# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry C.
# This journal is © The Royal Society of Chemistry 2022

####################################################################### 
# 
# 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_3
_database_code_depnum_ccdc_archive 'CCDC 2072355'
loop_
_audit_author_name
_audit_author_address
'Mengmeng Lun'
;South China Normal University
China
;
_audit_update_record             
;
2021-03-23 deposited with the CCDC.	2022-07-12 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C24.06 H0 Br12 Cl4.02 N4.02 O4.02 Pb4'
_chemical_formula_weight         2339.71

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'
N N 0.0061 0.0033 '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'
Cl Cl 0.1484 0.1585 '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'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_H-M   'P -3 c 1'

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

_cell_length_a                   17.4023(3)
_cell_length_b                   17.4023(3)
_cell_length_c                   7.9318(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     2080.25(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    383(2)
_cell_measurement_reflns_used    1787
_cell_measurement_theta_min      2.315
_cell_measurement_theta_max      21.9620

_exptl_crystal_description       needle
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    3.735
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2040
_exptl_absorpt_coefficient_mu    27.958
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.204
_exptl_absorpt_correction_T_max  0.247
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      383(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            7372
_diffrn_reflns_av_R_equivalents  0.0638
_diffrn_reflns_av_sigmaI/netI    0.0476
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         2.34
_diffrn_reflns_theta_max         24.97
_reflns_number_total             1224
_reflns_number_gt                610
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0020P)²+22.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   .
_refine_ls_hydrogen_treatment    .
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.00111(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         1224
_refine_ls_number_parameters     83
_refine_ls_number_restraints     17
_refine_ls_R_factor_all          0.2357
_refine_ls_R_factor_gt           0.1587
_refine_ls_wR_factor_ref         0.3100
_refine_ls_wR_factor_gt          0.2931
_refine_ls_goodness_of_fit_ref   1.176
_refine_ls_restrained_S_all      1.187
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.001

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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.3333 0.6667 0.43936(14) 0.0952(4) Uani 1 3 d S . .
Br1 Br 0.20228(17) 0.53556(17) 0.6768(3) 0.1642(14) Uani 1 1 d . . .
Br2 Br 0.1303(4) 0.1341(4) 0.3284(5) 0.332(4) Uani 1 1 d . . .
Pb2 Pb 0.0000 0.0000 0.4341(3) 0.2423(13) Uani 1 3 d S . .
O1 O 0.2565(16) 0.3464(15) 0.497(5) 0.308(15) Uani 0.67 1 d PD . .
C4 C 0.185(4) 0.300(4) 0.559(8) 0.34(3) Uiso 0.67 1 d PD . .
C5 C 0.3274(14) 0.3274(14) 0.7500 0.103(11) Uani 1 2 d SD . .
C3 C 0.170(9) 0.248(9) 0.595(9) 0.86(18) Uani 0.67 1 d PD . .
N1 N 0.222(4) 0.293(4) 0.701(9) 0.44(4) Uiso 0.67 1 d PD . .
C6 C 0.173(2) 0.200(4) 0.730(13) 0.56(4) Uani 0.67 1 d PD . .
Cl1 Cl 0.360(2) 0.3548(18) 0.919(6) 0.92(4) Uani 0.67 1 d PD . .
C2 C 0.275(3) 0.273(3) 0.479(7) 0.33(3) Uiso 0.83 1 d PD . .
C1 C 0.317(3) 0.233(3) 0.657(7) 0.27(3) Uiso 0.67 1 d PD . .


_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 Br1 2.958(2) 3_565 ?
Pb1 Br1 2.958(2) . ?
Pb1 Br1 2.958(2) 2_665 ?
Pb1 Br1 3.089(2) 12_565 ?
Pb1 Br1 3.089(2) 10_665 ?
Pb1 Br1 3.089(2) 11 ?
Br1 Pb1 3.089(2) 10_666 ?
Br2 Br2 1.249(8) 4 ?
Br2 Pb2 2.449(4) . ?
Br2 Pb2 2.974(4) 7_556 ?
Br2 Pb2 3.103(4) 4 ?
Pb2 Pb2 1.045(5) 7_556 ?
Pb2 Br2 2.449(4) 3 ?
Pb2 Br2 2.449(4) 2 ?
Pb2 Br2 2.974(4) 9_556 ?
Pb2 Br2 2.974(4) 8_556 ?
Pb2 Br2 2.974(4) 7_556 ?
Pb2 Pb2 2.921(5) 4 ?
Pb2 Br2 3.103(4) 5 ?
Pb2 Br2 3.103(4) 6 ?
Pb2 Br2 3.103(4) 4 ?
O1 C2 1.46(7) . ?
O1 C4 1.19(6) . ?
O1 C3 1.80(11) . ?
C4 C3 0.86(16) . ?
C4 C2 1.93(10) . ?
C4 N1 1.33(10) . ?
C5 N1 1.66(6) . ?
C5 N1 1.66(6) 4_556 ?
C5 C1 1.73(6) . ?
C5 C1 1.73(6) 4_556 ?
C5 C6 2.49(4) 4_556 ?
C5 C6 2.49(4) . ?
C5 Cl1 1.44(5) . ?
C5 Cl1 1.44(5) 4_556 ?
C3 C6 1.37(15) . ?
C3 N1 1.20(11) . ?
C3 C6 2.14(16) 4_556 ?
C3 C2 1.88(15) . ?
N1 C1 2.39(9) . ?
N1 C6 2.01(8) 4_556 ?
N1 C6 1.42(8) . ?
N1 N1 2.28(15) 4_556 ?
N1 C2 2.09(9) . ?
N1 C1 1.19(9) 4_556 ?
C6 N1 2.01(8) 4_556 ?
C6 C1 1.98(9) 4_556 ?
C6 C6 0.88(13) 4_556 ?
C6 C3 2.14(16) 4_556 ?
Cl1 Cl1 2.68(9) 4_556 ?
C2 C1 1.88(8) . ?
C1 C6 1.98(9) 4_556 ?
C1 N1 1.19(9) 4_556 ?

