# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2024

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_triag2pbcl4_iv_100_00
_database_code_depnum_ccdc_archive 'CCDC 2314654'
loop_
_audit_author_name
_audit_author_address
'Szymon Sobczak'
;Department of Materials Chemistry, Adam Mickiewicz University
Poland
;
_audit_update_record             
;
2024-03-04 deposited with the CCDC.	2024-03-21 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT972_triag2pbcl4_iv_100_00 
;
PROBLEM: Check Calcd Resid. Dens.  1.05Ang From Pb1            -5.47 eA-3
RESPONSE: Residual density near heavy atom.
;
_vrf_PLAT112_triag2pbcl4_iv_100_00 
;
PROBLEM: ADDSYM Detects New (Pseudo) Symm. Elem         n        100 %Fit
RESPONSE: The symmetry has been thoroughly inspected by the presence of the systematic absences in the raw diffraction data
;
_vrf_PLAT113_triag2pbcl4_iv_100_00 
;
PROBLEM: ADDSYM Suggests Possible Pseudo/New  Space Group       Pnma Check
RESPONSE: look PLAT112
;
# Added during the CSD deposition process: Friday 15 December 2023 12:43 PM
# end Validation Reply Form

_audit_creation_date             2023-12-15
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        Tz2PbCl4
_chemical_formula_moiety         'Cl4 Pb, 2(C2 H4 N3)'
_chemical_formula_sum            'C4 H8 Cl4 N6 Pb'
_chemical_formula_weight         489.15
_chemical_melting_point          ?
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'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
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'

_cell_length_a                   21.419(2)
_cell_length_b                   8.3049(4)
_cell_length_c                   7.3363(4)
_cell_angle_alpha                90
_cell_angle_beta                 90.149(6)
_cell_angle_gamma                90
_cell_volume                     1305.01(16)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    5873
_cell_measurement_temperature    100.2(8)
_cell_measurement_theta_max      28.3430
_cell_measurement_theta_min      3.6670
_shelx_estimated_absorpt_T_max   0.290
_shelx_estimated_absorpt_T_min   0.048
_exptl_absorpt_coefficient_mu    13.726
_exptl_absorpt_correction_T_max  0.776
_exptl_absorpt_correction_T_min  0.491
_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_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.490
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             896
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

_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0374
_diffrn_reflns_av_unetI/netI     0.0328
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.907
_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       -9
_diffrn_reflns_number            14033
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.907
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         28.802
_diffrn_reflns_theta_min         2.630
_diffrn_ambient_temperature      100.15
_diffrn_detector_area_resol_mean 8.0772
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.907
_diffrn_measurement_details      .
_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_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2544
_reflns_number_total             3071
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_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  (Sheldrick, 2015)'
_refine_diff_density_max         1.901
_refine_diff_density_min         -5.705
_refine_diff_density_rms         0.235
_refine_ls_extinction_coef       0.0045(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   1.239
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     137
_refine_ls_number_reflns         3071
_refine_ls_number_restraints     151
_refine_ls_R_factor_all          0.0784
_refine_ls_R_factor_gt           0.0641
_refine_ls_restrained_S_all      1.285
_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)+(0.0271P)²+28.7927P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1213
_refine_ls_wR_factor_ref         0.1297
_refine_special_details          ?
_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. Uiso/Uaniso restraints and constraints
Uanis(Cl2) \\sim Ueq, Uanis(Pb1) \\sim Ueq, Uanis(Cl1) \\sim Ueq, Uanis(Cl4)
\\sim Ueq, Uanis(Cl3) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(N3A) \\sim Ueq, Uanis(N2A) \\sim Ueq, Uanis(C1A) \\sim Ueq, Uanis(C2A)
\\sim Ueq, Uanis(N1A) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(N2B) \\sim Ueq, Uanis(C1B) \\sim Ueq, Uanis(N1B) \\sim Ueq, Uanis(N3B)
\\sim Ueq, Uanis(C2B) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
4. 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
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)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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 0.25000(3) 0.49134(4) 0.36607(5) 0.0387(2) Uani 1 1 d . U . . .
Cl1 Cl 0.2498(2) 0.7642(3) 0.1436(3) 0.0526(10) Uani 1 1 d . U . . .
Cl2 Cl 0.2499(2) 0.1794(3) 0.5361(4) 0.0522(10) Uani 1 1 d . U . . .
Cl4 Cl 0.3827(2) 0.4815(3) 0.3640(6) 0.0553(10) Uani 1 1 d . U . . .
Cl3 Cl 0.1172(2) 0.4816(3) 0.3641(5) 0.0548(10) Uani 1 1 d . U . . .
N2A N 0.3953(5) 0.3997(12) 0.8570(15) 0.043(3) Uani 1 1 d D U . . .
H2A H 0.376224 0.307604 0.877297 0.051 Uiso 1 1 calc R U . . .
N1B N 0.0869(5) 0.6496(12) 0.8317(15) 0.045(2) Uani 1 1 d D U . . .
H1B H 0.091533 0.754893 0.833307 0.054 Uiso 1 1 calc R U . . .
N1A N 0.4130(6) 0.6489(12) 0.8323(15) 0.046(3) Uani 1 1 d D U . . .
H1A H 0.408447 0.754226 0.833230 0.056 Uiso 1 1 calc R U . . .
N2B N 0.1040(6) 0.3998(12) 0.8570(15) 0.044(2) Uani 1 1 d D U . . .
H2B H 0.123020 0.307812 0.878371 0.053 Uiso 1 1 calc R U . . .
C1A C 0.3694(7) 0.5409(14) 0.8748(19) 0.045(3) Uani 1 1 d D U . . .
H1AA H 0.327665 0.562476 0.910995 0.054 Uiso 1 1 calc R U . . .
C1B C 0.1302(7) 0.5410(14) 0.8738(19) 0.045(3) Uani 1 1 d D U . . .
H1BA H 0.172088 0.561996 0.909305 0.054 Uiso 1 1 calc R U . . .
N3A N 0.4549(6) 0.4132(12) 0.8037(18) 0.053(3) Uani 1 1 d D U . . .
N3B N 0.0444(6) 0.4132(12) 0.8028(17) 0.051(3) Uani 1 1 d D U . . .
C2A C 0.4657(7) 0.5674(15) 0.787(2) 0.053(4) Uani 1 1 d D U . . .
H2AA H 0.504047 0.614616 0.750195 0.063 Uiso 1 1 calc R U . . .
C2B C 0.0342(7) 0.5679(14) 0.786(2) 0.050(3) Uani 1 1 d D U . . .
H2BA H -0.003973 0.615479 0.747631 0.060 Uiso 1 1 calc R U . . .

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 0.1012(5) 0.0074(2) 0.0074(2) -0.00026(12) 0.00036(19) 0.0000(2)
Cl1 0.131(3) 0.0153(11) 0.0117(12) 0.0041(9) -0.0003(15) 0.0008(15)
Cl2 0.123(3) 0.0158(12) 0.0179(12) 0.0075(9) 0.0006(15) 0.0006(15)
Cl4 0.088(3) 0.0113(12) 0.067(2) 0.0001(12) -0.0170(19) -0.0045(14)
Cl3 0.085(3) 0.0109(12) 0.068(2) 0.0007(12) 0.0189(19) 0.0033(14)
N2A 0.055(6) 0.023(5) 0.050(6) 0.003(4) -0.012(5) 0.004(4)
N1B 0.062(5) 0.023(4) 0.049(5) 0.003(3) 0.020(4) -0.001(3)
N1A 0.069(7) 0.020(4) 0.050(6) -0.001(4) -0.020(5) 0.000(5)
N2B 0.059(5) 0.022(4) 0.051(5) 0.002(3) 0.018(4) -0.004(3)
C1A 0.061(7) 0.031(6) 0.042(6) 0.001(5) -0.001(5) 0.008(5)
C1B 0.064(5) 0.025(4) 0.047(6) 0.003(4) 0.010(4) -0.005(4)
N3A 0.066(7) 0.023(5) 0.071(7) -0.001(5) -0.032(5) 0.002(5)
N3B 0.058(5) 0.025(4) 0.071(6) -0.001(4) 0.025(4) -0.002(3)
C2A 0.058(7) 0.028(5) 0.073(8) 0.001(5) -0.023(6) 0.000(5)
C2B 0.058(5) 0.026(4) 0.066(7) 0.001(4) 0.022(4) -0.002(4)

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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 2.793(2) . ?
Pb1 Cl1 2.875(2) 4_576 ?
Pb1 Cl2 2.806(3) 4_565 ?
Pb1 Cl2 2.875(3) . ?
Pb1 Cl4 2.844(5) . ?
Pb1 Cl3 2.845(4) . ?
N2A H2A 0.8800 . ?
N2A C1A 1.305(14) . ?
N2A N3A 1.340(15) . ?
N1B H1B 0.8800 . ?
N1B C1B 1.329(15) . ?
N1B C2B 1.358(16) . ?
N1A H1A 0.8800 . ?
N1A C1A 1.333(15) . ?
N1A C2A 1.358(16) . ?
N2B H2B 0.8800 . ?
N2B C1B 1.305(14) . ?
N2B N3B 1.340(15) . ?
C1A H1AA 0.9500 . ?
C1B H1BA 0.9500 . ?
N3A C2A 1.307(15) . ?
N3B C2B 1.309(14) . ?
C2A H2AA 0.9500 . ?
C2B H2BA 0.9500 . ?

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 80.844(13) . 4_576 ?
Cl1 Pb1 Cl2 84.59(8) . 4_565 ?
Cl1 Pb1 Cl2 169.94(8) . . ?
Cl1 Pb1 Cl4 91.14(12) . . ?
Cl1 Pb1 Cl3 91.17(12) . . ?
Cl2 Pb1 Cl1 165.44(8) 4_565 4_576 ?
Cl2 Pb1 Cl1 109.21(8) . 4_576 ?
Cl2 Pb1 Cl2 85.35(3) 4_565 . ?
Cl2 Pb1 Cl4 88.81(12) 4_565 . ?
Cl2 Pb1 Cl3 89.02(12) 4_565 . ?
Cl4 Pb1 Cl1 91.55(12) . 4_576 ?
Cl4 Pb1 Cl2 88.75(11) . . ?
Cl4 Pb1 Cl3 176.67(8) . . ?
Cl3 Pb1 Cl1 91.18(12) . 4_576 ?
Cl3 Pb1 Cl2 88.56(11) . . ?
Pb1 Cl1 Pb1 170.68(11) . 4_575 ?
Pb1 Cl2 Pb1 146.06(11) 4_566 . ?
C1A N2A H2A 124.5 . . ?
C1A N2A N3A 111.1(11) . . ?
N3A N2A H2A 124.5 . . ?
C1B N1B H1B 126.4 . . ?
C1B N1B C2B 107.3(11) . . ?
C2B N1B H1B 126.4 . . ?
C1A N1A H1A 126.1 . . ?
C1A N1A C2A 107.8(11) . . ?
C2A N1A H1A 126.1 . . ?
C1B N2B H2B 124.4 . . ?
C1B N2B N3B 111.3(11) . . ?
N3B N2B H2B 124.4 . . ?
N2A C1A N1A 106.4(12) . . ?
N2A C1A H1AA 126.8 . . ?
N1A C1A H1AA 126.8 . . ?
N1B C1B H1BA 126.6 . . ?
N2B C1B N1B 106.8(12) . . ?
N2B C1B H1BA 126.6 . . ?
C2A N3A N2A 106.1(12) . . ?
C2B N3B N2B 105.6(12) . . ?
N1A C2A H2AA 125.7 . . ?
N3A C2A N1A 108.6(13) . . ?
N3A C2A H2AA 125.7 . . ?
N1B C2B H2BA 125.4 . . ?
N3B C2B N1B 109.1(13) . . ?
N3B C2B H2BA 125.4 . . ?

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 0.6(16) . . . . ?
N2B N3B C2B N1B -0.8(16) . . . . ?
C1A N2A N3A C2A -0.4(15) . . . . ?
C1A N1A C2A N3A -0.6(16) . . . . ?
C1B N1B C2B N3B 1.2(16) . . . . ?
C1B N2B N3B C2B 0.1(15) . . . . ?
N3A N2A C1A N1A 0.0(15) . . . . ?
N3B N2B C1B N1B 0.6(15) . . . . ?
C2A N1A C1A N2A 0.4(15) . . . . ?
C2B N1B C1B N2B -1.1(15) . . . . ?

_shelx_res_file                  
;
TITL triag2pbcl4_05_100_00c_a.res in P2(1)/c
    triag2pbcl4_iv_100_00.res
    created by SHELXL-2019/2 at 16:40:54 on 01-Mar-2024
REM Old TITL TRIAG2PbCl4_05_100_00c in P21/c #14
REM SHELXT solution in P2(1)/c: R1 0.401, Rweak 0.177, Alpha 0.022
REM <I/s> 1.357 for 199 systematic absences, Orientation a'=c, b'=-b, c'=a
REM Formula found by SHELXT: C7 N2B Cl4 Pb
CELL 0.71073 21.4193 8.3049 7.3363 90 90.149 90
ZERR 4 0.0021 0.0004 0.0004 0 0.006 0
LATT 1
SYMM -X,0.5+Y,0.5-Z
SFAC C H Cl N Pb
UNIT 16 32 16 24 4
ISOR 0.01 0.02 Cl2 Pb1 Cl1 Cl4 Cl3
RIGU Cl2 Pb1 Cl1 Cl4 Cl3
RIGU N3B N2B C1B C2B N1B
ISOR 0.01 0.02 N3A N2A C1A C2A N1A
RIGU N2B C1B N1B N3B C2B
ISOR 0.01 0.02 N2B C1B N1B N3B C2B
SADI N3A N2A N3B N2B
SADI N3B C2B N3A C2A
SADI N2A C1A N2B C1B
SADI N1B C1B N1A C1A
SADI N1B C2B N1A C2A

L.S. 45
PLAN  5
SIZE 0.12 0.16 0.50
TEMP -173
CONF
BOND
list 4
MORE -1
BOND $H
fmap 2
acta 50
OMIT -24 3 2
OMIT -24 4 1
OMIT -24 5 2
OMIT -23 1 2
OMIT -23 1 4
OMIT -23 4 1
OMIT -22 1 3
OMIT -22 2 1
OMIT -22 3 2
OMIT -22 4 3
OMIT -22 5 2
OMIT -21 4 1
OMIT 0 2 0
OMIT 0 4 0
OMIT 1 2 0
OMIT 8 0 0
OMIT 22 1 2
OMIT 22 2 1
OMIT 22 3 2
OMIT 23 5 2
OMIT 24 2 1
OMIT 24 3 2
OMIT 25 1 2
OMIT 25 3 0
OMIT 25 4 1
OMIT 27 3 0
REM <olex2.extras>
REM <HklSrc "%.\\triag2pbcl4_iv_100_00.hkl">
REM </olex2.extras>

WGHT    0.027100   28.792702
EXTI    0.004493
FVAR       2.81372
PB1   5    0.250003    0.491337    0.366066    11.00000    0.10125    0.00743 =
         0.00738   -0.00026    0.00036    0.00003
CL1   3    0.249832    0.764190    0.143606    11.00000    0.13072    0.01530 =
         0.01171    0.00406   -0.00032    0.00078
CL2   3    0.249938    0.179379    0.536061    11.00000    0.12299    0.01582 =
         0.01791    0.00752    0.00056    0.00063
CL4   3    0.382702    0.481533    0.363982    11.00000    0.08758    0.01132 =
         0.06677    0.00014   -0.01698   -0.00446
CL3   3    0.117232    0.481568    0.364079    11.00000    0.08526    0.01087 =
         0.06829    0.00071    0.01892    0.00326
N2A   4    0.395332    0.399656    0.857017    11.00000    0.05482    0.02328 =
         0.05026    0.00343   -0.01157    0.00390
AFIX  43
H2A   2    0.376224    0.307604    0.877297    11.00000   -1.20000
AFIX   0

N1B   4    0.086906    0.649614    0.831744    11.00000    0.06198    0.02295 =
         0.04944    0.00279    0.01979   -0.00132
AFIX  43
H1B   2    0.091533    0.754893    0.833307    11.00000   -1.20000
AFIX   0

N1A   4    0.413004    0.648922    0.832323    11.00000    0.06900    0.02026 =
         0.04988   -0.00127   -0.01985   -0.00027
AFIX  43
H1A   2    0.408447    0.754226    0.833230    11.00000   -1.20000
AFIX   0

N2B   4    0.104008    0.399848    0.856961    11.00000    0.05937    0.02250 =
         0.05059    0.00165    0.01793   -0.00380
AFIX  43
H2B   2    0.123020    0.307812    0.878371    11.00000   -1.20000
AFIX   0

C1A   1    0.369392    0.540895    0.874846    11.00000    0.06115    0.03106 =
         0.04246    0.00069   -0.00106    0.00802
AFIX  43
H1AA  2    0.327665    0.562476    0.910995    11.00000   -1.20000
AFIX   0

C1B   1    0.130188    0.540962    0.873818    11.00000    0.06364    0.02496 =
         0.04651    0.00305    0.00998   -0.00484
AFIX  43
H1BA  2    0.172088    0.561996    0.909305    11.00000   -1.20000
AFIX   0

N3A   4    0.454915    0.413195    0.803745    11.00000    0.06557    0.02350 =
         0.07079   -0.00051   -0.03246    0.00197
N3B   4    0.044442    0.413191    0.802843    11.00000    0.05812    0.02460 =
         0.07052   -0.00111    0.02544   -0.00181
C2A   1    0.465730    0.567445    0.787345    11.00000    0.05772    0.02811 =
         0.07272    0.00104   -0.02311    0.00002
AFIX  43
H2AA  2    0.504047    0.614616    0.750195    11.00000   -1.20000
AFIX   0

C2B   1    0.034212    0.567929    0.785893    11.00000    0.05808    0.02597 =
         0.06587    0.00093    0.02168   -0.00170
AFIX  43
H2BA  2   -0.003973    0.615479    0.747631    11.00000   -1.20000
AFIX   0
HKLF 4




REM  triag2pbcl4_05_100_00c_a.res in P2(1)/c
REM wR2 = 0.1297, GooF = S = 1.239, Restrained GooF = 1.285 for all data
REM R1 = 0.0641 for 2544 Fo > 4sig(Fo) and 0.0784 for all 3071 data
REM 137 parameters refined using 151 restraints

END

WGHT      0.0271     28.7616

REM Highest difference peak  1.901,  deepest hole -5.705,  1-sigma level  0.235
Q1    1   0.2736  0.5342  0.3537  11.00000  0.05    1.90
Q2    1   0.2265  0.5333  0.3802  11.00000  0.05    1.85
Q3    1   0.2519  0.6142  0.3642  11.00000  0.05    1.64
Q4    1   0.1716  0.5226  0.3633  11.00000  0.05    1.41
Q5    1   0.2500  0.3790  0.3740  11.00000  0.05    1.36
;
_shelx_res_checksum              65775
_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
;
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_triag2pbcl4_03_200_00
_database_code_depnum_ccdc_archive 'CCDC 2314658'
loop_
_audit_author_name
_audit_author_address
'Szymon Sobczak'
;Department of Materials Chemistry, Adam Mickiewicz University
Poland
;
_audit_update_record             
;
2024-03-04 deposited with the CCDC.	2024-03-21 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT972_triag2pbcl4_03_200_00 
;
PROBLEM: Check Calcd Resid. Dens.  0.98Ang From Pb1            -3.52 eA-3
RESPONSE: Residual density near heavy atom.
;
_vrf_PLAT112_triag2pbcl4_03_200_00 
;
PROBLEM: ADDSYM Detects New (Pseudo) Symm. Elem         n        100 %Fit
RESPONSE: The symmetry has been thoroughly inspected by the presence of systematic absences in the raw diffraction data
;
_vrf_PLAT113_triag2pbcl4_03_200_00 
;
PROBLEM: ADDSYM Suggests Possible Pseudo/New  Space Group       Pnma Check
RESPONSE: The symmetry has been thoroughly inspected by the presence of systematic absences in the raw diffraction data
;
_vrf_PLAT972_triag2pbcl4_03_200_00_2 
;
PROBLEM: Check Calcd Resid. Dens.  0.98Ang From Pb1            -3.39 eA-3
RESPONSE: Residual density near heavy atom.
;
# Added during the CSD deposition process: Friday 15 December 2023 12:43 PM
# end Validation Reply Form

_audit_creation_date             2023-12-15
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        Tz2PbCl4
_chemical_formula_moiety         'Cl4 Pb, 2(C2 H4 N3)'
_chemical_formula_sum            'C4 H8 Cl4 N6 Pb'
_chemical_formula_weight         489.15
_chemical_melting_point          ?
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'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
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'

_cell_length_a                   21.4424(18)
_cell_length_b                   8.2994(3)
_cell_length_c                   7.4252(4)
_cell_angle_alpha                90
_cell_angle_beta                 90.093(5)
_cell_angle_gamma                90
_cell_volume                     1321.38(14)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    5584
_cell_measurement_temperature    199.99(10)
_cell_measurement_theta_max      28.5760
_cell_measurement_theta_min      2.5240
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    13.556
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.16005
_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_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.459
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             896
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

_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0407
_diffrn_reflns_av_unetI/netI     0.0327
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.902
_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            14455
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.902
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         28.920
_diffrn_reflns_theta_min         2.632
_diffrn_ambient_temperature      200.15
_diffrn_detector_area_resol_mean 8.0772
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.902
_diffrn_measurement_details      .
_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_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2470
_reflns_number_total             3145
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_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)'
_refine_diff_density_max         1.632
_refine_diff_density_min         -3.104
_refine_diff_density_rms         0.193
_refine_ls_extinction_coef       0.0112(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   1.155
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     145
_refine_ls_number_reflns         3127
_refine_ls_number_restraints     61
_refine_ls_R_factor_all          0.0576
_refine_ls_R_factor_gt           0.0419
_refine_ls_restrained_S_all      1.152
_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)+(0.0359P)²+5.1929P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0903
_refine_ls_wR_factor_ref         0.0980
_refine_special_details          ?
_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.a Aromatic/amide H refined with riding coordinates:
 N1B(H1B), N1A(H1A), C1A(H1AA), C1B(H1BA), C2A(H2AA), C2B(H2BA)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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 0.25001(2) 0.49423(2) 0.36234(3) 0.03693(16) Uani 1 1 d . . . . .
Cl1 Cl 0.24984(13) 0.7636(2) 0.1371(2) 0.0584(6) Uani 1 1 d . . . . .
Cl2 Cl 0.25006(14) 0.1898(2) 0.5453(3) 0.0629(7) Uani 1 1 d . . . . .
Cl4 Cl 0.38293(13) 0.4877(2) 0.3583(4) 0.0598(6) Uani 1 1 d . . . . .
Cl3 Cl 0.11704(13) 0.4876(2) 0.3581(4) 0.0598(6) Uani 1 1 d . . . . .
N2A N 0.3959(4) 0.3925(8) 0.8521(10) 0.0526(19) Uani 1 1 d D . . . .
N1B N 0.0891(4) 0.6429(8) 0.8291(10) 0.0553(18) Uani 1 1 d D . . . .
H1B H 0.094184 0.748127 0.831885 0.066 Uiso 1 1 calc R U . . .
N1A N 0.4110(4) 0.6413(8) 0.8289(10) 0.057(2) Uani 1 1 d D . . . .
H1A H 0.405762 0.746504 0.831098 0.069 Uiso 1 1 calc R U . . .
N2B N 0.1043(4) 0.3936(8) 0.8522(11) 0.0536(18) Uani 1 1 d D . . . .
C1A C 0.3681(5) 0.5321(10) 0.8693(14) 0.057(2) Uani 1 1 d D . . . .
H1AA H 0.326049 0.551088 0.903513 0.068 Uiso 1 1 calc R U . . .
C1B C 0.1315(5) 0.5324(10) 0.8674(14) 0.059(2) Uani 1 1 d D . . . .
H1BA H 0.173805 0.551120 0.899725 0.070 Uiso 1 1 calc R U . . .
N3A N 0.4559(4) 0.4090(8) 0.8001(13) 0.065(2) Uani 1 1 d D . . . .
N3B N 0.0442(4) 0.4083(8) 0.7998(12) 0.061(2) Uani 1 1 d D . . . .
C2A C 0.4640(4) 0.5635(9) 0.7838(15) 0.062(3) Uani 1 1 d D . . . .
H2AA H 0.501510 0.613953 0.745926 0.075 Uiso 1 1 calc R U . . .
C2B C 0.0368(4) 0.5630(9) 0.7851(14) 0.061(2) Uani 1 1 d D . . . .
H2BA H -0.000931 0.613347 0.747938 0.074 Uiso 1 1 calc R U . . .
H2B H 0.119(4) 0.289(10) 0.863(10) 0.05(2) Uiso 1 1 d . . . . .
H2A H 0.381(4) 0.284(12) 0.865(12) 0.07(3) Uiso 1 1 d . . . . .

