# Supplementary Information (SI) for Journal of Materials Chemistry A.
# This journal is © The Royal Society of Chemistry 2026

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

data_DMBA_pbi
_database_code_depnum_ccdc_archive 'CCDC 2490415'
loop_
_audit_author_name
_audit_author_address
'Migon Choi'
;Duke University
United States of America
;
_audit_update_record             
;
2025-09-22 deposited with the CCDC.	2026-04-01 downloaded from the CCDC.
;
_audit_creation_date             2024-01-31
_audit_creation_method           
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        (DMeBA)2PbI4_298K
_chemical_formula_moiety         'I4 Pb, 2(C6 H16 N)'
_chemical_formula_sum            'C12 H32 I4 N2 Pb'
_chemical_formula_weight         919.18
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Pb I N C'
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      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   34.2229(19)
_cell_length_b                   8.4548(3)
_cell_length_c                   8.8239(3)
_cell_angle_alpha                90
_cell_angle_beta                 90.303(4)
_cell_angle_gamma                90
_cell_volume                     2553.14(19)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    3532
_cell_measurement_temperature    296.8(4)
_cell_measurement_theta_max      28.1510
_cell_measurement_theta_min      2.9920
_shelx_estimated_absorpt_T_max   0.945
_shelx_estimated_absorpt_T_min   0.725
_exptl_absorpt_coefficient_mu    11.440
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.61006
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear yellowish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.391
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1648
_exptl_crystal_preparation       ?
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.005
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0355
_diffrn_reflns_av_unetI/netI     0.0296
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_h_min       -42
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            10227
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.370
_diffrn_reflns_theta_min         2.381
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      296.8(4)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     -8.00  78.00   0.50   80.00    --    5.03  39.00  -9.00  172
  2  ω    -10.00  41.00   0.50   80.00    --   -6.28  82.00 150.00  102
  3  ω    -22.00  25.00   0.50   80.00    --   -6.28 -99.00 -60.00   94
  4  ω    -21.00  27.00   0.50   80.00    --   -6.28 -99.00-180.00   96
  5  ω     -1.00  27.00   0.50   80.00    --   -6.28 -99.00  90.00   56
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  
'XtaLAB Synergy, Single source at offset/far, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0207210000
_diffrn_orient_matrix_UB_12      -0.0004176000
_diffrn_orient_matrix_UB_13      0.0026465000
_diffrn_orient_matrix_UB_21      0.0002077000
_diffrn_orient_matrix_UB_22      -0.0730750000
_diffrn_orient_matrix_UB_23      -0.0394601000
_diffrn_orient_matrix_UB_31      0.0005402000
_diffrn_orient_matrix_UB_32      0.0411956000
_diffrn_orient_matrix_UB_33      -0.0699866000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2171
_reflns_number_total             2599
_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 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_refine_diff_density_max         1.961
_refine_diff_density_min         -1.206
_refine_diff_density_rms         0.172
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     56
_refine_ls_number_reflns         2599
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0463
_refine_ls_R_factor_gt           0.0363
_refine_ls_restrained_S_all      1.037
_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)+(0.0573P)²+7.8881P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0923
_refine_ls_wR_factor_ref         0.0971
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C5) = Uanis(C3) = Uanis(C6) = Uanis(C4) = Uanis(C1) = Uanis(C2) =
Uanis(N4)
3.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B)
3.b Idealised Me refined as rotating group:
 N4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C4(H4D,H4E,H4F)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.250000 0.250000 0.000000 0.04096(14) Uani 1 2 d S . P . .
I2 I 0.26445(2) 0.06324(6) 0.30872(5) 0.05841(18) Uani 1 1 d . . . . .
I3 I 0.15734(2) 0.19848(8) 0.01540(7) 0.06788(19) Uani 1 1 d . . . . .
C1 C 0.1005(4) 0.2369(15) 0.4426(17) 0.1007(14) Uani 1 1 d . . . . .
