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

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

data_[c7h16n]pbi3-213k(1)
_database_code_depnum_ccdc_archive 'CCDC 2272301'
loop_
_audit_author_name
_audit_author_address
'Xiaotong Sun'
;Southeast University
China
;
_audit_update_record             
;
2023-06-26 deposited with the CCDC.	2023-10-05 downloaded from the CCDC.
;
_audit_creation_date             2023-06-26
_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        '[C7H16N]PbI3'
_chemical_formula_moiety         'I3 Pb, C7 H16 N'
_chemical_formula_sum            'C7 H16 I3 N Pb'
_chemical_formula_weight         702.10
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P  21/c'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   11.9805(9)
_cell_length_b                   16.4269(12)
_cell_length_c                   7.8664(4)
_cell_angle_alpha                90
_cell_angle_beta                 102.060(3)
_cell_angle_gamma                90
_cell_volume                     1513.96(18)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    5367
_cell_measurement_temperature    213.00
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      2.48
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    17.226
_exptl_absorpt_correction_T_max  0.7464
_exptl_absorpt_correction_T_min  0.6154
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1027 before and 0.0732 after correction.
The Ratio of minimum to maximum transmission is 0.8245.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    3.080
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             1224
_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  0.1132
_diffrn_reflns_av_unetI/netI     0.0749
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            43114
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.635
_diffrn_reflns_theta_min         2.135
_diffrn_ambient_temperature      213
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3285
_reflns_number_total             5521
_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       'SAINT V8.40B (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_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         4.384
_refine_diff_density_min         -1.867
_refine_diff_density_rms         0.404
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     112
_refine_ls_number_reflns         5521
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1104
_refine_ls_R_factor_gt           0.0529
_refine_ls_restrained_S_all      1.062
_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)+(0.0521P)²+15.4191P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1080
_refine_ls_wR_factor_ref         0.1484
_refine_special_details          ?
_olex2_refinement_description    
;
1.a Ternary CH refined with riding coordinates:
 C007(H007)
1.b Secondary CH2 refined with riding coordinates:
 C006(H00A,H00B), C009(H00F,H00G), C10(H10A,H10B)
1.c Idealised Me refined as rotating group:
 C008(H00C,H00D,H00E), C5(H5A,H5B,H5C), C7(H7A,H7B,H7C)
;
_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 0.28425(3) 0.75039(2) 0.42295(5) 0.03019(12) Uani 1 1 d . . . . .
I002 I 0.09297(6) 0.67992(4) 0.11412(9) 0.03428(17) Uani 1 1 d . . . . .
I003 I 0.47626(6) 0.67106(5) 0.23527(9) 0.03815(18) Uani 1 1 d . . . . .
I004 I 0.28446(6) 0.59433(4) 0.66414(9) 0.03610(17) Uani 1 1 d . . . . .
N005 N 0.7161(8) 0.5973(6) 0.8325(11) 0.038(2) Uani 1 1 d . . . . .
C006 C 0.7363(11) 0.6148(7) 0.6507(13) 0.042(3) Uani 1 1 d . . . . .
H00A H 0.714359 0.566672 0.577755 0.051 Uiso 1 1 calc R U . . .
H00B H 0.686458 0.659697 0.600002 0.051 Uiso 1 1 calc R U . . .
C007 C 0.8557(11) 0.6363(8) 0.6460(14) 0.049(3) Uani 1 1 d . . . . .
H007 H 0.887432 0.685524 0.711172 0.059 Uiso 1 1 calc R U . . .
C008 C 0.5933(11) 0.5783(10) 0.813(2) 0.071(5) Uani 1 1 d . . . . .
H00C H 0.548163 0.621187 0.746902 0.107 Uiso 1 1 calc R U . . .
H00D H 0.574717 0.574528 0.927075 0.107 Uiso 1 1 calc R U . . .
H00E H 0.576482 0.526913 0.752555 0.107 Uiso 1 1 calc R U . . .
C009 C 0.9396(13) 0.5709(10) 0.624(2) 0.070(4) Uani 1 1 d . . . . .
H00F H 1.020210 0.579892 0.676674 0.084 Uiso 1 1 calc R U . . .
H00G H 0.914404 0.514117 0.624210 0.084 Uiso 1 1 calc R U . . .
C5 C 0.7433(11) 0.6712(8) 0.9479(19) 0.057(4) Uani 1 1 d . . . . .
H5A H 0.823827 0.684058 0.963177 0.086 Uiso 1 1 calc R U . . .
H5B H 0.725296 0.659979 1.060211 0.086 Uiso 1 1 calc R U . . .
H5C H 0.698287 0.717088 0.894433 0.086 Uiso 1 1 calc R U . . .
C7 C 0.7867(13) 0.5274(9) 0.911(2) 0.067(4) Uani 1 1 d . . . . .
H7A H 0.775642 0.482163 0.829547 0.100 Uiso 1 1 calc R U . . .
H7B H 0.764263 0.511231 1.017173 0.100 Uiso 1 1 calc R U . . .
