# Supplementary Information (SI) for Chemical Science.
# This journal is © The Royal Society of Chemistry 2026

####################################################################### 
# 
# 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_3D_auto
_database_code_depnum_ccdc_archive 'CCDC 2312099'
loop_
_audit_author_name
_audit_author_address
'Hongliang Dai'
;Jiangxi Normal University
China
;
_audit_update_record             
;
2023-12-05 deposited with the CCDC.	2026-04-16 downloaded from the CCDC.
;
_audit_creation_date             2023-12-05
_audit_creation_method           
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_chemical_name_systematic        ?
_chemical_formula_moiety         'Br6 Pb2, C6 H9 N3'
_chemical_formula_sum            'C6 H9 Br6 N3 Pb2'
_chemical_formula_weight         1008.068
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
_atom_type_scat_dispersion_source
Br -0.28346 2.55990 17.17890 5.23580 5.63770 3.98510 2.17230 16.57960 0.26090
41.43280 2.95570 'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
C 0.00347 0.00161 2.31000 1.02000 1.58860 0.86500 20.84390 10.20750 0.56870
51.65120 0.21560 'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
H 0.00000 0.00000 0.49300 0.32291 0.14019 0.04081 10.51090 26.12570 3.14236
57.79970 0.00304 'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
N 0.00653 0.00323 12.21260 3.13220 2.01250 1.16630 0.00570 9.89330 28.99750
0.58260 -11.52900 'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
Pb -3.20855 10.15389 31.06170 13.06370 18.44200 5.96960 0.69020 2.35760 8.61800
47.25790 13.41180 'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           52
_space_group_name_H-M_alt        'P n n a'
_space_group_name_Hall           '-P 2a 2bc'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 x,y,z
2 x,-y+1/2,-z+1/2
3 -x+1/2,y+1/2,-z+1/2
4 -x+1/2,-y,z
5 -x,-y,-z
6 -x,y-1/2,z-1/2
7 x-1/2,-y-1/2,z-1/2
8 x-1/2,y,-z

_symmetry_Int_Tables_number      52
_cell_length_a                   23.9011(15)
_cell_length_b                   15.7772(10)
_cell_length_c                   9.6867(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3652.8(4)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    5812
_cell_measurement_temperature    295.00(10)
_cell_measurement_theta_max      28.5620
_cell_measurement_theta_min      3.6400
_exptl_absorpt_coefficient_mu    31.525
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.26843
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.116a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    3.666
_exptl_crystal_description       block
_exptl_crystal_F_000             3399.330
_exptl_crystal_preparation       ?
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_diffrn_reflns_av_R_equivalents  0.0459
_diffrn_reflns_av_unetI/netI     0.0391
_diffrn_reflns_Laue_measured_fraction_full 0.9961
_diffrn_reflns_Laue_measured_fraction_max 0.8442
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            17692
_diffrn_reflns_point_group_measured_fraction_full 0.9961
_diffrn_reflns_point_group_measured_fraction_max 0.8442
_diffrn_reflns_theta_full        25.2417
_diffrn_reflns_theta_max         28.84
_diffrn_reflns_theta_min         3.41
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      295.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.5594
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.9961
_diffrn_measured_fraction_theta_max 0.8442
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     -8.00  17.00   1.00   29.15    --   -7.31-113.00 163.00   25
  2  ω      3.00  48.00   1.00   29.15    --   -7.31  22.00 163.00   45
  3  ω     -9.00  72.00   1.00   29.15    --    6.30  38.00-120.00   81
  4  ω    -14.00  11.00   1.00   29.15    --   -7.31 -99.00-120.00   25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0256988000
_diffrn_orient_matrix_UB_12      -0.0222016000
_diffrn_orient_matrix_UB_13      0.0052097000
_diffrn_orient_matrix_UB_21      -0.0136638000
_diffrn_orient_matrix_UB_22      0.0381251000
_diffrn_orient_matrix_UB_23      0.0191160000
_diffrn_orient_matrix_UB_31      -0.0055850000
_diffrn_orient_matrix_UB_32      0.0087219000
_diffrn_orient_matrix_UB_33      -0.0705084000
_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              'SuperNova (Mo) X-ray Source'
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              31
_reflns_limit_h_min              0
_reflns_limit_k_max              19
_reflns_limit_k_min              0
_reflns_limit_l_max              12
_reflns_limit_l_min              0
_reflns_number_gt                2931
_reflns_number_total             4042
_reflns_threshold_expression     I>=2u(I)
_computing_cell_refinement       'CrysAlisPro 1.171.41.116a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.116a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.116a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.5 (Bourhis et al., 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_refine_diff_density_max         1.8409
_refine_diff_density_min         -2.3889
_refine_diff_density_rms         0.4988
_refine_ls_d_res_high            0.7368
_refine_ls_d_res_low             5.9753
_refine_ls_goodness_of_fit_ref   1.0612
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    16
_refine_ls_number_parameters     157
_refine_ls_number_reflns         4042
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0615
_refine_ls_R_factor_gt           0.0352
_refine_ls_restrained_S_all      1.0612
_refine_ls_shift/su_max          0.0004
_refine_ls_shift/su_mean         0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0352P)²+3.3767P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0731
_refine_ls_wR_factor_ref         0.0867
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups, All N(H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C5(H5), N1(H1), C1(H1a), C4(H4)
2.b X=CH2 refined with riding coordinates:
 N3(H3a,H3b), N2(H2a,H2b)
;
_atom_sites_solution_primary     direct
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_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Pb1 Pb 0.257233(13) 0.191826(19) 0.04628(3) 0.02386(11) Uani 1.000000 1 . . .