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 0.0830(3) 0.01322(16) 0.01457(17) -0.00035(8) 0.00046(13) 0.00005(12)
Cl1 0.125(2) 0.0263(9) 0.0237(9) 0.0103(7) 0.0002(10) -0.0004(10)
Cl2 0.124(2) 0.0299(9) 0.0344(11) 0.0166(8) 0.0018(11) 0.0022(11)
Cl4 0.0787(16) 0.0182(9) 0.0823(19) 0.0008(8) -0.0084(13) -0.0029(8)
Cl3 0.0800(16) 0.0188(9) 0.0807(18) 0.0011(8) 0.0115(13) 0.0019(9)
N2A 0.069(5) 0.025(3) 0.064(5) 0.008(3) -0.011(4) -0.002(3)
N1B 0.082(5) 0.023(3) 0.062(5) 0.004(3) 0.018(4) -0.004(3)
N1A 0.090(6) 0.020(3) 0.062(5) 0.003(3) -0.017(4) 0.002(4)
N2B 0.070(4) 0.022(3) 0.069(5) 0.004(3) 0.012(3) -0.001(3)
C1A 0.080(7) 0.035(4) 0.055(6) 0.005(4) 0.004(5) 0.014(4)
C1B 0.081(5) 0.035(4) 0.060(6) 0.005(3) 0.007(4) -0.009(3)
N3A 0.062(5) 0.024(4) 0.110(7) 0.002(4) -0.031(5) 0.003(3)
N3B 0.064(4) 0.027(3) 0.091(6) 0.001(3) 0.022(4) -0.003(3)
C2A 0.056(6) 0.027(4) 0.104(8) 0.003(4) -0.033(5) 0.000(4)
C2B 0.066(5) 0.026(4) 0.091(7) 0.003(3) 0.023(4) -0.001(3)

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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 2.7919(16) . ?
Pb1 Cl1 2.8639(16) 4_576 ?
Pb1 Cl2 2.8064(18) 4_565 ?
Pb1 Cl2 2.8684(17) . ?
Pb1 Cl4 2.851(3) . ?
Pb1 Cl3 2.852(3) . ?
N2A C1A 1.310(10) . ?
N2A N3A 1.350(10) . ?
N2A H2A 0.96(10) . ?
N1B H1B 0.8800 . ?
N1B C1B 1.322(11) . ?
N1B C2B 1.344(11) . ?
N1A H1A 0.8800 . ?
N1A C1A 1.326(11) . ?
N1A C2A 1.351(11) . ?
N2B C1B 1.296(10) . ?
N2B N3B 1.351(10) . ?
N2B H2B 0.93(8) . ?
C1A H1AA 0.9500 . ?
C1B H1BA 0.9500 . ?
N3A C2A 1.300(10) . ?
N3B C2B 1.299(10) . ?
C2A H2AA 0.9500 . ?
C2B H2BA 0.9500 . ?

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 82.229(8) . 4_576 ?
Cl1 Pb1 Cl2 86.18(5) . 4_565 ?
Cl1 Pb1 Cl2 171.47(5) . . ?
Cl1 Pb1 Cl2 106.31(5) 4_576 . ?
Cl1 Pb1 Cl4 90.53(7) . . ?
Cl1 Pb1 Cl3 90.49(7) . . ?
Cl2 Pb1 Cl1 168.41(5) 4_565 4_576 ?
Cl2 Pb1 Cl2 85.288(18) 4_565 . ?
Cl2 Pb1 Cl4 88.79(8) 4_565 . ?
Cl2 Pb1 Cl3 88.97(8) 4_565 . ?
Cl4 Pb1 Cl1 91.34(7) . 4_576 ?
Cl4 Pb1 Cl2 89.34(7) . . ?
Cl4 Pb1 Cl3 177.48(6) . . ?
Cl3 Pb1 Cl1 91.09(7) . 4_576 ?
Cl3 Pb1 Cl2 89.31(7) . . ?
Pb1 Cl1 Pb1 171.37(8) . 4_575 ?
Pb1 Cl2 Pb1 151.25(8) 4_566 . ?
C1A N2A N3A 111.9(7) . . ?
C1A N2A H2A 132(6) . . ?
N3A N2A H2A 116(6) . . ?
C1B N1B H1B 126.7 . . ?
C1B N1B C2B 106.5(7) . . ?
C2B N1B H1B 126.7 . . ?
C1A N1A H1A 125.9 . . ?
C1A N1A C2A 108.3(7) . . ?
C2A N1A H1A 125.9 . . ?
C1B N2B N3B 112.0(7) . . ?
C1B N2B H2B 132(5) . . ?
N3B N2B H2B 116(5) . . ?
N2A C1A N1A 105.5(9) . . ?
N2A C1A H1AA 127.3 . . ?
N1A C1A H1AA 127.3 . . ?
N1B C1B H1BA 126.6 . . ?
N2B C1B N1B 106.7(9) . . ?
N2B C1B H1BA 126.6 . . ?
C2A N3A N2A 104.7(7) . . ?
C2B N3B N2B 103.4(7) . . ?
N1A C2A H2AA 125.2 . . ?
N3A C2A N1A 109.7(8) . . ?
N3A C2A H2AA 125.2 . . ?
N1B C2B H2BA 124.3 . . ?
N3B C2B N1B 111.4(8) . . ?
N3B C2B H2BA 124.3 . . ?

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 1.5(10) . . . . ?
N2B N3B C2B N1B -1.1(9) . . . . ?
C1A N2A N3A C2A -0.7(10) . . . . ?
C1A N1A C2A N3A -1.9(11) . . . . ?
C1B N1B C2B N3B 2.0(11) . . . . ?
C1B N2B N3B C2B -0.3(10) . . . . ?
N3A N2A C1A N1A -0.4(11) . . . . ?
N3B N2B C1B N1B 1.5(11) . . . . ?
C2A N1A C1A N2A 1.4(11) . . . . ?
C2B N1B C1B N2B -2.1(11) . . . . ?

_shelx_res_file                  
;
TITL triag2pbcl4_03_200_00_a.res in P2(1)/c
    triag2pbcl4_03_200_00.res
    created by SHELXL-2019/2 at 17:16:50 on 01-Mar-2024
REM Old TITL TRIAG2PbCl4_03_200_00 in P2(1)/c
REM SHELXT solution in P2(1)/c: R1 0.294, Rweak 0.070, Alpha 0.027
REM <I/s> 0.934 for 202 systematic absences, Orientation as input
REM Formula found by SHELXT: C9 N2 Cl4 Pb
CELL 0.71073 21.4424 8.2994 7.4252 90 90.093 90
ZERR 4 0.0018 0.0003 0.0004 0 0.005 0
LATT 1
SYMM -X,0.5+Y,0.5-Z
SFAC C H Cl N Pb
UNIT 16 32 16 24 4
RIGU Cl2 Pb1 Cl1 Cl4 Cl3
RIGU N3B N2B C1B C2B N1B
RIGU N2B C1B N1B N3B C2B
SADI N3A N2A N3B N2B
SADI N3B C2B N3A C2A
SADI N2A C1A N2B C1B
SADI N1B C1B N1A C1A
SADI N1B C2B N1A C2A

L.S. 50 0 0
PLAN  5
TEMP -73
CONF
list 4
MORE -1
BOND $H
fmap 2 53
acta 50
OMIT -4 0 2
OMIT 0 2 0
OMIT 0 4 0
OMIT 1 2 0
OMIT 3 0 0
OMIT 3 1 0
OMIT 3 2 0
OMIT 3 4 0
OMIT 4 0 0
OMIT 4 1 0
OMIT 4 3 0
OMIT 5 1 0
OMIT 5 2 0
OMIT 8 0 0
OMIT 22 1 2
OMIT 23 3 0
OMIT 24 0 0
OMIT 24 2 1
REM <olex2.extras>
REM <HklSrc "%.\\triag2pbcl4_03_200_00.hkl">
REM </olex2.extras>

WGHT    0.035900    5.192900
EXTI    0.011159
FVAR       0.29907
PB1   5    0.250006    0.494231    0.362341    11.00000    0.08301    0.01322 =
         0.01457   -0.00035    0.00046    0.00005
CL1   3    0.249843    0.763592    0.137096    11.00000    0.12507    0.02634 =
         0.02375    0.01034    0.00023   -0.00043
CL2   3    0.250064    0.189835    0.545287    11.00000    0.12434    0.02985 =
         0.03437    0.01663    0.00178    0.00222
CL4   3    0.382932    0.487668    0.358264    11.00000    0.07872    0.01823 =
         0.08230    0.00079   -0.00845   -0.00295
CL3   3    0.117037    0.487617    0.358094    11.00000    0.07998    0.01882 =
         0.08069    0.00110    0.01152    0.00187
N2A   4    0.395922    0.392516    0.852075    11.00000    0.06882    0.02512 =
         0.06388    0.00796   -0.01056   -0.00242
N1B   4    0.089119    0.642935    0.829090    11.00000    0.08165    0.02285 =
         0.06159    0.00375    0.01822   -0.00363
AFIX  43
H1B   2    0.094184    0.748127    0.831885    11.00000   -1.20000
AFIX   0

N1A   4    0.410963    0.641345    0.828901    11.00000    0.08991    0.02007 =
         0.06212    0.00308   -0.01673    0.00187
AFIX  43
H1A   2    0.405762    0.746504    0.831098    11.00000   -1.20000
AFIX   0

N2B   4    0.104298    0.393607    0.852203    11.00000    0.06954    0.02240 =
         0.06892    0.00412    0.01245   -0.00101
C1A   1    0.368084    0.532104    0.869300    11.00000    0.07993    0.03462 =
         0.05507    0.00537    0.00439    0.01424
AFIX  43
H1AA  2    0.326049    0.551088    0.903513    11.00000   -1.20000
AFIX   0

C1B   1    0.131538    0.532418    0.867367    11.00000    0.08073    0.03523 =
         0.05962    0.00536    0.00670   -0.00908
AFIX  43
H1BA  2    0.173805    0.551120    0.899725    11.00000   -1.20000
AFIX   0

N3A   4    0.455898    0.408959    0.800081    11.00000    0.06155    0.02376 =
         0.10988    0.00169   -0.03063    0.00310
N3B   4    0.044215    0.408318    0.799791    11.00000    0.06408    0.02651 =
         0.09129    0.00054    0.02228   -0.00282
C2A   1    0.463994    0.563468    0.783798    11.00000    0.05644    0.02664 =
         0.10383    0.00294   -0.03257    0.00014
AFIX  43
H2AA  2    0.501510    0.613953    0.745926    11.00000   -1.20000
AFIX   0

C2B   1    0.036750    0.563040    0.785080    11.00000    0.06597    0.02649 =
         0.09141    0.00269    0.02304   -0.00071
AFIX  43
H2BA  2   -0.000931    0.613347    0.747938    11.00000   -1.20000
AFIX   0
H2B   2    0.119408    0.289084    0.862659    11.00000    0.04793

H2A   2    0.381075    0.284289    0.864971    11.00000    0.07043
HKLF 4




REM  triag2pbcl4_03_200_00_a.res in P2(1)/c
REM wR2 = 0.0980, GooF = S = 1.155, Restrained GooF = 1.152 for all data
REM R1 = 0.0419 for 2452 Fo > 4sig(Fo) and 0.0576 for all 3127 data
REM 145 parameters refined using 61 restraints

END

WGHT      0.0359      5.2334

REM Highest difference peak  1.632,  deepest hole -3.104,  1-sigma level  0.193
Q1    1   0.2768  0.5767  0.3466  11.00000  0.05    1.63
Q2    1   0.2579  0.6041  0.3564  11.00000  0.05    1.59
Q3    1   0.2239  0.5766  0.3800  11.00000  0.05    1.53
Q4    1   0.2562  0.3836  0.3595  11.00000  0.05    1.45
Q5    1   0.2286  0.4054  0.3792  11.00000  0.05    1.39
;
_shelx_res_checksum              95862
_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
;
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_triag2pbcl4_iv_150_00
_database_code_depnum_ccdc_archive 'CCDC 2314656'
loop_
_audit_author_name
_audit_author_address
'Szymon Sobczak'
;Department of Materials Chemistry, Adam Mickiewicz University
Poland
;
_audit_update_record             
;
2024-03-04 deposited with the CCDC.	2024-03-21 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT972_triag2pbcl4_iv_150_00 
;
PROBLEM: Check Calcd Resid. Dens.  1.01Ang From Pb1            -5.23 eA-3
RESPONSE: Residual density near heavy atom.
;
_vrf_PLAT112_triag2pbcl4_iv_150_00 
;
PROBLEM: ADDSYM Detects New (Pseudo) Symm. Elem         n        100 %Fit
RESPONSE: The symmetry has been thoroughly inspected by the presence of the systematic absences in the raw diffraction data
;
_vrf_PLAT113_triag2pbcl4_iv_150_00 
;
PROBLEM: ADDSYM Suggests Possible Pseudo/New  Space Group       Pnma Check
RESPONSE: look PLAT112
;
# Added during the CSD deposition process: Friday 15 December 2023 12:43 PM
# end Validation Reply Form

_audit_creation_date             2023-12-15
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        Tz2PbCl4
_chemical_formula_moiety         'Cl4 Pb, 2(C2 H4 N3)'
_chemical_formula_sum            'C4 H8 Cl4 N6 Pb'
_chemical_formula_weight         489.15
_chemical_melting_point          ?
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'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
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'

_cell_length_a                   21.429(2)
_cell_length_b                   8.3075(4)
_cell_length_c                   7.3768(4)
_cell_angle_alpha                90
_cell_angle_beta                 90.111(6)
_cell_angle_gamma                90
_cell_volume                     1313.21(17)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    5663
_cell_measurement_temperature    149.95(10)
_cell_measurement_theta_max      28.4290
_cell_measurement_theta_min      3.6620
_shelx_estimated_absorpt_T_max   0.291
_shelx_estimated_absorpt_T_min   0.049
_exptl_absorpt_coefficient_mu    13.640
_exptl_absorpt_correction_T_max  0.777
_exptl_absorpt_correction_T_min  0.493
_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_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.474
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             896
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

_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0379
_diffrn_reflns_av_unetI/netI     0.0317
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.892
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            14206
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.892
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         28.984
_diffrn_reflns_theta_min         2.630
_diffrn_ambient_temperature      150.15
_diffrn_detector_area_resol_mean 8.0772
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.892
_diffrn_measurement_details      .
_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_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2518
_reflns_number_total             3100
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_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)'
_refine_diff_density_max         1.522
_refine_diff_density_min         -5.245
_refine_diff_density_rms         0.233
_refine_ls_extinction_coef       0.0065(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   1.231
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     137
_refine_ls_number_reflns         3100
_refine_ls_number_restraints     151
_refine_ls_R_factor_all          0.0713
_refine_ls_R_factor_gt           0.0561
_refine_ls_restrained_S_all      1.270
_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)+(0.0340P)²+19.0164P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1165
_refine_ls_wR_factor_ref         0.1259
_refine_special_details          ?
_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. Uiso/Uaniso restraints and constraints
Uanis(Cl2) \\sim Ueq, Uanis(Pb1) \\sim Ueq, Uanis(Cl1) \\sim Ueq, Uanis(Cl4)
\\sim Ueq, Uanis(Cl3) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(N3A) \\sim Ueq, Uanis(N2A) \\sim Ueq, Uanis(C1A) \\sim Ueq, Uanis(C2A)
\\sim Ueq, Uanis(N1A) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(N2B) \\sim Ueq, Uanis(C1B) \\sim Ueq, Uanis(N1B) \\sim Ueq, Uanis(N3B)
\\sim Ueq, Uanis(C2B) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
4. 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
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)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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 0.25000(2) 0.49268(4) 0.36465(4) 0.0388(2) Uani 1 1 d . U . . .
Cl1 Cl 0.2499(2) 0.7642(3) 0.1410(3) 0.0557(9) Uani 1 1 d . U . . .
Cl2 Cl 0.2498(2) 0.1840(3) 0.5404(4) 0.0577(9) Uani 1 1 d . U . . .
Cl4 Cl 0.38277(19) 0.4844(3) 0.3614(5) 0.0590(9) Uani 1 1 d . U . . .
Cl3 Cl 0.11728(19) 0.4845(3) 0.3617(5) 0.0590(9) Uani 1 1 d . U . . .
N2A N 0.3954(5) 0.3969(11) 0.8554(14) 0.048(2) Uani 1 1 d D U . . .
H2A H 0.376464 0.304801 0.876103 0.057 Uiso 1 1 calc R U . . .
N1B N 0.0882(5) 0.6466(11) 0.8314(14) 0.050(2) Uani 1 1 d D U . . .
H1B H 0.092944 0.751741 0.834260 0.059 Uiso 1 1 calc R U . . .
N1A N 0.4123(5) 0.6459(11) 0.8312(14) 0.051(3) Uani 1 1 d D U . . .
H1A H 0.407386 0.751028 0.832314 0.062 Uiso 1 1 calc R U . . .
N2B N 0.1043(5) 0.3972(11) 0.8554(14) 0.048(2) Uani 1 1 d D U . . .
H2B H 0.123119 0.304867 0.876307 0.058 Uiso 1 1 calc R U . . .
C1A C 0.3690(7) 0.5377(14) 0.8727(18) 0.051(3) Uani 1 1 d D U . . .
H1AA H 0.327157 0.558550 0.907997 0.062 Uiso 1 1 calc R U . . .
C1B C 0.1313(7) 0.5379(14) 0.8719(19) 0.053(3) Uani 1 1 d D U . . .
H1BA H 0.173365 0.558099 0.905980 0.064 Uiso 1 1 calc R U . . .
N3A N 0.4553(5) 0.4101(11) 0.8020(17) 0.058(3) Uani 1 1 d D U . . .
N3B N 0.0446(5) 0.4110(11) 0.8028(16) 0.054(2) Uani 1 1 d D U . . .
C2A C 0.4654(6) 0.5658(13) 0.787(2) 0.055(3) Uani 1 1 d D U . . .
H2AA H 0.503555 0.614208 0.750309 0.066 Uiso 1 1 calc R U . . .
C2B C 0.0353(7) 0.5663(13) 0.785(2) 0.057(3) Uani 1 1 d D U . . .
H2BA H -0.002463 0.614976 0.745456 0.068 Uiso 1 1 calc R U . . .

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 0.0953(4) 0.0101(2) 0.0109(2) -0.00022(11) 0.00042(17) -0.00012(18)
Cl1 0.129(3) 0.0205(11) 0.0173(11) 0.0061(8) 0.0004(14) 0.0008(14)
Cl2 0.124(3) 0.0232(12) 0.0260(13) 0.0120(9) 0.0010(15) 0.0002(15)
Cl4 0.089(2) 0.0140(11) 0.074(2) 0.0007(11) -0.0134(18) -0.0037(13)
Cl3 0.089(2) 0.0143(12) 0.074(2) 0.0012(11) 0.0154(18) 0.0032(13)
N2A 0.059(6) 0.026(4) 0.058(5) 0.003(4) -0.008(4) 0.002(4)
N1B 0.070(5) 0.025(4) 0.053(5) 0.002(3) 0.017(4) -0.005(3)
N1A 0.075(6) 0.023(4) 0.056(5) 0.000(4) -0.016(5) 0.000(4)
N2B 0.059(5) 0.028(4) 0.058(5) 0.002(3) 0.018(4) -0.002(3)
C1A 0.069(7) 0.035(5) 0.051(6) -0.001(5) -0.002(5) 0.009(5)
C1B 0.072(5) 0.033(4) 0.055(6) 0.005(4) 0.008(4) -0.007(4)
N3A 0.072(7) 0.026(4) 0.077(6) -0.001(4) -0.027(5) 0.002(5)
N3B 0.061(5) 0.028(4) 0.073(6) -0.002(4) 0.024(4) -0.002(3)
C2A 0.057(7) 0.032(5) 0.076(7) 0.003(5) -0.019(6) 0.000(5)
C2B 0.066(5) 0.030(4) 0.075(7) 0.000(4) 0.016(4) -0.002(4)

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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 2.794(2) . ?
Pb1 Cl1 2.870(2) 4_576 ?
Pb1 Cl2 2.806(2) 4_565 ?
Pb1 Cl2 2.873(2) . ?
Pb1 Cl4 2.846(4) . ?
Pb1 Cl3 2.845(4) . ?
N2A H2A 0.8800 . ?
N2A C1A 1.306(13) . ?
N2A N3A 1.347(14) . ?
N1B H1B 0.8800 . ?
N1B C1B 1.325(15) . ?
N1B C2B 1.358(15) . ?
N1A H1A 0.8800 . ?
N1A C1A 1.327(15) . ?
N1A C2A 1.360(15) . ?
N2B H2B 0.8800 . ?
N2B C1B 1.309(13) . ?
N2B N3B 1.342(13) . ?
C1A H1AA 0.9500 . ?
C1B H1BA 0.9500 . ?
N3A C2A 1.316(14) . ?
N3B C2B 1.312(14) . ?
C2A H2AA 0.9500 . ?
C2B H2BA 0.9500 . ?