H7C H 0.866557 0.543088 0.936103 0.100 Uiso 1 1 calc R U . . .
C10 C 0.8876(17) 0.6224(11) 0.471(2) 0.086(6) Uani 1 1 d . . . . .
H10A H 0.830438 0.597132 0.378259 0.103 Uiso 1 1 calc R U . . .
H10B H 0.936325 0.662957 0.430763 0.103 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 I002 3.1886(8) . ?
Pb01 I002 3.2037(8) 4_576 ?
Pb01 I003 3.2605(8) 4_576 ?
Pb01 I003 3.2541(8) . ?
Pb01 I004 3.1889(8) . ?
Pb01 I004 3.2641(8) 4_575 ?
N005 C006 1.527(13) . ?
N005 C008 1.480(15) . ?
N005 C5 1.511(15) . ?
N005 C7 1.481(16) . ?
C006 H00A 0.9800 . ?
C006 H00B 0.9800 . ?
C006 C007 1.481(17) . ?
C007 H007 0.9900 . ?
C007 C009 1.51(2) . ?
C007 C10 1.524(17) . ?
C008 H00C 0.9700 . ?
C008 H00D 0.9700 . ?
C008 H00E 0.9700 . ?
C009 H00F 0.9800 . ?
C009 H00G 0.9800 . ?
C009 C10 1.50(2) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C5 H5C 0.9700 . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C7 H7C 0.9700 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
I002 Pb01 I002 90.96(2) . 4_576 ?
I002 Pb01 I003 88.06(2) 4_576 4_576 ?
I002 Pb01 I003 177.96(2) . 4_576 ?
I002 Pb01 I003 177.30(2) 4_576 . ?
I002 Pb01 I003 88.43(2) . . ?
I002 Pb01 I004 94.16(2) . . ?
I002 Pb01 I004 96.16(2) 4_576 4_575 ?
I002 Pb01 I004 84.41(2) . 4_575 ?
I003 Pb01 I003 92.64(2) . 4_576 ?
I003 Pb01 I004 86.40(2) . 4_575 ?
I003 Pb01 I004 93.92(2) 4_576 4_575 ?
I004 Pb01 I002 85.40(2) . 4_576 ?
I004 Pb01 I003 92.02(2) . . ?
I004 Pb01 I003 87.54(2) . 4_576 ?
I004 Pb01 I004 177.89(2) . 4_575 ?
Pb01 I002 Pb01 75.948(17) . 4_575 ?
Pb01 I003 Pb01 74.278(17) . 4_575 ?
Pb01 I004 Pb01 75.100(16) . 4_576 ?
C008 N005 C006 107.0(10) . . ?
C008 N005 C5 108.4(9) . . ?
C008 N005 C7 110.5(11) . . ?
C5 N005 C006 110.8(9) . . ?
C7 N005 C006 110.2(9) . . ?
C7 N005 C5 109.9(11) . . ?
N005 C006 H00A 108.7 . . ?
N005 C006 H00B 108.7 . . ?
H00A C006 H00B 107.6 . . ?
C007 C006 N005 114.3(9) . . ?
C007 C006 H00A 108.7 . . ?
C007 C006 H00B 108.7 . . ?
C006 C007 H007 116.7 . . ?
C006 C007 C009 120.3(11) . . ?
C006 C007 C10 114.4(11) . . ?
C009 C007 H007 116.7 . . ?
C009 C007 C10 59.2(10) . . ?
C10 C007 H007 116.7 . . ?
N005 C008 H00C 109.5 . . ?
N005 C008 H00D 109.5 . . ?
N005 C008 H00E 109.5 . . ?
H00C C008 H00D 109.5 . . ?
H00C C008 H00E 109.5 . . ?
H00D C008 H00E 109.5 . . ?
C007 C009 H00F 117.7 . . ?
C007 C009 H00G 117.7 . . ?
H00F C009 H00G 114.8 . . ?
C10 C009 C007 61.0(10) . . ?
C10 C009 H00F 117.7 . . ?
C10 C009 H00G 117.7 . . ?
N005 C5 H5A 109.5 . . ?
N005 C5 H5B 109.5 . . ?
N005 C5 H5C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
N005 C7 H7A 109.5 . . ?
N005 C7 H7B 109.5 . . ?
N005 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C007 C10 H10A 117.8 . . ?
C007 C10 H10B 117.8 . . ?
C009 C10 C007 59.8(10) . . ?
C009 C10 H10A 117.8 . . ?
C009 C10 H10B 117.8 . . ?
H10A C10 H10B 114.9 . . ?

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
N005 C006 C007 C009 90.6(13) . . . . ?
N005 C006 C007 C10 157.8(12) . . . . ?
C006 C007 C009 C10 102.0(13) . . . . ?
C006 C007 C10 C009 -112.0(14) . . . . ?
C008 N005 C006 C007 179.2(11) . . . . ?
C5 N005 C006 C007 61.2(13) . . . . ?
