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

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

data_2R
_database_code_depnum_ccdc_archive 'CCDC 2323588'
loop_
_audit_author_name
_audit_author_address
'Changchun Fan'
;southeast university
China
;
_audit_update_record             
;
2024-01-05 deposited with the CCDC.	2024-06-13 downloaded from the CCDC.
;
_audit_creation_date             2024-01-05
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'I6 Pb2, C7 H11 N2'
_chemical_formula_sum            'C7 H11 I6 N2 Pb2'
_chemical_formula_weight         1298.96
_chemical_absolute_configuration rmad
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C1 H1 N1 I1 Pb1'
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           20
_space_group_name_H-M_alt        'C 2 2 21'
_space_group_name_Hall           'C 2c 2'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'-x, y, -z+1/2'
'x, -y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'

_cell_length_a                   12.9873(5)
_cell_length_b                   18.8387(7)
_cell_length_c                   17.5741(8)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4299.7(3)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    5889
_cell_measurement_temperature    269.0(6)
_cell_measurement_theta_max      30.7170
_cell_measurement_theta_min      2.2200
_shelx_estimated_absorpt_T_max   0.085
_shelx_estimated_absorpt_T_min   0.085
_exptl_absorpt_coefficient_mu    24.245
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.57418
_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            'metallic dark red'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    4.013
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             4392
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0289
_diffrn_reflns_av_unetI/netI     0.0387
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.829
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            11070
_diffrn_reflns_point_group_measured_fraction_full 0.978
_diffrn_reflns_point_group_measured_fraction_max 0.758
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.503
_diffrn_reflns_theta_min         1.905
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      269.0(6)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.829
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω      0.00  28.00   0.50    1.00    --   -6.24 -99.00   0.00   56
  2  ω    -15.00  28.00   0.50    1.00    --   -6.24 -99.00-120.00   86
  3  ω    -19.00  15.00   0.50    1.00    --   -6.24  57.00 150.00   68
  4  ω     18.00  64.00   0.50    1.00    --   -6.24  78.00 150.00   92
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0032862000
_diffrn_orient_matrix_UB_12      -0.0011933000
_diffrn_orient_matrix_UB_13      0.0402848000
_diffrn_orient_matrix_UB_21      0.0289822000
_diffrn_orient_matrix_UB_22      -0.0318282000
_diffrn_orient_matrix_UB_23      -0.0024028000
_diffrn_orient_matrix_UB_31      0.0461462000
_diffrn_orient_matrix_UB_32      0.0200740000
_diffrn_orient_matrix_UB_33      -0.0013809000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_reflns_Friedel_coverage         0.668
_reflns_Friedel_fraction_full    0.954
_reflns_Friedel_fraction_max     0.672
_reflns_number_gt                4276
_reflns_number_total             4978
_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 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_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         1.504
_refine_diff_density_min         -0.848
_refine_diff_density_rms         0.179
_refine_ls_abs_structure_details 
;
 Flack x determined using 1538 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.006(8)
_refine_ls_extinction_coef       0.000459(16)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   0.974
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     160
_refine_ls_number_reflns         4978
_refine_ls_number_restraints     60
_refine_ls_R_factor_all          0.0361
_refine_ls_R_factor_gt           0.0286
_refine_ls_restrained_S_all      0.971
_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)+(0.0266P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0593
_refine_ls_wR_factor_ref         0.0612
_refine_special_details          ?
_olex2_refinement_description    
;
1. Rigid body (RIGU) restrains
 C5, C1, H1A, H1B, H1C, C2, N1, H2, C3, H1D, H1E, H1F, C4, N2, H4, C7, H5, C6,
 H7, H6
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
2.a Ternary CH refined with riding coordinates:
 C2(H2)
2.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C7(H7), C6(H6)
2.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), N1(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
Pb2 Pb 0.99615(3) 0.37635(2) 0.38089(2) 0.03443(11) Uani 1 1 d . . . . .
Pb1 Pb 0.50657(3) 0.37743(2) 0.37898(2) 0.03136(10) Uani 1 1 d . . . . .
I6 I 0.500000 0.50079(5) 0.250000 0.0357(2) Uani 1 2 d S T P . .
I5 I 0.53982(10) 0.500000 0.500000 0.0516(3) Uani 1 2 d S T P . .
I8 I 0.500000 0.25956(4) 0.250000 0.0319(2) Uani 1 2 d S T P . .
I4 I 0.75422(7) 0.35874(3) 0.36219(4) 0.04123(16) Uani 1 1 d . . . . .
I9 I 0.25767(7) 0.40511(4) 0.39393(4) 0.04503(18) Uani 1 1 d . . . . .
I3 I 1.000000 0.25479(4) 0.250000 0.0360(2) Uani 1 2 d S T P . .
I1 I 0.95859(10) 0.500000 0.500000 0.0511(3) Uani 1 2 d S T P . .
I7 I 0.48420(8) 0.26406(4) 0.50815(5) 0.0617(3) Uani 1 1 d . . . . .
C1 C 0.3416(10) 0.1252(7) 0.1121(6) 0.064(3) Uani 1 1 d . . . . .
H1A H 0.353522 0.074933 0.120325 0.095 Uiso 1 1 calc R U . . .
H1B H 0.397506 0.152260 0.134343 0.095 Uiso 1 1 calc R U . . .
H1C H 0.338071 0.134668 0.057929 0.095 Uiso 1 1 calc R U . . .
C4 C 0.2522(10) 0.0735(4) 0.2734(5) 0.0365(18) Uani 1 1 d . . . . .
H4 H 0.253356 0.030648 0.245935 0.044 Uiso 1 1 calc R U . . .
C5 C 0.2564(11) 0.0723(5) 0.3507(5) 0.043(2) Uani 1 1 d . . . . .
H5 H 0.258757 0.028723 0.376695 0.052 Uiso 1 1 calc R U . . .
C7 C 0.2545(11) 0.1973(5) 0.3507(6) 0.056(2) Uani 1 1 d . . . . .
H7 H 0.257278 0.240735 0.377022 0.067 Uiso 1 1 calc R U . . .
N2 N 0.2483(8) 0.1981(3) 0.2758(4) 0.0405(17) Uani 1 1 d . . . . .
N1 N 0.1557(8) 0.1025(6) 0.1181(5) 0.070(3) Uani 1 1 d . . . . .
H1D H 0.182129 0.062789 0.097448 0.106 Uiso 1 1 calc R U . . .
H1E H 0.121823 0.127239 0.082134 0.106 Uiso 1 1 calc R U . . .
H1F H 0.111893 0.090823 0.155728 0.106 Uiso 1 1 calc R U . . .
C2 C 0.2404(11) 0.1466(5) 0.1494(6) 0.047(2) Uani 1 1 d . . . . .
H2 H 0.226321 0.197140 0.137747 0.057 Uiso 1 1 calc R U . . .
C3 C 0.2464(8) 0.1375(4) 0.2350(5) 0.0317(16) Uani 1 1 d . . . . .
I2 I 1.000000 0.48746(4) 0.250000 0.0337(2) Uani 1 2 d S T P . .
C6 C 0.2570(11) 0.1356(6) 0.3913(7) 0.058(3) Uani 1 1 d . . . . .
H6 H 0.259183 0.135910 0.444804 0.069 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 3.1765(10) . ?
Pb2 I3 3.2462(7) . ?
Pb2 I1 3.1695(4) . ?
Pb2 I7 3.2900(8) 8_556 ?
Pb2 I2 3.1105(7) . ?
Pb1 I6 3.2474(7) . ?
Pb1 I5 3.1688(4) . ?
Pb1 I8 3.1744(7) . ?
Pb1 I4 3.2490(10) . ?
Pb1 I9 3.2849(10) . ?
Pb1 I7 3.1303(8) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C1 H1C 0.9700 . ?
C1 C2 1.523(17) . ?
C4 H4 0.9400 . ?
C4 C5 1.361(13) . ?
C4 C3 1.383(10) . ?
C5 H5 0.9400 . ?
C5 C6 1.390(14) . ?
C7 H7 0.9400 . ?
C7 N2 1.320(13) . ?
C7 C6 1.364(15) . ?
N2 C3 1.349(9) . ?
N1 H1D 0.9000 . ?
N1 H1E 0.9000 . ?
N1 H1F 0.9000 . ?
N1 C2 1.484(14) . ?
C2 H2 0.9900 . ?
C2 C3 1.516(13) . ?
C6 H6 0.9400 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
I4 Pb2 I3 82.428(14) . . ?
I4 Pb2 I7 86.02(2) . 8_556 ?
I3 Pb2 I7 81.577(19) . 8_556 ?
I1 Pb2 I4 89.59(3) . . ?
I1 Pb2 I3 171.42(3) . . ?
I1 Pb2 I7 101.082(19) . 8_556 ?
I2 Pb2 I4 90.554(15) . . ?
I2 Pb2 I3 87.159(18) . . ?
I2 Pb2 I1 89.788(14) . . ?
I2 Pb2 I7 168.56(2) . 8_556 ?
I6 Pb1 I4 92.303(15) . . ?
I6 Pb1 I9 85.203(14) . . ?
I5 Pb1 I6 87.170(13) . . ?
I5 Pb1 I8 173.06(3) . . ?
I5 Pb1 I4 90.29(3) . . ?
I5 Pb1 I9 87.98(3) . . ?
I8 Pb1 I6 90.083(19) . . ?
I8 Pb1 I4 83.450(14) . . ?
I8 Pb1 I9 98.147(16) . . ?
I4 Pb1 I9 177.029(19) . . ?
I7 Pb1 I6 172.74(2) . . ?
I7 Pb1 I5 91.324(19) . . ?
I7 Pb1 I8 92.18(2) . . ?
I7 Pb1 I4 94.81(2) . . ?
I7 Pb1 I9 87.65(2) . . ?
Pb1 I6 Pb1 88.62(2) . 3_655 ?
Pb1 I5 Pb1 164.33(5) 4_566 . ?
Pb1 I8 Pb1 91.22(2) . 3_655 ?
Pb2 I4 Pb1 163.43(2) . . ?
Pb2 I3 Pb2 90.27(2) . 3_755 ?
Pb2 I1 Pb2 162.29(5) 4_566 . ?
Pb1 I7 Pb2 166.91(3) . 8_456 ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
C5 C4 H4 119.9 . . ?
C5 C4 C3 120.2(8) . . ?
C3 C4 H4 119.9 . . ?
C4 C5 H5 120.0 . . ?
C4 C5 C6 120.0(9) . . ?
C6 C5 H5 120.0 . . ?
N2 C7 H7 118.9 . . ?
N2 C7 C6 122.2(9) . . ?
C6 C7 H7 118.9 . . ?
C7 N2 C3 121.5(8) . . ?
H1D N1 H1E 109.5 . . ?
H1D N1 H1F 109.5 . . ?
H1E N1 H1F 109.5 . . ?
C2 N1 H1D 109.5 . . ?
C2 N1 H1E 109.5 . . ?
C2 N1 H1F 109.5 . . ?
C1 C2 H2 109.0 . . ?
N1 C2 C1 109.3(9) . . ?
N1 C2 H2 109.0 . . ?
N1 C2 C3 110.0(9) . . ?
C3 C2 C1 110.6(11) . . ?
C3 C2 H2 109.0 . . ?
C4 C3 C2 125.9(8) . . ?
N2 C3 C4 118.6(8) . . ?
N2 C3 C2 115.6(7) . . ?
Pb2 I2 Pb2 95.41(3) 3_755 . ?
C5 C6 H6 121.2 . . ?
C7 C6 C5 117.5(11) . . ?
C7 C6 H6 121.2 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 C2 C3 C4 -68.7(14) . . . . ?
C1 C2 C3 N2 109.8(10) . . . . ?
C4 C5 C6 C7 -1(2) . . . . ?
C5 C4 C3 N2 2.1(16) . . . . ?
C5 C4 C3 C2 -179.4(13) . . . . ?
C7 N2 C3 C4 -0.6(16) . . . . ?
C7 N2 C3 C2 -179.3(12) . . . . ?
N2 C7 C6 C5 2(2) . . . . ?
N1 C2 C3 C4 52.1(16) . . . . ?
N1 C2 C3 N2 -129.3(10) . . . . ?
C3 C4 C5 C6 -1(2) . . . . ?
C6 C7 N2 C3 -2(2) . . . . ?

_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 1.422
_oxdiff_exptl_absorpt_empirical_full_min 0.645
####################################################################### 
# 
# 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_3R-240K
_database_code_depnum_ccdc_archive 'CCDC 2323590'
loop_
_audit_author_name
_audit_author_address
'Changchun Fan'
;southeast university
China
;
_audit_update_record             
;
2024-01-05 deposited with the CCDC.	2024-06-13 downloaded from the CCDC.
;
_audit_creation_date             2024-01-05
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'I6 Pb2, C7 H12 N2'
_chemical_formula_sum            'C7 H12 I6 N2 Pb2'
_chemical_formula_weight         1299.97
_chemical_absolute_configuration ad
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C H N I Pb'
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           20
_space_group_name_H-M_alt        'C 2 2 21'
_space_group_name_Hall           'C 2c 2'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'-x, y, -z+1/2'
'x, -y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'

