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#$Date: 2024-05-05 05:50:17 +0300 (Sun, 05 May 2024) $
#$Revision: 291625 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/55/7715597.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7715597
loop_
_publ_author_name
'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'
_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                   21.4566(15)
_cell_length_b                   8.3029(3)
_cell_length_c                   7.4446(3)
_cell_measurement_reflns_used    5622
_cell_measurement_temperature    220.00(10)
_cell_measurement_theta_max      28.6400
_cell_measurement_theta_min      3.6580
_cell_volume                     1326.27(12)
_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 2019/2 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      220.15
_diffrn_detector_area_resol_mean 8.0772
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.892
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0417
_diffrn_reflns_av_unetI/netI     0.0335
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.892
_diffrn_reflns_limit_h_max       26
_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            14514
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.892
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         29.054
_diffrn_reflns_theta_min         2.630
_exptl_absorpt_coefficient_mu    13.506
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.14354
_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    2.450
_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         1.796
_refine_diff_density_min         -2.283
_refine_diff_density_rms         0.189
_refine_ls_extinction_coef       0.0129(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2019/2 (Sheldrick 2019)'
_refine_ls_goodness_of_fit_ref   1.110
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     77
_refine_ls_number_reflns         3145
_refine_ls_number_restraints     61
_refine_ls_restrained_S_all      1.116
_refine_ls_R_factor_all          0.0555
_refine_ls_R_factor_gt           0.0402
_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/[σ²(Fo²)+(0.0360P)²+4.0888P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0852
_refine_ls_wR_factor_ref         0.0931
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2441
_reflns_number_total             3158
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4dt00406j2.cif
_cod_data_source_block           triag2pbcl4_08_220_00
_cod_depositor_comments
'Adding full bibliography for 7715584--7715597.cif.'
_cod_database_code               7715597
_shelx_shelxl_version_number     2018/3
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_max   0.294
_shelx_estimated_absorpt_t_min   0.049
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2. Restrained distances
 N3A-N2A \\sim N3B-N2B
 with sigma of 0.02
 N3B-C2B \\sim N3A-C2A
 with sigma of 0.02
 N2A-C1A \\sim N2B-C1B
 with sigma of 0.02
 N1B-C1B \\sim N1A-C1A
 with sigma of 0.02
 N1B-C2B \\sim N1A-C2A
 with sigma of 0.02
3. Rigid body (RIGU) restrains
 Cl2, Pb1, Cl1, Cl4, Cl3
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N3B, N2B, C1B, C2B, N1B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N2B, C1B, N1B, N3B, C2B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Fixed U11: N2A(0.064921) N1B(0.088372) N1A(0.07993) N2B(0.070382)
 C1A(0.07772) C1B(0.082748) N3A(0.074042) N3B(0.06014) C2A(0.065863)
 C2B(0.059547)
 Fixed U12: N2A(-0.003513) N1B(-0.00403) N1A(0.007169) N2B(-0.003555)
 C1A(0.012914) C1B(-0.010694) N3A(0.004549) N3B(-0.00287) C2A(-0.004224) C2B(-
 0.002761)
 Fixed U13: N2A(-0.008679) N1B(0.014691) N1A(-0.015731) N2B(0.006042) C1A(-
 0.000349) C1B(-0.006384) N3A(-0.025803) N3B(0.024063) C2A(-0.026637)
 C2B(0.026644)
 Fixed U22: N2A(0.02857) N1B(0.02152) N1A(0.01973) N2B(0.03038) C1A(0.03681)
 C1B(0.03949) N3A(0.02448) N3B(0.0257) C2A(0.02629) C2B(0.02592)
 Fixed U23: N2A(0.00493) N1B(-0.00062) N1A(0.00101) N2B(0.00785) C1A(0.00953)
 C1B(0.00593) N3A(0.00158) N3B(0.00033) C2A(0.00633) C2B(0.0021)
 Fixed U33: N2A(0.0617) N1B(0.06141) N1A(0.06483) N2B(0.05999) C1A(0.06243)
 C1B(0.05435) N3A(0.10023) N3B(0.10598) C2A(0.10624) C2B(0.10568)
5.a Aromatic/amide H refined with riding coordinates:
 N2A(H2A), N1B(H1B), N1A(H1A), N2B(H2B), C1A(H1AA), C1B(H1BA), C2A(H2AA),
 C2B(H2BA)
;
_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
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.24999(2) 0.49490(2) 0.36087(3) 0.03479(14) Uani 1 1 d . . . . .