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 81.448(12) . 4_576 ?
Cl1 Pb1 Cl2 170.64(8) . . ?
Cl1 Pb1 Cl2 85.36(8) . 4_565 ?
Cl1 Pb1 Cl2 107.91(8) 4_576 . ?
Cl1 Pb1 Cl4 90.82(11) . . ?
Cl1 Pb1 Cl3 90.86(11) . . ?
Cl2 Pb1 Cl1 166.80(8) 4_565 4_576 ?
Cl2 Pb1 Cl2 85.29(3) 4_565 . ?
Cl2 Pb1 Cl4 88.85(12) 4_565 . ?
Cl2 Pb1 Cl3 88.91(12) 4_565 . ?
Cl4 Pb1 Cl1 91.46(11) . 4_576 ?
Cl4 Pb1 Cl2 89.11(11) . . ?
Cl3 Pb1 Cl1 91.15(11) . 4_576 ?
Cl3 Pb1 Cl2 88.84(11) . . ?
Cl3 Pb1 Cl4 177.08(8) . . ?
Pb1 Cl1 Pb1 170.92(10) . 4_575 ?
Pb1 Cl2 Pb1 148.37(11) 4_566 . ?
C1A N2A H2A 124.2 . . ?
C1A N2A N3A 111.7(10) . . ?
N3A N2A H2A 124.2 . . ?
C1B N1B H1B 126.2 . . ?
C1B N1B C2B 107.7(10) . . ?
C2B N1B H1B 126.2 . . ?
C1A N1A H1A 126.0 . . ?
C1A N1A C2A 108.1(10) . . ?
C2A N1A H1A 126.0 . . ?
C1B N2B H2B 124.1 . . ?
C1B N2B N3B 111.8(10) . . ?
N3B N2B H2B 124.1 . . ?
N2A C1A N1A 106.3(12) . . ?
N2A C1A H1AA 126.9 . . ?
N1A C1A H1AA 126.9 . . ?
N1B C1B H1BA 126.9 . . ?
N2B C1B N1B 106.2(12) . . ?
N2B C1B H1BA 126.9 . . ?
C2A N3A N2A 105.2(10) . . ?
C2B N3B N2B 104.9(10) . . ?
N1A C2A H2AA 125.6 . . ?
N3A C2A N1A 108.7(12) . . ?
N3A C2A H2AA 125.6 . . ?
N1B C2B H2BA 125.3 . . ?
N3B C2B N1B 109.3(12) . . ?
N3B C2B H2BA 125.3 . . ?

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 0.3(14) . . . . ?
N2B N3B C2B N1B -1.9(14) . . . . ?
C1A N2A N3A C2A 0.1(14) . . . . ?
C1A N1A C2A N3A -0.6(15) . . . . ?
C1B N1B C2B N3B 2.4(15) . . . . ?
C1B N2B N3B C2B 0.7(14) . . . . ?
N3A N2A C1A N1A -0.4(15) . . . . ?
N3B N2B C1B N1B 0.8(14) . . . . ?
C2A N1A C1A N2A 0.6(15) . . . . ?
C2B N1B C1B N2B -1.9(15) . . . . ?

_shelx_res_file                  
;
TITL triag2pbcl4_04_150_00_a.res in P2(1)/c
    triag2pbcl4_iv_150_00.res
    created by SHELXL-2019/2 at 16:51:39 on 01-Mar-2024
REM Old TITL TRIAG2PbCl4_04_150_00 in P2(1)/c
REM SHELXT solution in P2(1)/c: R1 0.362, Rweak 0.145, Alpha 0.027
REM <I/s> 1.180 for 198 systematic absences, Orientation as input
REM Formula found by SHELXT: C7 N3 Cl4 Pb
CELL 0.71073 21.4288 8.3075 7.3768 90 90.111 90
ZERR 4 0.0022 0.0004 0.0004 0 0.006 0
LATT 1
SYMM -X,0.5+Y,0.5-Z
SFAC C H Cl N Pb
UNIT 16 32 16 24 4
ISOR 0.01 0.02 Cl2 Pb1 Cl1 Cl4 Cl3
RIGU Cl2 Pb1 Cl1 Cl4 Cl3
RIGU N3B N2B C1B C2B N1B
ISOR 0.01 0.02 N3A N2A C1A C2A N1A
RIGU N2B C1B N1B N3B C2B
ISOR 0.01 0.02 N2B C1B N1B N3B C2B
SADI N3A N2A N3B N2B
SADI N3B C2B N3A C2A
SADI N2A C1A N2B C1B
SADI N1B C1B N1A C1A
SADI N1B C2B N1A C2A

L.S. 44
PLAN  5
SIZE 0.12 0.16 0.50
TEMP -123
CONF
list 4
MORE -1
BOND $H
fmap 2 53
acta 50
OMIT -24 2 1
OMIT -24 5 2
OMIT -22 2 3
OMIT 0 2 0
OMIT 0 4 0
OMIT 1 2 0
OMIT 4 1 0
OMIT 5 0 0
OMIT 8 0 0
OMIT 22 0 0
OMIT 22 1 2
OMIT 23 3 0
OMIT 23 5 2
OMIT 24 2 1
OMIT 25 3 0
REM <olex2.extras>
REM <HklSrc "%.\\triag2pbcl4_iv_150_00.hkl">
REM </olex2.extras>

WGHT    0.034000   19.016401
EXTI    0.006459
FVAR       0.29459
PB1   5    0.250000    0.492682    0.364652    11.00000    0.09531    0.01009 =
         0.01095   -0.00022    0.00042   -0.00012
CL1   3    0.249878    0.764151    0.141021    11.00000    0.12917    0.02051 =
         0.01730    0.00613    0.00042    0.00077
CL2   3    0.249813    0.184026    0.540444    11.00000    0.12405    0.02317 =
         0.02599    0.01196    0.00096    0.00024
CL4   3    0.382767    0.484368    0.361373    11.00000    0.08889    0.01403 =
         0.07415    0.00066   -0.01341   -0.00369
CL3   3    0.117276    0.484459    0.361671    11.00000    0.08869    0.01430 =
         0.07397    0.00122    0.01545    0.00323
N2A   4    0.395421    0.396935    0.855409    11.00000    0.05891    0.02602 =
         0.05757    0.00297   -0.00823    0.00166
AFIX  43
H2A   2    0.376464    0.304801    0.876103    11.00000   -1.20000
AFIX   0

N1B   4    0.088184    0.646556    0.831440    11.00000    0.07020    0.02531 =
         0.05323    0.00154    0.01673   -0.00456
AFIX  43
H1B   2    0.092944    0.751741    0.834260    11.00000   -1.20000
AFIX   0

N1A   4    0.412251    0.645851    0.831187    11.00000    0.07465    0.02279 =
         0.05629    0.00011   -0.01610   -0.00038
AFIX  43
H1A   2    0.407386    0.751028    0.832314    11.00000   -1.20000
AFIX   0

N2B   4    0.104341    0.397247    0.855414    11.00000    0.05948    0.02755 =
         0.05848    0.00213    0.01780   -0.00197
AFIX  43
H2B   2    0.123119    0.304867    0.876307    11.00000   -1.20000
AFIX   0

C1A   1    0.368997    0.537703    0.872716    11.00000    0.06854    0.03492 =
         0.05094   -0.00055   -0.00214    0.00938
AFIX  43
H1AA  2    0.327157    0.558550    0.907997    11.00000   -1.20000
AFIX   0

C1B   1    0.131312    0.537934    0.871881    11.00000    0.07191    0.03291 =
         0.05543    0.00471    0.00804   -0.00668
AFIX  43
H1BA  2    0.173365    0.558099    0.905980    11.00000   -1.20000
AFIX   0

N3A   4    0.455266    0.410119    0.801984    11.00000    0.07189    0.02632 =
         0.07670   -0.00078   -0.02655    0.00234
N3B   4    0.044610    0.411002    0.802831    11.00000    0.06119    0.02847 =
         0.07297   -0.00156    0.02408   -0.00193
C2A   1    0.465408    0.565787    0.786585    11.00000    0.05750    0.03206 =
         0.07586    0.00260   -0.01940   -0.00016
AFIX  43
H2AA  2    0.503555    0.614208    0.750309    11.00000   -1.20000
AFIX   0

C2B   1    0.035318    0.566307    0.784863    11.00000    0.06632    0.02977 =
         0.07452    0.00037    0.01604   -0.00170
AFIX  43
H2BA  2   -0.002463    0.614976    0.745456    11.00000   -1.20000
AFIX   0
HKLF 4




REM  triag2pbcl4_04_150_00_a.res in P2(1)/c
REM wR2 = 0.1259, GooF = S = 1.231, Restrained GooF = 1.270 for all data
REM R1 = 0.0561 for 2518 Fo > 4sig(Fo) and 0.0713 for all 3100 data
REM 137 parameters refined using 151 restraints

END

WGHT      0.0336     18.9071

REM Highest difference peak  1.522,  deepest hole -5.245,  1-sigma level  0.233
Q1    1   0.2787  0.5622  0.3404  11.00000  0.05    1.52
Q2    1   0.2220  0.5658  0.3870  11.00000  0.05    1.47
Q3    1   0.2517  0.6118  0.3570  11.00000  0.05    1.36
Q4    1   0.1764  0.5396  0.3625  11.00000  0.05    1.26
Q5    1   0.2460  0.3760  0.3869  11.00000  0.05    1.24
;
_shelx_res_checksum              64244
_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
;
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_triag2pbcl4_iv_130_00
_database_code_depnum_ccdc_archive 'CCDC 2314655'
loop_
_audit_author_name
_audit_author_address
'Szymon Sobczak'
;Department of Materials Chemistry, Adam Mickiewicz University
Poland
;
_audit_update_record             
;
2024-03-04 deposited with the CCDC.	2024-03-21 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT972_triag2pbcl4_iv_130_00 
;
PROBLEM: Check Calcd Resid. Dens.  1.03Ang From Pb1            -5.28 eA-3
RESPONSE: Residual density near heavy atom.
;
_vrf_PLAT112_triag2pbcl4_iv_130_00 
;
PROBLEM: ADDSYM Detects New (Pseudo) Symm. Elem         n        100 %Fit
RESPONSE: The symmetry has been thoroughly inspected by the presence of the systematic absences in the raw diffraction data
;
_vrf_PLAT113_triag2pbcl4_iv_130_00 
;
PROBLEM: ADDSYM Suggests Possible Pseudo/New  Space Group       Pnma Check
RESPONSE: look PLAT112
;
# Added during the CSD deposition process: Friday 15 December 2023 12:43 PM
# end Validation Reply Form

_audit_creation_date             2023-12-15
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        Tz2PbCl4
_chemical_formula_moiety         'Cl4 Pb, 2(C2 H4 N3)'
_chemical_formula_sum            'C4 H8 Cl4 N6 Pb'
_chemical_formula_weight         489.15
_chemical_melting_point          ?
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'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
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'

_cell_length_a                   21.423(2)
_cell_length_b                   8.3075(4)
_cell_length_c                   7.3587(4)
_cell_angle_alpha                90
_cell_angle_beta                 90.112(6)
_cell_angle_gamma                90
_cell_volume                     1309.63(16)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    5726
_cell_measurement_temperature    130.01(11)
_cell_measurement_theta_max      28.5030
_cell_measurement_theta_min      2.6110
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    13.677
_exptl_absorpt_correction_T_max  0.777
_exptl_absorpt_correction_T_min  0.492
_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_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.481
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             896
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

_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0376
_diffrn_reflns_av_unetI/netI     0.0316
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.890
_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       -9
_diffrn_reflns_number            14134
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.890
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         29.014
_diffrn_reflns_theta_min         2.630
_diffrn_ambient_temperature      130.15
_diffrn_detector_area_resol_mean 8.0772
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.890
_diffrn_measurement_details      .
_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_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2529
_reflns_number_total             3091
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_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  (Sheldrick, 2015)'
_refine_diff_density_max         1.573
_refine_diff_density_min         -5.442
_refine_diff_density_rms         0.239
_refine_ls_extinction_coef       0.0061(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   1.255
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     137
_refine_ls_number_reflns         3091
_refine_ls_number_restraints     151
_refine_ls_R_factor_all          0.0734
_refine_ls_R_factor_gt           0.0597
_refine_ls_restrained_S_all      1.299
_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)+(0.0311P)²+21.0634P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1189
_refine_ls_wR_factor_ref         0.1267
_refine_special_details          ?
_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. Uiso/Uaniso restraints and constraints
Uanis(Cl2) \\sim Ueq, Uanis(Pb1) \\sim Ueq, Uanis(Cl1) \\sim Ueq, Uanis(Cl4)
\\sim Ueq, Uanis(Cl3) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(N3A) \\sim Ueq, Uanis(N2A) \\sim Ueq, Uanis(C1A) \\sim Ueq, Uanis(C2A)
\\sim Ueq, Uanis(N1A) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(N2B) \\sim Ueq, Uanis(C1B) \\sim Ueq, Uanis(N1B) \\sim Ueq, Uanis(N3B)
\\sim Ueq, Uanis(C2B) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
4. 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
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)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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 0.25000(3) 0.49215(4) 0.36524(4) 0.0389(2) Uani 1 1 d . U . . .
Cl1 Cl 0.2499(2) 0.7642(3) 0.1421(3) 0.0546(9) Uani 1 1 d . U . . .
Cl2 Cl 0.2500(2) 0.1822(3) 0.5385(4) 0.0559(9) Uani 1 1 d . U . . .
Cl4 Cl 0.3829(2) 0.4832(3) 0.3625(5) 0.0579(9) Uani 1 1 d . U . . .
Cl3 Cl 0.1173(2) 0.4832(3) 0.3625(5) 0.0580(9) Uani 1 1 d . U . . .
N2A N 0.3958(5) 0.3987(11) 0.8565(14) 0.043(2) Uani 1 1 d D U . . .
H2A H 0.376777 0.306618 0.877364 0.051 Uiso 1 1 calc R U . . .
N1B N 0.0878(5) 0.6474(11) 0.8314(14) 0.048(2) Uani 1 1 d D U . . .
H1B H 0.092728 0.752530 0.832683 0.057 Uiso 1 1 calc R U . . .
N1A N 0.4126(5) 0.6473(11) 0.8320(14) 0.048(3) Uani 1 1 d D U . . .
H1A H 0.407862 0.752515 0.834117 0.057 Uiso 1 1 calc R U . . .
N2B N 0.1043(5) 0.3988(12) 0.8567(14) 0.047(2) Uani 1 1 d D U . . .
H2B H 0.123167 0.306715 0.878347 0.056 Uiso 1 1 calc R U . . .
C1A C 0.3696(7) 0.5392(14) 0.8736(18) 0.049(3) Uani 1 1 d D U . . .
H1AA H 0.327743 0.560027 0.909159 0.059 Uiso 1 1 calc R U . . .
C1B C 0.1309(7) 0.5390(13) 0.8729(19) 0.049(3) Uani 1 1 d D U . . .
H1BA H 0.172835 0.559468 0.907730 0.059 Uiso 1 1 calc R U . . .
N3A N 0.4550(6) 0.4116(12) 0.8033(17) 0.057(3) Uani 1 1 d D U . . .
N3B N 0.0448(5) 0.4117(12) 0.8031(16) 0.053(2) Uani 1 1 d D U . . .
C2A C 0.4652(7) 0.5670(14) 0.786(2) 0.054(3) Uani 1 1 d D U . . .
H2AA H 0.503103 0.614957 0.746536 0.065 Uiso 1 1 calc R U . . .
C2B C 0.0351(7) 0.5674(14) 0.787(2) 0.055(3) Uani 1 1 d D U . . .
H2BA H -0.002954 0.615964 0.749108 0.066 Uiso 1 1 calc R U . . .

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 0.0980(4) 0.0091(2) 0.0096(2) -0.00024(11) 0.00038(18) -0.00006(19)
Cl1 0.130(3) 0.0179(11) 0.0161(12) 0.0062(9) 0.0001(14) -0.0002(14)
Cl2 0.125(3) 0.0205(12) 0.0218(12) 0.0096(9) 0.0008(15) 0.0001(15)
Cl4 0.090(3) 0.0129(12) 0.071(2) 0.0009(12) -0.0140(18) -0.0042(14)
Cl3 0.090(3) 0.0132(12) 0.071(2) 0.0010(12) 0.0167(18) 0.0039(14)
N2A 0.050(6) 0.025(4) 0.052(5) 0.003(4) -0.010(4) 0.003(4)
N1B 0.068(5) 0.024(4) 0.052(5) 0.002(3) 0.018(4) -0.002(3)
N1A 0.068(6) 0.022(4) 0.054(5) 0.000(4) -0.020(5) 0.000(4)
N2B 0.059(5) 0.026(4) 0.055(5) 0.003(3) 0.019(4) -0.003(3)
C1A 0.066(7) 0.035(5) 0.046(6) 0.001(5) 0.000(5) 0.010(5)
C1B 0.067(5) 0.027(4) 0.054(6) 0.005(4) 0.010(4) -0.006(3)
N3A 0.069(7) 0.025(5) 0.076(7) -0.002(4) -0.032(5) 0.003(5)
N3B 0.060(5) 0.027(4) 0.071(6) -0.002(4) 0.026(4) -0.002(3)
C2A 0.060(7) 0.030(5) 0.073(7) 0.003(5) -0.023(6) 0.001(5)
C2B 0.063(5) 0.029(4) 0.073(7) -0.001(4) 0.019(4) -0.002(4)

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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 2.793(2) . ?
Pb1 Cl1 2.872(2) 4_576 ?
Pb1 Cl2 2.806(2) 4_565 ?
Pb1 Cl2 2.874(2) . ?
Pb1 Cl4 2.848(4) . ?
Pb1 Cl3 2.844(4) . ?
N2A H2A 0.8800 . ?
N2A C1A 1.302(13) . ?
N2A N3A 1.333(14) . ?
N1B H1B 0.8800 . ?
N1B C1B 1.324(15) . ?
N1B C2B 1.351(15) . ?
N1A H1A 0.8800 . ?
N1A C1A 1.323(15) . ?
N1A C2A 1.353(15) . ?
N2B H2B 0.8800 . ?
N2B C1B 1.301(13) . ?
N2B N3B 1.338(14) . ?
C1A H1AA 0.9500 . ?
C1B H1BA 0.9500 . ?
N3A C2A 1.316(14) . ?
N3B C2B 1.316(14) . ?
C2A H2AA 0.9500 . ?
C2B H2BA 0.9500 . ?

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 81.187(12) . 4_576 ?
Cl1 Pb1 Cl2 170.34(8) . . ?
Cl1 Pb1 Cl2 85.05(8) . 4_565 ?
Cl1 Pb1 Cl2 108.48(8) 4_576 . ?
Cl1 Pb1 Cl4 90.95(11) . . ?
Cl1 Pb1 Cl3 91.00(11) . . ?
Cl2 Pb1 Cl1 166.24(8) 4_565 4_576 ?
Cl2 Pb1 Cl2 85.28(3) 4_565 . ?
Cl2 Pb1 Cl4 88.78(12) 4_565 . ?
Cl2 Pb1 Cl3 88.98(12) 4_565 . ?
Cl4 Pb1 Cl1 91.46(11) . 4_576 ?
Cl4 Pb1 Cl2 88.88(11) . . ?
Cl3 Pb1 Cl1 91.23(11) . 4_576 ?
Cl3 Pb1 Cl2 88.80(11) . . ?
Cl3 Pb1 Cl4 176.90(8) . . ?
Pb1 Cl1 Pb1 170.83(10) . 4_575 ?
Pb1 Cl2 Pb1 147.41(11) 4_566 . ?
C1A N2A H2A 124.2 . . ?
C1A N2A N3A 111.6(10) . . ?
N3A N2A H2A 124.2 . . ?
C1B N1B H1B 126.2 . . ?
C1B N1B C2B 107.7(11) . . ?
C2B N1B H1B 126.2 . . ?
C1A N1A H1A 126.1 . . ?
C1A N1A C2A 107.7(10) . . ?
C2A N1A H1A 126.1 . . ?
C1B N2B H2B 124.1 . . ?
C1B N2B N3B 111.8(11) . . ?
N3B N2B H2B 124.1 . . ?
N2A C1A N1A 106.6(12) . . ?
N2A C1A H1AA 126.7 . . ?
N1A C1A H1AA 126.7 . . ?
N1B C1B H1BA 126.8 . . ?
N2B C1B N1B 106.5(12) . . ?
N2B C1B H1BA 126.8 . . ?
C2A N3A N2A 105.4(11) . . ?
C2B N3B N2B 104.8(11) . . ?
N1A C2A H2AA 125.6 . . ?
N3A C2A N1A 108.7(12) . . ?
N3A C2A H2AA 125.6 . . ?
N1B C2B H2BA 125.4 . . ?
N3B C2B N1B 109.2(12) . . ?
N3B C2B H2BA 125.4 . . ?

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 1.4(14) . . . . ?
N2B N3B C2B N1B -0.6(14) . . . . ?
C1A N2A N3A C2A -0.6(14) . . . . ?
C1A N1A C2A N3A -1.7(15) . . . . ?
C1B N1B C2B N3B 1.1(15) . . . . ?
C1B N2B N3B C2B -0.1(14) . . . . ?
N3A N2A C1A N1A -0.4(14) . . . . ?
N3B N2B C1B N1B 0.8(15) . . . . ?
C2A N1A C1A N2A 1.3(15) . . . . ?
C2B N1B C1B N2B -1.1(15) . . . . ?