C7 N005 C006 C007 -60.7(14) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_[c7h16n]pbbr3-233k_auto
_database_code_depnum_ccdc_archive 'CCDC 2272303'
loop_
_audit_author_name
_audit_author_address
'Xiaotong Sun'
;Southeast University
China
;
_audit_update_record             
;
2023-06-26 deposited with the CCDC.	2023-10-05 downloaded from the CCDC.
;
_audit_creation_date             2023-06-25
_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        C7H16PbBr3
_chemical_formula_moiety         'Br3 Pb, C7 H16 N'
_chemical_formula_sum            'C7 H16 Br3 N Pb'
_chemical_formula_weight         561.13
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           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, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z'

_cell_length_a                   15.8846(8)
_cell_length_b                   7.6949(3)
_cell_length_c                   22.2250(10)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2716.6(2)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    5175
_cell_measurement_temperature    232.99(10)
_cell_measurement_theta_max      30.3920
_cell_measurement_theta_min      2.2510
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    21.206
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.06412
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.63a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.744
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             2016
_exptl_crystal_preparation       1
_exptl_crystal_recrystallization_method 1
_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  0.0686
_diffrn_reflns_av_unetI/netI     0.0520
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.843
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            17313
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.843
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.668
_diffrn_reflns_theta_min         1.833
_diffrn_ambient_temperature      233
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.843
_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 -38.00   0.50    1.28    --    4.71 -46.00  32.00   60
  2  ω    -34.00   0.00   0.50    1.28    --    4.71 -46.00  32.00   68
  3  ω    -13.00  36.00   0.50    1.28    --    4.71 -99.00 -30.00   98
  4  ω    -76.00   8.00   0.50    1.28    --   -5.49 -38.00-180.00  168
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2393
_reflns_number_total             3541
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.63a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.63a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.63a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_refine_diff_density_max         1.495
_refine_diff_density_min         -1.664
_refine_diff_density_rms         0.270
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     112
_refine_ls_number_reflns         3541
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0888
_refine_ls_R_factor_gt           0.0498
_refine_ls_restrained_S_all      1.076
_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)+(0.0495P)²+8.4394P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1020
_refine_ls_wR_factor_ref         0.1148
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C5(H5)
2.b Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C6(H6A,H6B), C7(H7A,H7B)
2.c Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C1(H1A,H1B,H1C), C2(H2A,H2B,H2C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.24965(2) 0.16986(4) 0.36027(2) 0.02680(12) Uani 1 1 d . . . . .
Br1 Br 0.31515(6) 0.40974(12) 0.45373(4) 0.0340(2) Uani 1 1 d . . . . .
Br2 Br 0.39864(6) -0.05192(13) 0.35974(4) 0.0380(2) Uani 1 1 d . . . . .
Br3 Br 0.32149(7) 0.41250(13) 0.26608(4) 0.0397(2) Uani 1 1 d . . . . .
N1 N 0.5912(5) 0.4614(11) 0.3587(3) 0.0366(18) Uani 1 1 d . . . . .
C5 C 0.6303(6) 0.2110(11) 0.4268(4) 0.035(2) Uani 1 1 d . . . . .
H5 H 0.682678 0.262762 0.442972 0.042 Uiso 1 1 calc R U . . .
C3 C 0.6726(7) 0.5556(14) 0.3684(5) 0.049(3) Uani 1 1 d . . . . .
H3A H 0.692777 0.533346 0.408872 0.073 Uiso 1 1 calc R U . . .
H3B H 0.663782 0.679454 0.363144 0.073 Uiso 1 1 calc R U . . .
H3C H 0.713945 0.515161 0.339511 0.073 Uiso 1 1 calc R U . . .
C4 C 0.6053(7) 0.2655(12) 0.3650(4) 0.040(2) Uani 1 1 d . . . . .
H4A H 0.553328 0.204831 0.353926 0.048 Uiso 1 1 calc R U . . .
H4B H 0.649260 0.229584 0.336727 0.048 Uiso 1 1 calc R U . . .
C6 C 0.5649(8) 0.1626(14) 0.4718(5) 0.054(3) Uani 1 1 d . . . . .
H6A H 0.505745 0.175922 0.460025 0.065 Uiso 1 1 calc R U . . .
H6B H 0.576669 0.186936 0.514206 0.065 Uiso 1 1 calc R U . . .
C1 C 0.5287(8) 0.5259(16) 0.4021(6) 0.067(4) Uani 1 1 d . . . . .
H1A H 0.550330 0.511929 0.442634 0.101 Uiso 1 1 calc R U . . .
H1B H 0.476894 0.460402 0.397839 0.101 Uiso 1 1 calc R U . . .
H1C H 0.517746 0.647933 0.394468 0.101 Uiso 1 1 calc R U . . .
C7 C 0.6147(8) 0.0224(14) 0.4419(6) 0.060(3) Uani 1 1 d . . . . .
H7A H 0.586146 -0.049461 0.411705 0.072 Uiso 1 1 calc R U . . .