H1A H 0.101824 0.125472 0.416841 0.121 Uiso 1 1 calc R U . . .
H1B H 0.097602 0.295460 0.348698 0.121 Uiso 1 1 calc R U . . .
C2 C 0.1371(4) 0.2822(16) 0.5131(16) 0.1007(14) Uani 1 1 d . . . . .
H2A H 0.138073 0.239643 0.615137 0.121 Uiso 1 1 calc R U . . .
H2B H 0.138229 0.396537 0.520367 0.121 Uiso 1 1 calc R U . . .
C3 C 0.0638(4) 0.2645(15) 0.5395(18) 0.1007(14) Uani 1 1 d . . . . .
N4 N 0.1711(3) 0.2252(12) 0.4281(13) 0.1007(14) Uani 1 1 d . . . . .
H4A H 0.167722 0.245752 0.329960 0.121 Uiso 1 1 calc R U . . .
H4B H 0.173660 0.121382 0.441425 0.121 Uiso 1 1 calc R U . . .
H4C H 0.192524 0.274028 0.461396 0.121 Uiso 1 1 calc R U . . .
C5 C 0.0604(3) 0.4270(16) 0.5935(15) 0.1007(14) Uani 1 1 d . . . . .
H5A H 0.074572 0.438219 0.687071 0.151 Uiso 1 1 calc R U . . .
H5B H 0.033371 0.451947 0.609702 0.151 Uiso 1 1 calc R U . . .
H5C H 0.071023 0.497817 0.519328 0.151 Uiso 1 1 calc R U . . .
C6 C 0.0636(3) 0.1559(17) 0.6745(14) 0.1007(14) Uani 1 1 d . . . . .
H6A H 0.068835 0.049678 0.642011 0.151 Uiso 1 1 calc R U . . .
H6B H 0.038448 0.159905 0.722139 0.151 Uiso 1 1 calc R U . . .
H6C H 0.083328 0.188833 0.745393 0.151 Uiso 1 1 calc R U . . .
C4 C 0.0282(4) 0.2290(15) 0.4435(17) 0.1007(14) Uani 1 1 d . . . . .
H4D H 0.020136 0.323238 0.391338 0.151 Uiso 1 1 calc R U . . .
H4E H 0.007407 0.192709 0.507199 0.151 Uiso 1 1 calc R U . . .
H4F H 0.034483 0.148489 0.370857 0.151 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 I2 3.1806(5) 6 ?
Pb1 I2 3.1850(4) . ?
Pb1 I2 3.1806(5) 4 ?
Pb1 I2 3.1850(4) 7 ?
Pb1 I3 3.2045(6) 7 ?
Pb1 I3 3.2045(6) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C1 C2 1.446(18) . ?
C1 C3 1.541(19) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C2 N4 1.470(15) . ?
C3 C5 1.459(16) . ?
C3 C6 1.504(19) . ?
C3 C4 1.509(19) . ?
N4 H4A 0.8900 . ?
N4 H4B 0.8900 . ?
N4 H4C 0.8900 . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
C4 H4D 0.9600 . ?
C4 H4E 0.9600 . ?
C4 H4F 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
I2 Pb1 I2 180.00(2) 6 4 ?
I2 Pb1 I2 90.986(5) 4 7 ?
I2 Pb1 I2 89.014(5) 6 7 ?
I2 Pb1 I2 90.985(5) 6 . ?
I2 Pb1 I2 89.015(5) 4 . ?
I2 Pb1 I2 180.0 . 7 ?
I2 Pb1 I3 92.609(16) . . ?
I2 Pb1 I3 93.782(16) 6 . ?
I2 Pb1 I3 92.609(16) 7 7 ?
I2 Pb1 I3 93.781(16) 4 7 ?
I2 Pb1 I3 86.218(16) 4 . ?
I2 Pb1 I3 87.391(16) . 7 ?
I2 Pb1 I3 87.391(16) 7 . ?
I2 Pb1 I3 86.219(16) 6 7 ?
