#------------------------------------------------------------------------------
#$Date: 2024-05-05 05:50:17 +0300 (Sun, 05 May 2024) $
#$Revision: 291625 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/55/7715588.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_7715588
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         'Cl2.286 Pb0.571, 1.143(C2 H4 N3)'
_chemical_formula_sum            'C2.29 H4.57 Cl2.29 N3.43 Pb0.57'
_chemical_formula_weight         279.52
_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            7
_cell_length_a                   7.4798(4)
_cell_length_b                   21.5667(13)
_cell_length_c                   8.3086(4)
_cell_measurement_reflns_used    5993
_cell_measurement_temperature    280.01(10)
_cell_measurement_theta_max      28.7960
_cell_measurement_theta_min      3.6460
_cell_volume                     1340.30(13)
_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      280.15
_diffrn_detector_area_resol_mean 8.0772
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.912
_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  0.0396
_diffrn_reflns_av_unetI/netI     0.0226
_diffrn_reflns_Laue_measured_fraction_full 0.972
_diffrn_reflns_Laue_measured_fraction_max 0.912
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            13755
_diffrn_reflns_point_group_measured_fraction_full 0.972
_diffrn_reflns_point_group_measured_fraction_max 0.912
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         28.970
_diffrn_reflns_theta_min         2.627
_exptl_absorpt_coefficient_mu    13.364
_exptl_absorpt_correction_T_max  0.248
_exptl_absorpt_correction_T_min  0.057
_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    2.424
_exptl_crystal_description       block
_exptl_crystal_F_000             896
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.496
_refine_diff_density_min         -1.216
_refine_diff_density_rms         0.134
_refine_ls_extinction_coef       0.0146(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.133
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     78
_refine_ls_number_reflns         1662
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.133
_refine_ls_R_factor_all          0.0325
_refine_ls_R_factor_gt           0.0244
_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/[σ²(Fo²)+(0.0243P)²+1.3366P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0546
_refine_ls_wR_factor_ref         0.0575
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1339
_reflns_number_total             1662
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4dt00406j2.cif
_cod_data_source_block           triag2pbcl4_iii_280_00
_cod_depositor_comments
'Adding full bibliography for 7715584--7715597.cif.'
_cod_database_code               7715588
_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   0.297
_shelx_estimated_absorpt_t_min   0.050
_olex2_refinement_description
;
1.a Aromatic/amide H refined with riding coordinates:
 N2(H2), N1(H1), C1(H1A), C2(H2A)
;
_shelx_res_file
;
TITL triag2pbcl4_280_a.res in Pnma
    triag2pbcl4_iii_280_00.res
    created by SHELXL-2018/3 at 11:23:07 on 04-Mar-2024
REM Old TITL TRIAG2PbCl4_280 in Pnma
REM SHELXT solution in Pnma: R1 0.099, Rweak 0.011, Alpha 0.014
REM <I/s> 1.866 for 218 systematic absences, Orientation as input
REM Formula found by SHELXT: C10 Cl4 Pb
CELL 0.71073 7.4798 21.5667 8.3086 90 90 90
ZERR 4 0.0004 0.0013 0.0004 0 0 0
LATT 1
SYMM 0.5-X,-Y,0.5+Z
SYMM -X,0.5+Y,-Z
SYMM 0.5+X,0.5-Y,0.5-Z
SFAC C H Cl N Pb
UNIT 16 32 16 24 4

L.S. 44
PLAN  2
SIZE 0.12 0.18 0.56
TEMP 7
CONF
list 4
MORE -1
BOND $H
fmap 2 53
acta 50
OMIT 0 0 2
OMIT 0 0 4
OMIT 0 0 6
OMIT 0 2 4
OMIT 0 3 1
OMIT 0 5 1
OMIT 0 7 1
OMIT 0 8 0
OMIT 1 0 3
OMIT 1 1 3
OMIT 1 1 5
OMIT 4 3 0
OMIT 5 0 1
OMIT 5 2 1
OMIT 5 2 3
OMIT 5 2 7
OMIT 5 4 3
OMIT 5 6 1
OMIT 5 6 3
OMIT 5 6 5
OMIT 5 6 7
OMIT 5 8 1
OMIT 5 8 3
OMIT 5 10 1
OMIT 5 10 3
OMIT 5 12 3
OMIT 5 14 1
OMIT 5 16 3
OMIT 7 3 3
OMIT 7 5 3
OMIT 8 0 2
OMIT 8 2 2
REM <olex2.extras>
REM <HklSrc "%.\\triag2pbcl4_iii_280_00.hkl">
REM </olex2.extras>

