Thermally responsive multistate fluorescence coupled with uniaxial negative thermal expansion in 1D lead halide hybrids.
Yang, Gang; Ye, Wei; Shen, Yueqi; Shao, Dong-Sheng; Liu, Jian-Lan; Tian, Zheng-Fang; Ning, Weihua; Ren, Xiao-Ming; Chemical science 16 (2025) 18766–18774; doi:10.1039/d5sc05322f

data_1575647
_publ_section_title
;
 Thermally responsive multistate fluorescence coupled with uniaxial
 negative thermal expansion in 1D lead halide hybrids.
;
_journal_issue                   40
_journal_name_full               'Chemical science'
_journal_page_first              18766
_journal_page_last               18774
_journal_paper_doi               10.1039/d5sc05322f
_journal_volume                  16
_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+0.001xFc^2^\l^3^/sin(2\q)]^-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/[\s^2^(Fo^2^)+(0.0469P)^2^+12.0344P] where P=(Fo^2^+2Fc^2^)/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_depositor_comments
'Adding full bibliography for 1575647--1575650.cif.'
_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'