I3 Pb1 I3 180.0 7 . ?
Pb1 I2 Pb1 147.440(19) 4_545 . ?
H1A C1 H1B 107.5 . . ?
C2 C1 H1A 108.4 . . ?
C2 C1 H1B 108.4 . . ?
C2 C1 C3 115.3(13) . . ?
C3 C1 H1A 108.4 . . ?
C3 C1 H1B 108.4 . . ?
C1 C2 H2A 109.1 . . ?
C1 C2 H2B 109.1 . . ?
C1 C2 N4 112.3(11) . . ?
H2A C2 H2B 107.9 . . ?
N4 C2 H2A 109.1 . . ?
N4 C2 H2B 109.1 . . ?
C5 C3 C1 113.0(11) . . ?
C5 C3 C6 108.4(12) . . ?
C5 C3 C4 107.8(11) . . ?
C6 C3 C1 110.7(11) . . ?
C6 C3 C4 108.4(11) . . ?
C4 C3 C1 108.4(13) . . ?
C2 N4 H4A 109.5 . . ?
C2 N4 H4B 109.5 . . ?
C2 N4 H4C 109.5 . . ?
H4A N4 H4B 109.5 . . ?
H4A N4 H4C 109.5 . . ?
H4B N4 H4C 109.5 . . ?
C3 C5 H5A 109.5 . . ?
C3 C5 H5B 109.5 . . ?
C3 C5 H5C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C3 C6 H6A 109.5 . . ?
C3 C6 H6B 109.5 . . ?
C3 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C3 C4 H4D 109.5 . . ?
C3 C4 H4E 109.5 . . ?
C3 C4 H4F 109.5 . . ?
H4D C4 H4E 109.5 . . ?
H4D C4 H4F 109.5 . . ?
H4E C4 H4F 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 C1 C3 C5 54.2(18) . . . . ?
C2 C1 C3 C6 -67.6(15) . . . . ?
C2 C1 C3 C4 173.6(11) . . . . ?
C3 C1 C2 N4 169.0(11) . . . . ?

_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 1.396
_oxdiff_exptl_absorpt_empirical_full_min 0.759
####################################################################### 
# 
# 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_DMB2A_pbi
_database_code_depnum_ccdc_archive 'CCDC 2490430'
_audit_update_record             
;
2025-11-19 deposited with the CCDC.	2026-04-01 downloaded from the CCDC.
;
_audit_creation_date             2025-09-22
_audit_creation_method           
;
Olex2 1.5
(compiled 2024.01.12 svn.r2f8d729c for OlexSys, GUI svn.r6928)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        '2:1, 2,3-Dimethylbutan-2-amine with PbI2'
_chemical_formula_moiety         '4(I6 Pb2), 8(C6 H16 N)'
_chemical_formula_sum            'C48 H128 I24 N8 Pb8'
_chemical_formula_weight         5520.70
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Pb N C I'
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           61
_space_group_name_H-M_alt        'P b c a'
_space_group_name_Hall           '-P 2ac 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z'
'x, -y-1/2, z-1/2'

_cell_length_a                   16.5610(5)
_cell_length_b                   7.9958(3)
_cell_length_c                   22.3017(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2953.16(17)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    9938
_cell_measurement_temperature    297.20
_cell_measurement_theta_max      30.5180
_cell_measurement_theta_min      2.4640
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    17.659
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.51260
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear yellowish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    3.104
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       irregular
_exptl_crystal_F_000             2400
_exptl_crystal_size_max          0.2
_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  0.0427
_diffrn_reflns_av_unetI/netI     0.0240
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            19749
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        24.485
_diffrn_reflns_theta_max         24.485
_diffrn_reflns_theta_min         2.973
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      297.20
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     -8.00  48.00   0.50    5.00    --    4.40  34.00-125.00  112