WGHT    0.024300    1.336600
EXTI    0.014637
FVAR       0.29497
PB1   5    0.349744    0.250000    0.496549    10.50000    0.02067    0.03270 =
         0.01739    0.00000   -0.00031    0.00000
CL3   3    0.343675    0.117242    0.493008    11.00000    0.08256    0.03470 =
         0.02710    0.00084   -0.00076   -0.00150
CL2   3    0.543480    0.250000    0.199863    10.50000    0.04776    0.08135 =
         0.04365    0.00000    0.02602    0.00000
N2    4    0.838371    0.104600    0.386996    11.00000    0.06663    0.04431 =
         0.03322    0.00314    0.00793   -0.00566
AFIX  43
H2    2    0.854594    0.122395    0.295526    11.00000    0.05233
AFIX   0
N1    4    0.818761    0.091311    0.636301    11.00000    0.06104    0.06381 =
         0.02447   -0.00673    0.00227    0.00099
AFIX  43
H1    2    0.819274    0.097146    0.738693    11.00000    0.06516
AFIX   0
C1    1    0.854666    0.132397    0.524925    11.00000    0.05837    0.04920 =
         0.05221   -0.01346    0.00603   -0.01081
AFIX  43
H1A   2    0.885906    0.173650    0.541411    11.00000    0.03956
AFIX   0
C2    1    0.780863    0.038092    0.558688    11.00000    0.09808    0.04781 =
         0.03405    0.00275    0.00808   -0.00173
AFIX  43
H2A   2    0.749800    0.001254    0.609710    11.00000    0.09671
AFIX   0
N3    4    0.793039    0.044598    0.404531    11.00000    0.10119    0.04058 =
         0.03563   -0.00472    0.00257   -0.00663

CL1   3    0.621345    0.250000    0.737400    10.50000    0.03586    0.07933 =
         0.03792    0.00000   -0.01742    0.00000
HKLF 4




REM  triag2pbcl4_280_a.res in Pnma
REM wR2 = 0.0575, GooF = S = 1.133, Restrained GooF = 1.133 for all data
REM R1 = 0.0244 for 1339 Fo > 4sig(Fo) and 0.0325 for all 1662 data
REM 78 parameters refined using 0 restraints