Pb2 Pb 0.006245(13) 0.184474(19) 0.04727(3) 0.02328(11) Uani 1.000000 1 . . .
Br4 Br 0.13325(4) 0.18058(6) 0.03669(10) 0.0352(2) Uani 1.000000 1 . . .
Br6 Br 0.0 0.0 0.0 0.1077(9) Uani 1.000000 2 S T P
Br5 Br -0.00099(4) 0.13738(5) 0.34841(9) 0.0339(2) Uani 1.000000 1 . . .
Br1 Br 0.25269(4) 0.36559(5) 0.15551(9) 0.0326(2) Uani 1.000000 1 . . .
Br2 Br 0.25 0.0 -0.01060(13) 0.0347(3) Uani 1.000000 2 S T P
Br7 Br 0.01901(5) 0.25 -0.25 0.0354(3) Uani 1.000000 2 S T P
Br8 Br -0.11615(4) 0.18528(7) -0.01926(10) 0.0421(3) Uani 1.000000 1 . . .
Br3 Br 0.25482(7) 0.25 -0.25 0.0542(4) Uani 1.000000 2 S T P
N3 N 0.1334(3) 0.4967(5) 0.2533(8) 0.048(2) Uani 1.000000 1 . . .
H3a H 0.1254(3) 0.5139(5) 0.3352(8) 0.057(3) Uiso 1.000000 1 R . .
H3b H 0.1555(3) 0.4543(5) 0.2420(8) 0.057(3) Uiso 1.000000 1 R . .
C2 C 0.1371(4) 0.5622(6) -0.0988(9) 0.039(2) Uani 1.000000 1 . . .
H2 H 0.1383(4) 0.6201(6) -0.0808(9) 0.047(3) Uiso 1.000000 1 R . .
N2 N 0.0789(4) 0.5979(6) 0.1572(8) 0.059(3) Uani 1.000000 1 . . .
H2a H 0.0700(4) 0.6168(6) 0.2375(8) 0.070(3) Uiso 1.000000 1 R . .
H2b H 0.0655(4) 0.6216(6) 0.0843(8) 0.070(3) Uiso 1.000000 1 R . .
C5 C 0.1360(4) 0.3908(7) -0.1554(10) 0.045(3) Uani 1.000000 1 . . .
H5 H 0.1361(4) 0.3333(7) -0.1771(10) 0.054(3) Uiso 1.000000 1 R . .
N1 N 0.1459(4) 0.4489(6) -0.2530(8) 0.058(3) Uani 1.000000 1 . . .
H1 H 0.1521(4) 0.4320(6) -0.3360(8) 0.069(3) Uiso 1.000000 1 R . .
C1 C 0.1466(5) 0.5309(8) -0.2271(11) 0.057(3) Uani 1.000000 1 . . .
H1a H 0.1539(5) 0.5684(8) -0.2990(11) 0.068(4) Uiso 1.000000 1 R . .
C4 C 0.1257(4) 0.4170(6) -0.0237(10) 0.035(2) Uani 1.000000 1 . . .
H4 H 0.1190(4) 0.3776(6) 0.0458(10) 0.042(3) Uiso 1.000000 1 R . .