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
Br1 Pb1 Br1 83.80(7) 3_565 . ?
Br1 Pb1 Br1 83.80(7) 3_565 2_665 ?
Br1 Pb1 Br1 83.80(7) . 2_665 ?
Br1 Pb1 Br1 98.29(10) 3_565 12_565 ?
Br1 Pb1 Br1 98.33(10) . 12_565 ?
Br1 Pb1 Br1 177.14(8) 2_665 12_565 ?
Br1 Pb1 Br1 98.33(10) 3_565 10_665 ?
Br1 Pb1 Br1 177.14(8) . 10_665 ?
Br1 Pb1 Br1 98.29(10) 2_665 10_665 ?
Br1 Pb1 Br1 79.51(7) 12_565 10_665 ?
Br1 Pb1 Br1 177.14(8) 3_565 11 ?
Br1 Pb1 Br1 98.29(10) . 11 ?
Br1 Pb1 Br1 98.33(10) 2_665 11 ?
Br1 Pb1 Br1 79.51(7) 12_565 11 ?
Br1 Pb1 Br1 79.51(7) 10_665 11 ?
Pb1 Br1 Pb1 81.94(5) . 10_666 ?
Br2 Br2 Pb2 109.80(12) 4 . ?
Br2 Br2 Pb2 128.97(13) 4 7_556 ?
Pb2 Br2 Pb2 19.28(9) . 7_556 ?
Br2 Br2 Pb2 47.95(9) 4 4 ?
Pb2 Br2 Pb2 62.17(12) . 4 ?
Pb2 Br2 Pb2 81.45(11) 7_556 4 ?
Pb2 Pb2 Br2 110.03(11) 7_556 3 ?
Pb2 Pb2 Br2 110.03(11) 7_556 . ?
Br2 Pb2 Br2 108.91(11) 3 . ?
Pb2 Pb2 Br2 110.03(11) 7_556 2 ?
Br2 Pb2 Br2 108.91(11) 3 2 ?
Br2 Pb2 Br2 108.91(11) . 2 ?
Pb2 Pb2 Br2 50.69(9) 7_556 9_556 ?
Br2 Pb2 Br2 160.72(9) 3 9_556 ?
Br2 Pb2 Br2 81.57(11) . 9_556 ?
Br2 Pb2 Br2 81.57(11) 2 9_556 ?
Pb2 Pb2 Br2 50.69(9) 7_556 8_556 ?
Br2 Pb2 Br2 81.57(11) 3 8_556 ?
Br2 Pb2 Br2 81.57(11) . 8_556 ?
Br2 Pb2 Br2 160.72(9) 2 8_556 ?
Br2 Pb2 Br2 84.15(13) 9_556 8_556 ?
Pb2 Pb2 Br2 50.69(9) 7_556 7_556 ?
Br2 Pb2 Br2 81.57(12) 3 7_556 ?
Br2 Pb2 Br2 160.72(9) . 7_556 ?
Br2 Pb2 Br2 81.57(12) 2 7_556 ?
Br2 Pb2 Br2 84.15(13) 9_556 7_556 ?
Br2 Pb2 Br2 84.15(13) 8_556 7_556 ?
Pb2 Pb2 Pb2 180.000(1) 7_556 4 ?
Br2 Pb2 Pb2 69.97(11) 3 4 ?
Br2 Pb2 Pb2 69.97(11) . 4 ?
Br2 Pb2 Pb2 69.97(11) 2 4 ?
Br2 Pb2 Pb2 129.31(9) 9_556 4 ?
Br2 Pb2 Pb2 129.31(9) 8_556 4 ?
Br2 Pb2 Pb2 129.31(9) 7_556 4 ?
Pb2 Pb2 Br2 132.14(8) 7_556 5 ?
Br2 Pb2 Br2 22.25(15) 3 5 ?
Br2 Pb2 Br2 98.5(3) . 5 ?
Br2 Pb2 Br2 95.0(3) 2 5 ?
Br2 Pb2 Br2 176.4(2) 9_556 5 ?
Br2 Pb2 Br2 99.4(2) 8_556 5 ?
Br2 Pb2 Br2 96.5(2) 7_556 5 ?
Pb2 Pb2 Br2 47.86(8) 4 5 ?
Pb2 Pb2 Br2 132.14(8) 7_556 6 ?
Br2 Pb2 Br2 98.5(3) 3 6 ?
Br2 Pb2 Br2 95.0(3) . 6 ?
Br2 Pb2 Br2 22.25(15) 2 6 ?
Br2 Pb2 Br2 96.5(2) 9_556 6 ?
Br2 Pb2 Br2 176.4(2) 8_556 6 ?
Br2 Pb2 Br2 99.4(2) 7_556 6 ?
Pb2 Pb2 Br2 47.86(8) 4 6 ?
Br2 Pb2 Br2 79.91(12) 5 6 ?
Pb2 Pb2 Br2 132.14(8) 7_556 4 ?
Br2 Pb2 Br2 95.0(3) 3 4 ?
Br2 Pb2 Br2 22.25(15) . 4 ?
Br2 Pb2 Br2 98.5(3) 2 4 ?
Br2 Pb2 Br2 99.4(2) 9_556 4 ?
Br2 Pb2 Br2 96.5(2) 8_556 4 ?
Br2 Pb2 Br2 176.4(2) 7_556 4 ?
Pb2 Pb2 Br2 47.86(8) 4 4 ?
Br2 Pb2 Br2 79.91(12) 5 4 ?
Br2 Pb2 Br2 79.91(13) 6 4 ?
C2 O1 C4 93(4) . . ?
C2 O1 C3 70(6) . . ?
C4 O1 C3 24(7) . . ?
C3 C4 O1 122(10) . . ?
C3 C4 C2 74(10) . . ?
O1 C4 C2 49(4) . . ?
C3 C4 N1 62(8) . . ?
O1 C4 N1 92(5) . . ?
C2 C4 N1 77(5) . . ?
N1 C5 N1 87(4) . 4_556 ?
N1 C5 C1 89(3) . . ?
N1 C5 C1 41(3) 4_556 . ?
N1 C5 C1 41(3) . 4_556 ?
N1 C5 C1 89(3) 4_556 4_556 ?
C1 C5 C1 117(4) . 4_556 ?
N1 C5 C6 53(3) . 4_556 ?
N1 C5 C6 33(3) 4_556 4_556 ?
C1 C5 C6 52(3) . 4_556 ?
C1 C5 C6 65(3) 4_556 4_556 ?
N1 C5 C6 33(3) . . ?
N1 C5 C6 53(3) 4_556 . ?
C1 C5 C6 65(3) . . ?
C1 C5 C6 52(3) 4_556 . ?
C6 C5 C6 20(3) 4_556 . ?
N1 C5 Cl1 121(3) . . ?
N1 C5 Cl1 91(3) 4_556 . ?
C1 C5 Cl1 123(3) . . ?
C1 C5 Cl1 80(2) 4_556 . ?
C6 C5 Cl1 107(3) 4_556 . ?
C6 C5 Cl1 115(3) . . ?
N1 C5 Cl1 91(3) . 4_556 ?
N1 C5 Cl1 121(3) 4_556 4_556 ?
C1 C5 Cl1 80(2) . 4_556 ?
C1 C5 Cl1 123(3) 4_556 4_556 ?
C6 C5 Cl1 115(3) 4_556 4_556 ?
C6 C5 Cl1 107(3) . 4_556 ?
Cl1 C5 Cl1 137(3) . 4_556 ?
C4 C3 C6 145(10) . . ?
C4 C3 N1 79(10) . . ?
C6 C3 N1 67(7) . . ?
C4 C3 O1 34(8) . . ?
C6 C3 O1 131(9) . . ?
N1 C3 O1 71(6) . . ?
C4 C3 C6 145(10) . 4_556 ?
C6 C3 C6 14(6) . 4_556 ?
N1 C3 C6 67(7) . 4_556 ?
O1 C3 C6 121(8) . 4_556 ?
C4 C3 C2 80(10) . . ?
C6 C3 C2 102(10) . . ?
N1 C3 C2 82(8) . . ?
O1 C3 C2 47(3) . . ?
C6 C3 C2 88(8) 4_556 . ?
C5 N1 C1 46(2) . . ?
C5 N1 C6 85(4) . 4_556 ?
C1 N1 C6 53(3) . 4_556 ?
C5 N1 C6 107(5) . . ?
C1 N1 C6 71(4) . . ?
C6 N1 C6 22(4) 4_556 . ?
C5 N1 N1 47(2) . 4_556 ?
C1 N1 N1 29(3) . 4_556 ?
C6 N1 N1 38(2) 4_556 4_556 ?
C6 N1 N1 61(4) . 4_556 ?
C5 N1 C3 137(10) . . ?
C1 N1 C3 94(10) . . ?
C6 N1 C3 79(9) 4_556 . ?
C6 N1 C3 62(8) . . ?
N1 N1 C3 108(10) 4_556 . ?
C5 N1 C2 76(3) . . ?
C1 N1 C2 49(3) . . ?
C6 N1 C2 86(4) 4_556 . ?
C6 N1 C2 91(5) . . ?
N1 N1 C2 78(4) 4_556 . ?
C3 N1 C2 63(7) . . ?
C5 N1 C1 72(4) . 4_556 ?
C1 N1 C1 106(6) . 4_556 ?
C6 N1 C1 91(6) 4_556 4_556 ?
C6 N1 C1 98(7) . 4_556 ?
N1 N1 C1 80(6) 4_556 4_556 ?
C3 N1 C1 146(8) . 4_556 ?
C2 N1 C1 149(6) . 4_556 ?
C5 N1 C4 131(5) . . ?
C1 N1 C4 113(6) . . ?
C6 N1 C4 118(5) 4_556 . ?
C6 N1 C4 101(6) . . ?
N1 N1 C4 139(7) 4_556 . ?
C3 N1 C4 39(8) . . ?
C2 N1 C4 65(5) . . ?
C1 N1 C4 141(8) 4_556 . ?
N1 C6 C1 73(3) 4_556 4_556 ?
N1 C6 N1 81(5) 4_556 . ?
C1 C6 N1 36(4) 4_556 . ?
N1 C6 C3 117(7) 4_556 . ?
C1 C6 C3 84(6) 4_556 . ?
N1 C6 C3 51(6) . . ?
N1 C6 C6 38(2) 4_556 4_556 ?
C1 C6 C6 104(10) 4_556 4_556 ?
N1 C6 C6 119(4) . 4_556 ?
C3 C6 C6 144(10) . 4_556 ?
N1 C6 C5 41.7(18) 4_556 . ?
C1 C6 C5 43.7(19) 4_556 . ?
N1 C6 C5 40(3) . . ?
C3 C6 C5 82(5) . . ?
C6 C6 C5 79.8(15) 4_556 . ?
N1 C6 C3 33(4) 4_556 4_556 ?
C1 C6 C3 83(5) 4_556 4_556 ?
N1 C6 C3 107(5) . 4_556 ?
C3 C6 C3 150(8) . 4_556 ?
C6 C6 C3 22(10) 4_556 4_556 ?
C5 C6 C3 70(3) . 4_556 ?
C5 Cl1 Cl1 21.3(15) . 4_556 ?
O1 C2 C1 123(4) . . ?
O1 C2 N1 58(3) . . ?
C1 C2 N1 74(3) . . ?
O1 C2 C4 38(2) . . ?
C1 C2 C4 111(4) . . ?
N1 C2 C4 38(3) . . ?
O1 C2 C3 64(5) . . ?
C1 C2 C3 93(5) . . ?
N1 C2 C3 35(3) . . ?
C4 C2 C3 26(5) . . ?
N1 C1 C6 54(3) . 4_556 ?
N1 C1 C5 44(2) . . ?
C6 C1 C5 84(3) 4_556 . ?
N1 C1 C2 57(3) . . ?
C6 C1 C2 93(4) 4_556 . ?
C5 C1 C2 81(3) . . ?
N1 C1 N1 70(6) . 4_556 ?
C6 C1 N1 45(4) 4_556 4_556 ?
C5 C1 N1 67(4) . 4_556 ?
C2 C1 N1 127(6) . 4_556 ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        24.97
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         4.311
_refine_diff_density_min         -6.448
_refine_diff_density_rms         0.478
# start Validation Reply Form
_vrf_PLAT213_3                   
;
PROBLEM: Atom C6              has ADP max/min Ratio .....        8.9 oblate
RESPONSE: This is due to the structural disorder of the cation.
;
_vrf_PLAT242_3                   
;
PROBLEM: Low    'MainMol' Ueq as Compared to Neighbors of         C5 Check 
RESPONSE: This is due to the structural disorder of the cation.
;
_vrf_PLAT082_3                   
;
PROBLEM: High R1 Value ..................................       0.16 Report
RESPONSE: The single crystal X-ray diffraction data of crystal become poor at 383k.
;
_vrf_PLAT220_3                   
;
PROBLEM: NonSolvent   Resd 1  C   Ueq(max)/Ueq(min) Range        8.3 Ratio 
RESPONSE:  The question is caused by slight distortion of structure and quasi-static motion of atoms.
;
_vrf_PLAT260_3                   
;
PROBLEM: Large Average Ueq of Residue Including       Cl1      0.549 Check 
RESPONSE: This is assigned to the thermal vibrations of atom.
;
# end Validation Reply Form
####################################################################### 
# 
# 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_1
_database_code_depnum_ccdc_archive 'CCDC 2094248'
loop_
_audit_author_name
_audit_author_address
'Mengmeng Lun'
;Southeast University
China
;
_audit_update_record             
;
2021-07-04 deposited with the CCDC.	2022-07-12 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C9 Br3 N2 O2 Pb'
_chemical_formula_sum            'C9 Br3 N2 O2 Pb'
_chemical_formula_weight         615.03

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Br Br -0.2901 2.4595 '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'
N N 0.0061 0.0033 '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'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      hexagonal
_space_group_IT_number           194
_space_group_name_H-M_alt        'P 63/m m c'
_space_group_name_Hall           '-P 6c 2c'

_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'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, z+1/2'
'y, -x+y, z+1/2'
'x-y, x, z+1/2'
'y, x, -z'
'x-y, -y, -z'
'-x, -x+y, -z'
'-y, -x, -z+1/2'
'-x+y, y, -z+1/2'
'x, x-y, -z+1/2'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'x, y, -z-1/2'
'-y, x-y, -z-1/2'
'-x+y, -x, -z-1/2'
'-y, -x, z'
'-x+y, y, z'
'x, x-y, z'
'y, x, z-1/2'
'x-y, -y, z-1/2'
'-x, -x+y, z-1/2'

_cell_length_a                   9.8400(7)
_cell_length_b                   9.8400(7)
_cell_length_c                   7.8271(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     656.33(10)
_cell_formula_units_Z            2
_cell_measurement_temperature    328(2)
_cell_measurement_reflns_used    888
_cell_measurement_theta_min      2.3640
_cell_measurement_theta_max      22.9700

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    3.112
_exptl_crystal_F_000             542
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_exptl_absorpt_coefficient_mu    21.973
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.30699
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      328(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            2628
_diffrn_reflns_av_unetI/netI     0.0231
_diffrn_reflns_av_R_equivalents  0.0295
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_theta_min         2.390
_diffrn_reflns_theta_max         30.219
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.899
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.899
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.899
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             364
_reflns_number_gt                213
_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-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.0926P)²+1.8300P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   .
_refine_ls_hydrogen_treatment    undef
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         364
_refine_ls_number_parameters     23
_refine_ls_number_restraints     42
_refine_ls_R_factor_all          0.1044
_refine_ls_R_factor_gt           0.0583
_refine_ls_wR_factor_ref         0.1896
_refine_ls_wR_factor_gt          0.1676
_refine_ls_goodness_of_fit_ref   1.122
_refine_ls_restrained_S_all      1.082
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.001