_shelx_res_file                  
;
TITL triag2pbcl4_06_130_00_a.res in P2(1)/c
    triag2pbcl4_iv_130_00.res
    created by SHELXL-2019/2 at 16:40:06 on 01-Mar-2024
REM Old TITL TRIAG2PbCl4_06_130_00 in P2(1)/c
REM SHELXT solution in P2(1)/c: R1 0.379, Rweak 0.157, Alpha 0.032
REM <I/s> 1.201 for 199 systematic absences, Orientation as input
REM Formula found by SHELXT: C5 N2B Cl4 Pb
CELL 0.71073 21.4229 8.3075 7.3587 90 90.112 90
ZERR 4 0.0022 0.0004 0.0004 0 0.006 0
LATT 1
SYMM -X,0.5+Y,0.5-Z
SFAC C H Cl N Pb
UNIT 16 32 16 24 4
ISOR 0.01 0.02 Cl2 Pb1 Cl1 Cl4 Cl3
RIGU Cl2 Pb1 Cl1 Cl4 Cl3
RIGU N3B N2B C1B C2B N1B
ISOR 0.01 0.02 N3A N2A C1A C2A N1A
RIGU N2B C1B N1B N3B C2B
ISOR 0.01 0.02 N2B C1B N1B N3B C2B
SADI N3A N2A N3B N2B
SADI N3B C2B N3A C2A
SADI N2A C1A N2B C1B
SADI N1B C1B N1A C1A
SADI N1B C2B N1A C2A

L.S. 44
PLAN  5
TEMP -143
CONF
list 4
MORE -1
BOND $H
fmap 2 53
acta 50
OMIT -22 2 1
OMIT -21 1 4
OMIT 0 2 0
OMIT 0 4 0
OMIT 1 2 0
OMIT 4 0 0
OMIT 4 1 0
OMIT 5 0 0
OMIT 8 0 0
OMIT 21 2 2
OMIT 22 1 2
OMIT 22 3 2
OMIT 22 4 1
OMIT 23 3 0
OMIT 23 5 2
OMIT 24 2 1
OMIT 25 3 0
OMIT 25 4 1
OMIT 28 2 1
REM <olex2.extras>
REM <HklSrc "%.\\triag2pbcl4_iv_130_00.hkl">
REM </olex2.extras>

WGHT    0.031100   21.063400
EXTI    0.006107
FVAR       2.87057
PB1   5    0.249995    0.492153    0.365243    11.00000    0.09797    0.00909 =
         0.00963   -0.00024    0.00038   -0.00006
CL1   3    0.249905    0.764157    0.142062    11.00000    0.12989    0.01786 =
         0.01612    0.00622    0.00011   -0.00024
CL2   3    0.250013    0.182156    0.538549    11.00000    0.12531    0.02052 =
         0.02178    0.00959    0.00083    0.00006
CL4   3    0.382865    0.483197    0.362541    11.00000    0.08981    0.01292 =
         0.07079    0.00088   -0.01404   -0.00422
CL3   3    0.117291    0.483208    0.362478    11.00000    0.08964    0.01317 =
         0.07120    0.00099    0.01668    0.00392
N2A   4    0.395789    0.398655    0.856464    11.00000    0.05029    0.02517 =
         0.05200    0.00261   -0.00998    0.00328
AFIX  43
H2A   2    0.376777    0.306618    0.877364    11.00000   -1.20000
AFIX   0

N1B   4    0.087844    0.647359    0.831368    11.00000    0.06819    0.02363 =
         0.05195    0.00231    0.01819   -0.00170
AFIX  43
H1B   2    0.092728    0.752530    0.832683    11.00000   -1.20000
AFIX   0

N1A   4    0.412592    0.647309    0.831986    11.00000    0.06785    0.02158 =
         0.05409    0.00033   -0.01981   -0.00028
AFIX  43
H1A   2    0.407862    0.752515    0.834117    11.00000   -1.20000
AFIX   0

N2B   4    0.104284    0.398829    0.856682    11.00000    0.05944    0.02587 =
         0.05540    0.00252    0.01864   -0.00292
AFIX  43
H2B   2    0.123167    0.306715    0.878347    11.00000   -1.20000
AFIX   0

C1A   1    0.369579    0.539173    0.873647    11.00000    0.06631    0.03470 =
         0.04634    0.00116    0.00033    0.00970
AFIX  43
H1AA  2    0.327743    0.560027    0.909159    11.00000   -1.20000
AFIX   0

C1B   1    0.130854    0.538985    0.872921    11.00000    0.06658    0.02726 =
         0.05421    0.00465    0.00997   -0.00608
AFIX  43
H1BA  2    0.172835    0.559468    0.907730    11.00000   -1.20000
AFIX   0

N3A   4    0.455017    0.411555    0.803262    11.00000    0.06898    0.02503 =
         0.07607   -0.00236   -0.03209    0.00297
N3B   4    0.044799    0.411745    0.803074    11.00000    0.06022    0.02693 =
         0.07069   -0.00207    0.02552   -0.00213
C2A   1    0.465158    0.567029    0.785517    11.00000    0.06006    0.03018 =
         0.07310    0.00326   -0.02329    0.00067
AFIX  43
H2AA  2    0.503103    0.614957    0.746536    11.00000   -1.20000
AFIX   0

C2B   1    0.035106    0.567436    0.786581    11.00000    0.06274    0.02863 =
         0.07279   -0.00065    0.01932   -0.00174
AFIX  43
H2BA  2   -0.002954    0.615964    0.749108    11.00000   -1.20000
AFIX   0
HKLF 4




REM  triag2pbcl4_06_130_00_a.res in P2(1)/c
REM wR2 = 0.1267, GooF = S = 1.255, Restrained GooF = 1.299 for all data
REM R1 = 0.0597 for 2529 Fo > 4sig(Fo) and 0.0734 for all 3091 data
REM 137 parameters refined using 151 restraints

END

WGHT      0.0304     21.2278

REM Highest difference peak  1.573,  deepest hole -5.442,  1-sigma level  0.239
Q1    1   0.2787  0.5606  0.3433  11.00000  0.05    1.57
Q2    1   0.2214  0.5633  0.3804  11.00000  0.05    1.56
Q3    1   0.2436  0.6053  0.3791  11.00000  0.05    1.47
Q4    1   0.2546  0.3748  0.3633  11.00000  0.05    1.21
Q5    1   0.2055  0.4025  0.3635  11.00000  0.05    1.18
;
_shelx_res_checksum              13642
_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
;
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_triag2pbcl4_iii_280_00
_database_code_depnum_ccdc_archive 'CCDC 2314661'
loop_
_audit_author_name
_audit_author_address
'Szymon Sobczak'
;Department of Materials Chemistry, Adam Mickiewicz University
Poland
;
_audit_update_record             
;
2024-03-04 deposited with the CCDC.	2024-03-21 downloaded from the CCDC.
;
_audit_creation_date             2023-12-15
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        Tz2PbCl4
_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_melting_point          ?
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'

_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.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'
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'

_cell_length_a                   7.4798(4)
_cell_length_b                   21.5667(13)
_cell_length_c                   8.3086(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1340.30(13)
_cell_formula_units_Z            7
_cell_measurement_reflns_used    5993
_cell_measurement_temperature    280.01(10)
_cell_measurement_theta_max      28.7960
_cell_measurement_theta_min      3.6460
_shelx_estimated_absorpt_T_max   0.297
_shelx_estimated_absorpt_T_min   0.050
_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_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.424
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             896
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

_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_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
_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_details      .
_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_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1339
_reflns_number_total             1662
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_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)'
_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_R_factor_all          0.0325
_refine_ls_R_factor_gt           0.0244
_refine_ls_restrained_S_all      1.133
_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
_refine_special_details          ?
_olex2_refinement_description    
;
1.a Aromatic/amide H refined with riding coordinates:
 N2(H2), N1(H1), C1(H1A), C2(H2A)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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_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_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) . . . . ?

_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
;
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_triag2pbcl4_iv_180_00
_database_code_depnum_ccdc_archive 'CCDC 2314657'
loop_
_audit_author_name
_audit_author_address
'Szymon Sobczak'
;Department of Materials Chemistry, Adam Mickiewicz University
Poland
;
_audit_update_record             
;
2024-03-04 deposited with the CCDC.	2024-03-21 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT972_triag2pbcl4_iv_180_00 
;
PROBLEM: Check Calcd Resid. Dens.  0.99Ang From Pb1            -4.41 eA-3
RESPONSE: Residual density near heavy atom.
;
_vrf_PLAT112_triag2pbcl4_iv_180_00 
;
PROBLEM: ADDSYM Detects New (Pseudo) Symm. Elem         n        100 %Fit
RESPONSE: The symmetry has been thoroughly inspected by the presence of the systematic absences in the raw diffraction data
;
_vrf_PLAT113_triag2pbcl4_iv_180_00 
;
PROBLEM: ADDSYM Suggests Possible Pseudo/New  Space Group       Pnma Check
RESPONSE: look PLAT112
;
# Added during the CSD deposition process: Friday 15 December 2023 12:43 PM
# end Validation Reply Form

_audit_creation_date             2023-12-15
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        Tz2PbCl4
_chemical_formula_moiety         'Cl4 Pb, 2(C2 H4 N3)'
_chemical_formula_sum            'C4 H8 Cl4 N6 Pb'
_chemical_formula_weight         489.15
_chemical_melting_point          ?
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'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
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'

_cell_length_a                   21.4212(18)
_cell_length_b                   8.2997(3)
_cell_length_c                   7.4042(3)
_cell_angle_alpha                90
_cell_angle_beta                 90.020(5)
_cell_angle_gamma                90
_cell_volume                     1316.39(13)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    5562
_cell_measurement_temperature    180.01(10)
_cell_measurement_theta_max      28.6500
_cell_measurement_theta_min      2.5300
_shelx_estimated_absorpt_T_max   0.292
_shelx_estimated_absorpt_T_min   0.049
_exptl_absorpt_coefficient_mu    13.607
_exptl_absorpt_correction_T_max  0.778
_exptl_absorpt_correction_T_min  0.495
_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_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.468
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             896
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

_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0380
_diffrn_reflns_av_unetI/netI     0.0314
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.894
_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            14257
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.894
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         28.972
_diffrn_reflns_theta_min         2.632
_diffrn_ambient_temperature      180.15
_diffrn_detector_area_resol_mean 8.0772
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.894
_diffrn_measurement_details      .
_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_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2487
_reflns_number_total             3117
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_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    'SHELXD  (Sheldrick, 2008)'
_refine_diff_density_max         1.712
_refine_diff_density_min         -4.308
_refine_diff_density_rms         0.209
_refine_ls_extinction_coef       0.0082(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   1.192
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     137
_refine_ls_number_reflns         3113
_refine_ls_number_restraints     61
_refine_ls_R_factor_all          0.0640
_refine_ls_R_factor_gt           0.0484
_refine_ls_restrained_S_all      1.188
_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)+(0.0356P)²+11.7192P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1039
_refine_ls_wR_factor_ref         0.1126
_refine_special_details          ?
_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.a Aromatic/amide H refined with riding coordinates:
 N2A(H2A), N1B(H1B), N1A(H1A), N2B(H2B), C1A(H1AA), C1B(H1BA), C2A(H2AA),
 C2B(H2BA)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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 0.25000(2) 0.49363(3) 0.36343(4) 0.03763(18) Uani 1 1 d . . . . .
Cl1 Cl 0.24984(16) 0.7640(3) 0.1389(3) 0.0573(8) Uani 1 1 d . . . . .
Cl2 Cl 0.24996(18) 0.1873(3) 0.5431(3) 0.0610(8) Uani 1 1 d . . . . .
Cl4 Cl 0.38285(16) 0.4863(3) 0.3596(5) 0.0598(8) Uani 1 1 d . . . . .
Cl3 Cl 0.11690(16) 0.4864(3) 0.3595(5) 0.0598(8) Uani 1 1 d . . . . .
N2A N 0.3958(5) 0.3948(9) 0.8530(13) 0.053(2) Uani 1 1 d D . . . .
H2A H 0.377242 0.302022 0.873642 0.064 Uiso 1 1 calc R U . . .
N1B N 0.0889(5) 0.6439(9) 0.8301(12) 0.054(2) Uani 1 1 d D . . . .
H1B H 0.094170 0.748985 0.832592 0.064 Uiso 1 1 calc R U . . .
N1A N 0.4109(5) 0.6439(9) 0.8300(12) 0.055(3) Uani 1 1 d D . . . .
H1A H 0.405629 0.749039 0.831349 0.066 Uiso 1 1 calc R U . . .
N2B N 0.1046(4) 0.3954(9) 0.8543(13) 0.052(2) Uani 1 1 d D . . . .
H2B H 0.123380 0.303082 0.875934 0.062 Uiso 1 1 calc R U . . .
C1A C 0.3686(6) 0.5345(12) 0.8711(16) 0.056(3) Uani 1 1 d D . . . .
H1AA H 0.326629 0.553541 0.906771 0.067 Uiso 1 1 calc R U . . .
C1B C 0.1312(6) 0.5353(11) 0.8691(16) 0.055(2) Uani 1 1 d D . . . .
H1BA H 0.173362 0.555264 0.902104 0.066 Uiso 1 1 calc R U . . .
N3A N 0.4557(5) 0.4092(10) 0.7989(16) 0.066(3) Uani 1 1 d D . . . .
N3B N 0.0444(5) 0.4096(9) 0.8014(14) 0.059(2) Uani 1 1 d D . . . .
C2A C 0.4640(6) 0.5646(11) 0.7852(19) 0.066(4) Uani 1 1 d D . . . .
H2AA H 0.501768 0.614959 0.749004 0.079 Uiso 1 1 calc R U . . .
C2B C 0.0356(6) 0.5654(11) 0.7851(18) 0.061(3) Uani 1 1 d D . . . .
H2BA H -0.002120 0.615413 0.747765 0.073 Uiso 1 1 calc R U . . .

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 0.0882(3) 0.01170(19) 0.01296(19) -0.00029(9) 0.00047(15) 0.00004(15)
Cl1 0.127(3) 0.0233(10) 0.0214(10) 0.0092(8) 0.0002(13) -0.0009(12)
Cl2 0.127(3) 0.0257(11) 0.0300(12) 0.0143(9) 0.0007(13) 0.0005(14)
Cl4 0.086(2) 0.0155(10) 0.078(2) 0.0005(10) -0.0104(15) -0.0024(11)
Cl3 0.084(2) 0.0165(10) 0.079(2) -0.0002(10) 0.0132(15) 0.0027(11)
N2A 0.076(7) 0.020(4) 0.064(6) 0.007(4) -0.006(5) 0.003(4)
N1B 0.082(5) 0.019(3) 0.060(5) 0.003(3) 0.024(4) -0.003(3)
N1A 0.090(8) 0.018(4) 0.057(6) 0.002(3) -0.020(5) 0.006(4)
N2B 0.066(5) 0.023(3) 0.066(6) 0.004(3) 0.019(4) 0.000(3)
C1A 0.083(9) 0.035(5) 0.050(7) 0.003(5) -0.002(6) 0.016(5)
C1B 0.080(6) 0.026(4) 0.058(6) 0.004(4) 0.012(4) -0.007(3)
N3A 0.071(7) 0.024(4) 0.104(9) -0.001(5) -0.035(6) 0.004(4)
N3B 0.068(5) 0.021(4) 0.088(7) 0.000(3) 0.029(4) -0.002(3)
C2A 0.070(8) 0.022(5) 0.105(10) 0.007(5) -0.032(7) -0.003(5)
C2B 0.070(6) 0.024(4) 0.088(8) 0.004(4) 0.024(5) -0.003(3)

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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 2.793(2) . ?
Pb1 Cl1 2.8648(19) 4_576 ?
Pb1 Cl2 2.807(2) 4_565 ?
Pb1 Cl2 2.870(2) . ?
Pb1 Cl4 2.847(4) . ?
Pb1 Cl3 2.852(3) . ?
N2A H2A 0.8800 . ?
N2A C1A 1.304(12) . ?
N2A N3A 1.351(12) . ?
N1B H1B 0.8800 . ?
N1B C1B 1.309(13) . ?
N1B C2B 1.355(13) . ?
N1A H1A 0.8800 . ?
N1A C1A 1.319(13) . ?
N1A C2A 1.355(13) . ?
N2B H2B 0.8800 . ?
N2B C1B 1.298(12) . ?
N2B N3B 1.354(12) . ?
C1A H1AA 0.9500 . ?
C1B H1BA 0.9500 . ?
N3A C2A 1.306(12) . ?
N3B C2B 1.313(12) . ?
C2A H2AA 0.9500 . ?
C2B H2BA 0.9500 . ?

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 81.930(9) . 4_576 ?
Cl1 Pb1 Cl2 85.81(7) . 4_565 ?
Cl1 Pb1 Cl2 171.09(7) . . ?
Cl1 Pb1 Cl2 106.98(7) 4_576 . ?
Cl1 Pb1 Cl4 90.70(9) . . ?
Cl1 Pb1 Cl3 90.57(9) . . ?
Cl2 Pb1 Cl1 167.74(7) 4_565 4_576 ?
Cl2 Pb1 Cl2 85.28(2) 4_565 . ?
Cl2 Pb1 Cl4 88.87(10) 4_565 . ?
Cl2 Pb1 Cl3 88.86(10) 4_565 . ?
Cl4 Pb1 Cl1 91.34(9) . 4_576 ?
Cl4 Pb1 Cl2 89.20(9) . . ?
Cl4 Pb1 Cl3 177.31(7) . . ?
Cl3 Pb1 Cl1 91.18(9) . 4_576 ?
Cl3 Pb1 Cl2 89.17(9) . . ?
Pb1 Cl1 Pb1 171.13(9) . 4_575 ?
Pb1 Cl2 Pb1 149.96(10) 4_566 . ?
C1A N2A H2A 123.9 . . ?
C1A N2A N3A 112.1(9) . . ?
N3A N2A H2A 123.9 . . ?
C1B N1B H1B 126.1 . . ?
C1B N1B C2B 107.8(9) . . ?
C2B N1B H1B 126.1 . . ?
C1A N1A H1A 126.3 . . ?
C1A N1A C2A 107.4(9) . . ?
C2A N1A H1A 126.3 . . ?
C1B N2B H2B 124.3 . . ?
C1B N2B N3B 111.4(9) . . ?
N3B N2B H2B 124.3 . . ?
N2A C1A N1A 106.3(11) . . ?
N2A C1A H1AA 126.8 . . ?
N1A C1A H1AA 126.8 . . ?
N1B C1B H1BA 126.5 . . ?
N2B C1B N1B 107.1(11) . . ?
N2B C1B H1BA 126.5 . . ?
C2A N3A N2A 103.8(9) . . ?
C2B N3B N2B 104.4(9) . . ?
N1A C2A H2AA 124.8 . . ?
N3A C2A N1A 110.3(10) . . ?
N3A C2A H2AA 124.8 . . ?
N1B C2B H2BA 125.3 . . ?
N3B C2B N1B 109.3(10) . . ?
N3B C2B H2BA 125.3 . . ?

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 0.2(13) . . . . ?
N2B N3B C2B N1B -1.0(12) . . . . ?
C1A N2A N3A C2A 0.2(13) . . . . ?
C1A N1A C2A N3A -0.5(14) . . . . ?
C1B N1B C2B N3B 1.8(13) . . . . ?
C1B N2B N3B C2B -0.1(12) . . . . ?
N3A N2A C1A N1A -0.5(13) . . . . ?
N3B N2B C1B N1B 1.3(13) . . . . ?
C2A N1A C1A N2A 0.6(13) . . . . ?
C2B N1B C1B N2B -1.8(13) . . . . ?

_shelx_res_file                  
;
TITL triag2pbcl4_07_180_00_a.res in P2(1)/c
    triag2pbcl4_iv_180_00.res
    created by SHELXL-2019/2 at 17:02:12 on 01-Mar-2024
REM Old TITL TRIAG2PbCl4_07_180_00 in P2(1)/c
REM SHELXT solution in P2(1)/c: R1 0.324, Rweak 0.113, Alpha 0.016
REM <I/s> 1.080 for 202 systematic absences, Orientation as input
REM Formula found by SHELXT: C8 N2 Cl4 Pb
CELL 0.71073 21.421209 8.299677 7.404236 90 90.0203 90
ZERR 4 0.001766 0.000311 0.000332 0 0.0049 0
LATT 1
SYMM -X,0.5+Y,0.5-Z
SFAC C H Cl N Pb
UNIT 16 32 16 24 4
RIGU Cl2 Pb1 Cl1 Cl4 Cl3
RIGU N3B N2B C1B C2B N1B
RIGU N2B C1B N1B N3B C2B
SADI N3A N2A N3B N2B
SADI N3B C2B N3A C2A
SADI N2A C1A N2B C1B
SADI N1B C1B N1A C1A
SADI N1B C2B N1A C2A

L.S. 24
PLAN  5
SIZE 0.12 0.16 0.50
TEMP -93
CONF
list 4
MORE -1
BOND $H
fmap 2
acta 50
OMIT -24 2 1
OMIT -23 2 2
OMIT -22 1 2
OMIT -22 2 3
OMIT 0 2 0
OMIT 0 4 0
OMIT 1 2 0
OMIT 3 0 0
OMIT 3 2 0
OMIT 3 4 0
OMIT 4 0 0
OMIT 4 1 0
OMIT 5 0 0
OMIT 22 2 1
OMIT 22 3 2
OMIT 22 4 1
OMIT 23 1 0
OMIT 23 3 0
OMIT 24 2 1
OMIT 25 3 0
REM <olex2.extras>
REM <HklSrc "%.\\triag2pbcl4_iv_180_00.hkl">
REM </olex2.extras>

WGHT    0.035600   11.719200
EXTI    0.008249
FVAR       2.95446
PB1   5    0.249997    0.493633    0.363432    11.00000    0.08823    0.01170 =
         0.01296   -0.00029    0.00047    0.00004
CL1   3    0.249844    0.763998    0.138909    11.00000    0.12722    0.02329 =
         0.02144    0.00917    0.00023   -0.00085
CL2   3    0.249957    0.187271    0.543143    11.00000    0.12736    0.02565 =
         0.03001    0.01432    0.00072    0.00051
CL4   3    0.382853    0.486302    0.359640    11.00000    0.08577    0.01555 =
         0.07813    0.00054   -0.01039   -0.00239
CL3   3    0.116905    0.486390    0.359521    11.00000    0.08431    0.01652 =
         0.07866   -0.00021    0.01324    0.00267
N2A   4    0.395784    0.394821    0.852988    11.00000    0.07598    0.01995 =
         0.06443    0.00686   -0.00573    0.00304
AFIX  43
H2A   2    0.377242    0.302022    0.873642    11.00000   -1.20000
AFIX   0

N1B   4    0.088920    0.643850    0.830095    11.00000    0.08198    0.01871 =
         0.06040    0.00267    0.02382   -0.00271
AFIX  43
H1B   2    0.094170    0.748985    0.832592    11.00000   -1.20000
AFIX   0

N1A   4    0.410896    0.643893    0.829958    11.00000    0.09012    0.01768 =
         0.05705    0.00157   -0.02000    0.00616
AFIX  43
H1A   2    0.405629    0.749039    0.831349    11.00000   -1.20000
AFIX   0