C3 C 0.1254(3) 0.5031(5) 0.0055(8) 0.0243(19) Uani 1.000000 1 . . .
C6 C 0.1118(4) 0.5349(6) 0.1461(8) 0.0265(18) Uani 1.000000 1 . . .


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 Br4 2.9701(9) . ?
Pb1 Br1 2.9406(9) . ?
Pb1 Br1 3.0294(9) 2 ?
Pb1 Br2 3.0811(4) . ?
Pb1 Br8 3.0394(10) 8_655 ?
Pb1 Br3 3.0137(3) . ?
Pb2 Br4 3.0379(9) . ?
Pb2 Br6 2.9501(3) . ?
Pb2 Br5 2.9918(9) 2 ?
Pb2 Br5 3.0151(9) . ?
Pb2 Br7 3.0747(3) . ?
Pb2 Br8 2.9955(10) . ?
N3 H3a 0.8600 . ?
N3 H3b 0.8600 . ?
N3 C6 1.307(11) . ?
C2 H2 0.9300 . ?
C2 C1 1.358(13) . ?
C2 C3 1.403(12) . ?
N2 H2a 0.8600 . ?
N2 H2b 0.8600 . ?
N2 C6 1.272(11) . ?
C5 H5 0.9300 . ?
C5 N1 1.338(13) . ?
C5 C4 1.363(13) . ?
N1 H1 0.8600 . ?
N1 C1 1.318(15) . ?
C1 H1a 0.9300 . ?
C4 H4 0.9300 . ?
C4 C3 1.388(11) . ?
C3 C6 1.487(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
Br1 Pb1 Br4 91.73(3) . . ?
Br1 Pb1 Br4 88.64(3) 2 . ?
Br2 Pb1 Br4 83.09(2) . . ?
Br2 Pb1 Br1 167.97(3) . . ?
Br2 Pb1 Br1 82.81(3) . 2 ?
Br8 Pb1 Br4 171.38(3) 8_655 . ?
Br8 Pb1 Br1 95.71(3) 8_655 . ?
Br8 Pb1 Br1 96.18(3) 8_655 2 ?
Br8 Pb1 Br2 90.41(2) 8_655 . ?
Br3 Pb1 Br4 88.24(4) . . ?
Br3 Pb1 Br1 93.326(18) . . ?
Br3 Pb1 Br1 176.83(4) . 2 ?
Br3 Pb1 Br2 97.34(2) . . ?
Br3 Pb1 Br8 86.99(4) . 8_655 ?
Br6 Pb2 Br4 91.45(2) . . ?
Br5 Pb2 Br4 95.06(3) 2 . ?
Br5 Pb2 Br4 94.87(3) . . ?
Br5 Pb2 Br6 167.52(2) 2 . ?
Br5 Pb2 Br6 84.501(18) . . ?
Br7 Pb2 Br4 82.88(3) . . ?
Br7 Pb2 Br6 101.033(8) . . ?
Br7 Pb2 Br5 90.355(18) . 2 ?
Br7 Pb2 Br5 174.05(2) . . ?
Br8 Pb2 Br4 165.61(3) . . ?
Br8 Pb2 Br6 85.49(2) . . ?
Br8 Pb2 Br5 90.70(3) . 2 ?
Br8 Pb2 Br5 98.81(3) . . ?
Br8 Pb2 Br7 83.91(3) . . ?
Pb2 Br4 Pb1 174.09(4) . . ?
Pb2 Br6 Pb2 180.0 5 . ?
Pb1 Br2 Pb1 159.40(5) 4 . ?
Pb2 Br7 Pb2 168.61(5) 2_554 . ?
Pb2 Br8 Pb1 172.33(4) . 8 ?
Pb1 Br3 Pb1 177.80(6) 2_554 . ?
H3b N3 H3a 120.0 . . ?
C6 N3 H3a 120.0 . . ?
C6 N3 H3b 120.0 . . ?
C1 C2 H2 121.6(6) . . ?
C3 C2 H2 121.6(6) . . ?
C3 C2 C1 116.7(9) . . ?
H2b N2 H2a 120.0 . . ?
C6 N2 H2a 120.0 . . ?
C6 N2 H2b 120.0 . . ?
N1 C5 H5 120.5(6) . . ?
C4 C5 H5 120.5(6) . . ?
C4 C5 N1 119.0(10) . . ?
H1 N1 C5 118.6(6) . . ?
C1 N1 C5 122.8(9) . . ?
C1 N1 H1 118.6(6) . . ?