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 1.0000 0.0000 0.5000 0.0973(2) Uani 1 12 d S TU P . .
Br1 Br 0.86346(8) 0.13654(8) 0.7500 0.1506(5) Uani 1 4 d S TU P . .
N1 N 0.6667 0.3333 0.143(2) 0.2914(3) Uani 1 6 d S TU P . .
C2 C 0.5788(14) 0.158(3) 0.4721(16) 0.2908(3) Uani 1 2 d S TU P . .
C1 C 0.5784(17) 0.157(3) 0.2500 0.2918(3) Uani 1 4 d S TU P . .
O1 O 0.6667 0.3333 0.509(2) 0.292(3) Uani 1 6 d S TU 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 Br1 3.0405(10) 15_546 ?
Pb1 Br1 3.0405(10) 3_765 ?
Pb1 Br1 3.0405(10) 13_756 ?
Pb1 Br1 3.0405(10) 2_645 ?
Pb1 Br1 3.0405(10) 14_666 ?
Pb1 Br1 3.0405(10) . ?
Br1 Pb1 3.0405(10) 4_755 ?
N1 O1 1.20(2) 16_556 ?
N1 N1 1.67(4) 16_556 ?
N1 C1 1.72(3) 3_665 ?
N1 C1 1.72(3) . ?
N1 C1 1.72(3) 2_655 ?
N1 C2 1.75(2) 16_556 ?
N1 C2 1.75(2) 17_656 ?
N1 C2 1.75(2) 18_666 ?
C2 O1 1.53(2) . ?
C2 C1 1.738(12) . ?
C2 N1 1.75(2) 16_556 ?
C1 N1 1.72(3) 16_556 ?
C1 C2 1.738(12) 16_556 ?
O1 N1 1.20(2) 16_556 ?
O1 C2 1.53(2) 2_655 ?
O1 C2 1.53(2) 3_665 ?

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
Br1 Pb1 Br1 180.0 15_546 3_765 ?
Br1 Pb1 Br1 83.03(2) 15_546 13_756 ?
Br1 Pb1 Br1 96.97(2) 3_765 13_756 ?
Br1 Pb1 Br1 96.97(2) 15_546 2_645 ?
Br1 Pb1 Br1 83.03(2) 3_765 2_645 ?
Br1 Pb1 Br1 96.97(2) 13_756 2_645 ?
Br1 Pb1 Br1 83.03(2) 15_546 14_666 ?
Br1 Pb1 Br1 96.97(2) 3_765 14_666 ?
Br1 Pb1 Br1 83.03(2) 13_756 14_666 ?
Br1 Pb1 Br1 180.00(4) 2_645 14_666 ?
Br1 Pb1 Br1 96.97(2) 15_546 . ?
Br1 Pb1 Br1 83.03(2) 3_765 . ?
Br1 Pb1 Br1 180.00(2) 13_756 . ?
Br1 Pb1 Br1 83.03(2) 2_645 . ?
Br1 Pb1 Br1 96.97(2) 14_666 . ?
Pb1 Br1 Pb1 80.12(3) 4_755 . ?
O1 N1 N1 180.0 16_556 16_556 ?
O1 N1 C1 119.0(7) 16_556 3_665 ?
N1 N1 C1 61.0(7) 16_556 3_665 ?
O1 N1 C1 119.0(7) 16_556 . ?
N1 N1 C1 61.0(7) 16_556 . ?
C1 N1 C1 98.4(9) 3_665 . ?
O1 N1 C1 119.0(7) 16_556 2_655 ?
N1 N1 C1 61.0(7) 16_556 2_655 ?
C1 N1 C1 98.4(9) 3_665 2_655 ?
C1 N1 C1 98.4(9) . 2_655 ?
O1 N1 C2 58.9(8) 16_556 16_556 ?
N1 N1 C2 121.1(8) 16_556 16_556 ?
C1 N1 C2 128.7(2) 3_665 16_556 ?
C1 N1 C2 60.1(7) . 16_556 ?
C1 N1 C2 128.7(2) 2_655 16_556 ?
O1 N1 C2 58.9(8) 16_556 17_656 ?
N1 N1 C2 121.1(8) 16_556 17_656 ?
C1 N1 C2 128.7(2) 3_665 17_656 ?
C1 N1 C2 128.7(2) . 17_656 ?
C1 N1 C2 60.1(7) 2_655 17_656 ?
C2 N1 C2 95.7(10) 16_556 17_656 ?
O1 N1 C2 58.9(8) 16_556 18_666 ?
N1 N1 C2 121.1(8) 16_556 18_666 ?
C1 N1 C2 60.1(7) 3_665 18_666 ?
C1 N1 C2 128.7(2) . 18_666 ?
C1 N1 C2 128.7(2) 2_655 18_666 ?
C2 N1 C2 95.7(10) 16_556 18_666 ?
C2 N1 C2 95.7(10) 17_656 18_666 ?
O1 C2 C1 101.3(16) . . ?
O1 C2 N1 42.2(10) . 16_556 ?
C1 C2 N1 59.1(12) . 16_556 ?
N1 C1 N1 58.1(15) . 16_556 ?
N1 C1 C2 60.8(11) . 16_556 ?
N1 C1 C2 118.8(18) 16_556 16_556 ?
N1 C1 C2 118.8(18) . . ?
N1 C1 C2 60.8(11) 16_556 . ?
C2 C1 C2 180(2) 16_556 . ?
N1 O1 C2 78.9(8) 16_556 . ?
N1 O1 C2 78.9(8) 16_556 2_655 ?
C2 O1 C2 116.4(5) . 2_655 ?
N1 O1 C2 78.9(8) 16_556 3_665 ?
C2 O1 C2 116.4(5) . 3_665 ?
C2 O1 C2 116.4(5) 2_655 3_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
O1 N1 C1 N1 180.004(2) 16_556 . . 16_556 ?
C1 N1 C1 N1 -49.9(7) 3_665 . . 16_556 ?
C1 N1 C1 N1 49.9(7) 2_655 . . 16_556 ?
C2 N1 C1 N1 180.002(3) 16_556 . . 16_556 ?
C2 N1 C1 N1 108.2(14) 17_656 . . 16_556 ?
C2 N1 C1 N1 -108.2(14) 18_666 . . 16_556 ?
O1 N1 C1 C2 0.002(2) 16_556 . . 16_556 ?
N1 N1 C1 C2 179.998(2) 16_556 . . 16_556 ?
C1 N1 C1 C2 130.1(7) 3_665 . . 16_556 ?
C1 N1 C1 C2 -130.1(7) 2_655 . . 16_556 ?
C2 N1 C1 C2 -71.8(14) 17_656 . . 16_556 ?
C2 N1 C1 C2 71.8(14) 18_666 . . 16_556 ?
O1 N1 C1 C2 180.003(4) 16_556 . . . ?
N1 N1 C1 C2 -0.001(3) 16_556 . . . ?
C1 N1 C1 C2 -49.9(7) 3_665 . . . ?
C1 N1 C1 C2 49.9(7) 2_655 . . . ?
C2 N1 C1 C2 180.000(3) 16_556 . . . ?
C2 N1 C1 C2 108.2(14) 17_656 . . . ?
C2 N1 C1 C2 -108.2(14) 18_666 . . . ?
O1 C2 C1 N1 0.000(3) . . . . ?
N1 C2 C1 N1 0.001(3) 16_556 . . . ?
O1 C2 C1 N1 -0.002(3) . . . 16_556 ?
C1 C2 O1 N1 0.002(3) . . . 16_556 ?
C1 C2 O1 C2 -71.6(12) . . . 2_655 ?
N1 C2 O1 C2 -71.6(12) 16_556 . . 2_655 ?
C1 C2 O1 C2 71.6(12) . . . 3_665 ?
N1 C2 O1 C2 71.6(12) 16_556 . . 3_665 ?

_refine_diff_density_max         0.826
_refine_diff_density_min         -1.470
_refine_diff_density_rms         0.179


# start Validation Reply Form
_vrf_PLAT374_1                   
;
PROBLEM: Long   N - N         Bond  N1       - N1_*     .       1.68 Ang.  
RESPONSE: This is because the structural disorder of the cation.
;
# end Validation Reply Form