Cl1 Cl 0.24975(11) 0.7632(2) 0.1348(2) 0.0582(6) Uani 1 1 d . . . . .
Cl2 Cl 0.24993(13) 0.1924(2) 0.5466(3) 0.0624(6) Uani 1 1 d . . . . .
Cl4 Cl 0.38298(12) 0.48898(18) 0.3562(4) 0.0586(6) Uani 1 1 d . . . . .
Cl3 Cl 0.11687(12) 0.48898(18) 0.3560(4) 0.0590(6) Uani 1 1 d . . . . .
N2A N 0.3958(3) 0.3915(7) 0.8492(9) 0.052 Uani 1 1 d D . . . .
H2A H 0.377761 0.299294 0.868502 0.062 Uiso 1 1 calc R U . . .
N1B N 0.0897(3) 0.6402(7) 0.8288(9) 0.057 Uani 1 1 d D . . . .
H1B H 0.094894 0.744080 0.832354 0.069 Uiso 1 1 calc R U . . .
N1A N 0.4102(3) 0.6398(7) 0.8273(9) 0.055 Uani 1 1 d D . . . .
H1A H 0.404985 0.743709 0.829031 0.066 Uiso 1 1 calc R U . . .
N2B N 0.1041(3) 0.3913(7) 0.8501(9) 0.054 Uani 1 1 d D . . . .
H2B H 0.122087 0.299077 0.870171 0.064 Uiso 1 1 calc R U . . .
C1A C 0.3679(5) 0.5307(9) 0.8656(13) 0.059 Uani 1 1 d D . . . .
H1AA H 0.326150 0.549021 0.898184 0.071 Uiso 1 1 calc R U . . .
C1B C 0.1319(5) 0.5298(9) 0.8658(13) 0.059 Uani 1 1 d D . . . .
H1BA H 0.173818 0.547646 0.897290 0.071 Uiso 1 1 calc R U . . .
N3A N 0.4556(3) 0.4077(7) 0.7990(11) 0.066 Uani 1 1 d D . . . .
N3B N 0.0443(3) 0.4078(7) 0.7990(11) 0.064 Uani 1 1 d D . . . .
C2A C 0.4630(4) 0.5620(9) 0.7849(14) 0.066 Uani 1 1 d D . . . .
H2AA H 0.500263 0.612489 0.749740 0.079 Uiso 1 1 calc R U . . .
C2B C 0.0371(4) 0.5618(9) 0.7846(14) 0.064 Uani 1 1 d D . . . .
H2BA H -0.000046 0.612226 0.748004 0.076 Uiso 1 1 calc R U . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 7 -8 0.0869
0 7 8 0.0832
-1 1 10 0.0738
-1 -12 1 0.4117
1 0 -10 0.0824
-2 12 -1 0.1383
-30 1 0 0.0656
30 0 0 0.0459
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Cl1 Pb1 Cl1 82.509(7) . 4_576 ?
Cl1 Pb1 Cl2 86.53(5) . 4_565 ?
Cl1 Pb1 Cl2 171.75(5) . . ?
Cl1 Pb1 Cl2 105.74(5) 4_576 . ?
Cl1 Pb1 Cl4 90.45(7) . . ?
Cl1 Pb1 Cl3 90.27(7) . . ?