_cell_length_a                   12.9493(3)
_cell_length_b                   18.7108(5)
_cell_length_c                   17.6439(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4274.97(19)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    9896
_cell_measurement_temperature    239.99(10)
_cell_measurement_theta_max      30.5500
_cell_measurement_theta_min      2.2360
_shelx_estimated_absorpt_T_max   0.085
_shelx_estimated_absorpt_T_min   0.085
_exptl_absorpt_coefficient_mu    24.385
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.27226
_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            'metallic dark red'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    4.040
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             4400
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0377
_diffrn_reflns_av_unetI/netI     0.0262
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            16605
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         1.913
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      239.99(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -24.00  52.00   0.50    2.60    --   -6.24  61.00  23.00  152
  2  ω    -18.00  28.00   0.50    2.60    --   -6.24 -99.00-150.00   92
  3  ω      1.00  27.00   0.50    2.60    --   -6.24 -99.00-120.00   52
  4  ω    -47.00  16.00   0.50    2.60    --    5.69 -57.00-150.00  126
  5  ω    -18.00  21.00   0.50    2.60    --    5.69 -99.00  30.00   78
  6  ω    -18.00   7.00   0.50    2.60    --   -6.24 -99.00  90.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0346994000
_diffrn_orient_matrix_UB_12      0.0187448000
_diffrn_orient_matrix_UB_13      -0.0239479000
_diffrn_orient_matrix_UB_21      0.0418129000
_diffrn_orient_matrix_UB_22      -0.0198475000
_diffrn_orient_matrix_UB_23      0.0151618000
_diffrn_orient_matrix_UB_31      -0.0068595000
_diffrn_orient_matrix_UB_32      -0.0262926000
_diffrn_orient_matrix_UB_33      -0.0285263000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_reflns_Friedel_coverage         0.793
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                3465
_reflns_number_total             3771
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_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    'olex2.solve 1.5 (Bourhis et al., 2015)'
_refine_diff_density_max         5.186
_refine_diff_density_min         -4.668
_refine_diff_density_rms         0.537
_refine_ls_abs_structure_details 
;
 Flack x determined using 1398 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.016(16)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     159
_refine_ls_number_reflns         3771
_refine_ls_number_restraints     66
_refine_ls_R_factor_all          0.0578
_refine_ls_R_factor_gt           0.0551
_refine_ls_restrained_S_all      1.061
_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)+(0.1238P)²+10.5576P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1602
_refine_ls_wR_factor_ref         0.1639
_refine_special_details          ?
_olex2_refinement_description    
;
1. Uiso/Uaniso restraints and constraints
Uanis(N1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
2. Rigid body (RIGU) restrains
 C6, N2, C7, C3, C4, C5, C2, N1, C1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3.a Ternary CH refined with riding coordinates:
 C2(H2A)
3.b Aromatic/amide H refined with riding coordinates:
 N2(H2), C4(H4), C5(H5), C6(H6), C7(H7)
3.c Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C), C1(H1D,H1E,H1F)
;
_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
Pb1 Pb 0.50244(4) 0.12423(3) 0.61994(4) 0.0211(3) Uani 1 1 d . . . . .
Pb2 Pb 0.50392(4) 0.37461(3) 0.37805(4) 0.0192(3) Uani 1 1 d . . . . .
I1 I 0.4676(2) 0.000000 0.500000 0.0396(7) Uani 1 2 d S T P . .
I2 I 0.500000 0.00919(10) 0.750000 0.0209(5) Uani 1 2 d S T P . .
I3 I 0.500000 0.24551(11) 0.750000 0.0214(5) Uani 1 2 d S T P . .
I4 I 0.25266(12) 0.13397(7) 0.62816(8) 0.0319(4) Uani 1 1 d . . . . .
I5 I 0.4925(3) 0.25770(12) 0.50483(10) 0.0615(7) Uani 1 1 d . . . . .
I6 I 0.5268(3) 0.500000 0.500000 0.0463(8) Uani 1 2 d S T P . .
I7 I 0.500000 0.49904(10) 0.250000 0.0212(4) Uani 1 2 d S T P . .
I8 I 0.500000 0.25656(10) 0.250000 0.0193(5) Uani 1 2 d S T P . .
I9 I 0.25417(13) 0.39414(11) 0.38929(9) 0.0458(4) Uani 1 1 d . . . . .
N1 N 0.6533(18) 0.6151(15) 0.1237(13) 0.085(7) Uani 1 1 d . U . . .
H1A H 0.640120 0.633745 0.077663 0.127 Uiso 1 1 calc R U . . .
H1B H 0.602108 0.626950 0.155818 0.127 Uiso 1 1 calc R U . . .
H1C H 0.657451 0.567221 0.120088 0.127 Uiso 1 1 calc R U . . .
N2 N 0.7561(17) 0.5594(9) 0.3497(9) 0.046(4) Uani 1 1 d . . . . .
H2 H 0.759743 0.516592 0.368914 0.055 Uiso 1 1 calc R U . . .
C1 C 0.839(2) 0.6224(16) 0.1166(13) 0.065(7) Uani 1 1 d . . . . .
H1D H 0.843598 0.570660 0.116829 0.098 Uiso 1 1 calc R U . . .
H1E H 0.897305 0.642468 0.143425 0.098 Uiso 1 1 calc R U . . .
H1F H 0.838701 0.639490 0.064685 0.098 Uiso 1 1 calc R U . . .
C2 C 0.749(2) 0.6429(14) 0.1516(14) 0.055(5) Uani 1 1 d . . . . .
H2A H 0.744985 0.695110 0.143013 0.065 Uiso 1 1 calc R U . . .
C3 C 0.7502(16) 0.6338(10) 0.2422(11) 0.036(4) Uani 1 1 d . . . . .
C4 C 0.7480(19) 0.6935(11) 0.2910(11) 0.043(4) Uani 1 1 d . . . . .
H4 H 0.744311 0.739425 0.269632 0.051 Uiso 1 1 calc R U . . .
C5 C 0.751(2) 0.6871(11) 0.3671(12) 0.046(4) Uani 1 1 d . . . . .
H5 H 0.750470 0.727029 0.399505 0.055 Uiso 1 1 calc R U . . .
C6 C 0.7544(17) 0.6192(11) 0.3936(13) 0.041(5) Uani 1 1 d . . . . .
H6 H 0.755758 0.612945 0.446450 0.050 Uiso 1 1 calc R U . . .
C7 C 0.7519(18) 0.5710(11) 0.2756(10) 0.037(4) Uani 1 1 d . . . . .
H7 H 0.749923 0.530542 0.244071 0.044 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 I1 3.1757(7) . ?
Pb1 I2 3.1465(15) . ?
Pb1 I3 3.2274(16) . ?
Pb1 I4 3.2429(17) . ?
Pb1 I5 3.2214(18) . ?
Pb1 I9 3.2819(19) 8_556 ?
Pb2 I4 3.2268(17) 8_556 ?
Pb2 I5 3.1323(18) . ?
Pb2 I6 3.1973(7) . ?
Pb2 I7 3.2446(15) . ?
Pb2 I8 3.1599(15) . ?
Pb2 I9 3.2607(18) . ?
N1 H1A 0.9000 . ?
N1 H1B 0.9000 . ?
N1 H1C 0.9000 . ?
N1 C2 1.43(3) . ?
N2 H2 0.8700 . ?
N2 C6 1.36(3) . ?
N2 C7 1.33(2) . ?
C1 H1D 0.9700 . ?
C1 H1E 0.9700 . ?
C1 H1F 0.9700 . ?
C1 C2 1.37(4) . ?
C2 H2A 0.9900 . ?
C2 C3 1.61(3) . ?
C3 C4 1.41(2) . ?
C3 C7 1.32(2) . ?
C4 H4 0.9400 . ?
C4 C5 1.35(3) . ?
C5 H5 0.9400 . ?
C5 C6 1.35(3) . ?
C6 H6 0.9400 . ?
C7 H7 0.9400 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
I1 Pb1 I3 170.76(5) . . ?
I1 Pb1 I4 85.93(5) . . ?
I1 Pb1 I5 98.14(4) . . ?
I1 Pb1 I9 91.81(6) . 8_556 ?
I2 Pb1 I1 89.07(3) . . ?
I2 Pb1 I3 87.84(4) . . ?
I2 Pb1 I4 89.76(3) . . ?
I2 Pb1 I5 171.77(6) . . ?
I2 Pb1 I9 88.54(3) . 8_556 ?
I3 Pb1 I4 85.35(3) . . ?
I3 Pb1 I9 96.81(4) . 8_556 ?
I4 Pb1 I9 177.19(4) . 8_556 ?
I5 Pb1 I3 84.42(4) . . ?
I5 Pb1 I4 86.82(7) . . ?
I5 Pb1 I9 95.15(7) . 8_556 ?
I4 Pb2 I7 91.59(3) 8_556 . ?
I4 Pb2 I9 176.09(4) 8_556 . ?
I5 Pb2 I4 92.11(7) . 8_556 ?
I5 Pb2 I6 92.08(4) . . ?
I5 Pb2 I7 176.09(7) . . ?
I5 Pb2 I8 91.24(4) . . ?
I5 Pb2 I9 89.30(7) . . ?
I6 Pb2 I4 88.10(6) . 8_556 ?
I6 Pb2 I7 86.76(3) . . ?
I6 Pb2 I9 88.21(7) . . ?
I7 Pb2 I9 86.93(3) . . ?
I8 Pb2 I4 87.54(3) . 8_556 ?
I8 Pb2 I6 174.61(6) . . ?
I8 Pb2 I7 90.20(4) . . ?
I8 Pb2 I9 96.08(4) . . ?
Pb1 I1 Pb1 163.64(10) . 4_556 ?
Pb1 I2 Pb1 93.67(6) 3_656 . ?
Pb1 I3 Pb1 90.65(6) 3_656 . ?
Pb2 I4 Pb1 172.43(5) 8_456 . ?
Pb2 I5 Pb1 171.77(10) . . ?
Pb2 I6 Pb2 169.36(12) 4_566 . ?
Pb2 I7 Pb2 88.29(5) . 3_655 ?
Pb2 I8 Pb2 91.31(5) . 3_655 ?
Pb2 I9 Pb1 166.02(7) . 8_456 ?
H1A N1 H1B 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1B N1 H1C 109.5 . . ?
C2 N1 H1A 109.5 . . ?
C2 N1 H1B 109.5 . . ?
C2 N1 H1C 109.5 . . ?
C6 N2 H2 122.4 . . ?
C7 N2 H2 122.4 . . ?
C7 N2 C6 115.1(19) . . ?
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 . . ?
N1 C2 H2A 104.9 . . ?
N1 C2 C3 108(2) . . ?
C1 C2 N1 119(3) . . ?
C1 C2 H2A 104.9 . . ?
C1 C2 C3 114(2) . . ?
C3 C2 H2A 104.9 . . ?
C4 C3 C2 121.5(18) . . ?
C7 C3 C2 122.7(18) . . ?
C7 C3 C4 116(2) . . ?
C3 C4 H4 118.7 . . ?
C5 C4 C3 123(2) . . ?
C5 C4 H4 118.7 . . ?
C4 C5 H5 122.4 . . ?
C4 C5 C6 115.3(19) . . ?
C6 C5 H5 122.4 . . ?
N2 C6 H6 117.4 . . ?
C5 C6 N2 125(2) . . ?
C5 C6 H6 117.4 . . ?
N2 C7 H7 116.9 . . ?
C3 C7 N2 126(2) . . ?
C3 C7 H7 116.9 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N1 H1A I5 0.90 2.95 3.69(2) 140.3 2_664 yes
N1 H1B I3 0.90 3.19 3.96(3) 144.7 2_664 yes
N1 H1B I7 0.90 3.20 3.69(2) 116.6 . yes
N2 H2 I4 0.87 2.82 3.639(18) 157.6 8_556 yes
C1 H1E I8 0.97 3.14 4.03(3) 152.5 5 yes
C2 H2A I4 0.99 3.21 4.20(3) 174.4 2_664 yes
C5 H5 I9 0.94 3.13 3.89(2) 139.3 5 yes
C6 H6 I4 0.94 3.23 4.15(2) 165.7 5 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
N1 C2 C3 C4 -113(3) . . . . ?
N1 C2 C3 C7 66(3) . . . . ?
C1 C2 C3 C4 113(3) . . . . ?
C1 C2 C3 C7 -68(3) . . . . ?
C2 C3 C4 C5 -179(3) . . . . ?
C2 C3 C7 N2 178(3) . . . . ?
C3 C4 C5 C6 -1(4) . . . . ?
C4 C3 C7 N2 -3(4) . . . . ?
C4 C5 C6 N2 1(4) . . . . ?
C6 N2 C7 C3 3(4) . . . . ?
C7 N2 C6 C5 -1(3) . . . . ?
C7 C3 C4 C5 2(3) . . . . ?

# end Validation Reply Form
_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 2.464
_oxdiff_exptl_absorpt_empirical_full_min 0.560
# start Validation Reply Form
_vrf_PLAT342_3R-240K             
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.03167 Ang.  
RESPONSE: The high thermal parameters of organic cations reduce the 
precision of C-C bonds
;
####################################################################### 
# 
# 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_3S-298K
_database_code_depnum_ccdc_archive 'CCDC 2323593'
loop_
_audit_author_name
_audit_author_address
'Changchun Fan'
;southeast university
China
;
_audit_update_record             
;
2024-01-05 deposited with the CCDC.	2024-06-13 downloaded from the CCDC.
;
_audit_creation_date             2024-01-05
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'I6 Pb2, C7 H11 N2'
_chemical_formula_sum            'C7 H11 I6 N2 Pb2'
_chemical_formula_weight         1298.96
_chemical_absolute_configuration .
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C1 H1 N1 I1 Pb1'
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           20
_space_group_name_H-M_alt        'C 2 2 21'
_space_group_name_Hall           'C 2c 2'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'-x, y, -z+1/2'
'x, -y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'

_cell_length_a                   12.9621(7)
_cell_length_b                   18.7875(13)
_cell_length_c                   17.6666(9)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4302.3(4)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    3248
_cell_measurement_temperature    298.53(10)
_cell_measurement_theta_max      30.6130
_cell_measurement_theta_min      3.9010
_shelx_estimated_absorpt_T_max   0.643
_shelx_estimated_absorpt_T_min   0.530
_exptl_absorpt_coefficient_mu    24.230
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.71819
_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            'metallic reddish red'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    4.011
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             4392
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0252
_diffrn_reflns_av_unetI/netI     0.0380
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.808
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            11819
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.759
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.652
_diffrn_reflns_theta_min         1.909
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      298.53(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.808
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -23.00  53.00   0.50    2.00    --   -7.05  38.00   0.00  152
  2  ω    -35.00  -3.00   0.50    2.00    --   -7.05  87.00 134.00   64
  3  ω    -18.00  14.00   0.50    2.00    --   -7.05 -99.00-120.00   64
  4  ω     -9.00  18.00   0.50    2.00    --   -7.05 -99.00-150.00   54
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0116812000
_diffrn_orient_matrix_UB_12      -0.0368952000
_diffrn_orient_matrix_UB_13      0.0005537000
_diffrn_orient_matrix_UB_21      -0.0476403000
_diffrn_orient_matrix_UB_22      0.0069374000
_diffrn_orient_matrix_UB_23      -0.0183189000
_diffrn_orient_matrix_UB_31      0.0242479000
_diffrn_orient_matrix_UB_32      -0.0041222000
_diffrn_orient_matrix_UB_33      -0.0357085000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_reflns_Friedel_coverage         0.716
_reflns_Friedel_fraction_full    0.958
_reflns_Friedel_fraction_max     0.700
_reflns_number_gt                3198
_reflns_number_total             5064
_reflns_odcompleteness_completeness 99.80
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_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    'olex2.solve (Bourhis et al., 2015)'
_refine_diff_density_max         1.955
_refine_diff_density_min         -2.707
_refine_diff_density_rms         0.293
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.41(2)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     176
_refine_ls_number_reflns         5064
_refine_ls_number_restraints     374
_refine_ls_R_factor_all          0.0791
_refine_ls_R_factor_gt           0.0424
_refine_ls_restrained_S_all      1.053
_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)+(0.0414P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0952
_refine_ls_wR_factor_ref         0.1058
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.58546
 0.41454
2. Restrained distances
 N1B-C2 = N1A-C2
 1.47 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
N2 \\sim H2 \\sim C2 \\sim H2A \\sim C3 \\sim C4 \\sim H4 \\sim C5 \\sim H5
\\sim C6 \\sim H6 \\sim C7 \\sim H7 \\sim N1A \\sim H1AA \\sim H1AB \\sim H1AC
\\sim C1A \\sim H1AD \\sim H1AE \\sim H1AF \\sim N1B \\sim H1BA \\sim H1BB
\\sim C1B \\sim H1BC \\sim H1BD \\sim H1BE: within 1.7A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 1.7A
Uanis(N1A) \\sim Ueq, Uanis(C1B) \\sim Ueq, Uanis(N1B) \\sim Ueq, Uanis(C1A)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 N2, H2, C2, C3, C4, H4, C5, H5, C6, H6, C7, H7, N1A, C1A, N1B, C1B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C7, C3, C4, C5, C6, N2, C2, N1B, C1A, N1A, C1B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: H2A(0.5) N1A(0.5) H1AA(0.5) H1AB(0.5) H1AC(0.5) C1A(0.5) H1AD(0.5)
 H1AE(0.5) H1AF(0.5) N1B(0.5) H1BA(0.5) H1BB(0.5) C1B(0.5) H1BC(0.5) H1BD(0.5)
 H1BE(0.5)
6.a Riding coordinates:
 N1A(H1AA,H1AB,H1AC), C1A(H1AD,H1AE,H1AF), C1B(H1BC,H1BD,H1BE)
6.b Ternary CH refined with riding coordinates:
 C2(H2A)
6.c Aromatic/amide H refined with riding coordinates:
 N2(H2), C4(H4), C5(H5), C6(H6), C7(H7)
6.d X=CH2 refined with riding coordinates:
 N1B(H1BA,H1BB)
;
_atom_sites_solution_hydrogens   mixed
_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
Pb1 Pb 0.50366(5) 0.87540(4) 1.11965(4) 0.0313(2) Uani 1 1 d . . . . .
Pb2 Pb 0.50125(5) 0.62501(4) 0.87857(4) 0.0313(2) Uani 1 1 d . . . . .
I1 I 0.500000 0.75564(12) 1.250000 0.0308(5) Uani 1 2 d S T P . .
I2 I 0.500000 0.99043(13) 1.250000 0.0333(5) Uani 1 2 d S T P . .
I3 I 0.5303(2) 1.000000 1.000000 0.0516(7) Uani 1 2 d S T P . .
I4 I 0.500000 0.50276(13) 0.750000 0.0326(5) Uani 1 2 d S T P . .
I5 I 0.4762(3) 0.500000 1.000000 0.0668(9) Uani 1 2 d S T P . .
I6 I 0.500000 0.74265(13) 0.750000 0.0342(6) Uani 1 2 d S T P . .
I7 I 0.75160(14) 0.86566(7) 1.12723(5) 0.0429(3) Uani 1 1 d . . . . .
I8 I 0.75135(15) 0.60834(7) 0.88967(6) 0.0575(4) Uani 1 1 d . . . . .
I9 I 0.4909(3) 0.74543(15) 1.00227(14) 0.0780(6) Uani 1 1 d . . . . .
N2 N 0.744(2) 0.9392(10) 0.8529(8) 0.083(5) Uani 1 1 d . U . . .
H2 H 0.734808 0.979246 0.875290 0.100 Uiso 1 1 calc R U . . .
C2 C 0.747(2) 0.8540(13) 0.6578(9) 0.085(6) Uani 1 1 d D U . . .
H2A H 0.749507 0.803493 0.644252 0.102 Uiso 0.5 1 calc R U P A 1
C3 C 0.748(2) 0.8671(9) 0.7430(6) 0.042(3) Uani 1 1 d . U . . .
C4 C 0.751(2) 0.8093(9) 0.7861(8) 0.056(4) Uani 1 1 d . U . . .
H4 H 0.748149 0.765066 0.762575 0.067 Uiso 1 1 calc R U . . .
C5 C 0.758(2) 0.8115(11) 0.8635(9) 0.064(5) Uani 1 1 d . U . . .
H5 H 0.763719 0.770996 0.893448 0.077 Uiso 1 1 calc R U . . .
C6 C 0.7543(19) 0.8783(12) 0.8920(11) 0.075(5) Uani 1 1 d . U . . .
H6 H 0.759627 0.882521 0.944281 0.091 Uiso 1 1 calc R U . . .
C7 C 0.750(2) 0.9345(9) 0.7757(9) 0.051(3) Uani 1 1 d . U . . .
H7 H 0.754749 0.975208 0.745981 0.061 Uiso 1 1 calc R U . . .
N1A N 0.821(3) 0.898(2) 0.617(2) 0.083(10) Uani 0.5 1 d D U P B 1
H1AA H 0.830971 0.879242 0.570626 0.100 Uiso 0.5 1 d R U P B 1
H1AB H 0.880681 0.897722 0.641706 0.100 Uiso 0.5 1 d R U P B 1
H1AC H 0.797871 0.941922 0.612266 0.100 Uiso 0.5 1 d R U P B 1
C1A C 0.657(3) 0.892(2) 0.625(2) 0.043(8) Uani 0.5 1 d . U P B 1
H1AD H 0.596411 0.880657 0.653503 0.065 Uiso 0.5 1 d R U P B 1
H1AE H 0.648111 0.877597 0.573353 0.065 Uiso 0.5 1 d R U P B 1
H1AF H 0.669521 0.942317 0.627103 0.065 Uiso 0.5 1 d R U P B 1
N1B N 0.655(3) 0.859(2) 0.615(2) 0.080(10) Uani 0.5 1 d D U P B 2
H1BA H 0.657703 0.872887 0.568661 0.096 Uiso 0.5 1 calc R U P B 2
H1BB H 0.596990 0.848470 0.635373 0.096 Uiso 0.5 1 calc R U P B 2
C1B C 0.852(3) 0.872(3) 0.626(3) 0.062(9) Uani 0.5 1 d . U P B 2
H1BC H 0.866858 0.921569 0.632893 0.093 Uiso 0.5 1 d R U P B 2
H1BD H 0.852288 0.861139 0.572643 0.093 Uiso 0.5 1 d R U P B 2
H1BE H 0.903728 0.843899 0.650833 0.093 Uiso 0.5 1 d R U P B 2