####################################################################### 
# 
# 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_3_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 2094204'
loop_
_audit_author_name
_audit_author_address
'Mnegmeng Lun'
;Southeast University
China
;
_audit_update_record             
;
2021-07-03 deposited with the CCDC.	2022-07-12 downloaded from the CCDC.
;
_audit_creation_date             2021-06-09
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Br6 Pb2, 2(C6 H14 N O)'
_chemical_formula_sum            'C12 H28 Br6 N2 O2 Pb2'
_chemical_formula_weight         1126.20
_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'
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'
O O 0.0106 0.0060 '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                   18.8860(8)
_cell_length_b                   7.9709(2)
_cell_length_c                   19.3167(9)
_cell_angle_alpha                90
_cell_angle_beta                 118.766(6)
_cell_angle_gamma                90
_cell_volume                     2549.0(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9483
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.6820
_cell_measurement_theta_min      2.1120
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    22.606
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.20068
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
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    2.935
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2016
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0587
_diffrn_reflns_av_unetI/netI     0.0523
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            22066
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.997
_diffrn_reflns_theta_max         24.997
_diffrn_reflns_theta_min         2.110
_diffrn_ambient_temperature      293
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_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                3468
_reflns_number_total             4494
_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       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_refine_diff_density_max         4.379
_refine_diff_density_min         -4.472
_refine_diff_density_rms         0.333
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     147
_refine_ls_number_reflns         4494
_refine_ls_number_restraints     170
_refine_ls_R_factor_all          0.1036
_refine_ls_R_factor_gt           0.0840
_refine_ls_restrained_S_all      1.074
_refine_ls_shift/su_max          0.045
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0662P)²+163.3354P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1991
_refine_ls_wR_factor_ref         0.2096
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N1-C2 = N1-C3
 1.5 with sigma of 0.001
 C3-C1
 2.6 with sigma of 0.002
 N1-C1
 1.5 with sigma of 0.001
3. Restrained planarity
 C3, C4, C5, C6
 with sigma of 0.1
4. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
Uanis(C4) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(Br1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O1) = Uanis(O2)
Uanis(C2) = Uanis(C7)
Uanis(C3) = Uanis(N1) = Uanis(C6) = Uanis(N2) = Uanis(O2) = Uanis(C10) =
Uanis(C11) = Uanis(C9) = Uanis(C12) = Uanis(C8) = Uanis(C7)
6.a Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B), C9(H9A,H9B), C10(H10A,
 H10B), C11(H11A,H11B), C12(H12A,H12B)
6.b Me refined with riding coordinates:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C)
6.c Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_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
Br1 Br 0.10355(5) 0.27261(12) 0.16860(10) 0.1315(6) Uani 1 1 d . U . . .
Br2 Br 0.32400(5) 0.22075(10) 0.17545(5) 0.0633(3) Uani 1 1 d . U . . .
Br3 Br 0.32382(4) 0.31749(10) 0.37002(5) 0.0616(2) Uani 1 1 d . U . . .
Br4 Br 0.17522(4) 0.71977(15) 0.30613(5) 0.0856(3) Uani 1 1 d . U . . .
Br5 Br 0.37823(3) 0.76883(8) 0.28519(4) 0.04046(19) Uani 1 1 d . U . . .
Br6 Br 0.16322(4) 0.81611(14) 0.09698(4) 0.0746(3) Uani 1 1 d . U . . .
Pb1 Pb 0.24247(2) 0.51534(3) 0.22656(2) 0.05621(10) Uani 1 1 d . U . . .
Pb2 Pb 0.24376(2) 1.01495(3) 0.23856(2) 0.05160(10) Uani 1 1 d . U . . .
C1 C 0.96208(4) 0.94123(4) 0.11768(11) 0.079(2) Uani 1 1 d D U . . .
H1A H 0.932834 1.018338 0.132718 0.119 Uiso 1 1 calc R U . . .
H1B H 1.015740 0.927057 0.160823 0.119 Uiso 1 1 calc R U . . .
H1C H 0.964867 0.984640 0.072694 0.119 Uiso 1 1 calc R U . . .
C2 C 0.94272(8) 0.73034(18) 0.18072(2) 0.0710(7) Uani 1 1 d D U . . .
H2A H 0.923646 0.815603 0.202801 0.106 Uiso 1 1 calc R U . . .
H2B H 0.918901 0.624579 0.181689 0.106 Uiso 1 1 calc R U . . .
H2C H 1.000447 0.722226 0.211204 0.106 Uiso 1 1 calc R U . . .
C3 C 0.95315(3) 0.63199(5) 0.07144(3) 0.0710(7) Uani 1 1 d D U . A 1
H3A H 1.007484 0.605433 0.112267 0.085 Uiso 1 1 calc R U . A 1
H3B H 0.954946 0.661010 0.023542 0.085 Uiso 1 1 calc R U . A 1
C4 C 0.8974(5) 0.4829(13) 0.0568(4) 0.0878(19) Uani 1 1 d . U . . .
H4A H 0.916086 0.387995 0.038566 0.105 Uiso 1 1 calc R U . A 1
H4B H 0.898254 0.451243 0.105676 0.105 Uiso 1 1 calc R U . A 1
C5 C 0.7873(4) 0.6396(12) 0.0359(3) 0.074(2) Uani 1 1 d . U . . .
H5A H 0.797340 0.591581 0.085957 0.089 Uiso 1 1 calc R U . . .
H5B H 0.729543 0.657068 0.004098 0.089 Uiso 1 1 calc R U . . .
C6 C 0.8300(4) 0.8050(12) 0.0503(4) 0.0710(7) Uani 1 1 d . U . . .
H6A H 0.812849 0.878801 0.079386 0.085 Uiso 1 1 calc R U . . .
H6B H 0.816866 0.858027 0.000379 0.085 Uiso 1 1 calc R U . . .
N1 N 0.91955(2) 0.77506(4) 0.09704(2) 0.0710(7) Uani 1 1 d D U . . .
O1 O 0.8138(3) 0.5267(8) -0.0033(3) 0.0710(7) Uani 1 1 d . U . . .
C7 C 0.6697(4) 0.3563(12) 0.4563(5) 0.0710(7) Uani 1 1 d . U . . .
H7A H 0.690268 0.448504 0.492689 0.106 Uiso 1 1 calc R U . . .
H7B H 0.675037 0.380908 0.410437 0.106 Uiso 1 1 calc R U . . .
H7C H 0.699629 0.256592 0.481258 0.106 Uiso 1 1 calc R U . . .
C8 C 0.5408(5) 0.4981(11) 0.4087(5) 0.0710(7) Uani 1 1 d . U . . .
H8A H 0.485840 0.485562 0.397798 0.106 Uiso 1 1 calc R U . . .
H8B H 0.541720 0.538172 0.362273 0.106 Uiso 1 1 calc R U . . .
H8C H 0.567912 0.577156 0.450909 0.106 Uiso 1 1 calc R U . . .
C9 C 0.5727(5) 0.2606(11) 0.5002(5) 0.0710(7) Uani 1 1 d . U . . .
H9A H 0.516173 0.265707 0.486493 0.085 Uiso 1 1 calc R U . . .
H9B H 0.603114 0.328585 0.546996 0.085 Uiso 1 1 calc R U . . .
C10 C 0.6020(5) 0.0791(12) 0.5177(5) 0.0710(7) Uani 1 1 d . U . . .
H10A H 0.659361 0.074935 0.534370 0.085 Uiso 1 1 calc R U . . .
H10B H 0.594087 0.036243 0.560423 0.085 Uiso 1 1 calc R U . . .
C11 C 0.5683(5) 0.0350(12) 0.3861(5) 0.0710(7) Uani 1 1 d . U . . .
H11A H 0.537971 -0.037546 0.341012 0.085 Uiso 1 1 calc R U . . .
H11B H 0.624833 0.027111 0.399735 0.085 Uiso 1 1 calc R U . . .
C12 C 0.5409(5) 0.2109(12) 0.3628(5) 0.0710(7) Uani 1 1 d . U . . .
H12A H 0.482996 0.217282 0.342849 0.085 Uiso 1 1 calc R U . . .
H12B H 0.552028 0.244966 0.320815 0.085 Uiso 1 1 calc R U . . .
N2 N 0.5834(4) 0.3300(10) 0.4326(4) 0.0710(7) Uani 1 1 d . U . . .
O2 O 0.5594(3) -0.0232(8) 0.4497(3) 0.0710(7) Uani 1 1 d . 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
Br1 Pb1 3.0089(9) . ?
Br1 Pb2 3.1004(9) 1_545 ?
Br2 Pb1 3.2129(10) . ?
Br2 Pb2 2.8727(11) 1_545 ?
Br3 Pb1 2.9033(8) . ?
Br4 Pb1 2.9171(12) . ?
Br5 Pb1 3.0240(7) . ?
Br5 Pb2 2.9846(7) . ?
Br6 Pb2 2.8812(9) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C1 N1 1.5000(5) . ?
C2 H2A 0.9600 . ?
C2 H2B 0.9600 . ?
C2 H2C 0.9600 . ?
C2 N1 1.5001(6) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C3 C4 1.521(10) . ?
C3 N1 1.4999(6) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C4 O1 1.482(9) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C5 C6 1.500(13) . ?
C5 O1 1.414(11) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C6 N1 1.504(7) . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C7 N2 1.480(11) . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C8 N2 1.516(11) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C9 C10 1.528(13) . ?
C9 N2 1.517(13) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C10 O2 1.421(10) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C11 C12 1.487(13) . ?
C11 O2 1.398(12) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C12 N2 1.524(11) . ?

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
Pb1 Br1 Pb2 81.65(2) . 1_545 ?
Pb2 Br2 Pb1 81.85(3) 1_545 . ?
Pb2 Br5 Pb1 83.177(17) . . ?
Br1 Pb1 Br2 82.92(3) . . ?
Br1 Pb1 Br5 177.95(3) . . ?
Br3 Pb1 Br1 88.40(3) . . ?
Br3 Pb1 Br2 77.56(2) . . ?
Br3 Pb1 Br4 88.00(3) . . ?
Br3 Pb1 Br5 92.39(2) . . ?
Br4 Pb1 Br1 91.86(4) . . ?
Br4 Pb1 Br2 164.74(3) . . ?
Br4 Pb1 Br5 86.28(2) . . ?
Br5 Pb1 Br2 99.09(2) . . ?
Br2 Pb2 Br1 87.20(3) 1_565 1_565 ?
Br2 Pb2 Br5 87.56(2) 1_565 . ?
Br2 Pb2 Br6 93.25(3) 1_565 . ?
Br5 Pb2 Br1 172.39(4) . 1_565 ?
Br6 Pb2 Br1 90.04(3) . 1_565 ?
Br6 Pb2 Br5 84.77(2) . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
N1 C1 H1A 109.5 . . ?
N1 C1 H1B 109.5 . . ?
N1 C1 H1C 109.5 . . ?
H2A C2 H2B 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
N1 C2 H2A 109.5 . . ?
N1 C2 H2B 109.5 . . ?
N1 C2 H2C 109.5 . . ?
H3A C3 H3B 108.6 . . ?
C4 C3 H3A 110.3 . . ?
C4 C3 H3B 110.3 . . ?
N1 C3 H3A 110.3 . . ?
N1 C3 H3B 110.3 . . ?
N1 C3 C4 106.9(4) . . ?
C3 C4 H4A 109.6 . . ?
C3 C4 H4B 109.6 . . ?
H4A C4 H4B 108.2 . . ?
O1 C4 C3 110.1(6) . . ?
O1 C4 H4A 109.6 . . ?
O1 C4 H4B 109.6 . . ?
H5A C5 H5B 108.0 . . ?
C6 C5 H5A 109.4 . . ?
C6 C5 H5B 109.4 . . ?
O1 C5 H5A 109.4 . . ?
O1 C5 H5B 109.4 . . ?
O1 C5 C6 111.2(7) . . ?
C5 C6 H6A 109.9 . . ?
C5 C6 H6B 109.9 . . ?
C5 C6 N1 108.7(6) . . ?
H6A C6 H6B 108.3 . . ?
N1 C6 H6A 109.9 . . ?
N1 C6 H6B 109.9 . . ?
C1 N1 C6 108.8(4) . . ?
C2 N1 C1 94.72(9) . . ?
C2 N1 C6 110.2(3) . . ?
C3 N1 C1 120.11(7) . . ?
C3 N1 C2 102.96(6) . . ?
C3 N1 C6 117.0(3) . . ?
C5 O1 C4 104.4(6) . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N2 C7 H7A 109.5 . . ?
N2 C7 H7B 109.5 . . ?
N2 C7 H7C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N2 C8 H8A 109.5 . . ?
N2 C8 H8B 109.5 . . ?
N2 C8 H8C 109.5 . . ?
H9A C9 H9B 108.1 . . ?
C10 C9 H9A 109.5 . . ?
C10 C9 H9B 109.5 . . ?
N2 C9 H9A 109.5 . . ?
N2 C9 H9B 109.5 . . ?
N2 C9 C10 110.6(8) . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 108.1 . . ?
O2 C10 C9 110.8(6) . . ?
O2 C10 H10A 109.5 . . ?
O2 C10 H10B 109.5 . . ?
H11A C11 H11B 107.7 . . ?
C12 C11 H11A 108.8 . . ?
C12 C11 H11B 108.8 . . ?
O2 C11 H11A 108.8 . . ?
O2 C11 H11B 108.8 . . ?
O2 C11 C12 114.0(9) . . ?
C11 C12 H12A 109.4 . . ?
C11 C12 H12B 109.4 . . ?
C11 C12 N2 111.2(6) . . ?
H12A C12 H12B 108.0 . . ?
N2 C12 H12A 109.4 . . ?
N2 C12 H12B 109.4 . . ?
C7 N2 C8 108.2(7) . . ?
C7 N2 C9 111.6(6) . . ?
C7 N2 C12 113.2(8) . . ?
C8 N2 C9 108.3(8) . . ?
C8 N2 C12 107.7(6) . . ?
C9 N2 C12 107.6(7) . . ?
C11 O2 C10 111.6(7) . . ?

