# Electronic Supplementary Material (ESI) for Materials Horizons.
# This journal is © The Royal Society of Chemistry 2023

####################################################################### 
# 
# 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_wa2pbbr4_auto
_database_code_depnum_ccdc_archive 'CCDC 2252913'
loop_
_audit_author_name
_audit_author_address
'Shihai You'
;Fujian Institute of Research on the Structure of Matter, Chinese Academy of Sciences
China
;
_audit_update_record             
;
2023-03-30 deposited with the CCDC.	2023-09-12 downloaded from the CCDC.
;
_audit_creation_date             2023-03-25
_audit_creation_method           
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Br4 Pb, 2(C5 H14 N)'
_chemical_formula_sum            'C10 H28 Br4 N2 Pb'
_chemical_formula_weight         703.17
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C H N Pb Br'
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'
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                   14.4011(5)
_cell_length_b                   8.2390(2)
_cell_length_c                   8.3208(2)
_cell_angle_alpha                90
_cell_angle_beta                 94.932(3)
_cell_angle_gamma                90
_cell_volume                     983.61(5)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    5570
_cell_measurement_temperature    100.0(8)
_cell_measurement_theta_max      30.8320
_cell_measurement_theta_min      2.8240
_shelx_estimated_absorpt_T_max   0.851
_shelx_estimated_absorpt_T_min   0.135
_exptl_absorpt_coefficient_mu    16.688
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.11356
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.73a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.374
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             648
_exptl_crystal_preparation       ?
_exptl_crystal_recrystallization_method ?
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.01
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0403
_diffrn_reflns_av_unetI/netI     0.0373
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.837
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            8946
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.837
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.443
_diffrn_reflns_theta_min         2.839
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.0(8)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.837
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -32.00  -6.00   0.50    0.32    --   -5.22  97.00 116.00   52
  2  ω    -17.00  27.00   0.50    0.32    --   -5.22 -99.00-150.00   88
  3  ω    -17.00  29.00   0.50    0.32    --    6.86 -99.00 -60.00   92
  4  ω    -23.00   6.00   0.50    0.32    --   -5.22 -97.00   7.00   58
  5  ω    -15.00  38.00   0.50    0.32    --    6.86 -97.00   7.00  106
  6  ω     -4.00  79.00   0.50    0.32    --    6.86  57.00-180.00  166
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0057544000
_diffrn_orient_matrix_UB_12      0.0381211000
_diffrn_orient_matrix_UB_13      -0.0749122000
_diffrn_orient_matrix_UB_21      0.0163531000
_diffrn_orient_matrix_UB_22      0.0711589000
_diffrn_orient_matrix_UB_23      0.0412450000
_diffrn_orient_matrix_UB_31      0.0463022000
_diffrn_orient_matrix_UB_32      -0.0298956000
_diffrn_orient_matrix_UB_33      0.0025547000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Mova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2200
_reflns_number_total             2496
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.73a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.73a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.73a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         1.523
_refine_diff_density_min         -1.626
_refine_diff_density_rms         0.295
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     81
_refine_ls_number_reflns         2496
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0363
_refine_ls_R_factor_gt           0.0296
_refine_ls_restrained_S_all      1.051
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0479P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0736
_refine_ls_wR_factor_ref         0.0761
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C1(H1D,H1E), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B)
2.b Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C), C5(H5A,H5B,H5C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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 1.000000 1.000000 0.500000 0.00973(9) Uani 1 2 d S . P . .
Br1 Br 1.00189(3) 0.80676(5) 0.80539(5) 0.01460(12) Uani 1 1 d . . . . .
Br2 Br 0.79203(3) 0.96151(6) 0.44852(5) 0.01473(12) Uani 1 1 d . . . . .
N1 N 0.8293(3) 0.9291(5) 1.0532(4) 0.0161(8) Uani 1 1 d . . . . .
H1A H 0.814935 0.828250 1.014023 0.019 Uiso 1 1 calc R U . . .
H1B H 0.804739 0.942553 1.149533 0.019 Uiso 1 1 calc R U . . .
H1C H 0.892322 0.940474 1.067261 0.019 Uiso 1 1 calc R U . . .
C1 C 0.7893(4) 1.0553(6) 0.9352(5) 0.0159(10) Uani 1 1 d . . . . .
H1D H 0.794014 1.163418 0.987162 0.019 Uiso 1 1 calc R U . . .
H1E H 0.826573 1.057709 0.840720 0.019 Uiso 1 1 calc R U . . .
C2 C 0.6893(4) 1.0222(6) 0.8791(6) 0.0170(10) Uani 1 1 d . . . . .
H2A H 0.652112 1.014919 0.973452 0.020 Uiso 1 1 calc R U . . .
H2B H 0.684581 0.916930 0.821594 0.020 Uiso 1 1 calc R U . . .
C3 C 0.6500(4) 1.1575(6) 0.7661(6) 0.0184(10) Uani 1 1 d . . . . .
H3A H 0.639849 1.255378 0.831295 0.022 Uiso 1 1 calc R U . . .
H3B H 0.697133 1.185211 0.690530 0.022 Uiso 1 1 calc R U . . .
C4 C 0.5595(4) 1.1149(6) 0.6690(6) 0.0213(11) Uani 1 1 d . . . . .