N2B   4    0.104619    0.395418    0.854315    11.00000    0.06596    0.02332 =
         0.06601    0.00437    0.01880    0.00004
AFIX  43
H2B   2    0.123380    0.303082    0.875934    11.00000   -1.20000
AFIX   0

C1A   1    0.368575    0.534451    0.871081    11.00000    0.08303    0.03478 =
         0.05039    0.00270   -0.00208    0.01598
AFIX  43
H1AA  2    0.326629    0.553541    0.906771    11.00000   -1.20000
AFIX   0

C1B   1    0.131198    0.535340    0.869145    11.00000    0.08024    0.02579 =
         0.05778    0.00436    0.01246   -0.00680
AFIX  43
H1BA  2    0.173362    0.555264    0.902104    11.00000   -1.20000
AFIX   0

N3A   4    0.455740    0.409207    0.798854    11.00000    0.07146    0.02373 =
         0.10422   -0.00100   -0.03521    0.00369
N3B   4    0.044376    0.409568    0.801372    11.00000    0.06802    0.02137 =
         0.08846    0.00026    0.02879   -0.00181
C2A   1    0.463955    0.564634    0.785192    11.00000    0.06973    0.02247 =
         0.10457    0.00653   -0.03239   -0.00266
AFIX  43
H2AA  2    0.501768    0.614959    0.749004    11.00000   -1.20000
AFIX   0

C2B   1    0.035630    0.565425    0.785145    11.00000    0.07049    0.02357 =
         0.08779    0.00433    0.02430   -0.00262
AFIX  43
H2BA  2   -0.002120    0.615413    0.747765    11.00000   -1.20000
AFIX   0
HKLF 4




REM  triag2pbcl4_07_180_00_a.res in P2(1)/c
REM wR2 = 0.1126, GooF = S = 1.192, Restrained GooF = 1.188 for all data
REM R1 = 0.0484 for 2483 Fo > 4sig(Fo) and 0.0640 for all 3113 data
REM 137 parameters refined using 61 restraints

END

WGHT      0.0350     11.7917

REM Highest difference peak  1.712,  deepest hole -4.308,  1-sigma level  0.209
Q1    1   0.2505  0.6131  0.3630  11.00000  0.05    1.71
Q2    1   0.2286  0.5733  0.3799  11.00000  0.05    1.71
Q3    1   0.2738  0.5764  0.3560  11.00000  0.05    1.52
Q4    1   0.2485  0.3897  0.3746  11.00000  0.05    1.51
Q5    1   0.2898  0.4008  0.3512  11.00000  0.05    1.37
;
_shelx_res_checksum              43830
_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
;
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_triag2pbcl4_iii_300_00
_database_code_depnum_ccdc_archive 'CCDC 2314662'
loop_
_audit_author_name
_audit_author_address
'Szymon Sobczak'
;Department of Materials Chemistry, Adam Mickiewicz University
Poland
;
_audit_update_record             
;
2024-03-04 deposited with the CCDC.	2024-03-21 downloaded from the CCDC.
;
_audit_creation_date             2023-12-15
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        Tz2PbCl4
_chemical_formula_moiety         'Cl4 Pb, 2(C2 H4 N3)'
_chemical_formula_sum            'C4 H8 Cl4 N6 Pb'
_chemical_formula_weight         489.15
_chemical_melting_point          ?
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'

_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.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'
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'

_cell_length_a                   7.4929(3)
_cell_length_b                   21.5667(10)
_cell_length_c                   8.3106(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1342.97(10)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    5848
_cell_measurement_temperature    300.00(10)
_cell_measurement_theta_max      28.7830
_cell_measurement_theta_min      3.6480
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    13.338
_exptl_absorpt_correction_T_max  0.248
_exptl_absorpt_correction_T_min  0.059
_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_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.419
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             896
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-10 4 1 0.0870
0 1 -12 0.2751
10 -4 -1 0.0624
1 -1 12 0.2688
1 1 12 0.2692
1 30 1 0.0854
-1 2 -12 0.2722
-1 -30 -1 0.0345

_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0465
_diffrn_reflns_av_unetI/netI     0.0252
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.919
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            13880
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.919
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         28.953
_diffrn_reflns_theta_min         3.661
_diffrn_ambient_temperature      300.15
_diffrn_detector_area_resol_mean 8.0772
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.919
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     23.00  48.00   1.00    5.00    --   17.79-139.00 143.00   25
  2  ω     16.00  41.00   1.00    5.00    --   17.79-130.00 -42.00   25
  3  ω    -62.00 -18.00   1.00    5.00    --  -18.57 130.00  29.00   44
  4  ω    -75.00 -47.00   1.00    5.00    --  -18.57 139.00-156.00   28
  5  ω     39.00  94.00   1.00    5.00    --   17.79 178.00  30.00   55
  6  ω     43.00  68.00   1.00    5.00    --   17.79 178.00-150.00   25
  7  ω    -47.00  61.00   1.00    5.00    --   17.79 -19.00 150.00  108
  8  ω    -32.00  11.00   1.00    5.00    --  -18.57 -77.00 120.00   43
  9  ω    -87.00   3.00   1.00    5.00    --  -18.57 -57.00  90.00   90
 10  ω    -84.00 -59.00   1.00    5.00    --  -18.57-178.00   0.00   25
 11  ω    -32.00  11.00   1.00    5.00    --  -18.57 -77.00 -30.00   43
 12  ω     -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       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1299
_reflns_number_total             1675
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_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  (Sheldrick, 2015)'
_refine_diff_density_max         1.214
_refine_diff_density_min         -1.129
_refine_diff_density_rms         0.141
_refine_ls_extinction_coef       0.0191(6)
_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   1.114
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     78
_refine_ls_number_reflns         1675
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0381
_refine_ls_R_factor_gt           0.0275
_refine_ls_restrained_S_all      1.114
_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)+(0.0248P)²+3.3492P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0608
_refine_ls_wR_factor_ref         0.0656
_refine_special_details          ?
_olex2_refinement_description    
;
1.a Aromatic/amide H refined with riding coordinates:
 N2(H2), N1(H1), C1(H1A), C2(H2A)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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 0.34453(3) 0.250000 0.49724(2) 0.02506(14) Uani 1 2 d S T P . .
Cl3 Cl 0.3394(2) 0.11734(8) 0.49452(13) 0.0525(5) Uani 1 1 d . . . . .
Cl2 Cl 0.5431(3) 0.250000 0.2037(3) 0.0625(6) Uani 1 2 d S T P . .
N2 N 0.8347(7) 0.1048(2) 0.3857(6) 0.0518(14) Uani 1 1 d . . . . .
H2 H 0.851018 0.122542 0.294150 0.07(2) Uiso 1 1 calc R . . . .
N1 N 0.8165(7) 0.0919(3) 0.6337(6) 0.0539(14) Uani 1 1 d . . . . .
H1 H 0.818649 0.097804 0.736047 0.08(2) Uiso 1 1 calc R . . . .
C1 C 0.8488(9) 0.1327(4) 0.5232(7) 0.0547(18) Uani 1 1 d . . . . .
H1A H 0.876827 0.174283 0.539518 0.07(2) Uiso 1 1 calc R . . . .
C2 C 0.7793(13) 0.0387(3) 0.5583(8) 0.068(2) Uani 1 1 d . . . . .
H2A H 0.748531 0.001960 0.610093 0.10(3) Uiso 1 1 calc R . . . .
N3 N 0.7917(10) 0.0449(3) 0.4039(6) 0.0690(18) Uani 1 1 d . . . . .
Cl1 Cl 0.6147(3) 0.250000 0.7381(2) 0.0562(6) 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 0.02267(18) 0.03392(19) 0.01860(17) 0.000 -0.00049(9) 0.000
Cl3 0.0924(15) 0.0356(7) 0.0294(7) 0.0008(5) -0.0011(6) -0.0019(7)
Cl2 0.0527(13) 0.0861(16) 0.0488(12) 0.000 0.0285(11) 0.000
N2 0.071(4) 0.048(3) 0.036(3) 0.009(2) 0.006(2) -0.004(2)
N1 0.070(4) 0.066(4) 0.026(2) -0.011(2) 0.002(2) -0.002(3)
C1 0.063(5) 0.051(4) 0.051(4) -0.010(3) 0.011(3) -0.010(3)
C2 0.118(7) 0.050(4) 0.035(3) 0.007(3) 0.008(4) 0.000(4)
N3 0.121(5) 0.051(4) 0.035(3) -0.005(2) 0.005(3) -0.009(3)
Cl1 0.0422(11) 0.0848(16) 0.0417(11) 0.000 -0.0204(9) 0.000

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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 2.8614(16) 7_565 ?
Pb1 Cl3 2.8614(16) . ?
Pb1 Cl2 2.809(2) 6_556 ?
Pb1 Cl2 2.8576(19) . ?
Pb1 Cl1 2.7931(18) 6_557 ?
Pb1 Cl1 2.8473(18) . ?
N2 H2 0.8600 . ?
N2 C1 1.296(8) . ?
N2 N3 1.340(7) . ?
N1 H1 0.8600 . ?
N1 C1 1.296(9) . ?
N1 C2 1.337(9) . ?
C1 H1A 0.9300 . ?
C2 H2A 0.9300 . ?
C2 N3 1.294(9) . ?

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 178.22(7) . 7_565 ?
Cl2 Pb1 Cl3 89.12(3) 6_556 7_565 ?
Cl2 Pb1 Cl3 90.01(3) . 7_565 ?
Cl2 Pb1 Cl3 90.01(3) . . ?
Cl2 Pb1 Cl3 89.12(3) 6_556 . ?
Cl2 Pb1 Cl2 84.903(16) 6_556 . ?
Cl2 Pb1 Cl1 171.79(7) 6_556 . ?
Cl1 Pb1 Cl3 90.86(3) . 7_565 ?
Cl1 Pb1 Cl3 89.88(3) 6_557 . ?
Cl1 Pb1 Cl3 90.86(3) . . ?
Cl1 Pb1 Cl3 89.88(3) 6_557 7_565 ?
Cl1 Pb1 Cl2 88.41(7) 6_557 6_556 ?
Cl1 Pb1 Cl2 103.31(7) . . ?
Cl1 Pb1 Cl2 173.31(7) 6_557 . ?
Cl1 Pb1 Cl1 83.381(8) 6_557 . ?
Pb1 Cl2 Pb1 157.85(11) 6_656 . ?
C1 N2 H2 124.2 . . ?
C1 N2 N3 111.6(5) . . ?
N3 N2 H2 124.2 . . ?
C1 N1 H1 126.6 . . ?
C1 N1 C2 106.9(5) . . ?
C2 N1 H1 126.6 . . ?
N2 C1 N1 107.1(6) . . ?
N2 C1 H1A 126.5 . . ?
N1 C1 H1A 126.5 . . ?
N1 C2 H2A 124.4 . . ?
N3 C2 N1 111.1(6) . . ?
N3 C2 H2A 124.4 . . ?
C2 N3 N2 103.3(5) . . ?
Pb1 Cl1 Pb1 172.74(10) 6_657 . ?

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 -1.2(8) . . . . ?
C1 N2 N3 C2 0.5(8) . . . . ?
C1 N1 C2 N3 1.5(9) . . . . ?
C2 N1 C1 N2 -1.1(8) . . . . ?
N3 N2 C1 N1 0.4(8) . . . . ?

_shelx_res_file                  
;
TITL triag2pbcl4_300b_a.res in Pnma
    triag2pbcl4_iii_300_00.res
    created by SHELXL-2018/3 at 13:11:08 on 15-Dec-2023
REM Old TITL TRIAG2PbCl4_300b in Pnma
REM SHELXT solution in Pnma: R1 0.100, Rweak 0.006, Alpha 0.037
REM <I/s> 1.671 for 218 systematic absences, Orientation as input
REM Formula found by SHELXT: C7 N4 Cl4 Pb
CELL 0.71073 7.4929 21.5667 8.3106 90 90 90
ZERR 4 0.0003 0.001 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
TEMP 27
CONF
list 4
MORE -1
BOND $H
fmap 2 53
acta 50
OMIT 0 0 2
OMIT 0 0 4
OMIT 0 1 1
OMIT 0 2 4
OMIT 0 3 1
OMIT 0 4 0
OMIT 0 5 1
OMIT 0 7 1
OMIT 0 8 0
OMIT 0 10 0
OMIT 1 0 3
OMIT 1 1 3
OMIT 1 1 5
OMIT 3 0 5
OMIT 3 0 10
OMIT 5 6 1
OMIT 8 0 2
OMIT 8 2 0
OMIT 8 4 2
OMIT 8 4 4
OMIT 8 6 2
OMIT 8 8 2
REM <olex2.extras>
REM <HklSrc "%.\\TRIAG2PbCl4_III_300_00.hkl">
REM </olex2.extras>

WGHT    0.024800    3.349200
EXTI    0.019127
FVAR       2.97348
PB1   5    0.344527    0.250000    0.497237    10.50000    0.02267    0.03392 =
         0.01860    0.00000   -0.00049    0.00000
CL3   3    0.339422    0.117337    0.494524    11.00000    0.09239    0.03563 =
         0.02944    0.00075   -0.00106   -0.00189
CL2   3    0.543081    0.250000    0.203664    10.50000    0.05270    0.08608 =
         0.04878    0.00000    0.02850    0.00000
N2    4    0.834749    0.104831    0.385697    11.00000    0.07141    0.04771 =
         0.03632    0.00932    0.00579   -0.00358
AFIX  43
H2    2    0.851018    0.122542    0.294150    11.00000    0.07275
AFIX   0
N1    4    0.816530    0.091851    0.633742    11.00000    0.06986    0.06552 =
         0.02626   -0.01072    0.00230   -0.00193
AFIX  43
H1    2    0.818649    0.097804    0.736047    11.00000    0.07663
AFIX   0
C1    1    0.848829    0.132745    0.523214    11.00000    0.06269    0.05078 =
         0.05075   -0.00989    0.01133   -0.00979
AFIX  43
H1A   2    0.876827    0.174283    0.539518    11.00000    0.06756
AFIX   0
C2    1    0.779303    0.038666    0.558331    11.00000    0.11818    0.05033 =
         0.03534    0.00678    0.00797   -0.00001
AFIX  43
H2A   2    0.748531    0.001960    0.610093    11.00000    0.09661
AFIX   0
N3    4    0.791673    0.044922    0.403924    11.00000    0.12124    0.05064 =
         0.03510   -0.00524    0.00487   -0.00888

CL1   3    0.614714    0.250000    0.738147    10.50000    0.04222    0.08479 =
         0.04171    0.00000   -0.02044    0.00000
HKLF 4




REM  triag2pbcl4_300b_a.res in Pnma
REM wR2 = 0.0656, GooF = S = 1.114, Restrained GooF = 1.114 for all data
REM R1 = 0.0275 for 1299 Fo > 4sig(Fo) and 0.0381 for all 1675 data
REM 78 parameters refined using 0 restraints

END

WGHT      0.0246      3.3953

REM Highest difference peak  1.214,  deepest hole -1.129,  1-sigma level  0.141
Q1    1   0.3430  0.2500  0.3940  10.50000  0.05    1.21
Q2    1   0.3531  0.2500  0.5983  10.50000  0.05    1.18
;
_shelx_res_checksum              24063
_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
;
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_triag2pbcl4_iii_320_00
_database_code_depnum_ccdc_archive 'CCDC 2314663'
loop_
_audit_author_name
_audit_author_address
'Szymon Sobczak'
;Department of Materials Chemistry, Adam Mickiewicz University
Poland
;
_audit_update_record             
;
2024-03-04 deposited with the CCDC.	2024-03-21 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT027_triag2pbcl4_iii_320_00 
;
PROBLEM: _diffrn_reflns_theta_full value (too) Low ......      20.00 Degree
RESPONSE: This data comes from high-temperature measurements which inflicted the data quality
;
# Added during the CSD deposition process: Friday 15 December 2023 12:43 PM
# end Validation Reply Form

_audit_creation_date             2023-12-15
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        Tz2PbCl4
_chemical_formula_moiety         'Cl4 Pb, 2(C2 H4 N3)'
_chemical_formula_sum            'C4 H8 Cl4 N6 Pb'
_chemical_formula_weight         489.15
_chemical_melting_point          ?
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'

_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.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x, y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z-1/2'
'x, -y-1/2, z'

_cell_length_a                   7.5195(2)
_cell_length_b                   21.5921(7)
_cell_length_c                   8.3020(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1347.93(7)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    7754
_cell_measurement_temperature    320.01(10)
_cell_measurement_theta_max      28.8260
_cell_measurement_theta_min      2.7170
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_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_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.410
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             896
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-10 -9 0 0.1475
10 9 0 0.1131
-3 29 0 0.0805
0 0 -12 0.2988
3 -29 0 0.0541
8 8 6 0.1664
-8 -8 -7 0.2105
-2 11 11 0.2718
7 2 -9 0.2378
-7 -2 9 0.2672

_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
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_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
_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  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω      4.00  30.00   1.00    5.00    --   17.79-130.00 -16.00   26
  2  ω    -84.00 -58.00   1.00    5.00    --  -18.72 138.00-129.00   26
  3  ω    -41.00 -15.00   1.00    5.00    --  -18.72 138.00-129.00   26
  4  ω    -65.00 -40.00   1.00    5.00    --  -18.72 130.00  55.00   25
  5  ω     41.00  94.00   1.00    5.00    --   17.79 178.00  90.00   53
  6  ω    -48.00  34.00   1.00    5.00    --   17.79 -57.00 150.00   82
  7  ω    -47.00  38.00   1.00    5.00    --   17.79 -57.00  60.00   85
  8  ω    -12.00  39.00   1.00    5.00    --   17.79  77.00  30.00   51
  9  ω     47.00  77.00   1.00    5.00    --   17.79-138.00 168.00   30
 10  ω    -35.00  -9.00   1.00    5.00    --  -18.72 -57.00  90.00   26
 11  ω    -88.00 -62.00   1.00    5.00    --  -18.72 -57.00  90.00   26
 12  ω    -90.00   6.00   1.00    5.00    --  -18.72 -37.00   0.00   96
 13  ω    -86.00 -12.00   1.00    5.00    --  -18.72 140.00-171.91   74
 14  ω    -26.00   3.00   1.00    5.00    --  -18.72 -57.00 120.00   29
 15  ω    -88.00 -37.00   1.00    5.00    --  -18.72 -57.00 120.00   51
 16  ω    -90.00   6.00   1.00    5.00    --  -18.72 -37.00 150.00   96
 17  ω    -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       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1180
_reflns_number_total             1768
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_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)'
_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+0.001xFc²λ³/sin(2θ)]^-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_R_factor_all          0.0496
_refine_ls_R_factor_gt           0.0266
_refine_ls_restrained_S_all      1.118
_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)+(0.0125P)²+2.0635P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0462
_refine_ls_wR_factor_ref         0.0515
_refine_special_details          ?
_olex2_refinement_description    
;
1.a Aromatic/amide H refined with riding coordinates:
 N2(H2), N1(H1), C1(H1A), C2(H2A)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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 0.33757(3) 0.250000 0.49791(3) 0.02856(10) Uani 1 2 d S T P . .
Cl3 Cl 0.3327(2) 0.11751(6) 0.49605(15) 0.0587(4) Uani 1 1 d . . . . .
Cl2 Cl 0.5410(3) 0.250000 0.2079(3) 0.0710(7) Uani 1 2 d S T P . .
N2 N 0.8273(7) 0.1049(3) 0.3835(6) 0.0621(15) Uani 1 1 d . . . . .
H2 H 0.841465 0.122313 0.291238 0.10(3) Uiso 1 1 calc R . . . .
N1 N 0.8098(7) 0.0923(3) 0.6314(6) 0.0603(15) Uani 1 1 d . . . . .
H1 H 0.810333 0.098562 0.733742 0.08(2) Uiso 1 1 calc R . . . .
C1 C 0.8417(8) 0.1335(3) 0.5207(7) 0.0618(17) Uani 1 1 d . . . . .
H1A H 0.869354 0.175008 0.536476 0.058(18) Uiso 1 1 calc R . . . .
C2 C 0.7761(11) 0.0385(4) 0.5571(7) 0.073(2) Uani 1 1 d . . . . .
H2A H 0.748225 0.001602 0.609111 0.13(3) Uiso 1 1 calc R . . . .
N3 N 0.7876(8) 0.0451(3) 0.4037(6) 0.0757(18) Uani 1 1 d . . . . .
Cl1 Cl 0.6061(3) 0.250000 0.7390(2) 0.0643(6) 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 0.02946(14) 0.03679(16) 0.01944(13) 0.000 -0.00046(12) 0.000
Cl3 0.1062(12) 0.0390(7) 0.0309(6) 0.0002(6) -0.0014(8) -0.0019(7)
Cl2 0.0630(14) 0.0960(19) 0.0541(12) 0.000 0.0346(11) 0.000
N2 0.093(5) 0.055(4) 0.038(3) 0.005(3) 0.012(3) -0.004(3)
N1 0.080(4) 0.072(4) 0.028(2) -0.008(3) 0.002(2) 0.001(3)
C1 0.075(4) 0.052(4) 0.059(4) -0.011(4) 0.009(3) -0.013(3)
C2 0.126(7) 0.052(5) 0.040(3) 0.004(3) 0.011(4) -0.003(4)
N3 0.139(6) 0.051(4) 0.038(3) -0.003(3) 0.002(3) -0.011(4)
Cl1 0.0528(12) 0.0940(19) 0.0460(11) 0.000 -0.0253(10) 0.000

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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 2.8611(14) 8_565 ?
Pb1 Cl3 2.8611(14) . ?
Pb1 Cl2 2.8094(19) 6_556 ?
Pb1 Cl2 2.8526(18) . ?
Pb1 Cl1 2.7929(18) 6_557 ?
Pb1 Cl1 2.8430(18) . ?
N2 H2 0.8600 . ?
N2 C1 1.300(7) . ?
N2 N3 1.335(7) . ?
N1 H1 0.8600 . ?
N1 C1 1.300(7) . ?
N1 C2 1.341(8) . ?
C1 H1A 0.9300 . ?
C2 H2A 0.9300 . ?
C2 N3 1.284(8) . ?

