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_7715591
_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      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
_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
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.5195(2)
_cell_length_b                   21.5921(7)
_cell_length_c                   8.3020(2)
_cell_measurement_reflns_used    7754
_cell_measurement_temperature    320.01(10)
_cell_measurement_theta_max      28.8260
_cell_measurement_theta_min      2.7170
_cell_volume                     1347.93(7)
_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    'SHELXS  (Sheldrick, 2008)'
_diffrn_ambient_temperature      320.15
_diffrn_detector_area_resol_mean 16.1544
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.944
_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      4.00  30.00   1.00    5.00    --   17.79-130.00 -16.00   26
  2  \w    -84.00 -58.00   1.00    5.00    --  -18.72 138.00-129.00   26
  3  \w    -41.00 -15.00   1.00    5.00    --  -18.72 138.00-129.00   26
  4  \w    -65.00 -40.00   1.00    5.00    --  -18.72 130.00  55.00   25
  5  \w     41.00  94.00   1.00    5.00    --   17.79 178.00  90.00   53
  6  \w    -48.00  34.00   1.00    5.00    --   17.79 -57.00 150.00   82
  7  \w    -47.00  38.00   1.00    5.00    --   17.79 -57.00  60.00   85
  8  \w    -12.00  39.00   1.00    5.00    --   17.79  77.00  30.00   51
  9  \w     47.00  77.00   1.00    5.00    --   17.79-138.00 168.00   30
 10  \w    -35.00  -9.00   1.00    5.00    --  -18.72 -57.00  90.00   26
 11  \w    -88.00 -62.00   1.00    5.00    --  -18.72 -57.00  90.00   26
 12  \w    -90.00   6.00   1.00    5.00    --  -18.72 -37.00   0.00   96
 13  \w    -86.00 -12.00   1.00    5.00    --  -18.72 140.00-171.91   74
 14  \w    -26.00   3.00   1.00    5.00    --  -18.72 -57.00 120.00   29
 15  \w    -88.00 -37.00   1.00    5.00    --  -18.72 -57.00 120.00   51
 16  \w    -90.00   6.00   1.00    5.00    --  -18.72 -37.00 150.00   96
 17  \w    -88.00  -8.00   1.00    5.00    --  -18.72 -57.00 -90.00   80
;
_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  0.0615
_diffrn_reflns_av_unetI/netI     0.0310
_diffrn_reflns_Laue_measured_fraction_full 0.978
_diffrn_reflns_Laue_measured_fraction_max 0.944
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            22255
_diffrn_reflns_point_group_measured_fraction_full 0.978
_diffrn_reflns_point_group_measured_fraction_max 0.944
_diffrn_reflns_theta_full        20.000
_diffrn_reflns_theta_max         29.160
_diffrn_reflns_theta_min         3.656
_exptl_absorpt_coefficient_mu    13.289
_exptl_absorpt_correction_T_max  0.190
_exptl_absorpt_correction_T_min  0.040
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
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    2.410
_exptl_crystal_description       block
_exptl_crystal_F_000             896
_exptl_crystal_recrystallization_method 'mounted in a glass capillary'
_exptl_crystal_size_max          0.616
_exptl_crystal_size_mid          0.261
_exptl_crystal_size_min          0.144
_refine_diff_density_max         1.590
_refine_diff_density_min         -1.113
_refine_diff_density_rms         0.140
_refine_ls_extinction_coef       0.00166(11)
_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   1.118
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     78
_refine_ls_number_reflns         1768
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.118
_refine_ls_R_factor_all          0.0496
_refine_ls_R_factor_gt           0.0266
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0125P)^2^+2.0635P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0462
_refine_ls_wR_factor_ref         0.0515
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1180
_reflns_number_total             1768
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00406j2.cif
_cod_data_source_block           triag2pbcl4_iii_320_00
_cod_depositor_comments
'Adding full bibliography for 7715584--7715597.cif.'
_cod_database_code               7715591
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1.a Aromatic/amide H refined with riding coordinates:
 N2(H2), N1(H1), C1(H1A), C2(H2A)
;
_shelx_res_checksum              48239
_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
;