H4A H 0.568686 1.013560 0.608327 0.026 Uiso 1 1 calc R U . . .
H4B H 0.544134 1.202146 0.589370 0.026 Uiso 1 1 calc R U . . .
C5 C 0.4778(4) 1.0920(7) 0.7700(6) 0.0261(12) Uani 1 1 d . . . . .
H5A H 0.422043 1.064252 0.699577 0.039 Uiso 1 1 calc R U . . .
H5B H 0.466888 1.192750 0.827997 0.039 Uiso 1 1 calc R U . . .
H5C H 0.491783 1.004104 0.847731 0.039 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 2.9968(4) 3_776 ?
Pb1 Br1 3.0031(4) 2_756 ?
Pb1 Br1 2.9968(4) . ?
Pb1 Br1 3.0031(4) 4_575 ?
Pb1 Br2 3.0056(5) 3_776 ?
Pb1 Br2 3.0056(5) . ?
N1 H1A 0.9100 . ?
N1 H1B 0.9100 . ?
N1 H1C 0.9100 . ?
N1 C1 1.510(6) . ?
C1 H1D 0.9900 . ?
C1 H1E 0.9900 . ?
C1 C2 1.500(7) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C2 C3 1.535(7) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C3 C4 1.514(7) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C4 C5 1.515(8) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?

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 3_776 . ?
Br1 Pb1 Br1 89.412(4) . 2_756 ?
Br1 Pb1 Br1 90.588(4) 3_776 2_756 ?
Br1 Pb1 Br1 89.412(4) 3_776 4_575 ?
Br1 Pb1 Br1 90.588(4) . 4_575 ?
Br1 Pb1 Br1 180.000(13) 4_575 2_756 ?
Br1 Pb1 Br2 83.655(13) 4_575 . ?
Br1 Pb1 Br2 89.936(13) 3_776 . ?
Br1 Pb1 Br2 83.655(13) 2_756 3_776 ?
Br1 Pb1 Br2 89.936(13) . 3_776 ?
Br1 Pb1 Br2 90.063(13) . . ?
Br1 Pb1 Br2 96.345(13) 4_575 3_776 ?
Br1 Pb1 Br2 90.064(13) 3_776 3_776 ?
Br1 Pb1 Br2 96.345(13) 2_756 . ?
Br2 Pb1 Br2 180.0 3_776 . ?
Pb1 Br1 Pb1 154.757(16) . 2_746 ?
H1A N1 H1B 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1B N1 H1C 109.5 . . ?
C1 N1 H1A 109.5 . . ?
C1 N1 H1B 109.5 . . ?
C1 N1 H1C 109.5 . . ?
N1 C1 H1D 109.1 . . ?
N1 C1 H1E 109.1 . . ?
H1D C1 H1E 107.9 . . ?
C2 C1 N1 112.3(4) . . ?
C2 C1 H1D 109.1 . . ?
C2 C1 H1E 109.1 . . ?
C1 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
C1 C2 C3 110.6(4) . . ?
H2A C2 H2B 108.1 . . ?
C3 C2 H2A 109.5 . . ?
C3 C2 H2B 109.5 . . ?
C2 C3 H3A 108.7 . . ?
C2 C3 H3B 108.7 . . ?
H3A C3 H3B 107.6 . . ?
C4 C3 C2 114.4(4) . . ?
C4 C3 H3A 108.7 . . ?
C4 C3 H3B 108.7 . . ?
C3 C4 H4A 108.8 . . ?
C3 C4 H4B 108.8 . . ?
C3 C4 C5 114.0(4) . . ?
H4A C4 H4B 107.6 . . ?
C5 C4 H4A 108.8 . . ?
C5 C4 H4B 108.8 . . ?
C4 C5 H5A 109.5 . . ?
C4 C5 H5B 109.5 . . ?
C4 C5 H5C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 C1 C2 C3 177.2(4) . . . . ?
C1 C2 C3 C4 164.6(4) . . . . ?
C2 C3 C4 C5 66.2(6) . . . . ?


_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 6.722
_oxdiff_exptl_absorpt_empirical_full_min 0.522
####################################################################### 
# 
# 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_220728e14_r_auto
_database_code_depnum_ccdc_archive 'CCDC 2252914'
loop_
_audit_author_name
_audit_author_address
'Shihai You'
;Fujian Institute of Research on the Structure of Matter, Chinese Academy of Sciences
China
;
_audit_update_record             
;
2023-03-30 deposited with the CCDC.	2023-09-12 downloaded from the CCDC.
;
_audit_creation_date             2023-03-25
_audit_creation_method           
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Br4 Pb, C9 H14 N, C5 H14 N'
_chemical_formula_sum            'C14 H28 Br4 N2 Pb'
_chemical_formula_weight         751.21
_chemical_absolute_configuration ad
_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'
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                   8.0160(3)
_cell_length_b                   8.4161(4)
_cell_length_c                   34.5711(19)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2332.29(19)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    6099
_cell_measurement_temperature    300.47(10)
_cell_measurement_theta_max      29.4920
_cell_measurement_theta_min      2.3520
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    14.084
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.16462
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.73a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.139
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1392
_exptl_crystal_preparation       ?