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 178.40(7) . 8_565 ?
Cl2 Pb1 Cl3 89.23(3) 6_556 8_565 ?
Cl2 Pb1 Cl3 90.13(3) . 8_565 ?
Cl2 Pb1 Cl3 90.13(3) . . ?
Cl2 Pb1 Cl3 89.23(3) 6_556 . ?
Cl2 Pb1 Cl2 84.970(14) 6_556 . ?
Cl2 Pb1 Cl1 172.71(7) 6_556 . ?
Cl1 Pb1 Cl3 90.74(3) . 8_565 ?
Cl1 Pb1 Cl3 89.78(3) 6_557 . ?
Cl1 Pb1 Cl3 90.74(3) . . ?
Cl1 Pb1 Cl3 89.78(3) 6_557 8_565 ?
Cl1 Pb1 Cl2 88.90(7) 6_557 6_556 ?
Cl1 Pb1 Cl2 102.32(7) . . ?
Cl1 Pb1 Cl2 173.87(7) 6_557 . ?
Cl1 Pb1 Cl1 83.804(8) 6_557 . ?
Pb1 Cl2 Pb1 159.89(10) 6_656 . ?
C1 N2 H2 124.2 . . ?
C1 N2 N3 111.6(5) . . ?
N3 N2 H2 124.2 . . ?
C1 N1 H1 126.2 . . ?
C1 N1 C2 107.5(5) . . ?
C2 N1 H1 126.2 . . ?
N2 C1 N1 106.3(6) . . ?
N2 C1 H1A 126.9 . . ?
N1 C1 H1A 126.9 . . ?
N1 C2 H2A 124.8 . . ?
N3 C2 N1 110.3(6) . . ?
N3 C2 H2A 124.8 . . ?
C2 N3 N2 104.3(6) . . ?
Pb1 Cl1 Pb1 173.31(9) 6_657 . ?

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 -0.8(8) . . . . ?
C1 N2 N3 C2 0.9(8) . . . . ?
C1 N1 C2 N3 0.5(9) . . . . ?
C2 N1 C1 N2 0.0(8) . . . . ?
N3 N2 C1 N1 -0.6(8) . . . . ?

_shelx_res_file                  
;
TITL TRIAG2PbCl4_320_00 in Pnma #62
    triag2pbcl4_iii_320_00.res
    created by SHELXL-2018/3 at 13:10:14 on 15-Dec-2023
CELL 0.71073 7.5195 21.5921 8.302 90 90 90
ZERR 4 0.0002 0.0007 0.0002 0 0 0
LATT 1
SYMM 0.5-X,-Y,0.5+Z
SYMM 0.5+X,0.5-Y,0.5-Z
SYMM -X,0.5+Y,-Z
SFAC C H Cl N Pb
UNIT 16 32 16 24 4

L.S. 44
PLAN  2
TEMP 47
CONF
MORE -1
BOND $H
fmap 2
acta 40
OMIT 0 0 2
OMIT 0 0 4
OMIT 0 1 1
OMIT 0 2 4
OMIT 0 3 1
OMIT 0 5 1
OMIT 0 7 1
OMIT 0 10 0
OMIT 0 14 0
OMIT 3 1 3
OMIT 3 3 1
OMIT 3 7 1
OMIT 3 7 3
REM <olex2.extras>
REM <HklSrc "%.\\TRIAG2PbCl4_III_320_00.hkl">
REM </olex2.extras>

WGHT    0.012500    2.063500
EXTI    0.001664
FVAR       2.18835
PB1   5    0.337573    0.250000    0.497912    10.50000    0.02946    0.03679 =
         0.01944    0.00000   -0.00046    0.00000
CL3   3    0.332674    0.117506    0.496047    11.00000    0.10619    0.03896 =
         0.03092    0.00017   -0.00142   -0.00191
CL2   3    0.540999    0.250000    0.207893    10.50000    0.06296    0.09605 =
         0.05406    0.00000    0.03463    0.00000
N2    4    0.827273    0.104891    0.383501    11.00000    0.09298    0.05480 =
         0.03847    0.00548    0.01180   -0.00449
AFIX  43
H2    2    0.841465    0.122313    0.291238    11.00000    0.09657
AFIX   0
N1    4    0.809844    0.092345    0.631423    11.00000    0.08027    0.07227 =
         0.02849   -0.00828    0.00155    0.00132
AFIX  43
H1    2    0.810333    0.098562    0.733742    11.00000    0.07815
AFIX   0
C1    1    0.841731    0.133466    0.520682    11.00000    0.07495    0.05197 =
         0.05859   -0.01120    0.00887   -0.01317
AFIX  43
H1A   2    0.869354    0.175008    0.536476    11.00000    0.05848
AFIX   0
C2    1    0.776063    0.038487    0.557051    11.00000    0.12621    0.05183 =
         0.03961    0.00373    0.01129   -0.00286
AFIX  43
H2A   2    0.748225    0.001602    0.609111    11.00000    0.12647
AFIX   0
N3    4    0.787633    0.045104    0.403700    11.00000    0.13866    0.05100 =
         0.03755   -0.00346    0.00215   -0.01058

CL1   3    0.606070    0.250000    0.739015    10.50000    0.05278    0.09402 =
         0.04603    0.00000   -0.02527    0.00000
HKLF 4




REM  TRIAG2PbCl4_320_00 in Pnma #62
REM wR2 = 0.0515, GooF = S = 1.118, Restrained GooF = 1.118 for all data
REM R1 = 0.0266 for 1180 Fo > 4sig(Fo) and 0.0496 for all 1768 data
REM 78 parameters refined using 0 restraints

END

WGHT      0.0125      2.0598

REM Highest difference peak  1.590,  deepest hole -1.113,  1-sigma level  0.140
Q1    1   0.7025  0.2500  0.4989  10.50000  0.05    1.59
Q2    1   0.5528  0.2500  0.0044  10.50000  0.05    1.36
;
_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
;
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_triag2pbcl4_ii_360_00
_database_code_depnum_ccdc_archive 'CCDC 2314665'
loop_
_audit_author_name
_audit_author_address
'Szymon Sobczak'
;Department of Materials Chemistry, Adam Mickiewicz University
Poland
;
_audit_update_record             
;
2024-03-04 deposited with the CCDC.	2024-03-21 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT110_triag2pbcl4_ii_360_00 
;
PROBLEM: ADDSYM Detects Potential Lattice Translation ...          ? Check
RESPONSE: The symmetry has been thoroughly inspected by the presence of systematic absences in the raw diffraction data
;
_vrf_PLAT112_triag2pbcl4_ii_360_00 
;
PROBLEM: ADDSYM Detects New (Pseudo) Symm. Elem         A        100 %Fit
RESPONSE: Look PLAT110
;
_vrf_PLAT113_triag2pbcl4_ii_360_00 
;
PROBLEM: ADDSYM Suggests Possible Pseudo/New  Space Group       Fmmm Check
RESPONSE: Look PLAT110
;
# Added during the CSD deposition process: Friday 15 December 2023 12:43 PM
# end Validation Reply Form

_audit_creation_date             2023-12-15
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        Tz2PbCl4
_chemical_formula_moiety         'Cl4 Pb, 2(C2 H4 N3)'
_chemical_formula_sum            'C4 H8 Cl4 N6 Pb'
_chemical_formula_weight         489.15
_chemical_melting_point          ?
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'

_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.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           63
_space_group_name_H-M_alt        'C m c m'
_space_group_name_Hall           '-C 2c 2'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'-x, y, -z+1/2'
'x, -y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x, y, -z-1/2'
'x, -y, z-1/2'
'-x, y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, y+1/2, -z-1/2'
'x+1/2, -y+1/2, z-1/2'
'-x+1/2, y+1/2, z'

_cell_length_a                   8.2929(2)
_cell_length_b                   7.5535(2)
_cell_length_c                   21.7496(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1362.40(7)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    5391
_cell_measurement_temperature    360.01(10)
_cell_measurement_theta_max      28.7730
_cell_measurement_theta_min      2.8120
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    13.148
_exptl_absorpt_correction_T_max  0.194
_exptl_absorpt_correction_T_min  0.041
_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_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.385
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             896
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 -10 11 0.1475
0 10 -11 0.1131
0 -4 -29 0.0805
12 0 0 0.2988
0 4 29 0.0541
-6 8 -10 0.1664
7 -8 9 0.2105
-11 -2 -11 0.2718
9 6 -4 0.2378
-9 -7 4 0.2672

_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0598
_diffrn_reflns_av_unetI/netI     0.0280
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.955
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            11518
_diffrn_reflns_point_group_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.955
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         29.073
_diffrn_reflns_theta_min         3.747
_diffrn_ambient_temperature      360.15
_diffrn_detector_area_resol_mean 16.1544
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.955
_diffrn_measurement_details      .
_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_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                729
_reflns_number_total             957
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_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  (Sheldrick, 2015)'
_refine_diff_density_max         0.773
_refine_diff_density_min         -1.031
_refine_diff_density_rms         0.130
_refine_ls_extinction_coef       0.00153(12)
_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   1.131
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     43
_refine_ls_number_reflns         957
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0369
_refine_ls_R_factor_gt           0.0233
_refine_ls_restrained_S_all      1.131
_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)+(0.0169P)²+1.5397P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0459
_refine_ls_wR_factor_ref         0.0502
_refine_special_details          ?
_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. Others
 Fixed Sof: H1A(0.5) H1B(0.5) C2(0.5) H2(0.5) N2(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 N1(H1A), N1(H1B), C2(H2), C1(H1)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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 0.24600(3) 0.250000 0.03021(14) Uani 1 4 d S T P . .
Cl2 Cl 0.500000 0.2469(3) 0.11864(9) 0.0682(6) Uani 1 2 d S T P . .
Cl1 Cl 0.7495(3) 0.4969(2) 0.250000 0.0855(7) Uani 1 2 d S T P . .
N1 N 0.1238(5) 0.2465(6) 0.1013(3) 0.0756(15) Uani 1 1 d . . . . .
H1A H 0.222412 0.246226 0.113549 0.091 Uiso 0.5 1 calc R U P A 9
H1B H 0.222412 0.246226 0.113549 0.091 Uiso 0.5 1 calc R U P B 10
C2 C 0.0772(9) 0.2475(9) 0.0437(3) 0.119(3) Uani 0.5 1 d . . P C 9
H2 H 0.143767 0.248147 0.009292 0.142 Uiso 0.5 1 calc R U P C 9
C1 C 0.000000 0.2459(9) 0.1364(4) 0.071(2) Uani 1 2 d S T P C .
H1 H 0.000001 0.245281 0.179200 0.14(6) Uiso 1 2 calc R . P . .
N2 N 0.0772(9) 0.2475(9) 0.0437(3) 0.119(3) Uani 0.5 1 d . . P C 10

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 0.02052(16) 0.03220(18) 0.0379(2) 0.000 0.000 0.000
Cl2 0.0339(8) 0.1291(18) 0.0418(9) 0.0002(10) 0.000 0.000
Cl1 0.0715(13) 0.0791(13) 0.1059(18) 0.000 0.000 -0.0493(12)
N1 0.036(2) 0.109(4) 0.082(4) 0.000(3) -0.011(2) -0.004(2)
C2 0.084(4) 0.213(9) 0.059(4) -0.004(4) 0.020(3) 0.001(4)
C1 0.067(5) 0.097(6) 0.051(5) -0.001(4) 0.000 0.000
N2 0.084(4) 0.213(9) 0.059(4) -0.004(4) 0.020(3) 0.001(4)

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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 2.8572(19) 10_556 ?
Pb1 Cl2 2.8571(19) . ?
Pb1 Cl1 2.8031(17) 5_445 ?
Pb1 Cl1 2.8031(17) 7_645 ?
Pb1 Cl1 2.8056(16) 3_655 ?
Pb1 Cl1 2.8056(17) . ?
N1 H1A 0.8600 . ?
N1 H1B 0.8600 . ?
N1 C2 1.311(9) . ?
N1 C1 1.280(7) . ?
N1 N2 1.311(9) . ?
C2 C2 1.280(14) 12 ?
C2 H2 0.9300 . ?
C1 H1 0.9300 . ?

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 179.71(8) . 10_556 ?
Cl1 Pb1 Cl2 90.10(3) 5_445 10_556 ?
Cl1 Pb1 Cl2 90.10(3) 5_445 . ?
Cl1 Pb1 Cl2 90.10(3) 7_645 . ?
Cl1 Pb1 Cl2 90.10(3) 7_645 10_556 ?
Cl1 Pb1 Cl2 89.90(3) 3_655 10_556 ?
Cl1 Pb1 Cl2 89.90(3) 3_655 . ?
Cl1 Pb1 Cl2 89.90(3) . . ?
Cl1 Pb1 Cl2 89.90(3) . 10_556 ?
Cl1 Pb1 Cl1 179.69(10) 5_445 . ?
Cl1 Pb1 Cl1 179.69(10) 7_645 3_655 ?
Cl1 Pb1 Cl1 84.657(2) 5_445 3_655 ?
Cl1 Pb1 Cl1 84.656(2) 7_645 . ?
Cl1 Pb1 Cl1 95.03(10) 3_655 . ?
Cl1 Pb1 Cl1 95.65(10) 5_445 7_645 ?
Pb1 Cl1 Pb1 179.69(10) 5 . ?
C2 N1 H1A 125.2 . . ?
C1 N1 H1A 125.2 . . ?
C1 N1 H1B 125.2 . . ?
C1 N1 C2 109.5(6) . . ?
C1 N1 N2 109.5(6) . . ?
N2 N1 H1B 125.2 . . ?
N1 C2 H2 126.4 . . ?
C2 C2 N1 107.2(4) 12 . ?
C2 C2 H2 126.4 12 . ?
N1 C1 N1 106.6(8) . 12 ?
N1 C1 H1 126.7 . . ?
N1 C1 H1 126.7 12 . ?

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
C2 N1 C1 N1 0.0(9) . . . 12 ?
C1 N1 C2 C2 0.0(6) . . . 12 ?
N2 N1 C1 N1 0.0(9) . . . 12 ?

_shelx_res_file                  
;
TITL triag2pbcl4_360_00_a.res in Cmcm
    triag2pbcl4_ii_360_00.res
    created by SHELXL-2018/3 at 13:08:17 on 15-Dec-2023
REM Old TITL TRIAG2PbCl4_360_00 in Cmcm
REM SHELXT solution in Cmcm: R1 0.103, Rweak 0.074, Alpha 0.010
REM <I/s> 2.360 for 63 systematic absences, Orientation as input
REM Formula found by SHELXT: C2 N4 Cl4 Pb
CELL 0.71073 8.2929 7.5535 21.7496 90 90 90
ZERR 4 0.0002 0.0002 0.0007 0 0 0
LATT 7
SYMM -X,-Y,0.5+Z
SYMM -X,+Y,0.5-Z
SYMM +X,-Y,-Z
SFAC C H Cl N Pb
UNIT 16 32 16 24 4
EADP C2 N2
EXYZ C2 N2

L.S. 44
PLAN  1
TEMP 87
CONF
list 4
MORE -1
BOND $H
fmap 2 53
acta 50
OMIT 0 0 6
OMIT 0 0 10
OMIT 0 0 16
OMIT 0 2 3
OMIT 1 1 0
OMIT 1 1 2
OMIT 1 1 4
OMIT 1 1 7
OMIT 2 0 0
OMIT 3 1 0
OMIT 3 1 4
OMIT 4 0 0
REM <olex2.extras>
REM <HklSrc "%.\\TRIAG2PbCl4_II_360_00.hkl">
REM </olex2.extras>

WGHT    0.016900    1.539700
EXTI    0.001532
FVAR       2.17665
PB1   5    0.500000    0.245998    0.250000    10.25000    0.02052    0.03220 =
         0.03791    0.00000    0.00000    0.00000
CL2   3    0.500000    0.246948    0.118636    10.50000    0.03392    0.12906 =
         0.04177    0.00020    0.00000    0.00000
CL1   3    0.749503    0.496850    0.250000    10.50000    0.07153    0.07914 =
         0.10595    0.00000    0.00000   -0.04925
N1    4    0.123829    0.246495    0.101278    11.00000    0.03627    0.10881 =
         0.08168    0.00008   -0.01120   -0.00371
PART 9
AFIX  43
H1A   2    0.222412    0.246226    0.113549    10.50000   -1.20000
AFIX  43
PART 10
H1B   2    0.222412    0.246226    0.113549    10.50000   -1.20000
AFIX   0
PART 9
C2    1    0.077190    0.247529    0.043700    10.50000    0.08384    0.21312 =
         0.05865   -0.00447    0.02015    0.00119
AFIX  43
H2    2    0.143767    0.248147    0.009292    10.50000   -1.20000
AFIX   0
PART 0
C1    1    0.000000    0.245947    0.136441    10.50000    0.06659    0.09661 =
         0.05072   -0.00106    0.00000    0.00000
AFIX  43
H1    2    0.000001    0.245281    0.179200    10.50000    0.14104
AFIX   0
PART 10
N2    4    0.077190    0.247529    0.043700    10.50000    0.08384    0.21312 =
         0.05865   -0.00447    0.02015    0.00119
HKLF 4




REM  triag2pbcl4_360_00_a.res in Cmcm
REM wR2 = 0.0502, GooF = S = 1.131, Restrained GooF = 1.131 for all data
REM R1 = 0.0233 for 729 Fo > 4sig(Fo) and 0.0369 for all 957 data
REM 43 parameters refined using 0 restraints

END

WGHT      0.0169      1.5284

REM Highest difference peak  0.773,  deepest hole -1.031,  1-sigma level  0.130
Q1    1   0.5000  0.3482  0.2500  10.25000  0.05    0.77
;
_shelx_res_checksum              44810
_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
;
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_triag2pbcl4_340a
_database_code_depnum_ccdc_archive 'CCDC 2314664'
loop_
_audit_author_name
_audit_author_address
'Szymon Sobczak'
;Department of Materials Chemistry, Adam Mickiewicz University
Poland
;
_audit_update_record             
;
2024-03-04 deposited with the CCDC.	2024-03-21 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT110_triag2pbcl4_340a    
;
PROBLEM: ADDSYM Detects Potential Lattice Translation ...          ? Check
RESPONSE: The symmetry has been thoroughly inspected by the presence of systematic absences in the raw diffraction data
;
_vrf_PLAT112_triag2pbcl4_340a    
;
PROBLEM: ADDSYM Detects New (Pseudo) Symm. Elem         A        100 %Fit
RESPONSE: Look PLAT110
;
_vrf_PLAT113_triag2pbcl4_340a    
;
PROBLEM: ADDSYM Suggests Possible Pseudo/New  Space Group       Fmmm Check
RESPONSE: Look PLAT110
;
# Added during the CSD deposition process: Friday 15 December 2023 12:43 PM
# end Validation Reply Form

_audit_creation_date             2023-12-15
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        Tz2PbCl4
_chemical_formula_moiety         'Cl4 Pb, 2(C2 H4 N3)'
_chemical_formula_sum            'C4 H8 Cl4 N6 Pb'
_chemical_formula_weight         489.15
_chemical_melting_point          ?
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'

_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.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           63
_space_group_name_H-M_alt        'C m c m'
_space_group_name_Hall           '-C 2c 2'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'-x, y, -z+1/2'
'x, -y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x, y, -z-1/2'
'x, -y, z-1/2'
'-x, y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, y+1/2, -z-1/2'
'x+1/2, -y+1/2, z-1/2'
'-x+1/2, y+1/2, z'

_cell_length_a                   8.2959(15)
_cell_length_b                   7.4918(15)
_cell_length_c                   21.829(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1356.7(5)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    2933
_cell_measurement_temperature    340.00(10)
_cell_measurement_theta_max      28.7340
_cell_measurement_theta_min      2.7760
_shelx_estimated_absorpt_T_max   0.300
_shelx_estimated_absorpt_T_min   0.051
_exptl_absorpt_coefficient_mu    13.203
_exptl_absorpt_correction_T_max  0.255
_exptl_absorpt_correction_T_min  0.059
_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_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.395
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             896
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
7 -8 1 0.0869
7 8 0 0.0832
1 11 -1 0.0738
-12 1 -1 0.4117
0 -11 1 0.0824
12 -1 -2 0.1383
1 0 -31 0.0656
0 0 31 0.0459

_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0512
_diffrn_reflns_av_unetI/netI     0.0280
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.918
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            7067
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.918
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         28.889
_diffrn_reflns_theta_min         3.782
_diffrn_ambient_temperature      340.15
_diffrn_detector_area_resol_mean 8.0772
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.918
_diffrn_measurement_details      .
_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_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                765
_reflns_number_total             905
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_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  (Sheldrick, 2015)'
_refine_diff_density_max         0.929
_refine_diff_density_min         -2.164
_refine_diff_density_rms         0.200
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.151
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     44
_refine_ls_number_reflns         905
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0429
_refine_ls_R_factor_gt           0.0343
_refine_ls_restrained_S_all      1.151
_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)+(0.0415P)²+9.5938P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0831
_refine_ls_wR_factor_ref         0.0913
_refine_special_details          ?
_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. Others
 Fixed Sof: H1A(0.5) H1B(0.5) C2(0.5) H2(0.5) N2(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 N1(H1A), N1(H1B), C2(H2), C1(H1)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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 0.24490(5) 0.250000 0.0262(6) Uani 1 4 d S T P . .
Cl2 Cl 0.500000 0.2447(4) 0.11861(14) 0.0657(12) Uani 1 2 d S T P . .
Cl1 Cl 0.7496(4) 0.4946(4) 0.250000 0.0851(14) Uani 1 2 d S T P . .
N1 N 0.1241(10) 0.2444(9) 0.1017(5) 0.076(3) Uani 1 1 d . . . . .
H1A H 0.222530 0.246236 0.114005 0.092 Uiso 0.5 1 calc R U P A 11
H1B H 0.222530 0.246236 0.114005 0.092 Uiso 0.5 1 calc R U P B 12
C2 C 0.080(2) 0.2427(17) 0.0445(6) 0.142(8) Uani 0.5 1 d . . P C 11
H2 H 0.147158 0.241656 0.010353 0.170 Uiso 0.5 1 calc R U P C 11
C1 C 0.000000 0.2431(16) 0.1374(7) 0.070(4) Uani 1 2 d S T P C .
H1 H 0.000000 0.241437 0.180032 0.7(9) Uiso 1 2 calc R . P . .
N2 N 0.080(2) 0.2427(17) 0.0445(6) 0.142(8) Uani 0.5 1 d . . P C 12

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 0.0195(6) 0.0241(6) 0.0349(6) 0.000 0.000 0.000
Cl2 0.0344(15) 0.124(4) 0.0389(15) 0.0005(12) 0.000 0.000
Cl1 0.073(3) 0.075(3) 0.107(3) 0.000 0.000 -0.054(2)
N1 0.035(4) 0.112(9) 0.082(6) 0.004(4) -0.013(4) -0.004(3)
C2 0.083(9) 0.29(3) 0.053(6) -0.005(7) 0.023(6) 0.000(7)
C1 0.066(10) 0.090(12) 0.052(8) 0.003(5) 0.000 0.000
N2 0.083(9) 0.29(3) 0.053(6) -0.005(7) 0.023(6) 0.000(7)

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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 2.868(3) 10_556 ?
Pb1 Cl2 2.868(3) . ?
Pb1 Cl1 2.790(2) 3_655 ?
Pb1 Cl1 2.790(2) . ?
Pb1 Cl1 2.799(2) 5_445 ?
Pb1 Cl1 2.799(2) 7_645 ?
N1 H1A 0.8600 . ?
N1 H1B 0.8600 . ?
N1 C2 1.302(17) . ?
N1 C1 1.292(13) . ?
N1 N2 1.302(17) . ?
C2 C2 1.33(3) 12 ?
C2 H2 0.9300 . ?
C1 H1 0.9300 . ?