N1 C1 C2 122.0(9) . . ?
H1a C1 C2 119.0(6) . . ?
H1a C1 N1 119.0(6) . . ?
H4 C4 C5 120.4(6) . . ?
C3 C4 C5 119.2(9) . . ?
C3 C4 H4 120.4(5) . . ?
C4 C3 C2 120.2(8) . . ?
C6 C3 C2 118.6(8) . . ?
C6 C3 C4 121.2(8) . . ?
N2 C6 N3 122.5(8) . . ?
C3 C6 N3 119.1(8) . . ?
C3 C6 N2 118.4(7) . . ?

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
N3 C6 C3 C2 -137.7(9) . . . . ?
N3 C6 C3 C4 43.3(10) . . . . ?
C2 C1 N1 C5 -0.2(14) . . . . ?
C2 C3 C4 C5 -1.8(10) . . . . ?
C2 C3 C6 N2 43.3(10) . . . . ?
N2 C6 C3 C4 -135.7(9) . . . . ?
C5 C4 C3 C6 177.2(8) . . . . ?


_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 2.317
_oxdiff_exptl_absorpt_empirical_full_min 0.572
####################################################################### 
# 
# 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_4d_auto
_database_code_depnum_ccdc_archive 'CCDC 2312100'
loop_
_audit_author_name
_audit_author_address
'Hongliang Dai'
;Jiangxi Normal University
China
;
_audit_update_record             
;
2023-12-05 deposited with the CCDC.	2026-04-16 downloaded from the CCDC.
;
_audit_creation_date             2023-12-05
_audit_creation_method           
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'I6 Pb2, C6 H9 N3'
_chemical_formula_sum            'C6 H8 I6 N3 Pb2'
_chemical_formula_weight         1297.93
_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'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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           52
_space_group_name_H-M_alt        'P n n a'
_space_group_name_Hall           '-P 2a 2bc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z'
'x, -y+1/2, -z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z'
'-x, y-1/2, z-1/2'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   25.5050(12)
_cell_length_b                   16.5271(9)
_cell_length_c                   10.0933(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4254.6(4)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    5675
_cell_measurement_temperature    295.00(10)
_cell_measurement_theta_max      28.5680
_cell_measurement_theta_min      3.9670
_shelx_estimated_absorpt_T_max   0.193
_shelx_estimated_absorpt_T_min   0.193
_exptl_absorpt_coefficient_mu    24.503
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.43424
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.116a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear dark red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    4.053
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             4376
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0408
_diffrn_reflns_av_unetI/netI     0.0366
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.853
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            17964
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.853
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.817
_diffrn_reflns_theta_min         3.285
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      295.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.5594
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.853
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     -7.00  18.00   1.00   21.02    --   -7.31  25.00 129.00   25
  2  ω    -51.00 -25.00   1.00   21.02    --    6.30 -19.00-150.00   26
  3  ω    -24.00  78.00   1.00   21.02    --    6.30  77.00 150.00  102
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0063095000
_diffrn_orient_matrix_UB_12      -0.0210147000
_diffrn_orient_matrix_UB_13      -0.0591757000
_diffrn_orient_matrix_UB_21      0.0066219000
_diffrn_orient_matrix_UB_22      -0.0348204000
_diffrn_orient_matrix_UB_23      0.0375566000
_diffrn_orient_matrix_UB_31      -0.0262481000
_diffrn_orient_matrix_UB_32      -0.0137333000
_diffrn_orient_matrix_UB_33      -0.0047860000
_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              'SuperNova (Mo) X-ray Source'
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3528
_reflns_number_total             4758
_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 1.171.41.116a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.116a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.116a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_refine_diff_density_max         2.629
_refine_diff_density_min         -2.429
_refine_diff_density_rms         0.400
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     157
_refine_ls_number_reflns         4758
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0640
_refine_ls_R_factor_gt           0.0419
_refine_ls_restrained_S_all      1.054
_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)+(0.0457P)²+22.5722P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0917
_refine_ls_wR_factor_ref         0.1038
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups, All N(H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C2(H2), C1(H1), N1(H1A), C5(H5)
2.b X=CH2 refined with riding coordinates:
 N3(H3A,H3B), N2(H2A,H2B)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_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
Pb2 Pb 0.24528(2) 0.19088(2) 0.95124(4) 0.02528(12) Uani 1 1 d . . . . .