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
C2 H2A Br1 0.96 2.79 3.435(2) 125.3 2_655 yes
C2 H2C Br4 0.96 2.90 3.8624(15) 176.4 1_655 yes
C3 H3A Br1 0.97 3.10 3.8296(10) 133.1 1_655 yes
C4 H4A Br6 0.97 2.82 3.541(9) 131.5 3_665 yes
C8 H8A Br5 0.96 3.12 3.567(8) 110.5 . yes
C11 H11A Br5 0.97 3.08 3.802(8) 132.0 1_545 yes
C12 H12B Br5 0.97 2.93 3.863(11) 162.9 2_645 yes

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
C3 C4 O1 C5 -71.4(8) . . . . ?
C4 C3 N1 C1 178.9(3) . . . . ?
C4 C3 N1 C2 75.5(3) . . . . ?
C4 C3 N1 C6 -45.5(5) . . . . ?
C5 C6 N1 C1 -175.1(5) . . . . ?
C5 C6 N1 C2 -72.5(6) . . . . ?
C5 C6 N1 C3 44.6(6) . . . . ?
C6 C5 O1 C4 70.4(7) . . . . ?
N1 C3 C4 O1 57.7(6) . . . . ?
O1 C5 C6 N1 -56.9(6) . . . . ?
C9 C10 O2 C11 58.5(10) . . . . ?
C10 C9 N2 C7 -70.5(8) . . . . ?
C10 C9 N2 C8 170.6(6) . . . . ?
C10 C9 N2 C12 54.3(8) . . . . ?
C11 C12 N2 C7 71.3(11) . . . . ?
C11 C12 N2 C8 -169.1(8) . . . . ?
C11 C12 N2 C9 -52.5(10) . . . . ?
C12 C11 O2 C10 -58.0(8) . . . . ?
N2 C9 C10 O2 -58.3(9) . . . . ?
O2 C11 C12 N2 55.5(10) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_5
_database_code_depnum_ccdc_archive 'CCDC 2094448'
loop_
_audit_author_name
_audit_author_address
'Mengmeng Lun'
;Southeast University
China
;
_audit_update_record             
;
2021-07-04 deposited with the CCDC.	2022-07-12 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C24 Br16 N4 O4 Pb4'
_chemical_formula_sum            'C24 Br16 N4 O4 Pb4'
_chemical_formula_weight         2515.60

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'
N N 0.0061 0.0033 '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'
Br Br -0.2901 2.4595 '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'

_space_group_crystal_system      trigonal
_space_group_IT_number           165
_space_group_name_H-M_alt        'P -3 c 1'
_space_group_name_Hall           '-P 3 2"c'

_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'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z+1/2'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z-1/2'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'

_cell_length_a                   17.425(2)
_cell_length_b                   17.425(2)
_cell_length_c                   7.9527(16)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     2091.1(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    383(2)
_cell_measurement_reflns_used    3403
_cell_measurement_theta_min      2.34
_cell_measurement_theta_max      20.95

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    3.995
_exptl_crystal_F_000             2184
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_absorpt_coefficient_mu    31.379
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      383(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            27913
_diffrn_reflns_av_unetI/netI     0.0511
_diffrn_reflns_av_R_equivalents  0.1557
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_theta_min         2.338
_diffrn_reflns_theta_max         22.783
_diffrn_reflns_theta_full        22.783
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             951
_reflns_number_gt                557
_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-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   .
_refine_ls_hydrogen_treatment    undef
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef       0.0068(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         951
_refine_ls_number_parameters     103
_refine_ls_number_restraints     66
_refine_ls_R_factor_all          0.2045
_refine_ls_R_factor_gt           0.1720
_refine_ls_wR_factor_ref         0.5125
_refine_ls_wR_factor_gt          0.4796
_refine_ls_goodness_of_fit_ref   2.073
_refine_ls_restrained_S_all      2.050
_refine_ls_shift/su_max          0.054
_refine_ls_shift/su_mean         0.012

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 0.3333 0.6667 0.44026(12) 0.1134(3) Uani 1 3 d S T P . .
Br1 Br 0.20223(10) 0.53514(9) 0.6743(3) 0.1953(10) Uani 1 1 d . . . . .
Br2 Br 0.12512(6) 0.12904(7) 0.3251(3) 0.3037(18) Uani 1 1 d D . . . .
Pb2 Pb 0.0000 0.0000 0.4362(2) 0.2275(7) Uani 1 3 d S T P . .
O1 O 0.3003(8) -0.0211(8) 0.472(4) 0.407(10) Uani 0.6667 1 d D U P . .
C4 C 0.284(3) 0.089(3) 0.592(6) 0.506(6) Uani 0.6667 1 d D U P . .
C5 C 0.3365(7) 0.0000 0.2500 0.132(4) Uani 1 2 d DS TU P . .
C3 C 0.291(4) 0.091(4) 0.565(8) 0.643(6) Uani 0.6666 1 d D U P . .
N1 N 0.2892(17) 0.1366(14) 0.302(4) 0.324(15) Uani 0.6666 1 d D U P . .
C6 C 0.21961(7) 0.06159(7) 0.3844(7) 0.970(6) Uani 0.6667 1 d D U P . .
Br3 Br 0.2646(5) -0.0336(10) 0.090(2) 1.375(14) Uani 0.6667 1 d D . P . .
C2 C 0.2379(9) -0.0160(10) 0.521(2) 0.200(5) Uani 0.8333 1 d D U P . .
C1 C 0.2124(12) -0.0383(10) 0.276(4) 0.192(5) Uani 0.6666 1 d D U 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 Br1 2.9495(17) 3_565 ?
Pb1 Br1 2.9496(17) . ?
Pb1 Br1 2.9496(17) 2_665 ?
Pb1 Br1 3.1159(18) 12_565 ?
Pb1 Br1 3.1160(18) 10_665 ?
Pb1 Br1 3.1160(18) 11 ?
Br1 Pb1 3.1159(18) 10_666 ?
Br2 Br2 1.200(4) 4 ?
Br2 Pb2 2.3847(14) . ?
Br2 Pb2 2.917(2) 7_556 ?
Br2 Pb2 3.037(2) 4 ?
Pb2 Pb2 1.016(4) 7_556 ?
Pb2 Br2 2.3847(14) 3 ?
Pb2 Br2 2.3847(14) 2 ?
Pb2 Br2 2.917(2) 8_556 ?
Pb2 Br2 2.917(2) 9_556 ?
Pb2 Br2 2.917(2) 7_556 ?
Pb2 Pb2 2.961(4) 4 ?
Pb2 Br2 3.037(2) 5 ?
Pb2 Br2 3.037(2) 6 ?
Pb2 Br2 3.037(2) 4 ?
O1 Br3 1.09(2) 5 ?
O1 C2 1.20(3) . ?
O1 C5 1.85(3) . ?
C4 C2 1.68(4) . ?
C4 Br3 1.83(5) 5 ?
C4 C6 1.91(5) . ?
C5 Br3 1.673(15) . ?
C5 Br3 1.673(15) 5 ?
C5 O1 1.85(3) 5 ?
C5 C1 1.93(2) 5 ?
C5 C1 1.93(2) . ?
C3 Br3 1.64(7) 5 ?
C3 C2 1.66(6) . ?
C3 C6 1.79(6) . ?
N1 C6 1.42(2) . ?
N1 C1 1.62(3) 5 ?
N1 Br3 2.07(3) 5 ?
C6 C1 1.52(3) 5 ?
C6 Br3 1.680(9) 5 ?
C6 C1 1.89(2) . ?
C6 C2 1.883(19) . ?
Br3 O1 1.09(2) 5 ?
Br3 C2 1.31(2) 5 ?
Br3 C3 1.64(7) 5 ?
Br3 C6 1.680(9) 5 ?
Br3 C1 1.72(3) . ?
Br3 C1 1.75(3) 5 ?
Br3 C4 1.83(5) 5 ?
Br3 N1 2.07(3) 5 ?
Br3 Br3 2.74(3) 5 ?
C2 Br3 1.31(2) 5 ?
C2 C1 1.99(3) . ?
C1 C1 1.23(3) 5 ?
C1 C6 1.52(3) 5 ?
C1 N1 1.62(3) 5 ?
C1 Br3 1.75(3) 5 ?