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 179.94(12) . 10_556 ?
Cl1 Pb1 Cl2 90.02(4) 3_655 10_556 ?
Cl1 Pb1 Cl2 90.02(4) 3_655 . ?
Cl1 Pb1 Cl2 90.02(4) . . ?
Cl1 Pb1 Cl2 90.02(4) . 10_556 ?
Cl1 Pb1 Cl2 89.98(4) 5_445 10_556 ?
Cl1 Pb1 Cl2 89.98(4) 5_445 . ?
Cl1 Pb1 Cl2 89.98(4) 7_645 . ?
Cl1 Pb1 Cl2 89.98(4) 7_645 10_556 ?
Cl1 Pb1 Cl1 179.97(15) 3_655 7_645 ?
Cl1 Pb1 Cl1 179.97(15) . 5_445 ?
Cl1 Pb1 Cl1 84.169(16) 3_655 5_445 ?
Cl1 Pb1 Cl1 84.169(15) . 7_645 ?
Cl1 Pb1 Cl1 95.86(15) 5_445 7_645 ?
Cl1 Pb1 Cl1 95.80(15) 3_655 . ?
Pb1 Cl1 Pb1 179.97(15) . 5 ?
C2 N1 H1A 124.6 . . ?
C1 N1 H1A 124.6 . . ?
C1 N1 H1B 124.6 . . ?
C1 N1 C2 110.8(11) . . ?
C1 N1 N2 110.8(11) . . ?
N2 N1 H1B 124.6 . . ?
N1 C2 C2 106.3(8) . 12 ?
N1 C2 H2 126.8 . . ?
C2 C2 H2 126.8 12 . ?
N1 C1 N1 105.7(14) . 12 ?
N1 C1 H1 127.2 . . ?
N1 C1 H1 127.2 12 . ?

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
C2 N1 C1 N1 -1.4(14) . . . 12 ?
C1 N1 C2 C2 0.9(9) . . . 12 ?
N2 N1 C1 N1 -1.4(14) . . . 12 ?

_shelx_res_file                  
;
TITL triag2pbcl4_340a_a.res in Cmcm
    triag2pbcl4_340a.res
    created by SHELXL-2018/3 at 13:08:43 on 15-Dec-2023
REM Old TITL TRIAG2PbCl4_340a in Cmcm
REM SHELXT solution in Cmcm: R1 0.107, Rweak 0.034, Alpha 0.009
REM <I/s> 2.044 for 63 systematic absences, Orientation as input
REM Formula found by SHELXT: C2 N4 Cl4 Pb
CELL 0.71073 8.2959 7.4918 21.8291 90 90 90
ZERR 4 0.0015 0.0015 0.0058 0 0 0
LATT 7
SYMM -X,-Y,0.5+Z
SYMM -X,+Y,0.5-Z
SYMM +X,-Y,-Z
SFAC C H Cl N Pb
UNIT 16 32 16 24 4
EADP C2 N2
EXYZ C2 N2

L.S. 44
PLAN  1
SIZE 0.12 0.18 0.56
TEMP 67
CONF
list 4
MORE -1
BOND $H
fmap 2 53
acta 50
OMIT 0 0 4
OMIT 0 0 6
OMIT 0 10 1
OMIT 1 1 0
OMIT 1 1 4
OMIT 2 0 0
OMIT 2 2 0
OMIT 3 1 1
OMIT 4 0 0
OMIT 4 0 2
OMIT 5 1 1
OMIT 6 2 0
OMIT 7 7 8
REM <olex2.extras>
REM <HklSrc "%.\\triag2pbcl4_340a.hkl">
REM </olex2.extras>

WGHT    0.041500    9.593801
SWAT    0.217481    0.1793
FVAR       2.86304
PB1   5    0.500000    0.244898    0.250000    10.25000    0.01946    0.02413 =
         0.03487    0.00000    0.00000    0.00000
CL2   3    0.500000    0.244711    0.118611    10.50000    0.03438    0.12389 =
         0.03895    0.00051    0.00000    0.00000
CL1   3    0.749580    0.494604    0.250000    10.50000    0.07335    0.07471 =
         0.10730    0.00000    0.00000   -0.05363
N1    4    0.124088    0.244426    0.101673    11.00000    0.03454    0.11249 =
         0.08229    0.00376   -0.01335   -0.00446
PART 11
AFIX  43
H1A   2    0.222530    0.246236    0.114005    10.50000   -1.20000
AFIX  43
PART 12
H1B   2    0.222530    0.246236    0.114005    10.50000   -1.20000
AFIX   0
PART 11
C2    1    0.079955    0.242691    0.044451    10.50000    0.08333    0.29000 =
         0.05261   -0.00544    0.02262    0.00049
AFIX  43
H2    2    0.147158    0.241656    0.010353    10.50000   -1.20000
AFIX   0
PART 0
C1    1    0.000000    0.243062    0.137432    10.50000    0.06647    0.08984 =
         0.05241    0.00251    0.00000    0.00000
AFIX  43
H1    2    0.000000    0.241437    0.180032    10.50000    0.67550
AFIX   0
PART 12
N2    4    0.079955    0.242691    0.044451    10.50000    0.08333    0.29000 =
         0.05261   -0.00544    0.02262    0.00049
HKLF 4




REM  triag2pbcl4_340a_a.res in Cmcm
REM wR2 = 0.0913, GooF = S = 1.151, Restrained GooF = 1.151 for all data
REM R1 = 0.0343 for 765 Fo > 4sig(Fo) and 0.0429 for all 905 data
REM 44 parameters refined using 0 restraints

END

WGHT      0.0383      7.7424

REM Highest difference peak  0.929,  deepest hole -2.164,  1-sigma level  0.200
Q1    1   0.4384  0.3531  0.2500  10.50000  0.05    0.93
;
_shelx_res_checksum              44794
_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
;
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_triag2pbcl4_temp2_3_370_00
_database_code_depnum_ccdc_archive 'CCDC 2314666'
loop_
_audit_author_name
_audit_author_address
'Szymon Sobczak'
;Department of Materials Chemistry, Adam Mickiewicz University
Poland
;
_audit_update_record             
;
2024-03-04 deposited with the CCDC.	2024-03-21 downloaded from the CCDC.
;
_audit_creation_date             2023-12-15
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_shelx_SHELXL_version_number     2018/3
loop_
_audit_author_email
szymon.sobczak@amu.edu.pl
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Cl4 Pb, 4(C H2 N1.5)'
_chemical_formula_sum            'C4 H8 Cl4 N6 Pb'
_chemical_formula_weight         489.15
_chemical_melting_point          ?
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'

_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.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           69
_space_group_name_H-M_alt        'F m m m'
_space_group_name_Hall           '-F 2 2'
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'

_cell_length_a                   7.5639(2)
_cell_length_b                   8.2984(2)
_cell_length_c                   21.7768(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1366.89(7)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    5053
_cell_measurement_temperature    370.00(10)
_cell_measurement_theta_max      28.5130
_cell_measurement_theta_min      2.7060
_shelx_estimated_absorpt_T_max   0.261
_shelx_estimated_absorpt_T_min   0.045
_exptl_absorpt_coefficient_mu    13.104
_exptl_absorpt_correction_T_max  0.194
_exptl_absorpt_correction_T_min  0.043
_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_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.377
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             896
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
10 0 -13 0.1475
-10 0 13 0.1131
5 0 28 0.0805
0 -12 -1 0.2988
-5 0 -28 0.0541
-8 6 12 0.1664
8 -7 -12 0.2105
2 11 11 0.2718
-6 -9 5 0.2378
7 9 -5 0.2672

_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0655
_diffrn_reflns_av_unetI/netI     0.0297
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.959
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            5515
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.959
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         29.009
_diffrn_reflns_theta_min         3.743
_diffrn_ambient_temperature      370.15
_diffrn_detector_area_resol_mean 16.1544
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.959
_diffrn_measurement_details      .
_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_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                515
_reflns_number_total             515
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_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)'
_refine_diff_density_max         0.835
_refine_diff_density_min         -1.082
_refine_diff_density_rms         0.145
_refine_ls_extinction_coef       0.00156(17)
_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   1.085
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     30
_refine_ls_number_reflns         515
_refine_ls_number_restraints     27
_refine_ls_R_factor_all          0.0219
_refine_ls_R_factor_gt           0.0219
_refine_ls_restrained_S_all      1.072
_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)+(0.0272P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0466
_refine_ls_wR_factor_ref         0.0466
_refine_special_details          ?
_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(N2) \\sim Ueq, Uanis(C2) \\sim Ueq: with sigma of 0.1 and sigma for
terminal atoms of 0.2
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)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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 0.02888(17) Uani 1 8 d S T P . .
Cl2 Cl 0.500000 0.000000 0.13111(11) 0.0678(7) Uani 1 4 d S T P . .
Cl1 Cl 0.250000 0.250000 0.000000 0.0838(9) Uani 1 4 d S T P . .
N1 N 0.500000 0.3757(7) 0.1486(4) 0.0770(19) Uani 1 2 d S T P . .
H1A H 0.500000 0.277223 0.136235 0.092 Uiso 0.5 2 calc R U P A 7
H1B H 0.500000 0.277223 0.136235 0.092 Uiso 0.5 2 calc R U P B 8
C1 C 0.500000 0.500000 0.1134(6) 0.074(3) Uani 1 4 d S T P C .
H1 H 0.500000 0.500000 0.070697 0.27(17) Uiso 1 4 calc R . P . .
C2 C 0.500000 0.4210(12) 0.2054(5) 0.125(4) Uani 0.5 2 d S TU P C 7
H2 H 0.500000 0.354325 0.239713 0.150 Uiso 0.5 2 calc R U P C 7
N2 N 0.500000 0.4210(12) 0.2054(5) 0.125(4) Uani 0.5 2 d S TU P C 8

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 0.0315(2) 0.0193(2) 0.0359(2) 0.000 0.000 0.000
Cl2 0.129(2) 0.0341(10) 0.0402(12) 0.000 0.000 0.000
Cl1 0.0802(16) 0.0744(16) 0.097(2) 0.000 0.000 0.0505(15)
N1 0.111(5) 0.038(3) 0.082(4) -0.010(3) 0.000 0.000
C1 0.095(8) 0.072(6) 0.054(6) 0.000 0.000 0.000
C2 0.234(13) 0.077(5) 0.064(4) 0.021(4) 0.000 0.000
N2 0.234(13) 0.077(5) 0.064(4) 0.021(4) 0.000 0.000

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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 2.855(2) 17_655 ?
Pb1 Cl2 2.855(2) . ?
Pb1 Cl1 2.80709(5) 15_545 ?
Pb1 Cl1 2.80709(5) 3_655 ?
Pb1 Cl1 2.80709(5) . ?
Pb1 Cl1 2.80709(5) 13_545 ?
N1 H1A 0.8600 . ?
N1 H1B 0.8600 . ?
N1 C1 1.285(10) . ?
N1 C2 1.293(13) . ?
N1 N2 1.293(13) . ?
C1 H1 0.9300 . ?
C2 C2 1.310(19) 2_665 ?
C2 H2 0.9300 . ?

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 17_655 ?
Cl1 Pb1 Cl2 90.0 15_545 . ?
Cl1 Pb1 Cl2 90.0 3_655 . ?
Cl1 Pb1 Cl2 90.0 3_655 17_655 ?
Cl1 Pb1 Cl2 90.0 . 17_655 ?
Cl1 Pb1 Cl2 90.0 . . ?
Cl1 Pb1 Cl2 90.0 13_545 . ?
Cl1 Pb1 Cl2 90.0 13_545 17_655 ?
Cl1 Pb1 Cl1 84.698(2) 15_545 13_545 ?
Cl1 Pb1 Cl1 95.302(2) 15_545 . ?
Cl1 Pb1 Cl1 84.698(2) 3_655 . ?
Cl1 Pb1 Cl1 95.302(2) 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 125.2 . . ?
C1 N1 H1B 125.2 . . ?
C1 N1 C2 109.7(8) . . ?
C1 N1 N2 109.7(8) . . ?
C2 N1 H1A 125.2 . . ?
N2 N1 H1B 125.2 . . ?
N1 C1 N1 106.8(11) . 2_665 ?
N1 C1 H1 126.6 . . ?
N1 C1 H1 126.6 2_665 . ?
N1 C2 C2 106.9(5) . 2_665 ?
N1 C2 H2 126.5 . . ?
C2 C2 H2 126.5 2_665 . ?

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(2) . . . 2_665 ?
C2 N1 C1 N1 0.000(1) . . . 2_665 ?
N2 N1 C1 N1 0.000(1) . . . 2_665 ?

_shelx_res_file                  
;
TITL triag2pbcl4_temp2_3_370_00_a.res in Fmmm
    triag2pbcl4_temp2_3_370_00.res
    created by SHELXL-2018/3 at 13:06:38 on 15-Dec-2023
REM Old TITL TRIAG2PbCl4_temp2_3_370_00 in Fmmm
REM SHELXT solution in Fmmm: R1 0.097, Rweak 0.329, Alpha 0.014
REM <I/s> 0.000 for 0 systematic absences, Orientation as input
REM Formula found by SHELXT: C6 Cl4 Pb
CELL 0.71073 7.5639 8.2984 21.7768 90 90 90
ZERR 4 0.0002 0.0002 0.0007 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
ISOR N2 C2
EXYZ C2 N2

L.S. 44 0 0
PLAN  1
SIZE 0.14 0.26 0.62
TEMP 97
CONF
list 4
MORE -1
BOND $H
fmap 2 53
acta 50
OMIT 0 0 6
OMIT 0 0 8
OMIT 0 0 10
OMIT 0 0 14
OMIT 0 2 0
OMIT 1 5 25
OMIT 2 0 4
REM <olex2.extras>
REM <HklSrc "%.\\triag2pbcl4_temp2_3_370_00.hkl">
REM </olex2.extras>

WGHT    0.027200
EXTI    0.001561
FVAR       0.21847
PB1   5    0.500000    0.000000    0.000000    10.12500    0.03147    0.01926 =
         0.03591    0.00000    0.00000    0.00000
CL2   3    0.500000    0.000000    0.131112    10.25000    0.12895    0.03415 =
         0.04018    0.00000    0.00000    0.00000
CL1   3    0.250000    0.250000    0.000000    10.25000    0.08024    0.07436 =
         0.09675    0.00000    0.00000    0.05054
N1    4    0.500000    0.375654    0.148592    10.50000    0.11089    0.03790 =
         0.08218   -0.01047    0.00000    0.00000
PART 7
AFIX  43
H1A   2    0.500000    0.277223    0.136235    10.25000   -1.20000
AFIX  43
PART 8
H1B   2    0.500000    0.277223    0.136235    10.25000   -1.20000
AFIX   0
PART 0
C1    1    0.500000    0.500000    0.113403    10.25000    0.09525    0.07205 =
         0.05373    0.00000    0.00000    0.00000
AFIX  43
H1    2    0.500000    0.500000    0.070697    10.25000    0.26750
AFIX   0
PART 7
C2    1    0.500000    0.421039    0.205398    10.25000    0.23388    0.07694 =
         0.06366    0.02086    0.00000    0.00000
AFIX  43
H2    2    0.500000    0.354325    0.239713    10.25000   -1.20000
AFIX   0
PART 8
N2    4    0.500000    0.421039    0.205398    10.25000    0.23388    0.07694 =
         0.06366    0.02086    0.00000    0.00000
HKLF 4




REM  triag2pbcl4_temp2_3_370_00_a.res in Fmmm
REM wR2 = 0.0466, GooF = S = 1.085, Restrained GooF = 1.072 for all data
REM R1 = 0.0219 for 515 Fo > 4sig(Fo) and 0.0219 for all 515 data
REM 30 parameters refined using 27 restraints

END

WGHT      0.0272      0.0000

REM Highest difference peak  0.835,  deepest hole -1.082,  1-sigma level  0.145
Q1    1   0.4192  0.0741  0.0000  10.50000  0.05    0.84
;
_shelx_res_checksum              29990
_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
;
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_triag2pbcl4_i_390_00
_database_code_depnum_ccdc_archive 'CCDC 2314667'
loop_
_audit_author_name
_audit_author_address
'Szymon Sobczak'
;Department of Materials Chemistry, Adam Mickiewicz University
Poland
;
_audit_update_record             
;
2024-03-04 deposited with the CCDC.	2024-03-21 downloaded from the CCDC.
;
_audit_creation_date             2023-12-15
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        (TzH)2PbCl4
_chemical_formula_moiety         'Cl4 Pb, 4(C H2 N1.5)'
_chemical_formula_sum            'C4 H8 Cl4 N6 Pb'
_chemical_formula_weight         489.15
_chemical_melting_point          ?
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'

_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.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           69
_space_group_name_H-M_alt        'F m m m'
_space_group_name_Hall           '-F 2 2'
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'

_cell_length_a                   7.6009(7)
_cell_length_b                   8.3017(6)
_cell_length_c                   21.798(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1375.4(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    4584
_cell_measurement_temperature    390.01(10)
_cell_measurement_theta_max      28.5420
_cell_measurement_theta_min      2.7170
_shelx_estimated_absorpt_T_max   0.263
_shelx_estimated_absorpt_T_min   0.046
_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_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.362
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_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
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_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
_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_details      .
_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_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                512
_reflns_number_total             513
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_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)'
_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_R_factor_all          0.0252
_refine_ls_R_factor_gt           0.0251
_refine_ls_restrained_S_all      1.037
_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
_refine_special_details          ?
_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)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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_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_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 ?

_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
;
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_triag2pbcl4_02_250_00
_database_code_depnum_ccdc_archive 'CCDC 2314660'
loop_
_audit_author_name
_audit_author_address
'Szymon Sobczak'
;Department of Materials Chemistry, Adam Mickiewicz University
Poland
;
_audit_update_record             
;
2024-03-04 deposited with the CCDC.	2024-03-21 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT112_triag2pbcl4_02_250_00 
;
PROBLEM: ADDSYM Detects New (Pseudo) Symm. Elem         n        100 %Fit
RESPONSE: The symmetry has been thoroughly inspected by the presence of systematic absences in the raw diffraction data
;
_vrf_PLAT113_triag2pbcl4_02_250_00 
;
PROBLEM: ADDSYM Suggests Possible Pseudo/New  Space Group       Pnma Check
RESPONSE: look PLAT112
;
_vrf_PLAT934_triag2pbcl4_02_250_00 
;
PROBLEM: Number of (Iobs-Icalc)/Sigma(W) > 10 Outliers ..          5 Check
RESPONSE: Some of the reflection with high errors were omitted
;
# Added during the CSD deposition process: Friday 15 December 2023 12:43 PM
# end Validation Reply Form

_audit_creation_date             2023-12-15
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        Tz2PbCl4
_chemical_formula_moiety         'Cl4 Pb, 2(C2 H4 N3)'
_chemical_formula_sum            'C4 H8 Cl4 N6 Pb'
_chemical_formula_weight         489.15
_chemical_melting_point          ?
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'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
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'

_cell_length_a                   21.4831(12)
_cell_length_b                   8.3057(3)
_cell_length_c                   7.4695(3)
_cell_angle_alpha                90
_cell_angle_beta                 90.036(4)
_cell_angle_gamma                90
_cell_volume                     1332.80(10)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    5770
_cell_measurement_temperature    249.99(10)
_cell_measurement_theta_max      28.5470
_cell_measurement_theta_min      3.6480
_shelx_estimated_absorpt_T_max   0.295
_shelx_estimated_absorpt_T_min   0.050
_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_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.438
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             896
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 -11 0.0824
-2 12 -1 0.1383
-30 1 0 0.0656
30 0 0 0.0459

_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_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
_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  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     23.00  48.00   1.00    5.00    --   17.79-139.00 143.00   25
  2  ω     16.00  41.00   1.00    5.00    --   17.79-130.00 -42.00   25
  3  ω    -62.00 -18.00   1.00    5.00    --  -18.57 130.00  29.00   44
  4  ω    -75.00 -47.00   1.00    5.00    --  -18.57 139.00-156.00   28
  5  ω     39.00  94.00   1.00    5.00    --   17.79 178.00  30.00   55
  6  ω     43.00  68.00   1.00    5.00    --   17.79 178.00-150.00   25
  7  ω    -47.00  61.00   1.00    5.00    --   17.79 -19.00 150.00  108
  8  ω    -32.00  11.00   1.00    5.00    --  -18.57 -77.00 120.00   43
  9  ω    -87.00   3.00   1.00    5.00    --  -18.57 -57.00  90.00   90
 10  ω    -84.00 -59.00   1.00    5.00    --  -18.57-178.00   0.00   25
 11  ω    -32.00  11.00   1.00    5.00    --  -18.57 -77.00 -30.00   43
 12  ω     -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       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2395
_reflns_number_total             3182
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_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)'
_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+0.001xFc²λ³/sin(2θ)]^-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_R_factor_all          0.0500
_refine_ls_R_factor_gt           0.0354
_refine_ls_restrained_S_all      1.251
_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)+(0.0308P)²+2.2842P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0849
_refine_ls_wR_factor_ref         0.0906
_refine_special_details          'Refined as a 2-component inversion twin.,Twin'
_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)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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 0.25000(2) 0.49578(2) 0.35727(3) 0.03100(14) Uani 1 1 d . . . . .
Cl1 Cl 0.24991(11) 0.7628(2) 0.1299(2) 0.0565(6) Uani 1 1 d . . . . .
Cl2 Cl 0.25017(12) 0.1965(2) 0.5475(3) 0.0625(6) Uani 1 1 d . . . . .
Cl4 Cl 0.38297(11) 0.49106(18) 0.3523(4) 0.0557(6) Uani 1 1 d . . . . .
Cl3 Cl 0.11696(11) 0.49115(18) 0.3522(4) 0.0557(6) Uani 1 1 d . . . . .
N2A N 0.3957(3) 0.3895(7) 0.8461(9) 0.0515(17) Uani 1 1 d . . . . .
H2A H 0.377695 0.297229 0.865169 0.062 Uiso 1 1 calc R U . . .
N1B N 0.0903(3) 0.6388(7) 0.8253(9) 0.0534(18) Uani 1 1 d . . . . .
H1B H 0.095820 0.742561 0.828035 0.064 Uiso 1 1 calc R U . . .
N1A N 0.4091(4) 0.6380(7) 0.8247(10) 0.0564(19) Uani 1 1 d . . . . .
H1A H 0.403351 0.741627 0.825996 0.068 Uiso 1 1 calc R U . . .
N2B N 0.1044(3) 0.3895(8) 0.8459(10) 0.0543(18) Uani 1 1 d . . . . .
H2B H 0.122439 0.297232 0.864748 0.065 Uiso 1 1 calc R U . . .
C1A C 0.3683(5) 0.5279(9) 0.8621(14) 0.057(2) Uani 1 1 d . . . . .
H1AA H 0.326604 0.545301 0.894635 0.068 Uiso 1 1 calc R U . . .
C1B C 0.1322(5) 0.5275(9) 0.8621(14) 0.054(2) Uani 1 1 d . . . . .
H1BA H 0.173984 0.544694 0.893813 0.065 Uiso 1 1 calc R U . . .
N3A N 0.4556(3) 0.4066(8) 0.7964(12) 0.065(2) Uani 1 1 d . . . . .
N3B N 0.0443(3) 0.4055(8) 0.7966(12) 0.065(2) Uani 1 1 d . . . . .
C2A C 0.4620(4) 0.5606(10) 0.7838(14) 0.064(3) Uani 1 1 d . . . . .
H2AA H 0.499181 0.612138 0.750047 0.077 Uiso 1 1 calc R U . . .
C2B C 0.0372(4) 0.5603(10) 0.7827(14) 0.064(3) Uani 1 1 d . . . . .
H2BA H 0.000074 0.611119 0.747556 0.076 Uiso 1 1 calc R U . . .