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.02
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0551
_diffrn_reflns_av_unetI/netI     0.0530
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            11584
_diffrn_reflns_point_group_measured_fraction_full 0.979
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        24.997
_diffrn_reflns_theta_max         24.997
_diffrn_reflns_theta_min         2.491
_diffrn_ambient_temperature      300.15
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -19.00   9.00   0.50    1.05    --    6.70  92.00 133.00   56
  2  ω    -17.00  27.00   0.50    1.05    --   -5.06 -99.00 150.00   88
  3  ω    -18.00  33.00   0.50    1.05    --   -5.06  38.00 -62.00  102
  4  ω      3.00  57.00   0.50    1.05    --    6.70  38.00-150.00  108
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.684
_reflns_Friedel_fraction_full    0.951
_reflns_Friedel_fraction_max     0.951
_reflns_number_gt                3336
_reflns_number_total             4020
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.73a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.73a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.73a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         1.370
_refine_diff_density_min         -1.213
_refine_diff_density_rms         0.190
_refine_ls_abs_structure_details 
;
 Flack x determined using 1161 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.024(13)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     158
_refine_ls_number_reflns         4020
_refine_ls_number_restraints     28
_refine_ls_R_factor_all          0.0606
_refine_ls_R_factor_gt           0.0458
_refine_ls_restrained_S_all      1.051
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0621P)²+1.0486P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1048
_refine_ls_wR_factor_ref         0.1099
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C13-C14 = C13-C12 = C11-C12 = C11-C10
 1.5 with sigma of 0.01
 C12-C11
 1.5 with sigma of 0.01
 C14-C13
 1.5 with sigma of 0.01
 C3-C2 = C2-C1
 1.5 with sigma of 0.01
 N2-C14
 1.5 with sigma of 0.01
 C11-C10
 1.5 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C7) \\sim Ueq, Uanis(C8) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C11) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C12) = Uanis(C11)
Uanis(C14) = Uanis(C13) = Uanis(C12) = Uanis(C11) = Uanis(C10)
4.a Ternary CH refined with riding coordinates:
 C3(H3)
4.b Secondary CH2 refined with riding coordinates:
 C14(H14A,H14B), C2(H2A,H2B), C13(H13A,H13B), C12(H12A,H12B), C11(H11A,H11B)
4.c Aromatic/amide H refined with riding coordinates:
 C8(H8), C9(H9), C5(H5), C6(H6), C7(H7)
4.d Fitted hexagon refined as free rotating group:
 C8(C9,C4,C5,C6,C7)
4.e Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C), N2(H2C,H2D,H2E), C1(H1D,H1E,H1F), C10(H10A,H10B,H10C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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 0.74091(6) 0.47652(6) 0.75253(2) 0.03858(19) Uani 1 1 d . . . . .
Br3 Br 0.4349(2) 0.2914(2) 0.76826(6) 0.0593(5) Uani 1 1 d . . . . .
Br2 Br 0.7699(2) 0.5388(2) 0.83919(5) 0.0641(5) Uani 1 1 d . . . . .
Br1 Br 0.7025(3) 0.4041(2) 0.67061(6) 0.0691(6) Uani 1 1 d . . . . .
Br4 Br 0.9491(2) 0.1851(2) 0.75873(6) 0.0651(6) Uani 1 1 d . . . . .
N1 N 0.8059(17) 0.0260(17) 0.6691(4) 0.056(4) Uani 1 1 d . . . . .
H1A H 0.915829 0.029315 0.665451 0.067 Uiso 1 1 calc R U . . .
H1B H 0.783026 -0.034396 0.689504 0.067 Uiso 1 1 calc R U . . .
H1C H 0.767788 0.123935 0.673097 0.067 Uiso 1 1 calc R U . . .
C8 C 0.605(2) 0.2360(19) 0.5523(5) 0.112(9) Uani 1 1 d G U . . .
H8 H 0.508988 0.278048 0.541458 0.135 Uiso 1 1 calc R U . . .
C9 C 0.5947(14) 0.1354(19) 0.5841(5) 0.087(8) Uani 1 1 d G . . . .
H9 H 0.491000 0.110150 0.594519 0.104 Uiso 1 1 calc R U . . .
C4 C 0.7389(18) 0.0725(14) 0.6004(3) 0.060(5) Uani 1 1 d G . . . .
C5 C 0.8938(14) 0.110(2) 0.5849(4) 0.088(8) Uani 1 1 d G . . . .
H5 H 0.990317 0.068113 0.595737 0.105 Uiso 1 1 calc R U . . .
C6 C 0.9046(19) 0.211(2) 0.5531(5) 0.116(10) Uani 1 1 d G . . . .
H6 H 1.008308 0.236010 0.542676 0.140 Uiso 1 1 calc R U . . .
C7 C 0.760(3) 0.2737(16) 0.5368(4) 0.118(9) Uani 1 1 d G U . . .
H7 H 0.767646 0.340978 0.515536 0.141 Uiso 1 1 calc R U . . .
N2 N 0.725(2) 0.934(2) 0.8183(4) 0.082(5) Uani 1 1 d D . . . .
H2C H 0.743850 0.980338 0.795522 0.098 Uiso 1 1 calc R U . . .
H2D H 0.616463 0.917790 0.821272 0.098 Uiso 1 1 calc R U . . .
