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_7249974
_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         'H2 O, Br10 Pb2, 2(C6 H18 N3)'
_chemical_formula_sum            'C12 H38 Br10 N6 O Pb2'
_chemical_formula_weight         1495.96
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_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                 96.191(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.8538(3)
_cell_length_b                   17.5673(4)
_cell_length_c                   13.8398(3)
_cell_measurement_reflns_used    20977
_cell_measurement_temperature    299.80(10)
_cell_measurement_theta_max      31.0300
_cell_measurement_theta_min      2.2770
_cell_volume                     3348.60(13)
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_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    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      299.80(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.880
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -20.00  20.00   0.50    0.40    --    5.69 -43.00  10.00   80
  2  \w    -67.00 -41.00   0.50    0.40    --    5.69 -43.00  10.00   52
  3  \w     16.00  79.00   0.50    0.40    --    5.69  43.00 162.00  126
  4  \w    -12.00  21.00   0.50    0.40    --    5.69 -36.00  85.63   66
  5  \w    -68.00 -27.00   0.50    0.40    --    5.69 -36.00  85.63   82
  6  \w    -68.00  21.00   0.50    0.40    --    5.69 -36.00 -81.67  178
  7  \w    -64.00  20.00   0.50    0.40    --    5.69 -33.00-144.33  168
  8  \w    -10.00  81.00   0.50    0.40    --    5.69  19.00 -30.00  182
  9  \w    -18.00  40.00   0.50    0.40    --    5.69 -99.00-180.00  116
 10  \w    -18.00  28.00   0.50    0.40    --   -6.24 -99.00 -60.00   92
 11  \w     -3.00  40.00   0.50    0.40    --    5.69 -99.00   0.00   86
 12  \w    -79.00  -2.00   0.50    0.40    --   -6.24 -43.00  10.00  154
 13  \w    -21.00  58.00   0.50    0.40    --   -6.24  43.00 162.00  158
 14  \w    -21.00  67.00   0.50    0.40    --   -6.24  38.00  30.00  176
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0066292000
_diffrn_orient_matrix_UB_12      0.0394890000
_diffrn_orient_matrix_UB_13      0.0091314000
_diffrn_orient_matrix_UB_21      0.0132252000
_diffrn_orient_matrix_UB_22      -0.0077883000
_diffrn_orient_matrix_UB_23      0.0499668000
_diffrn_orient_matrix_UB_31      0.0493270000
_diffrn_orient_matrix_UB_32      -0.0032136000
_diffrn_orient_matrix_UB_33      -0.0088064000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1092
_diffrn_reflns_av_unetI/netI     0.0769
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.880
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            98359
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.880
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.876
_diffrn_reflns_theta_min         1.879
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    21.993
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.03468
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.967
_exptl_crystal_description       block
_exptl_crystal_F_000             2696
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.962
_refine_diff_density_min         -2.385
_refine_diff_density_rms         0.236
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     289
_refine_ls_number_reflns         9279
_refine_ls_number_restraints     319
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0912
_refine_ls_R_factor_gt           0.0516
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0144P)^2^+29.6271P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0813
_refine_ls_wR_factor_ref         0.0889
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6756
_reflns_number_total             9279
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5ce00003c2.cif
_cod_data_source_block           PMA
_cod_depositor_comments
'Adding full bibliography for 7249974--7249975.cif.'
_cod_database_code               7249974
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'H C N Br Pb'
_shelx_estimated_absorpt_t_max   0.096
_shelx_estimated_absorpt_t_min   0.096
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H) groups, All N(H,H) groups, All N(H,H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 C1-N1
 1.507 with sigma of 0.001
 O1-H1f = O1-H1g
 0.85 with sigma of 0.02
 H1f-H1g
 1.34 with sigma of 0.04
3. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
Uanis(N1) \\sim Ueq, Uanis(C1) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
5. Rigid body (RIGU) restrains
 C1, H1a, H1b, C2, N1, H2a, H2b, N2, H1c, H1d, H1e, C3, C6, H2, H3a, H3b, C4,
 C5, H6a, H6b, H4a, H4b, N3, H5a, H5b, H3c, H3d
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N4, C7, H7a, H7b, C8, H8a, H8b, N5, H4c, H4d, H4e, C9, C12, H5, H9a, H9b, C10,
  C11, H12a, H12b, H10a, H10b, N6, H11a, H11b, H6c, H6d
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6.a Riding coordinates:
 N1(H1c,H1d,H1e), N2(H2), N4(H4c,H4d,H4e), N5(H5)
6.b Secondary CH2 refined with riding coordinates:
 C1(H1a,H1b), C2(H2a,H2b), C3(H3a,H3b), C4(H4a,H4b), C5(H5a,H5b), C6(H6a,H6b),
 N3(H3c,H3d), C7(H7a,H7b), C8(H8a,H8b), C9(H9a,H9b), C10(H10a,H10b), C11(H11a,
 H11b), C12(H12a,H12b), N6(H6c,H6d)
;
_shelx_res_checksum              86467
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 14.606
_oxdiff_exptl_absorpt_empirical_full_min 0.466