H7B H 0.657140 -0.038436 0.465939 0.072 Uiso 1 1 calc R U . . .
C2 C 0.5625(9) 0.497(2) 0.2957(6) 0.081(5) Uani 1 1 d . . . . .
H2A H 0.554003 0.620562 0.290379 0.121 Uiso 1 1 calc R U . . .
H2B H 0.509921 0.436017 0.288276 0.121 Uiso 1 1 calc R U . . .
H2C H 0.604816 0.456205 0.267521 0.121 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb1 Br1 2.9672(9) . ?
Pb1 Br1 3.0627(9) 8_655 ?
Pb1 Br2 3.1831(10) 8_665 ?
Pb1 Br2 2.9178(10) . ?
Pb1 Br3 3.0283(10) . ?
Pb1 Br3 3.0953(10) 8_655 ?
N1 C3 1.498(12) . ?
N1 C4 1.530(12) . ?
N1 C1 1.470(13) . ?
N1 C2 1.498(13) . ?
C5 H5 0.9900 . ?
C5 C4 1.490(13) . ?
C5 C6 1.488(14) . ?
C5 C7 1.510(14) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C3 H3C 0.9700 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 C7 1.494(16) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C1 H1C 0.9700 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C2 H2C 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
Br1 Pb1 Br1 92.85(3) . 8_655 ?
Br1 Pb1 Br2 81.01(3) . 8_665 ?
Br1 Pb1 Br2 101.15(3) 8_655 8_665 ?
Br1 Pb1 Br3 88.18(3) . . ?
Br1 Pb1 Br3 85.29(3) 8_655 8_655 ?
Br1 Pb1 Br3 178.11(3) . 8_655 ?
Br2 Pb1 Br1 94.72(3) . . ?
Br2 Pb1 Br1 83.86(3) . 8_655 ?
Br2 Pb1 Br2 173.51(3) . 8_665 ?
Br2 Pb1 Br3 85.36(3) . 8_655 ?
Br2 Pb1 Br3 92.99(3) . . ?
Br3 Pb1 Br1 176.76(3) . 8_655 ?
Br3 Pb1 Br2 99.07(3) 8_655 8_665 ?
Br3 Pb1 Br2 82.05(3) . 8_665 ?
Br3 Pb1 Br3 93.70(3) . 8_655 ?
Pb1 Br1 Pb1 79.28(2) . 8_665 ?
Pb1 Br2 Pb1 78.06(2) . 8_655 ?
Pb1 Br3 Pb1 77.84(2) . 8_665 ?
C3 N1 C4 109.7(8) . . ?
C1 N1 C3 108.9(9) . . ?
C1 N1 C4 111.7(8) . . ?
C1 N1 C2 110.3(10) . . ?
C2 N1 C3 108.1(8) . . ?
C2 N1 C4 108.0(9) . . ?
C4 C5 H5 116.4 . . ?
C4 C5 C7 115.5(9) . . ?
C6 C5 H5 116.4 . . ?
C6 C5 C4 120.2(9) . . ?
C6 C5 C7 59.8(7) . . ?
C7 C5 H5 116.4 . . ?
N1 C3 H3A 109.5 . . ?
N1 C3 H3B 109.5 . . ?
N1 C3 H3C 109.5 . . ?
H3A C3 H3B 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
N1 C4 H4A 108.8 . . ?
N1 C4 H4B 108.8 . . ?
C5 C4 N1 113.7(8) . . ?
C5 C4 H4A 108.8 . . ?
C5 C4 H4B 108.8 . . ?
H4A C4 H4B 107.7 . . ?
C5 C6 H6A 117.7 . . ?
C5 C6 H6B 117.7 . . ?
C5 C6 C7 60.8(7) . . ?
H6A C6 H6B 114.8 . . ?
C7 C6 H6A 117.7 . . ?
C7 C6 H6B 117.7 . . ?
N1 C1 H1A 109.5 . . ?
N1 C1 H1B 109.5 . . ?
N1 C1 H1C 109.5 . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C5 C7 H7A 117.8 . . ?
C5 C7 H7B 117.8 . . ?
C6 C7 C5 59.4(7) . . ?
C6 C7 H7A 117.8 . . ?
C6 C7 H7B 117.8 . . ?
H7A C7 H7B 115.0 . . ?
N1 C2 H2A 109.5 . . ?
N1 C2 H2B 109.5 . . ?
N1 C2 H2C 109.5 . . ?
H2A C2 H2B 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C3 N1 C4 C5 65.2(10) . . . . ?
C4 C5 C6 C7 103.8(10) . . . . ?
C4 C5 C7 C6 -111.5(10) . . . . ?
C6 C5 C4 N1 90.3(11) . . . . ?
C1 N1 C4 C5 -55.7(12) . . . . ?
C7 C5 C4 N1 158.7(9) . . . . ?
C2 N1 C4 C5 -177.2(9) . . . . ?

