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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/1/57/56/1575650.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_1575650
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         'Cl3 Pb, C7 H15 Cl N'
_chemical_formula_sum            'C7 H15 Cl4 N Pb'
_chemical_formula_weight         462.19
_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                   7.9422(4)
_cell_length_b                   9.3809(5)
_cell_length_c                   17.8601(11)
_cell_measurement_reflns_used    4336
_cell_measurement_temperature    390(2)
_cell_measurement_theta_max      27.8120
_cell_measurement_theta_min      2.4240
_cell_volume                     1330.67(13)
_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      390.15
_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  0.0608
_diffrn_reflns_av_unetI/netI     0.0267
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            9329
_diffrn_reflns_theta_full        24.98
_diffrn_reflns_theta_max         24.98
_diffrn_reflns_theta_min         2.28
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    13.443
_exptl_crystal_density_diffrn    2.307
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             856
_refine_diff_density_max         1.969
_refine_diff_density_min         -0.916
_refine_diff_density_rms         0.179
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     70
_refine_ls_number_reflns         1252
_refine_ls_number_restraints     49
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0611
_refine_ls_R_factor_gt           0.0501
_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)+(0.0664P)²+8.2480P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1342
_refine_ls_wR_factor_ref         0.1404
_reflns_number_gt                991
_reflns_number_total             1252
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            d5sc05322f2.cif
_cod_data_source_block           1_CCDC3
_cod_database_code               1575650
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  {H1A,H1B} of C1, {H4A,H4B} of C4, {H2A,H2B} of C2, {H5A,H5B} of C5
 At 1.5 times of:
  {H3A,H3B} of C3
2. Restrained distances
 C1-C2
 1.6 with sigma of 0.02
3. Rigid bond restraints
 C1, C2
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 Cl3
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C2
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 N1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C4, C5
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C5, C4, C3, C2, C1, N1, Cl3
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
Cl3 \\sim C1 \\sim C2 \\sim C3 \\sim N1 \\sim C4 \\sim C5: 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_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 0.15952(8) 0.7500 0.24629(3) 0.0713(3) Uani 1 2 d S . .
Cl1 Cl -0.0227(7) 0.7500 0.3712(3) 0.1063(16) Uani 1 2 d S . .
Cl2 Cl 0.3962(5) 0.5480(4) 0.3049(3) 0.1169(13) Uani 1 1 d . . .
Cl3 Cl 0.6143(14) 0.7500 0.4682(7) 0.243(5) Uani 1 2 d SU . .
N1 N 0.216(4) 0.7500 0.5891(17) 0.185(6) Uani 1 2 d SU . .
C1 C 0.387(4) 0.7500 0.4788(19) 0.218(6) Uani 1 2 d SDU . .
H1A H 0.3345 0.8348 0.4583 0.262 Uiso 0.50 1 calc PR . .
H1B H 0.3345 0.6652 0.4583 0.262 Uiso 0.50 1 calc PR . .
C2 C 0.391(5) 0.7500 0.5666(19) 0.206(6) Uani 1 2 d SDU . .
H2A H 0.4486 0.6659 0.5853 0.247 Uiso 0.50 1 calc PR . .
H2B H 0.4486 0.8341 0.5853 0.247 Uiso 0.50 1 calc PR . .
C3 C 0.254(5) 0.7500 0.6711(19) 0.205(8) Uani 1 2 d SU . .
H3A H 0.1522 0.7500 0.7006 0.307 Uiso 1 2 d SR . .
H3B H 0.3178 0.6646 0.6838 0.307 Uiso 1 1 d R . .
C4 C 0.124(3) 0.625(3) 0.5741(15) 0.200(6) Uani 1 1 d U . .
H4A H 0.1710 0.5419 0.5989 0.239 Uiso 1 1 calc R . .
H4B H 0.1127 0.6067 0.5208 0.239 Uiso 1 1 calc R . .
C5 C -0.051(3) 0.677(3) 0.6118(14) 0.203(7) Uani 1 1 d U . .
H5A H -0.1462 0.6408 0.5832 0.243 Uiso 1 1 calc R . .