Pb1 Pb 0.49615(2) 0.18672(2) 0.95128(4) 0.02512(12) Uani 1 1 d . . . . .
I4 I 0.37018(2) 0.18142(5) 0.95735(8) 0.0385(2) Uani 1 1 d . . . . .
I1 I 0.50191(2) 0.13116(4) 0.64729(7) 0.03281(17) Uani 1 1 d . . . . .
I5 I 0.24719(2) 0.12951(4) 0.64832(7) 0.03083(17) Uani 1 1 d . . . . .
I8 I 0.11983(2) 0.18630(5) 0.98303(8) 0.0440(2) Uani 1 1 d . . . . .
I7 I 0.250000 0.000000 1.02338(11) 0.0378(2) Uani 1 2 d S T P . .
I2 I 0.48230(4) 0.250000 1.250000 0.0403(3) Uani 1 2 d S T P . .
I6 I 0.25000(5) 0.250000 1.250000 0.0617(4) Uani 1 2 d S T P . .
I3 I 0.500000 0.000000 1.000000 0.1166(8) Uani 1 2 d S . P . .
C4 C 0.3748(3) 0.0783(7) 0.4799(11) 0.033(2) Uani 1 1 d . . . . .
H4 H 0.380146 0.115764 0.547380 0.040 Uiso 1 1 calc R U . . .
C3 C 0.3747(3) -0.0049(7) 0.5055(10) 0.030(3) Uani 1 1 d . . . . .
C6 C 0.3871(4) -0.0343(7) 0.6423(10) 0.037(2) Uani 1 1 d . . . . .
C2 C 0.3638(4) -0.0568(8) 0.4059(11) 0.043(3) Uani 1 1 d . . . . .
H2 H 0.362639 -0.112023 0.423174 0.051 Uiso 1 1 calc R U . . .
N3 N 0.3681(4) 0.0054(6) 0.7419(11) 0.051(3) Uani 1 1 d . . . . .
H3A H 0.375515 -0.009279 0.821505 0.061 Uiso 1 1 calc R U . . .
H3B H 0.348186 0.046581 0.728531 0.061 Uiso 1 1 calc R U . . .
N2 N 0.4167(4) -0.0953(7) 0.6549(10) 0.060(3) Uani 1 1 d . . . . .
H2A H 0.425110 -0.112271 0.732597 0.072 Uiso 1 1 calc R U . . .
H2B H 0.428333 -0.119853 0.585767 0.072 Uiso 1 1 calc R U . . .
C1 C 0.3548(6) -0.0303(10) 0.2827(13) 0.069(4) Uani 1 1 d . . . . .
H1 H 0.347072 -0.066406 0.214849 0.083 Uiso 1 1 calc R U . . .
N1 N 0.3571(4) 0.0489(9) 0.2595(11) 0.070(4) Uani 1 1 d . . . . .
H1A H 0.351913 0.065608 0.179856 0.084 Uiso 1 1 calc R U . . .
C5 C 0.3668(4) 0.1026(8) 0.3515(13) 0.043(3) Uani 1 1 d . . . . .
H5 H 0.368219 0.157257 0.329867 0.052 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
Pb2 I4 3.1898(6) . ?
Pb2 I5 3.2217(8) . ?
Pb2 I5 3.1343(8) 3_556 ?
Pb2 I8 3.2166(7) . ?
Pb2 I7 3.2399(5) . ?
Pb2 I6 3.1721(4) . ?
Pb1 I4 3.2148(6) . ?
Pb1 I1 3.1736(8) 3_556 ?
Pb1 I1 3.2061(8) . ?
Pb1 I8 3.2233(7) 6_657 ?
Pb1 I2 3.2108(4) . ?
Pb1 I3 3.1264(4) . ?
C4 H4 0.9300 . ?
C4 C3 1.399(14) . ?
C4 C5 1.372(15) . ?
C3 C6 1.498(14) . ?
C3 C2 1.351(15) . ?
C6 N3 1.295(14) . ?
C6 N2 1.266(14) . ?
C2 H2 0.9300 . ?
C2 C1 1.338(18) . ?
N3 H3A 0.8600 . ?
N3 H3B 0.8600 . ?
N2 H2A 0.8600 . ?
N2 H2B 0.8600 . ?
C1 H1 0.9300 . ?
C1 N1 1.33(2) . ?
N1 H1A 0.8600 . ?
N1 C5 1.308(18) . ?
C5 H5 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
I4 Pb2 I5 89.305(19) . . ?