_olex2_exptl_crystal_mounting_method 1
_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
;
####################################################################### 
# 
# 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_[c7h16n]pbi3-298k
_database_code_depnum_ccdc_archive 'CCDC 2272302'
loop_
_audit_author_name
_audit_author_address
'Xiaotong Sun'
;Southeast University
China
;
_audit_update_record             
;
2023-06-26 deposited with the CCDC.	2023-10-05 downloaded from the CCDC.
;
_audit_creation_date             2023-06-26
_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        '[C7H16N]PbI3-298K'
_chemical_formula_moiety         'I3 Pb, C7 N'
_chemical_formula_sum            'C7 I3 N Pb'
_chemical_formula_weight         685.97
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   11.554(3)
_cell_length_b                   17.566(4)
_cell_length_c                   7.9189(16)
_cell_angle_alpha                90
_cell_angle_beta                 101.329(5)
_cell_angle_gamma                90
_cell_volume                     1575.9(6)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    4334
_cell_measurement_temperature    298.00
_cell_measurement_theta_max      27.22
_cell_measurement_theta_min      2.33
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    16.547
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6122
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0882 before and 0.0703 after correction.
The Ratio of minimum to maximum transmission is 0.8205.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.891
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             1160
_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  0.1241
_diffrn_reflns_av_unetI/netI     0.0657
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            42542
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.503
_diffrn_reflns_theta_min         2.139
_diffrn_ambient_temperature      298.00
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2402
_reflns_number_total             4778
_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       'SAINT V8.40B (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_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         2.059
_refine_diff_density_min         -1.595
_refine_diff_density_rms         0.236
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     147
_refine_ls_number_reflns         4778
_refine_ls_number_restraints     154
_refine_ls_R_factor_all          0.1205
_refine_ls_R_factor_gt           0.0482
_refine_ls_restrained_S_all      1.036
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0455P)²+8.2083P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1003
_refine_ls_wR_factor_ref         0.1372
_refine_special_details          ?
_olex2_refinement_description    
;
1. Restrained distances
 C6-C7
 1.5 with sigma of 0.01
 C5-C7 = C5-C6
 1.5 with sigma of 0.01
 C5-C4A = C5-C4B
 1.5 with sigma of 0.01
 N1-C4A = N1-C4B
 1.47 with sigma of 0.01
 N1-C3B \\sim N1-C3A \\sim N1-C2A \\sim N1-C2B \\sim N1-C1A \\sim N1-C1B
 with sigma of 0.02
2. Uiso/Uaniso restraints and constraints
C3A \\sim N1 \\sim C4B \\sim C2A \\sim C1A \\sim C4A \\sim C2B \\sim C1B \\sim
C3B \\sim C5 \\sim C7 \\sim C6: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
3. Others
 Sof(C4B)=1-FVAR(1)
 Sof(C4A)=FVAR(1)
 Sof(C2A)=Sof(C1A)=Sof(C3A)=1-FVAR(2)
 Sof(C2B)=Sof(C1B)=Sof(C3B)=FVAR(2)
;
_atom_sites_solution_hydrogens   .
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.68518(3) 0.74984(2) 0.55679(4) 0.05199(9) Uani 1 1 d . . . . .
I3 I 0.48800(6) 0.67467(4) 0.25233(8) 0.06609(18) Uani 1 1 d . . . . .
I2 I 0.87818(6) 0.67727(4) 0.36473(8) 0.06816(19) Uani 1 1 d . . . . .
I1 I 0.68960(6) 0.60458(4) 0.80758(7) 0.06922(19) Uani 1 1 d . . . . .
N1 N 0.7354(7) 0.4286(4) 0.3257(8) 0.094(2) Uani 1 1 d D U . . .
C4B C 0.7573(8) 0.3961(15) 0.1634(15) 0.113(3) Uani 0.24(2) 1 d D U P A 2
C2A C 0.8168(15) 0.4435(12) 0.4966(18) 0.119(5) Uani 0.759(12) 1 d D U P A 2
C1A C 0.6369(13) 0.4847(9) 0.333(2) 0.115(5) Uani 0.759(12) 1 d D U P A 2
C3A C 0.6799(16) 0.3508(8) 0.300(2) 0.118(4) Uani 0.759(12) 1 d D U P A 2
C7 C 0.8702(12) 0.3345(5) 0.0153(14) 0.147(3) Uani 1 1 d D U . . .
C6 C 0.9360(10) 0.4063(6) -0.0031(12) 0.144(3) Uani 1 1 d D U . . .
C5 C 0.8860(7) 0.3931(5) 0.1553(10) 0.130(2) Uani 1 1 d D U . . .
C4A C 0.8022(9) 0.4522(7) 0.1932(13) 0.113(3) Uani 0.76(2) 1 d D U P A 1
C2B C 0.710(4) 0.3747(15) 0.462(3) 0.113(5) Uani 0.241(12) 1 d D U P A 1
C1B C 0.639(2) 0.4800(16) 0.232(5) 0.106(7) Uani 0.241(12) 1 d D U P A 1
C3B C 0.748(5) 0.3467(10) 0.387(5) 0.110(5) Uani 0.241(12) 1 d D 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 I3 3.2540(8) . ?
