#------------------------------------------------------------------------------
#$Date: 2025-09-10 01:21:40 +0300 (Wed, 10 Sep 2025) $
#$Revision: 302077 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/57/56/1575649.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_1575649
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
_chemical_name_systematic        Cl-150K
_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                   8.0114(4)
_cell_length_b                   9.1767(4)
_cell_length_c                   17.0882(7)
_cell_measurement_reflns_used    4730
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.3760
_cell_measurement_theta_min      2.3650
_cell_volume                     1256.29(10)
_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  0.0721
_diffrn_reflns_av_unetI/netI     0.0544
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            5490
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         2.38
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    14.239
_exptl_crystal_density_diffrn    2.444
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             856
_refine_diff_density_max         1.649
_refine_diff_density_min         -2.076
_refine_diff_density_rms         0.333
_refine_ls_extinction_coef       0.0012(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.731
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     72
_refine_ls_number_reflns         1179
_refine_ls_number_restraints     66
_refine_ls_restrained_S_all      0.804
_refine_ls_R_factor_all          0.0408
_refine_ls_R_factor_gt           0.0371
_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)+(0.1333P)²+8.6796P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1155
_refine_ls_wR_factor_ref         0.1219
_reflns_number_gt                1055
_reflns_number_total             1179
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            d5sc05322f2.cif
_cod_data_source_block           1_CCDC2
_cod_database_code               1575649
_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-C4 = N1-C2
 1.4 with sigma of 0.02
 C5-C4 = C2-C1
 1.5 with sigma of 0.02
 Cl3-C1
 1.9 with sigma of 0.02
3. Rigid bond restraints
 C5, C4, C3, N1, C2, C1, 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
C5 \\sim C4 \\sim C3 \\sim N1 \\sim C2 \\sim C1 \\sim Cl3: within 2A with sigma
of 0.01 and sigma for terminal atoms of 0.02 within 2A
Uanis(Cl2) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(Pb1) \\sim Ueq: with sigma of 0.000001 and sigma for terminal atoms of
0.002
5. Others
 Fixed Sof: H1A(0.5) H1B(0.5) H2A(0.5) H2B(0.5) H3A(0.5) H3B(0.5) H3C(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 0.17132(5) 0.7500 0.24464(2) 0.0084(3) Uani 1 2 d SU . .
Cl1 Cl 0.0135(3) 0.7500 0.37986(15) 0.0157(6) Uani 1 2 d S . .
Cl2 Cl 0.4085(2) 0.54259(19) 0.30180(11) 0.0164(5) Uani 1 1 d U . .
Cl3 Cl 0.6367(5) 0.7500 0.4584(2) 0.0452(10) Uani 1 2 d SDU . .
N1 N 0.2347(12) 0.7500 0.6012(6) 0.024(2) Uani 1 2 d SDU . .
C1 C 0.4124(18) 0.7500 0.4820(10) 0.061(4) Uani 1 2 d SDU . .
H1A H 0.3572 0.8377 0.4604 0.073 Uiso 0.50 1 calc PR . .
H1B H 0.3572 0.6623 0.4604 0.073 Uiso 0.50 1 calc PR . .
C2 C 0.4046(17) 0.7500 0.5682(9) 0.046(3) Uani 1 2 d SDU . .
H2A H 0.4645 0.6630 0.5879 0.056 Uiso 0.50 1 calc PR . .
H2B H 0.4645 0.8370 0.5879 0.056 Uiso 0.50 1 calc PR . .
C3 C 0.2730(18) 0.7500 0.6841(8) 0.030(3) Uani 1 2 d SDU . .
H3A H 0.3491 0.8306 0.6959 0.045 Uiso 0.50 1 calc PR A -1
H3B H 0.3260 0.6575 0.6983 0.045 Uiso 0.50 1 calc PR A -1
H3C H 0.1697 0.7619 0.7141 0.045 Uiso 0.50 1 calc PR A -1
C4 C 0.1287(12) 0.6234(9) 0.5797(6) 0.0275(18) Uani 1 1 d DU . .
H4A H 0.1659 0.5338 0.6068 0.033 Uiso 1 1 calc R . .
H4B H 0.1300 0.6063 0.5225 0.033 Uiso 1 1 calc R . .
C5 C -0.0442(12) 0.6702(11) 0.6075(6) 0.033(2) Uani 1 1 d DU . .
