# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2020

####################################################################### 
# 
# 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_T2PbCl4_93K
_database_code_depnum_ccdc_archive 'CCDC 2024190'
loop_
_audit_author_name
_audit_author_address
'Yuan-Yuan Guo'
;University of St Andrews
United Kingdom
;
_audit_update_record             
;
2020-08-20 deposited with the CCDC.	2020-11-17 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT112_T2PbCl4_93K         
;
PROBLEM: ADDSYM Detects New (Pseudo) Symm. Elem         n        100 %Fit
RESPONSE: Caused by chiral space group, P212121
;
_vrf_PLAT112_T2PbCl4_93K_2       
;
PROBLEM: ADDSYM Detects New (Pseudo) Symm. Elem         n        100 %Fit
RESPONSE: Caused by chiral space group, P212121
;
_vrf_PLAT927_T2PbCl4_93K         
;
PROBLEM: Reported and Calculated  wR2 Differ by .........     0.0075 Check
RESPONSE: Caused by the units Z value manually multiply by four, to keep the formula be consistent to the other temperatures'
;
_vrf_PLAT987_T2PbCl4_93K         
;
PROBLEM: The Flack x is >> 0 -  Do a BASF/TWIN Refinement     Please Check
RESPONSE: Caused by chiral space group, P212121
;
_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'Cl12 Pb3, 6(C2 H4 N3)'
_chemical_formula_sum            'C4 H8 Cl4 N6 Pb'
_chemical_formula_weight         489.15

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Pb Pb -3.3944 10.1111 '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'
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'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'

_cell_length_a                   8.313(4)
_cell_length_b                   21.426(9)
_cell_length_c                   21.959(8)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3911(3)
_cell_formula_units_Z            12
_cell_measurement_temperature    93(2)
_cell_measurement_reflns_used    10045
_cell_measurement_theta_min      2.1
_cell_measurement_theta_max      27.4

_exptl_crystal_description       Platelet
_exptl_crystal_colour            Colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    2.492
_exptl_crystal_F_000             2688
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.01
_exptl_absorpt_coefficient_mu    13.739
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.412
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      93(2)
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Rotating Anode'
_diffrn_measurement_device_type  
;
Rigaku Pilatus 200K
;
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            50108
_diffrn_reflns_av_unetI/netI     0.0438
_diffrn_reflns_av_R_equivalents  0.0754
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         1.855
_diffrn_reflns_theta_max         25.348
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             7112
_reflns_number_gt                5237
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.773
_reflns_Friedel_fraction_max     0.993
_reflns_Friedel_fraction_full    0.996

_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.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Ortep for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0321P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 2052 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.497(14)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         7112
_refine_ls_number_parameters     406
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0407
_refine_ls_R_factor_gt           0.0314
_refine_ls_wR_factor_ref         0.0708
_refine_ls_wR_factor_gt          0.0690
_refine_ls_goodness_of_fit_ref   0.892
_refine_ls_restrained_S_all      0.892
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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 0.50835(13) 0.48563(2) 0.62787(3) 0.01398(13) Uani 1 1 d . . . . .
Pb2 Pb -0.00833(15) 0.48856(2) 0.79476(3) 0.01757(15) Uani 1 1 d . . . . .
Pb3 Pb 0.99055(14) 0.49675(3) 0.46119(3) 0.02156(17) Uani 1 1 d . . . . .
Cl1 Cl 0.5167(6) 0.62010(16) 0.62888(19) 0.0248(9) Uani 1 1 d . . . . .
Cl2 Cl 0.5191(6) 0.35312(16) 0.6286(2) 0.0307(10) Uani 1 1 d . . . . .
Cl3 Cl 0.6793(6) 0.48510(18) 0.7381(2) 0.0272(10) Uani 1 1 d . . . . .
Cl4 Cl 0.2365(6) 0.48362(17) 0.70219(19) 0.0219(10) Uani 1 1 d . . . . .
Cl5 Cl 1.2638(6) 0.48866(19) 0.5346(2) 0.0296(10) Uani 1 1 d . . . . .
Cl6 Cl 0.8214(6) 0.48596(18) 0.5715(2) 0.0283(10) Uani 1 1 d . . . . .
Cl7 Cl -0.0170(6) 0.62202(18) 0.78806(18) 0.0255(9) Uani 1 1 d . . . . .
Cl8 Cl -0.0188(6) 0.35567(17) 0.8048(2) 0.0269(9) Uani 1 1 d . . . . .
Cl9 Cl 0.2646(6) 0.4942(2) 0.8692(2) 0.0352(10) Uani 1 1 d . . . . .
Cl10 Cl -0.1786(6) 0.4998(2) 0.9049(2) 0.0368(10) Uani 1 1 d . . . . .
Cl11 Cl 0.9818(6) 0.36429(16) 0.45279(19) 0.0274(9) Uani 1 1 d . . . . .
Cl12 Cl 0.9817(6) 0.63090(17) 0.4706(2) 0.0285(9) Uani 1 1 d . . . . .
N1 N 0.898(2) 0.6334(7) 0.6304(8) 0.026(4) Uani 1 1 d . . . . .
H1 H 0.807434 0.614567 0.626714 0.032 Uiso 1 1 calc R U . . .
N2 N 0.912(2) 0.6955(8) 0.6409(8) 0.033(4) Uani 1 1 d . . . . .
N3 N 1.1478(19) 0.6494(8) 0.6362(8) 0.031(4) Uani 1 1 d . . . . .
H2 H 1.250473 0.644542 0.636366 0.037 Uiso 1 1 calc R U . . .
C1 C 1.067(2) 0.7035(10) 0.6460(9) 0.027(4) Uani 1 1 d . . . . .
H3 H 1.115741 0.741464 0.655152 0.033 Uiso 1 1 calc R U . . .
C2 C 1.037(2) 0.6048(7) 0.6264(8) 0.028(4) Uani 1 1 d . . . . .
H4 H 1.055459 0.562801 0.618385 0.034 Uiso 1 1 calc R U . . .
N4 N -0.0977(19) 0.3415(8) 0.6313(8) 0.029(4) Uani 1 1 d . . . . .
H5 H -0.186429 0.359528 0.621380 0.035 Uiso 1 1 calc R U . . .
N5 N -0.0893(19) 0.2825(8) 0.6576(8) 0.029(4) Uani 1 1 d . . . . .
N6 N 0.1516(18) 0.3247(6) 0.6429(7) 0.022(3) Uani 1 1 d . . . . .
H6 H 0.254466 0.329132 0.642545 0.026 Uiso 1 1 calc R U . . .
C3 C 0.067(2) 0.2740(8) 0.6635(10) 0.027(4) Uani 1 1 d . . . . .
H7 H 0.114311 0.238267 0.679547 0.033 Uiso 1 1 calc R U . . .
C4 C 0.042(2) 0.3662(8) 0.6233(8) 0.024(4) Uani 1 1 d . . . . .
H8 H 0.063412 0.405470 0.607123 0.028 Uiso 1 1 calc R U . . .
N7 N 0.603(2) 0.6361(8) 0.7898(7) 0.027(4) Uani 1 1 d . . . . .
H9 H 0.693823 0.617565 0.784135 0.033 Uiso 1 1 calc R U . . .
N8 N 0.586(2) 0.6989(8) 0.8037(7) 0.026(4) Uani 1 1 d . . . . .
N9 N 0.3513(19) 0.6516(8) 0.7976(7) 0.030(4) Uani 1 1 d . . . . .
H10 H 0.248814 0.646342 0.798600 0.036 Uiso 1 1 calc R U . . .
C5 C 0.433(2) 0.7050(10) 0.8071(9) 0.029(5) Uani 1 1 d . . . . .
H11 H 0.383230 0.742853 0.815479 0.034 Uiso 1 1 calc R U . . .
C6 C 0.462(2) 0.6090(8) 0.7863(8) 0.027(4) Uani 1 1 d . . . . .
H12 H 0.443894 0.567138 0.777495 0.033 Uiso 1 1 calc R U . . .
N10 N 0.599(2) 0.3425(9) 0.8068(8) 0.031(4) Uani 1 1 d . . . . .
H13 H 0.689006 0.360556 0.798577 0.037 Uiso 1 1 calc R U . . .
N11 N 0.5865(19) 0.2843(8) 0.8289(8) 0.028(4) Uani 1 1 d . . . . .
N12 N 0.3506(19) 0.3283(7) 0.8170(7) 0.028(4) Uani 1 1 d . . . . .
H14 H 0.247902 0.333314 0.816977 0.034 Uiso 1 1 calc R U . . .
C7 C 0.433(2) 0.2769(8) 0.8354(9) 0.023(4) Uani 1 1 d . . . . .
H15 H 0.384879 0.240965 0.850741 0.028 Uiso 1 1 calc R U . . .
C8 C 0.458(2) 0.3684(9) 0.7994(9) 0.030(5) Uani 1 1 d . . . . .
H16 H 0.438164 0.408197 0.784329 0.036 Uiso 1 1 calc R U . . .
N13 N 1.600(2) 0.3502(8) 0.4568(8) 0.033(4) Uani 1 1 d . . . . .
H17 H 1.689829 0.368217 0.448662 0.040 Uiso 1 1 calc R U . . .
N14 N 1.5872(19) 0.2913(8) 0.4779(8) 0.031(4) Uani 1 1 d . . . . .
N15 N 1.3514(19) 0.3349(8) 0.4665(8) 0.033(4) Uani 1 1 d . . . . .
H18 H 1.248682 0.339482 0.466605 0.039 Uiso 1 1 calc R U . . .
C9 C 1.432(2) 0.2824(9) 0.4832(9) 0.030(5) Uani 1 1 d . . . . .
H19 H 1.383956 0.245661 0.496527 0.036 Uiso 1 1 calc R U . . .
C10 C 1.457(2) 0.3773(9) 0.4501(9) 0.035(5) Uani 1 1 d . . . . .
H20 H 1.436086 0.417663 0.436638 0.041 Uiso 1 1 calc R U . . .
N16 N 1.602(2) 0.6445(8) 0.4715(8) 0.031(4) Uani 1 1 d . . . . .
H21 H 1.694276 0.627056 0.465662 0.037 Uiso 1 1 calc R U . . .
N17 N 1.584(2) 0.7051(8) 0.4880(8) 0.035(4) Uani 1 1 d . . . . .
N18 N 1.351(2) 0.6586(8) 0.4781(7) 0.033(4) Uani 1 1 d . . . . .
H22 H 1.248866 0.653287 0.478261 0.039 Uiso 1 1 calc R U . . .
C11 C 1.429(2) 0.7113(10) 0.4902(10) 0.038(5) Uani 1 1 d . . . . .
H23 H 1.377970 0.748723 0.499256 0.046 Uiso 1 1 calc R U . . .
C12 C 1.4629(19) 0.6151(8) 0.4656(7) 0.023(4) Uani 1 1 d . . . . .
H24 H 1.446077 0.573553 0.455064 0.027 Uiso 1 1 calc R U . . .