Pb1 I3 3.2761(9) 4_576 ?
Pb1 I2 3.2006(9) . ?
Pb1 I2 3.2284(8) 4_576 ?
Pb1 I1 3.2366(9) 4_575 ?
Pb1 I1 3.2276(9) . ?
N1 C4B 1.473(9) . ?
N1 C2A 1.512(12) . ?
N1 C1A 1.516(12) . ?
N1 C3A 1.505(13) . ?
N1 C4A 1.479(8) . ?
N1 C2B 1.509(16) . ?
N1 C1B 1.509(16) . ?
N1 C3B 1.514(15) . ?
C4B C5 1.503(8) . ?
C7 C6 1.495(9) . ?
C7 C5 1.497(8) . ?
C6 C5 1.498(8) . ?
C5 C4A 1.490(8) . ?

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
I3 Pb1 I3 93.66(3) . 4_576 ?
I2 Pb1 I3 179.59(2) . 4_576 ?
I2 Pb1 I3 178.81(2) 4_576 . ?
I2 Pb1 I3 85.63(2) 4_576 4_576 ?
I2 Pb1 I3 86.45(2) . . ?
I2 Pb1 I2 94.27(3) . 4_576 ?
I2 Pb1 I1 92.82(2) . . ?
I2 Pb1 I1 93.20(2) 4_576 4_575 ?
I2 Pb1 I1 85.93(2) . 4_575 ?
I1 Pb1 I3 87.57(2) . 4_576 ?
I1 Pb1 I3 93.67(2) 4_575 4_576 ?
I1 Pb1 I3 93.40(2) . . ?
I1 Pb1 I3 87.79(2) 4_575 . ?
I1 Pb1 I2 85.62(2) . 4_576 ?
I1 Pb1 I1 178.23(3) . 4_575 ?
Pb1 I3 Pb1 74.65(2) . 4_575 ?
Pb1 I2 Pb1 76.03(2) . 4_575 ?
Pb1 I1 Pb1 75.54(2) . 4_576 ?
C4B N1 C2A 131.7(10) . . ?
C4B N1 C1A 122.9(11) . . ?
C4B N1 C3A 71.0(12) . . ?
C2A N1 C1A 101.2(11) . . ?
C3A N1 C2A 116.8(12) . . ?
C3A N1 C1A 107.0(11) . . ?
C4A N1 C2B 152.5(17) . . ?
C4A N1 C1B 85.4(16) . . ?
C4A N1 C3B 118(2) . . ?
C2B N1 C1B 120(2) . . ?
C2B N1 C3B 36(2) . . ?
C1B N1 C3B 138(3) . . ?
N1 C4B C5 113.1(8) . . ?
C6 C7 C5 60.1(4) . . ?
C7 C6 C5 60.0(5) . . ?
C7 C5 C4B 94.5(9) . . ?
C7 C5 C6 59.9(4) . . ?
C6 C5 C4B 125.3(9) . . ?
C4A C5 C7 129.7(9) . . ?
C4A C5 C6 115.6(8) . . ?
N1 C4A C5 113.5(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 C4B C5 C7 160.6(16) . . . . ?
N1 C4B C5 C6 -143.6(13) . . . . ?
C2A N1 C4B C5 -15(3) . . . . ?
C1A N1 C4B C5 137.4(15) . . . . ?
C3A N1 C4B C5 -124.2(19) . . . . ?
C7 C6 C5 C4B -72.5(15) . . . . ?
C7 C6 C5 C4A -122.7(10) . . . . ?
C7 C5 C4A N1 96.0(12) . . . . ?
C6 C7 C5 C4B 128.6(12) . . . . ?
C6 C7 C5 C4A 99.7(12) . . . . ?
C6 C5 C4A N1 167.0(8) . . . . ?
C2B N1 C4A C5 8(3) . . . . ?
C1B N1 C4A C5 -150.3(15) . . . . ?
C3B N1 C4A C5 -8(2) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_20221211-3pbbr2_auto
_database_code_depnum_ccdc_archive 'CCDC 2272304'
loop_
_audit_author_name
_audit_author_address
'Xiaotong Sun'
;Southeast University
China
;
_audit_update_record             
;
2023-06-26 deposited with the CCDC.	2023-10-05 downloaded from the CCDC.
