
N1 C2 C1 118.2(12) . . ?
N1 C2 H2A 107.8 . . ?
N1 C2 H2B 107.8 . . ?
C1 C2 H2A 107.8 . . ?
C1 C2 H2B 107.8 . . ?
H2A C2 H2B 107.1 . . ?
N1 C3 H3A 109.5 . . ?
N1 C3 H3B 109.5 . . ?
N1 C3 H3C 109.5 . . ?
N1 C4 H4A 110.7 . . ?
N1 C4 H4B 110.7 . . ?
H4A C4 H4B 108.8 . . ?
C5 C4 N1 105.1(7) . . ?
C5 C4 H4A 110.7 . . ?
C5 C4 H4B 110.7 . . ?
C4 C5 C5 105.9(5) . 7_565 ?
C4 C5 H5A 110.6 . . ?
C4 C5 H5B 110.6 . . ?
C5 C5 H5A 110.6 7_565 . ?
C5 C5 H5B 110.6 7_565 . ?
H5A C5 H5B 108.7 . . ?
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 2.7771(10) . ?
Pb1 Br2 3.0698(7) 6_556 ?
Pb1 Br2 3.0698(7) 4_455 ?
Pb1 Br2 3.0177(7) . ?
Pb1 Br2 3.0177(7) 7_565 ?
Br2 Pb1 3.0698(7) 6_656 ?
Br3 C1 1.972(14) . ?
N1 C2 1.433(9) . ?
N1 C3 1.423(9) . ?
N1 C4 1.520(10) . ?
N1 C4 1.520(10) 7_565 ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C1 C2 1.488(10) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C4 C5 1.514(13) . ?
C5 C5 1.515(19) 7_565 ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
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
Br1 Pb1 Br2 Pb1 124.79(2) . . . 6_656 ?
Br2 Pb1 Br2 Pb1 132.30(18) 4_455 . . 6_656 ?
Br2 Pb1 Br2 Pb1 34.53(2) 7_565 . . 6_656 ?
Br2 Pb1 Br2 Pb1 -150.45(3) 6_556 . . 6_656 ?
Br3 C1 C2 N1 180.000(3) . . . . ?
N1 C4 C5 C5 -24.9(7) . . . 7_565 ?
C2 N1 C4 C5 167.1(9) . . . . ?
C3 N1 C2 C1 180.000(4) . . . . ?
C3 N1 C4 C5 -77.0(9) . . . . ?
C4 N1 C2 C1 -59.7(7) . . . . ?
C4 N1 C2 C1 59.7(7) 7_565 . . . ?
C4 N1 C4 C5 39.6(11) 7_565 . . . ?