_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 Cl4 2.788(5) . ?
Pb1 Cl3 2.808(5) . ?
Pb1 Cl2 2.841(4) . ?
Pb1 Cl1 2.882(4) . ?
Pb1 Cl6 2.882(5) . ?
Pb1 Cl5 2.886(5) 1_455 ?
Pb2 Cl9 2.800(5) . ?
Pb2 Cl10 2.813(4) . ?
Pb2 Cl8 2.857(4) . ?
Pb2 Cl7 2.864(4) . ?
Pb2 Cl4 2.879(5) . ?
Pb2 Cl3 2.880(5) 1_455 ?
Pb3 Cl5 2.791(5) . ?
Pb3 Cl6 2.809(5) . ?
Pb3 Cl11 2.845(4) . ?
Pb3 Cl9 2.874(5) 2_664 ?
Pb3 Cl10 2.874(5) 2_564 ?
Pb3 Cl12 2.883(4) . ?
N1 C2 1.31(2) . ?
N1 N2 1.36(2) . ?
N2 C1 1.31(2) . ?
N3 C2 1.34(2) . ?
N3 C1 1.36(3) . ?
N4 C4 1.29(2) . ?
N4 N5 1.39(2) . ?
N5 C3 1.32(2) . ?
N6 C4 1.34(2) . ?
N6 C3 1.37(2) . ?
N7 C6 1.31(2) . ?
N7 N8 1.39(2) . ?
N8 C5 1.28(2) . ?
N9 C6 1.32(3) . ?
N9 C5 1.35(3) . ?
N10 C8 1.31(3) . ?
N10 N11 1.34(2) . ?
N11 C7 1.30(2) . ?
N12 C8 1.30(2) . ?
N12 C7 1.36(2) . ?
N13 C10 1.33(3) . ?
N13 N14 1.35(2) . ?
N14 C9 1.31(2) . ?
N15 C10 1.31(2) . ?
N15 C9 1.36(2) . ?
N16 C12 1.33(2) . ?
N16 N17 1.36(2) . ?
N17 C11 1.29(2) . ?
N18 C11 1.33(3) . ?
N18 C12 1.34(2) . ?