_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 I1 3.2200(19) . ?
Pb1 I2 3.1584(19) . ?
Pb1 I3 3.1729(9) . ?
Pb1 I7 3.222(2) . ?
Pb1 I8 3.289(2) 8_467 ?
Pb1 I9 3.208(2) . ?
Pb2 I4 3.230(2) . ?
Pb2 I5 3.1974(9) . ?
Pb2 I6 3.1693(19) . ?
Pb2 I7 3.242(2) 8_467 ?
Pb2 I8 3.263(2) . ?
Pb2 I9 3.148(2) . ?
N2 H2 0.8600 . ?
N2 C6 1.34(2) . ?
N2 C7 1.367(18) . ?
C2 H2A 0.9800 . ?
C2 C3 1.53(2) . ?
C2 N1A 1.46(2) . ?
C2 C1A 1.48(5) . ?
C2 N1B 1.41(2) . ?
C2 C1B 1.51(6) . ?
C3 C4 1.33(2) . ?
C3 C7 1.39(2) . ?
C4 H4 0.9300 . ?
C4 C5 1.370(19) . ?
C5 H5 0.9300 . ?
C5 C6 1.35(3) . ?
C6 H6 0.9300 . ?
C7 H7 0.9300 . ?
N1A H1AA 0.8901 . ?
N1A H1AB 0.8900 . ?
N1A H1AC 0.8900 . ?
C1A H1AD 0.9600 . ?
C1A H1AE 0.9599 . ?
C1A H1AF 0.9599 . ?
N1B H1BA 0.8600 . ?
N1B H1BB 0.8600 . ?
C1B H1BC 0.9603 . ?
C1B H1BD 0.9599 . ?
C1B H1BE 0.9599 . ?

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
I1 Pb1 I7 86.86(3) . . ?
I1 Pb1 I8 94.94(3) . 8_467 ?
I2 Pb1 I1 87.50(4) . . ?
I2 Pb1 I3 89.00(4) . . ?
I2 Pb1 I7 91.35(3) . . ?
I2 Pb1 I8 87.59(3) . 8_467 ?
I2 Pb1 I9 172.48(6) . . ?
I3 Pb1 I1 173.51(5) . . ?
I3 Pb1 I7 87.76(6) . . ?
I3 Pb1 I8 90.37(6) . 8_467 ?
I3 Pb1 I9 97.85(5) . . ?
I7 Pb1 I8 177.87(5) . 8_467 ?
I9 Pb1 I1 85.97(5) . . ?
I9 Pb1 I7 92.02(7) . . ?
I9 Pb1 I8 89.25(7) . 8_467 ?
I4 Pb2 I7 90.64(3) . 8_467 ?
I4 Pb2 I8 88.80(3) . . ?
I5 Pb2 I4 87.08(4) . . ?
I5 Pb2 I7 87.69(6) . 8_467 ?
I5 Pb2 I8 89.43(7) . . ?
I6 Pb2 I4 89.53(4) . . ?
I6 Pb2 I5 173.02(6) . . ?
I6 Pb2 I7 86.25(3) . 8_467 ?
I6 Pb2 I8 96.61(3) . . ?
I7 Pb2 I8 177.08(4) 8_467 . ?
I9 Pb2 I4 177.18(7) . . ?
I9 Pb2 I5 93.31(5) . . ?
I9 Pb2 I6 89.78(6) . . ?
I9 Pb2 I7 86.58(7) . 8_467 ?
I9 Pb2 I8 94.00(7) . . ?
Pb1 I1 Pb1 91.34(6) 3_657 . ?
Pb1 I2 Pb1 93.65(6) . 3_657 ?
Pb1 I3 Pb1 167.49(10) . 4_577 ?
Pb2 I4 Pb2 89.37(6) 3_656 . ?
Pb2 I5 Pb2 168.36(12) 4_567 . ?
Pb2 I6 Pb2 91.57(6) . 3_656 ?
Pb1 I7 Pb2 172.38(4) . 8_567 ?
Pb2 I8 Pb1 167.45(5) . 8_567 ?
Pb2 I9 Pb1 173.46(11) . . ?
C6 N2 H2 121.5 . . ?
C6 N2 C7 117.0(18) . . ?
C7 N2 H2 121.5 . . ?
C3 C2 H2A 113.4 . . ?
N1A C2 H2A 113.4 . . ?
N1A C2 C3 113(3) . . ?
N1A C2 C1A 93(3) . . ?
C1A C2 H2A 113.4 . . ?
C1A C2 C3 109(3) . . ?
N1B C2 C3 122(3) . . ?
N1B C2 C1B 123(3) . . ?
C1B C2 C3 109(3) . . ?
C4 C3 C2 115.7(17) . . ?
C4 C3 C7 120.4(14) . . ?
C7 C3 C2 123.8(17) . . ?
C3 C4 H4 118.3 . . ?
C3 C4 C5 123.3(17) . . ?
C5 C4 H4 118.3 . . ?
C4 C5 H5 123.3 . . ?
C6 C5 C4 113.4(17) . . ?
C6 C5 H5 123.3 . . ?
N2 C6 C5 127.0(18) . . ?
N2 C6 H6 116.5 . . ?
C5 C6 H6 116.5 . . ?
N2 C7 C3 118.1(16) . . ?
N2 C7 H7 121.0 . . ?
C3 C7 H7 121.0 . . ?
C2 N1A H1AA 109.5 . . ?
C2 N1A H1AB 108.9 . . ?
C2 N1A H1AC 110.1 . . ?
H1AA N1A H1AB 109.5 . . ?
H1AA N1A H1AC 109.5 . . ?
H1AB N1A H1AC 109.5 . . ?
C2 C1A H1AD 109.5 . . ?
C2 C1A H1AE 109.6 . . ?
C2 C1A H1AF 109.3 . . ?
H1AD C1A H1AE 109.5 . . ?
H1AD C1A H1AF 109.5 . . ?
H1AE C1A H1AF 109.5 . . ?
C2 N1B H1BA 120.0 . . ?
C2 N1B H1BB 120.0 . . ?
H1BA N1B H1BB 120.0 . . ?
C2 C1B H1BC 110.2 . . ?
C2 C1B H1BD 108.7 . . ?
C2 C1B H1BE 109.5 . . ?
H1BC C1B H1BD 109.5 . . ?
H1BC C1B H1BE 109.5 . . ?
H1BD C1B H1BE 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
C2 C3 C4 C5 177(3) . . . . ?
C2 C3 C7 N2 176(3) . . . . ?
C3 C4 C5 C6 4(4) . . . . ?
C4 C3 C7 N2 -6(4) . . . . ?
C4 C5 C6 N2 1(4) . . . . ?
C6 N2 C7 C3 10(5) . . . . ?
C7 N2 C6 C5 -8(4) . . . . ?
C7 C3 C4 C5 -1(4) . . . . ?
N1A C2 C3 C4 -132(3) . . . . ?
N1A C2 C3 C7 46(4) . . . . ?
C1A C2 C3 C4 126(3) . . . . ?
C1A C2 C3 C7 -56(4) . . . . ?
N1B C2 C3 C4 102(3) . . . . ?
N1B C2 C3 C7 -80(4) . . . . ?
C1B C2 C3 C4 -106(3) . . . . ?
C1B C2 C3 C7 72(4) . . . . ?

_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 1.378
_oxdiff_exptl_absorpt_empirical_full_min 0.732
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.58546
2 0.41454

# start Validation Reply Form
_vrf_PLAT342_3S-298K             
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............       0.0218 Ang.  
RESPONSE: Organic cation in this structure inherently exhibit higher 
thermal parameters, which consequently lower the precision of 
the C-C bonds
;
_vrf_PLAT972_3S-298K             
;
PROBLEM: Check Calcd Resid. Dens.  0.00Ang From I6             -2.56 eA-3  
RESPONSE: This is caused by the heavy atomic effect of iodine
;
####################################################################### 
# 
# 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_3Rac-240K
_database_code_depnum_ccdc_archive 'CCDC 2323591'
loop_
_audit_author_name
_audit_author_address
'Changchun Fan'
;southeast university
China
;
_audit_update_record             
;
2024-01-05 deposited with the CCDC.	2024-06-13 downloaded from the CCDC.
;
_audit_creation_date             2024-01-05
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'I6 Pb2, 0.5(C14 H16 N4)'
_chemical_formula_sum            'C7 H8 I6 N2 Pb2'
_chemical_formula_weight         1295.93
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C H N I Pb'
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           64
_space_group_name_H-M_alt        'C m c e'
_space_group_name_Hall           '-C 2bc 2'
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'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1, z+1/2'
'x+1/2, -y+1/2, -z'
'-x+1/2, y+1, -z+1/2'
'-x, -y, -z'
'x, y-1/2, -z-1/2'
'-x, y, z'
'x, -y-1/2, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, y, -z-1/2'
'-x+1/2, y+1/2, z'
'x+1/2, -y, z-1/2'

_cell_length_a                   12.9279(4)
_cell_length_b                   18.7521(6)
_cell_length_c                   17.6600(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4281.2(2)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    7853
_cell_measurement_temperature    239.97(10)
_cell_measurement_theta_max      30.2530
_cell_measurement_theta_min      2.2780
_shelx_estimated_absorpt_T_max   0.085
_shelx_estimated_absorpt_T_min   0.085
_exptl_absorpt_coefficient_mu    24.349
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.07620
_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            'metallic reddish red'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    4.021
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             4368
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0828
_diffrn_reflns_av_unetI/netI     0.0556
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.832
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            15242
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.832
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.618
_diffrn_reflns_theta_min         2.172
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      239.97(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.832
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     -9.00  67.00   0.50    1.50    --    5.69  38.00 -30.00  152
  2  ω     -9.00  28.00   0.50    1.50    --   -6.24 -99.00-150.00   74
  3  ω    -22.00  10.00   0.50    1.50    --   -6.24 -94.00  39.00   64
  4  ω    -74.00  -4.00   0.50    1.50    --   -6.24 -42.00 149.00  140
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0147940000
_diffrn_orient_matrix_UB_12      -0.0508550000
_diffrn_orient_matrix_UB_13      -0.0029482000
_diffrn_orient_matrix_UB_21      -0.0152481000
_diffrn_orient_matrix_UB_22      0.0039783000
_diffrn_orient_matrix_UB_23      0.0348684000
_diffrn_orient_matrix_UB_31      -0.0340868000
_diffrn_orient_matrix_UB_32      0.0202628000
_diffrn_orient_matrix_UB_33      -0.0143184000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2333
_reflns_number_total             2864
_reflns_odcompleteness_completeness 99.84
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         3.238
_refine_diff_density_min         -2.918
_refine_diff_density_rms         0.471
_refine_ls_extinction_coef       0.000063(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     90
_refine_ls_number_reflns         2864
_refine_ls_number_restraints     74
_refine_ls_R_factor_all          0.0667
_refine_ls_R_factor_gt           0.0561
_refine_ls_restrained_S_all      1.034
_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)+(0.0848P)²+77.6044P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1520
_refine_ls_wR_factor_ref         0.1619
_refine_special_details          ?
_olex2_refinement_description    
;
1. Shared sites
{N1, C1}
2. Restrained distances
 C4-C6 = C4-C7
 2.38 with sigma of 0.01
 C3-C6
 2.74 with sigma of 0.01
 C5-C7
 2.72 with sigma of 0.01
 C6-N2
 1.34 with sigma of 0.01
 C7-N2
 1.34 with sigma of 0.01
 C3-C4 = C5-C4 = C3-C7 = C5-C6
 1.37 with sigma of 0.01
 C2-C3
 1.49 with sigma of 0.01
 C4-N2
 2.74 with sigma of 0.01
 C6-C7
 2.33 with sigma of 0.01
 C3-C5
 2.36 with sigma of 0.01
 N2-C3 = N2-C5
 2.34 with sigma of 0.01
 C2-C6
 4.25 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C2) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C5) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uiso(N1) = Uiso(C1)
4. Rigid body (RIGU) restrains
 C5, C6, C7, N2, C3, C4, C2, N1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: N1(0.5) H1A(0.5) H1B(0.5) H1C(0.5) C1(0.5)
6.a Riding coordinates:
 N1(H1A,H1B,H1C)
6.b Aromatic/amide H refined with riding coordinates:
 N2(H2), C4(H4), C5(H5), C6(H6), C7(H7)
;
_atom_sites_solution_hydrogens   mixed
_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 0.25134(2) 0.12491(2) 0.12078(2) 0.02295(19) Uani 1 1 d . . . . .
I1 I 0.27781(10) 0.000000 0.000000 0.0447(3) Uani 1 2 d S T P . .
I2 I 0.500000 0.13472(4) 0.12780(5) 0.0307(2) Uani 1 2 d S T P . .
I3 I 0.250000 0.250000 0.000000 0.0739(5) Uani 1 2 d S . P . .
I4 I 0.250000 0.00565(5) 0.250000 0.0254(2) Uani 1 2 d S T P . .
I5 I 0.250000 0.24356(5) 0.250000 0.0248(2) Uani 1 2 d S T P . .
I6 I 0.000000 0.10775(7) 0.10978(6) 0.0426(3) Uani 1 2 d S T P . .
N1 N 0.0954(14) 0.3781(6) 0.3795(8) 0.081(5) Uiso 0.5 1 d . . P . .
H1A H 0.143869 0.383244 0.344113 0.098 Uiso 0.5 1 d R U P . .
H1B H 0.093309 0.417124 0.408203 0.098 Uiso 0.5 1 d R U P . .
H1C H 0.110249 0.340504 0.408203 0.098 Uiso 0.5 1 d R U P . .
N2 N 0.000000 0.4374(5) 0.1429(6) 0.066(4) Uani 1 2 d DS T P . .
H2 H 0.000000 0.477823 0.119831 0.079 Uiso 1 2 calc R U P . .
C1 C 0.0954(14) 0.3781(6) 0.3795(8) 0.081(5) Uiso 0.5 1 d . . P . .
C2 C 0.000000 0.3671(12) 0.3419(6) 0.083(6) Uani 1 2 d DS TU P . .
C3 C 0.000000 0.3724(5) 0.2568(5) 0.040(3) Uani 1 2 d DS T P . .
C4 C 0.000000 0.3094(4) 0.2164(6) 0.051(3) Uani 1 2 d DS T P . .
H4 H 0.000000 0.265700 0.241312 0.061 Uiso 1 2 calc R U P . .
C5 C 0.000000 0.3126(5) 0.1387(6) 0.059(4) Uani 1 2 d DS TU P . .
H5 H 0.000000 0.270595 0.110616 0.071 Uiso 1 2 calc R U P . .
C6 C 0.000000 0.3769(6) 0.1021(5) 0.061(4) Uani 1 2 d DS T P . .
H6 H 0.000000 0.378743 0.049493 0.073 Uiso 1 2 calc R U P . .
C7 C 0.000000 0.4362(4) 0.2187(6) 0.049(3) Uani 1 2 d DS T P . .
H7 H 0.000000 0.478759 0.245657 0.059 Uiso 1 2 calc R 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 I1 3.1864(3) . ?
Pb1 I2 3.2223(3) . ?
Pb1 I3 3.1704(3) . ?
Pb1 I4 3.1952(7) . ?
Pb1 I5 3.1873(7) . ?
Pb1 I6 3.2710(4) . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 H1C 0.8900 . ?
N1 C2 1.416(18) . ?
N2 H2 0.8600 . ?
N2 C6 1.345(8) . ?
N2 C7 1.338(7) . ?
C2 C3 1.507(8) . ?
C3 C4 1.379(7) . ?
C3 C7 1.372(7) . ?
C4 H4 0.9300 . ?
C4 C5 1.375(8) . ?
C5 H5 0.9300 . ?
C5 C6 1.368(8) . ?
C6 H6 0.9300 . ?
C7 H7 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
I1 Pb1 I2 87.74(3) . . ?
I1 Pb1 I4 87.946(13) . . ?
I1 Pb1 I5 173.23(2) . . ?
I1 Pb1 I6 89.69(3) . . ?
I2 Pb1 I6 177.33(2) . . ?
I3 Pb1 I1 95.402(10) . . ?
I3 Pb1 I2 89.377(17) . . ?
I3 Pb1 I4 176.642(15) . . ?
I3 Pb1 I5 88.005(13) . . ?
I3 Pb1 I6 91.57(2) . . ?
I4 Pb1 I2 91.024(17) . . ?
I4 Pb1 I6 88.17(2) . . ?
I5 Pb1 I2 86.448(17) . . ?
I5 Pb1 I4 88.69(2) . . ?
I5 Pb1 I6 96.07(2) . . ?
Pb1 I1 Pb1 167.67(5) 3 . ?
Pb1 I2 Pb1 172.11(3) 11_655 . ?
Pb1 I3 Pb1 180.0 . 13 ?
Pb1 I4 Pb1 91.16(2) 8_545 . ?
Pb1 I5 Pb1 91.45(2) . 8_545 ?
Pb1 I6 Pb1 166.80(5) . 11 ?
H1A N1 H1B 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1B N1 H1C 109.5 . . ?
C2 N1 H1A 107.4 . . ?
C2 N1 H1B 111.1 . . ?
C2 N1 H1C 109.9 . . ?
C6 N2 H2 119.3 . . ?
C7 N2 H2 119.3 . . ?
C7 N2 C6 121.4(5) . . ?
N1 C2 N1 121.2(16) 11 . ?
N1 C2 C3 117.3(8) 11 . ?
N1 C2 C3 117.3(8) . . ?
C4 C3 C2 117.4(11) . . ?
C7 C3 C2 123.1(11) . . ?
C7 C3 C4 119.6(5) . . ?
C3 C4 H4 120.7 . . ?
C5 C4 C3 118.6(5) . . ?
C5 C4 H4 120.7 . . ?
C4 C5 H5 119.7 . . ?
C6 C5 C4 120.6(5) . . ?
C6 C5 H5 119.7 . . ?
N2 C6 C5 119.5(5) . . ?
N2 C6 H6 120.3 . . ?
C5 C6 H6 120.3 . . ?
N2 C7 C3 120.4(5) . . ?
N2 C7 H7 119.8 . . ?
C3 C7 H7 119.8 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 C2 C3 C4 -101.4(16) 11 . . . ?
N1 C2 C3 C4 101.4(16) . . . . ?
N1 C2 C3 C7 -78.6(16) . . . . ?
N1 C2 C3 C7 78.6(16) 11 . . . ?
C2 C3 C4 C5 180.000(2) . . . . ?
C2 C3 C7 N2 180.000(2) . . . . ?
C3 C4 C5 C6 0.000(2) . . . . ?
C4 C3 C7 N2 0.000(1) . . . . ?
C4 C5 C6 N2 0.000(2) . . . . ?
C6 N2 C7 C3 0.000(2) . . . . ?
C7 N2 C6 C5 0.000(2) . . . . ?
C7 C3 C4 C5 0.000(1) . . . . ?