H2E H 0.779156 0.841996 0.819315 0.098 Uiso 1 1 calc R U . . .
C3 C 0.722(2) -0.0439(17) 0.6332(5) 0.054(4) Uani 1 1 d D . . . .
H3 H 0.603375 -0.058403 0.638822 0.065 Uiso 1 1 calc R U . . .
C14 C 0.787(4) 1.040(3) 0.8499(7) 0.173(7) Uani 1 1 d D . . . .
H14A H 0.743369 1.146555 0.845728 0.208 Uiso 1 1 calc R U . . .
H14B H 0.907546 1.046316 0.848473 0.208 Uiso 1 1 calc R U . . .
C2 C 0.798(2) -0.2038(18) 0.6259(5) 0.073(6) Uani 1 1 d D . . . .
H2A H 0.788230 -0.267459 0.649187 0.087 Uiso 1 1 calc R U . . .
H2B H 0.915865 -0.190395 0.620462 0.087 Uiso 1 1 calc R U . . .
C1 C 0.719(4) -0.292(3) 0.5930(6) 0.112(9) Uani 1 1 d D . . . .
H1D H 0.766735 -0.256691 0.569032 0.169 Uiso 1 1 calc R U . . .
H1E H 0.601041 -0.271770 0.592838 0.169 Uiso 1 1 calc R U . . .
H1F H 0.738293 -0.403803 0.596054 0.169 Uiso 1 1 calc R U . . .
C13 C 0.738(4) 0.987(4) 0.8896(8) 0.173(7) Uani 1 1 d D . . . .
H13A H 0.790328 0.885602 0.895547 0.208 Uiso 1 1 calc R U . . .
H13B H 0.618385 0.974692 0.891399 0.208 Uiso 1 1 calc R U . . .
C12 C 0.798(5) 1.113(4) 0.9171(9) 0.173(7) Uani 1 1 d D . . . .
H12A H 0.918871 1.109716 0.918026 0.208 Uiso 1 1 calc R U . . .
H12B H 0.765431 1.215781 0.907128 0.208 Uiso 1 1 calc R U . . .
C10 C 0.802(5) 1.239(4) 0.9776(11) 0.173(7) Uani 1 1 d D . . . .
H10A H 0.850143 1.309822 0.958876 0.260 Uiso 1 1 calc R U . . .
H10B H 0.885634 1.206516 0.995701 0.260 Uiso 1 1 calc R U . . .
H10C H 0.713670 1.293193 0.991102 0.260 Uiso 1 1 calc R U . . .
C11 C 0.732(5) 1.096(4) 0.9573(9) 0.173(7) Uani 1 1 d D U . . .
H11A H 0.771114 0.998202 0.969228 0.208 Uiso 1 1 calc R U . . .
H11B H 0.610918 1.096574 0.957541 0.208 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 Br3 2.9564(17) . ?
Pb1 Br3 3.0861(17) 3_656 ?
Pb1 Br2 3.0502(19) . ?
Pb1 Br1 2.913(2) . ?
Pb1 Br4 3.0677(16) 3_756 ?
Pb1 Br4 2.9738(16) . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 H1C 0.8900 . ?
N1 C3 1.53(2) . ?
C8 H8 0.9300 . ?
C8 C9 1.3900 . ?
C8 C7 1.3900 . ?
C9 H9 0.9300 . ?
C9 C4 1.3900 . ?
C4 C5 1.3900 . ?
C4 C3 1.506(19) . ?
C5 H5 0.9300 . ?
C5 C6 1.3900 . ?
C6 H6 0.9300 . ?
C6 C7 1.3900 . ?
C7 H7 0.9300 . ?
N2 H2C 0.8900 . ?
N2 H2D 0.8900 . ?
N2 H2E 0.8900 . ?
N2 C14 1.494(13) . ?
C3 H3 0.9800 . ?
C3 C2 1.498(12) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C14 C13 1.495(9) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C2 C1 1.498(12) . ?
C1 H1D 0.9600 . ?
C1 H1E 0.9600 . ?
C1 H1F 0.9600 . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C13 C12 1.501(13) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C12 C11 1.494(9) . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C10 C11 1.505(9) . ?
C11 H11A 0.9700 . ?
C11 H11B 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
Br3 Pb1 Br3 96.69(2) . 3_656 ?
Br3 Pb1 Br2 88.46(5) . . ?
Br3 Pb1 Br4 91.01(6) . . ?
Br3 Pb1 Br4 175.69(6) . 3_756 ?
Br2 Pb1 Br3 96.65(5) . 3_656 ?
Br2 Pb1 Br4 87.98(6) . 3_756 ?
Br1 Pb1 Br3 88.91(6) . . ?
Br1 Pb1 Br3 84.54(6) . 3_656 ?
Br1 Pb1 Br2 177.22(6) . . ?
Br1 Pb1 Br4 87.53(6) . . ?
Br1 Pb1 Br4 94.69(6) . 3_756 ?
Br4 Pb1 Br3 81.32(6) 3_756 3_656 ?
Br4 Pb1 Br3 168.83(6) . 3_656 ?
Br4 Pb1 Br2 91.62(6) . . ?
Br4 Pb1 Br4 91.525(18) . 3_756 ?
Pb1 Br3 Pb1 142.06(7) . 3_646 ?