;
_audit_creation_date             2023-04-10
_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        '[C7H16N]PbBr2-233K'
_chemical_formula_moiety         'Br3 Pb, C7 N'
_chemical_formula_sum            'C7 Br3 N Pb'
_chemical_formula_weight         545.00
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C H Br Pb N'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z'

_cell_length_a                   17.0361(8)
_cell_length_b                   7.6699(3)
_cell_length_c                   21.3038(12)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2783.7(2)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    4170
_cell_measurement_temperature    298.23(10)
_cell_measurement_theta_max      30.6110
_cell_measurement_theta_min      2.3970
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    20.692
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.08434
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.63a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.601
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             1888
_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  0.0495
_diffrn_reflns_av_unetI/netI     0.0526
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.808
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            13361
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.808
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.912
_diffrn_reflns_theta_min         2.255
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      298
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.808
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     11.00  75.00   0.50    2.01    --    4.71  38.00-150.00  128
  2  ω    -45.00  -5.00   0.50    2.01    --   -5.49 -27.00-144.00   80
  3  ω    -11.00  33.00   0.50    2.01    --    4.71 -99.00-180.00   88
;
_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      0.0402887000
_diffrn_orient_matrix_UB_12      0.0148757000
_diffrn_orient_matrix_UB_13      -0.0065649000
_diffrn_orient_matrix_UB_21      0.0099461000
_diffrn_orient_matrix_UB_22      -0.0288597000
_diffrn_orient_matrix_UB_23      0.0306130000
_diffrn_orient_matrix_UB_31      0.0035801000
_diffrn_orient_matrix_UB_32      -0.0865689000
_diffrn_orient_matrix_UB_33      -0.0113068000
_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                1970
_reflns_number_total             3552
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.63a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.63a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.63a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         1.546
_refine_diff_density_min         -2.464
_refine_diff_density_rms         0.359
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     175
_refine_ls_number_reflns         3552
_refine_ls_number_restraints     315
_refine_ls_R_factor_all          0.1511
_refine_ls_R_factor_gt           0.0805
_refine_ls_restrained_S_all      1.024
_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)+(0.0828P)²+82.7711P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1858
_refine_ls_wR_factor_ref         0.2240
_refine_special_details          ?
_olex2_refinement_description    
;
1. Restrained distances
 C13A-C12A
 2.55 with sigma of 0.02
 C10A-C14A
 2.5 with sigma of 0.02
 C13A-C14A
 2.5 with sigma of 0.02
 N005-C14B \\sim N005-C14A \\sim N005-C10B \\sim N005-C10A \\sim N005-C12B
\\sim N005-C12A \\sim C7A-
 C13A \\sim C7B-C13B \\sim N005-C13A \\sim N005-C13B \\sim C7A-C11A \\sim
C7B-C11B \\sim C9A-C7A \\sim C9B-
 C7B \\sim C9A-C11A \\sim C9B-C11B
 with sigma of 0.02
2. Uiso/Uaniso restraints and constraints
C11A \\sim N005 \\sim C10B \\sim C12B \\sim C13B \\sim C14B \\sim C14A \\sim
C12A \\sim C10A \\sim C13A \\sim C7B \\sim C7A \\sim C9B \\sim C11B \\sim C9A:
within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
3. Others
 Sof(C10B)=Sof(C12B)=Sof(C14B)=1-FVAR(1)
 Sof(C14A)=Sof(C12A)=Sof(C10A)=FVAR(1)
 Sof(C7B)=Sof(C13B)=1-FVAR(2)
 Sof(C13A)=Sof(C7A)=FVAR(2)
 Sof(C9B)=Sof(C11B)=1-FVAR(3)
 Sof(C9A)=Sof(C11A)=FVAR(3)
;
_atom_sites_solution_hydrogens   .
_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
Pb01 Pb 0.75011(5) 0.65241(8) 0.65286(3) 0.0486(3) Uani 1 1 d . . . . .
Br02 Br 0.67779(14) 0.4044(3) 0.56048(11) 0.0714(6) Uani 1 1 d . . . . .
Br03 Br 0.68176(14) 0.4037(3) 0.75036(11) 0.0711(6) Uani 1 1 d . . . . .
Br04 Br 0.61233(12) 0.8991(3) 0.65067(12) 0.0714(6) Uani 1 1 d . . . . .
N005 N 0.4323(12) 0.417(3) 0.6368(10) 0.101(5) Uani 1 1 d D U . . .
C7B C 0.384(4) 0.206(5) 0.541(4) 0.112(6) Uani 0.33(5) 1 d D U P A 2
C9B C 0.339(2) 0.050(6) 0.568(2) 0.113(6) Uani 0.74(4) 1 d D U P A 2
C10B C 0.476(4) 0.520(10) 0.585(3) 0.104(8) Uani 0.43(4) 1 d D U P A 2
C11B C 0.413(2) 0.020(6) 0.528(2) 0.113(6) Uani 0.74(4) 1 d D U P A 2
C12B C 0.496(4) 0.384(10) 0.687(3) 0.102(9) Uani 0.43(4) 1 d D U P A 2
C13B C 0.448(5) 0.294(12) 0.581(4) 0.108(5) Uani 0.33(5) 1 d D U P A 2
C14B C 0.358(3) 0.529(10) 0.643(4) 0.106(8) Uani 0.43(4) 1 d D U P A 2
C14A C 0.350(2) 0.415(6) 0.667(2) 0.105(9) Uani 0.57(4) 1 d D U P A 1
C12A C 0.487(3) 0.483(6) 0.689(2) 0.103(9) Uani 0.57(4) 1 d D U P A 1
C10A C 0.440(3) 0.577(6) 0.594(2) 0.105(8) Uani 0.57(4) 1 d D U P A 1
C13A C 0.453(2) 0.230(5) 0.617(2) 0.108(6) Uani 0.67(5) 1 d D U P A 1
C7A C 0.396(3) 0.194(6) 0.563(2) 0.111(6) Uani 0.67(5) 1 d D U P A 1
C9A C 0.363(8) 0.054(11) 0.519(4) 0.112(6) Uani 0.26(4) 1 d D U P A 1
C11A C 0.402(8) 0.001(8) 0.581(5) 0.112(6) Uani 0.26(4) 1 d D 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
Pb01 Br02 3.002(2) . ?
