#------------------------------------------------------------------------------
#$Date: 2024-05-05 05:50:17 +0300 (Sun, 05 May 2024) $
#$Revision: 291625 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/55/7715595.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_7715595
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, 4(C H2 N1.5)'
_chemical_formula_sum            'C4 H8 Cl4 N6 Pb'
_chemical_formula_weight         489.15
_chemical_name_systematic        (TzH)2PbCl4
_space_group_crystal_system      orthorhombic
_space_group_IT_number           69
_space_group_name_Hall           '-F 2 2'
_space_group_name_H-M_alt        'F m m m'
_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                   7.6009(7)
_cell_length_b                   8.3017(6)
_cell_length_c                   21.798(2)
_cell_measurement_reflns_used    4584
_cell_measurement_temperature    390.01(10)
_cell_measurement_theta_max      28.5420
_cell_measurement_theta_min      2.7170
_cell_volume                     1375.5(2)
_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      390.15
_diffrn_detector_area_resol_mean 16.1544
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.952
_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  0.0767
_diffrn_reflns_av_unetI/netI     0.0323
_diffrn_reflns_Laue_measured_fraction_full 0.975
_diffrn_reflns_Laue_measured_fraction_max 0.952
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            6239
_diffrn_reflns_point_group_measured_fraction_full 0.975
_diffrn_reflns_point_group_measured_fraction_max 0.952
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         29.013
_diffrn_reflns_theta_min         3.739
_exptl_absorpt_coefficient_mu    13.023
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.06892
_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    2.362
_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         1.470
_refine_diff_density_min         -1.286
_refine_diff_density_rms         0.185
_refine_ls_extinction_coef       0.00175(19)
_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   1.038
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     30
_refine_ls_number_reflns         513
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0252
_refine_ls_R_factor_gt           0.0251
_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)+(0.0325P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0524
_refine_ls_wR_factor_ref         0.0525
_reflns_Friedel_coverage         0.000
_reflns_number_gt                512
_reflns_number_total             513
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4dt00406j2.cif
_cod_data_source_block           triag2pbcl4_i_390_00
_cod_depositor_comments
'Adding full bibliography for 7715584--7715597.cif.'
_cod_original_cell_volume        1375.4(2)
_cod_database_code               7715595
_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   0.263
_shelx_estimated_absorpt_t_min   0.046
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
2. Shared sites
{C2, N2}
3. Uiso/Uaniso restraints and constraints
Uanis(C2) = Uanis(N2)
4. Rigid body (RIGU) restrains
 C2, N2, N1, C1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: H1A(0.25) H1B(0.25) C2(0.25) H2(0.25) N2(0.25)
6.a Aromatic/amide H refined with riding coordinates:
 N1(H1A), N1(H1B), C1(H1), C2(H2)
;
_shelx_res_file
;
TITL triag2pbcl4_temp2_4_390_00_a.res in Fmmm
    triag2pbcl4_i_390_00.res
    created by SHELXL-2018/3 at 13:05:56 on 15-Dec-2023
REM Old TITL TRIAG2PbCl4_temp2_4_390_00 in Fmm2
REM SHELXT solution in Fmmm: R1 0.093, Rweak 0.358, Alpha 0.039
REM <I/s> 0.000 for 0 systematic absences, Orientation as input
REM Formula found by SHELXT: C6 Cl4 Pb
CELL 0.71073 7.6009 8.3017 21.7977 90 90 90
ZERR 4 0.0007 0.0006 0.0021 0 0 0
LATT 4
SYMM -X,-Y,+Z
SYMM -X,+Y,-Z
SYMM +X,-Y,-Z
SFAC C H Cl N Pb
UNIT 16 32 16 24 4
EADP C2 N2
RIGU C2 N2 N1 C1
EXYZ C2 N2