  2  ω    -23.00  21.00   0.50    5.00    --   -5.65 -99.00  60.00   88
  3  ω    -23.00  24.00   0.50    5.00    --   -5.65 -99.00-150.00   94
  4  ω    -32.00  -5.00   0.50    5.00    --   -5.65  91.00   7.00   54
  5  ω     -1.00  40.00   0.50    5.00    --   -5.65  91.00   7.00   82
  6  ω    -14.00  26.00   0.50    5.00    --   -5.65 -99.00 120.00   80
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  
'XtaLAB Synergy, Single source at offset/far, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0617319000
_diffrn_orient_matrix_UB_12      0.0255552000
_diffrn_orient_matrix_UB_13      -0.0126818000
_diffrn_orient_matrix_UB_21      0.0618361000
_diffrn_orient_matrix_UB_22      -0.0297522000
_diffrn_orient_matrix_UB_23      0.0056460000
_diffrn_orient_matrix_UB_31      -0.0151772000
_diffrn_orient_matrix_UB_32      -0.0172179000
_diffrn_orient_matrix_UB_33      -0.0286222000
_diffrn_oxdiff_digest_frames     
;
015f40445058a2f9f2a153e8bda2c3de63000251b74
;
_diffrn_oxdiff_digest_hkl        
;
011f996b07803faf1250bf52098e1f2f7c7f0c
;
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2224
_reflns_number_total             2428
_reflns_odcompleteness_completeness 99.94
_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 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_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    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         0.629
_refine_diff_density_min         -1.882
_refine_diff_density_rms         0.159
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.169
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     105
_refine_ls_number_reflns         2428
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0270
_refine_ls_R_factor_gt           0.0243
_refine_ls_restrained_S_all      1.169
_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)+(0.0270P)²+2.5189P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0565
_refine_ls_wR_factor_ref         0.0575
_refine_special_details          
;
The deepest residual density is located close to the Pb atom,
which is consistent with Fourier truncation artifacts around heavy atoms.
No chemically meaningful features were observed in the residual map.
;
_olex2_refinement_description    
;
1.a Ternary CH refined with riding coordinates:
 C2(H2)
1.b Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C9(H9A,H9B,H9C), C11(H11A,
 H11B,H11C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb2 Pb 0.24738(2) 0.92827(3) 0.15097(2) 0.03720(9) Uani 1 1 d . . . . .
I2 I 0.09735(2) 0.65706(4) 0.16524(2) 0.03958(11) Uani 1 1 d . . . . .
I3 I 0.18653(2) 1.17547(5) 0.05195(2) 0.04736(12) Uani 1 1 d . . . . .
I4 I 0.15098(2) 1.17272(5) 0.24459(2) 0.04755(12) Uani 1 1 d . . . . .
N1 N -0.0562(4) 1.3002(7) 0.1827(2) 0.0615(15) Uani 1 1 d . . . . .
H1A H -0.003265 1.316853 0.179206 0.092 Uiso 1 1 calc GR . . . .
H1B H -0.065861 1.236009 0.214507 0.092 Uiso 1 1 calc GR . . . .
H1C H -0.081019 1.398096 0.187247 0.092 Uiso 1 1 calc GR . . . .
C2 C -0.0608(4) 1.3261(8) 0.0743(3) 0.0552(17) Uani 1 1 d . . . . .
H2 H -0.003106 1.348973 0.079696 0.066 Uiso 1 1 calc R . . . .
C4 C -0.0882(3) 1.2128(8) 0.1257(3) 0.0481(14) Uani 1 1 d . . . . .
C6 C -0.1058(5) 1.4936(10) 0.0756(4) 0.082(2) Uani 1 1 d . . . . .
H6A H -0.160452 1.477129 0.062588 0.124 Uiso 1 1 calc GR . . . .
H6B H -0.079389 1.571220 0.049185 0.124 Uiso 1 1 calc GR . . . .
H6C H -0.105572 1.537351 0.115637 0.124 Uiso 1 1 calc GR . . . .
C7 C -0.0456(5) 1.0404(9) 0.1229(4) 0.078(2) Uani 1 1 d . . . . .