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
Br1 Pb1 Br1 84.42(6) 3_565 . ?
Br1 Pb1 Br1 84.42(6) 3_565 2_665 ?
Br1 Pb1 Br1 84.42(6) . 2_665 ?
Br1 Pb1 Br1 98.10(5) 3_565 12_565 ?
Br1 Pb1 Br1 98.41(6) . 12_565 ?
Br1 Pb1 Br1 176.37(6) 2_665 12_565 ?
Br1 Pb1 Br1 98.41(6) 3_565 10_665 ?
Br1 Pb1 Br1 176.37(6) . 10_665 ?
Br1 Pb1 Br1 98.09(5) 2_665 10_665 ?
Br1 Pb1 Br1 78.98(5) 12_565 10_665 ?
Br1 Pb1 Br1 176.37(6) 3_565 11 ?
Br1 Pb1 Br1 98.09(5) . 11 ?
Br1 Pb1 Br1 98.41(6) 2_665 11 ?
Br1 Pb1 Br1 78.98(5) 12_565 11 ?
Br1 Pb1 Br1 78.98(5) 10_665 11 ?
Pb1 Br1 Pb1 81.87(3) . 10_666 ?
Br2 Br2 Pb2 111.47(7) 4 . ?
Br2 Br2 Pb2 130.21(5) 4 7_556 ?
Pb2 Br2 Pb2 18.87(8) . 7_556 ?
Br2 Br2 Pb2 46.94(4) 4 4 ?
Pb2 Br2 Pb2 64.90(8) . 4 ?
Pb2 Br2 Pb2 83.77(3) 7_556 4 ?
Pb2 Pb2 Br2 111.74(7) 7_556 . ?
Pb2 Pb2 Br2 111.74(7) 7_556 3 ?
Br2 Pb2 Br2 107.12(7) . 3 ?
Pb2 Pb2 Br2 111.74(7) 7_556 2 ?
Br2 Pb2 Br2 107.12(7) . 2 ?
Br2 Pb2 Br2 107.11(7) 3 2 ?
Pb2 Pb2 Br2 49.40(5) 7_556 8_556 ?
Br2 Pb2 Br2 83.59(6) . 8_556 ?
Br2 Pb2 Br2 83.59(6) 3 8_556 ?
Br2 Pb2 Br2 161.13(8) 2 8_556 ?
Pb2 Pb2 Br2 49.40(5) 7_556 9_556 ?
Br2 Pb2 Br2 83.59(6) . 9_556 ?
Br2 Pb2 Br2 161.13(8) 3 9_556 ?
Br2 Pb2 Br2 83.59(6) 2 9_556 ?
Br2 Pb2 Br2 82.23(7) 8_556 9_556 ?
Pb2 Pb2 Br2 49.40(5) 7_556 7_556 ?
Br2 Pb2 Br2 161.13(8) . 7_556 ?
Br2 Pb2 Br2 83.59(6) 3 7_556 ?
Br2 Pb2 Br2 83.59(6) 2 7_556 ?
Br2 Pb2 Br2 82.23(7) 8_556 7_556 ?
Br2 Pb2 Br2 82.23(7) 9_556 7_556 ?
Pb2 Pb2 Pb2 180.0 7_556 4 ?
Br2 Pb2 Pb2 68.26(7) . 4 ?
Br2 Pb2 Pb2 68.26(7) 3 4 ?
Br2 Pb2 Pb2 68.26(7) 2 4 ?
Br2 Pb2 Pb2 130.60(5) 8_556 4 ?
Br2 Pb2 Pb2 130.60(5) 9_556 4 ?
Br2 Pb2 Pb2 130.60(5) 7_556 4 ?
Pb2 Pb2 Br2 133.17(4) 7_556 5 ?
Br2 Pb2 Br2 96.68(7) . 5 ?
Br2 Pb2 Br2 21.58(8) 3 5 ?
Br2 Pb2 Br2 93.07(7) 2 5 ?
Br2 Pb2 Br2 101.21(4) 8_556 5 ?
Br2 Pb2 Br2 176.57(7) 9_556 5 ?
Br2 Pb2 Br2 98.23(4) 7_556 5 ?
Pb2 Pb2 Br2 46.83(4) 4 5 ?
Pb2 Pb2 Br2 133.17(4) 7_556 6 ?
Br2 Pb2 Br2 93.07(7) . 6 ?
Br2 Pb2 Br2 96.68(7) 3 6 ?
Br2 Pb2 Br2 21.58(8) 2 6 ?
Br2 Pb2 Br2 176.57(7) 8_556 6 ?
Br2 Pb2 Br2 98.23(4) 9_556 6 ?
Br2 Pb2 Br2 101.21(4) 7_556 6 ?
Pb2 Pb2 Br2 46.83(4) 4 6 ?
Br2 Pb2 Br2 78.34(6) 5 6 ?
Pb2 Pb2 Br2 133.17(4) 7_556 4 ?
Br2 Pb2 Br2 21.58(8) . 4 ?
Br2 Pb2 Br2 93.07(7) 3 4 ?
Br2 Pb2 Br2 96.68(7) 2 4 ?
Br2 Pb2 Br2 98.23(4) 8_556 4 ?
Br2 Pb2 Br2 101.21(4) 9_556 4 ?
Br2 Pb2 Br2 176.57(7) 7_556 4 ?
Pb2 Pb2 Br2 46.83(4) 4 4 ?
Br2 Pb2 Br2 78.34(6) 5 4 ?
Br2 Pb2 Br2 78.34(6) 6 4 ?
Br3 O1 C2 69.8(14) 5 . ?
Br3 O1 C5 63.3(16) 5 . ?
C2 O1 C5 122(2) . . ?
C2 C4 Br3 43.7(14) . 5 ?
C2 C4 C6 62.7(16) . . ?
Br3 C4 C6 53.3(14) 5 . ?
Br3 C5 Br3 110.0(12) . 5 ?
Br3 C5 O1 122.4(9) . . ?
Br3 C5 O1 35.6(7) 5 . ?
Br3 C5 O1 35.6(7) . 5 ?
Br3 C5 O1 122.4(9) 5 5 ?
O1 C5 O1 152.1(13) . 5 ?
Br3 C5 C1 57.6(10) . 5 ?
Br3 C5 C1 56.5(10) 5 5 ?
O1 C5 C1 85.8(11) . 5 ?
O1 C5 C1 67.4(11) 5 5 ?
Br3 C5 C1 56.5(10) . . ?
Br3 C5 C1 57.6(10) 5 . ?
O1 C5 C1 67.4(11) . . ?
O1 C5 C1 85.8(11) 5 . ?
C1 C5 C1 37.2(12) 5 . ?
Br3 C3 C2 47.0(19) 5 . ?
Br3 C3 C6 58(2) 5 . ?
C2 C3 C6 66(2) . . ?
C6 N1 C1 59.6(12) . 5 ?
C6 N1 Br3 53.8(10) . 5 ?
C1 N1 Br3 54.0(13) 5 5 ?
N1 C6 C1 66.5(14) . 5 ?
N1 C6 Br3 83.1(14) . 5 ?
C1 C6 Br3 64.7(10) 5 5 ?
N1 C6 C3 88(2) . . ?
C1 C6 C3 118(2) 5 . ?
Br3 C6 C3 56(2) 5 . ?
N1 C6 C1 105.6(14) . . ?
C1 C6 C1 40.5(12) 5 . ?
Br3 C6 C1 58.4(9) 5 . ?
C3 C6 C1 110(2) . . ?
N1 C6 C2 123.7(14) . . ?
C1 C6 C2 94.8(9) 5 . ?
Br3 C6 C2 42.8(7) 5 . ?
C3 C6 C2 54(2) . . ?
C1 C6 C2 63.8(10) . . ?
N1 C6 C4 92.7(17) . . ?
C1 C6 C4 123.3(19) 5 . ?
Br3 C6 C4 60.6(18) 5 . ?
C3 C6 C4 6(2) . . ?
C1 C6 C4 112.6(18) . . ?
C2 C6 C4 52.7(15) . . ?
O1 Br3 C2 59.1(15) 5 5 ?
O1 Br3 C3 104(3) 5 5 ?
C2 Br3 C3 67(2) 5 5 ?
O1 Br3 C5 81.0(15) 5 . ?
C2 Br3 C5 127.6(12) 5 . ?
C3 Br3 C5 163(2) 5 . ?
O1 Br3 C6 134.3(16) 5 5 ?
C2 Br3 C6 76.8(10) 5 5 ?
C3 Br3 C6 65(2) 5 5 ?
C5 Br3 C6 122.3(10) . 5 ?
O1 Br3 C1 131.3(18) 5 . ?
C2 Br3 C1 111.5(14) 5 . ?
C3 Br3 C1 115(3) 5 . ?
C5 Br3 C1 69.3(10) . . ?
C6 Br3 C1 53.1(8) 5 . ?
O1 Br3 C1 92.2(16) 5 5 ?
C2 Br3 C1 79.8(14) 5 5 ?
C3 Br3 C1 126(2) 5 5 ?
C5 Br3 C1 68.5(11) . 5 ?
C6 Br3 C1 66.8(9) 5 5 ?
C1 Br3 C1 41.5(12) . 5 ?
O1 Br3 C4 100(2) 5 5 ?
C2 Br3 C4 62.4(15) 5 5 ?
C3 Br3 C4 5(2) 5 5 ?
C5 Br3 C4 166.7(17) . 5 ?
C6 Br3 C4 66.0(18) 5 5 ?
C1 Br3 C4 117.4(19) . 5 ?
C1 Br3 C4 124.4(18) 5 5 ?
O1 Br3 N1 177.0(19) 5 5 ?
C2 Br3 N1 118.0(13) 5 5 ?
C3 Br3 N1 73(2) 5 5 ?
C5 Br3 N1 101.7(12) . 5 ?
C6 Br3 N1 43.2(8) 5 5 ?
C1 Br3 N1 49.5(10) . 5 ?
C1 Br3 N1 87.7(11) 5 5 ?
C4 Br3 N1 77.4(19) 5 5 ?
O1 Br3 Br3 98.1(17) 5 5 ?
C2 Br3 Br3 114.5(12) 5 5 ?
C3 Br3 Br3 154(2) 5 5 ?
C5 Br3 Br3 35.0(6) . 5 ?
C6 Br3 Br3 88.9(6) 5 5 ?
C1 Br3 Br3 38.2(8) . 5 ?
C1 Br3 Br3 37.4(9) 5 5 ?
C4 Br3 Br3 154.9(18) 5 5 ?
N1 Br3 Br3 83.7(11) 5 5 ?
O1 C2 Br3 51.1(12) . 5 ?
O1 C2 C3 98(2) . . ?
Br3 C2 C3 66(2) 5 . ?
O1 C2 C4 104(2) . . ?
Br3 C2 C4 73.8(18) 5 . ?
C3 C2 C4 8(3) . . ?
O1 C2 C6 110.4(16) . . ?
Br3 C2 C6 60.3(8) 5 . ?
C3 C2 C6 60(2) . . ?
C4 C2 C6 64.6(19) . . ?
O1 C2 C1 77.7(18) . . ?
Br3 C2 C1 59.8(11) 5 . ?
C3 C2 C1 112(2) . . ?
C4 C2 C1 118(2) . . ?
C6 C2 C1 58.3(8) . . ?
C1 C1 C6 86(3) 5 5 ?
C1 C1 N1 137(4) 5 5 ?
C6 C1 N1 53.9(13) 5 5 ?
C1 C1 Br3 71(2) 5 . ?
C6 C1 Br3 62.1(12) 5 . ?
N1 C1 Br3 76.5(17) 5 . ?
C1 C1 Br3 67.9(19) 5 5 ?
C6 C1 Br3 153.8(14) 5 5 ?
N1 C1 Br3 149.1(19) 5 5 ?
Br3 C1 Br3 104.4(12) . 5 ?
C1 C1 C6 53.4(17) 5 . ?
C6 C1 C6 111.9(13) 5 . ?
N1 C1 C6 149.3(17) 5 . ?
Br3 C1 C6 123.9(11) . . ?
Br3 C1 C6 54.8(7) 5 . ?
C1 C1 C5 71.4(6) 5 . ?
C6 C1 C5 116.3(16) 5 . ?
N1 C1 C5 110.1(17) 5 . ?
Br3 C1 C5 54.2(7) . . ?
Br3 C1 C5 53.8(7) 5 . ?
C6 C1 C5 100.6(7) . . ?
C1 C1 C2 100(3) 5 . ?
C6 C1 C2 157.2(15) 5 . ?
N1 C1 C2 122.9(18) 5 . ?
Br3 C1 C2 140.6(13) . . ?
Br3 C1 C2 40.5(9) 5 . ?
C6 C1 C2 57.9(9) . . ?
C5 C1 C2 86.4(10) . . ?