Pb1 Br4 Pb1 156.54(8) . 3_746 ?
H1A N1 H1B 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1B N1 H1C 109.5 . . ?
C3 N1 H1A 109.5 . . ?
C3 N1 H1B 109.5 . . ?
C3 N1 H1C 109.5 . . ?
C9 C8 H8 120.0 . . ?
C9 C8 C7 120.0 . . ?
C7 C8 H8 120.0 . . ?
C8 C9 H9 120.0 . . ?
C8 C9 C4 120.0 . . ?
C4 C9 H9 120.0 . . ?
C9 C4 C3 118.6(12) . . ?
C5 C4 C9 120.0 . . ?
C5 C4 C3 121.3(12) . . ?
C4 C5 H5 120.0 . . ?
C6 C5 C4 120.0 . . ?
C6 C5 H5 120.0 . . ?
C5 C6 H6 120.0 . . ?
C5 C6 C7 120.0 . . ?
C7 C6 H6 120.0 . . ?
C8 C7 H7 120.0 . . ?
C6 C7 C8 120.0 . . ?
C6 C7 H7 120.0 . . ?
H2C N2 H2D 109.5 . . ?
H2C N2 H2E 109.5 . . ?
H2D N2 H2E 109.5 . . ?
C14 N2 H2C 109.5 . . ?
C14 N2 H2D 109.5 . . ?
C14 N2 H2E 109.5 . . ?
N1 C3 H3 108.4 . . ?
C4 C3 N1 108.8(12) . . ?
C4 C3 H3 108.4 . . ?
C2 C3 N1 107.8(13) . . ?
C2 C3 C4 114.9(14) . . ?
C2 C3 H3 108.4 . . ?
N2 C14 H14A 108.8 . . ?
N2 C14 H14B 108.8 . . ?
N2 C14 C13 114(2) . . ?
H14A C14 H14B 107.7 . . ?
C13 C14 H14A 108.8 . . ?
C13 C14 H14B 108.8 . . ?
C3 C2 H2A 108.8 . . ?
C3 C2 H2B 108.8 . . ?
C3 C2 C1 113.7(16) . . ?
H2A C2 H2B 107.7 . . ?
C1 C2 H2A 108.8 . . ?
C1 C2 H2B 108.8 . . ?
C2 C1 H1D 109.5 . . ?
C2 C1 H1E 109.5 . . ?
C2 C1 H1F 109.5 . . ?
H1D C1 H1E 109.5 . . ?
H1D C1 H1F 109.5 . . ?
H1E C1 H1F 109.5 . . ?
C14 C13 H13A 110.4 . . ?
C14 C13 H13B 110.4 . . ?
C14 C13 C12 107(2) . . ?
H13A C13 H13B 108.6 . . ?
C12 C13 H13A 110.4 . . ?
C12 C13 H13B 110.4 . . ?
C13 C12 H12A 108.7 . . ?
C13 C12 H12B 108.7 . . ?
H12A C12 H12B 107.6 . . ?
C11 C12 C13 114(3) . . ?
C11 C12 H12A 108.7 . . ?
C11 C12 H12B 108.7 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C11 C10 H10A 109.5 . . ?
C11 C10 H10B 109.5 . . ?
C11 C10 H10C 109.5 . . ?
C12 C11 C10 103(3) . . ?
C12 C11 H11A 111.2 . . ?
C12 C11 H11B 111.2 . . ?
C10 C11 H11A 111.2 . . ?
C10 C11 H11B 111.2 . . ?
H11A C11 H11B 109.1 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 C3 C2 C1 175.9(17) . . . . ?
C8 C9 C4 C5 0.0 . . . . ?
C8 C9 C4 C3 -176.3(13) . . . . ?
C9 C8 C7 C6 0.0 . . . . ?
C9 C4 C5 C6 0.0 . . . . ?
C9 C4 C3 N1 -118.2(13) . . . . ?
C9 C4 C3 C2 120.9(15) . . . . ?
C4 C5 C6 C7 0.0 . . . . ?
C4 C3 C2 C1 -63(2) . . . . ?
C5 C4 C3 N1 65.6(15) . . . . ?
C5 C4 C3 C2 -55.4(18) . . . . ?
C5 C6 C7 C8 0.0 . . . . ?
C7 C8 C9 C4 0.0 . . . . ?
N2 C14 C13 C12 -176(3) . . . . ?
C3 C4 C5 C6 176.2(13) . . . . ?
C14 C13 C12 C11 169(3) . . . . ?
C13 C12 C11 C10 -177(3) . . . . ?


_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;

# start Validation Reply Form
_vrf_PLAT342_220728e14_r_auto    
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.03615 Ang.         51 Note   
RESPONSE: This is likely related to the weak diffraction of the crystal.
;
# 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_220728e4_ss_auto
_database_code_depnum_ccdc_archive 'CCDC 2252915'
loop_
_audit_author_name
_audit_author_address
'Shihai You'
;Fujian Institute of Research on the Structure of Matter, Chinese Academy of Sciences
China
;
_audit_update_record             
;
2023-03-30 deposited with the CCDC.	2023-09-12 downloaded from the CCDC.