H5A H -0.1314 0.6325 0.5717 0.039 Uiso 1 1 calc R . .
H5B H -0.0662 0.6325 0.6608 0.039 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 91.10(6) . 7_575 ?
Cl1 Pb1 Cl2 83.88(6) . 6_556 ?
Cl1 Pb1 Cl2 91.10(6) . . ?
Cl1 Pb1 Cl2 83.88(6) . 4_465 ?
Cl2 Pb1 Cl2 80.46(7) 6_556 4_465 ?
Cl2 Pb1 Cl2 97.86(6) . 6_556 ?
Cl2 Pb1 Cl2 97.86(6) 7_575 4_465 ?
Cl2 Pb1 Cl2 83.39(7) 7_575 . ?
Cl2 Pb1 Cl2 174.84(4) 7_575 6_556 ?
Cl2 Pb1 Cl2 174.84(4) . 4_465 ?
Pb1 Cl2 Pb1 87.30(5) . 6_656 ?
C2 N1 C4 115.7(7) . 7_575 ?
C2 N1 C4 115.7(7) . . ?
C3 N1 C2 100.2(11) . . ?
C3 N1 C4 111.3(7) . 7_575 ?
C3 N1 C4 111.3(7) . . ?
C4 N1 C4 102.9(10) . 7_575 ?
Cl3 C1 H1A 110.7 . . ?
Cl3 C1 H1B 110.7 . . ?
H1A C1 H1B 108.8 . . ?
C2 C1 Cl3 105.1(10) . . ?
C2 C1 H1A 110.7 . . ?
C2 C1 H1B 110.7 . . ?
N1 C2 C1 114.9(13) . . ?
N1 C2 H2A 108.5 . . ?
N1 C2 H2B 108.5 . . ?
C1 C2 H2A 108.5 . . ?
C1 C2 H2B 108.5 . . ?
H2A C2 H2B 107.5 . . ?
N1 C3 H3A 109.5 . . ?
N1 C3 H3B 109.5 . . ?
N1 C3 H3C 109.5 . . ?
N1 C4 H4A 111.2 . . ?
N1 C4 H4B 111.2 . . ?
N1 C4 C5 102.8(7) . . ?
H4A C4 H4B 109.1 . . ?
C5 C4 H4A 111.2 . . ?
C5 C4 H4B 111.2 . . ?
C4 C5 H5A 110.5 . . ?
C4 C5 H5B 110.5 . . ?
C5 C5 C4 106.4(5) 7_575 . ?
C5 C5 H5A 110.5 7_575 . ?
C5 C5 H5B 110.5 7_575 . ?
H5A C5 H5B 108.6 . . ?
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 2.634(3) . ?
Pb1 Cl2 2.9472(18) 4_465 ?
Pb1 Cl2 2.9472(18) 6_556 ?
Pb1 Cl2 2.8614(18) 7_575 ?
Pb1 Cl2 2.8614(18) . ?
Cl2 Pb1 2.9472(18) 6_656 ?
Cl3 C1 1.842(14) . ?
N1 C2 1.473(15) . ?
N1 C3 1.450(14) . ?
N1 C4 1.485(10) 7_575 ?
N1 C4 1.485(10) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C1 C2 1.474(17) . ?
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 1.526(12) . ?
C5 C5 1.46(2) 7_575 ?
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
Cl1 Pb1 Cl2 Pb1 -125.51(5) . . . 6_656 ?
Cl2 Pb1 Cl2 Pb1 150.52(7) 6_556 . . 6_656 ?
Cl2 Pb1 Cl2 Pb1 -34.52(7) 7_575 . . 6_656 ?
Cl2 Pb1 Cl2 Pb1 -138.9(4) 4_465 . . 6_656 ?
Cl3 C1 C2 N1 180.000(3) . . . . ?
N1 C4 C5 C5 25.5(7) . . . 7_575 ?
C2 N1 C4 C5 -168.7(10) . . . . ?
C3 N1 C2 C1 180.000(4) . . . . ?
C3 N1 C4 C5 77.8(10) . . . . ?
C4 N1 C2 C1 -60.3(8) 7_575 . . . ?
C4 N1 C2 C1 60.3(8) . . . . ?
C4 N1 C4 C5 -41.5(11) 7_575 . . . ?