H7A H -0.068491 0.975242 0.090941 0.094 Uiso 1 1 calc GR . . . .
H7B H -0.052960 0.982780 0.160229 0.094 Uiso 1 1 calc GR . . . .
H7C H 0.011029 1.056293 0.115635 0.094 Uiso 1 1 calc GR . . . .
C9 C -0.0719(6) 1.2436(13) 0.0138(3) 0.094(3) Uani 1 1 d . . . . .
H9A H -0.046406 1.135727 0.014079 0.141 Uiso 1 1 calc GR . . . .
H9B H -0.047837 1.311990 -0.016686 0.141 Uiso 1 1 calc GR . . . .
H9C H -0.128483 1.230598 0.005746 0.141 Uiso 1 1 calc GR . . . .
C11 C -0.1764(5) 1.1951(13) 0.1336(5) 0.098(3) Uani 1 1 d . . . . .
H11A H -0.187208 1.126538 0.168035 0.146 Uiso 1 1 calc GR . . . .
H11B H -0.199300 1.143830 0.098594 0.146 Uiso 1 1 calc GR . . . .
H11C H -0.200127 1.303537 0.139363 0.146 Uiso 1 1 calc GR . . . .


_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 I2 3.1718(4) 7_665 ?
Pb2 I2 3.3133(4) . ?
Pb2 I3 3.1303(4) . ?
Pb2 I3 3.1875(4) 7_655 ?
Pb2 I4 3.2754(4) . ?
Pb2 I4 3.3715(4) 7_655 ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 H1C 0.8900 . ?
N1 C4 1.544(8) . ?
C2 H2 0.9800 . ?
C2 C4 1.529(9) . ?
C2 C6 1.533(9) . ?
C2 C9 1.513(9) . ?
C4 C7 1.550(9) . ?
C4 C11 1.479(9) . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 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
I2 Pb2 I2 167.378(15) 7_665 . ?
I2 Pb2 I3 99.028(11) 7_665 7_655 ?
I2 Pb2 I4 83.262(11) 7_665 7_655 ?
I2 Pb2 I4 85.309(10) . 7_655 ?
I2 Pb2 I4 89.253(11) 7_665 . ?
I3 Pb2 I2 88.144(11) . 7_665 ?
I3 Pb2 I2 84.782(10) 7_655 . ?
I3 Pb2 I2 103.864(11) . . ?
I3 Pb2 I3 91.275(13) . 7_655 ?
I3 Pb2 I4 170.894(13) 7_655 . ?
I3 Pb2 I4 82.721(11) 7_655 7_655 ?
I3 Pb2 I4 168.595(13) . 7_655 ?
I3 Pb2 I4 85.178(11) . . ?
I4 Pb2 I2 87.925(10) . . ?
I4 Pb2 I4 102.135(14) . 7_655 ?
Pb2 I2 Pb2 76.105(8) 7_655 . ?
Pb2 I3 Pb2 78.531(10) . 7_665 ?
Pb2 I4 Pb2 73.954(9) . 7_665 ?
H1A N1 H1B 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1B N1 H1C 109.5 . . ?
C4 N1 H1A 109.5 . . ?
C4 N1 H1B 109.5 . . ?
C4 N1 H1C 109.5 . . ?
C4 C2 H2 108.0 . . ?
C4 C2 C6 111.1(6) . . ?
C6 C2 H2 108.0 . . ?
C9 C2 H2 108.0 . . ?
C9 C2 C4 111.9(6) . . ?
C9 C2 C6 109.7(7) . . ?
N1 C4 C7 106.3(5) . . ?
C2 C4 N1 104.3(5) . . ?
C2 C4 C7 111.2(5) . . ?
C11 C4 N1 106.5(6) . . ?
C11 C4 C2 116.0(6) . . ?
C11 C4 C7 111.7(7) . . ?
C2 C6 H6A 109.5 . . ?
C2 C6 H6B 109.5 . . ?