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
Cl4 Pb1 Cl3 84.57(15) . . ?
Cl4 Pb1 Cl2 90.39(12) . . ?
Cl3 Pb1 Cl2 88.59(13) . . ?
Cl4 Pb1 Cl1 91.75(12) . . ?
Cl3 Pb1 Cl1 89.15(12) . . ?
Cl2 Pb1 Cl1 176.73(14) . . ?
Cl4 Pb1 Cl6 169.58(13) . . ?
Cl3 Pb1 Cl6 85.04(18) . . ?
Cl2 Pb1 Cl6 88.65(13) . . ?
Cl1 Pb1 Cl6 88.80(12) . . ?
Cl4 Pb1 Cl5 81.08(18) . 1_455 ?
Cl3 Pb1 Cl5 165.58(14) . 1_455 ?
Cl2 Pb1 Cl5 92.78(13) . 1_455 ?
Cl1 Pb1 Cl5 90.00(12) . 1_455 ?
Cl6 Pb1 Cl5 109.33(16) . 1_455 ?
Cl9 Pb2 Cl10 84.36(15) . . ?
Cl9 Pb2 Cl8 91.31(14) . . ?
Cl10 Pb2 Cl8 90.18(14) . . ?
Cl9 Pb2 Cl7 90.41(14) . . ?
Cl10 Pb2 Cl7 86.92(14) . . ?
Cl8 Pb2 Cl7 176.48(15) . . ?
Cl9 Pb2 Cl4 80.85(18) . . ?
Cl10 Pb2 Cl4 165.06(15) . . ?
Cl8 Pb2 Cl4 92.27(12) . . ?
Cl7 Pb2 Cl4 91.05(12) . . ?
Cl9 Pb2 Cl3 169.75(14) . 1_455 ?
Cl10 Pb2 Cl3 85.40(16) . 1_455 ?
Cl8 Pb2 Cl3 88.87(13) . 1_455 ?
Cl7 Pb2 Cl3 88.90(13) . 1_455 ?
Cl4 Pb2 Cl3 109.38(15) . 1_455 ?
Cl5 Pb3 Cl6 84.51(16) . . ?
Cl5 Pb3 Cl11 89.79(13) . . ?
Cl6 Pb3 Cl11 87.77(12) . . ?
Cl5 Pb3 Cl9 80.42(17) . 2_664 ?
Cl6 Pb3 Cl9 164.93(15) . 2_664 ?
Cl11 Pb3 Cl9 92.27(13) . 2_664 ?
Cl5 Pb3 Cl10 169.91(14) . 2_564 ?
Cl6 Pb3 Cl10 85.48(17) . 2_564 ?
Cl11 Pb3 Cl10 88.58(14) . 2_564 ?
Cl9 Pb3 Cl10 109.59(15) 2_664 2_564 ?
Cl5 Pb3 Cl12 92.38(12) . . ?
Cl6 Pb3 Cl12 90.44(12) . . ?
Cl11 Pb3 Cl12 177.05(13) . . ?
Cl9 Pb3 Cl12 90.07(14) 2_664 . ?
Cl10 Pb3 Cl12 88.94(14) 2_564 . ?
Pb1 Cl3 Pb2 145.95(19) . 1_655 ?
Pb1 Cl4 Pb2 170.41(19) . . ?
Pb3 Cl5 Pb1 169.9(2) . 1_655 ?
Pb3 Cl6 Pb1 145.3(2) . . ?
Pb2 Cl9 Pb3 170.9(2) . 2_665 ?
Pb2 Cl10 Pb3 145.70(19) . 2_565 ?
C2 N1 N2 113.4(15) . . ?
C1 N2 N1 103.1(17) . . ?
C2 N3 C1 107.1(16) . . ?
N2 C1 N3 111(2) . . ?
N1 C2 N3 105.1(14) . . ?
C4 N4 N5 112.5(15) . . ?
C3 N5 N4 102.4(16) . . ?
C4 N6 C3 106.5(16) . . ?
N5 C3 N6 111.3(18) . . ?
N4 C4 N6 107.2(15) . . ?
C6 N7 N8 110.6(15) . . ?
C5 N8 N7 102.3(17) . . ?
C6 N9 C5 105.2(16) . . ?
N8 C5 N9 114(2) . . ?
N7 C6 N9 107.9(15) . . ?
C8 N10 N11 111.6(16) . . ?
C7 N11 N10 103.4(16) . . ?
C8 N12 C7 106.2(17) . . ?
N11 C7 N12 111.3(18) . . ?
N12 C8 N10 107.5(16) . . ?
C10 N13 N14 112.1(16) . . ?
C9 N14 N13 104.1(16) . . ?
C10 N15 C9 108.5(17) . . ?
N14 C9 N15 109.9(19) . . ?
N15 C10 N13 105.3(16) . . ?
C12 N16 N17 112.4(16) . . ?
C11 N17 N16 102.8(19) . . ?
C11 N18 C12 107.1(16) . . ?
N17 C11 N18 113(2) . . ?
N16 C12 N18 104.7(14) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N1 H1 Cl1 0.86 2.42 3.185(17) 148.5 . yes
N3 H2 Cl1 0.86 2.28 3.135(16) 172.3 1_655 yes
N4 H5 Cl2 0.86 2.46 3.196(17) 144.4 1_455 yes
N4 H5 Cl6 0.86 2.92 3.428(17) 119.4 1_455 yes
N6 H6 Cl2 0.86 2.28 3.130(16) 170.0 . yes
N7 H9 Cl7 0.86 2.41 3.171(18) 148.3 1_655 yes
N10 H13 Cl3 0.86 2.98 3.472(18) 118.2 . yes
N10 H13 Cl8 0.86 2.43 3.188(18) 146.6 1_655 yes
N12 H14 Cl8 0.86 2.28 3.137(17) 171.6 . yes
N13 H17 Cl10 0.86 2.99 3.472(18) 117.6 2_664 yes
N13 H17 Cl11 0.86 2.43 3.191(18) 147.7 1_655 yes
N15 H18 Cl11 0.86 2.30 3.151(17) 169.7 . yes
N16 H21 Cl12 0.86 2.39 3.166(17) 149.9 1_655 yes
N18 H22 Cl12 0.86 2.28 3.135(17) 173.6 . yes

_refine_diff_density_max         1.780
_refine_diff_density_min         -2.181
_refine_diff_density_rms         0.158

####################################################################### 
# 
# 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_T2PbCl4_298K
_database_code_depnum_ccdc_archive 'CCDC 2024193'
loop_
_audit_author_name
_audit_author_address
'Yuan-Yuan Guo'
;University of St Andrews
United Kingdom
;
_audit_update_record             
;
2020-08-20 deposited with the CCDC.	2020-11-17 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT242_T2PbCl4_298K        
;
PROBLEM: Low    'MainMol' Ueq as Compared to Neighbors of        Pb1 Check
RESPONSE: Caused by the disorder of Cl, see text
;
_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'Cl4 Pb, 2(C2 H4 N3)'
_chemical_formula_sum            'C4 H8 Cl4 N6 Pb'
_chemical_formula_weight         489.15

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Pb Pb -3.3944 10.1111 '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'
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'

_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'

_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.
;

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                   8.3092(5)
_cell_length_b                   7.5086(5)
_cell_length_c                   21.5925(17)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1347.17(16)
_cell_formula_units_Z            4
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    948
_cell_measurement_theta_min      1.9
_cell_measurement_theta_max      27.5

_exptl_crystal_description       Platelet
_exptl_crystal_colour            Colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    2.412
_exptl_crystal_F_000             896
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.06
_exptl_absorpt_coefficient_mu    13.296
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.394
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Sealed Tube'
_diffrn_measurement_device_type  
;
Rigaku Mercury2 (2x2 bin mode)
;
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            5443
_diffrn_reflns_av_unetI/netI     0.0255
_diffrn_reflns_av_R_equivalents  0.0491
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         1.886
_diffrn_reflns_theta_max         24.987
_diffrn_reflns_theta_full        24.987
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.994
_reflns_number_total             653
_reflns_number_gt                636
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Ortep for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0234P)²+6.7571P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_extinction_coef       0.0063(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         653
_refine_ls_number_parameters     46
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0250
_refine_ls_R_factor_gt           0.0240
_refine_ls_wR_factor_ref         0.0559
_refine_ls_wR_factor_gt          0.0555
_refine_ls_goodness_of_fit_ref   1.229
_refine_ls_restrained_S_all      1.228
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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 0.15445(5) 0.750000 0.0276(2) Uani 1 4 d S T P . .
Cl1 Cl 0.500000 0.1596(4) 0.61726(11) 0.0548(6) Uani 1 2 d S T P . .
Cl2 Cl 0.7338(5) 0.4185(6) 0.750000 0.1224(18) Uani 1 2 d S T P . .
C1 C 0.000000 0.1506(15) 0.6333(6) 0.071(3) Uani 1 2 d S T P . .
H1 H 0.000000 0.122003 0.675250 0.085 Uiso 1 2 calc R U P . .
N1 N 0.1235(8) 0.1741(9) 0.5988(4) 0.0674(19) Uani 1 1 d D . . . .
H2 H 0.227(4) 0.168(13) 0.611(5) 0.10(3) Uiso 1 1 d D . . . .
N2 N 0.0791(9) 0.2140(13) 0.5421(4) 0.079(2) Uani 0.5 1 d . . P . .
H3 H 0.141177 0.235844 0.511180 0.094 Uiso 0.5 1 calc R U P . .
C2 C 0.0791(9) 0.2140(13) 0.5421(4) 0.079(2) Uani 0.5 1 d . . P . .


_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 2.776(3) 3_656 ?
Pb1 Cl2 2.776(3) . ?
Pb1 Cl2 2.834(3) 5_445 ?
Pb1 Cl2 2.834(3) 7_646 ?
Pb1 Cl1 2.866(2) 10_557 ?
Pb1 Cl1 2.866(2) . ?
C1 N1 1.280(10) . ?
C1 N1 1.281(10) 12 ?
N1 N2 1.313(10) . ?
N2 N2 1.315(15) 12 ?