_refine_diff_density_max         5.715
_refine_diff_density_min         -3.087
_refine_diff_density_rms         0.606


# start Validation Reply Form
_vrf_THETM01_5                   
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550
RESPONSE:This is related to the crystal quality. The crystal was poorly diffracting at high angle. 
;
_vrf_PLAT084_5                   
;
PROBLEM: High wR2 Value (i.e. > 0.25) ...................       0.51 Report
RESPONSE: The single crystal X-ray diffraction data of crystal become poor at 383k.
;
_vrf_PLAT082_5                   
;
PROBLEM: High R1 Value ..................................       0.17 Report
RESPONSE: The single crystal X-ray diffraction data of crystal become poor at 383k.
;
_vrf_PLAT220_5                   
;
PROBLEM: NonSolvent   Resd 1  C   Ueq(max)/Ueq(min) Range        7.3 Ratio 
RESPONSE:  The question is caused by slight distortion of structure and quasi-static motion of atoms.
;
_vrf_PLAT260_5                   
;
PROBLEM: Large Average Ueq of Residue Including       Br3      0.569 Check 
RESPONSE: This is assigned to the thermal vibrations of atom.
;
# end Validation Reply Form
####################################################################### 
# 
# 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_1_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 2067453'
loop_
_audit_author_name
_audit_author_address
'Mengmeng Lun'
;Southeast University
China
;
_audit_update_record             
;
2021-07-12 deposited with the CCDC.	2022-07-12 downloaded from the CCDC.
;
_audit_creation_date             2021-05-17
# publcif _publ_body_element loop end
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_shelx_SHELXL_version_number     2014/7
_publcif_funding_html            
;
;

_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C6 H13 Br4 N O Pb'
_chemical_formula_sum            'C6 H13 Br4 N O Pb'
_chemical_formula_weight         642.00
_chemical_absolute_configuration ?
_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'
N N 0.0061 0.0033 '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'
Br Br -0.2901 2.4595 '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           19
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'
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                   8.0355(2)
_cell_length_b                   9.4769(2)
_cell_length_c                   17.5267(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1334.69(5)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9951
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30.44
_cell_measurement_theta_min      2.32
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    24.584
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    3.195
_exptl_crystal_density_meas      3.195
_exptl_crystal_density_method    ?
_exptl_crystal_description       Block
_exptl_crystal_F_000             1144
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.5
_exptl_transmission_factor_max   0.304
_exptl_transmission_factor_min   0.293
_diffrn_reflns_av_R_equivalents  0.0845
_diffrn_reflns_av_unetI/netI     0.0513
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            33467
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.528
_diffrn_reflns_theta_min         2.324
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.749
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                3460
_reflns_number_total             4090
_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       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_refine_diff_density_max         2.092
_refine_diff_density_min         -4.354
_refine_diff_density_rms         0.510
_refine_ls_abs_structure_details 
;
 Flack x determined using 1310 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.016(10)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     119
_refine_ls_number_reflns         4090
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0610
_refine_ls_R_factor_gt           0.0502
_refine_ls_restrained_S_all      1.068
_refine_ls_shift/su_max          0.060
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1055P)²+6.6076P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1554
_refine_ls_wR_factor_ref         0.1653
_refine_special_details          ?
_olex2_refinement_description    
;
1. Restrained distances
 C1-Br1
 1.95 with sigma of 0.001
2.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B)
2.b Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C)
;
_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 0.41345(2) 0.25889(2) 0.50065(2) 0.03304(4) Uani 1 1 d . . . . .
Br1 Br 0.47363(6) 0.67927(15) 0.57983(11) 0.1557(7) Uani 1 1 d D . . . .
Br2 Br 0.20418(8) 0.05962(6) 0.57878(3) 0.04373(13) Uani 1 1 d . . . . .
Br3 Br 0.61791(7) 0.02582(5) 0.45362(3) 0.04236(13) Uani 1 1 d . . . . .
Br4 Br 0.63838(7) 0.28654(6) 0.63135(3) 0.04181(13) Uani 1 1 d . . . . .
N1 N 0.7401(5) 0.7556(4) 0.6624(2) 0.0308(9) Uani 1 1 d . . . . .
O1 O 0.9212(5) 0.9741(4) 0.7388(3) 0.0492(11) Uani 1 1 d . . . . .
C1 C 0.70875(6) 0.73002(19) 0.5799(4) 0.087(2) Uani 1 1 d D . . . .
H1A H 0.7772 0.6536 0.5606 0.104 Uiso 1 1 calc R U . . .
H1B H 0.7290 0.8143 0.5499 0.104 Uiso 1 1 calc R U . . .
C2 C 0.7058(9) 0.6493(7) 0.7200(4) 0.0557(17) Uani 1 1 d . . . . .
H2A H 0.5910 0.6219 0.7172 0.083 Uiso 1 1 calc R U . . .
H2B H 0.7287 0.6874 0.7697 0.083 Uiso 1 1 calc R U . . .
H2C H 0.7751 0.5684 0.7113 0.083 Uiso 1 1 calc R U . . .
C3 C 0.9298(7) 0.7731(6) 0.6585(4) 0.0473(14) Uani 1 1 d . . . . .
H3A H 0.9810 0.6812 0.6521 0.057 Uiso 1 1 calc R U . . .
H3B H 0.9582 0.8300 0.6144 0.057 Uiso 1 1 calc R U . . .
C4 C 0.9971(8) 0.8404(8) 0.7276(4) 0.0569(18) Uani 1 1 d . . . . .
H4A H 0.9761 0.7807 0.7715 0.068 Uiso 1 1 calc R U . . .
H4B H 1.1165 0.8520 0.7225 0.068 Uiso 1 1 calc R U . . .
C5 C 0.7545(8) 0.9638(7) 0.7481(4) 0.0605(18) Uani 1 1 d . . . . .
H5A H 0.7088 1.0572 0.7566 0.073 Uiso 1 1 calc R U . . .
H5B H 0.7314 0.9073 0.7930 0.073 Uiso 1 1 calc R U . . .
C6 C 0.6686(6) 0.8968(6) 0.6787(4) 0.0418(14) Uani 1 1 d . . . . .
H6A H 0.5503 0.8878 0.6886 0.050 Uiso 1 1 calc R U . . .
H6B H 0.6828 0.9573 0.6345 0.050 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 2.8756(6) . ?
Pb1 Br2 3.2177(6) 4_556 ?
Pb1 Br3 3.2319(6) 4_456 ?
Pb1 Br3 2.8735(5) . ?
Pb1 Br4 3.2285(6) 4_456 ?
Pb1 Br4 2.9296(6) . ?
Br1 C1 1.9496(8) . ?
Br2 Pb1 3.2177(6) 4_456 ?
Br3 Pb1 3.2319(6) 4_556 ?
Br4 Pb1 3.2285(6) 4_556 ?
N1 C1 1.487(8) . ?
N1 C2 1.453(8) . ?
N1 C3 1.535(7) . ?
N1 C6 1.485(7) . ?
O1 C4 1.420(8) . ?
O1 C5 1.353(8) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 H2A 0.9600 . ?
C2 H2B 0.9600 . ?
C2 H2C 0.9600 . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C3 C4 1.471(9) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C5 C6 1.537(9) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?

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 168.997(18) . 4_556 ?
Br2 Pb1 Br3 107.658(15) 4_556 4_456 ?
Br2 Pb1 Br3 82.343(16) . 4_456 ?
Br2 Pb1 Br4 104.971(15) 4_556 4_456 ?
Br2 Pb1 Br4 81.563(16) . 4_456 ?
Br2 Pb1 Br4 92.705(17) . . ?
Br3 Pb1 Br2 88.062(17) . . ?
Br3 Pb1 Br2 82.627(15) . 4_556 ?
Br3 Pb1 Br3 167.558(17) . 4_456 ?
Br3 Pb1 Br4 86.580(17) . . ?
Br3 Pb1 Br4 94.783(16) . 4_456 ?
Br4 Pb1 Br2 80.941(16) . 4_556 ?
Br4 Pb1 Br3 101.708(16) . 4_456 ?
Br4 Pb1 Br3 76.044(15) 4_456 4_456 ?
Br4 Pb1 Br4 174.048(15) . 4_456 ?
Pb1 Br2 Pb1 82.388(14) . 4_456 ?
Pb1 Br3 Pb1 82.167(13) . 4_556 ?
Pb1 Br4 Pb1 81.382(13) . 4_556 ?
C1 N1 C3 98.2(3) . . ?
C2 N1 C1 122.1(4) . . ?
C2 N1 C3 107.1(4) . . ?
C2 N1 C6 114.7(4) . . ?
C6 N1 C1 105.5(4) . . ?
C6 N1 C3 107.2(4) . . ?
C5 O1 C4 112.2(5) . . ?
Br1 C1 H1A 111.4 . . ?
Br1 C1 H1B 111.4 . . ?
N1 C1 Br1 101.9(3) . . ?
N1 C1 H1A 111.4 . . ?
N1 C1 H1B 111.4 . . ?
H1A C1 H1B 109.3 . . ?
N1 C2 H2A 109.5 . . ?
N1 C2 H2B 109.5 . . ?
N1 C2 H2C 109.5 . . ?
H2A C2 H2B 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
N1 C3 H3A 109.2 . . ?
N1 C3 H3B 109.2 . . ?
H3A C3 H3B 107.9 . . ?
C4 C3 N1 112.1(5) . . ?
C4 C3 H3A 109.2 . . ?
C4 C3 H3B 109.2 . . ?
O1 C4 C3 110.0(5) . . ?
O1 C4 H4A 109.7 . . ?
O1 C4 H4B 109.7 . . ?
C3 C4 H4A 109.7 . . ?
C3 C4 H4B 109.7 . . ?
H4A C4 H4B 108.2 . . ?
O1 C5 H5A 109.2 . . ?
O1 C5 H5B 109.1 . . ?
O1 C5 C6 112.3(5) . . ?
H5A C5 H5B 107.9 . . ?
C6 C5 H5A 109.2 . . ?
C6 C5 H5B 109.1 . . ?
N1 C6 C5 110.5(4) . . ?
N1 C6 H6A 109.5 . . ?
N1 C6 H6B 109.5 . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
H6A C6 H6B 108.1 . . ?

