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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/1/57/56/1575648.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_1575648
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 H15 Br N'
_chemical_formula_sum            'C7 H15 Br4 N Pb'
_chemical_formula_weight         640.03
_chemical_name_systematic        BR-HTP
_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   mixed
_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
;
2025-07-29 deposited with the CCDC.	2025-09-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.2813(6)
_cell_length_b                   9.5881(7)
_cell_length_c                   18.1544(18)
_cell_measurement_reflns_used    3776
_cell_measurement_temperature    321(2)
_cell_measurement_theta_max      28.1110
_cell_measurement_theta_min      2.6950
_cell_volume                     1441.5(2)
_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      321.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  Rigaku
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0455
_diffrn_reflns_av_unetI/netI     0.0301
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            6917
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        24.994
_diffrn_reflns_theta_max         24.994
_diffrn_reflns_theta_min         2.244
_exptl_absorpt_coefficient_mu    22.757
_exptl_crystal_density_diffrn    2.949
_exptl_crystal_description       block
_exptl_crystal_F_000             1144
_refine_diff_density_max         1.550
_refine_diff_density_min         -1.447
_refine_diff_density_rms         0.208
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     70
_refine_ls_number_reflns         1356
_refine_ls_number_restraints     46
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0554
_refine_ls_R_factor_gt           0.0431
_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)+(0.0599P)²+11.8779P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1128
_refine_ls_wR_factor_ref         0.1190
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1115
_reflns_number_total             1356
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d5sc05322f2.cif
_cod_data_source_block           1_CCDC1
_cod_database_code               1575648
_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:
  {H4A,H4B} of C4, {H2A,H2B} of C2, {H5A,H5B} of C5, {H1A,H1B} of C1
 At 1.5 times of:
  {H3A,H3B} of C3
2. Restrained distances
 N1-C4 = N1-C3 = N1-C2
 1.4 with sigma of 0.02
 C2-C1 = C5-C4
 1.5 with sigma of 0.02
 Br3-C1
 1.9 with sigma of 0.02
3. Rigid bond restraints
 C2, C1, C3, C5, C4, 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
C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim N1: 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 Riding coordinates:
 C3(H3A,H3B)
6.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C4(H4A,H4B), C5(H5A,H5B)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-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_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 0.66700(7) 0.250000 0.24511(3) 0.0480(3) Uani 1 2 d S T P . .
Br1 Br 0.4977(2) 0.250000 0.37805(10) 0.0655(5) Uani 1 2 d S T P . .
Br2 Br 0.90221(14) 0.46084(12) 0.30434(8) 0.0670(4) Uani 1 1 d . . . . .
Br3 Br 1.1337(3) 0.250000 0.46432(15) 0.1190(11) Uani 1 2 d DS T P . .
N1 N 0.7190(18) 0.250000 0.5953(10) 0.086(3) Uani 1 2 d DS TU P . .
C1 C 0.908(2) 0.250000 0.4845(14) 0.129(6) Uani 1 2 d DS TU P . .
H1A H 0.859203 0.331824 0.462444 0.154 Uiso 0.5 1 calc R U P . .
H1B H 0.859203 0.168176 0.462444 0.154 Uiso 0.5 1 calc R U P . .
C2 C 0.876(3) 0.250000 0.5634(14) 0.114(5) Uani 1 2 d DS TU P . .
H2A H 0.931353 0.169009 0.583170 0.137 Uiso 0.5 1 calc R U P . .
H2B H 0.931353 0.330991 0.583170 0.137 Uiso 0.5 1 calc R U P . .
C3 C 0.773(3) 0.250000 0.6716(11) 0.095(5) Uani 1 2 d DS TU P . .
H3A H 0.680914 0.250000 0.703584 0.143 Uiso 1 2 d R U P . .
H3B H 0.836994 0.168250 0.680754 0.143 Uiso 1 1 d R U . . .
C4 C 0.6159(17) 0.3685(16) 0.5803(11) 0.100(4) Uani 1 1 d D U . . .
H4A H 0.606844 0.385051 0.527731 0.120 Uiso 1 1 calc R U . . .