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 88.8(2) 3_656 . ?
Cl2 Pb1 Cl2 84.277(8) 3_656 5_445 ?
Cl2 Pb1 Cl2 173.1(2) . 5_445 ?
Cl2 Pb1 Cl2 173.1(2) 3_656 7_646 ?
Cl2 Pb1 Cl2 84.277(8) . 7_646 ?
Cl2 Pb1 Cl2 102.6(2) 5_445 7_646 ?
Cl2 Pb1 Cl1 89.45(4) 3_656 10_557 ?
Cl2 Pb1 Cl1 89.45(4) . 10_557 ?
Cl2 Pb1 Cl1 90.48(3) 5_445 10_557 ?
Cl2 Pb1 Cl1 90.48(3) 7_646 10_557 ?
Cl2 Pb1 Cl1 89.45(4) 3_656 . ?
Cl2 Pb1 Cl1 89.45(4) . . ?
Cl2 Pb1 Cl1 90.48(3) 5_445 . ?
Cl2 Pb1 Cl1 90.48(3) 7_646 . ?
Cl1 Pb1 Cl1 178.45(11) 10_557 . ?
Pb1 Cl2 Pb1 173.1(2) . 5 ?
N1 C1 N1 106.5(11) . 12 ?
C1 N1 N2 110.5(7) . . ?
N1 N2 N2 106.3(4) . 12 ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N1 H2 Cl1 0.90(2) 2.27(3) 3.156(6) 167(10) . yes
N2 H3 N2 0.86 2.62 3.416(14) 154.2 13_556 yes

_refine_diff_density_max         1.091
_refine_diff_density_min         -1.261
_refine_diff_density_rms         0.171

####################################################################### 
# 
# 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_T2PbBr4-II_173K
_database_code_depnum_ccdc_archive 'CCDC 2024194'
loop_
_audit_author_name
_audit_author_address
'Yuan-Yuan Guo'
;University of St Andrews
United Kingdom
;
_audit_update_record             
;
2020-08-20 deposited with the CCDC.	2020-11-17 downloaded from the CCDC.
;
_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'Br4 Pb, 2(C2 H4 N3)'
_chemical_formula_sum            'C4 H8 Br4 N6 Pb'
_chemical_formula_weight         666.99

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 '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'
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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_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.
;

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                   9.6451(7)
_cell_length_b                   8.4001(5)
_cell_length_c                   8.3932(5)
_cell_angle_alpha                90
_cell_angle_beta                 97.016(8)
_cell_angle_gamma                90
_cell_volume                     674.92(8)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    921
_cell_measurement_theta_min      2.4
_cell_measurement_theta_max      27.5

_exptl_crystal_description       Block
_exptl_crystal_colour            Yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    3.282
_exptl_crystal_F_000             592
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.13
_exptl_absorpt_coefficient_mu    24.319
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.515
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Sealed Tube'
_diffrn_measurement_device_type  
;
Rigaku Mercury2 (2x2 bin mode)
;
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            5445
_diffrn_reflns_av_unetI/netI     0.0347
_diffrn_reflns_av_R_equivalents  0.0484
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         3.227
_diffrn_reflns_theta_max         24.988
_diffrn_reflns_theta_full        24.988
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             1172
_reflns_number_gt                1076
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Ortep for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0438P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_extinction_coef       0.0057(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         1172
_refine_ls_number_parameters     71
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0285
_refine_ls_R_factor_gt           0.0263
_refine_ls_wR_factor_ref         0.0675
_refine_ls_wR_factor_gt          0.0668
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_restrained_S_all      1.082
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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 0.500000 0.500000 0.01156(18) Uani 1 2 d S . P . .
Br1 Br 0.19187(6) 0.56392(8) 0.44150(7) 0.0198(2) Uani 1 1 d . . . . .
Br2 Br 0.49181(7) 0.28205(8) 0.78074(8) 0.0218(2) Uani 1 1 d . . . . .
N1 N 0.2124(7) 0.4730(7) 1.0530(8) 0.0257(14) Uani 1 1 d . . . . .
H1 H 0.253709 0.511912 1.140998 0.031 Uiso 1 1 calc R U . . .
N2 N 0.1154(6) 0.3565(7) 1.0460(7) 0.0271(13) Uani 1 1 d . . . . .
N3 N 0.1538(6) 0.4337(7) 0.8066(7) 0.0226(13) Uani 1 1 d . . . . .
H2 H 0.147345 0.439191 0.703612 0.027 Uiso 1 1 calc R U . . .
C1 C 0.0813(7) 0.3352(8) 0.8930(8) 0.0237(15) Uani 1 1 d . . . . .
H1A H 0.015549 0.261677 0.848624 0.028 Uiso 1 1 calc R U . . .
C2 C 0.2363(8) 0.5198(8) 0.9094(9) 0.0227(16) Uani 1 1 d . . . . .
H2A H 0.298785 0.597890 0.885369 0.027 Uiso 1 1 calc R U . . .


_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 Br2 2.9926(6) . ?
Pb1 Br2 2.9926(6) 3_666 ?
Pb1 Br2 2.9951(6) 4_565 ?
Pb1 Br2 2.9951(6) 2_656 ?
Pb1 Br1 3.0009(6) . ?
Pb1 Br1 3.0009(6) 3_666 ?
N1 C2 1.314(10) . ?
N1 N2 1.350(9) . ?
N2 C1 1.298(9) . ?
N3 C2 1.316(10) . ?
N3 C1 1.350(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
Br2 Pb1 Br2 180.0 . 3_666 ?
Br2 Pb1 Br2 89.920(6) . 4_565 ?
Br2 Pb1 Br2 90.080(6) 3_666 4_565 ?
Br2 Pb1 Br2 90.080(6) . 2_656 ?
Br2 Pb1 Br2 89.920(6) 3_666 2_656 ?
Br2 Pb1 Br2 180.00(2) 4_565 2_656 ?
Br2 Pb1 Br1 96.744(18) . . ?
Br2 Pb1 Br1 83.257(18) 3_666 . ?
Br2 Pb1 Br1 95.147(18) 4_565 . ?
Br2 Pb1 Br1 84.853(18) 2_656 . ?
Br2 Pb1 Br1 83.256(19) . 3_666 ?
Br2 Pb1 Br1 96.743(19) 3_666 3_666 ?
Br2 Pb1 Br1 84.853(18) 4_565 3_666 ?
Br2 Pb1 Br1 95.147(18) 2_656 3_666 ?
Br1 Pb1 Br1 180.0 . 3_666 ?
Pb1 Br2 Pb1 165.12(3) . 2_646 ?
C2 N1 N2 112.0(6) . . ?
C1 N2 N1 103.5(6) . . ?
C2 N3 C1 107.2(6) . . ?
N2 C1 N3 111.2(6) . . ?
N1 C2 N3 106.1(6) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N1 H1 Br1 0.86 2.70 3.379(7) 137.1 1_556 yes
N1 H1 Br2 0.86 3.01 3.654(6) 133.3 3_667 yes
N3 H2 Br1 0.86 2.52 3.316(6) 154.2 . yes

_refine_diff_density_max         2.279
_refine_diff_density_min         -1.081
_refine_diff_density_rms         0.322

####################################################################### 
# 
# 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_T2PbCl4_173K
_database_code_depnum_ccdc_archive 'CCDC 2024192'
loop_
_audit_author_name
_audit_author_address
'Yuan-Yuan Guo'
;University of St Andrews
United Kingdom
;
_audit_update_record             
;
2020-08-20 deposited with the CCDC.	2020-11-17 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT242_T2PbCl4_173K        
;
PROBLEM: Low    'MainMol' Ueq as Compared to Neighbors of        Pb1 Check
RESPONSE: Caused by the disorder of Cl, see text
;
_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'Cl4 Pb, 2(C2 H4 N3)'
_chemical_formula_sum            'C4 H8 Cl4 N6 Pb'
_chemical_formula_weight         489.15

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Pb Pb -3.3944 10.1111 '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'
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'

_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'

_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.
;

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                   8.3060(5)
_cell_length_b                   7.4959(5)
_cell_length_c                   21.5814(17)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1343.68(16)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    961
_cell_measurement_theta_min      1.9
_cell_measurement_theta_max      27.5