C2 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C4 C7 H7A 109.5 . . ?
C4 C7 H7B 109.5 . . ?
C4 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C2 C9 H9A 109.5 . . ?
C2 C9 H9B 109.5 . . ?
C2 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C4 C11 H11A 109.5 . . ?
C4 C11 H11B 109.5 . . ?
C4 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 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
C6 C2 C4 N1 -68.4(6) . . . . ?
C6 C2 C4 C7 177.4(6) . . . . ?
C6 C2 C4 C11 48.3(9) . . . . ?
C9 C2 C4 N1 168.5(6) . . . . ?
C9 C2 C4 C7 54.3(8) . . . . ?
C9 C2 C4 C11 -74.7(9) . . . . ?

_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 1.491
_oxdiff_exptl_absorpt_empirical_full_min 0.692
####################################################################### 
# 
# 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_NMB2A_pbi
_database_code_depnum_ccdc_archive 'CCDC 2490431'
loop_
_audit_author_name
_audit_author_address
'Migon Choi'
;Duke University
United States of America
;
_audit_update_record             
;
2025-09-22 deposited with the CCDC.	2026-04-01 downloaded from the CCDC.
;
_audit_creation_date             2025-09-22
_audit_creation_method           
;
Olex2 1.5
(compiled 2024.01.12 svn.r2f8d729c for OlexSys, GUI svn.r6928)
;
_shelx_SHELXL_version_number     2019/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'I3 Pb, C5 H14 N'
_chemical_formula_sum            'C5 H14 I3 N Pb'
_chemical_formula_weight         676.06
_chemical_absolute_configuration rm
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Pb C N I'
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           19
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'

_cell_length_a                   8.0027(3)
_cell_length_b                   10.9820(5)
_cell_length_c                   16.2078(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1424.43(10)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    4884
_cell_measurement_temperature    296.92(17)
_cell_measurement_theta_max      27.1280
_cell_measurement_theta_min      2.5130
_shelx_estimated_absorpt_T_max   0.262
_shelx_estimated_absorpt_T_min   0.121
_exptl_absorpt_coefficient_mu    18.302
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.42204
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear yellowish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    3.152
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             1168
_exptl_crystal_preparation       ?
_exptl_crystal_recrystallization_method ?
_exptl_crystal_size_max          0.2
_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  0.0289
_diffrn_reflns_av_unetI/netI     0.0276
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            12190
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.966
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.482
_diffrn_reflns_theta_min         2.240
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      296.92(17)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -34.00  43.00   0.50   25.00    --   -5.65  89.00 -57.00  154
  2  ω    -67.00  -9.00   0.50   25.00    --    4.40 -57.00 120.00  116
  3  ω    -23.00  28.00   0.50   25.00    --   -5.65 -99.00  30.00  102
  4  ω    -41.00  22.00   0.50   25.00    --   -5.65 -89.00-172.00  126
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  
'XtaLAB Synergy, Single source at offset/far, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0820291000
_diffrn_orient_matrix_UB_12      0.0244438000
_diffrn_orient_matrix_UB_13      0.0014873000
_diffrn_orient_matrix_UB_21      -0.0284327000
_diffrn_orient_matrix_UB_22      0.0534125000
_diffrn_orient_matrix_UB_23      -0.0202050000
_diffrn_orient_matrix_UB_31      -0.0179210000
_diffrn_orient_matrix_UB_32      0.0268832000
_diffrn_orient_matrix_UB_33      0.0387739000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_reflns_Friedel_coverage         0.725
_reflns_Friedel_fraction_full    0.992
_reflns_Friedel_fraction_max     0.960
_reflns_number_gt                2291
_reflns_number_total             3162
_reflns_odcompleteness_completeness 99.65
_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 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_refine_diff_density_max         0.863
_refine_diff_density_min         -0.702
_refine_diff_density_rms         0.113
_refine_ls_abs_structure_details 
;
 Flack x determined using 791 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.009(6)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     63
_refine_ls_number_reflns         3162
_refine_ls_number_restraints     157
_refine_ls_R_factor_all          0.0496
_refine_ls_R_factor_gt           0.0317
_refine_ls_restrained_S_all      1.075
_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)+(0.0448P)²+0.3871P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0798
_refine_ls_wR_factor_ref         0.0856
_refine_special_details          ?
