Revisiting a (001)-oriented layered lead chloride templated by 1,2,4-triazolium: structural phase transitions, lattice dynamics and broadband photoluminescence.
Mączka, Mirosław; Sobczak, Szymon; Ptak, Maciej; Smółka, Szymon; Fedoruk, Katarzyna; Dybała, Filip; Herman, Artur P.; Paraguassu, Waldeci; Zaręba, Jan K; Kudrawiec, Robert; Sieradzki, Adam; Katrusiak, Andrzej; Dalton transactions (Cambridge, England : 2003) 53 (2024) 6906–6919; doi:10.1039/d4dt00406j

data_7715596
_publ_section_title
;
 Revisiting a (001)-oriented layered lead chloride templated by
 1,2,4-triazolium: structural phase transitions, lattice dynamics and
 broadband photoluminescence.
;
_journal_issue                   16
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6906
_journal_page_last               6919
_journal_paper_doi               10.1039/d4dt00406j
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'Cl4 Pb, 2(C2 H4 N3)'
_chemical_formula_sum            'C4 H8 Cl4 N6 Pb'
_chemical_formula_weight         489.15
_chemical_name_systematic        Tz2PbCl4
_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   geom
_audit_creation_date             2023-12-15
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-03-04 deposited with the CCDC.	2024-03-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.036(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.4831(12)
_cell_length_b                   8.3057(3)
_cell_length_c                   7.4695(3)
_cell_measurement_reflns_used    5770
_cell_measurement_temperature    249.99(10)
_cell_measurement_theta_max      28.5470
_cell_measurement_theta_min      3.6480
_cell_volume                     1332.80(10)
_computing_cell_refinement       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_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      250.15
_diffrn_detector_area_resol_mean 8.0772
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.896
_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     23.00  48.00   1.00    5.00    --   17.79-139.00 143.00   25
  2  \w     16.00  41.00   1.00    5.00    --   17.79-130.00 -42.00   25
  3  \w    -62.00 -18.00   1.00    5.00    --  -18.57 130.00  29.00   44
  4  \w    -75.00 -47.00   1.00    5.00    --  -18.57 139.00-156.00   28
  5  \w     39.00  94.00   1.00    5.00    --   17.79 178.00  30.00   55
  6  \w     43.00  68.00   1.00    5.00    --   17.79 178.00-150.00   25
  7  \w    -47.00  61.00   1.00    5.00    --   17.79 -19.00 150.00  108
  8  \w    -32.00  11.00   1.00    5.00    --  -18.57 -77.00 120.00   43
  9  \w    -87.00   3.00   1.00    5.00    --  -18.57 -57.00  90.00   90
 10  \w    -84.00 -59.00   1.00    5.00    --  -18.57-178.00   0.00   25
 11  \w    -32.00  11.00   1.00    5.00    --  -18.57 -77.00 -30.00   43
 12  \w     -5.00  39.00   1.00    5.00    --  -18.57  57.00 -30.00   44
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0431
_diffrn_reflns_av_unetI/netI     0.0339
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.896
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            14644
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.896
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         29.030
_diffrn_reflns_theta_min         2.629
_exptl_absorpt_coefficient_mu    13.440
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.13442
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.438
_exptl_crystal_description       block
_exptl_crystal_F_000             896
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         2.168
_refine_diff_density_min         -1.577
_refine_diff_density_rms         0.214
_refine_ls_extinction_coef       0.0151(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.251
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     138
_refine_ls_number_reflns         3182
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.251
_refine_ls_R_factor_all          0.0500
_refine_ls_R_factor_gt           0.0354
_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^)+(0.0308P)^2^+2.2842P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0849
_refine_ls_wR_factor_ref         0.0906
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2395
_reflns_number_total             3182
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00406j2.cif
_cod_data_source_block           triag2pbcl4_02_250_00
_cod_depositor_comments
'Adding full bibliography for 7715584--7715597.cif.'
_cod_database_code               7715596
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.295
_shelx_estimated_absorpt_t_min   0.050
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: -9(10)
 10(10)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
3.a Aromatic/amide H refined with riding coordinates:
 N2A(H2A), N1B(H1B), N1A(H1A), N2B(H2B), C1A(H1AA), C1B(H1BA), C2A(H2AA),
 C2B(H2BA)
;
_shelx_res_checksum              57899
_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
;