H4B H 0.656796 0.452158 0.603867 0.120 Uiso 1 1 calc R U . . .
C5 C 0.4562(17) 0.3261(17) 0.6125(11) 0.104(4) Uani 1 1 d D U . . .
H5A H 0.444963 0.361680 0.662275 0.124 Uiso 1 1 calc R U . . .
H5B H 0.367912 0.361684 0.582850 0.124 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'
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'
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 90.93(4) . 7_565 ?
Br1 Pb1 Br2 84.00(4) . 4_455 ?
Br1 Pb1 Br2 90.93(4) . . ?
Br1 Pb1 Br2 84.00(4) . 6_556 ?
Br2 Pb1 Br2 97.05(4) 7_565 4_455 ?
Br2 Pb1 Br2 80.94(5) 4_455 6_556 ?
Br2 Pb1 Br2 84.52(5) 7_565 . ?
Br2 Pb1 Br2 174.71(3) . 4_455 ?
Br2 Pb1 Br2 174.71(3) 7_565 6_556 ?
Br2 Pb1 Br2 97.05(4) . 6_556 ?
Pb1 Br2 Pb1 85.22(3) . 6_656 ?
C2 N1 C3 96.1(18) . . ?
C2 N1 C4 117.5(11) . . ?
C2 N1 C4 117.5(11) . 7_565 ?
C4 N1 C3 111.2(13) 7_565 . ?
C4 N1 C3 111.2(13) . . ?
C4 N1 C4 103.4(17) 7_565 . ?
Br3 C1 H1A 109.3 . . ?
Br3 C1 H1B 109.3 . . ?
H1A C1 H1B 108.0 . . ?
C2 C1 Br3 111.6(15) . . ?
C2 C1 H1A 109.3 . . ?
C2 C1 H1B 109.3 . . ?
N1 C2 C1 125(2) . . ?
N1 C2 H2A 106.2 . . ?
N1 C2 H2B 106.2 . . ?
C1 C2 H2A 106.2 . . ?
C1 C2 H2B 106.2 . . ?
H2A C2 H2B 106.4 . . ?
N1 C3 H3A 109.3 . . ?
N1 C3 H3B 109.6(6) . 7_565 ?
N1 C3 H3B 109.6 . . ?
H3A C3 H3B 109.5 . 7_565 ?
H3A C3 H3B 109.5 . . ?
H3B C3 H3B 109.5 . 7_565 ?
N1 C4 H4A 111.1 . . ?
N1 C4 H4B 111.1 . . ?
N1 C4 C5 103.5(13) . . ?
H4A C4 H4B 109.0 . . ?
C5 C4 H4A 111.1 . . ?
C5 C4 H4B 111.1 . . ?
C4 C5 H5A 110.6 . . ?
C4 C5 H5B 110.6 . . ?
C5 C5 C4 105.7(9) 7_565 . ?
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 2.7913(19) . ?
Pb1 Br2 3.0062(12) . ?
Pb1 Br2 3.1146(12) 4_455 ?
Pb1 Br2 3.0061(12) 7_565 ?
Pb1 Br2 3.1146(12) 6_556 ?
Br3 C1 1.903(16) . ?
N1 C2 1.425(17) . ?
N1 C3 1.455(17) . ?
N1 C4 1.448(14) . ?
N1 C4 1.448(14) 7_565 ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C1 C2 1.455(18) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 H3A 0.9599 . ?
C3 H3B 0.9599 . ?
C3 H3B 0.9599 7_565 ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C4 C5 1.502(15) . ?
C5 C5 1.46(3) 7_565 ?
C5 H5A 0.9700 . ?
C5 H5B 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
Br3 C1 C2 N1 180.000(5) . . . . ?
N1 C4 C5 C5 -25.0(14) . . . 7_565 ?
C2 N1 C4 C5 172.4(17) . . . . ?
C3 N1 C2 C1 180.000(6) . . . . ?
C3 N1 C4 C5 -78.3(17) . . . . ?
C4 N1 C2 C1 62.3(15) 7_565 . . . ?
C4 N1 C2 C1 -62.3(15) . . . . ?
C4 N1 C4 C5 41(2) 7_565 . . . ?