# end Validation Reply Form
_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 3.921
_oxdiff_exptl_absorpt_empirical_full_min 0.394
# start Validation Reply Form
_vrf_PLAT971_3Rac-240K           
;
PROBLEM: Check Calcd Resid. Dens.  0.68Ang From I2              3.28 eA-3  
RESPONSE: This is caused by the heavy atomic effect of iodine
;
_vrf_PLAT972_3Rac-240K           
;
PROBLEM: Check Calcd Resid. Dens.  0.96Ang From Pb1            -2.97 eA-3  
RESPONSE: This is caused by the heavy atomic effect of lead.
;
####################################################################### 
# 
# 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_2S
_database_code_depnum_ccdc_archive 'CCDC 2323595'
loop_
_audit_author_name
_audit_author_address
'Changchun Fan'
;southeast university
China
;
_audit_update_record             
;
2024-01-05 deposited with the CCDC.	2024-06-13 downloaded from the CCDC.
;
_audit_creation_date             2024-01-05
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'I6 Pb2, C7 H12 N2'
_chemical_formula_sum            'C7 H12 I6 N2 Pb2'
_chemical_formula_weight         1299.97
_chemical_absolute_configuration rm
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C1 H1 N1 Pb1 I1'
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           20
_space_group_name_H-M_alt        'C 2 2 21'
_space_group_name_Hall           'C 2c 2'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'-x, y, -z+1/2'
'x, -y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'

_cell_length_a                   12.9972(3)
_cell_length_b                   18.8397(7)
_cell_length_c                   17.5687(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4301.9(2)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    5335
_cell_measurement_temperature    267.4(4)
_cell_measurement_theta_max      29.8800
_cell_measurement_theta_min      2.1710
_shelx_estimated_absorpt_T_max   0.085
_shelx_estimated_absorpt_T_min   0.085
_exptl_absorpt_coefficient_mu    24.232
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.03814
_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            'metallic dark red'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    4.014
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             4400
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0588
_diffrn_reflns_av_unetI/netI     0.0670
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            10901
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.492
_diffrn_reflns_theta_min         1.904
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      267.4(4)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_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    -15.00  44.00   0.50    1.60    --    7.97 -99.00  90.00  118
  2  ω    -16.00  29.00   0.50    1.60    --   -8.51 -99.00  60.00   90
  3  ω     -3.00  73.00   0.50    1.60    --    7.97  21.00-132.00  152
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0119119000
_diffrn_orient_matrix_UB_12      0.0355306000
_diffrn_orient_matrix_UB_13      0.0100566000
_diffrn_orient_matrix_UB_21      0.0086825000
_diffrn_orient_matrix_UB_22      0.0107934000
_diffrn_orient_matrix_UB_23      -0.0381353000
_diffrn_orient_matrix_UB_31      -0.0525426000
_diffrn_orient_matrix_UB_32      -0.0062606000
_diffrn_orient_matrix_UB_33      -0.0085972000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_reflns_Friedel_coverage         0.777
_reflns_Friedel_fraction_full    0.974
_reflns_Friedel_fraction_max     0.966
_reflns_number_gt                3513
_reflns_number_total             4402
_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 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_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         4.469
_refine_diff_density_min         -2.678
_refine_diff_density_rms         0.541
_refine_ls_abs_structure_details 
;
 Flack x determined using 1208 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.002(15)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     159
_refine_ls_number_reflns         4402
_refine_ls_number_restraints     60
_refine_ls_R_factor_all          0.0856
_refine_ls_R_factor_gt           0.0681
_refine_ls_restrained_S_all      0.999
_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)+(0.1209P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1653
_refine_ls_wR_factor_ref         0.1807
_refine_special_details          ?
_olex2_refinement_description    
;
1. Rigid body (RIGU) restrains
 N1, C2, C1, N2, C3, C4, C5, C6, C7
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
2.a Ternary CH refined with riding coordinates:
 C2(H2A)
2.b Aromatic/amide H refined with riding coordinates:
 C4(H4), N2(H2), C5(H5), C6(H6), C7(H7)
2.c Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C), C1(H1D,H1E,H1F)
;
_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
Pb01 Pb 0.50668(7) 0.62261(5) 0.37886(6) 0.0320(3) Uani 1 1 d . . . . .
Pb02 Pb 0.99605(7) 0.62364(5) 0.38087(6) 0.0354(3) Uani 1 1 d . . . . .
I003 I 0.500000 0.74056(14) 0.250000 0.0327(6) Uani 1 2 d S T P . .
I004 I 1.000000 0.51248(14) 0.250000 0.0344(6) Uani 1 2 d S T P . .
I005 I 0.75446(14) 0.64122(10) 0.36212(11) 0.0421(5) Uani 1 1 d . . . . .
I006 I 0.5395(2) 0.500000 0.500000 0.0521(8) Uani 1 2 d S T P . .
I007 I 0.25772(14) 0.59471(12) 0.39403(10) 0.0456(5) Uani 1 1 d . . . . .
I008 I 0.500000 0.49943(15) 0.250000 0.0364(6) Uani 1 2 d S T P . .
I009 I 1.000000 0.74501(15) 0.250000 0.0362(6) Uani 1 2 d S T P . .
I00A I 0.9583(2) 0.500000 0.500000 0.0509(8) Uani 1 2 d S T P . .
I00B I 0.4843(2) 0.73602(13) 0.50824(12) 0.0621(7) Uani 1 1 d . . . . .
C4 C 0.243(2) 0.4265(13) 0.2265(14) 0.036(5) Uani 1 1 d . . . . .
H4 H 0.238825 0.468765 0.254770 0.044 Uiso 1 1 calc R U . . .
N2 N 0.2515(19) 0.3030(11) 0.2234(13) 0.046(4) Uani 1 1 d . . . . .
H2 H 0.255643 0.262018 0.245981 0.055 Uiso 1 1 calc R U . . .
C3 C 0.252(2) 0.3619(13) 0.2644(15) 0.037(4) Uani 1 1 d . . . . .
C2 C 0.253(2) 0.3534(19) 0.3512(15) 0.054(6) Uani 1 1 d . . . . .
H2A H 0.262859 0.302552 0.363435 0.065 Uiso 1 1 calc R U . . .
C5 C 0.242(2) 0.4295(15) 0.1471(14) 0.041(5) Uani 1 1 d . . . . .
H5 H 0.242557 0.472875 0.120675 0.049 Uiso 1 1 calc R U . . .
N1 N 0.3403(18) 0.3936(17) 0.3828(14) 0.068(9) Uani 1 1 d . . . . .
H1A H 0.398942 0.379441 0.360246 0.081 Uiso 1 1 calc R U . . .
H1B H 0.344492 0.385640 0.433261 0.081 Uiso 1 1 calc R U . . .
H1C H 0.330683 0.440223 0.374374 0.081 Uiso 1 1 calc R U . . .
C6 C 0.241(2) 0.3642(17) 0.1090(19) 0.052(6) Uani 1 1 d . . . . .
H6 H 0.236120 0.363135 0.055647 0.062 Uiso 1 1 calc R U . . .
C7 C 0.245(2) 0.3059(15) 0.1464(16) 0.049(6) Uani 1 1 d . . . . .
H7 H 0.243856 0.263020 0.119064 0.059 Uiso 1 1 calc R U . . .
C1 C 0.151(2) 0.379(2) 0.3875(17) 0.065(10) Uani 1 1 d . . . . .
H1D H 0.152891 0.429804 0.394599 0.097 Uiso 1 1 calc R U . . .
H1E H 0.141433 0.355731 0.436403 0.097 Uiso 1 1 calc R U . . .
H1F H 0.093874 0.366612 0.354215 0.097 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
Pb01 I003 3.173(2) . ?
Pb01 I005 3.253(2) . ?
Pb01 I006 3.1699(10) . ?
Pb01 I007 3.289(2) . ?
Pb01 I008 3.243(2) . ?
Pb01 I00B 3.133(2) . ?
Pb02 I004 3.111(2) . ?
Pb02 I005 3.174(2) . ?
Pb02 I009 3.243(2) . ?
Pb02 I00A 3.1697(11) . ?
Pb02 I00B 3.288(2) 8_566 ?
C4 H4 0.9400 . ?
C4 C3 1.39(3) . ?
C4 C5 1.40(4) . ?
N2 H2 0.8700 . ?
N2 C3 1.32(3) . ?
N2 C7 1.36(3) . ?
C3 C2 1.53(4) . ?
C2 H2A 0.9900 . ?
C2 N1 1.47(4) . ?
C2 C1 1.55(4) . ?
C5 H5 0.9400 . ?
C5 C6 1.40(4) . ?
N1 H1A 0.9000 . ?
N1 H1B 0.9000 . ?
N1 H1C 0.9000 . ?
C6 H6 0.9400 . ?
C6 C7 1.28(4) . ?
C7 H7 0.9400 . ?
C1 H1D 0.9700 . ?
C1 H1E 0.9700 . ?
C1 H1F 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
I003 Pb01 I005 83.52(4) . . ?
I003 Pb01 I007 98.21(4) . . ?
I003 Pb01 I008 90.14(6) . . ?
I005 Pb01 I007 176.95(6) . . ?
I006 Pb01 I003 173.19(6) . . ?
I006 Pb01 I005 90.34(7) . . ?
I006 Pb01 I007 87.80(7) . . ?
I006 Pb01 I008 87.18(4) . . ?
I008 Pb01 I005 92.32(4) . . ?
I008 Pb01 I007 85.17(4) . . ?
I00B Pb01 I003 92.15(6) . . ?
I00B Pb01 I005 94.81(6) . . ?
I00B Pb01 I006 91.28(5) . . ?
I00B Pb01 I007 87.65(6) . . ?
I00B Pb01 I008 172.71(6) . . ?
I004 Pb02 I005 90.57(4) . . ?
I004 Pb02 I009 87.15(6) . . ?
I004 Pb02 I00A 89.76(4) . . ?
I004 Pb02 I00B 168.59(7) . 8_566 ?
I005 Pb02 I009 82.44(4) . . ?
I005 Pb02 I00B 86.08(6) . 8_566 ?
I009 Pb02 I00B 81.60(5) . 8_566 ?
I00A Pb02 I005 89.54(7) . . ?
I00A Pb02 I009 171.38(6) . . ?
I00A Pb02 I00B 101.10(5) . 8_566 ?
Pb01 I003 Pb01 91.11(7) 3_655 . ?
Pb02 I004 Pb02 95.36(8) 3_755 . ?
Pb02 I005 Pb01 163.47(7) . . ?
Pb01 I006 Pb01 164.52(12) . 4_566 ?
Pb01 I008 Pb01 88.62(8) . 3_655 ?
Pb02 I009 Pb02 90.33(8) 3_755 . ?
Pb02 I00A Pb02 162.18(11) . 4_566 ?
Pb01 I00B Pb02 166.91(8) . 8_466 ?
C3 C4 H4 119.5 . . ?
C3 C4 C5 121(3) . . ?
C5 C4 H4 119.5 . . ?
C3 N2 H2 119.7 . . ?
C3 N2 C7 121(2) . . ?
C7 N2 H2 119.7 . . ?
C4 C3 C2 125(3) . . ?
N2 C3 C4 118(3) . . ?
N2 C3 C2 117(3) . . ?
C3 C2 H2A 108.5 . . ?
C3 C2 C1 111(3) . . ?
N1 C2 C3 109(2) . . ?
N1 C2 H2A 108.5 . . ?
N1 C2 C1 110(3) . . ?
C1 C2 H2A 108.5 . . ?
C4 C5 H5 121.9 . . ?
C4 C5 C6 116(3) . . ?
C6 C5 H5 121.9 . . ?
C2 N1 H1A 109.5 . . ?
C2 N1 H1B 109.5 . . ?
C2 N1 H1C 109.5 . . ?
H1A N1 H1B 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1B N1 H1C 109.5 . . ?
C5 C6 H6 119.7 . . ?
C7 C6 C5 121(3) . . ?
C7 C6 H6 119.7 . . ?
N2 C7 H7 118.4 . . ?
C6 C7 N2 123(3) . . ?
C6 C7 H7 118.4 . . ?
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 . . ?