I4 Pb2 I8 172.00(3) . . ?
I4 Pb2 I7 84.883(17) . . ?
I5 Pb2 I4 92.13(2) 3_556 . ?
I5 Pb2 I5 89.64(2) 3_556 . ?
I5 Pb2 I8 94.00(2) 3_556 . ?
I5 Pb2 I7 84.61(2) . . ?
I5 Pb2 I7 173.55(2) 3_556 . ?
I5 Pb2 I6 90.716(16) 3_556 . ?
I8 Pb2 I5 95.87(2) . . ?
I8 Pb2 I7 89.518(18) . . ?
I6 Pb2 I4 87.64(3) . . ?
I6 Pb2 I5 176.94(3) . . ?
I6 Pb2 I8 87.14(3) . . ?
I6 Pb2 I7 94.87(2) . . ?
I4 Pb1 I8 166.93(2) . 6_657 ?
I1 Pb1 I4 94.48(2) 3_556 . ?
I1 Pb1 I4 93.220(19) . . ?
I1 Pb1 I1 88.25(2) 3_556 . ?
I1 Pb1 I8 98.71(2) . 6_657 ?
I1 Pb1 I8 91.22(2) 3_556 6_657 ?
I1 Pb1 I2 89.460(16) 3_556 . ?
I1 Pb1 I2 175.56(2) . . ?
I2 Pb1 I4 83.17(2) . . ?
I2 Pb1 I8 85.14(2) . 6_657 ?
I3 Pb1 I4 90.083(17) . . ?
I3 Pb1 I1 82.319(15) . . ?
I3 Pb1 I1 169.749(18) . 3_556 ?
I3 Pb1 I8 86.264(18) . 6_657 ?
I3 Pb1 I2 100.210(10) . . ?
Pb2 I4 Pb1 175.10(3) . . ?
Pb1 I1 Pb1 91.50(2) 3_556 . ?
Pb2 I5 Pb2 90.33(2) 3_556 . ?
Pb2 I8 Pb1 173.68(3) . 6_557 ?
Pb2 I7 Pb2 154.02(4) 2 . ?
Pb1 I2 Pb1 167.36(3) 3_557 . ?
Pb2 I6 Pb2 175.66(4) 3_557 . ?
Pb1 I3 Pb1 180.0 . 5_657 ?
C3 C4 H4 121.3 . . ?
C5 C4 H4 121.3 . . ?
C5 C4 C3 117.5(11) . . ?
C4 C3 C6 119.3(10) . . ?
C2 C3 C4 119.2(10) . . ?
C2 C3 C6 121.5(11) . . ?
N3 C6 C3 118.1(10) . . ?
N2 C6 C3 118.5(10) . . ?
N2 C6 N3 123.3(11) . . ?
C3 C2 H2 119.4 . . ?
C1 C2 C3 121.3(13) . . ?
C1 C2 H2 119.4 . . ?
C6 N3 H3A 120.0 . . ?
C6 N3 H3B 120.0 . . ?
H3A N3 H3B 120.0 . . ?
C6 N2 H2A 120.0 . . ?
C6 N2 H2B 120.0 . . ?
H2A N2 H2B 120.0 . . ?
C2 C1 H1 120.7 . . ?
N1 C1 C2 118.6(12) . . ?
N1 C1 H1 120.7 . . ?
C1 N1 H1A 118.3 . . ?
C5 N1 C1 123.4(11) . . ?
C5 N1 H1A 118.3 . . ?
C4 C5 H5 120.0 . . ?
N1 C5 C4 120.0(12) . . ?
N1 C5 H5 120.0 . . ?

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
C4 C3 C6 N3 40.5(14) . . . . ?
C4 C3 C6 N2 -137.6(11) . . . . ?
C4 C3 C2 C1 2.0(16) . . . . ?
C3 C4 C5 N1 3.0(15) . . . . ?
C3 C2 C1 N1 1(2) . . . . ?
C6 C3 C2 C1 -177.3(11) . . . . ?
C2 C3 C6 N3 -140.3(11) . . . . ?
C2 C3 C6 N2 41.6(15) . . . . ?
C2 C1 N1 C5 -1(2) . . . . ?
C1 N1 C5 C4 -0.5(19) . . . . ?
C5 C4 C3 C6 175.6(8) . . . . ?
C5 C4 C3 C2 -3.7(13) . . . . ?

_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 1.937
_oxdiff_exptl_absorpt_empirical_full_min 0.604