END

WGHT      0.0243      1.3366

REM Highest difference peak  1.496,  deepest hole -1.216,  1-sigma level  0.134
Q1    1   0.3444  0.2500  0.3934  10.50000  0.05    1.50
Q2    1   0.3501  0.2500  0.6077  10.50000  0.05    1.43
;
_shelx_res_checksum              23204
_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+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, 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 0.34974(3) 0.250000 0.49655(2) 0.02359(12) Uani 1 2 d S T P . .
Cl3 Cl 0.3437(2) 0.11724(6) 0.49301(10) 0.0481(4) Uani 1 1 d . . . . .
Cl2 Cl 0.5435(3) 0.250000 0.1999(2) 0.0576(5) Uani 1 2 d S T P . .
N2 N 0.8384(6) 0.1046(2) 0.3870(5) 0.0481(11) Uani 1 1 d . . . . .
H2 H 0.854594 0.122395 0.295526 0.052(15) Uiso 1 1 calc R . . . .
N1 N 0.8188(6) 0.0913(2) 0.6363(5) 0.0498(11) Uani 1 1 d . . . . .
H1 H 0.819274 0.097146 0.738693 0.065(16) Uiso 1 1 calc R . . . .
C1 C 0.8547(8) 0.1324(3) 0.5249(6) 0.0533(15) Uani 1 1 d . . . . .
H1A H 0.885906 0.173650 0.541411 0.040(12) Uiso 1 1 calc R . . . .
C2 C 0.7809(10) 0.0381(3) 0.5587(6) 0.0600(16) Uani 1 1 d . . . . .
H2A H 0.749800 0.001254 0.609710 0.10(2) Uiso 1 1 calc R . . . .
N3 N 0.7930(8) 0.04460(19) 0.4045(5) 0.0591(13) Uani 1 1 d . . . . .
Cl1 Cl 0.6213(2) 0.250000 0.73740(19) 0.0510(5) Uani 1 2 d S T P . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Pb1 0.02067(15) 0.03270(16) 0.01739(14) 0.000 -0.00031(7) 0.000
Cl3 0.0826(12) 0.0347(6) 0.0271(6) 0.0008(4) -0.0008(5) -0.0015(6)
Cl2 0.0478(11) 0.0814(13) 0.0437(9) 0.000 0.0260(8) 0.000
N2 0.067(3) 0.044(2) 0.033(2) 0.0031(18) 0.0079(18) -0.0057(19)
N1 0.061(3) 0.064(3) 0.024(2) -0.0067(19) 0.0023(17) 0.001(2)
C1 0.058(4) 0.049(3) 0.052(3) -0.013(2) 0.006(2) -0.011(3)
C2 0.098(5) 0.048(3) 0.034(2) 0.003(2) 0.008(3) -0.002(3)
N3 0.101(4) 0.041(3) 0.036(2) -0.0047(18) 0.003(2) -0.007(2)
Cl1 0.0359(8) 0.0793(12) 0.0379(9) 0.000 -0.0174(7) 0.000
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
8 1 -7 0.0869
-8 0 -7 0.0832
-11 -1 -1 0.0738
-1 -1 12 0.4117
11 1 0 0.0824
1 -2 -12 0.1383
0 -30 -1 0.0656
0 30 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
Cl3 Pb1 Cl3 177.84(6) 7_565 . ?
Cl2 Pb1 Cl3 88.92(3) 6_556 . ?
Cl2 Pb1 Cl3 89.95(2) . . ?
Cl2 Pb1 Cl3 89.95(2) . 7_565 ?
Cl2 Pb1 Cl3 88.92(3) 6_556 7_565 ?
Cl2 Pb1 Cl2 84.984(14) 6_556 . ?
Cl2 Pb1 Cl1 170.90(5) 6_556 . ?
Cl1 Pb1 Cl3 91.06(3) . . ?
Cl1 Pb1 Cl3 89.91(2) 6_557 7_565 ?
Cl1 Pb1 Cl3 91.06(3) . 7_565 ?
Cl1 Pb1 Cl3 89.91(2) 6_557 . ?
Cl1 Pb1 Cl2 87.77(5) 6_557 6_556 ?
Cl1 Pb1 Cl2 104.12(5) . . ?
Cl1 Pb1 Cl2 172.75(5) 6_557 . ?
Cl1 Pb1 Cl1 83.129(7) 6_557 . ?
Pb1 Cl2 Pb1 155.91(8) 6_656 . ?
C1 N2 H2 124.1 . . ?
C1 N2 N3 111.8(4) . . ?
N3 N2 H2 124.1 . . ?
C1 N1 H1 126.8 . . ?
C1 N1 C2 106.4(4) . . ?
C2 N1 H1 126.8 . . ?
N2 C1 N1 107.0(5) . . ?
N2 C1 H1A 126.5 . . ?
N1 C1 H1A 126.5 . . ?
N1 C2 H2A 124.2 . . ?
N3 C2 N1 111.6(4) . . ?
N3 C2 H2A 124.2 . . ?
C2 N3 N2 103.3(4) . . ?
Pb1 Cl1 Pb1 172.27(7) 6_657 . ?
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 Cl3 2.8637(14) . ?
Pb1 Cl3 2.8636(14) 7_565 ?
Pb1 Cl2 2.8126(16) 6_556 ?
Pb1 Cl2 2.8594(15) . ?
Pb1 Cl1 2.7937(15) 6_557 ?
Pb1 Cl1 2.8516(14) . ?
N2 H2 0.8600 . ?
N2 C1 1.299(6) . ?
N2 N3 1.346(6) . ?
N1 H1 0.8600 . ?
N1 C1 1.309(7) . ?
N1 C2 1.347(7) . ?
C1 H1A 0.9300 . ?
C2 H2A 0.9300 . ?
C2 N3 1.292(7) . ?
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
N1 C2 N3 N2 -0.7(6) . . . . ?
C1 N2 N3 C2 0.8(6) . . . . ?
C1 N1 C2 N3 0.4(7) . . . . ?
C2 N1 C1 N2 0.1(7) . . . . ?
N3 N2 C1 N1 -0.6(7) . . . . ?