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 C2 N1 -59(4) . . . . ?
C4 C3 C2 C1 63(4) . . . . ?
C4 C5 C6 C7 -3(4) . . . . ?
N2 C3 C2 N1 125(3) . . . . ?
N2 C3 C2 C1 -112(3) . . . . ?
C3 C4 C5 C6 5(4) . . . . ?
C3 N2 C7 C6 1(5) . . . . ?
C5 C4 C3 N2 -4(4) . . . . ?
C5 C4 C3 C2 -180(3) . . . . ?
C5 C6 C7 N2 0(5) . . . . ?
C7 N2 C3 C4 1(4) . . . . ?
C7 N2 C3 C2 177(3) . . . . ?

# end Validation Reply Form
_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 7.513
_oxdiff_exptl_absorpt_empirical_full_min 0.298
# start Validation Reply Form
_vrf_PLAT342_2S                  
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.03667 Ang.  
RESPONSE: Organic cation in this structure inherently exhibit higher 
thermal parameters, which consequently lower the precision of 
the C-C bonds.
;
####################################################################### 
# 
# 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_3S-425K
_database_code_depnum_ccdc_archive 'CCDC 2323594'
loop_
_audit_author_name
_audit_author_address
'Changchun Fan'
;southeast university
China
;
_audit_update_record             
;
2024-01-05 deposited with the CCDC.	2024-06-13 downloaded from the CCDC.
;
_audit_creation_date             2023-09-09
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '0.5(I12 Pb4), C7 H12 N2'
_chemical_formula_sum            'C7 H12 I6 N2 Pb2'
_chemical_formula_weight         1299.97
_chemical_absolute_configuration ad
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C H N I Pb'
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           21
_space_group_name_H-M_alt        'C 2 2 2'
_space_group_name_Hall           'C 2 2'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-x, y, -z'
'x, -y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z'
'-x+1/2, y+1/2, -z'
'x+1/2, -y+1/2, -z'

_cell_length_a                   9.4743(7)
_cell_length_b                   17.7301(12)
_cell_length_c                   6.5088(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1093.35(13)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    2570
_cell_measurement_temperature    425.00(10)
_cell_measurement_theta_max      30.9050
_cell_measurement_theta_min      2.4210
_shelx_estimated_absorpt_T_max   0.199
_shelx_estimated_absorpt_T_min   0.199
_exptl_absorpt_coefficient_mu    23.836
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.09991
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.84a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            ?
_exptl_crystal_density_diffrn    3.949
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1100
_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  0.0729
_diffrn_reflns_av_unetI/netI     0.0503
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.886
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            6242
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.851
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.565
_diffrn_reflns_theta_min         2.297
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      425.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.886
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -17.00  33.00   0.50    1.10    --    4.67 -99.00-150.00  100
  2  ω    -64.00  -4.00   0.50    1.10    --   -5.45 -38.00-150.00  120
  3  ω    -78.00  -3.00   0.50    1.10    --   -5.45 -57.00   0.00  150
  4  ω    -75.00   7.00   0.50    1.10    --   -5.45 -38.00  90.00  164
  5  ω      9.00  41.00   0.50    1.10    --    4.67  38.00  30.00   64
  6  ω     52.00  78.00   0.50    1.10    --    4.67  38.00  30.00   52
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0148587000
_diffrn_orient_matrix_UB_12      -0.0065014000
_diffrn_orient_matrix_UB_13      0.0394836000
_diffrn_orient_matrix_UB_21      0.0960230000
_diffrn_orient_matrix_UB_22      -0.0348889000
_diffrn_orient_matrix_UB_23      0.0032046000
_diffrn_orient_matrix_UB_31      0.0493288000
_diffrn_orient_matrix_UB_32      0.0659247000
_diffrn_orient_matrix_UB_33      0.0055952000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_reflns_Friedel_coverage         0.651
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.803
_reflns_number_gt                1136
_reflns_number_total             1443
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.84a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.84a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.84a (Rigaku OD, 2023)'
_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         1.819
_refine_diff_density_min         -1.738
_refine_diff_density_rms         0.254
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.52(5)
_refine_ls_extinction_coef       0.0019(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.107
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     94
_refine_ls_number_reflns         1443
_refine_ls_number_restraints     114
_refine_ls_R_factor_all          0.0566
_refine_ls_R_factor_gt           0.0414
_refine_ls_restrained_S_all      1.067
_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)+(0.0429P)²+6.0408P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1052
_refine_ls_wR_factor_ref         0.1096
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.47887
 0.52113
2. Uiso/Uaniso restraints and constraints
Uanis(C1) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(N2) \\sim
Ueq, Uanis(C4) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C5)
\\sim Ueq, Uanis(N1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms
of 0.02
3. Rigid body (RIGU) restrains
 N1, N2, C1, C2, C3, C4, C5, C6, C7
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Fixed Sof: N1(0.25) H1A(0.25) H1B(0.25) H1C(0.25) C1(0.25) H1D(0.25)
 H1E(0.25) H1F(0.25) C2(0.25) H2(0.25) C7(0.25) H7(0.25) C3(0.25) C4(0.25)
 H4(0.25) C5(0.25) H5(0.25) C6(0.25) H6(0.25) N2(0.25) H2A(0.25)
5.a Ternary CH refined with riding coordinates:
 C2(H2)
5.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C4(H4), C5(H5), C6(H6), N2(H2A)
5.c Fitted hexagon refined as free rotating group:
 C7(C3,C4,C5,C6,N2)
5.d Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C), 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 0.500000 0.63009(3) -0.500000 0.0488(3) Uani 1 2 d S T P . .
I1 I 0.26566(13) 0.500000 -0.500000 0.0524(4) Uani 1 2 d S T P . .
I2 I 0.500000 0.63097(10) -1.000000 0.1000(8) Uani 1 2 d S T P . .
I3 I 0.750000 0.750000 -0.499(2) 0.1172(8) Uani 1 2 d S T P . .
N1 N 0.974(5) 0.376(3) -1.208(8) 0.044(11) Uani 0.25 1 d . U P A -1
H1A H 0.993461 0.407108 -1.311705 0.053 Uiso 0.25 1 calc R U P A -1
H1B H 0.881584 0.374675 -1.187072 0.053 Uiso 0.25 1 calc R U P A -1
H1C H 1.005746 0.330150 -1.236923 0.053 Uiso 0.25 1 calc R U P A -1
C1 C 0.939(9) 0.360(4) -0.877(13) 0.053(14) Uani 0.25 1 d . U P A -1
H1D H 0.937553 0.387751 -0.750200 0.079 Uiso 0.25 1 calc R U P A -1
H1E H 0.974941 0.309995 -0.851129 0.079 Uiso 0.25 1 calc R U P A -1
H1F H 0.845399 0.356490 -0.931213 0.079 Uiso 0.25 1 calc R U P A -1
C2 C 1.038(5) 0.401(3) -1.037(9) 0.045(9) Uani 0.25 1 d . U P A -1
H2 H 1.137438 0.385812 -1.027125 0.054 Uiso 0.25 1 calc R U P A -1
C7 C 0.879(3) 0.5188(13) -0.993(18) 0.047(8) Uani 0.25 1 d G U P A -1
H7 H 0.804051 0.484888 -0.994349 0.057 Uiso 0.25 1 calc R U P A -1
C3 C 1.017(3) 0.4924(14) -1.01(2) 0.047(7) Uani 0.25 1 d G U P A -1
C4 C 1.129(3) 0.5430(18) -1.005(19) 0.050(8) Uani 0.25 1 d G U P A -1
H4 H 1.221098 0.525440 -1.014947 0.060 Uiso 0.25 1 calc R U P A -1
C5 C 1.103(2) 0.6200(16) -0.988(12) 0.042(9) Uani 0.25 1 d G U P A -1
H5 H 1.178037 0.653833 -0.986680 0.050 Uiso 0.25 1 calc R U P A -1
C6 C 0.965(2) 0.6463(12) -0.974(7) 0.032(10) Uani 0.25 1 d G U P A -1
H6 H 0.947984 0.697755 -0.962249 0.038 Uiso 0.25 1 calc R U P A -1
N2 N 0.853(2) 0.5957(14) -0.976(10) 0.046(9) Uani 0.25 1 d G U P A -1
H2A H 0.767930 0.611959 -0.966820 0.055 Uiso 0.25 1 calc R U P A -1


_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 I1 3.2015(9) . ?
Pb1 I1 3.2015(9) 2_665 ?
Pb1 I2 3.25444(19) 1_556 ?
Pb1 I2 3.25444(19) . ?
Pb1 I3 3.1827(4) . ?
Pb1 I3 3.1827(4) 3_654 ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 H1C 0.8900 . ?
N1 C2 1.34(7) . ?
C1 H1D 0.9600 . ?
C1 H1E 0.9600 . ?
C1 H1F 0.9600 . ?
C1 C2 1.59(9) . ?
C2 H2 0.9800 . ?
C2 C3 1.64(6) . ?
C7 H7 0.9300 . ?
C7 C3 1.3900 . ?
C7 N2 1.3900 . ?
C3 C4 1.3900 . ?
C4 H4 0.9300 . ?
C4 C5 1.3900 . ?
C5 H5 0.9300 . ?
C5 C6 1.3900 . ?
C6 H6 0.9300 . ?
C6 N2 1.3900 . ?
N2 H2A 0.8600 . ?

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
I1 Pb1 I1 87.81(3) . 2_665 ?
I1 Pb1 I2 90.20(2) 2_665 . ?
I1 Pb1 I2 90.20(2) 2_665 1_556 ?
I1 Pb1 I2 90.20(2) . . ?
I1 Pb1 I2 90.20(2) . 1_556 ?
I2 Pb1 I2 179.46(6) 1_556 . ?
I3 Pb1 I1 175.82(2) 3_654 2_665 ?
I3 Pb1 I1 175.82(2) . . ?
I3 Pb1 I1 88.003(17) . 2_665 ?
I3 Pb1 I1 88.003(17) 3_654 . ?
I3 Pb1 I2 89.8(3) . 1_556 ?
I3 Pb1 I2 89.9(3) 3_654 1_556 ?
I3 Pb1 I2 89.8(3) 3_654 . ?
I3 Pb1 I2 89.9(3) . . ?
I3 Pb1 I3 96.180(17) . 3_654 ?
Pb1 I1 Pb1 92.19(3) 2_665 . ?
Pb1 I2 Pb1 179.46(6) . 1_554 ?
Pb1 I3 Pb1 179.9(5) . 6_665 ?
H1A N1 H1B 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1B N1 H1C 109.5 . . ?
C2 N1 H1A 109.5 . . ?
C2 N1 H1B 109.5 . . ?
C2 N1 H1C 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 . . ?
N1 C2 C1 97(6) . . ?
N1 C2 H2 113.1 . . ?
N1 C2 C3 112(6) . . ?
C1 C2 H2 113.1 . . ?
C1 C2 C3 108(5) . . ?
C3 C2 H2 113.1 . . ?
C3 C7 H7 120.0 . . ?
C3 C7 N2 120.0 . . ?
N2 C7 H7 120.0 . . ?
C7 C3 C2 117(2) . . ?
C4 C3 C2 123(2) . . ?
C4 C3 C7 120.0 . . ?
C3 C4 H4 120.0 . . ?
C5 C4 C3 120.0 . . ?
C5 C4 H4 120.0 . . ?
C4 C5 H5 120.0 . . ?
C4 C5 C6 120.0 . . ?
C6 C5 H5 120.0 . . ?
C5 C6 H6 120.0 . . ?
C5 C6 N2 120.0 . . ?
N2 C6 H6 120.0 . . ?
C7 N2 H2A 120.0 . . ?
C6 N2 C7 120.0 . . ?
C6 N2 H2A 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
N1 C2 C3 C7 59(7) . . . . ?
N1 C2 C3 C4 -118(6) . . . . ?
C1 C2 C3 C7 -46(8) . . . . ?
C1 C2 C3 C4 136(7) . . . . ?
C2 C3 C4 C5 177(10) . . . . ?
C7 C3 C4 C5 0.0 . . . . ?
C3 C7 N2 C6 0.0 . . . . ?
C3 C4 C5 C6 0.0 . . . . ?
C4 C5 C6 N2 0.0 . . . . ?
C5 C6 N2 C7 0.0 . . . . ?
N2 C7 C3 C2 -177(9) . . . . ?
N2 C7 C3 C4 0.0 . . . . ?

_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 5.399
_oxdiff_exptl_absorpt_empirical_full_min 0.221
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.47887
2 0.52113

####################################################################### 
# 
# 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_3R-425K
_database_code_depnum_ccdc_archive 'CCDC 2323597'
loop_
_audit_author_name
_audit_author_address
'Changchun Fan'
;southeast university
China
;
_audit_update_record             
;
2024-01-05 deposited with the CCDC.	2024-06-13 downloaded from the CCDC.
;
_audit_creation_date             2023-09-14
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '0.5(I12 Pb4), C7 H12 N2'
_chemical_formula_sum            'C7 H12 I6 N2 Pb2'
_chemical_formula_weight         1299.97
_chemical_absolute_configuration ad
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C H N I Pb'
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           21
_space_group_name_H-M_alt        'C 2 2 2'
_space_group_name_Hall           'C 2 2'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-x, y, -z'
'x, -y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z'
'-x+1/2, y+1/2, -z'
'x+1/2, -y+1/2, -z'