_olex2_refinement_description    
;
1. Restrained distances
 C5-C3 = C6-C3 = C6-C4 = N-C3 = N-C2
 1.5 with sigma of 0.02
 N-C2 = C5-C3 = N-C3 = C6-C3
 1.5 with sigma of 0.02
 C6-C4
 1.5 with sigma of 0.02
 C6-C3 = C6-C4 = C5-C3
 1.54 with sigma of 0.02
2. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
C6 \\sim N \\sim C2 \\sim C3 \\sim C5 \\sim C4: within 2A with sigma of 0.04
and sigma for terminal atoms of 0.08 within 2A
N \\sim HA \\sim HB \\sim C2 \\sim C3 \\sim H3 \\sim C5 \\sim C6 \\sim C4 \\sim
H6B \\sim H5A \\sim H5B \\sim H5C \\sim H6A \\sim H4A \\sim H4B \\sim H4C:
within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
Uanis(C2) = Uanis(N) = Uanis(C3) = Uanis(C5) = Uanis(C6) = Uanis(C4)
4.a Riding coordinates:
 C2(H2A,H2B,H2C)
4.b Ternary CH refined with riding coordinates:
 C3(H3)
4.c Secondary CH2 refined with riding coordinates:
 N(HA,HB), C6(H6A,H6B)
4.d Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C5(H5A,H5B,H5C)
;
_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 -0.04396(5) 0.74818(5) -0.00008(3) 0.07623(17) Uani 1 1 d . U . . .
I2 I 0.21088(16) 0.58288(9) -0.10970(6) 0.1038(3) Uani 1 1 d . U . . .
I3 I 0.19569(15) 0.68268(11) 0.15077(5) 0.1076(3) Uani 1 1 d . U . . .
I4 I -0.30185(14) 0.53378(7) 0.04616(7) 0.0991(3) Uani 1 1 d . U . . .
N N -0.197(4) 0.669(2) 0.2683(18) 0.259(5) Uani 1 1 d D U . . .
HA H -0.291003 0.675943 0.239008 0.311 Uiso 1 1 calc R U . . .
HB H -0.113122 0.681997 0.233492 0.311 Uiso 1 1 calc R U . . .
C2 C -0.186(6) 0.540(3) 0.2960(19) 0.259(5) Uani 1 1 d D U . . .
H2A H -0.279072 0.519041 0.330424 0.389 Uiso 1 1 d R U . . .
H2B H -0.184412 0.487321 0.248504 0.389 Uiso 1 1 d R U . . .
H2C H -0.083792 0.528911 0.326564 0.389 Uiso 1 1 d R U . . .
C3 C -0.196(4) 0.774(3) 0.329(2) 0.259(5) Uani 1 1 d D U . . .
H3 H -0.208818 0.854151 0.302732 0.311 Uiso 1 1 calc R U . . .
C4 C -0.494(5) 0.756(3) 0.3266(19) 0.259(5) Uani 1 1 d D U . . .
H4A H -0.473767 0.821427 0.288365 0.389 Uiso 1 1 calc R U . . .
H4B H -0.589691 0.775271 0.359788 0.389 Uiso 1 1 calc R U . . .
H4C H -0.514003 0.682257 0.296647 0.389 Uiso 1 1 calc R U . . .
C5 C -0.055(4) 0.770(3) 0.391(2) 0.259(5) Uani 1 1 d D U . . .
H5A H -0.073971 0.829034 0.433597 0.389 Uiso 1 1 calc R U . . .
H5B H 0.048835 0.788152 0.363516 0.389 Uiso 1 1 calc R U . . .