_exptl_crystal_description       Platelet
_exptl_crystal_colour            Colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    2.418
_exptl_crystal_F_000             896
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.06
_exptl_absorpt_coefficient_mu    13.331
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.403
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Sealed Tube'
_diffrn_measurement_device_type  
;
Rigaku Mercury2 (2x2 bin mode)
;
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            5412
_diffrn_reflns_av_unetI/netI     0.0269
_diffrn_reflns_av_R_equivalents  0.0506
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         1.887
_diffrn_reflns_theta_max         24.989
_diffrn_reflns_theta_full        24.989
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.994
_reflns_number_total             651
_reflns_number_gt                624
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Ortep for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0192P)²+13.5951P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_extinction_coef       0.0084(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         651
_refine_ls_number_parameters     46
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0288
_refine_ls_R_factor_gt           0.0269
_refine_ls_wR_factor_ref         0.0623
_refine_ls_wR_factor_gt          0.0616
_refine_ls_goodness_of_fit_ref   1.235
_refine_ls_restrained_S_all      1.234
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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 0.15139(6) 0.750000 0.0271(3) Uani 1 4 d S T P . .
Cl1 Cl 0.500000 0.1567(4) 0.61714(12) 0.0530(7) Uani 1 2 d S T P . .
Cl2 Cl 0.7326(6) 0.4152(8) 0.750000 0.127(2) Uani 1 2 d S T P . .
C1 C 0.000000 0.1467(18) 0.6329(7) 0.070(4) Uani 1 2 d S T P . .
H1 H 0.000000 0.115534 0.674593 0.085 Uiso 1 2 calc R U P . .
N1 N 0.1245(9) 0.1724(10) 0.5984(4) 0.066(2) Uani 1 1 d D . . . .
H2 H 0.227(5) 0.156(13) 0.611(5) 0.08(3) Uiso 1 1 d D . . . .
N2 N 0.0791(10) 0.2124(14) 0.5420(4) 0.074(2) Uani 0.5 1 d . . P . .
H3 H 0.140913 0.234421 0.510953 0.089 Uiso 0.5 1 calc R U P . .
C2 C 0.0791(10) 0.2124(14) 0.5420(4) 0.074(2) Uani 0.5 1 d . . P . .


_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 2.764(3) 3_656 ?
Pb1 Cl2 2.764(3) . ?
Pb1 Cl2 2.841(3) 5_445 ?
Pb1 Cl2 2.841(3) 7_646 ?
Pb1 Cl1 2.868(3) . ?
Pb1 Cl1 2.868(3) 10_557 ?
C1 N1 1.288(12) 12 ?
C1 N1 1.288(12) . ?
N1 N2 1.310(12) . ?
N2 N2 1.314(17) 12 ?

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 88.7(3) 3_656 . ?
Cl2 Pb1 Cl2 84.228(10) 3_656 5_445 ?
Cl2 Pb1 Cl2 172.9(3) . 5_445 ?
Cl2 Pb1 Cl2 172.9(3) 3_656 7_646 ?
Cl2 Pb1 Cl2 84.227(10) . 7_646 ?
Cl2 Pb1 Cl2 102.9(3) 5_445 7_646 ?
Cl2 Pb1 Cl1 89.43(5) 3_656 . ?
Cl2 Pb1 Cl1 89.43(5) . . ?
Cl2 Pb1 Cl1 90.50(4) 5_445 . ?
Cl2 Pb1 Cl1 90.50(4) 7_646 . ?
Cl2 Pb1 Cl1 89.43(5) 3_656 10_557 ?
Cl2 Pb1 Cl1 89.43(5) . 10_557 ?
Cl2 Pb1 Cl1 90.50(4) 5_445 10_557 ?
Cl2 Pb1 Cl1 90.50(4) 7_646 10_557 ?
Cl1 Pb1 Cl1 178.40(13) . 10_557 ?
Pb1 Cl2 Pb1 172.9(3) . 5 ?
N1 C1 N1 106.8(12) 12 . ?
C1 N1 N2 109.9(8) . . ?
N1 N2 N2 106.7(5) . 12 ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N1 H2 Cl1 0.91(2) 2.27(4) 3.147(7) 163(9) . yes
N2 H3 N2 0.86 2.62 3.415(16) 153.9 13_556 yes

_refine_diff_density_max         1.191
_refine_diff_density_min         -1.471
_refine_diff_density_rms         0.198

####################################################################### 
# 
# 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_T2PbCl4_125K
_database_code_depnum_ccdc_archive 'CCDC 2024191'
loop_
_audit_author_name
_audit_author_address
'Yuan-Yuan Guo'
;University of St Andrews
United Kingdom
;
_audit_update_record             
;
2020-08-20 deposited with the CCDC.	2020-11-17 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT112_T2PbCl4_125K        
;
PROBLEM: ADDSYM Detects New (Pseudo) Symm. Elem         n        100 %Fit
RESPONSE: Caused by chiral space group, P212121
;
_vrf_PLAT112_T2PbCl4_125K_2      
;
PROBLEM: ADDSYM Detects New (Pseudo) Symm. Elem         n        100 %Fit
RESPONSE: Caused by chiral space group, P212121
;
_vrf_PLAT972_T2PbCl4_125K        
;
PROBLEM: Check Calcd Resid. Dens.  0.75A   From Pb1            -3.01 eA-3
RESPONSE: Caused by massive atom Pb
;
_vrf_PLAT987_T2PbCl4_125K        
;
PROBLEM: The Flack x is >> 0 -  Do a BASF/TWIN Refinement     Please Check
RESPONSE: Caused by chiral space group, P212121
;
_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'Cl12 Pb3, 6(C2 H4 N3)'
_chemical_formula_sum            'C4 H8 Cl4 N6 Pb'
_chemical_formula_weight         489.15

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Pb Pb -3.3944 10.1111 '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'
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'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'

_cell_length_a                   8.321(5)
_cell_length_b                   21.465(12)
_cell_length_c                   22.084(10)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3944(4)
_cell_formula_units_Z            12
_cell_measurement_temperature    125(2)
_cell_measurement_reflns_used    10371
_cell_measurement_theta_min      3
_cell_measurement_theta_max      27.4

_exptl_crystal_description       Platelet
_exptl_crystal_colour            Colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    2.471
_exptl_crystal_F_000             2688
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.01
_exptl_absorpt_coefficient_mu    13.623
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.255
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      125(2)
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Rotating Anode'
_diffrn_measurement_device_type  
;
Rigaku Pilatus 200K
;
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            49442
_diffrn_reflns_av_unetI/netI     0.0531
_diffrn_reflns_av_R_equivalents  0.0895
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         2.616
_diffrn_reflns_theta_max         24.998
_diffrn_reflns_theta_full        24.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             6913
_reflns_number_gt                4720
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.770
_reflns_Friedel_fraction_max     0.995
_reflns_Friedel_fraction_full    0.995