;
_audit_creation_date             2023-03-25
_audit_creation_method           
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Br4 Pb, C9 H14 N, C5 H14 N'
_chemical_formula_sum            'C14 H28 Br4 N2 Pb'
_chemical_formula_weight         751.21
_chemical_absolute_configuration ad
_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'
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                   8.0152(3)
_cell_length_b                   8.4073(3)
_cell_length_c                   34.5750(15)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2329.88(16)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    6767
_cell_measurement_temperature    300.40(10)
_cell_measurement_theta_max      29.3490
_cell_measurement_theta_min      2.3420
_shelx_estimated_absorpt_T_max   0.766
_shelx_estimated_absorpt_T_min   0.165
_exptl_absorpt_coefficient_mu    14.098
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.10071
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.73a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.142
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1392
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.02
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0512
_diffrn_reflns_av_unetI/netI     0.0456
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            12417
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         2.356
_diffrn_ambient_temperature      300.15
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -36.00  35.00   0.50    1.47    --    6.70 -86.00  84.00  142
  2  ω    -18.00  12.00   0.50    1.47    --   -5.06 -99.00  30.00   60
  3  ω    -13.00  28.00   0.50    1.47    --   -5.06 -99.00 -60.00   82
  4  ω      0.00  28.00   0.50    1.47    --   -5.06 -99.00 -90.00   56
  5  ω    -15.00  11.00   0.50    1.47    --    6.70  86.00-157.00   52
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.692
_reflns_Friedel_fraction_full    0.961
_reflns_Friedel_fraction_max     0.961
_reflns_number_gt                3398
_reflns_number_total             4026
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.73a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.73a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.73a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         1.360
_refine_diff_density_min         -1.250
_refine_diff_density_rms         0.247
_refine_ls_abs_structure_details 
;
 Flack x determined using 1153 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.001(12)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.107
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     182
_refine_ls_number_reflns         4026
_refine_ls_number_restraints     28
_refine_ls_R_factor_all          0.0597
_refine_ls_R_factor_gt           0.0460
_refine_ls_restrained_S_all      1.105
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0568P)²+8.7364P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1110
_refine_ls_wR_factor_ref         0.1172
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C8-C7 = C7-C6
 1.5 with sigma of 0.01
 N1-C8
 1.5 with sigma of 0.01
 C5-C4 = C4-C3 = C3-C2 = C2-C1
 1.5 with sigma of 0.01
 C3-C1
 2.4 with sigma of 0.02
 C5-C3
 2.4 with sigma of 0.02
 C4-C2
 2.4 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C12) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C2) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C3) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4.a Ternary CH refined with riding coordinates:
 C8(H8)
4.b Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C5(H5A,H5B), C4(H4A,H4B), C3(H3A,H3B), C2(H2D,H2E)
4.c Aromatic/amide H refined with riding coordinates:
 C14(H14), C10(H10), C11(H11), C12(H12), C13(H13)
4.d Fitted hexagon refined as free rotating group:
 C14(C9,C10,C11,C12,C13)
4.e Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C), N2(H2A,H2B,H2C), C6(H6A,H6B,H6C), C1(H1D,H1E,H1F)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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 0.25856(7) 0.47973(6) 0.75247(2) 0.0396(2) Uani 1 1 d . . . . .
Br3 Br 0.5651(3) 0.2943(2) 0.76794(6) 0.0609(6) Uani 1 1 d . . . . .
Br1 Br 0.2301(3) 0.5420(3) 0.83909(6) 0.0653(5) Uani 1 1 d . . . . .
Br2 Br 0.0517(2) 0.1871(2) 0.75907(7) 0.0663(6) Uani 1 1 d . . . . .
Br4 Br 0.2952(3) 0.4078(3) 0.67043(6) 0.0731(7) Uani 1 1 d . . . . .
N1 N 0.194(2) 0.0285(19) 0.6687(4) 0.067(5) Uani 1 1 d D . . . .
H1A H 0.083657 0.022084 0.665691 0.080 Uiso 1 1 calc R U . . .
H1B H 0.223133 0.129928 0.671506 0.080 Uiso 1 1 calc R U . . .
H1C H 0.223838 -0.026000 0.689653 0.080 Uiso 1 1 calc R U . . .
N2 N 0.274(3) 0.936(2) 0.8195(5) 0.097(7) Uani 1 1 d . . . . .
H2A H 0.264308 0.986683 0.797050 0.117 Uiso 1 1 calc R U . . .
H2B H 0.212560 0.847414 0.818873 0.117 Uiso 1 1 calc R U . . .
H2C H 0.380480 0.909952 0.823386 0.117 Uiso 1 1 calc R U . . .
C8 C 0.278(2) -0.039(2) 0.6340(5) 0.062(5) Uani 1 1 d D . . . .
H8 H 0.396848 -0.054784 0.639983 0.074 Uiso 1 1 calc R U . . .
C7 C 0.201(3) -0.199(2) 0.6257(6) 0.074(7) Uani 1 1 d D . . . .
H7A H 0.083892 -0.183114 0.619620 0.089 Uiso 1 1 calc R U . . .
H7B H 0.206729 -0.263302 0.648946 0.089 Uiso 1 1 calc R U . . .
C14 C 0.1074(18) 0.112(2) 0.5854(5) 0.088(9) Uani 1 1 d G . . . .