H5C H -0.048584 0.690212 0.414875 0.389 Uiso 1 1 calc R U . . .
C6 C -0.343(4) 0.740(3) 0.382(2) 0.259(5) Uani 1 1 d D U . . .
H6A H -0.350106 0.792775 0.429568 0.311 Uiso 1 1 calc R U . . .
H6B H -0.333359 0.656427 0.400078 0.311 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 I2 3.2575(11) . ?
Pb1 I2 3.2338(11) 3_465 ?
Pb1 I3 3.2988(11) 3_465 ?
Pb1 I3 3.1895(11) . ?
Pb1 I4 3.2195(11) . ?
Pb1 I4 3.1695(11) 3_565 ?
N HA 0.8900 . ?
N HB 0.8900 . ?
N C2 1.498(17) . ?
N C3 1.518(18) . ?
C2 H2A 0.9602 . ?
C2 H2B 0.9600 . ?
C2 H2C 0.9600 . ?
C3 H3 0.9800 . ?
C3 C5 1.514(15) . ?
C3 C6 1.495(15) . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?
C4 C6 1.514(15) . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
I2 Pb1 I2 178.52(4) 3_465 . ?
I2 Pb1 I3 96.89(3) . 3_465 ?
I2 Pb1 I3 83.81(3) 3_465 3_465 ?
I3 Pb1 I2 85.18(3) . . ?
I3 Pb1 I2 94.15(3) . 3_465 ?
I3 Pb1 I3 177.69(3) . 3_465 ?
I3 Pb1 I4 92.41(3) . . ?
I4 Pb1 I2 84.41(3) . 3_465 ?
I4 Pb1 I2 93.85(3) 3_565 3_465 ?
I4 Pb1 I2 84.82(3) 3_565 . ?
I4 Pb1 I2 96.94(3) . . ?
I4 Pb1 I3 89.05(3) 3_565 . ?
I4 Pb1 I3 86.32(3) . 3_465 ?
I4 Pb1 I3 92.16(3) 3_565 3_465 ?
I4 Pb1 I4 177.80(4) 3_565 . ?
Pb1 I2 Pb1 76.114(19) 3_565 . ?
Pb1 I3 Pb1 76.134(19) . 3_565 ?
Pb1 I4 Pb1 77.553(19) 3_465 . ?
HA N HB 106.7 . . ?
C2 N HA 106.9 . . ?
C2 N HB 106.9 . . ?
C2 N C3 122(3) . . ?
C3 N HA 106.9 . . ?
C3 N HB 106.9 . . ?
N C2 H2A 110.3 . . ?
N C2 H2B 109.2 . . ?
N C2 H2C 108.9 . . ?
H2A C2 H2B 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
N C3 H3 113.2 . . ?
C5 C3 N 114(3) . . ?
C5 C3 H3 113.2 . . ?
C6 C3 N 100(3) . . ?
C6 C3 H3 113.2 . . ?
C6 C3 C5 102(3) . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C6 C4 H4A 109.5 . . ?
C6 C4 H4B 109.5 . . ?
C6 C4 H4C 109.5 . . ?
C3 C5 H5A 109.5 . . ?
C3 C5 H5B 109.5 . . ?
C3 C5 H5C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C3 C6 C4 105(3) . . ?
C3 C6 H6A 110.7 . . ?
C3 C6 H6B 110.7 . . ?
C4 C6 H6A 110.7 . . ?
C4 C6 H6B 110.7 . . ?
H6A C6 H6B 108.8 . . ?

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
N C3 C6 C4 -69(3) . . . . ?
C2 N C3 C5 51(5) . . . . ?
C2 N C3 C6 -57(5) . . . . ?
C5 C3 C6 C4 174(3) . . . . ?

_olex2_submission_original_sample_id 
'N-Methylbutan-2-amine with PbI2 (1:1 ratio)'
_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 2.170
_oxdiff_exptl_absorpt_empirical_full_min 0.662