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 0.0589(2) 0.01587(16) 0.01820(17) -0.00037(7) 0.00036(11) 0.00004(10)
Cl1 0.1049(17) 0.0327(10) 0.0319(9) 0.0144(7) 0.0001(10) 0.0004(9)
Cl2 0.1079(17) 0.0387(10) 0.0408(11) 0.0219(8) 0.0018(10) 0.0027(11)
Cl4 0.0567(12) 0.0234(9) 0.0870(19) 0.0002(7) -0.0039(11) -0.0013(7)
Cl3 0.0561(12) 0.0240(9) 0.0871(19) 0.0001(7) 0.0047(11) 0.0022(7)
N2A 0.059(5) 0.030(3) 0.066(5) 0.005(3) 0.000(3) -0.002(3)
N1B 0.078(5) 0.020(3) 0.062(5) 0.001(3) 0.014(4) -0.007(3)
N1A 0.083(5) 0.021(3) 0.065(5) 0.004(3) -0.006(4) 0.007(3)
N2B 0.064(5) 0.029(3) 0.070(5) 0.008(3) 0.001(4) 0.005(3)
C1A 0.075(6) 0.040(5) 0.055(6) 0.006(4) 0.006(5) 0.011(4)
C1B 0.061(6) 0.045(5) 0.056(6) 0.006(4) -0.006(4) -0.011(4)
N3A 0.055(5) 0.028(4) 0.112(7) 0.002(4) -0.012(4) 0.002(3)
N3B 0.057(5) 0.032(4) 0.107(7) 0.002(4) 0.014(4) -0.006(3)
C2A 0.060(6) 0.030(4) 0.103(8) 0.006(4) -0.016(5) 0.000(4)
C2B 0.058(6) 0.033(4) 0.100(8) 0.006(4) 0.018(5) 0.004(4)

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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 2.7936(15) . ?
Pb1 Cl1 2.8576(15) 4_576 ?
Pb1 Cl2 2.8633(16) . ?
Pb1 Cl2 2.8114(17) 4_565 ?
Pb1 Cl4 2.857(2) . ?
Pb1 Cl3 2.858(2) . ?
N2A H2A 0.8700 . ?
N2A C1A 1.297(10) . ?
N2A N3A 1.347(9) . ?
N1B H1B 0.8700 . ?
N1B C1B 1.318(11) . ?
N1B C2B 1.352(11) . ?
N1A H1A 0.8700 . ?
N1A C1A 1.297(11) . ?
N1A C2A 1.341(11) . ?
N2B H2B 0.8700 . ?
N2B C1B 1.298(10) . ?
N2B N3B 1.349(10) . ?
C1A H1AA 0.9400 . ?
C1B H1BA 0.9400 . ?
N3A C2A 1.290(12) . ?
N3B C2B 1.299(12) . ?
C2A H2AA 0.9400 . ?
C2B H2BA 0.9400 . ?

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 82.889(7) . 4_576 ?
Cl1 Pb1 Cl2 104.81(5) 4_576 . ?
Cl1 Pb1 Cl2 87.16(5) . 4_565 ?
Cl1 Pb1 Cl2 172.30(5) . . ?
Cl1 Pb1 Cl4 90.19(6) . . ?
Cl1 Pb1 Cl3 90.13(7) . . ?
Cl1 Pb1 Cl3 91.02(7) 4_576 . ?
Cl2 Pb1 Cl1 170.05(5) 4_565 4_576 ?
Cl2 Pb1 Cl2 85.140(15) 4_565 . ?
Cl2 Pb1 Cl4 88.83(8) 4_565 . ?
Cl2 Pb1 Cl3 89.04(8) 4_565 . ?
Cl4 Pb1 Cl1 91.15(7) . 4_576 ?
Cl4 Pb1 Cl2 89.63(7) . . ?
Cl4 Pb1 Cl3 177.83(6) . . ?
Cl3 Pb1 Cl2 89.77(7) . . ?
Pb1 Cl1 Pb1 172.01(8) . 4_575 ?
Pb1 Cl2 Pb1 154.36(9) 4_566 . ?
C1A N2A H2A 124.3 . . ?
C1A N2A N3A 111.4(7) . . ?
N3A N2A H2A 124.3 . . ?
C1B N1B H1B 126.7 . . ?
C1B N1B C2B 106.6(7) . . ?
C2B N1B H1B 126.7 . . ?
C1A N1A H1A 126.7 . . ?
C1A N1A C2A 106.5(7) . . ?
C2A N1A H1A 126.7 . . ?
C1B N2B H2B 123.9 . . ?
C1B N2B N3B 112.2(7) . . ?
N3B N2B H2B 123.9 . . ?
N2A C1A H1AA 126.3 . . ?
N1A C1A N2A 107.3(9) . . ?
N1A C1A H1AA 126.3 . . ?
N1B C1B H1BA 126.7 . . ?
N2B C1B N1B 106.7(8) . . ?
N2B C1B H1BA 126.7 . . ?
C2A N3A N2A 103.2(6) . . ?
C2B N3B N2B 103.4(6) . . ?
N1A C2A H2AA 124.2 . . ?
N3A C2A N1A 111.6(7) . . ?
N3A C2A H2AA 124.2 . . ?
N1B C2B H2BA 124.5 . . ?
N3B C2B N1B 111.1(7) . . ?
N3B C2B H2BA 124.5 . . ?

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 0.5(9) . . . . ?
N2B N3B C2B N1B -1.3(9) . . . . ?
C1A N2A N3A C2A -0.1(9) . . . . ?
C1A N1A C2A N3A -0.7(11) . . . . ?
C1B N1B C2B N3B 1.8(10) . . . . ?
C1B N2B N3B C2B 0.4(10) . . . . ?
N3A N2A C1A N1A -0.4(11) . . . . ?
N3B N2B C1B N1B 0.7(11) . . . . ?
C2A N1A C1A N2A 0.7(11) . . . . ?
C2B N1B C1B N2B -1.5(11) . . . . ?

_shelx_res_file                  
;
TITL triag2pbcl4_02_250_00_a.res in P2(1)/c
    triag2pbcl4_02_250_00.res
    created by SHELXL-2018/3 at 13:12:26 on 15-Dec-2023
REM Old TITL TRIAG2PbCl4_02_250_00 in P2(1)/c
REM SHELXT solution in P2(1)/c: R1 0.195, Rweak 0.024, Alpha 0.014
REM <I/s> 0.773 for 204 systematic absences, Orientation as input
REM Formula found by SHELXT: C10 Cl4 Pb
CELL 0.71073 21.4831 8.3057 7.4695 90 90.036 90
ZERR 4 0.0012 0.0003 0.0003 0 0.004 0
LATT 1
SYMM -X,0.5+Y,0.5-Z
SFAC C H Cl N Pb
UNIT 16 32 16 24 4

L.S. 44
PLAN  6
SIZE 0.12 0.18 0.56
TEMP -23
CONF
list 4
MORE -1
BOND $H
fmap 2
acta 50
TWIN -1 0 0 0 -1 0 0 0 -1 2
REM <olex2.extras>
REM <HklSrc "%.\\triag2pbcl4_02_250_00.hkl">
REM </olex2.extras>

WGHT    0.030800    2.284200
EXTI    0.015067
BASF   9.82115
FVAR       0.29877
PB1   5    0.249998    0.495781    0.357272    11.00000    0.05892    0.01587 =
         0.01820   -0.00037    0.00036    0.00004
CL1   3    0.249910    0.762799    0.129852    11.00000    0.10491    0.03273 =
         0.03194    0.01439    0.00015    0.00041
CL2   3    0.250173    0.196485    0.547504    11.00000    0.10793    0.03871 =
         0.04076    0.02186    0.00181    0.00266
CL4   3    0.382969    0.491059    0.352269    11.00000    0.05670    0.02342 =
         0.08703    0.00024   -0.00389   -0.00126
CL3   3    0.116964    0.491145    0.352150    11.00000    0.05606    0.02402 =
         0.08709    0.00012    0.00470    0.00219
N2A   4    0.395719    0.389451    0.846147    11.00000    0.05888    0.02960 =
         0.06600    0.00530   -0.00050   -0.00202
AFIX  43
H2A   2    0.377695    0.297229    0.865169    11.00000   -1.20000
AFIX   0

N1B   4    0.090327    0.638810    0.825341    11.00000    0.07825    0.01968 =
         0.06231    0.00144    0.01370   -0.00740
AFIX  43
H1B   2    0.095820    0.742561    0.828035    11.00000   -1.20000
AFIX   0

N1A   4    0.409149    0.637966    0.824723    11.00000    0.08348    0.02104 =
         0.06475    0.00380   -0.00557    0.00653
AFIX  43
H1A   2    0.403351    0.741627    0.825996    11.00000   -1.20000
AFIX   0

N2B   4    0.104383    0.389455    0.845915    11.00000    0.06401    0.02873 =
         0.07019    0.00782    0.00096    0.00488
AFIX  43
H2B   2    0.122439    0.297232    0.864748    11.00000   -1.20000
AFIX   0

C1A   1    0.368324    0.527928    0.862064    11.00000    0.07517    0.04046 =
         0.05484    0.00582    0.00609    0.01125
AFIX  43
H1AA  2    0.326604    0.545301    0.894635    11.00000   -1.20000
AFIX   0

C1B   1    0.132163    0.527474    0.862079    11.00000    0.06092    0.04460 =
         0.05647    0.00588   -0.00636   -0.01110
AFIX  43
H1BA  2    0.173984    0.544694    0.893813    11.00000   -1.20000
AFIX   0

N3A   4    0.455591    0.406611    0.796448    11.00000    0.05534    0.02850 =
         0.11186    0.00234   -0.01161    0.00230
N3B   4    0.044300    0.405481    0.796559    11.00000    0.05665    0.03232 =
         0.10696    0.00218    0.01423   -0.00555
C2A   1    0.462041    0.560597    0.783775    11.00000    0.06001    0.03041 =
         0.10269    0.00650   -0.01594   -0.00046
AFIX  43
H2AA  2    0.499181    0.612138    0.750047    11.00000   -1.20000
AFIX   0

C2B   1    0.037229    0.560332    0.782667    11.00000    0.05774    0.03323 =
         0.10007    0.00564    0.01775    0.00363
AFIX  43
H2BA  2    0.000074    0.611119    0.747556    11.00000   -1.20000
AFIX   0
HKLF 4




REM  triag2pbcl4_02_250_00_a.res in P2(1)/c
REM wR2 = 0.0906, GooF = S = 1.251, Restrained GooF = 1.251 for all data
REM R1 = 0.0354 for 2395 Fo > 4sig(Fo) and 0.0500 for all 3182 data
REM 138 parameters refined using 0 restraints

END

WGHT      0.0308      2.2894

REM Highest difference peak  2.168,  deepest hole -1.577,  1-sigma level  0.214
Q1    1   0.2518  0.3950  0.3592  11.00000  0.05    2.17
Q2    1   0.2550  0.6003  0.3538  11.00000  0.05    2.12
Q3    1   0.1323  0.5837  0.3804  11.00000  0.05    0.77
Q4    1   0.2483  0.5178  0.9952  11.00000  0.05    0.74
Q5    1   0.3728  0.5912  0.3419  11.00000  0.05    0.69
Q6    1   0.2582  0.6820  0.1820  11.00000  0.05    0.68
;
_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
;
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 -9(10)
2 10(10)

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_triag2pbcl4_08_220_00
_database_code_depnum_ccdc_archive 'CCDC 2314659'
loop_
_audit_author_name
_audit_author_address
'Szymon Sobczak'
;Department of Materials Chemistry, Adam Mickiewicz University
Poland
;
_audit_update_record             
;
2024-03-04 deposited with the CCDC.	2024-03-21 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT112_triag2pbcl4_08_220_00 
;
PROBLEM: ADDSYM Detects New (Pseudo) Symm. Elem         n        100 %Fit
RESPONSE: The symmetry has been thoroughly inspected by the presence of systematic absences in the raw diffraction data
;
_vrf_PLAT113_triag2pbcl4_08_220_00 
;
PROBLEM: ADDSYM Suggests Possible Pseudo/New  Space Group       Pnma Check
RESPONSE: look PLAT112
;
_vrf_PLAT972_triag2pbcl4_08_220_00 
;
PROBLEM: Check Calcd Resid. Dens.  0.98Ang From Pb1            -2.89 eA-3
RESPONSE: Residual density near heavy atom.
;
# Added during the CSD deposition process: Friday 15 December 2023 12:43 PM
# end Validation Reply Form

_audit_creation_date             2023-12-15
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        Tz2PbCl4
_chemical_formula_moiety         'Cl4 Pb, 2(C2 H4 N3)'
_chemical_formula_sum            'C4 H8 Cl4 N6 Pb'
_chemical_formula_weight         489.15
_chemical_melting_point          ?
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'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
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'

_cell_length_a                   21.4566(15)
_cell_length_b                   8.3029(3)
_cell_length_c                   7.4446(3)
_cell_angle_alpha                90
_cell_angle_beta                 90.036(4)
_cell_angle_gamma                90
_cell_volume                     1326.27(12)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    5622
_cell_measurement_temperature    220.00(10)
_cell_measurement_theta_max      28.6400
_cell_measurement_theta_min      3.6580
_shelx_estimated_absorpt_T_max   0.294
_shelx_estimated_absorpt_T_min   0.049
_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_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.450
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             896
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

_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_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
_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_details      .
_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_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2441
_reflns_number_total             3158
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_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)'
_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_R_factor_all          0.0555
_refine_ls_R_factor_gt           0.0402
_refine_ls_restrained_S_all      1.116
_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
_refine_special_details          ?
_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)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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_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 0.0744(2) 0.01421(15) 0.01580(16) -0.00036(7) 0.00012(12) -0.00010(10)
Cl1 0.1196(18) 0.0287(9) 0.0263(9) 0.0121(6) 0.0000(10) 0.0005(9)
Cl2 0.1181(18) 0.0330(9) 0.0363(11) 0.0187(8) 0.0010(10) 0.0012(11)
Cl4 0.0721(14) 0.0208(9) 0.0829(18) 0.0004(7) -0.0066(11) -0.0018(8)
Cl3 0.0729(14) 0.0197(9) 0.0843(18) 0.0009(7) 0.0082(12) 0.0031(7)
N2A 0.065 0.029 0.062 0.005 0.000 0.000
N1B 0.088 0.022 0.061 0.000 0.015 0.000
N1A 0.080 0.020 0.065 0.001 0.000 0.007
N2B 0.070 0.030 0.060 0.008 0.006 0.000
C1A 0.078 0.037 0.062 0.010 0.000 0.013
C1B 0.083 0.039 0.054 0.006 0.000 0.000
N3A 0.074 0.024 0.100 0.002 0.000 0.005
N3B 0.060 0.026 0.106 0.000 0.024 0.000
C2A 0.066 0.026 0.106 0.006 0.000 0.000
C2B 0.060 0.026 0.106 0.002 0.027 0.000

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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_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_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) . . . . ?

_shelx_res_file                  
;
TITL triag2pbcl4_08_220_00_a.res in P2(1)/c
    triag2pbcl4_08_220_00.res
    created by SHELXL-2019/2 at 17:27:05 on 01-Mar-2024
REM Old TITL TRIAG2PbCl4_08_220_00 in P2(1)/c
REM SHELXT solution in P2(1)/c: R1 0.255, Rweak 0.042, Alpha 0.014
REM <I/s> 0.920 for 202 systematic absences, Orientation as input
REM Formula found by SHELXT: C7 N3 Cl4 Pb
CELL 0.71073 21.4566 8.3029 7.4446 90 90.036 90
ZERR 4 0.0015 0.0003 0.0003 0 0.004 0
LATT 1
SYMM -X,0.5+Y,0.5-Z
SFAC C H Cl N Pb
UNIT 16 32 16 24 4
RIGU Cl2 Pb1 Cl1 Cl4 Cl3
RIGU N3B N2B C1B C2B N1B
RIGU N2B C1B N1B N3B C2B
SADI N3A N2A N3B N2B
SADI N3B C2B N3A C2A
SADI N2A C1A N2B C1B
SADI N1B C1B N1A C1A
SADI N1B C2B N1A C2A

L.S. 44 0 0
PLAN  6
SIZE 0.12 0.16 0.50
TEMP -53
CONF
list 4
MORE -1
BOND $H
fmap 2 53
acta 50
OMIT 0 2 0
OMIT 0 3 1
OMIT 1 2 0
OMIT 3 0 0
OMIT 3 1 0
OMIT 3 2 0
OMIT 3 4 0
OMIT 4 1 0
OMIT 4 3 0
OMIT 5 1 0
OMIT 5 2 0
OMIT 7 2 0
OMIT 8 0 0
REM <olex2.extras>
REM <HklSrc "%.\\triag2pbcl4_08_220_00.hkl">
REM </olex2.extras>

WGHT    0.036000    4.088800
EXTI    0.012924
FVAR       0.30050
PB1   5    0.249987    0.494903    0.360867    11.00000    0.07437    0.01421 =
         0.01580   -0.00036    0.00012   -0.00010
CL1   3    0.249754    0.763176    0.134755    11.00000    0.11959    0.02873 =
         0.02633    0.01208    0.00003    0.00050
CL2   3    0.249932    0.192390    0.546579    11.00000    0.11809    0.03297 =
         0.03628    0.01871    0.00098    0.00115
CL4   3    0.382982    0.488982    0.356194    11.00000    0.07210    0.02083 =
         0.08294    0.00042   -0.00663   -0.00184
CL3   3    0.116866    0.488985    0.356001    11.00000    0.07290    0.01971 =
         0.08428    0.00093    0.00822    0.00306
N2A   4    0.395795    0.391529    0.849210    11.00000   10.06491   10.02857 =
        10.06170   10.00493  -10.00864  -10.00351
AFIX  43
H2A   2    0.377761    0.299294    0.868502    11.00000   -1.20000
AFIX   0

N1B   4    0.089706    0.640207    0.828817    11.00000   10.08839   10.02152 =
        10.06141  -10.00062   10.01473  -10.00403
AFIX  43
H1B   2    0.094894    0.744080    0.832354    11.00000   -1.20000
AFIX   0

N1A   4    0.410230    0.639818    0.827269    11.00000   10.07991   10.01973 =
        10.06483   10.00101  -10.01569   10.00717
AFIX  43
H1A   2    0.404985    0.743709    0.829031    11.00000   -1.20000
AFIX   0

N2B   4    0.104148    0.391311    0.850083    11.00000   10.07039   10.03038 =
        10.05999   10.00785   10.00608  -10.00355
AFIX  43
H2B   2    0.122087    0.299077    0.870171    11.00000   -1.20000
AFIX   0

C1A   1    0.367877    0.530732    0.865649    11.00000   10.07772   10.03681 =
        10.06243   10.00953  -10.00031   10.01292
AFIX  43
H1AA  2    0.326150    0.549021    0.898184    11.00000   -1.20000
AFIX   0

C1B   1    0.131949    0.529829    0.865813    11.00000   10.08274   10.03949 =
        10.05435   10.00593  -10.00635  -10.01069
AFIX  43
H1BA  2    0.173818    0.547646    0.897290    11.00000   -1.20000
AFIX   0

N3A   4    0.455608    0.407687    0.799020    11.00000   10.07401   10.02448 =
        10.10023   10.00158  -10.02574   10.00455
N3B   4    0.044278    0.407801    0.798983    11.00000   10.06017   10.02570 =
        10.10598   10.00033   10.02413  -10.00287
C2A   1    0.463010    0.561963    0.784885    11.00000   10.06583   10.02629 =
        10.10624   10.00633  -10.02657  -10.00422
AFIX  43
H2AA  2    0.500263    0.612489    0.749740    11.00000   -1.20000
AFIX   0

C2B   1    0.037069    0.561762    0.784569    11.00000   10.05958   10.02592 =
        10.10568   10.00210   10.02671  -10.00276
AFIX  43
H2BA  2   -0.000046    0.612226    0.748004    11.00000   -1.20000
AFIX   0
HKLF 4




REM  triag2pbcl4_08_220_00_a.res in P2(1)/c
REM wR2 = 0.0931, GooF = S = 1.110, Restrained GooF = 1.116 for all data
REM R1 = 0.0402 for 2428 Fo > 4sig(Fo) and 0.0555 for all 3145 data
REM 77 parameters refined using 61 restraints

END

WGHT      0.0357      3.0079

REM Highest difference peak  1.796,  deepest hole -2.283,  1-sigma level  0.189
Q1    1   0.2755  0.5845  0.3432  11.00000  0.05    1.80
Q2    1   0.2652  0.3916  0.3497  11.00000  0.05    1.66
Q3    1   0.2320  0.4306  0.2622  11.00000  0.05    0.79
Q4    1   0.2807  0.5537  0.4437  11.00000  0.05    0.70
Q5    1   0.3222  0.5443  0.3580  11.00000  0.05    0.66
Q6    1   0.1782  0.5408  0.3571  11.00000  0.05    0.66
;
_shelx_res_checksum              47646
_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
;