L.S. 44 0 0
PLAN  1
SIZE 0.616 0.26 0.14
TEMP 117
CONF
BOND
list 4
MORE -1
BOND $H
fmap 2 53
acta 50
OMIT 0 0 10
OMIT 0 0 12
OMIT 0 0 14
OMIT 0 0 16
OMIT 0 2 0
OMIT 0 2 16
OMIT 0 4 0
OMIT 2 0 4
OMIT 4 6 22
OMIT 5 3 25
REM <olex2.extras>
REM <HklSrc "%.\\TRIAG2PbCl4_I_390_00.hkl">
REM </olex2.extras>

WGHT    0.032500
EXTI    0.001747
FVAR       2.13321
PB1   5    0.500000    0.000000    0.000000    10.12500    0.03456    0.02030 =
         0.03877    0.00000    0.00000    0.00000
CL2   3    0.500000    0.000000    0.131147    10.25000    0.13752    0.03674 =
         0.04410    0.00000    0.00000    0.00000
CL1   3    0.250000    0.250000    0.000000    10.25000    0.08277    0.07431 =
         0.10978    0.00000    0.00000    0.05092
N1    4    0.500000    0.376723    0.148968    10.50000    0.12271    0.03981 =
         0.08234   -0.01107    0.00000    0.00000
PART 5
AFIX  43
H1A   2    0.500000    0.278196    0.136782    10.25000   -1.20000
AFIX  43
PART 6
H1B   2    0.500000    0.278196    0.136782    10.25000   -1.20000
AFIX   0
PART 0
C1    1    0.500000    0.500000    0.113677    10.25000    0.10601    0.06844 =
         0.05768    0.00000    0.00000    0.00000
AFIX  43
H1    2    0.500000    0.500000    0.071012    10.25000    0.14825
AFIX   0
PART 5
C2    1    0.500000    0.423154    0.206504    10.25000    0.25082    0.08348 =
         0.05878    0.02380    0.00000    0.00000
AFIX  43
H2    2    0.500000    0.356588    0.240820    10.25000   -1.20000
AFIX   0
PART 6
N2    4    0.500000    0.423154    0.206504    10.25000    0.25082    0.08348 =
         0.05878    0.02380    0.00000    0.00000
HKLF 4




REM  triag2pbcl4_temp2_4_390_00_a.res in Fmmm
REM wR2 = 0.0525, GooF = S = 1.038, Restrained GooF = 1.037 for all data
REM R1 = 0.0251 for 512 Fo > 4sig(Fo) and 0.0252 for all 513 data
REM 30 parameters refined using 15 restraints