H14 H 0.011477 0.070217 0.596534 0.106 Uiso 1 1 calc R U . . .
C9 C 0.263(2) 0.0739(16) 0.6003(3) 0.059(5) Uani 1 1 d G . . . .
C10 C 0.4065(18) 0.137(2) 0.5837(5) 0.098(10) Uani 1 1 d G . . . .
H10 H 0.510814 0.111251 0.593673 0.118 Uiso 1 1 calc R U . . .
C11 C 0.394(3) 0.239(2) 0.5521(6) 0.142(15) Uani 1 1 d G . . . .
H11 H 0.489873 0.280715 0.540940 0.170 Uiso 1 1 calc R U . . .
C12 C 0.238(4) 0.2770(18) 0.5371(4) 0.128(11) Uani 1 1 d G U . . .
H12 H 0.229734 0.344931 0.516002 0.153 Uiso 1 1 calc R U . . .
C13 C 0.095(3) 0.214(3) 0.5538(5) 0.127(13) Uani 1 1 d G . . . .
H13 H -0.009466 0.239684 0.543799 0.152 Uiso 1 1 calc R U . . .
C5 C 0.217(4) 1.038(4) 0.8507(7) 0.129(12) Uani 1 1 d D . . . .
H5A H 0.095701 1.040714 0.849830 0.155 Uiso 1 1 calc R U . . .
H5B H 0.256269 1.144615 0.845614 0.155 Uiso 1 1 calc R U . . .
C4 C 0.268(4) 0.993(3) 0.8906(7) 0.141(13) Uani 1 1 d D . . . .
H4A H 0.388374 0.990902 0.892736 0.170 Uiso 1 1 calc R U . . .
H4B H 0.224416 0.889098 0.897323 0.170 Uiso 1 1 calc R U . . .
C3 C 0.196(5) 1.118(5) 0.9167(8) 0.180(18) Uani 1 1 d D U . . .
H3A H 0.221164 1.222950 0.906495 0.216 Uiso 1 1 calc R U . . .
H3B H 0.075613 1.106795 0.917865 0.216 Uiso 1 1 calc R U . . .
C6 C 0.282(5) -0.288(3) 0.5931(8) 0.141(14) Uani 1 1 d D . . . .
H6A H 0.237252 -0.251307 0.568890 0.211 Uiso 1 1 calc R U . . .
H6B H 0.260383 -0.399511 0.595879 0.211 Uiso 1 1 calc R U . . .
H6C H 0.400216 -0.269483 0.593570 0.211 Uiso 1 1 calc R U . . .
C1 C 0.204(7) 1.242(7) 0.9790(12) 0.30(4) Uani 1 1 d D . . . .
H1D H 0.181617 1.328739 0.961886 0.448 Uiso 1 1 calc R U . . .
H1E H 0.287070 1.272839 0.997572 0.448 Uiso 1 1 calc R U . . .
H1F H 0.103587 1.212046 0.992275 0.448 Uiso 1 1 calc R U . . .
C2 C 0.267(7) 1.102(6) 0.9561(9) 0.28(3) Uani 1 1 d D U . . .
H2D H 0.388352 1.103064 0.954960 0.332 Uiso 1 1 calc R U . . .
H2E H 0.231711 1.002841 0.967802 0.332 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 Br3 2.9587(19) . ?
Pb1 Br3 3.0804(19) 3_656 ?
Pb1 Br1 3.049(2) . ?
Pb1 Br2 3.0633(18) 3_556 ?
Pb1 Br2 2.9753(18) . ?
Pb1 Br4 2.915(2) . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 H1C 0.8900 . ?
N1 C8 1.491(12) . ?
N2 H2A 0.8900 . ?
N2 H2B 0.8900 . ?
N2 H2C 0.8900 . ?
N2 C5 1.45(3) . ?
C8 H8 0.9800 . ?
C8 C7 1.504(12) . ?
C8 C9 1.51(2) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C7 C6 1.504(13) . ?
C14 H14 0.9300 . ?
C14 C9 1.3900 . ?
C14 C13 1.3900 . ?
C9 C10 1.3900 . ?
C10 H10 0.9300 . ?
C10 C11 1.3900 . ?
C11 H11 0.9300 . ?
C11 C12 1.3900 . ?
C12 H12 0.9300 . ?
C12 C13 1.3900 . ?
C13 H13 0.9300 . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C5 C4 1.487(13) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C4 C3 1.500(13) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C3 C2 1.483(13) . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
C1 H1D 0.9600 . ?
C1 H1E 0.9600 . ?
C1 H1F 0.9600 . ?
C1 C2 1.505(13) . ?
C2 H2D 0.9700 . ?
C2 H2E 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
Br3 Pb1 Br3 96.48(3) . 3_656 ?
Br3 Pb1 Br1 88.57(6) . . ?
Br3 Pb1 Br2 90.76(6) . . ?
Br3 Pb1 Br2 176.08(6) . 3_556 ?
Br1 Pb1 Br3 96.43(6) . 3_656 ?
Br1 Pb1 Br2 88.25(6) . 3_556 ?
Br2 Pb1 Br3 81.60(6) 3_556 3_656 ?
Br2 Pb1 Br3 169.43(6) . 3_656 ?
Br2 Pb1 Br1 91.43(6) . . ?
