Enhanced luminescence in 1D corrugated lead bromides via reduced flexibility of trivalent cations
Fan, Chang-Chun; Fang, Zi-Han; Jiao, Shu-Lin; Yu, Jing-Xue; Liu, Cheng-Dong; Wang, Wei; Jin, Ming-Liang; Liang, Bei-Dou; Han, Xiang-Bin; CrystEngComm 27 (2025) 1997–2003; doi:10.1039/D5CE00003C

data_7249975
_publ_section_title
;
 Enhanced luminescence in 1D corrugated lead bromides via reduced
 flexibility of trivalent cations
;
_journal_issue                   13
_journal_name_full               CrystEngComm
_journal_page_first              1997
_journal_page_last               2003
_journal_paper_doi               10.1039/D5CE00003C
_journal_volume                  27
_journal_year                    2025
_chemical_formula_moiety         'Br5 Pb, 0.5(H4 O2), C7 H20 N3'
_chemical_formula_sum            'C7 H22 Br5 N3 O Pb'
_chemical_formula_weight         771.01
_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_Hall           '-P 2yb'
_space_group_name_H-M_alt        'P 1 21/m 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2024-11-21
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-11-21 deposited with the CCDC.	2025-02-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.9020(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.2495(2)
_cell_length_b                   8.7968(2)
_cell_length_c                   10.3341(2)
_cell_measurement_reflns_used    4042
_cell_measurement_temperature    282.00
_cell_measurement_theta_max      68.112
_cell_measurement_theta_min      4.372
_cell_volume                     911.72(3)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_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      282.00
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0504
_diffrn_reflns_av_unetI/netI     0.0432
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            7544
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.233
_diffrn_reflns_theta_min         4.372
_diffrn_source_current           1.2
_diffrn_source_power             0.06
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    30.770
_exptl_absorpt_correction_T_max  0.7531
_exptl_absorpt_correction_T_min  0.5335
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0924 before and 0.0522 after correction.
The Ratio of minimum to maximum transmission is 0.7084.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'metallic light white'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    white
_exptl_crystal_density_diffrn    2.809
_exptl_crystal_description       plate
_exptl_crystal_F_000             700
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.926
_refine_diff_density_min         -1.074
_refine_diff_density_rms         0.200
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     107
_refine_ls_number_reflns         1786
_refine_ls_number_restraints     61
_refine_ls_restrained_S_all      1.141
_refine_ls_R_factor_all          0.0322
_refine_ls_R_factor_gt           0.0301
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0120P)^2^+3.5358P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0661
_refine_ls_wR_factor_ref         0.0670
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1676
_reflns_number_total             1786
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5ce00003c2.cif
_cod_data_source_block           MPMA
_cod_depositor_comments
'Adding full bibliography for 7249974--7249975.cif.'
_cod_database_code               7249975
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.063
_shelx_estimated_absorpt_t_min   0.063
_olex2_refinement_description
;
1. Restrained distances
 C3-C4
 2.5 with sigma of 0.01
 C5-C4
 1.53 with sigma of 0.01
 N3-C5
 1.49 with sigma of 0.01
 C5-N2
 2.48 with sigma of 0.01
2. Uiso/Uaniso restraints and constraints
Uanis(N2) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C4) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C5) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3. Rigid body (RIGU) restrains
 N1, N2, C1, C2, C3, N3, C4, C5
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Fixed Sof: H1D(0.5) H1E(0.5) H1A(0.5) H1B(0.5) H1C(0.5) N3(0.5) H3C(0.5)
 H3D(0.5) H3E(0.5) C4(0.5) H4A(0.5) H4B(0.5) C5(0.5) H5A(0.5) H5B(0.5)
5.a Free rotating group:
 O1(H1D,H1E)
5.b Ternary CH refined with riding coordinates:
 N1(H1), N2(H2)
5.c Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B)
5.d Me refined with riding coordinates:
 C1(H1A,H1B,H1C)
5.e Idealised Me refined as rotating group:
 N3(H3C,H3D,H3E)
;
_shelx_res_checksum              62330
_olex2_submission_special_instructions 'No special instructions were received'