_cell_length_a                   9.4786(5)
_cell_length_b                   17.7233(10)
_cell_length_c                   6.5033(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1092.50(11)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    5220
_cell_measurement_temperature    425.0(3)
_cell_measurement_theta_max      30.2670
_cell_measurement_theta_min      2.4040
_shelx_estimated_absorpt_T_max   0.199
_shelx_estimated_absorpt_T_min   0.199
_exptl_absorpt_coefficient_mu    23.855
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.06058
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.84a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            ?
_exptl_crystal_density_diffrn    3.952
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1100
_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  0.0753
_diffrn_reflns_av_unetI/netI     0.0451
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.928
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            12319
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.896
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.822
_diffrn_reflns_theta_min         2.298
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      425.0(3)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.928
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     18.00  67.00   0.50    0.80    --    4.67  57.00 -60.00   98
  2  ω    -17.00  18.00   0.50    0.80    --    4.67 -38.00-150.00   70
  3  ω    -58.00 -22.00   0.50    0.80    --    4.67 -38.00-150.00   72
  4  ω    -67.00  18.00   0.50    0.80    --    4.67 -33.00 -98.67  170
  5  ω    -64.00  18.00   0.50    0.80    --    4.67 -38.00 -30.00  164
  6  ω    -63.00  18.00   0.50    0.80    --    4.67 -28.00  48.39  162
  7  ω    -21.00  18.00   0.50    0.80    --    4.67 -24.00  80.44   78
  8  ω    -68.00  17.00   0.50    0.80    --    4.67 -38.00 150.00  170
  9  ω    -67.00  12.00   0.50    0.80    --   -5.45 -77.00 150.00  158
 10  ω    -77.00 -24.00   0.50    0.80    --   -5.45 -57.00  30.00  106
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0241383000
_diffrn_orient_matrix_UB_12      0.0156265000
_diffrn_orient_matrix_UB_13      0.0940798000
_diffrn_orient_matrix_UB_21      0.0079509000
_diffrn_orient_matrix_UB_22      -0.0368282000
_diffrn_orient_matrix_UB_23      0.0410839000
_diffrn_orient_matrix_UB_31      0.0703701000
_diffrn_orient_matrix_UB_32      -0.0011456000
_diffrn_orient_matrix_UB_33      -0.0368695000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_reflns_Friedel_coverage         0.663
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.853
_reflns_number_gt                1149
_reflns_number_total             1553
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.84a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.84a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.84a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         1.319
_refine_diff_density_min         -1.503
_refine_diff_density_rms         0.149
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.36(4)
_refine_ls_extinction_coef       0.00251(17)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     88
_refine_ls_number_reflns         1553
_refine_ls_number_restraints     118
_refine_ls_R_factor_all          0.0557
_refine_ls_R_factor_gt           0.0327
_refine_ls_restrained_S_all      1.027
_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)+(0.0198P)²+5.0050P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0723
_refine_ls_wR_factor_ref         0.0770
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.64474
 0.35526
2. Restrained distances
 N1-C2
 1.37 with sigma of 0.02
 C2-C1
 1.53 with sigma of 0.02
 C2-C3
 1.53 with sigma of 0.02
 N1-C1
 2.2 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(N1) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C3) \\sim
Ueq, Uanis(C7) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(N2) \\sim Ueq, Uanis(C5)
\\sim Ueq, Uanis(C6) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms
of 0.02
Uanis(C3) = Uanis(C7)
4. Rigid body (RIGU) restrains
 N1, N2, C1, C2, C3, C4, C5, C6, C7
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: N1(0.25) H1A(0.25) H1B(0.25) H1C(0.25) C1(0.25) H1D(0.25)
 H1E(0.25) H1F(0.25) C2(0.25) H2(0.25) C7(0.25) H7(0.25) C3(0.25) C4(0.25)
 H4(0.25) C5(0.25) H5(0.25) C6(0.25) H6(0.25) N2(0.25) H2A(0.25)
6.a Ternary CH refined with riding coordinates:
 C2(H2)
6.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C4(H4), C5(H5), C6(H6), N2(H2A)
6.c Fitted hexagon refined as free rotating group:
 C7(C3,C4,C5,C6,N2)
6.d Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C), 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 0.500000 0.36972(3) 1.000000 0.0514(2) Uani 1 2 d S T P . .
I1 I 0.500000 0.36857(7) 0.500000 0.0957(5) Uani 1 2 d S T P . .
I2 I 0.250000 0.250000 0.9912(18) 0.1160(7) Uani 1 2 d S T P . .
I3 I 0.73350(10) 0.500000 1.000000 0.0550(3) Uani 1 2 d S T P . .
N1 N -0.020(8) 0.626(3) 0.703(6) 0.077(14) Uani 0.25 1 d D U P A -1
H1A H -0.061076 0.669098 0.667757 0.093 Uiso 0.25 1 calc R U P A -1
H1B H 0.043563 0.634303 0.800769 0.093 Uiso 0.25 1 calc R U P A -1
H1C H -0.085759 0.594178 0.751187 0.093 Uiso 0.25 1 calc R U P A -1
C1 C -0.047(10) 0.632(5) 0.367(8) 0.096(18) Uani 0.25 1 d D U P A -1
H1D H -0.142653 0.635462 0.414127 0.144 Uiso 0.25 1 calc R U P A -1
H1E H -0.044132 0.602002 0.243322 0.144 Uiso 0.25 1 calc R U P A -1
H1F H -0.011288 0.681405 0.338144 0.144 Uiso 0.25 1 calc R U P A -1
C2 C 0.044(4) 0.5941(15) 0.533(8) 0.058(9) Uani 0.25 1 d D U P A -1
H2 H 0.144740 0.607055 0.522673 0.069 Uiso 0.25 1 calc R U P A -1
C7 C 0.127(2) 0.4584(13) 0.502(16) 0.054(4) Uani 0.25 1 d G U P A -1
H7 H 0.219372 0.476055 0.511367 0.065 Uiso 0.25 1 calc R U P A -1
C3 C 0.015(3) 0.5090(10) 0.505(17) 0.054(4) Uani 0.25 1 d DG U P A -1
C4 C -0.123(2) 0.4827(10) 0.491(13) 0.046(7) Uani 0.25 1 d G U P A -1
H4 H -0.197549 0.516588 0.493089 0.056 Uiso 0.25 1 calc R U P A -1
C5 C -0.1484(17) 0.4058(11) 0.473(7) 0.040(8) Uani 0.25 1 d G U P A -1
H5 H -0.240568 0.388202 0.462926 0.048 Uiso 0.25 1 calc R U P A -1
C6 C -0.0364(18) 0.3552(9) 0.469(5) 0.033(8) Uani 0.25 1 d G U P A -1
H6 H -0.053618 0.303741 0.456983 0.040 Uiso 0.25 1 calc R U P A -1
N2 N 0.1014(17) 0.3815(12) 0.484(10) 0.054(8) Uani 0.25 1 d G U P A -1
H2A H 0.170712 0.350214 0.481382 0.065 Uiso 0.25 1 calc R U P A -1


_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 I1 3.2517(2) . ?
Pb1 I1 3.25171(19) 1_556 ?
Pb1 I2 3.1813(4) . ?
Pb1 I2 3.1813(4) 3_657 ?
Pb1 I3 3.1984(7) 2_665 ?
Pb1 I3 3.1984(7) . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 H1C 0.8900 . ?
N1 C2 1.38(2) . ?
C1 H1D 0.9600 . ?
C1 H1E 0.9600 . ?
C1 H1F 0.9600 . ?
C1 C2 1.54(3) . ?
C2 H2 0.9800 . ?
C2 C3 1.54(2) . ?
C7 H7 0.9300 . ?
C7 C3 1.3900 . ?
C7 N2 1.3900 . ?
C3 C4 1.3900 . ?
C4 H4 0.9300 . ?
C4 C5 1.3900 . ?
C5 H5 0.9300 . ?
C5 C6 1.3900 . ?
C6 H6 0.9300 . ?
C6 N2 1.3900 . ?
N2 H2A 0.8600 . ?

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
I1 Pb1 I1 179.28(5) . 1_556 ?
I2 Pb1 I1 90.8(2) 3_657 . ?
I2 Pb1 I1 90.8(2) . 1_556 ?
I2 Pb1 I1 88.7(2) . . ?
I2 Pb1 I1 88.7(2) 3_657 1_556 ?
I2 Pb1 I2 96.333(16) . 3_657 ?
I2 Pb1 I3 88.055(14) 3_657 . ?
I2 Pb1 I3 175.51(6) 3_657 2_665 ?
I2 Pb1 I3 175.51(6) . . ?
I2 Pb1 I3 88.055(14) . 2_665 ?
I3 Pb1 I1 90.259(17) 2_665 1_556 ?
I3 Pb1 I1 90.259(17) . . ?
I3 Pb1 I1 90.259(17) . 1_556 ?
I3 Pb1 I1 90.259(17) 2_665 . ?
I3 Pb1 I3 87.58(3) 2_665 . ?
Pb1 I1 Pb1 179.28(5) 1_554 . ?
Pb1 I2 Pb1 177.9(4) . 6 ?
Pb1 I3 Pb1 92.42(3) 2_665 . ?
H1A N1 H1B 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1B N1 H1C 109.5 . . ?
C2 N1 H1A 109.5 . . ?
C2 N1 H1B 109.5 . . ?
C2 N1 H1C 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 . . ?
N1 C2 C1 98(2) . . ?
N1 C2 H2 113.2 . . ?
N1 C2 C3 114(5) . . ?
C1 C2 H2 113.2 . . ?
C1 C2 C3 104(5) . . ?
C3 C2 H2 113.2 . . ?
C3 C7 H7 120.0 . . ?
C3 C7 N2 120.0 . . ?
N2 C7 H7 120.0 . . ?
C7 C3 C2 120(2) . . ?
C7 C3 C4 120.0 . . ?
C4 C3 C2 120(2) . . ?
C3 C4 H4 120.0 . . ?
C5 C4 C3 120.0 . . ?
C5 C4 H4 120.0 . . ?
C4 C5 H5 120.0 . . ?
C4 C5 C6 120.0 . . ?
C6 C5 H5 120.0 . . ?
C5 C6 H6 120.0 . . ?
C5 C6 N2 120.0 . . ?
N2 C6 H6 120.0 . . ?
C7 N2 H2A 120.0 . . ?
C6 N2 C7 120.0 . . ?
C6 N2 H2A 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
N1 C2 C3 C7 -121(5) . . . . ?
N1 C2 C3 C4 56(7) . . . . ?
C1 C2 C3 C7 133(5) . . . . ?
C1 C2 C3 C4 -49(7) . . . . ?
C2 C3 C4 C5 -178(8) . . . . ?
C7 C3 C4 C5 0.0 . . . . ?
C3 C7 N2 C6 0.0 . . . . ?
C3 C4 C5 C6 0.0 . . . . ?
C4 C5 C6 N2 0.0 . . . . ?
C5 C6 N2 C7 0.0 . . . . ?
N2 C7 C3 C2 178(8) . . . . ?
N2 C7 C3 C4 0.0 . . . . ?

_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 8.513
_oxdiff_exptl_absorpt_empirical_full_min 0.371
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.64474
2 0.35526

####################################################################### 
# 
# 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_3S-245K
_database_code_depnum_ccdc_archive 'CCDC 2323592'
loop_
_audit_author_name
_audit_author_address
'Changchun Fan'
;southeast university
China
;
_audit_update_record             
;
2024-01-05 deposited with the CCDC.	2024-06-13 downloaded from the CCDC.
;
_audit_creation_date             2024-01-05
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C7 H12 N2, I6 Pb2'
_chemical_formula_sum            'C7 H12 I6 N2 Pb2'
_chemical_formula_weight         1299.97
_chemical_absolute_configuration ad
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C H N I Pb'
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           20
_space_group_name_H-M_alt        'C 2 2 21'
_space_group_name_Hall           'C 2c 2'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'-x, y, -z+1/2'
'x, -y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'

_cell_length_a                   12.9335(6)
_cell_length_b                   18.7349(8)
_cell_length_c                   17.6358(8)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4273.3(3)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    6768
_cell_measurement_temperature    245.03(10)
_cell_measurement_theta_max      30.6550
_cell_measurement_theta_min      2.1820
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    24.395
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.19883
_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            'metallic reddish red'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    4.041
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             4400
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0663
_diffrn_reflns_av_unetI/netI     0.0612
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.839
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            15592
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.794
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.780
_diffrn_reflns_theta_min         1.913
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      245.03(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.839
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω      9.00  35.00   0.50    1.10    --   -6.24  57.00   0.00   52
  2  ω     50.00  76.00   0.50    1.10    --    5.69  38.00 -60.00   52
  3  ω    -69.00  21.00   0.50    1.10    --    5.69 -17.00 -53.00  180
  4  ω    -14.00  24.00   0.50    1.10    --    5.69 -99.00 -90.00   76
  5  ω    -17.00  28.00   0.50    1.10    --   -6.24 -99.00  60.00   90
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0511923000
_diffrn_orient_matrix_UB_12      0.0114719000
_diffrn_orient_matrix_UB_13      -0.0076432000
_diffrn_orient_matrix_UB_21      -0.0156857000
_diffrn_orient_matrix_UB_22      -0.0360305000
_diffrn_orient_matrix_UB_23      -0.0046000000
_diffrn_orient_matrix_UB_31      -0.0118750000
_diffrn_orient_matrix_UB_32      -0.0019960000
_diffrn_orient_matrix_UB_33      0.0392004000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_reflns_Friedel_coverage         0.727
_reflns_Friedel_fraction_full    0.992
_reflns_Friedel_fraction_max     0.740
_reflns_number_gt                3776
_reflns_number_total             5320
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_refine_diff_density_max         4.880
_refine_diff_density_min         -4.819
_refine_diff_density_rms         0.649
_refine_ls_abs_structure_details 
;
 Flack x determined using 1214 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.00(3)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     159
_refine_ls_number_reflns         5320
_refine_ls_number_restraints     37
_refine_ls_R_factor_all          0.0900
_refine_ls_R_factor_gt           0.0684
_refine_ls_restrained_S_all      1.022
_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)+(0.1106P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1748
_refine_ls_wR_factor_ref         0.1865
_refine_special_details          ?
_olex2_refinement_description    
;
1. Restrained distances
 C2-C6
 4.25 with sigma of 0.02
 N2-C3 = N2-C5
 2.34 with sigma of 0.01
 C3-C5
 2.36 with sigma of 0.01
 C6-C7
 2.33 with sigma of 0.01
 C4-N2
 2.74 with sigma of 0.01
 C1-C2
 1.53 with sigma of 0.01
 C2-N1
 1.48 with sigma of 0.01
 C2-C3
 1.49 with sigma of 0.01
 C3-C4 = C5-C4 = C3-C7 = C5-C6
 1.37 with sigma of 0.01
 C7-N2
 1.34 with sigma of 0.01
 C6-N2
 1.34 with sigma of 0.01
 C5-C7
 2.72 with sigma of 0.01
 C3-C6
 2.74 with sigma of 0.01
 C4-C6 = C4-C7
 2.38 with sigma of 0.01
2. Uiso/Uaniso restraints and constraints
Uanis(C5) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3.a Ternary CH refined with riding coordinates:
 C2(H2)
3.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C7(H7), N2(H2A)
3.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), N1(H1D,H1E,H1F)
;
_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
C1 C 0.8447(17) 0.6161(15) 0.3828(13) 0.067(8) Uani 1 1 d D U . . .
H1A H 0.838076 0.624904 0.436782 0.101 Uiso 1 1 calc GR . . . .
H1B H 0.907704 0.638123 0.364238 0.101 Uiso 1 1 calc GR . . . .
H1C H 0.847368 0.565085 0.373675 0.101 Uiso 1 1 calc GR . . . .
C2 C 0.7526(15) 0.6477(12) 0.3417(7) 0.063(7) Uani 1 1 d D . . . .
H2 H 0.753388 0.699957 0.349935 0.075 Uiso 1 1 calc R . . . .
C3 C 0.750(2) 0.6344(7) 0.2575(5) 0.039(5) Uani 1 1 d D . . . .
C4 C 0.751(2) 0.6941(6) 0.2116(8) 0.048(5) Uani 1 1 d D . . . .
H4 H 0.749806 0.740040 0.232918 0.057 Uiso 1 1 calc R . . . .
C5 C 0.754(2) 0.6852(7) 0.1345(8) 0.050(5) Uani 1 1 d D U . . .
H5 H 0.755468 0.725403 0.102568 0.060 Uiso 1 1 calc R . . . .
C6 C 0.756(2) 0.6181(8) 0.1038(6) 0.061(8) Uani 1 1 d D . . . .
H6 H 0.756749 0.612071 0.050925 0.073 Uiso 1 1 calc R . . . .
C7 C 0.752(2) 0.5678(6) 0.2252(7) 0.044(5) Uani 1 1 d D . . . .
H7 H 0.749213 0.526931 0.256100 0.053 Uiso 1 1 calc R . . . .
I1 I 0.500000 0.24532(11) 0.750000 0.0240(5) Uani 1 2 d S T P . .
I2 I 0.500000 0.00914(10) 0.750000 0.0235(5) Uani 1 2 d S T P . .
I3 I 0.5315(2) 0.000000 0.500000 0.0436(8) Uani 1 2 d S T P . .
I4 I 0.74731(14) 0.13404(7) 0.62782(8) 0.0357(4) Uani 1 1 d . . . . .
I5 I 0.5069(3) 0.25714(13) 0.50413(11) 0.0655(7) Uani 1 1 d . . . . .
I6 I 0.500000 0.25683(11) 0.250000 0.0219(5) Uani 1 2 d S T P . .
I7 I 0.500000 0.49846(11) 0.250000 0.0245(4) Uani 1 2 d S T P . .
I8 I 0.4746(3) 0.500000 0.500000 0.0517(9) Uani 1 2 d S T P . .
I9 I 0.74642(16) 0.39343(10) 0.38917(9) 0.0496(4) Uani 1 1 d . . . . .
N1 N 0.6581(18) 0.6190(16) 0.3771(13) 0.113(10) Uani 1 1 d D U . . .
H1D H 0.602208 0.637385 0.353883 0.169 Uiso 1 1 calc GR . . . .
H1E H 0.657010 0.630906 0.426563 0.169 Uiso 1 1 calc GR . . . .
H1F H 0.657482 0.571143 0.372580 0.169 Uiso 1 1 calc GR . . . .
N2 N 0.757(2) 0.5608(6) 0.1497(7) 0.060(6) Uani 1 1 d D . . . .
H2A H 0.761825 0.518329 0.130011 0.072 Uiso 1 1 calc R . . . .
Pb1 Pb 0.49765(5) 0.12431(3) 0.61993(4) 0.0237(3) Uani 1 1 d . . . . .
Pb2 Pb 0.49611(5) 0.37466(3) 0.37821(4) 0.0219(2) Uani 1 1 d . . . . .