END

WGHT      0.0325      0.0000

REM Highest difference peak  1.470,  deepest hole -1.286,  1-sigma level  0.185
Q1    1   0.4288  0.0929  0.0000  10.50000  0.05    1.47
;
_shelx_res_checksum              76434
_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, z'
'-x, y, -z'
'x, -y, -z'
'x, y+1/2, z+1/2'
'-x, -y+1/2, z+1/2'
'-x, y+1/2, -z+1/2'
'x, -y+1/2, -z+1/2'
'x+1/2, y, z+1/2'
'-x+1/2, -y, z+1/2'
'-x+1/2, y, -z+1/2'
'x+1/2, -y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z'
'-x+1/2, y+1/2, -z'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x, y, -z'
'x, -y, z'
'-x, y, z'
'-x, -y+1/2, -z+1/2'
'x, y+1/2, -z+1/2'
'x, -y+1/2, z+1/2'
'-x, y+1/2, z+1/2'
'-x+1/2, -y, -z+1/2'
'x+1/2, y, -z+1/2'
'x+1/2, -y, z+1/2'
'-x+1/2, y, z+1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, y+1/2, -z'
'x+1/2, -y+1/2, z'
'-x+1/2, y+1/2, z'
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 0.500000 0.000000 0.000000 0.03121(19) Uani 1 8 d S T P . .
Cl2 Cl 0.500000 0.000000 0.13115(12) 0.0728(9) Uani 1 4 d S T P . .
Cl1 Cl 0.250000 0.250000 0.000000 0.0890(10) Uani 1 4 d S T P . .
N1 N 0.500000 0.3767(8) 0.1490(4) 0.082(2) Uani 1 2 d S T P . .
H1A H 0.500000 0.278196 0.136782 0.098 Uiso 0.5 2 calc R U P A 5
H1B H 0.500000 0.278196 0.136782 0.098 Uiso 0.5 2 calc R U P B 6
C1 C 0.500000 0.500000 0.1137(6) 0.077(3) Uani 1 4 d S T P C .
H1 H 0.500000 0.500000 0.071012 0.15(9) Uiso 1 4 calc R . P . .
C2 C 0.500000 0.4232(13) 0.2065(5) 0.131(5) Uani 0.5 2 d S T P C 5
H2 H 0.500000 0.356588 0.240820 0.157 Uiso 0.5 2 calc R U P C 5
N2 N 0.500000 0.4232(13) 0.2065(5) 0.131(5) Uani 0.5 2 d S T P C 6
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 0.0346(2) 0.0203(2) 0.0388(3) 0.000 0.000 0.000
Cl2 0.138(3) 0.0367(11) 0.0441(13) 0.000 0.000 0.000
Cl1 0.0828(19) 0.0743(19) 0.110(3) 0.000 0.000 0.0509(17)
N1 0.123(7) 0.040(3) 0.082(4) -0.011(3) 0.000 0.000
C1 0.106(10) 0.068(6) 0.058(6) 0.000 0.000 0.000
C2 0.251(15) 0.083(6) 0.059(4) 0.024(4) 0.000 0.000
N2 0.251(15) 0.083(6) 0.059(4) 0.024(4) 0.000 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_
_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
Cl2 Pb1 Cl2 180.0 17_655 . ?
Cl1 Pb1 Cl2 90.0 15_545 . ?
Cl1 Pb1 Cl2 90.0 15_545 17_655 ?
Cl1 Pb1 Cl2 90.0 3_655 17_655 ?
Cl1 Pb1 Cl2 90.0 3_655 . ?
Cl1 Pb1 Cl2 90.0 . . ?
Cl1 Pb1 Cl2 90.0 . 17_655 ?
Cl1 Pb1 Cl2 90.0 13_545 17_655 ?
Cl1 Pb1 Cl2 90.0 13_545 . ?
Cl1 Pb1 Cl1 84.953(7) 15_545 13_545 ?
Cl1 Pb1 Cl1 95.047(7) 15_545 . ?
Cl1 Pb1 Cl1 84.953(7) 3_655 . ?
Cl1 Pb1 Cl1 95.047(7) 3_655 13_545 ?
Cl1 Pb1 Cl1 180.0 . 13_545 ?
Cl1 Pb1 Cl1 180.0 15_545 3_655 ?
Pb1 Cl1 Pb1 180.0 13_455 . ?
C1 N1 H1A 125.1 . . ?
C1 N1 H1B 125.1 . . ?
C1 N1 C2 109.8(8) . . ?
C1 N1 N2 109.8(8) . . ?
C2 N1 H1A 125.1 . . ?
N2 N1 H1B 125.1 . . ?
N1 C1 N1 106.1(12) . 2_665 ?
N1 C1 H1 126.9 . . ?
N1 C1 H1 126.9 2_665 . ?
N1 C2 H2 126.5 . . ?
C2 C2 N1 107.1(5) 2_665 . ?
C2 C2 H2 126.5 2_665 . ?
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 Cl2 2.859(3) . ?
Pb1 Cl2 2.859(3) 17_655 ?
Pb1 Cl1 2.81394(16) 15_545 ?
Pb1 Cl1 2.81394(15) 3_655 ?
Pb1 Cl1 2.81394(16) . ?
Pb1 Cl1 2.81394(16) 13_545 ?
N1 H1A 0.8600 . ?
N1 H1B 0.8600 . ?
N1 C1 1.280(11) . ?
N1 C2 1.312(13) . ?
N1 N2 1.312(13) . ?
C1 H1 0.9300 . ?
C2 C2 1.28(2) 2_665 ?
C2 H2 0.9300 . ?
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
C1 N1 C2 C2 0.000(3) . . . 2_665 ?
C2 N1 C1 N1 0.000(1) . . . 2_665 ?
N2 N1 C1 N1 0.000(1) . . . 2_665 ?