_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.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Ortep for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0290P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 1804 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.44(3)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         6913
_refine_ls_number_parameters     406
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0454
_refine_ls_R_factor_gt           0.0339
_refine_ls_wR_factor_ref         0.0717
_refine_ls_wR_factor_gt          0.0692
_refine_ls_goodness_of_fit_ref   0.868
_refine_ls_restrained_S_all      0.868
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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 0.50728(13) 0.48629(3) 0.62831(3) 0.01518(15) Uani 1 1 d . . . . .
Pb2 Pb -0.00732(15) 0.48880(3) 0.79510(3) 0.01912(18) Uani 1 1 d . . . . .
Pb3 Pb 0.99162(15) 0.49686(3) 0.46164(3) 0.0249(2) Uani 1 1 d . . . . .
Cl1 Cl 0.5145(6) 0.6204(2) 0.6297(2) 0.0280(11) Uani 1 1 d . . . . .
Cl2 Cl 0.5178(6) 0.3538(2) 0.6291(3) 0.0368(13) Uani 1 1 d . . . . .
Cl3 Cl 0.6829(6) 0.4860(3) 0.7373(3) 0.0333(12) Uani 1 1 d . . . . .
Cl4 Cl 0.2364(7) 0.4846(2) 0.7028(2) 0.0262(12) Uani 1 1 d . . . . .
Cl5 Cl 1.2638(7) 0.4890(3) 0.5354(3) 0.0348(12) Uani 1 1 d . . . . .
Cl6 Cl 0.8180(6) 0.4863(3) 0.5705(3) 0.0327(12) Uani 1 1 d . . . . .
Cl7 Cl -0.0150(6) 0.6226(2) 0.7887(2) 0.0289(11) Uani 1 1 d . . . . .
Cl8 Cl -0.0162(7) 0.3560(2) 0.8048(2) 0.0318(11) Uani 1 1 d . . . . .
Cl9 Cl 0.2647(7) 0.4944(3) 0.8697(3) 0.0417(14) Uani 1 1 d . . . . .
Cl10 Cl -0.1822(7) 0.4992(3) 0.9036(3) 0.0460(15) Uani 1 1 d . . . . .
Cl11 Cl 0.9845(6) 0.3645(2) 0.4538(2) 0.0324(11) Uani 1 1 d . . . . .
Cl12 Cl 0.9832(6) 0.6310(2) 0.4708(2) 0.0321(11) Uani 1 1 d . . . . .
N1 N 0.894(2) 0.6339(8) 0.6308(9) 0.030(4) Uani 1 1 d . . . . .
H1 H 0.802969 0.615530 0.627058 0.036 Uiso 1 1 calc R U . . .
N2 N 0.910(2) 0.6968(8) 0.6413(9) 0.040(5) Uani 1 1 d . . . . .
N3 N 1.145(2) 0.6484(9) 0.6359(9) 0.035(5) Uani 1 1 d . . . . .
H2 H 1.247918 0.643320 0.635572 0.042 Uiso 1 1 calc R U . . .
C1 C 1.066(2) 0.7036(10) 0.6458(10) 0.031(5) Uani 1 1 d . . . . .
H3 H 1.116511 0.741169 0.654574 0.038 Uiso 1 1 calc R U . . .
C2 C 1.035(2) 0.6039(10) 0.6270(10) 0.032(5) Uani 1 1 d . . . . .
H4 H 1.052906 0.561795 0.619766 0.039 Uiso 1 1 calc R U . . .
N4 N -0.101(2) 0.3426(9) 0.6316(9) 0.038(5) Uani 1 1 d . . . . .
H5 H -0.190057 0.360728 0.622783 0.046 Uiso 1 1 calc R U . . .
N5 N -0.089(2) 0.2821(8) 0.6574(9) 0.033(4) Uani 1 1 d . . . . .
N6 N 0.150(2) 0.3258(8) 0.6432(8) 0.031(4) Uani 1 1 d . . . . .
H6 H 0.252403 0.330334 0.642825 0.037 Uiso 1 1 calc R U . . .
C3 C 0.065(2) 0.2766(10) 0.6638(11) 0.032(5) Uani 1 1 d . . . . .
H7 H 0.112837 0.241761 0.681163 0.039 Uiso 1 1 calc R U . . .
C4 C 0.037(3) 0.3665(11) 0.6233(11) 0.039(6) Uani 1 1 d . . . . .
H8 H 0.057740 0.405334 0.606347 0.046 Uiso 1 1 calc R U . . .
N7 N 0.603(2) 0.6364(8) 0.7906(8) 0.028(4) Uani 1 1 d . . . . .
H9 H 0.693762 0.618564 0.784136 0.034 Uiso 1 1 calc R U . . .
N8 N 0.587(2) 0.6986(9) 0.8052(8) 0.033(5) Uani 1 1 d . . . . .
N9 N 0.353(2) 0.6510(9) 0.7991(8) 0.030(4) Uani 1 1 d . . . . .
H10 H 0.250990 0.645776 0.799799 0.036 Uiso 1 1 calc R U . . .
C5 C 0.434(3) 0.7040(10) 0.8092(11) 0.039(6) Uani 1 1 d . . . . .
H11 H 0.383408 0.741473 0.818199 0.047 Uiso 1 1 calc R U . . .
C6 C 0.466(2) 0.6078(9) 0.7876(9) 0.028(5) Uani 1 1 d . . . . .
H12 H 0.449587 0.565846 0.779251 0.034 Uiso 1 1 calc R U . . .
N10 N 0.602(2) 0.3424(9) 0.8064(9) 0.034(5) Uani 1 1 d . . . . .
H13 H 0.692560 0.359770 0.797715 0.040 Uiso 1 1 calc R U . . .
N11 N 0.589(2) 0.2854(9) 0.8284(10) 0.038(5) Uani 1 1 d . . . . .
N12 N 0.353(2) 0.3293(8) 0.8160(8) 0.033(4) Uani 1 1 d . . . . .
H14 H 0.250311 0.334413 0.815810 0.040 Uiso 1 1 calc R U . . .
C7 C 0.433(2) 0.2770(9) 0.8340(10) 0.025(4) Uani 1 1 d . . . . .
H15 H 0.384042 0.240751 0.848116 0.030 Uiso 1 1 calc R U . . .
C8 C 0.460(2) 0.3699(9) 0.7993(9) 0.026(5) Uani 1 1 d . . . . .
H16 H 0.440448 0.410098 0.785291 0.031 Uiso 1 1 calc R U . . .
N13 N 1.603(2) 0.3495(10) 0.4583(10) 0.041(5) Uani 1 1 d . . . . .
H17 H 1.692749 0.367393 0.450308 0.050 Uiso 1 1 calc R U . . .
N14 N 1.590(2) 0.2924(9) 0.4785(9) 0.040(5) Uani 1 1 d . . . . .
N15 N 1.353(2) 0.3356(9) 0.4670(9) 0.040(5) Uani 1 1 d . . . . .
H18 H 1.250890 0.340761 0.467476 0.049 Uiso 1 1 calc R U . . .
C9 C 1.433(2) 0.2824(10) 0.4824(10) 0.032(5) Uani 1 1 d . . . . .
H19 H 1.385091 0.245041 0.493731 0.038 Uiso 1 1 calc R U . . .
C10 C 1.459(3) 0.3768(11) 0.4517(10) 0.037(5) Uani 1 1 d . . . . .
H20 H 1.439248 0.417260 0.438613 0.044 Uiso 1 1 calc R U . . .
N16 N 1.603(2) 0.6446(9) 0.4718(8) 0.035(5) Uani 1 1 d . . . . .
H21 H 1.694648 0.627407 0.465773 0.042 Uiso 1 1 calc R U . . .
N17 N 1.586(2) 0.7055(9) 0.4886(9) 0.041(5) Uani 1 1 d . . . . .
N18 N 1.353(2) 0.6582(9) 0.4785(8) 0.036(5) Uani 1 1 d . . . . .
H22 H 1.251023 0.652780 0.478932 0.043 Uiso 1 1 calc R U . . .
C11 C 1.431(3) 0.7102(11) 0.4903(11) 0.051(7) Uani 1 1 d . . . . .
H23 H 1.377988 0.747402 0.499060 0.061 Uiso 1 1 calc R U . . .
C12 C 1.467(2) 0.6147(10) 0.4654(9) 0.032(5) Uani 1 1 d . . . . .
H24 H 1.451260 0.573286 0.454562 0.038 Uiso 1 1 calc R U . . .