Br2 Pb1 Br2 91.62(2) . 3_556 ?
Br4 Pb1 Br3 89.02(7) . . ?
Br4 Pb1 Br3 84.78(6) . 3_656 ?
Br4 Pb1 Br1 177.42(7) . . ?
Br4 Pb1 Br2 94.19(7) . 3_556 ?
Br4 Pb1 Br2 87.67(7) . . ?
Pb1 Br3 Pb1 142.37(8) . 3_646 ?
Pb1 Br2 Pb1 155.93(8) . 3_546 ?
H1A N1 H1B 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1B N1 H1C 109.5 . . ?
C8 N1 H1A 109.5 . . ?
C8 N1 H1B 109.5 . . ?
C8 N1 H1C 109.5 . . ?
H2A N2 H2B 109.5 . . ?
H2A N2 H2C 109.5 . . ?
H2B N2 H2C 109.5 . . ?
C5 N2 H2A 109.5 . . ?
C5 N2 H2B 109.5 . . ?
C5 N2 H2C 109.5 . . ?
N1 C8 H8 108.8 . . ?
N1 C8 C7 107.8(15) . . ?
N1 C8 C9 110.0(14) . . ?
C7 C8 H8 108.8 . . ?
C7 C8 C9 112.4(15) . . ?
C9 C8 H8 108.8 . . ?
C8 C7 H7A 108.7 . . ?
C8 C7 H7B 108.7 . . ?
C8 C7 C6 114.1(19) . . ?
H7A C7 H7B 107.6 . . ?
C6 C7 H7A 108.7 . . ?
C6 C7 H7B 108.7 . . ?
C9 C14 H14 120.0 . . ?
C9 C14 C13 120.0 . . ?
C13 C14 H14 120.0 . . ?
C14 C9 C8 120.4(14) . . ?
C10 C9 C8 119.6(14) . . ?
C10 C9 C14 120.0 . . ?
C9 C10 H10 120.0 . . ?
C9 C10 C11 120.0 . . ?
C11 C10 H10 120.0 . . ?
C10 C11 H11 120.0 . . ?
C10 C11 C12 120.0 . . ?
C12 C11 H11 120.0 . . ?
C11 C12 H12 120.0 . . ?
C11 C12 C13 120.0 . . ?
C13 C12 H12 120.0 . . ?
C14 C13 H13 120.0 . . ?
C12 C13 C14 120.0 . . ?
C12 C13 H13 120.0 . . ?
N2 C5 H5A 108.1 . . ?
N2 C5 H5B 108.1 . . ?
N2 C5 C4 117(2) . . ?
H5A C5 H5B 107.3 . . ?
C4 C5 H5A 108.1 . . ?
C4 C5 H5B 108.1 . . ?
C5 C4 H4A 110.5 . . ?
C5 C4 H4B 110.5 . . ?
C5 C4 C3 106.1(16) . . ?
H4A C4 H4B 108.7 . . ?
C3 C4 H4A 110.5 . . ?
C3 C4 H4B 110.5 . . ?
C4 C3 H3A 109.7 . . ?
C4 C3 H3B 109.7 . . ?
H3A C3 H3B 108.2 . . ?
C2 C3 C4 109.8(18) . . ?
C2 C3 H3A 109.7 . . ?
C2 C3 H3B 109.7 . . ?
C7 C6 H6A 109.5 . . ?
C7 C6 H6B 109.5 . . ?
C7 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
H1D C1 H1E 109.5 . . ?
H1D C1 H1F 109.5 . . ?
H1E C1 H1F 109.5 . . ?
C2 C1 H1D 109.5 . . ?
C2 C1 H1E 109.5 . . ?
C2 C1 H1F 109.5 . . ?
C3 C2 C1 106.4(18) . . ?
C3 C2 H2D 110.5 . . ?
C3 C2 H2E 110.5 . . ?
C1 C2 H2D 110.5 . . ?
C1 C2 H2E 110.5 . . ?
H2D C2 H2E 108.6 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 C8 C7 C6 -176(2) . . . . ?
N1 C8 C9 C14 -62.6(17) . . . . ?
N1 C8 C9 C10 118.8(15) . . . . ?
N2 C5 C4 C3 179(3) . . . . ?
C8 C9 C10 C11 178.5(13) . . . . ?
C7 C8 C9 C14 57.5(19) . . . . ?
C7 C8 C9 C10 -121.0(17) . . . . ?
C14 C9 C10 C11 0.0 . . . . ?
C9 C8 C7 C6 63(3) . . . . ?
C9 C14 C13 C12 0.0 . . . . ?
C9 C10 C11 C12 0.0 . . . . ?
C10 C11 C12 C13 0.0 . . . . ?
C11 C12 C13 C14 0.0 . . . . ?
C13 C14 C9 C8 -178.5(14) . . . . ?
C13 C14 C9 C10 0.0 . . . . ?
C5 C4 C3 C2 -169(5) . . . . ?
C4 C3 C2 C1 174(5) . . . . ?


_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;


# start Validation Reply Form
_vrf_PLAT342_220728e4_ss_auto    
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.03615 Ang.         51 Note   
RESPONSE: This is likely related to the weak diffraction of the crystal.
;
# end Validation Reply Form