H5B H -0.0599 0.6408 0.6626 0.243 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'
Cl Cl 0.1484 0.1585 '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
Cl1 Pb1 Cl2 92.89(13) . 7_575 ?
Cl1 Pb1 Cl2 82.81(13) . 6_556 ?
Cl1 Pb1 Cl2 92.89(13) . . ?
Cl1 Pb1 Cl2 82.81(13) . 4_465 ?
Cl2 Pb1 Cl2 79.40(16) 6_556 4_465 ?
Cl2 Pb1 Cl2 98.78(14) . 6_556 ?
Cl2 Pb1 Cl2 98.78(14) 7_575 4_465 ?
Cl2 Pb1 Cl2 82.74(18) 7_575 . ?
Cl2 Pb1 Cl2 175.50(10) 7_575 6_556 ?
Cl2 Pb1 Cl2 175.50(11) . 4_465 ?
Pb1 Cl2 Pb1 85.85(10) . 6_656 ?
C2 N1 C3 94(3) . . ?
C4 N1 C2 116(2) . . ?
C4 N1 C2 116(2) 7_575 . ?
C4 N1 C3 107(2) . . ?
C4 N1 C3 107(2) 7_575 . ?
C4 N1 C4 113(3) . 7_575 ?
Cl3 C1 H1A 112.8 . . ?
Cl3 C1 H1B 112.8 . . ?
H1A C1 H1B 110.2 . . ?
C2 C1 Cl3 95(2) . . ?
C2 C1 H1A 112.8 . . ?
C2 C1 H1B 112.8 . . ?
N1 C2 C1 105(3) . . ?
N1 C2 H2A 110.8 . . ?
N1 C2 H2B 110.8 . . ?
C1 C2 H2A 110.8 . . ?
C1 C2 H2B 110.8 . . ?
H2A C2 H2B 108.9 . . ?
N1 C3 H3A 111.3 . . ?
N1 C3 H3B 109.5 . . ?
H3A C3 H3B 107.9 . . ?
N1 C4 H4A 112.4 . . ?
N1 C4 H4B 112.4 . . ?
N1 C4 C5 97(3) . . ?
H4A C4 H4B 110.0 . . ?
C5 C4 H4A 112.4 . . ?
C5 C4 H4B 112.4 . . ?
C4 C5 H5A 110.2 . . ?
C4 C5 H5B 110.2 . . ?
C5 C5 C4 107.4(14) 7_575 . ?
C5 C5 H5A 110.2 7_575 . ?
C5 C5 H5B 110.2 7_575 . ?
H5A C5 H5B 108.5 . . ?
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 Cl1 2.659(5) . ?
Pb1 Cl2 2.966(4) 6_556 ?
Pb1 Cl2 2.966(4) 4_465 ?
Pb1 Cl2 2.867(4) 7_575 ?
Pb1 Cl2 2.867(4) . ?
Cl2 Pb1 2.966(4) 6_656 ?
Cl3 C1 1.82(3) . ?
N1 C2 1.45(4) . ?
N1 C3 1.50(4) . ?
N1 C4 1.41(3) 7_575 ?
N1 C4 1.41(3) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C1 C2 1.569(19) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 H3A 0.9658 . ?
C3 H3B 0.9738 . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C4 C5 1.62(3) . ?
C5 C5 1.38(5) 7_575 ?
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
Cl1 Pb1 Cl2 Pb1 -130.41(12) . . . 6_656 ?
Cl2 Pb1 Cl2 Pb1 146.42(16) 6_556 . . 6_656 ?
Cl2 Pb1 Cl2 Pb1 -37.86(16) 7_575 . . 6_656 ?
Cl2 Pb1 Cl2 Pb1 -147.9(8) 4_465 . . 6_656 ?
Cl3 C1 C2 N1 180.000(8) . . . . ?
N1 C4 C5 C5 24(2) . . . 7_575 ?
C2 N1 C4 C5 178(2) . . . . ?
C3 N1 C2 C1 180.000(9) . . . . ?
C3 N1 C4 C5 74(3) . . . . ?
C4 N1 C2 C1 69(2) . . . . ?
C4 N1 C2 C1 -69(2) 7_575 . . . ?
C4 N1 C4 C5 -44(4) 7_575 . . . ?