_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 Cl4 2.790(5) . ?
Pb1 Cl3 2.815(5) . ?
Pb1 Cl2 2.846(5) . ?
Pb1 Cl1 2.879(5) . ?
Pb1 Cl6 2.883(5) . ?
Pb1 Cl5 2.885(6) 1_455 ?
Pb2 Cl9 2.802(6) . ?
Pb2 Cl10 2.812(6) . ?
Pb2 Cl8 2.860(5) . ?
Pb2 Cl7 2.876(5) . ?
Pb2 Cl4 2.877(5) . ?
Pb2 Cl3 2.878(5) 1_455 ?
Pb3 Cl5 2.794(6) . ?
Pb3 Cl6 2.813(5) . ?
Pb3 Cl11 2.848(5) . ?
Pb3 Cl9 2.876(6) 2_664 ?
Pb3 Cl10 2.877(6) 2_564 ?
Pb3 Cl12 2.888(5) . ?
N1 C2 1.34(3) . ?
N1 N2 1.38(2) . ?
N2 C1 1.31(2) . ?
N3 C2 1.34(3) . ?
N3 C1 1.38(3) . ?
N4 C4 1.27(3) . ?
N4 N5 1.42(2) . ?
N5 C3 1.30(2) . ?
N6 C3 1.35(3) . ?
N6 C4 1.35(3) . ?
N7 C6 1.29(2) . ?
N7 N8 1.38(2) . ?
N8 C5 1.28(3) . ?
N9 C5 1.34(3) . ?
N9 C6 1.34(3) . ?
N10 N11 1.32(2) . ?
N10 C8 1.34(3) . ?
N11 C7 1.32(2) . ?
N12 C8 1.30(2) . ?
N12 C7 1.36(3) . ?
N13 N14 1.31(3) . ?
N13 C10 1.34(3) . ?
N14 C9 1.32(2) . ?
N15 C10 1.29(3) . ?
N15 C9 1.36(3) . ?
N16 C12 1.31(2) . ?
N16 N17 1.37(2) . ?
N17 C11 1.30(3) . ?
N18 C11 1.31(3) . ?
N18 C12 1.36(3) . ?

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
Cl4 Pb1 Cl3 85.15(17) . . ?
Cl4 Pb1 Cl2 90.45(15) . . ?
Cl3 Pb1 Cl2 88.63(16) . . ?
Cl4 Pb1 Cl1 91.35(15) . . ?
Cl3 Pb1 Cl1 88.98(15) . . ?
Cl2 Pb1 Cl1 176.88(15) . . ?
Cl4 Pb1 Cl6 170.15(15) . . ?
Cl3 Pb1 Cl6 85.0(2) . . ?
Cl2 Pb1 Cl6 88.59(15) . . ?
Cl1 Pb1 Cl6 89.20(15) . . ?
Cl4 Pb1 Cl5 81.5(2) . 1_455 ?
Cl3 Pb1 Cl5 166.60(17) . 1_455 ?
Cl2 Pb1 Cl5 92.67(16) . 1_455 ?
Cl1 Pb1 Cl5 90.12(15) . 1_455 ?
Cl6 Pb1 Cl5 108.33(18) . 1_455 ?
Cl9 Pb2 Cl10 85.05(18) . . ?
Cl9 Pb2 Cl8 91.11(16) . . ?
Cl10 Pb2 Cl8 90.13(17) . . ?
Cl9 Pb2 Cl7 90.22(17) . . ?
Cl10 Pb2 Cl7 87.16(16) . . ?
Cl8 Pb2 Cl7 176.86(16) . . ?
Cl9 Pb2 Cl4 81.3(2) . . ?
Cl10 Pb2 Cl4 166.17(17) . . ?
Cl8 Pb2 Cl4 92.28(15) . . ?
Cl7 Pb2 Cl4 90.73(15) . . ?
Cl9 Pb2 Cl3 170.23(17) . 1_455 ?
Cl10 Pb2 Cl3 85.2(2) . 1_455 ?
Cl8 Pb2 Cl3 89.37(16) . 1_455 ?
Cl7 Pb2 Cl3 88.83(15) . 1_455 ?
Cl4 Pb2 Cl3 108.44(17) . 1_455 ?
Cl5 Pb3 Cl6 85.05(18) . . ?
Cl5 Pb3 Cl11 89.56(16) . . ?
Cl6 Pb3 Cl11 87.75(15) . . ?
Cl5 Pb3 Cl9 81.0(2) . 2_664 ?
Cl6 Pb3 Cl9 166.06(17) . 2_664 ?
Cl11 Pb3 Cl9 92.13(16) . 2_664 ?
Cl5 Pb3 Cl10 170.61(17) . 2_564 ?
Cl6 Pb3 Cl10 85.6(2) . 2_564 ?
Cl11 Pb3 Cl10 89.04(16) . 2_564 ?
Cl9 Pb3 Cl10 108.33(18) 2_664 2_564 ?
Cl5 Pb3 Cl12 92.24(15) . . ?
Cl6 Pb3 Cl12 90.47(16) . . ?
Cl11 Pb3 Cl12 177.35(14) . . ?
Cl9 Pb3 Cl12 90.07(17) 2_664 . ?
Cl10 Pb3 Cl12 88.87(16) 2_564 . ?
Pb1 Cl3 Pb2 147.6(2) . 1_655 ?
Pb1 Cl4 Pb2 170.6(2) . . ?
Pb3 Cl5 Pb1 170.1(2) . 1_655 ?
Pb3 Cl6 Pb1 147.0(2) . . ?
Pb2 Cl9 Pb3 171.0(2) . 2_665 ?
Pb2 Cl10 Pb3 147.7(2) . 2_565 ?
C2 N1 N2 113.5(17) . . ?
C1 N2 N1 102.4(18) . . ?
C2 N3 C1 108.0(18) . . ?
N2 C1 N3 112(2) . . ?
N3 C2 N1 104.4(18) . . ?
C4 N4 N5 111.3(18) . . ?
C3 N5 N4 101.3(18) . . ?
C3 N6 C4 104.7(18) . . ?
N5 C3 N6 114(2) . . ?
N4 C4 N6 109(2) . . ?
C6 N7 N8 112.9(17) . . ?
C5 N8 N7 101.3(19) . . ?
C5 N9 C6 105.5(17) . . ?
N8 C5 N9 114(2) . . ?
N7 C6 N9 106.0(17) . . ?
N11 N10 C8 112.2(18) . . ?
C7 N11 N10 104.2(19) . . ?
C8 N12 C7 107.6(18) . . ?
N11 C7 N12 110(2) . . ?
N12 C8 N10 106.1(17) . . ?
N14 N13 C10 111.9(19) . . ?
N13 N14 C9 104.8(19) . . ?
C10 N15 C9 107.9(18) . . ?
N14 C9 N15 109(2) . . ?
N15 C10 N13 106(2) . . ?
C12 N16 N17 114.3(18) . . ?
C11 N17 N16 100(2) . . ?
C11 N18 C12 106.7(18) . . ?
N17 C11 N18 115(2) . . ?
N16 C12 N18 103.9(17) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N1 H1 Cl1 0.86 2.40 3.174(18) 149.4 . yes
N3 H2 Cl1 0.86 2.28 3.133(18) 174.1 1_655 yes
N4 H5 Cl2 0.86 2.44 3.182(19) 144.9 1_455 yes
N4 H5 Cl6 0.86 2.93 3.44(2) 119.1 1_455 yes
N6 H6 Cl2 0.86 2.29 3.137(17) 170.5 . yes
N7 H9 Cl7 0.86 2.43 3.194(18) 148.8 1_655 yes
N10 H13 Cl3 0.86 3.02 3.50(2) 117.7 . yes
N10 H13 Cl8 0.86 2.43 3.188(19) 147.3 1_655 yes
N12 H14 Cl8 0.86 2.28 3.133(18) 172.7 . yes
N13 H17 Cl10 0.86 3.04 3.53(2) 117.7 2_664 yes
N13 H17 Cl11 0.86 2.43 3.194(19) 148.4 1_655 yes
N15 H18 Cl11 0.86 2.29 3.145(18) 170.1 . yes
N16 H21 Cl12 0.86 2.40 3.180(17) 150.2 1_655 yes
N18 H22 Cl12 0.86 2.28 3.140(17) 173.4 . yes

_refine_diff_density_max         1.255
_refine_diff_density_min         -3.435
_refine_diff_density_rms         0.239