_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
C1 C2 1.515(13) . ?
C2 C3 1.507(11) . ?
C2 N1 1.473(13) . ?
C3 C4 1.380(10) . ?
C3 C7 1.372(10) . ?
C4 C5 1.370(10) . ?
C5 C6 1.370(10) . ?
C6 N2 1.344(10) . ?
C7 N2 1.339(10) . ?
I1 Pb1 3.2253(16) 3_656 ?
I1 Pb1 3.2253(16) . ?
I2 Pb1 3.1494(15) . ?
I2 Pb1 3.1495(15) 3_656 ?
I3 Pb1 3.1763(8) . ?
I3 Pb1 3.1763(8) 4_556 ?
I4 Pb1 3.2371(19) . ?
I4 Pb2 3.2237(19) 8_556 ?
I5 Pb1 3.221(2) . ?
I5 Pb2 3.1303(19) . ?
I6 Pb2 3.1604(16) 3_655 ?
I6 Pb2 3.1604(16) . ?
I7 Pb2 3.2395(16) . ?
I7 Pb2 3.2395(16) 3_655 ?
I8 Pb2 3.1945(7) . ?
I8 Pb2 3.1946(7) 4_566 ?
I9 Pb1 3.270(2) 8_556 ?
I9 Pb2 3.262(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C3 C2 C1 115.1(18) . . ?
N1 C2 C1 108(2) . . ?
N1 C2 C3 109.8(18) . . ?
C4 C3 C2 116.4(13) . . ?
C7 C3 C2 124.0(13) . . ?
C7 C3 C4 119.6(7) . . ?
C5 C4 C3 119.0(7) . . ?
C6 C5 C4 120.2(7) . . ?
N2 C6 C5 119.7(7) . . ?
N2 C7 C3 120.1(7) . . ?
Pb1 I1 Pb1 90.68(6) 3_656 . ?
Pb1 I2 Pb1 93.51(6) . 3_656 ?
Pb1 I3 Pb1 164.15(11) . 4_556 ?
Pb2 I4 Pb1 172.48(5) 8_556 . ?
Pb2 I5 Pb1 172.49(12) . . ?
Pb2 I6 Pb2 91.39(5) 3_655 . ?
Pb2 I7 Pb2 88.56(5) . 3_655 ?
Pb2 I8 Pb2 169.99(14) . 4_566 ?
Pb2 I9 Pb1 166.46(7) . 8_556 ?
C7 N2 C6 121.3(7) . . ?
I1 Pb1 I4 85.44(3) . . ?
I1 Pb1 I9 96.64(4) . 8_456 ?
I2 Pb1 I1 87.91(4) . . ?
I2 Pb1 I3 88.93(3) . . ?
I2 Pb1 I4 89.87(3) . . ?
I2 Pb1 I5 172.15(6) . . ?
I2 Pb1 I9 88.61(3) . 8_456 ?
I3 Pb1 I1 170.99(6) . . ?
I3 Pb1 I4 86.12(6) . . ?
I3 Pb1 I5 98.00(5) . . ?
I3 Pb1 I9 91.71(6) . 8_456 ?
I4 Pb1 I9 177.37(4) . 8_456 ?
I5 Pb1 I1 84.69(4) . . ?
I5 Pb1 I4 86.95(8) . . ?
I5 Pb1 I9 94.83(8) . 8_456 ?
I4 Pb2 I7 91.64(3) 8_456 . ?
I4 Pb2 I9 176.38(4) 8_456 . ?
I5 Pb2 I4 91.85(8) . 8_456 ?
I5 Pb2 I6 90.89(5) . . ?
I5 Pb2 I7 176.42(8) . . ?
I5 Pb2 I8 92.52(5) . . ?
I5 Pb2 I9 89.40(8) . . ?
I6 Pb2 I4 87.53(3) . 8_456 ?
I6 Pb2 I7 90.03(4) . . ?
I6 Pb2 I8 174.79(6) . . ?
I6 Pb2 I9 95.85(4) . . ?
I7 Pb2 I9 87.06(3) . . ?
I8 Pb2 I4 88.41(7) . 8_456 ?
I8 Pb2 I7 86.81(3) . . ?
I8 Pb2 I9 88.13(7) . . ?

_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 2.741
_oxdiff_exptl_absorpt_empirical_full_min 0.545
####################################################################### 
# 
# 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_2Rac
_database_code_depnum_ccdc_archive 'CCDC 2323589'
loop_
_audit_author_name
_audit_author_address
'Changchun Fan'
;southeast university
China
;
_audit_update_record             
;
2024-01-05 deposited with the CCDC.	2024-06-13 downloaded from the CCDC.
;
_audit_creation_date             2024-01-05
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'I6 Pb2, 0.5(C14 H24 N4)'
_chemical_formula_sum            'C7 H12 I6 N2 Pb2'
_chemical_formula_weight         1299.97
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C1 H1 N1 Pb1 I1'
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           64
_space_group_name_H-M_alt        'C m c e'
_space_group_name_Hall           '-C 2bc 2'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y+1/2, z+1/2'
'-x, y+1/2, -z+1/2'
'x, -y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1, z+1/2'
'-x+1/2, y+1, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x, y-1/2, -z-1/2'
'x, -y-1/2, z-1/2'
'-x, y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, y, -z-1/2'
'x+1/2, -y, z-1/2'
'-x+1/2, y+1/2, z'

_cell_length_a                   12.9548(6)
_cell_length_b                   18.8648(9)
_cell_length_c                   17.6101(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4303.7(3)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    4263
_cell_measurement_temperature    299.13(10)
_cell_measurement_theta_max      30.7780
_cell_measurement_theta_min      2.1960
_shelx_estimated_absorpt_T_max   0.085
_shelx_estimated_absorpt_T_min   0.085
_exptl_absorpt_coefficient_mu    24.222
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.11415
_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            'metallic reddish red'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    4.013
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             4400
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0394
_diffrn_reflns_av_unetI/netI     0.0380
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.819
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            13562
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.819
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.555
_diffrn_reflns_theta_min         2.159
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      299.13(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.819
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -26.00   6.00   0.50    1.50    --    5.69  94.00  61.00   64
  2  ω    -20.00  44.00   0.50    1.50    --   -6.24  38.00 -60.00  128
  3  ω    -18.00  31.00   0.50    1.50    --    5.69 -99.00-180.00   98
  4  ω    -13.00  32.00   0.50    1.50    --    5.69 -94.00 -49.00   90
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0153755000
_diffrn_orient_matrix_UB_12      -0.0505868000
_diffrn_orient_matrix_UB_13      0.0006706000
_diffrn_orient_matrix_UB_21      -0.0079125000
_diffrn_orient_matrix_UB_22      -0.0054840000
_diffrn_orient_matrix_UB_23      -0.0366875000
_diffrn_orient_matrix_UB_31      0.0363751000
_diffrn_orient_matrix_UB_32      0.0201836000
_diffrn_orient_matrix_UB_33      -0.0082485000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2076
_reflns_number_total             2819
_reflns_odcompleteness_completeness 99.63
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         2.491
_refine_diff_density_min         -4.696
_refine_diff_density_rms         0.325
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     96
_refine_ls_number_reflns         2819
_refine_ls_number_restraints     66
_refine_ls_R_factor_all          0.0762
_refine_ls_R_factor_gt           0.0517
_refine_ls_restrained_S_all      1.048
_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)+(0.0321P)²+157.0801P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1058
_refine_ls_wR_factor_ref         0.1151
_refine_special_details          ?
_olex2_refinement_description    
;
1. Shared sites
{C1, N1}
2. Restrained distances
 C2-N1
 1.51 with sigma of 0.01
 C1-C2
 1.51 with sigma of 0.01
 C2-C3
 1.51 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C1) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C2) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C1) = Uanis(N1)
4. Rigid body (RIGU) restrains
 C4, C5, C6, C7, N2, C3, C2, N1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: C1(0.5) H1A(0.5) H1B(0.5) H1C(0.5) N1(0.5) H1D(0.5) H1E(0.5)
 H1F(0.5)
6.a Riding coordinates:
 C1(H1A,H1B,H1C), N1(H1D,H1E,H1F)
6.b Aromatic/amide H refined with riding coordinates:
 N2(H2), C7(H7), C5(H5), C6(H6), C4(H4)
;
_atom_sites_solution_hydrogens   mixed
_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 0.25405(3) 0.37595(2) 0.61993(2) 0.03606(14) Uani 1 1 d . . . . .
I4 I 0.28522(10) 0.500000 0.500000 0.0558(3) Uani 1 2 d S T P . .
I1 I 0.250000 0.49376(5) 0.750000 0.0387(2) Uani 1 2 d S T P . .
I5 I 0.000000 0.40201(7) 0.60550(7) 0.0514(3) Uani 1 2 d S T P . .
I2 I 0.250000 0.25778(5) 0.750000 0.0389(2) Uani 1 2 d S T P . .
I6 I 0.250000 0.250000 0.500000 0.1171(8) Uani 1 2 d S . P . .
I3 I 0.500000 0.35982(6) 0.63685(7) 0.0467(3) Uani 1 2 d S T P . .
N2 N 0.000000 0.1919(8) 0.7241(9) 0.053(3) Uani 1 2 d S T P . .
H2 H 0.000000 0.230321 0.750465 0.064 Uiso 1 2 calc R U P . .
C7 C 0.000000 0.1942(10) 0.6466(12) 0.060(4) Uani 1 2 d S T P . .
H7 H 0.000000 0.237507 0.621452 0.072 Uiso 1 2 calc R U P . .
C5 C 0.000000 0.0706(11) 0.6430(12) 0.060(4) Uani 1 2 d S T P A .
H5 H 0.000000 0.028673 0.615222 0.072 Uiso 1 2 calc R U P . .
C2 C 0.000000 0.1341(16) 0.8439(10) 0.102(6) Uani 1 2 d DS TU P . .
H2A H 0.000000 0.176(14) 0.884(14) 0.123 Uiso 1 2 d S U P . .
C6 C 0.000000 0.1334(10) 0.6070(11) 0.053(4) Uani 1 2 d S T P . .
H6 H 0.000000 0.134781 0.554191 0.064 Uiso 1 2 calc R U P . .
C3 C 0.000000 0.1271(10) 0.7588(10) 0.055(3) Uani 1 2 d DS T P A .
C4 C 0.000000 0.0686(10) 0.7179(11) 0.054(4) Uani 1 2 d S T P . .
H4 H 0.000000 0.024915 0.742390 0.065 Uiso 1 2 calc R U P A .
C1 C 0.0983(11) 0.1153(8) 0.8836(9) 0.096(5) Uani 0.5 1 d D U P A 9
H1A H 0.154789 0.135980 0.856163 0.144 Uiso 0.5 1 d R U P A 9
H1B H 0.107169 0.064820 0.885963 0.144 Uiso 0.5 1 d R U P A 9
H1C H 0.096609 0.134290 0.934203 0.144 Uiso 0.5 1 d R U P A 9
N1 N 0.0983(11) 0.1153(8) 0.8836(9) 0.096(5) Uani 0.5 1 d D . P A 10
H1D H 0.130999 0.155400 0.895073 0.115 Uiso 0.5 1 d R U P A 10
H1E H 0.137909 0.089110 0.853323 0.115 Uiso 0.5 1 d R U P A 10
H1F H 0.085049 0.091360 0.926083 0.115 Uiso 0.5 1 d R U P A 10


_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 I4 3.1780(4) . ?
Pb1 I1 3.1921(8) . ?
Pb1 I5 3.3374(5) . ?
Pb1 I2 3.1967(8) . ?
Pb1 I6 3.1793(4) . ?
Pb1 I3 3.2146(5) . ?
N2 H2 0.8600 . ?
N2 C7 1.37(2) . ?
N2 C3 1.37(2) . ?
C7 H7 0.9300 . ?
C7 C6 1.34(3) . ?
C5 H5 0.9300 . ?
C5 C6 1.34(3) . ?
C5 C4 1.32(3) . ?
C2 H2A 1.1(3) . ?
C2 C3 1.504(10) . ?
C2 C1 1.497(7) . ?
C2 C1 1.496(7) 12 ?
C2 N1 1.497(7) . ?
C6 H6 0.9300 . ?
C3 C4 1.32(2) . ?
C4 H4 0.9300 . ?
C1 H1A 0.9601 . ?
C1 H1B 0.9599 . ?
C1 H1C 0.9601 . ?
N1 H1D 0.8901 . ?
N1 H1E 0.8900 . ?
N1 H1F 0.8899 . ?

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 Pb1 I1 88.065(16) . . ?
I4 Pb1 I5 88.06(3) . . ?
I4 Pb1 I2 172.64(3) . . ?
I4 Pb1 I6 96.372(10) . . ?
I4 Pb1 I3 90.31(3) . . ?
I1 Pb1 I5 86.32(2) . . ?
I1 Pb1 I2 88.34(2) . . ?
I1 Pb1 I3 90.90(2) . . ?
I2 Pb1 I5 98.11(3) . . ?
I2 Pb1 I3 83.33(2) . . ?
I6 Pb1 I1 175.367(18) . . ?
I6 Pb1 I5 92.48(2) . . ?
I6 Pb1 I2 87.397(17) . . ?
I6 Pb1 I3 90.41(2) . . ?
I3 Pb1 I5 176.82(3) . . ?
Pb1 I4 Pb1 165.40(5) . 4_566 ?
Pb1 I1 Pb1 91.74(3) . 7_546 ?
Pb1 I5 Pb1 160.91(5) . 12 ?
Pb1 I2 Pb1 91.58(3) 7_546 . ?
Pb1 I6 Pb1 180.000(16) 13_556 . ?
Pb1 I3 Pb1 164.77(4) 12_655 . ?
C7 N2 H2 120.9 . . ?
C7 N2 C3 118.3(15) . . ?
C3 N2 H2 120.9 . . ?
N2 C7 H7 120.2 . . ?
C6 C7 N2 119.6(18) . . ?
C6 C7 H7 120.2 . . ?
C6 C5 H5 120.1 . . ?
C4 C5 H5 120.1 . . ?
C4 C5 C6 120(2) . . ?
C3 C2 H2A 137(10) . . ?
C1 C2 H2A 82(7) 12 . ?
C1 C2 H2A 82(7) . . ?
C1 C2 C3 116.4(12) 12 . ?
C1 C2 C3 116.4(12) . . ?
C1 C2 C1 117(2) 12 . ?
N1 C2 H2A 82(7) . . ?
N1 C2 C3 116.4(12) . . ?
C7 C6 C5 120(2) . . ?
C7 C6 H6 119.8 . . ?
C5 C6 H6 119.7 . . ?
N2 C3 C2 111.4(18) . . ?
C4 C3 N2 120.4(17) . . ?
C4 C3 C2 128(2) . . ?
C5 C4 H4 119.2 . . ?
C3 C4 C5 121.5(19) . . ?
C3 C4 H4 119.2 . . ?
C2 C1 H1A 108.4 . . ?
C2 C1 H1B 110.9 . . ?
C2 C1 H1C 109.0 . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C2 N1 H1D 108.0 . . ?
C2 N1 H1E 110.0 . . ?
C2 N1 H1F 110.4 . . ?
H1D N1 H1E 109.5 . . ?
H1D N1 H1F 109.5 . . ?
H1E N1 H1F 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
N2 C7 C6 C5 0.000(7) . . . . ?
N2 C3 C4 C5 0.000(6) . . . . ?
C7 N2 C3 C2 180.000(6) . . . . ?
C7 N2 C3 C4 0.000(6) . . . . ?
C2 C3 C4 C5 180.000(6) . . . . ?
C6 C5 C4 C3 0.000(6) . . . . ?
C3 N2 C7 C6 0.000(6) . . . . ?
C4 C5 C6 C7 0.000(6) . . . . ?
C1 C2 C3 N2 108(2) 12 . . . ?
C1 C2 C3 N2 -108(2) . . . . ?
C1 C2 C3 C4 72(2) . . . . ?
C1 C2 C3 C4 -72(2) 12 . . . ?
N1 C2 C3 N2 -108(2) . . . . ?
N1 C2 C3 C4 72(2) . . . . ?