Pb01 Br02 3.019(2) 8_765 ?
Pb01 Br03 3.062(2) 8_765 ?
Pb01 Br03 3.051(2) . ?
Pb01 Br04 3.015(2) . ?
Pb01 Br04 3.045(2) 8_755 ?
N005 C10B 1.537(18) . ?
N005 C12B 1.536(18) . ?
N005 C13B 1.536(18) . ?
N005 C14B 1.535(18) . ?
N005 C14A 1.537(16) . ?
N005 C12A 1.537(17) . ?
N005 C10A 1.530(17) . ?
N005 C13A 1.535(16) . ?
C7B C9B 1.536(19) . ?
C7B C11B 1.535(19) . ?
C7B C13B 1.533(19) . ?
C9B C11B 1.538(18) . ?
C13A C7A 1.530(18) . ?
C7A C9A 1.536(19) . ?
C7A C11A 1.534(19) . ?
C9A C11A 1.535(19) . ?

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
Br02 Pb01 Br02 98.35(8) . 8_765 ?
Br02 Pb01 Br03 177.64(7) 8_765 . ?
Br02 Pb01 Br03 83.40(7) 8_765 8_765 ?
Br02 Pb01 Br03 83.88(7) . . ?
Br02 Pb01 Br03 177.76(7) . 8_765 ?
Br02 Pb01 Br04 94.90(7) 8_765 8_755 ?
Br02 Pb01 Br04 84.34(7) . 8_755 ?
Br02 Pb01 Br04 93.90(7) . . ?
Br03 Pb01 Br03 94.38(8) . 8_765 ?
Br04 Pb01 Br02 84.55(6) . 8_765 ?
Br04 Pb01 Br03 84.87(6) . 8_765 ?
Br04 Pb01 Br03 84.56(6) 8_755 . ?
Br04 Pb01 Br03 96.07(7) . . ?
Br04 Pb01 Br03 96.91(7) 8_755 8_765 ?
Br04 Pb01 Br04 178.06(10) . 8_755 ?
Pb01 Br02 Pb01 79.12(5) . 8_755 ?
Pb01 Br03 Pb01 77.71(6) . 8_755 ?
Pb01 Br04 Pb01 78.52(5) . 8_765 ?
C12B N005 C10B 104(4) . . ?
C13B N005 C10B 72(5) . . ?
C13B N005 C12B 108(5) . . ?
C14B N005 C10B 100(4) . . ?
C14B N005 C12B 128(5) . . ?
C14B N005 C13B 124(5) . . ?
C12A N005 C14A 105(4) . . ?
C10A N005 C14A 109.5(16) . . ?
C10A N005 C12A 97(3) . . ?
C10A N005 C13A 125(3) . . ?
C13A N005 C14A 108.0(16) . . ?
C13A N005 C12A 111.6(18) . . ?
C11B C7B C9B 60.1(8) . . ?
C13B C7B C9B 119(6) . . ?
C13B C7B C11B 107(5) . . ?
C7B C9B C11B 59.9(8) . . ?
C7B C11B C9B 60.0(8) . . ?
C7B C13B N005 125(6) . . ?
C7A C13A N005 103(3) . . ?
C13A C7A C9A 145(5) . . ?
C13A C7A C11A 87(5) . . ?
C11A C7A C9A 60.0(8) . . ?
C11A C9A C7A 59.9(8) . . ?
C7A C11A C9A 60.1(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
N005 C13A C7A C9A -171(11) . . . . ?
N005 C13A C7A C11A -153(6) . . . . ?
C9B C7B C13B N005 -76(10) . . . . ?
C10B N005 C13B C7B -117(10) . . . . ?
C11B C7B C13B N005 -141(8) . . . . ?
C12B N005 C13B C7B 144(8) . . . . ?
C13B C7B C9B C11B -94(5) . . . . ?
C13B C7B C11B C9B 114(6) . . . . ?
C14B N005 C13B C7B -26(12) . . . . ?
C14A N005 C13A C7A 68(4) . . . . ?
C12A N005 C13A C7A -177(4) . . . . ?
C10A N005 C13A C7A -62(4) . . . . ?
C13A C7A C9A C11A 21(15) . . . . ?
C13A C7A C11A C9A -168(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 7.161
_oxdiff_exptl_absorpt_empirical_full_min 0.478