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
C1 H1B Br1 0.97 3.01 3.621(5) 122.4 4_566
C1 H1B Br3 0.97 2.77 3.646(4) 150.8 1_565
C2 H2B Br2 0.96 2.97 3.699(7) 133.8 3_656
C3 H3A Br3 0.97 2.91 3.765(6) 147.0 4_556
C3 H3B Br2 0.97 3.01 3.767(6) 136.3 1_665
C6 H6B Br4 0.97 3.14 3.793(5) 126.0 1_565

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_123
_database_code_depnum_ccdc_archive 'CCDC 2096017'
loop_
_audit_author_name
_audit_author_address
'Mengmeng Lun'
;Southeast University
China
;
_audit_update_record             
;
2021-07-12 deposited with the CCDC.	2022-07-12 downloaded from the CCDC.
;
_audit_creation_date             2021-05-17
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C6 H13 Br3 Cl N O Pb'
_chemical_formula_sum            'C6 H13 Br3 Cl N O Pb'
_chemical_formula_weight         597.54
_chemical_absolute_configuration ?
_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'
N N 0.0061 0.0033 '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'
Cl Cl 0.1484 0.1585 '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'
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           19
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'
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                   8.0374(3)
_cell_length_b                   9.4801(4)
_cell_length_c                   17.5303(8)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1335.73(10)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9941
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      30.48
_cell_measurement_theta_min      2.32
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    21.773
_exptl_absorpt_correction_T_max  0.102
_exptl_absorpt_correction_T_min  0.092
_exptl_absorpt_correction_type   None
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    2.971
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       Block
_exptl_crystal_F_000             1072
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.105
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0990
_diffrn_reflns_av_unetI/netI     0.0543
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            32172
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.498
_diffrn_reflns_theta_min         2.324
_diffrn_ambient_temperature      298(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.748
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                3448
_reflns_number_total             4086
_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       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    ?
_refine_diff_density_max         0.777
_refine_diff_density_min         -4.520
_refine_diff_density_rms         0.402
_refine_ls_abs_structure_details 
;
 Flack x determined using 1310 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.012(6)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.129
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     119
_refine_ls_number_reflns         4086
_refine_ls_number_restraints     81
_refine_ls_R_factor_all          0.0383
_refine_ls_R_factor_gt           0.0272
_refine_ls_restrained_S_all      1.119
_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)+(0.0001P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0544
_refine_ls_wR_factor_ref         0.0627
_refine_special_details          ?
_olex2_refinement_description    
;
1. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
2. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
3.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B)
3.b Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C)
;
_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 0.08656(2) 0.25888(2) 0.50065(2) 0.03274(8) Uani 1 1 d . U . . .
Br1 Br 0.36155(9) 0.21348(8) 0.36867(4) 0.04168(17) Uani 1 1 d . U . . .
Br2 Br -0.20458(10) 0.44027(8) 0.42133(4) 0.04435(18) Uani 1 1 d . U . . .
Br3 Br -0.11796(9) 0.02597(7) 0.45347(5) 0.04233(18) Uani 1 1 d . U . . .
Cl1 Cl 0.5268(2) 0.8223(3) 0.41982(14) 0.0619(6) Uani 1 1 d . U . . .
O1 O 0.0760(7) 0.5242(6) 0.2597(4) 0.0540(14) Uani 1 1 d . U . . .
N1 N 0.2569(6) 0.7446(5) 0.3379(3) 0.0281(10) Uani 1 1 d . U . . .
C1 C 0.3311(9) 0.6031(7) 0.3184(5) 0.0447(17) Uani 1 1 d . U . . .
H1A H 0.4494 0.6141 0.3092 0.054 Uiso 1 1 calc R U . . .
H1B H 0.3173 0.5397 0.3614 0.054 Uiso 1 1 calc R U . . .
C2 C 0.2506(10) 0.5394(9) 0.2490(5) 0.053(2) Uani 1 1 d . U . . .
H2A H 0.2714 0.5992 0.2052 0.064 Uiso 1 1 calc R U . . .
H2B H 0.2995 0.4477 0.2390 0.064 Uiso 1 1 calc R U . . .
C3 C -0.0008(10) 0.6577(9) 0.2716(5) 0.053(2) Uani 1 1 d . U . . .
H3A H -0.1199 0.6456 0.2775 0.064 Uiso 1 1 calc R U . . .
H3B H 0.0187 0.7181 0.2279 0.064 Uiso 1 1 calc R U . . .
C4 C 0.0706(8) 0.7253(8) 0.3424(5) 0.0449(17) Uani 1 1 d . U . . .
H4A H 0.0442 0.6670 0.3862 0.054 Uiso 1 1 calc R U . . .
H4B H 0.0185 0.8165 0.3499 0.054 Uiso 1 1 calc R U . . .
C5 C 0.3117(9) 0.7920(9) 0.4154(4) 0.0450(17) Uani 1 1 d . U . . .
H5A H 0.2819 0.7207 0.4526 0.054 Uiso 1 1 calc R U . . .
H5B H 0.2534 0.8782 0.4286 0.054 Uiso 1 1 calc R U . . .
C6 C 0.3013(11) 0.8546(8) 0.2794(5) 0.053(2) Uani 1 1 d . U . . .
H6A H 0.2408 0.8368 0.2332 0.080 Uiso 1 1 calc R U . . .
H6B H 0.4186 0.8506 0.2692 0.080 Uiso 1 1 calc R U . . .
H6C H 0.2730 0.9463 0.2986 0.080 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 Br1 3.2285(8) . ?
Pb1 Br1 2.9305(8) 4_456 ?
Pb1 Br2 2.8729(8) 4_556 ?
Pb1 Br2 3.2197(8) . ?
Pb1 Br3 3.2322(7) 4_556 ?
Pb1 Br3 2.8742(7) . ?
Br1 Pb1 2.9304(8) 4_556 ?
Br2 Pb1 2.8729(8) 4_456 ?
Br3 Pb1 3.2322(7) 4_456 ?
Cl1 C5 1.754(7) . ?
O1 C2 1.424(10) . ?
O1 C3 1.423(10) . ?
N1 C1 1.507(8) . ?
N1 C4 1.511(8) . ?
N1 C5 1.497(9) . ?
N1 C6 1.505(9) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C1 C2 1.504(11) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C3 C4 1.509(11) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?

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
Br1 Pb1 Br1 174.06(2) 4_456 . ?
Br1 Pb1 Br2 80.87(2) 4_456 . ?
Br1 Pb1 Br3 101.68(2) 4_456 4_556 ?
Br1 Pb1 Br3 76.080(19) . 4_556 ?
Br2 Pb1 Br1 105.03(2) . . ?
Br2 Pb1 Br1 92.70(2) 4_556 4_456 ?
Br2 Pb1 Br1 81.58(2) 4_556 . ?
Br2 Pb1 Br2 168.90(2) 4_556 . ?
Br2 Pb1 Br3 82.35(2) 4_556 4_556 ?
Br2 Pb1 Br3 88.07(2) 4_556 . ?
Br2 Pb1 Br3 107.73(2) . 4_556 ?
Br3 Pb1 Br1 94.76(2) . . ?
Br3 Pb1 Br1 86.60(2) . 4_456 ?
Br3 Pb1 Br2 82.55(2) . . ?
Br3 Pb1 Br3 167.57(2) . 4_556 ?
Pb1 Br1 Pb1 81.392(18) 4_556 . ?
Pb1 Br2 Pb1 82.419(19) 4_456 . ?
Pb1 Br3 Pb1 82.176(17) . 4_456 ?
C3 O1 C2 110.9(6) . . ?
C1 N1 C4 107.2(5) . . ?
C5 N1 C1 110.9(5) . . ?
C5 N1 C4 106.3(5) . . ?
C5 N1 C6 109.9(6) . . ?
C6 N1 C1 111.6(6) . . ?
C6 N1 C4 110.7(6) . . ?
N1 C1 H1A 109.3 . . ?
N1 C1 H1B 109.3 . . ?
H1A C1 H1B 107.9 . . ?
C2 C1 N1 111.7(6) . . ?
C2 C1 H1A 109.3 . . ?
C2 C1 H1B 109.3 . . ?
O1 C2 C1 111.0(7) . . ?
O1 C2 H2A 109.4 . . ?
O1 C2 H2B 109.4 . . ?
C1 C2 H2A 109.4 . . ?
C1 C2 H2B 109.4 . . ?
H2A C2 H2B 108.0 . . ?
O1 C3 H3A 109.8 . . ?
O1 C3 H3B 109.8 . . ?
O1 C3 C4 109.5(7) . . ?
H3A C3 H3B 108.2 . . ?
C4 C3 H3A 109.8 . . ?
C4 C3 H3B 109.8 . . ?
N1 C4 H4A 109.1 . . ?
N1 C4 H4B 109.1 . . ?
C3 C4 N1 112.7(6) . . ?
C3 C4 H4A 109.1 . . ?
C3 C4 H4B 109.1 . . ?
H4A C4 H4B 107.8 . . ?
Cl1 C5 H5A 109.2 . . ?
Cl1 C5 H5B 109.2 . . ?
N1 C5 Cl1 112.3(5) . . ?
N1 C5 H5A 109.2 . . ?
N1 C5 H5B 109.2 . . ?
H5A C5 H5B 107.9 . . ?
N1 C6 H6A 109.5 . . ?
N1 C6 H6B 109.5 . . ?
N1 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?

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
C1 H1B Br1 0.97 3.12 3.805(7) 129.3 .
C1 H1B Br1 0.97 3.12 3.805(7) 129.3 .
C1 H1B Br1 0.97 3.12 3.805(7) 129.3 .
C1 H1B Br1 0.97 3.12 3.805(7) 129.3 .
C2 H2A Br3 0.97 3.12 3.709(9) 120.6 3
C2 H2A Br3 0.97 3.12 3.709(9) 120.6 3
C2 H2A Br3 0.97 3.12 3.709(9) 120.6 3
C2 H2A Br3 0.97 3.12 3.709(9) 120.6 3
C4 H4A Br2 0.97 3.00 3.756(8) 135.8 .
C4 H4A Br2 0.97 3.00 3.756(8) 135.8 .
C4 H4A Br2 0.97 3.00 3.756(8) 135.8 .
C4 H4A Br2 0.97 3.00 3.756(8) 135.8 .
C4 H4B Br3 0.97 2.91 3.770(7) 149.0 1_565
C4 H4B Br3 0.97 2.91 3.770(7) 149.0 1_565
C4 H4B Br3 0.97 2.91 3.770(7) 149.0 1_565
C4 H4B Br3 0.97 2.91 3.770(7) 149.0 1_565
C5 H5A Br3 0.97 2.97 3.833(9) 148.7 4_556
C5 H5A Br3 0.97 2.97 3.833(9) 148.7 4_556
C5 H5A Br3 0.97 2.97 3.833(9) 148.7 4_556
C5 H5A Br3 0.97 2.97 3.833(9) 148.7 4_556
C6 H6A Br2 0.96 2.90 3.694(8) 141.4 3
C6 H6A Br2 0.96 2.90 3.694(8) 141.4 3
C6 H6A Br2 0.96 2.90 3.694(8) 141.4 3
C6 H6A Br2 0.96 2.90 3.694(8) 141.4 3
C6 H6C Br1 0.96 2.90 3.776(8) 151.7 1_565
C6 H6C Br1 0.96 2.90 3.776(8) 151.7 1_565
C6 H6C Br1 0.96 2.90 3.776(8) 151.7 1_565
C6 H6C Br1 0.96 2.90 3.776(8) 151.7 1_565

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
O1 C3 C4 N1 58.2(9) . . . . ?
N1 C1 C2 O1 -57.7(9) . . . . ?
C1 N1 C4 C3 -53.2(8) . . . . ?
C1 N1 C5 Cl1 64.7(7) . . . . ?
C2 O1 C3 C4 -60.8(9) . . . . ?
C3 O1 C2 C1 61.4(10) . . . . ?
C4 N1 C1 C2 52.3(8) . . . . ?
C4 N1 C5 Cl1 -179.1(6) . . . . ?
C5 N1 C1 C2 168.0(7) . . . . ?
C5 N1 C4 C3 -171.9(7) . . . . ?
C6 N1 C1 C2 -69.2(8) . . . . ?
C6 N1 C4 C3 68.8(8) . . . . ?
C6 N1 C5 Cl1 -59.2(7) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