# end Validation Reply Form
_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 3.736
_oxdiff_exptl_absorpt_empirical_full_min 0.443
_vrf_PLAT342_2Rac                
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............       0.03 Ang.  
RESPONSE: Organic cation in this structure inherently exhibit higher 
thermal parameters, which consequently lower the precision of 
the C-C bonds.
;
# start Validation Reply Form
_vrf_PLAT972_2Rac                
;
PROBLEM: Check Calcd Resid. Dens.  0.00Ang From I6             -4.69 eA-3  
RESPONSE: This is caused by the heavy atomic effect of iodine
;
####################################################################### 
# 
# 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_3R-298K
_database_code_depnum_ccdc_archive 'CCDC 2323596'
loop_
_audit_author_name
_audit_author_address
'Changchun Fan'
;southeast university
China
;
_audit_update_record             
;
2024-01-05 deposited with the CCDC.	2024-06-13 downloaded from the CCDC.
;
_audit_creation_date             2024-01-05
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'I6 Pb2, C7 H12 N2'
_chemical_formula_sum            'C7 H12 I6 N2 Pb2'
_chemical_formula_weight         1299.97
_chemical_absolute_configuration ad
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C H N I Pb'
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           20
_space_group_name_H-M_alt        'C 2 2 21'
_space_group_name_Hall           'C 2c 2'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'-x, y, -z+1/2'
'x, -y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'

_cell_length_a                   12.9629(3)
_cell_length_b                   18.7955(5)
_cell_length_c                   17.6714(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4305.53(19)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    16647
_cell_measurement_temperature    297.98(10)
_cell_measurement_theta_max      30.4920
_cell_measurement_theta_min      2.4300
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    24.212
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.27583
_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            'metallic pinkish red'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   pinkish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    4.011
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             4400
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0746
_diffrn_reflns_av_unetI/netI     0.0412
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.925
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            59812
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.897
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.914
_diffrn_reflns_theta_min         1.908
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      297.98(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.925
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -68.00 -42.00   0.50    0.25    --    5.69 -38.00  30.00   52
  2  ω    -58.00  20.00   0.50    0.25    --    5.69 -38.00  90.00  156
  3  ω    -32.00  20.00   0.50    0.25    --    5.69 -38.00  30.00  104
  4  ω    -65.00  20.00   0.50    0.25    --    5.69 -29.00 -13.03  170
  5  ω    -68.00  20.00   0.50    0.25    --    5.69 -38.00-180.00  176
  6  ω     -6.00  79.00   0.50    0.25    --    5.69  77.00-180.00  170
  7  ω    -22.00  10.00   0.50    0.25    --   -6.24  30.00-144.33   64
  8  ω     -5.00  40.00   0.50    0.25    --    5.69 -99.00-180.00   90
  9  ω     28.00  69.00   0.50    0.25    --   -6.24  30.00-144.33   82
 10  ω    -22.00  69.00   0.50    0.25    --   -6.24  31.00 -73.99  182
 11  ω    -75.00   9.00   0.50    0.25    --   -6.24 -38.00-120.00  168
 12  ω    -18.00  26.00   0.50    0.25    --   -6.24 -99.00  30.00   88
 13  ω    -18.00  28.00   0.50    0.25    --   -6.24 -99.00 120.00   92
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0241828000
_diffrn_orient_matrix_UB_12      0.0143535000
_diffrn_orient_matrix_UB_13      -0.0326099000
_diffrn_orient_matrix_UB_21      0.0188808000
_diffrn_orient_matrix_UB_22      -0.0342734000
_diffrn_orient_matrix_UB_23      -0.0095203000
_diffrn_orient_matrix_UB_31      -0.0452985000
_diffrn_orient_matrix_UB_32      -0.0066250000
_diffrn_orient_matrix_UB_33      -0.0213720000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_reflns_Friedel_coverage         0.772
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.863
_reflns_number_gt                4234
_reflns_number_total             6128
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         3.013
_refine_diff_density_min         -5.375
_refine_diff_density_rms         0.501
_refine_ls_abs_structure_details 
;
 Flack x determined using 1543 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.019(18)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.991
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     179
_refine_ls_number_reflns         6128
_refine_ls_number_restraints     100
_refine_ls_R_factor_all          0.0767
_refine_ls_R_factor_gt           0.0488
_refine_ls_restrained_S_all      0.991
_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)+(0.0928P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1343
_refine_ls_wR_factor_ref         0.1492
_refine_special_details          ?
_olex2_refinement_description    
;
1. Restrained distances
 C2-C1A = C2-C1B
 1.53 with sigma of 0.02
 N1A-C2 = N1B-C2
 1.47 with sigma of 0.02
2. Uiso/Uaniso restraints and constraints
N1B: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08 within
1.7A
Uanis(C2) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N1A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C1A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C1B) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N1B) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3. Rigid body (RIGU) restrains
 N2, C3, C4, C5, C6, C7
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C7, N2, C5, C4, C6, C3, C2, C1B, N1A, N1B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Fixed Sof: N1A(0.5) H1AA(0.5) H1AB(0.5) H1AC(0.5) C1A(0.5) H1AD(0.5)
 H1AE(0.5) H1AF(0.5) N1B(0.5) H1BA(0.5) H1BB(0.5) H1BC(0.5) C1B(0.5) H1BD(0.5)
 H1BE(0.5) H1BF(0.5)
5.a Ternary CH refined with riding coordinates:
 C2(H2A)
5.b Aromatic/amide H refined with riding coordinates:
 N2(H2), C4(H4), C5(H5), C6(H6), C7(H7)
5.c Idealised Me refined as rotating group:
 N1A(H1AA,H1AB,H1AC), C1A(H1AD,H1AE,H1AF), N1B(H1BA,H1BB,H1BC), C1B(H1BD,H1BE,
 H1BF)
;
_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 0.50112(3) 0.12466(2) 0.61979(3) 0.02951(18) Uani 1 1 d . . . . .
Pb2 Pb 0.50333(3) 0.37497(2) 0.37868(3) 0.02803(18) Uani 1 1 d . . . . .
I1 I 0.500000 0.00914(8) 0.750000 0.0308(3) Uani 1 2 d S T P . .
I2 I 0.47078(17) 0.000000 0.500000 0.0557(5) Uani 1 2 d S T P . .
I3 I 0.75273(9) 0.10889(7) 0.61095(6) 0.0584(3) Uani 1 1 d . . . . .
I4 I 0.25164(9) 0.13405(5) 0.62691(5) 0.0436(3) Uani 1 1 d . . . . .
I5 I 0.500000 0.24432(8) 0.750000 0.0308(3) Uani 1 2 d S T P . .
I6 I 0.4965(2) 0.25463(10) 0.50270(9) 0.0788(5) Uani 1 1 d . . . . .
I7 I 0.500000 0.25722(8) 0.250000 0.0291(3) Uani 1 2 d S T P . .
I8 I 0.5242(2) 0.500000 0.500000 0.0627(6) Uani 1 2 d S T P . .
I9 I 0.500000 0.49688(8) 0.250000 0.0305(3) Uani 1 2 d S T P . .
N2 N 0.7564(14) 0.4388(8) 0.6481(7) 0.076(4) Uani 1 1 d . . . . .
H2 H 0.760651 0.479988 0.627060 0.091 Uiso 1 1 calc R U . . .
C2 C 0.7499(12) 0.3575(10) 0.8442(10) 0.081(4) Uani 1 1 d D U . . .
H2A H 0.749759 0.306485 0.855716 0.097 Uiso 1 1 calc R U . A 1
C3 C 0.7499(12) 0.3685(6) 0.7570(7) 0.045(3) Uani 1 1 d . . . . .
C4 C 0.7495(13) 0.3083(7) 0.7133(8) 0.057(3) Uani 1 1 d . . . . .
H4 H 0.748592 0.263710 0.736158 0.069 Uiso 1 1 calc R U . . .
C5 C 0.7502(16) 0.3134(9) 0.6364(9) 0.069(4) Uani 1 1 d . . . . .
H5 H 0.747293 0.273191 0.605820 0.083 Uiso 1 1 calc R U . . .
C6 C 0.7554(14) 0.3796(10) 0.6066(11) 0.079(5) Uani 1 1 d . . . . .
H6 H 0.758453 0.384045 0.554228 0.095 Uiso 1 1 calc R U . . .
C7 C 0.7507(14) 0.4323(8) 0.7239(8) 0.056(3) Uani 1 1 d . . . . .
H7 H 0.747145 0.473003 0.753704 0.067 Uiso 1 1 calc R U . . .
N1A N 0.667(2) 0.391(2) 0.883(2) 0.079(11) Uani 0.5 1 d D U P B 1
H1AA H 0.607377 0.376800 0.862615 0.095 Uiso 0.5 1 calc R U P B 1
H1AB H 0.672589 0.438060 0.877794 0.095 Uiso 0.5 1 calc R U P B 1
H1AC H 0.668754 0.379462 0.931382 0.095 Uiso 0.5 1 calc R U P B 1
C1A C 0.850(3) 0.390(2) 0.870(3) 0.067(12) Uani 0.5 1 d D U P B 1
H1AD H 0.905404 0.373161 0.838632 0.101 Uiso 0.5 1 calc R U P B 1
H1AE H 0.863157 0.376819 0.921664 0.101 Uiso 0.5 1 calc R U P B 1
H1AF H 0.845890 0.440931 0.866351 0.101 Uiso 0.5 1 calc R U P B 1
N1B N 0.836(3) 0.373(3) 0.891(2) 0.094(13) Uani 0.5 1 d D U P B 2
H1BA H 0.855933 0.417586 0.883003 0.112 Uiso 0.5 1 calc R U P B 2
H1BB H 0.887469 0.343464 0.879312 0.112 Uiso 0.5 1 calc R U P B 2
H1BC H 0.818568 0.367224 0.939069 0.112 Uiso 0.5 1 calc R U P B 2
C1B C 0.643(2) 0.366(2) 0.872(2) 0.057(8) Uani 0.5 1 d D U P B 2
H1BD H 0.617115 0.411312 0.856935 0.085 Uiso 0.5 1 calc R U P B 2
H1BE H 0.642938 0.362480 0.926315 0.085 Uiso 0.5 1 calc R U P B 2
H1BF H 0.600885 0.328833 0.851231 0.085 Uiso 0.5 1 calc R U P B 2


_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 I1 3.1638(11) . ?
Pb1 I2 3.1821(6) . ?
Pb1 I3 3.2788(13) . ?
Pb1 I4 3.2412(12) . ?
Pb1 I5 3.2176(11) . ?
Pb1 I6 3.2020(15) . ?
Pb2 I3 3.2678(12) 8_456 ?
Pb2 I4 3.2247(12) 8_556 ?
Pb2 I6 3.1507(14) . ?
Pb2 I7 3.1735(11) . ?
Pb2 I8 3.1925(5) . ?
Pb2 I9 3.2284(12) . ?
N2 H2 0.8600 . ?
N2 C6 1.33(2) . ?
N2 C7 1.348(19) . ?
C2 H2A 0.9800 . ?
C2 C3 1.554(19) . ?
C2 N1A 1.42(2) . ?
C2 C1A 1.51(2) . ?
C2 N1B 1.42(2) . ?
C2 C1B 1.47(2) . ?
C3 C4 1.371(16) . ?
C3 C7 1.335(16) . ?
C4 H4 0.9300 . ?
C4 C5 1.36(2) . ?
C5 H5 0.9300 . ?
C5 C6 1.35(2) . ?
C6 H6 0.9300 . ?
C7 H7 0.9300 . ?
N1A H1AA 0.8900 . ?
N1A H1AB 0.8900 . ?
N1A H1AC 0.8900 . ?
C1A H1AD 0.9600 . ?
C1A H1AE 0.9600 . ?
C1A H1AF 0.9600 . ?
N1B H1BA 0.8900 . ?
N1B H1BB 0.8900 . ?
N1B H1BC 0.8900 . ?
C1B H1BD 0.9600 . ?
C1B H1BE 0.9600 . ?
C1B H1BF 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
I1 Pb1 I2 88.73(2) . . ?
I1 Pb1 I3 88.69(2) . . ?
I1 Pb1 I4 90.260(18) . . ?
I1 Pb1 I5 87.68(3) . . ?
I1 Pb1 I6 173.47(4) . . ?
I2 Pb1 I3 91.41(4) . . ?
I2 Pb1 I4 86.71(4) . . ?
I2 Pb1 I5 171.83(4) . . ?
I2 Pb1 I6 97.44(4) . . ?
I4 Pb1 I3 177.87(3) . . ?
I5 Pb1 I3 95.84(3) . . ?
I5 Pb1 I4 85.967(19) . . ?
I6 Pb1 I3 93.26(5) . . ?
I6 Pb1 I4 87.98(5) . . ?
I6 Pb1 I5 85.92(3) . . ?
I4 Pb2 I3 177.26(3) 8_556 8_456 ?
I4 Pb2 I9 91.668(19) 8_556 . ?
I6 Pb2 I3 89.97(6) . 8_456 ?
I6 Pb2 I4 90.67(5) . 8_556 ?
I6 Pb2 I7 89.85(3) . . ?
I6 Pb2 I8 93.65(4) . . ?
I6 Pb2 I9 177.52(5) . . ?
I7 Pb2 I3 95.25(3) . 8_456 ?
I7 Pb2 I4 87.420(19) . 8_556 ?
I7 Pb2 I8 174.69(4) . . ?
I7 Pb2 I9 89.43(3) . . ?
I8 Pb2 I3 88.75(5) . 8_456 ?
I8 Pb2 I4 88.55(5) . 8_556 ?
I8 Pb2 I9 87.23(2) . . ?
I9 Pb2 I3 87.73(2) . 8_456 ?
Pb1 I1 Pb1 93.33(4) 3_656 . ?
Pb1 I2 Pb1 165.80(8) 4_556 . ?
Pb2 I3 Pb1 167.91(5) 8_556 . ?
Pb2 I4 Pb1 172.68(3) 8_456 . ?
Pb1 I5 Pb1 91.31(4) . 3_656 ?
Pb2 I6 Pb1 175.31(8) . . ?
Pb2 I7 Pb2 91.56(4) 3_655 . ?
Pb2 I8 Pb2 170.27(9) . 4_566 ?
Pb2 I9 Pb2 89.57(4) 3_655 . ?
C6 N2 H2 121.0 . . ?
C6 N2 C7 118.1(15) . . ?
C7 N2 H2 121.0 . . ?
C3 C2 H2A 109.6 . . ?
N1A C2 H2A 109.6 . . ?
N1A C2 C3 115(2) . . ?
N1A C2 C1A 109(3) . . ?
C1A C2 H2A 109.6 . . ?
C1A C2 C3 104(2) . . ?
N1B C2 C3 123(2) . . ?
N1B C2 C1B 122(3) . . ?
C1B C2 C3 109(2) . . ?
C4 C3 C2 116.7(13) . . ?
C7 C3 C2 123.6(13) . . ?
C7 C3 C4 119.6(14) . . ?
C3 C4 H4 119.8 . . ?
C5 C4 C3 120.3(14) . . ?
C5 C4 H4 119.8 . . ?
C4 C5 H5 121.5 . . ?
C6 C5 C4 117.0(15) . . ?
C6 C5 H5 121.5 . . ?
N2 C6 C5 123.7(18) . . ?
N2 C6 H6 118.2 . . ?
C5 C6 H6 118.2 . . ?
N2 C7 H7 119.4 . . ?
C3 C7 N2 121.2(15) . . ?
C3 C7 H7 119.4 . . ?
C2 N1A H1AA 109.5 . . ?
C2 N1A H1AB 109.5 . . ?
C2 N1A H1AC 109.5 . . ?
H1AA N1A H1AB 109.5 . . ?
H1AA N1A H1AC 109.5 . . ?
H1AB N1A H1AC 109.5 . . ?
C2 C1A H1AD 109.5 . . ?
C2 C1A H1AE 109.5 . . ?
C2 C1A H1AF 109.5 . . ?
H1AD C1A H1AE 109.5 . . ?
H1AD C1A H1AF 109.5 . . ?
H1AE C1A H1AF 109.5 . . ?
C2 N1B H1BA 109.5 . . ?
C2 N1B H1BB 109.5 . . ?
C2 N1B H1BC 109.5 . . ?
H1BA N1B H1BB 109.5 . . ?
H1BA N1B H1BC 109.5 . . ?
H1BB N1B H1BC 109.5 . . ?
C2 C1B H1BD 109.5 . . ?
C2 C1B H1BE 109.5 . . ?
C2 C1B H1BF 109.5 . . ?
H1BD C1B H1BE 109.5 . . ?
H1BD C1B H1BF 109.5 . . ?
H1BE C1B H1BF 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
C2 C3 C4 C5 -179.5(19) . . . . ?
C2 C3 C7 N2 176.3(18) . . . . ?
C3 C4 C5 C6 2(3) . . . . ?
C4 C3 C7 N2 -4(3) . . . . ?
C4 C5 C6 N2 -2(3) . . . . ?
C6 N2 C7 C3 4(3) . . . . ?
C7 N2 C6 C5 -1(3) . . . . ?
C7 C3 C4 C5 0(2) . . . . ?
N1A C2 C3 C4 -123(2) . . . . ?
N1A C2 C3 C7 57(3) . . . . ?
C1A C2 C3 C4 117(3) . . . . ?
C1A C2 C3 C7 -62(3) . . . . ?
N1B C2 C3 C4 110(3) . . . . ?
N1B C2 C3 C7 -70(4) . . . . ?
C1B C2 C3 C4 -99(2) . . . . ?
C1B C2 C3 C7 81(3) . . . . ?

# end Validation Reply Form
_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 2.286
_oxdiff_exptl_absorpt_empirical_full_min 0.569
# start Validation Reply Form
_vrf_PLAT342_3R-298K             
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.0214 Ang.  
RESPONSE: The high thermal parameters of organic cations reduce the 
precision of C-C bonds
;