####################################################################### 
# 
# 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_T4Pb3I10_2H2O_93K
_database_code_depnum_ccdc_archive 'CCDC 2024195'
loop_
_audit_author_name
_audit_author_address
'Yuan-Yuan Guo'
;University of St Andrews
United Kingdom
;
_audit_update_record             
;
2020-08-20 deposited with the CCDC.	2020-11-17 downloaded from the CCDC.
;
_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '2(I5 Pb1.50), 4(C2 H4 N3), 2(H2 O)'
_chemical_formula_sum            'C8 H20 I10 N12 O2 Pb3'
_chemical_formula_weight         2206.93

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 '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'
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 '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'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           64
_space_group_name_H-M_alt        'C m c a'
_space_group_name_Hall           '-C 2bc 2'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y+1/2, z+1/2'
'-x, y+1/2, -z+1/2'
'x, -y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1, z+1/2'
'-x+1/2, y+1, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x, y-1/2, -z-1/2'
'x, -y-1/2, z-1/2'
'-x, y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, y, -z-1/2'
'x+1/2, -y, z-1/2'
'-x+1/2, y+1/2, z'

_cell_length_a                   9.6028(12)
_cell_length_b                   20.805(2)
_cell_length_c                   19.776(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3951.0(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    93(2)
_cell_measurement_reflns_used    6321
_cell_measurement_theta_min      2.1
_cell_measurement_theta_max      27.5

_exptl_crystal_description       Prism
_exptl_crystal_colour            Yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    3.710
_exptl_crystal_F_000             3776
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_exptl_absorpt_coefficient_mu    20.593
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.571
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      93(2)
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Rotating Anode'
_diffrn_measurement_device_type  
;
Rigaku Pilatus 200K
;
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            20834
_diffrn_reflns_av_unetI/netI     0.0174
_diffrn_reflns_av_R_equivalents  0.0443
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         3.659
_diffrn_reflns_theta_max         24.997
_diffrn_reflns_theta_full        24.997
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             1847
_reflns_number_gt                1797
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Ortep for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0161P)²+1.7211P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1847
_refine_ls_number_parameters     91
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0159
_refine_ls_R_factor_gt           0.0151
_refine_ls_wR_factor_ref         0.0338
_refine_ls_wR_factor_gt          0.0336
_refine_ls_goodness_of_fit_ref   1.180
_refine_ls_restrained_S_all      1.180
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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 0.500000 0.500000 0.01300(7) Uani 1 4 d S T P . .
Pb2 Pb 0.500000 0.63382(2) 0.35456(2) 0.01416(6) Uani 1 2 d S T P . .
I1 I 0.500000 0.77822(2) 0.38651(2) 0.01496(8) Uani 1 2 d S T P . .
I2 I 0.500000 0.52624(2) 0.65713(2) 0.01671(8) Uani 1 2 d S T P . .
I3 I 0.73070(2) 0.61088(2) 0.47630(2) 0.01527(7) Uani 1 1 d . . . . .
I4 I 0.250000 0.64058(2) 0.250000 0.03375(11) Uani 1 2 d S T P . .
N1 N 0.5715(3) 0.56166(14) 0.82751(15) 0.0175(6) Uani 1 1 d . . . . .
H1 H 0.624312 0.589765 0.808591 0.021 Uiso 0.5 1 calc R U P . .
N2 N 0.500000 0.4801(2) 0.8844(3) 0.0320(12) Uani 1 2 d S T P . .
H2 H 0.500001 0.446230 0.909342 0.038 Uiso 1 2 calc R U P . .
N3 N 0.9294(3) 0.70940(14) 0.84030(16) 0.0200(7) Uani 1 1 d . . . . .
H3 H 0.876559 0.694610 0.808838 0.024 Uiso 0.5 1 calc R U P . .
N4 N 1.000000 0.7537(2) 0.9320(2) 0.0169(9) Uani 1 2 d S T P . .
H4 H 0.999998 0.773002 0.970448 0.020 Uiso 1 2 calc R U P . .
C1 C 0.6127(4) 0.51137(18) 0.86136(19) 0.0224(8) Uani 1 1 d . . . . .
H5 H 0.704714 0.499202 0.868372 0.027 Uiso 1 1 calc R U . . .
C2 C 0.8883(4) 0.73585(18) 0.8966(2) 0.0224(8) Uani 1 1 d . . . . .
H6 H 0.796183 0.741390 0.909849 0.027 Uiso 1 1 calc R U . . .
O1 O 0.750000 0.64436(17) 0.750000 0.0214(8) Uani 1 2 d S T P . .
H7 H 0.693600 0.622487 0.772600 0.59(17) Uiso 1 1 d R . . . .


_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 I2 3.1550(6) . ?
Pb1 I2 3.1551(6) 9_666 ?
Pb1 I3 3.2326(3) . ?
Pb1 I3 3.2326(3) 9_666 ?
Pb1 I3 3.2326(3) 12_655 ?
Pb1 I3 3.2326(3) 4_566 ?
Pb2 I1 3.0699(5) . ?
Pb2 I4 3.1716(3) . ?
Pb2 I4 3.1716(3) 14_556 ?
Pb2 I3 3.3062(4) . ?
Pb2 I3 3.3063(4) 12_655 ?
Pb2 I2 3.3381(5) 9_666 ?
N1 C1 1.303(5) . ?
N1 N1 1.372(6) 12_655 ?
N2 C1 1.342(5) 12_655 ?
N2 C1 1.342(5) . ?
N3 C2 1.303(5) . ?
N3 N3 1.355(6) 12_755 ?
N4 C2 1.334(4) 12_755 ?
N4 C2 1.334(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
I2 Pb1 I2 180.0 . 9_666 ?
I2 Pb1 I3 91.107(6) . . ?
I2 Pb1 I3 88.892(6) 9_666 . ?
I2 Pb1 I3 88.894(7) . 9_666 ?
I2 Pb1 I3 91.107(7) 9_666 9_666 ?
I3 Pb1 I3 180.0 . 9_666 ?
I2 Pb1 I3 91.106(7) . 12_655 ?
I2 Pb1 I3 88.893(7) 9_666 12_655 ?
I3 Pb1 I3 86.522(11) . 12_655 ?
I3 Pb1 I3 93.478(11) 9_666 12_655 ?
I2 Pb1 I3 88.894(7) . 4_566 ?
I2 Pb1 I3 91.107(7) 9_666 4_566 ?
I3 Pb1 I3 93.478(11) . 4_566 ?
I3 Pb1 I3 86.522(12) 9_666 4_566 ?
I3 Pb1 I3 180.0 12_655 4_566 ?
I1 Pb2 I4 95.210(9) . . ?
I1 Pb2 I4 95.209(9) . 14_556 ?
I4 Pb2 I4 98.389(12) . 14_556 ?
I1 Pb2 I3 89.508(7) . . ?
I4 Pb2 I3 171.235(8) . . ?
I4 Pb2 I3 88.508(12) 14_556 . ?
I1 Pb2 I3 89.507(7) . 12_655 ?
I4 Pb2 I3 88.508(12) . 12_655 ?
I4 Pb2 I3 171.235(8) 14_556 12_655 ?
I3 Pb2 I3 84.141(14) . 12_655 ?
I1 Pb2 I2 172.099(10) . 9_666 ?
I4 Pb2 I2 89.944(9) . 9_666 ?
I4 Pb2 I2 89.944(9) 14_556 9_666 ?
I3 Pb2 I2 84.633(7) . 9_666 ?
I3 Pb2 I2 84.634(7) 12_655 9_666 ?
Pb1 I2 Pb2 76.063(7) . 9_666 ?
Pb1 I3 Pb2 75.487(8) . . ?
Pb2 I4 Pb2 174.919(15) 14_456 . ?
C1 N1 N1 107.7(2) . 12_655 ?
C1 N2 C1 107.4(5) 12_655 . ?
C2 N3 N3 107.6(2) . 12_755 ?
C2 N4 C2 107.0(4) 12_755 . ?
N1 C1 N2 108.6(3) . . ?
N3 C2 N4 108.8(3) . . ?

_refine_diff_density_max         0.799
_refine_diff_density_min         -1.554
_refine_diff_density_rms         0.196