Cl2 Pb1 Cl1 169.04(5) 4_565 4_576 ?
Cl2 Pb1 Cl2 85.221(16) 4_565 . ?
Cl2 Pb1 Cl4 88.87(8) 4_565 . ?
Cl2 Pb1 Cl3 88.85(8) 4_565 . ?
Cl4 Pb1 Cl1 91.31(7) . 4_576 ?
Cl4 Pb1 Cl2 89.51(7) . . ?
Cl4 Pb1 Cl3 177.57(5) . . ?
Cl3 Pb1 Cl1 91.08(7) . 4_576 ?
Cl3 Pb1 Cl2 89.45(7) . . ?
Pb1 Cl1 Pb1 171.65(7) . 4_575 ?
Pb1 Cl2 Pb1 152.44(8) 4_566 . ?
C1A N2A H2A 124.0 . . ?
C1A N2A N3A 112.1(6) . . ?
N3A N2A H2A 124.0 . . ?
C1B N1B H1B 126.5 . . ?
C1B N1B C2B 107.0(7) . . ?
C2B N1B H1B 126.5 . . ?
C1A N1A H1A 126.2 . . ?
C1A N1A C2A 107.6(6) . . ?
C2A N1A H1A 126.2 . . ?
C1B N2B H2B 124.1 . . ?
C1B N2B N3B 111.9(7) . . ?
N3B N2B H2B 124.1 . . ?
N2A C1A N1A 105.8(8) . . ?
N2A C1A H1AA 127.1 . . ?
N1A C1A H1AA 127.1 . . ?
N1B C1B H1BA 126.8 . . ?
N2B C1B N1B 106.3(8) . . ?
N2B C1B H1BA 126.8 . . ?
C2A N3A N2A 103.8(6) . . ?
C2B N3B N2B 103.8(6) . . ?
N1A C2A H2AA 124.6 . . ?
N3A C2A N1A 110.7(7) . . ?
N3A C2A H2AA 124.6 . . ?
N1B C2B H2BA 124.5 . . ?
N3B C2B N1B 111.0(7) . . ?
N3B C2B H2BA 124.5 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb1 Cl1 2.7920(15) . ?
Pb1 Cl1 2.8622(15) 4_576 ?
Pb1 Cl2 2.8094(17) 4_565 ?
Pb1 Cl2 2.8671(16) . ?
Pb1 Cl4 2.854(3) . ?
Pb1 Cl3 2.857(3) . ?
N2A H2A 0.8700 . ?
N2A C1A 1.308(9) . ?
N2A N3A 1.344(8) . ?
N1B H1B 0.8700 . ?
N1B C1B 1.318(10) . ?
N1B C2B 1.345(10) . ?
N1A H1A 0.8700 . ?
N1A C1A 1.315(10) . ?
N1A C2A 1.342(10) . ?
N2B H2B 0.8700 . ?
N2B C1B 1.301(9) . ?
N2B N3B 1.346(9) . ?
C1A H1AA 0.9400 . ?
C1B H1BA 0.9400 . ?
N3A C2A 1.295(10) . ?
N3B C2B 1.292(10) . ?
C2A H2AA 0.9400 . ?
C2B H2BA 0.9400 . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N2A N3A C2A N1A 0.9(9) . . . . ?
N2B N3B C2B N1B -1.4(9) . . . . ?
C1A N2A N3A C2A -0.2(9) . . . . ?
C1A N1A C2A N3A -1.3(10) . . . . ?
C1B N1B C2B N3B 2.4(10) . . . . ?
C1B N2B N3B C2B 0.0(9) . . . . ?
N3A N2A C1A N1A -0.6(10) . . . . ?
N3B N2B C1B N1B 1.4(10) . . . . ?
C2A N1A C1A N2A 1.1(10) . . . . ?
C2B N1B C1B N2B -2.2(10) . . . . ?
